# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_complex1 _database_code_depnum_ccdc_archive 'CCDC 816625' #TrackingRef 'CIFFileDLorcy.cif' _audit_creation_date 2011-07-08T08:13:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H26 N2 Pt S8' _chemical_formula_sum 'C32 H26 N2 Pt S8' _chemical_formula_weight 890.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.2927(4) _cell_length_b 20.7303(7) _cell_length_c 13.1062(4) _cell_angle_alpha 90 _cell_angle_beta 106.7260(10) _cell_angle_gamma 90 _cell_volume 3198.57(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5389 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.34 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.937 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.906 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.0648 _diffrn_reflns_number 21234 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 7265 _reflns_number_gt 5233 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # 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^)+(0.0299P)^2^+1.7070P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7265 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.526 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.157 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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' 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 0.615681(15) 0.045440(9) 0.371399(16) 0.01826(6) Uani 1 1 d . . . N1 N 0.7092(3) 0.0167(2) 0.5222(3) 0.0227(10) Uani 1 1 d . . . N11 N 0.5239(3) 0.08727(19) 0.4631(3) 0.0195(9) Uani 1 1 d . . . C12 C 0.8023(4) -0.0200(3) 0.5449(5) 0.0294(13) Uani 1 1 d . . . H12 H 0.8326 -0.0321 0.4887 0.035 Uiso 1 1 calc R . . C13 C 0.8558(5) -0.0410(3) 0.6465(5) 0.0360(15) Uani 1 1 d . . . H13 H 0.9223 -0.0669 0.6603 0.043 Uiso 1 1 calc R . . C14 C 0.8114(5) -0.0237(3) 0.7276(5) 0.0363(15) Uani 1 1 d . . . H14 H 0.8465 -0.0379 0.7983 0.044 Uiso 1 1 calc R . . C15 C 0.7155(5) 0.0143(3) 0.7056(4) 0.0305(13) Uani 1 1 d . . . H15 H 0.6835 0.0263 0.7608 0.037 Uiso 1 1 calc R . . C16 C 0.6665(4) 0.0349(2) 0.6022(4) 0.0221(12) Uani 1 1 d . . . C17 C 0.5661(4) 0.0766(3) 0.5699(4) 0.0222(11) Uani 1 1 d . . . C18 C 0.5130(5) 0.1031(3) 0.6408(4) 0.0309(13) Uani 1 1 d . . . H18 H 0.5422 0.0952 0.7151 0.037 Uiso 1 1 calc R . . C19 C 0.4171(5) 0.1409(3) 0.6018(5) 0.0369(15) Uani 1 1 d . . . H19 H 0.3804 0.1599 0.6491 0.044 Uiso 1 1 calc R . . C20 C 0.3761(4) 0.1507(3) 0.4949(5) 0.0316(14) Uani 1 1 d . . . H20 H 0.3096 0.1759 0.4672 0.038 Uiso 1 1 calc R . . C21 C 0.4307(4) 0.1241(2) 0.4267(5) 0.0261(13) Uani 1 1 d . . . H21 H 0.4019 0.132 0.3524 0.031 Uiso 1 1 calc R . . S1A S 1.21065(11) -0.17109(7) 0.13773(12) 0.0299(3) Uani 1 1 d . . . S2A S 1.18898(11) -0.18752(7) 0.35392(12) 0.0308(3) Uani 1 1 d . . . S3A S 0.98136(11) -0.07858(7) 0.07898(12) 0.0291(3) Uani 1 1 d . . . S4A S 0.96449(11) -0.09793(7) 0.29663(12) 0.0290(3) Uani 1 1 d . . . S1B S 0.11261(11) 0.26985(7) -0.23854(11) 0.0279(3) Uani 1 1 d . . . S2B S 0.06659(11) 0.27267(7) -0.02974(11) 0.0268(3) Uani 1 1 d . . . S3B S 0.32533(10) 0.17214(7) -0.14131(11) 0.0239(3) Uani 1 1 d . . . S4B S 0.28078(10) 0.17762(7) 0.06847(11) 0.0249(3) Uani 1 1 d . . . C1A C 1.3892(5) -0.2588(3) 0.1780(5) 0.0382(15) Uani 1 1 d . . . H1A1 H 1.4361 -0.2881 0.2314 0.057 Uiso 1 1 calc R . . H1A2 H 1.4377 -0.226 0.1594 0.057 Uiso 1 1 calc R . . H1A3 H 1.3497 -0.2832 0.1141 0.057 Uiso 1 1 calc R . . C2A C 1.3038(4) -0.2266(3) 0.2225(5) 0.0279(13) Uani 1 1 d . . . C3A C 1.2921(4) -0.2339(3) 0.3173(5) 0.0340(14) Uani 1 1 d . . . C4A C 1.3608(5) -0.2781(3) 0.4037(5) 0.0438(17) Uani 1 1 d . . . H4A1 H 1.3888 -0.3147 0.3711 0.066 Uiso 1 1 calc R . . H4A2 H 1.3129 -0.2939 0.4465 0.066 Uiso 1 1 calc R . . H4A3 H 1.4255 -0.2543 0.4494 0.066 Uiso 1 1 calc R . . C5A C 1.1314(4) -0.1535(3) 0.2278(4) 0.0256(13) Uani 1 1 d . . . C6A C 1.0376(4) -0.1158(3) 0.2024(4) 0.0238(12) Uani 1 1 d . . . C7A C 0.7943(4) 0.0033(3) 0.0288(4) 0.0279(13) Uani 1 1 d . . . H7A1 H 0.7412 0.0263 0.0592 0.042 Uiso 1 1 calc R . . H7A2 H 0.7516 -0.0241 -0.03 0.042 Uiso 1 1 calc R . . H7A3 H 0.8393 0.0346 0.0022 0.042 Uiso 1 1 calc R . . C8A C 0.8710(4) -0.0373(2) 0.1122(5) 0.0244(13) Uani 1 1 d . . . C9A C 0.8643(4) -0.0453(3) 0.2120(4) 0.0243(12) Uani 1 1 d . . . C10A C 0.7822(4) -0.0170(3) 0.2558(4) 0.0223(11) Uani 1 1 d . . . C11A C 0.7148(4) 0.0059(2) 0.2968(4) 0.0211(11) Uani 1 1 d . . . C1B C -0.0667(5) 0.3512(3) -0.3280(4) 0.0346(14) Uani 1 1 d . . . H1B1 H -0.1317 0.3742 -0.3164 0.052 Uiso 1 1 calc R . . H1B2 H -0.0937 0.3201 -0.3862 0.052 Uiso 1 1 calc R . . H1B3 H -0.0152 0.3821 -0.3467 0.052 Uiso 1 1 calc R . . C2B C -0.0048(4) 0.3161(2) -0.2282(4) 0.0240(12) Uani 1 1 d . . . C3B C -0.0263(4) 0.3175(2) -0.1340(4) 0.0227(12) Uani 1 1 d . . . C4B C -0.1160(4) 0.3541(3) -0.1050(5) 0.0381(15) Uani 1 1 d . . . H4B1 H -0.1648 0.3754 -0.1684 0.057 Uiso 1 1 calc R . . H4B2 H -0.0811 0.3866 -0.0513 0.057 Uiso 1 1 calc R . . H4B3 H -0.1617 0.3245 -0.0759 0.057 Uiso 1 1 calc R . . C5B C 0.1489(4) 0.2410(2) -0.1072(4) 0.0229(12) Uani 1 1 d . . . C6B C 0.2375(4) 0.2012(2) -0.0673(4) 0.0203(11) Uani 1 1 d . . . C7B C 0.5012(4) 0.0844(3) -0.0656(4) 0.0257(12) Uani 1 1 d . . . H7B1 H 0.5466 0.0627 -0.0008 0.039 Uiso 1 1 calc R . . H7B2 H 0.5504 0.1124 -0.0931 0.039 Uiso 1 1 calc R . . H7B3 H 0.4659 0.052 -0.1194 0.039 Uiso 1 1 calc R . . C8B C 0.4108(4) 0.1239(2) -0.0402(4) 0.0203(11) Uani 1 1 d . . . C9B C 0.3931(4) 0.1267(2) 0.0569(4) 0.0189(11) Uani 1 1 d . . . C10B C 0.4578(4) 0.0961(2) 0.1514(4) 0.0215(11) Uani 1 1 d . . . C11B C 0.5181(4) 0.0754(2) 0.2347(4) 0.0208(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02216(10) 0.01958(11) 0.01457(11) 0.00077(10) 0.00773(7) 0.00198(9) N1 0.020(2) 0.024(2) 0.021(3) -0.003(2) 0.0010(18) 0.0003(17) N11 0.023(2) 0.017(2) 0.019(3) 0.0002(18) 0.0078(18) 0.0012(16) C12 0.030(3) 0.029(3) 0.029(4) -0.004(3) 0.007(3) -0.001(2) C13 0.033(3) 0.036(4) 0.032(4) 0.005(3) -0.002(3) 0.012(3) C14 0.046(4) 0.037(4) 0.020(3) -0.001(3) -0.001(3) 0.008(3) C15 0.044(3) 0.031(3) 0.017(3) -0.001(3) 0.009(3) -0.003(3) C16 0.032(3) 0.019(3) 0.018(3) -0.004(2) 0.011(2) -0.001(2) C17 0.034(3) 0.021(3) 0.014(3) 0.001(2) 0.010(2) -0.005(2) C18 0.046(3) 0.036(3) 0.015(3) 0.000(3) 0.015(3) -0.002(3) C19 0.052(4) 0.036(4) 0.031(4) -0.008(3) 0.026(3) 0.009(3) C20 0.032(3) 0.028(3) 0.038(4) -0.002(3) 0.016(3) 0.008(2) C21 0.023(3) 0.023(3) 0.031(3) 0.003(2) 0.006(2) 0.002(2) S1A 0.0293(7) 0.0369(9) 0.0265(8) 0.0048(7) 0.0129(6) 0.0096(6) S2A 0.0299(7) 0.0395(9) 0.0234(8) 0.0008(7) 0.0084(6) 0.0062(6) S3A 0.0287(7) 0.0376(9) 0.0255(8) 0.0054(7) 0.0151(6) 0.0090(6) S4A 0.0308(7) 0.0357(9) 0.0241(8) 0.0028(7) 0.0136(6) 0.0066(6) S1B 0.0325(7) 0.0364(9) 0.0168(8) 0.0047(6) 0.0104(6) 0.0039(6) S2B 0.0281(7) 0.0364(8) 0.0178(8) 0.0034(6) 0.0096(6) 0.0075(6) S3B 0.0257(6) 0.0323(8) 0.0160(7) 0.0017(6) 0.0095(5) 0.0042(5) S4B 0.0272(6) 0.0330(8) 0.0165(7) 0.0026(6) 0.0097(5) 0.0043(6) C1A 0.042(3) 0.038(4) 0.041(4) 0.011(3) 0.023(3) 0.013(3) C2A 0.023(3) 0.031(3) 0.035(4) 0.007(3) 0.016(2) 0.004(2) C3A 0.026(3) 0.038(4) 0.038(4) 0.007(3) 0.010(3) 0.003(2) C4A 0.038(3) 0.054(4) 0.038(4) 0.014(3) 0.009(3) 0.019(3) C5A 0.023(3) 0.030(3) 0.024(3) -0.001(2) 0.008(2) -0.002(2) C6A 0.023(2) 0.031(3) 0.020(3) -0.001(2) 0.011(2) 0.000(2) C7A 0.027(3) 0.031(3) 0.030(4) -0.001(3) 0.016(2) -0.001(2) C8A 0.023(3) 0.019(3) 0.037(4) -0.002(3) 0.018(2) 0.000(2) C9A 0.020(2) 0.026(3) 0.028(3) -0.001(3) 0.010(2) -0.002(2) C10A 0.025(3) 0.023(3) 0.020(3) 0.002(2) 0.007(2) -0.003(2) C11A 0.028(3) 0.022(3) 0.014(3) 0.002(2) 0.006(2) -0.001(2) C1B 0.040(3) 0.034(3) 0.025(4) 0.005(3) 0.001(3) 0.001(3) C2B 0.027(3) 0.019(3) 0.024(3) 0.005(2) 0.004(2) -0.001(2) C3B 0.025(3) 0.021(3) 0.021(3) 0.005(2) 0.005(2) 0.000(2) C4B 0.036(3) 0.049(4) 0.029(4) 0.003(3) 0.010(3) 0.016(3) C5B 0.029(3) 0.026(3) 0.016(3) -0.003(2) 0.011(2) -0.003(2) C6B 0.027(3) 0.025(3) 0.010(3) -0.001(2) 0.008(2) -0.003(2) C7B 0.028(3) 0.028(3) 0.021(3) 0.003(2) 0.006(2) 0.004(2) C8B 0.023(2) 0.021(3) 0.015(3) -0.001(2) 0.003(2) -0.003(2) C9B 0.022(2) 0.016(3) 0.020(3) 0.002(2) 0.009(2) -0.0018(19) C10B 0.025(3) 0.018(3) 0.023(3) -0.003(2) 0.009(2) 0.000(2) C11B 0.026(3) 0.018(3) 0.021(3) -0.001(2) 0.009(2) 0.003(2) #----------------------------------------------------------------------------# # 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 C11A 1.948(5) . ? Pt1 C11B 1.949(5) . ? Pt1 N11 2.061(4) . ? Pt1 N1 2.068(4) . ? N1 C12 1.334(6) . ? N1 C16 1.354(6) . ? N11 C21 1.346(6) . ? N11 C17 1.364(6) . ? C12 C13 1.375(8) . ? C12 H12 0.95 . ? C13 C14 1.376(8) . ? C13 H13 0.95 . ? C14 C15 1.377(7) . ? C14 H14 0.95 . ? C15 C16 1.383(7) . ? C15 H15 0.95 . ? C16 C17 1.466(7) . ? C17 C18 1.392(7) . ? C18 C19 1.386(7) . ? C18 H18 0.95 . ? C19 C20 1.360(8) . ? C19 H19 0.95 . ? C20 C21 1.378(7) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? S1A C2A 1.771(5) . ? S1A C5A 1.771(6) . ? S2A C5A 1.749(6) . ? S2A C3A 1.765(6) . ? S3A C6A 1.745(5) . ? S3A C8A 1.762(5) . ? S4A C6A 1.763(5) . ? S4A C9A 1.775(5) . ? S1B C5B 1.755(5) . ? S1B C2B 1.770(5) . ? S2B C5B 1.753(5) . ? S2B C3B 1.771(5) . ? S3B C8B 1.748(5) . ? S3B C6B 1.753(5) . ? S4B C6B 1.772(5) . ? S4B C9B 1.779(5) . ? C1A C2A 1.495(7) . ? C1A H1A1 0.98 . ? C1A H1A2 0.98 . ? C1A H1A3 0.98 . ? C2A C3A 1.301(8) . ? C3A C4A 1.511(8) . ? C4A H4A1 0.98 . ? C4A H4A2 0.98 . ? C4A H4A3 0.98 . ? C5A C6A 1.354(7) . ? C7A C8A 1.483(7) . ? C7A H7A1 0.98 . ? C7A H7A2 0.98 . ? C7A H7A3 0.98 . ? C8A C9A 1.344(7) . ? C9A C10A 1.424(7) . ? C10A C11A 1.207(7) . ? C1B C2B 1.498(7) . ? C1B H1B1 0.98 . ? C1B H1B2 0.98 . ? C1B H1B3 0.98 . ? C2B C3B 1.336(7) . ? C3B C4B 1.475(7) . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? C5B C6B 1.348(7) . ? C7B C8B 1.493(7) . ? C7B H7B1 0.98 . ? C7B H7B2 0.98 . ? C7B H7B3 0.98 . ? C8B C9B 1.352(7) . ? C9B C10B 1.415(7) . ? C10B C11B 1.208(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 C11A Pt1 C11B 88.9(2) . . ? C11A Pt1 N11 174.54(18) . . ? C11B Pt1 N11 96.11(18) . . ? C11A Pt1 N1 95.87(19) . . ? C11B Pt1 N1 175.18(18) . . ? N11 Pt1 N1 79.10(16) . . ? C12 N1 C16 119.0(5) . . ? C12 N1 Pt1 125.6(4) . . ? C16 N1 Pt1 115.3(3) . . ? C21 N11 C17 119.3(5) . . ? C21 N11 Pt1 125.8(4) . . ? C17 N11 Pt1 114.8(3) . . ? N1 C12 C13 122.5(6) . . ? N1 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C12 C13 C14 118.7(5) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 119.6(5) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.1(5) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? N1 C16 C15 121.1(5) . . ? N1 C16 C17 115.0(5) . . ? C15 C16 C17 123.9(5) . . ? N11 C17 C18 120.6(5) . . ? N11 C17 C16 115.6(5) . . ? C18 C17 C16 123.9(5) . . ? C19 C18 C17 119.3(5) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C18 119.2(5) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 120.2(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? N11 C21 C20 121.4(5) . . ? N11 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C2A S1A C5A 95.5(3) . . ? C5A S2A C3A 95.1(3) . . ? C6A S3A C8A 96.5(3) . . ? C6A S4A C9A 95.3(2) . . ? C5B S1B C2B 95.3(2) . . ? C5B S2B C3B 95.8(3) . . ? C8B S3B C6B 96.2(2) . . ? C6B S4B C9B 95.4(2) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C3A C2A C1A 127.1(5) . . ? C3A C2A S1A 116.5(4) . . ? C1A C2A S1A 116.4(4) . . ? C2A C3A C4A 126.5(5) . . ? C2A C3A S2A 118.8(4) . . ? C4A C3A S2A 114.7(5) . . ? C3A C4A H4A1 109.5 . . ? C3A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C3A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C6A C5A S2A 123.3(4) . . ? C6A C5A S1A 123.3(4) . . ? S2A C5A S1A 113.4(3) . . ? C5A C6A S3A 124.4(4) . . ? C5A C6A S4A 121.3(4) . . ? S3A C6A S4A 114.3(3) . . ? C8A C7A H7A1 109.5 . . ? C8A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C8A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C9A C8A C7A 125.7(5) . . ? C9A C8A S3A 116.6(4) . . ? C7A C8A S3A 117.7(4) . . ? C8A C9A C10A 126.2(5) . . ? C8A C9A S4A 117.3(4) . . ? C10A C9A S4A 116.5(4) . . ? C11A C10A C9A 177.4(6) . . ? C10A C11A Pt1 175.7(5) . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C3B C2B C1B 127.6(5) . . ? C3B C2B S1B 117.7(4) . . ? C1B C2B S1B 114.6(4) . . ? C2B C3B C4B 127.7(5) . . ? C2B C3B S2B 116.5(4) . . ? C4B C3B S2B 115.8(4) . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C6B C5B S2B 122.8(4) . . ? C6B C5B S1B 122.6(4) . . ? S2B C5B S1B 114.5(3) . . ? C5B C6B S3B 123.6(4) . . ? C5B C6B S4B 122.3(4) . . ? S3B C6B S4B 114.0(3) . . ? C8B C7B H7B1 109.5 . . ? C8B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C8B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C9B C8B C7B 124.3(5) . . ? C9B C8B S3B 117.7(4) . . ? C7B C8B S3B 117.9(4) . . ? C8B C9B C10B 127.1(5) . . ? C8B C9B S4B 116.4(4) . . ? C10B C9B S4B 116.5(4) . . ? C11B C10B C9B 173.8(5) . . ? C10B C11B Pt1 177.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11A Pt1 N1 C12 -3.0(4) . . . . ? N11 Pt1 N1 C12 179.2(4) . . . . ? C11A Pt1 N1 C16 -179.4(4) . . . . ? N11 Pt1 N1 C16 2.8(3) . . . . ? C11B Pt1 N11 C21 -2.1(4) . . . . ? N1 Pt1 N11 C21 178.4(4) . . . . ? C11B Pt1 N11 C17 179.5(4) . . . . ? N1 Pt1 N11 C17 0.0(3) . . . . ? C16 N1 C12 C13 0.9(8) . . . . ? Pt1 N1 C12 C13 -175.4(4) . . . . ? N1 C12 C13 C14 0.4(9) . . . . ? C12 C13 C14 C15 -0.5(9) . . . . ? C13 C14 C15 C16 -0.6(9) . . . . ? C12 N1 C16 C15 -2.0(7) . . . . ? Pt1 N1 C16 C15 174.6(4) . . . . ? C12 N1 C16 C17 178.4(4) . . . . ? Pt1 N1 C16 C17 -5.0(6) . . . . ? C14 C15 C16 N1 1.9(8) . . . . ? C14 C15 C16 C17 -178.6(5) . . . . ? C21 N11 C17 C18 0.5(7) . . . . ? Pt1 N11 C17 C18 179.0(4) . . . . ? C21 N11 C17 C16 178.9(4) . . . . ? Pt1 N11 C17 C16 -2.6(5) . . . . ? N1 C16 C17 N11 5.1(7) . . . . ? C15 C16 C17 N11 -174.5(5) . . . . ? N1 C16 C17 C18 -176.6(5) . . . . ? C15 C16 C17 C18 3.8(8) . . . . ? N11 C17 C18 C19 -0.5(8) . . . . ? C16 C17 C18 C19 -178.8(5) . . . . ? C17 C18 C19 C20 0.9(9) . . . . ? C18 C19 C20 C21 -1.2(9) . . . . ? C17 N11 C21 C20 -0.8(7) . . . . ? Pt1 N11 C21 C20 -179.1(4) . . . . ? C19 C20 C21 N11 1.2(8) . . . . ? C5A S1A C2A C3A -3.8(5) . . . . ? C5A S1A C2A C1A 177.6(4) . . . . ? C1A C2A C3A C4A -1.6(10) . . . . ? S1A C2A C3A C4A -180.0(5) . . . . ? C1A C2A C3A S2A 176.9(5) . . . . ? S1A C2A C3A S2A -1.5(7) . . . . ? C5A S2A C3A C2A 6.0(5) . . . . ? C5A S2A C3A C4A -175.3(5) . . . . ? C3A S2A C5A C6A 173.8(5) . . . . ? C3A S2A C5A S1A -8.1(3) . . . . ? C2A S1A C5A C6A -174.4(5) . . . . ? C2A S1A C5A S2A 7.6(3) . . . . ? S2A C5A C6A S3A 177.4(3) . . . . ? S1A C5A C6A S3A -0.4(7) . . . . ? S2A C5A C6A S4A -0.3(7) . . . . ? S1A C5A C6A S4A -178.1(3) . . . . ? C8A S3A C6A C5A -177.1(5) . . . . ? C8A S3A C6A S4A 0.7(3) . . . . ? C9A S4A C6A C5A 176.5(5) . . . . ? C9A S4A C6A S3A -1.3(3) . . . . ? C6A S3A C8A C9A 0.6(5) . . . . ? C6A S3A C8A C7A -179.8(4) . . . . ? C7A C8A C9A C10A 0.7(9) . . . . ? S3A C8A C9A C10A -179.7(4) . . . . ? C7A C8A C9A S4A 178.7(4) . . . . ? S3A C8A C9A S4A -1.6(6) . . . . ? C6A S4A C9A C8A 1.8(5) . . . . ? C6A S4A C9A C10A -179.9(4) . . . . ? C5B S1B C2B C3B 2.4(5) . . . . ? C5B S1B C2B C1B -179.5(4) . . . . ? C1B C2B C3B C4B -0.1(9) . . . . ? S1B C2B C3B C4B 177.7(4) . . . . ? C1B C2B C3B S2B -177.7(4) . . . . ? S1B C2B C3B S2B 0.1(6) . . . . ? C5B S2B C3B C2B -2.6(5) . . . . ? C5B S2B C3B C4B 179.6(4) . . . . ? C3B S2B C5B C6B 179.9(4) . . . . ? C3B S2B C5B S1B 4.1(3) . . . . ? C2B S1B C5B C6B -179.9(5) . . . . ? C2B S1B C5B S2B -4.0(3) . . . . ? S2B C5B C6B S3B -176.7(3) . . . . ? S1B C5B C6B S3B -1.2(7) . . . . ? S2B C5B C6B S4B -0.9(6) . . . . ? S1B C5B C6B S4B 174.6(3) . . . . ? C8B S3B C6B C5B -177.9(4) . . . . ? C8B S3B C6B S4B 6.0(3) . . . . ? C9B S4B C6B C5B 178.7(4) . . . . ? C9B S4B C6B S3B -5.1(3) . . . . ? C6B S3B C8B C9B -4.9(4) . . . . ? C6B S3B C8B C7B 177.3(4) . . . . ? C7B C8B C9B C10B 3.0(8) . . . . ? S3B C8B C9B C10B -174.6(4) . . . . ? C7B C8B C9B S4B 179.6(4) . . . . ? S3B C8B C9B S4B 2.0(5) . . . . ? C6B S4B C9B C8B 1.9(4) . . . . ? C6B S4B C9B C10B 178.9(4) . . . . ? data_complex2 _database_code_depnum_ccdc_archive 'CCDC 816626' #TrackingRef 'CIFFileDLorcy.cif' _audit_creation_date 2012-05-15T11:59:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C40 H42 N2 Pt S8)' _chemical_formula_sum 'C80 H84 N4 Pt2 S16' _chemical_formula_weight 2004.65 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c m n' _symmetry_space_group_name_Hall '-P 2n 2ac' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x, -y-1/2, z' _cell_length_a 17.6121(12) _cell_length_b 21.4397(14) _cell_length_c 38.038(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 14363.1(16) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5103 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.28 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6024 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 0.718 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # 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 0.500 0.209 0.000 1031 338 ' ' 2 0.000 0.015 0.500 1031 338 ' ' 3 0.178 0.750 0.770 235 52 ' ' 4 0.186 0.152 0.668 9 2 ' ' 5 0.186 0.348 0.668 9 1 ' ' 6 0.321 0.750 0.270 235 52 ' ' 7 0.314 0.152 0.168 9 1 ' ' 8 0.314 