# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dong-Youn Noh' _publ_contact_author_email DYNOH@SWU.AC.KR _publ_section_title ; Heteroleptic binuclear palladium(II) and platinum(II) complexes containing 1,2-bis(diphenylphosphino)acetylene and 1,2-benzenedithiolates: syntheses, X-ray crystal structures, electrochemistry and photoluminescence properties ; loop_ _publ_author_name 'Dong-Youn Noh' 'Chang Seop Hong' 'Jae Il Kim' 'Myong-Gu Seo' 'Kyong-Soon Shin' 'Kyung-In Son' # Attachment 'pd_bdtEND.cif' data_pd_bdt_[Pd(bdt)]2(u-dppa)2 _database_code_depnum_ccdc_archive 'CCDC 699934' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H51 Cl9 P4 Pd2 S4' _chemical_formula_weight 1640.05 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.7965(3) _cell_length_b 14.0504(3) _cell_length_c 36.1985(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.5380(10) _cell_angle_gamma 90.00 _cell_volume 7003.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5733 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 24.995 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6912 _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega & phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69043 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.39 _reflns_number_total 17498 _reflns_number_gt 9528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEXll' _computing_cell_refinement 'Bruker SMART APEXll' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^)+(0.0702P)^2^+2.4323P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17498 _refine_ls_number_parameters 775 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.026 _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 Pd1 Pd 0.16000(2) 0.60183(2) 0.084412(9) 0.03712(10) Uani 1 1 d . . . Pd2 Pd 0.54422(2) 0.30471(3) 0.151901(10) 0.04128(11) Uani 1 1 d . . . P1 P 0.12884(8) 0.47207(9) 0.12059(3) 0.0401(3) Uani 1 1 d . . . P2 P 0.27673(8) 0.52771(9) 0.05243(3) 0.0396(3) Uani 1 1 d . . . P3 P 0.38735(8) 0.28128(9) 0.16778(3) 0.0424(3) Uani 1 1 d . . . P4 P 0.52477(8) 0.46444(9) 0.14262(3) 0.0395(3) Uani 1 1 d . . . C1 C 0.2300(3) 0.4056(3) 0.13757(13) 0.0421(11) Uani 1 1 d . . . C2 C 0.2974(3) 0.3609(3) 0.15053(13) 0.0430(11) Uani 1 1 d . . . C3 C 0.3730(3) 0.4929(3) 0.08304(12) 0.0427(11) Uani 1 1 d . . . C4 C 0.4367(3) 0.4838(3) 0.10647(12) 0.0404(11) Uani 1 1 d . . . C5 C 0.2358(3) 0.4198(4) 0.02921(12) 0.0443(11) Uani 1 1 d . . . C6 C 0.2885(4) 0.3371(4) 0.03123(15) 0.0601(14) Uani 1 1 d . . . H6 H 0.3477 0.3348 0.0449 0.072 Uiso 1 1 calc R . . C7 C 0.2526(5) 0.2568(5) 0.01264(18) 0.0799(19) Uani 1 1 d . . . H7 H 0.2890 0.2011 0.0133 0.096 Uiso 1 1 calc R . . C8 C 0.1649(5) 0.2590(5) -0.00655(18) 0.0776(18) Uani 1 1 d . . . H8 H 0.1406 0.2044 -0.0184 0.093 Uiso 1 1 calc R . . C9 C 0.1132(4) 0.3404(5) -0.00838(16) 0.0758(18) Uani 1 1 d . . . H9 H 0.0538 0.3419 -0.0220 0.091 Uiso 1 1 calc R . . C10 C 0.1465(4) 0.4203(4) 0.00932(14) 0.0586(14) Uani 1 1 d . . . H10 H 0.1094 0.4756 0.0081 0.070 Uiso 1 1 calc R . . C11 C 0.3424(3) 0.5972(3) 0.01981(13) 0.0448(11) Uani 1 1 d . . . C12 C 0.3276(4) 0.5862(4) -0.01773(14) 0.0621(15) Uani 1 1 d . . . H12 H 0.2850 0.5397 -0.0272 0.075 Uiso 1 1 calc R . . C13 C 0.3752(5) 0.6433(5) -0.04151(18) 0.082(2) Uani 1 1 d . . . H13 H 0.3636 0.6359 -0.0669 0.098 Uiso 1 1 calc R . . C14 C 0.4389(6) 0.7102(5) -0.0283(2) 0.091(2) Uani 1 1 d . . . H14 H 0.4714 0.7482 -0.0446 0.109 Uiso 1 1 calc R . . C15 C 0.4553(5) 0.7218(5) 0.0093(2) 0.086(2) Uani 1 1 d . . . H15 H 0.4989 0.7678 0.0184 0.103 Uiso 1 1 calc R . . C16 C 0.4075(4) 0.6659(4) 0.03348(16) 0.0659(15) Uani 1 1 d . . . H16 H 0.4187 0.6740 0.0589 0.079 Uiso 1 1 calc R . . C17 C 0.4775(3) 0.5251(4) 0.18147(14) 0.0484(12) Uani 1 1 d . . . C18 C 0.4096(4) 0.5959(4) 0.17800(18) 0.0713(17) Uani 1 1 d . . . H18 H 0.3857 0.6151 0.1546 0.086 Uiso 1 1 calc R . . C19 C 0.3762(5) 0.6393(6) 0.2092(3) 0.102(3) Uani 1 1 d . . . H19 H 0.3289 0.6865 0.2069 0.123 Uiso 1 1 calc R . . C20 C 0.4135(8) 0.6118(7) 0.2432(3) 0.118(4) Uani 1 1 d . . . H20 H 0.3919 0.6417 0.2640 0.142 Uiso 1 1 calc R . . C21 C 0.4810(7) 0.5424(6) 0.2476(2) 0.102(3) Uani 1 1 d . . . H21 H 0.5064 0.5257 0.2711 0.123 Uiso 1 1 calc R . . C22 C 0.5116(5) 0.4967(5) 0.21660(16) 0.0721(17) Uani 1 1 d . . . H22 H 0.5554 0.4466 0.2193 0.086 Uiso 1 1 calc R . . C23 C 0.6231(3) 0.5388(3) 0.12824(13) 0.0435(11) Uani 1 1 d . . . C24 C 0.6967(4) 0.5658(5) 0.15265(16) 0.0705(17) Uani 1 1 d . . . H24 H 0.6959 0.5474 0.1773 0.085 Uiso 1 1 calc R . . C25 C 0.7720(4) 0.6197(5) 0.14136(18) 0.082(2) Uani 1 1 d . . . H25 H 0.8220 0.6370 0.1584 0.098 Uiso 1 1 calc R . . C26 C 0.7746(4) 0.6483(5) 0.10566(19) 0.0744(17) Uani 1 1 d . . . H26 H 0.8260 0.6852 0.0984 0.089 Uiso 1 1 calc R . . C27 C 0.7016(4) 0.6228(4) 0.08049(17) 0.0704(17) Uani 1 1 d . . . H27 H 0.7028 0.6423 0.0560 0.084 Uiso 1 1 calc R . . C28 C 0.6254(4) 0.5674(4) 0.09178(15) 0.0618(15) Uani 1 1 d . . . H28 H 0.5757 0.5494 0.0747 0.074 Uiso 1 1 calc R . . C29 C 0.0562(3) 0.3836(4) 0.09570(13) 0.0454(11) Uani 1 1 d . . . C30 C 0.0795(4) 0.2877(4) 0.09695(15) 0.0613(15) Uani 1 1 d . . . H30 H 0.1345 0.2677 0.1110 0.074 Uiso 1 1 calc R . . C31 C 0.0224(5) 0.2216(5) 0.07775(19) 0.0786(18) Uani 1 1 d . . . H31 H 0.0388 0.1573 0.0787 0.094 Uiso 1 1 calc R . . C32 C -0.0593(5) 0.2516(6) 0.05700(18) 0.085(2) Uani 1 1 d . . . H32 H -0.0982 0.2074 0.0439 0.102 Uiso 1 1 calc R . . C33 C -0.0829(4) 0.3448(6) 0.05568(18) 0.087(2) Uani 1 1 d . . . H33 H -0.1377 0.3643 0.0415 0.105 Uiso 1 1 calc R . . C34 C -0.0264(4) 0.4123(4) 0.07529(16) 0.0702(17) Uani 1 1 d . . . H34 H -0.0443 0.4761 0.0746 0.084 Uiso 1 1 calc R . . C35 C 0.0713(3) 0.4885(3) 0.16414(13) 0.0441(11) Uani 1 1 d . . . C36 C -0.0246(4) 0.4651(4) 0.16783(16) 0.0675(16) Uani 1 1 d . . . H36 H -0.0623 0.4431 0.1474 0.081 Uiso 1 1 calc R . . C37 C -0.0651(5) 0.4739(5) 0.2015(2) 0.088(2) Uani 1 1 d . . . H37 H -0.1302 0.4592 0.2038 0.106 Uiso 1 1 calc R . . C38 C -0.0086(6) 0.5042(5) 0.23117(19) 0.087(2) Uani 1 1 d . . . H38 H -0.0350 0.5077 0.2542 0.105 Uiso 1 1 calc R . . C39 C 0.0847(5) 0.5294(5) 0.22812(16) 0.082(2) Uani 1 1 d . . . H39 H 0.1219 0.5514 0.2487 0.098 Uiso 1 1 calc R . . C40 C 0.1248(4) 0.5223(4) 0.19397(15) 0.0687(16) Uani 1 1 d . . . H40 H 0.1888 0.5408 0.1915 0.082 Uiso 1 1 calc R . . C41 C 0.3255(3) 0.1723(4) 0.15256(15) 0.0491(12) Uani 1 1 d . . . C42 C 0.2620(4) 0.1262(4) 0.17451(17) 0.0639(15) Uani 1 1 d . . . H42 H 0.2575 0.1448 0.1990 0.077 Uiso 1 1 calc R . . C43 C 0.2052(4) 0.0525(5) 0.1602(2) 0.0776(18) Uani 1 1 d . . . H43 H 0.1621 0.0221 0.1751 0.093 Uiso 1 1 calc R . . C44 C 0.2117(5) 0.0244(5) 0.1250(2) 0.085(2) Uani 1 1 d . . . H44 H 0.1734 -0.0254 0.1156 0.102 Uiso 1 1 calc R . . C45 C 0.2754(5) 0.0695(5) 0.10290(18) 0.084(2) Uani 1 1 d . . . H45 H 0.2794 0.0503 0.0785 0.101 Uiso 1 1 calc R . . C46 C 0.3336(5) 0.1434(4) 0.11687(17) 0.0708(16) Uani 1 1 d . . . H46 H 0.3775 0.1728 0.1021 0.085 Uiso 1 1 calc R . . C47 C 0.3766(3) 0.2919(3) 0.21735(13) 0.0464(12) Uani 1 1 d . . . C48 C 0.2964(4) 0.3343(4) 0.23198(15) 0.0609(14) Uani 1 1 d . . . H48 H 0.2449 0.3564 0.2165 0.073 Uiso 1 1 calc R . . C49 C 0.2950(5) 0.3430(5) 0.27024(17) 0.0753(17) Uani 1 1 d . . . H49 H 0.2418 0.3716 0.2803 0.090 Uiso 1 1 calc R . . C50 C 0.3688(5) 0.3109(5) 0.29303(16) 0.0762(18) Uani 1 1 d . . . H50 H 0.3666 0.3177 0.3185 0.091 Uiso 1 1 calc R . . C51 C 0.4461(5) 0.2688(5) 0.27855(18) 0.083(2) Uani 1 1 d . . . H51 H 0.4962 0.2455 0.2944 0.100 Uiso 1 1 calc R . . C52 C 0.4524(4) 0.2596(4) 0.24056(15) 0.0643(15) Uani 1 1 d . . . H52 H 0.5068 0.2321 0.2310 0.077 Uiso 1 1 calc R . . S1 S 0.04717(9) 0.68484(9) 0.11483(4) 0.0489(3) Uani 1 1 d . . . S2 S 0.17316(9) 0.72801(9) 0.04546(4) 0.0506(3) Uani 1 1 d . . . C53 C 0.0871(3) 0.8097(3) 0.05954(13) 0.0461(11) Uani 1 1 d . . . C54 C 0.0727(4) 0.8947(4) 0.04028(15) 0.0616(14) Uani 1 1 d . . . H54 H 0.1092 0.9071 0.0201 0.074 Uiso 1 1 calc R . . C55 C 0.0073(5) 0.9594(4) 0.05016(17) 0.0700(16) Uani 1 1 d . . . H55 H -0.0012 1.0157 0.0368 0.084 Uiso 1 1 calc R . . C56 C -0.0471(5) 0.9422(4) 0.07999(18) 0.0748(18) Uani 1 1 d . . . H56 H -0.0921 0.9871 0.0868 0.090 Uiso 1 1 calc R . . C57 C -0.0353(4) 0.8579(4) 0.10006(15) 0.0617(14) Uani 1 1 d . . . H57 H -0.0725 0.8462 0.1201 0.074 Uiso 1 1 calc R . . C58 C 0.0328(3) 0.7913(3) 0.08981(14) 0.0465(12) Uani 1 1 d . . . S3 S 0.56695(10) 0.14426(10) 0.15855(5) 0.0646(4) Uani 1 1 d . . . S4 S 0.70641(9) 0.32133(10) 0.14493(4) 0.0526(3) Uani 1 1 d . . . C59 C 0.7525(4) 0.2063(4) 0.15088(13) 0.0530(13) Uani 1 1 d . . . C60 C 0.8525(4) 0.1911(5) 0.14947(15) 0.0694(17) Uani 1 1 d . . . H60 H 0.8932 0.2418 0.1447 0.083 Uiso 1 1 calc R . . C61 C 0.8913(5) 0.1005(5) 0.15516(17) 0.080(2) Uani 1 1 d . . . H61 H 0.9577 0.0908 0.1541 0.096 Uiso 1 1 calc R . . C62 C 0.8322(5) 0.0261(5) 0.16219(17) 0.080(2) Uani 1 1 d . . . H62 H 0.8586 -0.0343 0.1661 0.097 Uiso 1 1 calc R . . C63 C 0.7331(5) 0.0394(4) 0.16356(15) 0.0722(17) Uani 1 1 d . . . H63 H 0.6930 -0.0118 0.1684 0.087 Uiso 1 1 calc R . . C64 C 0.6933(4) 0.1298(4) 0.15768(14) 0.0570(14) Uani 1 1 d . . . C65 C 0.4545(7) 0.8711(8) 0.1350(3) 0.154(3) Uani 1 1 d DU . . H65 H 0.4660 0.9284 0.1205 0.185 Uiso 1 1 calc R . . Cl1 Cl 0.4383(2) 0.9020(2) 0.17925(8) 0.1504(10) Uani 1 1 d DU . . Cl2 Cl 0.3482(3) 0.8148(2) 0.11729(12) 0.242(2) Uani 1 1 d DU . . Cl3 Cl 0.5492(3) 0.7940(3) 0.13175(11) 0.2092(16) Uani 1 1 d DU . . C66 C 0.7325(5) 0.7625(5) 0.2548(2) 0.097(2) Uani 1 1 d DU . . H66 H 0.7405 0.7691 0.2818 0.116 Uiso 1 1 calc R . . Cl4 Cl 0.7749(2) 0.8650(2) 0.23564(8) 0.1569(11) Uani 1 1 d DU . . Cl5 Cl 0.61224(19) 0.7501(2) 0.24327(11) 0.1876(14) Uani 1 1 d DU . . Cl6 Cl 0.79386(19) 0.6622(2) 0.24286(7) 0.1418(9) Uani 1 1 d DU . . C67 C 0.6498(7) 0.0273(9) 0.0637(3) 0.195(4) Uani 1 1 d DU . . H67 H 0.6636 0.0602 0.0873 0.234 Uiso 1 1 calc R . . Cl7 Cl 0.5246(2) 0.0237(3) 0.05114(11) 0.2034(15) Uani 1 1 d DU . . Cl8 Cl 0.6872(3) -0.0951(3) 0.06591(15) 0.2334(18) Uani 1 1 d DU . . Cl9 Cl 0.7068(3) 0.0764(4) 0.0301(2) 0.409(5) Uani 1 1 d DU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03406(18) 0.0401(2) 0.03685(19) 0.00007(16) -0.00058(13) 0.00282(15) Pd2 0.03451(18) 0.0471(2) 0.0419(2) 0.00319(17) 0.00017(14) 0.00586(16) P1 0.0346(6) 0.0415(7) 0.0438(7) 0.0022(5) 0.0005(5) 0.0038(5) P2 0.0341(6) 0.0483(7) 0.0359(6) 0.0020(5) -0.0010(5) 0.0038(5) P3 0.0363(6) 0.0440(7) 0.0467(7) 0.0058(6) 0.0007(5) 0.0031(5) P4 0.0324(6) 0.0464(7) 0.0391(6) 0.0039(5) -0.0023(5) 0.0024(5) C1 0.038(2) 0.043(3) 0.045(3) 0.002(2) 0.005(2) -0.004(2) C2 0.037(2) 0.045(3) 0.047(3) 0.000(2) 0.003(2) -0.003(2) C3 0.039(2) 0.048(3) 0.041(3) 0.007(2) 0.008(2) 0.000(2) C4 0.037(2) 0.043(3) 0.041(3) 0.005(2) 0.003(2) -0.005(2) C5 0.045(3) 0.055(3) 0.033(2) -0.002(2) 0.005(2) 0.000(2) C6 0.064(3) 0.054(3) 0.062(4) -0.005(3) -0.001(3) 0.007(3) C7 0.096(5) 0.057(4) 0.087(5) -0.013(3) 0.008(4) 0.003(4) C8 0.091(5) 0.066(4) 0.076(4) -0.019(4) 0.015(4) -0.024(4) C9 0.064(4) 0.102(5) 0.061(4) -0.021(4) 0.000(3) -0.030(4) C10 0.045(3) 0.073(4) 0.058(3) -0.010(3) -0.002(2) -0.002(3) C11 0.037(2) 0.049(3) 0.049(3) 0.007(2) 0.007(2) 0.006(2) C12 0.076(4) 0.067(4) 0.044(3) 0.007(3) 0.008(3) 0.002(3) C13 0.106(5) 0.086(5) 0.055(4) 0.015(4) 0.021(4) 0.020(4) C14 0.091(5) 0.083(5) 0.105(6) 0.032(5) 0.044(5) 0.009(4) C15 0.078(4) 0.080(5) 0.101(6) 0.023(4) 0.010(4) -0.023(4) C16 0.066(4) 0.075(4) 0.057(3) 0.006(3) 0.006(3) -0.008(3) C17 0.044(3) 0.046(3) 0.056(3) -0.004(2) 0.007(2) -0.005(2) C18 0.056(3) 0.072(4) 0.087(4) -0.015(3) 0.008(3) 0.006(3) C19 0.071(5) 0.089(6) 0.152(8) -0.046(6) 0.040(5) 0.005(4) C20 0.137(8) 0.128(8) 0.098(7) -0.057(6) 0.068(6) -0.048(7) C21 0.145(8) 0.101(6) 0.063(4) -0.024(4) 0.028(5) -0.026(6) C22 0.093(5) 0.069(4) 0.055(4) -0.010(3) 0.013(3) -0.007(3) C23 0.035(2) 0.049(3) 0.046(3) 0.000(2) 0.002(2) 0.001(2) C24 0.052(3) 0.097(5) 0.061(4) 0.018(3) -0.011(3) -0.023(3) C25 0.061(4) 0.112(6) 0.070(4) 0.008(4) -0.016(3) -0.034(4) C26 0.050(3) 0.078(4) 0.096(5) 0.004(4) 0.010(3) -0.015(3) C27 0.064(4) 0.086(5) 0.062(4) 0.012(3) 0.015(3) -0.011(3) C28 0.053(3) 0.077(4) 0.056(3) -0.001(3) 0.007(3) -0.017(3) C29 0.038(2) 0.051(3) 0.047(3) -0.001(2) 0.003(2) -0.005(2) C30 0.054(3) 0.062(4) 0.067(4) -0.006(3) -0.002(3) -0.007(3) C31 0.073(4) 0.062(4) 0.100(5) -0.019(4) 0.001(4) -0.015(3) C32 0.086(5) 0.095(6) 0.073(4) -0.019(4) -0.001(4) -0.038(4) C33 0.062(4) 0.104(6) 0.091(5) 0.000(4) -0.031(3) -0.020(4) C34 0.061(3) 0.070(4) 0.077(4) 0.004(3) -0.018(3) -0.008(3) C35 0.044(3) 0.042(3) 0.047(3) 0.003(2) 0.002(2) 0.007(2) C36 0.059(3) 0.080(4) 0.065(4) 0.004(3) 0.016(3) 0.002(3) C37 0.077(4) 0.114(6) 0.076(5) 0.008(4) 0.027(4) 0.002(4) C38 0.106(6) 0.095(5) 0.064(4) 0.018(4) 0.033(4) 0.035(5) C39 0.097(5) 0.101(5) 0.046(3) -0.019(3) -0.002(3) 0.025(4) C40 0.064(4) 0.083(4) 0.059(4) -0.014(3) 0.005(3) 0.004(3) C41 0.042(3) 0.046(3) 0.059(3) 0.003(3) -0.001(2) 0.007(2) C42 0.064(3) 0.053(4) 0.074(4) 0.003(3) 0.007(3) -0.009(3) C43 0.069(4) 0.059(4) 0.105(5) 0.000(4) 0.004(4) -0.015(3) C44 0.073(4) 0.057(4) 0.122(6) -0.009(4) -0.014(4) -0.010(3) C45 0.109(5) 0.077(5) 0.065(4) -0.017(4) -0.010(4) 0.003(4) C46 0.080(4) 0.063(4) 0.069(4) -0.003(3) -0.002(3) -0.001(3) C47 0.050(3) 0.043(3) 0.046(3) 0.007(2) 0.002(2) -0.004(2) C48 0.057(3) 0.073(4) 0.053(3) 0.005(3) 0.006(3) 0.009(3) C49 0.079(4) 0.083(5) 0.066(4) -0.007(4) 0.023(3) 0.005(4) C50 0.103(5) 0.081(5) 0.044(3) 0.001(3) 0.009(3) 0.008(4) C51 0.096(5) 0.090(5) 0.062(4) 0.024(4) -0.012(4) 0.013(4) C52 0.063(3) 0.076(4) 0.053(3) 0.009(3) -0.003(3) 0.015(3) S1 0.0494(7) 0.0470(7) 0.0512(7) 0.0012(6) 0.0105(6) 0.0075(6) S2 0.0561(7) 0.0482(8) 0.0481(7) 0.0075(6) 0.0080(6) 0.0091(6) C53 0.052(3) 0.042(3) 0.043(3) -0.003(2) -0.005(2) 0.005(2) C54 0.080(4) 0.051(3) 0.053(3) -0.001(3) -0.002(3) 0.013(3) C55 0.098(5) 0.046(3) 0.065(4) 0.005(3) -0.002(3) 0.013(3) C56 0.086(4) 0.048(4) 0.089(5) -0.013(3) -0.007(4) 0.030(3) C57 0.068(4) 0.057(4) 0.060(3) -0.008(3) 0.007(3) 0.017(3) C58 0.047(3) 0.037(3) 0.054(3) -0.006(2) -0.004(2) 0.005(2) S3 0.0532(8) 0.0498(8) 0.0911(11) 0.0055(8) 0.0078(7) 0.0109(7) S4 0.0378(6) 0.0630(9) 0.0572(8) 0.0071(7) 0.0044(6) 0.0071(6) C59 0.048(3) 0.073(4) 0.038(3) -0.004(3) 0.001(2) 0.019(3) C60 0.050(3) 0.095(5) 0.064(4) -0.002(3) 0.009(3) 