# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Derek Woollins' 'Stephen M. Aucott' 'Pravat Bhattacharyya' 'Heather L. Milton' 'Alexandra M. Z. Slawin' _publ_contact_author_name 'Prof Derek Woollins' _publ_contact_author_address ; Prof Derek Woollins School of Chemistry University of St Andrews St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email JDW3@ST-AND.AC.UK _publ_section_title ; N-Metallation of MS2N2 Rings. X-ray Crystal Structures of [(h5-C5Me5)Ir(S2N2)Au(PPh3)][ClO4], [{(h5-C5H5)Co(S2N2)Au}2(m2-dppm)][ClO4]2 [{(h5-C5Me5)Ir(S2N2)Au}2(m2-dppm)][ClO4]2 and [Au(dppeS-P)Cl]2. ; data_0 _database_code_CSD 213795 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Au(dppeS-P)Cl]2 ; _chemical_name_common - _chemical_melting_point - _chemical_formula_moiety 'C52 H48 Au2 Cl2 P4 S2' _chemical_formula_sum 'C52 H48 Au2 Cl2 P4 S2' _chemical_formula_weight 1325.74 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' Au Au -2.0133 8.8022 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0993(8) _cell_length_b 13.0681(10) _cell_length_c 19.3948(14) _cell_angle_alpha 84.7350(10) _cell_angle_beta 76.4830(10) _cell_angle_gamma 64.9000(10) _cell_volume 2476.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour colOurless _exptl_crystal_size_max .18 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 6.273 _exptl_absorpt_correction_type MULTISCAN _exptl_absorpt_correction_T_min 0.647074 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details - _exptl_special_details ; - ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 12636 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 23.36 _reflns_number_total 7038 _reflns_number_gt 5031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00047(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7038 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _refine_ls_shift/su_max 0.005 _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 Au1 Au -0.26463(3) -0.07209(3) 0.164476(16) 0.02326(12) Uani 1 1 d . . . Cl1 Cl -0.4432(2) -0.0174(2) 0.10894(11) 0.0330(5) Uani 1 1 d . . . P1 P -0.0909(2) -0.11004(19) 0.21744(11) 0.0209(5) Uani 1 1 d . . . C1 C -0.1417(7) -0.0554(7) 0.3085(4) 0.022(2) Uani 1 1 d . . . C2 C -0.0616(8) -0.1040(8) 0.3573(4) 0.030(2) Uani 1 1 d . . . H2A H 0.0170 -0.1733 0.3466 0.036 Uiso 1 1 calc R . . C3 C -0.0969(9) -0.0511(8) 0.4221(5) 0.036(2) Uani 1 1 d . . . H3A H -0.0415 -0.0837 0.4559 0.044 Uiso 1 1 calc R . . C4 C -0.2105(9) 0.0476(9) 0.4378(5) 0.039(3) Uani 1 1 d . . . H4A H -0.2331 0.0835 0.4824 0.047 Uiso 1 1 calc R . . C5 C -0.2929(8) 0.0959(8) 0.3900(4) 0.033(2) Uani 1 1 d . . . H5A H -0.3715 0.1650 0.4011 0.040 Uiso 1 1 calc R . . C6 C -0.2595(8) 0.0421(8) 0.3251(4) 0.028(2) Uani 1 1 d . . . H6A H -0.3176 0.0725 0.2925 0.033 Uiso 1 1 calc R . . C7 C 0.0189(8) -0.0428(7) 0.1706(4) 0.023(2) Uani 1 1 d . . . C8 C 0.0059(8) 0.0031(7) 0.1044(4) 0.026(2) Uani 1 1 d . . . H8A H -0.0610 -0.0006 0.0830 0.031 Uiso 1 1 calc R . . C9 C 0.0885(8) 0.0543(7) 0.0686(4) 0.032(2) Uani 1 1 d . . . H9A H 0.0791 0.0848 0.0228 0.039 Uiso 1 1 calc R . . C10 C 0.1847(9) 0.0610(8) 0.0997(5) 0.036(2) Uani 1 1 d . . . H10A H 0.2413 0.0966 0.0754 0.043 Uiso 1 1 calc R . . C11 C 0.1988(8) 0.0163(8) 0.1657(5) 0.034(2) Uani 1 1 d . . . H11A H 0.2658 0.0207 0.1866 0.040 Uiso 1 1 calc R . . C12 C 0.1163(8) -0.0352(8) 0.2022(5) 0.032(2) Uani 1 1 d . . . H12A H 0.1257 -0.0649 0.2482 0.038 Uiso 1 1 calc R . . S2 S 0.1993(2) -0.4506(2) 0.33666(11) 0.0293(6) Uani 1 1 d . . . P2 P 0.0690(2) -0.46447(19) 0.28946(10) 0.0196(5) Uani 1 1 d . . . C13 C 0.1499(7) -0.5448(7) 0.2077(4) 0.021(2) Uani 1 1 d . . . C14 C 0.0771(8) -0.5420(7) 0.1579(4) 0.027(2) Uani 1 1 d . . . H14A H -0.0175 -0.4941 0.1658 0.032 Uiso 1 1 calc R . . C15 C 0.1404(9) -0.6084(8) 0.0965(4) 0.036(3) Uani 1 1 d . . . H15A H 0.0900 -0.6040 0.0620 0.043 Uiso 1 1 calc R . . C16 C 0.2779(9) -0.6809(8) 0.0862(5) 0.037(2) Uani 1 1 d . . . H16A H 0.3211 -0.7288 0.0455 0.044 Uiso 1 1 calc R . . C17 C 0.3511(8) -0.6832(7) 0.1349(5) 0.031(2) Uani 1 1 d . . . H17A H 0.4458 -0.7308 0.1267 0.037 Uiso 1 1 calc R . . C18 C 0.2887(8) -0.6172(7) 0.1960(4) 0.027(2) Uani 1 1 d . . . H18A H 0.3401 -0.6212 0.2299 0.033 Uiso 1 1 calc R . . C19 C -0.0368(7) -0.5291(7) 0.3451(4) 0.022(2) Uani 1 1 d . . . C20 C -0.0241(8) -0.5553(7) 0.4151(4) 0.027(2) Uani 1 1 d . . . H20A H 0.0368 -0.5377 0.4338 0.032 Uiso 1 1 calc R . . C21 C -0.1009(8) -0.6072(7) 0.4573(4) 0.033(2) Uani 1 1 d . . . H21A H -0.0911 -0.6262 0.5047 0.039 Uiso 1 1 calc R . . C22 C -0.1912(8) -0.6316(8) 0.4314(4) 0.035(2) Uani 1 1 d . . . H22A H -0.2448 -0.6656 0.4612 0.043 Uiso 1 1 calc R . . C23 C -0.2036(9) -0.6071(9) 0.3627(5) 0.041(3) Uani 1 1 d . . . H23A H -0.2652 -0.6247 0.3448 0.050 Uiso 1 1 calc R . . C24 C -0.1263(8) -0.5562(8) 0.3190(4) 0.035(2) Uani 1 1 d . . . H24A H -0.1347 -0.5400 0.2711 0.042 Uiso 1 1 calc R . . C25 C 0.0204(8) -0.2589(7) 0.2214(4) 0.0220(19) Uani 1 1 d . . . H25A H 0.0588 -0.2902 0.1725 0.026 Uiso 1 1 calc R . . H25B H 0.0971 -0.2667 0.2423 0.026 Uiso 1 1 calc R . . C26 C -0.0524(7) -0.3278(7) 0.2650(4) 0.025(2) Uani 1 1 d . . . H26A H -0.1096 -0.3399 0.2372 0.030 Uiso 1 1 calc R . . H26B H -0.1130 -0.2850 0.3086 0.030 Uiso 1 1 calc R . . Au2 Au -0.23114(3) -0.30676(3) 0.099658(16) 0.02065(11) Uani 1 1 d . . . Cl2 Cl -0.03224(19) -0.29104(19) 0.04561(10) 0.0287(5) Uani 1 1 d . . . P3 P -0.41060(19) -0.34535(19) 0.14835(10) 0.0194(5) Uani 1 1 d . . . C31 C -0.3550(7) -0.4917(7) 0.1743(4) 0.022(2) Uani 1 1 d . . . C32 C -0.4323(8) -0.5321(8) 0.2274(4) 0.027(2) Uani 1 1 d . . . H32A H -0.5180 -0.4806 0.2531 0.033 Uiso 1 1 calc R . . C33 C -0.3865(9) -0.6449(9) 0.2432(5) 0.035(2) Uani 1 1 d . . . H33A H -0.4411 -0.6712 0.2790 0.042 Uiso 1 1 calc R . . C34 C -0.2606(9) -0.7208(8) 0.2070(5) 0.040(2) Uani 1 1 d . . . H34A H -0.2281 -0.7986 0.2189 0.048 Uiso 1 1 calc R . . C35 C -0.1828(9) -0.6836(9) 0.1542(5) 0.036(2) Uani 1 1 d . . . H35A H -0.0976 -0.7359 0.1286 0.043 Uiso 1 1 calc R . . C36 C -0.2288(8) -0.5703(8) 0.1383(4) 0.030(2) Uani 1 1 d . . . H36A H -0.1738 -0.5450 0.1021 0.036 Uiso 1 1 calc R . . C37 C -0.5254(7) -0.3252(7) 0.0911(4) 0.020(2) Uani 1 1 d . . . C38 C -0.5651(7) -0.2256(7) 0.0521(4) 0.021(2) Uani 1 1 d . . . H38A H -0.5286 -0.1725 0.0548 0.026 Uiso 1 1 calc R . . C39 C -0.6575(8) -0.2035(8) 0.0094(4) 0.026(2) Uani 1 1 d . . . H39A H -0.6838 -0.1359 -0.0174 0.031 Uiso 1 1 calc R . . C40 C -0.7111(8) -0.2807(9) 0.0061(4) 0.034(2) Uani 1 1 d . . . H40A H -0.7737 -0.2663 -0.0235 0.041 Uiso 1 1 calc R . . C41 C -0.6749(9) -0.3769(9) 0.0447(5) 0.036(2) Uani 1 1 d . . . H41A H -0.7144 -0.4283 0.0431 0.043 Uiso 1 1 calc R . . C42 C -0.5817(8) -0.4005(8) 0.0861(4) 0.029(2) Uani 1 1 d . . . H42A H -0.5552 -0.4693 0.1118 0.035 Uiso 1 1 calc R . . S4 S -0.7074(2) -0.2638(2) 0.39560(11) 0.0299(6) Uani 1 1 d . . . P4 P -0.57059(19) -0.20151(19) 0.36733(10) 0.0199(5) Uani 1 1 d . . . C43 C -0.6442(7) -0.0529(7) 0.3484(4) 0.020(2) Uani 1 1 d . . . C44 C -0.5685(8) 0.0034(8) 0.3090(4) 0.028(2) Uani 1 1 d . . . H44A H -0.4726 -0.0369 0.2938 0.034 Uiso 1 1 calc R . . C45 C -0.6290(9) 0.1156(8) 0.2915(5) 0.035(2) Uani 1 1 d . . . H45A H -0.5753 0.1521 0.2648 0.042 Uiso 1 1 calc R . . C46 C -0.7664(10) 0.1739(9) 0.3128(5) 0.045(3) Uani 1 1 d . . . H46A H -0.8096 0.2511 0.3005 0.053 Uiso 1 1 calc R . . C47 C -0.8434(9) 0.1191(9) 0.3530(5) 0.040(3) Uani 1 1 d . . . H47A H -0.9389 0.1604 0.3691 0.048 Uiso 1 1 calc R . . C48 C -0.7851(8) 0.0096(8) 0.3694(4) 0.027(2) Uani 1 1 d . . . H48A H -0.8401 -0.0262 0.3955 0.033 Uiso 1 1 calc R . . C49 C -0.4684(7) -0.2241(7) 0.4330(4) 0.022(2) Uani 1 1 d . . . C50 C -0.4217(9) -0.1481(9) 0.4474(5) 0.041(3) Uani 1 1 d . . . H50A H -0.4402 -0.0795 0.4218 0.049 Uiso 1 1 calc R . . C51 C -0.3461(9) -0.1731(11) 0.5005(5) 0.049(3) Uani 1 1 d . . . H51A H -0.3149 -0.1203 0.5113 0.059 Uiso 1 1 calc R . . C52 C -0.3174(9) -0.2713(11) 0.5363(5) 0.053(3) Uani 1 1 d . . . H52A H -0.2652 -0.2870 0.5715 0.064 Uiso 1 1 calc R . . C53 C -0.3630(9) -0.3498(9) 0.5224(5) 0.049(3) Uani 1 1 d . . . H53A H -0.3427 -0.4185 0.5480 0.059 Uiso 1 1 calc R . . C54 C -0.4377(9) -0.3264(8) 0.4715(5) 0.039(2) Uani 1 1 d . . . H54A H -0.4693 -0.3795 0.4617 0.046 Uiso 1 1 calc R . . C55 C -0.5196(7) -0.2623(7) 0.2269(4) 0.023(2) Uani 1 1 d . . . H55A H -0.5628 -0.1823 0.2129 0.028 Uiso 1 1 calc R . . H55B H -0.5932 -0.2877 0.2455 0.028 Uiso 1 1 calc R . . C56 C -0.4485(7) -0.2686(7) 0.2860(4) 0.0195(19) Uani 1 1 d . . . H56A H -0.3861 -0.2307 0.2708 0.023 Uiso 1 1 calc R . . H56B H -0.3932 -0.3488 0.2954 0.023 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 Au1 0.02168(19) 0.0247(2) 0.0239(2) -0.00106(16) -0.00594(14) -0.00930(17) Cl1 0.0294(11) 0.0340(15) 0.0402(13) 0.0031(11) -0.0156(10) -0.0141(11) P1 0.0203(11) 0.0237(15) 0.0188(11) -0.0020(10) -0.0032(9) -0.0092(10) C1 0.020(4) 0.023(6) 0.022(5) -0.006(4) 0.005(4) -0.011(4) C2 0.024(5) 0.045(7) 0.022(5) -0.006(4) -0.005(4) -0.014(4) C3 0.033(5) 0.051(7) 0.028(5) -0.003(5) -0.006(4) -0.020(5) C4 0.042(6) 0.048(8) 0.027(5) -0.018(5) 0.006(5) -0.023(6) C5 0.029(5) 0.028(6) 0.028(5) -0.009(4) 0.008(4) -0.004(4) C6 0.021(4) 0.038(6) 0.023(5) -0.003(4) 0.001(4) -0.012(4) C7 0.026(4) 0.013(5) 0.026(5) -0.003(4) 0.003(4) -0.009(4) C8 0.026(4) 0.022(6) 0.027(5) -0.007(4) -0.001(4) -0.010(4) C9 0.038(5) 0.022(6) 0.024(5) -0.003(4) 0.004(4) -0.005(5) C10 0.041(6) 0.035(7) 0.036(6) -0.003(5) 0.003(4) -0.025(5) C11 0.022(5) 0.034(7) 0.042(6) -0.014(5) 0.004(4) -0.012(4) C12 0.025(5) 0.035(7) 0.034(5) -0.003(4) -0.006(4) -0.012(5) S2 0.0348(12) 0.0377(16) 0.0195(11) -0.0047(10) -0.0054(9) -0.0182(12) P2 0.0215(11) 0.0201(14) 0.0154(11) -0.0019(9) -0.0052(9) -0.0058(10) C13 0.017(4) 0.025(6) 0.019(4) -0.002(4) 0.000(3) -0.008(4) C14 0.019(4) 0.023(6) 0.033(5) -0.010(4) -0.003(4) -0.003(4) C15 0.041(6) 0.056(8) 0.019(5) -0.016(5) 0.002(4) -0.029(5) C16 0.036(5) 0.046(7) 0.028(5) -0.014(5) 0.003(4) -0.019(5) C17 0.018(4) 0.019(6) 0.044(6) -0.009(4) 0.010(4) -0.003(4) C18 0.022(4) 0.030(6) 0.025(5) 0.002(4) -0.001(4) -0.008(4) C19 0.020(4) 0.013(5) 0.024(5) -0.003(4) -0.001(4) 0.000(4) C20 0.035(5) 0.027(6) 0.020(5) -0.002(4) -0.008(4) -0.014(4) C21 0.042(5) 0.024(6) 0.023(5) -0.003(4) 0.000(4) -0.009(5) C22 0.039(5) 0.049(7) 0.021(5) 0.002(5) 0.005(4) -0.026(5) C23 0.033(5) 0.061(8) 0.039(6) 0.010(5) -0.007(4) -0.031(5) C24 0.045(5) 0.045(7) 0.022(5) 0.006(4) -0.013(4) -0.024(5) C25 0.029(5) 0.014(5) 0.025(5) 0.007(4) -0.012(4) -0.008(4) C26 0.013(4) 0.036(6) 0.024(5) -0.009(4) -0.004(3) -0.007(4) Au2 0.01986(18) 0.0268(2) 0.01709(19) -0.00184(15) -0.00247(13) -0.01174(17) Cl2 0.0274(11) 0.0395(15) 0.0233(11) 0.0022(10) -0.0010(9) -0.0205(11) P3 0.0158(10) 0.0252(15) 0.0166(11) -0.0054(10) 0.0000(8) -0.0088(10) C31 0.022(4) 0.027(6) 0.024(5) -0.001(4) -0.010(4) -0.014(4) C32 0.026(5) 0.029(7) 0.029(5) 0.000(4) -0.005(4) -0.015(4) C33 0.037(5) 0.045(8) 0.029(5) 0.007(5) -0.008(4) -0.023(5) C34 0.057(6) 0.026(7) 0.039(6) -0.003(5) -0.016(5) -0.015(5) C35 0.032(5) 0.029(7) 0.037(6) -0.003(5) -0.011(4) 0.000(5) C36 0.019(4) 0.042(7) 0.030(5) -0.019(5) -0.001(4) -0.013(5) C37 0.014(4) 0.035(6) 0.015(4) -0.003(4) -0.001(3) -0.014(4) C38 0.025(4) 0.023(6) 0.017(4) -0.004(4) 0.000(4) -0.012(4) C39 0.029(5) 0.024(6) 0.020(5) -0.001(4) -0.002(4) -0.009(4) C40 0.033(5) 0.054(8) 0.022(5) -0.005(5) -0.009(4) -0.020(5) C41 0.040(5) 0.045(7) 0.031(6) -0.002(5) -0.014(4) -0.022(5) C42 0.026(5) 0.028(6) 0.029(5) 0.002(4) -0.006(4) -0.006(4) S4 0.0367(12) 0.0343(16) 0.0266(12) 0.0016(10) -0.0079(10) -0.0219(12) P4 0.0180(11) 0.0250(15) 0.0145(11) -0.0026(9) -0.0018(8) -0.0074(10) C43 0.025(4) 0.027(6) 0.013(4) -0.011(4) 0.001(3) -0.015(4) C44 0.027(5) 0.019(6) 0.030(5) -0.005(4) 0.008(4) -0.007(4) C45 0.038(6) 0.025(7) 0.040(6) -0.002(5) -0.003(4) -0.013(5) C46 0.066(7) 0.023(7) 0.043(6) 0.002(5) -0.022(5) -0.013(6) C47 0.030(5) 0.037(8) 0.037(6) -0.004(5) 0.000(4) -0.002(5) C48 0.029(5) 0.030(7) 0.012(4) 0.002(4) 0.000(4) -0.006(5) C49 0.018(4) 0.023(6) 0.019(5) -0.006(4) 0.000(4) -0.005(4) C50 0.043(5) 0.056(8) 0.032(5) -0.001(5) -0.006(4) -0.031(6) C51 0.044(6) 0.069(10) 0.045(7) -0.017(6) -0.006(5) -0.031(6) C52 0.035(6) 0.082(10) 0.033(6) -0.014(6) -0.020(5) -0.006(6) C53 0.054(6) 0.050(8) 0.033(6) -0.007(5) -0.023(5) -0.004(6) C54 0.053(6) 0.024(7) 0.035(6) -0.005(5) -0.022(5) -0.004(5) C55 0.013(4) 0.023(6) 0.023(5) -0.004(4) -0.001(3) 