# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name B.Singh M.Drew G.Kociok-Kohn K.Molloy N.Singh _publ_contact_author_name 'Nanhai Singh' _publ_contact_author_email nsingh@bhu.ac.in data_complex1 _database_code_depnum_ccdc_archive 'CCDC 745652' #TrackingRef '- CIF_ALL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H87 Cu2 N O7 P4 S3' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 293(2) _chemical_formula_weight 1581.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 19.785(2) _cell_length_b 16.651(2) _cell_length_c 24.213(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.180(2) _cell_angle_gamma 90.00 _cell_volume 7955.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6369 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.51 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51499 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.1028 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.40 _reflns_number_total 19704 _reflns_number_gt 11621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep3 _computing_publication_material ? _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^)+(0.1098P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 19704 _refine_ls_number_parameters 921 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1319 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2209 _refine_ls_wR_factor_gt 0.1691 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.25632(3) 0.89004(3) 0.31693(2) 0.02501(15) Uani 1 1 d . . . Cu2 Cu 1.22224(2) 0.63426(3) 0.40496(2) 0.02187(15) Uani 1 1 d . . . S1 S 1.22347(6) 0.74637(6) 0.46663(5) 0.0251(3) Uani 1 1 d . . . S2 S 1.24089(5) 0.75154(6) 0.34742(5) 0.0241(2) Uani 1 1 d . . . P3 P 1.31535(5) 0.55830(7) 0.42065(5) 0.0234(3) Uani 1 1 d . . . S3 S 1.22827(6) 0.94435(7) 0.45316(5) 0.0290(3) Uani 1 1 d . . . P4 P 1.12236(5) 0.57980(7) 0.37578(5) 0.0203(2) Uani 1 1 d . . . P2 P 1.16679(6) 0.93431(6) 0.26362(5) 0.0224(3) Uani 1 1 d . . . P1 P 1.36380(6) 0.91104(7) 0.29734(5) 0.0277(3) Uani 1 1 d . . . O1 O 1.28370(16) 0.93551(19) 0.49467(13) 0.0333(8) Uani 1 1 d . . . C8 C 1.2325(2) 0.8018(3) 0.40851(19) 0.0254(10) Uani 1 1 d . . . C75 C 1.0514(2) 0.5986(3) 0.41724(19) 0.0238(9) Uani 1 1 d . . . C33 C 1.1526(2) 0.8875(2) 0.19546(18) 0.0232(9) Uani 1 1 d . . . C51 C 1.3413(2) 0.4987(3) 0.36243(19) 0.0258(10) Uani 1 1 d . . . C28 C 1.1995(2) 1.0926(3) 0.2878(2) 0.0274(10) Uani 1 1 d . . . H28 H 1.2116 1.0725 0.3230 0.033 Uiso 1 1 calc R . . C15 C 1.3740(2) 0.9598(3) 0.23104(19) 0.0263(10) Uani 1 1 d . . . C34 C 1.0888(2) 0.8830(3) 0.16768(19) 0.0268(10) Uani 1 1 d . . . H34 H 1.0514 0.9027 0.1845 0.032 Uiso 1 1 calc R . . C64 C 1.1424(2) 0.4215(3) 0.40866(19) 0.0257(10) Uani 1 1 d . . . H64 H 1.1584 0.4440 0.4423 0.031 Uiso 1 1 calc R . . C71 C 1.1128(2) 0.6719(3) 0.21912(19) 0.0282(10) Uani 1 1 d . . . H71 H 1.1437 0.6834 0.1930 0.034 Uiso 1 1 calc R . . C44 C 1.0668(2) 0.8463(3) 0.31149(19) 0.0248(10) Uani 1 1 d . . . H44 H 1.0961 0.8031 0.3084 0.030 Uiso 1 1 calc R . . C70 C 1.1346(2) 0.6369(3) 0.26858(19) 0.0255(10) Uani 1 1 d . . . H70 H 1.1803 0.6246 0.2757 0.031 Uiso 1 1 calc R . . C45 C 1.3921(2) 0.6105(3) 0.44713(19) 0.0255(10) Uani 1 1 d . . . C27 C 1.1718(2) 1.0417(2) 0.24667(18) 0.0213(9) Uani 1 1 d . . . C67 C 1.0955(2) 0.3537(3) 0.3094(2) 0.0310(11) Uani 1 1 d . . . H67 H 1.0794 0.3310 0.2759 0.037 Uiso 1 1 calc R . . C69 C 1.0894(2) 0.6197(2) 0.30813(18) 0.0213(9) Uani 1 1 d . . . C65 C 1.1424(2) 0.3383(3) 0.4024(2) 0.0287(10) Uani 1 1 d . . . H65 H 1.1580 0.3055 0.4317 0.034 Uiso 1 1 calc R . . C32 C 1.1534(2) 1.0721(2) 0.19496(18) 0.0230(9) Uani 1 1 d . . . H32 H 1.1343 1.0384 0.1674 0.028 Uiso 1 1 calc R . . C31 C 1.1632(2) 1.1532(3) 0.1835(2) 0.0273(10) Uani 1 1 d . . . H31 H 1.1509 1.1735 0.1484 0.033 Uiso 1 1 calc R . . C73 C 0.9995(2) 0.6730(2) 0.24673(19) 0.0266(10) Uani 1 1 d . . . H73 H 0.9539 0.6850 0.2393 0.032 Uiso 1 1 calc R . . C5 C 1.1529(2) 0.9240(3) 0.48476(19) 0.0289(10) Uani 1 1 d . . . C7 C 1.0319(3) 0.9107(3) 0.4787(2) 0.0333(11) Uani 1 1 d . . . H7 H 0.9907 0.9130 0.4578 0.040 Uiso 1 1 calc R . . N1 N 1.23407(19) 0.8822(2) 0.40252(15) 0.0260(8) Uani 1 1 d . . . C68 C 1.0957(2) 0.4364(3) 0.3155(2) 0.0276(10) Uani 1 1 d . . . H68 H 1.0803 0.4688 0.2860 0.033 Uiso 1 1 calc R . . C66 C 1.1189(2) 0.3051(3) 0.3525(2) 0.0280(10) Uani 1 1 d . . . H66 H 1.1188 0.2496 0.3481 0.034 Uiso 1 1 calc R . . C41 C 0.9799(2) 0.9753(3) 0.32233(19) 0.0283(10) Uani 1 1 d . . . H41 H 0.9508 1.0185 0.3258 0.034 Uiso 1 1 calc R . . C61 C 1.2431(2) 0.4563(3) 0.5570(2) 0.0324(11) Uani 1 1 d . . . H61 H 1.2199 0.4745 0.5866 0.039 Uiso 1 1 calc R . . C39 C 1.0849(2) 0.9233(2) 0.29368(18) 0.0224(9) Uani 1 1 d . . . C4 C 1.1546(3) 0.9060(3) 0.5411(2) 0.0348(11) Uani 1 1 d . . . H4 H 1.1957 0.9040 0.5622 0.042 Uiso 1 1 calc R . . C30 C 1.1911(2) 1.2028(3) 0.2242(2) 0.0333(11) Uani 1 1 d . . . H30 H 1.1980 1.2568 0.2166 0.040 Uiso 1 1 calc R . . C6 C 1.0909(2) 0.9257(3) 0.45350(19) 0.0303(11) Uani 1 1 d . . . H6 H 1.0894 0.9370 0.4158 0.036 Uiso 1 1 calc R . . C42 C 0.9609(2) 0.8995(3) 0.33886(19) 0.0270(10) Uani 1 1 d . . . H42 H 0.9191 0.8916 0.3533 0.032 Uiso 1 1 calc R . . C80 C 1.0008(2) 0.5416(3) 0.42480(19) 0.0250(10) Uani 1 1 d . . . H80 H 1.0059 0.4892 0.4124 0.030 Uiso 1 1 calc R . . C2 C 1.0326(3) 0.8923(3) 0.5347(2) 0.0299(11) Uani 1 1 d . . . C57 C 1.2993(2) 0.4841(3) 0.47379(19) 0.0256(10) Uani 1 1 d . . . C63 C 1.1190(2) 0.4712(2) 0.36574(18) 0.0213(9) Uani 1 1 d . . . C76 C 1.0432(2) 0.6754(3) 0.43799(19) 0.0274(10) Uani 1 1 d . . . H76 H 1.0774 0.7132 0.4351 0.033 Uiso 1 1 calc R . . C38 C 1.2079(2) 0.8562(3) 0.17020(19) 0.0296(11) Uani 1 1 d . . . H38 H 1.2508 0.8578 0.1887 0.036 Uiso 1 1 calc R . . C79 C 0.9429(2) 0.5630(3) 0.45072(19) 0.0275(10) Uani 1 1 d . . . H79 H 0.9097 0.5248 0.4559 0.033 Uiso 1 1 calc R . . C58 C 1.3128(2) 0.4022(3) 0.4687(2) 0.0282(10) Uani 1 1 d . . . H58 H 1.3366 0.3839 0.4395 0.034 Uiso 1 1 calc R . . C72 C 1.0447(2) 0.6902(2) 0.20819(19) 0.0268(10) Uani 1 1 d . . . H72 H 1.0298 0.7140 0.1748 0.032 Uiso 1 1 calc R . . C74 C 1.0216(2) 0.6375(2) 0.29705(19) 0.0241(9) Uani 1 1 d . . . H74 H 0.9907 0.6258 0.3231 0.029 Uiso 1 1 calc R . . C29 C 1.2091(2) 1.1734(3) 0.2765(2) 0.0318(11) Uani 1 1 d . . . H29 H 1.2275 1.2075 0.3041 0.038 Uiso 1 1 calc R . . C3 C 1.0949(3) 0.8911(3) 0.5653(2) 0.0353(12) Uani 1 1 d . . . H3 H 1.0963 0.8801 0.6030 0.042 Uiso 1 1 calc R . . C60 C 1.2566(2) 0.3750(3) 0.5509(2) 0.0370(12) Uani 1 1 d . . . H60 H 1.2423 0.3383 0.5766 0.044 Uiso 1 1 calc R . . C40 C 1.0423(2) 0.9871(3) 0.30051(18) 0.0249(10) Uani 1 1 d . . . H40 H 1.0552 1.0384 0.2905 0.030 Uiso 1 1 calc R . . C16 C 1.3494(2) 1.0386(3) 0.2229(2) 0.0317(11) Uani 1 1 d . . . H16 H 1.3282 1.0639 0.2511 0.038 Uiso 1 1 calc R . . C21 C 1.4159(2) 0.8218(3) 0.2926(2) 0.0334(11) Uani 1 1 d . . . C78 C 0.9350(2) 0.6400(3) 0.4685(2) 0.0311(11) Uani 1 1 d . . . H78 H 0.8955 0.6545 0.4845 0.037 Uiso 1 1 calc R . . C46 C 1.4057(2) 0.6850(3) 0.4244(2) 0.0342(12) Uani 1 1 d . . . H46 H 1.3759 0.7066 0.3968 0.041 Uiso 1 1 calc R . . C18 C 1.3872(2) 1.0403(4) 0.1316(2) 0.0415(14) Uani 1 1 d . . . H18 H 1.3926 1.0674 0.0986 0.050 Uiso 1 1 calc R . . C36 C 1.1362(2) 0.8195(3) 0.0905(2) 0.0318(11) Uani 1 1 d . . . H36 H 1.1308 0.7969 0.0553 0.038 Uiso 1 1 calc R . . C20 C 1.4036(2) 0.9224(3) 0.1878(2) 0.0332(11) Uani 1 1 d . . . H20 H 1.4196 0.8700 0.1919 0.040 Uiso 1 1 calc R . . C49 C 1.4944(2) 0.6229(3) 0.5063(2) 0.0368(12) Uani 1 1 d . . . H49 H 1.5242 0.6017 0.5340 0.044 Uiso 1 1 calc R . . C62 C 1.2648(2) 0.5096(3) 0.51843(19) 0.0288(10) Uani 1 1 d . . . H62 H 1.2559 0.5641 0.5224 0.035 Uiso 1 1 calc R . . C26 C 1.3855(3) 0.7534(3) 0.2693(2) 0.0366(12) Uani 1 1 d . . . H26 H 1.3396 0.7544 0.2578 0.044 Uiso 1 1 calc R . . C50 C 1.4365(2) 0.5795(3) 0.48860(19) 0.0291(10) Uani 1 1 d . . . H50 H 1.4278 0.5301 0.5045 0.035 Uiso 1 1 calc R . . C17 C 1.3561(2) 1.0786(3) 0.1741(2) 0.0365(12) Uani 1 1 d . . . H17 H 1.3401 1.1309 0.1695 0.044 Uiso 1 1 calc R . . C9 C 1.4144(2) 0.9746(3) 0.3468(2) 0.0324(11) Uani 1 1 d . . . C14 C 1.4017(2) 0.9679(3) 0.4027(2) 0.0378(12) Uani 1 1 d . . . H14 H 1.3689 0.9323 0.4136 0.045 Uiso 1 1 calc R . . C35 C 1.0802(2) 0.8494(3) 0.1151(2) 0.0287(10) Uani 1 1 d . . . H35 H 1.0373 0.8470 0.0966 0.034 Uiso 1 1 calc R . . C59 C 1.2910(2) 0.3484(3) 0.5070(2) 0.0361(12) Uani 1 1 d . . . H59 H 1.2997 0.2939 0.5030 0.043 Uiso 1 1 calc R . . C37 C 1.1997(3) 0.8228(3) 0.1178(2) 0.0388(12) Uani 1 1 d . . . H37 H 1.2370 0.8027 0.1011 0.047 Uiso 1 1 calc R . . C54 C 1.3704(3) 0.4098(4) 0.2696(2) 0.0477(15) Uani 1 1 d . . . H54 H 1.3804 0.3806 0.2384 0.057 Uiso 1 1 calc R . . C43 C 1.0047(2) 0.8358(3) 0.33372(19) 0.0286(10) Uani 1 1 d . . . H43 H 0.9924 0.7850 0.3454 0.034 Uiso 1 1 calc R . . C10 C 1.4644(2) 1.0271(3) 0.3317(2) 0.0414(13) Uani 1 1 d . . . H10 H 1.4734 1.0316 0.2947 0.050 Uiso 1 1 calc R . . C22 C 1.4839(2) 0.8189(3) 0.3094(2) 0.0386(12) Uani 1 1 d . . . H22 H 1.5051 0.8645 0.3245 0.046 Uiso 1 1 calc R . . C56 C 1.2912(3) 0.4541(3) 0.3327(2) 0.0421(14) Uani 1 1 d . . . H56 H 1.2471 0.4548 0.3435 0.051 Uiso 1 1 calc R . . C13 C 1.4385(3) 1.0148(4) 0.4421(2) 0.0482(15) Uani 1 1 d . . . H13 H 1.4295 1.0107 0.4792 0.058 Uiso 1 1 calc R . . C47 C 1.4636(3) 0.7270(3) 0.4426(2) 0.0428(13) Uani 1 1 d . . . H47 H 1.4726 0.7768 0.4273 0.051 Uiso 1 1 calc R . . C77 C 0.9851(2) 0.6966(3) 0.4628(2) 0.0340(11) Uani 1 1 d . . . H77 H 0.9798 0.7487 0.4757 0.041 Uiso 1 1 calc R . . C11 C 1.5012(3) 1.0729(4) 0.3715(2) 0.0488(15) Uani 1 1 d . . . H11 H 1.5347 1.1077 0.3610 0.059 Uiso 1 1 calc R . . C19 C 1.4096(3) 0.9634(4) 0.1380(2) 0.0482(15) Uani 1 1 d . . . H19 H 1.4290 0.9379 0.1089 0.058 Uiso 1 1 calc R . . C52 C 1.4057(3) 0.4984(3) 0.3448(2) 0.0405(13) Uani 1 1 d . . . H52 H 1.4399 0.5278 0.3640 0.049 Uiso 1 1 calc R . . C48 C 1.5083(2) 0.6945(3) 0.4842(2) 0.0390(13) Uani 1 1 d . . . H48 H 1.5474 0.7222 0.4964 0.047 Uiso 1 1 calc R . . C53 C 1.4199(3) 0.4544(4) 0.2983(3) 0.0557(16) Uani 1 1 d . . . H53 H 1.4635 0.4551 0.2864 0.067 Uiso 1 1 calc R . . C25 C 1.4228(3) 0.6825(3) 0.2630(2) 0.0455(14) Uani 1 1 d . . . H25 H 1.4023 0.6371 0.2470 0.055 Uiso 1 1 calc R . . C24 C 1.4899(3) 0.6820(4) 0.2807(3) 0.0538(16) Uani 1 1 d . . . H24 H 1.5152 0.6355 0.2770 0.065 Uiso 1 1 calc R . . C23 C 1.5210(3) 0.7499(3) 0.3043(2) 0.0455(14) Uani 1 1 d . . . H23 H 1.5667 0.7487 0.3165 0.055 Uiso 1 1 calc R . . C12 C 1.4877(3) 1.0668(4) 0.4270(3) 0.0512(15) Uani 1 1 d . . . H12 H 1.5119 1.0977 0.4537 0.061 Uiso 1 1 calc R . . C55 C 1.3064(3) 0.4090(4) 0.2874(3) 0.0519(16) Uani 1 1 d . . . H55 H 1.2729 0.3778 0.2690 0.062 Uiso 1 1 calc R . . O2 O 1.22019(17) 1.02174(18) 0.42722(14) 0.0373(8) Uani 1 1 d . . . O7 O 1.3350(2) 0.8299(3) 0.57977(18) 0.0633(12) Uani 1 1 d . . . H7A H 1.3066 0.8316 0.5534 0.095 Uiso 1 1 calc R . . C1 C 0.9679(3) 0.8741(3) 0.5616(2) 0.0379(12) Uani 1 1 d . . . H1A H 0.9654 0.8176 0.5690 0.057 Uiso 1 1 calc R . . H1B H 0.9297 0.8898 0.5372 0.057 Uiso 1 1 calc R . . H1C H 0.9673 0.9034 0.5957 0.057 Uiso 1 1 calc R . . O4 O 1.3302(2) 0.9468(3) 0.6568(2) 0.0636(12) Uani 1 1 d . . . H4A H 1.3413 0.9087 0.6380 0.095 Uiso 1 1 calc R . . O3 O 1.3439(3) 1.3945(3) 0.1278(2) 0.0760(14) Uani 1 1 d . . . H3A H 1.3350 1.4414 0.1347 0.114 Uiso 1 1 calc R . . O6 O 1.2117(3) 1.3207(3) 0.1120(2) 0.0840(15) Uani 1 1 d . . . H6A H 1.2368 1.3556 0.1259 0.126 Uiso 1 1 calc R . . C85 C 1.3731(3) 0.7607(4) 0.5769(3) 0.0525(16) Uani 1 1 d . . . H85A H 1.4138 0.7723 0.5591 0.079 Uiso 1 1 calc R . . H85B H 1.3473 0.7207 0.5559 0.079 Uiso 1 1 calc R . . H85C H 1.3847 0.7409 0.6136 0.079 Uiso 1 1 calc R . . C81 C 1.3743(4) 1.3903(5) 0.0750(3) 0.073(2) Uani 1 1 d . . . H81A H 1.3484 1.4224 0.0482 0.109 Uiso 1 1 calc R . . H81B H 1.3746 1.3356 0.0626 0.109 Uiso 1 1 calc R . . H81C H 1.4199 1.4102 0.0793 0.109 Uiso 1 1 calc R . . C82 C 1.2720(3) 0.9255(5) 0.6852(3) 0.078(2) Uani 1 1 d . . . H82A H 1.2803 0.9371 0.7239 0.117 Uiso 1 1 calc R . . H82B H 1.2630 0.8692 0.6803 0.117 Uiso 1 1 calc R . . H82C H 1.2337 0.9559 0.6703 0.117 Uiso 1 1 calc R . . C84 C 1.1853(3) 1.3459(5) 0.0606(3) 0.070(2) Uani 1 1 d . . . H84A H 1.1880 1.4033 0.0584 0.106 Uiso 1 1 calc R . . H84B H 1.1389 1.3293 0.0551 0.106 Uiso 1 1 calc R . . H84C H 1.2108 1.3224 0.0325 0.106 Uiso 1 1 calc R . . O O 1.2595(3) 0.1834(3) 0.4195(2) 0.0900(16) Uiso 1 1 d . . . H0 H 1.2569 0.1519 0.4452 0.135 Uiso 1 1 calc R . . C C 1.3278(4) 0.1863(4) 0.4041(3) 0.080(2) Uiso 1 1 d . . . H0A H 1.3361 0.2372 0.3874 0.119 Uiso 1 1 calc R . . H0B H 1.3349 0.1440 0.3782 0.119 Uiso 1 1 calc R . . H0C H 1.3583 0.1795 0.4365 0.119 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 0.0273(3) 0.0264(3) 0.0222(3) 0.0050(2) 0.0077(2) 0.0034(2) Cu2 0.0201(3) 0.0216(3) 0.0241(3) 0.0013(2) 0.0032(2) 0.0010(2) S1 0.0325(6) 0.0236(6) 0.0203(6) 0.0013(5) 0.0087(5) 0.0001(5) S2 0.0298(6) 0.0222(5) 0.0209(6) 0.0017(4) 0.0063(5) 0.0011(4) P3 0.0204(5) 0.0278(6) 0.0224(6) 0.0034(5) 0.0046(5) 0.0037(5) S3 0.0415(7) 0.0236(6) 0.0231(6) -0.0005(5) 0.0112(5) -0.0014(5) P4 0.0196(5) 0.0190(5) 0.0225(6) 0.0008(4) 0.0025(4) 0.0005(4) P2 0.0270(6) 0.0189(6) 0.0220(6) 0.0017(5) 0.0060(5) 0.0025(4) P1 0.0278(6) 0.0335(7) 0.0225(6) 0.0053(5) 0.0069(5) 0.0048(5) O1 0.0422(19) 0.0325(19) 0.0253(18) -0.0039(14) 0.0043(15) -0.0048(15) C8 0.028(2) 0.023(2) 0.025(3) 0.0077(19) 0.0070(19) -0.0006(18) C75 0.023(2) 0.025(2) 0.024(2) 0.0046(19) 0.0038(18) 0.0038(18) C33 0.031(2) 0.019(2) 0.020(2) 0.0006(17) 0.0048(19) -0.0016(18) C51 0.021(2) 0.033(3) 0.024(2) 0.004(2) 0.0085(18) 0.0045(19) C28 0.028(2) 0.028(2) 0.026(3) 0.000(2) 0.006(2) 0.0032(19) C15 0.017(2) 0.039(3) 0.024(2) 0.002(2) 0.0048(18) 0.0005(19) C34 0.033(2) 0.021(2) 0.028(3) 0.0005(19) 0.013(2) 0.0028(19) C64 0.025(2) 0.026(2) 0.026(2) -0.0022(19) 0.0025(19) 0.0003(18) C71 0.037(3) 0.026(2) 0.022(2) -0.0005(19) 0.009(2) -0.011(2) C44 0.026(2) 0.023(2) 0.026(3) -0.0014(19) 0.0039(19) 0.0032(18) C70 0.029(2) 0.024(2) 0.024(2) -0.0041(19) 0.0020(19) -0.0021(18) C45 0.024(2) 0.026(2) 0.027(3) 0.0019(19) 0.0084(19) 0.0014(18) C27 0.021(2) 0.020(2) 0.024(2) 0.0022(18) 0.0079(17) 0.0004(17) C67 0.038(3) 0.023(2) 0.032(3) -0.006(2) 0.002(2) -0.002(2) C69 0.028(2) 0.016(2) 0.021(2) 0.0024(17) 0.0037(18) -0.0032(17) C65 0.027(2) 0.026(2) 0.033(3) 0.006(2) 0.005(2) 0.0030(19) C32 0.028(2) 0.020(2) 0.022(2) -0.0032(18) 0.0079(18) -0.0021(18) C31 0.032(2) 0.022(2) 0.029(3) 0.0065(19) 0.009(2) 0.0010(19) C73 0.030(2) 0.018(2) 0.031(3) -0.0031(19) 0.000(2) 0.0004(18) C5 0.043(3) 0.023(2) 0.022(2) 0.0012(19) 0.010(2) 0.008(2) C7 0.043(3) 0.032(3) 0.025(3) -0.006(2) 0.010(2) -0.002(2) N1 0.034(2) 0.0232(19) 0.021(2) -0.0002(15) 0.0085(17) 