0.348 0.168 9 1 ' ' 9 0.678 0.250 0.730 235 52 ' ' 10 0.686 0.652 0.831 9 1 ' ' 11 0.686 0.848 0.831 9 1 ' ' 12 0.821 0.250 0.230 235 51 ' ' 13 0.814 0.652 0.331 9 1 ' ' 14 0.814 0.848 0.331 9 1 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_unetI/netI 0.0881 _diffrn_reflns_number 70212 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 16876 _reflns_number_gt 9669 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # 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^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 16876 _refine_ls_number_parameters 744 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.101 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.65 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.141 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in C 2/c CELL 0.71073 24.4240 3.9155 27.2910 90.000 107.981 90.000 ZERR 8.00 0.0016 0.0002 0.0015 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 128 112 16 8 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.057500 0.650700 FVAR 0.40742 C1 1 0.454255 0.561464 0.181153 11.00000 0.02705 0.03635 = 0.02544 0.00018 0.00365 -0.00985 AFIX 137 H1A 2 0.452345 0.387428 0.206381 11.00000 -1.50000 H1B 2 0.425159 0.737424 0.179337 11.00000 -1.50000 H1C 2 0.492581 0.666031 0.191656 11.00000 -1.50000 AFIX 0 C2 1 0.443006 0.397839 0.129040 11.00000 0.02543 0.02454 = 0.02199 0.00511 0.00378 -0.00233 C3 1 0.485076 0.368908 0.105861 11.00000 0.02409 0.03763 = 0.03042 0.00430 0.00639 -0.00459 AFIX 43 H3 2 0.522487 0.453924 0.123187 11.00000 -1.20000 AFIX 0 C4 1 0.474539 0.216302 0.056907 11.00000 0.02734 0.04167 = 0.03431 0.00191 0.01443 -0.00038 AFIX 43 H4 2 0.504608 0.203662 0.041691 11.00000 -1.20000 AFIX 0 C5 1 0.421355 0.086435 0.031195 11.00000 0.03173 0.03313 = 0.02401 -0.00005 0.00905 0.00309 AFIX 43 H5 2 0.414474 -0.016794 -0.001659 11.00000 -1.20000 AFIX 0 C6 1 0.376954 0.107461 0.053955 11.00000 0.02423 0.02351 = 0.02160 0.00211 0.00393 0.00162 C7 1 0.387009 0.267447 0.102605 11.00000 0.02278 0.02095 = 0.02093 0.00428 0.00513 0.00080 N8 3 0.344065 0.302571 0.124628 11.00000 0.02207 0.02186 = 0.02069 0.00183 0.00410 -0.00208 C9 1 0.292631 0.178654 0.098931 11.00000 0.02262 0.01837 = 0.01971 0.00308 0.00302 -0.00002 C10 1 0.284069 0.003247 0.051207 11.00000 0.02206 0.02585 = 0.02206 -0.00213 0.00226 -0.00105 AFIX 43 H10 2 0.247271 -0.093266 0.034812 11.00000 -1.20000 AFIX 0 N11 3 0.323999 -0.032009 0.028811 11.00000 0.02495 0.02871 = 0.02307 -0.00193 0.00452 0.00071 C12 1 0.244383 0.230614 0.120263 11.00000 0.02263 0.01883 = 0.01934 0.00176 0.00410 -0.00096 C13 1 0.253823 0.390708 0.167879 11.00000 0.02276 0.02393 = 0.02259 -0.00178 0.00145 -0.00030 AFIX 43 H13 2 0.291668 0.462454 0.186577 11.00000 -1.20000 AFIX 0 C14 1 0.209470 0.447805 0.188609 11.00000 0.03001 0.02442 = 0.01911 -0.00276 0.00513 0.00085 AFIX 43 H14 2 0.217016 0.554527 0.221289 11.00000 -1.20000 AFIX 0 C15 1 0.153778 0.347357 0.161111 11.00000 0.02625 0.02289 = 0.02466 0.00312 0.00966 0.00172 C16 1 0.143411 0.190577 0.113422 11.00000 0.02190 0.03655 = 0.02550 -0.00293 0.00453 -0.00717 AFIX 43 H16 2 0.105389 0.123076 0.094525 11.00000 -1.20000 AFIX 0 C17 1 0.187799 0.132386 0.093370 11.00000 0.02683 0.02925 = 0.01981 -0.00255 0.00520 -0.00530 AFIX 43 H17 2 0.180025 0.023960 0.060793 11.00000 -1.20000 AFIX 0 O18 4 0.106556 0.391256 0.177574 11.00000 0.02918 0.03933 = 0.02977 -0.00548 0.01272 -0.00171 C19 1 0.114666 0.562855 0.225349 11.00000 0.03924 0.03421 = 0.03492 -0.00509 0.01953 0.00188 AFIX 137 H19A 2 0.141982 0.434113 0.253085 11.00000 -1.50000 H19B 2 0.077728 0.579952 0.232312 11.00000 -1.50000 H19C 2 0.129865 0.792497 0.223500 11.00000 -1.50000 HKLF 4 REM import in C 2/c REM R1 = 0.0459 for 2176 Fo > 4sig(Fo) and 0.0605 for all 2808 data REM 174 parameters refined using 0 restraints END WGHT 0.0567 0.6601 REM Highest difference peak 0.27, deepest hole -0.22, 1-sigma level 0.04 Q1 1 0.2487 0.3640 0.1395 11.00000 0.05 0.27 Q2 1 0.3807 0.2614 0.0726 11.00000 0.05 0.25 Q3 1 0.2665 0.2327 0.1100 11.00000 0.05 0.25 Q4 1 0.2197 0.1175 0.1098 11.00000 0.05 0.25 Q5 1 0.4103 0.4103 0.1129 11.00000 0.05 0.23 Q6 1 0.4194 0.2418 0.1217 11.00000 0.05 0.22 Q7 1 0.1511 0.2101 0.1425 11.00000 0.05 0.21 Q8 1 0.3695 0.2592 0.1150 11.00000 0.05 0.21 Q9 1 0.1799 0.4553 0.1695 11.00000 0.05 0.20 Q10 1 0.3495 0.0845 0.0392 11.00000 0.05 0.20 Q11 1 0.2861 0.1788 0.0718 11.00000 0.05 0.20 Q12 1 0.3193 0.1613 0.1152 11.00000 0.05 0.19 Q13 1 0.3144 0.2589 0.1072 11.00000 0.05 0.19 Q14 1 0.3857 0.1184 0.0873 11.00000 0.05 0.18 Q15 1 0.4486 0.4546 0.1548 11.00000 0.05 0.18 Q16 1 0.1301 0.4162 0.1654 11.00000 0.05 0.17 Q17 1 0.4645 0.2842 0.1238 11.00000 0.05 0.17 Q18 1 0.4286 0.5121 0.2032 11.00000 0.05 0.16 Q19 1 0.4800 0.2313 0.0857 11.00000 0.05 0.16 Q20 1 0.1824 0.3218 0.1780 11.00000 0.05 0.16 ; #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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' 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 0.623314(14) 0.084091(12) 0.506060(6) 0.03132(8) Uani 1 1 d . . . N1 N 0.6858(3) 0.0881(2) 0.46052(12) 0.0281(12) Uani 1 1 d . . . N11 N 0.5396(3) 0.0823(2) 0.46819(12) 0.0266(11) Uani 1 1 d . . . C112 C 0.7625(4) 0.0918(3) 0.45894(16) 0.0337(7) Uani 1 1 d . . . H112 H 0.7908 0.0946 0.4802 0.04 Uiso 1 1 calc R . . C113 C 0.8011(4) 0.0917(3) 0.42675(16) 0.0337(7) Uani 1 1 d . . . H113 H 0.8549 0.0941 0.4264 0.04 Uiso 1 1 calc R . . C114 C 0.7616(4) 0.0880(3) 0.39572(16) 0.0337(7) Uani 1 1 d . . . C115 C 0.6830(4) 0.0860(3) 0.39759(16) 0.0337(7) Uani 1 1 d . . . H115 H 0.6541 0.0843 0.3765 0.04 Uiso 1 1 calc R . . C116 C 0.6461(4) 0.0864(3) 0.42989(16) 0.0337(7) Uani 1 1 d . . . C117 C 0.5629(3) 0.0843(3) 0.43450(16) 0.0262(13) Uani 1 1 d . . . C118 C 0.5122(3) 0.0849(3) 0.40726(14) 0.0270(14) Uani 1 1 d . . . H118 H 0.531 0.0854 0.3839 0.032 Uiso 1 1 calc R . . C119 C 0.4350(4) 0.0846(3) 0.41254(15) 0.0292(14) Uani 1 1 d . . . C120 C 0.4111(4) 0.0816(3) 0.44826(16) 0.0361(16) Uani 1 1 d . . . H120 H 0.3585 0.0806 0.4538 0.043 Uiso 1 1 calc R . . C121 C 0.4640(4) 0.0802(3) 0.47468(16) 0.0363(16) Uani 1 1 d . . . H121 H 0.447 0.0775 0.4984 0.044 Uiso 1 1 calc R . . C122 C 0.8029(4) 0.0872(3) 0.36066(17) 0.0369(16) Uani 1 1 d . . . C123 C 0.8562(4) 0.0300(3) 0.36036(19) 0.054(2) Uani 1 1 d . . . H12A H 0.8259 -0.0083 0.3617 0.081 Uiso 1 1 calc R . . H12B H 0.8906 0.0321 0.3806 0.081 Uiso 1 1 calc R . . H12C H 0.8859 0.0298 0.3386 0.081 Uiso 1 1 calc R . . C124 C 0.8497(4) 0.1472(3) 0.35704(17) 0.0477(18) Uani 1 1 d . . . H12D H 0.8778 0.1463 0.3348 0.072 Uiso 1 1 calc R . . H12E H 0.8856 0.1502 0.3767 0.072 Uiso 1 1 calc R . . H12F H 0.8157 0.1833 0.3574 0.072 Uiso 1 1 calc R . . C125 C 0.7506(4) 0.0826(3) 0.32941(15) 0.0398(17) Uani 1 1 d . . . H12G H 0.7207 0.0442 0.331 0.06 Uiso 1 1 calc R . . H12H H 0.7807 0.0821 0.3077 0.06 Uiso 1 1 calc R . . H12I H 0.7163 0.1186 0.3291 0.06 Uiso 1 1 calc R . . C126 C 0.3759(4) 0.0857(3) 0.38336(16) 0.0346(15) Uani 1 1 d . . . C127 C 0.4143(4) 0.0891(3) 0.34646(18) 0.050(2) Uani 1 1 d . . . H12J H 0.4459 0.1267 0.345 0.075 Uiso 1 1 calc R . . H12K H 0.3751 0.0907 0.3282 0.075 Uiso 1 1 calc R . . H12L H 0.4461 0.0522 0.3429 0.075 Uiso 1 1 calc R . . C128 C 0.3249(4) 0.1425(3) 0.38815(19) 0.0509(19) Uani 1 1 d . . . H12M H 0.3024 0.1417 0.4117 0.076 Uiso 1 1 calc R . . H12N H 0.2844 0.1417 0.3705 0.076 Uiso 1 1 calc R . . H12O H 0.355 0.1806 0.3853 0.076 Uiso 1 1 calc R . . C129 C 0.3280(4) 0.0273(3) 0.38522(17) 0.0447(18) Uani 1 1 d . . . H12P H 0.3605 -0.0094 0.3821 0.067 Uiso 1 1 calc R . . H12Q H 0.2896 0.0283 0.3666 0.067 Uiso 1 1 calc R . . H12R H 0.3028 0.0252 0.4082 0.067 Uiso 1 1 calc R . . S1A S 1.03183(10) 0.08846(9) 0.68050(4) 0.0425(4) Uani 1 1 d . . . S2A S 0.87223(10) 0.08321(9) 0.70294(5) 0.0457(5) Uani 1 1 d . . . S3A S 0.97729(10) 0.08681(8) 0.59831(4) 0.0408(4) Uani 1 1 d . . . S4A S 0.81813(10) 0.08504(9) 0.62169(4) 0.0421(4) Uani 1 1 d . . . C1A C 1.0833(5) 0.0794(4) 0.74927(18) 0.064(2) Uani 1 1 d . . . H1A1 H 1.0849 0.1159 0.7648 0.097 Uiso 1 1 calc R . . H1A2 H 1.129 0.0788 0.7345 0.097 Uiso 1 1 calc R . . H1A3 H 1.0813 0.0414 0.7635 0.097 Uiso 1 1 calc R . . C2A C 1.0137(4) 0.0829(3) 0.72616(17) 0.0430(18) Uani 1 1 d . . . C3A C 0.9415(5) 0.0813(3) 0.73684(16) 0.0447(18) Uani 1 1 d . . . C4A C 0.9127(5) 0.0785(4) 0.77370(17) 0.060(2) Uani 1 1 d . . . H4A1 H 0.9555 0.0739 0.7899 0.09 Uiso 1 1 calc R . . H4A2 H 0.8785 0.0427 0.7762 0.09 Uiso 1 1 calc R . . H4A3 H 0.8851 0.117 0.7792 0.09 Uiso 1 1 calc R . . C5A C 0.9376(4) 0.0859(3) 0.66735(15) 0.0330(15) Uani 1 1 d . . . C6A C 0.9144(4) 0.0863(3) 0.63431(16) 0.0352(16) Uani 1 1 d . . . C7A C 0.9348(4) 0.0886(3) 0.52822(17) 0.0504(19) Uani 1 1 d . . . H7A1 H 0.9543 0.0473 0.5219 0.076 Uiso 1 1 calc R . . H7A2 H 0.9754 0.1196 0.5258 0.076 Uiso 1 1 calc R . . H7A3 H 0.8926 0.0996 0.5126 0.076 Uiso 1 1 calc R . . C8A C 0.9077(4) 0.0876(3) 0.56536(17) 0.0361(16) Uani 1 1 d . . . C9A C 0.8346(4) 0.0860(3) 0.57543(16) 0.0339(15) Uani 1 1 d . . . C10A C 0.7684(4) 0.0861(3) 0.55393(16) 0.0327(15) Uani 1 1 d . . . C11A C 0.7117(4) 0.0862(3) 0.53721(15) 0.0331(15) Uani 1 1 d . . . S1B S 0.30541(10) 0.08297(8) 0.71798(4) 0.0378(4) Uani 1 1 d . . . S2B S 0.47180(10) 0.08321(9) 0.72384(4) 0.0429(4) Uani 1 1 d . . . S3B S 0.32225(10) 0.08298(8) 0.63190(4) 0.0364(4) Uani 1 1 d . . . S4B S 0.48845(10) 0.08054(9) 0.63971(4) 0.0397(4) Uani 1 1 d . . . C1B C 0.2879(4) 0.0833(3) 0.79007(15) 0.0477(19) Uani 1 1 d . . . H1B1 H 0.2641 0.0421 0.7918 0.072 Uiso 1 1 calc R . . H1B2 H 0.249 0.1148 0.7851 0.072 Uiso 1 1 calc R . . H1B3 H 0.3132 0.0933 0.8123 0.072 Uiso 1 1 calc R . . C2B C 0.3451(4) 0.0829(3) 0.76101(16) 0.0362(16) Uani 1 1 d . . . C3B C 0.4187(4) 0.0842(3) 0.76289(18) 0.0414(17) Uani 1 1 d . . . C4B C 0.4664(4) 0.0838(3) 0.79571(15) 0.0466(19) Uani 1 1 d . . . H4B1 H 0.4963 0.1223 0.7969 0.07 Uiso 1 1 calc R . . H4B2 H 0.5007 0.0478 0.7953 0.07 Uiso 1 1 calc R . . H4B3 H 0.4334 0.0811 0.8164 0.07 Uiso 1 1 calc R . . C5B C 0.3922(4) 0.0830(3) 0.69589(16) 0.0321(15) Uani 1 1 d . . . C6B C 0.3992(3) 0.0813(3) 0.66129(16) 0.0283(14) Uani 1 1 d . . . C7B C 0.3325(4) 0.0788(3) 0.55951(16) 0.0462(18) Uani 1 1 d . . . H7B1 H 0.3239 0.1218 0.5517 0.069 Uiso 1 1 calc R . . H7B2 H 0.2835 0.0581 0.5632 0.069 Uiso 1 1 calc R . . H7B3 H 0.3613 0.0562 0.5415 0.069 Uiso 1 1 calc R . . C8B C 0.3765(4) 0.0791(3) 0.59338(15) 0.0331(15) Uani 1 1 d . . . C9B C 0.4514(4) 0.0783(3) 0.59658(14) 0.0288(14) Uani 1 1 d . . . C10B C 0.5068(4) 0.0786(3) 0.56819(16) 0.0367(16) Uani 1 1 d . . . C11B C 0.5529(3) 0.0802(3) 0.54571(15) 0.0286(14) Uani 1 1 d . . . Pt2 Pt 0.866451(19) 0.25 0.470566(8) 0.02918(10) Uani 1 2 d S . . N2 N 0.8032(4) 0.25 0.51532(18) 0.0302(17) Uani 1 2 d S . . N22 N 0.9508(4) 0.25 0.50713(17) 0.0297(17) Uani 1 2 d S . . C212 C 0.7271(5) 0.25 0.5184(3) 0.042(2) Uani 1 2 d S . . H212 H 0.6972 0.25 0.4976 0.051 Uiso 1 2 calc SR . . C213 C 0.6899(5) 0.25 0.5511(2) 0.039(2) Uani 1 2 d S . . H213 H 0.636 0.25 0.5517 0.047 Uiso 1 2 calc SR . . C214 C 0.7289(5) 0.25 0.5821(2) 0.034(2) Uani 1 2 d S . . C215 C 0.8097(5) 0.25 0.5807(2) 0.033(2) Uani 1 2 d S . . H215 H 0.8384 0.25 0.6018 0.04 Uiso 1 2 calc SR . . C216 C 0.8470(5) 0.25 0.5480(2) 0.029(2) Uani 1 2 d S . . C217 C 0.9269(4) 0.25 0.5424(2) 0.0261(19) Uani 1 2 d S . . C218 C 0.9799(4) 0.25 0.5691(2) 0.0233(19) Uani 1 2 d S . . H218 H 0.963 0.25 0.5928 0.028 Uiso 1 2 calc SR . . C219 C 1.0572(5) 0.25 0.5622(2) 0.029(2) Uani 1 2 d S . . C220 C 1.0769(5) 0.25 0.5276(2) 0.034(2) Uani 1 2 d S . . H220 H 1.1294 0.25 0.5217 0.041 Uiso 1 2 calc SR . . C221 C 1.0264(5) 0.25 0.5013(2) 0.039(2) Uani 1 2 d S . . H221 H 1.0443 0.25 0.4778 0.047 Uiso 1 2 calc SR . . C222 C 0.6879(5) 0.25 0.6179(2) 0.035(2) Uani 1 2 d S . . C223 C 0.6390(3) 0.1911(3) 0.61906(18) 0.0460(18) Uani 1 1 d . . . H22A H 0.6034 0.1914 0.5992 0.069 Uiso 1 1 calc R . . H22B H 0.6105 0.1899 0.6412 0.069 Uiso 1 1 calc R . . H22C H 0.6717 0.1542 0.6175 0.069 Uiso 1 1 calc R . . C224 C 0.7423(6) 0.25 0.6486(2) 0.047(3) Uani 1 2 d S . . H22D H 0.7759 0.2127 0.6468 0.07 Uiso 0.5 1 d P . . H22E H 0.7143 0.25 0.6705 0.07 Uiso 1 2 d S . . H22F H 0.7759 0.2873 0.6468 0.07 Uiso 0.5 1 d P . . C226 C 1.1169(5) 0.25 0.5919(2) 0.033(2) Uani 1 2 d S . . C227 C 1.1666(4) 0.1923(3) 0.58735(17) 0.051(2) Uani 1 1 d . . . H22G H 1.205 0.1912 0.606 0.076 Uiso 1 1 calc R . . H22H H 1.1917 0.1939 0.5644 0.076 Uiso 1 1 calc R . . H22I H 1.1349 0.1548 0.5887 0.076 Uiso 1 1 calc R . . C228 C 1.0817(5) 0.25 0.6290(2) 0.044(3) Uani 1 2 d S . . H22J H 1.1223 0.25 0.6467 0.067 Uiso 1 2 calc SR . . H22K H 1.0503 0.2127 0.632 0.067 Uiso 0.5 1 calc PR . . H22L H 1.0503 0.2873 0.632 0.067 Uiso 0.5 1 calc PR . . S1C S 0.45264(15) 0.25 0.29812(6) 0.0481(7) Uani 1 2 d S . . S2C S 0.61191(15) 0.25 0.27409(7) 0.0439(6) Uani 1 2 d S . . S3C S 0.51041(14) 0.25 0.38006(6) 0.0389(6) Uani 1 2 d S . . S4C S 0.66860(13) 0.25 0.35496(6) 0.0395(6) Uani 1 2 d S . . C1C C 0.3984(6) 0.25 0.2298(3) 0.060(3) Uani 1 2 d S . . H1C1 H 0.3535 0.25 0.245 0.091 Uiso 1 2 calc SR . . H1C2 H 0.3978 0.2127 0.2149 0.091 Uiso 0.5 1 calc PR . . H1C3 H 0.3978 0.2873 0.2149 0.091 Uiso 0.5 1 calc PR . . C2C C 0.4696(6) 0.25 0.2523(3) 0.047(3) Uani 1 2 d S . . C3C C 0.5408(6) 0.25 0.2410(2) 0.040(2) Uani 1 2 d S . . C4C C 0.5711(6) 0.25 0.2036(2) 0.058(3) Uani 1 2 d S . . H4C1 H 0.6268 0.25 0.2041 0.087 Uiso 1 2 calc SR . . H4C2 H 0.5531 0.2873 0.1913 0.087 Uiso 0.5 1 calc PR . . H4C3 H 0.5531 0.2127 0.1913 0.087 Uiso 0.5 1 calc PR . . C5C C 0.5498(5) 0.25 0.3096(2) 0.029(2) Uani 1 2 d S . . C6C C 0.5716(5) 0.25 0.3438(2) 0.028(2) Uani 1 2 d S . . C7C C 0.5564(5) 0.25 0.4489(2) 0.042(2) Uani 1 2 d S . . H7C1 H 0.5008 0.25 0.4498 0.063 Uiso 1 2 calc SR . . H7C2 H 0.5759 0.2873 0.4607 0.063 Uiso 0.5 1 calc PR . . H7C3 H 0.5759 0.2127 0.4607 0.063 Uiso 0.5 1 calc PR . . C8C C 0.5811(5) 0.25 0.4125(2) 0.028(2) Uani 1 2 d S . . C9C C 0.6535(5) 0.25 0.4012(2) 0.032(2) Uani 1 2 d S . . C10C C 0.7196(5) 0.25 0.4233(2) 0.029(2) Uani 1 2 d S . . C11C C 0.7792(5) 0.25 0.4394(2) 0.0252(19) Uani 1 2 d S . . S1D S 1.19058(13) 0.25 0.25993(6) 0.0357(6) Uani 1 2 d S . . S2D S 1.02386(14) 0.25 0.25431(6) 0.0399(6) Uani 1 2 d S . . S3D S 1.17189(13) 0.25 0.34649(6) 0.0402(6) Uani 1 2 d S . . S4D S 1.00557(13) 0.25 0.33752(6) 0.0354(6) Uani 1 2 d S . . C1D C 1.2064(6) 0.25 0.1865(2) 0.050(3) Uani 1 2 d S . . H1D1 H 1.2585 0.25 0.1955 0.075 Uiso 1 2 calc SR . . H1D2 H 1.1982 0.2873 0.1721 0.075 Uiso 0.5 1 calc PR . . H1D3 H 1.1982 0.2127 0.1721 0.075 Uiso 0.5 1 calc PR . . C2D C 1.1513(5) 0.25 0.2169(2) 0.034(2) Uani 1 2 d S . . C3D C 1.0757(6) 0.25 0.2151(3) 0.049(2) Uani 1 2 d S . . C4D C 1.0299(5) 0.25 0.1819(2) 0.049(2) Uani 1 2 d S . . H4D1 H 0.9757 0.25 0.1877 0.074 Uiso 1 2 calc SR . . H4D2 H 1.042 0.2127 0.1681 0.074 Uiso 0.5 1 calc PR . . H4D3 H 1.042 0.2873 0.1681 0.074 Uiso 0.5 1 calc PR . . C5D C 1.1040(5) 0.25 0.2818(2) 0.027(2) Uani 1 2 d S . . C6D C 1.0959(5) 0.25 0.3169(2) 0.029(2) Uani 1 2 d S . . C7D C 1.1578(6) 0.25 0.4188(2) 0.061(3) Uani 1 2 d S . . H7D1 H 1.2126 0.25 0.4142 0.091 Uiso 1 2 calc SR . . H7D2 H 1.1442 0.2127 0.4323 0.091 Uiso 0.5 1 calc PR . . H7D3 H 1.1442 0.2873 0.4323 0.091 Uiso 0.5 1 calc PR . . C8D C 1.1155(5) 0.25 0.3844(2) 0.036(2) Uani 1 2 d S . . C9D C 1.0399(5) 0.25 0.3816(2) 0.027(2) Uani 1 2 d S . . C10D C 0.9856(5) 0.25 0.4083(2) 0.036(2) Uani 1 2 d S . . C11D C 0.9357(5) 0.25 0.4305(2) 0.030(2) Uani 1 2 d S . . 