# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Andrei Vedernikov' _publ_contact_author_name 'Andrei Vedernikov' _publ_contact_author_address ; Chemistry & Biochemistry University of Maryland College Park Maryland 20742 UNITED STATES OF AMERICA ; _publ_contact_author_email AVEDERNI@UMD.EDU _publ_section_title ; Aryl-Bromide Reductive Elimination from an Isolated Pt(IV) Complex ; # Attachment 'ar32.cif' data_ar32 _database_code_depnum_ccdc_archive 'CCDC 763113' #TrackingRef 'ar32.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 Br F5 N2 P2 Pt' _chemical_formula_sum 'C24 H28 Br F5 N2 P2 Pt' _chemical_formula_weight 776.42 _chemical_absolute_configuration ad 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.8747(3) _cell_length_b 15.3391(5) _cell_length_c 10.0545(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.294(2) _cell_angle_gamma 90.00 _cell_volume 1368.37(8) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2350 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.84 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 6.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2830 _exptl_absorpt_correction_T_max 0.5515 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14770 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.84 _reflns_number_total 6166 _reflns_number_gt 4989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution SIR-97 _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. The peripheral aromatic fragments exhibit large-amplitude thermal motion. ; _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^)+(0.0410P)^2^+0.4117P] 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 -0.015(9) _refine_ls_number_reflns 6166 _refine_ls_number_parameters 324 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.38500(3) 0.12614(2) 0.13199(3) 0.03121(9) Uani 1 1 d . . . Br2 Br 0.22102(12) 0.23129(7) 0.00939(11) 0.0482(3) Uani 1 1 d . . . P3 P 0.5505(2) 0.03899(15) 0.2386(2) 0.0305(5) Uani 1 1 d . . . P4 P 0.3929(2) 0.21582(15) 0.3125(2) 0.0323(5) Uani 1 1 d . . . C5 C 0.6044(9) 0.0931(6) 0.3960(9) 0.032(2) Uani 1 1 d . . . N6 N 0.7012(8) 0.0532(5) 0.4783(7) 0.0325(16) Uani 1 1 d . . . C7 C 0.7554(10) 0.1033(5) 0.5795(8) 0.034(2) Uani 1 1 d . . . C8 C 0.8656(10) 0.0661(6) 0.6735(9) 0.039(2) Uani 1 1 d . . . H8 H 0.8925 0.0063 0.6674 0.047 Uiso 1 1 calc R . . C9 C 0.9291(8) 0.1168(9) 0.7693(8) 0.041(2) Uani 1 1 d . . . H9 H 1.0036 0.0929 0.8280 0.050 Uiso 1 1 calc R . . C10 C 0.8860(10) 0.2051(8) 0.7830(9) 0.052(3) Uani 1 1 d . . . H10 H 0.9320 0.2394 0.8514 0.062 Uiso 1 1 calc R . . C11 C 0.7804(9) 0.2422(6) 0.7010(9) 0.040(2) Uani 1 1 d . . . H11 H 0.7514 0.3013 0.7126 0.049 Uiso 1 1 calc R . . C12 C 0.7149(9) 0.1916(6) 0.5984(8) 0.0329(19) Uani 1 1 d . . . N13 N 0.6025(7) 0.2276(5) 0.5183(7) 0.0315(15) Uani 1 1 d . . . C14 C 0.5494(9) 0.1778(6) 0.4215(9) 0.030(2) Uani 1 1 d . . . C15 C 0.3440(9) 0.0413(6) -0.0267(9) 0.0321(19) Uani 1 1 d . . . C16 C 0.2464(10) -0.0262(8) -0.0142(9) 0.044(2) Uani 1 1 d . . . C17 C 0.1924(10) -0.0782(7) -0.1204(10) 0.048(2) Uani 1 1 d . . . C18 C 0.2421(10) -0.0586(6) -0.2459(9) 0.041(2) Uani 1 1 d . . . C19 C 0.3447(10) 0.0055(7) -0.2619(8) 0.041(2) Uani 1 1 d . . . C20 C 0.3931(9) 0.0569(6) -0.1538(8) 0.0354(19) Uani 1 1 d . . . F21 F 0.4908(4) 0.1216(5) -0.1778(4) 0.0450(11) Uani 1 1 d . . . F22 F 0.4030(6) 0.0213(5) -0.3833(5) 0.0537(14) Uani 1 1 d . . . F23 F 0.1977(7) -0.1073(4) -0.3512(6) 0.0621(16) Uani 1 1 d . . . F24 F 0.0921(6) -0.1451(4) -0.1002(6) 0.0559(16) Uani 1 1 d . . . F25 F 0.1923(6) -0.0488(4) 0.1077(5) 0.0459(13) Uani 1 1 d . . . C26 C 0.4844(11) -0.0669(6) 0.2897(10) 0.041(2) Uani 1 1 d . . . H26A H 0.5550 -0.0916 0.3560 0.062 Uiso 1 1 calc R . . H26B H 0.4776 -0.1056 0.2123 0.062 Uiso 1 1 calc R . . H26C H 0.3847 -0.0610 0.3287 0.062 Uiso 1 1 calc R . . C27 C 0.4301(13) 0.3303(7) 0.2870(12) 0.051(3) Uani 1 1 d . . . H27A H 0.4497 0.3585 0.3732 0.077 Uiso 1 1 calc R . . H27B H 0.3424 0.3576 0.2430 0.077 Uiso 1 1 calc R . . H27C H 0.5184 0.3370 0.2311 0.077 Uiso 1 1 calc R . . C28 C 0.7356(9) 0.0212(6) 0.1548(9) 0.038(2) Uani 1 1 d . . . C29 C 0.8126(9) 0.1104(8) 0.1452(9) 0.048(3) Uani 1 1 d . . . H29A H 0.8333 0.1331 0.2349 0.073 Uiso 1 1 calc R . . H29B H 0.7462 0.1509 0.0964 0.073 Uiso 1 1 calc R . . H29C H 0.9075 0.1043 0.0981 0.073 Uiso 1 1 calc R . . C30 C 0.7067(10) -0.0143(7) 0.0147(9) 0.043(2) Uani 1 1 d . . . H30A H 0.8029 -0.0293 -0.0254 0.064 Uiso 1 1 calc R . . H30B H 0.6552 0.0301 -0.0396 0.064 Uiso 1 1 calc R . . H30C H 0.6433 -0.0665 0.0192 0.064 Uiso 1 1 calc R . . C31 C 0.8333(10) -0.0442(8) 