0.0005(16) C68 0.032(2) 0.024(2) 0.026(3) 0.0032(19) 0.003(2) 0.0033(19) C66 0.030(2) 0.018(2) 0.037(3) 0.000(2) 0.011(2) 0.0027(18) C41 0.033(2) 0.024(2) 0.029(3) 0.002(2) 0.007(2) 0.0109(19) C61 0.025(2) 0.049(3) 0.024(3) 0.002(2) 0.004(2) 0.000(2) C39 0.028(2) 0.021(2) 0.019(2) -0.0028(17) 0.0043(18) 0.0005(18) C4 0.043(3) 0.034(3) 0.027(3) -0.002(2) 0.005(2) 0.006(2) C30 0.032(3) 0.021(2) 0.047(3) 0.003(2) 0.010(2) -0.003(2) C6 0.050(3) 0.025(2) 0.016(2) -0.0016(19) 0.007(2) 0.000(2) C42 0.024(2) 0.032(3) 0.026(3) -0.001(2) 0.0092(19) 0.0017(19) C80 0.024(2) 0.026(2) 0.025(3) 0.0040(19) 0.0032(19) 0.0013(18) C2 0.044(3) 0.022(2) 0.026(3) -0.0065(19) 0.017(2) 0.004(2) C57 0.016(2) 0.035(3) 0.026(3) 0.003(2) 0.0007(18) 0.0012(18) C63 0.019(2) 0.020(2) 0.026(2) -0.0005(18) 0.0097(18) 0.0001(17) C76 0.028(2) 0.025(2) 0.030(3) -0.003(2) 0.006(2) 0.0023(19) C38 0.026(2) 0.038(3) 0.026(3) -0.005(2) 0.010(2) 0.002(2) C79 0.023(2) 0.028(2) 0.032(3) 0.009(2) 0.0104(19) -0.0022(19) C58 0.028(2) 0.032(3) 0.025(3) 0.003(2) 0.0002(19) 0.004(2) C72 0.038(3) 0.016(2) 0.025(3) -0.0009(18) 0.000(2) -0.0030(19) C74 0.027(2) 0.017(2) 0.028(3) -0.0031(18) -0.0003(19) 0.0025(17) C29 0.035(3) 0.025(2) 0.036(3) -0.006(2) 0.004(2) -0.007(2) C3 0.047(3) 0.036(3) 0.025(3) 0.003(2) 0.016(2) 0.016(2) C60 0.031(3) 0.040(3) 0.038(3) 0.013(2) -0.005(2) -0.006(2) C40 0.032(2) 0.022(2) 0.021(2) 0.0034(18) 0.0046(19) 0.0034(18) C16 0.031(2) 0.035(3) 0.030(3) 0.002(2) 0.005(2) -0.004(2) C21 0.036(3) 0.038(3) 0.028(3) 0.008(2) 0.014(2) 0.002(2) C78 0.025(2) 0.041(3) 0.029(3) 0.005(2) 0.008(2) 0.003(2) C46 0.022(2) 0.045(3) 0.036(3) 0.012(2) 0.000(2) 0.000(2) C18 0.030(3) 0.066(4) 0.027(3) 0.020(3) 0.000(2) -0.003(3) C36 0.046(3) 0.026(2) 0.024(3) -0.006(2) 0.009(2) -0.001(2) C20 0.029(2) 0.042(3) 0.030(3) 0.008(2) 0.010(2) 0.005(2) C49 0.027(2) 0.044(3) 0.039(3) 0.000(2) 0.001(2) 0.002(2) C62 0.024(2) 0.037(3) 0.025(3) 0.003(2) 0.0024(19) 0.001(2) C26 0.033(3) 0.048(3) 0.030(3) 0.005(2) 0.011(2) 0.004(2) C50 0.026(2) 0.034(3) 0.027(3) 0.001(2) 0.001(2) 0.004(2) C17 0.034(3) 0.035(3) 0.040(3) 0.017(2) 0.000(2) -0.010(2) C9 0.033(3) 0.040(3) 0.024(3) 0.002(2) 0.004(2) 0.001(2) C14 0.031(3) 0.056(3) 0.028(3) 0.002(2) 0.009(2) 0.001(2) C35 0.038(3) 0.020(2) 0.029(3) 0.0018(19) 0.005(2) -0.0016(19) C59 0.033(3) 0.033(3) 0.040(3) 0.008(2) -0.005(2) -0.003(2) C37 0.038(3) 0.041(3) 0.039(3) -0.008(2) 0.017(2) 0.000(2) C54 0.052(3) 0.062(4) 0.031(3) -0.015(3) 0.011(3) 0.016(3) C43 0.038(3) 0.021(2) 0.027(3) -0.0002(19) 0.007(2) -0.002(2) C10 0.039(3) 0.054(3) 0.032(3) 0.005(3) 0.003(2) -0.010(3) C22 0.033(3) 0.044(3) 0.039(3) -0.002(2) 0.004(2) 0.010(2) C56 0.029(3) 0.057(4) 0.041(3) -0.020(3) 0.009(2) 0.005(2) C13 0.044(3) 0.073(4) 0.027(3) -0.008(3) -0.002(2) -0.003(3) C47 0.040(3) 0.046(3) 0.043(3) 0.010(3) 0.005(2) -0.013(2) C77 0.037(3) 0.030(3) 0.036(3) -0.002(2) 0.008(2) 0.005(2) C11 0.043(3) 0.059(4) 0.043(4) 0.004(3) -0.004(3) -0.019(3) C19 0.046(3) 0.074(4) 0.025(3) 0.009(3) 0.011(2) 0.010(3) C52 0.032(3) 0.056(3) 0.035(3) -0.007(3) 0.014(2) 0.004(2) C48 0.027(2) 0.047(3) 0.043(3) -0.002(3) 0.003(2) -0.010(2) C53 0.042(3) 0.083(5) 0.045(4) -0.008(3) 0.022(3) 0.000(3) C25 0.048(3) 0.046(3) 0.043(3) 0.001(3) 0.013(3) 0.007(3) C24 0.058(4) 0.052(4) 0.053(4) 0.004(3) 0.018(3) 0.027(3) C23 0.036(3) 0.052(4) 0.049(4) 0.004(3) 0.006(3) 0.010(3) C12 0.043(3) 0.064(4) 0.045(4) -0.008(3) -0.008(3) -0.008(3) C55 0.045(3) 0.064(4) 0.047(4) -0.027(3) 0.008(3) 0.002(3) O2 0.059(2) 0.0211(17) 0.034(2) 0.0050(15) 0.0173(17) 0.0034(15) O7 0.068(3) 0.070(3) 0.049(3) -0.006(2) -0.013(2) 0.017(2) C1 0.053(3) 0.028(3) 0.034(3) -0.007(2) 0.016(3) 0.003(2) O4 0.061(3) 0.074(3) 0.060(3) -0.007(2) 0.028(2) -0.013(2) O3 0.111(4) 0.073(3) 0.047(3) 0.004(2) 0.021(3) 0.012(3) O6 0.105(4) 0.072(4) 0.078(4) 0.020(3) 0.022(3) -0.008(3) C85 0.043(3) 0.050(4) 0.066(4) -0.005(3) 0.008(3) 0.008(3) C81 0.078(5) 0.096(6) 0.046(4) 0.007(4) 0.012(4) 0.007(4) C82 0.058(4) 0.095(6) 0.084(6) -0.017(4) 0.028(4) -0.014(4) C84 0.054(4) 0.087(5) 0.071(5) 0.014(4) 0.009(4) 0.005(4) _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 N1 2.154(4) . ? Cu1 P2 2.2391(13) . ? Cu1 P1 2.2399(13) . ? Cu1 S2 2.4472(12) . ? Cu2 P4 2.2413(12) . ? Cu2 P3 2.2441(12) . ? Cu2 S1 2.3894(12) . ? Cu2 S2 2.4426(12) . ? S1 C8 1.703(4) . ? S2 C8 1.718(5) . ? P3 C45 1.825(5) . ? P3 C57 1.829(5) . ? P3 C51 1.828(5) . ? S3 O2 1.437(3) . ? S3 O1 1.440(3) . ? S3 N1 1.615(4) . ? S3 C5 1.759(5) . ? P4 C75 1.812(4) . ? P4 C63 1.825(4) . ? P4 C69 1.842(4) . ? P2 C33 1.828(4) . ? P2 C39 1.834(4) . ? P2 C27 1.839(4) . ? P1 C21 1.817(5) . ? P1 C15 1.824(5) . ? P1 C9 1.839(5) . ? C8 N1 1.346(5) . ? C75 C76 1.387(6) . ? C75 C80 1.402(6) . ? C33 C34 1.387(6) . ? C33 C38 1.394(6) . ? C51 C52 1.374(6) . ? C51 C56 1.395(7) . ? C28 C29 1.388(6) . ? C28 C27 1.390(6) . ? C28 H28 0.9300 . ? C15 C20 1.385(6) . ? C15 C16 1.407(6) . ? C34 C35 1.390(6) . ? C34 H34 0.9300 . ? C64 C63 1.382(6) . ? C64 C65 1.394(6) . ? C64 H64 0.9300 . ? C71 C70 1.373(6) . ? C71 C72 1.388(6) . ? C71 H71 0.9300 . ? C44 C43 1.388(6) . ? C44 C39 1.406(6) . ? C44 H44 0.9300 . ? C70 C69 1.387(6) . ? C70 H70 0.9300 . ? C45 C50 1.385(6) . ? C45 C46 1.391(6) . ? C27 C32 1.375(6) . ? C67 C66 1.376(6) . ? C67 C68 1.384(6) . ? C67 H67 0.9300 . ? C69 C74 1.381(6) . ? C65 C66 1.378(6) . ? C65 H65 0.9300 . ? C32 C31 1.395(6) . ? C32 H32 0.9300 . ? C31 C30 1.372(7) . ? C31 H31 0.9300 . ? C73 C72 1.369(6) . ? C73 C74 1.396(6) . ? C73 H73 0.9300 . ? C5 C6 1.393(6) . ? C5 C4 1.394(7) . ? C7 C6 1.380(6) . ? C7 C2 1.389(7) . ? C7 H7 0.9300 . ? C68 C63 1.395(6) . ? C68 H68 0.9300 . ? C66 H66 0.9300 . ? C41 C42 1.384(6) . ? C41 C40 1.391(6) . ? C41 H41 0.9300 . ? C61 C62 1.379(6) . ? C61 C60 1.390(7) . ? C61 H61 0.9300 . ? C39 C40 1.374(6) . ? C4 C3 1.378(7) . ? C4 H4 0.9300 . ? C30 C29 1.380(7) . ? C30 H30 0.9300 . ? C6 H6 0.9300 . ? C42 C43 1.382(6) . ? C42 H42 0.9300 . ? C80 C79 1.391(6) . ? C80 H80 0.9300 . ? C2 C3 1.391(7) . ? C2 C1 1.508(6) . ? C57 C62 1.387(6) . ? C57 C58 1.395(6) . ? C76 C77 1.381(6) . ? C76 H76 0.9300 . ? C38 C37 1.384(7) . ? C38 H38 0.9300 . ? C79 C78 1.365(6) . ? C79 H79 0.9300 . ? C58 C59 1.380(7) . ? C58 H58 0.9300 . ? C72 H72 0.9300 . ? C74 H74 0.9300 . ? C29 H29 0.9300 . ? C3 H3 0.9300 . ? C60 C59 1.378(7) . ? C60 H60 0.9300 . ? C40 H40 0.9300 . ? C16 C17 1.371(7) . ? C16 H16 0.9300 . ? C21 C22 1.378(7) . ? C21 C26 1.389(7) . ? C78 C77 1.382(6) . ? C78 H78 0.9300 . ? C46 C47 1.387(7) . ? C46 H46 0.9300 . ? C18 C19 1.360(8) . ? C18 C17 1.392(8) . ? C18 H18 0.9300 . ? C36 C37 1.378(7) . ? C36 C35 1.389(6) . ? C36 H36 0.9300 . ? C20 C19 1.398(7) . ? C20 H20 0.9300 . ? C49 C48 1.342(7) . ? C49 C50 1.396(6) . ? C49 H49 0.9300 . ? C62 H62 0.9300 . ? C26 C25 1.406(7) . ? C26 H26 0.9300 . ? C50 H50 0.9300 . ? C17 H17 0.9300 . ? C9 C10 1.388(7) . ? C9 C14 1.400(7) . ? C14 C13 1.397(7) . ? C14 H14 0.9300 . ? C35 H35 0.9300 . ? C59 H59 0.9300 . ? C37 H37 0.9300 . ? C54 C55 1.369(7) . ? C54 C53 1.376(8) . ? C54 H54 0.9300 . ? C43 H43 0.9300 . ? C10 C11 1.393(7) . ? C10 H10 0.9300 . ? C22 C23 1.374(7) . ? C22 H22 0.9300 . ? C56 C55 1.380(7) . ? C56 H56 0.9300 . ? C13 C12 1.372(8) . ? C13 H13 0.9300 . ? C47 C48 1.401(7) . ? C47 H47 0.9300 . ? C77 H77 0.9300 . ? C11 C12 1.393(8) . ? C11 H11 0.9300 . ? C19 H19 0.9300 . ? C52 C53 1.389(8) . ? C52 H52 0.9300 . ? C48 H48 0.9300 . ? C53 H53 0.9300 . ? C25 C24 1.365(8) . ? C25 H25 0.9300 . ? C24 C23 1.390(8) . ? C24 H24 0.9300 . ? C23 H23 0.9300 . ? C12 H12 0.9300 . ? C55 H55 0.9300 . ? O7 C85 1.383(6) . ? O7 H7A 0.8200 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? O4 C82 1.427(7) . ? O4 H4A 0.8200 . ? O3 C81 1.454(8) . ? O3 H3A 0.8200 . ? O6 C84 1.379(8) . ? O6 H6A 0.8210 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? O C 1.427(8) . ? O H0 0.8200 . ? C H0A 0.9600 . ? C H0B 0.9600 . ? C H0C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 P2 111.48(11) . . ? N1 Cu1 P1 118.50(11) . . ? P2 Cu1 P1 123.36(5) . . ? N1 Cu1 S2 67.27(10) . . ? P2 Cu1 S2 111.92(4) . . ? P1 Cu1 S2 110.63(4) . . ? P4 Cu2 P3 121.30(5) . . ? P4 Cu2 S1 118.79(4) . . ? P3 Cu2 S1 111.33(5) . . ? P4 Cu2 S2 108.06(4) . . ? P3 Cu2 S2 113.01(4) . . ? S1 Cu2 S2 74.74(4) . . ? C8 S1 Cu2 84.51(16) . . ? C8 S2 Cu2 82.55(15) . . ? C8 S2 Cu1 79.77(15) . . ? Cu2 S2 Cu1 162.33(5) . . ? C45 P3 C57 104.9(2) . . ? C45 P3 C51 104.9(2) . . ? C57 P3 C51 104.4(2) . . ? C45 P3 Cu2 116.26(15) . . ? C57 P3 Cu2 108.53(14) . . ? C51 P3 Cu2 116.67(15) . . ? O2 S3 O1 116.8(2) . . ? O2 S3 N1 104.8(2) . . ? O1 S3 N1 111.8(2) . . ? O2 S3 C5 107.0(2) . . ? O1 S3 C5 107.7(2) . . ? N1 S3 C5 108.4(2) . . ? C75 P4 C63 102.86(19) . . ? C75 P4 C69 101.1(2) . . ? C63 P4 C69 103.39(19) . . ? C75 P4 Cu2 117.16(15) . . ? C63 P4 Cu2 117.77(14) . . ? C69 P4 Cu2 112.40(14) . . ? C33 P2 C39 103.5(2) . . ? C33 P2 C27 102.7(2) . . ? C39 P2 C27 104.44(19) . . ? C33 P2 Cu1 116.33(15) . . ? C39 P2 Cu1 115.03(15) . . ? C27 P2 Cu1 113.32(14) . . ? C21 P1 C15 102.1(2) . . ? C21 P1 C9 103.1(2) . . ? C15 P1 C9 103.1(2) . . ? C21 P1 Cu1 115.94(16) . . ? C15 P1 Cu1 115.07(14) . . ? C9 P1 Cu1 115.59(16) . . ? N1 C8 S1 129.2(4) . . ? N1 C8 S2 112.8(3) . . ? S1 C8 S2 118.0(3) . . ? C76 C75 C80 118.2(4) . . ? C76 C75 P4 118.4(3) . . ? C80 C75 P4 123.0(3) . . ? C34 C33 C38 118.9(4) . . ? C34 C33 P2 122.4(3) . . ? C38 C33 P2 118.7(3) . . ? C52 C51 C56 118.6(4) . . ? C52 C51 P3 124.1(4) . . ? C56 C51 P3 117.3(3) . . ? C29 C28 C27 120.1(4) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C20 C15 C16 118.3(4) . . ? C20 C15 P1 123.0(4) . . ? C16 C15 P1 118.6(3) . . ? C33 C34 C35 120.9(4) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C63 C64 C65 121.1(4) . . ? C63 C64 H64 119.4 . . ? C65 C64 H64 119.4 . . ? C70 C71 C72 119.9(4) . . ? C70 C71 H71 120.1 . . ? C72 C71 H71 120.1 . . ? C43 C44 C39 119.1(4) . . ? C43 C44 H44 120.5 . . ? C39 C44 H44 120.5 . . ? C71 C70 C69 120.8(4) . . ? C71 C70 H70 119.6 . . ? C69 C70 H70 119.6 . . ? C50 C45 C46 119.3(4) . . ? C50 C45 P3 123.0(3) . . ? C46 C45 P3 117.7(3) . . ? C32 C27 C28 119.5(4) . . ? C32 C27 P2 123.1(3) . . ? C28 C27 P2 117.2(3) . . ? C66 C67 C68 120.4(5) . . ? C66 C67 H67 119.8 . . ? C68 C67 H67 119.8 . . ? C74 C69 C70 119.2(4) . . ? C74 C69 P4 121.7(3) . . ? C70 C69 P4 119.0(3) . . ? C66 C65 C64 119.4(4) . . ? C66 C65 H65 120.3 . . ? C64 C65 H65 120.3 . . ? C27 C32 C31 120.4(4) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C30 C31 C32 119.6(4) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C72 C73 C74 120.4(4) . . ? C72 C73 H73 119.8 . . ? C74 C73 H73 119.8 . . ? C6 C5 C4 119.6(4) . . ? C6 C5 S3 120.0(4) . . ? C4 C5 S3 120.4(4) . . ? C6 C7 C2 121.6(5) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? C8 N1 S3 123.5(3) . . ? C8 N1 Cu1 99.9(3) . . ? S3 N1 Cu1 136.2(2) . . ? C67 C68 C63 120.4(4) . . ? C67 C68 H68 119.8 . . ? C63 C68 H68 119.8 . . ? C67 C66 C65 120.2(4) . . ? C67 C66 H66 119.9 . . ? C65 C66 H66 119.9 . . ? C42 C41 C40 120.4(4) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C62 C61 C60 118.9(5) . . ? C62 C61 H61 120.5 . . ? C60 C61 H61 120.5 . . ? C40 C39 C44 119.7(4) . . ? C40 C39 P2 122.6(3) . . ? C44 C39 P2 117.7(3) . . ? C3 C4 C5 119.6(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C31 C30 C29 120.6(4) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C7 C6 C5 119.7(4) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C41 C42 C43 119.2(4) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C79 C80 C75 120.3(4) . . ? C79 C80 H80 119.9 . . ? C75 C80 H80 119.9 . . ? C3 C2 C7 117.8(4) . . ? C3 C2 C1 121.0(4) . . ? C7 C2 C1 121.2(5) . . ? C62 C57 C58 118.4(4) . . ? C62 C57 P3 117.5(3) . . ? C58 C57 P3 123.6(4) . . ? C64 C63 C68 118.5(4) . . ? C64 C63 P4 119.1(3) . . ? C68 C63 P4 122.3(3) . . ? C77 C76 C75 121.1(4) . . ? C77 C76 H76 119.4 . . ? C75 C76 H76 119.4 . . ? C37 C38 C33 120.6(4) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C78 C79 C80 120.0(4) . . ? C78 C79 H79 120.0 . . ? C80 C79 H79 120.0 . . ? C59 C58 C57 120.2(5) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C73 C72 C71 119.8(4) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C69 C74 C73 119.9(4) . . ? C69 C74 H74 120.1 . . ? C73 C74 H74 120.1 . . ? C30 C29 C28 119.7(4) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C4 C3 C2 121.7(5) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C59 C60 C61 120.2(5) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C39 C40 C41 120.4(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C17 C16 C15 121.3(5) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C22 C21 C26 118.4(5) . . ? C22 C21 P1 123.8(4) . . ? C26 C21 P1 117.7(4) . . ? C79 C78 C77 120.7(4) . . ? C79 C78 H78 119.7 . . ? C77 C78 H78 119.7 . . ? C47 C46 C45 120.2(5) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C19 C18 C17 120.3(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C37 C36 C35 120.6(4) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C15 C20 C19 119.9(5) . . ? C15 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C48 C49 C50 121.7(5) . . ? C48 C49 H49 119.2 . . ? C50 C49 H49 119.2 . . ? C61 C62 C57 121.7(5) . . ? C61 C62 H62 119.1 . . ? C57 C62 H62 119.1 . . ? C21 C26 C25 121.1(5) . . ? C21 C26 H26 119.4 . . ? C25 C26 H26 119.5 . . ? C45 C50 C49 119.5(5) . . ? C45 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C16 C17 C18 119.4(5) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C10 C9 C14 119.1(5) . . ? C10 C9 P1 123.7(4) . . ? C14 C9 P1 117.1(4) . . ? C13 C14 C9 119.6(5) . . ? C13 C14 H14 120.2 . . ? C9 C14 H14 120.2 . . ? C34 C35 C36 119.2(4) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C60 C59 C58 120.4(5) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C36 C37 C38 119.8(5) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C55 C54 C53 119.1(5) . . ? C55 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? C42 C43 C44 121.1(4) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C9 C10 C11 120.6(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C23 C22 C21 121.4(5) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C55 C56 C51 120.8(5) . . ? C55 C56 H56 119.6 . . ? C51 C56 H56 119.6 . . ? C12 C13 C14 121.1(5) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C46 C47 C48 119.8(5) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C78 C77 C76 119.6(4) . . ? C78 C77 H77 120.2 . . ? C76 C77 H77 120.2 . . ? C12 C11 C10 120.1(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C51 C52 C53 120.0(5) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C49 C48 C47 119.5(5) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C54 C53 C52 121.1(5) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C24 C25 C26 118.5(6) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? C25 