# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Agusti Lledos' _publ_contact_author_email AGUSTI@KLINGON.UAB.ES _publ_section_title ; Aromatic C-F Activation by Complexes Containing the {Pt2S2} Core via Nucleophilic Substitution: A Combined Experimental and Theoretical Study ; loop_ _publ_author_name 'A Lledos' 'Pilar Gonzalez-Duarte' 'Ruben Mas-Balleste' 'Ainara Nova' 'Gregori Ujaque' # Attachment 'cif_II.txt' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-04-22 at 11:45:47 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : e:\xprogs\wingx\files\archive.dat # CIF files read : ub01nf1n archi data_II _database_code_depnum_ccdc_archive 'CCDC 717503' _audit_creation_date 2005-04-22T11:45:47-00:00 _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 'C33 H26 F4 P2 Pt1 S2' _chemical_formula_sum 'C33 H26 F4 P2 Pt1 S2' _chemical_formula_weight 819.69 _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 13.393(4) _cell_length_b 21.653(6) _cell_length_c 12.975(3) _cell_angle_alpha 90 _cell_angle_beta 113.829(4) _cell_angle_gamma 90 _cell_volume 3442.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1011 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 25.86 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.431089 _exptl_absorpt_correction_T_max 0.88 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_unetI/netI 0.0589 _diffrn_reflns_number 28890 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.44 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 7064 _reflns_number_gt 4923 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SMART' _computing_structure_solution 'DIRDIF Beurskens(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)' #----------------------------------------------------------------------------# # 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 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0400+0.0000*P+(0.0346P)^2^+0.0000sin\q/\l] where P = 0.10000Fo^2^ + 0.90000Fc^2^ ; _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 7064 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.398 _refine_ls_restrained_S_all 1.398 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.504 _refine_diff_density_min -1.286 _refine_diff_density_rms 0.144 #----------------------------------------------------------------------------# # SQUEEZE RESULTS #----------------------------------------------------------------------------# 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 1 0.526 0.250 0.054 315.0 84.2 2 0.474 0.750 0.034 315.0 84.7 _platon_squeeze_details ; ? ; #----------------------------------------------------------------------------# # 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 0.068175(15) 0.997005(8) 0.733522(14) 0.01482(7) Uani 1 1 d . . . S1 S -0.06948(11) 0.92466(6) 0.68207(11) 0.0195(3) Uani 1 1 d . . . S2 S -0.05536(11) 1.06984(6) 0.62577(11) 0.0210(3) Uani 1 1 d . . . P1 P 0.20204(11) 1.06901(6) 0.79416(11) 0.0175(3) Uani 1 1 d . . . P2 P 0.19014(11) 0.92360(6) 0.83250(11) 0.0163(3) Uani 1 1 d . . . C1 C -0.1846(4) 0.9667(2) 0.5966(4) 0.0188(11) Uani 1 1 d . . . C2 C -0.2869(5) 0.9375(3) 0.5492(4) 0.0257(12) Uani 1 1 d . . . C3 C -0.3782(5) 0.9679(3) 0.4796(5) 0.0271(13) Uani 1 1 d . . . C4 C -0.3716(5) 1.0281(3) 0.4514(4) 0.0294(14) Uani 1 1 d . . . C5 C -0.2731(5) 1.0578(3) 0.4968(5) 0.0269(13) Uani 1 1 d . . . C6 C -0.1765(5) 1.0292(2) 0.5694(4) 0.0210(12) Uani 1 1 d . . . C7 C 0.3271(4) 1.0445(2) 0.7803(5) 0.0219(11) Uani 1 1 d . . . H7A H 0.3095 1.0354 0.7017 0.026 Uiso 1 1 calc R . . H7B H 0.3783 1.0787 0.8019 0.026 Uiso 1 1 calc R . . C8 C 0.3830(5) 0.9884(2) 0.8502(4) 0.0236(12) Uani 1 1 d . . . H8A H 0.3982 0.9971 0.9284 0.028 Uiso 1 1 calc R . . H8B H 0.4526 0.9827 0.8447 0.028 Uiso 1 1 calc R . . C9 C 0.3193(4) 0.9275(2) 0.8174(4) 0.0196(11) Uani 1 1 d . . . H9A H 0.366 0.8948 0.8627 0.024 Uiso 1 1 calc R . . H9B H 0.3051 0.9187 0.7394 0.024 Uiso 1 1 calc R . . C10 C 0.1750(5) 1.1425(2) 0.7211(4) 0.0212(11) Uani 1 1 d . . . C11 C 0.1793(5) 1.1995(2) 0.7746(5) 0.0293(13) Uani 1 1 d . . . H11 H 0.1941 1.2006 0.851 0.035 Uiso 1 1 calc R . . C12 C 0.1615(6) 1.2538(3) 0.7138(5) 0.0403(16) Uani 1 1 d . . . H12 H 0.1613 1.2912 0.749 0.048 Uiso 1 1 calc R . . C13 C 0.1441(6) 1.2533(3) 0.6022(6) 0.0404(17) Uani 1 1 d . . . H13 H 0.1359 1.2903 0.5631 0.049 Uiso 1 1 calc R . . C14 C 0.1389(5) 1.1977(3) 0.5476(5) 0.0332(14) Uani 1 1 d . . . H14 H 0.1257 1.1974 0.4715 0.04 Uiso 1 1 calc R . . C15 C 0.1532(5) 1.1423(2) 0.6057(5) 0.0276(13) Uani 1 1 d . . . H15 H 0.1484 1.105 0.5682 0.033 Uiso 1 1 calc R . . C16 C 0.2464(5) 1.0881(2) 0.9436(4) 0.0204(11) Uani 1 1 d . . . C17 C 0.1766(5) 1.0773(2) 0.9953(4) 0.0216(11) Uani 1 1 d . . . H17 H 0.1066 1.0623 0.9537 0.026 Uiso 1 1 calc R . . C18 C 0.2109(5) 1.0888(2) 1.1108(5) 0.0301(14) Uani 1 1 d . . . H18 H 0.1643 1.081 1.1464 0.036 Uiso 1 1 calc R . . C19 C 0.3132(5) 1.1114(2) 1.1705(4) 0.0280(13) Uani 1 1 d . . . H19 H 0.3359 1.1187 1.2472 0.034 Uiso 1 1 calc R . . C20 C 0.3846(5) 1.1237(3) 1.1192(5) 0.0310(14) Uani 1 1 d . . . H20 H 0.4542 1.1391 1.1607 0.037 Uiso 1 1 calc R . . C21 C 0.3496(5) 1.1124(3) 1.0050(5) 0.0294(13) Uani 1 1 d . . . H21 H 0.3956 1.1211 0.969 0.035 Uiso 1 1 calc R . . C22 C 0.2223(4) 0.9251(2) 0.9823(4) 0.0164(10) Uani 1 1 d . . . C23 C 0.1382(5) 0.9327(2) 1.0175(4) 0.0235(12) Uani 1 1 d . . . H23 H 0.0669 0.9369 0.9643 0.028 Uiso 1 1 calc R . . C24 C 0.1594(5) 0.9340(2) 1.1311(5) 0.0288(13) Uani 1 1 d . . . H24 H 0.1023 0.9381 1.1539 0.035 Uiso 1 1 calc R . . C25 C 0.2652(6) 0.9293(3) 1.2103(5) 0.0346(14) Uani 1 1 d . . . H25 H 0.2796 0.931 1.2867 0.042 Uiso 1 1 calc R . . C26 C 0.3489(5) 0.9221(3) 1.1764(5) 0.0356(15) Uani 1 1 d . . . H26 H 0.4203 0.919 1.23 0.043 Uiso 1 1 calc R . . C27 C 0.3284(5) 0.9193(3) 1.0635(4) 0.0295(13) Uani 1 1 d . . . H27 H 0.3858 0.9134 1.0415 0.035 Uiso 1 1 calc R . . C28 C 0.1517(5) 0.8439(2) 0.7917(4) 0.0222(12) Uani 1 1 d . . . C29 C 0.1300(5) 0.8247(3) 0.6820(5) 0.0291(13) Uani 1 1 