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 _publ_contact_author_name 'Alexander Rothenberger' _publ_contact_author_address ; Institut fur Anorganische Chemie University of Karlsruhe Engesserstr. 15 Karlsruhe 76131 GERMANY ; _publ_contact_author_phone 'Int + 721 608 2849' _publ_contact_author_fax 'Int + 721 608 8440' _publ_contact_author_email rothenberger@chemie.uni-karlsruhe.de _publ_section_title ; A strategy for the built-up of transition metal complexes containing tripodal [RPOS2]2- and [RPS3]2- ligands ; loop_ _publ_author_name _publ_author_address 'Alexander Rothenberger' ; Institut fuer Anorganische Chemie der Universitaet Engesserstrasse 15 76131 Karlsruhe Deutschland ; 'Weifeng Shi.' ; Institut fuer Anorganische Chemie der Universitaet Engesserstrasse 15 76131 Karlsruhe Deutschland ; 'Christopher E. Anson' ; Institut fuer Anorganische Chemie der Universitaet Engesserstrasse 15 76131 Karlsruhe Deutschland ; data_1 _database_code_depnum_ccdc_archive 'CCDC 276586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H78 Cl4 Cu4 O2 P6 S6' _chemical_formula_weight 1941.64 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.960(3) _cell_length_b 22.853(5) _cell_length_c 15.976(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.02(3) _cell_angle_gamma 90.00 _cell_volume 4354.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.387 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'stoe stadi v' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28160 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 31.82 _reflns_number_total 10288 _reflns_number_gt 7874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'kuma ccd 1.168' _computing_cell_refinement 'kuma ccd 1.168' _computing_data_reduction 'kuma ccd 1.168' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^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 10288 _refine_ls_number_parameters 507 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.1188(3) 1.29881(13) -0.0435(2) 0.0646(9) Uani 1 1 d D . . Cu1 Cu 0.62012(3) 1.075446(15) -0.00826(3) 0.02533(11) Uani 1 1 d . . . Cu2 Cu 0.50622(3) 0.999421(15) -0.14825(3) 0.02933(12) Uani 1 1 d . . . P1 P 0.38601(6) 1.08194(3) -0.01355(5) 0.01928(15) Uani 1 1 d . . . P2 P 0.72265(6) 1.15017(3) -0.02389(5) 0.02162(16) Uani 1 1 d . . . P3 P 0.51165(6) 0.99904(3) -0.28579(5) 0.02287(17) Uani 1 1 d . . . S1 S 0.53319(6) 1.09094(3) 0.09751(5) 0.02242(16) Uani 1 1 d . . . S2 S 0.41941(6) 1.08106(3) -0.12785(5) 0.02321(16) Uani 1 1 d . . . S3 S 0.70412(6) 0.98628(3) -0.00410(5) 0.02457(16) Uani 1 1 d . . . Cl1 Cl 1.04559(9) 0.96831(6) -0.29383(9) 0.0693(3) Uani 1 1 d . B . C1 C 0.3040(2) 1.14774(12) -0.0212(2) 0.0250(6) Uani 1 1 d . . . C2 C 0.2824(3) 1.16517(16) 0.0517(2) 0.0402(8) Uani 1 1 d . A . H2A H 0.3093 1.1424 0.1058 0.048 Uiso 1 1 calc R . . C3 C 0.2215(3) 1.21578(19) 0.0482(3) 0.0544(11) Uani 1 1 d . . . H3A H 0.2080 1.2280 0.0999 0.065 Uiso 1 1 calc R A . C4 C 0.1805(3) 1.24831(15) -0.0311(3) 0.0428(9) Uani 1 1 d . A . C5 C 0.2012(3) 1.23135(15) -0.1048(3) 0.0402(8) Uani 1 1 d . . . H5A H 0.1735 1.2539 -0.1591 0.048 Uiso 1 1 calc R A . C6 C 0.2625(3) 1.18128(14) -0.1000(2) 0.0349(7) Uani 1 1 d . A . H6A H 0.2766 1.1695 -0.1516 0.042 Uiso 1 1 calc R . . C7 C 0.1164(8) 1.3290(4) 0.0321(5) 0.050(3) Uiso 0.55(2) 1 d PD A 1 H7A H 0.1666 1.3629 0.0450 0.074 Uiso 0.55(2) 1 calc PR A 1 H7B H 0.1411 1.3029 0.0850 0.074 Uiso 0.55(2) 1 calc PR A 1 H7C H 0.0398 1.3423 0.0191 0.074 Uiso 0.55(2) 1 calc PR A 1 C7A C 0.0716(14) 1.3045(8) 0.0320(9) 0.083(5) Uiso 0.45(2) 1 d PD A 2 H7AA H 0.0192 1.2724 0.0263 0.125 Uiso 0.45(2) 1 calc PR A 2 H7AB H 0.0323 1.3420 0.0253 0.125 Uiso 0.45(2) 1 calc PR A 2 H7AC H 0.1335 1.3028 0.0919 0.125 Uiso 0.45(2) 1 calc PR A 2 C8 C 0.8332(2) 1.12591(12) -0.0599(2) 0.0250(6) Uani 1 1 d . . . C9 C 0.9422(3) 1.1196(2) 0.0009(3) 0.0539(11) Uani 1 1 d . . . H9A H 0.9635 1.1328 0.0618 0.065 Uiso 1 1 calc R . . C10 C 1.0221(3) 1.0939(3) -0.0264(3) 0.0707(15) Uani 1 1 d . . . H10A H 1.0972 1.0893 0.0163 0.085 Uiso 1 1 calc R . . C11 C 0.9932(3) 1.07576(19) -0.1127(3) 0.0505(10) Uani 1 1 d . . . H11A H 1.0476 1.0580 -0.1306 0.061 Uiso 1 1 calc R . . C12 C 0.8856(3) 1.08282(18) -0.1747(3) 0.0445(9) Uani 1 1 d . . . H12A H 0.8659 1.0710 -0.2361 0.053 Uiso 1 1 calc R . . C13 C 0.8052(3) 1.10730(16) -0.1479(2) 0.0379(8) Uani 1 1 d . . . H13A H 0.7302 1.1112 -0.1908 0.045 Uiso 1 1 calc R . . C14 C 0.7968(2) 1.19228(13) 0.0795(2) 0.0271(6) Uani 1 1 d . . . C15 C 0.8327(3) 1.16317(16) 0.1631(2) 0.0388(8) Uani 1 1 d . . . H15A H 0.8165 1.1228 0.1650 0.047 Uiso 1 1 calc R . . C16 C 0.8916(3) 1.1929(2) 0.2428(3) 0.0479(9) Uani 1 1 d . . . H16A H 0.9181 1.1724 0.2990 0.057 Uiso 1 1 calc R . . C17 C 0.9123(3) 1.25200(19) 0.2416(3) 0.0482(10) Uani 1 1 d . . . H17A H 0.9511 1.2724 0.2969 0.058 Uiso 1 1 calc R . . C18 C 0.8764(3) 1.28148(17) 0.1597(3) 0.0504(10) Uani 1 1 d . . . H18A H 0.8912 1.3221 0.1586 0.061 Uiso 1 1 calc R . . C19 C 0.8190(3) 1.25190(15) 0.0793(2) 0.0408(8) Uani 1 1 d . . . H19A H 0.7944 1.2725 0.0232 0.049 Uiso 1 1 calc R . . C20 C 0.6462(2) 1.20659(12) -0.1051(2) 0.0246(6) Uani 1 1 d . . . C21 C 0.6865(3) 1.23502(14) -0.1634(2) 0.0329(7) Uani 1 1 d . . . H21A H 0.7577 1.2246 -0.1629 0.039 Uiso 1 1 calc R . . C22 C 0.6236(3) 1.27845(16) -0.2222(3) 0.0441(8) Uani 1 1 d . . . H22A H 0.6509 1.2974 -0.2623 0.053 Uiso 1 1 calc R . . C23 C 0.5205(3) 1.29363(16) -0.2216(3) 0.0463(9) Uani 1 1 d . . . H23A H 0.4770 1.3233 -0.2615 0.056 Uiso 1 1 calc R . . C24 C 0.4804(3) 1.26637(15) -0.1639(3) 0.0416(8) Uani 1 1 d . . . H24A H 0.4102 1.2777 -0.1633 0.050 Uiso 1 1 calc R . . C25 C 0.5415(2) 1.22258(13) -0.1068(2) 0.0314(7) Uani 1 1 d . . . H25A H 0.5121 1.2031 -0.0684 0.038 Uiso 1 1 calc R . . C26 C 0.6177(2) 0.95181(13) -0.29839(19) 0.0248(6) Uani 1 1 d . . . C27 C 0.5999(3) 0.91675(14) -0.3739(2) 0.0309(7) Uani 1 1 d . . . H27A H 0.5277 0.9151 -0.4218 0.037 Uiso 1 1 calc R . . C28 C 0.6867(3) 0.88441(14) -0.3793(2) 0.0360(7) Uani 1 1 d . . . H28A H 0.6734 0.8598 -0.4304 0.043 Uiso 1 1 calc R . . C29 C 0.7932(3) 0.88732(15) -0.3114(2) 0.0379(8) Uani 1 1 d . . . H29A H 0.8529 0.8656 -0.3164 0.046 Uiso 1 1 calc R . . C30 C 0.8115(3) 0.92158(17) -0.2371(3) 0.0423(8) Uani 1 1 d . . . H30A H 0.8844 0.9236 -0.1901 0.051 Uiso 1 1 calc R . . C31 C 0.7244(3) 0.95350(16) -0.2296(2) 0.0351(7) Uani 1 1 d . . . H31A H 0.7378 0.9767 -0.1771 0.042 Uiso 1 1 calc R . . C32 C 0.5315(3) 1.06858(13) -0.3336(2) 0.0279(6) Uani 1 1 d . . . C33 C 0.4676(3) 1.11643(14) -0.3269(2) 0.0366(7) Uani 1 1 d . . . H33A H 0.4178 1.1123 -0.2966 0.044 Uiso 1 1 calc R . . C34 C 0.4772(4) 1.16981(16) -0.3646(2) 0.0473(9) Uani 1 1 d . . . H34A H 0.4322 1.2020 -0.3617 0.057 Uiso 1 1 calc R . . C35 C 0.5524(4) 1.17652(16) -0.4068(2) 0.0478(9) Uani 1 1 d . . . H35A H 0.5601 1.2134 -0.4311 0.057 Uiso 1 1 calc R . . C36 C 0.6158(3) 1.12946(16) -0.4131(2) 0.0420(8) Uani 1 1 d . . . H36A H 0.6665 1.1339 -0.4425 0.050 Uiso 1 1 calc R . . C37 C 0.6055(3) 1.07559(14) -0.3767(2) 0.0320(7) Uani 1 1 d . . . H37A H 0.6494 1.0434 -0.3812 0.038 Uiso 1 1 calc R . . C38 C 0.3782(2) 0.97322(13) -0.3715(2) 0.0254(6) Uani 1 1 d . . . C39 C 0.3313(3) 0.92292(15) -0.3533(2) 0.0357(7) Uani 1 1 d . . . H39A H 0.3701 0.9021 -0.2985 0.043 Uiso 1 1 calc R . . C40 C 0.2282(3) 0.90237(18) -0.4141(2) 0.0446(9) Uani 1 1 d . . . H40A H 0.1973 0.8675 -0.4011 0.054 Uiso 1 1 calc R . . C41 C 0.1713(3) 0.93264(19) -0.4928(3) 0.0490(9) Uani 1 1 d . . . H41A H 0.1003 0.9191 -0.5340 0.059 Uiso 1 1 calc R . . C42 C 0.2169(3) 0.9827(2) -0.5122(3) 0.0495(10) Uani 1 1 d . . . H42A H 0.1771 1.0036 -0.5668 0.059 Uiso 1 1 calc R . . C43 C 0.3203(3) 1.00257(15) -0.4528(2) 0.0365(8) Uani 1 1 d . . . H43A H 0.3520 1.0365 -0.4674 0.044 Uiso 1 1 calc R . . C44 C 1.1600(3) 1.0148(2) -0.2722(4) 0.0601(12) Uani 1 1 d . . . Cl2 Cl 1.1064(4) 1.08873(19) -0.2933(4) 0.0548(18) Uani 0.61(4) 1 d P B 1 Cl2A Cl 1.132(2) 1.0809(11) -0.319(2) 0.111(9) Uani 0.39(4) 1 d P B 2 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 O1 0.0670(19) 0.0491(17) 0.071(2) -0.0052(15) 0.0199(16) 0.0342(14) Cu1 0.02248(19) 0.0240(2) 0.0325(2) 0.00055(14) 0.01398(16) -0.00125(13) Cu2 0.0419(2) 0.0277(2) 0.0241(2) 0.00236(14) 0.01900(18) 0.00443(15) P1 0.0178(3) 0.0205(3) 0.0208(4) 0.0002(3) 0.0088(3) 0.0023(2) P2 0.0185(3) 0.0226(4) 0.0251(4) 0.0002(3) 0.0100(3) 0.0000(2) P3 0.0250(4) 0.0261(4) 0.0191(4) 0.0011(3) 0.0104(3) 0.0019(3) S1 0.0219(3) 0.0253(3) 0.0200(3) -0.0011(3) 0.0081(3) -0.0010(2) S2 0.0229(3) 0.0273(4) 0.0209(3) 0.0022(3) 0.0102(3) 0.0047(3) S3 0.0200(3) 0.0231(3) 0.0339(4) 0.0011(3) 0.0140(3) 0.0010(2) Cl1 0.0408(5) 0.0693(7) 0.0807(8) 0.0176(6) 0.0051(5) -0.0094(5) C1 0.0214(13) 0.0227(14) 0.0317(16) -0.0002(11) 0.0112(12) 0.0026(10) C2 0.0468(19) 0.0421(19) 0.0329(18) -0.0017(15) 0.0169(15) 0.0159(15) C3 0.058(2) 0.060(3) 0.049(2) -0.0149(19) 0.0248(19) 0.023(2) C4 0.0332(17) 0.0306(17) 0.058(2) -0.0049(16) 0.0102(16) 0.0147(14) C5 0.0385(18) 0.0342(18) 0.050(2) 0.0087(15) 0.0203(16) 0.0134(14) C6 0.0336(16) 0.0333(17) 0.0419(19) 0.0073(14) 0.0193(14) 0.0100(13) C8 0.0214(13) 0.0234(14) 0.0323(16) -0.0024(12) 0.0130(12) -0.0004(10) C9 0.0260(17) 0.092(3) 0.038(2) -0.019(2) 0.0066(15) 0.0155(18) C10 0.0283(19) 0.120(4) 0.058(3) -0.027(3) 0.0105(18) 0.021(2) C11 0.0334(19) 0.065(3) 0.061(3) -0.016(2) 0.0273(18) 0.0054(16) C12 0.0389(19) 0.060(2) 0.0382(19) -0.0140(17) 0.0188(16) 0.0032(16) C13 0.0270(16) 0.052(2) 0.0331(17) -0.0093(15) 0.0103(13) 0.0034(14) C14 0.0207(13) 0.0323(16) 0.0295(16) -0.0030(12) 0.0111(12) -0.0001(11) C15 0.0344(17) 0.045(2) 0.0347(18) 0.0000(15) 0.0114(14) -0.0037(14) C16 0.0386(19) 0.071(3) 0.0297(19) -0.0020(17) 0.0088(15) -0.0038(18) C17 0.0316(17) 0.069(3) 0.038(2) -0.0211(19) 0.0076(15) -0.0030(17) C18 0.046(2) 0.039(2) 0.053(2) -0.0169(18) 0.0062(18) -0.0049(16) C19 0.0419(19) 0.0327(18) 0.0402(19) -0.0055(15) 0.0077(15) -0.0036(14) C20 0.0223(13) 0.0200(13) 0.0284(15) -0.0014(11) 0.0065(11) -0.0006(10) C21 0.0336(16) 0.0329(17) 0.0340(17) 0.0036(13) 0.0153(13) 0.0017(13) C22 0.055(2) 0.0356(19) 0.042(2) 0.0072(15) 0.0186(17) -0.0016(16) C23 0.0416(19) 0.0314(18) 0.050(2) 0.0100(16) 0.0002(16) 0.0057(14) C24 0.0292(16) 0.0299(17) 0.060(2) 0.0021(16) 0.0107(16) 