C24 C23 121.1(5) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C22 C23 C24 119.5(5) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C13 C12 C11 119.5(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C54 C55 C56 120.4(5) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C85 O7 H7A 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C82 O4 H4A 109.5 . . ? C81 O3 H3A 109.5 . . ? C84 O6 H6A 109.6 . . ? O7 C85 H85A 109.5 . . ? O7 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? O7 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? O3 C81 H81A 109.5 . . ? O3 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? O3 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O4 C82 H82A 109.5 . . ? O4 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O4 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O6 C84 H84A 109.5 . . ? O6 C84 H84B 109.6 . . ? H84A C84 H84B 109.5 . . ? O6 C84 H84C 109.4 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C O H0 109.5 . . ? O C H0A 109.5 . . ? O C H0B 109.5 . . ? H0A C H0B 109.5 . . ? O C H0C 109.5 . . ? H0A C H0C 109.5 . . ? H0B C H0C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P4 Cu2 S1 C8 -99.75(15) . . . . ? P3 Cu2 S1 C8 111.93(15) . . . . ? S2 Cu2 S1 C8 2.76(15) . . . . ? P4 Cu2 S2 C8 113.11(15) . . . . ? P3 Cu2 S2 C8 -109.83(15) . . . . ? S1 Cu2 S2 C8 -2.75(15) . . . . ? P4 Cu2 S2 Cu1 113.98(17) . . . . ? P3 Cu2 S2 Cu1 -108.96(17) . . . . ? S1 Cu2 S2 Cu1 -1.88(17) . . . . ? N1 Cu1 S2 C8 -2.80(18) . . . . ? P2 Cu1 S2 C8 -107.84(15) . . . . ? P1 Cu1 S2 C8 110.47(15) . . . . ? N1 Cu1 S2 Cu2 -3.7(2) . . . . ? P2 Cu1 S2 Cu2 -108.72(17) . . . . ? P1 Cu1 S2 Cu2 109.59(17) . . . . ? P4 Cu2 P3 C45 -177.45(17) . . . . ? S1 Cu2 P3 C45 -30.04(18) . . . . ? S2 Cu2 P3 C45 51.84(17) . . . . ? P4 Cu2 P3 C57 -59.54(17) . . . . ? S1 Cu2 P3 C57 87.87(16) . . . . ? S2 Cu2 P3 C57 169.75(16) . . . . ? P4 Cu2 P3 C51 57.94(17) . . . . ? S1 Cu2 P3 C51 -154.65(16) . . . . ? S2 Cu2 P3 C51 -72.77(17) . . . . ? P3 Cu2 P4 C75 124.11(16) . . . . ? S1 Cu2 P4 C75 -20.96(17) . . . . ? S2 Cu2 P4 C75 -103.10(16) . . . . ? P3 Cu2 P4 C63 0.54(18) . . . . ? S1 Cu2 P4 C63 -144.53(16) . . . . ? S2 Cu2 P4 C63 133.33(16) . . . . ? P3 Cu2 P4 C69 -119.47(15) . . . . ? S1 Cu2 P4 C69 95.46(15) . . . . ? S2 Cu2 P4 C69 13.32(16) . . . . ? N1 Cu1 P2 C33 -141.35(19) . . . . ? P1 Cu1 P2 C33 67.84(17) . . . . ? S2 Cu1 P2 C33 -68.16(16) . . . . ? N1 Cu1 P2 C39 -20.15(19) . . . . ? P1 Cu1 P2 C39 -170.96(15) . . . . ? S2 Cu1 P2 C39 53.04(16) . . . . ? N1 Cu1 P2 C27 99.91(18) . . . . ? P1 Cu1 P2 C27 -50.89(16) . . . . ? S2 Cu1 P2 C27 173.10(15) . . . . ? N1 Cu1 P1 C21 87.0(2) . . . . ? P2 Cu1 P1 C21 -124.11(19) . . . . ? S2 Cu1 P1 C21 12.38(19) . . . . ? N1 Cu1 P1 C15 -154.0(2) . . . . ? P2 Cu1 P1 C15 -5.11(19) . . . . ? S2 Cu1 P1 C15 131.38(17) . . . . ? N1 Cu1 P1 C9 -33.9(2) . . . . ? P2 Cu1 P1 C9 115.01(18) . . . . ? S2 Cu1 P1 C9 -108.50(18) . . . . ? Cu2 S1 C8 N1 175.7(4) . . . . ? Cu2 S1 C8 S2 -4.3(2) . . . . ? Cu2 S2 C8 N1 -175.8(3) . . . . ? Cu1 S2 C8 N1 4.5(3) . . . . ? Cu2 S2 C8 S1 4.2(2) . . . . ? Cu1 S2 C8 S1 -175.5(3) . . . . ? C63 P4 C75 C76 173.0(4) . . . . ? C69 P4 C75 C76 -80.3(4) . . . . ? Cu2 P4 C75 C76 42.1(4) . . . . ? C63 P4 C75 C80 -13.5(4) . . . . ? C69 P4 C75 C80 93.2(4) . . . . ? Cu2 P4 C75 C80 -144.3(3) . . . . ? C39 P2 C33 C34 26.3(4) . . . . ? C27 P2 C33 C34 -82.2(4) . . . . ? Cu1 P2 C33 C34 153.4(3) . . . . ? C39 P2 C33 C38 -154.6(4) . . . . ? C27 P2 C33 C38 96.9(4) . . . . ? Cu1 P2 C33 C38 -27.4(4) . . . . ? C45 P3 C51 C52 -1.1(5) . . . . ? C57 P3 C51 C52 -111.2(4) . . . . ? Cu2 P3 C51 C52 129.1(4) . . . . ? C45 P3 C51 C56 -177.7(4) . . . . ? C57 P3 C51 C56 72.2(4) . . . . ? Cu2 P3 C51 C56 -47.5(4) . . . . ? C21 P1 C15 C20 11.5(4) . . . . ? C9 P1 C15 C20 118.3(4) . . . . ? Cu1 P1 C15 C20 -114.9(4) . . . . ? C21 P1 C15 C16 -169.8(4) . . . . ? C9 P1 C15 C16 -63.0(4) . . . . ? Cu1 P1 C15 C16 63.8(4) . . . . ? C38 C33 C34 C35 -1.3(6) . . . . ? P2 C33 C34 C35 177.8(3) . . . . ? C72 C71 C70 C69 -0.2(7) . . . . ? C57 P3 C45 C50 18.4(4) . . . . ? C51 P3 C45 C50 -91.2(4) . . . . ? Cu2 P3 C45 C50 138.3(3) . . . . ? C57 P3 C45 C46 -161.3(4) . . . . ? C51 P3 C45 C46 89.0(4) . . . . ? Cu2 P3 C45 C46 -41.4(4) . . . . ? C29 C28 C27 C32 -0.6(6) . . . . ? C29 C28 C27 P2 175.5(3) . . . . ? C33 P2 C27 C32 12.1(4) . . . . ? C39 P2 C27 C32 -95.6(4) . . . . ? Cu1 P2 C27 C32 138.5(3) . . . . ? C33 P2 C27 C28 -163.8(3) . . . . ? C39 P2 C27 C28 88.4(3) . . . . ? Cu1 P2 C27 C28 -37.5(4) . . . . ? C71 C70 C69 C74 0.6(6) . . . . ? C71 C70 C69 P4 -175.5(3) . . . . ? C75 P4 C69 C74 -13.6(4) . . . . ? C63 P4 C69 C74 92.7(4) . . . . ? Cu2 P4 C69 C74 -139.3(3) . . . . ? C75 P4 C69 C70 162.4(3) . . . . ? C63 P4 C69 C70 -91.4(4) . . . . ? Cu2 P4 C69 C70 36.7(4) . . . . ? C63 C64 C65 C66 0.3(6) . . . . ? C28 C27 C32 C31 0.9(6) . . . . ? P2 C27 C32 C31 -175.0(3) . . . . ? C27 C32 C31 C30 -0.3(6) . . . . ? O2 S3 C5 C6 55.6(4) . . . . ? O1 S3 C5 C6 -178.1(3) . . . . ? N1 S3 C5 C6 -56.9(4) . . . . ? O2 S3 C5 C4 -124.4(4) . . . . ? O1 S3 C5 C4 2.0(4) . . . . ? N1 S3 C5 C4 123.1(4) . . . . ? S1 C8 N1 S3 0.8(6) . . . . ? S2 C8 N1 S3 -179.2(2) . . . . ? S1 C8 N1 Cu1 174.9(3) . . . . ? S2 C8 N1 Cu1 -5.1(3) . . . . ? O2 S3 N1 C8 -170.1(4) . . . . ? O1 S3 N1 C8 62.4(4) . . . . ? C5 S3 N1 C8 -56.2(4) . . . . ? O2 S3 N1 Cu1 18.3(4) . . . . ? O1 S3 N1 Cu1 -109.2(3) . . . . ? C5 S3 N1 Cu1 132.3(3) . . . . ? P2 Cu1 N1 C8 109.2(3) . . . . ? P1 Cu1 N1 C8 -98.4(3) . . . . ? S2 Cu1 N1 C8 3.6(2) . . . . ? P2 Cu1 N1 S3 -77.9(3) . . . . ? P1 Cu1 N1 S3 74.5(3) . . . . ? S2 Cu1 N1 S3 176.4(3) . . . . ? C66 C67 C68 C63 -0.7(7) . . . . ? C68 C67 C66 C65 0.4(7) . . . . ? C64 C65 C66 C67 -0.2(7) . . . . ? C43 C44 C39 C40 2.6(7) . . . . ? C43 C44 C39 P2 -179.1(3) . . . . ? C33 P2 C39 C40 -108.3(4) . . . . ? C27 P2 C39 C40 -1.1(4) . . . . ? Cu1 P2 C39 C40 123.7(3) . . . . ? C33 P2 C39 C44 73.4(4) . . . . ? C27 P2 C39 C44 -179.4(3) . . . . ? Cu1 P2 C39 C44 -54.5(4) . . . . ? C6 C5 C4 C3 -0.8(7) . . . . ? S3 C5 C4 C3 179.2(4) . . . . ? C32 C31 C30 C29 -0.5(7) . . . . ? C2 C7 C6 C5 -1.2(7) . . . . ? C4 C5 C6 C7 0.8(7) . . . . ? S3 C5 C6 C7 -179.2(3) . . . . ? C40 C41 C42 C43 0.3(7) . . . . ? C76 C75 C80 C79 2.3(7) . . . . ? P4 C75 C80 C79 -171.3(3) . . . . ? C6 C7 C2 C3 1.5(7) . . . . ? C6 C7 C2 C1 -178.6(4) . . . . ? C45 P3 C57 C62 83.7(4) . . . . ? C51 P3 C57 C62 -166.2(3) . . . . ? Cu2 P3 C57 C62 -41.2(4) . . . . ? C45 P3 C57 C58 -104.0(4) . . . . ? C51 P3 C57 C58 6.1(4) . . . . ? Cu2 P3 C57 C58 131.1(3) . . . . ? C65 C64 C63 C68 -0.6(6) . . . . ? C65 C64 C63 P4 -178.4(3) . . . . ? C67 C68 C63 C64 0.8(6) . . . . ? C67 C68 C63 P4 178.5(3) . . . . ? C75 P4 C63 C64 -77.1(4) . . . . ? C69 P4 C63 C64 178.0(3) . . . . ? Cu2 P4 C63 C64 53.4(4) . . . . ? C75 P4 C63 C68 105.2(4) . . . . ? C69 P4 C63 C68 0.4(4) . . . . ? Cu2 P4 C63 C68 -124.3(3) . . . . ? C80 C75 C76 C77 -3.4(7) . . . . ? P4 C75 C76 C77 170.4(4) . . . . ? C34 C33 C38 C37 1.4(7) . . . . ? P2 C33 C38 C37 -177.7(4) . . . . ? C75 C80 C79 C78 0.6(7) . . . . ? C62 C57 C58 C59 1.1(6) . . . . ? P3 C57 C58 C59 -171.2(3) . . . . ? C74 C73 C72 C71 0.2(6) . . . . ? C70 C71 C72 C73 -0.2(6) . . . . ? C70 C69 C74 C73 -0.6(6) . . . . ? P4 C69 C74 C73 175.4(3) . . . . ? C72 C73 C74 C69 0.2(6) . . . . ? C31 C30 C29 C28 0.7(7) . . . . ? C27 C28 C29 C30 -0.2(7) . . . . ? C5 C4 C3 C2 1.1(7) . . . . ? C7 C2 C3 C4 -1.4(7) . . . . ? C1 C2 C3 C4 178.7(4) . . . . ? C62 C61 C60 C59 0.1(7) . . . . ? C44 C39 C40 C41 -3.3(7) . . . . ? P2 C39 C40 C41 178.5(3) . . . . ? C42 C41 C40 C39 1.8(7) . . . . ? C20 C15 C16 C17 -1.8(7) . . . . ? P1 C15 C16 C17 179.4(4) . . . . ? C15 P1 C21 C22 89.3(5) . . . . ? C9 P1 C21 C22 -17.4(5) . . . . ? Cu1 P1 C21 C22 -144.8(4) . . . . ? C15 P1 C21 C26 -88.9(4) . . . . ? C9 P1 C21 C26 164.4(4) . . . . ? Cu1 P1 C21 C26 37.0(4) . . . . ? C80 C79 C78 C77 -2.4(7) . . . . ? C50 C45 C46 C47 0.7(7) . . . . ? P3 C45 C46 C47 -179.5(4) . . . . ? C16 C15 C20 C19 1.1(7) . . . . ? P1 C15 C20 C19 179.8(4) . . . . ? C60 C61 C62 C57 0.1(7) . . . . ? C58 C57 C62 C61 -0.7(7) . . . . ? P3 C57 C62 C61 172.0(3) . . . . ? C22 C21 C26 C25 0.1(7) . . . . ? P1 C21 C26 C25 178.4(4) . . . . ? C46 C45 C50 C49 -0.8(7) . . . . ? P3 C45 C50 C49 179.5(4) . . . . ? C48 C49 C50 C45 0.2(8) . . . . ? C15 C16 C17 C18 0.8(7) . . . . ? C19 C18 C17 C16 1.1(8) . . . . ? C21 P1 C9 C10 86.7(5) . . . . ? C15 P1 C9 C10 -19.3(5) . . . . ? Cu1 P1 C9 C10 -145.7(4) . . . . ? C21 P1 C9 C14 -92.3(4) . . . . ? C15 P1 C9 C14 161.8(4) . . . . ? Cu1 P1 C9 C14 35.3(4) . . . . ? C10 C9 C14 C13 1.1(8) . . . . ? P1 C9 C14 C13 -179.9(4) . . . . ? C33 C34 C35 C36 0.6(6) . . . . ? C37 C36 C35 C34 0.1(7) . . . . ? C61 C60 C59 C58 0.3(7) . . . . ? C57 C58 C59 C60 -0.9(7) . . . . ? C35 C36 C37 C38 0.1(7) . . . . ? C33 C38 C37 C36 -0.8(7) . . . . ? C41 C42 C43 C44 -1.0(7) . . . . ? C39 C44 C43 C42 -0.4(7) . . . . ? C14 C9 C10 C11 -0.5(8) . . . . ? P1 C9 C10 C11 -179.4(4) . . . . ? C26 C21 C22 C23 -1.1(8) . . . . ? P1 C21 C22 C23 -179.2(4) . . . . ? C52 C51 C56 C55 1.8(8) . . . . ? P3 C51 C56 C55 178.5(5) . . . . ? C9 C14 C13 C12 -0.9(8) . . . . ? C45 C46 C47 C48 -0.1(8) . . . . ? C79 C78 C77 C76 1.3(7) . . . . ? C75 C76 C77 C78 1.7(7) . . . . ? C9 C10 C11 C12 -0.3(9) . . . . ? C17 C18 C19 C20 -1.8(8) . . . . ? C15 C20 C19 C18 0.7(8) . . . . ? C56 C51 C52 C53 -0.1(8) . . . . ? P3 C51 C52 C53 -176.6(4) . . . . ? C50 C49 C48 C47 0.4(8) . . . . ? C46 C47 C48 C49 -0.5(8) . . . . ? C55 C54 C53 C52 -0.2(10) . . . . ? C51 C52 C53 C54 -0.7(9) . . . . ? C21 C26 C25 C24 0.7(8) . . . . ? C26 C25 C24 C23 -0.5(9) . . . . ? C21 C22 C23 C24 1.3(9) . . . . ? C25 C24 C23 C22 -0.5(9) . . . . ? C14 C13 C12 C11 0.0(9) . . . . ? C10 C11 C12 C13 0.6(9) . . . . ? C53 C54 C55 C56 1.8(10) . . . . ? C51 C56 C55 C54 -2.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.344 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.137 #end data_complex3 _database_code_depnum_ccdc_archive 'CCDC 745653' #TrackingRef '- CIF_ALL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C91 H80 Cl6 Cu2 N2 Ni O4 P4 S6' _chemical_formula_sum 'C91 H80 Cl6 Cu2 N2 Ni O4 P4 S6' _chemical_melting_point ? _exptl_crystal_description Block _exptl_crystal_colour Mehroon _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1980.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.144(5) _cell_length_b 13.801(5) _cell_length_c 25.209(5) _cell_angle_alpha 85.998(5) _cell_angle_beta 83.325(5) _cell_angle_gamma 81.990(5) _cell_volume 4491(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.1 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8242 _exptl_absorpt_correction_T_max 0.9159 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29778 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.1107 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.11 _reflns_number_total 21371 _reflns_number_gt 12256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1735P)^2^+2.3186P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21371 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1531 _refine_ls_R_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.3193 _refine_ls_wR_factor_gt 0.2294 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.50864(7) 0.10100(6) 0.69612(3) 0.0274(2) Uani 1 1 d . . . Cu1 Cu 0.27938(7) 0.31639(6) 0.85492(3) 0.0283(2) Uani 1 1 d . . . Cu2 Cu 0.50962(7) 0.30276(6) 0.71825(3) 0.0288(2) Uani 1 1 d . . . P4 P 0.51532(15) 0.45011(13) 0.67914(7) 0.0291(4) Uani 1 1 d . . . S5 S 0.82819(16) 0.20702(15) 0.57856(8) 0.0393(5) Uani 1 1 d . . . S6 S 0.45229(16) -0.03426(12) 0.79188(7) 0.0330(4) Uani 1 1 d . . . S4 S 0.60644(15) 0.12125(15) 0.62159(7) 0.0356(4) Uani 1 1 d . . . P3 P 0.39564(15) 0.04682(13) 0.65072(7) 0.0297(4) Uani 1 1 d . . . P1 P 0.37529(14) 0.38437(13) 0.90713(7) 0.0281(4) Uani 1 1 d . . . S2 S 0.31402(15) 0.14111(12) 0.85899(7) 0.0311(4) Uani 1 1 d . . . S1 S 0.36620(14) 0.27093(12) 0.76800(7) 0.0291(4) Uani 1 1 d . . . S3 S 0.63425(14) 0.17290(13) 0.72324(7) 0.0305(4) Uani 1 1 d . . . P2 P 0.10887(15) 0.36267(13) 0.84982(7) 0.0293(4) Uani 1 1 d . . . O3 O 0.3553(4) -0.0674(4) 0.8095(2) 0.0390(13) Uani 1 1 d . . . O1 O 0.7547(4) 0.2217(4) 0.5399(2) 0.0464(14) Uani 1 1 d . . . N2 N 0.4373(5) 0.0809(4) 0.7679(2) 0.0318(13) Uani 1 1 d . . . O2 O 0.9075(5) 0.2706(4) 0.5759(3) 0.0521(16) Uani 1 1 d . . . C3 C 0.3701(5) 0.5176(5) 0.8981(3) 0.0300(15) Uani 1 1 d . . . C13 C 0.3320(5) 0.3671(4) 0.9788(3) 0.0254(14) Uani 1 1 d . . . N1 N 0.7733(5) 0.2118(5) 0.6413(3) 0.0360(14) Uani 1 1 d . . . C18 C 0.2258(6) 0.3718(5) 0.9938(3) 0.0326(16) Uani 1 1 d . . . H18 H 0.1805 0.3841 0.9677 0.039 Uiso 1 1 calc R . . C83 C 0.3216(5) 0.1482(5) 0.6147(3) 0.0272(14) Uani 1 1 d . . . C44 C 0.3785(5) 0.1511(5) 0.7972(3) 0.0259(14) Uani 1 1 d . . . C16 C 0.2549(6) 0.3382(5) 1.0855(3) 0.0341(17) Uani 1 1 d . . . H16 H 0.2296 0.3280 1.1212 0.041 Uiso 1 1 calc R . . C71 C 0.2923(6) -0.0127(5) 0.6877(3) 0.0342(16) Uani 1 1 d . . . C38 C 0.4756(7) -0.0589(5) 0.8985(3) 0.0374(18) Uani 1 1 d . . . H38 H 0.4045 -0.0592 0.9044 0.045 Uiso 1 1 calc R . . C46 C 0.6334(7) 0.4863(6) 0.7576(3) 0.0413(19) Uani 1 1 d . . . H46 H 0.6462 0.4185 0.7628 0.050 Uiso 1 1 calc R . . C11 C 0.6895(6) 0.3650(6) 0.9129(3) 0.0409(18) Uani 1 1 d . . . H11 H 0.7380 0.4069 0.9157 0.049 Uiso 1 1 calc R . . C51 C 0.3882(6) 0.5184(5) 0.6685(3) 0.0331(16) Uani 1 1 d . . . C14 C 0.3987(6) 0.3475(5) 1.0177(3) 0.0310(15) Uani 1 1 d . . . H14 H 0.4696 0.3439 1.0082 0.037 Uiso 1 1 calc R . . C57 C 0.5886(6) 0.4612(5) 0.6133(3) 0.0308(15) Uani 1 1 d . . . C25 C 0.0341(6) 0.3283(5) 0.9129(3) 0.0306(15) Uani 1 1 d . . . C50 C 0.5524(6) 0.6301(6) 0.7135(3) 0.0400(18) Uani 1 1 d . . . H50 H 0.5103 0.6594 0.6880 0.048 Uiso 1 1 calc R . . C88 C 0.3491(6) 0.2419(5) 0.6147(3) 0.0308(15) Uani 1 1 d . . . H88 H 0.4076 0.2518 0.6301 0.037 Uiso 1 1 calc R . . C4 C 0.3819(6) 0.5580(5) 0.8462(3) 0.0358(17) Uani 1 1 d . . . H4 H 0.3955 0.5171 0.8177 0.043 Uiso 1 1 calc R . . C43 C 0.6305(6) -0.0435(6) 0.8376(3) 0.0425(19) Uani 1 1 d . . . H43 H 0.6628 -0.0323 0.8033 0.051 Uiso 1 1 calc R . . C2 C 0.3506(5) 0.5801(5) 0.9401(3) 0.0306(15) Uani 1 1 d . . . H2 H 0.3436 0.5539 0.9751 0.037 Uiso 1 1 calc R . . C64 C 0.8906(6) 0.0861(5) 0.5760(3) 0.0327(16) Uani 1 1 d . . . C49 C 0.5968(7) 0.6876(6) 0.7443(3) 0.044(2) Uani 1 1 d . . . H49 H 0.5836 0.7556 0.7402 0.053 Uiso 1 1 calc R . . C56 C 0.3725(6) 0.5834(6) 0.6251(3) 0.0393(18) Uani 1 1 d . . . H56 H 0.4275 0.5951 0.5999 0.047 Uiso 1 1 calc R . . C36 C 0.0955(6) 0.3036(6) 0.7482(3) 0.0358(17) Uani 1 1 d . . . H36 H 0.1609 0.3228 0.7403 0.043 Uiso 1 1 calc R . . C6 C 0.3529(6) 0.7197(6) 0.8785(3) 0.0416(19) Uani 1 1 d . . . H6 H 0.3463 0.7874 