0.2318(10) 0.053(3) Uani 1 1 d . . . H31A H 0.9292 -0.0519 0.1867 0.079 Uiso 1 1 calc R . . H31B H 0.7808 -0.1003 0.2359 0.079 Uiso 1 1 calc R . . H31C H 0.8528 -0.0225 0.3222 0.079 Uiso 1 1 calc R . . C32 C 0.2211(9) 0.2072(6) 0.4151(9) 0.039(2) Uani 1 1 d . . . C33 C 0.2535(10) 0.2341(7) 0.5604(9) 0.046(2) Uani 1 1 d . . . H33A H 0.1589 0.2355 0.6087 0.070 Uiso 1 1 calc R . . H33B H 0.2998 0.2921 0.5625 0.070 Uiso 1 1 calc R . . H33C H 0.3224 0.1919 0.6024 0.070 Uiso 1 1 calc R . . C34 C 0.1645(9) 0.1133(9) 0.4098(9) 0.047(3) Uani 1 1 d . . . H34A H 0.0784 0.1070 0.4684 0.071 Uiso 1 1 calc R . . H34B H 0.2455 0.0739 0.4393 0.071 Uiso 1 1 calc R . . H34C H 0.1333 0.0988 0.3184 0.071 Uiso 1 1 calc R . . C35 C 0.0972(11) 0.2669(8) 0.3565(11) 0.062(3) Uani 1 1 d . . . H35A H 0.0752 0.2502 0.2640 0.093 Uiso 1 1 calc R . . H35B H 0.1317 0.3276 0.3596 0.093 Uiso 1 1 calc R . . H35C H 0.0058 0.2610 0.4086 0.093 Uiso 1 1 calc R . . 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 0.02985(13) 0.03342(15) 0.02999(14) 0.0009(2) -0.00731(9) -0.0024(2) Br2 0.0498(6) 0.0454(6) 0.0484(6) -0.0015(5) -0.0249(5) 0.0088(5) P3 0.0318(10) 0.0314(12) 0.0281(11) 0.0014(9) -0.0046(9) 0.0006(9) P4 0.0307(10) 0.0323(12) 0.0335(12) -0.0009(10) -0.0093(9) -0.0025(9) C5 0.026(4) 0.032(5) 0.037(5) 0.002(3) -0.001(4) 0.001(3) N6 0.035(4) 0.037(4) 0.026(4) 0.001(3) -0.004(3) 0.004(3) C7 0.043(4) 0.042(7) 0.018(4) 0.011(3) 0.004(3) 0.015(4) C8 0.047(5) 0.040(5) 0.030(5) 0.020(4) -0.005(4) 0.009(4) C9 0.032(4) 0.058(7) 0.035(4) 0.000(6) 0.000(3) -0.002(6) C10 0.033(5) 0.090(9) 0.031(5) -0.005(5) -0.012(4) 0.004(5) C11 0.037(5) 0.041(5) 0.043(5) -0.009(4) -0.007(4) 0.002(4) C12 0.036(4) 0.047(5) 0.015(4) -0.002(4) -0.001(3) -0.004(4) N13 0.026(3) 0.035(4) 0.034(4) -0.004(3) -0.002(3) -0.004(3) C14 0.028(4) 0.033(5) 0.030(5) -0.002(4) -0.003(4) 0.000(4) C15 0.028(4) 0.029(5) 0.040(5) 0.011(4) 0.004(4) 0.007(3) C16 0.035(5) 0.068(7) 0.027(5) 0.006(5) -0.007(4) -0.003(5) C17 0.035(5) 0.062(7) 0.046(6) -0.010(5) -0.003(4) -0.008(5) C18 0.037(5) 0.051(6) 0.035(5) -0.022(4) -0.008(4) 0.004(4) C19 0.041(5) 0.060(6) 0.023(4) 0.002(4) 0.001(4) 0.011(5) C20 0.034(4) 0.043(5) 0.029(5) 0.007(4) -0.006(4) 0.000(4) F21 0.042(2) 0.052(3) 0.041(2) 0.014(4) -0.0017(19) -0.011(4) F22 0.060(3) 0.071(4) 0.029(3) 0.004(3) -0.003(3) 0.007(3) F23 0.061(4) 0.074(4) 0.051(4) -0.029(3) -0.012(3) -0.005(3) F24 0.055(3) 0.053(4) 0.059(4) -0.019(3) 0.001(3) -0.025(3) F25 0.045(3) 0.063(4) 0.030(3) -0.007(2) 0.006(2) -0.017(3) C26 0.053(6) 0.036(5) 0.034(5) 0.001(4) -0.011(4) -0.003(5) C27 0.061(7) 0.029(5) 0.063(7) -0.002(5) -0.016(6) -0.009(5) C28 0.028(4) 0.036(5) 0.049(5) -0.003(4) -0.006(4) 0.004(4) C29 0.033(4) 0.070(8) 0.043(5) 0.001(5) 0.006(3) -0.013(5) C30 0.040(5) 0.057(6) 0.032(5) -0.002(4) 0.003(4) 0.010(4) C31 0.038(5) 0.075(7) 0.045(6) -0.003(5) 0.000(4) 0.020(5) C32 0.029(4) 0.041(5) 0.046(5) -0.006(4) -0.006(4) 0.002(4) C33 0.041(5) 0.052(6) 0.046(6) -0.018(5) 0.003(4) -0.004(5) C34 0.038(4) 0.066(8) 0.039(4) -0.010(6) -0.003(3) -0.003(6) C35 0.045(6) 0.071(8) 0.070(8) 0.007(6) -0.001(5) 0.009(5) _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 C15 2.084(9) . ? Pt1 P3 2.241(2) . ? Pt1 P4 2.277(2) . ? Pt1 Br2 2.4815(10) . ? P3 C26 1.806(10) . ? P3 C5 1.841(9) . ? P3 C28 1.883(8) . ? P4 C27 1.806(10) . ? P4 C14 1.844(9) . ? P4 C32 1.865(9) . ? C5 N6 1.329(11) . ? C5 C14 1.412(12) . ? N6 C7 1.355(11) . ? C7 C12 1.415(13) . ? C7 C8 1.461(12) . ? C8 C9 1.351(14) . ? C8 H8 0.9500 . ? C9 C10 1.416(17) . ? C9 H9 0.9500 . ? C10 C11 1.359(13) . ? C10 H10 0.9500 . ? C11 C12 1.406(12) . ? C11 H11 0.9500 . ? C12 N13 1.383(11) . ? N13 C14 1.316(10) . ? C15 C16 1.358(13) . ? C15 C20 1.380(12) . ? C16 F25 1.370(10) . ? C16 C17 1.408(14) . ? C17 F24 1.377(11) . ? C17 C18 1.380(14) . ? C18 F23 1.347(10) . ? C18 C19 1.353(13) . ? C19 F22 1.358(9) . ? C19 C20 1.403(13) . ? C20 F21 1.343(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C31 1.525(13) . ? C28 C30 1.526(12) . ? C28 C29 1.534(14) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.526(16) . ? C32 C33 1.538(12) . ? C32 C35 1.538(14) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 C15 Pt1 P3 95.5(2) . . ? C15 Pt1 P4 171.4(2) . . ? P3 Pt1 P4 88.34(8) . . ? C15 Pt1 Br2 86.3(2) . . ? P3 Pt1 Br2 174.86(7) . . ? P4 Pt1 Br2 90.60(6) . . ? C26 P3 C5 103.9(4) . . ? C26 P3 C28 106.8(5) . . ? C5 P3 C28 103.8(4) . . ? C26 P3 Pt1 117.3(3) . . ? C5 P3 Pt1 107.3(3) . . ? C28 P3 Pt1 116.2(3) . . ? C27 P4 C14 104.7(5) . . ? C27 P4 C32 107.5(5) . . ? C14 P4 C32 105.2(4) . . ? C27 P4 Pt1 118.5(4) . . ? C14 P4 Pt1 107.0(3) . . ? C32 P4 Pt1 112.8(3) . . ? N6 C5 C14 122.2(9) . . ? N6 C5 P3 118.6(7) . . ? C14 C5 P3 119.1(7) . . ? C5 N6 C7 114.8(7) . . ? N6 C7 C12 123.9(8) . . ? N6 C7 C8 119.0(8) . . ? C12 C7 C8 117.0(8) . . ? C9 C8 C7 119.9(9) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.7(9) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 121.7(9) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 118.8(9) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N13 C12 C11 119.2(8) . . ? N13 C12 C7 119.0(8) . . ? C11 C12 C7 121.7(8) . . ? C14 N13 C12 116.1(7) . . ? N13 C14 C5 123.2(8) . . ? N13 C14 P4 120.5(6) . . ? C5 C14 P4 116.2(7) . . ? C16 C15 C20 115.7(9) . . ? C16 C15 Pt1 120.4(6) . . ? C20 C15 Pt1 123.2(6) . . ? C15 C16 F25 120.9(9) . . ? C15 C16 C17 124.7(9) . . ? F25 C16 C17 114.5(9) . . ? F24 C17 C18 121.2(8) . . ? F24 C17 C16 121.4(9) . . ? C18 C17 C16 117.4(9) . . ? F23 C18 C19 119.7(8) . . ? F23 C18 C17 120.3(9) . . ? C19 C18 C17 119.9(8) . . ? C18 C19 F22 120.5(8) . . ? C18 C19 C20 120.7(8) . . ? F22 C19 C20 118.7(8) . . ? F21 C20 C15 120.9(8) . . ? F21 C20 C19 117.6(7) . . ? C15 C20 C19 121.5(8) . . ? P3 C26 H26A 109.5 . . ? P3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P4 C27 H27A 109.5 . . ? P4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? P4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C28 C30 108.4(8) . . ? C31 C28 C29 111.7(7) . . ? C30 C28 C29 109.0(8) . . ? C31 C28 P3 111.1(6) . . ? C30 C28 P3 109.5(6) . . ? C29 C28 P3 107.0(6) . . ? 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 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 109.9(8) . . ? C34 C32 C35 108.5(8) . . ? C33 C32 C35 108.7(8) . . ? C34 C32 P4 108.7(6) . . ? C33 C32 P4 111.6(6) . . ? C35 C32 P4 109.4(7) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.640 _refine_diff_density_min -1.719 _refine_diff_density_rms 0.152 # Attachment 'ar34.cif' data_ar34 _database_code_depnum_ccdc_archive 'CCDC 763114' #TrackingRef 'ar34.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H32 Br2 F6 N2 P2 Pt' _chemical_formula_sum 'C30 H32 Br2 F6 N2 P2 Pt' _chemical_formula_weight 951.43 _chemical_absolute_configuration ad 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.3414(2) _cell_length_b 12.3660(3) _cell_length_c 30.6670(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3921.75(15) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4846 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.70 _exptl_crystal_description rods _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 5.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2775 _exptl_absorpt_correction_T_max 0.4794 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22362 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.70 _reflns_number_total 8896 _reflns_number_gt 6359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _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. The lattice contains also severely disordered pentane solvent, as indicated by several residual electron-density peaks (within 1.0-1.7 e/A**3) present in areas between molecules of the Pt-compound. The pentane solvent could not be modeled by discrete atoms, and was therefore excluded from the structural model. ; _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^)+(0.0789P)^2^+7.5669P] 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 -0.017(12) _refine_ls_number_reflns 8896 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _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 0.16605(4) 0.00723(3) 0.132558(13) 0.02887(12) Uani 1 1 d . . . Br2 Br 0.24344(12) 0.06737(10) 0.20519(4) 0.0420(3) Uani 1 1 d . . . Br3 Br 0.08479(12) -0.05790(10) 0.06123(4) 0.0386(3) Uani 1 1 d . . . P4 P -0.0524(3) -0.0123(3) 0.16352(9) 0.0319(6) Uani 1 1 d . . . P5 P 0.1089(3) 0.1922(2) 0.11961(10) 0.0329(7) Uani 1 1 d . . . C6 C -0.1117(12) 0.1268(11) 0.1676(4) 0.039(3) Uani 1 1 d . . . N7 N -0.2281(10) 0.1401(8) 0.1864(3) 0.038(2) Uani 1 1 d . . . C8 C -0.2707(13) 0.2448(11) 0.1895(4) 0.047(3) Uani 1 1 d . . . C9 C -0.3947(13) 0.2617(11) 0.2106(4) 0.047(3) Uani 1 1 d . . . H9 H -0.4450 0.2031 0.2212 0.057 Uiso 1 1 calc R . . C10 C -0.4339(14) 0.3629(14) 0.2142(5) 0.063(4) Uani 1 1 d . . . H10 H -0.5160 0.3758 0.2271 0.075 Uiso 1 1 calc R . . C11 C -0.3593(15) 0.4556(14) 0.1998(5) 0.065(4) Uani 1 1 d . . . H11 H -0.3898 0.5268 0.2051 0.079 Uiso 1 1 calc R . . C12 C -0.2471(14) 0.4399(11) 0.1789(4) 0.055(4) Uani 1 1 d . . . H12 H -0.2000 0.4998 0.1678 0.066 Uiso 1 1 calc R . . C13 C -0.1980(12) 0.3306(9) 0.1734(4) 0.037(3) Uani 1 1 d . . . N14 N -0.0818(10) 0.3169(8) 0.1540(3) 0.036(2) Uani 1 1 d . . . C15 C -0.0395(12) 0.2155(10) 0.1490(4) 0.038(3) Uani 1 1 d . . . C16 C 0.2313(12) -0.1501(9) 0.1480(4) 0.035(3) Uani 1 1 d . . . C17 C 0.3529(11) -0.1734(10) 0.1637(4) 0.038(3) Uani 1 1 d . . . C18 C 0.3940(12) -0.2752(11) 0.1724(4) 0.042(3) Uani 1 1 d . . . C19 C 0.3142(13) -0.3621(10) 0.1668(5) 0.049(3) Uani 1 1 d . . . C20 C 0.1977(13) -0.3452(9) 0.1497(4) 0.043(3) Uani 1 1 d . . . C21 C 0.1554(11) -0.2401(8) 0.1412(4) 0.036(3) Uani 1 1 d . . . F22 F 0.4410(6) -0.0944(6) 0.1716(2) 0.0447(18) Uani 1 1 d . . . F23 F 0.5181(7) -0.2926(6) 0.1885(3) 0.054(2) Uani 1 1 d . . . F24 F 0.3577(7) -0.4652(5) 0.1749(3) 0.061(2) Uani 1 1 d . . . F25 F 0.1149(7) -0.4295(5) 0.1404(3) 0.055(2) Uani 1 1 d . . . F26 F 0.0323(6) -0.2337(5) 0.1272(3) 0.0459(18) Uani 1 1 d . . . C27 C 0.3493(10) 0.0297(9) 0.1034(3) 0.033(3) Uani 1 1 d . . . C28 C 0.4328(12) 0.1102(11) 0.1156(4) 0.044(3) Uani 1 1 d . . . H28 H 0.4105 0.1564 0.1392 0.053 Uiso 1 1 calc R . . C29 C 0.5529(11) 0.1257(11) 0.0935(5) 0.049(4) Uani 1 1 d . . . H29 H 0.6078 0.1842 0.1012 0.059 Uiso 1 1 calc R . . C30 C 0.5866(11) 0.0589(12) 0.0626(4) 0.041(3) Uani 1 1 d . . . C31 C 0.5068(13) -0.0248(12) 0.0503(4) 0.055(4) Uani 1 1 d . . . H31 H 0.5337 -0.0724 0.0278 0.065 Uiso 1 1 calc R . . C32 C 0.3897(11) -0.0406(11) 0.0699(4) 0.045(3) Uani 1 1 d . . . H32 H 0.3357 -0.0987 0.0610 0.054 Uiso 1 1 calc R . . F33 F 0.7011(6) 0.0709(7) 0.0423(3) 0.065(2) Uani 1 1 d . . . C34 C -0.1771(10) -0.0675(10) 0.1284(4) 0.042(3) Uani 1 1 d . . . H34A H -0.2623 -0.0519 0.1409 0.063 Uiso 1 1 calc R . . H34B H -0.1657 -0.1460 0.1260 0.063 Uiso 1 1 calc R . . H34C H -0.1706 -0.0346 0.0994 0.063 Uiso 1 1 calc R . . C35 C -0.0882(12) -0.0701(10) 0.2194(4) 0.044(3) Uani 1 1 d . . . C36 C -0.2245(12) -0.1117(12) 0.2222(4) 0.050(3) Uani 1 1 d . . . H36A H -0.2423 -0.1583 0.1971 0.075 Uiso 1 1 calc R . . H36B H -0.2848 -0.0506 0.2222 0.075 Uiso 1 1 calc R . . H36C H -0.2352 -0.1533 0.2492 0.075 Uiso 1 1 calc R . . C37 C -0.0646(13) 0.0148(11) 0.2563(4) 0.048(3) Uani 1 1 d . . . H37A H -0.1274 0.0737 0.2535 0.073 Uiso 1 1 calc R . . H37B H 0.0232 0.0439 0.2537 0.073 Uiso 1 1 calc R . . H37C H -0.0748 -0.0201 0.2848 0.073 Uiso 1 1 calc R . . C38 C 0.0043(13) -0.1697(10) 0.2248(4) 0.043(3) Uani 1 1 d . . . H38A H 0.0041 -0.1934 0.2553 0.065 Uiso 1 1 calc R . . H38B H 0.0922 -0.1491 0.2163 0.065 Uiso 1 1 calc R . . H38C H -0.0257 -0.2290 0.2062 0.065 Uiso 1 1 calc R . . C39 C 0.2131(12) 0.2935(9) 0.1434(4) 0.036(3) Uani 1 1 d . . . H39A H 0.1655 0.3617 0.1462 0.054 Uiso 1 1 calc R . . H39B H 0.2885 0.3044 0.1245 0.054 Uiso 1 1 calc R . . H39C H 0.2417 0.2694 0.1722 0.054 Uiso 1 1 calc R . . C40 C 0.0750(13) 0.2468(10) 0.0627(4) 0.042(3) Uani 1 1 d . . . C41 C -0.0522(12) 0.2019(11) 0.0468(4) 0.046(3) Uani 1 1 d . . . H41A H -0.0627 0.2185 0.0157 0.069 Uiso 1 1 calc R . . H41B H -0.1232 0.2348 0.0633 0.069 Uiso 1 1 calc R . . H41C H -0.0534 0.1234 0.0510 0.069 Uiso 1 1 calc R . . C42 C 0.1903(13) 0.2153(10) 0.0332(4) 0.045(3) Uani 1 1 d . . . H42A H 0.2089 0.1381 0.0367 0.067 Uiso 1 1 calc R . . H42B H 0.2666 0.2576 0.0416 0.067 Uiso 1 1 calc R . . H42C H 0.1687 0.2303 0.0027 0.067 Uiso 1 1 calc R . . C43 C 0.0686(15) 0.3736(11) 0.0640(4) 0.055(4) Uani 1 1 d . . . H43A H 0.1536 0.4026 0.0719 0.082 Uiso 1 1 calc R . . H43B H 0.0044 0.3965 0.0856 0.082 Uiso 1 1 calc R . . H43C H 0.0438 0.4010 0.0352 0.082 Uiso 1 1 calc R . . 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 0.02869(19) 0.0238(2) 0.0341(2) 0.0035(2) 0.00095(18) 0.00277(19) Br2 0.0457(7) 0.0411(7) 0.0392(6) 0.0026(6) -0.0049(6) -0.0003(6) Br3 0.0413(6) 0.0347(6) 0.0398(7) 0.0002(6) -0.0011(6) 0.0002(5) P4 0.0281(13) 0.0307(16) 0.0371(14) 0.0050(15) 0.0016(11) 0.0050(13) P5 0.0346(16) 0.0268(15) 0.0373(17) 0.0034(13) -0.0012(13) 0.0007(12) C6 0.034(7) 0.047(8) 0.036(7) 0.008(6) -0.001(5) 0.010(6) N7 0.041(6) 0.036(6) 0.037(5) 0.004(4) 0.003(5) 0.008(5) C8 0.039(7) 0.062(9) 0.039(7) -0.001(6) -0.003(6) 0.026(7) C9 0.038(7) 0.058(9) 0.046(8) 0.000(7) 0.009(6) 0.018(6) C10 0.047(9) 0.089(13) 0.052(9) -0.008(8) 0.009(7) 0.037(9) C11 0.068(10) 0.068(10) 0.060(9) -0.013(8) -0.010(8) 0.043(8) C12 0.052(8) 0.050(8) 0.062(9) -0.002(7) -0.005(7) 0.030(7) C13 0.049(8) 0.032(6) 0.029(6) -0.002(5) -0.021(5) 0.015(5) N14 0.043(6) 0.029(5) 0.037(6) -0.006(4) 0.000(5) 0.009(5) C15 0.038(7) 0.037(7) 0.038(7) 0.006(5) -0.009(5) 0.005(5) C16 0.039(7) 0.021(6) 0.043(7) 0.006(5) 0.005(6) 0.003(5) C17 0.033(7) 0.036(6) 0.046(7) 0.009(6) 0.011(6) 0.010(6) C18 0.030(7) 0.043(8) 0.053(8) 0.006(6) -0.003(6) 0.006(6) C19 0.045(8) 0.039(7) 0.065(9) 0.012(7) 0.001(7) 0.014(6) C20 0.049(8) 0.024(6) 0.057(8) 0.007(6) -0.001(6) -0.004(5) C21 0.035(6) 0.023(5) 0.050(7) 0.005(5) -0.007(6) 0.008(5) F22 0.038(4) 0.039(4) 0.057(4) 0.017(4) -0.013(3) -0.008(3) F23 0.053(5) 0.038(4) 0.072(5) 0.007(4) -0.009(4) 0.010(4) F24 0.055(5) 0.031(4) 0.096(6) 0.018(4) -0.003(4) 0.013(3) F25 0.057(4) 0.021(3) 0.086(6) 0.008(4) 0.001(4) 0.000(3) F26 0.036(4) 0.030(3) 0.071(5) 0.001(4) -0.006(4) 0.000(3) C27 0.028(6) 0.044(7) 0.027(5) 0.016(5) 0.003(5) 0.010(5) C28 0.037(7) 0.046(8) 0.049(8) 0.004(6) -0.014(6) 0.009(6) C29 0.026(6) 0.048(8) 0.073(10) 0.024(8) -0.008(7) -0.011(6) C30 0.023(6) 0.059(8) 0.041(7) 0.022(7) 0.007(6) 0.005(6) C31 0.044(7) 0.064(11) 0.056(8) 0.009(7) 0.020(6) 0.012(7) C32 0.036(6) 0.057(8) 0.042(7) 0.017(6) 0.012(6) 0.012(6) F33 0.031(4) 0.090(6) 0.076(5) 0.041(5) 0.011(4) -0.006(4) C34 0.027(6) 0.048(7) 0.050(7) 0.001(6) -0.005(6) -0.006(5) C35 0.040(7) 0.039(7) 0.054(8) 0.022(6) -0.001(6) 0.001(6) C36 0.040(7) 0.058(9) 0.052(8) 0.012(7) 0.001(6) -0.008(6) C37 0.057(7) 0.053(8) 0.035(6) 0.013(7) 0.010(6) 0.011(7) C38 0.042(7) 0.036(7) 0.052(8) 0.016(6) 0.005(6) 0.001(6) C39 0.044(7) 0.033(6) 0.031(6) -0.002(5) -0.005(5) 0.008(5) C40 0.048(7) 0.030(7) 0.049(7) 0.005(6) 0.011(7) -0.009(6) C41 0.040(8) 0.056(9) 0.042(7) 0.003(6) -0.004(6) 0.013(6) C42 0.051(8) 0.045(7) 0.038(7) 0.017(6) 0.009(6) 0.006(6) C43 0.067(9) 0.054(9) 0.043(8) 0.021(7) -0.002(7) 0.006(7) _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 C27 2.113(10) . ? Pt1 C16 2.113(11) . ? Pt1 P5 2.396(3) . ? Pt1 P4 2.462(3) . ? Pt1 Br3 2.4777(13) . ? Pt1 Br2 2.4809(12) . ? P4 C34 1.813(11) . ? P4 C6 1.830(13) . ? P4 C35 1.894(12) . ? P5 C15 1.803(13) . ? P5 C39 1.805(12) . ? P5 C40 1.905(13) . ? C6 N7 1.345(15) . ? C6 C15 1.444(17) . ? N7 C8 1.371(15) . ? C8 C13 1.391(18) . ? C8 C9 1.452(17) . ? C9 C10 1.320(19) . ? C9 H9 0.9500 . ? C10 C11 1.45(2) . ? C10 H10 0.9500 . ? C11 C12 1.34(2) . ? C11 H11 0.9500 . ? C12 C13 1.454(16) . ? C12 H12 0.9500 . ? C13 N14 1.351(15) . ? N14 C15 1.337(15) . ? C16 C17 1.377(17) . ? C16 C21 1.378(16) . ? C17 C18 1.355(17) . ? C17 F22 1.358(14) . ? C18 C19 1.366(18) . ? C18 F23 1.392(14) . ? C19 C20 1.329(18) . ? C19 F24 1.375(14) . ? C20 F25 1.379(14) . ? C20 C21 1.396(15) . ? C21 F26 1.346(13) . ? C27 C28 1.370(17) . ? C27 C32 1.410(17) . ? C28 C29 1.428(18) . ? C28 H28 0.9500 . ? C29 C30 1.304(19) . ? C29 H29 0.9500 . ? C30 F33 1.346(13) . ? C30 C31 1.376(19) . ? C31 C32 1.366(17) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.503(17) . ? C35 C37 1.562(18) . ? C35 C38 1.568(17) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.508(18) . ? C40 C42 1.546(18) . ? C40 C43 1.570(17) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? 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 C27 Pt1 C16 85.9(4) . . ? C27 Pt1 P5 91.5(3) . . ? C16 Pt1 P5 174.3(3) . . ? C27 Pt1 P4 176.9(3) . . ? C16 Pt1 P4 96.7(3) . . ? P5 Pt1 P4 86.06(11) . . ? C27 Pt1 Br3 88.5(3) . . ? C16 Pt1 Br3 90.4(3) . . ? P5 Pt1 Br3 94.61(8) . . ? P4 Pt1 Br3 89.85(8) . . ? C27 Pt1 Br2 92.9(3) . . ? C16 Pt1 Br2 88.4(3) . . ? P5 Pt1 Br2 86.69(8) . . ? P4 Pt1 Br2 88.80(8) . . ? Br3 Pt1 Br2 178.06(5) . . ? C34 P4 C6 99.0(6) . . ? C34 P4 C35 104.8(6) . . ? C6 P4 C35 103.1(6) . . ? C34 P4 Pt1 117.4(4) . . ? C6 P4 Pt1 104.0(4) . . ? C35 P4 Pt1 124.4(4) . . ? C15 P5 C39 101.3(6) . . ? C15 P5 C40 104.2(6) . . ? C39 P5 C40 103.5(5) . . ? C15 P5 Pt1 106.2(4) . . ? C39 P5 Pt1 116.6(4) . . ? C40 P5 Pt1 122.4(4) . . ? N7 C6 C15 122.7(11) . . ? N7 C6 P4 116.4(10) . . ? C15 C6 P4 120.9(9) . . ? C6 N7 C8 115.6(11) . . ? N7 C8 C13 121.5(11) . . ? N7 C8 C9 116.8(13) . . ? C13 C8 C9 121.7(12) . . ? C10 C9 C8 116.5(14) . . ? C10 C9 H9 121.8 . . ? C8 C9 H9 121.8 . . ? C9 C10 C11 124.0(13) . . ? C9 C10 H10 118.0 . . ? C11 C10 H10 118.0 . . ? C12 C11 C10 119.5(13) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 119.5(15) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? N14 C13 C8 122.8(10) . . ? N14 C13 C12 118.6(12) . . ? C8 C13 C12 118.7(12) . . ? C15 N14 C13 117.3(11) . . ? N14 C15 C6 119.8(11) . . ? N14 C15 P5 119.1(9) . . ? C6 C15 P5 121.1(9) . . ? C17 C16 C21 113.8(10) . . ? C17 C16 Pt1 124.2(9) . . ? C21 C16 Pt1 121.9(8) . . ? C18 C17 F22 115.0(11) . . ? C18 C17 C16 123.4(12) . . ? F22 C17 C16 121.6(10) . . ? C17 C18 C19 121.0(12) . . ? C17 C18 F23 120.2(12) . . ? C19 C18 F23 118.7(11) . . ? C20 C19 C18 118.3(11) . . ? C20 C19 F24 120.8(12) . . ? C18 C19 F24 120.6(12) . . ? C19 C20 F25 121.7(11) . . ? C19 C20 C21 120.2(12) . . ? F25 C20 C21 118.0(11) . . ? F26 C21 C16 