d . . . H29 H 0.1314 0.8535 0.6294 0.035 Uiso 1 1 calc R . . C30 C 0.1065(6) 0.7641(3) 0.6504(6) 0.0369(15) Uani 1 1 d . . . H30 H 0.0938 0.752 0.5774 0.044 Uiso 1 1 calc R . . C31 C 0.1017(6) 0.7213(3) 0.7265(5) 0.0368(15) Uani 1 1 d . . . H31 H 0.0858 0.6803 0.705 0.044 Uiso 1 1 calc R . . C32 C 0.1205(6) 0.7393(3) 0.8343(6) 0.0430(18) Uani 1 1 d . . . H32 H 0.1162 0.7102 0.8852 0.052 Uiso 1 1 calc R . . C33 C 0.1457(5) 0.7998(3) 0.8681(5) 0.0338(14) Uani 1 1 d . . . H33 H 0.1586 0.8113 0.9415 0.041 Uiso 1 1 calc R . . F1 F -0.2954(3) 0.87734(15) 0.5731(3) 0.0324(8) Uani 1 1 d . . . F2 F -0.4752(3) 0.93791(18) 0.4339(3) 0.0396(9) Uani 1 1 d . . . F3 F -0.4617(3) 1.05814(18) 0.3790(3) 0.0396(9) Uani 1 1 d . . . F4 F -0.2687(3) 1.11828(15) 0.4696(3) 0.0340(8) 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 0.01626(10) 0.01434(10) 0.01340(9) -0.00113(8) 0.00552(6) 0.00030(9) S1 0.0180(7) 0.0197(6) 0.0190(6) 0.0016(5) 0.0055(5) 0.0003(5) S2 0.0230(7) 0.0171(6) 0.0211(6) 0.0012(5) 0.0070(6) 0.0035(5) P1 0.0214(8) 0.0165(6) 0.0157(6) -0.0024(5) 0.0086(6) -0.0002(5) P2 0.0183(7) 0.0155(6) 0.0152(6) -0.0019(5) 0.0070(5) -0.0008(5) C1 0.014(3) 0.031(3) 0.011(2) -0.001(2) 0.005(2) 0.007(2) C2 0.031(3) 0.033(3) 0.015(2) 0.000(2) 0.011(2) 0.001(3) C3 0.018(3) 0.050(4) 0.016(3) -0.003(3) 0.011(2) -0.002(3) C4 0.026(4) 0.051(4) 0.011(2) 0.005(2) 0.008(2) 0.014(3) C5 0.029(3) 0.035(3) 0.020(3) -0.001(2) 0.014(3) 0.004(3) C6 0.024(3) 0.026(3) 0.013(2) -0.005(2) 0.007(2) 0.007(2) C7 0.023(3) 0.020(2) 0.024(3) 0.000(2) 0.011(2) -0.004(2) C8 0.024(3) 0.026(3) 0.025(3) -0.006(2) 0.015(2) -0.001(2) C9 0.019(3) 0.016(2) 0.022(3) -0.001(2) 0.007(2) 0.001(2) C10 0.023(3) 0.018(2) 0.022(3) -0.005(2) 0.007(2) -0.010(2) C11 0.043(4) 0.020(3) 0.022(3) -0.004(2) 0.011(3) -0.001(3) C12 0.055(5) 0.020(3) 0.038(4) -0.008(3) 0.011(3) -0.002(3) C13 0.053(5) 0.019(3) 0.040(4) 0.009(3) 0.010(3) -0.007(3) C14 0.049(4) 0.024(3) 0.023(3) 0.004(2) 0.010(3) -0.001(3) C15 0.040(4) 0.019(3) 0.023(3) -0.004(2) 0.013(3) -0.002(2) C16 0.030(3) 0.014(2) 0.019(2) -0.001(2) 0.012(2) 0.005(2) C17 0.022(3) 0.018(2) 0.026(3) -0.007(2) 0.010(2) -0.003(2) C18 0.047(4) 0.025(3) 0.026(3) 0.005(2) 0.022(3) 0.008(3) C19 0.038(4) 0.023(3) 0.014(2) 0.001(2) 0.002(2) 0.011(3) C20 0.026(3) 0.029(3) 0.028(3) -0.014(2) 0.002(3) 0.002(3) C21 0.022(3) 0.033(3) 0.031(3) -0.009(3) 0.009(3) -0.004(3) C22 0.020(3) 0.013(2) 0.017(2) -0.0037(19) 0.007(2) -0.001(2) C23 0.023(3) 0.022(3) 0.024(3) 0.004(2) 0.008(2) 0.006(2) C24 0.047(4) 0.021(3) 0.027(3) 0.009(2) 0.025(3) 0.017(3) C25 0.050(4) 0.037(3) 0.019(3) 0.000(3) 0.017(3) 0.001(3) C26 0.029(4) 0.051(4) 0.015(3) 0.002(3) -0.003(3) 0.005(3) C27 0.028(3) 0.041(3) 0.020(3) 0.000(2) 0.010(3) -0.001(3) C28 0.023(3) 0.018(2) 0.024(3) -0.003(2) 0.007(2) 0.004(2) C29 0.037(4) 0.027(3) 0.022(3) -0.004(2) 0.012(3) -0.006(3) C30 0.043(4) 0.032(3) 0.037(3) -0.011(3) 0.016(3) -0.004(3) C31 0.043(4) 0.019(3) 0.046(4) -0.010(3) 0.015(3) 0.001(3) C32 0.071(5) 0.013(3) 0.043(4) -0.003(3) 0.021(4) -0.009(3) C33 0.047(4) 0.026(3) 0.027(3) -0.002(2) 0.014(3) -0.001(3) F1 0.031(2) 0.0374(19) 0.0273(17) -0.0030(14) 0.0100(15) -0.0097(16) F2 0.0197(19) 0.070(3) 0.0246(17) -0.0063(17) 0.0041(15) -0.0112(18) F3 0.0212(19) 0.068(3) 0.0267(18) 0.0081(17) 0.0069(15) 0.0177(18) F4 0.038(2) 0.0314(17) 0.0288(17) 0.0065(14) 0.0097(16) 0.0145(16) #----------------------------------------------------------------------------# # 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 P1 2.2638(14) . ? Pt1 P2 2.2691(14) . ? Pt1 S1 2.3031(14) . ? Pt1 S2 2.3044(13) . ? S1 C1 1.747(5) . ? S2 C6 1.727(6) . ? P1 C10 1.812(5) . ? P1 C16 1.831(5) . ? P1 C7 1.834(6) . ? P2 C22 1.813(5) . ? P2 C28 1.818(5) . ? P2 C9 1.819(5) . ? C1 C2 1.405(8) . ? C1 C6 1.414(8) . ? C2 F1 1.355(6) . ? C2 C3 1.360(8) . ? C3 F2 1.357(7) . ? C3 C4 1.367(9) . ? C4 F3 1.358(6) . ? C4 C5 1.369(9) . ? C5 F4 1.363(6) . ? C5 C6 1.400(8) . ? C7 C8 1.519(7) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.536(7) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 C15 1.405(7) . ? C10 C11 1.405(7) . ? C11 C12 1.383(8) . ? C11 H11 0.93 . ? C12 C13 1.371(9) . ? C12 H12 0.93 . ? C13 C14 1.384(8) . ? C13 H13 0.93 . ? C14 C15 1.388(7) . ? C14 H14 0.93 . ? C15 H15 0.93 . ? C16 C17 1.374(8) . ? C16 C21 1.389(8) . ? C17 C18 1.400(7) . ? C17 H17 0.93 . ? C18 C19 1.364(9) . ? C18 H18 0.93 . ? C19 C20 1.394(9) . ? C19 H19 0.93 . ? C20 C21 1.383(8) . ? C20 H20 0.93 . ? C21 H21 0.93 . ? C22 C23 1.385(8) . ? C22 C27 1.391(7) . ? C23 C24 1.384(7) . ? C23 H23 0.93 . ? C24 C25 1.377(9) . ? C24 H24 0.93 . ? C25 C26 1.370(9) . ? C25 H25 0.93 . ? C26 C27 1.379(7) . ? C26 H26 0.93 . ? C27 H27 0.93 . ? C28 C29 1.396(7) . ? C28 C33 1.402(8) . ? C29 C30 1.373(8) . ? C29 H29 0.93 . ? C30 C31 1.374(9) . ? C30 H30 0.93 . ? C31 C32 1.374(9) . ? C31 H31 0.93 . ? C32 C33 1.380(8) . ? C32 H32 0.93 . ? C33 H33 0.93 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 89.88(5) . . ? P1 Pt1 S1 176.43(5) . . ? P2 Pt1 S1 89.80(5) . . ? P1 Pt1 S2 90.75(5) . . ? P2 Pt1 S2 177.45(5) . . ? S1 Pt1 S2 89.73(5) . . ? C1 S1 Pt1 103.15(19) . . ? C6 S2 Pt1 103.26(18) . . ? C10 P1 C16 105.4(2) . . ? C10 P1 C7 101.5(2) . . ? C16 P1 C7 104.5(3) . . ? C10 P1 Pt1 117.41(18) . . ? C16 P1 Pt1 113.37(18) . . ? C7 P1 Pt1 113.14(17) . . ? C22 P2 C28 104.3(2) . . ? C22 P2 C9 106.8(2) . . ? C28 P2 C9 100.5(2) . . ? C22 P2 Pt1 113.51(17) . . ? C28 P2 Pt1 116.48(18) . . ? C9 P2 Pt1 113.89(17) . . ? C2 C1 C6 118.7(5) . . ? C2 C1 S1 119.9(4) . . ? C6 C1 S1 121.3(4) . . ? F1 C2 C3 118.8(5) . . ? F1 C2 C1 119.3(5) . . ? C3 C2 C1 121.9(5) . . ? F2 C3 C2 120.2(6) . . ? F2 C3 C4 119.6(5) . . ? C2 C3 C4 120.2(6) . . ? F3 C4 C3 120.4(6) . . ? F3 C4 C5 120.4(6) . . ? C3 C4 C5 119.2(5) . . ? F4 C5 C4 118.3(5) . . ? F4 C5 C6 118.4(5) . . ? C4 C5 C6 123.3(5) . . ? C5 C6 C1 116.7(5) . . ? C5 C6 S2 120.9(4) . . ? C1 C6 S2 122.4(4) . . ? C8 C7 P1 115.0(4) . . ? C8 C7 H7A 108.5 . . ? P1 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? P1 