Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Parola, Stephane' 'Cedric, Desroches' 'Vadim, Kessler' 'Cesar, Lopes' _publ_contact_author_name 'Dr Stephane Parola' _publ_contact_author_address ; Dr Stephane Parola LMI UMR CNRS 5615 Universite Claude Bernard Lyon1 Bat. Berthollet, 43 Bd 11 novembre Villeurbanne 69622 FRANCE ; _publ_contact_author_email 'STEPHANE.PAROLA@UNIV-LYON1.FR' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Design and synthesis of multifunctional thiacalixarenes and related metal derivatives for the preparation of sol-gel hybrid materials with non linear optical properties ; data_calix1tm _database_code_CSD 193184 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H96 O4 S4' _chemical_formula_weight 1345.89 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.009(4) _cell_length_b 23.370(4) _cell_length_c 17.968(3) _cell_angle_alpha 90.00 _cell_angle_beta 125.796(15) _cell_angle_gamma 90.00 _cell_volume 7837(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 999(I>2sigma(I)) _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 20.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 1.20 _exptl_crystal_size_mid 1.00 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8220 _exptl_absorpt_correction_T_max 0.9429 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 Bruker SMART CCD 1k _diffrn_measurement_method Bruker SMART _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11918 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 20.00 _reflns_number_total 3654 _reflns_number_gt 2045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0965P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3654 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1195 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 S1 S 0.70634(8) 0.14886(6) 0.96347(10) 0.0788(5) Uani 1 1 d . . . S2 S 0.55451(9) 0.15080(6) 0.58353(10) 0.0811(6) Uani 1 1 d . . . O1 O 0.43469(19) 0.09734(16) 0.5859(2) 0.0756(11) Uani 1 1 d . . . O2 O 0.6122(2) 0.20252(16) 0.7712(2) 0.0801(12) Uani 1 1 d . . . C201 C 0.6272(3) 0.1459(2) 0.7728(4) 0.0623(14) Uani 1 1 d . . . C202 C 0.6676(3) 0.1158(2) 0.8558(4) 0.0612(15) Uani 1 1 d . . . C102 C 0.6410(3) 0.2410(2) 0.9699(3) 0.0708(16) Uani 1 1 d . . . H10A H 0.6821 0.2599 0.9848 0.085 Uiso 1 1 calc R . . C205 C 0.6579(3) 0.0293(2) 0.7750(5) 0.0764(17) Uani 1 1 d . . . C203 C 0.6166(3) 0.0596(3) 0.6934(4) 0.0763(16) Uani 1 1 d . . . H20A H 0.5993 0.0407 0.6386 0.092 Uiso 1 1 calc R . . C204 C 0.6002(3) 0.1171(2) 0.6905(4) 0.0650(15) Uani 1 1 d . . . C117 C 0.4267(4) 0.1551(2) 0.5660(3) 0.0643(14) Uani 1 1 d . . . C8 C 0.6827(3) 0.0588(2) 0.8554(4) 0.0726(16) Uani 1 1 d . . . H8A H 0.7105 0.0394 0.9110 0.087 Uiso 1 1 calc R . . C118 C 0.4813(3) 0.1851(2) 0.5703(3) 0.0627(15) Uani 1 1 d . . . C105 C 0.5816(5) 0.4449(3) 0.9775(7) 0.096(2) Uani 1 1 d . . . C101 C 0.6339(3) 0.1835(2) 0.9529(3) 0.0620(15) Uani 1 1 d . . . C111 C 0.5616(5) 0.5618(3) 0.9743(8) 