# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fad13cs _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H30 F3 N3 O3 Pt S' _chemical_formula_weight 848.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.0939(12) _cell_length_b 19.1285(16) _cell_length_c 26.663(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7188.3(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8823 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.30 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 4.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5106 _exptl_absorpt_correction_T_max 0.7946 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83984 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.71 _reflns_number_total 8947 _reflns_number_gt 7627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There is a poorly-resolved region of residual elelctron density. this could not be adequately modelled and so was "removed" using the program SQUEEZE, which is part of the PLATON system. The void volume per cell was 1031.2\%A^3^, with a void electron count per cell of 363. This additional solvent was NOT taken account of when calculating derived parameters such as the formula weight, because the nature of the solvent was uncertain. The triflate anion is disordered over two positions, ca. 90:10%. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.053 0.081 0.129 128 46 ' ' 2 -0.053 0.581 0.371 128 45 ' ' 3 0.052 0.419 0.629 128 45 ' ' 4 -0.053 0.919 0.871 128 45 ' ' 5 0.447 0.581 0.129 128 46 ' ' 6 0.447 0.919 0.629 128 45 ' ' 7 0.553 0.081 0.371 128 46 ' ' 8 0.553 0.419 0.871 128 45 ' ' _platon_squeeze_details ; ; _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^)+(0.0268P)^2^+7.9702P] 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 'rigid methyls others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8947 _refine_ls_number_parameters 469 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.892148(7) 0.101164(5) 0.646940(3) 0.01820(4) Uani 1 1 d . . . N1 N 0.82777(16) 0.08029(11) 0.71323(9) 0.0229(5) Uani 1 1 d . . . N2 N 0.78102(16) 0.06196(12) 0.60016(9) 0.0245(5) Uani 1 1 d . . . N3 N 0.96854(16) 0.11604(12) 0.58315(8) 0.0224(5) Uani 1 1 d . . . C1 C 0.98881(18) 0.14380(13) 0.69288(9) 0.0193(5) Uani 1 1 d . . . C2 C 1.07019(19) 0.17965(13) 0.67934(10) 0.0218(5) Uani 1 1 d . . . H2 H 1.0842 0.1866 0.6449 0.026 Uiso 1 1 calc R . . C3 C 1.13207(19) 0.20583(14) 0.71590(10) 0.0234(5) Uani 1 1 d . . . C4 C 1.1109(2) 0.19362(15) 0.76644(10) 0.0269(6) Uani 1 1 d . . . H4 H 1.1537 0.2095 0.7915 0.032 Uiso 1 1 calc R . . C5 C 1.0295(2) 0.15923(15) 0.78085(10) 0.0262(6) Uani 1 1 d . . . H5 H 1.0160 0.1523 0.8154 0.031 Uiso 1 1 calc R . . C6 C 0.9666(2) 0.13440(14) 0.74406(10) 0.0217(5) Uani 1 1 d . . . C7 C 0.8775(2) 0.09935(13) 0.75494(10) 0.0231(5) Uani 1 1 d . . . C8 C 0.8406(2) 0.08456(16) 0.80244(11) 0.0316(7) Uani 1 1 d . . . H8 H 0.8750 0.0976 0.8316 0.038 Uiso 1 1 calc R . . C9 C 0.7551(2) 0.05127(17) 0.80702(12) 0.0353(7) Uani 1 1 d . . . H9 H 0.7300 0.0412 0.8393 0.042 Uiso 1 1 calc R . . C10 C 0.7055(2) 0.03251(15) 0.76463(12) 0.0318(7) Uani 1 1 d . . . H10 H 0.6464 0.0089 0.7673 0.038 Uiso 1 1 calc R . . C11 C 0.7429(2) 0.04839(14) 0.71831(11) 0.0264(6) Uani 1 1 d . . . H11 H 0.7079 0.0365 0.6891 0.032 Uiso 1 1 calc R . . C12 C 1.2190(2) 0.24651(17) 0.70163(12) 0.0322(7) Uani 1 1 d . . . H12A H 1.2010 0.2945 0.6930 0.048 Uiso 1 1 calc R . . H12B H 1.2495 0.2243 0.6727 0.048 Uiso 1 1 calc R . . H12C H 1.2634 0.2473 0.7299 0.048 Uiso 1 1 calc R . . C21 C 0.80772(18) 0.18974(14) 0.63920(9) 0.0212(5) Uani 1 1 d . . . C22 C 0.8208(2) 0.25515(14) 0.66099(10) 0.0239(5) Uani 1 1 d . . . H22 H 0.8769 0.2637 0.6798 0.029 Uiso 1 1 calc R . . C23 C 0.7536(2) 0.30874(15) 0.65602(10) 0.0281(6) Uani 1 1 d . . . C24 C 0.6729(2) 0.29560(16) 0.62720(11) 0.0312(6) Uani 1 1 d . . . H24 H 0.6266 0.3313 0.6236 0.037 Uiso 1 1 calc R . . C25 C 0.6589(2) 0.23236(16) 0.60394(10) 0.0284(6) Uani 1 1 d . . . H25 H 0.6041 0.2249 0.5839 0.034 Uiso 1 1 calc R . . C26 C 0.72580(19) 0.17904(15) 