 
data_sad_a
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C40 H62 Cl2 Fe N2'
_chemical_formula_sum
 'C40 H62 Cl2 Fe N2' 
_chemical_formula_weight          697.66

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'
 'Fe'  'Fe'   0.3463   0.8444
 '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/c'
_space_group_name_Hall            '-P 2ybc'
 
_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+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    13.173(2)
_cell_length_b                    17.403(2)
_cell_length_c                    17.237(2)
_cell_angle_alpha                 90
_cell_angle_beta                  108.58(2)
_cell_angle_gamma                 90
_cell_volume                      3745.6(9)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9978 
_cell_measurement_theta_min       2.341 
_cell_measurement_theta_max       25.903  
 
_exptl_crystal_description        block 
_exptl_crystal_colour             orange  
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.237          
_exptl_crystal_F_000              1504
_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     0.575
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.6894  
_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             107288
_diffrn_reflns_av_unetI/netI      0.0267
_diffrn_reflns_av_R_equivalents   0.0622
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          1.631
_diffrn_reflns_theta_max          26.029
_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   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              7385
_reflns_number_gt                 6136
_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 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)+(0.0325P)²+2.4952P] 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          7385
_refine_ls_number_parameters      422
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0431
_refine_ls_R_factor_gt            0.0317
_refine_ls_wR_factor_ref          0.0764
_refine_ls_wR_factor_gt           0.0715
_refine_ls_goodness_of_fit_ref    1.033
_refine_ls_restrained_S_all       1.033
_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
Fe1 Fe 0.25597(2) 0.37027(2) 0.68275(2) 0.01192(7) Uani 1 1 d . . . . .
Cl1 Cl 0.34513(3) 0.48458(2) 0.69362(3) 0.01842(10) Uani 1 1 d . . . . .
Cl2 Cl 0.14698(3) 0.34593(3) 0.55338(3) 0.01807(10) Uani 1 1 d . . . . .
N1 N 0.47709(10) 0.28085(8) 0.72103(8) 0.0110(3) Uani 1 1 d . . . . .
N2 N 0.05666(11) 0.37573(8) 0.75035(9) 0.0135(3) Uani 1 1 d . . . . .
C1 C 0.37300(13) 0.27998(10) 0.70817(9) 0.0112(3) Uani 1 1 d . . . . .
C2 C 0.33985(13) 0.19507(10) 0.70634(10) 0.0128(3) Uani 1 1 d . . . . .
C3 C 0.44490(13) 0.15228(10) 0.74852(11) 0.0145(4) Uani 1 1 d . . . . .
H3A H 0.4550 0.1455 0.8075 0.017 Uiso 1 1 calc R U . . .
H3B H 0.4444 0.1010 0.7235 0.017 Uiso 1 1 calc R U . . .
C4 C 0.53421(13) 0.20212(9) 0.73646(10) 0.0133(3) Uani 1 1 d . . . . .
C5 C 0.25604(14) 0.17992(10) 0.74853(12) 0.0185(4) Uani 1 1 d . . . . .
H5A H 0.1953 0.2148 0.7265 0.028 Uiso 1 1 calc R U . . .
H5B H 0.2878 0.1886 0.8075 0.028 Uiso 1 1 calc R U . . .
H5C H 0.2312 0.1266 0.7387 0.028 Uiso 1 1 calc R U . . .
C6 C 0.29073(14) 0.17140(10) 0.61556(11) 0.0165(4) Uani 1 1 d . . . . .
H6A H 0.2266 0.2023 0.5899 0.025 Uiso 1 1 calc R U . . .
H6B H 0.2713 0.1168 0.6123 0.025 Uiso 1 1 calc R U . . .
H6C H 0.3432 0.1801 0.5869 0.025 Uiso 1 1 calc R U . . .
C7 C 0.63319(13) 0.20351(10) 0.81208(11) 0.0169(4) Uani 1 1 d . . . . .
H7A H 0.6859 0.2394 0.8033 0.025 Uiso 1 1 calc R U . . .
H7B H 0.6644 0.1519 0.8221 0.025 Uiso 1 1 calc R U . . .
H7C H 0.6131 0.2202 0.8595 0.025 Uiso 1 1 calc R U . . .
C8 C 0.56950(14) 0.17787(10) 0.66380(11) 0.0181(4) Uani 1 1 d . . . . .
H8A H 0.5068 0.1748 0.6145 0.027 Uiso 1 1 calc R U . . .
H8B H 0.6043 0.1275 0.6749 0.027 Uiso 1 1 calc R U . . .
H8C H 0.6201 0.2158 0.6554 0.027 Uiso 1 1 calc R U . . .
C9 C 0.53922(12) 0.34788(9) 0.71153(10) 0.0112(3) Uani 1 1 d . . . . .
C10 C 0.53960(13) 0.36681(10) 0.63230(10) 0.0131(3) Uani 1 1 d . . . . .
C11 C 0.60876(13) 0.42502(10) 0.62474(11) 0.0160(4) Uani 1 1 d . . . . .
H11 H 0.6118 0.4378 0.5719 0.019 Uiso 1 1 calc R U . . .
C12 C 0.67272(14) 0.46446(10) 0.69183(11) 0.0191(4) Uani 1 1 d . . . . .
H12 H 0.7205 0.5030 0.6854 0.023 Uiso 1 1 calc R U . . .
C13 C 0.66686(13) 0.44758(10) 0.76845(11) 0.0165(4) Uani 1 1 d . . . . .
H13 H 0.7091 0.4764 0.8142 0.020 Uiso 1 1 calc R U . . .
C14 C 0.60071(13) 0.38951(10) 0.78074(10) 0.0130(3) Uani 1 1 d . . . . .
C15 C 0.46545(13) 0.33237(10) 0.55324(10) 0.0155(4) Uani 1 1 d . . . . .
H15 H 0.4237 0.2897 0.5675 0.019 Uiso 1 1 calc R U . . .
C16 C 0.38659(15) 0.39381(11) 0.50528(11) 0.0219(4) Uani 1 1 d . . . . .
H16A H 0.4256 0.4331 0.4855 0.033 Uiso 1 1 calc R U . . .
H16B H 0.3509 0.4177 0.5412 0.033 Uiso 1 1 calc R U . . .
H16C H 0.3329 0.3698 0.4586 0.033 Uiso 1 1 calc R U . . .
C17 C 0.52709(15) 0.30000(11) 0.49858(11) 0.0208(4) Uani 1 1 d . . . . .
H17A H 0.4767 0.2757 0.4502 0.031 Uiso 1 1 calc R U . . .
H17B H 0.5791 0.2618 0.5293 0.031 Uiso 1 1 calc R U . . .
H17C H 0.5648 0.3418 0.4813 0.031 Uiso 1 1 calc R U . . .
C18 C 0.59429(13) 0.37943(10) 0.86685(10) 0.0158(4) Uani 1 1 d . . . . .
H18 H 0.5467 0.3346 0.8666 0.019 Uiso 1 1 calc R U . . .
C19 C 0.70391(14) 0.36440(11) 0.93093(11) 0.0216(4) Uani 1 1 d . . . . .
H19A H 0.7373 0.3196 0.9145 0.032 Uiso 1 1 calc R U . . .
H19B H 0.6945 0.3545 0.9842 0.032 Uiso 1 1 calc R U . . .
H19C H 0.7499 0.4095 0.9350 0.032 Uiso 1 1 calc R U . . .
C20 C 0.54514(14) 0.45138(11) 0.89253(11) 0.0200(4) Uani 1 1 d . . . . .
H20A H 0.4767 0.4633 0.8507 0.030 Uiso 1 1 calc R U . . .
H20B H 0.5942 0.4949 0.8983 0.030 Uiso 1 1 calc R U . . .
H20C H 0.5331 0.4418 0.9450 0.030 Uiso 1 1 calc R U . . .
C21 C 0.16082(13) 0.37568(10) 0.76359(10) 0.0134(3) Uani 1 1 d . . . . .
C22 C 0.21517(13) 0.38700(10) 0.85609(11) 0.0160(4) Uani 1 1 d . . . . .
C23 C 0.12756(14) 0.36710(11) 0.89426(11) 0.0196(4) Uani 1 1 d . . . . .
H23A H 0.1338 0.3128 0.9123 0.023 Uiso 1 1 calc R U . . .
H23B H 0.1337 0.4004 0.9421 0.023 Uiso 1 1 calc R U . . .
C24 C 0.02054(14) 0.38077(11) 0.82709(11) 0.0176(4) Uani 1 1 d . . . . .
C25 C 0.31442(14) 0.33692(11) 0.89142(11) 0.0210(4) Uani 1 1 d . . . . .
H25A H 0.3635 0.3445 0.8597 0.031 Uiso 1 1 calc R U . . .
H25B H 0.2931 0.2828 0.8887 0.031 Uiso 1 1 calc R U . . .
H25C H 0.3504 0.3513 0.9486 0.031 Uiso 1 1 calc R U . . .
C26 C 0.24947(14) 0.47221(11) 0.86956(11) 0.0202(4) Uani 1 1 d . . . . .
H26A H 0.2981 0.4842 0.8384 0.030 Uiso 1 1 calc R U . . .
H26B H 0.2861 0.4813 0.9279 0.030 Uiso 1 1 calc R U . . .
H26C H 0.1859 0.5051 0.8509 0.030 Uiso 1 1 calc R U . . .
C27 C -0.02990(14) 0.45866(11) 0.83285(11) 0.0214(4) Uani 1 1 d . . . . .
H27A H -0.0923 0.4666 0.7841 0.032 Uiso 1 1 calc R U . . .
H27B H 0.0227 0.4994 0.8363 0.032 Uiso 1 1 calc R U . . .
H27C H -0.0524 0.4599 0.8818 0.032 Uiso 1 1 calc R U . . .
C28 C -0.06123(15) 0.31868(12) 0.82703(12) 0.0236(4) Uani 1 1 d . . . . .
H28A H -0.1263 0.3267 0.7805 0.035 Uiso 1 1 calc R U . . .
H28B H -0.0788 0.3214 0.8781 0.035 Uiso 1 1 calc R U . . .
H28C H -0.0311 0.2680 0.8225 0.035 Uiso 1 1 calc R U . . .
C29 C -0.02611(13) 0.38103(10) 0.66964(10) 0.0146(4) Uani 1 1 d . . . . .
C30 C -0.08045(13) 0.31488(10) 0.63084(11) 0.0162(4) Uani 1 1 d . . . . .
C31 C -0.16425(14) 0.32477(11) 0.55780(11) 0.0188(4) Uani 1 1 d . . . . .
H31 H -0.2027 0.2809 0.5311 0.023 Uiso 1 1 calc R U . . .
C32 C -0.19301(14) 0.39623(11) 0.52326(11) 0.0188(4) Uani 1 1 d . . . . .
H32 H -0.2511 0.4014 0.4739 0.023 Uiso 1 1 calc R U . . .
C33 C -0.13677(13) 0.46003(11) 0.56088(11) 0.0177(4) Uani 1 1 d . . . . .
H33 H -0.1560 0.5091 0.5365 0.021 Uiso 1 1 calc R U . . .
C34 C -0.05190(13) 0.45417(10) 0.63427(11) 0.0155(4) Uani 1 1 d . . . . .
C35 C -0.05074(14) 0.23290(10) 0.65941(11) 0.0181(4) Uani 1 1 d . . . . .
H35 H 0.0087 0.2346 0.7128 0.022 Uiso 1 1 calc R U . . .
C36 C -0.01128(15) 0.18891(11) 0.59722(12) 0.0222(4) Uani 1 1 d . . . . .
H36A H -0.0713 0.1807 0.5469 0.033 Uiso 1 1 calc R U . . .
H36B H 0.0180 0.1391 0.6204 0.033 Uiso 1 1 calc R U . . .
H36C H 0.0446 0.2188 0.5847 0.033 Uiso 1 1 calc R U . . .
C37 C -0.14547(14) 0.18911(11) 0.67214(12) 0.0230(4) Uani 1 1 d . . . . .
H37A H -0.2033 0.1851 0.6199 0.035 Uiso 1 1 calc R U . . .
H37B H -0.1714 0.2168 0.7116 0.035 Uiso 1 1 calc R U . . .
H37C H -0.1221 0.1375 0.6930 0.035 Uiso 1 1 calc R U . . .
C38 C 0.00898(13) 0.52780(10) 0.66698(11) 0.0164(4) Uani 1 1 d . . . . .
H38 H 0.0605 0.5172 0.7226 0.020 Uiso 1 1 calc R U . . .
C39 C -0.06639(15) 0.59260(11) 0.67406(12) 0.0216(4) Uani 1 1 d . . . . .
H39A H -0.0245 0.6389 0.6955 0.032 Uiso 1 1 calc R U . . .
H39B H -0.1053 0.5768 0.7113 0.032 Uiso 1 1 calc R U . . .
H39C H -0.1176 0.6035 0.6199 0.032 Uiso 1 1 calc R U . . .
C40 C 0.07248(14) 0.55342(11) 0.61123(11) 0.0200(4) Uani 1 1 d . . . . .
H40A H 0.1191 0.5114 0.6054 0.030 Uiso 1 1 calc R U . . .
H40B H 0.1163 0.5982 0.6352 0.030 Uiso 1 1 calc R U . . .
H40C H 0.0228 0.5670 0.5573 0.030 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
Fe1 C1 2.1464(17) . ?
Fe1 C21 2.1529(17) . ?
Fe1 Cl2 2.2745(7) . ?
Fe1 Cl1 2.2873(5) . ?
N1 C1 1.317(2) . ?
N1 C9 1.464(2) . ?
N1 C4 1.545(2) . ?
N2 C21 1.317(2) . ?
N2 C29 1.472(2) . ?
N2 C24 1.544(2) . ?
C1 C2 1.538(2) . ?
C2 C5 1.526(2) . ?
C2 C3 1.535(2) . ?
C2 C6 1.547(2) . ?
C3 C4 1.528(2) . ?
C4 C7 1.522(2) . ?
C4 C8 1.528(2) . ?
C9 C10 1.406(2) . ?
C9 C14 1.410(2) . ?
C10 C11 1.396(2) . ?
C10 C15 1.524(2) . ?
C11 C12 1.377(3) . ?
C12 C13 1.379(3) . ?
C13 C14 1.394(2) . ?
C14 C18 1.524(2) . ?
C15 C17 1.534(2) . ?
C15 C16 1.536(2) . ?
C18 C19 1.535(2) . ?
C18 C20 1.538(2) . ?
C21 C22 1.538(2) . ?
C22 C25 1.527(2) . ?
C22 C23 1.539(2) . ?
C22 C26 1.546(3) . ?
C23 C24 1.531(2) . ?
C24 C28 1.525(3) . ?
C24 C27 1.527(3) . ?
C29 C34 1.405(2) . ?
C29 C30 1.407(2) . ?
C30 C31 1.396(2) . ?
C30 C35 1.519(3) . ?
C31 C32 1.379(3) . ?
C32 C33 1.377(3) . ?
C33 C34 1.400(2) . ?
C34 C38 1.521(2) . ?
C35 C36 1.536(3) . ?
C35 C37 1.536(2) . ?
C38 C40 1.528(2) . ?
C38 C39 1.533(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
C1 Fe1 C21 115.36(6) . . ?
C1 Fe1 Cl2 104.58(5) . . ?
C21 Fe1 Cl2 109.08(5) . . ?
C1 Fe1 Cl1 107.66(5) . . ?
C21 Fe1 Cl1 107.37(5) . . ?
Cl2 Fe1 Cl1 112.92(2) . . ?
C1 N1 C9 125.40(14) . . ?
C1 N1 C4 116.26(13) . . ?
C9 N1 C4 117.84(12) . . ?
C21 N2 C29 125.51(14) . . ?
C21 N2 C24 116.09(14) . . ?
C29 N2 C24 117.93(13) . . ?
N1 C1 C2 106.73(14) . . ?
N1 C1 Fe1 131.86(12) . . ?
C2 C1 Fe1 121.21(11) . . ?
C5 C2 C3 111.74(14) . . ?
C5 C2 C1 113.57(14) . . ?
C3 C2 C1 104.41(13) . . ?
C5 C2 C6 107.66(14) . . ?
C3 C2 C6 111.92(14) . . ?
C1 C2 C6 107.53(13) . . ?
C4 C3 C2 106.09(13) . . ?
C7 C4 C8 107.76(14) . . ?
C7 C4 C3 112.28(14) . . ?
C8 C4 C3 113.78(14) . . ?
C7 C4 N1 111.76(13) . . ?
C8 C4 N1 111.26(13) . . ?
C3 C4 N1 99.96(12) . . ?
C10 C9 C14 121.49(15) . . ?
C10 C9 N1 118.06(14) . . ?
C14 C9 N1 120.38(15) . . ?
C11 C10 C9 117.71(15) . . ?
C11 C10 C15 116.96(15) . . ?
C9 C10 C15 125.22(15) . . ?
C12 C11 C10 121.74(16) . . ?
C11 C12 C13 119.47(16) . . ?
C12 C13 C14 121.90(16) . . ?
C13 C14 C9 117.54(16) . . ?
C13 C14 C18 117.58(15) . . ?
C9 C14 C18 124.74(15) . . ?
C10 C15 C17 112.33(14) . . ?
C10 C15 C16 109.78(15) . . ?
C17 C15 C16 108.95(15) . . ?
C14 C18 C19 112.90(14) . . ?
C14 C18 C20 110.23(14) . . ?
C19 C18 C20 108.50(15) . . ?
N2 C21 C22 107.14(14) . . ?
N2 C21 Fe1 132.61(13) . . ?
C22 C21 Fe1 120.12(11) . . ?
C25 C22 C21 113.39(14) . . ?
C25 C22 C23 111.37(15) . . ?
C21 C22 C23 104.45(14) . . ?
C25 C22 C26 108.38(14) . . ?
C21 C22 C26 107.20(14) . . ?
C23 C22 C26 112.00(15) . . ?
C24 C23 C22 106.08(14) . . ?
C28 C24 C27 107.88(15) . . ?
C28 C24 C23 111.73(15) . . ?
C27 C24 C23 113.81(15) . . ?
C28 C24 N2 111.68(14) . . ?
C27 C24 N2 111.43(14) . . ?
C23 C24 N2 100.26(13) . . ?
C34 C29 C30 121.25(16) . . ?
C34 C29 N2 118.08(15) . . ?
C30 C29 N2 120.62(15) . . ?
C31 C30 C29 117.66(16) . . ?
C31 C30 C35 117.15(16) . . ?
C29 C30 C35 125.08(15) . . ?
C32 C31 C30 122.02(17) . . ?
C33 C32 C31 119.44(16) . . ?
C32 C33 C34 121.46(17) . . ?
C33 C34 C29 118.10(16) . . ?
C33 C34 C38 116.65(16) . . ?
C29 C34 C38 125.17(15) . . ?
C30 C35 C36 110.56(15) . . ?
C30 C35 C37 112.03(15) . . ?
C36 C35 C37 108.86(15) . . ?
C34 C38 C40 110.02(15) . . ?
C34 C38 C39 111.77(14) . . ?
C40 C38 C39 109.50(15) . . ?
 