0.025(3) C61 0.060(4) 0.105(6) 0.076(4) 0.006(4) 0.014(3) 0.039(4) C62 0.084(5) 0.089(5) 0.070(4) 0.005(4) 0.015(3) 0.049(4) C63 0.083(4) 0.065(4) 0.069(4) 0.006(3) 0.009(3) 0.027(3) C64 0.059(3) 0.062(4) 0.050(3) -0.004(3) 0.002(3) 0.023(3) C65 0.169(8) 0.153(9) 0.141(7) -0.017(7) 0.015(7) 0.037(6) Cl1 0.156(2) 0.147(2) 0.148(2) -0.0455(18) 0.0030(18) -0.0078(18) Cl2 0.248(4) 0.147(3) 0.309(5) -0.115(3) -0.161(3) 0.086(3) Cl3 0.185(3) 0.207(4) 0.242(4) -0.037(3) 0.070(3) 0.053(3) C66 0.114(5) 0.106(5) 0.070(4) 0.002(4) 0.001(4) -0.008(4) Cl4 0.155(2) 0.157(2) 0.157(2) 0.0525(19) -0.0024(18) -0.0529(19) Cl5 0.0960(17) 0.171(3) 0.296(4) -0.036(3) 0.012(2) -0.0206(18) Cl6 0.147(2) 0.146(2) 0.1267(18) -0.0316(16) -0.0377(15) 0.0346(17) C67 0.154(7) 0.240(11) 0.192(11) 0.006(9) 0.018(7) 0.083(9) Cl7 0.144(2) 0.232(4) 0.236(4) 0.014(3) 0.034(2) 0.000(2) Cl8 0.195(3) 0.165(3) 0.340(6) -0.013(3) 0.016(4) 0.015(3) Cl9 0.159(3) 0.348(7) 0.733(14) 0.289(9) 0.127(6) 0.026(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 Pd1 S2 2.2795(13) . ? Pd1 S1 2.2820(12) . ? Pd1 P2 2.2908(12) . ? Pd1 P1 2.3008(13) . ? Pd2 S4 2.2793(12) . ? Pd2 P4 2.2827(13) . ? Pd2 S3 2.2867(15) . ? Pd2 P3 2.2970(12) . ? P1 C1 1.758(5) . ? P1 C29 1.803(5) . ? P1 C35 1.823(5) . ? P2 C3 1.746(5) . ? P2 C5 1.807(5) . ? P2 C11 1.817(5) . ? P3 C2 1.756(5) . ? P3 C47 1.815(5) . ? P3 C41 1.821(5) . ? P4 C4 1.751(5) . ? P4 C17 1.801(5) . ? P4 C23 1.815(5) . ? C1 C2 1.194(6) . ? C3 C4 1.190(6) . ? C5 C6 1.369(7) . ? C5 C10 1.388(6) . ? C6 C7 1.390(8) . ? C7 C8 1.357(9) . ? C8 C9 1.347(9) . ? C9 C10 1.359(8) . ? C11 C12 1.370(7) . ? C11 C16 1.388(7) . ? C12 C13 1.373(8) . ? C13 C14 1.354(10) . ? C14 C15 1.376(10) . ? C15 C16 1.375(8) . ? C17 C18 1.366(7) . ? C17 C22 1.387(7) . ? C18 C19 1.387(9) . ? C19 C20 1.360(12) . ? C20 C21 1.350(12) . ? C21 C22 1.381(9) . ? C23 C24 1.357(7) . ? C23 C28 1.382(7) . ? C24 C25 1.369(8) . ? C25 C26 1.356(8) . ? C26 C27 1.364(8) . ? C27 C28 1.389(7) . ? C29 C34 1.380(7) . ? C29 C30 1.385(7) . ? C30 C31 1.378(7) . ? C31 C32 1.382(9) . ? C32 C33 1.350(10) . ? C33 C34 1.393(8) . ? C35 C40 1.356(7) . ? C35 C36 1.378(7) . ? C36 C37 1.376(8) . ? C37 C38 1.357(9) . ? C38 C39 1.347(9) . ? C39 C40 1.389(8) . ? C41 C46 1.365(7) . ? C41 C42 1.380(7) . ? C42 C43 1.380(8) . ? C43 C44 1.341(9) . ? C44 C45 1.380(9) . ? C45 C46 1.387(9) . ? C47 C52 1.377(7) . ? C47 C48 1.390(7) . ? C48 C49 1.392(7) . ? C49 C50 1.348(8) . ? C50 C51 1.353(9) . ? C51 C52 1.389(8) . ? S1 C58 1.753(5) . ? S2 C53 1.750(5) . ? C53 C58 1.390(7) . ? C53 C54 1.391(7) . ? C54 C55 1.345(7) . ? C55 C56 1.374(8) . ? C56 C57 1.394(8) . ? C57 C58 1.392(7) . ? S3 C64 1.758(5) . ? S4 C59 1.745(5) . ? C59 C64 1.380(7) . ? C59 C60 1.400(7) . ? C60 C61 1.391(8) . ? C61 C62 1.358(9) . ? C62 C63 1.385(8) . ? C63 C64 1.395(7) . ? C65 Cl1 1.686(9) . ? C65 Cl3 1.707(9) . ? C65 Cl2 1.753(10) . ? C66 Cl5 1.695(7) . ? C66 Cl6 1.712(7) . ? C66 Cl4 1.717(7) . ? C67 Cl9 1.641(10) . ? C67 Cl7 1.759(10) . ? C67 Cl8 1.796(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pd1 S1 89.07(5) . . ? S2 Pd1 P2 87.46(4) . . ? S1 Pd1 P2 176.29(5) . . ? S2 Pd1 P1 173.34(5) . . ? S1 Pd1 P1 88.48(4) . . ? P2 Pd1 P1 95.12(4) . . ? S4 Pd2 P4 89.45(5) . . ? S4 Pd2 S3 89.05(5) . . ? P4 Pd2 S3 177.28(5) . . ? S4 Pd2 P3 171.48(5) . . ? P4 Pd2 P3 94.23(4) . . ? S3 Pd2 P3 87.57(5) . . ? C1 P1 C29 102.3(2) . . ? C1 P1 C35 98.3(2) . . ? C29 P1 C35 105.1(2) . . ? C1 P1 Pd1 116.58(15) . . ? C29 P1 Pd1 112.30(17) . . ? C35 P1 Pd1 119.88(16) . . ? C3 P2 C5 105.3(2) . . ? C3 P2 C11 100.0(2) . . ? C5 P2 C11 107.6(2) . . ? C3 P2 Pd1 109.73(16) . . ? C5 P2 Pd1 114.05(15) . . ? C11 P2 Pd1 118.58(16) . . ? C2 P3 C47 101.6(2) . . ? C2 P3 C41 96.9(2) . . ? C47 P3 C41 107.6(2) . . ? C2 P3 Pd2 118.38(16) . . ? C47 P3 Pd2 111.78(16) . . ? C41 P3 Pd2 118.42(16) . . ? C4 P4 C17 104.0(2) . . ? C4 P4 C23 101.1(2) . . ? C17 P4 C23 105.4(2) . . ? C4 P4 Pd2 109.41(16) . . ? C17 P4 Pd2 113.30(17) . . ? C23 P4 Pd2 121.69(15) . . ? C2 C1 P1 177.3(4) . . ? C1 C2 P3 172.2(4) . . ? C4 C3 P2 169.1(5) . . ? C3 C4 P4 175.7(4) . . ? C6 C5 C10 118.9(5) . . ? C6 C5 P2 122.5(4) . . ? C10 C5 P2 118.6(4) . . ? C5 C6 C7 119.4(5) . . ? C8 C7 C6 120.7(6) . . ? C9 C8 C7 119.7(6) . . ? C8 C9 C10 121.1(6) . . ? C9 C10 C5 120.2(6) . . ? C12 C11 C16 119.0(5) . . ? C12 C11 P2 122.3(4) . . ? C16 C11 P2 118.6(4) . . ? C11 C12 C13 120.6(6) . . ? C14 C13 C12 120.6(6) . . ? C13 C14 C15 119.7(6) . . ? C16 C15 C14 120.4(7) . . ? C15 C16 C11 119.7(6) . . ? C18 C17 C22 119.0(5) . . ? C18 C17 P4 123.5(4) . . ? C22 C17 P4 117.4(4) . . ? C17 C18 C19 120.4(7) . . ? C20 C19 C18 119.0(8) . . ? C21 C20 C19 122.2(8) . . ? C20 C21 C22 118.8(8) . . ? C21 C22 C17 120.5(7) . . ? C24 C23 C28 118.7(5) . . ? C24 C23 P4 121.1(4) . . ? C28 C23 P4 120.2(4) . . ? C23 C24 C25 120.7(5) . . ? C26 C25 C24 121.0(5) . . ? C25 C26 C27 119.8(6) . . ? C26 C27 C28 119.5(6) . . ? C23 C28 C27 120.4(5) . . ? C34 C29 C30 118.9(5) . . ? C34 C29 P1 118.8(4) . . ? C30 C29 P1 122.3(4) . . ? C31 C30 C29 121.0(6) . . ? C30 C31 C32 119.3(6) . . ? C33 C32 C31 120.1(6) . . ? C32 C33 C34 121.1(6) . . ? C29 C34 C33 119.5(6) . . ? C40 C35 C36 119.1(5) . . ? C40 C35 P1 119.2(4) . . ? C36 C35 P1 121.7(4) . . ? C37 C36 C35 120.6(6) . . ? C38 C37 C36 119.0(6) . . ? C39 C38 C37 121.5(6) . . ? C38 C39 C40 119.3(6) . . ? C35 C40 C39 120.4(6) . . ? C46 C41 C42 119.8(5) . . ? C46 C41 P3 118.2(4) . . ? C42 C41 P3 121.5(4) . . ? C43 C42 C41 120.2(6) . . ? C44 C43 C42 120.4(6) . . ? C43 C44 C45 119.9(6) . . ? C44 C45 C46 120.4(6) . . ? C41 C46 C45 119.2(6) . . ? C52 C47 C48 120.1(5) . . ? C52 C47 P3 118.1(4) . . ? C48 C47 P3 121.8(4) . . ? C47 C48 C49 118.5(5) . . ? C50 C49 C48 121.5(6) . . ? C49 C50 C51 119.5(6) . . ? C50 C51 C52 121.6(6) . . ? C47 C52 C51 118.8(5) . . ? C58 S1 Pd1 104.21(17) . . ? C53 S2 Pd1 104.40(17) . . ? C58 C53 C54 119.2(5) . . ? C58 C53 S2 121.1(4) . . ? C54 C53 S2 119.7(4) . . ? C55 C54 C53 121.6(6) . . ? C54 C55 C56 119.8(5) . . ? C55 C56 C57 120.5(5) . . ? C58 C57 C56 119.4(5) . . ? C53 C58 C57 119.4(5) . . ? C53 C58 S1 121.1(4) . . ? C57 C58 S1 119.5(4) . . ? C64 S3 Pd2 104.0(2) . . ? C59 S4 Pd2 104.12(19) . . ? C64 C59 C60 118.8(5) . . ? C64 C59 S4 121.9(4) . . ? C60 C59 S4 119.3(5) . . ? C61 C60 C59 120.3(6) . . ? C62 C61 C60 120.2(6) . . ? C61 C62 C63 120.5(6) . . ? C62 C63 C64 119.8(6) . . ? C59 C64 C63 120.3(5) . . ? C59 C64 S3 120.8(4) . . ? C63 C64 S3 118.9(5) . . ? Cl1 C65 Cl3 112.1(6) . . ? Cl1 C65 Cl2 107.9(6) . . ? Cl3 C65 Cl2 108.3(6) . . ? Cl5 C66 Cl6 110.2(4) . . ? Cl5 C66 Cl4 109.8(4) . . ? Cl6 C66 Cl4 113.7(4) . . ? Cl9 C67 Cl7 109.2(6) . . ? Cl9 C67 Cl8 106.6(6) . . ? Cl7 C67 Cl8 105.0(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.532 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.096 # Attachment 'Pd_Cl2bdtEND.cif' data_squeezed_[Pd(Cl2bdt)]2(u-dppa)2 _database_code_depnum_ccdc_archive 'CCDC 699935' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H48 Cl4 O2 P4 Pd2 S4' _chemical_formula_sum 'C64 H44 Cl4 O0 P4 Pd2 S4' _chemical_formula_weight 1419.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pd Pd -0.9988 1.0072 '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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.9243(13) _cell_length_b 17.0332(13) _cell_length_c 17.4498(13) _cell_angle_alpha 90.00 _cell_angle_beta 124.389(5) _cell_angle_gamma 90.00 _cell_volume 6603.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8832 _cell_measurement_theta_min 2.395 _cell_measurement_theta_max 28.292 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8301 _exptl_absorpt_correction_T_max 0.9716 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega & phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32067 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8196 _reflns_number_gt 5236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEXll' _computing_cell_refinement 'Bruker SMART APEXll' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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. SQUEEZE was used and two water molecules were removed. ; _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^)+(0.0699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8196 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Pd1 Pd 0.651878(10) 0.426645(17) 0.803290(14) 0.05522(11) Uani 1 1 d . . . C1 C 0.52271(13) 0.32452(19) 0.7508(2) 0.0550(8) Uani 1 1 d . . . C2 C 0.52633(14) 0.5052(2) 0.7780(2) 0.0581(8) Uani 1 1 d . . . P2 P 0.60506(3) 0.49728(6) 0.85682(5) 0.0569(2) Uani 1 1 d . . . C3 C 0.61384(14) 0.4536(2) 0.9585(2) 0.0606(9) Uani 1 1 d . . . C4 C 0.5746(2) 0.4678(3) 0.9830(3) 0.0877(12) Uani 1 1 d . . . H4 H 0.5413 0.4997 0.9458 0.105 Uiso 1 1 calc R . . C5 C 0.5840(3) 0.4356(3) 1.0613(4) 0.1070(17) Uani 1 1 d . . . H5 H 0.5566 0.4456 1.0765 0.128 Uiso 1 1 calc R . . C6 C 0.6318(2) 0.3895(3) 1.1174(3) 0.0961(14) Uani 1 1 d . . . H6 H 0.6381 0.3694 1.1718 0.115 Uiso 1 1 calc R . . C7 C 0.6709(2) 0.3728(4) 1.0939(3) 0.1144(18) Uani 1 1 d . . . H7 H 0.7038 0.3403 1.1316 0.137 Uiso 1 1 calc R . . C8 C 0.66152(18) 0.4043(3) 1.0135(3) 0.1006(16) Uani 1 1 d . . . H8 H 0.6878 0.3919 0.9967 0.121 Uiso 1 1 calc R . . C9 C 0.62453(15) 0.5999(2) 0.8857(2) 0.0652(9) Uani 1 1 d . . . C10 C 0.67033(18) 0.6224(3) 0.9744(3) 0.0936(14) Uani 1 1 d . . . H10 H 0.6912 0.5850 1.0208 0.112 Uiso 1 1 calc R . . C11 C 0.6851(2) 0.7015(4) 0.9938(4) 0.1127(18) Uani 1 1 d . . . H11 H 0.7157 0.7167 1.0537 0.135 Uiso 1 1 calc R . . C12 C 0.6556(3) 0.7562(4) 0.9269(4) 0.1125(18) Uani 1 1 d . . . H12 H 0.6663 0.8088 0.9408 0.135 Uiso 1 1 calc R . . C13 C 0.6106(3) 0.7353(3) 0.8400(4) 0.1079(16) Uani 1 1 d . . . H13 H 0.5898 0.7734 0.7943 0.129 Uiso 1 1 calc R . . C14 C 0.5954(2) 0.6561(3) 0.8188(3) 0.0811(12) Uani 1 1 d . . . H14 H 0.5652 0.6416 0.7585 0.097 Uiso 1 1 calc R . . S2 S 0.71879(4) 0.52794(6) 0.85027(6) 0.0624(2) Uani 1 1 d . . . C15 C 0.77390(14) 0.4923(2) 0.8348(2) 0.0631(9) Uani 1 1 d . . . C16 C 0.82310(19) 0.5387(3) 0.8575(3) 0.0879(12) Uani 1 1 d . . . Cl2 Cl 0.82742(7) 0.63423(9) 0.89503(13) 0.1342(6) Uani 1 1 d . . . C17 C 0.8673(2) 0.5118(4) 0.8490(4) 0.1029(15) Uani 1 1 d . . . H17 H 0.8997 0.5440 0.8649 0.123 Uiso 1 1 calc R . . C18 C 0.8642(2) 0.4377(4) 0.8171(4) 0.0979(15) Uani 1 1 d . . . H18 H 0.8946 0.4190 0.8119 0.117 Uiso 1 1 calc R . . C19 C 0.81605(17) 0.3910(3) 0.7928(3) 0.0748(10) Uani 1 1 d . . . Cl1 Cl 0.81357(6) 0.29792(8) 0.75387(10) 0.1104(4) Uani 1 1 d . . . C20 C 0.77024(14) 0.4174(2) 0.8015(2) 0.0620(9) Uani 1 1 d . . . S1 S 0.71033(4) 0.35529(7) 0.77152(7) 0.0778(3) Uani 1 1 d . . . P1 P 0.58809(3) 0.31946(6) 0.75111(5) 0.0541(2) Uani 1 1 d . . . C21 C 0.55525(13) 0.2879(2) 0.63166(19) 0.0543(8) Uani 1 1 d . . . C22 C 0.56786(16) 0.3253(2) 0.5754(2) 0.0687(10) Uani 1 1 d . . . H22 H 0.5940 0.3679 0.5975 0.082 Uiso 1 1 calc R . . C23 C 0.5414(2) 0.2991(3) 0.4848(3) 0.0870(13) Uani 1 1 d . . . H23 H 0.5504 0.3239 0.4466 0.104 Uiso 1 1 calc R . . C24 C 0.5024(2) 0.2376(3) 0.4515(3) 0.0926(14) Uani 1 1 d . . . H24 H 0.4845 0.2210 0.3905 0.111 Uiso 1 1 calc R . . C25 C 0.4900(2) 0.2009(3) 0.5069(3) 0.0981(14) Uani 1 1 d . . . H25 H 0.4634 0.1588 0.4839 0.118 Uiso 1 1 calc R . . C26 C 0.51644(18) 0.2251(3) 0.5979(2) 0.0810(11) Uani 1 1 d . . . H26 H 0.5079 0.1990 0.6360 0.097 Uiso 1 1 calc R . . C27 C 0.62302(14) 0.2329(2) 0.8228(2) 0.0659(9) Uani 1 1 d . . . C28 C 0.65062(17) 0.1778(3) 0.8004(3) 0.0830(12) Uani 1 1 d . . . H28 H 0.6508 0.1836 0.7476 0.100 Uiso 1 1 calc R . . C29 C 0.6785(2) 0.1122(3) 0.8597(4) 0.1045(15) Uani 1 1 d . . . H29 H 0.6962 0.0738 0.8447 0.125 Uiso 1 1 calc R . . C30 C 0.6796(2) 0.1048(4) 0.9374(4) 0.123(2) Uani 1 1 d . . . H30 H 0.6989 0.0620 0.9762 0.148 Uiso 1 1 calc R . . C31 C 0.6531(3) 0.1588(5) 0.9598(4) 0.140(2) Uani 1 1 d . . . H31 H 0.6541 0.1527 1.0136 0.167 Uiso 1 1 calc R . . C32 C 0.62432(19) 0.2233(3) 0.9027(3) 0.0999(15) Uani 1 1 d . . . H32 H 0.6059 0.2602 0.9182 0.120 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03956(13) 0.0834(2) 0.04399(13) -0.00471(11) 0.02437(10) -0.00023(12) C1 0.0535(17) 0.066(2) 0.0474(14) -0.0020(14) 0.0300(14) 0.0012(15) C2 0.0463(14) 0.068(2) 0.0562(16) -0.0036(14) 0.0268(13) 0.0007(15) P2 0.0364(4) 0.0859(7) 0.0450(4) -0.0114(4) 0.0211(3) -0.0039(4) C3 0.0469(16) 0.088(3) 0.0465(15) -0.0114(15) 0.0262(14) -0.0054(17) C4 0.091(3) 0.105(3) 0.097(3) 0.011(3) 0.071(3) 0.022(3) C5 0.127(4) 0.130(4) 0.114(4) 0.017(3) 0.098(4) 0.024(4) C6 0.112(4) 0.122(4) 0.067(2) -0.009(3) 0.059(3) -0.007(3) C7 0.088(3) 0.182(6) 0.064(2) 0.033(3) 0.038(2) 0.034(4) C8 0.061(2) 0.185(5) 0.0564(19) 0.023(2) 0.0335(18) 0.029(3) C9 0.0528(18) 0.089(3) 0.0622(18) -0.0177(19) 0.0378(16) -0.0136(18) C10 0.064(2) 0.107(4) 0.081(2) -0.030(2) 0.024(2) -0.015(2) C11 0.086(3) 0.130(5) 0.096(3) -0.041(3) 0.036(3) -0.042(3) C12 0.127(4) 0.112(4) 0.121(4) -0.037(4) 0.084(4) -0.054(4) C13 0.139(4) 0.110(4) 0.100(3) -0.016(3) 0.082(3) -0.046(3) C14 0.096(3) 0.095(3) 0.071(2) -0.020(2) 0.059(2) -0.029(3) S2 0.0512(4) 0.0799(6) 0.0600(4) 0.0019(4) 0.0338(4) 0.0011(4) C15 0.0471(17) 0.086(3) 0.0601(17) 0.0157(18) 0.0326(15) 0.0047(17) C16 0.072(3) 0.101(3) 0.105(3) 0.012(3) 0.058(2) -0.001(2) Cl2 0.1366(12) 0.1123(11) 0.2043(16) -0.0383(11) 0.1268(13) -0.0428(9) C17 0.075(3) 0.123(5) 0.138(4) 0.010(3) 0.076(3) -0.011(3) C18 0.074(3) 0.132(4) 0.116(4) 0.031(3) 0.071(3) 0.023(3) C19 0.062(2) 0.099(3) 0.076(2) 0.023(2) 0.0467(18) 0.019(2) Cl1 0.0989(8) 0.1259(11) 0.1342(10) -0.0039(8) 0.0827(8) 0.0247(8) C20 0.0463(16) 0.089(3) 0.0540(16) 0.0135(17) 0.0303(14) 0.0085(17) S1 0.0583(5) 0.0971(8) 0.0920(6) -0.0207(6) 0.0510(5) -0.0052(5) P1 0.0439(4) 0.0778(6) 0.0427(4) -0.0016(4) 0.0257(3) 0.0027(4) C21 0.0477(16) 0.070(2) 0.0441(14) -0.0029(14) 0.0254(13) 0.0040(16) C22 0.066(2) 0.092(3) 0.0503(16) -0.0018(17) 0.0340(16) -0.002(2) C23 0.094(3) 0.119(4) 0.0565(19) 0.003(2) 0.048(2) 0.001(3) C24 0.098(3) 0.119(4) 0.0550(19) -0.021(2) 0.040(2) -0.007(3) C25 0.109(3) 0.111(4) 0.068(2) -0.029(2) 0.046(2) -0.032(3) C26 0.086(3) 0.099(3) 0.063(2) -0.012(2) 0.044(2) -0.015(2) C27 0.0474(17) 0.088(3) 0.0526(16) 0.0085(17) 0.0226(14) 0.0051(18) C28 0.071(2) 0.093(3) 0.077(2) 0.013(2) 0.037(2) 0.012(2) C29 0.075(3) 0.101(4) 0.112(4) 0.027(3) 0.037(3) 0.029(3) C30 0.082(3) 0.159(6) 0.096(3) 0.068(4) 0.031(3) 0.035(4) C31 