 
data_sad_a
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C40 H62 Cl6 Co2 Li N2, C20 H32 N, C4 H8 O'
_chemical_formula_sum
 'C64 H102 Cl6 Co2 Li N3 O' 
_chemical_formula_weight          1266.98

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Li'  'Li'  -0.0003   0.0001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       tetragonal
_space_group_IT_number            81
_space_group_name_H-M_alt         'P -4'
_space_group_name_Hall            'P -4'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 'y, -x, -z'
 '-y, x, -z'
 
_cell_length_a                    25.322(2)
_cell_length_b                    25.322(2)
_cell_length_c                    10.553(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      6766.6(17)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     8924 
_cell_measurement_theta_min       2.24 
_cell_measurement_theta_max       21.278  
 
_exptl_crystal_description        needle
_exptl_crystal_colour             blue  
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.244          
_exptl_crystal_F_000              2696
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.04 
_exptl_absorpt_coefficient_mu     0.767
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan  
_exptl_absorpt_correction_T_min   0.6849  
_exptl_absorpt_correction_T_max   0.7452  
_exptl_absorpt_process_details    'SADABS-2012/1' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'rotating anode'                       
_diffrn_measurement_device_type   'Smart APEX II Ultra' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             101142
_diffrn_reflns_av_unetI/netI      0.0528
_diffrn_reflns_av_R_equivalents   0.0912
_diffrn_reflns_limit_h_min        -30
_diffrn_reflns_limit_h_max        30
_diffrn_reflns_limit_k_min        -30
_diffrn_reflns_limit_k_max        30
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          1.137
_diffrn_reflns_theta_max          25.365
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              12397
_reflns_number_gt                 10659
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.886
_reflns_Friedel_fraction_max      0.999
_reflns_Friedel_fraction_full     1.000
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'APEX2 v2012.2'
_computing_cell_refinement        'SAINT V7.68A'
_computing_data_reduction         'SAINT V7.68A'
_computing_structure_solution     'SHELXS-2012 (Sheldrick, 2012)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     'XSHELL in SHELXTL-97'
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0201P)²+1.8688P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Flack x determined using 4532 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack    0.011(7)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          12397
_refine_ls_number_parameters      746
_refine_ls_number_restraints      176
_refine_ls_R_factor_all           0.0462
_refine_ls_R_factor_gt            0.0330
_refine_ls_wR_factor_ref          0.0643
_refine_ls_wR_factor_gt           0.0602
_refine_ls_goodness_of_fit_ref    1.022
_refine_ls_restrained_S_all       1.027
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Li1 Li 0.7607(3) 0.2106(3) 0.6213(7) 0.0257(17) Uani 1 1 d . . . . .
Co2 Co 0.88222(2) 0.23988(2) 0.60528(5) 0.01282(12) Uani 1 1 d . . . . .
Co1 Co 0.63951(2) 0.20846(2) 0.66475(5) 0.01671(13) Uani 1 1 d . . . . .
Cl1 Cl 0.89762(4) 0.32291(4) 0.53691(11) 0.0213(2) Uani 1 1 d . . . . .
Cl2 Cl 0.82895(4) 0.19110(4) 0.47057(9) 0.0191(2) Uani 1 1 d . . . . .
Cl3 Cl 0.82465(4) 0.24635(4) 0.77066(10) 0.0187(2) Uani 1 1 d . . . . .
Cl4 Cl 0.61684(4) 0.25772(4) 0.83692(10) 0.0267(2) Uani 1 1 d . . . . .
Cl5 Cl 0.70204(4) 0.14524(4) 0.70460(10) 0.0210(2) Uani 1 1 d . . . . .
Cl6 Cl 0.68945(4) 0.26147(4) 0.53509(10) 0.0228(2) Uani 1 1 d . . . . .
N1 N 0.97958(12) 0.18857(12) 0.7218(3) 0.0115(7) Uani 1 1 d . . . . .
N2 N 0.54191(12) 0.14414(12) 0.6048(3) 0.0149(7) Uani 1 1 d . . . . .
N3 N 0.73946(12) 0.32093(12) 1.0911(3) 0.0128(7) Uani 1 1 d . . . . .
C1 C 0.95346(15) 0.20270(14) 0.6215(4) 0.0124(8) Uani 1 1 d . . . . .
C2 C 0.98654(15) 0.18969(15) 0.5049(4) 0.0137(9) Uani 1 1 d . . . . .
C3 C 1.04243(15) 0.17961(16) 0.5580(4) 0.0154(9) Uani 1 1 d . . . . .
H3A H 1.0593 0.1496 0.5134 0.018 Uiso 1 1 calc R U . . .
H3B H 1.0648 0.2113 0.5471 0.018 Uiso 1 1 calc R U . . .
C4 C 1.03548(15) 0.16684(15) 0.6989(4) 0.0144(9) Uani 1 1 d . . . . .
C5 C 0.96232(16) 0.13942(16) 0.4464(4) 0.0180(9) Uani 1 1 d . . . . .
H5A H 0.9257 0.1465 0.4213 0.027 Uiso 1 1 calc R U . . .
H5B H 0.9630 0.1108 0.5089 0.027 Uiso 1 1 calc R U . . .
H5C H 0.9828 0.1290 0.3717 0.027 Uiso 1 1 calc R U . . .
C6 C 0.98611(16) 0.23368(15) 0.4058(4) 0.0180(9) Uani 1 1 d . . . . .
H6A H 1.0096 0.2241 0.3356 0.027 Uiso 1 1 calc R U . . .
H6B H 0.9984 0.2667 0.4445 0.027 Uiso 1 1 calc R U . . .
H6C H 0.9501 0.2385 0.3737 0.027 Uiso 1 1 calc R U . . .
C7 C 1.03751(16) 0.10758(15) 0.7293(4) 0.0182(9) Uani 1 1 d . . . . .
H7A H 1.0135 0.0885 0.6726 0.027 Uiso 1 1 calc R U . . .
H7B H 1.0267 0.1019 0.8174 0.027 Uiso 1 1 calc R U . . .
H7C H 1.0736 0.0945 0.7172 0.027 Uiso 1 1 calc R U . . .
C8 C 1.07652(15) 0.19514(16) 0.7807(4) 0.0186(9) Uani 1 1 d . . . . .
H8A H 1.1117 0.1811 0.7618 0.028 Uiso 1 1 calc R U . . .
H8B H 1.0684 0.1894 0.8705 0.028 Uiso 1 1 calc R U . . .
H8C H 1.0757 0.2331 0.7623 0.028 Uiso 1 1 calc R U . . .
C9 C 0.95769(14) 0.18881(15) 0.8501(4) 0.0125(8) Uani 1 1 d . . . . .
C10 C 0.92823(15) 0.14503(15) 0.8918(4) 0.0137(8) Uani 1 1 d . . . . .
C11 C 0.91088(16) 0.14513(16) 1.0169(4) 0.0189(9) Uani 1 1 d . . . . .
H11 H 0.8913 0.1158 1.0472 0.023 Uiso 1 1 calc R U . . .
C12 C 0.92128(15) 0.18660(15) 1.0986(4) 0.0184(9) Uani 1 1 d . . . . .
H12 H 0.9099 0.1853 1.1843 0.022 Uiso 1 1 calc R U . . .
C13 C 0.94867(15) 0.23012(16) 1.0532(4) 0.0171(9) Uani 1 1 d . . . . .
H13 H 0.9552 0.2590 1.1086 0.021 Uiso 1 1 calc R U . . .
C14 C 0.96676(15) 0.23271(15) 0.9293(4) 0.0140(9) Uani 1 1 d . . . . .
C15 C 0.91149(16) 0.09880(15) 0.8078(4) 0.0170(9) Uani 1 1 d . . . . .
H15 H 0.9297 0.1024 0.7241 0.020 Uiso 1 1 calc R U . . .
C16 C 0.92681(17) 0.04487(15) 0.8657(4) 0.0246(11) Uani 1 1 d . . . . .
H16A H 0.9206 0.0169 0.8034 0.037 Uiso 1 1 calc R U . . .
H16B H 0.9053 0.0383 0.9413 0.037 Uiso 1 1 calc R U . . .
H16C H 0.9643 0.0453 0.8892 0.037 Uiso 1 1 calc R U . . .
C17 C 0.85155(15) 0.10048(16) 0.7852(4) 0.0217(10) Uani 1 1 d . . . . .
H17A H 0.8422 0.1337 0.7432 0.033 Uiso 1 1 calc R U . . .
H17B H 0.8331 0.0981 0.8666 0.033 Uiso 1 1 calc R U . . .
H17C H 0.8412 0.0707 0.7313 0.033 Uiso 1 1 calc R U . . .
C18 C 0.99214(15) 0.28422(15) 0.8842(4) 0.0175(9) Uani 1 1 d . . . . .
H18 H 1.0051 0.2791 0.7955 0.021 Uiso 1 1 calc R U . . .
C19 C 0.95053(17) 0.32815(16) 0.8838(4) 0.0229(10) Uani 1 1 d . . . . .
H19A H 0.9658 0.3603 0.8473 0.034 Uiso 1 1 calc R U . . .
H19B H 0.9391 0.3352 0.9708 0.034 Uiso 1 1 calc R U . . .
H19C H 0.9201 0.3170 0.8329 0.034 Uiso 1 1 calc R U . . .
C20 C 1.03897(17) 0.30015(18) 0.9672(5) 0.0273(11) Uani 1 1 d . . . . .
H20A H 1.0642 0.2709 0.9716 0.041 Uiso 1 1 calc R U . . .
H20B H 1.0264 0.3086 1.0527 0.041 Uiso 1 1 calc R U . . .
H20C H 1.0563 0.3312 0.9306 0.041 Uiso 1 1 calc R U . . .
C21 C 0.56842(15) 0.18765(15) 0.5892(4) 0.0155(9) Uani 1 1 d . . . . .
C22 C 0.53403(15) 0.22678(15) 0.5163(4) 0.0176(9) Uani 1 1 d . . . . .
C23 C 0.47780(15) 0.20366(16) 0.5285(4) 0.0205(10) Uani 1 1 d . . . . .
H23A H 0.4582 0.2218 0.5970 0.025 Uiso 1 1 calc R U . . .
H23B H 0.4582 0.2082 0.4482 0.025 Uiso 1 1 calc R U . . .
C24 C 0.48395(15) 0.14500(16) 0.5594(4) 0.0182(9) Uani 1 1 d . . . . .
C25 C 0.55433(17) 0.22651(17) 0.3781(4) 0.0258(10) Uani 1 1 d . . . . .
H25A H 0.5504 0.1910 0.3423 0.039 Uiso 1 1 calc R U . . .
H25B H 0.5917 0.2366 0.3767 0.039 Uiso 1 1 calc R U . . .
H25C H 0.5338 0.2517 0.3276 0.039 Uiso 1 1 calc R U . . .
C26 C 0.53772(17) 0.28271(16) 0.5679(4) 0.0252(11) Uani 1 1 d . . . . .
H26A H 0.5738 0.2960 0.5565 0.038 Uiso 1 1 calc R U . . .
H26B H 0.5288 0.2827 0.6582 0.038 Uiso 1 1 calc R U . . .
H26C H 0.5130 0.3055 0.5221 0.038 Uiso 1 1 calc R U . . .
C27 C 0.44728(16) 0.12746(17) 0.6661(4) 0.0255(10) Uani 1 1 d . . . . .
H27A H 0.4105 0.1295 0.6373 0.038 Uiso 1 1 calc R U . . .
H27B H 0.4522 0.1506 0.7396 0.038 Uiso 1 1 calc R U . . .
H27C H 0.4556 0.0910 0.6899 0.038 Uiso 1 1 calc R U . . .
C28 C 0.47561(16) 0.10806(17) 0.4472(4) 0.0237(10) Uani 1 1 d . . . . .
H28A H 0.4386 0.1095 0.4204 0.035 Uiso 1 1 calc R U . . .
H28B H 0.4846 0.0719 0.4721 0.035 Uiso 1 1 calc R U . . .
H28C H 0.4983 0.1191 0.3768 0.035 Uiso 1 1 calc R U . . .
C29 C 0.56540(14) 0.09538(15) 0.6543(4) 0.0149(9) Uani 1 1 d . . . . .
C30 C 0.56191(15) 0.08333(16) 0.7840(4) 0.0173(9) Uani 1 1 d . . . . .
C31 C 0.58356(15) 0.03567(16) 0.8235(4) 0.0196(9) Uani 1 1 d . . . . .
H31 H 0.5813 0.0263 0.9105 0.024 Uiso 1 1 calc R U . . .
C32 C 0.60812(16) 0.00156(16) 0.7411(4) 0.0214(10) Uani 1 1 d . . . . .
H32 H 0.6221 -0.0309 0.7710 0.026 Uiso 1 1 calc R U . . .
C33 C 0.61234(15) 0.01494(16) 0.6141(4) 0.0191(9) Uani 1 1 d . . . . .
H33 H 0.6299 -0.0084 0.5577 0.023 Uiso 1 1 calc R U . . .
C34 C 0.59142(15) 0.06184(15) 0.5678(4) 0.0150(9) Uani 1 1 d . . . . .
C35 C 0.53965(16) 0.12037(17) 0.8847(4) 0.0226(10) Uani 1 1 d . . . . .
H35 H 0.5257 0.1527 0.8418 0.027 Uiso 1 1 calc R U . . .
C36 C 0.58297(17) 0.13695(18) 0.9781(4) 0.0296(11) Uani 1 1 d . . . . .
H36A H 0.6133 0.1508 0.9310 0.044 Uiso 1 1 calc R U . . .
H36B H 0.5940 0.1063 1.0282 0.044 Uiso 1 1 calc R U . . .
H36C H 0.5693 0.1644 1.0347 0.044 Uiso 1 1 calc R U . . .
C37 C 0.49420(18) 0.09433(19) 0.9594(4) 0.0326(12) Uani 1 1 d . . . . .
H37A H 0.4665 0.0831 0.9004 0.049 Uiso 1 1 calc R U . . .
H37B H 0.4795 0.1198 1.0198 0.049 Uiso 1 1 calc R U . . .
H37C H 0.5077 0.0636 1.0054 0.049 Uiso 1 1 calc R U . . .
C38 C 0.60047(16) 0.07493(16) 0.4284(4) 0.0185(9) Uani 1 1 d . . . . .
H38 H 0.5807 0.1081 0.4082 0.022 Uiso 1 1 calc R U . . .
C39 C 0.65947(16) 0.08466(17) 0.4021(4) 0.0243(10) Uani 1 1 d . . . . .
H39A H 0.6642 0.0946 0.3131 0.036 Uiso 1 1 calc R U . . .
H39B H 0.6795 0.0524 0.4199 0.036 Uiso 1 1 calc R U . . .
H39C H 0.6723 0.1132 0.4567 0.036 Uiso 1 1 calc R U . . .
C40 C 0.58060(17) 0.03141(17) 0.3406(4) 0.0257(10) Uani 1 1 d . . . . .
H40A H 0.5831 0.0433 0.2524 0.039 Uiso 1 1 calc R U . . .
H40B H 0.5437 0.0233 0.3609 0.039 Uiso 1 1 calc R U . . .
H40C H 0.6022 -0.0003 0.3521 0.039 Uiso 1 1 calc R U . . .
C41 C 0.71312(16) 0.28015(15) 1.0561(4) 0.0156(9) Uani 1 1 d . . . . .
H41 H 0.6832 0.2821 1.0019 0.019 Uiso 1 1 calc R U . . .
C42 C 0.73373(16) 0.22922(15) 1.1081(4) 0.0184(9) Uani 1 1 d . . . . .
C43 C 0.78759(18) 0.24641(15) 1.1621(5) 0.0280(11) Uani 1 1 d . . . . .
H43A H 0.7934 0.2300 1.2461 0.034 Uiso 1 1 calc R U . . .
H43B H 0.8164 0.2350 1.1048 0.034 Uiso 1 1 calc R U . . .
C44 C 0.78744(16) 0.30685(15) 1.1745(4) 0.0181(9) Uani 1 1 d . . . . .
C45 C 0.6944(2) 0.21058(18) 1.2083(5) 0.0355(12) Uani 1 1 d . . . . .
H45A H 0.6599 0.2048 1.1688 0.053 Uiso 1 1 calc R U . . .
H45B H 0.6912 0.2375 1.2746 0.053 Uiso 1 1 calc R U . . .
H45C H 0.7070 0.1775 1.2458 0.053 Uiso 1 1 calc R U . . .
C46 C 0.73938(18) 0.18688(16) 1.0070(4) 0.0251(11) Uani 1 1 d . . . . .
H46A H 0.7046 0.1789 0.9709 0.038 Uiso 1 1 calc R U . . .
H46B H 0.7542 0.1548 1.0450 0.038 Uiso 1 1 calc R U . . .
H46C H 0.7629 0.1996 0.9399 0.038 Uiso 1 1 calc R U . . .
C47 C 0.77856(17) 0.32738(17) 1.3075(4) 0.0233(10) Uani 1 1 d . . . . .
H47A H 0.7735 0.3657 1.3048 0.035 Uiso 1 1 calc R U . . .
H47B H 0.8093 0.3191 1.3601 0.035 Uiso 1 1 calc R U . . .
H47C H 0.7471 0.3106 1.3436 0.035 Uiso 1 1 calc R U . . .
C48 C 0.83716(15) 0.33111(17) 1.1184(4) 0.0243(10) Uani 1 1 d . . . . .
H48A H 0.8429 0.3170 1.0330 0.036 Uiso 1 1 calc R U . . .
H48B H 0.8675 0.3224 1.1720 0.036 Uiso 1 1 calc R U . . .
H48C H 0.8331 0.3696 1.1139 0.036 Uiso 1 1 calc R U . . .
C49 C 0.72446(16) 0.37567(15) 1.0666(4) 0.0169(9) Uani 1 1 d . . . . .
C50 C 0.68866(16) 0.39933(16) 1.1511(4) 0.0187(9) Uani 1 1 d . . . . .
C51 C 0.68094(17) 0.45387(16) 1.1378(4) 0.0235(10) Uani 1 1 d . . . . .
H51 H 0.6576 0.4717 1.1937 0.028 Uiso 1 1 calc R U . . .
C52 C 0.70695(17) 0.48202(17) 1.0442(4) 0.0247(10) Uani 1 1 d . . . . .
H52 H 0.7031 0.5193 1.0399 0.030 Uiso 1 1 calc R U . . .
C53 C 0.73845(17) 0.45630(16) 0.9570(4) 0.0236(10) Uani 1 1 d . . . . .
H53 H 0.7542 0.4759 0.8903 0.028 Uiso 1 1 calc R U . . .
C54 C 0.74767(16) 0.40209(16) 0.9648(4) 0.0191(9) Uani 1 1 d . . . . .
C55 C 0.65480(17) 0.36876(17) 1.2442(4) 0.0242(10) Uani 1 1 d . . . . .
H55 H 0.6709 0.3330 1.2554 0.029 Uiso 1 1 calc R U . . .
C56 C 0.6513(2) 0.39495(18) 1.3749(4) 0.0348(12) Uani 1 1 d . . . . .
H56A H 0.6869 0.4039 1.4045 0.052 Uiso 1 1 calc R U . . .
H56B H 0.6347 0.3705 1.4349 0.052 Uiso 1 1 calc R U . . .
H56C H 0.6300 0.4272 1.3688 0.052 Uiso 1 1 calc R U . . .
C57 C 0.59937(18) 0.36135(19) 1.1876(5) 0.0376(13) Uani 1 1 d . . . . .
H57A H 0.5831 0.3960 1.1735 0.056 Uiso 1 1 calc R U . . .
H57B H 0.5775 0.3408 1.2464 0.056 Uiso 1 1 calc R U . . .
H57C H 0.6021 0.3425 1.1067 0.056 Uiso 1 1 calc R U . . .
C58 C 0.77584(16) 0.37365(16) 0.8571(4) 0.0193(10) Uani 1 1 d . . . . .
H58 H 0.7844 0.3371 0.8864 0.023 Uiso 1 1 calc R U . . .
C59 C 0.73788(18) 0.36919(17) 0.7447(4) 0.0271(11) Uani 1 1 d . . . . .
H59A H 0.7552 0.3500 0.6755 0.041 Uiso 1 1 calc R U . . .
H59B H 0.7281 0.4046 0.7157 0.041 Uiso 1 1 calc R U . . .