0.8725 0.050 Uiso 1 1 calc R . . C12 C 0.5863(5) 0.4027(5) 0.9092(3) 0.0319(15) Uani 1 1 d . . . H12 H 0.5664 0.4700 0.9095 0.038 Uiso 1 1 calc R . . C30 C 0.0525(6) 0.2341(5) 0.9332(3) 0.041(2) Uani 1 1 d . . . H30 H 0.1004 0.1893 0.9143 0.050 Uiso 1 1 calc R . . C76 C 0.2922(7) -0.1136(6) 0.6890(3) 0.045(2) Uani 1 1 d . . . H76 H 0.3454 -0.1534 0.6704 0.054 Uiso 1 1 calc R . . C77 C 0.4557(6) -0.0444(5) 0.6030(3) 0.0377(18) Uani 1 1 d . . . C19 C 0.0606(6) 0.4934(5) 0.8368(3) 0.0302(15) Uani 1 1 d . . . C52 C 0.3041(6) 0.5038(5) 0.7068(3) 0.0332(16) Uani 1 1 d . . . H52 H 0.3145 0.4607 0.7363 0.040 Uiso 1 1 calc R . . C37 C 0.5242(6) -0.0427(5) 0.8462(3) 0.0366(18) Uani 1 1 d . . . C65 C 0.8514(7) 0.0203(6) 0.5472(3) 0.0434(19) Uani 1 1 d . . . H65 H 0.7932 0.0400 0.5295 0.052 Uiso 1 1 calc R . . C26 C -0.0342(6) 0.3972(6) 0.9425(3) 0.0357(17) Uani 1 1 d . . . H26 H -0.0459 0.4621 0.9297 0.043 Uiso 1 1 calc R . . C63 C 0.6896(6) 0.1758(6) 0.6560(3) 0.0322(16) Uani 1 1 d . . . C1 C 0.3418(6) 0.6784(5) 0.9307(3) 0.0352(17) Uani 1 1 d . . . H1 H 0.3281 0.7190 0.9593 0.042 Uiso 1 1 calc R . . C31 C 0.0482(6) 0.3064(5) 0.8000(3) 0.0338(16) Uani 1 1 d . . . C62 C 0.5674(6) 0.4057(6) 0.5729(3) 0.0428(19) Uani 1 1 d . . . H62 H 0.5183 0.3627 0.5802 0.051 Uiso 1 1 calc R . . C45 C 0.5700(6) 0.5279(5) 0.7200(3) 0.0321(16) Uani 1 1 d . . . C58 C 0.6626(7) 0.5246(7) 0.6014(3) 0.054(2) Uani 1 1 d . . . H58 H 0.6776 0.5634 0.6275 0.065 Uiso 1 1 calc R . . C7 C 0.5134(6) 0.3415(5) 0.9053(3) 0.0352(17) Uani 1 1 d . . . C72 C 0.2125(7) 0.0439(6) 0.7165(3) 0.0438(19) Uani 1 1 d . . . H72 H 0.2139 0.1111 0.7164 0.053 Uiso 1 1 calc R . . C27 C -0.0836(6) 0.3673(6) 0.9909(3) 0.0409(19) Uani 1 1 d . . . H27 H -0.1289 0.4127 1.0106 0.049 Uiso 1 1 calc R . . C15 C 0.3607(6) 0.3331(5) 1.0708(3) 0.0363(17) Uani 1 1 d . . . H15 H 0.4062 0.3199 1.0968 0.044 Uiso 1 1 calc R . . C5 C 0.3737(6) 0.6600(5) 0.8361(3) 0.0362(17) Uani 1 1 d . . . H5 H 0.3822 0.6868 0.8012 0.043 Uiso 1 1 calc R . . C28 C -0.0671(6) 0.2715(6) 1.0105(3) 0.0418(19) Uani 1 1 d . . . H28 H -0.1014 0.2521 1.0430 0.050 Uiso 1 1 calc R . . C32 C -0.0461(7) 0.2722(7) 0.8127(4) 0.058(3) Uani 1 1 d . . . H32 H -0.0764 0.2700 0.8479 0.069 Uiso 1 1 calc R . . C87 C 0.2899(6) 0.3190(6) 0.5922(3) 0.0408(18) Uani 1 1 d . . . H87 H 0.3076 0.3817 0.5934 0.049 Uiso 1 1 calc R . . C73 C 0.1317(7) 0.0049(7) 0.7452(3) 0.049(2) Uani 1 1 d . . . H73 H 0.0783 0.0447 0.7637 0.059 Uiso 1 1 calc R . . C86 C 0.2042(6) 0.3073(5) 0.5674(3) 0.0363(17) Uani 1 1 d . . . H86 H 0.1667 0.3607 0.5508 0.044 Uiso 1 1 calc R . . C39 C 0.5354(7) -0.0742(5) 0.9409(3) 0.042(2) Uani 1 1 d . . . H39 H 0.5033 -0.0833 0.9754 0.051 Uiso 1 1 calc R . . C23 C -0.0541(7) 0.6237(6) 0.7992(3) 0.0429(19) Uani 1 1 d . . . H23 H -0.1100 0.6449 0.7800 0.052 Uiso 1 1 calc R . . C84 C 0.2340(6) 0.1363(5) 0.5909(3) 0.0350(16) Uani 1 1 d . . . H84 H 0.2149 0.0740 0.5907 0.042 Uiso 1 1 calc R . . C60 C 0.6924(7) 0.4729(6) 0.5112(3) 0.044(2) Uani 1 1 d . . . H60 H 0.7289 0.4756 0.4774 0.053 Uiso 1 1 calc R . . C78 C 0.5413(7) -0.1080(6) 0.6169(3) 0.046(2) Uani 1 1 d . . . H78 H 0.5699 -0.1000 0.6481 0.055 Uiso 1 1 calc R . . C8 C 0.5452(6) 0.2403(6) 0.9024(4) 0.0423(19) Uani 1 1 d . . . H8 H 0.4979 0.1982 0.8977 0.051 Uiso 1 1 calc R . . C59 C 0.7132(8) 0.5290(8) 0.5508(3) 0.063(3) Uani 1 1 d . . . H59 H 0.7630 0.5711 0.5430 0.076 Uiso 1 1 calc R . . C22 C -0.0032(7) 0.6911(6) 0.8191(3) 0.045(2) Uani 1 1 d . . . H22 H -0.0248 0.7576 0.8129 0.054 Uiso 1 1 calc R . . C67 C 0.9893(8) -0.1038(7) 0.5714(4) 0.058(3) Uani 1 1 d . . . C29 C 0.0017(7) 0.2039(6) 0.9810(3) 0.046(2) Uani 1 1 d . . . H29 H 0.0131 0.1388 0.9937 0.055 Uiso 1 1 calc R . . C79 C 0.5845(8) -0.1838(6) 0.5840(4) 0.054(2) Uani 1 1 d . . . H79 H 0.6410 -0.2269 0.5937 0.064 Uiso 1 1 calc R . . C54 C 0.1906(7) 0.6155(6) 0.6570(3) 0.045(2) Uani 1 1 d . . . H54 H 0.1249 0.6475 0.6524 0.054 Uiso 1 1 calc R . . C17 C 0.1873(6) 0.3587(5) 1.0465(3) 0.0338(16) Uani 1 1 d . . . H17 H 0.1163 0.3635 1.0560 0.041 Uiso 1 1 calc R . . C10 C 0.7196(7) 0.2637(6) 0.9123(4) 0.048(2) Uani 1 1 d . . . H10 H 0.7878 0.2375 0.9158 0.058 Uiso 1 1 calc R . . C69 C 1.0239(7) -0.0374(7) 0.6007(4) 0.052(2) Uani 1 1 d . . . H69 H 1.0809 -0.0573 0.6193 0.062 Uiso 1 1 calc R . . C48 C 0.6610(7) 0.6441(7) 0.7813(3) 0.048(2) Uani 1 1 d . . . H48 H 0.6919 0.6832 0.8016 0.057 Uiso 1 1 calc R . . C40 C 0.6416(7) -0.0763(5) 0.9330(3) 0.0397(18) Uani 1 1 d . . . C41 C 0.7087(8) -0.0973(6) 0.9785(4) 0.053(2) Uani 1 1 d . . . H41A H 0.6659 -0.1060 1.0116 0.079 Uiso 1 1 calc R . . H41B H 0.7467 -0.0433 0.9805 0.079 Uiso 1 1 calc R . . H41C H 0.7562 -0.1559 0.9723 0.079 Uiso 1 1 calc R . . C9 C 0.6477(7) 0.2039(7) 0.9066(4) 0.055(2) Uani 1 1 d . . . H9 H 0.6681 0.1368 0.9055 0.066 Uiso 1 1 calc R . . C74 C 0.1314(8) -0.0937(8) 0.7461(4) 0.059(3) Uani 1 1 d . . . H74 H 0.0769 -0.1213 0.7655 0.071 Uiso 1 1 calc R . . C20 C 0.1126(6) 0.5621(5) 0.8564(3) 0.0417(19) Uani 1 1 d . . . H20 H 0.1696 0.5413 0.8750 0.050 Uiso 1 1 calc R . . C82 C 0.4177(7) -0.0548(6) 0.5551(3) 0.046(2) Uani 1 1 d . . . H82 H 0.3634 -0.0103 0.5440 0.055 Uiso 1 1 calc R . . C24 C -0.0224(6) 0.5238(6) 0.8076(3) 0.0400(18) Uani 1 1 d . . . H24 H -0.0565 0.4781 0.7938 0.048 Uiso 1 1 calc R . . C61 C 0.6179(7) 0.4136(6) 0.5226(3) 0.0413(19) Uani 1 1 d . . . H61 H 0.6008 0.3779 0.4957 0.050 Uiso 1 1 calc R . . C70 C 0.9769(6) 0.0570(6) 0.6032(3) 0.0397(18) Uani 1 1 d . . . H70 H 1.0023 0.1013 0.6228 0.048 Uiso 1 1 calc R . . C55 C 0.2757(7) 0.6302(6) 0.6196(3) 0.048(2) Uani 1 1 d . . . H55 H 0.2655 0.6732 0.5900 0.058 Uiso 1 1 calc R . . C85 C 0.1754(6) 0.2145(6) 0.5678(3) 0.0413(19) Uani 1 1 d . . . H85 H 0.1167 0.2051 0.5525 0.050 Uiso 1 1 calc R . . C53 C 0.2076(7) 0.5517(6) 0.7013(4) 0.045(2) Uani 1 1 d . . . H53 H 0.1531 0.5418 0.7273 0.054 Uiso 1 1 calc R . . C21 C 0.0798(8) 0.6614(6) 0.8482(4) 0.053(2) Uani 1 1 d . . . H21 H 0.1132 0.7075 0.8621 0.063 Uiso 1 1 calc R . . C47 C 0.6791(7) 0.5474(7) 0.7885(3) 0.049(2) Uani 1 1 d . . . H47 H 0.7220 0.5195 0.8139 0.059 Uiso 1 1 calc R . . C42 C 0.6882(7) -0.0613(6) 0.8814(4) 0.050(2) Uani 1 1 d . . . H42 H 0.7596 -0.0631 0.8758 0.060 Uiso 1 1 calc R . . C75 C 0.2103(9) -0.1536(7) 0.7188(4) 0.062(3) Uani 1 1 d . . . H75 H 0.2088 -0.2209 0.7202 0.074 Uiso 1 1 calc R . . C80 C 0.5436(8) -0.1946(6) 0.5377(3) 0.054(3) Uani 1 1 d . . . H80 H 0.5725 -0.2451 0.5158 0.065 Uiso 1 1 calc R . . C81 C 0.4608(8) -0.1318(7) 0.5234(4) 0.059(3) Uani 1 1 d . . . H81 H 0.4327 -0.1404 0.4922 0.071 Uiso 1 1 calc R . . C66 C 0.8995(9) -0.0739(7) 0.5453(4) 0.059(3) Uani 1 1 d . . . H66 H 0.8731 -0.1188 0.5266 0.070 Uiso 1 1 calc R . . C35 C 0.0473(7) 0.2728(7) 0.7082(4) 0.050(2) Uani 1 1 d . . . H35 H 0.0795 0.2722 0.6734 0.060 Uiso 1 1 calc R . . C34 C -0.0488(8) 0.2428(7) 0.7198(4) 0.060(3) Uani 1 1 d . . . H34 H -0.0825 0.2238 0.6926 0.072 Uiso 1 1 calc R . . C33 C -0.0954(9) 0.2407(9) 0.7718(4) 0.073(3) Uani 1 1 d . . . H33 H -0.1594 0.2185 0.7797 0.088 Uiso 1 1 calc R . . C68 C 1.0379(11) -0.2107(8) 0.5690(5) 0.095(5) Uani 1 1 d . . . H68A H 1.0017 -0.2441 0.5465 0.143 Uiso 1 1 calc R . . H68B H 1.0334 -0.2416 0.6044 0.143 Uiso 1 1 calc R . . H68C H 1.1091 -0.2137 0.5547 0.143 Uiso 1 1 calc R . . O4 O 0.5187(5) -0.0821(3) 0.74885(19) 0.0412(14) Uani 1 1 d . . . Cl3 Cl 1.0023(4) -0.4669(3) 0.56395(17) 0.1110(13) Uani 1 1 d . . . Cl4 Cl 0.8942(3) -0.4519(4) 0.66942(16) 0.1214(15) Uani 1 1 d . . . C90 C 0.9595(16) -0.5258(12) 0.6203(7) 0.138(7) Uani 1 1 d . . . H90A H 1.0181 -0.5650 0.6348 0.165 Uiso 1 1 calc R . . H90B H 0.9139 -0.5705 0.6116 0.165 Uiso 1 1 calc R . . Cl1 Cl -0.1753(2) 0.05006(18) 1.05887(9) 0.0598(6) Uani 1 1 d . . . Cl2 Cl -0.0007(2) 0.0369(2) 1.12011(12) 0.0777(8) Uani 1 1 d . . . C89 C -0.1353(8) 0.0407(8) 1.1239(4) 0.064(3) Uani 1 1 d . . . H89A H -0.1687 0.0965 1.1436 0.077 Uiso 1 1 calc R . . H89B H -0.1557 -0.0183 1.1430 0.077 Uiso 1 1 calc R . . Cl6 Cl -0.1371(3) -0.0345(3) 0.74068(16) 0.1079(13) Uani 1 1 d . . . Cl5 Cl -0.1831(3) -0.1987(3) 0.68458(18) 0.1121(13) Uani 1 1 d . . . C91 C -0.2127(8) -0.0815(9) 0.6930(4) 0.078(4) Uani 1 1 d . . . H91A H -0.2855 -0.0682 0.7056 0.093 Uiso 1 1 calc R . . H91B H -0.2017 -0.0461 0.6586 0.093 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 0.0348(5) 0.0282(4) 0.0187(4) -0.0021(3) 0.0017(4) -0.0062(4) Cu1 0.0333(5) 0.0275(4) 0.0247(4) -0.0059(3) 0.0042(3) -0.0095(3) Cu2 0.0358(5) 0.0264(4) 0.0238(4) -0.0004(3) 0.0036(4) -0.0087(3) P4 0.0335(10) 0.0291(9) 0.0241(9) 0.0016(7) 0.0025(7) -0.0078(7) S5 0.0368(11) 0.0438(10) 0.0343(10) 0.0024(8) 0.0059(8) -0.0057(8) S6 0.0545(12) 0.0231(8) 0.0208(8) -0.0004(6) 0.0003(8) -0.0066(7) S4 0.0337(10) 0.0520(11) 0.0207(8) -0.0042(8) 0.0020(7) -0.0075(8) P3 0.0385(11) 0.0277(8) 0.0236(9) -0.0029(7) 0.0004(8) -0.0087(7) P1 0.0327(10) 0.0270(8) 0.0252(9) -0.0029(7) 0.0014(7) -0.0096(7) S2 0.0446(11) 0.0291(8) 0.0199(8) -0.0009(7) 0.0062(7) -0.0136(7) S1 0.0359(10) 0.0263(8) 0.0237(8) -0.0007(7) 0.0051(7) -0.0071(7) S3 0.0377(10) 0.0324(9) 0.0213(8) -0.0039(7) 0.0017(7) -0.0078(7) P2 0.0323(10) 0.0311(9) 0.0254(9) -0.0056(7) 0.0048(7) -0.0113(7) O3 0.058(4) 0.035(3) 0.028(3) 0.002(2) -0.007(2) -0.017(2) O1 0.038(3) 0.064(4) 0.030(3) 0.010(3) 0.003(2) 0.006(3) N2 0.040(4) 0.033(3) 0.020(3) 0.001(2) 0.007(2) -0.006(3) O2 0.049(4) 0.049(3) 0.057(4) -0.009(3) 0.021(3) -0.020(3) C3 0.029(4) 0.031(3) 0.028(4) 0.002(3) 0.006(3) -0.008(3) C13 0.031(4) 0.019(3) 0.026(3) -0.001(3) 0.001(3) -0.007(3) N1 0.033(3) 0.040(3) 0.034(3) -0.006(3) 0.004(3) -0.007(3) C18 0.036(4) 0.037(4) 0.025(4) -0.003(3) 0.002(3) -0.009(3) C83 0.032(4) 0.030(3) 0.021(3) -0.004(3) 0.001(3) -0.010(3) C44 0.037(4) 0.024(3) 0.020(3) 0.000(3) -0.004(3) -0.015(3) C16 0.043(4) 0.027(3) 0.032(4) -0.002(3) 0.008(3) -0.013(3) C71 0.049(5) 0.033(4) 0.021(3) -0.004(3) -0.006(3) -0.007(3) C38 0.052(5) 0.033(4) 0.032(4) 0.000(3) -0.005(3) -0.021(3) C46 0.053(5) 0.037(4) 0.032(4) 0.007(3) -0.006(4) -0.002(4) C11 0.038(4) 0.054(5) 0.032(4) 0.001(4) 0.000(3) -0.014(4) C51 0.042(4) 0.035(4) 0.023(3) -0.002(3) 0.006(3) -0.016(3) C14 0.029(4) 0.034(4) 0.032(4) -0.004(3) 0.005(3) -0.015(3) C57 0.040(4) 0.030(3) 0.022(3) 0.001(3) -0.001(3) -0.006(3) C25 0.040(4) 0.039(4) 0.016(3) -0.002(3) 0.003(3) -0.020(3) C50 0.045(5) 0.040(4) 0.036(4) -0.005(3) -0.004(3) -0.003(3) C88 0.037(4) 0.034(4) 0.022(3) -0.001(3) -0.003(3) -0.007(3) C4 0.043(4) 0.041(4) 0.023(4) -0.004(3) 0.007(3) -0.011(3) C43 0.043(5) 0.049(5) 0.031(4) 0.006(4) 0.004(3) -0.001(4) C2 0.029(4) 0.036(4) 0.026(4) -0.001(3) 0.001(3) -0.008(3) C64 0.034(4) 0.040(4) 0.022(3) 0.001(3) 0.005(3) -0.008(3) C49 0.059(5) 0.033(4) 0.042(5) -0.016(3) 0.001(4) -0.011(4) C56 0.046(5) 0.040(4) 0.027(4) 0.004(3) 0.002(3) 0.000(3) C36 0.030(4) 0.051(4) 0.026(4) -0.005(3) 0.002(3) -0.006(3) C6 0.035(4) 0.041(4) 0.047(5) 0.003(4) 0.000(4) -0.005(3) C12 0.029(4) 0.039(4) 0.027(4) 0.000(3) 0.004(3) -0.007(3) C30 0.033(4) 0.034(4) 0.053(5) 0.003(4) 0.016(4) -0.014(3) C76 0.078(6) 0.033(4) 0.033(4) 0.006(3) -0.010(4) -0.042(4) C77 0.053(5) 0.027(3) 0.030(4) -0.006(3) 0.007(3) 0.001(3) C19 0.036(4) 0.028(3) 0.024(3) -0.001(3) 0.009(3) -0.004(3) C52 0.039(4) 0.027(3) 0.031(4) 0.010(3) 0.004(3) -0.006(3) C37 0.055(5) 0.020(3) 0.033(4) 0.002(3) 0.001(4) -0.007(3) C65 0.052(5) 0.053(5) 0.024(4) 0.003(3) 0.001(3) -0.007(4) C26 0.030(4) 0.048(4) 0.029(4) -0.006(3) 0.004(3) -0.010(3) C63 0.029(4) 0.044(4) 0.024(3) -0.006(3) 0.000(3) -0.006(3) C1 0.034(4) 0.033(4) 0.041(4) -0.011(3) 0.002(3) -0.013(3) C31 0.030(4) 0.036(4) 0.037(4) -0.009(3) 0.003(3) -0.014(3) C62 0.043(5) 0.047(5) 0.041(5) -0.010(4) 0.004(4) -0.020(4) C45 0.032(4) 0.039(4) 0.025(4) -0.006(3) 0.002(3) -0.005(3) C58 0.057(6) 0.078(6) 0.033(4) -0.013(4) 0.016(4) -0.038(5) C7 0.035(4) 0.037(4) 0.033(4) -0.006(3) 0.002(3) -0.003(3) C72 0.051(5) 0.038(4) 0.041(5) 0.010(4) -0.003(4) -0.008(4) C27 0.032(4) 0.046(4) 0.041(5) -0.009(4) 0.010(3) -0.002(3) C15 0.043(5) 0.037(4) 0.030(4) 0.003(3) -0.001(3) -0.012(3) C5 0.048(5) 0.032(4) 0.029(4) 0.006(3) 0.003(3) -0.018(3) C28 0.047(5) 0.039(4) 0.039(4) 0.006(3) 0.005(4) -0.017(4) C32 0.054(6) 0.077(7) 0.047(5) -0.008(5) 0.002(4) -0.031(5) C87 0.047(5) 0.038(4) 0.039(4) 0.009(3) -0.007(4) -0.014(3) C73 0.043(5) 0.066(6) 0.039(5) 0.016(4) 0.001(4) -0.027(4) C86 0.036(4) 0.037(4) 0.034(4) -0.004(3) -0.003(3) 0.002(3) C39 0.062(6) 0.033(4) 0.030(4) 0.000(3) 0.008(4) -0.012(4) C23 0.045(5) 0.046(5) 0.037(4) 0.005(4) -0.001(4) -0.006(4) C84 0.044(4) 0.033(4) 0.030(4) -0.003(3) -0.002(3) -0.011(3) C60 0.055(5) 0.051(5) 0.022(4) 0.010(3) 0.010(3) -0.007(4) C78 0.061(6) 0.044(4) 0.032(4) -0.013(4) -0.003(4) 0.004(4) C8 0.030(4) 0.034(4) 0.062(6) -0.007(4) 0.004(4) -0.005(3) C59 0.083(7) 0.082(7) 0.033(5) -0.003(5) 0.022(5) -0.059(6) C22 0.054(5) 0.036(4) 0.039(5) 0.003(3) 0.014(4) -0.005(4) C67 0.069(7) 0.048(5) 0.042(5) 0.009(4) 0.026(5) 0.014(5) C29 0.058(6) 0.034(4) 0.041(5) 0.011(4) 0.006(4) -0.009(4) C79 0.069(6) 0.043(5) 0.045(5) -0.005(4) -0.006(5) 0.010(4) C54 0.043(5) 0.050(5) 0.040(5) 0.000(4) -0.003(4) -0.001(4) C17 0.034(4) 0.031(4) 0.038(4) -0.006(3) -0.001(3) -0.011(3) C10 0.036(5) 0.055(5) 0.049(5) -0.001(4) 0.001(4) 0.002(4) C69 0.038(5) 0.070(6) 0.041(5) 0.016(5) 0.009(4) -0.008(4) C48 0.063(6) 0.059(5) 0.027(4) -0.012(4) -0.003(4) -0.025(4) C40 0.058(5) 0.028(4) 0.034(4) -0.002(3) -0.010(4) -0.001(3) C41 0.076(7) 0.038(4) 0.045(5) -0.002(4) -0.024(5) 0.001(4) C9 0.044(5) 0.044(5) 0.075(7) -0.013(5) -0.001(5) 0.001(4) C74 0.072(7) 0.071(6) 0.037(5) 0.022(5) -0.009(5) -0.033(5) C20 0.043(5) 0.034(4) 0.050(5) -0.006(4) -0.002(4) -0.012(3) C82 0.065(6) 0.057(5) 0.013(3) -0.014(3) -0.005(3) 0.008(4) C24 0.044(5) 0.043(4) 0.031(4) -0.011(3) 0.005(3) -0.003(4) C61 0.051(5) 0.051(5) 0.022(4) -0.006(3) 0.000(3) -0.009(4) C70 0.028(4) 0.057(5) 0.033(4) 0.008(4) 0.001(3) -0.009(3) C55 0.056(6) 0.051(5) 0.032(4) -0.002(4) 0.003(4) 0.003(4) C85 0.035(4) 0.064(5) 0.027(4) -0.007(4) -0.003(3) -0.013(4) C53 0.044(5) 0.041(4) 0.049(5) -0.010(4) 0.013(4) -0.012(4) C21 0.063(6) 0.038(4) 0.058(6) 0.000(4) -0.001(5) -0.019(4) C47 0.061(6) 0.055(5) 0.036(5) 0.006(4) -0.012(4) -0.026(4) C42 0.038(5) 0.051(5) 0.056(6) 0.004(4) -0.001(4) 0.000(4) C75 0.102(9) 0.057(6) 0.036(5) 0.015(4) -0.019(5) -0.043(6) C80 0.092(8) 0.041(4) 0.029(4) -0.016(4) -0.004(4) 0.000(5) C81 0.086(8) 0.059(6) 0.035(5) -0.018(4) -0.023(5) 0.008(5) C66 0.087(8) 0.047(5) 0.041(5) -0.010(4) 0.002(5) -0.010(5) C35 0.047(5) 0.061(5) 0.043(5) -0.024(4) -0.003(4) -0.002(4) C34 0.060(6) 0.069(6) 0.059(6) -0.022(5) -0.013(5) -0.018(5) C33 0.068(7) 0.106(9) 0.060(7) -0.031(6) -0.003(5) -0.048(6) C68 0.120(11) 0.059(7) 0.080(9) 0.016(6) 0.042(8) 0.032(7) O4 