0.114(4) 0.200(7) 0.087(3) 0.071(4) 0.047(3) 0.046(5) C32 0.082(3) 0.156(4) 0.058(2) 0.030(3) 0.037(2) 0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S2 2.2861(10) . ? Pd1 P2 2.2889(9) . ? Pd1 S1 2.2906(10) . ? Pd1 P1 2.3120(9) . ? C1 C1 1.206(6) 2_656 ? C1 P1 1.760(3) . ? C2 C2 1.183(6) 2_656 ? C2 P2 1.764(3) . ? P2 C3 1.812(3) . ? P2 C9 1.813(4) . ? C3 C4 1.366(5) . ? C3 C8 1.372(5) . ? C4 C5 1.357(6) . ? C5 C6 1.345(7) . ? C6 C7 1.357(6) . ? C7 C8 1.386(6) . ? C9 C14 1.363(5) . ? C9 C10 1.381(5) . ? C10 C11 1.390(7) . ? C11 C12 1.348(7) . ? C12 C13 1.350(7) . ? C13 C14 1.397(6) . ? S2 C15 1.760(4) . ? C15 C20 1.382(5) . ? C15 C16 1.394(5) . ? C16 C17 1.360(6) . ? C16 Cl2 1.733(5) . ? C17 C18 1.362(7) . ? C18 C19 1.369(6) . ? C19 C20 1.400(5) . ? C19 Cl1 1.710(5) . ? C20 S1 1.744(4) . ? P1 C27 1.815(4) . ? P1 C21 1.826(3) . ? C21 C22 1.364(4) . ? C21 C26 1.373(5) . ? C22 C23 1.390(5) . ? C23 C24 1.358(6) . ? C24 C25 1.342(6) . ? C25 C26 1.387(5) . ? C27 C28 1.383(5) . ? C27 C32 1.385(5) . ? C28 C29 1.416(6) . ? C29 C30 1.345(7) . ? C30 C31 1.350(8) . ? C31 C32 1.389(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pd1 P2 87.76(3) . . ? S2 Pd1 S1 88.70(4) . . ? P2 Pd1 S1 171.76(3) . . ? S2 Pd1 P1 175.45(3) . . ? P2 Pd1 P1 96.78(3) . . ? S1 Pd1 P1 86.84(3) . . ? C1 C1 P1 177.01(17) 2_656 . ? C2 C2 P2 174.8(2) 2_656 . ? C2 P2 C3 103.30(16) . . ? C2 P2 C9 100.03(17) . . ? C3 P2 C9 105.46(16) . . ? C2 P2 Pd1 114.73(11) . . ? C3 P2 Pd1 112.74(12) . . ? C9 P2 Pd1 118.73(11) . . ? C4 C3 C8 118.2(4) . . ? C4 C3 P2 122.5(3) . . ? C8 C3 P2 119.3(3) . . ? C5 C4 C3 120.4(4) . . ? C6 C5 C4 121.7(4) . . ? C5 C6 C7 119.3(4) . . ? C6 C7 C8 119.7(5) . . ? C3 C8 C7 120.5(4) . . ? C14 C9 C10 118.8(4) . . ? C14 C9 P2 120.2(3) . . ? C10 C9 P2 120.9(3) . . ? C9 C10 C11 119.5(5) . . ? C12 C11 C10 120.8(5) . . ? C11 C12 C13 120.4(5) . . ? C12 C13 C14 119.7(5) . . ? C9 C14 C13 120.7(4) . . ? C15 S2 Pd1 104.27(14) . . ? C20 C15 C16 118.3(4) . . ? C20 C15 S2 121.1(3) . . ? C16 C15 S2 120.6(3) . . ? C17 C16 C15 121.9(5) . . ? C17 C16 Cl2 118.8(4) . . ? C15 C16 Cl2 119.3(3) . . ? C16 C17 C18 120.0(5) . . ? C17 C18 C19 119.7(4) . . ? C18 C19 C20 121.2(4) . . ? C18 C19 Cl1 118.7(3) . . ? C20 C19 Cl1 120.1(3) . . ? C15 C20 C19 119.0(3) . . ? C15 C20 S1 121.4(3) . . ? C19 C20 S1 119.7(3) . . ? C20 S1 Pd1 104.54(13) . . ? C1 P1 C27 99.78(16) . . ? C1 P1 C21 99.94(14) . . ? C27 P1 C21 105.98(16) . . ? C1 P1 Pd1 118.80(11) . . ? C27 P1 Pd1 112.94(11) . . ? C21 P1 Pd1 117.09(12) . . ? C22 C21 C26 119.6(3) . . ? C22 C21 P1 121.8(3) . . ? C26 C21 P1 118.6(2) . . ? C21 C22 C23 119.5(4) . . ? C24 C23 C22 120.7(4) . . ? C25 C24 C23 119.8(4) . . ? C24 C25 C26 120.7(4) . . ? C21 C26 C25 119.8(4) . . ? C28 C27 C32 119.5(4) . . ? C28 C27 P1 120.6(3) . . ? C32 C27 P1 119.8(3) . . ? C27 C28 C29 118.5(4) . . ? C30 C29 C28 120.7(5) . . ? C29 C30 C31 120.9(5) . . ? C30 C31 C32 120.2(5) . . ? C27 C32 C31 120.1(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.789 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.073 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.063 424.6 30.5 2 0.000 0.500 0.740 424.5 30.5 _platon_squeeze_details ; ; # Attachment 'Pd_tdtEND.cif' data_squeezed_[Pd(tdt)]2(u-dppa)2 _database_code_depnum_ccdc_archive 'CCDC 699936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H56 Cl4 P4 Pd2 S4' _chemical_formula_sum 'C66 H52 Cl0 P4 Pd2 S4' _chemical_formula_weight 1310.00 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' Pd Pd -0.9988 1.0072 '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 10.8273(7) _cell_length_b 14.6236(10) _cell_length_c 21.0611(13) _cell_angle_alpha 97.031(2) _cell_angle_beta 97.023(2) _cell_angle_gamma 91.372(2) _cell_volume 3282.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8239 _cell_measurement_theta_min 2.243 _cell_measurement_theta_max 27.299 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9233 _exptl_absorpt_correction_T_max 0.9454 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54698 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0981 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 28.48 _reflns_number_total 16198 _reflns_number_gt 8971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEXll' _computing_cell_refinement 'Bruker SMART APEXll' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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. SQUEEZE was used and two methylene chloride molecules were removed. ; _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^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16198 _refine_ls_number_parameters 687 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _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 Pd1 Pd -0.07987(2) 0.750240(17) 0.407110(12) 0.03999(8) Uani 1 1 d . . . Pd2 Pd 0.19000(3) 0.71192(2) 0.107563(13) 0.04947(9) Uani 1 1 d . . . P1 P 0.04679(9) 0.63590(6) 0.37519(4) 0.0429(2) Uani 1 1 d . . . P2 P 0.00546(9) 0.85849(6) 0.35338(4) 0.0419(2) Uani 1 1 d . . . P3 P 0.23246(9) 0.61764(7) 0.18549(4) 0.0506(2) Uani 1 1 d . . . P4 P -0.00501(9) 0.75075(6) 0.13296(4) 0.0437(2) Uani 1 1 d . . . C1 C 0.1128(3) 0.6431(2) 0.30386(18) 0.0470(8) Uani 1 1 d . . . C2 C 0.1548(3) 0.6364(3) 0.25412(18) 0.0487(9) Uani 1 1 d . . . C3 C -0.0057(3) 0.8274(2) 0.26920(16) 0.0447(8) Uani 1 1 d . . . C4 C -0.0079(3) 0.7981(2) 0.21356(17) 0.0455(8) Uani 1 1 d . . . S1 S -0.16281(9) 0.64596(7) 0.46471(5) 0.0538(2) Uani 1 1 d . . . S2 S -0.20218(9) 0.85959(6) 0.45193(5) 0.0519(2) Uani 1 1 d . . . S3 S 0.38209(11) 0.67606(10) 0.07886(6) 0.0790(4) Uani 1 1 d . . . S4 S 0.15243(12) 0.78144(8) 0.01651(5) 0.0722(3) Uani 1 1 d . . . C5 C -0.2643(4) 0.8065(3) 0.51179(18) 0.0551(10) Uani 1 1 d . . . C6 C -0.3322(4) 0.8572(4) 0.5552(2) 0.0744(13) Uani 1 1 d . . . H6 H -0.3459 0.9189 0.5513 0.089 Uiso 1 1 calc R . . C7 C -0.3794(5) 0.8178(5) 0.6037(2) 0.0939(17) Uani 1 1 d . . . H7 H -0.4248 0.8527 0.6320 0.113 Uiso 1 1 calc R . . C8 C -0.3593(5) 0.7252(4) 0.6106(2) 0.0853(15) Uani 1 1 d . . . C9 C -0.4016(10) 0.6904(7) 0.6678(4) 0.193(4) Uani 1 1 d . . . H9A H -0.3530 0.7205 0.7062 0.289 Uiso 1 1 calc R . . H9B H -0.3913 0.6251 0.6651 0.289 Uiso 1 1 calc R . . H9C H -0.4878 0.7031 0.6693 0.289 Uiso 1 1 calc R . . C10 C -0.2942(4) 0.6749(3) 0.5675(2) 0.0683(12) Uani 1 1 d . . . H10 H -0.2820 0.6129 0.5711 0.082 Uiso 1 1 calc R . . C11 C -0.2461(3) 0.7141(3) 0.51858(18) 0.0545(10) Uani 1 1 d . . . C12 C 0.2804(6) 0.7568(3) -0.0248(2) 0.0785(15) Uani 1 1 d . . . C13 C 0.2825(7) 0.7840(4) -0.0864(2) 0.1025(19) Uani 1 1 d . . . H13 H 0.2163 0.8151 -0.1051 0.123 Uiso 1 1 calc R . . C14 C 0.3864(9) 0.7636(5) -0.1197(3) 0.120(3) Uani 1 1 d . . . C15 C 0.3980(9) 0.7899(7) -0.1828(4) 0.175(4) Uani 1 1 d . . . H15A H 0.4574 0.8407 -0.1787 0.263 Uiso 1 1 calc R . . H15B H 0.3186 0.8079 -0.2019 0.263 Uiso 1 1 calc R . . H15C H 0.4256 0.7386 -0.2097 0.263 Uiso 1 1 calc R . . C16 C 0.4825(9) 0.7205(6) -0.0908(4) 0.135(3) Uani 1 1 d . . . H16 H 0.5521 0.7100 -0.1121 0.162 Uiso 1 1 calc R . . C17 C 0.4821(5) 0.6920(4) -0.0321(3) 0.102(2) Uani 1 1 d . . . H17 H 0.5484 0.6599 -0.0148 0.123 Uiso 1 1 calc R . . C18 C 0.3807(5) 0.7115(4) 0.0024(2) 0.0803(15) Uani 1 1 d . . . C19 C -0.0628(4) 0.9709(2) 0.35958(16) 0.0482(9) Uani 1 1 d . . . C20 C -0.0099(4) 1.0425(2) 0.40344(18) 0.0574(10) Uani 1 1 d . . . H20 H 0.0654 1.0352 0.4284 0.069 Uiso 1 1 calc R . . C21 C -0.0679(5) 1.1252(3) 0.4106(2) 0.0707(12) Uani 1 1 d . . . H21 H -0.0308 1.1737 0.4400 0.085 Uiso 1 1 calc R . . C22 C -0.1775(5) 1.1365(3) 0.3758(2) 0.0791(14) Uani 1 1 d . . . H22 H -0.2169 1.1923 0.3811 0.095 Uiso 1 1 calc R . . C23 C -0.2313(5) 1.0642(3) 0.3317(3) 0.0835(14) Uani 1 1 d . . . H23 H -0.3069 1.0717 0.3071 0.100 Uiso 1 1 calc R . . C24 C -0.1750(4) 0.9828(3) 0.3240(2) 0.0690(12) Uani 1 1 d . . . H24 H -0.2124 0.9346 0.2945 0.083 Uiso 1 1 calc R . . C25 C 0.1722(3) 0.8761(2) 0.37679(17) 0.0497(9) Uani 1 1 d . . . C26 C 0.2521(4) 0.8948(3) 0.3342(2) 0.0716(12) Uani 1 1 d . . . H26 H 0.2209 0.9015 0.2920 0.086 Uiso 1 1 calc R . . C27 C 0.3792(5) 0.9039(4) 0.3534(3) 0.0929(17) Uani 1 1 d . . . H27 H 0.4337 0.9168 0.3246 0.111 Uiso 1 1 calc R . . C28 C 0.4230(5) 0.8933(4) 0.4159(4) 0.1000(19) Uani 1 1 d . . . H28 H 0.5084 0.8977 0.4289 0.120 Uiso 1 1 calc R . . C29 C 0.3461(6) 0.8769(4) 0.4581(3) 0.0994(18) Uani 1 1 d . . . H29 H 0.3779 0.8718 0.5006 0.119 Uiso 1 1 calc R . . C30 C 0.2202(4) 0.8673(3) 0.4395(2) 0.0740(13) Uani 1 1 d . . . H30 H 0.1670 0.8549 0.4691 0.089 Uiso 1 1 calc R . . C31 C -0.0247(3) 0.5206(2) 0.35100(17) 0.0464(8) Uani 1 1 d . . . C32 C 0.0192(4) 0.4444(3) 0.3780(2) 0.0621(11) Uani 1 1 d . . . H32 H 0.0811 0.4515 0.4132 0.075 Uiso 1 1 calc R . . C33 C -0.0284(5) 0.3583(3) 0.3529(2) 0.0810(14) Uani 1 1 d . . . H33 H 0.0018 0.3071 0.3710 0.097 Uiso 1 1 calc R . . C34 C -0.1186(5) 0.3466(3) 0.3022(2) 0.0796(14) Uani 1 1 d . . . H34 H -0.1492 0.2875 0.2853 0.096 Uiso 1 1 calc R . . C35 C -0.1664(4) 0.4225(3) 0.2748(2) 0.0763(13) Uani 1 1 d . . . H35 H -0.2299 0.4148 0.2404 0.092 Uiso 1 1 calc R . . C36 C -0.1179(4) 0.5087(3) 0.2995(2) 0.0645(11) Uani 1 1 d . . . H36 H -0.1482 0.5598 0.2814 0.077 Uiso 1 1 calc R . . C37 C 0.1834(3) 0.6228(2) 0.43223(17) 0.0485(9) Uani 1 1 d . . . C38 C 0.1676(4) 0.6124(3) 0.49526(18) 0.0611(10) Uani 1 1 d . . . H38 H 0.0885 0.6151 0.5082 0.073 Uiso 1 1 calc R . . C39 C 0.2699(5) 0.5981(3) 0.5391(2) 0.0754(13) Uani 1 1 d . . . H39 H 0.2591 0.5887 0.5810 0.090 Uiso 1 1 calc R . . C40 C 0.3850(4) 0.5979(4) 0.5207(2) 0.0835(15) Uani 1 1 d . . . H40 H 0.4534 0.5886 0.5501 0.100 Uiso 1 1 calc R . . C41 C 0.4020(5) 0.6110(4) 0.4596(3) 0.0920(16) Uani 1 1 d . . . H41 H 0.4821 0.6118 0.4479 0.110 Uiso 1 1 calc R . . C42 C 0.3024(4) 0.6233(3) 0.4149(2) 0.0744(13) Uani 1 1 d . . . H42 H 0.3150 0.6319 0.3732 0.089 Uiso 1 1 calc R . . C43 C 0.1879(4) 0.4978(3) 0.15724(18) 0.0599(10) Uani 1 1 d . . . C44 C 0.1278(6) 0.4436(3) 0.1919(3) 0.0960(18) Uani 1 1 d . . . H44 H 0.1083 0.4677 0.2323 0.115 Uiso 1 1 calc R . . C45 C 0.0947(7) 0.3525(4) 0.1681(4) 0.128(3) Uani 1 1 d . . . H45 H 0.0587 0.3149 0.1939 0.154 Uiso 1 1 calc R . . C46 C 0.1141(7) 0.3178(4) 0.1081(3) 0.112(2) Uani 1 1 d . . . H46 H 0.0868 0.2582 0.0909 0.134 Uiso 1 1 calc R . . C47 C 0.1744(7) 0.3722(5) 0.0735(3) 0.115(2) Uani 1 1 d . . . H47 H 0.1901 0.3484 0.0324 0.139 Uiso 1 1 calc R . . C48 C 0.2137(6) 0.4617(4) 0.0968(2) 0.0899(16) Uani 1 1 d . . . H48 H 0.2567 0.4971 0.0722 0.108 Uiso 1 1 calc R . . C49 C -0.1144(3) 0.6529(2) 0.12375(16) 0.0483(9) Uani 1 1 d . . . C50 C -0.2198(4) 0.6556(3) 0.1535(2) 0.0634(11) Uani 1 1 d . . . H50 H -0.2355 0.7080 0.1806 0.076 Uiso 1 1 calc R . . C51 C -0.3026(5) 0.5811(4) 0.1434(2) 0.0814(14) Uani 1 1 d . . . H51 H -0.3756 0.5838 0.1626 0.098 Uiso 1 1 calc R . . C52 C -0.2780(5) 0.5032(4) 0.1052(2) 0.0834(15) Uani 1 1 d . . . H52 H -0.3337 0.4526 0.0989 0.100 Uiso 1 1 calc R . . C53 C -0.1700(5) 0.4992(3) 0.0757(2) 0.0754(13) Uani 1 1 d . . . H53 H -0.1526 0.4459 0.0499 0.090 Uiso 1 1 calc R . . C54 C -0.0899(4) 0.5741(3) 0.08494(19) 0.0578(10) Uani 1 1 d . . . H54 H -0.0180 0.5722 0.0649 0.069 Uiso 1 1 calc R . . C55 C -0.0847(4) 0.8383(3) 0.09078(16) 0.0521(9) Uani 1 1 d . . . C56 C -0.1948(4) 0.8200(3) 0.0516(2) 0.0700(12) Uani 1 1 d . . . H56 H -0.2342 0.7620 0.0473 0.084 Uiso 1 1 calc R . . C57 C -0.2470(5) 0.8878(4) 0.0184(2) 0.0907(16) Uani 1 1 d . . . H57 H -0.3206 0.8743 -0.0093 0.109 Uiso 1 1 calc R . . C58 C -0.1943(6) 0.9732(4) 0.0249(3) 0.0972(17) Uani 1 1 d . . . H58 H -0.2324 1.0185 0.0030 0.117 Uiso 1 1 calc R . . C59 C -0.0836(6) 0.9928(4) 0.0644(3) 0.0995(18) Uani 1 1 d . . . H59 H -0.0467 1.0517 0.0695 0.119 Uiso 1 1 calc R . . C60 C -0.0277(5) 0.9255(3) 0.0961(2) 0.0795(14) Uani 1 1 d . . . H60 H 0.0488 0.9382 0.1213 0.095 Uiso 1 1 calc R . . C61 C 0.3891(4) 0.6183(4) 0.22875(18) 0.0655(12) Uani 1 1 d . . . C62 C 0.4511(4) 0.7027(4) 0.2465(3) 0.0925(17) Uani 1 1 d . . . H62 H 0.4217 0.7554 0.2300 0.111 Uiso 1 1 calc R . . C63 C 0.5609(5) 0.7065(6) 0.2906(3) 0.128(3) Uani 1 1 d . . . H63 H 0.6038 0.7626 0.3045 0.154 Uiso 1 1 calc R . . C64 C 0.6038(6) 0.6288(8) 0.3126(3) 0.135(3) Uani 1 1 d . . . H64 H 0.6761 0.6324 0.3417 0.162 Uiso 1 1 calc R . . C65 C 0.5436(6) 0.5456(7) 0.2933(3) 0.123(2) Uani 1 1 d . . . H65 H 0.5758 0.4928 0.3084 0.148 Uiso 1 1 calc R . . C66 C 0.4349(4) 0.5395(4) 0.2511(2) 0.0878(15) Uani 1 1 d . . . H66 H 0.3929 0.4828 0.2380 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04269(16) 0.04085(15) 0.03551(14) 0.00051(10) 0.00579(11) 0.00057(11) Pd2 0.04814(17) 0.05973(19) 0.03956(16) -0.00004(13) 0.00989(12) -0.00768(13) P1 0.0460(5) 0.0444(5) 0.0383(5) 0.0033(4) 0.0075(4) 0.0030(4) P2 0.0492(5) 0.0399(5) 0.0345(4) -0.0016(4) 0.0040(4) -0.0010(4) P3 0.0439(5) 0.0674(6) 0.0393(5) 0.0006(4) 0.0068(4) 0.0042(5) P4 0.0505(5) 0.0460(5) 0.0331(4) 0.0002(4) 0.0053(4) -0.0026(4) C1 0.047(2) 0.044(2) 0.050(2) 0.0051(16) 0.0063(17) 0.0014(16) C2 0.046(2) 0.053(2) 0.046(2) 0.0009(17) 0.0082(17) 0.0039(17) C3 0.057(2) 0.0386(19) 0.0383(19) 0.0033(15) 0.0052(16) 0.0020(16) C4 0.050(2) 0.044(2) 0.041(2) 0.0016(15) 0.0037(16) 0.0031(16) S1 0.0558(6) 0.0516(6) 0.0574(6) 0.0117(4) 0.0158(5) 0.0019(4) S2 0.0555(6) 0.0481(5) 0.0521(5) -0.0020(4) 0.0152(4) 0.0046(4) S3 0.0550(7) 0.1116(10) 0.0705(7) -0.0025(7) 0.0247(6) -0.0052(6) S4 0.0927(9) 0.0759(7) 0.0525(6) 0.0164(5) 0.0211(6) -0.0058(6) C5 0.051(2) 0.068(3) 0.044(2) -0.0041(18) 0.0096(17) -0.0017(19) C6 0.073(3) 0.084(3) 0.066(3) -0.005(2) 0.025(2) 0.008(2) C7 0.088(4) 0.128(5) 0.067(3) -0.016(3) 0.043(3) -0.003(3) C8 0.082(4) 0.115(5) 0.061(3) 0.005(3) 0.025(3) -0.015(3) C9 0.243(11) 0.211(10) 0.137(7) 0.033(7) 0.072(7) -0.037(8) C10 0.062(3) 0.088(3) 0.058(3) 0.016(2) 0.014(2) -0.007(2) C11 0.048(2) 0.072(3) 0.043(2) 0.0056(18) 0.0061(17) -0.0040(19) C12 0.111(4) 0.067(3) 0.056(3) -0.008(2) 0.032(3) -0.037(3) C13 0.154(6) 0.089(4) 0.068(3) 0.004(3) 0.043(4) -0.037(4) C14 0.175(8) 0.121(6) 0.063(4) -0.014(3) 0.055(5) -0.070(5) C15 0.211(9) 0.221(10) 0.100(5) 0.022(6) 0.053(6) -0.039(7) C16 0.151(7) 0.152(7) 0.100(6) -0.044(5) 0.086(5) -0.085(6) C17 0.088(4) 0.120(4) 0.094(4) -0.033(3) 0.047(3) -0.052(3) C18 0.082(3) 0.088(3) 0.067(3) -0.022(3) 0.036(3) -0.041(3) C19 0.062(2) 0.043(2) 0.0403(19) 0.0025(15) 0.0100(17) -0.0038(17) C20 