122.6(9) . . ? F26 C21 C20 114.3(10) . . ? C16 C21 C20 123.0(11) . . ? C28 C27 C32 117.4(11) . . ? C28 C27 Pt1 123.0(9) . . ? C32 C27 Pt1 119.5(9) . . ? C27 C28 C29 121.1(13) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C28 119.5(13) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 F33 120.1(13) . . ? C29 C30 C31 121.0(11) . . ? F33 C30 C31 118.9(13) . . ? C32 C31 C30 121.2(13) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C27 119.7(13) . . ? C31 C32 H32 120.2 . . ? C27 C32 H32 120.2 . . ? P4 C34 H34A 109.5 . . ? P4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? P4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C37 109.6(11) . . ? C36 C35 C38 107.3(10) . . ? C37 C35 C38 110.9(10) . . ? C36 C35 P4 111.3(9) . . ? C37 C35 P4 111.8(8) . . ? C38 C35 P4 105.8(8) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P5 C39 H39A 109.5 . . ? P5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C42 113.0(11) . . ? C41 C40 C43 109.8(12) . . ? C42 C40 C43 107.4(10) . . ? C41 C40 P5 109.0(8) . . ? C42 C40 P5 107.7(9) . . ? C43 C40 P5 109.8(9) . . ? 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 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? # start Validation Reply Form _vrf_PLAT602_ar34 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: These voids are occupied by severely disordered pentane solvent, which could not be modeled by discrete atoms, and was thus excluded from the structural model. ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.763 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.196 # Attachment 'ar36.cif' data_ar36 _database_code_depnum_ccdc_archive 'CCDC 763115' #TrackingRef 'ar36.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H32 F6 N2 P2 Pt' _chemical_formula_sum 'C30 H32 F6 N2 P2 Pt' _chemical_formula_weight 791.61 _chemical_absolute_configuration ad 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.8934(2) _cell_length_b 15.6326(5) _cell_length_c 24.5087(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3024.24(17) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3731 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 4.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3266 _exptl_absorpt_correction_T_max 0.4466 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f scan' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16709 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.91 _reflns_number_total 6644 _reflns_number_gt 5375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _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^)+(0.0747P)^2^+0.6035P] 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 -0.002(11) _refine_ls_number_reflns 6644 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _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 -0.12626(4) -0.141312(19) -0.170136(12) 0.03957(11) Uani 1 1 d . . . P2 P -0.2395(3) -0.01698(15) -0.20260(9) 0.0458(6) Uani 1 1 d . . . P3 P -0.1747(3) -0.08999(13) -0.08442(9) 0.0398(5) Uani 1 1 d . . . C4 C -0.2944(11) 0.0095(5) -0.0905(4) 0.042(2) Uani 1 1 d . . . N5 N -0.3730(11) 0.0430(4) -0.0485(3) 0.0421(14) Uani 1 1 d . . . C6 C -0.4480(11) 0.1203(5) -0.0552(4) 0.044(2) Uani 1 1 d . . . C7 C -0.5392(12) 0.1570(6) -0.0123(5) 0.061(3) Uani 1 1 d . . . H7 H -0.5515 0.1279 0.0215 0.074 Uiso 1 1 calc R . . C8 C -0.6111(16) 0.2366(7) -0.0202(5) 0.072(3) Uani 1 1 d . . . H8 H -0.6766 0.2618 0.0081 0.086 Uiso 1 1 calc R . . C9 C -0.5884(17) 0.2811(7) -0.0698(6) 0.083(5) Uani 1 1 d . . . H9 H -0.6348 0.3369 -0.0732 0.099 Uiso 1 1 calc R . . C10 C -0.5047(16) 0.2480(6) -0.1122(5) 0.068(3) Uani 1 1 d . . . H10 H -0.4917 0.2792 -0.1452 0.081 Uiso 1 1 calc R . . C11 C -0.4346(13) 0.1637(6) -0.1063(4) 0.053(2) Uani 1 1 d . . . N12 N -0.3622(11) 0.1268(4) -0.1508(3) 0.0482(17) Uani 1 1 d . . . C13 C -0.2997(11) 0.0480(5) -0.1434(4) 0.0404(19) Uani 1 1 d . . . C14 C -0.0460(12) -0.2603(6) -0.1421(3) 0.045(2) Uani 1 1 d . . . C15 C -0.1571(12) -0.3240(6) -0.1286(4) 0.047(2) Uani 1 1 d . . . C16 C -0.1118(17) -0.4048(7) -0.1125(4) 0.061(3) Uani 1 1 d . . . C17 C 0.0558(19) -0.4251(8) -0.1099(4) 0.071(3) Uani 1 1 d . . . C18 C 0.1697(12) -0.3646(7) -0.1204(4) 0.057(3) Uani 1 1 d . . . C19 C 0.1226(15) -0.2845(6) -0.1374(4) 0.052(2) Uani 1 1 d . . . F20 F -0.3293(10) -0.3102(5) -0.1333(4) 0.093(2) Uani 1 1 d . . . F21 F -0.2400(13) -0.4696(5) -0.1043(4) 0.107(3) Uani 1 1 d . . . F22 F 0.1049(12) -0.5056(4) -0.0941(3) 0.087(2) Uani 1 1 d . . . F23 F 0.3338(12) -0.3891(5) -0.1150(3) 0.098(3) Uani 1 1 d . . . F24 F 0.2445(9) -0.2315(5) -0.1458(3) 0.085(2) Uani 1 1 d . . . C25 C -0.0769(11) -0.1887(6) -0.2481(4) 0.047(2) Uani 1 1 d . . . C26 C 0.0360(11) -0.1476(8) -0.2832(4) 0.060(3) Uani 1 1 d . . . H26 H 0.0907 -0.0964 -0.2718 0.071 Uiso 1 1 calc R . . C27 C 0.0703(13) -0.1827(8) -0.3370(4) 0.065(3) Uani 1 1 d . . . H27 H 0.1500 -0.1566 -0.3608 0.078 Uiso 1 1 calc R . . C28 C -0.0169(14) -0.2550(8) -0.3521(4) 0.062(3) Uani 1 1 d . . . C29 C -0.1358(14) -0.2926(6) -0.3195(4) 0.055(2) Uani 1 1 d . . . H29 H -0.1993 -0.3402 -0.3323 0.066 Uiso 1 1 calc R . . C30 C -0.1625(12) -0.2598(6) -0.2671(4) 0.051(2) Uani 1 1 d . . . H30 H -0.2419 -0.2873 -0.2439 0.061 Uiso 1 1 calc R . . F31 F 0.0147(10) -0.2880(5) -0.4019(3) 0.087(2) Uani 1 1 d . . . C32 C -0.2997(15) -0.1513(7) -0.0381(4) 0.061(3) Uani 1 1 d . . . H32A H -0.3371 -0.1147 -0.0079 0.092 Uiso 1 1 calc R . . H32B H -0.2319 -0.1986 -0.0236 0.092 Uiso 1 1 calc R . . H32C H -0.3989 -0.1742 -0.0572 0.092 Uiso 1 1 calc R . . C33 C 0.0185(12) -0.0562(6) -0.0455(4) 0.046(2) Uani 1 1 d . . . C34 C -0.0190(16) 0.0063(7) 0.0012(4) 0.067(3) Uani 1 1 d . . . H34A H 0.0845 0.0160 0.0224 0.101 Uiso 1 1 calc R . . H34B H -0.1067 -0.0178 0.0249 0.101 Uiso 1 1 calc R . . H34C H -0.0587 0.0608 -0.0140 0.101 Uiso 1 1 calc R . . C35 C 0.1043(19) -0.1349(7) -0.0225(6) 0.092(5) Uani 1 1 d . . . H35A H 0.1647 -0.1648 -0.0518 0.138 Uiso 1 1 calc R . . H35B H 0.0189 -0.1730 -0.0067 0.138 Uiso 1 1 calc R . . H35C H 0.1850 -0.1178 0.0058 0.138 Uiso 1 1 calc R . . C36 C 0.132(2) -0.0151(9) -0.0859(5) 0.084(4) Uani 1 1 d . . . H36A H 0.2409 -0.0018 -0.0686 0.125 Uiso 1 1 calc R . . H36B H 0.0798 0.0378 -0.0992 0.125 Uiso 1 1 calc R . . H36C H 0.1507 -0.0542 -0.1166 0.125 Uiso 1 1 calc R . . C37 C -0.1211(17) 0.0550(7) -0.2432(4) 0.069(3) Uani 1 1 d . . . H37A H -0.1740 0.1117 -0.2420 0.103 Uiso 1 1 calc R . . H37B H -0.1185 0.0344 -0.2810 0.103 Uiso 1 1 calc R . . H37C H -0.0051 0.0587 -0.2291 0.103 Uiso 1 1 calc R . . C38 C -0.4442(16) -0.0338(8) -0.2386(5) 0.070(3) Uani 1 1 d . . . C39 C -0.405(2) -0.0714(8) -0.2916(6) 0.099(5) Uani 1 1 d . . . H39A H -0.5109 -0.0876 -0.3100 0.148 Uiso 1 1 calc R . . H39B H -0.3346 -0.1223 -0.2865 0.148 Uiso 1 1 calc R . . H39C H -0.3444 -0.0295 -0.3140 0.148 Uiso 1 1 calc R . . C40 C -0.534(2) 0.0488(10) -0.2522(7) 0.105(6) Uani 1 1 d . . . H40A H -0.4556 0.0876 -0.2708 0.157 Uiso 1 1 calc R . . H40B H -0.5747 0.0756 -0.2185 0.157 Uiso 1 1 calc R . . H40C H -0.6308 0.0367 -0.2761 0.157 Uiso 1 1 calc R . . C41 C -0.5574(19) -0.0861(13) -0.2001(8) 0.142(9) Uani 1 1 d . . . H41A H -0.5550 -0.0606 -0.1636 0.214 Uiso 1 1 calc R . . H41B H -0.5156 -0.1451 -0.1982 0.214 Uiso 1 1 calc R . . H41C H -0.6740 -0.0861 -0.2139 0.214 Uiso 1 1 calc R . . 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 0.04554(18) 0.03956(16) 0.03362(15) -0.00582(13) 0.00169(15) -0.00542(15) P2 0.0600(15) 0.0463(13) 0.0311(12) 0.0015(10) -0.0021(10) -0.0101(11) P3 0.0551(14) 0.0331(11) 0.0313(10) 0.0006(8) 0.0000(9) -0.0002(9) C4 0.050(5) 0.034(4) 0.042(5) 0.002(4) -0.010(4) 0.000(4) N5 0.050(4) 0.041(3) 0.035(3) -0.001(3) -0.003(4) -0.008(4) C6 0.038(4) 0.044(5) 0.051(5) -0.016(4) -0.004(4) 0.000(3) C7 0.048(5) 0.057(6) 0.079(7) -0.022(5) -0.011(5) 0.003(4) C8 0.070(7) 0.071(7) 0.075(8) -0.033(6) -0.028(7) 0.016(6) C9 0.099(10) 0.046(6) 0.104(10) -0.031(6) -0.062(8) 0.030(6) C10 0.094(8) 0.034(5) 0.075(8) -0.004(5) -0.041(7) 0.013(5) C11 0.064(6) 0.038(5) 0.055(6) -0.013(4) -0.020(5) 0.001(4) N12 0.066(5) 0.036(4) 0.043(4) 0.004(3) -0.008(4) -0.005(4) C13 0.053(5) 0.030(4) 0.038(5) 0.003(3) -0.010(4) -0.001(3) C14 0.062(5) 0.045(5) 0.028(4) -0.011(4) -0.002(4) 0.000(4) C15 0.057(7) 0.040(4) 0.044(5) 0.003(4) 0.006(4) 0.002(4) C16 0.076(7) 0.063(6) 0.043(5) 0.002(4) 0.007(6) 0.001(6) C17 0.117(11) 0.058(7) 0.039(6) 0.000(5) 0.002(6) 0.017(7) C18 0.059(6) 0.063(6) 0.048(5) -0.014(5) -0.012(4) 0.022(5) C19 0.056(5) 0.056(5) 0.045(5) -0.012(4) -0.002(5) -0.001(6) F20 0.094(6) 0.079(5) 0.107(6) -0.001(4) 0.021(4) -0.007(4) F21 0.144(7) 0.075(5) 0.101(6) 0.005(5) 0.027(6) -0.033(5) F22 0.147(7) 0.059(4) 0.055(4) 0.012(3) 0.005(4) 0.036(5) F23 0.122(7) 0.089(5) 0.082(5) 0.001(4) -0.022(5) 0.018(5) F24 0.080(5) 0.074(4) 0.099(6) 0.008(4) 0.005(4) 0.000(4) C25 0.054(6) 0.048(5) 0.038(5) -0.004(4) 0.002(4) 0.001(4) C26 0.035(5) 0.085(7) 0.059(6) -0.015(6) -0.004(4) 0.001(5) C27 0.056(6) 0.091(8) 0.047(6) 0.006(6) 0.001(5) 0.032(5) C28 0.065(7) 0.083(8) 0.037(5) -0.007(5) 0.007(5) 0.035(6) C29 0.062(6) 0.056(5) 0.047(5) -0.015(4) -0.008(5) 0.010(5) C30 0.057(6) 0.053(5) 0.041(5) -0.018(4) -0.003(4) 0.000(4) F31 0.111(5) 0.104(6) 0.045(4) -0.022(4) 0.000(4) 0.042(5) C32 