# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H82 I2 N4 O Pt' _chemical_formula_sum 'C58 H82 I2 N4 O Pt' _chemical_formula_weight 1300.17 _chemical_compound_source synthesis 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' I I -0.3257 6.8362 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 2 21 21' _symmetry_space_group_name_Hall 'P 2bc 2' _symmetry_Int_Tables_number 18 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 10.6105(2) _cell_length_b 13.0106(2) _cell_length_c 20.7461(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2863.98(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3850 _cell_measurement_theta_min 3.3941 _cell_measurement_theta_max 74.0660 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.193 _exptl_crystal_size_mid 0.123 _exptl_crystal_size_min 0.052 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 13.343 _exptl_absorpt_correction_T_min 0.30659 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6821 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 74.23 _reflns_number_total 4885 _reflns_number_gt 3873 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SIR2004(Burla, 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _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^ > 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^)+(0.0879P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(13) _refine_ls_number_reflns 4885 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1516 _refine_ls_wR_factor_gt 0.1366 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 C1 C 0.1012(8) 0.9749(6) 0.5963(4) 0.0229(16) Uani 1 1 d . . . C2 C 0.0827(11) 0.9979(9) 0.7050(4) 0.040(2) Uani 1 1 d . . . H2 H 0.0682 1.0299 0.7444 0.049 Uiso 1 1 calc R . . C3 C 0.1224(13) 0.9014(8) 0.6961(4) 0.042(3) Uani 1 1 d . . . H3 H 0.1373 0.8521 0.7276 0.050 Uiso 1 1 calc R . . C4 C 0.1767(12) 0.7903(7) 0.6053(4) 0.031(2) Uani 1 1 d . . . C5 C 0.3028(12) 0.7604(7) 0.6104(4) 0.031(2) Uani 1 1 d . . . C6 C 0.3347(11) 0.6594(8) 0.5929(5) 0.038(2) Uani 1 1 d . . . H6 H 0.4182 0.6379 0.5945 0.046 Uiso 1 1 calc R . . C7 C 0.2408(12) 0.5919(7) 0.5734(5) 0.040(2) Uani 1 1 d . . . H7 H 0.2622 0.5245 0.5632 0.048 Uiso 1 1 calc R . . C8 C 0.1194(12) 0.6218(7) 0.5687(5) 0.038(2) Uani 1 1 d . . . H8 H 0.0595 0.5753 0.5538 0.046 Uiso 1 1 calc R . . C9 C 0.0812(11) 0.7226(7) 0.5860(4) 0.034(2) Uani 1 1 d . . . C10 C 0.4083(12) 0.8324(8) 0.6357(6) 0.042(3) Uani 1 1 d . . . H10 H 0.3797 0.9038 0.6321 0.051 Uiso 1 1 calc R . . C11 C 0.5312(13) 0.8196(9) 0.5966(8) 0.056(3) Uani 1 1 d . . . H11A H 0.5982 0.8562 0.6175 0.084 Uiso 1 1 calc R . . H11B H 0.5192 0.8467 0.5539 0.084 Uiso 1 1 calc R . . H11C H 0.5524 0.7480 0.5939 0.084 Uiso 1 1 calc R . . C12 C 0.4359(16) 0.8087(11) 0.7066(6) 0.059(3) Uani 1 1 d . . . H12A H 0.4400 0.7356 0.7126 0.089 Uiso 1 1 calc R . . H12B H 0.3700 0.8366 0.7330 0.089 Uiso 1 1 calc R . . H12C H 0.5150 0.8389 0.7186 0.089 Uiso 1 1 calc R . . C13 C -0.0567(12) 0.7486(9) 0.5880(4) 0.041(3) Uani 1 1 d . . . H13 H -0.0638 0.8236 0.5895 0.049 Uiso 1 1 calc R . . C14 C -0.1292(15) 0.7118(10) 0.5291(5) 0.057(3) Uani 1 1 d . . . H14A H -0.0955 0.7439 0.4912 0.085 Uiso 1 1 calc R . . H14B H -0.2165 0.7297 0.5336 0.085 Uiso 1 1 calc R . . H14C H -0.1213 0.6385 0.5254 0.085 Uiso 1 1 calc R . . C15 C -0.1198(17) 0.7056(12) 0.6498(6) 0.056(4) Uani 1 1 d . . . H15A H -0.1077 0.6326 0.6517 0.084 Uiso 1 1 calc R . . H15B H -0.2084 0.7206 0.6489 0.084 Uiso 1 1 calc R . . H15C H -0.0824 0.7371 0.6871 0.084 Uiso 1 1 calc R . . C16 C 0.0204(11) 1.1481(7) 0.6405(4) 0.030(2) Uani 1 1 d . . . C17 C -0.1040(12) 1.1680(7) 0.6518(4) 0.034(2) Uani 1 1 d . . . C18 C -0.1402(14) 1.2711(9) 0.6510(5) 0.044(3) Uani 1 1 d . . . H18 H -0.2242 1.2878 0.6585 0.053 Uiso 1 1 calc R . . C19 C -0.0549(12) 1.3491(8) 0.6395(5) 0.040(2) Uani 1 1 d . . . H19 H -0.0818 1.4171 0.6383 0.048 Uiso 1 1 calc R . . C20 C 0.0696(11) 1.3258(7) 0.6299(5) 0.038(2) Uani 1 1 d . . . H20 H 0.1263 1.3791 0.6228 0.045 Uiso 1 1 calc R . . C21 C 0.1148(12) 1.2247(7) 0.6304(4) 0.035(2) Uani 1 1 d . . . C22 C -0.2028(11) 1.0863(8) 0.6675(5) 0.040(2) Uani 1 1 d . . . H22 H -0.1724 1.0203 0.6509 0.047 Uiso 1 1 calc R . . C23 C -0.2180(17) 1.0763(11) 0.7414(6) 0.064(4) Uani 1 1 d . . . H23A H -0.1424 1.0479 0.7596 0.096 Uiso 1 1 calc R . . H23B H -0.2879 1.0319 0.7509 0.096 Uiso 1 1 calc R . . H23C H -0.2332 1.1430 0.7597 0.096 Uiso 1 1 calc R . . C24 C -0.3293(13) 1.1082(12) 0.6369(8) 0.062(4) Uani 1 1 d . . . H24A H -0.3623 1.1715 0.6536 0.093 Uiso 1 1 calc R . . H24B H -0.3865 1.0532 0.6466 0.093 Uiso 1 1 calc R . . H24C H -0.3194 1.1137 0.5910 0.093 Uiso 1 1 calc R . . C25 C 0.2501(13) 1.1997(8) 0.6266(4) 0.039(2) Uani 1 1 d . . . H25 H 0.2577 1.1281 0.6125 0.047 Uiso 1 1 calc R . . C26 C 0.3221(16) 1.2674(10) 0.5773(8) 0.060(3) Uani 1 1 d . . . H26A H 0.2770 1.2683 0.5372 0.090 Uiso 1 1 calc R . . H26B H 0.4049 1.2396 0.5705 0.090 Uiso 1 1 calc R . . H26C H 0.3290 1.3362 0.5937 0.090 Uiso 1 1 calc R . . C27 C 0.3124(15) 1.2088(18) 0.6936(7) 0.089(7) Uani 1 1 d . . . H27A H 0.3031 1.2777 0.7093 0.133 Uiso 1 1 calc R . . H27B H 0.4003 1.1923 0.6902 0.133 Uiso 1 1 calc R . . H27C H 0.2725 1.1619 0.7229 0.133 Uiso 1 1 calc R . . C28 C 0.6419(19) 0.473(2) 0.5584(9) 0.106(9) Uani 1 1 d . . . H28A H 0.7140 0.5186 0.5622 0.127 Uiso 1 1 calc R . . H28B H 0.6770 0.4054 0.5506 0.127 Uiso 1 1 calc R . . C29 C 0.594(2) 0.4668(15) 0.6225(9) 0.096(6) Uani 1 1 d . . . H29A H 0.6190 0.5266 0.6464 0.143 Uiso 1 1 calc R . . H29B H 0.6265 0.4064 0.6432 0.143 Uiso 1 1 calc R . . H29C H 0.5034 0.4631 0.6212 0.143 Uiso 1 1 calc R . . N1 N 0.0672(9) 1.0414(6) 0.6446(3) 0.0296(17) Uani 1 1 d . . . N2 N 0.1370(9) 0.8901(6) 0.6293(4) 0.0302(17) Uani 1 1 d . . . I1 I 0.34464(7) 1.0000 0.5000 0.02938(19) Uani 1 2 d S . . I2 I -0.14471(7) 1.0000 0.5000 0.03146(19) Uani 1 2 d S . . Pt1 Pt 0.10009(4) 1.0000 0.5000 0.02039(15) Uani 1 2 d S . . O1 O 0.5885(18) 0.5000 0.5000 0.100(5) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(4) 0.022(4) 0.031(4) 0.000(3) -0.002(3) 0.001(3) C2 0.066(6) 0.035(4) 0.021(3) -0.008(4) -0.006(3) 0.009(8) C3 0.073(8) 0.031(4) 0.021(3) 0.005(3) -0.002(4) 0.011(5) C4 0.042(6) 0.025(4) 0.027(3) 0.001(3) 0.004(4) -0.004(4) C5 0.042(6) 0.024(4) 0.029(4) 0.001(3) 0.003(4) 0.006(4) C6 0.032(6) 0.030(5) 0.053(5) 0.004(4) 0.011(4) 0.009(4) C7 0.048(7) 0.020(4) 0.052(5) -0.003(4) 0.013(5) 0.004(4) C8 0.044(6) 0.027(4) 0.043(4) 0.003(3) 0.001(5) 0.000(5) C9 0.041(6) 0.027(4) 0.035(4) 0.004(3) 0.006(4) -0.004(5) C10 0.041(7) 0.024(4) 0.062(6) 0.009(4) 0.000(5) -0.001(5) C11 0.036(7) 0.035(6) 0.096(10) 0.009(6) -0.007(7) 0.002(5) C12 0.059(9) 0.053(7) 0.065(7) 0.017(6) -0.021(7) -0.008(7) C13 0.051(7) 0.045(6) 0.026(4) -0.002(4) -0.003(4) 0.001(5) C14 0.071(10) 0.058(7) 0.041(5) -0.007(5) -0.016(6) -0.003(7) C15 0.044(8) 0.078(9) 0.047(5) 0.017(6) 0.002(6) -0.007(8) C16 0.047(6) 0.019(4) 0.024(3) -0.007(3) -0.004(4) 0.005(4) C17 0.047(7) 0.024(4) 0.029(4) -0.005(3) 0.002(4) 0.009(5) C18 0.055(9) 0.039(6) 0.038(4) -0.006(4) 0.003(5) 0.023(5) C19 0.053(7) 0.028(5) 0.038(5) -0.003(3) -0.002(5) 0.005(5) C20 