Supplementary Material (ESI) for Chemical Science This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Nianyong Zhu' _publ_contact_author_email nzhu@hkucc.hku.hk loop_ _publ_author_name R.Sun A.Chow 'Xiao-Hua Li.' J.Yan S.S-Y.Che 'Chi-Ming Che.' data_mar1922 _database_code_depnum_ccdc_archive 'CCDC 756500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 F6 N4 P Pt' _chemical_formula_sum 'C27 H31 F6 N4 P Pt' _chemical_formula_weight 751.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 13.381(3) _cell_length_b 14.391(3) _cell_length_c 16.034(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.16(3) _cell_angle_gamma 90.00 _cell_volume 2879.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 4.991 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch IPDS mar300' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21084 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.63 _reflns_number_total 5218 _reflns_number_gt 3402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia,1999)' _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^)+(0.0050P)^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_extinction_coef ? _refine_ls_number_reflns 5218 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 0.736 _refine_ls_restrained_S_all 0.736 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.6998(6) 0.3558(5) 0.1208(5) 0.0684(19) Uani 1 1 d . . . H2 H 0.6832 0.3107 0.1553 0.082 Uiso 1 1 calc R . . C3 C 0.6204(7) 0.3923(7) 0.0485(6) 0.089(3) Uani 1 1 d . . . H3 H 0.5501 0.3730 0.0353 0.107 Uiso 1 1 calc R . . C4 C 0.6431(7) 0.4583(6) -0.0062(5) 0.089(3) Uani 1 1 d . . . H4 H 0.5882 0.4813 -0.0560 0.107 Uiso 1 1 calc R . . C5 C 0.7469(7) 0.4895(5) 0.0135(5) 0.076(2) Uani 1 1 d . . . H5 H 0.7621 0.5329 -0.0233 0.092 Uiso 1 1 calc R . . C6 C 0.8280(6) 0.4556(5) 0.0886(4) 0.0606(17) Uani 1 1 d . . . C7 C 0.9384(6) 0.4905(4) 0.1181(4) 0.0609(17) Uani 1 1 d . . . C8 C 0.9798(7) 0.5624(5) 0.0836(5) 0.076(2) Uani 1 1 d . . . H8 H 0.9364 0.5937 0.0326 0.091 Uiso 1 1 calc R . . C9 C 1.0845(8) 0.5874(5) 0.1243(6) 0.087(2) Uani 1 1 d . . . H9 H 1.1120 0.6360 0.1007 0.104 Uiso 1 1 calc R . . C10 C 1.1514(6) 0.5412(5) 0.2009(5) 0.074(2) Uani 1 1 d . . . H10 H 1.2227 0.5584 0.2289 0.089 Uiso 1 1 calc R . . C11 C 1.1080(6) 0.4692(4) 0.2336(4) 0.0596(16) Uani 1 1 d . . . C12 C 1.1647(6) 0.4109(5) 0.3117(4) 0.0639(18) Uani 1 1 d . . . C13 C 1.2710(6) 0.4201(6) 0.3634(5) 0.082(2) Uani 1 1 d . . . H13 H 1.3119 0.4665 0.3509 0.098 Uiso 1 1 calc R . . C14 C 1.3168(7) 0.3607(7) 0.4339(6) 0.090(3) Uani 1 1 d . . . H14 H 1.3886 0.3676 0.4700 0.108 Uiso 1 1 calc R . . C15 C 1.2570(7) 0.2918(6) 0.4506(5) 0.085(2) Uani 1 1 d . . . H15 H 1.2875 0.2491 0.4963 0.102 Uiso 1 1 calc R . . C16 C 1.1506(6) 0.2870(5) 0.3981(5) 0.077(2) Uani 1 1 d . . . H16 H 1.1095 0.2407 0.4106 0.092 Uiso 1 1 calc R . . C17 C 0.8704(5) 0.2530(5) 0.2937(4) 0.0632(17) Uani 1 1 d . . . C18 C 0.7818(7) 0.1848(6) 0.3729(6) 0.089(3) Uani 1 1 d . . . H18 H 0.7476 0.1760 0.4136 0.107 Uiso 1 1 calc R . . C19 C 0.7962(8) 0.1205(6) 0.3167(6) 0.096(3) Uani 1 1 d . . . H19 H 0.7738 0.0589 0.3111 0.116 Uiso 1 1 calc R . . C20 C 0.8357(9) 0.3494(6) 0.4097(7) 0.101(3) Uani 1 1 d . . . H20A H 0.7693 0.3602 0.4195 0.121 Uiso 1 1 calc R . . H20B H 0.8495 0.4025 0.3781 0.121 Uiso 1 1 calc R . . C21 C 0.9347(8) 0.3357(7) 0.5057(8) 0.124(4) Uani 1 1 d . . . H21A H 0.9227 0.2791 0.5336 0.149 Uiso 1 1 calc R . . H21B H 1.0008 0.3282 0.4946 0.149 Uiso 1 1 calc R . . C22 C 0.9466(12) 0.4104(9) 0.5657(10) 0.163(5) Uani 1 1 d . . . H22A H 0.8826 0.4166 0.5802 0.195 Uiso 1 1 calc R . . H22B H 0.9569 0.4679 0.5382 0.195 Uiso 1 1 calc R . . C23 C 1.0422(11) 0.3921(11) 0.6495(9) 0.179(6) Uani 1 1 d . . . H23A H 1.0515 0.4431 0.6902 0.269 Uiso 1 1 calc R . . H23B H 1.1052 0.3857 0.6346 0.269 Uiso 1 1 calc R . . H23C H 1.0308 0.3360 0.6771 0.269 Uiso 1 1 calc R . . C24 C 0.8781(9) 0.1168(7) 0.1992(7) 0.109(3) Uani 1 1 d . . . H24A H 0.9229 0.1577 0.1796 0.130 Uiso 1 1 calc R . . H24B H 0.8135 0.1037 0.1483 0.130 Uiso 1 1 calc R . . C25 C 0.9369(10) 0.0280(10) 0.2343(8) 0.165(6) Uani 1 1 d . . . H25A H 1.0047 0.0441 0.2805 0.198 Uiso 1 1 calc R . . H25B H 0.8958 -0.0063 0.2631 0.198 Uiso 1 1 calc R . . C26 C 0.9577(11) -0.0295(11) 0.1780(11) 0.201(7) Uani 1 1 d . . . H26A H 1.0054 0.0012 0.1534 0.242 Uiso 1 1 calc R . . H26B H 0.8914 -0.0431 0.1289 0.242 Uiso 1 1 calc R . . C27 C 1.0093(14) -0.1213(10) 0.2216(12) 0.209(7) Uani 1 1 d . . . H27A H 1.0201 -0.1607 0.1773 0.314 Uiso 1 1 calc R . . H27B H 0.9629 -0.1520 0.2467 0.314 Uiso 1 1 calc R . . H27C H 1.0770 -0.1087 0.2681 0.314 Uiso 1 1 calc R . . P1 P 0.14818(18) 0.22160(15) 0.09787(13) 0.0747(6) Uani 1 1 d . . . Pt1 Pt 0.94091(2) 0.348301(17) 0.244316(16) 0.05464(11) Uani 1 1 d . . . F1 F 0.1467(7) 0.2396(5) 0.0039(4) 0.202(4) Uani 1 1 d . . . F2 F 0.0324(4) 0.2625(5) 0.0676(4) 0.142(2) Uani 1 1 d . . . F3 F 0.1859(7) 0.3195(5) 0.1218(6) 0.211(4) Uani 1 1 d . . . F4 F 0.2586(6) 0.1770(6) 0.1267(6) 0.204(4) Uani 1 1 d . . . F5 F 0.1014(8) 0.1241(5) 