0.078(3) 0.043(2) 0.049(2) -0.0027(17) 0.0043(19) -0.0024(19) C21 0.104(4) 0.049(2) 0.056(3) -0.0037(19) 0.008(3) 0.002(2) C22 0.109(4) 0.045(3) 0.086(3) 0.009(2) 0.019(3) 0.022(3) C23 0.082(3) 0.066(3) 0.100(4) 0.009(3) -0.005(3) 0.019(3) C24 0.073(3) 0.047(2) 0.079(3) -0.003(2) -0.013(2) 0.006(2) C25 0.052(2) 0.046(2) 0.049(2) -0.0027(16) 0.0066(18) -0.0051(17) C26 0.060(3) 0.087(3) 0.063(3) -0.009(2) 0.009(2) -0.012(2) C27 0.060(3) 0.106(4) 0.108(4) -0.028(3) 0.033(3) -0.010(3) C28 0.054(3) 0.088(4) 0.146(6) -0.014(4) -0.010(4) 0.005(3) C29 0.079(4) 0.115(5) 0.096(4) 0.023(3) -0.028(3) -0.017(3) C30 0.065(3) 0.089(3) 0.065(3) 0.017(2) -0.010(2) -0.010(2) C31 0.045(2) 0.046(2) 0.048(2) 0.0023(16) 0.0110(16) 0.0017(16) C32 0.073(3) 0.049(2) 0.064(3) 0.011(2) 0.003(2) 0.000(2) C33 0.104(4) 0.049(3) 0.088(3) 0.013(2) -0.005(3) 0.001(2) C34 0.091(4) 0.061(3) 0.083(3) -0.001(2) 0.012(3) -0.020(3) C35 0.076(3) 0.072(3) 0.073(3) -0.004(2) -0.009(2) -0.010(2) C36 0.062(3) 0.056(2) 0.072(3) 0.011(2) -0.005(2) 0.001(2) C37 0.051(2) 0.047(2) 0.048(2) 0.0030(16) 0.0074(17) 0.0039(17) C38 0.058(2) 0.079(3) 0.045(2) 0.008(2) 0.0010(19) 0.003(2) C39 0.081(3) 0.093(3) 0.048(2) 0.012(2) -0.009(2) -0.003(3) C40 0.055(3) 0.118(4) 0.073(3) 0.011(3) -0.014(2) 0.001(3) C41 0.057(3) 0.143(5) 0.078(4) 0.026(3) 0.003(3) 0.007(3) C42 0.057(3) 0.107(4) 0.061(3) 0.018(3) 0.007(2) 0.010(2) C43 0.062(3) 0.070(3) 0.045(2) -0.0015(19) 0.0033(19) 0.017(2) C44 0.133(5) 0.072(3) 0.084(3) -0.020(3) 0.056(3) -0.021(3) C45 0.170(7) 0.078(4) 0.136(6) -0.029(4) 0.073(5) -0.032(4) C46 0.151(6) 0.075(4) 0.099(5) -0.024(4) 0.008(4) -0.002(4) C47 0.182(7) 0.088(4) 0.068(3) -0.022(3) 0.012(4) 0.032(4) C48 0.134(5) 0.080(4) 0.056(3) -0.004(2) 0.027(3) 0.013(3) C49 0.052(2) 0.051(2) 0.0401(19) 0.0015(16) 0.0039(16) -0.0069(17) C50 0.055(2) 0.066(3) 0.069(3) -0.005(2) 0.021(2) -0.006(2) C51 0.068(3) 0.087(4) 0.089(3) 0.000(3) 0.026(3) -0.023(3) C52 0.083(4) 0.076(3) 0.085(3) 0.004(3) 0.001(3) -0.029(3) C53 0.081(3) 0.060(3) 0.076(3) -0.013(2) -0.002(3) -0.012(2) C54 0.055(2) 0.054(2) 0.060(2) -0.0067(19) 0.0074(19) -0.0082(19) C55 0.065(3) 0.053(2) 0.0368(19) 0.0009(16) 0.0069(17) 0.0007(19) C56 0.085(3) 0.054(2) 0.064(3) 0.000(2) -0.009(2) 0.004(2) C57 0.108(4) 0.073(3) 0.081(3) 0.010(3) -0.030(3) 0.017(3) C58 0.124(5) 0.080(4) 0.086(4) 0.030(3) -0.018(3) 0.006(3) C59 0.123(5) 0.063(3) 0.117(5) 0.035(3) 0.011(4) -0.003(3) C60 0.090(4) 0.059(3) 0.086(3) 0.017(2) -0.004(3) -0.011(2) C61 0.045(2) 0.105(4) 0.042(2) -0.007(2) 0.0073(18) 0.011(2) C62 0.057(3) 0.105(4) 0.100(4) -0.037(3) -0.004(3) 0.011(3) C63 0.061(4) 0.174(7) 0.121(5) -0.073(5) -0.007(3) 0.006(4) C64 0.062(4) 0.247(11) 0.085(4) -0.022(6) 0.001(3) 0.037(6) C65 0.069(4) 0.202(8) 0.104(5) 0.045(5) 0.001(4) 0.038(5) C66 0.058(3) 0.130(5) 0.082(3) 0.036(3) 0.008(3) 0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2778(9) . ? Pd1 S2 2.2890(10) . ? Pd1 S1 2.2930(10) . ? Pd1 P2 2.2943(9) . ? Pd2 S4 2.2765(11) . ? Pd2 P3 2.2816(11) . ? Pd2 S3 2.2910(12) . ? Pd2 P4 2.3078(10) . ? P1 C1 1.754(4) . ? P1 C37 1.818(4) . ? P1 C31 1.825(4) . ? P2 C3 1.764(4) . ? P2 C19 1.815(4) . ? P2 C25 1.816(4) . ? P3 C2 1.756(4) . ? P3 C43 1.815(4) . ? P3 C61 1.824(4) . ? P4 C4 1.757(4) . ? P4 C49 1.811(4) . ? P4 C55 1.821(4) . ? C1 C2 1.186(5) . ? C3 C4 1.195(4) . ? S1 C11 1.764(4) . ? S2 C5 1.751(4) . ? S3 C18 1.750(6) . ? S4 C12 1.746(6) . ? C5 C11 1.393(6) . ? C5 C6 1.397(6) . ? C6 C7 1.377(7) . ? C7 C8 1.399(8) . ? C8 C10 1.372(7) . ? C8 C9 1.480(9) . ? C10 C11 1.386(6) . ? C12 C18 1.385(7) . ? C12 C13 1.406(7) . ? C13 C14 1.416(10) . ? C14 C16 1.350(11) . ? C14 C15 1.448(9) . ? C16 C17 1.351(10) . ? C17 C18 1.405(7) . ? C19 C20 1.372(5) . ? C19 C24 1.373(5) . ? C20 C21 1.377(6) . ? C21 C22 1.342(6) . ? C22 C23 1.385(7) . ? C23 C24 1.351(6) . ? C25 C26 1.366(6) . ? C25 C30 1.381(5) . ? C26 C27 1.385(6) . ? C27 C28 1.370(8) . ? C28 C29 1.329(8) . ? C29 C30 1.370(7) . ? C31 C36 1.379(5) . ? C31 C32 1.381(5) . ? C32 C33 1.367(6) . ? C33 C34 1.348(6) . ? C34 C35 1.394(6) . ? C35 C36 1.370(6) . ? C37 C42 1.381(6) . ? C37 C38 1.385(5) . ? C38 C39 1.391(6) . ? C39 C40 1.350(7) . ? C40 C41 1.357(7) . ? C41 C42 1.373(6) . ? C43 C44 1.347(6) . ? C43 C48 1.381(6) . ? C44 C45 1.388(7) . ? C45 C46 1.346(8) . ? C46 C47 1.349(9) . ? C47 C48 1.377(8) . ? C49 C50 1.366(5) . ? C49 C54 1.379(5) . ? C50 C51 1.374(6) . ? C51 C52 1.362(7) . ? C52 C53 1.389(7) . ? C53 C54 1.360(6) . ? C55 C56 1.365(5) . ? C55 C60 1.389(6) . ? C56 C57 1.376(6) . ? C57 C58 1.345(7) . ? C58 C59 1.375(7) . ? C59 C60 1.368(7) . ? C61 C62 1.378(7) . ? C61 C66 1.379(7) . ? C62 C63 1.411(8) . ? C63 C64 1.350(11) . ? C64 C65 1.359(10) . ? C65 C66 1.379(8) . ? 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 Pd1 S2 172.76(3) . . ? P1 Pd1 S1 86.02(4) . . ? S2 Pd1 S1 88.68(4) . . ? P1 Pd1 P2 95.16(3) . . ? S2 Pd1 P2 89.97(3) . . ? S1 Pd1 P2 177.64(3) . . ? S4 Pd2 P3 169.01(4) . . ? S4 Pd2 S3 88.53(5) . . ? P3 Pd2 S3 85.82(4) . . ? S4 Pd2 P4 89.29(4) . . ? P3 Pd2 P4 96.34(3) . . ? S3 Pd2 P4 177.81(4) . . ? C1 P1 C37 101.81(17) . . ? C1 P1 C31 96.04(16) . . ? C37 P1 C31 106.36(17) . . ? C1 P1 Pd1 117.58(12) . . ? C37 P1 Pd1 115.13(12) . . ? C31 P1 Pd1 117.24(12) . . ? C3 P2 C19 102.39(16) . . ? C3 P2 C25 102.77(17) . . ? C19 P2 C25 107.67(17) . . ? C3 P2 Pd1 114.10(12) . . ? C19 P2 Pd1 116.34(12) . . ? C25 P2 Pd1 112.26(13) . . ? C2 P3 C43 101.10(19) . . ? C2 P3 C61 96.39(17) . . ? C43 P3 C61 106.4(2) . . ? C2 P3 Pd2 117.54(13) . . ? C43 P3 Pd2 112.79(13) . . ? C61 P3 Pd2 119.94(16) . . ? C4 P4 C49 102.82(17) . . ? C4 P4 C55 100.71(16) . . ? C49 P4 C55 105.92(18) . . ? C4 P4 Pd2 114.45(12) . . ? C49 P4 Pd2 113.43(13) . . ? C55 P4 Pd2 117.73(13) . . ? C2 C1 P1 171.8(3) . . ? C1 C2 P3 172.2(3) . . ? C4 C3 P2 173.3(3) . . ? C3 C4 P4 176.9(3) . . ? C11 S1 Pd1 104.00(14) . . ? C5 S2 Pd1 103.95(14) . . ? C18 S3 Pd2 104.3(2) . . ? C12 S4 Pd2 104.7(2) . . ? C11 C5 C6 118.0(4) . . ? C11 C5 S2 121.7(3) . . ? C6 C5 S2 120.2(3) . . ? C7 C6 C5 121.4(5) . . ? C6 C7 C8 120.1(5) . . ? C10 C8 C7 118.6(5) . . ? C10 C8 C9 124.4(7) . . ? C7 C8 C9 116.9(6) . . ? C8 C10 C11 121.7(5) . . ? C10 C11 C5 120.2(4) . . ? C10 C11 S1 119.6(3) . . ? C5 C11 S1 120.2(3) . . ? C18 C12 C13 119.4(5) . . ? C18 C12 S4 121.1(4) . . ? C13 C12 S4 119.5(5) . . ? C12 C13 C14 119.2(7) . . ? C16 C14 C13 119.1(6) . . ? C16 C14 C15 117.5(8) . . ? C13 C14 C15 123.4(9) . . ? C14 C16 C17 122.9(7) . . ? C16 C17 C18 119.4(7) . . ? C12 C18 C17 119.9(5) . . ? C12 C18 S3 121.0(4) . . ? C17 C18 S3 119.1(5) . . ? C20 C19 C24 118.9(4) . . ? C20 C19 P2 121.1(3) . . ? C24 C19 P2 119.8(3) . . ? C19 C20 C21 120.2(4) . . ? C22 C21 C20 120.7(4) . . ? C21 C22 C23 119.2(4) . . ? C24 C23 C22 120.7(5) . . ? C23 C24 C19 120.4(4) . . ? C26 C25 C30 118.8(4) . . ? C26 C25 P2 122.5(3) . . ? C30 C25 P2 118.7(3) . . ? C25 C26 C27 120.6(5) . . ? C28 C27 C26 118.6(5) . . ? C29 C28 C27 121.4(5) . . ? C28 C29 C30 120.3(5) . . ? C29 C30 C25 120.2(5) . . ? C36 C31 C32 119.2(3) . . ? C36 C31 P1 118.0(3) . . ? C32 C31 P1 122.4(3) . . ? C33 C32 C31 119.9(4) . . ? C34 C33 C32 120.9(4) . . ? C33 C34 C35 120.4(4) . . ? C36 C35 C34 118.7(4) . . ? C35 C36 C31 120.9(4) . . ? C42 C37 C38 118.9(4) . . ? C42 C37 P1 122.3(3) . . ? C38 C37 P1 118.8(3) . . ? C37 C38 C39 119.9(4) . . ? C40 C39 C38 119.8(4) . . ? C39 C40 C41 120.7(4) . . ? C40 C41 C42 120.7(5) . . ? C41 C42 C37 119.8(4) . . ? C44 C43 C48 118.9(4) . . ? C44 C43 P3 122.8(3) . . ? C48 C43 P3 118.3(4) . . ? C43 C44 C45 120.8(5) . . ? C46 C45 C44 120.8(6) . . ? C45 C46 C47 118.1(6) . . ? C46 C47 C48 122.6(5) . . ? C47 C48 C43 118.7(5) . . ? C50 C49 C54 119.6(4) . . ? C50 C49 P4 122.0(3) . . ? C54 C49 P4 118.4(3) . . ? C49 C50 C51 120.2(4) . . ? C52 C51 C50 120.0(5) . . ? C51 C52 C53 120.3(4) . . ? C54 C53 C52 119.2(4) . . ? C53 C54 C49 120.7(4) . . ? C56 C55 C60 118.9(4) . . ? C56 C55 P4 122.4(3) . . ? C60 C55 P4 118.5(3) . . ? C55 C56 C57 119.6(4) . . ? C58 C57 C56 121.7(5) . . ? C57 C58 C59 119.3(5) . . ? C60 C59 C58 119.9(5) . . ? C59 C60 C55 120.4(5) . . ? C62 C61 C66 121.4(4) . . ? C62 C61 P3 117.3(4) . . ? C66 C61 P3 120.6(4) . . ? C61 C62 C63 117.7(6) . . ? C64 C63 C62 120.2(7) . . ? C63 C64 C65 121.6(7) . . ? C64 C65 C66 119.9(7) . . ? C65 C66 C61 119.2(6) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.48 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.152 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.080 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.208 0.000 0.000 483.8 131.5 _platon_squeeze_details ; ; # Attachment 'pt_Cl2bdtEND.cif' data_pt_cdt_[Pt(Cl2bdt)]2(u-dppa)2 _database_code_depnum_ccdc_archive 'CCDC 699937' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H46 Cl4 O P4 Pt2 S4' _chemical_formula_weight 1615.11 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.3763(16) _cell_length_b 11.0230(4) _cell_length_c 31.0144(12) _cell_angle_alpha 90.00 _cell_angle_beta 118.554(2) _cell_angle_gamma 90.00 _cell_volume 12725.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6288 _exptl_absorpt_coefficient_mu 4.833 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6017 _exptl_absorpt_correction_T_max 0.7537 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega & phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59345 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0961 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 28.36 _reflns_number_total 15807 _reflns_number_gt 8828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEXll' _computing_cell_refinement 'Bruker SMART APEXll' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^)+(0.0454P)^2^+25.8902P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15807 _refine_ls_number_parameters 764 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.1235 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _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 Pt1 Pt 0.106513(7) 1.01100(2) 0.087086(10) 0.03938(9) Uani 1 1 d . . . Pt2 Pt 0.139929(8) 0.67754(3) 0.306970(10) 0.04449(9) Uani 1 1 d . A . S1 S 0.08345(6) 1.19347(18) 0.04908(7) 0.0526(5) Uani 1 1 d . . . S2 S 0.13280(5) 0.98756(17) 0.03777(7) 0.0487(5) Uani 1 1 d . . . S3 S 0.10744(5) 0.55314(18) 0.33150(7) 0.0525(5) Uani 1 1 d . . . S4 S 0.19106(6) 0.5819(2) 0.36367(8) 0.0631(6) Uani 1 1 d . . . P1 P 0.08312(5) 1.05865(17) 0.13774(7) 0.0427(5) Uani 1 1 d . A . P2 P 0.12485(5) 0.81978(17) 0.11544(7) 0.0410(4) Uani 1 1 d . A . P3 P 0.08791(5) 0.77886(18) 0.25644(7) 0.0435(5) Uani 1 1 d . . . P4 P 0.17609(5) 0.79071(19) 0.28725(7) 0.0474(5) Uani 1 1 d . . . C1 C 0.08571(19) 0.9492(7) 0.1813(3) 0.0464(18) Uani 1 1 d . . . C2 C 0.08798(18) 0.8788(7) 0.2118(3) 0.0448(18) Uani 1 1 d . A . C3 C 0.14797(19) 0.8050(6) 0.1802(3) 0.0452(18) Uani 1 1 d . . . C4 C 0.16081(19) 0.8004(7) 0.2232(3) 0.0480(19) Uani 1 1 d . A . C5 C 0.10223(19) 1.2154(7) 0.0102(3) 0.0467(18) Uani 1 1 d . . . C6 C 0.0967(2) 1.3213(7) -0.0164(3) 0.054(2) Uani 1 1 d . . . C7 C 0.1115(3) 1.3398(9) -0.0467(3) 0.079(3) Uani 1 1 d . . . H7 H 0.1075 1.4127 -0.0637 0.094 Uiso 1 1 calc R . . C8 C 0.1318(3) 1.2530(9) -0.0520(3) 0.084(3) Uani 1 1 d . . . H8 H 0.1420 1.2656 -0.0724 0.101 Uiso 1 1 calc R . . C9 C 0.1373(2) 1.1447(8) -0.0267(3) 0.065(2) Uani 1 1 d . . . C10 C 0.12349(18) 1.1243(7) 0.0052(2) 0.0457(18) Uani 1 1 d . . . C11 C 0.1403(2) 0.4640(7) 0.3786(3) 0.056(2) Uani 1 1 d . . . C12 C 0.1306(2) 0.3750(8) 0.4026(3) 0.065(2) Uani 1 1 d . . . C13 C 0.1557(3) 0.3063(8) 0.4408(4) 0.078(3) Uani 1 1 d . . . H13 H 0.1486 0.2484 0.4562 0.094 Uiso 1 1 calc R . . C14 C 0.1915(3) 0.3250(9) 0.4556(4) 0.085(3) Uani 1 1 d . . . H14 H 0.2087 0.2804 0.4816 0.103 Uiso 1 1 calc R . . C15 C 0.2020(3) 0.4078(8) 0.4326(3) 0.076(3) Uani 1 1 d . . . C16 C 0.1769(2) 0.4802(7) 0.3938(3) 0.061(2) Uani 1 1 d . . . C17 C 0.1042(2) 1.1889(7) 0.1771(3) 0.053(2) Uani 1 1 d . . . C18 C 0.1303(2) 1.2537(7) 0.1737(3) 0.060(2) Uani 1 1 d . A . H18 H 0.1376 1.2304 0.1510 0.072 Uiso 1 1 calc R . . C19 C 0.1460(3) 1.3533(8) 0.2032(4) 0.082(3) Uani 1 1 d . . . H19 H 0.1641 1.3956 0.2008 0.099 Uiso 1 1 calc R A . C20 C 0.1351(3) 1.3892(10) 0.2353(5) 0.108(5) Uani 1 1 d . A . H20 H 0.1451 1.4578 0.2545 0.130 Uiso 1 1 calc R . . C21 C 0.1096(4) 1.3254(12) 0.2396(4) 0.116(4) Uani 1 1 d . . . H21 H 0.1021 1.3502 0.2620 0.139 Uiso 1 1 calc R A . C22 C 0.0943(3) 1.2233(9) 0.2111(3) 0.078(3) Uani 1 1 d . A . H22 H 0.0773 1.1785 0.2151 0.094 Uiso 1 1 calc R . . C23 C 0.03519(19) 1.0911(7) 0.1069(2) 0.0461(18) Uani 1 1 d . . . C24 C 0.0220(2) 1.2058(8) 0.1007(3) 0.068(3) Uani 1 1 d . A . H24 H 0.0379 1.2708 0.1130 0.082 Uiso 1 1 calc R . . C25 C -0.0149(2) 1.2276(10) 0.0761(4) 0.079(3) Uani 1 1 d . . . H25 H -0.0233 1.3067 0.0732 0.095 Uiso 1 1 calc R A . C26 C -0.0383(3) 1.1372(11) 0.0565(3) 0.075(3) Uani 1 1 d . A . H26 H -0.0628 1.1528 0.0399 0.090 Uiso 1 1 calc R . . C27 C -0.0258(3) 1.0219(11) 0.0612(4) 0.088(3) Uani 1 1 d . . . H27 H -0.0420 0.9585 0.0468 0.106 Uiso 1 1 calc R A . C28 C 0.0112(2) 0.9969(8) 0.0875(4) 0.075(3) Uani 1 1 d . A . H28 H 0.0194 0.9173 0.0918 0.090 Uiso 1 1 calc R . . C29 C 0.1564(2) 0.7437(7) 0.0999(3) 0.0503(19) Uani 1 1 d . . . C30 C 0.1911(2) 0.7855(11) 0.1220(4) 0.089(3) Uani 1 1 d . A . H30 H 0.1982 0.8496 0.1442 0.107 Uiso 1 1 calc R . . C31 C 0.2154(4) 0.7281(18) 0.1100(6) 0.143(6) Uani 1 1 d . . . H31 H 0.2389 0.7570 0.1233 0.171 Uiso 1 1 calc R A . C32 C 0.2056(5) 0.6329(18) 0.0798(7) 0.147(7) Uani 1 1 d . A . H32 H 0.2227 0.5919 0.0746 0.176 Uiso 1 1 calc R . . C33 C 0.1709(5) 0.5952(12) 0.0565(5) 0.126(5) Uani 1 1 d . . . H33 H 0.1638 0.5328 0.0336 0.151 Uiso 1 1 calc R A . C34 C 0.1461(3) 0.6513(9) 0.0673(4) 0.086(3) Uani 1 1 d . A . H34 H 0.1224 0.6251 0.0521 0.103 Uiso 1 1 calc R . . C35 C 0.08843(19) 0.7146(6) 0.0978(3) 0.0451(18) Uani 1 1 d . . . C36 C 0.0548(2) 0.7429(7) 0.0598(3) 0.056(2) Uani 1 1 d . A . H36 H 0.0510 0.8179 0.0444 0.068 Uiso 1 1 calc R . . C37 C 0.0267(2) 0.6597(8) 0.0443(3) 0.071(3) Uani 1 1 d . . . H37 H 0.0039 0.6796 0.0192 0.086 Uiso 1 1 calc R A . C38 C 0.0328(3) 0.5512(9) 0.0659(4) 0.087(3) Uani 1 1 d . A . H38 H 0.0142 0.4952 0.0554 0.105 Uiso 1 1 calc R . . C39 C 0.0665(3) 0.5201(9) 0.1037(4) 0.101(4) Uani 1 1 d . . . H39 H 0.0705 0.4434 0.1179 0.122 Uiso 1 1 calc R A . C40 C 0.0938(2) 0.6035(7) 0.1200(4) 0.076(3) Uani 1 1 d . A . H40 H 0.1161 