# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_1 _database_code_depnum_ccdc_archive 'CCDC 919435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 F3 N O2 Pt S' _chemical_formula_weight 548.44 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' O O 0.0492 0.0322 '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' S S 0.3331 0.5567 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 4.67050(10) _cell_length_b 13.9784(3) _cell_length_c 12.7548(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.458(2) _cell_angle_gamma 90.00 _cell_volume 830.19(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6081 _cell_measurement_theta_min 3.1589 _cell_measurement_theta_max 73.4737 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 17.389 _exptl_absorpt_correction_T_min 0.12168 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_detector_area_resol_mean 10.5357 _diffrn_measurement_method '/w scan' _diffrn_reflns_number 8410 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 73.63 _reflns_number_total 2974 _reflns_number_gt 2800 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_cell_refinement 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_data_reduction 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Stereochemical Workstation (Siemens, 1989)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0547P)^2^+1.4492P] 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 0.05(2) _refine_ls_number_reflns 2974 _refine_ls_number_parameters 228 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 0.19257(6) 0.85329(5) 0.19805(2) 0.04301(12) Uani 1 1 d . . . S1 S 0.4803(6) 0.72577(18) 0.17607(19) 0.0503(5) Uani 1 1 d . . . C2 C 0.286(3) 0.6250(10) 0.2194(11) 0.074(3) Uani 1 1 d . . . H2A H 0.0988 0.6231 0.1823 0.111 Uiso 1 1 calc R . . H2B H 0.2654 0.6304 0.2935 0.111 Uiso 1 1 calc R . . H2C H 0.3878 0.5673 0.2057 0.111 Uiso 1 1 calc R . . C3 C 0.478(3) 0.6947(10) 0.0403(10) 0.073(3) Uani 1 1 d . . . H3A H 0.6061 0.6420 0.0322 0.110 Uiso 1 1 calc R . . H3B H 0.5395 0.7486 0.0012 0.110 Uiso 1 1 calc R . . H3C H 0.2870 0.6768 0.0143 0.110 Uiso 1 1 calc R . . O4 O 0.0238(14) 0.8467(14) 0.0397(4) 0.054(2) Uani 1 1 d . . . C5 C 0.094(2) 0.9037(8) -0.0309(8) 0.053(2) Uani 1 1 d . . . O6 O 0.217(3) 0.9810(8) -0.0219(8) 0.092(3) Uani 1 1 d . . . C7 C -0.022(3) 0.8725(10) -0.1429(8) 0.060(4) Uani 1 1 d . . . F8 F 0.055(3) 0.7853(7) -0.1626(8) 0.125(5) Uani 1 1 d . . . F9 F -0.3022(17) 0.8784(10) -0.1559(6) 0.099(5) Uani 1 1 d . . . F10 F 0.070(2) 0.9281(8) -0.2172(7) 0.094(3) Uani 1 1 d . . . C11 C 0.3355(17) 0.8653(15) 0.3471(6) 0.043(3) Uani 1 1 d . . . C12 C 0.541(3) 0.8148(9) 0.4082(8) 0.059(3) Uani 1 1 d . . . H12 H 0.6331 0.7632 0.3796 0.070 Uiso 1 1 calc R . . C13 C 0.612(2) 0.8413(15) 0.5145(8) 0.061(4) Uani 1 1 d . . . H13 H 0.7525 0.8061 0.5532 0.074 Uiso 1 1 calc R . . C14 C 0.489(2) 0.9138(8) 0.5621(8) 0.056(3) Uani 1 1 d . . . H14 H 0.5391 0.9272 0.6326 0.067 Uiso 1 1 calc R . . C15 C 0.281(2) 0.9701(8) 0.5029(8) 0.053(2) Uani 1 1 d . . . C16 C 0.144(3) 1.0529(10) 0.5430(8) 0.062(3) Uani 1 1 d . . . H16 H 0.1926 1.0708 0.6123 0.074 Uiso 1 1 calc R . . C17 C -0.054(3) 1.1067(14) 0.4852(10) 0.064(4) Uani 1 1 d . . . H17 H -0.1348 1.1608 0.5135 0.077 Uiso 1 1 calc R . . C18 C -0.136(3) 1.0768(8) 0.3773(9) 0.055(2) Uani 1 1 d . . . C19 C -0.351(2) 1.1235(8) 0.3101(9) 0.057(2) Uani 1 1 d . . . H19 H -0.4488 1.1765 0.3332 0.068 Uiso 1 1 calc R . . C20 C -0.408(3) 1.0887(9) 0.2122(9) 0.061(3) Uani 1 1 d . . . H20 H -0.5498 1.1179 0.1679 0.073 Uiso 1 1 calc R . . C21 C -0.261(2) 1.0098(8) 0.1749(8) 0.051(2) Uani 1 1 d . . . H21 H -0.3073 0.9867 0.1073 0.061 Uiso 1 1 calc R . . N22 N -0.0556(16) 0.9682(6) 0.2362(6) 0.0449(17) Uani 1 1 d . . . C23 C 0.001(2) 0.9992(7) 0.3369(7) 0.0437(19) Uani 1 1 d . . . C24 C 0.211(2) 0.9435(8) 0.3981(7) 0.044(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.05260(19) 0.04140(19) 0.03444(16) -0.0006(3) -0.00039(11) -0.0029(3) S1 0.0579(13) 0.0438(12) 0.0484(11) -0.0022(10) -0.0005(9) 0.0027(10) C2 0.088(8) 0.058(7) 0.074(8) 0.017(6) -0.006(7) -0.001(6) C3 0.096(9) 0.065(8) 0.059(6) -0.013(6) 0.005(6) 0.008(7) O4 0.073(3) 0.055(6) 0.031(2) -0.009(5) -0.008(2) 0.001(6) C5 0.061(6) 0.052(6) 0.048(5) 0.006(4) 0.006(4) 0.008(5) O6 0.138(9) 0.067(6) 0.067(5) 0.010(4) -0.009(6) -0.030(6) C7 0.074(6) 0.064(12) 0.041(4) 0.008(5) -0.001(4) 0.016(6) F8 0.223(14) 0.085(6) 0.061(5) -0.024(5) -0.027(7) 0.057(8) F9 0.077(4) 0.156(14) 0.061(4) 0.006(5) -0.010(3) 0.011(6) F10 0.118(7) 0.114(7) 0.050(4) 0.011(4) 0.012(5) 0.005(5) C11 0.042(3) 0.052(9) 0.033(3) -0.008(5) -0.004(3) -0.017(5) C12 0.075(7) 0.061(6) 0.039(4) 0.001(4) 0.002(5) -0.015(5) C13 0.059(5) 0.071(12) 0.053(5) 0.010(7) -0.004(4) 0.001(7) C14 0.065(6) 0.061(7) 0.038(4) -0.005(4) -0.013(4) -0.009(5) C15 0.052(5) 0.066(7) 0.041(5) 0.001(4) 0.005(4) -0.011(5) C16 0.075(7) 0.071(8) 0.038(5) -0.012(5) 0.005(5) -0.021(6) C17 0.080(12) 0.066(7) 0.049(8) 0.000(6) 0.017(7) 0.007(8) C18 0.064(6) 0.048(6) 0.055(6) 0.000(4) 0.018(5) -0.011(4) C19 0.062(6) 0.052(6) 0.057(6) 0.005(4) 0.018(5) 0.005(5) C20 0.069(6) 0.056(7) 0.057(6) 0.007(5) 0.005(5) 0.000(5) C21 0.061(6) 0.053(6) 0.038(4) 0.004(4) 0.000(4) -0.003(4) N22 0.047(4) 0.044(4) 0.043(4) -0.001(3) -0.002(3) -0.003(3) C23 0.051(5) 0.041(5) 0.039(4) -0.005(3) 0.006(3) -0.014(4) C24 0.047(4) 0.055(5) 0.031(4) -0.005(4) 0.003(3) -0.013(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 1.972(8) . ? Pt1 N22 2.062(8) . ? Pt1 O4 2.113(5) . ? Pt1 S1 2.263(3) . ? S1 C3 1.785(12) . ? S1 C2 1.788(14) . ? O4 C5 1.265(17) . ? C5 O6 1.223(15) . ? C5 C7 1.551(15) . ? C7 F8 1.300(16) . ? C7 F9 1.309(14) . ? C7 F10 1.323(15) . ? C11 C12 1.382(18) . ? C11 C24 1.42(2) . ? C12 C13 1.420(14) . ? C13 C14 1.33(2) . ? C14 C15 1.424(16) . ? C15 C24 1.401(13) . ? C15 C16 1.436(17) . ? C16 C17 1.36(2) . ? C17 C18 1.461(18) . ? C18 C23 1.379(15) . ? C18 C19 1.425(17) . ? C19 C20 1.348(16) . ? C20 C21 1.403(17) . ? C21 N22 1.324(13) . ? N22 C23 1.360(11) . ? C23 C24 1.436(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pt1 N22 82.0(6) . . ? C11 Pt1 O4 176.8(8) . . ? N22 Pt1 O4 94.9(5) . . ? C11 Pt1 S1 91.5(5) . . ? N22 Pt1 S1 173.4(2) . . ? O4 Pt1 S1 91.6(4) . . ? C3 S1 C2 98.2(7) . . ? C3 S1 Pt1 110.7(5) . . ? C2 S1 Pt1 105.1(5) . . ? C5 O4 Pt1 123.7(10) . . ? O6 C5 O4 129.4(12) . . ? O6 C5 C7 117.6(10) . . ? O4 C5 C7 112.7(11) . . ? F8 C7 F9 108.9(13) . . ? F8 C7 F10 107.6(11) . . ? F9 C7 F10 104.5(10) . . ? F8 C7 C5 111.0(10) . . ? F9 C7 C5 111.9(9) . . ? F10 C7 C5 112.6(11) . . ? C12 C11 C24 115.2(9) . . ? C12 C11 Pt1 132.0(12) . . ? C24 C11 Pt1 112.8(9) . . ? C11 C12 C13 120.4(13) . . ? C14 C13 C12 123.8(13) . . ? C13 C14 C15 118.7(9) . . ? C24 C15 C14 117.2(10) . . ? C24 C15 C16 118.5(10) . . ? C14 C15 C16 124.3(9) . . ? C17 C16 C15 123.7(11) . . ? C16 C17 C18 117.9(14) . . ? C23 C18 C19 117.4(10) . . ? C23 C18 C17 118.8(12) . . ? C19 C18 C17 123.7(11) . . ? C20 C19 C18 118.1(10) . . ? C19 C20 C21 122.1(11) . . ? N22 C21 C20 119.8(9) . . ? C21 N22 C23 119.8(9) . . ? C21 N22 Pt1 126.6(7) . . ? C23 N22 Pt1 113.6(6) . . ? N22 C23 C18 122.8(10) . . ? N22 C23 C24 114.5(8) . . ? C18 C23 C24 122.8(9) . . ? C15 C24 C11 124.7(10) . . ? C15 C24 C23 118.2(9) . . ? C11 C24 C23 117.1(8) . . ? 