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 C9 115.9(5) . . ? C7 C8 H8A 108.3 . . ? C9 C8 H8A 108.3 . . ? C7 C8 H8B 108.3 . . ? C9 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C8 C9 P2 117.2(4) . . ? C8 C9 H9A 108 . . ? P2 C9 H9A 108 . . ? C8 C9 H9B 108 . . ? P2 C9 H9B 108 . . ? H9A C9 H9B 107.3 . . ? C15 C10 C11 118.6(5) . . ? C15 C10 P1 117.8(4) . . ? C11 C10 P1 123.6(4) . . ? C12 C11 C10 120.2(5) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C11 120.8(6) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 120.0(5) . . ? C12 C13 H13 120 . . ? C14 C13 H13 120 . . ? C13 C14 C15 120.5(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 119.9(5) . . ? C14 C15 H15 120 . . ? C10 C15 H15 120 . . ? C17 C16 C21 120.1(5) . . ? C17 C16 P1 119.0(4) . . ? C21 C16 P1 121.0(4) . . ? C16 C17 C18 119.8(5) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 119.4(6) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 121.5(5) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 118.5(6) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C20 C21 C16 120.6(6) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C23 C22 C27 118.6(5) . . ? C23 C22 P2 118.9(4) . . ? C27 C22 P2 122.5(4) . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.0(6) . . ? C25 C24 H24 120 . . ? C23 C24 H24 120 . . ? C26 C25 C24 119.8(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.6(6) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.3(6) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C29 C28 C33 118.1(5) . . ? C29 C28 P2 119.8(4) . . ? C33 C28 P2 122.1(4) . . ? C30 C29 C28 121.1(6) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 120.1(6) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C32 119.9(5) . . ? C30 C31 H31 120 . . ? C32 C31 H31 120 . . ? C31 C32 C33 120.8(6) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C28 119.9(5) . . ? C32 C33 H33 120 . . ? C28 C33 H33 120 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 S1 C1 -178.90(18) . . . . ? S2 Pt1 S1 C1 -1.40(18) . . . . ? P1 Pt1 S2 C6 -176.81(18) . . . . ? S1 Pt1 S2 C6 -0.35(18) . . . . ? P2 Pt1 P1 C10 165.1(2) . . . . ? S2 Pt1 P1 C10 -12.4(2) . . . . ? P2 Pt1 P1 C16 -71.48(19) . . . . ? S2 Pt1 P1 C16 110.99(19) . . . . ? P2 Pt1 P1 C7 47.30(19) . . . . ? S2 Pt1 P1 C7 -130.23(19) . . . . ? P1 Pt1 P2 C22 77.64(19) . . . . ? S1 Pt1 P2 C22 -98.81(19) . . . . ? P1 Pt1 P2 C28 -161.3(2) . . . . ? S1 Pt1 P2 C28 22.3(2) . . . . ? P1 Pt1 P2 C9 -44.93(18) . . . . ? S1 Pt1 P2 C9 138.62(18) . . . . ? Pt1 S1 C1 C2 -179.4(4) . . . . ? Pt1 S1 C1 C6 3.6(4) . . . . ? C6 C1 C2 F1 178.9(4) . . . . ? S1 C1 C2 F1 1.8(7) . . . . ? C6 C1 C2 C3 -1.0(8) . . . . ? S1 C1 C2 C3 -178.1(4) . . . . ? F1 C2 C3 F2 -1.0(8) . . . . ? C1 C2 C3 F2 178.9(5) . . . . ? F1 C2 C3 C4 -178.1(5) . . . . ? C1 C2 C3 C4 1.8(8) . . . . ? F2 C3 C4 F3 0.7(8) . . . . ? C2 C3 C4 F3 177.8(5) . . . . ? F2 C3 C4 C5 -179.2(5) . . . . ? C2 C3 C4 C5 -2.1(8) . . . . ? F3 C4 C5 F4 1.5(8) . . . . ? C3 C4 C5 F4 -178.6(5) . . . . ? F3 C4 C5 C6 -178.1(5) . . . . ? C3 C4 C5 C6 1.8(8) . . . . ? F4 C5 C6 C1 179.3(4) . . . . ? C4 C5 C6 C1 -1.0(8) . . . . ? F4 C5 C6 S2 1.5(7) . . . . ? C4 C5 C6 S2 -178.8(4) . . . . ? C2 C1 C6 C5 0.6(7) . . . . ? S1 C1 C6 C5 177.6(4) . . . . ? C2 C1 C6 S2 178.4(4) . . . . ? S1 C1 C6 S2 -4.6(6) . . . . ? Pt1 S2 C6 C5 -179.6(4) . . . . ? Pt1 S2 C6 C1 2.8(4) . . . . ? C10 P1 C7 C8 170.3(4) . . . . ? C16 P1 C7 C8 60.8(4) . . . . ? Pt1 P1 C7 C8 -63.0(4) . . . . ? P1 C7 C8 C9 65.6(5) . . . . ? C7 C8 C9 P2 -63.3(6) . . . . ? C22 P2 C9 C8 -68.7(4) . . . . ? C28 P2 C9 C8 -177.2(4) . . . . ? Pt1 P2 C9 C8 57.5(4) . . . . ? C16 P1 C10 C15 171.7(5) . . . . ? C7 P1 C10 C15 63.0(5) . . . . ? Pt1 P1 C10 C15 -60.9(5) . . . . ? C16 P1 C10 C11 -5.5(6) . . . . ? C7 P1 C10 C11 -114.3(5) . . . . ? Pt1 P1 C10 C11 121.8(5) . . . . ? C15 C10 C11 C12 0.4(9) . . . . ? P1 C10 C11 C12 177.7(5) . . . . ? C10 C11 C12 C13 -2.8(11) . . . . ? C11 C12 C13 C14 3.2(11) . . . . ? C12 C13 C14 C15 -1.3(11) . . . . ? C13 C14 C15 C10 -1.1(10) . . . . ? C11 C10 C15 C14 1.5(9) . . . . ? P1 C10 C15 C14 -175.9(5) . . . . ? C10 P1 C16 C17 106.9(4) . . . . ? C7 P1 C16 C17 -146.5(4) . . . . ? Pt1 P1 C16 C17 -22.8(5) . . . . ? C10 P1 C16 C21 -74.0(5) . . . . ? C7 P1 C16 C21 32.6(5) . . . . ? Pt1 P1 C16 C21 156.2(4) . . . . ? C21 C16 C17 C18 -2.1(8) . . . . ? P1 C16 C17 C18 176.9(4) . . . . ? C16 C17 C18 C19 0.8(8) . . . . ? C17 C18 C19 C20 0.3(8) . . . . ? C18 C19 C20 C21 -0.1(8) . . . . ? C19 C20 C21 C16 -1.3(9) . . . . ? C17 C16 C21 C20 2.4(8) . . . . ? P1 C16 C21 C20 -176.6(4) . . . . ? C28 P2 C22 C23 -84.4(4) . . . . ? C9 P2 C22 C23 169.7(4) . . . . ? Pt1 P2 C22 C23 43.4(4) . . . . ? C28 P2 C22 C27 95.9(5) . . . . ? C9 P2 C22 C27 -10.0(5) . . . . ? Pt1 P2 C22 C27 -136.4(4) . . . . ? C27 C22 C23 C24 -0.4(8) . . . . ? P2 C22 C23 C24 179.9(4) . . . . ? C22 C23 C24 C25 1.6(8) . . . . ? C23 C24 C25 C26 -1.3(9) . . . . ? C24 C25 C26 C27 -0.2(10) . . . . ? C25 C26 C27 C22 1.4(10) . . . . ? C23 C22 C27 C26 -1.1(8) . . . . ? P2 C22 C27 C26 178.6(5) . . . . ? C22 P2 C28 C29 -174.8(5) . . . . ? C9 P2 C28 C29 -64.2(5) . . . . ? Pt1 P2 C28 C29 59.3(5) . . . . ? C22 P2 C28 C33 3.5(6) . . . . ? C9 P2 C28 C33 114.1(5) . . . . ? Pt1 P2 C28 C33 -122.4(5) . . . . ? C33 C28 C29 C30 -1.9(9) . . . . ? P2 C28 C29 C30 176.5(5) . . . . ? C28 C29 C30 C31 1.4(10) . . . . ? C29 C30 C31 C32 0.0(11) . . . . ? C30 C31 C32 C33 -0.9(12) . . . . ? C31 C32 C33 C28 0.4(11) . . . . ? C29 C28 C33 C32 1.0(10) . . . . ? P2 C28 C33 C32 -177.3(5) . . . . ? # Attachment 'cif717504.txt' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-03-18 at 13:27:58 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : f:\xprogs\wingx\files\archive.reqdat # CIF files read : ub01nf1n cifdep_iv #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_IV _database_code_depnum_ccdc_archive 'CCDC 717504' _audit_creation_date 2009-03-18T13:27:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C59 H52 F4 N P4 Pt2 S2' _chemical_formula_sum 'C59 H52 F4 N P4 Pt2 S2' _chemical_formula_weight 1429.2 _chemical_melting_point 0 _chemical_compound_source 'synthesis as described' _chemical_enantioexcess_bulk 0 _chemical_enantioexcess_crystal 0 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' _space_group_IT_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7777(5) _cell_length_b 19.9091(6) _cell_length_c 24.4992(9) _cell_angle_alpha 90 _cell_angle_beta 95.906(2) _cell_angle_gamma 90 _cell_volume 6199.