0.076(4) 0.020(2) 0.023(3) -0.0003(19) 0.007(3) -0.001(2) Cl3 0.133(3) 0.091(2) 0.102(3) -0.004(2) -0.010(2) 0.005(2) Cl4 0.110(3) 0.165(4) 0.091(3) -0.049(3) -0.012(2) -0.003(3) C90 0.19(2) 0.096(12) 0.115(14) -0.009(10) 0.001(13) 0.005(12) Cl1 0.0702(16) 0.0682(15) 0.0458(13) -0.0070(11) 0.0058(11) -0.0336(12) Cl2 0.0580(16) 0.109(2) 0.0661(18) 0.0073(16) 0.0040(13) -0.0269(15) C89 0.066(7) 0.067(6) 0.067(7) -0.025(5) 0.003(5) -0.032(5) Cl6 0.065(2) 0.161(4) 0.093(3) 0.006(2) -0.0055(18) -0.007(2) Cl5 0.117(3) 0.090(2) 0.121(3) 0.015(2) 0.011(2) -0.016(2) C91 0.057(7) 0.103(9) 0.060(7) 0.023(6) 0.006(5) 0.013(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 Ni1 N2 1.959(5) . ? Ni1 S4 2.174(2) . ? Ni1 P3 2.213(2) . ? Ni1 S3 2.234(2) . ? Ni1 Cu2 2.8798(15) . ? Cu1 P1 2.256(2) . ? Cu1 P2 2.259(2) . ? Cu1 S2 2.396(2) . ? Cu1 S1 2.4308(19) . ? Cu2 P4 2.204(2) . ? Cu2 S1 2.219(2) . ? Cu2 S3 2.260(2) . ? P4 C45 1.809(7) . ? P4 C57 1.826(7) . ? P4 C51 1.839(8) . ? S5 O1 1.434(6) . ? S5 O2 1.446(6) . ? S5 N1 1.662(6) . ? S5 C64 1.756(8) . ? S6 O3 1.426(6) . ? S6 O4 1.447(5) . ? S6 N2 1.654(6) . ? S6 C37 1.742(9) . ? S4 C63 1.748(8) . ? P3 C71 1.816(8) . ? P3 C77 1.836(7) . ? P3 C83 1.838(7) . ? P1 C7 1.825(8) . ? P1 C3 1.830(7) . ? P1 C13 1.840(7) . ? S2 C44 1.691(7) . ? S1 C44 1.757(7) . ? S3 C63 1.765(7) . ? P2 C31 1.833(8) . ? P2 C25 1.839(7) . ? P2 C19 1.848(7) . ? N2 C44 1.356(9) . ? C3 C4 1.386(10) . ? C3 C2 1.391(10) . ? C13 C14 1.378(10) . ? C13 C18 1.397(10) . ? N1 C63 1.275(9) . ? C18 C17 1.375(10) . ? C18 H18 0.9300 . ? C83 C88 1.391(9) . ? C83 C84 1.391(10) . ? C16 C17 1.390(11) . ? C16 C15 1.390(10) . ? C16 H16 0.9300 . ? C71 C72 1.384(11) . ? C71 C76 1.390(10) . ? C38 C39 1.386(12) . ? C38 C37 1.413(10) . ? C38 H38 0.9300 . ? C46 C45 1.377(11) . ? C46 C47 1.422(12) . ? C46 H46 0.9300 . ? C11 C12 1.395(11) . ? C11 C10 1.399(12) . ? C11 H11 0.9300 . ? C51 C56 1.382(10) . ? C51 C52 1.407(9) . ? C14 C15 1.385(10) . ? C14 H14 0.9300 . ? C57 C58 1.391(10) . ? C57 C62 1.393(10) . ? C25 C30 1.364(10) . ? C25 C26 1.404(10) . ? C50 C49 1.377(11) . ? C50 C45 1.398(10) . ? C50 H50 0.9300 . ? C88 C87 1.360(10) . ? C88 H88 0.9300 . ? C4 C5 1.404(10) . ? C4 H4 0.9300 . ? C43 C37 1.387(11) . ? C43 C42 1.401(12) . ? C43 H43 0.9300 . ? C2 C1 1.351(10) . ? C2 H2 0.9300 . ? C64 C65 1.389(11) . ? C64 C70 1.390(11) . ? C49 C48 1.382(12) . ? C49 H49 0.9300 . ? C56 C55 1.362(12) . ? C56 H56 0.9300 . ? C36 C35 1.370(11) . ? C36 C31 1.379(10) . ? C36 H36 0.9300 . ? C6 C5 1.375(11) . ? C6 C1 1.396(11) . ? C6 H6 0.9300 . ? C12 C7 1.380(10) . ? C12 H12 0.9300 . ? C30 C29 1.377(10) . ? C30 H30 0.9300 . ? C76 C75 1.396(12) . ? C76 H76 0.9300 . ? C77 C82 1.384(11) . ? C77 C78 1.390(12) . ? C19 C24 1.388(11) . ? C19 C20 1.390(10) . ? C52 C53 1.363(11) . ? C52 H52 0.9300 . ? C65 C66 1.365(12) . ? C65 H65 0.9300 . ? C26 C27 1.378(10) . ? C26 H26 0.9300 . ? C1 H1 0.9300 . ? C31 C32 1.383(11) . ? C62 C61 1.366(10) . ? C62 H62 0.9300 . ? C58 C59 1.370(11) . ? C58 H58 0.9300 . ? C7 C8 1.405(10) . ? C72 C73 1.367(11) . ? C72 H72 0.9300 . ? C27 C28 1.376(11) . ? C27 H27 0.9300 . ? C15 H15 0.9300 . ? C5 H5 0.9300 . ? C28 C29 1.394(11) . ? C28 H28 0.9300 . ? C32 C33 1.403(13) . ? C32 H32 0.9300 . ? C87 C86 1.383(11) . ? C87 H87 0.9300 . ? C73 C74 1.360(13) . ? C73 H73 0.9300 . ? C86 C85 1.385(11) . ? C86 H86 0.9300 . ? C39 C40 1.384(12) . ? C39 H39 0.9300 . ? C23 C22 1.370(12) . ? C23 C24 1.392(11) . ? C23 H23 0.9300 . ? C84 C85 1.371(11) . ? C84 H84 0.9300 . ? C60 C61 1.355(11) . ? C60 C59 1.379(12) . ? C60 H60 0.9300 . ? C78 C79 1.396(11) . ? C78 H78 0.9300 . ? C8 C9 1.384(12) . ? C8 H8 0.9300 . ? C59 H59 0.9300 . ? C22 C21 1.385(13) . ? C22 H22 0.9300 . ? C67 C69 1.370(14) . ? C67 C66 1.415(15) . ? C67 C68 1.526(13) . ? C29 H29 0.9300 . ? C79 C80 1.367(13) . ? C79 H79 0.9300 . ? C54 C53 1.392(12) . ? C54 C55 1.405(12) . ? C54 H54 0.9300 . ? C17 H17 0.9300 . ? C10 C9 1.365(13) . ? C10 H10 0.9300 . ? C69 C70 1.365(12) . ? C69 H69 0.9300 . ? C48 C47 1.326(12) . ? C48 H48 0.9300 . ? C40 C42 1.387(11) . ? C40 C41 1.515(11) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C9 H9 0.9300 . ? C74 C75 1.382(15) . ? C74 H74 0.9300 . ? C20 C21 1.387(11) . ? C20 H20 0.9300 . ? C82 C81 1.390(11) . ? C82 H82 0.9300 . ? C24 H24 0.9300 . ? C61 H61 0.9300 . ? C70 H70 0.9300 . ? C55 H55 0.9300 . ? C85 H85 0.9300 . ? C53 H53 0.9300 . ? C21 H21 0.9300 . ? C47 H47 0.9300 . ? C42 H42 0.9300 . ? C75 H75 0.9300 . ? C80 C81 1.359(13) . ? C80 H80 0.9300 . ? C81 H81 0.9300 . ? C66 H66 0.9300 . ? C35 C34 1.378(13) . ? C35 H35 0.9300 . ? C34 C33 1.380(14) . ? C34 H34 0.9300 . ? C33 H33 0.9300 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? Cl3 C90 1.665(17) . ? Cl4 C90 1.732(16) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? Cl1 C89 1.771(11) . ? Cl2 C89 1.754(11) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? Cl6 C91 1.849(13) . ? Cl5 C91 1.633(12) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 S4 172.5(2) . . ? N2 Ni1 P3 97.6(2) . . ? S4 Ni1 P3 89.17(8) . . ? N2 Ni1 S3 95.2(2) . . ? S4 Ni1 S3 78.34(8) . . ? P3 Ni1 S3 166.41(8) . . ? N2 Ni1 Cu2 88.56(18) . . ? S4 Ni1 Cu2 90.26(6) . . ? P3 Ni1 Cu2 125.12(6) . . ? S3 Ni1 Cu2 50.56(5) . . ? P1 Cu1 P2 124.51(7) . . ? P1 Cu1 S2 112.36(8) . . ? P2 Cu1 S2 109.31(7) . . ? P1 Cu1 S1 115.29(7) . . ? P2 Cu1 S1 110.44(7) . . ? S2 Cu1 S1 73.53(6) . . ? P4 Cu2 S1 119.05(8) . . ? P4 Cu2 S3 130.65(8) . . ? S1 Cu2 S3 110.08(7) . . ? P4 Cu2 Ni1 142.52(6) . . ? S1 Cu2 Ni1 79.42(5) . . ? S3 Cu2 Ni1 49.75(5) . . ? C45 P4 C57 104.5(3) . . ? C45 P4 C51 103.8(3) . . ? C57 P4 C51 102.9(3) . . ? C45 P4 Cu2 111.1(3) . . ? C57 P4 Cu2 118.5(2) . . ? C51 P4 Cu2 114.4(2) . . ? O1 S5 O2 119.5(4) . . ? O1 S5 N1 113.1(3) . . ? O2 S5 N1 104.1(3) . . ? O1 S5 C64 108.4(4) . . ? O2 S5 C64 107.4(4) . . ? N1 S5 C64 103.0(3) . . ? O3 S6 O4 119.3(3) . . ? O3 S6 N2 111.5(3) . . ? O4 S6 N2 101.6(3) . . ? O3 S6 C37 108.4(3) . . ? O4 S6 C37 106.6(4) . . ? N2 S6 C37 108.8(3) . . ? C63 S4 Ni1 89.6(2) . . ? C71 P3 C77 103.0(3) . . ? C71 P3 C83 101.1(3) . . ? C77 P3 C83 109.0(3) . . ? C71 P3 Ni1 118.4(2) . . ? C77 P3 Ni1 113.0(3) . . ? C83 P3 Ni1 111.2(2) . . ? C7 P1 C3 103.5(3) . . ? C7 P1 C13 101.7(3) . . ? C3 P1 C13 102.3(3) . . ? C7 P1 Cu1 119.3(2) . . ? C3 P1 Cu1 115.3(3) . . ? C13 P1 Cu1 112.6(2) . . ? C44 S2 Cu1 87.3(2) . . ? C44 S1 Cu2 112.1(2) . . ? C44 S1 Cu1 84.8(2) . . ? Cu2 S1 Cu1 135.85(9) . . ? C63 S3 Ni1 87.2(3) . . ? C63 S3 Cu2 99.1(3) . . ? Ni1 S3 Cu2 79.69(8) . . ? C31 P2 C25 102.6(3) . . ? C31 P2 C19 100.7(4) . . ? C25 P2 C19 104.1(3) . . ? C31 P2 Cu1 117.5(2) . . ? C25 P2 Cu1 110.2(3) . . ? C19 P2 Cu1 119.6(2) . . ? C44 N2 S6 120.1(5) . . ? C44 N2 Ni1 126.0(5) . . ? S6 N2 Ni1 113.9(3) . . ? C4 C3 C2 118.7(7) . . ? C4 C3 P1 117.7(5) . . ? C2 C3 P1 123.6(5) . . ? C14 C13 C18 119.1(6) . . ? C14 C13 P1 123.5(5) . . ? C18 C13 P1 117.4(5) . . ? C63 N1 S5 121.3(6) . . ? C17 C18 C13 121.0(7) . . ? C17 C18 H18 119.5 . . ? C13 C18 H18 119.5 . . ? C88 C83 C84 118.5(7) . . ? C88 C83 P3 118.8(5) . . ? C84 C83 P3 122.5(5) . . ? N2 C44 S2 129.5(5) . . ? N2 C44 S1 116.7(5) . . ? S2 C44 S1 113.8(4) . . ? C17 C16 C15 119.5(7) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C72 C71 C76 119.0(8) . . ? C72 C71 P3 118.9(6) . . ? C76 C71 P3 122.1(6) . . ? C39 C38 C37 119.1(8) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C45 C46 C47 119.7(8) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C12 C11 C10 119.6(8) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C56 C51 C52 119.2(7) . . ? C56 C51 P4 122.8(6) . . ? C52 C51 P4 118.0(6) . . ? C13 C14 C15 120.3(7) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C58 C57 C62 118.5(7) . . ? C58 C57 P4 122.9(6) . . ? C62 C57 P4 118.5(6) . . ? C30 C25 C26 119.6(7) . . ? C30 C25 P2 118.0(6) . . ? C26 C25 P2 122.2(6) . . ? C49 C50 C45 120.7(8) . . ? C49 C50 H50 119.7 . . ? C45 C50 H50 119.7 . . ? C87 C88 C83 119.6(7) . . ? C87 C88 H88 120.2 . . ? C83 C88 H88 120.2 . . ? C3 C4 C5 120.8(7) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C37 C43 C42 118.7(7) . . ? C37 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? C1 C2 C3 120.9(7) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C65 C64 C70 120.9(7) . . ? C65 C64 S5 118.9(6) . . ? C70 C64 S5 120.2(6) . . ? C50 C49 C48 119.7(8) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C55 C56 C51 119.4(8) . . ? C55 C56 H56 120.3 . . ? C51 C56 H56 120.3 . . ? C35 C36 C31 120.9(7) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C5 C6 C1 119.8(7) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C7 C12 C11 120.9(7) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C25 C30 C29 121.2(7) . . ? C25 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C71 C76 C75 118.5(9) . . ? C71 C76 H76 120.7 . . ? C75 C76 H76 120.7 . . ? C82 C77 C78 118.8(7) . . ? C82 C77 P3 123.1(6) . . ? C78 C77 P3 118.0(6) . . ? C24 C19 C20 120.3(7) . . ? C24 C19 P2 122.4(6) . . ? C20 C19 P2 117.3(6) . . ? C53 C52 C51 121.2(7) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C43 C37 C38 120.3(8) . . ? C43 C37 S6 119.7(6) . . ? C38 C37 S6 119.7(6) . . ? C66 C65 C64 119.1(9) . . ? C66 C65 H65 120.4 . . ? C64 C65 H65 120.4 . . ? C27 C26 C25 119.2(7) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? N1 C63 S4 133.0(6) . . ? N1 C63 S3 122.1(6) . . ? S4 C63 S3 104.8(4) . . ? C2 C1 C6 120.8(7) . . ? C2 C1 H1 119.6 . . ? C6 C1 H1 119.6 . . ? C36 C31 C32 119.9(7) . . ? C36 C31 P2 118.8(5) . . ? C32 C31 P2 121.2(6) . . ? C61 C62 C57 120.7(7) . . ? C61 C62 H62 119.6 . . ? C57 C62 H62 119.6 . . ? C46 C45 C50 118.5(7) . . ? C46 C45 P4 119.7(6) . . ? C50 C45 P4 121.8(6) . . ? C59 C58 C57 119.1(8) . . ? C59 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C12 C7 C8 119.0(7) . . ? C12 C7 P1 123.2(6) . . ? C8 C7 P1 117.7(6) . . ? C73 C72 C71 122.5(8) . . ? C73 C72 H72 118.7 . . ? C71 C72 H72 118.7 . . ? C28 C27 C26 121.1(7) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C14 C15 C16 120.4(7) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C6 C5 C4 119.0(7) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C27 C28 C29 119.2(7) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C31 C32 C33 119.1(9) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C88 C87 C86 122.2(7) . . ? C88 C87 H87 118.9 . . ? C86 C87 H87 118.9 . . ? C74 C73 C72 118.4(9) . . ? C74 C73 H73 120.8 . . ? C72 C73 H73 120.8 . . ? C87 C86 C85 118.6(7) . . ? C87 C86 H86 120.7 . . ? C85 C86 H86 120.7 . . ? C40 C39 C38 121.6(7) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C22 C23 C24 120.4(8) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C85 C84 C83 121.5(7) . . ? C85 C84 H84 119.2 . . ? C83 C84 H84 119.2 . . ? C61 C60 C59 118.7(7) . . ? C61 C60 H60 120.6 . . ? C59 C60 H60 120.6 . . ? C77 C78 C79 120.1(8) . . ? C77 C78 H78 119.9 . . ? C79 C78 H78 119.9 . . ? C9 C8 C7 119.3(8) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C58 C59 C60 121.9(8) . . ? C58 C59 H59 119.0 . . ? C60 C59 H59 119.0 . . ? C23 C22 C21 120.9(8) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C69 C67 C66 118.5(8) . . ? C69 C67 C68 123.2(11) . . ? C66 C67 C68 118.1(11) . . ? C30 C29 C28 119.7(7) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C80 C79 C78 120.0(9) . . ? C80 C79 H79 120.0 . . ? C78 C79 H79 120.0 . . ? C53 C54 C55 118.1(8) . . ? C53 C54 H54 121.0 . . ? C55 C54 H54 121.0 . . ? C18 C17 C16 119.7(7) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C9 C10 C11 119.1(8) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C70 C69 C67 121.8(9) . . ? C70 C69 H69 119.1 . . ? C67 C69 H69 119.1 . . ? C47 C48 C49 121.0(8) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C39 C40 C42 118.6(8) . . ? C39 C40 C41 122.3(8) . . ? C42 C40 C41 119.0(8) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C10 C9 C8 122.0(8) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C73 C74 C75 121.3(9) . . ? C73 C74 H74 119.3 . . ? C75 C74 H74 119.3 . . ? C21 C20 C19 120.1(8) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C77 C82 C81 120.0(8) . . ? C77 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C19 C24 C23 119.1(8) . . ? C19 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C60 C61 C62 121.0(7) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C69 C70 C64 119.0(8) . . ? C69 C70 H70 120.5 . . ? C64 C70 H70 120.5 . . ? C56 C55 C54 122.2(8) . . ? C56 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? C84 C85 C86 119.6(8) . . ? C84 C85 H85 120.2 . . ? C86 C85 H85 120.2 . . ? C52 C53 C54 120.0(8) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C22 C21 C20 119.2(8) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C48 C47 C46 120.4(8) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C40 C42 C43 121.7(8) . . ? C40 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? C74 C75 C76 120.3(9) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C81 C80 C79 120.2(8) . . ? C81 C80 H80 119.9 . . ? C79 C80 H80 119.9 . . ? C80 C81 C82 120.7(8) . . ? C80 C81 H81 119.6 . . ? C82 C81 H81 119.6 . . ? C65 C66 C67 120.6(9) . . ? C65 C66 H66 119.7 . . ? C67 C66 H66 119.7 . . ? C36 C35 C34 119.8(8) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C34 C33 120.2(9) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C33 C32 119.8(9) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? Cl3 C90 Cl4 115.4(9) . . ? Cl3 C90 H90A 108.4 . . ? Cl4 C90 H90A 108.4 . . ? Cl3 C90 H90B 108.4 . . ? Cl4 C90 H90B 108.4 . . ? H90A C90 H90B 107.5 . . ? Cl2 C89 Cl1 110.1(6) . . ? Cl2 C89 H89A 109.6 . . ? Cl1 C89 H89A 109.6 . . ? Cl2 C89 H89B 109.6 . . ? Cl1 C89 H89B 109.6 . . ? H89A C89 H89B 108.1 . . ? Cl5 C91 Cl6 113.9(6) . . ? Cl5 C91 H91A 108.8 . . ? Cl6 C91 H91A 108.8 . . ? Cl5 C91 H91B 108.8 . . ? Cl6 C91 H91B 108.8 . . ? H91A C91 H91B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 Cu2 P4 -154.7(2) . . . . ? S4 Ni1 Cu2 P4 32.77(12) . . . . ? P3 Ni1 Cu2 P4 -56.40(13) . . . . ? S3 Ni1 Cu2 P4 107.38(12) . . . . ? N2 Ni1 Cu2 S1 -30.1(2) . . . . ? S4 Ni1 Cu2 S1 157.39(8) . . . . ? P3 Ni1 Cu2 S1 68.22(9) . . . . ? S3 Ni1 Cu2 S1 -128.00(8) . . . . ? N2 Ni1 Cu2 S3 97.9(2) . . . . ? S4 Ni1 Cu2 S3 -74.61(8) . . . . ? P3 Ni1 Cu2 S3 -163.78(9) . . . . ? S1 Cu2 P4 C45 93.8(3) . . . . ? S3 Cu2 P4 C45 -80.2(3) . . . . ? Ni1 Cu2 P4 C45 -153.9(2) . . . . ? S1 Cu2 P4 C57 -145.1(3) . . . . ? S3 Cu2 P4 C57 40.9(3) . . . . ? Ni1 Cu2 P4 C57 -32.9(3) . . . . ? S1 Cu2 P4 C51 -23.4(3) . . . . ? S3 Cu2 P4 C51 162.6(3) . . . . ? Ni1 Cu2 P4 C51 88.9(3) . . . . ? N2 Ni1 S4 C63 -31.8(14) . . . . ? P3 Ni1 S4 C63 174.3(3) . . . . ? S3 Ni1 S4 C63 -0.3(3) . . . . ? Cu2 Ni1 S4 C63 49.2(3) . . . . ? N2 Ni1 P3 C71 -9.0(3) . . . . ? S4 Ni1 P3 C71 167.7(3) . . . . ? S3 Ni1 P3 C71 -169.2(4) . . . . ? Cu2 Ni1 P3 C71 -102.6(3) . . . . ? N2 