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 167.32(14) . . . . ?
C4 N1 C1 C2 -4.40(18) . . . . ?
C9 N1 C1 Fe1 -7.5(2) . . . . ?
C4 N1 C1 Fe1 -179.20(11) . . . . ?
N1 C1 C2 C5 140.66(15) . . . . ?
Fe1 C1 C2 C5 -43.87(18) . . . . ?
N1 C1 C2 C3 18.69(17) . . . . ?
Fe1 C1 C2 C3 -165.84(11) . . . . ?
N1 C1 C2 C6 -100.34(15) . . . . ?
Fe1 C1 C2 C6 75.13(15) . . . . ?
C5 C2 C3 C4 -149.04(14) . . . . ?
C1 C2 C3 C4 -25.88(17) . . . . ?
C6 C2 C3 C4 90.14(16) . . . . ?
C2 C3 C4 C7 140.88(14) . . . . ?
C2 C3 C4 C8 -96.39(16) . . . . ?
C2 C3 C4 N1 22.27(16) . . . . ?
C1 N1 C4 C7 -130.59(15) . . . . ?
C9 N1 C4 C7 57.03(19) . . . . ?
C1 N1 C4 C8 108.90(16) . . . . ?
C9 N1 C4 C8 -63.48(18) . . . . ?
C1 N1 C4 C3 -11.60(18) . . . . ?
C9 N1 C4 C3 176.02(13) . . . . ?
C1 N1 C9 C10 -81.4(2) . . . . ?
C4 N1 C9 C10 90.22(18) . . . . ?
C1 N1 C9 C14 101.63(19) . . . . ?
C4 N1 C9 C14 -86.76(18) . . . . ?
C14 C9 C10 C11 4.3(2) . . . . ?
N1 C9 C10 C11 -172.61(14) . . . . ?
C14 C9 C10 C15 -171.58(15) . . . . ?
N1 C9 C10 C15 11.5(2) . . . . ?
C9 C10 C11 C12 -1.7(2) . . . . ?
C15 C10 C11 C12 174.53(16) . . . . ?
C10 C11 C12 C13 -1.6(3) . . . . ?
C11 C12 C13 C14 2.4(3) . . . . ?
C12 C13 C14 C9 0.1(2) . . . . ?
C12 C13 C14 C18 -175.74(16) . . . . ?
C10 C9 C14 C13 -3.5(2) . . . . ?
N1 C9 C14 C13 173.32(14) . . . . ?
C10 C9 C14 C18 171.96(15) . . . . ?
N1 C9 C14 C18 -11.2(2) . . . . ?
C11 C10 C15 C17 56.8(2) . . . . ?
C9 C10 C15 C17 -127.29(17) . . . . ?
C11 C10 C15 C16 -64.63(19) . . . . ?
C9 C10 C15 C16 111.32(18) . . . . ?
C13 C14 C18 C19 -57.6(2) . . . . ?
C9 C14 C18 C19 126.89(17) . . . . ?
C13 C14 C18 C20 63.92(19) . . . . ?
C9 C14 C18 C20 -111.59(18) . . . . ?
C29 N2 C21 C22 167.90(15) . . . . ?
C24 N2 C21 C22 -4.1(2) . . . . ?
C29 N2 C21 Fe1 -7.8(3) . . . . ?
C24 N2 C21 Fe1 -179.77(12) . . . . ?
N2 C21 C22 C25 139.26(16) . . . . ?
Fe1 C21 C22 C25 -44.42(19) . . . . ?
N2 C21 C22 C23 17.84(18) . . . . ?
Fe1 C21 C22 C23 -165.85(11) . . . . ?
N2 C21 C22 C26 -101.16(16) . . . . ?
Fe1 C21 C22 C26 75.15(15) . . . . ?
C25 C22 C23 C24 -147.45(15) . . . . ?
C21 C22 C23 C24 -24.70(18) . . . . ?
C26 C22 C23 C24 90.99(17) . . . . ?
C22 C23 C24 C28 139.83(15) . . . . ?
C22 C23 C24 C27 -97.68(17) . . . . ?
C22 C23 C24 N2 21.39(17) . . . . ?
C21 N2 C24 C28 -129.74(16) . . . . ?
C29 N2 C24 C28 57.6(2) . . . . ?
C21 N2 C24 C27 109.53(17) . . . . ?
C29 N2 C24 C27 -63.10(19) . . . . ?
C21 N2 C24 C23 -11.25(19) . . . . ?
C29 N2 C24 C23 176.11(14) . . . . ?
C21 N2 C29 C34 -81.7(2) . . . . ?
C24 N2 C29 C34 90.13(19) . . . . ?
C21 N2 C29 C30 100.7(2) . . . . ?
C24 N2 C29 C30 -87.44(19) . . . . ?
C34 C29 C30 C31 -2.9(2) . . . . ?
N2 C29 C30 C31 174.60(15) . . . . ?
C34 C29 C30 C35 173.14(16) . . . . ?
N2 C29 C30 C35 -9.4(3) . . . . ?
C29 C30 C31 C32 0.9(3) . . . . ?
C35 C30 C31 C32 -175.42(16) . . . . ?
C30 C31 C32 C33 1.0(3) . . . . ?
C31 C32 C33 C34 -1.0(3) . . . . ?
C32 C33 C34 C29 -0.9(3) . . . . ?
C32 C33 C34 C38 175.99(16) . . . . ?
C30 C29 C34 C33 2.9(2) . . . . ?
N2 C29 C34 C33 -174.68(15) . . . . ?
C30 C29 C34 C38 -173.70(16) . . . . ?
N2 C29 C34 C38 8.7(2) . . . . ?
C31 C30 C35 C36 62.7(2) . . . . ?
C29 C30 C35 C36 -113.34(19) . . . . ?
C31 C30 C35 C37 -58.9(2) . . . . ?
C29 C30 C35 C37 125.05(18) . . . . ?
C33 C34 C38 C40 -68.82(19) . . . . ?
C29 C34 C38 C40 107.81(19) . . . . ?
C33 C34 C38 C39 53.1(2) . . . . ?
C29 C34 C38 C39 -130.32(18) . . . . ?
 