0.040(6) 0.024(4) 0.049(5) -0.004(4) -0.005(4) -0.004(4) C21 0.050(7) 0.028(4) 0.028(4) -0.006(3) -0.010(4) 0.006(5) C22 0.035(6) 0.037(5) 0.047(5) -0.011(4) 0.016(5) 0.001(5) C23 0.079(12) 0.050(7) 0.064(7) 0.001(5) 0.029(7) -0.012(7) C24 0.028(6) 0.070(9) 0.087(9) -0.041(8) 0.011(6) -0.010(6) C25 0.050(7) 0.034(5) 0.034(4) -0.003(4) -0.008(5) 0.002(5) C26 0.051(8) 0.042(6) 0.087(9) 0.006(6) 0.012(8) -0.012(6) C27 0.030(7) 0.17(2) 0.062(7) -0.049(10) -0.005(6) 0.017(11) C28 0.055(10) 0.17(3) 0.090(11) 0.007(13) 0.011(8) 0.014(14) C29 0.095(15) 0.084(12) 0.108(13) 0.022(10) -0.008(11) 0.053(11) N1 0.041(5) 0.022(3) 0.026(3) -0.003(3) -0.004(3) 0.008(3) N2 0.034(5) 0.029(4) 0.028(3) 0.003(3) 0.005(3) 0.008(3) I1 0.0256(4) 0.0320(3) 0.0305(3) -0.0005(7) 0.000 0.000 I2 0.0247(4) 0.0379(4) 0.0317(3) 0.0027(8) 0.000 0.000 Pt1 0.0235(2) 0.0175(2) 0.0202(2) -0.00066(18) 0.000 0.000 O1 0.079(12) 0.111(14) 0.110(13) 0.010(14) 0.000 0.000 _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 C1 N2 1.354(11) . ? C1 N1 1.373(10) . ? C1 Pt1 2.024(7) . ? C2 C3 1.337(15) . ? C2 N1 1.383(11) . ? C2 H2 0.9300 . ? C3 N2 1.401(11) . ? C3 H3 0.9300 . ? C4 C5 1.397(17) . ? C4 C9 1.402(16) . ? C4 N2 1.454(12) . ? C5 C6 1.404(13) . ? C5 C10 1.552(16) . ? C6 C7 1.389(17) . ? C6 H6 0.9300 . ? C7 C8 1.349(18) . ? C7 H7 0.9300 . ? C8 C9 1.418(14) . ? C8 H8 0.9300 . ? C9 C13 1.502(18) . ? C10 C12 1.531(17) . ? C10 C11 1.545(19) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.520(14) . ? C13 C15 1.551(16) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.366(17) . ? C16 C21 1.428(16) . ? C16 N1 1.476(11) . ? C17 C18 1.396(14) . ? C17 C22 1.528(16) . ? C18 C19 1.381(19) . ? C18 H18 0.9300 . ? C19 C20 1.371(18) . ? C19 H19 0.9300 . ? C20 C21 1.400(14) . ? C20 H20 0.9300 . ? C21 C25 1.474(18) . ? C22 C24 1.51(2) . ? C22 C23 1.548(16) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C27 1.544(16) . ? C25 C26 1.550(18) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 O1 1.38(2) . ? C28 C29 1.43(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? I1 Pt1 2.5948(9) . ? I2 Pt1 2.5974(8) . ? Pt1 C1 2.024(7) 3_576 ? O1 C28 1.38(2) 3_566 ? 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 N2 C1 N1 102.6(6) . . ? N2 C1 Pt1 129.3(6) . . ? N1 C1 Pt1 128.2(6) . . ? C3 C2 N1 107.3(7) . . ? C3 C2 H2 126.4 . . ? N1 C2 H2 126.4 . . ? C2 C3 N2 105.7(8) . . ? C2 C3 H3 127.2 . . ? N2 C3 H3 127.2 . . ? C5 C4 C9 122.6(9) . . ? C5 C4 N2 120.1(10) . . ? C9 C4 N2 116.7(11) . . ? C4 C5 C6 118.2(10) . . ? C4 C5 C10 123.2(9) . . ? C6 C5 C10 118.6(11) . . ? C7 C6 C5 119.7(11) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C8 C7 C6 121.5(10) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 121.5(11) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C4 C9 C8 116.5(11) . . ? C4 C9 C13 123.7(9) . . ? C8 C9 C13 119.6(10) . . ? C12 C10 C11 108.7(12) . . ? C12 C10 C5 110.0(9) . . ? C11 C10 C5 111.4(10) . . ? C12 C10 H10 108.9 . . ? C11 C10 H10 108.9 . . ? C5 C10 H10 108.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 113.5(10) . . ? C9 C13 C15 111.3(10) . . ? C14 C13 C15 109.4(11) . . ? C9 C13 H13 107.5 . . ? C14 C13 H13 107.5 . . ? C15 C13 H13 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 124.8(9) . . ? C17 C16 N1 119.5(9) . . ? C21 C16 N1 115.4(9) . . ? C16 C17 C18 116.5(11) . . ? C16 C17 C22 124.6(9) . . ? C18 C17 C22 118.8(11) . . ? C19 C18 C17 121.9(13) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C20 C19 C18 119.6(10) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 122.5(11) . . ? C19 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C20 C21 C16 114.6(11) . . ? C20 C21 C25 122.7(11) . . ? C16 C21 C25 122.5(9) . . ? C24 C22 C17 112.9(11) . . ? C24 C22 C23 109.8(11) . . ? C17 C22 C23 109.9(10) . . ? C24 C22 H22 108.0 . . ? C17 C22 H22 108.0 . . ? C23 C22 H22 108.0 . . ? 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 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 110.6(10) . . ? C21 C25 C26 113.0(11) . . ? C27 C25 C26 109.8(13) . . ? C21 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1 C28 C29 133.2(19) . . ? O1 C28 H28A 103.9 . . ? C29 C28 H28A 103.9 . . ? O1 C28 H28B 103.9 . . ? C29 C28 H28B 103.9 . . ? H28A C28 H28B 105.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C1 N1 C2 111.8(7) . . ? C1 N1 C16 129.7(7) . . ? C2 N1 C16 118.5(7) . . ? C1 N2 C3 112.6(8) . . ? C1 N2 C4 129.5(7) . . ? C3 N2 C4 117.7(8) . . ? C1 Pt1 C1 179.3(5) 3_576 . ? C1 Pt1 I1 89.7(2) 3_576 . ? C1 Pt1 I1 89.7(2) . . ? C1 Pt1 I2 90.3(2) 3_576 . ? C1 Pt1 I2 90.3(2) . . ? I1 Pt1 I2 180.0 . . ? C28 O1 C28 132(2) . 3_566 ? 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 N1 C2 C3 N2 3.2(14) . . . . ? C9 C4 C5 C6 2.4(13) . . . . ? N2 C4 C5 C6 173.3(8) . . . . ? C9 C4 C5 C10 -176.1(8) . . . . ? N2 C4 C5 C10 -5.2(13) . . . . ? C4 C5 C6 C7 -2.0(14) . . . . ? C10 C5 C6 C7 176.6(9) . . . . ? C5 C6 C7 C8 2.1(15) . . . . ? C6 C7 C8 C9 -2.5(15) . . . . ? C5 C4 C9 C8 -2.7(13) . . . . ? N2 C4 C9 C8 -173.9(8) . . . . ? C5 C4 C9 C13 172.1(9) . . . . ? N2 C4 C9 C13 0.9(12) . . . . ? C7 C8 C9 C4 2.7(14) . . . . ? C7 C8 C9 C13 -172.3(9) . . . . ? C4 C5 C10 C12 99.1(12) . . . . ? C6 C5 C10 C12 -79.4(13) . . . . ? C4 C5 C10 C11 -140.3(10) . . . . ? C6 C5 C10 C11 41.3(12) . . . . ? C4 C9 C13 C14 138.6(10) . . . . ? C8 C9 C13 C14 -46.8(13) . . . . ? C4 C9 C13 C15 -97.4(12) . . . . ? C8 C9 C13 C15 77.2(12) . . . . ? C21 C16 C17 C18 2.3(13) . . . . ? N1 C16 C17 C18 176.1(8) . . . . ? C21 C16 C17 C22 -175.2(8) . . . . ? N1 C16 C17 C22 -1.4(13) . . . . ? C16 C17 C18 C19 0.0(14) . . . . ? C22 C17 C18 C19 177.7(9) . . . . ? C17 C18 C19 C20 -1.5(16) . . . . ? C18 C19 C20 C21 0.9(16) . . . . ? C19 C20 C21 C16 1.1(14) . . . . ? C19 C20 C21 C25 -173.8(9) . . . . ? C17 C16 C21 C20 -2.8(13) . . . . ? N1 C16 C21 C20 -176.9(8) . . . . ? C17 C16 C21 C25 172.1(9) . . . . ? N1 C16 C21 C25 -2.0(12) . . . . ? C16 C17 C22 C24 -142.5(10) . . . . ? C18 C17 C22 C24 40.1(12) . . . . ? C16 C17 C22 C23 94.5(12) . . . . ? C18 C17 C22 C23 -82.9(13) . . . . ? C20 C21 C25 C27 82.1(15) . . . . ? C16 C21 C25 C27 -92.4(14) . . . . ? C20 C21 C25 C26 -41.4(13) . . . . ? C16 C21 C25 C26 144.0(10) . . . . ? N2 C1 N1 C2 0.3(11) . . . . ? Pt1 C1 N1 C2 -178.8(7) . . . . ? N2 C1 N1 C16 179.4(10) . . . . ? Pt1 C1 N1 C16 0.3(16) . . . . ? C3 C2 N1 C1 -2.3(14) . . . . ? C3 C2 N1 C16 178.5(10) . . . . ? C17 C16 N1 C1 106.0(12) . . . . ? C21 C16 N1 C1 -79.6(12) . . . . ? C17 C16 N1 C2 -75.0(12) . . . . ? C21 C16 N1 C2 99.4(11) . . . . ? N1 C1 N2 C3 1.8(12) . . . . ? Pt1 C1 N2 C3 -179.1(8) . . . . ? N1 C1 N2 C4 176.2(11) . . . . ? Pt1 C1 N2 C4 -4.7(16) . . . . ? C2 C3 N2 C1 -3.2(15) . . . . ? C2 C3 N2 C4 -178.4(11) . . . . ? C5 C4 N2 C1 108.7(12) . . . . ? C9 C4 N2 C1 -79.8(13) . . . . ? C5 C4 N2 C3 -77.1(13) . . . . ? C9 C4 N2 C3 94.4(12) . . . . ? N2 C1 Pt1 C1 -69.0(8) . . . 3_576 ? N1 C1 Pt1 C1 109.8(9) . . . 3_576 ? N2 C1 Pt1 I1 -69.1(8) . . . . ? N1 C1 Pt1 I1 109.8(8) . . . . ? N2 C1 Pt1 I2 110.9(8) . . . . ? N1 C1 Pt1 I2 -70.2(8) . . . . ? C29 C28 O1 C28 164(4) . . . 