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 0.03892(15) 0.03664(15) 0.01839(12) 0.00022(11) -0.00038(12) 0.00049(12) N1 0.039(3) 0.032(3) 0.013(2) 0.001(2) 0.004(2) -0.005(3) N11 0.028(3) 0.032(3) 0.020(3) 0.000(2) -0.003(2) 0.005(2) C112 0.0394(17) 0.0333(16) 0.0285(15) -0.0012(15) 0.0037(13) -0.0006(15) C113 0.0394(17) 0.0333(16) 0.0285(15) -0.0012(15) 0.0037(13) -0.0006(15) C114 0.0394(17) 0.0333(16) 0.0285(15) -0.0012(15) 0.0037(13) -0.0006(15) C115 0.0394(17) 0.0333(16) 0.0285(15) -0.0012(15) 0.0037(13) -0.0006(15) C116 0.0394(17) 0.0333(16) 0.0285(15) -0.0012(15) 0.0037(13) -0.0006(15) C117 0.023(3) 0.021(3) 0.035(3) 0.002(3) 0.003(3) 0.005(3) C118 0.031(3) 0.034(3) 0.016(3) 0.002(3) 0.007(3) 0.004(3) C119 0.038(4) 0.030(3) 0.020(3) 0.003(3) -0.001(3) -0.001(3) C120 0.026(3) 0.052(4) 0.030(4) 0.006(4) 0.002(3) 0.004(3) C121 0.045(4) 0.045(4) 0.020(3) 0.003(3) 0.000(3) -0.001(3) C122 0.030(4) 0.040(4) 0.040(4) -0.006(3) 0.002(3) -0.005(3) C123 0.053(5) 0.053(5) 0.055(5) -0.010(4) 0.012(4) -0.005(4) C124 0.040(4) 0.059(5) 0.044(4) -0.010(4) 0.012(3) -0.003(4) C125 0.038(4) 0.058(5) 0.023(3) -0.008(3) 0.010(3) -0.015(4) C126 0.039(4) 0.040(4) 0.025(3) 0.000(3) -0.004(3) -0.007(3) C127 0.042(4) 0.069(5) 0.041(4) -0.002(4) -0.004(3) -0.015(4) C128 0.038(4) 0.055(5) 0.060(5) 0.011(4) -0.004(4) 0.014(4) C129 0.036(4) 0.059(5) 0.039(4) 0.002(4) -0.005(3) -0.007(4) S1A 0.0463(11) 0.0511(11) 0.0301(9) 0.0031(9) -0.0029(8) 0.0019(9) S2A 0.0495(11) 0.0540(11) 0.0335(9) 0.0065(9) 0.0032(9) 0.0029(10) S3A 0.0424(10) 0.0491(11) 0.0310(9) 0.0007(9) -0.0016(8) -0.0015(9) S4A 0.0364(10) 0.0601(12) 0.0298(9) -0.0008(9) -0.0019(8) -0.0010(9) C1A 0.080(6) 0.087(6) 0.026(4) -0.003(4) -0.015(4) -0.002(5) C2A 0.056(5) 0.047(4) 0.026(3) 0.005(4) -0.010(3) 0.001(4) C3A 0.074(5) 0.039(4) 0.021(3) -0.008(3) 0.006(4) 0.005(4) C4A 0.083(6) 0.071(6) 0.025(4) -0.004(4) 0.012(4) 0.006(5) C5A 0.042(4) 0.035(4) 0.022(3) 0.002(3) -0.003(3) -0.006(3) C6A 0.037(4) 0.045(4) 0.024(3) -0.004(3) 0.003(3) 0.001(3) C7A 0.050(4) 0.065(5) 0.037(4) -0.001(4) 0.001(4) -0.006(4) C8A 0.031(4) 0.046(4) 0.031(4) -0.004(3) -0.003(3) 0.003(3) C9A 0.049(4) 0.029(4) 0.024(3) 0.002(3) -0.002(3) 0.004(3) C10A 0.039(4) 0.035(4) 0.025(3) 0.001(3) -0.001(3) 0.004(3) C11A 0.051(4) 0.031(4) 0.017(3) 0.004(3) 0.001(3) 0.004(3) S1B 0.0406(10) 0.0472(11) 0.0255(8) -0.0004(8) 0.0035(7) -0.0056(9) S2B 0.0429(10) 0.0563(12) 0.0294(9) 0.0016(9) -0.0018(8) -0.0068(9) S3B 0.0384(10) 0.0465(10) 0.0245(8) -0.0022(8) 0.0010(7) -0.0004(9) S4B 0.0392(10) 0.0592(12) 0.0208(8) -0.0007(9) 0.0015(7) -0.0048(9) C1B 0.062(5) 0.061(5) 0.020(3) 0.000(4) 0.006(3) -0.005(4) C2B 0.056(4) 0.033(4) 0.019(3) -0.002(3) 0.002(3) -0.006(3) C3B 0.051(5) 0.039(4) 0.034(4) -0.004(4) 0.006(4) -0.009(4) C4B 0.066(5) 0.055(5) 0.018(3) 0.004(3) -0.008(3) -0.002(4) C5B 0.041(4) 0.029(3) 0.027(3) 0.001(3) -0.005(3) -0.008(3) C6B 0.028(3) 0.032(3) 0.026(3) -0.002(3) 0.005(3) -0.004(3) C7B 0.058(5) 0.048(4) 0.032(4) -0.005(4) -0.004(4) 0.003(4) C8B 0.045(4) 0.035(4) 0.020(3) -0.001(3) 0.006(3) 0.004(3) C9B 0.042(4) 0.030(3) 0.015(3) 0.001(3) 0.002(3) -0.001(3) C10B 0.043(4) 0.043(4) 0.024(3) 0.000(3) -0.004(3) 0.001(3) C11B 0.033(3) 0.033(4) 0.020(3) 0.000(3) -0.006(3) 0.005(3) Pt2 0.03084(19) 0.0368(2) 0.01994(17) 0 -0.00116(15) 0 N2 0.016(4) 0.043(5) 0.031(4) 0 -0.003(3) 0 N22 0.033(4) 0.029(4) 0.028(4) 0 0.012(4) 0 C212 0.038(6) 0.053(6) 0.036(5) 0 -0.008(5) 0 C213 0.023(5) 0.066(7) 0.027(5) 0 0.002(4) 0 C214 0.028(5) 0.037(5) 0.037(5) 0 0.006(4) 0 C215 0.044(6) 0.037(5) 0.019(4) 0 0.006(4) 0 C216 0.030(5) 0.026(5) 0.030(5) 0 0.003(4) 0 C217 0.017(4) 0.031(5) 0.030(5) 0 0.002(4) 0 C218 0.017(4) 0.032(5) 0.020(4) 0 0.000(3) 0 C219 0.027(5) 0.028(5) 0.033(5) 0 0.002(4) 0 C220 0.018(4) 0.065(7) 0.019(4) 0 0.002(4) 0 C221 0.038(5) 0.061(7) 0.020(5) 0 0.007(4) 0 C222 0.040(6) 0.052(6) 0.013(4) 0 0.012(4) 0 C223 0.039(4) 0.050(4) 0.048(4) 0.004(4) 0.017(3) -0.005(4) C224 0.063(7) 0.048(6) 0.029(5) 0 0.010(5) 0 C226 0.028(5) 0.051(6) 0.022(5) 0 -0.012(4) 0 C227 0.040(4) 0.073(5) 0.040(4) -0.006(4) -0.010(3) 0.015(4) C228 0.041(6) 0.062(7) 0.030(5) 0 -0.001(5) 0 S1C 0.0486(16) 0.0645(18) 0.0311(13) 0 -0.0160(12) 0 S2C 0.0511(16) 0.0464(15) 0.0343(14) 0 -0.0063(12) 0 S3C 0.0400(14) 0.0436(15) 0.0329(13) 0 -0.0103(11) 0 S4C 0.0346(14) 0.0599(17) 0.0238(12) 0 -0.0077(11) 0 C1C 0.061(7) 0.087(9) 0.033(6) 0 -0.020(5) 0 C2C 0.054(7) 0.044(6) 0.042(6) 0 -0.018(6) 0 C3C 0.061(7) 0.029(5) 0.031(5) 0 0.001(5) 0 C4C 0.062(7) 0.077(8) 0.034(6) 0 -0.007(6) 0 C5C 0.049(6) 0.016(4) 0.023(5) 0 -0.008(4) 0 C6C 0.026(5) 0.025(5) 0.034(5) 0 -0.011(4) 0 C7C 0.044(6) 0.055(6) 0.026(5) 0 -0.002(5) 0 C8C 0.027(5) 0.022(5) 0.034(5) 0 -0.004(4) 0 C9C 0.039(5) 0.026(5) 0.030(5) 0 -0.015(4) 0 C10C 0.049(6) 0.016(4) 0.022(5) 0 0.003(4) 0 C11C 0.035(5) 0.017(4) 0.024(4) 0 -0.002(4) 0 S1D 0.0365(13) 0.0463(15) 0.0244(12) 0 0.0040(10) 0 S2D 0.0361(13) 0.0536(16) 0.0299(13) 0 -0.0035(11) 0 S3D 0.0303(13) 0.0678(18) 0.0225(12) 0 0.0015(10) 0 S4D 0.0323(13) 0.0482(15) 0.0257(12) 0 0.0026(10) 0 C1D 0.072(7) 0.057(7) 0.020(5) 0 0.007(5) 0 C2D 0.048(6) 0.029(5) 0.027(5) 0 -0.004(4) 0 C3D 0.048(5) 0.059(5) 0.042(4) 0 -0.006(4) 0 C4D 0.048(5) 0.059(5) 0.042(4) 0 -0.006(4) 0 C5D 0.033(5) 0.029(5) 0.019(4) 0 -0.001(4) 0 C6D 0.040(5) 0.023(5) 0.023(5) 0 0.002(4) 0 C7D 0.048(6) 0.118(10) 0.017(5) 0 -0.006(5) 0 C8D 0.034(5) 0.057(6) 0.018(4) 0 0.004(4) 0 C9D 0.025(5) 0.029(5) 0.027(5) 0 -0.004(4) 0 C10D 0.039(6) 0.029(5) 0.039(6) 0 0.005(5) 0 C11D 0.029(5) 0.031(5) 0.031(5) 0 -0.010(4) 0 #----------------------------------------------------------------------------# # 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 C11B 1.954(6) . ? Pt1 C11A 1.957(7) . ? Pt1 N1 2.054(4) . ? Pt1 N11 2.061(5) . ? N1 C112 1.355(8) . ? N1 C116 1.359(7) . ? N11 C117 1.346(7) . ? N11 C121 1.356(8) . ? C112 C113 1.400(8) . ? C112 H112 0.95 . ? C113 C114 1.372(8) . ? C113 H113 0.95 . ? C114 C115 1.386(8) . ? C114 C122 1.519(8) . ? C115 C116 1.390(8) . ? C115 H115 0.95 . ? C116 C117 1.477(8) . ? C117 C118 1.368(8) . ? C118 C119 1.374(8) . ? C118 H118 0.95 . ? C119 C120 1.424(8) . ? C119 C126 1.522(8) . ? C120 C121 1.371(8) . ? C120 H120 0.95 . ? C121 H121 0.95 . ? C122 C125 1.507(8) . ? C122 C124 1.534(9) . ? C122 C123 1.545(9) . ? C123 H12A 0.98 . ? C123 H12B 0.98 . ? C123 H12C 0.98 . ? C124 H12D 0.98 . ? C124 H12E 0.98 . ? C124 H12F 0.98 . ? C125 H12G 0.98 . ? C125 H12H 0.98 . ? C125 H12I 0.98 . ? C126 C129 1.512(8) . ? C126 C128 1.524(9) . ? C126 C127 1.560(9) . ? C127 H12J 0.98 . ? C127 H12K 0.98 . ? C127 H12L 0.98 . ? C128 H12M 0.98 . ? C128 H12N 0.98 . ? C128 H12O 0.98 . ? C129 H12P 0.98 . ? C129 H12Q 0.98 . ? C129 H12R 0.98 . ? S1A C5A 1.734(6) . ? S1A C2A 1.770(7) . ? S2A C3A 1.776(7) . ? S2A C5A 1.778(6) . ? S3A C8A 1.753(6) . ? S3A C6A 1.762(6) . ? S4A C6A 1.762(7) . ? S4A C9A 1.783(6) . ? C1A C2A 1.510(9) . ? C1A H1A1 0.98 . ? C1A H1A2 0.98 . ? C1A H1A3 0.98 . ? C2A C3A 1.336(9) . ? C3A C4A 1.492(9) . ? C4A H4A1 0.98 . ? C4A H4A2 0.98 . ? C4A H4A3 0.98 . ? C5A C6A 1.322(8) . ? C7A C8A 1.491(9) . ? C7A H7A1 0.98 . ? C7A H7A2 0.98 . ? C7A H7A3 0.98 . ? C8A C9A 1.343(9) . ? C9A C10A 1.424(8) . ? C10A C11A 1.184(8) . ? S1B C5B 1.745(7) . ? S1B C2B 1.780(6) . ? S2B C3B 1.756(7) . ? S2B C5B 1.759(6) . ? S3B C8B 1.751(6) . ? S3B C6B 1.757(6) . ? S4B C9B 1.767(6) . ? S4B C6B 1.773(6) . ? C1B C2B 1.495(8) . ? C1B H1B1 0.98 . ? C1B H1B2 0.98 . ? C1B H1B3 0.98 . ? C2B C3B 1.298(9) . ? C3B C4B 1.506(9) . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? C5B C6B 1.322(8) . ? C7B C8B 1.504(8) . ? C7B H7B1 0.98 . ? C7B H7B2 0.98 . ? C7B H7B3 0.98 . ? C8B C9B 1.324(8) . ? C9B C10B 1.456(8) . ? C10B C11B 1.180(8) . ? Pt2 C11C 1.941(9) . ? Pt2 C11D 1.952(9) . ? Pt2 N2 2.034(7) . ? Pt2 N22 2.035(7) . ? N2 C212 1.347(11) . ? N2 C216 1.464(10) . ? N22 C221 1.350(11) . ? N22 C217 1.407(10) . ? C212 C213 1.406(12) . ? C212 H212 0.95 . ? C213 C214 1.364(11) . ? C213 H213 0.95 . ? C214 C215 1.424(12) . ? C214 C222 1.542(11) . ? C215 C216 1.404(11) . ? C215 H215 0.95 . ? C216 C217 1.423(11) . ? C217 C218 1.379(10) . ? C218 C219 1.387(11) . ? C218 H218 0.95 . ? C219 C220 1.362(11) . ? C219 C226 1.546(11) . ? C220 C221 1.337(11) . ? C220 H220 0.95 . ? C221 H221 0.95 . ? C222 C224 1.508(12) . ? C222 C223 1.530(8) . ? C222 C223 1.530(8) 8_565 ? C223 H22A 0.98 . ? C223 H22B 0.98 . ? C223 H22C 0.98 . ? C224 H22D 0.997 . ? C224 H22E 0.972 . ? C224 H22F 0.997(6) . ? C226 C227 1.525(8) 8_565 ? C226 C227 1.525(8) . ? C226 C228 1.541(12) . ? C227 H22G 0.98 . ? C227 H22H 0.98 . ? C227 H22I 0.98 . ? C228 H22J 0.98 . ? C228 H22K 0.98 . ? C228 H22L 0.98 . ? S1C C5C 1.766(9) . ? S1C C2C 1.770(10) . ? S2C C5C 1.739(9) . ? S2C C3C 1.777(10) . ? S3C C6C 1.750(9) . ? S3C C8C 1.754(8) . ? S4C C6C 1.761(8) . ? S4C C9C 1.779(9) . ? C1C C2C 1.518(12) . ? C1C H1C1 0.98 . ? C1C H1C2 0.98 . ? C1C H1C3 0.98 . ? C2C C3C 1.325(13) . ? C3C C4C 1.518(13) . ? C4C H4C1 0.98 . ? C4C H4C2 0.98 . ? C4C H4C3 0.98 . ? C5C C6C 1.356(11) . ? C7C C8C 1.449(11) . ? C7C H7C1 0.98 . ? C7C H7C2 0.98 . ? C7C H7C3 0.98 . ? C8C C9C 1.346(12) . ? C9C C10C 1.438(11) . ? C10C C11C 1.214(11) . ? S1D C5D 1.736(9) . ? S1D C2D 1.776(9) . ? S2D C3D 1.749(10) . ? S2D C5D 1.755(8) . ? S3D C6D 1.748(9) . ? S3D C8D 1.752(9) . ? S4D C6D 1.774(9) . ? S4D C9D 1.781(8) . ? C1D C2D 1.511(12) . ? C1D H1D1 0.98 . ? C1D H1D2 0.98 . ? C1D H1D3 0.98 . ? C2D C3D 1.334(13) . ? C3D C4D 1.498(12) . ? C4D H4D1 0.98 . ? C4D H4D2 0.98 . ? C4D H4D3 0.98 . ? C5D C6D 1.345(11) . ? C7D C8D 1.504(12) . ? C7D H7D1 0.98 . ? C7D H7D2 0.98 . ? C7D H7D3 0.98 . ? C8D C9D 1.336(11) . ? C9D C10D 1.397(12) . ? C10D C11D 1.218(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11B Pt1 C11A 92.2(2) . . ? C11B Pt1 N1 173.0(2) . . ? C11A Pt1 N1 94.8(2) . . ? C11B Pt1 N11 94.9(2) . . ? C11A Pt1 N11 172.9(2) . . ? N1 Pt1 N11 78.13(19) . . ? C112 N1 C116 118.4(5) . . ? C112 N1 Pt1 125.0(4) . . ? C116 N1 Pt1 116.5(4) . . ? C117 N11 C121 118.3(5) . . ? C117 N11 Pt1 116.6(4) . . ? C121 N11 Pt1 125.2(4) . . ? N1 C112 C113 121.5(6) . . ? N1 C112 H112 119.3 . . ? C113 C112 H112 119.3 . . ? C114 C113 C112 120.4(6) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C113 C114 C115 117.6(6) . . ? C113 C114 C122 120.9(6) . . ? C115 C114 C122 121.5(6) . . ? C114 C115 C116 120.8(6) . . ? C114 C115 H115 119.6 . . ? C116 C115 H115 119.6 . . ? N1 C116 C115 121.2(6) . . ? N1 C116 C117 114.1(5) . . ? C115 C116 C117 124.7(6) . . ? N11 C117 C118 121.5(5) . . ? N11 C117 C116 114.6(5) . . ? C118 C117 C116 123.9(5) . . ? C117 C118 C119 122.3(5) . . ? C117 C118 H118 118.8 . . ? C119 C118 H118 118.8 . . ? C118 C119 C120 115.6(5) . . ? C118 C119 C126 124.7(5) . . ? C120 C119 C126 119.6(5) . . ? C121 C120 C119 120.0(6) . . ? C121 C120 H120 120 . . ? C119 C120 H120 120 . . ? N11 C121 C120 122.2(6) . . ? N11 C121 H121 118.9 . . ? C120 C121 H121 118.9 . . ? C125 C122 C114 113.6(5) . . ? C125 C122 C124 108.2(5) . . ? C114 C122 C124 109.1(5) . . ? C125 C122 C123 108.3(5) . . ? C114 C122 C123 107.8(5) . . ? C124 C122 C123 109.8(5) . . ? C122 C123 H12A 109.5 . . ? C122 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? C122 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? C122 C124 H12D 109.5 . . ? C122 C124 H12E 109.5 . . ? H12D C124 H12E 109.5 . . ? C122 C124 H12F 109.5 . . ? H12D C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C122 C125 H12G 109.5 . . ? C122 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C122 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C129 C126 C119 109.6(5) . . ? C129 C126 C128 109.0(5) . . ? C119 C126 C128 109.2(5) . . ? C129 C126 C127 108.8(5) . . ? C119 C126 C127 111.1(5) . . ? C128 C126 C127 109.0(5) . . ? C126 C127 H12J 109.5 . . ? C126 C127 H12K 109.5 . . ? H12J C127 H12K 109.5 . . ? C126 C127 H12L 109.5 . . ? H12J C127 H12L 109.5 . . ? H12K C127 H12L 109.5 . . ? C126 C128 H12M 109.5 . . ? C126 C128 H12N 109.5 . . ? H12M C128 H12N 109.5 . . ? C126 C128 H12O 109.5 . . ? H12M C128 H12O 109.5 . . ? H12N C128 H12O 109.5 . . ? C126 C129 H12P 109.5 . . ? C126 C129 H12Q 109.5 . . ? H12P C129 H12Q 109.5 . . ? C126 C129 H12R 109.5 . . ? H12P C129 H12R 109.5 . . ? H12Q C129 H12R 109.5 . . ? C5A S1A C2A 96.2(3) . . ? C3A S2A C5A 96.2(3) . . ? C8A S3A C6A 96.6(3) . . ? C6A S4A C9A 96.4(3) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C3A C2A C1A 126.5(6) . . ? C3A C2A S1A 118.1(5) . . ? C1A C2A S1A 115.4(5) . . ? C2A C3A C4A 127.7(7) . . ? C2A C3A S2A 115.7(5) . . ? C4A C3A S2A 116.7(6) . . ? C3A C4A H4A1 109.5 . . ? C3A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C3A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C6A C5A S1A 124.8(5) . . ? C6A C5A S2A 121.6(5) . . ? S1A C5A S2A 113.7(3) . . ? C5A C6A S4A 123.8(5) . . ? C5A C6A S3A 123.0(5) . . ? S4A C6A S3A 113.2(3) . . ? C8A C7A H7A1 109.5 . . ? C8A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C8A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C9A C8A C7A 125.3(6) . . ? C9A C8A S3A 117.8(5) . . ? C7A C8A S3A 116.9(5) . . ? C8A C9A C10A 128.4(6) . . ? C8A C9A S4A 116.0(5) . . ? C10A C9A S4A 115.7(5) . . ? C11A C10A C9A 177.4(7) . . ? C10A C11A Pt1 175.0(6) . . ? C5B S1B C2B 95.7(3) . . ? C3B S2B C5B 95.0(3) . . ? C8B S3B C6B 96.3(3) . . ? C9B S4B C6B 95.9(3) . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C3B C2B C1B 129.1(6) . . ? C3B C2B S1B 116.3(5) . . ? C1B C2B S1B 114.6(5) . . ? C2B C3B C4B 127.1(6) . . ? C2B C3B S2B 119.0(6) . . ? C4B C3B S2B 113.8(5) . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C6B C5B S1B 124.1(5) . . ? C6B C5B S2B 121.9(5) . . ? S1B C5B S2B 114.0(3) . . ? C5B C6B S3B 124.1(5) . . ? C5B C6B S4B 122.9(5) . . ? S3B C6B S4B 112.9(3) . . ? C8B C7B H7B1 109.5 . . ? C8B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C8B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C9B C8B C7B 126.3(6) . . ? C9B C8B S3B 117.8(5) . . ? C7B C8B S3B 115.8(5) . . ? C8B C9B C10B 126.8(5) . . ? C8B C9B S4B 116.9(5) . . ? C10B C9B S4B 116.1(5) . . ? C11B C10B C9B 178.1(7) . . ? C10B C11B Pt1 175.8(5) . . ? C11C Pt2 C11D 91.0(3) . . ? C11C Pt2 N2 94.5(3) . . ? C11D Pt2 N2 174.5(3) . . ? C11C Pt2 N22 174.5(3) . . ? C11D Pt2 N22 94.5(3) . . ? N2 Pt2 N22 80.1(3) . . ? C212 N2 C216 116.8(7) . . ? C212 N2 Pt2 128.2(6) . . ? C216 N2 Pt2 115.1(5) . . ? C221 N22 C217 116.8(7) . . ? C221 N22 Pt2 127.5(6) . . ? C217 N22 Pt2 115.7(5) . . ? N2 C212 C213 122.7(9) . . ? N2 C212 H212 118.6 . . ? C213 C212 H212 118.6 . . ? C214 C213 C212 122.1(8) . . ? C214 C213 H213 119 . . ? C212 C213 H213 119 . . ? C213 C214 C215 118.0(8) . . ? C213 C214 C222 121.9(8) . . ? C215 C214 C222 120.1(8) . . ? C216 C215 C214 120.1(8) . . ? C216 C215 H215 120 . . ? C214 C215 H215 120 . . ? C215 C216 C217 126.5(8) . . ? C215 C216 N2 120.4(8) . . ? C217 C216 N2 113.1(7) . . ? C218 C217 N22 120.0(7) . . ? C218 C217 C216 124.0(8) . . ? N22 C217 C216 116.1(7) . . ? C217 C218 C219 121.7(8) . . ? C217 C218 H218 119.2 . . ? C219 C218 H218 119.2 . . ? C220 C219 C218 115.7(8) . . ? C220 C219 C226 122.3(8) . . ? C218 C219 C226 122.0(7) . . ? C221 C220 C219 123.5(8) . . ? C221 C220 H220 118.3 . . ? C219 C220 H220 118.3 . . ? C220 C221 N22 122.4(8) . . ? C220 C221 H221 118.8 . . ? N22 C221 H221 118.8 . . ? C224 C222 C223 109.7(5) . . ? C224 C222 C223 109.7(5) . 8_565 ? C223 C222 C223 111.3(7) . 8_565 ? C224 C222 C214 112.6(7) . . ? C223 C222 C214 106.7(5) . . ? C223 C222 C214 106.7(5) 8_565 . ? C222 C223 H22A 109.5 . . ? C222 C223 H22B 109.5 . . ? H22A C223 H22B 109.5 . . ? C222 C223 H22C 109.5 . . ? H22A C223 H22C 109.5 . . ? H22B C223 H22C 109.5 . . ? C222 C224 H22D 108.9(6) . . ? C222 C224 H22E 109.9 . . ? H22D C224 H22E 111.1(6) . . ? C222 C224 H22F 108.9(6) . . ? H22D C224 H22F 106.8(10) . . ? H22E C224 H22F 111.1(6) . . ? C227 C226 C227 108.4(8) 8_565 . ? C227 C226 C228 109.6(5) 8_565 . ? C227 C226 C228 109.6(5) . . ? C227 C226 C219 107.9(5) 8_565 . ? C227 C226 C219 107.9(5) . . ? C228 C226 C219 113.4(7) . . ? C226 C227 H22G 109.5 . . ? C226 C227 H22H 109.5 . . ? H22G C227 H22H 109.5 . . ? C226 C227 H22I 109.5 . . ? H22G C227 H22I 109.5 . . ? H22H C227 H22I 109.5 . . ? C226 C228 H22J 109.5 . . ? C226 C228 H22K 109.5 . . ? H22J C228 H22K 109.5 . . ? C226 C228 H22L 109.5 . . ? H22J C228 H22L 109.5 . . ? H22K C228 H22L 109.5 . . ? C5C S1C C2C 94.6(5) . . ? C5C S2C C3C 96.2(4) . . ? C6C S3C C8C 96.8(4) . . ? C6C S4C C9C 95.3(4) . . ? C2C C1C H1C1 109.5 . . ? C2C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? C2C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? C3C C2C C1C 126.8(10) . . ? C3C C2C S1C 118.6(8) . . ? C1C C2C S1C 114.5(8) . . ? C2C C3C C4C 129.5(10) . . ? C2C C3C S2C 115.9(8) . . ? C4C C3C S2C 114.5(8) . . ? C3C C4C H4C1 109.5 . . ? C3C C4C H4C2 109.5 . . ? H4C1 C4C H4C2 109.5 . . ? C3C C4C H4C3 109.5 . . ? H4C1 C4C H4C3 109.5 . . ? H4C2 C4C H4C3 109.5 . . ? C6C C5C S2C 124.5(7) . . ? C6C C5C S1C 120.8(7) . . ? S2C C5C S1C 114.6(5) . . ? C5C C6C S3C 125.5(7) . . ? C5C C6C S4C 120.4(7) . . ? S3C C6C S4C 114.1(5) . . ? C8C C7C H7C1 109.5 . . ? C8C C7C H7C2 109.5 . . ? H7C1 C7C H7C2 109.5 . . ? C8C C7C H7C3 109.5 . . ? H7C1 C7C H7C3 109.5 . . ? H7C2 C7C H7C3 109.5 . . ? C9C C8C C7C 126.1(8) . . ? C9C C8C S3C 116.5(7) . . ? C7C C8C S3C 117.4(7) . . ? C8C C9C C10C 125.4(8) . . ? C8C C9C S4C 117.3(7) . . ? C10C C9C S4C 117.2(7) . . ? C11C C10C C9C 174.4(9) . . ? C10C C11C Pt2 172.6(7) . . ? C5D S1D C2D 95.6(4) . . ? C3D S2D C5D 95.1(4) . . ? C6D S3D C8D 95.5(4) . . ? C6D S4D C9D 96.4(4) . . ? C2D C1D H1D1 109.5 . . ? C2D C1D H1D2 109.5 . . ? H1D1 C1D H1D2 109.5 . . ? C2D C1D H1D3 109.5 . . ? H1D1 C1D H1D3 109.5 . . ? H1D2 C1D H1D3 109.5 . . ? C3D C2D C1D 126.9(9) . . ? C3D C2D S1D 116.0(7) . . ? C1D C2D S1D 117.1(7) . . ? C2D C3D C4D 125.6(9) . . ? C2D C3D S2D 118.4(8) . . ? C4D C3D S2D 116.0(7) . . ? C3D C4D H4D1 109.5 . . ? C3D C4D H4D2 109.5 . . ? H4D1 C4D H4D2 109.5 . . ? C3D C4D H4D3 109.5 . . ? H4D1 C4D H4D3 109.5 . . ? H4D2 C4D H4D3 109.5 . . ? C6D C5D S1D 124.6(7) . . ? C6D C5D S2D 120.4(7) . . ? S1D C5D S2D 115.0(5) . . ? C5D C6D S3D 124.0(7) . . ? C5D C6D S4D 122.3(7) . . ? S3D C6D S4D 113.7(5) . . ? C8D C7D H7D1 109.5 . . ? C8D C7D H7D2 109.5 . . ? H7D1 C7D H7D2 109.5 . . ? C8D C7D H7D3 109.5 . . ? H7D1 C7D H7D3 109.5 . . ? H7D2 C7D H7D3 109.5 . . ? C9D C8D C7D 124.4(8) . . ? C9D C8D S3D 119.8(7) . . ? C7D C8D S3D 115.8(7) . . ? C8D C9D C10D 128.5(8) . . ? C8D C9D S4D 114.6(7) . . ? C10D C9D S4D 117.0(6) . . ? C11D C10D C9D 177.0(9) . . ? C10D C11D Pt2 172.4(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11A Pt1 N1 C112 -0.9(5) . . . . ? N11 Pt1 N1 C112 179.2(5) . . . . ? C11A Pt1 N1 C116 178.6(4) . . . . ? N11 Pt1 N1 C116 -1.4(4) . . . . ? C11B Pt1 N11 C117 -179.9(4) . . . . ? N1 Pt1 N11 C117 0.2(4) . . . . ? C11B Pt1 N11 C121 0.8(5) . . . . ? N1 Pt1 N11 C121 -179.0(5) . . . . ? C116 N1 C112 C113 -2.3(8) . . . . ? Pt1 