# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yun Chi' _publ_contact_author_email YCHI@MX.NTHU.EDU.TW _publ_section_title ; Emissive Pt(II) Complexes Bearing both Cyclometalated Ligand and 2-Pyridyl Hexafluoropropoxide Ancillary Chelate ; loop_ _publ_author_name 'Yun Chi.' 'Sheng-Yuan Chang.' 'Pi-Tai Chou.' 'Chang-Ming Jiang.' ; Gene-Hsiang Lee ; 'Yi-Chih Lin.' # Attachment 'X-ray.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 689096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H12 F6 N2 O Pt' _chemical_formula_weight 593.40 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.2684(4) _cell_length_b 15.7447(10) _cell_length_c 15.5024(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.748(1) _cell_angle_gamma 90.00 _cell_volume 1772.04(18) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3793 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 24.54 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 7.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2399 _exptl_absorpt_correction_T_max 0.5020 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17608 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0405 _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 -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4076 _reflns_number_gt 3489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0207P)^2^+0.2037P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00150(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4076 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 Pt Pt 0.86473(2) 0.368646(9) 0.549619(10) 0.02939(7) Uani 1 1 d . . . O1 O 0.8602(4) 0.28793(17) 0.44319(17) 0.0390(7) Uani 1 1 d . . . N1 N 0.9866(5) 0.2636(2) 0.6031(2) 0.0322(8) Uani 1 1 d . . . N2 N 0.7615(4) 0.4681(2) 0.4846(2) 0.0304(7) Uani 1 1 d . . . C1 C 1.0855(6) 0.2610(3) 0.6785(3) 0.0415(11) Uani 1 1 d . . . H1A H 1.0925 0.3099 0.7122 0.050 Uiso 1 1 calc R . . C2 C 1.1769(7) 0.1896(3) 0.7084(3) 0.0507(13) Uani 1 1 d . . . H2A H 1.2427 0.1902 0.7613 0.061 Uiso 1 1 calc R . . C3 C 1.1693(8) 0.1173(3) 0.6587(3) 0.0565(14) Uani 1 1 d . . . H3A H 1.2298 0.0681 0.6771 0.068 Uiso 1 1 calc R . . C4 C 1.0702(7) 0.1196(3) 0.5811(3) 0.0499(13) Uani 1 1 d . . . H4A H 1.0620 0.0711 0.5469 0.060 Uiso 1 1 calc R . . C5 C 0.9831(6) 0.1928(3) 0.5536(3) 0.0363(10) Uani 1 1 d . . . C6 C 0.8818(6) 0.2046(2) 0.4648(3) 0.0363(10) Uani 1 1 d . . . C7 C 0.6909(8) 0.1621(3) 0.4666(3) 0.0513(13) Uani 1 1 d . . . C8 C 0.9944(8) 0.1638(3) 0.3935(3) 0.0478(12) Uani 1 1 d . . . C9 C 0.7072(6) 0.4644(3) 0.4001(3) 0.0405(10) Uani 1 1 d . . . H9A H 0.7198 0.4136 0.3704 0.049 Uiso 1 1 calc R . . C10 C 0.6343(6) 0.5335(3) 0.3572(3) 0.0423(11) Uani 1 1 d . . . H10A H 0.6000 0.5297 0.2987 0.051 Uiso 1 1 calc R . . C11 C 0.6120(6) 0.6082(3) 0.4009(3) 0.0462(12) Uani 1 1 d . . . H11A H 0.5588 0.6551 0.3731 0.055 Uiso 1 1 calc R . . C12 C 0.6697(6) 0.6125(3) 0.4865(3) 0.0400(10) Uani 1 1 d . . . H12A H 0.6579 0.6631 0.5166 0.048 Uiso 1 1 calc R . . C13 C 0.7451(5) 0.5423(2) 0.5280(3) 0.0327(9) Uani 1 1 d . . . C14 C 0.8005(6) 0.5344(3) 0.6196(3) 0.0353(10) Uani 1 1 