H59C H 0.7061 0.3501 0.7710 0.041 Uiso 1 1 calc R U . . .
C60 C 0.82714(16) 0.40002(17) 0.8165(4) 0.0247(10) Uani 1 1 d . . . . .
H60A H 0.8440 0.3789 0.7499 0.037 Uiso 1 1 calc R U . . .
H60B H 0.8509 0.4026 0.8895 0.037 Uiso 1 1 calc R U . . .
H60C H 0.8196 0.4355 0.7841 0.037 Uiso 1 1 calc R U . . .
O1 O 0.57218(17) 0.51341(16) 1.2590(4) 0.0627(11) Uani 1 1 d D U . . .
C61 C 0.5586(5) 0.5392(4) 1.1429(9) 0.060(3) Uani 0.682(14) 1 d D U P A 1
H61A H 0.5199 0.5420 1.1316 0.072 Uiso 0.682(14) 1 calc R U P A 1
H61B H 0.5743 0.5213 1.0685 0.072 Uiso 0.682(14) 1 calc R U P A 1
C62 C 0.5842(5) 0.5931(4) 1.1680(8) 0.056(2) Uani 0.682(14) 1 d D U P A 1
H62A H 0.5731 0.6200 1.1053 0.067 Uiso 0.682(14) 1 calc R U P A 1
H62B H 0.6232 0.5909 1.1708 0.067 Uiso 0.682(14) 1 calc R U P A 1
C63 C 0.5592(6) 0.6036(4) 1.3047(9) 0.062(3) Uani 0.682(14) 1 d D U P A 1
H63A H 0.5804 0.6291 1.3544 0.075 Uiso 0.682(14) 1 calc R U P A 1
H63B H 0.5223 0.6163 1.2988 0.075 Uiso 0.682(14) 1 calc R U P A 1
C64 C 0.5621(3) 0.5486(2) 1.3595(5) 0.0578(16) Uani 1 1 d D U . . .
H64A H 0.5907 0.5465 1.4231 0.069 Uiso 0.682(14) 1 calc R U P A 1
H64B H 0.5284 0.5394 1.4014 0.069 Uiso 0.682(14) 1 calc R U P A 1
H64C H 0.5815 0.5380 1.4369 0.069 Uiso 0.318(14) 1 calc R U P A 2
H64D H 0.5239 0.5504 1.3787 0.069 Uiso 0.318(14) 1 calc R U P A 2
C61' C 0.5819(11) 0.5490(8) 1.1465(18) 0.063(4) Uani 0.318(14) 1 d D U P A 2
H61C H 0.6203 0.5547 1.1346 0.075 Uiso 0.318(14) 1 calc R U P A 2
H61D H 0.5674 0.5329 1.0685 0.075 Uiso 0.318(14) 1 calc R U P A 2
C62' C 0.5549(11) 0.6002(7) 1.1739(18) 0.059(3) Uani 0.318(14) 1 d D U P A 2
H62C H 0.5159 0.5974 1.1781 0.071 Uiso 0.318(14) 1 calc R U P A 2
H62D H 0.5658 0.6294 1.1172 0.071 Uiso 0.318(14) 1 calc R U P A 2
C63' C 0.5825(10) 0.6015(7) 1.3082(18) 0.053(4) Uani 0.318(14) 1 d D U P A 2
H63C H 0.6215 0.6021 1.3013 0.063 Uiso 0.318(14) 1 calc R U P A 2
H63D H 0.5704 0.6317 1.3602 0.063 Uiso 0.318(14) 1 calc R U P A 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Li1 Cl5 2.390(7) . ?
Li1 Cl6 2.396(7) . ?
Li1 Cl2 2.401(7) . ?
Li1 Cl3 2.435(7) . ?
Li1 Co1 3.102(7) . ?
Li1 Co2 3.171(7) . ?
Co2 C1 2.042(4) . ?
Co2 Cl1 2.2568(11) . ?
Co2 Cl3 2.2799(11) . ?
Co2 Cl2 2.3167(11) . ?
Co1 C21 2.038(4) . ?
Co1 Cl4 2.2773(12) . ?
Co1 Cl5 2.2907(12) . ?
Co1 Cl6 2.2964(12) . ?
N1 C1 1.298(5) . ?
N1 C9 1.463(5) . ?
N1 C4 1.538(5) . ?
N2 C21 1.301(5) . ?
N2 C29 1.466(5) . ?
N2 C24 1.544(5) . ?
N3 C41 1.284(5) . ?
N3 C49 1.460(5) . ?
N3 C44 1.542(5) . ?
C1 C2 1.525(5) . ?
C2 C6 1.528(5) . ?
C2 C5 1.542(5) . ?
C2 C3 1.543(5) . ?
C3 C4 1.532(5) . ?
C4 C8 1.529(5) . ?
C4 C7 1.535(5) . ?
C9 C10 1.407(5) . ?
C9 C14 1.410(5) . ?
C10 C11 1.391(6) . ?
C10 C15 1.528(5) . ?
C11 C12 1.384(6) . ?
C12 C13 1.387(6) . ?
C13 C14 1.388(5) . ?
C14 C18 1.530(5) . ?
C15 C17 1.537(5) . ?
C15 C16 1.546(5) . ?
C18 C20 1.529(6) . ?
C18 C19 1.532(5) . ?
C21 C22 1.527(5) . ?
C22 C26 1.520(5) . ?
C22 C23 1.545(5) . ?
C22 C25 1.547(6) . ?
C23 C24 1.529(5) . ?
C24 C28 1.524(6) . ?
C24 C27 1.525(6) . ?
C29 C30 1.406(6) . ?
C29 C34 1.410(5) . ?
C30 C31 1.390(5) . ?
C30 C35 1.525(6) . ?
C31 C32 1.374(6) . ?
C32 C33 1.386(6) . ?
C33 C34 1.389(5) . ?
C34 C38 1.526(5) . ?
C35 C36 1.533(6) . ?
C35 C37 1.543(6) . ?
C38 C40 1.525(6) . ?
C38 C39 1.539(6) . ?
C41 C42 1.496(5) . ?
C42 C46 1.520(6) . ?
C42 C45 1.526(6) . ?
C42 C43 1.541(6) . ?
C43 C44 1.536(5) . ?
C44 C47 1.513(6) . ?
C44 C48 1.521(6) . ?
C49 C54 1.395(6) . ?
C49 C50 1.406(6) . ?
C50 C51 1.402(6) . ?
C50 C55 1.516(6) . ?
C51 C52 1.385(6) . ?
C52 C53 1.381(6) . ?
C53 C54 1.395(5) . ?
C54 C58 1.523(6) . ?
C55 C56 1.533(6) . ?
C55 C57 1.537(6) . ?
C58 C60 1.522(6) . ?
C58 C59 1.531(6) . ?
O1 C64 1.408(6) . ?
O1 C61 1.430(9) . ?
O1 C61' 1.511(17) . ?
C61 C62 1.535(12) . ?
C62 C63 1.598(13) . ?
C63 C64 1.510(10) . ?
C64 C63' 1.534(17) . ?
C61' C62' 1.495(19) . ?
C62' C63' 1.58(2) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
Cl5 Li1 Cl6 92.6(2) . . ?
Cl5 Li1 Cl2 123.3(3) . . ?
Cl6 Li1 Cl2 113.6(3) . . ?
Cl5 Li1 Cl3 115.6(3) . . ?
Cl6 Li1 Cl3 123.1(3) . . ?
Cl2 Li1 Cl3 91.5(2) . . ?
Cl5 Li1 Co1 47.13(13) . . ?
Cl6 Li1 Co1 47.25(13) . . ?
Cl2 Li1 Co1 143.8(3) . . ?
Cl3 Li1 Co1 124.7(3) . . ?
Cl5 Li1 Co2 141.7(3) . . ?
Cl6 Li1 Co2 125.8(3) . . ?
Cl2 Li1 Co2 46.65(12) . . ?
Cl3 Li1 Co2 45.70(12) . . ?
Co1 Li1 Co2 166.4(3) . . ?
C1 Co2 Cl1 107.68(10) . . ?
C1 Co2 Cl3 122.26(11) . . ?
Cl1 Co2 Cl3 106.76(4) . . ?
C1 Co2 Cl2 108.67(11) . . ?
Cl1 Co2 Cl2 113.65(4) . . ?
Cl3 Co2 Cl2 97.80(4) . . ?
C1 Co2 Li1 138.18(17) . . ?
Cl1 Co2 Li1 113.75(14) . . ?
Cl3 Co2 Li1 49.85(14) . . ?
Cl2 Co2 Li1 48.91(14) . . ?
C21 Co1 Cl4 103.36(11) . . ?
C21 Co1 Cl5 120.12(11) . . ?
Cl4 Co1 Cl5 114.24(4) . . ?
C21 Co1 Cl6 113.85(12) . . ?
Cl4 Co1 Cl6 107.10(5) . . ?
Cl5 Co1 Cl6 97.88(4) . . ?
C21 Co1 Li1 145.10(18) . . ?
Cl4 Co1 Li1 110.95(14) . . ?
Cl5 Co1 Li1 49.88(14) . . ?
Cl6 Co1 Li1 50.00(14) . . ?
Co2 Cl2 Li1 84.44(17) . . ?
Co2 Cl3 Li1 84.45(18) . . ?
Co1 Cl5 Li1 82.99(18) . . ?
Co1 Cl6 Li1 82.75(18) . . ?
C1 N1 C9 124.1(3) . . ?
C1 N1 C4 116.1(3) . . ?
C9 N1 C4 119.7(3) . . ?
C21 N2 C29 123.3(3) . . ?
C21 N2 C24 116.1(3) . . ?
C29 N2 C24 120.5(3) . . ?
C41 N3 C49 125.3(3) . . ?
C41 N3 C44 112.8(3) . . ?
C49 N3 C44 121.7(3) . . ?
N1 C1 C2 108.6(3) . . ?
N1 C1 Co2 130.2(3) . . ?
C2 C1 Co2 121.1(3) . . ?
C1 C2 C6 113.0(3) . . ?
C1 C2 C5 106.4(3) . . ?
C6 C2 C5 108.9(3) . . ?
C1 C2 C3 104.3(3) . . ?
C6 C2 C3 112.1(3) . . ?
C5 C2 C3 111.9(3) . . ?
C4 C3 C2 106.4(3) . . ?
C8 C4 C3 111.8(3) . . ?
C8 C4 C7 108.5(3) . . ?
C3 C4 C7 113.9(3) . . ?
C8 C4 N1 111.7(3) . . ?
C3 C4 N1 100.5(3) . . ?
C7 C4 N1 110.3(3) . . ?
C10 C9 C14 121.5(4) . . ?
C10 C9 N1 119.2(3) . . ?
C14 C9 N1 119.4(3) . . ?
C11 C10 C9 117.6(4) . . ?
C11 C10 C15 117.7(3) . . ?
C9 C10 C15 124.7(4) . . ?
C12 C11 C10 122.2(4) . . ?
C11 C12 C13 118.9(4) . . ?
C12 C13 C14 121.9(4) . . ?
C13 C14 C9 117.9(4) . . ?
C13 C14 C18 118.2(4) . . ?
C9 C14 C18 123.8(3) . . ?
C10 C15 C17 110.0(3) . . ?
C10 C15 C16 112.2(3) . . ?
C17 C15 C16 109.5(3) . . ?
C20 C18 C14 111.9(3) . . ?
C20 C18 C19 110.1(3) . . ?
C14 C18 C19 109.3(3) . . ?
N2 C21 C22 108.6(3) . . ?
N2 C21 Co1 128.7(3) . . ?
C22 C21 Co1 122.2(3) . . ?
C26 C22 C21 112.9(3) . . ?
C26 C22 C23 112.3(3) . . ?
C21 C22 C23 103.8(3) . . ?
C26 C22 C25 108.7(3) . . ?
C21 C22 C25 106.4(3) . . ?
C23 C22 C25 112.6(3) . . ?
C24 C23 C22 107.0(3) . . ?
C28 C24 C27 108.1(3) . . ?
C28 C24 C23 114.6(4) . . ?
C27 C24 C23 112.2(3) . . ?
C28 C24 N2 111.3(3) . . ?
C27 C24 N2 110.2(3) . . ?
C23 C24 N2 100.2(3) . . ?
C30 C29 C34 121.9(4) . . ?
C30 C29 N2 120.3(3) . . ?
C34 C29 N2 117.8(3) . . ?
C31 C30 C29 117.1(4) . . ?
C31 C30 C35 118.1(4) . . ?
C29 C30 C35 124.6(4) . . ?
C32 C31 C30 122.3(4) . . ?
C31 C32 C33 119.5(4) . . ?
C32 C33 C34 121.3(4) . . ?
C33 C34 C29 117.8(4) . . ?
C33 C34 C38 117.9(4) . . ?
C29 C34 C38 124.3(4) . . ?
C30 C35 C36 110.6(3) . . ?
C30 C35 C37 111.6(4) . . ?
C36 C35 C37 108.8(4) . . ?
C40 C38 C34 112.3(3) . . ?
C40 C38 C39 109.1(3) . . ?
C34 C38 C39 110.7(3) . . ?
N3 C41 C42 114.0(4) . . ?
C41 C42 C46 112.5(3) . . ?
C41 C42 C45 107.1(3) . . ?
C46 C42 C45 109.2(3) . . ?
C41 C42 C43 101.6(3) . . ?
C46 C42 C43 112.1(4) . . ?
C45 C42 C43 114.1(4) . . ?
C44 C43 C42 108.1(3) . . ?
C47 C44 C48 110.2(3) . . ?
C47 C44 C43 114.9(4) . . ?
C48 C44 C43 111.6(4) . . ?
C47 C44 N3 109.4(3) . . ?
C48 C44 N3 109.7(3) . . ?
C43 C44 N3 100.6(3) . . ?
C54 C49 C50 123.8(4) . . ?
C54 C49 N3 118.8(3) . . ?
C50 C49 N3 117.4(3) . . ?
C51 C50 C49 116.5(4) . . ?
C51 C50 C55 119.2(4) . . ?
C49 C50 C55 123.9(4) . . ?
C52 C51 C50 120.8(4) . . ?
C53 C52 C51 120.5(4) . . ?
C52 C53 C54 121.4(4) . . ?
C53 C54 C49 116.5(4) . . ?
C53 C54 C58 120.0(4) . . ?
C49 C54 C58 123.0(3) . . ?
C50 C55 C56 113.3(4) . . ?
C50 C55 C57 109.1(4) . . ?
C56 C55 C57 110.5(4) . . ?
C60 C58 C54 113.7(3) . . ?
C60 C58 C59 110.5(3) . . ?
C54 C58 C59 108.6(3) . . ?
C64 O1 C61 108.2(5) . . ?
C64 O1 C61' 104.1(9) . . ?
O1 C61 C62 99.0(7) . . ?
C61 C62 C63 97.9(9) . . ?
C64 C63 C62 99.9(7) . . ?
O1 C64 C63 107.7(5) . . ?
O1 C64 C63' 103.1(9) . . ?
C62' C61' O1 106.9(14) . . ?
C61' C62' C63' 89.3(16) . . ?
C64 C63' C62' 98.6(13) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 N1 C1 C2 -172.0(3) . . . . ?
C4 N1 C1 C2 3.6(4) . . . . ?
C9 N1 C1 Co2 11.2(5) . . . . ?
C4 N1 C1 Co2 -173.2(3) . . . . ?
N1 C1 C2 C6 -137.0(3) . . . . ?
Co2 C1 C2 C6 40.1(4) . . . . ?
N1 C1 C2 C5 103.4(4) . . . . ?
Co2 C1 C2 C5 -79.4(3) . . . . ?
N1 C1 C2 C3 -15.0(4) . . . . ?
Co2 C1 C2 C3 162.1(2) . . . . ?
C1 C2 C3 C4 20.6(4) . . . . ?
C6 C2 C3 C4 143.2(3) . . . . ?
C5 C2 C3 C4 -94.1(4) . . . . ?
C2 C3 C4 C8 -136.5(3) . . . . ?
C2 C3 C4 C7 100.1(4) . . . . ?
C2 C3 C4 N1 -17.9(4) . . . . ?
C1 N1 C4 C8 128.1(4) . . . . ?
C9 N1 C4 C8 -56.1(4) . . . . ?
C1 N1 C4 C3 9.4(4) . . . . ?
C9 N1 C4 C3 -174.8(3) . . . . ?
C1 N1 C4 C7 -111.2(4) . . . . ?
C9 N1 C4 C7 64.6(4) . . . . ?
C1 N1 C9 C10 84.4(5) . . . . ?
C4 N1 C9 C10 -91.0(4) . . . . ?
C1 N1 C9 C14 -95.9(4) . . . . ?
C4 N1 C9 C14 88.6(4) . . . . ?
C14 C9 C10 C11 -3.7(5) . . . . ?
N1 C9 C10 C11 176.0(3) . . . . ?
C14 C9 C10 C15 172.9(3) . . . . ?
N1 C9 C10 C15 -7.4(5) . . . . ?
C9 C10 C11 C12 0.7(6) . . . . ?
C15 C10 C11 C12 -176.2(4) . . . . ?
C10 C11 C12 C13 1.8(6) . . . . ?
C11 C12 C13 C14 -1.3(6) . . . . ?
C12 C13 C14 C9 -1.6(6) . . . . ?
C12 C13 C14 C18 174.5(4) . . . . ?
C10 C9 C14 C13 4.1(5) . . . . ?
N1 C9 C14 C13 -175.5(3) . . . . ?
C10 C9 C14 C18 -171.8(3) . . . . ?
N1 C9 C14 C18 8.6(5) . . . . ?
C11 C10 C15 C17 67.1(4) . . . . ?
C9 C10 C15 C17 -109.5(4) . . . . ?
C11 C10 C15 C16 -55.1(5) . . . . ?
C9 C10 C15 C16 128.3(4) . . . . ?
C13 C14 C18 C20 56.8(5) . . . . ?
C9 C14 C18 C20 -127.3(4) . . . . ?
C13 C14 C18 C19 -65.4(5) . . . . ?
C9 C14 C18 C19 110.5(4) . . . . ?
C29 N2 C21 C22 170.7(3) . . . . ?
C24 N2 C21 C22 -5.3(5) . . . . ?
C29 N2 C21 Co1 -17.2(6) . . . . ?
C24 N2 C21 Co1 166.8(3) . . . . ?
N2 C21 C22 C26 138.3(4) . . . . ?
Co1 C21 C22 C26 -34.5(5) . . . . ?
N2 C21 C22 C23 16.4(4) . . . . ?
Co1 C21 C22 C23 -156.3(3) . . . . ?
N2 C21 C22 C25 -102.5(4) . . . . ?
Co1 C21 C22 C25 84.8(4) . . . . ?
C26 C22 C23 C24 -143.6(4) . . . . ?
C21 C22 C23 C24 -21.3(4) . . . . ?
C25 C22 C23 C24 93.3(4) . . . . ?
C22 C23 C24 C28 -101.5(4) . . . . ?
C22 C23 C24 C27 134.7(4) . . . . ?
C22 C23 C24 N2 17.8(4) . . . . ?
C21 N2 C24 C28 113.5(4) . . . . ?
C29 N2 C24 C28 -62.7(5) . . . . ?
C21 N2 C24 C27 -126.6(4) . . . . ?
C29 N2 C24 C27 57.3(5) . . . . ?
C21 N2 C24 C23 -8.2(4) . . . . ?
C29 N2 C24 C23 175.7(3) . . . . ?
C21 N2 C29 C30 95.0(5) . . . . ?
C24 N2 C29 C30 -89.2(4) . . . . ?
C21 N2 C29 C34 -84.7(5) . . . . ?
C24 N2 C29 C34 91.2(4) . . . . ?
C34 C29 C30 C31 -2.4(6) . . . . ?
N2 C29 C30 C31 178.0(3) . . . . ?
C34 C29 C30 C35 173.2(4) . . . . ?
N2 C29 C30 C35 -6.5(6) . . . . ?
C29 C30 C31 C32 0.9(6) . . . . ?
C35 C30 C31 C32 -175.0(4) . . . . ?
C30 C31 C32 C33 0.8(6) . . . . ?
C31 C32 C33 C34 -1.1(6) . . . . ?
C32 C33 C34 C29 -0.4(6) . . . . ?
C32 C33 C34 C38 176.7(4) . . . . ?
C30 C29 C34 C33 2.1(6) . . . . ?
N2 C29 C34 C33 -178.2(3) . . . . ?
C30 C29 C34 C38 -174.7(4) . . . . ?
N2 C29 C34 C38 5.0(5) . . . . ?
C31 C30 C35 C36 60.8(5) . . . . ?
C29 C30 C35 C36 -114.7(4) . . . . ?
C31 C30 C35 C37 -60.5(5) . . . . ?
C29 C30 C35 C37 124.0(4) . . . . ?
C33 C34 C38 C40 56.1(5) . . . . ?
C29 C34 C38 C40 -127.0(4) . . . . ?
C33 C34 C38 C39 -66.1(5) . . . . ?
C29 C34 C38 C39 110.8(4) . . . . ?
C49 N3 C41 C42 -172.4(3) . . . . ?
C44 N3 C41 C42 2.3(5) . . . . ?
N3 C41 C42 C46 -132.0(4) . . . . ?
N3 C41 C42 C45 107.9(4) . . . . ?
N3 C41 C42 C43 -12.0(5) . . . . ?
C41 C42 C43 C44 16.8(4) . . . . ?
C46 C42 C43 C44 137.2(4) . . . . ?
C45 C42 C43 C44 -98.0(4) . . . . ?
C42 C43 C44 C47 101.9(4) . . . . ?
C42 C43 C44 C48 -131.7(4) . . . . ?
C42 C43 C44 N3 -15.5(4) . . . . ?
C41 N3 C44 C47 -112.8(4) . . . . ?
C49 N3 C44 C47 62.1(4) . . . . ?
C41 N3 C44 C48 126.2(4) . . . . ?
C49 N3 C44 C48 -58.9(5) . . . . ?
C41 N3 C44 C43 8.5(4) . . . . ?
C49 N3 C44 C43 -176.5(3) . . . . ?
C41 N3 C49 C54 -98.4(5) . . . . ?
C44 N3 C49 C54 87.3(5) . . . . ?
C41 N3 C49 C50 84.0(5) . . . . ?
C44 N3 C49 C50 -90.2(4) . . . . ?
C54 C49 C50 C51 -6.9(6) . . . . ?
N3 C49 C50 C51 170.5(3) . . . . ?
C54 C49 C50 C55 166.8(4) . . . . ?
N3 C49 C50 C55 -15.8(6) . . . . ?
C49 C50 C51 C52 1.1(6) . . . . ?
C55 C50 C51 C52 -172.8(4) . . . . ?
C50 C51 C52 C53 4.1(7) . . . . ?
C51 C52 C53 C54 -4.0(7) . . . . ?
C52 C53 C54 C49 -1.4(6) . . . . ?
C52 C53 C54 C58 171.1(4) . . . . ?
C50 C49 C54 C53 7.0(6) . . . . ?
N3 C49 C54 C53 -170.3(4) . . . . ?
C50 C49 C54 C58 -165.3(4) . . . . ?
N3 C49 C54 C58 17.4(6) . . . . ?
C51 C50 C55 C56 -47.9(5) . . . . ?
C49 C50 C55 C56 138.6(4) . . . . ?
C51 C50 C55 C57 75.6(5) . . . . ?
C49 C50 C55 C57 -97.9(5) . . . . ?
C53 C54 C58 C60 50.3(5) . . . . ?
C49 C54 C58 C60 -137.6(4) . . . . ?
C53 C54 C58 C59 -73.2(5) . . . . ?
C49 C54 C58 C59 98.9(5) . . . . ?
C64 O1 C61 C62 44.8(10) . . . . ?
C61' O1 C61 C62 -40(2) . . . . ?
O1 C61 C62 C63 -50.4(13) . . . . ?
C61 C62 C63 C64 39.1(13) . . . . ?
C61 O1 C64 C63 -18.9(8) . . . . ?
C61' O1 C64 C63 6.9(12) . . . . ?
C61 O1 C64 C63' -41.8(11) . . . . ?
C61' O1 C64 C63' -16.0(14) . . . . ?
C62 C63 C64 O1 -14.2(11) . . . . ?
C62 C63 C64 C63' 67(2) . . . . ?
C64 O1 C61' C62' -24(2) . . . . ?
C61 O1 C61' C62' 79(3) . . . . ?
O1 C61' C62' C63' 50(3) . . . . ?
O1 C64 C63' C62' 48.2(18) . . . . ?
C63 C64 C63' C62' -57(2) . . . . ?
C61' C62' C63' C64 -57(2) . . . . ?
 