3_566 ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 74.23 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 2.721 _refine_diff_density_min -2.256 _refine_diff_density_rms 0.193 _database_code_depnum_ccdc_archive 'CCDC 969273' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H84 I2 N4 Pt, B F24' _chemical_formula_sum 'C86 H84 B F24 I2 N4 Pt' _chemical_formula_weight 2089.27 _chemical_compound_source synthesis 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' B B 0.0090 0.0039 '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' I I -0.3257 6.8362 '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' Pt Pt -4.5932 6.9264 '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 2/n' _symmetry_space_group_name_Hall '-P 2yac' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 19.6292(2) _cell_length_b 21.8184(2) _cell_length_c 20.7055(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.328(1) _cell_angle_gamma 90.00 _cell_volume 8842.42(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19660 _cell_measurement_theta_min 2.9442 _cell_measurement_theta_max 74.4940 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.087 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.028 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4132 _exptl_absorpt_coefficient_mu 9.286 _exptl_absorpt_correction_T_min 0.52531 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37621 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 74.66 _reflns_number_total 17385 _reflns_number_gt 14372 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SIR2004(Burla, 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _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^ > 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^)+(0.0758P)^2^+4.9860P] 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 17385 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _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 C1 C 0.78710(18) 0.49638(17) 0.15911(18) 0.0228(7) Uani 1 1 d . . . C2 C 0.84579(19) 0.4669(2) 0.07436(18) 0.0304(8) Uani 1 1 d . . . H2 H 0.8694 0.4425 0.0467 0.036 Uiso 1 1 calc R . . C3 C 0.83281(19) 0.5269(2) 0.06753(18) 0.0294(8) Uani 1 1 d . . . H3 H 0.8461 0.5520 0.0344 0.035 Uiso 1 1 calc R . . C4 C 0.76651(19) 0.60574(19) 0.12083(18) 0.0264(8) Uani 1 1 d . . . C5 C 0.80464(19) 0.6521(2) 0.15309(19) 0.0288(8) Uani 1 1 d . . . C6 C 0.7773(2) 0.7113(2) 0.1503(2) 0.0347(9) Uani 1 1 d . . . H6 H 0.8009 0.7432 0.1717 0.042 Uiso 1 1 calc R . . C7 C 0.7153(2) 0.7230(2) 0.1160(2) 0.0381(9) Uani 1 1 d . . . H7 H 0.6972 0.7624 0.1153 0.046 Uiso 1 1 calc R . . C8 C 0.6801(2) 0.6761(2) 0.0827(2) 0.0362(9) Uani 1 1 d . . . H8 H 0.6391 0.6850 0.0591 0.043 Uiso 1 1 calc R . . C9 C 0.7045(2) 0.6165(2) 0.08390(19) 0.0298(8) Uani 1 1 d . . . C10 C 0.87500(19) 0.6416(2) 0.18665(19) 0.0302(8) Uani 1 1 d . . . H10 H 0.8820 0.5973 0.1908 0.036 Uiso 1 1 calc R . . C11 C 0.9300(2) 0.6670(2) 0.1445(2) 0.0393(10) Uani 1 1 d . . . H11A H 0.9251 0.6483 0.1024 0.059 Uiso 1 1 calc R . . H11B H 0.9745 0.6581 0.1646 0.059 Uiso 1 1 calc R . . H11C H 0.9246 0.7106 0.1400 0.059 Uiso 1 1 calc R . . C12 C 0.8821(2) 0.6692(2) 0.2545(2) 0.0405(10) Uani 1 1 d . . . H12A H 0.8809 0.7131 0.2514 0.061 Uiso 1 1 calc R . . H12B H 0.9247 0.6566 0.2762 0.061 Uiso 1 1 calc R . . H12C H 0.8451 0.6553 0.2785 0.061 Uiso 1 1 calc R . . C13 C 0.6676(2) 0.5666(2) 0.04410(19) 0.0338(9) Uani 1 1 d . . . H13 H 0.6796 0.5271 0.0644 0.041 Uiso 1 1 calc R . . C14 C 0.6908(2) 0.5654(3) -0.0253(2) 0.0438(11) Uani 1 1 d . . . H14A H 0.6800 0.6039 -0.0461 0.066 Uiso 1 1 calc R . . H14B H 0.6677 0.5330 -0.0493 0.066 Uiso 1 1 calc R . . H14C H 0.7393 0.5587 -0.0237 0.066 Uiso 1 1 calc R . . C15 C 0.5899(2) 0.5730(3) 0.0411(2) 0.0441(11) Uani 1 1 d . . . H15A H 0.5757 0.5788 0.0840 0.066 Uiso 1 1 calc R . . H15B H 0.5691 0.5366 0.0226 0.066 Uiso 1 1 calc R . . H15C H 0.5762 0.6078 0.0147 0.066 Uiso 1 1 calc R . . C16 C 0.8155(2) 0.38491(19) 0.15069(19) 0.0257(8) Uani 1 1 d . . . C17 C 0.8754(2) 0.3567(2) 0.1778(2) 0.0290(8) Uani 1 1 d . . . C18 C 0.8707(2) 0.2966(2) 0.1979(2) 0.0326(8) Uani 1 1 d . . . H18 H 0.9095 0.2771 0.2168 0.039 Uiso 1 1 calc R . . C19 C 0.8095(2) 0.2644(2) 0.1908(2) 0.0354(9) Uani 1 1 d . . . H19 H 0.8069 0.2246 0.2065 0.043 Uiso 1 1 calc R . . C20 C 0.7521(2) 0.2924(2) 0.1599(2) 0.0337(9) Uani 1 1 d . . . H20 H 0.7117 0.2702 0.1538 0.040 Uiso 1 1 calc R . . C21 C 0.75346(19) 0.3519(2) 0.13832(19) 0.0278(8) Uani 1 1 d . . . C22 C 0.9460(2) 0.3869(2) 0.1776(2) 0.0314(9) Uani 1 1 d . . . H22 H 0.9398 0.4313 0.1722 0.038 Uiso 1 1 calc R . . C23 C 0.9812(2) 0.3620(2) 0.1194(2) 0.0394(10) Uani 1 1 d . . . H23A H 0.9828 0.3181 0.1215 0.059 Uiso 1 1 calc R . . H23B H 1.0269 0.3780 0.1203 0.059 Uiso 1 1 calc R . . H23C H 0.9560 0.3744 0.0800 0.059 Uiso 1 1 calc R . . C24 C 0.9915(2) 0.3752(2) 0.2394(2) 0.0382(10) Uani 1 1 d . . . H24A H 1.0016 0.3322 0.2430 0.057 Uiso 1 1 calc R . . H24B H 0.9683 0.3882 0.2762 0.057 Uiso 1 1 calc R . . H24C H 1.0333 0.3978 0.2378 0.057 Uiso 1 1 calc R . . C25 C 0.6937(2) 0.3789(2) 0.0968(2) 0.0337(9) Uani 1 1 d . . . H25 H 0.6929 0.4232 0.1047 0.040 Uiso 1 1 calc R . . C26 C 0.7041(3) 0.3687(3) 0.0248(2) 0.0491(12) Uani 1 1 d . . . H26A H 0.7471 0.3860 0.0150 0.074 Uiso 1 1 calc R . . H26B H 0.6678 0.3883 -0.0012 0.074 Uiso 1 1 calc R . . H26C H 0.7039 0.3256 0.0157 0.074 Uiso 1 1 calc R . . C27 C 0.6248(2) 0.3525(2) 0.1131(3) 0.0431(11) Uani 1 1 d . . . H27A H 0.6194 0.3121 0.0951 0.065 Uiso 1 1 calc R . . H27B H 0.5886 0.3783 0.0951 0.065 Uiso 1 1 calc R . . H27C H 0.6232 0.3504 0.1593 0.065 Uiso 1 1 calc R . . C28 C 0.27761(19) 0.8827(2) 0.1559(2) 0.0329(9) Uani 1 1 d . . . C29 C 0.2934(2) 0.8516(3) 0.0542(2) 0.0476(13) Uani 1 1 d . . . H29 H 0.2953 0.8265 0.0180 0.057 Uiso 1 1 calc R . . C30 C 0.3087(2) 0.9117(3) 0.0578(2) 0.0462(12) Uani 1 1 d . . . H30 H 0.3226 0.9362 0.0244 0.055 Uiso 1 1 calc R . . C31 C 0.3147(3) 0.9923(2) 0.1420(3) 0.0451(12) Uani 1 1 d . . . C32 C 0.3824(3) 1.0093(2) 0.1564(3) 0.0451(11) Uani 1 1 d . . . C33 C 0.3939(4) 1.0699(3) 0.1741(4) 0.0693(18) Uani 1 1 d . . . H33 H 0.4385 1.0830 0.1845 0.083 Uiso 1 1 calc R . . C34 C 0.3407(5) 1.1115(3) 0.1766(4) 0.091(3) Uani 1 1 d . . . H34 H 0.3497 1.1515 0.1900 0.109 Uiso 1 1 calc R . . C35 C 0.2748(4) 1.0937(3) 0.1592(4) 0.084(2) Uani 1 1 d . . . H35 H 0.2398 1.1224 0.1600 0.100 Uiso 1 1 calc R . . C36 C 0.2590(3) 1.0336(3) 0.1404(3) 0.0583(16) Uani 1 1 d . . . C37 C 0.4426(2) 0.9661(2) 0.1490(2) 0.0406(10) Uani 1 1 d . . . H37 H 0.4257 0.9239 0.1503 0.049 Uiso 1 1 calc R . . C38 C 0.5002(3) 0.9731(3) 0.2021(3) 0.0548(14) Uani 1 1 d . . . H38A H 0.5237 1.0111 0.1962 0.082 Uiso 1 1 calc R . . H38B H 0.5316 0.9396 0.1999 0.082 Uiso 1 1 calc R . . H38C H 0.4815 0.9732 0.2436 0.082 Uiso 1 1 calc R . . C39 C 0.4717(2) 0.9762(3) 0.0835(2) 0.0530(14) Uani 1 1 d . . . H39A H 0.4895 1.0171 0.0815 0.080 Uiso 1 1 calc R . . H39B H 0.4363 0.9706 0.0495 0.080 Uiso 1 1 calc R . . H39C H 0.5077 0.9473 0.0782 0.080 Uiso 1 1 calc R . . C40 C 0.1892(3) 1.0165(3) 0.1133(3) 0.069(2) Uani 1 1 d . . . H40 H 0.1854 0.9718 0.1163 0.082 Uiso 1 1 calc R . . C41 C 0.1327(3) 1.0437(4) 0.1508(5) 0.101(3) Uani 