d . . . C15 C 0.7923(7) 0.6016(3) 0.6777(3) 0.0492(12) Uani 1 1 d . . . H15A H 0.7641 0.6560 0.6578 0.059 Uiso 1 1 calc R . . C16 C 0.8261(7) 0.5871(3) 0.7648(3) 0.0573(14) Uani 1 1 d . . . H16A H 0.8243 0.6320 0.8038 0.069 Uiso 1 1 calc R . . C17 C 0.8622(7) 0.5064(4) 0.7932(3) 0.0565(13) Uani 1 1 d . . . H17A H 0.8789 0.4960 0.8522 0.068 Uiso 1 1 calc R . . C18 C 0.8742(6) 0.4401(3) 0.7358(3) 0.0452(11) Uani 1 1 d . . . H18A H 0.8988 0.3859 0.7571 0.054 Uiso 1 1 calc R . . C19 C 0.8508(5) 0.4515(3) 0.6462(3) 0.0331(9) Uani 1 1 d . . . F1 F 0.5907(4) 0.1976(2) 0.5270(2) 0.0694(9) Uani 1 1 d . . . F2 F 0.5956(5) 0.1694(3) 0.3920(2) 0.0871(11) Uani 1 1 d . . . F3 F 0.6973(5) 0.07878(19) 0.4857(2) 0.0745(9) Uani 1 1 d . . . F4 F 0.9305(5) 0.18477(19) 0.31522(17) 0.0693(9) Uani 1 1 d . . . F5 F 0.9991(5) 0.07875(16) 0.39576(19) 0.0683(9) Uani 1 1 d . . . F6 F 1.1699(4) 0.18958(19) 0.4012(2) 0.0675(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.03198(10) 0.02859(9) 0.02724(10) 0.00207(6) -0.00233(6) -0.00046(6) O1 0.060(2) 0.0299(15) 0.0265(16) 0.0013(12) -0.0056(14) 0.0075(13) N1 0.035(2) 0.0308(18) 0.0298(19) 0.0021(14) -0.0045(15) -0.0028(14) N2 0.0274(18) 0.0317(17) 0.0320(19) 0.0045(14) -0.0003(14) -0.0017(14) C1 0.048(3) 0.040(2) 0.034(3) 0.0027(19) -0.014(2) -0.003(2) C2 0.059(3) 0.045(3) 0.046(3) 0.010(2) -0.022(2) -0.003(2) C3 0.071(4) 0.041(3) 0.055(3) 0.015(2) -0.020(3) 0.008(2) C4 0.066(3) 0.035(3) 0.047(3) 0.003(2) -0.015(3) 0.004(2) C5 0.043(3) 0.032(2) 0.034(2) 0.0036(18) -0.0078(19) -0.0031(18) C6 0.047(3) 0.029(2) 0.032(2) 0.0016(17) -0.0074(19) 0.0007(18) C7 0.062(3) 0.052(3) 0.038(3) 0.003(2) -0.016(3) -0.009(3) C8 0.068(4) 0.034(2) 0.041(3) 0.001(2) 0.000(2) 0.008(2) C9 0.047(3) 0.042(3) 0.032(2) 0.0017(19) -0.001(2) 0.005(2) C10 0.041(3) 0.053(3) 0.033(2) 0.012(2) -0.002(2) 0.000(2) C11 0.036(3) 0.049(3) 0.054(3) 0.019(2) 0.004(2) 0.006(2) C12 0.037(3) 0.033(2) 0.050(3) 0.004(2) 0.004(2) 0.0023(18) C13 0.029(2) 0.032(2) 0.037(2) 0.0020(18) 0.0037(18) -0.0028(17) C14 0.031(2) 0.038(2) 0.038(3) -0.0013(19) 0.0066(19) -0.0039(17) C15 0.055(3) 0.041(2) 0.051(3) -0.006(2) 0.007(2) -0.004(2) C16 0.068(4) 0.062(3) 0.042(3) -0.023(3) 0.003(3) -0.005(3) C17 0.064(4) 0.075(4) 0.031(3) -0.007(3) -0.001(2) 0.002(3) C18 0.054(3) 0.050(3) 0.032(3) 0.005(2) 0.003(2) 0.007(2) C19 0.030(2) 0.041(2) 0.029(2) -0.0024(18) 0.0019(18) -0.0033(18) F1 0.0532(19) 0.085(2) 0.071(2) -0.0039(17) 0.0089(16) -0.0057(16) F2 0.082(2) 0.118(3) 0.058(2) 0.012(2) -0.0371(18) -0.036(2) F3 0.082(2) 0.0477(18) 0.093(2) 0.0065(17) -0.0024(19) -0.0239(16) F4 0.110(3) 0.066(2) 0.0308(16) -0.0037(14) -0.0021(16) 0.0258(18) F5 0.110(3) 0.0313(15) 0.064(2) -0.0076(13) 0.0084(18) 0.0146(15) F6 0.067(2) 0.067(2) 0.070(2) -0.0042(16) 0.0197(17) 0.0034(16) _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 Pt N2 1.989(3) . ? Pt C19 1.992(4) . ? Pt N1 2.033(3) . ? Pt O1 2.082(3) . ? O1 C6 1.361(4) . ? N1 C1 1.343(5) . ? N1 C5 1.353(5) . ? N2 C9 1.351(5) . ? N2 C13 1.357(5) . ? C1 C2 1.375(6) . ? C2 C3 1.374(7) . ? C3 C4 1.372(7) . ? C4 C5 1.373(6) . ? C5 C6 1.542(5) . ? C6 