0.002(4) C56 0.018(4) 0.019(5) 0.020(4) -0.010(4) 0.000(3) -0.006(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 Au1 P1 2.245(2) . ? Au1 Cl1 2.292(2) . ? Au1 Au2 3.2626(5) . ? P1 C25 1.815(8) . ? P1 C7 1.824(8) . ? P1 C1 1.835(8) . ? C1 C2 1.377(11) . ? C1 C6 1.380(11) . ? C2 C3 1.382(11) . ? C3 C4 1.364(12) . ? C4 C5 1.377(12) . ? C5 C6 1.392(11) . ? C7 C8 1.379(11) . ? C7 C12 1.403(11) . ? C8 C9 1.382(11) . ? C9 C10 1.379(12) . ? C10 C11 1.371(13) . ? C11 C12 1.387(11) . ? S2 P2 1.958(3) . ? P2 C13 1.807(7) . ? P2 C26 1.825(9) . ? P2 C19 1.827(8) . ? C13 C14 1.385(10) . ? C13 C18 1.400(10) . ? C14 C15 1.396(10) . ? C15 C16 1.390(12) . ? C16 C17 1.374(11) . ? C17 C18 1.387(11) . ? C19 C24 1.393(11) . ? C19 C20 1.394(11) . ? C20 C21 1.385(11) . ? C21 C22 1.376(11) . ? C22 C23 1.365(12) . ? C23 C24 1.392(11) . ? C25 C26 1.529(11) . ? Au2 P3 2.2359(19) . ? Au2 Cl2 2.2974(17) . ? P3 C37 1.802(7) . ? P3 C31 1.806(9) . ? P3 C55 1.813(7) . ? C31 C36 1.400(10) . ? C31 C32 1.395(10) . ? C32 C33 1.371(12) . ? C33 C34 1.386(12) . ? C34 C35 1.372(12) . ? C35 C36 1.377(12) . ? C37 C42 1.392(11) . ? C37 C38 1.396(11) . ? C38 C39 1.386(10) . ? C39 C40 1.384(11) . ? C40 C41 1.358(13) . ? C41 C42 1.372(11) . ? S4 P4 1.961(3) . ? P4 C43 1.799(9) . ? P4 C49 1.822(8) . ? P4 C56 1.828(7) . ? C43 C44 1.397(10) . ? C43 C48 1.399(10) . ? C44 C45 1.377(12) . ? C45 C46 1.362(12) . ? C46 C47 1.399(12) . ? C47 C48 1.340(12) . ? C49 C50 1.374(11) . ? C49 C54 1.417(12) . ? C50 C51 1.407(13) . ? C51 C52 1.350(14) . ? C52 C53 1.391(14) . ? C53 C54 1.367(12) . ? C55 C56 1.515(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 174.93(8) . . ? P1 Au1 Au2 108.71(6) . . ? Cl1 Au1 Au2 75.86(6) . . ? C25 P1 C7 105.6(4) . . ? C25 P1 C1 106.1(4) . . ? C7 P1 C1 103.8(3) . . ? C25 P1 Au1 114.9(3) . . ? C7 P1 Au1 110.7(3) . . ? C1 P1 Au1 114.7(3) . . ? C2 C1 C6 120.5(7) . . ? C2 C1 P1 122.0(6) . . ? C6 C1 P1 117.3(7) . . ? C1 C2 C3 119.3(9) . . ? C4 C3 C2 120.5(9) . . ? C3 C4 C5 120.8(8) . . ? C4 C5 C6 119.2(8) . . ? C1 C6 C5 119.7(8) . . ? C8 C7 C12 119.0(7) . . ? C8 C7 P1 120.7(6) . . ? C12 C7 P1 120.2(6) . . ? C7 C8 C9 121.0(8) . . ? C10 C9 C8 119.7(8) . . ? C11 C10 C9 120.1(8) . . ? C10 C11 C12 120.8(8) . . ? C11 C12 C7 119.3(8) . . ? C13 P2 C26 105.3(4) . . ? C13 P2 C19 107.6(3) . . ? C26 P2 C19 104.6(3) . . ? C13 P2 S2 112.9(3) . . ? C26 P2 S2 112.6(3) . . ? C19 P2 S2 113.2(3) . . ? C14 C13 C18 118.8(7) . . ? C14 C13 P2 122.0(6) . . ? C18 C13 P2 119.1(6) . . ? C13 C14 C15 121.1(7) . . ? C16 C15 C14 119.3(8) . . ? C17 C16 C15 119.9(8) . . ? C16 C17 C18 121.0(8) . . ? C17 C18 C13 119.8(8) . . ? C24 C19 C20 119.1(7) . . ? C24 C19 P2 121.9(6) . . ? C20 C19 P2 119.0(6) . . ? C21 C20 C19 119.5(8) . . ? C22 C21 C20 121.0(8) . . ? C23 C22 C21 119.9(8) . . ? C22 C23 C24 120.3(8) . . ? C23 C24 C19 120.2(8) . . ? C26 C25 P1 113.0(5) . . ? C25 C26 P2 111.4(5) . . ? P3 Au2 Cl2 172.69(8) . . ? P3 Au2 Au1 110.80(5) . . ? Cl2 Au2 Au1 76.11(5) . . ? C37 P3 C31 105.2(4) . . ? C37 P3 C55 104.1(3) . . ? C31 P3 C55 106.5(4) . . ? C37 P3 Au2 115.2(2) . . ? C31 P3 Au2 110.4(2) . . ? C55 P3 Au2 114.6(3) . . ? C36 C31 C32 117.6(8) . . ? C36 C31 P3 118.6(6) . . ? C32 C31 P3 123.8(6) . . ? C33 C32 C31 121.1(8) . . ? C32 C33 C34 120.1(8) . . ? C35 C34 C33 120.1(9) . . ? C34 C35 C36 119.8(8) . . ? C35 C36 C31 121.3(8) . . ? C42 C37 C38 118.1(7) . . ? C42 C37 P3 123.8(7) . . ? C38 C37 P3 118.0(6) . . ? C39 C38 C37 120.5(7) . . ? C40 C39 C38 119.4(8) . . ? C41 C40 C39 120.6(8) . . ? C40 C41 C42 120.4(9) . . ? C41 C42 C37 120.9(9) . . ? C43 P4 C49 108.4(4) . . ? C43 P4 C56 105.5(4) . . ? C49 P4 C56 105.3(3) . . ? C43 P4 S4 112.7(3) . . ? C49 P4 S4 113.1(3) . . ? C56 P4 S4 111.3(3) . . ? C44 C43 C48 117.1(8) . . ? C44 C43 P4 123.1(6) . . ? C48 C43 P4 119.6(6) . . ? C45 C44 C43 121.8(8) . . ? C46 C45 C44 119.5(9) . . ? C45 C46 C47 119.3(10) . . ? C48 C47 C46 121.3(9) . . ? C47 C48 C43 120.9(8) . . ? C50 C49 C54 119.1(8) . . ? C50 C49 P4 124.0(7) . . ? C54 C49 P4 116.9(6) . . ? C49 C50 C51 119.2(10) . . ? C52 C51 C50 120.7(10) . . ? C51 C52 C53 121.1(10) . . ? C54 C53 C52 119.0(11) . . ? C53 C54 C49 120.8(9) . . ? C56 C55 P3 115.1(5) . . ? C55 C56 P4 111.5(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 Cl1 Au1 P1 C25 -159.5(8) . . . . ? Au2 Au1 P1 C25 -5.5(3) . . . . ? Cl1 Au1 P1 C7 -40.0(9) . . . . ? Au2 Au1 P1 C7 114.1(3) . . . . ? Cl1 Au1 P1 C1 77.1(9) . . . . ? Au2 Au1 P1 C1 -128.8(3) . . . . ? C25 P1 C1 C2 26.4(7) . . . . ? C7 P1 C1 C2 -84.6(7) . . . . ? Au1 P1 C1 C2 154.4(6) . . . . ? C25 P1 C1 C6 -158.1(6) . . . . ? C7 P1 C1 C6 90.8(7) . . . . ? Au1 P1 C1 C6 -30.1(7) . . . . ? C6 C1 C2 C3 -3.2(12) . . . . ? P1 C1 C2 C3 172.1(6) . . . . ? C1 C2 C3 C4 0.7(13) . . . . ? C2 C3 C4 C5 0.6(14) . . . . ? C3 C4 C5 C6 0.5(13) . . . . ? C2 C1 C6 C5 4.3(12) . . . . ? P1 C1 C6 C5 -171.2(6) . . . . ? C4 C5 C6 C1 -3.0(12) . . . . ? C25 P1 C7 C8 112.8(7) . . . . ? C1 P1 C7 C8 -135.8(7) . . . . ? Au1 P1 C7 C8 -12.2(7) . . . . ? C25 P1 C7 C12 -68.4(7) . . . . ? C1 P1 C7 C12 43.0(7) . . . . ? Au1 P1 C7 C12 166.6(6) . . . . ? C12 C7 C8 C9 1.1(12) . . . . ? P1 C7 C8 C9 179.9(6) . . . . ? C7 C8 C9 C10 -0.7(12) . . . . ? C8 C9 C10 C11 0.4(13) . . . . ? C9 C10 C11 C12 -0.5(13) . . . . ? C10 C11 C12 C7 0.9(13) . . . . ? C8 C7 C12 C11 -1.2(12) . . . . ? P1 C7 C12 C11 -180.0(6) . . . . ? C26 P2 C13 C14 -40.8(8) . . . . ? C19 P2 C13 C14 70.3(8) . . . . ? S2 P2 C13 C14 -164.1(6) . . . . ? C26 P2 C13 C18 143.0(7) . . . . ? C19 P2 C13 C18 -105.9(7) . . . . ? S2 P2 C13 C18 19.7(7) . . . . ? C18 C13 C14 C15 -1.0(13) . . . . ? P2 C13 C14 C15 -177.3(7) . . . . ? C13 C14 C15 C16 1.9(13) . . . . ? C14 C15 C16 C17 -2.6(14) . . . . ? C15 C16 C17 C18 2.5(14) . . . . ? C16 C17 C18 C13 -1.6(13) . . . . ? C14 C13 C18 C17 0.9(12) . . . . ? P2 C13 C18 C17 177.2(6) . . . . ? C13 P2 C19 C24 -48.2(8) . . . . ? C26 P2 C19 C24 63.4(8) . . . . ? S2 P2 C19 C24 -173.7(6) . . . . ? C13 P2 C19 C20 129.6(6) . . . . ? C26 P2 C19 C20 -118.8(7) . . . . ? S2 P2 C19 C20 4.1(7) . . . . ? C24 C19 C20 C21 -0.3(12) . . . . ? P2 C19 C20 C21 -178.2(6) . . . . ? C19 C20 C21 C22 -1.0(13) . . . . ? C20 C21 C22 C23 1.5(14) . . . . ? C21 C22 C23 C24 -0.7(15) . . . . ? C22 C23 C24 C19 -0.6(15) . . . . ? C20 C19 C24 C23 1.1(13) . . . . ? P2 C19 C24 C23 178.9(7) . . . . ? C7 P1 C25 C26 174.8(5) . . . . ? C1 P1 C25 C26 65.0(6) . . . . ? Au1 P1 C25 C26 -62.8(6) . . . . ? P1 C25 C26 P2 -163.2(4) . . . . ? C13 P2 C26 C25 -70.1(6) . . . . ? C19 P2 C26 C25 176.6(5) . . . . ? S2 P2 C26 C25 53.3(6) . . . . ? P1 Au1 Au2 P3 119.45(8) . . . . ? Cl1 Au1 Au2 P3 -62.83(8) . . . . ? P1 Au1 Au2 Cl2 -58.06(8) . . . . ? Cl1 Au1 Au2 Cl2 119.66(8) . . . . ? Cl2 Au2 P3 C37 -92.0(7) . . . . ? Au1 Au2 P3 C37 107.4(3) . . . . ? Cl2 Au2 P3 C31 26.9(7) . . . . ? Au1 Au2 P3 C31 -133.7(3) . . . . ? Cl2 Au2 P3 C55 147.1(6) . . . . ? Au1 Au2 P3 C55 -13.5(3) . . . . ? C37 P3 C31 C36 98.6(6) . . . . ? C55 P3 C31 C36 -151.3(6) . . . . ? Au2 P3 C31 C36 -26.3(7) . . . . ? C37 P3 C31 C32 -79.7(7) . . . . ? C55 P3 C31 C32 30.4(7) . . . . ? Au2 P3 C31 C32 155.4(6) . . . . ? C36 C31 C32 C33 -0.5(12) . . . . ? P3 C31 C32 C33 177.8(6) . . . . ? C31 C32 C33 C34 1.1(13) . . . . ? C32 C33 C34 C35 -1.6(13) . . . . ? C33 C34 C35 C36 1.5(13) . . . . ? C34 C35 C36 C31 -1.0(13) . . . . ? C32 C31 C36 C35 0.5(11) . . . . ? P3 C31 C36 C35 -177.9(6) . . . . ? C31 P3 C37 C42 15.0(7) . . . . ? C55 P3 C37 C42 -96.8(7) . . . . ? Au2 P3 C37 C42 136.8(6) . . . . ? C31 P3 C37 C38 -168.2(6) . . . . ? C55 P3 C37 C38 80.0(6) . . . . ? Au2 P3 C37 C38 -46.4(6) . . . . ? C42 C37 C38 C39 -0.4(11) . . . . ? P3 C37 C38 C39 -177.4(5) . . . . ? C37 C38 C39 C40 0.5(11) . . . . ? C38 C39 C40 C41 0.6(12) . . . . ? C39 C40 C41 C42 -1.8(13) . . . . ? C40 C41 C42 C37 1.9(13) . . . . ? C38 C37 C42 C41 -0.8(11) . . . . ? P3 C37 C42 C41 176.0(6) . . . . ? C49 P4 C43 C44 72.7(7) . . . . ? C56 P4 C43 C44 -39.7(7) . . . . ? S4 P4 C43 C44 -161.4(6) . . . . ? C49 P4 C43 C48 -111.9(6) . . . . ? C56 P4 C43 C48 135.7(6) . . . . ? S4 P4 C43 C48 14.0(7) . . . . ? C48 C43 C44 C45 0.3(12) . . . . ? P4 C43 C44 C45 175.8(7) . . . . ? C43 C44 C45 C46 -0.2(13) . . . . ? C44 C45 C46 C47 1.0(14) . . . . ? C45 C46 C47 C48 -1.8(14) . . . . ? C46 C47 C48 C43 1.9(13) . . . . ? C44 C43 C48 C47 -1.1(12) . . . . ? P4 C43 C48 C47 -176.8(7) . . . . ? C43 P4 C49 C50 -18.8(7) . . . . ? C56 P4 C49 C50 93.7(7) . . . . ? S4 P4 C49 C50 -144.5(6) . . . . ? C43 P4 C49 C54 160.5(6) . . . . ? C56 P4 C49 C54 -87.0(6) . . . . ? S4 P4 C49 C54 34.8(7) . . . . ? C54 C49 C50 C51 -0.8(12) . . . . ? P4 C49 C50 C51 178.5(6) . . . . ? C49 C50 C51 C52 1.1(13) . . . . ? C50 C51 C52 C53 -0.9(15) . . . . ? C51 C52 C53 C54 0.2(14) . . . . ? C52 C53 C54 C49 0.1(13) . . . . ? C50 C49 C54 C53 0.2(12) . . . . ? P4 C49 C54 C53 -179.1(7) . . . . ? C37 P3 C55 C56 177.4(6) . . . . ? C31 P3 C55 C56 66.6(7) . . . . ? Au2 P3 C55 C56 -55.8(7) . . . . ? P3 C55 C56 P4 -170.6(4) . . . . ? C43 P4 C56 C55 -68.6(6) . . . . ? C49 P4 C56 C55 176.9(6) . . . . ? S4 P4 C56 C55 54.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 23.36 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.474 _refine_diff_density_min -1.484 _refine_diff_density_rms 0.153 data_1 _database_code_CSD 213796 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(h5-C5Me5)Ir(S2N2)Au(PPh3)][ClO4] ; _chemical_name_common - _chemical_melting_point - _chemical_formula_moiety 'C28 H30 Au Cl Ir N2 O4 P S2' _chemical_formula_sum 'C28 H30 Au Cl Ir N2 O4 P S2' _chemical_formula_weight 978.25 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0057(17) _cell_length_b 11.2301(15) _cell_length_c 21.098(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.213(2) _cell_angle_gamma 90.00 _cell_volume 3049.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 159 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 2.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 9.477 _exptl_absorpt_correction_type MULTISCAN _exptl_absorpt_correction_T_min 0.631559 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details - _exptl_special_details ; - ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 14834 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.29 _reflns_number_total 4361 _reflns_number_gt 3616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00027(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4361 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0464 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.840139(17) 0.66207(2) 0.065494(10) 0.01924(8) Uani 1 1 d . . . N1 N 0.8677(3) 0.4979(4) 0.0279(2) 0.0185(11) Uani 1 1 d . . . S1 S 0.94666(11) 0.41553(13) 0.07220(7) 0.0230(4) Uani 1 1 d . . . N2 N 0.9666(3) 0.2970(4) 0.0366(2) 0.0227(11) Uani 1 1 d . . . S2 S 0.90389(11) 0.28239(13) -0.03746(7) 0.0239(3) Uani 1 1 d . . . P1 P 0.80023(11) 0.84545(14) 0.09590(7) 0.0198(3) Uani 1 1 d . . . C1 C 0.7461(4) 0.9259(5) 0.0243(3) 0.0215(14) Uani 1 1 d . . . C2 C 0.8100(5) 0.9767(5) -0.0161(3) 0.0294(15) Uani 1 1 d . . . H2A H 0.8825 0.9830 -0.0020 0.035 Uiso 1 1 calc R . . C3 C 0.7702(6) 1.0179(5) -0.0760(3) 0.0315(16) Uani 1 1 d . . . H3A H 0.8148 1.0538 -0.1025 0.038 Uiso 1 1 calc R . . C4 C 0.6666(6) 1.0069(5) -0.0973(3) 0.0362(17) Uani 1 1 d . . . H4A H 0.6400 1.0323 -0.1394 0.043 Uiso 1 1 calc R . . C5 C 0.6005(5) 0.9601(5) -0.0590(3) 0.0319(16) Uani 1 1 d . . . H5A H 0.5282 0.9553 -0.0740 0.038 Uiso 1 1 calc R . . C6 C 0.6393(4) 0.9193(5) 0.0022(3) 0.0244(14) Uani 1 1 d . . . H6A H 0.5934 0.8869 0.0289 0.029 Uiso 1 1 calc R . . C7 C 0.9064(4) 0.9322(5) 0.1367(2) 0.0197(13) Uani 1 1 d . . . C8 C 0.9876(4) 0.8726(5) 0.1749(3) 0.0240(14) Uani 1 1 d . . . H8A H 0.9893 0.7880 0.1747 0.029 Uiso 1 1 calc R . . C9 C 1.0653(5) 0.9349(6) 0.2129(3) 0.0317(16) Uani 1 1 d . . . H9A H 1.1196 0.8937 0.2389 0.038 Uiso 1 1 calc R . . C10 C 1.0622(5) 1.0587(6) 0.2123(3) 0.0320(16) Uani 1 1 d . . . H10A H 1.1153 1.1022 0.2380 0.038 Uiso 1 1 calc R . . C11 C 0.9832(5) 1.1195(6) 0.1749(3) 0.0347(17) Uani 1 1 d . . . H11A H 0.9821 1.2041 0.1748 0.042 Uiso 1 1 calc R . . C12 C 0.9059(5) 1.0563(5) 0.1376(3) 0.0271(14) Uani 1 1 d . . . H12A H 0.8514 1.0981 0.1121 0.032 Uiso 1 1 calc R . . C13 C 0.7024(4) 0.8488(6) 0.1492(3) 0.0257(15) Uani 1 1 d . . . C14 C 0.6785(4) 0.7445(6) 0.1796(3) 0.0279(15) Uani 1 1 d . . . H14A H 0.7090 0.6711 0.1698 0.033 Uiso 1 1 calc R . . C15 C 0.6097(5) 0.7484(7) 0.2241(3) 0.0413(19) Uani 1 1 d . . . H15A H 0.5944 0.6776 0.2457 0.050 Uiso 1 1 calc