Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Tong, Ye-Xiang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Zheng, Shao-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Shi, Jian-Xin' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Lee, Hong Kay' ; Department of Chemistry The Chinese University of Hong Kong Hong Kong P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; _publ_contact_author 'Chen, Xiao-Ming' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to J. Chem. Soc., Dalton Trans. Xiao-Ming Chen September 3, 2001 ; #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, crystal structures and properties of six cubane-like transition metal complexes of di-2-pyridyl ketone in gem-diol form ; #============================================================ data_complex_1 _database_code_CSD 170212 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H38 Cl4 Mn4 N8 O9' _chemical_formula_weight 1184.38 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+1/4, x+1/4, z+1/4' '-y+1/4, -x+3/4, z+3/4' 'y+3/4, -x+1/4, -z+3/4' '-y+3/4, x+3/4, -z+1/4' 'x+1/4, z+1/4, y+1/4' '-x+3/4, z+3/4, -y+1/4' '-x+1/4, -z+3/4, y+3/4' 'x+3/4, -z+1/4, -y+3/4' 'z+1/4, y+1/4, x+1/4' 'z+3/4, -y+1/4, -x+3/4' '-z+3/4, y+3/4, -x+1/4' '-z+1/4, -y+3/4, x+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' 'y+3/4, x+3/4, z+3/4' '-y+3/4, -x+5/4, z+5/4' 'y+5/4, -x+3/4, -z+5/4' '-y+5/4, x+5/4, -z+3/4' 'x+3/4, z+3/4, y+3/4' '-x+5/4, z+5/4, -y+3/4' '-x+3/4, -z+5/4, y+5/4' 'x+5/4, -z+3/4, -y+5/4' 'z+3/4, y+3/4, x+3/4' 'z+5/4, -y+3/4, -x+5/4' '-z+5/4, y+5/4, -x+3/4' '-z+3/4, -y+5/4, x+5/4' _cell_length_a 24.287(6) _cell_length_b 24.287(6) _cell_length_c 24.287(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14326(6) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7176 _exptl_absorpt_coefficient_mu 1.321 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.554 _exptl_absorpt_correction_T_max 0.662 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 120 _diffrn_standards_decay_% none _diffrn_reflns_number 3866 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1139 _reflns_number_gt 886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+20.2848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(7) _refine_ls_number_reflns 1139 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 1.00306(4) 0.82017(3) 0.67284(3) 0.04434(19) Uani 1 d . . . Cl1 Cl 0.96390(11) 0.91287(9) 0.66928(10) 0.1077(8) Uani 1 d . . . N1 N 0.96785(19) 0.80630(18) 0.75664(19) 0.0515(12) Uani 1 d . . . N2 N 0.9122(2) 0.6573(2) 0.69982(19) 0.0589(14) Uani 1 d . . . O1 O 0.94180(13) 0.75612(14) 0.66616(12) 0.0422(9) Uani 1 d . . . O2 O 0.85810(15) 0.79212(16) 0.68999(16) 0.0548(11) Uani 1 d . . . H2 H 0.8387 0.7821 0.6602 0.100 Uiso 1 d R . . C1 C 0.9881(3) 0.8275(3) 0.8027(2) 0.0667(19) Uani 1 d . . . H1A H 1.0194 0.8514 0.8002 0.100 Uiso 1 d R . . C2 C 0.9637(3) 0.8181(3) 0.8535(3) 0.077(2) Uani 1 d . . . H2A H 0.9809 0.8318 0.8864 0.100 Uiso 1 d R . . C3 C 0.9171(3) 0.7876(3) 0.8560(3) 0.079(2) Uani 1 d . . . H3A H 0.8991 0.7820 0.8908 0.100 Uiso 1 d R . . C4 C 0.8959(3) 0.7669(3) 0.8091(3) 0.070(2) Uani 1 d . . . H4A H 0.8631 0.7449 0.8103 0.100 Uiso 1 d R . . C5 C 0.9222(2) 0.7767(2) 0.7592(2) 0.0496(15) Uani 1 d . . . C6 C 0.9009(2) 0.7555(3) 0.7042(2) 0.0451(14) Uani 1 d . . . C7 C 0.8775(2) 0.6981(3) 0.7098(2) 0.0515(16) Uani 1 d . . . C8 C 0.8241(3) 0.6887(3) 0.7219(3) 0.077(2) Uani 1 d . . . H8A H 0.7996 0.7189 0.7292 0.100 Uiso 1 d R . . C9 C 0.8051(3) 0.6336(3) 0.7232(3) 0.086(2) Uani 1 d . . . H9A H 0.7675 0.6245 0.7317 0.100 Uiso 1 d R . . C10 C 0.8409(3) 0.5923(3) 0.7130(3) 0.078(2) Uani 1 d . . . H10A H 0.8292 0.5546 0.7142 0.100 Uiso 1 d R . . C11 C 0.8938(3) 0.6048(3) 0.7016(3) 0.070(2) Uani 1 d . . . H11A H 0.9188 0.5752 0.6940 0.100 Uiso 1 d R . . O1W O 1.0037(6) 1.0000 0.7500 0.120(6) Uani 0.50 d SP . . H1W H 0.9849 0.9933 0.7140 0.100 Uiso 0.50 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0512(4) 0.0405(4) 0.0413(4) -0.0004(4) 0.0000(4) 0.0007(4) Cl1 0.1515(19) 0.0741(12) 0.0974(15) 0.0003(12) 0.0025(15) 0.0193(14) N1 0.063(3) 0.050(2) 0.041(2) -0.009(2) 0.001(2) 0.005(2) N2 0.068(3) 0.060(3) 0.049(3) 0.005(2) 0.009(3) -0.012(3) O1 0.0444(17) 0.0458(18) 0.0364(16) 0.0013(18) 0.0067(16) 0.0014(17) O2 0.046(2) 0.061(2) 0.058(2) 0.000(2) 0.0031(18) 0.0117(18) C1 0.081(4) 0.059(3) 0.060(3) -0.012(3) 0.004(3) 0.015(4) C2 0.102(5) 0.084(5) 0.044(3) -0.019(3) 0.000(4) 0.016(4) C3 0.083(5) 0.108(6) 0.045(3) -0.007(4) 0.019(3) 0.023(5) C4 0.075(4) 0.080(5) 0.054(4) 0.006(3) 0.018(3) 0.010(4) C5 0.052(3) 0.049(3) 0.048(3) 0.005(3) 0.005(3) 0.015(3) C6 0.039(3) 0.056(3) 0.041(3) 0.001(3) 0.009(2) 0.003(3) C7 0.043(3) 0.066(4) 0.046(3) -0.006(3) 0.008(3) 0.004(3) C8 0.067(4) 0.093(5) 0.072(4) 0.002(4) 0.029(4) -0.005(4) C9 0.072(4) 0.102(6) 0.085(5) -0.001(4) 0.031(4) -0.033(4) C10 0.093(5) 0.077(4) 0.066(4) 0.000(4) 0.030(4) -0.031(4) C11 0.087(5) 0.052(4) 0.071(4) 0.012(3) 0.013(4) -0.010(4) O1W 0.071(8) 0.187(15) 0.101(9) -0.080(11) 0.000 0.000 _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 Mn1 O1 2.159(4) . ? Mn1 O1 2.182(3) 39_465 ? Mn1 N2 2.228(5) 26_664 ? Mn1 N1 2.233(5) . ? Mn1 O1 2.292(4) 26_664 ? Mn1 Cl1 2.445(2) . ? Cl1 O1W 3.042(5) . ? N1 C5 1.324(7) . ? N1 C1 1.327(8) . ? N2 C7 1.323(8) . ? N2 C11 1.352(8) . ? N2 Mn1 2.228(5) 26_664 ? O1 C6 1.357(6) . ? O1 Mn1 2.182(3) 16_646 ? O1 Mn1 2.292(4) 26_664 ? O2 C6 1.411(7) . ? O2 Cl1 3.303(5) 16_646 ? C1 C2 1.387(9) . ? C2 C3 1.356(11) . ? C3 C4 1.347(10) . ? C4 C5 1.391(8) . ? C5 C6 1.521(8) . ? C6 C7 1.511(8) . ? C7 C8 1.349(9) . ? C8 C9 1.417(11) . ? C9 C10 1.351(10) . ? C10 C11 1.347(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O1 81.55(13) . 39_465 ? O1 Mn1 N2 146.69(16) . 26_664 ? O1 Mn1 N2 107.00(16) 39_465 26_664 ? O1 Mn1 N1 72.30(14) . . ? O1 Mn1 N1 153.60(16) 39_465 . ? N2 Mn1 N1 97.05(17) 26_664 . ? O1 Mn1 O1 79.33(13) . 26_664 ? O1 Mn1 O1 78.60(13) 39_465 26_664 ? N2 Mn1 O1 71.31(16) 26_664 26_664 ? N1 Mn1 O1 99.57(14) . 26_664 ? O1 Mn1 Cl1 113.13(11) . . ? O1 Mn1 Cl1 95.79(11) 39_465 . ? N2 Mn1 Cl1 98.26(15) 26_664 . ? N1 Mn1 Cl1 91.27(13) . . ? O1 Mn1 Cl1 165.69(11) 26_664 . ? Mn1 Cl1 O1W 119.6(2) . . ? C5 N1 C1 118.8(5) . . ? C5 N1 Mn1 116.4(4) . . ? C1 N1 Mn1 124.7(4) . . ? C7 N2 C11 119.3(6) . . ? C7 N2 Mn1 117.3(4) . 26_664 ? C11 N2 Mn1 123.1(5) . 26_664 ? C6 O1 Mn1 117.5(3) . . ? C6 O1 Mn1 125.2(3) . 16_646 ? Mn1 O1 Mn1 101.00(13) . 16_646 ? C6 O1 Mn1 111.7(3) . 26_664 ? Mn1 O1 Mn1 100.05(13) . 26_664 ? Mn1 O1 Mn1 96.91(13) 16_646 26_664 ? C6 O2 Cl1 87.0(3) . 16_646 ? N1 C1 C2 121.9(7) . . ? C3 C2 C1 119.1(6) . . ? C4 C3 C2 119.0(6) . . ? C3 C4 C5 119.9(7) . . ? N1 C5 C4 121.2(6) . . ? N1 C5 C6 115.4(5) . . ? C4 C5 C6 123.5(5) . . ? O1 C6 O2 111.4(4) . . ? O1 C6 C7 110.3(5) . . ? O2 C6 C7 109.1(4) . . ? O1 C6 C5 110.1(4) . . ? O2 C6 C5 104.6(4) . . ? C7 C6 C5 111.1(4) . . ? N2 C7 C8 121.7(6) . . ? N2 C7 C6 115.8(5) . . ? C8 C7 C6 122.5(6) . . ? C7 C8 C9 118.6(7) . . ? C10 C9 C8 119.1(7) . . ? C11 C10 C9 119.0(7) . . ? C10 C11 N2 122.3(7) . . ? _diffrn_measured_fraction_theta_max 0.527 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.536 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.063 #==================================================END data_complex_2 _database_code_CSD 144517 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H49 Cl Mn4 N8 O20' _chemical_formula_weight 1337.18 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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 12.927(8) _cell_length_b 14.245(10) _cell_length_c 15.943(7) _cell_angle_alpha 89.84(1) _cell_angle_beta 72.58(1) _cell_angle_gamma 86.02(1) _cell_volume 2794(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.36 _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 1.014 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 0.846 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% none _diffrn_reflns_number 9845 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9827 _reflns_number_gt 7311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+2.7793P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9827 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.080 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.16878(4) 0.81232(4) 0.26117(4) 0.02952(15) Uani 1 d . . . Mn2 Mn 0.39394(4) 0.66375(4) 0.17262(4) 0.03050(15) Uani 1 d . . . Mn3 Mn 0.26095(4) 0.66547(4) 0.38856(4) 0.03009(15) Uani 1 d . . . Mn4 Mn 0.41044(5) 0.84814(4) 0.29518(4) 0.03491(16) Uani 1 d . . . N1 N 0.1148(2) 0.7314(2) 0.1603(2) 0.0331(7) Uani 1 d . . . N2 N 0.3364(2) 0.5204(2) 0.1695(2) 0.0355(8) Uani 1 d . . . N3 N 0.1123(3) 0.7228(2) 0.4946(2) 0.0380(8) Uani 1 d . . . N4 N 0.3847(3) 0.8700(2) 0.4404(2) 0.0440(9) Uani 1 d . . . N5 N 0.1946(3) 0.9421(2) 0.1830(2) 0.0368(8) Uani 1 d . . . N6 N 0.3576(2) 0.7096(2) 0.0498(2) 0.0345(7) Uani 1 d . . . N7 N 0.3772(3) 0.6457(2) 0.4648(2) 0.0356(8) Uani 1 d . . . N8 N 0.5842(3) 0.7931(2) 0.2672(2) 0.0419(8) Uani 1 d . . . O1W O 0.2139(2) 0.52190(19) 0.41228(19) 0.0473(7) Uani 1 d . . . H1WA H 0.1944 0.4927 0.4614 0.050 Uiso 1 d R . . H1WB H 0.1629 0.5074 0.3886 0.050 Uiso 1 d R . . O2W O 0.1731(3) 0.4431(2) 0.5702(2) 0.0619(9) Uani 1 d . . . H2WA H 0.1432 0.4752 0.6244 0.050 Uiso 1 d R . . H2WB H 0.1431 0.3857 0.5824 0.050 Uiso 1 d R . . O1 O 0.22096(19) 0.66364(16) 0.26605(16) 0.0277(5) Uani 1 d . . . O2 O 0.0750(2) 0.57216(18) 0.31385(17) 0.0367(6) Uani 1 d . . . H2 H 0.0351 0.6246 0.3348 0.050 Uiso 1 d R . . O3 O 0.2420(2) 0.81784(17) 0.36637(15) 0.0299(6) Uani 1 d . . . O4 O 0.1564(2) 0.95730(18) 0.43234(19) 0.0462(7) Uani 1 d . . . H4 H 0.2175 0.9893 0.3958 0.050 Uiso 1 d R . . O5 O 0.3515(2) 0.81317(17) 0.18650(16) 0.0308(6) Uani 1 d . . . O6 O 0.4755(2) 0.8933(2) 0.08086(18) 0.0433(7) Uani 1 d . . . H6 H 0.5233 0.8371 0.0835 0.050 Uiso 1 d R . . O7 O 0.42036(19) 0.68552(17) 0.29825(16) 0.0309(6) Uani 1 d . . . O8 O 0.5355(2) 0.55188(18) 0.28777(18) 0.0417(7) Uani 1 d . . . H8 H 0.5549 0.5570 0.2244 0.050 Uiso 1 d R . . O9 O 0.0067(2) 0.8507(2) 0.3282(2) 0.0485(7) Uani 1 d . . . O10 O -0.0632(2) 0.7161(2) 0.3728(2) 0.0533(8) Uani 1 d . . . O11 O 0.5562(2) 0.6080(2) 0.11519(19) 0.0450(7) Uani 1 d . . . O12 O 0.6165(3) 0.7392(2) 0.0507(2) 0.0605(9) Uani 1 d . . . O13 O 0.4648(4) 0.9850(3) 0.2703(3) 0.0902(13) Uani 1 d . . . O14 O 0.3055(4) 1.0433(5) 0.3199(4) 0.159(3) Uani 1 d . . . C1 C 0.0769(3) 0.7694(3) 0.0980(3) 0.0417(10) Uani 1 d . . . H1A H 0.0750 0.8366 0.0926 0.080 Uiso 1 d R . . C2 C 0.0398(4) 0.7177(3) 0.0420(3) 0.0485(11) Uani 1 d . . . H2A H 0.0167 0.7470 -0.0043 0.080 Uiso 1 d R . . C3 C 0.0371(4) 0.6231(3) 0.0538(3) 0.0511(12) Uani 1 d . . . H3A H 0.0095 0.5850 0.0169 0.080 Uiso 1 d R . . C4 C 0.0730(3) 0.5826(3) 0.1185(3) 0.0407(10) Uani 1 d . . . H4A H 0.0703 0.5162 0.1281 0.080 Uiso 1 d R . . C5 C 0.1141(3) 0.6386(3) 0.1697(2) 0.0317(8) Uani 1 d . . . C6 C 0.1610(3) 0.5990(2) 0.2420(2) 0.0284(8) Uani 1 d . . . C7 C 0.2324(3) 0.5087(2) 0.2082(2) 0.0298(8) Uani 1 d . . . C8 C 0.1908(3) 0.4215(3) 0.2180(3) 0.0385(9) Uani 1 d . . . H8A H 0.1149 0.4151 0.2464 0.080 Uiso 1 d R . . C9 C 0.2613(4) 0.3439(3) 0.1862(3) 0.0456(11) Uani 1 d . . . H9A H 0.2352 0.2821 0.1918 0.080 Uiso 1 d R . . C10 C 0.3687(4) 0.3552(3) 0.1457(3) 0.0472(11) Uani 1 d . . . H10A H 0.4186 0.3017 0.1232 0.080 Uiso 1 d R . . C11 C 0.4033(3) 0.4441(3) 0.1381(3) 0.0449(10) Uani 1 d . . . H11A H 0.4787 0.4525 0.1097 0.080 Uiso 1 d R . . C12 C 0.0307(4) 0.6737(3) 0.5407(3) 0.0512(12) Uani 1 d . . . H12A H 0.0379 0.6062 0.5354 0.080 Uiso 1 d R . . C13 C -0.0641(4) 0.7172(4) 0.5944(3) 0.0613(14) Uani 1 d . . . H13A H -0.1222 0.6804 0.6264 0.080 Uiso 1 d R . . C14 C -0.0746(4) 0.8118(4) 0.6019(3) 0.0639(15) Uani 1 d . . . H14A H -0.1399 0.8427 0.6403 0.080 Uiso 1 d R . . C15 C 0.0083(4) 0.8637(3) 0.5551(3) 0.0521(12) Uani 1 d . . . H15A H 0.0024 0.9312 0.5593 0.080 Uiso 1 d R . . C16 C 0.1009(3) 0.8164(3) 0.5015(2) 0.0375(9) Uani 1 d . . . C17 C 0.1964(3) 0.8667(3) 0.4453(2) 0.0356(9) Uani 1 d . . . C18 C 0.2829(4) 0.8734(3) 0.4923(3) 0.0407(10) Uani 1 d . . . C19 C 0.2580(5) 0.8868(4) 0.5814(3) 0.0626(14) Uani 1 d . . . H19A H 0.1840 0.8881 0.6183 0.080 Uiso 1 d R . . C20 C 0.3418(6) 0.8975(4) 0.6167(4) 0.0834(19) Uani 1 d . . . H20A H 0.3270 0.9080 0.6788 0.080 Uiso 1 d R . . C21 C 0.4465(6) 0.8940(4) 0.5636(4) 0.0777(17) Uani 1 d . . . H21A H 0.5056 0.9018 0.5873 0.080 Uiso 1 d R . . C22 C 0.4650(5) 0.8799(4) 0.4760(4) 0.0623(14) Uani 1 d . . . H22A H 0.5385 0.8761 0.4380 0.080 Uiso 1 d R . . C23 C 0.1215(4) 1.0162(3) 0.1983(3) 0.0483(11) Uani 1 d . . . H23A H 0.0529 1.0109 0.2423 0.080 Uiso 1 d R . . C24 C 0.1412(4) 1.0996(3) 0.1544(3) 0.0566(13) Uani 1 d . . . H24A H 0.0861 1.1507 0.1656 0.080 Uiso 1 d R . . C25 C 0.2412(4) 1.1074(3) 0.0942(3) 0.0568(13) Uani 1 d . . . H25A H 0.2573 1.1644 0.0621 0.080 Uiso 1 d R . . C26 C 0.3185(4) 1.0331(3) 0.0797(3) 0.0459(11) Uani 1 d . . . H26A H 0.3897 1.0381 0.0394 0.080 Uiso 1 d R . . C27 C 0.2923(3) 0.9514(3) 0.1246(2) 0.0343(9) Uani 1 d . . . C28 C 0.3697(3) 0.8636(3) 0.1096(2) 0.0327(9) Uani 1 d . . . C29 C 0.3529(3) 0.8016(3) 0.0368(2) 0.0348(9) Uani 1 d . . . C30 C 0.3364(4) 0.8379(4) -0.0387(3) 0.0576(13) Uani 1 d . . . H30A H 0.3370 0.9044 -0.0484 0.080 Uiso 1 d R . . C31 C 0.3203(5) 0.7775(4) -0.0997(3) 0.0669(15) Uani 1 d . . . H31A H 0.3071 0.8017 -0.1521 0.080 Uiso 1 d R . . C32 C 0.3228(4) 0.6837(4) -0.0862(3) 0.0550(12) Uani 1 d . . . H32A H 0.3107 0.6407 -0.1279 0.080 Uiso 1 d R . . C33 C 0.3428(3) 0.6519(3) -0.0111(3) 0.0437(10) Uani 1 d . . . H33A H 0.3466 0.5854 -0.0015 0.080 Uiso 1 d R . . C34 C 0.3482(4) 0.6389(3) 0.5527(3) 0.0456(11) Uani 1 d . . . H34A H 0.2723 0.6451 0.5848 0.080 Uiso 1 d R . . C35 C 0.4229(4) 0.6227(3) 0.5974(3) 0.0546(12) Uani 1 d . . . H35A H 0.3995 0.6196 0.6604 0.080 Uiso 1 d R . . C36 C 0.5299(4) 0.6124(4) 0.5516(3) 0.0564(13) Uani 1 d . . . H36A H 0.5831 0.5991 0.5819 0.080 Uiso 1 d R . . C37 C 0.5607(4) 0.6200(3) 0.4616(3) 0.0483(11) Uani 1 d . . . H37A H 0.6361 0.6135 0.4279 0.080 Uiso 1 d R . . C38 C 0.4824(3) 0.6375(3) 0.4202(3) 0.0360(9) Uani 1 d . . . C39 C 0.5087(3) 0.6457(3) 0.3200(3) 0.0341(9) Uani 1 d . . . C40 C 0.6063(3) 0.7032(3) 0.2818(3) 0.0368(9) Uani 1 d . . . C41 C 0.7125(3) 0.6640(4) 0.2615(3) 0.0472(11) Uani 1 d . . . H41A H 0.7262 0.5986 0.2722 0.080 Uiso 1 d R . . C42 C 0.7954(4) 0.7199(4) 0.2269(3) 0.0576(13) Uani 1 d . . . H42A H 0.8694 0.6945 0.2136 0.080 Uiso 1 d R . . C43 C 0.7732(4) 0.8116(4) 0.2106(4) 0.0657(15) Uani 1 d . . . H43A H 0.8307 0.8518 0.1852 0.080 Uiso 1 d R . . C44 C 0.6670(4) 0.8460(3) 0.2317(3) 0.0561(12) Uani 1 d . . . H44A H 0.6511 0.9108 0.2201 0.080 Uiso 1 d R . . C45 C 0.6308(3) 0.6573(3) 0.0695(3) 0.0420(10) Uani 1 d . . . C46 C 0.7424(3) 0.6086(3) 0.0374(3) 0.0512(12) Uani 1 d . . . H46A H 0.7924 0.6516 0.0042 0.080 Uiso 1 d R . . H46B H 0.7649 0.5873 0.0868 0.080 Uiso 1 d R . . H46C H 0.7412 0.5556 0.0006 0.080 Uiso 1 d R . . C47 C -0.0698(3) 0.8030(3) 0.3688(3) 0.0427(10) Uani 1 d . . . C48 C -0.1754(4) 0.8557(3) 0.4157(3) 0.0580(13) Uani 1 d . . . H48A H -0.2280 0.8123 0.4441 0.080 Uiso 1 d R . . H48B H -0.1645 0.8976 0.4589 0.080 Uiso 1 d R . . H48C H -0.2012 0.8914 0.3739 0.080 Uiso 1 d R . . C49 C 0.4001(4) 1.0520(4) 0.2830(3) 0.0550(12) Uani 