Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Elena Lalinde' _publ_contact_author_address ; Grupo de Sintesis Quimica de la Rio Universidad de la Rioja UA-CSIC C/Madre de Dios n 51 Logrono (La Rioja) E-26006 SPAIN ; _publ_contact_author_email ELENA.LALINDE@UNIRIOJA.ES _publ_section_title ; One-Dimensional Phosphinite Platinum Chains Based on Hydrogen Bonding Interactions and Phosphinite Tetranuclear Platinum(II)-Thallium(I) Complexes ; loop_ _publ_author_name 'Elena Pena' 'Alvaro Diez' 'Juan Fornies' 'Julio Gomez' 'Antonio Martin' 'Teresa Moreno' 'Sergio Sanchez' data_complex1.Me2CO _database_code_depnum_ccdc_archive 'CCDC 640148' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H38 F5 O4 P3 Pt' _chemical_formula_weight 1025.75 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pt Pt -1.7033 8.3905 '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 12.5500(7) _cell_length_b 13.5977(7) _cell_length_c 24.6710(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.102(12) _cell_angle_gamma 90.00 _cell_volume 4177.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.2 _cell_measurement_theta_max 15.9 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.539 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3318 _exptl_absorpt_correction_T_max 0.5380 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7660 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.97 _reflns_number_total 7301 _reflns_number_gt 6019 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7301 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.805325(15) 0.734981(15) 0.184830(8) 0.02304(9) Uani 1 1 d . . . P1 P 0.68114(11) 0.61965(11) 0.20507(6) 0.0269(3) Uani 1 1 d . . . P2 P 0.92488(11) 0.67465(10) 0.25582(6) 0.0244(3) Uani 1 1 d . . . P3 P 0.91828(11) 0.86228(11) 0.16848(6) 0.0253(3) Uani 1 1 d . . . O1 O 0.7300(3) 0.5171(3) 0.22429(18) 0.0363(10) Uani 1 1 d . . . O2 O 0.9156(3) 0.5611(3) 0.26168(16) 0.0294(9) Uani 1 1 d . . . O3 O 0.9536(3) 0.9175(3) 0.22396(16) 0.0290(9) Uani 1 1 d . . . F1 F 0.7743(3) 0.6554(3) 0.06358(15) 0.0466(9) Uani 1 1 d . . . F2 F 0.6386(3) 0.6976(3) -0.02585(15) 0.0544(10) Uani 1 1 d . . . F3 F 0.4854(3) 0.8371(4) -0.02167(16) 0.0669(13) Uani 1 1 d . . . F4 F 0.4720(3) 0.9365(3) 0.07215(16) 0.0570(11) Uani 1 1 d . . . F5 F 0.6084(3) 0.8994(3) 0.16121(14) 0.0408(8) Uani 1 1 d . . . C1 C 0.6978(4) 0.7752(4) 0.1166(2) 0.0268(12) Uani 1 1 d . . . C2 C 0.7007(5) 0.7279(4) 0.0677(2) 0.0351(14) Uani 1 1 d . . . C3 C 0.6321(5) 0.7472(5) 0.0210(3) 0.0404(16) Uani 1 1 d . . . C4 C 0.5541(5) 0.8180(5) 0.0221(3) 0.0440(16) Uani 1 1 d . . . C5 C 0.5483(5) 0.8676(5) 0.0703(2) 0.0366(14) Uani 1 1 d . . . C6 C 0.6206(5) 0.8459(4) 0.1162(2) 0.0328(13) Uani 1 1 d . . . C7 C 0.6091(4) 0.6645(4) 0.2597(2) 0.0302(13) Uani 1 1 d . . . C8 C 0.5745(5) 0.5991(5) 0.2972(3) 0.0500(18) Uani 1 1 d . . . H8A H 0.5846 0.5304 0.2931 0.060 Uiso 1 1 calc R . . C9 C 0.5259(6) 0.6339(6) 0.3402(3) 0.0519(19) Uani 1 1 d . . . H9A H 0.5021 0.5888 0.3655 0.062 Uiso 1 1 calc R . . C10 C 0.5112(5) 0.7319(5) 0.3472(3) 0.0441(17) Uani 1 1 d . . . H10A H 0.4785 0.7548 0.3775 0.053 Uiso 1 1 calc R . . C11 C 0.5437(5) 0.7984(5) 0.3103(3) 0.0385(15) Uani 1 1 d . . . H11A H 0.5314 0.8668 0.3143 0.046 Uiso 1 1 calc R . . C12 C 0.5944(5) 0.7641(4) 0.2672(2) 0.0334(14) Uani 1 1 d . . . H12A H 0.6194 0.8096 0.2425 0.040 Uiso 1 1 calc R . . C13 C 0.5785(4) 0.5834(4) 0.1513(2) 0.0283(12) Uani 1 1 d . . . C14 C 0.5993(5) 0.5051(5) 0.1174(2) 0.0365(14) Uani 1 1 d . . . H14A H 0.6666 0.4724 0.1235 0.044 Uiso 1 1 calc R . . C15 C 0.5251(5) 0.4745(5) 0.0757(3) 0.0409(15) Uani 1 1 d . . . H15A H 0.5412 0.4217 0.0529 0.049 Uiso 1 1 calc R . . C16 C 0.4266(5) 0.5204(5) 0.0669(3) 0.0442(16) Uani 1 1 d . . . H16A H 0.3749 0.4993 0.0379 0.053 Uiso 1 1 calc R . . C17 C 0.4029(5) 0.5972(5) 0.1002(3) 0.0490(18) Uani 1 1 d . . . H17A H 0.3343 0.6277 0.0946 0.059 Uiso 1 1 calc R . . C18 C 0.4787(5) 0.6294(5) 0.1416(3) 0.0405(15) Uani 1 1 d . . . H18A H 0.4628 0.6834 0.1637 0.049 Uiso 1 1 calc R . . C19 C 0.9067(4) 0.7268(4) 0.3219(2) 0.0301(13) Uani 1 1 d . . . C20 C 0.9498(5) 0.6785(6) 0.3687(3) 0.0465(17) Uani 1 1 d . . . H20A H 0.9921 0.6211 0.3663 0.056 Uiso 1 1 calc R . . C21 C 0.9309(6) 0.7144(7) 0.4194(3) 0.066(2) Uani 1 1 d . . . H21A H 0.9621 0.6821 0.4517 0.080 Uiso 1 1 calc R . . C22 C 0.8682(6) 0.7952(7) 0.4236(3) 0.065(2) Uani 1 1 d . . . H22A H 0.8542 0.8175 0.4585 0.078 Uiso 1 1 calc R . . C23 C 0.8257(6) 0.8440(7) 0.3778(3) 0.066(3) Uani 1 1 d . . . H23A H 0.7827 0.9007 0.3810 0.079 Uiso 1 1 calc R . . C24 C 0.8447(5) 0.8114(5) 0.3259(3) 0.0456(17) Uani 1 1 d . . . H24A H 0.8160 0.8463 0.2940 0.055 Uiso 1 1 calc R . . C25 C 1.0675(4) 0.6907(4) 0.2498(2) 0.0264(12) Uani 1 1 d . . . C26 C 1.1276(5) 0.7657(4) 0.2763(2) 0.0307(13) Uani 1 1 d . . . H26A H 1.0945 0.8123 0.2975 0.037 Uiso 1 1 calc R . . C27 C 1.2362(5) 0.7725(4) 0.2718(3) 0.0350(14) Uani 1 1 d . . . H27A H 1.2776 0.8240 0.2900 0.042 Uiso 1 1 calc R . . C28 C 1.2845(5) 0.7049(5) 0.2410(3) 0.0422(16) Uani 1 1 d . . . H28A H 1.3593 0.7094 0.2386 0.051 Uiso 1 1 calc R . . C29 C 1.2250(5) 0.6309(5) 0.2137(3) 0.0420(16) Uani 1 1 d . . . H29A H 1.2584 0.5847 0.1924 0.050 Uiso 1 1 calc R . . C30 C 1.1152(5) 0.6244(4) 0.2177(2) 0.0337(13) Uani 1 1 d . . . H30A H 1.0732 0.5745 0.1984 0.040 Uiso 1 1 calc R . . C31 C 1.0368(4) 0.8310(4) 0.1371(3) 0.0336(14) Uani 1 1 d . . . C32 C 1.1261(5) 0.8903(5) 0.1439(3) 0.0420(16) Uani 1 1 d . . . H32A H 1.1294 0.9441 0.1686 0.050 Uiso 1 1 calc R . . C33 C 1.2119(5) 0.8718(6) 0.1144(3) 0.0532(19) Uani 1 1 d . . . H33A H 1.2729 0.9138 0.1184 0.064 Uiso 1 1 calc R . . C34 C 1.2082(6) 0.7933(6) 0.0800(3) 0.056(2) Uani 1 1 d . . . H34A H 1.2677 0.7798 0.0608 0.067 Uiso 1 1 calc R . . C35 C 1.1198(7) 0.7335(6) 0.0727(3) 0.060(2) Uani 1 1 d . . . H35A H 1.1172 0.6796 0.0481 0.072 Uiso 1 1 calc R . . C36 C 1.0343(6) 0.7523(5) 0.1015(3) 0.0473(17) Uani 1 1 d . . . H36A H 0.9731 0.7106 