0.60991(10) 0.0240(6) Uani 1 1 d . . . C27 C 0.7145(2) 0.10979(15) 0.58693(11) 0.0267(6) Uani 1 1 d . . . C28 C 0.6437(2) 0.09058(18) 0.55311(13) 0.0379(7) Uani 1 1 d . . . H28 H 0.5976 0.1239 0.5430 0.045 Uiso 1 1 calc R . . C29 C 0.6402(2) 0.0239(2) 0.53440(14) 0.0454(9) Uani 1 1 d . . . H29 H 0.5922 0.0113 0.5111 0.054 Uiso 1 1 calc R . . C30 C 0.7068(2) -0.02539(18) 0.54943(13) 0.0393(8) Uani 1 1 d . . . H30 H 0.7041 -0.0723 0.5377 0.047 Uiso 1 1 calc R . . C31 C 0.7769(2) -0.00369(16) 0.58198(11) 0.0292(6) Uani 1 1 d . . . H31 H 0.8241 -0.0363 0.5920 0.035 Uiso 1 1 calc R . . C32 C 0.7660(3) 0.37648(17) 0.68307(14) 0.0409(8) Uani 1 1 d . . . H32A H 0.7157 0.4089 0.6730 0.061 Uiso 1 1 calc R . . H32B H 0.8280 0.3966 0.6746 0.061 Uiso 1 1 calc R . . H32C H 0.7625 0.3684 0.7193 0.061 Uiso 1 1 calc R . . C41 C 0.97304(18) 0.01123(13) 0.64822(10) 0.0218(5) Uani 1 1 d . . . C42 C 0.97515(19) -0.04198(14) 0.68407(12) 0.0275(6) Uani 1 1 d . . . H42 H 0.9364 -0.0381 0.7131 0.033 Uiso 1 1 calc R . . C43 C 1.0331(2) -0.10083(15) 0.67821(14) 0.0353(7) Uani 1 1 d . . . C44 C 1.0891(2) -0.10649(17) 0.63570(15) 0.0399(8) Uani 1 1 d . . . H44 H 1.1277 -0.1467 0.6311 0.048 Uiso 1 1 calc R . . C45 C 1.0896(2) -0.05383(17) 0.59968(13) 0.0358(7) Uani 1 1 d . . . H45 H 1.1294 -0.0577 0.5711 0.043 Uiso 1 1 calc R . . C46 C 1.03142(19) 0.00466(15) 0.60570(11) 0.0265(6) Uani 1 1 d . . . C47 C 1.02803(19) 0.06234(15) 0.57014(10) 0.0253(6) Uani 1 1 d . . . C48 C 1.0784(2) 0.06673(18) 0.52524(12) 0.0344(7) Uani 1 1 d . . . H48 H 1.1192 0.0296 0.5155 0.041 Uiso 1 1 calc R . . C49 C 1.0695(2) 0.1243(2) 0.49523(12) 0.0392(8) Uani 1 1 d . . . H49 H 1.1034 0.1268 0.4645 0.047 Uiso 1 1 calc R . . C50 C 1.0113(2) 0.17888(17) 0.50947(11) 0.0328(7) Uani 1 1 d . . . H50 H 1.0058 0.2195 0.4892 0.039 Uiso 1 1 calc R . . C51 C 0.96120(19) 0.17312(15) 0.55372(10) 0.0272(6) Uani 1 1 d . . . H51 H 0.9206 0.2102 0.5637 0.033 Uiso 1 1 calc R . . C52 C 1.0324(3) -0.15761(17) 0.71734(16) 0.0503(10) Uani 1 1 d . . . H52A H 1.0651 -0.1990 0.7043 0.075 Uiso 1 1 calc R . . H52B H 0.9667 -0.1697 0.7256 0.075 Uiso 1 1 calc R . . H52C H 1.0649 -0.1410 0.7476 0.075 Uiso 1 1 calc R . . C99 C 0.2884(3) 0.2130(3) 0.54262(13) 0.0379(9) Uani 0.898(5) 1 d PD A 1 F1 F 0.32140(19) 0.27810(18) 0.54317(11) 0.0583(8) Uani 0.898(5) 1 d PD A 1 F2 F 0.21746(17) 0.2094(2) 0.57543(9) 0.0570(9) Uani 0.898(5) 1 d PD A 1 F3 F 0.25243(18) 0.2018(2) 0.49699(9) 0.0478(7) Uani 0.898(5) 1 d PD A 1 S1 S 0.38162(7) 0.14983(8) 0.55630(4) 0.0393(4) Uani 0.898(5) 1 d PD A 1 O1 O 0.43748(19) 0.15043(19) 0.51099(12) 0.0474(8) Uani 0.898(5) 1 d PD A 1 O2 O 0.3310(2) 0.08581(18) 0.56485(11) 0.0516(9) Uani 0.898(5) 1 d PD A 1 O3 O 0.4276(2) 0.1787(2) 0.59951(11) 0.0599(11) Uani 0.898(5) 1 d PD A 1 C99' C 0.2798(13) 0.2452(11) 0.5470(7) 0.033(9) Uiso 0.102(5) 1 d PD A 2 F1' F 0.3151(13) 0.3092(10) 0.5443(7) 0.026(5) Uiso 0.102(5) 1 d PD A 2 F2' F 0.2042(14) 0.2505(13) 0.5771(8) 0.050(7) Uiso 0.102(5) 1 d PD A 2 F3' F 0.2460(16) 0.2304(11) 0.5015(7) 0.032(6) Uiso 0.102(5) 1 d PD A 2 S1' S 0.3663(7) 0.1815(7) 0.5697(4) 0.047(3) Uiso 0.102(5) 1 d PD A 2 O1' O 0.4392(12) 0.1788(11) 0.5308(7) 0.027(5) Uiso 0.102(5) 1 d PD A 2 O2' O 0.3089(16) 0.1188(11) 0.5746(10) 0.041(7) Uiso 0.102(5) 1 d PD A 2 O3' O 0.3969(17) 0.2107(14) 0.6161(7) 0.046(7) Uiso 0.102(5) 1 d PD A 2 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 0.01746(5) 0.01840(6) 0.01873(6) -0.00220(4) -0.00003(4) 0.00194(4) N1 0.0257(11) 0.0180(10) 0.0249(11) -0.0004(9) 0.0030(9) 0.0002(9) N2 0.0213(11) 0.0275(13) 0.0248(12) -0.0011(9) 0.0017(9) 0.0018(9) N3 0.0188(11) 0.0270(12) 0.0213(11) -0.0043(9) -0.0028(9) -0.0001(9) C1 0.0210(12) 0.0175(12) 0.0193(12) -0.0025(10) -0.0024(10) 0.0016(10) C2 0.0241(13) 0.0203(13) 0.0211(13) 0.0005(10) -0.0005(10) 0.0023(10) C3 0.0244(13) 0.0214(13) 0.0244(13) -0.0006(11) -0.0011(10) -0.0011(10) C4 0.0315(14) 0.0260(14) 0.0232(13) -0.0055(11) -0.0049(12) 0.0009(12) C5 0.0336(15) 0.0272(14) 0.0179(13) -0.0024(11) 0.0020(11) 0.0013(12) C6 0.0266(13) 0.0196(13) 0.0188(12) 0.0004(10) 