1 d . . . C50 C 0.4282(6) 1.1455(4) 0.2531(5) 0.101(2) Uani 1 d . . . H50A H 0.5051 1.1460 0.2255 0.080 Uiso 1 d R . . H50B H 0.3905 1.1639 0.2114 0.080 Uiso 1 d R . . H50C H 0.4065 1.1889 0.3022 0.080 Uiso 1 d R . . Cl1 Cl 0.11028(11) 0.63582(11) 0.78216(8) 0.0655(4) Uani 1 d . . . O15 O 0.1592(6) 0.5671(5) 0.8260(5) 0.159(3) Uani 1 d . . . O16 O 0.1770(5) 0.7074(4) 0.7623(4) 0.148(3) Uani 1 d . . . O17 O 0.0953(4) 0.5934(4) 0.7081(3) 0.1080(17) Uani 1 d . . . O18 O 0.0094(4) 0.6616(4) 0.8427(3) 0.1179(18) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0299(3) 0.0255(3) 0.0307(3) 0.0010(2) -0.0055(2) -0.0018(2) Mn2 0.0293(3) 0.0283(3) 0.0302(3) 0.0003(2) -0.0033(2) -0.0018(2) Mn3 0.0295(3) 0.0280(3) 0.0292(3) 0.0021(2) -0.0037(2) -0.0002(2) Mn4 0.0332(3) 0.0340(3) 0.0371(3) -0.0006(3) -0.0093(3) -0.0049(3) N1 0.0299(17) 0.0342(18) 0.0332(18) 0.0016(14) -0.0063(14) -0.0032(13) N2 0.0312(17) 0.0274(17) 0.0424(19) -0.0027(14) -0.0032(15) 0.0010(13) N3 0.0372(18) 0.039(2) 0.0308(18) 0.0040(15) -0.0012(15) 0.0044(15) N4 0.053(2) 0.039(2) 0.046(2) -0.0035(16) -0.0220(18) -0.0068(17) N5 0.0375(18) 0.0291(17) 0.0390(19) 0.0017(14) -0.0050(15) 0.0012(14) N6 0.0326(17) 0.0372(19) 0.0318(18) -0.0014(14) -0.0067(14) -0.0031(14) N7 0.0356(18) 0.0363(18) 0.0333(18) 0.0065(14) -0.0085(15) -0.0003(14) N8 0.0328(18) 0.046(2) 0.046(2) 0.0029(16) -0.0080(16) -0.0093(15) O1W 0.0568(19) 0.0388(16) 0.0452(17) 0.0107(13) -0.0112(14) -0.0152(14) O2W 0.058(2) 0.064(2) 0.055(2) 0.0170(17) -0.0031(16) -0.0116(17) O1 0.0265(13) 0.0250(13) 0.0297(13) -0.0022(10) -0.0057(10) -0.0020(10) O2 0.0317(14) 0.0316(14) 0.0375(15) -0.0024(12) 0.0043(12) -0.0047(11) O3 0.0335(14) 0.0287(13) 0.0253(13) -0.0028(10) -0.0060(11) -0.0003(11) O4 0.0572(19) 0.0289(15) 0.0459(17) -0.0016(13) -0.0086(14) 0.0099(13) O5 0.0361(14) 0.0270(13) 0.0269(13) 0.0032(10) -0.0057(11) -0.0025(11) O6 0.0330(15) 0.0431(17) 0.0477(17) 0.0134(13) -0.0017(13) -0.0082(12) O7 0.0262(13) 0.0350(14) 0.0301(14) 0.0059(11) -0.0068(11) -0.0003(11) O8 0.0449(16) 0.0355(15) 0.0407(16) 0.0002(13) -0.0090(13) 0.0072(13) O9 0.0349(16) 0.0497(18) 0.0511(18) -0.0038(15) 0.0017(14) -0.0027(14) O10 0.0462(18) 0.0421(19) 0.060(2) 0.0002(15) -0.0003(15) 0.0046(14) O11 0.0328(15) 0.0529(18) 0.0421(17) 0.0050(14) -0.0009(13) -0.0013(13) O12 0.0512(19) 0.050(2) 0.070(2) 0.0068(17) -0.0041(17) 0.0041(16) O13 0.126(4) 0.057(2) 0.078(3) 0.001(2) -0.022(3) 0.023(2) O14 0.084(4) 0.202(7) 0.181(6) 0.125(5) -0.018(4) -0.038(4) C1 0.040(2) 0.043(2) 0.043(2) 0.0055(19) -0.0148(19) -0.0016(19) C2 0.046(3) 0.060(3) 0.043(3) 0.002(2) -0.021(2) 0.002(2) C3 0.048(3) 0.054(3) 0.058(3) -0.016(2) -0.027(2) 0.000(2) C4 0.036(2) 0.039(2) 0.048(3) -0.0098(19) -0.0146(19) -0.0036(18) C5 0.0227(18) 0.033(2) 0.035(2) -0.0018(16) -0.0017(15) -0.0008(15) C6 0.0272(18) 0.0239(18) 0.031(2) -0.0019(15) -0.0035(15) -0.0032(15) C7 0.031(2) 0.0255(19) 0.030(2) -0.0016(15) -0.0056(16) -0.0021(15) C8 0.042(2) 0.032(2) 0.041(2) -0.0014(18) -0.0112(19) -0.0038(18) C9 0.058(3) 0.027(2) 0.048(3) -0.0034(18) -0.011(2) -0.0045(19) C10 0.056(3) 0.027(2) 0.052(3) -0.0067(19) -0.009(2) 0.0093(19) C11 0.040(2) 0.036(2) 0.050(3) -0.0047(19) -0.001(2) 0.0052(19) C12 0.048(3) 0.052(3) 0.043(3) 0.010(2) 0.002(2) 0.002(2) C13 0.049(3) 0.071(4) 0.048(3) 0.019(3) 0.006(2) 0.003(3) C14 0.052(3) 0.074(4) 0.044(3) 0.009(3) 0.013(2) 0.019(3) C15 0.056(3) 0.051(3) 0.038(2) -0.001(2) -0.001(2) 0.016(2) C16 0.044(2) 0.037(2) 0.027(2) 0.0014(17) -0.0066(17) 0.0088(18) C17 0.045(2) 0.029(2) 0.029(2) -0.0013(16) -0.0069(17) 0.0061(17) C18 0.059(3) 0.031(2) 0.033(2) -0.0034(17) -0.015(2) 0.0006(19) C19 0.081(4) 0.069(3) 0.040(3) -0.008(2) -0.023(3) -0.002(3) C20 0.126(6) 0.086(4) 0.052(3) -0.017(3) -0.049(4) -0.001(4) C21 0.099(5) 0.082(4) 0.070(4) -0.007(3) -0.050(4) -0.018(4) C22 0.069(3) 0.063(3) 0.067(3) -0.002(3) -0.036(3) -0.016(3) C23 0.049(3) 0.035(2) 0.053(3) 0.002(2) -0.003(2) 0.001(2) C24 0.059(3) 0.034(2) 0.069(3) 0.005(2) -0.008(3) 0.007(2) C25 0.074(3) 0.030(2) 0.060(3) 0.013(2) -0.010(3) -0.005(2) C26 0.055(3) 0.036(2) 0.041(2) 0.0093(19) -0.005(2) -0.006(2) C27 0.041(2) 0.031(2) 0.029(2) 0.0034(16) -0.0088(17) -0.0045(17) C28 0.034(2) 0.031(2) 0.029(2) 0.0066(16) -0.0034(16) -0.0043(16) C29 0.032(2) 0.040(2) 0.028(2) 0.0038(17) -0.0031(16) -0.0005(17) C30 0.081(4) 0.055(3) 0.035(3) 0.003(2) -0.017(2) 0.005(3) C31 0.081(4) 0.087(4) 0.035(3) -0.001(3) -0.024(3) 0.014(3) C32 0.051(3) 0.073(4) 0.040(3) -0.014(2) -0.012(2) -0.001(2) C33 0.036(2) 0.052(3) 0.039(2) -0.011(2) -0.0060(19) -0.0035(19) C34 0.053(3) 0.048(3) 0.033(2) 0.0074(19) -0.009(2) 0.003(2) C35 0.069(3) 0.058(3) 0.035(2) 0.006(2) -0.016(2) 0.006(2) C36 0.058(3) 0.068(3) 0.050(3) 0.007(2) -0.028(2) 0.006(2) C37 0.048(3) 0.056(3) 0.041(3) 0.002(2) -0.016(2) 0.005(2) C38 0.039(2) 0.033(2) 0.037(2) 0.0035(17) -0.0135(18) 0.0021(17) C39 0.034(2) 0.032(2) 0.036(2) 0.0017(17) -0.0106(17) 0.0008(16) C40 0.034(2) 0.044(2) 0.033(2) 0.0010(18) -0.0106(17) -0.0015(18) C41 0.033(2) 0.066(3) 0.041(2) 0.001(2) -0.0098(19) 0.002(2) C42 0.030(2) 0.083(4) 0.057(3) -0.003(3) -0.011(2) 0.000(2) C43 0.038(3) 0.077(4) 0.077(4) 0.003(3) -0.006(3) -0.021(3) C44 0.044(3) 0.051(3) 0.071(3) 0.003(2) -0.010(2) -0.014(2) C45 0.040(2) 0.050(3) 0.033(2) -0.004(2) -0.0079(19) 0.000(2) C46 0.034(2) 0.063(3) 0.048(3) -0.005(2) -0.001(2) 0.005(2) C47 0.035(2) 0.047(3) 0.041(2) -0.005(2) -0.0041(19) 0.0007(19) C48 0.042(3) 0.056(3) 0.065(3) -0.005(2) -0.001(2) 0.005(2) C49 0.062(3) 0.051(3) 0.057(3) 0.011(2) -0.023(3) -0.013(3) C50 0.134(6) 0.053(4) 0.137(6) 0.033(4) -0.068(5) -0.028(4) Cl1 0.0600(8) 0.0883(10) 0.0507(7) -0.0071(7) -0.0165(6) -0.0222(7) O15 0.197(7) 0.139(5) 0.188(7) -0.001(5) -0.137(6) 0.015(5) O16 0.170(6) 0.166(6) 0.114(4) 0.010(4) -0.027(4) -0.115(5) O17 0.108(4) 0.159(5) 0.064(3) -0.035(3) -0.032(3) -0.026(3) O18 0.079(3) 0.163(5) 0.096(4) -0.052(3) 0.000(3) -0.013(3) _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 Mn1 O9 2.082(3) . ? Mn1 O3 2.162(3) . ? Mn1 O1 2.186(3) . ? Mn1 N5 2.215(3) . ? Mn1 N1 2.279(3) . ? Mn1 O5 2.306(3) . ? Mn2 O11 2.119(3) . ? Mn2 O5 2.156(3) . ? Mn2 O7 2.157(3) . ? Mn2 N2 2.227(3) . ? Mn2 N6 2.232(3) . ? Mn2 O1 2.286(3) . ? Mn3 O1 2.165(3) . ? Mn3 O7 2.169(3) . ? Mn3 O1W 2.174(3) . ? Mn3 N7 2.202(3) . ? Mn3 O3 2.207(3) . ? Mn3 N3 2.250(3) . ? Mn4 O13 2.114(5) . ? Mn4 O5 2.163(3) . ? Mn4 O3 2.206(3) . ? Mn4 N8 2.240(4) . ? Mn4 N4 2.257(4) . ? Mn4 O7 2.312(3) . ? N1 C5 1.329(5) . ? N1 C1 1.331(5) . ? N2 C7 1.324(5) . ? N2 C11 1.339(5) . ? N3 C16 1.333(5) . ? N3 C12 1.334(5) . ? N4 C18 1.326(5) . ? N4 C22 1.340(6) . ? N5 C23 1.339(5) . ? N5 C27 1.341(5) . ? N6 C29 1.326(5) . ? N6 C33 1.339(5) . ? N7 C38 1.329(5) . ? N7 C34 1.343(5) . ? N8 C40 1.329(5) . ? N8 C44 1.333(5) . ? O1W O2W 2.674(4) . ? O1W O2 2.776(4) . ? O2W O10 2.765(5) 2_566 ? O2W O17 2.972(6) . ? O1 C6 1.369(4) . ? O2 C6 1.411(4) . ? O2 O10 2.602(4) . ? O3 C17 1.385(4) . ? O4 C17 1.395(5) . ? O4 O14 2.583(6) . ? O5 C28 1.386(4) . ? O6 C28 1.402(4) . ? O6 O12 2.702(4) . ? O7 C39 1.376(4) . ? O8 C39 1.415(5) . ? O8 O11 2.803(4) . ? O9 C47 1.251(5) . ? O10 C47 1.239(5) . ? O11 C45 1.274(5) . ? O12 C45 1.219(5) . ? O13 C49 1.201(6) . ? O14 C49 1.203(7) . ? C1 C2 1.371(6) . ? C2 C3 1.362(6) . ? C3 C4 1.363(6) . ? C4 C5 1.382(5) . ? C5 C6 1.543(5) . ? C6 C7 1.529(5) . ? C7 C8 1.378(5) . ? C8 C9 1.376(6) . ? C9 C10 1.366(6) . ? C10 C11 1.364(6) . ? C12 C13 1.374(6) . ? C13 C14 1.346(7) . ? C14 C15 1.372(7) . ? C15 C16 1.376(6) . ? C16 C17 1.515(6) . ? C17 C18 1.529(6) . ? C18 C19 1.371(6) . ? C19 C20 1.379(8) . ? C20 C21 1.362(9) . ? C21 C22 1.357(7) . ? C23 C24 1.376(6) . ? C24 C25 1.372(7) . ? C25 C26 1.373(6) . ? C26 C27 1.374(5) . ? C27 C28 1.518(5) . ? C28 C29 1.535(5) . ? C29 C30 1.377(6) . ? C30 C31 1.372(7) . ? C31 C32 1.353(7) . ? C32 C33 1.368(6) . ? C34 C35 1.369(6) . ? C35 C36 1.355(7) . ? C36 C37 1.375(6) . ? C37 C38 1.374(6) . ? C38 C39 1.537(5) . ? C39 C40 1.521(5) . ? C40 C41 1.388(6) . ? C41 C42 1.361(6) . ? C42 C43 1.358(7) . ? C43 C44 1.368(7) . ? C45 C46 1.498(6) . ? C47 C48 1.495(6) . ? C49 C50 1.447(7) . ? Cl1 O16 1.357(5) . ? Cl1 O18 1.396(5) . ? Cl1 O17 1.398(4) . ? Cl1 O15 1.422(6) . ? 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 O9 Mn1 O3 101.14(12) . . ? O9 Mn1 O1 115.98(11) . . ? O3 Mn1 O1 80.04(9) . . ? O9 Mn1 N5 94.78(12) . . ? O3 Mn1 N5 110.57(11) . . ? O1 Mn1 N5 145.41(11) . . ? O9 Mn1 N1 89.59(12) . . ? O3 Mn1 N1 151.67(11) . . ? O1 Mn1 N1 71.70(11) . . ? N5 Mn1 N1 94.35(13) . . ? O9 Mn1 O5 164.51(11) . . ? O3 Mn1 O5 77.24(10) . . ? O1 Mn1 O5 79.14(9) . . ? N5 Mn1 O5 71.85(10) . . ? N1 Mn1 O5 99.00(10) . . ? O11 Mn2 O5 121.99(11) . . ? O11 Mn2 O7 92.24(11) . . ? O5 Mn2 O7 81.83(9) . . ? O11 Mn2 N2 89.63(12) . . ? O5 Mn2 N2 146.96(11) . . ? O7 Mn2 N2 108.38(11) . . ? O11 Mn2 N6 98.37(11) . . ? O5 Mn2 N6 73.10(11) . . ? O7 Mn2 N6 154.75(11) . . ? N2 Mn2 N6 94.61(12) . . ? O11 Mn2 O1 154.83(10) . . ? O5 Mn2 O1 80.21(9) . . ? O7 Mn2 O1 78.49(9) . . ? N2 Mn2 O1 71.67(10) . . ? N6 Mn2 O1 99.76(11) . . ? O1 Mn3 O7 80.91(10) . . ? O1 Mn3 O1W 89.86(10) . . ? O7 Mn3 O1W 117.57(10) . . ? O1 Mn3 N7 151.77(11) . . ? O7 Mn3 N7 73.44(11) . . ? O1W Mn3 N7 91.65(12) . . ? O1 Mn3 O3 79.51(9) . . ? O7 Mn3 O3 80.29(9) . . ? O1W Mn3 O3 157.72(11) . . ? N7 Mn3 O3 107.00(11) . . ? O1 Mn3 N3 107.90(11) . . ? O7 Mn3 N3 149.69(12) . . ? O1W Mn3 N3 91.85(12) . . ? N7 Mn3 N3 100.22(13) . . ? O3 Mn3 N3 73.24(11) . . ? O13 Mn4 O5 105.62(14) . . ? O13 Mn4 O3 124.39(14) . . ? O5 Mn4 O3 79.41(10) . . ? O13 Mn4 N8 88.39(16) . . ? O5 Mn4 N8 109.81(11) . . ? O3 Mn4 N8 143.24(12) . . ? O13 Mn4 N4 90.43(15) . . ? O5 Mn4 N4 151.17(12) . . ? O3 Mn4 N4 71.77(11) . . ? N8 Mn4 N4 94.13(13) . . ? O13 Mn4 O7 158.30(14) . . ? O5 Mn4 O7 78.20(9) . . ? O3 Mn4 O7 77.24(9) . . ? N8 Mn4 O7 70.47(11) . . ? N4 Mn4 O7 95.76(11) . . ? C5 N1 C1 118.0(3) . . ? C5 N1 Mn1 116.1(3) . . ? C1 N1 Mn1 125.7(3) . . ? C7 N2 C11 118.3(3) . . ? C7 N2 Mn2 118.1(2) . . ? C11 N2 Mn2 123.3(3) . . ? C16 N3 C12 118.6(4) . . ? C16 N3 Mn3 114.4(3) . . ? C12 N3 Mn3 126.2(3) . . ? C18 N4 C22 119.2(4) . . ? C18 N4 Mn4 116.7(3) . . ? C22 N4 Mn4 124.1(3) . . ? C23 N5 C27 118.1(3) . . ? C23 N5 Mn1 122.9(3) . . ? C27 N5 Mn1 118.6(2) . . ? C29 N6 C33 118.6(4) . . ? C29 N6 Mn2 116.1(3) . . ? C33 N6 Mn2 125.3(3) . . ? C38 N7 C34 118.5(3) . . ? C38 N7 Mn3 117.4(3) . . ? C34 N7 Mn3 124.1(3) . . ? C40 N8 C44 118.4(4) . . ? C40 N8 Mn4 119.0(3) . . ? C44 N8 Mn4 122.4(3) . . ? Mn3 O1W O2W 122.91(15) . . ? Mn3 O1W O2 83.83(11) . . ? O2W O1W O2 130.18(14) . . ? O1W O2W O10 127.92(17) . 2_566 ? O1W O2W O17 108.84(17) . . ? O10 O2W O17 109.16(16) 2_566 . ? C6 O1 Mn3 125.6(2) . . ? C6 O1 Mn1 117.3(2) . . ? Mn3 O1 Mn1 99.31(10) . . ? C6 O1 Mn2 112.8(2) . . ? Mn3 O1 Mn2 97.81(10) . . ? Mn1 O1 Mn2 99.45(10) . . ? C6 O2 O10 109.9(2) . . ? C6 O2 O1W 92.5(2) . . ? O10 O2 O1W 116.13(14) . . ? C17 O3 Mn1 124.9(2) . . ? C17 O3 Mn4 115.3(2) . . ? Mn1 O3 Mn4 102.16(10) . . ? C17 O3 Mn3 110.8(2) . . ? Mn1 O3 Mn3 98.77(10) . . ? Mn4 O3 Mn3 101.49(10) . . ? C17 O4 O14 110.0(3) . . ? C28 O5 Mn2 116.8(2) . . ? C28 O5 Mn4 124.5(2) . . ? Mn2 O5 Mn4 101.08(10) . . ? C28 O5 Mn1 111.8(2) . . ? Mn2 O5 Mn1 99.72(10) . . ? Mn4 O5 Mn1 98.97(10) . . ? C28 O6 O12 108.2(2) . . ? C39 O7 Mn2 123.5(2) . . ? C39 O7 Mn3 117.1(2) . . ? Mn2 O7 Mn3 101.73(11) . . ? C39 O7 Mn4 114.5(2) . . ? Mn2 O7 Mn4 96.44(9) . . ? Mn3 O7 Mn4 99.32(10) . . ? C39 O8 O11 91.7(2) . . ? C47 O9 Mn1 131.6(3) . . ? C47 O10 O2 140.3(3) . . ? C45 O11 Mn2 122.7(3) . . ? C45 O11 O8 124.6(3) . . ? Mn2 O11 O8 82.75(10) . . ? C45 O12 O6 145.5(3) . . ? C49 O13 Mn4 120.0(4) . . ? C49 O14 O4 149.9(5) . . ? N1 C1 C2 123.4(4) . . ? C3 C2 C1 117.9(4) . . ? C2 C3 C4 119.9(4) . . ? C3 C4 C5 118.9(4) . . ? N1 C5 C4 121.8(4) . . ? N1 C5 C6 115.3(3) . . ? C4 C5 C6 122.9(3) . . ? O1 C6 O2 112.1(3) . . ? O1 C6 C7 109.8(3) . . ? O2 C6 C7 105.7(3) . . ? O1 C6 C5 110.5(3) . . ? O2 C6 C5 109.0(3) . . ? C7 C6 C5 109.6(3) . . ? N2 C7 C8 122.6(3) . . ? N2 C7 C6 115.3(3) . . ? C8 C7 C6 122.1(3) . . ? C9 C8 C7 118.1(4) . . ? C10 C9 C8 119.8(4) . . ? C11 C10 C9 118.6(4) . . ? N2 C11 C10 122.7(4) . . ? N3 C12 C13 121.6(5) . . ? C14 C13 C12 119.4(5) . . ? C13 C14 C15 119.9(4) . . ? C14 C15 C16 118.2(4) . . ? N3 C16 C15 122.2(4) . . ? N3 C16 C17 115.1(3) . . ? C15 C16 C17 122.7(4) . . ? O3 C17 O4 111.6(3) . . ? O3 C17 C16 109.6(3) . . ? O4 C17 C16 106.9(3) . . ? O3 C17 C18 109.0(3) . . ? O4 C17 C18 109.0(3) . . ? C16 C17 C18 110.8(3) . . ? N4 C18 C19 121.5(4) . . ? N4 C18 C17 115.4(3) . . ? C19 C18 C17 122.9(4) . . ? C18 C19 C20 118.4(5) . . ? C21 C20 C19 120.2(5) . . ? C22 C21 C20 118.1(5) . . ? N4 C22 C21 122.6(6) . . ? N5 C23 C24 122.8(4) . . ? C25 C24 C23 118.3(4) . . ? C24 C25 C26 119.7(4) . . ? C25 C26 C27 118.8(4) . . ? N5 C27 C26 122.3(4) . . ? N5 C27 C28 114.8(3) . . ? C26 C27 C28 122.8(4) . . ? O5 C28 O6 111.9(3) . . ? O5 C28 C27 110.0(3) . . ? O6 C28 C27 107.1(3) . . ? O5 C28 C29 109.5(3) . . ? O6 C28 C29 108.3(3) . . ? C27 C28 C29 110.0(3) . . ? N6 C29 C30 121.4(4) . . ? N6 C29 C28 115.9(3) . . ? C30 C29 C28 122.7(4) . . ? C31 C30 C29 118.9(5) . . ? C32 C31 C30 120.1(5) . . ? C31 C32 C33 118.1(4) . . ? N6 C33 C32 122.9(4) . . ? N7 C34 C35 122.3(4) . . ? C36 C35 C34 119.0(4) . . ? C35 C36 C37 119.2(4) . . ? C38 C37 C36 119.3(4) . . ? N7 C38 C37 121.6(4) . . ? N7 C38 C39 115.2(3) . . ? C37 C38 C39 123.1(4) . . ? O7 C39 O8 111.6(3) . . ? O7 C39 C40 109.7(3) . . ? O8 C39 C40 108.9(3) . . ? O7 C39 C38 110.6(3) . . ? O8 C39 C38 104.5(3) . . ? C40 C39 C38 111.5(3) . . ? N8 C40 C41 121.6(4) . . ? N8 C40 C39 116.1(3) . . ? C41 C40 C39 122.3(4) . . ? C42 C41 C40 118.8(5) . . ? C43 C42 C41 119.8(4) . . ? C42 C43 C44 118.7(5) . . ? N8 C44 C43 122.7(5) . . ? O12 C45 O11 124.5(4) . . ? O12 C45 C46 119.5(4) . . ? O11 C45 C46 116.0(4) . . ? O10 C47 O9 124.3(4) . . ? O10 C47 C48 118.6(4) . . ? O9 C47 C48 117.1(4) . . ? O13 C49 O14 120.3(6) . . ? O13 C49 C50 123.5(6) . . ? O14 C49 C50 116.1(6) . . ? O16 Cl1 O18 113.3(4) . . ? O16 Cl1 O17 113.3(3) . . ? O18 Cl1 O17 109.7(3) . . ? O16 Cl1 O15 107.1(4) . . ? O18 Cl1 O15 104.5(4) . . ? O17 Cl1 O15 108.5(4) . . ? Cl1 O17 O2W 146.5(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.919 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.070 #============================================END data_complex_3 _database_code_CSD 144518 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H50.50 Cl Co4 N8 O20.80' _chemical_formula_weight 1367.45 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.893(11) _cell_length_b 14.228(11) _cell_length_c 16.048(8) _cell_angle_alpha 89.430(1) _cell_angle_beta 72.39(1) _cell_angle_gamma 86.610(1) _cell_volume 2801(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.837 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 11017 _diffrn_reflns_av_R_equivalents 0.0119 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11000 _reflns_number_gt 8313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+3.2462P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11000 _refine_ls_number_parameters 766 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.17685(4) 0.80675(3) 0.26043(3) 0.02847(11) Uani 1 d . . . Co2 Co 0.39005(4) 0.66562(3) 0.17813(3) 0.02829(11) Uani 1 d . . . Co3 Co 0.40701(4) 0.84068(3) 0.29897(3) 