0.0967 0.057 Uiso 1 1 calc R . . C37 C 0.8573(4) 0.9559(5) 0.1214(2) 0.0331(13) Uani 1 1 d . . . C38 C 0.8646(6) 0.9509(6) 0.0662(3) 0.056(2) Uani 1 1 d . . . H38A H 0.9044 0.8995 0.0521 0.067 Uiso 1 1 calc R . . C39 C 0.8146(7) 1.0197(9) 0.0318(3) 0.094(4) Uani 1 1 d . . . H39A H 0.8194 1.0159 -0.0063 0.113 Uiso 1 1 calc R . . C40 C 0.7572(7) 1.0946(8) 0.0520(4) 0.088(4) Uani 1 1 d . . . H40A H 0.7237 1.1429 0.0278 0.106 Uiso 1 1 calc R . . C41 C 0.7479(5) 1.1000(6) 0.1067(4) 0.062(2) Uani 1 1 d . . . H41A H 0.7077 1.1514 0.1205 0.074 Uiso 1 1 calc R . . C42 C 0.7973(4) 1.0305(4) 0.1409(3) 0.0353(14) Uani 1 1 d . . . H42A H 0.7904 1.0333 0.1788 0.042 Uiso 1 1 calc R . . C43 C 0.8474(6) 0.4331(5) 0.0540(3) 0.0426(16) Uani 1 1 d . . . O4 O 0.8405(10) 0.4724(7) 0.0117(4) 0.069(3) Uani 0.60 1 d P A 1 C44 C 0.7916(13) 0.3415(11) 0.0631(8) 0.074(4) Uani 0.60 1 d P A 1 H44A H 0.7722 0.3406 0.1003 0.110 Uiso 0.60 1 calc PR A 1 H44B H 0.8387 0.2857 0.0580 0.110 Uiso 0.60 1 calc PR A 1 H44C H 0.7264 0.3368 0.0369 0.110 Uiso 0.60 1 calc PR A 1 C45 C 0.9187(12) 0.4727(13) 0.1046(7) 0.050(4) Uani 0.60 1 d P A 1 H45A H 0.8734 0.4955 0.1316 0.075 Uiso 0.60 1 calc PR A 1 H45B H 0.9622 0.5276 0.0938 0.075 Uiso 0.60 1 calc PR A 1 H45C H 0.9661 0.4202 0.1205 0.075 Uiso 0.60 1 calc PR A 1 O4' O 0.7675(11) 0.3884(11) 0.0314(6) 0.057(4) Uani 0.40 1 d P A 2 C44' C 0.8785(19) 0.437(3) 0.1119(11) 0.100(15) Uani 0.40 1 d P A 2 H44D H 0.8201 0.4113 0.1308 0.151 Uiso 0.40 1 calc PR A 2 H44E H 0.8938 0.5051 0.1231 0.151 Uiso 0.40 1 calc PR A 2 H44F H 0.9430 0.3967 0.1213 0.151 Uiso 0.40 1 calc PR A 2 C45' C 0.9150(16) 0.4884(16) 0.0163(8) 0.050(5) Uani 0.40 1 d P A 2 H45D H 0.8783 0.4872 -0.0211 0.075 Uiso 0.40 1 calc PR A 2 H45E H 0.9853 0.4566 0.0173 0.075 Uiso 0.40 1 calc PR A 2 H45F H 0.9247 0.5567 0.0286 0.075 Uiso 0.40 1 calc PR A 2 H1 H 0.815(6) 0.533(6) 0.245(3) 0.070(18) Uiso 1 1 d . . . H2 H 0.995(6) 0.962(6) 0.227(3) 0.070(18) Uiso 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 Pt 0.01940(12) 0.02291(13) 0.02656(13) -0.00431(9) 0.00187(8) 0.00185(8) P1 0.0215(7) 0.0252(8) 0.0331(8) -0.0041(6) 0.0005(6) 0.0004(6) P2 0.0207(7) 0.0248(8) 0.0275(7) -0.0046(6) 0.0026(6) 0.0003(6) P3 0.0215(7) 0.0264(8) 0.0283(7) -0.0012(6) 0.0041(6) 0.0015(6) O1 0.024(2) 0.025(2) 0.057(3) 0.0015(19) -0.0059(19) 0.0002(17) O2 0.0204(19) 0.029(2) 0.038(2) -0.0008(17) -0.0027(16) -0.0012(16) O3 0.028(2) 0.024(2) 0.035(2) -0.0024(17) 0.0055(17) -0.0031(17) F1 0.046(2) 0.046(2) 0.047(2) -0.0145(18) 0.0017(17) 0.0144(18) F2 0.050(2) 0.073(3) 0.037(2) -0.018(2) -0.0054(18) 0.003(2) F3 0.054(3) 0.099(4) 0.042(2) -0.003(2) -0.0172(19) 0.028(2) F4 0.044(2) 0.067(3) 0.056(2) 0.000(2) -0.0069(19) 0.026(2) F5 0.040(2) 0.044(2) 0.040(2) -0.0085(16) 0.0068(16) 0.0112(16) C1 0.021(3) 0.032(3) 0.026(3) 0.003(2) -0.004(2) 0.001(2) C2 0.029(3) 0.034(3) 0.042(4) -0.008(3) 0.002(3) 0.002(3) C3 0.035(3) 0.055(4) 0.030(3) -0.013(3) -0.001(3) -0.007(3) C4 0.030(3) 0.058(5) 0.041(4) -0.002(3) -0.008(3) 0.002(3) C5 0.032(3) 0.041(4) 0.036(3) 0.004(3) 0.001(3) 0.010(3) C6 0.033(3) 0.033(3) 0.034(3) -0.004(3) 0.008(3) -0.005(3) C7 0.022(3) 0.041(4) 0.026(3) -0.003(2) -0.004(2) 0.002(2) C8 0.049(4) 0.046(4) 0.058(4) 0.009(3) 0.019(3) 0.000(3) C9 0.063(5) 0.062(5) 0.034(4) 0.019(3) 0.020(3) 0.008(4) C10 0.036(4) 0.065(5) 0.032(3) -0.007(3) 0.008(3) -0.004(3) C11 0.033(3) 0.043(4) 0.041(4) -0.011(3) 0.011(3) -0.006(3) C12 0.038(3) 0.035(3) 0.028(3) -0.002(2) 0.008(3) -0.010(3) C13 0.021(3) 0.029(3) 0.035(3) -0.001(2) 0.004(2) -0.001(2) C14 0.026(3) 0.047(4) 0.036(3) -0.010(3) 0.004(3) 0.002(3) C15 0.039(4) 0.043(4) 0.040(4) -0.013(3) 0.002(3) -0.001(3) C16 0.039(4) 0.052(4) 0.037(4) -0.007(3) -0.009(3) -0.002(3) C17 0.022(3) 0.060(5) 0.062(5) -0.007(4) -0.007(3) 0.010(3) C18 0.029(3) 0.044(4) 0.048(4) -0.010(3) 0.003(3) 0.007(3) C19 0.021(3) 0.040(3) 0.030(3) -0.013(3) 0.001(2) -0.008(2) C20 0.041(4) 0.068(5) 0.032(3) -0.005(3) 0.009(3) -0.006(3) C21 0.052(5) 0.110(7) 0.037(4) -0.012(4) 0.006(3) -0.008(5) C22 0.043(4) 0.117(7) 0.038(4) -0.039(5) 0.018(3) -0.015(5) C23 0.039(4) 0.093(7) 0.068(6) -0.049(5) 0.011(4) 0.004(4) C24 0.030(3) 0.056(4) 0.051(4) -0.023(3) 0.006(3) 0.004(3) C25 0.023(3) 0.026(3) 0.029(3) -0.001(2) 0.000(2) 0.002(2) C26 0.028(3) 0.032(3) 0.031(3) -0.002(2) -0.001(2) 0.002(2) C27 0.029(3) 0.034(3) 0.042(4) 0.000(3) 0.002(3) -0.002(3) C28 0.019(3) 0.050(4) 0.059(4) 0.003(3) 0.011(3) 0.000(3) C29 0.027(3) 0.055(4) 0.045(4) -0.002(3) 0.012(3) 0.011(3) C30 0.033(3) 0.034(3) 0.034(3) -0.001(3) 0.004(3) 0.004(3) C31 0.024(3) 0.032(3) 0.046(4) -0.003(3) 0.010(3) 0.007(2) C32 0.031(3) 0.040(4) 0.058(4) 0.001(3) 0.017(3) 0.003(3) C33 0.039(4) 0.070(5) 0.056(4) 0.015(4) 0.026(3) 0.010(4) C34 0.055(5) 0.076(5) 0.043(4) 0.022(4) 0.026(3) 0.036(4) C35 0.064(5) 0.075(6) 0.045(4) -0.012(4) 0.018(4) 0.025(4) C36 0.046(4) 0.051(4) 0.046(4) -0.013(3) 0.007(3) 0.005(3) C37 0.024(3) 0.040(4) 0.035(3) 0.008(3) 0.001(2) 0.005(3) C38 0.046(4) 0.088(6) 0.037(4) 0.013(4) 0.012(3) 0.029(4) C39 0.086(7) 0.157(10) 0.044(5) 0.045(6) 0.024(5) 0.065(7) C40 0.066(6) 0.134(9) 0.069(6) 0.067(6) 0.025(5) 0.062(6) C41 0.036(4) 0.064(5) 0.088(6) 0.034(4) 0.019(4) 0.028(4) C42 0.028(3) 0.037(4) 0.041(3) 0.009(3) 0.004(3) 0.006(3) C43 0.040(4) 0.038(4) 0.051(4) 0.003(3) 0.011(3) 0.016(3) O4 0.108(9) 0.051(6) 0.051(6) -0.007(5) 0.019(7) 0.015(7) C44 0.065(10) 0.051(9) 0.107(14) -0.009(9) 0.023(10) -0.007(8) C45 0.042(10) 0.061(9) 0.047(9) -0.006(7) 0.005(7) 0.013(7) O4' 0.055(9) 0.049(9) 0.067(9) -0.002(7) 0.010(7) 0.019(7) C44' 0.032(15) 0.21(4) 0.064(15) 0.07(2) 0.013(12) 0.063(19) C45' 0.053(12) 0.052(12) 0.048(11) -0.002(9) 0.016(11) 0.004(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C1 2.095(5) . ? Pt P3 2.3043(14) . ? Pt P1 2.3087(15) . ? Pt P2 2.3113(14) . ? P1 O1 1.572(4) . ? P1 C13 1.800(6) . ? P1 C7 1.819(6) . ? P2 O2 1.557(4) . ? P2 C19 1.817(6) . ? P2 C25 1.828(5) . ? P3 O3 1.576(4) . ? P3 C31 