_refine_diff_density_max    0.373
_refine_diff_density_min   -0.325
_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          'C40 H62 Cl Fe N2'
_chemical_formula_sum
 'C40 H62 Cl Fe N2' 
_chemical_formula_weight          662.21

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'
 'Fe'  'Fe'   0.3463   0.8444
 '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/c'
_space_group_name_Hall            '-P 2ybc'
 
_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+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    11.224(2)
_cell_length_b                    19.524(3)
_cell_length_c                    16.903(2)
_cell_angle_alpha                 90
_cell_angle_beta                  97.29(2)
_cell_angle_gamma                 90
_cell_volume                      3674.1(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9997 
_cell_measurement_theta_min       2.3115 
_cell_measurement_theta_max       27.4725  
 
_exptl_crystal_description        block 
_exptl_crystal_colour             red  
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.197          
_exptl_crystal_F_000              1436
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.1 
_exptl_crystal_size_mid           0.09
_exptl_crystal_size_min           0.05 
_exptl_absorpt_coefficient_mu     0.512
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.7114 
_exptl_absorpt_correction_T_max   0.7456 
_exptl_absorpt_process_details    'SADABS-2008/4'
 
_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             110950
_diffrn_reflns_av_unetI/netI      0.0167
_diffrn_reflns_av_R_equivalents   0.0377
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -25
_diffrn_reflns_limit_k_max        25
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          1.601
_diffrn_reflns_theta_max          27.491
_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   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              8434
_reflns_number_gt                 7579
_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)+(0.0277P)²+2.4159P] 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          8434
_refine_ls_number_parameters      413
_refine_ls_number_restraints      124
_refine_ls_R_factor_all           0.0338
_refine_ls_R_factor_gt            0.0300
_refine_ls_wR_factor_ref          0.0733
_refine_ls_wR_factor_gt           0.0715
_refine_ls_goodness_of_fit_ref    1.031
_refine_ls_restrained_S_all       1.023
_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
Cl Cl 1.05038(3) 0.48929(2) 0.79132(2) 0.02497(8) Uani 1 1 d . U . . .
N1 N 0.63044(9) 0.47851(5) 0.77756(6) 0.0126(2) Uani 1 1 d . U . . .
Fe1 Fe 0.87444(2) 0.54318(2) 0.75537(2) 0.01405(5) Uani 1 1 d . U . . .
N2 N 0.86081(9) 0.68583(5) 0.67471(6) 0.0124(2) Uani 1 1 d . U . . .
C1 C 0.72402(11) 0.48915(6) 0.73685(7) 0.0130(2) Uani 1 1 d . U . . .
C2 C 0.71035(11) 0.43859(6) 0.66633(7) 0.0152(2) Uani 1 1 d . U . . .
C3 C 0.57827(11) 0.41565(7) 0.66023(7) 0.0168(2) Uani 1 1 d . U . . .
H3A H 0.5275 0.4441 0.6209 0.020 Uiso 1 1 calc R U . . .
H3B H 0.5702 0.3671 0.6433 0.020 Uiso 1 1 calc R U . . .
C4 C 0.54030(11) 0.42463(6) 0.74365(7) 0.0149(2) Uani 1 1 d . U . . .
C5 C 0.74087(13) 0.46961(7) 0.58813(8) 0.0203(3) Uani 1 1 d . U . . .
H5A H 0.7290 0.4351 0.5458 0.031 Uiso 1 1 calc R U . . .
H5B H 0.8248 0.4847 0.5950 0.031 Uiso 1 1 calc R U . . .
H5C H 0.6883 0.5089 0.5735 0.031 Uiso 1 1 calc R U . . .
C6 C 0.79781(12) 0.37826(7) 0.68722(8) 0.0198(3) Uani 1 1 d . U . . .
H6A H 0.7853 0.3435 0.6451 0.030 Uiso 1 1 calc R U . . .
H6B H 0.7829 0.3580 0.7381 0.030 Uiso 1 1 calc R U . . .
H6C H 0.8807 0.3950 0.6917 0.030 Uiso 1 1 calc R U . . .
C7 C 0.55192(12) 0.35904(7) 0.79370(8) 0.0193(3) Uani 1 1 d . U . . .
H7A H 0.4965 0.3243 0.7685 0.029 Uiso 1 1 calc R U . . .
H7B H 0.5322 0.3689 0.8474 0.029 Uiso 1 1 calc R U . . .
H7C H 0.6345 0.3419 0.7973 0.029 Uiso 1 1 calc R U . . .
C8 C 0.41016(12) 0.44847(7) 0.74009(8) 0.0196(3) Uani 1 1 d . U . . .
H8A H 0.3964 0.4872 0.7032 0.029 Uiso 1 1 calc R U . . .
H8B H 0.3944 0.4627 0.7934 0.029 Uiso 1 1 calc R U . . .
H8C H 0.3561 0.4108 0.7214 0.029 Uiso 1 1 calc R U . . .
C9 C 0.62255(11) 0.51000(6) 0.85472(7) 0.0131(2) Uani 1 1 d . U . . .
C10 C 0.68967(11) 0.48258(6) 0.92383(7) 0.0145(2) Uani 1 1 d . U . . .
C11 C 0.68056(12) 0.51408(7) 0.99707(8) 0.0176(3) Uani 1 1 d . U . . .
H11 H 0.7255 0.4963 1.0440 0.021 Uiso 1 1 calc R U . . .
C12 C 0.60783(12) 0.57037(7) 1.00274(8) 0.0184(3) Uani 1 1 d . U . . .
H12 H 0.6020 0.5906 1.0532 0.022 Uiso 1 1 calc R U . . .
C13 C 0.54346(12) 0.59712(7) 0.93464(8) 0.0175(3) Uani 1 1 d . U . . .
H13 H 0.4939 0.6361 0.9389 0.021 Uiso 1 1 calc R U . . .
C14 C 0.54946(11) 0.56830(6) 0.85970(7) 0.0141(2) Uani 1 1 d . U . . .
C15 C 0.77425(11) 0.42168(7) 0.92411(7) 0.0164(2) Uani 1 1 d . U . . .
H15 H 0.7746 0.4054 0.8681 0.020 Uiso 1 1 calc R U . . .
C16 C 0.73508(13) 0.36248(7) 0.97469(8) 0.0219(3) Uani 1 1 d . U . . .
H16A H 0.6529 0.3488 0.9543 0.033 Uiso 1 1 calc R U . . .
H16B H 0.7380 0.3774 1.0303 0.033 Uiso 1 1 calc R U . . .
H16C H 0.7893 0.3235 0.9718 0.033 Uiso 1 1 calc R U . . .
C17 C 0.90189(12) 0.44306(8) 0.95778(8) 0.0232(3) Uani 1 1 d . U . . .
H17A H 0.9570 0.4047 0.9534 0.035 Uiso 1 1 calc R U . . .
H17B H 0.9037 0.4559 1.0140 0.035 Uiso 1 1 calc R U . . .
H17C H 0.9267 0.4823 0.9275 0.035 Uiso 1 1 calc R U . . .
C18 C 0.48086(12) 0.60452(7) 0.78816(8) 0.0167(2) Uani 1 1 d . U . . .
H18 H 0.4877 0.5762 0.7396 0.020 Uiso 1 1 calc R U . . .
C19 C 0.34668(12) 0.61316(8) 0.79617(8) 0.0225(3) Uani 1 1 d . U . . .
H19A H 0.3045 0.6309 0.7460 0.034 Uiso 1 1 calc R U . . .
H19B H 0.3375 0.6454 0.8394 0.034 Uiso 1 1 calc R U . . .
H19C H 0.3126 0.5687 0.8082 0.034 Uiso 1 1 calc R U . . .
C20 C 0.53539(13) 0.67502(7) 0.77569(8) 0.0216(3) Uani 1 1 d . U . . .
H20A H 0.6186 0.6695 0.7648 0.032 Uiso 1 1 calc R U . . .
H20B H 0.5340 0.7028 0.8239 0.032 Uiso 1 1 calc R U . . .
H20C H 0.4885 0.6979 0.7304 0.032 Uiso 1 1 calc R U . . .
C21 C 0.87302(10) 0.64522(7) 0.73858(7) 0.0140(2) Uani 1 1 d . U . . .
C22 C 0.90867(11) 0.69115(7) 0.81173(7) 0.0167(2) Uani 1 1 d . U . . .
C23 C 0.87732(12) 0.76404(7) 0.78090(8) 0.0183(3) Uani 1 1 d . U . . .
H23A H 0.7967 0.7775 0.7934 0.022 Uiso 1 1 calc R U . . .
H23B H 0.9368 0.7974 0.8062 0.022 Uiso 1 1 calc R U . . .
C24 C 0.87953(11) 0.76251(6) 0.69050(8) 0.0150(2) Uani 1 1 d . U . . .
C25 C 0.84586(13) 0.67261(8) 0.88429(8) 0.0242(3) Uani 1 1 d . U . . .
H25A H 0.7587 0.6762 0.8701 0.036 Uiso 1 1 calc R U . . .
H25B H 0.8719 0.7042 0.9282 0.036 Uiso 1 1 calc R U . . .
H25C H 0.8668 0.6256 0.9010 0.036 Uiso 1 1 calc R U . . .
C26 C 1.04509(12) 0.68249(7) 0.83654(8) 0.0216(3) Uani 1 1 d . U . . .
H26A H 1.0882 0.6940 0.7914 0.032 Uiso 1 1 calc R U . . .
H26B H 1.0624 0.6349 0.8526 0.032 Uiso 1 1 calc R U . . .
H26C H 1.0713 0.7130 0.8814 0.032 Uiso 1 1 calc R U . . .
C27 C 0.78062(12) 0.80697(7) 0.64664(8) 0.0205(3) Uani 1 1 d . U . . .
H27A H 0.7793 0.8009 0.5890 0.031 Uiso 1 1 calc R U . . .
H27B H 0.7962 0.8552 0.6605 0.031 Uiso 1 1 calc R U . . .
H27C H 0.7029 0.7934 0.6623 0.031 Uiso 1 1 calc R U . . .
C28 C 0.99799(12) 0.78672(7) 0.66431(8) 0.0188(3) Uani 1 1 d . U . . .
H28A H 0.9961 0.7796 0.6068 0.028 Uiso 1 1 calc R U . . .
H28B H 1.0646 0.7605 0.6928 0.028 Uiso 1 1 calc R U . . .
H28C H 1.0093 0.8355 0.6766 0.028 Uiso 1 1 calc R U . . .
C29 C 0.84761(11) 0.66001(6) 0.59326(7) 0.0126(2) Uani 1 1 d . U . . .
C30 C 0.95033(11) 0.63698(6) 0.56056(7) 0.0140(2) Uani 1 1 d . U . . .
C31 C 0.93643(12) 0.61613(7) 0.48097(8) 0.0172(3) Uani 1 1 d . U . . .
H31 H 1.0050 0.6015 0.4579 0.021 Uiso 1 1 calc R U . . .
C32 C 0.82583(12) 0.61621(7) 0.43474(8) 0.0180(3) Uani 1 1 d . U . . .
H32 H 0.8187 0.6022 0.3805 0.022 Uiso 1 1 calc R U . . .
C33 C 0.72546(12) 0.63688(7) 0.46820(7) 0.0169(2) Uani 1 1 d . U . . .
H33 H 0.6492 0.6361 0.4366 0.020 Uiso 1 1 calc R U . . .
C34 C 0.73354(11) 0.65884(6) 0.54725(7) 0.0142(2) Uani 1 1 d . U . . .
C35 C 1.07523(11) 0.62976(7) 0.60708(8) 0.0161(2) Uani 1 1 d . U . . .
H35 H 1.0719 0.6449 0.6633 0.019 Uiso 1 1 calc R U . . .
C36 C 1.11449(12) 0.55444(7) 0.60801(8) 0.0201(3) Uani 1 1 d . U . . .
H36A H 1.1219 0.5395 0.5535 0.030 Uiso 1 1 calc R U . . .
H36B H 1.0544 0.5262 0.6300 0.030 Uiso 1 1 calc R U . . .
H36C H 1.1922 0.5495 0.6412 0.030 Uiso 1 1 calc R U . . .
C37 C 1.16860(12) 0.67365(7) 0.57123(9) 0.0233(3) Uani 1 1 d . U . . .
H37A H 1.1749 0.6582 0.5168 0.035 Uiso 1 1 calc R U . . .
H37B H 1.2468 0.6690 0.6039 0.035 Uiso 1 1 calc R U . . .
H37C H 1.1436 0.7218 0.5702 0.035 Uiso 1 1 calc R U . . .
C38 C 0.61706(11) 0.67736(7) 0.57950(8) 0.0166(2) Uani 1 1 d . U . . .
H38 H 0.6381 0.6963 0.6345 0.020 Uiso 1 1 calc R U . . .
C39 C 0.54520(13) 0.73207(7) 0.52861(9) 0.0245(3) Uani 1 1 d . U . . .
H39A H 0.5975 0.7711 0.5211 0.037 Uiso 1 1 calc R U . . .
H39B H 0.4777 0.7474 0.5557 0.037 Uiso 1 1 calc R U . . .
H39C H 0.5145 0.7126 0.4766 0.037 Uiso 1 1 calc R U . . .
C40 C 0.53788(12) 0.61420(7) 0.58543(8) 0.0195(3) Uani 1 1 d . U . . .
H40A H 0.5225 0.5921 0.5331 0.029 Uiso 1 1 calc R U . . .
H40B H 0.4615 0.6281 0.6029 0.029 Uiso 1 1 calc R U . . .
H40C H 0.5790 0.5819 0.6241 0.029 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
Cl Fe1 2.2519(5) . ?
N1 C1 1.3429(16) . ?
N1 C9 1.4546(15) . ?
N1 C4 1.5204(15) . ?
Fe1 C1 1.9816(13) . ?
Fe1 C21 2.0121(13) . ?
N2 C21 1.3325(16) . ?
N2 C29 1.4560(15) . ?
N2 C24 1.5304(16) . ?
C1 C2 1.5404(17) . ?
C2 C5 1.5318(18) . ?
C2 C3 1.5395(18) . ?
C2 C6 1.5452(18) . ?
C3 C4 1.5341(17) . ?
C4 C8 1.5269(18) . ?
C4 C7 1.5312(18) . ?
C9 C14 1.4119(17) . ?
C9 C10 1.4127(17) . ?
C10 C11 1.3976(18) . ?
C10 C15 1.5211(18) . ?
C11 C12 1.3797(19) . ?
C12 C13 1.3815(19) . ?
C13 C14 1.3955(18) . ?
C14 C18 1.5228(18) . ?
C15 C17 1.5309(18) . ?
C15 C16 1.5346(18) . ?
C18 C20 1.5317(18) . ?
C18 C19 1.5384(18) . ?
C21 C22 1.5387(17) . ?
C22 C25 1.5336(18) . ?
C22 C23 1.5407(19) . ?
C22 C26 1.5446(18) . ?
C23 C24 1.5316(18) . ?
C24 C27 1.5253(18) . ?
C24 C28 1.5287(18) . ?
C29 C34 1.4113(17) . ?
C29 C30 1.4138(17) . ?
C30 C31 1.3951(18) . ?
C30 C35 1.5244(17) . ?
C31 C32 1.3805(19) . ?
C32 C33 1.3833(19) . ?
C33 C34 1.3953(18) . ?
C34 C38 1.5225(17) . ?
C35 C36 1.5347(18) . ?
C35 C37 1.5366(18) . ?
C38 C40 1.5306(18) . ?
C38 C39 1.5348(18) . ?
 