R . . C16 C 0.5632(5) 0.8543(8) 0.2375(3) 0.046(2) Uani 1 1 d . . . H16A H 0.5151 0.8561 0.2674 0.055 Uiso 1 1 calc R . . C17 C 0.5867(5) 0.9566(7) 0.2074(3) 0.0385(18) Uani 1 1 d . . . H17A H 0.5554 1.0294 0.2174 0.046 Uiso 1 1 calc R . . C18 C 0.6548(4) 0.9562(6) 0.1630(3) 0.0265(15) Uani 1 1 d . . . H18A H 0.6694 1.0277 0.1419 0.032 Uiso 1 1 calc R . . Ir1 Ir 0.806018(16) 0.44197(2) -0.058411(10) 0.01617(8) Uani 1 1 d . . . C21 C 0.6475(4) 0.4204(5) -0.1033(3) 0.0197(13) Uani 1 1 d . . . C22 C 0.6597(4) 0.5431(5) -0.0824(2) 0.0180(13) Uani 1 1 d . . . C23 C 0.7362(4) 0.5959(5) -0.1152(2) 0.0198(14) Uani 1 1 d . . . C24 C 0.7730(4) 0.5066(5) -0.1560(2) 0.0189(13) Uani 1 1 d . . . C25 C 0.7152(4) 0.3994(5) -0.1512(2) 0.0210(14) Uani 1 1 d . . . C26 C 0.5734(4) 0.3337(5) -0.0817(3) 0.0265(14) Uani 1 1 d . . . H26A H 0.5062 0.3398 -0.1092 0.040 Uiso 1 1 calc R . . H26B H 0.5642 0.3514 -0.0373 0.040 Uiso 1 1 calc R . . H26C H 0.6008 0.2528 -0.0842 0.040 Uiso 1 1 calc R . . C27 C 0.6003(4) 0.6010(5) -0.0360(3) 0.0257(14) Uani 1 1 d . . . H27A H 0.5384 0.6394 -0.0592 0.039 Uiso 1 1 calc R . . H27B H 0.6439 0.6611 -0.0115 0.039 Uiso 1 1 calc R . . H27C H 0.5793 0.5410 -0.0067 0.039 Uiso 1 1 calc R . . C28 C 0.7706(4) 0.7220(5) -0.1114(3) 0.0231(14) Uani 1 1 d . . . H28A H 0.7247 0.7695 -0.1425 0.035 Uiso 1 1 calc R . . H28B H 0.8420 0.7272 -0.1210 0.035 Uiso 1 1 calc R . . H28C H 0.7678 0.7525 -0.0682 0.035 Uiso 1 1 calc R . . C29 C 0.8495(5) 0.5288(6) -0.2011(3) 0.0307(16) Uani 1 1 d . . . H29A H 0.8130 0.5575 -0.2420 0.046 Uiso 1 1 calc R . . H29B H 0.8860 0.4545 -0.2080 0.046 Uiso 1 1 calc R . . H29C H 0.8999 0.5888 -0.1828 0.046 Uiso 1 1 calc R . . C30 C 0.7211(5) 0.2888(5) -0.1906(3) 0.0293(15) Uani 1 1 d . . . H30A H 0.6711 0.2947 -0.2300 0.044 Uiso 1 1 calc R . . H30B H 0.7045 0.2192 -0.1660 0.044 Uiso 1 1 calc R . . H30C H 0.7914 0.2805 -0.2017 0.044 Uiso 1 1 calc R . . Cl1 Cl 0.67675(12) 0.36436(17) 0.15295(8) 0.0393(4) Uani 1 1 d . . . O1 O 0.5986(3) 0.2739(4) 0.1514(2) 0.0445(12) Uani 1 1 d . . . O2 O 0.6748(4) 0.4382(4) 0.2094(2) 0.0545(14) Uani 1 1 d . . . O3 O 0.7769(3) 0.3097(5) 0.1575(2) 0.0543(14) Uani 1 1 d . . . O4 O 0.6568(4) 0.4393(5) 0.0978(3) 0.079(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01855(13) 0.02480(14) 0.01382(13) -0.00184(10) 0.00044(9) 0.00063(11) N1 0.018(3) 0.025(3) 0.013(2) 0.002(2) 0.002(2) 0.003(2) S1 0.0218(8) 0.0271(9) 0.0186(8) 0.0047(7) -0.0023(6) 0.0005(7) N2 0.017(3) 0.026(3) 0.023(3) 0.006(2) -0.002(2) -0.001(2) S2 0.0225(8) 0.0236(8) 0.0247(8) -0.0011(7) 0.0003(6) 0.0036(7) P1 0.0178(8) 0.0255(9) 0.0155(8) -0.0025(7) 0.0011(6) 0.0003(7) C1 0.026(3) 0.017(3) 0.019(3) -0.004(3) -0.003(3) 0.001(3) C2 0.030(4) 0.033(4) 0.023(3) 0.001(3) -0.004(3) -0.006(3) C3 0.058(5) 0.023(4) 0.014(3) 0.003(3) 0.007(3) -0.012(3) C4 0.060(5) 0.022(4) 0.022(4) 0.003(3) -0.010(4) 0.007(4) C5 0.033(4) 0.038(4) 0.021(3) 0.000(3) -0.004(3) 0.017(3) C6 0.022(3) 0.024(4) 0.026(3) -0.003(3) 0.001(3) 0.002(3) C7 0.021(3) 0.030(4) 0.009(3) -0.003(3) 0.005(2) -0.007(3) C8 0.019(3) 0.028(4) 0.026(3) -0.007(3) 0.007(3) 0.004(3) C9 0.016(3) 0.055(5) 0.024(4) -0.014(3) 0.001(3) 0.003(3) C10 0.026(4) 0.050(5) 0.021(3) -0.012(3) 0.006(3) -0.018(4) C11 0.045(4) 0.035(4) 0.025(4) -0.002(3) 0.012(3) -0.016(4) C12 0.034(4) 0.032(4) 0.013(3) 0.002(3) -0.003(3) -0.006(3) C13 0.019(3) 0.038(4) 0.019(3) -0.008(3) 0.000(3) -0.001(3) C14 0.018(3) 0.040(4) 0.025(3) -0.003(3) -0.003(3) -0.007(3) C15 0.019(3) 0.078(6) 0.027(4) 0.009(4) 0.005(3) -0.017(4) C16 0.019(4) 0.090(6) 0.030(4) -0.021(4) 0.012(3) -0.013(4) C17 0.023(4) 0.064(5) 0.028(4) -0.019(4) 0.003(3) 0.006(4) C18 0.020(3) 0.037(4) 0.021(3) -0.012(3) -0.001(3) 0.002(3) Ir1 0.01455(13) 0.02137(14) 0.01246(13) -0.00020(10) 0.00146(9) 0.00089(10) C21 0.014(3) 0.024(3) 0.019(3) -0.003(3) -0.006(2) 0.003(3) C22 0.015(3) 0.024(3) 0.013(3) 0.000(3) -0.004(2) 0.003(3) C23 0.019(3) 0.026(3) 0.013(3) 0.006(3) -0.002(2) 0.003(3) C24 0.015(3) 0.028(3) 0.013(3) 0.008(3) -0.003(2) 0.003(3) C25 0.019(3) 0.027(3) 0.015(3) -0.002(3) -0.002(3) 0.005(3) C26 0.020(3) 0.029(4) 0.030(4) -0.008(3) 0.003(3) -0.004(3) C27 0.021(3) 0.030(4) 0.025(3) -0.003(3) 0.001(3) 0.005(3) C28 0.019(3) 0.023(3) 0.025(3) 0.007(3) -0.003(3) -0.001(3) C29 0.032(4) 0.045(4) 0.016(3) 0.005(3) 0.008(3) 0.002(3) C30 0.034(4) 0.035(4) 0.017(3) -0.013(3) -0.003(3) 0.013(3) Cl1 0.0227(9) 0.0616(12) 0.0330(10) 0.0219(9) 0.0015(7) -0.0008(8) O1 0.037(3) 0.053(3) 0.043(3) 0.005(2) 0.001(2) -0.009(3) O2 0.064(4) 0.043(3) 0.058(3) -0.005(3) 0.015(3) 0.003(3) O3 0.025(3) 0.092(4) 0.046(3) 0.003(3) 0.002(2) 0.018(3) O4 0.045(3) 0.121(5) 0.067(4) 0.067(4) -0.006(3) -0.011(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 Au1 N1 2.059(4) . ? Au1 P1 2.2400(15) . ? N1 S1 1.584(4) . ? N1 Ir1 1.984(4) . ? S1 N2 1.568(5) . ? N2 S2 1.664(5) . ? S2 Ir1 2.2060(15) . ? P1 C7 1.806(6) . ? P1 C1 1.814(6) . ? P1 C13 1.814(6) . ? C1 C2 1.396(8) . ? C1 C6 1.402(8) . ? C2 C3 1.376(8) . ? C3 C4 1.364(9) . ? C4 C5 1.366(9) . ? C5 C6 1.395(8) . ? C7 C12 1.394(8) . ? C7 C8 1.403(8) . ? C8 C9 1.386(8) . ? C9 C10 1.391(9) . ? C10 C11 1.384(9) . ? C11 C12 1.381(8) . ? C13 C14 1.392(8) . ? C13 C18 1.405(8) . ? C14 C15 1.389(8) . ? C15 C16 1.381(10) . ? C16 C17 1.368(10) . ? C17 C18 1.379(8) . ? Ir1 C21 2.157(5) . ? Ir1 C24 2.167(5) . ? Ir1 C25 2.189(5) . ? Ir1 C22 2.212(5) . ? Ir1 C23 2.223(5) . ? C21 C22 1.449(8) . ? C21 C25 1.451(8) . ? C21 C26 1.487(8) . ? C22 C23 1.421(7) . ? C22 C27 1.481(7) . ? C23 C24 1.447(8) . ? C23 C28 1.483(8) . ? C24 C25 1.430(8) . ? C24 C29 1.493(7) . ? C25 C30 1.504(8) . ? Cl1 O4 1.429(5) . ? Cl1 O3 1.430(5) . ? Cl1 O1 1.434(5) . ? Cl1 O2 1.455(5) . ? 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 Au1 P1 173.71(12) . . ? S1 N1 Ir1 120.0(3) . . ? S1 N1 Au1 115.4(2) . . ? Ir1 N1 Au1 124.6(2) . . ? N2 S1 N1 110.5(2) . . ? S1 N2 S2 116.2(3) . . ? N2 S2 Ir1 107.42(18) . . ? C7 P1 C1 107.9(3) . . ? C7 P1 C13 104.5(3) . . ? C1 P1 C13 106.4(3) . . ? C7 P1 Au1 116.1(2) . . ? C1 P1 Au1 107.33(18) . . ? C13 P1 Au1 114.1(2) . . ? C2 C1 C6 117.8(5) . . ? C2 C1 P1 121.2(4) . . ? C6 C1 P1 120.0(4) . . ? C3 C2 C1 121.3(6) . . ? C4 C3 C2 119.8(6) . . ? C3 C4 C5 121.0(6) . . ? C4 C5 C6 119.9(6) . . ? C5 C6 C1 120.1(6) . . ? C12 C7 C8 118.3(5) . . ? C12 C7 P1 122.7(4) . . ? C8 C7 P1 118.5(4) . . ? C9 C8 C7 121.2(6) . . ? C8 C9 C10 118.7(6) . . ? C11 C10 C9 121.1(6) . . ? C12 C11 C10 119.5(6) . . ? C11 C12 C7 121.1(6) . . ? C14 C13 C18 119.5(6) . . ? C14 C13 P1 119.4(5) . . ? C18 C13 P1 121.0(5) . . ? C15 C14 C13 119.6(6) . . ? C16 C15 C14 120.5(7) . . ? C17 C16 C15 119.7(6) . . ? C16 C17 C18 121.3(7) . . ? C17 C18 C13 119.3(6) . . ? N1 Ir1 C21 132.45(19) . . ? N1 Ir1 C24 139.9(2) . . ? C21 Ir1 C24 64.7(2) . . ? N1 Ir1 C25 170.17(19) . . ? C21 Ir1 C25 39.0(2) . . ? C24 Ir1 C25 38.3(2) . . ? N1 Ir1 S2 85.81(13) . . ? C21 Ir1 S2 119.01(15) . . ? C24 Ir1 S2 119.52(15) . . ? C25 Ir1 S2 102.95(15) . . ? N1 Ir1 C22 105.63(18) . . ? C21 Ir1 C22 38.7(2) . . ? C24 Ir1 C22 64.1(2) . . ? C25 Ir1 C22 64.6(2) . . ? S2 Ir1 C22 156.34(15) . . ? N1 Ir1 C23 109.24(19) . . ? C21 Ir1 C23 63.8(2) . . ? C24 Ir1 C23 38.5(2) . . ? C25 Ir1 C23 63.9(2) . . ? S2 Ir1 C23 156.87(14) . . ? C22 Ir1 C23 37.36(19) . . ? C22 C21 C25 108.4(5) . . ? C22 C21 C26 125.2(5) . . ? C25 C21 C26 126.3(5) . . ? C22 C21 Ir1 72.7(3) . . ? C25 C21 Ir1 71.7(3) . . ? C26 C21 Ir1 124.0(4) . . ? C23 C22 C21 107.6(5) . . ? C23 C22 C27 127.3(5) . . ? C21 C22 C27 125.1(5) . . ? C23 C22 Ir1 71.7(3) . . ? C21 C22 Ir1 68.6(3) . . ? C27 C22 Ir1 126.0(4) . . ? C22 C23 C24 108.3(5) . . ? C22 C23 C28 126.8(5) . . ? C24 C23 C28 124.8(5) . . ? C22 C23 Ir1 70.9(3) . . ? C24 C23 Ir1 68.7(3) . . ? C28 C23 Ir1 128.0(4) . . ? C25 C24 C23 108.6(5) . . ? C25 C24 C29 126.2(5) . . ? C23 C24 C29 124.8(5) . . ? C25 C24 Ir1 71.7(3) . . ? C23 C24 Ir1 72.9(3) . . ? C29 C24 Ir1 127.0(4) . . ? C24 C25 C21 106.9(5) . . ? C24 C25 C30 126.0(5) . . ? C21 C25 C30 127.1(5) . . ? C24 C25 Ir1 70.0(3) . . ? C21 C25 Ir1 69.3(3) . . ? C30 C25 Ir1 127.7(4) . . ? O4 Cl1 O3 111.4(3) . . ? O4 Cl1 O1 110.6(3) . . ? O3 Cl1 O1 109.4(3) . . ? O4 Cl1 O2 108.0(4) . . ? O3 Cl1 O2 108.1(3) . . ? O1 Cl1 O2 109.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au1 N1 S1 172.8(9) . . . . ? P1 Au1 N1 Ir1 -5.4(14) . . . . ? Ir1 N1 S1 N2 2.0(4) . . . . ? Au1 N1 S1 N2 -176.3(2) . . . . ? N1 S1 N2 S2 0.2(4) . . . . ? S1 N2 S2 Ir1 -1.9(3) . . . . ? N1 Au1 P1 C7 -132.3(12) . . . . ? N1 Au1 P1 C1 -11.5(12) . . . . ? N1 Au1 P1 C13 106.1(12) . . . . ? C7 P1 C1 C2 45.5(5) . . . . ? C13 P1 C1 C2 157.1(5) . . . . ? Au1 P1 C1 C2 -80.4(5) . . . . ? C7 P1 C1 C6 -146.5(4) . . . . ? C13 P1 C1 C6 -34.9(5) . . . . ? Au1 P1 C1 C6 87.6(5) . . . . ? C6 C1 C2 C3 -0.7(9) . . . . ? P1 C1 C2 C3 167.6(5) . . . . ? C1 C2 C3 C4 -1.4(9) . . . . ? C2 C3 C4 C5 2.8(10) . . . . ? C3 C4 C5 C6 -2.0(9) . . . . ? C4 C5 C6 C1 -0.2(9) . . . . ? C2 C1 C6 C5 1.5(8) . . . . ? P1 C1 C6 C5 -166.9(4) . . . . ? C1 P1 C7 C12 34.9(5) . . . . ? C13 P1 C7 C12 -78.0(5) . . . . ? Au1 P1 C7 C12 155.4(4) . . . . ? C1 P1 C7 C8 -152.2(4) . . . . ? C13 P1 C7 C8 94.8(5) . . . . ? Au1 P1 C7 C8 -31.7(5) . . . . ? C12 C7 C8 C9 0.3(8) . . . . ? P1 C7 C8 C9 -172.8(4) . . . . ? C7 C8 C9 C10 -0.6(8) . . . . ? C8 C9 C10 C11 0.3(9) . . . . ? C9 C10 C11 C12 0.1(9) . . . . ? C10 C11 C12 C7 -0.3(9) . . . . ? C8 C7 C12 C11 0.1(8) . . . . ? P1 C7 C12 C11 173.0(4) . . . . ? C7 P1 C13 C14 -112.2(5) . . . . ? C1 P1 C13 C14 133.8(5) . . . . ? Au1 P1 C13 C14 15.7(5) . . . . ? C7 P1 C13 C18 64.2(5) . . . . ? C1 P1 C13 C18 -49.8(5) . . . . ? Au1 P1 C13 C18 -168.0(4) . . . . ? C18 C13 C14 C15 -1.4(8) . . . . ? P1 C13 C14 C15 175.0(4) . . . . ? C13 C14 C15 C16 1.4(9) . . . . ? C14 C15 C16 C17 -1.3(10) . . . . ? C15 C16 C17 C18 1.2(10) . . . . ? C16 C17 C18 C13 -1.2(9) . . . . ? C14 C13 C18 C17 1.3(9) . . . . ? P1 C13 C18 C17 -175.1(4) . . . . ? S1 N1 Ir1 C21 123.7(3) . . . . ? Au1 N1 Ir1 C21 -58.1(4) . . . . ? S1 N1 Ir1 C24 -135.4(3) . . . . ? Au1 N1 Ir1 C24 42.7(4) . . . . ? S1 N1 Ir1 C25 150.7(10) . . . . ? Au1 N1 Ir1 C25 -31.1(13) . . . . ? S1 N1 Ir1 S2 -2.6(3) . . . . ? Au1 N1 Ir1 S2 175.6(2) . . . . ? S1 N1 Ir1 C22 156.4(3) . . . . ? Au1 N1 Ir1 C22 -25.5(3) . . . . ? S1 N1 Ir1 C23 -164.6(3) . . . . ? Au1 N1 Ir1 C23 13.6(3) . . . . ? N2 S2 Ir1 N1 2.3(2) . . . . ? N2 S2 Ir1 C21 -134.8(2) . . . . ? N2 S2 Ir1 C24 149.5(2) . . . . ? N2 S2 Ir1 C25 -173.1(2) . . . . ? N2 S2 Ir1 C22 -118.1(4) . . . . ? N2 S2 Ir1 C23 134.4(4) . . . . ? N1 Ir1 C21 C22 56.1(4) . . . . ? C24 Ir1 C21 C22 -79.5(3) . . . . ? C25 Ir1 C21 C22 -116.8(5) . . . . ? S2 Ir1 C21 C22 169.3(2) . . . . ? C23 Ir1 C21 C22 -36.6(3) . . . . ? N1 Ir1 C21 C25 172.9(3) . . . . ? C24 Ir1 C21 C25 37.3(3) . . . . ? S2 Ir1 C21 C25 -73.9(3) . . . . ? C22 Ir1 C21 C25 116.8(5) . . . . ? C23 Ir1 C21 C25 80.2(3) . . . . ? N1 Ir1 C21 C26 -65.1(5) . . . . ? C24 Ir1 C21 C26 159.3(5) . . . . ? C25 Ir1 C21 C26 122.0(6) . . . . ? S2 Ir1 C21 C26 48.1(5) . . . . ? C22 Ir1 C21 C26 -121.2(6) . . . . ? C23 Ir1 C21 C26 -157.8(5) . . . . ? C25 C21 C22 C23 -1.8(6) . . . . ? C26 C21 C22 C23 -178.7(5) . . . . ? Ir1 C21 C22 C23 61.5(4) . . . . ? C25 C21 C22 C27 177.0(5) . . . . ? C26 C21 C22 C27 0.1(9) . . . . ? Ir1 C21 C22 C27 -119.7(5) . . . . ? C25 C21 C22 Ir1 -63.3(4) . . . . ? C26 C21 C22 Ir1 119.8(5) . . . . ? N1 Ir1 C22 C23 101.4(3) . . . . ? C21 Ir1 C22 C23 -118.1(4) . . . . ? C24 Ir1 C22 C23 -37.0(3) . . . . ? C25 Ir1 C22 C23 -79.7(3) . . . . ? S2 Ir1 C22 C23 -141.9(3) . . . . ? N1 Ir1 C22 C21 -140.5(3) . . . . ? C24 Ir1 C22 C21 81.2(3) . . . . ? C25 Ir1 C22 C21 38.5(3) . . . . ? S2 Ir1 C22 C21 -23.8(5) . . . . ? C23 Ir1 C22 C21 118.1(4) . . . . ? N1 Ir1 C22 C27 -22.0(5) . . . . ? C21 Ir1 C22 C27 118.5(6) . . . . ? C24 Ir1 C22 C27 -160.3(6) . . . . ? C25 Ir1 C22 C27 157.0(6) . . . . ? S2 Ir1 C22 C27 94.8(6) . . . . ? C23 Ir1 C22 C27 -123.3(6) . . . . ? C21 C22 C23 C24 -0.8(6) . . . . ? C27 C22 C23 C24 -179.6(5) . . . . ? Ir1 C22 C23 C24 58.7(4) . . . . ? C21 C22 C23 C28 176.8(5) . . . . ? C27 C22 C23 C28 -1.9(9) . . . . ? Ir1 C22 C23 C28 -123.7(5) . . . . ? C21 C22 C23 Ir1 -59.5(4) . . . . ? C27 C22 C23 Ir1 121.8(5) . . . . ? N1 Ir1 C23 C22 -90.8(3) . . . . ? C21 Ir1 C23 C22 37.9(3) . . . . ? C24 Ir1 C23 C22 119.5(5) . . . . ? C25 Ir1 C23 C22 81.6(3) . . . . ? S2 Ir1 C23 C22 140.9(3) . . . . ? N1 Ir1 C23 C24 149.7(3) . . . . ? C21 Ir1 C23 C24 -81.6(3) . . . . ? C25 Ir1 C23 C24 -38.0(3) . . . . ? S2 Ir1 