1.809(6) . ? P3 C37 1.826(6) . ? O1 H1 1.14(8) . ? O2 H1 1.34(8) . ? O3 H2 0.80(8) . ? F1 C2 1.363(7) . ? F2 C3 1.350(7) . ? F3 C4 1.322(7) . ? F4 C5 1.345(7) . ? F5 C6 1.351(6) . ? C1 C6 1.364(8) . ? C1 C2 1.372(8) . ? C2 C3 1.375(9) . ? C3 C4 1.375(9) . ? C4 C5 1.375(9) . ? C5 C6 1.394(8) . ? C7 C12 1.382(8) . ? C7 C8 1.391(9) . ? C8 C9 1.372(9) . ? C8 H8A 0.9500 . ? C9 C10 1.359(10) . ? C9 H9A 0.9500 . ? C10 C11 1.380(9) . ? C10 H10A 0.9500 . ? C11 C12 1.384(8) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.394(8) . ? C13 C14 1.398(8) . ? C14 C15 1.364(8) . ? C14 H14A 0.9500 . ? C15 C16 1.377(9) . ? C15 H15A 0.9500 . ? C16 C17 1.384(9) . ? C16 H16A 0.9500 . ? C17 C18 1.378(9) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.380(9) . ? C19 C24 1.400(9) . ? C20 C21 1.390(10) . ? C20 H20A 0.9500 . ? C21 C22 1.362(12) . ? C21 H21A 0.9500 . ? C22 C23 1.363(12) . ? C22 H22A 0.9500 . ? C23 C24 1.402(9) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.383(8) . ? C25 C30 1.383(8) . ? C26 C27 1.383(8) . ? C26 H26A 0.9500 . ? C27 C28 1.380(9) . ? C27 H27A 0.9500 . ? C28 C29 1.378(9) . ? C28 H28A 0.9500 . ? C29 C30 1.397(8) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.375(8) . ? C31 C36 1.383(9) . ? C32 C33 1.394(8) . ? C32 H32A 0.9500 . ? C33 C34 1.362(11) . ? C33 H33A 0.9500 . ? C34 C35 1.370(12) . ? C34 H34A 0.9500 . ? C35 C36 1.381(10) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.379(9) . ? C37 C42 1.385(8) . ? C38 C39 1.362(10) . ? C38 H38A 0.9500 . ? C39 C40 1.376(13) . ? C39 H39A 0.9500 . ? C40 C41 1.370(11) . ? C40 H40A 0.9500 . ? C41 C42 1.365(9) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 O4 1.166(12) . ? C43 O4' 1.245(15) . ? C43 C44' 1.43(3) . ? C43 C44 1.460(16) . ? C43 C45 1.539(18) . ? C43 C45' 1.53(2) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 0.9800 . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt P3 90.69(16) . . ? C1 Pt P1 88.07(16) . . ? P3 Pt P1 173.97(5) . . ? C1 Pt P2 174.02(16) . . ? P3 Pt P2 92.49(5) . . ? P1 Pt P2 89.27(5) . . ? O1 P1 C13 101.3(2) . . ? O1 P1 C7 106.5(3) . . ? C13 P1 C7 105.2(2) . . ? O1 P1 Pt 114.77(16) . . ? C13 P1 Pt 117.85(19) . . ? C7 P1 Pt 110.1(2) . . ? O2 P2 C19 106.5(3) . . ? O2 P2 C25 102.2(2) . . ? C19 P2 C25 105.1(2) . . ? O2 P2 Pt 111.92(15) . . ? C19 P2 Pt 113.5(2) . . ? C25 P2 Pt 116.49(18) . . ? O3 P3 C31 109.0(3) . . ? O3 P3 C37 105.7(3) . . ? C31 P3 C37 101.2(3) . . ? O3 P3 Pt 108.61(16) . . ? C31 P3 Pt 117.0(2) . . ? C37 P3 Pt 114.6(2) . . ? P1 O1 H1 106(4) . . ? P2 O2 H1 109(3) . . ? P3 O3 H2 124(6) . . ? C6 C1 C2 114.9(5) . . ? C6 C1 Pt 125.2(4) . . ? C2 C1 Pt 119.9(4) . . ? F1 C2 C1 119.8(5) . . ? F1 C2 C3 115.8(5) . . ? C1 C2 C3 124.4(6) . . ? F2 C3 C4 119.0(6) . . ? F2 C3 C2 121.6(6) . . ? C4 C3 C2 119.4(6) . . ? F3 C4 C5 120.7(6) . . ? F3 C4 C3 121.0(6) . . ? C5 C4 C3 118.3(6) . . ? F4 C5 C4 119.1(5) . . ? F4 C5 C6 120.9(5) . . ? C4 C5 C6 120.0(6) . . ? F5 C6 C1 121.7(5) . . ? F5 C6 C5 115.2(5) . . ? C1 C6 C5 123.1(5) . . ? C12 C7 C8 118.6(6) . . ? C12 C7 P1 121.0(4) . . ? C8 C7 P1 120.2(5) . . ? C9 C8 C7 119.9(7) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 121.1(6) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C9 C10 C11 120.2(6) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 119.1(6) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? C7 C12 C11 121.0(6) . . ? C7 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C18 C13 C14 118.0(5) . . ? C18 C13 P1 123.3(5) . . ? C14 C13 P1 118.7(4) . . ? C15 C14 C13 121.5(6) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C14 C15 C16 119.8(6) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C15 C16 C17 120.2(6) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C18 C17 C16 120.0(6) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C13 120.5(6) . . ? C17 C18 H18A 119.7 . . ? C13 C18 H18A 119.7 . . ? C20 C19 C24 119.7(6) . . ? C20 C19 P2 119.1(5) . . ? C24 C19 P2 121.2(5) . . ? C19 C20 C21 119.6(7) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? C22 C21 C20 121.1(8) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C23 C22 C21 120.0(7) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.7(8) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C19 C24 C23 118.9(7) . . ? C19 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? C26 C25 C30 120.1(5) . . ? C26 C25 P2 122.1(4) . . ? C30 C25 P2 117.8(4) . . ? C25 C26 C27 119.8(5) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C28 C27 C26 120.2(6) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 C27 120.5(5) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C30 119.4(6) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? C25 C30 C29 120.0(6) . . ? C25 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C32 C31 C36 119.0(6) . . ? C32 C31 P3 120.8(5) . . ? C36 C31 P3 119.9(5) . . ? C31 C32 C33 120.1(7) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 119.9(7) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C33 C34 C35 120.7(6) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.6 . . ? C34 C35 C36 119.4(7) . . ? C34 C35 H35A 120.3 . . ? C36 C35 H35A 120.3 . . ? C35 C36 C31 120.8(7) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? C38 C37 C42 119.0(6) . . ? C38 C37 P3 121.4(5) . . ? C42 C37 P3 119.5(4) . . ? C39 C38 C37 120.0(7) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C40 120.2(7) . . ? C38 C39 H39A 119.9 . . ? C40 C39 H39A 119.9 . . ? C41 C40 C39 120.6(7) . . ? C41 C40 H40A 119.7 . . ? C39 C40 H40A 119.7 . . ? C42 C41 C40 119.0(7) . . ? C42 C41 H41A 120.5 . . ? C40 C41 H41A 120.5 . . ? C41 C42 C37 121.1(6) . . ? C41 C42 H42A 119.4 . . ? C37 C42 H42A 119.4 . . ? O4 C43 O4' 81.7(11) . . ? O4 C43 C44' 148.9(18) . . ? O4' C43 C44' 124.7(15) . . ? O4 C43 C44 122.9(12) . . ? O4' C43 C44 43.6(9) . . ? C44' C43 C44 87.4(16) . . ? O4 C43 C45 122.4(10) . . ? O4' C43 C45 152.9(11) . . ? C44' C43 C45 28.5(13) . . ? C44 C43 C45 114.6(11) . . ? O4 C43 C45' 38.4(9) . . ? O4' C43 C45' 116.3(13) . . ? C44' C43 C45' 119.0(15) . . ? C44 C43 C45' 145.4(12) . . ? C45 C43 C45' 90.6(11) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? C43 C44' H44D 109.5 . . ? C43 C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C43 C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? C43 C45' H45D 109.5 . . ? C43 C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? C43 C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.027 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.120 #===END data_complex3.2CHCl3 _database_code_depnum_ccdc_archive 'CCDC 640149' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H80 Cl6 O6 P6 Pt2 Tl2' _chemical_formula_weight 2406.