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 N1 C9 122.31(10) . . ?
C1 N1 C4 116.12(10) . . ?
C9 N1 C4 121.14(10) . . ?
C1 Fe1 C21 120.89(5) . . ?
C1 Fe1 Cl 119.62(4) . . ?
C21 Fe1 Cl 119.45(4) . . ?
C21 N2 C29 123.21(10) . . ?
C21 N2 C24 116.30(10) . . ?
C29 N2 C24 119.93(10) . . ?
N1 C1 C2 106.84(10) . . ?
N1 C1 Fe1 135.03(9) . . ?
C2 C1 Fe1 117.56(8) . . ?
C5 C2 C3 112.09(11) . . ?
C5 C2 C1 113.78(11) . . ?
C3 C2 C1 103.82(10) . . ?
C5 C2 C6 107.06(11) . . ?
C3 C2 C6 111.84(11) . . ?
C1 C2 C6 108.28(10) . . ?
C4 C3 C2 106.42(10) . . ?
N1 C4 C8 113.05(10) . . ?
N1 C4 C7 111.37(10) . . ?
C8 C4 C7 106.90(11) . . ?
N1 C4 C3 100.16(10) . . ?
C8 C4 C3 112.00(11) . . ?
C7 C4 C3 113.46(11) . . ?
C14 C9 C10 120.61(11) . . ?
C14 C9 N1 119.75(11) . . ?
C10 C9 N1 119.64(11) . . ?
C11 C10 C9 118.33(12) . . ?
C11 C10 C15 117.19(11) . . ?
C9 C10 C15 124.46(11) . . ?
C12 C11 C10 121.50(12) . . ?
C11 C12 C13 119.65(12) . . ?
C12 C13 C14 121.58(12) . . ?
C13 C14 C9 118.33(12) . . ?
C13 C14 C18 117.12(11) . . ?
C9 C14 C18 124.48(11) . . ?
C10 C15 C17 110.01(11) . . ?
C10 C15 C16 111.57(11) . . ?
C17 C15 C16 108.61(11) . . ?
C14 C18 C20 110.85(11) . . ?
C14 C18 C19 112.52(11) . . ?
C20 C18 C19 109.05(11) . . ?
N2 C21 C22 107.08(11) . . ?
N2 C21 Fe1 134.56(9) . . ?
C22 C21 Fe1 117.85(9) . . ?
C25 C22 C21 113.96(11) . . ?
C25 C22 C23 112.34(11) . . ?
C21 C22 C23 103.98(10) . . ?
C25 C22 C26 107.31(11) . . ?
C21 C22 C26 107.58(11) . . ?
C23 C22 C26 111.65(11) . . ?
C24 C23 C22 106.71(10) . . ?
C27 C24 C28 106.82(11) . . ?
C27 C24 N2 113.36(10) . . ?
C28 C24 N2 110.92(10) . . ?
C27 C24 C23 111.77(11) . . ?
C28 C24 C23 114.06(11) . . ?
N2 C24 C23 100.01(10) . . ?
C34 C29 C30 120.48(11) . . ?
C34 C29 N2 120.20(11) . . ?
C30 C29 N2 119.32(11) . . ?
C31 C30 C29 118.22(11) . . ?
C31 C30 C35 116.96(11) . . ?
C29 C30 C35 124.75(11) . . ?
C32 C31 C30 121.87(12) . . ?
C31 C32 C33 119.30(12) . . ?
C32 C33 C34 121.59(12) . . ?
C33 C34 C29 118.48(11) . . ?
C33 C34 C38 117.48(11) . . ?
C29 C34 C38 123.99(11) . . ?
C30 C35 C36 109.75(11) . . ?
C30 C35 C37 111.94(11) . . ?
C36 C35 C37 109.22(11) . . ?
C34 C38 C40 111.36(11) . . ?
C34 C38 C39 112.26(11) . . ?
C40 C38 C39 109.22(11) . . ?
 
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 170.76(10) . . . . ?
C4 N1 C1 C2 -1.81(14) . . . . ?
C9 N1 C1 Fe1 -0.02(19) . . . . ?
C4 N1 C1 Fe1 -172.59(9) . . . . ?
N1 C1 C2 C5 139.06(11) . . . . ?
Fe1 C1 C2 C5 -48.27(13) . . . . ?
N1 C1 C2 C3 16.95(13) . . . . ?
Fe1 C1 C2 C3 -170.38(8) . . . . ?
N1 C1 C2 C6 -102.04(12) . . . . ?
Fe1 C1 C2 C6 70.62(12) . . . . ?
C5 C2 C3 C4 -148.81(11) . . . . ?
C1 C2 C3 C4 -25.59(13) . . . . ?
C6 C2 C3 C4 90.93(12) . . . . ?
C1 N1 C4 C8 -133.31(12) . . . . ?
C9 N1 C4 C8 54.02(15) . . . . ?
C1 N1 C4 C7 106.31(12) . . . . ?
C9 N1 C4 C7 -66.36(14) . . . . ?
C1 N1 C4 C3 -13.98(13) . . . . ?
C9 N1 C4 C3 173.35(10) . . . . ?
C2 C3 C4 N1 23.56(12) . . . . ?
C2 C3 C4 C8 143.65(11) . . . . ?
C2 C3 C4 C7 -95.21(12) . . . . ?
C1 N1 C9 C14 100.90(14) . . . . ?
C4 N1 C9 C14 -86.90(14) . . . . ?
C1 N1 C9 C10 -78.09(15) . . . . ?
C4 N1 C9 C10 94.12(14) . . . . ?
C14 C9 C10 C11 0.80(18) . . . . ?
N1 C9 C10 C11 179.78(11) . . . . ?
C14 C9 C10 C15 -177.67(11) . . . . ?
N1 C9 C10 C15 1.31(18) . . . . ?
C9 C10 C11 C12 0.29(19) . . . . ?
C15 C10 C11 C12 178.88(12) . . . . ?
C10 C11 C12 C13 -0.9(2) . . . . ?
C11 C12 C13 C14 0.4(2) . . . . ?
C12 C13 C14 C9 0.69(19) . . . . ?
C12 C13 C14 C18 -176.34(12) . . . . ?
C10 C9 C14 C13 -1.28(18) . . . . ?
N1 C9 C14 C13 179.74(11) . . . . ?
C10 C9 C14 C18 175.51(11) . . . . ?
N1 C9 C14 C18 -3.46(18) . . . . ?
C11 C10 C15 C17 -58.60(15) . . . . ?
C9 C10 C15 C17 119.89(13) . . . . ?
C11 C10 C15 C16 62.00(15) . . . . ?
C9 C10 C15 C16 -119.51(13) . . . . ?
C13 C14 C18 C20 66.36(15) . . . . ?
C9 C14 C18 C20 -110.47(14) . . . . ?
C13 C14 C18 C19 -56.05(15) . . . . ?
C9 C14 C18 C19 127.12(13) . . . . ?
C29 N2 C21 C22 169.23(10) . . . . ?
C24 N2 C21 C22 -2.14(14) . . . . ?
C29 N2 C21 Fe1 -2.05(18) . . . . ?
C24 N2 C21 Fe1 -173.43(9) . . . . ?
N2 C21 C22 C25 138.95(11) . . . . ?
Fe1 C21 C22 C25 -48.07(14) . . . . ?
N2 C21 C22 C23 16.32(13) . . . . ?
Fe1 C21 C22 C23 -170.70(8) . . . . ?
N2 C21 C22 C26 -102.22(12) . . . . ?
Fe1 C21 C22 C26 70.77(12) . . . . ?
C25 C22 C23 C24 -148.00(11) . . . . ?
C21 C22 C23 C24 -24.31(13) . . . . ?
C26 C22 C23 C24 91.40(12) . . . . ?
C21 N2 C24 C27 -131.97(12) . . . . ?
C29 N2 C24 C27 56.35(15) . . . . ?
C21 N2 C24 C28 107.85(12) . . . . ?
C29 N2 C24 C28 -63.83(14) . . . . ?
C21 N2 C24 C23 -12.86(13) . . . . ?
C29 N2 C24 C23 175.46(10) . . . . ?
C22 C23 C24 C27 142.35(11) . . . . ?
C22 C23 C24 C28 -96.34(12) . . . . ?
C22 C23 C24 N2 22.08(12) . . . . ?
C21 N2 C29 C34 102.31(14) . . . . ?
C24 N2 C29 C34 -86.62(14) . . . . ?
C21 N2 C29 C30 -78.47(15) . . . . ?
C24 N2 C29 C30 92.60(13) . . . . ?
C34 C29 C30 C31 2.81(18) . . . . ?
N2 C29 C30 C31 -176.41(11) . . . . ?
C34 C29 C30 C35 -174.00(11) . . . . ?
N2 C29 C30 C35 6.78(18) . . . . ?
C29 C30 C31 C32 -1.33(19) . . . . ?
C35 C30 C31 C32 175.73(12) . . . . ?
C30 C31 C32 C33 -0.6(2) . . . . ?
C31 C32 C33 C34 1.1(2) . . . . ?
C32 C33 C34 C29 0.33(19) . . . . ?
C32 C33 C34 C38 -177.22(12) . . . . ?
C30 C29 C34 C33 -2.32(18) . . . . ?
N2 C29 C34 C33 176.88(11) . . . . ?
C30 C29 C34 C38 175.05(11) . . . . ?
N2 C29 C34 C38 -5.74(18) . . . . ?
C31 C30 C35 C36 -59.48(15) . . . . ?
C29 C30 C35 C36 117.37(13) . . . . ?
C31 C30 C35 C37 61.96(15) . . . . ?
C29 C30 C35 C37 -121.19(13) . . . . ?
C33 C34 C38 C40 67.18(15) . . . . ?
C29 C34 C38 C40 -110.23(13) . . . . ?
C33 C34 C38 C39 -55.64(15) . . . . ?
C29 C34 C38 C39 126.95(13) . . . . ?
 