0.093(7) 0.040(5) 0.051(6) 0.005(5) 0.007(5) -0.003(5) C33 0.062(6) 0.041(5) 0.037(5) -0.013(4) -0.016(4) 0.004(4) C34 0.092(8) 0.066(7) 0.043(6) -0.018(5) -0.019(6) 0.001(6) C35 0.127(11) 0.056(6) 0.094(9) -0.020(6) -0.066(9) 0.030(8) C36 0.081(8) 0.102(9) 0.068(7) -0.019(7) 0.001(8) -0.026(9) C37 0.075(7) 0.083(7) 0.050(6) 0.016(5) 0.012(6) -0.017(7) C38 0.074(8) 0.074(8) 0.064(7) 0.005(6) -0.013(6) -0.002(6) C39 0.136(13) 0.072(8) 0.089(10) -0.032(7) -0.033(9) 0.020(9) C40 0.111(12) 0.094(11) 0.109(12) -0.001(9) -0.064(10) 0.025(9) C41 0.077(9) 0.21(2) 0.143(15) 0.083(15) -0.053(10) -0.083(11) _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 C14 2.082(9) . ? Pt1 C25 2.086(9) . ? Pt1 P3 2.281(2) . ? Pt1 P2 2.282(3) . ? P2 C37 1.769(10) . ? P2 C13 1.835(9) . ? P2 C38 1.860(12) . ? P3 C32 1.784(10) . ? P3 C4 1.825(9) . ? P3 C33 1.874(9) . ? C4 N5 1.312(11) . ? C4 C13 1.429(12) . ? N5 C6 1.355(11) . ? C6 C7 1.398(14) . ? C6 C11 1.428(14) . ? C7 C8 1.381(14) . ? C7 H7 0.9500 . ? C8 C9 1.413(19) . ? C8 H8 0.9500 . ? C9 C10 1.335(18) . ? C9 H9 0.9500 . ? C10 C11 1.437(13) . ? C10 H10 0.9500 . ? C11 N12 1.361(13) . ? N12 C13 1.340(10) . ? C14 C15 1.367(13) . ? C14 C19 1.388(15) . ? C15 C16 1.372(14) . ? C15 F20 1.381(12) . ? C16 C17 1.362(18) . ? C16 F21 1.445(15) . ? C17 C18 1.330(16) . ? C17 F22 1.373(13) . ? C18 F23 1.357(12) . ? C18 C19 1.372(14) . ? C19 F24 1.287(12) . ? C25 C30 1.382(13) . ? C25 C26 1.395(14) . ? C26 C27 1.454(14) . ? C26 H26 0.9500 . ? C27 C28 1.374(17) . ? C27 H27 0.9500 . ? C28 F31 1.350(11) . ? C28 C29 1.365(16) . ? C29 C30 1.399(12) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.483(16) . ? C33 C35 1.513(14) . ? C33 C34 1.534(13) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.458(18) . ? C38 C40 1.511(18) . ? C38 C41 1.536(19) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? 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 C14 Pt1 C25 85.9(3) . . ? C14 Pt1 P3 93.5(2) . . ? C25 Pt1 P3 178.9(3) . . ? C14 Pt1 P2 174.3(3) . . ? C25 Pt1 P2 93.2(3) . . ? P3 Pt1 P2 87.47(8) . . ? C37 P2 C13 103.3(5) . . ? C37 P2 C38 106.4(6) . . ? C13 P2 C38 103.2(5) . . ? C37 P2 Pt1 122.1(5) . . ? C13 P2 Pt1 107.3(3) . . ? C38 P2 Pt1 112.6(4) . . ? C32 P3 C4 102.9(5) . . ? C32 P3 C33 106.1(5) . . ? C4 P3 C33 102.9(4) . . ? C32 P3 Pt1 119.4(4) . . ? C4 P3 Pt1 108.1(3) . . ? C33 P3 Pt1 115.5(3) . . ? N5 C4 C13 121.9(8) . . ? N5 C4 P3 121.4(7) . . ? C13 C4 P3 116.7(7) . . ? C4 N5 C6 117.9(7) . . ? N5 C6 C7 120.0(9) . . ? N5 C6 C11 119.8(8) . . ? C7 C6 C11 120.1(9) . . ? C8 C7 C6 118.5(11) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C9 120.8(11) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 122.8(10) . . ? C10 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C9 C10 C11 117.9(12) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? N12 C11 C6 122.3(8) . . ? N12 C11 C10 117.9(10) . . ? C6 C11 C10 119.7(10) . . ? C13 N12 C11 115.7(8) . . ? N12 C13 C4 121.5(8) . . ? N12 C13 P2 119.8(6) . . ? C4 C13 P2 118.4(6) . . ? C15 C14 C19 113.4(9) . . ? C15 C14 Pt1 122.3(7) . . ? C19 C14 Pt1 124.3(7) . . ? C14 C15 C16 125.0(10) . . ? C14 C15 F20 119.9(8) . . ? C16 C15 F20 115.1(9) . . ? C17 C16 C15 118.7(11) . . ? C17 C16 F21 120.7(11) . . ? C15 C16 F21 120.2(11) . . ? C18 C17 C16 118.8(11) . . ? C18 C17 F22 121.0(12) . . ? C16 C17 F22 120.0(12) . . ? C17 C18 F23 115.2(11) . . ? C17 C18 C19 121.6(10) . . ? F23 C18 C19 123.1(11) . . ? F24 C19 C18 115.7(10) . . ? F24 C19 C14 121.9(9) . . ? C18 C19 C14 122.3(10) . . ? C30 C25 C26 118.4(9) . . ? C30 C25 Pt1 120.2(7) . . ? C26 C25 Pt1 121.3(7) . . ? C25 C26 C27 120.3(11) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 117.5(11) . . ? C28 C27 H27 121.3 . . ? C26 C27 H27 121.3 . . ? F31 C28 C29 119.4(11) . . ? F31 C28 C27 117.8(11) . . ? C29 C28 C27 122.8(9) . . ? C28 C29 C30 118.9(10) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C25 C30 C29 122.0(10) . . ? C25 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? P3 C32 H32A 109.5 . . ? P3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 109.3(11) . . ? C36 C33 C34 109.8(9) . . ? C35 C33 C34 109.1(9) . . ? C36 C33 P3 105.9(7) . . ? C35 C33 P3 109.0(7) . . ? C34 C33 P3 113.7(7) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P2 C37 H37A 109.5 . . ? P2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C40 104.3(11) . . ? C39 C38 C41 117.1(13) . . ? C40 C38 C41 108.5(13) . . ? C39 C38 P2 107.3(10) . . ? C40 C38 P2 113.1(9) . . ? C41 C38 P2 106.8(8) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 2.064 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.151