_refine_diff_density_max    0.324
_refine_diff_density_min   -0.269
_refine_diff_density_rms    0.052

_shelxl_version_number 2013-4



 
data_p-1_a
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C20 H32 N, C4 H8 Cl3 Co O'
_chemical_formula_sum
 'C24 H40 Cl3 Co N O' 
_chemical_formula_weight          523.85

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    12.8180(10)
_cell_length_b                    14.3010(10)
_cell_length_c                    15.8490(10)
_cell_angle_alpha                 90.11(2)
_cell_angle_beta                  99.65(2)
_cell_angle_gamma                 108.68(2)
_cell_volume                      2708.5(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9048 
_cell_measurement_theta_min       2.6115 
_cell_measurement_theta_max       25.6205  
 
_exptl_crystal_description        block 
_exptl_crystal_colour             blue 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.285          
_exptl_crystal_F_000              1108
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.1 
_exptl_absorpt_coefficient_mu     0.945
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.6798  
_exptl_absorpt_correction_T_max   0.7453  
_exptl_absorpt_process_details    'SADABS-2012/1'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'INCOATEC Mo Microsource'                       
_diffrn_measurement_device_type   'Bruker Smart APEX II Quazar' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             61259
_diffrn_reflns_av_unetI/netI      0.0249
_diffrn_reflns_av_R_equivalents   0.0391
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.306
_diffrn_reflns_theta_max          25.684
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              10296
_reflns_number_gt                 8902
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'APEX2 v2012.2'
_computing_cell_refinement        'SAINT V8.30C' 
_computing_data_reduction         'SAINT V8.30C' 
_computing_structure_solution     'SHELXS-2012 (Sheldrick, 2012)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     'XP Version 5.1'
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0284P)²+1.7599P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          10296
_refine_ls_number_parameters      557
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0350
_refine_ls_R_factor_gt            0.0282
_refine_ls_wR_factor_ref          0.0713
_refine_ls_wR_factor_gt           0.0668
_refine_ls_goodness_of_fit_ref    1.047
_refine_ls_restrained_S_all       1.047
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Co1 Co -0.25117(2) 0.59227(2) 0.69438(2) 0.01918(7) Uani 1 1 d . . . . .
Co2 Co 0.24029(2) 0.95475(2) 0.80763(2) 0.01759(6) Uani 1 1 d . . . . .
Cl1 Cl -0.36512(4) 0.51425(4) 0.78495(3) 0.02879(11) Uani 1 1 d . . . . .
Cl2 Cl -0.24001(6) 0.50254(4) 0.58237(3) 0.03908(14) Uani 1 1 d . . . . .
Cl3 Cl -0.24677(4) 0.74637(3) 0.66384(3) 0.02222(10) Uani 1 1 d . . . . .
Cl4 Cl 0.22673(4) 0.84497(3) 0.90994(3) 0.02602(11) Uani 1 1 d . . . . .
Cl5 Cl 0.22297(4) 1.09972(3) 0.84536(3) 0.02489(10) Uani 1 1 d . . . . .
Cl6 Cl 0.36635(4) 0.95336(4) 0.72396(3) 0.02921(11) Uani 1 1 d . . . . .
O1 O -0.10052(11) 0.61490(9) 0.77367(8) 0.0231(3) Uani 1 1 d . . . . .
O2 O 0.09801(10) 0.89941(9) 0.71759(8) 0.0184(3) Uani 1 1 d . . . . .
N1 N -0.72182(12) 0.40534(10) 0.70398(9) 0.0150(3) Uani 1 1 d . . . . .
N2 N 0.72208(12) 1.03618(10) 0.80300(9) 0.0142(3) Uani 1 1 d . . . . .
C1 C -0.63763(15) 0.38431(12) 0.68743(11) 0.0168(4) Uani 1 1 d . . . . .
H1 H -0.5637 0.4163 0.7173 0.020 Uiso 1 1 calc R U . . .
C2 C -0.66349(15) 0.30609(13) 0.61794(11) 0.0194(4) Uani 1 1 d . . . . .
C3 C -0.78944(15) 0.28907(14) 0.58479(12) 0.0230(4) Uani 1 1 d . . . . .
H3A H -0.7995 0.3182 0.5286 0.028 Uiso 1 1 calc R U . . .
H3B H -0.8314 0.2174 0.5774 0.028 Uiso 1 1 calc R U . . .
C4 C -0.83344(14) 0.33879(13) 0.65122(11) 0.0184(4) Uani 1 1 d . . . . .
C5 C -0.59006(17) 0.34774(15) 0.55087(12) 0.0270(4) Uani 1 1 d . . . . .
H5A H -0.6081 0.2983 0.5031 0.040 Uiso 1 1 calc R U . . .
H5B H -0.5111 0.3638 0.5771 0.040 Uiso 1 1 calc R U . . .
H5C H -0.6040 0.4077 0.5295 0.040 Uiso 1 1 calc R U . . .
C6 C -0.63792(17) 0.21496(14) 0.65543(13) 0.0258(4) Uani 1 1 d . . . . .
H6A H -0.6841 0.1896 0.6991 0.039 Uiso 1 1 calc R U . . .
H6B H -0.5586 0.2337 0.6816 0.039 Uiso 1 1 calc R U . . .
H6C H -0.6548 0.1635 0.6095 0.039 Uiso 1 1 calc R U . . .
C7 C -0.90512(15) 0.39956(14) 0.61154(12) 0.0225(4) Uani 1 1 d . . . . .
H7A H -0.8686 0.4405 0.5685 0.034 Uiso 1 1 calc R U . . .
H7B H -0.9142 0.4422 0.6564 0.034 Uiso 1 1 calc R U . . .
H7C H -0.9788 0.3551 0.5842 0.034 Uiso 1 1 calc R U . . .
C8 C -0.89674(16) 0.26671(14) 0.71035(12) 0.0252(4) Uani 1 1 d . . . . .
H8A H -0.9678 0.2237 0.6775 0.038 Uiso 1 1 calc R U . . .
H8B H -0.9115 0.3037 0.7565 0.038 Uiso 1 1 calc R U . . .
H8C H -0.8516 0.2264 0.7351 0.038 Uiso 1 1 calc R U . . .
C9 C -0.70899(14) 0.48498(12) 0.76723(11) 0.0156(3) Uani 1 1 d . . . . .
C10 C -0.69507(14) 0.57958(13) 0.73680(11) 0.0165(4) Uani 1 1 d . . . . .
C11 C -0.67967(14) 0.65593(13) 0.79768(11) 0.0181(4) Uani 1 1 d . . . . .
H11 H -0.6725 0.7206 0.7796 0.022 Uiso 1 1 calc R U . . .
C12 C -0.67477(15) 0.63859(13) 0.88381(11) 0.0186(4) Uani 1 1 d . . . . .
H12 H -0.6647 0.6913 0.9241 0.022 Uiso 1 1 calc R U . . .
C13 C -0.68434(14) 0.54492(13) 0.91187(11) 0.0181(4) Uani 1 1 d . . . . .
H13 H -0.6791 0.5348 0.9714 0.022 Uiso 1 1 calc R U . . .
C14 C -0.70152(14) 0.46520(13) 0.85427(11) 0.0161(3) Uani 1 1 d . . . . .
C15 C -0.68603(15) 0.60303(13) 0.64429(11) 0.0189(4) Uani 1 1 d . . . . .
H15 H -0.7106 0.5389 0.6094 0.023 Uiso 1 1 calc R U . . .
C16 C -0.76081(17) 0.66269(15) 0.60700(12) 0.0264(4) Uani 1 1 d . . . . .
H16A H -0.7329 0.7290 0.6357 0.040 Uiso 1 1 calc R U . . .
H16B H -0.8375 0.6294 0.6159 0.040 Uiso 1 1 calc R U . . .
H16C H -0.7601 0.6680 0.5454 0.040 Uiso 1 1 calc R U . . .
C17 C -0.56369(17) 0.65727(15) 0.63779(13) 0.0293(4) Uani 1 1 d . . . . .
H17A H -0.5574 0.6678 0.5775 0.044 Uiso 1 1 calc R U . . .
H17B H -0.5174 0.6174 0.6614 0.044 Uiso 1 1 calc R U . . .
H17C H -0.5381 0.7213 0.6703 0.044 Uiso 1 1 calc R U . . .
C18 C -0.70284(15) 0.36567(13) 0.88791(11) 0.0182(4) Uani 1 1 d . . . . .
H18 H -0.7224 0.3170 0.8377 0.022 Uiso 1 1 calc R U . . .
C19 C -0.58691(16) 0.37165(14) 0.93647(12) 0.0236(4) Uani 1 1 d . . . . .
H19A H -0.5863 0.3051 0.9507 0.035 Uiso 1 1 calc R U . . .
H19B H -0.5694 0.4135 0.9894 0.035 Uiso 1 1 calc R U . . .
H19C H -0.5308 0.4001 0.9005 0.035 Uiso 1 1 calc R U . . .
C20 C -0.79050(16) 0.32795(14) 0.94545(12) 0.0247(4) Uani 1 1 d . . . . .
H20A H -0.8633 0.3290 0.9152 0.037 Uiso 1 1 calc R U . . .
H20B H -0.7685 0.3706 0.9982 0.037 Uiso 1 1 calc R U . . .
H20C H -0.7958 0.2601 0.9597 0.037 Uiso 1 1 calc R U . . .
C21 C 0.63684(14) 0.96881(13) 0.82096(11) 0.0167(4) Uani 1 1 d . . . . .
H21 H 0.5629 0.9595 0.7917 0.020 Uiso 1 1 calc R U . . .
C22 C 0.66178(14) 0.90636(13) 0.89066(11) 0.0175(4) Uani 1 1 d . . . . .
C23 C 0.78890(15) 0.95976(13) 0.92282(11) 0.0200(4) Uani 1 1 d . . . . .
H23A H 0.8007 0.9972 0.9781 0.024 Uiso 1 1 calc R U . . .
H23B H 0.8290 0.9108 0.9313 0.024 Uiso 1 1 calc R U . . .
C24 C 0.83319(14) 1.03082(13) 0.85418(11) 0.0176(4) Uani 1 1 d . . . . .
C25 C 0.58954(16) 0.90913(14) 0.95810(12) 0.0231(4) Uani 1 1 d . . . . .
H25A H 0.6054 0.9778 0.9788 0.035 Uiso 1 1 calc R U . . .
H25B H 0.6069 0.8705 1.0063 0.035 Uiso 1 1 calc R U . . .
H25C H 0.5102 0.8809 0.9323 0.035 Uiso 1 1 calc R U . . .
C26 C 0.63451(16) 0.79942(13) 0.85466(12) 0.0240(4) Uani 1 1 d . . . . .
H26A H 0.5547 0.7724 0.8302 0.036 Uiso 1 1 calc R U . . .
H26B H 0.6528 0.7589 0.9009 0.036 Uiso 1 1 calc R U . . .
H26C H 0.6788 0.7990 0.8100 0.036 Uiso 1 1 calc R U . . .
C27 C 0.89101(15) 0.98942(14) 0.79406(12) 0.0228(4) Uani 1 1 d . . . . .
H27A H 0.8429 0.9229 0.7716 0.034 Uiso 1 1 calc R U . . .
H27B H 0.9623 0.9861 0.8255 0.034 Uiso 1 1 calc R U . . .
H27C H 0.9050 1.0326 0.7464 0.034 Uiso 1 1 calc R U . . .
C28 C 0.91004(15) 1.13267(13) 0.89165(12) 0.0228(4) Uani 1 1 d . . . . .
H28A H 0.9829 1.1282 0.9183 0.034 Uiso 1 1 calc R U . . .
H28B H 0.8765 1.1564 0.9349 0.034 Uiso 1 1 calc R U . . .
H28C H 0.9201 1.1789 0.8458 0.034 Uiso 1 1 calc R U . . .
C29 C 0.71167(14) 1.10779(12) 0.73912(11) 0.0156(3) Uani 1 1 d . . . . .
C30 C 0.70398(14) 1.19785(13) 0.76854(11) 0.0171(4) Uani 1 1 d . . . . .
C31 C 0.69447(16) 1.26580(13) 0.70735(12) 0.0212(4) Uani 1 1 d . . . . .
H31 H 0.6911 1.3281 0.7249 0.025 Uiso 1 1 calc R U . . .
C32 C 0.68992(17) 1.24406(14) 0.62128(12) 0.0246(4) Uani 1 1 d . . . . .
H32 H 0.6851 1.2920 0.5807 0.029 Uiso 1 1 calc R U . . .
C33 C 0.69227(16) 1.15289(13) 0.59411(12) 0.0218(4) Uani 1 1 d . . . . .
H33 H 0.6869 1.1384 0.5347 0.026 Uiso 1 1 calc R U . . .
C34 C 0.70243(14) 1.08168(13) 0.65234(11) 0.0172(4) Uani 1 1 d . . . . .
C35 C 0.69604(15) 1.21931(13) 0.86083(11) 0.0188(4) Uani 1 1 d . . . . .
H35 H 0.7166 1.1682 0.8966 0.023 Uiso 1 1 calc R U . . .
C36 C 0.77610(17) 1.32124(14) 0.89690(12) 0.0246(4) Uani 1 1 d . . . . .
H36A H 0.8517 1.3281 0.8873 0.037 Uiso 1 1 calc R U . . .
H36B H 0.7767 1.3280 0.9585 0.037 Uiso 1 1 calc R U . . .
H36C H 0.7511 1.3728 0.8679 0.037 Uiso 1 1 calc R U . . .
C37 C 0.57508(16) 1.21099(15) 0.86665(12) 0.0265(4) Uani 1 1 d . . . . .
H37A H 0.5539 1.2617 0.8332 0.040 Uiso 1 1 calc R U . . .
H37B H 0.5693 1.2206 0.9267 0.040 Uiso 1 1 calc R U . . .
H37C H 0.5249 1.1453 0.8438 0.040 Uiso 1 1 calc R U . . .
C38 C 0.69473(15) 0.97957(13) 0.61889(11) 0.0182(4) Uani 1 1 d . . . . .
H38 H 0.7140 0.9422 0.6691 0.022 Uiso 1 1 calc R U . . .
C39 C 0.57562(16) 0.92229(14) 0.57358(13) 0.0255(4) Uani 1 1 d . . . . .
H39A H 0.5580 0.9534 0.5204 0.038 Uiso 1 1 calc R U . . .
H39B H 0.5225 0.9230 0.6112 0.038 Uiso 1 1 calc R U . . .
H39C H 0.5702 0.8538 0.5601 0.038 Uiso 1 1 calc R U . . .
C40 C 0.77703(16) 0.98492(14) 0.55816(12) 0.0245(4) Uani 1 1 d . . . . .
H40A H 0.7738 0.9179 0.5416 0.037 Uiso 1 1 calc R U . . .
H40B H 0.8530 1.0223 0.5871 0.037 Uiso 1 1 calc R U . . .
H40C H 0.7571 1.0181 0.5068 0.037 Uiso 1 1 calc R U . . .
C41 C -0.04243(19) 0.54257(17) 0.77860(15) 0.0354(5) Uani 1 1 d . . . . .
H41A H 0.0060 0.5526 0.7346 0.042 Uiso 1 1 calc R U . . .
H41B H -0.0964 0.4746 0.7700 0.042 Uiso 1 1 calc R U . . .
C42 C 0.02724(19) 0.55991(19) 0.86795(17) 0.0455(6) Uani 1 1 d . . . . .
H42A H 0.0357 0.4975 0.8900 0.055 Uiso 1 1 calc R U . . .
H42B H 0.1024 0.6087 0.8687 0.055 Uiso 1 1 calc R U . . .
C43 C -0.04002(19) 0.59936(18) 0.91958(14) 0.0399(6) Uani 1 1 d . . . . .
H43A H -0.1034 0.5454 0.9349 0.048 Uiso 1 1 calc R U . . .
H43B H 0.0072 0.6371 0.9725 0.048 Uiso 1 1 calc R U . . .
C44 C -0.08017(17) 0.66552(15) 0.85785(12) 0.0284(4) Uani 1 1 d . . . . .
H44A H -0.1498 0.6737 0.8708 0.034 Uiso 1 1 calc R U . . .
H44B H -0.0226 0.7315 0.8606 0.034 Uiso 1 1 calc R U . . .
C45 C 0.06880(17) 0.79675(13) 0.68567(12) 0.0238(4) Uani 1 1 d . . . . .
H45A H -0.0014 0.7555 0.7033 0.029 Uiso 1 1 calc R U . . .
H45B H 0.1292 0.7694 0.7081 0.029 Uiso 1 1 calc R U . . .
C46 C 0.05401(17) 0.79930(14) 0.58899(12) 0.0261(4) Uani 1 1 d . . . . .
H46A H -0.0010 0.7372 0.5606 0.031 Uiso 1 1 calc R U . . .
H46B H 0.1259 0.8110 0.5688 0.031 Uiso 1 1 calc R U . . .
C47 C 0.01076(15) 0.88636(14) 0.57319(12) 0.0215(4) Uani 1 1 d . . . . .
H47A H 0.0224 0.9130 0.5166 0.026 Uiso 1 1 calc R U . . .
H47B H -0.0697 0.8677 0.5767 0.026 Uiso 1 1 calc R U . . .
C48 C 0.08245(15) 0.95983(13) 0.64590(11) 0.0211(4) Uani 1 1 d . . . . .
H48A H 0.1553 0.9981 0.6305 0.025 Uiso 1 1 calc R U . . .
H48B H 0.0441 1.0063 0.6600 0.025 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Co1 O1 2.0487(14) . ?
Co1 Cl2 2.2388(7) . ?
Co1 Cl3 2.2423(5) . ?
Co1 Cl1 2.2592(7) . ?
Co2 O2 2.0463(13) . ?
Co2 Cl5 2.2450(5) . ?
Co2 Cl4 2.2480(7) . ?
Co2 Cl6 2.2603(6) . ?
O1 C41 1.451(2) . ?
O1 C44 1.460(2) . ?
O2 C48 1.455(2) . ?
O2 C45 1.460(2) . ?
N1 C1 1.275(2) . ?
N1 C9 1.466(2) . ?
N1 C4 1.541(2) . ?
N2 C21 1.278(2) . ?
N2 C29 1.462(2) . ?
N2 C24 1.541(2) . ?
C1 C2 1.486(2) . ?
C2 C5 1.533(3) . ?
C2 C6 1.540(3) . ?
C2 C3 1.551(3) . ?
C3 C4 1.545(2) . ?
C4 C7 1.521(2) . ?
C4 C8 1.524(3) . ?
C9 C14 1.402(2) . ?
C9 C10 1.404(2) . ?
C10 C11 1.399(2) . ?
C10 C15 1.520(2) . ?
C11 C12 1.382(3) . ?
C12 C13 1.387(3) . ?
C13 C14 1.396(2) . ?
C14 C18 1.517(2) . ?
C15 C16 1.527(3) . ?
C15 C17 1.532(3) . ?
C18 C20 1.530(3) . ?
C18 C19 1.530(3) . ?
C21 C22 1.479(2) . ?
C22 C25 1.535(2) . ?
C22 C26 1.541(2) . ?
C22 C23 1.556(2) . ?
C23 C24 1.543(2) . ?
C24 C27 1.524(3) . ?
C24 C28 1.525(2) . ?
C29 C34 1.400(2) . ?
C29 C30 1.407(2) . ?
C30 C31 1.393(3) . ?
C30 C35 1.521(2) . ?
C31 C32 1.386(3) . ?
C32 C33 1.383(3) . ?
C33 C34 1.398(3) . ?
C34 C38 1.520(2) . ?
C35 C36 1.532(3) . ?
C35 C37 1.535(3) . ?
C38 C40 1.528(3) . ?
C38 C39 1.532(3) . ?
C41 C42 1.516(3) . ?
C42 C43 1.509(4) . ?
C43 C44 1.505(3) . ?
C45 C46 1.514(3) . ?
C46 C47 1.522(3) . ?
C47 C48 1.516(3) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Co1 Cl2 103.14(4) . . ?
O1 Co1 Cl3 102.77(4) . . ?
Cl2 Co1 Cl3 113.52(2) . . ?
O1 Co1 Cl1 98.59(4) . . ?
Cl2 Co1 Cl1 117.61(3) . . ?
Cl3 Co1 Cl1 117.31(3) . . ?
O2 Co2 Cl5 100.01(4) . . ?
O2 Co2 Cl4 105.94(4) . . ?
Cl5 Co2 Cl4 115.46(2) . . ?
O2 Co2 Cl6 98.23(4) . . ?
Cl5 Co2 Cl6 119.17(3) . . ?
Cl4 Co2 Cl6 114.04(2) . . ?
C41 O1 C44 109.41(15) . . ?
C41 O1 Co1 122.21(13) . . ?
C44 O1 Co1 119.01(11) . . ?
C48 O2 C45 109.24(13) . . ?
C48 O2 Co2 117.21(10) . . ?
C45 O2 Co2 117.18(10) . . ?
C1 N1 C9 121.57(14) . . ?
C1 N1 C4 112.75(14) . . ?
C9 N1 C4 125.69(14) . . ?
C21 N2 C29 122.11(15) . . ?
C21 N2 C24 112.58(14) . . ?
C29 N2 C24 125.30(13) . . ?
N1 C1 C2 115.15(16) . . ?
C1 C2 C5 108.06(15) . . ?
C1 C2 C6 109.56(15) . . ?
C5 C2 C6 110.01(16) . . ?
C1 C2 C3 101.33(14) . . ?
C5 C2 C3 113.01(15) . . ?
C6 C2 C3 114.34(16) . . ?
C4 C3 C2 108.10(14) . . ?
C7 C4 C8 109.17(15) . . ?
C7 C4 N1 111.31(14) . . ?
C8 C4 N1 108.61(14) . . ?
C7 C4 C3 113.63(15) . . ?
C8 C4 C3 113.61(15) . . ?
N1 C4 C3 100.16(13) . . ?
C14 C9 C10 123.74(16) . . ?
C14 C9 N1 119.10(15) . . ?
C10 C9 N1 116.92(15) . . ?
C11 C10 C9 116.77(16) . . ?
C11 C10 C15 119.77(15) . . ?
C9 C10 C15 123.24(15) . . ?
C12 C11 C10 120.97(16) . . ?
C11 C12 C13 120.60(16) . . ?
C12 C13 C14 121.29(16) . . ?
C13 C14 C9 116.53(16) . . ?
C13 C14 C18 119.69(16) . . ?
C9 C14 C18 123.62(15) . . ?
C10 C15 C16 112.59(15) . . ?
C10 C15 C17 109.72(15) . . ?
C16 C15 C17 110.81(16) . . ?
C14 C18 C20 111.84(15) . . ?
C14 C18 C19 110.49(15) . . ?
C20 C18 C19 110.18(15) . . ?
N2 C21 C22 115.07(15) . . ?
C21 C22 C25 107.85(15) . . ?
C21 C22 C26 109.96(14) . . ?
C25 C22 C26 110.25(15) . . ?
C21 C22 C23 101.53(14) . . ?
C25 C22 C23 113.24(15) . . ?
C26 C22 C23 113.52(15) . . ?
C24 C23 C22 107.62(14) . . ?
C27 C24 C28 109.35(15) . . ?
C27 C24 N2 108.46(14) . . ?
C28 C24 N2 111.32(14) . . ?
C27 C24 C23 113.79(15) . . ?
C28 C24 C23 113.36(15) . . ?
N2 C24 C23 100.19(13) . . ?
C34 C29 C30 123.35(16) . . ?
C34 C29 N2 119.24(15) . . ?
C30 C29 N2 117.27(15) . . ?
C31 C30 C29 116.93(16) . . ?
C31 C30 C35 119.82(16) . . ?
C29 C30 C35 123.05(15) . . ?
C32 C31 C30 121.15(17) . . ?
C33 C32 C31 120.35(17) . . ?
C32 C33 C34 121.30(17) . . ?
C33 C34 C29 116.77(16) . . ?
C33 C34 C38 119.36(16) . . ?
C29 C34 C38 123.72(16) . . ?
C30 C35 C36 112.18(15) . . ?
C30 C35 C37 109.70(15) . . ?
C36 C35 C37 110.30(15) . . ?
C34 C38 C40 111.88(15) . . ?
C34 C38 C39 111.07(15) . . ?
C40 C38 C39 109.70(15) . . ?
O1 C41 C42 105.03(18) . . ?
C43 C42 C41 103.04(17) . . ?
C44 C43 C42 101.69(18) . . ?
O1 C44 C43 104.71(17) . . ?
O2 C45 C46 105.51(15) . . ?
C45 C46 C47 101.76(15) . . ?
C48 C47 C46 101.85(14) . . ?
O2 C48 C47 104.66(14) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 N1 C1 C2 -176.29(15) . . . . ?
C4 N1 C1 C2 3.8(2) . . . . ?
N1 C1 C2 C5 125.47(17) . . . . ?
N1 C1 C2 C6 -114.67(18) . . . . ?
N1 C1 C2 C3 6.5(2) . . . . ?
C1 C2 C3 C4 -13.93(19) . . . . ?
C5 C2 C3 C4 -129.31(16) . . . . ?
C6 C2 C3 C4 103.81(18) . . . . ?
C1 N1 C4 C7 -132.70(16) . . . . ?
C9 N1 C4 C7 47.4(2) . . . . ?
C1 N1 C4 C8 107.07(17) . . . . ?
C9 N1 C4 C8 -72.8(2) . . . . ?
C1 N1 C4 C3 -12.24(18) . . . . ?
C9 N1 C4 C3 167.89(15) . . . . ?
C2 C3 C4 C7 134.32(16) . . . . ?
C2 C3 C4 C8 -100.06(18) . . . . ?
C2 C3 C4 N1 15.55(18) . . . . ?
C1 N1 C9 C14 -83.8(2) . . . . ?
C4 N1 C9 C14 96.1(2) . . . . ?
C1 N1 C9 C10 90.8(2) . . . . ?
C4 N1 C9 C10 -89.4(2) . . . . ?
C14 C9 C10 C11 -4.0(3) . . . . ?
N1 C9 C10 C11 -178.24(15) . . . . ?
C14 C9 C10 C15 170.55(16) . . . . ?
N1 C9 C10 C15 -3.7(2) . . . . ?
C9 C10 C11 C12 2.1(3) . . . . ?
C15 C10 C11 C12 -172.58(16) . . . . ?
C10 C11 C12 C13 0.4(3) . . . . ?
C11 C12 C13 C14 -1.4(3) . . . . ?
C12 C13 C14 C9 -0.3(3) . . . . ?
C12 C13 C14 C18 175.42(16) . . . . ?
C10 C9 C14 C13 3.1(3) . . . . ?
N1 C9 C14 C13 177.21(15) . . . . ?
C10 C9 C14 C18 -172.47(16) . . . . ?
N1 C9 C14 C18 1.7(2) . . . . ?
C11 C10 C15 C16 -52.8(2) . . . . ?
C9 C10 C15 C16 132.84(18) . . . . ?
C11 C10 C15 C17 71.1(2) . . . . ?
C9 C10 C15 C17 -103.3(2) . . . . ?
C13 C14 C18 C20 56.6(2) . . . . ?
C9 C14 C18 C20 -128.05(18) . . . . ?
C13 C14 C18 C19 -66.6(2) . . . . ?
C9 C14 C18 C19 108.82(19) . . . . ?
C29 N2 C21 C22 -176.54(14) . . . . ?
C24 N2 C21 C22 4.6(2) . . . . ?
N2 C21 C22 C25 125.94(16) . . . . ?
N2 C21 C22 C26 -113.81(17) . . . . ?
N2 C21 C22 C23 6.7(2) . . . . ?
C21 C22 C23 C24 -15.03(18) . . . . ?
C25 C22 C23 C24 -130.38(16) . . . . ?
C26 C22 C23 C24 102.92(17) . . . . ?
C21 N2 C24 C27 105.76(17) . . . . ?
C29 N2 C24 C27 -73.0(2) . . . . ?
C21 N2 C24 C28 -133.89(16) . . . . ?
C29 N2 C24 C28 47.3(2) . . . . ?
C21 N2 C24 C23 -13.71(18) . . . . ?
C29 N2 C24 C23 167.51(15) . . . . ?
C22 C23 C24 C27 -98.53(17) . . . . ?
C22 C23 C24 C28 135.67(16) . . . . ?
C22 C23 C24 N2 16.99(17) . . . . ?
C21 N2 C29 C34 -83.6(2) . . . . ?
C24 N2 C29 C34 95.0(2) . . . . ?
C21 N2 C29 C30 92.2(2) . . . . ?
C24 N2 C29 C30 -89.1(2) . . . . ?
C34 C29 C30 C31 -4.6(3) . . . . ?
N2 C29 C30 C31 179.79(15) . . . . ?
C34 C29 C30 C35 170.25(16) . . . . ?
N2 C29 C30 C35 -5.4(2) . . . . ?
C29 C30 C31 C32 1.6(3) . . . . ?
C35 C30 C31 C32 -173.35(17) . . . . ?
C30 C31 C32 C33 1.4(3) . . . . ?
C31 C32 C33 C34 -1.8(3) . . . . ?
C32 C33 C34 C29 -0.9(3) . . . . ?
C32 C33 C34 C38 174.85(17) . . . . ?
C30 C29 C34 C33 4.2(3) . . . . ?
N2 C29 C34 C33 179.76(15) . . . . ?
C30 C29 C34 C38 -171.35(16) . . . . ?
N2 C29 C34 C38 4.2(3) . . . . ?
C31 C30 C35 C36 -52.0(2) . . . . ?
C29 C30 C35 C36 133.34(18) . . . . ?
C31 C30 C35 C37 71.0(2) . . . . ?
C29 C30 C35 C37 -103.7(2) . . . . ?
C33 C34 C38 C40 53.7(2) . . . . ?
C29 C34 C38 C40 -130.87(18) . . . . ?
C33 C34 C38 C39 -69.3(2) . . . . ?
C29 C34 C38 C39 106.2(2) . . . . ?
C44 O1 C41 C42 -6.9(2) . . . . ?
Co1 O1 C41 C42 -153.01(14) . . . . ?
O1 C41 C42 C43 29.1(2) . . . . ?
C41 C42 C43 C44 -39.5(2) . . . . ?
C41 O1 C44 C43 -18.2(2) . . . . ?
Co1 O1 C44 C43 129.14(14) . . . . ?
C42 C43 C44 O1 35.6(2) . . . . ?
C48 O2 C45 C46 9.79(19) . . . . ?
Co2 O2 C45 C46 -126.57(13) . . . . ?
O2 C45 C46 C47 -31.50(19) . . . . ?
C45 C46 C47 C48 40.64(18) . . . . ?
C45 O2 C48 C47 16.26(18) . . . . ?
Co2 O2 C48 C47 152.60(11) . . . . ?
C46 C47 C48 O2 -35.44(18) . . . . ?
 
_refine_diff_density_max    0.500
_refine_diff_density_min   -0.315
_refine_diff_density_rms    0.051

_shelxl_version_number 2013-4



 
data_sad_a
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          '2(C20 H32 N), Cl4 Co'
_chemical_formula_sum
 'C40 H64 Cl4 Co N2' 
_chemical_formula_weight          773.66