0.0066(13) C25 0.0264(14) 0.0252(15) 0.0439(19) -0.0010(13) 0.0152(13) 0.0008(11) C26 0.0245(13) 0.0285(15) 0.0235(14) 0.0036(11) 0.0118(11) 0.0022(11) C27 0.0334(16) 0.0340(17) 0.0265(16) -0.0052(13) 0.0132(13) -0.0013(12) C28 0.0429(18) 0.0326(17) 0.0384(18) -0.0073(14) 0.0221(15) 0.0010(14) C29 0.0368(17) 0.0385(18) 0.046(2) 0.0029(15) 0.0241(16) 0.0084(14) C30 0.0274(16) 0.059(2) 0.0374(19) 0.0004(16) 0.0089(14) 0.0100(15) C31 0.0278(15) 0.0461(19) 0.0288(16) -0.0036(14) 0.0083(13) 0.0054(13) C32 0.0346(16) 0.0280(15) 0.0184(14) 0.0010(11) 0.0074(12) -0.0038(12) C33 0.0480(19) 0.0320(17) 0.0318(17) 0.0027(13) 0.0179(15) 0.0056(14) C34 0.072(3) 0.0310(18) 0.0351(19) 0.0008(15) 0.0167(18) 0.0058(17) C35 0.075(3) 0.0340(19) 0.0318(18) 0.0039(15) 0.0182(18) -0.0137(18) C36 0.052(2) 0.044(2) 0.0328(18) 0.0003(15) 0.0192(16) -0.0186(16) C37 0.0362(17) 0.0365(17) 0.0233(15) 0.0002(12) 0.0115(13) -0.0055(13) C38 0.0250(14) 0.0306(15) 0.0225(14) 0.0004(11) 0.0114(11) 0.0026(11) C39 0.0355(17) 0.0384(18) 0.0317(17) 0.0023(13) 0.0115(14) -0.0041(13) C40 0.0396(19) 0.054(2) 0.039(2) -0.0036(17) 0.0137(16) -0.0117(16) C41 0.0310(18) 0.065(3) 0.044(2) -0.0085(18) 0.0066(16) -0.0086(17) C42 0.0349(19) 0.066(3) 0.036(2) 0.0099(18) 0.0008(15) 0.0018(18) C43 0.0366(18) 0.043(2) 0.0260(17) 0.0083(14) 0.0084(14) 0.0000(14) C44 0.034(2) 0.061(3) 0.081(3) -0.009(2) 0.019(2) -0.0062(18) Cl2 0.0520(15) 0.055(2) 0.0503(19) 0.0079(11) 0.0120(12) -0.0022(11) Cl2A 0.079(7) 0.114(6) 0.091(10) 0.041(7) -0.019(7) -0.035(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C4 1.374(4) . ? O1 C7 1.401(8) . ? O1 C7A 1.556(13) . ? Cu1 P2 2.2368(8) . ? Cu1 S3 2.2989(9) . ? Cu1 S1 2.3957(9) . ? Cu1 S2 2.5585(13) . ? Cu1 Cu2 2.7599(9) . ? Cu2 P3 2.2258(9) . ? Cu2 S2 2.2671(8) . ? Cu2 S1 2.3465(9) 3_675 ? Cu2 S3 2.7115(14) . ? P1 C1 1.818(3) . ? P1 S3 2.0327(10) 3_675 ? P1 S2 2.0348(11) . ? P1 S1 2.0449(13) . ? P2 C20 1.822(3) . ? P2 C14 1.827(3) . ? P2 C8 1.827(3) . ? P3 C26 1.820(3) . ? P3 C32 1.824(3) . ? P3 C38 1.834(3) . ? S1 Cu2 2.3465(9) 3_675 ? S3 P1 2.0326(10) 3_675 ? Cl1 C44 1.745(4) . ? C1 C2 1.360(4) . ? C1 C6 1.391(4) . ? C2 C3 1.389(5) . ? C3 C4 1.383(6) . ? C4 C5 1.362(5) . ? C5 C6 1.378(4) . ? C8 C9 1.374(4) . ? C8 C13 1.375(4) . ? C9 C10 1.401(5) . ? C10 C11 1.345(6) . ? C11 C12 1.369(5) . ? C12 C13 1.389(5) . ? C14 C19 1.393(5) . ? C14 C15 1.399(5) . ? C15 C16 1.380(5) . ? C16 C17 1.379(6) . ? C17 C18 1.381(6) . ? C18 C19 1.383(5) . ? C20 C21 1.394(4) . ? C20 C25 1.395(4) . ? C21 C22 1.391(5) . ? C22 C23 1.384(5) . ? C23 C24 1.371(6) . ? C24 C25 1.376(5) . ? C26 C31 1.390(4) . ? C26 C27 1.390(4) . ? C27 C28 1.377(4) . ? C28 C29 1.384(5) . ? C29 C30 1.363(5) . ? C30 C31 1.388(5) . ? C32 C37 1.392(4) . ? C32 C33 1.402(5) . ? C33 C34 1.388(5) . ? C34 C35 1.393(6) . ? C35 C36 1.381(6) . ? C36 C37 1.390(5) . ? C38 C39 1.384(4) . ? C38 C43 1.391(4) . ? C39 C40 1.390(5) . ? C40 C41 1.371(5) . ? C41 C42 1.378(6) . ? C42 C43 1.381(5) . ? C44 Cl2A 1.661(14) . ? C44 Cl2 1.808(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 O1 C7 119.8(4) . . ? C4 O1 C7A 110.0(6) . . ? C7 O1 C7A 31.1(6) . . ? P2 Cu1 S3 112.62(3) . . ? P2 Cu1 S1 115.45(3) . . ? S3 Cu1 S1 117.30(3) . . ? P2 Cu1 S2 110.68(3) . . ? S3 Cu1 S2 113.44(3) . . ? S1 Cu1 S2 84.15(3) . . ? P2 Cu1 Cu2 122.88(3) . . ? S3 Cu1 Cu2 64.06(3) . . ? S1 Cu1 Cu2 114.49(3) . . ? S2 Cu1 Cu2 50.29(3) . . ? P3 Cu2 S2 110.74(3) . . ? P3 Cu2 S1 115.64(3) . 3_675 ? S2 Cu2 S1 119.17(3) . 3_675 ? P3 Cu2 S3 116.96(4) . . ? S2 Cu2 S3 109.07(3) . . ? S1 Cu2 S3 82.56(3) 3_675 . ? P3 Cu2 Cu1 126.09(3) . . ? S2 Cu2 Cu1 60.24(3) . . ? S1 Cu2 Cu1 113.19(3) 3_675 . ? S3 Cu2 Cu1 49.68(2) . . ? C1 P1 S3 106.94(10) . 3_675 ? C1 P1 S2 105.76(10) . . ? S3 P1 S2 116.89(5) 3_675 . ? C1 P1 S1 107.31(10) . . ? S3 P1 S1 110.39(4) 3_675 . ? S2 P1 S1 109.03(5) . . ? C20 P2 C14 102.59(14) . . ? C20 P2 C8 105.40(14) . . ? C14 P2 C8 104.16(13) . . ? C20 P2 Cu1 116.00(9) . . ? C14 P2 Cu1 115.25(10) . . ? C8 P2 Cu1 112.15(10) . . ? C26 P3 C32 103.52(14) . . ? C26 P3 C38 105.02(13) . . ? C32 P3 C38 102.35(14) . . ? C26 P3 Cu2 115.37(10) . . ? C32 P3 Cu2 118.30(10) . . ? C38 P3 Cu2 110.73(10) . . ? P1 S1 Cu2 87.48(3) . 3_675 ? P1 S1 Cu1 84.81(4) . . ? Cu2 S1 Cu1 109.85(3) 3_675 . ? P1 S2 Cu2 115.39(4) . . ? P1 S2 Cu1 80.87(4) . . ? Cu2 S2 Cu1 69.47(2) . . ? P1 S3 Cu1 113.11(4) 3_675 . ? P1 S3 Cu2 78.39(3) 3_675 . ? Cu1 S3 Cu2 66.26(2) . . ? C2 C1 C6 118.6(3) . . ? C2 C1 P1 119.7(2) . . ? C6 C1 P1 121.7(2) . . ? C1 C2 C3 120.9(3) . . ? C4 C3 C2 119.5(3) . . ? C5 C4 O1 114.5(3) . . ? C5 C4 C3 120.3(3) . . ? O1 C4 C3 125.2(4) . . ? C4 C5 C6 119.5(3) . . ? C5 C6 C1 121.2(3) . . ? C9 C8 C13 118.6(3) . . ? C9 C8 P2 121.7(2) . . ? C13 C8 P2 119.4(2) . . ? C8 C9 C10 120.3(3) . . ? C11 C10 C9 120.3(4) . . ? C10 C11 C12 120.2(3) . . ? C11 C12 C13 119.9(3) . . ? C8 C13 C12 120.7(3) . . ? C19 C14 C15 118.4(3) . . ? C19 C14 P2 123.3(2) . . ? C15 C14 P2 118.3(2) . . ? C16 C15 C14 120.3(3) . . ? C17 C16 C15 120.7(4) . . ? C16 C17 C18 119.7(3) . . ? C17 C18 C19 120.1(4) . . ? C18 C19 C14 120.8(3) . . ? C21 C20 C25 118.7(3) . . ? C21 C20 P2 124.3(2) . . ? C25 C20 P2 117.0(2) . . ? C22 C21 C20 120.7(3) . . ? C23 C22 C21 119.1(3) . . ? C24 C23 C22 120.7(3) . . ? C23 C24 C25 120.3(3) . . ? C24 C25 C20 120.4(3) . . ? C31 C26 C27 118.6(3) . . ? C31 C26 P3 117.2(2) . . ? C27 C26 P3 124.2(2) . . ? C28 C27 C26 120.1(3) . . ? C27 C28 C29 120.8(3) . . ? C30 C29 C28 119.5(3) . . ? C29 C30 C31 120.4(3) . . ? C30 C31 C26 120.6(3) . . ? C37 C32 C33 119.4(3) . . ? C37 C32 P3 123.0(2) . . ? C33 C32 P3 117.6(2) . . ? C34 C33 C32 119.8(3) . . ? C33 C34 C35 120.4(4) . . ? C36 C35 C34 119.9(3) . . ? C35 C36 C37 120.1(3) . . ? C36 C37 C32 120.4(3) . . ? C39 C38 C43 118.4(3) . . ? C39 C38 P3 118.3(2) . . ? C43 C38 P3 123.3(2) . . ? C38 C39 C40 121.0(3) . . ? C41 C40 C39 119.7(4) . . ? C40 C41 C42 120.1(3) . . ? C41 C42 C43 120.3(3) . . ? C42 C43 C38 120.5(3) . . ? Cl2A C44 Cl1 116.3(7) . . ? Cl2A C44 Cl2 20.8(18) . . ? Cl1 C44 Cl2 107.3(3) . . ? _diffrn_measured_fraction_theta_max 0.691 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.128 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.208 data_w1832 _database_code_depnum_ccdc_archive 'CCDC 276587' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C200 H216 Cu14 O28 P14 S14' _chemical_formula_weight 4839.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.1353(9) _cell_length_b 19.6186(10) _cell_length_c 20.0847(11) _cell_angle_alpha 95.756(4) _cell_angle_beta 111.961(4) _cell_angle_gamma 113.646(4) _cell_volume 5481.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 71109 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 54.05 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 1.625 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5220 _exptl_absorpt_correction_T_max 0.8810 _exptl_absorpt_process_details 'x-red 32' _exptl_special_details ; ? ; _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 'stoe ipds 2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42933 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.16 _reflns_number_total 21979 _reflns_number_gt 14349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1697P)^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 21979 _refine_ls_number_parameters 1098 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_ref 0.2526 _refine_ls_wR_factor_gt 0.2222 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.42002(6) 0.34089(5) 0.44109(5) 0.0469(2) Uani 1 1 d . . . Cu2 Cu 0.31320(6) 0.42127(5) 0.47034(5) 0.0465(2) Uani 1 1 d . . . Cu3 Cu 0.47227(6) 0.54273(5) 0.61737(5) 0.04539(19) Uani 1 1 d . . . Cu4 Cu 0.42689(7) 0.70049(5) 0.37376(5) 0.0554(2) Uani 1 1 d . . . Cu5 Cu 0.41101(6) 0.55161(5) 0.39367(5) 0.0505(2) Uani 1 1 d . . . Cu6 Cu 0.38382(7) 0.52940(5) 0.22798(5) 0.0546(2) Uani 1 1 d . . . Cu7 Cu 0.15700(7) 0.47786(7) 0.32587(6) 0.0627(3) Uani 1 1 d . . . S1 S 0.30986(12) 0.30905(10) 0.48443(9) 0.0448(3) Uani 1 1 d . . . S2 S 0.48697(12) 0.44129(9) 0.65318(9) 0.0442(3) Uani 1 1 d . . . S3 S 0.56017(12) 0.34879(10) 0.51930(10) 0.0462(4) Uani 1 1 d . . . S4 S 0.39144(12) 0.34351(10) 0.32314(9) 0.0455(3) Uani 1 1 d . . . S5 S 0.27630(11) 0.44033(10) 0.35623(9) 0.0454(3) Uani 1 1 d . . . S6 S 0.68010(11) 0.48523(10) 0.44979(9) 0.0443(3) Uani 1 1 d . . . S7 S 0.35076(17) 0.62858(15) 0.25255(13) 0.0709(5) Uani 1 1 d . . . P1 P 0.38600(12) 0.32484(10) 0.59797(10) 0.0451(4) Uani 1 1 d . . . P2 P 0.28360(12) 0.37328(10) 0.27425(9) 0.0449(4) Uani 1 1 d . . . P3 P 0.68186(12) 0.39969(10) 0.50276(10) 0.0443(4) Uani 1 1 d . . . P4 P 0.21014(18) 0.58444(16) 0.21059(13) 0.0702(6) Uani 1 1 d . . . P5 P 0.45584(14) 0.82169(11) 0.41511(11) 0.0520(4) Uani 1 1 d . . . P6 P 0.01106(15) 0.40127(15) 0.31040(17) 0.0747(6) Uani 1 1 d . . . P7 P 0.42372(15) 0.51456(12) 0.13591(10) 0.0550(4) Uani 1 1 d . . . O1 O 0.4320(4) 0.2732(3) 0.6116(3) 0.0533(11) Uani 1 1 d . . . O2 O 0.1100(7) 0.2287(5) 0.7257(6) 0.111(3) Uani 1 1 d . . . O3 O 0.2960(3) 0.4138(3) 0.2168(2) 0.0495(11) Uani 1 1 d . . . O4 O -0.0931(6) 0.0860(5) 0.1258(5) 0.120(3) Uani 1 1 d . . . O5 O 0.7720(3) 0.4284(3) 0.5749(3) 0.0495(10) Uani 1 1 d . . . O6 O 0.6761(5) 0.1662(4) 0.2844(4) 0.0756(16) Uani 1 1 d . . . O7 O 0.1581(5) 0.5348(5) 0.2476(4) 0.085(2) Uani 1 1 d . . . O8 O 0.0239(6) 0.4095(6) -0.1124(4) 0.105(3) Uani 1 1 d . . . O9 O 0.1867(6) 0.6575(5) 0.2169(4) 0.094(2) Uani 1 1 d . . . O10 O 0.2413(12) 0.7203(7) 0.1440(8) 0.168(6) Uani 1 1 d . . . C1 C 0.3008(5) 0.3002(4) 0.6350(4) 0.0518(16) Uani 1 1 d . . . C2 C 0.2520(7) 0.3387(6) 0.6371(6) 0.072(2) Uani 1 1 d . . . H2A H 0.2627 0.3822 0.6178 0.086 Uiso 1 1 calc R . . C3 C 0.1862(6) 0.3180(6) 0.6663(5) 0.071(2) Uani 1 1 d . . . H3A H 0.1528 0.3465 0.6671 0.085 Uiso 1 1 calc R . . C4 C 0.1714(8) 0.2548(6) 0.6936(6) 0.079(3) Uani 1 1 d . . . C5 C 0.2221(13) 0.2173(9) 0.6941(11) 0.139(7) Uani 1 1 d . . . H5A H 0.2128 0.1749 0.7149 0.167 Uiso 1 1 calc R . . C6 C 0.2869(10) 0.2380(6) 0.6655(8) 0.095(4) Uani 1 1 d . . . H6A H 0.3218 0.2104 0.6665 0.114 Uiso 1 1 calc R . . C7 C 0.0601(8) 0.2629(9) 0.7297(8) 0.105(4) Uani 1 1 d . . . H7A H 0.0207 0.2368 0.7535 0.157 Uiso 1 1 calc R . . H7B H 0.0187 0.2601 0.6790 0.157 Uiso 1 1 calc R . . H7C H 0.1033 0.3176 0.7596 