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100.00(10) _cell_measurement_reflns_used 3506 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 20.84 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2788 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 0.910 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100.00(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_unetI/netI 0.0749 _diffrn_reflns_number 7575 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 22.02 _diffrn_reflns_theta_full 22.02 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 7575 _reflns_number_gt 5380 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SADABS/XPREP' _computing_structure_solution 'DIRDIF2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7575 _refine_ls_number_parameters 649 _refine_ls_number_restraints 696 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.678 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.147 #----------------------------------------------------------------------------# # 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 0.52936(3) 0.050715(16) 0.142113(14) 0.01535(11) Uani 1 1 d . . . Pt2 Pt 0.51707(3) 0.217322(17) 0.115503(14) 0.01656(11) Uani 1 1 d . . . S1 S 0.64763(17) 0.13932(10) 0.14393(9) 0.0187(6) Uani 1 1 d . . . S2 S 0.46078(17) 0.11765(10) 0.06664(9) 0.0174(5) Uani 1 1 d . . . C1 C 0.3219(7) 0.1171(4) 0.0523(3) 0.0181(19) Uani 1 1 d U . . C2 C 0.2758(7) 0.1043(4) -0.0005(4) 0.0238(19) Uani 1 1 d U . . C3 C 0.1683(8) 0.1077(5) -0.0104(4) 0.029(2) Uani 1 1 d U . . N4 N 0.1036(6) 0.1207(3) 0.0256(3) 0.0267(18) Uani 1 1 d U . . C5 C 0.1451(7) 0.1315(4) 0.0756(4) 0.026(2) Uani 1 1 d U . . C6 C 0.2513(7) 0.1287(4) 0.0912(4) 0.0230(19) Uani 1 1 d U . . F7 F 0.3358(4) 0.0910(2) -0.04082(19) 0.0290(13) Uani 1 1 d U . . F8 F 0.1261(4) 0.0955(3) -0.0627(2) 0.0380(14) Uani 1 1 d U . . F9 F 0.0792(4) 0.1434(2) 0.1130(2) 0.0332(13) Uani 1 1 d U . . F10 F 0.2870(4) 0.1353(2) 0.1446(2) 0.0274(13) Uani 1 1 d U . . P1 P 0.40097(19) 0.29590(11) 0.07619(10) 0.0235(6) Uani 1 1 d . . . P2 P 0.59833(19) 0.29243(11) 0.17395(10) 0.0219(6) Uani 1 1 d . . . C11 C 0.4673(7) 0.3748(4) 0.0669(4) 0.035(3) Uani 1 1 d . . . H11A H 0.5266 0.3667 0.046 0.042 Uiso 1 1 calc R . . H11B H 0.4192 0.4048 0.0456 0.042 Uiso 1 1 calc R . . C12 C 0.5074(7) 0.4097(4) 0.1215(4) 0.032(3) Uani 1 1 d . . . H12A H 0.4534 0.407 0.1465 0.038 Uiso 1 1 calc R . . H12B H 0.5197 0.4569 0.1145 0.038 Uiso 1 1 calc R . . C13 C 0.6105(7) 0.3779(4) 0.1492(4) 0.032(3) Uani 1 1 d . . . H13A H 0.6369 0.406 0.18 0.039 Uiso 1 1 calc R . . H13B H 0.6626 0.3784 0.1231 0.039 Uiso 1 1 calc R . . C14 C 0.2408(8) 0.2713(4) -0.0101(4) 0.032(2) Uani 1 1 d U . . H14 H 0.1915 0.28 0.0144 0.038 Uiso 1 1 calc R . . C15 C 0.2091(9) 0.2550(4) -0.0651(4) 0.042(2) Uani 1 1 d U . . H15 H 0.1376 0.2521 -0.0766 0.05 Uiso 1 1 calc R . . C16 C 0.2797(9) 0.2432(5) -0.1021(5) 0.047(3) Uani 1 1 d U . . H16 H 0.2561 0.2326 -0.1382 0.056 Uiso 1 1 calc R . . C17 C 0.3877(9) 0.2471(5) -0.0856(4) 0.043(2) Uani 1 1 d U . . H17 H 0.4362 0.2398 -0.1108 0.052 Uiso 1 1 calc R . . C18 C 0.4220(9) 0.2620(4) -0.0313(4) 0.039(2) Uani 1 1 d U . . H18 H 0.4937 0.2639 -0.0202 0.047 Uiso 1 1 calc R . . C19 C 0.3498(7) 0.2742(4) 0.0070(4) 0.026(2) Uani 1 1 d U . . C20 C 0.2550(7) 0.2868(4) 0.1536(4) 0.027(2) Uani 1 1 d U . . H20 H 0.2951 0.2509 0.1682 0.033 Uiso 1 1 calc R . . C21 C 0.1636(7) 0.3057(5) 0.1772(4) 0.032(2) Uani 1 1 d U . . H21 H 0.1436 0.283 0.2077 0.038 Uiso 1 1 calc R . . C22 C 0.1049(8) 0.3577(5) 0.1547(4) 0.037(2) Uani 1 1 d U . . H22 H 0.0432 0.3698 0.1693 0.044 Uiso 1 1 calc R . . C23 C 0.1357(8) 0.3923(5) 0.1108(4) 0.038(2) Uani 1 1 d U . . H23 H 0.0946 0.4278 0.0964 0.046 Uiso 1 1 calc R . . C24 C 0.2243(7) 0.3763(4) 0.0877(4) 0.030(2) Uani 1 1 d U . . H24 H 0.2446 0.4013 0.0585 0.036 Uiso 1 1 calc R . . C25 C 0.2859(7) 0.3210(4) 0.1088(4) 0.024(2) Uani 1 1 d U . . C26 C 0.5523(7) 0.3491(4) 0.2743(4) 0.031(2) Uani 1 1 d U . . H26 H 0.5957 0.3846 0.2666 0.037 Uiso 1 1 calc R . . C27 C 0.5050(8) 0.3496(5) 0.3231(4) 0.034(2) Uani 1 1 d U . . H27 H 0.5182 0.3842 0.3484 0.04 Uiso 1 1 calc R . . C28 C 0.4389(8) 0.2979(5) 0.3331(4) 0.038(2) Uani 1 1 d U . . H28 H 0.4049 0.2983 0.3649 0.045 Uiso 1 1 calc R . . C29 C 0.4220(7) 0.2456(5) 0.2969(4) 0.030(2) Uani 1 1 d U . . H29 H 0.3785 0.2102 0.3047 0.036 Uiso 1 1 calc R . . C30 C 0.4685(7) 0.2457(4) 0.2499(3) 0.022(2) Uani 1 1 d U . . H30 H 0.4548 0.2102 0.2255 0.027 Uiso 1 1 calc R . . C31 C 0.5359(7) 0.2963(4) 0.2364(3) 0.019(2) Uani 1 1 d U . . C32 C 0.7597(7) 0.2363(4) 0.2451(4) 0.025(2) Uani 1 1 d U . . H32 H 0.7096 0.2335 0.2699 0.03 Uiso 1 1 calc R . . C33 C 0.8581(7) 0.2079(5) 0.2586(4) 0.036(2) Uani 1 1 d U . . H33 H 0.875 0.1868 0.2922 0.043 Uiso 1 1 calc R . . C34 C 0.9316(8) 0.2121(5) 0.2195(4) 0.037(2) Uani 1 1 d U . . H34 H 0.9978 0.193 0.2276 0.044 Uiso 1 1 calc R . . C35 C 0.9081(8) 0.2437(5) 0.1698(4) 0.039(2) Uani 1 1 d U . . H35 H 0.9574 0.2458 0.1445 0.047 Uiso 1 1 calc R . . C36 C 0.8069(7) 0.2732(4) 0.1581(4) 0.032(2) Uani 1 1 d U . . H36 H 0.7901 0.2955 0.125 0.039 Uiso 1 1 calc R . . C37 C 0.7342(7) 0.2688(4) 0.1952(4) 0.022(2) Uani 1 1 d U . . P3 P 0.40333(18) -0.03017(11) 0.14544(9) 0.0171(6) Uani 1 1 d . . . P4 P 0.63815(19) -0.00101(11) 0.20720(10) 0.0204(6) Uani 1 1 d . . . C38 C 0.4539(7) -0.1157(4) 0.1513(3) 0.020(2) Uani 1 1 d . . . H38A H 0.3952 -0.1464 0.1528 0.023 Uiso 1 1 calc R . . H38B H 0.4876 -0.1263 0.1186 0.023 Uiso 1 1 