0.0019(10) 0.0027(10) C7 0.0276(14) 0.0204(13) 0.0214(13) -0.0001(10) 0.0022(10) 0.0040(10) C8 0.0372(17) 0.0312(16) 0.0264(15) 0.0007(12) 0.0079(13) 0.0007(13) C9 0.0385(17) 0.0350(17) 0.0325(16) 0.0054(13) 0.0151(14) -0.0014(13) C10 0.0291(15) 0.0239(14) 0.0423(18) 0.0033(13) 0.0102(13) -0.0019(12) C11 0.0254(13) 0.0198(13) 0.0339(15) 0.0003(11) 0.0021(12) -0.0005(11) C12 0.0303(15) 0.0332(16) 0.0331(16) -0.0013(13) -0.0049(12) -0.0078(13) C21 0.0195(12) 0.0255(13) 0.0185(12) 0.0030(10) 0.0048(9) 0.0010(10) C22 0.0247(13) 0.0216(13) 0.0253(13) 0.0031(10) 0.0047(11) 0.0014(11) C23 0.0328(15) 0.0249(14) 0.0266(14) 0.0041(11) 0.0093(12) 0.0032(12) C24 0.0322(15) 0.0326(16) 0.0288(14) 0.0122(12) 0.0110(12) 0.0121(13) C25 0.0253(14) 0.0371(16) 0.0229(14) 0.0094(12) 0.0047(11) 0.0060(12) C26 0.0236(13) 0.0280(15) 0.0205(13) 0.0046(11) 0.0027(10) 0.0031(11) C27 0.0229(13) 0.0320(16) 0.0252(14) 0.0021(12) 0.0022(11) 0.0028(11) C28 0.0315(16) 0.046(2) 0.0359(17) -0.0055(15) -0.0102(14) 0.0091(14) C29 0.0328(17) 0.060(2) 0.044(2) -0.0142(17) -0.0139(15) 0.0024(16) C30 0.0354(17) 0.0400(19) 0.0425(19) -0.0146(15) -0.0035(14) -0.0043(14) C31 0.0258(14) 0.0309(15) 0.0308(15) -0.0065(12) 0.0007(12) 0.0000(12) C32 0.047(2) 0.0249(15) 0.051(2) 0.0007(15) 0.0046(16) 0.0067(14) C41 0.0190(12) 0.0178(12) 0.0285(14) -0.0062(10) -0.0063(10) -0.0009(10) C42 0.0220(13) 0.0219(14) 0.0386(16) -0.0017(12) -0.0062(12) -0.0032(11) C43 0.0283(15) 0.0199(14) 0.058(2) -0.0035(14) -0.0128(15) -0.0009(12) C44 0.0289(16) 0.0265(16) 0.064(2) -0.0164(15) -0.0098(15) 0.0109(12) C45 0.0283(16) 0.0355(17) 0.0434(18) -0.0124(14) -0.0025(13) 0.0065(13) C46 0.0228(13) 0.0281(15) 0.0285(14) -0.0088(11) -0.0027(11) 0.0011(11) C47 0.0194(13) 0.0290(15) 0.0274(14) -0.0083(11) -0.0028(10) 0.0012(11) C48 0.0300(15) 0.0427(19) 0.0307(16) -0.0106(14) 0.0036(13) 0.0063(13) C49 0.0333(17) 0.060(2) 0.0240(15) -0.0049(15) 0.0071(13) -0.0001(15) C50 0.0264(15) 0.0446(18) 0.0273(15) 0.0055(13) 0.0001(12) 0.0011(13) C51 0.0217(13) 0.0337(15) 0.0262(14) -0.0002(12) -0.0018(11) 0.0044(11) C52 0.046(2) 0.0237(16) 0.081(3) 0.0105(17) -0.0129(19) 0.0044(15) C99 0.0315(19) 0.052(3) 0.0297(19) -0.0052(17) 0.0059(14) -0.0105(17) F1 0.0546(16) 0.0414(17) 0.079(2) -0.0114(14) 0.0162(13) -0.0058(14) F2 0.0373(13) 0.094(3) 0.0403(13) -0.0134(14) 0.0153(10) -0.0144(14) F3 0.0387(13) 0.074(2) 0.0303(12) 0.0002(13) -0.0080(9) 0.0068(15) S1 0.0362(5) 0.0554(9) 0.0262(5) 0.0078(5) -0.0087(4) -0.0131(5) O1 0.0364(15) 0.066(2) 0.0396(17) 0.0101(16) 0.0010(12) 0.0048(14) O2 0.069(2) 0.0484(19) 0.0378(16) 0.0050(14) -0.0069(15) -0.0165(17) O3 0.060(2) 0.082(3) 0.0385(17) 0.0094(17) -0.0272(15) -0.0285(19) _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 C1 2.005(2) . ? Pt1 N1 2.027(2) . ? Pt1 N3 2.033(2) . ? Pt1 C41 2.064(3) . ? Pt1 C21 2.081(3) . ? Pt1 N2 2.138(2) . ? N1 C11 1.350(3) . ? N1 C7 1.364(4) . ? N2 C31 1.347(4) . ? N2 C27 1.356(4) . ? N3 C51 1.349(4) . ? N3 C47 1.371(3) . ? C1 C2 1.384(4) . ? C1 C6 1.412(4) . ? C2 C3 1.401(4) . ? C3 C4 1.400(4) . ? C3 C12 1.501(4) . ? C4 C5 1.377(4) . ? C5 C6 1.405(4) . ? C6 C7 1.452(4) . ? C7 C8 1.398(4) . ? C8 C9 1.369(4) . ? C9 C10 1.376(5) . ? C10 C11 1.377(4) . ? C21 C22 1.392(4) . ? C21 C26 1.409(4) . ? C22 C23 1.401(4) . ? C23 C24 1.395(4) . ? C23 C32 1.493(4) . ? C24 C25 1.374(4) . ? C25 C26 1.398(4) . ? C26 C27 1.468(4) . ? C27 C28 1.394(4) . ? C28 C29 1.371(5) . ? C29 C30 1.389(5) . ? C30 C31 1.379(4) . ? C41 C42 1.396(4) . ? C41 C46 1.407(4) . ? C42 C43 1.399(4) . ? C43 C44 1.386(5) . ? C43 C52 1.506(5) . ? C44 C45 1.392(5) . ? C45 C46 1.397(4) . ? C46 C47 1.455(4) . ? C47 C48 1.395(4) . ? C48 C49 1.367(5) . ? C49 C50 1.381(5) . ? C50 C51 1.379(4) . ? C99 F1 1.329(5) . ? C99 F2 1.331(4) . ? C99 F3 1.336(4) . ? C99 S1 1.822(5) . ? S1 O3 1.432(3) . ? S1 O2 1.435(3) . ? S1 O1 1.442(3) . ? C99' F1' 1.323(14) . ? C99' F3' 1.332(14) . ? C99' F2' 1.338(14) . ? C99' S1' 1.828(16) . ? S1' O3' 1.424(13) . ? S1' O2' 1.451(13) . ? S1' O1' 1.461(13) . ? 