0.157 Uiso 1 1 calc R . . C8 C 0.1709(5) 0.2837(4) 0.2289(4) 0.0514(15) Uani 1 1 d . . . C9 C 0.1195(6) 0.2618(5) 0.1522(5) 0.067(2) Uani 1 1 d . . . H9A H 0.1441 0.2929 0.1243 0.081 Uiso 1 1 calc R . . C10 C 0.0309(7) 0.1937(6) 0.1144(5) 0.088(3) Uani 1 1 d . . . H10A H -0.0029 0.1767 0.0611 0.106 Uiso 1 1 calc R . . C11 C -0.0058(7) 0.1521(6) 0.1564(6) 0.088(3) Uani 1 1 d . . . C12 C 0.0439(7) 0.1743(6) 0.2334(6) 0.087(3) Uani 1 1 d . . . H12A H 0.0177 0.1444 0.2613 0.105 Uiso 1 1 calc R . . C13 C 0.1329(6) 0.2408(5) 0.2704(5) 0.072(2) Uani 1 1 d . . . H13A H 0.1674 0.2567 0.3236 0.086 Uiso 1 1 calc R . . C14 C -0.1506(12) 0.0645(10) 0.0459(8) 0.176(10) Uani 1 1 d . . . H14A H -0.2110 0.0172 0.0304 0.264 Uiso 1 1 calc R . . H14B H -0.1161 0.0549 0.0199 0.264 Uiso 1 1 calc R . . H14C H -0.1639 0.1069 0.0330 0.264 Uiso 1 1 calc R . . C15 C 0.6734(5) 0.3262(4) 0.4360(4) 0.0472(14) Uani 1 1 d . . . C16 C 0.6008(6) 0.2925(5) 0.3628(4) 0.0575(17) Uani 1 1 d . . . H16A H 0.5505 0.3059 0.3481 0.069 Uiso 1 1 calc R . . C17 C 0.5998(7) 0.2406(5) 0.3113(5) 0.066(2) Uani 1 1 d . . . H17A H 0.5502 0.2195 0.2611 0.079 Uiso 1 1 calc R . . C18 C 0.6721(6) 0.2184(5) 0.3324(5) 0.0619(19) Uani 1 1 d . . . C19 C 0.7415(7) 0.2494(5) 0.4041(5) 0.067(2) Uani 1 1 d . . . H19A H 0.7900 0.2342 0.4192 0.080 Uiso 1 1 calc R . . C20 C 0.7438(5) 0.3021(5) 0.4555(4) 0.0543(16) Uani 1 1 d . . . H20A H 0.7939 0.3230 0.5054 0.065 Uiso 1 1 calc R . . C21 C 0.6073(12) 0.1361(9) 0.2086(7) 0.115(4) Uani 1 1 d . . . H21A H 0.6187 0.0996 0.1815 0.172 Uiso 1 1 calc R . . H21B H 0.6119 0.1788 0.1862 0.172 Uiso 1 1 calc R . . H21C H 0.5433 0.1089 0.2052 0.172 Uiso 1 1 calc R . . C22 C 0.1578(7) 0.5347(6) 0.1119(5) 0.070(2) Uani 1 1 d . . . C23 C 0.0740(7) 0.4645(7) 0.0825(5) 0.078(3) Uani 1 1 d . . . H23A H 0.0457 0.4445 0.1136 0.093 Uiso 1 1 calc R . . C24 C 0.0327(7) 0.4245(7) 0.0084(5) 0.081(3) Uani 1 1 d . . . H24A H -0.0240 0.3758 -0.0117 0.097 Uiso 1 1 calc R . . C25 C 0.0731(8) 0.4546(7) -0.0388(5) 0.082(3) Uani 1 1 d . . . C26 C 0.1557(8) 0.5239(7) -0.0104(6) 0.084(3) Uani 1 1 d . . . H26A H 0.1833 0.5448 -0.0416 0.101 Uiso 1 1 calc R . . C27 C 0.1993(7) 0.5643(6) 0.0684(5) 0.075(2) Uani 1 1 d . . . H27A H 0.2574 0.6120 0.0899 0.089 Uiso 1 1 calc R . . C28 C 0.0525(13) 0.4389(11) -0.1648(7) 0.134(6) Uani 1 1 d . . . H28A H 0.0126 0.3995 -0.2140 0.200 Uiso 1 1 calc R . . H28B H 0.1197 0.4521 -0.1487 0.200 Uiso 1 1 calc R . . H28C H 0.0454 0.4857 -0.1684 0.200 Uiso 1 1 calc R . . C29 C 0.1993(16) 0.7132(11) 0.1838(8) 0.134(6) Uani 1 1 d . . . C30 C 0.1542(12) 0.7623(9) 0.1951(9) 0.150(8) Uani 1 1 d . . . H30A H 0.1673 0.8025 0.1695 0.226 Uiso 1 1 calc R . . H30B H 0.1809 0.7871 0.2489 0.226 Uiso 1 1 calc R . . H30C H 0.0849 0.7293 0.1741 0.226 Uiso 1 1 calc R . . C31 C 0.5303(6) 0.8928(5) 0.3831(5) 0.0621(19) Uani 1 1 d . . . C32 C 0.5301(12) 0.8661(7) 0.3172(8) 0.109(5) Uani 1 1 d . . . H32A H 0.4906 0.8126 0.2892 0.131 Uiso 1 1 calc R . . C33 C 0.5881(14) 0.9175(7) 0.2907(10) 0.147(7) Uani 1 1 d . . . H33A H 0.5902 0.8986 0.2463 0.177 Uiso 1 1 calc R . . C34 C 0.6419(11) 0.9960(7) 0.3302(9) 0.111(4) Uani 1 1 d . . . H34A H 0.6783 1.0317 0.3113 0.133 Uiso 1 1 calc R . . C35 C 0.6426(8) 1.0220(6) 0.3957(7) 0.083(3) Uani 1 1 d . . . H35A H 0.6810 1.0757 0.4231 0.099 Uiso 1 1 calc R . . C36 C 0.5879(6) 0.9711(5) 0.4233(6) 0.067(2) Uani 1 1 d . . . H36A H 0.5899 0.9900 0.4697 0.080 Uiso 1 1 calc R . . C37 C 0.5265(5) 0.8565(4) 0.5170(4) 0.0551(17) Uani 1 1 d . . . C38 C 0.4960(6) 0.8811(5) 0.5654(5) 0.0617(19) Uani 1 1 d . . . H38A H 0.4389 0.8854 0.5458 0.074 Uiso 1 1 calc R . . C39 C 0.5504(8) 0.8999(6) 0.6439(6) 0.082(3) Uani 1 1 d . . . H39A H 0.5300 0.9172 0.6769 0.098 Uiso 1 1 calc R . . C40 C 0.6316(8) 0.8934(6) 0.6726(6) 0.085(3) Uani 1 1 d . . . H40A H 0.6686 0.9074 0.7255 0.102 Uiso 1 1 calc R . . C41 C 0.6607(7) 0.8660(6) 0.6244(6) 0.081(3) Uani 1 1 d . . . H41A H 0.7160 0.8593 0.6441 0.097 Uiso 1 1 calc R . . C42 C 0.6085(6) 0.8489(5) 0.5478(5) 0.067(2) Uani 1 1 d . . . H42A H 0.6295 0.8314 0.5153 0.081 Uiso 1 1 calc R . . C43 C 0.3553(6) 0.8397(5) 0.3992(5) 0.0593(18) Uani 1 1 d . . . C44 C 0.3525(6) 0.9074(5) 0.3869(5) 0.0626(19) Uani 1 1 d . . . H44A H 0.4046 0.9466 0.3833 0.075 Uiso 1 1 calc R . . C45 C 0.2751(7) 0.9190(6) 0.3797(6) 0.077(3) Uani 1 1 d . . . H45A H 0.2747 0.9657 0.3713 0.092 Uiso 1 1 calc R . . C46 C 0.1991(8) 0.8623(7) 0.3848(7) 0.093(3) Uani 1 1 d . . . H46A H 0.1462 0.8700 0.3803 0.111 Uiso 1 1 calc R . . C47 C 0.2001(9) 0.7943(8) 0.3966(9) 0.107(4) Uani 1 1 d . . . H47A H 0.1490 0.7566 0.4024 0.128 Uiso 1 1 calc R . . C48 C 0.2750(7) 0.7804(6) 0.4001(7) 0.085(3) Uani 1 1 d . . . H48A H 0.2719 0.7314 0.4030 0.102 Uiso 1 1 calc R . . C49 C -0.0822(5) 0.3578(5) 0.2115(5) 0.102(4) Uani 1 1 d G . . C50 C -0.1706(6) 0.3558(6) 0.1885(7) 0.193(11) Uani 1 1 d G . . H50A H -0.1848 0.3774 0.2241 0.232 Uiso 1 1 calc R . . C51 C -0.2381(5) 0.3222(7) 0.1134(8) 0.247(18) Uani 1 1 d G . . H51A H -0.2985 0.3208 0.0976 0.296 Uiso 1 1 calc R . . C52 C -0.2172(7) 0.2906(7) 0.0613(5) 0.230(17) Uani 1 1 d G . . H52A H -0.2634 0.2677 0.0100 0.276 Uiso 1 1 calc R . . C53 C -0.1289(8) 0.2926(6) 0.0844(5) 0.156(8) Uani 1 1 d G . . H53A H -0.1147 0.2710 0.0488 0.188 Uiso 1 1 calc R . . C54 C -0.0614(5) 0.3262(6) 0.1595(5) 0.113(4) Uani 1 1 d G . . H54A H -0.0010 0.3276 0.1752 0.136 Uiso 1 1 calc R . . C55 C -0.0291(6) 0.4572(6) 0.3537(7) 0.084(3) Uani 1 1 d . . . C56 C -0.0963(11) 0.4253(8) 0.3811(13) 0.150(8) Uani 1 1 d . . . H56A H -0.1233 0.3714 0.3776 0.180 Uiso 1 1 calc R . . C57 C -0.1229(14) 0.4717(10) 0.4128(14) 0.172(10) Uani 1 1 d . . . H57A H -0.1686 0.4491 0.4307 0.206 Uiso 1 1 calc R . . C58 C -0.0870(9) 0.5477(8) 0.4194(9) 0.109(4) Uani 1 1 d . . . H58A H -0.1058 0.5785 0.4427 0.130 Uiso 1 1 calc R . . C59 C -0.0212(7) 0.5818(6) 0.3916(6) 0.074(2) Uani 1 1 d . . . H59A H 0.0029 0.6352 0.3936 0.089 Uiso 1 1 calc R . . C60 C 0.0075(6) 0.5356(6) 0.3613(6) 0.070(2) Uani 1 1 d . . . H60A H 0.0547 0.5591 0.3449 0.084 Uiso 1 1 calc R . . C61 C -0.0087(7) 0.3173(6) 0.3482(8) 0.088(3) Uani 1 1 d . . . C62 C 0.0642(7) 0.3216(7) 0.4098(8) 0.097(4) Uani 1 1 d . . . H62A H 0.1247 0.3672 0.4326 0.116 Uiso 1 1 calc R . . C63 C 0.0503(9) 0.2602(8) 0.4389(9) 0.109(4) Uani 1 1 d . . . H63A H 0.1027 0.2663 0.4829 0.131 Uiso 1 1 calc R . . C64 C -0.0308(10) 0.1919(8) 0.4109(11) 0.126(6) Uani 1 1 d . . . H64A H -0.0375 0.1513 0.4339 0.151 Uiso 1 1 calc R . . C65 C -0.1081(9) 0.1858(7) 0.3418(10) 0.121(5) Uani 1 1 d . . . H65A H -0.1672 0.1389 0.3172 0.145 Uiso 1 1 calc R . . C66 C -0.0958(8) 0.2464(6) 0.3129(9) 0.109(5) Uani 1 1 d . . . H66A H -0.1464 0.2414 0.2681 0.130 Uiso 1 1 calc R . . C67 C 0.5322(6) 0.5040(5) 0.1654(4) 0.0612(19) Uani 1 1 d . . . C68 C 0.6074(6) 0.5462(6) 0.1495(5) 0.073(2) Uani 1 1 d . . . H68A H 0.6034 0.5827 0.1223 0.088 Uiso 1 1 calc R . . C69 C 0.6885(7) 0.5356(7) 0.1731(5) 0.083(3) Uani 1 1 d . . . H69A H 0.7386 0.5636 0.1610 0.100 Uiso 1 1 calc R . . C70 C 0.6950(9) 0.4829(8) 0.2151(5) 0.092(3) Uani 1 1 d . . . H70A H 0.7500 0.4755 0.2320 0.111 Uiso 1 1 calc R . . C71 C 0.6217(8) 0.4424(6) 0.2314(5) 0.075(2) Uani 1 1 d . . . H71A H 0.6261 0.4069 0.2598 0.090 Uiso 1 1 calc R . . C72 C 0.5415(7) 0.4527(6) 0.2070(5) 0.070(2) Uani 1 1 d . . . H72A H 0.4915 0.4240 0.2190 0.084 Uiso 1 1 calc R . . C73 C 0.3369(6) 0.4274(5) 0.0552(4) 0.061(2) Uani 1 1 d . . . C74 C 0.3639(7) 0.3912(5) 0.0104(5) 0.071(2) Uani 1 1 d . . . H74A H 0.4294 0.4117 0.0219 0.085 Uiso 1 1 calc R . . C75 C 0.2957(8) 0.3260(5) -0.0501(5) 0.078(3) Uani 1 1 d . . . H75A H 0.3145 0.3019 -0.0802 0.094 Uiso 1 1 calc R . . C76 C 0.2001(8) 0.2956(6) -0.0671(5) 0.078(3) Uani 1 1 d . . . H76A H 0.1535 0.2514 -0.1094 0.094 Uiso 1 1 calc R . . C77 C 0.1715(8) 0.3293(6) -0.0229(6) 0.086(3) Uani 1 1 d . . . H77A H 0.1058 0.3073 -0.0344 0.103 Uiso 1 1 calc R . . C78 C 0.2397(7) 0.3958(5) 0.0389(5) 0.072(2) Uani 1 1 d . . . H78A H 0.2207 0.4192 0.0693 0.087 Uiso 1 1 calc R . . C79 C 0.4483(5) 0.5953(4) 0.0952(4) 0.0557(17) Uani 1 1 d . . . C80 C 0.4235(6) 0.5864(5) 0.0191(4) 0.0597(18) Uani 1 1 d . . . H80A H 0.3896 0.5358 -0.0154 0.072 Uiso 1 1 calc R . . C81 C 0.4483(8) 0.6510(6) -0.0058(5) 0.076(2) Uani 1 1 d . . . H81A H 0.4342 0.6439 -0.0573 0.091 Uiso 1 1 calc R . . C82 C 0.4919(8) 0.7242(7) 0.0400(6) 0.090(3) Uani 1 1 d . . . H82A H 0.5044 0.7674 0.0204 0.108 Uiso 1 1 calc R . . C83 C 0.5180(10) 0.7353(6) 0.1160(7) 0.102(4) Uani 1 1 d . . . H83A H 0.5511 0.7863 0.1497 0.123 Uiso 1 1 calc R . . C84 C 0.4944(9) 0.6689(6) 0.1425(5) 0.089(3) Uani 1 1 d . . . H84A H 0.5111 0.6759 0.1944 0.107 Uiso 1 1 calc R . . O11 O 0.915(2) 1.0446(17) 0.5340(17) 0.289(11) Uiso 1 1 d . . . C85 C 0.957(2) 1.0374(19) 0.6002(18) 0.228(12) Uiso 1 1 d . . . H85A H 0.9457 1.0653 0.6368 0.273 Uiso 1 1 calc R . . H85B H 1.0264 1.0615 0.6169 0.273 Uiso 1 1 calc R . . C86 C 0.920(2) 0.9564(19) 0.5981(17) 0.223(12) Uiso 1 1 d . . . H86A H 0.9740 0.9444 0.6186 0.268 Uiso 1 1 calc R . . H86B H 0.8862 0.9455 0.6294 0.268 Uiso 1 1 calc R . . C87 C 0.859(2) 0.911(2) 0.5254(18) 0.234(12) Uiso 1 1 d . . . H87A H 0.8015 0.8677 0.5230 0.280 Uiso 1 1 calc R . . H87B H 0.8908 0.8884 0.5050 0.280 Uiso 1 1 calc R . . C88 C 0.832(2) 0.9590(18) 0.4820(18) 0.224(12) Uiso 1 1 d . . . H88A H 0.7686 0.9518 0.4739 0.269 Uiso 1 1 calc R . . H88B H 0.8321 0.9476 0.4327 0.269 Uiso 1 1 calc R . . O12 O 0.6959(10) 0.7633(8) 0.8894(8) 0.163(4) Uiso 1 1 d D . . C89 C 0.6112(13) 0.7679(11) 0.8821(13) 0.171(7) Uiso 1 1 d D . . H89A H 0.5945 0.7511 0.9220 0.205 Uiso 1 1 calc R . . H89B H 0.5566 0.7336 0.8327 0.205 Uiso 1 1 calc R . . C90 C 0.6329(14) 0.8518(11) 0.8893(12) 0.155(6) Uiso 1 1 d D . . H90A H 0.5831 0.8557 0.8469 0.186 Uiso 1 1 calc R . . H90B H 0.6379 0.8767 0.9371 0.186 Uiso 1 1 calc R . . C91 C 0.7238(15) 0.8869(11) 0.8876(13) 0.164(7) Uiso 1 1 d D . . H91A H 0.7185 0.9135 0.8480 0.197 Uiso 1 1 calc R . . H91B H 0.7726 0.9268 0.9363 0.197 Uiso 1 1 calc R . . C92 C 0.7542(8) 0.8334(7) 0.8739(7) 0.149(6) Uiso 1 1 d D . . H92A H 0.8231 0.8541 0.9074 0.179 Uiso 1 1 calc R . . H92B H 0.7431 0.8210 0.8211 0.179 Uiso 1 1 calc R . . O13 O 0.3052(8) 0.0757(7) 0.8890(7) 0.206(6) Uiso 1 1 d RD . . C93 C 0.2737(8) 0.0206(7) 0.8224(7) 0.166(7) Uiso 