0.03197(12) Uani 1 d . . . Co4 Co 0.26351(4) 0.66938(3) 0.38879(3) 0.02842(11) Uani 1 d . . . O1 O 0.0198(2) 0.84077(18) 0.33055(17) 0.0430(6) Uani 1 d . . . O2 O -0.0664(2) 0.70975(18) 0.37450(19) 0.0495(7) Uani 1 d . . . C1 C -0.0636(3) 0.7977(3) 0.3697(2) 0.0362(8) Uani 1 d . . . C2 C -0.1661(3) 0.8569(3) 0.4142(3) 0.0550(11) Uani 1 d . . . H2A H -0.2239 0.8166 0.4411 0.080 Uiso 1 d R . . H2B H -0.1531 0.8958 0.4581 0.080 Uiso 1 d R . . H2C H -0.1864 0.8960 0.3719 0.080 Uiso 1 d R . . O3 O 0.55112(19) 0.62078(18) 0.12235(16) 0.0394(6) Uani 1 d . . . O4 O 0.6233(2) 0.7425(2) 0.0422(2) 0.0575(8) Uani 1 d . . . C3 C 0.6305(3) 0.6631(3) 0.0706(2) 0.0371(8) Uani 1 d . . . C4 C 0.7397(3) 0.6079(3) 0.0432(3) 0.0482(10) Uani 1 d . . . H4A H 0.7931 0.6458 0.0052 0.080 Uiso 1 d R . . H4B H 0.7614 0.5914 0.0939 0.080 Uiso 1 d R . . H4C H 0.7338 0.5516 0.0129 0.080 Uiso 1 d R . . O5 O 0.4318(3) 0.9760(2) 0.2700(2) 0.0656(9) Uani 1 d . . . O6 O 0.3033(3) 1.0716(3) 0.3461(3) 0.1208(19) Uani 1 d . . . C5 C 0.3924(4) 1.0565(3) 0.2870(3) 0.0519(11) Uani 1 d . . . C6 C 0.4436(5) 1.1371(4) 0.2423(4) 0.0860(18) Uani 1 d . . . H6A H 0.5101 1.1162 0.1989 0.080 Uiso 1 d R . . H6B H 0.3964 1.1705 0.2145 0.080 Uiso 1 d R . . H6C H 0.4598 1.1782 0.2833 0.080 Uiso 1 d R . . O1W O 0.2261(2) 0.52708(17) 0.40862(17) 0.0426(6) Uani 1 d . . . H1WA H 0.2093 0.4993 0.4569 0.050 Uiso 1 d R . . H1WB H 0.1502 0.5338 0.3869 0.050 Uiso 1 d R . . O11 O 0.22136(17) 0.66755(15) 0.27010(14) 0.0270(5) Uani 1 d . . . O12 O 0.07664(18) 0.57168(16) 0.31810(15) 0.0351(6) Uani 1 d . . . H12 H 0.0266 0.6266 0.3429 0.050 Uiso 1 d R . . N11 N 0.1165(2) 0.7366(2) 0.16532(18) 0.0328(6) Uani 1 d . . . N12 N 0.3403(2) 0.52741(19) 0.17529(18) 0.0314(6) Uani 1 d . . . C10 C 0.0781(3) 0.7767(3) 0.1034(3) 0.0419(9) Uani 1 d . . . H10A H 0.0802 0.8437 0.0965 0.080 Uiso 1 d R . . C11 C 0.0366(3) 0.7257(3) 0.0491(3) 0.0475(10) Uani 1 d . . . H11A H 0.0110 0.7562 0.0049 0.080 Uiso 1 d R . . C12 C 0.0312(3) 0.6299(3) 0.0610(3) 0.0491(10) Uani 1 d . . . H12A H 0.0023 0.5923 0.0248 0.080 Uiso 1 d R . . C13 C 0.0682(3) 0.5882(3) 0.1254(3) 0.0422(9) Uani 1 d . . . H13A H 0.0640 0.5217 0.1353 0.080 Uiso 1 d R . . C14 C 0.1126(3) 0.6426(2) 0.1752(2) 0.0318(8) Uani 1 d . . . C15 C 0.1605(3) 0.6007(2) 0.2457(2) 0.0297(7) Uani 1 d . . . C16 C 0.2348(3) 0.5130(2) 0.2107(2) 0.0298(7) Uani 1 d . . . C17 C 0.1943(3) 0.4239(2) 0.2161(2) 0.0371(8) Uani 1 d . . . H17A H 0.1179 0.4156 0.2418 0.080 Uiso 1 d R . . C18 C 0.2666(3) 0.3479(3) 0.1836(3) 0.0470(10) Uani 1 d . . . H18A H 0.2416 0.2854 0.1869 0.080 Uiso 1 d R . . C19 C 0.3752(3) 0.3621(3) 0.1461(3) 0.0454(10) Uani 1 d . . . H19A H 0.4265 0.3102 0.1225 0.080 Uiso 1 d R . . C20 C 0.4092(3) 0.4520(3) 0.1434(3) 0.0420(9) Uani 1 d . . . H20A H 0.4851 0.4620 0.1173 0.080 Uiso 1 d R . . O21 O 0.24751(18) 0.81812(15) 0.36339(14) 0.0293(5) Uani 1 d . . . O22 O 0.1595(2) 0.95775(17) 0.42901(17) 0.0439(6) Uani 1 d . . . H22 H 0.2169 0.9938 0.3980 0.050 Uiso 1 d R . . N21 N 0.3930(3) 0.8671(2) 0.4352(2) 0.0396(7) Uani 1 d . . . N22 N 0.1211(2) 0.7202(2) 0.48959(19) 0.0359(7) Uani 1 d . . . C21 C 0.4749(4) 0.8760(3) 0.4698(3) 0.0529(11) Uani 1 d . . . H21A H 0.5484 0.8698 0.4317 0.080 Uiso 1 d R . . C22 C 0.4571(4) 0.8932(4) 0.5572(3) 0.0659(13) Uani 1 d . . . H22A H 0.5163 0.8998 0.5809 0.080 Uiso 1 d R . . C23 C 0.3517(5) 0.9010(4) 0.6107(3) 0.0702(14) Uani 1 d . . . H23A H 0.3369 0.9128 0.6721 0.080 Uiso 1 d R . . C24 C 0.2665(4) 0.8924(3) 0.5762(3) 0.0541(11) Uani 1 d . . . H24A H 0.1921 0.8981 0.6127 0.080 Uiso 1 d R . . C25 C 0.2905(3) 0.8752(2) 0.4877(2) 0.0373(8) Uani 1 d . . . C26 C 0.2015(3) 0.8677(2) 0.4421(2) 0.0343(8) Uani 1 d . . . C27 C 0.1067(3) 0.8143(3) 0.4979(2) 0.0356(8) Uani 1 d . . . C28 C 0.0127(3) 0.8581(3) 0.5532(3) 0.0497(10) Uani 1 d . . . H28A H 0.0055 0.9254 0.5586 0.080 Uiso 1 d R . . C29 C -0.0705(4) 0.8033(3) 0.5999(3) 0.0588(13) Uani 1 d . . . H29A H -0.1361 0.8323 0.6389 0.080 Uiso 1 d R . . C30 C -0.0560(3) 0.7074(3) 0.5908(3) 0.0574(12) Uani 1 d . . . H30A H -0.1126 0.6682 0.6227 0.080 Uiso 1 d R . . C31 C 0.0388(3) 0.6679(3) 0.5357(3) 0.0465(10) Uani 1 d . . . H31A H 0.0471 0.6007 0.5285 0.080 Uiso 1 d R . . O31 O 0.35661(18) 0.80698(15) 0.18946(14) 0.0291(5) Uani 1 d . . . O32 O 0.47925(19) 0.89001(17) 0.08190(16) 0.0402(6) Uani 1 d . . . H32 H 0.5232 0.8361 0.0723 0.050 Uiso 1 d R . . N31 N 0.1986(2) 0.9341(2) 0.19135(19) 0.0338(7) Uani 1 d . . . N32 N 0.3599(2) 0.7017(2) 0.05711(18) 0.0327(7) Uani 1 d . . . C32 C 0.1239(3) 1.0078(3) 0.2100(3) 0.0453(10) Uani 1 d . . . H32A H 0.0567 1.0014 0.2556 0.080 Uiso 1 d R . . C33 C 0.1409(4) 1.0916(3) 0.1656(3) 0.0546(11) Uani 1 d . . . H33A H 0.0858 1.1424 0.1792 0.080 Uiso 1 d R . . C34 C 0.2387(4) 1.1016(3) 0.1010(3) 0.0507(11) Uani 1 d . . . H34A H 0.2520 1.1592 0.0690 0.080 Uiso 1 d R . . C35 C 0.3170(3) 1.0279(3) 0.0831(3) 0.0440(9) Uani 1 d . . . H35A H 0.3864 1.0340 0.0397 0.080 Uiso 1 d R . . C36 C 0.2941(3) 0.9446(2) 0.1294(2) 0.0322(8) Uani 1 d . . . C37 C 0.3736(3) 0.8587(2) 0.1126(2) 0.0305(7) Uani 1 d . . . C38 C 0.3556(3) 0.7946(2) 0.0418(2) 0.0339(8) Uani 1 d . . . C39 C 0.3386(3) 0.8296(3) -0.0346(3) 0.0486(10) Uani 1 d . . . H39A H 0.3388 0.8960 -0.0455 0.080 Uiso 1 d R . . C40 C 0.3218(4) 0.7672(3) -0.0943(3) 0.0556(11) Uani 1 d . . . H40A H 0.3090 0.7901 -0.1471 0.080 Uiso 1 d R . . C41 C 0.3238(3) 0.6725(3) -0.0775(3) 0.0488(10) Uani 1 d . . . H41A H 0.3109 0.6280 -0.1173 0.080 Uiso 1 d R . . C42 C 0.3439(3) 0.6427(3) -0.0018(2) 0.0388(9) Uani 1 d . . . H42A H 0.3474 0.5764 0.0094 0.080 Uiso 1 d R . . O41 O 0.41415(17) 0.68325(15) 0.30101(14) 0.0287(5) Uani 1 d . . . O42 O 0.5354(2) 0.55290(17) 0.29102(17) 0.0400(6) Uani 1 d . . . H42 H 0.5501 0.5583 0.2277 0.050 Uiso 1 d R . . N41 N 0.3692(2) 0.6512(2) 0.46788(18) 0.0337(7) Uani 1 d . . . N42 N 0.5734(2) 0.7974(2) 0.2684(2) 0.0387(7) Uani 1 d . . . C43 C 0.3388(3) 0.6456(3) 0.5555(2) 0.0421(9) Uani 1 d . . . H43A H 0.2626 0.6549 0.5868 0.080 Uiso 1 d R . . C44 C 0.4121(4) 0.6264(3) 0.6017(3) 0.0483(10) Uani 1 d . . . H44A H 0.3874 0.6232 0.6644 0.080 Uiso 1 d R . . C45 C 0.5208(4) 0.6122(3) 0.5566(3) 0.0509(10) Uani 1 d . . . H45A H 0.5729 0.5976 0.5874 0.080 Uiso 1 d R . . C46 C 0.5536(3) 0.6188(3) 0.4663(3) 0.0435(9) Uani 1 d . . . H46A H 0.6293 0.6101 0.4332 0.080 Uiso 1 d R . . C47 C 0.4762(3) 0.6388(2) 0.4238(2) 0.0327(8) Uani 1 d . . . C48 C 0.5046(3) 0.6460(2) 0.3236(2) 0.0316(8) Uani 1 d . . . C49 C 0.6002(3) 0.7088(3) 0.2853(2) 0.0350(8) Uani 1 d . . . C50 C 0.7081(3) 0.6744(3) 0.2667(3) 0.0462(10) Uani 1 d . . . H50A H 0.7248 0.6103 0.2797 0.080 Uiso 1 d R . . C51 C 0.7891(3) 0.7340(4) 0.2304(3) 0.0582(12) Uani 1 d . . . H51A H 0.8641 0.7126 0.2189 0.080 Uiso 1 d R . . C52 C 0.7616(4) 0.8250(4) 0.2114(3) 0.0656(14) Uani 1 d . . . H52A H 0.8176 0.8667 0.1840 0.080 Uiso 1 d R . . C53 C 0.6538(3) 0.8558(3) 0.2310(3) 0.0539(11) Uani 1 d . . . H53A H 0.6352 0.9193 0.2177 0.080 Uiso 1 d R . . Cl1 Cl 0.10585(10) 0.64126(11) 0.78724(8) 0.0694(4) Uani 1 d . . . O7 O 0.0055(4) 0.6671(4) 0.8476(3) 0.131(2) Uani 1 d U . . O8 O 0.1745(5) 0.7124(4) 0.7673(4) 0.155(2) Uani 1 d U . . O9 O 0.0910(3) 0.5976(3) 0.7139(2) 0.1020(14) Uani 1 d U . . O10 O 0.1558(6) 0.5722(5) 0.8312(5) 0.185(3) Uani 1 d U . . O2W O 0.1796(2) 0.4497(2) 0.5705(2) 0.0582(8) Uani 1 d . . . H2WA H 0.1465 0.4941 0.6230 0.100 Uiso 1 d R . . H2WB H 0.1469 0.3954 0.5952 0.100 Uiso 1 d R . . O3W O 0.1386(11) 0.9269(9) 0.8346(13) 0.224(8) Uani 0.50 d PU . . H3WA H 0.2093 0.9364 0.8078 0.150 Uiso 0.50 d PR . . H3WB H 0.1062 0.8965 0.8923 0.150 Uiso 0.50 d PR . . O4W O -0.027(6) 1.014(4) 0.012(6) 0.26(3) Uani 0.30 d PU . . H4WA H -0.0632 1.0268 0.0713 0.150 Uiso 0.30 d PR . . H4WB H 0.0485 0.9860 -0.0155 0.150 Uiso 0.30 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0273(2) 0.0240(2) 0.0308(2) 0.00152(18) -0.00341(19) -0.00350(18) Co2 0.0260(2) 0.0246(2) 0.0300(2) 0.00093(18) -0.00164(19) -0.00370(18) Co3 0.0307(3) 0.0272(2) 0.0358(3) 0.00151(19) -0.0059(2) -0.00687(19) Co4 0.0267(2) 0.0258(2) 0.0285(2) 0.00254(18) -0.00184(19) -0.00300(18) O1 0.0301(14) 0.0421(15) 0.0475(16) -0.0034(12) 0.0023(12) -0.0041(11) O2 0.0333(15) 0.0382(16) 0.0647(19) 0.0029(13) 0.0035(13) -0.0025(12) C1 0.0287(19) 0.042(2) 0.035(2) -0.0042(16) -0.0057(15) 0.0008(16) C2 0.033(2) 0.056(3) 0.064(3) -0.010(2) 0.000(2) 0.0058(19) O3 0.0279(13) 0.0436(15) 0.0394(14) 0.0026(12) 0.0010(11) -0.0024(11) O4 0.0410(16) 0.0455(17) 0.069(2) 0.0142(15) 0.0079(14) -0.0012(13) C3 0.033(2) 0.044(2) 0.0295(19) -0.0034(16) -0.0030(15) -0.0019(16) C4 0.030(2) 0.054(3) 0.052(2) -0.002(2) 0.0004(18) -0.0007(18) O5 0.092(3) 0.0337(16) 0.062(2) 0.0014(14) -0.0084(18) -0.0116(16) O6 0.079(3) 0.059(2) 0.173(5) 0.019(3) 0.038(3) 0.005(2) C5 0.061(3) 0.041(2) 0.061(3) 0.001(2) -0.029(2) -0.008(2) C6 0.117(5) 0.051(3) 0.092(4) 0.022(3) -0.031(4) -0.030(3) O1W 0.0474(16) 0.0348(14) 0.0424(15) 0.0082(11) -0.0079(12) -0.0087(12) O11 0.0246(11) 0.0235(11) 0.0302(12) -0.0008(9) -0.0035(9) -0.0045(9) O12 0.0297(13) 0.0312(13) 0.0369(14) 0.0009(10) 0.0023(10) -0.0079(10) N11 0.0295(15) 0.0342(16) 0.0322(16) 0.0007(12) -0.0054(12) -0.0022(12) N12 0.0277(15) 0.0261(14) 0.0358(16) -0.0018(12) -0.0024(12) -0.0020(12) C10 0.035(2) 0.046(2) 0.045(2) 0.0032(18) -0.0123(17) -0.0017(17) C11 0.042(2) 0.062(3) 0.041(2) 0.0044(19) -0.0156(18) -0.002(2) C12 0.041(2) 0.058(3) 0.052(3) -0.008(2) -0.019(2) -0.0044(19) C13 0.035(2) 0.041(2) 0.051(2) -0.0076(18) -0.0133(18) -0.0043(16) C14 0.0214(16) 0.0343(19) 0.0350(19) -0.0030(15) -0.0014(14) -0.0019(14) C15 0.0272(17) 0.0278(17) 0.0306(18) -0.0008(14) -0.0025(14) -0.0068(14) C16 0.0325(18) 0.0283(17) 0.0266(17) 0.0022(14) -0.0056(14) -0.0039(14) C17 0.038(2) 0.0292(18) 0.042(2) -0.0007(16) -0.0081(17) -0.0078(15) C18 0.056(3) 0.0272(19) 0.054(3) -0.0054(17) -0.009(2) -0.0092(17) C19 0.047(2) 0.0288(19) 0.052(2) -0.0061(17) -0.0033(19) 0.0038(17) C20 0.035(2) 0.034(2) 0.048(2) -0.0033(17) 0.0008(17) 0.0024(16) O21 0.0330(13) 0.0261(12) 0.0259(12) -0.0019(9) -0.0042(10) -0.0026(10) O22 0.0519(17) 0.0276(13) 0.0483(16) -0.0023(11) -0.0105(13) 0.0053(12) N21 0.0444(19) 0.0348(17) 0.0429(18) 0.0006(14) -0.0170(15) -0.0100(14) N22 0.0320(16) 0.0403(17) 0.0303(16) 0.0055(13) -0.0026(13) 0.0004(13) C21 0.057(3) 0.050(3) 0.059(3) -0.001(2) -0.026(2) -0.013(2) C22 0.076(4) 0.074(3) 0.063(3) -0.008(3) -0.042(3) -0.015(3) C23 0.095(4) 0.077(4) 0.049(3) -0.014(2) -0.037(3) -0.004(3) C24 0.068(3) 0.054(3) 0.042(2) -0.008(2) -0.020(2) 0.003(2) C25 0.051(2) 0.0244(17) 0.037(2) -0.0025(15) -0.0138(18) -0.0019(16) C26 0.040(2) 0.0280(18) 0.0300(18) -0.0028(14) -0.0051(15) 0.0039(15) C27 0.037(2) 0.037(2) 0.0291(18) -0.0011(15) -0.0041(15) -0.0003(16) C28 0.048(2) 0.053(3) 0.037(2) -0.0039(19) -0.0006(19) 0.013(2) C29 0.044(2) 0.075(3) 0.039(2) 0.005(2) 0.0118(19) 0.016(2) C30 0.044(2) 0.067(3) 0.044(2) 0.015(2) 0.0103(19) 0.001(2) C31 0.039(2) 0.048(2) 0.044(2) 0.0121(18) 0.0012(18) -0.0061(18) O31 0.0327(13) 0.0247(11) 0.0266(12) 0.0049(9) -0.0037(10) -0.0055(9) O32 0.0320(13) 0.0364(14) 0.0450(15) 0.0085(11) 0.0001(11) -0.0082(11) N31 0.0340(16) 0.0290(15) 0.0348(16) 0.0042(12) -0.0051(13) -0.0036(12) N32 0.0284(15) 0.0349(16) 0.0289(15) -0.0010(12) 0.0008(12) -0.0038(12) C32 0.043(2) 0.032(2) 0.053(2) 0.0000(17) -0.0033(19) 0.0017(17) C33 0.059(3) 0.030(2) 0.065(3) 0.0041(19) -0.005(2) 0.0076(19) C34 0.059(3) 0.028(2) 0.058(3) 0.0111(18) -0.009(2) -0.0045(18) C35 0.046(2) 0.038(2) 0.043(2) 0.0096(17) -0.0046(18) -0.0096(18) C36 0.0344(19) 0.0317(18) 0.0294(18) 0.0028(14) -0.0074(15) -0.0053(15) C37 0.0308(18) 0.0263(17) 0.0299(18) 0.0078(14) -0.0015(14) -0.0066(14) C38 0.0288(18) 0.0346(19) 0.0323(19) 0.0033(15) -0.0002(15) -0.0019(15) C39 0.059(3) 0.046(2) 0.038(2) 0.0075(18) -0.0107(19) -0.003(2) C40 0.063(3) 0.069(3) 0.034(2) -0.002(2) -0.014(2) 0.001(2) C41 0.044(2) 0.058(3) 0.042(2) -0.009(2) -0.0097(19) -0.005(2) C42 0.037(2) 0.041(2) 0.036(2) -0.0057(16) -0.0059(16) -0.0024(16) O41 0.0251(12) 0.0283(12) 0.0302(12) 0.0025(10) -0.0049(10) -0.0015(9) O42 0.0415(15) 0.0319(13) 0.0419(15) 0.0002(11) -0.0075(12) 0.0068(11) N41 0.0368(17) 0.0311(15) 0.0311(16) 0.0043(12) -0.0071(13) -0.0029(13) N42 0.0309(16) 0.0385(18) 0.0427(18) 0.0034(14) -0.0041(14) -0.0085(13) C43 0.047(2) 0.040(2) 0.035(2) 0.0050(16) -0.0049(17) -0.0005(17) C44 0.058(3) 0.053(2) 0.034(2) 0.0067(18) -0.0140(19) 0.000(2) C45 0.057(3) 0.055(3) 0.046(2) 0.008(2) -0.026(2) -0.003(2) C46 0.037(2) 0.050(2) 0.044(2) 0.0063(18) -0.0130(18) -0.0016(17) C47 0.0352(19) 0.0290(18) 0.0338(19) 0.0039(14) -0.0103(15) -0.0020(14) C48 0.0280(18) 0.0322(18) 0.0331(18) 0.0037(14) -0.0070(15) -0.0008(14) C49 0.0310(19) 0.045(2) 0.0282(18) 0.0011(15) -0.0064(15) -0.0083(16) C50 0.030(2) 0.062(3) 0.045(2) 0.0018(19) -0.0091(17) -0.0019(18) C51 0.029(2) 0.089(4) 0.054(3) -0.003(2) -0.0077(19) -0.006(2) C52 0.039(3) 0.082(4) 0.070(3) 0.008(3) -0.004(2) -0.030(2) C53 0.046(2) 0.053(3) 0.058(3) 0.006(2) -0.006(2) -0.021(2) Cl1 0.0587(7) 0.1004(10) 0.0516(7) -0.0043(6) -0.0153(6) -0.0309(7) O7 0.088(3) 0.194(6) 0.094(3) -0.061(3) 0.001(3) -0.026(3) O8 0.168(5) 0.156(5) 0.131(4) -0.014(4) -0.011(4) -0.113(4) O9 0.091(3) 0.156(4) 0.062(2) -0.026(2) -0.023(2) -0.030(3) O10 0.225(7) 0.180(6) 0.220(7) 0.020(5) -0.172(6) -0.008(5) O2W 0.0512(18) 0.0553(18) 0.0600(19) 0.0177(15) -0.0037(15) -0.0110(14) O3W 0.133(11) 0.152(12) 0.39(2) 0.106(14) -0.091(14) -0.016(9) O4W 0.35(7) 0.15(4) 0.38(5) 0.11(4) -0.26(6) 0.04(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.029(3) . ? Co1 O11 2.047(3) . ? Co1 N31 2.103(3) . ? Co1 O21 2.126(2) . ? Co1 N11 2.185(3) . ? Co1 O31 2.252(3) . ? Co2 O31 2.030(3) . ? Co2 O3 2.062(3) . ? Co2 O41 2.107(2) . ? Co2 N12 2.109(3) . ? Co2 N32 2.145(3) . ? Co2 O11 2.227(3) . ? Co3 O5 1.998(3) . ? Co3 O21 2.046(3) . ? Co3 N42 2.105(3) . ? Co3 O31 2.118(2) . ? Co3 N21 2.173(3) . ? Co3 O41 2.237(3) . ? Co4 O41 2.044(2) . ? Co4 O1W 2.108(3) . ? Co4 N41 2.129(3) . ? Co4 O11 2.134(2) . ? Co4 N22 2.140(3) . ? Co4 O21 2.161(3) . ? O1 C1 1.260(4) . ? O2 C1 1.255(4) . ? C1 C2 1.509(5) . ? O3 C3 1.284(4) . ? O4 C3 1.224(5) . ? C3 C4 1.514(5) . ? O5 C5 1.223(5) . ? O6 C5 1.257(6) . ? C5 C6 1.433(6) . ? O11 C15 1.398(4) . ? O12 C15 1.404(4) . ? N11 C10 1.346(5) . ? N11 C14 1.347(4) . ? N12 C16 1.333(4) . ? N12 C20 1.351(4) . ? C10 C11 1.382(6) . ? C11 C12 1.377(6) . ? C12 C13 1.378(6) . ? C13 C14 1.382(5) . ? C14 C15 1.543(5) . ? C15 C16 1.529(5) . ? C16 C17 1.391(5) . ? C17 C18 1.381(5) . ? C18 C19 1.373(6) . ? C19 C20 1.373(5) . ? O21 C26 1.400(4) . ? O22 C26 1.400(4) . ? N21 C25 1.334(5) . ? N21 C21 1.346(5) . ? N22 C27 1.343(5) . ? N22 C31 1.354(5) . ? C21 C22 1.373(6) . ? C22 C23 1.370(7) . ? C23 C24 1.384(6) . ? C24 C25 1.380(5) . ? C25 C26 1.545(5) . ? C26 C27 1.518(5) . ? C27 C28 1.384(5) . ? C28 C29 1.386(6) . ? C29 C30 1.369(6) . ? C30 C31 1.366(5) . ? O31 C37 1.396(4) . ? O32 C37 1.399(4) . ? N31 C36 1.344(4) . ? N31 C32 1.352(5) . ? N32 C42 1.340(5) . ? N32 C38 1.342(4) . ? C32 C33 1.377(5) . ? C33 C34 1.383(6) . ? C34 C35 1.380(6) . ? C35 C36 1.392(5) . ? C36 C37 1.519(5) . ? C37 C38 1.543(5) . ? C38 C39 1.392(5) . ? C39 C40 1.385(6) . ? C40 C41 1.372(6) . ? C41 C42 1.374(5) . ? O41 C48 1.398(4) . ? O42 C48 1.418(4) . ? N41 C43 1.344(5) . ? N41 C47 1.348(4) . ? N42 