N1 C112 C113 177.2(4) . . . . ? N1 C112 C113 C114 0.3(9) . . . . ? C112 C113 C114 C115 1.5(9) . . . . ? C112 C113 C114 C122 -179.5(5) . . . . ? C113 C114 C115 C116 -1.3(9) . . . . ? C122 C114 C115 C116 179.7(6) . . . . ? C112 N1 C116 C115 2.5(8) . . . . ? Pt1 N1 C116 C115 -177.0(4) . . . . ? C112 N1 C116 C117 -178.3(5) . . . . ? Pt1 N1 C116 C117 2.2(7) . . . . ? C114 C115 C116 N1 -0.7(9) . . . . ? C114 C115 C116 C117 -179.9(6) . . . . ? C121 N11 C117 C118 0.8(8) . . . . ? Pt1 N11 C117 C118 -178.4(4) . . . . ? C121 N11 C117 C116 -179.8(5) . . . . ? Pt1 N11 C117 C116 0.9(6) . . . . ? N1 C116 C117 N11 -2.0(8) . . . . ? C115 C116 C117 N11 177.2(5) . . . . ? N1 C116 C117 C118 177.2(5) . . . . ? C115 C116 C117 C118 -3.5(10) . . . . ? N11 C117 C118 C119 1.1(9) . . . . ? C116 C117 C118 C119 -178.1(6) . . . . ? C117 C118 C119 C120 -2.0(9) . . . . ? C117 C118 C119 C126 179.5(6) . . . . ? C118 C119 C120 C121 1.0(9) . . . . ? C126 C119 C120 C121 179.5(6) . . . . ? C117 N11 C121 C120 -1.9(9) . . . . ? Pt1 N11 C121 C120 177.3(5) . . . . ? C119 C120 C121 N11 0.9(10) . . . . ? C113 C114 C122 C125 179.7(6) . . . . ? C115 C114 C122 C125 -1.4(9) . . . . ? C113 C114 C122 C124 -59.5(8) . . . . ? C115 C114 C122 C124 119.5(6) . . . . ? C113 C114 C122 C123 59.7(8) . . . . ? C115 C114 C122 C123 -121.4(6) . . . . ? C118 C119 C126 C129 118.7(6) . . . . ? C120 C119 C126 C129 -59.7(7) . . . . ? C118 C119 C126 C128 -122.0(6) . . . . ? C120 C119 C126 C128 59.6(7) . . . . ? C118 C119 C126 C127 -1.6(8) . . . . ? C120 C119 C126 C127 179.9(6) . . . . ? C5A S1A C2A C3A -2.6(6) . . . . ? C5A S1A C2A C1A 176.5(5) . . . . ? C1A C2A C3A C4A 2.8(12) . . . . ? S1A C2A C3A C4A -178.2(6) . . . . ? C1A C2A C3A S2A -177.6(6) . . . . ? S1A C2A C3A S2A 1.4(8) . . . . ? C5A S2A C3A C2A 0.5(6) . . . . ? C5A S2A C3A C4A -179.8(5) . . . . ? C2A S1A C5A C6A -177.6(6) . . . . ? C2A S1A C5A S2A 2.8(4) . . . . ? C3A S2A C5A C6A 178.1(6) . . . . ? C3A S2A C5A S1A -2.3(4) . . . . ? S1A C5A C6A S4A -178.8(4) . . . . ? S2A C5A C6A S4A 0.7(9) . . . . ? S1A C5A C6A S3A 2.2(9) . . . . ? S2A C5A C6A S3A -178.2(4) . . . . ? C9A S4A C6A C5A -179.8(6) . . . . ? C9A S4A C6A S3A -0.7(4) . . . . ? C8A S3A C6A C5A -179.6(6) . . . . ? C8A S3A C6A S4A 1.3(4) . . . . ? C6A S3A C8A C9A -1.6(6) . . . . ? C6A S3A C8A C7A 179.7(5) . . . . ? C7A C8A C9A C10A -1.2(11) . . . . ? S3A C8A C9A C10A -179.8(5) . . . . ? C7A C8A C9A S4A 179.9(5) . . . . ? S3A C8A C9A S4A 1.3(7) . . . . ? C6A S4A C9A C8A -0.3(6) . . . . ? C6A S4A C9A C10A -179.3(5) . . . . ? C5B S1B C2B C3B 1.3(6) . . . . ? C5B S1B C2B C1B 179.6(5) . . . . ? C1B C2B C3B C4B 2.6(12) . . . . ? S1B C2B C3B C4B -179.3(5) . . . . ? C1B C2B C3B S2B 179.9(5) . . . . ? S1B C2B C3B S2B -2.0(8) . . . . ? C5B S2B C3B C2B 1.6(6) . . . . ? C5B S2B C3B C4B 179.3(5) . . . . ? C2B S1B C5B C6B 178.0(6) . . . . ? C2B S1B C5B S2B -0.2(4) . . . . ? C3B S2B C5B C6B -178.9(6) . . . . ? C3B S2B C5B S1B -0.6(4) . . . . ? S1B C5B C6B S3B 3.7(8) . . . . ? S2B C5B C6B S3B -178.3(3) . . . . ? S1B C5B C6B S4B -179.3(3) . . . . ? S2B C5B C6B S4B -1.3(8) . . . . ? C8B S3B C6B C5B -179.9(6) . . . . ? C8B S3B C6B S4B 2.8(4) . . . . ? C9B S4B C6B C5B -180.0(6) . . . . ? C9B S4B C6B S3B -2.6(4) . . . . ? C6B S3B C8B C9B -2.1(6) . . . . ? C6B S3B C8B C7B 179.5(5) . . . . ? C7B C8B C9B C10B 1.9(11) . . . . ? S3B C8B C9B C10B -176.3(5) . . . . ? C7B C8B C9B S4B 178.7(5) . . . . ? S3B C8B C9B S4B 0.5(7) . . . . ? C6B S4B C9B C8B 1.3(5) . . . . ? C6B S4B C9B C10B 178.5(5) . . . . ? N22 Pt2 N2 C216 0.000(2) . . . . ? C11D Pt2 N22 C221 0.000(2) . . . . ? N2 Pt2 N22 C221 180.000(2) . . . . ? C11D Pt2 N22 C217 180.000(2) . . . . ? N2 Pt2 N22 C217 0.000(2) . . . . ? C216 N2 C212 C213 0.000(3) . . . . ? Pt2 N2 C212 C213 180.000(2) . . . . ? N2 C212 C213 C214 0.000(3) . . . . ? C212 C213 C214 C215 0.000(3) . . . . ? C212 C213 C214 C222 180.000(3) . . . . ? C213 C214 C215 C216 0.000(3) . . . . ? C222 C214 C215 C216 180.000(3) . . . . ? C214 C215 C216 C217 180.000(3) . . . . ? C214 C215 C216 N2 0.000(3) . . . . ? C212 N2 C216 C215 0.000(3) . . . . ? Pt2 N2 C216 C215 180.000(2) . . . . ? C212 N2 C216 C217 180.000(2) . . . . ? Pt2 N2 C216 C217 0.000(2) . . . . ? C221 N22 C217 C218 0.000(3) . . . . ? Pt2 N22 C217 C218 180.000(2) . . . . ? C221 N22 C217 C216 180.000(2) . . . . ? Pt2 N22 C217 C216 0.000(2) . . . . ? C215 C216 C217 C218 0.000(3) . . . . ? N2 C216 C217 C218 180.000(2) . . . . ? C215 C216 C217 N22 180.000(2) . . . . ? N2 C216 C217 N22 0.000(2) . . . . ? N22 C217 C218 C219 0.000(3) . . . . ? C216 C217 C218 C219 180.000(3) . . . . ? C217 C218 C219 C220 0.000(3) . . . . ? C217 C218 C219 C226 180.000(2) . . . . ? C218 C219 C220 C221 0.000(3) . . . . ? C226 C219 C220 C221 180.000(3) . . . . ? C219 C220 C221 N22 0.000(3) . . . . ? C217 N22 C221 C220 0.000(3) . . . . ? Pt2 N22 C221 C220 180.000(2) . . . . ? C213 C214 C222 C224 180.000(3) . . . . ? C215 C214 C222 C224 0.000(3) . . . . ? C213 C214 C222 C223 59.6(5) . . . . ? C215 C214 C222 C223 -120.4(5) . . . . ? C213 C214 C222 C223 -59.6(5) . . . 8_565 ? C215 C214 C222 C223 120.4(5) . . . 8_565 ? C220 C219 C226 C227 58.5(5) . . . 8_565 ? C218 C219 C226 C227 -121.5(5) . . . 8_565 ? C220 C219 C226 C227 -58.5(5) . . . . ? C218 C219 C226 C227 121.5(5) . . . . ? C220 C219 C226 C228 180.000(3) . . . . ? C218 C219 C226 C228 0.000(3) . . . . ? C5C S1C C2C C3C 0.0000(10) . . . . ? C5C S1C C2C C1C 180 . . . . ? C1C C2C C3C C4C 0.000(2) . . . . ? S1C C2C C3C C4C 180.0000(10) . . . . ? C1C C2C C3C S2C 180 . . . . ? S1C C2C C3C S2C 0.0000(10) . . . . ? C5C S2C C3C C2C 0 . . . . ? C5C S2C C3C C4C 180 . . . . ? C3C S2C C5C C6C 180.0000(10) . . . . ? C3C S2C C5C S1C 0 . . . . ? C2C S1C C5C C6C 180.0000(10) . . . . ? C2C S1C C5C S2C 0 . . . . ? S2C C5C C6C S3C 180 . . . . ? S1C C5C C6C S3C 0.0000(10) . . . . ? S2C C5C C6C S4C 0.0000(10) . . . . ? S1C C5C C6C S4C 180 . . . . ? C8C S3C C6C S4C 0 . . . . ? C9C S4C C6C C5C 180.0000(10) . . . . ? C9C S4C C6C S3C 0 . . . . ? C6C S3C C8C C9C 0.0000(10) . . . . ? C6C S3C C8C C7C 180.000(2) . . . . ? C7C C8C C9C C10C 0.000(3) . . . . ? S3C C8C C9C C10C 180.000(2) . . . . ? C7C C8C C9C S4C 180.0000(10) . . . . ? S3C C8C C9C S4C 0.000(2) . . . . ? C6C S4C C9C C8C 0.0000(10) . . . . ? C6C S4C C9C C10C 180.0000(10) . . . . ? C5D S1D C2D C3D 0 . . . . ? C5D S1D C2D C1D 180 . . . . ? C1D C2D C3D C4D 0.0000(10) . . . . ? S1D C2D C3D C4D 180 . . . . ? C1D C2D C3D S2D 180 . . . . ? S1D C2D C3D S2D 0 . . . . ? C5D S2D C3D C2D 0 . . . . ? C5D S2D C3D C4D 180 . . . . ? C2D S1D C5D C6D 180.0000(10) . . . . ? C2D S1D C5D S2D 0 . . . . ? C3D S2D C5D C6D 180.0000(10) . . . . ? C3D S2D C5D S1D 0 . . . . ? S1D C5D C6D S3D 0.0000(10) . . . . ? S2D C5D C6D S3D 180 . . . . ? S1D C5D C6D S4D 180 . . . . ? S2D C5D C6D S4D 0.0000(10) . . . . ? C8D S3D C6D S4D 0 . . . . ? C9D S4D C6D C5D 180.0000(10) . . . . ? C9D S4D C6D S3D 0 . . . . ? C6D S3D C8D C9D 0.0000(10) . . . . ? C6D S3D C8D C7D 180.000(2) . . . . ? C7D C8D C9D C10D 0.000(2) . . . . ? S3D C8D C9D C10D 180.000(2) . . . . ? C7D C8D C9D S4D 180.0000(10) . . . . ? S3D C8D C9D S4D 0.000(2) . . . . ? C6D S4D C9D C8D 0.0000(10) . . . . ? C6D S4D C9D C10D 180.0000(10) . . . . ? data_complex4 _database_code_depnum_ccdc_archive 'CCDC 816627' #TrackingRef 'CIFFileDLorcy.cif' _audit_creation_date 2011-07-08T08:26:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C58 H48 P2 Pt S8, 2(C2 H3 N)' _chemical_formula_sum 'C62 H54 N2 P2 Pt S8' _chemical_formula_weight 1340.58 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2106(9) _cell_length_b 11.4614(9) _cell_length_c 15.8523(13) _cell_angle_alpha 103.405(4) _cell_angle_beta 102.101(4) _cell_angle_gamma 105.756(5) _cell_volume 1498.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9840 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.4 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.922 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_number 22108 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 6734 _reflns_number_gt 6454 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # 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^)+(0.0375P)^2^+0.6183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6734 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.057 _refine_diff_density_min -0.71 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # 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' 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' N N 0.0061 0.0033 '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 P1 P 0.00216(9) -0.19698(7) 0.01000(5) 0.01795(16) Uani 1 1 d . . . Pt1 Pt 0 0 0 0.01805(6) Uani 1 2 d S . . C21 C -0.0834(4) -0.2606(3) 0.0914(2) 0.0211(6) Uani 1 1 d . . . C23 C -0.0155(4) -0.1943(3) 0.1833(2) 0.0291(7) Uani 1 1 d . . . H23 H 0.072 -0.1176 0.2026 0.035 Uiso 1 1 calc R . . C24 C -0.0767(5) -0.2412(4) 0.2466(3) 0.0353(8) Uani 1 1 d . . . H24 H -0.0297 -0.1964 0.3094 0.042 Uiso 1 1 calc R . . C25 C -0.2045(5) -0.3517(4) 0.2197(3) 0.0374(9) Uani 1 1 d . . . H25 H -0.2459 -0.382 0.2636 0.045 Uiso 1 1 calc R . . C26 C -0.2724(4) -0.4182(4) 0.1283(3) 0.0363(9) Uani 1 1 d . . . H26 H -0.3599 -0.4948 0.1092 0.044 Uiso 1 1 calc R . . C27 C -0.2108(4) -0.3716(3) 0.0644(2) 0.0281(7) Uani 1 1 d . . . H27 H -0.2572 -0.417 0.0017 0.034 Uiso 1 1 calc R . . C28 C 0.2035(4) -0.1997(3) 0.0419(2) 0.0204(6) Uani 1 1 d . . . C29 C 0.2350(4) -0.3048(3) 0.0611(2) 0.0249(7) Uani 1 1 d . . . H29 H 0.1507 -0.3781 0.0558 0.03 Uiso 1 1 calc R . . C30 C 0.3906(4) -0.3020(3) 0.0880(2) 0.0283(7) Uani 1 1 d . . . H30 H 0.4117 -0.3739 0.1005 0.034 Uiso 1 1 calc R . . C31 C 0.5133(4) -0.1960(3) 0.0965(2) 0.0284(7) Uani 1 1 d . . . H31 H 0.6188 -0.195 0.1144 0.034 Uiso 1 1 calc R . . C32 C 0.4836(4) -0.0902(3) 0.0790(2) 0.0284(7) Uani 1 1 d . . . H32 H 0.5686 -0.0166 0.0855 0.034 Uiso 1 1 calc R . . C33 C 0.3290(4) -0.0924(3) 0.0519(2) 0.0259(7) Uani 1 1 d . . . H33 H 0.3088 -0.0198 0.04 0.031 Uiso 1 1 calc R . . C34 C -0.1081(4) -0.3199(3) -0.0981(2) 0.0220(6) Uani 1 1 d . . . C35 C -0.0600(4) -0.4199(3) -0.1362(2) 0.0272(7) Uani 1 1 d . . . H35 H 0.0382 -0.4249 -0.1068 0.033 Uiso 1 1 calc R . . C36 C -0.1555(5) -0.5125(3) -0.2171(2) 0.0360(9) Uani 1 1 d . . . H36 H -0.122 -0.5802 -0.2433 0.043 Uiso 1 1 calc R . . C37 C -0.2992(5) -0.5062(4) -0.2595(3) 0.0411(9) Uani 1 1 d . . . H37 H -0.3653 -0.5706 -0.314 0.049 Uiso 1 1 calc R . . C38 C -0.3473(5) -0.4065(4) -0.2229(3) 0.0449(10) Uani 1 1 d . . . H38 H -0.4456 -0.4022 -0.2528 0.054 Uiso 1 1 calc R . . C39 C -0.2522(4) -0.3129(4) -0.1425(2) 0.0350(8) Uani 1 1 d . . . H39 H -0.285 -0.2441 -0.1178 0.042 Uiso 1 1 calc R . . S1 S -0.32174(13) 0.19621(11) 0.55796(7) 0.0441(2) Uani 1 1 d . . . S2 S -0.20315(13) -0.01796(12) 0.51611(7) 0.0458(3) Uani 1 1 d . . . S3 S -0.26703(14) 0.25958(10) 0.37373(7) 0.0432(2) Uani 1 1 d . . . S4 S -0.13109(13) 0.05306(10) 0.33842(6) 0.0392(2) Uani 1 1 d . . . C1 C -0.4295(6) 0.1220(5) 0.6938(3) 0.0516(11) Uani 1 1 d . . . H1A H -0.4521 0.0529 0.7209 0.077 Uiso 1 1 calc R . . H1B H -0.5283 0.1338 0.6666 0.077 Uiso 1 1 calc R . . H1C H -0.3592 0.201 0.7408 0.077 Uiso 1 1 calc R . . C2 C -0.3507(5) 0.0886(4) 0.6214(2) 0.0419(10) Uani 1 1 d . . . C3 C -0.2980(5) -0.0081(4) 0.6024(3) 0.0421(10) Uani 1 1 d . . . C4 C -0.3062(6) -0.1130(5) 0.6464(3) 0.0540(12) Uani 1 1 d . . . H4A H -0.3525 -0.0969 0.6964 0.081 Uiso 1 1 calc R . . H4B H -0.1997 -0.1145 0.6699 0.081 Uiso 1 1 calc R . . H4C H -0.3717 -0.1952 0.6015 0.081 Uiso 1 1 calc R . . C5 C -0.2447(5) 0.1085(4) 0.4832(2) 0.0390(9) Uani 1 1 d . . . C6 C -0.2176(5) 0.1368(4) 0.4094(2) 0.0380(9) Uani 1 1 d . . . C7 C -0.2740(6) 0.2876(4) 0.2041(3) 0.0466(11) Uani 1 1 d . . . H7A H -0.2457 0.2582 0.1487 0.07 Uiso 1 1 calc R . . H7B H -0.2166 0.379 0.2329 0.07 Uiso 1 1 calc R . . H7C H -0.3877 0.2724 0.1889 0.07 Uiso 1 1 calc R . . C8 C -0.2314(4) 0.2163(3) 0.2681(2) 0.0307(8) Uani 1 1 d . . . C9 C -0.1668(4) 0.1241(3) 0.2522(2) 0.0260(7) Uani 1 1 d . . . C10 C -0.1195(4) 0.0809(3) 0.1742(2) 0.0227(7) Uani 1 1 d . . . C11 C -0.0744(4) 0.0442(3) 0.1091(2) 0.0204(6) Uani 1 1 d . . . C101 C 0.8224(10) 0.5887(7) 0.5616(4) 0.109(3) Uani 1 1 d . . . H10A H 0.8391 0.507 0.5579 0.163 Uiso 1 1 calc R . . H10B H 0.7714 0.6084 0.6089 0.163 Uiso 1 1 calc R . . H10C H 0.9242 0.656 0.5764 0.163 Uiso 1 1 calc R . . C102 C 0.7274(9) 0.5812(6) 0.4794(4) 0.096(2) Uani 1 1 d . . . N103 N 0.6545(13) 0.5740(9) 0.4118(6) 0.218(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0188(4) 0.0157(4) 0.0226(4) 0.0074(3) 0.0078(3) 0.0081(3) Pt1 0.02045(9) 0.01682(9) 0.02156(10) 0.00796(6) 0.00876(6) 0.00976(7) C21 0.0238(16) 0.0177(15) 0.0317(17) 0.0127(13) 0.0144(13) 0.0132(13) C23 0.0327(18) 0.0265(17) 0.0331(19) 0.0130(14) 0.0104(15) 0.0136(16) C24 0.047(2) 0.041(2) 0.034(2) 0.0205(17) 0.0204(17) 0.0236(19) C25 0.052(2) 0.039(2) 0.050(2) 0.0317(19) 0.035(2) 0.030(2) C26 0.034(2) 0.0270(19) 0.062(3) 0.0233(18) 0.0287(19) 0.0139(17) C27 0.0286(17) 0.0226(16) 0.041(2) 0.0137(14) 0.0148(15) 0.0131(15) C28 0.0219(15) 0.0238(16) 0.0203(15) 0.0081(12) 0.0096(12) 0.0116(13) C29 0.0244(16) 0.0205(16) 0.0297(17) 0.0073(13) 0.0065(13) 0.0089(14) C30 0.0314(18) 0.0252(17) 0.0309(18) 0.0074(14) 0.0056(14) 0.0175(15) C31 0.0243(17) 0.0353(19) 0.0279(18) 0.0087(15) 0.0061(14) 0.0157(16) C32 0.0228(16) 0.0311(18) 0.0343(19) 0.0157(15) 0.0105(14) 0.0071(15) C33 0.0253(17) 0.0266(17) 0.0305(18) 0.0139(14) 0.0086(14) 0.0111(15) C34 0.0222(15) 0.0181(15) 0.0256(16) 0.0067(12) 0.0075(13) 0.0062(13) C35 0.0275(17) 0.0244(17) 0.0325(18) 0.0093(14) 0.0093(14) 0.0121(15) C36 0.045(2) 0.0259(18) 0.035(2) 0.0008(15) 0.0119(17) 0.0166(18) C37 0.041(2) 0.035(2) 0.035(2) -0.0038(16) 0.0037(17) 0.0100(18) C38 0.034(2) 0.041(2) 0.046(2) -0.0010(18) -0.0038(17) 0.0163(19) C39 0.0314(19) 0.033(2) 0.038(2) 0.0004(16) 0.0049(16) 0.0189(17) S1 0.0541(6) 0.0482(6) 0.0308(5) 0.0044(4) 0.0223(5) 0.0178(5) S2 0.0527(6) 0.0668(7) 0.0343(5) 0.0232(5) 0.0219(5) 0.0320(6) S3 0.0616(7) 0.0420(6) 0.0426(6) 0.0129(4) 0.0333(5) 0.0294(5) S4 0.0556(6) 0.0543(6) 0.0309(5) 0.0220(4) 0.0255(4) 0.0373(5) C1 0.056(3) 0.059(3) 0.031(2) 0.003(2) 0.0215(19) 0.008(2) C2 0.038(2) 0.055(3) 0.0242(19) 0.0065(17) 0.0123(16) 0.005(2) C3 0.035(2) 0.058(3) 0.030(2) 0.0131(18) 0.0117(16) 0.009(2) C4 0.053(3) 0.068(3) 0.046(3) 0.025(2) 0.020(2) 0.016(2) C5 0.043(2) 0.047(2) 0.0286(19) 0.0077(17) 0.0162(17) 0.017(2) C6 0.048(2) 0.043(2) 0.031(2) 0.0099(17) 0.0211(17) 0.021(2) C7 0.065(3) 0.050(3) 0.056(3) 0.031(2) 0.037(2) 0.040(2) C8 0.0367(19) 0.0292(18) 0.0344(19) 0.0121(15) 0.0189(16) 0.0153(16) C9 0.0272(17) 0.0303(18) 0.0258(17) 0.0109(14) 0.0123(14) 0.0123(15) C10 0.0201(15) 0.0238(16) 0.0279(17) 0.0123(13) 0.0078(13) 0.0090(14) C11 0.0235(15) 0.0184(15) 0.0258(16) 0.0133(12) 0.0092(13) 0.0101(13) C101 0.137(7) 0.092(5) 0.069(4) 0.008(4) -0.007(4) 0.037(5) C102 0.113(6) 0.074(4) 0.068(4) -0.003(3) -0.018(4) 0.034(4) N103 0.247(12) 0.161(8) 0.150(7) -0.013(6) -0.098(7) 0.089(8) #----------------------------------------------------------------------------# # 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 P1 C34 1.824(3) . ? P1 C28 1.828(3) . ? P1 C21 1.835(3) . ? P1 Pt1 2.3047(8) . ? Pt1 C11 2.000(3) . ? Pt1 C11 2.000(3) 2 ? Pt1 P1 2.3047(8) 2 ? C21 C27 1.380(5) . ? C21 C23 1.392(5) . ? C23 C24 1.392(5) . ? C23 H23 0.95 . ? C24 C25 1.378(6) . ? C24 H24 0.95 . ? C25 C26 1.386(6) . ? C25 H25 0.95 . ? C26 C27 1.400(5) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 C33 1.391(4) . ? C28 C29 1.397(4) . ? C29 C30 1.396(5) . ? C29 H29 0.95 . ? C30 C31 1.374(5) . ? C30 H30 0.95 . ? C31 C32 1.388(5) . ? C31 H31 0.95 . ? C32 C33 1.390(5) . ? C32 H32 0.95 . ? C33 H33 0.95 . ? C34 C35 1.394(4) . ? C34 C39 1.399(5) . ? C35 C36 1.391(5) . ? C35 H35 0.95 . ? C36 C37 1.382(5) . ? C36 H36 0.95 . ? C37 C38 1.383(5) . ? C37 H37 0.95 . ? C38 C39 1.389(5) . ? C38 H38 0.95 . ? C39 H39 0.95 . ? S1 C5 1.762(4) . ? S1 C2 1.764(4) . ? S2 C5 1.757(4) . ? S2 C3 1.769(4) . ? S3 C8 1.759(4) . ? S3 C6 1.765(4) . ? S4 C9 1.765(3) . ? S4 C6 1.765(4) . ? C1 C2 1.512(6) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.324(6) . ? C3 C4 1.516(6) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C6 1.338(5) . ? C7 C8 1.497(5) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C9 1.347(5) . ? C9 C10 1.422(5) . ? C10 C11 1.219(4) . ? C101 C102 1.378(8) . ? C101 H10A 0.98 . ? C101 H10B 0.98 . ? C101 H10C 0.98 . ? C102 N103 1.111(9) . ? 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 C34 P1 C28 108.87(14) . . ? C34 P1 C21 103.16(15) . . ? C28 P1 C21 102.94(14) . . ? C34 P1 Pt1 110.45(10) . . ? C28 P1 Pt1 111.24(10) . . ? C21 P1 Pt1 119.44(10) . . ? C11 Pt1 C11 180 . 2 ? C11 Pt1 P1 95.01(8) . . ? C11 Pt1 P1 84.99(8) 2 . ? C11 Pt1 P1 84.99(8) . 2 ? C11 Pt1 P1 95.01(8) 2 2 ? P1 Pt1 P1 180 . 2 ? C27 C21 C23 119.5(3) . . ? C27 C21 P1 122.3(3) . . ? C23 C21 P1 118.2(2) . . ? C21 C23 C24 119.5(3) . . ? C21 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 121.0(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C27 119.4(4) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C21 C27 C26 120.9(3) . . ? C21 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C33 C28 C29 119.0(3) . . ? C33 C28 P1 119.4(2) . . ? C29 C28 P1 121.5(2) . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H29 120 . . ? C28 C29 H29 120 . . ? C31 C30 C29 120.4(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.2(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 119.8(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C28 C33 C32 120.7(3) . . ? C28 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C34 C39 119.4(3) . . ? C35 C34 P1 124.2(2) . . ? C39 C34 P1 116.3(2) . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.0(3) . . ? C37 C36 H36 120 . . ? C35 C36 H36 120 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C39 120.2(4) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C34 120.0(3) . . ? C38 C39 H39 120 . . ? C34 C39 H39 120 . . ? C5 S1 C2 95.5(2) . . ? C5 S2 C3 95.4(2) . . ? C8 S3 C6 95.07(17) . . ? C9 S4 C6 95.37(17) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 128.0(4) . . ? C3 C2 S1 117.3(3) . . ? C1 C2 S1 114.7(3) . . ? C2 C3 C4 128.1(4) . . ? C2 C3 S2 117.3(3) . . ? C4 C3 S2 114.6(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 S2 123.2(3) . . ? C6 C5 S1 123.3(3) . . ? S2 C5 S1 113.5(2) . . ? C5 C6 S4 122.8(3) . . ? C5 C6 S3 123.2(3) . . ? S4 C6 S3 114.1(2) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C7 125.9(3) . . ? C9 C8 S3 117.7(3) . . ? C7 C8 S3 116.4(3) . . ? C8 C9 C10 126.7(3) . . ? C8 C9 S4 116.8(3) . . ? C10 C9 S4 116.5(2) . . ? C11 C10 C9 177.9(3) . . ? C10 C11 Pt1 174.4(3) . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N103 C102 C101 177.5(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C34 P1 Pt1 C11 128.18(14) . . . . ? C28 P1 Pt1 C11 -110.80(14) . . . . ? C21 P1 Pt1 C11 8.88(15) . . . . ? C34 P1 Pt1 C11 -51.82(14) . . . 2 ? C28 P1 Pt1 C11 69.20(14) . . . 2 ? C21 P1 Pt1 C11 -171.13(15) . . . 2 ? C34 P1 C21 C27 -5.0(3) . . . . ? C28 P1 C21 C27 -118.2(3) . . . . ? Pt1 P1 C21 C27 118.0(2) . . . . ? C34 P1 C21 C23 174.4(2) . . . . ? C28 P1 C21 C23 61.2(3) . . . . ? Pt1 P1 C21 C23 -62.6(3) . . . . ? C27 C21 C23 C24 0.2(5) . . . . ? P1 C21 C23 C24 -179.2(3) . . . . ? C21 C23 C24 C25 -0.6(5) . . . . ? C23 C24 C25 C26 0.8(5) . . . . ? C24 C25 C26 C27 -0.5(5) . . . . ? C23 C21 C27 C26 0.0(5) . . . . ? P1 C21 C27 C26 179.4(2) . . . . ? C25 C26 C27 C21 0.1(5) . . . . ? C34 P1 C28 C33 118.7(3) . . . . ? C21 P1 C28 C33 -132.3(3) . . . . ? Pt1 P1 C28 C33 -3.2(3) . . . . ? C34 P1 C28 C29 -64.7(3) . . . . ? C21 P1 C28 C29 44.3(3) . . . . ? Pt1 P1 C28 C29 173.4(2) . . . . ? C33 C28 C29 C30 -1.3(5) . . . . ? P1 C28 C29 C30 -177.9(2) . . . . ? C28 C29 C30 C31 0.5(5) . . . . ? C29 C30 C31 C32 0.5(5) . . . . ? C30 C31 C32 C33 -0.7(5) . . . . ? C29 C28 C33 C32 1.2(5) . . . . ? P1 C28 C33 C32 177.8(3) . . . . ? C31 C32 C33 C28 -0.2(5) . . . . ? C28 P1 C34 C35 16.1(3) . . . . ? C21 P1 C34 C35 -92.8(3) . . . . ? Pt1 P1 C34 C35 138.5(3) . . . . ? C28 P1 C34 C39 -166.1(3) . . . . ? C21 P1 C34 C39 85.1(3) . . . . ? Pt1 P1 C34 C39 -43.7(3) . . . . ? C39 C34 C35 C36 -0.7(5) . . . . ? P1 C34 C35 C36 177.1(3) . . . . ? C34 C35 C36 C37 -0.7(6) . . . . ? C35 C36 C37 C38 1.4(6) . . . . ? C36 C37 C38 C39 -0.8(7) . . . . ? C37 C38 C39 C34 -0.6(7) . . . . ? C35 C34 C39 C38 1.3(6) . . . . ? P1 C34 C39 C38 -176.7(3) . . . . ? C5 S1 C2 C3 5.9(4) . . . . ? C5 S1 C2 C1 -176.0(3) . . . . ? C1 C2 C3 C4 1.7(7) . . . . ? S1 C2 C3 C4 179.6(3) . . . . ? C1 C2 C3 S2 -177.4(3) . . . . ? S1 C2 C3 S2 0.4(5) . . . . ? C5 S2 C3 C2 -6.5(4) . . . . ? C5 S2 C3 C4 174.3(3) . . . . ? C3 S2 C5 C6 -171.0(4) . . . . ? C3 S2 C5 S1 10.1(3) . . . . ? C2 S1 C5 C6 171.2(4) . . . . ? C2 S1 C5 S2 -10.0(3) . . . . ? S2 C5 C6 S4 -2.0(6) . . . . ? S1 C5 C6 S4 176.7(2) . . . . ? S2 C5 C6 S3 177.2(2) . . . . ? S1 C5 C6 S3 -4.1(6) . . . . ? C9 S4 C6 C5 170.5(4) . . . . ? C9 S4 C6 S3 -8.8(3) . . . . ? C8 S3 C6 C5 -169.7(4) . . . . ? C8 S3 C6 S4 9.6(3) . . . . ? C6 S3 C8 C9 -7.1(3) . . . . ? C6 S3 C8 C7 173.8(3) . . . . ? C7 C8 C9 C10 3.3(6) . . . . ? S3 C8 C9 C10 -175.7(3) . . . . ? C7 C8 C9 S4 -178.9(3) . . . . ? S3 C8 C9 S4 2.1(4) . . . . ? C6 S4 C9 C8 4.1(3) . . . . ? C6 S4 C9 C10 -177.9(3) . . . . ? #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 816628' #TrackingRef 'CIFFileDLorcy.cif' _audit_creation_date 2012-05-15T17:01:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C48 H42 P2 Pt S8)' _chemical_formula_sum 'C96 H84 P4 Pt2 S16' _chemical_formula_weight 2264.65 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 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' _cell_length_a 12.5211(4) _cell_length_b 23.7040(8) _cell_length_c 33.0267(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9802.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9702 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.45 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.307 _exptl_absorpt_correction_T_max 0.848 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # 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 -0.122 0.015 0.558 145 27 ' ' 2 0.122 0.515 0.942 145 27 ' ' 3 0.137 0.792 0.753 23 3 ' ' 4 0.378 0.485 0.442 145 27 ' ' 5 0.363 0.208 0.253 23 3 ' ' 6 0.622 -0.015 0.058 145 27 ' ' 7 0.637 0.708 0.247 23 3 ' ' 8 0.862 0.292 0.747 23 3 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_unetI/netI 0.0922 _diffrn_reflns_number 48559 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 20527 _reflns_number_gt 16284 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # 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^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 20527 _refine_ls_number_parameters 775 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.02 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.057(4) _refine_diff_density_max 1.489 _refine_diff_density_min -1.752 _refine_diff_density_rms 0.131 _iucr_refine_instructions_details ; .res file for SHELXL : sqz_ren2.res ................................................................. TITL import in P 21 21 21 CELL 0.71073 12.5211 23.7040 33.0267 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0008 0.0011 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H P S PT UNIT 384 336 16 64 8 MERG 2 EADP C1a c2a c3a c4a EADP c1b c2b c3b c4b EADP C133 c153 EADP c233 c253 EADP C221 > c226 EADP c227 > c232 FLAT c221 > c226 FLAT c227 > c232 EADP C241 > c246 FLAT c241 > c246 EADP C247 > c252 FLAT C247 > c252 EADP C121 > c126 FLAT c121 > c126 EADP C127 > c132 FLAT C127 > c132 EADP C141 > c146 FLAT c141 > c146 EADP C147 > c152 FLAT C147 > c152 EADP C11a c11b EADP c11c c11d FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.032400 FVAR 1.28274 MOLE 1 PT1 5 0.539631 0.801815 0.058310 11.00000 0.02447 0.02104 = 0.02060 0.00075 -0.00150 0.00238 P1 3 0.661315 0.761638 0.015294 11.00000 0.02724 0.02241 = 0.02030 0.00147 -0.00165 0.00068 P11 3 0.612203 0.743243 0.106374 11.00000 0.02366 0.02385 = 0.02194 0.00150 0.00044 0.00167 C121 1 0.749085 0.808730 -0.010367 11.00000 0.06547 0.04988 = 0.04111 0.00428 0.01274 -0.01451 C122 1 0.797497 0.851740 0.012685 11.00000 0.06547 0.04988 = 0.04111 0.00428 0.01274 -0.01451 AFIX 43 H122 2 0.778654 0.856087 0.040373 11.00000 -1.20000 AFIX 0 C123 1 0.871601 0.887543 -0.004241 11.00000 0.06547 0.04988 = 0.04111 0.00428 0.01274 -0.01451 AFIX 43 H123 2 0.905765 0.915199 0.012057 11.00000 -1.20000 AFIX 0 C124 1 0.896800 0.883282 -0.045527 11.00000 0.06547 0.04988 = 0.04111 0.00428 0.01274 -0.01451 AFIX 43 H124 2 0.941515 0.910393 -0.058232 11.00000 -1.20000 AFIX 0 C125 1 0.855879 0.839688 -0.066707 11.00000 0.06547 0.04988 = 0.04111 0.00428 0.01274 -0.01451 AFIX 43 H125 2 0.876627 0.834427 -0.094116 11.00000 -1.20000 AFIX 0 C126 1 0.784452 0.802603 -0.049296 11.00000 0.06547 0.04988 = 0.04111 0.00428 0.01274 -0.01451 AFIX 43 H126 2 0.758949 0.771738 -0.064891 11.00000 -1.20000 AFIX 0 C127 1 0.609256 0.715378 -0.024519 11.00000 0.03696 0.04044 = 0.03510 -0.00860 -0.00487 0.00648 C128 1 0.534373 0.736875 -0.050528 11.00000 0.03696 0.04044 = 0.03510 -0.00860 -0.00487 0.00648 AFIX 43 H128 2 0.506624 0.773735 -0.046423 11.00000 -1.20000 AFIX 0 C129 1 0.499179 0.704389 -0.083010 11.00000 0.03696 0.04044 = 0.03510 -0.00860 -0.00487 0.00648 AFIX 43 H129 2 0.446792 0.719005 -0.100980 11.00000 -1.20000 AFIX 0 C130 1 0.540830 0.650102 -0.089306 11.00000 0.03696 0.04044 = 0.03510 -0.00860 -0.00487 0.00648 AFIX 43 H130 2 0.515908 0.627507 -0.111104 11.00000 -1.20000 AFIX 0 C131 1 0.616810 0.630450 -0.063947 11.00000 0.03696 0.04044 = 0.03510 -0.00860 -0.00487 0.00648 AFIX 43 H131 2 0.647043 0.594213 -0.068373 11.00000 -1.20000 AFIX 0 C132 1 0.650865 0.662788 -0.031562 11.00000 0.03696 0.04044 = 0.03510 -0.00860 -0.00487 0.00648 AFIX 43 H132 2 0.704048 0.648293 -0.013880 11.00000 -1.20000 AFIX 0 C133 1 0.750969 0.719160 0.046323 11.00000 0.02608 0.02740 = 0.02805 0.00313 0.00031 0.00363 AFIX 23 H13A 2 0.788652 0.691455 0.029029 11.00000 -1.20000 H13B 2 0.805142 0.743820 0.059108 11.00000 -1.20000 AFIX 0 C141 1 0.713732 0.777004 0.137041 11.00000 0.02712 0.05567 = 0.02972 -0.00846 0.00401 -0.00237 C142 1 0.775291 0.746570 0.164378 11.00000 0.02712 0.05567 = 0.02972 -0.00846 0.00401 -0.00237 AFIX 43 H142 2 0.762087 0.707469 0.168219 11.00000 -1.20000 AFIX 0 C143 1 0.856108 0.772980 0.186151 11.00000 0.02712 0.05567 = 0.02972 -0.00846 0.00401 -0.00237 AFIX 43 H143 2 0.898866 0.751623 0.204308 11.00000 -1.20000 AFIX 0 C144 1 0.874690 0.830216 0.181546 11.00000 0.02712 0.05567 = 0.02972 -0.00846 0.00401 -0.00237 AFIX 43 H144 2 0.930004 0.847979 0.196550 11.00000 -1.20000 AFIX 0 C145 1 0.814437 0.860731 0.155822 11.00000 0.02712 0.05567 = 0.02972 -0.00846 0.00401 -0.00237 AFIX 43 H145 2 0.827893 0.899969 0.152948 11.00000 -1.20000 AFIX 0 C146 1 0.731408 0.835543 0.132957 11.00000 0.02712 0.05567 = 0.02972 -0.00846 0.00401 -0.00237 AFIX 43 H146 2 0.688552 0.857578 0.115257 11.00000 -1.20000 AFIX 0 C147 1 0.532481 0.704537 0.142720 11.00000 0.03243 0.03445 = 0.03570 0.00652 0.00119 -0.00613 C148 1 0.549720 0.648714 0.151413 11.00000 0.03243 0.03445 = 0.03570 0.00652 0.00119 -0.00613 AFIX 43 H148 2 0.604002 0.628397 0.137584 11.00000 -1.20000 AFIX 0 C149 1 0.487618 0.621941 0.180489 11.00000 0.03243 0.03445 = 0.03570 0.00652 0.00119 -0.00613 AFIX 43 H149 2 0.500057 0.583259 0.186350 11.00000 -1.20000 AFIX 0 C150 1 0.410488 0.649603 0.200440 11.00000 0.03243 0.03445 = 0.03570 0.00652 0.00119 -0.00613 AFIX 43 H150 2 0.369928 0.630835 0.220677 11.00000 -1.20000 AFIX 0 C151 1 0.390607 0.704396 0.191641 11.00000 0.03243 0.03445 = 0.03570 0.00652 0.00119 -0.00613 AFIX 43 H151 2 0.334827 0.723963 0.205167 11.00000 -1.20000 AFIX 0 C152 1 0.451815 0.731684 0.162911 11.00000 0.03243 0.03445 = 0.03570 0.00652 0.00119 -0.00613 AFIX 43 H152 2 0.437691 0.770189 0.156995 11.00000 -1.20000 AFIX 0 C153 1 0.688333 0.688304 0.078928 11.00000 0.02608 0.02740 = 0.02805 0.00313 0.00031 0.00363 AFIX 23 H15A 2 0.737345 0.668329 0.097576 11.00000 -1.20000 H15B 2 0.639239 0.660411 0.066627 11.00000 -1.20000 AFIX 0 S4A 4 0.429814 0.902093 -0.092646 11.00000 0.02609 0.03393 = 0.02989 0.00628 0.00074 0.00979 S3A 4 0.259950 0.985736 -0.078357 11.00000 0.05010 0.03944 = 0.02902 0.00646 0.00013 0.02214 S2A 4 0.373282 0.903348 -0.189370 11.00000 0.03079 0.03664 = 0.03248 0.00064 0.00181 0.01067 S1A 4 0.206541 0.988172 -0.174723 11.00000 0.03685 0.03753 = 0.02685 0.00103 -0.00191 0.01727 C1A 1 0.134166 0.981873 -0.253977 11.00000 0.03929 0.05580 = 0.03134 -0.00029 0.00156 0.00685 AFIX 137 H1A1 2 0.144328 0.963411 -0.280245 11.00000 -1.50000 H1A2 2 0.147226 1.022451 -0.256769 11.00000 -1.50000 H1A3 2 0.060813 0.975667 -0.244636 11.00000 -1.50000 AFIX 0 C2A 1 0.211418 0.957359 -0.223589 11.00000 0.03929 0.05580 = 0.03134 -0.00029 0.00156 0.00685 C3A 1 0.285922 0.919500 -0.230443 11.00000 0.03929 0.05580 = 0.03134 -0.00029 0.00156 0.00685 C4A 1 0.305476 0.887113 -0.268369 11.00000 0.03929 0.05580 = 0.03134 -0.00029 0.00156 0.00685 AFIX 137 H4A1 2 0.317651 0.847335 -0.261729 11.00000 -1.50000 H4A2 2 0.368486 0.902348 -0.282162 11.00000 -1.50000 H4A3 2 0.243156 0.890346 -0.286170 11.00000 -1.50000 AFIX 0 C5A 1 0.303325 0.944055 -0.152977 11.00000 0.02394 0.02449 = 0.03499 0.00513 -0.00322 0.01080 C6A 1 0.327080 0.944078 -0.113603 11.00000 0.03067 0.02824 = 0.02256 0.00482 -0.00393 0.00757 C7A 1 0.270021 0.971176 0.005080 11.00000 0.06645 0.04065 = 0.03545 0.00562 0.01492 0.00799 AFIX 137 H7A1 2 0.308237 0.951286 0.026685 11.00000 -1.50000 H7A2 2 0.193733 0.962191 0.006630 11.00000 -1.50000 H7A3 2 0.280035 1.011936 0.008278 11.00000 -1.50000 AFIX 0 C8A 1 0.313827 0.952618 -0.036068 11.00000 0.03670 0.02048 = 0.02683 -0.00156 0.00363 0.00814 C9A 1 0.391207 0.914082 -0.041551 11.00000 0.03109 0.03012 = 0.01857 -0.00271 -0.00053 -0.00013 C10A 1 0.442614 0.881348 -0.010895 11.00000 0.02854 0.02406 = 0.02785 0.00181 0.00012 -0.00415 C11A 1 0.484394 0.851603 0.014139 11.00000 0.04078 0.02434 = 0.02010 0.00065 -0.00619 -0.00283 S1B 4 0.060663 0.937747 0.268912 11.00000 0.07250 0.03523 = 0.04707 -0.01290 0.02601 -0.01283 S2B 4 0.144443 0.822170 0.269087 11.00000 0.04666 0.04193 = 0.05107 0.00354 -0.00432 -0.00803 S3B 4 0.156481 0.957795 0.178978 11.00000 0.04929 0.04030 = 0.03693 -0.00621 0.00558 0.01705 S4B 4 0.231318 0.841069 0.176310 11.00000 0.03931 0.03299 = 0.04752 -0.00495 0.00623 0.00764 C1B 1 0.027967 0.936610 0.351069 11.00000 0.09814 0.06898 = 0.04370 -0.00955 0.01024 -0.05273 AFIX 137 H1B1 2 -0.039967 0.919797 0.359527 11.00000 -1.50000 H1B2 2 0.016352 0.976056 0.343351 11.00000 -1.50000 H1B3 2 0.079008 0.934891 0.373530 11.00000 -1.50000 AFIX 0 C2B 1 0.071302 0.904818 0.315799 11.00000 0.09814 0.06898 = 0.04370 -0.00955 0.01024 -0.05273 C3B 1 0.107080 0.852920 0.316306 11.00000 0.09814 0.06898 = 0.04370 -0.00955 0.01024 -0.05273 C4B 1 0.119357 0.812686 0.352392 11.00000 0.09814 0.06898 = 0.04370 -0.00955 0.01024 -0.05273 AFIX 137 H4B1 2 0.194235 0.811902 0.361012 11.00000 -1.50000 H4B2 2 0.097082 0.774660 0.344374 11.00000 -1.50000 H4B3 2 0.074598 0.825796 0.374842 11.00000 -1.50000 AFIX 0 C5B 1 0.129729 0.885599 0.242288 11.00000 0.03630 0.03616 = 0.03902 -0.00406 -0.00632 -0.00620 C6B 1 0.168165 0.893926 0.205042 11.00000 0.03060 0.03731 = 0.04124 -0.00760 -0.00749 0.00506 C7B 1 0.297143 0.988301 0.118567 11.00000 0.07106 0.05060 = 0.04688 0.00602 0.01622 0.00719 AFIX 137 H7B1 2 0.352555 0.974039 0.100281 11.00000 -1.50000 H7B2 2 0.326795 1.018556 0.135377 11.00000 -1.50000 H7B3 2 0.237290 1.003024 0.102632 11.00000 -1.50000 AFIX 0 C8B 1 0.260331 0.943452 0.143988 11.00000 0.04590 0.04156 = 0.02660 -0.01006 -0.00298 0.02057 C9B 1 0.293682 0.889396 0.142776 11.00000 0.03558 0.04376 = 0.02887 -0.00986 0.00368 -0.00528 C10B 1 0.374295 0.865602 0.116680 11.00000 0.04428 0.03381 = 0.03005 0.00073 -0.00591 0.00130 C11B 1 0.436694 0.840199 0.096339 11.00000 0.04078 0.02434 = 0.02010 0.00065 -0.00619 -0.00283 MOLE 2 PT2 5 0.252609 0.184093 0.053990 11.00000 0.02625 0.03592 = 0.01923 0.00130 -0.00023 -0.01327 P2 3 0.380558 0.221418 0.012667 11.00000 0.03628 0.05227 = 0.02006 0.00118 0.00013 -0.02337 P22 3 0.336277 0.232659 0.105033 11.00000 0.03529 0.03906 = 0.02056 0.00212 -0.00600 -0.01799 C221 1 0.462586 0.172317 -0.015812 11.00000 0.04414 0.09761 = 0.06368 -0.00352 0.01788 -0.00467 C222 1 0.446601 0.115529 -0.013795 11.00000 0.04414 0.09761 = 0.06368 -0.00352 0.01788 -0.00467 AFIX 43 H222 2 0.389574 0.100521 0.001824 11.00000 -1.20000 AFIX 0 C223 1 0.514405 0.080111 -0.034758 11.00000 0.04414 0.09761 = 0.06368 -0.00352 0.01788 -0.00467 AFIX 43 H223 2 0.499963 0.040768 -0.034473 11.00000 -1.20000 AFIX 0 C224 1 0.598794 0.098280 -0.055298 11.00000 0.04414 0.09761 = 0.06368 -0.00352 0.01788 -0.00467 AFIX 43 H224 2 0.646887 0.072766 -0.067932 11.00000 -1.20000 AFIX 0 C225 1 0.613334 0.155152 -0.057445 11.00000 0.04414 0.09761 = 0.06368 -0.00352 0.01788 -0.00467 AFIX 43 H225 2 0.672105 0.169108 -0.072631 11.00000 -1.20000 AFIX 0 C226 1 0.547514 0.193104 -0.038823 11.00000 0.04414 0.09761 = 0.06368 -0.00352 0.01788 -0.00467 AFIX 43 H226 2 0.559185 0.232535 -0.041451 11.00000 -1.20000 AFIX 0 C227 1 0.333558 0.271415 -0.024368 11.00000 0.08840 0.05258 = 0.04119 0.00668 -0.02311 -0.01842 C228 1 0.275983 0.254427 -0.057057 11.00000 0.08840 0.05258 = 0.04119 0.00668 -0.02311 -0.01842 AFIX 43 H228 2 0.262107 0.215309 -0.060445 11.00000 -1.20000 AFIX 0 C229 1 0.236657 0.291897 -0.085675 11.00000 0.08840 0.05258 = 0.04119 0.00668 -0.02311 -0.01842 AFIX 43 H229 2 0.196796 0.277941 -0.108006 11.00000 -1.20000 AFIX 0 C230 1 0.253704 0.346373 -0.082362 11.00000 0.08840 0.05258 = 0.04119 0.00668 -0.02311 -0.01842 AFIX 43 H230 2 0.225329 0.372121 -0.101603 11.00000 -1.20000 AFIX 0 C231 1 0.314451 0.365194 -0.049888 11.00000 0.08840 0.05258 = 0.04119 0.00668 -0.02311 -0.01842 AFIX 43 H231 2 0.328817 0.404385 -0.047338 11.00000 -1.20000 AFIX 0 C232 1 0.354595 0.328449 -0.021167 11.00000 0.08840 0.05258 = 0.04119 0.00668 -0.02311 -0.01842 AFIX 43 H232 2 0.396432 0.342348 0.000657 11.00000 -1.20000 AFIX 0 C233 1 0.480251 0.257564 0.044526 11.00000 0.04851 0.06801 = 0.02925 0.01009 -0.01209 -0.03953 AFIX 23 H23A 2 0.533592 0.230132 0.054622 11.00000 -1.20000 H23B 2 0.518007 0.286737 0.028549 11.00000 -1.20000 AFIX 0 C241 1 0.429281 0.191601 0.135168 11.00000 0.05135 0.07212 = 0.04248 -0.00646 -0.01171 0.00512 C242 1 0.489502 0.216625 0.165345 11.00000 0.05135 0.07212 = 0.04248 -0.00646 -0.01171 0.00512 AFIX 43 H242 2 0.479075 0.255390 0.171484 11.00000 -1.20000 AFIX 0 C243 1 0.563904 0.186254 0.186468 11.00000 0.05135 0.07212 = 0.04248 -0.00646 -0.01171 0.00512 AFIX 43 H243 2 0.605298 0.204581 0.206670 11.00000 -1.20000 AFIX 0 C244 1 0.579791 0.130815 0.179236 11.00000 0.05135 0.07212 = 0.04248 -0.00646 -0.01171 0.00512 AFIX 43 H244 2 0.631769 0.110005 0.193933 11.00000 -1.20000 AFIX 0 C245 1 0.519020 0.105714 0.150243 11.00000 0.05135 0.07212 = 0.04248 -0.00646 -0.01171 0.00512 AFIX 43 H245 2 0.527463 0.066439 0.145494 11.00000 -1.20000 AFIX 0 C246 1 0.445565 0.135305 0.127501 11.00000 0.05135 0.07212 = 0.04248 -0.00646 -0.01171 0.00512 AFIX 43 H246 2 0.406514 0.116882 0.106683 11.00000 -1.20000 AFIX 0 C247 1 0.261894 0.270150 0.143688 11.00000 0.04353 0.03786 = 0.03207 -0.00364 -0.00404 -0.00485 C248 1 0.270843 0.327717 0.150286 11.00000 0.04353 0.03786 = 0.03207 -0.00364 -0.00404 -0.00485 AFIX 43 H248 2 0.317074 0.349390 0.133605 11.00000 -1.20000 AFIX 0 C249 1 0.212967 0.354571 0.181106 11.00000 0.04353 0.03786 = 0.03207 -0.00364 -0.00404 -0.00485 AFIX 43 H249 2 0.220280 0.394016 0.185376 11.00000 -1.20000 AFIX 0 C250 1 0.146202 0.323583 0.204850 11.00000 0.04353 0.03786 = 0.03207 -0.00364 -0.00404 -0.00485 AFIX 43 H250 2 0.106868 0.341421 0.225853 11.00000 -1.20000 AFIX 0 C251 1 0.135466 0.265998 0.198447 11.00000 0.04353 0.03786 = 0.03207 -0.00364 -0.00404 -0.00485 AFIX 43 H251 2 0.089348 0.244335 0.215179 11.00000 -1.20000 AFIX 0 C252 1 0.192566 0.240082 0.167394 11.00000 0.04353 0.03786 = 0.03207 -0.00364 -0.00404 -0.00485 AFIX 43 H252 2 0.183243 0.200877 0.162582 11.00000 -1.20000 AFIX 0 C253 1 0.421226 0.284963 0.080238 11.00000 0.04851 0.06801 = 0.02925 0.01009 -0.01209 -0.03953 AFIX 23 H25A 2 0.376949 0.316705 0.070351 11.00000 -1.20000 H25B 2 0.473629 0.300076 0.099890 11.00000 -1.20000 AFIX 0 S1C 4 -0.089537 0.038260 -0.192411 11.00000 0.03413 0.02805 = 0.02395 0.00220 -0.00602 -0.00260 S2C 4 0.069285 0.128526 -0.199798 11.00000 0.03419 0.03629 = 0.03168 0.00319 0.00159 -0.00693 S3C 4 -0.042038 0.029473 -0.095987 11.00000 0.04696 0.03195 = 0.02545 -0.00096 -0.00470 -0.01339 S4C 4 0.129301 0.114286 -0.104114 11.00000 0.02372 0.02476 = 0.02329 -0.00018 -0.00178 -0.00039 C1C 1 -0.172216 0.060341 -0.268427 11.00000 0.04045 0.07152 = 0.02694 0.01001 -0.00983 -0.01381 AFIX 137 H1C1 2 -0.244245 0.069438 -0.258827 11.00000 -1.50000 H1C2 2 -0.166655 0.019626 -0.273129 11.00000 -1.50000 H1C3 2 -0.158214 0.080549 -0.293763 11.00000 -1.50000 AFIX 0 C2C 1 -0.092098 0.077766 -0.237214 11.00000 0.03682 0.03562 = 0.02204 0.00688 -0.00177 0.00516 C3C 1 -0.019746 0.119377 -0.240182 11.00000 0.02686 0.04676 = 0.02211 0.00563 0.00183 0.00330 C4C 1 -0.007262 0.160313 -0.275200 11.00000 0.06024 0.06008 = 0.04828 0.02907 -0.01175 -0.01935 AFIX 137 H4C1 2 -0.040943 0.144465 -0.299450 11.00000 -1.50000 H4C2 2 0.068823 0.166700 -0.280436 11.00000 -1.50000 H4C3 2 -0.041606 0.196208 -0.268325 11.00000 -1.50000 AFIX 0 C5C 1 0.003407 0.080644 -0.167746 11.00000 0.02961 0.01823 = 0.02276 -0.00088 -0.00382 0.00895 C6C 1 0.027008 0.076396 -0.128203 11.00000 0.01938 0.01714 = 0.03192 -0.00597 -0.00125 -0.00047 C7C 1 -0.028500 0.032984 -0.011983 11.00000 0.06314 0.04230 = 0.02529 0.00345 -0.00674 -0.01701 AFIX 137 H7C1 2 -0.003536 -0.005962 -0.008889 11.00000 -1.50000 H7C2 2 -0.106758 0.033630 -0.011901 11.00000 -1.50000 H7C3 2 -0.001566 0.055899 0.010505 11.00000 -1.50000 AFIX 0 C8C 1 0.012315 0.056807 -0.051721 11.00000 0.03663 0.02191 = 0.02434 -0.00269 -0.00544 -0.00140 C9C 1 0.089889 0.095515 -0.054299 11.00000 0.02945 0.01801 = 0.02245 0.00019 -0.00263 0.00155 C10C 1 0.144542 0.121425 -0.021437 11.00000 0.02517 0.02455 = 0.02646 -0.00152 0.00389 0.00125 C11C 1 0.185967 0.143509 0.007490 11.00000 0.02499 0.03039 = 0.02247 -0.00087 0.00154 -0.00944 S1D 4 -0.180795 0.051648 0.276782 11.00000 0.03886 0.03409 = 0.03277 -0.00047 0.01115 -0.00683 S2D 4 -0.108303 0.169310 0.270172 11.00000 0.03532 0.03175 = 0.03551 0.00274 0.00446 -0.00144 S3D 4 -0.132661 0.036515 0.177578 11.00000 0.04069 0.04080 = 0.02957 -0.00054 0.00896 -0.01432 S4D 4 -0.054620 0.153314 0.175954 11.00000 0.03869 0.03687 = 0.03372 0.00780 0.00640 -0.00825 C1D 1 -0.201709 0.058505 0.359945 11.00000 0.04237 0.05594 = 0.02674 -0.00051 0.00459 -0.01424 AFIX 137 H1D1 2 -0.169949 0.076232 0.383895 11.00000 -1.50000 H1D2 2 -0.177599 0.019260 0.358059 11.00000 -1.50000 H1D3 2 -0.279730 0.059437 0.362206 11.00000 -1.50000 AFIX 0 C2D 1 -0.167274 0.090506 0.322129 11.00000 0.03133 0.04742 = 0.02885 -0.00286 0.00242 -0.00383 C3D 1 -0.135383 0.143797 0.319092 11.00000 0.02660 0.02920 = 0.03746 0.00193 0.00240 -0.00244 C4D 1 -0.119266 0.186248 0.352336 11.00000 0.03835 0.04136 = 0.04561 -0.00423 -0.00308 0.00960 AFIX 137 H4D1 2 -0.147149 0.171039 0.377823 11.00000 -1.50000 H4D2 2 -0.157266 0.221141 0.345571 11.00000 -1.50000 H4D3 2 -0.042873 0.194246 0.355292 11.00000 -1.50000 AFIX 0 C5D 1 -0.129576 0.105034 0.245069 11.00000 0.02864 0.03157 = 0.03778 0.00434 0.00656 -0.00421 C6D 1 -0.107405 0.098682 0.205783 11.00000 0.02804 0.03447 = 0.02848 0.00185 0.01019 -0.00516 C7D 1 -0.030510 0.009143 0.104876 11.00000 0.04880 0.05739 = 0.02952 0.00711 0.01008 -0.00285 AFIX 137 H7D1 2 -0.099805 -0.001480 0.093378 11.00000 -1.50000 H7D2 2 0.002892 -0.024029 0.117256 11.00000 -1.50000 H7D3 2 0.015775 0.023736 0.083361 11.00000 -1.50000 AFIX 0 C8D 1 -0.047040 0.055589 0.137689 11.00000 0.03147 0.05259 = 0.02115 -0.00082 0.00467 -0.00497 C9D 1 -0.007096 0.107430 0.137282 11.00000 0.03034 0.04445 = 0.02547 0.00658 0.00258 -0.01177 C10D 1 0.070047 0.129933 0.109178 11.00000 0.03886 0.04274 = 0.02458 0.00406 -0.00036 -0.00066 C11D 1 0.138947 0.151129 0.089795 11.00000 0.02499 0.03039 = 0.02247 -0.00087 0.00154 -0.00944 HKLF 4 REM import in P 21 21 21 REM R1 = 0.0433 for 16284 Fo > 4sig(Fo) and 0.0621 for all 20527 data REM 775 parameters refined using 24 restraints END WGHT 0.0339 0.0000 REM Highest difference peak 1.49, deepest hole -1.75, 1-sigma level 0.13 Q1 1 0.5398 0.8368 0.0582 11.00000 0.05 1.49 Q2 1 0.2542 0.2182 0.0206 11.00000 0.05 1.25 Q3 1 0.5406 0.7763 0.0265 11.00000 0.05 1.15 Q4 1 0.2414 0.1557 0.0863 11.00000 0.05 1.15 Q5 1 0.2568 0.2176 0.0881 11.00000 0.05 1.15 Q6 1 0.5521 0.7740 0.0913 11.00000 0.05 1.08 Q7 1 0.6429 0.8036 0.0569 11.00000 0.05 1.05 Q8 1 0.2540 0.1559 0.0209 11.00000 0.05 1.03 Q9 1 0.5426 0.8364 0.0935 11.00000 0.05 1.02 Q10 1 0.4579 0.8016 0.0585 11.00000 0.05 0.94 Q11 1 0.2769 0.1830 0.1087 11.00000 0.05 0.92 Q12 1 0.3404 0.1837 0.0552 11.00000 0.05 0.90 Q13 1 0.6672 0.9797 0.1097 11.00000 0.05 0.88 Q14 1 0.5391 0.8380 0.0236 11.00000 0.05 0.87 Q15 1 0.2679 0.1833 -0.0011 11.00000 0.05 0.83 Q16 1 0.2485 0.3630 -0.0438 11.00000 0.05 0.83 Q17 1 0.2422 0.1476 0.0513 11.00000 0.05 0.80 Q18 1 0.5049 0.8030 0.0057 11.00000 0.05 0.80 Q19 1 0.2806 0.1564 0.0503 11.00000 0.05 0.78 Q20 1 0.5776 0.8012 0.0048 11.00000 0.05 0.76 ; #----------------------------------------------------------------------------# # 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' 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' 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 0.53963(2) 0.801815(9) 0.058310(7) 0.02204(6) Uani 1 1 d . . . P1 P 0.66132(16) 0.76164(6) 0.01529(5) 0.0233(4) Uani 1 1 d . . . P11 P 0.61220(15) 0.74324(6) 0.10637(5) 0.0231(4) Uani 1 1 d . . . C121 C 0.7491(8) 0.8087(3) -0.0104(2) 0.0522(9) Uani 1 1 d D . . C122 C 0.7975(7) 0.8517(3) 0.0127(2) 0.0522(9) Uani 1 1 d D . . H122 H 0.7787 0.8561 0.0404 0.063 Uiso 1 1 calc R . . C123 C 0.8716(7) 0.8875(3) -0.0042(2) 0.0522(9) Uani 1 1 d D . . H123 H 0.9058 0.9152 0.0121 0.063 Uiso 1 1 calc R . . C124 C 0.8968(7) 0.8833(3) -0.0455(2) 0.0522(9) Uani 1 1 d D . . H124 H 0.9415 0.9104 -0.0582 0.063 Uiso 1 1 calc R . . C125 C 0.8559(7) 0.8397(3) -0.0667(2) 0.0522(9) Uani 1 1 d D . . H125 H 0.8766 0.8344 -0.0941 0.063 Uiso 1 1 calc R . . C126 C 0.7845(7) 0.8026(3) -0.0493(2) 0.0522(9) Uani 1 1 d D . . H126 H 0.7589 0.7717 -0.0649 0.063 Uiso 1 1 calc R . . C127 C 0.6093(6) 0.7154(3) -0.0245(2) 0.0375(7) Uani 1 1 d D . . C128 C 0.5344(6) 0.7369(3) -0.05053(18) 0.0375(7) Uani 1 1 d D . . H128 H 0.5066 0.7737 -0.0464 0.045 Uiso 1 1 calc R . . C129 C 0.4992(6) 0.7044(3) -0.08301(19) 0.0375(7) Uani 1 1 d D . . H129 H 0.4468 0.719 -0.101 0.045 Uiso 1 1 calc R . . C130 C 0.5408(7) 0.6501(3) -0.0893(2) 0.0375(7) Uani 1 1 d D . . H130 H 0.5159 0.6275 -0.1111 0.045 Uiso 1 1 calc R . . C131 C 0.6168(6) 0.6305(3) -0.06395(19) 0.0375(7) Uani 1 1 d D . . H131 H 0.647 0.5942 -0.0684 0.045 Uiso 1 1 calc R . . C132 C 0.6509(6) 0.6628(3) -0.0316(2) 0.0375(7) Uani 1 1 d D . . H132 H 0.704 0.6483 -0.0139 0.045 Uiso 1 1 calc R . . C133 C 0.7510(6) 0.7192(2) 0.04632(17) 0.0272(10) Uani 1 1 d . . . H13A H 0.7887 0.6915 0.029 0.033 Uiso 1 1 calc R . . H13B H 0.8051 0.7438 0.0591 0.033 Uiso 1 1 calc R . . C141 C 0.7137(6) 0.7770(3) 0.13704(19) 0.0375(7) Uani 1 1 d D . . C142 C 0.7753(6) 0.7466(3) 0.16438(18) 0.0375(7) Uani 1 1 d D . . H142 H 0.7621 0.7075 0.1682 0.045 Uiso 1 1 calc R . . C143 C 0.8561(6) 0.7730(3) 0.1862(2) 0.0375(7) Uani 1 1 d D . . H143 H 0.8989 0.7516 0.2043 0.045 Uiso 1 1 calc R . . C144 C 0.8747(6) 0.8302(3) 0.1815(2) 0.0375(7) Uani 1 1 d D . . H144 H 0.93 0.848 0.1966 0.045 Uiso 1 1 calc R . . C145 C 0.8144(6) 0.8607(3) 0.15582(19) 0.0375(7) Uani 1 1 d D . . H145 H 0.8279 0.9 0.1529 0.045 Uiso 1 1 calc R . . C146 C 0.7314(6) 0.8355(3) 0.13296(19) 0.0375(7) Uani 1 1 d D . . H146 H 0.6886 0.8576 0.1153 0.045 Uiso 1 1 calc R . . C147 C 0.5325(6) 0.7045(3) 0.14272(19) 0.0342(7) Uani 1 1 d D . . C148 C 0.5497(6) 0.6487(3) 0.15141(18) 0.0342(7) Uani 1 1 d D . . H148 H 0.604 0.6284 0.1376 0.041 Uiso 1 1 calc R . . C149 C 0.4876(6) 0.6219(3) 0.18049(19) 0.0342(7) Uani 1 1 d D . . H149 H 0.5001 0.5833 0.1864 0.041 Uiso 1 1 calc R . . C150 C 0.4105(6) 0.6496(3) 0.2004(2) 0.0342(7) Uani 1 1 d D . . H150 H 0.3699 0.6308 0.2207 0.041 Uiso 1 1 calc R . . C151 C 0.3906(6) 0.7044(3) 0.19164(19) 0.0342(7) Uani 1 1 d D . . H151 H 0.3348 0.724 0.2052 0.041 Uiso 1 1 calc R . . C152 C 0.4518(6) 0.7317(3) 0.16291(19) 0.0342(7) Uani 1 1 d D . . H152 H 0.4377 0.7702 0.157 0.041 Uiso 1 1 calc R . . C153 C 0.6883(6) 0.6883(2) 0.07893(17) 0.0272(10) Uani 1 1 d . . . H15A H 0.7373 0.6683 0.0976 0.033 Uiso 1 1 calc R . . H15B H 0.6392 0.6604 0.0666 0.033 Uiso 1 1 calc R . . S4A S 0.42981(15) 0.90209(7) -0.09265(5) 0.0300(4) Uani 1 1 d . . . S3A S 0.25995(19) 0.98574(7) -0.07836(5) 0.0395(5) Uani 1 1 d . . . S2A S 0.37328(16) 0.90335(7) -0.18937(5) 0.0333(4) Uani 1 1 d . . . S1A S 0.20654(16) 0.98817(7) -0.17472(5) 0.0337(4) Uani 1 1 d . . . C1A C 0.1342(6) 0.9819(3) -0.2540(2) 0.0421(10) Uani 1 1 d . . . H1A1 H 0.1443 0.9634 -0.2802 0.063 Uiso 1 1 calc R . . H1A2 H 0.1472 1.0225 -0.2568 0.063 Uiso 1 1 calc R . . H1A3 H 0.0608 0.9757 -0.2446 0.063 Uiso 1 1 calc R . . C2A C 0.2114(7) 0.9574(3) -0.2236(2) 0.0421(10) Uani 1 1 d . . . C3A C 0.2859(7) 0.9195(3) -0.2304(2) 0.0421(10) Uani 1 1 d . . . C4A C 0.3055(7) 0.8871(3) -0.26837(19) 0.0421(10) Uani 1 1 d . . . H4A1 H 0.3177 0.8473 -0.2617 0.063 Uiso 1 1 calc R . . H4A2 H 0.3685 0.9023 -0.2822 0.063 Uiso 1 1 calc R . . H4A3 H 0.2432 0.8903 -0.2862 0.063 Uiso 1 1 calc R . . C5A C 0.3033(6) 0.9441(2) -0.15298(19) 0.0278(16) Uani 1 1 d . . . C6A C 0.3271(6) 0.9441(2) -0.11360(17) 0.0272(15) Uani 1 1 d . . . C7A C 0.2700(8) 0.9712(3) 0.0051(2) 0.048(2) Uani 1 1 d . . . H7A1 H 0.3082 0.9513 0.0267 0.071 Uiso 1 1 calc R . . H7A2 H 0.1937 0.9622 0.0066 0.071 Uiso 1 1 calc R . . H7A3 H 0.28 1.0119 0.0083 0.071 Uiso 1 1 calc R . . C8A C 0.3138(6) 0.9526(2) -0.03607(18) 0.0280(16) Uani 1 1 d . . . C9A C 0.3912(6) 0.9141(2) -0.04155(17) 0.0266(15) Uani 1 1 d . . . C10A C 0.4426(6) 0.8813(2) -0.01090(18) 0.0268(16) Uani 1 1 d . . . C11A C 0.4844(6) 0.8516(2) 0.01414(17) 0.0284(12) Uani 1 1 d . . . S1B S 0.0607(2) 0.93775(7) 0.26891(6) 0.0516(6) Uani 1 1 d . . . S2B S 0.14444(19) 0.82217(8) 0.26909(6) 0.0466(5) Uani 1 1 d . . . S3B S 0.15648(19) 0.95779(7) 0.17898(6) 0.0422(5) Uani 1 1 d . . . S4B S 0.23132(17) 0.84107(7) 0.17631(6) 0.0399(5) Uani 1 1 d . . . C1B C 0.0280(9) 0.9366(3) 0.3511(2) 0.0703(16) Uani 1 1 d . . . H1B1 H -0.04 0.9198 0.3595 0.105 Uiso 1 1 calc R . . H1B2 H 0.0164 0.9761 0.3434 0.105 Uiso 1 1 calc R . . H1B3 H 0.079 0.9349 0.3735 0.105 Uiso 1 1 calc R . . C2B C 0.0713(9) 0.9048(4) 0.3158(2) 0.0703(16) Uani 1 1 d . . . C3B C 0.1071(9) 0.8529(4) 0.3163(2) 0.0703(16) Uani 1 1 d . . . C4B C 0.1194(9) 0.8127(3) 0.3524(2) 0.0703(16) Uani 1 1 d . . . H4B1 H 0.1942 0.8119 0.361 0.105 Uiso 1 1 calc R . . H4B2 H 0.0971 0.7747 0.3444 0.105 Uiso 1 1 calc R . . H4B3 H 0.0746 0.8258 0.3748 0.105 Uiso 1 1 calc R . . C5B C 0.1297(7) 0.8856(3) 0.2423(2) 0.0372(18) Uani 1 1 d . . . C6B C 0.1682(6) 0.8939(3) 0.2050(2) 0.0364(18) Uani 1 1 d . . . C7B C 0.2971(8) 0.9883(3) 0.1186(2) 0.056(3) Uani 1 1 d . . . H7B1 H 0.3526 0.974 0.1003 0.084 Uiso 1 1 calc R . . H7B2 H 0.3268 1.0186 0.1354 0.084 Uiso 1 1 calc R . . H7B3 H 0.2373 1.003 0.1026 0.084 Uiso 1 1 calc R . . C8B C 0.2603(7) 0.9435(3) 0.14399(18) 0.0380(19) Uani 1 1 d . . . C9B C 0.2937(6) 0.8894(3) 0.14278(19) 0.0361(18) Uani 1 1 d . . . C10B C 0.3743(7) 0.8656(3) 0.1167(2) 0.0360(18) Uani 1 1 d . . . C11B C 0.4367(6) 0.8402(2) 0.09634(18) 0.0284(12) Uani 1 1 d . . . Pt2 Pt 0.25261(2) 0.184093(9) 0.053990(7) 0.02714(7) Uani 1 1 d . . . P2 P 0.38056(17) 0.22142(8) 0.01267(5) 0.0362(5) Uani 1 1 d . . . P22 P 0.33628(17) 0.23266(7) 0.10503(5) 0.0316(4) Uani 1 1 d . . . C221 C 0.4626(8) 0.1723(4) -0.0158(3) 0.0685(11) Uani 1 1 d D . . C222 C 0.4466(8) 0.1155(4) -0.0138(2) 0.0685(11) Uani 1 1 d D . . H222 H 0.3896 0.1005 0.0018 0.082 Uiso 1 1 calc R . . C223 C 0.5144(7) 0.0801(4) -0.0348(2) 0.0685(11) Uani 1 1 d D . . H223 H 0.5 0.0408 -0.0345 0.082 Uiso 1 1 calc R . . C224 C 0.5988(7) 0.0983(4) -0.0553(3) 0.0685(11) Uani 1 1 d D . . H224 H 0.6469 0.0728 -0.0679 0.082 Uiso 1 1 calc R . . C225 C 0.6133(7) 0.1552(4) -0.0574(3) 0.0685(11) Uani 1 1 d D . . H225 H 0.6721 0.1691 -0.0726 0.082 Uiso 1 1 calc R . . C226 C 0.5475(7) 0.1931(4) -0.0388(2) 0.0685(11) Uani 1 1 d D . . H226 H 0.5592 0.2325 -0.0415 0.082 Uiso 1 1 calc R . . C227 C 0.3336(8) 0.2714(3) -0.0244(2) 0.0607(11) Uani 1 1 d D . . C228 C 0.2760(7) 0.2544(3) -0.0571(2) 0.0607(11) Uani 1 1 d D . . H228 H 0.2621 0.2153 -0.0604 0.073 Uiso 1 1 calc R . . C229 C 0.2367(8) 0.2919(3) -0.0857(2) 0.0607(11) Uani 1 1 d D . . H229 H 0.1968 0.2779 -0.108 0.073 Uiso 1 1 calc R . . C230 C 0.2537(9) 0.3464(3) -0.0824(2) 0.0607(11) Uani 1 1 d D . . H230 H 0.2253 0.3721 -0.1016 0.073 Uiso 1 1 calc R . . C231 C 0.3145(8) 0.3652(3) -0.0499(2) 0.0607(11) Uani 1 1 d D . . H231 H 0.3288 0.4044 -0.0473 0.073 Uiso 1 1 calc R . . C232 C 0.3546(8) 0.3284(3) -0.0212(2) 0.0607(11) Uani 1 1 d D . . H232 H 0.3964 0.3423 0.0007 0.073 Uiso 1 1 calc R . . C233 C 0.4803(7) 0.2576(3) 0.04453(19) 0.0486(16) Uani 1 1 d . . . H23A H 0.5336 0.2301 0.0546 0.058 Uiso 1 1 calc R . . H23B H 0.518 0.2867 0.0285 0.058 Uiso 1 1 calc R . . C241 C 0.4293(7) 0.1916(4) 0.1352(2) 0.0553(10) Uani 1 1 d D . . C242 C 0.4895(7) 0.2166(4) 0.1653(2) 0.0553(10) Uani 1 1 d D . . H242 H 0.4791 0.2554 0.1715 0.066 Uiso 1 1 calc R . . C243 C 0.5639(7) 0.1863(3) 0.1865(2) 0.0553(10) Uani 1 1 d D . . H243 H 0.6053 0.2046 0.2067 0.066 Uiso 1 1 calc R . . C244 C 0.5798(8) 0.1308(3) 0.1792(2) 0.0553(10) Uani 1 1 d D . . H244 H 0.6318 0.11 0.1939 0.066 Uiso 1 1 calc R . . C245 C 0.5190(7) 0.1057(4) 0.1502(2) 0.0553(10) Uani 1 1 d D . . H245 H 0.5275 0.0664 0.1455 0.066 Uiso 1 1 calc R . . C246 C 0.4456(8) 0.1353(3) 0.1275(2) 0.0553(10) Uani 1 1 d D . . H246 H 0.4065 0.1169 0.1067 0.066 Uiso 1 1 calc R . . C247 C 0.2619(7) 0.2701(3) 0.14369(19) 0.0378(7) Uani 1 1 d D . . C248 C 0.2708(6) 0.3277(3) 0.15029(19) 0.0378(7) Uani 1 1 d D . . H248 H 0.3171 0.3494 0.1336 0.045 Uiso 1 1 calc R . . C249 C 0.2130(6) 0.3546(3) 0.18111(19) 0.0378(7) Uani 1 1 d D . . H249 H 0.2203 0.394 0.1854 0.045 Uiso 1 1 calc R . . C250 C 0.1462(7) 0.3236(3) 0.20485(19) 0.0378(7) Uani 1 1 d D . . H250 H 0.1069 0.3414 0.2259 0.045 Uiso 1 1 calc R . . C251 C 0.1355(7) 0.2660(3) 0.19845(19) 0.0378(7) Uani 1 1 d D . . H251 H 0.0893 0.2443 0.2152 0.045 Uiso 1 1 calc R . . C252 C 0.1926(6) 0.2401(3) 0.16739(19) 0.0378(7) Uani 1 1 d D . . H252 H 0.1832 0.2009 0.1626 0.045 Uiso 1 1 calc R . . C253 C 0.4212(7) 0.2850(3) 0.0802(2) 0.0486(16) Uani 1 1 d . . . H25A H 0.3769 0.3167 0.0704 0.058 Uiso 1 1 calc R . . H25B H 0.4736 0.3001 0.0999 0.058 Uiso 1 1 calc R . . S1C S -0.08954(16) 0.03826(6) -0.19241(5) 0.0287(4) Uani 1 1 d . . . S2C S 0.06928(16) 0.12853(7) -0.19980(5) 0.0341(4) Uani 1 1 d . . . S3C S -0.04204(19) 0.02947(7) -0.09599(5) 0.0348(4) Uani 1 1 d . . . S4C S 0.12930(15) 0.11429(6) -0.10411(4) 0.0239(4) Uani 1 1 d . . . C1C C -0.1722(7) 0.0603(3) -0.26843(19) 0.046(2) Uani 1 1 d . . . H1C1 H -0.2442 0.0694 -0.2588 0.069 Uiso 1 1 calc R . . H1C2 H -0.1667 0.0196 -0.2731 0.069 Uiso 1 1 calc R . . H1C3 H -0.1582 0.0805 -0.2938 0.069 Uiso 1 1 calc R . . C2C