 
data_mm109_0m 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C40 H46 Dy2 N8 O14' 
_chemical_formula_weight          1187.85
 
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' 
 'Dy'  'Dy'  -0.1892   4.4098 
 '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' 
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P -1' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    10.4807(5) 
_cell_length_b                    10.5015(5) 
_cell_length_c                    11.4678(5) 
_cell_angle_alpha                 64.937(2) 
_cell_angle_beta                  66.519(2) 
_cell_angle_gamma                 79.936(2) 
_cell_volume                      1048.63(8) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     100(1) 
_cell_measurement_reflns_used     9309 
_cell_measurement_theta_min       2.341 
_cell_measurement_theta_max       36.318 
 
_exptl_crystal_description        rod 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.881 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              586 
_exptl_absorpt_coefficient_mu     3.614 
_exptl_absorpt_correction_type    MULTI-SCAN 
_exptl_absorpt_correction_T_min   0.5318 
_exptl_absorpt_correction_T_max   0.6709 
_exptl_absorpt_process_details    sadabs 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(1) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker Kappa APEXII CCD'
_diffrn_measurement_method        ' φ & ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          0 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             56987 
_diffrn_reflns_av_R_equivalents   0.0250 
_diffrn_reflns_av_sigmaI/netI     0.0172 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        17 
_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          2.12 
_diffrn_reflns_theta_max          36.43 
_reflns_number_total              10134 
_reflns_number_gt                 9729 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'APEX2 (Bruker, 2006)'
_computing_cell_refinement        'SAINT (Bruker, 2006)' 
_computing_data_reduction         'SAINT (Bruker, 2006)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0197P)²+0.1937P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     refall 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          10134 
_refine_ls_number_parameters      381 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0155 
_refine_ls_R_factor_gt            0.0145 
_refine_ls_wR_factor_ref          0.0358 
_refine_ls_wR_factor_gt           0.0354 
_refine_ls_goodness_of_fit_ref    1.072 
_refine_ls_restrained_S_all       1.072 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Dy1 Dy 0.145947(4) 0.087075(4) -0.005196(4) 0.00785(1) Uani 1 1 d . . . 
O1 O 0.07517(9) -0.30517(8) 0.43055(8) 0.01599(13) Uani 1 1 d . . . 
O2 O 0.18126(8) -0.08860(8) 0.16995(8) 0.01373(13) Uani 1 1 d . . . 
O3 O -0.09153(7) 0.03782(7) 0.10408(7) 0.00976(11) Uani 1 1 d . . . 
O4 O -0.21883(9) -0.07842(8) 0.37896(8) 0.01409(13) Uani 1 1 d . . . 
O5 O 0.27249(9) 0.25123(9) 0.00672(8) 0.01580(13) Uani 1 1 d . . . 
O6 O 0.07485(9) 0.18648(9) 0.17558(9) 0.01669(14) Uani 1 1 d . . . 
O7 O 0.21749(11) 0.30838(10) 0.18311(10) 0.02343(17) Uani 1 1 d . . . 
N1 N 0.38414(9) -0.00947(9) -0.09671(9) 0.01195(13) Uani 1 1 d . . . 
N2 N 0.28585(9) 0.24159(9) -0.25218(9) 0.01159(13) Uani 1 1 d . . . 
N3 N 0.01218(9) 0.29968(9) -0.11161(9) 0.01160(13) Uani 1 1 d . . . 
N4 N 0.18806(10) 0.25018(9) 0.12463(9) 0.01302(14) Uani 1 1 d . . . 
C1 C 0.09827(15) -0.20467(15) 0.47412(13) 0.0234(2) Uani 1 1 d . . . 
C2 C 0.18724(11) -0.32528(10) 0.32441(10) 0.01263(15) Uani 1 1 d . . . 
C3 C 0.23938(12) -0.46059(11) 0.34542(11) 0.01552(17) Uani 1 1 d . . . 
C4 C 0.35208(12) -0.48931(11) 0.24157(12) 0.01590(17) Uani 1 1 d . . . 
C5 C 0.41309(11) -0.38019(11) 0.11705(11) 0.01425(16) Uani 1 1 d . . . 
C6 C 0.35845(10) -0.24241(10) 0.09112(10) 0.01183(15) Uani 1 1 d . . . 
C7 C 0.24046(10) -0.21261(10) 0.19317(10) 0.01138(15) Uani 1 1 d . . . 
C8 C 0.42793(10) -0.13535(11) -0.04344(10) 0.01269(15) Uani 1 1 d . . . 
C9 C 0.47722(11) 0.07457(11) -0.23768(11) 0.01501(17) Uani 1 1 d . . . 
C10 C 0.43566(11) 0.22859(11) -0.27754(10) 0.01371(16) Uani 1 1 d . . . 
C11 C 0.23571(11) 0.38837(10) -0.28997(10) 0.01333(16) Uani 1 1 d . . . 
C12 C 0.08114(11) 0.38819(11) -0.25868(10) 0.01483(16) Uani 1 1 d . . . 
C13 C -0.10886(11) 0.33936(10) -0.04888(10) 0.01197(15) Uani 1 1 d . . . 
C14 C -0.19146(10) 0.26445(10) 0.09721(10) 0.01062(14) Uani 1 1 d . . . 
C15 C -0.28677(11) 0.34444(10) 0.16639(11) 0.01360(16) Uani 1 1 d . . . 
C16 C -0.35840(12) 0.28458(11) 0.30716(11) 0.01558(17) Uani 1 1 d . . . 
C17 C -0.33650(11) 0.14264(11) 0.38118(11) 0.01431(16) Uani 1 1 d . . . 
C18 C -0.24584(10) 0.06117(10) 0.31341(10) 0.01089(14) Uani 1 1 d . . . 
C19 C -0.17436(10) 0.11928(9) 0.16867(9) 0.00938(13) Uani 1 1 d . . . 
C20 C -0.25494(13) -0.13110(12) 0.52508(11) 0.01762(18) Uani 1 1 d . . . 
H1 H -0.422(2) 0.3410(19) 0.3547(19) 0.021(4) Uiso 1 1 d . . . 
H2 H -0.383(2) 0.1024(19) 0.477(2) 0.024(4) Uiso 1 1 d . . . 
H3 H -0.2942(18) 0.4374(18) 0.1161(18) 0.018(4) Uiso 1 1 d . . . 
H4 H -0.221(2) -0.076(2) 0.547(2) 0.024(4) Uiso 1 1 d . . . 
H5 H -0.2162(19) -0.2229(19) 0.5522(19) 0.022(4) Uiso 1 1 d . . . 
H6 H -0.356(2) -0.140(2) 0.574(2) 0.028(5) Uiso 1 1 d . . . 
H7 H -0.1481(19) 0.4251(18) -0.1002(18) 0.020(4) Uiso 1 1 d . . . 
H8 H 0.042(2) 0.485(2) -0.283(2) 0.023(4) Uiso 1 1 d . . . 
H9 H 0.0645(18) 0.3455(17) -0.3146(18) 0.016(4) Uiso 1 1 d . . . 
H10 H 0.2844(19) 0.4433(18) -0.3831(19) 0.019(4) Uiso 1 1 d . . . 
H11 H 0.2568(17) 0.4265(17) -0.2392(17) 0.013(4) Uiso 1 1 d . . . 
H12 H 0.2679(18) 0.2070(17) -0.3027(17) 0.015(4) Uiso 1 1 d . . . 
H13 H 0.4562(17) 0.2661(16) -0.2238(17) 0.012(3) Uiso 1 1 d . . . 
H14 H 0.490(2) 0.287(2) -0.379(2) 0.029(5) Uiso 1 1 d . . . 
H15 H 0.5778(19) 0.0617(19) -0.2430(19) 0.021(4) Uiso 1 1 d . . . 
H16 H 0.4629(18) 0.0404(17) -0.3007(17) 0.014(4) Uiso 1 1 d . . . 
H17 H 0.516(2) -0.176(2) -0.087(2) 0.028(5) Uiso 1 1 d . . . 
H18 H 0.4932(18) -0.3946(18) 0.0455(18) 0.017(4) Uiso 1 1 d . . . 
H19 H 0.3864(18) -0.5815(18) 0.2555(18) 0.016(4) Uiso 1 1 d . . . 
H20 H 0.025(2) -0.215(2) 0.558(2) 0.024(4) Uiso 1 1 d . . . 
H21 H 0.100(2) -0.112(2) 0.408(2) 0.030(5) Uiso 1 1 d . . . 
H22 H 0.1913(19) -0.5303(19) 0.4292(19) 0.020(4) Uiso 1 1 d . . . 
H23 H 0.183(3) -0.221(2) 0.481(2) 0.044(6) Uiso 1 1 d . . . 
 
 
_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 
Dy1 O2 2.1884(7) . ? 
Dy1 O3 2.3169(7) 2 ? 
Dy1 O3 2.3341(7) . ? 
Dy1 O5 2.4275(8) . ? 
Dy1 O6 2.5046(8) . ? 
Dy1 N1 2.5081(9) . ? 
Dy1 N3 2.5300(8) . ? 
Dy1 N2 2.5365(8) . ? 
Dy1 N4 2.8799(8) . ? 
Dy1 Dy1 3.76804(17) 2 ? 
O1 C2 1.3775(13) . ? 
O1 C1 1.4333(15) . ? 
O2 C7 1.3066(12) . ? 
O3 C19 1.3413(11) . ? 
O3 Dy1 2.3169(7) 2 ? 
O4 C18 1.3730(12) . ? 
O4 C20 1.4282(13) . ? 
O5 N4 1.2841(12) . ? 
O6 N4 1.2611(12) . ? 
O7 N4 1.2232(11) . ? 
N1 C8 1.2878(13) . ? 
N1 C9 1.4763(13) . ? 
N2 C10 1.4708(14) . ? 
N2 C11 1.4738(13) . ? 
N2 H12 0.890(17) . ? 
N3 C13 1.2815(13) . ? 
N3 C12 1.4718(13) . ? 
C1 H20 0.932(19) . ? 
C1 H21 0.94(2) . ? 
C1 H23 0.90(2) . ? 
C2 C3 1.3854(14) . ? 
C2 C7 1.4245(14) . ? 
C3 C4 1.4012(16) . ? 
C3 H22 0.927(19) . ? 
C4 C5 1.3796(16) . ? 
C4 H19 0.941(17) . ? 
C5 C6 1.4112(14) . ? 
C5 H18 0.955(17) . ? 
C6 C7 1.4208(14) . ? 
C6 C8 1.4479(14) . ? 
C8 H17 0.98(2) . ? 
C9 C10 1.5169(15) . ? 
C9 H15 1.019(18) . ? 
C9 H16 0.999(17) . ? 
C10 H13 0.960(16) . ? 
C10 H14 1.02(2) . ? 
C11 C12 1.5135(15) . ? 
C11 H10 0.938(18) . ? 
C11 H11 0.938(16) . ? 
C12 H8 0.988(18) . ? 
C12 H9 1.001(17) . ? 
C13 C14 1.4631(14) . ? 
C13 H7 0.970(17) . ? 
C14 C15 1.4045(13) . ? 
C14 C19 1.4111(13) . ? 
C15 C16 1.3800(15) . ? 
C15 H3 0.907(17) . ? 
C16 C17 1.3996(15) . ? 
C16 H1 0.968(18) . ? 
C17 C18 1.3891(13) . ? 
C17 H2 0.933(19) . ? 
C18 C19 1.4140(13) . ? 
C20 H4 0.890(19) . ? 
C20 H5 0.949(18) . ? 
C20 H6 0.98(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 
O2 Dy1 O3 99.35(3) . 2 ? 
O2 Dy1 O3 88.96(3) . . ? 
O3 Dy1 O3 71.78(3) 2 . ? 
O2 Dy1 O5 93.12(3) . . ? 
O3 Dy1 O5 157.14(3) 2 . ? 
O3 Dy1 O5 127.88(3) . . ? 
O2 Dy1 O6 76.84(3) . . ? 
O3 Dy1 O6 149.81(3) 2 . ? 
O3 Dy1 O6 78.18(2) . . ? 
O5 Dy1 O6 52.02(3) . . ? 
O2 Dy1 N1 72.87(3) . . ? 
O3 Dy1 N1 82.03(3) 2 . ? 
O3 Dy1 N1 145.25(3) . . ? 
O5 Dy1 N1 83.46(3) . . ? 
O6 Dy1 N1 123.72(3) . . ? 
O2 Dy1 N3 153.18(3) . . ? 
O3 Dy1 N3 91.27(3) 2 . ? 
O3 Dy1 N3 70.99(3) . . ? 
O5 Dy1 N3 85.94(3) . . ? 
O6 Dy1 N3 81.61(3) . . ? 
N1 Dy1 N3 133.36(3) . . ? 
O2 Dy1 N2 138.51(3) . . ? 
O3 Dy1 N2 84.87(3) 2 . ? 
O3 Dy1 N2 130.61(3) . . ? 
O5 Dy1 N2 73.18(3) . . ? 
O6 Dy1 N2 118.07(3) . . ? 
N1 Dy1 N2 66.86(3) . . ? 
N3 Dy1 N2 66.59(3) . . ? 
O2 Dy1 N4 82.44(3) . . ? 
O3 Dy1 N4 174.90(3) 2 . ? 
O3 Dy1 N4 103.57(2) . . ? 
O5 Dy1 N4 26.27(3) . . ? 
O6 Dy1 N4 25.91(3) . . ? 
N1 Dy1 N4 103.07(3) . . ? 
N3 Dy1 N4 85.14(3) . . ? 
N2 Dy1 N4 96.97(3) . . ? 
O2 Dy1 Dy1 95.09(2) . 2 ? 
O3 Dy1 Dy1 36.042(18) 2 2 ? 
O3 Dy1 Dy1 35.737(16) . 2 ? 
O5 Dy1 Dy1 161.26(2) . 2 ? 
O6 Dy1 Dy1 113.865(19) . 2 ? 
N1 Dy1 Dy1 115.07(2) . 2 ? 
N3 Dy1 Dy1 79.15(2) . 2 ? 
N2 Dy1 Dy1 110.38(2) . 2 ? 
N4 Dy1 Dy1 139.267(19) . 2 ? 
C2 O1 C1 114.27(9) . . ? 
C7 O2 Dy1 137.33(6) . . ? 
C19 O3 Dy1 128.90(6) . 2 ? 
C19 O3 Dy1 118.14(6) . . ? 
Dy1 O3 Dy1 108.22(3) 2 . ? 
C18 O4 C20 117.06(8) . . ? 
N4 O5 Dy1 96.93(6) . . ? 
N4 O6 Dy1 93.91(6) . . ? 
C8 N1 C9 114.40(9) . . ? 
C8 N1 Dy1 126.65(7) . . ? 
C9 N1 Dy1 117.95(6) . . ? 
C10 N2 C11 113.06(8) . . ? 
C10 N2 Dy1 110.99(6) . . ? 
C11 N2 Dy1 111.94(6) . . ? 
C10 N2 H12 109.4(11) . . ? 
C11 N2 H12 107.1(11) . . ? 
Dy1 N2 H12 103.8(11) . . ? 
C13 N3 C12 116.83(8) . . ? 
C13 N3 Dy1 126.17(7) . . ? 
C12 N3 Dy1 116.98(6) . . ? 
O7 N4 O6 122.54(9) . . ? 
O7 N4 O5 120.99(9) . . ? 
O6 N4 O5 116.47(8) . . ? 
O7 N4 Dy1 172.64(8) . . ? 
O6 N4 Dy1 60.19(5) . . ? 
O5 N4 Dy1 56.80(5) . . ? 
O1 C1 H20 106.2(12) . . ? 
O1 C1 H21 111.0(12) . . ? 
H20 C1 H21 111.1(17) . . ? 
O1 C1 H23 108.5(15) . . ? 
H20 C1 H23 113.5(19) . . ? 
H21 C1 H23 106.5(19) . . ? 
O1 C2 C3 117.99(9) . . ? 
O1 C2 C7 120.95(9) . . ? 
C3 C2 C7 120.85(9) . . ? 
C2 C3 C4 121.19(10) . . ? 
C2 C3 H22 115.8(11) . . ? 
C4 C3 H22 122.9(11) . . ? 
C5 C4 C3 119.16(9) . . ? 
C5 C4 H19 119.8(11) . . ? 
C3 C4 H19 121.1(11) . . ? 
C4 C5 C6 120.70(10) . . ? 
C4 C5 H18 121.7(10) . . ? 
C6 C5 H18 117.6(10) . . ? 
C5 C6 C7 120.79(9) . . ? 
C5 C6 C8 116.72(9) . . ? 
C7 C6 C8 122.49(9) . . ? 
O2 C7 C6 122.59(9) . . ? 
O2 C7 C2 120.45(9) . . ? 
C6 C7 C2 116.95(9) . . ? 
N1 C8 C6 127.02(9) . . ? 
N1 C8 H17 126.0(11) . . ? 
C6 C8 H17 106.9(11) . . ? 
N1 C9 C10 110.23(8) . . ? 
N1 C9 H15 110.0(10) . . ? 
C10 C9 H15 110.4(10) . . ? 
N1 C9 H16 106.3(10) . . ? 
C10 C9 H16 108.2(9) . . ? 
H15 C9 H16 111.7(14) . . ? 
N2 C10 C9 108.99(8) . . ? 
N2 C10 H13 110.0(10) . . ? 
C9 C10 H13 109.8(9) . . ? 
N2 C10 H14 109.7(12) . . ? 
C9 C10 H14 111.5(11) . . ? 
H13 C10 H14 106.8(15) . . ? 
N2 C11 C12 108.18(8) . . ? 
N2 C11 H10 111.2(11) . . ? 
C12 C11 H10 111.6(11) . . ? 
N2 C11 H11 107.6(10) . . ? 
C12 C11 H11 112.6(10) . . ? 
H10 C11 H11 105.5(15) . . ? 
N3 C12 C11 108.49(8) . . ? 
N3 C12 H8 111.9(11) . . ? 
C11 C12 H8 111.6(11) . . ? 
N3 C12 H9 108.0(10) . . ? 
C11 C12 H9 109.3(10) . . ? 
H8 C12 H9 107.5(14) . . ? 
N3 C13 C14 123.99(9) . . ? 
N3 C13 H7 118.5(11) . . ? 
C14 C13 H7 117.5(11) . . ? 
C15 C14 C19 120.55(9) . . ? 
C15 C14 C13 117.05(8) . . ? 
C19 C14 C13 122.36(8) . . ? 
C16 C15 C14 120.56(9) . . ? 
C16 C15 H3 121.9(11) . . ? 
C14 C15 H3 117.4(11) . . ? 
C15 C16 C17 119.59(9) . . ? 
C15 C16 H1 120.1(11) . . ? 
C17 C16 H1 120.3(11) . . ? 
C18 C17 C16 120.45(9) . . ? 
C18 C17 H2 119.8(11) . . ? 
C16 C17 H2 119.8(11) . . ? 
O4 C18 C17 123.78(9) . . ? 
O4 C18 C19 115.30(8) . . ? 
C17 C18 C19 120.92(9) . . ? 
O3 C19 C14 122.13(8) . . ? 
O3 C19 C18 120.17(8) . . ? 
C14 C19 C18 117.68(8) . . ? 
O4 C20 H4 110.3(12) . . ? 
O4 C20 H5 106.8(11) . . ? 
H4 C20 H5 110.8(16) . . ? 
O4 C20 H6 111.1(12) . . ? 
H4 C20 H6 110.3(17) . . ? 
H5 C20 H6 107.4(16) . . ? 
 