C23 C24 21.4(6) . . . . ? C22 Ir1 C23 C24 -119.5(5) . . . . ? N1 Ir1 C23 C28 31.5(5) . . . . ? C21 Ir1 C23 C28 160.2(6) . . . . ? C24 Ir1 C23 C28 -118.2(6) . . . . ? C25 Ir1 C23 C28 -156.2(6) . . . . ? S2 Ir1 C23 C28 -96.8(6) . . . . ? C22 Ir1 C23 C28 122.2(6) . . . . ? C22 C23 C24 C25 3.2(6) . . . . ? C28 C23 C24 C25 -174.5(5) . . . . ? Ir1 C23 C24 C25 63.2(4) . . . . ? C22 C23 C24 C29 176.4(5) . . . . ? C28 C23 C24 C29 -1.3(9) . . . . ? Ir1 C23 C24 C29 -123.5(5) . . . . ? C22 C23 C24 Ir1 -60.0(4) . . . . ? C28 C23 C24 Ir1 122.3(5) . . . . ? N1 Ir1 C24 C25 -164.7(3) . . . . ? C21 Ir1 C24 C25 -37.9(3) . . . . ? S2 Ir1 C24 C25 72.5(3) . . . . ? C22 Ir1 C24 C25 -81.1(3) . . . . ? C23 Ir1 C24 C25 -117.0(4) . . . . ? N1 Ir1 C24 C23 -47.7(4) . . . . ? C21 Ir1 C24 C23 79.1(3) . . . . ? C25 Ir1 C24 C23 117.0(4) . . . . ? S2 Ir1 C24 C23 -170.5(3) . . . . ? C22 Ir1 C24 C23 35.9(3) . . . . ? N1 Ir1 C24 C29 73.4(6) . . . . ? C21 Ir1 C24 C29 -159.9(6) . . . . ? C25 Ir1 C24 C29 -122.0(7) . . . . ? S2 Ir1 C24 C29 -49.5(6) . . . . ? C22 Ir1 C24 C29 157.0(6) . . . . ? C23 Ir1 C24 C29 121.0(6) . . . . ? C23 C24 C25 C21 -4.2(6) . . . . ? C29 C24 C25 C21 -177.4(5) . . . . ? Ir1 C24 C25 C21 59.7(4) . . . . ? C23 C24 C25 C30 173.3(5) . . . . ? C29 C24 C25 C30 0.2(9) . . . . ? Ir1 C24 C25 C30 -122.7(5) . . . . ? C23 C24 C25 Ir1 -64.0(4) . . . . ? C29 C24 C25 Ir1 122.9(6) . . . . ? C22 C21 C25 C24 3.7(6) . . . . ? C26 C21 C25 C24 -179.4(5) . . . . ? Ir1 C21 C25 C24 -60.2(4) . . . . ? C22 C21 C25 C30 -173.8(5) . . . . ? C26 C21 C25 C30 3.0(9) . . . . ? Ir1 C21 C25 C30 122.3(6) . . . . ? C22 C21 C25 Ir1 63.9(4) . . . . ? C26 C21 C25 Ir1 -119.2(5) . . . . ? N1 Ir1 C25 C24 85.7(12) . . . . ? C21 Ir1 C25 C24 117.9(5) . . . . ? S2 Ir1 C25 C24 -121.6(3) . . . . ? C22 Ir1 C25 C24 79.7(3) . . . . ? C23 Ir1 C25 C24 38.1(3) . . . . ? N1 Ir1 C25 C21 -32.2(13) . . . . ? C24 Ir1 C25 C21 -117.9(5) . . . . ? S2 Ir1 C25 C21 120.5(3) . . . . ? C22 Ir1 C25 C21 -38.2(3) . . . . ? C23 Ir1 C25 C21 -79.8(3) . . . . ? N1 Ir1 C25 C30 -153.7(10) . . . . ? C21 Ir1 C25 C30 -121.5(7) . . . . ? C24 Ir1 C25 C30 120.6(6) . . . . ? S2 Ir1 C25 C30 -1.1(5) . . . . ? C22 Ir1 C25 C30 -159.7(6) . . . . ? C23 Ir1 C25 C30 158.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.745 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.126 data_3 _database_code_CSD 213797 _audit_creation_method SHELXL-97 _chemical_name_systematic ; - ; _chemical_name_common - _chemical_melting_point - _chemical_formula_moiety 'C44 H53 Au2 Ir2 N4 P2 S4.[Cl O4]2.[C2 H2 Cl2]' _chemical_formula_sum 'C46 H55 Au2 Cl4 Ir2 N4 O8 P2 S4' _chemical_formula_weight 1902.25 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' 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 32.363(8) _cell_length_b 10.367(3) _cell_length_c 16.838(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5649(3) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 307 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 2.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3588 _exptl_absorpt_coefficient_mu 10.321 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.702289 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details - _exptl_special_details ; - ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 23332 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.33 _reflns_number_total 7349 _reflns_number_gt 7056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0455P)^2^+5.5123P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 7349 _refine_ls_number_parameters 649 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.0661(2) 0.5236(8) 0.8086(5) 0.0207(19) Uani 1 1 d . . . C31 C -0.0181(3) 0.4990(11) 0.6540(6) 0.028(2) Uani 1 1 d . . . C32 C -0.0461(3) 0.4330(10) 0.7053(6) 0.027(2) Uani 1 1 d . . . C33 C -0.0278(3) 0.3124(10) 0.7262(7) 0.030(2) Uani 1 1 d . . . C34 C 0.0127(3) 0.3064(12) 0.6869(6) 0.032(3) Uani 1 1 d . . . C35 C 0.0183(3) 0.4212(11) 0.6404(6) 0.028(3) Uani 1 1 d . . . C36 C -0.0265(3) 0.6252(12) 0.6139(7) 0.037(3) Uani 1 1 d . . . H36A H -0.0398 0.6095 0.5626 0.055 Uiso 1 1 calc R . . H36B H -0.0004 0.6711 0.6055 0.055 Uiso 1 1 calc R . . H36C H -0.0447 0.6775 0.6474 0.055 Uiso 1 1 calc R . . C37 C -0.0882(3) 0.4790(10) 0.7296(8) 0.035(3) Uani 1 1 d . . . H37A H -0.1087 0.4500 0.6906 0.053 Uiso 1 1 calc R . . H37B H -0.0883 0.5734 0.7323 0.053 Uiso 1 1 calc R . . H37C H -0.0951 0.4435 0.7819 0.053 Uiso 1 1 calc R . . C38 C -0.0445(4) 0.2088(11) 0.7750(8) 0.041(3) Uani 1 1 d . . . H38A H -0.0607 0.1501 0.7416 0.061 Uiso 1 1 calc R . . H38B H -0.0623 0.2454 0.8163 0.061 Uiso 1 1 calc R . . H38C H -0.0217 0.1612 0.7998 0.061 Uiso 1 1 calc R . . C39 C 0.0428(4) 0.1969(11) 0.6906(8) 0.045(3) Uani 1 1 d . . . H39A H 0.0371 0.1364 0.6472 0.067 Uiso 1 1 calc R . . H39B H 0.0399 0.1522 0.7416 0.067 Uiso 1 1 calc R . . H39C H 0.0710 0.2302 0.6854 0.067 Uiso 1 1 calc R . . C40 C 0.0536(4) 0.4525(15) 0.5867(7) 0.051(4) Uani 1 1 d . . . H40A H 0.0482 0.4174 0.5337 0.076 Uiso 1 1 calc R . . H40B H 0.0790 0.4143 0.6080 0.076 Uiso 1 1 calc R . . H40C H 0.0569 0.5463 0.5832 0.076 Uiso 1 1 calc R . . Ir1 Ir 0.010835(11) 0.47066(4) 0.76976(2) 0.02041(10) Uani 1 1 d . . . S2 S -0.01249(7) 0.5395(3) 0.88380(17) 0.0302(6) Uani 1 1 d . . . N2 N 0.0279(3) 0.5904(9) 0.9365(5) 0.031(2) Uani 1 1 d . . . S1 S 0.07095(7) 0.5805(2) 0.89540(16) 0.0224(5) Uani 1 1 d . . . Au1 Au 0.120396(10) 0.50531(3) 0.74494(3) 0.02150(9) Uani 1 1 d . . . P1 P 0.17481(8) 0.4652(3) 0.66521(17) 0.0238(6) Uani 1 1 d . . . C1 C 0.1603(3) 0.3458(9) 0.5921(7) 0.030(3) Uani 1 1 d . . . C2 C 0.1490(3) 0.3794(11) 0.5150(7) 0.034(3) Uani 1 1 d . . . H2A H 0.1531 0.4647 0.4961 0.041 Uiso 1 1 calc R . . C3 C 0.1310(4) 0.2837(12) 0.4646(7) 0.047(3) Uani 1 1 d . . . H3A H 0.1225 0.3059 0.4123 0.056 Uiso 1 1 calc R . . C4 C 0.1259(4) 0.1611(12) 0.4912(8) 0.045(3) Uani 1 1 d . . . H4A H 0.1138 0.0978 0.4576 0.053 Uiso 1 1 calc R . . C5 C 0.1385(4) 0.1280(12) 0.5674(8) 0.041(3) Uani 1 1 d . . . H5A H 0.1353 0.0416 0.5853 0.049 Uiso 1 1 calc R . . C6 C 0.1553(3) 0.2189(10) 0.6174(7) 0.030(2) Uani 1 1 d . . . H6A H 0.1636 0.1949 0.6695 0.036 Uiso 1 1 calc R . . C7 C 0.2196(3) 0.4021(10) 0.7152(6) 0.027(2) Uani 1 1 d . . . C8 C 0.2568(4) 0.3791(12) 0.6735(7) 0.041(3) Uani 1 1 d . . . H8A H 0.2573 0.3941 0.6178 0.049 Uiso 1 1 calc R . . C9 C 0.2920(4) 0.3363(13) 0.7094(8) 0.048(3) Uani 1 1 d . . . H9A H 0.3165 0.3209 0.6798 0.057 Uiso 1 1 calc R . . C10 C 0.2906(4) 0.3158(12) 0.7921(9) 0.052(4) Uani 1 1 d . . . H10A H 0.3146 0.2883 0.8196 0.062 Uiso 1 1 calc R . . C11 C 0.2544(4) 0.3355(10) 0.8329(8) 0.042(3) Uani 1 1 d . . . H11A H 0.2535 0.3186 0.8884 0.051 Uiso 1 1 calc R . . C12 C 0.2196(3) 0.3794(10) 0.7950(7) 0.034(3) Uani 1 1 d . . . H12A H 0.1951 0.3940 0.8247 0.041 Uiso 1 1 calc R . . C13 C 0.1925(3) 0.6063(9) 0.6084(7) 0.028(2) Uani 1 1 d . . . H13A H 0.2191 0.5848 0.5828 0.033 Uiso 1 1 calc R . . H13B H 0.1722 0.6238 0.5656 0.033 Uiso 1 1 calc R . . C14 C 0.2158(3) 0.8716(9) 0.5934(7) 0.027(3) Uani 1 1 d . . . C15 C 0.2048(3) 0.8641(11) 0.5143(7) 0.035(3) Uani 1 1 d . . . H15A H 0.1883 0.7941 0.4964 0.041 Uiso 1 1 calc R . . C16 C 0.2175(4) 0.9566(11) 0.4612(8) 0.044(3) Uani 1 1 d . . . H16A H 0.2094 0.9494 0.4072 0.053 Uiso 1 1 calc R . . C17 C 0.2412(4) 1.0579(13) 0.4839(9) 0.050(4) Uani 1 1 d . . . H17A H 0.2501 1.1199 0.4461 0.061 Uiso 1 1 calc R . . C18 C 0.2520(4) 1.0694(12) 0.5620(11) 0.056(4) Uani 1 1 d . . . H18A H 0.2680 1.1413 0.5786 0.068 Uiso 1 1 calc R . . C19 C 0.2399(3) 0.9767(11) 0.6183(9) 0.044(3) Uani 1 1 d . . . H19A H 0.2243 1.0221 0.6605 0.053 Uiso 1 1 calc R . . H19B H 0.2653 0.9418 0.6430 0.053 Uiso 1 1 calc R . . C20 C 0.2431(3) 0.7227(9) 0.7304(7) 0.030(2) Uani 1 1 d . . . C21 C 0.2836(3) 0.7289(12) 0.6998(8) 0.044(3) Uani 1 1 d . . . H21A H 0.2882 0.7527 0.6460 0.053 Uiso 1 1 calc R . . C22 C 0.3162(3) 0.7003(11) 0.7485(9) 0.051(4) Uani 1 1 d . . . H22A H 0.3435 0.7021 0.7276 0.062 Uiso 1 1 calc R . . C23 C 0.3104(4) 0.6696(13) 0.8252(10) 0.055(4) Uani 1 1 d . . . H23A H 0.3336 0.6536 0.8583 0.066 Uiso 1 1 calc R . . C24 C 0.2704(4) 0.6609(13) 0.8570(8) 0.054(4) Uani 1 1 d . . . H24A H 0.2661 0.6353 0.9105 0.065 Uiso 1 1 calc R . . C25 C 0.2366(3) 0.6915(11) 0.8069(8) 0.036(3) Uani 1 1 d . . . H25A H 0.2093 0.6899 0.8274 0.043 Uiso 1 1 calc R . . P3 P 0.19913(8) 0.7520(3) 0.66632(17) 0.0248(6) Uani 1 1 d . . . Au3 Au 0.140388(10) 0.80587(3) 0.72945(2) 0.02134(9) Uani 1 1 d . . . N3 N 0.0844(2) 0.8588(7) 0.7775(5) 0.0220(18) Uani 1 1 d . . . S3 S 0.04717(7) 0.8232(2) 0.71832(16) 0.0266(6) Uani 1 1 d . . . N4 N 0.0046(2) 0.8511(8) 0.7589(5) 0.030(2) Uani 1 1 d . . . S4 S 0.00659(8) 0.9078(3) 0.85146(17) 0.0304(6) Uani 1 1 d . . . Ir3 Ir 0.072110(11) 0.93227(3) 0.88369(2) 0.02075(9) Uani 1 1 d . . . C41 C 0.0940(3) 0.9014(9) 1.0041(6) 0.027(2) Uani 1 1 d . . . C42 C 0.1301(3) 0.9324(11) 0.9563(7) 0.029(3) Uani 1 1 d . . . C43 C 0.1239(3) 1.0552(11) 0.9214(7) 0.030(3) Uani 1 1 d . . . C44 C 0.0849(4) 1.1043(10) 0.9491(6) 0.029(3) Uani 1 1 d . . . C45 C 0.0674(3) 1.0131(11) 1.0014(6) 0.032(3) Uani 1 1 d . . . C46 C 0.0890(4) 0.7860(11) 1.0545(7) 0.038(3) Uani 1 1 d . . . H46A H 0.1011 0.8025 1.1069 0.057 Uiso 1 1 calc R . . H46B H 0.1031 0.7127 1.0297 0.057 Uiso 1 1 calc R . . H46C H 0.0595 0.7663 1.0603 0.057 Uiso 1 1 calc R . . C47 C 0.1674(3) 0.8447(11) 0.9482(7) 0.036(3) Uani 1 1 d . . . H47A H 0.1881 0.8683 0.9881 0.055 Uiso 1 1 calc R . . H47B H 0.1792 0.8543 0.8950 0.055 Uiso 1 1 calc R . . H47C H 0.1589 0.7550 0.9563 0.055 Uiso 1 1 calc R . . C48 C 0.1537(4) 1.1249(12) 0.8676(6) 0.037(3) Uani 1 1 d . . . H48A H 0.1735 1.1737 0.8997 0.056 Uiso 1 1 calc R . . H48B H 0.1383 1.1842 0.8332 0.056 Uiso 1 1 calc R . . H48C H 0.1685 1.0620 0.8348 0.056 Uiso 1 1 calc R . . C49 C 0.0684(4) 1.2371(10) 0.9301(7) 0.039(3) Uani 1 1 d . . . H49A H 0.0790 1.2991 0.9690 0.058 Uiso 1 1 calc R . . H49B H 0.0382 1.2359 0.9322 0.058 Uiso 1 1 calc R . . H49C H 0.0774 1.2623 0.8767 0.058 Uiso 1 1 calc R . . C50 C 0.0282(4) 1.0268(12) 1.0500(7) 0.039(3) Uani 1 1 d . . . H50A H 0.0348 1.0656 1.1016 0.058 Uiso 1 1 calc R . . H50B H 0.0158 0.9415 1.0583 0.058 Uiso 1 1 calc R . . H50C H 0.0085 1.0821 1.0216 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.17650(9) 0.4752(3) 1.00320(17) 0.0374(7) Uani 1 1 d . . . O1 O 0.1454(4) 0.4945(14) 1.0604(7) 0.108(5) Uani 1 1 d . . . O2 O 0.1610(3) 0.5086(9) 0.9254(5) 0.054(2) Uani 1 1 d . . . O3 O 0.2102(4) 0.5562(10) 1.0185(7) 0.091(4) Uani 1 1 d . . . O4 O 0.1918(3) 0.3472(8) 1.0041(6) 0.065(3) Uani 1 1 d . . . Cl2 Cl -0.09138(8) 0.2349(3) 0.97912(16) 0.0320(6) Uani 1 1 d . . . O5 O -0.1070(3) 0.1347(8) 0.9289(5) 0.049(2) Uani 1 1 d . . . O6 O -0.0481(2) 0.2379(10) 0.9789(5) 0.052(2) Uani 1 1 d . . . O7 O -0.1055(4) 0.3546(9) 0.9474(8) 0.084(4) Uani 1 1 d . . . O8 O -0.1063(3) 0.2272(15) 1.0568(6) 0.090(4) Uani 1 1 d . . . C60 C 0.1382(4) 1.0329(13) 1.2662(10) 0.058(4) Uani 1 1 d . . . H60A H 0.1316 0.9466 1.2880 0.070 Uiso 1 1 calc R . . H60B H 0.1618 1.0685 1.2968 0.070 Uiso 1 1 calc R . . Cl3 Cl 0.09521(11) 1.1347(4) 1.2765(3) 0.0658(10) Uani 1 1 d . . . Cl4 Cl 0.15210(14) 1.0186(4) 1.1658(3) 0.0800(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.019(4) 0.016(4) 0.026(5) 0.002(4) 0.004(4) 0.001(3) C31 0.036(6) 0.029(6) 0.018(6) 0.005(5) -0.009(5) -0.010(5) C32 0.023(5) 0.038(6) 0.019(6) -0.003(5) -0.007(4) 0.000(5) C33 0.044(6) 0.029(6) 0.017(6) -0.004(5) 0.002(5) -0.020(5) C34 0.035(6) 0.048(7) 0.013(5) -0.008(5) -0.011(5) -0.006(5) C35 0.028(6) 0.041(7) 0.015(6) 0.002(5) 0.001(4) -0.014(5) C36 0.042(6) 0.045(7) 0.024(6) 0.004(6) -0.014(5) -0.009(6) C37 0.021(5) 0.041(6) 0.045(7) -0.006(6) 0.001(5) -0.001(5) C38 0.043(7) 0.035(6) 0.045(8) -0.004(6) 0.004(6) -0.016(5) C39 0.043(7) 0.034(7) 0.056(9) -0.011(6) 0.000(6) -0.006(6) C40 0.045(7) 0.089(11) 0.019(7) -0.002(7) 0.003(6) -0.003(7) Ir1 0.02375(19) 0.02162(18) 0.0159(2) 0.00235(16) -0.00015(15) -0.00442(15) S2 0.0266(13) 0.0414(16) 0.0225(15) -0.0049(13) 0.0050(12) -0.0067(11) N2 0.031(5) 0.036(5) 0.024(5) -0.005(4) 0.005(4) -0.003(4) S1 0.0275(12) 0.0209(12) 0.0189(15) -0.0007(11) -0.0009(10) -0.0012(10) Au1 0.02338(18) 0.02086(18) 0.0203(2) -0.00146(15) 0.00198(16) -0.00101(15) P1 0.0274(14) 0.0208(14) 0.0230(16) -0.0005(12) 0.0039(12) 0.0024(11) C1 0.036(6) 0.018(5) 0.035(7) -0.007(5) 0.010(5) -0.002(5) C2 0.052(7) 0.026(6) 0.023(6) -0.004(5) 0.010(5) -0.001(5) C3 0.079(9) 0.042(8) 