C49 1.335(5) . ? N42 C53 1.356(5) . ? C43 C44 1.381(6) . ? C44 C45 1.373(6) . ? C45 C46 1.385(5) . ? C46 C47 1.385(5) . ? C47 C48 1.540(5) . ? C48 C49 1.535(5) . ? C49 C50 1.390(5) . ? C50 C51 1.370(6) . ? C51 C52 1.377(7) . ? C52 C53 1.375(6) . ? Cl1 O8 1.356(5) . ? Cl1 O7 1.393(4) . ? Cl1 O9 1.405(4) . ? Cl1 O10 1.437(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O11 112.87(10) . . ? O1 Co1 N31 94.80(11) . . ? O11 Co1 N31 149.95(10) . . ? O1 Co1 O21 97.90(11) . . ? O11 Co1 O21 81.35(9) . . ? N31 Co1 O21 107.17(11) . . ? O1 Co1 N11 88.39(12) . . ? O11 Co1 N11 76.07(10) . . ? N31 Co1 N11 93.98(12) . . ? O21 Co1 N11 157.24(10) . . ? O1 Co1 O31 165.58(9) . . ? O11 Co1 O31 79.89(8) . . ? N31 Co1 O31 74.42(10) . . ? O21 Co1 O31 76.78(9) . . ? N11 Co1 O31 101.69(10) . . ? O31 Co2 O3 116.47(10) . . ? O31 Co2 O41 82.48(9) . . ? O3 Co2 O41 91.59(10) . . ? O31 Co2 N12 151.04(11) . . ? O3 Co2 N12 91.21(11) . . ? O41 Co2 N12 106.39(10) . . ? O31 Co2 N32 76.96(10) . . ? O3 Co2 N32 95.51(11) . . ? O41 Co2 N32 159.33(10) . . ? N12 Co2 N32 92.87(11) . . ? O31 Co2 O11 80.85(8) . . ? O3 Co2 O11 158.18(9) . . ? O41 Co2 O11 77.00(9) . . ? N12 Co2 O11 74.68(9) . . ? N32 Co2 O11 101.64(10) . . ? O5 Co3 O21 112.83(12) . . ? O5 Co3 N42 95.37(14) . . ? O21 Co3 N42 149.60(11) . . ? O5 Co3 O31 96.88(12) . . ? O21 Co3 O31 81.57(10) . . ? N42 Co3 O31 107.01(11) . . ? O5 Co3 N21 91.15(12) . . ? O21 Co3 N21 76.34(11) . . ? N42 Co3 N21 92.60(12) . . ? O31 Co3 N21 157.91(11) . . ? O5 Co3 O41 165.67(11) . . ? O21 Co3 O41 79.69(8) . . ? N42 Co3 O41 74.10(10) . . ? O31 Co3 O41 77.52(8) . . ? N21 Co3 O41 98.89(10) . . ? O41 Co4 O1W 111.81(9) . . ? O41 Co4 N41 77.19(11) . . ? O1W Co4 N41 89.58(11) . . ? O41 Co4 O11 80.46(10) . . ? O1W Co4 O11 89.51(9) . . ? N41 Co4 O11 155.51(10) . . ? O41 Co4 N22 153.46(11) . . ? O1W Co4 N22 93.91(11) . . ? N41 Co4 N22 97.36(13) . . ? O11 Co4 N22 107.12(11) . . ? O41 Co4 O21 81.54(9) . . ? O1W Co4 O21 160.59(10) . . ? N41 Co4 O21 107.60(10) . . ? O11 Co4 O21 78.59(8) . . ? N22 Co4 O21 75.37(10) . . ? C1 O1 Co1 137.2(2) . . ? O2 C1 O1 124.5(3) . . ? O2 C1 C2 118.5(3) . . ? O1 C1 C2 117.0(3) . . ? C3 O3 Co2 130.6(2) . . ? O4 C3 O3 124.9(3) . . ? O4 C3 C4 119.1(3) . . ? O3 C3 C4 115.9(3) . . ? C5 O5 Co3 144.0(3) . . ? O5 C5 O6 120.3(4) . . ? O5 C5 C6 122.9(5) . . ? O6 C5 C6 116.8(5) . . ? C15 O11 Co1 117.8(2) . . ? C15 O11 Co4 126.22(19) . . ? Co1 O11 Co4 100.71(9) . . ? C15 O11 Co2 111.04(18) . . ? Co1 O11 Co2 98.74(9) . . ? Co4 O11 Co2 97.47(10) . . ? C10 N11 C14 118.1(3) . . ? C10 N11 Co1 127.8(3) . . ? C14 N11 Co1 114.0(2) . . ? C16 N12 C20 118.0(3) . . ? C16 N12 Co2 117.8(2) . . ? C20 N12 Co2 124.1(2) . . ? N11 C10 C11 123.0(4) . . ? C12 C11 C10 118.4(4) . . ? C11 C12 C13 119.2(4) . . ? C12 C13 C14 119.6(4) . . ? N11 C14 C13 121.7(3) . . ? N11 C14 C15 115.5(3) . . ? C13 C14 C15 122.8(3) . . ? O11 C15 O12 111.2(3) . . ? O11 C15 C16 108.8(3) . . ? O12 C15 C16 106.4(3) . . ? O11 C15 C14 109.4(3) . . ? O12 C15 C14 110.3(3) . . ? C16 C15 C14 110.7(3) . . ? N12 C16 C17 122.4(3) . . ? N12 C16 C15 115.9(3) . . ? C17 C16 C15 121.7(3) . . ? C18 C17 C16 118.4(3) . . ? C19 C18 C17 119.6(3) . . ? C20 C19 C18 118.6(3) . . ? N12 C20 C19 122.9(3) . . ? C26 O21 Co3 116.0(2) . . ? C26 O21 Co1 126.2(2) . . ? Co3 O21 Co1 103.31(10) . . ? C26 O21 Co4 110.00(19) . . ? Co3 O21 Co4 99.34(9) . . ? Co1 O21 Co4 97.36(9) . . ? C25 N21 C21 118.9(4) . . ? C25 N21 Co3 114.0(2) . . ? C21 N21 Co3 127.1(3) . . ? C27 N22 C31 117.9(3) . . ? C27 N22 Co4 115.3(2) . . ? C31 N22 Co4 126.0(3) . . ? N21 C21 C22 122.6(4) . . ? C23 C22 C21 118.2(4) . . ? C22 C23 C24 120.0(4) . . ? C25 C24 C23 118.6(4) . . ? N21 C25 C24 121.7(4) . . ? N21 C25 C26 115.5(3) . . ? C24 C25 C26 122.7(4) . . ? O21 C26 O22 112.1(3) . . ? O21 C26 C27 108.3(3) . . ? O22 C26 C27 107.1(3) . . ? O21 C26 C25 108.2(3) . . ? O22 C26 C25 109.9(3) . . ? C27 C26 C25 111.3(3) . . ? N22 C27 C28 122.1(3) . . ? N22 C27 C26 114.5(3) . . ? C28 C27 C26 123.3(3) . . ? C27 C28 C29 119.0(4) . . ? C30 C29 C28 118.7(4) . . ? C31 C30 C29 119.7(4) . . ? N22 C31 C30 122.4(4) . . ? C37 O31 Co2 117.72(19) . . ? C37 O31 Co3 126.5(2) . . ? Co2 O31 Co3 102.24(10) . . ? C37 O31 Co1 109.85(19) . . ? Co2 O31 Co1 98.43(9) . . ? Co3 O31 Co1 96.92(10) . . ? C36 N31 C32 118.5(3) . . ? C36 N31 Co1 118.2(2) . . ? C32 N31 Co1 123.2(2) . . ? C42 N32 C38 118.5(3) . . ? C42 N32 Co2 127.3(3) . . ? C38 N32 Co2 114.2(2) . . ? N31 C32 C33 122.4(4) . . ? C32 C33 C34 118.9(4) . . ? C35 C34 C33 119.4(4) . . ? C34 C35 C36 118.8(4) . . ? N31 C36 C35 122.0(3) . . ? N31 C36 C37 115.3(3) . . ? C35 C36 C37 122.7(3) . . ? O31 C37 O32 112.6(3) . . ? O31 C37 C36 109.3(3) . . ? O32 C37 C36 107.9(3) . . ? O31 C37 C38 108.1(3) . . ? O32 C37 C38 108.2(3) . . ? C36 C37 C38 110.7(3) . . ? N32 C38 C39 121.3(3) . . ? N32 C38 C37 115.9(3) . . ? C39 C38 C37 122.8(3) . . ? C40 C39 C38 119.1(4) . . ? C41 C40 C39 119.3(4) . . ? C40 C41 C42 118.5(4) . . ? N32 C42 C41 123.3(4) . . ? C48 O41 Co4 117.7(2) . . ? C48 O41 Co2 124.65(19) . . ? Co4 O41 Co2 104.33(11) . . ? C48 O41 Co3 111.84(19) . . ? Co4 O41 Co3 96.96(9) . . ? Co2 O41 Co3 96.02(9) . . ? C43 N41 C47 118.2(3) . . ? C43 N41 Co4 126.3(3) . . ? C47 N41 Co4 115.3(2) . . ? C49 N42 C53 119.0(3) . . ? C49 N42 Co3 118.5(2) . . ? C53 N42 Co3 122.4(3) . . ? N41 C43 C44 122.8(4) . . ? C45 C44 C43 118.9(4) . . ? C44 C45 C46 119.0(4) . . ? C45 C46 C47 119.3(4) . . ? N41 C47 C46 121.7(3) . . ? N41 C47 C48 115.2(3) . . ? C46 C47 C48 123.1(3) . . ? O41 C48 O42 111.6(3) . . ? O41 C48 C49 108.7(3) . . ? O42 C48 C49 109.1(3) . . ? O41 C48 C47 109.9(3) . . ? O42 C48 C47 105.8(3) . . ? C49 C48 C47 111.8(3) . . ? N42 C49 C50 122.2(3) . . ? N42 C49 C48 115.9(3) . . ? C50 C49 C48 121.9(3) . . ? C51 C50 C49 118.6(4) . . ? C50 C51 C52 119.3(4) . . ? C53 C52 C51 120.0(4) . . ? N42 C53 C52 120.9(4) . . ? O8 Cl1 O7 113.3(4) . . ? O8 Cl1 O9 113.9(3) . . ? O7 Cl1 O9 110.4(3) . . ? O8 Cl1 O10 105.7(4) . . ? O7 Cl1 O10 105.0(4) . . ? O9 Cl1 O10 107.9(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.840 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.068 #============================================================END data_complex_4 _database_code_CSD 144515 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H57 Cl2 N8 O27.50 Zn4' _chemical_formula_weight 1518.40 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.328(6) _cell_length_b 24.181(12) _cell_length_c 16.060(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.25(1) _cell_angle_gamma 90.00 _cell_volume 5905(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3100 _exptl_absorpt_coefficient_mu 1.791 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.957 _exptl_absorpt_correction_T_max 0.605 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10881 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.1147 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.02 _reflns_number_total 10386 _reflns_number_gt 5626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10386 _refine_ls_number_parameters 812 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1432 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 1.035 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.81653(5) 0.15097(3) 0.37214(5) 0.0286(2) Uani 1 d . . . Zn2 Zn 0.68307(5) 0.15775(3) 0.51290(5) 0.0285(2) Uani 1 d . . . Zn3 Zn 0.66539(5) 0.25026(4) 0.36429(5) 0.0289(2) Uani 1 d . . . Zn4 Zn 0.83393(5) 0.25432(4) 0.50595(5) 0.0305(2) Uani 1 d . . . O1 O 0.8248(3) 0.16712(18) 0.5000(3) 0.0273(11) Uani 1 d . . . O2 O 0.9615(3) 0.1488(2) 0.5725(3) 0.0369(13) Uani 1 d . . . H2 H 0.9809 0.1619 0.5244 0.080 Uiso 1 d R . . O3 O 0.6991(3) 0.24527(19) 0.5029(3) 0.0269(11) Uani 1 d . . . O4 O 0.6476(3) 0.2724(2) 0.6241(3) 0.0374(13) Uani 1 d . . . H4 H 0.6534 0.2290 0.6367 0.080 Uiso 1 d R . . O5 O 0.8010(3) 0.23903(18) 0.3695(3) 0.0278(11) Uani 1 d . . . O6 O 0.8538(3) 0.2541(2) 0.2445(3) 0.0335(12) Uani 1 d . . . H6 H 0.8896 0.2148 0.2521 0.080 Uiso 1 d R . . O7 O 0.6727(3) 0.16550(17) 0.3838(3) 0.0254(11) Uani 1 d . . . O8 O 0.5361(3) 0.14692(19) 0.3115(3) 0.0331(12) Uani 1 d . . . H8 H 0.5138 0.1540 0.3591 0.080 Uiso 1 d R . . O9 O 0.9271(3) 0.1612(2) 0.3172(3) 0.0372(13) Uani 1 d . . . O10 O 1.0278(3) 0.1490(2) 0.4265(3) 0.0431(14) Uani 1 d . . . O11 O 0.5702(3) 0.1729(2) 0.5641(3) 0.0369(13) Uani 1 d . . . O12 O 0.4701(3) 0.1488(2) 0.4588(3) 0.0452(15) Uani 1 d . . . N1 N 0.8469(4) 0.0732(2) 0.4290(4) 0.0310(15) Uani 1 d . . . N2 N 0.7488(4) 0.1333(2) 0.6294(3) 0.0306(14) Uani 1 d . . . N3 N 0.5522(4) 0.2763(2) 0.4129(4) 0.0318(15) Uani 1 d . . . N4 N 0.7875(4) 0.3360(3) 0.5248(4) 0.0398(17) Uani 1 d . . . N5 N 0.9463(4) 0.2785(2) 0.4551(4) 0.0349(15) Uani 1 d . . . N6 N 0.7134(4) 0.3281(2) 0.3286(4) 0.0349(15) Uani 1 d . . . N7 N 0.7474(4) 0.1200(2) 0.2606(4) 0.0322(15) Uani 1 d . . . N8 N 0.6503(4) 0.0770(2) 0.4686(4) 0.0328(15) Uani 1 d . . . C1 C 0.8445(5) 0.0247(3) 0.3895(5) 0.044(2) Uani 1 d . . . H1A H 0.8280 0.0244 0.3298 0.080 Uiso 1 d R . . C2 C 0.8644(6) -0.0244(3) 0.4297(6) 0.056(3) Uani 1 d . . . H2A H 0.8582 -0.0590 0.4002 0.080 Uiso 1 d R . . C3 C 0.8911(6) -0.0228(3) 0.5125(6) 0.057(3) Uani 1 d . . . H3A H 0.9088 -0.0566 0.5413 0.080 Uiso 1 d R . . C4 C 0.8959(5) 0.0265(3) 0.5557(5) 0.045(2) Uani 1 d . . . H4A H 0.9133 0.0275 0.6152 0.080 Uiso 1 d R . . C5 C 0.8728(4) 0.0745(3) 0.5103(5) 0.0297(17) Uani 1 d . . . C6 C 0.8734(4) 0.1312(3) 0.5530(4) 0.0289(17) Uani 1 d . . . C7 C 0.8359(5) 0.1269(3) 0.6348(4) 0.0307(18) Uani 1 d . . . C8 C 0.8867(5) 0.1133(3) 0.7090(5) 0.038(2) Uani 1 d . . . H8A H 0.9493 0.1094 0.7114 0.080 Uiso 1 d R . . C9 C 0.8450(6) 0.1044(3) 0.7788(5) 0.042(2) Uani 1 d . . . H9A H 0.8789 0.0954 0.8315 0.080 Uiso 1 d R . . C10 C 0.7562(6) 0.1100(3) 0.7734(5) 0.046(2) Uani 1 d . . . H10A H 0.7267 0.1028 0.8216 0.080 Uiso 1 d R . . C11 C 0.7103(5) 0.1251(3) 0.6987(5) 0.041(2) Uani 1 d . . . H11A H 0.6477 0.1296 0.6953 0.080 Uiso 1 d R . . C12 C 0.4703(5) 0.2772(3) 0.3715(5) 0.043(2) Uani 1 d . . . H12A H 0.4624 0.2652 0.3140 0.080 Uiso 1 d R . . C13 C 0.3988(5) 0.2922(4) 0.4077(5) 0.049(2) Uani 1 d . . . H13A H 0.3412 0.2912 0.3764 0.080 Uiso 1 d R . . C14 C 0.4101(5) 0.3090(4) 0.4896(6) 0.056(3) Uani 1 d . . . H14A H 0.3605 0.3214 0.5155 0.080 Uiso 1 d R . . C15 C 0.4932(5) 0.3082(4) 0.5339(5) 0.051(2) Uani 1 d . . . H15A H 0.5020 0.3195 0.5916 0.080 Uiso 1 d R . . C16 C 0.5622(5) 0.2909(3) 0.4940(5) 0.0338(19) Uani 1 d . . . C17 C 0.6548(5) 0.2851(3) 0.5402(4) 0.0304(18) Uani 1 d . . . C18 C 0.7047(5) 0.3402(3) 0.5405(5) 0.0365(19) Uani 1 d . . . C19 C 0.6679(6) 0.3896(4) 0.5526(6) 0.060(3) Uani 1 d . . . H19A H 0.6085 0.3917 0.5654 0.080 Uiso 1 d R . . C20 C 0.7170(8) 0.4375(4) 0.5468(7) 0.081(4) Uani 1 d . . . H20A H 0.6926 0.4734 0.5545 0.080 Uiso 1 d R . . C21 C 0.8011(7) 0.4337(4) 0.5288(6) 0.072(3) Uani 1 d . . . H21A H 0.8365 0.4658 0.5232 0.080 Uiso 1 d R . . C22 C 0.8343(6) 0.3813(4) 0.5187(5) 0.048(2) Uani 1 d . . . H22A H 0.8937 0.3769 0.5069 0.080 Uiso 1 d R . . C23 C 1.0260(5) 0.2854(3) 0.4993(5) 0.044(2) Uani 1 d . . . H23A H 1.0319 0.2812 0.5592 0.080 Uiso 1 d R . . C24 C 1.0982(5) 0.2981(3) 0.4622(6) 0.054(2) Uani 1 d . . . H24A H 1.1540 0.3033 0.4958 0.080 Uiso 1 d R . . C25 C 1.0917(5) 0.3036(4) 0.3771(6) 0.052(2) Uani 1 d . . . H25A H 1.1418 0.3131 0.3498 0.080 Uiso 1 d R . . C26 C 1.0098(5) 0.2957(3) 0.3314(6) 0.046(2) Uani 1 d . . . H26A H 1.0029 0.2980 0.2712 0.080 Uiso 1 d R . . C27 C 0.9390(5) 0.2837(3) 0.3726(5) 0.0302(18) Uani 1 d . . . C28 C 0.8460(5) 0.2749(3) 0.3263(5) 0.0326(18) Uani 1 d . . . C29 C 0.7967(5) 0.3297(3) 0.3137(4) 0.0304(17) Uani 1 d . . . C30 C 0.8340(5) 0.3771(3) 0.2889(5) 0.041(2) Uani 1 d . . . H30A H 0.8935 0.3765 0.2762 0.080 Uiso 1 d R . . C31 C 0.7854(6) 0.4242(4) 0.2807(6) 0.059(3) Uani 1 d . . . H31A H 0.8115 0.4582 0.2655 0.080 Uiso 1 d R . . C32 C 0.6998(6) 0.4231(4) 0.2963(6) 0.059(3) Uani 1 d . . . H32A H 0.6648 0.4562 0.2906 0.080 Uiso 1 d R . . C33 C 0.6657(5) 0.3744(3) 0.3194(5) 0.046(2) Uani 1 d . . . H33A H 0.6049 0.3730 0.3281 0.080 Uiso 1 d R . . C34 C 0.7863(5) 0.1067(3) 0.1927(5) 0.042(2) Uani 1 d . . . H34A H 0.8491 0.1094 0.1958 0.080 Uiso 1 d R . . C35 C 0.7394(6) 0.0880(4) 0.1199(5) 0.052(2) Uani 1 d . . . H35A H 0.7681 0.0783 0.0721 0.080 Uiso 1 d R . . C36 C 0.6495(6) 0.0838(3) 0.1153(5) 0.050(2) Uani 1 d . . . H36A H 0.6148 0.0722 0.0644 0.080 Uiso 1 d R . . C37 C 0.6095(5) 0.0972(3) 0.1842(5) 0.042(2) Uani 1 d . . . H37A H 0.5470 0.0939 0.1830 0.080 Uiso 1 d R . . C38 C 0.6600(4) 0.1143(3) 0.2568(4) 0.0267(17) Uani 1 d . . . C39 C 0.6222(4) 0.1267(3) 0.3382(5) 0.0309(18) Uani 1 d . . . C40 C 0.6168(5) 0.0737(3) 0.3893(5) 0.0307(18) Uani 1 d . . . C41 C 0.5763(5) 0.0274(3) 0.3537(5) 0.042(2) Uani 1 d . . . H41A H 0.5518 0.0267 0.2956 0.080 Uiso 1 d R . . C42 C 0.5737(6) -0.0181(4) 0.4048(6) 0.061(3) Uani 1 d . . . H42A H 0.5439 -0.0510 0.3829 0.080 Uiso 1 d R . . C43 C 0.6101(6) -0.0165(4) 0.4859(6) 0.062(3) Uani 1 d . . . H43A H 0.6093 -0.0485 0.5213 0.080 Uiso 1 d R . . C44 C 0.6471(5) 0.0321(3) 0.5157(5) 0.041(2) Uani 1 d . . . H44A H 0.6744 0.0339 0.5728 0.080 Uiso 1 d R . . C45 C 1.0059(5) 0.1559(3) 0.3502(5) 0.0344(18) Uani 1 d . . . C46 C 1.0758(5) 0.1583(4) 0.2931(5) 0.060(3) Uani 1 d . . . H46A H 1.1327 0.1539 0.3250 0.080 Uiso 1 d R . . H46B H 1.0659 0.1288 0.2530 0.080 Uiso 1 d R . . H46C H 1.0733 0.1931 0.2642 0.080 Uiso 1 d R . . C47 C 0.4920(5) 0.1631(3) 0.5314(5) 0.038(2) Uani 1 d . . . C48 C 0.4223(5) 0.1709(4) 0.5887(6) 0.063(3) Uani 1 d . . . H48A H 0.3656 0.1626 0.5587 0.080 Uiso 1 d R . . H48B H 0.4337 0.1468 0.6363 0.080 Uiso 1 d R . . H48C H 0.4233 0.2086 0.6074 0.080 Uiso 1 d R . . O1W O 0.9004(3) 0.2535(2) 0.6286(3) 0.0426(14) Uani 1 d . . . H1WA H 0.8590 0.2458 0.6722 0.080 Uiso 1 d R . . H1WB H 0.9407 0.2272 0.6134 0.080 Uiso 1 d R . . O2W O 0.5973(3) 0.2442(2) 0.2428(3) 0.0426(14) Uani 1 d . . . H2WA H 0.6404 0.2397 0.2131 0.080 Uiso 1 d R . . H2WB H 0.5812 0.2092 0.2397 0.080 Uiso 1 d R . . O3W O 0.7979(4) 0.2731(3) 0.7436(4) 0.073(2) Uani 1 d . . . H3WA H 0.8014 0.2846 0.8024 0.080 Uiso 1 d R . . H3WB H 0.7399 0.2758 0.7209 0.080 Uiso 1 d R . . O4W O 0.8051(4) 0.3554(3) 0.8686(4) 0.0656(18) Uani 1 d . . . H4WA H 0.8247 0.3792 0.8220 0.080 Uiso 1 d R . . H4WB H 0.8562 0.3672 0.9075 0.080 Uiso 1 d R . . O5W O 0.7041(4) 0.2561(3) 0.1277(4) 0.0701(19) Uani 1 d . . . H5WB H 0.7619 0.2509 0.1497 0.080 Uiso 1 d R . . H5WA H 0.7155 0.2969 0.1192 0.080 Uiso 1 d R . . O6W O 0.6990(4) 0.3349(3) 0.0011(4) 0.083(2) Uani 1 d . . . H6WA H 0.7108 0.2997 -0.0181 0.080 Uiso 1 d R . . H6WB H 0.6490 0.3466 -0.0189 0.080 Uiso 1 d R . . O7W O 0.7800(5) 0.4568(4) 0.7884(5) 0.131(3) Uani 1 d . . . H7WA H 0.7803 0.4606 0.8455 0.080 Uiso 1 d R . . H7WB H 0.7597 0.4926 0.7610 0.080 Uiso 1 d R . . O8W O 0.5975(17) 0.5602(10) 0.5175(17) 0.252(15) Uani 0.50 d P . . H8WA H 0.6424 0.5622 0.4865 0.080 Uiso 0.50 d PR . . H8WB H 0.5845 0.5295 0.5368 0.080 Uiso 0.50 d PR . . Cl1 Cl 0.94529(15) 0.54023(10) 0.65569(17) 0.0611(7) Uani 1 d . . . O13 O 0.9611(4) 0.5772(3) 0.7250(4) 0.0680(19) Uani 1 d . . . O14 O 0.8775(5) 0.5604(3) 0.5962(4) 0.080(2) Uani 1 d . . . O15 O 1.0213(5) 0.5334(4) 0.6195(7) 0.150(4) Uani 1 d . . . O16 O 0.9184(6) 0.4889(3) 0.6843(6) 0.124(3) Uani 1 d . . . Cl2 Cl 0.51000(17) 0.48015(12) 0.6818(2) 