1 1 d RD . . H93B H 0.2442 -0.0324 0.8269 0.199 Uiso 1 1 calc R . . H93A H 0.3288 0.0277 0.8130 0.199 Uiso 1 1 calc R . . C94 C 0.2026(13) 0.0298(12) 0.7586(10) 0.150(6) Uiso 1 1 d D . . H94B H 0.2334 0.0657 0.7342 0.180 Uiso 1 1 calc R . . H94A H 0.1527 -0.0209 0.7206 0.180 Uiso 1 1 calc R . . C95 C 0.1643(17) 0.0630(16) 0.7987(13) 0.207(10) Uiso 1 1 d D . . H95B H 0.1385 0.0942 0.7710 0.249 Uiso 1 1 calc R . . H95A H 0.1122 0.0211 0.8037 0.249 Uiso 1 1 calc R . . C96 C 0.2384(16) 0.1095(13) 0.8683(12) 0.188(9) Uiso 1 1 d D . . H96B H 0.2139 0.1105 0.9057 0.226 Uiso 1 1 calc R . . H96A H 0.2718 0.1634 0.8669 0.226 Uiso 1 1 calc R . . O14 O 0.9783(17) 0.1326(14) 0.8509(14) 0.243(8) Uiso 1 1 d . . . C97 C 0.9927(17) 0.1105(14) 0.9174(13) 0.173(8) Uiso 1 1 d . . . H97A H 0.9517 0.1191 0.9376 0.208 Uiso 1 1 calc R . . H97B H 1.0602 0.1434 0.9555 0.208 Uiso 1 1 calc R . . C98 C 0.9701(19) 0.0289(15) 0.9035(14) 0.187(9) Uiso 1 1 d . . . H98A H 0.9316 0.0023 0.9284 0.224 Uiso 1 1 calc R . . H98B H 1.0290 0.0237 0.9216 0.224 Uiso 1 1 calc R . . C99 C 0.9118(17) -0.0045(14) 0.8169(13) 0.171(8) Uiso 1 1 d . . . H99A H 0.9382 -0.0329 0.7964 0.205 Uiso 1 1 calc R . . H99B H 0.8440 -0.0406 0.8021 0.205 Uiso 1 1 calc R . . C100 C 0.920(3) 0.059(2) 0.792(2) 0.256(14) Uiso 1 1 d . . . H10B H 0.8554 0.0529 0.7628 0.307 Uiso 1 1 calc R . . H10C H 0.9486 0.0602 0.7566 0.307 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 Cu1 0.0500(4) 0.0476(4) 0.0485(4) 0.0132(4) 0.0260(4) 0.0249(4) Cu2 0.0513(4) 0.0448(4) 0.0521(4) 0.0151(4) 0.0275(4) 0.0268(4) Cu3 0.0471(4) 0.0462(4) 0.0494(4) 0.0145(4) 0.0238(3) 0.0261(3) Cu4 0.0630(5) 0.0484(5) 0.0603(5) 0.0162(4) 0.0254(4) 0.0338(4) Cu5 0.0490(4) 0.0500(5) 0.0546(5) 0.0107(4) 0.0260(4) 0.0242(4) Cu6 0.0618(5) 0.0533(5) 0.0478(4) 0.0169(4) 0.0246(4) 0.0264(4) Cu7 0.0533(5) 0.0726(6) 0.0586(5) 0.0069(5) 0.0196(4) 0.0350(5) S1 0.0483(8) 0.0418(8) 0.0502(8) 0.0138(7) 0.0271(7) 0.0221(7) S2 0.0497(8) 0.0421(8) 0.0451(8) 0.0127(7) 0.0232(7) 0.0243(7) S3 0.0488(8) 0.0447(8) 0.0510(8) 0.0146(7) 0.0263(7) 0.0239(7) S4 0.0496(8) 0.0450(8) 0.0464(8) 0.0103(7) 0.0252(7) 0.0240(7) S5 0.0455(8) 0.0494(9) 0.0473(8) 0.0130(7) 0.0241(7) 0.0253(7) S6 0.0448(8) 0.0457(8) 0.0501(8) 0.0139(7) 0.0255(7) 0.0249(7) S7 0.0728(13) 0.0750(14) 0.0678(12) 0.0181(11) 0.0273(10) 0.0425(11) P1 0.0522(9) 0.0415(8) 0.0501(9) 0.0158(7) 0.0282(7) 0.0245(7) P2 0.0442(8) 0.0455(9) 0.0438(8) 0.0090(7) 0.0210(7) 0.0201(7) P3 0.0479(9) 0.0463(9) 0.0473(8) 0.0129(7) 0.0241(7) 0.0280(7) P4 0.0778(14) 0.0787(15) 0.0607(12) 0.0162(11) 0.0288(11) 0.0464(12) P5 0.0594(10) 0.0437(9) 0.0627(10) 0.0193(8) 0.0294(9) 0.0308(8) P6 0.0462(10) 0.0647(13) 0.1014(18) 0.0050(13) 0.0262(11) 0.0269(10) P7 0.0639(11) 0.0546(10) 0.0417(8) 0.0155(8) 0.0237(8) 0.0238(9) O1 0.065(3) 0.051(3) 0.064(3) 0.025(2) 0.035(2) 0.037(2) O2 0.124(7) 0.101(6) 0.152(8) 0.043(6) 0.114(6) 0.045(5) O3 0.051(3) 0.055(3) 0.041(2) 0.012(2) 0.022(2) 0.023(2) O4 0.079(5) 0.080(5) 0.114(6) 0.006(4) 0.026(5) -0.018(4) O5 0.052(3) 0.054(3) 0.051(2) 0.012(2) 0.024(2) 0.032(2) O6 0.094(4) 0.066(4) 0.082(4) 0.009(3) 0.047(4) 0.048(3) O7 0.075(4) 0.124(6) 0.066(4) 0.041(4) 0.036(3) 0.050(4) O8 0.107(6) 0.151(8) 0.053(3) 0.013(4) 0.023(4) 0.074(6) O9 0.098(5) 0.100(5) 0.085(5) 0.016(4) 0.023(4) 0.068(5) O10 0.282(18) 0.106(8) 0.142(10) 0.050(8) 0.094(11) 0.116(10) C1 0.054(4) 0.051(4) 0.056(4) 0.016(3) 0.030(3) 0.025(3) C2 0.082(6) 0.077(6) 0.092(6) 0.043(5) 0.058(5) 0.048(5) C3 0.070(5) 0.083(6) 0.083(6) 0.029(5) 0.052(5) 0.038(5) C4 0.090(6) 0.069(6) 0.096(7) 0.030(5) 0.067(6) 0.028(5) C5 0.212(17) 0.109(10) 0.230(18) 0.109(12) 0.190(16) 0.098(11) C6 0.139(10) 0.066(6) 0.146(10) 0.056(7) 0.109(9) 0.061(6) C7 0.070(6) 0.145(12) 0.106(8) 0.049(9) 0.044(6) 0.050(7) C8 0.049(4) 0.044(4) 0.053(4) 0.008(3) 0.022(3) 0.017(3) C9 0.051(4) 0.064(5) 0.060(4) 0.012(4) 0.020(3) 0.011(4) C10 0.078(6) 0.074(6) 0.055(5) 0.000(4) 0.011(4) 0.008(5) C11 0.064(5) 0.064(5) 0.088(7) 0.009(5) 0.024(5) 0.000(4) C12 0.066(5) 0.066(6) 0.086(6) 0.019(5) 0.032(5) -0.005(4) C13 0.060(5) 0.063(5) 0.067(5) 0.015(4) 0.026(4) 0.011(4) C14 0.114(11) 0.126(12) 0.105(10) 0.015(9) -0.010(9) -0.046(10) C15 0.057(4) 0.048(4) 0.054(4) 0.018(3) 0.032(3) 0.032(3) C16 0.065(4) 0.057(4) 0.059(4) 0.018(4) 0.027(4) 0.037(4) C17 0.076(5) 0.058(5) 0.065(5) 0.005(4) 0.031(4) 0.038(4) C18 0.081(5) 0.048(4) 0.072(5) 0.016(4) 0.048(4) 0.033(4) C19 0.079(5) 0.066(5) 0.079(5) 0.017(5) 0.044(5) 0.050(4) C20 0.060(4) 0.057(4) 0.055(4) 0.015(3) 0.027(3) 0.036(3) C21 0.156(13) 0.106(9) 0.101(9) -0.002(7) 0.062(9) 0.082(9) C22 0.076(5) 0.084(6) 0.061(5) 0.024(5) 0.030(4) 0.048(5) C23 0.071(6) 0.099(7) 0.066(5) 0.028(5) 0.027(4) 0.045(5) C24 0.074(6) 0.092(7) 0.063(5) 0.008(5) 0.027(4) 0.036(5) C25 0.080(6) 0.116(9) 0.053(4) 0.015(5) 0.026(4) 0.057(6) C26 0.088(7) 0.110(8) 0.073(6) 0.025(6) 0.042(5) 0.059(7) C27 0.064(5) 0.085(6) 0.068(5) 0.017(5) 0.025(4) 0.037(5) C28 0.173(15) 0.189(17) 0.069(7) 0.026(9) 0.068(9) 0.103(13) C29 0.199(18) 0.116(12) 0.074(8) 0.016(8) 0.046(10) 0.080(12) C30 0.158(14) 0.122(11) 0.114(10) -0.023(9) -0.018(10) 0.102(11) C31 0.071(5) 0.053(4) 0.077(5) 0.026(4) 0.040(4) 0.036(4) C32 0.193(14) 0.065(6) 0.122(9) 0.041(6) 0.119(10) 0.062(8) C33 0.26(2) 0.066(7) 0.179(14) 0.041(8) 0.183(16) 0.049(9) C34 0.149(12) 0.067(7) 0.156(12) 0.044(7) 0.116(11) 0.042(7) C35 0.086(6) 0.059(5) 0.123(8) 0.034(6) 0.064(6) 0.036(5) C36 0.063(5) 0.055(4) 0.084(6) 0.020(4) 0.037(4) 0.026(4) C37 0.060(4) 0.039(3) 0.064(4) 0.018(3) 0.024(3) 0.026(3) C38 0.064(5) 0.055(4) 0.067(5) 0.024(4) 0.033(4) 0.025(4) C39 0.102(7) 0.069(6) 0.081(6) 0.027(5) 0.054(6) 0.034(5) C40 0.082(6) 0.072(6) 0.072(6) 0.026(5) 0.016(5) 0.028(5) C41 0.073(6) 0.067(5) 0.072(6) 0.014(5) 0.005(5) 0.033(5) C42 0.063(5) 0.050(4) 0.072(5) 0.007(4) 0.015(4) 0.030(4) C43 0.068(5) 0.056(4) 0.062(4) 0.023(4) 0.029(4) 0.036(4) C44 0.064(5) 0.048(4) 0.074(5) 0.017(4) 0.026(4) 0.032(4) C45 0.069(5) 0.064(5) 0.094(7) 0.024(5) 0.024(5) 0.040(4) C46 0.082(7) 0.110(9) 0.116(9) 0.045(8) 0.047(6) 0.068(7) C47 0.087(7) 0.117(9) 0.167(12) 0.086(10) 0.071(8) 0.071(7) C48 0.073(6) 0.082(6) 0.129(9) 0.061(7) 0.056(6) 0.048(5) C49 0.060(6) 0.075(7) 0.130(10) 0.001(7) 0.009(6) 0.034(5) C50 0.069(8) 0.113(11) 0.26(2) -0.043(13) -0.031(11) 0.045(8) C51 0.119(14) 0.114(14) 0.28(3) -0.039(16) -0.094(18) 0.051(12) C52 0.142(17) 0.101(12) 0.21(2) -0.011(13) -0.097(16) 0.020(11) C53 0.136(14) 0.100(10) 0.112(11) 0.000(8) -0.020(10) 0.026(9) C54 0.086(8) 0.101(9) 0.094(8) 0.010(7) -0.005(6) 0.040(7) C55 0.055(5) 0.077(6) 0.129(9) 0.022(6) 0.045(5) 0.037(4) C56 0.138(11) 0.088(8) 0.34(3) 0.104(13) 0.189(16) 0.074(8) C57 0.203(17) 0.129(12) 0.38(3) 0.150(18) 0.25(2) 0.131(13) C58 0.108(9) 0.090(8) 0.192(14) 0.057(9) 0.107(10) 0.067(7) C59 0.069(5) 0.076(6) 0.096(7) 0.027(5) 0.048(5) 0.041(5) C60 0.059(5) 0.074(6) 0.090(6) 0.021(5) 0.039(4) 0.038(4) C61 0.055(5) 0.061(5) 0.138(9) 0.004(6) 0.042(6) 0.026(4) C62 0.060(6) 0.080(7) 0.144(10) 0.012(7) 0.053(6) 0.027(5) C63 0.088(8) 0.114(10) 0.153(12) 0.061(10) 0.070(8) 0.054(7) C64 0.101(9) 0.081(8) 0.223(18) 0.052(10) 0.090(11) 0.052(7) C65 0.073(7) 0.057(6) 0.211(16) 0.020(8) 0.060(9) 0.021(5) C66 0.058(6) 0.061(6) 0.177(13) 0.018(7) 0.036(7) 0.021(5) C67 0.068(5) 0.068(5) 0.041(3) 0.016(3) 0.025(3) 0.026(4) C68 0.062(5) 0.090(6) 0.058(4) 0.022(5) 0.023(4) 0.031(5) C69 0.069(6) 0.111(8) 0.060(5) 0.016(5) 0.022(4) 0.043(6) C70 0.111(8) 0.131(10) 0.055(5) 0.024(6) 0.031(5) 0.083(8) C71 0.103(7) 0.081(6) 0.064(5) 0.028(5) 0.045(5) 0.055(6) C72 0.096(6) 0.072(5) 0.058(4) 0.022(4) 0.044(5) 0.045(5) C73 0.066(5) 0.056(4) 0.046(4) 0.017(3) 0.018(3) 0.022(4) C74 0.085(6) 0.059(5) 0.059(4) 0.015(4) 0.033(4) 0.025(4) C75 0.101(7) 0.059(5) 0.061(5) 0.008(4) 0.034(5) 0.030(5) C76 0.090(7) 0.058(5) 0.060(5) 0.006(4) 0.020(5) 0.027(5) C77 0.074(6) 0.063(5) 0.083(6) 0.010(5) 0.012(5) 0.023(5) C78 0.069(5) 0.066(5) 0.065(5) 0.019(4) 0.016(4) 0.030(4) C79 0.060(4) 0.050(4) 0.055(4) 0.018(3) 0.026(3) 0.024(3) C80 0.069(5) 0.060(4) 0.054(4) 0.021(4) 0.027(4) 0.035(4) C81 0.093(7) 0.080(6) 0.067(5) 0.033(5) 0.039(5) 0.047(5) C82 0.103(8) 0.077(7) 0.091(7) 0.045(6) 0.048(6) 0.035(6) C83 0.141(11) 0.050(5) 0.098(8) 0.019(5) 0.067(8) 0.018(6) C84 0.126(9) 0.061(5) 0.061(5) 0.008(4) 0.048(6) 0.024(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S4 2.2430(18) . ? Cu1 S3 2.2561(18) . ? Cu1 S1 2.2590(17) . ? Cu1 Cu3 2.9624(11) 2_666 ? Cu1 Cu2 3.0193(12) . ? Cu2 S1 2.2286(18) . ? Cu2 S6 2.2481(19) 2_666 ? Cu2 S5 2.2515(17) . ? Cu2 Cu3 3.0308(13) . ? Cu3 S6 2.2372(18) 2_666 ? Cu3 S4 2.2494(19) 2_666 ? Cu3 S2 2.2573(17) . ? Cu3 Cu1 2.9624(11) 2_666 ? Cu4 O1 2.153(5) 2_666 ? Cu4 P5 2.222(2) . ? Cu4 S7 2.254(3) . ? Cu4 S3 2.4144(18) 2_666 ? Cu4 Cu5 2.9057(12) . ? Cu5 S5 2.2339(19) . ? Cu5 S3 2.239(2) 2_666 ? Cu5 S2 2.2410(18) 2_666 ? Cu6 O3 2.089(5) . ? Cu6 P7 2.229(2) . ? Cu6 S7 2.291(3) . ? Cu6 S2 2.3834(18) 2_666 ? Cu7 O7 2.020(6) . ? Cu7 O5 2.119(5) 2_666 ? Cu7 P6 2.218(2) . ? Cu7 S5 2.3363(19) . ? S1 P1 2.075(2) . ? S2 P1 2.080(2) . ? S2 Cu5 2.2410(18) 2_666 ? S2 Cu6 2.3834(18) 2_666 ? S3 P3 2.090(2) . ? S3 Cu5 2.239(2) 2_666 ? S3 Cu4 2.4143(18) 2_666 ? S4 P2 2.084(2) . ? S4 Cu3 2.2494(19) 2_666 ? S5 P2 2.076(2) . ? S6 P3 2.080(2) . ? S6 Cu3 2.2372(18) 2_666 ? S6 Cu2 2.2480(19) 2_666 ? S7 P4 1.982(3) . ? P1 O1 1.503(5) . ? P1 C1 1.799(7) . ? P2 O3 1.497(5) . ? P2 C8 1.813(7) . ? P3 O5 1.505(5) . ? P3 C15 1.788(7) . ? P4 O7 1.497(7) . ? P4 O9 1.642(8) . ? P4 C22 1.808(10) . ? P5 C43 1.815(8) . ? P5 C37 1.824(8) . ? P5 C31 1.831(8) . ? P6 C55 1.815(11) . ? P6 C61 1.845(12) . ? P6 C49 1.849(7) . ? P7 C79 1.826(7) . ? P7 C67 1.834(9) . ? P7 C73 1.834(8) . ? O1 Cu4 2.153(5) 2_666 ? O2 C7 1.300(15) . ? O2 C4 1.388(10) . ? O4 C11 1.377(11) . ? O4 C14 1.440(16) . ? O5 Cu7 2.119(5) 2_666 ? O6 C18 1.376(11) . ? O6 C21 1.405(15) . ? O8 C25 1.372(12) . ? O8 C28 1.402(15) . ? O9 C29 1.322(19) . ? O10 C29 1.24(2) . ? C1 C2 1.340(12) . ? C1 C6 1.397(11) . ? C2 C3 1.398(11) . ? C3 C4 1.376(13) . ? C4 C5 1.343(17) . ? C5 C6 1.376(15) . ? C8 C9 1.373(11) . ? C8 C13 1.390(11) . ? C9 C10 1.405(12) . ? C10 C11 1.377(14) . ? C11 C12 1.374(15) . ? C12 C13 1.393(12) . ? C15 C16 1.388(11) . ? C15 C20 1.403(10) . ? C16 C17 1.368(12) . ? C17 C18 1.407(12) . ? C18 C19 1.350(13) . ? C19 C20 1.364(12) . ? C22 C27 1.357(13) . ? C22 C23 1.386(14) . ? C23 C24 1.366(14) . ? C24 C25 1.415(14) . ? C25 C26 1.369(16) . ? C26 C27 1.441(14) . ? C29 C30 1.50(2) . ? C31 C32 1.374(14) . ? C31 C36 1.387(12) . ? C32 C33 1.409(14) . ? C33 C34 1.386(18) . ? C34 C35 1.357(17) . ? C35 C36 1.389(12) . ? C37 C42 1.384(11) . ? C37 C38 1.393(12) . ? C38 C39 1.415(13) . ? C39 C40 1.357(16) . ? C40 C41 1.395(16) . ? C41 C42 1.380(13) . ? C43 C44 1.391(11) . ? C43 C48 1.408(12) . ? C44 C45 1.392(12) . ? C45 C46 1.380(15) . ? C46 C47 1.383(15) . ? C47 C48 1.395(14) . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C55 C60 1.376(14) . ? C55 C56 1.410(14) . ? C56 C57 1.371(19) . ? C57 C58 1.334(18) . ? C58 C59 1.404(14) . ? C59 C60 1.380(13) . ? C61 C62 1.355(17) . ? C61 C66 1.418(14) . ? C62 C63 1.365(17) . ? C63 C64 1.347(19) . ? C64 C65 1.47(2) . ? C65 C66 1.350(18) . ? C67 C72 1.391(11) . ? C67 C68 1.398(12) . ? C68 C69 1.399(14) . ? C69 C70 1.412(15) . ? C70 C71 1.370(16) . ? C71 C72 1.381(14) . ? C73 C74 1.403(13) . ? C73 C78 1.411(13) . ? C74 C75 1.381(13) . ? C75 C76 1.383(15) . ? C76 C77 1.390(16) . ? C77 C78 1.406(14) . ? C79 C84 1.364(12) . ? C79 C80 1.397(11) . ? C80 C81 1.375(12) . ? C81 C82 1.352(15) . ? C82 C83 1.387(15) . ? C83 C84 1.422(14) . ? O11 C85 1.31(3) . ? O11 C88 1.60(3) . ? C85 C86 1.45(4) . ? C86 C87 1.37(4) . ? C87 C88 1.44(3) . ? O12 C89 1.443(15) . ? O12 C92 1.484(14) . ? C89 C90 1.514(19) . ? C90 C91 1.44(2) . ? C91 C92 1.39(2) . ? O13 C93 1.3979 . ? O13 C96 1.492(18) . ? C93 C94 1.487(17) . ? C94 C95 1.46(2) . ? C95 C96 1.37(2) . ? O14 C97 1.41(2) . ? O14 C100 1.45(4) . ? C97 C98 1.46(3) . ? C98 C99 1.55(3) . ? C99 C100 1.37(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Cu1 S3 119.14(7) . . ? S4 Cu1 S1 125.18(7) . . ? S3 Cu1 S1 114.72(7) . . ? S4 Cu1 Cu3 48.84(5) . 2_666 ? S3 Cu1 Cu3 87.79(5) . 2_666 ? S1 Cu1 Cu3 144.44(6) . 2_666 ? S4 Cu1 Cu2 100.29(5) . . ? S3 Cu1 Cu2 129.62(6) . . ? S1 Cu1 Cu2 47.29(5) . . ? Cu3 Cu1 Cu2 97.18(3) 2_666 . ? S1 Cu2 S6 128.56(7) . 2_666 ? S1 Cu2 S5 119.67(7) . . ? S6 Cu2 S5 110.55(7) 2_666 . ? S1 Cu2 Cu1 48.15(5) . . ? S6 Cu2 Cu1 145.74(6) 2_666 . ? S5 Cu2 Cu1 89.88(5) . . ? S1 Cu2 Cu3 104.98(5) . . ? S6 Cu2 Cu3 47.34(5) 2_666 . ? S5 Cu2 Cu3 125.20(6) . . ? Cu1 Cu2 Cu3 98.45(3) . . ? S6 Cu3 S4 132.04(7) 2_666 2_666 ? S6 Cu3 S2 112.90(7) 2_666 . ? S4 Cu3 S2 113.43(7) 2_666 . ? S6 Cu3 Cu1 104.53(5) 2_666 2_666 ? S4 Cu3 Cu1 48.65(5) 2_666 2_666 ? S2 Cu3 Cu1 131.90(5) . 2_666 ? S6 Cu3 Cu2 47.64(5) 2_666 . ? S4 Cu3 Cu2 148.24(5) 2_666 . ? S2 Cu3 Cu2 85.05(5) . . ? Cu1 Cu3 Cu2 99.66(3) 2_666 . ? O1 Cu4 P5 97.88(15) 2_666 . ? O1 Cu4 S7 95.30(16) 2_666 . ? P5 Cu4 S7 126.00(9) . . ? O1 Cu4 S3 95.39(13) 2_666 2_666 ? P5 Cu4 S3 104.28(8) . 2_666 ? S7 Cu4 S3 126.25(8) . 2_666 ? O1 Cu4 Cu5 84.73(13) 2_666 . ? P5 Cu4 Cu5 152.91(7) . . ? S7 Cu4 Cu5 80.24(7) . . ? S3 Cu4 Cu5 48.70(5) 2_666 . ? S5 Cu5 S3 117.39(7) . 2_666 ? S5 Cu5 S2 119.81(7) . 2_666 ? S3 Cu5 S2 122.77(7) 2_666 2_666 ? S5 Cu5 Cu4 126.90(6) . . ? S3 Cu5 Cu4 54.12(5) 2_666 . ? S2 Cu5 Cu4 91.46(5) 2_666 . ? O3 Cu6 P7 101.36(15) . . ? O3 Cu6 S7 123.26(16) . . ? P7 Cu6 S7 120.71(9) . . ? O3 Cu6 S2 98.40(13) . 2_666 ? P7 Cu6 S2 110.60(8) . 2_666 ? S7 Cu6 S2 100.04(8) . 2_666 ? O7 Cu7 O5 101.4(3) . 2_666 ? O7 Cu7 P6 113.3(2) . . ? O5 Cu7 P6 108.43(15) 2_666 . ? O7 Cu7 S5 110.4(2) . . ? O5 Cu7 S5 96.55(13) 2_666 . ? P6 Cu7 S5 123.04(9) . . ? P1 S1 Cu2 108.31(9) . . ? P1 S1 Cu1 104.72(9) . . ? Cu2 S1 Cu1 84.56(6) . . ? P1 S2 Cu5 98.45(9) . 2_666 ? P1 S2 Cu3 124.74(9) . . ? Cu5 S2 Cu3 93.27(6) 2_666 . ? P1 S2 Cu6 117.50(8) . 2_666 ? Cu5 S2 Cu6 85.52(6) 2_666 2_666 ? Cu3 S2 Cu6 117.14(8) . 2_666 ? P3 S3 Cu5 100.38(9) . 2_666 ? P3 S3 Cu1 121.59(9) . . ? Cu5 S3 Cu1 91.44(7) 2_666 . ? P3 S3 Cu4 118.28(9) . 2_666 ? Cu5 S3 Cu4 77.18(6) 2_666 2_666 ? Cu1 S3 Cu4 120.12(7) . 2_666 ? P2 S4 Cu1 111.86(9) . . ? P2 S4 Cu3 105.40(9) . 2_666 ? Cu1 S4 Cu3 82.51(6) . 2_666 ? P2 S5 Cu5 100.77(8) . . ? P2 S5 Cu2 119.87(9) . . ? Cu5 S5 Cu2 95.37(7) . . ? P2 S5 Cu7 121.37(9) . . ? Cu5 S5 Cu7 104.22(8) . . ? Cu2 S5 Cu7 109.48(7) . . ? P3 S6 Cu3 108.27(8) . 2_666 ? P3 S6 Cu2 106.18(9) . 2_666 ? Cu3 S6 Cu2 85.02(6) 2_666 2_666 ? P4 S7 Cu4 111.88(14) . . ? P4 S7 Cu6 108.24(14) . . ? Cu4 S7 Cu6 115.71(10) . . ? O1 P1 C1 109.0(3) . . ? O1 P1 S1 112.4(2) . . ? C1 P1 S1 106.2(3) . . ? O1 P1 S2 111.0(2) . . ? C1 P1 S2 107.5(3) . . ? S1 P1 S2 110.46(9) . . ? O3 P2 C8 109.0(3) . . ? O3 P2 S5 111.1(2) . . ? C8 P2 S5 106.7(3) . . ? O3 P2 S4 112.1(2) . . ? C8 P2 S4 107.4(3) . . ? S5 P2 S4 110.45(10) . . ? O5 P3 C15 109.9(3) . . ? O5 P3 S6 113.1(2) . . ? C15 P3 S6 104.2(2) . . ? O5 P3 S3 111.4(2) . . ? C15 P3 S3 106.8(2) . . ? S6 P3 S3 111.07(10) . . ? O7 P4 O9 102.4(5) . . ? O7 P4 C22 110.7(5) . . ? O9 P4 C22 107.4(4) . . ? O7 P4 S7 120.1(3) . . ? O9 P4 S7 107.7(3) . . ? C22 P4 S7 107.9(3) . . ? C43 P5 C37 103.7(4) . . ? C43 P5 C31 105.9(4) . . ? C37 P5 C31 103.4(4) . . ? C43 P5 Cu4 118.6(3) . . ? C37 P5 Cu4 109.2(2) . . ? C31 P5 Cu4 114.4(3) . . ? C55 P6 C61 104.8(5) . . ? C55 P6 C49 103.7(5) . . ? C61 P6 C49 103.5(5) . . ? C55 P6 Cu7 110.1(3) . . ? C61 P6 Cu7 118.7(3) . . ? C49 P6 Cu7 114.6(3) . . ? C79 P7 C67 104.1(4) . . ? C79 P7 C73 104.8(3) . . ? C67 P7 C73 101.9(4) . . ? C79 P7 Cu6 115.0(3) . . ? C67 P7 Cu6 113.4(2) . . ? C73 P7 Cu6 116.1(3) . . ? P1 O1 Cu4 127.4(3) . 2_666 ? C7 O2 C4 120.4(10) . . ? P2 O3 Cu6 131.4(3) . . ? C11 O4 C14 116.4(10) . . ? P3 O5 Cu7 133.6(3) . 2_666 ? C18 O6 C21 118.6(8) . . ? P4 O7 Cu7 150.5(4) . . ? C25 O8 C28 119.0(11) . . ? C29 O9 P4 130.8(11) . . ? C2 C1 C6 118.1(8) . . ? C2 C1 P1 124.6(6) . . ? C6 C1 P1 117.3(7) . . ? C1 C2 C3 123.1(8) . . ? C4 C3 C2 117.6(9) . . ? C5 C4 C3 119.9(8) . . ? C5 C4 O2 116.1(9) . . ? C3 C4 O2 123.9(10) . . ? C4 C5 C6 122.3(10) . . ? C5 C6 C1 119.0(11) . . ? C9 C8 C13 119.9(7) . . ? C9 C8 P2 118.4(5) . . ? C13 C8 P2 121.5(6) . . ? C8 C9 C10 120.7(8) . . ? C11 C10 C9 118.4(8) . . ? C12 C11 O4 114.9(9) . . ? C12 C11 C10 121.5(8) . . ? O4 C11 C10 123.6(10) . . ? C11 C12 C13 119.7(8) . . ? C8 C13 C12 119.6(8) . . ? C16 C15 C20 116.8(7) . . ? C16 C15 P3 122.7(5) . . ? C20 C15 P3 120.4(6) . . ? C17 C16 C15 121.6(7) . . ? C16 C17 C18 120.1(8) . . ? C19 C18 O6 117.6(8) . . ? C19 C18 C17 118.5(8) . . ? O6 C18 C17 123.9(8) . . ? C18 C19 C20 121.7(8) . . ? C19 C20 C15 121.2(8) . . ? C27 C22 C23 121.3(9) . . ? C27 C22 P4 121.4(8) . . ? C23 C22 P4 117.3(7) . . ? C24 C23 C22 119.3(9) . . ? C23 C24 C25 120.8(10) . . ? C26 C25 O8 124.5(10) . . ? C26 C25 C24 120.3(9) . . ? O8 C25 C24 115.2(10) . . ? C25 C26 C27 117.9(9) . . ? C22 C27 C26 120.4(10) . . ? O10 C29 O9 121.2(18) . . ? O10 C29 C30 124.4(17) . . ? O9 C29 C30 114.3(17) . . ? C32 C31 C36 119.3(8) . . ? C32 C31 P5 117.6(7) . . ? C36 C31 P5 123.0(7) . . ? C31 C32 C33 120.4(11) . . ? C34 C33 C32 119.2(11) . . ? C35 C34 C33 120.1(10) . . ? C34 C35 C36 120.9(10) . . ? C31 C36 C35 120.1(9) . . ? C42 C37 C38 118.4(8) . . ? C42 C37 P5 118.0(7) . . ? C38 C37 P5 123.1(6) . . ? C37 C38 C39 119.7(9) . . ? C40 C39 C38 120.6(11) . . ? C39 C40 C41 119.9(10) . . ? C42 C41 C40 119.5(10) . . ? C41 C42 C37 121.8(10) . . ? C44 C43 C48 118.4(8) . . ? C44 C43 P5 124.8(6) . . ? C48 C43 P5 116.9(6) . . ? C43 C44 C45 121.5(8) . . ? C46 C45 C44 119.6(8) . . ? C45 C46 C47 119.9(9) . . ? C46 C47 C48 121.0(10) . . ? C47 C48 C43 119.4(9) . . ? C50 C49 C54 120.0 . . ? C50 C49 P6 122.5(5) . . ? C54 C49 P6 117.5(5) . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C53 C54 C49 120.0 . . ? C60 C55 C56 116.7(10) . . ? C60 C55 P6 119.3(8) . . ? C56 C55 P6 124.0(9) . . ? C57 C56 C55 120.1(11) . . ? C58 C57 C56 122.3(11) . . ? C57 C58 C59 119.7(12) . . ? C60 C59 C58 118.2(10) . . ? C55 C60 C59 122.9(9) . . ? C62 C61 C66 118.4(11) . . ? C62 C61 P6 119.0(8) . . ? C66 C61 P6 122.5(10) . . ? C61 C62 C63 119.7(11) . . ? C64 C63 C62 126.1(15) . . ? C63 C64 C65 114.1(13) . . ? C66 C65 C64 120.5(11) . . ? C65 C66 C61 121.2(13) . . ? C72 C67 C68 118.1(9) . . ? C72 C67 P7 118.7(6) . . ? C68 C67 P7 123.2(7) . . ? C67 C68 C69 120.8(9) . . ? C68 C69 C70 119.3(10) . . ? C71 C70 C69 119.6(10) . . ? C70 C71 C72 120.5(9) . . ? C71 C72 C67 121.6(9) . . ? C74 C73 C78 119.6(8) . . ? C74 C73 P7 122.6(7) . . ? C78 C73 P7 117.8(7) . . ? C75 C74 C73 120.4(10) . . ? C74 C75 C76 120.2(10) . . ? C75 C76 C77 120.7(9) . . ? C76 C77 C78 120.1(10) . . ? C77 C78 C73 119.1(10) . . ? C84 C79 C80 118.1(7) . . ? C84 C79 P7 117.7(6) . . ? C80 C79 P7 124.2(6) . . ? C81 C80 C79 119.9(8) . . ? C82 C81 C80 122.6(9) . . ? C81 C82 C83 119.0(9) . . ? C82 C83 C84 118.7(10) . . ? C79 C84 C83 121.6(9) . . ? C85 O11 C88 106(3) . . ? O11 C85 C86 111(3) . . ? C87 C86 C85 109(3) . . ? C86 C87 C88 108(3) . . ? C87 C88 O11 102(3) . . ? C89 O12 C92 106.5(11) . . ? O12 C89 C90 107.4(13) . . ? C91 C90 C89 103.0(15) . . ? C92 C91 C90 113.2(16) . . ? C91 C92 O12 105.0(12) . . ? C93 O13 C96 104.1(10) . . ? O13 C93 C94 109.9(9) . . ? C95 C94 C93 99.8(14) . . ? C96 C95 C94 107.1(18) . . ? C95 C96 O13 107.3(16) . . ? C97 O14 C100 104(2) . . ? O14 C97 C98 111(2) . . ? C97 C98 C99 104(2) . . ? C100 C99 C98 105(2) . . ? C99 C100 O14 114(3) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 2.970 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.163 data_3 _database_code_depnum_ccdc_archive 'CCDC 276588' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H46 Fe2 O6 P2 S6' _chemical_formula_weight 868.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.760(2) _cell_length_b 17.020(3) _cell_length_c 11.300(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.91(3) _cell_angle_gamma 90.00 _cell_volume 1945.