0.5846 0.1464 0.091 Uiso 1 1 calc R . . C41 C 0.1809(2) 0.9466(7) 0.3069(3) 0.053(2) Uani 1 1 d . A . C42 C 0.1895(2) 1.0370(9) 0.2840(3) 0.076(3) Uani 1 1 d . . . H42 H 0.1925 1.0183 0.2569 0.091 Uiso 1 1 calc R A . C43 C 0.1936(3) 1.1543(10) 0.3001(4) 0.097(4) Uani 1 1 d . A . H43 H 0.1995 1.2138 0.2839 0.116 Uiso 1 1 calc R . . C44 C 0.1894(3) 1.1854(10) 0.3391(5) 0.101(4) Uani 1 1 d . . . H44 H 0.1921 1.2653 0.3499 0.121 Uiso 1 1 calc R A . C45 C 0.1810(3) 1.0954(13) 0.3618(5) 0.128(5) Uani 1 1 d . A . H45 H 0.1782 1.1142 0.3890 0.154 Uiso 1 1 calc R . . C47A C 0.0496(2) 0.6956(9) 0.2160(4) 0.052(5) Uani 0.582(9) 1 d PGU A 1 C48A C 0.0497(2) 0.5709(9) 0.2094(4) 0.068(4) Uani 0.582(9) 1 d PGU A 1 H48A H 0.0707 0.5267 0.2270 0.082 Uiso 0.582(9) 1 calc PR A 1 C49A C 0.0183(3) 0.5123(8) 0.1764(4) 0.100(7) Uani 0.582(9) 1 d PGU A 1 H49A H 0.0184 0.4288 0.1719 0.121 Uiso 0.582(9) 1 calc PR A 1 C50A C -0.0131(2) 0.5783(10) 0.1500(4) 0.103(7) Uani 0.582(9) 1 d PGU A 1 H50A H -0.0341 0.5391 0.1279 0.123 Uiso 0.582(9) 1 calc PR A 1 C51A C -0.0132(2) 0.7030(10) 0.1566(4) 0.097(6) Uani 0.582(9) 1 d PGU A 1 H51A H -0.0342 0.7472 0.1390 0.116 Uiso 0.582(9) 1 calc PR A 1 C52A C 0.0182(3) 0.7616(7) 0.1896(4) 0.069(5) Uani 0.582(9) 1 d PGU A 1 H52A H 0.0181 0.8451 0.1941 0.083 Uiso 0.582(9) 1 calc PR A 1 C46 C 0.1764(3) 0.9750(10) 0.3453(4) 0.103(4) Uani 1 1 d . . . H46 H 0.1702 0.9152 0.3611 0.123 Uiso 1 1 calc R A . C47B C 0.0470(3) 0.6885(13) 0.2206(6) 0.044(7) Uani 0.418(9) 1 d PGU A 2 C48B C 0.0283(4) 0.6332(13) 0.2420(4) 0.057(5) Uani 0.418(9) 1 d PGU A 2 H48B H 0.0355 0.6459 0.2750 0.068 Uiso 0.418(9) 1 calc PR A 2 C49B C -0.0009(3) 0.5589(13) 0.2140(6) 0.063(6) Uani 0.418(9) 1 d PGU A 2 H49B H -0.0133 0.5218 0.2283 0.076 Uiso 0.418(9) 1 calc PR A 2 C50B C -0.0115(4) 0.5399(17) 0.1646(6) 0.18(2) Uiso 0.418(9) 1 d PG A 2 H50B H -0.0311 0.4902 0.1459 0.213 Uiso 0.418(9) 1 calc PR A 2 C51B C 0.0071(5) 0.595(2) 0.1433(5) 0.179(18) Uiso 0.418(9) 1 d PG A 2 H51B H 0.0000 0.5826 0.1102 0.214 Uiso 0.418(9) 1 calc PR A 2 C52B C 0.0363(5) 0.6696(17) 0.1713(6) 0.115(13) Uani 0.418(9) 1 d PGU A 2 H52B H 0.0488 0.7066 0.1570 0.138 Uiso 0.418(9) 1 calc PR A 2 C60 C 0.2282(3) 0.6491(12) 0.2836(4) 0.111(4) Uani 1 1 d . . . H60 H 0.2095 0.6213 0.2541 0.134 Uiso 1 1 calc R A . C53B C 0.0780(3) 0.8797(10) 0.2922(4) 0.054(5) Uani 0.506(8) 1 d PGU A 1 C54B C 0.0614(3) 0.8339(9) 0.3182(4) 0.066(5) Uani 0.506(8) 1 d PGU A 1 H54B H 0.0548 0.7527 0.3151 0.079 Uiso 0.506(8) 1 calc PR A 1 C55B C 0.0548(3) 0.9097(12) 0.3487(4) 0.082(6) Uani 0.506(8) 1 d PGU A 1 H55B H 0.0437 0.8791 0.3661 0.098 Uiso 0.506(8) 1 calc PR A 1 C56B C 0.0646(4) 1.0312(11) 0.3534(4) 0.093(9) Uani 0.506(8) 1 d PGU A 1 H56B H 0.0602 1.0819 0.3738 0.112 Uiso 0.506(8) 1 calc PR A 1 C57B C 0.0812(4) 1.0769(9) 0.3274(5) 0.096(7) Uani 0.506(8) 1 d PGU A 1 H57B H 0.0878 1.1582 0.3305 0.115 Uiso 0.506(8) 1 calc PR A 1 C58B C 0.0879(3) 1.0012(11) 0.2969(4) 0.078(6) Uani 0.506(8) 1 d PGU A 1 H58B H 0.0989 1.0317 0.2795 0.094 Uiso 0.506(8) 1 calc PR A 1 C59 C 0.2217(2) 0.7359(9) 0.3090(3) 0.064(2) Uani 1 1 d . A . C53A C 0.0696(3) 0.8845(10) 0.2856(4) 0.042(5) Uani 0.494(8) 1 d PGU A 2 C54A C 0.0872(3) 0.8989(11) 0.3363(4) 0.063(5) Uani 0.494(8) 1 d PGU A 2 H54A H 0.1077 0.8535 0.3557 0.075 Uiso 0.494(8) 1 calc PR A 2 C55A C 0.0743(3) 0.9813(12) 0.3580(3) 0.084(7) Uani 0.494(8) 1 d PGU A 2 H55A H 0.0861 0.9910 0.3919 0.101 Uiso 0.494(8) 1 calc PR A 2 C56A C 0.0437(3) 1.0493(11) 0.3290(5) 0.078(6) Uani 0.494(8) 1 d PGU A 2 H56A H 0.0351 1.1044 0.3436 0.094 Uiso 0.494(8) 1 calc PR A 2 C57A C 0.0261(3) 1.0348(11) 0.2783(5) 0.079(6) Uani 0.494(8) 1 d PGU A 2 H57A H 0.0057 1.0803 0.2590 0.095 Uiso 0.494(8) 1 calc PR A 2 C58A C 0.0391(3) 0.9525(12) 0.2566(3) 0.071(5) Uani 0.494(8) 1 d PGU A 2 H58A H 0.0273 0.9428 0.2227 0.086 Uiso 0.494(8) 1 calc PR A 2 C61 C 0.2629(4) 0.6001(18) 0.3014(7) 0.179(8) Uani 1 1 d . A . H61 H 0.2676 0.5400 0.2842 0.215 Uiso 1 1 calc R . . C62 C 0.2895(4) 0.644(2) 0.3447(9) 0.171(10) Uani 1 1 d . . . H62 H 0.3128 0.6143 0.3566 0.205 Uiso 1 1 calc R A . C63 C 0.2832(4) 0.7279(18) 0.3704(8) 0.169(9) Uani 1 1 d . A . H63 H 0.3017 0.7542 0.4003 0.202 Uiso 1 1 calc R . . C64 C 0.2486(3) 0.7770(11) 0.3524(5) 0.122(5) Uani 1 1 d . . . H64 H 0.2441 0.8367 0.3700 0.146 Uiso 1 1 calc R A . Cl1 Cl 0.07022(7) 1.4363(2) -0.01049(9) 0.0768(7) Uani 1 1 d . . . Cl2 Cl 0.16356(8) 1.0342(2) -0.03434(11) 0.0968(9) Uani 1 1 d . . . Cl3 Cl 0.08538(8) 0.3510(2) 0.38460(11) 0.0976(9) Uani 1 1 d . . . Cl4 Cl 0.24682(7) 0.4257(3) 0.45084(11) 0.1138(11) Uani 1 1 d . . . O1 O 0.2338(4) 0.3197(12) 0.0176(4) 0.228(6) 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 Pt1 0.04498(16) 0.03738(17) 0.03831(16) 0.00093(13) 0.02195(13) -0.00363(13) Pt2 0.04831(17) 0.04658(18) 0.03564(16) 0.00174(13) 0.01768(13) 0.00114(14) S1 0.0680(13) 0.0481(12) 0.0524(12) 0.0114(9) 0.0374(11) 0.0081(10) S2 0.0572(11) 0.0484(12) 0.0507(11) 0.0051(9) 0.0339(10) 0.0043(10) S3 0.0617(12) 0.0469(11) 0.0521(12) 0.0038(9) 0.0296(10) 0.0028(10) S4 0.0557(13) 0.0717(15) 0.0526(13) 0.0170(11) 0.0186(11) 0.0107(11) P1 0.0476(11) 0.0407(11) 0.0411(11) 0.0016(9) 0.0223(9) 0.0008(9) P2 0.0458(10) 0.0405(11) 0.0375(10) 0.0023(9) 0.0206(9) 0.0010(9) P3 0.0498(11) 0.0456(11) 0.0374(10) 0.0011(9) 0.0226(9) 0.0006(9) P4 0.0444(11) 0.0574(13) 0.0372(11) 0.0018(9) 0.0170(9) 0.0005(10) C1 0.048(4) 0.053(5) 0.042(4) 0.005(4) 0.025(4) 0.013(4) C2 0.049(4) 0.043(4) 0.045(4) 0.001(4) 0.025(4) -0.001(4) C3 0.050(4) 0.045(4) 0.043(4) 0.000(4) 0.024(4) 0.003(4) C4 0.048(4) 0.054(5) 0.037(4) 0.003(4) 0.016(4) 0.011(4) C5 0.053(5) 0.048(5) 0.039(4) 0.004(4) 0.022(4) -0.001(4) C6 0.070(5) 0.047(5) 0.048(5) 0.012(4) 0.030(4) 0.004(4) C7 0.105(8) 0.062(6) 0.076(7) 0.027(5) 0.050(6) 0.008(6) C8 0.135(9) 0.073(7) 0.078(7) 0.019(6) 0.079(7) 0.008(7) C9 0.092(6) 0.063(6) 0.061(5) 0.004(5) 0.053(5) 0.004(5) C10 0.048(4) 0.058(5) 0.038(4) 0.006(4) 0.027(4) 0.002(4) C11 0.076(6) 0.041(5) 0.052(5) -0.002(4) 0.030(5) 0.006(4) C12 0.087(6) 0.045(5) 0.078(6) 0.003(5) 0.052(5) 0.003(5) C13 0.118(9) 0.047(5) 0.077(7) 0.021(5) 0.052(7) 0.014(6) C14 0.127(10) 0.064(7) 0.061(6) 0.022(5) 0.042(7) 0.032(7) C15 0.099(7) 0.064(6) 0.056(6) 0.011(5) 0.031(5) 0.025(6) C16 0.079(6) 0.059(5) 0.043(5) 0.003(4) 0.027(4) 0.013(5) C17 0.054(5) 0.050(5) 0.048(5) -0.004(4) 0.020(4) -0.001(4) C18 0.062(5) 0.047(5) 0.063(6) -0.005(4) 0.023(5) 0.001(4) C19 0.081(7) 0.048(6) 0.096(8) -0.011(5) 0.024(6) -0.008(5) C20 0.097(9) 0.068(8) 0.118(10) -0.052(7) 0.017(8) -0.006(7) C21 0.132(11) 0.120(11) 0.098(9) -0.066(8) 0.056(8) 0.000(9) C22 0.100(7) 0.074(7) 0.078(7) -0.026(5) 0.056(6) -0.018(6) C23 0.052(5) 0.053(5) 0.036(4) 0.004(4) 0.024(4) 0.001(4) C24 0.044(5) 0.058(6) 0.098(7) 0.014(5) 0.030(5) -0.001(4) C25 0.062(6) 0.080(7) 0.098(8) 0.030(6) 0.039(6) 0.013(6) C26 0.063(6) 0.108(9) 0.052(5) 0.001(6) 0.026(5) 0.008(6) C27 0.062(6) 0.110(9) 0.077(7) -0.041(6) 0.020(5) -0.029(6) C28 0.062(6) 0.068(6) 0.092(7) -0.017(5) 0.033(5) -0.008(5) C29 0.060(5) 0.053(5) 0.048(5) 0.014(4) 0.034(4) 0.013(4) C30 0.062(6) 0.128(9) 0.090(7) -0.004(7) 0.046(6) 0.016(6) C31 0.084(9) 0.24(2) 0.122(12) 0.020(12) 0.059(9) 0.052(11) C32 0.153(15) 0.195(19) 0.149(16) 0.059(13) 0.118(14) 0.095(15) C33 0.186(14) 0.108(10) 0.134(12) -0.027(9) 0.118(12) 0.019(11) C34 0.108(8) 0.079(7) 0.104(8) -0.022(6) 0.077(7) 0.004(6) C35 0.047(4) 0.040(4) 0.046(4) 0.000(3) 0.020(4) 0.002(3) C36 0.072(6) 0.047(5) 0.053(5) 0.002(4) 0.032(5) -0.004(4) C37 0.059(5) 0.065(6) 0.072(6) 0.000(5) 0.016(5) -0.011(5) C38 0.086(8) 0.065(7) 0.102(8) -0.008(6) 0.038(7) -0.031(6) C39 0.094(8) 0.055(6) 0.125(10) 0.028(6) 0.027(8) -0.003(6) C40 0.068(6) 0.048(5) 0.093(7) 0.024(5) 0.023(5) -0.014(5) C41 0.052(5) 0.062(5) 0.047(5) -0.007(4) 0.027(4) -0.006(4) C42 0.079(7) 0.078(7) 0.064(6) 0.001(5) 0.029(5) 0.002(5) C43 0.119(9) 0.060(7) 0.086(8) -0.006(6) 0.029(7) -0.011(6) C44 0.094(8) 0.073(8) 0.124(10) -0.041(8) 0.043(8) -0.022(6) C45 0.164(12) 0.134(12) 0.130(11) -0.071(10) 0.105(10) -0.068(10) C47A 0.064(10) 0.059(10) 0.037(11) 0.003(9) 0.028(8) -0.001(8) C48A 0.058(8) 0.068(8) 0.059(10) -0.010(8) 0.013(7) -0.004(7) C49A 0.106(12) 0.072(10) 0.067(11) -0.026(9) -0.004(9) -0.018(8) C50A 0.055(9) 0.137(12) 0.076(12) -0.070(12) -0.002(8) -0.033(9) C51A 0.056(9) 0.101(10) 0.103(14) 0.022(10) 0.014(8) -0.016(8) C52A 0.052(8) 0.070(9) 0.073(11) -0.008(8) 0.020(8) -0.001(6) C46 0.152(10) 0.095(8) 0.102(8) -0.052(7) 0.094(8) -0.073(7) C47B 0.036(12) 0.056(17) 0.049(13) -0.007(13) 0.028(11) 0.003(11) C48B 0.052(11) 0.066(13) 0.051(11) -0.002(9) 0.024(9) -0.013(9) C49B 0.055(11) 0.088(16) 0.064(13) -0.016(11) 0.043(10) -0.021(9) C52B 0.079(16) 0.22(3) 0.074(14) -0.077(19) 0.057(14) -0.09(2) C60 0.097(8) 0.154(12) 0.101(9) 0.034(8) 0.063(7) 0.056(8) C53B 0.052(11) 0.062(10) 0.045(12) 0.008(10) 0.022(8) 0.005(9) C54B 0.090(13) 0.066(10) 0.066(12) 0.017(8) 0.057(11) 0.037(9) C55B 0.104(17) 0.094(12) 0.059(12) -0.006(10) 0.049(11) 0.019(11) C56B 0.12(2) 0.102(14) 0.087(18) -0.032(15) 0.068(17) 0.006(16) C57B 0.16(2) 0.080(12) 0.065(13) -0.013(10) 0.072(13) 0.006(13) C58B 0.101(14) 0.068(10) 0.084(14) -0.029(10) 0.059(11) -0.010(10) C59 0.046(5) 0.087(7) 0.055(5) 0.026(5) 0.021(5) 0.010(5) C53A 0.045(9) 0.046(11) 0.044(9) -0.018(9) 0.029(7) -0.006(7) C54A 0.066(11) 0.077(13) 0.045(8) -0.018(9) 0.026(7) 0.000(9) C55A 0.074(13) 0.12(2) 0.059(11) -0.055(12) 0.031(9) -0.011(12) C56A 0.077(14) 0.082(14) 0.095(11) -0.039(12) 0.056(11) -0.013(10) C57A 0.069(11) 0.094(15) 0.088(10) 0.003(11) 0.048(9) 0.026(10) C58A 0.071(11) 0.096(14) 0.055(9) 0.004(9) 0.036(8) 0.027(9) C61 0.119(12) 0.27(2) 0.182(17) 0.072(16) 0.099(12) 0.107(15) C62 0.057(9) 0.21(2) 0.22(3) 0.11(2) 0.053(12) 0.030(13) C63 0.072(11) 0.19(2) 0.169(18) 0.052(15) -0.003(10) 0.018(11) C64 0.071(7) 0.128(10) 0.105(9) 0.016(8) -0.008(7) 0.002(7) Cl1 0.0966(17) 0.0570(13) 0.0825(16) 0.0174(12) 0.0473(14) 0.0171(12) Cl2 0.132(2) 0.0942(19) 0.114(2) 0.0248(16) 0.099(2) 0.0301(17) Cl3 0.118(2) 0.0620(16) 0.135(2) 0.0164(16) 0.078(2) -0.0064(15) Cl4 0.0824(19) 0.128(3) 0.101(2) 0.0454(19) 0.0189(16) 0.0333(18) O1 0.293(15) 0.261(15) 0.154(10) 0.059(9) 0.126(10) -0.038(11) _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 Pt1 P2 2.2730(18) . ? Pt1 P1 2.284(2) . ? Pt1 S2 2.2971(19) . ? Pt1 S1 2.2997(19) . ? Pt2 P4 2.275(2) . ? Pt2 S4 2.293(2) . ? Pt2 P3 2.2933(19) . ? Pt2 S3 2.314(2) . ? S1 C5 1.750(8) . ? S2 C10 1.751(7) . ? S3 C11 1.758(8) . ? S4 C16 1.739(9) . ? P1 C1 1.774(8) . ? P1 C17 1.818(8) . ? P1 C23 1.820(7) . ? P2 C3 1.771(8) . ? P2 C35 1.794(7) . ? P2 C29 1.828(8) . ? P3 C53B 1.758(8) . ? P3 C47A 1.762(7) . ? P3 C2 1.772(8) . ? P3 C47B 1.842(11) . ? P3 C53A 1.856(8) . ? P4 C4 1.774(8) . ? P4 C41 1.802(8) . ? P4 C59 1.819(8) . ? C1 C2 1.191(9) . ? C3 C4 1.177(9) . ? C5 C6 1.382(10) . ? C5 C10 1.406(10) . ? C6 C7 1.374(12) . ? C6 Cl1 1.759(8) . ? C7 C8 1.350(12) . ? C8 C9 1.387(11) . ? C9 C10 1.389(10) . ? C9 Cl2 1.739(9) . ? C11 C16 1.401(11) . ? C11 C12 1.408(11) . ? C12 C13 1.379(12) . ? C12 Cl3 1.741(9) . ? C13 C14 1.374(13) . ? C14 C15 1.357(13) . ? C15 C16 1.411(11) . ? C15 Cl4 1.715(10) . ? C17 C22 1.360(11) . ? C17 C18 1.364(11) . ? C18 C19 1.380(11) . ? C19 C20 1.344(15) . ? C20 C21 1.348(16) . ? C21 C22 1.386(13) . ? C23 C24 1.358(10) . ? C23 C28 1.374(10) . ? C24 C25 1.395(11) . ? C25 C26 1.329(12) . ? C26 C27 1.358(13) . ? C27 C28 1.407(12) . ? C29 C34 1.352(11) . ? C29 C30 1.370(11) . ? C30 C31 1.405(16) . ? C31 C32 1.33(2) . ? C32 C33 1.354(19) . ? C33 C34 1.393(15) . ? C35 C40 1.370(10) . ? C35 C36 1.382(10) . ? C36 C37 1.396(10) . ? C37 C38 1.335(12) . ? C38 C39 1.391(13) . ? C39 C40 1.370(12) . ? C41 C46 1.331(12) . ? C41 C42 1.370(12) . ? C42 C43 1.367(12) . ? C43 C44 1.349(16) . ? C44 C45 1.360(16) . ? C45 C46 1.403(15) . ? C47A C48A 1.3900 . ? C47A C52A 1.3900 . ? C48A C49A 1.3900 . ? C49A C50A 1.3900 . ? C50A C51A 1.3900 . ? C51A C52A 1.3900 . ? C47B C48B 1.3900 . ? C47B C52B 1.3900 . ? C48B C49B 1.3900 . ? C49B C50B 1.3900 . ? C50B C51B 1.3900 . ? C51B C52B 1.3900 . ? C60 C59 1.347(14) . ? C60 C61 1.410(15) . ? C53B C54B 1.3900 . ? C53B C58B 1.3900 . ? C54B C55B 1.3900 . ? C55B C56B 1.3900 . ? C56B C57B 1.3900 . ? C57B C58B 1.3900 . ? C59 C64 1.360(13) . ? C53A C54A 1.3900 . ? C53A C58A 1.3900 . ? C54A C55A 1.3900 . ? C55A C56A 1.3900 . ? C56A C57A 1.3900 . ? C57A C58A 1.3900 . ? C61 C62 1.36(2) . ? C62 C63 1.33(3) . ? C63 C64 1.404(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 P2 Pt1 P1 97.34(7) . . ? P2 Pt1 S2 88.19(7) . . ? P1 Pt1 S2 172.79(7) . . ? P2 Pt1 S1 172.86(7) . . ? P1 Pt1 S1 86.19(7) . . ? S2 Pt1 S1 88.83(7) . . ? P4 Pt2 S4 86.98(8) . . ? P4 Pt2 P3 95.75(7) . . ? S4 Pt2 P3 174.48(8) . . ? P4 Pt2 S3 175.12(7) . . ? S4 Pt2 S3 88.16(8) . . ? P3 Pt2 S3 89.13(7) . . ? C5 S1 Pt1 104.6(3) . . ? C10 S2 Pt1 103.9(2) . . ? C11 S3 Pt2 104.1(3) . . ? C16 S4 Pt2 105.5(3) . . ? C1 P1 C17 101.1(4) . . ? C1 P1 C23 100.5(3) . . ? C17 P1 C23 105.3(4) . . ? C1 P1 Pt1 118.5(2) . . ? C17 P1 Pt1 114.1(3) . . ? C23 P1 Pt1 115.2(2) . . ? C3 P2 C35 102.4(3) . . ? C3 P2 C29 100.2(3) . . ? C35 P2 C29 104.8(4) . . ? C3 P2 Pt1 115.2(2) . . ? C35 P2 Pt1 113.3(2) . . ? C29 P2 Pt1 118.8(2) . . ? C53B P3 C47A 111.2(6) . . ? C53B P3 C2 101.0(5) . . ? C47A P3 C2 96.5(4) . . ? C53B P3 C47B 106.3(6) . . ? C47A P3 C47B 7.0(7) . . ? C2 P3 C47B 102.6(5) . . ? C53B P3 C53A 9.6(6) . . ? C47A P3 C53A 102.5(5) . . ? C2 P3 C53A 98.5(5) . . ? C47B P3 C53A 98.1(6) . . ? C53B P3 Pt2 108.6(4) . . ? C47A P3 Pt2 119.4(3) . . ? C2 P3 Pt2 118.5(2) . . ? C47B P3 Pt2 118.0(5) . . ? C53A P3 Pt2 117.5(4) . . ? C4 P4 C41 104.0(4) . . ? C4 P4 C59 100.9(4) . . ? C41 P4 C59 105.3(4) . . ? C4 P4 Pt2 113.7(3) . . ? C41 P4 Pt2 114.5(3) . . ? C59 P4 Pt2 116.8(3) . . ? C2 C1 P1 177.7(8) . . ? C1 C2 P3 175.3(7) . . ? C4 C3 P2 174.1(7) . . ? C3 C4 P4 174.7(7) . . ? C6 C5 C10 118.2(7) . . ? C6 C5 S1 121.5(6) . . ? C10 C5 S1 120.2(5) . . ? C7 C6 C5 122.1(8) . . ? C7 C6 Cl1 119.1(6) . . ? C5 C6 Cl1 118.8(6) . . ? C8 C7 C6 120.4(8) . . ? C7 C8 C9 119.0(9) . . ? C8 C9 C10 122.0(8) . . ? C8 C9 Cl2 118.1(7) . . ? C10 C9 Cl2 119.9(6) . . ? C9 C10 C5 118.3(7) . . ? C9 C10 S2 119.6(6) . . ? C5 C10 S2 122.1(5) . . ? C16 C11 C12 117.8(8) . . ? C16 C11 S3 121.3(6) . . ? C12 C11 S3 120.9(7) . . ? C13 C12 C11 122.5(9) . . ? C13 