0.0715(6) 0.217(4) Uani 1 1 d . . . F6 F 0.1488(7) 0.2042(6) 0.1924(4) 0.191(4) Uani 1 1 d . . . C1 C 0.8085(6) 0.3861(5) 0.1442(4) 0.0728(18) Uani 0.50 1 d P . . N1' N 0.8085(6) 0.3861(5) 0.1442(4) 0.0728(18) Uani 0.50 1 d P . . N1 N 1.1027(5) 0.3439(4) 0.3309(4) 0.0547(14) Uani 0.50 1 d P . . C1' C 1.1027(5) 0.3439(4) 0.3309(4) 0.0547(14) Uani 0.50 1 d P . . N2 N 1.0049(4) 0.4472(3) 0.1915(3) 0.0539(12) Uani 1 1 d . . . N3 N 0.8278(5) 0.2662(4) 0.3581(4) 0.0707(16) Uani 1 1 d . . . N4 N 0.8497(6) 0.1632(4) 0.2702(4) 0.0785(18) 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 C2 0.067(5) 0.066(5) 0.077(5) -0.007(4) 0.032(4) 0.005(4) C3 0.075(5) 0.084(6) 0.099(6) -0.030(5) 0.019(5) 0.005(5) C4 0.094(7) 0.089(7) 0.068(5) -0.004(4) 0.010(5) 0.027(5) C5 0.104(6) 0.063(5) 0.066(5) 0.010(4) 0.036(4) 0.026(4) C6 0.079(5) 0.052(4) 0.055(4) -0.003(3) 0.029(3) 0.007(4) C7 0.087(5) 0.044(4) 0.063(4) -0.001(3) 0.041(4) 0.010(4) C8 0.108(6) 0.056(5) 0.073(5) 0.016(4) 0.043(5) 0.003(4) C9 0.126(7) 0.053(5) 0.103(6) 0.014(4) 0.068(6) -0.008(5) C10 0.098(5) 0.053(4) 0.085(5) -0.002(4) 0.050(4) -0.018(4) C11 0.076(5) 0.047(4) 0.069(4) -0.001(3) 0.041(4) -0.001(4) C12 0.066(5) 0.058(5) 0.071(4) -0.008(3) 0.028(4) 0.002(4) C13 0.075(5) 0.081(6) 0.093(6) -0.005(5) 0.034(5) -0.008(4) C14 0.069(5) 0.108(8) 0.090(6) -0.007(5) 0.025(5) 0.012(5) C15 0.080(6) 0.091(6) 0.083(5) 0.017(5) 0.029(5) 0.020(5) C16 0.076(5) 0.070(5) 0.088(5) 0.017(4) 0.035(4) 0.011(4) C17 0.062(4) 0.065(5) 0.071(4) 0.007(3) 0.033(3) 0.010(4) C18 0.103(7) 0.082(6) 0.100(6) 0.022(5) 0.058(5) -0.013(5) C19 0.141(8) 0.060(5) 0.119(7) 0.013(5) 0.085(7) -0.018(5) C20 0.134(8) 0.071(6) 0.139(8) 0.005(5) 0.097(7) 0.005(5) C21 0.114(8) 0.130(9) 0.152(10) -0.064(8) 0.074(8) -0.010(7) C22 0.207(14) 0.135(11) 0.219(14) -0.032(11) 0.165(13) -0.030(10) C23 0.172(13) 0.215(16) 0.123(10) -0.046(10) 0.019(9) 0.000(12) C24 0.155(9) 0.073(6) 0.134(8) -0.005(6) 0.095(7) -0.009(6) C25 0.237(16) 0.111(11) 0.215(14) -0.022(9) 0.165(13) 0.027(10) C26 0.161(13) 0.130(13) 0.33(2) -0.028(15) 0.109(14) -0.013(10) C27 0.240(16) 0.105(11) 0.32(2) 0.041(13) 0.139(16) 0.044(12) P1 0.0964(15) 0.0602(13) 0.0798(13) 0.0132(10) 0.0466(11) 0.0168(11) Pt1 0.06584(18) 0.04278(16) 0.06383(17) 0.00670(12) 0.03366(13) 0.00312(13) F1 0.338(10) 0.193(7) 0.145(5) 0.088(5) 0.172(6) 0.141(7) F2 0.112(4) 0.156(6) 0.160(5) 0.034(4) 0.054(4) 0.045(4) F3 0.222(8) 0.111(5) 0.235(9) -0.007(6) 0.005(7) -0.054(6) F4 0.146(6) 0.272(10) 0.230(8) 0.117(7) 0.112(6) 0.126(7) F5 0.300(11) 0.078(4) 0.237(9) 0.005(5) 0.053(8) -0.021(6) F6 0.265(9) 0.221(8) 0.114(5) 0.059(5) 0.100(5) 0.116(7) C1 0.098(5) 0.050(4) 0.075(4) -0.006(3) 0.036(4) 0.004(4) N1' 0.098(5) 0.050(4) 0.075(4) -0.006(3) 0.036(4) 0.004(4) N1 0.068(4) 0.045(3) 0.058(3) 0.009(3) 0.031(3) 0.006(3) C1' 0.068(4) 0.045(3) 0.058(3) 0.009(3) 0.031(3) 0.006(3) N2 0.070(4) 0.037(3) 0.064(3) 0.002(2) 0.037(3) 0.006(3) N3 0.075(4) 0.072(4) 0.079(4) 0.008(3) 0.043(3) -0.001(3) N4 0.103(5) 0.051(4) 0.102(5) 0.007(3) 0.061(4) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C3 1.364(10) . ? C2 C1 1.432(9) . ? C2 H2 0.9300 . ? C3 C4 1.397(12) . ? C3 H3 0.9300 . ? C4 C5 1.384(10) . ? C4 H4 0.9300 . ? C5 C6 1.386(9) . ? C5 H5 0.9300 . ? C6 C1 1.425(9) . ? C6 C7 1.468(9) . ? C7 N2 1.344(8) . ? C7 C8 1.381(9) . ? C8 C9 1.363(11) . ? C8 H8 0.9300 . ? C9 C10 1.400(10) . ? C9 H9 0.9300 . ? C10 C11 1.380(9) . ? C10 H10 0.9300 . ? C11 N2 1.337(8) . ? C11 C12 1.470(9) . ? C12 C13 1.369(9) . ? C12 N1 1.379(9) . ? C13 C14 1.372(11) . ? C13 H13 0.9300 . ? C14 C15 1.361(11) . ? C14 H14 0.9300 . ? C15 C16 1.369(10) . ? C15 H15 0.9300 . ? C16 N1 1.321(8) . ? C16 H16 0.9300 . ? C17 N4 1.347(8) . ? C17 N3 1.361(8) . ? C17 Pt1 1.984(7) . ? C18 C19 1.354(12) . ? C18 N3 1.383(9) . ? C18 H18 0.9300 . ? C19 N4 1.353(9) . ? C19 H19 0.9300 . ? C20 N3 1.438(9) . ? C20 C21 1.640(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.413(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.507(16) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N4 1.482(10) . ? C24 C25 1.500(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.326(15) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.537(18) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? P1 F3 1.500(7) . ? P1 F4 1.521(6) . ? P1 F1 1.521(5) . ? P1 F5 1.533(7) . ? P1 F6 1.534(6) . ? P1 F2 1.562(5) . ? Pt1 C1 1.990(7) . ? Pt1 N2 2.000(5) . ? Pt1 N1 2.109(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 C1 120.7(8) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 121.1(8) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 120.3(8) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.3(7) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C1 121.9(7) . . ? C5 C6 C7 122.7(7) . . ? C1 C6 C7 115.3(6) . . ? N2 C7 C8 117.6(7) . . ? N2 C7 C6 113.3(6) . . ? C8 C7 C6 129.0(7) . . ? C9 C8 C7 119.8(7) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 121.0(7) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 117.9(7) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? N2 