_diffrn_measured_fraction_theta_max    0.988 
_diffrn_reflns_theta_full              36.43 
_diffrn_measured_fraction_theta_full   0.988 
_refine_diff_density_max    1.117 
_refine_diff_density_min   -0.657 
_refine_diff_density_rms    0.093 
 
data_mm008a 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C40 H46 Eu2 N8 O14' 
_chemical_formula_weight          1166.77 
  
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Eu'  'Eu'  -0.1578   3.6682 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    10.5977(5) 
_cell_length_b                    10.6420(5) 
_cell_length_c                    11.5192(6) 
_cell_angle_alpha                 65.341(2) 
_cell_angle_beta                  64.813(2) 
_cell_angle_gamma                 80.419(2) 
_cell_volume                      1068.32(9) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     9973 
_cell_measurement_theta_min       2.34 
_cell_measurement_theta_max       30.50 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.23 
_exptl_crystal_size_mid           0.14 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.814 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              580 
_exptl_absorpt_coefficient_mu     2.986 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5467 
_exptl_absorpt_correction_T_max   0.7158 
_exptl_absorpt_process_details    'SADABS, Bruker (2003)' 
  
_exptl_special_details 
; 
 Data collection is performed with four batch runs at phi = 0.00 deg 
 (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg 
 (600 frames), and at phi = 270.00 deg (600 frames). 
 A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor 
 crystal and diffractometer stability. Frame width = 0.30 deg in omega. 
 Data is merged, corrected for decay (if any), and treated with multi-scan 
 absorption corrections (if required). All symmetry-equivalent reflections 
 are merged for centrosymmetric data. 
 Friedel pairs are not merged for noncentrosymmetric data. 
; 
  
_diffrn_ambient_temperature       200(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             19057 
_diffrn_reflns_av_R_equivalents   0.0195 
_diffrn_reflns_av_sigmaI/netI     0.0208 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.12 
_diffrn_reflns_theta_max          30.54 
_reflns_number_total              6170 
_reflns_number_gt                 5886 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'APEX II, Bruker (2009)' 
_computing_cell_refinement        'APEX II, Bruker (2009)' 
_computing_data_reduction         'XPREP, Bruker (2009)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'SHELXTL, Bruker (2004)' 
_computing_publication_material   'SHELXTL, Bruker (2004)' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0253P)²+0.3377P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6170 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0194 
_refine_ls_R_factor_gt            0.0181 
_refine_ls_wR_factor_ref          0.0447 
_refine_ls_wR_factor_gt           0.0440 
_refine_ls_goodness_of_fit_ref    1.058 
_refine_ls_restrained_S_all       1.058 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Eu1 Eu 0.649559(7) 0.580112(8) -0.000901(7) 0.01666(3) Uani 1 1 d . . . 
N1 N 0.89291(15) 0.48538(17) -0.09391(15) 0.0227(3) Uani 1 1 d . . . 
N2 N 0.80461(15) 0.73081(16) -0.25225(15) 0.0229(3) Uani 1 1 d . . . 
H2A H 0.7969 0.6938 -0.3092 0.027 Uiso 1 1 calc R . . 
N3 N 0.52630(16) 0.79232(16) -0.11721(15) 0.0232(3) Uani 1 1 d . . . 
N4 N 0.68304(17) 0.74551(18) 0.13189(17) 0.0286(3) Uani 1 1 d . . . 
O1 O 0.67795(13) 0.40070(14) 0.17497(13) 0.0257(3) Uani 1 1 d . . . 
O2 O 0.57164(14) 0.18759(15) 0.43591(14) 0.0310(3) Uani 1 1 d . . . 
O3 O 0.40355(12) 0.54210(13) 0.10649(12) 0.0198(2) Uani 1 1 d . . . 
O4 O 0.22808(19) 0.43701(16) 0.38501(15) 0.0388(4) Uani 1 1 d . . . 
O5 O 0.77071(15) 0.74877(17) 0.01321(14) 0.0338(3) Uani 1 1 d . . . 
O6 O 0.57223(14) 0.67716(17) 0.18418(15) 0.0335(3) Uani 1 1 d . . . 
O7 O 0.7060(2) 0.8054(2) 0.1904(2) 0.0585(6) Uani 1 1 d . . . 
C1 C 0.73615(18) 0.27979(19) 0.19440(18) 0.0219(3) Uani 1 1 d . . . 
C2 C 0.68219(19) 0.1674(2) 0.32538(18) 0.0249(3) Uani 1 1 d . . . 
C3 C 0.7316(2) 0.0358(2) 0.3426(2) 0.0311(4) Uani 1 1 d . . . 
H3A H 0.6888 -0.0386 0.4292 0.037 Uiso 1 1 calc R . . 
C4 C 0.8439(2) 0.0094(2) 0.2350(2) 0.0322(4) Uani 1 1 d . . . 
H4A H 0.8758 -0.0823 0.2474 0.039 Uiso 1 1 calc R . . 
C5 C 0.9074(2) 0.1177(2) 0.1112(2) 0.0281(4) Uani 1 1 d . . . 
H5A H 0.9877 0.1015 0.0399 0.034 Uiso 1 1 calc R . . 
C6 C 0.85501(18) 0.2523(2) 0.08867(18) 0.0230(3) Uani 1 1 d . . . 
C7 C 0.6091(3) 0.2714(3) 0.4871(2) 0.0414(5) Uani 1 1 d . . . 
H7A H 0.5275 0.2825 0.5650 0.062 Uiso 1 1 calc R . . 
H7B H 0.6417 0.3624 0.4125 0.062 Uiso 1 1 calc R . . 
H7C H 0.6836 0.2266 0.5189 0.062 Uiso 1 1 calc R . . 
C8 C 0.92959(17) 0.3601(2) -0.04458(18) 0.0242(3) Uani 1 1 d . . . 
H8A H 1.0161 0.3348 -0.1022 0.029 Uiso 1 1 calc R . . 
C9 C 0.99429(19) 0.5710(2) -0.23240(19) 0.0291(4) Uani 1 1 d . . . 
H9A H 0.9991 0.5376 -0.3025 0.035 Uiso 1 1 calc R . . 
H9B H 1.0880 0.5622 -0.2307 0.035 Uiso 1 1 calc R . . 
C10 C 0.95242(18) 0.7203(2) -0.27266(18) 0.0265(4) Uani 1 1 d . . . 
H10A H 0.9665 0.7596 -0.2148 0.032 Uiso 1 1 calc R . . 
H10B H 1.0112 0.7736 -0.3714 0.032 Uiso 1 1 calc R . . 
C11 C 0.7573(2) 0.8738(2) -0.29628(19) 0.0283(4) Uani 1 1 d . . . 
H11A H 0.8110 0.9243 -0.3971 0.034 Uiso 1 1 calc R . . 
H11B H 0.7724 0.9212 -0.2452 0.034 Uiso 1 1 calc R . . 
C12 C 0.6033(2) 0.8730(2) -0.26609(19) 0.0290(4) Uani 1 1 d . . . 
H12A H 0.5686 0.9689 -0.2914 0.035 Uiso 1 1 calc R . . 
H12B H 0.5891 0.8314 -0.3222 0.035 Uiso 1 1 calc R . . 
C13 C 0.40814(19) 0.83875(19) -0.05692(19) 0.0242(3) Uani 1 1 d . . . 
H13A H 0.3782 0.9233 -0.1109 0.029 Uiso 1 1 calc R . . 
C14 C 0.31945(16) 0.62749(18) 0.16505(17) 0.0198(3) Uani 1 1 d . . . 
C15 C 0.31589(17) 0.77044(19) 0.08952(18) 0.0218(3) Uani 1 1 d . . . 
C16 C 0.2205(2) 0.8545(2) 0.1527(2) 0.0296(4) Uani 1 1 d . . . 
H16A H 0.2168 0.9501 0.0990 0.035 Uiso 1 1 calc R . . 
C17 C 0.1319(2) 0.8005(3) 0.2917(2) 0.0374(5) Uani 1 1 d . . . 
H17A H 0.0688 0.8585 0.3341 0.045 Uiso 1 1 calc R . . 
C18 C 0.1364(2) 0.6616(2) 0.3676(2) 0.0354(4) Uani 1 1 d . . . 
H18A H 0.0753 0.6236 0.4631 0.042 Uiso 1 1 calc R . . 
C19 C 0.2288(2) 0.5759(2) 0.30729(18) 0.0266(4) Uani 1 1 d . . . 
C20 C 0.3032(5) 0.3992(4) 0.4659(5) 0.0883(14) Uani 1 1 d . . . 
H20A H 0.2953 0.2989 0.5185 0.132 Uiso 1 1 calc R . . 
H20B H 0.2666 0.4463 0.5307 0.132 Uiso 1 1 calc R . . 
H20C H 0.4014 0.4254 0.4063 0.132 Uiso 1 1 calc R . . 
  
  
_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 
Eu1 O1 2.2226(13) . ? 
Eu1 O3 2.3736(11) 2_665 ? 
Eu1 O3 2.3832(11) . ? 
Eu1 O5 2.4668(13) . ? 
Eu1 O6 2.5204(13) . ? 
Eu1 N1 2.5493(15) . ? 
Eu1 N3 2.5660(16) . ? 
Eu1 N2 2.5706(14) . ? 
Eu1 N4 2.9121(15) . ? 
Eu1 C14 3.2668(16) . ? 
Eu1 Eu1 3.8301(2) 2_665 ? 
N1 C8 1.278(3) . ? 
N1 C9 1.478(2) . ? 
N2 C11 1.464(3) . ? 
N2 C10 1.474(2) . ? 
N3 C13 1.279(2) . ? 
N3 C12 1.469(2) . ? 
N4 O7 1.212(2) . ? 
N4 O6 1.260(2) . ? 
N4 O5 1.274(2) . ? 
O1 C1 1.304(2) . ? 
O2 C2 1.384(2) . ? 
O2 C7 1.434(3) . ? 
O3 C14 1.3437(19) . ? 
O3 Eu1 2.3735(11) 2_665 ? 
O4 C19 1.371(2) . ? 
O4 C20 1.369(3) . ? 
C1 C6 1.423(2) . ? 
C1 C2 1.422(3) . ? 
C2 C3 1.374(3) . ? 
C3 C4 1.398(3) . ? 
C4 C5 1.373(3) . ? 
C5 C6 1.405(3) . ? 
C6 C8 1.448(3) . ? 
C9 C10 1.504(3) . ? 
C11 C12 1.517(3) . ? 
C13 C15 1.463(2) . ? 
C14 C15 1.406(3) . ? 
C14 C19 1.412(2) . ? 
C15 C16 1.403(2) . ? 
C16 C17 1.381(3) . ? 
C17 C18 1.373(3) . ? 
C18 C19 1.388(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 Eu1 O3 98.81(5) . 2_665 ? 
O1 Eu1 O3 91.24(5) . . ? 
O3 Eu1 O3 72.74(4) 2_665 . ? 
O1 Eu1 O5 95.38(5) . . ? 
O3 Eu1 O5 157.35(4) 2_665 . ? 
O3 Eu1 O5 124.66(4) . . ? 
O1 Eu1 O6 78.11(5) . . ? 
O3 Eu1 O6 149.64(4) 2_665 . ? 
O3 Eu1 O6 77.11(4) . . ? 
O5 Eu1 O6 51.16(4) . . ? 
O1 Eu1 N1 72.03(5) . . ? 
O3 Eu1 N1 83.23(4) 2_665 . ? 
O3 Eu1 N1 148.32(4) . . ? 
O5 Eu1 N1 84.48(5) . . ? 
O6 Eu1 N1 123.04(5) . . ? 
O1 Eu1 N3 156.06(5) . . ? 
O3 Eu1 N3 89.27(5) 2_665 . ? 
O3 Eu1 N3 69.58(4) . . ? 
O5 Eu1 N3 84.76(5) . . ? 
O6 Eu1 N3 83.54(5) . . ? 
N1 Eu1 N3 131.59(5) . . ? 
O1 Eu1 N2 136.83(5) . . ? 
O3 Eu1 N2 84.31(4) 2_665 . ? 
O3 Eu1 N2 129.87(5) . . ? 
O5 Eu1 N2 73.29(4) . . ? 
O6 Eu1 N2 118.78(5) . . ? 
N1 Eu1 N2 65.58(5) . . ? 
N3 Eu1 N2 66.11(5) . . ? 
O1 Eu1 N4 84.76(5) . . ? 
O3 Eu1 N4 173.26(4) 2_665 . ? 
O3 Eu1 N4 101.58(4) . . ? 
O5 Eu1 N4 25.74(4) . . ? 
O6 Eu1 N4 25.54(4) . . ? 
N1 Eu1 N4 103.36(5) . . ? 
N3 Eu1 N4 85.26(5) . . ? 
N2 Eu1 N4 97.04(5) . . ? 
O1 Eu1 C14 96.91(5) . . ? 
O3 Eu1 C14 91.79(4) 2_665 . ? 
O3 Eu1 C14 20.90(4) . . ? 
O5 Eu1 C14 103.97(4) . . ? 
O6 Eu1 C14 59.13(4) . . ? 
N1 Eu1 C14 166.89(5) . . ? 
N3 Eu1 C14 60.14(5) . . ? 
N2 Eu1 C14 126.14(5) . . ? 
N4 Eu1 C14 82.07(4) . . ? 
O1 Eu1 Eu1 96.22(4) . 2_665 ? 
O3 Eu1 Eu1 36.46(3) 2_665 2_665 ? 
O3 Eu1 Eu1 36.28(3) . 2_665 ? 
O5 Eu1 Eu1 157.78(4) . 2_665 ? 
O6 Eu1 Eu1 113.33(3) . 2_665 ? 
N1 Eu1 Eu1 117.16(3) . 2_665 ? 
N3 Eu1 Eu1 77.00(3) . 2_665 ? 
N2 Eu1 Eu1 109.72(3) . 2_665 ? 
N4 Eu1 Eu1 137.75(3) . 2_665 ? 
C14 Eu1 Eu1 55.81(3) . 2_665 ? 
C8 N1 C9 114.51(15) . . ? 
C8 N1 Eu1 125.74(11) . . ? 
C9 N1 Eu1 118.46(12) . . ? 
C11 N2 C10 113.05(14) . . ? 
C11 N2 Eu1 112.71(10) . . ? 
C10 N2 Eu1 110.81(11) . . ? 
C13 N3 C12 116.93(16) . . ? 
C13 N3 Eu1 126.44(12) . . ? 
C12 N3 Eu1 116.51(12) . . ? 
O7 N4 O6 122.29(17) . . ? 
O7 N4 O5 121.30(17) . . ? 
O6 N4 O5 116.41(14) . . ? 
O7 N4 Eu1 173.91(17) . . ? 
O6 N4 Eu1 59.58(8) . . ? 
O5 N4 Eu1 57.21(8) . . ? 
C1 O1 Eu1 137.32(11) . . ? 
C2 O2 C7 112.71(15) . . ? 
C14 O3 Eu1 127.02(10) . 2_665 ? 
C14 O3 Eu1 119.85(9) . . ? 
Eu1 O3 Eu1 107.26(4) 2_665 . ? 
C19 O4 C20 115.3(2) . . ? 
N4 O5 Eu1 97.05(10) . . ? 
N4 O6 Eu1 94.88(10) . . ? 
O1 C1 C6 122.93(16) . . ? 
O1 C1 C2 120.61(16) . . ? 
C6 C1 C2 116.46(17) . . ? 
C3 C2 O2 118.66(17) . . ? 
C3 C2 C1 121.19(17) . . ? 
O2 C2 C1 120.01(17) . . ? 
C2 C3 C4 121.15(19) . . ? 
C5 C4 C3 119.19(19) . . ? 
C4 C5 C6 120.74(18) . . ? 
C5 C6 C1 120.78(17) . . ? 
C5 C6 C8 116.86(16) . . ? 
C1 C6 C8 122.34(17) . . ? 
N1 C8 C6 127.73(16) . . ? 
N1 C9 C10 110.63(15) . . ? 
N2 C10 C9 109.53(15) . . ? 
N2 C11 C12 108.82(15) . . ? 
N3 C12 C11 109.05(15) . . ? 
N3 C13 C15 124.42(17) . . ? 
O3 C14 C15 122.51(15) . . ? 
O3 C14 C19 120.67(16) . . ? 
C15 C14 C19 116.82(15) . . ? 
O3 C14 Eu1 39.25(7) . . ? 
C15 C14 Eu1 98.03(10) . . ? 
C19 C14 Eu1 132.92(13) . . ? 
C14 C15 C16 120.58(16) . . ? 
C14 C15 C13 122.67(15) . . ? 
C16 C15 C13 116.74(17) . . ? 
C17 C16 C15 121.1(2) . . ? 
C18 C17 C16 118.89(18) . . ? 
C17 C18 C19 121.17(18) . . ? 
O4 C19 C18 119.69(17) . . ? 
O4 C19 C14 118.91(16) . . ? 
C18 C19 C14 121.32(19) . . ? 
  