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 627 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 26 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'stoe ipds 1' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8829 _diffrn_reflns_av_R_equivalents 0.1237 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.88 _reflns_number_total 3680 _reflns_number_gt 1956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe winexpose' _computing_cell_refinement 'stoe winexpose' _computing_data_reduction 'stoe winexpose' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1240P)^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 3680 _refine_ls_number_parameters 204 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1527 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2340 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P -0.09373(18) -0.01845(15) 0.1727(2) 0.0325(5) Uani 1 1 d . . . Fe1 Fe 0.02623(10) 0.10551(8) 0.04132(11) 0.0341(4) Uani 1 1 d . . . S1 S 0.02780(19) 0.07009(16) 0.2588(2) 0.0426(6) Uani 1 1 d . . . S2 S -0.17210(17) 0.01000(14) -0.01409(19) 0.0330(5) Uani 1 1 d . . . S3 S 0.0076(2) 0.12530(16) -0.1843(2) 0.0414(6) Uani 1 1 d . . . O1 O -0.5069(5) -0.0696(5) 0.4060(6) 0.055(2) Uani 1 1 d . . . O2 O 0.1966(6) 0.1781(5) 0.1197(6) 0.0501(18) Uani 1 1 d . . . O3 O -0.0905(6) 0.2094(4) 0.0313(7) 0.0535(19) Uani 1 1 d D A . C1 C -0.2230(7) -0.0280(6) 0.2407(7) 0.0320(19) Uani 1 1 d . . . C2 C -0.1904(8) -0.0476(6) 0.3675(8) 0.039(2) Uani 1 1 d . . . H2A H -0.1011 -0.0521 0.4186 0.046 Uiso 1 1 calc R . . C3 C -0.2869(8) -0.0603(7) 0.4176(9) 0.045(2) Uani 1 1 d . . . H3A H -0.2631 -0.0736 0.5032 0.054 Uiso 1 1 calc R . . C4 C -0.4186(8) -0.0542(7) 0.3461(9) 0.047(3) Uani 1 1 d . . . C5 C -0.4569(8) -0.0310(7) 0.2212(8) 0.046(3) Uani 1 1 d . . . H5A H -0.5466 -0.0234 0.1737 0.056 Uiso 1 1 calc R . . C6 C -0.3567(7) -0.0192(7) 0.1664(9) 0.045(3) Uani 1 1 d . . . H6A H -0.3801 -0.0055 0.0809 0.054 Uiso 1 1 calc R . . C7 C -0.6452(9) -0.0526(11) 0.3347(11) 0.084(5) Uani 1 1 d . . . H7A H -0.6993 -0.0656 0.3853 0.126 Uiso 1 1 calc R . . H7B H -0.6734 -0.0837 0.2582 0.126 Uiso 1 1 calc R . . H7C H -0.6549 0.0028 0.3132 0.126 Uiso 1 1 calc R . . C8 C 0.2326(11) 0.2173(9) 0.2375(13) 0.081(5) Uani 1 1 d . . . H8A H 0.1767 0.2639 0.2297 0.097 Uiso 1 1 calc R . . H8B H 0.2176 0.1823 0.3002 0.097 Uiso 1 1 calc R . . C9 C 0.3658(13) 0.2403(13) 0.2784(16) 0.108(6) Uani 1 1 d . . . H9A H 0.4158 0.2137 0.3572 0.129 Uiso 1 1 calc R . . H9B H 0.3740 0.2972 0.2920 0.129 Uiso 1 1 calc R . . C10 C 0.4155(11) 0.2162(11) 0.1739(13) 0.086(5) Uani 1 1 d . . . H10A H 0.4624 0.2598 0.1512 0.103 Uiso 1 1 calc R . . H10B H 0.4759 0.1714 0.2001 0.103 Uiso 1 1 calc R . . C11 C 0.2980(10) 0.1946(10) 0.0669(12) 0.080(5) Uani 1 1 d . . . H11A H 0.2713 0.2379 0.0064 0.095 Uiso 1 1 calc R . . H11B H 0.3158 0.1481 0.0240 0.095 Uiso 1 1 calc R . . C12 C -0.2084(12) 0.2130(8) 0.0661(16) 0.089(5) Uani 1 1 d D . . C13 C -0.2962(14) 0.2689(13) -0.025(2) 0.085(4) Uiso 0.66(3) 1 d PD A 1 H13A H -0.3588 0.2937 0.0097 0.102 Uiso 0.66(3) 1 calc PR A 1 H13B H -0.3452 0.2431 -0.1044 0.102 Uiso 0.66(3) 1 calc PR A 1 C14 C -0.1941(17) 0.3294(10) -0.041(3) 0.085(4) Uiso 0.66(3) 1 d PD A 1 H14A H -0.2281 0.3551 -0.1231 0.102 Uiso 0.66(3) 1 calc PR A 1 H14B H -0.1737 0.3696 0.0252 0.102 Uiso 0.66(3) 1 calc PR A 1 C13A C -0.262(5) 0.2928(15) 0.031(4) 0.085(4) Uiso 0.34(3) 1 d PD A 2 H13C H -0.2183 0.3325 0.0940 0.102 Uiso 0.34(3) 1 calc PR A 2 H13D H -0.3583 0.2954 0.0104 0.102 Uiso 0.34(3) 1 calc PR A 2 C14A C -0.2205(18) 0.296(4) -0.086(3) 0.085(4) Uiso 0.34(3) 1 d PD A 2 H14C H -0.2395 0.3478 -0.1268 0.102 Uiso 0.34(3) 1 calc PR A 2 H14D H -0.2643 0.2554 -0.1469 0.102 Uiso 0.34(3) 1 calc PR A 2 C15 C -0.0763(12) 0.2821(6) -0.0299(13) 0.068(3) Uani 1 1 d 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 P1 0.0222(9) 0.0521(15) 0.0227(11) 0.0043(10) 0.0072(7) 0.0011(9) Fe1 0.0272(5) 0.0471(8) 0.0290(7) 0.0012(6) 0.0107(4) -0.0008(5) S1 0.0347(10) 0.0638(17) 0.0281(12) -0.0036(11) 0.0089(8) -0.0086(10) S2 0.0238(9) 0.0505(14) 0.0233(11) 0.0051(10) 0.0065(7) 0.0015(8) S3 0.0395(11) 0.0547(16) 0.0322(13) 0.0084(11) 0.0152(9) 0.0092(10) O1 0.035(3) 0.107(7) 0.028(3) 0.021(4) 0.015(3) 0.001(3) O2 0.044(3) 0.078(5) 0.035(4) -0.015(3) 0.022(3) -0.019(3) O3 0.052(4) 0.055(5) 0.066(5) 0.012(4) 0.036(3) 0.014(3) C1 0.028(4) 0.055(6) 0.015(4) -0.003(4) 0.011(3) -0.002(3) C2 0.037(4) 0.051(6) 0.028(5) 0.002(4) 0.011(3) 0.006(4) C3 0.037(4) 0.078(8) 0.024(5) 0.011(5) 0.016(4) 0.007(4) C4 0.029(4) 0.089(8) 0.030(5) 0.000(5) 0.018(3) 0.001(4) C5 0.028(4) 0.095(9) 0.018(5) 0.010(5) 0.012(3) 0.003(4) C6 0.021(4) 0.082(8) 0.032(5) 0.011(5) 0.009(3) 0.010(4) C7 0.034(5) 0.175(16) 0.055(8) 0.017(9) 0.030(5) 0.007(7) C8 0.055(6) 0.121(12) 0.083(9) -0.063(9) 0.045(6) -0.047(7) C9 0.060(8) 0.18(2) 0.092(12) -0.044(12) 0.032(7) -0.037(9) C10 0.052(6) 0.138(14) 0.074(9) -0.026(9) 0.030(6) -0.033(7) C11 0.049(6) 0.137(13) 0.065(8) -0.022(8) 0.034(5) -0.045(7) C12 0.071(8) 0.074(10) 0.154(15) 0.023(9) 0.078(9) 0.028(7) C15 0.090(8) 0.031(6) 0.095(10) 0.022(6) 0.048(7) 0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.810(7) . ? P1 S1 2.015(3) . ? P1 S3 2.025(3) 3 ? P1 S2 2.047(3) . ? Fe1 O2 2.137(6) . ? Fe1 O3 2.149(7) . ? Fe1 S3 2.511(3) . ? Fe1 S1 2.525(3) . ? Fe1 S2 2.584(2) . ? Fe1 S2 2.599(3) 3 ? S2 Fe1 2.599(3) 3 ? S3 P1 2.025(3) 3 ? O1 C4 1.366(10) . ? O1 C7 1.460(11) . ? O2 C8 1.420(13) . ? O2 C11 1.438(11) . ? O3 C12 1.451(9) . ? O3 C15 1.451(10) . ? C1 C2 1.396(12) . ? C1 C6 1.405(10) . ? C2 C3 1.359(12) . ? C3 C4 1.376(11) . ? C4 C5 1.386(12) . ? C5 C6 1.430(11) . ? C8 C9 1.404(15) . ? C9 C10 1.51(2) . ? C10 C11 1.467(16) . ? C12 C13 1.479(15) . ? C12 C13A 1.477(16) . ? C13 C14 1.562(17) . ? C14 C15 1.471(14) . ? C13A C14A 1.53(2) . ? C14A C15 1.483(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 S1 109.2(3) . . ? C1 P1 S3 107.0(3) . 3 ? S1 P1 S3 115.66(13) . 3 ? C1 P1 S2 110.6(3) . . ? S1 P1 S2 107.01(14) . . ? S3 P1 S2 107.32(14) 3 . ? O2 Fe1 O3 87.1(3) . . ? O2 Fe1 S3 95.95(19) . . ? O3 Fe1 S3 89.6(2) . . ? O2 Fe1 S1 90.82(19) . . ? O3 Fe1 S1 93.3(2) . . ? S3 Fe1 S1 172.76(10) . . ? O2 Fe1 S2 170.2(2) . . ? O3 Fe1 S2 94.87(19) . . ? S3 Fe1 S2 93.71(8) . . ? S1 Fe1 S2 79.45(8) . . ? O2 Fe1 S2 91.1(2) . 3 ? O3 Fe1 S2 169.08(19) . 3 ? S3 Fe1 S2 79.85(8) . 3 ? S1 Fe1 S2 97.50(9) . 3 ? S2 Fe1 S2 88.72(7) . 3 ? P1 S1 Fe1 85.44(10) . . ? P1 S2 Fe1 83.27(10) . . ? P1 S2 Fe1 83.67(10) . 3 ? Fe1 S2 Fe1 91.28(7) . 3 ? P1 S3 Fe1 86.42(11) 3 . ? C4 O1 C7 116.0(7) . . ? C8 O2 C11 107.1(8) . . ? C8 O2 Fe1 125.6(6) . . ? C11 O2 Fe1 127.3(7) . . ? C12 O3 C15 109.7(8) . . ? C12 O3 Fe1 124.7(6) . . ? C15 O3 Fe1 124.9(5) . . ? C2 C1 C6 119.2(7) . . ? C2 C1 P1 119.8(6) . . ? C6 C1 P1 121.0(6) . . ? C3 C2 C1 120.4(8) . . ? C2 C3 C4 121.6(9) . . ? O1 C4 C3 116.4(8) . . ? O1 C4 C5 122.9(7) . . ? C3 C4 C5 120.6(7) . . ? C4 C5 C6 118.4(7) . . ? C1 C6 C5 119.7(8) . . ? C9 C8 O2 111.2(10) . . ? C8 C9 C10 105.1(11) . . ? C11 C10 C9 106.1(10) . . ? O2 C11 C10 105.6(10) . . ? O3 C12 C13 104.5(10) . . ? O3 C12 C13A 105.3(18) . . ? C13 C12 C13A 28.7(17) . . ? C12 C13 C14 101.3(11) . . ? C15 C14 C13 104.5(8) . . ? C12 C13A C14A 94(3) . . ? C13A C14A C15 101(2) . . ? C14 C15 O3 106.2(9) . . ? C14 C15 C14A 29.3(19) . . ? O3 C15 C14A 94(2) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.659 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.164 data_4 _database_code_depnum_ccdc_archive 'CCDC 276589' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H68 Ni4 O16 P4 S8' _chemical_formula_weight 1468.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 26.921(5) _cell_length_b 13.001(3) _cell_length_c 18.206(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6372(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 18656 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 53.78 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 1.585 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 'stoe ipds 2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35061 _diffrn_reflns_av_R_equivalents 0.1692 _diffrn_reflns_av_sigmaI/netI 0.1373 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.04 _reflns_number_total 13469 _reflns_number_gt 6422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1472P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(4) _refine_ls_number_reflns 13469 _refine_ls_number_parameters 657 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1927 _refine_ls_R_factor_gt 0.1262 _refine_ls_wR_factor_ref 0.3167 _refine_ls_wR_factor_gt 0.2775 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.35220(7) 0.20710(19) 0.62259(12) 0.0675(6) Uani 1 1 d . . . Ni2 Ni 0.39494(7) -0.25254(17) 0.54776(12) 0.0616(5) Uani 1 1 d . . . Ni3 Ni 0.48812(8) -0.0228(2) 0.72223(14) 0.0783(7) Uani 1 1 d D . . Ni4 Ni 0.25686(7) -0.02863(18) 0.44951(14) 0.0691(6) Uani 1 1 d D . . S1 S 0.43394(14) 0.2362(3) 0.6142(2) 0.0641(10) Uani 1 1 d D . . S2 S 0.36408(15) 0.1747(4) 0.7416(2) 0.0716(11) Uani 1 1 d D . . S3 S 0.33980(15) 0.2293(4) 0.5030(2) 0.0656(11) Uani 1 1 d D . . S4 S 0.27005(14) 0.1702(4) 0.6314(3) 0.0719(11) Uani 1 1 d D . . S5 S 0.47589(14) -0.2179(4) 0.5398(3) 0.0768(12) Uani 1 1 d D . . S6 S 0.40644(15) -0.2807(4) 0.6664(2) 0.0718(12) Uani 1 1 d D . . S7 S 0.38200(14) -0.2164(3) 0.4289(2) 0.0621(10) Uani 1 1 d D . . S8 S 0.31468(13) -0.2853(3) 0.5563(2) 0.0643(10) Uani 1 1 d D . . P1 P 0.43899(17) 0.2118(4) 0.7247(3) 0.0787(13) Uani 1 1 d . . . P2 P 0.26551(15) 0.2042(4) 0.5206(3) 0.0670(12) Uani 1 1 d . . . P3 P 0.48024(15) -0.2562(4) 0.6490(3) 0.0711(13) Uani 1 1 d . . . P4 P 0.30975(14) -0.2584(3) 0.4458(3) 0.0634(10) Uani 1 1 d . . . O1 O 0.4731(4) 0.1296(10) 0.7502(7) 0.081(4) Uani 1 1 d . . . O2 O 0.5037(5) 0.5853(12) 0.8838(10) 0.107(5) Uani 1 1 d . . . O3 O 0.2417(4) 0.1209(8) 0.4740(6) 0.067(3) Uani 1 1 d . . . O4 O 0.1476(5) 0.5834(10) 0.4691(9) 0.092(4) Uani 1 1 d . . . O5 O 0.5021(4) -0.1723(12) 0.6993(7) 0.090(4) Uani 1 1 d . . . O7 O 0.2713(4) -0.1745(9) 0.4237(6) 0.071(3) Uani 1 1 d . . . O8 O 0.2627(6) -0.6502(11) 0.2912(8) 0.104(5) Uani 1 1 d . . . O13 O 0.4124(4) -0.0554(10) 0.7360(8) 0.083(4) Uani 1 1 d D . . H131 H 0.406(3) -0.121(4) 0.737(6) 0.125 Uiso 1 1 d D . . H132 H 0.395(2) -0.001(4) 0.721(7) 0.125 Uiso 1 1 d D . . O14 O 0.4838(6) 0.0101(12) 0.6131(8) 0.101(4) Uani 1 1 d D . . H141 H 0.457(3) 0.051(5) 0.602(4) 0.152 Uiso 1 1 d D . . H142 H 0.466(4) -0.040(4) 0.588(3) 0.152 Uiso 1 1 d D . . O15 O 0.2841(7) -0.0503(9) 0.5539(10) 0.119(6) Uani 1 1 d D . . H151 H 0.303(8) -0.099(6) 0.572(13) 0.178 Uiso 1 1 d D . . H152 H 0.296(4) 0.006(11) 0.575(16) 0.178 Uiso 1 1 d D . . O16 O 0.3277(4) 0.0105(9) 0.4098(8) 0.082(4) Uani 1 1 d D . . H161 H 0.344(3) -0.048(4) 0.398(7) 0.123 Uiso 1 1 d D . . H162 H 0.341(2) 0.058(7) 0.441(6) 0.123 