_refine_diff_density_max    0.367
_refine_diff_density_min   -0.288
_refine_diff_density_rms    0.045

_shelxl_version_number 2013-4



  
data_p-1_a
 
_audit_creation_method            SHELXL-2014
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C70 H67 B F21 Fe N2' 
_chemical_formula_sum
 'C70 H67 B F21 Fe N2' 
_chemical_formula_weight          1401.91

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0015   0.0009
 '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'
 'B'  'B'   0.0004   0.0004
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0096   0.0061
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0030   0.0019
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.2886   0.5448
 '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                    13.666(2)
_cell_length_b                    15.211(2)
_cell_length_c                    18.071(3)
_cell_angle_alpha                 68.51(2)
_cell_angle_beta                  89.00(2)
_cell_angle_gamma                 68.72(2)
_cell_volume                      3228.0(10)
_cell_formula_units_Z             2
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9225 
_cell_measurement_theta_min       2.268 
_cell_measurement_theta_max       18.939 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             blue 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.442          
_exptl_crystal_F_000              1442
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.124 
_exptl_crystal_size_mid           0.100 
_exptl_crystal_size_min           0.062 
_exptl_absorpt_coefficient_mu     0.184
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8271 
_exptl_absorpt_correction_T_max   0.8617 
_exptl_absorpt_process_details    'SADABS-2012/1' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.56086
_diffrn_radiation_type            AgK\a
_diffrn_source                    'INCOATEC Ag Microsource'                       
_diffrn_measurement_device_type   'Bruker Smart Apex II Quazar' 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             111967
_diffrn_reflns_av_unetI/netI      0.0305
_diffrn_reflns_av_R_equivalents   0.0553
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          1.491
_diffrn_reflns_theta_max          19.829
_diffrn_reflns_theta_full         19.665
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.994
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              11911
_reflns_number_gt                 9623
_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 v2012.2-0'
_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     'XSHELL in SHELXTL-97' 
_computing_publication_material   'SHELXP 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)+(0.0285P)²+2.1416P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          11911
_refine_ls_number_parameters      958
_refine_ls_number_restraints      554
_refine_ls_R_factor_all           0.0463
_refine_ls_R_factor_gt            0.0320
_refine_ls_wR_factor_ref          0.0767
_refine_ls_wR_factor_gt           0.0707
_refine_ls_goodness_of_fit_ref    1.024
_refine_ls_restrained_S_all       1.018
_refine_ls_shift/su_max           0.000
_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
C1A C 0.02804(13) 0.91704(13) 0.43176(10) 0.0129(4) Uani 1 1 d . . . . .
Fe1 Fe 0.5000 0.0000 0.0000 0.01320(8) Uani 1 2 d S . P . .
N1A N 0.04654(11) 0.81894(10) 0.46357(8) 0.0110(3) Uani 1 1 d . . . . .
B1 B 0.17856(15) 0.50432(15) 0.16529(12) 0.0125(4) Uani 1 1 d . . . . .
C2A C 0.03219(14) 0.94716(13) 0.34181(10) 0.0153(4) Uani 1 1 d . . . . .
Fe2 Fe 0.0000 1.0000 0.5000 0.01494(9) Uani 1 2 d S . P . .
C3A C 0.09773(16) 1.01294(15) 0.31184(11) 0.0232(4) Uani 1 1 d . . . . .
H3A H 0.1007 1.0294 0.2543 0.035 Uiso 1 1 calc R U . . .
H3B H 0.1697 0.9753 0.3409 0.035 Uiso 1 1 calc R U . . .
H3C H 0.0648 1.0763 0.3211 0.035 Uiso 1 1 calc R U . . .
C4A C -0.08161(15) 1.00905(14) 0.29758(11) 0.0212(4) Uani 1 1 d . . . . .
H4A H -0.0805 1.0251 0.2400 0.032 Uiso 1 1 calc R U . . .
H4B H -0.1115 1.0727 0.3067 0.032 Uiso 1 1 calc R U . . .
H4C H -0.1252 0.9687 0.3179 0.032 Uiso 1 1 calc R U . . .
C5A C 0.08307(15) 0.84387(13) 0.33214(10) 0.0167(4) Uani 1 1 d . . . . .
H5A H 0.0486 0.8471 0.2830 0.020 Uiso 1 1 calc R U . . .
H5B H 0.1595 0.8273 0.3280 0.020 Uiso 1 1 calc R U . . .
C6A C 0.06738(14) 0.76241(13) 0.40656(10) 0.0143(4) Uani 1 1 d . . . . .
C7A C -0.02750(15) 0.73714(14) 0.39287(11) 0.0189(4) Uani 1 1 d . . . . .
H7A H -0.0131 0.7020 0.3556 0.028 Uiso 1 1 calc R U . . .
H7B H -0.0906 0.8005 0.3701 0.028 Uiso 1 1 calc R U . . .
H7C H -0.0397 0.6926 0.4441 0.028 Uiso 1 1 calc R U . . .
C8A C 0.16474(15) 0.66299(14) 0.43955(11) 0.0195(4) Uani 1 1 d . . . . .
H8A H 0.1750 0.6281 0.4022 0.029 Uiso 1 1 calc R U . . .
H8B H 0.1546 0.6188 0.4918 0.029 Uiso 1 1 calc R U . . .
H8C H 0.2272 0.6781 0.4459 0.029 Uiso 1 1 calc R U . . .
C9A C 0.03970(14) 0.77024(13) 0.54819(10) 0.0116(4) Uani 1 1 d . . . . .
C10A C 0.13232(14) 0.72116(13) 0.60397(10) 0.0128(4) Uani 1 1 d . . . . .
C11A C 0.12256(14) 0.67494(13) 0.68457(10) 0.0152(4) Uani 1 1 d . . . . .
H11 H 0.1841 0.6401 0.7233 0.018 Uiso 1 1 calc R U . . .
C12A C 0.02584(14) 0.67871(13) 0.70928(10) 0.0146(4) Uani 1 1 d . . . . .
H12 H 0.0211 0.6458 0.7644 0.018 Uiso 1 1 calc R U . . .
C13A C -0.06446(14) 0.73051(13) 0.65366(10) 0.0147(4) Uani 1 1 d . . . . .
H13 H -0.1311 0.7339 0.6715 0.018 Uiso 1 1 calc R U . . .
C14A C -0.06025(14) 0.77787(13) 0.57214(10) 0.0129(4) Uani 1 1 d . . . . .
C15A C -0.16405(14) 0.84104(13) 0.51536(11) 0.0157(4) Uani 1 1 d . . . . .
H15 H -0.1466 0.8625 0.4592 0.019 Uiso 1 1 calc R U . . .
C16A C -0.22441(15) 0.93775(14) 0.53115(12) 0.0224(4) Uani 1 1 d . . . . .
H16A H -0.2891 0.9796 0.4926 0.034 Uiso 1 1 calc R U . . .
H16B H -0.1796 0.9770 0.5252 0.034 Uiso 1 1 calc R U . . .
H16C H -0.2432 0.9185 0.5858 0.034 Uiso 1 1 calc R U . . .
C17A C -0.23437(15) 0.78054(15) 0.52216(11) 0.0208(4) Uani 1 1 d . . . . .
H17A H -0.2988 0.8235 0.4835 0.031 Uiso 1 1 calc R U . . .
H17B H -0.2536 0.7597 0.5766 0.031 Uiso 1 1 calc R U . . .
H17C H -0.1958 0.7196 0.5108 0.031 Uiso 1 1 calc R U . . .
C18A C 0.23994(14) 0.72295(14) 0.58289(11) 0.0162(4) Uani 1 1 d . . . . .
H18 H 0.2351 0.7544 0.5231 0.019 Uiso 1 1 calc R U . . .
C19A C 0.32676(14) 0.61537(14) 0.61278(11) 0.0216(4) Uani 1 1 d . . . . .
H19A H 0.3929 0.6192 0.5930 0.032 Uiso 1 1 calc R U . . .
H19B H 0.3054 0.5722 0.5929 0.032 Uiso 1 1 calc R U . . .
H19C H 0.3375 0.5858 0.6716 0.032 Uiso 1 1 calc R U . . .
C19 C 0.55001(16) -0.12730(16) 0.21923(12) 0.0268(5) Uani 1 1 d . . . . .
H191 H 0.5262 -0.1091 0.1628 0.040 Uiso 1 1 calc R U . . .
H192 H 0.4892 -0.1211 0.2493 0.040 Uiso 1 1 calc R U . . .
H193 H 0.6020 -0.1979 0.2419 0.040 Uiso 1 1 calc R U . . .
C18 C 0.60091(15) -0.05526(14) 0.22489(11) 0.0192(4) Uani 1 1 d . . . . .
H181 H 0.5466 0.0162 0.2008 0.023 Uiso 1 1 calc R U . . .
C20A C 0.26817(15) 0.78984(15) 0.61817(12) 0.0230(4) Uani 1 1 d . . . . .
H20A H 0.3360 0.7936 0.6025 0.034 Uiso 1 1 calc R U . . .
H20B H 0.2738 0.7598 0.6768 0.034 Uiso 1 1 calc R U . . .
H20C H 0.2127 0.8588 0.5977 0.034 Uiso 1 1 calc R U . . .
C20 C 0.63336(16) -0.07876(17) 0.31298(11) 0.0283(5) Uani 1 1 d . . . . .
H201 H 0.6672 -0.0330 0.3158 0.042 Uiso 1 1 calc R U . . .
H202 H 0.6833 -0.1499 0.3388 0.042 Uiso 1 1 calc R U . . .
H203 H 0.5703 -0.0683 0.3406 0.042 Uiso 1 1 calc R U . . .
C1' C 0.15260(13) 0.56963(13) 0.06710(10) 0.0118(4) Uani 1 1 d . . . . .
C2' C 0.09848(13) 0.67541(13) 0.03672(10) 0.0131(4) Uani 1 1 d . . . . .
F2' F 0.06022(8) 0.72197(7) 0.08826(6) 0.0169(2) Uani 1 1 d . . . . .