C7 1.542(7) . ? C6 C8 1.546(6) . ? C7 F2 1.324(5) . ? C7 F1 1.337(6) . ? C7 F3 1.345(6) . ? C8 F4 1.320(5) . ? C8 F5 1.340(5) . ? C8 F6 1.339(6) . ? C9 C10 1.369(6) . ? C10 C11 1.372(6) . ? C11 C12 1.373(7) . ? C12 C13 1.380(6) . ? C13 C14 1.462(6) . ? C14 C15 1.393(6) . ? C14 C19 1.412(6) . ? C15 C16 1.380(7) . ? C16 C17 1.368(7) . ? C17 C18 1.377(6) . ? C18 C19 1.402(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt C19 80.44(15) . . ? N2 Pt N1 173.13(13) . . ? C19 Pt N1 105.22(15) . . ? N2 Pt O1 95.03(12) . . ? C19 Pt O1 174.94(14) . . ? N1 Pt O1 79.45(12) . . ? C6 O1 Pt 113.3(2) . . ? C1 N1 C5 117.6(4) . . ? C1 N1 Pt 125.8(3) . . ? C5 N1 Pt 116.3(3) . . ? C9 N2 C13 119.3(3) . . ? C9 N2 Pt 122.9(3) . . ? C13 N2 Pt 117.8(3) . . ? N1 C1 C2 123.2(4) . . ? C3 C2 C1 118.9(4) . . ? C4 C3 C2 118.4(4) . . ? C5 C4 C3 120.6(4) . . ? N1 C5 C4 121.3(4) . . ? N1 C5 C6 113.7(3) . . ? C4 C5 C6 124.9(4) . . ? O1 C6 C5 112.4(3) . . ? O1 C6 C7 109.3(4) . . ? C5 C6 C7 108.9(4) . . ? O1 C6 C8 106.4(3) . . ? C5 C6 C8 110.0(4) . . ? C7 C6 C8 109.9(4) . . ? F2 C7 F1 107.2(5) . . ? F2 C7 F3 106.8(4) . . ? F1 C7 F3 105.5(4) . . ? F2 C7 C6 112.3(4) . . ? F1 C7 C6 110.6(4) . . ? F3 C7 C6 114.0(4) . . ? F4 C8 F5 106.3(4) . . ? F4 C8 F6 107.4(4) . . ? F5 C8 F6 106.1(4) . . ? F4 C8 C6 112.2(4) . . ? F5 C8 C6 114.2(4) . . ? F6 C8 C6 110.2(4) . . ? N2 C9 C10 121.7(4) . . ? C9 C10 C11 119.6(4) . . ? C10 C11 C12 118.8(4) . . ? C11 C12 C13 120.5(4) . . ? N2 C13 C12 120.1(4) . . ? N2 C13 C14 112.4(3) . . ? C12 C13 C14 127.3(4) . . ? C15 C14 C19 122.2(4) . . ? C15 C14 C13 123.0(4) . . ? C19 C14 C13 114.7(4) . . ? C16 C15 C14 119.7(5) . . ? C17 C16 C15 119.4(5) . . ? C16 C17 C18 120.9(5) . . ? C17 C18 C19 122.4(4) . . ? C18 C19 C14 115.1(4) . . ? C18 C19 Pt 130.8(3) . . ? C14 C19 Pt 114.1(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.685 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.111 data_2a _database_code_depnum_ccdc_archive 'CCDC 689097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H12 F6 N2 O Pt' _chemical_formula_weight 617.42 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.2213(12) _cell_length_b 7.2387(6) _cell_length_c 16.4625(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.989(2) _cell_angle_gamma 90.00 _cell_volume 1867.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2998 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 22.84 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 7.590 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.1709 _exptl_absorpt_correction_T_max 0.8630 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13984 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4291 _reflns_number_gt 3572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0538P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4291 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _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 Pt Pt 0.049634(17) 0.82994(4) 0.161093(17) 0.02538(13) Uani 1 1 d . . . O1 O 0.0222(4) 0.8921(8) 0.2722(4) 0.0381(13) Uani 1 1 d . . . N1 N -0.0796(4) 0.8387(8) 0.1233(5) 0.0298(14) Uani 