Uiso 1 1 d D . . C1 C 0.4573(4) 0.3211(8) 0.7758(7) 0.083(5) Uani 1 1 d G . . C2 C 0.4345(4) 0.4157(10) 0.7651(6) 0.087(6) Uani 1 1 d G . . H2A H 0.4073 0.4216 0.7320 0.104 Uiso 1 1 calc R . . C3 C 0.4514(4) 0.5019(8) 0.8027(8) 0.087(6) Uani 1 1 d G . . H3A H 0.4358 0.5667 0.7954 0.104 Uiso 1 1 calc R . . C4 C 0.4912(5) 0.4934(9) 0.8510(8) 0.103(8) Uani 1 1 d G . . C5 C 0.5140(4) 0.3987(10) 0.8617(7) 0.093(6) Uani 1 1 d G . . H5A H 0.5412 0.3929 0.8948 0.112 Uiso 1 1 calc R . . C6 C 0.4971(4) 0.3125(8) 0.8241(7) 0.097(6) Uani 1 1 d G . . H6A H 0.5127 0.2478 0.8314 0.116 Uiso 1 1 calc R . . C7 C 0.5477(8) 0.5813(17) 0.9280(14) 0.115(9) Uani 1 1 d . . . H7A H 0.5542 0.6494 0.9489 0.172 Uiso 1 1 calc R . . H7B H 0.5759 0.5602 0.8975 0.172 Uiso 1 1 calc R . . H7C H 0.5430 0.5314 0.9677 0.172 Uiso 1 1 calc R . . C8 C 0.2286(4) 0.3167(8) 0.5036(7) 0.074(5) Uani 1 1 d G . . C9 C 0.1835(4) 0.3075(7) 0.4671(8) 0.083(5) Uani 1 1 d G . . H9A H 0.1726 0.2421 0.4503 0.100 Uiso 1 1 calc R . . C10 C 0.1543(3) 0.3941(8) 0.4551(8) 0.085(6) Uani 1 1 d G . . H10A H 0.1234 0.3878 0.4302 0.102 Uiso 1 1 calc R . . C11 C 0.1702(4) 0.4898(6) 0.4796(7) 0.071(5) Uani 1 1 d G . . C12 C 0.2153(4) 0.4990(7) 0.5161(7) 0.091(6) Uani 1 1 d G . . H12A H 0.2262 0.5645 0.5328 0.109 Uiso 1 1 calc R . . C13 C 0.2445(3) 0.4125(10) 0.5281(7) 0.074(5) Uani 1 1 d G . . H13A H 0.2754 0.4188 0.5530 0.088 Uiso 1 1 calc R . . C15 C 0.5153(4) -0.3721(7) 0.6631(8) 0.081(6) Uani 1 1 d G . . C16 C 0.5025(4) -0.4610(9) 0.6252(7) 0.079(5) Uani 1 1 d G . . H16A H 0.4744 -0.4611 0.5935 0.095 Uiso 1 1 calc R . . C17 C 0.5308(4) -0.5497(7) 0.6334(7) 0.087(5) Uani 1 1 d G . . H17A H 0.5221 -0.6104 0.6075 0.105 Uiso 1 1 calc R . . C18 C 0.5719(4) -0.5495(8) 0.6796(7) 0.070(5) Uani 1 1 d G . . C19 C 0.5847(4) -0.4606(10) 0.7176(7) 0.095(7) Uani 1 1 d G . . H19A H 0.6128 -0.4605 0.7492 0.114 Uiso 1 1 calc R . . C20 C 0.5564(5) -0.3719(8) 0.7094(7) 0.095(6) Uani 1 1 d G . . H20A H 0.5652 -0.3112 0.7353 0.114 Uiso 1 1 calc R . . C22 C 0.2954(4) -0.3756(6) 0.3978(6) 0.074(5) Uani 1 1 d G . . C23 C 0.2543(4) -0.3774(6) 0.3516(6) 0.081(5) Uani 1 1 d G . . H23A H 0.2352 -0.3168 0.3446 0.097 Uiso 1 1 calc R . . C24 C 0.2412(4) -0.4678(8) 0.3158(7) 0.079(5) Uani 1 1 d G . . H24A H 0.2131 -0.4690 0.2843 0.095 Uiso 1 1 calc R . . C25 C 0.2692(5) -0.5565(6) 0.3261(7) 0.084(6) Uani 1 1 d G . . C26 C 0.3103(4) -0.5547(6) 0.3723(7) 0.089(6) Uani 1 1 d G . . H26A H 0.3295 -0.6153 0.3794 0.106 Uiso 1 1 calc R . . C27 C 0.3234(4) -0.4643(8) 0.4081(6) 0.070(5) Uani 1 1 d G . . H27A H 0.3515 -0.4630 0.4397 0.085 Uiso 1 1 calc R . . C28 C 0.2223(14) -0.6556(18) 0.2418(19) 0.182(18) Uani 1 1 d . . . H28A H 0.2209 -0.7245 0.2200 0.273 Uiso 1 1 calc R . . H28B H 0.2267 -0.6043 0.2029 0.273 Uiso 1 1 calc R . . H28C H 0.1913 -0.6418 0.2683 0.273 Uiso 1 1 calc R . . O9 O 0.4968(5) -0.0567(9) 0.8354(7) 0.076(3) Uani 1 1 d . . . C29 C 0.4868(8) -0.1524(12) 0.8666(10) 0.082(5) Uani 1 1 d . . . H29A H 0.5048 -0.2074 0.8400 0.098 Uiso 1 1 calc R . . H29B H 0.4508 -0.1675 0.8646 0.098 Uiso 1 1 calc R . . C30 C 0.5045(9) -0.1459(19) 0.9459(14) 0.113(7) Uani 1 1 d . . . H30A H 0.4795 -0.1135 0.9784 0.135 Uiso 1 1 calc R . . H30B H 0.5141 -0.2140 0.9657 0.135 Uiso 1 1 calc R . . C31 C 0.5477(8) -0.079(2) 0.9333(12) 0.129(10) Uani 1 1 d . . . H31A H 0.5759 -0.1190 0.9130 0.155 Uiso 1 1 calc R . . H31B H 0.5585 -0.0460 0.9796 0.155 Uiso 1 1 calc R . . C32 C 0.5300(7) 0.0017(18) 0.8781(10) 0.094(7) Uani 1 1 d . . . H32A H 0.5129 0.0596 0.9029 0.113 Uiso 1 1 calc R . . H32B H 0.5578 0.0287 0.8482 0.113 Uiso 1 1 calc R . . O10 O 0.5651(5) 0.0081(10) 0.7142(8) 0.091(4) Uani 1 1 d . . . C33 C 0.5873(11) 0.1033(16) 0.6886(14) 0.116(9) Uani 1 1 d . . . H33A H 0.5725 0.1249 0.6412 0.140 Uiso 1 1 calc R . . H33B H 0.5825 0.1590 0.7250 0.140 Uiso 1 1 calc R . . C34 C 0.6391(13) 0.079(2) 0.680(2) 0.19(2) Uani 1 1 d . . . H34A H 0.6526 0.1130 0.6355 0.229 Uiso 1 1 calc R . . H34B H 0.6582 0.1037 0.7232 0.229 Uiso 1 1 calc R . . C35 C 0.6424(11) -0.022(3) 0.674(2) 0.178(18) Uani 1 1 d . . . H35A H 0.6748 -0.0448 0.6943 0.213 Uiso 1 1 calc R . . H35B H 0.6418 -0.0410 0.6214 0.213 Uiso 1 1 calc R . . C36 C 0.6023(6) -0.078(2) 0.7122(15) 0.109(7) Uani 1 1 d . . . H36A H 0.6123 -0.1011 0.7619 0.131 Uiso 1 1 calc R . . H36B H 0.5903 -0.1381 0.6834 0.131 Uiso 1 1 calc R . . O11 O 0.1865(5) -0.0762(9) 0.4867(9) 0.089(4) Uani 1 1 d . . . C37 C 0.1463(8) -0.0125(16) 0.4784(14) 0.095(6) Uani 1 1 d . . . H37A H 0.1468 0.0241 0.4307 0.115 Uiso 1 1 calc R . . H37B H 0.1436 0.0379 0.5190 0.115 Uiso 1 1 calc R . . C38 C 0.1019(7) -0.101(2) 0.4820(18) 0.119(9) Uani 1 1 d . . . H38A H 0.0701 -0.0715 0.4994 0.143 Uiso 1 1 calc R . . H38B H 0.0967 -0.1341 0.4336 0.143 Uiso 1 1 calc R . . C39 C 0.1227(8) -0.1727(17) 0.5352(15) 0.104(7) Uani 1 1 d . . . H39A H 0.1066 -0.2410 0.5324 0.125 Uiso 1 1 calc R . . H39B H 0.1203 -0.1459 0.5860 0.125 Uiso 1 1 calc R . . C40 C 0.1761(10) -0.1765(18) 0.5087(14) 0.110(7) Uani 1 1 d . . . H40A H 0.1987 -0.1982 0.5488 0.132 Uiso 1 1 calc R . . H40B H 0.1797 -0.2249 0.4671 0.132 Uiso 1 1 calc R . . O12 O 0.2293(5) -0.0085(11) 0.3430(7) 0.090(4) Uani 1 1 d . . . C41 C 0.2365(10) 0.0794(13) 0.3036(12) 0.108(9) Uani 1 1 d . . . H41A H 0.2722 0.0911 0.2943 0.129 Uiso 1 1 calc R . . H41B H 0.2227 0.1397 0.3299 0.129 Uiso 1 1 calc R . . C42 C 0.2083(8) 0.0605(14) 0.2313(12) 0.086(6) Uani 1 1 d . . . H42A H 0.1733 0.0836 0.2352 0.103 Uiso 1 1 calc R . . H42B H 0.2244 0.0969 0.1899 0.103 Uiso 1 1 calc R . . C43 C 0.2112(10) -0.056(2) 0.2210(14) 0.120(8) Uani 1 1 d . . . H43A H 0.2427 -0.0768 0.1971 0.143 Uiso 1 1 calc R . . H43B H 0.1827 -0.0825 0.1925 0.143 Uiso 1 1 calc R . . C44 C 0.2091(11) -0.0901(15) 0.3021(14) 0.114(8) Uani 1 1 d . . . H44A H 0.1744 -0.1036 0.3172 0.137 Uiso 1 1 calc R . . H44B H 0.2288 -0.1536 0.3095 0.137 Uiso 1 1 calc R . . O6 O 0.5996(5) -0.6402(11) 0.6782(8) 0.095(4) Uiso 1 1 d . . . C14 C 0.0988(6) 0.5775(15) 0.4325(10) 0.080(5) Uani 1 1 d . . . H14A H 0.0852 0.6469 0.4267 0.120 Uiso 1 1 calc R . . H14B H 0.0761 0.5360 0.4624 0.120 Uiso 1 1 calc R . . H14C H 0.1027 0.5455 0.3841 0.120 Uiso 1 1 calc R . . C21 C 0.6440(11) -0.6368(19) 0.7257(19) 0.169(16) Uani 1 1 d . . . H21A H 0.6617 -0.7025 0.7225 0.254 Uiso 1 1 calc R . . H21B H 0.6339 -0.6246 0.7766 0.254 Uiso 1 1 calc R . . H21C H 0.6660 -0.5811 0.7094 0.254 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 0.0491(10) 0.1017(17) 0.0518(12) 0.0093(11) 0.0040(9) 0.0134(10) Ni2 0.0420(9) 0.0912(15) 0.0515(11) 0.0028(10) 0.0000(8) -0.0022(8) Ni3 0.0534(11) 0.1153(19) 0.0661(13) -0.0003(13) -0.0074(10) 0.0107(11) Ni4 0.0521(10) 0.0886(14) 0.0667(13) 0.0085(12) -0.0062(10) -0.0015(10) S1 0.052(2) 0.086(3) 0.055(3) -0.002(2) 0.0016(18) -0.0010(17) S2 0.060(2) 0.090(3) 0.064(3) 0.004(2) -0.0005(19) 0.008(2) S3 0.0490(19) 0.090(3) 0.057(3) 0.000(2) 0.0011(17) -0.0053(18) S4 0.053(2) 0.091(3) 0.072(3) 0.009(2) 0.0020(19) 0.0000(19) S5 0.0485(19) 0.116(4) 0.066(3) 0.004(3) 0.0059(19) -0.003(2) S6 0.052(2) 0.112(3) 0.051(2) 0.008(2) -0.0019(18) 0.019(2) S7 0.0540(19) 0.075(2) 0.057(2) 0.003(2) 0.0026(16) -0.0014(18) S8 0.0477(19) 0.087(3) 0.059(3) 0.005(2) 0.0016(18) -0.0044(17) P1 0.056(2) 0.121(4) 0.059(3) 0.002(3) 0.000(2) 0.010(2) P2 0.053(2) 0.082(3) 0.066(3) 0.014(2) 0.002(2) 0.0035(19) P3 0.046(2) 0.113(4) 0.054(3) 0.004(2) -0.0068(18) 0.002(2) P4 0.050(2) 0.085(3) 0.055(3) 0.001(2) -0.0057(19) -0.0074(18) O1 0.068(7) 0.099(9) 0.078(8) 0.020(7) -0.032(6) 0.000(6) O2 0.083(9) 0.111(11) 0.127(13) -0.049(10) -0.027(8) 0.016(8) O3 0.041(5) 0.081(7) 0.080(8) 0.004(6) 0.000(5) -0.007(5) O4 0.070(7) 0.073(8) 0.133(13) 0.016(7) -0.026(7) 0.002(6) O5 0.046(6) 0.154(12) 0.069(8) -0.016(8) -0.022(5) 0.010(6) O7 0.051(5) 0.107(8) 0.056(6) 0.009(6) -0.020(5) -0.010(5) O8 0.146(13) 0.089(9) 0.078(9) -0.015(7) -0.024(9) -0.025(9) O13 0.063(6) 0.087(8) 0.100(10) 0.015(7) -0.015(6) 0.010(6) O14 0.122(12) 0.119(11) 0.064(8) -0.025(8) 0.007(8) 0.005(9) O15 0.191(17) 0.058(8) 0.107(12) -0.002(8) -0.060(11) 0.019(9) O16 0.058(6) 0.072(7) 0.117(10) 0.013(7) -0.017(7) -0.005(5) C1 0.058(9) 0.131(17) 0.060(11) 0.000(11) -0.006(8) 0.018(10) C2 0.061(10) 0.139(18) 0.061(11) 0.012(11) 0.005(8) -0.016(11) C3 0.117(16) 0.033(8) 0.110(16) -0.020(9) 0.022(13) -0.012(9) C4 0.064(11) 0.119(18) 0.12(2) 0.051(16) -0.009(11) 0.024(11) C5 0.092(13) 0.119(17) 0.068(12) -0.015(12) 0.026(10) 0.025(13) C6 0.061(10) 0.15(2) 0.076(13) -0.008(13) -0.007(9) -0.002(11) C7 0.099(14) 0.113(16) 0.13(2) -0.053(14) -0.072(15) 0.027(12) C8 0.053(9) 0.105(14) 0.065(11) -0.003(10) -0.004(8) 0.010(8) C9 0.089(12) 0.057(10) 0.102(15) 0.000(9) -0.012(11) 0.016(9) C10 0.055(9) 0.074(12) 0.126(17) 0.004(11) -0.015(10) 0.012(8) C11 0.082(11) 0.048(9) 0.081(11) 0.038(8) -0.004(9) -0.008(8) C12 0.079(12) 0.096(14) 0.098(15) 0.020(12) -0.013(11) -0.015(10) C13 0.048(8) 0.111(14) 0.062(10) 0.012(10) -0.009(7) 0.009(8) C15 0.042(8) 0.080(12) 0.122(17) 0.027(11) -0.015(9) 0.017(7) C16 0.087(11) 0.058(10) 0.091(13) 0.016(10) -0.025(10) 0.010(8) C17 0.069(10) 0.112(15) 0.081(13) 0.000(12) -0.002(9) 0.003(10) C18 0.054(8) 0.057(10) 0.098(14) -0.009(9) -0.002(8) 0.011(7) C19 0.099(14) 0.108(16) 0.079(13) 0.046(13) 0.025(11) 0.019(12) C20 0.117(17) 0.079(13) 0.089(15) -0.009(11) 0.013(13) -0.029(12) C22 0.084(11) 0.072(11) 0.068(11) 0.013(9) -0.026(9) -0.022(9) C23 0.097(13) 0.087(12) 0.058(11) -0.022(9) 0.021(9) -0.021(10) C24 0.109(14) 0.062(10) 0.066(11) -0.001(8) -0.028(10) -0.022(10) C25 0.102(13) 0.030(8) 0.121(16) -0.004(9) -0.056(12) -0.013(8) C26 0.121(16) 0.061(11) 0.084(14) 0.004(10) 0.036(12) -0.003(10) C27 0.079(11) 0.051(9) 0.082(12) -0.001(8) -0.030(9) -0.005(7) C28 0.30(5) 0.079(16) 0.16(3) -0.008(17) -0.12(3) -0.06(2) O9 0.083(7) 0.069(7) 0.076(8) -0.013(6) -0.028(6) 0.007(6) C29 0.123(16) 0.049(10) 0.074(12) 0.000(9) 0.006(11) 0.026(9) C30 0.120(18) 0.132(19) 0.086(15) 0.018(15) -0.005(14) 0.032(14) C31 0.065(11) 0.25(3) 0.074(15) 0.066(18) -0.019(10) -0.022(15) C32 0.069(10) 0.155(19) 0.059(11) -0.045(12) 0.005(8) -0.006(11) O10 0.071(7) 0.100(9) 0.100(10) -0.015(8) 0.006(7) -0.012(7) C33 0.18(2) 0.067(13) 0.106(18) -0.029(12) 0.036(17) -0.017(14) C34 0.19(3) 0.11(2) 0.27(5) -0.02(2) 0.18(3) 0.00(2) C35 