calc R . . C39 C 0.5338(7) -0.1275(4) 0.2025(4) 0.025(2) Uani 1 1 d . . . H39A H 0.5026 -0.1125 0.2348 0.029 Uiso 1 1 calc R . . H39B H 0.5468 -0.1754 0.2064 0.029 Uiso 1 1 calc R . . C40 C 0.6384(7) -0.0919(4) 0.2004(4) 0.020(2) Uani 1 1 d . . . H40A H 0.6648 -0.103 0.1658 0.025 Uiso 1 1 calc R . . H40B H 0.6877 -0.11 0.2294 0.025 Uiso 1 1 calc R . . C41 C 0.3469(7) -0.0563(4) 0.0361(3) 0.022(2) Uani 1 1 d U . . H41 H 0.4191 -0.0571 0.034 0.027 Uiso 1 1 calc R . . C42 C 0.2797(7) -0.0706(4) -0.0095(4) 0.027(2) Uani 1 1 d U . . H42 H 0.3065 -0.0823 -0.0421 0.033 Uiso 1 1 calc R . . C43 C 0.1718(7) -0.0679(4) -0.0073(4) 0.029(2) Uani 1 1 d U . . H43 H 0.1263 -0.0775 -0.0384 0.035 Uiso 1 1 calc R . . C44 C 0.1321(7) -0.0509(4) 0.0409(4) 0.027(2) Uani 1 1 d U . . H44 H 0.0597 -0.0491 0.0423 0.032 Uiso 1 1 calc R . . C45 C 0.1990(7) -0.0365(4) 0.0874(3) 0.019(2) Uani 1 1 d U . . H45 H 0.1714 -0.0242 0.1197 0.023 Uiso 1 1 calc R . . C46 C 0.3079(7) -0.0403(4) 0.0861(3) 0.0180(19) Uani 1 1 d U . . C47 C 0.2582(7) -0.0715(4) 0.2176(4) 0.022(2) Uani 1 1 d U . . H47 H 0.2482 -0.11 0.1963 0.027 Uiso 1 1 calc R . . C48 C 0.2037(7) -0.0626(4) 0.2628(4) 0.025(2) Uani 1 1 d U . . H48 H 0.1557 -0.0952 0.2712 0.03 Uiso 1 1 calc R . . C49 C 0.2190(7) -0.0062(4) 0.2961(4) 0.026(2) Uani 1 1 d U . . H49 H 0.1819 -0.0012 0.3266 0.032 Uiso 1 1 calc R . . C50 C 0.2878(7) 0.0412(4) 0.2838(4) 0.026(2) Uani 1 1 d U . . H50 H 0.3 0.0781 0.3068 0.032 Uiso 1 1 calc R . . C51 C 0.3416(7) 0.0359(4) 0.2370(3) 0.025(2) Uani 1 1 d U . . H51 H 0.3854 0.0705 0.2279 0.029 Uiso 1 1 calc R . . C52 C 0.3294(7) -0.0212(4) 0.2041(3) 0.020(2) Uani 1 1 d U . . C53 C 0.8427(7) 0.0307(4) 0.2535(4) 0.021(2) Uani 1 1 d U . . H53 H 0.8136 0.0327 0.2867 0.025 Uiso 1 1 calc R . . C54 C 0.9491(7) 0.0402(4) 0.2528(4) 0.022(2) Uani 1 1 d U . . H54 H 0.9914 0.0485 0.2853 0.027 Uiso 1 1 calc R . . C55 C 0.9927(7) 0.0373(4) 0.2037(4) 0.023(2) Uani 1 1 d U . . H55 H 1.0645 0.0443 0.2026 0.028 Uiso 1 1 calc R . . C56 C 0.9282(7) 0.0240(4) 0.1558(4) 0.026(2) Uani 1 1 d U . . H56 H 0.9577 0.0216 0.1227 0.031 Uiso 1 1 calc R . . C57 C 0.8216(7) 0.0142(4) 0.1562(4) 0.023(2) Uani 1 1 d U . . H57 H 0.7794 0.0052 0.1238 0.027 Uiso 1 1 calc R . . C58 C 0.7780(6) 0.0182(4) 0.2058(3) 0.0157(19) Uani 1 1 d U . . C59 C 0.6222(7) -0.0303(5) 0.3188(4) 0.028(2) Uani 1 1 d U . . H59 H 0.6332 -0.0752 0.3107 0.034 Uiso 1 1 calc R . . C60 C 0.6133(7) -0.0110(5) 0.3727(4) 0.034(2) Uani 1 1 d U . . H60 H 0.6228 -0.0428 0.4007 0.041 Uiso 1 1 calc R . . C61 C 0.5910(8) 0.0529(5) 0.3849(4) 0.038(2) Uani 1 1 d U . . H61 H 0.5816 0.0647 0.4208 0.046 Uiso 1 1 calc R . . C62 C 0.5821(7) 0.1013(5) 0.3438(4) 0.033(2) Uani 1 1 d U . . H62 H 0.5675 0.1456 0.3525 0.039 Uiso 1 1 calc R . . C63 C 0.5945(7) 0.0843(5) 0.2901(4) 0.029(2) Uani 1 1 d U . . H63 H 0.5894 0.1172 0.263 0.035 Uiso 1 1 calc R . . C64 C 0.6148(7) 0.0180(4) 0.2766(3) 0.021(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0146(2) 0.01418(19) 0.0168(2) 0.00019(16) -0.00062(15) -0.00024(16) Pt2 0.0170(2) 0.01476(19) 0.0176(2) -0.00108(16) 0.00019(15) 0.00072(17) S1 0.0173(14) 0.0144(12) 0.0241(15) -0.0002(10) 0.0002(11) -0.0012(10) S2 0.0176(14) 0.0167(13) 0.0177(14) -0.0017(10) 0.0006(11) 0.0013(10) C1 0.018(4) 0.013(4) 0.023(4) -0.004(4) -0.002(4) -0.001(3) C2 0.023(4) 0.028(4) 0.020(4) 0.000(3) -0.001(4) 0.001(3) C3 0.027(4) 0.033(4) 0.026(4) -0.002(4) -0.009(4) 0.000(4) N4 0.020(4) 0.025(4) 0.034(4) 0.001(3) -0.005(3) 0.003(3) C5 0.022(4) 0.022(4) 0.035(4) -0.001(3) 0.004(4) 0.001(4) C6 0.021(4) 0.019(4) 0.029(4) -0.001(3) 0.002(4) 0.002(3) F7 0.029(3) 0.040(3) 0.017(3) -0.002(2) -0.003(2) 0.003(2) F8 0.035(3) 0.046(3) 0.030(3) -0.001(3) -0.009(3) -0.002(3) F9 0.025(3) 0.034(3) 0.043(3) -0.002(2) 0.011(3) 0.000(2) F10 0.024(3) 0.031(3) 0.028(3) -0.004(2) 0.007(2) 0.000(2) P1 0.0245(16) 0.0212(14) 0.0241(15) -0.0010(11) -0.0002(12) 0.0052(11) P2 0.0206(15) 0.0167(13) 0.0279(15) -0.0051(11) 0.0008(12) -0.0002(11) C11 0.034(7) 0.019(5) 0.053(8) -0.004(5) 0.010(6) -0.001(5) C12 0.042(7) 0.010(5) 0.043(7) -0.004(5) 0.004(5) -0.002(5) C13 0.033(7) 0.018(6) 0.045(7) -0.008(5) -0.001(5) 0.000(5) C14 0.042(5) 0.022(4) 0.030(4) 0.005(4) -0.002(4) 0.004(4) C15 0.053(5) 0.029(4) 0.041(5) 0.009(4) -0.011(4) 0.006(4) C16 0.063(5) 0.036(5) 0.039(5) 0.004(4) -0.004(4) 0.006(4) C17 0.059(5) 0.034(4) 0.036(5) -0.009(4) 0.003(4) 0.010(4) C18 0.050(5) 0.032(4) 0.034(5) 0.001(4) 0.000(4) 0.006(4) C19 0.032(4) 0.023(4) 0.023(4) 0.007(4) -0.001(4) 0.008(4) C20 0.029(4) 0.026(4) 0.025(4) -0.004(4) -0.003(4) -0.010(4) C21 0.026(5) 0.035(4) 0.034(4) -0.006(4) 0.006(4) -0.004(4) C22 0.029(5) 0.040(5) 0.041(5) -0.012(4) 0.003(4) -0.001(4) C23 0.034(5) 0.037(4) 0.042(5) -0.011(4) -0.005(4) 0.015(4) C24 0.030(4) 0.029(4) 0.029(4) -0.005(4) 0.001(4) 0.010(4) C25 0.024(4) 0.024(4) 0.022(4) -0.003(4) -0.002(4) -0.001(4) C26 0.031(5) 0.027(4) 0.032(5) -0.002(4) -0.011(4) 0.004(4) C27 0.036(5) 0.032(4) 0.030(5) -0.013(4) -0.007(4) 0.009(4) C28 0.038(5) 0.044(5) 0.030(4) 0.001(4) 0.002(4) 0.005(4) C29 0.034(5) 0.030(4) 0.026(4) -0.002(4) 0.003(4) 0.004(4) C30 0.029(4) 0.022(4) 0.015(4) -0.007(4) 0.000(4) 0.005(4) C31 0.024(4) 0.014(4) 0.019(4) 0.001(3) -0.004(4) 0.003(3) C32 0.023(4) 0.020(4) 0.031(4) -0.013(4) -0.002(4) -0.003(4) C33 0.030(5) 0.031(4) 0.043(5) -0.013(4) -0.006(4) 0.000(4) C34 0.025(4) 0.029(4) 0.054(5) -0.015(4) -0.005(4) -0.001(4) C35 0.028(5) 0.036(4) 0.054(5) -0.011(4) 0.006(4) -0.007(4) C36 0.028(5) 0.026(4) 0.042(5) -0.005(4) 0.000(4) -0.004(4) C37 0.021(4) 0.015(4) 0.029(4) -0.010(4) -0.003(4) -0.002(3) P3 0.0144(14) 0.0152(13) 0.0210(14) -0.0002(10) -0.0013(11) 0.0000(10) P4 0.0207(15) 0.0196(14) 0.0206(15) 0.0007(11) 0.0007(12) -0.0017(11) C38 0.017(6) 0.017(5) 0.024(6) 0.007(4) 0.002(4) 0.003(4) C39 0.031(6) 0.018(5) 0.023(6) 0.011(4) -0.005(5) -0.002(5) C40 0.021(6) 0.011(5) 0.028(6) 0.010(4) 0.001(5) 0.002(4) C41 0.020(4) 0.021(4) 0.025(4) 0.004(4) 0.001(4) -0.001(4) C42 0.029(4) 0.030(4) 