0.019(7) -0.003(6) 0.001(6) -0.008(7) C4 0.054(8) 0.039(7) 0.040(9) -0.022(6) 0.015(6) -0.009(6) C5 0.041(7) 0.032(7) 0.048(9) -0.017(6) 0.007(6) 0.001(6) C6 0.030(6) 0.026(6) 0.036(7) -0.001(5) 0.002(5) 0.003(5) C7 0.025(5) 0.033(6) 0.022(6) 0.003(5) -0.001(4) -0.005(4) C8 0.042(7) 0.046(7) 0.034(7) 0.000(6) 0.000(5) 0.019(6) C9 0.033(7) 0.049(8) 0.061(10) 0.001(7) -0.003(6) 0.006(6) C10 0.050(8) 0.044(7) 0.062(10) 0.013(7) -0.037(7) 0.012(6) C11 0.062(8) 0.026(6) 0.039(8) 0.012(6) -0.009(6) 0.001(6) C12 0.044(7) 0.023(6) 0.034(7) 0.012(5) 0.001(5) 0.012(5) C13 0.029(6) 0.021(5) 0.033(6) 0.001(5) -0.003(5) 0.000(4) C14 0.027(5) 0.008(5) 0.047(8) 0.005(5) 0.007(5) 0.003(4) C15 0.047(7) 0.026(6) 0.030(7) 0.003(5) 0.004(5) 0.004(5) C16 0.064(9) 0.025(6) 0.043(8) 0.011(6) 0.026(6) 0.003(6) C17 0.042(8) 0.044(8) 0.065(11) 0.016(8) -0.002(7) 0.010(6) C18 0.037(7) 0.021(6) 0.112(15) -0.004(8) 0.010(8) -0.006(6) C19 0.030(7) 0.033(6) 0.070(10) -0.004(7) 0.006(6) -0.001(5) C20 0.032(5) 0.028(5) 0.031(7) -0.004(5) -0.007(5) -0.004(4) C21 0.034(7) 0.046(8) 0.052(8) -0.008(6) 0.000(6) 0.010(6) C22 0.031(6) 0.042(7) 0.081(12) 0.003(7) -0.013(7) 0.008(5) C23 0.042(8) 0.057(9) 0.065(11) -0.001(8) -0.025(7) 0.010(7) C24 0.070(9) 0.048(8) 0.045(9) -0.002(6) -0.023(7) -0.006(7) C25 0.032(6) 0.029(6) 0.045(8) 0.002(6) -0.011(5) 0.005(5) P3 0.0219(13) 0.0244(14) 0.0280(16) -0.0020(12) 0.0014(11) 0.0006(11) Au3 0.02199(17) 0.02199(19) 0.0200(2) -0.00379(17) -0.00069(16) 0.00238(15) N3 0.021(4) 0.024(4) 0.021(5) -0.002(4) 0.003(3) -0.003(3) S3 0.0270(12) 0.0244(13) 0.0283(16) -0.0034(11) -0.0049(11) 0.0028(10) N4 0.023(4) 0.034(5) 0.034(6) -0.001(4) -0.001(4) 0.001(4) S4 0.0246(13) 0.0334(15) 0.0333(16) 0.0023(13) 0.0028(11) 0.0059(11) Ir3 0.02690(19) 0.01640(18) 0.0190(2) 0.00065(17) 0.00174(17) 0.00322(16) C41 0.042(6) 0.017(5) 0.021(6) -0.005(5) -0.003(5) 0.000(5) C42 0.039(6) 0.029(6) 0.018(6) 0.002(5) -0.009(5) 0.001(5) C43 0.039(6) 0.033(6) 0.019(6) -0.009(5) 0.005(5) -0.002(5) C44 0.052(7) 0.020(5) 0.016(6) -0.009(5) 0.004(5) 0.004(5) C45 0.049(7) 0.034(6) 0.014(6) -0.003(5) 0.005(5) 0.000(5) C46 0.061(8) 0.024(6) 0.030(7) 0.004(5) -0.005(6) 0.005(6) C47 0.030(6) 0.035(7) 0.044(7) -0.017(5) -0.015(5) 0.005(5) C48 0.053(7) 0.040(7) 0.019(6) 0.008(5) 0.007(5) -0.007(6) C49 0.073(9) 0.014(5) 0.030(7) 0.004(5) 0.006(6) 0.006(6) C50 0.040(7) 0.040(7) 0.036(8) -0.008(6) 0.020(6) 0.006(6) Cl1 0.0445(16) 0.0381(15) 0.0295(16) -0.0060(13) -0.0069(13) 0.0094(13) O1 0.132(11) 0.138(12) 0.052(8) 0.025(7) 0.049(7) 0.085(9) O2 0.057(6) 0.064(6) 0.041(6) -0.006(5) -0.022(4) 0.020(5) O3 0.115(9) 0.068(7) 0.090(9) 0.037(6) -0.068(8) -0.036(7) O4 0.085(7) 0.039(5) 0.072(7) -0.017(5) -0.035(6) 0.025(5) Cl2 0.0302(14) 0.0378(15) 0.0282(15) -0.0050(12) -0.0004(11) -0.0004(12) O5 0.071(6) 0.032(5) 0.043(5) -0.006(4) 0.012(4) -0.020(4) O6 0.035(5) 0.076(7) 0.046(6) -0.010(5) 0.000(4) 0.015(5) O7 0.101(8) 0.043(6) 0.108(9) -0.009(6) -0.069(7) 0.021(6) O8 0.061(6) 0.178(13) 0.033(6) -0.012(7) 0.014(5) -0.034(8) C60 0.056(8) 0.042(7) 0.077(11) 0.011(8) -0.016(8) 0.001(6) Cl3 0.060(2) 0.062(2) 0.075(3) -0.007(2) 0.0044(19) 0.0098(17) Cl4 0.078(3) 0.072(3) 0.090(3) -0.017(2) 0.026(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 S1 1.584(9) . ? N1 Ir1 1.983(8) . ? N1 Au1 2.066(8) . ? C31 C32 1.427(15) . ? C31 C35 1.444(16) . ? C31 C36 1.496(16) . ? C31 Ir1 2.182(10) . ? C32 C33 1.427(15) . ? C32 C37 1.502(15) . ? C32 Ir1 2.173(10) . ? C33 C38 1.457(15) . ? C33 C34 1.470(15) . ? C33 Ir1 2.189(9) . ? C34 C35 1.436(16) . ? C34 C39 1.495(16) . ? C34 Ir1 2.202(11) . ? C35 C40 1.493(16) . ? C35 Ir1 2.251(11) . ? Ir1 S2 2.183(3) . ? S2 N2 1.665(9) . ? N2 S1 1.560(9) . ? Au1 P1 2.253(3) . ? Au1 Au3 3.1930(9) . ? P1 C1 1.807(11) . ? P1 C7 1.800(10) . ? P1 C13 1.840(10) . ? C1 C6 1.392(15) . ? C1 C2 1.394(16) . ? C2 C3 1.430(16) . ? C3 C4 1.358(18) . ? C4 C5 1.389(19) . ? C5 C6 1.376(16) . ? C7 C12 1.363(15) . ? C7 C8 1.414(15) . ? C8 C9 1.363(16) . ? C9 C10 1.41(2) . ? C10 C11 1.372(19) . ? C11 C12 1.374(16) . ? C13 P3 1.811(10) . ? C14 C15 1.381(16) . ? C14 C19 1.403(15) . ? C14 P3 1.826(10) . ? C15 C16 1.373(16) . ? C16 C17 1.356(19) . ? C17 C18 1.37(2) . ? C18 C19 1.405(19) . ? C20 C25 1.344(17) . ? C20 C21 1.409(16) . ? C20 P3 1.813(10) . ? C21 C22 1.369(17) . ? C22 C23 1.34(2) . ? C23 C24 1.402(19) . ? C24 C25 1.417(16) . ? P3 Au3 2.249(3) . ? Au3 N3 2.058(8) . ? N3 S3 1.608(8) . ? N3 Ir3 1.983(8) . ? S3 N4 1.564(8) . ? N4 S4 1.667(9) . ? S4 Ir3 2.203(3) . ? Ir3 C44 2.136(10) . ? Ir3 C45 2.157(11) . ? Ir3 C41 2.171(11) . ? Ir3 C43 2.200(11) . ? Ir3 C42 2.239(11) . ? C41 C45 1.443(15) . ? C41 C42 1.456(15) . ? C41 C46 1.475(15) . ? C42 C43 1.416(16) . ? C42 C47 1.516(15) . ? C43 C44 1.441(15) . ? C43 C48 1.506(15) . ? C44 C45 1.410(16) . ? C44 C49 1.510(15) . ? C45 C50 1.518(15) . ? Cl1 O3 1.401(10) . ? Cl1 O1 1.408(11) . ? Cl1 O4 1.416(9) . ? Cl1 O2 1.445(9) . ? Cl2 O8 1.397(10) . ? Cl2 O6 1.400(8) . ? Cl2 O7 1.426(10) . ? Cl2 O5 1.433(8) . ? C60 Cl3 1.756(13) . ? C60 Cl4 1.756(18) . ? 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 N1 Ir1 119.7(4) . . ? S1 N1 Au1 115.4(4) . . ? Ir1 N1 Au1 124.8(4) . . ? C32 C31 C35 110.2(9) . . ? C32 C31 C36 125.2(10) . . ? C35 C31 C36 124.4(10) . . ? C32 C31 Ir1 70.5(6) . . ? C35 C31 Ir1 73.6(6) . . ? C36 C31 Ir1 126.8(8) . . ? C31 C32 C33 107.8(9) . . ? C31 C32 C37 126.2(10) . . ? C33 C32 C37 126.0(10) . . ? C31 C32 Ir1 71.2(6) . . ? C33 C32 Ir1 71.5(6) . . ? C37 C32 Ir1 125.2(7) . . ? C32 C33 C38 129.1(10) . . ? C32 C33 C34 107.3(9) . . ? C38 C33 C34 123.6(10) . . ? C32 C33 Ir1 70.3(6) . . ? C38 C33 Ir1 125.1(8) . . ? C34 C33 Ir1 71.0(6) . . ? C35 C34 C33 108.7(10) . . ? C35 C34 C39 124.8(10) . . ? C33 C34 C39 126.4(11) . . ? C35 C34 Ir1 73.0(6) . . ? C33 C34 Ir1 69.9(6) . . ? C39 C34 Ir1 125.4(7) . . ? C34 C35 C31 106.0(9) . . ? C34 C35 C40 127.3(11) . . ? C31 C35 C40 126.8(11) . . ? C34 C35 Ir1 69.4(6) . . ? C31 C35 Ir1 68.4(6) . . ? C40 C35 Ir1 128.2(8) . . ? N1 Ir1 C32 168.3(4) . . ? N1 Ir1 C31 130.1(4) . . ? C32 Ir1 C31 38.3(4) . . ? N1 Ir1 C33 146.4(4) . . ? C32 Ir1 C33 38.2(4) . . ? C31 Ir1 C33 63.7(4) . . ? N1 Ir1 S2 86.1(2) . . ? C32 Ir1 S2 101.8(3) . . ? C31 Ir1 S2 126.4(3) . . ? C33 Ir1 S2 110.0(3) . . ? N1 Ir1 C34 113.4(4) . . ? C32 Ir1 C34 64.4(4) . . ? C31 Ir1 C34 63.3(4) . . ? C33 Ir1 C34 39.1(4) . . ? S2 Ir1 C34 145.1(3) . . ? N1 Ir1 C35 106.6(3) . . ? C32 Ir1 C35 64.3(4) . . ? C31 Ir1 C35 38.0(4) . . ? C33 Ir1 C35 64.3(4) . . ? S2 Ir1 C35 164.3(3) . . ? C34 Ir1 C35 37.6(4) . . ? N2 S2 Ir1 107.5(3) . . ? S1 N2 S2 116.3(5) . . ? N2 S1 N1 110.3(4) . . ? N1 Au1 P1 172.1(2) . . ? N1 Au1 Au3 97.2(2) . . ? P1 Au1 Au3 88.46(7) . . ? C1 P1 C7 106.2(5) . . ? C1 P1 C13 105.7(5) . . ? C7 P1 C13 106.4(5) . . ? C1 P1 Au1 109.3(3) . . ? C7 P1 Au1 114.7(3) . . ? C13 P1 Au1 113.9(3) . . ? C6 C1 C2 119.3(10) . . ? C6 C1 P1 118.0(9) . . ? C2 C1 P1 122.2(8) . . ? C1 C2 C3 119.2(10) . . ? C4 C3 C2 120.2(12) . . ? C3 C4 C5 120.1(12) . . ? C6 C5 C4 120.8(12) . . ? C5 C6 C1 120.5(12) . . ? C12 C7 C8 117.5(10) . . ? C12 C7 P1 121.5(8) . . ? C8 C7 P1 121.0(8) . . ? C9 C8 C7 123.0(12) . . ? C8 C9 C10 117.4(12) . . ? C11 C10 C9 120.0(11) . . ? C10 C11 C12 121.0(12) . . ? C7 C12 C11 121.0(11) . . ? P3 C13 P1 114.8(6) . . ? C15 C14 C19 118.3(10) . . ? C15 C14 P3 122.3(8) . . ? C19 C14 P3 119.4(9) . . ? C14 C15 C16 120.8(11) . . ? C17 C16 C15 121.8(14) . . ? C18 C17 C16 118.9(13) . . ? C17 C18 C19 121.2(13) . . ? C18 C19 C14 119.0(13) . . ? C25 C20 C21 120.5(10) . . ? C25 C20 P3 119.1(8) . . ? C21 C20 P3 120.3(10) . . ? C22 C21 C20 119.2(13) . . ? C23 C22 C21 121.2(12) . . ? C22 C23 C24 120.8(12) . . ? C23 C24 C25 118.0(13) . . ? C20 C25 C24 120.2(11) . . ? C20 P3 C13 106.0(5) . . ? C20 P3 C14 106.3(5) . . ? C13 P3 C14 103.8(5) . . ? C20 P3 Au3 115.1(4) . . ? C13 P3 Au3 111.2(4) . . ? C14 P3 Au3 113.5(3) . . ? N3 Au3 P3 174.9(2) . . ? N3 Au3 Au1 92.8(2) . . ? P3 Au3 Au1 88.13(7) . . ? S3 N3 Ir3 119.8(4) . . ? S3 N3 Au3 110.8(4) . . ? Ir3 N3 Au3 129.3(4) . . ? N4 S3 N3 110.3(5) . . ? S3 N4 S4 116.1(5) . . ? N4 S4 Ir3 107.9(3) . . ? N3 Ir3 C44 138.3(4) . . ? N3 Ir3 C45 172.4(4) . . ? C44 Ir3 C45 38.3(4) . . ? N3 Ir3 C41 136.0(3) . . ? C44 Ir3 C41 65.1(4) . . ? C45 Ir3 C41 39.0(4) . . ? N3 Ir3 S4 85.8(2) . . ? C44 Ir3 S4 114.2(3) . . ? C45 Ir3 S4 101.7(3) . . ? C41 Ir3 S4 121.8(3) . . ? N3 Ir3 C43 109.2(4) . . ? C44 Ir3 C43 38.8(4) . . ? C45 Ir3 C43 64.1(4) . . ? C41 Ir3 C43 64.4(4) . . ? S4 Ir3 C43 150.6(3) . . ? N3 Ir3 C42 108.9(4) . . ? C44 Ir3 C42 63.6(4) . . ? C45 Ir3 C42 63.7(4) . . ? C41 Ir3 C42 38.5(4) . . ? S4 Ir3 C42 160.2(3) . . ? C43 Ir3 C42 37.2(4) . . ? C45 C41 C42 106.5(9) . . ? C45 C41 C46 127.2(10) . . ? C42 C41 C46 125.8(10) . . ? C45 C41 Ir3 70.0(6) . . ? C42 C41 Ir3 73.3(6) . . ? C46 C41 Ir3 128.4(7) . . ? C43 C42 C41 108.4(9) . . ? C43 C42 C47 127.8(10) . . ? C41 C42 C47 123.8(10) . . ? C43 C42 Ir3 69.9(6) . . ? C41 C42 Ir3 68.2(6) . . ? C47 C42 Ir3 128.1(8) . . ? C42 C43 C44 107.8(10) . . ? C42 C43 C48 126.2(10) . . ? C44 C43 C48 125.9(10) . . ? C42 C43 Ir3 72.9(6) . . ? C44 C43 Ir3 68.2(6) . . ? C48 C43 Ir3 126.2(8) . . ? C45 C44 C43 108.5(10) . . ? C45 C44 C49 127.0(10) . . ? C43 C44 C49 124.2(10) . . ? C45 C44 Ir3 71.6(6) . . ? C43 C44 Ir3 73.0(6) . . ? C49 C44 Ir3 125.7(8) . . ? C44 C45 C41 108.6(9) . . ? C44 C45 C50 127.6(10) . . ? C41 C45 C50 123.8(10) . . ? C44 C45 Ir3 70.0(6) . . ? C41 C45 Ir3 71.0(6) . . ? C50 C45 Ir3 126.2(8) . . ? O3 Cl1 O1 110.3(10) . . ? O3 Cl1 O4 106.7(7) . . ? O1 Cl1 O4 112.1(8) . . ? O3 Cl1 O2 107.1(6) . . ? O1 Cl1 O2 109.7(7) . . ? O4 Cl1 O2 110.8(6) . . ? O8 Cl2 O6 110.5(6) . . ? O8 Cl2 O7 106.8(9) . . ? O6 Cl2 O7 107.5(7) . . ? O8 Cl2 O5 112.9(7) . . ? O6 Cl2 O5 111.6(6) . . ? O7 Cl2 O5 107.3(6) . . ? Cl3 C60 Cl4 110.4(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C35 C31 C32 C33 0.8(12) . . . . ? C36 C31 C32 C33 175.6(10) . . . . ? Ir1 C31 C32 C33 -62.5(7) . . . . ? C35 C31 C32 C37 -176.4(10) . . . . ? C36 C31 C32 C37 -1.5(17) . . . . ? Ir1 C31 C32 C37 120.3(11) . . . . ? C35 C31 C32 Ir1 63.3(7) . . . . ? C36 C31 C32 Ir1 -121.9(11) . . . . ? C31 C32 C33 C38 -177.8(11) . . . . ? C37 C32 C33 C38 -0.7(18) . . . . ? Ir1 C32 C33 C38 119.8(12) . . . . ? C31 C32 C33 C34 0.6(12) . . . . ? C37 C32 C33 C34 177.8(10) . . . . ? Ir1 C32 C33 C34 -61.7(7) . . . . ? C31 C32 C33 Ir1 62.3(7) . . . . ? C37 C32 C33 Ir1 -120.5(11) . . . . ? C32 C33 C34 C35 -1.8(12) . . . . ? C38 C33 C34 C35 176.8(10) . . . . ? Ir1 C33 C34 C35 -63.1(7) . . . . ? C32 C33 C34 C39 -178.9(10) . . . . ? C38 C33 C34 C39 -0.4(17) . . . . ? Ir1 C33 C34 C39 119.8(11) . . . . ? C32 C33 C34 Ir1 61.3(7) . . . . ? C38 C33 C34 Ir1 -120.1(11) . . . . ? C33 C34 C35 C31 2.2(11) . . . . ? C39 C34 C35 C31 179.4(10) . . . . ? Ir1 C34 C35 C31 -58.9(7) . . . . ? C33 C34 C35 C40 -175.9(10) . . . . ? C39 C34 C35 C40 1.3(18) . . . . ? Ir1 C34 C35 C40 122.9(11) . . . . ? C33 C34 C35 Ir1 61.2(7) . . . . ? C39 C34 C35 Ir1 -121.7(10) . . . . ? C32 C31 C35 C34 -1.9(12) . . . . ? C36 C31 C35 C34 -176.8(10) . . . . ? Ir1 C31 C35 C34 59.5(7) . . . . ? C32 C31 C35 C40 176.3(11) . . . . ? C36 C31 C35 C40 1.3(18) . . . . ? Ir1 C31 C35 C40 -122.3(11) . . . . ? C32 C31 C35 Ir1 -61.4(7) . . . . ? C36 C31 C35 Ir1 123.7(11) . . . . ? S1 N1 Ir1 C32 135.5(16) . . . . ? Au1 N1 Ir1 C32 -47(2) . . . . ? S1 N1 Ir1 C31 138.4(5) . . . . ? Au1 N1 Ir1 C31 -43.7(7) . . . . ? S1 N1 Ir1 C33 -118.8(7) . . . . ? Au1 N1 Ir1 C33 59.1(9) . . . . ? S1 N1 Ir1 S2 2.4(5) . . . . ? Au1 N1 Ir1 S2 -179.7(4) . . . . ? S1 N1 Ir1 C34 -147.6(5) . . . . ? Au1 N1 Ir1 C34 30.3(6) . . . . ? S1 N1 Ir1 C35 172.9(5) . . . . ? Au1 N1 Ir1 C35 -9.2(6) . . . . ? C31 C32 Ir1 N1 4(2) . . . . ? C33 C32 Ir1 N1 120.6(17) . . . . ? C37 C32 Ir1 N1 -117.9(17) . . . . ? C33 C32 Ir1 C31 117.0(9) . . . . ? C37 C32 Ir1 C31 -121.5(12) . . . . ? C31 C32 Ir1 C33 -117.0(9) . . . . ? C37 C32 Ir1 C33 121.5(12) . . . . ? C31 C32 Ir1 S2 135.5(6) . . . . ? C33 C32 Ir1 S2 -107.4(6) . . . . ? C37 C32 Ir1 S2 14.0(9) . . . . ? C31 C32 Ir1 C34 -78.6(7) . . . . ? C33 C32 Ir1 C34 38.5(6) . . . . ? C37 C32 Ir1 C34 159.9(11) . . . . ? C31 C32 Ir1 C35 -36.7(6) . . . . ? C33 C32 Ir1 C35 80.4(7) . . . . ? C37 C32 Ir1 C35 -158.2(10) . . . . ? C32 C31 Ir1 N1 -179.1(6) . . . . ? C35 C31 Ir1 N1 61.9(7) . . . . ? C36 C31 Ir1 N1 -59.1(11) . . . . ? C35 C31 Ir1 C32 -119.1(9) . . . . ? C36 C31 Ir1 C32 120.0(13) . . . . ? C32 C31 Ir1 C33 37.9(6) . . . . ? C35 C31 Ir1 C33 -81.2(7) . . . . ? C36 C31 Ir1 C33 157.9(11) . . . . ? C32 C31 Ir1 S2 -58.4(7) . . . . ? C35 C31 Ir1 S2 -177.5(5) . . . . ? C36 C31 Ir1 S2 61.6(10) . . . . ? C32 C31 Ir1 C34 81.8(7) . . . . ? C35 C31 Ir1 C34 -37.2(6) . . . . ? C36 C31 Ir1 C34 -158.2(11) . . . . ? C32 C31 Ir1 C35 119.1(9) . . . . ? C36 C31 Ir1 C35 -120.9(12) . . . . ? C32 C33 Ir1 N1 -161.6(7) . . . . ? C38 C33 Ir1 N1 73.8(12) . . . . ? C34 C33 Ir1 N1 -44.5(10) . . . . ? C38 C33 Ir1 C32 -124.6(12) . . . . ? C34 C33 Ir1 C32 117.2(9) . . . . ? C32 C33 Ir1 C31 -38.0(6) . . . . ? C38 C33 Ir1 C31 -162.5(11) . . . . ? C34 C33 Ir1 C31 79.2(7) . . . . ? C32 C33 Ir1 S2 83.7(6) . . . . ? C38 C33 Ir1 S2 -40.9(10) . . . . ? C34 C33 Ir1 S2 -159.2(5) . . . . ? C32 C33 Ir1 C34 -117.2(9) . . . . ? C38 C33 Ir1 C34 118.2(12) . . . . ? C32 C33 Ir1 C35 -80.4(7) . . . . ? C38 C33 Ir1 C35 155.0(11) . . . . ? C34 C33 Ir1 C35 36.7(6) . . . . ? C35 C34 Ir1 N1 -87.0(6) . . . . ? C33 C34 Ir1 N1 155.0(6) . . . . ? C39 C34 Ir1 N1 34.0(11) . . . . ? C35 C34 Ir1 C32 80.4(7) . . . . ? C33 C34 Ir1 C32 -37.6(6) . . . . ? C39 C34 Ir1 C32 -158.6(11) . . . . ? C35 C34 Ir1 C31 37.6(6) . . . . ? C33 C34 Ir1 C31 -80.4(7) . . . . ? C39 C34 Ir1 C31 158.6(11) . . . . ? C35 C34 Ir1 C33 118.0(9) . . . . ? C39 C34 Ir1 C33 -121.0(13) . . . . ? C35 C34 Ir1 S2 153.7(5) . . . . ? C33 C34 Ir1 S2 35.7(9) . . . . ? C39 C34 Ir1 S2 -85.3(11) . . . . ? C33 C34 Ir1 C35 -118.0(9) . . . . ? C39 C34 Ir1 C35 121.0(12) . . . . ? C34 C35 Ir1 N1 107.1(6) . . . . ? C31 C35 Ir1 N1 -135.3(6) . . . . ? C40 C35 Ir1 N1 -14.7(12) . . . . ? C34 C35 Ir1 C32 -80.8(6) . . . . ? C31 C35 Ir1 C32 36.9(6) . . . . ? C40 C35 Ir1 C32 157.4(12) . . . . ? C34 C35 Ir1 C31 -117.7(8) . . . . ? C40 C35 Ir1 C31 120.5(14) . . . . ? C34 C35 Ir1 C33 -38.2(6) . . . . ? C31 C35 Ir1 C33 79.5(6) . . . . ? C40 C35 Ir1 C33 -160.0(12) . . . . ? C34 C35 Ir1 S2 -110.2(11) . . . . ? C31 C35 Ir1 S2 7.4(14) . . . . ? C40 C35 Ir1 S2 127.9(11) . . . . ? C31 C35 Ir1 C34 117.7(8) . . . . ? C40 C35 Ir1 C34 -121.8(14) . . . . ? N1 Ir1 S2 N2 -1.6(4) . . . . ? C32 Ir1 S2 N2 -173.0(5) . . . . ? C31 Ir1 S2 N2 -140.4(5) . . . . ? C33 Ir1 S2 N2 148.1(5) . . . . ? C34 Ir1 S2 N2 125.1(6) . . . . ? C35 Ir1 S2 N2 -146.0(11) . . . . ? Ir1 S2 N2 S1 0.8(7) . . . . ? S2 N2 S1 N1 0.8(8) . . . . ? Ir1 N1 S1 N2 -2.4(7) . . . . ? Au1 N1 S1 N2 179.5(5) . . . . ? S1 N1 Au1 P1 158.9(13) . . . . ? Ir1 N1 Au1 P1 -19(2) . . . . ? S1 N1 Au1 Au3 -66.2(4) . . . . ? Ir1 N1 Au1 Au3 115.8(4) . . . . ? N1 Au1 P1 C1 -0.2(18) . . . . ? Au3 Au1 P1 C1 -135.6(4) . . . . ? N1 Au1 P1 C7 -119.3(17) . . . . ? Au3 Au1 P1 C7 105.4(4) . . . . ? N1 Au1 P1 C13 117.7(17) . . . . ? Au3 Au1 P1 C13 -17.6(4) . . . . ? C7 P1 C1 C6 51.9(9) . . . . ? C13 P1 C1 C6 164.7(8) . . . . ? Au1 P1 C1 C6 -72.3(9) . . . . ? C7 P1 C1 C2 -136.6(9) . . . . ? C13 P1 C1 C2 -23.8(10) . . . . ? Au1 P1 C1 C2 99.2(9) . . . . ? C6 C1 C2 C3 2.3(16) . . . . ? P1 C1 C2 C3 -169.0(9) . . . . ? C1 C2 C3 C4 -1.4(18) . . . . ? C2 C3 C4 C5 -0.4(19) . . . . ? C3 C4 C5 C6 1.3(18) . . . . ? C4 C5 C6 C1 -0.4(16) . . . . ? C2 C1 C6 C5 -1.5(16) . . . . ? P1 C1 C6 C5 170.3(8) . . . . ? C1 P1 C7 C12 -119.8(10) . . . . ? C13 P1 C7 C12 128.0(10) . . . . ? Au1 P1 C7 C12 1.0(11) . . . . ? C1 P1 C7 C8 62.7(10) . . . . ? C13 P1 C7 C8 -49.6(11) . . . . ? Au1 P1 C7 C8 -176.5(8) . . . . ? C12 C7 C8 C9 -0.3(19) . . . . ? P1 C7 C8 C9 177.3(10) . . . . ? C7 C8 C9 C10 -1(2) . . . . ? C8 C9 C10 C11 2(2) . . . . ? C9 C10 C11 C12 -2.2(19) . . . . ? C8 C7 C12 C11 -0.1(17) . . . . ? P1 C7 C12 C11 -177.7(8) . . . . ? C10 C11 C12 C7 1.3(18) . . . . ? C1 P1 C13 P3 168.2(6) . . . . ? C7 P1 C13 P3 -79.2(6) . . . . ? Au1 P1 C13 P3 48.3(6) . . . . ? C19 C14 C15 C16 0.6(16) . . . . ? P3 C14 C15 C16 179.1(9) . . . . ? C14 C15 C16 C17 0.3(18) . . . . ? C15 C16 C17 C18 -1.4(19) . . . . ? C16 C17 C18 C19 2(2) . . . . ? C17 C18 C19 C14 -0.7(18) . . . . ? C15 C14 C19 C18 -0.4(15) . . . . ? P3 C14 C19 C18 -179.0(9) . . . . ? C25 C20 C21 C22 1.3(18) . . . . ? P3 C20 C21 C22 -176.8(9) . . . . ? C20 C21 C22 C23 -2(2) . . . . ? C21 C22 C23 C24 3(2) . . . . ? C22 C23 C24 C25 -3(2) . . . . ? C21 C20 C25 C24 -1.8(17) . . . . ? P3 C20 C25 C24 176.4(9) . . . . ? C23 C24 C25 C20 2.6(18) . . . . ? C25 C20 P3 C13 -101.2(9) . . . . ? C21 C20 P3 C13 77.0(10) . . . . ? C25 C20 P3 C14 148.8(9) . . . . ? C21 C20 P3 C14 -33.1(10) . . . . ? C25 C20 P3 Au3 22.1(10) . . . . ? C21 C20 P3 Au3 -159.7(8) . . . . ? P1 C13 P3 C20 68.9(7) . . . . ? P1 C13 P3 C14 -179.3(5) . . . . ? P1 C13 P3 Au3 -56.9(6) . . . . ? C15 C14 P3 C20 139.5(9) . . . . ? C19 C14 P3 C20 -42.0(9) . . . . ? C15 C14 P3 C13 28.0(9) . . . . ? C19 C14 P3 C13 -153.5(8) . . . . ? C15 C14 P3 Au3 -92.9(8) . . . . ? C19 C14 P3 Au3 85.6(8) . . . . ? C20 P3 Au3 N3 171(3) . . . . ? C13 P3 Au3 N3 -68(3) . . . . ? C14 P3 Au3 N3 48(3) . . . . ? C20 P3 Au3 Au1 -87.5(4) . . . . ? C13 P3 Au3 Au1 33.0(4) . . . . ? C14 P3 Au3 Au1 149.6(4) . . . . ? N1 Au1 Au3 N3 -7.4(3) . . . . ? P1 Au1 Au3 N3 167.0(2) . . . . ? N1 Au1 Au3 P3 177.5(3) . . . . ? P1 Au1 Au3 P3 -8.07(10) . . . . ? P3 Au3 N3 S3 33(3) . . . . ? Au1 Au3 N3 S3 -68.4(4) . . . . ? P3 Au3 N3 Ir3 -152(2) . . . . ? Au1 Au3 N3 Ir3 107.2(5) . . . . ? Ir3 N3 S3 N4 -1.8(7) . . . . ? Au3 N3 S3 N4 174.4(4) . . . . ? N3 S3 N4 S4 -0.7(7) . . . . ? S3 N4 S4 Ir3 2.5(6) . . . . ? S3 N3 Ir3 C44 -119.7(6) . . . . ? Au3 N3 Ir3 C44 65.0(8) . . . . ? S3 N3 Ir3 C45 -179(3) . . . . ? Au3 N3 Ir3 C45 6(3) . . . . ? S3 N3 Ir3 C41 135.8(5) . . . . ? Au3 N3 Ir3 C41 -39.5(8) . . . . ? S3 N3 Ir3 S4 2.6(5) . . . . ? Au3 N3 Ir3 S4 -172.7(5) . . . . ? S3 N3 Ir3 C43 -151.5(5) . . . . ? Au3 N3 Ir3 C43 33.1(6) . . . . ? S3 N3 Ir3 C42 169.1(5) . . . . ? Au3 N3 Ir3 C42 -6.3(6) . . . . ? N4 S4 Ir3 N3 -2.7(4) . . . . ? N4 S4 Ir3 C44 139.3(5) . . . . ? N4 S4 Ir3 C45 177.6(5) . . . . ? N4 S4 Ir3 C41 -146.1(4) . . . . ? N4 S4 Ir3 C43 120.2(7) . . . . ? N4 S4 Ir3 C42 -141.7(9) . . . . ? N3 Ir3 C41 C45 171.5(6) . . . . ? C44 Ir3 C41 C45 36.8(6) . . . . ? S4 Ir3 C41 C45 -67.3(6) . . . . ? C43 Ir3 C41 C45 79.8(7) . . . . ? C42 Ir3 C41 C45 115.1(9) . . . . ? N3 Ir3 C41 C42 56.4(8) . . . . ? C44 Ir3 C41 C42 -78.3(7) . . . . ? C45 Ir3 C41 C42 -115.1(9) . . . . ? S4 Ir3 C41 C42 177.6(5) . . . . ? C43 Ir3 C41 C42 -35.3(6) . . . . ? N3 Ir3 C41 C46 -66.4(12) . . . . ? C44 Ir3 C41 C46 158.9(11) . . . . ? C45 Ir3 C41 C46 122.1(13) . . . . ? S4 Ir3 C41 C46 54.8(11) . . . . ? C43 Ir3 C41 C46 -158.0(11) . . . . ? C42 Ir3 C41 C46 -122.8(12) . . . . ? C45 C41 C42 C43 -4.1(12) . . . . ? C46 C41 C42 C43 -175.8(10) . . . . ? Ir3 C41 C42 C43 58.5(8) . . . . ? C45 C41 C42 C47 175.3(10) . . . . ? C46 C41 C42 C47 3.6(17) . . . . ? Ir3 C41 C42 C47 -122.1(10) . . . . ? C45 C41 C42 Ir3 -62.6(7) . . . . ? C46 C41 C42 Ir3 125.7(11) . . . . ? N3 Ir3 C42 C43 97.2(7) . . . . ? C44 Ir3 C42 C43 -38.1(6) . . . . ? C45 Ir3 C42 C43 -81.1(7) . . . . ? C41 Ir3 C42 C43 -120.5(9) . . . . ? S4 Ir3 C42 C43 -126.5(8) . . . . ? N3 Ir3 C42 C41 -142.3(6) . . . . ? C44 Ir3 C42 C41 82.4(6) . . . . ? C45 Ir3 C42 C41 39.4(6) . . . . ? S4 Ir3 C42 C41 -6.0(12) . . . . ? C43 Ir3 C42 C41 120.5(9) . . . . ? N3 Ir3 C42 C47 -25.7(11) . . . . ? C44 Ir3 C42 C47 -161.0(11) . . . . ? C45 Ir3 C42 C47 156.0(11) . . . . ? C41 Ir3 C42 C47 116.6(12) . . . . ? S4 Ir3 C42 C47 110.6(11) . . . . ? C43 Ir3 C42 C47 -122.9(13) . . . . ? C41 C42 C43 C44 2.1(13) . . . . ? C47 C42 C43 C44 -177.3(10) . . . . ? Ir3 C42 C43 C44 59.5(8) . . . . ? C41 C42 C43 C48 179.8(10) . . . . ? C47 C42 C43 C48 0.5(19) . . . . ? Ir3 C42 C43 C48 -122.8(12) . . . . ? C41 C42 C43 Ir3 -57.4(7) . . . . ? C47 C42 C43 Ir3 123.2(11) . . . . ? N3 Ir3 C43 C42 -96.2(7) . . . . ? C44 Ir3 C43 C42 117.9(10) . . . . ? C45 Ir3 C43 C42 79.9(7) . . . . ? C41 Ir3 C43 C42 36.5(6) . . . . ? S4 Ir3 C43 C42 146.3(6) . . . . ? N3 Ir3 C43 C44 145.9(6) . . . . ? C45 Ir3 C43 C44 -38.0(6) . . . . ? C41 Ir3 C43 C44 -81.4(7) . . . . ? S4 Ir3 C43 C44 28.4(10) . . . . ? C42 Ir3 C43 C44 -117.9(10) . . . . ? N3 Ir3 C43 C48 26.6(11) . . . . ? C44 Ir3 C43 C48 -119.3(13) . . . . ? C45 Ir3 C43 C48 -157.3(11) . . . . ? C41 Ir3 C43 C48 159.3(11) . . . . ? S4 Ir3 C43 C48 -90.9(10) . . . . ? C42 Ir3 C43 C48 122.8(12) . . . . ? C42 C43 C44 C45 0.8(13) . . . . ? C48 C43 C44 C45 -177.0(11) . . . . ? Ir3 C43 C44 C45 63.3(8) . . . . ? C42 C43 C44 C49 175.4(10) . . . . ? C48 C43 C44 C49 -2.3(18) . . . . ? Ir3 C43 C44 C49 -122.0(11) . . . . ? C42 C43 C44 Ir3 -62.5(8) . . . . ? C48 C43 C44 Ir3 119.8(11) . . . . ? N3 Ir3 C44 C45 -169.5(6) . . . . ? C41 Ir3 C44 C45 -37.3(6) . . . . ? S4 Ir3 C44 C45 78.0(7) . . . . ? C43 Ir3 C44 C45 -116.8(9) . . . . ? C42 Ir3 C44 C45 -80.2(7) . . . . ? N3 Ir3 C44 C43 -52.7(9) . . . . ? C45 Ir3 C44 C43 116.8(9) . . . . ? C41 Ir3 C44 C43 79.5(7) . . . . ? S4 Ir3 C44 C43 -165.2(5) . . . . ? C42 Ir3 C44 C43 36.6(7) . . . . ? N3 Ir3 C44 C49 67.6(12) . . . . ? C45 Ir3 C44 C49 -122.9(13) . . . . ? C41 Ir3 C44 C49 -160.2(11) . . . . ? S4 Ir3 C44 C49 -44.9(10) . . . . ? C43 Ir3 C44 C49 120.3(12) . . . . ? C42 Ir3 C44 C49 156.9(11) . . . . ? C43 C44 C45 C41 -3.4(12) . . . . ? C49 C44 C45 C41 -177.9(11) . . . . ? Ir3 C44 C45 C41 60.8(8) . . . . ? C43 C44 C45 C50 174.9(11) . . . . ? C49 C44 C45 C50 0.4(19) . . . . ? Ir3 C44 C45 C50 -120.9(12) . . . . ? C43 C44 C45 Ir3 -64.2(7) . . . . ? C49 C44 C45 Ir3 121.3(12) . . . . ? C42 C41 C45 C44 4.6(12) . . . . ? C46 C41 C45 C44 176.2(11) . . . . ? Ir3 C41 C45 C44 -60.2(8) . . . . ? C42 C41 C45 C50 -173.8(10) . . . . ? C46 C41 C45 C50 -2.2(18) . . . . ? Ir3 C41 C45 C50 121.4(11) . . . . ? C42 C41 C45 Ir3 64.8(7) . . . . ? C46 C41 C45 Ir3 -123.6(11) . . . . ? N3 Ir3 C45 C44 67(3) . . . . ? C41 Ir3 C45 C44 119.0(9) . . . . ? S4 Ir3 C45 C44 -114.3(6) . . . . ? C43 Ir3 C45 C44 38.4(7) . . . . ? C42 Ir3 C45 C44 80.0(7) . . . . ? N3 Ir3 C45 C41 -51(3) . . . . ? C44 Ir3 C45 C41 -119.0(9) . . . . ? S4 Ir3 C45 C41 126.8(6) . . . . ? C43 Ir3 C45 C41 -80.6(7) . . . . ? C42 Ir3 C45 C41 -39.0(6) . . . . ? N3 Ir3 C45 C50 -170(2) . . . . ? C44 Ir3 C45 C50 122.5(13) . . . . ? C41 Ir3 C45 C50 -118.5(12) . . . . ? S4 Ir3 C45 C50 8.3(10) . . . . ? C43 Ir3 C45 C50 161.0(11) . . . . ? C42 Ir3 C45 C50 -157.5(11) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.679 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.119 data_4 _database_code_CSD 213798 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [{(h5-C5H5)Co(S2N2)Au}2(m2-dppm)][ClO4]2 ; _chemical_name_common - _chemical_melting_point - _chemical_formula_moiety 'C35 H32 Au2 Cl2 Co2 N4 O8 P2 S4' _chemical_formula_sum 'C35 H32 Au2 Cl2 Co2 N4 O8 P2 S4' _chemical_formula_weight 1409.52 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.6124(17) _cell_length_b 12.5497(14) _cell_length_c 24.402(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.373(2) _cell_angle_gamma 90.00 _cell_volume 4447.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 61 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2696 _exptl_absorpt_coefficient_mu 7.