1 1 d . . . N2 N 0.1756(4) 0.8286(8) 0.2111(4) 0.0278(14) Uani 1 1 d . . . C1 C 0.0869(5) 0.7611(9) 0.0581(5) 0.0256(15) Uani 1 1 d . . . C2 C 0.0439(6) 0.7030(11) -0.0219(6) 0.0367(19) Uani 1 1 d . . . H2 H -0.0165 0.6936 -0.0358 0.044 Uiso 1 1 calc R . . C3 C 0.0869(6) 0.6573(12) -0.0833(6) 0.043(2) Uani 1 1 d . . . H3 H 0.0548 0.6208 -0.1377 0.052 Uiso 1 1 calc R . . C4 C 0.1737(6) 0.6643(11) -0.0665(6) 0.041(2) Uani 1 1 d . . . H4 H 0.2013 0.6354 -0.1093 0.049 Uiso 1 1 calc R . . C5 C 0.2222(5) 0.7141(10) 0.0138(6) 0.0308(17) Uani 1 1 d . . . C6 C 0.3142(6) 0.7193(12) 0.0384(6) 0.039(2) Uani 1 1 d . . . H6 H 0.3451 0.6930 -0.0020 0.047 Uiso 1 1 calc R . . C7 C 0.3573(5) 0.7613(12) 0.1187(6) 0.040(2) Uani 1 1 d . . . H7 H 0.4179 0.7663 0.1333 0.048 Uiso 1 1 calc R . . C8 C 0.3125(5) 0.7980(10) 0.1813(6) 0.0319(18) Uani 1 1 d . . . C9 C 0.2248(5) 0.8005(9) 0.1574(5) 0.0294(17) Uani 1 1 d . . . C10 C 0.1768(5) 0.7612(9) 0.0736(5) 0.0253(15) Uani 1 1 d . . . C11 C 0.3519(6) 0.8269(10) 0.2670(6) 0.040(2) Uani 1 1 d . . . H11 H 0.4123 0.8253 0.2869 0.047 Uiso 1 1 calc R . . C12 C 0.3026(6) 0.8574(10) 0.3217(6) 0.043(2) Uani 1 1 d . . . H12 H 0.3288 0.8796 0.3795 0.052 Uiso 1 1 calc R . . C13 C 0.2139(6) 0.8561(10) 0.2927(5) 0.0352(19) Uani 1 1 d . . . H13 H 0.1801 0.8748 0.3313 0.042 Uiso 1 1 calc R . . C14 C -0.1265(5) 0.8486(10) 0.0440(6) 0.0334(18) Uani 1 1 d . . . H14 H -0.0982 0.8590 0.0004 0.040 Uiso 1 1 calc R . . C15 C -0.2146(6) 0.8444(10) 0.0226(6) 0.041(2) Uani 1 1 d . . . H15 H -0.2464 0.8526 -0.0345 0.049 Uiso 1 1 calc R . . C16 C -0.2556(6) 0.8278(11) 0.0864(7) 0.046(2) Uani 1 1 d . . . H16 H -0.3160 0.8178 0.0736 0.055 Uiso 1 1 calc R . . C17 C -0.2072(6) 0.8260(11) 0.1688(6) 0.041(2) Uani 1 1 d . . . H17 H -0.2340 0.8178 0.2136 0.049 Uiso 1 1 calc R . . C18 C -0.1195(5) 0.8364(9) 0.1854(6) 0.0336(18) Uani 1 1 d . . . C19 C -0.0587(5) 0.8492(10) 0.2744(5) 0.0312(17) Uani 1 1 d . . . C20 C -0.0894(6) 1.0042(12) 0.3233(6) 0.045(2) Uani 1 1 d . . . C21 C -0.0576(7) 0.6627(12) 0.3200(6) 0.044(2) Uani 1 1 d . . . F1 F -0.0997(5) 1.1584(6) 0.2803(4) 0.0638(18) Uani 1 1 d . . . F2 F -0.1652(3) 0.9671(7) 0.3397(4) 0.0563(15) Uani 1 1 d . . . F3 F -0.0349(4) 1.0374(8) 0.3963(4) 0.0573(15) Uani 1 1 d . . . F4 F -0.1355(4) 0.6080(8) 0.3251(4) 0.0675(18) Uani 1 1 d . . . F5 F -0.0096(5) 0.6678(7) 0.3976(4) 0.0692(19) Uani 1 1 d . . . F6 F -0.0278(4) 0.5319(7) 0.2804(3) 0.0594(16) 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 Pt 0.02289(19) 0.02952(17) 0.02634(19) -0.00028(11) 0.01106(12) -0.00035(11) O1 0.030(3) 0.055(3) 0.033(3) -0.010(3) 0.016(3) -0.007(3) N1 0.021(3) 0.031(3) 0.040(4) -0.002(3) 0.014(3) 0.002(2) N2 0.023(3) 0.032(3) 0.029(4) 0.000(3) 0.009(3) 0.000(2) C1 0.020(4) 0.025(3) 0.031(4) 0.000(3) 0.007(3) -0.003(3) C2 0.028(5) 0.043(4) 0.039(5) -0.002(4) 0.008(4) 0.002(3) C3 0.043(6) 0.059(5) 0.028(5) -0.007(4) 0.009(4) 0.006(4) C4 0.043(5) 0.050(5) 0.034(5) 0.000(4) 0.018(4) 0.015(4) C5 0.024(4) 0.033(4) 0.041(5) 0.000(3) 0.018(4) 0.002(3) C6 0.036(5) 0.047(4) 0.040(5) 0.000(4) 0.021(4) 0.006(4) C7 0.017(4) 0.048(4) 0.056(6) 