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 C11 Pt1 S1 C3 -170.6(7) . . . . ? O4 Pt1 S1 C3 9.6(6) . . . . ? C11 Pt1 S1 C2 84.3(6) . . . . ? O4 Pt1 S1 C2 -95.5(6) . . . . ? N22 Pt1 O4 C5 76.9(11) . . . . ? Pt1 O4 C5 C7 170.3(8) . . . . ? O6 C5 C7 F8 131.1(14) . . . . ? O4 C5 C7 F8 -54.4(15) . . . . ? O6 C5 C7 F9 -106.9(14) . . . . ? O4 C5 C7 F9 67.5(15) . . . . ? O6 C5 C7 F10 10.4(16) . . . . ? O4 C5 C7 F10 -175.1(11) . . . . ? N22 Pt1 C11 C12 -178.9(14) . . . . ? S1 Pt1 C11 C12 2.1(13) . . . . ? N22 Pt1 C11 C24 -2.3(8) . . . . ? S1 Pt1 C11 C24 178.7(8) . . . . ? C24 C11 C12 C13 0.8(17) . . . . ? Pt1 C11 C12 C13 177.4(11) . . . . ? C11 C12 C13 C14 1(2) . . . . ? C12 C13 C14 C15 -2(2) . . . . ? C13 C14 C15 C24 1.8(16) . . . . ? C13 C14 C15 C16 -176.6(12) . . . . ? C24 C15 C16 C17 1.0(18) . . . . ? C14 C15 C16 C17 179.4(13) . . . . ? C15 C16 C17 C18 2(2) . . . . ? C16 C17 C18 C23 -3.6(19) . . . . ? C16 C17 C18 C19 176.6(12) . . . . ? C23 C18 C19 C20 0.5(15) . . . . ? C17 C18 C19 C20 -179.7(12) . . . . ? C18 C19 C20 C21 -0.9(17) . . . . ? C19 C20 C21 N22 -1.1(17) . . . . ? C20 C21 N22 C23 3.5(15) . . . . ? C20 C21 N22 Pt1 -179.1(8) . . . . ? C11 Pt1 N22 C21 -174.8(9) . . . . ? O4 Pt1 N22 C21 5.1(9) . . . . ? S1 Pt1 N22 C21 -166.2(15) . . . . ? C11 Pt1 N22 C23 2.8(7) . . . . ? O4 Pt1 N22 C23 -177.3(7) . . . . ? C21 N22 C23 C18 -4.0(14) . . . . ? Pt1 N22 C23 C18 178.2(7) . . . . ? C21 N22 C23 C24 175.1(8) . . . . ? Pt1 N22 C23 C24 -2.7(9) . . . . ? C19 C18 C23 N22 1.9(14) . . . . ? C17 C18 C23 N22 -177.9(11) . . . . ? C19 C18 C23 C24 -177.1(9) . . . . ? C17 C18 C23 C24 3.1(16) . . . . ? C14 C15 C24 C11 -0.5(15) . . . . ? C16 C15 C24 C11 178.1(10) . . . . ? C14 C15 C24 C23 179.9(9) . . . . ? C16 C15 C24 C23 -1.6(14) . . . . ? C12 C11 C24 C15 -0.8(16) . . . . ? Pt1 C11 C24 C15 -178.0(8) . . . . ? C12 C11 C24 C23 178.8(10) . . . . ? Pt1 C11 C24 C23 1.6(12) . . . . ? N22 C23 C24 C15 -179.6(8) . . . . ? C18 C23 C24 C15 -0.5(14) . . . . ? N22 C23 C24 C11 0.7(12) . . . . ? C18 C23 C24 C11 179.9(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C3 H3A O6 0.96 2.40 3.326(17) 160.8 2_645 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.963 _refine_diff_density_min -1.478 _refine_diff_density_rms 0.125 ####################################################################### # # 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 _database_code_depnum_ccdc_archive 'CCDC 919436' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H32 N P2 Pt, C2 F3 O2' _chemical_formula_sum 'C41 H32 F3 N O2 P2 Pt' _chemical_formula_weight 884.71 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 11.6274(2) _cell_length_b 13.9851(2) _cell_length_c 21.7088(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.0050(10) _cell_angle_gamma 90.00 _cell_volume 3527.91(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12824 _cell_measurement_theta_min 2.9024 _cell_measurement_theta_max 28.1691 _exptl_crystal_description plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 4.121 _exptl_absorpt_correction_T_min 0.43315 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1544 _diffrn_measurement_method '/w scan' _diffrn_reflns_number 34752 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 28.24 _reflns_number_total 7775 _reflns_number_gt 6306 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_cell_refinement 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_data_reduction 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Stereochemical Workstation (Siemens, 1989)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0184P)^2^+4.5295P] 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 7775 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 Pt1 Pt 0.922625(9) 0.253887(9) 0.175004(5) 0.02871(4) Uani 1 1 d . . . P1 P 0.74353(7) 0.22002(6) 0.13827(4) 0.03150(18) Uani 1 1 d . . . P2 P 0.84279(7) 0.23871(6) 0.27096(4) 0.03295(19) Uani 1 1 d . . . C1 C 0.7163(3) 0.0973(2) 0.11581(16) 0.0391(8) Uani 1 1 d . . . C2 C 0.6077(4) 0.0573(3) 0.1160(2) 0.0614(12) Uani 1 1 d . . . H2 H 0.5465 0.0923 0.1308 0.074 Uiso 1 1 calc R . . C3 C 0.5898(5) -0.0345(4) 0.0943(3) 0.0787(15) Uani 1 1 d . . . H3 H 0.5167 -0.0613 0.0954 0.094 Uiso 1 1 calc R . . C4 C 0.6769(5) -0.0859(3) 0.0715(2) 0.0760(15) Uani 1 1 d . . . H4 H 0.6633 -0.1471 0.0561 0.091 Uiso 1 1 calc R . . C5 C 0.7852(5) -0.0479(3) 0.0711(2) 0.0705(14) Uani 1 1 d . . . H5 H 0.8452 -0.0832 0.0553 0.085 Uiso 1 1 calc R . . C6 C 0.8055(4) 0.0425(3) 0.09407(19) 0.0526(10) Uani 1 1 d . . . H6 H 0.8799 0.0671 0.0950 0.063 Uiso 1 1 calc R . . C7 C 0.6878(3) 0.2917(3) 0.07408(16) 0.0355(7) Uani 1 1 d . . . C8 C 0.7015(3) 0.3898(3) 0.07813(19) 0.0479(9) Uani 1 1 d . . . H8 H 0.7402 0.4161 0.1123 0.058 Uiso 1 1 calc R . . C9 C 0.6587(4) 0.4485(3) 0.0325(2) 0.0630(12) Uani 1 1 d . . . H9 H 0.6669 0.5145 0.0359 0.076 Uiso 1 1 calc R . . C10 C 0.6034(4) 0.4094(4) -0.0185(2) 0.0641(13) Uani 1 1 d . . . H10 H 0.5754 0.4490 -0.0500 0.077 Uiso 1 1 calc R . . C11 C 0.5891(3) 0.3124(4) -0.02343(18) 0.0570(11) Uani 1 1 d . . . H11 H 0.5512 0.2865 -0.0580 0.068 Uiso 1 1 calc R . . C12 C 0.6310(3) 0.2534(3) 0.02301(16) 0.0450(9) Uani 1 1 d . . . H12 H 0.6209 0.1876 0.0199 0.054 Uiso 1 1 calc R . . C13 C 0.6455(3) 0.2474(3) 0.20000(16) 0.0416(8) Uani 1 1 d . . . H13A H 0.6401 0.3161 0.2056 0.050 Uiso 1 1 calc R . . H13B H 0.5692 0.2229 0.1897 0.050 Uiso 1 1 calc R . . C14 C 0.6930(3) 0.2007(3) 0.25849(16) 0.0409(8) Uani 1 1 d . . . H14A H 0.6891 0.1317 0.2546 0.049 Uiso 1 1 calc R . . H14B H 0.6479 0.2197 0.2932 0.049 Uiso 1 1 calc R . . C15 C 0.9016(3) 0.1482(2) 0.32344(15) 0.0351(8) Uani 1 1 d . . . C16 C 0.8328(3) 0.1037(3) 0.36593(18) 0.0482(9) Uani 1 1 d . . . H16 H 0.7549 0.1183 0.3668 0.058 Uiso 1 1 calc R . . C17 C 0.8804(4) 0.0377(3) 0.4072(2) 0.0548(11) Uani 1 1 d . . . H17 H 0.8339 0.0088 0.4358 0.066 Uiso 1 1 calc R . . C18 C 0.9940(4) 0.0145(3) 0.40631(18) 0.0511(10) Uani 1 1 d . . . H18 H 1.0249 -0.0299 0.4341 0.061 Uiso 1 1 calc R . . C19 C 1.0624(4) 0.0573(3) 0.36408(19) 0.0542(10) Uani 1 1 d . . . H19 H 1.1403 0.0423 0.3635 0.065 Uiso 1 1 calc R . . C20 C 1.0158(3) 0.1227(3) 0.32235(17) 0.0446(9) Uani 1 1 d . . . H20 H 1.0624 0.1499 0.2931 0.054 Uiso 1 1 calc R . . C21 C 0.8340(3) 0.3481(2) 0.31619(16) 0.0372(8) Uani 1 1 d . . . C22 C 0.7838(4) 0.3485(3) 0.3732(2) 0.0628(13) Uani 1 1 d . . . H22 H 0.7528 0.2924 0.3885 0.075 Uiso 1 1 calc R . . C23 C 0.7793(5) 0.4318(3) 0.4078(2) 0.0776(16) Uani 1 1 d . . . H23 H 0.7439 0.4316 0.4455 0.093 Uiso 1 1 calc R . . C24 C 0.8269(5) 0.5138(3) 0.3863(2) 0.0737(14) Uani 1 1 d . . . H24 H 0.8254 0.5693 0.4100 0.088 Uiso 1 1 calc R . . C25 C 0.8764(5) 0.5150(3) 0.3305(2) 0.0708(14) Uani 1 1 d . . . H25 H 0.9076 0.5715 0.3159 0.085 Uiso 1 1 calc R . . C26 C 0.8807(4) 0.4324(3) 0.29548(18) 0.0497(10) Uani 1 1 d . . . H26 H 0.9154 0.4339 0.2575 0.060 Uiso 1 1 calc R . . N27 N 1.0895(2) 0.2980(2) 0.20268(13) 0.0371(6) Uani 