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.781946 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details - _exptl_special_details ; - ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 18831 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 23.31 _reflns_number_total 6345 _reflns_number_gt 4182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 6345 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Au1 Au 1.02045(3) 0.17385(4) 0.10019(2) 0.02176(15) Uani 1 1 d . . . P1 P 1.1161(2) 0.2925(2) 0.14565(14) 0.0215(8) Uani 1 1 d . . . Co1 Co 0.83303(12) 0.10643(13) 0.00619(7) 0.0262(4) Uani 1 1 d . . . N1 N 0.9304(6) 0.0697(7) 0.0558(4) 0.021(2) Uani 1 1 d . . . S1 S 0.9538(2) -0.0521(3) 0.06705(14) 0.0277(8) Uani 1 1 d . . . C1 C 1.0734(8) 0.4262(9) 0.1358(5) 0.022(3) Uani 1 1 d . . . Cl1 Cl 0.8325(2) 0.0332(2) -0.19266(14) 0.0303(8) Uani 1 1 d . . . O1 O 0.8142(10) -0.0051(9) -0.1401(5) 0.085(4) Uani 1 1 d . . . S2 S 0.8003(3) -0.0540(3) -0.00650(16) 0.0396(10) Uani 1 1 d . . . N2 N 0.8791(8) -0.1233(8) 0.0322(5) 0.034(3) Uani 1 1 d . . . C2 C 0.9952(8) 0.4488(11) 0.0987(5) 0.027(3) Uani 1 1 d . . . H2A H 0.9622 0.3916 0.0803 0.032 Uiso 1 1 calc R . . Cl2 Cl 0.7996(3) -0.0129(4) 0.38831(17) 0.0512(11) Uani 1 1 d . . . O2 O 0.7654(8) -0.0123(9) -0.2304(6) 0.079(4) Uani 1 1 d . . . Au3 Au 0.91819(3) 0.15862(4) 0.20962(2) 0.02120(15) Uani 1 1 d . . . P3 P 1.0349(2) 0.2514(3) 0.25492(14) 0.0210(8) Uani 1 1 d . . . Co3 Co 0.79149(12) -0.07339(13) 0.18012(7) 0.0237(4) Uani 1 1 d . . . N3 N 0.8053(6) 0.0695(8) 0.1744(4) 0.024(3) Uani 1 1 d . . . S3 S 0.7329(2) 0.1393(2) 0.13808(14) 0.0269(8) Uani 1 1 d . . . C3 C 0.9661(11) 0.5475(11) 0.0886(6) 0.040(4) Uani 1 1 d . . . H3A H 0.9149 0.5592 0.0617 0.049 Uiso 1 1 calc R . . O3 O 0.8217(8) 0.1461(7) -0.1952(4) 0.058(3) Uani 1 1 d . . . S4 S 0.6730(2) -0.0643(3) 0.12403(15) 0.0331(9) Uani 1 1 d . . . N4 N 0.6586(7) 0.0628(8) 0.1087(4) 0.030(3) Uani 1 1 d . . . C4 C 1.0078(10) 0.6335(11) 0.1160(6) 0.040(4) Uani 1 1 d . . . H4A H 0.9863 0.7040 0.1083 0.048 Uiso 1 1 calc R . . O4 O 0.9189(8) -0.0007(9) -0.2072(7) 0.095(5) Uani 1 1 d . . . C5 C 1.0805(10) 0.6145(10) 0.1543(6) 0.037(4) Uani 1 1 d . . . H5A H 1.1092 0.6727 0.1743 0.044 Uiso 1 1 calc R . . O5 O 0.7793(14) 0.052(2) 0.4297(10) 0.248(16) Uani 1 1 d . . . C6 C 1.1137(10) 0.5131(10) 0.1649(6) 0.037(4) Uani 1 1 d . . . H6A H 1.1644 0.5021 0.1922 0.045 Uiso 1 1 calc R . . O6 O 0.8754(10) -0.0685(16) 0.4088(11) 0.218(14) Uani 1 1 d . . . C7 C 1.2282(9) 0.3005(9) 0.1221(6) 0.025(3) Uani 1 1 d . . . O7 O 0.8158(11) 0.0478(11) 0.3436(6) 0.117(6) Uani 1 1 d . . . C8 C 1.2351(9) 0.3055(10) 0.0666(6) 0.035(4) Uani 1 1 d . . . H8A H 1.1801 0.3006 0.0421 0.042 Uiso 1 1 calc R . . O8 O 0.7221(6) -0.0828(7) 0.3724(4) 0.042(3) Uani 1 1 d . . . C9 C 1.3168(10) 0.3172(10) 0.0443(6) 0.037(4) Uani 1 1 d . . . H9A H 1.3187 0.3177 0.0055 0.044 Uiso 1 1 calc R . . C10 C 1.3977(10) 0.3285(10) 0.0810(6) 0.035(4) Uani 1 1 d . . . H10A H 1.4551 0.3389 0.0669 0.042 Uiso 1 1 calc R . . C11 C 1.3946(9) 0.3247(10) 0.1366(7) 0.037(4) Uani 1 1 d . . . H11A H 1.4497 0.3308 0.1610 0.044 Uiso 1 1 calc R . . C12 C 1.3091(9) 0.3115(10) 0.1582(6) 0.030(3) Uani 1 1 d . . . H12A H 1.3067 0.3101 0.1969 0.036 Uiso 1 1 calc R . . C13 C 1.1385(8) 0.2640(9) 0.2191(5) 0.019(3) Uani 1 1 d . . . H13A H 1.1775 0.3217 0.2369 0.023 Uiso 1 1 calc R . . H13B H 1.1740 0.1968 0.2240 0.023 Uiso 1 1 calc R . . C14 C 1.0700(8) 0.1935(9) 0.3216(5) 0.022(3) Uani 1 1 d . . . C15 C 1.1544(9) 0.1463(10) 0.3367(6) 0.032(3) Uani 1 1 d . . . H15A H 1.1995 0.1443 0.3116 0.038 Uiso 1 1 calc R . . C16 C 1.1728(11) 0.1016(11) 0.3890(6) 0.040(4) Uani 1 1 d . . . H16A H 1.2314 0.0703 0.3992 0.048 Uiso 1 1 calc R . . C17 C 1.1099(10) 0.1015(10) 0.4255(5) 0.031(3) Uani 1 1 d . . . H17A H 1.1242 0.0691 0.4606 0.037 Uiso 1 1 calc R . . C18 C 1.0256(10) 0.1480(12) 0.4121(6) 0.046(4) Uani 1 1 d . . . H18A H 0.9812 0.1494 0.4377 0.056 Uiso 1 1 calc R . . C19 C 1.0067(10) 0.1933(13) 0.3601(6) 0.050(4) Uani 1 1 d . . . H19A H 0.9482 0.2253 0.3504 0.060 Uiso 1 1 calc R . . C20 C 1.0048(8) 0.3875(9) 0.2676(5) 0.021(3) Uani 1 1 d . . . C21 C 0.9301(8) 0.4335(10) 0.2363(5) 0.024(3) Uani 1 1 d . . . H21A H 0.8934 0.3920 0.2098 0.029 Uiso 1 1 calc R . . C22 C 0.9088(8) 0.5404(10) 0.2437(6) 0.030(3) Uani 1 1 d . . . H22A H 0.8574 0.5719 0.2225 0.036 Uiso 1 1 calc R . . C23 C 0.9635(10) 0.6006(11) 0.2826(6) 0.038(4) Uani 1 1 d . . . H23A H 0.9495 0.6736 0.2879 0.046 Uiso 1 1 calc R . . C24 C 1.0380(10) 0.5543(11) 0.3135(6) 0.038(4) Uani 1 1 d . . . H24A H 1.0751 0.5956 0.3399 0.046 Uiso 1 1 calc R . . C25 C 1.0592(8) 0.4473(10) 0.3060(6) 0.028(3) Uani 1 1 d . . . H25A H 1.1106 0.4158 0.3272 0.034 Uiso 1 1 calc R . . C26 C 0.7381(11) 0.1635(12) -0.0536(7) 0.050(4) Uani 1 1 d . . . H26A H 0.6960 0.1193 -0.0795 0.060 Uiso 1 1 calc R . . C27 C 0.8253(10) 0.1991(9) -0.0631(5) 0.032(4) Uani 1 1 d . . . H27A H 0.8566 0.1849 -0.0968 0.038 Uiso 1 1 calc R . . C28 C 0.8606(11) 0.2620(10) -0.0169(6) 0.034(4) Uani 1 1 d . . . H28A H 0.9226 0.2966 -0.0121 0.041 Uiso 1 1 calc R . . C29 C 0.7961(11) 0.2666(10) 0.0209(6) 0.038(4) Uani 1 1 d . . . H29A H 0.8033 0.3044 0.0572 0.046 Uiso 1 1 calc R . . C30 C 0.7183(10) 0.2020(11) -0.0012(6) 0.039(4) Uani 1 1 d . . . H30A H 0.6603 0.1897 0.0162 0.047 Uiso 1 1 calc R . . C31 C 0.7740(9) -0.2222(10) 0.2102(6) 0.034(4) Uani 1 1 d . . . H31A H 0.7149 -0.2631 0.2054 0.041 Uiso 1 1 calc R . . C32 C 0.8394(9) -0.2248(10) 0.1744(6) 0.034(4) Uani 1 1 d . . . H32A H 0.8368 -0.2684 0.1400 0.041 Uiso 1 1 calc R . . C33 C 0.9129(9) -0.1593(10) 0.1958(6) 0.032(3) Uani 1 1 d . . . H33A H 0.9707 -0.1465 0.1783 0.039 Uiso 1 1 calc R . . C34 C 0.8913(10) -0.1136(10) 0.2462(5) 0.030(3) Uani 1 1 d . . . H34A H 0.9302 -0.0633 0.2706 0.036 Uiso 1 1 calc R . . C35 C 0.8004(9) -0.1527(10) 0.2542(6) 0.029(3) Uani 1 1 d . . . H35A H 0.7651 -0.1366 0.2861 0.035 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 Au1 0.0218(3) 0.0175(3) 0.0249(3) -0.0002(2) -0.0019(2) -0.0026(2) P1 0.0200(19) 0.0158(17) 0.028(2) -0.0011(15) 0.0000(15) 0.0003(14) Co1 0.0314(11) 0.0210(10) 0.0245(11) 0.0013(8) -0.0041(8) -0.0035(8) N1 0.022(6) 0.023(6) 0.016(6) 0.001(4) -0.008(4) -0.010(5) S1 0.031(2) 0.0208(18) 0.031(2) -0.0001(15) 0.0012(16) 0.0013(16) C1 0.026(8) 0.010(7) 0.032(8) -0.001(6) 0.010(6) -0.001(6) Cl1 0.032(2) 0.0213(18) 0.034(2) -0.0045(15) -0.0099(16) 0.0059(15) O1 0.159(14) 0.046(7) 0.055(9) 0.015(6) 0.038(8) 0.023(8) S2 0.045(2) 0.025(2) 0.046(3) -0.0031(17) -0.0075(19) -0.0125(18) N2 0.039(7) 0.025(6) 0.039(8) -0.002(5) 0.005(6) 0.001(5) C2 0.008(7) 0.031(8) 0.040(9) 0.004(7) -0.005(6) 0.011(6) Cl2 0.034(2) 0.074(3) 0.043(3) 0.007(2) -0.0069(18) -0.006(2) O2 0.050(8) 0.070(8) 0.110(11) -0.038(8) -0.025(7) -0.003(7) Au3 0.0170(3) 0.0186(3) 0.0271(3) -0.0006(2) -0.0011(2) -0.0010(2) P3 0.0209(19) 0.0165(18) 0.025(2) -0.0021(14) -0.0020(15) 0.0006(15) Co3 0.0236(10) 0.0174(9) 0.0297(11) 0.0011(8) 0.0007(8) -0.0010(8) N3 0.014(6) 0.023(6) 0.033(7) 0.008(5) -0.009(5) -0.001(5) S3 0.0235(19) 0.0240(19) 0.032(2) 0.0046(15) -0.0033(15) -0.0006(15) C3 0.057(11) 0.030(9) 0.031(9) -0.002(7) -0.007(8) -0.010(8) O3 0.113(10) 0.017(5) 0.042(7) -0.006(5) -0.005(6) 0.018(6) S4 0.033(2) 0.0254(19) 0.038(2) 0.0009(16) -0.0047(17) -0.0071(17) N4 0.041(7) 0.023(6) 0.025(7) 0.000(5) -0.002(5) -0.001(5) C4 0.042(10) 0.033(9) 0.049(10) 0.024(8) 0.029(8) 0.016(7) O4 0.046(8) 0.046(7) 0.201(17) -0.004(9) 0.046(9) -0.009(6) C5 0.038(10) 0.019(8) 0.057(11) 0.005(7) 0.023(8) -0.005(7) O5 0.17(2) 0.35(3) 0.25(3) -0.26(3) 0.110(19) -0.14(2) C6 0.037(9) 0.031(9) 0.043(10) 0.006(7) 0.002(7) -0.004(7) O6 0.062(11) 0.19(2) 0.37(3) 0.19(2) -0.112(16) -0.045(12) C7 0.023(8) 0.019(7) 0.034(9) -0.012(6) 0.010(6) -0.005(6) O7 0.168(16) 0.097(11) 0.077(11) 0.039(9) -0.031(10) -0.071(11) C8 0.027(8) 0.033(9) 0.045(10) -0.014(7) 0.002(7) 0.005(7) O8 0.037(6) 0.049(6) 0.041(7) 0.008(5) 0.007(5) -0.012(5) C9 0.040(9) 0.041(9) 0.032(9) 0.001(7) 0.014(7) 0.008(8) C10 0.032(9) 0.018(7) 0.057(11) -0.001(7) 0.016(8) 0.000(7) C11 0.022(8) 0.020(7) 0.068(12) 0.002(8) -0.002(7) 0.001(6) C12 0.022(8) 0.035(8) 0.034(9) -0.004(7) 0.008(6) 0.009(6) C13 0.017(7) 0.016(7) 0.021(8) -0.001(5) -0.007(5) -0.005(5) C14 0.023(8) 0.020(7) 0.019(7) 0.005(6) -0.013(6) -0.002(6) C15 0.034(9) 0.031(8) 0.027(8) -0.008(6) -0.008(6) 0.009(7) C16 0.058(11) 0.039(9) 0.022(9) 0.003(7) -0.005(8) 0.002(8) C17 0.040(9) 0.035(8) 0.014(8) 0.000(6) -0.008(7) -0.007(7) C18 0.039(10) 0.068(12) 0.035(10) 0.010(8) 0.020(8) -0.006(9) C19 0.023(9) 0.081(13) 0.044(11) 0.004(9) -0.005(7) 0.011(8) C20 0.025(8) 0.012(7) 0.027(8) 0.001(6) -0.001(6) -0.001(6) C21 0.004(6) 0.035(8) 0.034(9) -0.005(6) 0.006(6) -0.008(6) C22 0.014(7) 0.028(8) 0.046(10) 0.010(7) -0.003(6) 0.003(6) C23 0.044(10) 0.016(7) 0.058(11) 0.009(7) 0.023(8) 0.010(7) C24 0.039(9) 0.030(8) 0.047(10) -0.007(7) 0.006(8) -0.007(7) C25 0.016(7) 0.018(7) 0.050(10) 0.001(7) 0.002(6) 0.009(6) C26 0.057(11) 0.041(9) 0.048(11) 0.005(8) -0.018(8) -0.022(9) C27 0.063(11) 0.011(7) 0.023(8) 0.005(6) 0.008(7) 0.004(7) C28 0.057(10) 0.017(7) 0.026(9) -0.011(6) -0.004(7) 0.004(7) C29 0.068(11) 0.010(7) 0.037(10) -0.005(6) 0.008(8) -0.005(7) C30 0.038(9) 0.035(9) 0.046(11) 0.017(7) 0.009(8) 0.023(7) C31 0.023(8) 0.025(8) 0.055(11) 0.010(7) 0.007(7) -0.006(6) C32 0.028(9) 0.030(8) 0.041(10) -0.004(7) -0.007(7) 0.005(7) C33 0.019(7) 0.026(8) 0.053(10) 0.007(7) 0.012(7) 0.005(7) C34 0.049(10) 0.024(7) 0.012(7) 0.006(6) -0.012(6) 0.006(7) C35 0.022(7) 0.032(8) 0.032(9) 0.016(7) 0.005(6) 0.007(7) _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 Au1 N1 2.072(9) . ? Au1 P1 2.249(3) . ? Au1 Au3 3.2072(8) . ? P1 C7 1.798(12) . ? P1 C1 1.798(12) . ? P1 C13 1.822(12) . ? Co1 N1 1.822(9) . ? Co1 C26 2.029(15) . ? Co1 C27 2.045(12) . ? Co1 C30 2.053(13) . ? Co1 C28 2.083(13) . ? Co1 S2 2.084(4) . ? Co1 C29 2.123(13) . ? N1 S1 1.584(10) . ? S1 N2 1.583(11) . ? C1 C6 1.395(17) . ? C1 C2 1.405(17) . ? Cl1 O2 1.391(11) . ? Cl1 O4 1.413(11) . ? Cl1 O1 1.423(11) . ? Cl1 O3 1.427(9) . ? S2 N2 1.654(12) . ? C2 C3 1.323(17) . ? C2 H2A 0.9500 . ? Cl2 O6 1.356(15) . ? Cl2 O5 1.357(16) . ? Cl2 O7 1.373(13) . ? Cl2 O8 1.452(9) . ? Au3 N3 2.096(9) . ? Au3 P3 2.251(3) . ? P3 C20 1.799(12) . ? P3 C14 1.804(12) . ? P3 C13 1.837(12) . ? Co3 N3 1.812(10) . ? Co3 C31 2.034(13) . ? Co3 C32 2.035(13) . ? Co3 C35 2.056(12) . ? Co3 C33 2.075(13) . ? Co3 S4 2.087(4) . ? Co3 C34 2.112(12) . ? N3 S3 1.569(10) . ? S3 N4 1.562(11) . ? C3 C4 1.376(19) . ? C3 H3A 0.9500 . ? S4 N4 1.648(10) . ? C4 C5 1.36(2) . ? C4 H4A 0.9500 . ? C5 C6 1.377(18) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.371(18) . ? C7 C12 1.399(18) . ? C8 C9 1.374(18) . ? C8 H8A 0.9500 . ? C9 C10 1.41(2) . ? C9 H9A 0.9500 . ? C10 C11 1.364(19) . ? C10 H10A 0.9500 . ? C11 C12 1.418(17) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.380(17) . ? C14 C19 1.387(19) . ? C15 C16 1.392(18) . ? C15 H15A 0.9500 . ? C16 C17 1.349(18) . ? C16 H16A 0.9500 . ? C17 C18 1.370(19) . ? C17 H17A 0.9500 . ? C18 C19 1.39(2) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.382(17) . ? C20 C21 1.386(17) . ? C21 C22 1.393(17) . ? C21 H21A 0.9500 . ? C22 C23 1.394(19) . ? C22 H22A 0.9500 . ? C23 C24 1.382(19) . ? C23 H23A 0.9500 . ? C24 C25 1.394(17) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.39(2) . ? C26 C30 1.43(2) . ? C26 H26A 1.0000 . ? C27 C28 1.426(18) . ? C27 H27A 1.0000 . ? C28 C29 1.391(19) . ? C28 H28A 1.0000 . ? C29 C30 1.45(2) . ? C29 H29A 1.0000 . ? C30 H30A 1.0000 . ? C31 C32 1.365(18) . ? C31 C35 1.405(19) . ? C31 H31A 1.0000 . ? C32 C33 1.406(18) . ? C32 H32A 1.0000 . ? C33 C34 1.424(18) . ? C33 H33A 1.0000 . ? C34 C35 1.449(18) . ? C34 H34A 1.0000 . ? C35 H35A 1.0000 . ? 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 Au1 P1 177.5(3) . . ? N1 Au1 Au3 94.0(3) . . ? P1 Au1 Au3 87.15(9) . . ? C7 P1 C1 102.7(6) . . ? C7 P1 C13 104.8(6) . . ? C1 P1 C13 109.7(6) . . ? C7 P1 Au1 114.7(4) . . ? C1 P1 Au1 111.4(4) . . ? C13 P1 Au1 112.9(4) . . ? N1 Co1 C26 171.2(5) . . ? N1 Co1 C27 131.4(5) . . ? C26 Co1 C27 40.0(6) . . ? N1 Co1 C30 140.9(5) . . ? C26 Co1 C30 40.9(6) . . ? C27 Co1 C30 68.0(6) . . ? N1 Co1 C28 104.8(5) . . ? C26 Co1 C28 67.2(6) . . ? C27 Co1 C28 40.4(5) . . ? C30 Co1 C28 67.0(6) . . ? N1 Co1 S2 90.2(3) . . ? C26 Co1 S2 96.1(4) . . ? C27 Co1 S2 115.8(4) . . ? C30 Co1 S2 112.3(5) . . ? C28 Co1 S2 155.9(4) . . ? N1 Co1 C29 108.7(5) . . ? C26 Co1 C29 67.7(6) . . ? C27 Co1 C29 67.0(5) . . ? C30 Co1 C29 40.7(6) . . ? C28 Co1 C29 38.6(5) . . ? S2 Co1 C29 151.8(4) . . ? S1 N1 Co1 119.8(6) . . ? S1 N1 Au1 113.9(5) . . ? Co1 N1 Au1 126.3(5) . . ? N2 S1 N1 109.2(5) . . ? C6 C1 C2 116.0(11) . . ? C6 C1 P1 122.7(10) . . ? C2 C1 P1 121.3(10) . . ? O2 Cl1 O4 107.1(8) . . ? O2 Cl1 O1 105.6(9) . . ? O4 Cl1 O1 112.8(9) . . ? O2 Cl1 O3 108.2(7) . . ? O4 Cl1 O3 112.7(7) . . ? O1 Cl1 O3 110.1(6) . . ? N2 S2 Co1 106.8(4) . . ? S1 N2 S2 113.9(6) . . ? C3 C2 C1 122.0(13) . . ? C3 C2 H2A 119.0 . . ? C1 C2 H2A 119.0 . . ? O6 Cl2 O5 105.7(17) . . ? O6 Cl2 O7 111.9(12) . . ? O5 Cl2 O7 109.3(16) . . ? O6 Cl2 O8 111.7(9) . . ? O5 Cl2 O8 109.5(9) . . ? O7 Cl2 O8 108.7(7) . . ? N3 Au3 P3 174.8(3) . . ? N3 Au3 Au1 96.2(3) . . ? P3 Au3 Au1 88.88(9) . . ? C20 P3 C14 106.1(6) . . ? C20 P3 C13 103.3(6) . . ? C14 P3 C13 107.3(6) . . ? C20 P3 Au3 112.9(4) . . ? C14 P3 Au3 111.0(4) . . ? C13 P3 Au3 115.5(4) . . ? N3 Co3 C31 163.1(6) . . ? N3 Co3 C32 151.2(5) . . ? C31 Co3 C32 39.2(5) . . ? N3 Co3 C35 123.4(5) . . ? C31 Co3 C35 40.2(5) . . ? C32 Co3 C35 67.6(6) . . ? N3 Co3 C33 115.3(5) . . ? C31 Co3 C33 66.1(5) . . ? C32 Co3 C33 40.0(5) . . ? C35 Co3 C33 67.5(5) . . ? N3 Co3 S4 89.3(3) . . ? C31 Co3 S4 99.1(4) . . ? C32 Co3 S4 105.8(4) . . ? C35 Co3 S4 124.8(4) . . ? C33 Co3 S4 141.2(4) . . ? N3 Co3 C34 102.8(5) . . ? C31 Co3 C34 67.0(5) . . ? C32 Co3 C34 67.4(5) . . ? C35 Co3 C34 40.7(5) . . ? C33 Co3 C34 39.8(5) . . ? S4 Co3 C34 