1 1 d . . . H41A H 0.1403 1.0330 0.1957 0.152 Uiso 1 1 calc R . . H41B H 0.0894 1.0279 0.1339 0.152 Uiso 1 1 calc R . . H41C H 0.1329 1.0875 0.1463 0.152 Uiso 1 1 calc R . . C42 C 0.1782(4) 1.0340(5) 0.0393(4) 0.105(4) Uani 1 1 d . . . H42A H 0.1705 1.0773 0.0352 0.158 Uiso 1 1 calc R . . H42B H 0.1393 1.0123 0.0199 0.158 Uiso 1 1 calc R . . H42C H 0.2180 1.0229 0.0178 0.158 Uiso 1 1 calc R . . C43 C 0.2586(2) 0.7712(2) 0.1291(2) 0.0352(9) Uani 1 1 d . . . C44 C 0.3106(2) 0.7355(3) 0.1603(2) 0.0419(11) Uani 1 1 d . . . C45 C 0.2943(3) 0.6759(3) 0.1755(3) 0.0519(13) Uani 1 1 d . . . H45 H 0.3271 0.6515 0.1977 0.062 Uiso 1 1 calc R . . C46 C 0.2304(3) 0.6517(3) 0.1585(3) 0.0584(14) Uani 1 1 d . . . H46 H 0.2204 0.6117 0.1700 0.070 Uiso 1 1 calc R . . C47 C 0.1816(3) 0.6868(3) 0.1244(3) 0.0523(13) Uani 1 1 d . . . H47 H 0.1393 0.6696 0.1121 0.063 Uiso 1 1 calc R . . C48 C 0.1940(2) 0.7472(3) 0.1080(2) 0.0439(11) Uani 1 1 d . . . C49 C 0.3837(2) 0.7587(3) 0.1708(2) 0.0440(11) Uani 1 1 d . . . H49 H 0.3823 0.8034 0.1754 0.053 Uiso 1 1 calc R . . C50 C 0.4221(3) 0.7435(3) 0.1111(3) 0.0598(15) Uani 1 1 d . . . H50A H 0.4249 0.6998 0.1062 0.090 Uiso 1 1 calc R . . H50B H 0.4674 0.7604 0.1163 0.090 Uiso 1 1 calc R . . H50C H 0.3982 0.7608 0.0732 0.090 Uiso 1 1 calc R . . C51 C 0.4217(3) 0.7319(3) 0.2321(3) 0.0530(13) Uani 1 1 d . . . H51A H 0.3943 0.7371 0.2682 0.079 Uiso 1 1 calc R . . H51B H 0.4644 0.7529 0.2406 0.079 Uiso 1 1 calc R . . H51C H 0.4300 0.6891 0.2257 0.079 Uiso 1 1 calc R . . C52 C 0.1434(2) 0.7815(3) 0.0626(2) 0.0480(12) Uani 1 1 d . . . H52 H 0.1532 0.8255 0.0661 0.058 Uiso 1 1 calc R . . C53 C 0.1526(3) 0.7605(4) -0.0073(3) 0.069(2) Uani 1 1 d . . . H53A H 0.1988 0.7681 -0.0174 0.104 Uiso 1 1 calc R . . H53B H 0.1218 0.7829 -0.0368 0.104 Uiso 1 1 calc R . . H53C H 0.1431 0.7175 -0.0112 0.104 Uiso 1 1 calc R . . C54 C 0.0684(2) 0.7706(3) 0.0765(3) 0.0584(15) Uani 1 1 d . . . H54A H 0.0552 0.7297 0.0639 0.088 Uiso 1 1 calc R . . H54B H 0.0397 0.7995 0.0524 0.088 Uiso 1 1 calc R . . H54C H 0.0634 0.7759 0.1220 0.088 Uiso 1 1 calc R . . C55 C 0.26070(18) 0.35510(18) 0.18932(17) 0.0247(7) Uani 1 1 d . . . C56 C 0.32587(19) 0.33457(19) 0.17545(18) 0.0262(8) Uani 1 1 d . . . H56 H 0.3640 0.3500 0.1995 0.031 Uiso 1 1 calc R . . C57 C 0.33537(19) 0.2921(2) 0.12717(19) 0.0293(8) Uani 1 1 d . . . C58 C 0.2799(2) 0.2675(2) 0.0897(2) 0.0310(8) Uani 1 1 d . . . H58 H 0.2864 0.2395 0.0568 0.037 Uiso 1 1 calc R . . C59 C 0.2149(2) 0.2862(2) 0.1030(2) 0.0325(9) Uani 1 1 d . . . C60 C 0.20580(19) 0.3290(2) 0.15214(19) 0.0286(8) Uani 1 1 d . . . H60 H 0.1616 0.3403 0.1603 0.034 Uiso 1 1 calc R . . C61 C 0.4064(2) 0.2731(2) 0.1154(2) 0.0360(9) Uani 1 1 d . . . C62 C 0.1538(2) 0.2625(3) 0.0639(3) 0.0498(13) Uani 1 1 d . . . C63 C 0.31548(16) 0.44761(19) 0.26367(17) 0.0249(8) Uani 1 1 d . . . C64 C 0.34335(17) 0.46472(19) 0.32538(17) 0.0254(7) Uani 1 1 d . . . H64 H 0.3243 0.4488 0.3616 0.030 Uiso 1 1 calc R . . C65 C 0.39870(19) 0.5048(2) 0.33424(19) 0.0289(8) Uani 1 1 d . . . C66 C 0.42777(18) 0.53058(19) 0.28118(18) 0.0274(8) Uani 1 1 d . . . H66 H 0.4650 0.5570 0.2869 0.033 Uiso 1 1 calc R . . C67 C 0.39973(17) 0.51582(19) 0.21965(18) 0.0247(7) Uani 1 1 d . . . C68 C 0.34479(17) 0.47551(19) 0.21154(17) 0.0241(7) Uani 1 1 d . . . H68 H 0.3268 0.4667 0.1697 0.029 Uiso 1 1 calc R . . C69 C 0.4282(2) 0.5204(2) 0.4011(2) 0.0362(9) Uani 1 1 d . . . C70 C 0.43030(18) 0.5397(2) 0.16060(18) 0.0287(8) Uani 1 1 d . . . C71 C 0.68437(18) 0.0650(2) 0.23630(19) 0.0284(8) Uani 1 1 d . . . C72 C 0.66956(19) 0.0926(2) 0.17562(19) 0.0298(8) Uani 1 1 d . . . H72 H 0.6974 0.0842 0.1423 0.036 Uiso 1 1 calc R . . C73 C 0.6146(2) 0.1323(2) 0.1637(2) 0.0318(8) Uani 1 1 d . . . C74 C 0.5724(2) 0.1478(2) 0.2124(2) 0.0324(8) Uani 1 1 d . . . H74 H 0.5359 0.1747 0.2046 0.039 Uiso 1 1 calc R . . C75 C 0.5869(2) 0.1216(2) 0.2726(2) 0.0358(9) Uani 1 1 d . . . C76 C 0.6413(2) 0.0818(2) 0.2847(2) 0.0336(9) Uani 1 1 d . . . H76 H 0.6497 0.0656 0.3261 0.040 Uiso 1 1 calc R . . C77 C 0.6008(2) 0.1579(2) 0.0973(2) 0.0375(9) Uani 1 1 d . . . C78 C 0.5415(2) 0.1358(3) 0.3260(3) 0.0457(11) Uani 1 1 d . . . C79 C 0.7615(2) -0.0278(2) 0.18978(19) 0.0312(8) Uani 1 1 d . . . C80 C 0.8245(2) -0.0571(2) 0.1871(2) 0.0335(9) Uani 1 1 d . . . H80 H 0.8601 -0.0466 0.2173 0.040 Uiso 1 1 calc R . . C81 C 0.8357(2) -0.1014(2) 0.1409(2) 0.0349(9) Uani 1 1 d . . . C82 C 0.7842(2) -0.1190(2) 0.0954(2) 0.0329(9) Uani 1 1 d . . . H82 H 0.7914 -0.1491 0.0648 0.039 Uiso 1 1 calc R . . C83 C 0.7214(2) -0.0903(2) 0.0972(2) 0.0323(8) Uani 1 1 d . . . C84 C 0.7100(2) -0.04584(19) 0.14379(19) 0.0290(8) Uani 1 1 d . . . H84 H 0.6670 -0.0279 0.1441 0.035 Uiso 1 1 calc R . . C85 C 0.9051(2) -0.1301(2) 0.1407(3) 0.0423(11) Uani 1 1 d . . . C86 C 0.6634(2) -0.1065(2) 0.0487(2) 0.0391(10) Uani 1 1 d . . . B1 B 0.2500 0.4012(3) 0.2500 0.0239(11) Uani 1 2 d S . . B2 B 0.7500 0.0199(3) 0.2500 0.0301(13) Uani 1 2 d S . . F1 F 0.10602(18) 0.2420(3) 0.0992(2) 0.0924(15) Uani 1 1 d . . . F2 F 0.1208(2) 0.3068(3) 0.0297(2) 0.1010(16) Uani 1 1 d . . . F3 F 0.16768(17) 0.2194(3) 0.0235(2) 0.116(2) Uani 1 1 d . . . F4 F 0.40976(15) 0.2357(2) 0.06504(16) 0.0728(12) Uani 1 1 d . . . F5 F 0.43837(13) 0.24615(15) 0.16704(14) 0.0493(7) Uani 1 1 d . . . F6 F 0.44619(13) 0.32168(16) 0.10372(16) 0.0550(8) Uani 1 1 d . . . F7 F 0.49606(17) 0.5275(2) 0.40431(14) 0.0794(14) Uani 1 1 d . . . F8 F 0.4007(3) 0.5683(2) 0.42536(16) 0.1041(19) Uani 1 1 d . . . F9 F 0.42007(16) 0.47522(16) 0.44399(12) 0.0516(7) Uani 1 1 d . . . F10 F 0.46287(12) 0.49578(12) 0.12972(12) 0.0361(6) Uani 1 1 d . . . F11 F 0.47561(12) 0.58494(12) 0.17382(11) 0.0355(5) Uani 1 1 d . . . F12 F 0.38231(12) 0.56245(13) 0.11688(11) 0.0357(5) Uani 1 1 d . . . F13 F 0.68284(15) -0.14425(17) 0.00241(15) 0.0620(9) Uani 1 1 d . . . F14 F 0.61230(15) -0.13456(16) 0.07635(16) 0.0565(8) Uani 1 1 d . . . F15 F 0.63605(15) -0.05745(15) 0.01859(14) 0.0506(7) Uani 1 1 d . . . F16 F 0.91041(16) -0.16969(18) 0.09254(17) 0.0670(10) Uani 1 1 d . . . F17 F 0.92163(18) -0.16174(19) 0.19532(17) 0.0714(10) Uani 1 1 d . . . F18 F 0.95466(14) -0.08867(17) 0.13793(19) 0.0661(9) Uani 1 1 d . . . F19 F 0.4837(3) 0.1614(3) 0.3053(2) 0.135(3) Uani 1 1 d . . . F20 F 0.5685(3) 0.1719(3) 0.3681(2) 0.147(3) Uani 1 1 d . . . F21 F 0.5232(2) 0.0870(2) 0.3562(2) 0.0998(17) Uani 1 1 d . . . F22 F 0.58914(18) 0.11305(16) 0.05254(14) 0.0570(8) Uani 1 1 d . . . F23 F 0.65514(15) 0.18807(15) 0.07705(13) 0.0484(7) Uani 1 1 d . . . F24 F 0.54975(18) 0.1968(2) 0.09087(17) 0.0736(12) Uani 1 1 d . . . I1 I 0.626915(11) 0.499751(11) 0.204115(11) 0.02552(8) Uani 1 1 d . . . I2 I 0.125660(12) 0.884354(14) 0.207290(12) 0.03318(8) Uani 1 1 d . . . N1 N 0.81733(15) 0.44800(16) 0.13061(14) 0.0247(6) Uani 1 1 d . . . N2 N 0.79568(15) 0.54487(16) 0.11912(14) 0.0235(6) Uani 1 1 d . . . N3 N 0.27420(17) 0.83435(19) 0.11450(17) 0.0350(8) Uani 1 1 d . . . N4 N 0.29990(17) 0.93029(19) 0.12053(17) 0.0349(8) Uani 1 1 d . . . Pt1 Pt 0.7500 0.496772(9) 0.2500 0.01882(7) Uani 1 2 d S . . Pt2 Pt 0.2500 0.883258(11) 0.2500 0.02553(7) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0209(16) 