0.0722(8) Uani 1 d . . . O17 O 0.4730(6) 0.4823(4) 0.7556(5) 0.124(3) Uani 1 d . . . O18 O 0.4854(6) 0.5292(3) 0.6365(6) 0.125(3) Uani 1 d . . . O19 O 0.6012(5) 0.4766(3) 0.6963(6) 0.115(3) Uani 1 d . . . O20 O 0.4764(5) 0.4330(3) 0.6380(5) 0.103(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0288(5) 0.0328(5) 0.0231(5) 0.0005(4) -0.0010(4) 0.0000(4) Zn2 0.0281(5) 0.0351(5) 0.0212(5) 0.0009(4) -0.0004(4) -0.0010(4) Zn3 0.0270(5) 0.0332(5) 0.0248(5) 0.0027(4) -0.0031(4) 0.0000(4) Zn4 0.0284(5) 0.0344(5) 0.0264(5) -0.0011(4) -0.0057(4) -0.0020(4) O1 0.026(3) 0.032(3) 0.022(3) -0.001(2) -0.001(2) 0.002(2) O2 0.027(3) 0.050(3) 0.032(3) 0.007(3) -0.003(2) 0.001(2) O3 0.025(3) 0.028(3) 0.026(3) -0.001(2) -0.002(2) 0.006(2) O4 0.040(3) 0.049(3) 0.022(3) -0.005(3) 0.001(2) 0.009(3) O5 0.029(3) 0.029(3) 0.024(3) 0.007(2) -0.002(2) -0.007(2) O6 0.033(3) 0.043(3) 0.024(3) -0.003(3) 0.001(2) -0.002(2) O7 0.031(3) 0.025(3) 0.018(3) -0.001(2) -0.006(2) -0.008(2) O8 0.027(3) 0.040(3) 0.031(3) -0.003(2) -0.003(2) 0.000(2) O9 0.027(3) 0.050(3) 0.034(3) 0.003(3) 0.000(2) 0.004(2) O10 0.024(3) 0.060(4) 0.045(4) 0.011(3) 0.005(3) 0.003(3) O11 0.024(3) 0.052(3) 0.034(3) -0.002(3) 0.002(2) 0.001(2) O12 0.035(3) 0.076(4) 0.025(3) -0.008(3) 0.004(2) -0.001(3) N1 0.032(4) 0.032(4) 0.028(4) -0.001(3) 0.001(3) 0.005(3) N2 0.035(4) 0.038(4) 0.018(3) 0.006(3) -0.002(3) -0.001(3) N3 0.033(4) 0.034(4) 0.026(4) 0.004(3) -0.004(3) 0.002(3) N4 0.039(4) 0.035(4) 0.042(4) -0.009(3) -0.007(3) -0.007(3) N5 0.029(4) 0.040(4) 0.032(4) 0.001(3) -0.009(3) -0.005(3) N6 0.039(4) 0.030(4) 0.035(4) 0.007(3) 0.000(3) 0.004(3) N7 0.035(4) 0.039(4) 0.022(4) -0.001(3) 0.002(3) -0.004(3) N8 0.035(4) 0.037(4) 0.027(4) 0.008(3) 0.002(3) -0.005(3) C1 0.055(6) 0.037(5) 0.040(5) -0.010(4) 0.005(4) -0.005(4) C2 0.089(7) 0.025(5) 0.053(6) 0.001(4) 0.006(5) 0.009(5) C3 0.082(7) 0.034(5) 0.054(7) 0.013(5) 0.007(5) 0.024(5) C4 0.052(5) 0.037(5) 0.042(5) 0.002(4) -0.002(4) 0.010(4) C5 0.021(4) 0.036(5) 0.031(5) 0.003(4) 0.003(3) 0.002(3) C6 0.025(4) 0.031(4) 0.027(4) -0.001(3) -0.011(3) 0.010(3) C7 0.035(4) 0.037(4) 0.020(4) 0.001(3) 0.005(3) 0.001(4) C8 0.038(5) 0.048(5) 0.024(5) 0.005(4) -0.009(4) 0.003(4) C9 0.056(6) 0.051(5) 0.018(4) -0.001(4) -0.005(4) 0.008(4) C10 0.071(6) 0.047(5) 0.021(5) 0.007(4) 0.008(4) 0.003(5) C11 0.042(5) 0.046(5) 0.036(5) 0.005(4) 0.008(4) -0.002(4) C12 0.032(5) 0.052(5) 0.042(5) 0.000(4) -0.007(4) 0.008(4) C13 0.038(5) 0.064(6) 0.042(6) 0.000(5) -0.013(4) 0.008(4) C14 0.037(5) 0.067(7) 0.065(7) -0.006(5) 0.007(5) 0.024(5) C15 0.041(5) 0.065(6) 0.045(6) -0.011(5) -0.005(4) 0.015(5) C16 0.030(4) 0.030(4) 0.040(5) -0.004(4) 0.001(4) 0.007(3) C17 0.034(4) 0.034(5) 0.022(4) -0.004(3) -0.001(3) 0.009(4) C18 0.042(5) 0.045(5) 0.021(4) -0.010(4) 0.000(4) 0.004(4) C19 0.070(7) 0.041(6) 0.072(7) -0.011(5) 0.017(5) 0.002(5) C20 0.101(9) 0.034(6) 0.107(10) -0.029(6) 0.010(7) 0.006(6) C21 0.086(8) 0.044(6) 0.085(8) -0.027(6) 0.008(7) -0.011(6) C22 0.052(6) 0.054(6) 0.035(5) -0.007(4) -0.007(4) -0.011(5) C23 0.042(5) 0.057(6) 0.030(5) 0.002(4) -0.014(4) -0.010(4) C24 0.035(5) 0.058(6) 0.063(7) 0.013(5) -0.015(5) -0.015(4) C25 0.034(5) 0.063(6) 0.055(7) 0.013(5) -0.002(4) -0.012(4) C26 0.031(5) 0.051(5) 0.054(6) 0.019(5) 0.005(4) -0.007(4) C27 0.029(4) 0.027(4) 0.031(5) 0.006(3) -0.011(3) -0.001(3) C28 0.027(4) 0.041(5) 0.028(5) 0.004(4) -0.004(3) -0.005(3) C29 0.027(4) 0.031(4) 0.031(5) 0.007(3) -0.003(3) -0.001(3) C30 0.041(5) 0.040(5) 0.041(5) 0.011(4) 0.000(4) -0.002(4) C31 0.063(6) 0.039(5) 0.072(7) 0.020(5) 0.004(5) 0.004(5) C32 0.055(6) 0.053(6) 0.068(7) 0.000(5) 0.006(5) 0.018(5) C33 0.044(5) 0.032(5) 0.061(6) 0.013(4) 0.000(4) 0.001(4) C34 0.037(5) 0.053(5) 0.036(5) -0.008(4) 0.010(4) -0.005(4) C35 0.057(6) 0.072(7) 0.027(5) -0.012(5) 0.009(4) -0.008(5) C36 0.064(6) 0.056(6) 0.029(5) -0.017(4) 0.000(4) -0.013(5) C37 0.043(5) 0.060(6) 0.022(4) -0.008(4) 0.003(4) -0.015(4) C38 0.027(4) 0.030(4) 0.022(4) -0.004(3) -0.002(3) -0.005(3) C39 0.020(4) 0.043(5) 0.030(5) -0.006(4) 0.004(3) 0.002(3) C40 0.036(4) 0.027(4) 0.029(5) 0.004(3) 0.003(4) -0.006(3) C41 0.051(5) 0.039(5) 0.035(5) -0.007(4) 0.006(4) -0.009(4) C42 0.082(7) 0.042(6) 0.056(7) 0.004(5) 0.002(5) -0.030(5) C43 0.089(8) 0.042(6) 0.053(7) 0.013(5) -0.001(6) -0.015(5) C44 0.049(5) 0.040(5) 0.033(5) 0.009(4) 0.000(4) -0.012(4) C45 0.032(4) 0.033(4) 0.040(5) 0.001(4) 0.008(4) 0.005(4) C46 0.044(5) 0.093(8) 0.042(6) -0.004(5) 0.004(4) -0.005(5) C47 0.029(5) 0.045(5) 0.041(5) 0.004(4) 0.013(4) 0.000(4) C48 0.041(5) 0.094(8) 0.056(6) -0.019(6) 0.016(5) -0.007(5) O1W 0.046(3) 0.049(3) 0.030(3) -0.002(3) -0.008(2) 0.005(3) O2W 0.043(3) 0.053(4) 0.029(3) 0.006(3) -0.009(2) -0.005(3) O3W 0.056(4) 0.126(6) 0.034(4) -0.017(4) -0.006(3) 0.014(4) O4W 0.047(4) 0.089(5) 0.057(4) -0.002(4) -0.007(3) -0.009(3) O5W 0.052(4) 0.109(6) 0.045(4) 0.008(4) -0.009(3) -0.023(4) O6W 0.060(4) 0.105(6) 0.079(5) 0.030(4) -0.014(4) -0.001(4) O7W 0.148(8) 0.141(8) 0.099(7) 0.055(6) -0.007(6) 0.017(6) O8W 0.25(3) 0.21(3) 0.31(4) 0.12(3) 0.08(3) -0.01(2) Cl1 0.0523(15) 0.0506(15) 0.0768(19) 0.0007(14) -0.0053(13) 0.0018(12) O13 0.071(5) 0.073(5) 0.058(4) -0.007(4) 0.001(3) -0.012(4) O14 0.116(6) 0.066(5) 0.053(5) 0.006(4) -0.006(4) 0.029(4) O15 0.074(6) 0.199(11) 0.183(10) -0.088(8) 0.044(6) 0.005(6) O16 0.153(8) 0.065(5) 0.133(8) 0.040(5) -0.067(6) -0.030(5) Cl2 0.0591(17) 0.0686(18) 0.093(2) -0.0160(17) 0.0240(16) -0.0064(14) O17 0.120(7) 0.170(9) 0.091(7) -0.029(6) 0.050(6) 0.006(6) O18 0.109(7) 0.086(6) 0.177(10) 0.038(6) 0.008(6) -0.003(5) O19 0.052(5) 0.084(6) 0.211(10) -0.024(6) 0.029(6) -0.001(4) O20 0.091(6) 0.093(6) 0.128(8) -0.042(5) 0.024(5) -0.029(5) _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 Zn1 O9 2.022(5) . ? Zn1 O1 2.078(5) . ? Zn1 N7 2.100(6) . ? Zn1 N1 2.117(6) . ? Zn1 O5 2.142(5) . ? Zn1 O7 2.264(5) . ? Zn2 O11 2.040(5) . ? Zn2 O7 2.068(4) . ? Zn2 N2 2.096(6) . ? Zn2 N8 2.116(6) . ? Zn2 O3 2.139(5) . ? Zn2 O1 2.220(4) . ? Zn3 O7 2.074(4) . ? Zn3 O5 2.088(5) . ? Zn3 N3 2.088(6) . ? Zn3 O2W 2.099(5) . ? Zn3 N6 2.125(6) . ? Zn3 O3 2.224(5) . ? Zn4 O3 2.072(4) . ? Zn4 N5 2.081(6) . ? Zn4 O1W 2.100(5) . ? Zn4 O1 2.115(5) . ? Zn4 N4 2.133(6) . ? Zn4 O5 2.216(5) . ? O1 C6 1.368(8) . ? O2 C6 1.412(8) . ? O3 C17 1.360(8) . ? O4 C17 1.401(8) . ? O5 C28 1.352(8) . ? O6 C28 1.425(8) . ? O7 C39 1.368(8) . ? O8 C39 1.423(8) . ? O9 C45 1.263(8) . ? O10 C45 1.241(9) . ? O11 C47 1.269(9) . ? O12 C47 1.223(9) . ? N1 C5 1.316(9) . ? N1 C1 1.332(9) . ? N2 C7 1.337(8) . ? N2 C11 1.338(9) . ? N3 C16 1.338(9) . ? N3 C12 1.346(9) . ? N4 C22 1.320(9) . ? N4 C18 1.329(9) . ? N5 C27 1.322(9) . ? N5 C23 1.344(9) . ? N6 C29 1.329(8) . ? N6 C33 1.337(9) . ? N7 C38 1.341(8) . ? N7 C34 1.346(9) . ? N8 C40 1.314(9) . ? N8 C44 1.328(9) . ? C1 C2 1.368(11) . ? C2 C3 1.341(12) . ? C3 C4 1.378(11) . ? C4 C5 1.391(10) . ? C5 C6 1.534(9) . ? C6 C7 1.503(9) . ? C7 C8 1.378(9) . ? C8 C9 1.376(10) . ? C9 C10 1.360(10) . ? C10 C11 1.363(10) . ? C12 C13 1.353(10) . ? C13 C14 1.367(11) . ? C14 C15 1.378(11) . ? C15 C16 1.370(10) . ? C16 C17 1.523(10) . ? C17 C18 1.536(10) . ? C18 C19 1.345(10) . ? C19 C20 1.391(12) . ? C20 C21 1.359(13) . ? C21 C22 1.381(12) . ? C23 C24 1.357(10) . ? C24 C25 1.365(11) . ? C25 C26 1.385(10) . ? C26 C27 1.371(9) . ? C27 C28 1.537(9) . ? C28 C29 1.526(10) . ? C29 C30 1.362(9) . ? C30 C31 1.358(10) . ? C31 C32 1.366(11) . ? C32 C33 1.359(11) . ? C34 C35 1.369(10) . ? C35 C36 1.374(11) . ? C36 C37 1.369(10) . ? C37 C38 1.378(9) . ? C38 C39 1.525(9) . ? C39 C40 1.530(10) . ? C40 C41 1.369(10) . ? C41 C42 1.378(11) . ? C42 C43 1.351(12) . ? C43 C44 1.365(11) . ? C45 C46 1.497(10) . ? C47 C48 1.507(10) . ? Cl1 O15 1.377(7) . ? Cl1 O16 1.404(7) . ? Cl1 O14 1.407(7) . ? Cl1 O13 1.425(6) . ? Cl2 O17 1.378(7) . ? Cl2 O19 1.390(7) . ? Cl2 O20 1.404(7) . ? Cl2 O18 1.417(8) . ? O1W O3W 2.614(8) . ? O2W O5W 2.635(8) . ? O3W O4W 2.819(8) . ? O4W O12 2.752(8) 4_666 ? O6W O10 2.770(8) 4_565 ? O2 O10 2.670(7) . ? O2 O1W 2.882(7) . ? O4 O11 2.800(7) . ? O4 O3W 2.806(8) . ? O6 O9 2.710(7) . ? O6 O5W 2.776(7) . ? O8 O12 2.688(7) . ? O8 O2W 2.809(7) . ? 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 O9 Zn1 O1 117.27(19) . . ? O9 Zn1 N7 91.8(2) . . ? O1 Zn1 N7 150.6(2) . . ? O9 Zn1 N1 98.4(2) . . ? O1 Zn1 N1 76.0(2) . . ? N7 Zn1 N1 96.4(2) . . ? O9 Zn1 O5 88.11(19) . . ? O1 Zn1 O5 79.95(17) . . ? N7 Zn1 O5 107.1(2) . . ? N1 Zn1 O5 155.4(2) . . ? O9 Zn1 O7 153.61(18) . . ? O1 Zn1 O7 80.09(16) . . ? N7 Zn1 O7 74.6(2) . . ? N1 Zn1 O7 105.40(19) . . ? O5 Zn1 O7 74.96(16) . . ? O11 Zn2 O7 115.21(19) . . ? O11 Zn2 N2 91.5(2) . . ? O7 Zn2 N2 152.7(2) . . ? O11 Zn2 N8 97.1(2) . . ? O7 Zn2 N8 76.2(2) . . ? N2 Zn2 N8 96.1(2) . . ? O11 Zn2 O3 87.94(19) . . ? O7 Zn2 O3 80.22(17) . . ? N2 Zn2 O3 107.4(2) . . ? N8 Zn2 O3 155.8(2) . . ? O11 Zn2 O1 155.36(19) . . ? O7 Zn2 O1 81.36(16) . . ? N2 Zn2 O1 75.3(2) . . ? N8 Zn2 O1 104.85(19) . . ? O3 Zn2 O1 76.63(16) . . ? O7 Zn3 O5 80.28(17) . . ? O7 Zn3 N3 105.9(2) . . ? O5 Zn3 N3 153.4(2) . . ? O7 Zn3 O2W 94.70(19) . . ? O5 Zn3 O2W 113.81(19) . . ? N3 Zn3 O2W 91.7(2) . . ? O7 Zn3 N6 154.4(2) . . ? O5 Zn3 N6 75.5(2) . . ? N3 Zn3 N6 99.5(2) . . ? O2W Zn3 N6 87.7(2) . . ? O7 Zn3 O3 78.11(17) . . ? O5 Zn3 O3 81.26(17) . . ? N3 Zn3 O3 75.0(2) . . ? O2W Zn3 O3 162.25(18) . . ? N6 Zn3 O3 105.8(2) . . ? O3 Zn4 N5 153.2(2) . . ? O3 Zn4 O1W 112.66(19) . . ? N5 Zn4 O1W 92.5(2) . . ? O3 Zn4 O1 80.42(17) . . ? N5 Zn4 O1 108.4(2) . . ? O1W Zn4 O1 93.12(19) . . ? O3 Zn4 N4 75.6(2) . . ? N5 Zn4 N4 95.9(2) . . ? O1W Zn4 N4 90.4(2) . . ? O1 Zn4 N4 155.2(2) . . ? O3 Zn4 O5 81.79(17) . . ? N5 Zn4 O5 75.8(2) . . ? O1W Zn4 O5 161.52(18) . . ? O1 Zn4 O5 77.50(16) . . ? N4 Zn4 O5 104.9(2) . . ? C6 O1 Zn1 117.1(4) . . ? C6 O1 Zn4 125.2(4) . . ? Zn1 O1 Zn4 103.15(19) . . ? C6 O1 Zn2 109.8(4) . . ? Zn1 O1 Zn2 97.73(18) . . ? Zn4 O1 Zn2 99.06(18) . . ? C6 O2 O10 105.4(4) . . ? C6 O2 O1W 89.7(4) . . ? O10 O2 O1W 116.6(2) . . ? C17 O3 Zn4 117.8(4) . . ? C17 O3 Zn2 126.8(4) . . ? Zn4 O3 Zn2 103.10(19) . . ? C17 O3 Zn3 109.6(4) . . ? Zn4 O3 Zn3 97.07(17) . . ? Zn2 O3 Zn3 96.57(18) . . ? C17 O4 O11 86.5(4) . . ? C17 O4 O3W 119.9(4) . . ? O11 O4 O3W 121.1(2) . . ? C28 O5 Zn3 117.7(4) . . ? C28 O5 Zn1 125.8(4) . . ? Zn3 O5 Zn1 103.74(18) . . ? C28 O5 Zn4 109.5(4) . . ? Zn3 O5 Zn4 96.85(18) . . ? Zn1 O5 Zn4 97.79(17) . . ? C28 O6 O9 88.5(4) . . ? C28 O6 O5W 117.3(4) . . ? O9 O6 O5W 124.6(2) . . ? C39 O7 Zn2 116.2(4) . . ? C39 O7 Zn3 125.5(4) . . ? Zn2 O7 Zn3 103.71(19) . . ? C39 O7 Zn1 109.9(4) . . ? Zn2 O7 Zn1 96.67(18) . . ? Zn3 O7 Zn1 100.09(17) . . ? C39 O8 O12 100.3(4) . . ? C39 O8 O2W 93.6(4) . . ? O12 O8 O2W 120.9(2) . . ? C45 O9 Zn1 127.9(5) . . ? C45 O9 O6 126.0(5) . . ? Zn1 O9 O6 87.98(19) . . ? C45 O10 O2 141.5(5) . . ? C47 O11 Zn2 127.2(5) . . ? C47 O11 O4 129.8(5) . . ? Zn2 O11 O4 87.08(19) . . ? C47 O12 O8 139.1(5) . . ? C5 N1 C1 118.6(7) . . ? C5 N1 Zn1 115.4(5) . . ? C1 N1 Zn1 125.9(5) . . ? C7 N2 C11 118.1(6) . . ? C7 N2 Zn2 117.0(5) . . ? C11 N2 Zn2 124.9(5) . . ? C16 N3 C12 117.5(6) . . ? C16 N3 Zn3 116.4(5) . . ? C12 N3 Zn3 126.0(5) . . ? C22 N4 C18 119.3(7) . . ? C22 N4 Zn4 124.4(6) . . ? C18 N4 Zn4 116.2(5) . . ? C27 N5 C23 118.4(7) . . ? C27 N5 Zn4 116.8(5) . . ? C23 N5 Zn4 124.7(6) . . ? C29 N6 C33 118.6(7) . . ? C29 N6 Zn3 116.7(5) . . ? C33 N6 Zn3 124.7(5) . . ? C38 N7 C34 118.6(6) . . ? C38 N7 Zn1 118.0(5) . . ? C34 N7 Zn1 123.3(5) . . ? C40 N8 C44 117.6(7) . . ? C40 N8 Zn2 115.4(5) . . ? C44 N8 Zn2 126.0(5) . . ? N1 C1 C2 123.3(8) . . ? C3 C2 C1 117.7(8) . . ? C2 C3 C4 121.0(8) . . ? C3 C4 C5 117.7(8) . . ? N1 C5 C4 121.7(7) . . ? N1 C5 C6 116.6(6) . . ? C4 C5 C6 121.7(7) . . ? O1 C6 O2 112.1(6) . . ? O1 C6 C7 110.5(6) . . ? O2 C6 C7 106.7(6) . . ? O1 C6 C5 108.5(6) . . ? O2 C6 C5 108.7(5) . . ? C7 C6 C5 110.3(6) . . ? N2 C7 C8 122.3(7) . . ? N2 C7 C6 115.1(6) . . ? C8 C7 C6 122.4(7) . . ? C9 C8 C7 118.1(7) . . ? C10 C9 C8 119.8(7) . . ? C9 C10 C11 119.0(7) . . ? N2 C11 C10 122.6(8) . . ? N3 C12 C13 123.1(8) . . ? C12 C13 C14 118.9(8) . . ? C13 C14 C15 119.3(8) . . ? C16 C15 C14 118.7(8) . . ? N3 C16 C15 122.3(7) . . ? N3 C16 C17 115.8(6) . . ? C15 C16 C17 121.9(7) . . ? O3 C17 O4 111.9(6) . . ? O3 C17 C16 109.7(6) . . ? O4 C17 C16 107.9(6) . . ? O3 C17 C18 109.9(6) . . ? O4 C17 C18 106.6(6) . . ? C16 C17 C18 110.8(6) . . ? N4 C18 C19 121.6(8) . . ? N4 C18 C17 114.8(6) . . ? C19 C18 C17 123.6(7) . . ? C18 C19 C20 119.3(9) . . ? C21 C20 C19 119.5(9) . . ? C20 C21 C22 117.5(9) . . ? N4 C22 C21 122.8(9) . . ? N5 C23 C24 122.2(8) . . ? C23 C24 C25 120.1(8) . . ? C24 C25 C26 117.7(8) . . ? C27 C26 C25 119.5(8) . . ? N5 C27 C26 122.1(7) . . ? N5 C27 C28 115.3(6) . . ? C26 C27 C28 122.6(7) . . ? O5 C28 O6 110.8(6) . . ? O5 C28 C29 110.4(6) . . ? O6 C28 C29 106.3(6) . . ? O5 C28 C27 110.0(6) . . ? O6 C28 C27 108.2(6) . . ? C29 C28 C27 110.9(6) . . ? N6 C29 C30 121.8(7) . . ? N6 C29 C28 114.9(6) . . ? C30 C29 C28 123.4(7) . . ? C31 C30 C29 119.2(8) . . ? C30 C31 C32 119.6(8) . . ? C33 C32 C31 118.5(8) . . ? N6 C33 C32 122.2(8) . . ? N7 C34 C35 122.2(7) . . ? C34 C35 C36 118.9(8) . . ? C37 C36 C35 119.2(8) . . ? C36 C37 C38 119.5(8) . . ? N7 C38 C37 121.4(7) . . ? N7 C38 C39 115.2(6) . . ? C37 C38 C39 123.4(6) . . ? O7 C39 O8 111.5(6) . . ? O7 C39 C38 110.1(5) . . ? O8 C39 C38 104.3(6) . . ? O7 C39 C40 110.6(6) . . ? O8 C39 C40 109.8(5) . . ? C38 C39 C40 110.4(6) . . ? N8 C40 C41 123.8(7) . . ? N8 C40 C39 115.3(6) . . ? C41 C40 C39 120.8(7) . . ? C40 C41 C42 116.7(8) . . ? C43 C42 C41 120.8(8) . . ? C42 C43 C44 117.8(8) . . ? N8 C44 C43 123.3(8) . . ? O10 C45 O9 123.6(7) . . ? O10 C45 C46 119.0(7) . . ? O9 C45 C46 117.3(7) . . ? O12 C47 O11 125.4(7) . . ? O12 C47 C48 119.2(7) . . ? O11 C47 C48 115.4(7) . . ? Zn4 O1W O3W 113.4(2) . . ? Zn4 O1W O2 81.58(18) . . ? O3W O1W O2 128.9(3) . . ? Zn3 O2W O5W 111.4(2) . . ? Zn3 O2W O8 81.09(18) . . ? O5W O2W O8 129.5(3) . . ? O1W O3W O4 91.7(2) . . ? O1W O3W O4W 131.2(3) . . ? O4 O3W O4W 116.5(3) . . ? O12 O4W O3W 107.5(3) 4_666 . ? O2W O5W O6 93.3(2) . . ? O15 Cl1 O16 109.3(6) . . ? O15 Cl1 O14 110.3(6) . . ? O16 Cl1 O14 107.8(5) . . ? O15 Cl1 O13 109.7(5) . . ? O16 Cl1 O13 109.1(5) . . ? O14 Cl1 O13 110.5(4) . . ? O17 Cl2 O19 111.9(6) . . ? O17 Cl2 O20 107.3(5) . . ? O19 Cl2 O20 109.4(5) . . ? O17 Cl2 O18 107.4(6) . . ? O19 Cl2 O18 109.5(5) . . ? O20 Cl2 O18 111.5(6) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.526 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.108 #=============================================END data_complex_5 _database_code_CSD 144516 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H49 Cd4 Cl N8 O20' _chemical_formula_weight 1567.02 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 '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 13.065(4) _cell_length_b 14.315(8) _cell_length_c 16.082(8) _cell_angle_alpha 90.53 _cell_angle_beta 108.10 _cell_angle_gamma 93.940(10) _cell_volume 2851(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 1.600 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_T_max 0.846 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 11227 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11210 _reflns_number_gt 7500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.1953P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11210 