C11 C10 119.0(6) . . ? N2 C11 C12 114.6(6) . . ? C10 C11 C12 126.4(7) . . ? C13 C12 N1 120.7(7) . . ? C13 C12 C11 124.4(7) . . ? N1 C12 C11 114.9(6) . . ? C12 C13 C14 119.8(8) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 119.7(8) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 118.1(8) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? N1 C16 C15 124.1(8) . . ? N1 C16 H16 117.9 . . ? C15 C16 H16 117.9 . . ? N4 C17 N3 104.2(6) . . ? N4 C17 Pt1 129.1(5) . . ? N3 C17 Pt1 126.6(5) . . ? C19 C18 N3 106.6(7) . . ? C19 C18 H18 126.7 . . ? N3 C18 H18 126.7 . . ? N4 C19 C18 106.7(7) . . ? N4 C19 H19 126.6 . . ? C18 C19 H19 126.6 . . ? N3 C20 C21 107.8(7) . . ? N3 C20 H20A 110.1 . . ? C21 C20 H20A 110.1 . . ? N3 C20 H20B 110.1 . . ? C21 C20 H20B 110.1 . . ? H20A C20 H20B 108.5 . . ? C22 C21 C20 113.7(11) . . ? C22 C21 H21A 108.8 . . ? C20 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? C20 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 C23 109.0(12) . . ? C21 C22 H22A 109.9 . . ? C23 C22 H22A 109.9 . . ? C21 C22 H22B 109.9 . . ? C23 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C25 109.9(8) . . ? N4 C24 H24A 109.7 . . ? C25 C24 H24A 109.7 . . ? N4 C24 H24B 109.7 . . ? C25 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C26 C25 C24 119.2(13) . . ? C26 C25 H25A 107.5 . . ? C24 C25 H25A 107.5 . . ? C26 C25 H25B 107.5 . . ? C24 C25 H25B 107.5 . . ? H25A C25 H25B 107.0 . . ? C25 C26 C27 113.4(16) . . ? C25 C26 H26A 108.9 . . ? C27 C26 H26A 108.9 . . ? C25 C26 H26B 108.9 . . ? C27 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? F3 P1 F4 96.8(5) . . ? F3 P1 F1 88.6(5) . . ? F4 P1 F1 92.1(4) . . ? F3 P1 F5 175.9(6) . . ? F4 P1 F5 87.3(5) . . ? F1 P1 F5 91.4(5) . . ? F3 P1 F6 91.1(5) . . ? F4 P1 F6 88.4(4) . . ? F1 P1 F6 179.4(4) . . ? F5 P1 F6 88.8(5) . . ? F3 P1 F2 86.0(4) . . ? F4 P1 F2 177.2(5) . . ? F1 P1 F2 88.3(4) . . ? F5 P1 F2 89.9(5) . . ? F6 P1 F2 91.1(4) . . ? C17 Pt1 C1 95.6(3) . . ? C17 Pt1 N2 177.2(2) . . ? C1 Pt1 N2 81.7(3) . . ? C17 Pt1 N1 103.8(2) . . ? C1 Pt1 N1 160.5(3) . . ? N2 Pt1 N1 78.8(2) . . ? C6 C1 C2 116.6(7) . . ? C6 C1 Pt1 112.7(5) . . ? C2 C1 Pt1 130.7(5) . . ? C16 N1 C12 117.5(6) . . ? C16 N1 Pt1 129.6(5) . . ? C12 N1 Pt1 112.9(4) . . ? C11 N2 C7 124.6(6) . . ? C11 N2 Pt1 118.4(4) . . ? C7 N2 Pt1 116.8(5) . . ? C17 N3 C18 110.3(7) . . ? C17 N3 C20 126.0(6) . . ? C18 N3 C20 123.5(7) . . ? C17 N4 C19 112.2(7) . . ? C17 N4 C24 124.2(7) . . ? C19 N4 C24 123.5(7) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.557 _refine_diff_density_min -1.787 _refine_diff_density_rms 0.125 data_mar1829 _database_code_depnum_ccdc_archive 'CCDC 756501' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H23 I3 N4 Pt' _chemical_formula_sum 'C23 H23 I3 N4 Pt' _chemical_formula_weight 931.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.652(2) _cell_length_b 11.015(2) _cell_length_c 14.031(3) _cell_angle_alpha 90.68(3) _cell_angle_beta 98.09(3) _cell_angle_gamma 90.57(3) _cell_volume 1323.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 8.816 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch IPDS mar300' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9699 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.1063 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.66 _reflns_number_total 4627 _reflns_number_gt 3195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SIR2004 (Giacovazzo et al, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+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_extinction_coef ? _refine_ls_number_reflns 4627 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.01637(4) 0.86409(3) 0.79849(2) 0.04282(14) Uani 1 1 d . . . N1 N 0.1270(9) 0.9437(7) 0.9061(6) 0.0499(19) Uani 1 1 d . . . N2 N -0.0490(9) 0.7486(7) 0.9142(5) 0.0418(19) Uani 0.50 1 d P . . C1' C -0.0490(9) 0.7486(7) 0.9142(5) 0.0418(19) Uani 0.50 1 d P . . N3 N -0.1259(9) 0.6708(7) 0.6508(5) 0.0496(19) Uani 1 1 d . . . N4 N -0.2956(9) 0.8155(7) 0.6437(5) 0.056(2) Uani 1 1 d . . . C1 C 0.0607(12) 1.0070(9) 0.7273(7) 0.064(3) Uani 0.50 1 d P . . N2' N 0.0607(12) 1.0070(9) 0.7273(7) 0.064(3) Uani 0.50 1 d P . . C2 C 0.0186(13) 1.0450(9) 0.6320(7) 0.061(3) Uani 1 1 d . . . H2 H -0.0568 1.0011 0.5915 0.073 Uiso 1 1 calc R . . C3 C 0.0861(16) 1.1449(11) 0.5975(9) 0.078(4) Uani 1 1 d . . . H3 H 0.0606 1.1665 0.5334 0.094 Uiso 1 1 calc R . . C4 C 0.1925(15) 1.2137(11) 0.6588(9) 0.078(4) Uani 1 1 d . . . H4 H 0.2357 1.2831 0.6356 0.094 Uiso 1 1 calc R . . C5 C 0.2358(14) 1.1825(10) 0.7521(9) 0.070(3) Uani 1 1 d . . . H5 H 0.3084 1.2295 0.7921 0.083 Uiso 1 1 calc R . . C6 C 0.1687(11) 1.0773(9) 0.7876(7) 0.056(3) Uani 1 1 d . . . C7 C 0.2100(11) 1.0412(9) 0.8866(7) 0.053(2) Uani 1 1 d . . . C8 C 0.3143(12) 1.0926(9) 0.9608(8) 0.062(3) Uani 1 1 d . . . H8 H 0.3711 1.1617 0.9493 0.074 Uiso 1 1 calc R . . C9 C 0.3345(13) 1.0429(11) 1.0507(9) 0.069(3) Uani 1 1 d . . . H9 H 0.4055 1.0778 1.0996 0.082 Uiso 1 1 calc R . . C10 C 0.2481(12) 0.9395(11) 1.0689(7) 0.067(3) Uani 1 1 