C3' C 0.08098(14) 0.73832(13) -0.04319(11) 0.0144(4) Uani 1 1 d . . . . .
F3' F 0.02641(8) 0.84035(7) -0.06795(6) 0.0212(2) Uani 1 1 d . . . . .
C4' C 0.12104(14) 0.69709(13) -0.09868(10) 0.0159(4) Uani 1 1 d . . . . .
F4' F 0.10794(9) 0.75783(8) -0.17660(6) 0.0250(3) Uani 1 1 d . . . . .
C5' C 0.17592(14) 0.59333(14) -0.07262(10) 0.0152(4) Uani 1 1 d . . . . .
F5' F 0.21646(9) 0.55077(8) -0.12571(6) 0.0234(2) Uani 1 1 d . . . . .
F6' F 0.24698(8) 0.43208(7) 0.02720(6) 0.0169(2) Uani 1 1 d . . . . .
C6' C 0.19043(13) 0.53288(12) 0.00808(10) 0.0128(4) Uani 1 1 d . . . . .
C7' C 0.26948(13) 0.54041(13) 0.19056(10) 0.0117(4) Uani 1 1 d . . . . .
C8' C 0.37197(14) 0.50439(13) 0.17186(10) 0.0137(4) Uani 1 1 d . . . . .
F8' F 0.39648(8) 0.43927(8) 0.13306(6) 0.0178(2) Uani 1 1 d . . . . .
F9' F 0.55191(8) 0.48441(8) 0.17444(6) 0.0219(2) Uani 1 1 d . . . . .
C9' C 0.45400(14) 0.52705(14) 0.19166(10) 0.0156(4) Uani 1 1 d . . . . .
C10' C 0.43496(14) 0.59426(14) 0.22992(10) 0.0163(4) Uani 1 1 d . . . . .
F10' F 0.51320(8) 0.61775(8) 0.25117(6) 0.0221(2) Uani 1 1 d . . . . .
C11' C 0.33395(14) 0.63757(13) 0.24537(10) 0.0159(4) Uani 1 1 d . . . . .
F11' F 0.31294(9) 0.70626(8) 0.28021(7) 0.0240(3) Uani 1 1 d . . . . .
C12' C 0.25459(13) 0.61060(13) 0.22604(10) 0.0133(4) Uani 1 1 d . . . . .
F12' F 0.15835(8) 0.65786(8) 0.24495(6) 0.0173(2) Uani 1 1 d . . . . .
C13' C 0.22160(13) 0.37871(13) 0.19132(10) 0.0119(4) Uani 1 1 d . . . . .
C14' C 0.16461(13) 0.33782(13) 0.15983(10) 0.0131(4) Uani 1 1 d . . . . .
F14' F 0.07625(8) 0.40189(7) 0.10646(6) 0.0162(2) Uani 1 1 d . . . . .
C15' C 0.19120(14) 0.23497(13) 0.17838(10) 0.0149(4) Uani 1 1 d . . . . .
F15' F 0.13238(8) 0.20254(8) 0.14369(6) 0.0210(2) Uani 1 1 d . . . . .
C16' C 0.27939(14) 0.16487(13) 0.23281(11) 0.0161(4) Uani 1 1 d . . . . .
F16' F 0.30850(9) 0.06416(8) 0.25073(7) 0.0247(3) Uani 1 1 d . . . . .
C17' C 0.33761(14) 0.19974(13) 0.26782(10) 0.0163(4) Uani 1 1 d . . . . .
F17' F 0.42328(8) 0.13242(8) 0.32251(6) 0.0229(2) Uani 1 1 d . . . . .
C18' C 0.30796(13) 0.30401(13) 0.24728(10) 0.0133(4) Uani 1 1 d . . . . .
F18' F 0.37028(8) 0.32904(8) 0.28686(6) 0.0179(2) Uani 1 1 d . . . . .
C19' C 0.07384(13) 0.52792(12) 0.21305(10) 0.0124(4) Uani 1 1 d . . . . .
C20' C -0.03187(14) 0.57008(13) 0.18002(10) 0.0151(4) Uani 1 1 d . . . . .
F20' F -0.05924(8) 0.60085(8) 0.10024(6) 0.0203(2) Uani 1 1 d . . . . .
F21' F -0.21586(8) 0.62504(9) 0.18824(7) 0.0287(3) Uani 1 1 d . . . . .
C21' C -0.11546(14) 0.58338(14) 0.22431(11) 0.0191(4) Uani 1 1 d . . . . .
F22' F -0.17749(9) 0.56671(9) 0.34972(7) 0.0308(3) Uani 1 1 d . . . . .
C22' C -0.09643(15) 0.55401(14) 0.30603(12) 0.0201(4) Uani 1 1 d . . . . .
F23' F 0.02710(9) 0.47863(8) 0.42281(6) 0.0247(3) Uani 1 1 d . . . . .
C23' C 0.00636(15) 0.51000(13) 0.34247(10) 0.0173(4) Uani 1 1 d . . . . .
F24' F 0.18678(8) 0.45225(8) 0.33628(6) 0.0187(2) Uani 1 1 d . . . . .
C24' C 0.08723(13) 0.49787(13) 0.29611(10) 0.0139(4) Uani 1 1 d . . . . .
N1 N 0.59115(11) 0.10555(11) 0.07046(8) 0.0126(3) Uani 1 1 d . . . . .
C1 C 0.51050(13) 0.11300(13) 0.02666(10) 0.0124(4) Uani 1 1 d . . . . .
C2 C 0.42723(13) 0.22074(13) 0.00161(10) 0.0138(4) Uani 1 1 d . . . . .
C3 C 0.43289(15) 0.28019(14) -0.08654(11) 0.0186(4) Uani 1 1 d . . . . .
H3AA H 0.3861 0.3523 -0.1023 0.028 Uiso 1 1 calc R U . . .
H3AB H 0.4103 0.2515 -0.1204 0.028 Uiso 1 1 calc R U . . .
H3AC H 0.5059 0.2748 -0.0932 0.028 Uiso 1 1 calc R U . . .
C4 C 0.31671(14) 0.21845(14) 0.00992(11) 0.0171(4) Uani 1 1 d . . . . .
H4AA H 0.2642 0.2884 -0.0053 0.026 Uiso 1 1 calc R U . . .
H4AB H 0.3138 0.1777 0.0657 0.026 Uiso 1 1 calc R U . . .
H4AC H 0.3011 0.1878 -0.0253 0.026 Uiso 1 1 calc R U . . .
C5 C 0.46170(14) 0.26306(14) 0.05804(11) 0.0164(4) Uani 1 1 d . . . . .
H5AA H 0.4483 0.3364 0.0291 0.020 Uiso 1 1 calc R U . . .
H5AB H 0.4215 0.2557 0.1046 0.020 Uiso 1 1 calc R U . . .
C6 C 0.58041(14) 0.20070(13) 0.08617(11) 0.0170(4) Uani 1 1 d . . . . .
C7 C 0.65161(15) 0.25160(15) 0.03735(13) 0.0242(4) Uani 1 1 d . . . . .
H7AA H 0.6454 0.3112 0.0492 0.036 Uiso 1 1 calc R U . . .
H7AB H 0.6297 0.2735 -0.0200 0.036 Uiso 1 1 calc R U . . .
H7AC H 0.7254 0.2026 0.0516 0.036 Uiso 1 1 calc R U . . .
C8 C 0.61099(16) 0.17521(15) 0.17455(12) 0.0257(5) Uani 1 1 d . . . . .
H8AA H 0.6011 0.2382 0.1823 0.039 Uiso 1 1 calc R U . . .
H8AB H 0.6854 0.1284 0.1911 0.039 Uiso 1 1 calc R U . . .
H8AC H 0.5661 0.1427 0.2070 0.039 Uiso 1 1 calc R U . . .
C9 C 0.68609(13) 0.01264(13) 0.09979(10) 0.0140(4) Uani 1 1 d . . . . .
C10 C 0.69318(14) -0.06172(14) 0.17590(11) 0.0162(4) Uani 1 1 d . . . . .
C11 C 0.78639(15) -0.14894(14) 0.20390(11) 0.0196(4) Uani 1 1 d . . . . .
H11A H 0.7934 -0.2006 0.2553 0.024 Uiso 1 1 calc R U . . .
C12 C 0.86882(15) -0.16177(14) 0.15835(11) 0.0202(4) Uani 1 1 d . . . . .
H12A H 0.9332 -0.2200 0.1797 0.024 Uiso 1 1 calc R U . . .
C13 C 0.85761(14) -0.08977(14) 0.08149(11) 0.0186(4) Uani 1 1 d . . . . .
H13A H 0.9135 -0.1007 0.0498 0.022 Uiso 1 1 calc R U . . .
C14 C 0.76542(14) -0.00141(13) 0.04992(11) 0.0151(4) Uani 1 1 d . . . . .
C15 C 0.75153(14) 0.06937(14) -0.03767(11) 0.0166(4) Uani 1 1 d . . . . .
H15A H 0.6889 0.1339 -0.0466 0.020 Uiso 1 1 calc R U . . .
C16 C 0.84727(15) 0.09802(15) -0.06074(12) 0.0248(4) Uani 1 1 d . . . . .
H16D H 0.8304 0.1504 -0.1153 0.037 Uiso 1 1 calc R U . . .
H16E H 0.9079 0.0372 -0.0584 0.037 Uiso 1 1 calc R U . . .
H16F H 0.8648 0.1248 -0.0232 0.037 Uiso 1 1 calc R U . . .
C17 C 0.72801(15) 0.02123(15) -0.09274(11) 0.0213(4) Uani 1 1 d . . . . .
H17D H 0.7178 0.0684 -0.1488 0.032 Uiso 1 1 calc R U . . .
H17E H 0.6636 0.0076 -0.0804 0.032 Uiso 1 1 calc R U . . .
H17F H 0.7876 -0.0431 -0.0843 0.032 Uiso 1 1 calc R U . . .
C1T C 0.5437(4) 0.2162(3) 0.5434(3) 0.0267(11) Uani 0.707(5) 1 d D U P A 1
C2T C 0.4715(4) 0.2621(4) 0.4743(3) 0.0247(12) Uani 0.707(5) 1 d D U P A 1
H2T H 0.4657 0.2246 0.4438 0.030 Uiso 0.707(5) 1 calc R U P A 1
C3T C 0.4085(4) 0.3640(4) 0.4517(3) 0.0332(12) Uani 0.707(5) 1 d D U P A 1
H3T H 0.3585 0.3981 0.4046 0.040 Uiso 0.707(5) 1 calc R U P A 1
C4T C 0.4175(5) 0.4170(4) 0.4969(3) 0.0440(13) Uani 0.707(5) 1 d D U P A 1
H4T H 0.3728 0.4872 0.4808 0.053 Uiso 0.707(5) 1 calc R U P A 1
C5T C 0.4901(4) 0.3703(4) 0.5649(3) 0.0353(12) Uani 0.707(5) 1 d D U P A 1
H5T H 0.4956 0.4082 0.5952 0.042 Uiso 0.707(5) 1 calc R U P A 1
C6T C 0.5550(4) 0.2685(4) 0.5891(3) 0.0272(13) Uani 0.707(5) 1 d D U P A 1
H6T H 0.6059 0.2352 0.6357 0.033 Uiso 0.707(5) 1 calc R U P A 1
F1 F 0.6074(2) 0.11584(17) 0.56679(14) 0.0499(8) Uani 0.707(5) 1 d D U P A 1
C1TA C 0.4358(10) 0.3749(8) 0.5075(7) 0.042(3) Uani 0.293(5) 1 d D U P A 2
H1TA H 0.3896 0.4445 0.4919 0.051 Uiso 0.104(5) 1 d R U P B 2
C2TA C 0.5117(9) 0.3281(9) 0.5751(6) 0.034(3) Uani 0.293(5) 1 d D U P A 2
H2TA H 0.5182 0.3654 0.6057 0.040 Uiso 0.293(5) 1 calc R U P A 2
C3TA C 0.5757(11) 0.2291(9) 0.5960(8) 0.034(3) Uani 0.293(5) 1 d D U P A 2
H3TA H 0.6287 0.1955 0.6414 0.041 Uiso 0.224(5) 1 d R U P C 2
C4TA C 0.5682(10) 0.1738(11) 0.5533(8) 0.039(3) Uani 0.293(5) 1 d D U P A 2
H4TA H 0.6133 0.1037 0.5694 0.046 Uiso 0.293(5) 1 calc R U P A 2
C5TA C 0.4949(12) 0.2210(9) 0.4873(8) 0.034(3) Uani 0.293(5) 1 d D U P A 2
H5TA H 0.4911 0.1810 0.4584 0.041 Uiso 0.258(5) 1 d R U P D 2
C6TA C 0.4285(11) 0.3201(9) 0.4629(7) 0.030(3) Uani 0.293(5) 1 d D U P A 2
H6TA H 0.3780 0.3514 0.4162 0.037 Uiso 0.293(5) 1 calc R U P A 2
F1A F 0.3792(9) 0.4727(8) 0.4810(6) 0.070(4) Uiso 0.189(5) 1 d D U P A 2
F1C F 0.6467(14) 0.1705(13) 0.6579(10) 0.044(6) Uani 0.068(4) 1 d D U P A 2
F1B F 0.494(3) 0.161(2) 0.451(2) 0.047(11) Uani 0.035(4) 1 d D 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
C1A N1A 1.313(2) . ?