C12 Cl3 118.1(7) . . ? C11 C12 Cl3 119.4(7) . . ? C14 C13 C12 118.7(9) . . ? C15 C14 C13 120.8(9) . . ? C14 C15 C16 121.8(10) . . ? C14 C15 Cl4 119.6(8) . . ? C16 C15 Cl4 118.7(8) . . ? C11 C16 C15 118.5(8) . . ? C11 C16 S4 120.8(6) . . ? C15 C16 S4 120.7(7) . . ? C22 C17 C18 118.4(8) . . ? C22 C17 P1 120.5(7) . . ? C18 C17 P1 121.1(7) . . ? C17 C18 C19 121.1(9) . . ? C20 C19 C18 119.9(10) . . ? C19 C20 C21 119.7(10) . . ? C20 C21 C22 120.9(11) . . ? C17 C22 C21 119.9(10) . . ? C24 C23 C28 118.3(7) . . ? C24 C23 P1 122.5(6) . . ? C28 C23 P1 119.2(6) . . ? C23 C24 C25 121.0(8) . . ? C26 C25 C24 121.1(9) . . ? C25 C26 C27 119.1(9) . . ? C26 C27 C28 120.9(9) . . ? C23 C28 C27 119.5(9) . . ? C34 C29 C30 120.9(9) . . ? C34 C29 P2 121.8(7) . . ? C30 C29 P2 117.3(7) . . ? C29 C30 C31 117.6(12) . . ? C32 C31 C30 121.2(15) . . ? C31 C32 C33 120.8(15) . . ? C32 C33 C34 119.1(13) . . ? C29 C34 C33 120.2(11) . . ? C40 C35 C36 119.1(7) . . ? C40 C35 P2 120.9(6) . . ? C36 C35 P2 120.0(6) . . ? C35 C36 C37 120.6(7) . . ? C38 C37 C36 119.1(8) . . ? C37 C38 C39 121.3(9) . . ? C40 C39 C38 119.4(9) . . ? C35 C40 C39 120.5(8) . . ? C46 C41 C42 118.7(9) . . ? C46 C41 P4 119.0(7) . . ? C42 C41 P4 122.3(7) . . ? C43 C42 C41 121.2(10) . . ? C44 C43 C42 121.3(11) . . ? C43 C44 C45 117.3(11) . . ? C44 C45 C46 121.8(11) . . ? C48A C47A C52A 120.0 . . ? C48A C47A P3 123.6(6) . . ? C52A C47A P3 116.4(6) . . ? C49A C48A C47A 120.0 . . ? C50A C49A C48A 120.0 . . ? C49A C50A C51A 120.0 . . ? C52A C51A C50A 120.0 . . ? C51A C52A C47A 120.0 . . ? C41 C46 C45 119.7(10) . . ? C48B C47B C52B 120.0 . . ? C48B C47B P3 122.4(9) . . ? C52B C47B P3 117.4(9) . . ? C49B C48B C47B 120.0 . . ? C50B C49B C48B 120.0 . . ? C49B C50B C51B 120.0 . . ? C52B C51B C50B 120.0 . . ? C51B C52B C47B 120.0 . . ? C59 C60 C61 120.7(14) . . ? C54B C53B C58B 120.0 . . ? C54B C53B P3 118.4(7) . . ? C58B C53B P3 121.5(7) . . ? C55B C54B C53B 120.0 . . ? C54B C55B C56B 120.0 . . ? C55B C56B C57B 120.0 . . ? C58B C57B C56B 120.0 . . ? C57B C58B C53B 120.0 . . ? C60 C59 C64 120.4(10) . . ? C60 C59 P4 119.8(8) . . ? C64 C59 P4 119.7(9) . . ? C54A C53A C58A 120.0 . . ? C54A C53A P3 120.0(7) . . ? C58A C53A P3 120.0(7) . . ? C55A C54A C53A 120.0 . . ? C56A C55A C54A 120.0 . . ? C55A C56A C57A 120.0 . . ? C56A C57A C58A 120.0 . . ? C57A C58A C53A 120.0 . . ? C62 C61 C60 117.8(18) . . ? C63 C62 C61 121.8(18) . . ? C62 C63 C64 120(2) . . ? C59 C64 C63 119.0(15) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.192 _refine_diff_density_min -1.591 _refine_diff_density_rms 0.143 # Attachment 'pt_tdtEND.cif' data_pt_tdt_[Pt(tdt)]2(u-dppa)2 _database_code_depnum_ccdc_archive 'CCDC 699938' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H57 Cl3 O2 P4 Pt2 S4' _chemical_formula_weight 1642.78 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' Pt Pt -1.7033 8.3905 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8814(8) _cell_length_b 14.7267(12) _cell_length_c 21.2919(16) _cell_angle_alpha 97.397(2) _cell_angle_beta 96.961(2) _cell_angle_gamma 92.179(3) _cell_volume 3353.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8140 _cell_measurement_theta_min 2.287 _cell_measurement_theta_max 27.004 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 4.549 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6591 _exptl_absorpt_correction_T_max 0.7413 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55310 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 28.35 _reflns_number_total 16442 _reflns_number_gt 11781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEXll' _computing_cell_refinement 'Bruker SMART APEXll' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^)+(0.0672P)^2^+4.5780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16442 _refine_ls_number_parameters 763 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Pt1 Pt 0.30866(2) 0.287636(16) 0.389030(11) 0.04042(8) Uani 1 1 d . . . Pt2 Pt 0.580230(19) 0.251713(14) 0.092920(10) 0.03409(7) Uani 1 1 d . . . P1 P 0.27396(14) 0.38212(11) 0.31387(8) 0.0409(3) Uani 1 1 d . . . P2 P 0.50026(14) 0.25007(10) 0.36462(7) 0.0370(3) Uani 1 1 d . . . P3 P 0.45584(14) 0.36359(10) 0.12427(8) 0.0366(3) Uani 1 1 d . . . P4 P 0.49298(14) 0.14519(10) 0.14518(7) 0.0352(3) Uani 1 1 d . . . S1 S 0.11708(17) 0.32457(15) 0.41757(10) 0.0628(5) Uani 1 1 d . . . S2 S 0.3395(2) 0.21326(14) 0.47751(10) 0.0631(5) Uani 1 1 d . . . S3 S 0.66383(15) 0.35522(11) 0.03497(9) 0.0487(4) Uani 1 1 d . . . S4 S 0.70353(15) 0.14318(11) 0.04929(8) 0.0452(4) Uani 1 1 d . . . C1 C 0.3513(5) 0.3644(4) 0.2458(3) 0.0392(13) Uani 1 1 d . . . C2 C 0.3905(6) 0.3572(4) 0.1959(3) 0.0405(13) Uani 1 1 d . . . C3 C 0.5042(6) 0.2024(4) 0.2842(3) 0.0398(13) Uani 1 1 d . . . C4 C 0.5034(6) 0.1748(4) 0.2285(3) 0.0400(13) Uani 1 1 d . . . C5 C 0.1165(8) 0.2886(6) 0.4921(4) 0.068(2) Uani 1 1 d . . . C6 C 0.0148(8) 0.3074(6) 0.5269(5) 0.081(3) Uani 1 1 d . A . H6 H -0.0506 0.3386 0.5090 0.097 Uiso 1 1 calc R . . C7 C 0.0103(13) 0.2814(9) 0.5853(6) 0.109(4) Uani 1 1 d . . . C8A C -0.069(3) 0.294(2) 0.6298(19) 0.144(17) Uani 0.393(18) 1 d P A 1 H8A1 H -0.1112 0.3494 0.6254 0.217 Uiso 0.393(18) 1 calc PR A 1 H8A2 H -0.0234 0.2987 0.6717 0.217 Uiso 0.393(18) 1 calc PR A 1 H8A3 H -0.1287 0.2429 0.6238 0.217 Uiso 0.393(18) 1 calc PR A 1 C8B C 0.0967(16) 0.2070(12) 0.6765(7) 0.086(6) Uani 0.607(18) 1 d P A 2 H8B1 H 0.1766 0.1937 0.6966 0.130 Uiso 0.607(18) 1 calc PR A 2 H8B2 H 0.0412 0.1538 0.6722 0.130 Uiso 0.607(18) 1 calc PR A 2 H8B3 H 0.0645 0.2569 0.7021 0.130 Uiso 0.607(18) 1 calc PR A 2 C9 C 0.1089(15) 0.2328(8) 0.6129(5) 0.109(4) Uani 1 1 d . A . C10 C 0.2110(11) 0.2124(7) 0.5797(4) 0.089(3) Uani 1 1 d . . . H9 H 0.2759 0.1809 0.5977 0.107 Uiso 1 1 calc R A . C11 C 0.2138(8) 0.2401(5) 0.5187(4) 0.065(2) Uani 1 1 d . A . C12 C 0.1188(6) 0.3825(5) 0.2702(3) 0.0502(16) Uani 1 1 d . . . C13 C 0.0533(7) 0.2998(6) 0.2507(4) 0.071(2) Uani 1 1 d . . . H13 H 0.0809 0.2471 0.2664 0.085 Uiso 1 1 calc R . . C14 C -0.0537(8) 0.2952(9) 0.2077(5) 0.097(3) Uani 1 1 d . . . H14 H -0.0966 0.2390 0.1936 0.116 Uiso 1 1 calc R . . C15 C -0.0963(8) 0.3726(10) 0.1861(5) 0.100(4) Uani 1 1 d . . . H15 H -0.1682 0.3691 0.1572 0.120 Uiso 1 1 calc R . . C16 C -0.0342(9) 0.4548(9) 0.2064(5) 0.097(4) Uani 1 1 d . . . H16 H -0.0643 0.5073 0.1914 0.116 Uiso 1 1 calc R . . C17 C 0.0755(7) 0.4619(6) 0.2500(4) 0.071(2) Uani 1 1 d . . . H17 H 0.1171 0.5184 0.2646 0.086 Uiso 1 1 calc R . . C18 C 0.3235(7) 0.5002(5) 0.3442(3) 0.0518(16) Uani 1 1 d . . . C19 C 0.2877(11) 0.5400(6) 0.4003(4) 0.090(3) Uani 1 1 d . . . H19 H 0.2352 0.5068 0.4214 0.108 Uiso 1 1 calc R . . C20 C 0.3276(14) 0.6275(7) 0.4260(5) 0.108(4) Uani 1 1 d . . . H20 H 0.3010 0.6530 0.4640 0.130 Uiso 1 1 calc R . . C21 C 0.4025(13) 0.6759(7) 0.3981(6) 0.113(4) Uani 1 1 d . . . H21 H 0.4290 0.7355 0.4159 0.136 Uiso 1 1 calc R . . C22 C 0.4406(16) 0.6388(8) 0.3437(8) 0.171(8) Uani 1 1 d . . . H22 H 0.4947 0.6729 0.3241 0.206 Uiso 1 1 calc R . . C23 C 0.4010(12) 0.5499(7) 0.3154(6) 0.120(5) Uani 1 1 d . . . H23 H 0.4278 0.5253 0.2773 0.144 Uiso 1 1 calc R . . C24 C 0.5770(6) 0.1643(4) 0.4076(3) 0.0461(15) Uani 1 1 d . . . C25 C 0.6844(7) 0.1828(5) 0.4474(3) 0.0533(17) Uani 1 1 d . . . H25 H 0.7227 0.2412 0.4522 0.064 Uiso 1 1 calc R . . C26 C 0.7385(9) 0.1172(7) 0.4809(4) 0.076(2) Uani 1 1 d . . . H26 H 0.8121 0.1315 0.5082 0.091 Uiso 1 1 calc R . . C27 C 0.6832(9) 0.0312(7) 0.4737(5) 0.085(3) Uani 1 1 d . . . H27 H 0.7193 -0.0138 0.4955 0.102 Uiso 1 1 calc R . . C28 C 0.5752(9) 0.0118(6) 0.4344(5) 0.092(3) Uani 1 1 d . . . H28 H 0.5368 -0.0466 0.4300 0.110 Uiso 1 1 calc R . . C29 C 0.5210(8) 0.0770(5) 0.4007(5) 0.075(2) Uani 1 1 d . . . H29 H 0.4474 0.0624 0.3736 0.090 Uiso 1 1 calc R . . C30 C 0.6116(5) 0.3479(4) 0.3748(3) 0.0405(13) Uani 1 1 d . . . C31 C 0.5958(7) 0.4237(5) 0.4169(4) 0.0567(18) Uani 1 1 d . . . H31 H 0.5268 0.4253 0.4388 0.068 Uiso 1 1 calc R . . C32 C 0.6794(8) 0.4965(6) 0.4274(5) 0.078(3) Uani 1 1 d . . . H32 H 0.6664 0.5478 0.4556 0.094 Uiso 1 1 calc R . . C33 C 0.7836(8) 0.4948(7) 0.3962(5) 0.082(3) Uani 1 1 d . . . H33 H 0.8416 0.5443 0.4043 0.098 Uiso 1 1 calc R . . C34 C 0.8016(8) 0.4201(7) 0.3532(5) 0.076(2) Uani 1 1 d . . . H34 H 0.8705 0.4192 0.3312 0.091 Uiso 1 1 calc R . . C35 C 0.7153(7) 0.3454(5) 0.3428(4) 0.0598(18) Uani 1 1 d . . . H35 H 0.7273 0.2940 0.3144 0.072 Uiso 1 1 calc R . . C36 C 0.3189(6) 0.3762(4) 0.0693(3) 0.0428(14) Uani 1 1 d . . . C37 C 0.3345(7) 0.3853(5) 0.0060(4) 0.0599(19) Uani 1 1 d . . . H37 H 0.4128 0.3825 -0.0072 0.072 Uiso 1 1 calc R . . C38 C 0.2323(8) 0.3986(6) -0.0368(4) 0.074(2) Uani 1 1 d . . . H38 H 0.2425 0.4055 -0.0787 0.088 Uiso 1 1 calc R . . C39 C 0.1168(8) 0.4015(7) -0.0179(5) 0.082(3) Uani 1 1 d . . . H39 H 0.0492 0.4123 -0.0466 0.098 Uiso 1 1 calc R . . C40 C 0.1003(8) 0.3888(8) 0.0425(5) 0.092(3) Uani 1 1 d . . . H40 H 0.0208 0.3874 0.0543 0.110 Uiso 1 1 calc R . . C41 C 0.2009(7) 0.3777(7) 0.0867(4) 0.072(2) Uani 1 1 d . . . H41 H 0.1888 0.3711 0.1284 0.087 Uiso 1 1 calc R . . C42 C 0.5284(5) 0.4796(4) 0.1474(3) 0.0404(13) Uani 1 1 d . . . C43 C 0.4831(7) 0.5540(5) 0.1220(4) 0.0589(18) Uani 1 1 d . . . H43 H 0.4190 0.5461 0.0883 0.071 Uiso 1 1 calc R . . C44 C 0.5324(9) 0.6405(5) 0.1461(5) 0.075(2) Uani 1 1 d . . . H44 H 0.5012 0.6908 0.1285 0.090 Uiso 1 1 calc R . . C45 C 0.6273(9) 0.6540(5) 0.1961(5) 0.074(2) Uani 1 1 d . . . H45 H 0.6597 0.7127 0.2127 0.089 Uiso 1 1 calc R . . C46 C 0.6726(8) 0.5784(6) 0.2208(4) 0.071(2) Uani 1 1 d . . . H46 H 0.7368 0.5863 0.2544 0.086 Uiso 1 1 calc R . . C47 C 0.6247(6) 0.4908(5) 0.1966(4) 0.0571(18) Uani 1 1 d . . . H47 H 0.6570 0.4402 0.2133 0.068 Uiso 1 1 calc R . . C48 C 0.5590(6) 0.0336(4) 0.1382(3) 0.0405(13) Uani 1 1 d . . . C49 C 0.6713(7) 0.0229(5) 0.1737(4) 0.063(2) Uani 1 1 d . . . H49 H 0.7086 0.0712 0.2031 0.076 Uiso 1 1 calc R . . C50 C 0.7285(9) -0.0597(6) 0.1658(5) 0.079(3) Uani 1 1 d . . . H50 H 0.8044 -0.0665 0.1895 0.095 Uiso 1 1 calc R . . C51 C 0.6728(8) -0.1311(5) 0.1229(4) 0.069(2) Uani 1 1 d . . . H51 H 0.7104 -0.1868 0.1178 0.083 Uiso 1 1 calc R . . C52 C 0.5636(8) -0.1204(5) 0.0883(4) 0.0605(19) Uani 1 1 d . . . H52 H 0.5265 -0.1690 0.0592 0.073 Uiso 1 1 calc R . . C53 C 0.5052(7) -0.0383(4) 0.0953(3) 0.0489(15) Uani 1 1 d . . . H53 H 0.4299 -0.0321 0.0709 0.059 Uiso 1 1 calc R . . C54 C 0.3264(5) 0.1258(4) 0.1214(3) 0.0396(13) Uani 1 1 d . . . C55 C 0.2789(7) 0.1328(6) 0.0593(4) 0.070(2) Uani 1 1 d . . . H55 H 0.3330 0.1437 0.0302 0.084 Uiso 1 1 calc R . . C56 C 0.1543(8) 0.1241(7) 0.0394(5) 0.086(3) Uani 1 1 d . . . H56 H 0.1245 0.1302 -0.0026 0.103 Uiso 1 1 calc R . . C57 C 0.0748(8) 0.1067(6) 0.0806(5) 0.078(3) Uani 1 1 d . . . H57 H -0.0100 0.1001 0.0671 0.093 Uiso 1 1 calc R . . C58 C 0.1189(7) 0.0988(6) 0.1422(5) 0.077(3) Uani 1 1 d . . . H58 H 0.0642 0.0858 0.1706 0.093 Uiso 1 1 calc R . . C59 C 0.2440(7) 0.1098(6) 0.1625(4) 0.0617(19) Uani 1 1 d . . . H59 H 0.2728 0.1064 0.2051 0.074 Uiso 1 1 calc R . . C60 C 0.7487(6) 0.2874(5) -0.0171(3) 0.0518(16) Uani 1 1 d . . . C61 C 0.7985(7) 0.3264(6) -0.0657(4) 0.066(2) Uani 1 1 d . B . H61 H 0.7865 0.3877 -0.0696 0.080 Uiso 1 1 calc R . . C62 C 0.8646(9) 0.2766(8) -0.1076(5) 0.087(3) Uani 1 1 d . . . C63A C 0.903(2) 0.3057(13) -0.1632(9) 0.103(7) Uani 0.560(17) 1 d P B 1 H63A H 0.8607 0.2683 -0.2003 0.154 Uiso 0.560(17) 1 calc PR B 1 H63B H 0.9911 0.2999 -0.1623 0.154 Uiso 0.560(17) 1 calc PR B 1 H63C H 0.8845 0.3686 -0.1647 0.154 Uiso 0.560(17) 1 calc PR B 1 C63B C 0.958(2) 0.1398(19) -0.1448(13) 0.112(10) Uani 0.440(17) 1 d P B 2 H63D H 0.9615 0.0760 -0.1399 0.167 Uiso 0.440(17) 1 calc PR B 2 H63E H 1.0408 0.1681 -0.1364 0.167 Uiso 0.440(17) 1 calc PR B 2 H63F H 0.9236 0.1458 -0.1876 0.167 Uiso 0.440(17) 1 calc PR B 2 C64 C 0.8825(9) 0.1842(8) -0.1004(4) 0.085(3) Uani 1 1 d . B . C65 C 0.8352(7) 0.1441(6) -0.0525(4) 0.069(2) Uani 1 1 d . . . H65 H 0.8488 0.0831 -0.0481 0.083 Uiso 1 1 calc R B . C66 C 0.7662(6) 0.1961(5) -0.0103(3) 0.0491(16) Uani 1 1 d . B . C67 C 0.0318(11) 0.0798(8) 0.3639(5) 0.102(3) Uani 1 1 d . . . H67 H 0.0662 0.1408 0.3835 0.122 Uiso 1 1 calc R . . Cl1 Cl 0.0231(3) 0.0141(3) 0.42251(17) 0.1296(12) Uani 1 1 d . . . Cl2 Cl 0.1293(5) 0.0356(4) 0.3101(2) 0.193(2) Uani 1 1 d . . . Cl3 Cl -0.1106(5) 0.0921(4) 0.3234(2) 0.185(2) Uani 1 1 d . . . O1 O 0.5343(13) 0.8676(7) 0.2852(5) 0.185(5) Uani 1 1 d . . . O2 O 0.3156(12) 0.8662(8) 0.3401(7) 0.193(5) 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 Pt1 0.04190(13) 0.04510(14) 0.03380(14) 0.00328(10) 0.00707(10) -0.00370(10) Pt2 0.03688(12) 0.03380(12) 0.03083(13) 0.00221(9) 0.00380(9) 0.00113(8) P1 0.0412(8) 0.0470(9) 0.0337(9) 0.0014(7) 0.0054(7) 0.0046(7) P2 0.0429(8) 0.0375(8) 0.0294(8) 0.0018(6) 0.0037(6) -0.0005(6) P3 0.0400(7) 0.0357(7) 0.0351(8) 0.0072(6) 0.0060(6) 0.0041(6) P4 0.0423(8) 0.0326(7) 0.0292(8) 0.0011(6) 0.0029(6) 0.0004(6) S1 0.0489(9) 0.0830(13) 0.0577(12) 0.0033(10) 0.0192(9) 0.0000(9) S2 0.0759(12) 0.0707(12) 0.0476(11) 0.0219(9) 0.0142(9) -0.0006(10) S3 0.0515(9) 0.0467(9) 0.0521(10) 0.0149(7) 0.0146(8) 0.0011(7) S4 0.0482(8) 0.0427(8) 0.0454(10) 0.0012(7) 0.0124(7) 0.0063(6) C1 0.041(3) 0.037(3) 0.041(4) 0.003(3) 0.008(3) 0.005(2) C2 0.044(3) 0.034(3) 0.042(4) 0.004(3) 0.002(3) 0.004(2) C3 0.046(3) 0.040(3) 0.032(3) 0.002(2) 0.000(3) 0.004(2) C4 0.050(3) 0.032(3) 0.038(4) 0.006(2) 0.002(3) 0.004(2) C5 0.080(5) 0.065(5) 0.055(5) -0.015(4) 0.031(4) -0.033(4) C6 0.072(5) 0.089(6) 0.078(6) -0.020(5) 0.038(5) -0.034(5) C7 0.137(11) 0.098(8) 0.090(9) -0.024(7) 0.069(8) -0.056(7) C8A 0.12(3) 0.13(3) 0.19(4) -0.02(2) 0.11(3) -0.04(2) C8B 0.106(12) 0.103(12) 0.051(9) 0.009(8) 0.025(8) -0.031(9) C9 0.161(12) 0.096(8) 0.071(7) -0.011(6) 0.062(8) -0.064(8) C10 0.125(8) 0.085(6) 0.056(6) 0.008(5) 0.025(6) -0.035(6) C11 0.087(6) 0.060(5) 0.046(5) 0.002(4) 0.020(4) -0.026(4) C12 0.043(3) 0.072(5) 0.035(4) 0.001(3) 0.008(3) 0.013(3) C13 0.052(4) 0.088(6) 0.061(5) -0.018(4) -0.007(4) 0.001(4) C14 0.059(5) 0.124(9) 0.090(8) -0.034(6) -0.013(5) 0.006(5) C15 0.044(5) 0.178(12) 0.068(7) -0.012(7) -0.008(4) 0.010(6) C16 0.061(5) 0.146(10) 0.091(8) 0.045(7) 0.002(5) 0.040(6) C17 0.057(4) 0.092(6) 0.070(6) 0.028(5) 0.005(4) 0.014(4) C18 0.060(4) 0.048(4) 0.044(4) -0.004(3) 0.003(3) 0.004(3) C19 0.151(9) 0.064(5) 0.060(6) -0.004(4) 0.042(6) 0.006(6) C20 0.190(13) 0.062(6) 