165.0(4) . . ? S3 N3 Co3 121.5(6) . . ? S3 N3 Au3 112.6(5) . . ? Co3 N3 Au3 125.9(5) . . ? N4 S3 N3 107.9(5) . . ? C2 C3 C4 121.9(14) . . ? C2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? N4 S4 Co3 106.1(4) . . ? S3 N4 S4 115.2(7) . . ? C5 C4 C3 117.8(13) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? C4 C5 C6 121.7(14) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 120.4(14) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? C8 C7 C12 117.8(12) . . ? C8 C7 P1 119.2(10) . . ? C12 C7 P1 122.7(10) . . ? C7 C8 C9 124.0(14) . . ? C7 C8 H8A 118.0 . . ? C9 C8 H8A 118.0 . . ? C8 C9 C10 117.6(14) . . ? C8 C9 H9A 121.2 . . ? C10 C9 H9A 121.2 . . ? C11 C10 C9 120.7(13) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C12 120.1(13) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C7 C12 C11 119.7(13) . . ? C7 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? P1 C13 P3 114.7(6) . . ? P1 C13 H13A 108.6 . . ? P3 C13 H13A 108.6 . . ? P1 C13 H13B 108.6 . . ? P3 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C19 117.5(12) . . ? C15 C14 P3 124.7(10) . . ? C19 C14 P3 117.8(10) . . ? C14 C15 C16 119.5(13) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C17 C16 C15 122.0(14) . . ? C17 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? C16 C17 C18 120.1(13) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C19 118.3(13) . . ? C17 C18 H18A 120.8 . . ? C19 C18 H18A 120.8 . . ? C14 C19 C18 122.6(14) . . ? C14 C19 H19A 118.7 . . ? C18 C19 H19A 118.7 . . ? C25 C20 C21 120.4(11) . . ? C25 C20 P3 120.0(9) . . ? C21 C20 P3 119.6(10) . . ? C20 C21 C22 120.2(12) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 119.4(12) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C24 C23 C22 120.0(12) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.5(14) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C20 C25 C24 119.5(13) . . ? C20 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C27 C26 C30 108.8(13) . . ? C27 C26 Co1 70.6(8) . . ? C30 C26 Co1 70.5(8) . . ? C27 C26 H26A 125.6 . . ? C30 C26 H26A 125.6 . . ? Co1 C26 H26A 125.6 . . ? C26 C27 C28 107.6(13) . . ? C26 C27 Co1 69.4(8) . . ? C28 C27 Co1 71.2(8) . . ? C26 C27 H27A 126.2 . . ? C28 C27 H27A 126.2 . . ? Co1 C27 H27A 126.2 . . ? C29 C28 C27 109.6(13) . . ? C29 C28 Co1 72.2(8) . . ? C27 C28 Co1 68.4(7) . . ? C29 C28 H28A 125.2 . . ? C27 C28 H28A 125.2 . . ? Co1 C28 H28A 125.2 . . ? C28 C29 C30 106.9(13) . . ? C28 C29 Co1 69.1(8) . . ? C30 C29 Co1 67.1(7) . . ? C28 C29 H29A 126.5 . . ? C30 C29 H29A 126.5 . . ? Co1 C29 H29A 126.5 . . ? C26 C30 C29 107.1(13) . . ? C26 C30 Co1 68.6(8) . . ? C29 C30 Co1 72.2(8) . . ? C26 C30 H30A 126.4 . . ? C29 C30 H30A 126.4 . . ? Co1 C30 H30A 126.4 . . ? C32 C31 C35 110.6(12) . . ? C32 C31 Co3 70.4(8) . . ? C35 C31 Co3 70.8(7) . . ? C32 C31 H31A 124.7 . . ? C35 C31 H31A 124.7 . . ? Co3 C31 H31A 124.7 . . ? C31 C32 C33 108.0(13) . . ? C31 C32 Co3 70.4(8) . . ? C33 C32 Co3 71.6(7) . . ? C31 C32 H32A 126.0 . . ? C33 C32 H32A 126.0 . . ? Co3 C32 H32A 126.0 . . ? C32 C33 C34 108.8(12) . . ? C32 C33 Co3 68.4(7) . . ? C34 C33 Co3 71.5(7) . . ? C32 C33 H33A 125.6 . . ? C34 C33 H33A 125.6 . . ? Co3 C33 H33A 125.6 . . ? C33 C34 C35 106.0(12) . . ? C33 C34 Co3 68.7(7) . . ? C35 C34 Co3 67.6(7) . . ? C33 C34 H34A 127.0 . . ? C35 C34 H34A 127.0 . . ? Co3 C34 H34A 127.0 . . ? C31 C35 C34 106.6(12) . . ? C31 C35 Co3 69.1(8) . . ? C34 C35 Co3 71.7(7) . . ? C31 C35 H35A 126.7 . . ? C34 C35 H35A 126.7 . . ? Co3 C35 H35A 126.7 . . ? 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 N1 Au1 P1 C7 -88(7) . . . . ? Au3 Au1 P1 C7 154.0(5) . . . . ? N1 Au1 P1 C1 28(7) . . . . ? Au3 Au1 P1 C1 -89.9(4) . . . . ? N1 Au1 P1 C13 152(7) . . . . ? Au3 Au1 P1 C13 34.0(4) . . . . ? C26 Co1 N1 S1 -134(4) . . . . ? C27 Co1 N1 S1 -123.0(7) . . . . ? C30 Co1 N1 S1 130.0(8) . . . . ? C28 Co1 N1 S1 -158.3(7) . . . . ? S2 Co1 N1 S1 2.7(6) . . . . ? C29 Co1 N1 S1 161.5(7) . . . . ? C26 Co1 N1 Au1 45(4) . . . . ? C27 Co1 N1 Au1 55.4(9) . . . . ? C30 Co1 N1 Au1 -51.5(11) . . . . ? C28 Co1 N1 Au1 20.2(8) . . . . ? S2 Co1 N1 Au1 -178.8(6) . . . . ? C29 Co1 N1 Au1 -20.1(8) . . . . ? P1 Au1 N1 S1 160(6) . . . . ? Au3 Au1 N1 S1 -82.5(5) . . . . ? P1 Au1 N1 Co1 -19(7) . . . . ? Au3 Au1 N1 Co1 98.9(6) . . . . ? Co1 N1 S1 N2 -2.9(8) . . . . ? Au1 N1 S1 N2 178.5(5) . . . . ? C7 P1 C1 C6 -64.9(12) . . . . ? C13 P1 C1 C6 46.1(12) . . . . ? Au1 P1 C1 C6 171.9(10) . . . . ? C7 P1 C1 C2 116.6(11) . . . . ? C13 P1 C1 C2 -132.4(11) . . . . ? Au1 P1 C1 C2 -6.7(12) . . . . ? N1 Co1 S2 N2 -1.7(5) . . . . ? C26 Co1 S2 N2 172.2(7) . . . . ? C27 Co1 S2 N2 135.7(6) . . . . ? C30 Co1 S2 N2 -148.9(6) . . . . ? C28 Co1 S2 N2 127.8(11) . . . . ? C29 Co1 S2 N2 -135.2(10) . . . . ? N1 S1 N2 S2 1.2(9) . . . . ? Co1 S2 N2 S1 0.5(8) . . . . ? C6 C1 C2 C3 5(2) . . . . ? P1 C1 C2 C3 -176.0(11) . . . . ? N1 Au1 Au3 N3 -7.5(4) . . . . ? P1 Au1 Au3 N3 170.2(3) . . . . ? N1 Au1 Au3 P3 171.5(3) . . . . ? P1 Au1 Au3 P3 -10.69(12) . . . . ? N3 Au3 P3 C20 -85(3) . . . . ? Au1 Au3 P3 C20 105.1(4) . . . . ? N3 Au3 P3 C14 34(3) . . . . ? Au1 Au3 P3 C14 -135.9(5) . . . . ? N3 Au3 P3 C13 156(3) . . . . ? Au1 Au3 P3 C13 -13.5(4) . . . . ? C31 Co3 N3 S3 -117.2(16) . . . . ? C32 Co3 N3 S3 125.8(10) . . . . ? C35 Co3 N3 S3 -129.5(7) . . . . ? C33 Co3 N3 S3 151.8(7) . . . . ? S4 Co3 N3 S3 2.9(7) . . . . ? C34 Co3 N3 S3 -168.1(7) . . . . ? C31 Co3 N3 Au3 66.6(18) . . . . ? C32 Co3 N3 Au3 -50.4(14) . . . . ? C35 Co3 N3 Au3 54.3(8) . . . . ? C33 Co3 N3 Au3 -24.4(9) . . . . ? S4 Co3 N3 Au3 -173.3(6) . . . . ? C34 Co3 N3 Au3 15.7(8) . . . . ? P3 Au3 N3 S3 113(3) . . . . ? Au1 Au3 N3 S3 -77.5(6) . . . . ? P3 Au3 N3 Co3 -71(3) . . . . ? Au1 Au3 N3 Co3 99.0(6) . . . . ? Co3 N3 S3 N4 -3.3(9) . . . . ? Au3 N3 S3 N4 173.4(5) . . . . ? C1 C2 C3 C4 -3(2) . . . . ? N3 Co3 S4 N4 -1.6(5) . . . . ? C31 Co3 S4 N4 163.6(6) . . . . ? C32 Co3 S4 N4 -156.8(6) . . . . ? C35 Co3 S4 N4 129.8(6) . . . . ? C33 Co3 S4 N4 -133.4(7) . . . . ? C34 Co3 S4 N4 142.3(15) . . . . ? N3 S3 N4 S4 1.6(9) . . . . ? Co3 S4 N4 S3 0.2(7) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 C6 2(2) . . . . ? C4 C5 C6 C1 1(2) . . . . ? C2 C1 C6 C5 -3.9(19) . . . . ? P1 C1 C6 C5 177.5(10) . . . . ? C1 P1 C7 C8 -75.0(11) . . . . ? C13 P1 C7 C8 170.4(10) . . . . ? Au1 P1 C7 C8 46.0(11) . . . . ? C1 P1 C7 C12 99.1(11) . . . . ? C13 P1 C7 C12 -15.5(12) . . . . ? Au1 P1 C7 C12 -139.9(9) . . . . ? C12 C7 C8 C9 2.1(19) . . . . ? P1 C7 C8 C9 176.6(10) . . . . ? C7 C8 C9 C10 -2(2) . . . . ? C8 C9 C10 C11 1.9(19) . . . . ? C9 C10 C11 C12 -1.3(19) . . . . ? C8 C7 C12 C11 -1.5(18) . . . . ? P1 C7 C12 C11 -175.7(9) . . . . ? C10 C11 C12 C7 1.1(18) . . . . ? C7 P1 C13 P3 179.9(6) . . . . ? C1 P1 C13 P3 70.3(8) . . . . ? Au1 P1 C13 P3 -54.6(7) . . . . ? C20 P3 C13 P1 -81.3(7) . . . . ? C14 P3 C13 P1 166.8(6) . . . . ? Au3 P3 C13 P1 42.5(7) . . . . ? C20 P3 C14 C15 -123.1(11) . . . . ? C13 P3 C14 C15 -13.2(12) . . . . ? Au3 P3 C14 C15 113.9(10) . . . . ? C20 P3 C14 C19 59.0(12) . . . . ? C13 P3 C14 C19 168.9(10) . . . . ? Au3 P3 C14 C19 -64.0(11) . . . . ? C19 C14 C15 C16 -0.4(19) . . . . ? P3 C14 C15 C16 -178.3(10) . . . . ? C14 C15 C16 C17 1(2) . . . . ? C15 C16 C17 C18 -1(2) . . . . ? C16 C17 C18 C19 1(2) . . . . ? C15 C14 C19 C18 0(2) . . . . ? P3 C14 C19 C18 178.1(12) . . . . ? C17 C18 C19 C14 0(2) . . . . ? C14 P3 C20 C25 42.2(12) . . . . ? C13 P3 C20 C25 -70.5(12) . . . . ? Au3 P3 C20 C25 164.0(9) . . . . ? C14 P3 C20 C21 -141.6(10) . . . . ? C13 P3 C20 C21 105.7(10) . . . . ? Au3 P3 C20 C21 -19.7(11) . . . . ? C25 C20 C21 C22 -0.5(19) . . . . ? P3 C20 C21 C22 -176.7(9) . . . . ? C20 C21 C22 C23 0.3(19) . . . . ? C21 C22 C23 C24 0(2) . . . . ? C22 C23 C24 C25 0(2) . . . . ? C21 C20 C25 C24 0(2) . . . . ? P3 C20 C25 C24 176.7(10) . . . . ? C23 C24 C25 C20 0(2) . . . . ? N1 Co1 C26 C27 12(4) . . . . ? C30 Co1 C26 C27 119.1(12) . . . . ? C28 Co1 C26 C27 38.4(8) . . . . ? S2 Co1 C26 C27 -123.6(8) . . . . ? C29 Co1 C26 C27 80.3(9) . . . . ? N1 Co1 C26 C30 -107(4) . . . . ? C27 Co1 C26 C30 -119.1(12) . . . . ? C28 Co1 C26 C30 -80.7(9) . . . . ? S2 Co1 C26 C30 117.3(8) . . . . ? C29 Co1 C26 C30 -38.8(8) . . . . ? C30 C26 C27 C28 -0.9(16) . . . . ? Co1 C26 C27 C28 -61.3(9) . . . . ? C30 C26 C27 Co1 60.4(10) . . . . ? N1 Co1 C27 C26 -177.5(8) . . . . ? C30 Co1 C27 C26 -38.1(9) . . . . ? C28 Co1 C27 C26 -118.0(12) . . . . ? S2 Co1 C27 C26 66.9(9) . . . . ? C29 Co1 C27 C26 -82.2(10) . . . . ? N1 Co1 C27 C28 -59.5(10) . . . . ? C26 Co1 C27 C28 118.0(12) . . . . ? C30 Co1 C27 C28 79.9(9) . . . . ? S2 Co1 C27 C28 -175.1(7) . . . . ? C29 Co1 C27 C28 35.8(8) . . . . ? C26 C27 C28 C29 -0.6(15) . . . . ? Co1 C27 C28 C29 -60.7(10) . . . . ? C26 C27 C28 Co1 60.1(9) . . . . ? N1 Co1 C28 C29 -101.6(9) . . . . ? C26 Co1 C28 C29 82.4(10) . . . . ? C27 Co1 C28 C29 120.4(13) . . . . ? C30 Co1 C28 C29 37.9(9) . . . . ? S2 Co1 C28 C29 131.3(10) . . . . ? N1 Co1 C28 C27 138.0(8) . . . . ? C26 Co1 C28 C27 -38.0(9) . . . . ? C30 Co1 C28 C27 -82.5(9) . . . . ? S2 Co1 C28 C27 10.9(16) . . . . ? C29 Co1 C28 C27 -120.4(13) . . . . ? C27 C28 C29 C30 1.7(15) . . . . ? Co1 C28 C29 C30 -56.6(9) . . . . ? C27 C28 C29 Co1 58.3(9) . . . . ? N1 Co1 C29 C28 90.5(9) . . . . ? C26 Co1 C29 C28 -80.9(10) . . . . ? C27 Co1 C29 C28 -37.4(9) . . . . ? C30 Co1 C29 C28 -119.9(12) . . . . ? S2 Co1 C29 C28 -139.5(8) . . . . ? N1 Co1 C29 C30 -149.6(8) . . . . ? C26 Co1 C29 C30 39.0(9) . . . . ? C27 Co1 C29 C30 82.5(9) . . . . ? C28 Co1 C29 C30 119.9(12) . . . . ? S2 Co1 C29 C30 -19.7(14) . . . . ? C27 C26 C30 C29 1.9(16) . . . . ? Co1 C26 C30 C29 62.4(9) . . . . ? C27 C26 C30 Co1 -60.5(10) . . . . ? C28 C29 C30 C26 -2.2(15) . . . . ? Co1 C29 C30 C26 -60.1(9) . . . . ? C28 C29 C30 Co1 57.9(9) . . . . ? N1 Co1 C30 C26 166.5(8) . . . . ? C27 Co1 C30 C26 37.2(8) . . . . ? C28 Co1 C30 C26 81.1(9) . . . . ? S2 Co1 C30 C26 -72.7(9) . . . . ? C29 Co1 C30 C26 117.1(12) . . . . ? N1 Co1 C30 C29 49.4(12) . . . . ? C26 Co1 C30 C29 -117.1(12) . . . . ? C27 Co1 C30 C29 -79.9(8) . . . . ? C28 Co1 C30 C29 -36.0(8) . . . . ? S2 Co1 C30 C29 170.1(7) . . . . ? N3 Co3 C31 C32 -137.3(15) . . . . ? C35 Co3 C31 C32 -121.3(12) . . . . ? C33 Co3 C31 C32 -38.5(8) . . . . ? S4 Co3 C31 C32 103.9(8) . . . . ? C34 Co3 C31 C32 -82.0(9) . . . . ? N3 Co3 C31 C35 -16(2) . . . . ? C32 Co3 C31 C35 121.3(12) . . . . ? C33 Co3 C31 C35 82.8(8) . . . . ? S4 Co3 C31 C35 -134.9(7) . . . . ? C34 Co3 C31 C35 39.3(7) . . . . ? C35 C31 C32 C33 2.5(16) . . . . ? Co3 C31 C32 C33 62.0(9) . . . . ? C35 C31 C32 Co3 -59.5(10) . . . . ? N3 Co3 C32 C31 155.7(10) . . . . ? C35 Co3 C32 C31 36.6(8) . . . . ? C33 Co3 C32 C31 117.7(13) . . . . ? S4 Co3 C32 C31 -85.0(9) . . . . ? C34 Co3 C32 C31 80.8(9) . . . . ? N3 Co3 C32 C33 38.0(15) . . . . ? C31 Co3 C32 C33 -117.7(13) . . . . ? C35 Co3 C32 C33 -81.1(9) . . . . ? S4 Co3 C32 C33 157.2(7) . . . . ? C34 Co3 C32 C33 -36.9(8) . . . . ? C31 C32 C33 C34 -0.9(15) . . . . ? Co3 C32 C33 C34 60.3(9) . . . . ? C31 C32 C33 Co3 -61.2(9) . . . . ? N3 Co3 C33 C32 -160.9(8) . . . . ? C31 Co3 C33 C32 37.7(8) . . . . ? C35 Co3 C33 C32 81.6(9) . . . . ? S4 Co3 C33 C32 -36.4(11) . . . . ? C34 Co3 C33 C32 119.8(12) . . . . ? N3 Co3 C33 C34 79.3(9) . . . . ? C31 Co3 C33 C34 -82.1(9) . . . . ? C32 Co3 C33 C34 -119.8(12) . . . . ? C35 Co3 C33 C34 -38.3(8) . . . . ? S4 Co3 C33 C34 -156.3(6) . . . . ? C32 C33 C34 C35 -0.9(14) . . . . ? Co3 C33 C34 C35 57.6(8) . . . . ? C32 C33 C34 Co3 -58.5(9) . . . . ? N3 Co3 C34 C33 -114.4(8) . . . . ? C31 Co3 C34 C33 79.8(8) . . . . ? C32 Co3 C34 C33 37.1(8) . . . . ? C35 Co3 C34 C33 118.6(11) . . . . ? S4 Co3 C34 C33 102.7(15) . . . . ? N3 Co3 C34 C35 127.0(8) . . . . ? C31 Co3 C34 C35 -38.8(8) . . . . ? C32 Co3 C34 C35 -81.5(8) . . . . ? C33 Co3 C34 C35 -118.6(11) . . . . ? S4 Co3 C34 C35 -15.9(19) . . . . ? C32 C31 C35 C34 -3.0(15) . . . . ? Co3 C31 C35 C34 -62.4(8) . . . . ? C32 C31 C35 Co3 59.3(10) . . . . ? C33 C34 C35 C31 2.3(14) . . . . ? Co3 C34 C35 C31 60.6(9) . . . . ? C33 C34 C35 Co3 -58.3(9) . . . . ? N3 Co3 C35 C31 174.5(7) . . . . ? C32 Co3 C35 C31 -35.7(8) . . . . ? C33 Co3 C35 C31 -79.2(8) . . . . ? S4 Co3 C35 C31 58.4(8) . . . . ? C34 Co3 C35 C31 -116.6(11) . . . . ? N3 Co3 C35 C34 -68.9(9) . . . . ? C31 Co3 C35 C34 116.6(11) . . . . ? C32 Co3 C35 C34 80.9(8) . . . . ? C33 Co3 C35 C34 37.4(7) . . . . ? S4 Co3 C35 C34 175.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.973 _refine_diff_density_min -1.445 _refine_diff_density_rms 0.217