0.108(2) Uani 1 1 d . . . C119 C 0.4732(3) 0.2430(2) 0.5540(3) 0.0729(16) Uani 1 1 d . . . H119 H 0.5088 0.2634 0.5559 0.087 Uiso 1 1 calc R . . C110 C 0.5150(4) 0.5283(4) 0.9015(7) 0.153(3) Uani 1 1 d . . . H11E H 0.4751 0.5449 0.8493 0.184 Uiso 1 1 calc R . . C209 C 0.7352(4) -0.1685(3) 0.8549(6) 0.121(2) Uani 1 1 d . . . H20B H 0.7627 -0.1480 0.9095 0.146 Uiso 1 1 calc R . . C103 C 0.5869(4) 0.2717(2) 0.9652(3) 0.0718(16) Uani 1 1 d . . . C109 C 0.6194(5) 0.5352(4) 1.0489(6) 0.116(2) Uani 1 1 d . . . H10D H 0.6530 0.5571 1.0995 0.139 Uiso 1 1 calc R . . C104 C 0.5906(3) 0.3338(3) 0.9768(4) 0.0858(19) Uani 1 1 d . . . C114 C 0.5583(4) 0.7239(2) 0.9160(5) 0.114(2) Uani 1 1 d . . . H11F H 0.5075 0.7321 0.8819 0.137 Uiso 1 1 calc R . . H11G H 0.5808 0.7362 0.9788 0.137 Uiso 1 1 calc R . . C107 C 0.6292(4) 0.4779(3) 1.0515(5) 0.107(2) Uani 1 1 d . . . H10E H 0.6686 0.4610 1.1038 0.128 Uiso 1 1 calc R . . C208 C 0.6863(4) -0.1406(3) 0.7759(5) 0.0846(18) Uani 1 1 d . . . C112 C 0.5478(4) 0.6258(3) 0.9680(6) 0.137(3) Uani 1 1 d . . . H11H H 0.4972 0.6318 0.9396 0.164 Uiso 1 1 calc R . . H11I H 0.5740 0.6411 1.0297 0.164 Uiso 1 1 calc R . . C210 C 0.6460(4) -0.1733(3) 0.6988(5) 0.102(2) Uani 1 1 d . . . H21A H 0.6113 -0.1557 0.6436 0.122 Uiso 1 1 calc R . . C401 C 0.6657(4) 0.2404(2) 0.7798(5) 0.123(3) Uani 1 1 d . . . C214 C 0.7167(5) -0.3245(3) 0.7806(6) 0.150(3) Uani 1 1 d . . . H21B H 0.6938 -0.3378 0.7182 0.180 Uiso 1 1 calc R . . H21C H 0.7676 -0.3318 0.8139 0.180 Uiso 1 1 calc R . . C206 C 0.6702(3) -0.0310(3) 0.7756(4) 0.0872(19) Uani 1 1 d . . . C207 C 0.6771(3) -0.0807(3) 0.7751(4) 0.0856(19) Uani 1 1 d . . . C108 C 0.5255(5) 0.4705(4) 0.9032(7) 0.152(3) Uani 1 1 d . . . H10F H 0.4931 0.4486 0.8517 0.182 Uiso 1 1 calc R . . C113 C 0.5681(4) 0.6589(2) 0.9154(5) 0.112(2) Uani 1 1 d . . . H11J H 0.5394 0.6456 0.8523 0.134 Uiso 1 1 calc R . . H11K H 0.6179 0.6510 0.9410 0.134 Uiso 1 1 calc R . . C106 C 0.5893(4) 0.3847(3) 0.9799(5) 0.100(2) Uani 1 1 d . . . C215 C 0.6908(5) -0.3573(3) 0.8205(6) 0.158(3) Uani 1 1 d . . . H21C' H 0.6399 -0.3502 0.7883 0.189 Uiso 1 1 calc R . . H21D H 0.7145 -0.3454 0.8838 0.189 Uiso 1 1 calc R . . C213 C 0.7053(5) -0.2593(3) 0.7781(7) 0.104(2) Uani 1 1 d . . . C211 C 0.7450(4) -0.2278(3) 0.8555(6) 0.127(3) Uani 1 1 d . . . H21E H 0.7796 -0.2458 0.9104 0.153 Uiso 1 1 calc R . . C212 C 0.6551(5) -0.2317(3) 0.7000(5) 0.110(2) Uani 1 1 d . . . H21F H 0.6260 -0.2525 0.6460 0.132 Uiso 1 1 calc R . . C115 C 0.5879(4) 0.7575(3) 0.8767(5) 0.133(3) Uani 1 1 d . . . H11L H 0.5639 0.7468 0.8129 0.160 Uiso 1 1 calc R . . H11M H 0.6384 0.7486 0.9091 0.160 Uiso 1 1 calc R . . C216 C 0.7028(5) -0.4209(3) 0.8181(7) 0.168(4) Uani 1 1 d . . . H21G H 0.6764 -0.4335 0.7548 0.201 Uiso 1 1 calc R . . H21H H 0.7533 -0.4279 0.8469 0.201 Uiso 1 1 calc R . . C116 C 0.5794(5) 0.8211(3) 0.8824(6) 0.171(4) Uani 1 1 d . . . H11N H 0.5996 0.8414 0.8562 0.256 Uiso 1 1 calc R . . H11O H 0.6037 0.8320 