0.066(7) -0.020(5) 0.017(7) 0.010(7) C21 0.161(12) 0.062(6) 0.100(9) -0.037(6) 0.014(8) -0.019(7) C22 0.224(17) 0.084(8) 0.204(16) -0.062(10) 0.125(14) -0.067(9) C23 0.171(11) 0.068(6) 0.119(9) -0.042(6) 0.086(9) -0.053(7) C24 0.051(4) 0.050(4) 0.038(4) 0.011(3) 0.004(3) 0.005(3) C25 0.063(4) 0.052(4) 0.043(4) 0.006(3) -0.003(3) 0.007(3) C26 0.080(6) 0.088(6) 0.057(5) 0.016(4) -0.015(4) 0.019(5) C27 0.092(7) 0.078(6) 0.092(7) 0.041(5) -0.001(6) 0.019(5) C28 0.093(7) 0.060(5) 0.127(9) 0.045(6) 0.000(6) -0.001(5) C29 0.077(5) 0.056(5) 0.091(7) 0.026(4) -0.004(5) -0.003(4) C30 0.044(3) 0.037(3) 0.038(3) 0.001(3) 0.002(3) -0.003(2) C31 0.055(4) 0.054(4) 0.056(5) -0.007(3) 0.007(3) -0.006(3) C32 0.084(6) 0.055(5) 0.085(7) -0.020(4) 0.006(5) -0.020(4) C33 0.073(6) 0.083(6) 0.080(7) -0.002(5) -0.003(5) -0.038(5) C34 0.057(5) 0.089(6) 0.081(7) 0.010(5) 0.013(4) -0.021(4) C35 0.057(4) 0.060(4) 0.061(5) 0.003(4) 0.012(4) -0.011(3) C36 0.048(3) 0.037(3) 0.043(4) 0.004(3) 0.002(3) 0.005(3) C37 0.052(4) 0.075(5) 0.054(5) 0.015(4) 0.004(3) 0.004(3) C38 0.081(6) 0.085(6) 0.052(5) 0.017(4) -0.015(4) 0.003(5) C39 0.052(5) 0.119(8) 0.072(6) 0.020(5) -0.012(4) 0.017(5) C40 0.043(4) 0.162(10) 0.074(7) 0.036(6) 0.003(4) 0.022(5) C41 0.051(4) 0.115(7) 0.056(5) 0.026(5) 0.012(4) 0.017(4) C42 0.044(3) 0.037(3) 0.041(4) 0.004(3) 0.010(3) 0.006(2) C43 0.074(5) 0.042(4) 0.059(5) 0.010(3) -0.006(4) 0.000(3) C44 0.096(6) 0.046(4) 0.084(6) 0.018(4) 0.003(5) -0.003(4) C45 0.091(6) 0.042(4) 0.085(7) -0.002(4) 0.014(5) -0.016(4) C46 0.070(5) 0.064(5) 0.072(6) 0.002(4) -0.012(4) -0.014(4) C47 0.054(4) 0.050(4) 0.063(5) 0.010(3) -0.005(3) -0.002(3) C48 0.050(3) 0.035(3) 0.035(3) 0.001(2) 0.001(3) 0.001(2) C49 0.066(5) 0.052(4) 0.066(5) 0.000(4) -0.009(4) 0.009(3) C50 0.084(6) 0.062(5) 0.087(7) 0.006(5) -0.012(5) 0.029(4) C51 0.094(6) 0.041(4) 0.074(6) 0.004(4) 0.016(5) 0.021(4) C52 0.085(5) 0.036(3) 0.057(5) -0.005(3) 0.008(4) 0.003(3) C53 0.062(4) 0.041(3) 0.040(4) -0.005(3) 0.003(3) 0.000(3) C54 0.043(3) 0.039(3) 0.035(3) 0.006(2) 0.001(3) 0.000(2) C55 0.058(4) 0.092(6) 0.059(5) 0.025(4) -0.005(4) -0.018(4) C56 0.068(5) 0.109(8) 0.076(7) 0.028(6) -0.026(5) -0.014(5) C57 0.047(4) 0.076(6) 0.102(8) -0.001(5) -0.009(5) -0.002(4) C58 0.047(4) 0.097(7) 0.082(7) -0.018(5) 0.020(4) -0.011(4) C59 0.050(4) 0.083(5) 0.048(4) -0.009(4) 0.011(3) -0.006(4) C60 0.042(3) 0.066(4) 0.047(4) 0.011(3) 0.002(3) -0.005(3) C61 0.062(5) 0.083(6) 0.060(5) 0.023(4) 0.014(4) 0.000(4) C62 0.079(6) 0.122(9) 0.072(7) 0.031(6) 0.039(5) 0.004(6) C63A 0.135(18) 0.090(13) 0.082(14) 0.005(10) 0.028(12) -0.022(12) C63B 0.11(2) 0.13(2) 0.10(2) 0.001(16) 0.057(16) 0.022(16) C64 0.080(6) 0.122(8) 0.060(6) 0.013(5) 0.037(5) 0.018(6) C65 0.068(5) 0.086(6) 0.056(5) 0.005(4) 0.026(4) 0.013(4) C66 0.041(3) 0.063(4) 0.042(4) 0.001(3) 0.009(3) 0.000(3) C67 0.127(9) 0.096(8) 0.076(7) 0.009(6) 0.001(6) -0.019(7) Cl1 0.127(3) 0.164(3) 0.111(3) 0.063(2) 0.017(2) 0.015(2) Cl2 0.237(5) 0.202(5) 0.152(4) -0.002(3) 0.111(4) -0.017(4) Cl3 0.188(4) 0.215(5) 0.141(4) 0.048(3) -0.055(3) 0.028(4) O1 0.270(14) 0.136(8) 0.156(10) -0.022(7) 0.094(10) 0.018(8) O2 0.209(12) 0.176(10) 0.229(13) 0.105(10) 0.072(10) 0.066(9) _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 Pt1 P1 2.2598(17) . ? Pt1 P2 2.2801(15) . ? Pt1 S2 2.2950(19) . ? Pt1 S1 2.3063(18) . ? Pt2 P3 2.2577(15) . ? Pt2 P4 2.2788(15) . ? Pt2 S4 2.3023(15) . ? Pt2 S3 2.3074(16) . ? P1 C1 1.757(6) . ? P1 C18 1.813(7) . ? P1 C12 1.827(7) . ? P2 C3 1.772(6) . ? P2 C30 1.821(6) . ? P2 C24 1.822(6) . ? P3 C2 1.771(7) . ? P3 C36 1.811(6) . ? P3 C42 1.836(6) . ? P4 C4 1.760(7) . ? P4 C48 1.814(6) . ? P4 C54 1.824(6) . ? S1 C5 1.736(9) . ? S2 C11 1.744(9) . ? S3 C60 1.764(7) . ? S4 C66 1.762(7) . ? C1 C2 1.187(8) . ? C3 C4 1.201(8) . ? C5 C11 1.403(12) . ? C5 C6 1.422(11) . ? C6 C7 1.355(15) . ? C7 C8A 1.36(3) . ? C7 C9 1.422(19) . ? C8B C9 1.471(17) . ? C9 C10 1.409(16) . ? C10 C11 1.413(12) . ? C12 C17 1.376(10) . ? C12 C13 1.377(11) . ? C13 C14 1.385(12) . ? C14 C15 1.360(16) . ? C15 C16 1.358(16) . ? C16 C17 1.412(12) . ? C18 C23 1.348(12) . ? C18 C19 1.369(10) . ? C19 C20 1.366(13) . ? C20 C21 1.308(16) . ? C21 C22 1.336(16) . ? C22 C23 1.397(14) . ? C24 C25 1.354(9) . ? C24 C29 1.384(10) . ? C25 C26 1.382(10) . ? C26 C27 1.362(13) . ? C27 C28 1.356(13) . ? C28 C29 1.378(11) . ? C30 C31 1.369(9) . ? C30 C35 1.386(9) . ? C31 C32 1.357(10) . ? C32 C33 1.382(12) . ? C33 C34 1.374(13) . ? C34 C35 1.396(11) . ? C36 C41 1.380(9) . ? C36 C37 1.400(10) . ? C37 C38 1.386(10) . ? C38 C39 1.366(12) . ? C39 C40 1.355(13) . ? C40 C41 1.383(11) . ? C42 C43 1.366(8) . ? C42 C47 1.377(9) . ? C43 C44 1.373(11) . ? C44 C45 1.379(12) . ? C45 C46 1.373(11) . ? C46 C47 1.384(10) . ? C48 C53 1.368(8) . ? C48 C49 1.383(9) . ? C49 C50 1.387(10) . ? C50 C51 1.370(12) . ? C51 C52 1.347(11) . ? C52 C53 1.386(9) . ? C54 C59 1.362(9) . ? C54 C55 1.378(10) . ? C55 C56 1.367(11) . ? C56 C57 1.345(13) . ? C57 C58 1.362(13) . ? C58 C59 1.374(10) . ? C60 C66 1.388(10) . ? C60 C61 1.399(10) . ? C61 C62 1.371(13) . ? C62 C64 1.408(14) . ? C62 C63A 1.413(19) . ? C63B C64 1.44(2) . ? C64 C65 1.383(12) . ? C65 C66 1.410(10) . ? C67 Cl1 1.684(11) . ? C67 Cl3 1.708(12) . ? C67 Cl2 1.737(12) . ? 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 Pt1 P2 95.39(5) . . ? P1 Pt1 S2 170.22(7) . . ? P2 Pt1 S2 89.72(7) . . ? P1 Pt1 S1 86.52(7) . . ? P2 Pt1 S1 177.86(7) . . ? S2 Pt1 S1 88.25(8) . . ? P3 Pt2 P4 94.68(5) . . ? P3 Pt2 S4 173.27(6) . . ? P4 Pt2 S4 90.27(6) . . ? P3 Pt2 S3 86.34(6) . . ? P4 Pt2 S3 176.97(6) . . ? S4 Pt2 S3 88.49(6) . . ? C1 P1 C18 101.1(3) . . ? C1 P1 C12 95.8(3) . . ? C18 P1 C12 107.4(3) . . ? C1 P1 Pt1 118.4(2) . . ? C18 P1 Pt1 112.3(2) . . ? C12 P1 Pt1 119.3(2) . . ? C3 P2 C30 102.8(3) . . ? C3 P2 C24 101.5(3) . . ? C30 P2 C24 105.5(3) . . ? C3 P2 Pt1 114.7(2) . . ? C30 P2 Pt1 113.6(2) . . ? C24 P2 Pt1 117.0(2) . . ? C2 P3 C36 101.2(3) . . ? C2 P3 C42 96.3(3) . . ? C36 P3 C42 105.7(3) . . ? C2 P3 Pt2 117.67(19) . . ? C36 P3 Pt2 116.2(2) . . ? C42 P3 Pt2 116.96(19) . . ? C4 P4 C48 102.1(3) . . ? C4 P4 C54 102.8(3) . . ? C48 P4 C54 107.0(3) . . ? C4 P4 Pt2 114.9(2) . . ? C48 P4 Pt2 115.9(2) . . ? C54 P4 Pt2 112.8(2) . . ? C5 S1 Pt1 104.1(3) . . ? C11 S2 Pt1 104.5(3) . . ? C60 S3 Pt2 104.0(2) . . ? C66 S4 Pt2 103.7(2) . . ? C2 C1 P1 171.4(5) . . ? C1 C2 P3 171.6(6) . . ? C4 C3 P2 175.9(5) . . ? C3 C4 P4 173.6(5) . . ? C11 C5 C6 118.8(8) . . ? C11 C5 S1 121.6(6) . . ? C6 C5 S1 119.6(8) . . ? C7 C6 C5 121.9(11) . . ? C6 C7 C8A 135(2) . . ? C6 C7 C9 119.7(10) . . ? C8A C7 C9 106(2) . . ? C10 C9 C7 120.1(10) . . ? C10 C9 C8B 123.8(15) . . ? C7 C9 C8B 116.1(13) . . ? C9 C10 C11 119.4(11) . . ? C5 C11 C10 120.2(8) . . ? C5 C11 S2 120.7(6) . . ? C10 C11 S2 119.1(8) . . ? C17 C12 C13 120.6(7) . . ? C17 C12 P1 120.5(6) . . ? C13 C12 P1 118.3(6) . . ? C12 C13 C14 120.0(9) . . ? C15 C14 C13 120.2(10) . . ? C16 C15 C14 120.3(9) . . ? C15 C16 C17 121.0(10) . . ? C12 C17 C16 117.9(9) . . ? C23 C18 C19 117.7(8) . . ? C23 C18 P1 122.5(6) . . ? C19 C18 P1 119.8(6) . . ? C20 C19 C18 121.4(10) . . ? C21 C20 C19 121.1(10) . . ? C20 C21 C22 119.1(10) . . ? C21 C22 C23 121.6(12) . . ? C18 C23 C22 119.1(10) . . ? C25 C24 C29 118.5(6) . . ? C25 C24 P2 123.0(5) . . ? C29 C24 P2 118.5(5) . . ? C24 C25 C26 121.8(7) . . ? C27 C26 C25 119.4(8) . . ? C28 C27 C26 119.5(8) . . ? C27 C28 C29 121.3(9) . . ? C28 C29 C24 119.6(8) . . ? C31 C30 C35 119.3(6) . . ? C31 C30 P2 119.5(5) . . ? C35 C30 P2 121.1(5) . . ? C32 C31 C30 121.0(7) . . ? C31 C32 C33 120.3(8) . . ? C34 C33 C32 120.0(8) . . ? C33 C34 C35 119.3(8) . . ? C30 C35 C34 120.0(7) . . ? C41 C36 C37 118.7(6) . . ? C41 C36 P3 123.4(5) . . ? C37 C36 P3 118.0(5) . . ? C38 C37 C36 119.5(7) . . ? C39 C38 C37 120.5(8) . . ? C40 C39 C38 120.2(8) . . ? C39 C40 C41 120.5(8) . . ? C36 C41 C40 120.4(8) . . ? C43 C42 C47 120.2(6) . . ? C43 C42 P3 122.5(5) . . ? C47 C42 P3 117.0(5) . . ? C42 C43 C44 120.0(7) . . ? C43 C44 C45 121.1(8) . . ? C46 C45 C44 118.2(7) . . ? C45 C46 C47 121.3(8) . . ? C42 C47 C46 119.1(7) . . ? C53 C48 C49 119.1(6) . . ? C53 C48 P4 121.7(5) . . ? C49 C48 P4 119.1(5) . . ? C48 C49 C50 120.3(7) . . ? C51 C50 C49 119.8(8) . . ? C52 C51 C50 119.7(7) . . ? C51 C52 C53 121.4(7) . . ? C48 C53 C52 119.7(7) . . ? C59 C54 C55 117.3(6) . . ? C59 C54 P4 123.7(5) . . ? C55 C54 P4 118.9(5) . . ? C56 C55 C54 121.7(8) . . ? C57 C56 C55 119.9(9) . . ? C56 C57 C58 119.8(8) . . ? C57 C58 C59 120.2(8) . . ? C54 C59 C58 121.0(8) . . ? C66 C60 C61 120.0(7) . . ? C66 C60 S3 120.6(5) . . ? C61 C60 S3 119.4(6) . . ? C62 C61 C60 121.8(8) . . ? C61 C62 C64 118.1(8) . . ? C61 C62 C63A 125.7(13) . . ? C64 C62 C63A 115.6(12) . . ? C65 C64 C62 121.4(8) . . ? C65 C64 C63B 125.1(14) . . ? C62 C64 C63B 113.4(14) . . ? C64 C65 C66 119.7(8) . . ? C60 C66 C65 119.1(7) . . ? C60 C66 S4 121.9(5) . . ? C65 C66 S4 119.0(6) . . ? Cl1 C67 Cl3 111.9(7) . . ? Cl1 C67 Cl2 111.6(7) . . ? Cl3 C67 Cl2 109.1(7) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.821 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.166 # Attachment 'pt_bdtEND.cif' data_pt_bdt_[Pt(bdt)]2(u-dppa)2 _database_code_depnum_ccdc_archive 'CCDC 699939' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H55 Cl3 O3 P4 Pt2 S4' _chemical_formula_weight 1632.74 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' Pt Pt -1.7033 8.3905 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6227(12) _cell_length_b 14.2985(12) _cell_length_c 23.709(3) _cell_angle_alpha 74.8850(10) _cell_angle_beta 86.5090(10) _cell_angle_gamma 71.5080(10) _cell_volume 3296.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 4.629 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4734 _exptl_absorpt_correction_T_max 0.5067 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32798 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.89 _diffrn_reflns_theta_max 27.18 _reflns_number_total 13065 _reflns_number_gt 10859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEXll' _computing_cell_refinement 'Bruker SMART APEXll' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^)+(0.0855P)^2^+7.2266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13065 _refine_ls_number_parameters 729 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Pt1 Pt 0.64425(2) 0.726798(17) 0.107337(10) 0.02871(9) Uani 1 1 d . . . S1 S 0.77844(18) 0.60587(13) 0.06268(8) 0.0407(4) Uani 1 1 d . . . S2 S 0.74764(18) 0.83995(13) 0.05433(8) 0.0391(4) Uani 1 1 d . . . P2 P 0.50019(16) 0.85227(12) 0.14337(7) 0.0298(3) Uani 1 1 d . . . P1 P 0.54231(17) 0.60974(12) 0.14865(7) 0.0315(3) Uani 1 1 d . . . C1 C 0.4552(6) 0.6211(5) 0.2131(3) 0.0330(14) Uani 1 1 d . . . C2 C 0.4016(7) 0.6169(5) 0.2593(3) 0.0353(14) Uani 1 1 d . . . C3 C 0.4894(7) 0.8272(5) 0.2198(3) 0.0341(14) Uani 1 1 d . . . C4 C 0.4774(7) 0.8028(5) 0.2718(3) 0.0372(15) Uani 1 1 d . . . C5 C 0.8476(7) 0.6774(5) 0.0044(3) 0.0375(15) Uani 1 1 d . . . C6 C 0.9126(8) 0.6333(6) -0.0389(3) 0.0485(18) Uani 1 1 d . . . H6 H 0.9169 0.5668 -0.0378 0.058 Uiso 1 1 calc R . . C7 C 0.9717(9) 0.6870(7) -0.0842(3) 0.058(2) Uani 1 1 d . . . H7 H 1.0151 0.6571 -0.1133 0.070 Uiso 1 1 calc R . . C8 C 0.9652(9) 0.7856(7) -0.0852(4) 0.065(2) Uani 1 1 d . . . H8 H 1.0051 0.8217 -0.1153 0.078 Uiso 1 1 calc R . . C9 C 0.9004(8) 0.8311(6) -0.0425(4) 0.052(2) Uani 1 1 d . . . H9 H 0.8972 0.8973 -0.0436 0.063 Uiso 1 1 calc R . . C10 C 0.8393(7) 0.7770(5) 0.0026(3) 0.0380(15) Uani 1 1 d . . . C11 C 0.5338(7) 0.9729(5) 0.1250(3) 0.0355(14) Uani 1 1 d . . . C12 C 0.4574(8) 1.0566(6) 0.0840(3) 0.0477(18) Uani 1 1 d . . . H12 H 0.3840 1.0524 0.0666 0.057 Uiso 1 1 calc R . . C13 C 0.4884(9) 1.1460(6) 0.0686(4) 0.057(2) Uani 1 1 d . . . H13 H 0.4343 1.2028 0.0422 0.068 Uiso 1 1 calc R . . C14 C 0.6024(11) 1.1510(7) 0.0931(4) 0.066(3) Uani 1 1 d . . . H14 H 0.6253 1.2107 0.0824 0.080 Uiso 1 1 calc R . . C15 C 0.6800(10) 1.0669(7) 0.1330(4) 0.065(2) Uani 1 1 d . . . H15 H 0.7564 1.0700 0.1486 0.078 Uiso 1 1 calc R . . C16 C 0.6466(9) 0.9785(6) 0.1502(4) 0.055(2) Uani 1 1 d . . . H16 H 0.6981 0.9230 0.1782 0.066 Uiso 1 1 calc R . . C17 C 0.3302(7) 0.8766(5) 0.1204(3) 0.0346(14) Uani 1 1 d . . . C18 C 0.3095(8) 0.8720(7) 0.0636(4) 0.056(2) Uani 1 1 d . . . H18 H 0.3805 0.8607 0.0386 0.067 Uiso 1 1 calc R . . C19 C 0.1815(10) 0.8845(7) 0.0446(5) 0.068(3) Uani 1 1 d . . . H19 H 0.1673 0.8816 0.0068 0.082 Uiso 1 1 calc R . . C20 C 0.0797(9) 0.9005(7) 0.0808(5) 0.072(3) Uani 1 1 d . . . H20 H -0.0047 0.9072 0.0682 0.086 Uiso 1 1 calc R . . C21 C 0.0979(8) 0.9072(7) 0.1361(5) 0.068(3) Uani 1 1 d . . . H21 H 0.0256 0.9201 0.1603 0.082 Uiso 1 1 calc R . . C22 C 0.2237(8) 0.8948(6) 0.1562(4) 0.0526(19) Uani 1 1 d . . . H22 H 0.2357 0.8988 0.1940 0.063 Uiso 1 1 calc R . . C23 C 0.4160(7) 0.6055(5) 0.1024(3) 0.0384(15) Uani 1 1 d . . . C24 C 0.4411(9) 0.6087(7) 0.0445(4) 0.057(2) Uani 1 1 d . . . H24 H 0.5232 0.6115 0.0296 0.069 Uiso 1 1 calc R . . C25 C 0.3427(10) 0.6079(8) 0.0081(4) 0.066(2) Uani 1 1 d . . . H25 H 0.3607 0.6089 -0.0309 0.079 Uiso 1 1 calc R . . C26 C 0.2226(10) 0.6056(8) 0.0287(4) 0.069(3) Uani 1 1 d . . . H26 H 0.1598 0.6021 0.0043 0.083 Uiso 1 1 calc R . . C27 C 0.1932(11) 0.6083(10) 0.0835(4) 0.084(3) Uani 1 1 d . . . H27 H 0.1076 0.6124 0.0965 0.100 Uiso 1 1 calc R . . C28 C 0.2904(9) 0.6051(8) 0.1221(4) 0.066(3) Uani 1 1 d . . . H28 H 0.2706 0.6026 0.1611 0.079 Uiso 1 1 calc R . . C29 C 0.6504(7) 0.4791(5) 0.1765(3) 0.0397(15) Uani 1 1 d . . . C30 C 0.7422(9) 0.4619(6) 0.2199(5) 0.067(3) Uani 1 1 d . . . H30 H 0.7520 0.5160 0.2322 0.080 Uiso 1 1 calc R . . C31 C 0.8188(10) 0.3632(8) 0.2447(6) 0.085(3) Uani 1 1 d . . . H31 H 0.8779 0.3503 0.2752 0.102 Uiso 1 1 calc R . . C32 C 0.8092(11) 0.2825(8) 0.2248(5) 0.079(3) Uani 1 1 d . . . H32 H 0.8633 0.2162 0.2407 0.095 Uiso 1 1 calc R . . C33 C 0.7219(14) 0.3020(7) 0.1831(6) 0.093(4) Uani 1 1 d . . . H33 H 0.7158 0.2486 0.1690 0.111 Uiso 1 1 calc R . . C34 C 0.6396(11) 0.3983(6) 0.1597(4) 0.067(3) Uani 1 1 d . . . H34 H 0.5754 0.4086 0.1319 0.081 Uiso 1 1 calc R . . Pt2 Pt 0.26678(2) 0.71895(2) 0.374550(10) 0.03520(9) Uani 1 1 d . . . S3 S 0.0774(2) 0.67708(18) 0.40577(9) 0.0533(5) Uani 1 1 d . . . S4 S 0.2253(2) 0.82011(18) 0.43906(9) 0.0557(5) Uani 1 1 d . . . P4 P 0.45767(17) 0.75840(13) 0.34821(7) 0.0337(4) Uani 1 1 d . . . P3 P 0.30307(17) 0.60299(14) 0.32142(7) 