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            19
_space_group_name_H-M_alt         'P 21 21 21'
_space_group_name_Hall            'P 2ac 2ab'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 
_cell_length_a                    10.020(2)
_cell_length_b                    14.726(2)
_cell_length_c                    28.284(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      4173.4(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9816 
_cell_measurement_theta_min       2.156 
_cell_measurement_theta_max       25.5765 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             blue 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.231          
_exptl_crystal_F_000              1652
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.08 
_exptl_crystal_size_min           0.06  
_exptl_absorpt_coefficient_mu     0.696
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.6970  
_exptl_absorpt_correction_T_max   0.7453  
_exptl_absorpt_process_details    'SADABS-2012/1' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'rotating anode'                       
_diffrn_measurement_device_type   'Smart APEX II Ultra' 
_diffrn_measurement_method        'omega and phi scans'  
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             78210
_diffrn_reflns_av_unetI/netI      0.0331
_diffrn_reflns_av_R_equivalents   0.0509
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -33
_diffrn_reflns_limit_l_max        34
_diffrn_reflns_theta_min          1.440
_diffrn_reflns_theta_max          26.031
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.989
_diffrn_reflns_point_group_measured_fraction_full  0.993
_reflns_number_total              8149
_reflns_number_gt                 7401
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.770
_reflns_Friedel_fraction_max      0.977
_reflns_Friedel_fraction_full     0.984
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'APEX2 v2012.2'
_computing_cell_refinement        'SAINT V7.68A'
_computing_data_reduction         'SAINT V7.68A'
_computing_structure_solution     'SHELXS-2012 (Sheldrick, 2012)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     'XSHELL in SHELXTL-97'
_computing_publication_material   'XSHELL in SHELXTL-97'
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0301P)²+0.3269P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Flack x determined using 3019 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack    0.005(5)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          8149
_refine_ls_number_parameters      505
_refine_ls_number_restraints      244
_refine_ls_R_factor_all           0.0324
_refine_ls_R_factor_gt            0.0270
_refine_ls_wR_factor_ref          0.0594
_refine_ls_wR_factor_gt           0.0581
_refine_ls_goodness_of_fit_ref    1.030
_refine_ls_restrained_S_all       1.040
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Co1 Co 0.30473(14) 0.20216(5) 0.34685(3) 0.01826(16) Uani 0.926(5) 1 d D U P A 1
Cl1 Cl 0.1285(2) 0.13862(18) 0.30622(9) 0.0252(4) Uani 0.926(5) 1 d D U P A 1
Cl2 Cl 0.42303(13) 0.08267(11) 0.37543(6) 0.0336(3) Uani 0.926(5) 1 d D U P A 1
Cl3 Cl 0.2162(3) 0.28231(17) 0.40903(7) 0.0297(5) Uani 0.926(5) 1 d D U P A 1
Cl4 Cl 0.43165(19) 0.29723(7) 0.30334(6) 0.0429(4) Uani 0.926(5) 1 d D U P A 1
Co1' Co 0.2689(12) 0.2020(7) 0.3424(4) 0.01826(16) Uani 0.074(5) 1 d D . P A 2
Cl1' Cl 0.099(3) 0.124(2) 0.3091(12) 0.028(5) Uani 0.074(5) 1 d D U P A 2
Cl2' Cl 0.4319(19) 0.1081(13) 0.3742(9) 0.0336(3) Uani 0.074(5) 1 d D U P A 2
Cl3' Cl 0.195(4) 0.290(2) 0.4042(10) 0.041(6) Uani 0.074(5) 1 d D U P A 2
Cl4' Cl 0.358(3) 0.2978(9) 0.2880(6) 0.048(4) Uani 0.074(5) 1 d D U P A 2
N1 N 0.35197(19) 0.44378(14) 0.52831(7) 0.0157(4) Uani 1 1 d D . . . .
N2 N 0.17440(19) 0.75741(13) 0.28732(7) 0.0152(4) Uani 1 1 d . . . . .
C4 C 0.4239(3) 0.43455(17) 0.57630(9) 0.0199(6) Uani 1 1 d D U . . .
C3 C 0.3761(11) 0.3389(4) 0.5917(2) 0.0223(12) Uani 0.72(3) 1 d D U P B 1
H3A H 0.4528 0.3024 0.6029 0.027 Uiso 0.72(3) 1 calc R U P B 1
H3B H 0.3106 0.3440 0.6178 0.027 Uiso 0.72(3) 1 calc R U P B 1
C3' C 0.414(2) 0.3308(9) 0.5841(7) 0.022(2) Uani 0.28(3) 1 d D U P B 2
H3'A H 0.5024 0.3021 0.5788 0.027 Uiso 0.28(3) 1 calc R U P B 2
H3'B H 0.3856 0.3176 0.6169 0.027 Uiso 0.28(3) 1 calc R U P B 2
C1 C 0.2990(2) 0.36968(17) 0.51467(9) 0.0196(5) Uani 1 1 d D . . . .
H1 H 0.2549 0.3637 0.4851 0.023 Uiso 1 1 calc R U . . .
C2 C 0.3117(3) 0.29357(18) 0.54867(9) 0.0243(5) Uani 1 1 d D U . . .
C5 C 0.1717(7) 0.2559(6) 0.5582(4) 0.0418(18) Uani 0.71(2) 1 d D U P B 1
H5A H 0.1762 0.2103 0.5834 0.063 Uiso 0.71(2) 1 calc R U P B 1
H5B H 0.1368 0.2278 0.5293 0.063 Uiso 0.71(2) 1 calc R U P B 1
H5C H 0.1126 0.3055 0.5680 0.063 Uiso 0.71(2) 1 calc R U P B 1
C6 C 0.3987(10) 0.2180(6) 0.5270(3) 0.0401(19) Uani 0.71(2) 1 d D U P B 1
H6A H 0.4904 0.2401 0.5234 0.060 Uiso 0.71(2) 1 calc R U P B 1
H6B H 0.3630 0.2010 0.4960 0.060 Uiso 0.71(2) 1 calc R U P B 1
H6C H 0.3981 0.1649 0.5479 0.060 Uiso 0.71(2) 1 calc R U P B 1
C5' C 0.1733(14) 0.2814(14) 0.5748(8) 0.036(3) Uani 0.29(2) 1 d D U P B 2
H5'A H 0.1810 0.2334 0.5986 0.053 Uiso 0.29(2) 1 calc R U P B 2
H5'B H 0.1046 0.2648 0.5517 0.053 Uiso 0.29(2) 1 calc R U P B 2
H5'C H 0.1485 0.3386 0.5902 0.053 Uiso 0.29(2) 1 calc R U P B 2
C6' C 0.350(2) 0.2047(11) 0.5251(8) 0.035(3) Uani 0.29(2) 1 d D U P B 2
H6'A H 0.4287 0.2141 0.5052 0.052 Uiso 0.29(2) 1 calc R U P B 2
H6'B H 0.2755 0.1833 0.5056 0.052 Uiso 0.29(2) 1 calc R U P B 2
H6'C H 0.3700 0.1593 0.5494 0.052 Uiso 0.29(2) 1 calc R U P B 2
C7 C 0.5724(3) 0.4484(2) 0.56885(10) 0.0267(6) Uani 1 1 d . . . . .
H7A H 0.6186 0.4444 0.5993 0.040 Uiso 1 1 calc R U . . .
H7B H 0.5879 0.5084 0.5549 0.040 Uiso 1 1 calc R U . . .
H7C H 0.6066 0.4014 0.5475 0.040 Uiso 1 1 calc R U . . .
C8 C 0.3722(3) 0.5030(2) 0.61131(9) 0.0273(6) Uani 1 1 d . . . . .
H8A H 0.2767 0.4926 0.6166 0.041 Uiso 1 1 calc R U . . .
H8B H 0.3857 0.5644 0.5988 0.041 Uiso 1 1 calc R U . . .
H8C H 0.4204 0.4964 0.6413 0.041 Uiso 1 1 calc R U . . .
C9 C 0.3388(2) 0.52951(17) 0.50276(8) 0.0159(5) Uani 1 1 d . . . . .
C10 C 0.4352(2) 0.55421(17) 0.46919(9) 0.0187(5) Uani 1 1 d . . . . .
C11 C 0.4198(3) 0.63814(18) 0.44729(9) 0.0241(6) Uani 1 1 d . . . . .
H11 H 0.4836 0.6572 0.4245 0.029 Uiso 1 1 calc R U . . .
C12 C 0.3133(3) 0.69450(19) 0.45795(9) 0.0261(6) Uani 1 1 d . . . . .
H12 H 0.3063 0.7525 0.4434 0.031 Uiso 1 1 calc R U . . .
C13 C 0.2175(2) 0.66634(17) 0.48969(9) 0.0215(6) Uani 1 1 d . . . . .
H13 H 0.1438 0.7049 0.4963 0.026 Uiso 1 1 calc R U . . .
C14 C 0.2265(2) 0.58235(17) 0.51233(8) 0.0169(5) Uani 1 1 d . . . . .
C15 C 0.5474(2) 0.49226(19) 0.45261(9) 0.0232(6) Uani 1 1 d . . . . .
H15 H 0.5501 0.4382 0.4740 0.028 Uiso 1 1 calc R U . . .
C16 C 0.5198(3) 0.4590(2) 0.40252(9) 0.0297(7) Uani 1 1 d . . . . .
H16A H 0.5935 0.4201 0.3920 0.045 Uiso 1 1 calc R U . . .
H16B H 0.5119 0.5112 0.3812 0.045 Uiso 1 1 calc R U . . .
H16C H 0.4365 0.4242 0.4021 0.045 Uiso 1 1 calc R U . . .
C17 C 0.6833(3) 0.5400(2) 0.45515(11) 0.0337(7) Uani 1 1 d . . . . .
H17A H 0.6967 0.5644 0.4870 0.051 Uiso 1 1 calc R U . . .
H17B H 0.6857 0.5897 0.4321 0.051 Uiso 1 1 calc R U . . .
H17C H 0.7542 0.4963 0.4479 0.051 Uiso 1 1 calc R U . . .
C18 C 0.1095(2) 0.54968(17) 0.54217(9) 0.0185(5) Uani 1 1 d . . . . .
H18 H 0.1387 0.4942 0.5597 0.022 Uiso 1 1 calc R U . . .
C19 C -0.0047(3) 0.5226(2) 0.50928(10) 0.0306(7) Uani 1 1 d . . . . .
H19A H -0.0787 0.4981 0.5280 0.046 Uiso 1 1 calc R U . . .
H19B H 0.0266 0.4762 0.4870 0.046 Uiso 1 1 calc R U . . .
H19C H -0.0352 0.5760 0.4917 0.046 Uiso 1 1 calc R U . . .
C20 C 0.0626(3) 0.61925(19) 0.57819(10) 0.0304(7) Uani 1 1 d . . . . .
H20A H -0.0108 0.5937 0.5968 0.046 Uiso 1 1 calc R U . . .
H20B H 0.0316 0.6739 0.5617 0.046 Uiso 1 1 calc R U . . .
H20C H 0.1367 0.6351 0.5992 0.046 Uiso 1 1 calc R U . . .
C21 C 0.1051(2) 0.77382(17) 0.25025(8) 0.0183(5) Uani 1 1 d . . . . .
H21 H 0.0475 0.7302 0.2363 0.022 Uiso 1 1 calc R U . . .
C22 C 0.1224(3) 0.86702(17) 0.23097(9) 0.0209(6) Uani 1 1 d . . . . .
C23 C 0.2442(3) 0.90095(18) 0.25908(9) 0.0221(6) Uani 1 1 d . . . . .
H23A H 0.3256 0.8977 0.2393 0.026 Uiso 1 1 calc R U . . .
H23B H 0.2307 0.9648 0.2689 0.026 Uiso 1 1 calc R U . . .
C24 C 0.2589(2) 0.83968(16) 0.30269(9) 0.0178(5) Uani 1 1 d . . . . .
C25 C 0.1472(3) 0.8642(2) 0.17747(9) 0.0320(7) Uani 1 1 d . . . . .
H25A H 0.0697 0.8372 0.1616 0.048 Uiso 1 1 calc R U . . .
H25B H 0.2267 0.8275 0.1709 0.048 Uiso 1 1 calc R U . . .
H25C H 0.1610 0.9260 0.1657 0.048 Uiso 1 1 calc R U . . .
C26 C -0.0077(3) 0.9195(2) 0.24143(10) 0.0298(7) Uani 1 1 d . . . . .
H26A H 0.0011 0.9822 0.2302 0.045 Uiso 1 1 calc R U . . .
H26B H -0.0244 0.9195 0.2756 0.045 Uiso 1 1 calc R U . . .
H26C H -0.0824 0.8900 0.2251 0.045 Uiso 1 1 calc R U . . .
C27 C 0.1981(2) 0.87992(17) 0.34731(9) 0.0221(5) Uani 1 1 d . . . . .
H27A H 0.2525 0.9313 0.3580 0.033 Uiso 1 1 calc R U . . .
H27B H 0.1953 0.8335 0.3721 0.033 Uiso 1 1 calc R U . . .
H27C H 0.1072 0.9009 0.3406 0.033 Uiso 1 1 calc R U . . .
C28 C 0.4029(2) 0.81200(19) 0.31234(9) 0.0239(6) Uani 1 1 d . . . . .
H28A H 0.4413 0.7848 0.2838 0.036 Uiso 1 1 calc R U . . .
H28B H 0.4051 0.7677 0.3382 0.036 Uiso 1 1 calc R U . . .
H28C H 0.4549 0.8657 0.3213 0.036 Uiso 1 1 calc R U . . .
C29 C 0.1687(2) 0.67180(16) 0.31316(8) 0.0159(5) Uani 1 1 d . . . . .
C30 C 0.0675(2) 0.65855(16) 0.34668(9) 0.0177(5) Uani 1 1 d . . . . .
C31 C 0.0702(3) 0.57732(17) 0.37158(9) 0.0211(6) Uani 1 1 d . . . . .
H31 H 0.0042 0.5665 0.3950 0.025 Uiso 1 1 calc R U . . .
C32 C 0.1656(3) 0.51208(18) 0.36326(9) 0.0229(6) Uani 1 1 d . . . . .
H32 H 0.1672 0.4582 0.3818 0.027 Uiso 1 1 calc R U . . .
C33 C 0.2591(3) 0.52498(18) 0.32796(9) 0.0214(6) Uani 1 1 d . . . . .
H33 H 0.3218 0.4782 0.3214 0.026 Uiso 1 1 calc R U . . .
C34 C 0.2634(2) 0.60493(17) 0.30185(9) 0.0179(5) Uani 1 1 d . . . . .
C35 C -0.0495(2) 0.72342(17) 0.35406(9) 0.0206(6) Uani 1 1 d . . . . .
H35 H -0.0283 0.7819 0.3377 0.025 Uiso 1 1 calc R U . . .
C36 C -0.0727(3) 0.74380(19) 0.40661(9) 0.0254(6) Uani 1 1 d . . . . .
H36A H -0.1490 0.7849 0.4100 0.038 Uiso 1 1 calc R U . . .
H36B H 0.0071 0.7725 0.4199 0.038 Uiso 1 1 calc R U . . .
H36C H -0.0911 0.6870 0.4235 0.038 Uiso 1 1 calc R U . . .
C37 C -0.1760(3) 0.6837(2) 0.33150(10) 0.0305(7) Uani 1 1 d . . . . .
H37A H -0.1607 0.6737 0.2977 0.046 Uiso 1 1 calc R U . . .
H37B H -0.2504 0.7262 0.3357 0.046 Uiso 1 1 calc R U . . .
H37C H -0.1978 0.6257 0.3467 0.046 Uiso 1 1 calc R U . . .
C38 C 0.3577(2) 0.61161(18) 0.25995(9) 0.0203(6) Uani 1 1 d . . . . .
H38 H 0.3587 0.6762 0.2490 0.024 Uiso 1 1 calc R U . . .
C39 C 0.3049(3) 0.5530(2) 0.21957(10) 0.0364(7) Uani 1 1 d . . . . .
H39A H 0.2153 0.5735 0.2107 0.055 Uiso 1 1 calc R U . . .
H39B H 0.3010 0.4894 0.2298 0.055 Uiso 1 1 calc R U . . .
H39C H 0.3646 0.5583 0.1922 0.055 Uiso 1 1 calc R U . . .
C40 C 0.5009(3) 0.5847(2) 0.27249(10) 0.0300(7) Uani 1 1 d . . . . .
H40A H 0.5588 0.5943 0.2450 0.045 Uiso 1 1 calc R U . . .
H40B H 0.5032 0.5204 0.2815 0.045 Uiso 1 1 calc R U . . .
H40C H 0.5324 0.6219 0.2989 0.045 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Co1 Cl4 2.2564(11) . ?
Co1 Cl2 2.2703(11) . ?
Co1 Cl3 2.2965(14) . ?
Co1 Cl1 2.3055(17) . ?
Co1' Cl1' 2.263(16) . ?
Co1' Cl4' 2.271(13) . ?
Co1' Cl3' 2.295(17) . ?
Co1' Cl2' 2.321(15) . ?
N1 C1 1.273(3) . ?
N1 C9 1.461(3) . ?
N1 C4 1.543(3) . ?
N2 C21 1.281(3) . ?
N2 C29 1.458(3) . ?
N2 C24 1.541(3) . ?
C4 C8 1.505(4) . ?
C4 C7 1.516(4) . ?
C4 C3' 1.546(13) . ?
C4 C3 1.550(5) . ?
C3 C2 1.531(5) . ?
C3' C2 1.537(12) . ?
C1 C2 1.482(4) . ?
C2 C6' 1.517(14) . ?
C2 C5 1.532(6) . ?
C2 C6 1.540(7) . ?
C2 C5' 1.582(12) . ?
C9 C14 1.395(3) . ?
C9 C10 1.402(3) . ?
C10 C11 1.391(4) . ?
C10 C15 1.521(3) . ?
C11 C12 1.385(4) . ?
C12 C13 1.378(4) . ?
C13 C14 1.396(3) . ?
C14 C18 1.522(3) . ?
C15 C16 1.524(4) . ?
C15 C17 1.534(4) . ?
C18 C20 1.519(4) . ?
C18 C19 1.528(3) . ?
C21 C22 1.487(4) . ?
C22 C25 1.534(4) . ?
C22 C23 1.540(4) . ?
C22 C26 1.544(4) . ?
C23 C24 1.535(4) . ?
C24 C27 1.522(3) . ?
C24 C28 1.523(3) . ?
C29 C30 1.402(3) . ?
C29 C34 1.404(3) . ?
C30 C31 1.388(3) . ?
C30 C35 1.526(3) . ?
C31 C32 1.376(4) . ?
C32 C33 1.382(4) . ?
C33 C34 1.390(4) . ?
C34 C38 1.519(3) . ?
C35 C36 1.534(4) . ?
C35 C37 1.535(4) . ?
C38 C39 1.527(4) . ?
C38 C40 1.530(3) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
Cl4 Co1 Cl2 112.38(6) . . ?
Cl4 Co1 Cl3 108.45(8) . . ?
Cl2 Co1 Cl3 109.12(8) . . ?
Cl4 Co1 Cl1 114.31(7) . . ?
Cl2 Co1 Cl1 105.24(8) . . ?
Cl3 Co1 Cl1 107.11(10) . . ?
Cl1' Co1' Cl4' 109.1(10) . . ?
Cl1' Co1' Cl3' 111.1(13) . . ?
Cl4' Co1' Cl3' 107.0(11) . . ?
Cl1' Co1' Cl2' 113.0(10) . . ?
Cl4' Co1' Cl2' 110.9(7) . . ?
Cl3' Co1' Cl2' 105.5(11) . . ?
C1 N1 C9 123.6(2) . . ?
C1 N1 C4 112.7(2) . . ?
C9 N1 C4 123.62(19) . . ?
C21 N2 C29 123.5(2) . . ?
C21 N2 C24 112.4(2) . . ?
C29 N2 C24 124.02(18) . . ?
C8 C4 C7 109.8(2) . . ?
C8 C4 N1 111.0(2) . . ?
C7 C4 N1 108.9(2) . . ?
C8 C4 C3' 123.1(10) . . ?
C7 C4 C3' 102.3(9) . . ?
N1 C4 C3' 100.6(5) . . ?
C8 C4 C3 108.5(4) . . ?
C7 C4 C3 117.7(5) . . ?
N1 C4 C3 100.6(2) . . ?
C2 C3 C4 107.6(3) . . ?
C2 C3' C4 107.5(7) . . ?
N1 C1 C2 114.5(2) . . ?
C1 C2 C6' 112.9(9) . . ?
C1 C2 C3 102.8(3) . . ?
C1 C2 C5 108.0(3) . . ?
C3 C2 C5 113.8(6) . . ?
C1 C2 C3' 102.1(5) . . ?
C6' C2 C3' 115.2(12) . . ?
C1 C2 C6 109.7(4) . . ?
C3 C2 C6 113.1(6) . . ?
C5 C2 C6 109.1(4) . . ?
C1 C2 C5' 108.2(6) . . ?
C6' C2 C5' 109.2(9) . . ?
C3' C2 C5' 108.8(14) . . ?
C14 C9 C10 122.9(2) . . ?
C14 C9 N1 117.3(2) . . ?
C10 C9 N1 119.8(2) . . ?
C11 C10 C9 117.1(2) . . ?
C11 C10 C15 118.5(2) . . ?
C9 C10 C15 124.2(2) . . ?
C12 C11 C10 121.4(2) . . ?
C13 C12 C11 119.9(2) . . ?
C12 C13 C14 121.4(2) . . ?
C9 C14 C13 117.2(2) . . ?
C9 C14 C18 123.5(2) . . ?
C13 C14 C18 119.0(2) . . ?
C10 C15 C16 110.2(2) . . ?
C10 C15 C17 111.5(2) . . ?
C16 C15 C17 110.6(2) . . ?
C20 C18 C14 113.4(2) . . ?
C20 C18 C19 110.6(2) . . ?
C14 C18 C19 108.8(2) . . ?
N2 C21 C22 114.3(2) . . ?
C21 C22 C25 110.8(2) . . ?
C21 C22 C23 101.7(2) . . ?
C25 C22 C23 112.9(2) . . ?
C21 C22 C26 107.0(2) . . ?
C25 C22 C26 109.8(2) . . ?
C23 C22 C26 114.1(2) . . ?
C24 C23 C22 107.5(2) . . ?
C27 C24 C28 109.6(2) . . ?
C27 C24 C23 113.5(2) . . ?
C28 C24 C23 113.1(2) . . ?
C27 C24 N2 108.65(18) . . ?
C28 C24 N2 111.1(2) . . ?
C23 C24 N2 100.50(18) . . ?
C30 C29 C34 123.1(2) . . ?
C30 C29 N2 119.2(2) . . ?
C34 C29 N2 117.8(2) . . ?
C31 C30 C29 116.7(2) . . ?
C31 C30 C35 119.0(2) . . ?
C29 C30 C35 124.1(2) . . ?
C32 C31 C30 121.9(2) . . ?
C31 C32 C33 119.9(2) . . ?
C32 C33 C34 121.4(2) . . ?
C33 C34 C29 116.9(2) . . ?
C33 C34 C38 119.2(2) . . ?
C29 C34 C38 123.5(2) . . ?
C30 C35 C36 111.8(2) . . ?
C30 C35 C37 109.8(2) . . ?
C36 C35 C37 110.6(2) . . ?
C34 C38 C39 109.4(2) . . ?
C34 C38 C40 112.7(2) . . ?
C39 C38 C40 110.6(2) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C1 N1 C4 C8 -124.8(2) . . . . ?
C9 N1 C4 C8 51.6(3) . . . . ?
C1 N1 C4 C7 114.2(2) . . . . ?
C9 N1 C4 C7 -69.5(3) . . . . ?
C1 N1 C4 C3' 7.1(11) . . . . ?
C9 N1 C4 C3' -176.5(11) . . . . ?
C1 N1 C4 C3 -10.1(5) . . . . ?
C9 N1 C4 C3 166.3(5) . . . . ?
C8 C4 C3 C2 129.4(6) . . . . ?
C7 C4 C3 C2 -105.2(6) . . . . ?
N1 C4 C3 C2 12.8(7) . . . . ?
C3' C4 C3 C2 -78.8(18) . . . . ?
C8 C4 C3' C2 110.0(12) . . . . ?
C7 C4 C3' C2 -126.2(13) . . . . ?
N1 C4 C3' C2 -13.9(16) . . . . ?
C3 C4 C3' C2 77.6(19) . . . . ?
C9 N1 C1 C2 -173.2(2) . . . . ?
C4 N1 C1 C2 3.1(3) . . . . ?
N1 C1 C2 C6' -136.2(10) . . . . ?
N1 C1 C2 C3 5.5(5) . . . . ?
N1 C1 C2 C5 126.1(5) . . . . ?
N1 C1 C2 C3' -12.0(11) . . . . ?
N1 C1 C2 C6 -115.1(5) . . . . ?
N1 C1 C2 C5' 102.8(11) . . . . ?
C4 C3 C2 C1 -11.6(7) . . . . ?
C4 C3 C2 C6' 121.8(12) . . . . ?
C4 C3 C2 C5 -128.1(6) . . . . ?
C4 C3 C2 C3' 78.0(19) . . . . ?
C4 C3 C2 C6 106.6(7) . . . . ?
C4 C3 C2 C5' -121.0(9) . . . . ?
C4 C3' C2 C1 15.7(17) . . . . ?
C4 C3' C2 C6' 138.4(15) . . . . ?
C4 C3' C2 C3 -79(2) . . . . ?
C4 C3' C2 C5 -109.7(12) . . . . ?
C4 C3' C2 C6 127.9(14) . . . . ?
C4 C3' C2 C5' -98.6(15) . . . . ?
C1 N1 C9 C14 85.9(3) . . . . ?
C4 N1 C9 C14 -90.1(3) . . . . ?
C1 N1 C9 C10 -92.3(3) . . . . ?
C4 N1 C9 C10 91.7(3) . . . . ?
C14 C9 C10 C11 4.2(4) . . . . ?
N1 C9 C10 C11 -177.7(2) . . . . ?
C14 C9 C10 C15 -170.5(2) . . . . ?
N1 C9 C10 C15 7.6(4) . . . . ?
C9 C10 C11 C12 -0.4(4) . . . . ?
C15 C10 C11 C12 174.6(2) . . . . ?
C10 C11 C12 C13 -2.2(4) . . . . ?
C11 C12 C13 C14 1.3(4) . . . . ?
C10 C9 C14 C13 -5.0(4) . . . . ?
N1 C9 C14 C13 176.8(2) . . . . ?
C10 C9 C14 C18 169.2(2) . . . . ?
N1 C9 C14 C18 -8.9(3) . . . . ?
C12 C13 C14 C9 2.2(4) . . . . ?
C12 C13 C14 C18 -172.3(2) . . . . ?
C11 C10 C15 C16 -67.6(3) . . . . ?
C9 C10 C15 C16 107.0(3) . . . . ?
C11 C10 C15 C17 55.6(3) . . . . ?
C9 C10 C15 C17 -129.8(3) . . . . ?
C9 C14 C18 C20 134.6(3) . . . . ?
C13 C14 C18 C20 -51.3(3) . . . . ?
C9 C14 C18 C19 -101.9(3) . . . . ?
C13 C14 C18 C19 72.3(3) . . . . ?
C29 N2 C21 C22 177.4(2) . . . . ?
C24 N2 C21 C22 0.1(3) . . . . ?
N2 C21 C22 C25 131.8(2) . . . . ?
N2 C21 C22 C23 11.5(3) . . . . ?
N2 C21 C22 C26 -108.4(2) . . . . ?
C21 C22 C23 C24 -18.3(2) . . . . ?
C25 C22 C23 C24 -137.1(2) . . . . ?
C26 C22 C23 C24 96.5(3) . . . . ?
C22 C23 C24 C27 -97.7(2) . . . . ?
C22 C23 C24 C28 136.7(2) . . . . ?
C22 C23 C24 N2 18.1(2) . . . . ?
C21 N2 C24 C27 107.7(2) . . . . ?
C29 N2 C24 C27 -69.6(3) . . . . ?
C21 N2 C24 C28 -131.7(2) . . . . ?
C29 N2 C24 C28 51.0(3) . . . . ?
C21 N2 C24 C23 -11.7(2) . . . . ?
C29 N2 C24 C23 171.0(2) . . . . ?
C21 N2 C29 C30 -83.5(3) . . . . ?
C24 N2 C29 C30 93.5(3) . . . . ?
C21 N2 C29 C34 94.3(3) . . . . ?
C24 N2 C29 C34 -88.7(3) . . . . ?
C34 C29 C30 C31 4.9(3) . . . . ?
N2 C29 C30 C31 -177.4(2) . . . . ?
C34 C29 C30 C35 -169.8(2) . . . . ?
N2 C29 C30 C35 7.9(3) . . . . ?
C29 C30 C31 C32 -1.3(4) . . . . ?
C35 C30 C31 C32 173.6(2) . . . . ?
C30 C31 C32 C33 -2.6(4) . . . . ?
C31 C32 C33 C34 3.2(4) . . . . ?
C32 C33 C34 C29 0.2(4) . . . . ?
C32 C33 C34 C38 -173.2(2) . . . . ?
C30 C29 C34 C33 -4.3(4) . . . . ?
N2 C29 C34 C33 177.9(2) . . . . ?
C30 C29 C34 C38 168.8(2) . . . . ?
N2 C29 C34 C38 -8.9(3) . . . . ?
C31 C30 C35 C36 52.0(3) . . . . ?
C29 C30 C35 C36 -133.5(2) . . . . ?
C31 C30 C35 C37 -71.2(3) . . . . ?
C29 C30 C35 C37 103.3(3) . . . . ?
C33 C34 C38 C39 72.0(3) . . . . ?
C29 C34 C38 C39 -101.0(3) . . . . ?
C33 C34 C38 C40 -51.4(3) . . . . ?
C29 C34 C38 C40 135.6(3) . . . . ?
 
_refine_diff_density_max    0.247
_refine_diff_density_min   -0.241
_refine_diff_density_rms    0.037

_shelxl_version_number 2013-4



 
data_pna21_a
 
_audit_creation_method            SHELXL-2012
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          '(C40 H62 Co2 N2)(c7 H8)'
_chemical_formula_sum
 'C47 H70 Co2 N2' 
_chemical_formula_weight          780.91

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            33
_space_group_name_H-M_alt         'P n a 21'
_space_group_name_Hall            'P 2c -2n'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z+1/2'
 
_cell_length_a                    22.773(2)
_cell_length_b                    10.794(2)
_cell_length_c                    16.689(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      4102.4(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9957 
_cell_measurement_theta_min       2.266 
_cell_measurement_theta_max       27.391 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.264          
_exptl_crystal_F_000              1680
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.05 
_exptl_crystal_size_mid           0.01
_exptl_crystal_size_min           0.01
_exptl_absorpt_coefficient_mu     0.843
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.3839  
_exptl_absorpt_correction_T_max   0.4305  
_exptl_absorpt_process_details    'SADABS-2012/1' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'rotating anode'                       
_diffrn_measurement_device_type   'Smart APEX II Ultra'
_diffrn_measurement_method        'omega scans'  
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             117899
_diffrn_reflns_av_unetI/netI      0.0293
_diffrn_reflns_av_R_equivalents   0.0614
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        29
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          1.788
_diffrn_reflns_theta_max          27.497
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              9411
_reflns_number_gt                 8853
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.931
_reflns_Friedel_fraction_max      0.997
_reflns_Friedel_fraction_full     1.000
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'APEX2 v2011.2'
_computing_cell_refinement        'SAINT V7.68A'
_computing_data_reduction         'SAINT V7.68A' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics      'shelXle v0.477'
_computing_publication_material   ?
 