0.9455 0.256 Uiso 1 1 calc R . . H11P H 0.5294 0.8303 0.8492 0.256 Uiso 1 1 calc R . . C303 C 0.4553(6) -0.0228(4) 0.6162(9) 0.237(6) Uani 1 1 d . . . H30A H 0.4466 -0.0631 0.6137 0.356 Uiso 1 1 calc R . . H30B H 0.4509 -0.0054 0.6611 0.356 Uiso 1 1 calc R . . H30C H 0.5028 -0.0165 0.6328 0.356 Uiso 1 1 calc R . . C302 C 0.4079(6) 0.0003(4) 0.5347(7) 0.170(4) Uani 1 1 d . . . H30D H 0.3743 -0.0245 0.4890 0.204 Uiso 1 1 calc R . . C301 C 0.4026(4) 0.0595(3) 0.5090(5) 0.119(2) Uani 1 1 d . . . H30E H 0.3524 0.0695 0.4656 0.143 Uiso 1 1 calc R . . H30F H 0.4258 0.0646 0.4785 0.143 Uiso 1 1 calc R . . C218 C 0.6808(5) -0.5151(4) 0.8519(7) 0.218(5) Uani 1 1 d . . . H21I H 0.6650 -0.5346 0.8842 0.327 Uiso 1 1 calc R . . H21J H 0.7285 -0.5271 0.8755 0.327 Uiso 1 1 calc R . . H21K H 0.6492 -0.5241 0.7877 0.327 Uiso 1 1 calc R . . C217 C 0.6802(6) -0.4531(3) 0.8647(8) 0.199(5) Uani 1 1 d . . . H21L H 0.6321 -0.4414 0.8422 0.239 Uiso 1 1 calc R . . H21M H 0.7115 -0.4444 0.9297 0.239 Uiso 1 1 calc R . . C402 C 0.6234(16) 0.3055(11) 0.7655(17) 0.159(10) Uiso 0.58(2) 1 d P . . C403 C 0.6729(8) 0.3425(6) 0.7677(9) 0.138(8) Uiso 0.58(2) 1 d P . . C40A C 0.6560(13) 0.2934(11) 0.7846(14) 0.106(10) Uiso 0.42(2) 1 d P . . C40B C 0.5940(15) 0.3222(11) 0.7599(17) 0.147(11) Uiso 0.42(2) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0627(11) 0.0867(10) 0.0751(11) -0.0065(9) 0.0337(9) 0.0029(9) S2 0.0866(13) 0.0978(11) 0.0800(11) 0.0152(9) 0.0605(11) 0.0197(9) O1 0.086(3) 0.067(2) 0.077(3) 0.007(2) 0.049(3) 0.006(2) O2 0.090(3) 0.065(2) 0.088(3) 0.006(2) 0.054(3) 0.026(2) C201 0.056(4) 0.067(4) 0.082(5) 0.000(4) 0.051(4) 0.000(3) C202 0.053(4) 0.065(4) 0.071(4) 0.009(3) 0.040(4) 0.010(3) C102 0.069(5) 0.077(4) 0.071(4) -0.014(3) 0.044(4) -0.010(4) C205 0.082(5) 0.076(4) 0.080(5) 0.001(4) 0.052(4) 0.010(4) C203 0.075(5) 0.086(4) 0.078(5) -0.009(4) 0.050(4) 0.002(4) C204 0.066(4) 0.065(4) 0.081(5) 0.002(3) 0.053(4) 0.006(3) C117 0.076(5) 0.061(4) 0.053(4) 0.007(3) 0.037(3) 0.005(4) C8 0.068(4) 0.074(4) 0.078(5) 0.010(4) 0.045(4) 0.015(3) C118 0.063(4) 0.078(4) 0.055(4) 0.010(3) 0.039(3) 0.005(3) C105 0.102(7) 0.052(5) 0.149(7) -0.011(5) 0.081(6) -0.002(5) C101 0.060(4) 0.067(4) 0.062(4) -0.009(3) 0.037(3) -0.006(3) C111 0.107(7) 0.072(5) 0.169(9) -0.021(6) 0.094(7) -0.008(6) C119 0.085(5) 0.069(4) 0.080(4) 0.011(3) 0.056(4) 0.001(4) C110 0.103(7) 0.092(6) 0.184(9) -0.002(6) 0.039(7) 0.008(6) C209 0.127(7) 0.086(5) 0.110(7) -0.011(5) 0.046(6) -0.010(5) C103 0.076(5) 0.075(4) 0.065(4) -0.016(3) 0.041(4) -0.016(4) C109 0.116(8) 0.102(7) 0.125(7) -0.026(5) 0.069(6) -0.012(5) C104 0.081(5) 0.089(5) 0.098(5) -0.019(4) 0.058(4) -0.013(4) C114 0.128(7) 0.081(5) 0.145(7) -0.006(4) 0.087(6) 0.014(4) C107 0.138(7) 0.060(5) 0.131(7) -0.019(5) 0.083(6) -0.004(5) C208 0.092(5) 0.079(5) 0.075(5) 0.014(5) 0.045(5) 0.016(4) C112 0.146(8) 0.089(5) 0.223(9) -0.007(5) 0.136(8) 0.004(5) C210 0.125(7) 0.097(5) 0.078(5) 0.004(4) 0.056(5) 