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.2674 _refine_ls_wR_factor_gt 0.2375 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.007 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.16175(4) -0.81636(4) 0.23702(3) 0.03165(13) Uani 1 d . . . Cd2 Cd 0.40057(4) -0.65839(4) 0.33501(3) 0.03334(13) Uani 1 d . . . Cd3 Cd 0.25905(4) -0.66053(4) 0.10827(3) 0.03312(13) Uani 1 d . . . Cd4 Cd 0.41595(4) -0.85469(4) 0.20692(4) 0.03804(14) Uani 1 d . . . O1 O 0.2206(4) -0.6609(3) 0.2363(3) 0.0320(12) Uani 1 d . . . O2 O 0.0738(4) -0.5728(4) 0.1868(3) 0.0375(13) Uani 1 d . . . H2 H 0.0275 -0.6309 0.1607 0.100 Uiso 1 d R . . O3 O 0.3512(4) -0.8147(3) 0.3159(3) 0.0298(11) Uani 1 d . . . O4 O 0.4773(4) -0.8935(4) 0.4198(4) 0.0449(15) Uani 1 d . . . H4 H 0.4919 -0.8473 0.3779 0.100 Uiso 1 d R . . O5 O 0.4252(4) -0.6845(4) 0.2038(3) 0.0330(12) Uani 1 d . . . O6 O 0.5386(4) -0.5492(4) 0.2133(3) 0.0464(15) Uani 1 d . . . H6 H 0.5455 -0.5234 0.2729 0.100 Uiso 1 d R . . O7 O 0.2387(4) -0.8185(3) 0.1303(3) 0.0336(12) Uani 1 d . . . O8 O 0.1574(5) -0.9582(4) 0.0632(4) 0.0507(17) Uani 1 d . . . H8 H 0.1768 -1.0014 0.1007 0.100 Uiso 1 d R . . O9 O -0.0065(5) -0.8662(4) 0.1715(5) 0.060(2) Uani 1 d . . . O10 O -0.0543(5) -0.7259(4) 0.1272(4) 0.0590(19) Uani 1 d . . . O11 O 0.5695(5) -0.5851(5) 0.3913(4) 0.0541(18) Uani 1 d . . . O12 O 0.6019(6) -0.7273(5) 0.4364(5) 0.071(2) Uani 1 d . . . O13 O 0.3191(6) -1.0190(6) 0.1949(5) 0.079(2) Uani 1 d . . . O14 O 0.4933(6) -1.0012(5) 0.2327(5) 0.078(2) Uani 1 d . . . O1W O 0.2041(5) -0.5105(4) 0.0847(4) 0.0544(17) Uani 1 d . . . H1WA H 0.1746 -0.4760 0.0362 0.100 Uiso 1 d R . . H1WB H 0.1608 -0.5041 0.1180 0.100 Uiso 1 d R . . O2W O -0.1673(5) -0.5673(5) 0.0714(4) 0.067(2) Uani 1 d . . . H2WA H -0.1687 -0.6324 0.0932 0.100 Uiso 1 d R . . H2WB H -0.1278 -0.5352 0.1256 0.100 Uiso 1 d R . . N1 N 0.1140(5) -0.7269(4) 0.3396(4) 0.0341(15) Uani 1 d . . . N2 N 0.3341(5) -0.5125(4) 0.3357(4) 0.0388(17) Uani 1 d . . . N3 N 0.1968(5) -0.9462(4) 0.3233(4) 0.0385(16) Uani 1 d . . . N4 N 0.3574(5) -0.7113(5) 0.4562(4) 0.0378(16) Uani 1 d . . . N5 N 0.3813(5) -0.6408(5) 0.0356(4) 0.0406(17) Uani 1 d . . . N6 N 0.5894(5) -0.7942(5) 0.2314(4) 0.0402(17) Uani 1 d . . . N7 N 0.1078(5) -0.7262(4) 0.0004(4) 0.0379(16) Uani 1 d . . . N8 N 0.3785(6) -0.8724(5) 0.0547(5) 0.0502(19) Uani 1 d . . . C1 C 0.0780(6) -0.7647(6) 0.4025(5) 0.045(2) Uani 1 d . . . H1A H 0.0784 -0.8312 0.4094 0.100 Uiso 1 d R . . C2 C 0.0438(6) -0.7111(6) 0.4583(5) 0.049(2) Uani 1 d . . . H2A H 0.0221 -0.7389 0.5049 0.100 Uiso 1 d R . . C3 C 0.0417(6) -0.6163(7) 0.4475(6) 0.051(2) Uani 1 d . . . H3A H 0.0150 -0.5782 0.4844 0.100 Uiso 1 d R . . C4 C 0.0777(6) -0.5771(6) 0.3825(6) 0.049(2) Uani 1 d . . . H4A H 0.0749 -0.5110 0.3736 0.100 Uiso 1 d R . . C5 C 0.1153(5) -0.6363(6) 0.3313(4) 0.0327(17) Uani 1 d . . . C6 C 0.1620(6) -0.5959(5) 0.2597(5) 0.0352(18) Uani 1 d . . . C7 C 0.2282(5) -0.5034(5) 0.2929(4) 0.0323(17) Uani 1 d . . . C8 C 0.1876(6) -0.4190(6) 0.2804(5) 0.042(2) Uani 1 d . . . H8A H 0.1128 -0.4139 0.2486 0.100 Uiso 1 d R . . C9 C 0.2557(7) -0.3387(5) 0.3112(5) 0.049(2) Uani 1 d . . . H9A H 0.2285 -0.2778 0.3019 0.100 Uiso 1 d R . . C10 C 0.3610(7) -0.3462(6) 0.3550(6) 0.053(3) Uani 1 d . . . H10A H 0.4094 -0.2918 0.3774 0.100 Uiso 1 d R . . C11 C 0.3959(7) -0.4351(6) 0.3672(6) 0.053(3) Uani 1 d . . . H11A H 0.4696 -0.4417 0.4011 0.100 Uiso 1 d R . . C12 C 0.1249(7) -1.0212(6) 0.3065(5) 0.048(2) Uani 1 d . . . H12A H 0.0550 -1.0162 0.2645 0.100 Uiso 1 d R . . C13 C 0.1470(9) -1.1041(6) 0.3492(7) 0.064(3) Uani 1 d . . . H13A H 0.0941 -1.1565 0.3393 0.100 Uiso 1 d R . . C14 C 0.2506(8) -1.1100(6) 0.4085(6) 0.054(3) Uani 1 d . . . H14A H 0.2681 -1.1651 0.4420 0.100 Uiso 1 d R . . C15 C 0.3254(7) -1.0330(6) 0.4205(5) 0.048(2) Uani 1 d . . . H15A H 0.3993 -1.0384 0.4549 0.100 Uiso 1 d R . . C16 C 0.2951(6) -0.9529(5) 0.3787(5) 0.0361(18) Uani 1 d . . . C17 C 0.3708(6) -0.8653(6) 0.3915(4) 0.0361(19) Uani 1 d . . . C18 C 0.3552(6) -0.8017(6) 0.4652(5) 0.0355(18) Uani 1 d . . . C19 C 0.3435(9) -0.8415(8) 0.5406(6) 0.068(3) Uani 1 d . . . H19A H 0.3473 -0.9077 0.5486 0.100 Uiso 1 d R . . C20 C 0.3275(9) -0.7812(9) 0.6032(6) 0.078(3) Uani 1 d . . . H20A H 0.3221 -0.8069 0.6568 0.100 Uiso 1 d R . . C21 C 0.3239(7) -0.6892(7) 0.5911(6) 0.056(3) Uani 1 d . . . H21A H 0.3066 -0.6489 0.6321 0.100 Uiso 1 d R . . C22 C 0.3420(7) -0.6556(7) 0.5178(5) 0.049(2) Uani 1 d . . . H22A H 0.3461 -0.5891 0.5101 0.100 Uiso 1 d R . . C23 C 0.3528(8) -0.6358(6) -0.0522(6) 0.053(2) Uani 1 d . . . H23A H 0.2778 -0.6430 -0.0861 0.100 Uiso 1 d R . . C24 C 0.4276(8) -0.6222(6) -0.0950(6) 0.060(3) Uani 1 d . . . H24A H 0.4045 -0.6173 -0.1575 0.100 Uiso 1 d R . . C25 C 0.5336(8) -0.6149(7) -0.0487(6) 0.061(3) Uani 1 d . . . H25A H 0.5855 -0.6045 -0.0794 0.100 Uiso 1 d R . . C26 C 0.5645(6) -0.6233(7) 0.0418(5) 0.049(2) Uani 1 d . . . H26A H 0.6396 -0.6178 0.0757 0.100 Uiso 1 d R . . C27 C 0.4850(7) -0.6363(6) 0.0811(5) 0.046(2) Uani 1 d . . . C28 C 0.5111(6) -0.6441(6) 0.1807(5) 0.0369(19) Uani 1 d . . . C29 C 0.6103(5) -0.7006(7) 0.2197(5) 0.045(2) Uani 1 d . . . C30 C 0.7114(6) -0.6587(7) 0.2387(6) 0.052(2) Uani 1 d . . . H30A H 0.7222 -0.5927 0.2311 0.100 Uiso 1 d R . . C31 C 0.7983(6) -0.7113(8) 0.2736(6) 0.061(3) Uani 1 d . . . H31A H 0.8718 -0.6857 0.2882 0.100 Uiso 1 d R . . C32 C 0.7795(7) -0.8049(8) 0.2836(9) 0.084(4) Uani 1 d . . . H32A H 0.8371 -0.8442 0.3090 0.100 Uiso 1 d R . . C33 C 0.6718(8) -0.8446(8) 0.2676(7) 0.074(4) Uani 1 d . . . H33A H 0.6598 -0.9109 0.2728 0.100 Uiso 1 d R . . C34 C 0.0224(7) -0.6812(7) -0.0457(6) 0.054(3) Uani 1 d . . . H34A H 0.0287 -0.6140 -0.0409 0.100 Uiso 1 d R . . C35 C -0.0698(8) -0.7259(8) -0.0984(6) 0.068(3) Uani 1 d . . . H35A H -0.1308 -0.6920 -0.1283 0.100 Uiso 1 d R . . C36 C -0.0798(9) -0.8197(7) -0.1043(6) 0.077(4) Uani 1 d . . . H36A H -0.1409 -0.8528 -0.1460 0.100 Uiso 1 d R . . C37 C 0.0072(8) -0.8687(7) -0.0563(6) 0.061(3) Uani 1 d . . . H37A H -0.0012 -0.9358 -0.0561 0.100 Uiso 1 d R . . C38 C 0.0958(6) -0.8197(5) -0.0057(4) 0.0373(19) Uani 1 d . . . C39 C 0.1946(6) -0.8676(5) 0.0515(5) 0.0360(18) Uani 1 d . . . C40 C 0.2803(7) -0.8737(6) 0.0053(5) 0.046(2) Uani 1 d . . . C41 C 0.2498(9) -0.8825(8) -0.0853(6) 0.070(3) Uani 1 d . . . H41A H 0.1755 -0.8822 -0.1207 0.100 Uiso 1 d R . . C42 C 0.3380(10) -0.8931(9) -0.1195(6) 0.084(4) Uani 1 d . . . H42A H 0.3204 -0.8997 -0.1820 0.100 Uiso 1 d R . . C43 C 0.4370(10) -0.8956(9) -0.0708(7) 0.084(4) Uani 1 d . . . H43A H 0.4936 -0.9054 -0.0955 0.100 Uiso 1 d R . . C44 C 0.4559(8) -0.8832(7) 0.0197(7) 0.067(3) Uani 1 d . . . H44A H 0.5284 -0.8812 0.0590 0.100 Uiso 1 d R . . C45 C -0.0739(6) -0.8110(6) 0.1280(5) 0.042(2) Uani 1 d . . . C46 C -0.1862(7) -0.8518(7) 0.0798(6) 0.057(3) Uani 1 d . . . H46A H -0.2287 -0.8037 0.0484 0.100 Uiso 1 d R . . H46B H -0.1822 -0.9000 0.0392 0.100 Uiso 1 d R . . H46C H -0.2192 -0.8781 0.1208 0.100 Uiso 1 d R . . C47 C 0.6325(6) -0.6456(6) 0.4283(5) 0.043(2) Uani 1 d . . . C48 C 0.7491(7) -0.6115(8) 0.4654(6) 0.063(3) Uani 1 d . . . H48A H 0.7891 -0.6637 0.4903 0.100 Uiso 1 d R . . H48B H 0.7759 -0.5859 0.4205 0.100 Uiso 1 d R . . H48C H 0.7572 -0.5643 0.5103 0.100 Uiso 1 d R . . C49 C 0.4110(7) -1.0487(6) 0.2186(5) 0.052(2) Uani 1 d . . . C50 C 0.4130(10) -1.1539(7) 0.2301(10) 0.104(5) Uani 1 d . . . H50A H 0.4859 -1.1718 0.2493 0.100 Uiso 1 d R . . H50B H 0.3779 -1.1719 0.2724 0.100 Uiso 1 d R . . H50C H 0.3747 -1.1846 0.1747 0.100 Uiso 1 d R . . Cl1 Cl -0.1107(2) -0.3636(2) 0.28010(16) 0.0726(8) Uani 1 d . . . O15 O -0.1006(8) -0.4094(8) 0.2085(6) 0.118(4) Uani 1 d . . . O16 O -0.1590(11) -0.4327(10) 0.3227(9) 0.174(6) Uani 1 d . . . O17 O -0.1795(10) -0.2987(10) 0.2607(8) 0.177(5) Uani 1 d . . . O18 O -0.0117(7) -0.3376(8) 0.3401(7) 0.120(4) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0338(2) 0.0258(2) 0.0338(2) 0.0021(2) 0.0081(2) 0.0034(2) Cd2 0.0336(2) 0.0296(3) 0.0329(2) 0.0005(2) 0.0046(2) 0.0031(2) Cd3 0.0345(2) 0.0291(3) 0.0322(2) 0.0034(2) 0.0056(2) 0.0007(2) Cd4 0.0392(3) 0.0347(3) 0.0417(3) 0.0014(2) 0.0135(2) 0.0086(2) O1 0.037(2) 0.025(2) 0.034(2) -0.0001(19) 0.0101(19) 0.010(2) O2 0.030(2) 0.033(3) 0.039(3) 0.001(2) -0.006(2) 0.004(2) O3 0.041(2) 0.027(2) 0.024(2) 0.0046(18) 0.0130(18) 0.010(2) O4 0.036(2) 0.046(3) 0.055(3) 0.020(2) 0.015(2) 0.015(2) O5 0.031(2) 0.037(3) 0.032(2) 0.001(2) 0.0111(19) 0.006(2) O6 0.053(3) 0.045(3) 0.037(3) -0.008(2) 0.010(2) -0.012(3) O7 0.034(2) 0.032(3) 0.030(2) -0.002(2) 0.0047(19) 0.000(2) O8 0.068(4) 0.030(3) 0.049(3) 0.001(2) 0.012(3) -0.007(3) O9 0.037(3) 0.047(3) 0.083(4) -0.006(3) 0.001(3) -0.003(3) O10 0.062(4) 0.048(4) 0.055(4) -0.003(3) 0.002(3) -0.002(3) O11 0.043(3) 0.060(4) 0.050(3) 0.000(3) 0.002(3) 0.004(3) O12 0.070(4) 0.055(4) 0.080(5) -0.006(4) 0.016(4) -0.011(3) O13 0.079(4) 0.086(5) 0.078(5) 0.020(4) 0.022(4) 0.045(4) O14 0.087(5) 0.055(4) 0.102(5) 0.003(4) 0.045(4) -0.002(4) O1W 0.068(4) 0.046(3) 0.050(3) 0.013(3) 0.017(3) 0.013(3) O2W 0.054(4) 0.075(4) 0.065(4) 0.031(3) 0.005(3) 0.013(3) N1 0.036(3) 0.035(3) 0.028(3) -0.002(2) 0.006(2) 0.005(3) N2 0.035(3) 0.032(3) 0.047(3) -0.003(3) 0.009(3) -0.002(3) N3 0.042(3) 0.031(3) 0.038(3) 0.005(3) 0.005(3) 0.012(3) N4 0.043(3) 0.040(3) 0.031(3) -0.006(3) 0.011(2) 0.009(3) N5 0.044(3) 0.039(4) 0.035(3) 0.006(3) 0.009(3) -0.007(3) N6 0.043(3) 0.035(3) 0.040(3) -0.004(3) 0.008(3) 0.010(3) N7 0.049(3) 0.025(3) 0.035(3) 0.005(2) 0.005(3) 0.003(3) N8 0.056(4) 0.044(4) 0.057(4) -0.007(3) 0.026(3) 0.006(3) C1 0.042(4) 0.051(5) 0.039(4) 0.000(4) 0.010(3) 0.001(4) C2 0.047(4) 0.054(5) 0.049(4) -0.003(4) 0.022(3) -0.015(4) C3 0.045(4) 0.058(5) 0.057(4) -0.008(4) 0.027(3) 0.003(4) C4 0.044(4) 0.038(4) 0.066(5) -0.009(4) 0.019(4) 0.004(4) C5 0.019(3) 0.051(4) 0.027(3) -0.004(3) 0.003(2) 0.015(3) C6 0.033(3) 0.031(4) 0.040(4) 0.001(3) 0.007(3) 0.011(3) C7 0.033(3) 0.031(4) 0.034(3) 0.001(3) 0.012(3) 0.001(3) C8 0.033(3) 0.043(4) 0.045(4) -0.007(3) 0.008(3) -0.001(3) C9 0.071(5) 0.024(4) 0.046(4) -0.008(3) 0.009(4) -0.001(4) C10 0.059(5) 0.034(4) 0.054(5) -0.009(4) 0.003(4) -0.009(4) C11 0.047(4) 0.037(4) 0.062(5) -0.006(4) -0.001(4) -0.005(4) C12 0.060(5) 0.031(4) 0.048(4) -0.003(3) 0.010(4) -0.006(4) C13 0.079(6) 0.029(4) 0.085(7) 0.008(4) 0.024(5) 0.015(4) C14 0.070(5) 0.029(4) 0.055(5) 0.007(4) 0.008(4) 0.011(4) C15 0.057(5) 0.033(4) 0.049(4) 0.012(3) 0.010(4) 0.010(4) C16 0.040(4) 0.033(4) 0.036(4) 0.002(3) 0.013(3) 0.005(3) C17 0.035(3) 0.046(4) 0.025(3) 0.006(3) 0.005(3) 0.009(3) C18 0.029(3) 0.047(4) 0.030(3) 0.003(3) 0.007(3) 0.003(3) C19 0.091(7) 0.075(7) 0.035(4) 0.000(4) 0.023(4) -0.020(6) C20 0.102(7) 0.096(9) 0.048(5) -0.007(5) 0.045(5) -0.018(7) C21 0.049(4) 0.069(6) 0.051(5) -0.018(4) 0.021(4) -0.001(4) C22 0.040(4) 0.057(5) 0.044(4) -0.008(4) 0.003(3) 0.006(4) C23 0.059(5) 0.048(5) 0.047(4) 0.015(4) 0.012(4) -0.004(4) C24 0.091(6) 0.045(5) 0.043(4) 0.013(4) 0.022(4) -0.015(5) C25 0.072(5) 0.063(6) 0.056(5) 0.007(4) 0.037(4) -0.008(5) C26 0.041(4) 0.068(6) 0.044(4) 0.002(4) 0.022(3) -0.001(4) C27 0.064(5) 0.034(4) 0.037(4) 0.001(3) 0.010(4) 0.005(4) C28 0.028(3) 0.044(4) 0.037(4) 0.003(3) 0.007(3) -0.003(3) C29 0.011(3) 0.078(6) 0.046(4) -0.002(4) 0.009(3) 0.002(3) C30 0.031(4) 0.075(6) 0.047(4) 0.002(4) 0.010(3) 0.000(4) C31 0.024(3) 0.094(7) 0.065(5) -0.008(5) 0.015(4) 0.005(4) C32 0.033(4) 0.069(7) 0.145(11) 0.019(7) 0.013(6) 0.025(5) C33 0.056(6) 0.075(7) 0.075(7) 0.019(6) -0.008(5) 0.024(5) C34 0.061(5) 0.049(5) 0.044(4) 0.003(4) 0.006(4) -0.001(4) C35 0.050(5) 0.081(7) 0.055(5) 0.030(5) -0.011(4) 0.001(5) C36 0.085(7) 0.069(6) 0.040(5) 0.023(4) -0.029(5) -0.033(5) C37 0.063(5) 0.068(6) 0.038(4) 0.012(4) 0.002(4) -0.020(5) C38 0.054(4) 0.025(3) 0.027(3) -0.005(3) 0.006(3) -0.007(3) C39 0.048(4) 0.028(4) 0.031(3) -0.001(3) 0.012(3) -0.005(3) C40 0.067(5) 0.037(4) 0.036(4) -0.003(3) 0.022(3) 0.002(4) C41 0.092(7) 0.071(7) 0.046(5) -0.009(5) 0.019(5) 0.002(6) C42 0.127(8) 0.094(9) 0.044(5) -0.010(5) 0.047(5) 0.001(7) C43 0.110(7) 0.092(8) 0.074(6) 0.018(6) 0.056(5) 0.032(7) C44 0.084(6) 0.060(6) 0.076(6) 0.012(5) 0.049(5) 0.017(5) C45 0.029(3) 0.044(4) 0.053(4) -0.008(4) 0.014(3) -0.008(3) C46 0.052(5) 0.061(6) 0.051(5) -0.008(4) 0.008(4) 0.003(4) C47 0.040(4) 0.041(4) 0.040(4) -0.009(3) 0.000(3) 0.000(4) C48 0.030(4) 0.094(8) 0.056(5) -0.007(5) 0.002(4) -0.003(5) C49 0.072(5) 0.050(5) 0.049(4) 0.012(4) 0.037(4) 0.016(4) C50 0.088(7) 0.040(5) 0.199(14) 0.041(7) 0.061(8) 0.022(5) Cl1 0.0635(13) 0.106(2) 0.0507(12) -0.0037(13) 0.0161(10) 0.0307(14) O15 0.124(6) 0.164(9) 0.070(5) -0.028(5) 0.028(5) 0.045(7) O16 0.190(10) 0.157(12) 0.205(11) -0.003(9) 0.118(9) -0.047(9) O17 0.172(8) 0.241(12) 0.123(9) 0.013(9) 0.025(7) 0.145(8) O18 0.086(6) 0.138(8) 0.113(7) -0.051(6) -0.004(5) 0.025(6) _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 Cd1 O9 2.187(6) . ? Cd1 O7 2.243(5) . ? Cd1 O1 2.306(5) . ? Cd1 N3 2.316(6) . ? Cd1 N1 2.337(6) . ? Cd1 O3 2.404(5) . ? Cd2 O5 2.263(5) . ? Cd2 O3 2.276(5) . ? Cd2 O11 2.283(6) . ? Cd2 N4 2.311(7) . ? Cd2 N2 2.318(7) . ? Cd2 O1 2.391(4) . ? Cd3 N5 2.258(7) . ? Cd3 O1 2.266(5) . ? Cd3 O5 2.286(4) . ? Cd3 O7 2.303(5) . ? Cd3 O1W 2.308(6) . ? Cd3 N7 2.320(6) . ? Cd4 O3 2.254(5) . ? Cd4 N6 2.283(7) . ? Cd4 N8 2.350(7) . ? Cd4 O7 2.356(5) . ? Cd4 O14 2.374(8) . ? Cd4 O5 2.433(5) . ? Cd4 O13 2.569(8) . ? O1 C6 1.365(9) . ? O2 C6 1.425(8) . ? O2 O10 2.642(8) . ? O2 O1W 2.820(9) . ? O2 O2W 3.127(7) . ? O3 C17 1.385(8) . ? O4 C17 1.411(9) . ? O4 O12 2.752(9) . ? O5 C28 1.381(9) . ? O6 C28 1.432(9) . ? O6 O11 2.822(8) . ? O7 C39 1.381(8) . ? O8 C39 1.388(9) . ? O8 O13 2.685(9) . ? O9 C45 1.270(10) . ? O10 C45 1.230(10) . ? O10 O2W 2.795(9) . ? O11 C47 1.258(10) . ? O12 C47 1.231(11) . ? O13 C49 1.247(11) . ? O14 C49 1.191(11) . ? O1W O2W 2.674(9) 2_545 ? O2W O15 3.028(12) . ? N1 C5 1.304(10) . ? N1 C1 1.345(11) . ? N2 C11 1.323(10) . ? N2 C7 1.356(9) . ? N3 C16 1.327(9) . ? N3 C12 1.344(10) . ? N4 C18 1.302(10) . ? N4 C22 1.339(11) . ? N5 C27 1.322(10) . ? N5 C23 1.347(11) . ? N6 C33 1.321(11) . ? N6 C29 1.375(12) . ? N7 C38 1.335(9) . ? N7 C34 1.344(11) . ? N8 C40 1.281(10) . ? N8 C44 1.319(13) . ? C1 C2 1.370(12) . ? C2 C3 1.370(13) . ? C3 C4 1.380(13) . ? C4 C5 1.391(11) . ? C5 C6 1.560(11) . ? C6 C7 1.527(10) . ? C7 C8 1.344(11) . ? C8 C9 1.390(11) . ? C9 C10 1.349(12) . ? C10 C11 1.376(13) . ? C12 C13 1.380(12) . ? C13 C14 1.401(13) . ? C14 C15 1.392(12) . ? C15 C16 1.354(11) . ? C16 C17 1.514(11) . ? C17 C18 1.560(11) . ? C18 C19 1.390(12) . ? C19 C20 1.394(15) . ? C20 C21 1.336(16) . ? C21 C22 1.357(13) . ? C23 C24 1.364(14) . ? C24 C25 1.350(13) . ? C25 C26 1.393(12) . ? C26 C27 1.376(13) . ? C27 C28 1.537(11) . ? C28 C29 1.540(11) . ? C29 C30 1.355(11) . ? C30 C31 1.378(13) . ? C31 C32 1.365(16) . ? C32 C33 1.425(14) . ? C34 C35 1.352(12) . ? C35 C36 1.341(15) . ? C36 C37 1.398(14) . ? C37 C38 1.337(11) . ? C38 C39 1.542(10) . ? C39 C40 1.531(12) . ? C40 C41 1.387(12) . ? C41 C42 1.440(17) . ? C42 C43 1.290(16) . ? C43 C44 1.405(15) . ? C45 C46 1.504(11) . ? C47 C48 1.498(11) . ? C49 C50 1.520(13) . ? Cl1 O17 1.309(12) . ? Cl1 O15 1.366(9) . ? Cl1 O18 1.377(9) . ? Cl1 O16 1.429(14) . ? 