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 Pt1 N1 81.46(10) . . ? C1 Pt1 N3 95.41(10) . . ? N1 Pt1 N3 173.92(9) . . ? C1 Pt1 C41 87.34(10) . . ? N1 Pt1 C41 93.93(10) . . ? N3 Pt1 C41 80.68(10) . . ? C1 Pt1 C21 96.77(10) . . ? N1 Pt1 C21 89.48(9) . . ? N3 Pt1 C21 96.08(9) . . ? C41 Pt1 C21 175.01(10) . . ? C1 Pt1 N2 175.30(9) . . ? N1 Pt1 N2 96.42(9) . . ? N3 Pt1 N2 87.07(9) . . ? C41 Pt1 N2 97.01(9) . . ? C21 Pt1 N2 78.98(10) . . ? C11 N1 C7 119.6(2) . . ? C11 N1 Pt1 124.98(19) . . ? C7 N1 Pt1 115.37(18) . . ? C31 N2 C27 120.3(2) . . ? C31 N2 Pt1 124.66(19) . . ? C27 N2 Pt1 114.92(18) . . ? C51 N3 C47 120.4(2) . . ? C51 N3 Pt1 124.02(18) . . ? C47 N3 Pt1 115.52(18) . . ? C2 C1 C6 119.9(2) . . ? C2 C1 Pt1 127.24(19) . . ? C6 C1 Pt1 112.81(19) . . ? C1 C2 C3 120.8(2) . . ? C4 C3 C2 118.5(3) . . ? C4 C3 C12 120.3(2) . . ? C2 C3 C12 121.2(2) . . ? C5 C4 C3 121.7(3) . . ? C4 C5 C6 119.5(3) . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C7 124.2(2) . . ? C1 C6 C7 116.4(2) . . ? N1 C7 C8 119.6(3) . . ? N1 C7 C6 113.9(2) . . ? C8 C7 C6 126.6(3) . . ? C9 C8 C7 120.2(3) . . ? C8 C9 C10 119.7(3) . . ? C9 C10 C11 119.0(3) . . ? N1 C11 C10 121.9(3) . . ? C22 C21 C26 118.1(2) . . ? C22 C21 Pt1 127.9(2) . . ? C26 C21 Pt1 113.9(2) . . ? C21 C22 C23 121.9(3) . . ? C24 C23 C22 118.1(3) . . ? C24 C23 C32 121.2(3) . . ? C22 C23 C32 120.7(3) . . ? C25 C24 C23 121.6(3) . . ? C24 C25 C26 119.6(3) . . ? C25 C26 C21 120.7(3) . . ? C25 C26 C27 122.5(3) . . ? C21 C26 C27 116.8(2) . . ? N2 C27 C28 119.0(3) . . ? N2 C27 C26 115.2(2) . . ? C28 C27 C26 125.8(3) . . ? C29 C28 C27 120.4(3) . . ? C28 C29 C30 120.2(3) . . ? C31 C30 C29 117.5(3) . . ? N2 C31 C30 122.6(3) . . ? C42 C41 C46 118.3(3) . . ? C42 C41 Pt1 129.1(2) . . ? C46 C41 Pt1 112.6(2) . . ? C41 C42 C43 121.5(3) . . ? C44 C43 C42 119.1(3) . . ? C44 C43 C52 120.9(3) . . ? C42 C43 C52 119.9(3) . . ? C43 C44 C45 120.7(3) . . ? C44 C45 C46 119.9(3) . . ? C45 C46 C41 120.5(3) . . ? C45 C46 C47 123.5(3) . . ? C41 C46 C47 116.0(2) . . ? N3 C47 C48 118.9(3) . . ? N3 C47 C46 115.0(2) . . ? C48 C47 C46 126.0(3) . . ? C49 C48 C47 120.3(3) . . ? C48 C49 C50 120.2(3) . . ? C51 C50 C49 118.6(3) . . ? N3 C51 C50 121.5(3) . . ? F1 C99 F2 107.7(4) . . ? F1 C99 F3 107.0(3) . . ? F2 C99 F3 107.8(3) . . ? F1 C99 S1 111.5(3) . . ? F2 C99 S1 112.1(3) . . ? F3 C99 S1 110.5(3) . . ? O3 S1 O2 115.20(18) . . ? O3 S1 O1 115.08(19) . . ? O2 S1 O1 114.3(2) . . ? O3 S1 C99 103.4(2) . . ? O2 S1 C99 103.85(19) . . ? O1 S1 C99 102.75(16) . . ? F1' C99' F3' 106.4(16) . . ? F1' C99' F2' 105.2(17) . . ? F3' C99' F2' 106.2(17) . . ? F1' C99' S1' 112.5(13) . . ? F3' C99' S1' 113.5(15) . . ? F2' C99' S1' 112.4(15) . . ? O3' S1' O2' 114.6(14) . . ? O3' S1' O1' 114.6(14) . . ? O2' S1' O1' 115.2(14) . . ? O3' S1' C99' 103.2(12) . . ? O2' S1' C99' 102.1(12) . . ? O1' S1' C99' 104.9(11) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.871 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 953979' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fad67bssq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H20 Cl2 F9 N3 O3 Pt S' _chemical_formula_weight 999.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3618(9) _cell_length_b 12.3271(11) _cell_length_c 14.6981(12) _cell_angle_alpha 81.352(2) _cell_angle_beta 88.049(2) _cell_angle_gamma 80.752(2) _cell_volume 1831.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7410 _cell_measurement_theta_min 28.57 _cell_measurement_theta_max 2.35 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 4.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4792 _exptl_absorpt_correction_T_max 0.6165 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.013 0.000 0.000 164 76 ' ' _platon_squeeze_details ; ; _diffrn_ambient_temperature 100(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 APEX CCD' _diffrn_measurement_method 'w-scan and phi scan' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22200 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.58 _reflns_number_total 8532 _reflns_number_gt 8063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of the three coordinated ligands is disordered