# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2320 data_[Pt(en)(bpy)](PF6)2.phen.2H2O(1) #------------------------------------------------------------------------------ _audit_creation_date 'Mon Apr 5 15:40:36 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 917.54 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H28 F12 N6 O2 P2 Pt ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.837(6) _cell_length_b 21.00(1) _cell_length_c 7.149(6) _cell_angle_alpha 91.38(6) _cell_angle_beta 104.02(5) _cell_angle_gamma 87.67(4) _cell_volume 1577(1) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.740 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892.00 _exptl_absorpt_coefficient_mu 4.639 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa_analytical _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.873 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -24.89 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 1 1 -1 4 1 -1 3 0 _diffrn_reflns_number 5900 _reflns_number_total 5572 _reflns_number_gt 3833 _reflns_threshold_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.091 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05851 _diffrn_orient_matrix_UB_12 0.03670 _diffrn_orient_matrix_UB_13 -0.05370 _diffrn_orient_matrix_UB_21 -0.07350 _diffrn_orient_matrix_UB_22 -0.02893 _diffrn_orient_matrix_UB_23 -0.02936 _diffrn_orient_matrix_UB_31 -0.01521 _diffrn_orient_matrix_UB_32 0.00936 _diffrn_orient_matrix_UB_33 0.13056 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pt' 'Pt' -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.08973(4) 0.22608(2) 0.35116(6) 0.0424(1) Uani 1.00 . . . P1 P 0.7130(4) 0.4179(2) 0.9179(7) 0.091(1) Uani 1.00 . . . P2 P 0.7852(3) 0.0426(1) 0.5981(4) 0.0588(9) Uani 1.00 . . . F1 F 0.751(1) 0.4323(6) 1.131(2) 0.205(6) Uani 1.00 . . . F2 F 0.5846(9) 0.3950(5) 0.934(2) 0.162(5) Uani 1.00 . . . F3 F 0.776(1) 0.3502(4) 0.960(2) 0.175(5) Uani 1.00 . . . F4 F 0.671(1) 0.3987(5) 0.694(2) 0.180(5) Uani 1.00 . . . F5 F 0.835(1) 0.4422(5) 0.883(3) 0.245(7) Uani 1.00 . . . F6 F 0.6558(9) 0.4848(4) 0.872(2) 0.200(5) Uani 1.00 . . . F7 F 0.7399(6) 0.0842(4) 0.7597(10) 0.097(3) Uani 1.00 . . . F8 F 0.6731(8) -0.0017(4) 0.589(1) 0.132(4) Uani 1.00 . . . F9 F 0.8760(7) 0.0045(3) 0.772(1) 0.106(3) Uani 1.00 . . . F10 F 0.8394(9) -0.0006(4) 0.452(1) 0.148(4) Uani 1.00 . . . F11 F 0.8985(6) 0.0896(3) 0.608(1) 0.094(3) Uani 1.00 . . . F12 F 0.6990(6) 0.0825(4) 0.432(1) 0.111(3) Uani 1.00 . . . O1 O -0.1112(7) 0.2229(3) 0.7614(9) 0.065(2) Uani 1.00 . . . O2 O 0.7740(8) 0.3032(4) 0.452(1) 0.096(3) Uani 1.00 . . . N1 N -0.0947(7) 0.2379(4) 0.197(1) 0.048(2) Uani 1.00 . . . N2 N 0.0474(7) 0.1323(4) 0.314(1) 0.056(3) Uani 1.00 . . . N3 N 0.2729(7) 0.2160(4) 0.4948(10) 0.048(2) Uani 1.00 . . . N4 N 0.1332(8) 0.3181(3) 0.394(1) 0.047(3) Uani 1.00 . . . N5 N 0.1673(8) 0.1535(4) 0.890(1) 0.054(3) Uani 1.00 . . . N6 N 0.1164(8) 0.2816(4) 0.872(1) 0.059(3) Uani 1.00 . . . C1 C -0.1624(9) 0.1774(5) 0.184(2) 0.064(4) Uani 1.00 . . . C2 C -0.071(1) 0.1238(5) 0.161(2) 