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 O9 Cd1 O7 104.1(2) . . ? O9 Cd1 O1 121.4(2) . . ? O7 Cd1 O1 78.62(18) . . ? O9 Cd1 N3 93.5(2) . . ? O7 Cd1 N3 112.1(2) . . ? O1 Cd1 N3 140.71(18) . . ? O9 Cd1 N1 91.9(2) . . ? O7 Cd1 N1 147.4(2) . . ? O1 Cd1 N1 68.8(2) . . ? N3 Cd1 N1 94.8(2) . . ? O9 Cd1 O3 161.5(2) . . ? O7 Cd1 O3 76.69(16) . . ? O1 Cd1 O3 77.05(16) . . ? N3 Cd1 O3 69.62(19) . . ? N1 Cd1 O3 96.94(18) . . ? O5 Cd2 O3 80.23(17) . . ? O5 Cd2 O11 92.0(2) . . ? O3 Cd2 O11 128.7(2) . . ? O5 Cd2 N4 151.2(2) . . ? O3 Cd2 N4 70.99(19) . . ? O11 Cd2 N4 104.4(2) . . ? O5 Cd2 N2 108.7(2) . . ? O3 Cd2 N2 143.33(19) . . ? O11 Cd2 N2 87.3(2) . . ? N4 Cd2 N2 95.8(2) . . ? O5 Cd2 O1 77.63(17) . . ? O3 Cd2 O1 77.86(16) . . ? O11 Cd2 O1 149.9(2) . . ? N4 Cd2 O1 97.59(19) . . ? N2 Cd2 O1 69.99(18) . . ? N5 Cd3 O1 149.51(19) . . ? N5 Cd3 O5 72.1(2) . . ? O1 Cd3 O5 79.76(17) . . ? N5 Cd3 O7 107.0(2) . . ? O1 Cd3 O7 78.22(18) . . ? O5 Cd3 O7 79.10(17) . . ? N5 Cd3 O1W 94.0(2) . . ? O1 Cd3 O1W 90.0(2) . . ? O5 Cd3 O1W 120.09(19) . . ? O7 Cd3 O1W 155.6(2) . . ? N5 Cd3 N7 102.3(2) . . ? O1 Cd3 N7 107.7(2) . . ? O5 Cd3 N7 146.4(2) . . ? O7 Cd3 N7 70.84(18) . . ? O1W Cd3 N7 93.1(2) . . ? O3 Cd4 N6 111.8(2) . . ? O3 Cd4 N8 145.7(2) . . ? N6 Cd4 N8 94.5(2) . . ? O3 Cd4 O7 77.46(17) . . ? N6 Cd4 O7 139.2(2) . . ? N8 Cd4 O7 68.2(2) . . ? O3 Cd4 O14 110.8(2) . . ? N6 Cd4 O14 84.8(2) . . ? N8 Cd4 O14 92.5(3) . . ? O7 Cd4 O14 130.7(2) . . ? O3 Cd4 O5 77.11(17) . . ? N6 Cd4 O5 69.01(19) . . ? N8 Cd4 O5 93.3(2) . . ? O7 Cd4 O5 75.18(16) . . ? O14 Cd4 O5 153.5(2) . . ? O3 Cd4 O13 90.3(2) . . ? N6 Cd4 O13 136.3(2) . . ? N8 Cd4 O13 84.8(2) . . ? O7 Cd4 O13 80.8(2) . . ? O14 Cd4 O13 51.7(2) . . ? O5 Cd4 O13 154.7(2) . . ? C6 O1 Cd3 123.7(4) . . ? C6 O1 Cd1 117.4(4) . . ? Cd3 O1 Cd1 99.69(18) . . ? C6 O1 Cd2 112.1(4) . . ? Cd3 O1 Cd2 98.83(19) . . ? Cd1 O1 Cd2 101.55(17) . . ? C6 O2 O10 108.9(4) . . ? C6 O2 O1W 94.7(4) . . ? O10 O2 O1W 115.8(3) . . ? C6 O2 O2W 157.1(5) . . ? O10 O2 O2W 57.2(2) . . ? O1W O2 O2W 107.6(2) . . ? C17 O3 Cd4 121.5(4) . . ? C17 O3 Cd2 115.9(4) . . ? Cd4 O3 Cd2 102.07(19) . . ? C17 O3 Cd1 112.1(4) . . ? Cd4 O3 Cd1 100.38(16) . . ? Cd2 O3 Cd1 102.04(18) . . ? C17 O4 O12 103.2(5) . . ? C28 O5 Cd2 123.6(4) . . ? C28 O5 Cd3 114.6(4) . . ? Cd2 O5 Cd3 102.10(19) . . ? C28 O5 Cd4 114.8(4) . . ? Cd2 O5 Cd4 97.13(19) . . ? Cd3 O5 Cd4 101.09(17) . . ? C28 O6 O11 97.2(4) . . ? C39 O7 Cd1 124.2(4) . . ? C39 O7 Cd3 110.7(4) . . ? Cd1 O7 Cd3 100.5(2) . . ? C39 O7 Cd4 113.7(4) . . ? Cd1 O7 Cd4 102.17(18) . . ? Cd3 O7 Cd4 102.97(18) . . ? C39 O8 O13 103.7(4) . . ? C45 O9 Cd1 120.8(5) . . ? C45 O10 O2 150.5(5) . . ? C45 O10 O2W 138.2(5) . . ? O2 O10 O2W 70.1(2) . . ? C47 O11 Cd2 107.8(5) . . ? C47 O11 O6 119.6(6) . . ? Cd2 O11 O6 82.0(2) . . ? C47 O12 O4 162.8(6) . . ? C49 O13 Cd4 86.4(6) . . ? C49 O13 O8 147.3(7) . . ? Cd4 O13 O8 88.1(3) . . ? C49 O14 Cd4 97.0(6) . . ? Cd3 O1W O2W 121.8(3) . 2_545 ? Cd3 O1W O2 81.3(2) . . ? O2W O1W O2 134.9(3) 2_545 . ? O10 O2W O15 112.1(3) . . ? O10 O2W O2 52.62(19) . . ? O15 O2W O2 68.5(2) . . ? C5 N1 C1 118.6(7) . . ? C5 N1 Cd1 118.0(5) . . ? C1 N1 Cd1 123.2(5) . . ? C11 N2 C7 117.4(7) . . ? C11 N2 Cd2 123.5(5) . . ? C7 N2 Cd2 118.6(5) . . ? C16 N3 C12 119.6(7) . . ? C16 N3 Cd1 119.3(5) . . ? C12 N3 Cd1 120.0(5) . . ? C18 N4 C22 119.9(7) . . ? C18 N4 Cd2 115.5(5) . . ? C22 N4 Cd2 124.4(6) . . ? C27 N5 C23 118.8(8) . . ? C27 N5 Cd3 118.4(5) . . ? C23 N5 Cd3 122.8(6) . . ? C33 N6 C29 118.4(7) . . ? C33 N6 Cd4 120.9(6) . . ? C29 N6 Cd4 120.1(5) . . ? C38 N7 C34 116.1(7) . . ? C38 N7 Cd3 116.4(5) . . ? C34 N7 Cd3 126.3(5) . . ? C40 N8 C44 119.6(8) . . ? C40 N8 Cd4 119.0(6) . . ? C44 N8 Cd4 121.4(6) . . ? N1 C1 C2 122.1(8) . . ? C1 C2 C3 119.1(8) . . ? C2 C3 C4 119.0(8) . . ? C3 C4 C5 118.0(8) . . ? N1 C5 C4 123.0(7) . . ? N1 C5 C6 116.4(6) . . ? C4 C5 C6 120.5(7) . . ? O1 C6 O2 111.3(6) . . ? O1 C6 C7 112.7(6) . . ? O2 C6 C7 105.5(6) . . ? O1 C6 C5 109.4(6) . . ? O2 C6 C5 108.0(6) . . ? C7 C6 C5 109.8(6) . . ? C8 C7 N2 121.7(6) . . ? C8 C7 C6 124.0(6) . . ? N2 C7 C6 114.2(6) . . ? C7 C8 C9 119.4(7) . . ? C10 C9 C8 119.9(8) . . ? C9 C10 C11 117.3(8) . . ? N2 C11 C10 124.2(8) . . ? N3 C12 C13 122.3(8) . . ? C12 C13 C14 117.5(9) . . ? C15 C14 C13 118.8(8) . . ? C16 C15 C14 119.6(8) . . ? N3 C16 C15 122.0(7) . . ? N3 C16 C17 115.5(6) . . ? C15 C16 C17 122.5(7) . . ? O3 C17 O4 111.8(6) . . ? O3 C17 C16 111.9(5) . . ? O4 C17 C16 107.3(6) . . ? O3 C17 C18 108.5(6) . . ? O4 C17 C18 108.2(5) . . ? C16 C17 C18 109.1(6) . . ? N4 C18 C19 121.1(8) . . ? N4 C18 C17 118.9(7) . . ? C19 C18 C17 119.9(8) . . ? C18 C19 C20 117.2(10) . . ? C21 C20 C19 121.1(10) . . ? C20 C21 C22 117.8(9) . . ? N4 C22 C21 122.6(9) . . ? N5 C23 C24 122.0(8) . . ? C25 C24 C23 119.4(9) . . ? C24 C25 C26 119.2(9) . . ? C27 C26 C25 118.4(8) . . ? N5 C27 C26 122.0(7) . . ? N5 C27 C28 115.8(8) . . ? C26 C27 C28 122.2(7) . . ? O5 C28 O6 111.8(6) . . ? O5 C28 C27 112.4(6) . . ? O6 C28 C27 103.8(6) . . ? O5 C28 C29 108.9(6) . . ? O6 C28 C29 108.3(6) . . ? C27 C28 C29 111.5(7) . . ? C30 C29 N6 123.2(8) . . ? C30 C29 C28 120.4(9) . . ? N6 C29 C28 116.3(6) . . ? C29 C30 C31 118.9(10) . . ? C32 C31 C30 118.8(8) . . ? C31 C32 C33 120.1(9) . . ? N6 C33 C32 120.0(10) . . ? N7 C34 C35 123.2(9) . . ? C36 C35 C34 119.8(9) . . ? C35 C36 C37 118.4(9) . . ? C38 C37 C36 118.4(9) . . ? N7 C38 C37 124.1(8) . . ? N7 C38 C39 113.8(6) . . ? C37 C38 C39 122.1(7) . . ? O7 C39 O8 111.6(6) . . ? O7 C39 C40 109.6(6) . . ? O8 C39 C40 108.1(6) . . ? O7 C39 C38 109.8(6) . . ? O8 C39 C38 106.4(6) . . ? C40 C39 C38 111.2(6) . . ? N8 C40 C41 123.5(9) . . ? N8 C40 C39 116.3(7) . . ? C41 C40 C39 120.2(8) . . ? C40 C41 C42 114.2(9) . . ? C43 C42 C41 123.4(10) . . ? C42 C43 C44 116.0(12) . . ? N8 C44 C43 123.3(10) . . ? O10 C45 O9 123.7(7) . . ? O10 C45 C46 118.4(8) . . ? O9 C45 C46 117.8(8) . . ? O12 C47 O11 123.4(8) . . ? O12 C47 C48 120.9(8) . . ? O11 C47 C48 115.7(8) . . ? O14 C49 O13 124.9(9) . . ? O14 C49 C50 120.1(9) . . ? O13 C49 C50 115.0(9) . . ? O17 Cl1 O15 113.7(7) . . ? O17 Cl1 O18 116.0(8) . . ? O15 Cl1 O18 111.7(6) . . ? O17 Cl1 O16 104.4(9) . . ? O15 Cl1 O16 104.9(8) . . ? O18 Cl1 O16 104.7(7) . . ? Cl1 O15 O2W 151.3(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.161 _refine_diff_density_min -1.896 _refine_diff_density_rms 0.266 #========================================END data_complex_6 _database_code_CSD 144519 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H63.50 Cl N8 Ni4 O27.25' _chemical_formula_weight 1481.87 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.943(3) _cell_length_b 24.582(8) _cell_length_c 21.892(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.60(1) _cell_angle_gamma 90.00 _cell_volume 6317(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour green _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3062 _exptl_absorpt_coefficient_mu 1.305 _exptl_absorpt_correction_type SEMI-EMPIRICAL _exptl_absorpt_correction_T_min 0.559 _exptl_absorpt_correction_T_max 0.683 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 120 _diffrn_standards_decay_% none _diffrn_reflns_number 11686 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11116 _reflns_number_gt 6402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.1174P)^2^+8.3065P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11116 _refine_ls_number_parameters 830 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.1391 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.2259 _refine_ls_wR_factor_gt 0.1875 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.111 _refine_ls_shift/su_mean 0.007 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.24953(7) 0.27264(3) 0.52263(4) 0.0394(2) Uani 1 d . . . Ni2 Ni 0.48626(7) 0.23764(3) 0.52578(4) 0.0365(2) Uani 1 d . . . Ni3 Ni 0.28175(7) 0.15531(3) 0.46858(4) 0.0350(2) Uani 1 d . . . Ni4 Ni 0.33051(7) 0.25141(3) 0.39168(4) 0.0365(2) Uani 1 d . . . O1 O 0.2045(3) 0.22880(16) 0.4358(2) 0.0347(10) Uani 1 d . . . O2 O 0.0320(4) 0.26612(18) 0.3906(2) 0.0504(13) Uani 1 d . . . H2 H 0.0733 0.2965 0.4206 0.080 Uiso 1 d R . . O3 O 0.4216(3) 0.18903(16) 0.44487(18) 0.0334(10) Uani 1 d . . . O4 O 0.5654(4) 0.12703(17) 0.4441(2) 0.0414(11) Uani 1 d . . . H4 H 0.5864 0.1490 0.4790 0.080 Uiso 1 d R . . O5 O 0.3794(3) 0.29160(15) 0.47526(19) 0.0342(10) Uani 1 d . . . O6 O 0.4319(4) 0.37821(17) 0.5124(2) 0.0492(13) Uani 1 d . . . H6 H 0.3449 0.3817 0.5180 0.080 Uiso 1 d R . . O7 O 0.3384(3) 0.20342(16) 0.54553(19) 0.0351(10) Uani 1 d . . . O8 O 0.3808(4) 0.19682(18) 0.6541(2) 0.0461(12) Uani 1 d . . . H8 H 0.4705 0.1833 0.6533 0.080 Uiso 1 d R . . O9 O 0.5070(4) 0.28359(18) 0.6024(2) 0.0462(12) Uani 1 d . . . O10 O 0.3282(4) 0.31224(19) 0.5985(2) 0.0502(13) Uani 1 d . . . O11 O 0.5995(4) 0.17788(19) 0.5537(2) 0.0477(13) Uani 1 d . . . O12 O 0.5958(4) 0.1621(2) 0.6521(2) 0.0599(15) Uani 1 d . . . O13 O 0.1326(4) 0.32796(18) 0.4868(2) 0.0535(14) Uani 1 d . . . O14 O 0.2160(4) 0.4074(2) 0.5089(3) 0.0778(19) Uani 1 d . . . N1 N 0.2169(5) 0.2163(2) 0.3205(3) 0.0449(15) Uani 1 d . . . N2 N 0.1104(4) 0.1388(2) 0.4648(2) 0.0417(14) Uani 1 d . . . N3 N 0.4718(4) 0.2424(2) 0.3513(3) 0.0415(14) Uani 1 d . . . N4 N 0.2993(4) 0.1105(2) 0.3921(3) 0.0413(14) Uani 1 d . . . N5 N 0.2980(5) 0.3293(2) 0.3663(3) 0.0466(15) Uani 1 d . . . N6 N 0.5967(4) 0.2854(2) 0.4865(3) 0.0421(14) Uani 1 d . . . N7 N 0.1465(4) 0.2318(2) 0.5728(3) 0.0432(15) Uani 1 d . . . N8 N 0.3375(5) 0.0985(2) 0.5344(3) 0.0441(15) Uani 1 d . . . C1 C 0.2341(7) 0.2065(3) 0.2628(4) 0.057(2) Uani 1 d . . . H1A H 0.3056 0.2176 0.2527 0.080 Uiso 1 d R . . C2 C 0.1558(7) 0.1830(4) 0.2177(4) 0.070(3) Uani 1 d . . . H2A H 0.1721 0.1768 0.1769 0.080 Uiso 1 d R . . C3 C 0.0537(8) 0.1692(4) 0.2327(4) 0.074(3) Uani 1 d . . . H3A H -0.0031 0.1521 0.2020 0.080 Uiso 1 d R . . C4 C 0.0334(6) 0.1781(3) 0.2916(4) 0.060(2) Uani 1 d . . . H4A H -0.0380 0.1681 0.3026 0.080 Uiso 1 d R . . C5 C 0.1169(6) 0.2027(3) 0.3342(3) 0.0437(18) Uani 1 d . . . C6 C 0.1003(5) 0.2191(3) 0.3990(3) 0.0421(18) Uani 1 d . . . C7 C 0.0401(6) 0.1752(3) 0.4294(3) 0.0442(18) Uani 1 d . . . C8 C -0.0752(6) 0.1721(3) 0.4250(4) 0.056(2) Uani 1 d . . . H8A H -0.1229 0.1982 0.4000 0.080 Uiso 1 d R . . C9 C -0.1202(7) 0.1318(4) 0.4549(4) 0.072(3) Uani 1 d . . . H9A H -0.2011 0.1293 0.4525 0.080 Uiso 1 d R . . C10 C -0.0515(7) 0.0958(3) 0.4898(4) 0.064(2) Uani 1 d . . . H10A H -0.0824 0.0668 0.5110 0.080 Uiso 1 d R . . C11 C 0.0634(6) 0.1001(3) 0.4934(3) 0.051(2) Uani 1 d . . . H11A H 0.1134 0.0747 0.5183 0.080 Uiso 1 d R . . C12 C 0.5108(6) 0.2771(3) 0.3126(3) 0.0508(19) Uani 1 d . . . H12A H 0.4685 0.3099 0.3010 0.080 Uiso 1 d R . . C13 C 0.6080(6) 0.2670(3) 0.2894(3) 0.058(2) Uani 1 d . . . H13A H 0.6352 0.2935 0.2634 0.080 Uiso 1 d R . . C14 C 0.6655(6) 0.2200(3) 0.3043(4) 0.057(2) Uani 1 d . . . H14A H 0.7318 0.2117 0.2870 0.080 Uiso 1 d R . . C15 C 0.6258(6) 0.1835(3) 0.3437(3) 0.0496(19) Uani 1 d . . . H15A H 0.6649 0.1500 0.3556 0.080 Uiso 1 d R . . C16 C 0.5296(5) 0.1961(3) 0.3659(3) 0.0391(17) Uani 1 d . . . C17 C 0.4782(5) 0.1581(2) 0.4078(3) 0.0365(16) Uani 1 d . . . C18 C 0.3960(6) 0.1176(2) 0.3718(3) 0.0388(17) Uani 1 d . . . C19 C 0.4220(6) 0.0894(3) 0.3214(3) 0.0496(19) Uani 1 d . . . H19A H 0.4929 0.0953 0.3077 0.080 Uiso 1 d R . . C20 C 0.3448(7) 0.0529(3) 0.2918(4) 0.062(2) Uani 1 d . . . H20A H 0.3600 0.0326 0.2568 0.080 Uiso 1 d R . . C21 C 0.2460(8) 0.0447(3) 0.3141(4) 0.073(3) Uani 1 d . . . H21A H 0.1900 0.0192 0.2943 0.080 Uiso 1 d R . . C22 C 0.2250(6) 0.0749(3) 0.3635(4) 0.055(2) Uani 1 d . . . H22A H 0.1551 0.0702 0.3786 0.080 Uiso 1 d R . . C23 C 0.2273(7) 0.3477(3) 0.3155(4) 0.061(2) Uani 1 d . . . H23A H 0.1871 0.3216 0.2870 0.080 Uiso 1 d R . . C24 C 0.2117(8) 0.4018(3) 0.3024(4) 0.073(3) Uani 1 d . . . H24A H 0.1578 0.4141 0.2670 0.080 Uiso 1 d R . . C25 C 0.2739(8) 0.4390(3) 0.3420(5) 0.084(3) Uani 1 d . . . H25A H 0.2664 0.4773 0.3336 0.080 Uiso 1 d R . . C26 C 0.3469(7) 0.4207(3) 0.3941(4) 0.062(2) Uani 1 d . . . H26A H 0.3916 0.4458 0.4221 0.080 Uiso 1 d R . . C27 C 0.3563(5) 0.3659(3) 0.4053(3) 0.0455(18) Uani 1 d . . . C28 C 0.4285(6) 0.3408(3) 0.4644(3) 0.0448(18) Uani 1 d . . . C29 C 0.5525(5) 0.3302(3) 0.4589(3) 0.0421(17) Uani 1 d . . . C30 C 0.6132(6) 0.3647(3) 0.4309(4) 0.059(2) Uani 1 d . . . H30A H 0.5781 0.3971 0.4116 0.080 Uiso 1 d R . . C31 C 0.7240(7) 0.3527(3) 0.4290(4) 0.070(3) Uani 1 d . . . H31A H 0.7690 0.3766 0.4085 0.080 Uiso 1 d R . . C32 C 0.7714(6) 0.3059(3) 0.4574(4) 0.064(2) Uani 1 d . . . H32A H 0.8493 0.2966 0.4570 0.080 Uiso 1 d R . . C33 C 0.7057(6) 0.2734(3) 0.4849(4) 0.052(2) Uani 1 d . . . H33A H 0.7375 0.2406 0.5047 0.080 Uiso 1 d R . . C34 C 0.0412(6) 0.2471(3) 0.5783(4) 0.060(2) Uani 1 d . . . H34A H 0.0077 0.2785 0.5560 0.080 Uiso 1 d R . . C35 C -0.0214(7) 0.2185(4) 0.6128(4) 0.067(2) Uani 1 d . . . H35A H -0.0979 0.2290 0.6151 0.080 Uiso 1 d R . . C36 C 0.0274(7) 0.1743(4) 0.6460(4) 0.075(3) Uani 1 d . . . H36A H -0.0143 0.1544 0.6721 0.080 Uiso 1 d R . . C37 C 0.1348(6) 0.1594(3) 0.6402(3) 0.057(2) Uani 1 d . . . H37A H 0.1698 0.1281 0.6621 0.080 Uiso 1 d R . . C38 C 0.1936(5) 0.1889(3) 0.6039(3) 0.0438(18) Uani 1 d . . . C39 C 0.3155(5) 0.1772(3) 0.5987(3) 0.0409(17) Uani 1 d . . . C40 C 0.3421(6) 0.1162(3) 0.5926(3) 0.0427(17) Uani 1 d . . . C41 C 0.3723(7) 0.0826(3) 0.6424(4) 0.061(2) Uani 1 d . . . H41A H 0.3755 0.0963 0.6838 0.080 Uiso 1 d R . . C42 C 0.3992(7) 0.0295(3) 0.6333(4) 0.070(3) Uani 1 d . . . H42A H 0.4188 0.0050 0.6677 0.080 Uiso 1 d R . . C43 C 0.3942(7) 0.0118(3) 0.5741(5) 0.072(3) Uani 1 d . . . H43A H 0.4127 -0.0253 0.5664 0.080 Uiso 1 d R . . C44 C 0.3643(6) 0.0466(3) 0.5262(4) 0.054(2) Uani 1 d . . . H44A H 0.3616 0.0340 0.4845 0.080 Uiso 1 d R . . C45 C 0.4335(6) 0.3109(3) 0.6213(3) 0.0463(18) Uani 1 d . . . C46 C 0.4700(7) 0.3451(3) 0.6770(3) 0.063(2) Uani 1 d . . . H46A H 0.5507 0.3413 0.6909 0.080 Uiso 1 d R . . H46B H 0.4520 0.3825 0.6670 0.080 Uiso 1 d R . . H46C H 0.4310 0.3335 0.7094 0.080 Uiso 1 d R . . C47 C 0.6274(6) 0.1515(3) 0.6036(4) 0.049(2) Uani 1 d . . . C48 C 0.7045(8) 0.1047(4) 0.6019(4) 0.087(3) Uani 1 d . . . H48A H 0.7206 0.0880 0.6422 0.080 Uiso 1 d R . . H48B H 0.6692 0.0786 0.5718 0.080 Uiso 1 d R . . H48C H 0.7742 0.1173 0.5909 0.080 Uiso 1 d R . . C49 C 0.1354(6) 0.3795(3) 0.4850(4) 0.063(2) Uani 1 d . . . C50 C 0.0313(8) 0.4076(4) 0.4520(6) 0.116(5) Uani 1 d . . . H50A H 0.0417 0.4463 0.4533 0.080 Uiso 1 d R . . H50B H 0.0165 0.3955 0.4096 0.080 Uiso 1 d R . . H50C H -0.0320 0.3982 0.4714 0.080 Uiso 1 d R . . Cl1 Cl 0.0466(3) 0.49581(13) 0.15688(18) 0.1480(14) Uani 1 d D A 2 O15 O 0.0451(8) 0.5494(2) 0.1817(4) 0.237(3) Uani 1 d DU A 2 O16 O 0.1586(5) 0.4805(4) 0.1558(5) 0.237(3) Uani 1 d DU A 2 O17 O -0.0003(8) 0.4571(3) 0.1963(4) 0.237(3) Uani 1 d DU A 2 O18 O -0.0285(7) 0.4947(4) 0.0979(3) 0.237(3) Uani 1 d DU A 2 O1W O 0.7488(6) 0.2284(4) 0.1652(4) 0.158(4) Uani 1 d U . . H1WA H 0.7808 0.2593 0.1926 0.150 Uiso 1 d R . . H1WB H 0.7410 0.2362 0.1226 0.150 Uiso 1 d R . . O2W O 0.6147(7) 0.4405(3) 0.5748(4) 0.141(3) Uani 1 d U . . H2WA H 0.5871 0.4597 0.6087 0.150 Uiso 1 d R . . H2WB H 0.5461 0.4166 0.5695 0.150 Uiso 1 d R . . O3W O 0.8903(8) 0.3026(4) 0.2688(4) 0.156(4) Uani 1 d U . . H3WA H 0.9320 0.3356 0.2902 0.150 Uiso 1 d R . . H3WB H 0.8919 0.2799 0.3057 0.150 Uiso 1 d R . . O4W O 0.7749(8) 0.4799(3) 0.5047(5) 0.166(4) Uani 1 d U . . H4WA H 0.7882 0.5161 0.5171 0.150 Uiso 1 d R . . H4WB H 0.6955 0.4612 0.4983 0.150 Uiso 1 d R . . O5W O 0.7736(8) 0.1164(5) 0.1612(5) 0.169(4) Uani 1 d U . . H5WA H 0.7321 0.0888 0.1957 0.150 Uiso 1 d R . . O6W O 0.6137(10) 0.4086(4) 0.2581(5) 0.185(5) Uani 1 d U . . H6WA H 0.6964 0.3970 0.2725 0.150 Uiso 1 d R . . H6WB H 0.6302 0.4258 0.2224 0.150 Uiso 1 d R . . O7W O 0.6965(13) 0.0653(6) 0.2629(7) 0.126(5) Uani 0.50 d PU . . H7WA H 0.7135 0.0294 0.2724 0.150 Uiso 0.50 d PR . . H7WB H 0.7527 0.0967 0.2786 0.150 Uiso 0.50 d PR . . O8W O 0.8504(12) 0.4132(6) 0.2937(7) 0.121(6) Uani 0.50 d PU . . H8WA H 0.8944 0.4184 0.2650 0.150 Uiso 0.50 d PR . . H8WB H 0.8303 0.4438 0.3143 0.150 Uiso 0.50 d PR . . O9W O 0.5042(14) 0.4989(7) 0.3091(9) 0.178(7) Uani 0.50 d PU . . H9WA H 0.4541 0.4830 0.2771 0.150 Uiso 0.50 d PR . . H9WB H 0.5386 0.4683 0.3306 0.150 Uiso 0.50 d PR . . O10W O 1.0736(12) 0.5746(7) 0.4044(8) 0.136(6) Uani 0.50 d PU . . H10B H 1.0652 0.6143 0.4164 0.150 Uiso 0.50 d PR . . H10C H 1.0294 0.5561 0.4290 0.150 Uiso 0.50 d PR . . O11W O 0.8093(17) 0.5784(9) 0.3692(7) 0.185(8) Uani 0.50 d PU . . H11B H 0.8459 0.5422 0.3615 0.150 Uiso 0.50 d PR . . H11C H 0.8436 0.5991 0.3428 0.150 Uiso 0.50 d PR . . O12W O 0.753(2) 0.4882(8) 0.3747(10) 0.211(11) Uani 0.50 d PU . . H12B H 0.7618 0.4894 0.4161 0.150 Uiso 0.50 d PR . . H12C H 0.7836 0.4520 0.3628 0.150 Uiso 0.50 d PR . . O13W O 0.975(3) 0.5116(16) 0.3199(16) 0.161(14) Uani 0.25 d PU . . H13B H 0.9984 0.5495 0.3364 0.150 Uiso 0.25 d PR . . H13C H 0.9964 0.4987 0.2842 0.150 Uiso 0.25 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0332(4) 0.0357(4) 0.0501(5) -0.0035(4) 0.0095(4) 0.0016(3) Ni2 0.0306(4) 0.0353(4) 0.0430(5) -0.0014(4) 0.0053(4) -0.0004(3) Ni3 0.0307(4) 0.0328(4) 0.0417(5) -0.0011(4) 0.0068(3) -0.0019(3) Ni4 0.0316(4) 0.0340(4) 0.0435(5) 0.0019(4) 0.0062(3) 0.0005(3) O1 0.023(2) 0.032(2) 0.047(3) -0.0014(19) 0.0017(19) -0.0007(17) O2 0.035(2) 0.046(3) 0.065(3) 0.004(2) -0.005(2) 0.008(2) O3 0.031(2) 0.035(2) 0.034(2) -0.0012(18) 0.0071(18) -0.0001(18) O4 0.039(2) 0.039(2) 0.046(3) 0.000(2) 0.008(2) 0.015(2) O5 0.031(2) 0.030(2) 0.042(2) 0.0043(19) 0.0060(19) -0.0045(17) O6 0.043(3) 0.035(2) 0.069(3) -0.009(2) 0.010(2) -0.006(2) O7 0.030(2) 0.041(2) 0.036(2) -0.0002(19) 0.0097(18) -0.0006(19) O8 0.047(3) 0.052(3) 0.039(3) 0.001(2) 0.005(2) 0.002(2) O9 0.043(3) 0.045(3) 0.049(3) -0.011(2) 0.007(2) -0.001(2) O10 0.041(3) 0.051(3) 0.058(3) -0.013(2) 0.008(2) 0.002(2) O11 0.047(3) 0.047(3) 0.046(3) 0.001(2) 0.000(2) 0.008(2) O12 0.058(3) 0.072(3) 0.047(3) 0.004(3) 0.004(3) 0.011(3) O13 0.047(3) 0.036(2) 0.077(4) 0.000(2) 0.011(3) 0.008(2) O14 0.047(3) 0.046(3) 0.139(5) -0.018(3) 0.014(3) 0.006(3) N1 0.044(3) 0.045(3) 0.046(3) -0.001(3) 0.010(3) -0.007(3) N2 0.040(3) 0.043(3) 0.043(3) -0.002(3) 0.010(3) -0.008(3) N3 0.032(3) 0.047(3) 0.046(3) 0.006(3) 0.008(2) 0.000(2) N4 0.034(3) 0.042(3) 0.047(3) -0.005(3) 0.005(3) -0.004(2) N5 0.038(3) 0.049(3) 0.053(4) 0.006(3) 0.006(3) 0.009(3) N6 0.026(3) 0.044(3) 0.054(3) 0.001(3) 0.002(3) -0.001(2) N7 0.034(3) 0.049(3) 0.047(3) -0.002(3) 0.009(3) -0.003(3) N8 0.041(3) 0.035(3) 0.057(4) 0.006(3) 0.014(3) -0.001(2) C1 0.050(4) 0.061(5) 0.056(5) -0.006(4) 0.004(4) -0.001(4) C2 0.069(6) 0.091(6) 0.048(5) -0.009(4) 0.003(4) -0.004(5) C3 0.069(6) 0.095(7) 0.052(5) -0.004(5) -0.006(4) -0.011(5) C4 0.038(4) 0.070(5) 0.067(5) -0.003(4) -0.003(4) -0.012(4) C5 0.040(4) 0.042(4) 0.046(4) 0.007(3) -0.001(3) 0.007(3) C6 0.026(3) 0.048(4) 0.049(4) -0.003(3) -0.001(3) -0.002(3) C7 0.038(4) 0.045(4) 0.047(4) -0.009(3) 0.001(3) -0.003(3) C8 0.030(3) 0.071(5) 0.068(5) 0.004(4) 0.010(3) -0.004(3) C9 0.038(4) 0.102(7) 0.076(6) 0.005(5) 0.013(4) -0.017(4) C10 0.054(5) 0.072(5) 0.067(5) 0.003(4) 0.014(4) -0.015(4) C11 0.047(4) 0.057(4) 0.049(4) 0.004(4) 0.008(3) -0.012(4) C12 0.051(4) 0.049(4) 0.054(4) 0.016(4) 0.015(4) 0.006(3) C13 0.065(5) 0.056(5) 0.059(5) 0.019(4) 0.030(4) -0.003(4) C14 0.046(4) 0.070(5) 0.059(5) 0.006(4) 0.020(4) 0.001(4) C15 0.043(4) 0.058(4) 0.048(4) -0.004(4) 0.007(3) -0.001(3) C16 0.037(3) 0.040(4) 0.040(4) -0.001(3) 0.007(3) -0.005(3) C17 0.036(3) 0.031(3) 0.043(4) 0.003(3) 0.009(3) 0.000(3) C18 0.043(4) 0.030(3) 0.040(4) 0.002(3) -0.001(3) 0.008(3) C19 0.053(4) 0.055(4) 0.043(4) -0.004(3) 0.016(3) 0.001(4) C20 0.069(5) 0.058(5) 0.060(5) -0.024(4) 0.018(4) -0.004(4) C21 0.068(5) 0.065(5) 0.081(6) -0.025(5) 0.001(5) -0.017(4) C22 0.050(4) 0.045(4) 0.068(5) -0.017(4) 0.008(4) -0.004(3) C23 0.064(5) 0.061(5) 0.053(5) 0.004(4) 0.002(4) 0.011(4) C24 0.082(6) 0.052(5) 0.083(6) 0.033(4) 0.007(5) 0.020(4) C25 0.086(6) 0.048(5) 0.115(8) 0.034(5) 0.010(6) 0.016(5) C26 0.069(5) 0.025(3) 0.089(6) 0.006(4) 0.005(5) -0.004(3) C27 0.032(3) 0.043(4) 0.062(5) 0.014(3) 0.008(3) 0.000(3) C28 0.041(4) 0.031(3) 0.062(5) -0.002(3) 0.009(3) 0.005(3) C29 0.029(3) 0.035(3) 0.062(4) -0.001(3) 0.008(3) -0.005(3) C30 0.044(4) 0.047(4) 0.087(6) 0.014(4) 0.011(4) -0.002(3) C31 0.047(4) 0.072(5) 0.091(6) 0.018(5) 0.013(4) -0.016(4) C32 0.036(4) 0.068(5) 0.091(6) -0.001(5) 0.016(4) 0.001(4) C33 0.035(4) 0.054(4) 0.066(5) 0.000(4) 0.003(4) -0.007(3) C34 0.042(4) 0.075(5) 0.064(5) -0.002(4) 0.015(4) 0.004(4) C35 0.052(4) 0.088(6) 0.070(5) -0.002(5) 0.031(4) 0.007(4) C36 0.055(5) 0.112(7) 0.067(5) -0.002(5) 0.037(4) -0.014(5) C37 0.047(4) 0.074(5) 0.058(5) 0.001(4) 0.026(4) -0.002(4) C38 0.038(4) 0.048(4) 0.046(4) -0.005(3) 0.011(3) -0.005(3) C39 0.038(3) 0.040(4) 0.045(4) 0.007(3) 0.009(3) -0.002(3) C40 0.046(4) 0.038(4) 0.045(4) -0.002(3) 0.010(3) -0.009(3) C41 0.071(5) 0.064(5) 0.052(5) 0.013(4) 0.018(4) -0.006(4) C42 0.079(6) 0.052(5) 0.077(6) 0.022(4) 0.011(5) 0.001(4) C43 0.076(6) 0.040(4) 0.100(7) 0.006(5) 0.020(5) 0.015(4) C44 0.063(5) 0.032(4) 0.066(5) 0.004(3) 0.014(4) 0.009(3) C45 0.060(4) 0.041(4) 0.039(4) -0.005(3) 0.015(3) -0.011(3) C46 0.059(5) 0.076(5) 0.054(5) -0.017(4) 0.008(4) -0.008(4) C47 0.039(4) 0.043(4) 0.063(5) 0.003(4) 0.002(4) 0.002(3) C48 0.089(6) 0.099(7) 0.077(6) 0.032(5) 0.024(5) 0.046(5) C49 0.044(4) 0.051(5) 0.095(6) -0.008(4) 0.012(4) 0.010(4) C50 0.059(6) 0.056(5) 0.215(13) 0.030(7) -0.018(7) 0.006(5) Cl1 0.146(3) 0.116(2) 0.180(3) 0.020(2) 0.025(3) 0.077(2) O15 0.209(6) 0.194(5) 0.307(7) -0.006(5) 0.047(5) 0.057(5) O16 0.209(6) 0.194(5) 0.307(7) -0.006(5) 0.047(5) 0.057(5) O17 0.209(6) 0.194(5) 0.307(7) -0.006(5) 0.047(5) 0.057(5) O18 0.209(6) 0.194(5) 0.307(7) -0.006(5) 0.047(5) 0.057(5) O1W 0.089(5) 0.245(10) 0.155(7) 0.103(7) 0.066(5) 0.035(6) O2W 0.135(7) 0.134(7) 0.139(7) -0.024(6) -0.010(6) -0.050(6) O3W 0.187(9) 0.136(7) 0.161(8) 0.064(6) 0.071(7) 0.042(6) O4W 0.163(8) 0.071(5) 0.262(11) -0.029(6) 0.035(8) -0.028(5) O5W 0.116(7) 0.219(11) 0.172(9) -0.003(8) 0.027(6) -0.007(7) O6W 0.241(11) 0.136(8) 0.147(8) -0.009(7) -0.043(8) 0.004(8) O7W 0.183(12) 0.100(9) 0.119(10) 0.041(8) 0.094(9) 0.074(9) O8W 0.111(11) 0.105(11) 0.126(12) 0.008(9) -0.038(10) 0.022(9) O9W 0.181(12) 0.111(11) 0.291(17) 0.018(12) 0.175(12) -0.053(10) O10W 0.094(10) 0.167(14) 0.154(13) 0.081(11) 0.045(9) 0.017(10) O11W 0.250(18) 0.221(18) 0.115(11) 0.081(11) 0.116(11) 0.092(15) O12W 0.31(3) 0.135(15) 0.175(18) 0.061(14) 0.009(18) 0.034(17) O13W 0.13(2) 0.19(3) 0.14(2) 0.08(2) -0.03(2) 0.04(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 Ni1 O13 2.003(5) . ? Ni1 O10 2.003(5) . ? Ni1 O7 2.019(4) . ? Ni1 N7 2.056(6) . ? Ni1 O5 2.071(4) . ? Ni1 O1 2.165(4) . ? Ni1 Ni2 2.9440(13) . ? Ni2 O9 2.001(5) . ? Ni2 O11 2.014(5) . ? Ni2 O5 2.023(4) . ? Ni2 N6 2.068(5) . ? Ni2 O7 2.072(4) . ? Ni2 O3 2.158(4) . ? Ni3 O3 2.016(4) . ? Ni3 N8 2.030(5) . ? Ni3 N4 2.047(5) . ? Ni3 O7 2.067(4) . ? Ni3 N2 2.073(5) . ? Ni3 O1 2.094(4) . ? Ni4 O1 2.011(4) . ? Ni4 N5 2.012(6) . ? Ni4 N3 2.056(5) . ? Ni4 N1 2.059(5) . ? Ni4 O5 2.067(4) . ? Ni4 O3 2.103(4) . ? O1 C6 1.373(7) . ? O2 C6 1.407(8) . ? O3 C17 1.377(7) . ? O4 C17 1.413(7) . ? O5 C28 1.383(7) . ? O6 C28 1.391(8) . ? O7 C39 1.401(8) . ? O8 C39 1.401(8) . ? O9 C45 1.235(8) . ? O10 C45 1.265(8) . ? O11 C47 1.262(8) . ? O12 C47 1.218(9) . ? O13 C49 1.269(9) . ? O14 C49 1.218(9) . ? N1 C5 1.327(9) . ? N1 C1 1.338(9) . ? N2 C11 1.320(9) . ? N2 C7 1.366(8) . ? N3 C16 1.339(8) . ? N3 C12 1.345(9) . ? N4 C22 1.320(8) . ? N4 C18 1.323(8) . ? N5 C27 1.344(9) . ? N5 C23 1.345(9) . ? N6 C29 1.319(8) . ? N6 C33 1.342(8) . ? N7 C38 1.323(8) . ? N7 C34 1.339(9) . ? N8 C44 1.334(8) . ? N8 C40 1.339(9) . ? C1 C2 1.359(10) . ? C2 C3 1.364(12) . ? C3 C4 1.371(12) . ? C4 C5 1.374(10) . ? C5 C6 1.522(10) . ? C6 C7 1.516(10) . ? C7 C8 1.364(9) . ? C8 C9 1.351(11) . ? C9 C10 1.346(11) . ? C10 C11 1.365(10) . ? C12 C13 1.373(10) . ? C13 C14 1.354(10) . ? C14 C15 1.386(10) . ? C15 C16 1.363(9) . ? C16 C17 1.516(9) . ? C17 C18 1.514(8) . ? C18 C19 1.386(9) . ? C19 C20 1.362(10) . ? C20 C21 1.372(12) . ? C21 C22 1.372(11) . ? C23 C24 1.367(11) . ? C24 C25 1.378(12) . ? C25 C26 1.378(12) . ? C26 C27 1.370(9) . ? C27 C28 1.545(9) . ? C28 C29 1.530(9) . ? C29 C30 1.337(10) . ? C30 C31 1.365(11) . ? C31 C32 1.380(11) . ? C32 C33 1.337(11) . ? C34 C35 1.354(11) . ? C35 C36 1.374(12) . ? C36 C37 1.362(11) . ? C37 C38 1.363(10) . ? C38 C39 1.508(9) . ? C39 C40 1.542(9) . ? C40 C41 1.364(10) . ? C41 C42 1.367(11) . ? C42 C43 1.357(12) . ? C43 C44 1.351(11) . ? C45 C46 1.480(10) . ? C47 C48 1.478(11) . ? C49 C50 1.487(11) . ? Cl1 O16 1.394(6) . ? Cl1 O15 1.427(6) . ? Cl1 O18 1.431(6) . ? Cl1 O17 1.463(6) . ? 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 O13 Ni1 O10 100.46(19) . . ? O13 Ni1 O7 165.04(18) . . ? O10 Ni1 O7 93.37(18) . . ? O13 Ni1 N7 95.6(2) . . ? O10 Ni1 N7 91.7(2) . . ? O7 Ni1 N7 78.16(19) . . ? O13 Ni1 O5 100.59(19) . . ? O10 Ni1 O5 91.44(18) . . ? O7 Ni1 O5 84.61(16) . . ? N7 Ni1 O5 162.63(19) . . ? O13 Ni1 O1 87.23(18) . . ? O10 Ni1 O1 166.50(17) . . ? O7 Ni1 O1 80.37(16) . . ? N7 Ni1 O1 98.62(19) . . ? O5 Ni1 O1 76.14(15) . . ? O13 Ni1 Ni2 143.62(15) . . ? O10 Ni1 Ni2 79.66(13) . . ? O7 Ni1 Ni2 44.70(11) . . ? N7 Ni1 Ni2 120.75(15) . . ? O5 Ni1 Ni2 43.37(11) . . ? O1 Ni1 Ni2 87.56(11) . . ? O9 Ni2 O11 100.63(18) . . ? O9 Ni2 O5 93.24(18) . . ? O11 Ni2 O5 164.84(18) . . ? O9 Ni2 N6 92.2(2) . . ? O11 Ni2 N6 95.5(2) . . ? O5 Ni2 N6 77.70(18) . . ? O9 Ni2 O7 91.88(18) . . ? O11 Ni2 O7 101.00(18) . . ? O5 Ni2 O7 84.50(16) . . ? N6 Ni2 O7 161.93(18) . . ? O9 Ni2 O3 166.29(17) . . ? O11 Ni2 O3 87.97(17) . . ? O5 Ni2 O3 79.62(16) . . ? N6 Ni2 O3 97.58(19) . . ? O7 Ni2 O3 75.89(16) . . ? O9 Ni2 Ni1 79.89(13) . . ? O11 Ni2 Ni1 143.95(14) . . ? O5 Ni2 Ni1 44.68(12) . . ? N6 Ni2 Ni1 120.53(15) . . ? O7 Ni2 Ni1 43.28(11) . . ? O3 Ni2 Ni1 86.87(11) . . ? O3 Ni3 N8 106.67(19) . . ? O3 Ni3 N4 78.25(19) . . ? N8 Ni3 N4 98.1(2) . . ? O3 Ni3 O7 79.17(16) . . ? N8 Ni3 O7 78.5(2) . . ? N4 Ni3 O7 155.06(18) . . ? O3 Ni3 N2 158.21(19) . . ? N8 Ni3 N2 94.9(2) . . ? N4 Ni3 N2 96.4(2) . . ? O7 Ni3 N2 108.48(19) . . ? O3 Ni3 O1 83.73(16) . . ? N8 Ni3 O1 154.6(2) . . ? N4 Ni3 O1 106.83(19) . . ? O7 Ni3 O1 80.98(16) . . ? N2 Ni3 O1 77.60(18) . . ? O1 Ni4 N5 105.8(2) . . ? O1 Ni4 N3 157.38(19) . . ? N5 Ni4 N3 96.7(2) . . ? O1 Ni4 N1 78.5(2) . . ? N5 Ni4 N1 97.1(2) . . ? N3 Ni4 N1 96.3(2) . . ? O1 Ni4 O5 79.70(16) . . ? N5 Ni4 O5 78.4(2) . . ? N3 Ni4 O5 108.12(19) . . ? N1 Ni4 O5 155.5(2) . . ? O1 Ni4 O3 83.61(16) . . ? N5 Ni4 O3 154.26(19) . . ? N3 Ni4 O3 77.16(19) . . ? N1 Ni4 O3 108.37(19) . . ? O5 Ni4 O3 79.94(15) . . ? C6 O1 Ni4 116.3(4) . . ? C6 O1 Ni3 110.2(4) . . ? Ni4 O1 Ni3 94.67(16) . . ? C6 O1 Ni1 130.8(4) . . ? Ni4 O1 Ni1 101.38(16) . . ? Ni3 O1 Ni1 96.10(16) . . ? C17 O3 Ni3 116.4(3) . . ? C17 O3 Ni4 109.6(3) . . ? Ni3 O3 Ni4 94.24(16) . . ? C17 O3 Ni2 130.5(3) . . ? Ni3 O3 Ni2 101.82(18) . . ? Ni4 O3 Ni2 96.97(16) . . ? C28 O5 Ni2 115.0(4) . . ? C28 O5 Ni4 109.0(4) . . ? Ni2 O5 Ni4 102.57(18) . . ? C28 O5 Ni1 131.5(4) . . ? Ni2 O5 Ni1 91.94(16) . . ? Ni4 O5 Ni1 102.71(17) . . ? C39 O7 Ni1 114.8(4) . . ? C39 O7 Ni3 109.2(4) . . ? Ni1 O7 Ni3 101.62(17) . . ? C39 O7 Ni2 131.6(4) . . ? Ni1 O7 Ni2 92.02(17) . . ? Ni3 O7 Ni2 103.06(18) . . ? C45 O9 Ni2 127.0(4) . . ? C45 O10 Ni1 126.5(4) . . ? C47 O11 Ni2 133.9(5) . . ? C49 O13 Ni1 132.1(5) . . ? C5 N1 C1 118.0(6) . . ? C5 N1 Ni4 115.5(5) . . ? C1 N1 Ni4 126.5(5) . . ? C11 N2 C7 118.1(6) . . ? C11 N2 Ni3 128.6(5) . . ? C7 N2 Ni3 113.2(4) . . ? C16 N3 C12 117.9(6) . . ? C16 N3 Ni4 114.6(4) . . ? C12 N3 Ni4 127.5(5) . . ? C22 N4 C18 118.7(6) . . ? C22 N4 Ni3 125.7(5) . . ? C18 N4 Ni3 115.5(4) . . ? C27 N5 C23 118.2(6) . . ? C27 N5 Ni4 114.2(4) . . ? C23 N5 Ni4 127.5(5) . . ? C29 N6 C33 118.7(6) . . ? C29 N6 Ni2 115.6(4) . . ? C33 N6 Ni2 125.6(5) . . ? C38 N7 C34 119.7(6) . . ? C38 N7 Ni1 115.1(4) . . ? C34 N7 Ni1 125.1(5) . . ? C44 N8 C40 118.1(6) . . ? C44 N8 Ni3 128.1(5) . . ? C40 N8 Ni3 113.7(4) . . ? N1 C1 C2 123.9(8) . . ? C3 C2 C1 117.2(8) . . ? C2 C3 C4 120.5(8) . . ? C3 C4 C5 118.5(8) . . ? N1 C5 C4 121.8(7) . . ? N1 C5 C6 114.9(6) . . ? C4 C5 C6 123.2(7) . . ? O1 C6 O2 112.0(5) . . ? O1 C6 C7 108.5(5) . . ? O2 C6 C7 109.3(5) . . ? O1 C6 C5 109.5(5) . . ? O2 C6 C5 105.5(5) . . ? C7 C6 C5 112.0(5) . . ? C8 C7 N2 120.7(7) . . ? C8 C7 C6 124.3(6) . . ? N2 C7 C6 115.0(6) . . ? C9 C8 C7 119.6(7) . . ? C10 C9 C8 120.1(7) . . ? C9 C10 C11 118.9(8) . . ? N2 C11 C10 122.6(7) . . ? N3 C12 C13 122.1(7) . . ? C14 C13 C12 119.5(7) . . ? C13 C14 C15 119.0(7) . . ? C16 C15 C14 118.9(7) . . ? N3 C16 C15 122.6(6) . . ? N3 C16 C17 114.9(6) . . ? C15 C16 C17 122.5(6) . . ? O3 C17 O4 111.0(5) . . ? O3 C17 C18 109.2(5) . . ? O4 C17 C18 106.1(5) . . ? O3 C17 C16 108.3(5) . . ? O4 C17 C16 109.6(5) . . ? C18 C17 C16 112.7(5) . . ? N4 C18 C19 122.6(6) . . ? N4 C18 C17 115.7(6) . . ? C19 C18 C17 121.7(6) . . ? C20 C19 C18 118.5(7) . . ? C19 C20 C21 118.5(7) . . ? C20 C21 C22 119.7(7) . . ? N4 C22 C21 121.9(8) . . ? N5 C23 C24 122.8(8) . . ? C23 C24 C25 118.5(8) . . ? C24 C25 C26 119.3(7) . . ? C27 C26 C25 119.2(7) . . ? N5 C27 C26 121.9(7) . . ? N5 C27 C28 114.1(6) . . ? C26 C27 C28 123.9(7) . . ? O5 C28 O6 113.7(6) . . ? O5 C28 C29 108.2(5) . . ? O6 C28 C29 106.1(5) . . ? O5 C28 C27 107.7(5) . . ? O6 C28 C27 107.5(5) . . ? C29 C28 C27 113.7(6) . . ? N6 C29 C30 122.4(6) . . ? N6 C29 C28 114.7(6) . . ? C30 C29 C28 122.8(6) . . ? C29 C30 C31 119.1(7) . . ? C30 C31 C32 119.1(8) . . ? C33 C32 C31 118.4(7) . . ? C32 C33 N6 122.1(7) . . ? N7 C34 C35 121.9(8) . . ? C34 C35 C36 118.8(8) . . ? C37 C36 C35 118.6(8) . . ? C38 C37 C36 120.4(8) . . ? N7 C38 C37 120.5(6) . . ? N7 C38 C39 116.0(6) . . ? C37 C38 C39 123.4(6) . . ? O8 C39 O7 113.4(5) . . ? O8 C39 C38 105.1(5) . . ? O7 C39 C38 108.2(5) . . ? O8 C39 C40 108.6(5) . . ? O7 C39 C40 107.5(5) . . ? C38 C39 C40 114.1(5) . . ? N8 C40 C41 121.4(6) . . ? N8 C40 C39 115.2(6) . . ? C41 C40 C39 123.3(6) . . ? C40 C41 C42 119.8(8) . . ? C43 C42 C41 118.5(8) . . ? C44 C43 C42 119.7(7) . . ? N8 C44 C43 122.5(8) . . ? O9 C45 O10 126.8(6) . . ? O9 C45 C46 117.6(7) . . ? O10 C45 C46 115.6(6) . . ? O12 C47 O11 124.7(7) . . ? O12 C47 C48 118.9(7) . . ? O11 C47 C48 116.4(7) . . ? O14 C49 O13 124.9(7) . . ? O14 C49 C50 118.2(7) . . ? O13 C49 C50 117.0(7) . . ? O16 Cl1 O15 109.6(5) . . ? O16 Cl1 O18 115.0(6) . . ? O15 Cl1 O18 108.1(5) . . ? O16 Cl1 O17 107.9(5) . . ? O15 Cl1 O17 110.1(5) . . ? O18 Cl1 O17 106.0(5) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.932 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.112 #_eof #End of Crystallographic Information File