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 
O1 Eu1 N1 C8 27.87(13) . . . . ? 
O3 Eu1 N1 C8 -73.71(14) 2_665 . . . ? 
O3 Eu1 N1 C8 -33.30(18) . . . . ? 
O5 Eu1 N1 C8 125.36(14) . . . . ? 
O6 Eu1 N1 C8 89.89(14) . . . . ? 
N3 Eu1 N1 C8 -156.67(13) . . . . ? 
N2 Eu1 N1 C8 -160.51(15) . . . . ? 
N4 Eu1 N1 C8 107.75(14) . . . . ? 
C14 Eu1 N1 C8 -5.5(3) . . . . ? 
Eu1 Eu1 N1 C8 -59.93(14) 2_665 . . . ? 
O1 Eu1 N1 C9 -165.89(13) . . . . ? 
O3 Eu1 N1 C9 92.54(12) 2_665 . . . ? 
O3 Eu1 N1 C9 132.95(12) . . . . ? 
O5 Eu1 N1 C9 -68.40(12) . . . . ? 
O6 Eu1 N1 C9 -103.87(13) . . . . ? 
N3 Eu1 N1 C9 9.57(15) . . . . ? 
N2 Eu1 N1 C9 5.73(12) . . . . ? 
N4 Eu1 N1 C9 -86.01(13) . . . . ? 
C14 Eu1 N1 C9 160.73(16) . . . . ? 
Eu1 Eu1 N1 C9 106.31(12) 2_665 . . . ? 
O1 Eu1 N2 C11 -147.89(11) . . . . ? 
O3 Eu1 N2 C11 115.29(11) 2_665 . . . ? 
O3 Eu1 N2 C11 53.44(12) . . . . ? 
O5 Eu1 N2 C11 -68.08(11) . . . . ? 
O6 Eu1 N2 C11 -43.87(12) . . . . ? 
N1 Eu1 N2 C11 -159.58(12) . . . . ? 
N3 Eu1 N2 C11 23.56(11) . . . . ? 
N4 Eu1 N2 C11 -58.06(11) . . . . ? 
C14 Eu1 N2 C11 27.24(13) . . . . ? 
Eu1 Eu1 N2 C11 88.72(11) 2_665 . . . ? 
O1 Eu1 N2 C10 -20.07(14) . . . . ? 
O3 Eu1 N2 C10 -116.89(11) 2_665 . . . ? 
O3 Eu1 N2 C10 -178.74(10) . . . . ? 
O5 Eu1 N2 C10 59.73(11) . . . . ? 
O6 Eu1 N2 C10 83.94(12) . . . . ? 
N1 Eu1 N2 C10 -31.76(11) . . . . ? 
N3 Eu1 N2 C10 151.38(12) . . . . ? 
N4 Eu1 N2 C10 69.76(12) . . . . ? 
C14 Eu1 N2 C10 155.05(10) . . . . ? 
Eu1 Eu1 N2 C10 -143.46(10) 2_665 . . . ? 
O1 Eu1 N3 C13 -3.1(2) . . . . ? 
O3 Eu1 N3 C13 107.31(14) 2_665 . . . ? 
O3 Eu1 N3 C13 35.48(14) . . . . ? 
O5 Eu1 N3 C13 -94.57(14) . . . . ? 
O6 Eu1 N3 C13 -43.14(14) . . . . ? 
N1 Eu1 N3 C13 -172.41(13) . . . . ? 
N2 Eu1 N3 C13 -168.60(16) . . . . ? 
N4 Eu1 N3 C13 -68.74(14) . . . . ? 
C14 Eu1 N3 C13 14.83(13) . . . . ? 
Eu1 Eu1 N3 C13 72.66(14) 2_665 . . . ? 
O1 Eu1 N3 C12 172.87(12) . . . . ? 
O3 Eu1 N3 C12 -76.71(12) 2_665 . . . ? 
O3 Eu1 N3 C12 -148.54(13) . . . . ? 
O5 Eu1 N3 C12 81.41(12) . . . . ? 
O6 Eu1 N3 C12 132.84(12) . . . . ? 
N1 Eu1 N3 C12 3.56(15) . . . . ? 
N2 Eu1 N3 C12 7.38(12) . . . . ? 
N4 Eu1 N3 C12 107.24(12) . . . . ? 
C14 Eu1 N3 C12 -169.19(14) . . . . ? 
Eu1 Eu1 N3 C12 -111.36(12) 2_665 . . . ? 
O1 Eu1 N4 O7 36.3(14) . . . . ? 
O3 Eu1 N4 O7 158.6(12) 2_665 . . . ? 
O3 Eu1 N4 O7 126.5(14) . . . . ? 
O5 Eu1 N4 O7 -77.7(14) . . . . ? 
O6 Eu1 N4 O7 109.6(14) . . . . ? 
N1 Eu1 N4 O7 -33.8(14) . . . . ? 
N3 Eu1 N4 O7 -165.5(14) . . . . ? 
N2 Eu1 N4 O7 -100.3(14) . . . . ? 
C14 Eu1 N4 O7 134.1(14) . . . . ? 
Eu1 Eu1 N4 O7 129.8(14) 2_665 . . . ? 
O1 Eu1 N4 O6 -73.27(12) . . . . ? 
O3 Eu1 N4 O6 49.0(4) 2_665 . . . ? 
O3 Eu1 N4 O6 16.92(13) . . . . ? 
O5 Eu1 N4 O6 172.7(2) . . . . ? 
N1 Eu1 N4 O6 -143.39(12) . . . . ? 
N3 Eu1 N4 O6 84.94(12) . . . . ? 
N2 Eu1 N4 O6 150.12(12) . . . . ? 
C14 Eu1 N4 O6 24.47(12) . . . . ? 
Eu1 Eu1 N4 O6 20.21(14) 2_665 . . . ? 
O1 Eu1 N4 O5 114.03(12) . . . . ? 
O3 Eu1 N4 O5 -123.7(4) 2_665 . . . ? 
O3 Eu1 N4 O5 -155.78(12) . . . . ? 
O6 Eu1 N4 O5 -172.7(2) . . . . ? 
N1 Eu1 N4 O5 43.91(13) . . . . ? 
N3 Eu1 N4 O5 -87.76(12) . . . . ? 
N2 Eu1 N4 O5 -22.58(13) . . . . ? 
C14 Eu1 N4 O5 -148.23(12) . . . . ? 
Eu1 Eu1 N4 O5 -152.49(10) 2_665 . . . ? 
O3 Eu1 O1 C1 41.68(17) 2_665 . . . ? 
O3 Eu1 O1 C1 114.41(16) . . . . ? 
O5 Eu1 O1 C1 -120.61(16) . . . . ? 
O6 Eu1 O1 C1 -169.04(17) . . . . ? 
N1 Eu1 O1 C1 -38.20(16) . . . . ? 
N3 Eu1 O1 C1 150.19(15) . . . . ? 
N2 Eu1 O1 C1 -49.38(19) . . . . ? 
N4 Eu1 O1 C1 -144.08(17) . . . . ? 
C14 Eu1 O1 C1 134.58(16) . . . . ? 
Eu1 Eu1 O1 C1 78.37(16) 2_665 . . . ? 
O1 Eu1 O3 C14 106.31(12) . . . . ? 
O3 Eu1 O3 C14 -154.85(15) 2_665 . . . ? 
O5 Eu1 O3 C14 8.90(14) . . . . ? 
O6 Eu1 O3 C14 28.80(12) . . . . ? 
N1 Eu1 O3 C14 162.76(11) . . . . ? 
N3 Eu1 O3 C14 -59.03(12) . . . . ? 
N2 Eu1 O3 C14 -88.11(12) . . . . ? 
N4 Eu1 O3 C14 21.40(13) . . . . ? 
Eu1 Eu1 O3 C14 -154.85(15) 2_665 . . . ? 
O1 Eu1 O3 Eu1 -98.84(5) . . . 2_665 ? 
O3 Eu1 O3 Eu1 0.0 2_665 . . 2_665 ? 
O5 Eu1 O3 Eu1 163.75(5) . . . 2_665 ? 
O6 Eu1 O3 Eu1 -176.35(6) . . . 2_665 ? 
N1 Eu1 O3 Eu1 -42.38(10) . . . 2_665 ? 
N3 Eu1 O3 Eu1 95.83(6) . . . 2_665 ? 
N2 Eu1 O3 Eu1 66.75(7) . . . 2_665 ? 
N4 Eu1 O3 Eu1 176.26(5) . . . 2_665 ? 
C14 Eu1 O3 Eu1 154.85(15) . . . 2_665 ? 
O7 N4 O5 Eu1 173.0(2) . . . . ? 
O6 N4 O5 Eu1 -7.03(19) . . . . ? 
O1 Eu1 O5 N4 -66.00(12) . . . . ? 
O3 Eu1 O5 N4 165.31(11) 2_665 . . . ? 
O3 Eu1 O5 N4 29.25(14) . . . . ? 
O6 Eu1 O5 N4 4.03(11) . . . . ? 
N1 Eu1 O5 N4 -137.32(12) . . . . ? 
N3 Eu1 O5 N4 89.95(12) . . . . ? 
N2 Eu1 O5 N4 156.56(13) . . . . ? 
C14 Eu1 O5 N4 32.51(13) . . . . ? 
Eu1 Eu1 O5 N4 55.22(17) 2_665 . . . ? 
O7 N4 O6 Eu1 -173.2(2) . . . . ? 
O5 N4 O6 Eu1 6.85(18) . . . . ? 
O1 Eu1 O6 N4 102.94(12) . . . . ? 
O3 Eu1 O6 N4 -169.90(10) 2_665 . . . ? 
O3 Eu1 O6 N4 -163.00(13) . . . . ? 
O5 Eu1 O6 N4 -4.06(11) . . . . ? 
N1 Eu1 O6 N4 43.80(14) . . . . ? 
N3 Eu1 O6 N4 -92.52(12) . . . . ? 
N2 Eu1 O6 N4 -34.34(13) . . . . ? 
C14 Eu1 O6 N4 -151.45(14) . . . . ? 
Eu1 Eu1 O6 N4 -165.35(11) 2_665 . . . ? 
Eu1 O1 C1 C6 30.2(3) . . . . ? 
Eu1 O1 C1 C2 -149.85(13) . . . . ? 
C7 O2 C2 C3 115.2(2) . . . . ? 
C7 O2 C2 C1 -69.0(2) . . . . ? 
O1 C1 C2 C3 172.11(16) . . . . ? 
C6 C1 C2 C3 -8.0(2) . . . . ? 
O1 C1 C2 O2 -3.5(2) . . . . ? 
C6 C1 C2 O2 176.39(15) . . . . ? 
O2 C2 C3 C4 -179.40(17) . . . . ? 
C1 C2 C3 C4 4.9(3) . . . . ? 
C2 C3 C4 C5 1.4(3) . . . . ? 
C3 C4 C5 C6 -4.3(3) . . . . ? 
C4 C5 C6 C1 0.9(3) . . . . ? 
C4 C5 C6 C8 179.41(16) . . . . ? 
O1 C1 C6 C5 -174.98(16) . . . . ? 
C2 C1 C6 C5 5.1(2) . . . . ? 
O1 C1 C6 C8 6.6(3) . . . . ? 
C2 C1 C6 C8 -173.33(15) . . . . ? 
C9 N1 C8 C6 178.61(16) . . . . ? 
Eu1 N1 C8 C6 -14.7(2) . . . . ? 
C5 C6 C8 N1 171.36(17) . . . . ? 
C1 C6 C8 N1 -10.2(3) . . . . ? 
C8 N1 C9 C10 -171.94(15) . . . . ? 
Eu1 N1 C9 C10 20.31(19) . . . . ? 
C11 N2 C10 C9 -176.89(14) . . . . ? 
Eu1 N2 C10 C9 55.48(15) . . . . ? 
N1 C9 C10 N2 -49.62(19) . . . . ? 
C10 N2 C11 C12 -177.94(14) . . . . ? 
Eu1 N2 C11 C12 -51.31(16) . . . . ? 
C13 N3 C12 C11 140.56(17) . . . . ? 
Eu1 N3 C12 C11 -35.82(19) . . . . ? 
N2 C11 C12 N3 57.02(19) . . . . ? 
C12 N3 C13 C15 178.44(16) . . . . ? 
Eu1 N3 C13 C15 -5.6(2) . . . . ? 
Eu1 O3 C14 C15 -90.65(17) 2_665 . . . ? 
Eu1 O3 C14 C15 58.80(18) . . . . ? 
Eu1 O3 C14 C19 88.86(18) 2_665 . . . ? 
Eu1 O3 C14 C19 -121.69(14) . . . . ? 
Eu1 O3 C14 Eu1 -149.45(17) 2_665 . . . ? 
O1 Eu1 C14 O3 -75.14(12) . . . . ? 
O3 Eu1 C14 O3 23.96(14) 2_665 . . . ? 
O5 Eu1 C14 O3 -172.47(12) . . . . ? 
O6 Eu1 C14 O3 -146.83(14) . . . . ? 
N1 Eu1 C14 O3 -43.3(2) . . . . ? 
N3 Eu1 C14 O3 112.09(13) . . . . ? 
N2 Eu1 C14 O3 108.21(12) . . . . ? 
N4 Eu1 C14 O3 -158.84(12) . . . . ? 
Eu1 Eu1 C14 O3 17.70(10) 2_665 . . . ? 
O1 Eu1 C14 C15 151.62(10) . . . . ? 
O3 Eu1 C14 C15 -109.28(10) 2_665 . . . ? 
O3 Eu1 C14 C15 -133.24(17) . . . . ? 
O5 Eu1 C14 C15 54.30(10) . . . . ? 
O6 Eu1 C14 C15 79.93(10) . . . . ? 
N1 Eu1 C14 C15 -176.57(16) . . . . ? 
N3 Eu1 C14 C15 -21.14(9) . . . . ? 
N2 Eu1 C14 C15 -25.02(11) . . . . ? 
N4 Eu1 C14 C15 67.92(10) . . . . ? 
Eu1 Eu1 C14 C15 -115.54(10) 2_665 . . . ? 
O1 Eu1 C14 C19 12.73(16) . . . . ? 
O3 Eu1 C14 C19 111.83(15) 2_665 . . . ? 
O3 Eu1 C14 C19 87.88(19) . . . . ? 
O5 Eu1 C14 C19 -84.59(15) . . . . ? 
O6 Eu1 C14 C19 -58.96(15) . . . . ? 
N1 Eu1 C14 C19 44.5(3) . . . . ? 
N3 Eu1 C14 C19 -160.03(16) . . . . ? 
N2 Eu1 C14 C19 -163.91(14) . . . . ? 
N4 Eu1 C14 C19 -70.96(15) . . . . ? 
Eu1 Eu1 C14 C19 105.58(16) 2_665 . . . ? 
O3 C14 C15 C16 176.10(15) . . . . ? 
C19 C14 C15 C16 -3.4(2) . . . . ? 
Eu1 C14 C15 C16 -150.76(14) . . . . ? 
O3 C14 C15 C13 -3.1(2) . . . . ? 
C19 C14 C15 C13 177.38(15) . . . . ? 
Eu1 C14 C15 C13 30.03(17) . . . . ? 
N3 C13 C15 C14 -24.4(3) . . . . ? 
N3 C13 C15 C16 156.35(17) . . . . ? 
C14 C15 C16 C17 2.7(3) . . . . ? 
C13 C15 C16 C17 -178.01(18) . . . . ? 
C15 C16 C17 C18 -1.2(3) . . . . ? 
C16 C17 C18 C19 0.5(3) . . . . ? 
C20 O4 C19 C18 -83.3(3) . . . . ? 
C20 O4 C19 C14 99.8(3) . . . . ? 
C17 C18 C19 O4 -178.24(19) . . . . ? 
C17 C18 C19 C14 -1.3(3) . . . . ? 
O3 C14 C19 O4 0.1(2) . . . . ? 
C15 C14 C19 O4 179.68(16) . . . . ? 
Eu1 C14 C19 O4 -47.2(2) . . . . ? 
O3 C14 C19 C18 -176.77(17) . . . . ? 
C15 C14 C19 C18 2.8(3) . . . . ? 
Eu1 C14 C19 C18 135.90(17) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.943 
_diffrn_reflns_theta_full              30.54 
_diffrn_measured_fraction_theta_full   0.943 
_refine_diff_density_max    0.954 
_refine_diff_density_min   -0.886 
_refine_diff_density_rms    0.090 
 
data_mm013 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C20 H23 Gd N4 O7' 
_chemical_formula_weight          588.67 
  
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Gd'  'Gd'  -0.1653   3.9035 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    10.5766(5) 
_cell_length_b                    10.5991(5) 
_cell_length_c                    11.5192(5) 
_cell_angle_alpha                 65.1840(10) 
_cell_angle_beta                  65.4820(10) 
_cell_angle_gamma                 80.2930(10) 
_cell_volume                      1066.38(8) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     9916 
_cell_measurement_theta_min       2.33 
_cell_measurement_theta_max       28.40 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             white 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.13 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.833 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              582 
_exptl_absorpt_coefficient_mu     3.160 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5566 
_exptl_absorpt_correction_T_max   0.7029 
_exptl_absorpt_process_details    'SADABS, Bruker (2003)' 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       200(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker APEX-II CCD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             10345 
_diffrn_reflns_av_R_equivalents   0.0709 
_diffrn_reflns_av_sigmaI/netI     0.0490 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.12 
_diffrn_reflns_theta_max          24.71 
_reflns_number_total              3531 
_reflns_number_gt                 3445 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'APEX II, Bruker (2009)' 
_computing_cell_refinement        'APEX II, Bruker (2009)' 
_computing_data_reduction         'XPREP, Bruker (2009)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'SHELXTL, Bruker (2004)' 
_computing_publication_material   'SHELXTL, Bruker (2004)' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0325P)²]' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3531 
_refine_ls_number_parameters      307 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0220 
_refine_ls_R_factor_gt            0.0215 
_refine_ls_wR_factor_ref          0.0534 
_refine_ls_wR_factor_gt           0.0531 
_refine_ls_goodness_of_fit_ref    1.012 
_refine_ls_restrained_S_all       1.012 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Gd1 Gd 0.147938(11) 0.082463(10) 0.498185(11) 0.01723(7) Uani 1 1 d . . . 
N1 N 0.3890(2) -0.0129(2) 0.4060(2) 0.0225(5) Uani 1 1 d . . . 
N2 N 0.2962(2) 0.2346(2) 0.2492(2) 0.0239(5) Uani 1 1 d . . . 
H2A H 0.2862 0.1986 0.1924 0.029 Uiso 1 1 calc R . . 
N3 N 0.0203(2) 0.2955(2) 0.3853(2) 0.0237(5) Uani 1 1 d . . . 
N4 N 0.1839(3) 0.2465(2) 0.6303(3) 0.0285(6) Uani 1 1 d . . . 
O1 O 0.17899(19) -0.09699(18) 0.67432(19) 0.0255(4) Uani 1 1 d . . . 
O2 O 0.0749(2) -0.31217(19) 0.9344(2) 0.0314(4) Uani 1 1 d . . . 
O3 O -0.09507(19) 0.04026(17) 0.60496(19) 0.0203(4) Uani 1 1 d . . . 
O5 O 0.2710(2) 0.2494(2) 0.5123(2) 0.0332(5) Uani 1 1 d . . . 
O6 O 0.0728(2) 0.1788(2) 0.6824(2) 0.0341(5) Uani 1 1 d . . . 
O7 O 0.2085(3) 0.3058(3) 0.6883(3) 0.0539(7) Uani 1 1 d . . . 
C1 C 0.2377(3) -0.2193(3) 0.6957(3) 0.0225(6) Uani 1 1 d . . . 
C2 C 0.1854(3) -0.3308(3) 0.8252(3) 0.0256(6) Uani 1 1 d . . . 
C3 C 0.2364(3) -0.4640(3) 0.8431(3) 0.0326(7) Uani 1 1 d . . . 
H3A H 0.1945 -0.5390 0.9290 0.039 Uiso 1 1 calc R . . 
C4 C 0.3483(3) -0.4895(3) 0.7367(3) 0.0323(7) Uani 1 1 d . . . 
H4A H 0.3820 -0.5814 0.7497 0.039 Uiso 1 1 calc R . . 
C5 C 0.4090(3) -0.3817(3) 0.6137(3) 0.0297(6) Uani 1 1 d . . . 
H5A H 0.4883 -0.3985 0.5430 0.036 Uiso 1 1 calc R . . 
C6 C 0.3563(3) -0.2460(3) 0.5896(3) 0.0241(6) Uani 1 1 d . . . 
C7 C 0.1099(4) -0.2235(4) 0.9835(4) 0.0470(8) Uani 1 1 d . . . 
H7A H 0.0286 -0.2136 1.0612 0.071 Uiso 1 1 calc R . . 
H7B H 0.1385 -0.1319 0.9084 0.071 Uiso 1 1 calc R . . 
H7C H 0.1863 -0.2648 1.0144 0.071 Uiso 1 1 calc R . . 
C8 C 0.4278(3) -0.1383(3) 0.4565(3) 0.0262(6) Uani 1 1 d . . . 
H8A H 0.5139 -0.1636 0.3994 0.031 Uiso 1 1 calc R . . 
C9 C 0.4863(3) 0.0721(3) 0.2674(3) 0.0313(7) Uani 1 1 d . . . 
H9A H 0.4873 0.0384 0.1989 0.038 Uiso 1 1 calc R . . 
H9B H 0.5813 0.0627 0.2668 0.038 Uiso 1 1 calc R . . 
C10 C 0.4445(3) 0.2232(3) 0.2271(3) 0.0275(6) Uani 1 1 d . . . 
H10A H 0.4611 0.2625 0.2838 0.033 Uiso 1 1 calc R . . 
H10B H 0.5013 0.2765 0.1284 0.033 Uiso 1 1 calc R . . 
C11 C 0.2480(3) 0.3792(3) 0.2070(3) 0.0295(6) Uani 1 1 d . . . 
H11A H 0.2999 0.4312 0.1068 0.035 Uiso 1 1 calc R . . 
H11B H 0.2642 0.4253 0.2588 0.035 Uiso 1 1 calc R . . 
C12 C 0.0944(3) 0.3781(3) 0.2378(3) 0.0297(6) Uani 1 1 d . . . 
H12A H 0.0587 0.4744 0.2140 0.036 Uiso 1 1 calc R . . 
H12B H 0.0792 0.3376 0.1813 0.036 Uiso 1 1 calc R . . 
C13 C -0.0994(3) 0.3377(3) 0.4465(3) 0.0246(6) Uani 1 1 d . . . 
H13A H -0.1336 0.4205 0.3932 0.030 Uiso 1 1 calc R . . 
C14 C -0.1788(3) 0.1233(3) 0.6670(3) 0.0218(6) Uani 1 1 d . A . 
C15 C -0.1870(3) 0.2680(3) 0.5921(3) 0.0229(6) Uani 1 1 d . . . 
C16 C -0.2820(3) 0.3495(3) 0.6580(3) 0.0309(6) Uani 1 1 d . . . 
H16A H -0.2908 0.4453 0.6060 0.037 Uiso 1 1 calc R . . 
C17 C -0.3630(3) 0.2922(3) 0.7976(3) 0.0382(7) Uani 1 1 d . . . 
H17A H -0.4266 0.3484 0.8419 0.046 Uiso 1 1 calc R . . 
C18 C -0.3509(4) 0.1522(3) 0.8729(3) 0.0406(8) Uani 1 1 d . A . 
H18A H -0.4058 0.1130 0.9694 0.049 Uiso 1 1 calc R . . 
C19 C -0.2603(3) 0.0690(3) 0.8097(3) 0.0293(6) Uani 1 1 d . . . 
O4' O -0.2762(18) -0.059(3) 0.888(2) 0.027(3) Uani 0.35 1 d PD A 1 
C20' C -0.1729(12) -0.0973(11) 0.9470(12) 0.042(2) Uani 0.35 1 d PD A 1 
H20A H -0.0808 -0.0693 0.8728 0.063 Uiso 0.35 1 calc PR A 1 
H20B H -0.1754 -0.1982 0.9985 0.063 Uiso 0.35 1 calc PR A 1 
H20C H -0.1919 -0.0506 1.0100 0.063 Uiso 0.35 1 calc PR A 1 
O4 O -0.2342(11) -0.0762(14) 0.8782(12) 0.0334(19) Uani 0.65 1 d PD A 2 
C20 C -0.2491(8) -0.1222(6) 1.0165(6) 0.0432(14) Uani 0.65 1 d PD A 2 
H20D H -0.2414 -0.2237 1.0552 0.065 Uiso 0.65 1 calc PR A 2 
H20E H -0.3402 -0.0947 1.0703 0.065 Uiso 0.65 1 calc PR A 2 
H20F H -0.1759 -0.0804 1.0206 0.065 Uiso 0.65 1 calc PR 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 
Gd1 O1 2.2237(17) . ? 
Gd1 O3 2.3474(17) 2_556 ? 
Gd1 O3 2.3708(18) . ? 
Gd1 O5 2.4587(19) . ? 
Gd1 O6 2.5149(18) . ? 
Gd1 N1 2.537(2) . ? 
Gd1 N2 2.554(2) . ? 
Gd1 N3 2.564(2) . ? 
Gd1 N4 2.900(2) . ? 
Gd1 Gd1 3.8112(2) 2_556 ? 
N1 C8 1.280(4) . ? 
N1 C9 1.470(4) . ? 
N2 C11 1.470(3) . ? 
N2 C10 1.473(4) . ? 
N3 C13 1.278(4) . ? 
N3 C12 1.464(4) . ? 
N4 O7 1.209(3) . ? 
N4 O6 1.262(3) . ? 
N4 O5 1.278(3) . ? 
O1 C1 1.310(3) . ? 
O2 C2 1.378(4) . ? 
O2 C7 1.441(4) . ? 
O3 C14 1.345(3) . ? 
O3 Gd1 2.3474(17) 2_556 ? 
C1 C2 1.408(4) . ? 
C1 C6 1.430(4) . ? 
C2 C3 1.385(4) . ? 
C3 C4 1.394(4) . ? 
C4 C5 1.363(4) . ? 
C5 C6 1.407(4) . ? 
C6 C8 1.444(4) . ? 
C9 C10 1.511(4) . ? 
C11 C12 1.513(4) . ? 
C13 C15 1.456(4) . ? 
C14 C19 1.405(4) . ? 
C14 C15 1.418(4) . ? 
C15 C16 1.398(4) . ? 
C16 C17 1.379(5) . ? 
C17 C18 1.385(5) . ? 
C18 C19 1.379(4) . ? 
C19 O4 1.444(12) . ? 
C19 O4' 1.27(3) . ? 
O4' C20' 1.433(16) . ? 
O4 C20 1.403(11) . ? 
  