d . . . H10 H 0.2598 0.9053 1.1298 0.080 Uiso 1 1 calc R . . C11 C 0.1443(11) 0.8891(9) 0.9937(7) 0.049(2) Uani 1 1 d . . . C12 C 0.0414(11) 0.7825(9) 0.9976(6) 0.050(2) Uani 1 1 d . . . C13 C 0.0272(13) 0.7191(10) 1.0821(7) 0.061(3) Uani 1 1 d . . . H13 H 0.0896 0.7398 1.1396 0.073 Uiso 1 1 calc R . . C14 C -0.0788(14) 0.6271(10) 1.0789(9) 0.072(3) Uani 1 1 d . . . H14 H -0.0901 0.5854 1.1347 0.086 Uiso 1 1 calc R . . C15 C -0.1684(14) 0.5955(11) 0.9948(9) 0.074(3) Uani 1 1 d . . . H15 H -0.2419 0.5329 0.9925 0.089 Uiso 1 1 calc R . . C16 C -0.1486(12) 0.6571(9) 0.9140(7) 0.055(3) Uani 1 1 d . . . H16 H -0.2078 0.6337 0.8560 0.066 Uiso 1 1 calc R . . C17 C -0.1550(12) 0.7782(8) 0.6904(6) 0.047(2) Uani 1 1 d . . . C18 C -0.2476(14) 0.6401(10) 0.5799(7) 0.065(3) Uani 1 1 d . . . H18 H -0.2558 0.5701 0.5418 0.078 Uiso 1 1 calc R . . C19 C -0.3485(13) 0.7268(11) 0.5762(7) 0.066(3) Uani 1 1 d . . . H19 H -0.4419 0.7290 0.5344 0.079 Uiso 1 1 calc R . . C20 C 0.0180(14) 0.6035(10) 0.6744(8) 0.073(3) Uani 1 1 d . . . H20A H 0.0652 0.6251 0.7393 0.088 Uiso 1 1 calc R . . H20B H -0.0062 0.5173 0.6728 0.088 Uiso 1 1 calc R . . C21 C 0.1272(18) 0.6278(17) 0.6092(11) 0.126(6) Uani 1 1 d . . . H21A H 0.0750 0.6221 0.5442 0.188 Uiso 1 1 calc R . . H21B H 0.2096 0.5695 0.6183 0.188 Uiso 1 1 calc R . . H21C H 0.1704 0.7080 0.6214 0.188 Uiso 1 1 calc R . . C22 C -0.3714(16) 0.9279(12) 0.6600(9) 0.092(4) Uani 1 1 d . . . H22A H -0.3284 0.9581 0.7236 0.110 Uiso 1 1 calc R . . H22B H -0.3430 0.9861 0.6139 0.110 Uiso 1 1 calc R . . C23 C -0.530(2) 0.9271(16) 0.6543(17) 0.170(9) Uani 1 1 d . . . H23A H -0.5734 0.8643 0.6102 0.256 Uiso 1 1 calc R . . H23B H -0.5698 1.0043 0.6319 0.256 Uiso 1 1 calc R . . H23C H -0.5588 0.9122 0.7168 0.256 Uiso 1 1 calc R . . I1 I 0.38862(10) 0.65976(8) 0.87736(7) 0.0815(3) Uani 1 1 d . . . I2 I 0.52784(9) 0.46940(6) 0.77097(5) 0.0653(2) Uani 1 1 d . . . I3 I 0.68497(11) 0.28956(7) 0.66465(6) 0.0816(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0447(2) 0.0463(2) 0.0346(2) -0.00815(13) -0.00339(15) -0.00267(15) N1 0.043(5) 0.051(5) 0.053(5) -0.009(4) 0.003(4) -0.002(4) N2 0.035(5) 0.053(5) 0.035(4) -0.005(3) -0.003(3) 0.006(4) C1' 0.035(5) 0.053(5) 0.035(4) -0.005(3) -0.003(3) 0.006(4) N3 0.060(6) 0.043(5) 0.041(4) -0.009(3) -0.008(4) 0.002(4) N4 0.050(5) 0.063(6) 0.047(5) -0.005(4) -0.022(4) -0.004(4) C1 0.066(7) 0.075(7) 0.054(6) -0.018(5) 0.016(5) -0.008(5) N2' 0.066(7) 0.075(7) 0.054(6) -0.018(5) 0.016(5) -0.008(5) C2 0.085(9) 0.045(6) 0.052(6) 0.002(4) 0.008(6) -0.001(5) C3 0.112(11) 0.069(8) 0.056(7) 0.010(6) 0.021(7) 0.015(7) C4 0.097(10) 0.063(8) 0.081(9) -0.010(6) 0.038(8) -0.024(7) C5 0.072(8) 0.059(7) 0.080(9) -0.015(6) 0.023(7) -0.015(6) C6 0.046(6) 0.061(7) 0.059(7) -0.021(5) 0.008(5) -0.007(5) C7 0.039(6) 0.062(7) 0.058(6) -0.016(5) 0.011(5) 0.001(5) C8 0.052(7) 0.060(7) 0.072(8) -0.031(6) 0.010(6) -0.011(5) C9 0.045(7) 0.081(9) 0.075(8) -0.029(6) -0.007(6) -0.005(6) C10 0.057(7) 0.105(9) 0.032(5) -0.026(5) -0.015(5) 0.008(6) C11 0.042(6) 0.054(6) 0.052(6) -0.008(4) 0.005(5) 0.004(4) C12 0.038(6) 0.067(7) 0.040(5) -0.013(4) -0.004(4) -0.002(5) C13 0.068(8) 0.076(8) 0.038(6) 0.002(5) 0.000(5) 0.019(6) C14 0.080(9) 0.070(8) 0.068(8) 0.016(6) 0.019(7) -0.009(7) C15 0.078(9) 0.069(8) 0.071(8) 0.009(6) 0.000(7) -0.010(6) C16 0.059(7) 0.053(6) 0.052(6) 0.001(5) 0.005(5) -0.003(5) C17 0.064(7) 0.039(5) 0.036(5) 0.006(4) 0.003(5) -0.007(4) C18 0.086(9) 0.059(7) 0.041(6) -0.015(5) -0.017(5) -0.003(6) C19 0.063(8) 0.068(8) 0.055(7) -0.009(5) -0.027(5) -0.013(6) C20 0.099(10) 0.047(7) 0.066(7) -0.014(5) -0.015(7) 0.021(6) C21 0.100(13) 0.198(18) 0.079(11) -0.005(11) 0.010(9) 0.047(12) C22 0.084(10) 0.090(10) 0.091(10) -0.031(7) -0.024(7) 0.036(8) C23 0.097(15) 0.125(16) 0.30(3) -0.066(16) 0.056(16) 0.020(11) I1 0.0688(6) 0.0779(6) 0.0981(6) -0.0101(4) 0.0138(5) -0.0055(4) I2 0.0649(5) 0.0596(5) 0.0661(5) 0.0001(3) -0.0077(4) -0.0140(3) I3 0.0970(7) 0.0731(5) 0.0664(5) -0.0113(4) -0.0168(4) 0.0070(4) _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 N1 2.001(8) . ? Pt1 C17 2.016(9) . ? Pt1 C1 2.031(10) . ? Pt1 N2 2.122(8) . ? N1 C7 1.338(12) . ? N1 C11 1.365(12) . ? N2 C16 1.320(12) . ? N2 C12 1.359(11) . ? N3 C17 1.343(11) . ? N3 C18 1.380(12) . ? N3 C20 1.454(13) . ? N4 C17 1.368(12) . ? N4 C19 1.382(12) . ? N4 C22 1.438(13) . ? C1 C6 1.392(13) . ? C1 C2 1.406(13) . ? C2 C3 1.365(15) . ? C2 H2 0.9300 . ? C3 C4 1.382(17) . ? C3 H3 0.9300 . ? C4 C5 1.359(16) . ? C4 H4 0.9300 . ? C5 C6 1.417(14) . ? C5 H5 0.9300 . ? C6 C7 1.447(14) . ? C7 C8 1.389(13) . ? C8 C9 1.371(15) . ? C8 H8 0.9300 . ? C9 C10 1.403(15) . ? C9 H9 0.9300 . ? C10 C11 1.392(14) . ? C10 H10 0.9300 . ? C11 C12 1.472(13) . ? C12 C13 1.403(13) . ? C13 C14 1.356(14) . ? C13 H13 0.9300 . ? C14 C15 1.358(16) . ? C14 H14 0.9300 . ? C15 C16 1.359(14) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 C19 1.297(14) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.430(16) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.364(19) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? I1 I2 2.9254(14) . ? I2 I3 2.9244(14) . ? 