0.062(3) Uani 1.00 . . . C3 C 0.339(1) 0.1586(5) 0.537(1) 0.056(3) Uani 1.00 . . . C4 C 0.466(1) 0.1561(6) 0.629(2) 0.071(4) Uani 1.00 . . . C5 C 0.528(1) 0.2095(8) 0.683(2) 0.081(5) Uani 1.00 . . . C6 C 0.465(1) 0.2692(6) 0.642(2) 0.070(4) Uani 1.00 . . . C7 C 0.3329(10) 0.2703(5) 0.546(1) 0.053(3) Uani 1.00 . . . C8 C 0.2545(10) 0.3286(5) 0.491(1) 0.052(3) Uani 1.00 . . . C9 C 0.300(1) 0.3872(6) 0.533(2) 0.078(4) Uani 1.00 . . . C10 C 0.221(2) 0.4383(6) 0.479(2) 0.093(6) Uani 1.00 . . . C11 C 0.094(1) 0.4305(5) 0.377(2) 0.082(5) Uani 1.00 . . . C12 C 0.055(1) 0.3687(5) 0.337(2) 0.066(4) Uani 1.00 . . . C13 C 0.193(1) 0.0916(5) 0.899(2) 0.065(4) Uani 1.00 . . . C14 C 0.310(1) 0.0648(6) 0.990(2) 0.081(5) Uani 1.00 . . . C15 C 0.404(1) 0.1029(7) 1.078(2) 0.080(5) Uani 1.00 . . . C16 C 0.3847(10) 0.1698(5) 1.073(1) 0.057(3) Uani 1.00 . . . C17 C 0.479(1) 0.2138(7) 1.156(2) 0.079(4) Uani 1.00 . . . C18 C 0.454(1) 0.2777(7) 1.144(2) 0.077(4) Uani 1.00 . . . C19 C 0.333(1) 0.3027(6) 1.049(1) 0.063(4) Uani 1.00 . . . C20 C 0.305(1) 0.3681(6) 1.037(2) 0.080(5) Uani 1.00 . . . C21 C 0.187(2) 0.3888(6) 0.945(2) 0.088(5) Uani 1.00 . . . C22 C 0.097(1) 0.3446(6) 0.868(2) 0.073(4) Uani 1.00 . . . C23 C 0.236(1) 0.2612(5) 0.965(1) 0.054(3) Uani 1.00 . . . C24 C 0.2610(9) 0.1922(5) 0.975(1) 0.050(3) Uani 1.00 . . . H1 H -0.1367 0.2695 0.2582 0.0580 Uiso 1.00 . . . H2 H -0.0956 0.2511 0.0702 0.0580 Uiso 1.00 . . . H3 H 0.1157 0.1093 0.2784 0.0674 Uiso 1.00 . . . H4 H 0.0361 0.1163 0.4317 0.0674 Uiso 1.00 . . . H5 H -0.1907 0.1720 0.2985 0.0764 Uiso 1.00 . . . H6 H -0.2336 0.1781 0.0761 0.0764 Uiso 1.00 . . . H7 H -0.0526 0.1253 0.0380 0.0740 Uiso 1.00 . . . H8 H -0.1056 0.0840 0.1756 0.0740 Uiso 1.00 . . . H9 H 0.2959 0.1200 0.5015 0.0667 Uiso 1.00 . . . H10 H 0.5096 0.1160 0.6539 0.0853 Uiso 1.00 . . . H11 H 0.6149 0.2071 0.7491 0.0971 Uiso 1.00 . . . H12 H 0.5090 0.3076 0.6778 0.0841 Uiso 1.00 . . . H13 H 0.3863 0.3926 0.5987 0.0933 Uiso 1.00 . . . H14 H 0.2508 0.4800 0.5099 0.1117 Uiso 1.00 . . . H15 H 0.0377 0.4661 0.3372 0.0985 Uiso 1.00 . . . H16 H -0.0296 0.3619 0.2664 0.0790 Uiso 1.00 . . . H17 H 0.1265 0.0639 0.8407 0.0780 Uiso 1.00 . . . H18 H 0.3240 0.0198 0.9892 0.0976 Uiso 1.00 . . . H19 H 0.4841 0.0848 1.1439 0.0956 Uiso 1.00 . . . H20 H 0.5619 0.1983 1.2216 0.0944 Uiso 1.00 . . . H21 H 0.5196 0.3061 1.2012 0.0928 Uiso 1.00 . . . H22 H 0.3679 0.3976 1.0931 0.0957 Uiso 1.00 . . . H23 H 0.1662 0.4331 0.9326 0.1055 Uiso 1.00 . . . H24 H 0.0136 0.3605 0.8077 0.0871 Uiso 1.00 . . . H25 H -0.1339(4) 0.1749(2) 0.7102(7) 0.083(1) Uiso 1.00 . . . H26 H -0.0234 0.2291 0.7723 0.0782 Uiso 1.00 . . . H27 H 0.801(1) 0.2778(6) 0.545(2) 0.083(6) Uiso 1.00 . . . H28 H 0.8256(9) 0.3429(5) 0.469(2) 0.083(5) Uiso 1.00 . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt1 0.0433(2) 0.0440(2) 0.0415(2) 0.0017(1) 0.0133(2) 0.0033(1) P1 0.072(3) 0.053(2) 0.142(4) -0.001(2) 0.015(2) 0.001(2) P2 0.062(2) 0.047(2) 0.068(2) -0.009(1) 0.017(2) -0.006(1) F1 0.25(1) 0.21(1) 0.130(9) 0.03(1) 0.017(9) -0.056(9) F2 0.110(7) 0.177(10) 0.22(1) -0.067(7) 0.067(7) -0.049(8) F3 0.20(1) 0.082(6) 0.23(1) 0.047(6) 0.028(9) 0.045(7) F4 0.22(1) 0.164(10) 0.157(10) -0.001(9) 0.054(9) -0.033(8) F5 0.125(9) 0.138(10) 0.50(3) -0.030(8) 0.12(1) 0.03(1) F6 0.133(8) 0.059(5) 0.39(2) 0.013(5) 0.023(10) -0.008(8) F7 0.080(5) 0.128(6) 0.083(5) 0.023(4) 0.027(4) -0.028(4) F8 0.139(7) 0.146(8) 0.120(7) -0.094(6) 0.035(6) -0.007(6) F9 0.111(6) 0.093(5) 0.109(6) 0.032(5) 0.017(5) 0.025(5) F10 0.199(10) 0.128(7) 0.127(7) 0.026(7) 0.065(7) -0.047(6) F11 0.067(5) 0.095(5) 0.122(6) -0.022(4) 0.023(4) 0.011(4) F12 0.065(5) 0.144(7) 0.112(6) -0.004(5) -0.007(4) 0.053(5) O1 0.067(5) 0.070(5) 0.059(5) -0.004(4) 0.016(4) 0.000(4) O2 0.102(7) 0.105(7) 0.081(6) 0.034(5) 0.030(5) -0.003(5) N1 0.037(5) 0.055(5) 0.052(5) 0.005(4) 0.008(4) 0.010(4) N2 0.050(5) 0.045(5) 0.074(6) 0.003(4) 0.015(5) 0.010(4) N3 0.047(5) 0.073(6) 0.027(4) -0.002(4) 0.015(4) 0.003(4) N4 0.061(6) 0.039(5) 0.045(5) -0.004(4) 0.018(4) -0.002(4) N5 0.053(5) 0.058(5) 0.054(5) -0.010(4) 0.017(4) 0.002(4) N6 0.070(6) 0.057(6) 0.056(5) -0.004(5) 0.025(5) 0.000(4) C1 0.033(6) 0.078(8) 0.078(8) -0.008(6) 0.009(5) -0.001(6) C2 0.057(7) 0.053(6) 0.067(7) -0.012(5) 0.000(6) -0.005(5) C3 0.065(7) 0.067(7) 0.039(5) 0.008(6) 0.021(5) 0.013(5) C4 0.049(7) 0.099(10) 0.061(7) 0.030(7) 0.010(6) 0.019(7) C5 0.058(8) 0.13(1) 0.049(7) -0.007(8) 0.001(6) 0.007(8) C6 0.060(7) 0.096(9) 0.057(7) -0.026(7) 0.017(6) -0.006(7) C7 0.057(7) 0.073(7) 0.034(5) -0.014(6) 0.018(5) -0.011(5) C8 0.055(7) 0.063(7) 0.042(6) -0.014(6) 0.020(5) -0.005(5) C9 0.087(10) 0.071(8) 0.077(9) -0.024(7) 0.020(7) -0.014(7) C10 0.13(1) 0.065(9) 0.10(1) -0.040(9) 0.05(1) -0.022(8) C11 0.11(1) 0.047(7) 0.10(1) 0.001(7) 0.048(9) -0.005(7) C12 0.073(8) 0.067(8) 0.061(7) 0.006(6) 0.024(6) 0.010(6) C13 0.064(8) 0.066(8) 0.066(7) 0.002(6) 0.019(6) 0.000(6) C14 0.10(1) 0.069(8) 0.077(9) 0.005(8) 0.021(8) 0.003(7) C15 0.082(9) 0.093(10) 0.065(8) 0.031(8) 0.024(7) 0.023(7) C16 0.052(7) 0.083(8) 0.039(6) 0.001(6) 0.021(5) 0.003(5) C17 0.047(7) 0.13(1) 0.054(7) -0.001(8) 0.006(6) -0.004(8) C18 0.068(8) 0.12(1) 0.052(7) -0.022(8) 0.027(6) -0.019(7) C19 0.071(8) 0.076(8) 0.050(6) -0.024(7) 0.028(6) -0.009(6) C20 0.09(1) 0.084(10) 0.068(8) -0.032(8) 0.031(8) -0.021(7) C21 0.13(1) 0.059(8) 0.09(1) -0.031(9) 0.050(9) -0.022(7) C22 0.076(8) 0.083(9) 0.066(8) 0.008(7) 0.030(7) 0.014(7) C23 0.057(7) 0.075(7) 0.038(5) -0.013(6) 0.025(5) -0.004(5) C24 0.051(6) 0.067(7) 0.038(5) -0.005(5) 0.018(5) -0.001(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on 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 calculated 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. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor 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 'w = 1/[\s^2^(Fo^2^) + 0.00020(Fo^2^)^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5572 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_all 0.1017 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_all 1.496 _refine_ls_goodness_of_fit_ref 1.496 _refine_ls_shift/su_max 0.0210 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -1.39 _refine_diff_density_max 1.42 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PT1 N1 2.044(7) 1_555 1_555 yes PT1 N2 2.037(8) 1_555 1_555 yes PT1 N3 2.007(8) 1_555 1_555 yes PT1 N4 2.007(7) 1_555 1_555 yes P1 F1 1.51(1) 1_555 1_555 yes P1 F2 1.521(9) 1_555 1_555 yes P1 F3 1.556(8) 1_555 1_555 yes P1 F4 1.60(1) 1_555 1_555 yes P1 F5 1.51(1) 1_555 1_555 yes P1 F6 1.524(9) 1_555 1_555 yes P2 F7 1.591(6) 1_555 1_555 yes P2 F8 1.548(7) 1_555 1_555 yes P2 F9 1.593(7) 1_555 1_555 yes P2 F10 1.570(8) 1_555 1_555 yes P2 F11 1.594(7) 1_555 1_555 yes P2 F12 1.562(7) 1_555 1_555 yes O1 H25 1.08 1_555 1_555 no O1 H26 0.95 1_555 1_555 no O2 H27 0.85 1_555 1_555 no O2 H28 1.01 1_555 1_555 no N1 C1 1.48(1) 1_555 1_555 yes N1 H1 0.956 1_555 1_555 no N1 H2 0.963 1_555 1_555 no N2 C2 1.48(1) 1_555 1_555 yes N2 H3 0.963 1_555 1_555 no N2 H4 0.965 1_555 1_555 no N3 C3 1.38(1) 1_555 1_555 yes N3 C7 1.34(1) 1_555 1_555 yes N4 C8 1.35(1) 1_555 1_555 yes N4 C12 1.34(1) 1_555 1_555 yes N5 C13 1.32(1) 1_555 1_555 yes N5 C24 1.35(1) 1_555 1_555 yes N6 C22 1.33(1) 1_555 1_555 yes N6 C23 1.37(1) 1_555 1_555 yes C1 C2 1.51(1) 1_555 1_555 yes C1 H5 0.972 1_555 1_555 no C1 H6 0.947 1_555 1_555 no C2 H7 0.980 1_555 1_555 no C2 H8 0.938 1_555 1_555 no C3 C4 1.37(1) 1_555 1_555 yes C3 H9 0.986 1_555 1_555 no C4 C5 1.33(2) 1_555 1_555 yes C4 H10 0.970 1_555 1_555 no C5 C6 1.40(2) 1_555 1_555 yes C5 H11 0.955 1_555 1_555 no C6 C7 1.43(1) 1_555 1_555 yes C6 H12 0.970 1_555 1_555 no C7 C8 1.47(1) 1_555 1_555 yes C8 C9 1.34(1) 1_555 1_555 yes C9 C10 1.35(2) 1_555 1_555 yes C9 H13 0.974 1_555 1_555 no C10 C11 1.40(2) 1_555 1_555 yes C10 H14 0.975 1_555 1_555 no C11 C12 1.38(1) 1_555 1_555 yes C11 H15 0.988 1_555 1_555 no C12 H16 0.980 1_555 1_555 no C13 C14 1.38(2) 1_555 1_555 yes C13 H17 0.970 1_555 1_555 no C14 C15 1.35(2) 1_555 1_555 yes C14 H18 0.970 1_555 1_555 no C15 C16 1.41(2) 1_555 1_555 yes C15 H19 1.004 1_555 1_555 no C16 C17 1.42(2) 1_555 1_555 yes C16 C24 1.42(1) 1_555 1_555 yes C17 C18 1.36(2) 1_555 1_555 yes C17 H20 0.987 1_555 1_555 no C18 C19 1.42(2) 1_555 1_555 yes C18 H21 0.963 1_555 1_555 no C19 C20 1.39(2) 1_555 1_555 yes C19 C23 1.40(1) 1_555 1_555 yes C20 C21 1.35(2) 1_555 1_555 yes C20 H22 0.963 1_555 1_555 no C21 C22 1.38(2) 1_555 1_555 yes C21 H23 1.000 1_555 1_555 no C22 H24 0.977 1_555 1_555 no C23 C24 1.46(1) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 PT1 N2 82.0(3) 1_555 1_555 1_555 yes N1 PT1 N3 177.9(3) 1_555 1_555 1_555 yes N1 PT1 N4 98.9(3) 1_555 1_555 1_555 yes N2 PT1 N3 98.9(3) 1_555 1_555 1_555 yes N2 PT1 N4 178.7(3) 1_555 1_555 1_555 yes N3 PT1 N4 80.3(3) 1_555 1_555 1_555 yes F1 P1 F2 91.2(7) 1_555 1_555 1_555 yes F1 P1 F3 88.6(6) 1_555 1_555 1_555 yes F1 P1 F4 176.9(7) 1_555 1_555 1_555 yes F1 P1 F5 93.5(8) 1_555 1_555 1_555 yes F1 P1 F6 92.6(7) 1_555 1_555 1_555 yes F2 P1 F3 92.0(6) 1_555 1_555 1_555 yes F2 P1 F4 86.8(6) 1_555 1_555 1_555 yes F2 P1 F5 174.7(9) 1_555 1_555 1_555 yes F2 P1 F6 90.4(6) 1_555 1_555 1_555 yes F3 P1 F4 89.1(6) 1_555 1_555 1_555 yes F3 P1 F5 90.6(6) 1_555 1_555 1_555 yes F3 P1 F6 177.3(7) 1_555 1_555 1_555 yes F4 P1 F5 88.6(8) 1_555 1_555 1_555 yes F4 P1 F6 89.9(7) 1_555 1_555 1_555 yes F5 P1 F6 86.9(6) 1_555 1_555 1_555 yes F7 P2 F8 88.9(5) 1_555 1_555 1_555 yes F7 P2 F9 86.2(4) 1_555 1_555 1_555 yes F7 P2 F10 175.3(5) 1_555 1_555 1_555 yes F7 P2 F11 90.0(4) 1_555 1_555 1_555 yes F7 P2 F12 92.6(4) 1_555 1_555 1_555 yes F8 P2 F9 92.8(5) 1_555 1_555 1_555 yes F8 P2 F10 92.4(5) 1_555 1_555 1_555 yes F8 P2 F11 178.6(5) 1_555 1_555 1_555 yes F8 P2 F12 89.2(4) 1_555 1_555 1_555 yes F9 P2 F10 89.2(5) 1_555 1_555 1_555 yes F9 P2 F11 88.0(4) 1_555 1_555 1_555 yes F9 P2 F12 177.6(5) 1_555 1_555 1_555 yes F10 P2 F11 88.7(5) 1_555 1_555 1_555 yes F10 P2 F12 92.0(5) 1_555 1_555 1_555 yes F11 P2 F12 89.9(4) 1_555 1_555 1_555 yes PT1 N1 C1 110.8(6) 1_555 1_555 1_555 yes PT1 N1 H1 110.1(6) 1_555 1_555 1_555 no PT1 N1 H2 109.8(5) 1_555 1_555 1_555 no C1 N1 H1 109.8(7) 1_555 1_555 1_555 no C1 N1 H2 108.4(8) 1_555 1_555 1_555 no H1 N1 H2 107.8(7) 1_555 1_555 1_555 no PT1 N2 C2 111.0(6) 1_555 1_555 1_555 yes PT1 N2 H3 109.7(6) 1_555 1_555 1_555 no PT1 N2 H4 109.5(6) 1_555 1_555 1_555 no C2 N2 H3 110.6(8) 1_555 1_555 1_555 no C2 N2 H4 108.8(8) 1_555 1_555 1_555 no H3 N2 H4 107.1(7) 1_555 1_555 1_555 no PT1 N3 C3 125.1(7) 1_555 1_555 1_555 yes PT1 N3 C7 115.3(7) 1_555 1_555 1_555 yes C3 N3 C7 119.5(9) 1_555 1_555 1_555 yes PT1 N4 C8 115.2(7) 1_555 1_555 1_555 yes PT1 N4 C12 126.7(7) 1_555 1_555 1_555 yes C8 N4 C12 118.2(9) 1_555 1_555 1_555 yes C13 N5 C24 117.6(9) 1_555 1_555 1_555 yes C22 N6 C23 115.0(10) 1_555 1_555 1_555 yes N1 C1 C2 107.8(8) 1_555 1_555 1_555 yes N1 C1 H5 110.1(9) 1_555 1_555 1_555 no N1 C1 H6 112.6(10) 1_555 1_555 1_555 no C2 C1 H5 107.5(10) 1_555 1_555 1_555 no C2 C1 H6 110(1) 1_555 1_555 1_555 no H5 C1 H6 107.9(9) 1_555 1_555 1_555 no N2 C2 C1 107.2(8) 1_555 1_555 1_555 yes N2 C2 H7 109.3(9) 1_555 1_555 1_555 no N2 C2 H8 112.9(9) 1_555 1_555 1_555 no C1 C2 H7 107.6(10) 1_555 1_555 1_555 no C1 C2 H8 111(1) 1_555 1_555 1_555 no H7 C2 H8 107.9(10) 1_555 1_555 1_555 no N3 C3 C4 121(1) 1_555 1_555 1_555 yes N3 C3 H9 119.9(10) 1_555 1_555 1_555 no C4 C3 H9 118(1) 1_555 1_555 1_555 no C3 C4 C5 120(1) 1_555 1_555 1_555 yes C3 C4 H10 119(1) 1_555 1_555 1_555 no C5 C4 H10 120(1) 1_555 1_555 1_555 no C4 C5 C6 120(1) 1_555 1_555 1_555 yes C4 C5 H11 117(1) 1_555 1_555 1_555 no C6 C5 H11 121(1) 1_555 1_555 1_555 no C5 C6 C7 117(1) 1_555 1_555 1_555 yes C5 C6 H12 119(1) 1_555 1_555 1_555 no C7 C6 H12 122(1) 1_555 1_555 1_555 no N3 C7 C6 120(1) 1_555 1_555 1_555 yes N3 C7 C8 115.1(9) 1_555 1_555 1_555 yes C6 C7 C8 124(1) 1_555 1_555 1_555 yes N4 C8 C7 114.1(9) 1_555 1_555 1_555 yes N4 C8 C9 123(1) 1_555 1_555 1_555 yes C7 C8 C9 122(1) 1_555 1_555 1_555 yes C8 C9 C10 118(1) 1_555 1_555 1_555 yes C8 C9 H13 122(1) 1_555 1_555 1_555 no C10 C9 H13 119(1) 1_555 1_555 1_555 no C9 C10 C11 120(1) 1_555 1_555 1_555 yes C9 C10 H14 122(1) 1_555 1_555 1_555 no C11 C10 H14 116(1) 1_555 1_555 1_555 no C10 C11 