0.023(4) -0.002(4) 0.003(4) 0.001(4) C43 0.033(4) 0.028(4) 0.026(4) -0.005(4) -0.001(4) -0.005(4) C44 0.025(4) 0.033(4) 0.024(4) -0.001(4) 0.002(4) -0.002(4) C45 0.024(4) 0.019(4) 0.016(4) -0.001(3) 0.006(4) -0.003(3) C46 0.020(4) 0.017(4) 0.017(4) 0.001(3) 0.000(3) -0.001(3) C47 0.017(4) 0.026(4) 0.024(4) 0.004(4) 0.000(4) 0.002(3) C48 0.023(4) 0.027(4) 0.025(4) 0.014(4) 0.001(4) -0.003(4) C49 0.025(4) 0.031(4) 0.024(4) 0.009(4) 0.006(4) 0.004(4) C50 0.026(4) 0.029(4) 0.025(4) 0.000(4) 0.005(4) 0.003(4) C51 0.026(4) 0.025(4) 0.022(4) 0.007(4) -0.001(4) 0.000(4) C52 0.021(4) 0.023(4) 0.016(4) 0.007(3) -0.006(3) 0.000(4) C53 0.024(4) 0.012(4) 0.025(4) 0.005(3) -0.005(4) -0.001(3) C54 0.018(4) 0.018(4) 0.029(4) -0.003(4) -0.006(4) -0.006(3) C55 0.020(4) 0.021(4) 0.030(4) 0.010(4) 0.003(4) 0.002(3) C56 0.025(4) 0.026(4) 0.026(4) 0.003(4) 0.002(4) 0.008(4) C57 0.020(4) 0.022(4) 0.026(4) 0.005(4) -0.005(4) 0.000(4) C58 0.015(4) 0.012(4) 0.019(4) 0.004(3) -0.002(3) 0.005(3) C59 0.026(4) 0.033(4) 0.026(4) 0.003(4) 0.001(4) -0.005(4) C60 0.032(5) 0.045(5) 0.027(4) 0.006(4) 0.004(4) -0.004(4) C61 0.037(5) 0.047(5) 0.031(5) -0.009(4) 0.002(4) -0.001(4) C62 0.031(4) 0.038(4) 0.027(4) -0.010(4) -0.005(4) 0.008(4) C63 0.024(4) 0.038(4) 0.024(4) 0.002(4) -0.002(4) 0.003(4) C64 0.017(4) 0.025(4) 0.019(4) 0.000(4) -0.004(3) 0.000(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P4 2.254(2) . ? Pt1 P3 2.285(2) . ? Pt1 S1 2.320(2) . ? Pt1 S2 2.373(2) . ? Pt2 P2 2.249(2) . ? Pt2 P1 2.298(2) . ? Pt2 S1 2.333(2) . ? Pt2 S2 2.390(2) . ? S2 C1 1.773(9) . ? C1 C2 1.390(11) . ? C1 C6 1.397(12) . ? C2 F7 1.336(9) . ? C2 C3 1.372(12) . ? C3 N4 1.295(11) . ? C3 F8 1.360(10) . ? N4 C5 1.301(11) . ? C5 F9 1.328(10) . ? C5 C6 1.373(12) . ? C6 F10 1.349(10) . ? P1 C19 1.805(9) . ? P1 C11 1.811(8) . ? P1 C25 1.814(9) . ? P2 C31 1.798(9) . ? P2 C13 1.819(9) . ? P2 C37 1.822(9) . ? C11 C12 1.547(12) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 C13 1.554(12) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C14 C15 1.405(13) . ? C14 C19 1.414(12) . ? C14 H14 0.93 . ? C15 C16 1.363(14) . ? C15 H15 0.93 . ? C16 C17 1.400(14) . ? C16 H16 0.93 . ? C17 C18 1.390(13) . ? C17 H17 0.93 . ? C18 C19 1.402(13) . ? C18 H18 0.93 . ? C20 C25 1.383(12) . ? C20 C21 1.408(12) . ? C20 H20 0.93 . ? C21 C22 1.361(12) . ? C21 H21 0.93 . ? C22 C23 1.369(13) . ? C22 H22 0.93 . ? C23 C24 1.354(12) . ? C23 H23 0.93 . ? C24 C25 1.419(12) . ? C24 H24 0.93 . ? C26 C27 1.396(13) . ? C26 C31 1.404(11) . ? C26 H26 0.93 . ? C27 C28 1.369(12) . ? C27 H27 0.93 . ? C28 C29 1.371(12) . ? C28 H28 0.93 . ? C29 C30 1.348(12) . ? C29 H29 0.93 . ? C30 C31 1.387(11) . ? C30 H30 0.93 . ? C32 C33 1.387(12) . ? C32 C37 1.391(12) . ? C32 H32 0.93 . ? C33 C34 1.411(13) . ? C33 H33 0.93 . ? C34 C35 1.376(13) . ? C34 H34 0.93 . ? C35 C36 1.422(12) . ? C35 H35 0.93 . ? C36 C37 1.369(12) . ? C36 H36 0.93 . ? P3 C52 1.807(9) . ? P3 C46 1.810(8) . ? P3 C38 1.823(8) . ? P4 C64 1.796(9) . ? P4 C40 1.817(8) . ? P4 C58 1.832(8) . ? C38 C39 1.551(11) . ? C38 H38A 0.97 . ? C38 H38B 0.97 . ? C39 C40 1.517(11) . ? C39 H39A 0.97 . ? C39 H39B 0.97 . ? C40 H40A 0.97 . ? C40 H40B 0.97 . ? C41 C42 1.367(12) . ? C41 C46 1.405(11) . ? C41 H41 0.93 . ? C42 C43 1.387(12) . ? C42 H42 0.93 . ? C43 C44 1.376(12) . ? C43 H43 0.93 . ? C44 C45 1.382(11) . ? C44 H44 0.93 . ? C45 C46 1.398(11) . ? C45 H45 0.93 . ? C47 C48 1.378(11) . ? C47 C52 1.414(11) . ? C47 H47 0.93 . ? C48 C49 1.391(12) . ? C48 H48 0.93 . ? C49 C50 1.345(11) . ? C49 H49 0.93 . ? C50 C51 1.400(12) . ? C50 H50 0.93 . ? C51 C52 1.394(11) . ? C51 H51 0.93 . ? C53 C54 1.375(11) . ? C53 C58 1.382(11) . ? C53 H53 0.93 . ? C54 C55 1.380(12) . ? C54 H54 0.93 . ? C55 C56 1.387(12) . ? C55 H55 0.93 . ? C56 C57 1.377(11) . ? C56 H56 0.93 . ? C57 C58 1.390(11) . ? C57 H57 0.93 . ? C59 C60 1.391(12) . ? C59 C64 1.408(11) . ? C59 H59 0.93 . ? C60 C61 1.345(12) . ? C60 H60 0.93 . ? C61 C62 1.391(12) . ? C61 H61 0.93 . ? C62 C63 1.383(12) . ? C62 H62 0.93 . ? C63 C64 1.393(11) . ? C63 H63 0.93 . ? 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 P4 Pt1 P3 92.20(8) . . ? P4 Pt1 S1 88.89(8) . . ? P3 Pt1 S1 174.39(8) . . ? P4 Pt1 S2 163.63(8) . . ? P3 Pt1 S2 102.62(8) . . ? S1 Pt1 S2 77.03(8) . . ? P2 Pt2 P1 92.87(8) . . ? P2 Pt2 S1 89.05(8) . . ? P1 Pt2 S1 171.62(8) . . ? P2 Pt2 S2 165.11(8) . . ? P1 Pt2 S2 101.96(8) . . ? S1 Pt2 S2 76.46(7) . . ? Pt1 S1 Pt2 93.21(8) . . ? C1 S2 Pt1 115.6(3) . . ? C1 S2 Pt2 110.4(3) . . ? Pt1 S2 Pt2 90.46(8) . . ? C2 C1 C6 115.1(8) . . ? C2 C1 S2 120.4(7) . . ? C6 C1 S2 124.6(7) . . ? F7 C2 C3 121.3(8) . . ? F7 C2 C1 120.2(8) . . ? C3 C2 C1 118.4(8) . . ? N4 C3 F8 117.3(8) . . ? N4 C3 C2 126.0(9) . . ? F8 C3 C2 116.7(9) . . ? C3 N4 C5 116.6(8) . . ? N4 C5 F9 117.0(8) . . ? N4 C5 C6 123.4(9) . . ? F9 C5 C6 119.6(9) . . ? F10 C6 C5 119.5(8) . . ? F10 C6 C1 120.0(8) . . ? C5 C6 C1 120.4(9) . . ? C19 P1 C11 102.6(4) . . ? C19 P1 C25 104.3(4) . . ? C11 P1 C25 103.2(4) . . ? C19 P1 Pt2 112.7(3) . . ? C11 P1 Pt2 110.7(3) . . ? C25 P1 Pt2 121.4(3) . . ? C31 P2 C13 107.7(4) . . ? C31 P2 C37 105.1(4) . . ? C13 P2 C37 103.0(4) . . ? C31 P2 Pt2 110.7(3) . . ? C13 P2 Pt2 117.4(3) . . ? C37 P2 Pt2 112.0(3) . . ? C12 C11 P1 113.5(7) . . ? C12 C11 H11A 108.9 . . ? P1 C11 H11A 108.9 . . ? C12 C11 H11B 108.9 . . ? P1 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 C13 112.7(7) . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C12 C13 P2 115.4(6) . . ? C12 C13 H13A 108.4 . . ? P2 C13 H13A 108.4 . . ? C12 C13 H13B 108.4 . . ? P2 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C19 118.2(9) . . ? C15 C14 H14 120.9 . . ? C19 C14 H14 120.9 . . ? C16 C15 C14 122.2(11) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 119.9(11) . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C18 C17 C16 119.5(10) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 120.9(10) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C14 119.3(9) . . ? C18 C19 P1 118.1(7) . . ? C14 C19 P1 122.6(7) . . ? C25 C20 C21 120.8(9) . . ? C25 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 118.8(9) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 120.6(10) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 122.1(10) . . ? C24 C23 H23 119 . . ? C22 C23 H23 119 . . ? C23 C24 C25 119.1(9) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C20 C25 C24 118.5(8) . . ? C20 C25 P1 121.6(7) . . ? C24 C25 P1 119.9(7) . . ? C27 C26 C31 121.6(9) . . ? C27 C26 H26 119.2 . . ? C31 C26 H26 119.2 . . ? C28 C27 C26 118.5(9) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 121.0(10) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C28 119.9(9) . . ? C30 C29 H29 120 . . ? C28 C29 H29 120 . . ? C29 C30 C31 122.9(8) . . ? C29 C30 H30 118.6 . . ? C31 C30 H30 118.6 . . ? C30 C31 C26 116.2(8) . . ? C30 C31 P2 120.8(6) . . ? C26 C31 P2 123.0(7) . . ? C33 C32 C37 121.6(9) . . ? C33 C32 H32 119.2 . . ? C37 C32 H32 119.2 . . ? C32 C33 C34 117.7(10) . . ? C32 C33 H33 121.2 . . ? C34 C33 H33 121.2 . . ? C35 C34 C33 121.8(10) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C34 C35 C36 118.7(10) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C37 C36 C35 120.3(9) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C32 119.9(9) . . ? C36 C37 P2 119.0(7) . . ? C32 C37 P2 120.1(7) . . ? C52 P3 C46 106.6(4) . . ? C52 P3 C38 103.8(4) . . ? C46 P3 C38 99.4(4) . . ? C52 P3 Pt1 112.8(3) . . ? C46 P3 Pt1 118.0(3) . . ? C38 P3 Pt1 114.6(3) . . ? C64 P4 C40 107.3(4) . . ? C64 P4 C58 103.4(4) . . ? C40 P4 C58 101.3(4) . . ? C64 P4 Pt1 115.0(3) . . ? C40 P4 Pt1 113.4(3) . . ? C58 P4 Pt1 115.1(3) . . ? C39 C38 P3 113.8(6) . . ? C39 C38 H38A 108.8 . . ? P3 C38 H38A 108.8 . . ? C39 C38 H38B 108.8 . . ? P3 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? C40 C39 C38 114.3(7) . . ? C40 C39 H39A 108.7 . . ? C38 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? C38 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C39 C40 P4 116.9(6) . . ? C39 C40 H40A 108.1 . . ? P4 C40 H40A 108.1 . . ? C39 C40 H40B 108.1 . . ? P4 C40 H40B 108.1 . . ? H40A C40 H40B 107.3 . . ? C42 C41 C46 120.8(9) . . ? C42 C41 H41 119.6 . . ? C46 C41 H41 119.6 . . ? C41 C42 C43 120.1(9) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 120.0(9) . . ? C44 C43 H43 120 . . ? C42 C43 H43 120 . . ? C43 C44 C45 120.5(9) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C46 120.2(8) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 118.4(8) . . ? C45 C46 P3 124.4(6) . . ? C41 C46 P3 117.1(7) . . ? C48 C47 C52 119.3(8) . . ? C48 C47 H47 120.4 . . ? C52 C47 H47 120.4 . . ? C47 C48 C49 121.6(8) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C50 C49 C48 119.3(9) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C49 C50 C51 121.2(9) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C52 C51 C50 120.0(8) . . ? C52 C51 H51 120 . . ? C50 C51 H51 120 . . ? C51 C52 C47 118.5(8) . . ? C51 C52 P3 120.2(7) . . ? C47 C52 P3 121.3(7) . . ? C54 C53 C58 121.4(9) . . ? C54 C53 H53 119.3 . . ? C58 C53 H53 119.3 . . ? C53 C54 C55 119.6(9) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C54 C55 C56 119.1(9) . . ? C54 C55 H55 120.4 . . ? C56 C55 H55 120.4 . . ? C57 C56 C55 121.6(9) . . ? C57 C56 H56 119.2 . . ? C55 C56 H56 119.2 . . ? C56 C57 C58 118.9(8) . . ? C56 C57 H57 120.6 . . ? C58 C57 H57 120.6 . . ? C53 C58 C57 119.4(8) . . ? C53 C58 P4 121.4(7) . . ? C57 C58 P4 118.9(7) . . ? C60 C59 C64 120.3(9) . . ? C60 C59 H59 119.8 . . ? C64 C59 H59 119.8 . . ? C61 C60 C59 120.8(9) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C60 C61 C62 119.9(9) . . ? C60 C61 H61 120 . . ? C62 C61 H61 120 . . ? C63 C62 C61 120.7(9) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C62 C63 C64 120.1(9) . . ? C62 C63 H63 120 . . ? C64 C63 H63 120 . . ? C63 C64 C59 118.1(8) . . ? C63 C64 P4 118.6(7) . . ? C59 C64 P4 123.2(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 P4 Pt1 S1 Pt2 -152.65(9) . . . . ? S2 Pt1 S1 Pt2 35.76(7) . . . . ? P2 Pt2 S1 Pt1 141.00(9) . . . . ? S2 Pt2 S1 Pt1 -35.56(7) . . . . ? P4 Pt1 S2 C1 -178.9(4) . . . . ? P3 Pt1 S2 C1 26.6(3) . . . . ? S1 Pt1 S2 C1 -147.7(3) . . . . ? P4 Pt1 S2 Pt2 -66.0(3) . . . . ? P3 Pt1 S2 Pt2 139.54(7) . . . . ? S1 Pt1 S2 Pt2 -34.72(7) . . . . ? P2 Pt2 S2 C1 138.8(4) . . . . ? P1 Pt2 S2 C1 -36.2(3) . . . . ? S1 Pt2 S2 C1 152.3(3) . . . . ? P2 Pt2 S2 Pt1 21.1(3) . . . . ? P1 Pt2 S2 Pt1 -153.83(8) . . . . ? S1 Pt2 S2 Pt1 34.60(7) . . . . ? Pt1 S2 C1 C2 -129.2(6) . . . . ? Pt2 S2 C1 C2 130.0(6) . . . . ? Pt1 S2 C1 C6 50.6(8) . . . . ? Pt2 S2 C1 C6 -50.2(8) . . . . ? C6 C1 C2 F7 -178.5(7) . . . . ? S2 C1 C2 F7 1.2(11) . . . . ? C6 C1 C2 C3 3.4(12) . . . . ? S2 C1 C2 C3 -176.8(7) . . . . ? F7 C2 C3 N4 -179.4(8) . . . . ? C1 C2 C3 N4 -1.4(15) . . . . ? F7 C2 C3 F8 1.3(13) . . . . ? C1 C2 C3 F8 179.3(7) . . . . ? F8 C3 N4 C5 179.3(7) . . . . ? C2 C3 N4 C5 0.0(14) . . . . ? C3 N4 C5 F9 -178.5(8) . . . . ? C3 N4 C5 C6 -1.0(13) . . . . ? N4 C5 C6 F10 -174.7(7) . . . . ? F9 C5 C6 F10 2.7(12) . . . . ? N4 C5 C6 C1 3.4(14) . . . . ? F9 C5 C6 C1 -179.2(7) . . . . ? C2 C1 C6 F10 173.6(7) . . . . ? S2 C1 C6 F10 -6.1(11) . . . . ? C2 C1 C6 C5 -4.4(12) . . . . ? S2 C1 C6 C5 175.8(7) . . . . ? P2 Pt2 P1 C19 155.2(3) . . . . ? S2 Pt2 P1 C19 -26.1(3) . . . . ? P2 Pt2 P1 C11 40.9(3) . . . . ? S2 Pt2 P1 C11 -140.4(3) . . . . ? P2 Pt2 P1 C25 -80.1(3) . . . . ? S2 Pt2 P1 C25 98.6(3) . . . . ? P1 Pt2 P2 C31 89.2(3) . . . . ? S1 Pt2 P2 C31 -99.0(3) . . . . ? S2 Pt2 P2 C31 -85.8(4) . . . . ? P1 Pt2 P2 C13 -35.1(4) . . . . ? S1 Pt2 P2 C13 136.8(4) . . . . ? S2 Pt2 P2 C13 149.9(4) . . . . ? P1 Pt2 P2 C37 -153.9(3) . . . . ? S1 Pt2 P2 C37 17.9(3) . . . . ? S2 Pt2 P2 C37 31.1(5) . . . . ? C19 P1 C11 C12 172.8(7) . . . . ? C25 P1 C11 C12 64.5(7) . . . . ? Pt2 P1 C11 C12 -66.7(7) . . . . ? P1 C11 C12 C13 78.0(9) . . . . ? C11 C12 C13 P2 -66.7(10) . . . . ? C31 P2 C13 C12 -76.2(8) . . . . ? C37 P2 C13 C12 173.1(7) . . . . ? Pt2 P2 C13 C12 49.6(8) . . . . ? C19 C14 C15 C16 -1.2(14) . . . . ? C14 C15 C16 C17 0.2(15) . . . . ? C15 