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 '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' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 12.126(2) _cell_length_b 12.9612(18) _cell_length_c 15.926(2) _cell_angle_alpha 97.277(17) _cell_angle_beta 108.073(17) _cell_angle_gamma 112.454(16) _cell_volume 2111.7(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.4 _cell_measurement_theta_max 18.0 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1154 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.461 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.1181 _exptl_absorpt_correction_T_max 0.2570 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7759 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 24.93 _reflns_number_total 7377 _reflns_number_gt 6470 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0276P)^2^+6.3688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7377 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt -0.157727(18) -0.154494(16) -0.249992(13) 0.01387(6) Uani 1 1 d . . . Tl Tl 0.09272(2) -0.03523(2) -0.070974(15) 0.02784(7) Uani 1 1 d . . . P1 P -0.16395(12) 0.00960(11) -0.17479(9) 0.0143(3) Uani 1 1 d . . . P2 P -0.08668(13) -0.08371(11) -0.35800(9) 0.0170(3) Uani 1 1 d . . . P3 P -0.14744(13) -0.32780(11) -0.29224(10) 0.0183(3) Uani 1 1 d . . . O1 O -0.0638(3) 0.0513(3) -0.0743(2) 0.0185(8) Uani 1 1 d . . . O2 O -0.0523(4) -0.1652(3) -0.4167(3) 0.0242(8) Uani 1 1 d . . . O3 O -0.1184(4) -0.3492(3) -0.3787(3) 0.0247(9) Uani 1 1 d . . . C1 C -0.2333(5) -0.2260(4) -0.1627(4) 0.0197(11) Uani 1 1 d . . . C2 C -0.2946(5) -0.2756(5) -0.1219(4) 0.0201(11) Uani 1 1 d . . . C3 C -0.3835(5) -0.3451(5) -0.0822(4) 0.0241(12) Uani 1 1 d . . . C4 C -0.3962(9) -0.2627(7) -0.0128(6) 0.069(3) Uani 1 1 d . . . H4A H -0.3122 -0.2173 0.0389 0.103 Uiso 1 1 calc R . . H4B H -0.4606 -0.3078 0.0098 0.103 Uiso 1 1 calc R . . H4C H -0.4239 -0.2100 -0.0425 0.103 Uiso 1 1 calc R . . C5 C -0.5157(6) -0.4183(5) -0.1600(4) 0.0332(14) Uani 1 1 d . . . H5A H -0.5494 -0.3671 -0.1868 0.050 Uiso 1 1 calc R . . H5B H -0.5755 -0.4674 -0.1358 0.050 Uiso 1 1 calc R . . H5C H -0.5075 -0.4675 -0.2073 0.050 Uiso 1 1 calc R . . C6 C -0.3355(6) -0.4272(7) -0.0404(6) 0.060(3) Uani 1 1 d . . . H6A H -0.2549 -0.3820 0.0141 0.090 Uiso 1 1 calc R . . H6B H -0.3196 -0.4720 -0.0858 0.090 Uiso 1 1 calc R . . H6C H -0.4013 -0.4805 -0.0228 0.090 Uiso 1 1 calc R . . C7 C -0.3237(5) -0.0214(4) -0.1733(4) 0.0175(11) Uani 1 1 d . . . C8 C -0.3313(5) 0.0557(5) -0.1082(4) 0.0234(12) Uani 1 1 d . . . H8 H -0.2551 0.1233 -0.0681 0.028 Uiso 1 1 calc R . . C9 C -0.4480(6) 0.0348(5) -0.1014(4) 0.0307(14) Uani 1 1 d . . . H9 H -0.4517 0.0863 -0.0555 0.037 Uiso 1 1 calc R . . C10 C -0.5600(6) -0.0616(5) -0.1616(4) 0.0308(14) Uani 1 1 d . . . H10 H -0.6406 -0.0760 -0.1571 0.037 Uiso 1 1 calc R . . C11 C -0.5544(5) -0.1365(5) -0.2279(4) 0.0288(13) Uani 1 1 d . . . H11 H -0.6317 -0.2011 -0.2706 0.035 Uiso 1 1 calc R . . C12 C -0.4361(5) -0.1179(4) -0.2323(4) 0.0208(11) Uani 1 1 d . . . H12 H -0.4323 -0.1718 -0.2763 0.025 Uiso 1 1 calc R . . C13 C -0.1296(5) 0.1417(4) -0.2124(4) 0.0180(11) Uani 1 1 d . . . C14 C -0.2136(5) 0.1473(5) -0.2921(4) 0.0212(12) Uani 1 1 d . . . H14 H -0.2935 0.0810 -0.3284 0.025 Uiso 1 1 calc R . . C15 C -0.1817(6) 0.2483(5) -0.3188(4) 0.0285(13) Uani 1 1 d . . . H15 H -0.2394 0.2514 -0.3735 0.034 Uiso 1 1 calc R . . C16 C -0.0660(6) 0.3448(5) -0.2659(4) 0.0321(14) Uani 1 1 d . . . H16 H -0.0434 0.4138 -0.2851 0.039 Uiso 1 1 calc R . . C17 C 0.0172(6) 0.3421(5) -0.1854(4) 0.0310(14) Uani 1 1 d . . . H17 H 0.0956 0.4095 -0.1484 0.037 Uiso 1 1 calc R . . C18 C -0.0142(5) 0.2399(5) -0.1585(4) 0.0254(13) Uani 1 1 d . . . H18 H 0.0432 0.2374 -0.1033 0.031 Uiso 1 1 calc R . . C19 C 0.0649(5) 0.0501(4) -0.3086(4) 0.0189(11) Uani 1 1 d . . . C20 C 0.1750(5) 0.0390(5) -0.2613(4) 0.0246(12) Uani 1 1 d . . . H20 H 0.1675 -0.0353 -0.2556 0.030 Uiso 1 1 calc R . . C21 C 0.2956(6) 0.1342(5) -0.2224(4) 0.0290(13) Uani 1 1 d . . . H21 H 0.3704 0.1254 -0.1904 0.035 Uiso 1 1 calc R . . C22 C 0.3067(6) 0.2418(5) -0.2301(4) 0.0309(14) Uani 1 1 d . . . H22 H 0.3893 0.3076 -0.2035 0.037 Uiso 1 1 calc R . . C23 C 0.1978(6) 0.2543(5) -0.2765(4) 0.0336(14) Uani 1 1 d . . . H23 H 0.2059 0.3289 -0.2816 0.040 Uiso 1 1 calc R . . C24 C 0.0770(6) 0.1593(5) -0.3158(4) 0.0275(13) Uani 1 1 d . . . H24 H 0.0025 0.1686 -0.3477 0.033 Uiso 1 1 calc R . . C25 C -0.2046(5) -0.0556(4) -0.4418(4) 0.0205(11) Uani 1 1 d . . . C26 C -0.1718(6) 0.0069(5) -0.5027(4) 0.0247(12) Uani 1 1 d . . . H26 H -0.0857 0.0373 -0.5001 0.030 Uiso 1 1 calc R . . C27 C -0.2653(6) 0.0244(5) -0.5669(4) 0.0296(13) Uani 1 1 d . . . H27 H -0.2423 0.0700 -0.6065 0.036 Uiso 1 1 calc R . . C28 C -0.3917(6) -0.0243(5) -0.5737(4) 0.0295(13) Uani 1 1 d . . . H28 H -0.4553 -0.0124 -0.6184 0.035 Uiso 1 1 calc R . . C29 C -0.4267(6) -0.0895(5) -0.5166(4) 0.0285(13) Uani 1 1 d . . . H29 H -0.5143 -0.1238 -0.5224 0.034 Uiso 1 1 calc R . . C30 C -0.3333(5) -0.1052(4) -0.4502(4) 0.0217(12) Uani 1 1 d . . . H30 H -0.3571 -0.1500 -0.4103 0.026 Uiso 1 1 calc R . . C31 C -0.0204(5) -0.3354(4) -0.1994(4) 0.0199(11) Uani 1 1 d . . . C32 C 0.0902(5) -0.3290(5) -0.2142(4) 0.0263(13) Uani 1 1 d . . . H32 H 0.0955 -0.3230 -0.2718 0.032 Uiso 1 1 calc R . . C33 C 0.1913(6) -0.3316(5) -0.1453(5) 0.0327(15) Uani 1 1 d . . . H33 H 0.2663 -0.3259 -0.1555 0.039 Uiso 1 1 calc R . . C34 C 0.1841(6) -0.3423(5) -0.0621(4) 0.0342(15) Uani 1 1 d . . . H34 H 0.2532 -0.3455 -0.0156 0.041 Uiso 1 1 calc R . . C35 C 0.0751(6) -0.3485(5) -0.0461(4) 0.0318(14) Uani 1 1 d . . . H35 H 0.0699 -0.3554 0.0114 0.038 Uiso 1 1 calc R . . C36 C -0.0244(6) -0.3447(5) -0.1143(4) 0.0285(13) Uani 1 1 d . . . H36 H -0.0981 -0.3484 -0.1030 0.034 Uiso 1 1 calc R . . C37 C -0.2965(5) -0.4527(4) -0.3118(4) 0.0188(11) Uani 1 1 d . . . C38 C -0.4110(5) -0.4580(5) -0.3705(4) 0.0246(12) Uani 1 1 d . . . H38 H -0.4093 -0.3931 -0.3930 0.030 Uiso 1 1 calc R . . C39 C -0.5284(6) -0.5562(5) -0.3975(4) 0.0278(13) Uani 1 1 d . . . H39 H -0.6060 -0.5589 -0.4387 0.033 Uiso 1 1 calc R . . C40 C -0.5310(6) -0.6499(5) -0.3638(4) 0.0285(13) Uani 1 1 d . . . H40 H -0.6109 -0.7172 -0.3815 0.034 Uiso 1 1 calc R . . C41 C -0.4176(6) -0.6459(5) -0.3044(4) 0.0292(13) Uani 1 1 d . . . H41 H -0.4201 -0.7108 -0.2817 0.035 Uiso 1 1 calc R . . C42 C -0.3007(6) -0.5484(5) -0.2779(4) 0.0249(12) Uani 1 1 d . . . H42 H -0.2233 -0.5461 -0.2368 0.030 Uiso 1 1 calc R . . C43 C -0.2008(5) 0.4244(5) 0.4698(4) 0.0229(12) Uani 1 1 d . . . H43 H -0.1506 0.4945 0.5243 0.027 Uiso 1 1 calc R . . Cl1 Cl -0.21989(16) 0.47030(14) 0.36894(11) 0.0386(4) Uani 1 1 d . . . Cl2 Cl -0.11387(15) 0.34208(13) 0.47523(12) 0.0373(4) Uani 1 1 d . . . Cl3 Cl -0.35278(14) 0.34257(13) 0.47233(11) 0.0332(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 Pt 0.01906(11) 0.01111(10) 0.01705(11) 0.00719(7) 0.01218(8) 0.00723(8) Tl 0.02681(12) 0.04793(15) 0.01989(12) 0.01335(10) 0.01321(10) 0.02328(11) P1 0.0178(6) 0.0124(6) 0.0145(6) 0.0044(5) 0.0078(5) 0.0071(5) P2 0.0251(7) 0.0134(6) 0.0202(7) 0.0082(5) 0.0161(6) 0.0093(6) P3 0.0248(7) 0.0123(6) 0.0239(7) 0.0074(5) 0.0154(6) 0.0088(6) O1 0.0191(18) 0.0194(19) 0.0156(18) 0.0051(15) 0.0055(15) 0.0080(15) O2 0.037(2) 0.022(2) 0.026(2) 0.0091(16) 0.0238(18) 0.0159(18) O3 0.039(2) 0.0165(19) 0.030(2) 0.0073(16) 0.0241(19) 0.0138(17) C1 0.026(3) 0.018(3) 0.023(3) 0.012(2) 0.013(2) 0.013(2) C2 0.025(3) 0.021(3) 0.016(3) 0.010(2) 0.009(2) 0.009(2) C3 0.024(3) 0.023(3) 0.023(3) 0.008(2) 0.015(2) 0.003(2) C4 0.085(6) 0.044(5) 0.057(5) -0.007(4) 0.061(5) -0.010(4) C5 0.032(3) 0.034(3) 0.029(3) 0.012(3) 0.014(3) 0.007(3) C6 0.027(4) 0.079(6) 0.076(6) 0.067(5) 0.017(4) 0.013(4) C7 0.021(3) 0.017(3) 0.018(3) 0.007(2) 0.008(2) 0.010(2) C8 0.024(3) 0.019(3) 0.029(3) 0.006(2) 0.010(2) 0.012(2) C9 0.039(3) 0.029(3) 0.037(4) 0.007(3) 0.022(3) 0.023(3) C10 0.026(3) 0.035(3) 0.043(4) 0.018(3) 0.020(3) 0.018(3) C11 0.017(3) 0.023(3) 0.037(3) 0.008(3) 0.006(3) 0.004(2) C12 0.026(3) 0.018(3) 0.022(3) 0.005(2) 0.012(2) 0.011(2) C13 0.022(3) 0.012(2) 0.023(3) 0.004(2) 0.012(2) 0.008(2) C14 0.022(3) 0.019(3) 0.021(3) 0.003(2) 0.007(2) 0.009(2) C15 0.036(3) 0.026(3) 0.031(3) 0.012(3) 0.013(3) 0.019(3) C16 0.042(4) 0.019(3) 0.044(4) 0.015(3) 0.023(3) 0.017(3) C17 0.032(3) 0.017(3) 0.036(4) 0.005(3) 0.013(3) 0.005(3) C18 0.022(3) 0.018(3) 0.027(3) 0.002(2) 0.007(2) 0.004(2) C19 0.028(3) 0.016(3) 0.022(3) 0.010(2) 0.020(2) 0.010(2) C20 0.033(3) 0.022(3) 0.023(3) 0.011(2) 0.015(3) 0.012(3) C21 0.032(3) 0.034(3) 0.021(3) 0.007(3) 0.012(3) 0.013(3) C22 0.031(3) 0.028(3) 0.025(3) 0.008(3) 0.014(3) 0.003(3) C23 0.037(4) 0.024(3) 0.042(4) 0.015(3) 0.020(3) 0.011(3) C24 0.030(3) 0.020(3) 0.039(4) 0.012(3) 0.020(3) 0.012(3) C25 0.031(3) 0.016(3) 0.018(3) 0.007(2) 0.014(2) 0.011(2) C26 0.036(3) 0.025(3) 0.027(3) 0.014(2) 0.022(3) 0.018(3) C27 0.049(4) 0.026(3) 0.025(3) 0.013(3) 0.021(3) 0.020(3) C28 0.040(4) 0.026(3) 0.023(3) 0.005(3) 0.010(3) 0.019(3) C29 0.028(3) 0.025(3) 0.026(3) 0.002(2) 0.008(3) 0.009(3) C30 0.028(3) 0.018(3) 0.019(3) 0.006(2) 0.011(2) 0.008(2) C31 0.025(3) 0.009(2) 0.028(3) 0.007(2) 0.012(2) 0.008(2) C32 0.023(3) 0.018(3) 0.039(3) 0.009(3) 0.017(3) 0.007(2) C33 0.022(3) 0.024(3) 0.053(4) 0.006(3) 0.018(3) 0.011(3) C34 0.028(3) 0.021(3) 0.036(4) -0.003(3) -0.005(3) 0.011(3) C35 0.042(4) 0.023(3) 0.030(3) 0.006(3) 0.012(3) 0.016(3) C36 0.031(3) 0.030(3) 0.031(3) 0.010(3) 0.015(3) 0.017(3) C37 0.026(3) 0.011(2) 0.023(3) 0.005(2) 0.015(2) 0.008(2) C38 0.025(3) 0.024(3) 0.033(3) 0.012(3) 0.018(3) 0.013(2) C39 0.026(3) 0.028(3) 0.027(3) -0.001(3) 0.013(3) 0.010(3) C40 0.030(3) 0.022(3) 0.034(3) 0.003(3) 0.024(3) 0.004(2) C41 0.040(4) 0.017(3) 0.031(3) 0.008(2) 0.021(3) 0.008(3) C42 0.034(3) 0.018(3) 0.028(3) 0.010(2) 0.014(3) 0.013(3) C43 0.024(3) 0.025(3) 0.019(3) 0.008(2) 0.010(2) 0.010(2) Cl1 0.0448(9) 0.0428(9) 0.0299(8) 0.0193(7) 0.0152(7) 0.0179(8) Cl2 0.0338(8) 0.0318(8) 0.0531(10) 0.0148(7) 0.0184(7) 0.0193(7) Cl3 0.0281(7) 0.0337(8) 0.0412(9) 0.0155(7) 0.0186(7) 0.0115(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C1 2.024(5) . ? Pt P2 2.2931(14) . ? Pt P3 2.3232(14) . ? Pt P1 2.3446(13) . ? Pt Tl 3.1090(11) . ? Tl O1 2.468(4) 2 ? Tl O1 2.538(3) . ? P1 O1 1.550(4) . ? P1 C13 1.826(5) . ? P1 C7 1.831(5) . ? P2 O2 1.578(4) . ? P2 C25 1.815(5) . ? P2 C19 1.824(5) . ? P3 O3 1.542(4) . ? P3 C37 1.809(5) . ? P3 C31 1.819(5) . ? O1 Tl 2.468(4) 2 ? C1 C2 1.196(7) . ? C2 C3 1.482(7) . ? C3 C5 1.521(8) . ? C3 C4 1.521(9) . ? C3 C6 1.525(9) . ? C7 C12 1.382(7) . ? C7 C8 1.396(7) . ? C8 C9 1.378(8) . ? C9 C10 1.384(8) . ? C10 C11 1.378(9) . ? C11 C12 1.387(8) . ? C13 C14 1.389(7) . ? C13 C18 1.390(7) . ? C14 C15 1.379(8) . ? C15 C16 1.379(8) . ? C16 C17 1.378(9) . ? C17 C18 1.393(8) . ? C19 C20 1.387(8) . ? C19 C24 1.389(7) . ? C20 C21 1.383(8) . ? C21 C22 1.374(8) . ? C22 C23 1.379(9) . ? C23 C24 1.383(8) . ? C25 C30 1.395(8) . ? C25 C26 1.396(7) . ? C26 C27 1.385(8) . ? C27 C28 1.379(9) . ? C28 C29 1.372(8) . ? C29 C30 1.389(8) . ? C31 C36 1.389(8) . ? C31 C32 1.407(8) . ? C32 C33 1.384(8) . ? C33 C34 1.375(9) . ? C34 C35 1.397(9) . ? C35 C36 1.372(8) . ? C37 C38 1.383(8) . ? C37 C42 1.404(7) . ? C38 C39 