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 Gd1 O3 98.87(6) . 2_556 ? 
O1 Gd1 O3 90.62(7) . . ? 
O3 Gd1 O3 72.25(7) 2_556 . ? 
O1 Gd1 O5 94.53(7) . . ? 
O3 Gd1 O5 157.32(7) 2_556 . ? 
O3 Gd1 O5 126.03(6) . . ? 
O1 Gd1 O6 77.51(7) . . ? 
O3 Gd1 O6 149.69(7) 2_556 . ? 
O3 Gd1 O6 77.68(6) . . ? 
O5 Gd1 O6 51.57(7) . . ? 
O1 Gd1 N1 72.24(7) . . ? 
O3 Gd1 N1 82.69(6) 2_556 . ? 
O3 Gd1 N1 147.12(6) . . ? 
O5 Gd1 N1 84.11(7) . . ? 
O6 Gd1 N1 123.22(7) . . ? 
O1 Gd1 N2 137.58(7) . . ? 
O3 Gd1 N2 84.34(6) 2_556 . ? 
O3 Gd1 N2 129.68(7) . . ? 
O5 Gd1 N2 73.46(7) . . ? 
O6 Gd1 N2 118.83(6) . . ? 
N1 Gd1 N2 66.22(7) . . ? 
O1 Gd1 N3 155.08(7) . . ? 
O3 Gd1 N3 90.02(6) 2_556 . ? 
O3 Gd1 N3 69.88(7) . . ? 
O5 Gd1 N3 85.34(7) . . ? 
O6 Gd1 N3 83.09(7) . . ? 
N1 Gd1 N3 132.30(7) . . ? 
N2 Gd1 N3 66.16(7) . . ? 
O1 Gd1 N4 84.01(7) . . ? 
O3 Gd1 N4 173.91(6) 2_556 . ? 
O3 Gd1 N4 102.45(6) . . ? 
O5 Gd1 N4 25.96(8) . . ? 
O6 Gd1 N4 25.71(7) . . ? 
N1 Gd1 N4 103.34(7) . . ? 
N2 Gd1 N4 97.18(7) . . ? 
N3 Gd1 N4 85.24(7) . . ? 
O1 Gd1 Gd1 95.84(5) . 2_556 ? 
O3 Gd1 Gd1 36.33(4) 2_556 2_556 ? 
O3 Gd1 Gd1 35.92(4) . 2_556 ? 
O5 Gd1 Gd1 159.10(5) . 2_556 ? 
O6 Gd1 Gd1 113.52(5) . 2_556 ? 
N1 Gd1 Gd1 116.36(5) . 2_556 ? 
N2 Gd1 Gd1 109.66(5) . 2_556 ? 
N3 Gd1 Gd1 77.66(5) . 2_556 ? 
N4 Gd1 Gd1 138.30(5) . 2_556 ? 
C8 N1 C9 114.6(2) . . ? 
C8 N1 Gd1 126.05(19) . . ? 
C9 N1 Gd1 118.04(17) . . ? 
C11 N2 C10 113.1(2) . . ? 
C11 N2 Gd1 112.68(16) . . ? 
C10 N2 Gd1 110.70(16) . . ? 
C13 N3 C12 117.5(2) . . ? 
C13 N3 Gd1 126.09(19) . . ? 
C12 N3 Gd1 116.38(16) . . ? 
O7 N4 O6 122.3(3) . . ? 
O7 N4 O5 120.8(3) . . ? 
O6 N4 O5 116.9(2) . . ? 
O7 N4 Gd1 173.7(2) . . ? 
O6 N4 Gd1 59.85(12) . . ? 
O5 N4 Gd1 57.37(12) . . ? 
C1 O1 Gd1 137.70(17) . . ? 
C2 O2 C7 112.3(2) . . ? 
C14 O3 Gd1 128.04(16) . 2_556 ? 
C14 O3 Gd1 119.12(15) . . ? 
Gd1 O3 Gd1 107.75(7) 2_556 . ? 
N4 O5 Gd1 96.67(16) . . ? 
N4 O6 Gd1 94.44(15) . . ? 
O1 C1 C2 120.9(3) . . ? 
O1 C1 C6 121.9(3) . . ? 
C2 C1 C6 117.2(2) . . ? 
O2 C2 C3 118.1(3) . . ? 
O2 C2 C1 120.8(2) . . ? 
C3 C2 C1 120.9(3) . . ? 
C2 C3 C4 120.9(3) . . ? 
C5 C4 C3 119.5(2) . . ? 
C4 C5 C6 121.2(3) . . ? 
C5 C6 C1 119.9(3) . . ? 
C5 C6 C8 117.3(3) . . ? 
C1 C6 C8 122.9(2) . . ? 
N1 C8 C6 127.8(2) . . ? 
N1 C9 C10 110.7(2) . . ? 
N2 C10 C9 109.4(2) . . ? 
N2 C11 C12 108.4(2) . . ? 
N3 C12 C11 109.2(2) . . ? 
N3 C13 C15 124.6(2) . . ? 
O3 C14 C19 120.7(2) . . ? 
O3 C14 C15 121.7(3) . . ? 
C19 C14 C15 117.6(2) . . ? 
C16 C15 C14 120.1(3) . . ? 
C16 C15 C13 117.4(2) . . ? 
C14 C15 C13 122.5(2) . . ? 
C17 C16 C15 120.7(3) . . ? 
C18 C17 C16 119.5(3) . . ? 
C17 C18 C19 120.8(3) . . ? 
O4 C19 O4' 17.0(11) . . ? 
O4 C19 C18 125.9(5) . . ? 
O4' C19 C18 112.7(8) . . ? 
O4 C19 C14 113.1(5) . . ? 
O4' C19 C14 125.4(8) . . ? 
C18 C19 C14 121.0(3) . . ? 
C20' O4' C19 108.0(18) . . ? 
C19 O4 C20 117.1(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 
O1 Gd1 N1 C8 26.9(2) . . . . ? 
O3 Gd1 N1 C8 -74.9(2) 2_556 . . . ? 
O3 Gd1 N1 C8 -34.8(3) . . . . ? 
O5 Gd1 N1 C8 123.6(2) . . . . ? 
O6 Gd1 N1 C8 88.1(2) . . . . ? 
N2 Gd1 N1 C8 -161.9(2) . . . . ? 
N3 Gd1 N1 C8 -158.2(2) . . . . ? 
N4 Gd1 N1 C8 106.1(2) . . . . ? 
Gd1 Gd1 N1 C8 -60.8(2) 2_556 . . . ? 
O1 Gd1 N1 C9 -166.7(2) . . . . ? 
O3 Gd1 N1 C9 91.5(2) 2_556 . . . ? 
O3 Gd1 N1 C9 131.7(2) . . . . ? 
O5 Gd1 N1 C9 -70.0(2) . . . . ? 
O6 Gd1 N1 C9 -105.4(2) . . . . ? 
N2 Gd1 N1 C9 4.53(19) . . . . ? 
N3 Gd1 N1 C9 8.2(2) . . . . ? 
N4 Gd1 N1 C9 -87.5(2) . . . . ? 
Gd1 Gd1 N1 C9 105.6(2) 2_556 . . . ? 
O1 Gd1 N2 C11 -146.21(16) . . . . ? 
O3 Gd1 N2 C11 116.82(17) 2_556 . . . ? 
O3 Gd1 N2 C11 55.53(18) . . . . ? 
O5 Gd1 N2 C11 -67.91(17) . . . . ? 
O6 Gd1 N2 C11 -42.54(19) . . . . ? 
N1 Gd1 N2 C11 -158.70(18) . . . . ? 
N3 Gd1 N2 C11 24.30(16) . . . . ? 
N4 Gd1 N2 C11 -57.24(17) . . . . ? 
Gd1 Gd1 N2 C11 90.34(16) 2_556 . . . ? 
O1 Gd1 N2 C10 -18.5(2) . . . . ? 
O3 Gd1 N2 C10 -115.47(16) 2_556 . . . ? 
O3 Gd1 N2 C10 -176.76(14) . . . . ? 
O5 Gd1 N2 C10 59.81(16) . . . . ? 
O6 Gd1 N2 C10 85.18(16) . . . . ? 
N1 Gd1 N2 C10 -30.98(15) . . . . ? 
N3 Gd1 N2 C10 152.01(17) . . . . ? 
N4 Gd1 N2 C10 70.47(16) . . . . ? 
Gd1 Gd1 N2 C10 -141.95(15) 2_556 . . . ? 
O1 Gd1 N3 C13 -6.6(3) . . . . ? 
O3 Gd1 N3 C13 104.9(2) 2_556 . . . ? 
O3 Gd1 N3 C13 33.9(2) . . . . ? 
O5 Gd1 N3 C13 -97.3(2) . . . . ? 
O6 Gd1 N3 C13 -45.5(2) . . . . ? 
N1 Gd1 N3 C13 -175.0(2) . . . . ? 
N2 Gd1 N3 C13 -171.3(2) . . . . ? 
N4 Gd1 N3 C13 -71.2(2) . . . . ? 
Gd1 Gd1 N3 C13 70.5(2) 2_556 . . . ? 
O1 Gd1 N3 C12 171.34(18) . . . . ? 
O3 Gd1 N3 C12 -77.16(18) 2_556 . . . ? 
O3 Gd1 N3 C12 -148.21(19) . . . . ? 
O5 Gd1 N3 C12 80.61(18) . . . . ? 
O6 Gd1 N3 C12 132.42(19) . . . . ? 
N1 Gd1 N3 C12 2.9(2) . . . . ? 
N2 Gd1 N3 C12 6.64(17) . . . . ? 
N4 Gd1 N3 C12 106.66(19) . . . . ? 
Gd1 Gd1 N3 C12 -111.60(18) 2_556 . . . ? 
O1 Gd1 N4 O7 38(2) . . . . ? 
O3 Gd1 N4 O7 156.7(19) 2_556 . . . ? 
O3 Gd1 N4 O7 127(2) . . . . ? 
O5 Gd1 N4 O7 -75(2) . . . . ? 
O6 Gd1 N4 O7 112(2) . . . . ? 
N1 Gd1 N4 O7 -32(2) . . . . ? 
N2 Gd1 N4 O7 -99(2) . . . . ? 
N3 Gd1 N4 O7 -164(2) . . . . ? 
Gd1 Gd1 N4 O7 130(2) 2_556 . . . ? 
O1 Gd1 N4 O6 -73.53(16) . . . . ? 
O3 Gd1 N4 O6 45.0(7) 2_556 . . . ? 
O3 Gd1 N4 O6 15.78(17) . . . . ? 
O5 Gd1 N4 O6 173.1(3) . . . . ? 
N1 Gd1 N4 O6 -143.65(16) . . . . ? 
N2 Gd1 N4 O6 149.17(16) . . . . ? 
N3 Gd1 N4 O6 83.95(17) . . . . ? 
Gd1 Gd1 N4 O6 18.5(2) 2_556 . . . ? 
O1 Gd1 N4 O5 113.39(16) . . . . ? 
O3 Gd1 N4 O5 -128.1(6) 2_556 . . . ? 
O3 Gd1 N4 O5 -157.30(15) . . . . ? 
O6 Gd1 N4 O5 -173.1(3) . . . . ? 
N1 Gd1 N4 O5 43.28(17) . . . . ? 
N2 Gd1 N4 O5 -23.91(16) . . . . ? 
N3 Gd1 N4 O5 -89.12(16) . . . . ? 
Gd1 Gd1 N4 O5 -154.55(13) 2_556 . . . ? 
O3 Gd1 O1 C1 41.4(3) 2_556 . . . ? 
O3 Gd1 O1 C1 113.6(3) . . . . ? 
O5 Gd1 O1 C1 -120.2(3) . . . . ? 
O6 Gd1 O1 C1 -169.2(3) . . . . ? 
N1 Gd1 O1 C1 -37.9(3) . . . . ? 
N2 Gd1 O1 C1 -49.9(3) . . . . ? 
N3 Gd1 O1 C1 151.1(3) . . . . ? 
N4 Gd1 O1 C1 -144.0(3) . . . . ? 
Gd1 Gd1 O1 C1 78.0(3) 2_556 . . . ? 
O1 Gd1 O3 C14 104.10(18) . . . . ? 
O3 Gd1 O3 C14 -156.8(2) 2_556 . . . ? 
O5 Gd1 O3 C14 8.0(2) . . . . ? 
O6 Gd1 O3 C14 27.03(18) . . . . ? 
N1 Gd1 O3 C14 161.06(17) . . . . ? 
N2 Gd1 O3 C14 -90.37(19) . . . . ? 
N3 Gd1 O3 C14 -60.04(18) . . . . ? 
N4 Gd1 O3 C14 20.09(19) . . . . ? 
Gd1 Gd1 O3 C14 -156.8(2) 2_556 . . . ? 
O1 Gd1 O3 Gd1 -99.11(7) . . . 2_556 ? 
O3 Gd1 O3 Gd1 0.0 2_556 . . 2_556 ? 
O5 Gd1 O3 Gd1 164.82(7) . . . 2_556 ? 
O6 Gd1 O3 Gd1 -176.18(8) . . . 2_556 ? 
N1 Gd1 O3 Gd1 -42.15(15) . . . 2_556 ? 
N2 Gd1 O3 Gd1 66.42(9) . . . 2_556 ? 
N3 Gd1 O3 Gd1 96.75(8) . . . 2_556 ? 
N4 Gd1 O3 Gd1 176.88(6) . . . 2_556 ? 
O7 N4 O5 Gd1 172.9(2) . . . . ? 
O6 N4 O5 Gd1 -6.7(3) . . . . ? 
O1 Gd1 O5 N4 -66.30(16) . . . . ? 
O3 Gd1 O5 N4 167.48(14) 2_556 . . . ? 
O3 Gd1 O5 N4 27.78(18) . . . . ? 
O6 Gd1 O5 N4 3.83(15) . . . . ? 
N1 Gd1 O5 N4 -137.89(16) . . . . ? 
N2 Gd1 O5 N4 155.20(17) . . . . ? 
N3 Gd1 O5 N4 88.70(16) . . . . ? 
Gd1 Gd1 O5 N4 53.3(2) 2_556 . . . ? 
O7 N4 O6 Gd1 -173.1(3) . . . . ? 
O5 N4 O6 Gd1 6.5(2) . . . . ? 
O1 Gd1 O6 N4 102.34(17) . . . . ? 
O3 Gd1 O6 N4 -171.45(13) 2_556 . . . ? 
O3 Gd1 O6 N4 -164.23(17) . . . . ? 
O5 Gd1 O6 N4 -3.86(15) . . . . ? 
N1 Gd1 O6 N4 43.59(19) . . . . ? 
N2 Gd1 O6 N4 -35.48(18) . . . . ? 
N3 Gd1 O6 N4 -93.38(17) . . . . ? 
Gd1 Gd1 O6 N4 -166.67(14) 2_556 . . . ? 
Gd1 O1 C1 C2 -149.3(2) . . . . ? 
Gd1 O1 C1 C6 30.4(4) . . . . ? 
C7 O2 C2 C3 117.5(3) . . . . ? 
C7 O2 C2 C1 -67.4(3) . . . . ? 
O1 C1 C2 O2 -2.9(4) . . . . ? 
C6 C1 C2 O2 177.3(2) . . . . ? 
O1 C1 C2 C3 172.1(3) . . . . ? 
C6 C1 C2 C3 -7.7(4) . . . . ? 
O2 C2 C3 C4 -179.7(3) . . . . ? 
C1 C2 C3 C4 5.1(4) . . . . ? 
C2 C3 C4 C5 0.5(4) . . . . ? 
C3 C4 C5 C6 -3.3(4) . . . . ? 
C4 C5 C6 C1 0.5(4) . . . . ? 
C4 C5 C6 C8 179.8(3) . . . . ? 
O1 C1 C6 C5 -174.8(2) . . . . ? 
C2 C1 C6 C5 4.9(4) . . . . ? 
O1 C1 C6 C8 5.9(4) . . . . ? 
C2 C1 C6 C8 -174.3(2) . . . . ? 
C9 N1 C8 C6 179.4(3) . . . . ? 
Gd1 N1 C8 C6 -13.8(4) . . . . ? 
C5 C6 C8 N1 170.6(3) . . . . ? 
C1 C6 C8 N1 -10.1(4) . . . . ? 
C8 N1 C9 C10 -170.3(2) . . . . ? 
Gd1 N1 C9 C10 21.7(3) . . . . ? 
C11 N2 C10 C9 -177.7(2) . . . . ? 
Gd1 N2 C10 C9 54.8(2) . . . . ? 
N1 C9 C10 N2 -50.3(3) . . . . ? 
C10 N2 C11 C12 -178.5(2) . . . . ? 
Gd1 N2 C11 C12 -52.0(2) . . . . ? 
C13 N3 C12 C11 142.7(2) . . . . ? 
Gd1 N3 C12 C11 -35.4(3) . . . . ? 
N2 C11 C12 N3 57.1(3) . . . . ? 
C12 N3 C13 C15 179.8(2) . . . . ? 
Gd1 N3 C13 C15 -2.3(4) . . . . ? 
Gd1 O3 C14 C19 90.2(3) 2_556 . . . ? 
Gd1 O3 C14 C19 -118.3(2) . . . . ? 
Gd1 O3 C14 C15 -90.5(3) 2_556 . . . ? 
Gd1 O3 C14 C15 61.0(3) . . . . ? 
O3 C14 C15 C16 175.7(2) . . . . ? 
C19 C14 C15 C16 -5.0(4) . . . . ? 
O3 C14 C15 C13 -4.3(4) . . . . ? 
C19 C14 C15 C13 175.0(3) . . . . ? 
N3 C13 C15 C16 153.8(3) . . . . ? 
N3 C13 C15 C14 -26.2(4) . . . . ? 
C14 C15 C16 C17 3.7(4) . . . . ? 
C13 C15 C16 C17 -176.4(3) . . . . ? 
C15 C16 C17 C18 -0.7(5) . . . . ? 
C16 C17 C18 C19 -0.9(5) . . . . ? 
C17 C18 C19 O4 177.0(7) . . . . ? 
C17 C18 C19 O4' -170.5(10) . . . . ? 
C17 C18 C19 C14 -0.7(5) . . . . ? 
O3 C14 C19 O4 4.9(7) . . . . ? 
C15 C14 C19 O4 -174.4(6) . . . . ? 
O3 C14 C19 O4' -8.6(11) . . . . ? 
C15 C14 C19 O4' 172.1(11) . . . . ? 
O3 C14 C19 C18 -177.1(3) . . . . ? 
C15 C14 C19 C18 3.6(4) . . . . ? 
O4 C19 O4' C20' 45(4) . . . . ? 
C18 C19 O4' C20' -98.5(11) . . . . ? 
C14 C19 O4' C20' 92.1(14) . . . . ? 
O4' C19 O4 C20 -73(4) . . . . ? 
C18 C19 O4 C20 -29.7(13) . . . . ? 
C14 C19 O4 C20 148.1(8) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.973 
_diffrn_reflns_theta_full              24.71 
_diffrn_measured_fraction_theta_full   0.973 
_refine_diff_density_max    1.208 
_refine_diff_density_min   -1.067 
_refine_diff_density_rms    0.099 


data_mm002

 

_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

 ?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          ?

_chemical_formula_sum

 'C40 H46 Ho2 N8 O14'

_chemical_formula_weight          1192.71

 

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'

 'O'  'O'   0.0106   0.0060

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 'Ho'  'Ho'  -0.2175   4.6783

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 

_symmetry_cell_setting            Triclinic

_symmetry_space_group_name_H-M    P-1

 

loop_

 _symmetry_equiv_pos_as_xyz

 'x, y, z'

 '-x, -y, -z'

 

_cell_length_a                    10.5330(7)

_cell_length_b                    10.5394(9)

_cell_length_c                    11.5002(9)

_cell_angle_alpha                 66.484(4)

_cell_angle_beta                  65.036(4)

_cell_angle_gamma                 79.837(4)

_cell_volume                      1061.21(14)

_cell_formula_units_Z             1

_cell_measurement_temperature     200(2)

_cell_measurement_reflns_used     4262

_cell_measurement_theta_min       4.68

_cell_measurement_theta_max       28.28

 

_exptl_crystal_description        block

_exptl_crystal_colour             yellow

_exptl_crystal_size_max           0.35

_exptl_crystal_size_mid           0.30

_exptl_crystal_size_min           0.20

_exptl_crystal_density_meas       n/a

_exptl_crystal_density_diffrn     1.866

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              588

_exptl_absorpt_coefficient_mu     3.779

_exptl_absorpt_correction_type    multi-scan

_exptl_absorpt_correction_T_min   0.3514

_exptl_absorpt_correction_T_max   0.5187

_exptl_absorpt_process_details    'SADABS, Bruker (2003)'

 

_exptl_special_details

;

 Data collection is performed with three batch runs at phi = 0.00 deg

 (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg

 (650 frames).

 Frame width = 0.30 deg in omega.

 Data is merged, corrected for decay (if any), and treated with multi-scan

 absorption corrections (if required). All symmetry-equivalent reflections

 are merged for centrosymmetric data.

 Friedel pairs are not merged for noncentrosymmetric data.

;

 

_diffrn_ambient_temperature       200(2)

_diffrn_radiation_wavelength      0.71073

_diffrn_radiation_type            MoK\a

_diffrn_radiation_source          'fine-focus sealed tube'

_diffrn_radiation_monochromator   graphite

_diffrn_measurement_device_type   'Bruker APEX-II CCD'

_diffrn_measurement_method        'φ and ω scans'

_diffrn_detector_area_resol_mean  ?

_diffrn_standards_number          0

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         <1

_diffrn_reflns_number             5037

_diffrn_reflns_av_R_equivalents   0.0096

_diffrn_reflns_av_sigmaI/netI     0.0207

_diffrn_reflns_limit_h_min        -13

_diffrn_reflns_limit_h_max        13

_diffrn_reflns_limit_k_min        -14

_diffrn_reflns_limit_k_max        7

_diffrn_reflns_limit_l_min        -15

_diffrn_reflns_limit_l_max        14

_diffrn_reflns_theta_min          4.68

_diffrn_reflns_theta_max          28.28

_reflns_number_total              4449

_reflns_number_gt                 4323

_reflns_threshold_expression      >2sigma(I)

 

_computing_data_collection        'APEX II, Bruker (2009)'

_computing_cell_refinement        'APEX II, Bruker (2009)'

_computing_data_reduction         'XPREP, Bruker (2009)'

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics     'SHELXTL, Bruker (2004)'

_computing_publication_material   'SHELXTL, Bruker (2004)'

 

_refine_special_details

;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;

 

_refine_ls_structure_factor_coef  Fsqd

_refine_ls_matrix_type            full

_refine_ls_weighting_scheme       calc

_refine_ls_weighting_details

 'calc w=1/[σ²(Fo²)+(0.0339P)²+0.4814P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary      direct

_atom_sites_solution_secondary    difmap

_atom_sites_solution_hydrogens    geom

_refine_ls_hydrogen_treatment     constr

_refine_ls_extinction_method      none

_refine_ls_extinction_coef        ?

_refine_ls_number_reflns          4449

_refine_ls_number_parameters      289

_refine_ls_number_restraints      0

_refine_ls_R_factor_all           0.0198

_refine_ls_R_factor_gt            0.0191

_refine_ls_wR_factor_ref          0.0508

_refine_ls_wR_factor_gt           0.0503

_refine_ls_goodness_of_fit_ref    1.037

_refine_ls_restrained_S_all       1.037

_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_symmetry_multiplicity

 _atom_site_calc_flag

 _atom_site_refinement_flags

 _atom_site_disorder_assembly

 _atom_site_disorder_group

Ho1 Ho 0.414586(9) 0.854412(10) 0.505068(10) 0.01560(5) Uani 1 1 d . . .

N1 N 0.2023(2) 0.9866(2) 0.6104(2) 0.0217(4) Uani 1 1 d . . .

N2 N 0.2616(2) 0.7142(2) 0.7495(2) 0.0227(4) Uani 1 1 d . . .

H2A H 0.2954 0.7276 0.8065 0.027 Uiso 1 1 calc R . .

N3 N 0.5111(2) 0.6173(2) 0.5959(2) 0.0219(4) Uani 1 1 d . . .

N4 N 0.2530(2) 0.8129(3) 0.3744(2) 0.0253(5) Uani 1 1 d . . .

O1 O 0.46255(17) 1.09025(18) 0.39631(18) 0.0179(3) Uani 1 1 d . . .

O2 O 0.57804(19) 1.2204(2) 0.1218(2) 0.0289(4) Uani 1 1 d . . .

O3 O 0.59012(19) 0.8213(2) 0.33051(19) 0.0255(4) Uani 1 1 d . . .

O4 O 0.8043(2) 0.9242(2) 0.0697(2) 0.0312(4) Uani 1 1 d . . .

O5 O 0.3153(2) 0.9255(2) 0.3256(2) 0.0308(4) Uani 1 1 d . . .

O6 O 0.2542(2) 0.7276(2) 0.4912(2) 0.0311(4) Uani 1 1 d . . .

O7 O 0.1944(3) 0.7837(3) 0.3173(3) 0.0460(6) Uani 1 1 d . . .

C1 C 0.3808(2) 1.1736(2) 0.3313(3) 0.0166(4) Uani 1 1 d . . .

C2 C 0.4387(3) 1.2452(3) 0.1877(3) 0.0218(5) Uani 1 1 d . . .

C3 C 0.3567(3) 1.3358(3) 0.1208(3) 0.0285(6) Uani 1 1 d . . .

H3A H 0.3972 1.3839 0.0240 0.034 Uiso 1 1 calc R . .

C4 C 0.2157(3) 1.3569(3) 0.1940(3) 0.0301(6) Uani 1 1 d . . .

H4A H 0.1610 1.4208 0.1478 0.036 Uiso 1 1 calc R . .

C5 C 0.1560(3) 1.2844(3) 0.3340(3) 0.0269(6) Uani 1 1 d . . .

H5A H 0.0600 1.2989 0.3844 0.032 Uiso 1 1 calc R . .

C6 C 0.2361(2) 1.1896(3) 0.4024(3) 0.0201(5) Uani 1 1 d . . .

C7 C 0.6314(3) 1.2542(4) -0.0226(3) 0.0369(7) Uani 1 1 d . . .

H7A H 0.7315 1.2314 -0.0561 0.055 Uiso 1 1 calc R . .

H7B H 0.6178 1.3534 -0.0679 0.055 Uiso 1 1 calc R . .

H7C H 0.5816 1.2012 -0.0435 0.055 Uiso 1 1 calc R . .

C8 C 0.1624(3) 1.1066(3) 0.5479(3) 0.0231(5) Uani 1 1 d . . .

H8A H 0.0794 1.1444 0.5994 0.028 Uiso 1 1 calc R . .

C9 C 0.1152(3) 0.9175(3) 0.7567(3) 0.0284(6) Uani 1 1 d . . .

H9A H 0.0183 0.9547 0.7774 0.034 Uiso 1 1 calc R . .

H9B H 0.1530 0.9345 0.8147 0.034 Uiso 1 1 calc R . .

C10 C 0.1154(3) 0.7634(3) 0.7877(3) 0.0252(5) Uani 1 1 d . . .

H10A H 0.0609 0.7140 0.8868 0.030 Uiso 1 1 calc R . .

H10B H 0.0721 0.7457 0.7341 0.030 Uiso 1 1 calc R . .

C11 C 0.2743(3) 0.5648(3) 0.7746(3) 0.0260(5) Uani 1 1 d . . .

H11A H 0.2357 0.5443 0.7191 0.031 Uiso 1 1 calc R . .

H11B H 0.2210 0.5115 0.8731 0.031 Uiso 1 1 calc R . .

C12 C 0.4272(3) 0.5244(3) 0.7350(3) 0.0290(6) Uani 1 1 d . . .

H12A H 0.4606 0.5289 0.8019 0.035 Uiso 1 1 calc R . .

H12B H 0.4391 0.4280 0.7380 0.035 Uiso 1 1 calc R . .

C13 C 0.6359(3) 0.5748(3) 0.5427(3) 0.0242(5) Uani 1 1 d . . .

H13A H 0.6614 0.4879 0.5973 0.029 Uiso 1 1 calc R . .

C14 C 0.7132(3) 0.7618(3) 0.3071(3) 0.0218(5) Uani 1 1 d . . .

C15 C 0.7428(3) 0.6435(3) 0.4091(3) 0.0227(5) Uani 1 1 d . . .

C16 C 0.8802(3) 0.5896(3) 0.3824(3) 0.0280(6) Uani 1 1 d . . .

H16A H 0.8983 0.5108 0.4514 0.034 Uiso 1 1 calc R . .

C17 C 0.9882(3) 0.6484(3) 0.2591(3) 0.0318(6) Uani 1 1 d . . .

H17A H 1.0812 0.6139 0.2442 0.038 Uiso 1 1 calc R . .

C18 C 0.9597(3) 0.7603(3) 0.1552(3) 0.0309(6) Uani 1 1 d . . .

H18A H 1.0339 0.8007 0.0689 0.037 Uiso 1 1 calc R . .

C19 C 0.8248(3) 0.8131(3) 0.1764(3) 0.0248(5) Uani 1 1 d . . .

C20 C 0.7054(4) 0.8995(4) 0.0259(4) 0.0460(8) Uani 1 1 d . . .

H20A H 0.6968 0.9822 -0.0498 0.069 Uiso 1 1 calc R . .

H20B H 0.6141 0.8779 0.1031 0.069 Uiso 1 1 calc R . .

H20C H 0.7378 0.8212 -0.0055 0.069 Uiso 1 1 calc R . .

 


 

_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

Ho1 O3 2.1837(18) . ?

Ho1 O1 2.3096(16) 2_676 ?

Ho1 O1 2.3295(18) . ?

Ho1 O6 2.4212(19) . ?

Ho1 O5 2.4953(19) . ?

Ho1 N3 2.507(2) . ?

Ho1 N1 2.523(2) . ?

Ho1 N2 2.526(2) . ?

Ho1 N4 2.879(2) . ?

Ho1 Ho1 3.7623(3) 2_676 ?

N1 C8 1.279(3) . ?

N1 C9 1.469(3) . ?

N2 C11 1.475(3) . ?

N2 C10 1.471(3) . ?

N3 C13 1.279(3) . ?

N3 C12 1.469(4) . ?

N4 O5 1.259(3) . ?

N4 O7 1.216(3) . ?

N4 O6 1.287(3) . ?

O1 C1 1.351(3) . ?

O1 Ho1 2.3096(16) 2_676 ?

O2 C2 1.372(3) . ?

O2 C7 1.418(3) . ?

O3 C14 1.303(3) . ?

O4 C19 1.383(4) . ?

O4 C20 1.431(4) . ?

C1 C6 1.409(3) . ?

C1 C2 1.409(4) . ?

C2 C3 1.391(3) . ?

C3 C4 1.393(4) . ?

C4 C5 1.381(4) . ?

C5 C6 1.402(3) . ?

C6 C8 1.464(4) . ?

C9 C10 1.518(4) . ?

C11 C12 1.509(4) . ?

C13 C15 1.447(4) . ?

C14 C19 1.421(4) . ?

C14 C15 1.425(4) . ?

C15 C16 1.409(4) . ?

C16 C17 1.369(4) . ?

C17 C18 1.400(4) . ?

C18 C19 1.387(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

O3 Ho1 O1 99.28(7) . 2_676 ?

O3 Ho1 O1 88.46(7) . . ?

O1 Ho1 O1 71.62(7) 2_676 . ?

O3 Ho1 O6 92.92(7) . . ?

O1 Ho1 O6 157.45(7) 2_676 . ?

O1 Ho1 O6 127.97(6) . . ?

O3 Ho1 O5 77.07(7) . . ?

O1 Ho1 O5 149.46(6) 2_676 . ?

O1 Ho1 O5 77.95(6) . . ?

O6 Ho1 O5 52.06(7) . . ?

O3 Ho1 N3 73.16(7) . . ?

O1 Ho1 N3 82.59(6) 2_676 . ?

O1 Ho1 N3 145.48(6) . . ?

O6 Ho1 N3 82.91(7) . . ?

O5 Ho1 N3 123.71(7) . . ?

O3 Ho1 N1 152.87(7) . . ?

O1 Ho1 N1 91.14(6) 2_676 . ?

O1 Ho1 N1 71.08(7) . . ?

O6 Ho1 N1 86.37(7) . . ?

O5 Ho1 N1 81.26(7) . . ?

N3 Ho1 N1 133.38(7) . . ?

O3 Ho1 N2 138.60(7) . . ?

O1 Ho1 N2 85.21(6) 2_676 . ?

O1 Ho1 N2 131.06(6) . . ?

O6 Ho1 N2 73.20(7) . . ?

O5 Ho1 N2 117.83(7) . . ?

N3 Ho1 N2 66.62(7) . . ?

N1 Ho1 N2 66.83(7) . . ?

O3 Ho1 N4 82.57(7) . . ?

O1 Ho1 N4 174.49(6) 2_676 . ?

O1 Ho1 N4 103.34(6) . . ?

O6 Ho1 N4 26.34(7) . . ?

O5 Ho1 N4 25.85(7) . . ?

N3 Ho1 N4 102.92(7) . . ?

N1 Ho1 N4 85.01(7) . . ?

N2 Ho1 N4 96.85(7) . . ?

O3 Ho1 Ho1 94.73(5) . 2_676 ?

O1 Ho1 Ho1 35.99(4) 2_676 2_676 ?

O1 Ho1 Ho1 35.63(4) . 2_676 ?

O6 Ho1 Ho1 161.42(5) . 2_676 ?

O5 Ho1 Ho1 113.54(5) . 2_676 ?

N3 Ho1 Ho1 115.53(5) . 2_676 ?

N1 Ho1 Ho1 79.13(5) . 2_676 ?

N2 Ho1 Ho1 110.82(5) . 2_676 ?

N4 Ho1 Ho1 138.93(5) . 2_676 ?

C8 N1 C9 117.1(2) . . ?

C8 N1 Ho1 126.19(17) . . ?

C9 N1 Ho1 116.68(16) . . ?

C11 N2 C10 112.6(2) . . ?

C11 N2 Ho1 111.45(15) . . ?

C10 N2 Ho1 112.16(16) . . ?

C13 N3 C12 114.9(2) . . ?

C13 N3 Ho1 126.26(19) . . ?

C12 N3 Ho1 117.95(16) . . ?

O5 N4 O7 123.4(2) . . ?

O5 N4 O6 115.9(2) . . ?

O7 N4 O6 120.7(2) . . ?

O5 N4 Ho1 59.79(12) . . ?

O7 N4 Ho1 173.1(2) . . ?

O6 N4 Ho1 56.56(11) . . ?

C1 O1 Ho1 128.32(14) . 2_676 ?

C1 O1 Ho1 118.48(14) . . ?

Ho1 O1 Ho1 108.38(7) 2_676 . ?

C2 O2 C7 118.0(2) . . ?

C14 O3 Ho1 137.63(17) . . ?

C19 O4 C20 114.1(2) . . ?

N4 O5 Ho1 94.36(15) . . ?

N4 O6 Ho1 97.10(14) . . ?

O1 C1 C6 121.9(2) . . ?

O1 C1 C2 120.1(2) . . ?

C6 C1 C2 117.9(2) . . ?

O2 C2 C3 123.6(2) . . ?

O2 C2 C1 115.9(2) . . ?

C3 C2 C1 120.5(2) . . ?

C4 C3 C2 120.8(3) . . ?

C5 C4 C3 119.6(2) . . ?

C4 C5 C6 120.4(2) . . ?

C1 C6 C5 120.6(2) . . ?

C1 C6 C8 122.2(2) . . ?

C5 C6 C8 117.2(2) . . ?

N1 C8 C6 124.4(2) . . ?

N1 C9 C10 108.6(2) . . ?

N2 C10 C9 108.0(2) . . ?

N2 C11 C12 108.4(2) . . ?

N3 C12 C11 110.7(2) . . ?

N3 C13 C15 127.6(2) . . ?

O3 C14 C19 120.7(2) . . ?

O3 C14 C15 122.5(2) . . ?

C19 C14 C15 116.8(2) . . ?

C16 C15 C14 120.3(3) . . ?

C16 C15 C13 117.4(2) . . ?

C14 C15 C13 122.3(2) . . ?

C17 C16 C15 121.4(3) . . ?

C16 C17 C18 119.0(3) . . ?

C19 C18 C17 121.0(3) . . ?

O4 C19 C18 118.0(3) . . ?

O4 C19 C14 120.8(2) . . ?

C18 C19 C14 121.0(3) . . ?

 

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

O3 Ho1 N1 C8 -10.3(3) . . . . ?

O1 Ho1 N1 C8 102.8(2) 2_676 . . . ?

O1 Ho1 N1 C8 32.7(2) . . . . ?

O6 Ho1 N1 C8 -99.6(2) . . . . ?

O5 Ho1 N1 C8 -47.5(2) . . . . ?

N3 Ho1 N1 C8 -176.31(18) . . . . ?

N2 Ho1 N1 C8 -172.9(2) . . . . ?

N4 Ho1 N1 C8 -73.2(2) . . . . ?

Ho1 Ho1 N1 C8 68.7(2) 2_676 . . . ?

O3 Ho1 N1 C9 168.44(18) . . . . ?

O1 Ho1 N1 C9 -78.44(18) 2_676 . . . ?

O1 Ho1 N1 C9 -148.54(19) . . . . ?

O6 Ho1 N1 C9 79.13(18) . . . . ?

O5 Ho1 N1 C9 131.28(18) . . . . ?

N3 Ho1 N1 C9 2.4(2) . . . . ?

N2 Ho1 N1 C9 5.86(17) . . . . ?

N4 Ho1 N1 C9 105.51(18) . . . . ?

Ho1 Ho1 N1 C9 -112.55(18) 2_676 . . . ?

O3 Ho1 N2 C11 -15.5(2) . . . . ?

O1 Ho1 N2 C11 -114.12(16) 2_676 . . . ?

O1 Ho1 N2 C11 -174.60(14) . . . . ?

O6 Ho1 N2 C11 59.30(16) . . . . ?

O5 Ho1 N2 C11 86.97(17) . . . . ?

N3 Ho1 N2 C11 -30.13(16) . . . . ?

N1 Ho1 N2 C11 152.58(18) . . . . ?

N4 Ho1 N2 C11 71.01(17) . . . . ?

Ho1 Ho1 N2 C11 -139.88(15) 2_676 . . . ?

O3 Ho1 N2 C10 -142.77(15) . . . . ?

O1 Ho1 N2 C10 118.62(16) 2_676 . . . ?

O1 Ho1 N2 C10 58.14(18) . . . . ?

O6 Ho1 N2 C10 -67.96(16) . . . . ?

O5 Ho1 N2 C10 -40.29(18) . . . . ?

N3 Ho1 N2 C10 -157.39(17) . . . . ?

N1 Ho1 N2 C10 25.32(15) . . . . ?

N4 Ho1 N2 C10 -56.24(16) . . . . ?

Ho1 Ho1 N2 C10 92.86(15) 2_676 . . . ?

O3 Ho1 N3 C13 24.4(2) . . . . ?

O1 Ho1 N3 C13 -77.7(2) 2_676 . . . ?

O1 Ho1 N3 C13 -36.3(3) . . . . ?

O6 Ho1 N3 C13 119.6(2) . . . . ?

O5 Ho1 N3 C13 85.5(2) . . . . ?

N1 Ho1 N3 C13 -162.23(19) . . . . ?

N2 Ho1 N3 C13 -165.7(2) . . . . ?

N4 Ho1 N3 C13 102.4(2) . . . . ?

Ho1 Ho1 N3 C13 -62.8(2) 2_676 . . . ?

O3 Ho1 N3 C12 -167.1(2) . . . . ?

O1 Ho1 N3 C12 90.79(19) 2_676 . . . ?

O1 Ho1 N3 C12 132.17(18) . . . . ?

O6 Ho1 N3 C12 -71.90(19) . . . . ?

O5 Ho1 N3 C12 -106.02(19) . . . . ?

N1 Ho1 N3 C12 6.3(2) . . . . ?

N2 Ho1 N3 C12 2.82(17) . . . . ?

N4 Ho1 N3 C12 -89.14(19) . . . . ?

Ho1 Ho1 N3 C12 105.68(18) 2_676 . . . ?

O3 Ho1 N4 O5 -75.61(16) . . . . ?

O1 Ho1 N4 O5 34.4(7) 2_676 . . . ?

O1 Ho1 N4 O5 11.02(16) . . . . ?

O6 Ho1 N4 O5 172.1(2) . . . . ?

N3 Ho1 N4 O5 -146.36(15) . . . . ?

N1 Ho1 N4 O5 80.22(16) . . . . ?

N2 Ho1 N4 O5 146.13(15) . . . . ?

Ho1 Ho1 N4 O5 13.06(19) 2_676 . . . ?

O3 Ho1 N4 O7 43.6(17) . . . . ?

O1 Ho1 N4 O7 153.7(15) 2_676 . . . ?

O1 Ho1 N4 O7 130.3(17) . . . . ?

O6 Ho1 N4 O7 -68.6(17) . . . . ?

O5 Ho1 N4 O7 119.3(18) . . . . ?

N3 Ho1 N4 O7 -27.1(17) . . . . ?

N1 Ho1 N4 O7 -160.5(17) . . . . ?

N2 Ho1 N4 O7 -94.6(17) . . . . ?

Ho1 Ho1 N4 O7 132.3(17) 2_676 . . . ?

O3 Ho1 N4 O6 112.29(16) . . . . ?

O1 Ho1 N4 O6 -137.7(6) 2_676 . . . ?

O1 Ho1 N4 O6 -161.08(15) . . . . ?

O5 Ho1 N4 O6 -172.1(2) . . . . ?

N3 Ho1 N4 O6 41.53(16) . . . . ?

N1 Ho1 N4 O6 -91.89(16) . . . . ?

N2 Ho1 N4 O6 -25.98(16) . . . . ?

Ho1 Ho1 N4 O6 -159.04(13) 2_676 . . . ?

O3 Ho1 O1 C1 102.24(16) . . . . ?

O1 Ho1 O1 C1 -157.45(19) 2_676 . . . ?

O6 Ho1 O1 C1 9.74(19) . . . . ?

O5 Ho1 O1 C1 25.14(16) . . . . ?

N3 Ho1 O1 C1 158.85(15) . . . . ?

N1 Ho1 O1 C1 -59.63(16) . . . . ?

N2 Ho1 O1 C1 -91.41(17) . . . . ?

N4 Ho1 O1 C1 20.25(17) . . . . ?

Ho1 Ho1 O1 C1 -157.45(19) 2_676 . . . ?

O3 Ho1 O1 Ho1 -100.31(8) . . . 2_676 ?

O1 Ho1 O1 Ho1 0.0 2_676 . . 2_676 ?

O6 Ho1 O1 Ho1 167.19(7) . . . 2_676 ?

O5 Ho1 O1 Ho1 -177.41(8) . . . 2_676 ?

N3 Ho1 O1 Ho1 -43.70(14) . . . 2_676 ?

N1 Ho1 O1 Ho1 97.82(8) . . . 2_676 ?

N2 Ho1 O1 Ho1 66.04(10) . . . 2_676 ?

N4 Ho1 O1 Ho1 177.70(6) . . . 2_676 ?

O1 Ho1 O3 C14 42.2(3) 2_676 . . . ?

O1 Ho1 O3 C14 113.3(3) . . . . ?

O6 Ho1 O3 C14 -118.7(3) . . . . ?

O5 Ho1 O3 C14 -168.7(3) . . . . ?

N3 Ho1 O3 C14 -37.0(2) . . . . ?

N1 Ho1 O3 C14 153.5(2) . . . . ?

N2 Ho1 O3 C14 -51.1(3) . . . . ?

N4 Ho1 O3 C14 -143.0(3) . . . . ?

Ho1 Ho1 O3 C14 78.2(3) 2_676 . . . ?

O7 N4 O5 Ho1 -172.8(2) . . . . ?

O6 N4 O5 Ho1 7.3(2) . . . . ?

O3 Ho1 O5 N4 99.77(16) . . . . ?

O1 Ho1 O5 N4 -173.88(13) 2_676 . . . ?

O1 Ho1 O5 N4 -169.03(16) . . . . ?

O6 Ho1 O5 N4 -4.43(14) . . . . ?

N3 Ho1 O5 N4 40.47(18) . . . . ?

N1 Ho1 O5 N4 -96.65(16) . . . . ?

N2 Ho1 O5 N4 -38.74(17) . . . . ?

Ho1 Ho1 O5 N4 -170.68(13) 2_676 . . . ?

O5 N4 O6 Ho1 -7.6(2) . . . . ?

O7 N4 O6 Ho1 172.5(2) . . . . ?

O3 Ho1 O6 N4 -66.74(15) . . . . ?

O1 Ho1 O6 N4 170.31(14) 2_676 . . . ?

O1 Ho1 O6 N4 23.59(18) . . . . ?

O5 Ho1 O6 N4 4.36(14) . . . . ?

N3 Ho1 O6 N4 -139.37(16) . . . . ?

N1 Ho1 O6 N4 86.09(15) . . . . ?

N2 Ho1 O6 N4 152.98(17) . . . . ?

Ho1 Ho1 O6 N4 47.5(3) 2_676 . . . ?

Ho1 O1 C1 C6 -90.4(3) 2_676 . . . ?

Ho1 O1 C1 C6 62.0(3) . . . . ?

Ho1 O1 C1 C2 91.3(2) 2_676 . . . ?

Ho1 O1 C1 C2 -116.4(2) . . . . ?

C7 O2 C2 C3 -19.5(4) . . . . ?

C7 O2 C2 C1 161.3(3) . . . . ?

O1 C1 C2 O2 2.0(3) . . . . ?

C6 C1 C2 O2 -176.4(2) . . . . ?

O1 C1 C2 C3 -177.2(2) . . . . ?

C6 C1 C2 C3 4.3(4) . . . . ?

O2 C2 C3 C4 -179.7(3) . . . . ?

C1 C2 C3 C4 -0.5(4) . . . . ?

C2 C3 C4 C5 -1.6(4) . . . . ?

C3 C4 C5 C6 -0.3(4) . . . . ?

O1 C1 C6 C5 175.4(2) . . . . ?

C2 C1 C6 C5 -6.2(3) . . . . ?

O1 C1 C6 C8 -6.4(4) . . . . ?

C2 C1 C6 C8 172.0(2) . . . . ?

C4 C5 C6 C1 4.3(4) . . . . ?

C4 C5 C6 C8 -174.0(2) . . . . ?

C9 N1 C8 C6 -179.7(2) . . . . ?

Ho1 N1 C8 C6 -1.0(3) . . . . ?

C1 C6 C8 N1 -25.4(4) . . . . ?

C5 C6 C8 N1 152.8(2) . . . . ?

C8 N1 C9 C10 144.1(2) . . . . ?

Ho1 N1 C9 C10 -34.7(3) . . . . ?

C11 N2 C10 C9 -179.6(2) . . . . ?

Ho1 N2 C10 C9 -53.0(2) . . . . ?

N1 C9 C10 N2 57.1(3) . . . . ?

C10 N2 C11 C12 -178.9(2) . . . . ?

Ho1 N2 C11 C12 54.1(2) . . . . ?

C13 N3 C12 C11 -166.3(2) . . . . ?

Ho1 N3 C12 C11 24.0(3) . . . . ?

N2 C11 C12 N3 -50.8(3) . . . . ?

C12 N3 C13 C15 -179.3(2) . . . . ?

Ho1 N3 C13 C15 -10.6(4) . . . . ?

Ho1 O3 C14 C19 -149.2(2) . . . . ?

Ho1 O3 C14 C15 31.0(4) . . . . ?

O3 C14 C15 C16 -174.9(2) . . . . ?

C19 C14 C15 C16 5.3(4) . . . . ?

O3 C14 C15 C13 4.6(4) . . . . ?

C19 C14 C15 C13 -175.2(2) . . . . ?

N3 C13 C15 C16 168.6(3) . . . . ?

N3 C13 C15 C14 -10.9(4) . . . . ?

C14 C15 C16 C17 -0.1(4) . . . . ?

C13 C15 C16 C17 -179.6(2) . . . . ?

C15 C16 C17 C18 -3.2(4) . . . . ?

C16 C17 C18 C19 1.0(4) . . . . ?

C20 O4 C19 C18 122.2(3) . . . . ?

C20 O4 C19 C14 -62.8(3) . . . . ?

C17 C18 C19 O4 179.6(2) . . . . ?

C17 C18 C19 C14 4.6(4) . . . . ?

O3 C14 C19 O4 -2.2(4) . . . . ?

C15 C14 C19 O4 177.6(2) . . . . ?

O3 C14 C19 C18 172.7(2) . . . . ?

C15 C14 C19 C18 -7.5(4) . . . . ?

 

_diffrn_measured_fraction_theta_max    0.847

_diffrn_reflns_theta_full              28.28

_diffrn_measured_fraction_theta_full   0.847

_refine_diff_density_max    0.778

_refine_diff_density_min   -0.993

_refine_diff_density_rms    0.091



data_mm001

 

_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

 ?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          ?

_chemical_formula_sum

 'C40 H46 N8 O14 Tb2'

_chemical_formula_weight          1180.69

 

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'

 'O'  'O'   0.0106   0.0060

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 'Tb'  'Tb'  -0.1723   4.1537

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 

_symmetry_cell_setting            Triclinic

_symmetry_space_group_name_H-M    P-1

 

loop_

 _symmetry_equiv_pos_as_xyz

 'x, y, z'

 '-x, -y, -z'

 

_cell_length_a                    10.5536(3)

_cell_length_b                    10.5537(3)

_cell_length_c                    11.4994(3)

_cell_angle_alpha                 66.1710(10)

_cell_angle_beta                  65.0160(10)

_cell_angle_gamma                 80.0090(10)

_cell_volume                      1061.98(5)

_cell_formula_units_Z             1

_cell_measurement_temperature     200(2)

_cell_measurement_reflns_used     7473

_cell_measurement_theta_min       2.36

_cell_measurement_theta_max       28.37

 

_exptl_crystal_description        block

_exptl_crystal_colour             yellow

_exptl_crystal_size_max           0.30

_exptl_crystal_size_mid           0.27

_exptl_crystal_size_min           0.25

_exptl_crystal_density_meas       n/a

_exptl_crystal_density_diffrn     1.846

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              584

_exptl_absorpt_coefficient_mu     3.381

_exptl_absorpt_correction_type    multi-scan

_exptl_absorpt_correction_T_min   0.4304

_exptl_absorpt_correction_T_max   0.4853

_exptl_absorpt_process_details    'SADABS, Bruker (2003)'

 

_exptl_special_details

;

 Data collection is performed with four batch runs at phi = 0.00 deg

 (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg

 (600 frames), and at phi = 270.00 deg (600 frames).

 A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor

 crystal and diffractometer stability. Frame width = 0.30 deg in omega.

 Data is merged, corrected for decay (if any), and treated with multi-scan

 absorption corrections (if required). All symmetry-equivalent reflections

 are merged for centrosymmetric data.

 Friedel pairs are not merged for noncentrosymmetric data.

;

 

_diffrn_ambient_temperature       200(2)

_diffrn_radiation_wavelength      0.71073

_diffrn_radiation_type            MoK\a

_diffrn_radiation_source          'fine-focus sealed tube'

_diffrn_radiation_monochromator   graphite

_diffrn_measurement_device_type   'Bruker APEX-II CCD'

_diffrn_measurement_method        'φ and ω scans'

_diffrn_detector_area_resol_mean  ?

_diffrn_standards_number          0

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         <1

_diffrn_reflns_number             8893

_diffrn_reflns_av_R_equivalents   0.0173

_diffrn_reflns_av_sigmaI/netI     0.0278

_diffrn_reflns_limit_h_min        -13

_diffrn_reflns_limit_h_max        13

_diffrn_reflns_limit_k_min        -13

_diffrn_reflns_limit_k_max        13

_diffrn_reflns_limit_l_min        -15

_diffrn_reflns_limit_l_max        14

_diffrn_reflns_theta_min          2.13

_diffrn_reflns_theta_max          27.88

_reflns_number_total              4922

_reflns_number_gt                 4752

_reflns_threshold_expression      >2sigma(I)

 

_computing_data_collection        'APEX II, Bruker (2009)'

_computing_cell_refinement        'APEX II, Bruker (2009)'

_computing_data_reduction         'XPREP, Bruker (2009)'

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics     'SHELXTL, Bruker (2004)'

_computing_publication_material   'SHELXTL, Bruker (2004)'

 

_refine_special_details

;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;

 

_refine_ls_structure_factor_coef  Fsqd

_refine_ls_matrix_type            full

_refine_ls_weighting_scheme       calc

_refine_ls_weighting_details

 'calc w=1/[σ²(Fo²)+(0.0322P)²+0.3331P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary      direct

_atom_sites_solution_secondary    difmap

_atom_sites_solution_hydrogens    geom

_refine_ls_hydrogen_treatment     constr

_refine_ls_extinction_method      none

_refine_ls_extinction_coef        ?

_refine_ls_number_reflns          4922

_refine_ls_number_parameters      289

_refine_ls_number_restraints      0

_refine_ls_R_factor_all           0.0215

_refine_ls_R_factor_gt            0.0206

_refine_ls_wR_factor_ref          0.0542

_refine_ls_wR_factor_gt           0.0538

_refine_ls_goodness_of_fit_ref    1.063

_refine_ls_restrained_S_all       1.063

_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_symmetry_multiplicity

 _atom_site_calc_flag

 _atom_site_refinement_flags

 _atom_site_disorder_assembly

 _atom_site_disorder_group

Tb1 Tb 0.415538(10) 0.353711(10) 1.002997(10) 0.01628(5) Uani 1 1 d . . .

N1 N 0.5113(2) 0.1147(2) 1.0952(2) 0.0218(4) Uani 1 1 d . . .

N2 N 0.2617(2) 0.2110(2) 1.2501(2) 0.0223(4) Uani 1 1 d . . .

H2A H 0.2966 0.2231 1.3069 0.027 Uiso 1 1 calc R . .

N3 N 0.2030(2) 0.4855(2) 1.1119(2) 0.0227(4) Uani 1 1 d . . .

N4 N 0.2523(2) 0.3143(2) 0.8718(2) 0.0262(4) Uani 1 1 d . . .

O1 O 0.59246(19) 0.31954(19) 0.82826(19) 0.0266(4) Uani 1 1 d . . .

O2 O 0.8084(2) 0.4231(2) 0.5684(2) 0.0314(4) Uani 1 1 d . . .

O3 O 0.46195(17) 0.59274(17) 0.89521(17) 0.0187(3) Uani 1 1 d . . .

O4 O 0.5761(2) 0.7269(2) 0.6212(2) 0.0347(4) Uani 1 1 d . . .

O5 O 0.2516(2) 0.2292(2) 0.9888(2) 0.0321(4) Uani 1 1 d . . .

O6 O 0.3175(2) 0.42578(19) 0.8212(2) 0.0323(4) Uani 1 1 d . . .

O7 O 0.1937(3) 0.2871(3) 0.8140(3) 0.0483(6) Uani 1 1 d . . .

C1 C 0.7149(3) 0.2601(3) 0.8067(3) 0.0225(5) Uani 1 1 d . . .

C2 C 0.8279(3) 0.3122(3) 0.6759(3) 0.0251(5) Uani 1 1 d . . .

C3 C 0.9615(3) 0.2603(3) 0.6567(3) 0.0309(6) Uani 1 1 d . . .

H3A H 1.0364 0.3016 0.5707 0.037 Uiso 1 1 calc R . .

C4 C 0.9888(3) 0.1486(3) 0.7609(3) 0.0321(6) Uani 1 1 d . . .

H4A H 1.0815 0.1146 0.7466 0.039 Uiso 1 1 calc R . .

C5 C 0.8803(3) 0.0885(3) 0.8843(3) 0.0290(5) Uani 1 1 d . . .

H5A H 0.8975 0.0090 0.9538 0.035 Uiso 1 1 calc R . .

C6 C 0.7439(3) 0.1427(2) 0.9094(3) 0.0231(5) Uani 1 1 d . . .

C7 C 0.7138(4) 0.3959(4) 0.5219(4) 0.0489(8) Uani 1 1 d . . .

H7A H 0.7053 0.4785 0.4455 0.073 Uiso 1 1 calc R . .

H7B H 0.6218 0.3722 0.5981 0.073 Uiso 1 1 calc R . .

H7C H 0.7492 0.3184 0.4903 0.073 Uiso 1 1 calc R . .

C8 C 0.6361(3) 0.0731(3) 1.0432(3) 0.0241(5) Uani 1 1 d . . .

H8A H 0.6613 -0.0135 1.0988 0.029 Uiso 1 1 calc R . .

C9 C 0.4260(3) 0.0207(3) 1.2349(3) 0.0293(6) Uani 1 1 d . . .

H9A H 0.4593 0.0236 1.3024 0.035 Uiso 1 1 calc R . .

H9B H 0.4367 -0.0754 1.2377 0.035 Uiso 1 1 calc R . .

C10 C 0.2738(3) 0.0623(3) 1.2741(3) 0.0269(5) Uani 1 1 d . . .

H10A H 0.2353 0.0434 1.2178 0.032 Uiso 1 1 calc R . .

H10B H 0.2199 0.0079 1.3727 0.032 Uiso 1 1 calc R . .

C11 C 0.1163(3) 0.2606(3) 1.2897(3) 0.0271(5) Uani 1 1 d . . .

H11A H 0.0626 0.2105 1.3894 0.033 Uiso 1 1 calc R . .

H11B H 0.0718 0.2437 1.2369 0.033 Uiso 1 1 calc R . .

C12 C 0.1166(3) 0.4143(3) 1.2590(3) 0.0286(5) Uani 1 1 d . . .

H12A H 0.0199 0.4510 1.2806 0.034 Uiso 1 1 calc R . .

H12B H 0.1549 0.4305 1.3169 0.034 Uiso 1 1 calc R . .

C13 C 0.1617(2) 0.6048(3) 1.0508(3) 0.0234(5) Uani 1 1 d . . .

H13A H 0.0785 0.6412 1.1030 0.028 Uiso 1 1 calc R . .

C14 C 0.2350(3) 0.6892(2) 0.9045(3) 0.0213(5) Uani 1 1 d . . .

C15 C 0.1546(3) 0.7835(3) 0.8365(3) 0.0272(5) Uani 1 1 d . . .

H15A H 0.0585 0.7958 0.8874 0.033 Uiso 1 1 calc R . .

C16 C 0.2133(3) 0.8585(3) 0.6969(3) 0.0334(6) Uani 1 1 d . . .

H16A H 0.1582 0.9224 0.6514 0.040 Uiso 1 1 calc R . .

C17 C 0.3541(3) 0.8400(3) 0.6229(3) 0.0325(6) Uani 1 1 d . . .

H17A H 0.3944 0.8898 0.5260 0.039 Uiso 1 1 calc R . .

C18 C 0.4364(3) 0.7500(3) 0.6887(3) 0.0239(5) Uani 1 1 d . . .

C19 C 0.3796(2) 0.6750(2) 0.8321(3) 0.0188(4) Uani 1 1 d . . .

C20 C 0.6285(3) 0.7524(4) 0.4788(3) 0.0445(7) Uani 1 1 d . . .

H20A H 0.7288 0.7316 0.4457 0.067 Uiso 1 1 calc R . .

H20B H 0.6134 0.8499 0.4284 0.067 Uiso 1 1 calc R . .

H20C H 0.5798 0.6934 0.4635 0.067 Uiso 1 1 calc R . .

 


 

_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

Tb1 O1 2.1992(18) . ?

Tb1 O3 2.3297(16) 2_667 ?

Tb1 O3 2.3515(16) . ?

Tb1 O5 2.4383(18) . ?

Tb1 O6 2.5080(19) . ?

Tb1 N1 2.523(2) . ?

Tb1 N3 2.547(2) . ?

Tb1 N2 2.544(2) . ?

Tb1 N4 2.893(2) . ?

Tb1 Tb1 3.7883(2) 2_667 ?

N1 C8 1.278(3) . ?

N1 C9 1.475(3) . ?

N2 C10 1.472(3) . ?

N2 C11 1.470(3) . ?

N3 C13 1.274(3) . ?

N3 C12 1.471(3) . ?

N4 O7 1.213(3) . ?

N4 O6 1.259(3) . ?

N4 O5 1.278(3) . ?

O1 C1 1.303(3) . ?

O2 C2 1.380(3) . ?

O2 C7 1.428(4) . ?

O3 C19 1.341(3) . ?

O3 Tb1 2.3297(16) 2_667 ?

O4 C18 1.378(3) . ?

O4 C20 1.411(4) . ?

C1 C2 1.425(4) . ?

C1 C6 1.420(4) . ?

C2 C3 1.380(4) . ?

C3 C4 1.393(4) . ?

C4 C5 1.371(4) . ?

C5 C6 1.407(4) . ?

C6 C8 1.449(4) . ?

C9 C10 1.510(4) . ?

C11 C12 1.514(4) . ?

C13 C14 1.467(4) . ?

C14 C15 1.399(3) . ?

C14 C19 1.412(3) . ?

C15 C16 1.376(4) . ?

C16 C17 1.391(4) . ?

C17 C18 1.385(4) . ?

C18 C19 1.407(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 Tb1 O3 99.47(7) . 2_667 ?

O1 Tb1 O3 89.76(6) . . ?

O3 Tb1 O3 71.95(6) 2_667 . ?

O1 Tb1 O5 93.37(7) . . ?

O3 Tb1 O5 157.21(6) 2_667 . ?

O3 Tb1 O5 127.18(6) . . ?

O1 Tb1 O6 77.20(7) . . ?

O3 Tb1 O6 149.95(6) 2_667 . ?

O3 Tb1 O6 78.14(6) . . ?

O5 Tb1 O6 51.60(6) . . ?

O1 Tb1 N1 72.62(7) . . ?

O3 Tb1 N1 82.34(6) 2_667 . ?

O3 Tb1 N1 146.02(6) . . ?

O5 Tb1 N1 83.67(7) . . ?

O6 Tb1 N1 123.51(6) . . ?

O1 Tb1 N3 154.04(7) . . ?

O3 Tb1 N3 90.35(6) 2_667 . ?

O3 Tb1 N3 70.41(6) . . ?

O5 Tb1 N3 86.09(7) . . ?

O6 Tb1 N3 82.28(7) . . ?

N1 Tb1 N3 132.87(7) . . ?

O1 Tb1 N2 137.99(7) . . ?

O3 Tb1 N2 84.52(6) 2_667 . ?

O3 Tb1 N2 130.27(6) . . ?

O5 Tb1 N2 73.41(6) . . ?

O6 Tb1 N2 118.19(7) . . ?

N1 Tb1 N2 66.47(7) . . ?

N3 Tb1 N2 66.49(7) . . ?

O1 Tb1 N4 83.07(7) . . ?

O3 Tb1 N4 174.41(6) 2_667 . ?

O3 Tb1 N4 103.19(6) . . ?

O5 Tb1 N4 26.00(6) . . ?

O6 Tb1 N4 25.72(6) . . ?

N1 Tb1 N4 103.20(6) . . ?

N3 Tb1 N4 85.33(6) . . ?

N2 Tb1 N4 96.95(7) . . ?

O1 Tb1 Tb1 95.66(5) . 2_667 ?

O3 Tb1 Tb1 36.17(4) 2_667 2_667 ?

O3 Tb1 Tb1 35.78(4) . 2_667 ?

O5 Tb1 Tb1 160.40(5) . 2_667 ?

O6 Tb1 Tb1 113.87(4) . 2_667 ?

N1 Tb1 Tb1 115.64(5) . 2_667 ?

N3 Tb1 Tb1 78.21(5) . 2_667 ?

N2 Tb1 Tb1 110.03(4) . 2_667 ?

N4 Tb1 Tb1 138.91(5) . 2_667 ?

C8 N1 C9 114.9(2) . . ?

C8 N1 Tb1 126.28(17) . . ?

C9 N1 Tb1 117.81(16) . . ?

C10 N2 C11 113.05(19) . . ?

C10 N2 Tb1 111.04(15) . . ?

C11 N2 Tb1 112.32(15) . . ?

C13 N3 C12 116.9(2) . . ?

C13 N3 Tb1 126.52(18) . . ?

C12 N3 Tb1 116.58(16) . . ?

O7 N4 O6 122.8(2) . . ?

O7 N4 O5 121.1(2) . . ?

O6 N4 O5 116.2(2) . . ?

O7 N4 Tb1 173.2(2) . . ?

O6 N4 Tb1 59.81(12) . . ?

O5 N4 Tb1 56.73(11) . . ?

C1 O1 Tb1 137.30(16) . . ?

C2 O2 C7 113.8(2) . . ?

C19 O3 Tb1 128.72(13) . 2_667 ?

C19 O3 Tb1 118.16(13) . . ?

Tb1 O3 Tb1 108.05(6) 2_667 . ?

C18 O4 C20 119.0(2) . . ?