0.001(4) 0.013(4) -0.001(3) C8 0.023(4) 0.030(4) 0.042(5) -0.003(3) 0.006(4) -0.002(3) C9 0.034(5) 0.026(3) 0.029(4) 0.006(3) 0.010(4) 0.003(3) C10 0.027(4) 0.027(3) 0.023(4) 0.006(3) 0.009(3) 0.004(3) C11 0.029(5) 0.036(4) 0.050(6) -0.004(4) 0.005(4) 0.000(3) C12 0.042(6) 0.036(4) 0.044(5) -0.005(4) -0.003(4) -0.001(4) C13 0.042(5) 0.034(4) 0.027(4) -0.004(3) 0.004(4) -0.002(3) C14 0.028(4) 0.033(4) 0.041(5) 0.002(3) 0.014(4) 0.005(3) C15 0.032(5) 0.038(4) 0.050(6) 0.004(4) 0.004(4) 0.006(3) C16 0.029(5) 0.046(5) 0.067(7) 0.007(4) 0.020(5) 0.006(4) C17 0.034(5) 0.049(5) 0.048(6) -0.006(4) 0.025(4) -0.007(4) C18 0.030(4) 0.030(4) 0.044(5) 0.002(3) 0.016(4) 0.000(3) C19 0.030(4) 0.033(4) 0.036(4) -0.005(3) 0.018(4) -0.001(3) C20 0.053(6) 0.039(4) 0.055(6) -0.006(4) 0.037(5) -0.002(4) C21 0.058(7) 0.041(5) 0.038(5) -0.001(4) 0.022(5) -0.003(4) F1 0.097(5) 0.033(3) 0.073(4) -0.001(2) 0.043(4) 0.003(3) F2 0.050(3) 0.065(3) 0.067(4) -0.015(3) 0.040(3) -0.007(3) F3 0.063(4) 0.067(4) 0.050(3) -0.029(3) 0.028(3) -0.015(3) F4 0.065(4) 0.057(3) 0.091(5) 0.026(3) 0.038(4) -0.011(3) F5 0.095(6) 0.066(4) 0.042(4) 0.010(3) 0.008(4) -0.006(3) F6 0.090(5) 0.037(3) 0.053(3) 0.000(2) 0.023(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N2 1.996(7) . ? Pt C1 2.005(8) . ? Pt N1 2.028(7) . ? Pt O1 2.042(6) . ? O1 C19 1.358(9) . ? N1 C14 1.331(11) . ? N1 C18 1.344(11) . ? N2 C13 1.342(10) . ? N2 C9 1.349(10) . ? C1 C2 1.387(11) . ? C1 C10 1.414(10) . ? C2 C3 1.408(13) . ? C3 C4 1.364(14) . ? C4 C5 1.399(13) . ? C5 C10 1.415(10) . ? C5 C6 1.442(12) . ? C6 C7 1.359(13) . ? C7 C8 1.431(12) . ? C8 C9 1.375(12) . ? C8 C11 1.406(13) . ? C9 C10 1.427(11) . ? C11 C12 1.368(14) . ? C12 C13 1.394(13) . ? C14 C15 1.382(12) . ? C15 C16 1.384(14) . ? C16 C17 1.381(14) . ? C17 C18 1.380(12) . ? C18 C19 1.544(12) . ? C19 C20 1.537(11) . ? C19 C21 1.542(11) . ? C20 F1 1.309(10) . ? C20 F3 1.316(11) . ? C20 F2 1.353(10) . ? C21 F6 1.311(10) . ? C21 F5 1.314(12) . ? C21 F4 1.349(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt C1 81.2(3) . . ? N2 Pt N1 173.6(3) . . ? C1 Pt N1 105.2(3) . . ? N2 Pt O1 94.0(2) . . ? C1 Pt O1 174.8(3) . . ? N1 Pt O1 79.7(3) . . ? C19 O1 Pt 114.2(5) . . ? C14 N1 C18 118.7(7) . . ? C14 N1 Pt 125.9(6) . . ? C18 N1 Pt 115.4(6) . . ? C13 N2 C9 118.7(7) . . ? C13 N2 Pt 124.8(6) . . ? C9 N2 Pt 116.5(6) . . ? C2 C1 C10 114.4(7) . . ? C2 C1 Pt 133.8(6) . . ? C10 C1 Pt 111.7(5) . . ? C1 C2 C3 122.2(8) . . ? C4 C3 C2 121.5(9) . . ? C3 C4 C5 120.0(8) . . ? C4 C5 C10 116.9(8) . . ? C4 C5 C6 124.1(8) . . ? C10 C5 C6 119.0(8) . . ? C7 C6 C5 120.9(8) . . ? C6 C7 C8 120.8(8) . . ? C9 C8 C11 116.9(8) . . ? C9 C8 C7 118.5(8) . . ? C11 C8 C7 124.6(8) . . ? N2 C9 C8 123.9(8) . . ? N2 C9 C10 113.4(7) . . ? C8 C9 C10 122.6(8) . . ? C1 C10 C5 125.0(7) . . ? C1 C10 C9 117.0(7) . . ? C5 C10 C9 118.0(7) . . ? C12 C11 C8 119.6(8) . . ? C11 C12 C13 120.0(9) . . ? N2 C13 C12 120.9(8) . . ? N1 C14 C15 122.7(8) . . ? C14 C15 C16 118.4(9) . . ? C17 C16 C15 118.9(9) . . ? C18 C17 C16 119.2(9) . . ? N1 C18 C17 121.7(8) . . ? N1 C18 C19 114.0(7) . . ? C17 C18 C19 124.3(8) . . ? O1 