0.12(2) 0.15(3) 0.26(4) 0.06(3) 0.13(3) 0.027(19) C36 0.039(8) 0.16(2) 0.123(19) -0.008(16) -0.010(10) -0.002(11) O11 0.074(8) 0.053(7) 0.140(13) -0.010(7) 0.018(8) 0.003(6) C37 0.097(14) 0.079(13) 0.110(17) -0.007(11) 0.003(12) 0.007(11) C38 0.057(11) 0.129(19) 0.17(3) 0.017(18) 0.005(13) -0.010(12) C39 0.087(13) 0.086(13) 0.14(2) -0.001(14) 0.030(14) 0.006(11) C40 0.14(2) 0.102(16) 0.090(16) -0.011(13) 0.022(14) -0.026(14) O12 0.087(8) 0.109(10) 0.075(9) -0.016(8) -0.013(7) 0.012(7) C41 0.19(2) 0.037(9) 0.100(15) 0.010(10) -0.059(16) -0.022(11) C42 0.100(13) 0.072(11) 0.085(14) 0.021(10) -0.021(11) -0.024(10) C43 0.114(17) 0.16(2) 0.080(14) 0.029(16) -0.034(13) -0.028(16) C44 0.17(2) 0.063(12) 0.108(18) 0.011(12) -0.022(17) -0.002(13) C14 0.060(9) 0.110(14) 0.070(12) 0.010(10) -0.008(8) 0.007(9) C21 0.20(3) 0.111(18) 0.20(3) -0.053(19) -0.13(3) 0.10(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S3 2.221(5) . ? Ni1 S2 2.230(5) . ? Ni1 S1 2.238(4) . ? Ni1 S4 2.269(4) . ? Ni2 S8 2.208(4) . ? Ni2 S6 2.213(5) . ? Ni2 S5 2.230(4) . ? Ni2 S7 2.242(5) . ? Ni3 O5 2.023(15) . ? Ni3 O14 2.036(15) . ? Ni3 O1 2.086(14) . ? Ni3 O13 2.098(12) . ? Ni3 O10 2.115(12) . ? Ni3 O9 2.121(13) . ? Ni4 O7 1.993(13) . ? Ni4 O3 2.036(11) . ? Ni4 O15 2.056(16) . ? Ni4 O12 2.093(14) . ? Ni4 O16 2.103(12) . ? Ni4 O11 2.104(13) . ? S1 P1 2.040(7) . ? S2 P1 2.096(6) . ? S3 P2 2.052(6) . ? S4 P2 2.069(7) . ? S5 P3 2.052(7) . ? S6 P3 2.037(6) . ? S7 P4 2.044(5) . ? S8 P4 2.046(7) . ? P1 O1 1.482(12) . ? P1 C1 1.769(11) . ? P2 O3 1.517(12) . ? P2 C8 1.795(9) . ? P3 O5 1.541(14) . ? P3 C15 1.797(9) . ? P4 O7 1.556(12) . ? P4 C22 1.798(8) . ? O2 C4 1.377(16) . ? O2 C7 1.43(2) . ? O4 C11 1.374(14) . ? O4 C14 1.47(2) . ? O8 C25 1.386(15) . ? O8 C28 1.41(3) . ? O13 H131 0.87(4) . ? O13 H132 0.89(4) . ? O14 H141 0.92(4) . ? O14 H142 0.93(4) . ? O15 H151 0.89(4) . ? O15 H152 0.89(4) . ? O16 H161 0.90(4) . ? O16 H162 0.92(4) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2A 0.9500 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C9 H9A 0.9500 . ? C10 C11 1.3900 . ? C10 H10A 0.9500 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C15 C16 1.3900 . ? C15 C20 1.3900 . ? C16 C17 1.3900 . ? C16 H16A 0.9500 . ? C17 C18 1.3900 . ? C17 H17A 0.9500 . ? C18 C19 1.3900 . ? C18 O6 1.395(16) . ? C19 C20 1.3900 . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C24 C25 1.3900 . ? C24 H24A 0.9500 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O9 C29 1.39(2) . ? O9 C32 1.41(2) . ? C29 C30 1.52(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.47(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.53(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? O10 C33 1.45(3) . ? O10 C36 1.51(3) . ? C33 C34 1.44(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.33(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.48(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O11 C37 1.37(2) . ? O11 C40 1.39(2) . ? C37 C38 1.66(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.46(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.52(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? O12 C41 1.36(2) . ? O12 C44 1.41(2) . ? C41 C42 1.54(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.52(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.54(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O6 C21 1.48(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 S3 Ni1 S2 176.6(2) . . ? S3 Ni1 S1 93.39(17) . . ? S2 Ni1 S1 87.53(17) . . ? S3 Ni1 S4 87.15(17) . . ? S2 Ni1 S4 91.79(18) . . ? S1 Ni1 S4 177.5(2) . . ? S8 Ni2 S6 92.07(18) . . ? S8 Ni2 S5 179.4(2) . . ? S6 Ni2 S5 87.72(18) . . ? S8 Ni2 S7 87.50(16) . . ? S6 Ni2 S7 177.3(2) . . ? S5 Ni2 S7 92.68(17) . . ? O5 Ni3 O14 90.6(6) . . ? O5 Ni3 O1 177.7(5) . . ? O14 Ni3 O1 91.6(5) . . ? O5 Ni3 O13 90.7(5) . . ? O14 Ni3 O13 95.9(6) . . ? O1 Ni3 O13 88.5(5) . . ? O5 Ni3 O10 89.2(5) . . ? O14 Ni3 O10 87.0(6) . . ? O1 Ni3 O10 91.5(5) . . ? O13 Ni3 O10 177.0(6) . . ? O5 Ni3 O9 88.9(5) . . ? O14 Ni3 O9 177.0(6) . . ? O1 Ni3 O9 88.9(5) . . ? O13 Ni3 O9 87.1(5) . . ? O10 Ni3 O9 89.9(6) . . ? O7 Ni4 O3 179.0(5) . . ? O7 Ni4 O15 91.0(5) . . ? O3 Ni4 O15 90.0(5) . . ? O7 Ni4 O12 88.3(5) . . ? O3 Ni4 O12 90.7(5) . . ? O15 Ni4 O12 179.3(6) . . ? O7 Ni4 O16 88.4(5) . . ? O3 Ni4 O16 91.5(4) . . ? O15 Ni4 O16 91.6(7) . . ? O12 Ni4 O16 88.4(6) . . ? O7 Ni4 O11 88.4(4) . . ? O3 Ni4 O11 91.7(4) . . ? O15 Ni4 O11 89.0(7) . . ? O12 Ni4 O11 90.9(6) . . ? O16 Ni4 O11 176.8(5) . . ? P1 S1 Ni1 88.4(2) . . ? P1 S2 Ni1 87.3(2) . . ? P2 S3 Ni1 88.5(2) . . ? P2 S4 Ni1 86.8(2) . . ? P3 S5 Ni2 86.8(2) . . ? P3 S6 Ni2 87.6(2) . . ? P4 S7 Ni2 86.9(2) . . ? P4 S8 Ni2 87.78(19) . . ? O1 P1 C1 103.9(7) . . ? O1 P1 S1 117.5(6) . . ? C1 P1 S1 114.3(5) . . ? O1 P1 S2 112.6(6) . . ? C1 P1 S2 112.1(5) . . ? S1 P1 S2 96.7(3) . . ? O3 P2 C8 104.6(6) . . ? O3 P2 S3 116.1(5) . . ? C8 P2 S3 112.5(5) . . ? O3 P2 S4 114.6(5) . . ? C8 P2 S4 112.0(5) . . ? S3 P2 S4 97.4(3) . . ? O5 P3 C15 107.9(7) . . ? O5 P3 S6 113.0(5) . . ? C15 P3 S6 111.0(5) . . ? O5 P3 S5 115.2(6) . . ? C15 P3 S5 111.9(5) . . ? S6 P3 S5 97.7(2) . . ? O7 P4 C22 109.0(6) . . ? O7 P4 S7 114.0(5) . . ? C22 P4 S7 110.9(5) . . ? O7 P4 S8 114.7(5) . . ? C22 P4 S8 110.3(5) . . ? S7 P4 S8 97.6(2) . . ? P1 O1 Ni3 136.7(7) . . ? C4 O2 C7 114.5(14) . . ? P2 O3 Ni4 136.0(6) . . ? C11 O4 C14 114.3(13) . . ? P3 O5 Ni3 137.0(7) . . ? P4 O7 Ni4 137.4(6) . . ? C25 O8 C28 115.7(17) . . ? Ni3 O13 H131 114(5) . . ? Ni3 O13 H132 108(5) . . ? H131 O13 H132 132(9) . . ? Ni3 O14 H141 113(5) . . ? Ni3 O14 H142 112(5) . . ? H141 O14 H142 83(7) . . ? Ni4 O15 H151 131(10) . . ? Ni4 O15 H152 115(10) . . ? H151 O15 H152 102(10) . . ? Ni4 O16 H161 108(4) . . ? Ni4 O16 H162 108(4) . . ? H161 O16 H162 122(10) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 120.9(7) . . ? C6 C1 P1 119.0(7) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? O2 C4 C5 126.8(11) . . ? O2 C4 C3 113.2(11) . . ? C5 C4 C3 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 120.0 . . ? C9 C8 P2 119.7(7) . . ? C13 C8 P2 120.3(7) . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? O4 C11 C12 112.2(9) . . ? O4 C11 C10 127.7(9) . . ? C12 C11 C10 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C8 120.0 . . ? C12 C13 H13A 120.0 . . ? C8 C13 H13A 120.0 . . ? C16 C15 C20 120.0 . . ? C16 C15 P3 119.7(7) . . ? C20 C15 P3 120.2(7) . . ? C17 C16 C15 120.0 . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 O6 114.3(10) . . ? C19 C18 O6 125.4(10) . . ? C20 C19 C18 120.0 . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C15 120.0 . . ? C19 C20 H20A 120.0 . . ? C15 C20 H20A 120.0 . . ? C23 C22 C27 120.0 . . ? C23 C22 P4 118.6(6) . . ? C27 C22 P4 121.4(6) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? O8 C25 C26 113.2(10) . . ? O8 C25 C24 126.7(10) . . ? C26 C25 C24 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 H27A 120.0 . . ? C22 C27 H27A 120.0 . . ? O8 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 O9 C32 112.3(16) . . ? C29 O9 Ni3 124.0(10) . . ? C32 O9 Ni3 119.6(12) . . ? O9 C29 C30 106.0(16) . . ? O9 C29 H29A 110.5 . . ? C30 C29 H29A 110.5 . . ? O9 C29 H29B 110.5 . . ? C30 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C31 C30 C29 97.6(19) . . ? C31 C30 H30A 112.2 . . ? C29 C30 H30A 112.2 . . ? C31 C30 H30B 112.2 . . ? C29 C30 H30B 112.2 . . ? H30A C30 H30B 109.8 . . ? C30 C31 C32 105.1(17) . . ? C30 C31 H31A 110.7 . . ? C32 C31 H31A 110.7 . . ? C30 C31 H31B 110.7 . . ? C32 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? O9 C32 C31 101.0(19) . . ? O9 C32 H32A 111.6 . . ? C31 C32 H32A 111.6 . . ? O9 C32 H32B 111.6 . . ? C31 C32 H32B 111.6 . . ? H32A C32 H32B 109.4 . . ? C33 O10 C36 110.8(16) . . ? C33 O10 Ni3 126.0(15) . . ? C36 O10 Ni3 120.8(11) . . ? C34 C33 O10 104(2) . . ? C34 C33 H33A 110.9 . . ? O10 C33 H33A 110.9 . . ? C34 C33 H33B 110.9 . . ? O10 C33 H33B 110.9 . . ? H33A C33 H33B 108.9 . . ? C35 C34 C33 107(3) . . ? C35 C34 H34A 110.4 . . ? C33 C34 H34A 110.4 . . ? C35 C34 H34B 110.4 . . ? C33 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? C34 C35 C36 114(2) . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C35 C36 O10 97(2) . . ? C35 C36 H36A 112.3 . . ? O10 C36 H36A 112.3 . . ? C35 C36 H36B 112.3 . . ? O10 C36 H36B 112.3 . . ? H36A C36 H36B 109.9 . . ? C37 O11 C40 116.1(17) . . ? C37 O11 Ni4 119.8(12) . . ? C40 O11 Ni4 123.2(13) . . ? O11 C37 C38 98.4(15) . . ? O11 C37 H37A 112.1 . . ? C38 C37 H37A 112.1 . . ? O11 C37 H37B 112.1 . . ? C38 C37 H37B 112.1 . . ? H37A C37 H37B 109.7 . . ? C39 C38 C37 101.1(18) . . ? C39 C38 H38A 111.6 . . ? C37 C38 H38A 111.6 . . ? C39 C38 H38B 111.6 . . ? C37 C38 H38B 111.6 . . ? H38A C38 H38B 109.4 . . ? C38 C39 C40 100(2) . . ? C38 C39 H39A 111.8 . . ? C40 C39 H39A 111.8 . . ? C38 C39 H39B 111.8 . . ? C40 C39 H39B 111.8 . . ? H39A C39 H39B 109.5 . . ? O11 C40 C39 104.5(19) . . ? O11 C40 H40A 110.8 . . ? C39 C40 H40A 110.8 . . ? O11 C40 H40B 110.8 . . ? C39 C40 H40B 110.8 . . ? H40A C40 H40B 108.9 . . ? C41 O12 C44 114.2(15) . . ? C41 O12 Ni4 122.8(12) . . ? C44 O12 Ni4 122.2(13) . . ? O12 C41 C42 104.3(14) . . ? O12 C41 H41A 110.9 . . ? C42 C41 H41A 110.9 . . ? O12 C41 H41B 110.9 . . ? C42 C41 H41B 110.9 . . ? H41A C41 H41B 108.9 . . ? C43 C42 C41 103.7(15) . . ? C43 C42 H42A 111.0 . . ? C41 C42 H42A 111.0 . . ? C43 C42 H42B 111.0 . . ? C41 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? C42 C43 C44 100(2) . . ? C42 C43 H43A 111.8 . . ? C44 C43 H43A 111.8 . . ? C42 C43 H43B 111.8 . . ? C44 C43 H43B 111.8 . . ? H43A C43 H43B 109.6 . . ? O12 C44 C43 105.8(18) . . ? O12 C44 H44A 110.6 . . ? C43 C44 H44A 110.6 . . ? O12 C44 H44B 110.6 . . ? C43 C44 H44B 110.6 . . ? H44A C44 H44B 108.7 . . ? C18 O6 C21 113.4(14) . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H131 S6 0.87(4) 2.45(5) 3.196(14) 145(9) . O13 H132 S2 0.89(4) 2.46(5) 3.263(13) 150(10) . O14 H141 S1 0.92(4) 2.50(5) 3.232(16) 137(7) . O14 H142 S5 0.93(4) 2.49(5) 3.257(15) 140(8) . O15 H151 S8 0.89(4) 2.45(5) 3.165(13) 138(8) . O15 H152 S4 0.89(4) 2.48(5) 3.217(15) 141(8) . O16 H161 S7 0.90(4) 2.48(5) 3.311(12) 153(10) . O16 H162 S3 0.92(4) 2.50(5) 3.329(13) 151(9) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.370 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.282