C12 117(1) 1_555 1_555 1_555 yes C10 C11 H15 122(1) 1_555 1_555 1_555 no C12 C11 H15 120(1) 1_555 1_555 1_555 no N4 C12 C11 122(1) 1_555 1_555 1_555 yes N4 C12 H16 118(1) 1_555 1_555 1_555 no C11 C12 H16 119(1) 1_555 1_555 1_555 no N5 C13 C14 123(1) 1_555 1_555 1_555 yes N5 C13 H17 118(1) 1_555 1_555 1_555 no C14 C13 H17 117(1) 1_555 1_555 1_555 no C13 C14 C15 119(1) 1_555 1_555 1_555 yes C13 C14 H18 122(1) 1_555 1_555 1_555 no C15 C14 H18 118(1) 1_555 1_555 1_555 no C14 C15 C16 120(1) 1_555 1_555 1_555 yes C14 C15 H19 121(1) 1_555 1_555 1_555 no C16 C15 H19 118(1) 1_555 1_555 1_555 no C15 C16 C17 124(1) 1_555 1_555 1_555 yes C15 C16 C24 115(1) 1_555 1_555 1_555 yes C17 C16 C24 120(1) 1_555 1_555 1_555 yes C16 C17 C18 121(1) 1_555 1_555 1_555 yes C16 C17 H20 118(1) 1_555 1_555 1_555 no C18 C17 H20 120(1) 1_555 1_555 1_555 no C17 C18 C19 121(1) 1_555 1_555 1_555 yes C17 C18 H21 117(1) 1_555 1_555 1_555 no C19 C18 H21 121(1) 1_555 1_555 1_555 no C18 C19 C20 121(1) 1_555 1_555 1_555 yes C18 C19 C23 119(1) 1_555 1_555 1_555 yes C20 C19 C23 118(1) 1_555 1_555 1_555 yes C19 C20 C21 119(1) 1_555 1_555 1_555 yes C19 C20 H22 122(1) 1_555 1_555 1_555 no C21 C20 H22 118(1) 1_555 1_555 1_555 no C20 C21 C22 119(1) 1_555 1_555 1_555 yes C20 C21 H23 121(1) 1_555 1_555 1_555 no C22 C21 H23 119(1) 1_555 1_555 1_555 no N6 C22 C21 125(1) 1_555 1_555 1_555 yes N6 C22 H24 116(1) 1_555 1_555 1_555 no C21 C22 H24 117(1) 1_555 1_555 1_555 no N6 C23 C19 123(1) 1_555 1_555 1_555 yes N6 C23 C24 116.6(9) 1_555 1_555 1_555 yes C19 C23 C24 120(1) 1_555 1_555 1_555 yes N5 C24 C16 123.6(10) 1_555 1_555 1_555 yes N5 C24 C23 118.8(9) 1_555 1_555 1_555 yes C16 C24 C23 117.6(10) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F1 C12 3.49(2) 1_555 1_656 ? F1 O2 3.55(2) 1_555 1_556 ? F2 C20 3.36(2) 1_555 1_555 ? F2 C6 3.42(1) 1_555 1_555 ? F2 C18 3.44(2) 1_555 1_555 ? F3 N1 3.03(1) 1_555 1_656 ? F3 O1 3.32(1) 1_555 1_655 ? F3 C12 3.56(2) 1_555 1_656 ? F4 O2 2.97(1) 1_555 1_555 ? F4 C6 3.54(2) 1_555 1_555 ? F5 C22 3.45(2) 1_555 1_655 ? F5 C11 3.51(2) 1_555 2_666 ? F5 C10 3.57(2) 1_555 2_666 ? F6 C20 3.17(2) 1_555 2_667 ? F6 C21 3.29(2) 1_555 2_667 ? F6 C10 3.56(2) 1_555 2_666 ? F7 C2 3.21(1) 1_555 1_656 ? F7 C4 3.22(1) 1_555 1_555 ? F7 O1 3.39(1) 1_555 1_655 ? F7 C5 3.39(2) 1_555 1_555 ? F7 C1 3.53(1) 1_555 1_656 ? F8 C14 3.28(1) 1_555 2_657 ? F8 C3 3.40(1) 1_555 2_656 ? F8 C15 3.50(1) 1_555 2_657 ? F9 N2 3.05(1) 1_555 2_656 ? F9 C2 3.32(1) 1_555 2_656 ? F9 C14 3.34(2) 1_555 2_657 ? F9 C13 3.37(1) 1_555 2_657 ? F10 C13 3.08(1) 1_555 2_656 ? F10 N2 3.30(1) 1_555 2_656 ? F10 F10 3.38(2) 1_555 2_756 ? F10 F11 3.44(1) 1_555 2_756 ? F10 C14 3.45(2) 1_555 2_656 ? F11 O1 2.991(10) 1_555 1_655 ? F11 N2 3.11(1) 1_555 1_655 ? F11 C13 3.36(1) 1_555 1_655 ? F11 C2 3.38(1) 1_555 1_655 ? F11 N5 3.42(1) 1_555 1_655 ? F11 C1 3.49(1) 1_555 1_655 ? F12 C1 3.32(1) 1_555 1_655 ? F12 C4 3.47(1) 1_555 1_555 ? F12 C15 3.58(1) 1_555 1_554 ? O1 N6 2.74(1) 1_555 1_555 ? O1 O2 2.82(1) 1_555 1_455 ? O1 N1 3.082(10) 1_555 1_556 ? O1 N5 3.23(1) 1_555 1_555 ? O1 