C1A C2A 1.525(2) . ?
C1A Fe2 2.0082(17) . ?
Fe1 C1 1.9987(17) . ?
Fe1 C1 1.9988(17) 2_655 ?
N1A C9A 1.453(2) . ?
N1A C6A 1.531(2) . ?
B1 C19' 1.653(3) . ?
B1 C1' 1.654(3) . ?
B1 C7' 1.659(3) . ?
B1 C13' 1.659(3) . ?
C2A C3A 1.527(3) . ?
C2A C4A 1.540(3) . ?
C2A C5A 1.545(2) . ?
Fe2 C1A 2.0082(17) 2_576 ?
C5A C6A 1.534(2) . ?
C6A C8A 1.523(3) . ?
C6A C7A 1.527(3) . ?
C9A C14A 1.403(2) . ?
C9A C10A 1.408(2) . ?
C10A C11A 1.395(2) . ?
C10A C18A 1.520(2) . ?
C11A C12A 1.376(3) . ?
C12A C13A 1.383(2) . ?
C13A C14A 1.394(2) . ?
C14A C15A 1.526(2) . ?
C15A C17A 1.530(3) . ?
C15A C16A 1.531(3) . ?
C18A C19A 1.531(3) . ?
C18A C20A 1.536(3) . ?
C19 C18 1.527(3) . ?
C18 C10 1.523(3) . ?
C18 C20 1.533(3) . ?
C1' C6' 1.387(2) . ?
C1' C2' 1.393(2) . ?
C2' F2' 1.356(2) . ?
C2' C3' 1.375(2) . ?
C3' F3' 1.352(2) . ?
C3' C4' 1.375(3) . ?
C4' F4' 1.343(2) . ?
C4' C5' 1.373(3) . ?
C5' F5' 1.350(2) . ?
C5' C6' 1.381(2) . ?
F6' C6' 1.3522(19) . ?
C7' C12' 1.390(2) . ?
C7' C8' 1.392(2) . ?
C8' F8' 1.3583(19) . ?
C8' C9' 1.374(3) . ?
F9' C9' 1.346(2) . ?
C9' C10' 1.382(3) . ?
C10' F10' 1.346(2) . ?
C10' C11' 1.371(3) . ?
C11' F11' 1.352(2) . ?
C11' C12' 1.381(2) . ?
C12' F12' 1.357(2) . ?
C13' C18' 1.390(2) . ?
C13' C14' 1.394(2) . ?
C14' F14' 1.355(2) . ?
C14' C15' 1.378(2) . ?
C15' F15' 1.347(2) . ?
C15' C16' 1.377(3) . ?
C16' F16' 1.345(2) . ?
C16' C17' 1.373(3) . ?
C17' F17' 1.351(2) . ?
C17' C18' 1.387(3) . ?
C18' F18' 1.356(2) . ?
C19' C20' 1.390(2) . ?
C19' C24' 1.393(2) . ?
C20' F20' 1.355(2) . ?
C20' C21' 1.380(3) . ?
F21' C21' 1.344(2) . ?
C21' C22' 1.376(3) . ?
F22' C22' 1.347(2) . ?
C22' C23' 1.372(3) . ?
F23' C23' 1.351(2) . ?
C23' C24' 1.375(3) . ?
F24' C24' 1.356(2) . ?
N1 C1 1.315(2) . ?
N1 C9 1.451(2) . ?
N1 C6 1.531(2) . ?
C1 C2 1.519(2) . ?
C2 C4 1.527(2) . ?
C2 C3 1.534(2) . ?
C2 C5 1.547(2) . ?
C5 C6 1.532(2) . ?
C6 C8 1.526(3) . ?
C6 C7 1.530(3) . ?
C9 C10 1.402(3) . ?
C9 C14 1.404(3) . ?
C10 C11 1.394(3) . ?
C11 C12 1.382(3) . ?
C12 C13 1.387(3) . ?
C13 C14 1.398(3) . ?
C14 C15 1.521(3) . ?
C15 C16 1.529(3) . ?
C15 C17 1.532(3) . ?
C1T F1 1.357(4) . ?
C1T C6T 1.384(5) . ?
C1T C2T 1.386(5) . ?
C2T C3T 1.375(5) . ?
C3T C4T 1.373(6) . ?
C4T C5T 1.376(6) . ?
C5T C6T 1.377(5) . ?
C1TA F1A 1.303(11) . ?
C1TA C6TA 1.380(11) . ?
C1TA C2TA 1.396(11) . ?
C2TA C3TA 1.347(10) . ?
C3TA F1C 1.292(14) . ?
C3TA C4TA 1.363(11) . ?
C4TA C5TA 1.353(11) . ?
C5TA F1B 1.315(15) . ?
C5TA C6TA 1.350(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
N1A C1A C2A 107.86(15) . . ?
N1A C1A Fe2 120.91(12) . . ?
C2A C1A Fe2 131.23(12) . . ?
C1 Fe1 C1 180.0 . 2_655 ?
C1A N1A C9A 120.13(14) . . ?
C1A N1A C6A 116.93(14) . . ?
C9A N1A C6A 122.81(13) . . ?
C19' B1 C1' 113.94(14) . . ?
C19' B1 C7' 112.94(14) . . ?
C1' B1 C7' 101.78(13) . . ?
C19' B1 C13' 102.59(14) . . ?
C1' B1 C13' 113.44(14) . . ?
C7' B1 C13' 112.60(14) . . ?
C1A C2A C3A 111.31(15) . . ?
C1A C2A C4A 108.66(15) . . ?
C3A C2A C4A 108.70(15) . . ?
C1A C2A C5A 104.09(14) . . ?
C3A C2A C5A 111.75(15) . . ?
C4A C2A C5A 112.26(15) . . ?
C1A Fe2 C1A 180.00(10) . 2_576 ?
C6A C5A C2A 107.05(14) . . ?
C8A C6A C7A 108.33(15) . . ?
C8A C6A N1A 111.53(14) . . ?
C7A C6A N1A 110.69(14) . . ?
C8A C6A C5A 113.28(15) . . ?
C7A C6A C5A 113.34(15) . . ?
N1A C6A C5A 99.50(13) . . ?
C14A C9A C10A 121.98(15) . . ?
C14A C9A N1A 118.65(15) . . ?
C10A C9A N1A 119.30(15) . . ?
C11A C10A C9A 117.58(16) . . ?
C11A C10A C18A 118.02(15) . . ?
C9A C10A C18A 124.20(15) . . ?
C12A C11A C10A 121.48(16) . . ?
C11A C12A C13A 119.79(16) . . ?
C12A C13A C14A 121.67(17) . . ?
C13A C14A C9A 117.41(16) . . ?
C13A C14A C15A 118.59(16) . . ?
C9A C14A C15A 123.83(15) . . ?
C14A C15A C17A 112.54(15) . . ?
C14A C15A C16A 110.06(15) . . ?
C17A C15A C16A 109.97(15) . . ?
C10A C18A C19A 112.02(15) . . ?
C10A C18A C20A 109.44(15) . . ?
C19A C18A C20A 110.36(15) . . ?
C10 C18 C19 109.80(15) . . ?
C10 C18 C20 112.88(16) . . ?
C19 C18 C20 110.27(16) . . ?
C6' C1' C2' 112.88(15) . . ?
C6' C1' B1 126.90(15) . . ?
C2' C1' B1 119.71(15) . . ?
F2' C2' C3' 116.21(15) . . ?
F2' C2' C1' 119.10(15) . . ?
C3' C2' C1' 124.68(16) . . ?
F3' C3' C4' 119.42(15) . . ?
F3' C3' C2' 121.04(16) . . ?
C4' C3' C2' 119.53(16) . . ?
F4' C4' C5' 120.94(16) . . ?
F4' C4' C3' 120.33(16) . . ?
C5' C4' C3' 118.71(16) . . ?
F5' C5' C4' 120.02(16) . . ?
F5' C5' C6' 120.18(15) . . ?
C4' C5' C6' 119.79(16) . . ?
F6' C6' C5' 114.83(15) . . ?
F6' C6' C1' 120.80(15) . . ?
C5' C6' C1' 124.37(16) . . ?
C12' C7' C8' 112.72(15) . . ?
C12' C7' B1 126.98(15) . . ?
C8' C7' B1 120.18(15) . . ?
F8' C8' C9' 115.65(15) . . ?
F8' C8' C7' 119.22(15) . . ?
C9' C8' C7' 125.11(16) . . ?
F9' C9' C8' 120.79(16) . . ?
F9' C9' C10' 120.07(16) . . ?
C8' C9' C10' 119.14(16) . . ?
F10' C10' C11' 120.34(16) . . ?
F10' C10' C9' 121.12(16) . . ?
C11' C10' C9' 118.54(16) . . ?
F11' C11' C10' 119.42(16) . . ?
F11' C11' C12' 120.37(16) . . ?
C10' C11' C12' 120.21(16) . . ?
F12' C12' C11' 114.71(15) . . ?
F12' C12' C7' 121.24(15) . . ?
C11' C12' C7' 124.06(16) . . ?
C18' C13' C14' 112.84(15) . . ?
C18' C13' B1 127.25(15) . . ?
C14' C13' B1 119.77(15) . . ?
F14' C14' C15' 115.81(15) . . ?
F14' C14' C13' 119.22(15) . . ?
C15' C14' C13' 124.97(16) . . ?
F15' C15' C16' 119.87(15) . . ?
F15' C15' C14' 120.82(16) . . ?
C16' C15' C14' 119.31(16) . . ?
F16' C16' C17' 120.62(16) . . ?
F16' C16' C15' 120.58(16) . . ?
C17' C16' C15' 118.80(16) . . ?
F17' C17' C16' 119.91(16) . . ?
F17' C17' C18' 120.17(16) . . ?
C16' C17' C18' 119.92(16) . . ?
F18' C18' C17' 114.53(15) . . ?
F18' C18' C13' 121.36(15) . . ?
C17' C18' C13' 124.11(16) . . ?
C20' C19' C24' 113.05(16) . . ?
C20' C19' B1 126.87(15) . . ?
C24' C19' B1 119.92(15) . . ?
F20' C20' C21' 115.32(15) . . ?
F20' C20' C19' 120.93(16) . . ?
C21' C20' C19' 123.75(17) . . ?
F21' C21' C22' 119.43(16) . . ?
F21' C21' C20' 120.50(17) . . ?
C22' C21' C20' 120.06(17) . . ?
F22' C22' C23' 120.52(17) . . ?
F22' C22' C21' 120.47(17) . . ?
C23' C22' C21' 119.00(17) . . ?
F23' C23' C22' 120.10(16) . . ?
F23' C23' C24' 120.89(16) . . ?
C22' C23' C24' 119.02(17) . . ?
F24' C24' C23' 115.81(15) . . ?
F24' C24' C19' 119.09(15) . . ?
C23' C24' C19' 125.10(16) . . ?
C1 N1 C9 121.17(14) . . ?
C1 N1 C6 116.42(14) . . ?
C9 N1 C6 122.39(13) . . ?
N1 C1 C2 108.28(15) . . ?
N1 C1 Fe1 125.24(13) . . ?
C2 C1 Fe1 126.48(12) . . ?
C1 C2 C4 110.57(14) . . ?
C1 C2 C3 107.80(14) . . ?
C4 C2 C3 109.25(15) . . ?
C1 C2 C5 103.62(14) . . ?
C4 C2 C5 113.52(15) . . ?
C3 C2 C5 111.84(14) . . ?
C6 C5 C2 106.86(14) . . ?
C8 C6 C7 108.05(16) . . ?
C8 C6 N1 112.02(15) . . ?
C7 C6 N1 110.41(14) . . ?
C8 C6 C5 112.84(16) . . ?
C7 C6 C5 113.93(16) . . ?
N1 C6 C5 99.48(13) . . ?
C10 C9 C14 122.40(16) . . ?
C10 C9 N1 118.52(16) . . ?
C14 C9 N1 119.04(15) . . ?
C11 C10 C9 117.55(17) . . ?
C11 C10 C18 119.33(17) . . ?
C9 C10 C18 122.89(16) . . ?
C12 C11 C10 121.28(18) . . ?
C11 C12 C13 120.04(17) . . ?
C12 C13 C14 121.10(18) . . ?
C13 C14 C9 117.38(17) . . ?
C13 C14 C15 119.18(16) . . ?
C9 C14 C15 123.22(16) . . ?
C14 C15 C16 113.03(15) . . ?
C14 C15 C17 110.53(15) . . ?
C16 C15 C17 109.74(15) . . ?
F1 C1T C6T 118.2(4) . . ?
F1 C1T C2T 118.8(4) . . ?
C6T C1T C2T 122.9(4) . . ?
C3T C2T C1T 117.5(4) . . ?
C4T C3T C2T 120.5(4) . . ?
C3T C4T C5T 121.2(4) . . ?
C4T C5T C6T 120.0(4) . . ?
C5T C6T C1T 117.9(4) . . ?
F1A C1TA C6TA 119.2(10) . . ?
F1A C1TA C2TA 120.4(10) . . ?
C6TA C1TA C2TA 120.0(9) . . ?
C3TA C2TA C1TA 118.6(10) . . ?
F1C C3TA C2TA 128.6(12) . . ?
F1C C3TA C4TA 109.4(11) . . ?
C2TA C3TA C4TA 122.0(11) . . ?
C5TA C4TA C3TA 118.4(11) . . ?
F1B C5TA C6TA 123.9(15) . . ?
F1B C5TA C4TA 113.5(15) . . ?
C6TA C5TA C4TA 122.6(11) . . ?
C5TA C6TA C1TA 118.4(10) . . ?
 