over two positions, ca 52:48% The triflate is disordered over two position, ca 73:28%. The dichloromethane is disordered over two positions, ca 54:46%. There is a poorly-resolved region of residual elelctron density. this could not be adequately modelled and so was "removed" using the program SQUEEZE, which is part of the PLATON system. The void volume per cell was 164 \%A^3^, with a void electron count per cell of 76. This additional solvent was NOT taken account of when calculating derived parameters such as the formula weight, because the nature of the solvent was uncertain. ; _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^)+(0.0448P)^2^+6.2670P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8532 _refine_ls_number_parameters 465 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.003 _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 0.985119(15) 0.720859(12) 0.730902(10) 0.02228(6) Uani 1 1 d . . . N1 N 1.1020(3) 0.7887(3) 0.6324(2) 0.0267(7) Uani 1 1 d . A . N2 N 1.0425(4) 0.5538(3) 0.7099(2) 0.0260(7) Uani 1 1 d . A . C1 C 1.0864(4) 0.9023(4) 0.6176(3) 0.0288(9) Uani 1 1 d . . . C2 C 1.1702(5) 0.9537(4) 0.5557(4) 0.0374(11) Uani 1 1 d . A . H2 H 1.1609 1.0325 0.5447 0.045 Uiso 1 1 calc R . . C3 C 1.2670(5) 0.8912(5) 0.5097(4) 0.0414(12) Uani 1 1 d . . . H3 H 1.3250 0.9267 0.4683 0.050 Uiso 1 1 calc R A . C4 C 1.2782(5) 0.7777(5) 0.5247(4) 0.0408(11) Uani 1 1 d . A . H4 H 1.3424 0.7336 0.4926 0.049 Uiso 1 1 calc R . . C5 C 1.1955(4) 0.7287(4) 0.5867(3) 0.0326(9) Uani 1 1 d . . . H5 H 1.2045 0.6499 0.5978 0.039 Uiso 1 1 calc R A . C6 C 0.9833(4) 0.9538(4) 0.6737(3) 0.0294(9) Uani 1 1 d . A . C7 C 0.9230(4) 0.8815(4) 0.7389(3) 0.0270(8) Uani 1 1 d . A . C8 C 0.8248(5) 0.9239(4) 0.7978(3) 0.0362(10) Uani 1 1 d . . . H8 H 0.7834 0.8759 0.8419 0.043 Uiso 1 1 calc R A . F1 F 0.6977(4) 1.0788(3) 0.8474(3) 0.0593(9) Uani 1 1 d . . . F2 F 0.9927(3) 1.1396(2) 0.6040(2) 0.0431(7) Uani 1 1 d . . . C9 C 0.7904(5) 1.0375(5) 0.7896(4) 0.0424(12) Uani 1 1 d . A . C10 C 0.8433(5) 1.1125(4) 0.7260(4) 0.0424(12) Uani 1 1 d . . . H10 H 0.8152 1.1904 0.7216 0.051 Uiso 1 1 calc R A . C11 C 0.9394(5) 1.0678(4) 0.6693(4) 0.0343(10) Uani 1 1 d . A . C21 C 0.9663(4) 0.5165(4) 0.6512(3) 0.0274(8) Uani 1 1 d . . . C22 C 0.9840(5) 0.4042(4) 0.6443(4) 0.0363(10) Uani 1 1 d . A . H22 H 0.9294 0.3767 0.6054 0.044 Uiso 1 1 calc R . . C23 C 1.0819(5) 0.3319(4) 0.6944(4) 0.0380(11) Uani 1 1 d . . . H23 H 1.0937 0.2548 0.6902 0.046 Uiso 1 1 calc R A . C24 C 1.1620(5) 0.3715(4) 0.7502(3) 0.0341(10) Uani 1 1 d . A . H24 H 1.2311 0.3232 0.7831 0.041 Uiso 1 1 calc R . . C25 C 1.1390(4) 0.4826(4) 0.7568(3) 0.0291(9) Uani 1 1 d . . . H25 H 1.1927 0.5107 0.7959 0.035 Uiso 1 1 calc R A . C26 C 0.8699(4) 0.6043(4) 0.6013(3) 0.0284(9) Uani 1 1 d . A . C27 C 0.8558(4) 0.7100(4) 0.6285(3) 0.0241(8) Uani 1 1 d . A . C28 C 0.7639(4) 0.7957(4) 0.5869(3) 0.0304(9) Uani 1 1 d . . . H28 H 0.7531 0.8671 0.6058 0.037 Uiso 1 1 calc R A . F3 F 0.5976(3) 0.8596(3) 0.4773(2) 0.0510(8) Uani 1 1 d . . . F4 F 0.8097(3) 0.4924(3) 0.4971(2) 0.0506(8) Uani 1 1 d . . . C29 C 0.6877(4) 0.7754(5) 0.5168(3) 0.0364(11) Uani 1 1 d . A . C30 C 0.7014(5) 0.6765(5) 0.4858(3) 0.0413(12) Uani 1 1 d . . . H30 H 0.6507 0.6657 0.4362 0.050 Uiso 1 1 calc R A . C31 C 0.7925(5) 0.5914(5) 0.5291(3) 0.0354(10) Uani 1 1 d . A . N3 N 0.8637(12) 0.6691(10) 0.8381(8) 0.026(3) Uiso 0.518(13) 1 d P A 1 C41 C 0.9088(13) 0.6648(10) 0.9254(8) 0.031(3) Uiso 0.518(13) 1 d P A 1 C42 C 0.8337(12) 0.6373(10) 1.0005(7) 0.036(2) Uiso 0.518(13) 1 d P A 1 H42 H 0.8645 0.6365 1.0607 0.043 Uiso 0.518(13) 1 calc PR A 1 C43 C 0.7142(12) 0.6113(11) 0.9877(8) 0.040(3) Uiso 0.518(13) 1 d P A 1 H43 H 0.6601 0.5932 1.0395 0.048 Uiso 0.518(13) 1 calc PR A 1 C44 C 0.6708(12) 0.6108(11) 0.9009(8) 0.033(3) Uiso 0.518(13) 1 d P A 1 H44 H 0.5891 0.5885 0.8918 0.040 Uiso 0.518(13) 1 calc PR A 1 C45 C 0.7477(13) 0.6432(11) 0.8272(9) 0.029(3) Uiso 0.518(13) 1 d P A 1 H45 H 0.7163 0.6470 0.7667 0.035 Uiso 0.518(13) 1 calc PR A 1 C46 C 1.0408(13) 0.6919(10) 0.9276(8) 0.032(3) Uiso 0.518(13) 