C1 3.37(1) 1_555 1_556 ? O1 C22 3.43(1) 1_555 1_555 ? O1 C2 3.51(1) 1_555 1_556 ? O2 N1 2.87(1) 1_555 1_655 ? O2 C1 3.37(1) 1_555 1_655 ? N3 C24 3.52(1) 1_555 1_555 ? N3 C23 3.58(1) 1_555 1_555 ? N3 N5 3.59(1) 1_555 1_555 ? N4 C22 3.53(1) 1_555 1_555 ? N4 N6 3.56(1) 1_555 1_555 ? N5 C3 3.48(1) 1_555 1_555 ? N6 C8 3.58(1) 1_555 1_555 ? C3 C16 3.48(1) 1_555 1_554 ? C3 C24 3.49(1) 1_555 1_555 ? C4 C16 3.50(1) 1_555 1_555 ? C5 C17 3.55(2) 1_555 1_555 ? C6 C18 3.54(2) 1_555 1_554 ? C6 C19 3.58(1) 1_555 1_555 ? C7 C23 3.41(1) 1_555 1_555 ? C7 C18 3.45(1) 1_555 1_554 ? C8 C19 3.50(1) 1_555 1_554 ? C8 C22 3.53(1) 1_555 1_555 ? C8 C20 3.54(2) 1_555 1_554 ? C9 C21 3.45(2) 1_555 1_555 ? C9 C20 3.57(2) 1_555 1_554 ? C11 C21 3.55(2) 1_555 1_554 ? C12 C21 3.48(2) 1_555 1_554 ? C12 C22 3.51(1) 1_555 1_554 ? #----------------------------------------------------------------------------- loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 F3 1_555 1_555 1_454 3.03(1) 0.956 2.687 101.570 yes N2 H3 F9 1_555 1_555 2_656 3.05(1) 0.963 2.393 124.815 yes N2 H3 F10 1_555 1_555 2_656 3.30(1) 0.963 2.935 103.934 yes N2 H4 F11 1_555 1_555 1_455 3.11(1) 0.965 2.252 147.430 yes N1 H2 O1 1_555 1_555 1_554 3.08(1) 0.963 2.224 147.811 yes N1 H1 O2 1_555 1_555 1_455 2.87(1) 0.956 1.982 153.219 yes O1 H26 N6 1_555 1_555 1_555 2.74(1) 0.96 1.89 ? yes O2 H27 O1 1_555 1_555 1_655 2.82(1) 0.85 1.98 ? yes #----------------------------------------------------------------------------- #===END data_[Pt(en)(phen)](PF6)2.phen.2H2O(2) #------------------------------------------------------------------------------ _audit_creation_date 'Mon Aug 22 11:45:23 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'SHELXL93' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 941.56 _chemical_formula_analytical ? _chemical_formula_sum 'C26 H28 F12 N6 O2 P2 Pt ' _chemical_formula_moiety 'C26 H28 F12 N6 O2 P2 Pt ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 6.945(5) _cell_length_b 35.895(8) _cell_length_c 13.249(5) _cell_angle_alpha 90 _cell_angle_beta 102.64(4) _cell_angle_gamma 90 _cell_volume 3223(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.7 _cell_measurement_theta_max 14.8 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832.00 _exptl_absorpt_coefficient_mu 4.542 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa_analytical _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.873 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.19 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -8 1 -1 -7 0 0 -6 1 _diffrn_reflns_number 7974 _reflns_number_total 7384 _reflns_number_gt 2782 _reflns_threshold_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.242 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.06063 _diffrn_orient_matrix_UB_12 -0.02276 _diffrn_orient_matrix_UB_13 -0.02360 _diffrn_orient_matrix_UB_21 0.10829 _diffrn_orient_matrix_UB_22 0.00092 _diffrn_orient_matrix_UB_23 0.06363 _diffrn_orient_matrix_UB_31 -0.07983 _diffrn_orient_matrix_UB_32 -0.01604 _diffrn_orient_matrix_UB_33 0.03711 