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 N1 Pt1 C17 177.7(3) . . ? N1 Pt1 C1 80.2(4) . . ? C17 Pt1 C1 100.7(4) . . ? N1 Pt1 N2 79.3(3) . . ? C17 Pt1 N2 99.8(3) . . ? C1 Pt1 N2 159.5(3) . . ? C7 N1 C11 123.5(8) . . ? C7 N1 Pt1 118.6(7) . . ? C11 N1 Pt1 117.7(6) . . ? C16 N2 C12 119.6(9) . . ? C16 N2 Pt1 128.0(7) . . ? C12 N2 Pt1 112.3(7) . . ? C17 N3 C18 109.3(8) . . ? C17 N3 C20 124.6(8) . . ? C18 N3 C20 126.0(9) . . ? C17 N4 C19 107.2(9) . . ? C17 N4 C22 126.2(8) . . ? C19 N4 C22 126.6(9) . . ? C6 C1 C2 118.1(9) . . ? C6 C1 Pt1 111.3(8) . . ? C2 C1 Pt1 130.6(8) . . ? C3 C2 C1 121.4(11) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 119.4(11) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 121.7(11) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 119.0(11) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 C6 C5 120.3(10) . . ? C1 C6 C7 118.7(9) . . ? C5 C6 C7 121.1(10) . . ? N1 C7 C8 118.2(10) . . ? N1 C7 C6 111.1(9) . . ? C8 C7 C6 130.7(10) . . ? C9 C8 C7 120.9(10) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.9(10) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 118.4(10) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? N1 C11 C10 119.1(10) . . ? N1 C11 C12 113.7(8) . . ? C10 C11 C12 127.1(10) . . ? N2 C12 C13 119.2(9) . . ? N2 C12 C11 116.8(9) . . ? C13 C12 C11 124.0(9) . . ? C14 C13 C12 119.1(10) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.5(11) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 118.6(11) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N2 C16 C15 122.9(10) . . ? N2 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? N3 C17 N4 106.5(8) . . ? N3 C17 Pt1 125.7(7) . . ? N4 C17 Pt1 127.7(7) . . ? C19 C18 N3 107.5(9) . . ? C19 C18 H18 126.3 . . ? N3 C18 H18 126.3 . . ? C18 C19 N4 109.5(9) . . ? C18 C19 H19 125.3 . . ? N4 C19 H19 125.3 . . ? C21 C20 N3 112.2(10) . . ? C21 C20 H20A 109.2 . . ? N3 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? N3 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 N4 118.2(13) . . ? C23 C22 H22A 107.8 . . ? N4 C22 H22A 107.8 . . ? C23 C22 H22B 107.8 . . ? N4 C22 H22B 107.8 . . ? H22A C22 H22B 107.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? I3 I2 I1 176.23(4) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 1.263 _refine_diff_density_min -2.389 _refine_diff_density_rms 0.190 data_andy2x _database_code_depnum_ccdc_archive 'CCDC 756623' #TrackingRef 'andy2x.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H46 N8 Pt2, 2(F6 P) ' _chemical_formula_sum 'C47 H46 F12 N8 P2 Pt2' _chemical_formula_weight 1403.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.526(4) _cell_length_b 22.046(4) _cell_length_c 23.559(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9622(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 4 _cell_measurement_theta_max 80 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5424 _exptl_absorpt_coefficient_mu 12.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79069 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 65.55 _reflns_number_total 7935 _reflns_number_gt 6859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0490P)^2^+100.4080P] 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_extinction_coef ? _refine_ls_number_reflns 7935 _refine_ls_number_parameters 642 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.873469(17) 0.042731(13) 0.367875(12) 0.02077(10) Uani 1 1 d . . . Pt2 Pt 0.846115(17) -0.094329(12) 0.274035(12) 0.01979(10) Uani 1 1 d . . . N1 N 0.8134(3) 0.0080(3) 0.4307(2) 0.0257(14) Uani 1 1 d . . . N2 N 0.9487(4) -0.0136(3) 0.4014(3) 0.0379(17) Uani 1 1 d . . . N3 N 0.9953(3) 0.1159(3) 0.3173(2) 0.0222(13) Uani 1 1 d . . . N4 N 0.9257(3) 0.0815(2) 0.2523(2) 0.0182(13) Uani 1 1 d . . . N5 N 0.8159(4) -0.1332(2) 0.3466(2) 0.0208(13) Uani 1 1 d . . . N6 N 0.9416(4) -0.1428(3) 0.2962(3) 0.0290(15) Uani 1 1 d . . . N7 N 0.8852(3) 0.0026(3) 0.1876(2) 0.0229(13) Uani 1 1 d . . . N8 N 0.9010(4) -0.0864(3) 0.1530(2) 0.0233(14) Uani 1 1 d . . . C1 C 0.7747(4) 0.0903(3) 0.3567(3) 0.0154(14) Uani 1 1 d . . . C2 C 0.7613(4) 0.1357(3) 0.3196(3) 0.0285(17) Uani 1 1 d . . . H2A H 0.7974 0.1467 0.2930 0.034 Uiso 1 1 calc R . . C3 C 0.6956(5) 0.1668(4) 0.3195(4) 0.0343(19) Uani 1 1 d . . . H3A H 0.6876 0.1991 0.2935 0.041 Uiso 1 1 calc R . . C4 C 0.6425(5) 0.1502(4) 0.3575(4) 0.039(2) Uani 1 1 d . . . H4A H 0.5971 0.1702 0.3575 0.047 Uiso 1 1 calc R . . C5 C 0.6566(5) 0.1039(4) 0.3959(4) 0.038(2) Uani 1 1 d . . . H5A H 0.6210 0.0920 0.4227 0.045 Uiso 1 1 calc R . . C6 C 0.7236(5) 0.0747(4) 0.3949(3) 0.0310(18) Uani 1 1 d . . . C7 C 0.7449(4) 0.0279(3) 0.4371(3) 0.0286(18) Uani 1 1 d . . . C8 C 0.7037(5) 0.0068(4) 0.4819(3) 0.036(2) Uani 1 1 d . . . H8A H 0.6550 0.0191 0.4866 0.043 Uiso 1 1 calc R . . C9 C 0.7361(5) -0.0333(4) 0.5198(4) 0.042(2) Uani 1 1 d . . . H9A H 0.7088 -0.0484 0.5508 0.051 Uiso 1 1 calc R . . C10 C 0.8073(5) -0.0518(4) 0.5134(3) 0.0318(19) Uani 1 1 d . . . H10A H 