Ni1 P3 C77 -129.5(3) . . . . ? S4 Ni1 P3 C77 47.2(3) . . . . ? S3 Ni1 P3 C77 70.3(4) . . . . ? Cu2 Ni1 P3 C77 136.9(3) . . . . ? N2 Ni1 P3 C83 107.5(3) . . . . ? S4 Ni1 P3 C83 -75.8(2) . . . . ? S3 Ni1 P3 C83 -52.7(4) . . . . ? Cu2 Ni1 P3 C83 13.9(2) . . . . ? P2 Cu1 P1 C7 -178.1(3) . . . . ? S2 Cu1 P1 C7 46.1(3) . . . . ? S1 Cu1 P1 C7 -35.5(3) . . . . ? P2 Cu1 P1 C3 -54.0(3) . . . . ? S2 Cu1 P1 C3 170.2(2) . . . . ? S1 Cu1 P1 C3 88.5(2) . . . . ? P2 Cu1 P1 C13 62.9(2) . . . . ? S2 Cu1 P1 C13 -72.9(2) . . . . ? S1 Cu1 P1 C13 -154.6(2) . . . . ? P1 Cu1 S2 C44 -106.1(2) . . . . ? P2 Cu1 S2 C44 111.4(2) . . . . ? S1 Cu1 S2 C44 5.1(2) . . . . ? P4 Cu2 S1 C44 -178.2(2) . . . . ? S3 Cu2 S1 C44 -3.1(3) . . . . ? Ni1 Cu2 S1 C44 36.7(2) . . . . ? P4 Cu2 S1 Cu1 -72.20(15) . . . . ? S3 Cu2 S1 Cu1 102.93(12) . . . . ? Ni1 Cu2 S1 Cu1 142.75(12) . . . . ? P1 Cu1 S1 C44 102.5(2) . . . . ? P2 Cu1 S1 C44 -109.8(2) . . . . ? S2 Cu1 S1 C44 -4.9(2) . . . . ? P1 Cu1 S1 Cu2 -14.01(15) . . . . ? P2 Cu1 S1 Cu2 133.64(12) . . . . ? S2 Cu1 S1 Cu2 -121.42(13) . . . . ? N2 Ni1 S3 C63 176.4(3) . . . . ? S4 Ni1 S3 C63 0.3(3) . . . . ? P3 Ni1 S3 C63 -23.3(4) . . . . ? Cu2 Ni1 S3 C63 -99.8(3) . . . . ? N2 Ni1 S3 Cu2 -83.83(18) . . . . ? S4 Ni1 S3 Cu2 100.12(7) . . . . ? P3 Ni1 S3 Cu2 76.5(3) . . . . ? P4 Cu2 S3 C63 -44.6(3) . . . . ? S1 Cu2 S3 C63 141.0(3) . . . . ? Ni1 Cu2 S3 C63 85.5(3) . . . . ? P4 Cu2 S3 Ni1 -130.05(9) . . . . ? S1 Cu2 S3 Ni1 55.56(8) . . . . ? P1 Cu1 P2 C31 174.0(3) . . . . ? S2 Cu1 P2 C31 -49.1(3) . . . . ? S1 Cu1 P2 C31 30.0(3) . . . . ? P1 Cu1 P2 C25 -69.0(3) . . . . ? S2 Cu1 P2 C25 67.9(2) . . . . ? S1 Cu1 P2 C25 147.0(2) . . . . ? P1 Cu1 P2 C19 51.5(3) . . . . ? S2 Cu1 P2 C19 -171.6(3) . . . . ? S1 Cu1 P2 C19 -92.6(3) . . . . ? O3 S6 N2 C44 52.0(7) . . . . ? O4 S6 N2 C44 -179.8(6) . . . . ? C37 S6 N2 C44 -67.6(7) . . . . ? O3 S6 N2 Ni1 -127.2(4) . . . . ? O4 S6 N2 Ni1 1.0(5) . . . . ? C37 S6 N2 Ni1 113.2(4) . . . . ? S4 Ni1 N2 C44 105.6(14) . . . . ? P3 Ni1 N2 C44 -100.8(6) . . . . ? S3 Ni1 N2 C44 74.6(6) . . . . ? Cu2 Ni1 N2 C44 24.5(6) . . . . ? S4 Ni1 N2 S6 -75.3(15) . . . . ? P3 Ni1 N2 S6 78.3(4) . . . . ? S3 Ni1 N2 S6 -106.3(3) . . . . ? Cu2 Ni1 N2 S6 -156.4(3) . . . . ? C7 P1 C3 C4 84.9(6) . . . . ? C13 P1 C3 C4 -169.7(6) . . . . ? Cu1 P1 C3 C4 -47.1(6) . . . . ? C7 P1 C3 C2 -97.8(7) . . . . ? C13 P1 C3 C2 7.5(7) . . . . ? Cu1 P1 C3 C2 130.1(6) . . . . ? C7 P1 C13 C14 12.3(6) . . . . ? C3 P1 C13 C14 -94.4(6) . . . . ? Cu1 P1 C13 C14 141.2(5) . . . . ? C7 P1 C13 C18 -166.0(5) . . . . ? C3 P1 C13 C18 87.3(5) . . . . ? Cu1 P1 C13 C18 -37.1(5) . . . . ? O1 S5 N1 C63 38.1(8) . . . . ? O2 S5 N1 C63 169.3(6) . . . . ? C64 S5 N1 C63 -78.7(7) . . . . ? C14 C13 C18 C17 1.0(10) . . . . ? P1 C13 C18 C17 179.3(5) . . . . ? C71 P3 C83 C88 133.0(6) . . . . ? C77 P3 C83 C88 -119.0(6) . . . . ? Ni1 P3 C83 C88 6.3(6) . . . . ? C71 P3 C83 C84 -41.8(6) . . . . ? C77 P3 C83 C84 66.2(7) . . . . ? Ni1 P3 C83 C84 -168.5(5) . . . . ? S6 N2 C44 S2 0.8(10) . . . . ? Ni1 N2 C44 S2 179.9(4) . . . . ? S6 N2 C44 S1 -179.4(4) . . . . ? Ni1 N2 C44 S1 -0.3(8) . . . . ? Cu1 S2 C44 N2 172.5(7) . . . . ? Cu1 S2 C44 S1 -7.3(3) . . . . ? Cu2 S1 C44 N2 -34.8(6) . . . . ? Cu1 S1 C44 N2 -172.6(6) . . . . ? Cu2 S1 C44 S2 145.0(3) . . . . ? Cu1 S1 C44 S2 7.3(3) . . . . ? C77 P3 C71 C72 -161.8(7) . . . . ? C83 P3 C71 C72 -49.1(7) . . . . ? Ni1 P3 C71 C72 72.7(7) . . . . ? C77 P3 C71 C76 19.8(7) . . . . ? C83 P3 C71 C76 132.5(7) . . . . ? Ni1 P3 C71 C76 -105.7(6) . . . . ? C45 P4 C51 C56 91.8(7) . . . . ? C57 P4 C51 C56 -17.0(7) . . . . ? Cu2 P4 C51 C56 -146.9(6) . . . . ? C45 P4 C51 C52 -87.6(6) . . . . ? C57 P4 C51 C52 163.6(6) . . . . ? Cu2 P4 C51 C52 33.6(6) . . . . ? C18 C13 C14 C15 -0.3(10) . . . . ? P1 C13 C14 C15 -178.5(5) . . . . ? C45 P4 C57 C58 -4.6(8) . . . . ? C51 P4 C57 C58 103.7(8) . . . . ? Cu2 P4 C57 C58 -128.9(7) . . . . ? C45 P4 C57 C62 177.3(6) . . . . ? C51 P4 C57 C62 -74.5(7) . . . . ? Cu2 P4 C57 C62 52.9(7) . . . . ? C31 P2 C25 C30 75.2(7) . . . . ? C19 P2 C25 C30 179.8(6) . . . . ? Cu1 P2 C25 C30 -50.8(7) . . . . ? C31 P2 C25 C26 -110.2(6) . . . . ? C19 P2 C25 C26 -5.5(7) . . . . ? Cu1 P2 C25 C26 123.9(6) . . . . ? C84 C83 C88 C87 0.6(10) . . . . ? P3 C83 C88 C87 -174.5(6) . . . . ? C2 C3 C4 C5 -0.5(11) . . . . ? P1 C3 C4 C5 176.8(6) . . . . ? C4 C3 C2 C1 1.0(11) . . . . ? P1 C3 C2 C1 -176.2(6) . . . . ? O1 S5 C64 C65 -11.2(7) . . . . ? O2 S5 C64 C65 -141.6(6) . . . . ? N1 S5 C64 C65 108.9(6) . . . . ? O1 S5 C64 C70 169.7(6) . . . . ? O2 S5 C64 C70 39.3(7) . . . . ? N1 S5 C64 C70 -70.2(6) . . . . ? C45 C50 C49 C48 1.3(12) . . . . ? C52 C51 C56 C55 -1.5(12) . . . . ? P4 C51 C56 C55 179.1(6) . . . . ? C10 C11 C12 C7 0.2(11) . . . . ? C26 C25 C30 C29 3.2(12) . . . . ? P2 C25 C30 C29 178.0(7) . . . . ? C72 C71 C76 C75 1.0(12) . . . . ? P3 C71 C76 C75 179.4(6) . . . . ? C71 P3 C77 C82 82.8(8) . . . . ? C83 P3 C77 C82 -24.0(8) . . . . ? Ni1 P3 C77 C82 -148.3(7) . . . . ? C71 P3 C77 C78 -95.0(7) . . . . ? C83 P3 C77 C78 158.2(6) . . . . ? Ni1 P3 C77 C78 33.9(7) . . . . ? C31 P2 C19 C24 16.2(7) . . . . ? C25 P2 C19 C24 -89.9(6) . . . . ? Cu1 P2 C19 C24 146.6(5) . . . . ? C31 P2 C19 C20 -162.2(6) . . . . ? C25 P2 C19 C20 91.7(6) . . . . ? Cu1 P2 C19 C20 -31.7(6) . . . . ? C56 C51 C52 C53 0.8(12) . . . . ? P4 C51 C52 C53 -179.8(6) . . . . ? C42 C43 C37 C38 0.6(11) . . . . ? C42 C43 C37 S6 -173.0(6) . . . . ? C39 C38 C37 C43 0.8(11) . . . . ? C39 C38 C37 S6 174.3(6) . . . . ? O3 S6 C37 C43 160.8(6) . . . . ? O4 S6 C37 C43 31.2(7) . . . . ? N2 S6 C37 C43 -77.7(6) . . . . ? O3 S6 C37 C38 -12.7(7) . . . . ? O4 S6 C37 C38 -142.4(6) . . . . ? N2 S6 C37 C38 108.7(6) . . . . ? C70 C64 C65 C66 -0.8(11) . . . . ? S5 C64 C65 C66 -179.8(6) . . . . ? C30 C25 C26 C27 -1.9(11) . . . . ? P2 C25 C26 C27 -176.6(6) . . . . ? S5 N1 C63 S4 -3.6(11) . . . . ? S5 N1 C63 S3 175.8(4) . . . . ? Ni1 S4 C63 N1 179.9(8) . . . . ? Ni1 S4 C63 S3 0.4(3) . . . . ? Ni1 S3 C63 N1 -180.0(7) . . . . ? Cu2 S3 C63 N1 100.9(7) . . . . ? Ni1 S3 C63 S4 -0.4(3) . . . . ? Cu2 S3 C63 S4 -79.5(3) . . . . ? C3 C2 C1 C6 -0.6(11) . . . . ? C5 C6 C1 C2 -0.4(12) . . . . ? C35 C36 C31 C32 4.1(13) . . . . ? C35 C36 C31 P2 -172.3(7) . . . . ? C25 P2 C31 C36 -169.6(6) . . . . ? C19 P2 C31 C36 83.2(7) . . . . ? Cu1 P2 C31 C36 -48.6(7) . . . . ? C25 P2 C31 C32 14.1(8) . . . . ? C19 P2 C31 C32 -93.2(8) . . . . ? Cu1 P2 C31 C32 135.1(7) . . . . ? C58 C57 C62 C61 -0.3(13) . . . . ? P4 C57 C62 C61 178.0(6) . . . . ? C47 C46 C45 C50 -0.1(11) . . . . ? C47 C46 C45 P4 177.9(6) . . . . ? C49 C50 C45 C46 -0.6(11) . . . . ? C49 C50 C45 P4 -178.5(6) . . . . ? C57 P4 C45 C46 -106.0(6) . . . . ? C51 P4 C45 C46 146.5(6) . . . . ? Cu2 P4 C45 C46 23.0(7) . . . . ? C57 P4 C45 C50 72.0(7) . . . . ? C51 P4 C45 C50 -35.5(7) . . . . ? Cu2 P4 C45 C50 -159.0(5) . . . . ? C62 C57 C58 C59 -1.1(14) . . . . ? P4 C57 C58 C59 -179.3(8) . . . . ? C11 C12 C7 C8 -3.0(11) . . . . ? C11 C12 C7 P1 173.6(6) . . . . ? C3 P1 C7 C12 13.6(7) . . . . ? C13 P1 C7 C12 -92.3(7) . . . . ? Cu1 P1 C7 C12 143.2(6) . . . . ? C3 P1 C7 C8 -169.8(6) . . . . ? C13 P1 C7 C8 84.3(7) . . . . ? Cu1 P1 C7 C8 -40.2(7) . . . . ? C76 C71 C72 C73 -1.8(13) . . . . ? P3 C71 C72 C73 179.7(7) . . . . ? C25 C26 C27 C28 0.1(12) . . . . ? C13 C14 C15 C16 0.0(10) . . . . ? C17 C16 C15 C14 -0.5(10) . . . . ? C1 C6 C5 C4 0.9(12) . . . . ? C3 C4 C5 C6 -0.4(12) . . . . ? C26 C27 C28 C29 0.6(13) . . . . ? C36 C31 C32 C33 -4.0(15) . . . . ? P2 C31 C32 C33 172.3(8) . . . . ? C83 C88 C87 C86 -2.1(12) . . . . ? C71 C72 C73 C74 1.3(14) . . . . ? C88 C87 C86 C85 3.0(12) . . . . ? C37 C38 C39 C40 -1.6(11) . . . . ? C88 C83 C84 C85 0.1(11) . . . . ? P3 C83 C84 C85 174.9(6) . . . . ? C82 C77 C78 C79 -3.2(13) . . . . ? P3 C77 C78 C79 174.7(7) . . . . ? C12 C7 C8 C9 3.6(12) . . . . ? P1 C7 C8 C9 -173.2(7) . . . . ? C57 C58 C59 C60 0.4(17) . . . . ? C61 C60 C59 C58 1.8(16) . . . . ? C24 C23 C22 C21 -0.5(12) . . . . ? C25 C30 C29 C28 -2.5(14) . . . . ? C27 C28 C29 C30 0.6(14) . . . . ? C77 C78 C79 C80 1.1(15) . . . . ? C13 C18 C17 C16 -1.5(10) . . . . ? C15 C16 C17 C18 1.2(10) . . . . ? C12 C11 C10 C9 1.9(13) . . . . ? C66 C67 C69 C70 -2.9(12) . . . . ? C68 C67 C69 C70 -178.1(8) . . . . ? C50 C49 C48 C47 -1.3(13) . . . . ? C38 C39 C40 C42 0.9(11) . . . . ? C38 C39 C40 C41 -177.3(7) . . . . ? C11 C10 C9 C8 -1.3(15) . . . . ? C7 C8 C9 C10 -1.5(15) . . . . ? C72 C73 C74 C75 0.0(14) . . . . ? C24 C19 C20 C21 2.0(12) . . . . ? P2 C19 C20 C21 -179.6(6) . . . . ? C78 C77 C82 C81 4.3(14) . . . . ? P3 C77 C82 C81 -173.5(7) . . . . ? C20 C19 C24 C23 -1.4(11) . . . . ? P2 C19 C24 C23 -179.7(6) . . . . ? C22 C23 C24 C19 0.6(11) . . . . ? C59 C60 C61 C62 -3.2(14) . . . . ? C57 C62 C61 C60 2.5(13) . . . . ? C67 C69 C70 C64 1.1(12) . . . . ? C65 C64 C70 C69 0.8(11) . . . . ? S5 C64 C70 C69 179.9(6) . . . . ? C51 C56 C55 C54 0.8(13) . . . . ? C53 C54 C55 C56 0.8(13) . . . . ? C83 C84 C85 C86 0.8(11) . . . . ? C87 C86 C85 C84 -2.3(11) . . . . ? C51 C52 C53 C54 0.8(12) . . . . ? C55 C54 C53 C52 -1.5(13) . . . . ? C23 C22 C21 C20 1.1(13) . . . . ? C19 C20 C21 C22 -1.8(13) . . . . ? C49 C48 C47 C46 0.6(13) . . . . ? C45 C46 C47 C48 0.1(13) . . . . ? C39 C40 C42 C43 0.5(12) . . . . ? C41 C40 C42 C43 178.8(8) . . . . ? C37 C43 C42 C40 -1.2(13) . . . . ? C73 C74 C75 C76 -0.7(15) . . . . ? C71 C76 C75 C74 0.2(13) . . . . ? C78 C79 C80 C81 -0.1(16) . . . . ? C79 C80 C81 C82 1.2(17) . . . . ? C77 C82 C81 C80 -3.3(16) . . . . ? C64 C65 C66 C67 -1.1(13) . . . . ? C69 C67 C66 C65 2.9(13) . . . . ? C68 C67 C66 C65 178.4(8) . . . . ? C31 C36 C35 C34 -1.1(13) . . . . ? C36 C35 C34 C33 -2.0(16) . . . . ? C35 C34 C33 C32 2.0(17) . . . . ? C31 C32 C33 C34 1.0(17) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.343 _refine_diff_density_min -1.394 _refine_diff_density_rms 0.211 #end data_complex2 _database_code_depnum_ccdc_archive 'CCDC 745654' #TrackingRef '- CIF_All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H37 N O2 P2 Pd S3' _chemical_formula_sum 'C44 H37 N O2 P2 Pd S3' _chemical_formula_weight 876.27 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3447(2) _cell_length_b 18.3512(2) _cell_length_c 25.5480(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7662.99(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 115341 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min 0.8305 _exptl_absorpt_correction_T_max 0.9131 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '519 1.2 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 114928 _diffrn_reflns_av_R_equivalents 0.0919 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8754 _reflns_number_gt 6307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0549P)^2^+6.8949P] 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 8754 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Pd Pd 0.454724(13) 0.105341(11) 0.241901(9) 0.02755(8) Uani 1 1 d . . . S1 S 0.46502(5) 0.11500(4) 0.33167(3) 0.03321(18) Uani 1 1 d . . . S2 S 0.38220(5) 0.21178(4) 0.26300(3) 0.03468(18) Uani 1 1 d . . . S3 S 0.40713(5) 0.22408(4) 0.42687(3) 0.0376(2) Uani 1 1 d . . . P1 P 0.51714(5) -0.00755(4) 0.24159(3) 0.03071(18) Uani 1 1 d . A . P2 P 0.44333(5) 0.12020(4) 0.15176(3) 0.02880(17) Uani 1 1 d . . . O1 O 0.36188(15) 0.27791(12) 0.45564(10) 0.0476(6) Uani 1 1 d . . . O2 O 0.49472(14) 0.22311(13) 0.43267(9) 0.0463(6) Uani 1 1 d . . . N N 0.38064(16) 0.23719(13) 0.36538(11) 0.0358(6) Uani 1 1 d . . . C1 C 0.40653(18) 0.19446(15) 0.32840(12) 0.0312(7) Uani 1 1 d . . . C2 C 0.3696(2) 0.13752(17) 0.44638(12) 0.0350(7) Uani 1 1 d . . . C3 C 0.2866(2) 0.12863(19) 0.45554(13) 0.0401(8) Uani 1 1 d . . . H3 H 0.2500 0.1681 0.4501 0.048 Uiso 1 1 calc R . . C4 C 0.2574(2) 0.06212(19) 0.47259(13) 0.0453(8) Uani 1 1 d . . . H4 H 0.2005 0.0565 0.4790 0.054 Uiso 1 1 calc R . . C5 C 0.3092(3) 0.0035(2) 0.48060(14) 0.0472(9) Uani 1 1 d . . . C6 C 0.3920(2) 0.0133(2) 0.47067(14) 0.0488(9) Uani 1 1 d . . . H6 H 0.4285 -0.0264 0.4757 0.059 Uiso 1 1 calc R . . C7 C 0.4229(2) 0.0794(2) 0.45361(13) 0.0429(8) Uani 1 1 d . . . H7 H 0.4797 0.0849 0.4469 0.051 Uiso 1 1 calc R . . C8 C 0.2762(3) -0.0688(2) 0.49901(17) 0.0672(12) Uani 1 1 d . . . H8A H 0.2417 -0.0613 0.5299 0.101 Uiso 1 1 calc R . . H8B H 0.3218 -0.1011 0.5080 0.101 Uiso 1 1 calc R . . H8C H 0.2436 -0.0910 0.4710 0.101 Uiso 1 1 calc R . . C9 C 0.55063(19) -0.04074(16) 0.30585(12) 0.0318(7) Uani 1 1 d . . . C10 C 0.6300(13) -0.0321(14) 0.3252(9) 0.059(5) Uani 0.49(3) 1 d P A 1 H10 H 0.6691 -0.0068 0.3046 0.071 Uiso 0.49(3) 1 calc PR A 1 C11 C 0.6531(15) -0.0586(16) 0.3727(8) 0.079(7) Uani 0.49(3) 1 d P A 1 H11 H 0.7085 -0.0531 0.3834 0.095 Uiso 0.49(3) 1 calc PR A 1 C13 C 0.5219(10) -0.1007(10) 0.3875(7) 0.054(5) Uani 0.49(3) 1 d P A 1 H13 H 0.4849 -0.1260 0.4096 0.065 Uiso 0.49(3) 1 calc PR A 1 C14 C 0.4946(8) -0.0740(10) 0.3395(7) 0.057(4) Uani 0.49(3) 1 d P A 1 H14 H 0.4387 -0.0783 0.3299 0.068 Uiso 0.49(3) 1 calc PR A 1 C10A C 0.6144(10) -0.0076(8) 0.3288(7) 0.032(2) Uani 0.51(3) 1 d P A 2 H10A H 0.6408 0.0315 0.3112 0.039 Uiso 0.51(3) 1 calc PR A 2 C11A C 0.6426(11) -0.0291(8) 0.3775(8) 0.045(3) Uani 0.51(3) 1 d P A 2 H11A H 0.6869 -0.0044 0.3937 0.054 Uiso 0.51(3) 1 calc PR A 2 C13A C 0.5397(16) -0.1212(12) 0.3797(8) 0.085(7) Uani 0.51(3) 1 d P A 2 H13A H 0.5111 -0.1597 0.3965 0.102 Uiso 0.51(3) 1 calc PR A 2 C14A C 0.5142(14) -0.0976(11) 0.3302(8) 0.075(6) Uani 0.51(3) 1 d P A 2 H14A H 0.4703 -0.1221 0.3133 0.090 Uiso 0.51(3) 1 calc PR A 2 C12 C 0.6027(2) -0.09080(19) 0.40353(15) 0.0476(9) Uani 1 1 d . . . H12 H 0.6203 -0.1077 0.4368 0.057 Uiso 1 1 calc R A 1 C15 C 0.4435(2) -0.07680(17) 0.22273(14) 0.0383(8) Uani 1 1 d . . . C16 C 0.3616(2) -0.0602(2) 0.22838(17) 0.0548(10) Uani 1 1 d . A . H16 H 0.3461 -0.0119 0.2374 0.066 Uiso 1 1 calc R . . C17 C 0.3019(3) -0.1123(2) 0.2211(2) 0.0661(13) Uani 1 1 d . . . H17 H 0.2459 -0.0999 0.2261 0.079 Uiso 1 1 calc R A . C18 C 0.3227(3) -0.1813(2) 0.20696(16) 0.0551(10) Uani 1 1 d . A . H18 H 0.2814 -0.2168 0.2010 0.066 Uiso 1 1 calc R . . C19 C 0.4021(3) -0.1988(2) 0.2015(2) 0.0848(18) Uani 1 1 d . . . H19 H 0.4168 -0.2470 0.1915 0.102 Uiso 1 1 calc R A . C20 C 0.4628(2) -0.1475(2) 0.2101(2) 0.0841(19) Uani 1 1 d . A . H20 H 0.5186 -0.1614 0.2074 0.101 Uiso 1 1 calc R . . C21 C 0.6118(2) -0.01021(17) 0.20378(12) 0.0345(7) Uani 1 1 d . . . C22 C 0.65679(19) 0.05396(19) 0.20362(14) 0.0402(8) Uani 1 1 d . A . H22 H 0.6358 0.0956 0.2211 0.048 Uiso 1 1 calc R . . C23 C 0.7318(2) 0.0584(2) 0.17842(15) 0.0514(9) Uani 1 1 d . . . H23 H 0.7621 0.1026 0.1788 0.062 Uiso 1 1 calc R A . C24 C 0.7618(3) -0.0016(3) 0.15308(15) 0.0616(12) Uani 1 1 d . A . H24 H 0.8131 0.0009 0.1357 0.074 Uiso 1 1 calc R . . C25 C 0.7181(3) -0.0653(3) 0.15272(18) 0.0794(16) Uani 1 1 d . . . H25 