0.0233(19) 0.0240(18) -0.0023(14) -0.0005(13) 0.0009(12) C2 0.0352(19) 0.033(2) 0.0236(18) -0.0042(17) 0.0095(14) 0.0014(15) C3 0.0332(19) 0.034(2) 0.0225(18) 0.0009(17) 0.0104(14) 0.0016(15) C4 0.0299(18) 0.0249(19) 0.0253(18) 0.0008(16) 0.0087(14) 0.0008(14) C5 0.0301(19) 0.030(2) 0.0268(19) 0.0016(17) 0.0060(14) -0.0027(15) C6 0.040(2) 0.026(2) 0.039(2) 0.0012(18) 0.0060(17) -0.0003(16) C7 0.044(2) 0.029(2) 0.042(2) 0.011(2) 0.0062(18) 0.0075(17) C8 0.035(2) 0.039(2) 0.035(2) 0.0112(19) 0.0004(16) 0.0042(17) C9 0.034(2) 0.033(2) 0.0229(18) 0.0044(17) 0.0055(14) -0.0024(15) C10 0.0289(18) 0.029(2) 0.033(2) 0.0008(17) 0.0045(15) -0.0020(14) C11 0.033(2) 0.041(3) 0.045(2) 0.007(2) 0.0061(17) -0.0009(17) C12 0.043(2) 0.037(2) 0.041(2) -0.001(2) -0.0033(18) -0.0016(18) C13 0.039(2) 0.039(2) 0.0226(18) 0.0078(18) -0.0015(15) -0.0041(17) C14 0.053(3) 0.051(3) 0.026(2) 0.004(2) -0.0019(18) -0.006(2) C15 0.036(2) 0.057(3) 0.038(2) 0.013(2) -0.0044(17) -0.007(2) C16 0.0298(19) 0.024(2) 0.0237(18) -0.0024(15) 0.0041(14) -0.0015(14) C17 0.0285(18) 0.028(2) 0.031(2) -0.0041(17) 0.0056(14) 0.0034(15) C18 0.0307(19) 0.028(2) 0.039(2) 0.0009(18) 0.0018(15) 0.0027(15) C19 0.038(2) 0.024(2) 0.044(2) -0.0001(19) 0.0052(17) 0.0020(16) C20 0.033(2) 0.027(2) 0.042(2) -0.0039(19) 0.0062(16) -0.0020(15) C21 0.0282(18) 0.027(2) 0.0282(19) -0.0106(17) 0.0040(14) 0.0015(14) C22 0.0272(19) 0.028(2) 0.039(2) -0.0024(18) 0.0041(15) 0.0008(14) C23 0.031(2) 0.041(3) 0.047(3) -0.005(2) 0.0121(17) 0.0038(17) C24 0.029(2) 0.036(2) 0.048(3) 0.000(2) -0.0019(17) 0.0029(16) C25 0.031(2) 0.031(2) 0.038(2) -0.0048(19) -0.0019(16) 0.0019(15) C26 0.049(3) 0.061(3) 0.035(2) -0.010(2) -0.0086(19) 0.011(2) C27 0.032(2) 0.035(2) 0.062(3) -0.010(2) -0.0006(19) -0.0022(17) C28 0.0240(18) 0.037(2) 0.038(2) 0.0044(19) 0.0069(15) 0.0049(14) C29 0.038(2) 0.077(4) 0.029(2) 0.000(2) 0.0078(17) 0.001(2) C30 0.040(2) 0.066(4) 0.034(2) 0.011(2) 0.0099(17) 0.003(2) C31 0.045(3) 0.039(3) 0.054(3) 0.018(2) 0.022(2) 0.0076(19) C32 0.047(3) 0.036(3) 0.054(3) 0.006(2) 0.018(2) -0.0047(19) C33 0.078(4) 0.043(3) 0.091(5) 0.002(3) 0.035(4) -0.015(3) C34 0.122(7) 0.033(3) 0.122(7) 0.005(4) 0.044(5) 0.001(4) C35 0.080(5) 0.043(4) 0.136(7) 0.012(4) 0.054(5) 0.020(3) C36 0.055(3) 0.047(3) 0.077(4) 0.028(3) 0.032(3) 0.018(2) C37 0.036(2) 0.042(3) 0.045(2) 0.009(2) 0.0063(17) -0.0049(18) C38 0.043(3) 0.066(4) 0.056(3) 0.011(3) 0.002(2) -0.017(2) C39 0.034(2) 0.074(4) 0.052(3) 0.014(3) 0.0093(19) 0.004(2) C40 0.043(3) 0.070(4) 0.096(5) 0.043(4) 0.030(3) 0.022(3) C41 0.062(4) 0.060(4) 0.192(9) 0.037(5) 0.066(5) 0.025(3) C42 0.052(4) 0.142(9) 0.122(7) 0.079(7) 0.009(4) 0.010(4) C43 0.034(2) 0.039(2) 0.033(2) -0.0111(19) 0.0075(16) 0.0027(17) C44 0.041(2) 0.045(3) 0.041(2) -0.012(2) 0.0039(18) 0.0059(19) C45 0.058(3) 0.042(3) 0.055(3) -0.011(3) 0.002(2) 0.011(2) C46 0.060(3) 0.038(3) 0.078(4) -0.013(3) 0.011(3) -0.002(2) C47 0.048(3) 0.045(3) 0.064(3) -0.021(3) 0.009(2) -0.011(2) C48 0.034(2) 0.053(3) 0.045(3) -0.020(2) 0.0072(18) 0.0031(19) C49 0.034(2) 0.052(3) 0.047(3) -0.011(2) 0.0051(18) 0.0101(19) C50 0.045(3) 0.078(4) 0.059(3) -0.015(3) 0.013(2) 0.010(3) C51 0.048(3) 0.048(3) 0.061(3) -0.008(3) -0.007(2) 0.015(2) C52 0.035(2) 0.066(4) 0.043(3) -0.014(3) 0.0009(18) 0.004(2) C53 0.053(3) 0.111(6) 0.042(3) -0.019(3) -0.006(2) 0.018(3) C54 0.035(3) 0.075(4) 0.064(3) -0.022(3) 0.001(2) 0.001(2) C55 0.0288(17) 0.0256(19) 0.0203(16) 0.0040(15) 0.0064(13) -0.0002(14) C56 0.0262(17) 0.029(2) 0.0233(18) -0.0004(16) 0.0020(13) 0.0023(14) C57 0.0297(19) 0.029(2) 0.0292(19) -0.0008(17) 0.0060(14) 0.0057(15) C58 0.033(2) 0.029(2) 0.031(2) -0.0058(18) 0.0028(15) 0.0048(15) C59 0.0294(19) 0.034(2) 0.035(2) -0.0093(18) 0.0032(15) 0.0009(15) C60 0.0260(18) 0.031(2) 0.0301(19) -0.0019(17) 0.0072(14) 0.0019(14) C61 0.034(2) 0.039(2) 0.036(2) -0.011(2) 0.0047(16) 0.0073(17) C62 0.030(2) 0.062(3) 0.057(3) -0.026(3) 0.0006(19) 0.006(2) C63 0.0215(17) 0.028(2) 0.0251(17) -0.0003(15) 0.0025(13) 0.0034(12) C64 0.0220(16) 0.030(2) 0.0244(17) 0.0006(16) 0.0063(13) 0.0017(13) C65 0.0282(19) 0.035(2) 0.0242(19) -0.0042(16) 0.0051(14) 0.0008(14) C66 0.0249(17) 0.029(2) 0.0286(19) -0.0002(16) 0.0020(13) -0.0044(13) C67 0.0222(16) 0.0287(19) 0.0237(18) 0.0006(16) 0.0042(13) 0.0025(13) C68 0.0230(16) 0.030(2) 0.0192(16) 0.0003(15) 0.0025(12) 0.0009(13) C69 0.040(2) 0.043(3) 0.027(2) -0.0027(19) 0.0060(16) -0.0061(18) C70 0.0267(17) 0.034(2) 0.0261(18) 0.0008(17) 0.0050(13) -0.0012(14) C71 0.0283(19) 0.025(2) 0.032(2) -0.0057(16) 0.0030(14) -0.0040(13) C72 0.0303(18) 0.031(2) 0.0289(19) -0.0023(17) 0.0053(14) 0.0003(15) C73 0.0310(19) 0.029(2) 0.035(2) -0.0022(18) 0.0041(15) -0.0019(15) C74 0.0314(19) 0.026(2) 0.040(2) -0.0051(18) 0.0076(15) -0.0020(14) C75 0.036(2) 0.031(2) 0.042(2) -0.0091(19) 0.0136(17) -0.0063(16) C76 0.038(2) 0.030(2) 0.033(2) -0.0051(18) 0.0048(16) -0.0058(16) C77 0.039(2) 0.031(2) 0.042(2) 0.002(2) 0.0061(17) 0.0059(17) C78 0.046(3) 0.041(3) 0.052(3) -0.009(2) 0.020(2) -0.007(2) C79 0.037(2) 0.029(2) 0.0275(19) 0.0000(17) 0.0033(15) 0.0005(15) C80 0.037(2) 0.028(2) 0.035(2) 0.0003(18) -0.0007(16) 0.0030(16) C81 0.031(2) 0.035(2) 0.039(2) -0.0002(19) 0.0010(16) 0.0060(16) C82 0.038(2) 0.029(2) 0.032(2) -0.0002(18) 0.0050(16) 0.0051(16) C83 0.033(2) 0.030(2) 0.033(2) 0.0004(18) 0.0012(15) 0.0040(15) C84 0.0309(19) 0.027(2) 0.0294(19) 0.0003(17) 0.0040(14) 0.0041(14) C85 0.033(2) 0.040(3) 0.054(3) -0.011(2) -0.0032(18) 0.0085(18) C86 0.039(2) 0.034(2) 0.043(2) -0.007(2) -0.0037(18) 0.0081(17) B1 0.020(2) 0.030(3) 0.022(3) 0.000 0.0038(19) 0.000 B2 0.031(3) 0.028(3) 0.031(3) 0.000 0.002(2) 0.000 F1 0.051(2) 0.128(4) 0.099(3) -0.045(3) 0.0095(18) -0.038(2) F2 0.080(3) 0.117(4) 0.097(3) -0.014(3) -0.054(2) 0.007(3) F3 0.0400(17) 0.158(5) 0.147(4) -0.130(4) -0.008(2) 0.008(2) F4 0.0379(15) 0.108(3) 0.071(2) -0.058(2) -0.0014(13) 0.0195(16) F5 0.0352(13) 0.0546(19) 0.0580(17) 0.0063(15) 0.0028(11) 0.0169(12) F6 0.0349(14) 0.058(2) 0.075(2) 0.0100(16) 0.0230(13) 0.0030(12) F7 0.0596(19) 0.142(4) 0.0350(15) -0.003(2) -0.0048(13) -0.048(2) F8 0.190(5) 0.073(3) 0.0423(18) -0.0313(19) -0.038(2) 0.072(3) F9 0.0726(19) 0.0533(19) 0.0276(13) 0.0064(13) -0.0042(12) -0.0093(14) F10 0.0357(12) 0.0428(15) 0.0318(12) -0.0017(11) 0.0154(10) -0.0004(10) F11 0.0397(12) 0.0370(14) 0.0307(12) 0.0017(11) 0.0080(9) -0.0126(10) F12 0.0348(12) 0.0449(15) 0.0275(11) 0.0106(11) 0.0028(9) 0.0001(10) F13 0.0527(16) 0.069(2) 0.0613(18) -0.0404(18) -0.0170(13) 0.0204(15) F14 0.0425(15) 0.057(2) 0.068(2) 0.0027(17) -0.0074(13) -0.0111(13) F15 0.0567(16) 0.0465(17) 0.0457(15) 0.0000(14) -0.0158(12) 0.0114(12) F16 0.0470(16) 0.077(3) 0.075(2) -0.0372(19) -0.0049(14) 0.0254(15) F17 0.064(2) 0.078(3) 0.071(2) 0.008(2) -0.0067(16) 0.0370(18) F18 0.0341(15) 0.056(2) 0.110(3) -0.014(2) 0.0146(15) 0.0028(13) F19 0.115(4) 0.215(7) 0.083(3) 0.026(4) 0.056(3) 0.106(4) F20 0.155(5) 0.187(6) 0.113(3) -0.112(4) 0.103(4) -0.115(5) F21 0.117(3) 0.055(2) 0.141(4) 0.017(3) 0.101(3) 0.003(2) F22 0.079(2) 0.0502(19) 0.0397(15) -0.0020(14) -0.0110(14) -0.0148(15) F23 0.0577(16) 0.0485(18) 