N4 O5 Tb1 97.27(13) . . ?

N4 O6 Tb1 94.47(14) . . ?

O1 C1 C2 120.5(2) . . ?

O1 C1 C6 122.9(2) . . ?

C2 C1 C6 116.5(2) . . ?

O2 C2 C3 118.2(2) . . ?

O2 C2 C1 120.6(2) . . ?

C3 C2 C1 120.9(3) . . ?

C2 C3 C4 121.3(3) . . ?

C5 C4 C3 119.2(3) . . ?

C4 C5 C6 120.9(3) . . ?

C5 C6 C1 120.8(2) . . ?

C5 C6 C8 117.1(2) . . ?

C1 C6 C8 122.2(2) . . ?

N1 C8 C6 127.6(2) . . ?

N1 C9 C10 110.6(2) . . ?

N2 C10 C9 109.0(2) . . ?

N2 C11 C12 108.5(2) . . ?

N3 C12 C11 108.9(2) . . ?

N3 C13 C14 123.8(2) . . ?

C15 C14 C19 120.4(2) . . ?

C15 C14 C13 117.2(2) . . ?

C19 C14 C13 122.4(2) . . ?

C16 C15 C14 120.7(2) . . ?

C17 C16 C15 119.4(2) . . ?

C16 C17 C18 120.8(3) . . ?

C17 C18 O4 123.6(2) . . ?

C17 C18 C19 120.8(2) . . ?

O4 C18 C19 115.6(2) . . ?

O3 C19 C18 120.0(2) . . ?

O3 C19 C14 122.3(2) . . ?

C18 C19 C14 117.7(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

O1 Tb1 N1 C8 25.4(2) . . . . ?

O3 Tb1 N1 C8 -77.0(2) 2_667 . . . ?

O3 Tb1 N1 C8 -36.4(3) . . . . ?

O5 Tb1 N1 C8 121.0(2) . . . . ?

O6 Tb1 N1 C8 86.4(2) . . . . ?

N3 Tb1 N1 C8 -160.35(18) . . . . ?

N2 Tb1 N1 C8 -164.4(2) . . . . ?

N4 Tb1 N1 C8 103.7(2) . . . . ?

Tb1 Tb1 N1 C8 -62.5(2) 2_667 . . . ?

O1 Tb1 N1 C9 -166.82(19) . . . . ?

O3 Tb1 N1 C9 90.70(18) 2_667 . . . ?

O3 Tb1 N1 C9 131.35(17) . . . . ?

O5 Tb1 N1 C9 -71.27(18) . . . . ?

O6 Tb1 N1 C9 -105.88(18) . . . . ?

N3 Tb1 N1 C9 7.4(2) . . . . ?

N2 Tb1 N1 C9 3.37(17) . . . . ?

N4 Tb1 N1 C9 -88.55(18) . . . . ?

Tb1 Tb1 N1 C9 105.22(17) 2_667 . . . ?

O1 Tb1 N2 C10 -16.4(2) . . . . ?

O3 Tb1 N2 C10 -114.50(16) 2_667 . . . ?

O3 Tb1 N2 C10 -175.22(14) . . . . ?

O5 Tb1 N2 C10 59.75(16) . . . . ?

O6 Tb1 N2 C10 86.25(17) . . . . ?

N1 Tb1 N2 C10 -30.49(15) . . . . ?

N3 Tb1 N2 C10 152.72(17) . . . . ?

N4 Tb1 N2 C10 70.92(16) . . . . ?

Tb1 Tb1 N2 C10 -140.59(14) 2_667 . . . ?

O1 Tb1 N2 C11 -144.12(15) . . . . ?

O3 Tb1 N2 C11 117.80(16) 2_667 . . . ?

O3 Tb1 N2 C11 57.09(18) . . . . ?

O5 Tb1 N2 C11 -67.94(16) . . . . ?

O6 Tb1 N2 C11 -41.44(17) . . . . ?

N1 Tb1 N2 C11 -158.18(17) . . . . ?

N3 Tb1 N2 C11 25.03(15) . . . . ?

N4 Tb1 N2 C11 -56.78(16) . . . . ?

Tb1 Tb1 N2 C11 91.72(15) 2_667 . . . ?

O1 Tb1 N3 C13 -8.5(3) . . . . ?

O3 Tb1 N3 C13 104.4(2) 2_667 . . . ?

O3 Tb1 N3 C13 33.69(19) . . . . ?

O5 Tb1 N3 C13 -98.2(2) . . . . ?

O6 Tb1 N3 C13 -46.4(2) . . . . ?

N1 Tb1 N3 C13 -175.79(18) . . . . ?

N2 Tb1 N3 C13 -171.8(2) . . . . ?

N4 Tb1 N3 C13 -72.1(2) . . . . ?

Tb1 Tb1 N3 C13 70.0(2) 2_667 . . . ?

O1 Tb1 N3 C12 169.00(17) . . . . ?

O3 Tb1 N3 C12 -78.14(17) 2_667 . . . ?

O3 Tb1 N3 C12 -148.82(18) . . . . ?

O5 Tb1 N3 C12 79.33(17) . . . . ?

O6 Tb1 N3 C12 131.09(17) . . . . ?

N1 Tb1 N3 C12 1.7(2) . . . . ?

N2 Tb1 N3 C12 5.73(16) . . . . ?

N4 Tb1 N3 C12 105.39(17) . . . . ?

Tb1 Tb1 N3 C12 -112.46(17) 2_667 . . . ?

O1 Tb1 N4 O7 39.4(17) . . . . ?

O3 Tb1 N4 O7 156.7(15) 2_667 . . . ?

O3 Tb1 N4 O7 127.5(17) . . . . ?

O5 Tb1 N4 O7 -73.3(17) . . . . ?

O6 Tb1 N4 O7 114.2(18) . . . . ?

N1 Tb1 N4 O7 -30.9(17) . . . . ?

N3 Tb1 N4 O7 -163.9(17) . . . . ?

N2 Tb1 N4 O7 -98.3(17) . . . . ?

Tb1 Tb1 N4 O7 130.0(17) 2_667 . . . ?

O1 Tb1 N4 O6 -74.82(15) . . . . ?

O3 Tb1 N4 O6 42.6(7) 2_667 . . . ?

O3 Tb1 N4 O6 13.30(16) . . . . ?

O5 Tb1 N4 O6 172.6(2) . . . . ?

N1 Tb1 N4 O6 -145.10(15) . . . . ?

N3 Tb1 N4 O6 81.91(15) . . . . ?

N2 Tb1 N4 O6 147.51(15) . . . . ?

Tb1 Tb1 N4 O6 15.85(18) 2_667 . . . ?

O1 Tb1 N4 O5 112.61(16) . . . . ?

O3 Tb1 N4 O5 -130.0(6) 2_667 . . . ?

O3 Tb1 N4 O5 -159.27(15) . . . . ?

O6 Tb1 N4 O5 -172.6(2) . . . . ?

N1 Tb1 N4 O5 42.34(16) . . . . ?

N3 Tb1 N4 O5 -90.65(15) . . . . ?

N2 Tb1 N4 O5 -25.05(16) . . . . ?

Tb1 Tb1 N4 O5 -156.71(13) 2_667 . . . ?

O3 Tb1 O1 C1 41.1(2) 2_667 . . . ?

O3 Tb1 O1 C1 112.8(2) . . . . ?

O5 Tb1 O1 C1 -120.0(2) . . . . ?

O6 Tb1 O1 C1 -169.3(2) . . . . ?

N1 Tb1 O1 C1 -37.7(2) . . . . ?

N3 Tb1 O1 C1 152.0(2) . . . . ?

N2 Tb1 O1 C1 -51.2(3) . . . . ?

N4 Tb1 O1 C1 -143.9(2) . . . . ?

Tb1 Tb1 O1 C1 77.4(2) 2_667 . . . ?

O1 Tb1 O3 C19 102.94(17) . . . . ?

O3 Tb1 O3 C19 -157.0(2) 2_667 . . . ?

O5 Tb1 O3 C19 8.88(19) . . . . ?

O6 Tb1 O3 C19 25.97(16) . . . . ?

N1 Tb1 O3 C19 160.22(16) . . . . ?

N3 Tb1 O3 C19 -59.97(16) . . . . ?

N2 Tb1 O3 C19 -91.07(17) . . . . ?

N4 Tb1 O3 C19 20.11(18) . . . . ?

Tb1 Tb1 O3 C19 -157.0(2) 2_667 . . . ?

O1 Tb1 O3 Tb1 -100.05(8) . . . 2_667 ?

O3 Tb1 O3 Tb1 0.0 2_667 . . 2_667 ?

O5 Tb1 O3 Tb1 165.90(7) . . . 2_667 ?

O6 Tb1 O3 Tb1 -177.01(8) . . . 2_667 ?

N1 Tb1 O3 Tb1 -42.76(14) . . . 2_667 ?

N3 Tb1 O3 Tb1 97.05(8) . . . 2_667 ?

N2 Tb1 O3 Tb1 65.94(10) . . . 2_667 ?

N4 Tb1 O3 Tb1 177.13(6) . . . 2_667 ?

O7 N4 O5 Tb1 172.4(2) . . . . ?

O6 N4 O5 Tb1 -7.2(2) . . . . ?

O1 Tb1 O5 N4 -66.63(15) . . . . ?

O3 Tb1 O5 N4 168.90(14) 2_667 . . . ?

O3 Tb1 O5 N4 25.63(18) . . . . ?

O6 Tb1 O5 N4 4.11(13) . . . . ?

N1 Tb1 O5 N4 -138.72(16) . . . . ?

N3 Tb1 O5 N4 87.36(15) . . . . ?

N2 Tb1 O5 N4 153.99(16) . . . . ?

Tb1 Tb1 O5 N4 50.8(2) 2_667 . . . ?

O7 N4 O6 Tb1 -172.7(2) . . . . ?

O5 N4 O6 Tb1 6.9(2) . . . . ?

O1 Tb1 O6 N4 100.74(15) . . . . ?

O3 Tb1 O6 N4 -172.45(13) 2_667 . . . ?

O3 Tb1 O6 N4 -166.77(16) . . . . ?

O5 Tb1 O6 N4 -4.15(14) . . . . ?

N1 Tb1 O6 N4 41.92(18) . . . . ?

N3 Tb1 O6 N4 -95.27(15) . . . . ?

N2 Tb1 O6 N4 -37.22(17) . . . . ?

Tb1 Tb1 O6 N4 -168.68(13) 2_667 . . . ?

Tb1 O1 C1 C2 -148.41(19) . . . . ?

Tb1 O1 C1 C6 31.4(4) . . . . ?

C7 O2 C2 C3 120.8(3) . . . . ?

C7 O2 C2 C1 -64.2(3) . . . . ?

O1 C1 C2 O2 -2.4(4) . . . . ?

C6 C1 C2 O2 177.9(2) . . . . ?

O1 C1 C2 C3 172.5(2) . . . . ?

C6 C1 C2 C3 -7.3(3) . . . . ?

O2 C2 C3 C4 179.9(2) . . . . ?

C1 C2 C3 C4 4.9(4) . . . . ?

C2 C3 C4 C5 0.7(4) . . . . ?

C3 C4 C5 C6 -3.5(4) . . . . ?

C4 C5 C6 C1 0.9(4) . . . . ?

C4 C5 C6 C8 -179.4(2) . . . . ?

O1 C1 C6 C5 -175.3(2) . . . . ?

C2 C1 C6 C5 4.4(3) . . . . ?

O1 C1 C6 C8 5.0(4) . . . . ?

C2 C1 C6 C8 -175.3(2) . . . . ?

C9 N1 C8 C6 -179.6(2) . . . . ?

Tb1 N1 C8 C6 -11.5(4) . . . . ?

C5 C6 C8 N1 169.4(2) . . . . ?

C1 C6 C8 N1 -10.9(4) . . . . ?

C8 N1 C9 C10 -167.6(2) . . . . ?

Tb1 N1 C9 C10 23.3(3) . . . . ?

C11 N2 C10 C9 -178.1(2) . . . . ?

Tb1 N2 C10 C9 54.6(2) . . . . ?

N1 C9 C10 N2 -51.0(3) . . . . ?

C10 N2 C11 C12 -179.3(2) . . . . ?

Tb1 N2 C11 C12 -52.7(2) . . . . ?

C13 N3 C12 C11 143.4(2) . . . . ?

Tb1 N3 C12 C11 -34.3(3) . . . . ?

N2 C11 C12 N3 56.7(3) . . . . ?

C12 N3 C13 C14 -179.6(2) . . . . ?

Tb1 N3 C13 C14 -2.1(3) . . . . ?

N3 C13 C14 C15 153.1(2) . . . . ?

N3 C13 C14 C19 -25.3(4) . . . . ?

C19 C14 C15 C16 3.5(4) . . . . ?

C13 C14 C15 C16 -174.8(2) . . . . ?

C14 C15 C16 C17 0.0(4) . . . . ?

C15 C16 C17 C18 -1.7(4) . . . . ?

C16 C17 C18 O4 179.8(3) . . . . ?

C16 C17 C18 C19 -0.1(4) . . . . ?

C20 O4 C18 C17 -23.9(4) . . . . ?

C20 O4 C18 C19 156.0(3) . . . . ?

Tb1 O3 C19 C18 91.3(2) 2_667 . . . ?

Tb1 O3 C19 C18 -117.1(2) . . . . ?

Tb1 O3 C19 C14 -89.3(2) 2_667 . . . ?

Tb1 O3 C19 C14 62.3(3) . . . . ?

C17 C18 C19 O3 -177.1(2) . . . . ?

O4 C18 C19 O3 3.0(3) . . . . ?

C17 C18 C19 C14 3.5(4) . . . . ?

O4 C18 C19 C14 -176.4(2) . . . . ?

C15 C14 C19 O3 175.5(2) . . . . ?

C13 C14 C19 O3 -6.3(3) . . . . ?

C15 C14 C19 C18 -5.2(3) . . . . ?

C13 C14 C19 C18 173.1(2) . . . . ?

 

_diffrn_measured_fraction_theta_max    0.974

_diffrn_reflns_theta_full              27.88

_diffrn_measured_fraction_theta_full   0.974

_refine_diff_density_max    0.702

_refine_diff_density_min   -1.048

_refine_diff_density_rms    0.116

 
data_mm002 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C40 H46 Ho2 N8 O14' 
_chemical_formula_weight          1192.71 
  
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ho'  'Ho'  -0.2175   4.6783 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    10.5104(4) 
_cell_length_b                    10.5297(4) 
_cell_length_c                    11.4828(4) 
_cell_angle_alpha                 66.414(2) 
_cell_angle_beta                  65.1260(10) 
_cell_angle_gamma                 79.981(2) 
_cell_volume                      1056.59(7) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     9900 
_cell_measurement_theta_min       2.34 
_cell_measurement_theta_max       28.31 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.21 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.874 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              588 
_exptl_absorpt_coefficient_mu     3.795 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5029 
_exptl_absorpt_correction_T_max   0.5174 
_exptl_absorpt_process_details    'SADABS, Bruker (2003)' 
  
_exptl_special_details 
; 
 Data collection is performed with three batch runs at phi = 0.00 deg 
 (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg 
 (650 frames). 
 Frame width = 0.30 deg in omega. 
 Data is merged, corrected for decay (if any), and treated with multi-scan 
 absorption corrections (if required). All symmetry-equivalent reflections 
 are merged for centrosymmetric data. 
 Friedel pairs are not merged for noncentrosymmetric data. 
; 
  
_diffrn_ambient_temperature       200(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker APEX-II CCD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             16595 
_diffrn_reflns_av_R_equivalents   0.0139 
_diffrn_reflns_av_sigmaI/netI     0.0132 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.11 
_diffrn_reflns_theta_max          28.31 
_reflns_number_total              5157 
_reflns_number_gt                 5109 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'APEX II, Bruker (2009)' 
_computing_cell_refinement        'APEX II, Bruker (2009)' 
_computing_data_reduction         'XPREP, Bruker (2009)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'SHELXTL, Bruker (2004)' 
_computing_publication_material   'SHELXTL, Bruker (2004)' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0218P)²+0.3973P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5157 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0131 
_refine_ls_R_factor_gt            0.0130 
_refine_ls_wR_factor_ref          0.0347 
_refine_ls_wR_factor_gt           0.0346 
_refine_ls_goodness_of_fit_ref    1.057 
_refine_ls_restrained_S_all       1.057 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ho1 Ho 0.414833(6) 0.854317(6) 0.504937(5) 0.01624(3) Uani 1 1 d . . . 
N1 N 0.20284(13) 0.98648(14) 0.61018(13) 0.0224(2) Uani 1 1 d . . . 
N2 N 0.26166(14) 0.71379(14) 0.74905(13) 0.0222(2) Uani 1 1 d . . . 
H2A H 0.2958 0.7271 0.8060 0.027 Uiso 1 1 calc R . . 
N3 N 0.51119(14) 0.61757(14) 0.59559(13) 0.0228(2) Uani 1 1 d . . . 
N4 N 0.25357(15) 0.81236(16) 0.37453(14) 0.0256(3) Uani 1 1 d . . . 
O1 O 0.46244(11) 1.09058(11) 0.39589(10) 0.01839(19) Uani 1 1 d . . . 
O2 O 0.57789(12) 1.22029(14) 0.12191(12) 0.0301(3) Uani 1 1 d . . . 
O3 O 0.59087(12) 0.82174(12) 0.33048(11) 0.0262(2) Uani 1 1 d . . . 
O4 O 0.80483(14) 0.92459(14) 0.06964(12) 0.0320(3) Uani 1 1 d . . . 
O5 O 0.31606(14) 0.92485(13) 0.32516(13) 0.0324(3) Uani 1 1 d . . . 
O6 O 0.25489(14) 0.72743(13) 0.49090(13) 0.0315(3) Uani 1 1 d . . . 
O7 O 0.19471(18) 0.78403(18) 0.31705(16) 0.0479(4) Uani 1 1 d . . . 
C1 C 0.38063(15) 1.17336(15) 0.33159(15) 0.0180(3) Uani 1 1 d . . . 
C2 C 0.43826(16) 1.24592(17) 0.18767(15) 0.0226(3) Uani 1 1 d . . . 
C3 C 0.35660(19) 1.33648(19) 0.12063(17) 0.0296(3) Uani 1 1 d . . . 
H3A H 0.3973 1.3848 0.0237 0.035 Uiso 1 1 calc R . . 
C4 C 0.21560(19) 1.35743(19) 0.19384(19) 0.0320(4) Uani 1 1 d . . . 
H4A H 0.1608 1.4215 0.1477 0.038 Uiso 1 1 calc R . . 
C5 C 0.15628(17) 1.28435(18) 0.33388(18) 0.0273(3) Uani 1 1 d . . . 
H5A H 0.0602 1.2986 0.3844 0.033 Uiso 1 1 calc R . . 
C6 C 0.23618(15) 1.18940(16) 0.40231(15) 0.0207(3) Uani 1 1 d . . . 
C7 C 0.6305(2) 1.2542(2) -0.02251(18) 0.0384(4) Uani 1 1 d . . . 
H7A H 0.7307 1.2315 -0.0564 0.058 Uiso 1 1 calc R . . 
H7B H 0.6169 1.3536 -0.0680 0.058 Uiso 1 1 calc R . . 
H7C H 0.5802 1.2011 -0.0430 0.058 Uiso 1 1 calc R . . 
C8 C 0.16223(16) 1.10602(17) 0.54790(16) 0.0232(3) Uani 1 1 d . . . 
H8A H 0.0787 1.1432 0.5993 0.028 Uiso 1 1 calc R . . 
C9 C 0.11532(18) 0.91680(18) 0.75683(16) 0.0290(3) Uani 1 1 d . . . 
H9A H 0.0183 0.9537 0.7774 0.035 Uiso 1 1 calc R . . 
H9B H 0.1530 0.9338 0.8151 0.035 Uiso 1 1 calc R . . 
C10 C 0.11571(17) 0.76301(18) 0.78755(16) 0.0265(3) Uani 1 1 d . . . 
H10A H 0.0615 0.7132 0.8869 0.032 Uiso 1 1 calc R . . 
H10B H 0.0719 0.7454 0.7342 0.032 Uiso 1 1 calc R . . 
C11 C 0.27467(18) 0.56442(17) 0.77440(16) 0.0269(3) Uani 1 1 d . . . 
H11A H 0.2361 0.5438 0.7187 0.032 Uiso 1 1 calc R . . 
H11B H 0.2210 0.5110 0.8730 0.032 Uiso 1 1 calc R . . 
C12 C 0.4276(2) 0.52361(18) 0.73536(17) 0.0303(3) Uani 1 1 d . . . 
H12A H 0.4612 0.5280 0.8023 0.036 Uiso 1 1 calc R . . 
H12B H 0.4394 0.4272 0.7383 0.036 Uiso 1 1 calc R . . 
C13 C 0.63662(18) 0.57503(16) 0.54271(17) 0.0248(3) Uani 1 1 d . . . 
H13A H 0.6623 0.4883 0.5978 0.030 Uiso 1 1 calc R . . 
C14 C 0.71351(17) 0.76177(17) 0.30732(16) 0.0225(3) Uani 1 1 d . . . 
C15 C 0.74336(17) 0.64405(16) 0.40878(16) 0.0231(3) Uani 1 1 d . . . 
C16 C 0.88053(18) 0.58886(18) 0.38287(19) 0.0289(3) Uani 1 1 d . . . 
H16A H 0.8985 0.5095 0.4518 0.035 Uiso 1 1 calc R . . 
C17 C 0.98809(18) 0.6490(2) 0.2589(2) 0.0331(4) Uani 1 1 d . . . 
H17A H 1.0813 0.6150 0.2437 0.040 Uiso 1 1 calc R . . 
C18 C 0.95948(18) 0.7605(2) 0.15542(19) 0.0324(4) Uani 1 1 d . . . 
H18A H 1.0338 0.8010 0.0689 0.039 Uiso 1 1 calc R . . 
C19 C 0.82524(17) 0.81315(18) 0.17623(16) 0.0257(3) Uani 1 1 d . . . 
C20 C 0.7062(3) 0.8996(3) 0.0260(2) 0.0483(5) Uani 1 1 d . . . 
H20A H 0.6975 0.9825 -0.0500 0.072 Uiso 1 1 calc R . . 
H20B H 0.6148 0.8778 0.1032 0.072 Uiso 1 1 calc R . . 
H20C H 0.7386 0.8214 -0.0055 0.072 Uiso 1 1 calc R . . 
  
  
_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 
Ho1 O3 2.1829(11) . ? 
Ho1 O1 2.3070(10) 2_676 ? 
Ho1 O1 2.3282(11) . ? 
Ho1 O6 2.4123(12) . ? 
Ho1 O5 2.4897(12) . ? 
Ho1 N3 2.5011(13) . ? 
Ho1 N2 2.5203(13) . ? 
Ho1 N1 2.5225(13) . ? 
Ho1 N4 2.8697(13) . ? 
Ho1 Ho1 3.75402(17) 2_676 ? 
N1 C8 1.276(2) . ? 
N1 C9 1.4708(19) . ? 
N2 C10 1.467(2) . ? 
N2 C11 1.473(2) . ? 
N3 C13 1.283(2) . ? 
N3 C12 1.474(2) . ? 
N4 O7 1.2135(18) . ? 
N4 O5 1.2553(19) . ? 
N4 O6 1.2808(19) . ? 
O1 C1 1.3426(17) . ? 
O1 Ho1 2.3070(10) 2_676 ? 
O2 C2 1.3747(19) . ? 
O2 C7 1.416(2) . ? 
O3 C14 1.3015(19) . ? 
O4 C19 1.380(2) . ? 
O4 C20 1.426(2) . ? 
C1 C2 1.411(2) . ? 
C1 C6 1.406(2) . ? 
C2 C3 1.386(2) . ? 
C3 C4 1.392(3) . ? 
C4 C5 1.378(2) . ? 
C5 C6 1.399(2) . ? 
C6 C8 1.463(2) . ? 
C9 C10 1.513(2) . ? 
C11 C12 1.509(3) . ? 
C13 C15 1.446(2) . ? 
C14 C15 1.417(2) . ? 
C14 C19 1.421(2) . ? 
C15 C16 1.411(2) . ? 
C16 C17 1.371(3) . ? 
C17 C18 1.393(3) . ? 
C18 C19 1.380(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 
O3 Ho1 O1 99.21(4) . 2_676 ? 
O3 Ho1 O1 88.50(4) . . ? 
O1 Ho1 O1 71.83(4) 2_676 . ? 
O3 Ho1 O6 92.99(5) . . ? 
O1 Ho1 O6 157.35(4) 2_676 . ? 
O1 Ho1 O6 127.86(4) . . ? 
O3 Ho1 O5 77.06(4) . . ? 
O1 Ho1 O5 149.62(4) 2_676 . ? 
O1 Ho1 O5 77.91(4) . . ? 
O6 Ho1 O5 52.02(4) . . ? 
O3 Ho1 N3 73.04(4) . . ? 
O1 Ho1 N3 82.59(4) 2_676 . ? 
O1 Ho1 N3 145.63(4) . . ? 
O6 Ho1 N3 82.82(4) . . ? 
O5 Ho1 N3 123.49(4) . . ? 
O3 Ho1 N2 138.61(4) . . ? 
O1 Ho1 N2 85.18(4) 2_676 . ? 
O1 Ho1 N2 131.04(4) . . ? 
O6 Ho1 N2 73.15(4) . . ? 
O5 Ho1 N2 117.79(4) . . ? 
N3 Ho1 N2 66.73(4) . . ? 
O3 Ho1 N1 152.93(4) . . ? 
O1 Ho1 N1 90.98(4) 2_676 . ? 
O1 Ho1 N1 70.87(4) . . ? 
O6 Ho1 N1 86.58(5) . . ? 
O5 Ho1 N1 81.49(4) . . ? 
N3 Ho1 N1 133.50(4) . . ? 
N2 Ho1 N1 66.85(4) . . ? 
O3 Ho1 N4 82.69(4) . . ? 
O1 Ho1 N4 174.63(4) 2_676 . ? 
O1 Ho1 N4 103.29(4) . . ? 
O6 Ho1 N4 26.28(4) . . ? 
O5 Ho1 N4 25.86(4) . . ? 
N3 Ho1 N4 102.78(4) . . ? 
N2 Ho1 N4 96.73(4) . . ? 
N1 Ho1 N4 85.19(4) . . ? 
O3 Ho1 Ho1 94.71(3) . 2_676 ? 
O1 Ho1 Ho1 36.10(3) 2_676 2_676 ? 
O1 Ho1 Ho1 35.73(2) . 2_676 ? 
O6 Ho1 Ho1 161.39(3) . 2_676 ? 
O5 Ho1 Ho1 113.60(3) . 2_676 ? 
N3 Ho1 Ho1 115.64(3) . 2_676 ? 
N2 Ho1 Ho1 110.83(3) . 2_676 ? 
N1 Ho1 Ho1 78.89(3) . 2_676 ? 
N4 Ho1 Ho1 138.97(3) . 2_676 ? 
C8 N1 C9 116.92(13) . . ? 
C8 N1 Ho1 126.43(10) . . ? 
C9 N1 Ho1 116.62(10) . . ? 
C10 N2 C11 113.00(13) . . ? 
C10 N2 Ho1 112.30(9) . . ? 
C11 N2 Ho1 111.43(9) . . ? 
C13 N3 C12 114.38(14) . . ? 
C13 N3 Ho1 126.46(11) . . ? 
C12 N3 Ho1 118.18(10) . . ? 
O7 N4 O5 122.88(15) . . ? 
O7 N4 O6 121.11(15) . . ? 
O5 N4 O6 116.01(13) . . ? 
O7 N4 Ho1 173.46(13) . . ? 
O5 N4 Ho1 59.91(8) . . ? 
O6 N4 Ho1 56.51(7) . . ? 
C1 O1 Ho1 128.36(9) . 2_676 ? 
C1 O1 Ho1 118.52(9) . . ? 
Ho1 O1 Ho1 108.17(4) 2_676 . ? 
C2 O2 C7 117.66(13) . . ? 
C14 O3 Ho1 137.77(10) . . ? 
C19 O4 C20 113.93(15) . . ? 
N4 O5 Ho1 94.23(9) . . ? 
N4 O6 Ho1 97.21(9) . . ? 
O1 C1 C2 120.12(13) . . ? 
O1 C1 C6 122.31(13) . . ? 
C2 C1 C6 117.56(13) . . ? 
O2 C2 C3 123.77(14) . . ? 
O2 C2 C1 115.41(13) . . ? 
C3 C2 C1 120.82(15) . . ? 
C2 C3 C4 120.70(15) . . ? 
C5 C4 C3 119.36(15) . . ? 
C4 C5 C6 120.62(15) . . ? 
C5 C6 C1 120.70(14) . . ? 
C5 C6 C8 117.18(14) . . ? 
C1 C6 C8 122.10(13) . . ? 
N1 C8 C6 124.13(14) . . ? 
N1 C9 C10 108.57(13) . . ? 
N2 C10 C9 108.31(13) . . ? 
N2 C11 C12 108.85(13) . . ? 
N3 C12 C11 110.11(13) . . ? 
N3 C13 C15 127.39(15) . . ? 
O3 C14 C15 122.80(14) . . ? 
O3 C14 C19 120.54(15) . . ? 
C15 C14 C19 116.66(14) . . ? 
C16 C15 C14 120.91(15) . . ? 
C16 C15 C13 116.80(15) . . ? 
C14 C15 C13 122.29(14) . . ? 
C17 C16 C15 120.46(16) . . ? 
C16 C17 C18 119.41(16) . . ? 
C19 C18 C17 121.24(17) . . ? 
O4 C19 C18 118.11(15) . . ? 
O4 C19 C14 120.80(15) . . ? 
C18 C19 C14 120.88(16) . . ? 
  
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 
O3 Ho1 N1 C8 -9.23(19) . . . . ? 
O1 Ho1 N1 C8 103.43(13) 2_676 . . . ? 
O1 Ho1 N1 C8 33.07(13) . . . . ? 
O6 Ho1 N1 C8 -99.11(13) . . . . ? 
O5 Ho1 N1 C8 -47.01(13) . . . . ? 
N3 Ho1 N1 C8 -175.85(12) . . . . ? 
N2 Ho1 N1 C8 -172.23(14) . . . . ? 
N4 Ho1 N1 C8 -72.79(13) . . . . ? 
Ho1 Ho1 N1 C8 69.21(13) 2_676 . . . ? 
O3 Ho1 N1 C9 168.82(11) . . . . ? 
O1 Ho1 N1 C9 -78.52(11) 2_676 . . . ? 
O1 Ho1 N1 C9 -148.88(12) . . . . ? 
O6 Ho1 N1 C9 78.94(11) . . . . ? 
O5 Ho1 N1 C9 131.03(12) . . . . ? 
N3 Ho1 N1 C9 2.19(14) . . . . ? 
N2 Ho1 N1 C9 5.81(11) . . . . ? 
N4 Ho1 N1 C9 105.25(11) . . . . ? 
Ho1 Ho1 N1 C9 -112.74(11) 2_676 . . . ? 
O3 Ho1 N2 C10 -143.29(10) . . . . ? 
O1 Ho1 N2 C10 118.24(10) 2_676 . . . ? 
O1 Ho1 N2 C10 57.48(11) . . . . ? 
O6 Ho1 N2 C10 -68.43(10) . . . . ? 
O5 Ho1 N2 C10 -40.86(11) . . . . ? 
N3 Ho1 N2 C10 -157.76(11) . . . . ? 
N1 Ho1 N2 C10 25.10(10) . . . . ? 
N4 Ho1 N2 C10 -56.71(10) . . . . ? 
Ho1 Ho1 N2 C10 92.35(10) 2_676 . . . ? 
O3 Ho1 N2 C11 -15.37(13) . . . . ? 
O1 Ho1 N2 C11 -113.84(10) 2_676 . . . ? 
O1 Ho1 N2 C11 -174.61(9) . . . . ? 
O6 Ho1 N2 C11 59.49(10) . . . . ? 
O5 Ho1 N2 C11 87.06(11) . . . . ? 
N3 Ho1 N2 C11 -29.84(10) . . . . ? 
N1 Ho1 N2 C11 153.02(11) . . . . ? 
N4 Ho1 N2 C11 71.21(10) . . . . ? 
Ho1 Ho1 N2 C11 -139.73(9) 2_676 . . . ? 
O3 Ho1 N3 C13 24.55(13) . . . . ? 
O1 Ho1 N3 C13 -77.48(13) 2_676 . . . ? 
O1 Ho1 N3 C13 -35.81(16) . . . . ? 
O6 Ho1 N3 C13 119.90(13) . . . . ? 
O5 Ho1 N3 C13 85.69(14) . . . . ? 
N2 Ho1 N3 C13 -165.40(14) . . . . ? 
N1 Ho1 N3 C13 -161.77(12) . . . . ? 
N4 Ho1 N3 C13 102.69(13) . . . . ? 
Ho1 Ho1 N3 C13 -62.52(13) 2_676 . . . ? 
O3 Ho1 N3 C12 -167.50(12) . . . . ? 
O1 Ho1 N3 C12 90.48(12) 2_676 . . . ? 
O1 Ho1 N3 C12 132.14(11) . . . . ? 
O6 Ho1 N3 C12 -72.14(12) . . . . ? 
O5 Ho1 N3 C12 -106.35(12) . . . . ? 
N2 Ho1 N3 C12 2.56(11) . . . . ? 
N1 Ho1 N3 C12 6.18(14) . . . . ? 
N4 Ho1 N3 C12 -89.35(12) . . . . ? 
Ho1 Ho1 N3 C12 105.44(11) 2_676 . . . ? 
O3 Ho1 N4 O7 41.7(11) . . . . ? 
O1 Ho1 N4 O7 152.8(10) 2_676 . . . ? 
O1 Ho1 N4 O7 128.4(11) . . . . ? 
O6 Ho1 N4 O7 -70.6(11) . . . . ? 
O5 Ho1 N4 O7 117.0(12) . . . . ? 
N3 Ho1 N4 O7 -29.0(11) . . . . ? 
N2 Ho1 N4 O7 -96.6(11) . . . . ? 
N1 Ho1 N4 O7 -162.6(11) . . . . ? 
Ho1 Ho1 N4 O7 130.5(11) 2_676 . . . ? 
O3 Ho1 N4 O5 -75.34(10) . . . . ? 
O1 Ho1 N4 O5 35.8(4) 2_676 . . . ? 
O1 Ho1 N4 O5 11.37(10) . . . . ? 
O6 Ho1 N4 O5 172.42(16) . . . . ? 
N3 Ho1 N4 O5 -146.03(10) . . . . ? 
N2 Ho1 N4 O5 146.38(10) . . . . ? 
N1 Ho1 N4 O5 80.40(10) . . . . ? 
Ho1 Ho1 N4 O5 13.44(12) 2_676 . . . ? 
O3 Ho1 N4 O6 112.24(10) . . . . ? 
O1 Ho1 N4 O6 -136.7(4) 2_676 . . . ? 
O1 Ho1 N4 O6 -161.06(9) . . . . ? 
O5 Ho1 N4 O6 -172.42(15) . . . . ? 
N3 Ho1 N4 O6 41.55(10) . . . . ? 
N2 Ho1 N4 O6 -26.05(10) . . . . ? 
N1 Ho1 N4 O6 -92.02(10) . . . . ? 
Ho1 Ho1 N4 O6 -158.98(8) 2_676 . . . ? 
O3 Ho1 O1 C1 102.64(10) . . . . ? 
O1 Ho1 O1 C1 -157.16(12) 2_676 . . . ? 
O6 Ho1 O1 C1 10.02(12) . . . . ? 
O5 Ho1 O1 C1 25.55(10) . . . . ? 
N3 Ho1 O1 C1 158.90(9) . . . . ? 
N2 Ho1 O1 C1 -90.93(10) . . . . ? 
N1 Ho1 O1 C1 -59.52(10) . . . . ? 
N4 Ho1 O1 C1 20.50(10) . . . . ? 
Ho1 Ho1 O1 C1 -157.16(12) 2_676 . . . ? 
O3 Ho1 O1 Ho1 -100.20(5) . . . 2_676 ? 
O1 Ho1 O1 Ho1 0.0 2_676 . . 2_676 ? 
O6 Ho1 O1 Ho1 167.18(4) . . . 2_676 ? 
O5 Ho1 O1 Ho1 -177.29(5) . . . 2_676 ? 
N3 Ho1 O1 Ho1 -43.93(9) . . . 2_676 ? 
N2 Ho1 O1 Ho1 66.24(6) . . . 2_676 ? 
N1 Ho1 O1 Ho1 97.64(5) . . . 2_676 ? 
N4 Ho1 O1 Ho1 177.67(4) . . . 2_676 ? 
O1 Ho1 O3 C14 42.81(16) 2_676 . . . ? 
O1 Ho1 O3 C14 114.13(16) . . . . ? 
O6 Ho1 O3 C14 -118.04(16) . . . . ? 
O5 Ho1 O3 C14 -167.93(17) . . . . ? 
N3 Ho1 O3 C14 -36.47(16) . . . . ? 
N2 Ho1 O3 C14 -50.35(19) . . . . ? 
N1 Ho1 O3 C14 153.63(14) . . . . ? 
N4 Ho1 O3 C14 -142.27(16) . . . . ? 
Ho1 Ho1 O3 C14 78.92(16) 2_676 . . . ? 
O7 N4 O5 Ho1 -173.06(15) . . . . ? 
O6 N4 O5 Ho1 7.03(14) . . . . ? 
O3 Ho1 O5 N4 100.07(10) . . . . ? 
O1 Ho1 O5 N4 -173.79(8) 2_676 . . . ? 
O1 Ho1 O5 N4 -168.69(10) . . . . ? 
O6 Ho1 O5 N4 -4.25(9) . . . . ? 
N3 Ho1 O5 N4 40.80(11) . . . . ? 
N2 Ho1 O5 N4 -38.43(11) . . . . ? 
N1 Ho1 O5 N4 -96.55(10) . . . . ? 
Ho1 Ho1 O5 N4 -170.42(8) 2_676 . . . ? 
O7 N4 O6 Ho1 172.79(15) . . . . ? 
O5 N4 O6 Ho1 -7.29(15) . . . . ? 
O3 Ho1 O6 N4 -66.83(10) . . . . ? 
O1 Ho1 O6 N4 170.40(9) 2_676 . . . ? 
O1 Ho1 O6 N4 23.59(11) . . . . ? 
O5 Ho1 O6 N4 4.18(9) . . . . ? 
N3 Ho1 O6 N4 -139.31(10) . . . . ? 
N2 Ho1 O6 N4 152.89(10) . . . . ? 
N1 Ho1 O6 N4 86.06(10) . . . . ? 
Ho1 Ho1 O6 N4 47.54(16) 2_676 . . . ? 
Ho1 O1 C1 C2 91.39(15) 2_676 . . . ? 
Ho1 O1 C1 C2 -116.66(13) . . . . ? 
Ho1 O1 C1 C6 -89.91(16) 2_676 . . . ? 
Ho1 O1 C1 C6 62.04(16) . . . . ? 
C7 O2 C2 C3 -19.3(2) . . . . ? 
C7 O2 C2 C1 160.98(16) . . . . ? 
O1 C1 C2 O2 2.6(2) . . . . ? 
C6 C1 C2 O2 -176.12(13) . . . . ? 
O1 C1 C2 C3 -177.14(15) . . . . ? 
C6 C1 C2 C3 4.1(2) . . . . ? 
O2 C2 C3 C4 179.97(16) . . . . ? 
C1 C2 C3 C4 -0.3(3) . . . . ? 
C2 C3 C4 C5 -1.7(3) . . . . ? 
C3 C4 C5 C6 -0.3(3) . . . . ? 
C4 C5 C6 C1 4.3(2) . . . . ? 
C4 C5 C6 C8 -173.97(16) . . . . ? 
O1 C1 C6 C5 175.18(14) . . . . ? 
C2 C1 C6 C5 -6.1(2) . . . . ? 
O1 C1 C6 C8 -6.6(2) . . . . ? 
C2 C1 C6 C8 172.10(14) . . . . ? 
C9 N1 C8 C6 -179.74(14) . . . . ? 
Ho1 N1 C8 C6 -1.7(2) . . . . ? 
C5 C6 C8 N1 153.43(16) . . . . ? 
C1 C6 C8 N1 -24.8(2) . . . . ? 
C8 N1 C9 C10 143.81(15) . . . . ? 
Ho1 N1 C9 C10 -34.42(17) . . . . ? 
C11 N2 C10 C9 -179.86(13) . . . . ? 
Ho1 N2 C10 C9 -52.77(14) . . . . ? 
N1 C9 C10 N2 56.71(17) . . . . ? 
C10 N2 C11 C12 -178.44(13) . . . . ? 
Ho1 N2 C11 C12 54.02(14) . . . . ? 
C13 N3 C12 C11 -166.59(14) . . . . ? 
Ho1 N3 C12 C11 24.03(18) . . . . ? 
N2 C11 C12 N3 -50.74(18) . . . . ? 
C12 N3 C13 C15 -179.52(16) . . . . ? 
Ho1 N3 C13 C15 -11.2(2) . . . . ? 
Ho1 O3 C14 C15 30.2(2) . . . . ? 
Ho1 O3 C14 C19 -149.75(13) . . . . ? 
O3 C14 C15 C16 -174.96(15) . . . . ? 
C19 C14 C15 C16 5.0(2) . . . . ? 
O3 C14 C15 C13 4.9(2) . . . . ? 
C19 C14 C15 C13 -175.14(14) . . . . ? 
N3 C13 C15 C16 169.35(16) . . . . ? 
N3 C13 C15 C14 -10.5(3) . . . . ? 
C14 C15 C16 C17 0.5(2) . . . . ? 
C13 C15 C16 C17 -179.38(15) . . . . ? 
C15 C16 C17 C18 -3.7(3) . . . . ? 
C16 C17 C18 C19 1.2(3) . . . . ? 
C20 O4 C19 C18 122.06(19) . . . . ? 
C20 O4 C19 C14 -63.2(2) . . . . ? 
C17 C18 C19 O4 179.36(16) . . . . ? 
C17 C18 C19 C14 4.6(3) . . . . ? 
O3 C14 C19 O4 -2.2(2) . . . . ? 
C15 C14 C19 O4 177.88(14) . . . . ? 
O3 C14 C19 C18 172.46(15) . . . . ? 
C15 C14 C19 C18 -7.5(2) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.983 
_diffrn_reflns_theta_full              28.31 
_diffrn_measured_fraction_theta_full   0.983 
_refine_diff_density_max    0.395 
_refine_diff_density_min   -0.781 
_refine_diff_density_rms    0.090 