1 1 d . . . C28 C 1.1315(3) 0.3228(3) 0.25933(18) 0.0492(10) Uani 1 1 d . . . H28 H 1.0827 0.3208 0.2923 0.059 Uiso 1 1 calc R . . C29 C 1.2445(4) 0.3511(4) 0.2699(2) 0.0648(13) Uani 1 1 d . . . H29 H 1.2707 0.3674 0.3094 0.078 Uiso 1 1 calc R . . C30 C 1.3185(4) 0.3549(3) 0.2214(2) 0.0628(12) Uani 1 1 d . . . H30 H 1.3950 0.3723 0.2285 0.075 Uiso 1 1 calc R . . C31 C 1.2787(3) 0.3329(3) 0.16259(19) 0.0460(9) Uani 1 1 d . . . C32 C 1.3469(3) 0.3370(3) 0.1091(2) 0.0567(11) Uani 1 1 d . . . H32 H 1.4242 0.3537 0.1136 0.068 Uiso 1 1 calc R . . C33 C 1.3025(3) 0.3174(3) 0.0529(2) 0.0523(11) Uani 1 1 d . . . H33 H 1.3498 0.3204 0.0193 0.063 Uiso 1 1 calc R . . C34 C 1.1838(3) 0.2918(3) 0.04299(17) 0.0395(8) Uani 1 1 d . . . C35 C 1.1330(3) 0.2758(3) -0.01531(18) 0.0479(10) Uani 1 1 d . . . H35 H 1.1764 0.2818 -0.0503 0.057 Uiso 1 1 calc R . . C36 C 1.0201(3) 0.2514(3) -0.02079(17) 0.0473(9) Uani 1 1 d . . . H36 H 0.9868 0.2403 -0.0597 0.057 Uiso 1 1 calc R . . C37 C 0.9526(3) 0.2427(3) 0.03141(16) 0.0400(8) Uani 1 1 d . . . H37 H 0.8757 0.2251 0.0264 0.048 Uiso 1 1 calc R . . C38 C 0.9980(3) 0.2595(2) 0.08973(14) 0.0284(6) Uani 1 1 d . . . C39 C 1.1147(3) 0.2841(2) 0.09480(16) 0.0333(7) Uani 1 1 d . . . C40 C 1.1626(3) 0.3048(2) 0.15442(16) 0.0361(8) Uani 1 1 d . . . C1A C 0.3989(5) 0.4077(4) 0.7955(2) 0.0725(14) Uani 1 1 d . . . F1A F 0.4901(5) 0.4649(3) 0.8076(3) 0.187(2) Uani 1 1 d . . . F2A F 0.3165(4) 0.4668(3) 0.79405(18) 0.152(2) Uani 1 1 d . . . F3A F 0.4205(4) 0.3810(3) 0.74050(15) 0.1411(18) Uani 1 1 d . . . C2A C 0.3991(4) 0.3294(3) 0.84423(19) 0.0530(10) Uani 1 1 d . . . O1A O 0.4722(3) 0.2672(2) 0.83822(15) 0.0685(9) Uani 1 1 d . . . O2A O 0.3286(3) 0.3393(3) 0.88376(16) 0.0882(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02326(6) 0.03605(7) 0.02695(7) 0.00019(6) 0.00269(4) -0.00111(5) P1 0.0271(4) 0.0341(4) 0.0332(4) -0.0016(4) 0.0008(3) -0.0007(3) P2 0.0290(4) 0.0414(5) 0.0287(4) -0.0002(4) 0.0044(3) -0.0021(4) C1 0.044(2) 0.0360(18) 0.037(2) 0.0017(16) -0.0029(16) -0.0051(16) C2 0.047(2) 0.052(2) 0.085(3) -0.007(2) -0.004(2) -0.008(2) C3 0.067(3) 0.060(3) 0.107(4) -0.005(3) -0.018(3) -0.025(3) C4 0.112(5) 0.041(2) 0.074(3) -0.008(2) -0.005(3) -0.015(3) C5 0.097(4) 0.043(2) 0.073(3) -0.009(2) 0.017(3) 0.005(3) C6 0.063(3) 0.041(2) 0.054(3) 0.0015(19) 0.009(2) -0.0007(19) C7 0.0285(17) 0.0413(18) 0.0368(19) -0.0015(16) 0.0038(14) 0.0057(14) C8 0.047(2) 0.047(2) 0.050(2) 0.0018(19) -0.0001(18) -0.0008(18) C9 0.066(3) 0.049(2) 0.075(3) 0.015(2) 0.009(3) 0.013(2) C10 0.050(3) 0.086(4) 0.056(3) 0.030(3) 0.008(2) 0.028(2) C11 0.044(2) 0.088(3) 0.038(2) 0.000(2) -0.0048(18) 0.013(2) C12 0.042(2) 0.052(2) 0.0398(19) -0.0041(19) -0.0045(16) 0.0045(18) C13 0.0276(16) 0.055(2) 0.0423(19) -0.0049(18) 0.0051(14) -0.0006(17) C14 0.0314(18) 0.054(2) 0.038(2) 0.0014(17) 0.0091(15) -0.0064(16) C15 0.043(2) 0.0358(18) 0.0269(17) -0.0023(14) 0.0023(15) -0.0017(15) C16 0.043(2) 0.051(2) 0.051(2) 0.0116(19) 0.0101(18) -0.0024(18) C17 0.061(3) 0.047(2) 0.057(3) 0.016(2) 0.013(2) -0.008(2) C18 0.067(3) 0.037(2) 0.049(2) 0.0103(18) -0.003(2) 0.0031(19) C19 0.053(2) 0.053(2) 0.058(3) 0.007(2) 0.008(2) 0.013(2) C20 0.045(2) 0.051(2) 0.039(2) 0.0065(17) 0.0107(17) 0.0049(18) C21 0.041(2) 0.0364(18) 0.0343(19) 0.0000(15) 0.0026(16) 0.0045(15) C22 0.093(4) 0.045(2) 0.052(3) -0.002(2) 0.027(2) -0.009(2) C23 0.117(5) 0.060(3) 0.058(3) -0.016(2) 0.035(3) -0.003(3) C24 0.110(4) 0.048(3) 0.063(3) -0.016(2) 0.006(3) 0.001(3) C25 0.102(4) 0.040(2) 0.070(3) -0.003(2) 0.014(3) -0.012(2) C26 0.064(3) 0.047(2) 0.039(2) 0.0004(18) 0.0087(19) -0.0053(19) N27 0.0331(15) 0.0374(16) 0.0409(17) 0.0007(13) 0.0002(13) -0.0005(13) C28 0.039(2) 0.066(3) 0.042(2) -0.001(2) -0.0011(17) -0.0083(19) C29 0.048(3) 0.088(3) 0.057(3) -0.007(2) -0.015(2) -0.012(2) C30 0.032(2) 0.078(3) 0.077(3) 0.003(3) -0.009(2) -0.009(2) C31 0.0286(18) 0.048(2) 0.061(3) 0.0077(19) -0.0017(18) -0.0014(16) C32 0.0248(19) 0.059(3) 0.087(3) 0.016(2) 0.013(2) -0.0029(17) C33 0.036(2) 0.055(2) 0.068(3) 0.014(2) 0.024(2) 0.0045(18) C34 0.0363(19) 0.0358(18) 0.047(2) 0.0088(17) 0.0154(16) 0.0060(15) C35 0.051(2) 0.051(2) 0.043(2) 0.0103(18) 0.0234(18) 0.0094(18) C36 0.051(2) 0.059(2) 0.0316(18) 0.0018(18) 0.0060(16) 0.005(2) C37 0.0364(18) 0.048(2) 0.0356(18) 0.0035(17) 0.0061(14) 0.0039(16) C38 0.0257(15) 0.0311(16) 0.0287(15) 0.0022(13) 0.0052(12) 0.0048(13) C39 0.0317(17) 0.0304(16) 0.0385(19) 0.0075(15) 0.0093(15) 0.0066(14) C40 0.0308(18) 0.0347(18) 0.043(2) 0.0057(16) 0.0035(15) -0.0011(14) C1A 0.069(3) 0.077(3) 0.074(3) 0.010(3) 0.036(3) 0.022(3) F1A 0.192(5) 0.120(4) 0.251(6) 0.056(4) 0.019(4) -0.065(4) F2A 0.157(4) 0.187(4) 0.118(3) 0.062(3) 0.066(3) 0.115(3) F3A 0.221(5) 0.146(3) 0.059(2) 0.031(2) 0.058(3) 0.084(3) C2A 0.041(2) 0.072(3) 0.046(2) -0.005(2) 0.0027(19) -0.005(2) O1A 0.0569(19) 0.078(2) 0.071(2) 0.0092(17) 0.0087(16) 0.0073(17) O2A 0.078(2) 0.112(3) 0.077(2) 0.008(2) 0.042(2) 0.012(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C38 2.077(3) . ? Pt1 N27 2.103(3) . ? Pt1 P1 2.2540(8) . ? Pt1 P2 2.3197(8) . ? P1 C1 1.809(4) . ? P1 C7 1.818(4) . ? P1 C13 1.830(3) . ? P2 C15 1.820(3) . ? P2 C21 1.822(4) . ? P2 C14 1.832(3) . ? C1 C2 1.381(5) . ? C1 C6 1.386(5) . ? C2 C3 1.381(6) . ? C2 H2 0.9300 . ? C3 C4 1.351(7) . ? C3 H3 0.9300 . ? C4 C5 1.366(7) . ? C4 H4 0.9300 . ? C5 C6 1.377(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.379(5) . ? C7 C8 1.383(5) . ? C8 C9 1.368(6) . ? C8 H8 0.9300 . ? C9 C10 1.375(6) . ? C9 H9 0.9300 . ? C10 C11 1.369(7) . ? C10 H10 0.9300 . ? C11 C12 1.379(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.515(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.376(5) . ? C15 C16 1.389(5) . ? C16 C17 1.388(5) . ? C16 H16 0.9300 . ? C17 C18 1.361(6) . ? C17 H17 0.9300 . ? C18 C19 1.372(5) . ? C18 H18 0.9300 . ? C19 C20 1.385(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C26 1.381(5) . ? C21 C22 1.388(5) . ? C22 C23 1.386(6) . ? C22 H22 0.9300 . ? C23 C24 1.363(7) . ? C23 H23 0.9300 . ? C24 C25 1.359(6) . ? C24 H24 0.9300 . ? C25 C26 1.385(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? N27 C28 1.352(5) . ? N27 C40 1.376(4) . ? C28 C29 1.383(5) . ? C28 H28 0.9300 . ? C29 C30 1.384(6) . ? C29 H29 0.9300 . ? C30 C31 1.376(6) . ? C30 H30 0.9300 . ? C31 C40 1.411(5) . ? C31 C32 1.430(6) . ? C32 C33 1.337(6) . ? C32 H32 0.9300 . ? C33 C34 1.434(5) . ? C33 H33 0.9300 . ? C34 C35 1.396(5) . ? C34 C39 1.409(5) . ? C35 C36 1.358(6) . ? C35 H35 0.9300 . ? C36 C37 1.406(5) . ? C36 H36 0.9300 . ? C37 C38 1.375(5) . ? C37 H37 0.9300 . ? C38 C39 1.400(4) . ? C39 C40 1.421(5) . ? C1A F2A 1.265(5) . ? C1A F3A 1.284(6) . ? C1A F1A 1.347(7) . ? C1A C2A 1.523(6) . ? C2A O2A 1.215(5) . ? C2A O1A 1.227(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C38 Pt1 N27 80.18(12) . . ? C38 Pt1 P1 96.10(9) . . ? N27 Pt1 P1 173.85(8) . . ? C38 Pt1 P2 176.66(8) . . ? N27 Pt1 P2 99.47(8) . . ? P1 Pt1 P2 84.53(3) . . ? C1 P1 C7 105.21(16) . . ? C1 P1 C13 106.78(17) . . ? C7 P1 C13 103.38(16) . . ? C1 P1 Pt1 116.45(12) . . ? C7 P1 Pt1 117.10(12) . . ? C13 P1 Pt1 106.74(12) . . ? C15 P2 C21 105.85(16) . . ? C15 P2 C14 103.03(17) . . ? C21 P2 C14 104.61(17) . . ? C15 P2 Pt1 118.18(11) . . ? C21 P2 Pt1 116.03(12) . . ? C14 P2 Pt1 107.58(12) . . ? C2 C1 C6 118.2(4) . . ? C2 C1 P1 122.3(3) . . ? C6 C1 P1 119.3(3) . . ? C3 C2 C1 120.2(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.9(5) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.1(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.6(4) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C12 C7 C8 119.2(3) . . ? C12 C7 P1 123.4(3) . . ? C8 C7 P1 117.5(3) . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.5(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 119.8(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C7 120.2(4) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 P1 107.8(2) . . ? C14 C13 H13A 110.1 . . ? P1 C13 H13A 110.1 . . ? C14 C13 H13B 110.1 . . ? P1 C13 H13B 110.1 . . ? H13A C13 H13B 108.5 . . ? C13 C14 P2 108.4(2) . . ? C13 C14 H14A 110.0 . . ? P2 C14 H14A 110.0 . . ? C13 C14 H14B 110.0 . . ? P2 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C20 C15 C16 118.3(3) . . ? C20 C15 P2 120.7(3) . . ? C16 C15 P2 121.0(3) . . ? C17 C16 C15 120.1(4) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 120.9(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.4(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C15 C20 C19 121.0(4) . . ? C15 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C26 C21 C22 118.0(3) . . ? C26 C21 P2 120.8(3) . . ? C22 C21 P2 121.2(3) . . ? C23 C22 C21 120.8(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.3(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 120.8(4) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 N27 C40 117.5(3) . . ? C28 N27 Pt1 129.4(2) . . ? C40 N27 Pt1 113.0(2) . . ? N27 C28 C29 122.3(4) . . ? N27 C28 H28 118.8 . . ? C29 C28 H28 118.8 . . ? C28 C29 C30 119.8(4) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.0(4) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C40 117.9(4) . . ? C30 C31 C32 124.5(4) . . ? C40 C31 C32 117.7(4) . . ? C33 C32 C31 121.7(4) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C32 C33 C34 121.8(4) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C35 C34 C39 118.4(3) . . ? C35 C34 C33 123.4(3) . . ? C39 C34 C33 118.2(4) . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 121.1(4) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C38 C37 C36 121.3(3) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C37 C38 C39 117.0(3) . . ? C37 C38 Pt1 130.8(2) . . ? C39 C38 Pt1 112.2(2) . . ? C38 C39 C34 122.3(3) . . ? C38 C39 C40 118.0(3) . . ? C34 C39 C40 119.7(3) . . ? N27 C40 C31 122.5(3) . . ? N27 C40 C39 116.5(3) . . ? C31 C40 C39 121.0(3) . . ? F2A C1A F3A 109.9(5) . . ? F2A C1A F1A 102.0(5) . . ? F3A C1A F1A 100.2(5) . . ? F2A C1A C2A 118.0(4) . . ? F3A C1A C2A 116.2(4) . . ? F1A C1A C2A 108.0(5) . . ? O2A C2A O1A 130.0(5) . . ? O2A C2A C1A 115.1(4) . . ? O1A C2A C1A 114.8(4) . . ? 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 C38 Pt1 P1 C1 78.58(16) . . . . ? P2 Pt1 P1 C1 -98.13(13) . . . . ? C38 Pt1 P1 C7 -47.14(15) . . . . ? P2 Pt1 P1 C7 136.15(13) . . . . ? C38 Pt1 P1 C13 -162.32(15) . . . . ? P2 Pt1 P1 C13 20.98(13) . . . . ? N27 Pt1 P2 C15 -64.42(15) . . . . ? P1 Pt1 P2 C15 120.30(13) . . . . ? N27 Pt1 P2 C21 62.91(15) . . . . ? P1 Pt1 P2 C21 -112.38(13) . . . . ? N27 Pt1 P2 C14 179.61(16) . . . . ? P1 Pt1 P2 C14 4.32(14) . . . . ? C7 P1 C1 C2 -74.6(4) . . . . ? C13 P1 C1 C2 34.8(4) . . . . ? Pt1 P1 C1 C2 153.9(3) . . . . ? C7 P1 C1 C6 101.4(3) . . . . ? C13 P1 C1 C6 -149.2(3) . . . . ? Pt1 P1 C1 C6 -30.1(3) . . . . ? C6 C1 C2 C3 -0.7(7) . . . . ? P1 C1 C2 C3 175.4(4) . . . . ? C1 C2 C3 C4 -1.3(8) . . . . ? C2 C3 C4 C5 1.6(8) . . . . ? C3 C4 C5 C6 0.2(8) . . . . ? C4 C5 C6 C1 -2.2(7) . . . . ? C2 C1 C6 C5 2.5(6) . . . . ? P1 C1 C6 C5 -173.7(3) . . . . ? C1 P1 C7 C12 3.9(3) . . . . ? C13 P1 C7 C12 -107.9(3) . . . . ? Pt1 P1 C7 C12 135.1(3) . . . . ? C1 P1 C7 C8 -177.6(3) . . . . ? C13 P1 C7 C8 70.5(3) . . . . ? Pt1 P1 C7 C8 -46.5(3) . . . . ? C12 C7 C8 C9 0.5(6) . . . . ? P1 C7 C8 C9 -178.0(3) . . . . ? C7 C8 C9 C10 -1.3(6) . . . . ? C8 C9 C10 C11 1.2(7) . . . . ? C9 C10 C11 C12 -0.4(7) . . . . ? C10 C11 C12 C7 -0.4(6) . . . . ? C8 C7 C12 C11 0.3(5) . . . . ? P1 C7 C12 C11 178.8(3) . . . . ? C1 P1 C13 C14 76.3(3) . . . . ? C7 P1 C13 C14 -173.0(2) . . . . ? Pt1 P1 C13 C14 -48.9(3) . . . . ? P1 C13 C14 P2 53.3(3) . . . . ? C15 P2 C14 C13 -160.5(2) . . . . ? C21 P2 C14 C13 89.0(3) . . . . ? Pt1 P2 C14 C13 -34.9(3) . . . . ? C21 P2 C15 C20 -101.1(3) . . . . ? C14 P2 C15 C20 149.3(3) . . . . ? Pt1 P2 C15 C20 30.9(3) . . . . ? C21 P2 C15 C16 78.3(3) . . . . ? C14 P2 C15 C16 -31.2(3) . . . . ? Pt1 P2 C15 C16 -149.6(3) . . . . ? C20 C15 C16 C17 2.0(6) . . . . ? P2 C15 C16 C17 -177.5(3) . . . . ? C15 C16 C17 C18 -0.7(6) . . . . ? C16 C17 C18 C19 0.0(7) . . . . ? C17 C18 C19 C20 -0.6(6) . . . . ? C16 C15 C20 C19 -2.6(6) . . . . ? P2 C15 C20 C19 176.9(3) . . . . ? C18 C19 C20 C15 1.9(6) . . . . ? C15 P2 C21 C26 128.6(3) . . . . ? C14 P2 C21 C26 -123.0(3) . . . . ? Pt1 P2 C21 C26 -4.7(4) . . . . ? C15 P2 C21 C22 -49.3(4) . . . . ? C14 P2 C21 C22 59.1(4) . . . . ? Pt1 P2 C21 C22 177.4(3) . . . . ? C26 C21 C22 C23 1.0(7) . . . . ? P2 C21 C22 C23 178.9(4) . . . . ? C21 C22 C23 C24 -1.5(8) . . . . ? C22 C23 C24 C25 1.5(9) . . . . ? C23 C24 C25 C26 -1.1(9) . . . . ? C22 C21 C26 C25 -0.5(6) . . . . ? P2 C21 C26 C25 -178.5(4) . . . . ? C24 C25 C26 C21 0.6(8) . . . . ? C38 Pt1 N27 C28 175.2(3) . . . . ? P2 Pt1 N27 C28 -8.1(3) . . . . ? C38 Pt1 N27 C40 -2.2(2) . . . . ? P2 Pt1 N27 C40 174.4(2) . . . . ? C40 N27 C28 C29 -2.2(6) . . . . ? Pt1 N27 C28 C29 -179.6(3) . . . . ? N27 C28 C29 C30 0.3(7) . . . . ? C28 C29 C30 C31 1.7(7) . . . . ? C29 C30 C31 C40 -1.5(7) . . . . ? C29 C30 C31 C32 178.3(4) . . . . ? C30 C31 C32 C33 -178.1(4) . . . . ? C40 C31 C32 C33 1.7(6) . . . . ? C31 C32 C33 C34 0.4(6) . . . . ? C32 C33 C34 C35 176.5(4) . . . . ? C32 C33 C34 C39 -2.3(6) . . . . ? C39 C34 C35 C36 -1.4(5) . . . . ? C33 C34 C35 C36 179.7(4) . . . . ? C34 C35 C36 C37 0.6(6) . . . . ? C35 C36 C37 C38 0.7(6) . . . . ? C36 C37 C38 C39 -1.1(5) . . . . ? C36 C37 C38 Pt1 179.5(3) . . . . ? N27 Pt1 C38 C37 -178.1(3) . . . . ? P1 Pt1 C38 C37 -3.1(3) . . . . ? N27 Pt1 C38 C39 2.4(2) . . . . ? P1 Pt1 C38 C39 177.5(2) . . . . ? C37 C38 C39 C34 0.1(5) . . . . ? Pt1 C38 C39 C34 179.7(3) . . . . ? C37 C38 C39 C40 178.1(3) . . . . ? Pt1 C38 C39 C40 -2.4(4) . . . . ? C35 C34 C39 C38 1.1(5) . . . . ? C33 C34 C39 C38 -180.0(3) . . . . ? C35 C34 C39 C40 -176.8(3) . . . . ? C33 C34 C39 C40 2.1(5) . . . . ? C28 N27 C40 C31 2.3(5) . . . . ? Pt1 N27 C40 C31 -179.9(3) . . . . ? C28 N27 C40 C39 -176.2(3) . . . . ? Pt1 N27 C40 C39 1.6(4) . . . . ? C30 C31 C40 N27 -0.5(6) . . . . ? C32 C31 C40 N27 179.6(3) . . . . ? C30 C31 C40 C39 177.9(4) . . . . ? C32 C31 C40 C39 -1.9(5) . . . . ? C38 C39 C40 N27 0.5(5) . . . . ? C34 C39 C40 N27 178.5(3) . . . . ? C38 C39 C40 C31 -178.0(3) . . . . ? C34 C39 C40 C31 0.0(5) . . . . ? F2A C1A C2A O2A -10.7(8) . . . . ? F3A C1A C2A O2A -144.5(5) . . . . ? F1A C1A C2A O2A 104.0(5) . . . . ? F2A C1A C2A O1A 170.8(5) . . . . ? F3A C1A C2A O1A 37.1(7) . . . . ? F1A C1A C2A O1A -74.4(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11 O1A 0.93 2.42 3.314(5) 161.5 1_554 C13 H13B F3A 0.97 2.54 3.318(5) 137.1 4_565 C14 H14B O1A 0.97 2.30 3.178(5) 149.6 4_565 C19 H19 F2A 0.93 2.59 3.387(6) 144.1 4_665 C35 H35 O2A 0.93 2.45 3.333(5) 158.5 1_654 _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.793 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.075 ####################################################################### # # 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 _database_code_depnum_ccdc_archive 'CCDC 919437' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H27 F3 N O2 P Pt' _chemical_formula_weight 740.61 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2693(17) _cell_length_b 11.3130(7) _cell_length_c 13.852(2) _cell_angle_alpha 87.140(8) _cell_angle_beta 72.665(15) _cell_angle_gamma 70.061(9) _cell_volume 1441.