1 d P A 1 C47 C 1.0976(12) 0.7205(9) 0.8437(8) 0.026(3) Uiso 0.518(13) 1 d P A 1 C48 C 1.2244(12) 0.7522(10) 0.8392(9) 0.031(3) Uiso 0.518(13) 1 d P A 1 H48 H 1.2624 0.7767 0.7815 0.037 Uiso 0.518(13) 1 calc PR A 1 F5 F 1.4127(7) 0.7791(7) 0.9153(5) 0.0442(18) Uiso 0.518(13) 1 d P A 1 F6 F 1.0642(8) 0.6608(7) 1.0895(5) 0.049(2) Uiso 0.518(13) 1 d P A 1 C49 C 1.2913(12) 0.7468(10) 0.9202(8) 0.035(3) Uiso 0.518(13) 1 d P A 1 C50 C 1.2383(12) 0.7174(10) 1.0045(8) 0.038(2) Uiso 0.518(13) 1 d P A 1 H50 H 1.2845 0.7159 1.0596 0.045 Uiso 0.518(13) 1 calc PR A 1 C51 C 1.1143(12) 0.6900(10) 1.0060(8) 0.038(2) Uiso 0.518(13) 1 d P A 1 N3' N 0.8856(12) 0.6563(10) 0.8378(8) 0.024(3) Uiso 0.482(13) 1 d P A 2 C41' C 0.9403(13) 0.6447(10) 0.9229(8) 0.027(3) Uiso 0.482(13) 1 d P A 2 C42' C 0.8709(13) 0.6016(11) 1.0006(8) 0.037(3) Uiso 0.482(13) 1 d P A 2 H42' H 0.9090 0.5915 1.0598 0.045 Uiso 0.482(13) 1 calc PR A 2 C43' C 0.7442(13) 0.5730(12) 0.9917(9) 0.041(3) Uiso 0.482(13) 1 d P A 2 H43' H 0.6946 0.5497 1.0445 0.050 Uiso 0.482(13) 1 calc PR A 2 C44' C 0.6949(14) 0.5802(13) 0.9028(9) 0.041(3) Uiso 0.482(13) 1 d P A 2 H44' H 0.6143 0.5558 0.8941 0.049 Uiso 0.482(13) 1 calc PR A 2 C45' C 0.7649(14) 0.6231(12) 0.8285(10) 0.029(4) Uiso 0.482(13) 1 d P A 2 H45' H 0.7297 0.6303 0.7686 0.035 Uiso 0.482(13) 1 calc PR A 2 C46' C 1.0730(12) 0.6747(10) 0.9203(7) 0.026(3) Uiso 0.482(13) 1 d P A 2 C47' C 1.1241(12) 0.7153(9) 0.8314(8) 0.020(3) Uiso 0.482(13) 1 d P A 2 C48' C 1.2469(12) 0.7395(9) 0.8229(8) 0.026(3) Uiso 0.482(13) 1 d P A 2 H48' H 1.2820 0.7648 0.7644 0.031 Uiso 0.482(13) 1 calc PR A 2 F5' F 1.4426(8) 0.7487(7) 0.8947(6) 0.047(2) Uiso 0.482(13) 1 d P A 2 F6' F 1.1085(7) 0.6197(7) 1.0820(4) 0.0382(19) Uiso 0.482(13) 1 d P A 2 C49' C 1.3200(13) 0.7263(11) 0.9017(9) 0.036(3) Uiso 0.482(13) 1 d P A 2 C50' C 1.2774(13) 0.6878(10) 0.9900(8) 0.038(3) Uiso 0.482(13) 1 d P A 2 H50' H 1.3310 0.6803 1.0425 0.045 Uiso 0.482(13) 1 calc PR A 2 C51' C 1.1533(12) 0.6615(10) 0.9962(7) 0.032(2) Uiso 0.482(13) 1 d P A 2 C91 C 0.4396(13) 0.0217(13) 0.7563(9) 0.041(3) Uiso 0.46(2) 1 d P B 1 H91A H 0.4764 0.0892 0.7303 0.049 Uiso 0.46(2) 1 calc PR B 1 H91B H 0.4679 0.0001 0.8210 0.049 Uiso 0.46(2) 1 calc PR B 1 Cl1 Cl 0.2653(4) 0.0497(4) 0.7515(6) 0.0514(13) Uiso 0.46(2) 1 d P B 1 Cl2 Cl 0.4961(4) -0.0866(7) 0.6928(3) 0.0597(16) Uiso 0.46(2) 1 d P B 1 C91' C 0.4133(17) 0.0637(17) 0.7366(13) 0.070(4) Uiso 0.54(2) 1 d P B 2 H91C H 0.4046 0.1258 0.6848 0.084 Uiso 0.54(2) 1 calc PR B 2 H91D H 0.4618 0.0853 0.7861 0.084 Uiso 0.54(2) 1 calc PR B 2 Cl1' Cl 0.2566(4) 0.0436(3) 0.7778(5) 0.0544(12) Uiso 0.54(2) 1 d P B 2 Cl2' Cl 0.5023(5) -0.0521(8) 0.6997(3) 0.0715(15) Uiso 0.54(2) 1 d P B 2 C99 C 0.5146(6) 0.4889(5) 0.6597(4) 0.0298(13) Uiso 0.718(4) 1 d PD C 1 F91 F 0.3913(5) 0.5113(4) 0.6351(4) 0.0419(12) Uiso 0.718(4) 1 d PD C 1 F92 F 0.5538(6) 0.5799(5) 0.6820(4) 0.0466(16) Uiso 0.718(4) 1 d PD C 1 F93 F 0.5840(5) 0.4659(4) 0.5846(3) 0.0544(12) Uiso 0.718(4) 1 d PD C 1 S1 S 0.54295(18) 0.37130(14) 0.75174(13) 0.0324(4) Uiso 0.718(4) 1 d PD C 1 O1 O 0.4622(6) 0.4116(5) 0.8250(4) 0.0556(15) Uiso 0.718(4) 1 d PD C 1 O2 O 0.5013(6) 0.2863(5) 0.7079(5) 0.0517(15) Uiso 0.718(4) 1 d PD C 1 O3 O 0.6854(7) 0.3668(6) 0.7616(5) 0.055(2) Uiso 0.718(4) 1 d PD C 1 C99' C 0.5788(12) 0.3714(10) 0.7266(8) 0.011(2) Uiso 0.282(4) 1 d PD C 2 F91' F 0.6345(15) 0.3686(14) 0.6430(10) 0.082(5) Uiso 0.282(4) 1 d PD C 2 F92' F 0.5079(16) 0.2922(15) 0.7438(12) 0.082(6) Uiso 0.282(4) 1 d PD C 2 F93' F 0.6732(11) 0.3501(10) 0.7855(8) 0.033(3) Uiso 0.282(4) 1 d PD C 2 S1' S 0.4739(4) 0.5089(4) 0.7246(3) 0.0375(12) Uiso 0.282(4) 1 d PD C 2 O1' O 0.5441(17) 0.5919(15) 0.7019(11) 0.048(5) Uiso 0.282(4) 1 d PD C 2 O2' O 0.4301(13) 0.4990(12) 0.8155(8) 0.045(3) Uiso 0.282(4) 1 d PD C 2 O3' O 0.3743(11) 0.5102(10) 0.6648(9) 0.028(3) Uiso 0.282(4) 1 d PD C 2 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 0.02533(9) 0.02260(9) 0.01985(8) -0.00017(5) -0.00514(5) -0.00839(6) N1 0.0243(17) 0.0294(18) 0.0259(17) 0.0031(14) -0.0078(13) -0.0082(14) N2 0.0285(17) 0.0283(18) 0.0228(17) -0.0025(14) -0.0008(13) -0.0106(14) C1 0.028(2) 0.029(2) 0.030(2) 0.0037(17) -0.0123(17) -0.0102(17) C2 0.035(2) 0.036(2) 0.040(3) 0.010(2) -0.008(2) -0.013(2) C3 0.032(2) 0.050(3) 0.040(3) 0.010(2) -0.001(2) -0.016(2) C4 0.028(2) 0.049(3) 0.043(3) 0.003(2) 0.002(2) -0.009(2) C5 0.026(2) 0.033(2) 0.038(2) -0.0014(19) -0.0030(18) -0.0070(18) C6 0.028(2) 0.028(2) 0.033(2) 0.0007(17) -0.0125(17) -0.0078(17) C7 0.027(2) 0.026(2) 0.030(2) -0.0043(16) -0.0088(16) -0.0068(16) C8 0.036(2) 0.039(3) 0.035(2) -0.007(2) -0.0023(19) -0.011(2) F1 0.055(2) 0.056(2) 0.069(2) -0.0250(18) 0.0115(17) -0.0024(17) F2 0.0459(17) 0.0297(14) 0.0535(18) 0.0047(13) -0.0091(14) -0.0136(12) C9 0.035(3) 0.045(3) 0.048(3) -0.020(2) -0.002(2) 0.000(2) C10 0.043(3) 0.031(2) 0.055(3) -0.009(2) -0.016(2) -0.006(2) C11 0.034(2) 0.028(2) 0.042(3) -0.0006(19) -0.0113(19) -0.0104(18) C21 0.026(2) 0.032(2) 0.027(2) -0.0068(17) 0.0028(16) -0.0118(17) C22 0.029(2) 0.041(3) 0.044(3) -0.019(2) 0.0002(19) -0.0095(19) C23 0.034(2) 0.033(2) 0.050(3) -0.014(2) 0.004(2) -0.0075(19) C24 0.032(2) 0.033(2) 0.036(2) -0.0029(19) 0.0027(18) -0.0054(18) C25 0.028(2) 0.031(2) 0.029(2) -0.0006(17) -0.0044(16) -0.0100(17) C26 0.0246(19) 0.040(2) 0.023(2) -0.0051(17) 0.0004(15) -0.0139(18) C27 0.0223(18) 0.033(2) 0.0185(18) -0.0007(15) -0.0009(14) -0.0111(16) C28 0.025(2) 0.037(2) 0.029(2) 0.0019(18) -0.0038(16) -0.0104(18) F3 0.0392(16) 0.062(2) 0.0477(18) 0.0088(15) -0.0181(14) -0.0083(15) F4 0.0430(17) 0.065(2) 0.0521(19) -0.0307(16) -0.0098(14) -0.0106(15) C29 0.026(2) 0.052(3) 0.029(2) 0.008(2) -0.0071(17) -0.011(2) C30 0.028(2) 0.069(4) 0.031(2) -0.009(2) -0.0069(18) -0.014(2) C31 0.028(2) 0.052(3) 0.033(2) -0.017(2) 0.0002(18) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N3' 1.986(12) . ? Pt1 C7 2.002(4) . ? Pt1 N1 2.026(4) . ? Pt1 C47 2.058(11) . ? Pt1 N3 2.072(11) . ? Pt1 C27 2.082(4) . ? Pt1 C47' 2.084(11) . ? Pt1 N2 2.116(4) . ? N1 C5 1.347(6) . ? N1 C1 1.368(6) . ? N2 C25 1.352(6) . ? N2 C21 1.365(5) . ? C1 C2 1.390(6) . ? C1 C6 1.451(7) . ? C2 C3 1.385(8) . ? C3 C4 1.370(8) . ? C4 C5 1.370(7) . ? C6 C11 1.398(6) . ? C6 C7 1.408(6) . ? C7 C8 1.401(7) . ? C8 C9 1.376(7) . ? F1 C9 1.349(6) . ? F2 C11 1.369(6) . ? C9 C10 1.378(8) . ? C10 C11 1.377(8) . ? C21 C22 1.386(7) . ? C21 C26 1.473(6) . ? C22 C23 1.389(7) . ? C23 C24 1.377(7) . ? C24 C25 1.370(7) . ? C26 C31 1.395(6) . ? C26 C27 1.404(6) . ? C27 C28 1.385(6) . ? C28 C29 1.394(6) . ? F3 C29 1.353(6) . ? F4 C31 1.356(6) . ? C29 C30 1.350(8) . ? C30 C31 1.385(8) . ? N3 C45 1.313(17) . ? N3 C41 1.371(16) . ? C41 C42 1.361(15) . ? C41 C46 1.462(16) . ? C42 C43 1.354(15) . ? C43 C44 1.370(16) . ? C44 C45 1.371(17) . ? C46 C47 1.370(16) . ? C46 C51 1.399(16) . ? C47 C48 1.427(16) . ? C48 C49 1.385(16) . ? F5 C49 1.376(13) . ? F6 C51 1.337(13) . ? C49 C50 1.361(16) . ? C50 C51 1.378(15) . ? N3' C41' 1.370(16) . ? N3' C45' 1.394(18) . ? C41' C42' 1.410(16) . ? C41' C46' 1.478(16) . ? C42' C43' 1.428(17) . ? C43' C44' 1.404(18) . ? C44' C45' 1.38(2) . ? C46' C51' 1.389(15) . ? C46' C47' 1.442(15) . ? C47' C48' 1.351(16) . ? C48' C49' 1.380(16) . ? F5' C49' 1.340(14) . ? F6' C51' 1.382(12) . ? C49' C50' 1.396(17) . ? C50' C51' 1.373(16) . ? C91 Cl2 1.756(14) . ? C91 Cl1 1.784(14) . ? C91' Cl2' 1.720(17) . ? C91' Cl1' 1.755(16) . ? C99 F91 1.314(7) . ? C99 F93 1.339(7) . ? C99 F92 1.339(7) . ? C99 S1 1.822(7) . ? S1 O2 1.438(7) . ? S1 O1 1.440(6) . ? S1 O3 1.479(7) . ? C99' F93' 1.297(13) . ? C99' F92' 1.304(15) . ? C99' F91' 1.343(15) . ? C99' S1' 1.858(13) . ? S1' O1' 1.344(14) . ? S1' O3' 1.375(11) . ? S1' O2' 1.391(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3' Pt1 C7 98.1(4) . . ? N3' Pt1 N1 173.4(4) . . ? C7 Pt1 N1 81.09(17) . . ? N3' Pt1 C47 74.9(5) . . ? C7 Pt1 C47 86.3(3) . . ? N1 Pt1 C47 98.5(4) . . ? N3' Pt1 N3 6.8(5) . . ? C7 Pt1 N3 92.6(4) . . ? N1 Pt1 N3 173.1(3) . . ? C47 Pt1 N3 78.4(5) . . ? N3' Pt1 C27 97.7(4) . . ? C7 Pt1 C27 95.71(17) . . ? N1 Pt1 C27 88.89(14) . . ? C47 Pt1 C27 172.6(3) . . ? N3 Pt1 C27 94.4(3) . . ? N3' Pt1 C47' 82.4(5) . . ? C7 