 _refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0250P)²+0.4409P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Flack x determined using 4024 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack    0.001(4)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          9411
_refine_ls_number_parameters      542
_refine_ls_number_restraints      352
_refine_ls_R_factor_all           0.0273
_refine_ls_R_factor_gt            0.0249
_refine_ls_wR_factor_ref          0.0560
_refine_ls_wR_factor_gt           0.0551
_refine_ls_goodness_of_fit_ref    1.080
_refine_ls_restrained_S_all       1.064
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Co1 Co 0.33604(2) 0.81732(3) 0.46928(2) 0.01382(7) Uani 1 1 d . . . . .
Co2 Co 0.34448(2) 1.05667(3) 0.50409(2) 0.01355(7) Uani 1 1 d . . . . .
N1 N 0.41305(8) 0.86284(17) 0.60254(11) 0.0146(4) Uani 1 1 d . . . . .
N2 N 0.23579(8) 0.99796(18) 0.42652(12) 0.0154(4) Uani 1 1 d . . . . .
C1 C 0.39274(10) 0.7821(2) 0.54568(14) 0.0152(5) Uani 1 1 d . . . . .
C2 C 0.42388(11) 0.6574(2) 0.56451(16) 0.0198(5) Uani 1 1 d . . . . .
C3 C 0.47179(11) 0.6917(2) 0.62619(16) 0.0200(5) Uani 1 1 d . . . . .
H3A H 0.4763 0.6246 0.6662 0.024 Uiso 1 1 calc R U . . .
H3B H 0.5099 0.7044 0.5990 0.024 Uiso 1 1 calc R U . . .
C4 C 0.45197(10) 0.8109(2) 0.66700(15) 0.0167(5) Uani 1 1 d . . . . .
C5 C 0.45385(12) 0.6042(3) 0.48999(16) 0.0315(7) Uani 1 1 d . . . . .
H5A H 0.4792 0.6675 0.4660 0.047 Uiso 1 1 calc R U . . .
H5B H 0.4240 0.5788 0.4511 0.047 Uiso 1 1 calc R U . . .
H5C H 0.4776 0.5323 0.5052 0.047 Uiso 1 1 calc R U . . .
C6 C 0.38065(13) 0.5609(2) 0.59891(18) 0.0274(6) Uani 1 1 d . . . . .
H6A H 0.3540 0.5329 0.5564 0.041 Uiso 1 1 calc R U . . .
H6B H 0.3578 0.5986 0.6423 0.041 Uiso 1 1 calc R U . . .
H6C H 0.4027 0.4900 0.6198 0.041 Uiso 1 1 calc R U . . .
C7 C 0.41773(11) 0.7821(2) 0.74394(15) 0.0216(5) Uani 1 1 d . . . . .
H7A H 0.3819 0.7364 0.7305 0.032 Uiso 1 1 calc R U . . .
H7B H 0.4073 0.8598 0.7708 0.032 Uiso 1 1 calc R U . . .
H7C H 0.4422 0.7318 0.7797 0.032 Uiso 1 1 calc R U . . .
C8 C 0.50241(11) 0.8972(2) 0.68780(16) 0.0230(5) Uani 1 1 d . . . . .
H8A H 0.5270 0.9099 0.6403 0.035 Uiso 1 1 calc R U . . .
H8B H 0.5260 0.8604 0.7307 0.035 Uiso 1 1 calc R U . . .
H8C H 0.4867 0.9770 0.7058 0.035 Uiso 1 1 calc R U . . .
C9 C 0.40525(10) 0.9926(2) 0.58695(14) 0.0156(5) Uani 1 1 d . . . . .
C10 C 0.43939(10) 1.0437(2) 0.52232(14) 0.0178(5) Uani 1 1 d . . . . .
C11 C 0.42495(10) 1.1632(2) 0.49503(16) 0.0207(5) Uani 1 1 d . . . . .
H11 H 0.4443 1.1963 0.4494 0.025 Uiso 1 1 calc R U . . .
C12 C 0.38232(11) 1.2338(2) 0.53456(15) 0.0212(5) Uani 1 1 d . . . . .
H12 H 0.3742 1.3156 0.5168 0.025 Uiso 1 1 calc R U . . .
C13 C 0.35164(11) 1.1852(2) 0.59984(15) 0.0198(5) Uani 1 1 d . . . . .
H13 H 0.3237 1.2358 0.6266 0.024 Uiso 1 1 calc R U . . .
C14 C 0.36111(11) 1.0627(2) 0.62726(15) 0.0175(5) Uani 1 1 d . . . . .
C15 C 0.49275(10) 0.9784(2) 0.48672(15) 0.0227(6) Uani 1 1 d . . . . .
H15 H 0.4984 0.8991 0.5168 0.027 Uiso 1 1 calc R U . . .
C16 C 0.54791(11) 1.0581(3) 0.5001(2) 0.0358(7) Uani 1 1 d . . . . .
H16A H 0.5439 1.1363 0.4708 0.054 Uiso 1 1 calc R U . . .
H16B H 0.5825 1.0134 0.4805 0.054 Uiso 1 1 calc R U . . .
H16C H 0.5524 1.0753 0.5574 0.054 Uiso 1 1 calc R U . . .
C17 C 0.48664(12) 0.9462(3) 0.39837(18) 0.0312(7) Uani 1 1 d . . . . .
H17A H 0.4821 1.0224 0.3671 0.047 Uiso 1 1 calc R U . . .
H17B H 0.4521 0.8934 0.3907 0.047 Uiso 1 1 calc R U . . .
H17C H 0.5218 0.9019 0.3804 0.047 Uiso 1 1 calc R U . . .
C18 C 0.32497(11) 1.0152(2) 0.69762(15) 0.0201(5) Uani 1 1 d . . . . .
H18 H 0.3306 0.9235 0.7012 0.024 Uiso 1 1 calc R U . . .
C19 C 0.34632(13) 1.0730(3) 0.77651(16) 0.0283(6) Uani 1 1 d . . . . .
H19A H 0.3373 1.1617 0.7767 0.042 Uiso 1 1 calc R U . . .
H19B H 0.3888 1.0613 0.7815 0.042 Uiso 1 1 calc R U . . .
H19C H 0.3265 1.0327 0.8217 0.042 Uiso 1 1 calc R U . . .
C20 C 0.25918(11) 1.0406(2) 0.68706(17) 0.0252(6) Uani 1 1 d . . . . .
H20A H 0.2468 1.0141 0.6335 0.038 Uiso 1 1 calc R U . . .
H20B H 0.2517 1.1295 0.6933 0.038 Uiso 1 1 calc R U . . .
H20C H 0.2370 0.9945 0.7276 0.038 Uiso 1 1 calc R U . . .
C21 C 0.27492(10) 1.0870(2) 0.44990(13) 0.0148(5) Uani 1 1 d . . . . .
C22 C 0.24632(11) 1.2119(2) 0.42685(15) 0.0188(5) Uani 1 1 d . . . . .
C23 C 0.19315(11) 1.1755(2) 0.37417(15) 0.0211(5) Uani 1 1 d . . . . .
H23A H 0.1595 1.2310 0.3851 0.025 Uiso 1 1 calc R U . . .
H23B H 0.2034 1.1819 0.3167 0.025 Uiso 1 1 calc R U . . .
C24 C 0.17751(11) 1.0418(2) 0.39560(16) 0.0208(5) Uani 1 1 d . . . . .
C25 C 0.28838(12) 1.2896(2) 0.37558(16) 0.0247(6) Uani 1 1 d . . . . .
H25A H 0.2678 1.3633 0.3558 0.037 Uiso 1 1 calc R U . . .
H25B H 0.3021 1.2402 0.3300 0.037 Uiso 1 1 calc R U . . .
H25C H 0.3221 1.3151 0.4081 0.037 Uiso 1 1 calc R U . . .
C26 C 0.22747(11) 1.2885(2) 0.50018(17) 0.0264(5) Uani 1 1 d . . . . .
H26A H 0.2045 1.3602 0.4824 0.040 Uiso 1 1 calc R U . . .
H26B H 0.2624 1.3171 0.5290 0.040 Uiso 1 1 calc R U . . .
H26C H 0.2035 1.2370 0.5358 0.040 Uiso 1 1 calc R U . . .
C27 C 0.13014(11) 1.0392(2) 0.46111(18) 0.0285(6) Uani 1 1 d . . . . .
H27A H 0.1184 0.9533 0.4714 0.043 Uiso 1 1 calc R U . . .
H27B H 0.0959 1.0869 0.4433 0.043 Uiso 1 1 calc R U . . .
H27C H 0.1459 1.0758 0.5104 0.043 Uiso 1 1 calc R U . . .
C28 C 0.15623(11) 0.9666(2) 0.32398(17) 0.0257(6) Uani 1 1 d . . . . .
H28A H 0.1851 0.9722 0.2806 0.039 Uiso 1 1 calc R U . . .
H28B H 0.1185 0.9994 0.3055 0.039 Uiso 1 1 calc R U . . .
H28C H 0.1514 0.8797 0.3398 0.039 Uiso 1 1 calc R U . . .
C29 C 0.25831(10) 0.8749(2) 0.41589(14) 0.0159(5) Uani 1 1 d . . . . .
C30 C 0.24612(10) 0.7792(2) 0.47263(17) 0.0183(5) Uani 1 1 d . . . . .
C31 C 0.27612(10) 0.6655(2) 0.46174(17) 0.0211(5) Uani 1 1 d . . . . .
H31 H 0.2676 0.5983 0.4966 0.025 Uiso 1 1 calc R U . . .
C32 C 0.31777(11) 0.6491(2) 0.40157(16) 0.0216(5) Uani 1 1 d . . . . .
H32 H 0.3378 0.5721 0.3971 0.026 Uiso 1 1 calc R U . . .
C33 C 0.33056(11) 0.7448(2) 0.34742(15) 0.0205(5) Uani 1 1 d . . . . .
H33 H 0.3603 0.7337 0.3082 0.025 Uiso 1 1 calc R U . . .
C34 C 0.29938(10) 0.8573(2) 0.35117(15) 0.0174(5) Uani 1 1 d . . . . .
C35 C 0.20290(11) 0.7913(2) 0.54109(16) 0.0229(5) Uani 1 1 d . . . . .
H35 H 0.1923 0.8808 0.5467 0.027 Uiso 1 1 calc R U . . .
C36 C 0.22831(12) 0.7468(2) 0.62107(16) 0.0284(6) Uani 1 1 d . . . . .
H36A H 0.2658 0.7885 0.6310 0.043 Uiso 1 1 calc R U . . .
H36B H 0.2345 0.6570 0.6189 0.043 Uiso 1 1 calc R U . . .
H36C H 0.2008 0.7665 0.6644 0.043 Uiso 1 1 calc R U . . .
C37 C 0.14655(12) 0.7186(3) 0.5219(2) 0.0378(8) Uani 1 1 d . . . . .
H37A H 0.1555 0.6298 0.5195 0.057 Uiso 1 1 calc R U . . .
H37B H 0.1309 0.7458 0.4702 0.057 Uiso 1 1 calc R U . . .
H37C H 0.1173 0.7336 0.5639 0.057 Uiso 1 1 calc R U . . .
C38 C 0.30638(11) 0.9505(2) 0.28359(15) 0.0183(5) Uani 1 1 d . . . . .
H38 H 0.2789 1.0208 0.2942 0.022 Uiso 1 1 calc R U . . .
C39 C 0.36813(11) 1.0040(3) 0.27584(16) 0.0250(6) Uani 1 1 d . . . . .
H39A H 0.3687 1.0659 0.2329 0.037 Uiso 1 1 calc R U . . .
H39B H 0.3958 0.9373 0.2632 0.037 Uiso 1 1 calc R U . . .
H39C H 0.3795 1.0432 0.3265 0.037 Uiso 1 1 calc R U . . .
C40 C 0.28848(13) 0.8909(2) 0.20345(16) 0.0266(6) Uani 1 1 d . . . . .
H40A H 0.2875 0.9545 0.1616 0.040 Uiso 1 1 calc R U . . .
H40B H 0.2495 0.8534 0.2088 0.040 Uiso 1 1 calc R U . . .
H40C H 0.3171 0.8269 0.1889 0.040 Uiso 1 1 calc R U . . .
C1A C 0.4397(3) 0.5210(5) 0.2473(4) 0.0249(14) Uani 0.452(5) 1 d D U P A 1
C2A C 0.4157(4) 0.5724(10) 0.1793(6) 0.026(2) Uani 0.452(5) 1 d D U P A 1
H2D H 0.3810 0.5377 0.1571 0.031 Uiso 0.452(5) 1 calc R U P A 1
C3A C 0.4419(3) 0.6757(6) 0.1422(4) 0.0336(16) Uani 0.452(5) 1 d D U P A 1
H3D H 0.4250 0.7099 0.0950 0.040 Uiso 0.452(5) 1 calc R U P A 1
C4A C 0.4917(3) 0.7268(6) 0.1742(4) 0.0276(15) Uani 0.452(5) 1 d D U P A 1
H4D H 0.5094 0.7970 0.1498 0.033 Uiso 0.452(5) 1 calc R U P A 1
C5A C 0.5160(3) 0.6748(7) 0.2429(4) 0.0271(16) Uani 0.452(5) 1 d D U P A 1
H5D H 0.5505 0.7095 0.2655 0.033 Uiso 0.452(5) 1 calc R U P A 1
C6A C 0.4903(6) 0.5740(12) 0.2778(8) 0.023(2) Uani 0.452(5) 1 d D U P A 1
H6D H 0.5077 0.5392 0.3244 0.027 Uiso 0.452(5) 1 calc R U P A 1
C7A C 0.4138(4) 0.4063(8) 0.2834(6) 0.031(2) Uani 0.452(5) 1 d D U P A 1
H7AD H 0.4210 0.3357 0.2478 0.047 Uiso 0.452(5) 1 calc R U P A 1
H7AE H 0.3714 0.4176 0.2904 0.047 Uiso 0.452(5) 1 calc R U P A 1
H7AF H 0.4320 0.3906 0.3356 0.047 Uiso 0.452(5) 1 calc R U P A 1
C1B C 0.4788(2) 0.6206(5) 0.2273(3) 0.0245(12) Uani 0.548(5) 1 d D U P A 2
C2B C 0.4358(3) 0.5928(9) 0.1711(5) 0.0300(19) Uani 0.548(5) 1 d D U P A 2
H2E H 0.4313 0.6436 0.1250 0.036 Uiso 0.548(5) 1 calc R U P A 2
C3B C 0.3992(2) 0.4909(6) 0.1820(3) 0.0332(14) Uani 0.548(5) 1 d D U P A 2
H3E H 0.3700 0.4728 0.1431 0.040 Uiso 0.548(5) 1 calc R U P A 2
C4B C 0.4046(3) 0.4164(8) 0.2481(4) 0.0325(17) Uani 0.548(5) 1 d D U P A 2
H4E H 0.3791 0.3477 0.2554 0.039 Uiso 0.548(5) 1 calc R U P A 2
C5B C 0.4480(3) 0.4430(5) 0.3043(3) 0.0316(14) Uani 0.548(5) 1 d D U P A 2
H5E H 0.4528 0.3914 0.3499 0.038 Uiso 0.548(5) 1 calc R U P A 2
C6B C 0.4841(5) 0.5451(10) 0.2933(6) 0.0247(19) Uani 0.548(5) 1 d D U P A 2
H6E H 0.5133 0.5634 0.3323 0.030 Uiso 0.548(5) 1 calc R U P A 2
C7B C 0.5181(3) 0.7304(7) 0.2157(5) 0.0423(18) Uani 0.548(5) 1 d D U P A 2
H7BD H 0.5226 0.7471 0.1583 0.063 Uiso 0.548(5) 1 calc R U P A 2
H7BE H 0.5567 0.7130 0.2392 0.063 Uiso 0.548(5) 1 calc R U P A 2
H7BF H 0.5008 0.8028 0.2421 0.063 Uiso 0.548(5) 1 calc R U P A 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Co1 C1 1.854(2) . ?
Co1 C29 2.077(2) . ?
Co1 C30 2.090(2) . ?
Co1 C31 2.136(2) . ?
Co1 C32 2.179(2) . ?
Co1 C33 2.183(2) . ?
Co1 C34 2.184(2) . ?
Co1 Co2 2.6550(6) . ?
Co2 C21 1.853(2) . ?
Co2 C9 2.075(2) . ?
Co2 C14 2.091(2) . ?
Co2 C13 2.123(2) . ?
Co2 C12 2.158(2) . ?
Co2 C11 2.169(2) . ?
Co2 C10 2.187(2) . ?
N1 C1 1.369(3) . ?
N1 C9 1.435(3) . ?
N1 C4 1.502(3) . ?
N2 C21 1.367(3) . ?
N2 C29 1.434(3) . ?
N2 C24 1.501(3) . ?
C1 C2 1.554(3) . ?
C2 C5 1.530(4) . ?
C2 C6 1.544(4) . ?
C2 C3 1.545(3) . ?
C3 C4 1.524(3) . ?
C4 C8 1.519(3) . ?
C4 C7 1.534(3) . ?
C9 C14 1.427(3) . ?
C9 C10 1.440(3) . ?
C10 C11 1.407(3) . ?
C10 C15 1.525(3) . ?
C11 C12 1.399(4) . ?
C12 C13 1.396(4) . ?
C13 C14 1.416(3) . ?
C14 C18 1.523(4) . ?
C15 C17 1.521(4) . ?
C15 C16 1.538(3) . ?
C18 C20 1.533(3) . ?
C18 C19 1.536(4) . ?
C21 C22 1.546(3) . ?
C22 C25 1.534(4) . ?
C22 C26 1.538(3) . ?
C22 C23 1.547(3) . ?
C23 C24 1.529(3) . ?
C24 C28 1.524(4) . ?
C24 C27 1.536(4) . ?
C29 C30 1.429(3) . ?
C29 C34 1.441(3) . ?
C30 C31 1.416(3) . ?
C30 C35 1.514(4) . ?
C31 C32 1.393(4) . ?
C32 C33 1.403(4) . ?
C33 C34 1.408(3) . ?
C34 C38 1.520(3) . ?
C35 C36 1.532(4) . ?
C35 C37 1.538(4) . ?
C38 C39 1.526(3) . ?
C38 C40 1.539(3) . ?
C1A C2A 1.375(10) . ?
C1A C6A 1.384(12) . ?
C1A C7A 1.498(10) . ?
C2A C3A 1.408(10) . ?
C3A C4A 1.370(9) . ?
C4A C5A 1.392(9) . ?
C5A C6A 1.366(11) . ?
C1B C6B 1.377(9) . ?
C1B C2B 1.389(9) . ?
C1B C7B 1.497(8) . ?
C2B C3B 1.392(8) . ?
C3B C4B 1.370(9) . ?
C4B C5B 1.392(9) . ?
C5B C6B 1.389(10) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C1 Co1 C29 161.80(10) . . ?
C1 Co1 C30 128.59(10) . . ?
C29 Co1 C30 40.12(9) . . ?
C1 Co1 C31 109.16(10) . . ?
C29 Co1 C31 70.12(9) . . ?
C30 Co1 C31 39.13(9) . . ?
C1 Co1 C32 108.59(10) . . ?
C29 Co1 C32 82.20(9) . . ?
C30 Co1 C32 70.27(10) . . ?
C31 Co1 C32 37.64(10) . . ?
C1 Co1 C33 127.38(10) . . ?
C29 Co1 C33 70.06(9) . . ?
C30 Co1 C33 84.16(10) . . ?
C31 Co1 C33 68.50(10) . . ?
C32 Co1 C33 37.54(10) . . ?
C1 Co1 C34 158.05(10) . . ?
C29 Co1 C34 39.44(9) . . ?
C30 Co1 C34 71.84(10) . . ?
C31 Co1 C34 81.61(10) . . ?
C32 Co1 C34 67.88(9) . . ?
C33 Co1 C34 37.62(9) . . ?
C1 Co1 Co2 89.91(7) . . ?
C29 Co1 Co2 82.19(6) . . ?
C30 Co1 Co2 104.89(6) . . ?
C31 Co1 Co2 143.67(7) . . ?
C32 Co1 Co2 159.76(7) . . ?
C33 Co1 Co2 123.84(7) . . ?
C34 Co1 Co2 91.89(6) . . ?
C21 Co2 C9 162.58(9) . . ?
C21 Co2 C14 128.98(10) . . ?
C9 Co2 C14 40.06(9) . . ?
C21 Co2 C13 108.52(10) . . ?
C9 Co2 C13 70.43(9) . . ?
C14 Co2 C13 39.26(9) . . ?
C21 Co2 C12 107.46(9) . . ?
C9 Co2 C12 82.64(9) . . ?
C14 Co2 C12 70.63(9) . . ?
C13 Co2 C12 38.06(10) . . ?
C21 Co2 C11 126.48(9) . . ?
C9 Co2 C11 70.11(9) . . ?
C14 Co2 C11 84.20(10) . . ?
C13 Co2 C11 68.95(10) . . ?
C12 Co2 C11 37.73(10) . . ?
C21 Co2 C10 157.50(9) . . ?
C9 Co2 C10 39.37(9) . . ?
C14 Co2 C10 71.72(9) . . ?
C13 Co2 C10 82.02(9) . . ?
C12 Co2 C10 68.24(9) . . ?
C11 Co2 C10 37.70(8) . . ?
C21 Co2 Co1 90.17(7) . . ?
C9 Co2 Co1 82.51(6) . . ?
C14 Co2 Co1 104.99(6) . . ?
C13 Co2 Co1 143.75(7) . . ?
C12 Co2 Co1 160.49(7) . . ?
C11 Co2 Co1 124.19(7) . . ?
C10 Co2 Co1 92.27(6) . . ?
C1 N1 C9 116.97(19) . . ?
C1 N1 C4 117.27(18) . . ?
C9 N1 C4 124.53(18) . . ?
C21 N2 C29 116.92(18) . . ?
C21 N2 C24 116.94(19) . . ?
C29 N2 C24 124.45(19) . . ?
N1 C1 C2 104.90(19) . . ?
N1 C1 Co1 125.57(17) . . ?
C2 C1 Co1 129.38(17) . . ?
C5 C2 C6 109.5(2) . . ?
C5 C2 C3 108.4(2) . . ?
C6 C2 C3 111.4(2) . . ?
C5 C2 C1 111.4(2) . . ?
C6 C2 C1 111.6(2) . . ?
C3 C2 C1 104.45(18) . . ?
C4 C3 C2 106.90(19) . . ?
N1 C4 C8 112.38(19) . . ?
N1 C4 C3 99.78(18) . . ?
C8 C4 C3 113.3(2) . . ?
N1 C4 C7 112.04(19) . . ?
C8 C4 C7 108.5(2) . . ?
C3 C4 C7 110.7(2) . . ?
C14 C9 N1 121.3(2) . . ?
C14 C9 C10 122.0(2) . . ?
N1 C9 C10 116.3(2) . . ?
C14 C9 Co2 70.58(13) . . ?
N1 C9 Co2 121.90(15) . . ?
C10 C9 Co2 74.52(13) . . ?
C11 C10 C9 117.9(2) . . ?
C11 C10 C15 118.9(2) . . ?
C9 C10 C15 123.0(2) . . ?
C11 C10 Co2 70.45(13) . . ?
C9 C10 Co2 66.11(13) . . ?
C15 C10 Co2 139.71(17) . . ?
C12 C11 C10 120.6(2) . . ?
C12 C11 Co2 70.70(14) . . ?
C10 C11 Co2 71.86(13) . . ?
C13 C12 C11 120.7(2) . . ?
C13 C12 Co2 69.60(13) . . ?
C11 C12 Co2 71.57(13) . . ?
C12 C13 C14 121.8(2) . . ?
C12 C13 Co2 72.33(14) . . ?
C14 C13 Co2 69.17(13) . . ?
C13 C14 C9 116.8(2) . . ?
C13 C14 C18 118.8(2) . . ?
C9 C14 C18 124.4(2) . . ?
C13 C14 Co2 71.57(14) . . ?
C9 C14 Co2 69.37(13) . . ?
C18 C14 Co2 130.52(17) . . ?
C17 C15 C10 114.2(2) . . ?
C17 C15 C16 110.1(2) . . ?
C10 C15 C16 109.6(2) . . ?
C14 C18 C20 112.3(2) . . ?
C14 C18 C19 110.7(2) . . ?
C20 C18 C19 109.6(2) . . ?
N2 C21 C22 105.50(19) . . ?
N2 C21 Co2 124.92(17) . . ?
C22 C21 Co2 129.45(16) . . ?
C25 C22 C26 108.9(2) . . ?
C25 C22 C21 110.7(2) . . ?
C26 C22 C21 112.9(2) . . ?
C25 C22 C23 108.1(2) . . ?
C26 C22 C23 111.7(2) . . ?
C21 C22 C23 104.46(18) . . ?
C24 C23 C22 106.79(19) . . ?
N2 C24 C28 112.5(2) . . ?
N2 C24 C23 99.91(19) . . ?
C28 C24 C23 113.2(2) . . ?
N2 C24 C27 111.8(2) . . ?
C28 C24 C27 109.0(2) . . ?
C23 C24 C27 110.3(2) . . ?
C30 C29 N2 121.2(2) . . ?
C30 C29 C34 121.8(2) . . ?
N2 C29 C34 116.6(2) . . ?
C30 C29 Co1 70.40(13) . . ?
N2 C29 Co1 121.92(15) . . ?
C34 C29 Co1 74.27(14) . . ?
C31 C30 C29 116.6(2) . . ?
C31 C30 C35 119.1(2) . . ?
C29 C30 C35 124.3(2) . . ?
C31 C30 Co1 72.22(13) . . ?
C29 C30 Co1 69.47(13) . . ?
C35 C30 Co1 129.81(18) . . ?
C32 C31 C30 122.1(2) . . ?
C32 C31 Co1 72.84(14) . . ?
C30 C31 Co1 68.65(12) . . ?
C31 C32 C33 120.8(2) . . ?
C31 C32 Co1 69.51(13) . . ?
C33 C32 Co1 71.38(14) . . ?
C32 C33 C34 120.1(2) . . ?
C32 C33 Co1 71.09(15) . . ?
C34 C33 Co1 71.23(14) . . ?
C33 C34 C29 118.3(2) . . ?
C33 C34 C38 119.0(2) . . ?
C29 C34 C38 122.5(2) . . ?
C33 C34 Co1 71.15(14) . . ?
C29 C34 Co1 66.28(13) . . ?
C38 C34 Co1 139.51(16) . . ?
C30 C35 C36 112.6(2) . . ?
C30 C35 C37 109.9(2) . . ?
C36 C35 C37 109.6(2) . . ?
C34 C38 C39 114.2(2) . . ?
C34 C38 C40 109.91(19) . . ?
C39 C38 C40 109.2(2) . . ?
C2A C1A C6A 117.9(7) . . ?
C2A C1A C7A 120.5(7) . . ?
C6A C1A C7A 121.4(7) . . ?
C1A C2A C3A 120.9(7) . . ?
C4A C3A C2A 119.9(7) . . ?
C3A C4A C5A 119.2(6) . . ?
C6A C5A C4A 120.2(8) . . ?
C5A C6A C1A 121.9(9) . . ?
C6B C1B C2B 118.4(7) . . ?
C6B C1B C7B 121.2(6) . . ?
C2B C1B C7B 120.4(6) . . ?
C1B C2B C3B 120.3(7) . . ?
C4B C3B C2B 121.1(6) . . ?
C3B C4B C5B 119.0(6) . . ?
C6B C5B C4B 119.7(6) . . ?
C1B C6B C5B 121.5(8) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 N1 C1 C2 162.61(19) . . . . ?
C4 N1 C1 C2 -5.3(3) . . . . ?
C9 N1 C1 Co1 -21.5(3) . . . . ?
C4 N1 C1 Co1 170.56(16) . . . . ?
C29 Co1 C1 N1 -51.6(4) . . . . ?
C30 Co1 C1 N1 -96.8(2) . . . . ?
C31 Co1 C1 N1 -136.14(19) . . . . ?
C32 Co1 C1 N1 -176.01(19) . . . . ?
C33 Co1 C1 N1 146.73(18) . . . . ?
C34 Co1 C1 N1 107.2(3) . . . . ?
Co2 Co1 C1 N1 12.32(19) . . . . ?
C29 Co1 C1 C2 123.3(3) . . . . ?
C30 Co1 C1 C2 78.1(2) . . . . ?
C31 Co1 C1 C2 38.7(2) . . . . ?
C32 Co1 C1 C2 -1.1(2) . . . . ?
C33 Co1 C1 C2 -38.4(3) . . . . ?
C34 Co1 C1 C2 -78.0(3) . . . . ?
Co2 Co1 C1 C2 -172.8(2) . . . . ?
N1 C1 C2 C5 -128.3(2) . . . . ?
Co1 C1 C2 C5 56.0(3) . . . . ?
N1 C1 C2 C6 109.0(2) . . . . ?
Co1 C1 C2 C6 -66.7(3) . . . . ?
N1 C1 C2 C3 -11.5(2) . . . . ?
Co1 C1 C2 C3 172.85(18) . . . . ?
C5 C2 C3 C4 142.5(2) . . . . ?
C6 C2 C3 C4 -97.0(2) . . . . ?
C1 C2 C3 C4 23.6(3) . . . . ?
C1 N1 C4 C8 140.0(2) . . . . ?
C9 N1 C4 C8 -26.9(3) . . . . ?
C1 N1 C4 C3 19.7(3) . . . . ?
C9 N1 C4 C3 -147.3(2) . . . . ?
C1 N1 C4 C7 -97.5(2) . . . . ?
C9 N1 C4 C7 95.5(3) . . . . ?
C2 C3 C4 N1 -25.1(2) . . . . ?
C2 C3 C4 C8 -144.8(2) . . . . ?
C2 C3 C4 C7 93.0(2) . . . . ?
C1 N1 C9 C14 104.5(3) . . . . ?
C4 N1 C9 C14 -88.5(3) . . . . ?
C1 N1 C9 C10 -68.4(3) . . . . ?
C4 N1 C9 C10 98.6(3) . . . . ?
C1 N1 C9 Co2 19.1(3) . . . . ?
C4 N1 C9 Co2 -173.91(16) . . . . ?
C14 C9 C10 C11 -4.9(3) . . . . ?
N1 C9 C10 C11 167.9(2) . . . . ?
Co2 C9 C10 C11 49.58(19) . . . . ?
C14 C9 C10 C15 170.5(2) . . . . ?
N1 C9 C10 C15 -16.6(3) . . . . ?
Co2 C9 C10 C15 -135.0(2) . . . . ?
C14 C9 C10 Co2 -54.5(2) . . . . ?
N1 C9 C10 Co2 118.35(19) . . . . ?
C9 C10 C11 C12 5.7(3) . . . . ?
C15 C10 C11 C12 -169.9(2) . . . . ?
Co2 C10 C11 C12 53.3(2) . . . . ?
C9 C10 C11 Co2 -47.62(18) . . . . ?
C15 C10 C11 Co2 136.8(2) . . . . ?
C10 C11 C12 C13 -2.6(4) . . . . ?
Co2 C11 C12 C13 51.3(2) . . . . ?
C10 C11 C12 Co2 -53.8(2) . . . . ?
C11 C12 C13 C14 -1.7(4) . . . . ?
Co2 C12 C13 C14 50.5(2) . . . . ?
C11 C12 C13 Co2 -52.2(2) . . . . ?
C12 C13 C14 C9 2.4(3) . . . . ?
Co2 C13 C14 C9 54.26(18) . . . . ?
C12 C13 C14 C18 -178.6(2) . . . . ?
Co2 C13 C14 C18 -126.7(2) . . . . ?
C12 C13 C14 Co2 -51.9(2) . . . . ?
N1 C9 C14 C13 -171.6(2) . . . . ?
C10 C9 C14 C13 1.0(3) . . . . ?
Co2 C9 C14 C13 -55.37(19) . . . . ?
N1 C9 C14 C18 9.5(3) . . . . ?
C10 C9 C14 C18 -178.0(2) . . . . ?
Co2 C9 C14 C18 125.7(2) . . . . ?
N1 C9 C14 Co2 -116.2(2) . . . . ?
C10 C9 C14 Co2 56.3(2) . . . . ?
C11 C10 C15 C17 -66.1(3) . . . . ?
C9 C10 C15 C17 118.6(3) . . . . ?
Co2 C10 C15 C17 27.4(4) . . . . ?
C11 C10 C15 C16 58.0(3) . . . . ?
C9 C10 C15 C16 -117.4(3) . . . . ?
Co2 C10 C15 C16 151.4(2) . . . . ?
C13 C14 C18 C20 48.7(3) . . . . ?
C9 C14 C18 C20 -132.4(2) . . . . ?
Co2 C14 C18 C20 -41.0(3) . . . . ?
C13 C14 C18 C19 -74.2(3) . . . . ?
C9 C14 C18 C19 104.8(3) . . . . ?
Co2 C14 C18 C19 -163.86(18) . . . . ?
C29 N2 C21 C22 159.76(19) . . . . ?
C24 N2 C21 C22 -6.1(3) . . . . ?
C29 N2 C21 Co2 -24.0(3) . . . . ?
C24 N2 C21 Co2 170.14(17) . . . . ?
C9 Co2 C21 N2 -50.7(4) . . . . ?
C14 Co2 C21 N2 -95.4(2) . . . . ?
C13 Co2 C21 N2 -134.24(19) . . . . ?
C12 Co2 C21 N2 -174.33(19) . . . . ?
C11 Co2 C21 N2 148.66(18) . . . . ?
C10 Co2 C21 N2 110.5(3) . . . . ?
Co1 Co2 C21 N2 14.14(19) . . . . ?
C9 Co2 C21 C22 124.6(3) . . . . ?
C14 Co2 C21 C22 79.8(2) . . . . ?
C13 Co2 C21 C22 41.0(2) . . . . ?
C12 Co2 C21 C22 0.9(2) . . . . ?
C11 Co2 C21 C22 -36.1(3) . . . . ?
C10 Co2 C21 C22 -74.2(3) . . . . ?
Co1 Co2 C21 C22 -170.6(2) . . . . ?
N2 C21 C22 C25 -126.6(2) . . . . ?
Co2 C21 C22 C25 57.4(3) . . . . ?
N2 C21 C22 C26 111.1(2) . . . . ?
Co2 C21 C22 C26 -64.9(3) . . . . ?
N2 C21 C22 C23 -10.5(2) . . . . ?
Co2 C21 C22 C23 173.51(17) . . . . ?
C25 C22 C23 C24 140.5(2) . . . . ?
C26 C22 C23 C24 -99.7(2) . . . . ?
C21 C22 C23 C24 22.7(3) . . . . ?
C21 N2 C24 C28 140.1(2) . . . . ?
C29 N2 C24 C28 -24.5(3) . . . . ?
C21 N2 C24 C23 19.8(3) . . . . ?
C29 N2 C24 C23 -144.8(2) . . . . ?
C21 N2 C24 C27 -96.9(2) . . . . ?
C29 N2 C24 C27 98.5(3) . . . . ?
C22 C23 C24 N2 -24.6(2) . . . . ?
C22 C23 C24 C28 -144.5(2) . . . . ?
C22 C23 C24 C27 93.2(2) . . . . ?
C21 N2 C29 C30 106.1(2) . . . . ?
C24 N2 C29 C30 -89.3(3) . . . . ?
C21 N2 C29 C34 -66.5(3) . . . . ?
C24 N2 C29 C34 98.2(3) . . . . ?
C21 N2 C29 Co1 20.9(3) . . . . ?
C24 N2 C29 Co1 -174.43(17) . . . . ?
N2 C29 C30 C31 -172.6(2) . . . . ?
C34 C29 C30 C31 -0.5(3) . . . . ?
Co1 C29 C30 C31 -56.47(18) . . . . ?
N2 C29 C30 C35 8.8(3) . . . . ?
C34 C29 C30 C35 -179.1(2) . . . . ?
Co1 C29 C30 C35 124.9(2) . . . . ?
N2 C29 C30 Co1 -116.1(2) . . . . ?
C34 C29 C30 Co1 56.0(2) . . . . ?
C29 C30 C31 C32 3.3(3) . . . . ?
C35 C30 C31 C32 -178.0(2) . . . . ?
Co1 C30 C31 C32 -51.7(2) . . . . ?
C29 C30 C31 Co1 55.07(18) . . . . ?
C35 C30 C31 Co1 -126.2(2) . . . . ?
C30 C31 C32 C33 -1.8(4) . . . . ?
Co1 C31 C32 C33 -51.7(2) . . . . ?
C30 C31 C32 Co1 49.9(2) . . . . ?
C31 C32 C33 C34 -2.8(4) . . . . ?
Co1 C32 C33 C34 -53.7(2) . . . . ?
C31 C32 C33 Co1 50.9(2) . . . . ?
C32 C33 C34 C29 5.5(3) . . . . ?
Co1 C33 C34 C29 -48.17(19) . . . . ?
C32 C33 C34 C38 -169.5(2) . . . . ?
Co1 C33 C34 C38 136.9(2) . . . . ?
C32 C33 C34 Co1 53.6(2) . . . . ?
C30 C29 C34 C33 -3.9(3) . . . . ?
N2 C29 C34 C33 168.6(2) . . . . ?
Co1 C29 C34 C33 50.4(2) . . . . ?
C30 C29 C34 C38 170.9(2) . . . . ?
N2 C29 C34 C38 -16.6(3) . . . . ?
Co1 C29 C34 C38 -134.8(2) . . . . ?
C30 C29 C34 Co1 -54.24(19) . . . . ?
N2 C29 C34 Co1 118.25(19) . . . . ?
C31 C30 C35 C36 49.0(3) . . . . ?
C29 C30 C35 C36 -132.4(2) . . . . ?
Co1 C30 C35 C36 -41.5(3) . . . . ?
C31 C30 C35 C37 -73.6(3) . . . . ?
C29 C30 C35 C37 105.0(3) . . . . ?
Co1 C30 C35 C37 -164.04(18) . . . . ?
C33 C34 C38 C39 -64.7(3) . . . . ?
C29 C34 C38 C39 120.6(2) . . . . ?
Co1 C34 C38 C39 29.9(4) . . . . ?
C33 C34 C38 C40 58.4(3) . . . . ?
C29 C34 C38 C40 -116.3(2) . . . . ?
Co1 C34 C38 C40 153.1(2) . . . . ?
C6A C1A C2A C3A -0.1(15) . . . . ?
C7A C1A C2A C3A -176.0(8) . . . . ?
C1A C2A C3A C4A -0.5(13) . . . . ?
C2A C3A C4A C5A 0.6(11) . . . . ?
C3A C4A C5A C6A -0.1(13) . . . . ?
C4A C5A C6A C1A -0.6(19) . . . . ?
C2A C1A C6A C5A 0.7(19) . . . . ?
C7A C1A C6A C5A 176.5(11) . . . . ?
C6B C1B C2B C3B 0.1(12) . . . . ?
C7B C1B C2B C3B -179.9(6) . . . . ?
C1B C2B C3B C4B 0.2(11) . . . . ?
C2B C3B C4B C5B -0.8(11) . . . . ?
C3B C4B C5B C6B 1.2(12) . . . . ?
C2B C1B C6B C5B 0.3(16) . . . . ?
C7B C1B C6B C5B -179.8(9) . . . . ?
C4B C5B C6B C1B -0.9(16) . . . . ?
 