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1069 _cell_measurement_theta_min 3.0457 _cell_measurement_theta_max 27.8014 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 4.971 _exptl_absorpt_correction_T_min 0.64630 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1544 _diffrn_measurement_method '/w scan' _diffrn_reflns_number 10415 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 28.07 _reflns_number_total 5899 _reflns_number_gt 5365 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_cell_refinement 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_data_reduction 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Stereochemical Workstation (Siemens, 1989)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0353P)^2^+1.8227P] 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 SHELXL _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5899 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.262319(16) 0.035449(13) 0.238327(11) 0.03081(7) Uani 1 1 d . . . P1 P 0.10454(11) 0.22016(9) 0.23181(8) 0.0279(2) Uani 1 1 d . . . C1 C -0.0627(5) 0.2584(4) 0.3382(3) 0.0330(9) Uani 1 1 d . . . C2 C -0.1897(5) 0.3539(5) 0.3377(4) 0.0470(12) Uani 1 1 d . . . H2 H -0.1937 0.3987 0.2798 0.056 Uiso 1 1 calc R . . C3 C -0.3106(6) 0.3837(6) 0.4217(4) 0.0612(15) Uani 1 1 d . . . H3 H -0.3947 0.4490 0.4205 0.073 Uiso 1 1 calc R . . C4 C -0.3074(6) 0.3178(6) 0.5068(4) 0.0600(15) Uani 1 1 d . . . H4 H -0.3899 0.3368 0.5627 0.072 Uiso 1 1 calc R . . C5 C -0.1830(7) 0.2240(6) 0.5096(4) 0.0613(15) Uani 1 1 d . . . H5 H -0.1803 0.1799 0.5679 0.074 Uiso 1 1 calc R . . C6 C -0.0606(6) 0.1942(5) 0.4258(4) 0.0493(12) Uani 1 1 d . . . H6 H 0.0239 0.1304 0.4285 0.059 Uiso 1 1 calc R . . C7 C 0.0514(4) 0.2394(4) 0.1157(3) 0.0300(8) Uani 1 1 d . . . C8 C 0.0905(5) 0.1357(4) 0.0501(4) 0.0436(11) Uani 1 1 d . . . H8 H 0.1455 0.0569 0.0652 0.052 Uiso 1 1 calc R . . C9 C 0.0491(7) 0.1478(5) -0.0369(4) 0.0556(13) Uani 1 1 d . . . H9 H 0.0759 0.0772 -0.0796 0.067 Uiso 1 1 calc R . . C10 C -0.0315(6) 0.2636(5) -0.0610(4) 0.0504(12) Uani 1 1 d . . . H10 H -0.0603 0.2713 -0.1193 0.061 Uiso 1 1 calc R . . C11 C -0.0690(5) 0.3676(5) 0.0019(4) 0.0461(11) Uani 1 1 d . . . H11 H -0.1227 0.4462 -0.0144 0.055 Uiso 1 1 calc R . . C12 C -0.0276(5) 0.3569(4) 0.0893(3) 0.0376(9) Uani 1 1 d . . . H12 H -0.0527 0.4283 0.1307 0.045 Uiso 1 1 calc R . . C13 C 0.1629(5) 0.3552(4) 0.2354(3) 0.0360(9) Uani 1 1 d . . . C14 C 0.2650(5) 0.3749(5) 0.1509(4) 0.0462(11) Uani 1 1 d . . . H14 H 0.3005 0.3217 0.0929 0.055 Uiso 1 1 calc R . . C15 C 0.3139(7) 0.4748(6) 0.1532(5) 0.0659(17) Uani 1 1 d . . . H15 H 0.3834 0.4877 0.0970 0.079 Uiso 1 1 calc R . . C16 C 0.2603(7) 0.5543(5) 0.2381(6) 0.076(2) Uani 1 1 d . . . H16 H 0.2932 0.6211 0.2392 0.091 Uiso 1 1 calc R . . C17 C 0.1590(8) 0.5359(6) 0.3208(6) 0.077(2) Uani 1 1 d . . . H17 H 0.1221 0.5913 0.3776 0.093 Uiso 1 1 calc R . . C18 C 0.1100(6) 0.4357(5) 0.3213(5) 0.0567(14) Uani 1 1 d . . . H18 H 0.0425 0.4225 0.3786 0.068 Uiso 1 1 calc R . . N19 N 0.4405(4) 0.1001(3) 0.2241(3) 0.0332(7) Uani 1 1 d . . . C20 C 0.4673(5) 0.1483(5) 0.3003(4) 0.0428(10) Uani 1 1 d . . . C21 C 0.5814(6) 0.1958(6) 0.2786(5) 0.0644(16) Uani 1 1 d . . . H21 H 0.6014 0.2271 0.3312 0.077 Uiso 1 1 calc R . . C22 C 0.6639(6) 0.1969(7) 0.1808(5) 0.0707(17) Uani 1 1 d . . . H22 H 0.7381 0.2306 0.1666 0.085 Uiso 1 1 calc R . . C23 C 0.6354(6) 0.1476(5) 0.1042(4) 0.0569(14) Uani 1 1 d . . . H23 H 0.6896 0.1472 0.0371 0.068 Uiso 1 1 calc R . . C24 C 0.5251(5) 0.0989(5) 0.1287(4) 0.0461(11) Uani 1 1 d . . . H24 H 0.5078 0.0633 0.0768 0.055 Uiso 1 1 calc R . . C25 C 0.3767(5) 0.1508(5) 0.4056(4) 0.0442(11) Uani 1 1 d . . . C26 C 0.3449(6) 0.0465(5) 0.4476(4) 0.0483(12) Uani 1 1 d . . . H26 H 0.3781 -0.0277 0.4077 0.058 Uiso 1 1 calc R . . C27 C 0.2647(7) 0.0511(7) 0.5476(4) 0.0675(16) Uani 1 1 d . . . H27 H 0.2444 -0.0197 0.5747 0.081 Uiso 1 1 calc R . . C28 C 0.2152(9) 0.1593(8) 0.6067(5) 0.085(2) Uani 1 1 d . . . H28 H 0.1616 0.1618 0.6743 0.102 Uiso 1 1 calc R . . C29 C 0.2438(9) 0.2636(8) 0.5674(5) 0.085(2) Uani 1 1 d . . . H29 H 0.2088 0.3372 0.6083 0.102 Uiso 1 1 calc R . . C30 C 0.3243(7) 0.2613(6) 0.4676(5) 0.0658(16) Uani 1 1 d . . . H30 H 0.3436 0.3329 0.4414 0.079 Uiso 1 1 calc R . . O31 O 0.4069(3) -0.1475(3) 0.2479(2) 0.0394(7) Uani 1 1 d . . . C32 C 0.4917(6) -0.2080(4) 0.1679(4) 0.0462(11) Uani 1 1 d . . . O33 O 0.5008(7) -0.1826(5) 0.0815(3) 0.111(2) Uani 1 1 d . . . C34 C 0.6048(6) -0.3292(5) 0.1846(4) 0.0570(14) Uani 1 1 d . . . F35 F 0.7309(5) -0.3313(6) 0.1552(7) 0.183(4) Uani 1 1 d . . . F36 F 0.6153(8) -0.4242(5) 0.1258(6) 0.162(3) Uani 1 1 d . . . F37 F 0.5761(6) -0.3727(5) 0.2702(4) 0.158(3) Uani 1 1 d . . . C38 C 0.1073(5) -0.0450(4) 0.2474(4) 0.0457(11) Uani 1 1 d . . . H38A H 0.1452 -0.1125 0.1964 0.068 Uiso 1 1 calc R . . H38B H 0.0226 0.0174 0.2368 0.068 Uiso 1 1 calc R . . H38C H 0.0817 -0.0773 0.3131 0.068 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 0.03200(10) 0.02710(10) 0.03305(10) 0.00190(6) -0.01305(7) -0.00691(6) P1 0.0290(5) 0.0262(5) 0.0297(5) 0.0018(4) -0.0096(4) -0.0099(4) C1 0.035(2) 0.035(2) 0.030(2) 0.0008(17) -0.0075(18) -0.0156(18) C2 0.038(3) 0.050(3) 0.039(2) 0.004(2) -0.001(2) -0.006(2) C3 0.042(3) 0.069(4) 0.051(3) -0.006(3) 0.000(2) -0.003(3) C4 0.057(3) 0.073(4) 0.037(3) -0.010(3) 0.009(2) -0.023(3) C5 0.079(4) 0.070(4) 0.032(3) 0.009(2) -0.010(3) -0.028(3) C6 0.051(3) 0.049(3) 0.040(3) 0.008(2) -0.012(2) -0.010(2) C7 0.028(2) 0.032(2) 0.032(2) 0.0047(16) -0.0090(17) -0.0130(16) C8 0.053(3) 0.032(2) 0.045(3) 0.0024(19) -0.021(2) -0.008(2) C9 0.078(4) 0.048(3) 0.047(3) -0.003(2) -0.028(3) -0.020(3) C10 0.061(3) 0.061(3) 0.039(3) 0.011(2) -0.026(2) -0.025(3) C11 0.045(3) 0.046(3) 0.044(3) 0.014(2) -0.016(2) -0.011(2) C12 0.037(2) 0.034(2) 0.038(2) 0.0013(18) -0.0100(19) -0.0072(18) C13 0.037(2) 0.028(2) 0.046(2) 0.0019(18) -0.019(2) -0.0096(17) C14 0.047(3) 0.043(3) 0.052(3) 0.006(2) -0.016(2) -0.019(2) C15 0.059(4) 0.062(4) 0.092(5) 0.030(3) -0.027(3) -0.039(3) C16 0.076(5) 0.047(3) 0.126(7) 0.002(4) -0.046(5) -0.035(3) C17 