0.8290 -0.0782 0.5403 0.038 Uiso 1 1 calc R . . C11 C 0.8466(4) -0.0308(3) 0.4666(3) 0.0262(17) Uani 1 1 d . . . C12 C 0.9202(5) -0.0439(3) 0.4503(3) 0.0297(18) Uani 1 1 d . . . C13 C 0.9654(5) -0.0855(4) 0.4784(3) 0.037(2) Uani 1 1 d . . . H13A H 0.9466 -0.1069 0.5101 0.044 Uiso 1 1 calc R . . C14 C 1.0349(6) -0.0966(4) 0.4620(4) 0.045(2) Uani 1 1 d . . . H14A H 1.0639 -0.1245 0.4826 0.054 Uiso 1 1 calc R . . C15 C 1.0630(5) -0.0664(4) 0.4146(4) 0.039(2) Uani 1 1 d . . . H15A H 1.1114 -0.0733 0.4030 0.047 Uiso 1 1 calc R . . C16 C 1.0194(5) -0.0260(4) 0.3846(3) 0.0317(18) Uani 1 1 d . . . H16A H 1.0383 -0.0064 0.3519 0.038 Uiso 1 1 calc R . . C17 C 0.9352(4) 0.0808(3) 0.3091(3) 0.0185(15) Uani 1 1 d . . . C18 C 1.0222(5) 0.1376(3) 0.2663(3) 0.0261(17) Uani 1 1 d . . . H18A H 1.0632 0.1629 0.2612 0.031 Uiso 1 1 calc R . . C19 C 0.9787(5) 0.1157(3) 0.2255(3) 0.0268(17) Uani 1 1 d . . . H19A H 0.9833 0.1223 0.1858 0.032 Uiso 1 1 calc R . . C20 C 1.0217(5) 0.1364(3) 0.3729(3) 0.0283(18) Uani 1 1 d . . . H20A H 1.0737 0.1271 0.3763 0.034 Uiso 1 1 calc R . . H20B H 0.9958 0.1144 0.4033 0.034 Uiso 1 1 calc R . . C21 C 1.0100(5) 0.2046(4) 0.3800(4) 0.038(2) Uani 1 1 d . . . H21A H 1.0408 0.2262 0.3523 0.046 Uiso 1 1 calc R . . H21B H 1.0261 0.2165 0.4185 0.046 Uiso 1 1 calc R . . C22 C 0.9309(5) 0.2255(4) 0.3718(4) 0.043(2) Uani 1 1 d . . . H22A H 0.9301 0.2704 0.3692 0.051 Uiso 1 1 calc R . . H22B H 0.9128 0.2093 0.3353 0.051 Uiso 1 1 calc R . . C23 C 0.8809(5) 0.2061(4) 0.4183(4) 0.043(2) Uani 1 1 d . . . H23A H 0.8314 0.2183 0.4088 0.052 Uiso 1 1 calc R . . H23B H 0.8954 0.2254 0.4540 0.052 Uiso 1 1 calc R . . H23C H 0.8830 0.1619 0.4224 0.052 Uiso 1 1 calc R . . C24 C 0.8634(4) 0.0535(3) 0.2246(3) 0.0247(17) Uani 1 1 d . . . H24A H 0.8379 0.0844 0.2016 0.030 Uiso 1 1 calc R . . H24B H 0.8295 0.0384 0.2538 0.030 Uiso 1 1 calc R . . C25 C 0.9224(4) -0.0458(3) 0.1128(3) 0.0244(17) Uani 1 1 d . . . H25A H 0.9413 -0.0553 0.0764 0.029 Uiso 1 1 calc R . . C26 C 0.9121(4) 0.0102(3) 0.1339(3) 0.0196(15) Uani 1 1 d . . . H26A H 0.9216 0.0476 0.1153 0.023 Uiso 1 1 calc R . . C27 C 0.8769(4) -0.0575(3) 0.2009(3) 0.0178(15) Uani 1 1 d . . . C28 C 0.8939(5) -0.1522(3) 0.1436(3) 0.0291(18) Uani 1 1 d . . . H28A H 0.8702 -0.1711 0.1769 0.035 Uiso 1 1 calc R . . H28B H 0.9425 -0.1704 0.1395 0.035 Uiso 1 1 calc R . . C29 C 0.8497(4) -0.1651(3) 0.0906(3) 0.0276(17) Uani 1 1 d . . . H29A H 0.8435 -0.2095 0.0869 0.033 Uiso 1 1 calc R . . H29B H 0.8774 -0.1510 0.0571 0.033 Uiso 1 1 calc R . . C30 C 0.7753(5) -0.1354(4) 0.0893(4) 0.038(2) Uani 1 1 d . . . H30A H 0.7808 -0.0908 0.0906 0.045 Uiso 1 1 calc R . . H30B H 0.7476 -0.1481 0.1232 0.045 Uiso 1 1 calc R . . C31 C 0.7335(6) -0.1530(4) 0.0360(4) 0.045(2) Uani 1 1 d . . . H31A H 0.6937 -0.1244 0.0302 0.054 Uiso 1 1 calc R . . H31B H 0.7142 -0.1941 0.0404 0.054 Uiso 1 1 calc R . . H31C H 0.7659 -0.1518 0.0031 0.054 Uiso 1 1 calc R . . C32 C 0.7433(4) -0.0623(3) 0.2777(3) 0.0218(16) Uani 1 1 d . . . C33 C 0.7060(4) -0.0229(3) 0.2416(3) 0.0267(17) Uani 1 1 d . . . H33A H 0.7284 -0.0100 0.2074 0.032 Uiso 1 1 calc R . . C34 C 0.6366(5) -0.0020(4) 0.2545(4) 0.034(2) Uani 1 1 d . . . H34A H 0.6132 0.0256 0.2297 0.041 Uiso 1 1 calc R . . C35 C 0.6015(5) -0.0214(4) 0.3035(4) 0.035(2) Uani 1 1 d . . . H35A H 0.5544 -0.0070 0.3123 0.042 Uiso 1 1 calc R . . C36 C 0.6365(4) -0.0623(3) 0.3395(4) 0.0296(18) Uani 1 1 d . . . H36A H 0.6124 -0.0771 0.3723 0.035 Uiso 1 1 calc R . . C37 C 0.7066(4) -0.0813(3) 0.3275(3) 0.0258(17) Uani 1 1 d . . . C38 C 0.7468(4) -0.1226(3) 0.3652(3) 0.0241(16) Uani 1 1 d . . . C39 C 0.7241(5) -0.1494(3) 0.4160(3) 0.0295(18) Uani 1 1 d . . . H39A H 0.6768 -0.1425 0.4302 0.035 Uiso 1 1 calc R . . C40 C 0.7722(5) -0.1861(4) 0.4451(3) 0.0331(19) Uani 1 1 d . . . H40A H 0.7576 -0.2043 0.4798 0.040 Uiso 1 1 calc R . . C41 C 0.8420(5) -0.1971(4) 0.4245(3) 0.0320(19) Uani 1 1 d . . . H41A H 0.8743 -0.2227 0.4447 0.038 Uiso 1 1 calc R . . C42 C 0.8628(4) -0.1695(3) 0.3736(3) 0.0261(17) Uani 1 1 d . . . C43 C 0.9342(4) -0.1755(3) 0.3452(3) 0.0270(17) Uani 1 1 d . . . C44 C 0.9903(5) -0.2103(3) 0.3660(4) 0.0339(19) Uani 1 1 d . . . H44A H 0.9841 -0.2328 0.4001 0.041 Uiso 1 1 calc R . . C45 C 1.0560(5) -0.2126(4) 0.3371(4) 0.042(2) Uani 1 1 d . . . H45A H 1.0948 -0.2364 0.3512 0.051 Uiso 1 1 calc R . . C46 C 1.0636(5) -0.1793(4) 0.2876(4) 0.040(2) Uani 1 1 d . . . H46A H 1.1075 -0.1801 0.2668 0.048 Uiso 1 1 calc R . . C47 C 1.0052(5) -0.1446(4) 0.2689(4) 0.0327(19) Uani 1 1 d . . . H47A H 1.0107 -0.1212 0.2353 0.039 Uiso 1 1 calc R . . P1 P 0.46931(11) 0.14751(8) 0.48121(8) 0.0238(4) Uani 1 1 d . . . F1 F 0.4113(3) 0.1995(3) 0.4738(2) 0.0644(18) Uani 1 1 d . . . F2 F 0.5328(3) 0.1968(2) 0.4811(2) 0.0526(15) Uani 1 1 d . . . F3 F 0.4074(3) 0.0973(3) 0.4804(2) 0.0529(15) Uani 1 1 d . . . F4 F 0.4640(3) 0.1518(2) 0.54875(18) 0.0377(11) Uani 1 1 d . . . F5 F 0.5288(3) 0.0947(2) 0.48798(18) 0.0380(12) Uani 1 1 d . . . F6 F 0.4768(2) 0.14232(19) 0.41349(17) 0.0309(10) Uani 1 1 d . . . P2 P 0.74172(13) 0.17891(9) 0.14936(9) 0.0332(5) Uani 1 1 d . . . F7 F 0.7789(3) 0.2364(2) 0.1213(2) 0.0537(15) Uani 1 1 d . . . F8 F 0.7993(3) 0.1352(3) 0.1192(2) 0.0534(14) Uani 1 1 d . . . F9 F 0.6887(3) 0.1732(2) 0.0961(2) 0.0400(11) Uani 1 1 d . . . F10 F 0.7045(3) 0.1205(2) 0.1782(2) 0.0478(13) Uani 1 1 d . . . F11 F 0.7952(3) 0.1850(2) 0.2021(2) 0.0477(13) Uani 1 1 d . . . F12 F 0.6827(3) 0.2211(2) 0.1806(2) 0.0467(13) 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 0.0194(2) 0.02262(16) 0.02031(16) -0.00100(11) 0.00245(13) -0.00383(13) Pt2 0.01804(19) 0.01825(16) 0.02306(16) 0.00306(11) 0.00134(13) 0.00068(12) N1 0.019(4) 0.034(3) 0.024(3) -0.003(3) 0.006(3) -0.010(3) N2 0.035(4) 0.045(4) 0.034(4) -0.006(3) 0.001(3) -0.007(4) N3 0.019(3) 0.024(3) 0.024(3) -0.001(2) 0.001(3) -0.003(3) N4 0.022(4) 0.010(2) 0.023(3) 0.004(2) 0.005(3) -0.001(2) N5 0.031(4) 0.017(3) 0.015(3) 0.004(2) 0.004(3) -0.007(3) N6 0.023(4) 0.033(3) 0.031(3) 0.004(3) 0.006(3) -0.001(3) N7 0.028(4) 0.017(3) 0.024(3) -0.001(2) -0.002(3) 0.002(3) N8 0.027(4) 0.022(3) 0.021(3) 0.001(2) 0.001(3) 0.002(3) C1 0.009(4) 0.024(3) 0.014(3) -0.008(2) 0.000(3) 0.001(3) C2 0.025(5) 0.031(4) 0.030(4) -0.008(3) 0.001(4) 0.004(3) C3 0.029(5) 0.035(4) 0.039(4) -0.006(3) -0.006(4) 0.008(4) C4 0.029(5) 0.046(5) 0.042(5) -0.014(4) -0.004(4) 0.007(4) C5 0.027(5) 0.043(5) 0.043(5) -0.018(4) 0.007(4) -0.009(4) C6 0.025(5) 0.037(4) 0.030(4) -0.012(3) 0.001(4) -0.002(4) C7 0.024(5) 0.035(4) 0.027(4) -0.006(3) 0.000(4) -0.013(4) C8 0.033(5) 0.042(5) 0.032(4) -0.008(4) 0.007(4) -0.014(4) C9 0.044(6) 0.049(5) 0.033(4) -0.003(4) 0.012(4) -0.025(5) C10 0.030(5) 0.039(4) 0.026(4) 0.000(3) 0.003(4) -0.014(4) C11 0.030(5) 0.029(4) 0.020(3) -0.001(3) 0.001(3) -0.014(3) C12 0.033(5) 0.034(4) 0.022(4) 0.002(3) -0.001(4) -0.013(4) C13 0.034(5) 0.047(5) 0.029(4) 0.015(4) -0.007(4) -0.009(4) C14 0.045(6) 0.052(5) 0.037(5) 0.013(4) -0.013(5) 0.006(5) C15 0.020(5) 0.051(5) 0.046(5) 0.015(4) -0.002(4) 0.001(4) C16 0.024(5) 0.039(4) 0.032(4) 0.000(3) -0.002(4) 0.002(4) C17 0.017(4) 0.016(3) 0.023(3) -0.003(3) -0.001(3) 0.005(3) C18 0.028(5) 0.021(3) 0.030(4) 0.001(3) 0.009(4) -0.006(3) C19 0.033(5) 0.025(4) 0.022(4) 0.000(3) 0.002(3) -0.003(4) C20 0.033(5) 0.029(4) 0.022(4) -0.006(3) -0.005(3) -0.008(4) C21 0.041(6) 0.033(4) 0.040(4) -0.013(4) -0.001(4) -0.013(4) C22 0.048(6) 0.028(4) 0.052(5) -0.016(4) 0.006(5) -0.003(4) C23 0.046(6) 0.029(4) 0.055(5) -0.014(4) 0.004(5) -0.001(4) C24 0.019(4) 0.024(4) 0.031(4) -0.005(3) 0.001(3) 0.004(3) C25 0.030(5) 0.024(4) 0.019(3) -0.001(3) 0.003(3) -0.006(3) C26 0.015(4) 0.026(4) 0.018(3) 0.001(3) -0.004(3) -0.002(3) C27 0.021(4) 0.017(3) 0.015(3) 0.009(3) -0.003(3) -0.001(3) C28 0.037(5) 0.014(3) 0.037(4) -0.004(3) -0.001(4) -0.003(3) C29 0.028(5) 0.024(4) 0.032(4) -0.008(3) 0.003(4) -0.005(3) C30 0.035(5) 0.028(4) 0.050(5) -0.007(4) -0.001(4) 0.005(4) C31 0.045(6) 0.046(5) 0.045(5) -0.001(4) -0.012(5) 0.001(5) C32 0.022(4) 0.017(3) 0.026(3) -0.005(3) -0.002(3) -0.005(3) C33 0.017(4) 0.028(4) 0.035(4) 0.001(3) -0.004(4) -0.001(3) C34 0.027(5) 0.029(4) 0.046(5) -0.006(4) -0.011(4) -0.004(4) C35 0.024(5) 0.035(4) 0.047(5) -0.008(4) -0.001(4) -0.005(4) C36 0.021(4) 0.028(4) 0.040(4) -0.003(3) 0.004(4) 0.003(3) C37 0.027(5) 0.019(3) 0.031(4) -0.002(3) 0.000(4) -0.003(3) C38 0.019(4) 0.027(4) 0.026(4) -0.002(3) 0.004(3) -0.010(3) C39 0.026(5) 0.032(4) 0.030(4) -0.005(3) 0.007(4) -0.004(4) C40 0.031(5) 0.034(4) 0.034(4) 0.003(3) 0.004(4) -0.011(4) C41 0.035(5) 0.028(4) 0.032(4) 0.007(3) -0.006(4) -0.002(4) C42 0.029(5) 0.016(3) 0.033(4) 0.010(3) -0.005(4) 0.004(3) C43 0.024(4) 0.022(4) 0.035(4) 0.004(3) 0.001(4) -0.004(3) C44 0.028(5) 0.026(4) 0.047(5) 0.002(3) -0.009(4) 0.005(4) C45 0.029(5) 0.039(5) 0.058(6) 0.010(4) -0.006(5) 0.011(4) C46 0.020(5) 0.040(5) 0.061(6) 0.010(4) 0.006(4) 0.012(4) C47 0.027(5) 0.029(4) 0.042(4) 0.001(3) 0.010(4) -0.006(4) P1 0.0211(11) 0.0268(9) 0.0234(9) -0.0029(7) -0.0011(8) -0.0012(8) F1 0.071(4) 0.081(4) 0.041(3) -0.018(3) -0.015(3) 0.048(4) F2 0.073(4) 0.047(3) 0.037(3) 0.014(2) -0.021(3) -0.035(3) F3 0.043(3) 0.083(4) 0.033(3) -0.006(2) 0.005(2) -0.036(3) F4 0.034(3) 0.050(3) 0.029(2) -0.009(2) -0.002(2) 0.003(2) F5 0.046(3) 0.039(3) 0.029(2) 0.0036(19) 0.009(2) 0.017(2) F6 0.032(3) 0.034(2) 0.026(2) 0.0029(17) -0.006(2) -0.005(2) P2 0.0316(13) 0.0284(10) 0.0396(11) 0.0067(9) 0.0012(10) 0.0042(9) F7 0.038(3) 0.047(3) 0.077(4) 0.025(3) -0.008(3) -0.005(3) F8 0.049(4) 0.062(3) 0.049(3) 0.002(3) 0.006(3) 0.025(3) F9 0.039(3) 0.036(2) 0.045(3) 0.001(2) -0.002(2) 0.004(2) F10 0.041(3) 0.039(3) 0.063(3) 0.020(2) 0.002(3) -0.004(2) F11 0.047(3) 0.035(3) 0.061(3) 0.004(2) -0.009(3) 0.005(2) F12 0.045(3) 0.045(3) 0.050(3) -0.002(2) 0.000(3) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C17 1.982(7) . ? Pt1 N1 2.004(6) . ? Pt1 N2 2.028(8) . ? Pt1 C1 2.125(7) . ? Pt2 C27 1.989(6) . ? Pt2 N5 1.993(5) . ? Pt2 C32 2.034(8) . ? Pt2 N6 2.132(7) . ? N1 C7 1.350(11) . ? N1 C11 1.351(10) . ? N2 C16 1.394(11) . ? N2 C12 1.432(10) . ? N3 C17 1.371(9) . ? N3 C18 1.387(9) . ? N3 