_refine_diff_density_max    0.211
_refine_diff_density_min   -0.270
_refine_diff_density_rms    0.040

_shelxl_version_number 2012-9



 
data_sad_a
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          '1(C40 H62 Co2 N2), 1(C F3 O3 S), 1.5(C7 H8)'
_chemical_formula_sum
 'C51.50 H74 Co2 F3 N2 O3 S' 
_chemical_formula_weight          976.04

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    21.3850(10)
_cell_length_b                    10.5130(10)
_cell_length_c                    22.5320(10)
_cell_angle_alpha                 90
_cell_angle_beta                  107.59(2)
_cell_angle_gamma                 90
_cell_volume                      4828.8(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9313
_cell_measurement_theta_min       2.2525 
_cell_measurement_theta_max       27.793 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             orange 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.343          
_exptl_crystal_F_000              2072
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.09 
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.03  
_exptl_absorpt_coefficient_mu     0.785
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.6859  
_exptl_absorpt_correction_T_max   0.7454  
_exptl_absorpt_process_details    'SADABS-2012/1'   
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                        
_diffrn_measurement_device_type   'Bruker Smart Apex II Quazar'
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             90157
_diffrn_reflns_av_unetI/netI      0.0321
_diffrn_reflns_av_R_equivalents   0.0554
_diffrn_reflns_limit_h_min        -26
_diffrn_reflns_limit_h_max        26
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          1.151
_diffrn_reflns_theta_max          26.423
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.995
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.995
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.995
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              9887
_reflns_number_gt                 8144
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'APEX2 v2011.2'
_computing_cell_refinement        'SAINT V7.68A'
_computing_data_reduction         'SAINT V7.68A' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics      'shelXle v0.477'
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0197P)²+6.9902P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          9887
_refine_ls_number_parameters      751
_refine_ls_number_restraints      1129
_refine_ls_R_factor_all           0.0581
_refine_ls_R_factor_gt            0.0441
_refine_ls_wR_factor_ref          0.0911
_refine_ls_wR_factor_gt           0.0867
_refine_ls_goodness_of_fit_ref    1.127
_refine_ls_restrained_S_all       1.106
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Co1 Co 0.23637(2) 0.67230(3) 0.45102(2) 0.01425(8) Uani 1 1 d . . . . .
Co2 Co 0.30894(2) 0.83018(3) 0.51866(2) 0.01548(8) Uani 1 1 d . . . . .
N1 N 0.23901(10) 0.90302(19) 0.38482(9) 0.0167(4) Uani 1 1 d . . . . .
N2 N 0.34355(9) 0.57705(19) 0.56481(9) 0.0165(4) Uani 1 1 d . . . . .
C1 C 0.20769(11) 0.7936(2) 0.38654(11) 0.0150(5) Uani 1 1 d . . . . .
C2 C 0.14968(12) 0.7876(2) 0.32554(11) 0.0174(5) Uani 1 1 d . . . . .
C3 C 0.14958(13) 0.9212(2) 0.29647(12) 0.0233(6) Uani 1 1 d . . . . .
H3A H 0.1380 0.9149 0.2506 0.028 Uiso 1 1 calc R U . . .
H3B H 0.1173 0.9772 0.3071 0.028 Uiso 1 1 calc R U . . .
C4 C 0.21888(13) 0.9744(3) 0.32362(12) 0.0242(6) Uani 1 1 d . . . . .
C5 C 0.15703(12) 0.6823(3) 0.28070(12) 0.0218(5) Uani 1 1 d . . . . .
H5A H 0.1505 0.5991 0.2975 0.033 Uiso 1 1 calc R U . . .
H5B H 0.2011 0.6862 0.2760 0.033 Uiso 1 1 calc R U . . .
H5C H 0.1242 0.6946 0.2400 0.033 Uiso 1 1 calc R U . . .
C6 C 0.08505(12) 0.7679(3) 0.34116(12) 0.0224(6) Uani 1 1 d . . . . .
H6A H 0.0479 0.7773 0.3032 0.034 Uiso 1 1 calc R U . . .
H6B H 0.0816 0.8315 0.3718 0.034 Uiso 1 1 calc R U . . .
H6C H 0.0845 0.6824 0.3584 0.034 Uiso 1 1 calc R U . . .
C7 C 0.26293(14) 0.9364(3) 0.28392(12) 0.0310(7) Uani 1 1 d . . . . .
H7A H 0.2664 0.8436 0.2831 0.047 Uiso 1 1 calc R U . . .
H7B H 0.3067 0.9734 0.3019 0.047 Uiso 1 1 calc R U . . .
H7C H 0.2438 0.9682 0.2414 0.047 Uiso 1 1 calc R U . . .
C8 C 0.22079(15) 1.1178(3) 0.33318(14) 0.0332(7) Uani 1 1 d . . . . .
H8A H 0.2081 1.1604 0.2926 0.050 Uiso 1 1 calc R U . . .
H8B H 0.2653 1.1437 0.3570 0.050 Uiso 1 1 calc R U . . .
H8C H 0.1902 1.1415 0.3561 0.050 Uiso 1 1 calc R U . . .
C9 C 0.28055(12) 0.9511(2) 0.44327(11) 0.0166(5) Uani 1 1 d . . . . .
C10 C 0.24730(12) 0.9954(2) 0.48621(12) 0.0193(5) Uani 1 1 d . . . . .
C11 C 0.28462(13) 1.0200(2) 0.54776(12) 0.0225(6) Uani 1 1 d . . . . .
H11 H 0.2632 1.0426 0.5776 0.027 Uiso 1 1 calc R U . . .
C12 C 0.35335(13) 1.0117(2) 0.56589(12) 0.0227(6) Uani 1 1 d . . . . .
H12 H 0.3783 1.0313 0.6075 0.027 Uiso 1 1 calc R U . . .
C13 C 0.38490(13) 0.9747(2) 0.52269(12) 0.0221(6) Uani 1 1 d . . . . .
H13 H 0.4315 0.9724 0.5355 0.027 Uiso 1 1 calc R U . . .
C14 C 0.35050(12) 0.9406(2) 0.46093(12) 0.0186(5) Uani 1 1 d . . . . .
C15 C 0.17427(12) 1.0293(2) 0.46585(12) 0.0210(5) Uani 1 1 d . . . . .
H15 H 0.1562 1.0113 0.4203 0.025 Uiso 1 1 calc R U . . .
C16 C 0.13404(13) 0.9537(3) 0.49927(13) 0.0276(6) Uani 1 1 d . . . . .
H16A H 0.0880 0.9805 0.4840 0.041 Uiso 1 1 calc R U . . .
H16B H 0.1510 0.9694 0.5442 0.041 Uiso 1 1 calc R U . . .
H16C H 0.1372 0.8628 0.4911 0.041 Uiso 1 1 calc R U . . .
C17 C 0.16723(15) 1.1726(3) 0.47557(14) 0.0327(7) Uani 1 1 d . . . . .
H17A H 0.1793 1.1909 0.5202 0.049 Uiso 1 1 calc R U . . .
H17B H 0.1217 1.1984 0.4556 0.049 Uiso 1 1 calc R U . . .
H17C H 0.1963 1.2197 0.4571 0.049 Uiso 1 1 calc R U . . .
C18 C 0.38869(12) 0.9033(2) 0.41683(12) 0.0208(5) Uani 1 1 d . . . . .
H18 H 0.3582 0.8576 0.3806 0.025 Uiso 1 1 calc R U . . .
C19 C 0.41311(13) 1.0239(3) 0.39218(13) 0.0263(6) Uani 1 1 d . . . . .
H19A H 0.4348 1.0003 0.3612 0.039 Uiso 1 1 calc R U . . .
H19B H 0.4443 1.0688 0.4268 0.039 Uiso 1 1 calc R U . . .
H19C H 0.3758 1.0797 0.3729 0.039 Uiso 1 1 calc R U . . .
C20 C 0.44681(13) 0.8158(3) 0.44660(13) 0.0280(6) Uani 1 1 d . . . . .
H20A H 0.4319 0.7432 0.4661 0.042 Uiso 1 1 calc R U . . .
H20B H 0.4803 0.8629 0.4783 0.042 Uiso 1 1 calc R U . . .
H20C H 0.4655 0.7850 0.4145 0.042 Uiso 1 1 calc R U . . .
C24 C 0.38800(12) 0.4871(3) 0.61169(12) 0.0232(6) Uani 1 1 d . . . . .
C23 C 0.40651(13) 0.5746(3) 0.66821(13) 0.0259(6) Uani 1 1 d . . . . .
H23A H 0.4524 0.5586 0.6938 0.031 Uiso 1 1 calc R U . . .
H23B H 0.3774 0.5592 0.6943 0.031 Uiso 1 1 calc R U . . .
C22 C 0.39884(12) 0.7130(2) 0.64378(12) 0.0219(6) Uani 1 1 d . . . . .
C21 C 0.35036(11) 0.7006(2) 0.57747(11) 0.0154(5) Uani 1 1 d . . . . .
C27 C 0.35213(14) 0.3669(3) 0.62060(14) 0.0293(6) Uani 1 1 d . . . . .
H27A H 0.3168 0.3893 0.6380 0.044 Uiso 1 1 calc R U . . .
H27B H 0.3830 0.3093 0.6492 0.044 Uiso 1 1 calc R U . . .
H27C H 0.3336 0.3246 0.5803 0.044 Uiso 1 1 calc R U . . .
C28 C 0.44843(13) 0.4505(3) 0.59207(14) 0.0316(7) Uani 1 1 d . . . . .
H28A H 0.4352 0.3928 0.5563 0.047 Uiso 1 1 calc R U . . .
H28B H 0.4806 0.4080 0.6268 0.047 Uiso 1 1 calc R U . . .
H28C H 0.4680 0.5273 0.5806 0.047 Uiso 1 1 calc R U . . .
C26 C 0.46477(12) 0.7724(3) 0.64348(13) 0.0279(6) Uani 1 1 d . . . . .
H26A H 0.4809 0.7290 0.6125 0.042 Uiso 1 1 calc R U . . .
H26B H 0.4969 0.7630 0.6848 0.042 Uiso 1 1 calc R U . . .
H26C H 0.4584 0.8629 0.6330 0.042 Uiso 1 1 calc R U . . .
C25 C 0.36891(14) 0.7942(3) 0.68498(12) 0.0278(6) Uani 1 1 d . . . . .
H25A H 0.3640 0.8821 0.6698 0.042 Uiso 1 1 calc R U . . .
H25B H 0.3978 0.7924 0.7280 0.042 Uiso 1 1 calc R U . . .
H25C H 0.3258 0.7599 0.6835 0.042 Uiso 1 1 calc R U . . .
C29 C 0.28730(11) 0.5390(2) 0.51364(11) 0.0153(5) Uani 1 1 d . . . . .
C30 C 0.29357(12) 0.5072(2) 0.45403(12) 0.0180(5) Uani 1 1 d . . . . .
C31 C 0.23483(12) 0.4884(2) 0.40570(12) 0.0192(5) Uani 1 1 d . . . . .
H31 H 0.2371 0.4643 0.3658 0.023 Uiso 1 1 calc R U . . .
C32 C 0.17302(12) 0.5040(2) 0.41413(12) 0.0191(5) Uani 1 1 d . . . . .
H32 H 0.1343 0.4922 0.3802 0.023 Uiso 1 1 calc R U . . .
C33 C 0.16860(11) 0.5370(2) 0.47300(12) 0.0183(5) Uani 1 1 d . . . . .
H33 H 0.1266 0.5503 0.4782 0.022 Uiso 1 1 calc R U . . .
C34 C 0.22509(11) 0.5508(2) 0.52463(11) 0.0171(5) Uani 1 1 d . . . . .
C35 C 0.35887(12) 0.4888(2) 0.44108(13) 0.0226(6) Uani 1 1 d . . . . .
H35 H 0.3943 0.5265 0.4764 0.027 Uiso 1 1 calc R U . . .
C36 C 0.36055(13) 0.5532(3) 0.38081(13) 0.0311(7) Uani 1 1 d . . . . .
H36A H 0.3328 0.5058 0.3451 0.047 Uiso 1 1 calc R U . . .
H36B H 0.4058 0.5548 0.3790 0.047 Uiso 1 1 calc R U . . .
H36C H 0.3442 0.6405 0.3797 0.047 Uiso 1 1 calc R U . . .
C37 C 0.37269(14) 0.3457(3) 0.43790(17) 0.0388(8) Uani 1 1 d . . . . .
H37A H 0.3426 0.3098 0.3998 0.058 Uiso 1 1 calc R U . . .
H37B H 0.3662 0.3028 0.4742 0.058 Uiso 1 1 calc R U . . .
H37C H 0.4181 0.3334 0.4377 0.058 Uiso 1 1 calc R U . . .
C38 C 0.21690(12) 0.5680(2) 0.58895(12) 0.0192(5) Uani 1 1 d . . . . .
H38 H 0.2615 0.5687 0.6202 0.023 Uiso 1 1 calc R U . . .
C39 C 0.18192(13) 0.6905(3) 0.59653(13) 0.0250(6) Uani 1 1 d . . . . .
H39A H 0.1387 0.6934 0.5652 0.038 Uiso 1 1 calc R U . . .
H39B H 0.2079 0.7638 0.5910 0.038 Uiso 1 1 calc R U . . .
H39C H 0.1767 0.6931 0.6382 0.038 Uiso 1 1 calc R U . . .
C40 C 0.17948(13) 0.4523(3) 0.60228(13) 0.0260(6) Uani 1 1 d . . . . .
H40A H 0.1348 0.4519 0.5733 0.039 Uiso 1 1 calc R U . . .
H40B H 0.1775 0.4569 0.6451 0.039 Uiso 1 1 calc R U . . .
H40C H 0.2022 0.3741 0.5969 0.039 Uiso 1 1 calc R U . . .
C41 C 0.63026(16) 0.4822(3) 0.17427(15) 0.0351(7) Uani 0.938(3) 1 d D U P A 1
C42 C 0.65980(18) 0.3724(3) 0.16165(19) 0.0385(9) Uani 0.938(3) 1 d D U P A 1
H42 H 0.6334 0.3061 0.1383 0.046 Uiso 0.938(3) 1 calc R U P A 1
C43 C 0.72732(18) 0.3579(3) 0.18268(16) 0.0373(8) Uani 0.938(3) 1 d D U P A 1
H43 H 0.7468 0.2826 0.1730 0.045 Uiso 0.938(3) 1 calc R U P A 1
C44 C 0.76648(18) 0.4521(4) 0.21755(16) 0.0383(8) Uani 0.938(3) 1 d D U P A 1
H44 H 0.8127 0.4416 0.2327 0.046 Uiso 0.938(3) 1 calc R U P A 1
C45 C 0.73720(18) 0.5625(3) 0.23016(16) 0.0416(8) Uani 0.938(3) 1 d D U P A 1
H45 H 0.7637 0.6289 0.2533 0.050 Uiso 0.938(3) 1 calc R U P A 1
C46 C 0.67017(18) 0.5764(3) 0.20942(18) 0.0371(8) Uani 0.938(3) 1 d D U P A 1
H46 H 0.6509 0.6517 0.2193 0.044 Uiso 0.938(3) 1 calc R U P A 1
C47 C 0.55716(18) 0.4992(4) 0.1507(2) 0.0560(11) Uani 0.938(3) 1 d D U P A 1
H47A H 0.5356 0.4183 0.1539 0.084 Uiso 0.938(3) 1 calc R U P A 1
H47B H 0.5445 0.5263 0.1070 0.084 Uiso 0.938(3) 1 calc R U P A 1
H47C H 0.5437 0.5639 0.1757 0.084 Uiso 0.938(3) 1 calc R U P A 1
C41' C 0.6963(14) 0.436(3) 0.1950(19) 0.037(2) Uani 0.062(3) 1 d D U P A 2
C42' C 0.6878(17) 0.562(3) 0.209(2) 0.037(3) Uani 0.062(3) 1 d D U P A 2
H42' H 0.7249 0.6130 0.2295 0.045 Uiso 0.062(3) 1 calc R U P A 2
C43' C 0.6254(18) 0.614(3) 0.195(2) 0.039(3) Uani 0.062(3) 1 d D U P A 2
H43' H 0.6195 0.6991 0.2057 0.047 Uiso 0.062(3) 1 calc R U P A 2
C44' C 0.5718(17) 0.541(4) 0.163(2) 0.039(4) Uani 0.062(3) 1 d D U P A 2
H44' H 0.5295 0.5781 0.1492 0.047 Uiso 0.062(3) 1 calc R U P A 2
C45' C 0.5800(16) 0.413(4) 0.153(2) 0.039(3) Uani 0.062(3) 1 d D U P A 2
H45' H 0.5428 0.3601 0.1367 0.047 Uiso 0.062(3) 1 calc R U P A 2
C46' C 0.6424(17) 0.363(3) 0.166(3) 0.037(3) Uani 0.062(3) 1 d D U P A 2
H46' H 0.6481 0.2771 0.1551 0.045 Uiso 0.062(3) 1 calc R U P A 2
C47' C 0.7645(17) 0.384(5) 0.210(3) 0.038(6) Uani 0.062(3) 1 d D U P A 2
H47D H 0.7909 0.4403 0.1920 0.057 Uiso 0.062(3) 1 calc R U P A 2
H47F H 0.7630 0.2990 0.1917 0.057 Uiso 0.062(3) 1 calc R U P A 2
H47G H 0.7843 0.3793 0.2549 0.057 Uiso 0.062(3) 1 calc R U P A 2
O1A O 0.5624(4) 0.8340(11) 0.2347(4) 0.0541(18) Uani 0.605(2) 1 d D U P B 1
O2A O 0.4788(2) 0.9987(4) 0.2270(3) 0.0624(13) Uani 0.605(2) 1 d D U P B 1
O3A O 0.5277(4) 0.8882(9) 0.3226(3) 0.0466(19) Uani 0.605(2) 1 d D U P B 1
S1A S 0.51109(6) 0.88631(11) 0.25641(7) 0.0337(4) Uani 0.605(2) 1 d D U P B 1
C1A C 0.4453(2) 0.7685(5) 0.2331(3) 0.0346(11) Uani 0.605(2) 1 d D U P B 1
F1A F 0.42415(15) 0.7511(3) 0.17258(14) 0.0482(9) Uani 0.605(2) 1 d D U P B 1
F2A F 0.3958(2) 0.8018(5) 0.2537(2) 0.0753(15) Uani 0.605(2) 1 d D U P B 1
F3A F 0.4641(6) 0.6572(6) 0.2583(6) 0.065(2) Uani 0.605(2) 1 d D U P B 1
O1B O 0.4761(10) 0.6730(10) 0.2575(11) 0.051(3) Uani 0.395(2) 1 d D U P B 2
O2B O 0.4047(3) 0.8647(6) 0.2387(3) 0.0411(16) Uani 0.395(2) 1 d D U P B 2
O3B O 0.5128(6) 0.8622(12) 0.3193(4) 0.035(2) Uani 0.395(2) 1 d D U P B 2
S1B S 0.46970(10) 0.80994(18) 0.26194(10) 0.0281(5) Uani 0.395(2) 1 d D U P B 2
C1B C 0.5076(4) 0.8649(7) 0.2045(4) 0.0393(15) Uani 0.395(2) 1 d D U P B 2
F1B F 0.5054(3) 0.9891(5) 0.1983(3) 0.0537(14) Uani 0.395(2) 1 d D U P B 2
F2B F 0.4765(3) 0.8153(6) 0.1486(2) 0.0688(17) Uani 0.395(2) 1 d D U P B 2
F3B F 0.5679(5) 0.8268(14) 0.2163(5) 0.057(2) Uani 0.395(2) 1 d D U P B 2
C1' C -0.0007(5) 0.4168(8) 0.4874(4) 0.045(2) Uani 0.5 1 d D U P C -1
C2' C -0.0078(3) 0.4396(7) 0.4260(3) 0.0465(15) Uani 0.5 1 d D U P C -1
H2' H -0.0102 0.3702 0.3984 0.056 Uiso 0.5 1 calc R U P C -1
C3' C -0.0115(3) 0.5621(7) 0.4038(4) 0.0546(17) Uani 0.5 1 d D U P C -1
H3' H -0.0167 0.5773 0.3611 0.066 Uiso 0.5 1 calc R U P C -1
C4' C -0.0077(3) 0.6615(8) 0.4435(4) 0.0504(16) Uani 0.5 1 d D U P C -1
H4' H -0.0093 0.7463 0.4286 0.060 Uiso 0.5 1 calc R U P C -1
C5' C -0.0013(5) 0.6391(9) 0.5056(4) 0.054(2) Uani 0.5 1 d D U P C -1
H5' H 0.0006 0.7093 0.5327 0.065 Uiso 0.5 1 calc R U P C -1
C6' C 0.0022(3) 0.5146(7) 0.5294(4) 0.0489(18) Uani 0.5 1 d D U P C -1
H6' H 0.0064 0.4986 0.5720 0.059 Uiso 0.5 1 calc R U P C -1
C7' C 0.0052(4) 0.2828(8) 0.5113(4) 0.0503(19) Uani 0.5 1 d D U P C -1
H7'A H -0.0122 0.2241 0.4764 0.075 Uiso 0.5 1 calc R U P C -1
H7'B H -0.0197 0.2736 0.5411 0.075 Uiso 0.5 1 calc R U P C -1
H7'C H 0.0515 0.2630 0.5320 0.075 Uiso 0.5 1 calc R U P C -1
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Co1 C1 1.891(2) . ?
Co1 C29 2.053(2) . ?
Co1 C30 2.112(2) . ?
Co1 C34 2.164(2) . ?
Co1 C31 2.182(2) . ?
Co1 C33 2.192(2) . ?
Co1 C32 2.231(2) . ?
Co1 Co2 2.4610(6) . ?
Co2 C21 1.920(2) . ?
Co2 C9 2.061(2) . ?
Co2 C14 2.128(2) . ?
Co2 C10 2.170(3) . ?
Co2 C13 2.206(2) . ?
Co2 C11 2.211(3) . ?
Co2 C12 2.251(3) . ?
N1 C1 1.338(3) . ?