0.078(5) 0.063(4) 0.102(5) -0.025(4) -0.025(4) -0.036(3) C18 0.059(3) 0.053(3) 0.064(3) -0.013(3) -0.014(3) -0.027(3) N19 0.0253(17) 0.0370(19) 0.0338(18) 0.0040(15) -0.0082(15) -0.0072(14) C20 0.039(2) 0.052(3) 0.045(3) 0.008(2) -0.019(2) -0.019(2) C21 0.060(4) 0.096(5) 0.059(3) 0.006(3) -0.025(3) -0.047(3) C22 0.049(3) 0.099(5) 0.077(4) 0.013(4) -0.015(3) -0.045(3) C23 0.040(3) 0.069(4) 0.050(3) 0.005(3) 0.003(2) -0.019(3) C24 0.045(3) 0.049(3) 0.043(3) 0.004(2) -0.014(2) -0.013(2) C25 0.040(3) 0.059(3) 0.040(2) 0.003(2) -0.019(2) -0.021(2) C26 0.048(3) 0.061(3) 0.040(3) 0.003(2) -0.017(2) -0.020(2) C27 0.076(4) 0.089(5) 0.049(3) 0.016(3) -0.021(3) -0.042(4) C28 0.093(5) 0.119(6) 0.042(3) -0.007(4) -0.003(3) -0.050(5) C29 0.100(6) 0.091(5) 0.060(4) -0.026(4) -0.007(4) -0.037(4) C30 0.074(4) 0.071(4) 0.059(4) -0.007(3) -0.017(3) -0.034(3) O31 0.0409(17) 0.0350(16) 0.0333(16) 0.0034(13) -0.0092(14) -0.0036(13) C32 0.054(3) 0.039(2) 0.035(2) 0.000(2) -0.009(2) -0.006(2) O33 0.151(5) 0.086(3) 0.038(2) -0.001(2) -0.022(3) 0.028(3) C34 0.042(3) 0.048(3) 0.058(3) 0.004(3) 0.002(2) -0.002(2) F35 0.055(3) 0.128(5) 0.338(10) 0.110(6) -0.039(4) -0.026(3) F36 0.179(6) 0.068(3) 0.208(7) -0.045(4) -0.079(5) 0.021(3) F37 0.126(4) 0.124(4) 0.095(3) 0.061(3) 0.018(3) 0.064(3) C38 0.050(3) 0.037(2) 0.058(3) 0.010(2) -0.025(2) -0.018(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C38 2.058(5) . ? Pt1 O31 2.121(3) . ? Pt1 N19 2.146(3) . ? Pt1 P1 2.1815(11) . ? P1 C7 1.828(4) . ? P1 C13 1.829(4) . ? P1 C1 1.832(4) . ? C1 C2 1.383(6) . ? C1 C6 1.385(6) . ? C2 C3 1.379(7) . ? C3 C4 1.365(8) . ? C4 C5 1.364(8) . ? C5 C6 1.386(7) . ? C7 C8 1.389(6) . ? C7 C12 1.396(6) . ? C8 C9 1.379(7) . ? C9 C10 1.376(7) . ? C10 C11 1.374(7) . ? C11 C12 1.385(6) . ? C13 C14 1.386(7) . ? C13 C18 1.388(7) . ? C14 C15 1.390(7) . ? C15 C16 1.369(9) . ? C16 C17 1.360(9) . ? C17 C18 1.388(7) . ? N19 C24 1.345(6) . ? N19 C20 1.349(6) . ? C20 C21 1.399(7) . ? C20 C25 1.474(7) . ? C21 C22 1.369(8) . ? C22 C23 1.371(8) . ? C23 C24 1.371(7) . ? C25 C26 1.385(7) . ? C25 C30 1.401(7) . ? C26 C27 1.377(7) . ? C27 C28 1.361(9) . ? C28 C29 1.361(10) . ? C29 C30 1.380(9) . ? O31 C32 1.244(5) . ? C32 O33 1.201(6) . ? C32 C34 1.525(7) . ? C34 F35 1.229(7) . ? C34 F37 1.252(7) . ? C34 F36 1.337(8) . ? 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 C38 Pt1 O31 87.75(16) . . ? C38 Pt1 N19 174.03(16) . . ? O31 Pt1 N19 86.64(13) . . ? C38 Pt1 P1 89.56(14) . . ? O31 Pt1 P1 177.13(9) . . ? N19 Pt1 P1 96.09(9) . . ? C7 P1 C13 102.63(19) . . ? C7 P1 C1 107.06(19) . . ? C13 P1 C1 103.0(2) . . ? C7 P1 Pt1 113.63(14) . . ? C13 P1 Pt1 116.14(14) . . ? C1 P1 Pt1 113.24(14) . . ? C2 C1 C6 117.9(4) . . ? C2 C1 P1 123.1(3) . . ? C6 C1 P1 118.9(4) . . ? C3 C2 C1 120.9(5) . . ? C4 C3 C2 120.4(5) . . ? C5 C4 C3 119.9(5) . . ? C4 C5 C6 120.1(5) . . ? C1 C6 C5 120.8(5) . . ? C8 C7 C12 118.0(4) . . ? C8 C7 P1 120.1(3) . . ? C12 C7 P1 121.9(3) . . ? C9 C8 C7 121.0(4) . . ? C10 C9 C8 120.6(5) . . ? C11 C10 C9 119.3(4) . . ? C10 C11 C12 120.8(4) . . ? C11 C12 C7 120.4(4) . . ? C14 C13 C18 119.7(4) . . ? C14 C13 P1 118.8(3) . . ? C18 C13 P1 121.5(4) . . ? C13 C14 C15 119.7(5) . . ? C16 C15 C14 120.2(6) . . ? C17 C16 C15 120.3(5) . . ? C16 C17 C18 120.8(6) . . ? C17 C18 C13 119.3(6) . . ? C24 N19 C20 118.8(4) . . ? C24 N19 Pt1 115.2(3) . . ? C20 N19 Pt1 125.8(3) . . ? N19 C20 C21 119.5(5) . . ? N19 C20 C25 120.1(4) . . ? C21 C20 C25 120.3(4) . . ? C22 C21 C20 120.9(5) . . ? C21 C22 C23 118.9(5) . . ? C24 C23 C22 118.6(5) . . ? N19 C24 C23 123.3(5) . . ? C26 C25 C30 118.1(5) . . ? C26 C25 C20 122.7(5) . . ? C30 C25 C20 119.2(5) . . ? C27 C26 C25 120.9(5) . . ? C28 C27 C26 120.1(6) . . ? C29 C28 C27 120.3(6) . . ? C28 C29 C30 120.7(6) . . ? C29 C30 C25 119.8(6) . . ? C32 O31 Pt1 118.4(3) . . ? O33 C32 O31 129.9(5) . . ? O33 C32 C34 116.4(5) . . ? O31 C32 C34 113.6(4) . . ? F35 C34 F37 111.6(7) . . ? F35 C34 F36 99.9(6) . . ? F37 C34 F36 100.8(6) . . ? F35 C34 C32 115.4(5) . . ? F37 C34 C32 116.6(5) . . ? F36 C34 C32 110.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C38 Pt1 P1 C7 -67.4(2) . . . . ? N19 Pt1 P1 C7 110.66(17) . . . . ? C38 Pt1 P1 C13 173.9(2) . . . . ? N19 Pt1 P1 C13 -8.06(19) . . . . ? C38 Pt1 P1 C1 55.0(2) . . . . ? N19 Pt1 P1 C1 -126.91(17) . . . . ? C7 P1 C1 C2 -37.6(4) . . . . ? C13 P1 C1 C2 70.2(4) . . . . ? Pt1 P1 C1 C2 -163.6(4) . . . . ? C7 P1 C1 C6 146.4(4) . . . . ? C13 P1 C1 C6 -105.9(4) . . . . ? Pt1 P1 C1 C6 20.3(4) . . . . ? C6 C1 C2 C3 -0.3(8) . . . . ? P1 C1 C2 C3 -176.4(4) . . . . ? C1 C2 C3 C4 -1.0(9) . . . . ? C2 C3 C4 C5 1.6(9) . . . . ? C3 C4 C5 C6 -1.0(9) . . . . ? C2 C1 C6 C5 0.9(8) . . . . ? P1 C1 C6 C5 177.2(4) . . . . ? C4 C5 C6 C1 -0.3(9) . . . . ? C13 P1 C7 C8 137.3(4) . . . . ? C1 P1 C7 C8 -114.7(4) . . . . ? Pt1 P1 C7 C8 11.1(4) . . . . ? C13 P1 C7 C12 -42.2(4) . . . . ? C1 P1 C7 C12 65.8(4) . . . . ? Pt1 P1 C7 C12 -168.4(3) . . . . ? C12 C7 C8 C9 -1.8(7) . . . . ? P1 C7 C8 C9 178.7(4) . . . . ? C7 C8 C9 C10 0.4(8) . . . . ? C8 C9 C10 C11 0.8(8) . . . . ? C9 C10 C11 C12 -0.6(8) . . . . ? C10 C11 C12 C7 -0.9(7) . . . . ? C8 C7 C12 C11 2.0(6) . . . . ? P1 C7 C12 C11 -178.5(3) . . . . ? C7 P1 C13 C14 -52.4(4) . . . . ? C1 P1 C13 C14 -163.5(4) . . . . ? Pt1 P1 C13 C14 72.1(4) . . . . ? C7 P1 C13 C18 129.2(4) . . . . ? C1 P1 C13 C18 18.1(5) . . . . ? Pt1 P1 C13 C18 -106.3(4) . . . . ? C18 C13 C14 C15 0.4(7) . . . . ? P1 C13 C14 C15 -178.1(4) . . . . ? C13 C14 C15 C16 -0.9(8) . . . . ? C14 C15 C16 C17 0.2(10) . . . . ? C15 C16 C17 C18 1.0(11) . . . . ? C16 C17 C18 C13 -1.5(10) . . . . ? C14 C13 C18 C17 0.8(8) . . . . ? P1 C13 C18 C17 179.2(5) . . . . ? O31 Pt1 N19 C24 89.2(3) . . . . ? P1 Pt1 N19 C24 -91.7(3) . . . . ? O31 Pt1 N19 C20 -95.6(4) . . . . ? P1 Pt1 N19 C20 83.5(4) . . . . ? C24 N19 C20 C21 0.1(7) . . . . ? Pt1 N19 C20 C21 -175.0(4) . . . . ? C24 N19 C20 C25 -179.9(4) . . . . ? Pt1 N19 C20 C25 5.0(6) . . . . ? N19 C20 C21 C22 1.6(9) . . . . ? C25 C20 C21 C22 -178.4(6) . . . . ? C20 C21 C22 C23 -1.6(10) . . . . ? C21 C22 C23 C24 -0.1(9) . . . . ? C20 N19 C24 C23 -1.9(7) . . . . ? Pt1 N19 C24 C23 173.8(4) . . . . ? C22 C23 C24 N19 1.9(8) . . . . ? N19 C20 C25 C26 48.7(7) . . . . ? C21 C20 C25 C26 -131.4(6) . . . . ? N19 C20 C25 C30 -133.6(5) . . . . ? C21 C20 C25 C30 46.4(7) . . . . ? C30 C25 C26 C27 -0.4(8) . . . . ? C20 C25 C26 C27 177.3(5) . . . . ? C25 C26 C27 C28 0.1(9) . . . . ? C26 C27 C28 C29 0.3(11) . . . . ? C27 C28 C29 C30 -0.5(13) . . . . ? C28 C29 C30 C25 0.2(11) . . . . ? C26 C25 C30 C29 0.2(9) . . . . ? C20 C25 C30 C29 -177.6(6) . . . . ? C38 Pt1 O31 C32 96.2(4) . . . . ? N19 Pt1 O31 C32 -81.7(4) . . . . ? Pt1 O31 C32 O33 -5.0(9) . . . . ? Pt1 O31 C32 C34 171.5(3) . . . . ? O33 C32 C34 F35 63.5(10) . . . . ? O31 C32 C34 F35 -113.5(7) . . . . ? O33 C32 C34 F37 -162.7(7) . . . . ? O31 C32 C34 F37 20.3(9) . . . . ? O33 C32 C34 F36 -48.7(8) . . . . ? O31 C32 C34 F36 134.3(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 F37 0.93 2.47 3.389(7) 169.2 2_556 C24 H24 O33 0.93 2.52 3.075(6) 118.2 2_655 _diffrn_measured_fraction_theta_max 0.842 