C20 1.467(9) . ? N4 C17 1.348(9) . ? N4 C19 1.390(10) . ? N4 C24 1.463(10) . ? N5 C42 1.343(10) . ? N5 C38 1.371(10) . ? N6 C47 1.344(10) . ? N6 C43 1.368(9) . ? N7 C26 1.370(9) . ? N7 C27 1.371(8) . ? N7 C24 1.476(9) . ? N8 C25 1.362(9) . ? N8 C27 1.370(9) . ? N8 C28 1.474(9) . ? C1 C2 1.350(10) . ? C1 C6 1.351(11) . ? C2 C3 1.397(11) . ? C3 C4 1.379(13) . ? C4 C5 1.389(13) . ? C5 C6 1.398(12) . ? C6 C7 1.486(11) . ? C7 C8 1.383(11) . ? C8 C9 1.390(13) . ? C9 C10 1.390(13) . ? C10 C11 1.398(11) . ? C11 C12 1.447(12) . ? C12 C13 1.406(12) . ? C13 C14 1.367(13) . ? C14 C15 1.400(12) . ? C15 C16 1.395(12) . ? C18 C19 1.345(11) . ? C20 C21 1.527(11) . ? C21 C22 1.548(13) . ? C22 C23 1.498(13) . ? C25 C26 1.344(10) . ? C28 C29 1.521(11) . ? C29 C30 1.526(12) . ? C30 C31 1.525(12) . ? C32 C33 1.397(10) . ? C32 C37 1.420(10) . ? C33 C34 1.400(12) . ? C34 C35 1.391(12) . ? C35 C36 1.397(12) . ? C36 C37 1.395(11) . ? C37 C38 1.473(11) . ? C38 C39 1.399(10) . ? C39 C40 1.387(12) . ? C40 C41 1.401(12) . ? C41 C42 1.399(11) . ? C42 C43 1.487(12) . ? C43 C44 1.382(11) . ? C44 C45 1.397(13) . ? C45 C46 1.386(12) . ? C46 C47 1.396(12) . ? P1 F1 1.581(6) . ? P1 F3 1.594(5) . ? P1 F4 1.597(5) . ? P1 F2 1.602(5) . ? P1 F6 1.606(4) . ? P1 F5 1.611(5) . ? P2 F7 1.588(5) . ? P2 F11 1.595(6) . ? P2 F9 1.599(5) . ? P2 F8 1.605(6) . ? P2 F10 1.610(5) . ? P2 F12 1.614(5) . ? 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 C17 Pt1 N1 176.5(3) . . ? C17 Pt1 N2 97.8(3) . . ? N1 Pt1 N2 82.0(3) . . ? C17 Pt1 C1 101.6(3) . . ? N1 Pt1 C1 78.6(3) . . ? N2 Pt1 C1 160.5(3) . . ? C27 Pt2 N5 178.7(3) . . ? C27 Pt2 C32 99.4(3) . . ? N5 Pt2 C32 81.3(3) . . ? C27 Pt2 N6 100.3(3) . . ? N5 Pt2 N6 78.9(3) . . ? C32 Pt2 N6 160.2(3) . . ? C7 N1 C11 124.2(7) . . ? C7 N1 Pt1 118.8(5) . . ? C11 N1 Pt1 116.8(5) . . ? C16 N2 C12 118.9(7) . . ? C16 N2 Pt1 130.9(6) . . ? C12 N2 Pt1 110.2(6) . . ? C17 N3 C18 111.4(6) . . ? C17 N3 C20 124.9(6) . . ? C18 N3 C20 123.1(6) . . ? C17 N4 C19 111.4(6) . . ? C17 N4 C24 122.8(6) . . ? C19 N4 C24 125.6(6) . . ? C42 N5 C38 123.7(6) . . ? C42 N5 Pt2 118.7(5) . . ? C38 N5 Pt2 117.6(5) . . ? C47 N6 C43 118.5(7) . . ? C47 N6 Pt2 128.7(5) . . ? C43 N6 Pt2 112.8(5) . . ? C26 N7 C27 111.7(6) . . ? C26 N7 C24 123.5(6) . . ? C27 N7 C24 124.7(6) . . ? C25 N8 C27 111.2(6) . . ? C25 N8 C28 124.6(6) . . ? C27 N8 C28 123.6(6) . . ? C2 C1 C6 119.4(7) . . ? C2 C1 Pt1 127.2(5) . . ? C6 C1 Pt1 113.2(5) . . ? C1 C2 C3 121.7(8) . . ? C4 C3 C2 119.3(8) . . ? C3 C4 C5 118.9(8) . . ? C4 C5 C6 119.6(8) . . ? C1 C6 C5 121.0(8) . . ? C1 C6 C7 116.0(7) . . ? C5 C6 C7 122.9(8) . . ? N1 C7 C8 119.7(8) . . ? N1 C7 C6 113.5(7) . . ? C8 C7 C6 126.7(8) . . ? C7 C8 C9 117.7(9) . . ? C10 C9 C8 121.8(8) . . ? C9 C10 C11 118.8(8) . . ? N1 C11 C10 117.8(8) . . ? N1 C11 C12 112.9(6) . . ? C10 C11 C12 129.3(8) . . ? C13 C12 N2 117.6(8) . . ? C13 C12 C11 124.5(7) . . ? N2 C12 C11 117.9(7) . . ? C14 C13 C12 122.9(8) . . ? C13 C14 C15 119.4(8) . . ? C16 C15 C14 119.5(8) . . ? N2 C16 C15 121.7(8) . . ? N4 C17 N3 103.9(6) . . ? N4 C17 Pt1 128.5(5) . . ? N3 C17 Pt1 127.5(5) . . ? C19 C18 N3 106.3(7) . . ? C18 C19 N4 107.0(6) . . ? N3 C20 C21 110.7(6) . . ? C20 C21 C22 114.4(7) . . ? C23 C22 C21 114.2(8) . . ? N4 C24 N7 111.6(6) . . ? C26 C25 N8 107.8(6) . . ? C25 C26 N7 106.3(6) . . ? N8 C27 N7 103.0(5) . . ? N8 C27 Pt2 128.1(5) . . ? N7 C27 Pt2 128.7(5) . . ? N8 C28 C29 110.8(6) . . ? C28 C29 C30 115.0(7) . . ? C29 C30 C31 111.4(7) . . ? C33 C32 C37 116.8(7) . . ? C33 C32 Pt2 130.7(6) . . ? C37 C32 Pt2 112.3(5) . . ? C32 C33 C34 121.7(8) . . ? C35 C34 C33 120.6(8) . . ? C34 C35 C36 119.0(8) . . ? C37 C36 C35 120.3(8) . . ? C36 C37 C32 121.5(7) . . ? C36 C37 C38 122.4(7) . . ? C32 C37 C38 116.1(7) . . ? N5 C38 C39 118.9(7) . . ? N5 C38 C37 112.6(6) . . ? C39 C38 C37 128.5(7) . . ? C40 C39 C38 118.4(8) . . ? C39 C40 C41 121.6(7) . . ? C42 C41 C40 118.4(8) . . ? N5 C42 C41 119.1(7) . . ? N5 C42 C43 114.6(6) . . ? C41 C42 C43 126.3(7) . . ? N6 C43 C44 121.1(8) . . ? N6 C43 C42 115.0(7) . . ? C44 C43 C42 123.9(7) . . ? C43 C44 C45 120.3(8) . . ? C46 C45 C44 118.6(8) . . ? C45 C46 C47 118.5(8) . . ? N6 C47 C46 123.0(8) . . ? F1 P1 F3 90.8(4) . . ? F1 P1 F4 91.4(3) . . ? F3 P1 F4 90.6(3) . . ? F1 P1 F2 90.4(4) . . ? F3 P1 F2 178.5(3) . . ? F4 P1 F2 90.4(3) . . ? F1 P1 F6 90.0(3) . . ? F3 P1 F6 90.0(2) . . ? F4 P1 F6 178.4(3) . . ? F2 P1 F6 89.0(3) . . ? F1 P1 F5 179.3(3) . . ? F3 P1 F5 89.5(3) . . ? F4 P1 F5 89.2(2) . . ? F2 P1 F5 89.3(3) . . ? F6 P1 F5 89.3(2) . . ? F7 P2 F11 89.4(3) . . ? F7 P2 F9 90.1(3) . . ? F11 P2 F9 179.4(3) . . ? F7 P2 F8 90.4(3) . . ? F11 P2 F8 89.0(3) . . ? F9 P2 F8 90.7(3) . . ? F7 P2 F10 179.6(4) . . ? F11 P2 F10 90.3(3) . . ? F9 P2 F10 90.3(3) . . ? F8 P2 F10 89.5(3) . . ? F7 P2 F12 91.3(3) . . ? F11 P2 F12 91.0(3) . . ? F9 P2 F12 89.3(3) . . ? F8 P2 F12 178.3(3) . . ? F10 P2 F12 88.8(3) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 65.55 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 3.163 _refine_diff_density_min -1.752 _refine_diff_density_rms 0.174