C -0.0921(6) 0.0778(3) -0.23721(18) 0.0315(17) Uani 1 1 d . . . C3C C -0.0197(6) 0.1194(3) -0.24018(18) 0.0319(17) Uani 1 1 d . . . C4C C -0.0073(8) 0.1603(3) -0.2752(2) 0.056(2) Uani 1 1 d . . . H4C1 H -0.0409 0.1445 -0.2994 0.084 Uiso 1 1 calc R . . H4C2 H 0.0688 0.1667 -0.2804 0.084 Uiso 1 1 calc R . . H4C3 H -0.0416 0.1962 -0.2683 0.084 Uiso 1 1 calc R . . C5C C 0.0034(6) 0.0806(2) -0.16775(17) 0.0235(15) Uani 1 1 d . . . C6C C 0.0270(5) 0.0764(2) -0.12820(17) 0.0228(14) Uani 1 1 d . . . C7C C -0.0285(8) 0.0330(3) -0.01198(18) 0.044(2) Uani 1 1 d . . . H7C1 H -0.0035 -0.006 -0.0089 0.065 Uiso 1 1 calc R . . H7C2 H -0.1068 0.0336 -0.0119 0.065 Uiso 1 1 calc R . . H7C3 H -0.0016 0.0559 0.0105 0.065 Uiso 1 1 calc R . . C8C C 0.0123(6) 0.0568(2) -0.05172(18) 0.0276(15) Uani 1 1 d . . . C9C C 0.0899(5) 0.0955(2) -0.05430(18) 0.0233(14) Uani 1 1 d . . . C10C C 0.1445(6) 0.1214(2) -0.02144(18) 0.0254(15) Uani 1 1 d . . . C11C C 0.1860(6) 0.1435(2) 0.00749(18) 0.0259(11) Uani 1 1 d . . . S1D S -0.18079(17) 0.05165(7) 0.27678(5) 0.0352(5) Uani 1 1 d . . . S2D S -0.10830(16) 0.16931(7) 0.27017(5) 0.0342(4) Uani 1 1 d . . . S3D S -0.13266(17) 0.03652(7) 0.17758(5) 0.0370(5) Uani 1 1 d . . . S4D S -0.05462(17) 0.15331(7) 0.17595(5) 0.0364(5) Uani 1 1 d . . . C1D C -0.2017(7) 0.0585(3) 0.35994(19) 0.042(2) Uani 1 1 d . . . H1D1 H -0.1699 0.0762 0.3839 0.063 Uiso 1 1 calc R . . H1D2 H -0.1776 0.0193 0.3581 0.063 Uiso 1 1 calc R . . H1D3 H -0.2797 0.0594 0.3622 0.063 Uiso 1 1 calc R . . C2D C -0.1673(6) 0.0905(3) 0.32213(19) 0.0359(18) Uani 1 1 d . . . C3D C -0.1354(6) 0.1438(3) 0.3191(2) 0.0311(16) Uani 1 1 d . . . C4D C -0.1193(7) 0.1862(3) 0.3523(2) 0.0418(19) Uani 1 1 d . . . H4D1 H -0.1471 0.171 0.3778 0.063 Uiso 1 1 calc R . . H4D2 H -0.1573 0.2211 0.3456 0.063 Uiso 1 1 calc R . . H4D3 H -0.0429 0.1942 0.3553 0.063 Uiso 1 1 calc R . . C5D C -0.1296(6) 0.1050(3) 0.2451(2) 0.0327(17) Uani 1 1 d . . . C6D C -0.1074(6) 0.0987(3) 0.20578(19) 0.0303(16) Uani 1 1 d . . . C7D C -0.0305(8) 0.0091(3) 0.1049(2) 0.045(2) Uani 1 1 d . . . H7D1 H -0.0998 -0.0015 0.0934 0.068 Uiso 1 1 calc R . . H7D2 H 0.0029 -0.024 0.1173 0.068 Uiso 1 1 calc R . . H7D3 H 0.0158 0.0237 0.0834 0.068 Uiso 1 1 calc R . . C8D C -0.0470(7) 0.0556(3) 0.13769(18) 0.0351(17) Uani 1 1 d . . . C9D C -0.0071(6) 0.1074(3) 0.13728(19) 0.0334(18) Uani 1 1 d . . . C10D C 0.0700(7) 0.1299(3) 0.10918(19) 0.0354(18) Uani 1 1 d . . . C11D C 0.1389(6) 0.1511(3) 0.08980(18) 0.0259(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02447(13) 0.02104(10) 0.02060(10) 0.00075(9) -0.00150(13) 0.00238(11) P1 0.0272(10) 0.0224(7) 0.0203(8) 0.0015(6) -0.0016(9) 0.0007(8) P11 0.0237(10) 0.0239(8) 0.0219(8) 0.0015(6) 0.0004(8) 0.0017(8) C121 0.065(3) 0.0499(18) 0.0411(17) 0.0043(13) 0.013(2) -0.0145(19) C122 0.065(3) 0.0499(18) 0.0411(17) 0.0043(13) 0.013(2) -0.0145(19) C123 0.065(3) 0.0499(18) 0.0411(17) 0.0043(13) 0.013(2) -0.0145(19) C124 0.065(3) 0.0499(18) 0.0411(17) 0.0043(13) 0.013(2) -0.0145(19) C125 0.065(3) 0.0499(18) 0.0411(17) 0.0043(13) 0.013(2) -0.0145(19) C126 0.065(3) 0.0499(18) 0.0411(17) 0.0043(13) 0.013(2) -0.0145(19) C127 0.0370(19) 0.0404(16) 0.0351(15) -0.0086(12) -0.0049(16) 0.0065(16) C128 0.0370(19) 0.0404(16) 0.0351(15) -0.0086(12) -0.0049(16) 0.0065(16) C129 0.0370(19) 0.0404(16) 0.0351(15) -0.0086(12) -0.0049(16) 0.0065(16) C130 0.0370(19) 0.0404(16) 0.0351(15) -0.0086(12) -0.0049(16) 0.0065(16) C131 0.0370(19) 0.0404(16) 0.0351(15) -0.0086(12) -0.0049(16) 0.0065(16) C132 0.0370(19) 0.0404(16) 0.0351(15) -0.0086(12) -0.0049(16) 0.0065(16) C133 0.026(3) 0.027(2) 0.028(2) 0.0031(17) 0.000(2) 0.004(2) C141 0.0271(17) 0.0557(17) 0.0297(14) -0.0085(13) 0.0040(14) -0.0024(17) C142 0.0271(17) 0.0557(17) 0.0297(14) -0.0085(13) 0.0040(14) -0.0024(17) C143 0.0271(17) 0.0557(17) 0.0297(14) -0.0085(13) 0.0040(14) -0.0024(17) C144 0.0271(17) 0.0557(17) 0.0297(14) -0.0085(13) 0.0040(14) -0.0024(17) C145 0.0271(17) 0.0557(17) 0.0297(14) -0.0085(13) 0.0040(14) -0.0024(17) C146 0.0271(17) 0.0557(17) 0.0297(14) -0.0085(13) 0.0040(14) -0.0024(17) C147 0.0324(17) 0.0344(14) 0.0357(15) 0.0065(11) 0.0012(15) -0.0061(16) C148 0.0324(17) 0.0344(14) 0.0357(15) 0.0065(11) 0.0012(15) -0.0061(16) C149 0.0324(17) 0.0344(14) 0.0357(15) 0.0065(11) 0.0012(15) -0.0061(16) C150 0.0324(17) 0.0344(14) 0.0357(15) 0.0065(11) 0.0012(15) -0.0061(16) C151 0.0324(17) 0.0344(14) 0.0357(15) 0.0065(11) 0.0012(15) -0.0061(16) C152 0.0324(17) 0.0344(14) 0.0357(15) 0.0065(11) 0.0012(15) -0.0061(16) C153 0.026(3) 0.027(2) 0.028(2) 0.0031(17) 0.000(2) 0.004(2) S4A 0.0261(10) 0.0339(8) 0.0299(8) 0.0063(7) 0.0007(9) 0.0098(9) S3A 0.0501(13) 0.0394(9) 0.0290(8) 0.0065(7) 0.0001(11) 0.0221(11) S2A 0.0308(11) 0.0366(9) 0.0325(9) 0.0006(7) 0.0018(9) 0.0107(9) S1A 0.0369(11) 0.0375(9) 0.0269(8) 0.0010(7) -0.0019(9) 0.0173(9) C1A 0.039(3) 0.056(2) 0.0313(18) -0.0003(17) 0.002(2) 0.007(2) C2A 0.039(3) 0.056(2) 0.0313(18) -0.0003(17) 0.002(2) 0.007(2) C3A 0.039(3) 0.056(2) 0.0313(18) -0.0003(17) 0.002(2) 0.007(2) C4A 0.039(3) 0.056(2) 0.0313(18) -0.0003(17) 0.002(2) 0.007(2) C5A 0.024(4) 0.024(3) 0.035(4) 0.005(3) -0.003(4) 0.011(3) C6A 0.031(4) 0.028(3) 0.023(3) 0.005(3) -0.004(3) 0.008(3) C7A 0.066(7) 0.041(4) 0.035(4) 0.006(3) 0.015(5) 0.008(5) C8A 0.037(4) 0.020(3) 0.027(3) -0.002(2) 0.004(4) 0.008(3) C9A 0.031(4) 0.030(3) 0.019(3) -0.003(2) -0.001(3) 0.000(3) C10A 0.029(4) 0.024(3) 0.028(3) 0.002(3) 0.000(4) -0.004(3) C11A 0.041(4) 0.024(2) 0.020(2) 0.0007(18) -0.006(3) -0.003(3) S1B 0.0725(18) 0.0352(9) 0.0471(11) -0.0129(8) 0.0260(13) -0.0128(12) S2B 0.0467(13) 0.0419(10) 0.0511(11) 0.0035(9) -0.0043(11) -0.0080(11) S3B 0.0493(14) 0.0403(10) 0.0369(10) -0.0062(8) 0.0056(11) 0.0171(11) S4B 0.0393(12) 0.0330(9) 0.0475(10) -0.0050(7) 0.0062(11) 0.0076(10) C1B 0.098(4) 0.069(3) 0.044(2) -0.010(2) 0.010(3) -0.053(3) C2B 0.098(4) 0.069(3) 0.044(2) -0.010(2) 0.010(3) -0.053(3) C3B 0.098(4) 0.069(3) 0.044(2) -0.010(2) 0.010(3) -0.053(3) C4B 0.098(4) 0.069(3) 0.044(2) -0.010(2) 0.010(3) -0.053(3) C5B 0.036(5) 0.036(4) 0.039(4) -0.004(3) -0.006(4) -0.006(4) C6B 0.031(4) 0.037(4) 0.041(4) -0.008(3) -0.007(4) 0.005(4) C7B 0.071(7) 0.051(5) 0.047(5) 0.006(4) 0.016(5) 0.007(5) C8B 0.046(5) 0.042(4) 0.027(3) -0.010(3) -0.003(4) 0.021(4) C9B 0.036(5) 0.044(4) 0.029(3) -0.010(3) 0.004(4) -0.005(4) C10B 0.044(5) 0.034(4) 0.030(4) 0.001(3) -0.006(4) 0.001(4) C11B 0.041(4) 0.024(2) 0.020(2) 0.0007(18) -0.006(3) -0.003(3) Pt2 0.02625(14) 0.03592(13) 0.01923(11) 0.00130(10) -0.00023(14) -0.01327(13) P2 0.0363(12) 0.0523(11) 0.0201(8) 0.0012(8) 0.0001(9) -0.0234(11) P22 0.0353(12) 0.0391(9) 0.0206(8) 0.0021(7) -0.0060(9) -0.0180(10) C221 0.044(2) 0.098(3) 0.064(2) -0.004(2) 0.018(2) -0.005(3) C222 0.044(2) 0.098(3) 0.064(2) -0.004(2) 0.018(2) -0.005(3) C223 0.044(2) 0.098(3) 0.064(2) -0.004(2) 0.018(2) -0.005(3) C224 0.044(2) 0.098(3) 0.064(2) -0.004(2) 0.018(2) -0.005(3) C225 0.044(2) 0.098(3) 0.064(2) -0.004(2) 0.018(2) -0.005(3) C226 0.044(2) 0.098(3) 0.064(2) -0.004(2) 0.018(2) -0.005(3) C227 0.088(3) 0.0526(18) 0.0412(17) 0.0067(14) -0.023(2) -0.018(2) C228 0.088(3) 0.0526(18) 0.0412(17) 0.0067(14) -0.023(2) -0.018(2) C229 0.088(3) 0.0526(18) 0.0412(17) 0.0067(14) -0.023(2) -0.018(2) C230 0.088(3) 0.0526(18) 0.0412(17) 0.0067(14) -0.023(2) -0.018(2) C231 0.088(3) 0.0526(18) 0.0412(17) 0.0067(14) -0.023(2) -0.018(2) C232 0.088(3) 0.0526(18) 0.0412(17) 0.0067(14) -0.023(2) -0.018(2) C233 0.049(4) 0.068(4) 0.029(2) 0.010(2) -0.012(3) -0.040(3) C241 0.051(2) 0.072(2) 0.0425(18) -0.0065(16) -0.0117(18) 0.005(2) C242 0.051(2) 0.072(2) 0.0425(18) -0.0065(16) -0.0117(18) 0.005(2) C243 0.051(2) 0.072(2) 0.0425(18) -0.0065(16) -0.0117(18) 0.005(2) C244 0.051(2) 0.072(2) 0.0425(18) -0.0065(16) -0.0117(18) 0.005(2) C245 0.051(2) 0.072(2) 0.0425(18) -0.0065(16) -0.0117(18) 0.005(2) C246 0.051(2) 0.072(2) 0.0425(18) -0.0065(16) -0.0117(18) 0.005(2) C247 0.044(2) 0.0379(15) 0.0321(15) -0.0036(11) -0.0040(15) -0.0049(17) C248 0.044(2) 0.0379(15) 0.0321(15) -0.0036(11) -0.0040(15) -0.0049(17) C249 0.044(2) 0.0379(15) 0.0321(15) -0.0036(11) -0.0040(15) -0.0049(17) C250 0.044(2) 0.0379(15) 0.0321(15) -0.0036(11) -0.0040(15) -0.0049(17) C251 0.044(2) 0.0379(15) 0.0321(15) -0.0036(11) -0.0040(15) -0.0049(17) C252 0.044(2) 0.0379(15) 0.0321(15) -0.0036(11) -0.0040(15) -0.0049(17) C253 0.049(4) 0.068(4) 0.029(2) 0.010(2) -0.012(3) -0.040(3) S1C 0.0341(11) 0.0281(8) 0.0239(8) 0.0022(6) -0.0060(9) -0.0026(9) S2C 0.0342(11) 0.0363(9) 0.0317(9) 0.0032(7) 0.0016(9) -0.0069(9) S3C 0.0470(13) 0.0320(8) 0.0255(8) -0.0010(6) -0.0047(10) -0.0134(10) S4C 0.0237(9) 0.0248(8) 0.0233(8) -0.0002(6) -0.0018(8) -0.0004(8) C1C 0.040(5) 0.072(5) 0.027(4) 0.010(4) -0.010(4) -0.014(5) C2C 0.037(5) 0.036(4) 0.022(3) 0.007(3) -0.002(4) 0.005(4) C3C 0.027(4) 0.047(4) 0.022(3) 0.006(3) 0.002(3) 0.003(4) C4C 0.060(6) 0.060(5) 0.048(4) 0.029(4) -0.012(5) -0.019(5) C5C 0.030(4) 0.018(3) 0.023(3) -0.001(2) -0.004(3) 0.009(3) C6C 0.019(4) 0.017(3) 0.032(3) -0.006(2) -0.001(3) 0.000(3) C7C 0.063(6) 0.042(4) 0.025(3) 0.003(3) -0.007(4) -0.017(5) C8C 0.037(4) 0.022(3) 0.024(3) -0.003(2) -0.005(4) -0.001(3) C9C 0.029(4) 0.018(3) 0.022(3) 0.000(3) -0.003(4) 0.002(3) C10C 0.025(4) 0.025(3) 0.026(3) -0.002(3) 0.004(3) 0.001(3) C11C 0.025(3) 0.030(2) 0.022(2) -0.0009(18) 0.002(2) -0.009(2) S1D 0.0389(12) 0.0341(9) 0.0328(9) -0.0005(7) 0.0112(10) -0.0068(9) S2D 0.0353(11) 0.0317(8) 0.0355(9) 0.0027(7) 0.0045(9) -0.0014(9) S3D 0.0407(12) 0.0408(9) 0.0296(9) -0.0005(7) 0.0090(10) -0.0143(10) S4D 0.0387(12) 0.0369(9) 0.0337(9) 0.0078(7) 0.0064(10) -0.0082(10) C1D 0.042(5) 0.056(4) 0.027(3) -0.001(3) 0.005(4) -0.014(4) C2D 0.031(4) 0.047(4) 0.029(4) -0.003(3) 0.002(4) -0.004(4) C3D 0.027(4) 0.029(3) 0.037(4) 0.002(3) 0.002(4) -0.002(3) C4D 0.038(5) 0.041(4) 0.046(4) -0.004(3) -0.003(4) 0.010(4) C5D 0.029(4) 0.032(3) 0.038(4) 0.004(3) 0.007(4) -0.004(4) C6D 0.028(4) 0.034(3) 0.028(3) 0.002(3) 0.010(4) -0.005(4) C7D 0.049(5) 0.057(4) 0.030(4) 0.007(3) 0.010(4) -0.003(5) C8D 0.031(4) 0.053(4) 0.021(3) -0.001(3) 0.005(4) -0.005(4) C9D 0.030(4) 0.044(4) 0.025(3) 0.007(3) 0.003(4) -0.012(4) C10D 0.039(5) 0.043(4) 0.025(3) 0.004(3) 0.000(4) -0.001(4) C11D 0.025(3) 0.030(2) 0.022(2) -0.0009(18) 0.002(2) -0.009(2) #----------------------------------------------------------------------------# # 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 C11A 2.000(6) . ? Pt1 C11B 2.017(7) . ? Pt1 P1 2.2906(17) . ? Pt1 P11 2.2963(16) . ? P1 C121 1.781(8) . ? P1 C133 1.823(6) . ? P1 C127 1.832(7) . ? P11 C147 1.811(7) . ? P11 C141 1.812(7) . ? P11 C153 1.851(6) . ? C121 C126 1.368(9) . ? C121 C122 1.409(10) . ? C122 C123 1.376(11) . ? C122 H122 0.95 . ? C123 C124 1.403(10) . ? C123 H123 0.95 . ? C124 C125 1.349(10) . ? C124 H124 0.95 . ? C125 C126 1.380(10) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C127 C128 1.370(10) . ? C127 C132 1.371(9) . ? C128 C129 1.392(9) . ? C128 H128 0.95 . ? C129 C130 1.404(9) . ? C129 H129 0.95 . ? C130 C131 1.350(10) . ? C130 H130 0.95 . ? C131 C132 1.383(9) . ? C131 H131 0.95 . ? C132 H132 0.95 . ? C133 C153 1.520(8) . ? C133 H13A 0.99 . ? C133 H13B 0.99 . ? C141 C142 1.389(10) . ? C141 C146 1.412(9) . ? C142 C143 1.390(10) . ? C142 H142 0.95 . ? C143 C144 1.385(9) . ? C143 H143 0.95 . ? C144 C145 1.347(10) . ? C144 H144 0.95 . ? C145 C146 1.417(10) . ? C145 H145 0.95 . ? C146 H146 0.95 . ? C147 C152 1.371(10) . ? C147 C148 1.371(8) . ? C148 C149 1.389(9) . ? C148 H148 0.95 . ? C149 C150 1.340(9) . ? C149 H149 0.95 . ? C150 C151 1.354(9) . ? C150 H150 0.95 . ? C151 C152 1.381(9) . ? C151 H151 0.95 . ? C152 H152 0.95 . ? C153 H15A 0.99 . ? C153 H15B 0.99 . ? S4A C6A 1.768(7) . ? S4A C9A 1.778(6) . ? S3A C8A 1.738(6) . ? S3A C6A 1.743(6) . ? S2A C5A 1.773(7) . ? S2A C3A 1.784(8) . ? S1A C5A 1.754(7) . ? S1A C2A 1.773(7) . ? C1A C2A 1.510(10) . ? C1A H1A1 0.98 . ? C1A H1A2 0.98 . ? C1A H1A3 0.98 . ? C2A C3A 1.314(10) . ? C3A C4A 1.489(9) . ? C4A H4A1 0.98 . ? C4A H4A2 0.98 . ? C4A H4A3 0.98 . ? C5A C6A 1.334(8) . ? C7A C8A 1.530(9) . ? C7A H7A1 0.98 . ? C7A H7A2 0.98 . ? C7A H7A3 0.98 . ? C8A C9A 1.344(9) . ? C9A C10A 1.429(9) . ? C10A C11A 1.206(8) . ? S1B C2B 1.739(9) . ? S1B C5B 1.746(7) . ? S2B C5B 1.754(7) . ? S2B C3B 1.784(9) . ? S3B C6B 1.748(7) . ? S3B C8B 1.773(8) . ? S4B C6B 1.759(7) . ? S4B C9B 1.774(7) . ? C1B C2B 1.490(11) . ? C1B H1B1 0.98 . ? C1B H1B2 0.98 . ? C1B H1B3 0.98 . ? C2B C3B 1.309(13) . ? C3B C4B 1.534(11) . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? C5B C6B 1.336(9) . ? C7B C8B 1.431(10) . ? C7B H7B1 0.98 . ? C7B H7B2 0.98 . ? C7B H7B3 0.98 . ? C8B C9B 1.348(9) . ? C9B C10B 1.442(10) . ? C10B C11B 1.193(9) . ? Pt2 C11C 1.995(6) . ? Pt2 C11D 2.009(7) . ? Pt2 P2 2.2830(19) . ? Pt2 P22 2.2945(17) . ? P2 C227 1.802(8) . ? P2 C221 1.815(10) . ? P2 C233 1.844(7) . ? P22 C247 1.813(7) . ? P22 C241 1.815(8) . ? P22 C253 1.827(7) . ? C221 C222 1.363(12) . ? C221 C226 1.397(12) . ? C222 C223 1.380(12) . ? C222 H222 0.95 . ? C223 C224 1.327(12) . ? C223 H223 0.95 . ? C224 C225 1.362(12) . ? C224 H224 0.95 . ? C225 C226 1.366(12) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C227 C228 1.359(10) . ? C227 C232 1.381(10) . ? C228 C229 1.387(10) . ? C228 H228 0.95 . ? C229 C230 1.313(10) . ? C229 H229 0.95 . ? C230 C231 1.388(11) . ? C230 H230 0.95 . ? C231 C232 1.382(10) . ? C231 H231 0.95 . ? C232 H232 0.95 . ? C233 C253 1.536(10) . ? C233 H23A 0.99 . ? C233 H23B 0.99 . ? C241 C246 1.373(11) . ? C241 C242 1.383(11) . ? C242 C243 1.369(11) . ? C242 H242 0.95 . ? C243 C244 1.350(11) . ? C243 H243 0.95 . ? C244 C245 1.360(11) . ? C244 H244 0.95 . ? C245 C246 1.379(11) . ? C245 H245 0.95 . ? C246 H246 0.95 . ? C247 C252 1.369(10) . ? C247 C248 1.386(8) . ? C248 C249 1.402(9) . ? C248 H248 0.95 . ? C249 C250 1.361(10) . ? C249 H249 0.95 . ? C250 C251 1.388(9) . ? C250 H250 0.95 . ? C251 C252 1.393(9) . ? C251 H251 0.95 . ? C252 H252 0.95 . ? C253 H25A 0.99 . ? C253 H25B 0.99 . ? S1C C5C 1.740(6) . ? S1C C2C 1.751(6) . ? S2C C3C 1.752(7) . ? S2C C5C 1.758(6) . ? S3C C8C 1.738(6) . ? S3C C6C 1.765(6) . ? S4C C6C 1.755(6) . ? S4C C9C 1.774(6) . ? C1C C2C 1.497(10) . ? C1C H1C1 0.98 . ? C1C H1C2 0.98 . ? C1C H1C3 0.98 . ? C2C C3C 1.343(10) . ? C3C C4C 1.518(8) . ? C4C H4C1 0.98 . ? C4C H4C2 0.98 . ? C4C H4C3 0.98 . ? C5C C6C 1.343(8) . ? C7C C8C 1.517(8) . ? C7C H7C1 0.98 . ? C7C H7C2 0.98 . ? C7C H7C3 0.98 . ? C8C C9C 1.339(8) . ? C9C C10C 1.422(8) . ? C10C C11C 1.207(8) . ? S1D C5D 1.763(6) . ? S1D C2D 1.766(7) . ? S2D C5D 1.755(7) . ? S2D C3D 1.758(7) . ? S3D C8D 1.758(7) . ? S3D C6D 1.772(6) . ? S4D C6D 1.756(6) . ? S4D C9D 1.780(7) . ? C1D C2D 1.524(9) . ? C1D H1D1 0.98 . ? C1D H1D2 0.98 . ? C1D H1D3 0.98 . ? C2D C3D 1.329(9) . ? C3D C4D 1.503(9) . ? C4D H4D1 0.98 . ? C4D H4D2 0.98 . ? C4D H4D3 0.98 . ? C5D C6D 1.335(9) . ? C7D C8D 1.559(9) . ? C7D H7D1 0.98 . ? C7D H7D2 0.98 . ? C7D H7D3 0.98 . ? C8D C9D 1.327(9) . ? C9D C10D 1.442(10) . ? C10D C11D 1.186(9) . ? 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 C11A Pt1 C11B 88.1(3) . . ? C11A Pt1 P1 91.3(2) . . ? C11B Pt1 P1 177.48(19) . . ? C11A Pt1 P11 176.3(2) . . ? C11B Pt1 P11 95.46(17) . . ? P1 Pt1 P11 85.08(6) . . ? C121 P1 C133 103.5(4) . . ? C121 P1 C127 104.7(3) . . ? C133 P1 C127 107.0(3) . . ? C121 P1 Pt1 116.4(3) . . ? C133 P1 Pt1 106.9(2) . . ? C127 P1 Pt1 117.2(3) . . ? C147 P11 C141 103.9(3) . . ? C147 P11 C153 104.6(3) . . ? C141 P11 C153 102.9(3) . . ? C147 P11 Pt1 123.1(2) . . ? C141 P11 Pt1 113.4(2) . . ? C153 P11 Pt1 106.90(19) . . ? C126 C121 C122 116.4(7) . . ? C126 C121 P1 125.5(6) . . ? C122 C121 P1 117.5(5) . . ? C123 C122 C121 121.1(7) . . ? C123 C122 H122 119.4 . . ? C121 C122 H122 119.4 . . ? C122 C123 C124 120.1(8) . . ? C122 C123 H123 119.9 . . ? C124 C123 H123 119.9 . . ? C125 C124 C123 118.3(7) . . ? C125 C124 H124 120.9 . . ? C123 C124 H124 120.9 . . ? C124 C125 C126 121.2(7) . . ? C124 C125 H125 119.4 . . ? C126 C125 H125 119.4 . . ? C121 C126 C125 122.3(7) . . ? C121 C126 H126 118.9 . . ? C125 C126 H126 118.9 . . ? C128 C127 C132 119.5(6) . . ? C128 C127 P1 118.1(5) . . ? C132 C127 P1 122.1(6) . . ? C127 C128 C129 119.6(6) . . ? C127 C128 H128 120.2 . . ? C129 C128 H128 120.2 . . ? C128 C129 C130 120.2(7) . . ? C128 C129 H129 119.9 . . ? C130 C129 H129 119.9 . . ? C131 C130 C129 119.1(6) . . ? C131 C130 H130 120.5 . . ? C129 C130 H130 120.5 . . ? C130 C131 C132 120.4(6) . . ? C130 C131 H131 119.8 . . ? C132 C131 H131 119.8 . . ? C127 C132 C131 121.2(7) . . ? C127 C132 H132 119.4 . . ? C131 C132 H132 119.4 . . ? C153 C133 P1 110.3(5) . . ? C153 C133 H13A 109.6 . . ? P1 C133 H13A 109.6 . . ? C153 C133 H13B 109.6 . . ? P1 C133 H13B 109.6 . . ? H13A C133 H13B 108.1 . . ? C142 C141 C146 119.1(7) . . ? C142 C141 P11 121.6(5) . . ? C146 C141 P11 119.4(6) . . ? C141 C142 C143 120.4(7) . . ? C141 C142 H142 119.8 . . ? C143 C142 H142 119.8 . . ? C144 C143 C142 120.4(7) . . ? C144 C143 H143 119.8 . . ? C142 C143 H143 119.8 . . ? C145 C144 C143 120.1(7) . . ? C145 C144 H144 120 . . ? C143 C144 H144 120 . . ? C144 C145 C146 121.4(7) . . ? C144 C145 H145 119.3 . . ? C146 C145 H145 119.3 . . ? C141 C146 C145 118.6(7) . . ? C141 C146 H146 120.7 . . ? C145 C146 H146 120.7 . . ? C152 C147 C148 117.9(6) . . ? C152 C147 P11 119.4(5) . . ? C148 C147 P11 122.8(6) . . ? C147 C148 C149 119.8(7) . . ? C147 C148 H148 120.1 . . ? C149 C148 H148 120.1 . . ? C150 C149 C148 121.3(6) . . ? C150 C149 H149 119.3 . . ? C148 C149 H149 119.3 . . ? C149 C150 C151 119.7(7) . . ? C149 C150 H150 120.1 . . ? C151 C150 H150 120.1 . . ? C150 C151 C152 119.7(7) . . ? C150 C151 H151 120.2 . . ? C152 C151 H151 120.2 . . ? C147 C152 C151 121.6(6) . . ? C147 C152 H152 119.2 . . ? C151 C152 H152 119.2 . . ? C133 C153 P11 105.9(4) . . ? C133 C153 H15A 110.6 . . ? P11 C153 H15A 110.6 . . ? C133 C153 H15B 110.6 . . ? P11 C153 H15B 110.6 . . ? H15A C153 H15B 108.7 . . ? C6A S4A C9A 94.8(3) . . ? C8A S3A C6A 95.4(3) . . ? C5A S2A C3A 95.5(3) . . ? C5A S1A C2A 95.9(3) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C3A C2A C1A 127.1(7) . . ? C3A C2A S1A 117.6(6) . . ? C1A C2A S1A 115.1(5) . . ? C2A C3A C4A 127.8(7) . . ? C2A C3A S2A 116.8(5) . . ? C4A C3A S2A 115.3(6) . . ? C3A C4A H4A1 109.5 . . ? C3A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C3A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C6A C5A S1A 123.6(5) . . ? C6A C5A S2A 123.4(5) . . ? S1A C5A S2A 112.8(3) . . ? C5A C6A S3A 122.9(5) . . ? C5A C6A S4A 122.9(5) . . ? S3A C6A S4A 114.1(3) . . ? C8A C7A H7A1 109.5 . . ? C8A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C8A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C9A C8A C7A 125.0(6) . . ? C9A C8A S3A 118.6(5) . . ? C7A C8A S3A 116.4(5) . . ? C8A C9A C10A 126.8(6) . . ? C8A C9A S4A 115.6(5) . . ? C10A C9A S4A 117.6(5) . . ? C11A C10A C9A 177.1(6) . . ? C10A C11A Pt1 174.4(7) . . ? C2B S1B C5B 95.3(4) . . ? C5B S2B C3B 93.6(4) . . ? C6B S3B C8B 95.4(3) . . ? C6B S4B C9B 94.3(3) . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C3B C2B C1B 126.1(8) . . ? C3B C2B S1B 117.3(7) . . ? C1B C2B S1B 116.2(7) . . ? C2B C3B C4B 128.9(8) . . ? C2B C3B S2B 117.5(7) . . ? C4B C3B S2B 113.5(7) . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C6B C5B S1B 122.5(5) . . ? C6B C5B S2B 123.6(6) . . ? S1B C5B S2B 113.9(4) . . ? C5B C6B S3B 123.5(5) . . ? C5B C6B S4B 123.6(5) . . ? S3B C6B S4B 112.9(4) . . ? C8B C7B H7B1 109.5 . . ? C8B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C8B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C9B C8B C7B 126.1(7) . . ? C9B C8B S3B 115.4(6) . . ? C7B C8B S3B 118.4(5) . . ? C8B C9B C10B 127.3(7) . . ? C8B C9B S4B 117.3(6) . . ? C10B C9B S4B 115.4(5) . . ? C11B C10B C9B 172.7(7) . . ? C10B C11B Pt1 175.3(6) . . ? C11C Pt2 C11D 88.2(3) . . ? C11C Pt2 P2 91.16(19) . . ? C11D Pt2 P2 179.35(19) . . ? C11C Pt2 P22 176.82(19) . . ? C11D Pt2 P22 94.94(18) . . ? P2 Pt2 P22 85.66(6) . . ? C227 P2 C221 104.8(4) . . ? C227 P2 C233 107.6(4) . . ? C221 P2 C233 102.2(4) . . ? C227 P2 Pt2 115.6(3) . . ? C221 P2 Pt2 117.3(3) . . ? C233 P2 Pt2 108.3(2) . . ? C247 P22 C241 101.9(3) . . ? C247 P22 C253 106.4(3) . . ? C241 P22 C253 103.7(4) . . ? C247 P22 Pt2 121.9(3) . . ? C241 P22 Pt2 115.3(3) . . ? C253 P22 Pt2 106.1(2) . . ? C222 C221 C226 119.1(9) . . ? C222 C221 P2 121.7(7) . . ? C226 C221 P2 119.1(8) . . ? C221 C222 C223 119.1(9) . . ? C221 C222 H222 120.5 . . ? C223 C222 H222 120.5 . . ? C224 C223 C222 123.3(10) . . ? C224 C223 H223 118.4 . . ? C222 C223 H223 118.4 . . ? C223 C224 C225 117.0(10) . . ? C223 C224 H224 121.5 . . ? C225 C224 H224 121.5 . . ? C224 C225 C226 123.2(9) . . ? C224 C225 H225 118.4 . . ? C226 C225 H225 118.4 . . ? C225 C226 C221 118.2(9) . . ? C225 C226 H226 120.9 . . ? C221 C226 H226 120.9 . . ? C228 C227 C232 116.9(7) . . ? C228 C227 P2 121.2(6) . . ? C232 C227 P2 122.0(6) . . ? C227 C228 C229 122.7(7) . . ? C227 C228 H228 118.7 . . ? C229 C228 H228 118.7 . . ? C230 C229 C228 121.0(8) . . ? C230 C229 H229 119.5 . . ? C228 C229 H229 119.5 . . ? C229 C230 C231 118.0(8) . . ? C229 C230 H230 121 . . ? C231 C230 H230 121 . . ? C232 C231 C230 121.8(7) . . ? C232 C231 H231 119.1 . . ? C230 C231 H231 119.1 . . ? C227 C232 C231 119.7(8) . . ? C227 C232 H232 120.2 . . ? C231 C232 H232 120.2 . . ? C253 C233 P2 108.0(6) . . ? C253 C233 H23A 110.1 . . ? P2 C233 H23A 110.1 . . ? C253 C233 H23B 110.1 . . ? P2 C233 H23B 110.1 . . ? H23A C233 H23B 108.4 . . ? C246 C241 C242 117.9(8) . . ? C246 C241 P22 121.0(6) . . ? C242 C241 P22 121.0(7) . . ? C243 C242 C241 120.8(8) . . ? C243 C242 H242 119.6 . . ? C241 C242 H242 119.6 . . ? C244 C243 C242 121.5(8) . . ? C244 C243 H243 119.3 . . ? C242 C243 H243 119.3 . . ? C243 C244 C245 117.9(8) . . ? C243 C244 H244 121.1 . . ? C245 C244 H244 121.1 . . ? C244 C245 C246 122.3(8) . . ? C244 C245 H245 118.9 . . ? C246 C245 H245 118.9 . . ? C241 C246 C245 119.5(8) . . ? C241 C246 H246 120.2 . . ? C245 C246 H246 120.2 . . ? C252 C247 C248 118.3(7) . . ? C252 C247 P22 118.2(5) . . ? C248 C247 P22 123.5(6) . . ? C247 C248 C249 121.3(7) . . ? C247 C248 H248 119.4 . . ? C249 C248 H248 119.4 . . ? C250 C249 C248 119.4(6) . . ? C250 C249 H249 120.3 . . ? C248 C249 H249 120.3 . . ? C249 C250 C251 120.2(7) . . ? C249 C250 H250 119.9 . . ? C251 C250 H250 119.9 . . ? C250 C251 C252 119.8(7) . . ? C250 C251 H251 120.1 . . ? C252 C251 H251 120.1 . . ? C247 C252 C251 121.1(6) . . ? C247 C252 H252 119.4 . . ? C251 C252 H252 119.4 . . ? C233 C253 P22 109.7(5) . . ? C233 C253 H25A 109.7 . . ? P22 C253 H25A 109.7 . . ? C233 C253 H25B 109.7 . . ? P22 C253 H25B 109.7 . . ? H25A C253 H25B 108.2 . . ? C5C S1C C2C 95.7(3) . . ? C3C S2C C5C 94.6(3) . . ? C8C S3C C6C 94.6(3) . . ? C6C S4C C9C 95.1(3) . . ? C2C C1C H1C1 109.5 . . ? C2C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? C2C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? C3C C2C C1C 127.2(6) . . ? C3C C2C S1C 116.2(5) . . ? C1C C2C S1C 116.5(5) . . ? C2C C3C C4C 126.5(6) . . ? C2C C3C S2C 117.7(5) . . ? C4C C3C S2C 115.8(6) . . ? C3C C4C H4C1 109.5 . . ? C3C C4C H4C2 109.5 . . ? H4C1 C4C H4C2 109.5 . . ? C3C C4C H4C3 109.5 . . ? H4C1 C4C H4C3 109.5 . . ? H4C2 C4C H4C3 109.5 . . ? C6C C5C S1C 124.0(5) . . ? C6C C5C S2C 122.1(5) . . ? S1C C5C S2C 113.9(3) . . ? C5C C6C S4C 124.3(5) . . ? C5C C6C S3C 121.7(5) . . ? S4C C6C S3C 114.0(3) . . ? C8C C7C H7C1 109.5 . . ? C8C C7C H7C2 109.5 . . ? H7C1 C7C H7C2 109.5 . . ? C8C C7C H7C3 109.5 . . ? H7C1 C7C H7C3 109.5 . . ? H7C2 C7C H7C3 109.5 . . ? C9C C8C C7C 123.7(6) . . ? C9C C8C S3C 119.1(5) . . ? C7C C8C S3C 117.2(5) . . ? C8C C9C C10C 126.6(6) . . ? C8C C9C S4C 115.6(5) . . ? C10C C9C S4C 117.7(5) . . ? C11C C10C C9C 176.6(7) . . ? C10C C11C Pt2 176.9(6) . . ? C5D S1D C2D 95.4(3) . . ? C5D S2D C3D 96.1(3) . . ? C8D S3D C6D 94.1(3) . . ? C6D S4D C9D 94.5(3) . . ? C2D C1D H1D1 109.5 . . ? C2D C1D H1D2 109.5 . . ? H1D1 C1D H1D2 109.5 . . ? C2D C1D H1D3 109.5 . . ? H1D1 C1D H1D3 109.5 . . ? H1D2 C1D H1D3 109.5 . . ? C3D C2D C1D 128.3(6) . . ? C3D C2D S1D 117.4(5) . . ? C1D C2D S1D 114.1(5) . . ? C2D C3D C4D 128.4(6) . . ? C2D C3D S2D 117.0(5) . . ? C4D C3D S2D 114.5(5) . . ? C3D C4D H4D1 109.5 . . ? C3D C4D H4D2 109.5 . . ? H4D1 C4D H4D2 109.5 . . ? C3D C4D H4D3 109.5 . . ? H4D1 C4D H4D3 109.5 . . ? H4D2 C4D H4D3 109.5 . . ? C6D C5D S2D 121.7(5) . . ? C6D C5D S1D 124.9(5) . . ? S2D C5D S1D 113.4(4) . . ? C5D C6D S4D 122.7(5) . . ? C5D C6D S3D 124.6(5) . . ? S4D C6D S3D 112.7(3) . . ? C8D C7D H7D1 109.5 . . ? C8D C7D H7D2 109.5 . . ? H7D1 C7D H7D2 109.5 . . ? C8D C7D H7D3 109.5 . . ? H7D1 C7D H7D3 109.5 . . ? H7D2 C7D H7D3 109.5 . . ? C9D C8D C7D 126.7(6) . . ? C9D C8D S3D 118.4(5) . . ? C7D C8D S3D 114.9(5) . . ? C8D C9D C10D 127.0(7) . . ? C8D C9D S4D 115.6(5) . . ? C10D C9D S4D 117.4(5) . . ? C11D C10D C9D 172.5(7) . . ? C10D C11D Pt2 176.4(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11A Pt1 P1 C121 55.0(4) . . . . ? P11 Pt1 P1 C121 -124.2(3) . . . . ? C11A Pt1 P1 C133 170.0(3) . . . . ? P11 Pt1 P1 C133 -9.2(2) . . . . ? C11A Pt1 P1 C127 -70.0(3) . . . . ? P11 Pt1 P1 C127 110.8(2) . . . . ? C11B Pt1 P11 C147 45.1(3) . . . . ? P1 Pt1 P11 C147 -137.4(3) . . . . ? C11B Pt1 P11 C141 -81.4(3) . . . . ? P1 Pt1 P11 C141 96.1(2) . . . . ? C11B Pt1 P11 C153 165.9(3) . . . . ? P1 Pt1 P11 C153 -16.5(2) . . . . ? C133 P1 C121 C126 99.8(8) . . . . ? C127 P1 C121 C126 -12.1(9) . . . . ? Pt1 P1 C121 C126 -143.3(7) . . . . ? C133 P1 C121 C122 -71.3(6) . . . . ? C127 P1 C121 C122 176.8(6) . . . . ? Pt1 P1 C121 C122 45.7(7) . . . . ? C126 C121 C122 C123 3.8(10) . . . . ? P1 C121 C122 C123 175.7(6) . . . . ? C121 C122 C123 C124 2.8(11) . . . . ? C122 C123 C124 C125 -7.2(12) . . . . ? C123 C124 C125 C126 5.0(13) . . . . ? C122 C121 C126 C125 -6.2(12) . . . . ? P1 C121 C126 C125 -177.4(7) . . . . ? C124 C125 C126 C121 1.9(14) . . . . ? C121 P1 C127 C128 -74.5(6) . . . . ? C133 P1 C127 C128 176.1(5) . . . . ? Pt1 P1 C127 C128 56.2(6) . . . . ? C121 P1 C127 C132 98.4(7) . . . . ? C133 P1 C127 C132 -11.0(7) . . . . ? Pt1 P1 C127 C132 -130.9(6) . . . . ? C132 C127 C128 C129 2.0(9) . . . . ? P1 C127 C128 C129 175.1(5) . . . . ? C127 C128 C129 C130 -0.6(9) . . . . ? C128 C129 C130 C131 -1.3(11) . . . . ? C129 C130 C131 C132 1.8(11) . . . . ? C128 C127 C132 C131 -1.5(11) . . . . ? P1 C127 C132 C131 -174.3(6) . . . . ? C130 C131 C132 C127 -0.4(12) . . . . ? C121 P1 C133 C153 163.9(4) . . . . ? C127 P1 C133 C153 -85.9(5) . . . . ? Pt1 P1 C133 C153 40.4(4) . . . . ? C147 P11 C141 C142 51.6(6) . . . . ? C153 P11 C141 C142 -57.2(6) . . . . ? Pt1 P11 C141 C142 -172.3(4) . . . . ? C147 P11 C141 C146 -128.8(6) . . . . ? C153 P11 C141 C146 122.4(6) . . . . ? Pt1 P11 C141 C146 7.3(6) . . . . ? C146 C141 C142 C143 -2.7(9) . . . . ? P11 C141 C142 C143 176.9(5) . . . . ? C141 C142 C143 C144 1.5(9) . . . . ? C142 C143 C144 C145 -0.1(10) . . . . ? C143 C144 C145 C146 -0.1(10) . . . . ? C142 C141 C146 C145 2.5(9) . . . . ? P11 C141 C146 C145 -177.1(5) . . . . ? C144 C145 C146 C141 -1.1(10) . . . . ? C141 P11 C147 C152 84.6(6) . . . . ? C153 P11 C147 C152 -167.9(5) . . . . ? Pt1 P11 C147 C152 -46.0(6) . . . . ? C141 P11 C147 C148 -94.8(6) . . . . ? C153 P11 C147 C148 12.7(6) . . . . ? Pt1 P11 C147 C148 134.6(5) . . . . ? C152 C147 C148 C149 -1.3(9) . . . . ? P11 C147 C148 C149 178.1(5) . . . . ? C147 C148 C149 C150 0.0(9) . . . . ? C148 C149 C150 C151 1.5(10) . . . . ? C149 C150 C151 C152 -1.6(10) . . . . ? C148 C147 C152 C151 1.1(10) . . . . ? P11 C147 C152 C151 -178.3(5) . . . . ? C150 C151 C152 C147 0.3(11) . . . . ? P1 C133 C153 P11 -54.4(5) . . . . ? C147 P11 C153 C133 176.5(4) . . . . ? C141 P11 C153 C133 -75.2(5) . . . . ? Pt1 P11 C153 C133 44.5(5) . . . . ? C5A S1A C2A C3A -7.3(7) . . . . ? C5A S1A C2A C1A 177.9(6) . . . . ? C1A C2A C3A C4A -7.0(14) . . . . ? S1A C2A C3A C4A 178.9(6) . . . . ? C1A C2A C3A S2A 174.4(6) . . . . ? S1A C2A C3A S2A 0.3(9) . . . . ? C5A S2A C3A C2A 6.7(7) . . . . ? C5A S2A C3A C4A -172.0(6) . . . . ? C2A S1A C5A C6A -173.2(6) . . . . ? C2A S1A C5A S2A 11.4(4) . . . . ? C3A S2A C5A C6A 173.3(6) . . . . ? C3A S2A C5A S1A -11.2(4) . . . . ? S1A C5A C6A S3A 3.2(9) . . . . ? S2A C5A C6A S3A 178.2(4) . . . . ? S1A C5A C6A S4A -176.5(4) . . . . ? S2A C5A C6A S4A -1.5(9) . . . . ? C8A S3A C6A C5A 168.5(6) . . . . ? C8A S3A C6A S4A -11.8(4) . . . . ? C9A S4A C6A C5A -168.3(6) . . . . ? C9A S4A C6A S3A 11.9(4) . . . . ? C6A S3A C8A C9A 7.0(6) . . . . ? C6A S3A C8A C7A -174.4(6) . . . . ? C7A C8A C9A C10A 3.6(11) . . . . ? S3A C8A C9A C10A -177.9(5) . . . . ? C7A C8A C9A S4A -178.1(6) . . . . ? S3A C8A C9A S4A 0.4(8) . . . . ? C6A S4A C9A C8A -7.4(6) . . . . ? C6A S4A C9A C10A 171.0(5) . . . . ? C5B S1B C2B C3B -10.1(10) . . . . ? C5B S1B C2B C1B 176.0(7) . . . . ? C1B C2B C3B C4B -3.3(19) . . . . ? S1B C2B C3B C4B -176.5(8) . . . . ? C1B C2B C3B S2B 174.8(8) . . . . ? S1B C2B C3B S2B 1.6(13) . . . . ? C5B S2B C3B C2B 7.7(10) . . . . ? C5B S2B C3B C4B -173.9(8) . . . . ? C2B S1B C5B C6B -164.5(7) . . . . ? C2B S1B C5B S2B 15.0(5) . . . . ? C3B S2B C5B C6B 165.4(8) . . . . ? C3B S2B C5B S1B -14.1(6) . . . . ? S1B C5B C6B S3B 1.3(10) . . . . ? S2B C5B C6B S3B -178.2(4) . . . . ? S1B C5B C6B S4B -176.2(4) . . . . ? S2B C5B C6B S4B 4.3(10) . . . . ? C8B S3B C6B C5B 160.9(7) . . . . ? C8B S3B C6B S4B -21.4(5) . . . . ? C9B S4B C6B C5B -161.5(7) . . . . ? C9B S4B C6B S3B 20.8(5) . . . . ? C6B S3B C8B C9B 13.5(6) . . . . ? C6B S3B C8B C7B -169.6(7) . . . . ? C7B C8B C9B C10B 1.6(13) . . . . ? S3B C8B C9B C10B 178.3(6) . . . . ? C7B C8B C9B S4B -177.5(7) . . . . ? S3B C8B C9B S4B -0.8(8) . . . . ? C6B S4B C9B C8B -12.2(7) . . . . ? C6B S4B C9B C10B 168.7(6) . . . . ? C11C Pt2 P2 C227 67.1(3) . . . . ? P22 Pt2 P2 C227 -112.9(3) . . . . ? C11C Pt2 P2 C221 -57.2(4) . . . . ? P22 Pt2 P2 C221 122.7(3) . . . . ? C11C Pt2 P2 C233 -172.1(4) . . . . ? P22 Pt2 P2 C233 7.9(3) . . . . ? C11D Pt2 P22 C247 -41.5(3) . . . . ? P2 Pt2 P22 C247 138.3(3) . . . . ? C11D Pt2 P22 C241 82.8(4) . . . . ? P2 Pt2 P22 C241 -97.5(3) . . . . ? C11D Pt2 P22 C253 -163.2(4) . . . . ? P2 Pt2 P22 C253 16.6(3) . . . . ? C227 P2 C221 C222 -127.5(8) . . . . ? C233 P2 C221 C222 120.3(7) . . . . ? Pt2 P2 C221 C222 2.1(9) . . . . ? C227 P2 C221 C226 55.7(8) . . . . ? C233 P2 C221 C226 -56.5(8) . . . . ? Pt2 P2 C221 C226 -174.7(6) . . . . ? C226 C221 C222 C223 -0.4(11) . . . . ? P2 C221 C222 C223 -177.2(7) . . . . ? C221 C222 C223 C224 3.7(12) . . . . ? C222 C223 C224 C225 -4.3(14) . . . . ? C223 C224 C225 C226 1.7(15) . . . . ? C224 C225 C226 C221 1.4(15) . . . . ? C222 C221 C226 C225 -2.0(13) . . . . ? P2 C221 C226 C225 174.9(7) . . . . ? C221 P2 C227 C228 58.4(8) . . . . ? C233 P2 C227 C228 166.6(7) . . . . ? Pt2 P2 C227 C228 -72.2(8) . . . . ? C221 P2 C227 C232 -121.2(9) . . . . ? C233 P2 C227 C232 -13.0(10) . . . . ? Pt2 P2 C227 C232 108.2(9) . . . . ? C232 C227 C228 C229 -1.8(12) . . . . ? P2 C227 C228 C229 178.6(8) . . . . ? C227 C228 C229 C230 0.0(13) . . . . ? C228 C229 C230 C231 1.5(15) . . . . ? C229 C230 C231 C232 -1.3(16) . . . . ? C228 C227 C232 C231 2.0(14) . . . . ? P2 C227 C232 C231 -178.4(7) . . . . ? C230 C231 C232 C227 -0.5(16) . . . . ? C227 P2 C233 C253 89.5(6) . . . . ? C221 P2 C233 C253 -160.5(5) . . . . ? Pt2 P2 C233 C253 -36.1(5) . . . . ? C247 P22 C241 C246 133.4(7) . . . . ? C253 P22 C241 C246 -116.3(7) . . . . ? Pt2 P22 C241 C246 -0.8(8) . . . . ? C247 P22 C241 C242 -49.6(7) . . . . ? C253 P22 C241 C242 60.8(7) . . . . ? Pt2 P22 C241 C242 176.2(5) . . . . ? C246 C241 C242 C243 0.8(11) . . . . ? P22 C241 C242 C243 -176.3(6) . . . . ? C241 C242 C243 C244 -1.3(11) . . . . ? C242 C243 C244 C245 -0.3(12) . . . . ? C243 C244 C245 C246 2.3(13) . . . . ? C242 C241 C246 C245 1.1(12) . . . . ? P22 C241 C246 C245 178.2(6) . . . . ? C244 C245 C246 C241 -2.7(14) . . . . ? C241 P22 C247 C252 -70.8(7) . . . . ? C253 P22 C247 C252 -179.1(6) . . . . ? Pt2 P22 C247 C252 59.4(6) . . . . ? C241 P22 C247 C248 109.8(6) . . . . ? C253 P22 C247 C248 1.5(7) . . . . ? Pt2 P22 C247 C248 -120.1(6) . . . . ? C252 C247 C248 C249 1.8(10) . . . . ? P22 C247 C248 C249 -178.8(5) . . . . ? C247 C248 C249 C250 -0.4(9) . . . . ? C248 C249 C250 C251 -0.2(11) . . . . ? C249 C250 C251 C252 -0.6(11) . . . . ? C248 C247 C252 C251 -2.5(11) . . . . ? P22 C247 C252 C251 178.0(6) . . . . ? C250 C251 C252 C247 2.0(11) . . . . ? P2 C233 C253 P22 51.5(6) . . . . ? C247 P22 C253 C233 -175.2(5) . . . . ? C241 P22 C253 C233 77.8(6) . . . . ? Pt2 P22 C253 C233 -44.1(6) . . . . ? C5C S1C C2C C3C 7.5(6) . . . . ? C5C S1C C2C C1C -174.4(6) . . . . ? C1C C2C C3C C4C 3.7(12) . . . . ? S1C C2C C3C C4C -178.4(6) . . . . ? C1C C2C C3C S2C -176.9(6) . . . . ? S1C C2C C3C S2C 1.0(8) . . . . ? C5C S2C C3C C2C -8.9(6) . . . . ? C5C S2C C3C C4C 170.6(6) . . . . ? C2C S1C C5C C6C 169.2(6) . . . . ? C2C S1C C5C S2C -13.3(4) . . . . ? C3C S2C C5C C6C -168.9(6) . . . . ? C3C S2C C5C S1C 13.6(4) . . . . ? S1C C5C C6C S4C 173.7(3) . . . . ? S2C C5C C6C S4C -3.6(8) . . . . ? S1C C5C C6C S3C -4.4(8) . . . . ? S2C C5C C6C S3C 178.3(3) . . . . ? C9C S4C C6C C5C 169.5(6) . . . . ? C9C S4C C6C S3C -12.3(4) . . . . ? C8C S3C C6C C5C -169.7(6) . . . . ? C8C S3C C6C S4C 12.0(4) . . . . ? C6C S3C C8C C9C -7.1(6) . . . . ? C6C S3C C8C C7C 175.6(6) . . . . ? C7C C8C C9C C10C -1.5(10) . . . . ? S3C C8C C9C C10C -178.7(5) . . . . ? C7C C8C C9C S4C 176.7(5) . . . . ? S3C C8C C9C S4C -0.4(7) . . . . ? C6C S4C C9C C8C 7.7(5) . . . . ? C6C S4C C9C C10C -173.8(5) . . . . ? C5D S1D C2D C3D 5.2(7) . . . . ? C5D S1D C2D C1D -178.7(6) . . . . ? C1D C2D C3D C4D 3.4(14) . . . . ? S1D C2D C3D C4D 178.8(6) . . . . ? C1D C2D C3D S2D -176.4(7) . . . . ? S1D C2D C3D S2D -0.9(9) . . . . ? C5D S2D C3D C2D -3.9(7) . . . . ? C5D S2D C3D C4D 176.3(6) . . . . ? C3D S2D C5D C6D -172.3(7) . . . . ? C3D S2D C5D S1D 7.3(5) . . . . ? C2D S1D C5D C6D 171.9(7) . . . . ? C2D S1D C5D S2D -7.6(5) . . . . ? S2D C5D C6D S4D 0.4(10) . . . . ? S1D C5D C6D S4D -179.1(4) . . . . ? S2D C5D C6D S3D -176.7(4) . . . . ? S1D C5D C6D S3D 3.8(11) . . . . ? C9D S4D C6D C5D 161.1(7) . . . . ? C9D S4D C6D S3D -21.5(5) . . . . ? C8D S3D C6D C5D -163.1(7) . . . . ? C8D S3D C6D S4D 19.6(5) . . . . ? C6D S3D C8D C9D -9.2(7) . . . . ? C6D S3D C8D C7D 173.6(6) . . . . ? C7D C8D C9D C10D -8.0(13) . . . . ? S3D C8D C9D C10D 175.1(6) . . . . ? C7D C8D C9D S4D 172.2(7) . . . . ? S3D C8D C9D S4D -4.7(9) . . . . ? C6D S4D C9D C8D 16.0(6) . . . . ? C6D S4D C9D C10D -163.8(6) . . . . ?