0.0404(14) 0.0005(13) 0.0121(12) -0.0088(13) F24 0.068(2) 0.088(3) 0.068(2) 0.033(2) 0.0247(16) 0.044(2) I1 0.02267(13) 0.03153(15) 0.02242(13) 0.00022(9) 0.00214(9) 0.00133(7) I2 0.02581(14) 0.04126(17) 0.03306(15) -0.00046(11) 0.00607(10) 0.00160(9) N1 0.0280(15) 0.0266(17) 0.0203(14) -0.0021(13) 0.0079(11) 0.0038(12) N2 0.0266(14) 0.0273(17) 0.0172(14) 0.0018(13) 0.0058(11) -0.0016(12) N3 0.0285(16) 0.046(2) 0.0310(17) -0.0024(17) 0.0071(13) 0.0039(14) N4 0.0277(16) 0.044(2) 0.0337(18) 0.0106(17) 0.0088(13) 0.0020(14) Pt1 0.02065(11) 0.01882(11) 0.01738(11) 0.000 0.00402(7) 0.000 Pt2 0.02404(12) 0.02569(13) 0.02770(13) 0.000 0.00760(8) 0.000 _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 C1 N2 1.362(5) . ? C1 N1 1.366(5) . ? C1 Pt1 2.069(4) . ? C2 C3 1.339(6) . ? C2 N1 1.392(5) . ? C2 H2 0.9300 . ? C3 N2 1.394(4) . ? C3 H3 0.9300 . ? C4 C5 1.399(6) . ? C4 C9 1.407(6) . ? C4 N2 1.448(5) . ? C5 C6 1.398(6) . ? C5 C10 1.516(5) . ? C6 C7 1.385(6) . ? C6 H6 0.9300 . ? C7 C8 1.387(7) . ? C7 H7 0.9300 . ? C8 C9 1.387(6) . ? C8 H8 0.9300 . ? C9 C13 1.517(6) . ? C10 C12 1.525(6) . ? C10 C11 1.543(5) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C15 1.526(6) . ? C13 C14 1.540(6) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.407(6) . ? C16 C21 1.421(5) . ? C16 N1 1.439(5) . ? C17 C18 1.381(6) . ? C17 C22 1.534(5) . ? C18 C19 1.389(6) . ? C18 H18 0.9300 . ? C19 C20 1.394(6) . ? C19 H19 0.9300 . ? C20 C21 1.374(6) . ? C20 H20 0.9300 . ? C21 C25 1.519(6) . ? C22 C24 1.525(6) . ? C22 C23 1.533(6) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C27 1.530(6) . ? C25 C26 1.536(6) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N3 1.358(6) . ? C28 N4 1.361(6) . ? C28 Pt2 2.061(4) . ? C29 C30 1.346(9) . ? C29 N3 1.384(6) . ? C29 H29 0.9300 . ? C30 N4 1.384(6) . ? C30 H30 0.9300 . ? C31 C32 1.390(8) . ? C31 C36 1.416(7) . ? C31 N4 1.446(7) . ? C32 C33 1.386(8) . ? C32 C37 1.528(7) . ? C33 C34 1.389(10) . ? C33 H33 0.9300 . ? C34 C35 1.372(12) . ? C34 H34 0.9300 . ? C35 C36 1.396(10) . ? C35 H35 0.9300 . ? C36 C40 1.489(10) . ? C37 C38 1.524(7) . ? C37 C39 1.528(6) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.520(8) . ? C40 C42 1.578(10) . ? C40 H40 0.9800 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.401(7) . ? C43 C48 1.411(6) . ? C43 N3 1.447(6) . ? C44 C45 1.382(8) . ? C44 C49 1.520(7) . ? C45 C46 1.382(8) . ? C45 H45 0.9300 . ? C46 C47 1.380(9) . ? C46 H46 0.9300 . ? C47 C48 1.386(8) . ? C47 H47 0.9300 . ? C48 C52 1.513(7) . ? C49 C50 1.533(6) . ? C49 C51 1.538(7) . ? C49 H49 0.9800 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C54 1.540(7) . ? C52 C53 1.543(7) . ? C52 H52 0.9800 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C60 1.398(5) . ? C55 C56 1.405(5) . ? C55 B1 1.635(6) . ? C56 C57 1.386(6) . ? C56 H56 0.9300 . ? C57 C58 1.396(6) . ? C57 C61 1.492(5) . ? C58 C59 1.388(6) . ? C58 H58 0.9300 . ? C59 C60 1.403(6) . ? C59 C62 1.488(6) . ? C60 H60 0.9300 . ? C61 F4 1.329(5) . ? C61 F5 1.335(5) . ? C61 F6 1.350(6) . ? C62 F3 1.301(6) . ? C62 F1 1.310(7) . ? C62 F2 1.335(8) . ? C63 C68 1.400(5) . ? C63 C64 1.402(5) . ? C63 B1 1.644(5) . ? C64 C65 1.396(5) . ? C64 H64 0.9300 . ? C65 C66 1.394(5) . ? C65 C69 1.499(6) . ? C66 C67 1.387(5) . ? C66 H66 0.9300 . ? C67 C68 1.392(5) . ? C67 C70 1.496(5) . ? C68 H68 0.9300 . ? C69 F8 1.295(6) . ? C69 F7 1.337(5) . ? C69 F9 1.344(6) . ? C70 F10 1.341(5) . ? C70 F11 1.343(5) . ? C70 F12 1.351(5) . ? C71 C72 1.404(6) . ? C71 C76 1.407(5) . ? C71 B2 1.629(6) . ? C72 C73 1.391(6) . ? C72 H72 0.9300 . ? C73 C74 1.393(6) . ? C73 C77 1.489(6) . ? C74 C75 1.382(7) . ? C74 H74 0.9300 . ? C75 C76 1.385(6) . ? C75 C78 1.504(6) . ? C76 H76 0.9300 . ? C77 F24 1.314(5) . ? C77 F23 1.347(5) . ? C77 F22 1.355(6) . ? C78 F20 1.260(7) . ? C78 F21 1.298(7) . ? C78 F19 1.309(7) . ? C79 C84 1.392(6) . ? C79 C80 1.398(6) . ? C79 B2 1.652(6) . ? C80 C81 1.389(6) . ? C80 H80 0.9300 . ? C81 C82 1.383(6) . ? C81 C85 1.500(6) . ? C82 C83 1.385(6) . ? C82 H82 0.9300 . ? C83 C84 1.399(6) . ? C83 C86 1.502(6) . ? C84 H84 0.9300 . ? C85 F16 1.328(6) . ? C85 F18 1.332(6) . ? C85 F17 1.344(6) . ? C86 F15 1.332(6) . ? C86 F13 1.340(5) . ? C86 F14 1.340(6) . ? B1 C55 1.635(6) 2 ? B1 C63 1.644(5) 2 ? B2 C71 1.629(6) 2_655 ? B2 C79 1.652(6) 2_655 ? I1 Pt1 2.5294(2) . ? I2 Pt2 2.5326(2) . ? Pt1 C1 2.069(4) 2_655 ? Pt1 I1 2.5294(2) 2_655 ? Pt2 C28 2.061(4) 2 ? Pt2 I2 2.5326(2) 2 ? 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 N2 C1 N1 105.1(3) . . ? N2 C1 Pt1 128.2(3) . . ? N1 C1 Pt1 126.2(3) . . ? C3 C2 N1 107.0(3) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 107.5(3) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? C5 C4 C9 123.3(4) . . ? C5 C4 N2 118.5(3) . . ? C9 C4 N2 117.8(4) . . ? C6 C5 C4 117.3(4) . . ? C6 C5 C10 119.6(4) . . ? C4 C5 C10 123.0(4) . . ? C7 C6 C5 120.7(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 120.3(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 121.6(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C4 116.7(4) . . ? C8 C9 C13 120.9(4) . . ? C4 C9 C13 122.3(4) . . ? C5 C10 C12 112.3(3) . . ? C5 C10 C11 109.8(3) . . ? C12 C10 C11 111.1(4) . . ? C5 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 113.0(4) . . ? C9 C13 C14 110.8(4) . . ? C15 C13 C14 109.2(4) . . ? C9 C13 H13 107.9 . . ? C15 C13 H13 107.9 . . ? C14 C13 H13 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.0(4) . . ? C17 C16 N1 119.7(3) . . ? C21 C16 N1 118.1(4) . . ? C18 C17 C16 117.6(4) . . ? C18 C17 C22 119.4(4) . . ? C16 C17 C22 122.5(4) . . ? C17 C18 C19 121.6(4) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C18 C19 C20 119.4(4) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 C19 121.9(4) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C16 117.2(4) . . ? C20 C21 C25 121.1(4) . . ? C16 C21 C25 121.4(4) . . ? C24 C22 C23 109.2(3) . . ? C24 C22 C17 113.4(4) . . ? C23 C22 C17 108.1(3) . . ? C24 C22 H22 108.7 . . ? C23 C22 H22 108.7 . . ? C17 C22 H22 108.7 . . ? 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 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 112.8(4) . . ? C21 C25 C26 109.8(4) . . ? C27 C25 C26 110.1(4) . . ? C21 C25 H25 108.0 . . ? C27 C25 H25 108.0 . . ? C26 C25 H25 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 N4 104.8(4) . . ? N3 C28 Pt2 126.7(3) . . ? N4 C28 Pt2 128.5(3) . . ? C30 C29 N3 106.8(4) . . ? C30 C29 H29 126.6 . . ? N3 C29 H29 126.6 . . ? C29 C30 N4 107.2(4) . . ? C29 C30 H30 126.4 . . ? N4 C30 H30 126.4 . . ? C32 C31 C36 124.0(5) . . ? C32 C31 N4 118.8(4) . . ? C36 C31 N4 116.9(5) . . ? C33 C32 C31 116.5(5) . . ? C33 C32 C37 120.1(5) . . ? C31 C32 C37 123.2(5) . . ? C32 C33 C34 121.6(7) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 120.2(7) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 121.5(6) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C31 115.9(6) . . ? C35 C36 C40 121.3(6) . . ? C31 C36 C40 122.4(6) . . ? C38 C37 C39 108.6(4) . . ? C38 C37 C32 113.8(5) . . ? C39 C37 C32 110.2(4) . . ? C38 C37 H37 108.0 . . ? C39 C37 H37 108.0 . . ? C32 C37 H37 108.0 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 C41 113.3(7) . . ? C36 C40 C42 111.1(5) . . ? C41 C40 C42 110.4(6) . . ? C36 C40 H40 107.2 . . ? C41 C40 H40 107.2 . . ? C42 C40 H40 107.