Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_method 'SHELXL-97 plus manual editing' _publ_contact_author_name 'Christine McKenzie' _publ_contact_author_address ; Chemistry Institute University of Odense Campusvej 55 Odense 5230 DENMARK ; _publ_contact_author_email CHK@CHEM.SDU.DK _publ_section_title ; Controlled formation and topologies of thiophenolate-based macrocycles: rings, cylinders and bowls ; loop_ _publ_author_name A.Christensen C.Mayer F.Jensen A.D.Bond C.J.McKenzie data_1 _database_code_depnum_ccdc_archive 'CCDC 282070' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C30 H38 N4 Ni2 S2 2+, 2(Cl O4 1-), 2(C2 H3 N) ; _chemical_formula_sum 'C34 H44 Cl2 N6 Ni2 O8 S2' _chemical_formula_weight 917.19 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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' _symmetry_space_group_name_Hall '-I 2ya' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 16.3627(9) _cell_length_b 11.4598(6) _cell_length_c 21.3431(14) _cell_angle_alpha 90.00 _cell_angle_beta 104.445(2) _cell_angle_gamma 90.00 _cell_volume 3875.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4432 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 25.69 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 22150 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 28.54 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 4928 _reflns_number_gt 3365 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-8 (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4928 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.621 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.079 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.248162(18) 0.01908(3) 0.074042(12) 0.02114(10) Uani 1 1 d . . . S1 S 0.33668(4) -0.02500(5) 0.01764(2) 0.02143(14) Uani 1 1 d . . . N1 N 0.33799(12) 0.04649(17) 0.14992(8) 0.0239(4) Uani 1 1 d . . . N2 N 0.15647(12) 0.05475(17) 0.11297(8) 0.0240(4) Uani 1 1 d . . . C1 C 0.40988(14) 0.0904(2) 0.03333(10) 0.0225(5) Uani 1 1 d . . . C2 C 0.44171(14) 0.1374(2) -0.01615(10) 0.0230(5) Uani 1 1 d . . . C3 C 0.50719(14) 0.2185(2) -0.00113(10) 0.0259(5) Uani 1 1 d . . . H3A H 0.5285 0.2496 -0.0352 0.031 Uiso 1 1 calc R . . C4 C 0.54245(14) 0.2557(2) 0.06193(10) 0.0249(5) Uani 1 1 d . . . C5 C 0.50881(14) 0.2087(2) 0.11030(10) 0.0267(5) Uani 1 1 d . . . H5A H 0.5318 0.2320 0.1539 0.032 Uiso 1 1 calc R . . C6 C 0.44249(14) 0.1286(2) 0.09691(10) 0.0240(5) Uani 1 1 d . . . C7 C 0.41143(15) 0.0869(2) 0.15180(10) 0.0265(5) Uani 1 1 d . . . H7A H 0.4500 0.0903 0.1932 0.032 Uiso 1 1 calc R . . C8 C 0.32387(16) 0.0090(2) 0.21274(10) 0.0304(6) Uani 1 1 d . . . H8A H 0.3739 0.0290 0.2479 0.036 Uiso 1 1 calc R . . H8B H 0.3164 -0.0768 0.2126 0.036 Uiso 1 1 calc R . . C9 C 0.24652(16) 0.0676(2) 0.22519(10) 0.0329(6) Uani 1 1 d . . . H9A H 0.2457 0.0546 0.2709 0.040 Uiso 1 1 calc R . . H9B H 0.2508 0.1528 0.2188 0.040 Uiso 1 1 calc R . . C10 C 0.16454(16) 0.0242(2) 0.18210(10) 0.0303(6) Uani 1 1 d . . . H10A H 0.1615 -0.0616 0.1863 0.036 Uiso 1 1 calc R . . H10B H 0.1168 0.0588 0.1964 0.036 Uiso 1 1 calc R . . C12 C 0.61441(15) 0.3453(2) 0.07920(11) 0.0309(6) Uani 1 1 d . . . C13 C 0.58260(18) 0.4552(2) 0.10648(14) 0.0453(7) Uani 1 1 d . . . H13A H 0.5346 0.4876 0.0742 0.068 Uiso 1 1 calc R . . H13B H 0.6280 0.5131 0.1170 0.068 Uiso 1 1 calc R . . H13C H 0.5649 0.4351 0.1457 0.068 Uiso 1 1 calc R . . C14 C 0.64531(19) 0.3796(3) 0.01998(13) 0.0487(8) Uani 1 1 d . . . H14A H 0.6669 0.3103 0.0025 0.073 Uiso 1 1 calc R . . H14B H 0.6905 0.4376 0.0324 0.073 Uiso 1 1 calc R . . H14C H 0.5984 0.4129 -0.0130 0.073 Uiso 1 1 calc R . . C15 C 0.68813(17) 0.2948(3) 0.13010(14) 0.0500(8) Uani 1 1 d . . . H15A H 0.7079 0.2233 0.1134 0.075 Uiso 1 1 calc R . . H15B H 0.6698 0.2768 0.1694 0.075 Uiso 1 1 calc R . . H15C H 0.7342 0.3518 0.1403 0.075 Uiso 1 1 calc R . . C11 C 0.08688(14) 0.1034(2) 0.08435(9) 0.0243(5) Uani 1 1 d . . . H11A H 0.0490 0.1196 0.1105 0.029 Uiso 1 1 calc R . . Cl1 Cl 0.54512(4) 0.23817(6) 0.30628(3) 0.03488(17) Uani 1 1 d . . . O1A O 0.59643(15) 0.1774(2) 0.27313(9) 0.0791(8) Uani 1 1 d . . . O1B O 0.59402(14) 0.2846(2) 0.36552(8) 0.0629(6) Uani 1 1 d . . . O1C O 0.50625(17) 0.3306(2) 0.26596(11) 0.0809(8) Uani 1 1 d . . . O1D O 0.4835(2) 0.1646(3) 0.31911(14) 0.1176(12) Uani 1 1 d . . . N100 N 0.2639(3) 0.2067(4) 0.4189(3) 0.145(2) Uani 1 1 d . . . C100 C 0.2086(2) 0.1481(3) 0.39840(19) 0.0660(10) Uani 1 1 d . . . C101 C 0.1383(2) 0.0759(3) 0.37286(18) 0.0648(9) Uani 1 1 d . . . H10C H 0.1035 0.0701 0.4040 0.097 Uiso 1 1 calc R . . H10D H 0.1579 -0.0021 0.3645 0.097 Uiso 1 1 calc R . . H10E H 0.1048 0.1094 0.3323 0.097 Uiso 1 1 calc R . . 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 0.02095(18) 0.02669(18) 0.01625(13) 0.00083(11) 0.00552(11) 0.00093(13) S1 0.0213(3) 0.0242(3) 0.0191(2) 0.0001(2) 0.0057(2) 0.0011(2) N1 0.0248(11) 0.0286(12) 0.0180(8) 0.0011(7) 0.0047(8) 0.0023(9) N2 0.0238(11) 0.0296(12) 0.0197(8) 0.0023(8) 0.0075(8) -0.0006(9) C1 0.0172(12) 0.0255(13) 0.0243(10) -0.0002(9) 0.0044(9) 0.0040(10) C2 0.0201(12) 0.0276(13) 0.0225(10) -0.0007(9) 0.0077(9) 0.0033(10) C3 0.0230(13) 0.0294(15) 0.0271(10) 0.0009(9) 0.0096(10) 0.0020(11) C4 0.0202(13) 0.0275(14) 0.0278(10) -0.0021(9) 0.0073(9) 0.0019(10) C5 0.0212(13) 0.0349(15) 0.0231(10) -0.0028(10) 0.0038(9) 0.0033(11) C6 0.0183(12) 0.0291(13) 0.0242(10) 0.0004(9) 0.0046(9) 0.0040(10) C7 0.0263(14) 0.0317(14) 0.0200(9) -0.0008(9) 0.0029(9) 0.0037(11) C8 0.0281(14) 0.0453(16) 0.0183(10) 0.0074(10) 0.0069(9) -0.0021(12) C9 0.0387(16) 0.0433(16) 0.0186(10) 0.0007(10) 0.0105(10) 0.0027(13) C10 0.0302(14) 0.0436(15) 0.0202(10) 0.0069(10) 0.0125(10) 0.0059(12) C12 0.0261(14) 0.0365(16) 0.0304(11) -0.0055(10) 0.0074(10) -0.0068(12) C13 0.0425(18) 0.0406(18) 0.0533(16) -0.0130(13) 0.0127(14) -0.0076(14) C14 0.0470(18) 0.059(2) 0.0448(15) -0.0120(14) 0.0198(14) -0.0234(16) C15 0.0311(17) 0.050(2) 0.0623(18) 0.0009(15) -0.0009(14) -0.0101(14) C11 0.0234(13) 0.0301(14) 0.0218(10) 0.0001(9) 0.0102(9) 0.0004(11) Cl1 0.0428(4) 0.0361(4) 0.0267(3) -0.0058(2) 0.0104(3) -0.0050(3) O1A 0.0857(18) 0.109(2) 0.0375(11) -0.0209(12) 0.0065(11) 0.0507(16) O1B 0.0696(15) 0.0876(17) 0.0317(10) -0.0232(10) 0.0133(10) -0.0198(13) O1C 0.0950(19) 0.0749(18) 0.0683(15) 0.0158(13) 0.0118(14) 0.0381(15) O1D 0.149(3) 0.117(2) 0.101(2) -0.0279(18) 0.057(2) -0.099(2) N100 0.079(3) 0.073(3) 0.249(6) 0.052(3) -0.022(3) -0.018(2) C100 0.051(2) 0.047(2) 0.099(3) 0.0260(19) 0.017(2) 0.0112(19) C101 0.048(2) 0.064(2) 0.084(2) 0.0083(19) 0.0202(18) 0.0115(19) _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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 1.5369 (0.0080) x + 10.9515 (0.0018) y - 6.2693 (0.0101) z = 0.1104 (0.0020) * -0.0217 (0.0007) N1 * 0.0215 (0.0006) N2 * 0.0227 (0.0007) S1 * -0.0225 (0.0007) S1_$1 0.0158 (0.0008) Ni1 Rms deviation of fitted atoms = 0.0221 10.7357 (0.0116) x - 8.5203 (0.0072) y - 0.8191 (0.0198) z = 3.5893 (0.0065) * 0.0137 (0.0016) C1 * -0.0042 (0.0015) C2 * -0.0051 (0.0016) C3 * 0.0049 (0.0017) C4 * 0.0045 (0.0016) C5 * -0.0137 (0.0016) C6 Rms deviation of fitted atoms = 0.0088 10.7357 (0.0116) x + 8.5203 (0.0072) y - 0.8191 (0.0198) z = 1.7786 (0.0016) Angle to previous plane (with approximate esd) = 83.94 ( 0.05 ) * -0.0137 (0.0016) C1_$1 * 0.0042 (0.0015) C2_$1 * 0.0051 (0.0016) C3_$1 * -0.0049 (0.0017) C4_$1 * -0.0045 (0.0016) C5_$1 * 0.0137 (0.0016) C6_$1 Rms deviation of fitted atoms = 0.0088 ; 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 N1 1.9220(18) . ? Ni1 N2 1.9313(19) . ? Ni1 S1 2.1578(6) 2 ? Ni1 S1 2.1615(6) . ? S1 C1 1.759(2) . ? S1 Ni1 2.1579(6) 2 ? N1 C7 1.279(3) . ? N1 C8 1.480(3) . ? N2 C11 1.278(3) . ? N2 C10 1.490(3) . ? C1 C2 1.397(3) . ? C1 C6 1.399(3) . ? C2 C3 1.394(3) . ? C2 C11 1.466(3) 2 ? C3 C4 1.392(3) . ? C3 H3A 0.9500 . ? C4 C5 1.394(3) . ? C4 C12 1.536(3) . ? C5 C6 1.396(3) . ? C5 H5A 0.9500 . ? C6 C7 1.468(3) . ? C7 H7A 0.9500 . ? C8 C9 1.514(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.509(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 C15 1.522(4) . ? C12 C14 1.525(3) . ? C12 C13 1.532(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C11 C2 1.466(3) 2 ? C11 H11A 0.9500 . ? Cl1 O1D 1.393(3) . ? Cl1 O1A 1.409(2) . ? Cl1 O1C 1.412(2) . ? Cl1 O1B 1.4203(18) . ? N100 C100 1.124(5) . ? C100 C101 1.411(5) . ? C101 H10C 0.9800 . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? 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 N1 Ni1 N2 96.65(8) . . ? N1 Ni1 S1 170.45(6) . 2 ? N2 Ni1 S1 92.67(6) . 2 ? N1 Ni1 S1 91.70(6) . . ? N2 Ni1 S1 171.65(6) . . ? S1 Ni1 S1 79.00(3) 2 . ? C1 S1 Ni1 104.49(7) . 2 ? C1 S1 Ni1 103.73(7) . . ? Ni1 S1 Ni1 94.67(3) 2 . ? C7 N1 C8 115.75(18) . . ? C7 N1 Ni1 126.92(15) . . ? C8 N1 Ni1 117.16(15) . . ? C11 N2 C10 115.09(19) . . ? C11 N2 Ni1 125.58(15) . . ? C10 N2 Ni1 119.33(15) . . ? C2 C1 C6 119.3(2) . . ? C2 C1 S1 120.68(16) . . ? C6 C1 S1 119.78(17) . . ? C3 C2 C1 119.55(19) . . ? C3 C2 C11 116.23(19) . 2 ? C1 C2 C11 124.2(2) . 2 ? C4 C3 C2 122.4(2) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C3 C4 C5 116.9(2) . . ? C3 C4 C12 123.0(2) . . ? C5 C4 C12 120.08(19) . . ? C4 C5 C6 122.2(2) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C7 117.19(19) . . ? C1 C6 C7 123.2(2) . . ? N1 C7 C6 127.02(19) . . ? N1 C7 H7A 116.5 . . ? C6 C7 H7A 116.5 . . ? N1 C8 C9 110.87(18) . . ? N1 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 113.7(2) . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N2 C10 C9 111.82(19) . . ? N2 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? N2 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C15 C12 C14 108.8(2) . . ? C15 C12 C13 109.0(2) . . ? C14 C12 C13 108.5(2) . . ? C15 C12 C4 109.9(2) . . ? C14 C12 C4 111.46(19) . . ? C13 C12 C4 109.1(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C11 C2 128.0(2) . 2 ? N2 C11 H11A 116.0 . . ? C2 C11 H11A 116.0 2 . ? O1D Cl1 O1A 110.56(19) . . ? O1D Cl1 O1C 109.6(2) . . ? O1A Cl1 O1C 107.37(15) . . ? O1D Cl1 O1B 109.06(15) . . ? O1A Cl1 O1B 110.99(14) . . ? O1C Cl1 O1B 109.23(15) . . ? N100 C100 C101 179.1(5) . . ? C100 C101 H10C 109.5 . . ? C100 C101 H10D 109.5 . . ? H10C C101 H10D 109.5 . . ? C100 C101 H10E 109.5 . . ? H10C C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 S1 C1 -49.43(9) . . . . ? S1 Ni1 S1 C1 132.75(7) 2 . . . ? N1 Ni1 S1 Ni1 -155.59(6) . . . 2 ? S1 Ni1 S1 Ni1 26.59(3) 2 . . 2 ? N2 Ni1 N1 C7 -146.8(2) . . . . ? S1 Ni1 N1 C7 33.0(2) . . . . ? N2 Ni1 N1 C8 38.19(17) . . . . ? S1 Ni1 N1 C8 -142.00(16) . . . . ? N1 Ni1 N2 C11 145.6(2) . . . . ? S1 Ni1 N2 C11 -36.5(2) 2 . . . ? N1 Ni1 N2 C10 -34.58(18) . . . . ? S1 Ni1 N2 C10 143.30(16) 2 . . . ? Ni1 S1 C1 C2 -41.2(2) 2 . . . ? Ni1 S1 C1 C2 -139.80(17) . . . . ? Ni1 S1 C1 C6 144.69(17) 2 . . . ? Ni1 S1 C1 C6 46.08(19) . . . . ? C6 C1 C2 C3 2.1(3) . . . . ? S1 C1 C2 C3 -172.08(17) . . . . ? C6 C1 C2 C11 179.4(2) . . . 2 ? S1 C1 C2 C11 5.2(3) . . . 2 ? C1 C2 C3 C4 -0.3(3) . . . . ? C11 C2 C3 C4 -177.8(2) 2 . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C2 C3 C4 C12 -179.8(2) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C12 C4 C5 C6 178.9(2) . . . . ? C4 C5 C6 C1 2.2(4) . . . . ? C4 C5 C6 C7 -178.9(2) . . . . ? C2 C1 C6 C5 -3.0(3) . . . . ? S1 C1 C6 C5 171.24(17) . . . . ? C2 C1 C6 C7 178.2(2) . . . . ? S1 C1 C6 C7 -7.6(3) . . . . ? C8 N1 C7 C6 179.2(2) . . . . ? Ni1 N1 C7 C6 4.1(4) . . . . ? C5 C6 C7 N1 155.5(2) . . . . ? C1 C6 C7 N1 -25.7(4) . . . . ? C7 N1 C8 C9 126.3(2) . . . . ? Ni1 N1 C8 C9 -58.1(2) . . . . ? N1 C8 C9 C10 70.7(3) . . . . ? C11 N2 C10 C9 -130.0(2) . . . . ? Ni1 N2 C10 C9 50.2(3) . . . . ? C8 C9 C10 N2 -65.9(3) . . . . ? C3 C4 C12 C15 -124.9(3) . . . . ? C5 C4 C12 C15 55.8(3) . . . . ? C3 C4 C12 C14 -4.3(3) . . . . ? C5 C4 C12 C14 176.5(2) . . . . ? C3 C4 C12 C13 115.6(3) . . . . ? C5 C4 C12 C13 -63.7(3) . . . . ? C10 N2 C11 C2 -176.2(2) . . . 2 ? Ni1 N2 C11 C2 3.6(4) . . . 2 ? #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 282071' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C30 H38 N4 Ni2 S2 2+, 2(Cl O4 -), 0.67(C H4 O) ; _chemical_formula_sum 'C30.67 H40.67 Cl2 N4 Ni2 O8.67 S2' _chemical_formula_weight 856.45 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' S S 0.1246 0.1234 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.071(3) _cell_length_b 13.6690(18) _cell_length_c 40.076(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.805(7) _cell_angle_gamma 90.00 _cell_volume 10677(3) _cell_formula_units_Z 12 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1220 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 20.79 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5328 _exptl_absorpt_coefficient_mu 1.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.792885 ; _exptl_special_details ; Methanol grossly disordered - modelled in approximate three sites. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 26785 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.1152 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 25.65 _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.932 _reflns_number_total 9431 _reflns_number_gt 5301 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-8 (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9431 _refine_ls_number_parameters 666 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.942 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.098 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.42239(3) 0.70386(5) 0.228188(16) 0.02696(17) Uani 1 1 d . . . S11 S 0.47769(6) 0.67133(9) 0.28034(3) 0.0279(3) Uani 1 1 d . . . N11 N 0.33952(19) 0.7360(3) 0.24211(11) 0.0279(10) Uani 1 1 d . . . N12 N 0.3862(2) 0.7309(3) 0.18016(11) 0.0287(10) Uani 1 1 d . . . C11 C 0.4612(2) 0.7737(3) 0.30400(13) 0.0262(11) Uani 1 1 d . . . C12 C 0.5116(2) 0.8115(3) 0.33064(12) 0.0254(11) Uani 1 1 d . . . C13 C 0.4950(2) 0.8869(3) 0.35125(13) 0.0270(12) Uani 1 1 d . . . H13A H 0.5300 0.9125 0.3694 0.032 Uiso 1 1 calc R . . C14 C 0.4290(2) 0.9248(4) 0.34575(12) 0.0272(12) Uani 1 1 d . . . C15 C 0.3793(3) 0.8843(4) 0.31901(13) 0.0284(12) Uani 1 1 d . . . H15A H 0.3335 0.9076 0.3151 0.034 Uiso 1 1 calc R . . C16 C 0.3944(2) 0.8107(4) 0.29778(12) 0.0260(11) Uani 1 1 d . . . C17 C 0.3366(2) 0.7763(4) 0.27057(13) 0.0293(12) Uani 1 1 d . . . H17A H 0.2922 0.7849 0.2745 0.035 Uiso 1 1 calc R . . C18 C 0.2728(2) 0.7073(4) 0.21928(13) 0.0337(13) Uani 1 1 d . . . H18A H 0.2352 0.7352 0.2284 0.040 Uiso 1 1 calc R . . H18B H 0.2685 0.6352 0.2194 0.040 Uiso 1 1 calc R . . C19 C 0.2649(3) 0.7416(4) 0.18277(13) 0.0335(13) Uani 1 1 d . . . H19A H 0.2705 0.8136 0.1828 0.040 Uiso 1 1 calc R . . H19B H 0.2178 0.7263 0.1695 0.040 Uiso 1 1 calc R . . C110 C 0.3158(2) 0.6956(4) 0.16491(14) 0.0333(13) Uani 1 1 d . . . H11A H 0.3144 0.6236 0.1671 0.040 Uiso 1 1 calc R . . H11B H 0.3030 0.7123 0.1402 0.040 Uiso 1 1 calc R . . C111 C 0.4126(2) 1.0084(4) 0.36802(13) 0.0314(12) Uani 1 1 d . . . C112 C 0.4444(3) 1.1029(4) 0.35824(16) 0.0454(15) Uani 1 1 d . . . H11C H 0.4941 1.0944 0.3619 0.068 Uiso 1 1 calc R . . H11D H 0.4351 1.1568 0.3726 0.068 Uiso 1 1 calc R . . H11E H 0.4244 1.1180 0.3340 0.068 Uiso 1 1 calc R . . C113 C 0.3350(3) 1.0238(5) 0.36230(17) 0.0492(16) Uani 1 1 d . . . H11F H 0.3139 0.9641 0.3686 0.074 Uiso 1 1 calc R . . H11G H 0.3152 1.0390 0.3381 0.074 Uiso 1 1 calc R . . H11H H 0.3263 1.0782 0.3766 0.074 Uiso 1 1 calc R . . C114 C 0.4427(3) 0.9861(4) 0.40606(15) 0.0443(15) Uani 1 1 d . . . H11I H 0.4220 0.9260 0.4124 0.066 Uiso 1 1 calc R . . H11J H 0.4328 1.0406 0.4200 0.066 Uiso 1 1 calc R . . H11K H 0.4924 0.9775 0.4101 0.066 Uiso 1 1 calc R . . C115 C 0.4176(3) 0.7740(4) 0.15969(13) 0.0288(12) Uani 1 1 d . . . H11L H 0.3930 0.7824 0.1365 0.035 Uiso 1 1 calc R . . Ni2 Ni 0.46432(3) 0.51280(5) 0.382745(16) 0.02698(17) Uani 1 1 d . . . S21 S 0.47916(6) 0.54777(9) 0.43679(3) 0.0291(3) Uani 1 1 d . . . N21 N 0.5054(2) 0.3852(3) 0.39222(11) 0.0293(10) Uani 1 1 d . . . N22 N 0.4394(2) 0.4942(3) 0.33416(10) 0.0266(9) Uani 1 1 d . . . C21 C 0.4477(3) 0.4433(4) 0.45389(13) 0.0315(12) Uani 1 1 d . . . C22 C 0.4093(3) 0.4529(4) 0.47880(13) 0.0313(12) Uani 1 1 d . . . C23 C 0.3936(3) 0.3700(4) 0.49537(14) 0.0360(13) Uani 1 1 d . . . H23A H 0.3676 0.3772 0.5122 0.043 Uiso 1 1 calc R . . C24 C 0.4145(3) 0.2765(4) 0.48837(14) 0.0400(14) Uani 1 1 d . A . C25 C 0.4498(3) 0.2699(4) 0.46262(14) 0.0416(15) Uani 1 1 d . . . H25A H 0.4634 0.2069 0.4566 0.050 Uiso 1 1 calc R . . C26 C 0.4665(3) 0.3512(4) 0.44506(13) 0.0332(13) Uani 1 1 d . . . C27 C 0.5024(3) 0.3316(4) 0.41788(14) 0.0373(14) Uani 1 1 d . . . H27A H 0.5264 0.2712 0.4196 0.045 Uiso 1 1 calc R . . C28 C 0.5468(3) 0.3480(4) 0.36928(14) 0.0395(14) Uani 1 1 d . . . H28A H 0.5624 0.2809 0.3764 0.047 Uiso 1 1 calc R . . H28B H 0.5880 0.3896 0.3716 0.047 Uiso 1 1 calc R . . C29 C 0.5080(3) 0.3464(4) 0.33224(14) 0.0367(13) Uani 1 1 d . . . H29A H 0.4651 0.3086 0.3301 0.044 Uiso 1 1 calc R . . H29B H 0.5360 0.3126 0.3185 0.044 Uiso 1 1 calc R . . C210 C 0.4905(3) 0.4477(4) 0.31784(14) 0.0334(13) Uani 1 1 d . . . H21A H 0.5326 0.4881 0.3221 0.040 Uiso 1 1 calc R . . H21B H 0.4715 0.4436 0.2927 0.040 Uiso 1 1 calc R . . C211 C 0.3997(3) 0.1868(4) 0.50836(13) 0.0464(15) Uani 1 1 d D . . C212 C 0.4336(4) 0.2065(7) 0.54716(19) 0.038(2) Uiso 0.60 1 d PD A 1 H21C H 0.4726 0.2510 0.5490 0.058 Uiso 0.60 1 calc PR A 1 H21D H 0.4496 0.1446 0.5586 0.058 Uiso 0.60 1 calc PR A 1 H21E H 0.3998 0.2363 0.5581 0.058 Uiso 0.60 1 calc PR A 1 C213 C 0.3217(4) 0.1819(9) 0.5058(3) 0.069(3) Uiso 0.60 1 d PD A 1 H21F H 0.2974 0.1701 0.4819 0.103 Uiso 0.60 1 calc PR A 1 H21G H 0.3063 0.2439 0.5136 0.103 Uiso 0.60 1 calc PR A 1 H21H H 0.3121 0.1285 0.5203 0.103 Uiso 0.60 1 calc PR A 1 C214 C 0.4254(7) 0.0910(9) 0.4982(3) 0.097(5) Uiso 0.60 1 d PD A 1 H21I H 0.4047 0.0782 0.4739 0.145 Uiso 0.60 1 calc PR A 1 H21J H 0.4129 0.0385 0.5122 0.145 Uiso 0.60 1 calc PR A 1 H21K H 0.4754 0.0936 0.5019 0.145 Uiso 0.60 1 calc PR A 1 C222 C 0.3423(7) 0.1299(12) 0.4831(4) 0.074(5) Uiso 0.40 1 d PD A 2 H22A H 0.3442 0.1447 0.4594 0.111 Uiso 0.40 1 calc PR A 2 H22B H 0.2975 0.1494 0.4867 0.111 Uiso 0.40 1 calc PR A 2 H22C H 0.3488 0.0595 0.4873 0.111 Uiso 0.40 1 calc PR A 2 C223 C 0.3793(9) 0.2051(15) 0.5412(4) 0.093(7) Uiso 0.40 1 d PD A 2 H22D H 0.3291 0.2046 0.5369 0.139 Uiso 0.40 1 calc PR A 2 H22E H 0.3968 0.2690 0.5504 0.139 Uiso 0.40 1 calc PR A 2 H22F H 0.3985 0.1538 0.5578 0.139 Uiso 0.40 1 calc PR A 2 C224 C 0.4639(6) 0.1204(12) 0.5142(4) 0.070(5) Uiso 0.40 1 d PD A 2 H22G H 0.4650 0.0871 0.4927 0.105 Uiso 0.40 1 calc PR A 2 H22H H 0.4620 0.0716 0.5318 0.105 Uiso 0.40 1 calc PR A 2 H22I H 0.5053 0.1604 0.5217 0.105 Uiso 0.40 1 calc PR A 2 C215 C 0.3822(2) 0.5192(4) 0.31402(13) 0.0280(12) Uani 1 1 d . . . H21L H 0.3763 0.5029 0.2905 0.034 Uiso 1 1 calc R . . Ni3 Ni 0.39531(3) 0.65030(5) 0.428686(15) 0.02620(17) Uani 1 1 d . . . S31 S 0.41694(6) 0.65703(9) 0.37802(3) 0.0263(3) Uani 1 1 d . . . N31 N 0.3229(2) 0.7455(3) 0.41591(10) 0.0272(10) Uani 1 1 d . . . N32 N 0.3815(2) 0.6299(3) 0.47419(10) 0.0285(10) Uani 1 1 d . . . C31 C 0.3338(2) 0.6326(3) 0.35179(12) 0.0252(11) Uani 1 1 d . . . C32 C 0.3252(2) 0.5702(4) 0.32334(12) 0.0271(12) Uani 1 1 d . . . C33 C 0.2600(2) 0.5567(4) 0.30198(12) 0.0259(11) Uani 1 1 d . . . H33A H 0.2552 0.5158 0.2824 0.031 Uiso 1 1 calc R . . C34 C 0.2018(2) 0.6010(4) 0.30830(13) 0.0280(12) Uani 1 1 d . . . C35 C 0.2115(2) 0.6645(4) 0.33589(12) 0.0265(11) Uani 1 1 d . . . H35A H 0.1729 0.6984 0.3400 0.032 Uiso 1 1 calc R . . C36 C 0.2762(2) 0.6810(3) 0.35813(12) 0.0257(11) Uani 1 1 d . . . C37 C 0.2793(2) 0.7472(4) 0.38674(13) 0.0278(12) Uani 1 1 d . . . H37A H 0.2454 0.7971 0.3835 0.033 Uiso 1 1 calc R . . C38 C 0.3169(3) 0.8206(4) 0.44113(13) 0.0299(12) Uani 1 1 d . . . H38A H 0.2781 0.8646 0.4311 0.036 Uiso 1 1 calc R . . H38B H 0.3594 0.8604 0.4467 0.036 Uiso 1 1 calc R . . C309 C 0.3056(3) 0.7752(4) 0.47370(14) 0.0382(14) Uani 1 1 d . . . H30A H 0.2956 0.8279 0.4888 0.046 Uiso 1 1 calc R . . H30B H 0.2648 0.7322 0.4677 0.046 Uiso 1 1 calc R . . C310 C 0.3656(3) 0.7164(4) 0.49341(14) 0.0375(13) Uani 1 1 d . . . H31A H 0.4065 0.7591 0.4993 0.045 Uiso 1 1 calc R . . H31B H 0.3557 0.6939 0.5152 0.045 Uiso 1 1 calc R . . C311 C 0.1309(2) 0.5758(4) 0.28564(13) 0.0308(12) Uani 1 1 d . . . C312 C 0.1289(3) 0.5899(5) 0.24710(14) 0.0406(14) Uani 1 1 d . . . H31C H 0.1379 0.6586 0.2428 0.061 Uiso 1 1 calc R . . H31D H 0.0835 0.5715 0.2332 0.061 Uiso 1 1 calc R . . H31E H 0.1639 0.5485 0.2409 0.061 Uiso 1 1 calc R . . C313 C 0.1164(3) 0.4693(4) 0.29198(18) 0.0543(17) Uani 1 1 d . . . H31F H 0.1177 0.4598 0.3164 0.081 Uiso 1 1 calc R . . H31G H 0.1513 0.4279 0.2856 0.081 Uiso 1 1 calc R . . H31H H 0.0710 0.4514 0.2781 0.081 Uiso 1 1 calc R . . C314 C 0.0755(3) 0.6390(5) 0.29473(15) 0.0438(15) Uani 1 1 d . . . H31I H 0.0764 0.6306 0.3191 0.066 Uiso 1 1 calc R . . H31J H 0.0306 0.6192 0.2808 0.066 Uiso 1 1 calc R . . H31K H 0.0839 0.7078 0.2902 0.066 Uiso 1 1 calc R . . C315 C 0.3876(3) 0.5469(4) 0.49004(13) 0.0324(12) Uani 1 1 d . . . H31L H 0.3767 0.5470 0.5118 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.33893(7) 0.42191(9) 0.21986(3) 0.0367(3) Uani 1 1 d . . . O1A O 0.2748(2) 0.4562(4) 0.22522(13) 0.0684(13) Uani 1 1 d . . . O1B O 0.3635(3) 0.3479(4) 0.24436(14) 0.0927(18) Uani 1 1 d . . . O1C O 0.3855(2) 0.5015(3) 0.22478(13) 0.0624(12) Uani 1 1 d . . . O1D O 0.3291(3) 0.3823(4) 0.18672(12) 0.0795(16) Uani 1 1 d . . . Cl2 Cl 0.14378(7) 0.59776(11) 0.42870(4) 0.0433(4) Uani 1 1 d . . . O2A O 0.2047(2) 0.5644(3) 0.45168(12) 0.0683(14) Uani 1 1 d . . . O2B O 0.0907(2) 0.6115(3) 0.44633(12) 0.0641(13) Uani 1 1 d . . . O2C O 0.1215(2) 0.5277(5) 0.40225(15) 0.100(2) Uani 1 1 d . . . O2D O 0.1566(2) 0.6883(4) 0.41486(15) 0.0871(18) Uani 1 1 d . . . Cl3 Cl 0.66197(8) 0.55167(12) 0.41025(4) 0.0501(4) Uani 1 1 d . . . O3A O 0.7000(4) 0.6363(5) 0.42219(19) 0.133(3) Uani 1 1 d . . . O3B O 0.6479(3) 0.4921(5) 0.43603(14) 0.100(2) Uani 1 1 d . . . O3C O 0.6983(3) 0.4958(4) 0.39075(13) 0.0783(15) Uani 1 1 d . . . O3D O 0.5985(2) 0.5830(3) 0.38817(12) 0.0621(13) Uani 1 1 d . . . O1S O 0.2159(4) 0.4096(6) 0.3771(2) 0.0573(16) Uiso 0.50 1 d PD B 1 H1S H 0.2264 0.4513 0.3638 0.086 Uiso 0.50 1 d PR B 1 C1S C 0.2770(6) 0.3832(11) 0.4035(3) 0.0573(16) Uiso 0.50 1 d PD B 1 H1S1 H 0.3177 0.4138 0.3985 0.086 Uiso 0.50 1 d PR B 1 H1S2 H 0.2826 0.3120 0.4041 0.086 Uiso 0.50 1 d PR B 1 H1S3 H 0.2716 0.4061 0.4259 0.086 Uiso 0.50 1 d PR B 1 O2S O 0.2980(7) 0.5024(10) 0.4133(4) 0.0573(16) Uiso 0.30 1 d PD C 2 H2S H 0.2615 0.5331 0.4128 0.086 Uiso 0.30 1 d PR C 2 C2S C 0.2821(12) 0.4169(13) 0.3936(6) 0.0573(16) Uiso 0.30 1 d PD C 2 H2S1 H 0.2448 0.4312 0.3735 0.086 Uiso 0.30 1 d PR C 2 H2S2 H 0.2676 0.3651 0.4073 0.086 Uiso 0.30 1 d PR C 2 H2S3 H 0.3226 0.3952 0.3860 0.086 Uiso 0.30 1 d PR C 2 O3S O 0.3560(10) 0.2900(16) 0.3835(5) 0.0573(16) Uiso 0.20 1 d PD D 3 H3S H 0.3669 0.3318 0.3704 0.086 Uiso 0.20 1 d PR D 3 C3S C 0.3065(15) 0.333(2) 0.4006(8) 0.0573(16) Uiso 0.20 1 d PD D 3 H3S1 H 0.3023 0.4029 0.3949 0.086 Uiso 0.20 1 d PR D 3 H3S2 H 0.3220 0.3252 0.4255 0.086 Uiso 0.20 1 d PR D 3 H3S3 H 0.2618 0.3013 0.3924 0.086 Uiso 0.20 1 d PR D 3 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 0.0268(3) 0.0254(4) 0.0303(4) -0.0017(3) 0.0100(3) -0.0021(3) S11 0.0315(7) 0.0228(7) 0.0315(7) 0.0013(5) 0.0119(5) 0.0002(5) N11 0.027(2) 0.024(2) 0.034(3) -0.0008(19) 0.0084(18) -0.0012(17) N12 0.026(2) 0.029(2) 0.030(3) -0.0074(19) 0.0054(19) -0.0039(18) C11 0.026(3) 0.026(3) 0.032(3) 0.007(2) 0.017(2) 0.002(2) C12 0.027(3) 0.026(3) 0.025(3) 0.003(2) 0.009(2) -0.001(2) C13 0.031(3) 0.024(3) 0.026(3) 0.000(2) 0.005(2) -0.002(2) C14 0.030(3) 0.028(3) 0.027(3) 0.002(2) 0.011(2) -0.001(2) C15 0.029(3) 0.027(3) 0.031(3) 0.004(2) 0.009(2) 0.002(2) C16 0.028(3) 0.027(3) 0.024(3) 0.003(2) 0.011(2) -0.002(2) C17 0.025(3) 0.032(3) 0.033(3) 0.003(2) 0.011(2) 0.004(2) C18 0.025(3) 0.040(3) 0.036(3) -0.007(2) 0.005(2) -0.007(2) C19 0.028(3) 0.035(3) 0.036(3) -0.006(2) 0.004(2) -0.006(2) C110 0.032(3) 0.038(3) 0.031(3) -0.004(2) 0.008(2) -0.007(2) C111 0.029(3) 0.035(3) 0.030(3) -0.001(2) 0.008(2) -0.004(2) C112 0.065(4) 0.030(3) 0.046(4) -0.007(3) 0.025(3) -0.006(3) C113 0.046(4) 0.051(4) 0.055(4) -0.021(3) 0.019(3) 0.008(3) C114 0.052(4) 0.049(4) 0.037(4) -0.005(3) 0.020(3) 0.003(3) C115 0.034(3) 0.025(3) 0.027(3) -0.005(2) 0.007(2) 0.000(2) Ni2 0.0294(4) 0.0268(4) 0.0264(4) 0.0031(3) 0.0098(3) 0.0057(3) S21 0.0288(7) 0.0299(7) 0.0284(7) 0.0029(6) 0.0064(5) 0.0041(5) N21 0.036(2) 0.029(2) 0.024(3) 0.0017(19) 0.0106(19) 0.0076(19) N22 0.032(2) 0.026(2) 0.027(2) 0.0027(18) 0.0157(19) 0.0036(18) C21 0.030(3) 0.034(3) 0.027(3) 0.004(2) 0.000(2) 0.004(2) C22 0.039(3) 0.033(3) 0.021(3) 0.006(2) 0.007(2) 0.000(2) C23 0.042(3) 0.038(3) 0.027(3) 0.007(2) 0.007(2) -0.003(3) C24 0.050(3) 0.038(3) 0.028(3) 0.009(2) 0.002(3) 0.001(3) C25 0.060(4) 0.030(3) 0.033(3) 0.001(2) 0.007(3) 0.004(3) C26 0.037(3) 0.029(3) 0.030(3) 0.006(2) 0.001(2) 0.009(2) C27 0.044(3) 0.032(3) 0.033(3) -0.004(3) 0.004(3) 0.010(3) C28 0.044(3) 0.037(3) 0.042(4) -0.001(3) 0.020(3) 0.015(3) C29 0.044(3) 0.032(3) 0.038(3) 0.002(3) 0.017(3) 0.015(3) C210 0.036(3) 0.037(3) 0.031(3) 0.002(2) 0.016(2) 0.013(2) C211 0.068(4) 0.036(3) 0.037(4) 0.007(3) 0.016(3) -0.002(3) C215 0.030(3) 0.029(3) 0.027(3) -0.004(2) 0.009(2) 0.001(2) Ni3 0.0280(3) 0.0282(4) 0.0235(4) 0.0017(3) 0.0085(3) 0.0037(3) S31 0.0266(6) 0.0274(7) 0.0261(7) 0.0013(5) 0.0088(5) 0.0024(5) N31 0.034(2) 0.027(2) 0.024(2) -0.0002(18) 0.014(2) -0.0004(18) N32 0.029(2) 0.033(3) 0.024(2) 0.0021(19) 0.0076(18) -0.0005(18) C31 0.026(3) 0.028(3) 0.022(3) 0.013(2) 0.006(2) -0.001(2) C32 0.030(3) 0.027(3) 0.025(3) -0.001(2) 0.009(2) 0.003(2) C33 0.029(3) 0.027(3) 0.023(3) -0.002(2) 0.008(2) 0.001(2) C34 0.028(3) 0.024(3) 0.032(3) 0.009(2) 0.008(2) -0.001(2) C35 0.024(3) 0.030(3) 0.027(3) 0.001(2) 0.008(2) 0.004(2) C36 0.029(3) 0.023(3) 0.027(3) 0.004(2) 0.011(2) 0.007(2) C37 0.026(3) 0.023(3) 0.036(3) 0.003(2) 0.009(2) 0.002(2) C38 0.034(3) 0.025(3) 0.033(3) -0.006(2) 0.011(2) 0.006(2) C309 0.041(3) 0.043(3) 0.032(3) -0.004(3) 0.014(3) -0.002(3) C310 0.055(4) 0.036(3) 0.026(3) -0.006(2) 0.021(3) 0.007(3) C311 0.029(3) 0.027(3) 0.035(3) -0.005(2) 0.007(2) 0.002(2) C312 0.030(3) 0.061(4) 0.031(3) -0.007(3) 0.007(2) 0.003(3) C313 0.054(4) 0.038(4) 0.065(5) 0.007(3) 0.003(3) -0.015(3) C314 0.032(3) 0.054(4) 0.043(4) -0.015(3) 0.004(3) 0.002(3) C315 0.036(3) 0.037(3) 0.024(3) 0.004(2) 0.007(2) -0.003(2) Cl1 0.0402(8) 0.0305(7) 0.0399(8) -0.0066(6) 0.0101(6) -0.0019(6) O1A 0.042(3) 0.073(3) 0.096(4) -0.016(3) 0.029(2) -0.005(2) O1B 0.136(5) 0.050(3) 0.078(4) 0.011(3) -0.002(3) 0.014(3) O1C 0.052(3) 0.056(3) 0.085(3) -0.008(2) 0.029(2) -0.022(2) O1D 0.109(4) 0.077(4) 0.052(3) -0.039(3) 0.020(3) -0.002(3) Cl2 0.0411(8) 0.0428(9) 0.0437(9) -0.0013(7) 0.0057(7) -0.0012(6) O2A 0.061(3) 0.053(3) 0.079(3) 0.004(2) -0.009(2) 0.009(2) O2B 0.073(3) 0.066(3) 0.064(3) -0.008(2) 0.038(2) -0.011(2) O2C 0.049(3) 0.144(5) 0.101(4) -0.080(4) 0.005(3) -0.001(3) O2D 0.047(3) 0.092(4) 0.122(5) 0.066(3) 0.021(3) 0.008(3) Cl3 0.0540(10) 0.0578(10) 0.0433(9) -0.0025(8) 0.0207(7) 0.0015(8) O3A 0.143(6) 0.095(5) 0.128(6) -0.035(4) -0.034(4) -0.024(4) O3B 0.090(4) 0.163(6) 0.060(3) 0.048(4) 0.045(3) 0.033(4) O3C 0.079(3) 0.098(4) 0.073(4) 0.017(3) 0.049(3) 0.035(3) O3D 0.049(3) 0.068(3) 0.070(3) 0.020(2) 0.017(2) 0.010(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. 18.3852 (0.0090) x + 5.4670 (0.0133) y - 9.9699 (0.0398) z = 7.4688 (0.0170) Angle to previous plane (with approximate esd) = 84.59 ( 0.12 ) * 0.0196 (0.0015) N21 * -0.0199 (0.0015) N22 * -0.0196 (0.0015) S21 * 0.0198 (0.0015) S31 0.0554 (0.0018) Ni2 Rms deviation of fitted atoms = 0.0197 11.8083 (0.0163) x + 10.0926 (0.0096) y + 7.2052 (0.0399) z = 14.3059 (0.0124) * 0.0276 (0.0014) N31 * -0.0276 (0.0015) N32 * 0.0277 (0.0015) S21 * -0.0278 (0.0015) S31 0.0140 (0.0017) Ni3 Rms deviation of fitted atoms = 0.0277 5.0248 (0.0197) x + 13.0876 (0.0044) y + 3.1892 (0.0403) z = 12.0958 (0.0095) * 0.0149 (0.0014) N11 * -0.0151 (0.0014) N12 * -0.0153 (0.0014) S11 * 0.0155 (0.0014) S11_$1 -0.0337 (0.0017) Ni1 Rms deviation of fitted atoms = 0.0152 14.2901 (0.0293) x + 1.3604 (0.0287) y + 20.2442 (0.0713) z = 16.1670 (0.0226) * 0.0217 (0.0033) C21 * -0.0093 (0.0033) C22 * -0.0107 (0.0034) C23 * 0.0185 (0.0036) C24 * -0.0066 (0.0037) C25 * -0.0136 (0.0034) C26 Rms deviation of fitted atoms = 0.0144 -5.8345 (0.0378) x - 10.4773 (0.0181) y + 25.0682 (0.0642) z = 0.2343 (0.0317) Angle to previous plane (with approximate esd) = 83.41 ( 0.15 ) * 0.0088 (0.0033) C31 * 0.0001 (0.0034) C32 * -0.0142 (0.0034) C33 * 0.0194 (0.0034) C34 * -0.0108 (0.0034) C35 * -0.0033 (0.0033) C36 Rms deviation of fitted atoms = 0.0114 7.6454 (0.0371) x + 9.3604 (0.0196) y - 27.8210 (0.0578) z = 2.3121 (0.0364) * -0.0013 (0.0033) C11 * -0.0034 (0.0033) C12 * 0.0018 (0.0034) C13 * 0.0046 (0.0034) C14 * -0.0095 (0.0035) C15 * 0.0078 (0.0034) C16 Rms deviation of fitted atoms = 0.0056 -7.6455 (0.0370) x + 9.3604 (0.0196) y + 27.8210 (0.0578) z = 8.5771 (0.0278) Angle to previous plane (with approximate esd) = 86.44 ( 0.12 ) * -0.0013 (0.0033) C11_$1 * -0.0034 (0.0033) C12_$1 * 0.0018 (0.0034) C13_$1 * 0.0046 (0.0034) C14_$1 * -0.0095 (0.0035) C15_$1 * 0.0078 (0.0034) C16_$1 Rms deviation of fitted atoms = 0.0056 ; 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 N12 1.924(4) . ? Ni1 N11 1.927(4) . ? Ni1 S11 2.1597(14) 2_655 ? Ni1 S11 2.1659(14) . ? S11 C11 1.766(5) . ? S11 Ni1 2.1597(14) 2_655 ? N11 C17 1.280(6) . ? N11 C18 1.484(6) . ? N12 C115 1.289(6) . ? N12 C110 1.480(6) . ? C11 C12 1.384(7) . ? C11 C16 1.398(7) . ? C12 C13 1.409(7) . ? C12 C115 1.474(7) 2_655 ? C13 C14 1.391(7) . ? C13 H13A 0.9500 . ? C14 C15 1.392(7) . ? C14 C111 1.534(7) . ? C15 C16 1.396(7) . ? C15 H15A 0.9500 . ? C16 C17 1.467(7) . ? C17 H17A 0.9500 . ? C18 C19 1.508(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C110 1.517(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C114 1.530(8) . ? C111 C112 1.534(8) . ? C111 C113 1.534(8) . ? C112 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C113 H11F 0.9800 . ? C113 H11G 0.9800 . ? C113 H11H 0.9800 . ? C114 H11I 0.9800 . ? C114 H11J 0.9800 . ? C114 H11K 0.9800 . ? C115 C12 1.474(7) 2_655 ? C115 H11L 0.9500 . ? Ni2 N22 1.908(4) . ? Ni2 N21 1.928(4) . ? Ni2 S21 2.1682(15) . ? Ni2 S31 2.1774(14) . ? S21 C21 1.765(6) . ? S21 Ni3 2.1543(14) . ? N21 C27 1.276(7) . ? N21 C28 1.469(7) . ? N22 C215 1.282(6) . ? N22 C210 1.484(6) . ? C21 C26 1.384(7) . ? C21 C22 1.405(7) . ? C22 C23 1.388(7) . ? C22 C315 1.461(7) . ? C23 C24 1.394(8) . ? C23 H23A 0.9500 . ? C24 C25 1.388(8) . ? C24 C211 1.532(8) . ? C25 C26 1.399(8) . ? C25 H25A 0.9500 . ? C26 C27 1.467(8) . ? C27 H27A 0.9500 . ? C28 C29 1.503(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C210 1.509(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C223 1.490(10) . ? C211 C214 1.498(9) . ? C211 C213 1.545(9) . ? C211 C224 1.547(10) . ? C211 C222 1.549(10) . ? C211 C212 1.565(8) . ? C212 H21C 0.9800 . ? C212 H21D 0.9800 . ? C212 H21E 0.9800 . ? C213 H21F 0.9800 . ? C213 H21G 0.9800 . ? C213 H21H 0.9800 . ? C214 H21I 0.9800 . ? C214 H21J 0.9800 . ? C214 H21K 0.9800 . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C223 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? C224 H22G 0.9800 . ? C224 H22H 0.9800 . ? C224 H22I 0.9800 . ? C215 C32 1.462(7) . ? C215 H21L 0.9500 . ? Ni3 N31 1.927(4) . ? Ni3 N32 1.929(4) . ? Ni3 S31 2.1774(14) . ? S31 C31 1.779(5) . ? N31 C37 1.282(6) . ? N31 C38 1.465(6) . ? N32 C315 1.292(6) . ? N32 C310 1.486(7) . ? C31 C32 1.401(7) . ? C31 C36 1.406(7) . ? C32 C33 1.394(7) . ? C33 C34 1.392(7) . ? C33 H33A 0.9500 . ? C34 C35 1.382(7) . ? C34 C311 1.534(7) . ? C35 C36 1.408(7) . ? C35 H35A 0.9500 . ? C36 C37 1.450(7) . ? C37 H37A 0.9500 . ? C38 C309 1.511(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C309 C310 1.506(8) . ? C309 H30A 0.9900 . ? C309 H30B 0.9900 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C314 1.518(7) . ? C311 C313 1.518(8) . ? C311 C312 1.547(8) . ? C312 H31C 0.9800 . ? C312 H31D 0.9800 . ? C312 H31E 0.9800 . ? C313 H31F 0.9800 . ? C313 H31G 0.9800 . ? C313 H31H 0.9800 . ? C314 H31I 0.9800 . ? C314 H31J 0.9800 . ? C314 H31K 0.9800 . ? C315 H31L 0.9500 . ? Cl1 O1D 1.404(5) . ? Cl1 O1B 1.414(5) . ? Cl1 O1C 1.417(4) . ? Cl1 O1A 1.434(4) . ? Cl2 O2D 1.405(5) . ? Cl2 O2A 1.419(4) . ? Cl2 O2C 1.419(5) . ? Cl2 O2B 1.424(5) . ? Cl3 O3B 1.396(5) . ? Cl3 O3A 1.406(6) . ? Cl3 O3C 1.413(5) . ? Cl3 O3D 1.431(4) . ? O1S C1S 1.462(9) . ? O1S H1S 0.8399 . ? C1S H1S1 0.9799 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9801 . ? O2S C2S 1.404(10) . ? O2S H2S 0.8400 . ? C2S H2S1 0.9799 . ? C2S H2S2 0.9802 . ? C2S H2S3 0.9800 . ? O3S C3S 1.459(10) . ? O3S H3S 0.8400 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9802 . ? C3S H3S3 0.9801 . ? 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 N12 Ni1 N11 95.77(17) . . ? N12 Ni1 S11 91.37(13) . 2_655 ? N11 Ni1 S11 172.32(13) . 2_655 ? N12 Ni1 S11 171.48(13) . . ? N11 Ni1 S11 92.65(13) . . ? S11 Ni1 S11 80.16(6) 2_655 . ? C11 S11 Ni1 102.83(16) . 2_655 ? C11 S11 Ni1 103.70(16) . . ? Ni1 S11 Ni1 94.95(6) 2_655 . ? C17 N11 C18 115.9(4) . . ? C17 N11 Ni1 125.6(3) . . ? C18 N11 Ni1 118.4(3) . . ? C115 N12 C110 116.7(4) . . ? C115 N12 Ni1 126.9(3) . . ? C110 N12 Ni1 116.5(3) . . ? C12 C11 C16 119.7(5) . . ? C12 C11 S11 120.9(4) . . ? C16 C11 S11 119.1(4) . . ? C11 C12 C13 119.6(4) . . ? C11 C12 C115 123.7(5) . 2_655 ? C13 C12 C115 116.6(4) . 2_655 ? C14 C13 C12 121.9(4) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C13 C14 C15 117.0(5) . . ? C13 C14 C111 121.0(4) . . ? C15 C14 C111 122.0(4) . . ? C14 C15 C16 122.4(5) . . ? C14 C15 H15A 118.8 . . ? C16 C15 H15A 118.8 . . ? C15 C16 C11 119.3(4) . . ? C15 C16 C17 115.9(4) . . ? C11 C16 C17 124.8(5) . . ? N11 C17 C16 127.2(5) . . ? N11 C17 H17A 116.4 . . ? C16 C17 H17A 116.4 . . ? N11 C18 C19 112.7(4) . . ? N11 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? N11 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C110 113.7(4) . . ? C18 C19 H19A 108.8 . . ? C110 C19 H19A 108.8 . . ? C18 C19 H19B 108.8 . . ? C110 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? N12 C110 C19 110.8(4) . . ? N12 C110 H11A 109.5 . . ? C19 C110 H11A 109.5 . . ? N12 C110 H11B 109.5 . . ? C19 C110 H11B 109.5 . . ? H11A C110 H11B 108.1 . . ? C114 C111 C112 109.4(4) . . ? C114 C111 C113 108.8(5) . . ? C112 C111 C113 108.4(5) . . ? C114 C111 C14 110.1(4) . . ? C112 C111 C14 108.6(4) . . ? C113 C111 C14 111.5(4) . . ? C111 C112 H11C 109.5 . . ? C111 C112 H11D 109.5 . . ? H11C C112 H11D 109.5 . . ? C111 C112 H11E 109.5 . . ? H11C C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C111 C113 H11F 109.5 . . ? C111 C113 H11G 109.5 . . ? H11F C113 H11G 109.5 . . ? C111 C113 H11H 109.5 . . ? H11F C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C111 C114 H11I 109.5 . . ? C111 C114 H11J 109.5 . . ? H11I C114 H11J 109.5 . . ? C111 C114 H11K 109.5 . . ? H11I C114 H11K 109.5 . . ? H11J C114 H11K 109.5 . . ? N12 C115 C12 125.3(5) . 2_655 ? N12 C115 H11L 117.3 . . ? C12 C115 H11L 117.3 2_655 . ? N22 Ni2 N21 94.34(17) . . ? N22 Ni2 S21 171.44(13) . . ? N21 Ni2 S21 93.01(13) . . ? N22 Ni2 S31 91.69(12) . . ? N21 Ni2 S31 173.57(13) . . ? S21 Ni2 S31 80.81(5) . . ? C21 S21 Ni3 104.21(18) . . ? C21 S21 Ni2 103.47(18) . . ? Ni3 S21 Ni2 94.40(5) . . ? C27 N21 C28 116.7(4) . . ? C27 N21 Ni2 125.3(4) . . ? C28 N21 Ni2 118.0(3) . . ? C215 N22 C210 116.5(4) . . ? C215 N22 Ni2 125.7(4) . . ? C210 N22 Ni2 117.8(3) . . ? C26 C21 C22 119.7(5) . . ? C26 C21 S21 119.5(4) . . ? C22 C21 S21 120.6(4) . . ? C23 C22 C21 119.3(5) . . ? C23 C22 C315 116.9(5) . . ? C21 C22 C315 123.7(5) . . ? C22 C23 C24 122.6(5) . . ? C22 C23 H23A 118.7 . . ? C24 C23 H23A 118.7 . . ? C25 C24 C23 116.2(5) . . ? C25 C24 C211 122.2(5) . . ? C23 C24 C211 121.6(5) . . ? C24 C25 C26 123.2(5) . . ? C24 C25 H25A 118.4 . . ? C26 C25 H25A 118.4 . . ? C21 C26 C25 118.8(5) . . ? C21 C26 C27 124.6(5) . . ? C25 C26 C27 116.5(5) . . ? N21 C27 C26 128.3(5) . . ? N21 C27 H27A 115.8 . . ? C26 C27 H27A 115.8 . . ? N21 C28 C29 112.7(4) . . ? N21 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? N21 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C28 C29 C210 112.5(5) . . ? C28 C29 H29A 109.1 . . ? C210 C29 H29A 109.1 . . ? C28 C29 H29B 109.1 . . ? C210 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? N22 C210 C29 110.3(4) . . ? N22 C210 H21A 109.6 . . ? C29 C210 H21A 109.6 . . ? N22 C210 H21B 109.6 . . ? C29 C210 H21B 109.6 . . ? H21A C210 H21B 108.1 . . ? C223 C211 C24 117.1(9) . . ? C214 C211 C24 115.9(7) . . ? C214 C211 C213 110.7(6) . . ? C24 C211 C213 108.6(6) . . ? C223 C211 C224 111.1(7) . . ? C24 C211 C224 106.9(8) . . ? C223 C211 C222 110.0(7) . . ? C24 C211 C222 105.5(8) . . ? C224 C211 C222 105.5(7) . . ? C214 C211 C212 108.9(6) . . ? C24 C211 C212 106.8(5) . . ? C213 C211 C212 105.4(5) . . ? C211 C212 H21C 109.5 . . ? C211 C212 H21D 109.5 . . ? H21C C212 H21D 109.5 . . ? C211 C212 H21E 109.5 . . ? H21C C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C211 C213 H21F 109.5 . . ? C211 C213 H21G 109.5 . . ? H21F C213 H21G 109.5 . . ? C211 C213 H21H 109.5 . . ? H21F C213 H21H 109.5 . . ? H21G C213 H21H 109.5 . . ? C211 C214 H21I 109.5 . . ? C211 C214 H21J 109.5 . . ? H21I C214 H21J 109.5 . . ? C211 C214 H21K 109.5 . . ? H21I C214 H21K 109.5 . . ? H21J C214 H21K 109.5 . . ? C211 C222 H22A 109.5 . . ? C211 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C211 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C211 C223 H22D 109.5 . . ? C211 C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C211 C223 H22F 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C211 C224 H22G 109.5 . . ? C211 C224 H22H 109.5 . . ? H22G C224 H22H 109.5 . . ? C211 C224 H22I 109.5 . . ? H22G C224 H22I 109.5 . . ? H22H C224 H22I 109.5 . . ? N22 C215 C32 127.2(5) . . ? N22 C215 H21L 116.4 . . ? C32 C215 H21L 116.4 . . ? N31 Ni3 N32 94.53(17) . . ? N31 Ni3 S21 172.75(13) . . ? N32 Ni3 S21 92.69(13) . . ? N31 Ni3 S31 91.68(13) . . ? N32 Ni3 S31 173.38(13) . . ? S21 Ni3 S31 81.13(5) . . ? C31 S31 Ni2 102.14(17) . . ? C31 S31 Ni3 100.11(17) . . ? Ni2 S31 Ni3 93.48(5) . . ? C37 N31 C38 117.8(4) . . ? C37 N31 Ni3 124.2(3) . . ? C38 N31 Ni3 118.0(3) . . ? C315 N32 C310 116.8(4) . . ? C315 N32 Ni3 125.0(4) . . ? C310 N32 Ni3 118.2(3) . . ? C32 C31 C36 119.1(4) . . ? C32 C31 S31 120.7(4) . . ? C36 C31 S31 120.0(4) . . ? C33 C32 C31 119.7(4) . . ? C33 C32 C215 117.2(4) . . ? C31 C32 C215 123.1(4) . . ? C34 C33 C32 122.4(5) . . ? C34 C33 H33A 118.8 . . ? C32 C33 H33A 118.8 . . ? C35 C34 C33 117.1(4) . . ? C35 C34 C311 123.2(4) . . ? C33 C34 C311 119.7(4) . . ? C34 C35 C36 122.6(4) . . ? C34 C35 H35A 118.7 . . ? C36 C35 H35A 118.7 . . ? C31 C36 C35 119.0(4) . . ? C31 C36 C37 123.7(4) . . ? C35 C36 C37 117.3(4) . . ? N31 C37 C36 126.9(4) . . ? N31 C37 H37A 116.6 . . ? C36 C37 H37A 116.6 . . ? N31 C38 C309 111.2(4) . . ? N31 C38 H38A 109.4 . . ? C309 C38 H38A 109.4 . . ? N31 C38 H38B 109.4 . . ? C309 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C310 C309 C38 113.9(4) . . ? C310 C309 H30A 108.8 . . ? C38 C309 H30A 108.8 . . ? C310 C309 H30B 108.8 . . ? C38 C309 H30B 108.8 . . ? H30A C309 H30B 107.7 . . ? N32 C310 C309 113.4(4) . . ? N32 C310 H31A 108.9 . . ? C309 C310 H31A 108.9 . . ? N32 C310 H31B 108.9 . . ? C309 C310 H31B 108.9 . . ? H31A C310 H31B 107.7 . . ? C314 C311 C313 109.0(5) . . ? C314 C311 C34 111.0(4) . . ? C313 C311 C34 107.7(4) . . ? C314 C311 C312 108.8(4) . . ? C313 C311 C312 109.0(5) . . ? C34 C311 C312 111.3(4) . . ? C311 C312 H31C 109.5 . . ? C311 C312 H31D 109.5 . . ? H31C C312 H31D 109.5 . . ? C311 C312 H31E 109.5 . . ? H31C C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? C311 C313 H31F 109.5 . . ? C311 C313 H31G 109.5 . . ? H31F C313 H31G 109.5 . . ? C311 C313 H31H 109.5 . . ? H31F C313 H31H 109.5 . . ? H31G C313 H31H 109.5 . . ? C311 C314 H31I 109.5 . . ? C311 C314 H31J 109.5 . . ? H31I C314 H31J 109.5 . . ? C311 C314 H31K 109.5 . . ? H31I C314 H31K 109.5 . . ? H31J C314 H31K 109.5 . . ? N32 C315 C22 128.4(5) . . ? N32 C315 H31L 115.8 . . ? C22 C315 H31L 115.8 . . ? O1D Cl1 O1B 109.2(3) . . ? O1D Cl1 O1C 111.5(3) . . ? O1B Cl1 O1C 110.1(3) . . ? O1D Cl1 O1A 109.8(3) . . ? O1B Cl1 O1A 107.8(4) . . ? O1C Cl1 O1A 108.3(3) . . ? O2D Cl2 O2A 109.2(3) . . ? O2D Cl2 O2C 110.8(4) . . ? O2A Cl2 O2C 109.7(3) . . ? O2D Cl2 O2B 108.0(3) . . ? O2A Cl2 O2B 110.5(3) . . ? O2C Cl2 O2B 108.6(3) . . ? O3B Cl3 O3A 114.7(5) . . ? O3B Cl3 O3C 108.4(4) . . ? O3A Cl3 O3C 108.9(4) . . ? O3B Cl3 O3D 108.9(3) . . ? O3A Cl3 O3D 107.2(4) . . ? O3C Cl3 O3D 108.6(3) . . ? C1S O1S H1S 109.3 . . ? O1S C1S H1S1 110.0 . . ? O1S C1S H1S2 109.4 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.0 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 108.8 . . ? O2S C2S H2S1 108.9 . . ? O2S C2S H2S2 110.2 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.4 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C3S O3S H3S 109.1 . . ? O3S C3S H3S1 108.3 . . ? O3S C3S H3S2 110.3 . . ? H3S1 C3S H3S2 109.5 . . ? O3S C3S H3S3 109.7 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Ni1 S11 C11 -49.3(2) . . . . ? S11 Ni1 S11 C11 127.97(16) 2_655 . . . ? N11 Ni1 S11 Ni1 -153.83(12) . . . 2_655 ? S11 Ni1 S11 Ni1 23.46(7) 2_655 . . 2_655 ? N12 Ni1 N11 C17 -145.1(4) . . . . ? S11 Ni1 N11 C17 33.7(4) . . . . ? N12 Ni1 N11 C18 38.6(4) . . . . ? S11 Ni1 N11 C18 -142.6(3) . . . . ? N11 Ni1 N12 C115 139.5(4) . . . . ? S11 Ni1 N12 C115 -37.7(4) 2_655 . . . ? N11 Ni1 N12 C110 -42.6(4) . . . . ? S11 Ni1 N12 C110 140.3(3) 2_655 . . . ? Ni1 S11 C11 C12 -43.7(4) 2_655 . . . ? Ni1 S11 C11 C12 -142.2(4) . . . . ? Ni1 S11 C11 C16 142.5(4) 2_655 . . . ? Ni1 S11 C11 C16 44.1(4) . . . . ? C16 C11 C12 C13 0.1(7) . . . . ? S11 C11 C12 C13 -173.6(4) . . . . ? C16 C11 C12 C115 176.8(4) . . . 2_655 ? S11 C11 C12 C115 3.0(7) . . . 2_655 ? C11 C12 C13 C14 0.2(7) . . . . ? C115 C12 C13 C14 -176.7(4) 2_655 . . . ? C12 C13 C14 C15 0.5(7) . . . . ? C12 C13 C14 C111 -178.6(5) . . . . ? C13 C14 C15 C16 -1.6(7) . . . . ? C111 C14 C15 C16 177.5(5) . . . . ? C14 C15 C16 C11 2.0(7) . . . . ? C14 C15 C16 C17 -179.5(5) . . . . ? C12 C11 C16 C15 -1.1(7) . . . . ? S11 C11 C16 C15 172.7(4) . . . . ? C12 C11 C16 C17 -179.5(5) . . . . ? S11 C11 C16 C17 -5.7(7) . . . . ? C18 N11 C17 C16 179.4(5) . . . . ? Ni1 N11 C17 C16 3.1(7) . . . . ? C15 C16 C17 N11 155.4(5) . . . . ? C11 C16 C17 N11 -26.2(8) . . . . ? C17 N11 C18 C19 131.1(5) . . . . ? Ni1 N11 C18 C19 -52.3(5) . . . . ? N11 C18 C19 C110 64.3(6) . . . . ? C115 N12 C110 C19 -121.5(5) . . . . ? Ni1 N12 C110 C19 60.3(5) . . . . ? C18 C19 C110 N12 -68.7(6) . . . . ? C13 C14 C111 C114 -47.6(6) . . . . ? C15 C14 C111 C114 133.3(5) . . . . ? C13 C14 C111 C112 72.1(6) . . . . ? C15 C14 C111 C112 -106.9(5) . . . . ? C13 C14 C111 C113 -168.4(5) . . . . ? C15 C14 C111 C113 12.5(7) . . . . ? C110 N12 C115 C12 -177.9(4) . . . 2_655 ? Ni1 N12 C115 C12 0.1(7) . . . 2_655 ? N21 Ni2 S21 C21 -48.4(2) . . . . ? S31 Ni2 S21 C21 129.76(18) . . . . ? N21 Ni2 S21 Ni3 -154.20(13) . . . . ? S31 Ni2 S21 Ni3 24.00(5) . . . . ? N22 Ni2 N21 C27 -143.0(4) . . . . ? S21 Ni2 N21 C27 32.6(4) . . . . ? N22 Ni2 N21 C28 40.4(4) . . . . ? S21 Ni2 N21 C28 -144.0(3) . . . . ? N21 Ni2 N22 C215 137.7(4) . . . . ? S31 Ni2 N22 C215 -40.1(4) . . . . ? N21 Ni2 N22 C210 -43.1(4) . . . . ? S31 Ni2 N22 C210 139.2(3) . . . . ? Ni3 S21 C21 C26 144.0(4) . . . . ? Ni2 S21 C21 C26 45.9(4) . . . . ? Ni3 S21 C21 C22 -42.1(4) . . . . ? Ni2 S21 C21 C22 -140.3(4) . . . . ? C26 C21 C22 C23 3.0(7) . . . . ? S21 C21 C22 C23 -170.8(4) . . . . ? C26 C21 C22 C315 179.4(4) . . . . ? S21 C21 C22 C315 5.5(7) . . . . ? C21 C22 C23 C24 0.0(7) . . . . ? C315 C22 C23 C24 -176.5(5) . . . . ? C22 C23 C24 C25 -2.6(8) . . . . ? C22 C23 C24 C211 176.7(5) . . . . ? C23 C24 C25 C26 2.2(8) . . . . ? C211 C24 C25 C26 -177.1(5) . . . . ? C22 C21 C26 C25 -3.4(7) . . . . ? S21 C21 C26 C25 170.5(4) . . . . ? C22 C21 C26 C27 175.7(4) . . . . ? S21 C21 C26 C27 -10.4(7) . . . . ? C24 C25 C26 C21 0.8(8) . . . . ? C24 C25 C26 C27 -178.4(5) . . . . ? C28 N21 C27 C26 178.6(5) . . . . ? Ni2 N21 C27 C26 1.9(8) . . . . ? C21 C26 C27 N21 -21.6(8) . . . . ? C25 C26 C27 N21 157.5(5) . . . . ? C27 N21 C28 C29 127.4(5) . . . . ? Ni2 N21 C28 C29 -55.7(6) . . . . ? N21 C28 C29 C210 66.4(6) . . . . ? C215 N22 C210 C29 -120.3(5) . . . . ? Ni2 N22 C210 C29 60.4(5) . . . . ? C28 C29 C210 N22 -68.0(6) . . . . ? C25 C24 C211 C223 163.5(9) . . . . ? C23 C24 C211 C223 -15.8(10) . . . . ? C25 C24 C211 C214 -0.4(9) . . . . ? C23 C24 C211 C214 -179.7(7) . . . . ? C25 C24 C211 C213 -125.6(6) . . . . ? C23 C24 C211 C213 55.1(7) . . . . ? C25 C24 C211 C224 38.2(9) . . . . ? C23 C24 C211 C224 -141.1(8) . . . . ? C25 C24 C211 C222 -73.8(8) . . . . ? C23 C24 C211 C222 106.9(8) . . . . ? C25 C24 C211 C212 121.1(6) . . . . ? C23 C24 C211 C212 -58.2(7) . . . . ? C210 N22 C215 C32 -176.8(5) . . . . ? Ni2 N22 C215 C32 2.5(7) . . . . ? C21 S21 Ni3 N32 48.5(2) . . . . ? Ni2 S21 Ni3 N32 153.64(13) . . . . ? C21 S21 Ni3 S31 -129.08(18) . . . . ? Ni2 S21 Ni3 S31 -23.97(5) . . . . ? N22 Ni2 S31 C31 51.0(2) . . . . ? S21 Ni2 S31 C31 -124.82(17) . . . . ? N22 Ni2 S31 Ni3 152.16(13) . . . . ? S21 Ni2 S31 Ni3 -23.70(5) . . . . ? N31 Ni3 S31 C31 -54.1(2) . . . . ? S21 Ni3 S31 C31 126.83(17) . . . . ? N31 Ni3 S31 Ni2 -157.07(12) . . . . ? S21 Ni3 S31 Ni2 23.84(5) . . . . ? N32 Ni3 N31 C37 -136.6(4) . . . . ? S31 Ni3 N31 C37 41.1(4) . . . . ? N32 Ni3 N31 C38 43.2(4) . . . . ? S31 Ni3 N31 C38 -139.1(3) . . . . ? N31 Ni3 N32 C315 143.5(4) . . . . ? S21 Ni3 N32 C315 -37.1(4) . . . . ? N31 Ni3 N32 C310 -39.5(4) . . . . ? S21 Ni3 N32 C310 139.9(3) . . . . ? Ni2 S31 C31 C32 -42.3(4) . . . . ? Ni3 S31 C31 C32 -138.1(4) . . . . ? Ni2 S31 C31 C36 141.8(4) . . . . ? Ni3 S31 C31 C36 46.0(4) . . . . ? C36 C31 C32 C33 -0.3(7) . . . . ? S31 C31 C32 C33 -176.2(4) . . . . ? C36 C31 C32 C215 177.9(4) . . . . ? S31 C31 C32 C215 2.0(7) . . . . ? N22 C215 C32 C33 -155.1(5) . . . . ? N22 C215 C32 C31 26.6(8) . . . . ? C31 C32 C33 C34 -1.9(7) . . . . ? C215 C32 C33 C34 179.7(5) . . . . ? C32 C33 C34 C35 3.7(7) . . . . ? C32 C33 C34 C311 -174.5(5) . . . . ? C33 C34 C35 C36 -3.4(7) . . . . ? C311 C34 C35 C36 174.7(5) . . . . ? C32 C31 C36 C35 0.6(7) . . . . ? S31 C31 C36 C35 176.5(4) . . . . ? C32 C31 C36 C37 -179.9(5) . . . . ? S31 C31 C36 C37 -4.0(7) . . . . ? C34 C35 C36 C31 1.3(7) . . . . ? C34 C35 C36 C37 -178.2(5) . . . . ? C38 N31 C37 C36 179.3(5) . . . . ? Ni3 N31 C37 C36 -1.0(7) . . . . ? C31 C36 C37 N31 -27.9(8) . . . . ? C35 C36 C37 N31 151.6(5) . . . . ? C37 N31 C38 C309 120.3(5) . . . . ? Ni3 N31 C38 C309 -59.5(5) . . . . ? N31 C38 C309 C310 66.1(6) . . . . ? C315 N32 C310 C309 -129.3(5) . . . . ? Ni3 N32 C310 C309 53.4(6) . . . . ? C38 C309 C310 N32 -63.3(6) . . . . ? C35 C34 C311 C314 7.3(7) . . . . ? C33 C34 C311 C314 -174.7(5) . . . . ? C35 C34 C311 C313 -112.0(6) . . . . ? C33 C34 C311 C313 66.1(6) . . . . ? C35 C34 C311 C312 128.6(5) . . . . ? C33 C34 C311 C312 -53.3(6) . . . . ? C310 N32 C315 C22 -173.6(5) . . . . ? Ni3 N32 C315 C22 3.5(7) . . . . ? C23 C22 C315 N32 -162.3(5) . . . . ? C21 C22 C315 N32 21.3(8) . . . . ? #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 282072' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C30 H38 N4 Ni2 S2 2+, 2(Cl O4 -), 0.5(C3 H7 N O), 0.5(C H4 O) ; _chemical_formula_sum 'C32 H43.50 Cl2 N4.50 Ni2 O9 S2' _chemical_formula_weight 887.65 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' S S 0.1246 0.1234 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.373(2) _cell_length_b 13.331(2) _cell_length_c 15.212(3) _cell_angle_alpha 102.565(4) _cell_angle_beta 100.972(4) _cell_angle_gamma 117.638(4) _cell_volume 2042.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5140 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 25.64 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 922 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.538 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.551574 ; _exptl_special_details ; Relatively high residual electron density associated with Ni atoms. DMF and methanol moieties included with half occupancy solely to provide satisfactory displacement parameters. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 17012 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _reflns_number_total 7118 _reflns_number_gt 5053 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-8 (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1443P)^2^+4.8208P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7118 _refine_ls_number_parameters 462 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.2101 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.100 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.142 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.17951(7) 0.22336(7) 0.32763(5) 0.0308(3) Uani 1 1 d . . . Ni2 Ni 0.32304(7) 0.23571(7) 0.17527(5) 0.0306(3) Uani 1 1 d . . . S1 S 0.35519(14) 0.35579(14) 0.31152(11) 0.0323(4) Uani 1 1 d . . . S2 S 0.12605(14) 0.16129(14) 0.17393(11) 0.0312(4) Uani 1 1 d . . . N1 N 0.2498(5) 0.2993(5) 0.4642(4) 0.0355(12) Uani 1 1 d . . . N2 N 0.0146(5) 0.0941(5) 0.3222(4) 0.0339(12) Uani 1 1 d . . . N3 N 0.2703(5) 0.1202(5) 0.0524(3) 0.0310(11) Uani 1 1 d . . . N4 N 0.5061(5) 0.3187(5) 0.1943(4) 0.0338(12) Uani 1 1 d . . . C1 C 0.4772(6) 0.3522(6) 0.3912(4) 0.0327(14) Uani 1 1 d . . . C2 C 0.5827(6) 0.3602(6) 0.3663(4) 0.0345(14) Uani 1 1 d . . . C3 C 0.6843(6) 0.3687(6) 0.4337(5) 0.0384(15) Uani 1 1 d . . . H3A H 0.7563 0.3746 0.4164 0.046 Uiso 1 1 calc R . . C4 C 0.6828(6) 0.3686(6) 0.5255(5) 0.0401(15) Uani 1 1 d . . . C5 C 0.5762(6) 0.3613(6) 0.5476(5) 0.0368(15) Uani 1 1 d . . . H5A H 0.5732 0.3622 0.6097 0.044 Uiso 1 1 calc R . . C6 C 0.4733(6) 0.3526(6) 0.4827(4) 0.0365(15) Uani 1 1 d . . . C7 C 0.3680(6) 0.3461(6) 0.5164(5) 0.0352(14) Uani 1 1 d . . . H7A H 0.3889 0.3798 0.5835 0.042 Uiso 1 1 calc R . . C8 C 0.1626(6) 0.3061(6) 0.5161(5) 0.0417(16) Uani 1 1 d . . . H8A H 0.1332 0.3585 0.4980 0.050 Uiso 1 1 calc R . . H8B H 0.2105 0.3427 0.5858 0.050 Uiso 1 1 calc R . . C9 C 0.0456(6) 0.1810(6) 0.4933(5) 0.0402(16) Uani 1 1 d . . . H9A H 0.0761 0.1270 0.5055 0.048 Uiso 1 1 calc R . . H9B H -0.0027 0.1869 0.5371 0.048 Uiso 1 1 calc R . . C10 C -0.0445(6) 0.1254(7) 0.3927(5) 0.0437(17) Uani 1 1 d . . . H10J H -0.0688 0.1826 0.3780 0.052 Uiso 1 1 calc R . . H10K H -0.1246 0.0512 0.3860 0.052 Uiso 1 1 calc R . . C11 C 0.7905(7) 0.3759(8) 0.5992(5) 0.0496(18) Uani 1 1 d . . . C12 C 0.8435(11) 0.4838(13) 0.6864(7) 0.107(5) Uani 1 1 d . . . H12A H 0.7731 0.4788 0.7095 0.161 Uiso 1 1 calc R . . H12B H 0.8837 0.5573 0.6707 0.161 Uiso 1 1 calc R . . H12C H 0.9087 0.4860 0.7362 0.161 Uiso 1 1 calc R . . C13 C 0.8987(11) 0.3837(16) 0.5636(7) 0.126(6) Uani 1 1 d . . . H13A H 0.9348 0.4543 0.5438 0.189 Uiso 1 1 calc R . . H13B H 0.8651 0.3102 0.5088 0.189 Uiso 1 1 calc R . . H13C H 0.9668 0.3916 0.6148 0.189 Uiso 1 1 calc R . . C14 C 0.7339(12) 0.2663(13) 0.6302(11) 0.132(6) Uani 1 1 d . . . H14A H 0.6634 0.2616 0.6530 0.197 Uiso 1 1 calc R . . H14B H 0.8017 0.2744 0.6818 0.197 Uiso 1 1 calc R . . H14C H 0.7003 0.1926 0.5757 0.197 Uiso 1 1 calc R . . C15 C -0.0520(6) -0.0119(6) 0.2623(5) 0.0359(15) Uani 1 1 d . . . H15A H -0.1317 -0.0642 0.2693 0.043 Uiso 1 1 calc R . . C16 C 0.0641(5) 0.0052(6) 0.1407(4) 0.0324(14) Uani 1 1 d . . . C17 C -0.0211(6) -0.0636(6) 0.1836(4) 0.0324(14) Uani 1 1 d . . . C18 C -0.0829(6) -0.1887(6) 0.1475(5) 0.0382(15) Uani 1 1 d . . . H18A H -0.1407 -0.2344 0.1761 0.046 Uiso 1 1 calc R . . C19 C -0.0640(6) -0.2513(6) 0.0698(5) 0.0364(14) Uani 1 1 d . . . C20 C 0.0238(6) -0.1792(6) 0.0330(5) 0.0363(15) Uani 1 1 d . . . H20A H 0.0402 -0.2176 -0.0186 0.044 Uiso 1 1 calc R . . C21 C 0.0892(6) -0.0537(6) 0.0674(4) 0.0308(13) Uani 1 1 d . . . C22 C 0.1779(6) 0.0092(6) 0.0192(4) 0.0334(14) Uani 1 1 d . . . H22A H 0.1653 -0.0374 -0.0429 0.040 Uiso 1 1 calc R . . C23 C 0.3384(6) 0.1615(6) -0.0154(4) 0.0364(15) Uani 1 1 d . . . H23A H 0.3184 0.2190 -0.0347 0.044 Uiso 1 1 calc R . . H23B H 0.3059 0.0911 -0.0737 0.044 Uiso 1 1 calc R . . C24 C 0.4836(6) 0.2222(6) 0.0285(5) 0.0396(16) Uani 1 1 d . . . H24A H 0.5025 0.1657 0.0508 0.047 Uiso 1 1 calc R . . H24B H 0.5231 0.2383 -0.0216 0.047 Uiso 1 1 calc R . . C25 C 0.5457(6) 0.3381(7) 0.1105(5) 0.0429(17) Uani 1 1 d . . . H25A H 0.6410 0.3781 0.1291 0.051 Uiso 1 1 calc R . . H25B H 0.5214 0.3927 0.0901 0.051 Uiso 1 1 calc R . . C26 C -0.1367(7) -0.3878(6) 0.0330(5) 0.0418(16) Uani 1 1 d . . . C27 C -0.1074(8) -0.4308(8) 0.1137(6) 0.059(2) Uani 1 1 d . . . H27A H -0.0144 -0.4000 0.1370 0.089 Uiso 1 1 calc R . . H27B H -0.1563 -0.5194 0.0903 0.089 Uiso 1 1 calc R . . H27C H -0.1325 -0.4008 0.1660 0.089 Uiso 1 1 calc R . . C28 C -0.1016(9) -0.4368(7) -0.0508(6) 0.061(2) Uani 1 1 d . . . H28A H -0.0086 -0.4063 -0.0296 0.091 Uiso 1 1 calc R . . H28B H -0.1229 -0.4100 -0.1030 0.091 Uiso 1 1 calc R . . H28C H -0.1507 -0.5254 -0.0732 0.091 Uiso 1 1 calc R . . C29 C -0.2850(7) -0.4378(7) -0.0033(6) 0.058(2) Uani 1 1 d . . . H29A H -0.3097 -0.4077 0.0492 0.087 Uiso 1 1 calc R . . H29B H -0.3333 -0.5264 -0.0264 0.087 Uiso 1 1 calc R . . H29C H -0.3050 -0.4106 -0.0556 0.087 Uiso 1 1 calc R . . C30 C 0.5961(6) 0.3609(6) 0.2731(5) 0.0371(15) Uani 1 1 d . . . H30A H 0.6819 0.3970 0.2712 0.045 Uiso 1 1 calc R . . Cl1 Cl 0.3894(2) 0.30920(19) 0.75431(14) 0.0616(6) Uani 1 1 d D . . O1A O 0.3873(6) 0.2802(7) 0.8368(4) 0.087(2) Uani 1 1 d D . . O1B O 0.3421(13) 0.3866(10) 0.7526(7) 0.195(7) Uani 1 1 d D . . O1C O 0.5141(6) 0.3646(9) 0.7512(5) 0.166(6) Uani 1 1 d D . . O1D O 0.3048(6) 0.2072(5) 0.6720(4) 0.085(2) Uani 1 1 d D . . Cl2 Cl 0.7901(2) 0.2163(2) 0.18813(16) 0.0635(6) Uani 1 1 d D . . O2A O 0.6654(7) 0.1130(7) 0.1355(8) 0.179(6) Uani 1 1 d D . . O2B O 0.8089(9) 0.2995(10) 0.1425(10) 0.197(6) Uani 1 1 d D . . O2C O 0.8798(8) 0.1829(9) 0.1929(5) 0.148(5) Uani 1 1 d D . . O2D O 0.7955(11) 0.2646(11) 0.2807(6) 0.176(5) Uani 1 1 d D . . O100 O 0.2524(16) 0.0736(15) 0.3613(12) 0.108(5) Uiso 0.50 1 d PD . . H100 H 0.2893 0.0565 0.3240 0.162 Uiso 0.50 1 d PR . . C100 C 0.252(2) 0.030(2) 0.4383(15) 0.105(8) Uiso 0.50 1 d PD . . H10A H 0.3326 0.0323 0.4638 0.157 Uiso 0.50 1 d PR . . H10B H 0.1785 -0.0537 0.4156 0.157 Uiso 0.50 1 d PR . . H10C H 0.2415 0.0806 0.4889 0.157 Uiso 0.50 1 d PR . . O101 O 0.3593(12) 0.0697(11) 0.2467(9) 0.073(3) Uiso 0.50 1 d PD . . N101 N 0.4462(14) -0.0473(13) 0.2389(10) 0.065(4) Uiso 0.50 1 d PD . . C101 C 0.440(2) 0.043(2) 0.2708(19) 0.112(8) Uiso 0.50 1 d PD . . H101 H 0.5131 0.1037 0.3253 0.134 Uiso 0.50 1 calc PR . . C102 C 0.338(2) -0.146(2) 0.1595(15) 0.106(8) Uiso 0.50 1 d PD . . H10D H 0.3568 -0.2091 0.1379 0.159 Uiso 0.50 1 calc PR . . H10E H 0.3216 -0.1176 0.1072 0.159 Uiso 0.50 1 calc PR . . H10F H 0.2612 -0.1792 0.1791 0.159 Uiso 0.50 1 calc PR . . C103 C 0.562(3) -0.040(3) 0.288(2) 0.132(10) Uiso 0.50 1 d P . . H10G H 0.5603 -0.1133 0.2553 0.198 Uiso 0.50 1 calc PR . . H10H H 0.5667 -0.0340 0.3539 0.198 Uiso 0.50 1 calc PR . . H10I H 0.6375 0.0310 0.2873 0.198 Uiso 0.50 1 calc 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 0.0292(4) 0.0384(5) 0.0274(4) 0.0128(4) 0.0143(3) 0.0174(4) Ni2 0.0301(4) 0.0388(5) 0.0262(4) 0.0151(4) 0.0140(3) 0.0174(4) S1 0.0320(8) 0.0363(9) 0.0300(8) 0.0135(7) 0.0136(7) 0.0171(7) S2 0.0301(8) 0.0404(9) 0.0283(8) 0.0158(7) 0.0132(6) 0.0195(7) N1 0.034(3) 0.043(3) 0.031(3) 0.015(2) 0.017(2) 0.019(3) N2 0.029(3) 0.045(3) 0.034(3) 0.016(3) 0.018(2) 0.021(3) N3 0.033(3) 0.040(3) 0.025(3) 0.016(2) 0.011(2) 0.020(3) N4 0.035(3) 0.040(3) 0.027(3) 0.015(2) 0.016(2) 0.017(2) C1 0.029(3) 0.032(3) 0.029(3) 0.008(3) 0.008(3) 0.012(3) C2 0.032(3) 0.038(4) 0.032(3) 0.010(3) 0.012(3) 0.018(3) C3 0.036(3) 0.048(4) 0.033(4) 0.011(3) 0.017(3) 0.023(3) C4 0.041(4) 0.046(4) 0.032(4) 0.011(3) 0.011(3) 0.024(3) C5 0.041(4) 0.038(4) 0.027(3) 0.010(3) 0.012(3) 0.018(3) C6 0.041(4) 0.036(4) 0.029(3) 0.012(3) 0.013(3) 0.018(3) C7 0.039(4) 0.040(4) 0.027(3) 0.014(3) 0.016(3) 0.019(3) C8 0.040(4) 0.052(4) 0.034(4) 0.013(3) 0.018(3) 0.023(3) C9 0.037(3) 0.046(4) 0.036(4) 0.010(3) 0.022(3) 0.019(3) C10 0.036(4) 0.051(4) 0.044(4) 0.014(3) 0.024(3) 0.019(3) C11 0.049(4) 0.075(5) 0.037(4) 0.020(4) 0.012(3) 0.042(4) C12 0.094(8) 0.178(13) 0.058(6) 0.005(7) -0.004(6) 0.104(9) C13 0.107(8) 0.291(19) 0.058(6) 0.068(9) 0.039(6) 0.157(12) C14 0.102(9) 0.151(12) 0.173(14) 0.117(12) 0.024(9) 0.073(9) C15 0.032(3) 0.037(4) 0.038(4) 0.017(3) 0.014(3) 0.015(3) C16 0.024(3) 0.041(4) 0.028(3) 0.014(3) 0.006(3) 0.014(3) C17 0.030(3) 0.042(4) 0.025(3) 0.013(3) 0.013(3) 0.018(3) C18 0.033(3) 0.048(4) 0.033(4) 0.020(3) 0.014(3) 0.017(3) C19 0.037(3) 0.039(4) 0.032(3) 0.012(3) 0.011(3) 0.020(3) C20 0.037(3) 0.054(4) 0.030(3) 0.021(3) 0.016(3) 0.029(3) C21 0.030(3) 0.043(4) 0.024(3) 0.017(3) 0.013(3) 0.019(3) C22 0.038(3) 0.045(4) 0.027(3) 0.018(3) 0.015(3) 0.025(3) C23 0.037(3) 0.051(4) 0.028(3) 0.021(3) 0.021(3) 0.022(3) C24 0.039(4) 0.055(4) 0.029(3) 0.020(3) 0.018(3) 0.023(3) C25 0.036(3) 0.056(4) 0.035(4) 0.023(3) 0.019(3) 0.017(3) C26 0.045(4) 0.040(4) 0.040(4) 0.016(3) 0.018(3) 0.019(3) C27 0.068(5) 0.057(5) 0.071(6) 0.035(4) 0.032(4) 0.038(4) C28 0.079(6) 0.044(4) 0.063(5) 0.018(4) 0.039(5) 0.029(4) C29 0.048(4) 0.035(4) 0.066(5) 0.008(4) 0.008(4) 0.013(4) C30 0.035(3) 0.042(4) 0.035(4) 0.014(3) 0.018(3) 0.019(3) Cl1 0.0702(13) 0.0590(12) 0.0408(11) 0.0242(10) 0.0280(10) 0.0167(11) O1A 0.084(4) 0.141(6) 0.062(4) 0.071(4) 0.043(4) 0.056(4) O1B 0.41(2) 0.174(10) 0.090(7) 0.054(7) 0.064(9) 0.224(13) O1C 0.072(5) 0.244(12) 0.054(5) 0.045(6) 0.030(4) -0.013(6) O1D 0.084(5) 0.061(4) 0.081(5) 0.021(4) 0.016(4) 0.021(4) Cl2 0.0686(13) 0.0786(15) 0.0706(14) 0.0339(12) 0.0333(11) 0.0523(12) O2A 0.083(6) 0.138(9) 0.236(14) 0.101(9) -0.009(7) 0.007(6) O2B 0.139(9) 0.175(11) 0.307(17) 0.186(12) 0.067(10) 0.065(8) O2C 0.198(9) 0.275(12) 0.059(5) 0.018(6) 0.021(5) 0.216(10) O2D 0.251(13) 0.239(13) 0.140(9) 0.046(9) 0.109(9) 0.197(12) _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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) -9.5021 (0.0109) x + 12.2923 (0.0074) y - 1.7967 (0.0208) z = 0.4556 (0.0056) * 0.0163 (0.0019) N1 * -0.0162 (0.0019) N2 * -0.0169 (0.0020) S1 * 0.0168 (0.0020) S2 -0.0044 (0.0023) Ni1 Rms deviation of fitted atoms = 0.0165 4.4473 (0.0155) x - 11.9542 (0.0079) y + 9.4095 (0.0154) z = 0.2633 (0.0051) * -0.0056 (0.0019) N3 * 0.0055 (0.0019) N4 * -0.0057 (0.0019) S1 * 0.0057 (0.0019) S2 0.0048 (0.0022) Ni2 Rms deviation of fitted atoms = 0.0056 -0.8823 (0.0331) x + 11.5466 (0.0180) y - 0.0821 (0.0411) z = 3.6150 (0.0179) * -0.0014 (0.0046) C1 * 0.0002 (0.0045) C2 * 0.0026 (0.0048) C3 * -0.0042 (0.0049) C4 * 0.0032 (0.0046) C5 * -0.0004 (0.0046) C6 Rms deviation of fitted atoms = 0.0025 9.0895 (0.0210) x - 6.7836 (0.0284) y + 7.9762 (0.0323) z = 1.6938 (0.0051) Angle to previous plane (with approximate esd) = 89.19 ( 0.21 ) * -0.0245 (0.0042) C16 * 0.0108 (0.0043) C17 * 0.0084 (0.0045) C18 * -0.0142 (0.0044) C19 * 0.0009 (0.0043) C20 * 0.0187 (0.0042) C21 Rms deviation of fitted atoms = 0.0149 ; 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 N1 1.917(5) . ? Ni1 N2 1.937(5) . ? Ni1 S2 2.1565(18) . ? Ni1 S1 2.1754(17) . ? Ni2 N3 1.908(5) . ? Ni2 N4 1.930(5) . ? Ni2 S2 2.1574(17) . ? Ni2 S1 2.1607(18) . ? S1 C1 1.774(6) . ? S2 C16 1.757(7) . ? N1 C7 1.286(8) . ? N1 C8 1.476(8) . ? N2 C15 1.256(8) . ? N2 C10 1.499(8) . ? N3 C22 1.280(8) . ? N3 C23 1.491(7) . ? N4 C30 1.270(8) . ? N4 C25 1.482(8) . ? C1 C2 1.390(8) . ? C1 C6 1.401(9) . ? C2 C3 1.404(9) . ? C2 C30 1.460(9) . ? C3 C4 1.401(9) . ? C3 H3A 0.9500 . ? C4 C5 1.388(9) . ? C4 C11 1.518(9) . ? C5 C6 1.395(9) . ? C5 H5A 0.9500 . ? C6 C7 1.462(9) . ? C7 H7A 0.9500 . ? C8 C9 1.521(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.492(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10J 0.9900 . ? C10 H10K 0.9900 . ? C11 C12 1.491(13) . ? C11 C13 1.506(11) . ? C11 C14 1.524(14) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.454(9) . ? C15 H15A 0.9500 . ? C16 C21 1.391(9) . ? C16 C17 1.417(8) . ? C17 C18 1.387(9) . ? C18 C19 1.417(9) . ? C18 H18A 0.9500 . ? C19 C20 1.383(9) . ? C19 C26 1.511(9) . ? C20 C21 1.388(9) . ? C20 H20A 0.9500 . ? C21 C22 1.471(8) . ? C22 H22A 0.9500 . ? C23 C24 1.513(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.493(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.515(10) . ? C26 C28 1.533(10) . ? C26 C29 1.561(10) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9500 . ? Cl1 O1C 1.383(6) . ? Cl1 O1A 1.392(5) . ? Cl1 O1D 1.397(5) . ? Cl1 O1B 1.405(7) . ? Cl2 O2C 1.370(5) . ? Cl2 O2B 1.387(7) . ? Cl2 O2D 1.389(7) . ? Cl2 O2A 1.413(6) . ? O100 C100 1.419(10) . ? O100 H100 0.8500 . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9799 . ? O101 C101 1.233(16) . ? N101 C101 1.233(16) . ? N101 C102 1.428(13) . ? N101 C103 1.43(3) . ? C101 H101 0.9500 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C103 H10G 0.9800 . ? C103 H10H 0.9800 . ? C103 H10I 0.9800 . ? 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 N1 Ni1 N2 96.5(2) . . ? N1 Ni1 S2 171.32(16) . . ? N2 Ni1 S2 92.09(16) . . ? N1 Ni1 S1 91.73(16) . . ? N2 Ni1 S1 171.73(17) . . ? S2 Ni1 S1 79.68(6) . . ? N3 Ni2 N4 95.9(2) . . ? N3 Ni2 S2 92.29(16) . . ? N4 Ni2 S2 171.76(16) . . ? N3 Ni2 S1 172.26(16) . . ? N4 Ni2 S1 91.78(16) . . ? S2 Ni2 S1 79.98(6) . . ? C1 S1 Ni2 102.6(2) . . ? C1 S1 Ni1 102.2(2) . . ? Ni2 S1 Ni1 93.74(7) . . ? C16 S2 Ni1 104.1(2) . . ? C16 S2 Ni2 103.4(2) . . ? Ni1 S2 Ni2 94.37(6) . . ? C7 N1 C8 115.7(5) . . ? C7 N1 Ni1 126.0(4) . . ? C8 N1 Ni1 118.4(4) . . ? C15 N2 C10 116.2(5) . . ? C15 N2 Ni1 126.9(4) . . ? C10 N2 Ni1 116.8(4) . . ? C22 N3 C23 114.9(5) . . ? C22 N3 Ni2 126.8(4) . . ? C23 N3 Ni2 118.3(4) . . ? C30 N4 C25 116.9(5) . . ? C30 N4 Ni2 125.6(4) . . ? C25 N4 Ni2 117.4(4) . . ? C2 C1 C6 119.9(6) . . ? C2 C1 S1 120.1(5) . . ? C6 C1 S1 119.7(5) . . ? C1 C2 C3 119.4(6) . . ? C1 C2 C30 124.1(6) . . ? C3 C2 C30 116.6(6) . . ? C4 C3 C2 122.1(6) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C5 C4 C3 116.8(6) . . ? C5 C4 C11 120.1(6) . . ? C3 C4 C11 123.1(6) . . ? C4 C5 C6 122.8(6) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C5 C6 C1 119.1(6) . . ? C5 C6 C7 116.7(6) . . ? C1 C6 C7 124.3(6) . . ? N1 C7 C6 126.4(6) . . ? N1 C7 H7A 116.8 . . ? C6 C7 H7A 116.8 . . ? N1 C8 C9 111.0(5) . . ? N1 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 113.8(6) . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 N2 112.2(5) . . ? C9 C10 H10J 109.2 . . ? N2 C10 H10J 109.2 . . ? C9 C10 H10K 109.2 . . ? N2 C10 H10K 109.2 . . ? H10J C10 H10K 107.9 . . ? C12 C11 C13 109.4(9) . . ? C12 C11 C4 108.7(7) . . ? C13 C11 C4 113.2(6) . . ? C12 C11 C14 106.1(10) . . ? C13 C11 C14 109.9(10) . . ? C4 C11 C14 109.3(7) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C17 127.4(6) . . ? N2 C15 H15A 116.3 . . ? C17 C15 H15A 116.3 . . ? C21 C16 C17 119.1(6) . . ? C21 C16 S2 121.0(5) . . ? C17 C16 S2 119.7(5) . . ? C18 C17 C16 118.9(6) . . ? C18 C17 C15 117.0(5) . . ? C16 C17 C15 124.1(6) . . ? C17 C18 C19 123.0(6) . . ? C17 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C20 C19 C18 115.5(6) . . ? C20 C19 C26 124.4(6) . . ? C18 C19 C26 120.1(6) . . ? C19 C20 C21 123.6(6) . . ? C19 C20 H20A 118.2 . . ? C21 C20 H20A 118.2 . . ? C20 C21 C16 119.7(5) . . ? C20 C21 C22 116.6(5) . . ? C16 C21 C22 123.6(6) . . ? N3 C22 C21 126.8(6) . . ? N3 C22 H22A 116.6 . . ? C21 C22 H22A 116.6 . . ? N3 C23 C24 111.9(5) . . ? N3 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? N3 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 114.0(6) . . ? C25 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? N4 C25 C24 112.0(5) . . ? N4 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? N4 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C19 C26 C27 109.5(6) . . ? C19 C26 C28 111.5(6) . . ? C27 C26 C28 110.3(6) . . ? C19 C26 C29 108.7(6) . . ? C27 C26 C29 108.8(6) . . ? C28 C26 C29 108.1(6) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C30 C2 127.3(6) . . ? N4 C30 H30A 116.3 . . ? C2 C30 H30A 116.3 . . ? O1C Cl1 O1A 110.4(4) . . ? O1C Cl1 O1D 110.7(4) . . ? O1A Cl1 O1D 111.5(4) . . ? O1C Cl1 O1B 109.9(6) . . ? O1A Cl1 O1B 109.5(5) . . ? O1D Cl1 O1B 104.7(6) . . ? O2C Cl2 O2B 113.2(6) . . ? O2C Cl2 O2D 108.4(5) . . ? O2B Cl2 O2D 109.6(8) . . ? O2C Cl2 O2A 109.1(5) . . ? O2B Cl2 O2A 107.0(6) . . ? O2D Cl2 O2A 109.5(6) . . ? C100 O100 H100 115.9 . . ? O100 C100 H10A 111.9 . . ? O100 C100 H10B 108.6 . . ? H10A C100 H10B 109.5 . . ? O100 C100 H10C 107.9 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C101 N101 C102 117(2) . . ? C101 N101 C103 115(2) . . ? C102 N101 C103 128(2) . . ? N101 C101 O101 133(2) . . ? N101 C101 H101 113.4 . . ? O101 C101 H101 113.4 . . ? N101 C102 H10D 109.5 . . ? N101 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? N101 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? N101 C103 H10G 109.5 . . ? N101 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? N101 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ni2 S1 C1 -50.5(3) . . . . ? S2 Ni2 S1 C1 129.4(2) . . . . ? N4 Ni2 S1 Ni1 -153.91(17) . . . . ? S2 Ni2 S1 Ni1 26.00(6) . . . . ? N1 Ni1 S1 C1 51.5(3) . . . . ? S2 Ni1 S1 C1 -129.8(2) . . . . ? N1 Ni1 S1 Ni2 155.20(17) . . . . ? S2 Ni1 S1 Ni2 -26.04(6) . . . . ? N2 Ni1 S2 C16 -48.1(3) . . . . ? S1 Ni1 S2 C16 131.2(2) . . . . ? N2 Ni1 S2 Ni2 -153.13(17) . . . . ? S1 Ni1 S2 Ni2 26.10(7) . . . . ? N3 Ni2 S2 C16 48.7(3) . . . . ? S1 Ni2 S2 C16 -131.9(2) . . . . ? N3 Ni2 S2 Ni1 154.33(16) . . . . ? S1 Ni2 S2 Ni1 -26.27(7) . . . . ? N2 Ni1 N1 C7 141.1(6) . . . . ? S1 Ni1 N1 C7 -38.3(6) . . . . ? N2 Ni1 N1 C8 -38.9(5) . . . . ? S1 Ni1 N1 C8 141.7(5) . . . . ? N1 Ni1 N2 C15 -146.9(6) . . . . ? S2 Ni1 N2 C15 34.3(6) . . . . ? N1 Ni1 N2 C10 37.5(5) . . . . ? S2 Ni1 N2 C10 -141.4(5) . . . . ? N4 Ni2 N3 C22 143.6(5) . . . . ? S2 Ni2 N3 C22 -36.4(5) . . . . ? N4 Ni2 N3 C23 -38.9(5) . . . . ? S2 Ni2 N3 C23 141.1(4) . . . . ? N3 Ni2 N4 C30 -142.2(6) . . . . ? S1 Ni2 N4 C30 38.4(6) . . . . ? N3 Ni2 N4 C25 39.7(5) . . . . ? S1 Ni2 N4 C25 -139.8(5) . . . . ? Ni2 S1 C1 C2 44.4(5) . . . . ? Ni1 S1 C1 C2 141.1(5) . . . . ? Ni2 S1 C1 C6 -141.6(5) . . . . ? Ni1 S1 C1 C6 -44.9(5) . . . . ? C6 C1 C2 C3 0.0(10) . . . . ? S1 C1 C2 C3 174.1(5) . . . . ? C6 C1 C2 C30 -179.8(6) . . . . ? S1 C1 C2 C30 -5.7(9) . . . . ? C1 C2 C3 C4 0.4(10) . . . . ? C30 C2 C3 C4 -179.8(6) . . . . ? C2 C3 C4 C5 -0.8(10) . . . . ? C2 C3 C4 C11 179.1(7) . . . . ? C3 C4 C5 C6 0.8(10) . . . . ? C11 C4 C5 C6 -179.0(7) . . . . ? C4 C5 C6 C1 -0.5(10) . . . . ? C4 C5 C6 C7 -179.7(6) . . . . ? C2 C1 C6 C5 0.0(10) . . . . ? S1 C1 C6 C5 -174.0(5) . . . . ? C2 C1 C6 C7 179.2(6) . . . . ? S1 C1 C6 C7 5.1(9) . . . . ? C8 N1 C7 C6 -179.1(6) . . . . ? Ni1 N1 C7 C6 0.9(10) . . . . ? C5 C6 C7 N1 -155.3(7) . . . . ? C1 C6 C7 N1 25.5(11) . . . . ? C7 N1 C8 C9 -124.4(6) . . . . ? Ni1 N1 C8 C9 55.6(7) . . . . ? N1 C8 C9 C10 -68.0(8) . . . . ? C8 C9 C10 N2 68.1(8) . . . . ? C15 N2 C10 C9 129.1(6) . . . . ? Ni1 N2 C10 C9 -54.7(7) . . . . ? C5 C4 C11 C12 -58.0(10) . . . . ? C3 C4 C11 C12 122.1(9) . . . . ? C5 C4 C11 C13 -179.8(9) . . . . ? C3 C4 C11 C13 0.3(12) . . . . ? C5 C4 C11 C14 57.4(11) . . . . ? C3 C4 C11 C14 -122.5(10) . . . . ? C10 N2 C15 C17 176.5(6) . . . . ? Ni1 N2 C15 C17 0.8(10) . . . . ? Ni1 S2 C16 C21 -141.5(5) . . . . ? Ni2 S2 C16 C21 -43.4(5) . . . . ? Ni1 S2 C16 C17 43.6(5) . . . . ? Ni2 S2 C16 C17 141.8(4) . . . . ? C21 C16 C17 C18 -3.7(9) . . . . ? S2 C16 C17 C18 171.2(5) . . . . ? C21 C16 C17 C15 178.3(6) . . . . ? S2 C16 C17 C15 -6.7(9) . . . . ? N2 C15 C17 C18 158.7(6) . . . . ? N2 C15 C17 C16 -23.4(11) . . . . ? C16 C17 C18 C19 0.7(9) . . . . ? C15 C17 C18 C19 178.7(6) . . . . ? C17 C18 C19 C20 1.6(9) . . . . ? C17 C18 C19 C26 -178.8(6) . . . . ? C18 C19 C20 C21 -0.8(9) . . . . ? C26 C19 C20 C21 179.6(6) . . . . ? C19 C20 C21 C16 -2.2(9) . . . . ? C19 C20 C21 C22 -179.2(6) . . . . ? C17 C16 C21 C20 4.5(9) . . . . ? S2 C16 C21 C20 -170.4(5) . . . . ? C17 C16 C21 C22 -178.8(5) . . . . ? S2 C16 C21 C22 6.3(8) . . . . ? C23 N3 C22 C21 -175.8(6) . . . . ? Ni2 N3 C22 C21 1.7(9) . . . . ? C20 C21 C22 N3 -160.7(6) . . . . ? C16 C21 C22 N3 22.4(10) . . . . ? C22 N3 C23 C24 -127.9(6) . . . . ? Ni2 N3 C23 C24 54.3(7) . . . . ? N3 C23 C24 C25 -65.7(8) . . . . ? C30 N4 C25 C24 125.3(6) . . . . ? Ni2 N4 C25 C24 -56.4(7) . . . . ? C23 C24 C25 N4 67.1(8) . . . . ? C20 C19 C26 C27 122.0(7) . . . . ? C18 C19 C26 C27 -57.5(8) . . . . ? C20 C19 C26 C28 -0.3(10) . . . . ? C18 C19 C26 C28 -179.8(6) . . . . ? C20 C19 C26 C29 -119.3(7) . . . . ? C18 C19 C26 C29 61.2(8) . . . . ? C25 N4 C30 C2 175.9(6) . . . . ? Ni2 N4 C30 C2 -2.3(10) . . . . ? C1 C2 C30 N4 -23.6(11) . . . . ? C3 C2 C30 N4 156.6(7) . . . . ? C102 N101 C101 O101 -3(4) . . . . ? C103 N101 C101 O101 178(3) . . . . ? #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 282073' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H32 N2 O2 Pd S2' _chemical_formula_sum 'C27 H32 N2 O2 Pd S2' _chemical_formula_weight 587.07 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 36.323(4) _cell_length_b 8.3434(12) _cell_length_c 8.5289(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.795(3) _cell_angle_gamma 90.00 _cell_volume 2539.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 364 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 20.12 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.513 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.515872 ; _exptl_special_details ; Tiny crystal - relatively weak diffraction (ca. 50% observed to 0.84 \%A resolution). C atoms refined isotropically. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 4803 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.1684 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.928 _reflns_number_total 2083 _reflns_number_gt 1093 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-8 (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2083 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1563 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2005 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.089 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.167 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.27163(13) 0.7500 0.0267(5) Uani 1 2 d S . . S1 S 0.45746(8) 0.0723(3) 0.7026(4) 0.0377(9) Uani 1 1 d . . . O1 O 0.3862(2) -0.2560(8) 0.4148(11) 0.054(2) Uani 1 1 d . . . N1 N 0.4590(2) 0.4432(9) 0.7155(10) 0.018(2) Uani 1 1 d . . . C1 C 0.4187(3) 0.1380(13) 0.5687(14) 0.033(3) Uiso 1 1 d . . . C2 C 0.3961(3) 0.0251(12) 0.4721(13) 0.031(3) Uiso 1 1 d . . . C3 C 0.3621(3) 0.0675(11) 0.3708(13) 0.028(3) Uiso 1 1 d . . . H3A H 0.3473 -0.0132 0.3107 0.034 Uiso 1 1 calc R . . C4 C 0.3502(3) 0.2258(12) 0.3584(13) 0.032(3) Uiso 1 1 d . . . C5 C 0.3716(3) 0.3396(13) 0.4466(14) 0.034(3) Uiso 1 1 d . . . H5A H 0.3636 0.4481 0.4402 0.041 Uiso 1 1 calc R . . C6 C 0.4060(3) 0.2971(12) 0.5483(13) 0.027(2) Uiso 1 1 d . . . C7 C 0.4243(3) 0.4301(11) 0.6425(12) 0.023(2) Uiso 1 1 d . . . H7A H 0.4087 0.5198 0.6521 0.028 Uiso 1 1 calc R . . C8 C 0.4692(3) 0.5925(12) 0.8036(14) 0.033(3) Uiso 1 1 d . . . H8A H 0.4772 0.5665 0.9182 0.039 Uiso 1 1 calc R . . H8B H 0.4466 0.6611 0.7928 0.039 Uiso 1 1 calc R . . C9 C 0.5000 0.6869(18) 0.7500 0.039(4) Uiso 1 2 d S . . H9A H 0.5113 0.7552 0.8363 0.047 Uiso 1 1 d R . . C10 C 0.4066(3) -0.1482(13) 0.4707(14) 0.038(3) Uiso 1 1 d . . . H10A H 0.4316 -0.1757 0.5181 0.046 Uiso 1 1 calc R . . C11 C 0.3121(3) 0.2650(12) 0.2533(13) 0.032(3) Uiso 1 1 d . . . C12 C 0.2818(4) 0.2267(17) 0.3419(19) 0.071(4) Uiso 1 1 d . . . H12A H 0.2870 0.2789 0.4466 0.107 Uiso 1 1 calc R . . H12B H 0.2805 0.1104 0.3560 0.107 Uiso 1 1 calc R . . H12C H 0.2578 0.2655 0.2815 0.107 Uiso 1 1 calc R . . C13 C 0.3064(4) 0.188(2) 0.090(2) 0.086(5) Uiso 1 1 d . . . H13A H 0.2816 0.2171 0.0292 0.130 Uiso 1 1 calc R . . H13B H 0.3081 0.0712 0.1011 0.130 Uiso 1 1 calc R . . H13C H 0.3257 0.2258 0.0323 0.130 Uiso 1 1 calc R . . C14 C 0.3094(4) 0.4439(16) 0.222(2) 0.078(5) Uiso 1 1 d . . . H14A H 0.3129 0.5015 0.3240 0.117 Uiso 1 1 calc R . . H14B H 0.2846 0.4694 0.1593 0.117 Uiso 1 1 calc R . . H14C H 0.3288 0.4766 0.1628 0.117 Uiso 1 1 calc R . . 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 Pd1 0.0149(6) 0.0265(7) 0.0359(9) 0.000 -0.0024(6) 0.000 S1 0.030(2) 0.0228(16) 0.055(3) 0.0039(13) -0.0052(18) -0.0027(11) O1 0.056(5) 0.022(4) 0.079(7) -0.003(4) 0.000(5) -0.014(4) N1 0.009(5) 0.028(5) 0.017(5) -0.002(4) 0.001(4) 0.000(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 Pd1 N1 2.046(7) . ? Pd1 N1 2.046(7) 6_657 ? Pd1 S1 2.255(3) . ? Pd1 S1 2.255(3) 6_657 ? S1 C1 1.727(11) . ? O1 C10 1.205(12) . ? N1 C7 1.304(12) . ? N1 C8 1.466(12) . ? C1 C6 1.406(14) . ? C1 C2 1.409(15) . ? C2 C3 1.414(15) . ? C2 C10 1.496(15) . ? C3 C4 1.388(13) . ? C3 H3A 0.9500 . ? C4 C5 1.362(14) . ? C4 C11 1.534(15) . ? C5 C6 1.426(14) . ? C5 H5A 0.9500 . ? C6 C7 1.455(13) . ? C7 H7A 0.9500 . ? C8 C9 1.507(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C8 1.507(12) 6_657 ? C9 H9A 0.9600 . ? C10 H10A 0.9500 . ? C11 C12 1.483(16) . ? C11 C14 1.516(15) . ? C11 C13 1.516(18) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 N1 Pd1 N1 91.2(4) . 6_657 ? N1 Pd1 S1 92.0(2) . . ? N1 Pd1 S1 175.9(2) 6_657 . ? N1 Pd1 S1 175.9(2) . 6_657 ? N1 Pd1 S1 92.0(2) 6_657 6_657 ? S1 Pd1 S1 84.92(15) . 6_657 ? C1 S1 Pd1 109.3(4) . . ? C7 N1 C8 116.4(8) . . ? C7 N1 Pd1 128.6(6) . . ? C8 N1 Pd1 114.4(6) . . ? C6 C1 C2 114.6(10) . . ? C6 C1 S1 126.1(9) . . ? C2 C1 S1 119.2(8) . . ? C1 C2 C3 122.5(10) . . ? C1 C2 C10 122.0(10) . . ? C3 C2 C10 115.5(9) . . ? C4 C3 C2 120.6(10) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 118.9(10) . . ? C5 C4 C11 122.2(9) . . ? C3 C4 C11 118.8(10) . . ? C4 C5 C6 120.6(10) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 122.7(10) . . ? C1 C6 C7 123.2(10) . . ? C5 C6 C7 113.8(9) . . ? N1 C7 C6 128.9(9) . . ? N1 C7 H7A 115.6 . . ? C6 C7 H7A 115.6 . . ? N1 C8 C9 114.8(9) . . ? N1 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N1 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.5 . . ? C8 C9 C8 116.9(12) . 6_657 ? C8 C9 H9A 108.3 . . ? C8 C9 H9A 107.9 6_657 . ? O1 C10 C2 125.9(11) . . ? O1 C10 H10A 117.0 . . ? C2 C10 H10A 117.0 . . ? C12 C11 C14 105.7(10) . . ? C12 C11 C13 113.0(11) . . ? C14 C11 C13 105.2(11) . . ? C12 C11 C4 109.3(10) . . ? C14 C11 C4 109.6(10) . . ? C13 C11 C4 113.7(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 S1 C1 31.0(5) . . . . ? S1 Pd1 S1 C1 -151.7(5) 6_657 . . . ? N1 Pd1 N1 C7 158.5(10) 6_657 . . . ? S1 Pd1 N1 C7 -19.0(8) . . . . ? N1 Pd1 N1 C8 -30.5(5) 6_657 . . . ? S1 Pd1 N1 C8 152.0(6) . . . . ? Pd1 S1 C1 C6 -28.4(11) . . . . ? Pd1 S1 C1 C2 154.1(8) . . . . ? C6 C1 C2 C3 -4.0(16) . . . . ? S1 C1 C2 C3 173.8(8) . . . . ? C6 C1 C2 C10 176.3(10) . . . . ? S1 C1 C2 C10 -5.9(15) . . . . ? C1 C2 C3 C4 2.3(17) . . . . ? C10 C2 C3 C4 -177.9(9) . . . . ? C2 C3 C4 C5 -0.6(16) . . . . ? C2 C3 C4 C11 -177.1(9) . . . . ? C3 C4 C5 C6 0.8(16) . . . . ? C11 C4 C5 C6 177.2(9) . . . . ? C2 C1 C6 C5 4.2(16) . . . . ? S1 C1 C6 C5 -173.4(8) . . . . ? C2 C1 C6 C7 176.7(10) . . . . ? S1 C1 C6 C7 -0.9(16) . . . . ? C4 C5 C6 C1 -2.8(16) . . . . ? C4 C5 C6 C7 -176.0(10) . . . . ? C8 N1 C7 C6 -179.3(10) . . . . ? Pd1 N1 C7 C6 -8.4(16) . . . . ? C1 C6 C7 N1 25.1(17) . . . . ? C5 C6 C7 N1 -161.8(10) . . . . ? C7 N1 C8 C9 -121.0(9) . . . . ? Pd1 N1 C8 C9 66.8(10) . . . . ? N1 C8 C9 C8 -35.4(6) . . . 6_657 ? C1 C2 C10 O1 166.1(12) . . . . ? C3 C2 C10 O1 -13.7(17) . . . . ? C5 C4 C11 C12 -96.9(12) . . . . ? C3 C4 C11 C12 79.4(12) . . . . ? C5 C4 C11 C14 18.5(15) . . . . ? C3 C4 C11 C14 -165.2(11) . . . . ? C5 C4 C11 C13 135.9(12) . . . . ? C3 C4 C11 C13 -47.8(14) . . . . ? #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 282074' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 N8 S4 Pd2, 3(C3 H7 NO)' _chemical_formula_sum 'C69 H97 N11 O3 Pd2 S4' _chemical_formula_weight 1469.62 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.286(7) _cell_length_b 10.232(2) _cell_length_c 20.489(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.30(3) _cell_angle_gamma 90.00 _cell_volume 7168(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7614 _exptl_absorpt_correction_T_max 0.9867 _exptl_absorpt_process_details 'SADABS v.2.03' _exptl_special_details ; Severe absorption problems - crystal was clearly far too large. The .raw output files are no longer available (deleted!), so no prospect for further "empirical" absorption correction. Despite several attempts, we have been unable to prepare more crystals of this compound, so these data are the best that exist. The data prove the connectivity, but do not permit anisotropic refinement. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method 'Thin slice \w scans' _diffrn_standards_number 0 _diffrn_reflns_number 35855 _diffrn_reflns_av_R_equivalents 0.2114 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 6324 _reflns_number_gt 3703 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v.5.0 (Bruker AXS, 1997)' _computing_cell_refinement 'SAINT v.5.0 (Bruker AXS, 1997)' _computing_data_reduction 'SAINT v.5.0 (Bruker AXS, 1997)' _computing_structure_solution 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_structure_refinement 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6324 _refine_ls_number_parameters 189 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.2704 _refine_ls_R_factor_gt 0.2157 _refine_ls_wR_factor_ref 0.4756 _refine_ls_wR_factor_gt 0.4593 _refine_ls_goodness_of_fit_ref 2.516 _refine_ls_restrained_S_all 2.514 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 10.137 _refine_diff_density_min -14.035 _refine_diff_density_rms 0.525 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.08019(4) 0.34482(14) 0.49534(9) 0.0211(5) Uiso 1 1 d . . . S1 S 0.10128(15) 0.2213(5) 0.4141(3) 0.0273(13) Uiso 1 1 d . . . S2 S 0.01990(14) 0.2638(5) 0.4645(3) 0.0255(13) Uiso 1 1 d . . . N1 N 0.1366(5) 0.4003(16) 0.5284(10) 0.027(4) Uiso 1 1 d . . . N2 N 0.0582(4) 0.4652(15) 0.5624(9) 0.021(4) Uiso 1 1 d . . . N3 N -0.0812(4) 0.0424(14) 0.4633(9) 0.015(3) Uiso 1 1 d . . . N4 N -0.1347(4) 0.1592(16) 0.2783(10) 0.026(4) Uiso 1 1 d . . . C1 C 0.1437(5) 0.2915(18) 0.3870(11) 0.021(4) Uiso 1 1 d . . . C2 C 0.1534(6) 0.2697(19) 0.3220(12) 0.024(5) Uiso 1 1 d . . . C3 C 0.1884(6) 0.3165(19) 0.3014(13) 0.028(5) Uiso 1 1 d . . . H3A H 0.1939 0.2997 0.2574 0.034 Uiso 1 1 calc R . . C4 C 0.2155(6) 0.385(2) 0.3399(13) 0.029(5) Uiso 1 1 d . . . C5 C 0.2554(7) 0.427(2) 0.3174(15) 0.042(6) Uiso 1 1 d . . . C51 C 0.2509(11) 0.443(4) 0.241(2) 0.109(14) Uiso 1 1 d . . . H51A H 0.2321 0.5126 0.2288 0.163 Uiso 1 1 calc R . . H51B H 0.2414 0.3605 0.2207 0.163 Uiso 1 1 calc R . . H51C H 0.2763 0.4648 0.2246 0.163 Uiso 1 1 calc R . . C52 C 0.2846(10) 0.319(3) 0.338(2) 0.089(11) Uiso 1 1 d . . . H52A H 0.2865 0.3092 0.3853 0.134 Uiso 1 1 calc R . . H52B H 0.3104 0.3415 0.3231 0.134 Uiso 1 1 calc R . . H52C H 0.2758 0.2362 0.3172 0.134 Uiso 1 1 calc R . . C53 C 0.2684(6) 0.554(2) 0.3476(14) 0.038(6) Uiso 1 1 d . . . H53A H 0.2711 0.5449 0.3954 0.057 Uiso 1 1 calc R . . H53B H 0.2490 0.6219 0.3355 0.057 Uiso 1 1 calc R . . H53C H 0.2936 0.5791 0.3319 0.057 Uiso 1 1 calc R . . C6 C 0.2059(5) 0.4081(19) 0.4047(12) 0.023(5) Uiso 1 1 d . . . H6A H 0.2236 0.4569 0.4330 0.028 Uiso 1 1 calc R . . C7 C 0.1714(5) 0.3621(18) 0.4287(12) 0.024(5) Uiso 1 1 d . . . C8 C 0.1661(6) 0.3980(19) 0.4962(12) 0.024(5) Uiso 1 1 d . . . H8A H 0.1895 0.4245 0.5203 0.029 Uiso 1 1 calc R . . C9 C 0.1408(6) 0.4260(19) 0.5985(12) 0.025(5) Uiso 1 1 d . . . H9A H 0.1690 0.4309 0.6129 0.030 Uiso 1 1 calc R . . H9B H 0.1294 0.3523 0.6220 0.030 Uiso 1 1 calc R . . C10 C 0.1209(6) 0.553(2) 0.6170(14) 0.036(6) Uiso 1 1 d . . . H10A H 0.1140 0.5473 0.6630 0.044 Uiso 1 1 calc R . . H10B H 0.1395 0.6266 0.6141 0.044 Uiso 1 1 calc R . . C11 C 0.0839(6) 0.5829(19) 0.5732(12) 0.026(5) Uiso 1 1 d . . . H11A H 0.0690 0.6531 0.5934 0.032 Uiso 1 1 calc R . . H11B H 0.0915 0.6152 0.5303 0.032 Uiso 1 1 calc R . . C12 C 0.0268(5) 0.4552(19) 0.5910(12) 0.026(5) Uiso 1 1 d . . . H12A H 0.0223 0.5243 0.6205 0.031 Uiso 1 1 calc R . . C13 C -0.0033(5) 0.3565(18) 0.5864(11) 0.020(4) Uiso 1 1 d . . . C14 C -0.0292(5) 0.3558(18) 0.6337(11) 0.021(4) Uiso 1 1 d . . . H14A H -0.0254 0.4176 0.6682 0.025 Uiso 1 1 calc R . . C15 C -0.0602(5) 0.2717(18) 0.6348(11) 0.020(4) Uiso 1 1 d . . . C16 C -0.0899(6) 0.2818(19) 0.6873(12) 0.027(5) Uiso 1 1 d . . . C161 C -0.1193(6) 0.172(2) 0.6836(13) 0.034(5) Uiso 1 1 d . . . H16A H -0.1339 0.1720 0.6406 0.051 Uiso 1 1 calc R . . H16B H -0.1376 0.1831 0.7178 0.051 Uiso 1 1 calc R . . H16C H -0.1056 0.0879 0.6901 0.051 Uiso 1 1 calc R . . C162 C -0.1109(8) 0.413(3) 0.6800(17) 0.059(8) Uiso 1 1 d . . . H16D H -0.1254 0.4173 0.6370 0.089 Uiso 1 1 calc R . . H16E H -0.0916 0.4837 0.6840 0.089 Uiso 1 1 calc R . . H16F H -0.1292 0.4216 0.7143 0.089 Uiso 1 1 calc R . . C163 C -0.0669(7) 0.277(2) 0.7567(14) 0.042(6) Uiso 1 1 d . . . H16G H -0.0476 0.3483 0.7602 0.062 Uiso 1 1 calc R . . H16H H -0.0534 0.1932 0.7623 0.062 Uiso 1 1 calc R . . H16I H -0.0852 0.2875 0.7907 0.062 Uiso 1 1 calc R . . C17 C -0.0645(5) 0.1770(18) 0.5847(11) 0.022(5) Uiso 1 1 d . . . H17A H -0.0846 0.1133 0.5851 0.027 Uiso 1 1 calc R . . C18 C -0.0388(5) 0.1773(16) 0.5344(11) 0.016(4) Uiso 1 1 d . . . C19 C -0.0075(5) 0.2660(17) 0.5327(11) 0.018(4) Uiso 1 1 d . . . C20 C -0.0463(5) 0.0823(18) 0.4806(11) 0.022(5) Uiso 1 1 d . . . H20A H -0.0250 0.0500 0.4583 0.027 Uiso 1 1 calc R . . C21 C -0.0848(5) -0.0543(18) 0.4122(11) 0.021(4) Uiso 1 1 d . . . H21A H -0.0925 -0.1390 0.4306 0.025 Uiso 1 1 calc R . . H21B H -0.0592 -0.0662 0.3935 0.025 Uiso 1 1 calc R . . C22 C -0.1157(6) -0.012(2) 0.3577(12) 0.029(5) Uiso 1 1 d . . . H22A H -0.1195 -0.0827 0.3250 0.035 Uiso 1 1 calc R . . H22B H -0.1410 0.0032 0.3769 0.035 Uiso 1 1 calc R . . C23 C -0.1038(5) 0.1107(18) 0.3241(12) 0.023(5) Uiso 1 1 d . . . H23A H -0.0970 0.1787 0.3574 0.027 Uiso 1 1 calc R . . H23B H -0.0803 0.0928 0.3005 0.027 Uiso 1 1 calc R . . C24 C -0.1250(6) 0.2061(19) 0.2239(12) 0.027(5) Uiso 1 1 d . . . H24A H -0.0986 0.1993 0.2133 0.032 Uiso 1 1 calc R . . O1 O 0.1804(6) 0.681(2) 0.5120(13) 0.081(7) Uiso 1 1 d D . . N5 N 0.1920(6) 0.8794(18) 0.4672(12) 0.047(6) Uiso 1 1 d D . . C31 C 0.1717(7) 0.795(2) 0.5027(14) 0.049(7) Uiso 1 1 d D . . H31 H 0.1491 0.8265 0.5215 0.059 Uiso 1 1 calc R . . C32 C 0.1797(8) 1.007(3) 0.4614(18) 0.069(9) Uiso 1 1 d D . . H32A H 0.1973 1.0555 0.4346 0.103 Uiso 1 1 calc R . . H32B H 0.1801 1.0467 0.5050 0.103 Uiso 1 1 calc R . . H32C H 0.1531 1.0096 0.4406 0.103 Uiso 1 1 calc R . . C33 C 0.2230(10) 0.838(3) 0.432(2) 0.094(12) Uiso 1 1 d D . . H33A H 0.2340 0.9130 0.4101 0.141 Uiso 1 1 calc R . . H33B H 0.2136 0.7734 0.3992 0.141 Uiso 1 1 calc R . . H33C H 0.2433 0.7983 0.4620 0.141 Uiso 1 1 calc R . . O2 O 0.0077(9) 0.387(2) 0.247(2) 0.033(8) Uiso 0.50 1 d PD A -1 N6 N -0.0062(12) 0.170(2) 0.2394(17) 0.028(9) Uiso 0.50 1 d PD A -1 C34 C -0.0106(11) 0.297(3) 0.2215(18) 0.031(11) Uiso 0.50 1 d PD A -1 H34 H -0.0293 0.3170 0.1864 0.038 Uiso 0.50 1 calc PR A -1 C35 C 0.0111(16) 0.140(4) 0.300(2) 0.051(14) Uiso 0.50 1 d PD A -1 H35A H 0.0124 0.0451 0.3054 0.077 Uiso 0.50 1 calc PR A -1 H35B H -0.0044 0.1776 0.3339 0.077 Uiso 0.50 1 calc PR A -1 H35C H 0.0376 0.1767 0.3045 0.077 Uiso 0.50 1 calc PR A -1 C36 C -0.0168(13) 0.068(3) 0.196(2) 0.037(12) Uiso 0.50 1 d PD A -1 H36A H -0.0112 -0.0157 0.2176 0.055 Uiso 0.50 1 calc PR A -1 H36B H -0.0019 0.0755 0.1572 0.055 Uiso 0.50 1 calc PR A -1 H36C H -0.0449 0.0743 0.1829 0.055 Uiso 0.50 1 calc PR A -1 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 1.8563(0.1473) x - 7.7435(0.0275) y + 13.2260(0.0635) z = 4.0410(0.0372) * -0.0109 (0.0056) Pd1 * -0.0899 (0.0063) S1 * 0.0964 (0.0066) S2 * 0.1010 (0.0069) N1 * -0.0966 (0.0070) N2 Rms deviation of fitted atoms = 0.0861 1.8563(0.1473) x + 7.7435(0.0275) y + 13.2260(0.0635) z = 2.5719(0.0126) Angle to previous plane (with approximate esd) = 81.64 ( 0.24 ) * 0.0109 (0.0056) Pd1_$1 * 0.0899 (0.0063) S1_$1 * -0.0964 (0.0067) S2_$1 * -0.1010 (0.0069) N1_$1 * 0.0966 (0.0070) N2_$1 Rms deviation of fitted atoms = 0.0861 ; 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 Pd1 N2 2.033(17) . ? Pd1 N1 2.078(16) . ? Pd1 S1 2.252(6) . ? Pd1 S2 2.273(5) . ? S1 C1 1.75(2) . ? S2 C19 1.74(2) . ? N1 C8 1.25(3) . ? N1 C9 1.46(3) . ? N2 C12 1.27(2) . ? N2 C11 1.50(2) . ? N3 C20 1.29(2) . ? N3 C21 1.44(3) . ? N4 C24 1.28(3) . ? N4 C23 1.45(3) . ? C1 C2 1.41(3) . ? C1 C7 1.43(3) . ? C2 C3 1.39(3) . ? C2 C24 1.46(3) 2 ? C3 C4 1.37(3) . ? C3 H3A 0.9500 . ? C4 C6 1.41(3) . ? C4 C5 1.54(3) . ? C5 C53 1.49(3) . ? C5 C52 1.53(4) . ? C5 C51 1.58(5) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C6 C7 1.40(3) . ? C6 H6A 0.9500 . ? C7 C8 1.46(3) . ? C8 H8A 0.9500 . ? C9 C10 1.53(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.53(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.44(3) . ? C12 H12A 0.9500 . ? C13 C14 1.36(3) . ? C13 C19 1.44(3) . ? C14 C15 1.37(3) . ? C14 H14A 0.9500 . ? C15 C17 1.41(3) . ? C15 C16 1.54(3) . ? C16 C161 1.51(3) . ? C16 C162 1.52(3) . ? C16 C163 1.57(3) . ? C161 H16A 0.9800 . ? C161 H16B 0.9800 . ? C161 H16C 0.9800 . ? C162 H16D 0.9800 . ? C162 H16E 0.9800 . ? C162 H16F 0.9800 . ? C163 H16G 0.9800 . ? C163 H16H 0.9800 . ? C163 H16I 0.9800 . ? C17 C18 1.41(3) . ? C17 H17A 0.9500 . ? C18 C19 1.41(2) . ? C18 C20 1.48(3) . ? C20 H20A 0.9500 . ? C21 C22 1.54(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.50(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C2 1.46(3) 2 ? C24 H24A 0.9500 . ? O1 C31 1.21(2) . ? N5 C31 1.36(3) . ? N5 C32 1.37(3) . ? N5 C33 1.40(3) . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O2 C34 1.22(2) . ? N6 C34 1.36(3) . ? N6 C35 1.37(3) . ? N6 C36 1.40(3) . ? C34 H34 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 N2 Pd1 N1 89.9(7) . . ? N2 Pd1 S1 174.9(5) . . ? N1 Pd1 S1 93.0(5) . . ? N2 Pd1 S2 91.9(4) . . ? N1 Pd1 S2 174.0(5) . . ? S1 Pd1 S2 85.7(2) . . ? C1 S1 Pd1 108.9(7) . . ? C19 S2 Pd1 107.8(7) . . ? C8 N1 C9 119.9(18) . . ? C8 N1 Pd1 126.4(17) . . ? C9 N1 Pd1 113.1(13) . . ? C12 N2 C11 120.5(18) . . ? C12 N2 Pd1 129.4(14) . . ? C11 N2 Pd1 110.0(12) . . ? C20 N3 C21 116.5(16) . . ? C24 N4 C23 117.9(17) . . ? C2 C1 C7 116.9(18) . . ? C2 C1 S1 119.5(15) . . ? C7 C1 S1 123.4(18) . . ? C3 C2 C1 120(2) . . ? C3 C2 C24 121(2) . 2 ? C1 C2 C24 119.2(18) . 2 ? C4 C3 C2 125(2) . . ? C4 C3 H3A 117.7 . . ? C2 C3 H3A 117.7 . . ? C3 C4 C6 116(2) . . ? C3 C4 C5 123(2) . . ? C6 C4 C5 121(2) . . ? C53 C5 C52 110(2) . . ? C53 C5 C4 111(2) . . ? C52 C5 C4 107(2) . . ? C53 C5 C51 109(2) . . ? C52 C5 C51 111(3) . . ? C4 C5 C51 108(2) . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C52 H52A 109.5 . . ? C5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C5 C53 H53A 109.5 . . ? C5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C7 C6 C4 123(2) . . ? C7 C6 H6A 118.7 . . ? C4 C6 H6A 118.7 . . ? C6 C7 C1 120(2) . . ? C6 C7 C8 114.8(18) . . ? C1 C7 C8 124.9(18) . . ? N1 C8 C7 132(2) . . ? N1 C8 H8A 114.0 . . ? C7 C8 H8A 114.0 . . ? N1 C9 C10 112.5(18) . . ? N1 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 112.9(19) . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N2 C11 C10 112.3(16) . . ? N2 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? N2 C12 C13 131(2) . . ? N2 C12 H12A 114.6 . . ? C13 C12 H12A 114.6 . . ? C14 C13 C19 120.5(17) . . ? C14 C13 C12 117.2(19) . . ? C19 C13 C12 122.2(19) . . ? C13 C14 C15 124(2) . . ? C13 C14 H14A 117.8 . . ? C15 C14 H14A 117.8 . . ? C14 C15 C17 117.2(19) . . ? C14 C15 C16 121.7(18) . . ? C17 C15 C16 121.2(17) . . ? C161 C16 C162 110.1(18) . . ? C161 C16 C15 112.9(18) . . ? C162 C16 C15 109(2) . . ? C161 C16 C163 108.1(19) . . ? C162 C16 C163 108(2) . . ? C15 C16 C163 108.4(17) . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C16 C162 H16D 109.5 . . ? C16 C162 H16E 109.5 . . ? H16D C162 H16E 109.5 . . ? C16 C162 H16F 109.5 . . ? H16D C162 H16F 109.5 . . ? H16E C162 H16F 109.5 . . ? C16 C163 H16G 109.5 . . ? C16 C163 H16H 109.5 . . ? H16G C163 H16H 109.5 . . ? C16 C163 H16I 109.5 . . ? H16G C163 H16I 109.5 . . ? H16H C163 H16I 109.5 . . ? C18 C17 C15 119.8(17) . . ? C18 C17 H17A 120.1 . . ? C15 C17 H17A 120.1 . . ? C17 C18 C19 122.6(18) . . ? C17 C18 C20 117.5(16) . . ? C19 C18 C20 119.8(18) . . ? C18 C19 C13 115.5(18) . . ? C18 C19 S2 117.9(16) . . ? C13 C19 S2 126.4(14) . . ? N3 C20 C18 121.4(18) . . ? N3 C20 H20A 119.3 . . ? C18 C20 H20A 119.3 . . ? N3 C21 C22 110.4(15) . . ? N3 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? N3 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C21 111.9(16) . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? N4 C23 C22 112.0(16) . . ? N4 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? N4 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N4 C24 C2 121.8(19) . 2 ? N4 C24 H24A 119.1 . . ? C2 C24 H24A 119.1 2 . ? C31 N5 C32 119.2(19) . . ? C31 N5 C33 121.6(19) . . ? C32 N5 C33 119(2) . . ? O1 C31 N5 125(2) . . ? O1 C31 H31 117.7 . . ? N5 C31 H31 117.7 . . ? N5 C32 H32A 109.5 . . ? N5 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N5 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 H33A 109.5 . . ? N5 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N5 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34 N6 C35 119(2) . . ? C34 N6 C36 122(2) . . ? C35 N6 C36 119(3) . . ? O2 C34 N6 125(2) . . ? O2 C34 H34 117.7 . . ? N6 C34 H34 117.7 . . ? N6 C35 H35A 109.5 . . ? N6 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N6 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N6 C36 H36A 109.5 . . ? N6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 S1 C1 -32.1(9) . . . . ? S2 Pd1 S1 C1 153.8(8) . . . . ? N2 Pd1 S2 C19 -31.6(8) . . . . ? S1 Pd1 S2 C19 153.0(7) . . . . ? N2 Pd1 N1 C8 -154.6(18) . . . . ? S1 Pd1 N1 C8 21.1(17) . . . . ? N2 Pd1 N1 C9 34.3(13) . . . . ? S1 Pd1 N1 C9 -150.0(12) . . . . ? N1 Pd1 N2 C12 -150.7(19) . . . . ? S2 Pd1 N2 C12 23.5(19) . . . . ? N1 Pd1 N2 C11 32.9(13) . . . . ? S2 Pd1 N2 C11 -152.8(12) . . . . ? Pd1 S1 C1 C2 -153.4(14) . . . . ? Pd1 S1 C1 C7 32.0(18) . . . . ? C7 C1 C2 C3 0(3) . . . . ? S1 C1 C2 C3 -175.1(15) . . . . ? C7 C1 C2 C24 -175.8(18) . . . 2 ? S1 C1 C2 C24 9(3) . . . 2 ? C1 C2 C3 C4 0(3) . . . . ? C24 C2 C3 C4 175(2) 2 . . . ? C2 C3 C4 C6 0(3) . . . . ? C2 C3 C4 C5 175(2) . . . . ? C3 C4 C5 C53 147(2) . . . . ? C6 C4 C5 C53 -37(3) . . . . ? C3 C4 C5 C52 -92(3) . . . . ? C6 C4 C5 C52 84(3) . . . . ? C3 C4 C5 C51 28(3) . . . . ? C6 C4 C5 C51 -157(2) . . . . ? C3 C4 C6 C7 1(3) . . . . ? C5 C4 C6 C7 -174.6(19) . . . . ? C4 C6 C7 C1 -2(3) . . . . ? C4 C6 C7 C8 -178.7(18) . . . . ? C2 C1 C7 C6 1(3) . . . . ? S1 C1 C7 C6 175.8(15) . . . . ? C2 C1 C7 C8 177.8(18) . . . . ? S1 C1 C7 C8 -7(3) . . . . ? C9 N1 C8 C7 173(2) . . . . ? Pd1 N1 C8 C7 2(3) . . . . ? C6 C7 C8 N1 162(2) . . . . ? C1 C7 C8 N1 -15(4) . . . . ? C8 N1 C9 C10 116(2) . . . . ? Pd1 N1 C9 C10 -72.2(18) . . . . ? N1 C9 C10 C11 33(3) . . . . ? C12 N2 C11 C10 106(2) . . . . ? Pd1 N2 C11 C10 -78(2) . . . . ? C9 C10 C11 N2 45(3) . . . . ? C11 N2 C12 C13 177(2) . . . . ? Pd1 N2 C12 C13 1(4) . . . . ? N2 C12 C13 C14 165(2) . . . . ? N2 C12 C13 C19 -18(4) . . . . ? C19 C13 C14 C15 0(3) . . . . ? C12 C13 C14 C15 177.4(19) . . . . ? C13 C14 C15 C17 2(3) . . . . ? C13 C14 C15 C16 -176.1(19) . . . . ? C14 C15 C16 C161 -174.1(19) . . . . ? C17 C15 C16 C161 7(3) . . . . ? C14 C15 C16 C162 63(3) . . . . ? C17 C15 C16 C162 -115(2) . . . . ? C14 C15 C16 C163 -54(2) . . . . ? C17 C15 C16 C163 127(2) . . . . ? C14 C15 C17 C18 -4(3) . . . . ? C16 C15 C17 C18 174.7(18) . . . . ? C15 C17 C18 C19 2(3) . . . . ? C15 C17 C18 C20 -175.5(17) . . . . ? C17 C18 C19 C13 0(3) . . . . ? C20 C18 C19 C13 178.4(17) . . . . ? C17 C18 C19 S2 -175.3(15) . . . . ? C20 C18 C19 S2 3(2) . . . . ? C14 C13 C19 C18 -2(3) . . . . ? C12 C13 C19 C18 -178.7(18) . . . . ? C14 C13 C19 S2 173.5(15) . . . . ? C12 C13 C19 S2 -3(3) . . . . ? Pd1 S2 C19 C18 -155.3(13) . . . . ? Pd1 S2 C19 C13 29.4(18) . . . . ? C21 N3 C20 C18 -177.4(18) . . . . ? C17 C18 C20 N3 30(3) . . . . ? C19 C18 C20 N3 -148.6(19) . . . . ? C20 N3 C21 C22 -128.9(19) . . . . ? N3 C21 C22 C23 64(2) . . . . ? C24 N4 C23 C22 -141(2) . . . . ? C21 C22 C23 N4 -173.3(18) . . . . ? C23 N4 C24 C2 -173.4(18) . . . 2 ? C32 N5 C31 O1 -178(3) . . . . ? C33 N5 C31 O1 7(5) . . . . ? C35 N6 C34 O2 19(7) . . . . ? C36 N6 C34 O2 -157(5) . . . . ? #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 282075' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 N12 O12 S4 Zn4, 5(C2 H3 N)' _chemical_formula_sum 'C70 H91 N17 O12 S4 Zn4' _chemical_formula_weight 1752.32 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' S S 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.567(2) _cell_length_b 22.548(3) _cell_length_c 26.568(3) _cell_angle_alpha 107.850(3) _cell_angle_beta 103.482(3) _cell_angle_gamma 102.425(3) _cell_volume 8207.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4957 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 15.79 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3640 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.463 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _exptl_special_details ; The crystal was relatively small and the unit cell is relatively large: the crystal diffracted relatively weakly. No appreciable data were observed beyond ca. 1 \%A and the data were truncated to this resolution. Within even this limit, only ca. 50% are observed at the 2\s(I) level and Rint is close to 15%. The resulting structure is of relatively low precision. The model is heavily restrained, with all chemically equivalent distances restrained to common values, with esd's of 0.002 \%A(!). Only Zn, S and O atoms are refined anisotropically. The acetonitrile solvent molecules are surprisingly well resolved and were refined using SAME restraints. On the basis of its displacement parameters, the molecule N10S-C20S might be refined with partial occupancy, but to do so complicates the empirical formula - under the circumstances, this was deemed unnecesary. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 65820 _diffrn_reflns_av_R_equivalents 0.1485 _diffrn_reflns_av_sigmaI/netI 0.2144 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 22.25 _diffrn_measured_fraction_theta_max 0.812 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.941 _reflns_number_total 16884 _reflns_number_gt 7972 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-8 (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1505P)^2^+23.2301P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16884 _refine_ls_number_parameters 984 _refine_ls_number_restraints 323 _refine_ls_R_factor_all 0.2123 _refine_ls_R_factor_gt 0.1007 _refine_ls_wR_factor_ref 0.3139 _refine_ls_wR_factor_gt 0.2526 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.493 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.143 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.20200(15) 0.57886(10) 0.08636(8) 0.0510(7) Uani 1 1 d . . . Zn2 Zn 0.41884(14) 0.74415(10) 0.38553(8) 0.0426(6) Uani 1 1 d . . . Zn3 Zn 0.02640(14) 0.48007(10) 0.32512(8) 0.0445(6) Uani 1 1 d . . . Zn4 Zn 0.30409(14) 0.31899(10) 0.15741(8) 0.0411(6) Uani 1 1 d . . . S1 S 0.2716(3) 0.5081(2) 0.1009(2) 0.0576(15) Uani 1 1 d D . . S2 S 0.3278(3) 0.7077(2) 0.29845(17) 0.0444(13) Uani 1 1 d D . . S3 S 0.1668(3) 0.55430(19) 0.36480(19) 0.0460(14) Uani 1 1 d D . . S4 S 0.1819(3) 0.3431(2) 0.18427(15) 0.0425(13) Uani 1 1 d D . . N1 N 0.0722(9) 0.5345(5) 0.0843(5) 0.048(4) Uiso 1 1 d D . . N2 N 0.2186(8) 0.6722(6) 0.1473(5) 0.038(4) Uiso 1 1 d D . . N3 N 0.5107(8) 0.7005(6) 0.3662(5) 0.043(4) Uiso 1 1 d D . . N4 N 0.3818(8) 0.7075(7) 0.4355(5) 0.051(4) Uiso 1 1 d D . . N5 N -0.0354(8) 0.5210(5) 0.2819(5) 0.046(4) Uiso 1 1 d D . . N6 N -0.0002(8) 0.3868(6) 0.2623(5) 0.040(4) Uiso 1 1 d D . . N7 N 0.4060(8) 0.3839(6) 0.2287(5) 0.043(4) Uiso 1 1 d D . . N8 N 0.3530(7) 0.3581(6) 0.1097(5) 0.038(4) Uiso 1 1 d D . . C1 C 0.1823(6) 0.4289(3) 0.0789(4) 0.038(5) Uiso 1 1 d GD . . C2 C 0.2138(4) 0.3746(5) 0.0714(4) 0.036(4) Uiso 1 1 d GD . . C3 C 0.1513(7) 0.3128(3) 0.0554(4) 0.043(5) Uiso 1 1 d G . . H3A H 0.1728 0.2757 0.0503 0.052 Uiso 1 1 calc R . . C4 C 0.0574(6) 0.3052(3) 0.0469(4) 0.043(5) Uiso 1 1 d GD . . C5 C 0.0260(4) 0.3595(5) 0.0544(4) 0.044(5) Uiso 1 1 d G . . H5A H -0.0382 0.3543 0.0486 0.053 Uiso 1 1 calc R . . C6 C 0.0884(6) 0.4213(3) 0.0704(4) 0.036(4) Uiso 1 1 d GD . . C7 C 0.0464(10) 0.4745(5) 0.0800(6) 0.045(5) Uiso 1 1 d D . . H7A H -0.0132 0.4616 0.0838 0.053 Uiso 1 1 calc R . . C8 C 0.0175(12) 0.5808(7) 0.0954(7) 0.071(6) Uiso 1 1 d D . . H8A H -0.0408 0.5563 0.0984 0.085 Uiso 1 1 calc R . . H8B H -0.0003 0.5911 0.0615 0.085 Uiso 1 1 calc R . . C9 C 0.0557(11) 0.6461(7) 0.1451(7) 0.065(6) Uiso 1 1 d D . . H9A H 0.0046 0.6654 0.1473 0.078 Uiso 1 1 calc R . . H9B H 0.0755 0.6373 0.1796 0.078 Uiso 1 1 calc R . . C10 C 0.1371(8) 0.6970(7) 0.1442(7) 0.050(5) Uiso 1 1 d D . . H10A H 0.1197 0.7055 0.1094 0.061 Uiso 1 1 calc R . . H10B H 0.1532 0.7386 0.1763 0.061 Uiso 1 1 calc R . . C11 C 0.2838(6) 0.7110(6) 0.1928(5) 0.037(5) Uiso 1 1 d D . . H11A H 0.2787 0.7491 0.2184 0.045 Uiso 1 1 calc R . . C12 C 0.4015(6) 0.6905(5) 0.2542(4) 0.042(5) Uiso 1 1 d GD . . C13 C 0.3670(5) 0.6899(5) 0.2008(4) 0.035(4) Uiso 1 1 d GD . . C14 C 0.4125(7) 0.6720(5) 0.1620(3) 0.039(5) Uiso 1 1 d G . . H14A H 0.3889 0.6716 0.1255 0.047 Uiso 1 1 calc R . . C15 C 0.4925(7) 0.6547(5) 0.1767(4) 0.055(5) Uiso 1 1 d GD . . C16 C 0.5270(5) 0.6552(5) 0.2301(4) 0.044(5) Uiso 1 1 d G . . H16A H 0.5817 0.6434 0.2401 0.053 Uiso 1 1 calc R . . C17 C 0.4815(6) 0.6731(5) 0.2688(3) 0.046(5) Uiso 1 1 d GD . . C18 C 0.5282(10) 0.6700(8) 0.3222(4) 0.046(5) Uiso 1 1 d D . . H18A H 0.5710 0.6457 0.3242 0.055 Uiso 1 1 calc R . . C19 C 0.5683(9) 0.6884(9) 0.4129(6) 0.060(6) Uiso 1 1 d D . . H19A H 0.6105 0.7305 0.4423 0.072 Uiso 1 1 calc R . . H19B H 0.6065 0.6614 0.3991 0.072 Uiso 1 1 calc R . . C20 C 0.5038(10) 0.6527(7) 0.4369(6) 0.045(5) Uiso 1 1 d D . . H20A H 0.5400 0.6341 0.4604 0.053 Uiso 1 1 calc R . . H20B H 0.4546 0.6156 0.4056 0.053 Uiso 1 1 calc R . . C21 C 0.4573(9) 0.6941(8) 0.4718(5) 0.041(5) Uiso 1 1 d D . . H21A H 0.4313 0.6707 0.4936 0.049 Uiso 1 1 calc R . . H21B H 0.5042 0.7361 0.4985 0.049 Uiso 1 1 calc R . . C22 C 0.3036(7) 0.6823(8) 0.4406(5) 0.046(5) Uiso 1 1 d D . . H22A H 0.2974 0.6621 0.4667 0.055 Uiso 1 1 calc R . . C23 C 0.1514(7) 0.6328(3) 0.3658(4) 0.035(4) Uiso 1 1 d GD . . C24 C 0.2251(6) 0.6883(5) 0.4018(4) 0.031(4) Uiso 1 1 d GD . . C25 C 0.2241(6) 0.7495(3) 0.4010(4) 0.048(5) Uiso 1 1 d G . . H25A H 0.2745 0.7874 0.4256 0.058 Uiso 1 1 calc R . . C26 C 0.1496(7) 0.7553(3) 0.3643(4) 0.042(5) Uiso 1 1 d GD . . C27 C 0.0759(6) 0.6998(5) 0.3283(4) 0.051(5) Uiso 1 1 d G . . H27A H 0.0249 0.7037 0.3032 0.061 Uiso 1 1 calc R . . C28 C 0.0768(6) 0.6386(3) 0.3290(4) 0.040(5) Uiso 1 1 d GD . . C29 C -0.0020(9) 0.5816(5) 0.2894(6) 0.061(6) Uiso 1 1 d D . . H29A H -0.0383 0.5924 0.2615 0.073 Uiso 1 1 calc R . . C30 C -0.1187(10) 0.4728(7) 0.2353(6) 0.059(6) Uiso 1 1 d D . . H30A H -0.1425 0.4957 0.2115 0.071 Uiso 1 1 calc R . . H30B H -0.1671 0.4599 0.2517 0.071 Uiso 1 1 calc R . . C31 C -0.1091(13) 0.4100(7) 0.1973(6) 0.058(6) Uiso 1 1 d D . . H31A H -0.1653 0.3895 0.1638 0.069 Uiso 1 1 calc R . . H31B H -0.0554 0.4224 0.1845 0.069 Uiso 1 1 calc R . . C32 C -0.0961(8) 0.3585(7) 0.2218(6) 0.045(5) Uiso 1 1 d D . . H32A H -0.1423 0.3503 0.2410 0.054 Uiso 1 1 calc R . . H32B H -0.1029 0.3167 0.1922 0.054 Uiso 1 1 calc R . . C33 C 0.0495(5) 0.3497(7) 0.2484(5) 0.040(5) Uiso 1 1 d D . . H33A H 0.0242 0.3094 0.2170 0.048 Uiso 1 1 calc R . . C34 C 0.2192(7) 0.3741(5) 0.26061(17) 0.045(5) Uiso 1 1 d GD . . C35 C 0.1472(5) 0.3728(5) 0.2833(3) 0.035(4) Uiso 1 1 d GD . . C36 C 0.1669(6) 0.3974(5) 0.3409(4) 0.039(5) Uiso 1 1 d G . . H36A H 0.1177 0.3965 0.3564 0.047 Uiso 1 1 calc R . . C37 C 0.2586(7) 0.4232(5) 0.37584(18) 0.037(5) Uiso 1 1 d GD . . C38 C 0.3306(5) 0.4245(5) 0.3532(3) 0.040(5) Uiso 1 1 d G . . H38A H 0.3933 0.4421 0.3770 0.048 Uiso 1 1 calc R . . C39 C 0.3109(6) 0.3999(5) 0.2955(3) 0.043(5) Uiso 1 1 d GD . . C40 C 0.3907(8) 0.4085(8) 0.2750(6) 0.046(5) Uiso 1 1 d D . . H40A H 0.4449 0.4404 0.3031 0.055 Uiso 1 1 calc R . . C41 C 0.5006(9) 0.4006(9) 0.2236(6) 0.051(5) Uiso 1 1 d D . . H41A H 0.5202 0.3607 0.2146 0.061 Uiso 1 1 calc R . . H41B H 0.5450 0.4329 0.2599 0.061 Uiso 1 1 calc R . . C42 C 0.5038(11) 0.4287(7) 0.1785(5) 0.044(5) Uiso 1 1 d D . . H42A H 0.5694 0.4487 0.1824 0.052 Uiso 1 1 calc R . . H42B H 0.4738 0.4637 0.1837 0.052 Uiso 1 1 calc R . . C43 C 0.4549(7) 0.3764(7) 0.1199(5) 0.045(5) Uiso 1 1 d D . . H43A H 0.4702 0.3935 0.0919 0.054 Uiso 1 1 calc R . . H43B H 0.4760 0.3374 0.1167 0.054 Uiso 1 1 calc R . . C44 C 0.3133(5) 0.3860(7) 0.0798(6) 0.044(5) Uiso 1 1 d D . . H44A H 0.3463 0.4122 0.0642 0.052 Uiso 1 1 calc R . . C45 C -0.0108(6) 0.2340(3) 0.0259(4) 0.048(5) Uiso 1 1 d D . . C46 C -0.0770(10) 0.2158(8) -0.0346(5) 0.072(6) Uiso 1 1 d D . . H46A H -0.1200 0.1714 -0.0478 0.108 Uiso 1 1 calc R . . H46B H -0.0400 0.2176 -0.0596 0.108 Uiso 1 1 calc R . . H46C H -0.1123 0.2469 -0.0342 0.108 Uiso 1 1 calc R . . C47 C -0.0694(11) 0.2369(8) 0.0666(5) 0.077(7) Uiso 1 1 d D . . H47A H -0.1140 0.1936 0.0555 0.116 Uiso 1 1 calc R . . H47B H -0.1030 0.2688 0.0650 0.116 Uiso 1 1 calc R . . H47C H -0.0280 0.2502 0.1048 0.116 Uiso 1 1 calc R . . C48 C 0.0380(10) 0.1802(7) 0.0260(6) 0.077(7) Uiso 1 1 d D . . H48A H -0.0091 0.1373 0.0124 0.115 Uiso 1 1 calc R . . H48B H 0.0773 0.1903 0.0641 0.115 Uiso 1 1 calc R . . H48C H 0.0765 0.1793 0.0015 0.115 Uiso 1 1 calc R . . C49 C 0.5431(7) 0.6302(5) 0.1335(4) 0.058(6) Uiso 1 1 d D . . C50 C 0.5326(11) 0.5553(5) 0.1158(7) 0.080(7) Uiso 1 1 d D . . H50A H 0.5652 0.5430 0.0887 0.121 Uiso 1 1 calc R . . H50B H 0.4666 0.5298 0.0988 0.121 Uiso 1 1 calc R . . H50C H 0.5595 0.5463 0.1488 0.121 Uiso 1 1 calc R . . C51 C 0.5024(10) 0.6441(8) 0.0800(6) 0.086(7) Uiso 1 1 d D . . H51A H 0.5335 0.6289 0.0526 0.128 Uiso 1 1 calc R . . H51B H 0.5127 0.6913 0.0901 0.128 Uiso 1 1 calc R . . H51C H 0.4356 0.6208 0.0637 0.128 Uiso 1 1 calc R . . C52 C 0.6489(8) 0.6704(7) 0.1605(6) 0.064(6) Uiso 1 1 d D . . H52A H 0.6819 0.6560 0.1341 0.095 Uiso 1 1 calc R . . H52B H 0.6746 0.6631 0.1947 0.095 Uiso 1 1 calc R . . H52C H 0.6565 0.7171 0.1697 0.095 Uiso 1 1 calc R . . C53 C 0.1581(6) 0.8267(3) 0.3671(4) 0.040(5) Uiso 1 1 d D . . C54 C 0.2456(7) 0.8849(6) 0.4090(5) 0.048(5) Uiso 1 1 d D . . H54A H 0.3018 0.8754 0.4030 0.071 Uiso 1 1 calc R . . H54B H 0.2475 0.8906 0.4474 0.071 Uiso 1 1 calc R . . H54C H 0.2425 0.9251 0.4029 0.071 Uiso 1 1 calc R . . C55 C 0.0685(7) 0.8421(7) 0.3764(5) 0.051(5) Uiso 1 1 d D . . H55A H 0.0136 0.8057 0.3502 0.076 Uiso 1 1 calc R . . H55B H 0.0656 0.8824 0.3701 0.076 Uiso 1 1 calc R . . H55C H 0.0701 0.8480 0.4148 0.076 Uiso 1 1 calc R . . C56 C 0.1555(9) 0.8173(7) 0.3060(4) 0.060(6) Uiso 1 1 d D . . H56A H 0.2117 0.8076 0.3002 0.089 Uiso 1 1 calc R . . H56B H 0.1526 0.8575 0.2996 0.089 Uiso 1 1 calc R . . H56C H 0.1006 0.7808 0.2797 0.089 Uiso 1 1 calc R . . C57 C 0.2792(7) 0.4476(5) 0.4404(2) 0.039(5) Uiso 1 1 d D . . C58 C 0.3305(10) 0.3992(6) 0.4538(7) 0.080(7) Uiso 1 1 d D . . H58A H 0.3854 0.4036 0.4415 0.120 Uiso 1 1 calc R . . H58B H 0.2885 0.3541 0.4342 0.120 Uiso 1 1 calc R . . H58C H 0.3498 0.4093 0.4941 0.120 Uiso 1 1 calc R . . C59 C 0.3463(10) 0.5194(5) 0.4713(7) 0.086(7) Uiso 1 1 d D . . H59A H 0.4014 0.5235 0.4592 0.129 Uiso 1 1 calc R . . H59B H 0.3652 0.5301 0.5117 0.129 Uiso 1 1 calc R . . H59C H 0.3144 0.5497 0.4624 0.129 Uiso 1 1 calc R . . C60 C 0.1919(8) 0.4409(8) 0.4604(7) 0.089(7) Uiso 1 1 d D . . H60A H 0.1501 0.3958 0.4412 0.134 Uiso 1 1 calc R . . H60B H 0.1594 0.4710 0.4516 0.134 Uiso 1 1 calc R . . H60C H 0.2116 0.4517 0.5008 0.134 Uiso 1 1 calc R . . N9 N 0.2054(10) 0.6117(8) 0.0024(7) 0.073(6) Uiso 1 1 d D . . O9A O 0.1383(10) 0.5948(9) 0.0181(6) 0.121(6) Uani 1 1 d D . . O9B O 0.2846(12) 0.6198(12) 0.0322(7) 0.167(9) Uani 1 1 d D . . O9C O 0.1950(11) 0.6316(9) -0.0366(7) 0.125(7) Uani 1 1 d D . . N10 N 0.5154(9) 0.8762(6) 0.4713(5) 0.052(4) Uiso 1 1 d D . . O10A O 0.4550(8) 0.8448(6) 0.4250(5) 0.058(4) Uani 1 1 d D . . O10B O 0.5507(9) 0.8391(6) 0.4890(5) 0.084(5) Uani 1 1 d D . . O10C O 0.5414(12) 0.9366(6) 0.4965(5) 0.104(6) Uani 1 1 d D . . N11 N -0.0649(11) 0.4874(6) 0.4004(6) 0.066(5) Uiso 1 1 d D . . O11A O -0.0429(9) 0.4442(6) 0.3688(5) 0.060(4) Uani 1 1 d D . . O11B O -0.0475(9) 0.5455(6) 0.4049(5) 0.067(4) Uani 1 1 d D . . O11C O -0.1026(10) 0.4774(7) 0.4347(6) 0.086(5) Uani 1 1 d D . . N12 N 0.3454(11) 0.1951(7) 0.1283(7) 0.080(6) Uiso 1 1 d D . . O12A O 0.2847(10) 0.2203(6) 0.1148(6) 0.085(5) Uani 1 1 d D . . O12B O 0.4113(14) 0.2431(8) 0.1628(11) 0.241(16) Uani 1 1 d D . . O12C O 0.3393(10) 0.1365(7) 0.1071(6) 0.096(5) Uani 1 1 d D . . Zn5 Zn 1.01083(13) 0.21756(10) 0.41976(8) 0.0376(6) Uani 1 1 d . . . Zn6 Zn 0.68915(13) 0.19816(9) 0.18757(8) 0.0390(6) Uani 1 1 d . . . Zn7 Zn 0.41538(13) -0.05900(9) 0.24874(8) 0.0377(6) Uani 1 1 d . . . Zn8 Zn 0.83908(13) -0.14904(10) 0.24166(8) 0.0381(6) Uani 1 1 d . . . S5 S 0.9617(3) 0.1116(2) 0.34963(18) 0.0465(13) Uani 1 1 d D . . S6 S 0.7763(3) 0.2244(2) 0.27255(17) 0.0464(14) Uani 1 1 d D . . S7 S 0.4816(3) 0.00115(19) 0.20859(17) 0.0446(13) Uani 1 1 d D . . S8 S 0.7220(3) -0.1147(2) 0.26769(16) 0.0456(14) Uani 1 1 d D . . N13 N 0.9329(8) 0.2049(5) 0.4721(5) 0.040(4) Uiso 1 1 d D . . N14 N 0.9698(8) 0.2931(5) 0.4109(4) 0.027(3) Uiso 1 1 d D . . N15 N 0.7577(8) 0.1470(6) 0.1390(5) 0.040(4) Uiso 1 1 d D . . N16 N 0.5668(7) 0.1270(6) 0.1472(4) 0.030(3) Uiso 1 1 d D . . N17 N 0.4355(8) 0.0154(6) 0.3243(5) 0.037(4) Uiso 1 1 d D . . N18 N 0.4738(8) -0.1196(6) 0.2738(4) 0.035(4) Uiso 1 1 d D . . N19 N 0.8216(7) -0.1517(7) 0.1664(5) 0.047(4) Uiso 1 1 d D . . N20 N 0.9652(8) -0.0743(5) 0.2781(4) 0.030(3) Uiso 1 1 d D . . C61 C 0.9377(7) 0.0623(4) 0.3907(4) 0.048(5) Uiso 1 1 d GD . . C62 C 0.9382(7) -0.0015(5) 0.3657(3) 0.029(4) Uiso 1 1 d GD . . C63 C 0.8982(7) -0.0503(3) 0.3824(4) 0.038(5) Uiso 1 1 d G . . H63A H 0.8985 -0.0940 0.3653 0.046 Uiso 1 1 calc R . . C64 C 0.8576(6) -0.0353(4) 0.4242(4) 0.025(4) Uiso 1 1 d GD A . C65 C 0.8572(6) 0.0285(4) 0.4492(3) 0.038(5) Uiso 1 1 d G . . H65A H 0.8295 0.0387 0.4778 0.045 Uiso 1 1 calc R . . C66 C 0.8972(7) 0.0773(3) 0.4325(4) 0.041(5) Uiso 1 1 d GD . . C67 C 0.8974(11) 0.1439(4) 0.4629(6) 0.050(5) Uiso 1 1 d D . . H67A H 0.8555 0.1408 0.4835 0.061 Uiso 1 1 calc R . . C68 C 0.9266(11) 0.2665(6) 0.5106(5) 0.045(5) Uiso 1 1 d D . . H68A H 0.9893 0.2918 0.5378 0.054 Uiso 1 1 calc R . . H68B H 0.8859 0.2545 0.5318 0.054 Uiso 1 1 calc R . . C69 C 0.8905(9) 0.3116(7) 0.4845(6) 0.038(5) Uiso 1 1 d D . . H69A H 0.8810 0.3470 0.5135 0.045 Uiso 1 1 calc R . . H69B H 0.8295 0.2862 0.4553 0.045 Uiso 1 1 calc R . . C70 C 0.9571(10) 0.3419(6) 0.4586(5) 0.039(5) Uiso 1 1 d D . . H70A H 0.9333 0.3738 0.4456 0.046 Uiso 1 1 calc R . . H70B H 1.0183 0.3663 0.4878 0.046 Uiso 1 1 calc R . . C71 C 0.9452(10) 0.2890(6) 0.3599(4) 0.043(5) Uiso 1 1 d D . . H71A H 0.9137 0.3189 0.3531 0.051 Uiso 1 1 calc R . . C72 C 0.8849(4) 0.2147(5) 0.2610(4) 0.033(4) Uiso 1 1 d GD . . C73 C 0.9586(6) 0.2450(4) 0.3108(3) 0.033(4) Uiso 1 1 d GD . . C74 C 1.0449(5) 0.2362(5) 0.3127(3) 0.031(4) Uiso 1 1 d G . . H74A H 1.0952 0.2569 0.3467 0.037 Uiso 1 1 calc R . . C75 C 1.0574(4) 0.1971(5) 0.2649(4) 0.035(4) Uiso 1 1 d GD . . C76 C 0.9837(6) 0.1668(4) 0.2151(3) 0.036(4) Uiso 1 1 d G . . H76A H 0.9922 0.1401 0.1824 0.043 Uiso 1 1 calc R . . C77 C 0.8975(5) 0.1756(5) 0.2132(3) 0.034(4) Uiso 1 1 d GD . . C78 C 0.8384(8) 0.1403(7) 0.1547(4) 0.036(4) Uiso 1 1 d D . . H78A H 0.8596 0.1128 0.1287 0.043 Uiso 1 1 calc R . . C79 C 0.7112(9) 0.1074(7) 0.0784(5) 0.048(5) Uiso 1 1 d D . . H79A H 0.7501 0.0810 0.0645 0.057 Uiso 1 1 calc R . . H79B H 0.7059 0.1372 0.0579 0.057 Uiso 1 1 calc R . . C80 C 0.6147(8) 0.0617(7) 0.0663(7) 0.043(5) Uiso 1 1 d D . . H80A H 0.5876 0.0368 0.0255 0.052 Uiso 1 1 calc R . . H80B H 0.6214 0.0297 0.0842 0.052 Uiso 1 1 calc R . . C81 C 0.5463(10) 0.0950(8) 0.0859(5) 0.042(5) Uiso 1 1 d D . . H81A H 0.5424 0.1285 0.0694 0.051 Uiso 1 1 calc R . . H81B H 0.4842 0.0617 0.0704 0.051 Uiso 1 1 calc R . . C82 C 0.5077(8) 0.1000(6) 0.1665(3) 0.028(4) Uiso 1 1 d D . . H82A H 0.4581 0.0613 0.1428 0.034 Uiso 1 1 calc R . . C83 C 0.4937(7) 0.0863(2) 0.2509(4) 0.027(4) Uiso 1 1 d GD . . C84 C 0.5183(7) 0.1303(4) 0.2259(3) 0.040(5) Uiso 1 1 d GD . . C85 C 0.5402(7) 0.1972(4) 0.2552(4) 0.040(5) Uiso 1 1 d G . . H85A H 0.5570 0.2273 0.2380 0.048 Uiso 1 1 calc R . . C86 C 0.5376(7) 0.2201(2) 0.3095(4) 0.051(5) Uiso 1 1 d GD . . C87 C 0.5131(7) 0.1761(4) 0.3346(3) 0.048(5) Uiso 1 1 d G . . H87A H 0.5113 0.1918 0.3717 0.058 Uiso 1 1 calc R . . C88 C 0.4911(7) 0.1092(4) 0.3053(4) 0.031(4) Uiso 1 1 d GD . . C89 C 0.4631(10) 0.0784(6) 0.3425(5) 0.042(5) Uiso 1 1 d D . . H89A H 0.4653 0.1040 0.3789 0.050 Uiso 1 1 calc R . . C90 C 0.4220(11) -0.0058(8) 0.3704(6) 0.046(5) Uiso 1 1 d D . . H90A H 0.3563 -0.0310 0.3616 0.055 Uiso 1 1 calc R . . H90B H 0.4412 0.0322 0.4060 0.055 Uiso 1 1 calc R . . C91 C 0.4849(11) -0.0489(6) 0.3732(6) 0.049(5) Uiso 1 1 d D . . H91A H 0.4925 -0.0550 0.4092 0.059 Uiso 1 1 calc R . . H91B H 0.5467 -0.0234 0.3753 0.059 Uiso 1 1 calc R . . C92 C 0.4600(12) -0.1167(7) 0.3280(5) 0.044(5) Uiso 1 1 d D . . H92A H 0.4972 -0.1414 0.3433 0.053 Uiso 1 1 calc R . . H92B H 0.3939 -0.1399 0.3203 0.053 Uiso 1 1 calc R . . C93 C 0.5264(10) -0.1496(7) 0.2528(4) 0.034(4) Uiso 1 1 d D . . H93A H 0.5558 -0.1700 0.2751 0.041 Uiso 1 1 calc R . . C94 C 0.6386(5) -0.1524(5) 0.1974(2) 0.040(5) Uiso 1 1 d GD . . C95 C 0.5497(6) -0.1583(5) 0.2011(3) 0.038(5) Uiso 1 1 d GD . . C96 C 0.4761(5) -0.1704(5) 0.1542(4) 0.038(5) Uiso 1 1 d G . . H96A H 0.4154 -0.1745 0.1568 0.045 Uiso 1 1 calc R . . C97 C 0.4912(5) -0.1766(5) 0.1036(3) 0.037(5) Uiso 1 1 d GD . . C98 C 0.5801(6) -0.1706(5) 0.0999(2) 0.045(5) Uiso 1 1 d G . . H98A H 0.5904 -0.1747 0.0653 0.054 Uiso 1 1 calc R . . C99 C 0.6537(4) -0.1585(5) 0.1468(3) 0.039(5) Uiso 1 1 d GD . . C100 C 0.7430(6) -0.1532(8) 0.1362(6) 0.042(5) Uiso 1 1 d D . . H10C H 0.7426 -0.1503 0.1012 0.050 Uiso 1 1 calc R . . C101 C 0.9003(8) -0.1474(7) 0.1436(6) 0.037(4) Uiso 1 1 d D . . H10D H 0.8803 -0.1458 0.1059 0.044 Uiso 1 1 calc R . . H10E H 0.9215 -0.1864 0.1404 0.044 Uiso 1 1 calc R . . C102 C 0.9791(10) -0.0853(7) 0.1831(5) 0.045(5) Uiso 1 1 d D . . H10F H 1.0281 -0.0791 0.1655 0.054 Uiso 1 1 calc R . . H10G H 0.9549 -0.0475 0.1875 0.054 Uiso 1 1 calc R . . C103 C 1.0237(9) -0.0842(9) 0.2411(5) 0.048(5) Uiso 1 1 d D . . H10H H 1.0368 -0.1262 0.2372 0.057 Uiso 1 1 calc R . . H10I H 1.0838 -0.0487 0.2592 0.057 Uiso 1 1 calc R . . C104 C 0.9807(10) -0.0238(7) 0.3223(5) 0.048(5) Uiso 1 1 d D . . H10J H 1.0365 0.0089 0.3289 0.058 Uiso 1 1 calc R . . C105 C 0.8125(8) -0.0909(5) 0.4421(6) 0.044(5) Uiso 1 1 d D . . C106 C 0.8952(13) -0.1153(14) 0.4635(11) 0.072(13) Uiso 0.50 1 d PD A 1 H10K H 0.9531 -0.0867 0.4643 0.108 Uiso 0.50 1 calc PR A 1 H10L H 0.8845 -0.1602 0.4385 0.108 Uiso 0.50 1 calc PR A 1 H10M H 0.9001 -0.1142 0.5013 0.108 Uiso 0.50 1 calc PR A 1 C107 C 0.7752(19) -0.0622(13) 0.4910(9) 0.062(12) Uiso 0.50 1 d PD A 1 H10N H 0.8271 -0.0402 0.5260 0.093 Uiso 0.50 1 calc PR A 1 H10O H 0.7304 -0.0978 0.4939 0.093 Uiso 0.50 1 calc PR A 1 H10P H 0.7447 -0.0306 0.4836 0.093 Uiso 0.50 1 calc PR A 1 C108 C 0.7330(14) -0.1494(11) 0.3936(8) 0.059(11) Uiso 0.50 1 d PD A 1 H10Q H 0.7601 -0.1793 0.3720 0.089 Uiso 0.50 1 calc PR A 1 H10R H 0.6963 -0.1327 0.3692 0.089 Uiso 0.50 1 calc PR A 1 H10S H 0.6929 -0.1730 0.4093 0.089 Uiso 0.50 1 calc PR A 1 C10A C 0.828(2) -0.1579(10) 0.4140(12) 0.073(13) Uiso 0.50 1 d PD A 2 H10T H 0.8944 -0.1520 0.4225 0.109 Uiso 0.50 1 calc PR A 2 H10U H 0.7983 -0.1740 0.3734 0.109 Uiso 0.50 1 calc PR A 2 H10V H 0.7999 -0.1898 0.4283 0.109 Uiso 0.50 1 calc PR A 2 C10B C 0.860(2) -0.0647(15) 0.5066(6) 0.096(16) Uiso 0.50 1 d PD A 2 H10W H 0.9273 -0.0580 0.5148 0.144 Uiso 0.50 1 calc PR A 2 H10X H 0.8341 -0.0967 0.5214 0.144 Uiso 0.50 1 calc PR A 2 H10Y H 0.8500 -0.0230 0.5242 0.144 Uiso 0.50 1 calc PR A 2 C10C C 0.7061(10) -0.1002(16) 0.4289(14) 0.122(19) Uiso 0.50 1 d PD A 2 H10Z H 0.6967 -0.0580 0.4460 0.183 Uiso 0.50 1 calc PR A 2 H11B H 0.6789 -0.1314 0.4441 0.183 Uiso 0.50 1 calc PR A 2 H11C H 0.6761 -0.1172 0.3884 0.183 Uiso 0.50 1 calc PR A 2 C109 C 1.1457(5) 0.1767(5) 0.2594(4) 0.050(5) Uiso 1 1 d D . . C110 C 1.1801(10) 0.1852(6) 0.2104(5) 0.049(5) Uiso 1 1 d D . . H11D H 1.2355 0.1710 0.2110 0.073 Uiso 1 1 calc R . . H11E H 1.1954 0.2313 0.2148 0.073 Uiso 1 1 calc R . . H11F H 1.1310 0.1584 0.1747 0.073 Uiso 1 1 calc R . . C111 C 1.1290(10) 0.1040(5) 0.2548(5) 0.047(5) Uiso 1 1 d D . . H11G H 1.1842 0.0911 0.2511 0.071 Uiso 1 1 calc R . . H11H H 1.0753 0.0754 0.2219 0.071 Uiso 1 1 calc R . . H11I H 1.1172 0.1000 0.2884 0.071 Uiso 1 1 calc R . . C112 C 1.2216(10) 0.2232(6) 0.3163(4) 0.064(6) Uiso 1 1 d D . . H11J H 1.2809 0.2146 0.3171 0.096 Uiso 1 1 calc R . . H11K H 1.2028 0.2153 0.3470 0.096 Uiso 1 1 calc R . . H11L H 1.2288 0.2689 0.3206 0.096 Uiso 1 1 calc R . . C113 C 0.5697(9) 0.2951(3) 0.3469(5) 0.084(7) Uiso 1 1 d D . . C114 C 0.4966(10) 0.3169(9) 0.3740(7) 0.098(8) Uiso 1 1 d D . . H11M H 0.5212 0.3639 0.3968 0.148 Uiso 1 1 calc R . . H11N H 0.4842 0.2924 0.3977 0.148 Uiso 1 1 calc R . . H11O H 0.4389 0.3080 0.3445 0.148 Uiso 1 1 calc R . . C115 C 0.5888(13) 0.3347(10) 0.3093(7) 0.132(10) Uiso 1 1 d D . . H11P H 0.6102 0.3818 0.3319 0.198 Uiso 1 1 calc R . . H11Q H 0.5314 0.3242 0.2789 0.198 Uiso 1 1 calc R . . H11R H 0.6365 0.3230 0.2935 0.198 Uiso 1 1 calc R . . C116 C 0.6626(10) 0.3117(10) 0.3947(7) 0.104(8) Uiso 1 1 d D . . H11S H 0.6838 0.3586 0.4178 0.156 Uiso 1 1 calc R . . H11T H 0.7101 0.3008 0.3782 0.156 Uiso 1 1 calc R . . H11U H 0.6521 0.2862 0.4178 0.156 Uiso 1 1 calc R . . C117 C 0.4156(6) -0.1895(6) 0.0482(3) 0.061(6) Uiso 1 1 d D . . C118 C 0.3198(9) -0.1968(8) 0.0582(7) 0.073(6) Uiso 1 1 d D . . H11V H 0.3007 -0.2369 0.0654 0.110 Uiso 1 1 calc R . . H11W H 0.2734 -0.1991 0.0250 0.110 Uiso 1 1 calc R . . H11X H 0.3252 -0.1588 0.0905 0.110 Uiso 1 1 calc R . . C119 C 0.4099(12) -0.2511(7) -0.0011(6) 0.090(7) Uiso 1 1 d D . . H11Y H 0.3890 -0.2904 0.0068 0.136 Uiso 1 1 calc R . . H11Z H 0.4714 -0.2471 -0.0056 0.136 Uiso 1 1 calc R . . H12A H 0.3657 -0.2544 -0.0356 0.136 Uiso 1 1 calc R . . C120 C 0.4463(12) -0.1266(6) 0.0357(8) 0.098(8) Uiso 1 1 d D . . H12B H 0.5067 -0.1225 0.0296 0.146 Uiso 1 1 calc R . . H12C H 0.4515 -0.0881 0.0675 0.146 Uiso 1 1 calc R . . H12D H 0.4001 -0.1295 0.0022 0.146 Uiso 1 1 calc R . . N21 N 1.1789(9) 0.2803(7) 0.4915(5) 0.066(5) Uiso 1 1 d D . . O21A O 1.1481(8) 0.2402(7) 0.4425(5) 0.069(4) Uani 1 1 d D . . O21B O 1.2644(9) 0.2972(7) 0.5135(6) 0.096(5) Uani 1 1 d D . . O21C O 1.1351(9) 0.3085(7) 0.5191(5) 0.083(5) Uani 1 1 d D . . N22 N 0.6631(11) 0.2966(7) 0.1623(7) 0.059(5) Uiso 1 1 d D . . O22A O 0.6946(12) 0.2577(8) 0.1336(8) 0.126(6) Uani 1 1 d D . . O22B O 0.6529(12) 0.2922(8) 0.2061(7) 0.134(7) Uani 1 1 d D . . O22C O 0.6550(9) 0.3481(7) 0.1569(6) 0.079(4) Uani 1 1 d D . . N23 N 0.2321(8) -0.1038(5) 0.2019(6) 0.050(4) Uiso 1 1 d D . . O23A O 0.2927(7) -0.1306(5) 0.2107(4) 0.047(3) Uani 1 1 d D . . O23B O 0.2499(8) -0.0435(6) 0.2241(5) 0.068(4) Uani 1 1 d D . . O23C O 0.1558(8) -0.1444(6) 0.1708(5) 0.068(4) Uani 1 1 d D . . N24 N 0.8816(10) -0.2582(6) 0.2407(6) 0.057(5) Uiso 1 1 d D . . O24A O 0.8501(8) -0.2215(6) 0.2714(5) 0.065(4) Uani 1 1 d D . . O24C O 0.8984(8) -0.3094(6) 0.2413(5) 0.066(4) Uani 1 1 d D . . O24B O 0.9031(10) -0.2460(7) 0.2020(6) 0.091(5) Uani 1 1 d D . . N1S N 0.2118(12) 0.0194(8) 0.3639(7) 0.085(6) Uiso 1 1 d D . . C1S C 0.2481(13) 0.0790(8) 0.3842(8) 0.068(6) Uiso 1 1 d D . . C2S C 0.2928(14) 0.1458(8) 0.4082(8) 0.081(7) Uiso 1 1 d D . . H2S1 H 0.2459 0.1682 0.4037 0.121 Uiso 1 1 d R . . H2S2 H 0.3378 0.1583 0.3900 0.121 Uiso 1 1 d R . . H2S3 H 0.3251 0.1584 0.4481 0.121 Uiso 1 1 d R . . N2S N 0.2839(11) -0.0419(8) 0.0502(7) 0.078(5) Uiso 1 1 d D . . C3S C 0.2529(13) -0.0173(9) 0.0871(7) 0.067(6) Uiso 1 1 d D . . C4S C 0.2207(15) 0.0115(11) 0.1297(8) 0.094(8) Uiso 1 1 d D . . H4S1 H 0.2665 0.0216 0.1659 0.141 Uiso 1 1 d R . . H4S2 H 0.1623 -0.0192 0.1259 0.141 Uiso 1 1 d R . . H4S3 H 0.2099 0.0519 0.1273 0.141 Uiso 1 1 d R . . N3S N 0.7777(13) -0.0175(9) 0.1213(7) 0.099(6) Uiso 1 1 d D . . C5S C 0.7621(13) 0.0030(9) 0.1656(7) 0.068(6) Uiso 1 1 d D . . C6S C 0.7446(14) 0.0251(10) 0.2156(7) 0.075(7) Uiso 1 1 d D . . H6S1 H 0.6786 0.0040 0.2084 0.113 Uiso 1 1 d R . . H6S2 H 0.7577 0.0727 0.2291 0.113 Uiso 1 1 d R . . H6S3 H 0.7824 0.0134 0.2438 0.113 Uiso 1 1 d R . . N4S N 0.7051(14) 0.5801(10) 0.2667(8) 0.118(7) Uiso 1 1 d D . . C7S C 0.7641(15) 0.6277(10) 0.3051(9) 0.093(8) Uiso 1 1 d D . . C8S C 0.8301(15) 0.6802(10) 0.3497(9) 0.105(8) Uiso 1 1 d D . . H8S1 H 0.8061 0.6946 0.3808 0.158 Uiso 1 1 d R . . H8S2 H 0.8469 0.7161 0.3368 0.158 Uiso 1 1 d R . . H8S3 H 0.8852 0.6674 0.3621 0.158 Uiso 1 1 d R . . N5S N 0.6770(11) 0.1619(8) 0.4415(7) 0.081(5) Uiso 1 1 d D . . C9S C 0.6910(14) 0.1311(10) 0.3989(7) 0.079(7) Uiso 1 1 d D . . C10S C 0.7040(14) 0.0978(10) 0.3496(7) 0.083(7) Uiso 1 1 d D . . H100 H 0.6437 0.0786 0.3199 0.125 Uiso 1 1 d R . . H101 H 0.7299 0.0629 0.3535 0.125 Uiso 1 1 d R . . H102 H 0.7465 0.1281 0.3401 0.125 Uiso 1 1 d R . . N6S N 0.9946(13) 0.0318(10) 0.0817(8) 0.122(7) Uiso 1 1 d D . . C11S C 0.9248(14) -0.0074(10) 0.0438(9) 0.096(8) Uiso 1 1 d D . . C12S C 0.8452(13) -0.0538(10) 0.0037(8) 0.086(7) Uiso 1 1 d D . . H12E H 0.8447 -0.0978 0.0023 0.129 Uiso 1 1 d R . . H12F H 0.8438 -0.0514 -0.0327 0.129 Uiso 1 1 d R . . H12G H 0.7906 -0.0447 0.0126 0.129 Uiso 1 1 d R . . N7S N 0.3659(13) 0.5335(15) 0.2682(13) 0.079(11) Uiso 0.50 1 d PD B 1 C13S C 0.2837(11) 0.5278(9) 0.2484(8) 0.071(6) Uiso 0.50 1 d PD B 1 C14S C 0.1940(12) 0.5278(9) 0.2265(8) 0.086(7) Uiso 0.50 1 d PD B 1 H14B H 0.1694 0.5414 0.2574 0.129 Uiso 0.50 1 d PR B 1 H14C H 0.1550 0.4837 0.2002 0.129 Uiso 0.50 1 d PR B 1 H14D H 0.1937 0.5585 0.2072 0.129 Uiso 0.50 1 d PR B 1 N7T N 0.1168(14) 0.5332(14) 0.2093(12) 0.066(10) Uiso 0.50 1 d PD C 2 C13T C 0.1940(12) 0.5278(9) 0.2265(8) 0.086(7) Uiso 0.50 1 d PD C 2 C14T C 0.2837(11) 0.5278(9) 0.2484(8) 0.071(6) Uiso 0.50 1 d PD C 2 H14E H 0.3059 0.5095 0.2158 0.106 Uiso 0.50 1 d PR C 2 H14F H 0.2863 0.5032 0.2707 0.106 Uiso 0.50 1 d PR C 2 H14G H 0.3255 0.5740 0.2691 0.106 Uiso 0.50 1 d PR C 2 N8S N 0.1600(18) 0.3566(14) -0.0668(13) 0.205(13) Uiso 1 1 d D . . C15S C 0.2166(16) 0.3286(12) -0.0549(11) 0.113(9) Uiso 1 1 d D . . C16S C 0.2808(12) 0.2974(9) -0.0415(7) 0.059(6) Uiso 1 1 d D . . H16B H 0.2483 0.2502 -0.0576 0.088 Uiso 1 1 d R . . H16C H 0.3070 0.3117 -0.0009 0.088 Uiso 1 1 d R . . H16D H 0.3309 0.3069 -0.0571 0.088 Uiso 1 1 d R . . N9S N 0.7425(13) 0.5313(12) 0.3792(10) 0.152(9) Uiso 1 1 d D . . C17S C 0.6655(13) 0.5286(11) 0.3844(9) 0.098(8) Uiso 1 1 d D . . C18S C 0.5808(12) 0.5200(9) 0.3936(8) 0.065(6) Uiso 1 1 d D . . H18B H 0.5411 0.4750 0.3705 0.097 Uiso 1 1 d R . . H18C H 0.5509 0.5507 0.3836 0.097 Uiso 1 1 d R . . H18D H 0.5901 0.5274 0.4331 0.097 Uiso 1 1 d R . . N10S N -0.332(3) 0.430(2) 0.0869(19) 0.29(2) Uiso 1 1 d D . . C19S C -0.268(3) 0.481(2) 0.104(2) 0.30(3) Uiso 1 1 d D . . C20S C -0.188(3) 0.534(2) 0.123(2) 0.30(3) Uiso 1 1 d D . . H20C H -0.1357 0.5220 0.1410 0.443 Uiso 1 1 d R . . H20D H -0.1934 0.5729 0.1504 0.443 Uiso 1 1 d R . . H20E H -0.1786 0.5437 0.0912 0.443 Uiso 1 1 d R . . 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 0.0572(16) 0.0371(15) 0.0362(14) 0.0023(12) -0.0014(11) 0.0055(12) Zn2 0.0440(14) 0.0389(15) 0.0351(14) 0.0126(12) 0.0021(10) 0.0076(11) Zn3 0.0437(14) 0.0296(14) 0.0388(14) -0.0023(11) 0.0034(11) 0.0025(11) Zn4 0.0404(14) 0.0361(14) 0.0336(14) 0.0057(11) 0.0037(10) 0.0059(11) S1 0.049(3) 0.031(3) 0.072(4) 0.007(3) 0.012(3) 0.000(3) S2 0.045(3) 0.037(3) 0.040(3) 0.009(3) 0.002(2) 0.011(3) S3 0.048(3) 0.022(3) 0.050(3) 0.007(3) 0.000(2) 0.003(3) S4 0.039(3) 0.041(3) 0.026(3) -0.002(3) 0.000(2) 0.002(3) O9A 0.094(13) 0.177(18) 0.047(10) 0.006(11) 0.003(9) 0.027(13) O9B 0.123(16) 0.34(3) 0.101(14) 0.127(18) 0.036(12) 0.124(19) O9C 0.098(13) 0.188(19) 0.093(13) 0.084(13) 0.011(10) 0.025(12) O10A 0.060(9) 0.051(9) 0.038(8) 0.010(7) -0.009(6) 0.002(7) O10B 0.069(10) 0.063(10) 0.079(11) 0.032(9) -0.028(8) -0.008(8) O10C 0.186(17) 0.038(10) 0.037(9) -0.005(8) -0.010(9) 0.011(10) O11A 0.085(10) 0.035(8) 0.066(9) 0.006(7) 0.045(8) 0.028(8) O11B 0.083(10) 0.051(10) 0.057(9) 0.006(8) 0.023(7) 0.021(8) O11C 0.112(13) 0.090(12) 0.082(11) 0.045(10) 0.052(9) 0.042(10) O12A 0.109(12) 0.050(10) 0.075(11) 0.008(8) 0.004(9) 0.035(9) O12B 0.19(2) 0.069(14) 0.28(3) -0.026(16) -0.14(2) 0.054(15) O12C 0.097(12) 0.049(11) 0.116(13) 0.017(10) 0.003(10) 0.025(9) Zn5 0.0424(14) 0.0331(14) 0.0251(13) 0.0020(11) 0.0047(10) 0.0076(11) Zn6 0.0394(14) 0.0298(14) 0.0264(13) -0.0001(11) -0.0039(10) 0.0008(11) Zn7 0.0451(14) 0.0299(14) 0.0259(13) 0.0043(11) 0.0038(10) 0.0051(11) Zn8 0.0383(13) 0.0348(14) 0.0322(13) 0.0074(11) 0.0049(10) 0.0082(11) S5 0.064(4) 0.032(3) 0.035(3) 0.005(3) 0.013(3) 0.011(3) S6 0.045(3) 0.053(4) 0.021(3) -0.004(3) -0.002(2) 0.015(3) S7 0.064(4) 0.027(3) 0.028(3) -0.001(2) 0.009(2) 0.008(3) S8 0.041(3) 0.060(4) 0.030(3) 0.013(3) 0.005(2) 0.016(3) O21A 0.050(9) 0.085(11) 0.040(9) -0.006(8) -0.003(7) 0.019(8) O21B 0.059(10) 0.100(13) 0.082(11) 0.020(10) -0.018(8) 0.002(9) O21C 0.071(10) 0.102(12) 0.040(9) 0.000(8) 0.003(7) 0.016(9) O22A 0.143(16) 0.073(13) 0.186(19) 0.051(13) 0.072(14) 0.058(12) O22B 0.143(17) 0.128(16) 0.123(16) 0.080(13) 0.017(12) 0.006(13) O22C 0.067(10) 0.060(10) 0.123(13) 0.058(10) 0.020(8) 0.020(8) O23A 0.047(8) 0.035(8) 0.049(8) 0.014(7) 0.007(6) 0.009(7) O23B 0.065(9) 0.054(10) 0.078(10) 0.022(8) 0.007(7) 0.028(8) O23C 0.037(8) 0.078(10) 0.071(10) 0.017(8) 0.000(7) 0.017(8) O24A 0.050(9) 0.038(9) 0.082(10) -0.014(8) 0.024(7) 0.014(7) O24C 0.073(10) 0.057(10) 0.071(10) 0.022(8) 0.019(7) 0.033(8) O24B 0.111(13) 0.085(12) 0.065(11) 0.021(9) 0.017(9) 0.029(10) _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 O9A 2.029(15) . ? Zn1 N1 2.032(12) . ? Zn1 N2 2.144(12) . ? Zn1 S1 2.190(5) . ? Zn1 O9B 2.397(18) . ? Zn2 N4 1.896(12) . ? Zn2 N3 1.979(12) . ? Zn2 O10A 2.070(12) . ? Zn2 S2 2.200(5) . ? Zn3 N5 1.901(12) . ? Zn3 O11A 1.988(12) . ? Zn3 N6 2.130(12) . ? Zn3 S3 2.227(5) . ? Zn4 N8 1.953(12) . ? Zn4 N7 2.036(12) . ? Zn4 O12A 2.081(13) . ? Zn4 S4 2.294(5) . ? S1 C1 1.837(3) . ? S2 C12 1.842(3) . ? S3 C23 1.831(3) . ? S4 C34 1.829(3) . ? N1 C7 1.287(5) . ? N1 C8 1.488(5) . ? N2 C11 1.287(5) . ? N2 C10 1.488(5) . ? N3 C18 1.286(5) . ? N3 C19 1.487(5) . ? N4 C22 1.286(5) . ? N4 C21 1.486(5) . ? N5 C29 1.287(5) . ? N5 C30 1.488(5) . ? N6 C33 1.287(5) . ? N6 C32 1.487(5) . ? N7 C40 1.287(5) . ? N7 C41 1.487(5) . ? N8 C44 1.285(5) . ? N8 C43 1.487(5) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 C44 1.466(4) . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 C45 1.567(3) . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 C7 1.468(4) . ? C7 H7A 0.9500 . ? C8 C9 1.526(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.525(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C13 1.465(4) . ? C11 H11A 0.9500 . ? C12 C13 1.3900 . ? C12 C17 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C14 H14A 0.9500 . ? C15 C16 1.3900 . ? C15 C49 1.570(3) . ? C16 C17 1.3900 . ? C16 H16A 0.9500 . ? C17 C18 1.465(4) . ? C18 H18A 0.9500 . ? C19 C20 1.525(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.526(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C24 1.465(4) . ? C22 H22A 0.9500 . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C25 H25A 0.9500 . ? C26 C27 1.3900 . ? C26 C53 1.563(3) . ? C27 C28 1.3900 . ? C27 H27A 0.9500 . ? C28 C29 1.468(4) . ? C29 H29A 0.9500 . ? C30 C31 1.526(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.525(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C35 1.467(4) . ? C33 H33A 0.9500 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C36 H36A 0.9500 . ? C37 C38 1.3900 . ? C37 C57 1.562(3) . ? C38 C39 1.3900 . ? C38 H38A 0.9500 . ? C39 C40 1.467(4) . ? C40 H40A 0.9500 . ? C41 C42 1.525(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.526(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9500 . ? C45 C47 1.565(3) . ? C45 C48 1.565(3) . ? C45 C46 1.565(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C51 1.567(3) . ? C49 C52 1.568(3) . ? C49 C50 1.569(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C56 1.563(3) . ? C53 C54 1.563(3) . ? C53 C55 1.563(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.562(3) . ? C57 C60 1.563(3) . ? C57 C59 1.563(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? N9 O9B 1.240(3) . ? N9 O9C 1.240(3) . ? N9 O9A 1.241(3) . ? N10 O10B 1.241(3) . ? N10 O10A 1.242(3) . ? N10 O10C 1.242(3) . ? N11 O11C 1.241(3) . ? N11 O11B 1.243(3) . ? N11 O11A 1.243(3) . ? N12 O12B 1.241(3) . ? N12 O12C 1.241(3) . ? N12 O12A 1.241(3) . ? Zn5 O21A 1.983(12) . ? Zn5 N14 2.002(11) . ? Zn5 N13 2.090(12) . ? Zn5 S5 2.364(5) . ? Zn6 N16 2.007(11) . ? Zn6 N15 2.095(12) . ? Zn6 S6 2.167(4) . ? Zn6 O22A 2.248(17) . ? Zn6 O22B 2.250(18) . ? Zn7 N18 1.988(11) . ? Zn7 O23A 2.013(11) . ? Zn7 N17 2.088(12) . ? Zn7 S7 2.199(5) . ? Zn8 N19 1.933(12) . ? Zn8 O24A 2.042(13) . ? Zn8 N20 2.079(11) . ? Zn8 S8 2.295(5) . ? S5 C61 1.822(3) . ? S6 C72 1.834(3) . ? S7 C83 1.846(3) . ? S8 C94 1.821(3) . ? N13 C67 1.289(5) . ? N13 C68 1.489(5) . ? N14 C71 1.286(5) . ? N14 C70 1.489(5) . ? N15 C78 1.286(5) . ? N15 C79 1.488(5) . ? N16 C82 1.285(5) . ? N16 C81 1.488(5) . ? N17 C89 1.287(5) . ? N17 C90 1.487(5) . ? N18 C93 1.288(5) . ? N18 C92 1.488(5) . ? N19 C100 1.286(5) . ? N19 C101 1.487(5) . ? N20 C104 1.289(5) . ? N20 C103 1.488(5) . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C62 C104 1.470(4) . ? C63 C64 1.3900 . ? C63 H63A 0.9500 . ? C64 C65 1.3900 . ? C64 C105 1.560(3) . ? C65 C66 1.3900 . ? C65 H65A 0.9500 . ? C66 C67 1.471(4) . ? C67 H67A 0.9500 . ? C68 C69 1.525(5) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.526(5) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C73 1.469(4) . ? C71 H71A 0.9500 . ? C72 C73 1.3900 . ? C72 C77 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C74 H74A 0.9500 . ? C75 C76 1.3900 . ? C75 C109 1.565(3) . ? C76 C77 1.3900 . ? C76 H76A 0.9500 . ? C77 C78 1.467(4) . ? C78 H78A 0.9500 . ? C79 C80 1.526(5) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.526(5) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C84 1.466(4) . ? C82 H82A 0.9500 . ? C83 C84 1.3900 . ? C83 C88 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? C85 H85A 0.9500 . ? C86 C87 1.3900 . ? C86 C113 1.571(3) . ? C87 C88 1.3900 . ? C87 H87A 0.9500 . ? C88 C89 1.466(4) . ? C89 H89A 0.9500 . ? C90 C91 1.525(5) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.527(5) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C95 1.468(4) . ? C93 H93A 0.9500 . ? C94 C95 1.3900 . ? C94 C99 1.3900 . ? C95 C96 1.3900 . ? C96 C97 1.3900 . ? C96 H96A 0.9500 . ? C97 C98 1.3900 . ? C97 C117 1.557(3) . ? C98 C99 1.3900 . ? C98 H98A 0.9500 . ? C99 C100 1.467(4) . ? C100 H10C 0.9500 . ? C101 C102 1.526(5) . ? C101 H10D 0.9900 . ? C101 H10E 0.9900 . ? C102 C103 1.525(5) . ? C102 H10F 0.9900 . ? C102 H10G 0.9900 . ? C103 H10H 0.9900 . ? C103 H10I 0.9900 . ? C104 H10J 0.9500 . ? C105 C106 1.562(3) . ? C105 C10B 1.562(3) . ? C105 C107 1.562(3) . ? C105 C10A 1.562(3) . ? C105 C10C 1.562(3) . ? C105 C108 1.562(3) . ? C106 H10K 0.9800 . ? C106 H10L 0.9800 . ? C106 H10M 0.9800 . ? C107 H10N 0.9800 . ? C107 H10O 0.9800 . ? C107 H10P 0.9800 . ? C108 H10Q 0.9800 . ? C108 H10R 0.9800 . ? C108 H10S 0.9800 . ? C10A H10T 0.9800 . ? C10A H10U 0.9800 . ? C10A H10V 0.9800 . ? C10B H10W 0.9800 . ? C10B H10X 0.9800 . ? C10B H10Y 0.9800 . ? C10C H10Z 0.9800 . ? C10C H11B 0.9800 . ? C10C H11C 0.9800 . ? C109 C112 1.564(3) . ? C109 C111 1.565(3) . ? C109 C110 1.565(3) . ? C110 H11D 0.9800 . ? C110 H11E 0.9800 . ? C110 H11F 0.9800 . ? C111 H11G 0.9800 . ? C111 H11H 0.9800 . ? C111 H11I 0.9800 . ? C112 H11J 0.9800 . ? C112 H11K 0.9800 . ? C112 H11L 0.9800 . ? C113 C115 1.568(3) . ? C113 C116 1.569(3) . ? C113 C114 1.569(3) . ? C114 H11M 0.9800 . ? C114 H11N 0.9800 . ? C114 H11O 0.9800 . ? C115 H11P 0.9800 . ? C115 H11Q 0.9800 . ? C115 H11R 0.9800 . ? C116 H11S 0.9800 . ? C116 H11T 0.9800 . ? C116 H11U 0.9800 . ? C117 C118 1.558(3) . ? C117 C119 1.558(3) . ? C117 C120 1.558(3) . ? C118 H11V 0.9800 . ? C118 H11W 0.9800 . ? C118 H11X 0.9800 . ? C119 H11Y 0.9800 . ? C119 H11Z 0.9800 . ? C119 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C120 H12D 0.9800 . ? N21 O21B 1.241(3) . ? N21 O21A 1.242(3) . ? N21 O21C 1.242(3) . ? N22 O22B 1.241(3) . ? N22 O22C 1.241(3) . ? N22 O22A 1.241(3) . ? N23 O23C 1.242(3) . ? N23 O23A 1.242(3) . ? N23 O23B 1.242(3) . ? N24 O24C 1.241(3) . ? N24 O24B 1.241(3) . ? N24 O24A 1.242(3) . ? N1S C1S 1.227(8) . ? C1S C2S 1.382(9) . ? C2S H2S1 0.9799 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9801 . ? N2S C3S 1.227(8) . ? C3S C4S 1.382(9) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9799 . ? C4S H4S3 0.9801 . ? N3S C5S 1.227(8) . ? C5S C6S 1.381(9) . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9799 . ? N4S C7S 1.227(8) . ? C7S C8S 1.382(9) . ? C8S H8S1 0.9801 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9801 . ? N5S C9S 1.227(8) . ? C9S C10S 1.382(9) . ? C10S H100 0.9799 . ? C10S H101 0.9801 . ? C10S H102 0.9800 . ? N6S C11S 1.227(8) . ? C11S C12S 1.382(9) . ? C12S H12E 0.9798 . ? C12S H12F 0.9798 . ? C12S H12G 0.9800 . ? N7S C13S 1.228(8) . ? C13S C14S 1.382(9) . ? C13S H14E 1.0107 . ? C13S H14F 0.9299 . ? C13S H14G 1.0003 . ? C14S H14B 0.9801 . ? C14S H14C 0.9801 . ? C14S H14D 0.9800 . ? N8S C15S 1.227(8) . ? C15S C16S 1.381(9) . ? C16S H16B 0.9803 . ? C16S H16C 0.9801 . ? C16S H16D 0.9797 . ? N9S C17S 1.228(8) . ? C17S C18S 1.382(9) . ? C18S H18B 0.9800 . ? C18S H18C 0.9799 . ? C18S H18D 0.9800 . ? N10S C19S 1.228(8) . ? C19S C20S 1.382(9) . ? C20S H20C 0.9801 . ? C20S H20D 0.9799 . ? C20S H20E 0.9799 . ? 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 O9A Zn1 N1 86.2(6) . . ? O9A Zn1 N2 97.0(6) . . ? N1 Zn1 N2 95.9(5) . . ? O9A Zn1 S1 135.3(5) . . ? N1 Zn1 S1 100.2(3) . . ? N2 Zn1 S1 125.7(3) . . ? O9A Zn1 O9B 57.0(4) . . ? N1 Zn1 O9B 142.3(5) . . ? N2 Zn1 O9B 96.9(7) . . ? S1 Zn1 O9B 100.7(5) . . ? N4 Zn2 N3 102.3(5) . . ? N4 Zn2 O10A 106.6(5) . . ? N3 Zn2 O10A 121.8(5) . . ? N4 Zn2 S2 119.5(4) . . ? N3 Zn2 S2 94.0(4) . . ? O10A Zn2 S2 112.9(3) . . ? N5 Zn3 O11A 115.6(5) . . ? N5 Zn3 N6 100.4(5) . . ? O11A Zn3 N6 94.4(5) . . ? N5 Zn3 S3 100.1(4) . . ? O11A Zn3 S3 122.5(4) . . ? N6 Zn3 S3 122.7(3) . . ? N8 Zn4 N7 93.7(5) . . ? N8 Zn4 O12A 101.1(6) . . ? N7 Zn4 O12A 129.1(5) . . ? N8 Zn4 S4 120.5(4) . . ? N7 Zn4 S4 96.4(3) . . ? O12A Zn4 S4 116.0(4) . . ? C1 S1 Zn1 108.2(4) . . ? C12 S2 Zn2 106.6(4) . . ? C23 S3 Zn3 106.8(4) . . ? C34 S4 Zn4 107.4(4) . . ? C7 N1 C8 125.0(12) . . ? C7 N1 Zn1 121.8(10) . . ? C8 N1 Zn1 112.7(10) . . ? C11 N2 C10 107.9(10) . . ? C11 N2 Zn1 133.1(9) . . ? C10 N2 Zn1 118.4(9) . . ? C18 N3 C19 106.5(10) . . ? C18 N3 Zn2 138.2(9) . . ? C19 N3 Zn2 114.4(10) . . ? C22 N4 C21 109.7(10) . . ? C22 N4 Zn2 135.1(9) . . ? C21 N4 Zn2 114.3(9) . . ? C29 N5 C30 125.3(11) . . ? C29 N5 Zn3 122.6(11) . . ? C30 N5 Zn3 111.6(9) . . ? C33 N6 C32 110.5(10) . . ? C33 N6 Zn3 134.8(9) . . ? C32 N6 Zn3 114.6(9) . . ? C40 N7 C41 122.0(11) . . ? C40 N7 Zn4 123.0(10) . . ? C41 N7 Zn4 115.1(9) . . ? C44 N8 C43 112.0(10) . . ? C44 N8 Zn4 127.4(9) . . ? C43 N8 Zn4 118.0(9) . . ? C2 C1 C6 120.0 . . ? C2 C1 S1 115.9(6) . . ? C6 C1 S1 124.1(6) . . ? C1 C2 C3 120.0 . . ? C1 C2 C44 117.1(9) . . ? C3 C2 C44 122.9(9) . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 C45 118.0(8) . . ? C5 C4 C45 121.9(8) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 114.1(9) . . ? C1 C6 C7 125.8(9) . . ? N1 C7 C6 134.4(12) . . ? N1 C7 H7A 112.8 . . ? C6 C7 H7A 112.8 . . ? N1 C8 C9 122.5(14) . . ? N1 C8 H8A 106.7 . . ? C9 C8 H8A 106.7 . . ? N1 C8 H8B 106.7 . . ? C9 C8 H8B 106.7 . . ? H8A C8 H8B 106.6 . . ? C10 C9 C8 116.0(15) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N2 C10 C9 109.4(12) . . ? N2 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? N2 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C13 112.3(10) . . ? N2 C11 H11A 123.8 . . ? C13 C11 H11A 123.8 . . ? C13 C12 C17 120.0 . . ? C13 C12 S2 114.8(6) . . ? C17 C12 S2 124.9(6) . . ? C14 C13 C12 120.0 . . ? C14 C13 C11 127.1(9) . . ? C12 C13 C11 112.9(9) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 C49 118.0(8) . . ? C14 C15 C49 121.9(8) . . ? C15 C16 C17 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C12 120.0 . . ? C16 C17 C18 111.5(8) . . ? C12 C17 C18 128.5(8) . . ? N3 C18 C17 119.2(11) . . ? N3 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? N3 C19 C20 108.6(11) . . ? N3 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? N3 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C19 C20 C21 115.8(13) . . ? C19 C20 H20A 108.3 . . ? C21 C20 H20A 108.3 . . ? C19 C20 H20B 108.3 . . ? C21 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? N4 C21 C20 110.7(12) . . ? N4 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? N4 C22 C24 112.4(10) . . ? N4 C22 H22A 123.8 . . ? C24 C22 H22A 123.8 . . ? C24 C23 C28 120.0 . . ? C24 C23 S3 115.9(6) . . ? C28 C23 S3 123.7(6) . . ? C23 C24 C25 120.0 . . ? C23 C24 C22 120.1(9) . . ? C25 C24 C22 119.9(9) . . ? C26 C25 C24 120.0 . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 C53 114.7(8) . . ? C27 C26 C53 125.3(8) . . ? C28 C27 C26 120.0 . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C23 120.0 . . ? C27 C28 C29 117.6(9) . . ? C23 C28 C29 122.4(9) . . ? N5 C29 C28 137.6(13) . . ? N5 C29 H29A 111.2 . . ? C28 C29 H29A 111.2 . . ? N5 C30 C31 118.9(13) . . ? N5 C30 H30A 107.6 . . ? C31 C30 H30A 107.6 . . ? N5 C30 H30B 107.6 . . ? C31 C30 H30B 107.6 . . ? H30A C30 H30B 107.0 . . ? C32 C31 C30 117.1(14) . . ? C32 C31 H31A 108.0 . . ? C30 C31 H31A 108.0 . . ? C32 C31 H31B 108.0 . . ? C30 C31 H31B 108.0 . . ? H31A C31 H31B 107.3 . . ? N6 C32 C31 104.9(12) . . ? N6 C32 H32A 110.8 . . ? C31 C32 H32A 110.8 . . ? N6 C32 H32B 110.8 . . ? C31 C32 H32B 110.8 . . ? H32A C32 H32B 108.8 . . ? N6 C33 C35 116.6(11) . . ? N6 C33 H33A 121.7 . . ? C35 C33 H33A 121.7 . . ? C35 C34 C39 120.0 . . ? C35 C34 S4 114.6(6) . . ? C39 C34 S4 125.3(6) . . ? C36 C35 C34 120.0 . . ? C36 C35 C33 117.7(9) . . ? C34 C35 C33 122.2(9) . . ? C37 C36 C35 120.0 . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 C57 120.8(7) . . ? C36 C37 C57 119.1(7) . . ? C37 C38 C39 120.0 . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C38 C39 C34 120.0 . . ? C38 C39 C40 116.5(9) . . ? C34 C39 C40 123.3(9) . . ? N7 C40 C39 136.3(12) . . ? N7 C40 H40A 111.8 . . ? C39 C40 H40A 111.8 . . ? N7 C41 C42 111.9(11) . . ? N7 C41 H41A 109.2 . . ? C42 C41 H41A 109.2 . . ? N7 C41 H41B 109.2 . . ? C42 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C41 C42 C43 111.9(13) . . ? C41 C42 H42A 109.2 . . ? C43 C42 H42A 109.2 . . ? C41 C42 H42B 109.2 . . ? C43 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? N8 C43 C42 108.7(11) . . ? N8 C43 H43A 109.9 . . ? C42 C43 H43A 109.9 . . ? N8 C43 H43B 109.9 . . ? C42 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? N8 C44 C2 115.4(10) . . ? N8 C44 H44A 122.3 . . ? C2 C44 H44A 122.3 . . ? C47 C45 C48 109.22(19) . . ? C47 C45 C46 109.18(19) . . ? C48 C45 C46 109.10(19) . . ? C47 C45 C4 105.5(9) . . ? C48 C45 C4 114.5(9) . . ? C46 C45 C4 109.3(9) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C52 108.81(19) . . ? C51 C49 C50 108.76(19) . . ? C52 C49 C50 108.85(19) . . ? C51 C49 C15 108.8(10) . . ? C52 C49 C15 108.1(9) . . ? C50 C49 C15 113.4(10) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C56 C53 C26 99.6(9) . . ? C56 C53 C54 109.49(19) . . ? C26 C53 C54 120.2(8) . . ? C56 C53 C55 109.53(19) . . ? C26 C53 C55 108.0(8) . . ? C54 C53 C55 109.42(19) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C37 C57 C58 99.7(9) . . ? C37 C57 C60 115.6(10) . . ? C58 C57 C60 109.6(2) . . ? C37 C57 C59 112.4(9) . . ? C58 C57 C59 109.5(2) . . ? C60 C57 C59 109.5(2) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O9B N9 O9C 120.1(16) . . ? O9B N9 O9A 119.0(17) . . ? O9C N9 O9A 119.6(17) . . ? N9 O9A Zn1 100.5(11) . . ? N9 O9B Zn1 83.1(12) . . ? O10B N10 O10A 110.6(12) . . ? O10B N10 O10C 123.3(13) . . ? O10A N10 O10C 126.0(13) . . ? N10 O10A Zn2 123.2(9) . . ? O11C N11 O11B 111.5(12) . . ? O11C N11 O11A 122.4(13) . . ? O11B N11 O11A 126.0(13) . . ? N11 O11A Zn3 111.1(10) . . ? O12B N12 O12C 131.3(17) . . ? O12B N12 O12A 102.9(15) . . ? O12C N12 O12A 125.6(17) . . ? N12 O12A Zn4 120.5(11) . . ? O21A Zn5 N14 111.0(5) . . ? O21A Zn5 N13 124.0(5) . . ? N14 Zn5 N13 93.3(4) . . ? O21A Zn5 S5 102.7(4) . . ? N14 Zn5 S5 124.9(3) . . ? N13 Zn5 S5 102.6(3) . . ? N16 Zn6 N15 93.0(5) . . ? N16 Zn6 S6 126.7(3) . . ? N15 Zn6 S6 103.6(3) . . ? N16 Zn6 O22A 103.8(6) . . ? N15 Zn6 O22A 83.7(5) . . ? S6 Zn6 O22A 127.9(5) . . ? N16 Zn6 O22B 105.0(6) . . ? N15 Zn6 O22B 139.5(5) . . ? S6 Zn6 O22B 94.3(4) . . ? O22A Zn6 O22B 57.1(4) . . ? N18 Zn7 O23A 90.5(5) . . ? N18 Zn7 N17 102.3(4) . . ? O23A Zn7 N17 119.3(5) . . ? N18 Zn7 S7 120.9(3) . . ? O23A Zn7 S7 124.5(3) . . ? N17 Zn7 S7 98.7(3) . . ? N19 Zn8 O24A 128.9(5) . . ? N19 Zn8 N20 96.0(5) . . ? O24A Zn8 N20 108.5(5) . . ? N19 Zn8 S8 106.1(3) . . ? O24A Zn8 S8 105.2(4) . . ? N20 Zn8 S8 111.6(3) . . ? C61 S5 Zn5 99.8(4) . . ? C72 S6 Zn6 100.7(3) . . ? C83 S7 Zn7 105.1(3) . . ? C94 S8 Zn8 94.7(3) . . ? C67 N13 C68 133.1(11) . . ? C67 N13 Zn5 111.8(10) . . ? C68 N13 Zn5 115.1(8) . . ? C71 N14 C70 125.5(10) . . ? C71 N14 Zn5 113.2(9) . . ? C70 N14 Zn5 120.7(8) . . ? C78 N15 C79 109.7(10) . . ? C78 N15 Zn6 128.8(9) . . ? C79 N15 Zn6 121.4(9) . . ? C82 N16 C81 114.4(10) . . ? C82 N16 Zn6 130.1(8) . . ? C81 N16 Zn6 115.1(8) . . ? C89 N17 C90 109.2(10) . . ? C89 N17 Zn7 134.4(9) . . ? C90 N17 Zn7 116.2(9) . . ? C93 N18 C92 123.6(10) . . ? C93 N18 Zn7 127.7(9) . . ? C92 N18 Zn7 108.0(8) . . ? C100 N19 C101 118.3(10) . . ? C100 N19 Zn8 120.6(9) . . ? C101 N19 Zn8 120.9(9) . . ? C104 N20 C103 127.6(11) . . ? C104 N20 Zn8 122.1(9) . . ? C103 N20 Zn8 109.6(9) . . ? C62 C61 C66 120.0 . . ? C62 C61 S5 112.1(6) . . ? C66 C61 S5 125.4(6) . . ? C61 C62 C63 120.0 . . ? C61 C62 C104 125.7(9) . . ? C63 C62 C104 114.3(9) . . ? C64 C63 C62 120.0 . . ? C64 C63 H63A 120.0 . . ? C62 C63 H63A 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 C105 119.2(8) . . ? C65 C64 C105 120.8(8) . . ? C66 C65 C64 120.0 . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 C67 116.4(8) . . ? C61 C66 C67 123.5(9) . . ? N13 C67 C66 143.8(14) . . ? N13 C67 H67A 108.1 . . ? C66 C67 H67A 108.1 . . ? N13 C68 C69 117.3(12) . . ? N13 C68 H68A 108.0 . . ? C69 C68 H68A 108.0 . . ? N13 C68 H68B 108.0 . . ? C69 C68 H68B 108.0 . . ? H68A C68 H68B 107.2 . . ? C68 C69 C70 112.2(12) . . ? C68 C69 H69A 109.2 . . ? C70 C69 H69A 109.2 . . ? C68 C69 H69B 109.2 . . ? C70 C69 H69B 109.2 . . ? H69A C69 H69B 107.9 . . ? N14 C70 C69 113.7(11) . . ? N14 C70 H70A 108.8 . . ? C69 C70 H70A 108.8 . . ? N14 C70 H70B 108.8 . . ? C69 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? N14 C71 C73 129.5(11) . . ? N14 C71 H71A 115.3 . . ? C73 C71 H71A 115.3 . . ? C73 C72 C77 120.0 . . ? C73 C72 S6 110.8(6) . . ? C77 C72 S6 128.6(6) . . ? C72 C73 C74 120.0 . . ? C72 C73 C71 119.0(8) . . ? C74 C73 C71 120.9(8) . . ? C75 C74 C73 120.0 . . ? C75 C74 H74A 120.0 . . ? C73 C74 H74A 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 C109 127.8(7) . . ? C76 C75 C109 112.0(7) . . ? C77 C76 C75 120.0 . . ? C77 C76 H76A 120.0 . . ? C75 C76 H76A 120.0 . . ? C76 C77 C72 120.0 . . ? C76 C77 C78 105.6(8) . . ? C72 C77 C78 134.3(8) . . ? N15 C78 C77 119.3(10) . . ? N15 C78 H78A 120.4 . . ? C77 C78 H78A 120.4 . . ? N15 C79 C80 112.3(11) . . ? N15 C79 H79A 109.1 . . ? C80 C79 H79A 109.1 . . ? N15 C79 H79B 109.1 . . ? C80 C79 H79B 109.1 . . ? H79A C79 H79B 107.9 . . ? C81 C80 C79 115.6(13) . . ? C81 C80 H80A 108.4 . . ? C79 C80 H80A 108.4 . . ? C81 C80 H80B 108.4 . . ? C79 C80 H80B 108.4 . . ? H80A C80 H80B 107.4 . . ? N16 C81 C80 117.3(11) . . ? N16 C81 H81A 108.0 . . ? C80 C81 H81A 108.0 . . ? N16 C81 H81B 108.0 . . ? C80 C81 H81B 108.0 . . ? H81A C81 H81B 107.2 . . ? N16 C82 C84 118.7(10) . . ? N16 C82 H82A 120.7 . . ? C84 C82 H82A 120.7 . . ? C84 C83 C88 120.0 . . ? C84 C83 S7 113.2(6) . . ? C88 C83 S7 126.4(6) . . ? C85 C84 C83 120.0 . . ? C85 C84 C82 124.7(8) . . ? C83 C84 C82 114.8(8) . . ? C84 C85 C86 120.0 . . ? C84 C85 H85A 120.0 . . ? C86 C85 H85A 120.0 . . ? C87 C86 C85 120.0 . . ? C87 C86 C113 117.0(8) . . ? C85 C86 C113 122.8(8) . . ? C88 C87 C86 120.0 . . ? C88 C87 H87A 120.0 . . ? C86 C87 H87A 120.0 . . ? C87 C88 C83 120.0 . . ? C87 C88 C89 105.0(8) . . ? C83 C88 C89 134.9(8) . . ? N17 C89 C88 117.7(10) . . ? N17 C89 H89A 121.2 . . ? C88 C89 H89A 121.2 . . ? N17 C90 C91 102.9(11) . . ? N17 C90 H90A 111.2 . . ? C91 C90 H90A 111.2 . . ? N17 C90 H90B 111.2 . . ? C91 C90 H90B 111.2 . . ? H90A C90 H90B 109.1 . . ? C90 C91 C92 121.4(14) . . ? C90 C91 H91A 107.0 . . ? C92 C91 H91A 107.0 . . ? C90 C91 H91B 107.0 . . ? C92 C91 H91B 107.0 . . ? H91A C91 H91B 106.7 . . ? N18 C92 C91 117.4(12) . . ? N18 C92 H92A 108.0 . . ? C91 C92 H92A 108.0 . . ? N18 C92 H92B 108.0 . . ? C91 C92 H92B 108.0 . . ? H92A C92 H92B 107.2 . . ? N18 C93 C95 132.5(11) . . ? N18 C93 H93A 113.8 . . ? C95 C93 H93A 113.8 . . ? C95 C94 C99 120.0 . . ? C95 C94 S8 108.7(6) . . ? C99 C94 S8 129.0(6) . . ? C96 C95 C94 120.0 . . ? C96 C95 C93 115.2(8) . . ? C94 C95 C93 124.7(8) . . ? C95 C96 C97 120.0 . . ? C95 C96 H96A 120.0 . . ? C97 C96 H96A 120.0 . . ? C98 C97 C96 120.0 . . ? C98 C97 C117 114.6(8) . . ? C96 C97 C117 125.4(8) . . ? C99 C98 C97 120.0 . . ? C99 C98 H98A 120.0 . . ? C97 C98 H98A 120.0 . . ? C98 C99 C94 120.0 . . ? C98 C99 C100 113.5(8) . . ? C94 C99 C100 126.5(8) . . ? N19 C100 C99 130.8(11) . . ? N19 C100 H10C 114.6 . . ? C99 C100 H10C 114.6 . . ? N19 C101 C102 108.2(11) . . ? N19 C101 H10D 110.1 . . ? C102 C101 H10D 110.1 . . ? N19 C101 H10E 110.1 . . ? C102 C101 H10E 110.1 . . ? H10D C101 H10E 108.4 . . ? C103 C102 C101 115.8(12) . . ? C103 C102 H10F 108.3 . . ? C101 C102 H10F 108.3 . . ? C103 C102 H10G 108.3 . . ? C101 C102 H10G 108.3 . . ? H10F C102 H10G 107.4 . . ? N20 C103 C102 113.7(11) . . ? N20 C103 H10H 108.8 . . ? C102 C103 H10H 108.8 . . ? N20 C103 H10I 108.8 . . ? C102 C103 H10I 108.8 . . ? H10H C103 H10I 107.7 . . ? N20 C104 C62 139.1(13) . . ? N20 C104 H10J 110.4 . . ? C62 C104 H10J 110.4 . . ? C64 C105 C106 103.4(14) . . ? C64 C105 C10B 104.5(15) . . ? C106 C105 C10B 62.9(11) . . ? C64 C105 C107 110.1(14) . . ? C106 C105 C107 109.6(2) . . ? C10B C105 C107 49.8(12) . . ? C64 C105 C10A 114.0(14) . . ? C106 C105 C10A 52.5(11) . . ? C10B C105 C10A 109.6(2) . . ? C107 C105 C10A 135.1(16) . . ? C64 C105 C10C 109.3(15) . . ? C106 C105 C10C 147.2(17) . . ? C10B C105 C10C 109.6(2) . . ? C107 C105 C10C 61.0(12) . . ? C10A C105 C10C 109.6(2) . . ? C64 C105 C108 114.3(13) . . ? C106 C105 C108 109.6(2) . . ? C10B C105 C108 141.0(16) . . ? C107 C105 C108 109.6(2) . . ? C10A C105 C108 58.3(12) . . ? C10C C105 C108 54.2(11) . . ? C105 C106 H10K 109.5 . . ? C105 C106 H10L 109.5 . . ? H10K C106 H10L 109.5 . . ? C105 C106 H10M 109.5 . . ? H10K C106 H10M 109.5 . . ? H10L C106 H10M 109.5 . . ? C105 C107 H10N 109.5 . . ? C105 C107 H10O 109.5 . . ? H10N C107 H10O 109.5 . . ? C105 C107 H10P 109.5 . . ? H10N C107 H10P 109.5 . . ? H10O C107 H10P 109.5 . . ? C105 C108 H10Q 109.5 . . ? C105 C108 H10R 109.5 . . ? H10Q C108 H10R 109.5 . . ? C105 C108 H10S 109.5 . . ? H10Q C108 H10S 109.5 . . ? H10R C108 H10S 109.5 . . ? C105 C10A H10T 109.5 . . ? C105 C10A H10U 109.5 . . ? H10T C10A H10U 109.5 . . ? C105 C10A H10V 109.5 . . ? H10T C10A H10V 109.5 . . ? H10U C10A H10V 109.5 . . ? C105 C10B H10W 109.5 . . ? C105 C10B H10X 109.5 . . ? H10W C10B H10X 109.5 . . ? C105 C10B H10Y 109.5 . . ? H10W C10B H10Y 109.5 . . ? H10X C10B H10Y 109.5 . . ? C105 C10C H10Z 109.5 . . ? C105 C10C H11B 109.5 . . ? H10Z C10C H11B 109.5 . . ? C105 C10C H11C 109.5 . . ? H10Z C10C H11C 109.5 . . ? H11B C10C H11C 109.5 . . ? C112 C109 C111 109.34(19) . . ? C112 C109 C110 109.23(19) . . ? C111 C109 C110 109.18(19) . . ? C112 C109 C75 102.8(9) . . ? C111 C109 C75 109.4(8) . . ? C110 C109 C75 116.6(8) . . ? C109 C110 H11D 109.5 . . ? C109 C110 H11E 109.5 . . ? H11D C110 H11E 109.5 . . ? C109 C110 H11F 109.5 . . ? H11D C110 H11F 109.5 . . ? H11E C110 H11F 109.5 . . ? C109 C111 H11G 109.5 . . ? C109 C111 H11H 109.5 . . ? H11G C111 H11H 109.5 . . ? C109 C111 H11I 109.5 . . ? H11G C111 H11I 109.5 . . ? H11H C111 H11I 109.5 . . ? C109 C112 H11J 109.5 . . ? C109 C112 H11K 109.5 . . ? H11J C112 H11K 109.5 . . ? C109 C112 H11L 109.5 . . ? H11J C112 H11L 109.5 . . ? H11K C112 H11L 109.5 . . ? C115 C113 C116 108.7(2) . . ? C115 C113 C114 108.71(19) . . ? C116 C113 C114 108.69(19) . . ? C115 C113 C86 107.9(12) . . ? C116 C113 C86 108.9(11) . . ? C114 C113 C86 113.9(11) . . ? C113 C114 H11M 109.5 . . ? C113 C114 H11N 109.5 . . ? H11M C114 H11N 109.5 . . ? C113 C114 H11O 109.5 . . ? H11M C114 H11O 109.5 . . ? H11N C114 H11O 109.5 . . ? C113 C115 H11P 109.5 . . ? C113 C115 H11Q 109.5 . . ? H11P C115 H11Q 109.5 . . ? C113 C115 H11R 109.5 . . ? H11P C115 H11R 109.5 . . ? H11Q C115 H11R 109.5 . . ? C113 C116 H11S 109.5 . . ? C113 C116 H11T 109.5 . . ? H11S C116 H11T 109.5 . . ? C113 C116 H11U 109.5 . . ? H11S C116 H11U 109.5 . . ? H11T C116 H11U 109.5 . . ? C97 C117 C118 108.9(9) . . ? C97 C117 C119 113.0(10) . . ? C118 C117 C119 110.3(2) . . ? C97 C117 C120 103.9(10) . . ? C118 C117 C120 110.2(2) . . ? C119 C117 C120 110.3(2) . . ? C117 C118 H11V 109.5 . . ? C117 C118 H11W 109.5 . . ? H11V C118 H11W 109.5 . . ? C117 C118 H11X 109.5 . . ? H11V C118 H11X 109.5 . . ? H11W C118 H11X 109.5 . . ? C117 C119 H11Y 109.5 . . ? C117 C119 H11Z 109.5 . . ? H11Y C119 H11Z 109.5 . . ? C117 C119 H12A 109.5 . . ? H11Y C119 H12A 109.5 . . ? H11Z C119 H12A 109.5 . . ? C117 C120 H12B 109.5 . . ? C117 C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C117 C120 H12D 109.5 . . ? H12B C120 H12D 109.5 . . ? H12C C120 H12D 109.5 . . ? O21B N21 O21A 115.4(13) . . ? O21B N21 O21C 116.9(14) . . ? O21A N21 O21C 127.4(14) . . ? N21 O21A Zn5 106.9(10) . . ? O22B N22 O22C 113.4(15) . . ? O22B N22 O22A 119.9(17) . . ? O22C N22 O22A 125.4(17) . . ? N22 O22A Zn6 91.3(11) . . ? N22 O22B Zn6 91.2(12) . . ? O23C N23 O23A 111.6(11) . . ? O23C N23 O23B 127.3(13) . . ? O23A N23 O23B 121.0(12) . . ? N23 O23A Zn7 106.9(9) . . ? O24C N24 O24B 108.4(12) . . ? O24C N24 O24A 130.6(14) . . ? O24B N24 O24A 121.1(14) . . ? N24 O24A Zn8 106.7(10) . . ? N1S C1S C2S 177(2) . . ? C1S C2S H2S1 108.1 . . ? C1S C2S H2S2 110.6 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.7 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 178(2) . . ? C3S C4S H4S1 109.8 . . ? C3S C4S H4S2 108.7 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.9 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N3S C5S C6S 179(2) . . ? C5S C6S H6S1 107.2 . . ? C5S C6S H6S2 110.2 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 111.0 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? N4S C7S C8S 178(3) . . ? C7S C8S H8S1 111.3 . . ? C7S C8S H8S2 107.8 . . ? H8S1 C8S H8S2 109.5 . . ? C7S C8S H8S3 109.2 . . ? H8S1 C8S H8S3 109.4 . . ? H8S2 C8S H8S3 109.5 . . ? N5S C9S C10S 177(2) . . ? C9S C10S H100 108.6 . . ? C9S C10S H101 109.9 . . ? H100 C10S H101 109.5 . . ? C9S C10S H102 109.9 . . ? H100 C10S H102 109.5 . . ? H101 C10S H102 109.5 . . ? N6S C11S C12S 176(2) . . ? C11S C12S H12E 110.4 . . ? C11S C12S H12F 108.7 . . ? H12E C12S H12F 109.5 . . ? C11S C12S H12G 109.3 . . ? H12E C12S H12G 109.5 . . ? H12F C12S H12G 109.5 . . ? N7S C13S C14S 174(2) . . ? C14S C13S H14G 109.6 . . ? H14E C13S H14G 105.4 . . ? H14F C13S H14G 111.9 . . ? C13S C14S H14B 108.0 . . ? C13S C14S H14C 110.2 . . ? H14B C14S H14C 109.5 . . ? C13S C14S H14D 110.1 . . ? H14B C14S H14D 109.5 . . ? H14C C14S H14D 109.5 . . ? N8S C15S C16S 180(3) . . ? C15S C16S H16B 107.6 . . ? C15S C16S H16C 110.4 . . ? H16B C16S H16C 109.4 . . ? C15S C16S H16D 110.4 . . ? H16B C16S H16D 109.5 . . ? H16C C16S H16D 109.5 . . ? N9S C17S C18S 172.6(19) . . ? C17S C18S H18B 108.7 . . ? C17S C18S H18C 110.3 . . ? H18B C18S H18C 109.5 . . ? C17S C18S H18D 109.4 . . ? H18B C18S H18D 109.5 . . ? H18C C18S H18D 109.5 . . ? N10S C19S C20S 173(3) . . ? C19S C20S H20C 108.6 . . ? C19S C20S H20D 112.1 . . ? H20C C20S H20D 109.5 . . ? C19S C20S H20E 107.7 . . ? H20C C20S H20E 109.5 . . ? H20D C20S H20E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9A Zn1 S1 C1 -73.7(8) . . . . ? N1 Zn1 S1 C1 21.3(6) . . . . ? N2 Zn1 S1 C1 126.2(6) . . . . ? O9B Zn1 S1 C1 -127.1(6) . . . . ? N4 Zn2 S2 C12 -130.8(6) . . . . ? N3 Zn2 S2 C12 -24.3(6) . . . . ? O10A Zn2 S2 C12 102.7(6) . . . . ? N5 Zn3 S3 C23 24.5(6) . . . . ? O11A Zn3 S3 C23 -105.0(5) . . . . ? N6 Zn3 S3 C23 133.9(5) . . . . ? N8 Zn4 S4 C34 -124.4(6) . . . . ? N7 Zn4 S4 C34 -26.4(5) . . . . ? O12A Zn4 S4 C34 113.1(6) . . . . ? O9A Zn1 N1 C7 121.7(14) . . . . ? N2 Zn1 N1 C7 -141.6(13) . . . . ? S1 Zn1 N1 C7 -13.7(13) . . . . ? O9B Zn1 N1 C7 109.1(15) . . . . ? O9A Zn1 N1 C8 -65.4(11) . . . . ? N2 Zn1 N1 C8 31.2(11) . . . . ? S1 Zn1 N1 C8 159.2(10) . . . . ? O9B Zn1 N1 C8 -78.0(15) . . . . ? O9A Zn1 N2 C11 -142.2(15) . . . . ? N1 Zn1 N2 C11 130.9(15) . . . . ? S1 Zn1 N2 C11 23.8(16) . . . . ? O9B Zn1 N2 C11 -84.7(15) . . . . ? O9A Zn1 N2 C10 47.9(11) . . . . ? N1 Zn1 N2 C10 -39.0(10) . . . . ? S1 Zn1 N2 C10 -146.1(9) . . . . ? O9B Zn1 N2 C10 105.4(10) . . . . ? N4 Zn2 N3 C18 131.4(17) . . . . ? O10A Zn2 N3 C18 -110.0(17) . . . . ? S2 Zn2 N3 C18 10.1(17) . . . . ? N4 Zn2 N3 C19 -35.6(11) . . . . ? O10A Zn2 N3 C19 83.0(11) . . . . ? S2 Zn2 N3 C19 -156.9(10) . . . . ? N3 Zn2 N4 C22 -132.8(17) . . . . ? O10A Zn2 N4 C22 98.4(17) . . . . ? S2 Zn2 N4 C22 -31.0(19) . . . . ? N3 Zn2 N4 C21 35.0(11) . . . . ? O10A Zn2 N4 C21 -93.8(11) . . . . ? S2 Zn2 N4 C21 136.9(9) . . . . ? O11A Zn3 N5 C29 119.6(14) . . . . ? N6 Zn3 N5 C29 -140.4(14) . . . . ? S3 Zn3 N5 C29 -14.2(15) . . . . ? O11A Zn3 N5 C30 -67.3(12) . . . . ? N6 Zn3 N5 C30 32.7(11) . . . . ? S3 Zn3 N5 C30 158.9(10) . . . . ? N5 Zn3 N6 C33 133.3(15) . . . . ? O11A Zn3 N6 C33 -109.6(15) . . . . ? S3 Zn3 N6 C33 24.1(17) . . . . ? N5 Zn3 N6 C32 -41.4(10) . . . . ? O11A Zn3 N6 C32 75.7(10) . . . . ? S3 Zn3 N6 C32 -150.7(8) . . . . ? N8 Zn4 N7 C40 140.2(13) . . . . ? O12A Zn4 N7 C40 -112.3(13) . . . . ? S4 Zn4 N7 C40 19.0(13) . . . . ? N8 Zn4 N7 C41 -40.3(10) . . . . ? O12A Zn4 N7 C41 67.2(12) . . . . ? S4 Zn4 N7 C41 -161.5(9) . . . . ? N7 Zn4 N8 C44 -116.5(14) . . . . ? O12A Zn4 N8 C44 112.5(14) . . . . ? S4 Zn4 N8 C44 -16.9(15) . . . . ? N7 Zn4 N8 C43 43.8(11) . . . . ? O12A Zn4 N8 C43 -87.2(11) . . . . ? S4 Zn4 N8 C43 143.4(9) . . . . ? Zn1 S1 C1 C2 163.9(4) . . . . ? Zn1 S1 C1 C6 -16.9(7) . . . . ? C6 C1 C2 C3 0.0 . . . . ? S1 C1 C2 C3 179.2(8) . . . . ? C6 C1 C2 C44 178.6(10) . . . . ? S1 C1 C2 C44 -2.2(10) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C44 C2 C3 C4 -178.5(11) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C2 C3 C4 C45 176.9(9) . . . . ? C3 C4 C5 C6 0.0 . . . . ? C45 C4 C5 C6 -176.7(10) . . . . ? C4 C5 C6 C1 0.0 . . . . ? C4 C5 C6 C7 -176.5(10) . . . . ? C2 C1 C6 C5 0.0 . . . . ? S1 C1 C6 C5 -179.2(8) . . . . ? C2 C1 C6 C7 176.1(11) . . . . ? S1 C1 C6 C7 -3.1(11) . . . . ? C8 N1 C7 C6 -178.7(15) . . . . ? Zn1 N1 C7 C6 -7(3) . . . . ? C5 C6 C7 N1 -164.1(16) . . . . ? C1 C6 C7 N1 20(2) . . . . ? C7 N1 C8 C9 122.9(19) . . . . ? Zn1 N1 C8 C9 -49.6(19) . . . . ? N1 C8 C9 C10 66(2) . . . . ? C11 N2 C10 C9 -117.1(15) . . . . ? Zn1 N2 C10 C9 55.2(15) . . . . ? C8 C9 C10 N2 -64.4(19) . . . . ? C10 N2 C11 C13 178.4(11) . . . . ? Zn1 N2 C11 C13 8(2) . . . . ? Zn2 S2 C12 C13 -157.8(5) . . . . ? Zn2 S2 C12 C17 27.9(7) . . . . ? C17 C12 C13 C14 0.0 . . . . ? S2 C12 C13 C14 -174.6(8) . . . . ? C17 C12 C13 C11 -178.5(10) . . . . ? S2 C12 C13 C11 6.9(9) . . . . ? N2 C11 C13 C14 49.1(17) . . . . ? N2 C11 C13 C12 -132.5(11) . . . . ? C12 C13 C14 C15 0.0 . . . . ? C11 C13 C14 C15 178.3(12) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C13 C14 C15 C49 176.4(11) . . . . ? C14 C15 C16 C17 0.0 . . . . ? C49 C15 C16 C17 -176.5(10) . . . . ? C15 C16 C17 C12 0.0 . . . . ? C15 C16 C17 C18 179.5(11) . . . . ? C13 C12 C17 C16 0.0 . . . . ? S2 C12 C17 C16 174.0(9) . . . . ? C13 C12 C17 C18 -179.4(13) . . . . ? S2 C12 C17 C18 -5.4(13) . . . . ? C19 N3 C18 C17 -179.7(12) . . . . ? Zn2 N3 C18 C17 13(3) . . . . ? C16 C17 C18 N3 162.1(12) . . . . ? C12 C17 C18 N3 -19(2) . . . . ? C18 N3 C19 C20 -118.9(15) . . . . ? Zn2 N3 C19 C20 52.2(16) . . . . ? N3 C19 C20 C21 -73.4(18) . . . . ? C22 N4 C21 C20 117.9(15) . . . . ? Zn2 N4 C21 C20 -53.0(15) . . . . ? C19 C20 C21 N4 74.3(17) . . . . ? C21 N4 C22 C24 -174.5(12) . . . . ? Zn2 N4 C22 C24 -6(2) . . . . ? Zn3 S3 C23 C24 163.2(5) . . . . ? Zn3 S3 C23 C28 -24.1(7) . . . . ? C28 C23 C24 C25 0.0 . . . . ? S3 C23 C24 C25 173.0(7) . . . . ? C28 C23 C24 C22 179.8(11) . . . . ? S3 C23 C24 C22 -7.2(10) . . . . ? N4 C22 C24 C23 124.9(12) . . . . ? N4 C22 C24 C25 -55.3(16) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C22 C24 C25 C26 -179.8(11) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C24 C25 C26 C53 -179.1(9) . . . . ? C25 C26 C27 C28 0.0 . . . . ? C53 C26 C27 C28 179.0(10) . . . . ? C26 C27 C28 C23 0.0 . . . . ? C26 C27 C28 C29 -178.8(12) . . . . ? C24 C23 C28 C27 0.0 . . . . ? S3 C23 C28 C27 -172.4(8) . . . . ? C24 C23 C28 C29 178.8(12) . . . . ? S3 C23 C28 C29 6.4(12) . . . . ? C30 N5 C29 C28 -178.7(17) . . . . ? Zn3 N5 C29 C28 -7(3) . . . . ? C27 C28 C29 N5 -166(2) . . . . ? C23 C28 C29 N5 15(3) . . . . ? C29 N5 C30 C31 123.1(19) . . . . ? Zn3 N5 C30 C31 -49.7(17) . . . . ? N5 C30 C31 C32 72(2) . . . . ? C33 N6 C32 C31 -119.5(14) . . . . ? Zn3 N6 C32 C31 56.5(14) . . . . ? C30 C31 C32 N6 -71.5(17) . . . . ? C32 N6 C33 C35 177.6(11) . . . . ? Zn3 N6 C33 C35 3(2) . . . . ? Zn4 S4 C34 C35 -161.8(4) . . . . ? Zn4 S4 C34 C39 20.7(7) . . . . ? C39 C34 C35 C36 0.0 . . . . ? S4 C34 C35 C36 -177.6(8) . . . . ? C39 C34 C35 C33 176.3(11) . . . . ? S4 C34 C35 C33 -1.3(10) . . . . ? N6 C33 C35 C36 45.3(16) . . . . ? N6 C33 C35 C34 -131.1(12) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C33 C35 C36 C37 -176.5(11) . . . . ? C35 C36 C37 C38 0.0 . . . . ? C35 C36 C37 C57 -177.3(9) . . . . ? C36 C37 C38 C39 0.0 . . . . ? C57 C37 C38 C39 177.3(9) . . . . ? C37 C38 C39 C34 0.0 . . . . ? C37 C38 C39 C40 174.7(11) . . . . ? C35 C34 C39 C38 0.0 . . . . ? S4 C34 C39 C38 177.4(8) . . . . ? C35 C34 C39 C40 -174.3(12) . . . . ? S4 C34 C39 C40 3.1(11) . . . . ? C41 N7 C40 C39 -174.7(15) . . . . ? Zn4 N7 C40 C39 5(3) . . . . ? C38 C39 C40 N7 163.6(17) . . . . ? C34 C39 C40 N7 -22(2) . . . . ? C40 N7 C41 C42 -122.8(16) . . . . ? Zn4 N7 C41 C42 57.7(15) . . . . ? N7 C41 C42 C43 -72.2(17) . . . . ? C44 N8 C43 C42 100.8(15) . . . . ? Zn4 N8 C43 C42 -62.4(14) . . . . ? C41 C42 C43 N8 72.3(16) . . . . ? C43 N8 C44 C2 -175.4(12) . . . . ? Zn4 N8 C44 C2 -14(2) . . . . ? C1 C2 C44 N8 133.6(12) . . . . ? C3 C2 C44 N8 -47.9(17) . . . . ? C3 C4 C45 C47 129.4(7) . . . . ? C5 C4 C45 C47 -53.8(9) . . . . ? C3 C4 C45 C48 9.3(10) . . . . ? C5 C4 C45 C48 -173.9(7) . . . . ? C3 C4 C45 C46 -113.4(7) . . . . ? C5 C4 C45 C46 63.4(9) . . . . ? C16 C15 C49 C51 -171.3(7) . . . . ? C14 C15 C49 C51 12.2(10) . . . . ? C16 C15 C49 C52 -53.2(9) . . . . ? C14 C15 C49 C52 130.3(8) . . . . ? C16 C15 C49 C50 67.5(9) . . . . ? C14 C15 C49 C50 -109.0(8) . . . . ? C25 C26 C53 C56 119.4(6) . . . . ? C27 C26 C53 C56 -59.7(8) . . . . ? C25 C26 C53 C54 0.1(10) . . . . ? C27 C26 C53 C54 -179.0(7) . . . . ? C25 C26 C53 C55 -126.3(7) . . . . ? C27 C26 C53 C55 54.6(9) . . . . ? C38 C37 C57 C58 -60.3(8) . . . . ? C36 C37 C57 C58 117.0(7) . . . . ? C38 C37 C57 C60 -177.6(7) . . . . ? C36 C37 C57 C60 -0.3(10) . . . . ? C38 C37 C57 C59 55.6(9) . . . . ? C36 C37 C57 C59 -127.1(7) . . . . ? O9B N9 O9A Zn1 -7(3) . . . . ? O9C N9 O9A Zn1 -173.6(17) . . . . ? N1 Zn1 O9A N9 -167.2(14) . . . . ? N2 Zn1 O9A N9 97.3(14) . . . . ? S1 Zn1 O9A N9 -66.5(16) . . . . ? O9B Zn1 O9A N9 3.6(14) . . . . ? O9C N9 O9B Zn1 172(2) . . . . ? O9A N9 O9B Zn1 6(2) . . . . ? O9A Zn1 O9B N9 -3.6(13) . . . . ? N1 Zn1 O9B N9 11(2) . . . . ? N2 Zn1 O9B N9 -97.5(14) . . . . ? S1 Zn1 O9B N9 134.1(14) . . . . ? O10B N10 O10A Zn2 1(2) . . . . ? O10C N10 O10A Zn2 178.4(14) . . . . ? N4 Zn2 O10A N10 57.0(14) . . . . ? N3 Zn2 O10A N10 -59.4(14) . . . . ? S2 Zn2 O10A N10 -169.9(12) . . . . ? O11C N11 O11A Zn3 -174.6(15) . . . . ? O11B N11 O11A Zn3 0(2) . . . . ? N5 Zn3 O11A N11 -56.3(13) . . . . ? N6 Zn3 O11A N11 -160.1(12) . . . . ? S3 Zn3 O11A N11 66.2(13) . . . . ? O12B N12 O12A Zn4 -8(3) . . . . ? O12C N12 O12A Zn4 177.2(15) . . . . ? N8 Zn4 O12A N12 95.2(15) . . . . ? N7 Zn4 O12A N12 -8.9(18) . . . . ? S4 Zn4 O12A N12 -132.6(14) . . . . ? O21A Zn5 S5 C61 97.9(5) . . . . ? N14 Zn5 S5 C61 -134.9(5) . . . . ? N13 Zn5 S5 C61 -31.8(5) . . . . ? N16 Zn6 S6 C72 122.9(5) . . . . ? N15 Zn6 S6 C72 18.6(5) . . . . ? O22A Zn6 S6 C72 -74.1(6) . . . . ? O22B Zn6 S6 C72 -124.8(6) . . . . ? N18 Zn7 S7 C83 -124.5(5) . . . . ? O23A Zn7 S7 C83 120.5(5) . . . . ? N17 Zn7 S7 C83 -14.5(5) . . . . ? N19 Zn8 S8 C94 31.6(6) . . . . ? O24A Zn8 S8 C94 -107.4(5) . . . . ? N20 Zn8 S8 C94 135.0(5) . . . . ? O21A Zn5 N13 C67 -99.2(12) . . . . ? N14 Zn5 N13 C67 142.7(11) . . . . ? S5 Zn5 N13 C67 15.8(12) . . . . ? O21A Zn5 N13 C68 82.8(11) . . . . ? N14 Zn5 N13 C68 -35.3(10) . . . . ? S5 Zn5 N13 C68 -162.2(9) . . . . ? O21A Zn5 N14 C71 97.4(11) . . . . ? N13 Zn5 N14 C71 -134.1(10) . . . . ? S5 Zn5 N14 C71 -26.2(12) . . . . ? O21A Zn5 N14 C70 -91.1(10) . . . . ? N13 Zn5 N14 C70 37.3(10) . . . . ? S5 Zn5 N14 C70 145.2(8) . . . . ? N16 Zn6 N15 C78 -137.7(14) . . . . ? S6 Zn6 N15 C78 -8.8(14) . . . . ? O22A Zn6 N15 C78 118.7(14) . . . . ? O22B Zn6 N15 C78 104.9(15) . . . . ? N16 Zn6 N15 C79 37.3(11) . . . . ? S6 Zn6 N15 C79 166.2(10) . . . . ? O22A Zn6 N15 C79 -66.2(11) . . . . ? O22B Zn6 N15 C79 -80.0(13) . . . . ? N15 Zn6 N16 C82 133.0(13) . . . . ? S6 Zn6 N16 C82 23.6(15) . . . . ? O22A Zn6 N16 C82 -142.7(13) . . . . ? O22B Zn6 N16 C82 -83.6(13) . . . . ? N15 Zn6 N16 C81 -38.8(9) . . . . ? S6 Zn6 N16 C81 -148.2(8) . . . . ? O22A Zn6 N16 C81 45.5(10) . . . . ? O22B Zn6 N16 C81 104.6(10) . . . . ? N18 Zn7 N17 C89 134.7(15) . . . . ? O23A Zn7 N17 C89 -127.8(15) . . . . ? S7 Zn7 N17 C89 10.2(16) . . . . ? N18 Zn7 N17 C90 -40.4(10) . . . . ? O23A Zn7 N17 C90 57.2(11) . . . . ? S7 Zn7 N17 C90 -164.9(9) . . . . ? O23A Zn7 N18 C93 102.1(14) . . . . ? N17 Zn7 N18 C93 -137.7(14) . . . . ? S7 Zn7 N18 C93 -29.6(15) . . . . ? O23A Zn7 N18 C92 -87.4(9) . . . . ? N17 Zn7 N18 C92 32.8(10) . . . . ? S7 Zn7 N18 C92 141.0(8) . . . . ? O24A Zn8 N19 C100 107.1(13) . . . . ? N20 Zn8 N19 C100 -133.2(13) . . . . ? S8 Zn8 N19 C100 -18.6(14) . . . . ? O24A Zn8 N19 C101 -77.3(12) . . . . ? N20 Zn8 N19 C101 42.4(11) . . . . ? S8 Zn8 N19 C101 157.0(10) . . . . ? N19 Zn8 N20 C104 130.7(12) . . . . ? O24A Zn8 N20 C104 -94.9(12) . . . . ? S8 Zn8 N20 C104 20.7(13) . . . . ? N19 Zn8 N20 C103 -40.9(9) . . . . ? O24A Zn8 N20 C103 93.5(9) . . . . ? S8 Zn8 N20 C103 -150.9(8) . . . . ? Zn5 S5 C61 C62 -159.2(4) . . . . ? Zn5 S5 C61 C66 38.8(6) . . . . ? C66 C61 C62 C63 0.0 . . . . ? S5 C61 C62 C63 -163.1(7) . . . . ? C66 C61 C62 C104 -178.1(11) . . . . ? S5 C61 C62 C104 18.7(11) . . . . ? C61 C62 C63 C64 0.0 . . . . ? C104 C62 C63 C64 178.3(10) . . . . ? C62 C63 C64 C65 0.0 . . . . ? C62 C63 C64 C105 179.6(9) . . . . ? C63 C64 C65 C66 0.0 . . . . ? C105 C64 C65 C66 -179.5(9) . . . . ? C64 C65 C66 C61 0.0 . . . . ? C64 C65 C66 C67 -177.3(11) . . . . ? C62 C61 C66 C65 0.0 . . . . ? S5 C61 C66 C65 160.7(8) . . . . ? C62 C61 C66 C67 177.1(11) . . . . ? S5 C61 C66 C67 -22.2(11) . . . . ? C68 N13 C67 C66 -173.7(17) . . . . ? Zn5 N13 C67 C66 9(3) . . . . ? C65 C66 C67 N13 166(2) . . . . ? C61 C66 C67 N13 -12(3) . . . . ? C67 N13 C68 C69 -122.4(18) . . . . ? Zn5 N13 C68 C69 55.1(15) . . . . ? N13 C68 C69 C70 -67.1(17) . . . . ? C71 N14 C70 C69 115.0(15) . . . . ? Zn5 N14 C70 C69 -55.3(15) . . . . ? C68 C69 C70 N14 63.9(17) . . . . ? C70 N14 C71 C73 176.8(13) . . . . ? Zn5 N14 C71 C73 -12(2) . . . . ? Zn6 S6 C72 C73 164.6(4) . . . . ? Zn6 S6 C72 C77 -24.8(7) . . . . ? C77 C72 C73 C74 0.0 . . . . ? S6 C72 C73 C74 171.5(7) . . . . ? C77 C72 C73 C71 176.5(10) . . . . ? S6 C72 C73 C71 -11.9(9) . . . . ? N14 C71 C73 C72 135.5(14) . . . . ? N14 C71 C73 C74 -48.0(19) . . . . ? C72 C73 C74 C75 0.0 . . . . ? C71 C73 C74 C75 -176.5(10) . . . . ? C73 C74 C75 C76 0.0 . . . . ? C73 C74 C75 C109 -174.8(9) . . . . ? C74 C75 C76 C77 0.0 . . . . ? C109 C75 C76 C77 175.6(8) . . . . ? C75 C76 C77 C72 0.0 . . . . ? C75 C76 C77 C78 177.0(10) . . . . ? C73 C72 C77 C76 0.0 . . . . ? S6 C72 C77 C76 -169.9(8) . . . . ? C73 C72 C77 C78 -176.0(13) . . . . ? S6 C72 C77 C78 14.1(13) . . . . ? C79 N15 C78 C77 179.5(11) . . . . ? Zn6 N15 C78 C77 -5(2) . . . . ? C76 C77 C78 N15 -171.0(12) . . . . ? C72 C77 C78 N15 5(2) . . . . ? C78 N15 C79 C80 127.1(14) . . . . ? Zn6 N15 C79 C80 -48.8(16) . . . . ? N15 C79 C80 C81 58.1(18) . . . . ? C82 N16 C81 C80 -114.1(15) . . . . ? Zn6 N16 C81 C80 59.1(15) . . . . ? C79 C80 C81 N16 -66.9(18) . . . . ? C81 N16 C82 C84 -176.2(11) . . . . ? Zn6 N16 C82 C84 11.9(19) . . . . ? Zn7 S7 C83 C84 -168.5(4) . . . . ? Zn7 S7 C83 C88 19.2(7) . . . . ? C88 C83 C84 C85 0.0 . . . . ? S7 C83 C84 C85 -172.8(7) . . . . ? C88 C83 C84 C82 -173.0(9) . . . . ? S7 C83 C84 C82 14.2(9) . . . . ? N16 C82 C84 C85 42.9(16) . . . . ? N16 C82 C84 C83 -144.5(11) . . . . ? C83 C84 C85 C86 0.0 . . . . ? C82 C84 C85 C86 172.3(10) . . . . ? C84 C85 C86 C87 0.0 . . . . ? C84 C85 C86 C113 174.6(10) . . . . ? C85 C86 C87 C88 0.0 . . . . ? C113 C86 C87 C88 -174.9(10) . . . . ? C86 C87 C88 C83 0.0 . . . . ? C86 C87 C88 C89 -176.3(10) . . . . ? C84 C83 C88 C87 0.0 . . . . ? S7 C83 C88 C87 171.8(8) . . . . ? C84 C83 C88 C89 174.9(14) . . . . ? S7 C83 C88 C89 -13.3(14) . . . . ? C90 N17 C89 C88 172.9(11) . . . . ? Zn7 N17 C89 C88 -2(2) . . . . ? C87 C88 C89 N17 177.4(12) . . . . ? C83 C88 C89 N17 2(2) . . . . ? C89 N17 C90 C91 -123.4(14) . . . . ? Zn7 N17 C90 C91 52.9(14) . . . . ? N17 C90 C91 C92 -72.0(18) . . . . ? C93 N18 C92 C91 121.9(17) . . . . ? Zn7 N18 C92 C91 -49.2(15) . . . . ? C90 C91 C92 N18 75.9(19) . . . . ? C92 N18 C93 C95 -179.8(14) . . . . ? Zn7 N18 C93 C95 -11(3) . . . . ? Zn8 S8 C94 C95 161.1(4) . . . . ? Zn8 S8 C94 C99 -36.6(7) . . . . ? C99 C94 C95 C96 0.0 . . . . ? S8 C94 C95 C96 164.2(7) . . . . ? C99 C94 C95 C93 -176.8(11) . . . . ? S8 C94 C95 C93 -12.6(10) . . . . ? N18 C93 C95 C96 -41(2) . . . . ? N18 C93 C95 C94 136.4(16) . . . . ? C94 C95 C96 C97 0.0 . . . . ? C93 C95 C96 C97 177.1(10) . . . . ? C95 C96 C97 C98 0.0 . . . . ? C95 C96 C97 C117 -179.5(10) . . . . ? C96 C97 C98 C99 0.0 . . . . ? C117 C97 C98 C99 179.6(9) . . . . ? C97 C98 C99 C94 0.0 . . . . ? C97 C98 C99 C100 -179.8(11) . . . . ? C95 C94 C99 C98 0.0 . . . . ? S8 C94 C99 C98 -160.6(9) . . . . ? C95 C94 C99 C100 179.7(12) . . . . ? S8 C94 C99 C100 19.1(13) . . . . ? C101 N19 C100 C99 178.7(14) . . . . ? Zn8 N19 C100 C99 -6(2) . . . . ? C98 C99 C100 N19 -168.7(16) . . . . ? C94 C99 C100 N19 12(2) . . . . ? C100 N19 C101 C102 120.8(16) . . . . ? Zn8 N19 C101 C102 -54.9(15) . . . . ? N19 C101 C102 C103 65.8(17) . . . . ? C104 N20 C103 C102 -111.8(17) . . . . ? Zn8 N20 C103 C102 59.2(14) . . . . ? C101 C102 C103 N20 -74.4(18) . . . . ? C103 N20 C104 C62 -178.8(15) . . . . ? Zn8 N20 C104 C62 11(3) . . . . ? C61 C62 C104 N20 -143.6(17) . . . . ? C63 C62 C104 N20 38(2) . . . . ? C63 C64 C105 C106 60.7(12) . . . . ? C65 C64 C105 C106 -119.8(11) . . . . ? C63 C64 C105 C10B 125.8(13) . . . . ? C65 C64 C105 C10B -54.7(13) . . . . ? C63 C64 C105 C107 177.8(11) . . . . ? C65 C64 C105 C107 -2.7(13) . . . . ? C63 C64 C105 C10A 6.1(15) . . . . ? C65 C64 C105 C10A -174.3(13) . . . . ? C63 C64 C105 C10C -117.0(13) . . . . ? C65 C64 C105 C10C 62.6(14) . . . . ? C63 C64 C105 C108 -58.4(13) . . . . ? C65 C64 C105 C108 121.2(12) . . . . ? C74 C75 C109 C112 -12.5(9) . . . . ? C76 C75 C109 C112 172.4(6) . . . . ? C74 C75 C109 C111 103.6(8) . . . . ? C76 C75 C109 C111 -71.5(7) . . . . ? C74 C75 C109 C110 -131.9(7) . . . . ? C76 C75 C109 C110 52.9(8) . . . . ? C87 C86 C113 C115 -177.2(7) . . . . ? C85 C86 C113 C115 8.1(10) . . . . ? C87 C86 C113 C116 65.0(10) . . . . ? C85 C86 C113 C116 -109.7(9) . . . . ? C87 C86 C113 C114 -56.4(10) . . . . ? C85 C86 C113 C114 128.8(8) . . . . ? C98 C97 C117 C118 178.7(7) . . . . ? C96 C97 C117 C118 -1.8(11) . . . . ? C98 C97 C117 C119 55.7(9) . . . . ? C96 C97 C117 C119 -124.7(8) . . . . ? C98 C97 C117 C120 -63.8(8) . . . . ? C96 C97 C117 C120 115.7(9) . . . . ? O21B N21 O21A Zn5 176.4(13) . . . . ? O21C N21 O21A Zn5 -10(2) . . . . ? N14 Zn5 O21A N21 70.6(12) . . . . ? N13 Zn5 O21A N21 -38.9(14) . . . . ? S5 Zn5 O21A N21 -153.8(11) . . . . ? O22B N22 O22A Zn6 7(2) . . . . ? O22C N22 O22A Zn6 173.7(16) . . . . ? N16 Zn6 O22A N22 94.9(12) . . . . ? N15 Zn6 O22A N22 -173.5(13) . . . . ? S6 Zn6 O22A N22 -71.1(13) . . . . ? O22B Zn6 O22A N22 -4.1(11) . . . . ? O22C N22 O22B Zn6 -175.2(13) . . . . ? O22A N22 O22B Zn6 -7(2) . . . . ? N16 Zn6 O22B N22 -92.8(12) . . . . ? N15 Zn6 O22B N22 20.6(16) . . . . ? S6 Zn6 O22B N22 137.4(11) . . . . ? O22A Zn6 O22B N22 4.1(11) . . . . ? O23C N23 O23A Zn7 169.4(11) . . . . ? O23B N23 O23A Zn7 -12.4(19) . . . . ? N18 Zn7 O23A N23 163.0(10) . . . . ? N17 Zn7 O23A N23 58.6(11) . . . . ? S7 Zn7 O23A N23 -68.0(11) . . . . ? O24C N24 O24A Zn8 -178.2(16) . . . . ? O24B N24 O24A Zn8 3(2) . . . . ? N19 Zn8 O24A N24 27.1(13) . . . . ? N20 Zn8 O24A N24 -87.2(11) . . . . ? S8 Zn8 O24A N24 153.2(10) . . . . ? #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 282076' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C91 H114 N12 O3 S6 Zn6 4+, 4(Cl O4 1-), 4(H2 O) ; _chemical_formula_sum 'C91 H122 Cl4 N12 O23 S6 Zn6' _chemical_formula_weight 2478.39 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' S S 0.1246 0.1234 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 16.2540(4) _cell_length_b 46.4678(12) _cell_length_c 16.5610(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.158(1) _cell_angle_gamma 90.00 _cell_volume 11885.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4673 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 22.82 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5120 _exptl_absorpt_coefficient_mu 1.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _exptl_special_details ; Perchlorate anions refined with restrained geometry and a single isotropic displacement parameter common to all O atoms. Lattice water molecules also refined with a single isotropic displacement parameter common to all. Solvent and counterions poorly resolved - likely to be much more present in the voids. A large part of the reason for the relatively high R factors. The problem is unfortunately too large (and the data too poor) for application of SQUEEZE. H atoms omitted from lattice water molecules so that atoms sites are 8 H per formula unit (32 per unit cell) short of the empirical formula. C100 refined with an isotropic displacement parameter. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 43241 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.1354 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -55 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.05 _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.959 _reflns_number_total 20184 _reflns_number_gt 10121 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-8 (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2500P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20184 _refine_ls_number_parameters 1072 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.1986 _refine_ls_R_factor_gt 0.1120 _refine_ls_wR_factor_ref 0.3889 _refine_ls_wR_factor_gt 0.3244 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.822 _refine_diff_density_min -1.545 _refine_diff_density_rms 0.185 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.63749(10) 0.11303(3) 0.59893(9) 0.0442(4) Uani 1 1 d . . . Zn2 Zn 0.65192(9) 0.06865(3) 0.77159(9) 0.0368(4) Uani 1 1 d . . . Zn3 Zn 0.85646(10) 0.17240(4) 0.71840(11) 0.0541(5) Uani 1 1 d . . . Zn4 Zn 0.91508(9) 0.10017(3) 0.70930(9) 0.0399(4) Uani 1 1 d . . . Zn5 Zn 0.66950(10) 0.15818(3) 0.86887(10) 0.0469(4) Uani 1 1 d . . . Zn6 Zn 0.87010(9) 0.12767(3) 0.96961(9) 0.0398(4) Uani 1 1 d . . . S1 S 0.5611(2) 0.07366(7) 0.6312(2) 0.0412(8) Uani 1 1 d . . . S2 S 0.77512(19) 0.08375(7) 0.69807(19) 0.0368(7) Uani 1 1 d . . . S3 S 0.9558(2) 0.14537(8) 0.6733(2) 0.0422(8) Uani 1 1 d . . . S4 S 0.9035(2) 0.13117(7) 0.84351(19) 0.0395(8) Uani 1 1 d . . . S5 S 0.7736(2) 0.15852(7) 1.0047(2) 0.0420(8) Uani 1 1 d . . . S6 S 0.71646(19) 0.10357(7) 0.87438(19) 0.0377(7) Uani 1 1 d . . . N1 N 0.5478(7) 0.0538(2) 0.8104(7) 0.040(2) Uani 1 1 d . . . N2 N 0.7174(6) 0.0312(2) 0.7919(6) 0.039(2) Uani 1 1 d . . . N3 N 0.6963(7) 0.1075(2) 0.5078(7) 0.046(3) Uani 1 1 d . . . N4 N 0.5237(7) 0.1269(3) 0.5087(7) 0.055(3) Uani 1 1 d . . . N5 N 0.8484(8) 0.2037(3) 0.6261(8) 0.058(3) Uani 1 1 d . . . N6 N 0.9055(10) 0.1991(3) 0.8114(9) 0.062(4) Uani 1 1 d . . . N7 N 1.0140(7) 0.0801(2) 0.8017(7) 0.043(3) Uani 1 1 d . . . N8 N 0.9479(7) 0.0811(2) 0.6093(7) 0.047(3) Uani 1 1 d . . . N9 N 0.6338(7) 0.1999(3) 0.8894(8) 0.056(3) Uani 1 1 d . . . N10 N 0.5526(6) 0.1422(2) 0.8644(7) 0.044(3) Uani 1 1 d . . . N11 N 0.8866(6) 0.0892(2) 1.0276(7) 0.044(3) Uani 1 1 d . . . N12 N 0.9754(6) 0.1465(3) 1.0596(7) 0.046(3) Uani 1 1 d . . . C1 C 0.4697(8) 0.0914(3) 0.6455(8) 0.041(3) Uani 1 1 d . . . C2 C 0.4243(8) 0.1114(3) 0.5868(8) 0.044(3) Uani 1 1 d . . . C3 C 0.3477(8) 0.1227(3) 0.5921(8) 0.048(3) Uani 1 1 d . . . H3A H 0.3183 0.1364 0.5504 0.057 Uiso 1 1 calc R . . C4 C 0.3104(7) 0.1153(3) 0.6560(9) 0.046(3) Uani 1 1 d D A . C5 C 0.3573(8) 0.0954(3) 0.7133(8) 0.045(3) Uani 1 1 d . . . H5A H 0.3362 0.0897 0.7584 0.054 Uiso 1 1 calc R . . C6 C 0.4357(8) 0.0829(3) 0.7091(8) 0.041(3) Uani 1 1 d . . . C7 C 0.4713(9) 0.0611(3) 0.7766(8) 0.045(3) Uani 1 1 d . . . H7A H 0.4299 0.0515 0.7967 0.053 Uiso 1 1 calc R . . C8 C 0.5694(8) 0.0324(3) 0.8803(8) 0.045(3) Uani 1 1 d . . . H8A H 0.5150 0.0249 0.8872 0.054 Uiso 1 1 calc R . . H8B H 0.6020 0.0421 0.9339 0.054 Uiso 1 1 calc R . . C9 C 0.6221(10) 0.0076(3) 0.8656(9) 0.054(4) Uani 1 1 d . . . H9A H 0.5930 -0.0006 0.8087 0.065 Uiso 1 1 calc R . . H9B H 0.6238 -0.0076 0.9082 0.065 Uiso 1 1 calc R . . C10 C 0.7195(9) 0.0160(3) 0.8716(9) 0.053(4) Uani 1 1 d . . . H10A H 0.7449 0.0286 0.9212 0.063 Uiso 1 1 calc R . . H10B H 0.7555 -0.0016 0.8784 0.063 Uiso 1 1 calc R . . C11 C 0.7516(9) 0.0178(3) 0.7442(9) 0.051(3) Uani 1 1 d . . . H11A H 0.7799 0.0003 0.7662 0.062 Uiso 1 1 calc R . . C12 C 0.7531(8) 0.0260(3) 0.6576(8) 0.043(3) Uani 1 1 d . . . C13 C 0.7511(8) 0.0023(3) 0.6047(8) 0.046(3) Uani 1 1 d . . . H13A H 0.7502 -0.0165 0.6272 0.055 Uiso 1 1 calc R . . C14 C 0.7503(8) 0.0050(3) 0.5213(8) 0.048(3) Uani 1 1 d D . . C15 C 0.7439(8) 0.0332(3) 0.4876(8) 0.043(3) Uani 1 1 d . . . H15A H 0.7383 0.0360 0.4293 0.052 Uiso 1 1 calc R . . C16 C 0.7458(7) 0.0573(3) 0.5399(7) 0.038(3) Uani 1 1 d . . . C17 C 0.7537(7) 0.0541(3) 0.6271(7) 0.037(3) Uani 1 1 d . . . C18 C 0.7355(8) 0.0844(3) 0.4933(8) 0.043(3) Uani 1 1 d . . . H18A H 0.7596 0.0853 0.4480 0.052 Uiso 1 1 calc R . . C19 C 0.6855(8) 0.1317(3) 0.4480(9) 0.054(4) Uani 1 1 d . . . H19A H 0.7212 0.1284 0.4101 0.065 Uiso 1 1 calc R . . H19B H 0.7054 0.1498 0.4799 0.065 Uiso 1 1 calc R . . C20 C 0.5910(10) 0.1345(4) 0.3953(11) 0.078(5) Uani 1 1 d . . . H20A H 0.5881 0.1476 0.3473 0.093 Uiso 1 1 calc R . . H20B H 0.5712 0.1154 0.3707 0.093 Uiso 1 1 calc R . . C21 C 0.5308(11) 0.1445(4) 0.4343(11) 0.073(5) Uani 1 1 d . . . H21A H 0.4731 0.1452 0.3908 0.087 Uiso 1 1 calc R . . H21B H 0.5466 0.1644 0.4541 0.087 Uiso 1 1 calc R . . C22 C 0.4465(9) 0.1242(3) 0.5146(8) 0.051(4) Uani 1 1 d . . . H22A H 0.3998 0.1311 0.4684 0.061 Uiso 1 1 calc R . . C23 C 0.2253(6) 0.1281(3) 0.6597(8) 0.054(4) Uani 1 1 d D . . C24 C 0.169(2) 0.1036(5) 0.673(2) 0.101(13) Uiso 0.50 1 d PD A 1 H24A H 0.2006 0.0931 0.7252 0.151 Uiso 0.50 1 calc PR A 1 H24B H 0.1559 0.0904 0.6247 0.151 Uiso 0.50 1 calc PR A 1 H24C H 0.1154 0.1113 0.6792 0.151 Uiso 0.50 1 calc PR A 1 C25 C 0.240(2) 0.1493(6) 0.7324(16) 0.117(15) Uiso 0.50 1 d PD A 1 H25A H 0.2764 0.1652 0.7242 0.176 Uiso 0.50 1 calc PR A 1 H25B H 0.2693 0.1395 0.7861 0.176 Uiso 0.50 1 calc PR A 1 H25C H 0.1844 0.1569 0.7338 0.176 Uiso 0.50 1 calc PR A 1 C26 C 0.176(2) 0.1435(7) 0.5776(14) 0.090(11) Uiso 0.50 1 d PD A 1 H26A H 0.2115 0.1592 0.5671 0.136 Uiso 0.50 1 calc PR A 1 H26B H 0.1219 0.1513 0.5827 0.136 Uiso 0.50 1 calc PR A 1 H26C H 0.1631 0.1298 0.5302 0.136 Uiso 0.50 1 calc PR A 1 C24A C 0.2328(19) 0.1604(3) 0.6629(17) 0.069(9) Uiso 0.50 1 d PD A 2 H24D H 0.2833 0.1663 0.6464 0.104 Uiso 0.50 1 calc PR A 2 H24E H 0.2397 0.1671 0.7207 0.104 Uiso 0.50 1 calc PR A 2 H24F H 0.1804 0.1689 0.6235 0.104 Uiso 0.50 1 calc PR A 2 C25A C 0.1558(17) 0.1187(6) 0.5804(12) 0.080(10) Uiso 0.50 1 d PD A 2 H25D H 0.1593 0.1304 0.5321 0.120 Uiso 0.50 1 calc PR A 2 H25E H 0.0989 0.1214 0.5881 0.120 Uiso 0.50 1 calc PR A 2 H25F H 0.1640 0.0984 0.5693 0.120 Uiso 0.50 1 calc PR A 2 C26A C 0.203(2) 0.1175(6) 0.7370(13) 0.079(10) Uiso 0.50 1 d PD A 2 H26D H 0.2319 0.1295 0.7862 0.118 Uiso 0.50 1 calc PR A 2 H26E H 0.2220 0.0975 0.7489 0.118 Uiso 0.50 1 calc PR A 2 H26F H 0.1400 0.1185 0.7257 0.118 Uiso 0.50 1 calc PR A 2 C27 C 0.7542(8) -0.0201(2) 0.4640(7) 0.050(4) Uani 1 1 d D . . C28 C 0.8474(8) -0.0232(5) 0.4637(13) 0.115(7) Uiso 1 1 d D . . H28A H 0.8852 -0.0269 0.5216 0.173 Uiso 1 1 calc R . . H28B H 0.8657 -0.0054 0.4424 0.173 Uiso 1 1 calc R . . H28C H 0.8514 -0.0393 0.4268 0.173 Uiso 1 1 calc R . . C29 C 0.6975(11) -0.0144(5) 0.3730(11) 0.138(9) Uiso 1 1 d D . . H29A H 0.6370 -0.0124 0.3716 0.208 Uiso 1 1 calc R . . H29B H 0.7027 -0.0305 0.3367 0.208 Uiso 1 1 calc R . . H29C H 0.7163 0.0034 0.3523 0.208 Uiso 1 1 calc R . . C30 C 0.7262(13) -0.0481(4) 0.4939(13) 0.129(8) Uiso 1 1 d D . . H30A H 0.7623 -0.0519 0.5524 0.194 Uiso 1 1 calc R . . H30B H 0.7328 -0.0638 0.4569 0.194 Uiso 1 1 calc R . . H30C H 0.6654 -0.0466 0.4918 0.194 Uiso 1 1 calc R . . C31 C 0.9148(8) 0.1470(3) 0.5597(8) 0.048(3) Uani 1 1 d . . . C32 C 0.9227(8) 0.1235(3) 0.5114(9) 0.047(3) Uani 1 1 d . . . C33 C 0.9042(9) 0.1272(4) 0.4238(9) 0.058(4) Uani 1 1 d . . . H33A H 0.9127 0.1112 0.3915 0.070 Uiso 1 1 calc R . . C34 C 0.8749(10) 0.1522(4) 0.3813(7) 0.059(4) Uani 1 1 d D . . C35 C 0.8629(11) 0.1749(4) 0.4312(9) 0.068(5) Uani 1 1 d . . . H35A H 0.8401 0.1925 0.4040 0.082 Uiso 1 1 calc R . . C36 C 0.8829(9) 0.1732(3) 0.5195(9) 0.051(4) Uani 1 1 d . . . C37 C 0.8615(10) 0.2001(3) 0.5569(10) 0.062(4) Uani 1 1 d . . . H37A H 0.8572 0.2169 0.5231 0.075 Uiso 1 1 calc R . . C38 C 0.8239(14) 0.2324(4) 0.6480(13) 0.092(6) Uani 1 1 d . . . H38A H 0.7623 0.2319 0.6455 0.111 Uiso 1 1 calc R . . H38B H 0.8290 0.2462 0.6042 0.111 Uiso 1 1 calc R . . C39 C 0.8752(11) 0.2436(3) 0.7322(10) 0.066(4) Uani 1 1 d . . . H39A H 0.8590 0.2639 0.7363 0.080 Uiso 1 1 calc R . . H39B H 0.9372 0.2432 0.7359 0.080 Uiso 1 1 calc R . . C40 C 0.8648(12) 0.2276(3) 0.8069(11) 0.070(5) Uani 1 1 d . . . H40A H 0.8927 0.2385 0.8598 0.084 Uiso 1 1 calc R . . H40B H 0.8026 0.2254 0.8008 0.084 Uiso 1 1 calc R . . C41 C 0.9749(15) 0.1964(3) 0.8739(14) 0.078(6) Uani 1 1 d . . . H41A H 0.9896 0.2125 0.9110 0.093 Uiso 1 1 calc R . . C42 C 1.0389(9) 0.1706(3) 0.8978(9) 0.054(4) Uani 1 1 d . . . C43 C 1.1223(11) 0.1785(4) 0.9400(10) 0.069(5) Uani 1 1 d . . . H43A H 1.1352 0.1980 0.9568 0.083 Uiso 1 1 calc R . . C44 C 1.1899(8) 0.1577(4) 0.9589(9) 0.072(5) Uani 1 1 d D B . C45 C 1.1669(9) 0.1293(4) 0.9327(9) 0.063(4) Uani 1 1 d . . . H45A H 1.2106 0.1150 0.9446 0.076 Uiso 1 1 calc R . . C46 C 1.0798(8) 0.1215(3) 0.8888(8) 0.040(3) Uani 1 1 d . . . C47 C 1.0146(8) 0.1419(3) 0.8758(8) 0.041(3) Uani 1 1 d . . . C48 C 1.0712(8) 0.0919(4) 0.8635(9) 0.054(4) Uani 1 1 d . . . H48A H 1.1141 0.0793 0.8977 0.065 Uiso 1 1 calc R . . C49 C 1.0206(9) 0.0500(3) 0.7831(9) 0.053(4) Uani 1 1 d . . . H49A H 0.9651 0.0404 0.7793 0.064 Uiso 1 1 calc R . . H49B H 1.0662 0.0411 0.8309 0.064 Uiso 1 1 calc R . . C50 C 1.0426(9) 0.0443(3) 0.6979(9) 0.052(4) Uani 1 1 d . . . H50A H 1.0931 0.0563 0.6982 0.063 Uiso 1 1 calc R . . H50B H 1.0597 0.0239 0.6968 0.063 Uiso 1 1 calc R . . C51 C 0.9720(9) 0.0504(3) 0.6205(10) 0.062(4) Uani 1 1 d . . . H51A H 0.9206 0.0391 0.6213 0.074 Uiso 1 1 calc R . . H51B H 0.9890 0.0439 0.5711 0.074 Uiso 1 1 calc R . . C52 C 0.9476(8) 0.0945(3) 0.5401(8) 0.051(4) Uani 1 1 d . . . H52A H 0.9671 0.0832 0.5018 0.062 Uiso 1 1 calc R . . C53 C 0.8551(10) 0.1559(3) 0.2865(7) 0.079(5) Uani 1 1 d D . . C54 C 0.8425(15) 0.1869(3) 0.2574(17) 0.143(9) Uiso 1 1 d D . . H54A H 0.7940 0.1952 0.2727 0.214 Uiso 1 1 calc R . . H54B H 0.8300 0.1877 0.1956 0.214 Uiso 1 1 calc R . . H54C H 0.8954 0.1978 0.2850 0.214 Uiso 1 1 calc R . . C55 C 0.7743(11) 0.1387(4) 0.2432(17) 0.143(9) Uiso 1 1 d D . . H55A H 0.7256 0.1464 0.2595 0.215 Uiso 1 1 calc R . . H55B H 0.7836 0.1185 0.2607 0.215 Uiso 1 1 calc R . . H55C H 0.7612 0.1401 0.1815 0.215 Uiso 1 1 calc R . . C56 C 0.9307(11) 0.1436(5) 0.2624(17) 0.143(9) Uiso 1 1 d D . . H56A H 0.9395 0.1234 0.2804 0.215 Uiso 1 1 calc R . . H56B H 0.9832 0.1546 0.2906 0.215 Uiso 1 1 calc R . . H56C H 0.9184 0.1447 0.2007 0.215 Uiso 1 1 calc R . . C57 C 1.2818(8) 0.1655(4) 1.0094(10) 0.118(9) Uani 1 1 d D . . C58 C 1.298(3) 0.1893(6) 0.952(2) 0.127(17) Uiso 0.50 1 d PD B 1 H58A H 1.2441 0.1931 0.9056 0.191 Uiso 0.50 1 calc PR B 1 H58B H 1.3430 0.1832 0.9278 0.191 Uiso 0.50 1 calc PR B 1 H58C H 1.3162 0.2069 0.9852 0.191 Uiso 0.50 1 calc PR B 1 C59 C 1.3525(18) 0.1434(6) 1.0217(19) 0.076(9) Uiso 0.50 1 d PD B 1 H59A H 1.3435 0.1278 1.0578 0.114 Uiso 0.50 1 calc PR B 1 H59B H 1.4088 0.1525 1.0490 0.114 Uiso 0.50 1 calc PR B 1 H59C H 1.3514 0.1356 0.9664 0.114 Uiso 0.50 1 calc PR B 1 C60 C 1.285(2) 0.1791(7) 1.0932(15) 0.090(11) Uiso 0.50 1 d PD B 1 H60A H 1.2770 0.1642 1.1319 0.135 Uiso 0.50 1 calc PR B 1 H60B H 1.2392 0.1935 1.0838 0.135 Uiso 0.50 1 calc PR B 1 H60C H 1.3416 0.1883 1.1182 0.135 Uiso 0.50 1 calc PR B 1 C58A C 1.294(3) 0.1430(7) 1.080(2) 0.17(2) Uiso 0.50 1 d PD B 2 H58D H 1.2394 0.1325 1.0717 0.248 Uiso 0.50 1 calc PR B 2 H58E H 1.3100 0.1527 1.1355 0.248 Uiso 0.50 1 calc PR B 2 H58F H 1.3394 0.1294 1.0787 0.248 Uiso 0.50 1 calc PR B 2 C59A C 1.298(2) 0.1947(5) 1.051(2) 0.101(13) Uiso 0.50 1 d PD B 2 H59D H 1.2951 0.1933 1.1088 0.151 Uiso 0.50 1 calc PR B 2 H59E H 1.2533 0.2082 1.0180 0.151 Uiso 0.50 1 calc PR B 2 H59F H 1.3550 0.2016 1.0518 0.151 Uiso 0.50 1 calc PR B 2 C60A C 1.3484(19) 0.1590(7) 0.965(2) 0.085(11) Uiso 0.50 1 d PD B 2 H60D H 1.3701 0.1393 0.9790 0.128 Uiso 0.50 1 calc PR B 2 H60E H 1.3966 0.1726 0.9848 0.128 Uiso 0.50 1 calc PR B 2 H60F H 1.3218 0.1609 0.9038 0.128 Uiso 0.50 1 calc PR B 2 C61 C 0.8242(9) 0.1921(3) 1.0104(8) 0.047(3) Uani 1 1 d . . . C62 C 0.9134(10) 0.1959(4) 1.0532(8) 0.059(4) Uani 1 1 d . . . C63 C 0.9479(11) 0.2245(4) 1.0648(9) 0.062(4) Uani 1 1 d . . . H63A H 1.0085 0.2264 1.0916 0.074 Uiso 1 1 calc R . . C64 C 0.9036(14) 0.2484(3) 1.0418(11) 0.071(5) Uani 1 1 d D . . C65 C 0.8166(14) 0.2443(3) 0.9998(11) 0.074(5) Uani 1 1 d . . . H65A H 0.7828 0.2610 0.9800 0.089 Uiso 1 1 calc R . . C66 C 0.7730(11) 0.2174(3) 0.9835(9) 0.056(4) Uani 1 1 d . . . C67 C 0.6834(12) 0.2182(4) 0.9333(11) 0.069(5) Uani 1 1 d . . . H67A H 0.6567 0.2363 0.9338 0.082 Uiso 1 1 calc R . . C68 C 0.5488(9) 0.2097(4) 0.8378(12) 0.075(5) Uani 1 1 d . . . H68A H 0.5468 0.2108 0.7776 0.090 Uiso 1 1 calc R . . H68B H 0.5378 0.2292 0.8563 0.090 Uiso 1 1 calc R . . C69 C 0.4774(10) 0.1887(4) 0.8465(11) 0.067(5) Uani 1 1 d . . . H69A H 0.4819 0.1873 0.9074 0.081 Uiso 1 1 calc R . . H69B H 0.4202 0.1972 0.8164 0.081 Uiso 1 1 calc R . . C70 C 0.4798(9) 0.1593(4) 0.8137(10) 0.061(4) Uani 1 1 d . . . H70A H 0.4253 0.1493 0.8115 0.074 Uiso 1 1 calc R . . H70B H 0.4824 0.1606 0.7549 0.074 Uiso 1 1 calc R . . C71 C 0.5370(8) 0.1209(3) 0.9066(8) 0.041(3) Uani 1 1 d . . . H71A H 0.4776 0.1168 0.8979 0.049 Uiso 1 1 calc R . . C72 C 0.5994(8) 0.1021(3) 0.9665(8) 0.041(3) Uani 1 1 d . . . C73 C 0.5694(9) 0.0917(3) 1.0328(8) 0.047(3) Uani 1 1 d . . . H73A H 0.5119 0.0959 1.0316 0.057 Uiso 1 1 calc R . . C74 C 0.6225(9) 0.0754(3) 1.1000(7) 0.046(3) Uani 1 1 d D . . C75 C 0.7070(9) 0.0702(3) 1.0995(8) 0.045(3) Uani 1 1 d . . . H75A H 0.7451 0.0597 1.1453 0.054 Uiso 1 1 calc R . . C76 C 0.7383(8) 0.0798(3) 1.0333(8) 0.038(3) Uani 1 1 d . . . C77 C 0.6825(7) 0.0954(3) 0.9637(7) 0.033(3) Uani 1 1 d . . . C78 C 0.8305(9) 0.0740(3) 1.0493(8) 0.048(3) Uani 1 1 d . . . H78A H 0.8518 0.0568 1.0797 0.058 Uiso 1 1 calc R . . C79 C 0.9783(9) 0.0800(3) 1.0613(11) 0.063(4) Uani 1 1 d . . . H79A H 1.0031 0.0788 1.0138 0.075 Uiso 1 1 calc R . . H79B H 0.9806 0.0604 1.0859 0.075 Uiso 1 1 calc R . . C80 C 1.0332(9) 0.1001(3) 1.1286(10) 0.059(4) Uani 1 1 d . . . H80A H 1.0029 0.1037 1.1711 0.071 Uiso 1 1 calc R . . H80B H 1.0885 0.0904 1.1582 0.071 Uiso 1 1 calc R . . C81 C 1.0532(9) 0.1283(4) 1.0972(9) 0.062(4) Uani 1 1 d . . . H81A H 1.0824 0.1250 1.0538 0.074 Uiso 1 1 calc R . . H81B H 1.0940 0.1389 1.1449 0.074 Uiso 1 1 calc R . . C82 C 0.9779(9) 0.1729(4) 1.0840(8) 0.053(4) Uani 1 1 d . . . H82A H 1.0287 0.1783 1.1281 0.063 Uiso 1 1 calc R . . C83 C 0.9407(10) 0.2788(3) 1.0577(10) 0.102(7) Uani 1 1 d D . . C84 C 0.8969(13) 0.2946(6) 1.1132(13) 0.145(10) Uiso 1 1 d D . . H84A H 0.9203 0.3142 1.1242 0.218 Uiso 1 1 calc R . . H84B H 0.9076 0.2843 1.1671 0.218 Uiso 1 1 calc R . . H84C H 0.8344 0.2955 1.0840 0.218 Uiso 1 1 calc R . . C85 C 0.9209(15) 0.2941(6) 0.9734(11) 0.162(11) Uiso 1 1 d D . . H85A H 0.9452 0.3136 0.9825 0.243 Uiso 1 1 calc R . . H85B H 0.8580 0.2953 0.9468 0.243 Uiso 1 1 calc R . . H85C H 0.9466 0.2835 0.9361 0.243 Uiso 1 1 calc R . . C86 C 1.0373(10) 0.2785(5) 1.1018(12) 0.106(7) Uiso 1 1 d D . . H86A H 1.0589 0.2983 1.1104 0.160 Uiso 1 1 calc R . . H86B H 1.0660 0.2681 1.0667 0.160 Uiso 1 1 calc R . . H86C H 1.0495 0.2689 1.1570 0.160 Uiso 1 1 calc R . . C87 C 0.5886(7) 0.0625(2) 1.1678(6) 0.053(4) Uani 1 1 d D . . C88 C 0.5895(10) 0.0301(3) 1.1576(10) 0.083(5) Uiso 1 1 d D . . H88A H 0.6483 0.0237 1.1626 0.124 Uiso 1 1 calc R . . H88B H 0.5502 0.0247 1.1016 0.124 Uiso 1 1 calc R . . H88C H 0.5704 0.0209 1.2020 0.124 Uiso 1 1 calc R . . C89 C 0.4965(7) 0.0718(3) 1.1606(10) 0.080(5) Uiso 1 1 d D . . H89A H 0.4576 0.0670 1.1039 0.121 Uiso 1 1 calc R . . H89B H 0.4952 0.0926 1.1697 0.121 Uiso 1 1 calc R . . H89C H 0.4774 0.0617 1.2037 0.121 Uiso 1 1 calc R . . C90 C 0.6462(8) 0.0703(3) 1.2567(8) 0.076(5) Uiso 1 1 d D . . H90A H 0.7057 0.0641 1.2639 0.114 Uiso 1 1 calc R . . H90B H 0.6249 0.0607 1.2989 0.114 Uiso 1 1 calc R . . H90C H 0.6452 0.0912 1.2646 0.114 Uiso 1 1 calc R . . C100 C 0.6903(8) 0.1579(3) 0.7083(8) 0.040(3) Uiso 1 1 d . . . O100 O 0.6266(7) 0.1415(3) 0.6976(9) 0.098(4) Uani 1 1 d . . . O101 O 0.7357(7) 0.1555(2) 0.6594(6) 0.068(3) Uani 1 1 d . . . O102 O 0.7174(10) 0.1715(2) 0.7760(7) 0.100(5) Uani 1 1 d . . . Cl1 Cl 0.3142(3) 0.05429(9) 0.9192(3) 0.0669(10) Uiso 1 1 d D . . O1A O 0.2643(12) 0.0477(4) 0.8363(8) 0.213(3) Uiso 1 1 d D . . O1B O 0.3489(12) 0.0817(3) 0.9207(13) 0.213(3) Uiso 1 1 d D . . O1C O 0.3816(10) 0.0344(4) 0.9464(12) 0.213(3) Uiso 1 1 d D . . O1D O 0.2627(11) 0.0530(4) 0.9722(11) 0.213(3) Uiso 1 1 d D . . Cl2 Cl 0.1526(5) 0.20980(19) 0.2928(5) 0.160(3) Uiso 1 1 d D . . O2A O 0.1752(13) 0.1999(4) 0.3794(9) 0.213(3) Uiso 1 1 d D . . O2B O 0.2023(12) 0.2337(3) 0.2927(13) 0.213(3) Uiso 1 1 d D . . O2C O 0.0649(8) 0.2168(4) 0.2686(12) 0.213(3) Uiso 1 1 d D . . O2D O 0.1679(13) 0.1876(4) 0.2451(12) 0.213(3) Uiso 1 1 d D . . Cl3 Cl 0.9202(5) 0.04654(17) 0.3139(5) 0.142(2) Uiso 1 1 d D . . O3A O 1.0004(9) 0.0352(4) 0.3344(12) 0.213(3) Uiso 1 1 d D . . O3B O 0.8615(11) 0.0258(4) 0.2615(12) 0.213(3) Uiso 1 1 d D . . O3C O 0.9124(13) 0.0707(3) 0.2604(12) 0.213(3) Uiso 1 1 d D . . O3D O 0.8900(13) 0.0531(4) 0.3800(10) 0.213(3) Uiso 1 1 d D . . Cl4 Cl 0.6456(5) 0.22851(18) 0.3915(5) 0.155(3) Uiso 1 1 d D . . O4A O 0.5655(9) 0.2290(4) 0.3318(11) 0.213(3) Uiso 1 1 d D . . O4B O 0.7114(10) 0.2357(4) 0.3586(12) 0.213(3) Uiso 1 1 d D . . O4C O 0.6629(13) 0.2015(3) 0.4309(12) 0.213(3) Uiso 1 1 d D . . O4D O 0.6476(13) 0.2487(4) 0.4563(11) 0.213(3) Uiso 1 1 d D . . O1W O 0.832(2) 0.0039(7) 0.099(2) 0.257(6) Uiso 1 1 d . . . O2W O 0.469(2) 0.1833(7) 0.253(2) 0.257(6) Uiso 1 1 d . . . O3W O 0.197(2) 0.1216(7) 0.349(2) 0.257(6) Uiso 1 1 d . . . O4W O 0.543(2) 0.1960(7) 0.112(2) 0.257(6) Uiso 1 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 0.0547(9) 0.0467(9) 0.0375(9) -0.0015(7) 0.0236(7) -0.0014(7) Zn2 0.0400(8) 0.0404(8) 0.0345(8) -0.0038(6) 0.0182(7) -0.0057(6) Zn3 0.0507(9) 0.0490(10) 0.0747(12) -0.0059(8) 0.0372(9) 0.0003(8) Zn4 0.0367(8) 0.0479(9) 0.0408(9) -0.0085(7) 0.0202(7) -0.0056(7) Zn5 0.0438(9) 0.0566(10) 0.0470(10) 0.0072(8) 0.0237(7) 0.0019(7) Zn6 0.0375(8) 0.0526(10) 0.0335(8) -0.0002(7) 0.0174(6) -0.0020(7) S1 0.0425(17) 0.051(2) 0.0361(18) 0.0028(14) 0.0210(15) 0.0049(15) S2 0.0407(17) 0.0416(18) 0.0337(17) -0.0058(13) 0.0197(14) -0.0053(14) S3 0.0403(17) 0.055(2) 0.0358(18) -0.0071(15) 0.0190(15) -0.0033(15) S4 0.0430(17) 0.047(2) 0.0357(17) -0.0080(14) 0.0234(14) -0.0080(15) S5 0.0436(18) 0.047(2) 0.0412(19) -0.0043(15) 0.0220(15) -0.0022(15) S6 0.0377(16) 0.0490(19) 0.0327(17) -0.0046(14) 0.0204(14) -0.0084(14) N1 0.039(6) 0.043(6) 0.042(6) -0.006(5) 0.020(5) -0.009(5) N2 0.040(6) 0.051(7) 0.033(6) 0.003(5) 0.022(5) 0.000(5) N3 0.045(6) 0.056(7) 0.041(6) 0.010(5) 0.019(5) -0.011(6) N4 0.059(7) 0.070(8) 0.049(7) 0.011(6) 0.036(6) 0.008(6) N5 0.066(8) 0.056(8) 0.059(8) 0.000(6) 0.028(7) 0.004(6) N6 0.083(10) 0.059(9) 0.062(9) -0.004(7) 0.045(8) -0.005(8) N7 0.044(6) 0.046(7) 0.045(7) -0.001(5) 0.022(6) 0.001(5) N8 0.045(6) 0.049(7) 0.057(8) -0.019(6) 0.030(6) -0.008(5) N9 0.046(7) 0.047(8) 0.076(9) -0.004(7) 0.021(6) -0.005(6) N10 0.041(6) 0.053(7) 0.037(6) 0.003(5) 0.010(5) 0.004(5) N11 0.035(6) 0.058(7) 0.044(7) 0.005(5) 0.018(5) 0.001(5) N12 0.033(6) 0.071(9) 0.038(6) 0.009(6) 0.017(5) -0.003(6) C1 0.036(7) 0.047(8) 0.042(8) -0.010(6) 0.017(6) -0.004(6) C2 0.033(7) 0.057(9) 0.045(8) -0.012(7) 0.015(6) -0.005(6) C3 0.037(7) 0.061(9) 0.044(8) 0.002(7) 0.010(6) -0.001(6) C4 0.035(7) 0.047(8) 0.063(9) -0.001(7) 0.026(7) 0.001(6) C5 0.032(6) 0.069(10) 0.038(8) -0.018(7) 0.016(6) -0.005(7) C6 0.034(6) 0.057(9) 0.036(7) -0.011(6) 0.017(6) -0.003(6) C7 0.043(8) 0.060(9) 0.037(8) -0.012(6) 0.020(6) -0.016(7) C8 0.046(7) 0.048(8) 0.048(8) 0.004(6) 0.024(7) 0.000(6) C9 0.083(10) 0.051(9) 0.042(8) 0.010(7) 0.039(8) -0.013(8) C10 0.050(8) 0.056(9) 0.052(9) 0.018(7) 0.016(7) 0.011(7) C11 0.048(8) 0.045(8) 0.063(10) 0.008(7) 0.018(7) -0.006(7) C12 0.057(8) 0.045(8) 0.034(7) -0.005(6) 0.024(6) -0.010(6) C13 0.058(8) 0.042(8) 0.045(8) -0.010(6) 0.026(7) -0.009(6) C14 0.036(7) 0.059(9) 0.050(9) -0.016(7) 0.018(6) -0.012(6) C15 0.051(8) 0.042(8) 0.045(8) -0.009(6) 0.027(7) -0.006(6) C16 0.027(6) 0.056(8) 0.031(7) -0.013(6) 0.010(5) -0.004(6) C17 0.025(6) 0.051(8) 0.032(7) 0.000(6) 0.007(5) -0.003(5) C18 0.048(8) 0.052(9) 0.040(8) -0.002(6) 0.026(6) -0.010(7) C19 0.041(7) 0.073(10) 0.051(9) 0.027(7) 0.016(7) 0.012(7) C20 0.066(10) 0.104(14) 0.068(11) 0.043(10) 0.028(9) 0.004(10) C21 0.072(10) 0.084(12) 0.069(11) 0.042(9) 0.031(9) 0.024(9) C22 0.050(8) 0.069(10) 0.038(8) 0.018(7) 0.021(7) 0.024(7) C23 0.025(6) 0.087(11) 0.052(9) -0.003(8) 0.017(6) -0.007(7) C27 0.068(9) 0.048(8) 0.047(8) -0.022(6) 0.036(7) -0.011(7) C31 0.041(7) 0.073(10) 0.039(8) -0.004(7) 0.025(6) -0.009(7) C32 0.027(6) 0.070(10) 0.055(9) 0.001(7) 0.026(6) -0.001(6) C33 0.054(8) 0.089(12) 0.044(9) -0.019(8) 0.035(7) -0.017(8) C34 0.065(10) 0.081(12) 0.038(8) 0.007(8) 0.028(7) 0.001(8) C35 0.089(12) 0.084(12) 0.037(8) -0.003(8) 0.027(8) -0.044(10) C36 0.050(8) 0.050(9) 0.058(9) -0.005(7) 0.024(7) -0.017(7) C37 0.073(10) 0.050(10) 0.063(11) 0.005(8) 0.020(9) 0.005(8) C38 0.122(16) 0.063(12) 0.102(16) 0.001(11) 0.047(14) 0.024(11) C39 0.087(11) 0.045(9) 0.068(11) 0.009(8) 0.027(9) 0.005(8) C40 0.112(13) 0.044(9) 0.077(11) 0.009(8) 0.062(11) 0.010(9) C41 0.139(17) 0.031(9) 0.110(15) -0.030(9) 0.106(15) -0.029(10) C42 0.065(9) 0.058(10) 0.056(9) -0.018(7) 0.045(8) -0.033(8) C43 0.076(11) 0.078(12) 0.079(12) -0.013(9) 0.058(10) -0.019(10) C44 0.063(10) 0.105(14) 0.055(10) -0.046(9) 0.031(8) -0.040(10) C45 0.052(9) 0.086(12) 0.060(10) -0.029(9) 0.031(8) -0.004(8) C46 0.042(7) 0.052(8) 0.036(7) -0.008(6) 0.027(6) -0.014(6) C47 0.040(7) 0.054(8) 0.037(7) -0.003(6) 0.022(6) -0.004(6) C48 0.032(7) 0.098(13) 0.036(8) -0.011(8) 0.018(6) -0.012(7) C49 0.047(8) 0.057(10) 0.055(9) -0.002(7) 0.015(7) 0.005(7) C50 0.045(8) 0.046(8) 0.064(10) -0.010(7) 0.014(7) -0.005(7) C51 0.053(9) 0.078(12) 0.060(10) -0.024(8) 0.026(8) -0.008(8) C52 0.038(7) 0.088(12) 0.034(8) -0.028(7) 0.020(6) -0.009(7) C53 0.092(13) 0.086(13) 0.070(12) 0.013(9) 0.039(10) 0.002(10) C57 0.094(14) 0.17(2) 0.113(17) -0.100(16) 0.071(13) -0.087(15) C61 0.061(9) 0.052(9) 0.036(7) -0.021(6) 0.028(7) -0.010(7) C62 0.069(10) 0.078(11) 0.033(8) -0.005(7) 0.021(7) -0.010(9) C63 0.081(11) 0.061(11) 0.045(9) -0.023(8) 0.022(8) -0.032(9) C64 0.106(15) 0.053(11) 0.064(11) -0.023(9) 0.042(11) -0.031(10) C65 0.127(16) 0.029(8) 0.085(12) -0.003(8) 0.059(12) -0.002(9) C66 0.080(11) 0.040(8) 0.061(10) -0.009(7) 0.043(9) -0.007(8) C67 0.076(12) 0.059(11) 0.086(13) 0.024(10) 0.047(10) 0.035(10) C68 0.050(9) 0.084(13) 0.086(13) 0.028(10) 0.014(9) 0.022(9) C69 0.051(9) 0.080(12) 0.079(12) 0.021(9) 0.034(8) 0.019(8) C70 0.042(8) 0.079(12) 0.060(10) 0.006(8) 0.011(7) 0.016(8) C71 0.030(6) 0.056(9) 0.037(7) -0.007(6) 0.009(6) -0.003(6) C72 0.034(6) 0.059(9) 0.032(7) -0.011(6) 0.013(6) -0.012(6) C73 0.048(8) 0.062(9) 0.040(8) -0.001(7) 0.025(7) -0.004(7) C74 0.055(8) 0.055(9) 0.032(7) -0.014(6) 0.021(7) -0.013(7) C75 0.062(9) 0.046(8) 0.024(7) 0.001(6) 0.010(6) -0.007(7) C76 0.041(7) 0.035(7) 0.045(8) -0.003(6) 0.024(6) -0.010(6) C77 0.038(6) 0.037(7) 0.030(7) -0.005(5) 0.019(6) -0.007(5) C78 0.053(8) 0.049(9) 0.042(8) 0.011(6) 0.014(7) 0.002(7) C79 0.043(8) 0.065(10) 0.091(12) 0.019(9) 0.036(8) 0.021(7) C80 0.045(8) 0.071(11) 0.061(10) 0.008(8) 0.018(7) 0.018(8) C81 0.054(9) 0.090(12) 0.044(9) 0.009(8) 0.022(7) 0.010(8) C82 0.045(8) 0.083(12) 0.030(7) -0.013(7) 0.012(6) -0.025(8) C83 0.15(2) 0.078(14) 0.086(14) -0.004(11) 0.047(14) 0.000(13) C87 0.053(8) 0.077(11) 0.028(7) 0.007(7) 0.012(6) -0.012(7) O100 0.057(7) 0.089(9) 0.141(12) 0.063(9) 0.022(7) 0.006(7) O101 0.089(8) 0.077(7) 0.053(6) 0.011(5) 0.043(6) 0.028(6) O102 0.179(13) 0.046(7) 0.045(7) -0.003(5) -0.007(8) 0.012(8) _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 N3 2.038(10) . ? Zn1 N4 2.086(12) . ? Zn1 O100 2.152(16) . ? Zn1 S1 2.364(4) . ? Zn1 S2 2.695(4) . ? Zn2 N2 2.013(10) . ? Zn2 N1 2.105(9) . ? Zn2 S1 2.346(3) . ? Zn2 S6 2.349(3) . ? Zn2 S2 2.739(3) . ? Zn3 N6 1.944(15) . ? Zn3 O101 2.056(12) . ? Zn3 N5 2.083(12) . ? Zn3 S3 2.343(3) . ? Zn3 S4 2.749(4) . ? Zn4 N7 2.064(11) . ? Zn4 N8 2.088(10) . ? Zn4 S3 2.334(4) . ? Zn4 S2 2.351(3) . ? Zn4 S4 2.704(3) . ? Zn5 N10 2.019(11) . ? Zn5 O102 2.024(14) . ? Zn5 N9 2.082(12) . ? Zn5 S5 2.356(4) . ? Zn5 S6 2.643(4) . ? Zn6 N11 2.005(11) . ? Zn6 N12 2.080(11) . ? Zn6 S4 2.321(3) . ? Zn6 S5 2.328(3) . ? Zn6 S6 2.743(3) . ? S1 C1 1.779(12) . ? S2 C17 1.773(13) . ? S3 C31 1.791(13) . ? S4 C47 1.788(12) . ? S5 C61 1.752(14) . ? S6 C77 1.774(11) . ? N1 C7 1.242(16) . ? N1 C8 1.483(16) . ? N2 C11 1.263(16) . ? N2 C10 1.488(16) . ? N3 C18 1.311(16) . ? N3 C19 1.474(16) . ? N4 C22 1.295(16) . ? N4 C21 1.511(17) . ? N5 C37 1.241(18) . ? N5 C38 1.47(2) . ? N6 C41 1.28(2) . ? N6 C40 1.474(19) . ? N7 C48 1.272(16) . ? N7 C49 1.445(17) . ? N8 C52 1.303(17) . ? N8 C51 1.478(19) . ? N9 C67 1.24(2) . ? N9 C68 1.453(18) . ? N10 C71 1.282(16) . ? N10 C70 1.455(17) . ? N11 C78 1.291(16) . ? N11 C79 1.484(16) . ? N12 C82 1.288(18) . ? N12 C81 1.486(18) . ? C1 C2 1.379(18) . ? C1 C6 1.392(17) . ? C2 C3 1.379(17) . ? C2 C22 1.477(18) . ? C3 C4 1.417(17) . ? C3 H3A 0.9500 . ? C4 C5 1.373(18) . ? C4 C23 1.525(9) . ? C5 C6 1.423(16) . ? C5 H5A 0.9500 . ? C6 C7 1.484(19) . ? C7 H7A 0.9500 . ? C8 C9 1.500(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.604(19) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.492(18) . ? C11 H11A 0.9500 . ? C12 C13 1.401(17) . ? C12 C17 1.402(17) . ? C13 C14 1.383(17) . ? C13 H13A 0.9500 . ? C14 C15 1.418(18) . ? C14 C27 1.516(9) . ? C15 C16 1.409(17) . ? C15 H15A 0.9500 . ? C16 C17 1.416(16) . ? C16 C18 1.458(18) . ? C18 H18A 0.9500 . ? C19 C20 1.52(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.41(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9500 . ? C23 C25A 1.505(10) . ? C23 C24A 1.507(10) . ? C23 C25 1.515(11) . ? C23 C26A 1.521(10) . ? C23 C24 1.521(11) . ? C23 C26 1.522(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C27 C30 1.511(10) . ? C27 C28 1.524(10) . ? C27 C29 1.524(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.387(19) . ? C31 C36 1.40(2) . ? C32 C33 1.398(19) . ? C32 C52 1.44(2) . ? C33 C34 1.36(2) . ? C33 H33A 0.9500 . ? C34 C35 1.39(2) . ? C34 C53 1.511(10) . ? C35 C36 1.398(19) . ? C35 H35A 0.9500 . ? C36 C37 1.48(2) . ? C37 H37A 0.9500 . ? C38 C39 1.48(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.50(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.56(3) . ? C41 H41A 0.9500 . ? C42 C43 1.37(2) . ? C42 C47 1.406(18) . ? C43 C44 1.42(2) . ? C43 H43A 0.9500 . ? C44 C45 1.40(2) . ? C44 C57 1.510(10) . ? C45 C46 1.423(19) . ? C45 H45A 0.9500 . ? C46 C47 1.387(18) . ? C46 C48 1.44(2) . ? C48 H48A 0.9500 . ? C49 C50 1.583(19) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.46(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9500 . ? C53 C54 1.512(10) . ? C53 C55 1.512(10) . ? C53 C56 1.518(10) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C59 1.504(10) . ? C57 C59A 1.507(11) . ? C57 C60 1.511(10) . ? C57 C60A 1.512(10) . ? C57 C58 1.537(11) . ? C57 C58A 1.538(11) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? C59A H59D 0.9800 . ? C59A H59E 0.9800 . ? C59A H59F 0.9800 . ? C60A H60D 0.9800 . ? C60A H60E 0.9800 . ? C60A H60F 0.9800 . ? C61 C62 1.41(2) . ? C61 C66 1.43(2) . ? C62 C63 1.43(2) . ? C62 C82 1.47(2) . ? C63 C64 1.31(2) . ? C63 H63A 0.9500 . ? C64 C65 1.38(2) . ? C64 C83 1.527(10) . ? C65 C66 1.42(2) . ? C65 H65A 0.9500 . ? C66 C67 1.44(2) . ? C67 H67A 0.9500 . ? C68 C69 1.56(2) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.47(2) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.465(18) . ? C71 H71A 0.9500 . ? C72 C77 1.402(16) . ? C72 C73 1.418(16) . ? C73 C74 1.400(18) . ? C73 H73A 0.9500 . ? C74 C75 1.398(18) . ? C74 C87 1.519(9) . ? C75 C76 1.417(16) . ? C75 H75A 0.9500 . ? C76 C77 1.422(17) . ? C76 C78 1.463(18) . ? C78 H78A 0.9500 . ? C79 C80 1.52(2) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.48(2) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9500 . ? C83 C86 1.511(10) . ? C83 C85 1.511(10) . ? C83 C84 1.515(10) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.517(10) . ? C87 C90 1.523(9) . ? C87 C89 1.527(9) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C100 O102 1.240(16) . ? C100 O100 1.254(16) . ? C100 O101 1.260(15) . ? Cl1 O1B 1.391(10) . ? Cl1 O1D 1.391(10) . ? Cl1 O1A 1.394(11) . ? Cl1 O1C 1.396(10) . ? Cl2 O2D 1.370(11) . ? Cl2 O2B 1.375(10) . ? Cl2 O2C 1.393(11) . ? Cl2 O2A 1.441(11) . ? Cl3 O3A 1.347(10) . ? Cl3 O3D 1.367(10) . ? Cl3 O3C 1.411(11) . ? Cl3 O3B 1.442(11) . ? Cl4 O4A 1.367(10) . ? Cl4 O4B 1.384(11) . ? Cl4 O4C 1.402(11) . ? Cl4 O4D 1.417(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 N4 91.4(4) . . ? N3 Zn1 O100 143.9(4) . . ? N4 Zn1 O100 95.1(4) . . ? N3 Zn1 S1 118.1(3) . . ? N4 Zn1 S1 89.4(3) . . ? O100 Zn1 S1 97.5(3) . . ? N3 Zn1 S2 84.0(3) . . ? N4 Zn1 S2 167.3(4) . . ? O100 Zn1 S2 95.6(3) . . ? S1 Zn1 S2 82.33(11) . . ? N2 Zn2 N1 95.7(4) . . ? N2 Zn2 S1 112.8(3) . . ? N1 Zn2 S1 91.0(3) . . ? N2 Zn2 S6 112.5(3) . . ? N1 Zn2 S6 103.0(3) . . ? S1 Zn2 S6 130.61(13) . . ? N2 Zn2 S2 82.8(3) . . ? N1 Zn2 S2 171.2(3) . . ? S1 Zn2 S2 81.68(10) . . ? S6 Zn2 S2 85.53(10) . . ? N6 Zn3 O101 135.6(5) . . ? N6 Zn3 N5 93.1(5) . . ? O101 Zn3 N5 94.8(4) . . ? N6 Zn3 S3 116.2(4) . . ? O101 Zn3 S3 107.1(3) . . ? N5 Zn3 S3 91.8(3) . . ? N6 Zn3 S4 84.1(4) . . ? O101 Zn3 S4 95.3(3) . . ? N5 Zn3 S4 168.0(3) . . ? S3 Zn3 S4 79.02(11) . . ? N7 Zn4 N8 93.7(4) . . ? N7 Zn4 S3 112.2(3) . . ? N8 Zn4 S3 90.9(3) . . ? N7 Zn4 S2 115.0(3) . . ? N8 Zn4 S2 106.3(3) . . ? S3 Zn4 S2 128.02(13) . . ? N7 Zn4 S4 82.5(3) . . ? N8 Zn4 S4 168.0(3) . . ? S3 Zn4 S4 80.13(11) . . ? S2 Zn4 S4 85.65(10) . . ? N10 Zn5 O102 131.6(5) . . ? N10 Zn5 N9 92.4(5) . . ? O102 Zn5 N9 91.9(5) . . ? N10 Zn5 S5 115.2(3) . . ? O102 Zn5 S5 113.0(4) . . ? N9 Zn5 S5 89.5(4) . . ? N10 Zn5 S6 84.7(3) . . ? O102 Zn5 S6 98.3(3) . . ? N9 Zn5 S6 168.7(4) . . ? S5 Zn5 S6 81.94(12) . . ? N11 Zn6 N12 94.3(4) . . ? N11 Zn6 S4 117.3(3) . . ? N12 Zn6 S4 104.1(3) . . ? N11 Zn6 S5 115.4(3) . . ? N12 Zn6 S5 91.7(3) . . ? S4 Zn6 S5 123.07(13) . . ? N11 Zn6 S6 82.7(3) . . ? N12 Zn6 S6 169.2(3) . . ? S4 Zn6 S6 86.42(11) . . ? S5 Zn6 S6 80.30(11) . . ? C1 S1 Zn2 102.0(4) . . ? C1 S1 Zn1 101.0(4) . . ? Zn2 S1 Zn1 95.05(13) . . ? C17 S2 Zn4 106.8(4) . . ? C17 S2 Zn1 91.9(4) . . ? Zn4 S2 Zn1 118.90(13) . . ? C17 S2 Zn2 94.4(4) . . ? Zn4 S2 Zn2 150.61(14) . . ? Zn1 S2 Zn2 79.46(9) . . ? C31 S3 Zn4 105.4(5) . . ? C31 S3 Zn3 104.1(5) . . ? Zn4 S3 Zn3 97.05(12) . . ? C47 S4 Zn6 104.4(4) . . ? C47 S4 Zn4 94.1(4) . . ? Zn6 S4 Zn4 142.93(15) . . ? C47 S4 Zn3 92.8(4) . . ? Zn6 S4 Zn3 129.71(14) . . ? Zn4 S4 Zn3 79.97(9) . . ? C61 S5 Zn6 102.8(4) . . ? C61 S5 Zn5 104.1(5) . . ? Zn6 S5 Zn5 95.56(12) . . ? C77 S6 Zn2 105.7(4) . . ? C77 S6 Zn5 94.2(4) . . ? Zn2 S6 Zn5 125.39(14) . . ? C77 S6 Zn6 94.2(4) . . ? Zn2 S6 Zn6 145.04(13) . . ? Zn5 S6 Zn6 80.17(10) . . ? C7 N1 C8 119.7(10) . . ? C7 N1 Zn2 124.1(9) . . ? C8 N1 Zn2 116.1(8) . . ? C11 N2 C10 115.3(11) . . ? C11 N2 Zn2 129.4(9) . . ? C10 N2 Zn2 115.1(8) . . ? C18 N3 C19 117.8(11) . . ? C18 N3 Zn1 127.3(8) . . ? C19 N3 Zn1 114.7(9) . . ? C22 N4 C21 115.9(12) . . ? C22 N4 Zn1 125.4(9) . . ? C21 N4 Zn1 118.3(9) . . ? C37 N5 C38 119.1(14) . . ? C37 N5 Zn3 126.5(11) . . ? C38 N5 Zn3 114.4(11) . . ? C41 N6 C40 113.3(15) . . ? C41 N6 Zn3 128.4(12) . . ? C40 N6 Zn3 117.9(12) . . ? C48 N7 C49 120.2(12) . . ? C48 N7 Zn4 127.4(10) . . ? C49 N7 Zn4 111.9(9) . . ? C52 N8 C51 120.0(11) . . ? C52 N8 Zn4 124.3(9) . . ? C51 N8 Zn4 115.7(9) . . ? C67 N9 C68 117.1(14) . . ? C67 N9 Zn5 124.8(10) . . ? C68 N9 Zn5 117.3(11) . . ? C71 N10 C70 118.2(11) . . ? C71 N10 Zn5 127.4(9) . . ? C70 N10 Zn5 114.1(9) . . ? C78 N11 C79 116.7(11) . . ? C78 N11 Zn6 128.4(9) . . ? C79 N11 Zn6 114.1(8) . . ? C82 N12 C81 118.0(13) . . ? C82 N12 Zn6 124.4(10) . . ? C81 N12 Zn6 117.6(10) . . ? C2 C1 C6 118.3(11) . . ? C2 C1 S1 120.3(9) . . ? C6 C1 S1 120.9(10) . . ? C3 C2 C1 120.5(12) . . ? C3 C2 C22 110.4(12) . . ? C1 C2 C22 129.0(11) . . ? C2 C3 C4 123.9(13) . . ? C2 C3 H3A 118.1 . . ? C4 C3 H3A 118.1 . . ? C5 C4 C3 114.1(10) . . ? C5 C4 C23 123.4(11) . . ? C3 C4 C23 122.6(12) . . ? C4 C5 C6 123.6(12) . . ? C4 C5 H5A 118.2 . . ? C6 C5 H5A 118.2 . . ? C1 C6 C5 119.6(13) . . ? C1 C6 C7 127.7(11) . . ? C5 C6 C7 112.7(11) . . ? N1 C7 C6 128.8(11) . . ? N1 C7 H7A 115.6 . . ? C6 C7 H7A 115.6 . . ? N1 C8 C9 113.5(10) . . ? N1 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 113.9(11) . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N2 C10 C9 108.2(10) . . ? N2 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? N2 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N2 C11 C12 128.1(13) . . ? N2 C11 H11A 115.9 . . ? C12 C11 H11A 115.9 . . ? C13 C12 C17 120.6(11) . . ? C13 C12 C11 113.2(12) . . ? C17 C12 C11 126.1(11) . . ? C14 C13 C12 122.9(12) . . ? C14 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C13 C14 C15 117.0(10) . . ? C13 C14 C27 124.6(12) . . ? C15 C14 C27 118.4(11) . . ? C16 C15 C14 120.5(12) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 121.5(12) . . ? C15 C16 C18 112.4(11) . . ? C17 C16 C18 126.0(11) . . ? C12 C17 C16 117.1(11) . . ? C12 C17 S2 120.4(9) . . ? C16 C17 S2 122.1(10) . . ? N3 C18 C16 126.4(11) . . ? N3 C18 H18A 116.8 . . ? C16 C18 H18A 116.8 . . ? N3 C19 C20 109.8(11) . . ? N3 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? N3 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C21 C20 C19 119.2(15) . . ? C21 C20 H20A 107.5 . . ? C19 C20 H20A 107.5 . . ? C21 C20 H20B 107.5 . . ? C19 C20 H20B 107.5 . . ? H20A C20 H20B 107.0 . . ? C20 C21 N4 116.0(13) . . ? C20 C21 H21A 108.3 . . ? N4 C21 H21A 108.3 . . ? C20 C21 H21B 108.3 . . ? N4 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? N4 C22 C2 126.0(12) . . ? N4 C22 H22A 117.0 . . ? C2 C22 H22A 117.0 . . ? C25A C23 C24A 110.5(9) . . ? C25A C23 C26A 109.1(9) . . ? C24A C23 C26A 109.5(9) . . ? C25 C23 C24 108.8(9) . . ? C25 C23 C26 108.3(9) . . ? C24 C23 C26 108.2(9) . . ? C25A C23 C4 107.2(15) . . ? C24A C23 C4 109.1(14) . . ? C25 C23 C4 111.4(17) . . ? C26A C23 C4 111.5(15) . . ? C24 C23 C4 107.8(17) . . ? C26 C23 C4 112.3(16) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C24A H24D 109.5 . . ? C23 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C23 C25A H25D 109.5 . . ? C23 C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? C23 C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C23 C26A H26D 109.5 . . ? C23 C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C23 C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C30 C27 C14 112.3(13) . . ? C30 C27 C28 108.6(8) . . ? C14 C27 C28 108.2(12) . . ? C30 C27 C29 108.8(8) . . ? C14 C27 C29 110.8(14) . . ? C28 C27 C29 108.0(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 119.8(13) . . ? C32 C31 S3 120.1(12) . . ? C36 C31 S3 119.8(11) . . ? C31 C32 C33 118.1(14) . . ? C31 C32 C52 127.9(13) . . ? C33 C32 C52 114.0(13) . . ? C34 C33 C32 124.7(14) . . ? C34 C33 H33A 117.7 . . ? C32 C33 H33A 117.7 . . ? C33 C34 C35 115.5(12) . . ? C33 C34 C53 123.9(14) . . ? C35 C34 C53 120.6(14) . . ? C34 C35 C36 123.1(16) . . ? C34 C35 H35A 118.4 . . ? C36 C35 H35A 118.4 . . ? C35 C36 C31 118.6(14) . . ? C35 C36 C37 112.2(14) . . ? C31 C36 C37 129.2(13) . . ? N5 C37 C36 128.9(15) . . ? N5 C37 H37A 115.6 . . ? C36 C37 H37A 115.6 . . ? N5 C38 C39 115.7(16) . . ? N5 C38 H38A 108.3 . . ? C39 C38 H38A 108.3 . . ? N5 C38 H38B 108.3 . . ? C39 C38 H38B 108.3 . . ? H38A C38 H38B 107.4 . . ? C38 C39 C40 115.5(16) . . ? C38 C39 H39A 108.4 . . ? C40 C39 H39A 108.4 . . ? C38 C39 H39B 108.4 . . ? C40 C39 H39B 108.4 . . ? H39A C39 H39B 107.5 . . ? N6 C40 C39 108.9(12) . . ? N6 C40 H40A 109.9 . . ? C39 C40 H40A 109.9 . . ? N6 C40 H40B 109.9 . . ? C39 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? N6 C41 C42 129.1(14) . . ? N6 C41 H41A 115.4 . . ? C42 C41 H41A 115.4 . . ? C43 C42 C47 122.7(15) . . ? C43 C42 C41 113.7(14) . . ? C47 C42 C41 123.6(13) . . ? C42 C43 C44 120.4(15) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C45 C44 C43 117.2(12) . . ? C45 C44 C57 121.2(16) . . ? C43 C44 C57 121.5(15) . . ? C44 C45 C46 121.6(14) . . ? C44 C45 H45A 119.2 . . ? C46 C45 H45A 119.2 . . ? C47 C46 C45 119.8(13) . . ? C47 C46 C48 127.6(12) . . ? C45 C46 C48 112.6(12) . . ? C46 C47 C42 117.9(12) . . ? C46 C47 S4 120.5(10) . . ? C42 C47 S4 121.2(10) . . ? N7 C48 C46 128.9(14) . . ? N7 C48 H48A 115.6 . . ? C46 C48 H48A 115.6 . . ? N7 C49 C50 113.8(11) . . ? N7 C49 H49A 108.8 . . ? C50 C49 H49A 108.8 . . ? N7 C49 H49B 108.8 . . ? C50 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? C51 C50 C49 114.7(11) . . ? C51 C50 H50A 108.6 . . ? C49 C50 H50A 108.6 . . ? C51 C50 H50B 108.6 . . ? C49 C50 H50B 108.6 . . ? H50A C50 H50B 107.6 . . ? C50 C51 N8 113.8(12) . . ? C50 C51 H51A 108.8 . . ? N8 C51 H51A 108.8 . . ? C50 C51 H51B 108.8 . . ? N8 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? N8 C52 C32 131.2(11) . . ? N8 C52 H52A 114.4 . . ? C32 C52 H52A 114.4 . . ? C34 C53 C54 113.7(15) . . ? C34 C53 C55 107.8(15) . . ? C54 C53 C55 109.9(9) . . ? C34 C53 C56 107.6(14) . . ? C54 C53 C56 108.4(8) . . ? C55 C53 C56 109.4(9) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C59 C57 C44 119.7(18) . . ? C59A C57 C44 117.8(19) . . ? C59 C57 C60 110.6(9) . . ? C44 C57 C60 110.8(16) . . ? C59A C57 C60A 110.5(9) . . ? C44 C57 C60A 114.8(16) . . ? C59 C57 C58 107.8(9) . . ? C44 C57 C58 99(2) . . ? C60 C57 C58 107.6(9) . . ? C59A C57 C58A 107.7(9) . . ? C44 C57 C58A 97(2) . . ? C60A C57 C58A 107.1(9) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C57 C58A H58D 109.5 . . ? C57 C58A H58E 109.5 . . ? H58D C58A H58E 109.5 . . ? C57 C58A H58F 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? C57 C59A H59D 109.5 . . ? C57 C59A H59E 109.5 . . ? H59D C59A H59E 109.5 . . ? C57 C59A H59F 109.5 . . ? H59D C59A H59F 109.5 . . ? H59E C59A H59F 109.5 . . ? C57 C60A H60D 109.5 . . ? C57 C60A H60E 109.5 . . ? H60D C60A H60E 109.5 . . ? C57 C60A H60F 109.5 . . ? H60D C60A H60F 109.5 . . ? H60E C60A H60F 109.5 . . ? C62 C61 C66 117.5(13) . . ? C62 C61 S5 121.9(12) . . ? C66 C61 S5 119.9(11) . . ? C61 C62 C63 118.6(15) . . ? C61 C62 C82 126.4(14) . . ? C63 C62 C82 114.9(14) . . ? C64 C63 C62 126.2(16) . . ? C64 C63 H63A 116.9 . . ? C62 C63 H63A 116.9 . . ? C63 C64 C65 114.3(13) . . ? C63 C64 C83 125.5(17) . . ? C65 C64 C83 120.1(17) . . ? C64 C65 C66 126.1(16) . . ? C64 C65 H65A 116.9 . . ? C66 C65 H65A 116.9 . . ? C65 C66 C61 117.2(15) . . ? C65 C66 C67 116.5(16) . . ? C61 C66 C67 126.0(14) . . ? N9 C67 C66 132.9(15) . . ? N9 C67 H67A 113.6 . . ? C66 C67 H67A 113.6 . . ? N9 C68 C69 110.5(13) . . ? N9 C68 H68A 109.6 . . ? C69 C68 H68A 109.6 . . ? N9 C68 H68B 109.6 . . ? C69 C68 H68B 109.6 . . ? H68A C68 H68B 108.1 . . ? C70 C69 C68 116.2(13) . . ? C70 C69 H69A 108.2 . . ? C68 C69 H69A 108.2 . . ? C70 C69 H69B 108.2 . . ? C68 C69 H69B 108.2 . . ? H69A C69 H69B 107.4 . . ? N10 C70 C69 113.8(13) . . ? N10 C70 H70A 108.8 . . ? C69 C70 H70A 108.8 . . ? N10 C70 H70B 108.8 . . ? C69 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? N10 C71 C72 128.1(11) . . ? N10 C71 H71A 116.0 . . ? C72 C71 H71A 116.0 . . ? C77 C72 C73 121.1(12) . . ? C77 C72 C71 125.6(11) . . ? C73 C72 C71 113.3(11) . . ? C74 C73 C72 121.7(12) . . ? C74 C73 H73A 119.2 . . ? C72 C73 H73A 119.2 . . ? C75 C74 C73 116.9(10) . . ? C75 C74 C87 121.3(12) . . ? C73 C74 C87 121.7(11) . . ? C74 C75 C76 122.7(12) . . ? C74 C75 H75A 118.7 . . ? C76 C75 H75A 118.7 . . ? C75 C76 C77 119.7(11) . . ? C75 C76 C78 113.3(12) . . ? C77 C76 C78 126.8(10) . . ? C72 C77 C76 117.7(10) . . ? C72 C77 S6 122.2(10) . . ? C76 C77 S6 119.9(8) . . ? N11 C78 C76 128.4(12) . . ? N11 C78 H78A 115.8 . . ? C76 C78 H78A 115.8 . . ? N11 C79 C80 112.9(12) . . ? N11 C79 H79A 109.0 . . ? C80 C79 H79A 109.0 . . ? N11 C79 H79B 109.0 . . ? C80 C79 H79B 109.0 . . ? H79A C79 H79B 107.8 . . ? C81 C80 C79 115.6(13) . . ? C81 C80 H80A 108.4 . . ? C79 C80 H80A 108.4 . . ? C81 C80 H80B 108.4 . . ? C79 C80 H80B 108.4 . . ? H80A C80 H80B 107.5 . . ? C80 C81 N12 113.5(12) . . ? C80 C81 H81A 108.9 . . ? N12 C81 H81A 108.9 . . ? C80 C81 H81B 108.9 . . ? N12 C81 H81B 108.9 . . ? H81A C81 H81B 107.7 . . ? N12 C82 C62 129.2(13) . . ? N12 C82 H82A 115.4 . . ? C62 C82 H82A 115.4 . . ? C86 C83 C85 109.9(9) . . ? C86 C83 C84 109.0(9) . . ? C85 C83 C84 109.0(9) . . ? C86 C83 C64 111.7(15) . . ? C85 C83 C64 108.6(16) . . ? C84 C83 C64 108.5(15) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C83 C85 H85A 109.5 . . ? C83 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C83 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C83 C86 H86A 109.5 . . ? C83 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C83 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 C74 106.9(11) . . ? C88 C87 C90 108.6(8) . . ? C74 C87 C90 111.5(10) . . ? C88 C87 C89 108.3(7) . . ? C74 C87 C89 113.9(11) . . ? C90 C87 C89 107.5(7) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? O102 C100 O100 118.8(15) . . ? O102 C100 O101 120.8(14) . . ? O100 C100 O101 118.5(14) . . ? C100 O100 Zn1 102.9(10) . . ? C100 O101 Zn3 108.9(9) . . ? C100 O102 Zn5 114.8(11) . . ? O1B Cl1 O1D 110.5(8) . . ? O1B Cl1 O1A 109.1(8) . . ? O1D Cl1 O1A 109.4(8) . . ? O1B Cl1 O1C 109.1(8) . . ? O1D Cl1 O1C 109.4(8) . . ? O1A Cl1 O1C 109.3(8) . . ? O2D Cl2 O2B 113.3(8) . . ? O2D Cl2 O2C 111.4(8) . . ? O2B Cl2 O2C 111.0(8) . . ? O2D Cl2 O2A 107.3(8) . . ? O2B Cl2 O2A 107.0(8) . . ? O2C Cl2 O2A 106.4(8) . . ? O3A Cl3 O3D 116.5(8) . . ? O3A Cl3 O3C 111.0(8) . . ? O3D Cl3 O3C 109.9(8) . . ? O3A Cl3 O3B 107.3(8) . . ? O3D Cl3 O3B 107.3(8) . . ? O3C Cl3 O3B 104.0(7) . . ? O4A Cl4 O4B 113.0(8) . . ? O4A Cl4 O4C 111.1(8) . . ? O4B Cl4 O4C 109.4(8) . . ? O4A Cl4 O4D 109.2(8) . . ? O4B Cl4 O4D 107.5(8) . . ? O4C Cl4 O4D 106.5(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn2 S1 C1 142.8(5) . . . . ? N1 Zn2 S1 C1 46.2(5) . . . . ? S6 Zn2 S1 C1 -61.9(5) . . . . ? S2 Zn2 S1 C1 -138.7(4) . . . . ? N2 Zn2 S1 Zn1 -114.8(3) . . . . ? N1 Zn2 S1 Zn1 148.6(3) . . . . ? S6 Zn2 S1 Zn1 40.43(17) . . . . ? S2 Zn2 S1 Zn1 -36.32(11) . . . . ? N3 Zn1 S1 C1 -140.8(6) . . . . ? N4 Zn1 S1 C1 -49.5(5) . . . . ? O100 Zn1 S1 C1 45.6(5) . . . . ? S2 Zn1 S1 C1 140.2(4) . . . . ? N3 Zn1 S1 Zn2 116.0(4) . . . . ? N4 Zn1 S1 Zn2 -152.8(3) . . . . ? O100 Zn1 S1 Zn2 -57.7(3) . . . . ? S2 Zn1 S1 Zn2 36.95(10) . . . . ? N7 Zn4 S2 C17 -87.7(5) . . . . ? N8 Zn4 S2 C17 14.4(6) . . . . ? S3 Zn4 S2 C17 118.8(4) . . . . ? S4 Zn4 S2 C17 -167.3(4) . . . . ? N7 Zn4 S2 Zn1 170.3(3) . . . . ? N8 Zn4 S2 Zn1 -87.6(4) . . . . ? S3 Zn4 S2 Zn1 16.9(2) . . . . ? S4 Zn4 S2 Zn1 90.73(14) . . . . ? N7 Zn4 S2 Zn2 46.7(5) . . . . ? N8 Zn4 S2 Zn2 148.8(4) . . . . ? S3 Zn4 S2 Zn2 -106.8(3) . . . . ? S4 Zn4 S2 Zn2 -32.9(3) . . . . ? N3 Zn1 S2 C17 -56.8(5) . . . . ? N4 Zn1 S2 C17 12.6(14) . . . . ? O100 Zn1 S2 C17 159.5(5) . . . . ? S1 Zn1 S2 C17 62.7(4) . . . . ? N3 Zn1 S2 Zn4 53.7(3) . . . . ? N4 Zn1 S2 Zn4 123.0(13) . . . . ? O100 Zn1 S2 Zn4 -90.0(3) . . . . ? S1 Zn1 S2 Zn4 173.12(15) . . . . ? N3 Zn1 S2 Zn2 -150.9(3) . . . . ? N4 Zn1 S2 Zn2 -81.6(13) . . . . ? O100 Zn1 S2 Zn2 65.4(3) . . . . ? S1 Zn1 S2 Zn2 -31.44(10) . . . . ? N2 Zn2 S2 C17 55.0(5) . . . . ? S1 Zn2 S2 C17 -59.4(4) . . . . ? S6 Zn2 S2 C17 168.4(4) . . . . ? N2 Zn2 S2 Zn4 -81.6(4) . . . . ? S1 Zn2 S2 Zn4 163.9(3) . . . . ? S6 Zn2 S2 Zn4 31.8(3) . . . . ? N2 Zn2 S2 Zn1 146.2(3) . . . . ? S1 Zn2 S2 Zn1 31.76(10) . . . . ? S6 Zn2 S2 Zn1 -100.40(11) . . . . ? N7 Zn4 S3 C31 136.4(5) . . . . ? N8 Zn4 S3 C31 42.1(5) . . . . ? S2 Zn4 S3 C31 -69.5(5) . . . . ? S4 Zn4 S3 C31 -146.0(4) . . . . ? N7 Zn4 S3 Zn3 -116.8(3) . . . . ? N8 Zn4 S3 Zn3 148.9(3) . . . . ? S2 Zn4 S3 Zn3 37.30(19) . . . . ? S4 Zn4 S3 Zn3 -39.19(12) . . . . ? N6 Zn3 S3 C31 -135.8(6) . . . . ? O101 Zn3 S3 C31 54.2(6) . . . . ? N5 Zn3 S3 C31 -41.5(6) . . . . ? S4 Zn3 S3 C31 146.4(5) . . . . ? N6 Zn3 S3 Zn4 116.4(4) . . . . ? O101 Zn3 S3 Zn4 -53.7(3) . . . . ? N5 Zn3 S3 Zn4 -149.3(4) . . . . ? S4 Zn3 S3 Zn4 38.58(11) . . . . ? N11 Zn6 S4 C47 -91.3(6) . . . . ? N12 Zn6 S4 C47 11.2(6) . . . . ? S5 Zn6 S4 C47 112.8(5) . . . . ? S6 Zn6 S4 C47 -171.3(5) . . . . ? N11 Zn6 S4 Zn4 26.2(4) . . . . ? N12 Zn6 S4 Zn4 128.7(4) . . . . ? S5 Zn6 S4 Zn4 -129.7(2) . . . . ? S6 Zn6 S4 Zn4 -53.7(2) . . . . ? N11 Zn6 S4 Zn3 162.6(3) . . . . ? N12 Zn6 S4 Zn3 -94.9(4) . . . . ? S5 Zn6 S4 Zn3 6.7(2) . . . . ? S6 Zn6 S4 Zn3 82.64(17) . . . . ? N7 Zn4 S4 C47 55.0(5) . . . . ? N8 Zn4 S4 C47 -16.9(18) . . . . ? S3 Zn4 S4 C47 -59.2(4) . . . . ? S2 Zn4 S4 C47 171.0(5) . . . . ? N7 Zn4 S4 Zn6 -65.5(4) . . . . ? N8 Zn4 S4 Zn6 -137.5(17) . . . . ? S3 Zn4 S4 Zn6 -179.7(3) . . . . ? S2 Zn4 S4 Zn6 50.4(3) . . . . ? N7 Zn4 S4 Zn3 147.1(3) . . . . ? N8 Zn4 S4 Zn3 75.2(17) . . . . ? S3 Zn4 S4 Zn3 32.87(10) . . . . ? S2 Zn4 S4 Zn3 -96.94(11) . . . . ? N6 Zn3 S4 C47 -57.3(6) . . . . ? O101 Zn3 S4 C47 167.3(5) . . . . ? N5 Zn3 S4 C47 19.8(18) . . . . ? S3 Zn3 S4 C47 60.9(4) . . . . ? N6 Zn3 S4 Zn6 54.0(4) . . . . ? O101 Zn3 S4 Zn6 -81.4(3) . . . . ? N5 Zn3 S4 Zn6 131.0(17) . . . . ? S3 Zn3 S4 Zn6 172.13(19) . . . . ? N6 Zn3 S4 Zn4 -151.0(4) . . . . ? O101 Zn3 S4 Zn4 73.6(3) . . . . ? N5 Zn3 S4 Zn4 -73.9(17) . . . . ? S3 Zn3 S4 Zn4 -32.86(10) . . . . ? N11 Zn6 S5 C61 140.7(6) . . . . ? N12 Zn6 S5 C61 45.2(5) . . . . ? S4 Zn6 S5 C61 -63.0(5) . . . . ? S6 Zn6 S5 C61 -142.2(5) . . . . ? N11 Zn6 S5 Zn5 -113.5(4) . . . . ? N12 Zn6 S5 Zn5 151.0(3) . . . . ? S4 Zn6 S5 Zn5 42.84(17) . . . . ? S6 Zn6 S5 Zn5 -36.38(11) . . . . ? N10 Zn5 S5 C61 -137.3(5) . . . . ? O102 Zn5 S5 C61 46.9(6) . . . . ? N9 Zn5 S5 C61 -44.9(5) . . . . ? S6 Zn5 S5 C61 142.5(4) . . . . ? N10 Zn5 S5 Zn6 118.0(4) . . . . ? O102 Zn5 S5 Zn6 -57.8(4) . . . . ? N9 Zn5 S5 Zn6 -149.6(3) . . . . ? S6 Zn5 S5 Zn6 37.79(11) . . . . ? N2 Zn2 S6 C77 -80.7(5) . . . . ? N1 Zn2 S6 C77 21.1(5) . . . . ? S1 Zn2 S6 C77 124.0(4) . . . . ? S2 Zn2 S6 C77 -161.0(4) . . . . ? N2 Zn2 S6 Zn5 172.2(3) . . . . ? N1 Zn2 S6 Zn5 -86.0(3) . . . . ? S1 Zn2 S6 Zn5 16.9(2) . . . . ? S2 Zn2 S6 Zn5 91.92(15) . . . . ? N2 Zn2 S6 Zn6 41.6(4) . . . . ? N1 Zn2 S6 Zn6 143.4(4) . . . . ? S1 Zn2 S6 Zn6 -113.7(2) . . . . ? S2 Zn2 S6 Zn6 -38.7(2) . . . . ? N10 Zn5 S6 C77 -54.6(5) . . . . ? O102 Zn5 S6 C77 174.1(6) . . . . ? N9 Zn5 S6 C77 20.6(18) . . . . ? S5 Zn5 S6 C77 61.8(4) . . . . ? N10 Zn5 S6 Zn2 58.1(3) . . . . ? O102 Zn5 S6 Zn2 -73.3(4) . . . . ? N9 Zn5 S6 Zn2 133.3(17) . . . . ? S5 Zn5 S6 Zn2 174.50(15) . . . . ? N10 Zn5 S6 Zn6 -148.1(3) . . . . ? O102 Zn5 S6 Zn6 80.6(4) . . . . ? N9 Zn5 S6 Zn6 -72.9(17) . . . . ? S5 Zn5 S6 Zn6 -31.70(9) . . . . ? N11 Zn6 S6 C77 56.1(5) . . . . ? N12 Zn6 S6 C77 -18.5(19) . . . . ? S4 Zn6 S6 C77 174.3(4) . . . . ? S5 Zn6 S6 C77 -61.3(4) . . . . ? N11 Zn6 S6 Zn2 -69.2(4) . . . . ? N12 Zn6 S6 Zn2 -143.8(18) . . . . ? S4 Zn6 S6 Zn2 48.9(3) . . . . ? S5 Zn6 S6 Zn2 173.4(3) . . . . ? N11 Zn6 S6 Zn5 149.7(3) . . . . ? N12 Zn6 S6 Zn5 75.1(18) . . . . ? S4 Zn6 S6 Zn5 -92.15(11) . . . . ? S5 Zn6 S6 Zn5 32.28(10) . . . . ? N2 Zn2 N1 C7 -143.2(10) . . . . ? S1 Zn2 N1 C7 -30.1(10) . . . . ? S6 Zn2 N1 C7 102.1(10) . . . . ? N2 Zn2 N1 C8 34.2(9) . . . . ? S1 Zn2 N1 C8 147.3(8) . . . . ? S6 Zn2 N1 C8 -80.5(8) . . . . ? N1 Zn2 N2 C11 132.5(12) . . . . ? S1 Zn2 N2 C11 39.0(12) . . . . ? S6 Zn2 N2 C11 -120.9(11) . . . . ? S2 Zn2 N2 C11 -38.8(11) . . . . ? N1 Zn2 N2 C10 -42.0(9) . . . . ? S1 Zn2 N2 C10 -135.5(8) . . . . ? S6 Zn2 N2 C10 64.6(9) . . . . ? S2 Zn2 N2 C10 146.7(9) . . . . ? N4 Zn1 N3 C18 -127.3(11) . . . . ? O100 Zn1 N3 C18 132.1(11) . . . . ? S1 Zn1 N3 C18 -37.2(12) . . . . ? S2 Zn1 N3 C18 40.8(11) . . . . ? N4 Zn1 N3 C19 46.9(9) . . . . ? O100 Zn1 N3 C19 -53.8(12) . . . . ? S1 Zn1 N3 C19 137.0(8) . . . . ? S2 Zn1 N3 C19 -145.0(9) . . . . ? N3 Zn1 N4 C22 151.9(12) . . . . ? O100 Zn1 N4 C22 -63.6(13) . . . . ? S1 Zn1 N4 C22 33.9(12) . . . . ? S2 Zn1 N4 C22 83.4(18) . . . . ? N3 Zn1 N4 C21 -35.1(11) . . . . ? O100 Zn1 N4 C21 109.3(11) . . . . ? S1 Zn1 N4 C21 -153.2(11) . . . . ? S2 Zn1 N4 C21 -103.7(16) . . . . ? N6 Zn3 N5 C37 142.9(14) . . . . ? O101 Zn3 N5 C37 -80.9(14) . . . . ? S3 Zn3 N5 C37 26.5(14) . . . . ? S4 Zn3 N5 C37 67(2) . . . . ? N6 Zn3 N5 C38 -37.6(13) . . . . ? O101 Zn3 N5 C38 98.7(12) . . . . ? S3 Zn3 N5 C38 -154.0(12) . . . . ? S4 Zn3 N5 C38 -113.8(18) . . . . ? O101 Zn3 N6 C41 133.4(12) . . . . ? N5 Zn3 N6 C41 -126.5(13) . . . . ? S3 Zn3 N6 C41 -32.9(14) . . . . ? S4 Zn3 N6 C41 41.8(13) . . . . ? O101 Zn3 N6 C40 -54.2(12) . . . . ? N5 Zn3 N6 C40 45.9(10) . . . . ? S3 Zn3 N6 C40 139.4(9) . . . . ? S4 Zn3 N6 C40 -145.9(10) . . . . ? N8 Zn4 N7 C48 127.2(10) . . . . ? S3 Zn4 N7 C48 34.7(11) . . . . ? S2 Zn4 N7 C48 -123.0(10) . . . . ? S4 Zn4 N7 C48 -41.4(10) . . . . ? N8 Zn4 N7 C49 -44.8(8) . . . . ? S3 Zn4 N7 C49 -137.3(7) . . . . ? S2 Zn4 N7 C49 65.0(8) . . . . ? S4 Zn4 N7 C49 146.6(8) . . . . ? N7 Zn4 N8 C52 -138.8(10) . . . . ? S3 Zn4 N8 C52 -26.5(10) . . . . ? S2 Zn4 N8 C52 103.8(10) . . . . ? S4 Zn4 N8 C52 -68(2) . . . . ? N7 Zn4 N8 C51 41.7(9) . . . . ? S3 Zn4 N8 C51 154.0(9) . . . . ? S2 Zn4 N8 C51 -75.7(9) . . . . ? S4 Zn4 N8 C51 112.5(16) . . . . ? N10 Zn5 N9 C67 146.3(13) . . . . ? O102 Zn5 N9 C67 -81.9(13) . . . . ? S5 Zn5 N9 C67 31.1(13) . . . . ? S6 Zn5 N9 C67 72(2) . . . . ? N10 Zn5 N9 C68 -44.1(11) . . . . ? O102 Zn5 N9 C68 87.7(11) . . . . ? S5 Zn5 N9 C68 -159.3(10) . . . . ? S6 Zn5 N9 C68 -118.6(18) . . . . ? O102 Zn5 N10 C71 137.0(11) . . . . ? N9 Zn5 N10 C71 -128.4(11) . . . . ? S5 Zn5 N10 C71 -37.8(12) . . . . ? S6 Zn5 N10 C71 40.7(11) . . . . ? O102 Zn5 N10 C70 -50.0(11) . . . . ? N9 Zn5 N10 C70 44.6(10) . . . . ? S5 Zn5 N10 C70 135.2(8) . . . . ? S6 Zn5 N10 C70 -146.3(9) . . . . ? N12 Zn6 N11 C78 127.8(12) . . . . ? S4 Zn6 N11 C78 -123.8(11) . . . . ? S5 Zn6 N11 C78 33.9(12) . . . . ? S6 Zn6 N11 C78 -41.7(11) . . . . ? N12 Zn6 N11 C79 -41.3(10) . . . . ? S4 Zn6 N11 C79 67.0(10) . . . . ? S5 Zn6 N11 C79 -135.3(9) . . . . ? S6 Zn6 N11 C79 149.1(9) . . . . ? N11 Zn6 N12 C82 -144.4(10) . . . . ? S4 Zn6 N12 C82 96.0(10) . . . . ? S5 Zn6 N12 C82 -28.8(10) . . . . ? S6 Zn6 N12 C82 -71(2) . . . . ? N11 Zn6 N12 C81 36.5(9) . . . . ? S4 Zn6 N12 C81 -83.1(8) . . . . ? S5 Zn6 N12 C81 152.1(8) . . . . ? S6 Zn6 N12 C81 110.0(18) . . . . ? Zn2 S1 C1 C2 145.2(10) . . . . ? Zn1 S1 C1 C2 47.6(11) . . . . ? Zn2 S1 C1 C6 -43.4(11) . . . . ? Zn1 S1 C1 C6 -141.0(10) . . . . ? C6 C1 C2 C3 0.8(19) . . . . ? S1 C1 C2 C3 172.4(10) . . . . ? C6 C1 C2 C22 179.1(13) . . . . ? S1 C1 C2 C22 -9(2) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C22 C2 C3 C4 -178.4(13) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C2 C3 C4 C23 -179.6(12) . . . . ? C3 C4 C5 C6 -1.0(19) . . . . ? C23 C4 C5 C6 178.5(12) . . . . ? C2 C1 C6 C5 -1.8(18) . . . . ? S1 C1 C6 C5 -173.4(9) . . . . ? C2 C1 C6 C7 177.7(12) . . . . ? S1 C1 C6 C7 6.1(19) . . . . ? C4 C5 C6 C1 2(2) . . . . ? C4 C5 C6 C7 -177.6(12) . . . . ? C8 N1 C7 C6 177.1(12) . . . . ? Zn2 N1 C7 C6 -5.6(19) . . . . ? C1 C6 C7 N1 29(2) . . . . ? C5 C6 C7 N1 -152.0(13) . . . . ? C7 N1 C8 C9 127.2(13) . . . . ? Zn2 N1 C8 C9 -50.3(13) . . . . ? N1 C8 C9 C10 70.0(15) . . . . ? C11 N2 C10 C9 -112.4(13) . . . . ? Zn2 N2 C10 C9 62.9(12) . . . . ? C8 C9 C10 N2 -76.4(14) . . . . ? C10 N2 C11 C12 174.3(12) . . . . ? Zn2 N2 C11 C12 0(2) . . . . ? N2 C11 C12 C13 -146.9(14) . . . . ? N2 C11 C12 C17 31(2) . . . . ? C17 C12 C13 C14 0(2) . . . . ? C11 C12 C13 C14 178.7(12) . . . . ? C12 C13 C14 C15 -5.4(19) . . . . ? C12 C13 C14 C27 175.7(12) . . . . ? C13 C14 C15 C16 5.2(18) . . . . ? C27 C14 C15 C16 -175.8(11) . . . . ? C14 C15 C16 C17 -0.3(18) . . . . ? C14 C15 C16 C18 -178.0(11) . . . . ? C13 C12 C17 C16 4.5(18) . . . . ? C11 C12 C17 C16 -173.4(12) . . . . ? C13 C12 C17 S2 -169.0(10) . . . . ? C11 C12 C17 S2 13.0(18) . . . . ? C15 C16 C17 C12 -4.6(16) . . . . ? C18 C16 C17 C12 172.8(11) . . . . ? C15 C16 C17 S2 168.8(9) . . . . ? C18 C16 C17 S2 -13.8(16) . . . . ? Zn4 S2 C17 C12 107.1(9) . . . . ? Zn1 S2 C17 C12 -131.8(9) . . . . ? Zn2 S2 C17 C12 -52.3(10) . . . . ? Zn4 S2 C17 C16 -66.1(9) . . . . ? Zn1 S2 C17 C16 55.0(9) . . . . ? Zn2 S2 C17 C16 134.5(9) . . . . ? C19 N3 C18 C16 -174.2(12) . . . . ? Zn1 N3 C18 C16 -0.2(19) . . . . ? C15 C16 C18 N3 146.3(13) . . . . ? C17 C16 C18 N3 -31(2) . . . . ? C18 N3 C19 C20 109.0(14) . . . . ? Zn1 N3 C19 C20 -65.8(14) . . . . ? N3 C19 C20 C21 71(2) . . . . ? C19 C20 C21 N4 -59(2) . . . . ? C22 N4 C21 C20 -142.3(16) . . . . ? Zn1 N4 C21 C20 44(2) . . . . ? C21 N4 C22 C2 -171.7(14) . . . . ? Zn1 N4 C22 C2 1(2) . . . . ? C3 C2 C22 N4 153.2(14) . . . . ? C1 C2 C22 N4 -25(2) . . . . ? C5 C4 C23 C25A -116.0(16) . . . . ? C3 C4 C23 C25A 63.5(17) . . . . ? C5 C4 C23 C24A 124.3(16) . . . . ? C3 C4 C23 C24A -56.2(18) . . . . ? C5 C4 C23 C25 72.8(19) . . . . ? C3 C4 C23 C25 -107.7(18) . . . . ? C5 C4 C23 C26A 3.3(19) . . . . ? C3 C4 C23 C26A -177.2(15) . . . . ? C5 C4 C23 C24 -46.5(19) . . . . ? C3 C4 C23 C24 133.0(17) . . . . ? C5 C4 C23 C26 -165.5(16) . . . . ? C3 C4 C23 C26 14(2) . . . . ? C13 C14 C27 C30 21.2(17) . . . . ? C15 C14 C27 C30 -157.7(12) . . . . ? C13 C14 C27 C28 -98.7(14) . . . . ? C15 C14 C27 C28 82.4(14) . . . . ? C13 C14 C27 C29 143.1(13) . . . . ? C15 C14 C27 C29 -35.8(15) . . . . ? Zn4 S3 C31 C32 -42.8(10) . . . . ? Zn3 S3 C31 C32 -144.4(9) . . . . ? Zn4 S3 C31 C36 143.9(9) . . . . ? Zn3 S3 C31 C36 42.3(10) . . . . ? C36 C31 C32 C33 4.5(18) . . . . ? S3 C31 C32 C33 -168.8(9) . . . . ? C36 C31 C32 C52 -174.9(12) . . . . ? S3 C31 C32 C52 11.8(18) . . . . ? C31 C32 C33 C34 -3(2) . . . . ? C52 C32 C33 C34 176.3(13) . . . . ? C32 C33 C34 C35 0(2) . . . . ? C32 C33 C34 C53 -179.8(13) . . . . ? C33 C34 C35 C36 3(2) . . . . ? C53 C34 C35 C36 -177.7(13) . . . . ? C34 C35 C36 C31 -1(2) . . . . ? C34 C35 C36 C37 -178.3(14) . . . . ? C32 C31 C36 C35 -2.4(18) . . . . ? S3 C31 C36 C35 171.0(10) . . . . ? C32 C31 C36 C37 173.8(13) . . . . ? S3 C31 C36 C37 -12.9(19) . . . . ? C38 N5 C37 C36 -177.2(16) . . . . ? Zn3 N5 C37 C36 2(2) . . . . ? C35 C36 C37 N5 158.5(16) . . . . ? C31 C36 C37 N5 -18(3) . . . . ? C37 N5 C38 C39 -129.4(17) . . . . ? Zn3 N5 C38 C39 51(2) . . . . ? N5 C38 C39 C40 -66(2) . . . . ? C41 N6 C40 C39 109.5(16) . . . . ? Zn3 N6 C40 C39 -64.0(16) . . . . ? C38 C39 C40 N6 70(2) . . . . ? C40 N6 C41 C42 -176.4(12) . . . . ? Zn3 N6 C41 C42 -4(2) . . . . ? N6 C41 C42 C43 150.9(15) . . . . ? N6 C41 C42 C47 -27(2) . . . . ? C47 C42 C43 C44 4(2) . . . . ? C41 C42 C43 C44 -173.9(13) . . . . ? C42 C43 C44 C45 0(2) . . . . ? C42 C43 C44 C57 -176.8(14) . . . . ? C43 C44 C45 C46 0(2) . . . . ? C57 C44 C45 C46 176.9(13) . . . . ? C44 C45 C46 C47 -4(2) . . . . ? C44 C45 C46 C48 176.6(13) . . . . ? C45 C46 C47 C42 7.6(17) . . . . ? C48 C46 C47 C42 -173.2(12) . . . . ? C45 C46 C47 S4 -165.5(10) . . . . ? C48 C46 C47 S4 13.8(17) . . . . ? C43 C42 C47 C46 -7.7(18) . . . . ? C41 C42 C47 C46 169.9(11) . . . . ? C43 C42 C47 S4 165.3(10) . . . . ? C41 C42 C47 S4 -17.1(17) . . . . ? Zn6 S4 C47 C46 94.7(10) . . . . ? Zn4 S4 C47 C46 -52.9(10) . . . . ? Zn3 S4 C47 C46 -133.1(10) . . . . ? Zn6 S4 C47 C42 -78.2(11) . . . . ? Zn4 S4 C47 C42 134.2(10) . . . . ? Zn3 S4 C47 C42 54.1(10) . . . . ? C49 N7 C48 C46 175.3(11) . . . . ? Zn4 N7 C48 C46 3.9(18) . . . . ? C47 C46 C48 N7 28(2) . . . . ? C45 C46 C48 N7 -153.1(13) . . . . ? C48 N7 C49 C50 -110.4(13) . . . . ? Zn4 N7 C49 C50 62.2(12) . . . . ? N7 C49 C50 C51 -71.7(16) . . . . ? C49 C50 C51 N8 65.7(16) . . . . ? C52 N8 C51 C50 124.7(13) . . . . ? Zn4 N8 C51 C50 -55.8(13) . . . . ? C51 N8 C52 C32 176.2(13) . . . . ? Zn4 N8 C52 C32 -3(2) . . . . ? C31 C32 C52 N8 19(2) . . . . ? C33 C32 C52 N8 -160.1(13) . . . . ? C33 C34 C53 C54 -167.4(14) . . . . ? C35 C34 C53 C54 13.3(19) . . . . ? C33 C34 C53 C55 70.6(17) . . . . ? C35 C34 C53 C55 -108.8(16) . . . . ? C33 C34 C53 C56 -47.4(18) . . . . ? C35 C34 C53 C56 133.3(15) . . . . ? C45 C44 C57 C59 8(2) . . . . ? C43 C44 C57 C59 -175.0(17) . . . . ? C45 C44 C57 C59A -167.4(18) . . . . ? C43 C44 C57 C59A 9(2) . . . . ? C45 C44 C57 C60 -122.0(17) . . . . ? C43 C44 C57 C60 55(2) . . . . ? C45 C44 C57 C60A 60(2) . . . . ? C43 C44 C57 C60A -123.7(19) . . . . ? C45 C44 C57 C58 125.1(18) . . . . ? C43 C44 C57 C58 -58.4(18) . . . . ? C45 C44 C57 C58A -53.0(19) . . . . ? C43 C44 C57 C58A 123.5(19) . . . . ? Zn6 S5 C61 C62 -45.4(10) . . . . ? Zn5 S5 C61 C62 -144.6(9) . . . . ? Zn6 S5 C61 C66 144.8(9) . . . . ? Zn5 S5 C61 C66 45.6(10) . . . . ? C66 C61 C62 C63 -1.9(17) . . . . ? S5 C61 C62 C63 -172.0(10) . . . . ? C66 C61 C62 C82 -178.1(12) . . . . ? S5 C61 C62 C82 11.8(18) . . . . ? C61 C62 C63 C64 3(2) . . . . ? C82 C62 C63 C64 179.2(14) . . . . ? C62 C63 C64 C65 -3(2) . . . . ? C62 C63 C64 C83 177.5(13) . . . . ? C63 C64 C65 C66 3(2) . . . . ? C83 C64 C65 C66 -177.6(14) . . . . ? C64 C65 C66 C61 -2(2) . . . . ? C64 C65 C66 C67 -175.7(15) . . . . ? C62 C61 C66 C65 1.8(18) . . . . ? S5 C61 C66 C65 172.0(10) . . . . ? C62 C61 C66 C67 174.5(13) . . . . ? S5 C61 C66 C67 -15.2(18) . . . . ? C68 N9 C67 C66 -172.0(16) . . . . ? Zn5 N9 C67 C66 -2(3) . . . . ? C65 C66 C67 N9 157.6(17) . . . . ? C61 C66 C67 N9 -15(3) . . . . ? C67 N9 C68 C69 -134.4(16) . . . . ? Zn5 N9 C68 C69 55.1(17) . . . . ? N9 C68 C69 C70 -65(2) . . . . ? C71 N10 C70 C69 111.2(15) . . . . ? Zn5 N10 C70 C69 -62.5(14) . . . . ? C68 C69 C70 N10 70.2(18) . . . . ? C70 N10 C71 C72 -174.9(12) . . . . ? Zn5 N10 C71 C72 -2.2(19) . . . . ? N10 C71 C72 C77 -29(2) . . . . ? N10 C71 C72 C73 148.4(13) . . . . ? C77 C72 C73 C74 3(2) . . . . ? C71 C72 C73 C74 -174.8(12) . . . . ? C72 C73 C74 C75 0.9(19) . . . . ? C72 C73 C74 C87 -175.9(11) . . . . ? C73 C74 C75 C76 -2.2(19) . . . . ? C87 C74 C75 C76 174.6(11) . . . . ? C74 C75 C76 C77 -0.3(18) . . . . ? C74 C75 C76 C78 175.3(12) . . . . ? C73 C72 C77 C76 -5.4(18) . . . . ? C71 C72 C77 C76 172.0(11) . . . . ? C73 C72 C77 S6 170.7(10) . . . . ? C71 C72 C77 S6 -11.9(18) . . . . ? C75 C76 C77 C72 4.1(17) . . . . ? C78 C76 C77 C72 -170.8(12) . . . . ? C75 C76 C77 S6 -172.1(9) . . . . ? C78 C76 C77 S6 13.0(17) . . . . ? Zn2 S6 C77 C72 -77.1(10) . . . . ? Zn5 S6 C77 C72 51.5(10) . . . . ? Zn6 S6 C77 C72 131.9(10) . . . . ? Zn2 S6 C77 C76 98.9(9) . . . . ? Zn5 S6 C77 C76 -132.5(9) . . . . ? Zn6 S6 C77 C76 -52.0(9) . . . . ? C79 N11 C78 C76 172.9(13) . . . . ? Zn6 N11 C78 C76 4(2) . . . . ? C75 C76 C78 N11 -146.2(14) . . . . ? C77 C76 C78 N11 29(2) . . . . ? C78 N11 C79 C80 -108.7(14) . . . . ? Zn6 N11 C79 C80 61.8(14) . . . . ? N11 C79 C80 C81 -72.3(16) . . . . ? C79 C80 C81 N12 64.4(16) . . . . ? C82 N12 C81 C80 131.2(14) . . . . ? Zn6 N12 C81 C80 -49.6(14) . . . . ? C81 N12 C82 C62 175.3(12) . . . . ? Zn6 N12 C82 C62 -3.8(19) . . . . ? C61 C62 C82 N12 22(2) . . . . ? C63 C62 C82 N12 -154.3(13) . . . . ? C63 C64 C83 C86 2(2) . . . . ? C65 C64 C83 C86 -178.1(14) . . . . ? C63 C64 C83 C85 123.1(17) . . . . ? C65 C64 C83 C85 -56.7(18) . . . . ? C63 C64 C83 C84 -118.5(17) . . . . ? C65 C64 C83 C84 61.7(18) . . . . ? C75 C74 C87 C88 -63.3(14) . . . . ? C73 C74 C87 C88 113.4(13) . . . . ? C75 C74 C87 C90 55.3(15) . . . . ? C73 C74 C87 C90 -128.1(12) . . . . ? C75 C74 C87 C89 177.1(11) . . . . ? C73 C74 C87 C89 -6.2(16) . . . . ? O102 C100 O100 Zn1 -159.6(11) . . . . ? O101 C100 O100 Zn1 5.3(14) . . . . ? N3 Zn1 O100 C100 -15.0(13) . . . . ? N4 Zn1 O100 C100 -114.5(9) . . . . ? S1 Zn1 O100 C100 155.4(8) . . . . ? S2 Zn1 O100 C100 72.5(8) . . . . ? O102 C100 O101 Zn3 6.9(15) . . . . ? O100 C100 O101 Zn3 -157.6(10) . . . . ? N6 Zn3 O101 C100 -20.4(12) . . . . ? N5 Zn3 O101 C100 -119.8(9) . . . . ? S3 Zn3 O101 C100 146.8(8) . . . . ? S4 Zn3 O101 C100 66.7(9) . . . . ? O100 C100 O102 Zn5 12.5(17) . . . . ? O101 C100 O102 Zn5 -152.0(11) . . . . ? N10 Zn5 O102 C100 -33.9(13) . . . . ? N9 Zn5 O102 C100 -128.7(11) . . . . ? S5 Zn5 O102 C100 141.0(10) . . . . ? S6 Zn5 O102 C100 56.3(11) . . . . ? #===END