Pt1 C47' 90.1(3) . . ? N1 Pt1 C47' 91.1(4) . . ? C47 Pt1 C47' 9.0(4) . . ? N3 Pt1 C47' 86.3(5) . . ? C27 Pt1 C47' 174.1(3) . . ? N3' Pt1 N2 84.6(4) . . ? C7 Pt1 N2 174.51(15) . . ? N1 Pt1 N2 96.82(14) . . ? C47 Pt1 N2 99.1(3) . . ? N3 Pt1 N2 89.7(3) . . ? C27 Pt1 N2 79.14(16) . . ? C47' Pt1 N2 95.0(3) . . ? C5 N1 C1 120.3(4) . . ? C5 N1 Pt1 123.7(3) . . ? C1 N1 Pt1 115.9(3) . . ? C25 N2 C21 120.1(4) . . ? C25 N2 Pt1 124.1(3) . . ? C21 N2 Pt1 115.4(3) . . ? N1 C1 C2 118.6(4) . . ? N1 C1 C6 113.2(4) . . ? C2 C1 C6 128.2(4) . . ? C3 C2 C1 120.7(5) . . ? C4 C3 C2 119.2(5) . . ? C5 C4 C3 119.2(5) . . ? N1 C5 C4 122.0(5) . . ? C11 C6 C7 117.5(4) . . ? C11 C6 C1 126.1(4) . . ? C7 C6 C1 116.4(4) . . ? C8 C7 C6 120.5(4) . . ? C8 C7 Pt1 126.2(3) . . ? C6 C7 Pt1 113.2(3) . . ? C9 C8 C7 117.8(5) . . ? F1 C9 C8 118.0(5) . . ? F1 C9 C10 117.3(5) . . ? C8 C9 C10 124.6(5) . . ? C11 C10 C9 115.9(5) . . ? F2 C11 C10 117.6(4) . . ? F2 C11 C6 118.7(4) . . ? C10 C11 C6 123.7(5) . . ? N2 C21 C22 119.3(4) . . ? N2 C21 C26 114.0(4) . . ? C22 C21 C26 126.7(4) . . ? C21 C22 C23 119.7(4) . . ? C24 C23 C22 120.3(5) . . ? C25 C24 C23 118.1(5) . . ? N2 C25 C24 122.4(4) . . ? C31 C26 C27 117.5(4) . . ? C31 C26 C21 125.5(4) . . ? C27 C26 C21 117.1(4) . . ? C28 C27 C26 120.3(4) . . ? C28 C27 Pt1 126.1(3) . . ? C26 C27 Pt1 113.6(3) . . ? C27 C28 C29 118.8(5) . . ? C30 C29 F3 118.8(4) . . ? C30 C29 C28 123.0(5) . . ? F3 C29 C28 118.2(5) . . ? C29 C30 C31 117.3(4) . . ? F4 C31 C30 118.0(4) . . ? F4 C31 C26 119.0(5) . . ? C30 C31 C26 123.0(5) . . ? C45 N3 C41 119.2(11) . . ? C45 N3 Pt1 124.3(9) . . ? C41 N3 Pt1 116.4(8) . . ? C42 C41 N3 121.0(11) . . ? C42 C41 C46 125.4(10) . . ? N3 C41 C46 113.6(10) . . ? C43 C42 C41 118.8(10) . . ? C42 C43 C44 120.5(11) . . ? C43 C44 C45 118.5(11) . . ? N3 C45 C44 121.8(12) . . ? C47 C46 C51 117.5(11) . . ? C47 C46 C41 115.9(10) . . ? C51 C46 C41 126.6(10) . . ? C46 C47 C48 119.8(10) . . ? C46 C47 Pt1 115.6(8) . . ? C48 C47 Pt1 124.4(9) . . ? C49 C48 C47 118.9(11) . . ? C50 C49 F5 118.7(10) . . ? C50 C49 C48 122.6(11) . . ? F5 C49 C48 118.5(10) . . ? C49 C50 C51 116.6(10) . . ? F6 C51 C50 115.8(10) . . ? F6 C51 C46 119.8(10) . . ? C50 C51 C46 124.5(11) . . ? C41' N3' C45' 120.2(11) . . ? C41' N3' Pt1 117.3(9) . . ? C45' N3' Pt1 122.5(9) . . ? N3' C41' C42' 118.9(11) . . ? N3' C41' C46' 113.6(10) . . ? C42' C41' C46' 127.5(10) . . ? C41' C42' C43' 121.0(11) . . ? C44' C43' C42' 118.3(12) . . ? C45' C44' C43' 119.0(13) . . ? C44' C45' N3' 122.4(13) . . ? C51' C46' C47' 118.3(10) . . ? C51' C46' C41' 124.7(10) . . ? C47' C46' C41' 117.0(9) . . ? C48' C47' C46' 120.4(10) . . ? C48' C47' Pt1 130.0(9) . . ? C46' C47' Pt1 109.5(8) . . ? C47' C48' C49' 118.0(11) . . ? F5' C49' C48' 119.0(11) . . ? F5' C49' C50' 116.0(10) . . ? C48' C49' C50' 124.9(11) . . ? C51' C50' C49' 115.7(11) . . ? C50' C51' F6' 117.8(10) . . ? C50' C51' C46' 122.6(10) . . ? F6' C51' C46' 119.6(10) . . ? Cl2 C91 Cl1 108.8(7) . . ? Cl2' C91' Cl1' 113.4(9) . . ? F91 C99 F93 106.5(5) . . ? F91 C99 F92 110.2(5) . . ? F93 C99 F92 105.7(5) . . ? F91 C99 S1 111.6(4) . . ? F93 C99 S1 110.3(4) . . ? F92 C99 S1 112.3(5) . . ? O2 S1 O1 117.7(4) . . ? O2 S1 O3 117.1(4) . . ? O1 S1 O3 115.8(4) . . ? O2 S1 C99 100.4(4) . . ? O1 S1 C99 102.1(3) . . ? O3 S1 C99 98.3(4) . . ? F93' C99' F92' 107.8(11) . . ? F93' C99' F91' 106.7(11) . . ? F92' C99' F91' 109.1(11) . . ? F93' C99' S1' 115.4(9) . . ? F92' C99' S1' 110.1(12) . . ? F91' C99' S1' 107.5(10) . . ? O1' S1' O3' 114.1(8) . . ? O1' S1' O2' 113.3(9) . . ? O3' S1' O2' 111.6(7) . . ? O1' S1' C99' 111.0(10) . . ? O3' S1' C99' 105.9(7) . . ? O2' S1' C99' 99.7(7) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.783 _refine_diff_density_min -1.398 _refine_diff_density_rms 0.136 # start Validation Reply Form _vrf_PLAT201_fad67bssq ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 14 RESPONSE: One of the three coordinated ligands (which contains 14 non-H atoms) is disordered over two positions, ca 52:48% ; # end Validation Reply Form #===END _database_code_depnum_ccdc_archive 'CCDC 953980'