C16 C17 C18 0.9(15) . . . . ? C16 C17 C18 C19 -1.0(14) . . . . ? C17 C18 C19 C14 0.0(14) . . . . ? C17 C18 C19 P1 -178.0(7) . . . . ? C15 C14 C19 C18 1.1(13) . . . . ? C15 C14 C19 P1 179.0(7) . . . . ? C11 P1 C19 C18 63.5(8) . . . . ? C25 P1 C19 C18 170.8(7) . . . . ? Pt2 P1 C19 C18 -55.6(8) . . . . ? C11 P1 C19 C14 -114.4(8) . . . . ? C25 P1 C19 C14 -7.1(8) . . . . ? Pt2 P1 C19 C14 126.5(7) . . . . ? C25 C20 C21 C22 1.0(13) . . . . ? C20 C21 C22 C23 -1.9(14) . . . . ? C21 C22 C23 C24 0.6(15) . . . . ? C22 C23 C24 C25 1.6(14) . . . . ? C21 C20 C25 C24 1.0(13) . . . . ? C21 C20 C25 P1 -178.0(7) . . . . ? C23 C24 C25 C20 -2.3(13) . . . . ? C23 C24 C25 P1 176.7(7) . . . . ? C19 P1 C25 C20 118.4(8) . . . . ? C11 P1 C25 C20 -134.7(8) . . . . ? Pt2 P1 C25 C20 -10.2(9) . . . . ? C19 P1 C25 C24 -60.6(8) . . . . ? C11 P1 C25 C24 46.3(8) . . . . ? Pt2 P1 C25 C24 170.9(6) . . . . ? C31 C26 C27 C28 -1.9(14) . . . . ? C26 C27 C28 C29 2.2(14) . . . . ? C27 C28 C29 C30 -1.9(15) . . . . ? C28 C29 C30 C31 1.4(14) . . . . ? C29 C30 C31 C26 -1.1(13) . . . . ? C29 C30 C31 P2 178.4(7) . . . . ? C27 C26 C31 C30 1.4(13) . . . . ? C27 C26 C31 P2 -178.1(7) . . . . ? C13 P2 C31 C30 146.2(7) . . . . ? C37 P2 C31 C30 -104.5(7) . . . . ? Pt2 P2 C31 C30 16.6(8) . . . . ? C13 P2 C31 C26 -34.4(8) . . . . ? C37 P2 C31 C26 75.0(8) . . . . ? Pt2 P2 C31 C26 -164.0(6) . . . . ? C37 C32 C33 C34 -1.0(13) . . . . ? C32 C33 C34 C35 0.7(14) . . . . ? C33 C34 C35 C36 0.4(14) . . . . ? C34 C35 C36 C37 -1.2(14) . . . . ? C35 C36 C37 C32 1.0(13) . . . . ? C35 C36 C37 P2 -168.3(7) . . . . ? C33 C32 C37 C36 0.2(13) . . . . ? C33 C32 C37 P2 169.3(6) . . . . ? C31 P2 C37 C36 -168.6(7) . . . . ? C13 P2 C37 C36 -55.9(8) . . . . ? Pt2 P2 C37 C36 71.2(7) . . . . ? C31 P2 C37 C32 22.2(8) . . . . ? C13 P2 C37 C32 134.8(7) . . . . ? Pt2 P2 C37 C32 -98.1(7) . . . . ? P4 Pt1 P3 C52 77.6(3) . . . . ? S2 Pt1 P3 C52 -109.4(3) . . . . ? P4 Pt1 P3 C46 -157.4(3) . . . . ? S2 Pt1 P3 C46 15.6(3) . . . . ? P4 Pt1 P3 C38 -40.9(3) . . . . ? S2 Pt1 P3 C38 132.1(3) . . . . ? P3 Pt1 P4 C64 -84.4(3) . . . . ? S1 Pt1 P4 C64 90.1(3) . . . . ? S2 Pt1 P4 C64 120.5(4) . . . . ? P3 Pt1 P4 C40 39.7(3) . . . . ? S1 Pt1 P4 C40 -145.8(3) . . . . ? S2 Pt1 P4 C40 -115.4(4) . . . . ? P3 Pt1 P4 C58 155.6(3) . . . . ? S1 Pt1 P4 C58 -29.9(3) . . . . ? S2 Pt1 P4 C58 0.5(5) . . . . ? C52 P3 C38 C39 -65.4(7) . . . . ? C46 P3 C38 C39 -175.2(6) . . . . ? Pt1 P3 C38 C39 58.0(7) . . . . ? P3 C38 C39 C40 -69.0(9) . . . . ? C38 C39 C40 P4 70.6(9) . . . . ? C64 P4 C40 C39 69.3(7) . . . . ? C58 P4 C40 C39 177.3(7) . . . . ? Pt1 P4 C40 C39 -58.9(7) . . . . ? C46 C41 C42 C43 1.7(13) . . . . ? C41 C42 C43 C44 -0.2(13) . . . . ? C42 C43 C44 C45 0.0(13) . . . . ? C43 C44 C45 C46 -1.3(13) . . . . ? C44 C45 C46 C41 2.6(12) . . . . ? C44 C45 C46 P3 -174.1(6) . . . . ? C42 C41 C46 C45 -2.8(12) . . . . ? C42 C41 C46 P3 174.2(6) . . . . ? C52 P3 C46 C45 4.3(8) . . . . ? C38 P3 C46 C45 111.9(7) . . . . ? Pt1 P3 C46 C45 -123.7(6) . . . . ? C52 P3 C46 C41 -172.5(6) . . . . ? C38 P3 C46 C41 -64.9(7) . . . . ? Pt1 P3 C46 C41 59.5(7) . . . . ? C52 C47 C48 C49 -1.5(13) . . . . ? C47 C48 C49 C50 0.5(13) . . . . ? C48 C49 C50 C51 2.4(13) . . . . ? C49 C50 C51 C52 -4.2(13) . . . . ? C50 C51 C52 C47 3.1(13) . . . . ? C50 C51 C52 P3 -177.0(7) . . . . ? C48 C47 C52 C51 -0.3(12) . . . . ? C48 C47 C52 P3 179.8(6) . . . . ? C46 P3 C52 C51 -121.9(7) . . . . ? C38 P3 C52 C51 133.7(7) . . . . ? Pt1 P3 C52 C51 9.0(8) . . . . ? C46 P3 C52 C47 58.0(8) . . . . ? C38 P3 C52 C47 -46.4(8) . . . . ? Pt1 P3 C52 C47 -171.1(6) . . . . ? C58 C53 C54 C55 0.1(12) . . . . ? C53 C54 C55 C56 -0.9(12) . . . . ? C54 C55 C56 C57 0.7(13) . . . . ? C55 C56 C57 C58 0.2(13) . . . . ? C54 C53 C58 C57 0.8(12) . . . . ? C54 C53 C58 P4 175.1(6) . . . . ? C56 C57 C58 C53 -1.0(12) . . . . ? C56 C57 C58 P4 -175.5(6) . . . . ? C64 P4 C58 C53 10.8(8) . . . . ? C40 P4 C58 C53 -100.3(7) . . . . ? Pt1 P4 C58 C53 137.1(6) . . . . ? C64 P4 C58 C57 -174.8(7) . . . . ? C40 P4 C58 C57 74.1(7) . . . . ? Pt1 P4 C58 C57 -48.6(7) . . . . ? C64 C59 C60 C61 4.1(14) . . . . ? C59 C60 C61 C62 -3.3(15) . . . . ? C60 C61 C62 C63 0.8(15) . . . . ? C61 C62 C63 C64 0.9(14) . . . . ? C62 C63 C64 C59 -0.2(13) . . . . ? C62 C63 C64 P4 -176.3(7) . . . . ? C60 C59 C64 C63 -2.3(13) . . . . ? C60 C59 C64 P4 173.7(7) . . . . ? C40 P4 C64 C63 -170.1(7) . . . . ? C58 P4 C64 C63 83.4(8) . . . . ? Pt1 P4 C64 C63 -42.9(8) . . . . ? C40 P4 C64 C59 14.0(9) . . . . ? C58 P4 C64 C59 -92.6(8) . . . . ? Pt1 P4 C64 C59 141.1(7) . . . . ? # start Validation Reply Form _vrf_PUBL006_GLOBAL ; PROBLEM: _publ_requested_journal is missing RESPONSE: It has to be added by the authors. ; _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: It has to be added by the authors. ; _vrf_THETM01_ub01nf1n ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The biggest and best looking crystals were chosen and tested for data collection. The best one was selected, but still diffracts weakly and it gives no detectable diffraction above 22.02 degrees in theta (0.95 Angstroms resolution). See attached document for additional information. ; _vrf_PLAT023_ub01nf1n ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.02 Deg. RESPONSE: The biggest and best looking crystals were chosen and tested for data collection. The best one was selected, but still diffracts weakly and it gives no detectable diffraction above 22.02 degrees in theta (0.95 Angstroms resolution). See attached document for additional information. ; _vrf_PLAT602_ub01nf1n ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Two 690 Angstroms**3 voids per unit cell containing 319 electrons each were found by the SQUEEZE procedure implemented in PLATON. They are filled by a very disordered mixture of the counterion and solvent molecules (methanol, water). It was not possible to find an ordered model even relaxing the crystal symmetry. ; # end Validation Reply Form # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF