# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Ramon Vilar-Compte' 'Jordi Benet-Buchholz' 'Carolina Mendoza' 'Miquel Pericas' _publ_contact_author_name 'Ramon Vilar-Compte' _publ_contact_author_email R.VILAR@IMPERIAL.AC.UK _publ_section_title ; Di-platinum complexes containing thiolato-urea ligands: structural and anion binding studies ; # Attachment '6_CM89_0m.cif' data_cm89_0m _database_code_depnum_ccdc_archive 'CCDC 707942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67.50 H84 F6 N4 O11 P4 Pt2 S4' _chemical_formula_weight 1883.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9595(10) _cell_length_b 21.1557(15) _cell_length_c 25.8230(18) _cell_angle_alpha 90.00 _cell_angle_beta 91.221(2) _cell_angle_gamma 90.00 _cell_volume 7624.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9099 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 39.30 _exptl_crystal_description Block _exptl_crystal_colour translucent _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3756 _exptl_absorpt_coefficient_mu 3.932 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.34103 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 120688 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 39.53 _reflns_number_total 43832 _reflns_number_gt 36118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+24.6199P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 43832 _refine_ls_number_parameters 908 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.004 _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 0.242419(6) 0.594130(4) 0.688482(3) 0.01326(2) Uani 1 1 d . . . S1 S 0.28552(5) 0.69437(3) 0.72228(2) 0.01611(9) Uani 1 1 d . . . P1 P 0.18684(5) 0.50425(3) 0.65071(2) 0.01545(10) Uani 1 1 d . . . C1 C 0.19936(18) 0.50349(13) 0.58067(9) 0.0170(4) Uani 1 1 d . . . N1 N 0.5547(2) 0.76871(19) 0.72023(14) 0.0380(7) Uani 1 1 d . . . H1A H 0.6013 0.7543 0.7404 0.046 Uiso 1 1 calc R . . O1 O 0.51190(19) 0.82109(17) 0.64638(13) 0.0409(7) Uani 1 1 d . . . Pt2 Pt 0.178463(6) 0.745105(4) 0.662955(3) 0.01371(2) Uani 1 1 d . . . S2 S 0.20017(4) 0.65236(3) 0.61301(2) 0.01500(9) Uani 1 1 d . . . P2 P 0.28539(5) 0.54597(3) 0.76408(2) 0.01625(10) Uani 1 1 d . . . C2 C 0.12333(19) 0.52237(13) 0.54817(10) 0.0191(4) Uani 1 1 d . . . H2 H 0.0639 0.5342 0.5626 0.023 Uiso 1 1 calc R . . N2 N 0.6704(2) 0.8089(2) 0.66751(15) 0.0409(8) Uani 1 1 d . . . H2A H 0.7120 0.8021 0.6930 0.049 Uiso 1 1 calc R . . O2 O 0.4302(3) 0.74324(17) 0.48911(17) 0.0551(10) Uani 1 1 d . . . P3 P 0.07237(5) 0.78696(3) 0.60462(2) 0.01640(10) Uani 1 1 d . . . C3 C 0.1342(2) 0.52389(15) 0.49456(10) 0.0234(5) Uani 1 1 d . . . H3 H 0.0822 0.5364 0.4725 0.028 Uiso 1 1 calc R . . N3 N 0.3720(2) 0.64339(15) 0.48812(9) 0.0265(5) Uani 1 1 d . . . H3A H 0.3784 0.6044 0.4768 0.032 Uiso 1 1 calc R . . P4 P 0.15547(5) 0.82835(3) 0.71695(2) 0.01713(11) Uani 1 1 d . . . C4 C 0.2219(2) 0.50702(16) 0.47337(10) 0.0252(5) Uani 1 1 d . . . H4 H 0.2295 0.5079 0.4369 0.030 Uiso 1 1 calc R . . N4 N 0.5132(3) 0.6644(3) 0.44897(15) 0.0551(12) Uani 1 1 d . . . H4A H 0.5154 0.6237 0.4420 0.066 Uiso 1 1 calc R . . C5 C 0.2981(2) 0.48895(16) 0.50567(11) 0.0247(5) Uani 1 1 d . . . H5 H 0.3576 0.4776 0.4912 0.030 Uiso 1 1 calc R . . C6 C 0.2874(2) 0.48747(14) 0.55914(10) 0.0210(4) Uani 1 1 d . . . H6 H 0.3398 0.4756 0.5811 0.025 Uiso 1 1 calc R . . C7 C 0.05877(19) 0.49400(13) 0.65871(10) 0.0182(4) Uani 1 1 d . . . C8 C 0.0138(2) 0.43824(14) 0.64203(10) 0.0215(4) Uani 1 1 d . . . H8 H 0.0512 0.4043 0.6293 0.026 Uiso 1 1 calc R . . C9 C -0.0854(2) 0.43221(15) 0.64407(11) 0.0237(5) Uani 1 1 d . . . H9 H -0.1155 0.3943 0.6326 0.028 Uiso 1 1 calc R . . C10 C -0.1404(2) 0.48155(17) 0.66278(12) 0.0256(5) Uani 1 1 d . . . H10 H -0.2081 0.4772 0.6642 0.031 Uiso 1 1 calc R . . C11 C -0.0969(2) 0.53714(17) 0.67946(13) 0.0263(5) Uani 1 1 d . . . H11 H -0.1348 0.5708 0.6923 0.032 Uiso 1 1 calc R . . C12 C 0.0029(2) 0.54365(14) 0.67732(11) 0.0214(4) Uani 1 1 d . . . H12 H 0.0326 0.5818 0.6885 0.026 Uiso 1 1 calc R . . C13 C 0.2434(2) 0.43076(13) 0.67176(10) 0.0201(4) Uani 1 1 d . . . H13A H 0.2073 0.3949 0.6563 0.024 Uiso 1 1 calc R . . H13B H 0.3092 0.4293 0.6582 0.024 Uiso 1 1 calc R . . C14 C 0.2489(2) 0.42175(14) 0.73085(11) 0.0241(5) Uani 1 1 d . . . H14A H 0.1853 0.4310 0.7453 0.029 Uiso 1 1 calc R . . H14B H 0.2642 0.3770 0.7386 0.029 Uiso 1 1 calc R . . C15 C 0.3241(2) 0.46404(14) 0.75773(11) 0.0227(5) Uani 1 1 d . . . H15A H 0.3837 0.4629 0.7377 0.027 Uiso 1 1 calc R . . H15B H 0.3388 0.4468 0.7926 0.027 Uiso 1 1 calc R . . C16 C 0.1892(2) 0.54386(13) 0.81015(9) 0.0183(4) Uani 1 1 d . . . C17 C 0.1072(2) 0.58013(15) 0.80199(11) 0.0244(5) Uani 1 1 d . . . H17 H 0.1022 0.6070 0.7726 0.029 Uiso 1 1 calc R . . C18 C 0.0321(3) 0.57729(19) 0.83688(14) 0.0322(7) Uani 1 1 d . . . H18 H -0.0243 0.6016 0.8309 0.039 Uiso 1 1 calc R . . C19 C 0.0404(3) 0.53863(18) 0.88042(13) 0.0322(7) Uani 1 1 d . . . H19 H -0.0104 0.5367 0.9042 0.039 Uiso 1 1 calc R . . C20 C 0.1221(3) 0.50312(16) 0.88913(11) 0.0267(6) Uani 1 1 d . . . H20 H 0.1273 0.4769 0.9189 0.032 Uiso 1 1 calc R . . C21 C 0.1967(2) 0.50567(14) 0.85444(10) 0.0215(5) Uani 1 1 d . . . H21 H 0.2530 0.4814 0.8608 0.026 Uiso 1 1 calc R . . C22 C 0.3846(2) 0.58528(14) 0.79707(10) 0.0203(4) Uani 1 1 d . . . C23 C 0.4756(2) 0.58118(18) 0.77568(13) 0.0282(6) Uani 1 1 d . . . H23 H 0.4852 0.5559 0.7458 0.034 Uiso 1 1 calc R . . C24 C 0.5525(3) 0.6144(2) 0.79839(17) 0.0375(8) Uani 1 1 d . . . H24 H 0.6143 0.6118 0.7839 0.045 Uiso 1 1 calc R . . C25 C 0.5382(3) 0.6509(2) 0.84196(18) 0.0392(8) Uani 1 1 d . . . H25 H 0.5906 0.6733 0.8573 0.047 Uiso 1 1 calc R . . C26 C 0.4480(3) 0.65536(19) 0.86368(15) 0.0336(7) Uani 1 1 d . . . H26 H 0.4390 0.6803 0.8938 0.040 Uiso 1 1 calc R . . C27 C 0.3710(2) 0.62294(15) 0.84092(12) 0.0255(5) Uani 1 1 d . . . H27 H 0.3090 0.6264 0.8552 0.031 Uiso 1 1 calc R . . C28 C 0.0175(2) 0.72950(14) 0.56080(10) 0.0210(4) Uani 1 1 d . . . C29 C -0.0386(2) 0.68195(15) 0.58218(12) 0.0244(5) Uani 1 1 d . . . H29 H -0.0447 0.6793 0.6187 0.029 Uiso 1 1 calc R . . C30 C -0.0856(2) 0.63845(17) 0.55022(15) 0.0310(6) Uani 1 1 d . . . H30 H -0.1245 0.6065 0.5648 0.037 Uiso 1 1 calc R . . C31 C -0.0753(3) 0.64186(18) 0.49665(15) 0.0367(8) Uani 1 1 d . . . H31 H -0.1081 0.6126 0.4747 0.044 Uiso 1 1 calc R . . C32 C -0.0174(4) 0.68784(19) 0.47556(13) 0.0398(9) Uani 1 1 d . . . H32 H -0.0092 0.6893 0.4391 0.048 Uiso 1 1 calc R . . C33 C 0.0292(3) 0.73209(17) 0.50730(11) 0.0303(6) Uani 1 1 d . . . H33 H 0.0686 0.7637 0.4926 0.036 Uiso 1 1 calc R . . C34 C 0.1283(2) 0.84533(14) 0.56420(10) 0.0209(4) Uani 1 1 d . . . C35 C 0.0805(3) 0.90045(16) 0.54849(12) 0.0278(6) Uani 1 1 d . . . H35 H 0.0164 0.9078 0.5587 0.033 Uiso 1 1 calc R . . C36 C 0.1273(3) 0.94452(18) 0.51789(14) 0.0364(8) Uani 1 1 d . . . H36 H 0.0954 0.9825 0.5082 0.044 Uiso 1 1 calc R . . C37 C 0.2192(3) 0.9337(2) 0.50151(16) 0.0410(9) Uani 1 1 d . . . H37 H 0.2502 0.9639 0.4804 0.049 Uiso 1 1 calc R . . C38 C 0.2665(3) 0.8782(3) 0.5161(2) 0.0523(14) Uani 1 1 d . . . H38 H 0.3292 0.8700 0.5041 0.063 Uiso 1 1 calc R . . C39 C 0.2217(3) 0.8350(2) 0.54803(16) 0.0387(9) Uani 1 1 d . . . H39 H 0.2551 0.7980 0.5590 0.046 Uiso 1 1 calc R . . C40 C -0.0337(2) 0.82326(14) 0.63194(10) 0.0208(4) Uani 1 1 d . . . H40A H -0.0729 0.8412 0.6031 0.025 Uiso 1 1 calc R . . H40B H -0.0721 0.7895 0.6481 0.025 Uiso 1 1 calc R . . C41 C -0.0166(2) 0.87537(14) 0.67219(10) 0.0223(5) Uani 1 1 d . . . H41A H -0.0789 0.8950 0.6802 0.027 Uiso 1 1 calc R . . H41B H 0.0242 0.9084 0.6568 0.027 Uiso 1 1 calc R . . C42 C 0.0310(2) 0.85288(14) 0.72288(10) 0.0219(5) Uani 1 1 d . . . H42A H -0.0062 0.8169 0.7365 0.026 Uiso 1 1 calc R . . H42B H 0.0281 0.8875 0.7486 0.026 Uiso 1 1 calc R . . C43 C 0.1917(2) 0.81141(13) 0.78334(9) 0.0192(4) Uani 1 1 d . . . C44 C 0.2689(2) 0.84216(16) 0.80731(11) 0.0233(5) Uani 1 1 d . . . H44 H 0.3026 0.8742 0.7895 0.028 Uiso 1 1 calc R . . C45 C 0.2962(2) 0.82538(19) 0.85787(12) 0.0309(7) Uani 1 1 d . . . H45 H 0.3487 0.8463 0.8745 0.037 Uiso 1 1 calc R . . C46 C 0.2473(3) 0.77845(19) 0.88402(11) 0.0317(7) Uani 1 1 d . . . H46 H 0.2668 0.7670 0.9182 0.038 Uiso 1 1 calc R . . C47 C 0.1693(3) 0.74805(17) 0.86001(11) 0.0285(6) Uani 1 1 d . . . H47 H 0.1351 0.7164 0.8781 0.034 Uiso 1 1 calc R . . C48 C 0.1419(2) 0.76422(15) 0.80975(10) 0.0235(5) Uani 1 1 d . . . H48 H 0.0893 0.7433 0.7932 0.028 Uiso 1 1 calc R . . C49 C 0.2221(3) 0.89693(14) 0.69430(12) 0.0282(6) Uani 1 1 d . . . C50 C 0.3001(4) 0.8879(2) 0.6649(2) 0.0507(13) Uani 1 1 d . . . H50 H 0.3226 0.8463 0.6584 0.061 Uiso 1 1 calc R . . C51 C 0.3471(6) 0.9395(3) 0.6441(3) 0.086(3) Uani 1 1 d . . . H51 H 0.4033 0.9337 0.6246 0.104 Uiso 1 1 calc R . . C52 C 0.3111(6) 0.9999(3) 0.6522(3) 0.084(3) Uani 1 1 d . . . H52 H 0.3415 1.0350 0.6366 0.101 Uiso 1 1 calc R . . C53 C 0.2321(5) 1.0097(2) 0.6823(2) 0.0557(13) Uani 1 1 d . . . H53 H 0.2091 1.0513 0.6880 0.067 Uiso 1 1 calc R . . C54 C 0.1865(3) 0.95854(16) 0.70429(15) 0.0344(7) Uani 1 1 d . . . H54 H 0.1326 0.9645 0.7256 0.041 Uiso 1 1 calc R . . C55 C 0.4077(2) 0.70849(16) 0.69970(11) 0.0237(5) Uani 1 1 d . . . H55A H 0.4450 0.6687 0.7013 0.028 Uiso 1 1 calc R . . H55B H 0.4053 0.7232 0.6633 0.028 Uiso 1 1 calc R . . C56 C 0.4559(3) 0.75859(19) 0.73417(14) 0.0331(7) Uani 1 1 d . . . H56A H 0.4202 0.7989 0.7308 0.040 Uiso 1 1 calc R . . H56B H 0.4535 0.7449 0.7708 0.040 Uiso 1 1 calc R . . C57 C 0.5758(2) 0.8004(2) 0.67604(16) 0.0339(7) Uani 1 1 d . . . C58 C 0.7050(3) 0.8289(2) 0.61752(19) 0.0404(9) Uani 1 1 d . . . H58A H 0.7680 0.8498 0.6223 0.048 Uiso 1 1 calc R . . H58B H 0.6598 0.8600 0.6021 0.048 Uiso 1 1 calc R . . C59 C 0.7151(4) 0.7738(3) 0.5809(2) 0.0499(11) Uani 1 1 d . . . H59A H 0.7542 0.7408 0.5976 0.075 Uiso 1 1 calc R . . H59B H 0.7462 0.7881 0.5493 0.075 Uiso 1 1 calc R . . H59C H 0.6516 0.7568 0.5720 0.075 Uiso 1 1 calc R . . C60 C 0.3130(2) 0.65413(14) 0.57727(9) 0.0204(4) Uani 1 1 d . . . H60A H 0.3520 0.6909 0.5886 0.024 Uiso 1 1 calc R . . H60B H 0.3502 0.6152 0.5845 0.024 Uiso 1 1 calc R . . C61 C 0.2899(2) 0.65896(17) 0.51917(10) 0.0252(5) Uani 1 1 d . . . H61A H 0.2365 0.6299 0.5102 0.030 Uiso 1 1 calc R . . H61B H 0.2687 0.7025 0.5109 0.030 Uiso 1 1 calc R . . C62 C 0.4392(3) 0.6871(2) 0.47601(13) 0.0352(8) Uani 1 1 d . . . C63 C 0.5900(3) 0.7054(4) 0.4309(3) 0.092(3) Uani 1 1 d . . . H63A H 0.5746 0.7497 0.4398 0.110 Uiso 1 1 calc R . . H63B H 0.5927 0.7024 0.3927 0.110 Uiso 1 1 calc R . . C64 C 0.6851(4) 0.6893(3) 0.4534(2) 0.0564(13) Uani 1 1 d . . . H64A H 0.6801 0.6840 0.4909 0.085 Uiso 1 1 calc R . . H64B H 0.7304 0.7234 0.4461 0.085 Uiso 1 1 calc R . . H64C H 0.7078 0.6499 0.4380 0.085 Uiso 1 1 calc R . . S1S S 0.45601(6) 0.50075(6) 0.36591(3) 0.03522(19) Uani 1 1 d . . . F1S F 0.31917(18) 0.42190(14) 0.39262(11) 0.0447(6) Uani 1 1 d . . . C1S C 0.4096(3) 0.4214(2) 0.37730(16) 0.0401(9) Uani 1 1 d . . . O2S O 0.55051(19) 0.4886(2) 0.34666(11) 0.0489(9) Uani 1 1 d . . . F2S F 0.4116(3) 0.38635(17) 0.33469(15) 0.0697(10) Uani 1 1 d . . . F3S F 0.4600(3) 0.3914(2) 0.41416(18) 0.0884(15) Uani 1 1 d . . . O3S O 0.4552(3) 0.5304(2) 0.41622(14) 0.0631(12) Uani 1 1 d . . . O1S O 0.3888(2) 0.52562(19) 0.32827(16) 0.0544(9) Uani 1 1 d . . . O2M O 0.4632(9) 0.9799(7) 0.5357(6) 0.111(5) Uani 0.50 1 d P . . H2M H 0.4916 0.9590 0.5130 0.167 Uiso 0.50 1 calc PR . . C2M C 0.5310(11) 1.0129(8) 0.5667(6) 0.082(5) Uani 0.50 1 d P . . H2M1 H 0.5031 1.0528 0.5783 0.123 Uiso 0.50 1 calc PR . . H2M2 H 0.5880 1.0217 0.5464 0.123 Uiso 0.50 1 calc PR . . H2M3 H 0.5490 0.9870 0.5968 0.123 Uiso 0.50 1 calc PR . . O1W O 0.5014(2) 0.84628(19) 0.54130(16) 0.0524(9) Uani 1 1 d . . . H1WA H 0.5000 0.8235 0.5731 0.079 Uiso 1 1 d R . . H1WB H 0.4808 0.8111 0.5210 0.079 Uiso 1 1 d R . . O2W O 0.6448(7) 0.9218(5) 0.5073(4) 0.097(4) Uani 0.50 1 d PD . . H2WA H 0.6733 0.8904 0.4864 0.145 Uiso 1 1 d R . . H2WB H 0.6091 0.9033 0.5159 0.058(19) Uiso 1 1 d RD . . O1M O 0.8373(3) 0.89788(18) 0.51568(14) 0.0577(10) Uani 1 1 d . . . H1M H 0.7778 0.9035 0.5168 0.087 Uiso 1 1 calc R . . C1M C 0.8602(7) 0.8683(3) 0.4682(2) 0.087(3) Uani 1 1 d . . . H1M1 H 0.8277 0.8904 0.4395 0.131 Uiso 1 1 calc R . . H1M2 H 0.8392 0.8241 0.4689 0.131 Uiso 1 1 calc R . . H1M3 H 0.9297 0.8699 0.4635 0.131 Uiso 1 1 calc R . . S1P S 0.83889(7) 0.70942(5) 0.75707(4) 0.03446(17) Uani 1 1 d . . . C1P C 0.8318(5) 0.7349(2) 0.8236(2) 0.0527(13) Uani 1 1 d . . . F1P F 0.8311(5) 0.6847(2) 0.85491(15) 0.122(2) Uani 1 1 d . . . F2P F 0.8985(3) 0.7756(3) 0.83644(16) 0.0998(17) Uani 1 1 d . . . F3P F 0.7473(3) 0.76424(19) 0.83063(19) 0.0839(14) Uani 1 1 d . . . O1P O 0.8352(3) 0.7693(2) 0.72911(16) 0.0579(10) Uani 1 1 d . . . O2P O 0.9307(3) 0.6817(2) 0.75325(16) 0.0698(13) Uani 1 1 d . . . O3P O 0.7570(4) 0.6703(3) 0.7475(2) 0.0933(19) 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 0.01669(3) 0.01452(4) 0.00855(3) -0.00038(2) -0.00022(2) -0.00049(3) S1 0.0197(2) 0.0168(2) 0.0117(2) -0.00180(17) -0.00258(17) 0.00013(19) P1 0.0190(3) 0.0160(3) 0.0113(2) -0.00127(18) 0.00083(18) -0.0017(2) C1 0.0197(9) 0.0191(10) 0.0123(8) -0.0029(7) 0.0000(7) -0.0025(8) N1 0.0255(12) 0.054(2) 0.0341(15) -0.0036(14) -0.0068(11) -0.0111(13) O1 0.0214(10) 0.0576(19) 0.0435(15) 0.0043(14) -0.0003(10) -0.0007(11) Pt2 0.01810(4) 0.01386(4) 0.00909(3) -0.00011(2) -0.00147(2) -0.00118(3) S2 0.0194(2) 0.0161(2) 0.00953(19) -0.00067(16) -0.00096(16) -0.00041(19) P2 0.0202(3) 0.0177(3) 0.0108(2) 0.00101(19) -0.00108(19) 0.0009(2) C2 0.0199(10) 0.0226(11) 0.0148(9) -0.0021(8) -0.0006(7) -0.0007(8) N2 0.0214(12) 0.055(2) 0.0461(19) -0.0048(16) -0.0014(12) -0.0043(13) O2 0.0485(18) 0.0438(18) 0.072(3) 0.0262(17) -0.0208(17) -0.0165(14) P3 0.0212(3) 0.0174(3) 0.0104(2) 0.00068(19) -0.00248(19) 0.0000(2) C3 0.0258(12) 0.0312(14) 0.0131(9) -0.0020(9) -0.0034(8) 0.0004(10) N3 0.0281(11) 0.0376(14) 0.0142(9) -0.0020(9) 0.0059(8) -0.0060(10) P4 0.0232(3) 0.0161(3) 0.0119(2) -0.00191(19) -0.0028(2) -0.0002(2) C4 0.0324(14) 0.0303(14) 0.0130(9) -0.0041(9) 0.0011(9) 0.0003(11) N4 0.0291(15) 0.102(4) 0.0347(17) 0.017(2) 0.0087(13) -0.0102(19) C5 0.0267(12) 0.0317(14) 0.0158(10) -0.0037(9) 0.0039(9) 0.0029(11) C6 0.0213(10) 0.0276(13) 0.0140(9) -0.0019(8) 0.0001(8) 0.0010(9) C7 0.0193(10) 0.0207(11) 0.0147(9) -0.0005(8) 0.0021(7) -0.0034(8) C8 0.0248(11) 0.0230(12) 0.0167(9) -0.0011(8) 0.0015(8) -0.0064(9) C9 0.0231(11) 0.0283(13) 0.0195(10) 0.0017(9) -0.0009(8) -0.0099(10) C10 0.0208(11) 0.0341(15) 0.0219(11) 0.0031(10) -0.0006(9) -0.0045(10) C11 0.0207(11) 0.0318(15) 0.0266(13) -0.0004(11) 0.0028(9) 0.0000(10) C12 0.0207(10) 0.0230(12) 0.0204(10) -0.0018(9) 0.0021(8) -0.0020(9) C13 0.0257(11) 0.0179(11) 0.0168(9) -0.0006(8) 0.0009(8) 0.0036(9) C14 0.0348(14) 0.0191(11) 0.0184(10) 0.0037(9) 0.0004(9) -0.0001(10) C15 0.0307(13) 0.0212(12) 0.0161(9) 0.0022(8) -0.0016(9) 0.0058(10) C16 0.0237(10) 0.0185(10) 0.0127(8) -0.0003(7) -0.0004(7) -0.0014(8) C17 0.0268(12) 0.0271(13) 0.0193(10) 0.0023(9) 0.0037(9) 0.0031(10) C18 0.0300(14) 0.0390(18) 0.0277(14) 0.0016(13) 0.0087(11) 0.0066(13) C19 0.0393(17) 0.0348(17) 0.0230(13) -0.0011(11) 0.0134(12) -0.0017(13) C20 0.0389(15) 0.0277(14) 0.0138(9) -0.0002(9) 0.0045(10) -0.0070(12) C21 0.0281(12) 0.0237(12) 0.0127(9) 0.0012(8) -0.0013(8) -0.0036(10) C22 0.0206(10) 0.0244(12) 0.0157(9) 0.0017(8) -0.0045(8) -0.0004(9) C23 0.0224(12) 0.0385(17) 0.0238(12) -0.0025(11) -0.0005(9) -0.0003(11) C24 0.0232(13) 0.049(2) 0.0403(19) -0.0051(16) -0.0023(13) -0.0025(14) C25 0.0273(15) 0.045(2) 0.045(2) -0.0075(17) -0.0119(14) -0.0055(14) C26 0.0311(15) 0.0346(17) 0.0346(16) -0.0105(13) -0.0090(12) -0.0033(13) C27 0.0262(12) 0.0265(13) 0.0237(12) -0.0051(10) -0.0050(10) -0.0008(10) C28 0.0258(11) 0.0213(11) 0.0156(9) -0.0020(8) -0.0069(8) 0.0010(9) C29 0.0261(12) 0.0245(13) 0.0225(11) -0.0038(9) -0.0038(9) -0.0028(10) C30 0.0282(14) 0.0274(14) 0.0369(16) -0.0078(12) -0.0097(12) -0.0018(11) C31 0.0442(19) 0.0311(16) 0.0338(16) -0.0118(13) -0.0200(15) 0.0027(14) C32 0.066(3) 0.0335(17) 0.0192(12) -0.0073(12) -0.0160(15) 0.0022(17) C33 0.0469(18) 0.0291(15) 0.0146(10) -0.0017(10) -0.0073(11) -0.0022(13) C34 0.0263(11) 0.0218(11) 0.0146(9) 0.0044(8) -0.0012(8) 0.0005(9) C35 0.0358(15) 0.0268(14) 0.0211(11) 0.0084(10) 0.0058(10) 0.0076(11) C36 0.055(2) 0.0279(16) 0.0268(14) 0.0131(12) 0.0064(14) 0.0050(15) C37 0.0381(18) 0.047(2) 0.0374(18) 0.0257(17) -0.0018(14) -0.0074(16) C38 0.0303(17) 0.069(3) 0.058(3) 0.043(2) 0.0090(17) 0.0056(18) C39 0.0287(15) 0.046(2) 0.0419(19) 0.0262(17) 0.0060(13) 0.0085(14) C40 0.0222(11) 0.0241(12) 0.0159(9) -0.0003(8) -0.0018(8) 0.0013(9) C41 0.0272(12) 0.0239(12) 0.0157(9) -0.0011(8) -0.0030(8) 0.0067(10) C42 0.0284(12) 0.0243(12) 0.0128(9) -0.0009(8) -0.0018(8) 0.0049(10) C43 0.0236(10) 0.0215(11) 0.0123(8) -0.0035(8) -0.0033(7) 0.0033(9) C44 0.0226(11) 0.0299(14) 0.0173(10) -0.0068(9) -0.0039(8) 0.0022(10) C45 0.0267(13) 0.0467(19) 0.0188(11) -0.0076(12) -0.0086(10) 0.0048(13) C46 0.0350(15) 0.0458(19) 0.0141(10) -0.0027(11) -0.0067(10) 0.0115(14) C47 0.0378(16) 0.0327(15) 0.0150(10) 0.0009(10) -0.0016(10) 0.0061(12) C48 0.0316(13) 0.0248(12) 0.0139(9) -0.0010(8) -0.0029(9) 0.0028(10) C49 0.0470(18) 0.0130(10) 0.0240(12) -0.0027(9) -0.0104(12) -0.0039(11) C50 0.060(3) 0.034(2) 0.060(3) -0.0135(19) 0.029(2) -0.0225(19) C51 0.108(5) 0.051(3) 0.102(5) -0.024(3) 0.069(5) -0.046(3) C52 0.135(7) 0.040(3) 0.080(4) -0.006(3) 0.042(4) -0.047(4) C53 0.087(4) 0.0217(17) 0.059(3) 0.0025(17) 0.002(3) -0.013(2) C54 0.051(2) 0.0201(13) 0.0324(16) -0.0010(11) -0.0023(14) -0.0026(13) C55 0.0198(10) 0.0299(14) 0.0211(11) -0.0044(10) -0.0011(8) -0.0033(10) C56 0.0280(14) 0.0422(19) 0.0292(14) -0.0121(13) 0.0005(11) -0.0129(13) C57 0.0220(12) 0.0410(19) 0.0384(17) -0.0092(14) -0.0018(12) -0.0046(12) C58 0.0249(14) 0.040(2) 0.056(2) -0.0026(18) 0.0071(15) -0.0022(14) C59 0.048(2) 0.049(3) 0.053(3) -0.001(2) 0.014(2) 0.001(2) C60 0.0247(11) 0.0256(12) 0.0109(8) -0.0001(8) 0.0009(7) -0.0003(9) C61 0.0246(12) 0.0399(16) 0.0112(9) 0.0033(9) 0.0027(8) -0.0033(11) C62 0.0284(14) 0.055(2) 0.0220(12) 0.0181(14) -0.0055(10) -0.0106(14) C63 0.0250(18) 0.155(7) 0.096(5) 0.091(5) 0.011(2) 0.000(3) C64 0.045(2) 0.061(3) 0.063(3) -0.003(3) -0.004(2) -0.008(2) S1S 0.0209(3) 0.0614(6) 0.0234(3) -0.0045(4) 0.0025(2) 0.0000(3) F1S 0.0355(12) 0.0517(15) 0.0478(14) -0.0101(12) 0.0186(10) 0.0018(11) C1S 0.0305(16) 0.055(2) 0.0353(17) 0.0033(17) 0.0104(13) 0.0152(16) O2S 0.0222(11) 0.100(3) 0.0249(11) -0.0084(14) 0.0060(9) -0.0040(14) F2S 0.078(2) 0.062(2) 0.071(2) -0.0262(17) 0.0431(19) -0.0029(17) F3S 0.057(2) 0.117(3) 0.091(3) 0.061(3) -0.001(2) 0.023(2) O3S 0.0525(19) 0.098(3) 0.0401(17) -0.0300(19) 0.0226(15) -0.023(2) O1S 0.0354(15) 0.061(2) 0.066(2) 0.0195(18) -0.0123(15) 0.0011(14) O2M 0.092(8) 0.100(10) 0.139(13) 0.045(8) -0.041(8) -0.023(7) C2M 0.089(10) 0.097(11) 0.059(7) -0.008(7) -0.012(7) -0.043(9) O1W 0.0391(16) 0.056(2) 0.061(2) 0.0144(17) -0.0061(15) -0.0045(15) O2W 0.065(5) 0.098(7) 0.126(9) 0.078(7) -0.034(6) -0.052(5) O1M 0.094(3) 0.0404(18) 0.0390(17) -0.0055(14) -0.0009(18) -0.0201(19) C1M 0.163(8) 0.062(4) 0.037(3) -0.012(2) 0.009(4) -0.046(5) S1P 0.0337(4) 0.0286(4) 0.0410(5) 0.0014(3) -0.0023(3) -0.0044(3) C1P 0.079(4) 0.038(2) 0.042(2) 0.0036(18) 0.022(2) 0.013(2) F1P 0.240(7) 0.083(3) 0.044(2) 0.030(2) 0.043(3) 0.069(4) F2P 0.072(3) 0.170(5) 0.057(2) -0.060(3) -0.0027(19) -0.008(3) F3P 0.091(3) 0.069(2) 0.095(3) -0.005(2) 0.060(2) 0.006(2) O1P 0.062(2) 0.058(2) 0.054(2) 0.0252(18) 0.0056(18) -0.0011(18) O2P 0.062(2) 0.101(3) 0.046(2) -0.026(2) -0.0054(17) 0.033(2) O3P 0.101(4) 0.097(4) 0.082(3) -0.017(3) 0.021(3) -0.069(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 Pt1 P1 2.2663(7) . ? Pt1 P2 2.2714(6) . ? Pt1 S1 2.3662(6) . ? Pt1 S2 2.3696(6) . ? S1 C55 1.839(3) . ? S1 Pt2 2.3737(6) . ? P1 C7 1.817(3) . ? P1 C1 1.821(2) . ? P1 C13 1.821(3) . ? C1 C2 1.397(4) . ? C1 C6 1.401(4) . ? N1 C57 1.362(6) . ? N1 C56 1.449(5) . ? O1 C57 1.242(5) . ? Pt2 P3 2.2698(7) . ? Pt2 P4 2.2732(7) . ? Pt2 S2 2.3711(6) . ? S2 C60 1.843(3) . ? P2 C22 1.812(3) . ? P2 C16 1.813(3) . ? P2 C15 1.824(3) . ? C2 C3 1.396(4) . ? N2 C57 1.356(5) . ? N2 C58 1.451(6) . ? O2 C62 1.242(6) . ? P3 C34 1.805(3) . ? P3 C28 1.819(3) . ? P3 C40 1.823(3) . ? C3 C4 1.397(4) . ? N3 C62 1.359(4) . ? N3 C61 1.450(4) . ? P4 C43 1.813(3) . ? P4 C42 1.823(3) . ? P4 C49 1.826(3) . ? C4 C5 1.391(4) . ? N4 C62 1.347(6) . ? N4 C63 1.463(7) . ? C5 C6 1.392(4) . ? C7 C12 1.399(4) . ? C7 C8 1.400(4) . ? C8 C9 1.393(4) . ? C9 C10 1.389(5) . ? C10 C11 1.388(5) . ? C11 C12 1.403(4) . ? C13 C14 1.538(4) . ? C14 C15 1.533(4) . ? C16 C17 1.391(4) . ? C16 C21 1.402(4) . ? C17 C18 1.398(4) . ? C18 C19 1.393(5) . ? C19 C20 1.380(5) . ? C20 C21 1.389(4) . ? C22 C23 1.398(4) . ? C22 C27 1.401(4) . ? C23 C24 1.401(5) . ? C24 C25 1.383(6) . ? C25 C26 1.392(6) . ? C26 C27 1.395(4) . ? C28 C29 1.396(4) . ? C28 C33 1.396(4) . ? C29 C30 1.391(4) . ? C30 C31 1.396(6) . ? C31 C32 1.384(6) . ? C32 C33 1.396(5) . ? C34 C39 1.395(5) . ? C34 C35 1.399(4) . ? C35 C36 1.394(5) . ? C36 C37 1.378(6) . ? C37 C38 1.395(6) . ? C38 C39 1.389(5) . ? C40 C41 1.530(4) . ? C41 C42 1.531(4) . ? C43 C44 1.393(4) . ? C43 C48 1.402(4) . ? C44 C45 1.398(4) . ? C45 C46 1.388(6) . ? C46 C47 1.398(5) . ? C47 C48 1.388(4) . ? C49 C50 1.356(6) . ? C49 C54 1.420(5) . ? C50 C51 1.387(7) . ? C51 C52 1.389(10) . ? C52 C53 1.380(9) . ? C53 C54 1.382(6) . ? C55 C56 1.530(4) . ? C58 C59 1.509(7) . ? C60 C61 1.531(4) . ? C63 C64 1.478(7) . ? S1S O1S 1.436(3) . ? S1S O2S 1.443(3) . ? S1S O3S 1.443(3) . ? S1S C1S 1.825(5) . ? F1S C1S 1.331(4) . ? C1S F2S 1.328(5) . ? C1S F3S 1.333(5) . ? O2M C2M 1.411(17) . ? O1M C1M 1.418(7) . ? S1P O2P 1.416(4) . ? S1P O3P 1.428(4) . ? S1P O1P 1.459(4) . ? S1P C1P 1.806(5) . ? C1P F2P 1.305(8) . ? C1P F1P 1.333(6) . ? C1P F3P 1.349(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 P1 Pt1 P2 94.32(2) . . ? P1 Pt1 S1 173.08(2) . . ? P2 Pt1 S1 91.41(2) . . ? P1 Pt1 S2 90.30(2) . . ? P2 Pt1 S2 175.32(2) . . ? S1 Pt1 S2 83.93(2) . . ? C55 S1 Pt1 105.01(10) . . ? C55 S1 Pt2 107.30(10) . . ? Pt1 S1 Pt2 90.89(2) . . ? C7 P1 C1 103.14(12) . . ? C7 P1 C13 106.58(13) . . ? C1 P1 C13 103.81(12) . . ? C7 P1 Pt1 112.33(9) . . ? C1 P1 Pt1 113.31(9) . . ? C13 P1 Pt1 116.46(9) . . ? C2 C1 C6 119.5(2) . . ? C2 C1 P1 120.42(19) . . ? C6 C1 P1 119.99(19) . . ? C57 N1 C56 120.3(3) . . ? P3 Pt2 P4 90.35(2) . . ? P3 Pt2 S2 92.92(2) . . ? P4 Pt2 S2 174.93(2) . . ? P3 Pt2 S1 176.08(2) . . ? P4 Pt2 S1 92.85(2) . . ? S2 Pt2 S1 83.74(2) . . ? C60 S2 Pt1 102.84(9) . . ? C60 S2 Pt2 112.09(10) . . ? Pt1 S2 Pt2 90.87(2) . . ? C22 P2 C16 105.78(12) . . ? C22 P2 C15 104.70(14) . . ? C16 P2 C15 105.09(13) . . ? C22 P2 Pt1 112.54(9) . . ? C16 P2 Pt1 112.91(9) . . ? C15 P2 Pt1 114.97(9) . . ? C3 C2 C1 120.3(2) . . ? C57 N2 C58 121.8(4) . . ? C34 P3 C28 106.21(13) . . ? C34 P3 C40 107.48(14) . . ? C28 P3 C40 100.80(13) . . ? C34 P3 Pt2 111.51(9) . . ? C28 P3 Pt2 114.36(9) . . ? C40 P3 Pt2 115.54(9) . . ? C2 C3 C4 119.8(3) . . ? C62 N3 C61 122.0(3) . . ? C43 P4 C42 102.93(12) . . ? C43 P4 C49 109.06(14) . . ? C42 P4 C49 107.06(16) . . ? C43 P4 Pt2 112.75(9) . . ? C42 P4 Pt2 114.80(10) . . ? C49 P4 Pt2 109.85(11) . . ? C5 C4 C3 120.0(3) . . ? C62 N4 C63 121.9(6) . . ? C4 C5 C6 120.3(3) . . ? C5 C6 C1 120.1(3) . . ? C12 C7 C8 119.3(2) . . ? C12 C7 P1 120.4(2) . . ? C8 C7 P1 120.1(2) . . ? C9 C8 C7 120.3(3) . . ? C10 C9 C8 120.2(3) . . ? C11 C10 C9 120.2(3) . . ? C10 C11 C12 120.0(3) . . ? C7 C12 C11 120.1(3) . . ? C14 C13 P1 114.46(19) . . ? C15 C14 C13 113.3(2) . . ? C14 C15 P2 113.2(2) . . ? C17 C16 C21 119.2(3) . . ? C17 C16 P2 120.4(2) . . ? C21 C16 P2 120.4(2) . . ? C16 C17 C18 120.3(3) . . ? C19 C18 C17 119.7(3) . . ? C20 C19 C18 120.4(3) . . ? C19 C20 C21 120.1(3) . . ? C20 C21 C16 120.3(3) . . ? C23 C22 C27 119.7(3) . . ? C23 C22 P2 118.5(2) . . ? C27 C22 P2 121.7(2) . . ? C22 C23 C24 119.9(3) . . ? C25 C24 C23 119.9(3) . . ? C24 C25 C26 120.9(3) . . ? C25 C26 C27 119.5(3) . . ? C26 C27 C22 120.2(3) . . ? C29 C28 C33 119.9(3) . . ? C29 C28 P3 117.9(2) . . ? C33 C28 P3 122.2(2) . . ? C30 C29 C28 120.2(3) . . ? C29 C30 C31 119.8(3) . . ? C32 C31 C30 120.0(3) . . ? C31 C32 C33 120.6(3) . . ? C28 C33 C32 119.5(3) . . ? C39 C34 C35 119.1(3) . . ? C39 C34 P3 119.0(2) . . ? C35 C34 P3 121.9(2) . . ? C36 C35 C34 119.7(3) . . ? C37 C36 C35 120.9(3) . . ? C36 C37 C38 119.7(3) . . ? C39 C38 C37 119.8(4) . . ? C38 C39 C34 120.7(3) . . ? C41 C40 P3 116.7(2) . . ? C40 C41 C42 114.5(2) . . ? C41 C42 P4 114.4(2) . . ? C44 C43 C48 120.2(2) . . ? C44 C43 P4 121.7(2) . . ? C48 C43 P4 118.0(2) . . ? C43 C44 C45 119.3(3) . . ? C46 C45 C44 120.6(3) . . ? C45 C46 C47 120.0(3) . . ? C48 C47 C46 119.9(3) . . ? C47 C48 C43 120.1(3) . . ? C50 C49 C54 121.3(4) . . ? C50 C49 P4 119.3(3) . . ? C54 C49 P4 119.3(3) . . ? C49 C50 C51 119.9(5) . . ? C50 C51 C52 119.4(6) . . ? C53 C52 C51 121.2(5) . . ? C52 C53 C54 119.6(5) . . ? C53 C54 C49 118.6(4) . . ? C56 C55 S1 109.1(2) . . ? N1 C56 C55 111.5(3) . . ? O1 C57 N2 122.9(4) . . ? O1 C57 N1 121.7(3) . . ? N2 C57 N1 115.5(4) . . ? N2 C58 C59 111.8(4) . . ? C61 C60 S2 109.16(19) . . ? N3 C61 C60 112.0(2) . . ? O2 C62 N4 124.4(4) . . ? O2 C62 N3 120.9(4) . . ? N4 C62 N3 114.7(4) . . ? N4 C63 C64 113.3(5) . . ? O1S S1S O2S 114.9(2) . . ? O1S S1S O3S 115.6(3) . . ? O2S S1S O3S 114.4(2) . . ? O1S S1S C1S 102.5(2) . . ? O2S S1S C1S 102.8(2) . . ? O3S S1S C1S 104.2(2) . . ? F2S C1S F1S 106.7(4) . . ? F2S C1S F3S 107.8(4) . . ? F1S C1S F3S 106.4(4) . . ? F2S C1S S1S 111.5(3) . . ? F1S C1S S1S 112.5(3) . . ? F3S C1S S1S 111.6(4) . . ? O2P S1P O3P 118.0(4) . . ? O2P S1P O1P 110.4(3) . . ? O3P S1P O1P 113.5(3) . . ? O2P S1P C1P 104.9(3) . . ? O3P S1P C1P 106.1(3) . . ? O1P S1P C1P 102.1(2) . . ? F2P C1P F1P 112.7(6) . . ? F2P C1P F3P 106.5(5) . . ? F1P C1P F3P 105.5(5) . . ? F2P C1P S1P 112.6(4) . . ? F1P C1P S1P 109.9(4) . . ? F3P C1P S1P 109.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pt1 S1 C55 -117.7(2) . . . . ? P2 Pt1 S1 C55 96.50(10) . . . . ? S2 Pt1 S1 C55 -83.92(10) . . . . ? P1 Pt1 S1 Pt2 -9.5(2) . . . . ? P2 Pt1 S1 Pt2 -155.31(2) . . . . ? S2 Pt1 S1 Pt2 24.26(2) . . . . ? P2 Pt1 P1 C7 93.90(9) . . . . ? S1 Pt1 P1 C7 -51.8(2) . . . . ? S2 Pt1 P1 C7 -85.36(9) . . . . ? P2 Pt1 P1 C1 -149.72(10) . . . . ? S1 Pt1 P1 C1 64.6(2) . . . . ? S2 Pt1 P1 C1 31.02(10) . . . . ? P2 Pt1 P1 C13 -29.40(10) . . . . ? S1 Pt1 P1 C13 -175.08(19) . . . . ? S2 Pt1 P1 C13 151.34(10) . . . . ? C7 P1 C1 C2 26.8(3) . . . . ? C13 P1 C1 C2 137.9(2) . . . . ? Pt1 P1 C1 C2 -94.9(2) . . . . ? C7 P1 C1 C6 -156.9(2) . . . . ? C13 P1 C1 C6 -45.9(3) . . . . ? Pt1 P1 C1 C6 81.4(2) . . . . ? C55 S1 Pt2 P3 113.4(4) . . . . ? Pt1 S1 Pt2 P3 7.4(4) . . . . ? C55 S1 Pt2 P4 -101.98(10) . . . . ? Pt1 S1 Pt2 P4 151.99(2) . . . . ? C55 S1 Pt2 S2 81.77(10) . . . . ? Pt1 S1 Pt2 S2 -24.25(2) . . . . ? P1 Pt1 S2 C60 -95.22(10) . . . . ? P2 Pt1 S2 C60 93.9(3) . . . . ? S1 Pt1 S2 C60 88.62(10) . . . . ? P1 Pt1 S2 Pt2 151.87(2) . . . . ? P2 Pt1 S2 Pt2 -19.1(3) . . . . ? S1 Pt1 S2 Pt2 -24.29(2) . . . . ? P3 Pt2 S2 C60 102.03(9) . . . . ? P4 Pt2 S2 C60 -127.8(3) . . . . ? S1 Pt2 S2 C60 -80.03(9) . . . . ? P3 Pt2 S2 Pt1 -153.72(2) . . . . ? P4 Pt2 S2 Pt1 -23.5(3) . . . . ? S1 Pt2 S2 Pt1 24.22(2) . . . . ? P1 Pt1 P2 C22 151.51(11) . . . . ? S1 Pt1 P2 C22 -32.38(11) . . . . ? S2 Pt1 P2 C22 -37.6(3) . . . . ? P1 Pt1 P2 C16 -88.81(10) . . . . ? S1 Pt1 P2 C16 87.29(10) . . . . ? S2 Pt1 P2 C16 82.1(3) . . . . ? P1 Pt1 P2 C15 31.76(12) . . . . ? S1 Pt1 P2 C15 -152.14(12) . . . . ? S2 Pt1 P2 C15 -157.3(3) . . . . ? C6 C1 C2 C3 1.4(4) . . . . ? P1 C1 C2 C3 177.7(2) . . . . ? P4 Pt2 P3 C34 83.26(11) . . . . ? S2 Pt2 P3 C34 -100.61(11) . . . . ? S1 Pt2 P3 C34 -132.1(3) . . . . ? P4 Pt2 P3 C28 -156.22(11) . . . . ? S2 Pt2 P3 C28 19.91(11) . . . . ? S1 Pt2 P3 C28 -11.6(4) . . . . ? P4 Pt2 P3 C40 -39.84(11) . . . . ? S2 Pt2 P3 C40 136.29(11) . . . . ? S1 Pt2 P3 C40 104.8(4) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? P3 Pt2 P4 C43 160.12(11) . . . . ? S2 Pt2 P4 C43 29.9(3) . . . . ? S1 Pt2 P4 C43 -17.60(11) . . . . ? P3 Pt2 P4 C42 42.66(10) . . . . ? S2 Pt2 P4 C42 -87.6(3) . . . . ? S1 Pt2 P4 C42 -135.06(10) . . . . ? P3 Pt2 P4 C49 -78.02(12) . . . . ? S2 Pt2 P4 C49 151.7(3) . . . . ? S1 Pt2 P4 C49 104.25(12) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C4 C5 C6 C1 0.8(5) . . . . ? C2 C1 C6 C5 -1.5(4) . . . . ? P1 C1 C6 C5 -177.8(2) . . . . ? C1 P1 C7 C12 -110.8(2) . . . . ? C13 P1 C7 C12 140.2(2) . . . . ? Pt1 P1 C7 C12 11.5(2) . . . . ? C1 P1 C7 C8 63.6(2) . . . . ? C13 P1 C7 C8 -45.4(2) . . . . ? Pt1 P1 C7 C8 -174.08(19) . . . . ? C12 C7 C8 C9 -0.1(4) . . . . ? P1 C7 C8 C9 -174.6(2) . . . . ? C7 C8 C9 C10 -0.1(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C9 C10 C11 C12 0.2(5) . . . . ? C8 C7 C12 C11 0.4(4) . . . . ? P1 C7 C12 C11 174.9(2) . . . . ? C10 C11 C12 C7 -0.4(5) . . . . ? C7 P1 C13 C14 -75.6(2) . . . . ? C1 P1 C13 C14 175.9(2) . . . . ? Pt1 P1 C13 C14 50.6(2) . . . . ? P1 C13 C14 C15 -73.4(3) . . . . ? C13 C14 C15 P2 76.8(3) . . . . ? C22 P2 C15 C14 179.5(2) . . . . ? C16 P2 C15 C14 68.2(2) . . . . ? Pt1 P2 C15 C14 -56.5(2) . . . . ? C22 P2 C16 C17 111.1(2) . . . . ? C15 P2 C16 C17 -138.4(2) . . . . ? Pt1 P2 C16 C17 -12.4(3) . . . . ? C22 P2 C16 C21 -68.9(2) . . . . ? C15 P2 C16 C21 41.6(3) . . . . ? Pt1 P2 C16 C21 167.64(19) . . . . ? C21 C16 C17 C18 -1.6(5) . . . . ? P2 C16 C17 C18 178.4(3) . . . . ? C16 C17 C18 C19 1.0(5) . . . . ? C17 C18 C19 C20 -0.2(6) . . . . ? C18 C19 C20 C21 0.0(5) . . . . ? C19 C20 C21 C16 -0.6(5) . . . . ? C17 C16 C21 C20 1.4(4) . . . . ? P2 C16 C21 C20 -178.7(2) . . . . ? C16 P2 C22 C23 165.6(2) . . . . ? C15 P2 C22 C23 54.9(3) . . . . ? Pt1 P2 C22 C23 -70.6(3) . . . . ? C16 P2 C22 C27 -19.0(3) . . . . ? C15 P2 C22 C27 -129.7(3) . . . . ? Pt1 P2 C22 C27 104.8(2) . . . . ? C27 C22 C23 C24 0.4(5) . . . . ? P2 C22 C23 C24 175.9(3) . . . . ? C22 C23 C24 C25 0.2(6) . . . . ? C23 C24 C25 C26 -0.1(7) . . . . ? C24 C25 C26 C27 -0.6(7) . . . . ? C25 C26 C27 C22 1.1(6) . . . . ? C23 C22 C27 C26 -1.1(5) . . . . ? P2 C22 C27 C26 -176.4(3) . . . . ? C34 P3 C28 C29 -174.2(2) . . . . ? C40 P3 C28 C29 -62.3(3) . . . . ? Pt2 P3 C28 C29 62.4(3) . . . . ? C34 P3 C28 C33 5.3(3) . . . . ? C40 P3 C28 C33 117.2(3) . . . . ? Pt2 P3 C28 C33 -118.2(3) . . . . ? C33 C28 C29 C30 -2.3(5) . . . . ? P3 C28 C29 C30 177.2(3) . . . . ? C28 C29 C30 C31 1.0(5) . . . . ? C29 C30 C31 C32 1.0(6) . . . . ? C30 C31 C32 C33 -1.7(6) . . . . ? C29 C28 C33 C32 1.6(5) . . . . ? P3 C28 C33 C32 -177.9(3) . . . . ? C31 C32 C33 C28 0.4(6) . . . . ? C28 P3 C34 C39 -87.1(3) . . . . ? C40 P3 C34 C39 165.6(3) . . . . ? Pt2 P3 C34 C39 38.0(3) . . . . ? C28 P3 C34 C35 92.6(3) . . . . ? C40 P3 C34 C35 -14.6(3) . . . . ? Pt2 P3 C34 C35 -142.2(2) . . . . ? C39 C34 C35 C36 -1.2(5) . . . . ? P3 C34 C35 C36 179.1(3) . . . . ? C34 C35 C36 C37 2.0(6) . . . . ? C35 C36 C37 C38 -0.5(7) . . . . ? C36 C37 C38 C39 -1.7(8) . . . . ? C37 C38 C39 C34 2.5(8) . . . . ? C35 C34 C39 C38 -1.1(7) . . . . ? P3 C34 C39 C38 178.7(4) . . . . ? C34 P3 C40 C41 -69.5(2) . . . . ? C28 P3 C40 C41 179.5(2) . . . . ? Pt2 P3 C40 C41 55.7(2) . . . . ? P3 C40 C41 C42 -66.2(3) . . . . ? C40 C41 C42 P4 68.9(3) . . . . ? C43 P4 C42 C41 175.5(2) . . . . ? C49 P4 C42 C41 60.6(2) . . . . ? Pt2 P4 C42 C41 -61.6(2) . . . . ? C42 P4 C43 C44 -122.2(2) . . . . ? C49 P4 C43 C44 -8.8(3) . . . . ? Pt2 P4 C43 C44 113.5(2) . . . . ? C42 P4 C43 C48 60.3(3) . . . . ? C49 P4 C43 C48 173.7(2) . . . . ? Pt2 P4 C43 C48 -64.0(2) . . . . ? C48 C43 C44 C45 0.1(4) . . . . ? P4 C43 C44 C45 -177.3(2) . . . . ? C43 C44 C45 C46 0.2(5) . . . . ? C44 C45 C46 C47 -0.8(5) . . . . ? C45 C46 C47 C48 1.0(5) . . . . ? C46 C47 C48 C43 -0.7(5) . . . . ? C44 C43 C48 C47 0.2(4) . . . . ? P4 C43 C48 C47 177.7(2) . . . . ? C43 P4 C49 C50 99.2(4) . . . . ? C42 P4 C49 C50 -150.1(4) . . . . ? Pt2 P4 C49 C50 -24.8(4) . . . . ? C43 P4 C49 C54 -85.9(3) . . . . ? C42 P4 C49 C54 24.8(3) . . . . ? Pt2 P4 C49 C54 150.0(2) . . . . ? C54 C49 C50 C51 0.3(8) . . . . ? P4 C49 C50 C51 175.1(6) . . . . ? C49 C50 C51 C52 -2.5(12) . . . . ? C50 C51 C52 C53 3.0(13) . . . . ? C51 C52 C53 C54 -1.2(12) . . . . ? C52 C53 C54 C49 -0.9(8) . . . . ? C50 C49 C54 C53 1.4(6) . . . . ? P4 C49 C54 C53 -173.4(4) . . . . ? Pt1 S1 C55 C56 -159.6(2) . . . . ? Pt2 S1 C55 C56 104.6(2) . . . . ? C57 N1 C56 C55 73.3(5) . . . . ? S1 C55 C56 N1 176.3(3) . . . . ? C58 N2 C57 O1 -15.3(7) . . . . ? C58 N2 C57 N1 166.1(4) . . . . ? C56 N1 C57 O1 -0.5(6) . . . . ? C56 N1 C57 N2 178.1(4) . . . . ? C57 N2 C58 C59 -83.4(5) . . . . ? Pt1 S2 C60 C61 151.7(2) . . . . ? Pt2 S2 C60 C61 -112.0(2) . . . . ? C62 N3 C61 C60 -85.6(4) . . . . ? S2 C60 C61 N3 -164.3(2) . . . . ? C63 N4 C62 O2 -1.9(7) . . . . ? C63 N4 C62 N3 177.4(4) . . . . ? C61 N3 C62 O2 -3.6(5) . . . . ? C61 N3 C62 N4 177.0(3) . . . . ? C62 N4 C63 C64 117.6(7) . . . . ? O1S S1S C1S F2S 63.1(4) . . . . ? O2S S1S C1S F2S -56.4(3) . . . . ? O3S S1S C1S F2S -176.0(3) . . . . ? O1S S1S C1S F1S -56.7(4) . . . . ? O2S S1S C1S F1S -176.3(3) . . . . ? O3S S1S C1S F1S 64.1(4) . . . . ? O1S S1S C1S F3S -176.2(3) . . . . ? O2S S1S C1S F3S 64.2(4) . . . . ? O3S S1S C1S F3S -55.4(4) . . . . ? O2P S1P C1P F2P 59.7(5) . . . . ? O3P S1P C1P F2P -174.6(5) . . . . ? O1P S1P C1P F2P -55.5(5) . . . . ? O2P S1P C1P F1P -66.8(6) . . . . ? O3P S1P C1P F1P 58.8(6) . . . . ? O1P S1P C1P F1P 177.9(5) . . . . ? O2P S1P C1P F3P 177.8(4) . . . . ? O3P S1P C1P F3P -56.5(5) . . . . ? O1P S1P C1P F3P 62.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 39.53 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 3.937 _refine_diff_density_min -4.294 _refine_diff_density_rms 0.185 # Attachment '7_CM113P-1.cif' data_cm113p-1 _database_code_depnum_ccdc_archive 'CCDC 707943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H74 F6 N4 O8 P4 Pt2 S4' _chemical_formula_weight 1903.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _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 12.3835(10) _cell_length_b 12.9382(11) _cell_length_c 13.7580(11) _cell_angle_alpha 66.789(3) _cell_angle_beta 87.151(4) _cell_angle_gamma 70.619(4) _cell_volume 1902.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 3.937 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8567 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43039 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 39.18 _reflns_number_total 18175 _reflns_number_gt 15000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1867P)^2^+7.0124P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18175 _refine_ls_number_parameters 445 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2775 _refine_ls_wR_factor_gt 0.2478 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.165 _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 0.931973(17) 0.545372(17) 0.602411(14) 0.01067(8) Uani 1 1 d . . . P1 P 0.76817(14) 0.54140(15) 0.68540(12) 0.0125(3) Uani 1 1 d . . . S1 S 0.90582(14) 0.44663(14) 0.49711(11) 0.0124(3) Uani 1 1 d . . . C1 C 0.7109(6) 0.4285(6) 0.6841(5) 0.0152(10) Uani 1 1 d . . . N1 N 1.0815(6) 0.1228(5) 0.7356(5) 0.0198(11) Uani 1 1 d . . . H1A H 1.0298 0.0937 0.7712 0.024 Uiso 1 1 calc R . . O1 O 1.2647(6) 0.0792(6) 0.6896(5) 0.0289(13) Uani 1 1 d . . . P2 P 0.98155(15) 0.63191(14) 0.70050(12) 0.0124(3) Uani 1 1 d . . . C2 C 0.7264(7) 0.3229(7) 0.7738(6) 0.0235(14) Uani 1 1 d . . . H2 H 0.7635 0.3109 0.8381 0.028 Uiso 1 1 calc R . . N2 N 1.2118(6) -0.0657(6) 0.8209(5) 0.0257(14) Uani 1 1 d . . . H2A H 1.1513 -0.0876 0.8402 0.031 Uiso 1 1 calc R . . C3 C 0.6878(9) 0.2344(9) 0.7697(8) 0.0322(18) Uani 1 1 d . . . H3 H 0.6985 0.1630 0.8313 0.039 Uiso 1 1 calc R . . C4 C 0.6340(9) 0.2503(8) 0.6765(7) 0.0297(17) Uani 1 1 d . . . H4 H 0.6085 0.1899 0.6738 0.036 Uiso 1 1 calc R . . C5 C 0.6177(7) 0.3560(8) 0.5865(7) 0.0255(15) Uani 1 1 d . . . H5 H 0.5807 0.3673 0.5224 0.031 Uiso 1 1 calc R . . C6 C 0.6554(6) 0.4454(7) 0.5899(5) 0.0188(12) Uani 1 1 d . . . H6 H 0.6435 0.5173 0.5285 0.023 Uiso 1 1 calc R . . C7 C 0.6527(6) 0.6810(6) 0.6163(5) 0.0157(11) Uani 1 1 d . . . C8 C 0.6480(6) 0.7366(6) 0.5055(5) 0.0191(12) Uani 1 1 d . . . H8 H 0.7078 0.7043 0.4688 0.023 Uiso 1 1 calc R . . C9 C 0.5556(7) 0.8394(7) 0.4490(6) 0.0237(14) Uani 1 1 d . . . H9 H 0.5512 0.8757 0.3737 0.028 Uiso 1 1 calc R . . C10 C 0.4694(7) 0.8889(7) 0.5033(7) 0.0255(15) Uani 1 1 d . . . H10 H 0.4060 0.9583 0.4649 0.031 Uiso 1 1 calc R . . C11 C 0.4765(7) 0.8370(7) 0.6124(7) 0.0252(15) Uani 1 1 d . . . H11 H 0.4191 0.8728 0.6490 0.030 Uiso 1 1 calc R . . C12 C 0.5666(6) 0.7327(7) 0.6700(6) 0.0204(13) Uani 1 1 d . . . H12 H 0.5697 0.6967 0.7453 0.024 Uiso 1 1 calc R . . C13 C 0.9248(6) 0.7940(6) 0.6467(5) 0.0157(11) Uani 1 1 d . . . C14 C 0.8649(6) 0.8587(6) 0.5461(5) 0.0162(11) Uani 1 1 d . . . H14 H 0.8506 0.8181 0.5065 0.019 Uiso 1 1 calc R . . C15 C 0.8262(7) 0.9830(6) 0.5039(5) 0.0210(14) Uani 1 1 d . . . H15 H 0.7873 1.0268 0.4345 0.025 Uiso 1 1 calc R . . C16 C 0.8435(8) 1.0434(6) 0.5614(6) 0.0253(16) Uani 1 1 d . . . H16 H 0.8158 1.1284 0.5321 0.030 Uiso 1 1 calc R . . C17 C 0.9017(9) 0.9794(7) 0.6625(6) 0.0294(19) Uani 1 1 d . . . H17 H 0.9134 1.0208 0.7025 0.035 Uiso 1 1 calc R . . C18 C 0.9426(8) 0.8552(7) 0.7052(5) 0.0249(16) Uani 1 1 d . . . H18 H 0.9828 0.8118 0.7741 0.030 Uiso 1 1 calc R . . C19 C 1.1374(6) 0.5880(7) 0.7157(5) 0.0197(13) Uani 1 1 d . . . C20 C 1.1996(7) 0.4657(8) 0.7556(7) 0.0300(18) Uani 1 1 d . . . H20 H 1.1601 0.4098 0.7758 0.036 Uiso 1 1 calc R . . C21 C 1.3192(8) 0.4252(11) 0.7661(9) 0.039(2) Uani 1 1 d . . . H21 H 1.3614 0.3418 0.7940 0.047 Uiso 1 1 calc R . . C22 C 1.3761(8) 0.5067(14) 0.7355(9) 0.050(4) Uani 1 1 d . . . H22 H 1.4578 0.4793 0.7426 0.059 Uiso 1 1 calc R . . C23 C 1.3162(9) 0.6262(14) 0.6953(9) 0.047(3) Uani 1 1 d . . . H23 H 1.3563 0.6816 0.6739 0.056 Uiso 1 1 calc R . . C24 C 1.1959(8) 0.6681(10) 0.6852(7) 0.0302(17) Uani 1 1 d . . . H24 H 1.1546 0.7516 0.6574 0.036 Uiso 1 1 calc R . . C25 C 0.7753(6) 0.5173(6) 0.8250(5) 0.0175(11) Uani 1 1 d . . . H25A H 0.6975 0.5250 0.8492 0.021 Uiso 1 1 calc R . . H25B H 0.8261 0.4342 0.8665 0.021 Uiso 1 1 calc R . . C26 C 0.8196(8) 0.6030(7) 0.8511(6) 0.0256(16) Uani 1 1 d . . . H26A H 0.7752 0.6866 0.8039 0.031 Uiso 1 1 calc R . . H26B H 0.8060 0.5932 0.9253 0.031 Uiso 1 1 calc R . . C27 C 0.9468(6) 0.5808(6) 0.8378(5) 0.0186(12) Uani 1 1 d . . . H27A H 0.9891 0.4939 0.8740 0.022 Uiso 1 1 calc R . . H27B H 0.9744 0.6213 0.8739 0.022 Uiso 1 1 calc R . . C28 C 0.9448(6) 0.2890(6) 0.5902(5) 0.0165(11) Uani 1 1 d . . . H28A H 0.8787 0.2774 0.6312 0.020 Uiso 1 1 calc R . . H28B H 0.9611 0.2382 0.5493 0.020 Uiso 1 1 calc R . . C29 C 1.0488(7) 0.2488(6) 0.6668(5) 0.0189(12) Uani 1 1 d . . . H29A H 1.1141 0.2640 0.6261 0.023 Uiso 1 1 calc R . . H29B H 1.0312 0.2963 0.7107 0.023 Uiso 1 1 calc R . . C30 C 1.1928(7) 0.0490(7) 0.7452(5) 0.0210(13) Uani 1 1 d . . . C31 C 1.3203(7) -0.1499(7) 0.8692(5) 0.0232(14) Uani 1 1 d . . . C32 C 1.3246(8) -0.2649(8) 0.9320(8) 0.036(2) Uani 1 1 d . . . H32 H 1.2563 -0.2845 0.9386 0.044 Uiso 1 1 calc R . . C33 C 1.4269(10) -0.3521(10) 0.9855(8) 0.0369(19) Uiso 1 1 d . . . H33 H 1.4286 -0.4311 1.0279 0.044 Uiso 1 1 calc R . . C34 C 1.5267(9) -0.3251(9) 0.9778(7) 0.0329(17) Uiso 1 1 d . . . H34 H 1.5969 -0.3852 1.0148 0.039 Uiso 1 1 calc R . . C35 C 1.5240(9) -0.2102(9) 0.9161(8) 0.0351(18) Uiso 1 1 d . . . H35 H 1.5924 -0.1910 0.9108 0.042 Uiso 1 1 calc R . . C36 C 1.4207(8) -0.1222(9) 0.8616(8) 0.0326(19) Uani 1 1 d . . . H36 H 1.4190 -0.0431 0.8192 0.039 Uiso 1 1 calc R . . S1S S 0.98310(16) -0.18487(16) 0.99673(12) 0.0199(3) Uani 1 1 d . . . O1S O 1.0227(7) -0.2020(7) 1.0997(5) 0.0381(19) Uani 1 1 d . . . C1S C 0.8263(9) -0.1331(12) 0.9949(9) 0.048(3) Uani 1 1 d . . . F1S F 0.7893(8) -0.0298(10) 1.0067(7) 0.082(4) Uani 1 1 d . . . O2S O 1.0016(6) -0.0877(6) 0.9077(5) 0.0305(13) Uani 1 1 d . . . F2S F 0.7772(7) -0.1129(9) 0.9035(7) 0.063(2) Uani 1 1 d . . . O3S O 1.0113(10) -0.2932(6) 0.9804(6) 0.053(3) Uani 1 1 d . . . F3S F 0.7924(10) -0.2079(12) 1.0752(10) 0.092(3) Uani 1 1 d U . . 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 0.00975(11) 0.01143(11) 0.01462(10) -0.00662(7) 0.00006(6) -0.00636(7) P1 0.0102(6) 0.0159(6) 0.0152(5) -0.0083(5) 0.0017(4) -0.0066(5) S1 0.0117(6) 0.0147(6) 0.0163(5) -0.0086(4) 0.0015(4) -0.0081(5) C1 0.014(2) 0.016(2) 0.019(2) -0.0096(18) 0.0000(17) -0.007(2) N1 0.024(3) 0.016(2) 0.021(2) -0.0072(17) 0.0028(19) -0.010(2) O1 0.025(3) 0.031(3) 0.025(2) -0.005(2) 0.0020(19) -0.010(2) P2 0.0143(6) 0.0127(6) 0.0135(5) -0.0062(4) -0.0011(4) -0.0072(5) C2 0.025(3) 0.023(3) 0.022(3) -0.008(2) -0.003(2) -0.010(3) N2 0.020(3) 0.022(3) 0.027(3) -0.003(2) -0.002(2) -0.006(2) C3 0.038(5) 0.028(4) 0.035(4) -0.012(3) -0.003(3) -0.016(4) C4 0.034(4) 0.025(3) 0.039(4) -0.015(3) -0.001(3) -0.017(3) C5 0.022(3) 0.029(3) 0.034(3) -0.018(3) -0.001(3) -0.011(3) C6 0.015(2) 0.023(3) 0.023(2) -0.012(2) -0.0027(19) -0.008(2) C7 0.014(2) 0.016(2) 0.020(2) -0.0090(18) 0.0018(18) -0.007(2) C8 0.016(3) 0.019(3) 0.023(2) -0.007(2) 0.001(2) -0.009(2) C9 0.021(3) 0.021(3) 0.026(3) -0.004(2) -0.002(2) -0.008(3) C10 0.019(3) 0.016(3) 0.038(4) -0.010(2) -0.004(3) -0.003(2) C11 0.019(3) 0.023(3) 0.034(3) -0.016(3) 0.001(2) -0.003(3) C12 0.014(2) 0.024(3) 0.026(3) -0.015(2) 0.002(2) -0.005(2) C13 0.022(3) 0.013(2) 0.016(2) -0.0068(17) -0.0011(19) -0.009(2) C14 0.017(3) 0.015(2) 0.018(2) -0.0076(17) -0.0020(18) -0.006(2) C15 0.022(3) 0.016(3) 0.022(2) -0.0075(19) -0.005(2) -0.002(2) C16 0.034(4) 0.015(3) 0.025(3) -0.008(2) -0.004(3) -0.006(3) C17 0.050(5) 0.017(3) 0.025(3) -0.012(2) -0.005(3) -0.011(3) C18 0.039(4) 0.020(3) 0.018(2) -0.008(2) -0.007(2) -0.011(3) C19 0.017(3) 0.026(3) 0.018(2) -0.010(2) -0.0026(19) -0.008(2) C20 0.018(3) 0.030(4) 0.041(4) -0.015(3) -0.010(3) -0.004(3) C21 0.017(3) 0.052(6) 0.044(5) -0.020(4) -0.006(3) -0.003(4) C22 0.017(3) 0.084(9) 0.038(5) -0.019(5) -0.002(3) -0.011(5) C23 0.027(4) 0.074(9) 0.042(5) -0.010(5) 0.000(4) -0.036(5) C24 0.022(3) 0.042(5) 0.030(3) -0.009(3) 0.000(3) -0.021(3) C25 0.018(3) 0.022(3) 0.016(2) -0.0087(19) 0.0043(18) -0.011(2) C26 0.034(4) 0.021(3) 0.024(3) -0.013(2) -0.006(3) -0.006(3) C27 0.022(3) 0.020(3) 0.015(2) -0.0048(18) -0.0032(19) -0.011(2) C28 0.018(3) 0.012(2) 0.027(3) -0.0089(19) 0.006(2) -0.013(2) C29 0.025(3) 0.017(2) 0.017(2) -0.0060(18) 0.000(2) -0.010(2) C30 0.023(3) 0.021(3) 0.017(2) -0.0068(19) -0.003(2) -0.006(2) C31 0.021(3) 0.025(3) 0.021(2) -0.007(2) -0.001(2) -0.006(3) C32 0.027(4) 0.024(4) 0.037(4) 0.002(3) 0.008(3) -0.002(3) C36 0.022(3) 0.036(4) 0.039(4) -0.014(3) -0.007(3) -0.008(3) S1S 0.0235(7) 0.0201(7) 0.0171(5) -0.0087(5) -0.0010(5) -0.0069(6) O1S 0.036(3) 0.049(4) 0.022(2) -0.020(2) -0.008(2) 0.003(3) C1S 0.028(4) 0.055(7) 0.035(4) 0.010(4) 0.000(3) -0.015(5) F1S 0.051(5) 0.101(7) 0.048(4) -0.034(4) -0.008(3) 0.038(5) O2S 0.028(3) 0.033(3) 0.031(3) -0.007(2) 0.004(2) -0.017(3) F2S 0.042(4) 0.076(6) 0.071(5) -0.015(4) -0.021(4) -0.032(4) O3S 0.087(7) 0.022(3) 0.043(4) -0.016(3) -0.027(4) 0.000(4) F3S 0.071(5) 0.097(5) 0.091(5) -0.004(4) 0.014(4) -0.048(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 Pt1 P2 2.2762(16) . ? Pt1 P1 2.2834(17) . ? Pt1 S1 2.3698(15) . ? Pt1 S1 2.3819(17) 2_766 ? P1 C7 1.811(6) . ? P1 C25 1.823(6) . ? P1 C1 1.829(7) . ? S1 C28 1.839(7) . ? S1 Pt1 2.3819(17) 2_766 ? C1 C2 1.395(10) . ? C1 C6 1.403(9) . ? N1 C30 1.369(9) . ? N1 C29 1.450(9) . ? O1 C30 1.207(11) . ? P2 C13 1.814(6) . ? P2 C19 1.819(7) . ? P2 C27 1.821(7) . ? C2 C3 1.400(14) . ? N2 C30 1.384(10) . ? N2 C31 1.407(9) . ? C3 C4 1.384(13) . ? C4 C5 1.397(13) . ? C5 C6 1.401(12) . ? C7 C8 1.400(9) . ? C7 C12 1.402(9) . ? C8 C9 1.395(9) . ? C9 C10 1.397(11) . ? C10 C11 1.374(12) . ? C11 C12 1.393(10) . ? C13 C14 1.394(8) . ? C13 C18 1.399(10) . ? C14 C15 1.390(9) . ? C15 C16 1.377(11) . ? C16 C17 1.391(10) . ? C17 C18 1.390(11) . ? C19 C24 1.378(14) . ? C19 C20 1.396(11) . ? C20 C21 1.391(12) . ? C21 C22 1.38(2) . ? C22 C23 1.36(2) . ? C23 C24 1.399(14) . ? C25 C26 1.549(12) . ? C26 C27 1.519(12) . ? C28 C29 1.516(10) . ? C31 C32 1.379(13) . ? C31 C36 1.394(14) . ? C32 C33 1.382(13) . ? C33 C34 1.380(17) . ? C34 C35 1.381(15) . ? C35 C36 1.397(13) . ? S1S O1S 1.431(6) . ? S1S O3S 1.432(7) . ? S1S O2S 1.443(7) . ? S1S C1S 1.829(11) . ? C1S F3S 1.310(15) . ? C1S F2S 1.316(16) . ? C1S F1S 1.33(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 P2 Pt1 P1 91.66(6) . . ? P2 Pt1 S1 172.63(6) . . ? P1 Pt1 S1 95.13(6) . . ? P2 Pt1 S1 91.98(6) . 2_766 ? P1 Pt1 S1 175.37(5) . 2_766 ? S1 Pt1 S1 81.38(7) . 2_766 ? C7 P1 C25 107.1(3) . . ? C7 P1 C1 103.5(3) . . ? C25 P1 C1 103.6(3) . . ? C7 P1 Pt1 109.5(2) . . ? C25 P1 Pt1 116.7(2) . . ? C1 P1 Pt1 115.4(2) . . ? C28 S1 Pt1 104.2(2) . . ? C28 S1 Pt1 104.4(2) . 2_766 ? Pt1 S1 Pt1 98.62(7) . 2_766 ? C2 C1 C6 119.2(7) . . ? C2 C1 P1 121.2(5) . . ? C6 C1 P1 119.5(5) . . ? C30 N1 C29 120.0(7) . . ? C13 P2 C19 107.0(4) . . ? C13 P2 C27 106.2(3) . . ? C19 P2 C27 102.3(3) . . ? C13 P2 Pt1 115.9(2) . . ? C19 P2 Pt1 109.2(2) . . ? C27 P2 Pt1 115.1(3) . . ? C1 C2 C3 120.5(7) . . ? C30 N2 C31 125.1(8) . . ? C4 C3 C2 120.4(9) . . ? C3 C4 C5 119.5(9) . . ? C4 C5 C6 120.5(7) . . ? C5 C6 C1 119.8(7) . . ? C8 C7 C12 119.4(6) . . ? C8 C7 P1 118.5(5) . . ? C12 C7 P1 122.0(5) . . ? C9 C8 C7 120.1(6) . . ? C8 C9 C10 119.9(7) . . ? C11 C10 C9 120.0(6) . . ? C10 C11 C12 120.9(7) . . ? C11 C12 C7 119.7(7) . . ? C14 C13 C18 119.4(6) . . ? C14 C13 P2 120.4(5) . . ? C18 C13 P2 120.2(5) . . ? C15 C14 C13 119.8(6) . . ? C16 C15 C14 120.9(6) . . ? C15 C16 C17 119.7(7) . . ? C18 C17 C16 120.2(7) . . ? C17 C18 C13 120.0(6) . . ? C24 C19 C20 119.2(8) . . ? C24 C19 P2 123.8(6) . . ? C20 C19 P2 116.9(7) . . ? C21 C20 C19 120.3(10) . . ? C22 C21 C20 119.6(10) . . ? C23 C22 C21 120.5(9) . . ? C22 C23 C24 120.5(13) . . ? C19 C24 C23 119.9(11) . . ? C26 C25 P1 115.6(5) . . ? C27 C26 C25 112.7(6) . . ? C26 C27 P2 114.6(4) . . ? C29 C28 S1 112.7(5) . . ? N1 C29 C28 111.6(7) . . ? O1 C30 N1 123.4(7) . . ? O1 C30 N2 123.8(7) . . ? N1 C30 N2 112.6(7) . . ? C32 C31 C36 118.9(8) . . ? C32 C31 N2 117.1(9) . . ? C36 C31 N2 123.9(8) . . ? C31 C32 C33 120.8(11) . . ? C34 C33 C32 120.4(11) . . ? C33 C34 C35 119.7(9) . . ? C34 C35 C36 120.0(12) . . ? C31 C36 C35 120.2(10) . . ? O1S S1S O3S 114.0(4) . . ? O1S S1S O2S 116.4(5) . . ? O3S S1S O2S 113.6(5) . . ? O1S S1S C1S 104.3(5) . . ? O3S S1S C1S 104.5(7) . . ? O2S S1S C1S 102.0(4) . . ? F3S C1S F2S 111.9(14) . . ? F3S C1S F1S 105.6(12) . . ? F2S C1S F1S 106.8(9) . . ? F3S C1S S1S 111.1(8) . . ? F2S C1S S1S 111.2(9) . . ? F1S C1S S1S 110.0(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 P1 C7 87.7(2) . . . . ? S1 Pt1 P1 C7 -95.2(2) . . . . ? S1 Pt1 P1 C7 -54.2(7) 2_766 . . . ? P2 Pt1 P1 C25 -34.1(3) . . . . ? S1 Pt1 P1 C25 143.0(3) . . . . ? S1 Pt1 P1 C25 -176.0(6) 2_766 . . . ? P2 Pt1 P1 C1 -156.1(2) . . . . ? S1 Pt1 P1 C1 21.0(2) . . . . ? S1 Pt1 P1 C1 62.0(7) 2_766 . . . ? P2 Pt1 S1 C28 81.3(5) . . . . ? P1 Pt1 S1 C28 -75.7(2) . . . . ? S1 Pt1 S1 C28 107.3(2) 2_766 . . . ? P2 Pt1 S1 Pt1 -26.0(4) . . . 2_766 ? P1 Pt1 S1 Pt1 176.93(5) . . . 2_766 ? S1 Pt1 S1 Pt1 0.0 2_766 . . 2_766 ? C7 P1 C1 C2 -137.7(6) . . . . ? C25 P1 C1 C2 -26.0(6) . . . . ? Pt1 P1 C1 C2 102.8(6) . . . . ? C7 P1 C1 C6 45.6(6) . . . . ? C25 P1 C1 C6 157.2(5) . . . . ? Pt1 P1 C1 C6 -74.0(5) . . . . ? P1 Pt1 P2 C13 -88.2(3) . . . . ? S1 Pt1 P2 C13 114.7(5) . . . . ? S1 Pt1 P2 C13 89.0(3) 2_766 . . . ? P1 Pt1 P2 C19 151.0(3) . . . . ? S1 Pt1 P2 C19 -6.2(5) . . . . ? S1 Pt1 P2 C19 -31.9(3) 2_766 . . . ? P1 Pt1 P2 C27 36.7(2) . . . . ? S1 Pt1 P2 C27 -120.4(5) . . . . ? S1 Pt1 P2 C27 -146.2(2) 2_766 . . . ? C6 C1 C2 C3 0.4(11) . . . . ? P1 C1 C2 C3 -176.4(7) . . . . ? C1 C2 C3 C4 0.2(14) . . . . ? C2 C3 C4 C5 -0.5(15) . . . . ? C3 C4 C5 C6 0.1(14) . . . . ? C4 C5 C6 C1 0.5(12) . . . . ? C2 C1 C6 C5 -0.8(10) . . . . ? P1 C1 C6 C5 176.1(6) . . . . ? C25 P1 C7 C8 163.3(6) . . . . ? C1 P1 C7 C8 -87.7(6) . . . . ? Pt1 P1 C7 C8 35.9(7) . . . . ? C25 P1 C7 C12 -18.7(8) . . . . ? C1 P1 C7 C12 90.3(7) . . . . ? Pt1 P1 C7 C12 -146.1(6) . . . . ? C12 C7 C8 C9 -2.9(12) . . . . ? P1 C7 C8 C9 175.2(7) . . . . ? C7 C8 C9 C10 1.9(13) . . . . ? C8 C9 C10 C11 0.7(14) . . . . ? C9 C10 C11 C12 -2.3(14) . . . . ? C10 C11 C12 C7 1.3(14) . . . . ? C8 C7 C12 C11 1.3(12) . . . . ? P1 C7 C12 C11 -176.7(7) . . . . ? C19 P2 C13 C14 115.7(6) . . . . ? C27 P2 C13 C14 -135.6(6) . . . . ? Pt1 P2 C13 C14 -6.3(7) . . . . ? C19 P2 C13 C18 -63.1(7) . . . . ? C27 P2 C13 C18 45.6(8) . . . . ? Pt1 P2 C13 C18 174.8(6) . . . . ? C18 C13 C14 C15 1.6(12) . . . . ? P2 C13 C14 C15 -177.2(6) . . . . ? C13 C14 C15 C16 -1.8(12) . . . . ? C14 C15 C16 C17 0.8(14) . . . . ? C15 C16 C17 C18 0.3(16) . . . . ? C16 C17 C18 C13 -0.4(16) . . . . ? C14 C13 C18 C17 -0.5(14) . . . . ? P2 C13 C18 C17 178.3(8) . . . . ? C13 P2 C19 C24 -3.0(7) . . . . ? C27 P2 C19 C24 -114.4(7) . . . . ? Pt1 P2 C19 C24 123.2(6) . . . . ? C13 P2 C19 C20 -179.5(6) . . . . ? C27 P2 C19 C20 69.0(6) . . . . ? Pt1 P2 C19 C20 -53.4(6) . . . . ? C24 C19 C20 C21 1.0(12) . . . . ? P2 C19 C20 C21 177.7(7) . . . . ? C19 C20 C21 C22 -0.8(15) . . . . ? C20 C21 C22 C23 -0.1(17) . . . . ? C21 C22 C23 C24 0.6(18) . . . . ? C20 C19 C24 C23 -0.5(13) . . . . ? P2 C19 C24 C23 -177.0(8) . . . . ? C22 C23 C24 C19 -0.3(16) . . . . ? C7 P1 C25 C26 -70.0(6) . . . . ? C1 P1 C25 C26 -179.0(5) . . . . ? Pt1 P1 C25 C26 53.0(6) . . . . ? P1 C25 C26 C27 -69.7(7) . . . . ? C25 C26 C27 P2 73.8(7) . . . . ? C13 P2 C27 C26 69.2(6) . . . . ? C19 P2 C27 C26 -178.7(6) . . . . ? Pt1 P2 C27 C26 -60.5(6) . . . . ? Pt1 S1 C28 C29 -40.2(5) . . . . ? Pt1 S1 C28 C29 62.8(5) 2_766 . . . ? C30 N1 C29 C28 128.4(7) . . . . ? S1 C28 C29 N1 -177.0(5) . . . . ? C29 N1 C30 O1 -9.3(11) . . . . ? C29 N1 C30 N2 174.6(6) . . . . ? C31 N2 C30 O1 22.7(13) . . . . ? C31 N2 C30 N1 -161.2(7) . . . . ? C30 N2 C31 C32 -171.4(8) . . . . ? C30 N2 C31 C36 12.1(13) . . . . ? C36 C31 C32 C33 -1.0(15) . . . . ? N2 C31 C32 C33 -177.6(9) . . . . ? C31 C32 C33 C34 0.7(16) . . . . ? C32 C33 C34 C35 0.0(16) . . . . ? C33 C34 C35 C36 -0.3(15) . . . . ? C32 C31 C36 C35 0.6(14) . . . . ? N2 C31 C36 C35 177.0(8) . . . . ? C34 C35 C36 C31 0.0(15) . . . . ? O1S S1S C1S F3S -54.8(14) . . . . ? O3S S1S C1S F3S 65.1(14) . . . . ? O2S S1S C1S F3S -176.4(12) . . . . ? O1S S1S C1S F2S 179.8(10) . . . . ? O3S S1S C1S F2S -60.3(11) . . . . ? O2S S1S C1S F2S 58.2(12) . . . . ? O1S S1S C1S F1S 61.7(8) . . . . ? O3S S1S C1S F1S -178.4(7) . . . . ? O2S S1S C1S F1S -59.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.812 _diffrn_reflns_theta_full 39.18 _diffrn_measured_fraction_theta_full 0.812 _refine_diff_density_max 11.483 _refine_diff_density_min -10.372 _refine_diff_density_rms 0.535 # Attachment '9_CM-55_0m.cif' data_cm-55_0m _database_code_depnum_ccdc_archive 'CCDC 707944' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H82 Cl14 N4 O2 P4 Pb2 Pt2 S2' _chemical_formula_weight 2476.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9783(11) _cell_length_b 18.2889(14) _cell_length_c 35.672(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.512(2) _cell_angle_gamma 90.00 _cell_volume 8373.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8710 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 39.30 _exptl_crystal_description Block _exptl_crystal_colour translucent _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4736 _exptl_absorpt_coefficient_mu 7.957 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.34103 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 168281 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 39.60 _reflns_number_total 42493 _reflns_number_gt 33542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+60.8430P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 42493 _refine_ls_number_parameters 885 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.007 _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 0.300995(11) 0.662561(7) 0.363771(4) 0.00768(3) Uani 1 1 d . . . Pb1 Pb 0.420779(13) 0.569320(8) 0.536675(5) 0.01364(3) Uani 1 1 d . . . S1 S 0.21488(7) 0.74894(5) 0.39704(3) 0.00981(16) Uani 1 1 d . . . P1 P 0.38382(8) 0.58978(5) 0.32609(3) 0.00946(18) Uani 1 1 d . . . Cl1 Cl 0.27599(9) 0.48012(6) 0.54946(3) 0.0193(2) Uani 1 1 d . . . N1 N 0.2546(3) 0.79295(19) 0.50970(11) 0.0160(7) Uani 1 1 d . . . H1A H 0.2627 0.8393 0.5162 0.019 Uiso 1 1 calc R . . O1 O 0.2813(3) 0.67419(17) 0.52647(10) 0.0186(6) Uani 1 1 d . . . C1 C 0.3748(3) 0.4926(2) 0.33516(13) 0.0131(7) Uani 1 1 d . . . H1B H 0.4102 0.4655 0.3167 0.016 Uiso 1 1 calc R . . H1C H 0.4121 0.4818 0.3608 0.016 Uiso 1 1 calc R . . P2 P 0.16816(8) 0.58246(5) 0.36576(3) 0.01005(18) Uani 1 1 d . . . Pt2 Pt 0.294799(11) 0.841877(7) 0.365021(4) 0.00763(3) Uani 1 1 d . . . Pb2 Pb 0.635142(14) 0.941907(8) 0.504871(5) 0.01676(3) Uani 1 1 d . . . S2 S 0.42950(7) 0.75519(5) 0.36521(3) 0.00907(16) Uani 1 1 d . . . Cl2 Cl 0.56029(9) 0.45244(6) 0.55445(4) 0.0207(2) Uani 1 1 d . . . O2 O 0.6884(3) 0.83420(17) 0.46685(11) 0.0216(7) Uani 1 1 d . . . N2 N 0.3353(4) 0.7620(2) 0.56979(12) 0.0220(9) Uani 1 1 d . . . H2A H 0.3469 0.7278 0.5873 0.026 Uiso 1 1 calc R . . C2 C 0.2624(4) 0.4649(2) 0.33244(13) 0.0153(8) Uani 1 1 d . . . H2B H 0.2624 0.4109 0.3305 0.018 Uiso 1 1 calc R . . H2C H 0.2214 0.4843 0.3089 0.018 Uiso 1 1 calc R . . P3 P 0.14833(8) 0.91197(5) 0.35785(3) 0.01049(18) Uani 1 1 d . . . N3 N 0.6833(3) 0.71826(19) 0.44433(12) 0.0152(7) Uani 1 1 d . . . H3A H 0.7046 0.6727 0.4473 0.018 Uiso 1 1 calc R . . Cl3 Cl 0.45507(11) 0.61955(6) 0.60923(3) 0.0239(2) Uani 1 1 d . . . C3 C 0.2090(3) 0.4871(2) 0.36636(13) 0.0144(8) Uani 1 1 d . . . H3B H 0.2576 0.4779 0.3900 0.017 Uiso 1 1 calc R . . H3C H 0.1471 0.4557 0.3668 0.017 Uiso 1 1 calc R . . P4 P 0.38575(8) 0.92348(5) 0.33515(3) 0.01006(18) Uani 1 1 d . . . Cl4 Cl 0.78207(10) 1.02174(6) 0.48346(4) 0.0241(2) Uani 1 1 d . . . N4 N 0.7567(4) 0.7437(2) 0.50640(12) 0.0205(8) Uani 1 1 d . . . H4A H 0.7831 0.7771 0.5228 0.025 Uiso 1 1 calc R . . C4 C 0.5226(3) 0.6064(2) 0.32889(12) 0.0112(7) Uani 1 1 d . . . Cl5 Cl 0.59525(11) 1.05851(6) 0.55211(4) 0.0242(2) Uani 1 1 d . . . C5 C 0.5937(3) 0.5730(2) 0.35724(12) 0.0132(7) Uani 1 1 d . . . H5A H 0.5693 0.5413 0.3751 0.016 Uiso 1 1 calc R . . Cl6 Cl 0.75646(13) 0.88099(6) 0.56344(4) 0.0291(3) Uani 1 1 d . . . C6 C 0.7000(4) 0.5864(2) 0.35921(13) 0.0147(8) Uani 1 1 d . . . H6A H 0.7482 0.5629 0.3780 0.018 Uiso 1 1 calc R . . C7 C 0.7355(4) 0.6342(3) 0.33368(14) 0.0178(8) Uani 1 1 d . . . H7A H 0.8081 0.6430 0.3351 0.021 Uiso 1 1 calc R . . C8 C 0.6663(4) 0.6689(3) 0.30627(14) 0.0196(9) Uani 1 1 d . . . H8A H 0.6914 0.7022 0.2893 0.024 Uiso 1 1 calc R . . C9 C 0.5597(4) 0.6554(2) 0.30351(13) 0.0163(8) Uani 1 1 d . . . H9A H 0.5122 0.6791 0.2846 0.020 Uiso 1 1 calc R . . C10 C 0.3335(3) 0.5999(2) 0.27604(12) 0.0128(7) Uani 1 1 d . . . C11 C 0.3710(4) 0.5560(2) 0.24883(14) 0.0185(9) Uani 1 1 d . . . H11A H 0.4235 0.5207 0.2567 0.022 Uiso 1 1 calc R . . C12 C 0.3327(4) 0.5634(3) 0.21070(15) 0.0236(10) Uani 1 1 d . . . H12A H 0.3596 0.5336 0.1926 0.028 Uiso 1 1 calc R . . C13 C 0.2555(5) 0.6139(3) 0.19884(15) 0.0256(10) Uani 1 1 d . . . H13A H 0.2285 0.6186 0.1727 0.031 Uiso 1 1 calc R . . C14 C 0.2175(5) 0.6584(3) 0.22598(16) 0.0279(11) Uani 1 1 d . . . H14A H 0.1652 0.6938 0.2181 0.034 Uiso 1 1 calc R . . C15 C 0.2557(4) 0.6508(2) 0.26387(14) 0.0188(9) Uani 1 1 d . . . H15A H 0.2287 0.6806 0.2820 0.023 Uiso 1 1 calc R . . C16 C 0.0636(3) 0.5922(2) 0.32602(12) 0.0119(7) Uani 1 1 d . . . C17 C 0.0029(4) 0.5323(2) 0.31128(15) 0.0194(9) Uani 1 1 d . . . H17A H 0.0167 0.4850 0.3218 0.023 Uiso 1 1 calc R . . C18 C -0.0771(4) 0.5423(3) 0.28136(17) 0.0252(11) Uani 1 1 d . . . H18A H -0.1170 0.5013 0.2712 0.030 Uiso 1 1 calc R . . C19 C -0.0998(4) 0.6111(3) 0.26608(14) 0.0213(9) Uani 1 1 d . . . H19A H -0.1548 0.6173 0.2456 0.026 Uiso 1 1 calc R . . C20 C -0.0411(4) 0.6712(3) 0.28094(14) 0.0201(9) Uani 1 1 d . . . H20A H -0.0569 0.7187 0.2710 0.024 Uiso 1 1 calc R . . C21 C 0.0404(4) 0.6611(2) 0.31033(13) 0.0166(8) Uani 1 1 d . . . H21A H 0.0811 0.7019 0.3200 0.020 Uiso 1 1 calc R . . C22 C 0.1033(3) 0.5906(2) 0.40746(12) 0.0130(7) Uani 1 1 d . . . C23 C 0.0030(4) 0.6196(2) 0.40511(14) 0.0178(8) Uani 1 1 d . . . H23A H -0.0318 0.6370 0.3815 0.021 Uiso 1 1 calc R . . C24 C -0.0462(4) 0.6231(3) 0.43705(15) 0.0211(10) Uani 1 1 d . . . H24A H -0.1146 0.6426 0.4353 0.025 Uiso 1 1 calc R . . C25 C 0.0045(4) 0.5982(3) 0.47146(15) 0.0216(10) Uani 1 1 d . . . H25A H -0.0296 0.5999 0.4932 0.026 Uiso 1 1 calc R . . C26 C 0.1051(4) 0.5707(3) 0.47443(14) 0.0207(9) Uani 1 1 d . . . H26A H 0.1401 0.5543 0.4982 0.025 Uiso 1 1 calc R . . C27 C 0.1543(4) 0.5673(2) 0.44230(14) 0.0178(8) Uani 1 1 d . . . H27A H 0.2233 0.5488 0.4443 0.021 Uiso 1 1 calc R . . C28 C 0.1696(4) 1.0097(2) 0.36032(13) 0.0152(8) Uani 1 1 d . . . H28A H 0.1014 1.0346 0.3545 0.018 Uiso 1 1 calc R . . H28B H 0.1994 1.0227 0.3867 0.018 Uiso 1 1 calc R . . C29 C 0.2420(4) 1.0393(2) 0.33355(14) 0.0166(8) Uani 1 1 d . . . H29A H 0.2184 1.0204 0.3077 0.020 Uiso 1 1 calc R . . H29B H 0.2364 1.0932 0.3326 0.020 Uiso 1 1 calc R . . C30 C 0.3563(4) 1.0182(2) 0.34536(13) 0.0153(8) Uani 1 1 d . . . H30A H 0.3752 1.0268 0.3729 0.018 Uiso 1 1 calc R . . H30B H 0.4003 1.0506 0.3321 0.018 Uiso 1 1 calc R . . C31 C 0.0684(3) 0.8985(2) 0.31226(12) 0.0117(7) Uani 1 1 d . . . C32 C 0.1012(4) 0.8539(2) 0.28436(13) 0.0148(8) Uani 1 1 d . . . H32A H 0.1662 0.8293 0.2895 0.018 Uiso 1 1 calc R . . C33 C 0.0401(4) 0.8450(2) 0.24933(14) 0.0200(9) Uani 1 1 d . . . H33A H 0.0641 0.8156 0.2304 0.024 Uiso 1 1 calc R . . C34 C -0.0570(4) 0.8795(3) 0.24195(15) 0.0218(9) Uani 1 1 d . . . H34A H -0.1001 0.8723 0.2183 0.026 Uiso 1 1 calc R . . C35 C -0.0902(4) 0.9241(3) 0.26923(16) 0.0231(10) Uani 1 1 d . . . H35A H -0.1558 0.9480 0.2640 0.028 Uiso 1 1 calc R . . C36 C -0.0287(4) 0.9340(3) 0.30400(15) 0.0211(9) Uani 1 1 d . . . H36A H -0.0521 0.9650 0.3224 0.025 Uiso 1 1 calc R . . C37 C 0.0602(3) 0.8947(2) 0.39195(12) 0.0137(8) Uani 1 1 d . . . C38 C 0.0633(4) 0.9388(3) 0.42422(14) 0.0203(9) Uani 1 1 d . . . H38A H 0.1111 0.9783 0.4285 0.024 Uiso 1 1 calc R . . C39 C -0.0051(4) 0.9238(3) 0.45013(15) 0.0239(11) Uani 1 1 d . . . H39A H -0.0053 0.9545 0.4716 0.029 Uiso 1 1 calc R . . C40 C -0.0725(4) 0.8645(3) 0.44479(16) 0.0283(13) Uani 1 1 d . . . H40A H -0.1182 0.8546 0.4627 0.034 Uiso 1 1 calc R . . C41 C -0.0731(4) 0.8200(3) 0.41350(16) 0.0243(11) Uani 1 1 d . . . H41A H -0.1184 0.7790 0.4102 0.029 Uiso 1 1 calc R . . C42 C -0.0078(4) 0.8346(2) 0.38662(15) 0.0196(9) Uani 1 1 d . . . H42A H -0.0094 0.8043 0.3649 0.024 Uiso 1 1 calc R . . C43 C 0.3652(3) 0.9145(2) 0.28400(12) 0.0142(8) Uani 1 1 d . . . C44 C 0.3647(4) 0.9757(3) 0.26024(14) 0.0193(9) Uani 1 1 d . . . H44A H 0.3696 1.0234 0.2709 0.023 Uiso 1 1 calc R . . C45 C 0.3571(5) 0.9669(3) 0.22134(15) 0.0286(12) Uani 1 1 d . . . H45A H 0.3559 1.0086 0.2054 0.034 Uiso 1 1 calc R . . C46 C 0.3514(5) 0.8974(4) 0.20566(15) 0.0316(13) Uani 1 1 d . . . H46A H 0.3479 0.8917 0.1790 0.038 Uiso 1 1 calc R . . C47 C 0.3507(5) 0.8362(3) 0.22868(15) 0.0266(11) Uani 1 1 d . . . H47A H 0.3459 0.7886 0.2179 0.032 Uiso 1 1 calc R . . C48 C 0.3572(4) 0.8452(2) 0.26769(13) 0.0180(8) Uani 1 1 d . . . H48A H 0.3561 0.8034 0.2834 0.022 Uiso 1 1 calc R . . C49 C 0.5274(3) 0.9187(2) 0.34656(12) 0.0129(7) Uani 1 1 d . . . C50 C 0.5872(4) 0.8831(2) 0.32266(15) 0.0190(9) Uani 1 1 d . . . H50A H 0.5540 0.8576 0.3010 0.023 Uiso 1 1 calc R . . C51 C 0.6954(4) 0.8848(3) 0.33055(17) 0.0237(10) Uani 1 1 d . . . H51A H 0.7358 0.8603 0.3143 0.028 Uiso 1 1 calc R . . C52 C 0.7443(4) 0.9218(3) 0.36190(16) 0.0235(10) Uani 1 1 d . . . H52A H 0.8182 0.9243 0.3666 0.028 Uiso 1 1 calc R . . C53 C 0.6856(4) 0.9556(3) 0.38668(15) 0.0244(10) Uani 1 1 d . . . H53A H 0.7193 0.9802 0.4086 0.029 Uiso 1 1 calc R . . C54 C 0.5771(4) 0.9532(3) 0.37920(14) 0.0211(9) Uani 1 1 d . . . H54A H 0.5369 0.9751 0.3964 0.025 Uiso 1 1 calc R . . C55 C 0.2817(3) 0.7532(2) 0.44626(11) 0.0128(7) Uani 1 1 d . . . H55A H 0.3127 0.7050 0.4540 0.015 Uiso 1 1 calc R . . H55B H 0.3385 0.7898 0.4484 0.015 Uiso 1 1 calc R . . C56 C 0.2023(3) 0.7745(2) 0.47200(12) 0.0145(8) Uani 1 1 d . . . H56A H 0.1612 0.8170 0.4610 0.017 Uiso 1 1 calc R . . H56B H 0.1538 0.7333 0.4737 0.017 Uiso 1 1 calc R . . C57 C 0.2913(4) 0.7407(2) 0.53509(12) 0.0147(8) Uani 1 1 d . . . C58 C 0.3657(5) 0.8361(3) 0.58127(15) 0.0246(10) Uani 1 1 d . . . H58A H 0.3777 0.8390 0.6093 0.030 Uiso 1 1 calc R . . H58B H 0.3083 0.8700 0.5718 0.030 Uiso 1 1 calc R . . C59 C 0.4644(6) 0.8598(4) 0.5660(3) 0.052(2) Uani 1 1 d . . . H59A H 0.4788 0.9113 0.5723 0.078 Uiso 1 1 calc R . . H59B H 0.4545 0.8536 0.5384 0.078 Uiso 1 1 calc R . . H59C H 0.5232 0.8298 0.5775 0.078 Uiso 1 1 calc R . . C60 C 0.5064(3) 0.7486(2) 0.41283(12) 0.0141(7) Uani 1 1 d . . . H60A H 0.4951 0.7927 0.4278 0.017 Uiso 1 1 calc R . . H60B H 0.4840 0.7053 0.4262 0.017 Uiso 1 1 calc R . . C61 C 0.6216(3) 0.7418(2) 0.40891(13) 0.0150(8) Uani 1 1 d . . . H61A H 0.6297 0.7060 0.3887 0.018 Uiso 1 1 calc R . . H61B H 0.6476 0.7896 0.4014 0.018 Uiso 1 1 calc R . . C62 C 0.7077(4) 0.7679(2) 0.47304(14) 0.0169(8) Uani 1 1 d . . . C63 C 0.7707(4) 0.6682(2) 0.51829(15) 0.0208(9) Uani 1 1 d . . . H63A H 0.8276 0.6654 0.5400 0.025 Uiso 1 1 calc R . . H63B H 0.7919 0.6392 0.4973 0.025 Uiso 1 1 calc R . . C64 C 0.6726(5) 0.6349(4) 0.52970(18) 0.0351(14) Uani 1 1 d . . . H64A H 0.6875 0.5852 0.5391 0.053 Uiso 1 1 calc R . . H64B H 0.6178 0.6335 0.5076 0.053 Uiso 1 1 calc R . . H64C H 0.6492 0.6647 0.5497 0.053 Uiso 1 1 calc R . . Cl1C Cl 0.06469(18) 0.20168(11) 0.32096(5) 0.0524(5) Uani 1 1 d . . . C1C C 0.0964(5) 0.2288(3) 0.36836(16) 0.0298(12) Uani 1 1 d . . . H1CA H 0.1173 0.1853 0.3842 0.036 Uiso 1 1 calc R . . H1CB H 0.0340 0.2502 0.3771 0.036 Uiso 1 1 calc R . . Cl2C Cl 0.1989(2) 0.29357(9) 0.37457(7) 0.0603(6) Uani 1 1 d . . . Cl1A Cl 0.34769(18) 0.31694(12) 0.27308(6) 0.0549(5) Uani 1 1 d . . . C1A C 0.4069(7) 0.2716(4) 0.3139(2) 0.0483(19) Uani 1 1 d . . . H1AA H 0.3528 0.2582 0.3295 0.058 Uiso 1 1 calc R . . H1AB H 0.4563 0.3055 0.3290 0.058 Uiso 1 1 calc R . . Cl2A Cl 0.47489(18) 0.19155(9) 0.30393(6) 0.0531(5) Uani 1 1 d . . . Cl1D Cl 0.1609(2) 0.68612(16) 0.63929(7) 0.0772(9) Uani 1 1 d . . . C1D C 0.1597(5) 0.6250(4) 0.60099(19) 0.0354(14) Uani 1 1 d . . . H1DA H 0.2126 0.5864 0.6081 0.043 Uiso 1 1 calc R . . H1DB H 0.1791 0.6518 0.5790 0.043 Uiso 1 1 calc R . . Cl2D Cl 0.03638(16) 0.58337(10) 0.58777(8) 0.0598(6) Uani 1 1 d . . . Cl1B Cl 0.91803(13) 0.10955(8) 0.40017(5) 0.0369(3) Uani 1 1 d . . . C1B C 0.9696(5) 0.1313(3) 0.44706(18) 0.0317(13) Uani 1 1 d . . . H1BA H 1.0393 0.1087 0.4533 0.038 Uiso 1 1 calc R . . H1BB H 0.9242 0.1104 0.4643 0.038 Uiso 1 1 calc R . . Cl2B Cl 0.98075(12) 0.22702(8) 0.45479(5) 0.0328(3) 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 0.00594(6) 0.00968(4) 0.00749(6) -0.00002(4) 0.00122(5) -0.00006(4) Pb1 0.01342(7) 0.01604(5) 0.01147(7) 0.00071(4) 0.00191(6) 0.00091(5) S1 0.0085(4) 0.0122(3) 0.0094(4) 0.0011(3) 0.0036(4) 0.0004(3) P1 0.0076(4) 0.0109(3) 0.0100(4) -0.0006(3) 0.0018(4) 0.0014(3) Cl1 0.0165(5) 0.0203(4) 0.0204(5) 0.0026(3) 0.0009(5) -0.0022(3) N1 0.021(2) 0.0158(13) 0.0107(16) -0.0018(11) 0.0027(16) 0.0029(12) O1 0.0216(18) 0.0172(13) 0.0149(15) -0.0012(10) -0.0042(15) -0.0004(11) C1 0.0121(18) 0.0118(13) 0.0156(19) 0.0000(11) 0.0023(17) 0.0023(11) P2 0.0075(4) 0.0117(4) 0.0107(5) 0.0000(3) 0.0003(4) -0.0010(3) Pt2 0.00635(6) 0.00990(4) 0.00679(6) 0.00088(4) 0.00145(5) 0.00093(4) Pb2 0.01505(8) 0.01935(6) 0.01533(7) -0.00079(5) 0.00048(7) 0.00225(5) S2 0.0073(4) 0.0104(3) 0.0098(4) 0.0001(3) 0.0021(4) -0.0002(3) Cl2 0.0151(5) 0.0217(4) 0.0248(6) 0.0013(4) 0.0017(5) 0.0042(3) O2 0.0262(19) 0.0159(13) 0.0214(17) -0.0022(11) -0.0011(16) 0.0003(12) N2 0.032(3) 0.0156(15) 0.0156(18) 0.0001(12) -0.005(2) 0.0025(14) C2 0.016(2) 0.0135(14) 0.018(2) -0.0010(12) 0.0043(18) -0.0010(12) P3 0.0084(5) 0.0134(4) 0.0100(5) 0.0016(3) 0.0025(4) 0.0024(3) N3 0.0097(16) 0.0166(14) 0.0175(18) -0.0022(12) -0.0044(16) 0.0022(11) Cl3 0.0347(7) 0.0200(4) 0.0139(5) -0.0007(3) -0.0068(5) 0.0087(4) C3 0.0125(19) 0.0139(14) 0.018(2) 0.0009(12) 0.0045(18) 0.0001(12) P4 0.0087(5) 0.0117(4) 0.0101(4) 0.0015(3) 0.0021(4) -0.0004(3) Cl4 0.0281(6) 0.0216(4) 0.0253(6) -0.0024(4) 0.0128(6) 0.0001(4) N4 0.026(2) 0.0159(15) 0.0177(19) -0.0012(12) -0.0034(18) -0.0008(13) C4 0.0087(17) 0.0143(14) 0.0111(17) -0.0022(11) 0.0034(15) 0.0017(11) Cl5 0.0281(6) 0.0248(5) 0.0219(6) -0.0019(4) 0.0107(5) 0.0035(4) C5 0.0107(18) 0.0184(15) 0.0105(17) 0.0000(12) 0.0017(16) -0.0001(12) Cl6 0.0416(8) 0.0203(5) 0.0209(6) -0.0044(4) -0.0102(6) 0.0056(5) C6 0.0122(19) 0.0211(16) 0.0104(18) -0.0011(13) 0.0007(17) 0.0026(13) C7 0.0094(19) 0.0281(19) 0.016(2) -0.0024(15) 0.0031(18) -0.0006(14) C8 0.010(2) 0.031(2) 0.018(2) 0.0046(16) 0.0032(19) -0.0030(15) C9 0.0126(19) 0.0196(16) 0.017(2) 0.0054(14) 0.0019(18) -0.0002(13) C10 0.0128(19) 0.0146(14) 0.0114(17) -0.0018(11) 0.0025(16) 0.0004(12) C11 0.019(2) 0.0207(18) 0.016(2) -0.0044(14) 0.0030(19) 0.0030(14) C12 0.027(3) 0.029(2) 0.015(2) -0.0090(16) 0.002(2) -0.0022(18) C13 0.024(3) 0.040(3) 0.010(2) -0.0013(17) -0.007(2) 0.000(2) C14 0.026(3) 0.037(3) 0.020(2) 0.0057(19) -0.001(2) 0.011(2) C15 0.018(2) 0.0243(19) 0.014(2) -0.0007(14) 0.0012(19) 0.0074(15) C16 0.0084(17) 0.0200(15) 0.0071(16) -0.0013(12) 0.0000(15) -0.0018(12) C17 0.014(2) 0.0186(17) 0.024(2) -0.0058(15) -0.001(2) -0.0018(14) C18 0.018(2) 0.026(2) 0.031(3) -0.0107(18) 0.000(2) -0.0031(17) C19 0.014(2) 0.037(2) 0.012(2) -0.0047(16) -0.003(2) 0.0003(17) C20 0.014(2) 0.028(2) 0.017(2) 0.0049(15) -0.001(2) -0.0025(15) C21 0.015(2) 0.0209(17) 0.0135(19) 0.0044(14) -0.0009(18) -0.0029(14) C22 0.0103(18) 0.0164(15) 0.0120(18) 0.0024(12) 0.0008(16) -0.0022(12) C23 0.0104(19) 0.0281(19) 0.016(2) 0.0061(15) 0.0042(18) 0.0032(14) C24 0.013(2) 0.031(2) 0.021(2) 0.0050(17) 0.008(2) 0.0043(16) C25 0.015(2) 0.033(2) 0.017(2) 0.0041(17) 0.007(2) 0.0003(16) C26 0.017(2) 0.033(2) 0.012(2) 0.0030(16) 0.001(2) 0.0013(17) C27 0.011(2) 0.0272(19) 0.016(2) 0.0025(15) 0.0024(19) 0.0019(14) C28 0.014(2) 0.0154(15) 0.017(2) -0.0012(13) 0.0048(18) 0.0021(12) C29 0.016(2) 0.0146(15) 0.019(2) 0.0053(13) 0.0018(19) 0.0027(13) C30 0.015(2) 0.0136(14) 0.017(2) 0.0006(12) 0.0025(18) -0.0009(12) C31 0.0089(17) 0.0174(15) 0.0081(16) 0.0029(11) -0.0005(15) 0.0005(12) C32 0.0131(19) 0.0159(15) 0.0144(19) -0.0015(12) -0.0012(18) 0.0013(12) C33 0.021(2) 0.0212(18) 0.015(2) -0.0012(14) -0.004(2) 0.0002(15) C34 0.022(2) 0.0237(19) 0.018(2) 0.0047(15) -0.004(2) -0.0044(16) C35 0.017(2) 0.030(2) 0.022(2) 0.0069(17) 0.000(2) 0.0046(17) C36 0.015(2) 0.030(2) 0.019(2) 0.0054(16) 0.004(2) 0.0077(16) C37 0.0113(18) 0.0175(15) 0.0131(18) 0.0047(12) 0.0046(17) 0.0061(12) C38 0.021(2) 0.0247(19) 0.017(2) 0.0037(15) 0.011(2) 0.0072(16) C39 0.024(3) 0.033(2) 0.017(2) 0.0056(17) 0.012(2) 0.0114(18) C40 0.021(3) 0.044(3) 0.023(3) 0.017(2) 0.014(2) 0.015(2) C41 0.014(2) 0.031(2) 0.030(3) 0.0102(18) 0.009(2) 0.0019(16) C42 0.014(2) 0.0219(18) 0.025(2) 0.0068(15) 0.007(2) 0.0031(14) C43 0.0113(19) 0.0196(16) 0.0122(18) 0.0037(12) 0.0030(17) -0.0024(12) C44 0.015(2) 0.027(2) 0.014(2) 0.0091(15) 0.0000(19) -0.0039(15) C45 0.024(3) 0.046(3) 0.016(2) 0.014(2) 0.003(2) -0.007(2) C46 0.023(3) 0.062(4) 0.010(2) 0.003(2) 0.002(2) -0.011(2) C47 0.026(3) 0.038(3) 0.016(2) -0.0073(18) 0.005(2) -0.009(2) C48 0.019(2) 0.0241(18) 0.0112(19) -0.0002(14) 0.0029(19) -0.0039(15) C49 0.0113(18) 0.0141(14) 0.0138(18) 0.0048(12) 0.0036(17) 0.0000(11) C50 0.013(2) 0.0209(17) 0.024(2) -0.0022(15) 0.005(2) 0.0003(14) C51 0.013(2) 0.026(2) 0.033(3) 0.0030(18) 0.008(2) 0.0035(15) C52 0.009(2) 0.034(2) 0.027(3) 0.0117(19) 0.002(2) 0.0006(16) C53 0.012(2) 0.046(3) 0.014(2) 0.0027(19) -0.004(2) -0.0032(18) C54 0.014(2) 0.037(2) 0.012(2) 0.0023(16) -0.001(2) -0.0011(17) C55 0.0118(18) 0.0171(14) 0.0097(16) 0.0008(12) 0.0027(16) 0.0016(12) C56 0.0121(19) 0.0215(16) 0.0101(18) 0.0015(13) 0.0027(17) 0.0070(13) C57 0.016(2) 0.0161(16) 0.0123(18) 0.0019(12) 0.0032(17) 0.0027(12) C58 0.031(3) 0.0221(19) 0.018(2) -0.0041(16) -0.003(2) 0.0018(18) C59 0.045(4) 0.044(4) 0.069(6) -0.011(4) 0.017(5) -0.015(3) C60 0.0117(18) 0.0189(15) 0.0117(17) 0.0000(13) 0.0017(16) 0.0019(13) C61 0.0093(18) 0.0200(17) 0.0156(19) -0.0034(13) 0.0012(17) 0.0002(12) C62 0.014(2) 0.0179(16) 0.019(2) -0.0019(13) 0.0036(19) -0.0031(13) C63 0.022(2) 0.0188(17) 0.021(2) 0.0026(15) 0.001(2) 0.0005(15) C64 0.036(4) 0.043(3) 0.027(3) 0.003(2) 0.009(3) -0.013(3) Cl1C 0.0641(13) 0.0703(12) 0.0207(7) 0.0041(7) -0.0005(9) 0.0413(10) C1C 0.034(3) 0.039(3) 0.017(2) 0.0078(19) 0.007(3) 0.010(2) Cl2C 0.0894(16) 0.0327(7) 0.0698(14) -0.0027(8) 0.0481(13) -0.0166(8) Cl1A 0.0599(13) 0.0663(12) 0.0352(9) -0.0221(8) -0.0036(10) 0.0223(10) C1A 0.050(5) 0.060(4) 0.035(4) -0.018(3) 0.009(4) 0.008(3) Cl2A 0.0728(14) 0.0322(7) 0.0616(12) 0.0057(7) 0.0332(11) 0.0030(8) Cl1D 0.0755(17) 0.1060(18) 0.0412(11) -0.0285(12) -0.0206(12) 0.0614(15) C1D 0.037(4) 0.040(3) 0.031(3) -0.002(2) 0.012(3) 0.007(2) Cl2D 0.0452(11) 0.0439(9) 0.0975(18) 0.0059(10) 0.0348(12) -0.0106(7) Cl1B 0.0350(8) 0.0379(7) 0.0353(8) 0.0050(6) -0.0025(8) -0.0040(6) C1B 0.028(3) 0.039(3) 0.028(3) 0.012(2) 0.002(3) -0.002(2) Cl2B 0.0281(7) 0.0401(7) 0.0317(7) 0.0009(5) 0.0093(7) -0.0029(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2715(10) . ? Pt1 P1 2.2718(9) . ? Pt1 S1 2.3550(8) . ? Pt1 S2 2.3725(9) . ? Pb1 Cl1 2.5794(11) . ? Pb1 O1 2.625(3) . ? Pb1 Cl3 2.7202(12) . ? Pb1 Cl2 2.8125(11) . ? S1 C55 1.842(5) . ? S1 Pt2 2.3707(8) . ? P1 C1 1.814(4) . ? P1 C4 1.814(4) . ? P1 C10 1.818(5) . ? N1 C57 1.354(6) . ? N1 C56 1.454(6) . ? O1 C57 1.257(5) . ? C1 C2 1.533(6) . ? P2 C16 1.820(5) . ? P2 C22 1.821(4) . ? P2 C3 1.821(4) . ? Pt2 P4 2.2646(9) . ? Pt2 P3 2.2756(10) . ? Pt2 S2 2.3592(9) . ? Pb2 O2 2.545(3) . ? Pb2 Cl4 2.6044(11) . ? Pb2 Cl6 2.6667(14) . ? Pb2 Cl5 2.8132(11) . ? S2 C60 1.842(5) . ? O2 C62 1.252(5) . ? N2 C57 1.342(6) . ? N2 C58 1.454(6) . ? C2 C3 1.536(5) . ? P3 C28 1.810(4) . ? P3 C31 1.812(5) . ? P3 C37 1.816(4) . ? N3 C62 1.370(6) . ? N3 C61 1.457(6) . ? P4 C43 1.812(5) . ? P4 C30 1.822(4) . ? P4 C49 1.825(5) . ? N4 C62 1.339(7) . ? N4 C63 1.448(6) . ? C4 C5 1.404(6) . ? C4 C9 1.408(5) . ? C5 C6 1.393(6) . ? C6 C7 1.389(6) . ? C7 C8 1.381(7) . ? C8 C9 1.395(6) . ? C10 C15 1.395(6) . ? C10 C11 1.402(5) . ? C11 C12 1.384(7) . ? C12 C13 1.383(8) . ? C13 C14 1.409(7) . ? C14 C15 1.376(8) . ? C16 C21 1.393(6) . ? C16 C17 1.405(6) . ? C17 C18 1.387(8) . ? C18 C19 1.386(8) . ? C19 C20 1.396(7) . ? C20 C21 1.387(7) . ? C22 C27 1.386(7) . ? C22 C23 1.396(6) . ? C23 C24 1.387(6) . ? C24 C25 1.382(7) . ? C25 C26 1.388(7) . ? C26 C27 1.393(6) . ? C28 C29 1.534(5) . ? C29 C30 1.530(7) . ? C31 C32 1.402(5) . ? C31 C36 1.409(6) . ? C32 C33 1.387(7) . ? C33 C34 1.399(7) . ? C34 C35 1.387(7) . ? C35 C36 1.384(8) . ? C37 C38 1.401(6) . ? C37 C42 1.405(6) . ? C38 C39 1.399(6) . ? C39 C40 1.389(8) . ? C40 C41 1.380(8) . ? C41 C42 1.396(6) . ? C43 C48 1.393(6) . ? C43 C44 1.404(6) . ? C44 C45 1.386(7) . ? C45 C46 1.386(9) . ? C46 C47 1.390(8) . ? C47 C48 1.391(7) . ? C49 C54 1.396(7) . ? C49 C50 1.397(5) . ? C50 C51 1.391(7) . ? C51 C52 1.379(8) . ? C52 C53 1.395(7) . ? C53 C54 1.395(7) . ? C55 C56 1.529(5) . ? C58 C59 1.527(9) . ? C60 C61 1.527(6) . ? C63 C64 1.520(7) . ? Cl1C C1C 1.752(6) . ? C1C Cl2C 1.771(7) . ? Cl1A C1A 1.751(9) . ? C1A Cl2A 1.772(7) . ? Cl1D C1D 1.764(7) . ? C1D Cl2D 1.772(7) . ? Cl1B C1B 1.753(7) . ? C1B Cl2B 1.774(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 93.92(3) . . ? P2 Pt1 S1 89.88(3) . . ? P1 Pt1 S1 173.01(3) . . ? P2 Pt1 S2 173.83(3) . . ? P1 Pt1 S2 92.21(3) . . ? S1 Pt1 S2 83.95(3) . . ? Cl1 Pb1 O1 88.92(8) . . ? Cl1 Pb1 Cl3 93.80(4) . . ? O1 Pb1 Cl3 84.12(8) . . ? Cl1 Pb1 Cl2 86.62(4) . . ? O1 Pb1 Cl2 173.81(8) . . ? Cl3 Pb1 Cl2 91.89(4) . . ? C55 S1 Pt1 108.49(12) . . ? C55 S1 Pt2 104.54(13) . . ? Pt1 S1 Pt2 87.94(3) . . ? C1 P1 C4 104.14(18) . . ? C1 P1 C10 104.6(2) . . ? C4 P1 C10 104.27(18) . . ? C1 P1 Pt1 114.84(12) . . ? C4 P1 Pt1 114.95(12) . . ? C10 P1 Pt1 112.88(13) . . ? C57 N1 C56 121.7(4) . . ? C57 O1 Pb1 129.0(3) . . ? C2 C1 P1 113.4(3) . . ? C16 P2 C22 104.28(19) . . ? C16 P2 C3 106.6(2) . . ? C22 P2 C3 103.77(18) . . ? C16 P2 Pt1 113.22(13) . . ? C22 P2 Pt1 114.67(14) . . ? C3 P2 Pt1 113.38(14) . . ? P4 Pt2 P3 93.48(4) . . ? P4 Pt2 S2 90.38(3) . . ? P3 Pt2 S2 170.12(4) . . ? P4 Pt2 S1 174.21(4) . . ? P3 Pt2 S1 92.31(3) . . ? S2 Pt2 S1 83.90(3) . . ? O2 Pb2 Cl4 90.52(8) . . ? O2 Pb2 Cl6 85.33(9) . . ? Cl4 Pb2 Cl6 95.22(5) . . ? O2 Pb2 Cl5 174.10(10) . . ? Cl4 Pb2 Cl5 87.62(3) . . ? Cl6 Pb2 Cl5 89.26(4) . . ? C60 S2 Pt2 110.30(12) . . ? C60 S2 Pt1 104.84(13) . . ? Pt2 S2 Pt1 87.80(3) . . ? C62 O2 Pb2 136.0(3) . . ? C57 N2 C58 126.2(4) . . ? C1 C2 C3 113.5(4) . . ? C28 P3 C31 103.9(2) . . ? C28 P3 C37 104.24(18) . . ? C31 P3 C37 104.1(2) . . ? C28 P3 Pt2 115.60(15) . . ? C31 P3 Pt2 112.50(13) . . ? C37 P3 Pt2 115.16(14) . . ? C62 N3 C61 119.3(4) . . ? C2 C3 P2 114.1(3) . . ? C43 P4 C30 106.5(2) . . ? C43 P4 C49 102.32(19) . . ? C30 P4 C49 103.6(2) . . ? C43 P4 Pt2 113.89(13) . . ? C30 P4 Pt2 113.16(13) . . ? C49 P4 Pt2 116.19(12) . . ? C62 N4 C63 126.7(4) . . ? C5 C4 C9 119.3(4) . . ? C5 C4 P1 120.5(3) . . ? C9 C4 P1 120.1(3) . . ? C6 C5 C4 120.0(4) . . ? C7 C6 C5 120.0(4) . . ? C8 C7 C6 120.7(4) . . ? C7 C8 C9 120.2(4) . . ? C8 C9 C4 119.8(4) . . ? C15 C10 C11 118.5(4) . . ? C15 C10 P1 120.8(3) . . ? C11 C10 P1 120.7(3) . . ? C12 C11 C10 120.9(4) . . ? C13 C12 C11 120.3(4) . . ? C12 C13 C14 119.2(5) . . ? C15 C14 C13 120.3(5) . . ? C14 C15 C10 120.8(4) . . ? C21 C16 C17 118.6(4) . . ? C21 C16 P2 119.6(3) . . ? C17 C16 P2 121.8(3) . . ? C18 C17 C16 120.1(4) . . ? C19 C18 C17 120.8(5) . . ? C18 C19 C20 119.6(5) . . ? C21 C20 C19 119.6(5) . . ? C20 C21 C16 121.3(4) . . ? C27 C22 C23 119.2(4) . . ? C27 C22 P2 119.3(3) . . ? C23 C22 P2 121.5(3) . . ? C24 C23 C22 120.4(5) . . ? C25 C24 C23 119.9(4) . . ? C24 C25 C26 120.4(4) . . ? C25 C26 C27 119.6(5) . . ? C22 C27 C26 120.5(4) . . ? C29 C28 P3 114.9(3) . . ? C30 C29 C28 113.5(4) . . ? C29 C30 P4 114.0(3) . . ? C32 C31 C36 118.4(4) . . ? C32 C31 P3 121.5(3) . . ? C36 C31 P3 120.1(3) . . ? C33 C32 C31 121.0(4) . . ? C32 C33 C34 119.7(4) . . ? C35 C34 C33 119.9(5) . . ? C36 C35 C34 120.5(5) . . ? C35 C36 C31 120.4(4) . . ? C38 C37 C42 120.1(4) . . ? C38 C37 P3 120.4(3) . . ? C42 C37 P3 119.4(3) . . ? C39 C38 C37 119.1(5) . . ? C40 C39 C38 120.7(5) . . ? C41 C40 C39 119.9(4) . . ? C40 C41 C42 120.7(5) . . ? C41 C42 C37 119.4(5) . . ? C48 C43 C44 118.7(4) . . ? C48 C43 P4 119.6(3) . . ? C44 C43 P4 121.5(3) . . ? C45 C44 C43 120.4(5) . . ? C44 C45 C46 120.1(5) . . ? C45 C46 C47 120.4(5) . . ? C46 C47 C48 119.4(5) . . ? C47 C48 C43 121.0(4) . . ? C54 C49 C50 119.3(4) . . ? C54 C49 P4 119.4(3) . . ? C50 C49 P4 121.3(4) . . ? C51 C50 C49 120.1(5) . . ? C52 C51 C50 120.3(4) . . ? C51 C52 C53 120.2(5) . . ? C54 C53 C52 119.7(5) . . ? C53 C54 C49 120.2(4) . . ? C56 C55 S1 108.6(3) . . ? N1 C56 C55 110.5(4) . . ? O1 C57 N2 121.4(4) . . ? O1 C57 N1 120.4(4) . . ? N2 C57 N1 118.2(4) . . ? N2 C58 C59 111.8(5) . . ? C61 C60 S2 109.0(3) . . ? N3 C61 C60 111.3(3) . . ? O2 C62 N4 122.2(4) . . ? O2 C62 N3 119.5(5) . . ? N4 C62 N3 118.2(4) . . ? N4 C63 C64 112.7(5) . . ? Cl1C C1C Cl2C 112.0(3) . . ? Cl1A C1A Cl2A 113.2(4) . . ? Cl1D C1D Cl2D 112.5(3) . . ? Cl1B C1B Cl2B 112.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 S1 C55 105.34(13) . . . . ? P1 Pt1 S1 C55 -131.7(3) . . . . ? S2 Pt1 S1 C55 -74.76(13) . . . . ? P2 Pt1 S1 Pt2 -150.01(4) . . . . ? P1 Pt1 S1 Pt2 -27.0(3) . . . . ? S2 Pt1 S1 Pt2 29.89(3) . . . . ? P2 Pt1 P1 C1 -35.65(18) . . . . ? S1 Pt1 P1 C1 -158.4(3) . . . . ? S2 Pt1 P1 C1 145.08(18) . . . . ? P2 Pt1 P1 C4 -156.46(15) . . . . ? S1 Pt1 P1 C4 80.8(4) . . . . ? S2 Pt1 P1 C4 24.27(15) . . . . ? P2 Pt1 P1 C10 84.10(14) . . . . ? S1 Pt1 P1 C10 -38.7(4) . . . . ? S2 Pt1 P1 C10 -95.16(14) . . . . ? Cl1 Pb1 O1 C57 144.4(3) . . . . ? Cl3 Pb1 O1 C57 50.5(3) . . . . ? Cl2 Pb1 O1 C57 100.6(8) . . . . ? C4 P1 C1 C2 -177.4(3) . . . . ? C10 P1 C1 C2 -68.3(3) . . . . ? Pt1 P1 C1 C2 56.0(3) . . . . ? P1 Pt1 P2 C16 -85.81(13) . . . . ? S1 Pt1 P2 C16 88.31(13) . . . . ? S2 Pt1 P2 C16 87.4(4) . . . . ? P1 Pt1 P2 C22 154.68(16) . . . . ? S1 Pt1 P2 C22 -31.19(16) . . . . ? S2 Pt1 P2 C22 -32.1(4) . . . . ? P1 Pt1 P2 C3 35.74(17) . . . . ? S1 Pt1 P2 C3 -150.13(17) . . . . ? S2 Pt1 P2 C3 -151.1(4) . . . . ? C55 S1 Pt2 P4 69.7(4) . . . . ? Pt1 S1 Pt2 P4 -38.8(4) . . . . ? C55 S1 Pt2 P3 -110.65(13) . . . . ? Pt1 S1 Pt2 P3 140.78(4) . . . . ? C55 S1 Pt2 S2 78.49(13) . . . . ? Pt1 S1 Pt2 S2 -30.07(3) . . . . ? P4 Pt2 S2 C60 103.94(14) . . . . ? P3 Pt2 S2 C60 -143.0(2) . . . . ? S1 Pt2 S2 C60 -75.18(14) . . . . ? P4 Pt2 S2 Pt1 -151.05(4) . . . . ? P3 Pt2 S2 Pt1 -38.0(2) . . . . ? S1 Pt2 S2 Pt1 29.83(3) . . . . ? P2 Pt1 S2 C60 81.3(4) . . . . ? P1 Pt1 S2 C60 -105.48(13) . . . . ? S1 Pt1 S2 C60 80.38(13) . . . . ? P2 Pt1 S2 Pt2 -29.1(4) . . . . ? P1 Pt1 S2 Pt2 144.09(4) . . . . ? S1 Pt1 S2 Pt2 -30.05(3) . . . . ? Cl4 Pb2 O2 C62 130.6(5) . . . . ? Cl6 Pb2 O2 C62 35.4(5) . . . . ? Cl5 Pb2 O2 C62 59.1(10) . . . . ? P1 C1 C2 C3 -74.2(4) . . . . ? P4 Pt2 P3 C28 -34.58(17) . . . . ? S2 Pt2 P3 C28 -147.4(2) . . . . ? S1 Pt2 P3 C28 145.45(16) . . . . ? P4 Pt2 P3 C31 84.59(13) . . . . ? S2 Pt2 P3 C31 -28.2(2) . . . . ? S1 Pt2 P3 C31 -95.37(13) . . . . ? P4 Pt2 P3 C37 -156.35(18) . . . . ? S2 Pt2 P3 C37 90.8(3) . . . . ? S1 Pt2 P3 C37 23.69(18) . . . . ? C1 C2 C3 P2 75.8(4) . . . . ? C16 P2 C3 C2 67.6(4) . . . . ? C22 P2 C3 C2 177.4(3) . . . . ? Pt1 P2 C3 C2 -57.6(4) . . . . ? P3 Pt2 P4 C43 -84.80(16) . . . . ? S2 Pt2 P4 C43 86.10(16) . . . . ? S1 Pt2 P4 C43 94.8(4) . . . . ? P3 Pt2 P4 C30 36.97(19) . . . . ? S2 Pt2 P4 C30 -152.13(18) . . . . ? S1 Pt2 P4 C30 -143.4(4) . . . . ? P3 Pt2 P4 C49 156.65(15) . . . . ? S2 Pt2 P4 C49 -32.45(15) . . . . ? S1 Pt2 P4 C49 -23.7(4) . . . . ? C1 P1 C4 C5 -41.5(4) . . . . ? C10 P1 C4 C5 -150.8(3) . . . . ? Pt1 P1 C4 C5 85.0(3) . . . . ? C1 P1 C4 C9 141.1(3) . . . . ? C10 P1 C4 C9 31.7(4) . . . . ? Pt1 P1 C4 C9 -92.4(3) . . . . ? C9 C4 C5 C6 -2.3(6) . . . . ? P1 C4 C5 C6 -179.7(3) . . . . ? C4 C5 C6 C7 1.5(6) . . . . ? C5 C6 C7 C8 0.2(6) . . . . ? C6 C7 C8 C9 -1.2(7) . . . . ? C7 C8 C9 C4 0.3(7) . . . . ? C5 C4 C9 C8 1.4(6) . . . . ? P1 C4 C9 C8 178.8(3) . . . . ? C1 P1 C10 C15 128.5(4) . . . . ? C4 P1 C10 C15 -122.4(4) . . . . ? Pt1 P1 C10 C15 3.0(4) . . . . ? C1 P1 C10 C11 -50.6(4) . . . . ? C4 P1 C10 C11 58.5(4) . . . . ? Pt1 P1 C10 C11 -176.1(3) . . . . ? C15 C10 C11 C12 0.7(7) . . . . ? P1 C10 C11 C12 179.8(4) . . . . ? C10 C11 C12 C13 -0.7(7) . . . . ? C11 C12 C13 C14 0.9(8) . . . . ? C12 C13 C14 C15 -1.0(9) . . . . ? C13 C14 C15 C10 0.9(8) . . . . ? C11 C10 C15 C14 -0.8(7) . . . . ? P1 C10 C15 C14 -179.9(4) . . . . ? C22 P2 C16 C21 92.2(3) . . . . ? C3 P2 C16 C21 -158.4(3) . . . . ? Pt1 P2 C16 C21 -33.1(3) . . . . ? C22 P2 C16 C17 -85.7(3) . . . . ? C3 P2 C16 C17 23.7(4) . . . . ? Pt1 P2 C16 C17 149.0(3) . . . . ? C21 C16 C17 C18 1.0(6) . . . . ? P2 C16 C17 C18 179.0(3) . . . . ? C16 C17 C18 C19 -1.2(7) . . . . ? C17 C18 C19 C20 0.1(7) . . . . ? C18 C19 C20 C21 1.2(7) . . . . ? C19 C20 C21 C16 -1.5(6) . . . . ? C17 C16 C21 C20 0.4(6) . . . . ? P2 C16 C21 C20 -177.6(3) . . . . ? C16 P2 C22 C27 163.4(3) . . . . ? C3 P2 C22 C27 52.0(4) . . . . ? Pt1 P2 C22 C27 -72.3(4) . . . . ? C16 P2 C22 C23 -16.3(4) . . . . ? C3 P2 C22 C23 -127.7(4) . . . . ? Pt1 P2 C22 C23 108.1(4) . . . . ? C27 C22 C23 C24 -1.7(7) . . . . ? P2 C22 C23 C24 177.9(4) . . . . ? C22 C23 C24 C25 0.3(7) . . . . ? C23 C24 C25 C26 1.0(8) . . . . ? C24 C25 C26 C27 -1.0(8) . . . . ? C23 C22 C27 C26 1.8(7) . . . . ? P2 C22 C27 C26 -177.9(4) . . . . ? C25 C26 C27 C22 -0.4(7) . . . . ? C31 P3 C28 C29 -70.8(4) . . . . ? C37 P3 C28 C29 -179.5(4) . . . . ? Pt2 P3 C28 C29 53.0(4) . . . . ? P3 C28 C29 C30 -71.2(5) . . . . ? C28 C29 C30 P4 75.7(4) . . . . ? C43 P4 C30 C29 65.6(3) . . . . ? C49 P4 C30 C29 173.0(3) . . . . ? Pt2 P4 C30 C29 -60.3(3) . . . . ? C28 P3 C31 C32 120.8(3) . . . . ? C37 P3 C31 C32 -130.3(3) . . . . ? Pt2 P3 C31 C32 -4.9(4) . . . . ? C28 P3 C31 C36 -58.4(4) . . . . ? C37 P3 C31 C36 50.5(4) . . . . ? Pt2 P3 C31 C36 175.8(3) . . . . ? C36 C31 C32 C33 0.4(6) . . . . ? P3 C31 C32 C33 -178.9(3) . . . . ? C31 C32 C33 C34 -1.7(6) . . . . ? C32 C33 C34 C35 2.0(7) . . . . ? C33 C34 C35 C36 -0.9(7) . . . . ? C34 C35 C36 C31 -0.4(7) . . . . ? C32 C31 C36 C35 0.7(6) . . . . ? P3 C31 C36 C35 180.0(4) . . . . ? C28 P3 C37 C38 -30.7(4) . . . . ? C31 P3 C37 C38 -139.4(4) . . . . ? Pt2 P3 C37 C38 97.0(4) . . . . ? C28 P3 C37 C42 152.2(4) . . . . ? C31 P3 C37 C42 43.6(4) . . . . ? Pt2 P3 C37 C42 -80.1(4) . . . . ? C42 C37 C38 C39 -2.5(7) . . . . ? P3 C37 C38 C39 -179.5(4) . . . . ? C37 C38 C39 C40 2.3(7) . . . . ? C38 C39 C40 C41 -0.5(8) . . . . ? C39 C40 C41 C42 -1.2(8) . . . . ? C40 C41 C42 C37 1.0(8) . . . . ? C38 C37 C42 C41 0.8(7) . . . . ? P3 C37 C42 C41 177.9(4) . . . . ? C30 P4 C43 C48 -164.7(4) . . . . ? C49 P4 C43 C48 87.0(4) . . . . ? Pt2 P4 C43 C48 -39.3(4) . . . . ? C30 P4 C43 C44 20.1(4) . . . . ? C49 P4 C43 C44 -88.3(4) . . . . ? Pt2 P4 C43 C44 145.5(3) . . . . ? C48 C43 C44 C45 -0.5(7) . . . . ? P4 C43 C44 C45 174.9(4) . . . . ? C43 C44 C45 C46 -0.9(8) . . . . ? C44 C45 C46 C47 1.5(9) . . . . ? C45 C46 C47 C48 -0.8(9) . . . . ? C46 C47 C48 C43 -0.6(8) . . . . ? C44 C43 C48 C47 1.2(7) . . . . ? P4 C43 C48 C47 -174.2(4) . . . . ? C43 P4 C49 C54 152.8(3) . . . . ? C30 P4 C49 C54 42.3(4) . . . . ? Pt2 P4 C49 C54 -82.5(3) . . . . ? C43 P4 C49 C50 -25.2(4) . . . . ? C30 P4 C49 C50 -135.8(3) . . . . ? Pt2 P4 C49 C50 99.5(3) . . . . ? C54 C49 C50 C51 -2.8(6) . . . . ? P4 C49 C50 C51 175.3(3) . . . . ? C49 C50 C51 C52 -0.2(7) . . . . ? C50 C51 C52 C53 2.3(7) . . . . ? C51 C52 C53 C54 -1.4(8) . . . . ? C52 C53 C54 C49 -1.6(8) . . . . ? C50 C49 C54 C53 3.7(7) . . . . ? P4 C49 C54 C53 -174.4(4) . . . . ? Pt1 S1 C55 C56 -150.8(2) . . . . ? Pt2 S1 C55 C56 116.4(3) . . . . ? C57 N1 C56 C55 -78.1(5) . . . . ? S1 C55 C56 N1 -168.5(3) . . . . ? Pb1 O1 C57 N2 -49.1(5) . . . . ? Pb1 O1 C57 N1 133.0(4) . . . . ? C58 N2 C57 O1 169.8(5) . . . . ? C58 N2 C57 N1 -12.3(7) . . . . ? C56 N1 C57 O1 0.4(6) . . . . ? C56 N1 C57 N2 -177.6(4) . . . . ? C57 N2 C58 C59 -74.4(8) . . . . ? Pt2 S2 C60 C61 -139.7(2) . . . . ? Pt1 S2 C60 C61 127.1(3) . . . . ? C62 N3 C61 C60 -77.3(5) . . . . ? S2 C60 C61 N3 -165.8(3) . . . . ? Pb2 O2 C62 N4 -36.7(7) . . . . ? Pb2 O2 C62 N3 146.8(3) . . . . ? C63 N4 C62 O2 171.2(4) . . . . ? C63 N4 C62 N3 -12.3(7) . . . . ? C61 N3 C62 O2 -9.0(6) . . . . ? C61 N3 C62 N4 174.4(4) . . . . ? C62 N4 C63 C64 -76.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 39.60 _diffrn_measured_fraction_theta_full 0.839 _refine_diff_density_max 4.462 _refine_diff_density_min -5.001 _refine_diff_density_rms 0.240 # Attachment 'cm100p-1b.cif' data_cm100p-1 _database_code_depnum_ccdc_archive 'CCDC 714217' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H86 F6 N4 O8 P4 Pt2 S4' _chemical_formula_weight 2023.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _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 12.5627(12) _cell_length_b 13.2661(13) _cell_length_c 14.3997(16) _cell_angle_alpha 64.734(5) _cell_angle_beta 79.444(5) _cell_angle_gamma 71.700(5) _cell_volume 2057.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7052 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 36.10 _exptl_crystal_description BLOCK _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 3.647 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4542 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41557 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.1114 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 36.46 _reflns_number_total 16989 _reflns_number_gt 12532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1465P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16989 _refine_ls_number_parameters 533 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.2187 _refine_ls_wR_factor_gt 0.1943 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.019 _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 C1 C 0.6123(4) 0.5958(5) 0.6999(6) 0.0198(12) Uani 1 1 d . . . P1 P 0.46073(10) 0.62227(12) 0.69919(13) 0.0141(3) Uani 1 1 d . . . Pt1 Pt 0.426350(13) 0.533184(15) 0.607273(17) 0.01317(7) Uani 1 1 d . . . S1 S 0.40756(9) 0.44460(10) 0.49943(11) 0.0106(2) Uani 1 1 d . . . C2 C 0.6674(5) 0.6815(6) 0.6485(7) 0.0335(18) Uani 1 1 d . . . H2 H 0.6261 0.7595 0.6149 0.040 Uiso 1 1 calc R . . O2 O 0.7874(4) -0.0016(5) 0.7039(5) 0.0323(12) Uani 1 1 d . . . P2 P 0.26025(10) 0.51508(12) 0.69752(13) 0.0129(3) Uani 1 1 d . . . C3 C 0.7838(6) 0.6525(9) 0.6466(10) 0.051(3) Uani 1 1 d . . . H3 H 0.8216 0.7116 0.6125 0.061 Uiso 1 1 calc R . . N1 N 0.6452(4) 0.0878(5) 0.7874(6) 0.0267(13) Uani 1 1 d . . . H3B H 0.6257 0.1061 0.8412 0.032 Uiso 1 1 calc R . . C4 C 0.8452(6) 0.5397(9) 0.6930(10) 0.055(3) Uani 1 1 d . . . H4 H 0.9248 0.5207 0.6909 0.066 Uiso 1 1 calc R . . N2 N 0.8175(5) 0.0091(7) 0.8510(7) 0.0405(18) Uani 1 1 d . . . H4B H 0.7827 0.0313 0.9007 0.049 Uiso 1 1 calc R . . C5 C 0.7898(6) 0.4552(7) 0.7424(9) 0.048(3) Uani 1 1 d . . . H5 H 0.8319 0.3770 0.7738 0.058 Uiso 1 1 calc R . . C6 C 0.6741(5) 0.4813(6) 0.7474(7) 0.0302(16) Uani 1 1 d . . . H6 H 0.6369 0.4218 0.7829 0.036 Uiso 1 1 calc R . . C7 C 0.4030(4) 0.7777(5) 0.6482(5) 0.0154(10) Uani 1 1 d . . . C8 C 0.4212(5) 0.8409(5) 0.6994(6) 0.0247(14) Uani 1 1 d . . . H8 H 0.4618 0.8022 0.7600 0.030 Uiso 1 1 calc R . . C9 C 0.3785(6) 0.9610(6) 0.6592(7) 0.0302(17) Uani 1 1 d . . . H9 H 0.3907 1.0046 0.6923 0.036 Uiso 1 1 calc R . . C10 C 0.3182(5) 1.0170(5) 0.5711(6) 0.0247(14) Uani 1 1 d . . . H10 H 0.2900 1.0987 0.5442 0.030 Uiso 1 1 calc R . . C11 C 0.2984(5) 0.9545(5) 0.5212(6) 0.0229(13) Uani 1 1 d . . . H11 H 0.2571 0.9932 0.4610 0.027 Uiso 1 1 calc R . . C12 C 0.3403(4) 0.8350(5) 0.5615(5) 0.0171(11) Uani 1 1 d . . . H12 H 0.3258 0.7918 0.5292 0.021 Uiso 1 1 calc R . . C13 C 0.4128(5) 0.5728(5) 0.8333(5) 0.0203(12) Uani 1 1 d . . . H13A H 0.4495 0.4896 0.8697 0.024 Uiso 1 1 calc R . . H13B H 0.4310 0.6165 0.8666 0.024 Uiso 1 1 calc R . . C14 C 0.2819(4) 0.5936(4) 0.8370(5) 0.0101(8) Uani 1 1 d U . . H14C H 0.2489 0.6003 0.9027 0.012 Uiso 1 1 calc R . . H14D H 0.2506 0.6682 0.7805 0.012 Uiso 1 1 calc R . . C15 C 0.2474(5) 0.5034(5) 0.8278(6) 0.0217(12) Uani 1 1 d . . . H15A H 0.1683 0.5078 0.8543 0.026 Uiso 1 1 calc R . . H15B H 0.2941 0.4270 0.8710 0.026 Uiso 1 1 calc R . . C16 C 0.1533(4) 0.6428(5) 0.6268(5) 0.0169(11) Uani 1 1 d . . . C17 C 0.1598(4) 0.6835(5) 0.5200(5) 0.0198(12) Uani 1 1 d . . . H17 H 0.2174 0.6427 0.4863 0.024 Uiso 1 1 calc R . . C18 C 0.0825(5) 0.7836(5) 0.4620(6) 0.0229(13) Uani 1 1 d . . . H18 H 0.0862 0.8104 0.3892 0.027 Uiso 1 1 calc R . . C19 C -0.0009(5) 0.8442(5) 0.5130(7) 0.0271(15) Uani 1 1 d . . . H19 H -0.0524 0.9139 0.4740 0.033 Uiso 1 1 calc R . . C20 C -0.0087(5) 0.8039(6) 0.6179(7) 0.0265(15) Uani 1 1 d . . . H20 H -0.0668 0.8449 0.6512 0.032 Uiso 1 1 calc R . . C21 C 0.0678(4) 0.7031(5) 0.6769(6) 0.0206(12) Uani 1 1 d . . . H21 H 0.0622 0.6757 0.7498 0.025 Uiso 1 1 calc R . . C22 C 0.2171(4) 0.3912(5) 0.7098(5) 0.0182(11) Uani 1 1 d . . . C23 C 0.1475(5) 0.3992(5) 0.6405(7) 0.0287(17) Uani 1 1 d . . . H23 H 0.1198 0.4715 0.5862 0.034 Uiso 1 1 calc R . . C24 C 0.1184(6) 0.3023(7) 0.6503(9) 0.038(2) Uani 1 1 d . . . H24 H 0.0712 0.3084 0.6026 0.046 Uiso 1 1 calc R . . C25 C 0.1580(6) 0.1969(7) 0.7293(8) 0.038(2) Uani 1 1 d . . . H25 H 0.1369 0.1311 0.7363 0.045 Uiso 1 1 calc R . . C26 C 0.2282(7) 0.1867(6) 0.7984(7) 0.0325(18) Uani 1 1 d . . . H26 H 0.2559 0.1138 0.8521 0.039 Uiso 1 1 calc R . . C27 C 0.2587(6) 0.2842(6) 0.7891(6) 0.0257(14) Uani 1 1 d . . . H27 H 0.3071 0.2775 0.8362 0.031 Uiso 1 1 calc R . . C55 C 0.4421(4) 0.2899(4) 0.5780(5) 0.0151(11) Uani 1 1 d . . . H55A H 0.3743 0.2699 0.6204 0.018 Uiso 1 1 calc R . . H55B H 0.4641 0.2474 0.5323 0.018 Uiso 1 1 calc R . . C56 C 0.5368(4) 0.2504(5) 0.6486(5) 0.0179(11) Uani 1 1 d . . . H56A H 0.6055 0.2679 0.6066 0.022 Uiso 1 1 calc R . . H56B H 0.5159 0.2936 0.6937 0.022 Uiso 1 1 calc R . . C57 C 0.5612(5) 0.1213(5) 0.7148(6) 0.0221(13) Uani 1 1 d . . . H57A H 0.4912 0.1024 0.7528 0.027 Uiso 1 1 calc R . . H57B H 0.5887 0.0774 0.6703 0.027 Uiso 1 1 calc R . . C58 C 0.7524(5) 0.0293(6) 0.7743(6) 0.0242(13) Uani 1 1 d . . . C59 C 0.9336(6) -0.0430(7) 0.8582(7) 0.0343(18) Uani 1 1 d . . . C60 C 1.0056(5) -0.0526(6) 0.7744(7) 0.0281(15) Uani 1 1 d . . . H60 H 0.9765 -0.0246 0.7089 0.034 Uiso 1 1 calc R . . C61 C 1.1197(5) -0.1031(6) 0.7870(7) 0.0300(17) Uani 1 1 d . . . H61 H 1.1681 -0.1094 0.7296 0.036 Uiso 1 1 calc R . . C62 C 1.1645(6) -0.1443(7) 0.8812(8) 0.038(2) Uani 1 1 d . . . H62 H 1.2429 -0.1784 0.8885 0.046 Uiso 1 1 calc R . . C63 C 1.0925(7) -0.1351(10) 0.9660(9) 0.051(3) Uani 1 1 d . . . H63 H 1.1226 -0.1605 1.0306 0.061 Uiso 1 1 calc R . . C64 C 0.9773(8) -0.0888(10) 0.9555(9) 0.052(3) Uani 1 1 d . . . H64 H 0.9282 -0.0881 1.0140 0.062 Uiso 1 1 calc R . . S1S S 0.44469(16) 0.77480(16) 1.02708(18) 0.0315(4) Uani 1 1 d . . . O1S O 0.4249(5) 0.7049(5) 0.9823(6) 0.0394(14) Uani 1 1 d . A . O2S O 0.4902(5) 0.7160(5) 1.1268(5) 0.0376(14) Uani 1 1 d . A . O3S O 0.3617(8) 0.8828(8) 1.0115(9) 0.082(3) Uani 1 1 d . A . C1S C 0.507(4) 0.866(5) 0.951(5) 0.056(4) Uani 0.160(8) 1 d PD A 1 F1S F 0.429(4) 0.932(3) 0.875(3) 0.054(2) Uani 0.160(8) 1 d PD A 1 F2S F 0.493(7) 0.945(6) 0.992(4) 0.124(7) Uani 0.160(8) 1 d PD . 1 F3S F 0.623(4) 0.824(8) 0.962(6) 0.105(5) Uani 0.160(8) 1 d PD A 1 C1S' C 0.5695(13) 0.8211(12) 0.9442(12) 0.056(4) Uani 0.840(8) 1 d P A 2 F1S' F 0.5457(7) 0.8821(6) 0.8497(6) 0.054(2) Uani 0.840(8) 1 d P A 2 F2S' F 0.6014(16) 0.8847(14) 0.9808(9) 0.124(7) Uani 0.840(8) 1 d P A 2 F3S' F 0.6510(6) 0.7284(11) 0.9503(8) 0.105(5) Uani 0.840(8) 1 d P A 2 C5T C 0.9441(13) 0.4631(12) 0.9592(13) 0.034(4) Uani 0.50 1 d PG B -1 C1T C 1.0274(14) 0.4112(12) 1.0294(14) 0.062(7) Uani 0.50 1 d PGDU B -1 H1TA H 1.0540 0.3285 1.0550 0.074 Uiso 0.50 1 d PR B -1 C2T C 1.0656(16) 0.479(2) 1.0611(14) 0.098(16) Uani 0.50 1 d PGD B -1 H2TA H 1.1231 0.4427 1.1096 0.118 Uiso 0.50 1 d PR B -1 C3T C 1.021(2) 0.598(2) 1.0225(18) 0.111(16) Uani 0.50 1 d PGDU B -1 H3TA H 1.0469 0.6442 1.0444 0.134 Uiso 0.50 1 d PR B -1 C4T C 0.937(2) 0.6496(11) 0.9523(18) 0.107(18) Uani 0.50 1 d PG B -1 H4TA H 0.9061 0.7319 0.9257 0.128 Uiso 0.50 1 d PR B -1 C6T C 0.8990(14) 0.5823(12) 0.9207(12) 0.054(7) Uani 0.50 1 d PGD B -1 H6TA H 0.9177 0.4166 0.9374 0.065 Uiso 0.50 1 d PR B -1 C7T C 0.810(4) 0.651(6) 0.854(4) 0.25(4) Uani 0.50 1 d PDU B -1 H7TD H 0.8060 0.6129 0.8096 0.380 Uiso 0.50 1 calc PR B -1 H7TE H 0.8229 0.7271 0.8107 0.380 Uiso 0.50 1 calc PR B -1 H7TF H 0.7385 0.6609 0.8944 0.380 Uiso 0.50 1 calc PR B -1 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 C1 0.0155(19) 0.024(3) 0.020(4) -0.009(2) -0.0042(18) -0.0043(17) P1 0.0130(5) 0.0142(5) 0.0129(8) -0.0027(5) -0.0033(4) -0.0031(4) Pt1 0.00971(8) 0.01294(9) 0.01343(13) -0.00187(7) -0.00043(6) -0.00340(5) S1 0.0086(4) 0.0114(5) 0.0120(7) -0.0041(4) -0.0006(4) -0.0034(3) C2 0.020(2) 0.031(3) 0.044(5) -0.004(3) -0.008(3) -0.011(2) O2 0.023(2) 0.046(3) 0.027(3) -0.018(3) -0.0045(18) -0.0007(19) P2 0.0113(4) 0.0139(5) 0.0122(8) -0.0036(5) 0.0017(4) -0.0050(4) C3 0.019(3) 0.051(5) 0.072(8) -0.005(5) -0.008(3) -0.018(3) N1 0.023(2) 0.025(3) 0.026(4) -0.009(2) -0.008(2) 0.0022(18) C4 0.014(2) 0.063(6) 0.071(8) -0.010(5) -0.010(3) -0.008(3) N2 0.027(3) 0.061(4) 0.037(5) -0.032(4) -0.012(3) 0.008(3) C5 0.018(3) 0.038(4) 0.073(8) -0.010(4) -0.018(3) 0.006(2) C6 0.021(2) 0.023(3) 0.040(5) -0.006(3) -0.012(2) -0.001(2) C7 0.0138(17) 0.015(2) 0.015(3) -0.003(2) -0.0015(16) -0.0048(15) C8 0.028(3) 0.021(3) 0.026(4) -0.010(3) -0.009(2) -0.002(2) C9 0.030(3) 0.019(3) 0.044(5) -0.014(3) -0.009(3) -0.004(2) C10 0.028(3) 0.016(2) 0.026(4) -0.005(2) -0.001(2) -0.0044(19) C11 0.022(2) 0.019(2) 0.019(4) -0.002(2) -0.003(2) 0.0001(18) C12 0.0172(19) 0.018(2) 0.012(3) -0.003(2) -0.0024(17) -0.0028(16) C13 0.021(2) 0.022(2) 0.013(3) -0.001(2) -0.0032(18) -0.0047(18) C14 0.0096(10) 0.0100(10) 0.0117(12) -0.0069(8) 0.0044(8) -0.0029(8) C15 0.021(2) 0.022(3) 0.020(4) -0.007(2) 0.005(2) -0.0095(19) C16 0.0106(16) 0.018(2) 0.021(3) -0.007(2) 0.0021(17) -0.0070(15) C17 0.0140(18) 0.018(2) 0.022(3) -0.003(2) -0.0005(18) -0.0030(16) C18 0.019(2) 0.021(3) 0.022(4) -0.002(2) -0.004(2) -0.0048(18) C19 0.019(2) 0.021(3) 0.037(5) -0.008(3) -0.009(2) -0.0008(19) C20 0.0139(19) 0.024(3) 0.038(5) -0.013(3) -0.003(2) 0.0003(18) C21 0.0162(19) 0.021(2) 0.025(4) -0.011(2) 0.0026(19) -0.0047(17) C22 0.0151(18) 0.021(2) 0.018(3) -0.007(2) 0.0049(18) -0.0087(16) C23 0.017(2) 0.019(2) 0.052(5) -0.014(3) -0.005(2) -0.0050(18) C24 0.023(3) 0.032(3) 0.067(7) -0.023(4) -0.010(3) -0.008(2) C25 0.031(3) 0.030(3) 0.058(7) -0.021(4) 0.010(3) -0.019(3) C26 0.044(4) 0.022(3) 0.029(5) -0.008(3) 0.014(3) -0.017(3) C27 0.032(3) 0.022(3) 0.021(4) -0.006(3) 0.002(2) -0.010(2) C55 0.0115(16) 0.0098(18) 0.021(3) -0.0025(19) -0.0028(16) -0.0034(13) C56 0.0167(19) 0.016(2) 0.015(3) -0.002(2) -0.0006(18) -0.0023(16) C57 0.019(2) 0.017(2) 0.023(4) -0.003(2) -0.003(2) -0.0018(17) C58 0.021(2) 0.026(3) 0.023(4) -0.008(3) -0.007(2) -0.0008(19) C59 0.022(3) 0.045(4) 0.034(5) -0.020(4) -0.011(3) 0.006(3) C60 0.024(2) 0.024(3) 0.032(5) -0.009(3) -0.010(2) 0.000(2) C61 0.021(2) 0.025(3) 0.042(5) -0.014(3) -0.006(3) 0.000(2) C62 0.026(3) 0.046(4) 0.043(6) -0.021(4) -0.014(3) 0.004(3) C63 0.031(3) 0.073(6) 0.046(7) -0.030(5) -0.021(4) 0.009(4) C64 0.037(4) 0.081(7) 0.038(7) -0.035(5) -0.016(4) 0.008(4) S1S 0.0367(8) 0.0279(8) 0.0298(12) -0.0137(8) -0.0147(7) 0.0017(6) O1S 0.050(3) 0.039(3) 0.036(4) -0.017(3) -0.003(3) -0.019(3) O2S 0.051(3) 0.031(3) 0.028(4) -0.001(2) -0.011(2) -0.016(2) O3S 0.084(6) 0.084(6) 0.076(8) -0.059(6) -0.049(5) 0.044(5) C1S 0.060(7) 0.051(7) 0.049(9) 0.011(6) -0.031(6) -0.033(6) F1S 0.089(5) 0.049(4) 0.022(4) 0.009(3) -0.015(3) -0.042(4) F2S 0.218(16) 0.159(12) 0.032(6) 0.024(6) -0.049(8) -0.164(13) F3S 0.035(4) 0.125(9) 0.062(7) 0.029(6) 0.007(4) 0.002(5) C1S' 0.060(7) 0.051(7) 0.049(9) 0.011(6) -0.031(6) -0.033(6) F1S' 0.089(5) 0.049(4) 0.022(4) 0.009(3) -0.015(3) -0.042(4) F2S' 0.218(16) 0.159(12) 0.032(6) 0.024(6) -0.049(8) -0.164(13) F3S' 0.035(4) 0.125(9) 0.062(7) 0.029(6) 0.007(4) 0.002(5) C5T 0.041(9) 0.043(10) 0.021(11) -0.016(9) 0.019(7) -0.022(7) C1T 0.055(9) 0.074(10) 0.047(10) -0.023(8) 0.015(7) -0.016(7) C2T 0.07(2) 0.21(5) 0.04(2) -0.03(3) 0.023(16) -0.10(3) C3T 0.14(3) 0.15(3) 0.11(3) -0.10(3) 0.08(3) -0.12(3) C4T 0.14(3) 0.18(4) 0.09(3) -0.11(3) 0.10(3) -0.12(3) C6T 0.065(15) 0.051(12) 0.029(15) -0.011(10) 0.014(11) -0.010(10) C7T 0.23(5) 0.24(5) 0.23(6) -0.06(4) -0.03(4) -0.04(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 C1 C2 1.382(9) . ? C1 C6 1.394(9) . ? C1 P1 1.825(5) . ? P1 C13 1.806(7) . ? P1 C7 1.811(5) . ? P1 Pt1 2.2805(16) . ? Pt1 P2 2.2705(13) . ? Pt1 S1 2.3719(12) 2_666 ? Pt1 S1 2.3904(14) . ? S1 C55 1.822(5) . ? S1 Pt1 2.3719(12) 2_666 ? C2 C3 1.387(9) . ? O2 C58 1.213(10) . ? P2 C15 1.796(8) . ? P2 C22 1.817(6) . ? P2 C16 1.819(6) . ? C3 C4 1.375(13) . ? N1 C58 1.351(8) . ? N1 C57 1.455(9) . ? C4 C5 1.369(13) . ? N2 C58 1.379(10) . ? N2 C59 1.406(9) . ? C5 C6 1.381(9) . ? C7 C12 1.389(9) . ? C7 C8 1.418(9) . ? C8 C9 1.397(9) . ? C9 C10 1.389(11) . ? C10 C11 1.402(11) . ? C11 C12 1.389(8) . ? C13 C14 1.574(7) . ? C14 C15 1.456(8) . ? C16 C17 1.391(10) . ? C16 C21 1.409(8) . ? C17 C18 1.395(8) . ? C18 C19 1.405(10) . ? C19 C20 1.367(12) . ? C20 C21 1.399(9) . ? C22 C23 1.394(10) . ? C22 C27 1.400(10) . ? C23 C24 1.389(9) . ? C24 C25 1.382(13) . ? C25 C26 1.385(14) . ? C26 C27 1.408(10) . ? C55 C56 1.523(8) . ? C56 C57 1.523(8) . ? C59 C60 1.396(12) . ? C59 C64 1.407(13) . ? C60 C61 1.388(9) . ? C61 C62 1.381(12) . ? C62 C63 1.406(14) . ? C63 C64 1.392(11) . ? S1S O1S 1.432(7) . ? S1S O2S 1.436(7) . ? S1S O3S 1.437(7) . ? S1S C1S 1.56(6) . ? S1S C1S' 1.885(15) . ? O3S C1S 1.86(6) . ? C1S F2S 1.37(5) . ? C1S F1S 1.40(4) . ? C1S F3S 1.40(4) . ? F2S F2S 1.62(10) 2_677 ? C1S' F1S' 1.285(15) . ? C1S' F3S' 1.31(2) . ? C1S' F2S' 1.349(18) . ? C5T C1T 1.3900 . ? C5T C6T 1.3900 . ? C1T C2T 1.3900 . ? C2T C3T 1.3900 . ? C3T C4T 1.3900 . ? C4T C6T 1.3900 . ? C6T C7T 1.42(4) . ? 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 C2 C1 C6 119.7(5) . . ? C2 C1 P1 123.0(5) . . ? C6 C1 P1 117.0(5) . . ? C13 P1 C7 105.0(3) . . ? C13 P1 C1 104.8(3) . . ? C7 P1 C1 106.5(3) . . ? C13 P1 Pt1 116.2(2) . . ? C7 P1 Pt1 114.6(2) . . ? C1 P1 Pt1 108.9(2) . . ? P2 Pt1 P1 91.72(6) . . ? P2 Pt1 S1 175.20(5) . 2_666 ? P1 Pt1 S1 92.06(5) . 2_666 ? P2 Pt1 S1 94.34(5) . . ? P1 Pt1 S1 173.89(5) . . ? S1 Pt1 S1 81.85(4) 2_666 . ? C55 S1 Pt1 102.62(17) . 2_666 ? C55 S1 Pt1 105.5(2) . . ? Pt1 S1 Pt1 98.15(4) 2_666 . ? C1 C2 C3 119.4(7) . . ? C15 P2 C22 103.0(3) . . ? C15 P2 C16 107.5(3) . . ? C22 P2 C16 106.3(3) . . ? C15 P2 Pt1 117.66(19) . . ? C22 P2 Pt1 115.07(18) . . ? C16 P2 Pt1 106.57(18) . . ? C4 C3 C2 121.1(8) . . ? C58 N1 C57 121.8(7) . . ? C5 C4 C3 119.0(6) . . ? C58 N2 C59 127.0(7) . . ? C4 C5 C6 121.3(7) . . ? C5 C6 C1 119.4(7) . . ? C12 C7 C8 119.8(5) . . ? C12 C7 P1 121.4(5) . . ? C8 C7 P1 118.8(5) . . ? C9 C8 C7 119.0(7) . . ? C10 C9 C8 120.2(7) . . ? C9 C10 C11 121.0(6) . . ? C12 C11 C10 118.8(7) . . ? C11 C12 C7 121.2(6) . . ? C14 C13 P1 106.9(4) . . ? C15 C14 C13 114.4(4) . . ? C14 C15 P2 112.6(4) . . ? C17 C16 C21 119.7(5) . . ? C17 C16 P2 118.4(4) . . ? C21 C16 P2 121.8(5) . . ? C16 C17 C18 120.7(6) . . ? C17 C18 C19 119.0(7) . . ? C20 C19 C18 120.7(6) . . ? C19 C20 C21 120.8(6) . . ? C20 C21 C16 119.2(7) . . ? C23 C22 C27 119.5(6) . . ? C23 C22 P2 121.8(5) . . ? C27 C22 P2 118.6(5) . . ? C24 C23 C22 120.4(7) . . ? C25 C24 C23 120.2(8) . . ? C24 C25 C26 120.3(7) . . ? C25 C26 C27 120.1(8) . . ? C22 C27 C26 119.4(7) . . ? C56 C55 S1 113.1(4) . . ? C57 C56 C55 111.5(5) . . ? N1 C57 C56 110.3(5) . . ? O2 C58 N1 124.3(7) . . ? O2 C58 N2 123.9(6) . . ? N1 C58 N2 111.7(7) . . ? C60 C59 N2 123.1(8) . . ? C60 C59 C64 119.4(7) . . ? N2 C59 C64 117.5(8) . . ? C61 C60 C59 119.8(8) . . ? C62 C61 C60 121.4(8) . . ? C61 C62 C63 119.1(7) . . ? C64 C63 C62 120.2(9) . . ? C63 C64 C59 119.9(9) . . ? O1S S1S O2S 117.1(4) . . ? O1S S1S O3S 116.1(5) . . ? O2S S1S O3S 114.9(5) . . ? O1S S1S C1S 113(2) . . ? O2S S1S C1S 112.3(18) . . ? O3S S1S C1S 77(2) . . ? O1S S1S C1S' 101.1(6) . . ? O2S S1S C1S' 100.9(5) . . ? O3S S1S C1S' 103.0(7) . . ? C1S S1S C1S' 26(2) . . ? S1S O3S C1S 54.5(18) . . ? F2S C1S F1S 98(4) . . ? F2S C1S F3S 95(7) . . ? F1S C1S F3S 141(7) . . ? F2S C1S S1S 107(5) . . ? F1S C1S S1S 101(3) . . ? F3S C1S S1S 111(5) . . ? F2S C1S O3S 75(4) . . ? F1S C1S O3S 70(3) . . ? F3S C1S O3S 149(5) . . ? S1S C1S O3S 48.7(18) . . ? C1S F2S F2S 160(7) . 2_677 ? F1S' C1S' F3S' 109.5(15) . . ? F1S' C1S' F2S' 109.1(10) . . ? F3S' C1S' F2S' 109.9(15) . . ? F1S' C1S' S1S 111.8(9) . . ? F3S' C1S' S1S 108.6(8) . . ? F2S' C1S' S1S 107.9(14) . . ? C1T C5T C6T 120.0 . . ? C5T C1T C2T 120.0 . . ? C3T C2T C1T 120.0 . . ? C2T C3T C4T 120.0 . . ? C3T C4T C6T 120.0 . . ? C4T C6T C5T 120.0 . . ? C4T C6T C7T 111(3) . . ? C5T C6T C7T 129(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 P1 C13 -124.0(7) . . . . ? C6 C1 P1 C13 61.8(7) . . . . ? C2 C1 P1 C7 -13.1(8) . . . . ? C6 C1 P1 C7 172.8(6) . . . . ? C2 C1 P1 Pt1 111.0(7) . . . . ? C6 C1 P1 Pt1 -63.1(7) . . . . ? C13 P1 Pt1 P2 35.1(2) . . . . ? C7 P1 Pt1 P2 -87.8(2) . . . . ? C1 P1 Pt1 P2 153.1(2) . . . . ? C13 P1 Pt1 S1 -147.9(2) . . . 2_666 ? C7 P1 Pt1 S1 89.3(2) . . . 2_666 ? C1 P1 Pt1 S1 -29.9(2) . . . 2_666 ? C13 P1 Pt1 S1 -152.4(4) . . . . ? C7 P1 Pt1 S1 84.7(4) . . . . ? C1 P1 Pt1 S1 -34.4(5) . . . . ? P2 Pt1 S1 C55 -77.36(17) . . . . ? P1 Pt1 S1 C55 110.2(4) . . . . ? S1 Pt1 S1 C55 105.59(17) 2_666 . . . ? P2 Pt1 S1 Pt1 177.06(5) . . . 2_666 ? P1 Pt1 S1 Pt1 4.6(4) . . . 2_666 ? S1 Pt1 S1 Pt1 0.0 2_666 . . 2_666 ? C6 C1 C2 C3 -1.2(14) . . . . ? P1 C1 C2 C3 -175.2(8) . . . . ? P1 Pt1 P2 C15 -28.9(2) . . . . ? S1 Pt1 P2 C15 -170.8(5) 2_666 . . . ? S1 Pt1 P2 C15 151.9(2) . . . . ? P1 Pt1 P2 C22 -150.6(3) . . . . ? S1 Pt1 P2 C22 67.5(6) 2_666 . . . ? S1 Pt1 P2 C22 30.2(3) . . . . ? P1 Pt1 P2 C16 91.8(2) . . . . ? S1 Pt1 P2 C16 -50.1(6) 2_666 . . . ? S1 Pt1 P2 C16 -87.4(2) . . . . ? C1 C2 C3 C4 1.3(18) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 C6 -0.9(19) . . . . ? C4 C5 C6 C1 1.0(17) . . . . ? C2 C1 C6 C5 0.0(13) . . . . ? P1 C1 C6 C5 174.4(8) . . . . ? C13 P1 C7 C12 -126.9(5) . . . . ? C1 P1 C7 C12 122.3(5) . . . . ? Pt1 P1 C7 C12 1.8(5) . . . . ? C13 P1 C7 C8 52.1(5) . . . . ? C1 P1 C7 C8 -58.7(6) . . . . ? Pt1 P1 C7 C8 -179.2(4) . . . . ? C12 C7 C8 C9 -2.1(10) . . . . ? P1 C7 C8 C9 178.9(5) . . . . ? C7 C8 C9 C10 0.7(11) . . . . ? C8 C9 C10 C11 0.4(11) . . . . ? C9 C10 C11 C12 0.0(10) . . . . ? C10 C11 C12 C7 -1.5(9) . . . . ? C8 C7 C12 C11 2.6(9) . . . . ? P1 C7 C12 C11 -178.5(5) . . . . ? C7 P1 C13 C14 68.0(4) . . . . ? C1 P1 C13 C14 -179.9(4) . . . . ? Pt1 P1 C13 C14 -59.7(4) . . . . ? P1 C13 C14 C15 82.6(6) . . . . ? C13 C14 C15 P2 -78.1(6) . . . . ? C22 P2 C15 C14 178.1(4) . . . . ? C16 P2 C15 C14 -69.8(4) . . . . ? Pt1 P2 C15 C14 50.4(5) . . . . ? C15 P2 C16 C17 167.6(4) . . . . ? C22 P2 C16 C17 -82.6(5) . . . . ? Pt1 P2 C16 C17 40.6(5) . . . . ? C15 P2 C16 C21 -9.9(5) . . . . ? C22 P2 C16 C21 99.9(5) . . . . ? Pt1 P2 C16 C21 -136.9(4) . . . . ? C21 C16 C17 C18 0.1(8) . . . . ? P2 C16 C17 C18 -177.5(5) . . . . ? C16 C17 C18 C19 1.2(9) . . . . ? C17 C18 C19 C20 -2.1(10) . . . . ? C18 C19 C20 C21 1.6(10) . . . . ? C19 C20 C21 C16 -0.2(9) . . . . ? C17 C16 C21 C20 -0.6(8) . . . . ? P2 C16 C21 C20 176.9(5) . . . . ? C15 P2 C22 C23 137.7(5) . . . . ? C16 P2 C22 C23 24.8(6) . . . . ? Pt1 P2 C22 C23 -93.0(5) . . . . ? C15 P2 C22 C27 -44.7(5) . . . . ? C16 P2 C22 C27 -157.7(5) . . . . ? Pt1 P2 C22 C27 84.6(5) . . . . ? C27 C22 C23 C24 0.7(10) . . . . ? P2 C22 C23 C24 178.2(6) . . . . ? C22 C23 C24 C25 0.2(12) . . . . ? C23 C24 C25 C26 -1.0(13) . . . . ? C24 C25 C26 C27 0.7(12) . . . . ? C23 C22 C27 C26 -0.9(10) . . . . ? P2 C22 C27 C26 -178.5(5) . . . . ? C25 C26 C27 C22 0.2(11) . . . . ? Pt1 S1 C55 C56 65.1(5) 2_666 . . . ? Pt1 S1 C55 C56 -37.2(5) . . . . ? S1 C55 C56 C57 178.6(4) . . . . ? C58 N1 C57 C56 -105.3(7) . . . . ? C55 C56 C57 N1 -175.2(5) . . . . ? C57 N1 C58 O2 -1.3(11) . . . . ? C57 N1 C58 N2 178.7(7) . . . . ? C59 N2 C58 O2 3.9(14) . . . . ? C59 N2 C58 N1 -176.0(8) . . . . ? C58 N2 C59 C60 18.9(14) . . . . ? C58 N2 C59 C64 -160.1(10) . . . . ? N2 C59 C60 C61 178.6(8) . . . . ? C64 C59 C60 C61 -2.4(13) . . . . ? C59 C60 C61 C62 -0.1(11) . . . . ? C60 C61 C62 C63 0.2(13) . . . . ? C61 C62 C63 C64 2.3(16) . . . . ? C62 C63 C64 C59 -4.9(17) . . . . ? C60 C59 C64 C63 4.9(16) . . . . ? N2 C59 C64 C63 -176.1(10) . . . . ? O1S S1S O3S C1S -109(2) . . . . ? O2S S1S O3S C1S 109(2) . . . . ? C1S' S1S O3S C1S 0(2) . . . . ? O1S S1S C1S F2S 164(4) . . . . ? O2S S1S C1S F2S -61(4) . . . . ? O3S S1S C1S F2S 51(4) . . . . ? C1S' S1S C1S F2S -129(7) . . . . ? O1S S1S C1S F1S 62(4) . . . . ? O2S S1S C1S F1S -163(3) . . . . ? O3S S1S C1S F1S -51(4) . . . . ? C1S' S1S C1S F1S 129(7) . . . . ? O1S S1S C1S F3S -94(6) . . . . ? O2S S1S C1S F3S 41(7) . . . . ? O3S S1S C1S F3S 152(7) . . . . ? C1S' S1S C1S F3S -27(6) . . . . ? O1S S1S C1S O3S 113.1(10) . . . . ? O2S S1S C1S O3S -111.7(9) . . . . ? C1S' S1S C1S O3S -180(5) . . . . ? S1S O3S C1S F2S -130(4) . . . . ? S1S O3S C1S F1S 125(3) . . . . ? S1S O3S C1S F3S -57(12) . . . . ? F1S C1S F2S F2S -83(25) . . . 2_677 ? F3S C1S F2S F2S 60(25) . . . 2_677 ? S1S C1S F2S F2S 173(23) . . . 2_677 ? O3S C1S F2S F2S -150(25) . . . 2_677 ? O1S S1S C1S' F1S' 62.7(12) . . . . ? O2S S1S C1S' F1S' -176.6(10) . . . . ? O3S S1S C1S' F1S' -57.7(12) . . . . ? C1S S1S C1S' F1S' -57(5) . . . . ? O1S S1S C1S' F3S' -58.2(11) . . . . ? O2S S1S C1S' F3S' 62.5(11) . . . . ? O3S S1S C1S' F3S' -178.5(10) . . . . ? C1S S1S C1S' F3S' -178(5) . . . . ? O1S S1S C1S' F2S' -177.3(11) . . . . ? O2S S1S C1S' F2S' -56.6(12) . . . . ? O3S S1S C1S' F2S' 62.3(12) . . . . ? C1S S1S C1S' F2S' 63(5) . . . . ? C6T C5T C1T C2T 0.0 . . . . ? C5T C1T C2T C3T 0.0 . . . . ? C1T C2T C3T C4T 0.0 . . . . ? C2T C3T C4T C6T 0.0 . . . . ? C3T C4T C6T C5T 0.0 . . . . ? C3T C4T C6T C7T 177(2) . . . . ? C1T C5T C6T C4T 0.0 . . . . ? C1T C5T C6T C7T -176(3) . . . . ? _diffrn_measured_fraction_theta_max 0.844 _diffrn_reflns_theta_full 36.46 _diffrn_measured_fraction_theta_full 0.844 _refine_diff_density_max 8.591 _refine_diff_density_min -8.022 _refine_diff_density_rms 0.371