C19 C20 107.0(6) . . ? O1 C19 C21 108.8(7) . . ? C20 C19 C21 110.4(7) . . ? O1 C19 C18 111.9(7) . . ? C20 C19 C18 109.1(7) . . ? C21 C19 C18 109.5(7) . . ? F1 C20 F3 107.4(8) . . ? F1 C20 F2 106.4(8) . . ? F3 C20 F2 106.5(7) . . ? F1 C20 C19 110.7(7) . . ? F3 C20 C19 112.3(8) . . ? F2 C20 C19 113.2(7) . . ? F6 C21 F5 107.6(8) . . ? F6 C21 F4 107.0(8) . . ? F5 C21 F4 106.0(8) . . ? F6 C21 C19 110.5(7) . . ? F5 C21 C19 112.2(7) . . ? F4 C21 C19 113.2(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.783 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.292 data_4a _database_code_depnum_ccdc_archive 'CCDC 689098' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H13 F6 N3 O Pt' _chemical_formula_weight 644.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' _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 7.3387(7) _cell_length_b 11.4663(11) _cell_length_c 12.3233(12) _cell_angle_alpha 99.759(2) _cell_angle_beta 98.064(2) _cell_angle_gamma 99.111(2) _cell_volume 994.09(17) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5805 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.34 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 7.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1415 _exptl_absorpt_correction_T_max 0.5991 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12850 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4546 _reflns_number_gt 4297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0198P)^2^+0.0461P] 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 4546 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0516 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.004 _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 Pt Pt 0.253529(16) 0.293364(11) 0.865324(9) 0.02408(5) Uani 1 1 d . . . O1 O 0.2658(4) 0.2076(2) 0.7074(2) 0.0375(6) Uani 1 1 d . . . N1 N 0.2265(4) 0.1430(2) 0.9273(2) 0.0259(6) Uani 1 1 d . . . N2 N 0.2358(4) -0.0650(3) 0.8983(2) 0.0332(6) Uani 1 1 d . . . N3 N 0.2977(4) 0.4364(3) 0.7892(2) 0.0270(6) Uani 1 1 d . . . C1 C 0.2199(4) 0.3591(3) 1.0198(3) 0.0250(6) Uani 1 1 d . . . C2 C 0.1931(5) 0.4742(3) 1.0668(3) 0.0309(7) Uani 1 1 d . . . H2 H 0.2026 0.5353 1.0234 0.037 Uiso 1 1 calc R . . C3 C 0.1540(5) 0.5023(3) 1.1728(3) 0.0332(8) Uani 1 1 d . . . H3 H 0.1411 0.5822 1.2018 0.040 Uiso 1 1 calc R . . C4 C 0.1330(5) 0.4157(3) 1.2378(3) 0.0326(8) Uani 1 1 d . . . H4 H 0.1048 0.4356 1.3109 0.039 Uiso 1 1 calc R . . C5 C 0.1536(5) 0.2998(3) 1.1956(3) 0.0298(7) Uani 1 1 d . . . H5 H 0.1347 0.2388 1.2385 0.036 Uiso 1 1 calc R . . C6 C 0.2022(4) 0.2724(3) 1.0896(3) 0.0238(6) Uani 1 1 d . . . C7 C 0.2271(4) 0.1532(3) 1.0374(3) 0.0247(6) Uani 1 1 d . . . C8 C 0.2546(4) 0.0515(3) 1.0863(3) 0.0265(7) Uani 1 1 d . . . C9 C 0.2954(5) 0.0532(3) 1.2023(3) 0.0344(8) Uani 1 1 d . . . H9 H 0.3044 0.1264 1.2539 0.041 Uiso 1 1 calc R . . C10 C 0.3219(5) -0.0481(4) 1.2413(3) 0.0415(9) Uani 1 1 d . . . H10 H 0.3500 -0.0450 1.3195 0.050 Uiso 1 1 calc R . . C11 C 0.3080(5) -0.1564(3) 1.1668(3) 0.0417(9) Uani 1 1 d . . . H11 H 0.3224 -0.2273 1.1948 0.050 Uiso 1 1 calc R . . C12 C 