0.014(5) C401 0.144(7) 0.040(4) 0.227(9) 0.005(4) 0.132(7) -0.014(4) C214 0.174(9) 0.077(5) 0.231(10) 0.006(5) 0.137(8) 0.017(5) C206 0.096(5) 0.070(4) 0.103(5) 0.006(4) 0.063(5) 0.015(4) C207 0.092(5) 0.070(4) 0.095(5) 0.006(4) 0.055(4) 0.014(4) C108 0.116(8) 0.078(6) 0.177(9) -0.012(6) 0.038(7) -0.003(5) C113 0.118(6) 0.092(5) 0.132(6) 0.000(4) 0.077(6) 0.014(4) C106 0.100(6) 0.083(5) 0.135(6) -0.022(5) 0.079(5) -0.014(4) C215 0.207(10) 0.080(5) 0.241(10) 0.022(5) 0.161(9) -0.003(5) C213 0.109(7) 0.081(5) 0.137(7) -0.006(6) 0.080(6) 0.004(5) C211 0.105(7) 0.091(6) 0.125(7) 0.026(5) 0.033(6) 0.021(5) C212 0.141(8) 0.090(6) 0.093(6) -0.010(5) 0.065(6) 0.004(5) C115 0.185(9) 0.116(6) 0.150(7) 0.014(5) 0.127(7) 0.011(5) C216 0.199(10) 0.084(6) 0.247(11) 0.025(6) 0.146(9) -0.008(5) C116 0.278(12) 0.088(5) 0.221(10) 0.020(5) 0.188(10) 0.027(6) C303 0.234(14) 0.107(7) 0.279(15) 0.051(8) 0.099(12) 0.000(7) C302 0.265(14) 0.090(7) 0.160(9) -0.043(6) 0.126(10) -0.039(7) C301 0.147(7) 0.087(5) 0.116(6) -0.024(5) 0.072(6) -0.009(5) C218 0.216(12) 0.148(8) 0.215(11) 0.010(7) 0.084(10) -0.013(8) C217 0.234(12) 0.090(6) 0.277(13) 0.006(7) 0.151(11) 0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C202 1.766(5) . ? S1 C101 1.760(5) . ? S2 C118 1.751(5) . ? S2 C204 1.748(5) . ? O1 C117 1.380(5) . ? O1 C301 1.429(6) . ? O2 C201 1.364(5) . ? O2 C401 1.448(6) . ? C201 C204 1.398(6) . ? C201 C202 1.400(6) . ? C202 C8 1.378(6) . ? C102 C101 1.369(6) . ? C102 C103 1.395(7) . ? C205 C8 1.385(7) . ? C205 C203 1.387(7) . ? C205 C206 1.437(7) . ? C203 C204 1.387(6) . ? C117 C118 1.402(7) . ? C117 C101 1.394(6) 2_656 ? C118 C119 1.375(6) . ? C105 C108 1.338(9) . ? C105 C107 1.363(8) . ? C105 C106 1.415(8) . ? C101 C117 1.394(6) 2_656 ? C111 C109 1.367(9) . ? C111 C110 1.354(9) . ? C111 C112 1.517(8) . ? C119 C103 1.387(7) 2_656 ? C110 C108 1.370(8) . ? C209 C208 1.356(8) . ? C209 C211 1.403(8) . ? C103 C119 1.387(7) 2_656 ? C103 C104 1.462(7) . ? C109 C107 1.355(8) . ? C104 C106 1.192(8) . ? C114 C115 1.463(7) . ? C114 C113 1.537(7) . ? C208 C210 1.365(8) . ? C208 C207 1.414(7) . ? C112 C113 1.493(8) . ? C210 C212 1.378(7) . ? C401 C40A 1.27(2) . ? C401 C402 1.74(3) . ? C214 C215 1.399(8) . ? C214 C213 1.543(8) . ? C206 C207 1.173(7) . ? C215 C216 1.516(8) . ? C213 C211 1.351(9) . ? C213 C212 1.351(9) . ? C115 C116 1.510(7) . ? C216 C217 1.431(11) . ? C303 C302 1.325(12) . ? C302 C301 1.442(9) . ? C218 C217 1.468(9) . ? C402 C40A 0.68(4) . ? C402 C40B 0.73(4) . ? C402 C403 1.41(3) . ? C403 C40A 1.30(2) . ? C403 C40B 1.80(3) . ? C40A C40B 1.39(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 C202 S1 C101 104.1(3) . . ? C118 S2 C204 105.5(2) . . ? C117 O1 C301 116.0(4) . . ? C201 O2 C401 113.8(4) . . ? O2 C201 C204 119.6(5) . . ? O2 C201 C202 120.9(5) . . ? C204 C201 C202 119.5(5) . . ? C8 C202 C201 119.5(5) . . ? C8 C202 S1 117.5(5) . . ? C201 C202 S1 122.8(4) . . ? C101 C102 C103 120.4(5) . . ? C8 C205 C203 117.3(5) . . ? C8 C205 C206 121.4(6) . . ? C203 C205 C206 121.2(6) . . ? C205 C203 C204 122.5(5) . . ? C201 C204 C203 118.9(5) . . ? C201 C204 S2 123.8(4) . . ? C203 C204 S2 117.0(5) . . ? O1 C117 C118 119.7(5) . . ? O1 C117 C101 119.4(5) . 