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.574 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.103 ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H29 F3 N O2 P Pt' _chemical_formula_weight 754.63 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3756(4) _cell_length_b 11.2883(4) _cell_length_c 14.2333(5) _cell_angle_alpha 87.582(3) _cell_angle_beta 73.443(3) _cell_angle_gamma 69.265(4) _cell_volume 1491.22(11) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5824 _cell_measurement_theta_min 2.9846 _cell_measurement_theta_max 27.9991 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 4.808 _exptl_absorpt_correction_T_min 0.67494 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1544 _diffrn_measurement_method '/w scan' _diffrn_reflns_number 10768 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 28.06 _reflns_number_total 6085 _reflns_number_gt 5422 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_cell_refinement 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_data_reduction 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Stereochemical Workstation (Siemens, 1989)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0269P)^2^+1.1709P] 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 SHELXL _refine_ls_extinction_coef 0.0038(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6085 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0647 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.271476(17) 0.037664(13) 0.231824(12) 0.04032(7) Uani 1 1 d . . . P1 P 0.10639(10) 0.22250(8) 0.23144(7) 0.0330(2) Uani 1 1 d . . . C1 C -0.0552(4) 0.2552(4) 0.3358(3) 0.0385(9) Uani 1 1 d . . . C2 C -0.1871(5) 0.3492(4) 0.3368(3) 0.0512(11) Uani 1 1 d . . . H2 H -0.1955 0.3945 0.2814 0.061 Uiso 1 1 calc R . . C3 C -0.3051(6) 0.3757(5) 0.4193(4) 0.0693(14) Uani 1 1 d . . . H3 H -0.3917 0.4391 0.4192 0.083 Uiso 1 1 calc R . . C4 C -0.2944(7) 0.3093(6) 0.5002(4) 0.0740(16) Uani 1 1 d . . . H4 H -0.3741 0.3268 0.5553 0.089 Uiso 1 1 calc R . . C5 C -0.1671(7) 0.2168(6) 0.5009(4) 0.0772(17) Uani 1 1 d . . . H5 H -0.1609 0.1712 0.5564 0.093 Uiso 1 1 calc R . . C6 C -0.0464(6) 0.1902(4) 0.4193(3) 0.0604(13) Uani 1 1 d . . . H6 H 0.0403 0.1284 0.4212 0.073 Uiso 1 1 calc R . . C7 C 0.0486(4) 0.2432(3) 0.1204(3) 0.0337(8) Uani 1 1 d . . . C8 C 0.0853(5) 0.1392(4) 0.0560(3) 0.0447(10) Uani 1 1 d . . . H8 H 0.1414 0.0593 0.0693 0.054 Uiso 1 1 calc R . . C9 C 0.0401(5) 0.1527(4) -0.0271(3) 0.0555(12) Uani 1 1 d . . . H9 H 0.0649 0.0820 -0.0689 0.067 Uiso 1 1 calc R . . C10 C -0.0415(5) 0.2699(4) -0.0486(3) 0.0529(11) Uani 1 1 d . . . H10 H -0.0737 0.2786 -0.1040 0.063 Uiso 1 1 calc R . . C11 C -0.0755(5) 0.3750(4) 0.0129(3) 0.0476(10) Uani 1 1 d . . . H11 H -0.1293 0.4549 -0.0020 0.057 Uiso 1 1 calc R . . C12 C -0.0303(4) 0.3619(3) 0.0954(3) 0.0390(9) Uani 1 1 d . . . H12 H -0.0526 0.4336 0.1355 0.047 Uiso 1 1 calc R . . C13 C 0.1580(4) 0.3597(3) 0.2377(3) 0.0397(9) Uani 1 1 d . . . C14 C 0.2556(5) 0.3833(4) 0.1572(4) 0.0540(11) Uani 1 1 d . . . H14 H 0.2910 0.3311 0.0999 0.065 Uiso 1 1 calc R . . C15 C 0.3009(6) 0.4832(5) 0.1613(5) 0.0725(16) Uani 1 1 d . . . H15 H 0.3674 0.4981 0.1073 0.087 Uiso 1 1 calc R . . C16 C 0.2465(7) 0.5615(5) 0.2464(6) 0.085(2) Uani 1 1 d . . . H16 H 0.2758 0.6298 0.2492 0.102 Uiso 1 1 calc R . . C17 C 0.1507(7) 0.5393(5) 0.3256(5) 0.0847(18) Uani 1 1 d . . . H17 H 0.1152 0.5923 0.3825 0.102 Uiso 1 1 calc R . . C18 C 0.1057(6) 0.4392(4) 0.3226(4) 0.0618(13) Uani 1 1 d . . . H18 H 0.0401 0.4246 0.3775 0.074 Uiso 1 1 calc R . . N19 N 0.4453(3) 0.1046(3) 0.2145(2) 0.0419(8) Uani 1 1 d . . . C20 C 0.4760(4) 0.1538(4) 0.2862(3) 0.0460(10) Uani 1 1 d . . . C21 C 0.5874(5) 0.2005(5) 0.2632(4) 0.0695(14) Uani 1 1 d . . . H21 H 0.6091 0.2329 0.3133 0.083 Uiso 1 1 calc R . . C22 C 0.6657(6) 0.1994(6) 0.1682(4) 0.0721(15) Uani 1 1 d . . . H22 H 0.7397 0.2316 0.1533 0.086 Uiso 1 1 calc R . . C23 C 0.6343(5) 0.1508(5) 0.0952(4) 0.0626(13) Uani 1 1 d . . . H23 H 0.6856 0.1498 0.0298 0.075 Uiso 1 1 calc R . . C24 C 0.5249(5) 0.1030(4) 0.1207(3) 0.0533(11) Uani 1 1 d . . . H24 H 0.5048 0.0680 0.0710 0.064 Uiso 1 1 calc R . . C25 C 0.3933(5) 0.1552(4) 0.3895(3) 0.0480(10) Uani 1 1 d . . . C26 C 0.3641(5) 0.0507(4) 0.4303(3) 0.0530(11) Uani 1 1 d . . . H26 H 0.3913 -0.0226 0.3907 0.064 Uiso 1 1 calc R . . C27 C 0.2947(5) 0.0546(5) 0.5296(4) 0.0602(12) Uani 1 1 d . . . H27 H 0.2759 -0.0166 0.5555 0.072 Uiso 1 1 calc R . . C28 C 0.2531(6) 0.1603(6) 0.5906(4) 0.0648(13) Uani 1 1 d . . . C28A C 0.1845(7) 0.1619(7) 0.6997(4) 0.099(2) Uani 1 1 d . . . H28A H 0.1191 0.2461 0.7240 0.149 Uiso 1 1 calc R . . H28B H 0.2579 0.1361 0.7328 0.149 Uiso 1 1 calc R . . H28C H 0.1328 0.1044 0.7118 0.149 Uiso 1 1 calc R . . C29 C 0.2792(6) 0.2651(5) 0.5493(4) 0.0704(14) Uani 1 1 d . . . H29 H 0.2490 0.3391 0.5888 0.084 Uiso 1 1 calc R . . C30 C 0.3492(5) 0.2632(5) 0.4504(3) 0.0588(12) Uani 1 1 d . . . H30 H 0.3667 0.3350 0.4248 0.071 Uiso 1 1 calc R . . O31 O 0.4175(4) -0.1475(3) 0.2422(2) 0.0633(9) Uani 1 1 d . . . C32 C 0.4922(6) -0.2117(5) 0.1685(4) 0.0677(14) Uani 1 1 d . . . O33 O 0.4996(7) -0.1892(5) 0.0829(4) 0.157(3) Uani 1 1 d . . . C34 C 0.5993(6) -0.3403(5) 0.1790(4) 0.0658(14) Uani 1 1 d . . . F35 F 0.7304(4) -0.3442(4) 0.1465(4) 0.1314(17) Uani 1 1 d . . . F36 F 0.5950(4) -0.4328(4) 0.1309(4) 0.1393(19) Uani 1 1 d . . . F37 F 0.5790(6) -0.3713(4) 0.2699(4) 0.178(3) Uani 1 1 d . . . C38 C 0.1240(5) -0.0462(4) 0.2424(4) 0.0541(12) Uani 1 1 d . . . H38A H 0.1601 -0.1116 0.1906 0.081 Uiso 1 1 calc R . . H38B H 0.0357 0.0162 0.2368 0.081 Uiso 1 1 calc R . . H38C H 0.1066 -0.0828 0.3048 0.081 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 0.03952(10) 0.02961(9) 0.05360(12) -0.00167(6) -0.02416(8) -0.00554(7) P1 0.0323(5) 0.0277(5) 0.0404(5) 0.0010(4) -0.0147(4) -0.0088(4) C1 0.043(2) 0.038(2) 0.038(2) -0.0015(16) -0.0126(18) -0.0169(18) C2 0.040(2) 0.058(3) 0.047(2) 0.000(2) -0.008(2) -0.011(2) C3 0.049(3) 0.083(4) 0.059(3) -0.018(3) 0.000(2) -0.013(3) C4 0.074(4) 0.085(4) 0.052(3) -0.019(3) 0.010(3) -0.036(3) C5 0.113(5) 0.088(4) 0.038(3) 0.010(3) -0.015(3) -0.051(4) C6 0.073(3) 0.056(3) 0.049(3) 0.007(2) -0.022(3) -0.017(3) C7 0.0306(19) 0.0339(19) 0.036(2) 0.0016(15) -0.0102(16) -0.0108(16) C8 0.050(2) 0.038(2) 0.043(2) 0.0004(17) -0.016(2) -0.0098(19) C9 0.070(3) 0.052(3) 0.042(2) -0.0062(19) -0.017(2) -0.018(2) C10 0.055(3) 0.068(3) 0.037(2) 0.009(2) -0.016(2) -0.021(2) C11 0.043(2) 0.050(2) 0.042(2) 0.0118(19) -0.0131(19) -0.008(2) C12 0.038(2) 0.036(2) 0.041(2) 0.0011(16) -0.0101(18) -0.0109(17) C13 0.037(2) 0.0290(19) 0.059(3) 0.0027(17) -0.023(2) -0.0116(16) C14 0.053(3) 0.047(2) 0.072(3) 0.013(2) -0.026(2) -0.025(2) C15 0.063(3) 0.057(3) 0.112(5) 0.026(3) -0.034(3) -0.035(3) C16 0.086(4) 0.052(3) 0.141(6) 0.007(4) -0.054(5) -0.039(3) C17 0.094(5) 0.062(3) 0.112(5) -0.023(3) -0.035(4) -0.036(3) C18 0.064(3) 0.053(3) 0.072(3) -0.015(2) -0.018(3) -0.023(2) N19 0.0337(18) 0.0414(18) 0.045(2) -0.0050(14) -0.0145(15) -0.0038(15) C20 0.037(2) 0.055(3) 0.048(2) -0.0018(19) -0.0152(19) -0.0153(19) C21 0.058(3) 0.110(4) 