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
C2A C1A N1A C9A -175.39(14) . . . . ?
Fe2 C1A N1A C9A 4.3(2) . . . . ?
C2A C1A N1A C6A 0.5(2) . . . . ?
Fe2 C1A N1A C6A -179.79(11) . . . . ?
N1A C1A C2A C3A -133.95(16) . . . . ?
Fe2 C1A C2A C3A 46.4(2) . . . . ?
N1A C1A C2A C4A 106.38(16) . . . . ?
Fe2 C1A C2A C4A -73.26(19) . . . . ?
N1A C1A C2A C5A -13.41(18) . . . . ?
Fe2 C1A C2A C5A 166.94(13) . . . . ?
C1A C2A C5A C6A 21.11(18) . . . . ?
C3A C2A C5A C6A 141.35(15) . . . . ?
C4A C2A C5A C6A -96.22(17) . . . . ?
C1A N1A C6A C8A 132.29(16) . . . . ?
C9A N1A C6A C8A -51.9(2) . . . . ?
C1A N1A C6A C7A -107.02(17) . . . . ?
C9A N1A C6A C7A 68.77(19) . . . . ?
C1A N1A C6A C5A 12.49(19) . . . . ?
C9A N1A C6A C5A -171.72(14) . . . . ?
C2A C5A C6A C8A -138.22(15) . . . . ?
C2A C5A C6A C7A 97.82(17) . . . . ?
C2A C5A C6A N1A -19.72(17) . . . . ?
C1A N1A C9A C14A 82.3(2) . . . . ?
C6A N1A C9A C14A -93.33(19) . . . . ?
C1A N1A C9A C10A -94.7(2) . . . . ?
C6A N1A C9A C10A 89.64(19) . . . . ?
C14A C9A C10A C11A 3.3(2) . . . . ?
N1A C9A C10A C11A -179.73(15) . . . . ?
C14A C9A C10A C18A -171.38(16) . . . . ?
N1A C9A C10A C18A 5.5(2) . . . . ?
C9A C10A C11A C12A -1.3(3) . . . . ?
C18A C10A C11A C12A 173.75(16) . . . . ?
C10A C11A C12A C13A -0.9(3) . . . . ?
C11A C12A C13A C14A 1.3(3) . . . . ?
C12A C13A C14A C9A 0.6(2) . . . . ?
C12A C13A C14A C15A -174.96(16) . . . . ?
C10A C9A C14A C13A -3.0(2) . . . . ?
N1A C9A C14A C13A -179.95(14) . . . . ?
C10A C9A C14A C15A 172.33(16) . . . . ?
N1A C9A C14A C15A -4.6(2) . . . . ?
C13A C14A C15A C17A -54.4(2) . . . . ?
C9A C14A C15A C17A 130.34(18) . . . . ?
C13A C14A C15A C16A 68.7(2) . . . . ?
C9A C14A C15A C16A -106.62(19) . . . . ?
C11A C10A C18A C19A 57.1(2) . . . . ?
C9A C10A C18A C19A -128.17(18) . . . . ?
C11A C10A C18A C20A -65.6(2) . . . . ?
C9A C10A C18A C20A 109.10(19) . . . . ?
C19' B1 C1' C6' -137.06(17) . . . . ?
C7' B1 C1' C6' 101.05(19) . . . . ?
C13' B1 C1' C6' -20.2(2) . . . . ?
C19' B1 C1' C2' 51.7(2) . . . . ?
C7' B1 C1' C2' -70.16(18) . . . . ?
C13' B1 C1' C2' 168.62(15) . . . . ?
C6' C1' C2' F2' -177.86(14) . . . . ?
B1 C1' C2' F2' -5.5(2) . . . . ?
C6' C1' C2' C3' 1.5(2) . . . . ?
B1 C1' C2' C3' 173.89(16) . . . . ?
F2' C2' C3' F3' -1.5(2) . . . . ?
C1' C2' C3' F3' 179.14(15) . . . . ?
F2' C2' C3' C4' 177.47(15) . . . . ?
C1' C2' C3' C4' -1.9(3) . . . . ?
F3' C3' C4' F4' 1.3(3) . . . . ?
C2' C3' C4' F4' -177.63(15) . . . . ?
F3' C3' C4' C5' -179.77(15) . . . . ?
C2' C3' C4' C5' 1.3(3) . . . . ?
F4' C4' C5' F5' -0.9(3) . . . . ?
C3' C4' C5' F5' -179.77(16) . . . . ?
F4' C4' C5' C6' 178.46(16) . . . . ?
C3' C4' C5' C6' -0.4(3) . . . . ?
F5' C5' C6' F6' 0.3(2) . . . . ?
C4' C5' C6' F6' -179.02(15) . . . . ?
F5' C5' C6' C1' 179.47(16) . . . . ?
C4' C5' C6' C1' 0.1(3) . . . . ?
C2' C1' C6' F6' 178.49(14) . . . . ?
B1 C1' C6' F6' 6.8(3) . . . . ?
C2' C1' C6' C5' -0.6(3) . . . . ?
B1 C1' C6' C5' -172.33(17) . . . . ?
C19' B1 C7' C12' -20.0(2) . . . . ?
C1' B1 C7' C12' 102.59(19) . . . . ?
C13' B1 C7' C12' -135.62(17) . . . . ?
C19' B1 C7' C8' 164.19(15) . . . . ?
C1' B1 C7' C8' -73.24(18) . . . . ?
C13' B1 C7' C8' 48.6(2) . . . . ?
C12' C7' C8' F8' -176.61(14) . . . . ?
B1 C7' C8' F8' -0.2(2) . . . . ?
C12' C7' C8' C9' 5.4(2) . . . . ?
B1 C7' C8' C9' -178.23(16) . . . . ?
F8' C8' C9' F9' -1.4(2) . . . . ?
C7' C8' C9' F9' 176.66(16) . . . . ?
F8' C8' C9' C10' 178.81(15) . . . . ?
C7' C8' C9' C10' -3.1(3) . . . . ?
F9' C9' C10' F10' -0.5(3) . . . . ?
C8' C9' C10' F10' 179.27(15) . . . . ?
F9' C9' C10' C11' 178.95(15) . . . . ?
C8' C9' C10' C11' -1.3(3) . . . . ?
F10' C10' C11' F11' 1.8(3) . . . . ?
C9' C10' C11' F11' -177.69(16) . . . . ?
F10' C10' C11' C12' -177.72(15) . . . . ?
C9' C10' C11' C12' 2.8(3) . . . . ?
F11' C11' C12' F12' -0.1(2) . . . . ?
C10' C11' C12' F12' 179.38(15) . . . . ?
F11' C11' C12' C7' -179.68(15) . . . . ?
C10' C11' C12' C7' -0.2(3) . . . . ?
C8' C7' C12' F12' 176.78(14) . . . . ?
B1 C7' C12' F12' 0.7(3) . . . . ?
C8' C7' C12' C11' -3.7(2) . . . . ?
B1 C7' C12' C11' -179.78(16) . . . . ?
C19' B1 C13' C18' -103.30(19) . . . . ?
C1' B1 C13' C18' 133.33(17) . . . . ?
C7' B1 C13' C18' 18.4(2) . . . . ?
C19' B1 C13' C14' 72.04(18) . . . . ?
C1' B1 C13' C14' -51.3(2) . . . . ?
C7' B1 C13' C14' -166.25(15) . . . . ?
C18' C13' C14' F14' 177.86(14) . . . . ?
B1 C13' C14' F14' 1.9(2) . . . . ?
C18' C13' C14' C15' -2.5(2) . . . . ?
B1 C13' C14' C15' -178.48(16) . . . . ?
F14' C14' C15' F15' 1.0(2) . . . . ?
C13' C14' C15' F15' -178.68(15) . . . . ?
F14' C14' C15' C16' -179.34(15) . . . . ?
C13' C14' C15' C16' 1.0(3) . . . . ?
F15' C15' C16' F16' 1.1(3) . . . . ?
C14' C15' C16' F16' -178.56(15) . . . . ?
F15' C15' C16' C17' -179.51(15) . . . . ?
C14' C15' C16' C17' 0.8(3) . . . . ?
F16' C16' C17' F17' -1.9(3) . . . . ?
C15' C16' C17' F17' 178.76(15) . . . . ?
F16' C16' C17' C18' 178.48(15) . . . . ?
C15' C16' C17' C18' -0.9(3) . . . . ?
F17' C17' C18' F18' -0.8(2) . . . . ?
C16' C17' C18' F18' 178.82(15) . . . . ?
F17' C17' C18' C13' 179.53(15) . . . . ?
C16' C17' C18' C13' -0.8(3) . . . . ?
C14' C13' C18' F18' -177.24(15) . . . . ?
B1 C13' C18' F18' -1.6(3) . . . . ?
C14' C13' C18' C17' 2.4(2) . . . . ?
B1 C13' C18' C17' 178.01(16) . . . . ?
C1' B1 C19' C20' 20.0(2) . . . . ?
C7' B1 C19' C20' 135.51(17) . . . . ?
C13' B1 C19' C20' -103.02(19) . . . . ?
C1' B1 C19' C24' -164.89(15) . . . . ?
C7' B1 C19' C24' -49.4(2) . . . . ?
C13' B1 C19' C24' 72.09(18) . . . . ?
C24' C19' C20' F20' -178.17(15) . . . . ?
B1 C19' C20' F20' -2.8(3) . . . . ?
C24' C19' C20' C21' 1.5(3) . . . . ?
B1 C19' C20' C21' 176.90(17) . . . . ?
F20' C20' C21' F21' -0.5(2) . . . . ?
C19' C20' C21' F21' 179.79(16) . . . . ?
F20' C20' C21' C22' 179.55(16) . . . . ?
C19' C20' C21' C22' -0.1(3) . . . . ?
F21' C21' C22' F22' 0.0(3) . . . . ?
C20' C21' C22' F22' 179.99(16) . . . . ?
F21' C21' C22' C23' 178.93(16) . . . . ?
C20' C21' C22' C23' -1.1(3) . . . . ?
F22' C22' C23' F23' 0.2(3) . . . . ?
C21' C22' C23' F23' -178.64(16) . . . . ?
F22' C22' C23' C24' 179.78(16) . . . . ?
C21' C22' C23' C24' 0.9(3) . . . . ?
F23' C23' C24' F24' 0.6(2) . . . . ?
C22' C23' C24' F24' -178.92(15) . . . . ?
F23' C23' C24' C19' -179.82(16) . . . . ?
C22' C23' C24' C19' 0.6(3) . . . . ?
C20' C19' C24' F24' 177.76(14) . . . . ?
B1 C19' C24' F24' 2.0(2) . . . . ?
C20' C19' C24' C23' -1.8(3) . . . . ?
B1 C19' C24' C23' -177.52(16) . . . . ?
C9 N1 C1 C2 -176.66(15) . . . . ?
C6 N1 C1 C2 1.5(2) . . . . ?
C9 N1 C1 Fe1 4.3(2) . . . . ?
C6 N1 C1 Fe1 -177.55(12) . . . . ?
N1 C1 C2 C4 -137.08(15) . . . . ?
Fe1 C1 C2 C4 41.9(2) . . . . ?
N1 C1 C2 C3 103.56(16) . . . . ?
Fe1 C1 C2 C3 -77.44(17) . . . . ?
N1 C1 C2 C5 -15.11(18) . . . . ?
Fe1 C1 C2 C5 163.90(12) . . . . ?
C1 C2 C5 C6 22.96(18) . . . . ?
C4 C2 C5 C6 142.93(15) . . . . ?
C3 C2 C5 C6 -92.89(17) . . . . ?
C1 N1 C6 C8 132.25(17) . . . . ?
C9 N1 C6 C8 -49.6(2) . . . . ?
C1 N1 C6 C7 -107.28(17) . . . . ?
C9 N1 C6 C7 70.8(2) . . . . ?
C1 N1 C6 C5 12.77(19) . . . . ?
C9 N1 C6 C5 -169.12(15) . . . . ?
C2 C5 C6 C8 -139.95(16) . . . . ?
C2 C5 C6 C7 96.36(17) . . . . ?
C2 C5 C6 N1 -21.08(17) . . . . ?
C1 N1 C9 C10 -92.3(2) . . . . ?
C6 N1 C9 C10 89.7(2) . . . . ?
C1 N1 C9 C14 85.2(2) . . . . ?
C6 N1 C9 C14 -92.8(2) . . . . ?
C14 C9 C10 C11 4.5(3) . . . . ?
N1 C9 C10 C11 -178.08(15) . . . . ?
C14 C9 C10 C18 -169.90(16) . . . . ?
N1 C9 C10 C18 7.5(3) . . . . ?
C19 C18 C10 C11 -72.1(2) . . . . ?
C20 C18 C10 C11 51.3(2) . . . . ?
C19 C18 C10 C9 102.2(2) . . . . ?
C20 C18 C10 C9 -134.31(18) . . . . ?
C9 C10 C11 C12 0.0(3) . . . . ?
C18 C10 C11 C12 174.59(17) . . . . ?
C10 C11 C12 C13 -3.5(3) . . . . ?
C11 C12 C13 C14 2.7(3) . . . . ?
C12 C13 C14 C9 1.6(3) . . . . ?
C12 C13 C14 C15 -173.19(16) . . . . ?
C10 C9 C14 C13 -5.3(3) . . . . ?
N1 C9 C14 C13 177.34(15) . . . . ?
C10 C9 C14 C15 169.27(16) . . . . ?
N1 C9 C14 C15 -8.1(2) . . . . ?
C13 C14 C15 C16 -50.4(2) . . . . ?
C9 C14 C15 C16 135.11(18) . . . . ?
C13 C14 C15 C17 73.0(2) . . . . ?
C9 C14 C15 C17 -101.4(2) . . . . ?
F1 C1T C2T C3T -179.5(5) . . . . ?
C6T C1T C2T C3T -0.5(7) . . . . ?
C1T C2T C3T C4T -0.4(7) . . . . ?
C2T C3T C4T C5T 0.8(8) . . . . ?
C3T C4T C5T C6T -0.4(8) . . . . ?
C4T C5T C6T C1T -0.5(7) . . . . ?
F1 C1T C6T C5T 179.9(4) . . . . ?
C2T C1T C6T C5T 1.0(7) . . . . ?
F1A C1TA C2TA C3TA -173.6(13) . . . . ?
C6TA C1TA C2TA C3TA -1.0(15) . . . . ?
C1TA C2TA C3TA F1C -176.1(17) . . . . ?
C1TA C2TA C3TA C4TA 0.0(15) . . . . ?
F1C C3TA C4TA C5TA 177.7(15) . . . . ?
C2TA C3TA C4TA C5TA 0.9(19) . . . . ?
C3TA C4TA C5TA F1B 180(2) . . . . ?
C3TA C4TA C5TA C6TA -1(2) . . . . ?
F1B C5TA C6TA C1TA 179(3) . . . . ?
C4TA C5TA C6TA C1TA 0(2) . . . . ?
F1A C1TA C6TA C5TA 173.9(13) . . . . ?
C2TA C1TA C6TA C5TA 1.1(19) . . . . ?
 
_refine_diff_density_max    0.328
_refine_diff_density_min   -0.409
_refine_diff_density_rms    0.048

_shelxl_version_number 2014-3