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 122.8(5) . . ? C44 C43 N3 117.8(4) . . ? C48 C43 N3 119.2(4) . . ? C45 C44 C43 117.1(5) . . ? C45 C44 C49 120.8(5) . . ? C43 C44 C49 121.8(5) . . ? C46 C45 C44 121.6(5) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C47 C46 C45 120.0(6) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 121.7(5) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C47 C48 C43 116.6(5) . . ? C47 C48 C52 120.2(5) . . ? C43 C48 C52 122.7(5) . . ? C44 C49 C50 109.2(4) . . ? C44 C49 C51 112.7(5) . . ? C50 C49 C51 110.2(4) . . ? C44 C49 H49 108.2 . . ? C50 C49 H49 108.2 . . ? C51 C49 H49 108.2 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 C54 113.6(5) . . ? C48 C52 C53 108.5(4) . . ? C54 C52 C53 108.1(4) . . ? C48 C52 H52 108.9 . . ? C54 C52 H52 108.9 . . ? C53 C52 H52 108.9 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 115.7(4) . . ? C60 C55 B1 122.4(3) . . ? C56 C55 B1 121.6(3) . . ? C57 C56 C55 122.3(4) . . ? C57 C56 H56 118.8 . . ? C55 C56 H56 118.8 . . ? C56 C57 C58 121.1(3) . . ? C56 C57 C61 118.8(4) . . ? C58 C57 C61 120.1(4) . . ? C59 C58 C57 117.9(4) . . ? C59 C58 H58 121.1 . . ? C57 C58 H58 121.1 . . ? C58 C59 C60 120.6(4) . . ? C58 C59 C62 120.5(4) . . ? C60 C59 C62 119.0(4) . . ? C55 C60 C59 122.4(3) . . ? C55 C60 H60 118.8 . . ? C59 C60 H60 118.8 . . ? F4 C61 F5 108.1(4) . . ? F4 C61 F6 106.1(4) . . ? F5 C61 F6 104.2(4) . . ? F4 C61 C57 113.7(4) . . ? F5 C61 C57 112.4(4) . . ? F6 C61 C57 111.8(4) . . ? F3 C62 F1 107.8(5) . . ? F3 C62 F2 107.4(5) . . ? F1 C62 F2 101.9(5) . . ? F3 C62 C59 113.6(4) . . ? F1 C62 C59 113.4(4) . . ? F2 C62 C59 112.1(5) . . ? C68 C63 C64 115.6(3) . . ? C68 C63 B1 119.8(3) . . ? C64 C63 B1 124.5(3) . . ? C65 C64 C63 122.2(3) . . ? C65 C64 H64 118.9 . . ? C63 C64 H64 118.9 . . ? C66 C65 C64 120.7(4) . . ? C66 C65 C69 118.9(4) . . ? C64 C65 C69 120.4(4) . . ? C67 C66 C65 118.2(4) . . ? C67 C66 H66 120.9 . . ? C65 C66 H66 120.9 . . ? C66 C67 C68 120.5(3) . . ? C66 C67 C70 120.9(3) . . ? C68 C67 C70 118.5(3) . . ? C67 C68 C63 122.8(3) . . ? C67 C68 H68 118.6 . . ? C63 C68 H68 118.6 . . ? F8 C69 F7 109.3(5) . . ? F8 C69 F9 105.2(4) . . ? F7 C69 F9 102.7(4) . . ? F8 C69 C65 113.4(4) . . ? F7 C69 C65 112.7(3) . . ? F9 C69 C65 112.8(4) . . ? F10 C70 F11 106.9(3) . . ? F10 C70 F12 106.1(3) . . ? F11 C70 F12 106.5(3) . . ? F10 C70 C67 112.1(3) . . ? F11 C70 C67 112.9(3) . . ? F12 C70 C67 111.9(3) . . ? C72 C71 C76 115.5(4) . . ? C72 C71 B2 121.5(3) . . ? C76 C71 B2 122.9(3) . . ? C73 C72 C71 122.1(4) . . ? C73 C72 H72 118.9 . . ? C71 C72 H72 118.9 . . ? C72 C73 C74 121.2(4) . . ? C72 C73 C77 118.7(4) . . ? C74 C73 C77 120.0(4) . . ? C75 C74 C73 117.3(4) . . ? C75 C74 H74 121.3 . . ? C73 C74 H74 121.3 . . ? C74 C75 C76 121.7(4) . . ? C74 C75 C78 119.1(4) . . ? C76 C75 C78 119.2(4) . . ? C75 C76 C71 122.1(4) . . ? C75 C76 H76 118.9 . . ? C71 C76 H76 118.9 . . ? F24 C77 F23 105.5(4) . . ? F24 C77 F22 108.0(4) . . ? F23 C77 F22 103.7(3) . . ? F24 C77 C73 114.8(4) . . ? F23 C77 C73 112.2(4) . . ? F22 C77 C73 111.8(4) . . ? F20 C78 F21 107.3(5) . . ? F20 C78 F19 105.6(6) . . ? F21 C78 F19 104.1(5) . . ? F20 C78 C75 113.2(4) . . ? F21 C78 C75 112.7(4) . . ? F19 C78 C75 113.2(5) . . ? C84 C79 C80 116.3(4) . . ? C84 C79 B2 124.1(3) . . ? C80 C79 B2 119.3(3) . . ? C81 C80 C79 122.1(4) . . ? C81 C80 H80 118.9 . . ? C79 C80 H80 118.9 . . ? C82 C81 C80 121.1(4) . . ? C82 C81 C85 120.0(4) . . ? C80 C81 C85 118.9(4) . . ? C81 C82 C83 117.6(4) . . ? C81 C82 H82 121.2 . . ? C83 C82 H82 121.2 . . ? C82 C83 C84 121.3(4) . . ? C82 C83 C86 120.5(4) . . ? C84 C83 C86 118.2(4) . . ? C79 C84 C83 121.5(4) . . ? C79 C84 H84 119.2 . . ? C83 C84 H84 119.2 . . ? F16 C85 F18 108.1(4) . . ? F16 C85 F17 105.7(4) . . ? F18 C85 F17 104.7(4) . . ? F16 C85 C81 113.3(4) . . ? F18 C85 C81 112.5(4) . . ? F17 C85 C81 111.9(4) . . ? F15 C86 F13 106.6(4) . . ? F15 C86 F14 106.2(4) . . ? F13 C86 F14 106.8(4) . . ? F15 C86 C83 112.4(4) . . ? F13 C86 C83 112.3(4) . . ? F14 C86 C83 112.1(4) . . ? C55 B1 C55 104.1(5) . 2 ? C55 B1 C63 113.00(18) . 2 ? C55 B1 C63 111.53(18) 2 2 ? C55 B1 C63 111.53(18) . . ? C55 B1 C63 113.00(18) 2 . ? C63 B1 C63 104.0(4) 2 . ? C71 B2 C71 105.7(5) 2_655 . ? C71 B2 C79 113.6(2) 2_655 2_655 ? C71 B2 C79 111.1(2) . 2_655 ? C71 B2 C79 111.1(2) 2_655 . ? C71 B2 C79 113.6(2) . . ? C79 B2 C79 102.0(5) 2_655 . ? C1 N1 C2 110.3(3) . . ? C1 N1 C16 126.4(3) . . ? C2 N1 C16 123.0(3) . . ? C1 N2 C3 110.1(3) . . ? C1 N2 C4 129.1(3) . . ? C3 N2 C4 120.5(3) . . ? C28 N3 C29 110.8(4) . . ? C28 N3 C43 127.5(4) . . ? C29 N3 C43 121.6(4) . . ? C28 N4 C30 110.5(4) . . ? C28 N4 C31 127.8(4) . . ? C30 N4 C31 121.7(4) . . ? C1 Pt1 C1 179.5(2) 2_655 . ? C1 Pt1 I1 92.88(10) 2_655 2_655 ? C1 Pt1 I1 87.13(10) . 2_655 ? C1 Pt1 I1 87.13(10) 2_655 . ? C1 Pt1 I1 92.88(10) . . ? I1 Pt1 I1 177.055(14) 2_655 . ? C28 Pt2 C28 179.4(3) 2 . ? C28 Pt2 I2 90.85(11) 2 . ? C28 Pt2 I2 89.15(11) . . ? C28 Pt2 I2 89.15(11) 2 2 ? C28 Pt2 I2 90.85(11) . 2 ? I2 Pt2 I2 178.917(16) . 2 ? 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 N1 C2 C3 N2 -0.7(4) . . . . ? C9 C4 C5 C6 3.0(6) . . . . ? N2 C4 C5 C6 175.8(3) . . . . ? C9 C4 C5 C10 -173.1(3) . . . . ? N2 C4 C5 C10 -0.3(5) . . . . ? C4 C5 C6 C7 -0.9(6) . . . . ? C10 C5 C6 C7 175.4(4) . . . . ? C5 C6 C7 C8 -1.3(6) . . . . ? C6 C7 C8 C9 1.6(7) . . . . ? C7 C8 C9 C4 0.4(6) . . . . ? C7 C8 C9 C13 -176.4(4) . . . . ? C5 C4 C9 C8 -2.8(6) . . . . ? N2 C4 C9 C8 -175.6(3) . . . . ? C5 C4 C9 C13 174.0(4) . . . . ? N2 C4 C9 C13 1.1(5) . . . . ? C6 C5 C10 C12 51.1(5) . . . . ? C4 C5 C10 C12 -132.9(4) . . . . ? C6 C5 C10 C11 -73.0(5) . . . . ? C4 C5 C10 C11 103.0(4) . . . . ? C8 C9 C13 C15 -36.9(5) . . . . ? C4 C9 C13 C15 146.4(4) . . . . ? C8 C9 C13 C14 86.0(5) . . . . ? C4 C9 C13 C14 -90.7(5) . . . . ? C21 C16 C17 C18 -6.0(6) . . . . ? N1 C16 C17 C18 178.3(3) . . . . ? C21 C16 C17 C22 166.0(4) . . . . ? N1 C16 C17 C22 -9.7(6) . . . . ? C16 C17 C18 C19 1.2(6) . . . . ? C22 C17 C18 C19 -171.1(4) . . . . ? C17 C18 C19 C20 3.0(7) . . . . ? C18 C19 C20 C21 -2.5(7) . . . . ? C19 C20 C21 C16 -2.1(6) . . . . ? C19 C20 C21 C25 171.6(4) . . . . ? C17 C16 C21 C20 6.4(6) . . . . ? N1 C16 C21 C20 -177.8(3) . . . . ? C17 C16 C21 C25 -167.2(3) . . . . ? N1 C16 C21 C25 8.6(6) . . . . ? C18 C17 C22 C24 -45.7(5) . . . . ? C16 C17 C22 C24 142.5(4) . . . . ? C18 C17 C22 C23 75.5(5) . . . . ? C16 C17 C22 C23 -96.3(5) . . . . ? C20 C21 C25 C27 32.4(6) . . . . ? C16 C21 C25 C27 -154.2(4) . . . . ? C20 C21 C25 C26 -90.8(5) . . . . ? C16 C21 C25 C26 82.6(5) . . . . ? N3 C29 C30 N4 1.0(5) . . . . ? C36 C31 C32 C33 4.2(8) . . . . ? N4 C31 C32 C33 177.3(5) . . . . ? C36 C31 C32 C37 -171.4(5) . . . . ? N4 C31 C32 C37 1.7(7) . . . . ? C31 C32 C33 C34 -0.6(10) . . . . ? C37 C32 C33 C34 175.1(6) . . . . ? C32 C33 C34 C35 -2.2(12) . . . . ? C33 C34 C35 C36 1.7(13) . . . . ? C34 C35 C36 C31 1.5(11) . . . . ? C34 C35 C36 C40 -171.8(7) . . . . ? C32 C31 C36 C35 -4.6(9) . . . . ? N4 C31 C36 C35 -177.9(5) . . . . ? C32 C31 C36 