0.058(3) -0.003(3) -0.016(3) -0.050(3) C22 0.051(3) 0.100(4) 0.071(4) -0.002(3) -0.007(3) -0.041(3) C23 0.046(3) 0.074(3) 0.053(3) -0.004(2) 0.000(2) -0.015(2) C24 0.049(3) 0.055(3) 0.049(3) -0.009(2) -0.016(2) -0.008(2) C25 0.041(2) 0.061(3) 0.050(3) -0.001(2) -0.020(2) -0.021(2) C26 0.053(3) 0.056(3) 0.059(3) 0.001(2) -0.027(2) -0.022(2) C27 0.061(3) 0.077(3) 0.059(3) 0.012(2) -0.023(3) -0.041(3) C28 0.058(3) 0.094(4) 0.052(3) 0.002(3) -0.011(2) -0.041(3) C28A 0.099(5) 0.147(6) 0.060(4) -0.002(4) 0.000(3) -0.072(5) C29 0.073(4) 0.080(4) 0.059(3) -0.013(3) -0.010(3) -0.034(3) C30 0.067(3) 0.062(3) 0.058(3) 0.001(2) -0.018(3) -0.034(3) O31 0.062(2) 0.0505(19) 0.066(2) -0.0094(16) -0.0262(18) 0.0008(16) C32 0.064(3) 0.073(4) 0.059(3) -0.012(3) -0.016(3) -0.016(3) O33 0.209(7) 0.127(4) 0.065(3) -0.004(3) -0.045(4) 0.026(4) C34 0.049(3) 0.050(3) 0.079(4) -0.006(3) -0.009(3) -0.002(2) F35 0.052(2) 0.086(3) 0.234(5) -0.031(3) -0.018(3) -0.0116(19) F36 0.091(3) 0.074(2) 0.237(5) -0.068(3) -0.019(3) -0.023(2) F37 0.180(5) 0.123(4) 0.117(4) 0.049(3) -0.023(3) 0.059(3) C38 0.065(3) 0.038(2) 0.071(3) 0.012(2) -0.036(3) -0.021(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C38 2.036(4) . ? Pt1 O31 2.132(3) . ? Pt1 N19 2.140(3) . ? Pt1 P1 2.1820(9) . ? P1 C13 1.822(4) . ? P1 C7 1.823(4) . ? P1 C1 1.828(4) . ? C1 C6 1.378(6) . ? C1 C2 1.400(6) . ? C2 C3 1.385(6) . ? C3 C4 1.357(8) . ? C4 C5 1.366(8) . ? C5 C6 1.393(7) . ? C7 C12 1.393(5) . ? C7 C8 1.393(5) . ? C8 C9 1.375(6) . ? C9 C10 1.371(6) . ? C10 C11 1.382(6) . ? C11 C12 1.368(5) . ? C13 C14 1.384(6) . ? C13 C18 1.391(6) . ? C14 C15 1.376(6) . ? C15 C16 1.383(8) . ? C16 C17 1.355(8) . ? C17 C18 1.373(7) . ? N19 C20 1.346(5) . ? N19 C24 1.352(5) . ? C20 C21 1.386(6) . ? C20 C25 1.474(6) . ? C21 C22 1.363(7) . ? C22 C23 1.361(7) . ? C23 C24 1.376(7) . ? C25 C30 1.384(6) . ? C25 C26 1.384(6) . ? C26 C27 1.386(6) . ? C27 C28 1.369(7) . ? C28 C29 1.377(7) . ? C28 C28A 1.511(7) . ? C29 C30 1.385(7) . ? O31 C32 1.195(6) . ? C32 O33 1.221(6) . ? C32 C34 1.517(7) . ? C34 F35 1.291(6) . ? C34 F36 1.293(6) . ? C34 F37 1.304(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C38 Pt1 O31 86.19(15) . . ? C38 Pt1 N19 173.32(14) . . ? O31 Pt1 N19 87.69(13) . . ? C38 Pt1 P1 89.60(12) . . ? O31 Pt1 P1 174.61(10) . . ? N19 Pt1 P1 96.66(8) . . ? C13 P1 C7 102.93(17) . . ? C13 P1 C1 103.20(18) . . ? C7 P1 C1 107.12(17) . . ? C13 P1 Pt1 115.85(12) . . ? C7 P1 Pt1 113.29(12) . . ? C1 P1 Pt1 113.33(13) . . ? C6 C1 C2 118.0(4) . . ? C6 C1 P1 119.3(3) . . ? C2 C1 P1 122.6(3) . . ? C3 C2 C1 120.8(4) . . ? C4 C3 C2 120.1(5) . . ? C3 C4 C5 120.2(5) . . ? C4 C5 C6 120.6(5) . . ? C1 C6 C5 120.2(5) . . ? C12 C7 C8 117.6(3) . . ? C12 C7 P1 122.1(3) . . ? C8 C7 P1 120.3(3) . . ? C9 C8 C7 121.0(4) . . ? C10 C9 C8 120.4(4) . . ? C9 C10 C11 119.5(4) . . ? C12 C11 C10 120.3(4) . . ? C11 C12 C7 121.1(4) . . ? C14 C13 C18 118.8(4) . . ? C14 C13 P1 119.3(3) . . ? C18 C13 P1 121.8(4) . . ? C15 C14 C13 120.6(5) . . ? C14 C15 C16 119.5(6) . . ? C17 C16 C15 120.4(5) . . ? C16 C17 C18 120.6(6) . . ? C17 C18 C13 120.1(5) . . ? C20 N19 C24 118.3(4) . . ? C20 N19 Pt1 126.5(3) . . ? C24 N19 Pt1 115.1(3) . . ? N19 C20 C21 120.1(4) . . ? N19 C20 C25 119.9(4) . . ? C21 C20 C25 120.0(4) . . ? C22 C21 C20 120.9(5) . . ? C23 C22 C21 119.3(5) . . ? C22 C23 C24 118.4(5) . . ? N19 C24 C23 123.1(4) . . ? C30 C25 C26 118.0(4) . . ? C30 C25 C20 118.9(4) . . ? C26 C25 C20 123.0(4) . . ? C25 C26 C27 120.5(4) . . ? C28 C27 C26 121.8(5) . . ? C27 C28 C29 117.5(5) . . ? C27 C28 C28A 121.6(5) . . ? C29 C28 C28A 120.8(5) . . ? C28 C29 C30 121.7(5) . . ? C25 C30 C29 120.5(5) . . ? C32 O31 Pt1 119.1(4) . . ? O31 C32 O33 130.0(6) . . ? O31 C32 C34 117.4(5) . . ? O33 C32 C34 112.6(5) . . ? F35 C34 F36 105.2(4) . . ? F35 C34 F37 107.3(6) . . ? F36 C34 F37 105.5(5) . . ? F35 C34 C32 111.9(5) . . ? F36 C34 C32 113.9(5) . . ? F37 C34 C32 112.5(4) . . ? 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 C38 Pt1 P1 C13 172.9(2) . . . . ? N19 Pt1 P1 C13 -9.45(18) . . . . ? C38 Pt1 P1 C7 -68.48(19) . . . . ? N19 Pt1 P1 C7 109.19(16) . . . . ? C38 Pt1 P1 C1 53.84(19) . . . . ? N19 Pt1 P1 C1 -128.49(16) . . . . ? C13 P1 C1 C6 -104.4(4) . . . . ? C7 P1 C1 C6 147.4(3) . . . . ? Pt1 P1 C1 C6 21.7(4) . . . . ? C13 P1 C1 C2 71.9(4) . . . . ? C7 P1 C1 C2 -36.4(4) . . . . ? Pt1 P1 C1 C2 -162.1(3) . . . . ? C6 C1 C2 C3 -0.2(7) . . . . ? P1 C1 C2 C3 -176.5(4) . . . . ? C1 C2 C3 C4 -0.7(8) . . . . ? C2 C3 C4 C5 0.5(9) . . . . ? C3 C4 C5 C6 0.6(9) . . . . ? C2 C1 C6 C5 1.3(7) . . . . ? P1 C1 C6 C5 177.7(4) . . . . ? C4 C5 C6 C1 -1.5(8) . . . . ? C13 P1 C7 C12 -39.4(4) . . . . ? C1 P1 C7 C12 69.1(4) . . . . ? Pt1 P1 C7 C12 -165.2(3) . . . . ? C13 P1 C7 C8 139.3(3) . . . . ? C1 P1 C7 C8 -112.3(3) . . . . ? Pt1 P1 C7 C8 13.4(4) . . . . ? C12 C7 C8 C9 -2.7(6) . . . . ? P1 C7 C8 C9 178.6(3) . . . . ? C7 C8 C9 C10 0.6(7) . . . . ? C8 C9 C10 C11 1.3(7) . . . . ? C9 C10 C11 C12 -1.1(7) . . . . ? C10 C11 C12 C7 -1.0(6) . . . . ? C8 C7 C12 C11 2.9(6) . . . . ? P1 C7 C12 C11 -178.4(3) . . . . ? C7 P1 C13 C14 -53.3(3) . . . . ? C1 P1 C13 C14 -164.7(3) . . . . ? Pt1 P1 C13 C14 70.9(3) . . . . ? C7 P1 C13 C18 129.0(4) . . . . ? C1 P1 C13 C18 17.6(4) . . . . ? Pt1 P1 C13 C18 -106.8(3) . . . . ? C18 C13 C14 C15 0.3(6) . . . . ? P1 C13 C14 C15 -177.4(4) . . . . ? C13 C14 C15 C16 -0.8(7) . . . . ? C14 C15 C16 C17 0.8(9) . . . . ? C15 C16 C17 C18 -0.3(9) . . . . ? C16 C17 C18 C13 -0.2(9) . . . . ? C14 C13 C18 C17 0.1(7) . . . . ? P1 C13 C18 C17 177.8(4) . . . . ? O31 Pt1 N19 C20 -94.1(3) . . . . ? P1 Pt1 N19 C20 82.7(3) . . . . ? O31 Pt1 N19 C24 90.1(3) . . . . ? P1 Pt1 N19 C24 -93.1(3) . . . . ? C24 N19 C20 C21 -0.4(6) . . . . ? Pt1 N19 C20 C21 -176.1(3) . . . . ? C24 N19 C20 C25 -178.9(4) . . . . ? Pt1 N19 C20 C25 5.4(5) . . . . ? N19 C20 C21 C22 1.2(8) . . . . ? C25 C20 C21 C22 179.7(5) . . . . ? C20 C21 C22 C23 -0.6(9) . . . . ? C21 C22 C23 C24 -0.7(8) . . . . ? C20 N19 C24 C23 -0.9(6) . . . . ? Pt1 N19 C24 C23 175.3(3) . . . . ? C22 C23 C24 N19 1.4(7) . . . . ? N19 C20 C25 C30 -137.0(4) . . . . ? C21 C20 C25 C30 44.5(6) . . . . ? N19 C20 C25 C26 46.7(6) . . . . ? C21 C20 C25 C26 -131.8(5) . . . . ? C30 C25 C26 C27 -1.0(7) . . . . ? C20 C25 C26 C27 175.4(4) . . . . ? C25 C26 C27 C28 -0.2(7) . . . . ? C26 C27 C28 C29 1.7(8) . . . . ? C26 C27 C28 C28A -176.8(5) . . . . ? C27 C28 C29 C30 -2.2(8) . . . . ? C28A C28 C29 C30 176.4(5) . . . . ? C26 C25 C30 C29 0.6(7) . . . . ? C20 C25 C30 C29 -175.9(4) . . . . ? C28 C29 C30 C25 1.0(8) . . . . ? C38 Pt1 O31 C32 92.0(4) . . . . ? N19 Pt1 O31 C32 -85.3(4) . . . . ? Pt1 O31 C32 O33 -0.6(10) . . . . ? Pt1 O31 C32 C34 177.3(4) . . . . ? O31 C32 C34 F35 -110.8(6) . . . . ? O33 C32 C34 F35 67.4(8) . . . . ? O31 C32 C34 F36 130.0(6) . . . . ? O33 C32 C34 F36 -51.7(8) . . . . ? O31 C32 C34 F37 10.1(8) . . . . ? O33 C32 C34 F37 -171.7(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 F37 0.93 2.70 3.624(7) 172.0 2_556 C24 H24 O33 0.93 2.54 3.068(6) 116.6 2_655 _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.657 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 919438'