0.0344(4) Uani 1 1 d . . . C35 C 0.4844(8) 0.8580(6) 0.3753(3) 0.0426(16) Uani 1 1 d . . . C36 C 0.5912(10) 0.8407(7) 0.4106(4) 0.060(2) Uani 1 1 d . . . H36 H 0.6563 0.7773 0.4198 0.072 Uiso 1 1 calc R . . C37 C 0.6003(15) 0.9207(10) 0.4326(4) 0.093(4) Uani 1 1 d . . . H37 H 0.6705 0.9081 0.4580 0.112 Uiso 1 1 calc R . . C38 C 0.5127(16) 1.0134(10) 0.4185(6) 0.095(4) Uani 1 1 d . . . H38 H 0.5221 1.0651 0.4332 0.114 Uiso 1 1 calc R . . C39 C 0.4081(14) 1.0315(9) 0.3817(6) 0.091(4) Uani 1 1 d . . . H39 H 0.3463 1.0963 0.3714 0.109 Uiso 1 1 calc R . . C40 C 0.3929(10) 0.9555(7) 0.3597(4) 0.067(2) Uani 1 1 d . . . H40 H 0.3218 0.9693 0.3346 0.080 Uiso 1 1 calc R . . C41 C 0.6039(7) 0.6485(5) 0.3696(3) 0.0391(15) Uani 1 1 d . . . C42 C 0.7204(8) 0.6409(8) 0.3398(4) 0.067(3) Uani 1 1 d . . . H42 H 0.7251 0.6917 0.3069 0.081 Uiso 1 1 calc R . . C43 C 0.8313(10) 0.5562(10) 0.3596(5) 0.087(4) Uani 1 1 d . . . H43 H 0.9116 0.5519 0.3407 0.105 Uiso 1 1 calc R . . C44 C 0.8227(10) 0.4797(8) 0.4065(5) 0.079(3) Uani 1 1 d . . . H44 H 0.8966 0.4223 0.4183 0.095 Uiso 1 1 calc R . . C45 C 0.7078(9) 0.4856(7) 0.4364(4) 0.068(3) Uani 1 1 d . . . H45 H 0.7035 0.4333 0.4686 0.081 Uiso 1 1 calc R . . C46 C 0.5966(9) 0.5715(6) 0.4181(3) 0.0520(19) Uani 1 1 d . . . H46 H 0.5180 0.5771 0.4384 0.062 Uiso 1 1 calc R . . C47 C 0.3906(8) 0.4725(5) 0.3609(3) 0.0421(16) Uani 1 1 d . . . C48 C 0.4914(11) 0.4096(7) 0.3380(4) 0.078(3) Uani 1 1 d . . . H48 H 0.5148 0.4310 0.2995 0.094 Uiso 1 1 calc R . . C49 C 0.5605(13) 0.3132(8) 0.3717(6) 0.100(4) Uani 1 1 d . . . H49 H 0.6307 0.2712 0.3556 0.120 Uiso 1 1 calc R . . C50 C 0.5276(12) 0.2797(7) 0.4271(4) 0.077(3) Uani 1 1 d . . . H50 H 0.5732 0.2147 0.4492 0.092 Uiso 1 1 calc R . . C51 C 0.4291(13) 0.3409(8) 0.4497(5) 0.086(3) Uani 1 1 d . . . H51 H 0.4063 0.3176 0.4881 0.103 Uiso 1 1 calc R . . C52 C 0.1590(7) 0.6010(6) 0.2839(3) 0.0428(16) Uani 1 1 d . . . C53 C 0.3583(10) 0.4385(7) 0.4185(4) 0.067(3) Uani 1 1 d . . . H53 H 0.2904 0.4803 0.4359 0.081 Uiso 1 1 calc R . . C54 C 0.0679(8) 0.6933(7) 0.2571(4) 0.056(2) Uani 1 1 d . . . H54 H 0.0723 0.7532 0.2642 0.067 Uiso 1 1 calc R . . C55 C -0.0296(10) 0.6973(10) 0.2199(5) 0.081(3) Uani 1 1 d . . . H55 H -0.0921 0.7595 0.2029 0.097 Uiso 1 1 calc R . . C56 C -0.0341(11) 0.6112(11) 0.2081(5) 0.085(4) Uani 1 1 d . . . H56 H -0.0978 0.6146 0.1817 0.102 Uiso 1 1 calc R . . C57 C 0.0540(11) 0.5186(10) 0.2346(5) 0.080(3) Uani 1 1 d . . . H57 H 0.0477 0.4596 0.2270 0.096 Uiso 1 1 calc R . . C58 C 0.1538(9) 0.5117(8) 0.2730(4) 0.062(2) Uani 1 1 d . . . H58 H 0.2147 0.4490 0.2906 0.074 Uiso 1 1 calc R . . C59 C 0.0866(8) 0.7951(7) 0.4771(4) 0.058(2) Uani 1 1 d . . . C60 C 0.0368(13) 0.8440(10) 0.5221(5) 0.092(4) Uani 1 1 d . . . H60 H 0.0736 0.8905 0.5298 0.110 Uiso 1 1 calc R . . C61 C -0.0699(13) 0.8213(13) 0.5552(5) 0.114(5) Uani 1 1 d . . . H61 H -0.1003 0.8499 0.5864 0.137 Uiso 1 1 calc R . . C62 C -0.1283(10) 0.7577(12) 0.5417(5) 0.092(4) Uani 1 1 d . . . H62 H -0.1998 0.7445 0.5631 0.111 Uiso 1 1 calc R . . C63 C -0.0838(8) 0.7136(9) 0.4975(4) 0.068(3) Uani 1 1 d . . . H63 H -0.1247 0.6702 0.4887 0.081 Uiso 1 1 calc R . . C64 C 0.0258(7) 0.7329(7) 0.4640(3) 0.055(2) Uani 1 1 d . . . C65 C 0.9328(11) 0.9583(8) 0.3267(5) 0.080(3) Uani 1 1 d . . . H65 H 0.9810 0.8923 0.3527 0.096 Uiso 1 1 calc R . . Cl1 Cl 1.0390(4) 0.9946(3) 0.27465(18) 0.1235(13) Uani 1 1 d . . . Cl2 Cl 0.8023(5) 0.9443(5) 0.2930(2) 0.1574(19) Uani 1 1 d . . . Cl3 Cl 0.8715(5) 1.0451(3) 0.36805(18) 0.1332(15) Uani 1 1 d . . . O1 O 0.3132(6) 0.3382(5) 0.1622(3) 0.0734(19) Uani 1 1 d . . . O2 O 0.1963(9) 0.2059(8) 0.2389(5) 0.145(5) Uani 1 1 d . . . O3A O 0.4592(15) 0.2077(12) 0.2547(7) 0.088(4) Uiso 0.50 1 d P . . O3B O 0.4441(17) 0.1386(13) 0.2320(7) 0.094(5) Uiso 0.50 1 d P . . 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 Pt1 0.03040(14) 0.02820(14) 0.02748(14) -0.00505(10) 0.00024(9) -0.01067(10) S1 0.0427(9) 0.0331(8) 0.0462(10) -0.0108(7) 0.0114(7) -0.0127(7) S2 0.0439(9) 0.0349(9) 0.0422(9) -0.0091(7) 0.0077(7) -0.0193(7) P2 0.0348(8) 0.0289(8) 0.0255(8) -0.0054(6) -0.0021(6) -0.0103(7) P1 0.0351(9) 0.0305(8) 0.0299(8) -0.0075(6) 0.0029(6) -0.0124(7) C1 0.036(3) 0.033(3) 0.031(3) -0.008(3) -0.002(3) -0.012(3) C2 0.038(4) 0.029(3) 0.035(4) -0.003(3) -0.004(3) -0.010(3) C3 0.038(4) 0.032(3) 0.032(4) -0.008(3) -0.002(3) -0.011(3) C4 0.044(4) 0.039(4) 0.033(4) -0.008(3) -0.003(3) -0.019(3) C5 0.034(3) 0.039(4) 0.036(4) -0.008(3) 0.002(3) -0.009(3) C6 0.048(4) 0.049(4) 0.045(4) -0.017(3) 0.001(3) -0.007(3) C7 0.056(5) 0.067(6) 0.038(4) -0.011(4) 0.013(4) -0.007(4) C8 0.060(5) 0.071(6) 0.052(5) 0.001(4) 0.021(4) -0.021(5) C9 0.051(5) 0.049(4) 0.051(5) -0.001(4) 0.015(4) -0.020(4) C10 0.038(4) 0.039(4) 0.038(4) -0.006(3) 0.005(3) -0.017(3) C11 0.044(4) 0.032(3) 0.032(3) -0.010(3) 0.000(3) -0.013(3) C12 0.049(4) 0.051(4) 0.039(4) -0.003(3) -0.006(3) -0.016(4) C13 0.077(6) 0.037(4) 0.051(5) 0.001(3) -0.016(4) -0.019(4) C14 0.106(8) 0.044(5) 0.062(5) -0.011(4) 0.005(5) -0.044(5) C15 0.071(6) 0.049(5) 0.082(6) -0.017(5) -0.013(5) -0.027(4) C16 0.064(5) 0.037(4) 0.064(5) -0.006(4) -0.020(4) -0.019(4) C17 0.040(4) 0.029(3) 0.035(3) -0.007(3) -0.003(3) -0.011(3) C18 0.049(5) 0.066(5) 0.051(5) -0.022(4) -0.012(4) -0.006(4) C19 0.069(6) 0.061(6) 0.074(6) -0.018(5) -0.032(5) -0.012(5) C20 0.046(5) 0.064(6) 0.101(8) 0.000(5) -0.024(5) -0.024(4) C21 0.033(4) 0.073(6) 0.081(7) 0.002(5) 0.001(4) -0.011(4) C22 0.044(4) 0.058(5) 0.047(4) -0.003(4) 0.003(3) -0.012(4) C23 0.046(4) 0.037(4) 0.035(4) -0.007(3) -0.003(3) -0.018(3) C24 0.059(5) 0.074(6) 0.049(5) -0.019(4) 0.004(4) -0.032(4) C25 0.093(7) 0.083(6) 0.036(4) -0.018(4) -0.006(4) -0.044(6) C26 0.068(6) 0.088(7) 0.061(6) -0.013(5) -0.018(5) -0.039(5) C27 0.065(6) 0.145(11) 0.060(6) -0.024(6) -0.004(5) -0.059(7) C28 0.067(6) 0.107(8) 0.043(5) -0.020(5) 0.007(4) -0.054(6) C29 0.045(4) 0.034(3) 0.036(4) -0.005(3) 0.011(3) -0.012(3) C30 0.056(5) 0.038(4) 0.100(7) -0.004(4) -0.027(5) -0.011(4) C31 0.047(5) 0.070(7) 0.114(9) 0.007(6) -0.017(5) -0.007(5) C32 0.074(7) 0.047(5) 0.100(9) -0.006(5) 0.017(6) -0.009(5) C33 0.134(11) 0.037(5) 0.101(9) -0.031(5) -0.016(8) -0.003(6) C34 0.099(7) 0.039(4) 0.057(5) -0.013(4) -0.014(5) -0.009(5) Pt2 0.03442(15) 0.04116(16) 0.02823(14) -0.00941(11) 0.00152(10) -0.00905(11) S3 0.0413(10) 0.0723(14) 0.0509(11) -0.0229(10) 0.0126(8) -0.0202(10) S4 0.0572(12) 0.0685(13) 0.0494(11) -0.0317(10) 0.0125(9) -0.0194(10) P4 0.0391(9) 0.0369(9) 0.0246(8) -0.0066(7) -0.0007(6) -0.0120(7) P3 0.0340(9) 0.0407(9) 0.0292(8) -0.0077(7) 0.0021(6) -0.0138(7) C35 0.058(4) 0.049(4) 0.029(3) -0.016(3) 0.006(3) -0.025(4) C36 0.087(6) 0.056(5) 0.048(5) -0.011(4) -0.005(4) -0.038(5) C37 0.151(12) 0.112(10) 0.050(6) -0.018(6) -0.017(6) -0.085(10) C38 0.157(13) 0.076(8) 0.081(8) -0.033(7) 0.019(8) -0.070(9) C39 0.114(10) 0.062(6) 0.104(9) -0.041(6) 0.023(8) -0.026(6) C40 0.082(7) 0.049(5) 0.073(6) -0.023(4) -0.001(5) -0.018(5) C41 0.038(4) 0.044(4) 0.037(4) -0.014(3) -0.003(3) -0.013(3) C42 0.044(5) 0.085(7) 0.057(5) -0.005(5) 0.012(4) -0.011(4) C43 0.043(5) 0.111(9) 0.079(7) -0.004(7) 0.007(5) -0.002(5) C44 0.051(5) 0.080(7) 0.076(7) -0.005(6) -0.013(5) 0.014(5) C45 0.063(6) 0.059(5) 0.066(6) 0.005(4) -0.014(5) -0.013(5) C46 0.058(5) 0.053(5) 0.037(4) -0.002(3) 0.000(3) -0.013(4) C47 0.058(5) 0.039(4) 0.032(4) -0.005(3) -0.001(3) -0.022(3) C48 0.095(8) 0.056(5) 0.053(5) 0.001(4) 0.018(5) 0.002(5) C49 0.117(10) 0.051(6) 0.092(9) -0.001(6) 0.009(7) 0.013(6) C50 0.115(9) 0.043(5) 0.056(6) 0.009(4) -0.021(6) -0.016(5) C51 0.130(10) 0.063(6) 0.053(6) 0.005(5) -0.004(6) -0.029(7) C52 0.042(4) 0.057(4) 0.036(4) -0.014(3) 0.007(3) -0.025(3) C53 0.089(7) 0.048(5) 0.055(5) 0.000(4) 0.013(5) -0.020(5) C54 0.049(5) 0.061(5) 0.052(5) 0.001(4) -0.011(4) -0.020(4) C55 0.053(6) 0.109(9) 0.074(7) 0.003(6) -0.016(5) -0.033(6) C56 0.063(6) 0.134(11) 0.067(6) -0.006(7) -0.017(5) -0.056(7) C57 0.070(7) 0.102(8) 0.095(8) -0.046(7) -0.002(6) -0.045(6) C58 0.054(5) 0.075(6) 0.069(6) -0.024(5) -0.004(4) -0.033(5) C59 0.046(5) 0.069(6) 0.045(4) -0.019(4) 0.010(4) 0.001(4) C60 0.100(9) 0.092(8) 0.089(8) -0.049(7) 0.023(7) -0.021(7) C61 0.084(9) 0.180(15) 0.074(8) -0.068(9) 0.041(7) -0.014(9) C62 0.049(6) 0.154(12) 0.059(6) -0.019(7) 0.016(5) -0.020(7) C63 0.040(4) 0.105(8) 0.045(5) -0.011(5) 0.007(4) -0.012(5) C64 0.034(4) 0.074(6) 0.042(4) -0.012(4) 0.003(3) 0.000(4) C65 0.088(8) 0.072(7) 0.062(6) -0.004(5) -0.012(5) -0.009(6) Cl1 0.113(3) 0.105(3) 0.120(3) -0.012(2) 0.030(2) -0.009(2) Cl2 0.149(4) 0.224(6) 0.132(4) -0.067(4) -0.012(3) -0.082(4) Cl3 0.176(4) 0.121(3) 0.106(3) -0.062(2) 0.016(3) -0.027(3) O1 0.050(3) 0.048(3) 0.115(6) -0.015(4) 0.003(3) -0.011(3) O2 0.089(6) 0.140(8) 0.175(9) 0.081(7) -0.064(6) -0.080(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2581(16) . ? Pt1 P2 2.2780(16) . ? Pt1 S2 2.3025(16) . ? Pt1 S1 2.3130(17) . ? S1 C5 1.765(7) . ? S2 C10 1.770(7) . ? P2 C3 1.757(7) . ? P2 C11 1.810(7) . ? P2 C17 1.817(7) . ? P1 C1 1.756(7) . ? P1 C23 1.809(7) . ? P1 C29 1.826(7) . ? C1 C2 1.198(9) . ? C2 P3 1.760(7) . ? C3 C4 1.200(9) . ? C4 P4 1.781(7) . ? C5 C6 1.380(10) . ? C5 C10 1.388(10) . ? C6 C7 1.389(11) . ? C7 C8 1.382(13) . ? C8 C9 1.378(12) . ? C9 C10 1.402(10) . ? C11 C12 1.381(10) . ? C11 C16 1.404(10) . ? C12 C13 1.372(11) . ? C13 C14 1.403(13) . ? C14 C15 1.376(13) . ? C15 C16 1.375(11) . ? C17 C22 1.372(10) . ? C17 C18 1.398(10) . ? C18 C19 1.402(12) . ? C19 C20 1.339(15) . ? C20 C21 1.368(14) . ? C21 C22 1.388(12) . ? C23 C24 1.373(11) . ? C23 C28 1.388(11) . ? C24 C25 1.401(12) . ? C25 C26 1.345(13) . ? C26 C27 1.326(14) . ? C27 C28 1.403(12) . ? C29 C34 1.354(11) . ? C29 C30 1.382(11) . ? C30 C31 1.378(12) . ? C31 C32 1.389(16) . ? C32 C33 1.311(16) . ? C33 C34 1.366(13) . ? Pt2 P3 2.2604(18) . ? Pt2 P4 2.2820(18) . ? Pt2 S4 2.301(2) . ? Pt2 S3 2.303(2) . ? S3 C64 1.747(8) . ? S4 C59 1.765(9) . ? P4 C41 1.809(7) . ? P4 C35 1.810(7) . ? P3 C47 1.822(7) . ? P3 C52 1.827(7) . ? C35 C36 1.371(11) . ? C35 C40 1.393(12) . ? C36 C37 1.405(13) . ? C37 C38 1.326(18) . ? C38 C39 1.372(18) . ? C39 C40 1.375(14) . ? C41 C42 1.374(11) . ? C41 C46 1.387(10) . ? C42 C43 1.393(13) . ? C43 C44 1.364(15) . ? C44 C45 1.364(14) . ? C45 C46 1.399(12) . ? C47 C48 1.350(12) . ? C47 C53 1.386(11) . ? C48 C49 1.391(13) . ? C49 C50 1.342(15) . ? C50 C51 1.320(16) . ? C51 C53 1.387(13) . ? C52 C54 1.382(11) . ? C52 C58 1.387(11) . ? C54 C55 1.380(12) . ? C55 C56 1.348(17) . ? C56 C57 1.369(16) . ? C57 C58 1.402(13) . ? C59 C64 1.356(13) . ? C59 C60 1.410(13) . ? C60 C61 1.414(18) . ? C61 C62 1.360(19) . ? C62 C63 1.347(15) . ? C63 C64 1.428(12) . ? C65 Cl1 1.712(12) . ? C65 Cl3 1.723(12) . ? C65 Cl2 1.732(12) . ? O3A O3B 1.30(2) . ? 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 Pt1 P2 94.18(6) . . ? P1 Pt1 S2 172.66(6) . . ? P2 Pt1 S2 90.72(6) . . ? P1 Pt1 S1 86.42(6) . . ? P2 Pt1 S1 174.58(6) . . ? S2 Pt1 S1 88.19(6) . . ? C5 S1 Pt1 103.8(2) . . ? C10 S2 Pt1 103.6(2) . . ? C3 P2 C11 101.9(3) . . ? C3 P2 C17 102.6(3) . . ? C11 P2 C17 107.8(3) . . ? C3 P2 Pt1 116.4(2) . . ? C11 P2 Pt1 115.6(2) . . ? C17 P2 Pt1 111.3(2) . . ? C1 P1 C23 101.4(3) . . ? C1 P1 C29 97.1(3) . . ? C23 P1 C29 107.4(3) . . ? C1 P1 Pt1 118.3(2) . . ? C23 P1 Pt1 114.1(2) . . ? C29 P1 Pt1 116.2(2) . . ? C2 C1 P1 172.5(6) . . ? C1 C2 P3 169.7(6) . . ? C4 C3 P2 173.8(6) . . ? C3 C4 P4 175.8(6) . . ? C6 C5 C10 120.1(7) . . ? C6 C5 S1 119.7(6) . . ? C10 C5 S1 120.2(5) . . ? C5 C6 C7 120.7(8) . . ? C8 C7 C6 119.2(7) . . ? C9 C8 C7 121.0(8) . . ? C8 C9 C10 119.6(8) . . ? C5 C10 C9 119.5(7) . . ? C5 C10 S2 121.7(5) . . ? C9 C10 S2 118.7(6) . . ? C12 C11 C16 119.6(7) . . ? C12 C11 P2 121.8(5) . . ? C16 C11 P2 118.5(5) . . ? C13 C12 C11 120.9(7) . . ? C12 C13 C14 119.5(7) . . ? C15 C14 C13 119.6(8) . . ? C16 C15 C14 121.1(8) . . ? C15 C16 C11 119.3(7) . . ? C22 C17 C18 119.0(7) . . ? C22 C17 P2 123.6(6) . . ? C18 C17 P2 117.3(6) . . ? C17 C18 C19 119.8(9) . . ? C20 C19 C18 119.9(9) . . ? C19 C20 C21 121.1(8) . . ? C20 C21 C22 120.3(9) . . ? C17 C22 C21 119.9(8) . . ? C24 C23 C28 117.8(7) . . ? C24 C23 P1 119.5(6) . . ? C28 C23 P1 122.6(6) . . ? C23 C24 C25 119.8(8) . . ? C26 C25 C24 121.0(8) . . ? C27 C26 C25 120.4(8) . . ? C26 C27 C28 120.3(9) . . ? C23 C28 C27 120.4(8) . . ? C34 C29 C30 118.8(7) . . ? C34 C29 P1 123.7(6) . . ? C30 C29 P1 117.3(6) . . ? C31 C30 C29 118.7(9) . . ? C30 C31 C32 121.0(11) . . ? C33 C32 C31 118.4(10) . . ? C32 C33 C34 122.0(10) . . ? C29 C34 C33 121.0(10) . . ? P3 Pt2 P4 95.00(6) . . ? P3 Pt2 S4 172.25(7) . . ? P4 Pt2 S4 89.86(7) . . ? P3 Pt2 S3 86.50(7) . . ? P4 Pt2 S3 177.24(7) . . ? S4 Pt2 S3 88.41(8) . . ? C64 S3 Pt2 104.2(3) . . ? C59 S4 Pt2 103.2(3) . . ? C4 P4 C41 102.9(3) . . ? C4 P4 C35 101.4(3) . . ? C41 P4 C35 106.3(3) . . ? C4 P4 Pt2 115.7(2) . . ? C41 P4 Pt2 112.0(2) . . ? C35 P4 Pt2 117.0(3) . . ? C2 P3 C47 100.7(3) . . ? C2 P3 C52 96.4(3) . . ? C47 P3 C52 107.8(3) . . ? C2 P3 Pt2 117.9(2) . . ? C47 P3 Pt2 114.6(2) . . ? C52 P3 Pt2 116.9(3) . . ? C36 C35 C40 118.9(8) . . ? C36 C35 P4 122.3(6) . . ? C40 C35 P4 118.8(6) . . ? C35 C36 C37 118.6(10) . . ? C38 C37 C36 122.6(11) . . ? C37 C38 C39 118.6(10) . . ? C38 C39 C40 121.2(11) . . ? C39 C40 C35 119.8(10) . . ? C42 C41 C46 120.1(7) . . ? C42 C41 P4 121.9(6) . . ? C46 C41 P4 118.0(6) . . ? C41 C42 C43 119.3(9) . . ? C44 C43 C42 120.2(9) . . ? C43 C44 C45 121.2(9) . . ? C44 C45 C46 119.2(9) . . ? C41 C46 C45 119.8(8) . . ? C48 C47 C53 118.4(8) . . ? C48 C47 P3 123.0(6) . . ? C53 C47 P3 118.4(6) . . ? C47 C48 C49 120.4(9) . . ? C50 C49 C48 121.1(11) . . ? C51 C50 C49 118.7(9) . . ? C50 C51 C53 122.7(10) . . ? C54 C52 C58 120.0(7) . . ? C54 C52 P3 118.1(6) . . ? C58 C52 P3 120.8(6) . . ? C47 C53 C51 118.7(9) . . ? C55 C54 C52 120.5(9) . . ? C56 C55 C54 120.0(10) . . ? C55 C56 C57 120.7(9) . . ? C56 C57 C58 120.8(10) . . ? C52 C58 C57 118.0(9) . . ? C64 C59 C60 119.4(9) . . ? C64 C59 S4 122.6(6) . . ? C60 C59 S4 117.9(9) . . ? C59 C60 C61 119.0(12) . . ? C62 C61 C60 120.4(10) . . ? C63 C62 C61 120.7(10) . . ? C62 C63 C64 120.4(11) . . ? C59 C64 C63 120.0(8) . . ? C59 C64 S3 121.1(6) . . ? C63 C64 S3 118.9(8) . . ? Cl1 C65 Cl3 112.2(7) . . ? Cl1 C65 Cl2 109.2(6) . . ? Cl3 C65 Cl2 109.5(7) . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.541 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.179