N1 C9 1.439(3) . ?
N1 C4 1.514(3) . ?
N2 C21 1.328(3) . ?
N2 C29 1.449(3) . ?
N2 C24 1.518(3) . ?
C1 C2 1.550(3) . ?
C2 C5 1.538(3) . ?
C2 C6 1.540(3) . ?
C2 C3 1.550(3) . ?
C3 C4 1.528(4) . ?
C4 C8 1.522(4) . ?
C4 C7 1.535(4) . ?
C9 C14 1.431(3) . ?
C9 C10 1.440(3) . ?
C10 C11 1.399(4) . ?
C10 C15 1.531(3) . ?
C11 C12 1.404(4) . ?
C12 C13 1.397(4) . ?
C13 C14 1.410(4) . ?
C14 C18 1.516(3) . ?
C15 C16 1.526(4) . ?
C15 C17 1.536(4) . ?
C18 C20 1.529(4) . ?
C18 C19 1.538(4) . ?
C24 C23 1.523(4) . ?
C24 C27 1.523(4) . ?
C24 C28 1.536(4) . ?
C23 C22 1.547(4) . ?
C22 C25 1.536(4) . ?
C22 C26 1.544(3) . ?
C22 C21 1.545(3) . ?
C29 C30 1.429(3) . ?
C29 C34 1.430(3) . ?
C30 C31 1.406(3) . ?
C30 C35 1.523(3) . ?
C31 C32 1.401(3) . ?
C32 C33 1.402(4) . ?
C33 C34 1.409(3) . ?
C34 C38 1.522(3) . ?
C35 C36 1.528(4) . ?
C35 C37 1.539(4) . ?
C38 C39 1.525(4) . ?
C38 C40 1.535(3) . ?
C41 C42 1.386(5) . ?
C41 C46 1.389(5) . ?
C41 C47 1.502(5) . ?
C42 C43 1.385(5) . ?
C43 C44 1.379(5) . ?
C44 C45 1.388(5) . ?
C45 C46 1.375(5) . ?
C41' C46' 1.378(14) . ?
C41' C42' 1.389(14) . ?
C41' C47' 1.497(16) . ?
C42' C43' 1.385(14) . ?
C43' C44' 1.382(14) . ?
C44' C45' 1.383(14) . ?
C45' C46' 1.382(14) . ?
O1A S1A 1.440(6) . ?
O2A S1A 1.426(4) . ?
O3A S1A 1.426(7) . ?
S1A C1A 1.828(5) . ?
C1A F3A 1.310(9) . ?
C1A F1A 1.313(6) . ?
C1A F2A 1.326(6) . ?
O1B S1B 1.452(11) . ?
O2B S1B 1.448(6) . ?
O3B S1B 1.449(8) . ?
S1B C1B 1.817(7) . ?
C1B F3B 1.298(10) . ?
C1B F1B 1.313(8) . ?
C1B F2B 1.339(8) . ?
C1' C2' 1.366(9) . ?
C1' C6' 1.387(9) . ?
C1' C7' 1.499(10) . ?
C2' C3' 1.376(8) . ?
C3' C4' 1.361(9) . ?
C4' C5' 1.384(9) . ?
C5' C6' 1.408(10) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C1 Co1 C29 166.02(9) . . ?
C1 Co1 C30 128.97(10) . . ?
C29 Co1 C30 40.10(10) . . ?
C1 Co1 C34 154.38(9) . . ?
C29 Co1 C34 39.55(9) . . ?
C30 Co1 C34 71.82(9) . . ?
C1 Co1 C31 106.39(10) . . ?
C29 Co1 C31 69.30(9) . . ?
C30 Co1 C31 38.18(9) . . ?
C34 Co1 C31 81.16(9) . . ?
C1 Co1 C33 121.89(10) . . ?
C29 Co1 C33 69.58(9) . . ?
C30 Co1 C33 82.85(9) . . ?
C34 Co1 C33 37.73(9) . . ?
C31 Co1 C33 67.24(9) . . ?
C1 Co1 C32 103.24(10) . . ?
C29 Co1 C32 81.42(9) . . ?
C30 Co1 C32 68.96(9) . . ?
C34 Co1 C32 67.76(9) . . ?
C31 Co1 C32 36.99(9) . . ?
C33 Co1 C32 36.94(9) . . ?
C1 Co1 Co2 91.06(7) . . ?
C29 Co1 Co2 86.03(7) . . ?
C30 Co1 Co2 106.47(7) . . ?
C34 Co1 Co2 96.84(7) . . ?
C31 Co1 Co2 143.61(7) . . ?
C33 Co1 Co2 129.36(7) . . ?
C32 Co1 Co2 164.58(7) . . ?
C21 Co2 C9 165.03(10) . . ?
C21 Co2 C14 128.18(10) . . ?
C9 Co2 C14 39.92(9) . . ?
C21 Co2 C10 155.12(10) . . ?
C9 Co2 C10 39.70(9) . . ?
C14 Co2 C10 71.38(9) . . ?
C21 Co2 C13 106.25(10) . . ?
C9 Co2 C13 68.83(10) . . ?
C14 Co2 C13 37.91(9) . . ?
C10 Co2 C13 80.05(10) . . ?
C21 Co2 C11 122.45(10) . . ?
C9 Co2 C11 69.55(10) . . ?
C14 Co2 C11 82.42(10) . . ?
C10 Co2 C11 37.24(9) . . ?
C13 Co2 C11 66.57(10) . . ?
C21 Co2 C12 103.57(10) . . ?
C9 Co2 C12 81.01(10) . . ?
C14 Co2 C12 68.40(10) . . ?
C10 Co2 C12 66.86(10) . . ?
C13 Co2 C12 36.51(9) . . ?
C11 Co2 C12 36.67(9) . . ?
C21 Co2 Co1 91.25(7) . . ?
C9 Co2 Co1 86.10(7) . . ?
C14 Co2 Co1 106.92(7) . . ?
C10 Co2 Co1 97.24(7) . . ?
C13 Co2 Co1 143.97(7) . . ?
C11 Co2 Co1 129.16(7) . . ?
C12 Co2 Co1 164.09(7) . . ?
C1 N1 C9 116.8(2) . . ?
C1 N1 C4 116.5(2) . . ?
C9 N1 C4 125.9(2) . . ?
C21 N2 C29 116.9(2) . . ?
C21 N2 C24 117.0(2) . . ?
C29 N2 C24 125.18(19) . . ?
N1 C1 C2 106.4(2) . . ?
N1 C1 Co1 123.59(18) . . ?
C2 C1 Co1 129.87(17) . . ?
C5 C2 C6 109.3(2) . . ?
C5 C2 C3 111.2(2) . . ?
C6 C2 C3 109.4(2) . . ?
C5 C2 C1 113.5(2) . . ?
C6 C2 C1 109.63(19) . . ?
C3 C2 C1 103.68(19) . . ?
C4 C3 C2 106.6(2) . . ?
N1 C4 C8 112.0(2) . . ?
N1 C4 C3 99.07(19) . . ?
C8 C4 C3 113.6(2) . . ?
N1 C4 C7 110.3(2) . . ?
C8 C4 C7 110.2(2) . . ?
C3 C4 C7 111.3(2) . . ?
C14 C9 N1 122.1(2) . . ?
C14 C9 C10 121.7(2) . . ?
N1 C9 C10 115.8(2) . . ?
C14 C9 Co2 72.57(14) . . ?
N1 C9 Co2 118.96(16) . . ?
C10 C9 Co2 74.22(14) . . ?
C11 C10 C9 118.4(2) . . ?
C11 C10 C15 118.6(2) . . ?
C9 C10 C15 122.7(2) . . ?
C11 C10 Co2 73.00(15) . . ?
C9 C10 Co2 66.07(13) . . ?
C15 C10 Co2 138.44(17) . . ?
C10 C11 C12 120.7(2) . . ?
C10 C11 Co2 69.76(14) . . ?
C12 C11 Co2 73.20(15) . . ?
C13 C12 C11 119.9(2) . . ?
C13 C12 Co2 69.99(14) . . ?
C11 C12 Co2 70.13(14) . . ?
C12 C13 C14 122.7(2) . . ?
C12 C13 Co2 73.50(15) . . ?
C14 C13 Co2 68.04(14) . . ?
C13 C14 C9 116.4(2) . . ?
C13 C14 C18 119.3(2) . . ?
C9 C14 C18 124.2(2) . . ?
C13 C14 Co2 74.05(15) . . ?
C9 C14 Co2 67.51(13) . . ?
C18 C14 Co2 131.83(17) . . ?
C16 C15 C10 114.0(2) . . ?
C16 C15 C17 110.2(2) . . ?
C10 C15 C17 108.7(2) . . ?
C14 C18 C20 113.3(2) . . ?
C14 C18 C19 109.4(2) . . ?
C20 C18 C19 109.6(2) . . ?
N2 C24 C23 99.0(2) . . ?
N2 C24 C27 112.0(2) . . ?
C23 C24 C27 113.9(2) . . ?
N2 C24 C28 111.1(2) . . ?
C23 C24 C28 111.3(2) . . ?
C27 C24 C28 109.3(2) . . ?
C24 C23 C22 107.3(2) . . ?
C25 C22 C26 109.0(2) . . ?
C25 C22 C21 110.5(2) . . ?
C26 C22 C21 112.1(2) . . ?
C25 C22 C23 109.1(2) . . ?
C26 C22 C23 112.5(2) . . ?
C21 C22 C23 103.5(2) . . ?
N2 C21 C22 106.7(2) . . ?
N2 C21 Co2 123.22(18) . . ?
C22 C21 Co2 129.96(18) . . ?
C30 C29 C34 122.6(2) . . ?
C30 C29 N2 121.4(2) . . ?
C34 C29 N2 115.5(2) . . ?
C30 C29 Co1 72.21(14) . . ?
C34 C29 Co1 74.43(14) . . ?
N2 C29 Co1 119.92(16) . . ?
C31 C30 C29 116.4(2) . . ?
C31 C30 C35 119.4(2) . . ?
C29 C30 C35 124.2(2) . . ?
C31 C30 Co1 73.58(14) . . ?
C29 C30 Co1 67.69(13) . . ?
C35 C30 Co1 130.86(18) . . ?
C32 C31 C30 122.5(2) . . ?
C32 C31 Co1 73.42(14) . . ?
C30 C31 Co1 68.24(14) . . ?
C31 C32 C33 119.6(2) . . ?
C31 C32 Co1 69.59(14) . . ?
C33 C32 Co1 70.01(14) . . ?
C32 C33 C34 121.4(2) . . ?
C32 C33 Co1 73.05(14) . . ?
C34 C33 Co1 70.06(13) . . ?
C33 C34 C29 117.3(2) . . ?
C33 C34 C38 118.8(2) . . ?
C29 C34 C38 123.8(2) . . ?
C33 C34 Co1 72.20(14) . . ?
C29 C34 Co1 66.02(13) . . ?
C38 C34 Co1 136.98(17) . . ?
C30 C35 C36 112.5(2) . . ?
C30 C35 C37 109.5(2) . . ?
C36 C35 C37 109.6(2) . . ?
C34 C38 C39 114.1(2) . . ?
C34 C38 C40 108.0(2) . . ?
C39 C38 C40 110.2(2) . . ?
C42 C41 C46 118.1(3) . . ?
C42 C41 C47 121.1(3) . . ?
C46 C41 C47 120.8(3) . . ?
C43 C42 C41 120.9(3) . . ?
C44 C43 C42 120.5(3) . . ?
C43 C44 C45 118.9(3) . . ?
C46 C45 C44 120.5(3) . . ?
C45 C46 C41 121.1(3) . . ?
C46' C41' C42' 119.7(16) . . ?
C46' C41' C47' 121.3(18) . . ?
C42' C41' C47' 119.0(18) . . ?
C43' C42' C41' 120.2(17) . . ?
C44' C43' C42' 119.7(18) . . ?
C43' C44' C45' 119.9(18) . . ?
C46' C45' C44' 120.0(18) . . ?
C41' C46' C45' 120.1(17) . . ?
O3A S1A O2A 114.0(5) . . ?
O3A S1A O1A 112.8(5) . . ?
O2A S1A O1A 118.1(5) . . ?
O3A S1A C1A 103.7(3) . . ?
O2A S1A C1A 101.8(3) . . ?
O1A S1A C1A 104.0(5) . . ?
F3A C1A F1A 106.9(7) . . ?
F3A C1A F2A 104.9(7) . . ?
F1A C1A F2A 109.8(5) . . ?
F3A C1A S1A 111.9(6) . . ?
F1A C1A S1A 112.8(4) . . ?
F2A C1A S1A 110.3(4) . . ?
O2B S1B O3B 116.9(7) . . ?
O2B S1B O1B 118.0(8) . . ?
O3B S1B O1B 112.9(10) . . ?
O2B S1B C1B 101.7(4) . . ?
O3B S1B C1B 102.4(5) . . ?
O1B S1B C1B 101.2(9) . . ?
F3B C1B F1B 109.3(9) . . ?
F3B C1B F2B 104.7(8) . . ?
F1B C1B F2B 107.2(7) . . ?
F3B C1B S1B 112.6(7) . . ?
F1B C1B S1B 112.4(5) . . ?
F2B C1B S1B 110.2(5) . . ?
C2' C1' C6' 122.0(9) . . ?
C2' C1' C7' 119.9(8) . . ?
C6' C1' C7' 118.1(8) . . ?
C1' C2' C3' 120.6(8) . . ?
C4' C3' C2' 119.6(7) . . ?
C3' C4' C5' 120.1(8) . . ?
C4' C5' C6' 121.4(9) . . ?
C1' C6' C5' 116.3(9) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 N1 C1 C2 160.2(2) . . . . ?
C4 N1 C1 C2 -10.2(3) . . . . ?
C9 N1 C1 Co1 -23.2(3) . . . . ?
C4 N1 C1 Co1 166.39(17) . . . . ?
C29 Co1 C1 N1 -61.6(5) . . . . ?
C30 Co1 C1 N1 -96.2(2) . . . . ?
C34 Co1 C1 N1 124.5(2) . . . . ?
C31 Co1 C1 N1 -131.47(19) . . . . ?
C33 Co1 C1 N1 155.50(18) . . . . ?
C32 Co1 C1 N1 -169.65(19) . . . . ?
Co2 Co1 C1 N1 16.16(19) . . . . ?
C29 Co1 C1 C2 114.2(4) . . . . ?
C30 Co1 C1 C2 79.6(2) . . . . ?
C34 Co1 C1 C2 -59.8(3) . . . . ?
C31 Co1 C1 C2 44.3(2) . . . . ?
C33 Co1 C1 C2 -28.7(2) . . . . ?
C32 Co1 C1 C2 6.1(2) . . . . ?
Co2 Co1 C1 C2 -168.1(2) . . . . ?
N1 C1 C2 C5 112.4(2) . . . . ?
Co1 C1 C2 C5 -63.9(3) . . . . ?
N1 C1 C2 C6 -125.1(2) . . . . ?
Co1 C1 C2 C6 58.6(3) . . . . ?
N1 C1 C2 C3 -8.4(2) . . . . ?
Co1 C1 C2 C3 175.32(18) . . . . ?
C5 C2 C3 C4 -99.3(2) . . . . ?
C6 C2 C3 C4 139.9(2) . . . . ?
C1 C2 C3 C4 23.0(3) . . . . ?
C1 N1 C4 C8 144.2(2) . . . . ?
C9 N1 C4 C8 -25.2(3) . . . . ?
C1 N1 C4 C3 24.1(3) . . . . ?
C9 N1 C4 C3 -145.4(2) . . . . ?
C1 N1 C4 C7 -92.7(3) . . . . ?
C9 N1 C4 C7 97.8(3) . . . . ?
C2 C3 C4 N1 -27.0(2) . . . . ?
C2 C3 C4 C8 -145.9(2) . . . . ?
C2 C3 C4 C7 89.0(3) . . . . ?
C1 N1 C9 C14 103.5(3) . . . . ?
C4 N1 C9 C14 -87.1(3) . . . . ?
C1 N1 C9 C10 -68.8(3) . . . . ?
C4 N1 C9 C10 100.6(3) . . . . ?
C1 N1 C9 Co2 16.7(3) . . . . ?
C4 N1 C9 Co2 -173.84(18) . . . . ?
C14 C9 C10 C11 -4.5(4) . . . . ?
N1 C9 C10 C11 167.8(2) . . . . ?
Co2 C9 C10 C11 52.8(2) . . . . ?
C14 C9 C10 C15 169.2(2) . . . . ?
N1 C9 C10 C15 -18.5(3) . . . . ?
Co2 C9 C10 C15 -133.5(2) . . . . ?
C14 C9 C10 Co2 -57.3(2) . . . . ?
N1 C9 C10 Co2 115.0(2) . . . . ?
C9 C10 C11 C12 5.2(4) . . . . ?
C15 C10 C11 C12 -168.8(2) . . . . ?
Co2 C10 C11 C12 54.8(2) . . . . ?
C9 C10 C11 Co2 -49.6(2) . . . . ?
C15 C10 C11 Co2 136.4(2) . . . . ?
C10 C11 C12 C13 -2.0(4) . . . . ?
Co2 C11 C12 C13 51.2(2) . . . . ?
C10 C11 C12 Co2 -53.2(2) . . . . ?
C11 C12 C13 C14 -2.1(4) . . . . ?
Co2 C12 C13 C14 49.1(2) . . . . ?
C11 C12 C13 Co2 -51.2(2) . . . . ?
C12 C13 C14 C9 2.7(4) . . . . ?
Co2 C13 C14 C9 54.13(19) . . . . ?
C12 C13 C14 C18 179.2(2) . . . . ?
Co2 C13 C14 C18 -129.4(2) . . . . ?
C12 C13 C14 Co2 -51.4(2) . . . . ?
N1 C9 C14 C13 -171.2(2) . . . . ?
C10 C9 C14 C13 0.6(3) . . . . ?
Co2 C9 C14 C13 -57.5(2) . . . . ?
N1 C9 C14 C18 12.5(4) . . . . ?
C10 C9 C14 C18 -175.6(2) . . . . ?
Co2 C9 C14 C18 126.3(2) . . . . ?
N1 C9 C14 Co2 -113.7(2) . . . . ?
C10 C9 C14 Co2 58.1(2) . . . . ?
C11 C10 C15 C16 -64.1(3) . . . . ?
C9 C10 C15 C16 122.2(3) . . . . ?
Co2 C10 C15 C16 32.3(4) . . . . ?
C11 C10 C15 C17 59.3(3) . . . . ?
C9 C10 C15 C17 -114.4(3) . . . . ?
Co2 C10 C15 C17 155.8(2) . . . . ?
C13 C14 C18 C20 43.0(3) . . . . ?
C9 C14 C18 C20 -140.8(2) . . . . ?
Co2 C14 C18 C20 -51.5(3) . . . . ?
C13 C14 C18 C19 -79.6(3) . . . . ?
C9 C14 C18 C19 96.6(3) . . . . ?
Co2 C14 C18 C19 -174.10(19) . . . . ?
C21 N2 C24 C23 20.4(3) . . . . ?
C29 N2 C24 C23 -148.2(2) . . . . ?
C21 N2 C24 C27 140.8(2) . . . . ?
C29 N2 C24 C27 -27.8(3) . . . . ?
C21 N2 C24 C28 -96.6(3) . . . . ?
C29 N2 C24 C28 94.7(3) . . . . ?
N2 C24 C23 C22 -24.8(2) . . . . ?
C27 C24 C23 C22 -143.7(2) . . . . ?
C28 C24 C23 C22 92.2(3) . . . . ?
C24 C23 C22 C25 140.2(2) . . . . ?
C24 C23 C22 C26 -98.7(2) . . . . ?
C24 C23 C22 C21 22.5(3) . . . . ?
C29 N2 C21 C22 162.74(19) . . . . ?
C24 N2 C21 C22 -6.9(3) . . . . ?
C29 N2 C21 Co2 -20.4(3) . . . . ?
C24 N2 C21 Co2 170.04(16) . . . . ?
C25 C22 C21 N2 -126.5(2) . . . . ?
C26 C22 C21 N2 111.6(2) . . . . ?
C23 C22 C21 N2 -9.9(3) . . . . ?
C25 C22 C21 Co2 56.9(3) . . . . ?
C26 C22 C21 Co2 -65.0(3) . . . . ?
C23 C22 C21 Co2 173.51(18) . . . . ?
C21 N2 C29 C30 102.1(3) . . . . ?
C24 N2 C29 C30 -89.3(3) . . . . ?
C21 N2 C29 C34 -70.5(3) . . . . ?
C24 N2 C29 C34 98.2(3) . . . . ?
C21 N2 C29 Co1 15.6(3) . . . . ?
C24 N2 C29 Co1 -175.75(17) . . . . ?
C34 C29 C30 C31 0.3(3) . . . . ?
N2 C29 C30 C31 -171.7(2) . . . . ?
Co1 C29 C30 C31 -57.0(2) . . . . ?
C34 C29 C30 C35 -177.5(2) . . . . ?
N2 C29 C30 C35 10.5(4) . . . . ?
Co1 C29 C30 C35 125.2(2) . . . . ?
C34 C29 C30 Co1 57.3(2) . . . . ?
N2 C29 C30 Co1 -114.7(2) . . . . ?
C29 C30 C31 C32 2.2(4) . . . . ?
C35 C30 C31 C32 -179.8(2) . . . . ?
Co1 C30 C31 C32 -51.8(2) . . . . ?
C29 C30 C31 Co1 53.96(19) . . . . ?
C35 C30 C31 Co1 -128.1(2) . . . . ?
C30 C31 C32 C33 -1.3(4) . . . . ?
Co1 C31 C32 C33 -50.9(2) . . . . ?
C30 C31 C32 Co1 49.6(2) . . . . ?
C31 C32 C33 C34 -2.2(4) . . . . ?
Co1 C32 C33 C34 -52.9(2) . . . . ?
C31 C32 C33 Co1 50.7(2) . . . . ?
C32 C33 C34 C29 4.5(3) . . . . ?
Co1 C33 C34 C29 -49.78(19) . . . . ?
C32 C33 C34 C38 -171.4(2) . . . . ?
Co1 C33 C34 C38 134.4(2) . . . . ?
C32 C33 C34 Co1 54.2(2) . . . . ?
C30 C29 C34 C33 -3.6(3) . . . . ?
N2 C29 C34 C33 168.9(2) . . . . ?
Co1 C29 C34 C33 52.7(2) . . . . ?
C30 C29 C34 C38 172.0(2) . . . . ?
N2 C29 C34 C38 -15.6(3) . . . . ?
Co1 C29 C34 C38 -131.7(2) . . . . ?
C30 C29 C34 Co1 -56.3(2) . . . . ?
N2 C29 C34 Co1 116.2(2) . . . . ?
C31 C30 C35 C36 46.1(3) . . . . ?
C29 C30 C35 C36 -136.1(3) . . . . ?
Co1 C30 C35 C36 -47.2(3) . . . . ?
C31 C30 C35 C37 -76.1(3) . . . . ?
C29 C30 C35 C37 101.7(3) . . . . ?
Co1 C30 C35 C37 -169.4(2) . . . . ?
C33 C34 C38 C39 -64.5(3) . . . . ?
C29 C34 C38 C39 120.0(3) . . . . ?
Co1 C34 C38 C39 30.0(3) . . . . ?
C33 C34 C38 C40 58.4(3) . . . . ?
C29 C34 C38 C40 -117.1(3) . . . . ?
Co1 C34 C38 C40 152.9(2) . . . . ?
C46 C41 C42 C43 -1.0(5) . . . . ?
C47 C41 C42 C43 179.0(4) . . . . ?
C41 C42 C43 C44 1.0(5) . . . . ?
C42 C43 C44 C45 -1.2(5) . . . . ?
C43 C44 C45 C46 1.5(5) . . . . ?
C44 C45 C46 C41 -1.5(5) . . . . ?
C42 C41 C46 C45 1.2(5) . . . . ?
C47 C41 C46 C45 -178.8(4) . . . . ?
C46' C41' C42' C43' 0(3) . . . . ?
C47' C41' C42' C43' 178(4) . . . . ?
C41' C42' C43' C44' -2(3) . . . . ?
C42' C43' C44' C45' 7(5) . . . . ?
C43' C44' C45' C46' -9(7) . . . . ?
C42' C41' C46' C45' -2(5) . . . . ?
C47' C41' C46' C45' -180(5) . . . . ?
C44' C45' C46' C41' 6(7) . . . . ?
O3A S1A C1A F3A -58.1(8) . . . . ?
O2A S1A C1A F3A -176.7(8) . . . . ?
O1A S1A C1A F3A 60.0(8) . . . . ?
O3A S1A C1A F1A -178.6(5) . . . . ?
O2A S1A C1A F1A 62.8(5) . . . . ?
O1A S1A C1A F1A -60.5(5) . . . . ?
O3A S1A C1A F2A 58.2(6) . . . . ?
O2A S1A C1A F2A -60.4(5) . . . . ?
O1A S1A C1A F2A 176.4(6) . . . . ?
O2B S1B C1B F3B 179.6(8) . . . . ?
O3B S1B C1B F3B 58.3(10) . . . . ?
O1B S1B C1B F3B -58.4(12) . . . . ?
O2B S1B C1B F1B 55.6(7) . . . . ?
O3B S1B C1B F1B -65.6(8) . . . . ?
O1B S1B C1B F1B 177.6(10) . . . . ?
O2B S1B C1B F2B -63.9(6) . . . . ?
O3B S1B C1B F2B 174.8(7) . . . . ?
O1B S1B C1B F2B 58.1(10) . . . . ?
C6' C1' C2' C3' 0.8(12) . . . . ?
C7' C1' C2' C3' -178.2(7) . . . . ?
C1' C2' C3' C4' 0.4(10) . . . . ?
C2' C3' C4' C5' -1.2(10) . . . . ?
C3' C4' C5' C6' 1.0(13) . . . . ?
C2' C1' C6' C5' -1.1(15) . . . . ?
C7' C1' C6' C5' 178.0(7) . . . . ?
C4' C5' C6' C1' 0.2(15) . . . . ?
 