2_656 ? C118 C117 C101 120.8(5) . 2_656 ? C202 C8 C205 122.3(5) . . ? C119 C118 C117 118.4(5) . . ? C119 C118 S2 118.6(5) . . ? C117 C118 S2 122.6(5) . . ? C108 C105 C107 118.4(6) . . ? C108 C105 C106 120.4(8) . . ? C107 C105 C106 121.2(8) . . ? C102 C101 C117 119.6(5) . 2_656 ? C102 C101 S1 116.5(5) . . ? C117 C101 S1 123.8(4) 2_656 . ? C109 C111 C110 116.7(7) . . ? C109 C111 C112 124.3(9) . . ? C110 C111 C112 119.0(10) . . ? C118 C119 C103 121.3(5) . 2_656 ? C111 C110 C108 121.3(8) . . ? C208 C209 C211 121.0(7) . . ? C102 C103 C119 119.5(5) . 2_656 ? C102 C103 C104 121.7(6) . . ? C119 C103 C104 118.8(6) 2_656 . ? C111 C109 C107 122.1(7) . . ? C106 C104 C103 175.2(7) . . ? C115 C114 C113 114.6(6) . . ? C105 C107 C109 120.2(7) . . ? C209 C208 C210 116.6(6) . . ? C209 C208 C207 121.0(7) . . ? C210 C208 C207 122.4(7) . . ? C113 C112 C111 115.4(6) . . ? C208 C210 C212 122.1(7) . . ? C40A C401 O2 115.6(11) . . ? C40A C401 C402 18.9(16) . . ? O2 C401 C402 98.7(10) . . ? C215 C214 C213 116.2(6) . . ? C207 C206 C205 176.8(7) . . ? C206 C207 C208 179.1(9) . . ? C105 C108 C110 121.2(8) . . ? C112 C113 C114 114.0(5) . . ? C104 C106 C105 175.3(8) . . ? C214 C215 C216 112.4(7) . . ? C211 C213 C212 117.5(7) . . ? C211 C213 C214 120.5(9) . . ? C212 C213 C214 122.0(8) . . ? C213 C211 C209 121.5(7) . . ? C213 C212 C210 121.3(7) . . ? C114 C115 C116 112.3(6) . . ? C217 C216 C215 111.3(7) . . ? C303 C302 C301 127.2(9) . . ? C302 C301 O1 112.6(6) . . ? C216 C217 C218 112.8(9) . . ? C40A C402 C40B 162(7) . . ? C40A C402 C403 67(4) . . ? C40B C402 C403 110(4) . . ? C40A C402 C401 37(3) . . ? C40B C402 C401 151(4) . . ? C403 C402 C401 99.1(19) . . ? C40A C403 C402 28.5(16) . . ? C40A C403 C40B 50.3(18) . . ? C402 C403 C40B 22.5(14) . . ? C402 C40A C403 85(4) . . ? C402 C40A C401 124(4) . . ? C403 C40A C401 139(2) . . ? C402 C40A C40B 10(3) . . ? C403 C40A C40B 83.7(17) . . ? C401 C40A C40B 129.6(17) . . ? C402 C40B C40A 9(3) . . ? C402 C40B C403 48(3) . . ? C40A C40B C403 46.0(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.380 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.043 data_ptcal1m _database_code_CSD 193185 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C124 H176 O4 P8 Pt4 S4' _chemical_formula_weight 2887.01 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' '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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 21.6628(17) _cell_length_b 21.6628(17) _cell_length_c 28.045(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13161(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 994(I>2sigma(I)) _cell_measurement_theta_min 1.19 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5792 _exptl_absorpt_coefficient_mu 