H 0.7397 -0.1066 0.1351 0.095 Uiso 1 1 calc R A . C26 C 0.6425(3) -0.0705(2) 0.17785(16) 0.0636(12) Uani 1 1 d . A . H26 H 0.6125 -0.1149 0.1772 0.076 Uiso 1 1 calc R . . C27 C 0.45131(18) 0.03875(15) 0.11049(12) 0.0305(6) Uani 1 1 d . . . C28 C 0.3828(2) -0.00535(17) 0.10481(14) 0.0397(8) Uani 1 1 d . . . H28 H 0.3314 0.0104 0.1181 0.048 Uiso 1 1 calc R . . C29 C 0.3889(2) -0.07236(18) 0.07974(15) 0.0478(9) Uani 1 1 d . . . H29 H 0.3420 -0.1026 0.0763 0.057 Uiso 1 1 calc R . . C30 C 0.4631(2) -0.09493(18) 0.05990(14) 0.0449(9) Uani 1 1 d . . . H30 H 0.4674 -0.1409 0.0430 0.054 Uiso 1 1 calc R . . C31 C 0.5309(2) -0.05117(19) 0.06454(13) 0.0444(8) Uani 1 1 d . . . H31 H 0.5817 -0.0665 0.0501 0.053 Uiso 1 1 calc R . . C32 C 0.5257(2) 0.01550(17) 0.09031(13) 0.0369(7) Uani 1 1 d . . . H32 H 0.5730 0.0451 0.0941 0.044 Uiso 1 1 calc R . . C33 C 0.52211(18) 0.18128(15) 0.12659(13) 0.0317(7) Uani 1 1 d . . . C34 C 0.53651(19) 0.19025(17) 0.07359(13) 0.0358(7) Uani 1 1 d . . . H34 H 0.5034 0.1652 0.0489 0.043 Uiso 1 1 calc R . . C35 C 0.5990(2) 0.23550(17) 0.05624(14) 0.0423(8) Uani 1 1 d . . . H35 H 0.6074 0.2426 0.0198 0.051 Uiso 1 1 calc R . . C36 C 0.6491(2) 0.27030(19) 0.09224(15) 0.0488(9) Uani 1 1 d . . . H36 H 0.6930 0.2999 0.0804 0.059 Uiso 1 1 calc R . . C37 C 0.6353(2) 0.26212(19) 0.14508(15) 0.0478(9) Uani 1 1 d . . . H37 H 0.6696 0.2863 0.1696 0.057 Uiso 1 1 calc R . . C38 C 0.5713(2) 0.21842(16) 0.16268(14) 0.0373(7) Uani 1 1 d . . . H38 H 0.5610 0.2138 0.1991 0.045 Uiso 1 1 calc R . . C39 C 0.34519(18) 0.15909(17) 0.13201(13) 0.0349(7) Uani 1 1 d . . . C40 C 0.3372(2) 0.2081(2) 0.09078(14) 0.0465(9) Uani 1 1 d . . . H40 H 0.3846 0.2259 0.0735 0.056 Uiso 1 1 calc R . . C41 C 0.2601(2) 0.2312(2) 0.07475(16) 0.0614(11) Uani 1 1 d . . . H41 H 0.2552 0.2649 0.0467 0.074 Uiso 1 1 calc R . . C42 C 0.1912(2) 0.2056(3) 0.09925(18) 0.0664(13) Uani 1 1 d . . . H42 H 0.1386 0.2211 0.0879 0.080 Uiso 1 1 calc R . . C43 C 0.1982(2) 0.1578(2) 0.14023(18) 0.0568(11) Uani 1 1 d . . . H43 H 0.1504 0.1400 0.1571 0.068 Uiso 1 1 calc R . . C44 C 0.2746(2) 0.13510(19) 0.15717(15) 0.0440(8) Uani 1 1 d . . . H44 H 0.2788 0.1029 0.1862 0.053 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 Pd 0.02481(13) 0.01997(12) 0.03789(15) -0.00155(9) 0.00241(9) -0.00075(9) S1 0.0339(4) 0.0268(4) 0.0389(4) -0.0035(3) 0.0001(3) 0.0053(3) S2 0.0347(4) 0.0257(4) 0.0437(5) -0.0008(3) 0.0023(3) 0.0046(3) S3 0.0339(4) 0.0347(4) 0.0443(5) -0.0089(3) 0.0020(4) -0.0014(3) P1 0.0311(4) 0.0201(4) 0.0409(5) -0.0013(3) -0.0004(3) 0.0006(3) P2 0.0237(4) 0.0233(4) 0.0394(4) -0.0020(3) 0.0020(3) -0.0010(3) O1 0.0514(15) 0.0389(13) 0.0525(15) -0.0150(11) 0.0068(12) 0.0000(11) O2 0.0304(13) 0.0516(15) 0.0570(15) -0.0102(12) -0.0038(11) -0.0061(11) N 0.0327(14) 0.0268(13) 0.0479(16) -0.0044(12) 0.0034(12) 0.0014(11) C1 0.0230(15) 0.0251(14) 0.0455(18) 0.0000(13) 0.0023(13) -0.0050(12) C2 0.0358(18) 0.0363(17) 0.0329(17) -0.0035(13) -0.0030(14) 0.0023(14) C3 0.0365(18) 0.0401(18) 0.0436(19) -0.0029(15) -0.0040(15) 0.0036(15) C4 0.043(2) 0.048(2) 0.045(2) -0.0036(16) -0.0009(16) -0.0078(17) C5 0.064(3) 0.0404(19) 0.037(2) -0.0032(15) -0.0031(17) -0.0057(18) C6 0.059(2) 0.042(2) 0.046(2) 0.0012(16) -0.0047(18) 0.0115(18) C7 0.0387(19) 0.050(2) 0.0397(19) -0.0014(16) -0.0010(15) 0.0093(16) C8 0.098(4) 0.043(2) 0.061(3) 0.0026(19) 0.002(2) -0.009(2) C9 0.0348(17) 0.0200(14) 0.0405(18) -0.0024(12) 0.0026(14) 0.0009(13) C10 0.031(8) 0.080(13) 0.067(9) 0.024(10) -0.008(6) -0.020(8) C11 0.067(12) 0.113(17) 0.058(9) 0.037(10) -0.039(8) -0.059(11) C13 0.054(6) 0.049(9) 0.060(7) 0.022(6) 0.026(6) 0.015(6) C14 0.033(4) 0.067(10) 0.070(8) 0.033(7) 0.014(5) 0.019(6) C10A 0.026(5) 0.033(5) 0.039(5) 0.009(4) 0.002(4) 0.003(4) C11A 0.033(5) 0.048(7) 0.053(6) 0.000(6) 0.000(4) -0.006(5) C13A 0.142(17) 0.046(9) 0.068(10) 0.040(7) -0.061(10) -0.054(10) C14A 0.083(12) 0.050(9) 0.091(11) 0.028(7) -0.044(10) -0.051(8) C12 0.061(3) 0.043(2) 0.039(2) 0.0020(16) -0.0070(18) -0.0036(18) C15 0.0408(19) 0.0248(15) 0.049(2) -0.0002(14) -0.0110(15) -0.0025(14) C16 0.047(2) 0.0349(19) 0.083(3) -0.0191(18) 0.023(2) -0.0105(16) C17 0.050(2) 0.054(3) 0.095(3) -0.023(2) 0.027(2) -0.018(2) C18 0.059(3) 0.0356(19) 0.071(3) -0.0010(18) -0.009(2) -0.0150(18) C19 0.051(3) 0.031(2) 0.172(5) -0.035(3) -0.041(3) 0.0069(19) C20 0.035(2) 0.034(2) 0.183(6) -0.036(3) -0.036(3) 0.0104(17) C21 0.0368(18) 0.0315(16) 0.0351(17) 0.0047(13) -0.0006(14) 0.0084(14) C22 0.0282(17) 0.0438(19) 0.049(2) -0.0041(15) 0.0008(15) 0.0028(14) C23 0.0314(19) 0.070(3) 0.052(2) 0.007(2) 0.0009(16) -0.0018(18) C24 0.048(2) 0.088(3) 0.049(2) 0.021(2) 0.0150(19) 0.026(2) C25 0.106(4) 0.066(3) 0.066(3) 0.013(2) 0.045(3) 0.048(3) C26 0.096(3) 0.038(2) 0.057(2) 0.0041(18) 0.029(2) 0.017(2) C27 0.0345(17) 0.0232(14) 0.0337(16) -0.0011(12) -0.0038(13) 0.0012(12) C28 0.0376(19) 0.0289(16) 0.053(2) -0.0029(14) -0.0052(15) -0.0020(14) C29 0.050(2) 0.0319(17) 0.062(2) -0.0054(16) -0.0142(18) -0.0042(16) C30 0.066(3) 0.0283(17) 0.040(2) -0.0061(14) -0.0080(17) 0.0065(17) C31 0.052(2) 0.0402(19) 0.041(2) -0.0059(15) 0.0042(16) 0.0095(17) C32 0.0368(18) 0.0332(17) 0.0406(19) -0.0045(14) 0.0020(14) 0.0007(14) C33 0.0260(15) 0.0238(14) 0.0453(19) -0.0016(13) 0.0037(13) 0.0013(12) C34 0.0330(18) 0.0306(16) 0.0438(19) -0.0016(13) 0.0032(14) 0.0010(13) C35 0.046(2) 0.0315(17) 0.049(2) 0.0014(15) 0.0149(16) 0.0000(15) C36 0.047(2) 0.0388(19) 0.061(2) -0.0076(17) 0.0176(18) -0.0159(16) C37 0.044(2) 0.0407(19) 0.059(2) -0.0084(17) 0.0044(17) -0.0161(16) C38 0.0374(18) 0.0305(16) 0.0442(19) -0.0050(14) 0.0065(15) -0.0051(14) C39 0.0246(16) 0.0321(16) 0.0481(19) -0.0077(14) -0.0018(14) 0.0015(13) C40 0.0341(19) 0.052(2) 0.053(2) 0.0050(17) -0.0028(16) 0.0117(16) C41 0.048(2) 0.078(3) 0.059(2) 0.001(2) -0.008(2) 0.027(2) C42 0.039(2) 0.089(3) 0.071(3) -0.030(3) -0.014(2) 0.022(2) C43 0.0292(19) 0.066(3) 0.075(3) -0.025(2) 0.0051(18) 0.0007(18) C44 0.0322(18) 0.0434(19) 0.056(2) -0.0107(16) 0.0047(16) 0.0015(15) _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 Pd S1 2.3064(8) . ? Pd P1 2.3092(8) . ? Pd P2 2.3265(9) . ? Pd S2 2.3476(8) . ? S1 C1 1.746(3) . ? S2 C1 1.747(3) . ? S3 O1 1.437(2) . ? S3 O2 1.439(2) . ? S3 N 1.647(3) . ? S3 C2 1.774(3) . ? P1 C15 1.816(3) . ? P1 C21 1.825(3) . ? P1 C9 1.835(3) . ? P2 C33 1.824(3) . ? P2 C39 1.827(3) . ? P2 C27 1.834(3) . ? N C1 1.298(4) . ? C2 C3 1.387(4) . ? C2 C7 1.389(5) . ? C3 C4 1.381(5) . ? C3 H3 0.9500 . ? C4 C5 1.384(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(5) . ? C5 C8 1.507(5) . ? C6 C7 1.384(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10A 1.341(19) . ? C9 C14A 1.353(15) . ? C9 C14 1.397(16) . ? C9 C10 1.40(2) . ? C10 C11 1.36(3) . ? C10 H10 0.9500 . ? C11 C12 1.28(2) . ? C11 H11 0.9500 . ? C13 C14 1.39(3) . ? C13 C12 1.40(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C10A C11A 1.39(3) . ? C10A H10A 0.9500 . ? C11A C12 1.465(19) . ? C11A H11A 0.9500 . ? C13A C12 1.320(18) . ? C13A C14A 1.40(2) . ? C13A H13A 0.9500 . ? C14A H14A 0.9500 . ? C12 H12 0.9500 . ? C15 C20 1.374(5) . ? C15 C16 1.380(5) . ? C16 C17 1.380(5) . ? C16 H16 0.9500 . ? C17 C18 1.360(5) . ? C17 H17 0.9500 . ? C18 C19 1.345(6) . ? C18 H18 0.9500 . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.384(5) . ? C21 C22 1.388(5) . ? C22 C23 1.388(5) . ? C22 H22 0.9500 . ? C23 C24 1.368(6) . ? C23 H23 0.9500 . ? C24 C25 1.369(7) . ? C24 H24 0.9500 . ? C25 C26 1.397(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.388(4) . ? C27 C28 1.390(4) . ? C28 C29 1.390(5) . ? C28 H28 0.9500 . ? C29 C30 1.378(5) . ? C29 H29 0.9500 . ? C30 C31 1.374(5) . ? C30 H30 0.9500 . ? C31 C32 1.392(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.384(5) . ? C33 C38 1.400(4) . ? C34 C35 1.389(4) . ? C34 H34 0.9500 . ? C35 C36 1.387(5) . ? C35 H35 0.9500 . ? C36 C37 1.377(5) . ? C36 H36 0.9500 . ? C37 C38 1.393(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.391(5) . ? C39 C44 1.392(5) . ? C40 C41 1.391(5) . ? C40 H40 0.9500 . ? C41 C42 1.372(6) . ? C41 H41 0.9500 . ? C42 C43 1.371(6) . ? C42 H42 0.9500 . ? C43 C44 1.386(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? 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 S1 Pd P1 92.30(3) . . ? S1 Pd P2 168.85(3) . . ? P1 Pd P2 97.88(3) . . ? S1 Pd S2 75.20(3) . . ? P1 Pd S2 166.00(3) . . ? P2 Pd S2 95.13(3) . . ? C1 S1 Pd 88.67(11) . . ? C1 S2 Pd 87.32(10) . . ? O1 S3 O2 117.89(15) . . ? O1 S3 N 104.62(14) . . ? O2 S3 N 111.20(14) . . ? O1 S3 C2 107.10(15) . . ? O2 S3 C2 107.67(15) . . ? N S3 C2 107.93(14) . . ? C15 P1 C21 113.76(16) . . ? C15 P1 C9 101.71(15) . . ? C21 P1 C9 102.23(14) . . ? C15 P1 Pd 109.63(11) . . ? C21 P1 Pd 113.61(10) . . ? C9 P1 Pd 115.25(10) . . ? C33 P2 C39 106.41(14) . . ? C33 P2 C27 104.36(14) . . ? C39 P2 C27 102.83(14) . . ? C33 P2 Pd 111.37(11) . . ? C39 P2 Pd 112.93(11) . . ? C27 P2 Pd 117.89(10) . . ? C1 N S3 121.3(2) . . ? N C1 S1 130.4(3) . . ? N C1 S2 120.8(2) . . ? S1 C1 S2 108.81(17) . . ? C3 C2 C7 120.0(3) . . ? C3 C2 S3 119.4(2) . . ? C7 C2 S3 120.6(3) . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 121.5(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 117.9(3) . . ? C4 C5 C8 120.8(4) . . ? C6 C5 C8 121.3(4) . . ? C7 C6 C5 121.7(3) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C2 119.2(3) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 120.4 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10A C9 C14A 119.4(10) . . ? C10A C9 C14 116.0(11) . . ? C14A C9 C10 109.5(10) . . ? C14 C9 C10 116.1(11) . . ? C10A C9 P1 118.2(8) . . ? C14A C9 P1 122.4(7) . . ? C14 C9 P1 120.0(7) . . ? C10 C9 P1 123.8(9) . . ? C11 C10 C9 122.2(17) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C12 C11 C10 122.2(17) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C14 C13 C12 121.1(13) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C9 119.0(13) . . ? C13 C14 H14 120.5 . . ? C9 C14 H14 120.5 . . ? C9 C10A C11A 121.5(14) . . ? C9 C10A H10A 119.3 . . ? C11A C10A H10A 119.3 . . ? C10A C11A C12 118.7(15) . . ? C10A C11A H11A 120.7 . . ? C12 C11A H11A 120.7 . . ? C12 C13A C14A 121.2(14) . . ? C12 C13A H13A 119.4 . . ? C14A C13A H13A 119.4 . . ? C9 C14A C13A 121.5(11) . . ? C9 C14A H14A 119.3 . . ? C13A C14A H14A 119.3 . . ? C11 C12 C13A 114.3(11) . . ? C11 C12 C13 119.1(11) . . ? C13A C12 C11A 117.7(11) . . ? C13 C12 C11A 112.8(11) . . ? C11 C12 H12 120.4 . . ? C13A C12 H12 120.7 . . ? C13 C12 H12 120.4 . . ? C11A C12 H12 121.6 . . ? C20 C15 C16 117.2(3) . . ? C20 C15 P1 124.8(3) . . ? C16 C15 P1 117.4(3) . . ? C17 C16 C15 121.3(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 119.5(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.8(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C15 C20 C19 120.9(4) . . ? C15 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C26 C21 C22 119.0(3) . . ? C26 C21 P1 125.6(3) . . ? C22 C21 P1 115.3(2) . . ? C23 C22 C21 121.3(3) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C24 C23 C22 119.3(4) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 121.2(4) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C21 C26 C25 119.0(4) . . ? C21 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C32 C27 C28 119.2(3) . . ? C32 C27 P2 121.8(2) . . ? C28 C27 P2 118.5(2) . . ? C27 C28 C29 120.3(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.3(3) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 120.0(3) . . ? C27 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C38 119.3(3) . . ? C34 C33 P2 122.5(2) . . ? C38 C33 P2 118.2(2) . . ? C33 C34 C35 120.6(3) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 120.3(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.1(3) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 119.9(3) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? C40 C39 C44 118.4(3) . . ? C40 C39 P2 123.0(2) . . ? C44 C39 P2 118.5(3) . . ? C39 C40 C41 120.3(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 120.4(4) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 119.9(4) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 120.4(4) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 120.5(4) . . ? C43 C44 H44 119.7 . . ? C39 C44 H44 119.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.898 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.093 #end # Attachment '- CIF_All.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 745655' #TrackingRef '- CIF_All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H37 N O2 P2 Pt S3' _chemical_formula_sum 'C44 H37 N O2 P2 Pt S3' _chemical_formula_weight 964.96 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.33090(10) _cell_length_b 18.3563(2) _cell_length_c 25.5228(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7651.09(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 100741 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 3.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2916 _exptl_absorpt_correction_T_max 0.6723 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '447 1.2 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 117355 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8720 _reflns_number_gt 6528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0279P)^2^+9.9593P] 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 8720 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.003 _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 Pt Pt 0.454382(7) 0.104562(7) 0.241635(5) 0.02543(5) Uani 1 1 d . . . S1 S 0.46334(5) 0.11393(5) 0.33215(3) 0.0314(2) Uani 1 1 d . . . S2 S 0.38269(5) 0.21181(5) 0.26302(3) 0.0326(2) Uani 1 1 d . . . S3 S 0.40663(6) 0.22438(5) 0.42732(4) 0.0362(2) Uani 1 1 d . . . P1 P 0.51529(6) -0.00742(5) 0.24061(4) 0.02823(19) Uani 1 1 d . A . P2 P 0.44348(5) 0.12034(5) 0.15270(3) 0.02629(19) Uani 1 1 d . . . O1 O 0.36164(17) 0.27845(15) 0.45601(10) 0.0458(7) Uani 1 1 d . . . O2 O 0.49426(15) 0.22301(16) 0.43307(10) 0.0451(7) Uani 1 1 d . . . N N 0.38035(18) 0.23736(16) 0.36568(12) 0.0340(7) Uani 1 1 d . . . C1 C 0.4065(2) 0.19438(19) 0.32874(14) 0.0307(8) Uani 1 1 d . . . C2 C 0.3694(2) 0.1381(2) 0.44688(14) 0.0350(8) Uani 1 1 d . . . C3 C 0.2857(2) 0.1294(2) 0.45623(15) 0.0389(9) Uani 1 1 d . . . H3 H 0.2493 0.1691 0.4510 0.047 Uiso 1 1 calc R . . C4 C 0.2559(3) 0.0628(2) 0.47313(15) 0.0423(9) Uani 1 1 d . . . H4 H 0.1989 0.0572 0.4794 0.051 Uiso 1 1 calc R . . C5 C 0.3083(3) 0.0042(2) 0.48099(15) 0.0481(11) Uani 1 1 d . . . C6 C 0.3910(3) 0.0132(2) 0.47146(16) 0.0482(10) Uani 1 1 d . . . H6 H 0.4273 -0.0265 0.4767 0.058 Uiso 1 1 calc R . . C7 C 0.4218(3) 0.0798(2) 0.45421(15) 0.0426(10) Uani 1 1 d . . . H7 H 0.4787 0.0851 0.4475 0.051 Uiso 1 1 calc R . . C8 C 0.2750(3) -0.0683(3) 0.49960(19) 0.0667(14) Uani 1 1 d . . . H8A H 0.2447 -0.0613 0.5324 0.100 Uiso 1 1 calc R . . H8B H 0.3204 -0.1022 0.5055 0.100 Uiso 1 1 calc R . . H8C H 0.2382 -0.0884 0.4729 0.100 Uiso 1 1 calc R . . C9 C 0.5491(2) -0.04000(19) 0.30512(13) 0.0291(7) Uani 1 1 d . . . C10 C 0.6291(14) -0.0301(16) 0.3249(10) 0.058(6) Uani 0.51(4) 1 d P A 1 H10 H 0.6680 -0.0029 0.3053 0.070 Uiso 0.51(4) 1 calc PR A 1 C11 C 0.6505(15) -0.0590(18) 0.3713(10) 0.079(8) Uani 0.51(4) 1 d P A 1 H11 H 0.7064 -0.0558 0.3813 0.095 Uiso 0.51(4) 1 calc PR A 1 C13 C 0.5210(10) -0.1000(10) 0.3855(7) 0.042(4) Uani 0.51(4) 1 d P A 1 H13 H 0.4836 -0.1256 0.4072 0.051 Uiso 0.51(4) 1 calc PR A 1 C14 C 0.4957(9) -0.0747(14) 0.3401(9) 0.046(5) Uani 0.51(4) 1 d P A 1 H14 H 0.4398 -0.0801 0.3308 0.055 Uiso 0.51(4) 1 calc PR A 1 C10A C 0.6127(13) -0.0074(12) 0.3264(9) 0.036(3) Uani 0.49(4) 1 d P A 2 H10A H 0.6384 0.0316 0.3083 0.044 Uiso 0.49(4) 1 calc PR A 2 C11A C 0.6442(11) -0.0295(10) 0.3769(7) 0.035(3) Uani 0.49(4) 1 d P A 2 H11A H 0.6900 -0.0061 0.3925 0.042 Uiso 0.49(4) 1 calc PR A 2 C13A C 0.538(2) -0.1208(17) 0.3802(10) 0.091(9) Uani 0.49(4) 1 d P A 2 H13A H 0.5105 -0.1600 0.3970 0.109 Uiso 0.49(4) 1 calc PR A 2 C14A C 0.510(2) -0.0942(16) 0.3288(11) 0.078(8) Uani 0.49(4) 1 d P A 2 H14A H 0.4633 -0.1158 0.3126 0.093 Uiso 0.49(4) 1 calc PR A 2 C12 C 0.6016(3) -0.0902(2) 0.40279(16) 0.0478(11) Uani 1 1 d . . . H12 H 0.6189 -0.1061 0.4364 0.057 Uiso 1 1 calc R A 1 C15 C 0.4422(2) -0.0772(2) 0.22246(15) 0.0343(8) Uani 1 1 d . . . C16 C 0.3597(3) -0.0611(2) 0.22821(18) 0.0518(11) Uani 1 1 d . A . H16 H 0.3435 -0.0129 0.2368 0.062 Uiso 1 1 calc R . . C17 C 0.3006(3) -0.1145(3) 0.2216(2) 0.0607(13) Uani 1 1 d . . . H17 H 0.2444 -0.1027 0.2265 0.073 Uiso 1 1 calc R A . C18 C 0.3221(3) -0.1835(2) 0.20813(17) 0.0487(10) Uani 1 1 d . A . H18 H 0.2812 -0.2193 0.2020 0.058 Uiso 1 1 calc R . . C19 C 0.4017(3) -0.2008(3) 0.2036(2) 0.0720(17) Uani 1 1 d . . . H19 H 0.4169 -0.2491 0.1946 0.086 Uiso 1 1 calc R A . C20 C 0.4616(3) -0.1488(3) 0.2118(3) 0.0710(17) Uani 1 1 d . A . H20 H 0.5176 -0.1628 0.2101 0.085 Uiso 1 1 calc R . . C21 C 0.6101(2) -0.0106(2) 0.20293(14) 0.0331(8) Uani 1 1 d . . . C22 C 0.6558(2) 0.0532(2) 0.20299(15) 0.0380(9) Uani 1 1 d . A . H22 H 0.6351 0.0952 0.2203 0.046 Uiso 1 1 calc R . . C23 C 0.7312(2) 0.0564(3) 0.17813(16) 0.0501(11) Uani 1 1 d . . . H23 H 0.7622 0.1002 0.1789 0.060 Uiso 1 1 calc R A . C24 C 0.7609(3) -0.0037(3) 0.15237(17) 0.0600(14) Uani 1 1 d . A . H24 H 0.8125 -0.0017 0.1352 0.072 Uiso 1 1 calc R . . C25 C 0.7161(3) -0.0663(3) 0.1515(2) 0.0724(17) Uani 1 1 d . . . H25 H 0.7367 -0.1076 0.1333 0.087 Uiso 1 1 calc R A . C26 C 0.6401(3) -0.0708(2) 0.17697(18) 0.0589(13) Uani 1 1 d . A . H26 H 0.6097 -0.1149 0.1763 0.071 Uiso 1 1 calc R . . C27 C 0.4514(2) 0.03895(19) 0.11139(13) 0.0297(7) Uani 1 1 d . . . C28 C 0.3828(2) -0.0058(2) 0.10596(15) 0.0378(9) Uani 1 1 d . . . H28 H 0.3317 0.0093 0.1199 0.045 Uiso 1 1 calc R . . C29 C 0.3888(3) -0.0721(2) 0.08048(16) 0.0451(10) Uani 1 1 d . . . H29 H 0.3418 -0.1023 0.0771 0.054 Uiso 1 1 calc R . . C30 C 0.4628(3) -0.0943(2) 0.05998(16) 0.0447(10) Uani 1 1 d . . . H30 H 0.4671 -0.1402 0.0430 0.054 Uiso 1 1 calc R . . C31 C 0.5297(3) -0.0502(2) 0.06407(15) 0.0425(10) Uani 1 1 d . . . H31 H 0.5802 -0.0652 0.0490 0.051 Uiso 1 1 calc R . . C32 C 0.5252(2) 0.0160(2) 0.08985(14) 0.0348(8) Uani 1 1 d . . . H32 H 0.5726 0.0458 0.0928 0.042 Uiso 1 1 calc R . . C33 C 0.5218(2) 0.18154(19) 0.12716(14) 0.0295(8) Uani 1 1 d . . . C34 C 0.5352(2) 0.1904(2) 0.07373(14) 0.0348(8) Uani 1 1 d . . . H34 H 0.5019 0.1649 0.0493 0.042 Uiso 1 1 calc R . . C35 C 0.5966(2) 0.2360(2) 0.05573(16) 0.0398(9) Uani 1 1 d . . . H35 H 0.6036 0.2437 0.0192 0.048 Uiso 1 1 calc R . . C36 C 0.6479(2) 0.2705(2) 0.09127(17) 0.0460(10) Uani 1 1 d . . . H36 H 0.6917 0.2999 0.0789 0.055 Uiso 1 1 calc R . . C37 C 0.6356(2) 0.2623(2) 0.14454(16) 0.0441(10) Uani 1 1 d . . . H37 H 0.6703 0.2868 0.1687 0.053 Uiso 1 1 calc R . . C38 C 0.5726(2) 0.2185(2) 0.16262(15) 0.0354(8) Uani 1 1 d . . . H38 H 0.5637 0.2134 0.1992 0.042 Uiso 1 1 calc R . . C39 C 0.3449(2) 0.1591(2) 0.13328(14) 0.0323(8) Uani 1 1 d . . . C40 C 0.3367(2) 0.2082(2) 0.09251(16) 0.0456(10) Uani 1 1 d . . . H40 H 0.3842 0.2264 0.0756 0.055 Uiso 1 1 calc R . . C41 C 0.2597(3) 0.2311(3) 0.07596(18) 0.0594(13) Uani 1 1 d . . . H41 H 0.2549 0.2650 0.0480 0.071 Uiso 1 1 calc R . . C42 C 0.1905(3) 0.2048(3) 0.1002(2) 0.0612(14) Uani 1 1 d . . . H42 H 0.1379 0.2200 0.0887 0.073 Uiso 1 1 calc R . . C43 C 0.1973(2) 0.1567(3) 0.14094(19) 0.0526(12) Uani 1 1 d . . . H43 H 0.1494 0.1383 0.1574 0.063 Uiso 1 1 calc R . . C44 C 0.2743(2) 0.1346(2) 0.15822(16) 0.0399(9) Uani 1 1 d . . . H44 H 0.2787 0.1026 0.1873 0.048 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 Pt 0.02523(7) 0.02474(7) 0.02633(8) -0.00139(5) 0.00158(5) -0.00093(5) S1 0.0356(5) 0.0314(5) 0.0271(5) -0.0023(3) 0.0003(4) 0.0046(4) S2 0.0358(5) 0.0300(5) 0.0319(5) -0.0013(4) 0.0012(4) 0.0051(4) S3 0.0355(5) 0.0414(6) 0.0316(5) -0.0077(4) 0.0030(4) -0.0022(4) P1 0.0311(4) 0.0246(4) 0.0290(5) -0.0017(4) -0.0004(4) 0.0013(4) P2 0.0244(4) 0.0280(5) 0.0264(5) -0.0018(3) 0.0007(3) -0.0012(4) O1 0.0540(16) 0.0443(16) 0.0391(16) -0.0140(12) 0.0086(13) 0.0016(13) O2 0.0340(14) 0.0594(19) 0.0421(16) -0.0071(13) -0.0029(12) -0.0074(13) N 0.0356(16) 0.0335(17) 0.0328(17) -0.0038(13) 0.0018(13) 0.0022(13) C1 0.0269(17) 0.0290(19) 0.036(2) -0.0038(15) 0.0013(15) -0.0052(15) C2 0.0346(19) 0.045(2) 0.0252(19) -0.0005(16) 0.0008(15) 0.0010(17) C3 0.038(2) 0.047(2) 0.032(2) -0.0051(17) -0.0001(17) 0.0027(18) C4 0.044(2) 0.051(3) 0.032(2) -0.0041(18) 0.0025(17) -0.006(2) C5 0.069(3) 0.048(3) 0.027(2) -0.0014(18) 0.0005(19) -0.009(2) C6 0.060(3) 0.047(3) 0.037(2) 0.0039(19) -0.002(2) 0.014(2) C7 0.040(2) 0.056(3) 0.032(2) 0.0022(18) 0.0000(17) 0.010(2) C8 0.098(4) 0.053(3) 0.049(3) 0.004(2) 0.007(3) -0.010(3) C9 0.0333(18) 0.0250(18) 0.0292(19) -0.0028(14) 0.0002(15) 0.0002(15) C10 0.025(8) 0.081(15) 0.069(10) 0.042(11) -0.020(6) -0.020(9) C11 0.073(11) 0.099(19) 0.066(11) 0.031(11) -0.049(9) -0.050(12) C13 0.045(6) 0.037(9) 0.045(7) 0.018(5) 0.018(6) 0.002(5) C14 0.025(5) 0.077(14) 0.035(9) 0.011(7) 0.004(5) 0.003(6) C10A 0.036(8) 0.043(8) 0.030(6) 0.018(5) -0.006(5) 0.007(5) C11A 0.031(5) 0.044(8) 0.029(5) 0.001(5) -0.001(4) -0.012(5) C13A 0.16(2) 0.054(14) 0.062(11) 0.030(9) -0.067(12) -0.044(14) C14A 0.125(19) 0.062(13) 0.046(12) 0.015(9) -0.040(12) -0.063(13) C12 0.066(3) 0.047(3) 0.030(2) 0.0061(18) -0.008(2) -0.001(2) C15 0.039(2) 0.0285(19) 0.035(2) 0.0011(16) -0.0073(16) 0.0020(16) C16 0.048(2) 0.039(2) 0.068(3) -0.018(2) 0.020(2) -0.011(2) C17 0.047(3) 0.053(3) 0.081(3) -0.022(3) 0.022(2) -0.019(2) C18 0.049(2) 0.039(2) 0.058(3) -0.006(2) -0.007(2) -0.012(2) C19 0.052(3) 0.033(3) 0.130(5) -0.026(3) -0.027(3) 0.002(2) C20 0.038(2) 0.039(3) 0.136(5) -0.028(3) -0.023(3) 0.007(2) C21 0.037(2) 0.039(2) 0.0234(18) 0.0041(15) 0.0002(15) 0.0060(17) C22 0.0306(19) 0.049(2) 0.034(2) -0.0020(17) 0.0014(16) 0.0040(17) C23 0.032(2) 0.077(3) 0.041(2) 0.010(2) 0.0003(18) 0.000(2) C24 0.044(3) 0.098(4) 0.038(2) 0.022(3) 0.013(2) 0.026(3) C25 0.093(4) 0.068(4) 0.055(3) 0.013(3) 0.039(3) 0.043(3) C26 0.084(3) 0.041(3) 0.052(3) 0.005(2) 0.028(3) 0.013(2) C27 0.0328(18) 0.0297(19) 0.0265(18) -0.0011(14) -0.0051(15) -0.0006(15) C28 0.035(2) 0.036(2) 0.042(2) -0.0050(17) -0.0027(17) -0.0027(17) C29 0.053(3) 0.034(2) 0.048(3) -0.0033(19) -0.013(2) -0.0073(19) C30 0.067(3) 0.033(2) 0.034(2) -0.0091(16) -0.011(2) 0.009(2) C31 0.050(2) 0.044(2) 0.034(2) -0.0057(17) 0.0034(18) 0.0073(19) C32 0.0324(19) 0.038(2) 0.034(2) -0.0030(16) -0.0010(15) 0.0003(16) C33 0.0256(16) 0.0298(19) 0.033(2) -0.0011(15) 0.0044(14) -0.0023(15) C34 0.036(2) 0.037(2) 0.032(2) -0.0009(16) 0.0021(15) -0.0010(16) C35 0.046(2) 0.038(2) 0.036(2) 0.0010(17) 0.0129(18) -0.0014(18) C36 0.045(2) 0.041(2) 0.053(3) -0.0033(19) 0.015(2) -0.0134(19) C37 0.045(2) 0.041(2) 0.046(3) -0.0066(18) 0.0026(19) -0.0153(19) C38 0.040(2) 0.034(2) 0.032(2) -0.0046(16) 0.0009(16) -0.0054(17) C39 0.0276(18) 0.036(2) 0.033(2) -0.0085(16) -0.0009(15) 0.0023(15) C40 0.035(2) 0.057(3) 0.045(2) 0.005(2) -0.0007(18) 0.0146(19) C41 0.052(3) 0.081(4) 0.046(3) 0.002(2) -0.006(2) 0.024(3) C42 0.037(2) 0.085(4) 0.062(3) -0.030(3) -0.016(2) 0.024(2) C43 0.029(2) 0.063(3) 0.066(3) -0.026(3) 0.002(2) 0.003(2) C44 0.0327(19) 0.043(2) 0.044(2) -0.0092(18) 0.0023(17) -0.0015(17) _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 Pt P1 2.2837(9) . ? Pt P2 2.2952(9) . ? Pt S1 2.3213(9) . ? Pt S2 2.3546(9) . ? S1 C1 1.747(4) . ? S2 C1 1.751(4) . ? S3 O1 1.436(3) . ? S3 O2 1.439(3) . ? S3 N 1.648(3) . ? S3 C2 1.769(4) . ? P1 C15 1.811(4) . ? P1 C21 1.824(4) . ? P1 C9 1.836(4) . ? P2 C33 1.823(3) . ? P2 C39 1.830(3) . ? P2 C27 1.833(4) . ? N C1 1.301(4) . ? C2 C7 1.383(5) . ? C2 C3 1.396(5) . ? C3 C4 1.384(6) . ? C3 H3 0.9500 . ? C4 C5 1.390(6) . ? C4 H4 0.9500 . ? C5 C6 1.381(6) . ? C5 C8 1.514(6) . ? C6 C7 1.393(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10A 1.32(2) . ? C9 C14A 1.33(3) . ? C9 C14 1.40(2) . ? C9 C10 1.41(2) . ? C10 C11 1.34(3) . ? C10 H10 0.9500 . ? C11 C12 1.27(2) . ? C11 H11 0.9500 . ? C13 C14 1.32(3) . ? C13 C12 1.40(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C10A C11A 1.44(3) . ? C10A H10A 0.9500 . ? C11A C12 1.470(19) . ? C11A H11A 0.9500 . ? C13A C12 1.31(2) . ? C13A C14A 1.47(3) . ? C13A H13A 0.9500 . ? C14A H14A 0.9500 . ? C12 H12 0.9500 . ? C15 C20 1.380(6) . ? C15 C16 1.387(5) . ? C16 C17 1.386(6) . ? C16 H16 0.9500 . ? C17 C18 1.359(6) . ? C17 H17 0.9500 . ? C18 C19 1.342(6) . ? C18 H18 0.9500 . ? C19 C20 1.383(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.378(6) . ? C21 C22 1.389(5) . ? C22 C23 1.387(5) . ? C22 H22 0.9500 . ? C23 C24 1.373(7) . ? C23 H23 0.9500 . ? C24 C25 1.361(8) . ? C24 H24 0.9500 . ? C25 C26 1.404(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.390(5) . ? C27 C28 1.396(5) . ? C28 C29 1.382(5) . ? C28 H28 0.9500 . ? C29 C30 1.378(6) . ? C29 H29 0.9500 . ? C30 C31 1.364(6) . ? C30 H30 0.9500 . ? C31 C32 1.385(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.391(5) . ? C33 C38 1.402(5) . ? C34 C35 1.385(5) . ? C34 H34 0.9500 . ? C35 C36 1.387(5) . ? C35 H35 0.9500 . ? C36 C37 1.382(6) . ? C36 H36 0.9500 . ? C37 C38 1.386(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.382(5) . ? C39 C44 1.391(5) . ? C40 C41 1.391(6) . ? C40 H40 0.9500 . ? C41 C42 1.377(7) . ? C41 H41 0.9500 . ? C42 C43 1.368(7) . ? C42 H42 0.9500 . ? C43 C44 1.392(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? 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 P1 Pt P2 97.82(3) . . ? P1 Pt S1 92.90(3) . . ? P2 Pt S1 168.47(3) . . ? P1 Pt S2 166.35(3) . . ? P2 Pt S2 94.89(3) . . ? S1 Pt S2 74.85(3) . . ? C1 S1 Pt 88.82(12) . . ? C1 S2 Pt 87.65(12) . . ? O1 S3 O2 117.98(17) . . ? O1 S3 N 104.69(16) . . ? O2 S3 N 111.03(16) . . ? O1 S3 C2 107.42(17) . . ? O2 S3 C2 107.31(18) . . ? N S3 C2 108.02(16) . . ? C15 P1 C21 113.69(18) . . ? C15 P1 C9 101.36(17) . . ? C21 P1 C9 101.96(16) . . ? C15 P1 Pt 110.63(12) . . ? C21 P1 Pt 113.89(12) . . ? C9 P1 Pt 114.44(11) . . ? C33 P2 C39 106.33(16) . . ? C33 P2 C27 104.31(16) . . ? C39 P2 C27 102.92(16) . . ? C33 P2 Pt 112.14(12) . . ? C39 P2 Pt 112.66(12) . . ? C27 P2 Pt 117.42(12) . . ? C1 N S3 121.2(3) . . ? N C1 S1 130.6(3) . . ? N C1 S2 120.7(3) . . ? S1 C1 S2 108.67(19) . . ? C7 C2 C3 119.6(4) . . ? C7 C2 S3 121.3(3) . . ? C3 C2 S3 119.1(3) . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.8(4) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 118.9(4) . . ? C6 C5 C8 120.8(4) . . ? C4 C5 C8 120.3(4) . . ? C5 C6 C7 121.0(4) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 119.9(4) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10A C9 C14A 122.2(14) . . ? C10A C9 C14 115.7(14) . . ? C14A C9 C10 112.3(14) . . ? C14 C9 C10 113.9(13) . . ? C10A C9 P1 117.3(10) . . ? C14A C9 P1 120.4(11) . . ? C14 C9 P1 122.2(9) . . ? C10 C9 P1 123.8(10) . . ? C11 C10 C9 120.3(18) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 124.9(19) . . ? C12 C11 H11 117.6 . . ? C10 C11 H11 117.6 . . ? C14 C13 C12 121.8(13) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C9 121.8(15) . . ? C13 C14 H14 119.1 . . ? C9 C14 H14 119.1 . . ? C9 C10A C11A 121.4(18) . . ? C9 C10A H10A 119.3 . . ? C11A C10A H10A 119.3 . . ? C10A C11A C12 116.5(16) . . ? C10A C11A H11A 121.8 . . ? C12 C11A H11A 121.8 . . ? C12 C13A C14A 119.7(19) . . ? C12 C13A H13A 120.1 . . ? C14A C13A H13A 120.1 . . ? C9 C14A C13A 120.1(19) . . ? C9 C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C11 C12 C13A 114.4(13) . . ? C11 C12 C13 116.8(12) . . ? C13A C12 C11A 120.1(13) . . ? C13 C12 C11A 113.6(11) . . ? C11 C12 H12 121.6 . . ? C13A C12 H12 119.9 . . ? C13 C12 H12 121.6 . . ? C11A C12 H12 120.0 . . ? C20 C15 C16 116.6(4) . . ? C20 C15 P1 124.9(3) . . ? C16 C15 P1 117.6(3) . . ? C17 C16 C15 120.9(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 119.5(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.7(4) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C15 C20 C19 121.6(4) . . ? C15 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C26 C21 C22 119.1(4) . . ? C26 C21 P1 125.5(3) . . ? C22 C21 P1 115.3(3) . . ? C23 C22 C21 120.8(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 119.8(4) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 121.1(5) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C21 C26 C25 119.3(5) . . ? C21 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C32 C27 C28 118.6(3) . . ? C32 C27 P2 122.4(3) . . ? C28 C27 P2 118.7(3) . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 120.0(4) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 121.0(4) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C31 C32 C27 120.0(4) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C34 C33 C38 118.9(3) . . ? C34 C33 P2 122.2(3) . . ? C38 C33 P2 118.8(3) . . ? C35 C34 C33 120.6(3) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 119.7(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C36 C35 120.4(4) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 119.9(4) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C33 120.3(4) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? C40 C39 C44 118.3(3) . . ? C40 C39 P2 122.9(3) . . ? C44 C39 P2 118.6(3) . . ? C39 C40 C41 120.9(4) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 119.9(4) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C43 C42 C41 120.2(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C39 C44 C43 120.6(4) . . ? C39 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.957 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.101