1.388(8) . ? C39 C40 1.383(8) . ? C40 C41 1.384(9) . ? C41 C42 1.382(8) . ? C43 Cl2 1.756(6) . ? C43 Cl3 1.756(5) . ? C43 Cl1 1.762(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 C1 Pt P2 175.58(16) . . ? C1 Pt P3 85.60(15) . . ? P2 Pt P3 92.86(5) . . ? C1 Pt P1 82.49(15) . . ? P2 Pt P1 99.46(5) . . ? P3 Pt P1 166.61(5) . . ? C1 Pt Tl 81.54(15) . . ? P2 Pt Tl 102.79(4) . . ? P3 Pt Tl 98.07(4) . . ? P1 Pt Tl 74.18(4) . . ? O1 Tl O1 77.69(12) 2 . ? O1 Tl Pt 116.39(8) 2 . ? O1 Tl Pt 67.44(8) . . ? O1 P1 C13 104.2(2) . . ? O1 P1 C7 108.8(2) . . ? C13 P1 C7 99.9(2) . . ? O1 P1 Pt 107.24(14) . . ? C13 P1 Pt 123.09(17) . . ? C7 P1 Pt 112.71(17) . . ? O2 P2 C25 105.1(2) . . ? O2 P2 C19 101.9(2) . . ? C25 P2 C19 107.4(2) . . ? O2 P2 Pt 115.39(15) . . ? C25 P2 Pt 112.69(18) . . ? C19 P2 Pt 113.44(17) . . ? O3 P3 C37 105.9(2) . . ? O3 P3 C31 105.7(2) . . ? C37 P3 C31 106.3(2) . . ? O3 P3 Pt 116.93(15) . . ? C37 P3 Pt 111.71(17) . . ? C31 P3 Pt 109.65(17) . . ? P1 O1 Tl 131.2(2) . 2 ? P1 O1 Tl 107.36(18) . . ? Tl O1 Tl 102.31(12) 2 . ? C2 C1 Pt 170.6(5) . . ? C1 C2 C3 173.1(6) . . ? C2 C3 C5 107.9(5) . . ? C2 C3 C4 108.9(5) . . ? C5 C3 C4 108.8(6) . . ? C2 C3 C6 110.3(5) . . ? C5 C3 C6 108.1(5) . . ? C4 C3 C6 112.8(6) . . ? C12 C7 C8 118.8(5) . . ? C12 C7 P1 123.2(4) . . ? C8 C7 P1 118.0(4) . . ? C9 C8 C7 120.7(5) . . ? C8 C9 C10 119.9(5) . . ? C11 C10 C9 120.0(5) . . ? C10 C11 C12 120.1(5) . . ? C7 C12 C11 120.5(5) . . ? C14 C13 C18 119.4(5) . . ? C14 C13 P1 122.7(4) . . ? C18 C13 P1 118.0(4) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 119.9(5) . . ? C17 C16 C15 120.5(6) . . ? C16 C17 C18 119.7(5) . . ? C13 C18 C17 119.9(5) . . ? C20 C19 C24 118.9(5) . . ? C20 C19 P2 115.9(4) . . ? C24 C19 P2 125.1(4) . . ? C21 C20 C19 121.0(5) . . ? C22 C21 C20 119.6(6) . . ? C21 C22 C23 120.0(6) . . ? C22 C23 C24 120.6(6) . . ? C23 C24 C19 119.8(6) . . ? C30 C25 C26 119.2(5) . . ? C30 C25 P2 119.2(4) . . ? C26 C25 P2 121.5(4) . . ? C27 C26 C25 119.7(5) . . ? C28 C27 C26 120.2(5) . . ? C29 C28 C27 120.8(6) . . ? C28 C29 C30 119.6(6) . . ? C29 C30 C25 120.3(5) . . ? C36 C31 C32 118.0(5) . . ? C36 C31 P3 124.3(4) . . ? C32 C31 P3 117.7(4) . . ? C33 C32 C31 120.3(6) . . ? C34 C33 C32 120.5(6) . . ? C33 C34 C35 119.9(6) . . ? C36 C35 C34 119.4(6) . . ? C35 C36 C31 121.9(6) . . ? C38 C37 C42 118.7(5) . . ? C38 C37 P3 117.5(4) . . ? C42 C37 P3 123.6(4) . . ? C37 C38 C39 121.5(5) . . ? C40 C39 C38 119.2(6) . . ? C39 C40 C41 120.2(5) . . ? C42 C41 C40 120.5(5) . . ? C41 C42 C37 119.9(5) . . ? Cl2 C43 Cl3 110.5(3) . . ? Cl2 C43 Cl1 109.7(3) . . ? Cl3 C43 Cl1 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.987 _refine_diff_density_min -1.567 _refine_diff_density_rms 0.124 #===END #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 642393' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common s63 _chemical_formula_sum 'C42 H41 O3 P3 Pt' _chemical_formula_weight 881.75 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.1175(4) _cell_length_b 18.3866(4) _cell_length_c 24.3578(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7666.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(10) _cell_measurement_reflns_used 10071 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description sheet _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7045 _exptl_absorpt_correction_T_max 0.8194 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100.0(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0146858 _diffrn_orient_matrix_ub_12 -0.0119785 _diffrn_orient_matrix_ub_13 0.0386938 _diffrn_orient_matrix_ub_21 0.0443338 _diffrn_orient_matrix_ub_22 -0.0304325 _diffrn_orient_matrix_ub_23 -0.013678 _diffrn_orient_matrix_ub_31 0.0350957 _diffrn_orient_matrix_ub_32 0.0434554 _diffrn_orient_matrix_ub_33 0.001087 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.1823 _diffrn_reflns_av_unetI/netI 0.0724 _diffrn_reflns_number 110865 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 7514 _reflns_number_gt 5251 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0000P)^2^+58.3521P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7514 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.142 _refine_diff_density_min -1.502 _refine_diff_density_rms 0.176 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.084471(13) 0.218795(13) 0.695714(10) 0.00747(7) Uani 1 1 d . . . P1 P 0.21911(8) 0.20577(9) 0.69080(7) 0.0089(4) Uani 1 1 d . . . P2 P 0.08728(10) 0.26833(9) 0.78191(6) 0.0126(4) Uani 1 1 d . . . P3 P -0.05003(9) 0.22831(9) 0.68932(7) 0.0089(4) Uani 1 1 d . . . O1 O 0.2652(2) 0.2401(2) 0.73943(18) 0.0118(11) Uani 1 1 d . . . O2 O 0.1683(3) 0.3036(3) 0.7996(2) 0.0211(12) Uani 1 1 d . . . O3 O -0.0891(3) 0.2328(2) 0.74773(17) 0.0137(10) Uani 1 1 d . . . C1 C -0.1009(3) 0.1552(4) 0.6534(3) 0.0108(7) Uani 1 1 d . . . C2 C -0.1743(4) 0.1661(4) 0.6307(3) 0.0135(15) Uani 1 1 d . . . H44 H -0.1962 0.2124 0.6306 0.016 Uiso 1 1 calc R . . C3 C -0.2146(4) 0.1086(4) 0.6082(3) 0.0170(16) Uani 1 1 d . . . H3 H -0.2639 0.1161 0.5932 0.02 Uiso 1 1 calc R . . C4 C -0.1823(4) 0.0396(4) 0.6079(3) 0.0190(17) Uani 1 1 d . . . H4 H -0.2096 0.0009 0.5925 0.023 Uiso 1 1 calc R . . C5 C -0.1096(4) 0.0284(4) 0.6304(3) 0.0189(17) Uani 1 1 d . . . H5 H -0.0879 -0.018 0.6302 0.023 Uiso 1 1 calc R . . C6 C -0.0684(4) 0.0856(3) 0.6534(3) 0.0122(16) Uani 1 1 d . . . H6 H -0.0194 0.0777 0.6688 0.015 Uiso 1 1 calc R . . C7 C -0.0787(4) 0.3077(3) 0.6510(3) 0.0108(14) Uani 1 1 d . . . C8 C -0.0552(4) 0.3157(4) 0.5966(3) 0.0211(18) Uani 1 1 d . . . H8 H -0.023 0.2808 0.5808 0.025 Uiso 1 1 calc R . . C9 C -0.0791(5) 0.3747(4) 0.5661(3) 0.0287(19) Uani 1 1 d . . . H9 H -0.0635 0.379 0.5296 0.034 Uiso 1 1 calc R . . C10 C -0.1263(4) 0.4276(4) 0.5894(3) 0.0266(19) Uani 1 1 d . . . H10 H -0.1425 0.4675 0.5689 0.032 Uiso 1 1 calc R . . C11 C -0.1491(4) 0.4203(4) 0.6437(3) 0.0241(18) Uani 1 1 d . . . H11 H -0.18 0.4561 0.6597 0.029 Uiso 1 1 calc R . . C12 C -0.1268(4) 0.3610(4) 0.6742(3) 