C40 168.6(5) . . . . ? N4 C31 C36 C40 -4.7(8) . . . . ? C33 C32 C37 C38 42.3(7) . . . . ? C31 C32 C37 C38 -142.3(5) . . . . ? C33 C32 C37 C39 -80.0(7) . . . . ? C31 C32 C37 C39 95.5(6) . . . . ? C35 C36 C40 C41 -44.5(8) . . . . ? C31 C36 C40 C41 142.7(6) . . . . ? C35 C36 C40 C42 80.5(8) . . . . ? C31 C36 C40 C42 -92.4(8) . . . . ? C48 C43 C44 C45 -5.9(7) . . . . ? N3 C43 C44 C45 178.2(4) . . . . ? C48 C43 C44 C49 167.8(4) . . . . ? N3 C43 C44 C49 -8.0(6) . . . . ? C43 C44 C45 C46 2.5(8) . . . . ? C49 C44 C45 C46 -171.4(5) . . . . ? C44 C45 C46 C47 1.3(9) . . . . ? C45 C46 C47 C48 -1.9(9) . . . . ? C46 C47 C48 C43 -1.3(8) . . . . ? C46 C47 C48 C52 171.3(5) . . . . ? C44 C43 C48 C47 5.4(7) . . . . ? N3 C43 C48 C47 -178.8(4) . . . . ? C44 C43 C48 C52 -167.1(4) . . . . ? N3 C43 C48 C52 8.7(6) . . . . ? C45 C44 C49 C50 86.4(6) . . . . ? C43 C44 C49 C50 -87.2(6) . . . . ? C45 C44 C49 C51 -36.5(6) . . . . ? C43 C44 C49 C51 149.9(4) . . . . ? C47 C48 C52 C54 42.7(7) . . . . ? C43 C48 C52 C54 -145.2(5) . . . . ? C47 C48 C52 C53 -77.6(6) . . . . ? C43 C48 C52 C53 94.6(6) . . . . ? C60 C55 C56 C57 1.3(6) . . . . ? B1 C55 C56 C57 175.2(4) . . . . ? C55 C56 C57 C58 0.0(6) . . . . ? C55 C56 C57 C61 179.7(4) . . . . ? C56 C57 C58 C59 -1.0(7) . . . . ? C61 C57 C58 C59 179.3(4) . . . . ? C57 C58 C59 C60 0.7(7) . . . . ? C57 C58 C59 C62 178.8(4) . . . . ? C56 C55 C60 C59 -1.6(6) . . . . ? B1 C55 C60 C59 -175.5(4) . . . . ? C58 C59 C60 C55 0.7(7) . . . . ? C62 C59 C60 C55 -177.5(4) . . . . ? C56 C57 C61 F4 -175.3(4) . . . . ? C58 C57 C61 F4 4.3(7) . . . . ? C56 C57 C61 F5 61.5(6) . . . . ? C58 C57 C61 F5 -118.8(4) . . . . ? C56 C57 C61 F6 -55.2(5) . . . . ? C58 C57 C61 F6 124.4(4) . . . . ? C58 C59 C62 F3 7.3(8) . . . . ? C60 C59 C62 F3 -174.5(5) . . . . ? C58 C59 C62 F1 130.8(5) . . . . ? C60 C59 C62 F1 -51.1(7) . . . . ? C58 C59 C62 F2 -114.6(5) . . . . ? C60 C59 C62 F2 63.6(6) . . . . ? C68 C63 C64 C65 -2.8(6) . . . . ? B1 C63 C64 C65 -179.4(4) . . . . ? C63 C64 C65 C66 1.3(6) . . . . ? C63 C64 C65 C69 -178.1(4) . . . . ? C64 C65 C66 C67 0.7(6) . . . . ? C69 C65 C66 C67 -179.8(4) . . . . ? C65 C66 C67 C68 -1.1(6) . . . . ? C65 C66 C67 C70 -177.4(4) . . . . ? C66 C67 C68 C63 -0.6(6) . . . . ? C70 C67 C68 C63 175.8(4) . . . . ? C64 C63 C68 C67 2.4(6) . . . . ? B1 C63 C68 C67 179.2(4) . . . . ? C66 C65 C69 F8 89.7(5) . . . . ? C64 C65 C69 F8 -90.9(6) . . . . ? C66 C65 C69 F7 -35.2(6) . . . . ? C64 C65 C69 F7 144.3(4) . . . . ? C66 C65 C69 F9 -150.9(4) . . . . ? C64 C65 C69 F9 28.5(6) . . . . ? C66 C67 C70 F10 107.6(4) . . . . ? C68 C67 C70 F10 -68.8(4) . . . . ? C66 C67 C70 F11 -13.2(5) . . . . ? C68 C67 C70 F11 170.5(3) . . . . ? C66 C67 C70 F12 -133.4(4) . . . . ? C68 C67 C70 F12 50.2(5) . . . . ? C76 C71 C72 C73 -2.2(6) . . . . ? B2 C71 C72 C73 -178.6(4) . . . . ? C71 C72 C73 C74 1.8(6) . . . . ? C71 C72 C73 C77 -177.7(4) . . . . ? C72 C73 C74 C75 -0.8(6) . . . . ? C77 C73 C74 C75 178.7(4) . . . . ? C73 C74 C75 C76 0.4(6) . . . . ? C73 C74 C75 C78 -178.3(4) . . . . ? C74 C75 C76 C71 -0.9(7) . . . . ? C78 C75 C76 C71 177.8(4) . . . . ? C72 C71 C76 C75 1.7(6) . . . . ? B2 C71 C76 C75 178.0(4) . . . . ? C72 C73 C77 F24 -177.3(4) . . . . ? C74 C73 C77 F24 3.2(6) . . . . ? C72 C73 C77 F23 -56.8(5) . . . . ? C74 C73 C77 F23 123.7(4) . . . . ? C72 C73 C77 F22 59.2(5) . . . . ? C74 C73 C77 F22 -120.3(4) . . . . ? C74 C75 C78 F20 -106.0(7) . . . . ? C76 C75 C78 F20 75.3(7) . . . . ? C74 C75 C78 F21 132.0(5) . . . . ? C76 C75 C78 F21 -46.7(7) . . . . ? C74 C75 C78 F19 14.2(7) . . . . ? C76 C75 C78 F19 -164.5(6) . . . . ? C84 C79 C80 C81 0.6(7) . . . . ? B2 C79 C80 C81 174.6(4) . . . . ? C79 C80 C81 C82 -0.7(7) . . . . ? C79 C80 C81 C85 179.1(4) . . . . ? C80 C81 C82 C83 0.9(7) . . . . ? C85 C81 C82 C83 -178.9(4) . . . . ? C81 C82 C83 C84 -1.0(7) . . . . ? C81 C82 C83 C86 179.1(4) . . . . ? C80 C79 C84 C83 -0.8(6) . . . . ? B2 C79 C84 C83 -174.5(4) . . . . ? C82 C83 C84 C79 1.0(7) . . . . ? C86 C83 C84 C79 -179.1(4) . . . . ? C82 C81 C85 F16 2.6(7) . . . . ? C80 C81 C85 F16 -177.2(5) . . . . ? C82 C81 C85 F18 125.7(5) . . . . ? C80 C81 C85 F18 -54.1(6) . . . . ? C82 C81 C85 F17 -116.7(5) . . . . ? C80 C81 C85 F17 63.5(6) . . . . ? C82 C83 C86 F15 -127.6(4) . . . . ? C84 C83 C86 F15 52.6(6) . . . . ? C82 C83 C86 F13 -7.3(7) . . . . ? C84 C83 C86 F13 172.8(4) . . . . ? C82 C83 C86 F14 112.9(5) . . . . ? C84 C83 C86 F14 -67.0(5) . . . . ? C60 C55 B1 C55 83.2(4) . . . 2 ? C56 C55 B1 C55 -90.3(4) . . . 2 ? C60 C55 B1 C63 -38.0(5) . . . 2 ? C56 C55 B1 C63 148.5(3) . . . 2 ? C60 C55 B1 C63 -154.6(3) . . . . ? C56 C55 B1 C63 31.8(5) . . . . ? C68 C63 B1 C55 42.9(5) . . . . ? C64 C63 B1 C55 -140.6(3) . . . . ? C68 C63 B1 C55 159.8(3) . . . 2 ? C64 C63 B1 C55 -23.7(5) . . . 2 ? C68 C63 B1 C63 -79.1(3) . . . 2 ? C64 C63 B1 C63 97.4(4) . . . 2 ? C72 C71 B2 C71 80.3(4) . . . 2_655 ? C76 C71 B2 C71 -95.8(4) . . . 2_655 ? C72 C71 B2 C79 -156.0(4) . . . 2_655 ? C76 C71 B2 C79 27.9(5) . . . 2_655 ? C72 C71 B2 C79 -41.8(6) . . . . ? C76 C71 B2 C79 142.1(4) . . . . ? C84 C79 B2 C71 -142.4(4) . . . 2_655 ? C80 C79 B2 C71 44.1(5) . . . 2_655 ? C84 C79 B2 C71 -23.4(6) . . . . ? C80 C79 B2 C71 163.1(4) . . . . ? C84 C79 B2 C79 96.3(4) . . . 2_655 ? C80 C79 B2 C79 -77.2(4) . . . 2_655 ? N2 C1 N1 C2 1.5(4) . . . . ? Pt1 C1 N1 C2 -170.3(3) . . . . ? N2 C1 N1 C16 -172.9(3) . . . . ? Pt1 C1 N1 C16 15.3(5) . . . . ? C3 C2 N1 C1 -0.5(4) . . . . ? C3 C2 N1 C16 174.1(4) . . . . ? C17 C16 N1 C1 -110.9(4) . . . . ? C21 C16 N1 C1 73.2(5) . . . . ? C17 C16 N1 C2 75.4(5) . . . . ? C21 C16 N1 C2 -100.5(4) . . . . ? N1 C1 N2 C3 -1.9(4) . . . . ? Pt1 C1 N2 C3 169.7(3) . . . . ? N1 C1 N2 C4 171.2(4) . . . . ? Pt1 C1 N2 C4 -17.2(5) . . . . ? C2 C3 N2 C1 1.6(4) . . . . ? C2 C3 N2 C4 -172.1(3) . . . . ? C5 C4 N2 C1 94.8(5) . . . . ? C9 C4 N2 C1 -92.0(5) . . . . ? C5 C4 N2 C3 -92.7(4) . . . . ? C9 C4 N2 C3 80.5(4) . . . . ? N4 C28 N3 C29 -0.6(4) . . . . ? Pt2 C28 N3 C29 176.7(3) . . . . ? N4 C28 N3 C43 174.6(4) . . . . ? Pt2 C28 N3 C43 -8.2(6) . . . . ? C30 C29 N3 C28 -0.3(5) . . . . ? C30 C29 N3 C43 -175.8(4) . . . . ? C44 C43 N3 C28 -78.2(5) . . . . ? C48 C43 N3 C28 105.7(5) . . . . ? C44 C43 N3 C29 96.4(5) . . . . ? C48 C43 N3 C29 -79.6(5) . . . . ? N3 C28 N4 C30 1.2(4) . . . . ? Pt2 C28 N4 C30 -176.0(3) . . . . ? N3 C28 N4 C31 -177.7(4) . . . . ? Pt2 C28 N4 C31 5.2(6) . . . . ? C29 C30 N4 C28 -1.4(5) . . . . ? C29 C30 N4 C31 177.5(4) . . . . ? C32 C31 N4 C28 101.1(5) . . . . ? C36 C31 N4 C28 -85.3(6) . . . . ? C32 C31 N4 C30 -77.7(6) . . . . ? C36 C31 N4 C30 95.9(5) . . . . ? N2 C1 Pt1 C1 172.6(4) . . . 2_655 ? N1 C1 Pt1 C1 -17.5(3) . . . 2_655 ? N2 C1 Pt1 I1 -95.9(3) . . . 2_655 ? N1 C1 Pt1 I1 74.0(3) . . . 2_655 ? N2 C1 Pt1 I1 81.1(3) . . . . ? N1 C1 Pt1 I1 -108.9(3) . . . . ? N3 C28 Pt2 C28 15.3(3) . . . 2 ? N4 C28 Pt2 C28 -168.1(4) . . . 2 ? N3 C28 Pt2 I2 -75.2(3) . . . . ? N4 C28 Pt2 I2 101.4(3) . . . . ? N3 C28 Pt2 I2 105.9(3) . . . 2 ? N4 C28 Pt2 I2 -77.5(3) . . . 2 ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.214 _refine_diff_density_min -1.900 _refine_diff_density_rms 0.127 #===END _database_code_depnum_ccdc_archive 'CCDC 969274'