0.2742(5) -0.1618(3) 1.0547(3) 0.0380(8) Uani 1 1 d . . . H12 H 0.2651 -0.2362 1.0049 0.046 Uiso 1 1 calc R . . C13 C 0.2524(5) -0.0573(3) 1.0119(3) 0.0289(7) Uani 1 1 d . . . C14 C 0.2298(5) 0.0349(3) 0.8629(3) 0.0312(7) Uani 1 1 d . . . H14 H 0.2276 0.0323 0.7853 0.037 Uiso 1 1 calc R . . C15 C 0.3456(5) 0.5524(3) 0.8395(3) 0.0316(7) Uani 1 1 d . . . H15 H 0.3732 0.5717 0.9188 0.038 Uiso 1 1 calc R . . C16 C 0.3566(5) 0.6453(3) 0.7813(3) 0.0365(8) Uani 1 1 d . . . H16 H 0.3879 0.7268 0.8199 0.044 Uiso 1 1 calc R . . C17 C 0.3215(5) 0.6178(4) 0.6661(3) 0.0402(9) Uani 1 1 d . . . H17 H 0.3244 0.6800 0.6239 0.048 Uiso 1 1 calc R . . C18 C 0.2823(5) 0.4986(4) 0.6131(3) 0.0380(9) Uani 1 1 d . . . H18 H 0.2628 0.4780 0.5338 0.046 Uiso 1 1 calc R . . C19 C 0.2714(4) 0.4087(3) 0.6757(3) 0.0295(7) Uani 1 1 d . . . C20 C 0.2358(5) 0.2734(3) 0.6273(3) 0.0316(8) Uani 1 1 d . . . C21 C 0.0321(5) 0.2340(4) 0.5654(3) 0.0417(9) Uani 1 1 d . . . C22 C 0.3739(6) 0.2474(4) 0.5464(3) 0.0476(10) Uani 1 1 d . . . F1 F -0.0858(3) 0.2525(3) 0.6358(2) 0.0637(7) Uani 1 1 d . . . F2 F -0.0084(4) 0.1188(2) 0.5181(2) 0.0717(8) Uani 1 1 d . . . F3 F -0.0109(4) 0.2943(3) 0.4842(2) 0.0703(8) Uani 1 1 d . . . F4 F 0.5475(3) 0.2980(3) 0.5941(2) 0.0736(9) Uani 1 1 d . . . F5 F 0.3405(4) 0.2897(3) 0.45110(18) 0.0611(7) Uani 1 1 d . . . F6 F 0.3692(4) 0.1304(3) 0.5152(2) 0.0694(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.02965(8) 0.02496(8) 0.01989(7) 0.00633(5) 0.00529(5) 0.00882(5) O1 0.0587(16) 0.0361(14) 0.0244(12) 0.0093(11) 0.0117(11) 0.0213(13) N1 0.0310(14) 0.0225(14) 0.0242(14) 0.0035(11) 0.0049(11) 0.0061(11) N2 0.0451(17) 0.0237(15) 0.0314(15) 0.0025(12) 0.0105(13) 0.0077(13) N3 0.0283(14) 0.0340(16) 0.0224(13) 0.0114(12) 0.0051(11) 0.0104(12) C1 0.0249(15) 0.0267(17) 0.0230(15) 0.0044(13) 0.0027(12) 0.0055(13) C2 0.0353(18) 0.0265(18) 0.0323(18) 0.0075(14) 0.0082(14) 0.0063(14) C3 0.0338(18) 0.0270(18) 0.038(2) 0.0007(15) 0.0093(15) 0.0068(15) C4 0.0354(18) 0.038(2) 0.0247(17) 0.0008(15) 0.0084(14) 0.0095(15) C5 0.0313(17) 0.0314(18) 0.0273(17) 0.0083(14) 0.0052(14) 0.0051(14) C6 0.0214(15) 0.0268(17) 0.0228(15) 0.0056(13) 0.0019(12) 0.0041(12) C7 0.0252(15) 0.0251(16) 0.0244(15) 0.0072(13) 0.0043(12) 0.0039(12) C8 0.0240(15) 0.0254(17) 0.0311(17) 0.0095(14) 0.0053(13) 0.0031(13) C9 0.045(2) 0.0286(18) 0.0315(18) 0.0110(15) 0.0041(15) 0.0087(16) C10 0.047(2) 0.040(2) 0.041(2) 0.0180(18) 0.0052(17) 0.0121(18) C11 0.043(2) 0.034(2) 0.056(2) 0.0251(19) 0.0104(18) 0.0115(17) C12 0.044(2) 0.0237(18) 0.050(2) 0.0105(16) 0.0127(17) 0.0101(15) C13 0.0274(16) 0.0265(17) 0.0340(18) 0.0072(14) 0.0069(14) 0.0055(13) C14 0.0389(19) 0.0295(18) 0.0264(17) 0.0029(14) 0.0096(14) 0.0090(15) C15 0.0273(17) 0.0347(19) 0.0338(18) 0.0096(15) 0.0057(14) 0.0055(14) C16 0.0321(18) 0.035(2) 0.047(2) 0.0186(17) 0.0120(16) 0.0051(15) C17 0.0340(19) 0.044(2) 0.049(2) 0.0267(19) 0.0081(17) 0.0050(17) C18 0.039(2) 0.051(2) 0.0316(19) 0.0229(18) 0.0082(15) 0.0124(17) C19 0.0249(16) 0.039(2) 0.0294(17) 0.0139(15) 0.0068(13) 0.0094(14) C20 0.0366(18) 0.041(2) 0.0211(16) 0.0080(14) 0.0061(14) 0.0150(16) C21 