0.0183(17) Uani 1 1 d . . . H12 H -0.1436 0.3563 0.7103 0.022 Uiso 1 1 calc R . . C13 C 0.2477(4) 0.1103(3) 0.6891(3) 0.0108(7) Uani 1 1 d . . . C14 C 0.2659(4) 0.0758(4) 0.7378(3) 0.0161(16) Uani 1 1 d . . . H14 H 0.2646 0.1017 0.7706 0.019 Uiso 1 1 calc R . . C15 C 0.2858(4) 0.0029(4) 0.7380(3) 0.0215(18) Uani 1 1 d . . . H15 H 0.2986 -0.0197 0.771 0.026 Uiso 1 1 calc R . . C16 C 0.2869(4) -0.0365(4) 0.6902(3) 0.0217(17) Uani 1 1 d . . . H16 H 0.2995 -0.0857 0.6908 0.026 Uiso 1 1 calc R . . C17 C 0.2694(4) -0.0028(4) 0.6413(3) 0.0164(17) Uani 1 1 d . . . H17 H 0.2709 -0.0292 0.6088 0.02 Uiso 1 1 calc R . . C18 C 0.2497(4) 0.0699(4) 0.6404(3) 0.0151(17) Uani 1 1 d . . . H18 H 0.2376 0.0922 0.6072 0.018 Uiso 1 1 calc R . . C19 C 0.2586(4) 0.2444(4) 0.6275(3) 0.0108(7) Uani 1 1 d . . . C20 C 0.2177(4) 0.2970(4) 0.5986(3) 0.0150(17) Uani 1 1 d . . . H20 H 0.1692 0.3123 0.6112 0.018 Uiso 1 1 calc R . . C21 C 0.2483(4) 0.3269(4) 0.5511(3) 0.0183(16) Uani 1 1 d . . . H21 H 0.221 0.363 0.5324 0.022 Uiso 1 1 calc R . . C22 C 0.3192(4) 0.3032(4) 0.5315(3) 0.0220(18) Uani 1 1 d . . . H22 H 0.3393 0.3223 0.4991 0.026 Uiso 1 1 calc R . . C23 C 0.3606(4) 0.2511(4) 0.5600(3) 0.0226(17) Uani 1 1 d . . . H23 H 0.4088 0.2354 0.5468 0.027 Uiso 1 1 calc R . . C24 C 0.3309(3) 0.2219(4) 0.6082(3) 0.0155(15) Uani 1 1 d . . . H24 H 0.3594 0.1873 0.6275 0.019 Uiso 1 1 calc R . . C25 C 0.0869(4) 0.1763(3) 0.6196(2) 0.0103(13) Uani 1 1 d . . . C26 C 0.0925(4) 0.1486(3) 0.5755(3) 0.0112(14) Uani 1 1 d . . . C27 C 0.0979(4) 0.1136(4) 0.5204(3) 0.0142(15) Uani 1 1 d . . . C28 C 0.0993(4) 0.0308(4) 0.5278(3) 0.0204(17) Uani 1 1 d . . . H28A H 0.1452 0.0171 0.548 0.031 Uiso 1 1 calc R . . H28B H 0.1002 0.0077 0.4924 0.031 Uiso 1 1 calc R . . H28C H 0.0536 0.0157 0.5475 0.031 Uiso 1 1 calc R . . C29 C 0.1715(4) 0.1397(4) 0.4908(3) 0.0204(17) Uani 1 1 d . . . H29A H 0.1706 0.1917 0.488 0.031 Uiso 1 1 calc R . . H29B H 0.1733 0.1188 0.4547 0.031 Uiso 1 1 calc R . . H29C H 0.2168 0.1248 0.5111 0.031 Uiso 1 1 calc R . . C30 C 0.0254(4) 0.1350(4) 0.4875(3) 0.0226(18) Uani 1 1 d . . . H30A H -0.0205 0.1188 0.5064 0.034 Uiso 1 1 calc R . . H30B H 0.0276 0.1127 0.4519 0.034 Uiso 1 1 calc R . . H30C H 0.0238 0.1869 0.4834 0.034 Uiso 1 1 calc R . . C31 C 0.0211(3) 0.3449(3) 0.7929(3) 0.0108(7) Uani 1 1 d . . . C32 C 0.0254(4) 0.4022(3) 0.7561(3) 0.0134(15) Uani 1 1 d . . . H32 H 0.0614 0.4007 0.7276 0.016 Uiso 1 1 calc R . . C33 C -0.0235(4) 0.4613(4) 0.7617(3) 0.0212(17) Uani 1 1 d . . . H33 H -0.0207 0.4995 0.7367 0.025 Uiso 1 1 calc R . . C34 C -0.0765(4) 0.4641(3) 0.8041(3) 0.0183(14) Uani 1 1 d . . . H34 H -0.1089 0.5044 0.8081 0.022 Uiso 1 1 calc R . . C35 C -0.0816(4) 0.4060(4) 0.8412(3) 0.0161(15) Uani 1 1 d . . . H35 H -0.1183 0.4072 0.8694 0.019 Uiso 1 1 calc R . . C36 C -0.0318(4) 0.3469(4) 0.8361(3) 0.0147(16) Uani 1 1 d . . . H36 H -0.0339 0.3089 0.8613 0.018 Uiso 1 1 calc R . . C37 C 0.0652(3) 0.2032(3) 0.8361(3) 0.0108(7) Uani 1 1 d . . . C38 C 0.0219(4) 0.1415(4) 0.8261(3) 0.0266(13) Uani 1 1 d . . . H38 H 0.0034 0.1321 0.7909 0.032 Uiso 1 1 calc R . . C39 C 0.0058(5) 0.0935(5) 0.8682(3) 0.036(2) Uani 1 1 d . . . H39 H -0.0236 0.052 0.8613 0.043 Uiso 1 1 calc R . . C40 C 0.0333(6) 0.1068(5) 0.9206(3) 0.043(3) Uani 1 1 d . . . H40 H 0.0231 0.0741 0.9488 0.051 Uiso 1 1 calc R . . C41 C 0.0758(5) 0.1685(5) 0.9307(3) 0.034(2) Uani 1 1 d . . . H41 H 0.0929 0.1784 0.9661 0.041 Uiso 1 1 calc R . . C42 C 0.0933(4) 0.2163(5) 0.8886(3) 0.0266(13) Uani 1 1 d . . . H42 H 0.1239 0.2571 0.8955 0.032 Uiso 1 1 calc R . . H2 H -0.136(4) 0.241(4) 0.752(3) 0.03(2) Uiso 1 1 d . . . H1 H 0.204(4) 0.289(4) 0.779(3) 0.02(2) Uiso 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 0.00309(10) 0.01180(11) 0.00753(11) -0.00365(13) 0.00024(12) 0.00058(12) P1 0.0035(7) 0.0128(9) 0.0104(9) -0.0046(8) -0.0008(7) 0.0006(6) P2 0.0073(7) 0.0189(10) 0.0116(8) -0.0076(7) -0.0014(8) 0.0013(8) P3 0.0052(7) 0.0108(9) 0.0107(9) -0.0011(8) -0.0002(7) 0.0018(7) O1 0.006(2) 0.016(3) 0.013(2) -0.009(2) 0.0010(19) 0.0022(19) O2 0.006(2) 0.035(3) 0.022(3) -0.019(3) -0.001(2) 0.001(2) O3 0.007(2) 0.020(3) 0.014(2) -0.003(2) 0.005(2) 0.002(2) C1 0.0088(15) 0.0127(16) 0.0111(16) -0.0024(13) -0.0006(12) 0.0007(12) C2 0.006(3) 0.019(4) 0.016(4) 0.003(3) -0.001(3) 0.000(3) C3 0.009(3) 0.028(5) 0.013(4) -0.005(3) -0.002(3) -0.009(3) C4 0.015(4) 0.022(4) 0.020(4) -0.004(4) 0.007(3) -0.010(3) C5 0.017(4) 0.020(4) 0.019(4) 0.003(4) 0.012(3) 0.002(3) C6 0.014(4) 0.014(4) 0.009(3) 0.003(3) -0.002(3) -0.008(3) C7 0.005(3) 0.008(3) 0.019(4) -0.003(3) -0.002(3) -0.004(3) C8 0.026(4) 0.020(4) 0.017(4) 0.003(3) 0.013(3) 0.007(3) C9 0.035(5) 0.035(5) 0.016(4) 0.012(4) 0.012(4) 0.001(4) C10 0.026(4) 0.019(4) 0.035(5) 0.012(4) -0.001(4) 0.006(3) C11 0.020(4) 0.019(4) 0.033(5) 0.001(4) -0.001(4) 0.005(3) C12 0.017(4) 0.015(4) 0.024(4) -0.001(3) 0.002(3) 0.003(3) C13 0.0088(15) 0.0127(16) 0.0111(16) -0.0024(13) -0.0006(12) 0.0007(12) C14 0.012(4) 0.015(4) 0.021(4) 0.000(3) 0.000(3) -0.003(3) C15 0.017(4) 0.024(4) 0.023(4) 0.006(4) -0.013(3) 0.002(3) C16 0.020(4) 0.014(4) 0.031(5) 0.000(4) -0.009(4) 0.004(3) C17 0.011(4) 0.017(4) 0.021(4) -0.004(3) -0.003(3) 0.006(3) C18 0.005(3) 0.025(4) 0.015(4) -0.004(3) -0.003(3) -0.001(3) C19 0.0088(15) 0.0127(16) 0.0111(16) -0.0024(13) -0.0006(12) 0.0007(12) C20 0.013(3) 0.016(4) 0.016(4) -0.010(3) 0.004(3) -0.002(3) C21 0.030(4) 0.011(4) 0.014(4) 0.003(3) -0.005(3) -0.010(3) C22 0.026(4) 0.030(5) 0.010(4) 0.001(3) 0.001(3) -0.017(4) C23 0.014(3) 0.032(4) 0.022(4) -0.008(4) 0.005(3) -0.011(4) C24 0.012(3) 0.016(4) 0.019(4) -0.004(4) 0.003(3) -0.002(3) C25 0.007(3) 0.014(3) 0.010(3) -0.004(3) 0.005(3) -0.001(3) C26 0.008(3) 0.013(3) 0.013(4) 0.004(3) 0.003(3) 0.002(3) C27 0.017(4) 0.015(4) 0.010(4) -0.002(3) -0.001(3) -0.004(3) C28 0.020(4) 0.026(4) 0.015(4) -0.004(3) 0.002(3) -0.005(3) C29 0.017(4) 0.030(5) 0.014(4) 0.000(4) 0.003(3) -0.002(3) C30 0.025(4) 0.026(5) 0.017(4) 