_refine_diff_density_max    0.346
_refine_diff_density_min   -0.357
_refine_diff_density_rms    0.059

_shelxl_version_number 2013-4



 
data_twin5
 
_audit_creation_method            SHELXL-2012
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          '(C40 H62 Cl Co N2) (c7 H8)'
_chemical_formula_sum
 'C47 H70 Cl Co N2' 
_chemical_formula_weight          757.43

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.683(2)
_cell_length_b                    11.794(2)
_cell_length_c                    19.932(2)
_cell_angle_alpha                 104.34(2)
_cell_angle_beta                  95.28(2)
_cell_angle_gamma                 105.55(2)
_cell_volume                      2093.8(7)
_cell_formula_units_Z             2
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     8428 
_cell_measurement_theta_min       2.216 
_cell_measurement_theta_max       25.302 
 
_exptl_crystal_description        needle 
_exptl_crystal_colour             orange 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.201          
_exptl_crystal_F_000              820
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.07
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.04  
_exptl_absorpt_coefficient_mu     0.507
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.686782  
_exptl_absorpt_correction_T_max   0.745210  
_exptl_absorpt_process_details    'TWINABS-2008/2' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'rotating anode'                       
_diffrn_measurement_device_type   'Smart APEX II Ultra' 
_diffrn_measurement_method        'omega and phi scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             49119
_diffrn_reflns_av_unetI/netI      0.0443
_diffrn_reflns_av_R_equivalents   0.0368
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          1.070
_diffrn_reflns_theta_max          25.390
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              7693
_reflns_number_gt                 6702
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. These statistics refer to single and
 composite reflections containing twin component 1 only.
;
 
_computing_data_collection        'APEX2 v2012.2'
_computing_cell_refinement        'SAINT V7.68A'
_computing_data_reduction         'SAINT V7.68A'
_computing_structure_solution     'SHELXS-2012 (Sheldrick, 2012)'
_computing_structure_refinement   'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics     'XSHELL in SHELXTL-97'
_computing_publication_material   'XSHELL in SHELXTL-97'
 
_refine_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0126P)²+1.6670P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          7693
_refine_ls_number_parameters      478
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0528
_refine_ls_R_factor_gt            0.0392
_refine_ls_wR_factor_ref          0.0736
_refine_ls_wR_factor_gt           0.0688
_refine_ls_goodness_of_fit_ref    1.065
_refine_ls_restrained_S_all       1.065
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Co1 Co 0.57050(4) -0.00106(3) 0.78156(2) 0.01476(8) Uani 1 1 d . . . . .
Cl1 Cl 0.33583(7) -0.07769(6) 0.78872(4) 0.02448(15) Uani 1 1 d . . . . .
N1 N 0.7477(2) 0.26134(17) 0.85864(10) 0.0132(4) Uani 1 1 d . . . . .
N2 N 0.7276(2) -0.15617(16) 0.69072(10) 0.0121(4) Uani 1 1 d . . . . .
C1 C 0.6582(2) 0.1733(2) 0.80457(12) 0.0135(5) Uani 1 1 d . . . . .
C2 C 0.6033(3) 0.2386(2) 0.75446(12) 0.0158(5) Uani 1 1 d . . . . .
C3 C 0.7143(3) 0.3672(2) 0.77578(13) 0.0186(5) Uani 1 1 d . . . . .
H3A H 0.7912 0.3698 0.7462 0.022 Uiso 1 1 calc R U . . .
H3B H 0.6659 0.4292 0.7702 0.022 Uiso 1 1 calc R U . . .
C4 C 0.7798(3) 0.3927(2) 0.85307(13) 0.0174(5) Uani 1 1 d . . . . .
C5 C 0.5895(3) 0.1717(2) 0.67681(13) 0.0213(6) Uani 1 1 d . . . . .
H5A H 0.5505 0.2158 0.6478 0.032 Uiso 1 1 calc R U . . .
H5B H 0.5236 0.0880 0.6665 0.032 Uiso 1 1 calc R U . . .
H5C H 0.6854 0.1683 0.6663 0.032 Uiso 1 1 calc R U . . .
C6 C 0.4513(3) 0.2431(2) 0.76855(14) 0.0221(6) Uani 1 1 d . . . . .
H6A H 0.4121 0.2834 0.7372 0.033 Uiso 1 1 calc R U . . .
H6B H 0.4580 0.2895 0.8175 0.033 Uiso 1 1 calc R U . . .
H6C H 0.3867 0.1594 0.7599 0.033 Uiso 1 1 calc R U . . .
C7 C 0.9417(3) 0.4606(2) 0.86836(14) 0.0250(6) Uani 1 1 d . . . . .
H7A H 0.9569 0.5433 0.8632 0.038 Uiso 1 1 calc R U . . .
H7B H 0.9909 0.4159 0.8352 0.038 Uiso 1 1 calc R U . . .
H7C H 0.9816 0.4661 0.9165 0.038 Uiso 1 1 calc R U . . .
C8 C 0.7091(3) 0.4693(2) 0.90464(14) 0.0241(6) Uani 1 1 d . . . . .
H8A H 0.7302 0.5520 0.8987 0.036 Uiso 1 1 calc R U . . .
H8B H 0.7483 0.4748 0.9529 0.036 Uiso 1 1 calc R U . . .
H8C H 0.6036 0.4303 0.8954 0.036 Uiso 1 1 calc R U . . .
C9 C 0.8021(3) 0.2354(2) 0.92227(12) 0.0150(5) Uani 1 1 d . . . . .
C10 C 0.7142(3) 0.2269(2) 0.97427(13) 0.0162(5) Uani 1 1 d . . . . .
C11 C 0.7677(3) 0.2005(2) 1.03449(13) 0.0214(6) Uani 1 1 d . . . . .
H11 H 0.7100 0.1949 1.0703 0.026 Uiso 1 1 calc R U . . .
C12 C 0.9025(3) 0.1824(2) 1.04291(14) 0.0236(6) Uani 1 1 d . . . . .
H12 H 0.9373 0.1649 1.0842 0.028 Uiso 1 1 calc R U . . .
C13 C 0.9859(3) 0.1899(2) 0.99092(13) 0.0221(6) Uani 1 1 d . . . . .
H13 H 1.0784 0.1770 0.9969 0.026 Uiso 1 1 calc R U . . .
C14 C 0.9391(3) 0.2158(2) 0.92989(13) 0.0180(6) Uani 1 1 d . . . . .
C15 C 0.5617(3) 0.2400(2) 0.96891(13) 0.0178(5) Uani 1 1 d . . . . .
H15 H 0.5391 0.2607 0.9242 0.021 Uiso 1 1 calc R U . . .
C16 C 0.5492(3) 0.3429(2) 1.03051(14) 0.0230(6) Uani 1 1 d . . . . .
H16A H 0.4516 0.3518 1.0238 0.035 Uiso 1 1 calc R U . . .
H16B H 0.6217 0.4202 1.0324 0.035 Uiso 1 1 calc R U . . .
H16C H 0.5665 0.3222 1.0746 0.035 Uiso 1 1 calc R U . . .
C17 C 0.4486(3) 0.1190(2) 0.96668(14) 0.0223(6) Uani 1 1 d . . . . .
H17A H 0.3510 0.1284 0.9613 0.033 Uiso 1 1 calc R U . . .
H17B H 0.4681 0.0980 1.0105 0.033 Uiso 1 1 calc R U . . .
H17C H 0.4545 0.0534 0.9268 0.033 Uiso 1 1 calc R U . . .
C18 C 1.0367(3) 0.2169(2) 0.87433(13) 0.0182(5) Uani 1 1 d . . . . .
H18 H 0.9878 0.2369 0.8343 0.022 Uiso 1 1 calc R U . . .
C19 C 1.0600(3) 0.0915(2) 0.84579(14) 0.0222(6) Uani 1 1 d . . . . .
H19A H 1.1269 0.0969 0.8119 0.033 Uiso 1 1 calc R U . . .
H19B H 0.9665 0.0305 0.8225 0.033 Uiso 1 1 calc R U . . .
H19C H 1.1014 0.0671 0.8847 0.033 Uiso 1 1 calc R U . . .
C20 C 1.1851(3) 0.3147(3) 0.90236(15) 0.0289(7) Uani 1 1 d . . . . .
H20A H 1.2392 0.3209 0.8635 0.043 Uiso 1 1 calc R U . . .
H20B H 1.2402 0.2915 0.9377 0.043 Uiso 1 1 calc R U . . .
H20C H 1.1708 0.3941 0.9237 0.043 Uiso 1 1 calc R U . . .
C21 C 0.6757(2) -0.1161(2) 0.74872(12) 0.0127(5) Uani 1 1 d . . . . .
C22 C 0.6940(3) -0.1979(2) 0.79620(12) 0.0157(5) Uani 1 1 d . . . . .
C23 C 0.8075(3) -0.2568(2) 0.76720(12) 0.0169(5) Uani 1 1 d . . . . .
H23A H 0.9063 -0.2077 0.7930 0.020 Uiso 1 1 calc R U . . .
H23B H 0.7873 -0.3410 0.7720 0.020 Uiso 1 1 calc R U . . .
C24 C 0.7955(3) -0.2597(2) 0.68962(13) 0.0155(5) Uani 1 1 d . . . . .
C25 C 0.5455(3) -0.2940(2) 0.78792(14) 0.0198(5) Uani 1 1 d . . . . .
H25A H 0.5566 -0.3541 0.8126 0.030 Uiso 1 1 calc R U . . .
H25B H 0.5086 -0.3360 0.7379 0.030 Uiso 1 1 calc R U . . .
H25C H 0.4767 -0.2532 0.8079 0.030 Uiso 1 1 calc R U . . .
C26 C 0.7382(3) -0.1262(2) 0.87429(13) 0.0215(6) Uani 1 1 d . . . . .
H26A H 0.7370 -0.1836 0.9025 0.032 Uiso 1 1 calc R U . . .
H26B H 0.6694 -0.0805 0.8878 0.032 Uiso 1 1 calc R U . . .
H26C H 0.8363 -0.0688 0.8824 0.032 Uiso 1 1 calc R U . . .
C27 C 0.9432(3) -0.2350(2) 0.66662(13) 0.0188(6) Uani 1 1 d . . . . .
H27A H 0.9792 -0.3057 0.6646 0.028 Uiso 1 1 calc R U . . .
H27B H 1.0116 -0.1619 0.7004 0.028 Uiso 1 1 calc R U . . .
H27C H 0.9341 -0.2216 0.6200 0.028 Uiso 1 1 calc R U . . .
C28 C 0.6967(3) -0.3816(2) 0.63936(13) 0.0191(6) Uani 1 1 d . . . . .
H28A H 0.7385 -0.4477 0.6423 0.029 Uiso 1 1 calc R U . . .
H28B H 0.6888 -0.3752 0.5912 0.029 Uiso 1 1 calc R U . . .
H28C H 0.5999 -0.3998 0.6526 0.029 Uiso 1 1 calc R U . . .
C29 C 0.7077(3) -0.1156(2) 0.62829(12) 0.0120(5) Uani 1 1 d . . . . .
C30 C 0.5724(3) -0.1661(2) 0.58209(12) 0.0127(5) Uani 1 1 d . . . . .
C31 C 0.5585(3) -0.1294(2) 0.52131(12) 0.0151(5) Uani 1 1 d . . . . .
H31 H 0.4687 -0.1633 0.4896 0.018 Uiso 1 1 calc R U . . .
C32 C 0.6705(3) -0.0454(2) 0.50564(13) 0.0161(5) Uani 1 1 d . . . . .
H32 H 0.6585 -0.0230 0.4633 0.019 Uiso 1 1 calc R U . . .
C33 C 0.8006(3) 0.0059(2) 0.55205(12) 0.0152(5) Uani 1 1 d . . . . .
H33 H 0.8772 0.0650 0.5416 0.018 Uiso 1 1 calc R U . . .
C34 C 0.8223(3) -0.0269(2) 0.61392(12) 0.0137(5) Uani 1 1 d . . . . .
C35 C 0.4399(3) -0.2572(2) 0.59461(12) 0.0147(5) Uani 1 1 d . . . . .
H35 H 0.4668 -0.2778 0.6388 0.018 Uiso 1 1 calc R U . . .
C36 C 0.3139(3) -0.2019(2) 0.60323(13) 0.0186(6) Uani 1 1 d . . . . .
H36A H 0.2320 -0.2602 0.6140 0.028 Uiso 1 1 calc R U . . .
H36B H 0.2832 -0.1847 0.5595 0.028 Uiso 1 1 calc R U . . .
H36C H 0.3459 -0.1254 0.6417 0.028 Uiso 1 1 calc R U . . .
C37 C 0.3879(3) -0.3759(2) 0.53396(14) 0.0204(6) Uani 1 1 d . . . . .
H37A H 0.3097 -0.4358 0.5460 0.031 Uiso 1 1 calc R U . . .
H37B H 0.4692 -0.4094 0.5258 0.031 Uiso 1 1 calc R U . . .
H37C H 0.3515 -0.3584 0.4913 0.031 Uiso 1 1 calc R U . . .
C38 C 0.9665(3) 0.0392(2) 0.66291(13) 0.0152(5) Uani 1 1 d . . . . .
H38 H 0.9692 0.0022 0.7029 0.018 Uiso 1 1 calc R U . . .
C39 C 1.0962(3) 0.0269(2) 0.62587(14) 0.0213(6) Uani 1 1 d . . . . .
H39A H 1.1847 0.0533 0.6610 0.032 Uiso 1 1 calc R U . . .
H39B H 1.1083 0.0784 0.5938 0.032 Uiso 1 1 calc R U . . .
H39C H 1.0782 -0.0590 0.5992 0.032 Uiso 1 1 calc R U . . .
C40 C 0.9821(3) 0.1755(2) 0.69265(14) 0.0199(6) Uani 1 1 d . . . . .
H40A H 1.0771 0.2173 0.7229 0.030 Uiso 1 1 calc R U . . .
H40B H 0.9049 0.1845 0.7202 0.030 Uiso 1 1 calc R U . . .
H40C H 0.9743 0.2122 0.6539 0.030 Uiso 1 1 calc R U . . .
C41 C 1.1555(3) 0.4767(2) 0.66445(14) 0.0199(6) Uani 1 1 d . . . . .
C42 C 1.2703(3) 0.4272(2) 0.66094(14) 0.0207(6) Uani 1 1 d . . . . .
H42 H 1.3442 0.4512 0.7010 0.025 Uiso 1 1 calc R U . . .
C43 C 1.2795(3) 0.3437(2) 0.60057(14) 0.0242(6) Uani 1 1 d . . . . .
H43 H 1.3592 0.3110 0.5995 0.029 Uiso 1 1 calc R U . . .
C44 C 1.1734(3) 0.3074(2) 0.54148(14) 0.0240(6) Uani 1 1 d . . . . .
H44 H 1.1796 0.2496 0.5000 0.029 Uiso 1 1 calc R U . . .
C45 C 1.0586(3) 0.3562(2) 0.54351(14) 0.0251(6) Uani 1 1 d . . . . .
H45 H 0.9859 0.3324 0.5030 0.030 Uiso 1 1 calc R U . . .
C46 C 1.0486(3) 0.4397(2) 0.60440(14) 0.0232(6) Uani 1 1 d . . . . .
H46 H 0.9686 0.4720 0.6053 0.028 Uiso 1 1 calc R U . . .
C47 C 1.1459(3) 0.5667(2) 0.73103(14) 0.0275(6) Uani 1 1 d . . . . .
H47A H 1.0436 0.5547 0.7359 0.041 Uiso 1 1 calc R U . . .
H47B H 1.1899 0.6506 0.7289 0.041 Uiso 1 1 calc R U . . .
H47C H 1.1979 0.5533 0.7715 0.041 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Co1 C1 1.920(2) . ?
Co1 C21 1.932(2) . ?
Co1 Cl1 2.2413(9) . ?
N1 C1 1.335(3) . ?
N1 C9 1.461(3) . ?
N1 C4 1.531(3) . ?
N2 C21 1.333(3) . ?
N2 C29 1.455(3) . ?
N2 C24 1.530(3) . ?
C1 C2 1.541(3) . ?
C2 C5 1.529(3) . ?
C2 C6 1.536(4) . ?
C2 C3 1.536(3) . ?
C3 C4 1.534(3) . ?
C4 C7 1.519(4) . ?
C4 C8 1.531(3) . ?
C9 C10 1.406(3) . ?
C9 C14 1.407(3) . ?
C10 C11 1.402(4) . ?
C10 C15 1.522(3) . ?
C11 C12 1.380(4) . ?
C12 C13 1.377(4) . ?
C13 C14 1.391(4) . ?
C14 C18 1.521(4) . ?
C15 C17 1.536(3) . ?
C15 C16 1.537(3) . ?
C18 C19 1.531(3) . ?
C18 C20 1.534(4) . ?
C21 C22 1.539(3) . ?
C22 C23 1.533(3) . ?
C22 C26 1.533(3) . ?
C22 C25 1.540(3) . ?
C23 C24 1.531(3) . ?
C24 C27 1.518(3) . ?
C24 C28 1.536(3) . ?
C29 C34 1.412(3) . ?
C29 C30 1.416(3) . ?
C30 C31 1.391(3) . ?
C30 C35 1.522(3) . ?
C31 C32 1.377(3) . ?
C32 C33 1.382(3) . ?
C33 C34 1.395(3) . ?
C34 C38 1.516(3) . ?
C35 C37 1.532(3) . ?
C35 C36 1.534(3) . ?
C38 C40 1.531(3) . ?
C38 C39 1.535(3) . ?
C41 C42 1.388(4) . ?
C41 C46 1.402(4) . ?
C41 C47 1.508(4) . ?
C42 C43 1.380(4) . ?
C43 C44 1.385(4) . ?
C44 C45 1.382(4) . ?
C45 C46 1.390(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C1 Co1 C21 122.33(10) . . ?
C1 Co1 Cl1 119.97(7) . . ?
C21 Co1 Cl1 117.66(7) . . ?
C1 N1 C9 121.95(19) . . ?
C1 N1 C4 116.30(19) . . ?
C9 N1 C4 121.55(18) . . ?
C21 N2 C29 122.98(19) . . ?
C21 N2 C24 116.15(19) . . ?
C29 N2 C24 120.52(18) . . ?
N1 C1 C2 106.52(19) . . ?
N1 C1 Co1 136.66(18) . . ?
C2 C1 Co1 116.34(16) . . ?
C5 C2 C6 107.9(2) . . ?
C5 C2 C3 112.4(2) . . ?
C6 C2 C3 111.90(19) . . ?
C5 C2 C1 113.43(19) . . ?
C6 C2 C1 107.0(2) . . ?
C3 C2 C1 104.18(19) . . ?
C4 C3 C2 106.29(19) . . ?
C7 C4 C8 106.8(2) . . ?
C7 C4 N1 112.4(2) . . ?
C8 C4 N1 112.0(2) . . ?
C7 C4 C3 112.0(2) . . ?
C8 C4 C3 113.6(2) . . ?
N1 C4 C3 100.20(17) . . ?
C10 C9 C14 120.9(2) . . ?
C10 C9 N1 119.1(2) . . ?
C14 C9 N1 119.9(2) . . ?
C11 C10 C9 118.2(2) . . ?
C11 C10 C15 117.1(2) . . ?
C9 C10 C15 124.6(2) . . ?
C12 C11 C10 121.4(2) . . ?
C13 C12 C11 119.3(2) . . ?
C12 C13 C14 122.1(3) . . ?
C13 C14 C9 118.0(2) . . ?
C13 C14 C18 118.0(2) . . ?
C9 C14 C18 123.9(2) . . ?
C10 C15 C17 110.8(2) . . ?
C10 C15 C16 111.8(2) . . ?
C17 C15 C16 109.1(2) . . ?
C14 C18 C19 111.9(2) . . ?
C14 C18 C20 111.9(2) . . ?
C19 C18 C20 109.1(2) . . ?
N2 C21 C22 106.64(19) . . ?
N2 C21 Co1 137.39(18) . . ?
C22 C21 Co1 115.54(16) . . ?
C23 C22 C26 113.4(2) . . ?
C23 C22 C21 104.06(19) . . ?
C26 C22 C21 112.83(19) . . ?
C23 C22 C25 111.91(19) . . ?
C26 C22 C25 107.0(2) . . ?
C21 C22 C25 107.63(19) . . ?
C24 C23 C22 106.27(19) . . ?
C27 C24 N2 113.0(2) . . ?
C27 C24 C23 111.7(2) . . ?
N2 C24 C23 100.00(18) . . ?
C27 C24 C28 107.5(2) . . ?
N2 C24 C28 110.89(19) . . ?
C23 C24 C28 113.8(2) . . ?
C34 C29 C30 120.5(2) . . ?
C34 C29 N2 120.2(2) . . ?
C30 C29 N2 119.4(2) . . ?
C31 C30 C29 118.1(2) . . ?
C31 C30 C35 117.4(2) . . ?
C29 C30 C35 124.5(2) . . ?
C32 C31 C30 122.1(2) . . ?
C31 C32 C33 119.3(2) . . ?
C32 C33 C34 121.6(2) . . ?
C33 C34 C29 118.4(2) . . ?
C33 C34 C38 117.4(2) . . ?
C29 C34 C38 124.1(2) . . ?
C30 C35 C37 111.5(2) . . ?
C30 C35 C36 110.95(19) . . ?
C37 C35 C36 108.6(2) . . ?
C34 C38 C40 110.6(2) . . ?
C34 C38 C39 112.0(2) . . ?
C40 C38 C39 108.9(2) . . ?
C42 C41 C46 117.9(2) . . ?
C42 C41 C47 120.9(2) . . ?
C46 C41 C47 121.3(2) . . ?
C43 C42 C41 121.4(2) . . ?
C42 C43 C44 120.4(3) . . ?
C45 C44 C43 119.2(2) . . ?
C44 C45 C46 120.4(2) . . ?
C45 C46 C41 120.6(2) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 N1 C1 C2 169.7(2) . . . . ?
C4 N1 C1 C2 -5.1(3) . . . . ?
C9 N1 C1 Co1 -1.6(4) . . . . ?
C4 N1 C1 Co1 -176.47(19) . . . . ?
N1 C1 C2 C5 141.6(2) . . . . ?
Co1 C1 C2 C5 -45.0(3) . . . . ?
N1 C1 C2 C6 -99.6(2) . . . . ?
Co1 C1 C2 C6 73.8(2) . . . . ?
N1 C1 C2 C3 19.1(2) . . . . ?
Co1 C1 C2 C3 -167.51(15) . . . . ?
C5 C2 C3 C4 -149.1(2) . . . . ?
C6 C2 C3 C4 89.4(2) . . . . ?
C1 C2 C3 C4 -25.9(2) . . . . ?
C1 N1 C4 C7 -130.0(2) . . . . ?
C9 N1 C4 C7 55.1(3) . . . . ?
C1 N1 C4 C8 109.8(2) . . . . ?
C9 N1 C4 C8 -65.1(3) . . . . ?
C1 N1 C4 C3 -10.9(3) . . . . ?
C9 N1 C4 C3 174.2(2) . . . . ?
C2 C3 C4 C7 141.5(2) . . . . ?
C2 C3 C4 C8 -97.5(2) . . . . ?
C2 C3 C4 N1 22.1(2) . . . . ?
C1 N1 C9 C10 -82.3(3) . . . . ?
C4 N1 C9 C10 92.3(3) . . . . ?
C1 N1 C9 C14 95.9(3) . . . . ?
C4 N1 C9 C14 -89.6(3) . . . . ?
C14 C9 C10 C11 1.1(3) . . . . ?
N1 C9 C10 C11 179.2(2) . . . . ?
C14 C9 C10 C15 -176.7(2) . . . . ?
N1 C9 C10 C15 1.5(3) . . . . ?
C9 C10 C11 C12 -0.4(4) . . . . ?
C15 C10 C11 C12 177.5(2) . . . . ?
C10 C11 C12 C13 -0.3(4) . . . . ?
C11 C12 C13 C14 0.3(4) . . . . ?
C12 C13 C14 C9 0.4(4) . . . . ?
C12 C13 C14 C18 -177.5(2) . . . . ?
C10 C9 C14 C13 -1.0(3) . . . . ?
N1 C9 C14 C13 -179.2(2) . . . . ?
C10 C9 C14 C18 176.7(2) . . . . ?
N1 C9 C14 C18 -1.5(3) . . . . ?
C11 C10 C15 C17 -62.7(3) . . . . ?
C9 C10 C15 C17 115.1(3) . . . . ?
C11 C10 C15 C16 59.3(3) . . . . ?
C9 C10 C15 C16 -122.9(3) . . . . ?
C13 C14 C18 C19 61.5(3) . . . . ?
C9 C14 C18 C19 -116.3(3) . . . . ?
C13 C14 C18 C20 -61.3(3) . . . . ?
C9 C14 C18 C20 121.0(3) . . . . ?
C29 N2 C21 C22 169.53(19) . . . . ?
C24 N2 C21 C22 -3.6(3) . . . . ?
C29 N2 C21 Co1 -2.2(4) . . . . ?
C24 N2 C21 Co1 -175.34(19) . . . . ?
N2 C21 C22 C23 18.5(2) . . . . ?
Co1 C21 C22 C23 -167.68(15) . . . . ?
N2 C21 C22 C26 141.8(2) . . . . ?
Co1 C21 C22 C26 -44.4(2) . . . . ?
N2 C21 C22 C25 -100.4(2) . . . . ?
Co1 C21 C22 C25 73.4(2) . . . . ?
C26 C22 C23 C24 -149.3(2) . . . . ?
C21 C22 C23 C24 -26.4(2) . . . . ?
C25 C22 C23 C24 89.5(2) . . . . ?
C21 N2 C24 C27 -131.6(2) . . . . ?
C29 N2 C24 C27 55.1(3) . . . . ?
C21 N2 C24 C23 -12.7(2) . . . . ?
C29 N2 C24 C23 174.02(19) . . . . ?
C21 N2 C24 C28 107.7(2) . . . . ?
C29 N2 C24 C28 -65.6(3) . . . . ?
C22 C23 C24 C27 143.1(2) . . . . ?
C22 C23 C24 N2 23.3(2) . . . . ?
C22 C23 C24 C28 -95.0(2) . . . . ?
C21 N2 C29 C34 101.7(3) . . . . ?
C24 N2 C29 C34 -85.4(3) . . . . ?
C21 N2 C29 C30 -78.4(3) . . . . ?
C24 N2 C29 C30 94.4(3) . . . . ?
C34 C29 C30 C31 2.5(3) . . . . ?
N2 C29 C30 C31 -177.35(19) . . . . ?
C34 C29 C30 C35 -176.8(2) . . . . ?
N2 C29 C30 C35 3.4(3) . . . . ?
C29 C30 C31 C32 -0.8(3) . . . . ?
C35 C30 C31 C32 178.6(2) . . . . ?
C30 C31 C32 C33 -1.1(4) . . . . ?
C31 C32 C33 C34 1.2(3) . . . . ?
C32 C33 C34 C29 0.5(3) . . . . ?
C32 C33 C34 C38 -177.2(2) . . . . ?
C30 C29 C34 C33 -2.3(3) . . . . ?
N2 C29 C34 C33 177.5(2) . . . . ?
C30 C29 C34 C38 175.2(2) . . . . ?
N2 C29 C34 C38 -5.0(3) . . . . ?
C31 C30 C35 C37 58.0(3) . . . . ?
C29 C30 C35 C37 -122.7(2) . . . . ?
C31 C30 C35 C36 -63.2(3) . . . . ?
C29 C30 C35 C36 116.1(2) . . . . ?
C33 C34 C38 C40 65.2(3) . . . . ?
C29 C34 C38 C40 -112.3(2) . . . . ?
C33 C34 C38 C39 -56.4(3) . . . . ?
C29 C34 C38 C39 126.1(2) . . . . ?
C46 C41 C42 C43 -0.3(4) . . . . ?
C47 C41 C42 C43 179.3(2) . . . . ?
C41 C42 C43 C44 0.1(4) . . . . ?
C42 C43 C44 C45 0.3(4) . . . . ?
C43 C44 C45 C46 -0.7(4) . . . . ?
C44 C45 C46 C41 0.6(4) . . . . ?
C42 C41 C46 C45 -0.1(4) . . . . ?
C47 C41 C46 C45 -179.7(2) . . . . ?
 
_refine_diff_density_max    0.298
_refine_diff_density_min   -0.334
_refine_diff_density_rms    0.056

_shelxl_version_number 2012-9