0.040(2) 0.043(2) 0.040(2) 0.0078(18) 0.0023(17) 0.0086(17) C22 0.049(2) 0.070(3) 0.0294(19) 0.011(2) 0.0110(17) 0.025(2) F1 0.0368(13) 0.0751(19) 0.0750(18) 0.0020(15) 0.0174(12) 0.0045(12) F2 0.0747(18) 0.0465(16) 0.0751(19) -0.0123(14) -0.0171(15) 0.0082(14) F3 0.0547(16) 0.086(2) 0.0666(18) 0.0378(16) -0.0215(13) 0.0053(14) F4 0.0376(13) 0.130(3) 0.0569(16) 0.0093(17) 0.0155(12) 0.0292(16) F5 0.0779(18) 0.088(2) 0.0278(12) 0.0214(13) 0.0207(12) 0.0254(15) F6 0.099(2) 0.076(2) 0.0474(15) 0.0060(14) 0.0326(15) 0.0480(17) _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 Pt C1 1.989(3) . ? Pt N1 1.994(3) . ? Pt N3 2.028(3) . ? Pt O1 2.047(2) . ? O1 C20 1.355(4) . ? N1 C7 1.341(4) . ? N1 C14 1.360(4) . ? N2 C14 1.298(4) . ? N2 C13 1.374(4) . ? N3 C15 1.336(5) . ? N3 C19 1.360(4) . ? C1 C2 1.403(5) . ? C1 C6 1.424(4) . ? C2 C3 1.373(5) . ? C3 C4 1.381(5) . ? C4 C5 1.382(5) . ? C5 C6 1.400(4) . ? C6 C7 1.459(4) . ? C7 C8 1.429(4) . ? C8 C9 1.415(5) . ? C8 C13 1.414(5) . ? C9 C10 1.361(5) . ? C10 C11 1.393(6) . ? C11 C12 1.358(5) . ? C12 C13 1.411(5) . ? C15 C16 1.381(5) . ? C16 C17 1.379(5) . ? C17 C18 1.378(6) . ? C18 C19 1.389(5) . ? C19 C20 1.531(5) . ? C20 C21 1.540(5) . ? C20 C22 1.546(5) . ? C21 F2 1.319(5) . ? C21 F1 1.323(5) . ? C21 F3 1.340(5) . ? C22 F4 1.321(5) . ? C22 F6 1.324(5) . ? C22 F5 1.351(4) . ? 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 C1 Pt N1 79.87(12) . . ? C1 Pt N3 106.27(12) . . ? N1 Pt N3 173.23(10) . . ? C1 Pt O1 173.08(11) . . ? N1 Pt O1 94.50(10) . . ? N3 Pt O1 79.56(10) . . ? C20 O1 Pt 114.5(2) . . ? C7 N1 C14 120.5(3) . . ? C7 N1 Pt 118.1(2) . . ? C14 N1 Pt 121.0(2) . . ? C14 N2 C13 116.1(3) . . ? C15 N3 C19 118.4(3) . . ? C15 N3 Pt 126.5(2) . . ? C19 N3 Pt 115.1(2) . . ? C2 C1 C6 115.3(3) . . ? C2 C1 Pt 130.0(2) . . ? C6 C1 Pt 114.4(2) . . ? C3 C2 C1 122.8(3) . . ? C2 C3 C4 120.8(3) . . ? C5 C4 C3 119.3(3) . . ? C4 C5 C6 119.9(3) . . ? C5 C6 C1 121.7(3) . . ? C5 C6 C7 124.3(3) . . ? C1 C6 C7 113.8(3) . . ? N1 C7 C8 117.9(3) . . ? N1 C7 C6 112.3(3) . . ? C8 C7 C6 129.8(3) . . ? C9 C8 C13 117.9(3) . . ? C9 C8 C7 125.3(3) . . ? C13 C8 C7 116.7(3) . . ? C10 C9 C8 121.2(4) . . ? C9 C10 C11 120.2(4) . . ? C12 C11 C10 120.8(3) . . ? C11 C12 C13 120.3(4) . . ? N2 C13 C12 118.0(3) . . ? N2 C13 C8 122.5(3) . . ? C12 C13 C8 119.5(3) . . ? N2 C14 N1 125.7(3) . . ? N3 C15 C16 122.9(3) . . ? C17 C16 C15 118.8(4) . . ? C18 C17 C16 118.9(3) . . ? C17 C18 C19 119.9(3) . . ? N3 C19 C18 120.9(3) . . ? N3 C19 C20 114.1(3) . . ? C18 C19 C20 125.0(3) . . ? O1 C20 C19 112.3(3) . . ? O1 C20 C21 109.5(3) . . ? C19 C20 C21 108.8(3) . . ? O1 C20 C22 106.4(3) . . ? C19 C20 C22 109.4(3) . . ? C21 C20 C22 110.5(3) . . ? F2 C21 F1 107.3(3) . . ? F2 C21 F3 106.2(3) . . ? F1 C21 F3 106.1(3) . . ? F2 C21 C20 112.7(3) . . ? F1 C21 C20 110.3(3) . . ? F3 C21 C20 113.8(3) . . ? F4 C22 F6 107.7(4) . . ? F4 C22 F5 106.3(4) . . ? F6 C22 F5 106.0(3) . . ? F4 C22 C20 110.6(3) . . ? F6 C22 C20 112.0(4) . . ? F5 C22 C20 113.8(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.910 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.103