0.000(4) -0.013(3) 0.001(4) C31 0.0088(15) 0.0127(16) 0.0111(16) -0.0024(13) -0.0006(12) 0.0007(12) C32 0.014(4) 0.012(4) 0.014(4) -0.007(3) 0.005(3) -0.010(3) C33 0.025(4) 0.017(4) 0.022(4) 0.001(3) 0.003(3) -0.006(3) C34 0.009(3) 0.013(3) 0.033(4) -0.008(4) -0.007(4) 0.001(3) C35 0.017(3) 0.019(4) 0.012(4) -0.009(3) 0.002(3) 0.003(4) C36 0.013(4) 0.019(4) 0.013(4) -0.001(3) 0.003(3) 0.000(3) C37 0.0088(15) 0.0127(16) 0.0111(16) -0.0024(13) -0.0006(12) 0.0007(12) C38 0.038(3) 0.034(3) 0.008(2) 0.001(3) 0.007(2) 0.016(3) C39 0.062(6) 0.022(5) 0.024(5) -0.003(4) 0.009(4) 0.005(4) C40 0.071(7) 0.040(6) 0.017(5) 0.015(4) 0.017(5) 0.043(5) C41 0.049(5) 0.038(5) 0.015(4) -0.001(4) -0.004(4) 0.028(5) C42 0.038(3) 0.034(3) 0.008(2) 0.001(3) 0.007(2) 0.016(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C25 2.013(6) . ? Pt1 P2 2.2892(16) . ? Pt1 P3 2.3141(15) . ? Pt1 P1 2.3202(15) . ? P1 O1 1.557(4) . ? P1 C13 1.823(6) . ? P1 C19 1.827(7) . ? P2 O2 1.591(5) . ? P2 C37 1.821(6) . ? P2 C31 1.827(6) . ? P3 O3 1.574(5) . ? P3 C7 1.802(6) . ? P3 C1 1.826(6) . ? C1 C2 1.387(8) . ? C1 C6 1.395(9) . ? C2 C3 1.376(9) . ? C2 H44 0.93 . ? C3 C4 1.384(10) . ? C3 H3 0.93 . ? C4 C5 1.375(9) . ? C4 H4 0.93 . ? C5 C6 1.385(9) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.391(9) . ? C7 C12 1.399(9) . ? C8 C9 1.377(10) . ? C8 H8 0.93 . ? C9 C10 1.388(10) . ? C9 H9 0.93 . ? C10 C11 1.384(10) . ? C10 H10 0.93 . ? C11 C12 1.374(10) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.381(9) . ? C13 C18 1.401(9) . ? C14 C15 1.384(9) . ? C14 H14 0.93 . ? C15 C16 1.372(10) . ? C15 H15 0.93 . ? C16 C17 1.375(10) . ? C16 H16 0.93 . ? C17 C18 1.379(9) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 C20 1.385(9) . ? C19 C24 1.387(9) . ? C20 C21 1.385(9) . ? C20 H20 0.93 . ? C21 C22 1.375(10) . ? C21 H21 0.93 . ? C22 C23 1.380(10) . ? C22 H22 0.93 . ? C23 C24 1.387(9) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C26 1.191(8) . ? C26 C27 1.492(9) . ? C27 C29 1.528(9) . ? C27 C30 1.529(9) . ? C27 C28 1.534(9) . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? C30 H30A 0.96 . ? C30 H30B 0.96 . ? C30 H30C 0.96 . ? C31 C32 1.384(9) . ? C31 C36 1.390(9) . ? C32 C33 1.380(9) . ? C32 H32 0.93 . ? C33 C34 1.375(9) . ? C33 H33 0.93 . ? C34 C35 1.403(9) . ? C34 H34 0.93 . ? C35 C36 1.387(9) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C37 C38 1.377(10) . ? C37 C42 1.388(9) . ? C38 C39 1.380(10) . ? C38 H38 0.93 . ? C39 C40 1.382(11) . ? C39 H39 0.93 . ? C40 C41 1.369(12) . ? C40 H40 0.93 . ? C41 C42 1.383(10) . ? C41 H41 0.93 . ? C42 H42 0.93 . ? O2 H1 0.84(7) . ? O3 H2 0.83(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 C25 Pt1 P2 177.52(19) . . ? C25 Pt1 P3 89.33(19) . . ? P2 Pt1 P3 93.01(6) . . ? C25 Pt1 P1 83.77(19) . . ? P2 Pt1 P1 93.87(6) . . ? P3 Pt1 P1 173.00(6) . . ? O1 P1 C13 105.8(3) . . ? O1 P1 C19 107.2(3) . . ? C13 P1 C19 104.8(3) . . ? O1 P1 Pt1 114.98(17) . . ? C13 P1 Pt1 111.6(2) . . ? C19 P1 Pt1 111.8(2) . . ? O2 P2 C37 104.6(3) . . ? O2 P2 C31 100.8(3) . . ? C37 P2 C31 105.8(3) . . ? O2 P2 Pt1 115.4(2) . . ? C37 P2 Pt1 113.5(2) . . ? C31 P2 Pt1 115.3(2) . . ? O3 P3 C7 108.1(3) . . ? O3 P3 C1 105.6(3) . . ? C7 P3 C1 102.6(3) . . ? O3 P3 Pt1 111.44(19) . . ? C7 P3 Pt1 111.5(2) . . ? C1 P3 Pt1 116.8(2) . . ? C2 C1 C6 119.6(6) . . ? C2 C1 P3 121.1(5) . . ? C6 C1 P3 119.0(5) . . ? C3 C2 C1 120.1(7) . . ? C3 C2 H44 119.9 . . ? C1 C2 H44 119.9 . . ? C2 C3 C4 120.4(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.8(7) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.5(7) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 119.6(6) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C8 C7 C12 118.8(6) . . ? C8 C7 P3 120.0(5) . . ? C12 C7 P3 121.2(5) . . ? C9 C8 C7 120.8(7) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.2(7) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.1(7) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C12 C11 C10 121.1(7) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C7 120.0(7) . . ? C11 C12 H12 120 . . ? C7 C12 H12 120 . . ? C14 C13 C18 118.6(6) . . ? C14 C13 P1 118.9(5) . . ? C18 C13 P1 122.5(5) . . ? C13 C14 C15 120.3(7) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.7(7) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 119.7(7) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.2(7) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.4(7) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C20 C19 C24 119.0(6) . . ? C20 C19 P1 120.9(5) . . ? C24 C19 P1 120.0(5) . . ? C21 C20 C19 120.8(6) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 119.8(7) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.0(7) . . ? C21 C22 H22 120 . . ? C23 C22 H22 120 . . ? C22 C23 C24 120.4(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 120.0(7) . . ? C23 C24 H24 120 . . ? C19 C24 H24 120 . . ? C26 C25 Pt1 175.8(6) . . ? C25 C26 C27 179.0(7) . . ? C26 C27 C29 109.9(5) . . ? C26 C27 C30 108.1(6) . . ? C29 C27 C30 109.9(5) . . ? C26 C27 C28 108.9(5) . . ? C29 C27 C28 110.7(6) . . ? C30 C27 C28 109.2(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 120.3(6) . . ? C32 C31 P2 117.3(5) . . ? C36 C31 P2 122.4(5) . . ? C33 C32 C31 120.3(6) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.2(7) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 119.8(6) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 120.0(6) . . ? C36 C35 H35 120 . . ? C34 C35 H35 120 . . ? C35 C36 C31 119.3(6) . . ? C35 C36 H36 120.4 . . ? C31 C36 H36 120.4 . . ? C38 C37 C42 119.4(7) . . ? C38 C37 P2 121.7(5) . . ? C42 C37 P2 118.8(5) . . ? C37 C38 C39 120.2(7) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C40 120.3(8) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 119.6(8) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 120.5(8) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 119.9(8) . . ? C41 C42 H42 120.1 . . ? C37 C42 H42 120.1 . . ? P2 O2 H1 111(5) . . ? P3 O3 H2 122(5) . . ?