4.446 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2396 _exptl_absorpt_correction_T_max 0.6648 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19821 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 20.00 _reflns_number_total 3053 _reflns_number_gt 2021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1062P)^2^+86.4948P] 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 3053 _refine_ls_number_parameters 245 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.081 _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 0.24990(3) 0.65545(3) 0.11775(2) 0.0773(4) Uani 1 1 d . . . S1 S 0.1689(3) 0.8152(3) -0.1251(2) 0.116(2) Uani 1 1 d . . . P1 P 0.1991(3) 0.5664(3) 0.1321(2) 0.118(2) Uani 1 1 d D . . P2 P 0.2929(3) 0.7512(2) 0.1089(2) 0.108(2) Uani 1 1 d D . . O1 O 0.0882(7) 0.7117(7) -0.1653(5) 0.124(5) Uani 1 1 d . . . C1 C 0.064(2) 0.722(2) -0.264(2) 0.37(3) Uiso 1 1 d D . . H21A H 0.0552 0.7345 -0.2965 0.559 Uiso 1 1 calc R . . H21B H 0.0533 0.7558 -0.2431 0.559 Uiso 1 1 calc R . . H21C H 0.0392 0.6869 -0.2563 0.559 Uiso 1 1 calc R . . C2 C 0.132(2) 0.707(2) -0.2590(15) 0.31(2) Uiso 1 1 d D . . H20A H 0.1579 0.7415 -0.2672 0.371 Uiso 1 1 calc R . . H20B H 0.1431 0.6712 -0.2780 0.371 Uiso 1 1 calc R . . C3 C 0.1332(19) 0.6925(18) -0.2043(15) 0.239(17) Uiso 1 1 d D . . H17A H 0.1351 0.6478 -0.2023 0.287 Uiso 1 1 calc R . . H17B H 0.1731 0.7072 -0.1936 0.287 Uiso 1 1 calc R . . C4 C 0.1122(9) 0.7006(12) -0.1206(7) 0.093(6) Uani 1 1 d . . . C5 C 0.1004(9) 0.6449(10) -0.0975(8) 0.097(6) Uani 1 1 d . . . C6 C 0.1443(9) 0.7448(11) -0.0979(7) 0.098(7) Uani 1 1 d . . . C7 C 0.1244(8) 0.6355(8) -0.0510(6) 0.080(5) Uani 1 1 d . . . H23A H 0.1167 0.5984 -0.0354 0.096 Uiso 1 1 calc R . . C8 C 0.1678(8) 0.7328(10) -0.0534(7) 0.087(6) Uani 1 1 d . . . H4A H 0.1917 0.7633 -0.0392 0.104 Uiso 1 1 calc R . . C9 C 0.1590(8) 0.6800(9) -0.0286(7) 0.076(5) Uani 1 1 d . . . C10 C 0.1861(8) 0.6682(8) 0.0172(8) 0.081(5) Uani 1 1 d . . . C11 C 0.2081(8) 0.6638(8) 0.0562(7) 0.077(5) Uani 1 1 d . . . C12 C 0.2999(9) 0.6472(8) 0.1802(8) 0.085(6) Uani 1 1 d . . . C13 C 0.3288(10) 0.6440(9) 0.2147(8) 0.086(6) Uani 1 1 d . . . C14 C 0.3648(9) 0.6458(11) 0.2554(7) 0.085(6) Uani 1 1 d . . . C15 C 0.3905(12) 0.6987(15) 0.2725(10) 0.149(10) Uani 1 1 d . . . H15A H 0.3849 0.7342 0.2544 0.179 Uiso 1 1 calc R . . C16 C 0.3755(11) 0.5962(14) 0.2826(9) 0.129(8) Uani 1 1 d . . . H13A H 0.3574 0.5590 0.2736 0.155 Uiso 1 1 calc R . . C17 C 0.4139(14) 0.5966(18) 0.3253(9) 0.173(14) Uani 1 1 d . . . H16A H 0.4237 0.5612 0.3424 0.208 Uiso 1 1 calc R . . C18 C 0.4243(13) 0.7047(18) 0.3145(12) 0.184(14) Uani 1 1 d . . . H18A H 0.4392 0.7422 0.3257 0.220 Uiso 1 1 calc R . . C19 C 0.433(2) 0.651(2) 0.3369(18) 0.22(2) Uiso 1 1 d . . . H14A H 0.4559 0.6528 0.3649 0.266 Uiso 1 1 calc R . . C101 C 0.169(2) 0.557(2) 0.1917(19) 0.33(3) Uiso 1 1 d D . . H29A H 0.1519 0.5157 0.1959 0.401 Uiso 1 1 calc R . . H29B H 0.2011 0.5632 0.2154 0.401 Uiso 1 1 calc R . . C102 C 0.118(2) 0.607(3) 0.1956(17) 0.44(4) Uiso 1 1 d D . . H31A H 0.0996 0.6062 0.2268 0.667 Uiso 1 1 calc R . . H31B H 0.0863 0.5997 0.1721 0.667 Uiso 1 1 calc R . . H31C H 0.1355 0.6473 0.1901 0.667 Uiso 1 1 calc R . . C103 C 0.243(6) 0.495(6) 0.122(2) 0.38(7) Uiso 0.50 1 d PD . . H32A H 0.2185 0.4655 0.1045 0.457 Uiso 0.50 1 calc PR . . H32B H 0.2806 0.5034 0.1051 0.457 Uiso 0.50 1 calc PR . . C104 C 0.257(2) 0.4711(18) 0.173(2) 0.37(3) Uiso 1 1 d D . . H28A H 0.2921 0.4445 0.1718 0.559 Uiso 1 1 calc R . . H28B H 0.2217 0.4484 0.1845 0.559 Uiso 1 1 calc R . . H28C H 0.2648 0.5053 0.1936 0.559 Uiso 1 1 calc R . . C105 C 0.1557(19) 0.533(2) 0.0878(17) 0.29(2) Uiso 1 1 d D . . H27A H 0.1280 0.5024 0.1014 0.354 Uiso 1 1 calc R . . H27B H 0.1311 0.5640 0.0718 0.354 Uiso 1 1 calc R . . C106 C 0.200(2) 0.501(2) 0.0513(13) 0.39(3) Uiso 1 1 d D . . H30A H 0.1765 0.4796 0.0278 0.582 Uiso 1 1 calc R . . H30B H 0.2266 0.4727 0.0678 0.582 Uiso 1 1 calc R . . H30C H 0.2251 0.5322 0.0360 0.582 Uiso 1 1 calc R . . C201 C 0.3162(18) 0.795(2) 0.1517(15) 0.30(2) Uiso 1 1 d D . . H25A H 0.3516 0.7755 0.1666 0.362 Uiso 1 1 calc R . . H25B H 0.3302 0.8337 0.1381 0.362 Uiso 1 1 calc R . . C202 C 0.2693(16) 0.8094(16) 0.1901(9) 0.246(17) Uiso 1 1 d D . . H26A H 0.2883 0.8341 0.2145 0.369 Uiso 1 1 calc R . . H26B H 0.2546 0.7715 0.2038 0.369 Uiso 1 1 calc R . . H26C H 0.2354 0.8316 0.1764 0.369 Uiso 1 1 calc R . . C203 C 0.3777(17) 0.7513(17) 0.1001(13) 0.226(15) Uiso 1 1 d D . . H1A H 0.3936 0.7931 0.1009 0.271 Uiso 1 1 calc R . . H1B H 0.3978 0.7276 0.1250 0.271 Uiso 1 1 calc R . . C204 C 0.3890(16) 0.7226(15) 0.0524(12) 0.217(14) Uiso 1 1 d D . . H22A H 0.4324 0.7228 0.0457 0.325 Uiso 1 1 calc R . . H22B H 0.3676 0.7458 0.0283 0.325 Uiso 1 1 calc R . . H22C H 0.3741 0.6809 0.0525 0.325 Uiso 1 1 calc R . . C205 C 0.2637(10) 0.7991(11) 0.0672(9) 0.136(8) Uiso 1 1 d D . . H12A H 0.2883 0.8365 0.0666 0.163 Uiso 1 1 calc R . . H12B H 0.2678 0.7795 0.0362 0.163 Uiso 1 1 calc R . . C206 C 0.1966(11) 0.8168(13) 0.0744(10) 0.171(11) Uiso 1 1 d D . . H2A H 0.1837 0.8435 0.0490 0.256 Uiso 1 1 calc R . . H2B H 0.1922 0.8378 0.1043 0.256 Uiso 1 1 calc R . . H2C H 0.1716 0.7802 0.0744 0.256 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0949(6) 0.0785(6) 0.0584(6) 0.0065(4) -0.0126(4) -0.0033(4) S1 0.096(4) 0.155(5) 0.098(4) 0.059(4) -0.023(3) -0.016(4) P1 0.145(5) 0.116(5) 0.094(5) 0.017(4) -0.008(4) -0.041(4) P2 0.135(5) 0.077(4) 0.112(5) 0.010(3) -0.043(4) -0.011(3) O1 0.151(13) 0.129(12) 0.093(11) 0.019(9) -0.022(10) -0.004(10) C4 0.090(14) 0.14(2) 0.045(13) 0.024(14) -0.034(11) 0.012(14) C5 0.110(16) 0.105(16) 0.077(16) -0.010(13) -0.010(13) 0.025(13) C6 0.088(14) 0.146(19) 0.061(14) 0.005(13) -0.047(12) 0.017(13) C7 0.098(14) 0.076(13) 0.065(14) 0.005(10) -0.021(11) 0.020(11) C8 0.076(13) 0.105(16) 0.079(15) -0.008(13) -0.012(11) -0.017(11) C9 0.086(13) 0.082(14) 0.061(13) 0.010(12) -0.010(11) -0.015(11) C10 0.074(13) 0.077(13) 0.092(17) 0.013(12) -0.016(12) 0.001(10) C11 0.073(12) 0.084(13) 0.075(14) 0.004(11) -0.007(11) 0.015(10) C12 0.098(16) 0.072(12) 0.087(16) -0.023(11) 0.018(13) 0.007(11) C13 0.103(16) 0.095(15) 0.059(14) 0.017(11) -0.009(13) 0.006(11) C14 0.087(14) 0.113(17) 0.054(14) 0.005(13) -0.019(11) 0.022(13) C15 0.13(2) 0.21(3) 0.11(2) -0.02(2) -0.032(17) -0.03(2) C16 0.13(2) 0.18(3) 0.079(18) -0.012(17) 0.010(15) 0.043(18) C17 0.19(3) 0.25(4) 0.077(19) 0.03(2) -0.013(18) 0.10(3) C18 0.15(2) 0.24(4) 0.17(3) -0.04(3) -0.03(2) -0.08(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 C11 1.96(2) . ? Pt1 C12 2.07(2) . ? Pt1 P1 2.258(6) . ? Pt1 P2 2.287(6) . ? S1 C5 1.75(2) 16_665 ? S1 C6 1.79(2) . ? P1 C105 1.72(5) . ? P1 C103 1.83(12) . ? P1 C101 1.81(5) . ? P2 C205 1.69(2) . ? P2 C201 1.61(4) . ? P2 C203 1.85(4) . ? O1 C4 1.38(2) . ? O1 C3 1.52(4) . ? C1 C2 1.52(2) . ? C2 C3 1.566(19) . ? C4 C6 1.34(3) . ? C4 C5 1.39(3) . ? C5 C7 1.42(2) . ? C5 S1 1.75(2) 11_565 ? C6 C8 1.37(2) . ? C7 C9 1.37(2) . ? C8 C9 1.35(2) . ? C9 C10 1.43(3) . ? C10 C11 1.20(2) . ? C12 C13 1.15(2) . ? C13 C14 1.38(3) . ? C14 C16 1.34(3) . ? C14 C15 1.36(3) . ? C15 C18 1.39(3) . ? C16 C17 1.46(3) . ? C17 C19 1.29(5) . ? C18 C19 1.34(4) . ? C101 C102 1.57(2) . ? C103 C104 1.54(2) . ? C105 C106 1.564(19) . ? C201 C202 1.512(19) . ? C203 C204 1.496(19) . ? C205 C206 1.516(17) . ? 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 C11 Pt1 C12 175.9(7) . . ? C11 Pt1 P1 90.6(5) . . ? C12 Pt1 P1 91.8(5) . . ? C11 Pt1 P2 90.5(5) . . ? C12 Pt1 P2 87.5(5) . . ? P1 Pt1 P2 173.2(3) . . ? C5 S1 C6 108.8(9) 16_665 . ? C105 P1 C103 80(3) . . ? C105 P1 C101 115(2) . . ? C103 P1 C101 103(2) . . ? C105 P1 Pt1 119.9(17) . . ? C103 P1 Pt1 116(4) . . ? C101 P1 Pt1 116.1(16) . . ? C205 P2 C201 106(2) . . ? C205 P2 C203 106.2(14) . . ? C201 P2 C203 77.7(16) . . ? C205 P2 Pt1 118.7(9) . . ? C201 P2 Pt1 125.5(18) . . ? C203 P2 Pt1 114.8(12) . . ? C4 O1 C3 111(2) . . ? C1 C2 C3 99(4) . . ? O1 C3 C2 129(3) . . ? C6 C4 C5 119.5(18) . . ? C6 C4 O1 120(2) . . ? C5 C4 O1 120(2) . . ? C4 C5 C7 119.0(19) . . ? C4 C5 S1 124.0(18) . 11_565 ? C7 C5 S1 116.5(18) . 11_565 ? C4 C6 C8 119(2) . . ? C4 C6 S1 124.0(16) . . ? C8 C6 S1 116.1(18) . . ? C9 C7 C5 121.3(18) . . ? C9 C8 C6 125.1(18) . . ? C8 C9 C7 115.9(17) . . ? C8 C9 C10 123.6(18) . . ? C7 C9 C10 120.5(17) . . ? C11 C10 C9 174(2) . . ? C10 C11 Pt1 175.8(17) . . ? C13 C12 Pt1 178(2) . . ? C12 C13 C14 175(2) . . ? C16 C14 C15 114(2) . . ? C16 C14 C13 123(2) . . ? C15 C14 C13 123(2) . . ? C14 C15 C18 126(3) . . ? C14 C16 C17 124(3) . . ? C19 C17 C16 113(4) . . ? C19 C18 C15 113(4) . . ? C17 C19 C18 129(5) . . ? C102 C101 P1 104(3) . . ? C104 C103 P1 104(6) . . ? C106 C105 P1 109(3) . . ? C202 C201 P2 116(3) . . ? C204 C203 P2 106(3) . . ? C206 C205 P2 115.0(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.182 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.142