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Pt' 'Pt' -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ 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_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.34936(6) 0.10689(1) 0.62188(3) 0.0478(1) Uani 1.00 . . . P1 P 0.2833(6) -0.0469(1) 0.7511(3) 0.077(1) Uani 1.00 . . . P2 P 0.0435(6) -0.1931(1) 0.7397(3) 0.0657(10) Uani 1.00 . . . F1 F 0.018(1) -0.1637(2) 0.6510(6) 0.105(3) Uani 1.00 . . . F2 F 0.069(2) -0.2227(3) 0.8285(8) 0.162(5) Uani 1.00 . . . F3 F 0.138(2) -0.2190(4) 0.675(1) 0.199(7) Uani 1.00 . . . F4 F -0.157(2) -0.2104(4) 0.6894(8) 0.181(6) Uani 1.00 . . . F5 F -0.047(3) -0.1671(4) 0.8034(10) 0.214(7) Uani 1.00 . . . F6 F 0.249(2) -0.1771(4) 0.7887(8) 0.170(6) Uani 1.00 . . . F7 F 0.125(1) -0.0157(2) 0.7071(7) 0.108(3) Uani 1.00 . . . F8 F 0.439(1) -0.0785(3) 0.7933(8) 0.129(4) Uani 1.00 . . . F9 F 0.210(2) -0.0699(4) 0.6510(8) 0.175(6) Uani 1.00 . . . F10 F 0.135(2) -0.0642(5) 0.803(1) 0.213(8) Uani 1.00 . . . F11 F 0.361(2) -0.0235(4) 0.850(1) 0.205(7) Uani 1.00 . . . F12 F 0.438(2) -0.0281(4) 0.705(1) 0.191(6) Uani 1.00 . . . O1 O 0.482(2) 0.1420(3) 0.3471(8) 0.110(4) Uani 1.00 . . . O2 O 0.730(1) 0.0317(3) 0.6454(9) 0.100(3) Uani 1.00 . . . N1 N 0.319(2) 0.0501(3) 0.6172(8) 0.072(3) Uani 1.00 . . . N2 N 0.249(1) 0.1020(3) 0.4663(7) 0.061(3) Uani 1.00 . . . N3 N 0.372(1) 0.1631(2) 0.6337(7) 0.048(2) Uani 1.00 . . . N4 N 0.461(1) 0.1112(3) 0.7757(7) 0.049(2) Uani 1.00 . . . N5 N -0.118(1) 0.1073(3) 0.6605(9) 0.064(3) Uani 1.00 . . . N6 N 0.023(2) 0.0657(3) 0.8318(9) 0.069(3) Uani 1.00 . . . C1 C 0.213(2) 0.0381(4) 0.512(1) 0.085(4) Uani 1.00 . . . C2 C 0.274(2) 0.0631(4) 0.435(1) 0.079(4) Uani 1.00 . . . C3 C 0.323(2) 0.1886(3) 0.5608(9) 0.057(3) Uani 1.00 . . . C4 C 0.344(2) 0.2260(4) 0.582(1) 0.070(4) Uani 1.00 . . . C5 C 0.416(2) 0.2388(3) 0.680(1) 0.064(3) Uani 1.00 . . . C6 C 0.469(2) 0.2116(4) 0.7604(9) 0.059(3) Uani 1.00 . . . C7 C 0.546(2) 0.2208(4) 0.864(1) 0.072(4) Uani 1.00 . . . C8 C 0.596(2) 0.1943(4) 0.9394(10) 0.070(4) Uani 1.00 . . . C9 C 0.573(2) 0.1562(4) 0.9128(9) 0.057(3) Uani 1.00 . . . C10 C 0.620(2) 0.1266(5) 0.9824(9) 0.070(4) Uani 1.00 . . . C11 C 0.592(2) 0.0906(4) 0.946(1) 0.070(4) Uani 1.00 . . . C12 C 0.511(2) 0.0838(3) 0.8439(10) 0.056(3) Uani 1.00 . . . C13 C 0.492(2) 0.1468(3) 0.8070(8) 0.047(3) Uani 1.00 . . . C14 C 0.443(2) 0.1741(3) 0.7327(8) 0.047(3) Uani 1.00 . . . C15 C -0.175(2) 0.1277(5) 0.577(1) 0.075(4) Uani 1.00 . . . C16 C -0.169(2) 0.1666(5) 0.576(1) 0.087(5) Uani 1.00 . . . C17 C -0.098(2) 0.1852(4) 0.669(2) 0.087(4) Uani 1.00 . . . C18 C -0.035(2) 0.1642(4) 0.760(1) 0.066(4) Uani 1.00 . . . C19 C 0.028(2) 0.1811(4) 0.856(1) 0.076(4) Uani 1.00 . . . C20 C 0.090(2) 0.1606(5) 0.943(1) 0.079(4) Uani 1.00 . . . C21 C 0.085(2) 0.1204(4) 0.938(1) 0.070(4) Uani 1.00 . . . C22 C 0.144(2) 0.0986(5) 1.027(1) 0.082(4) Uani 1.00 . . . C23 C 0.138(2) 0.0610(5) 1.017(1) 0.089(5) Uani 1.00 . . . C24 C 0.079(2) 0.0462(4) 0.917(1) 0.092(5) Uani 1.00 . . . C25 C 0.020(2) 0.1032(4) 0.843(1) 0.061(3) Uani 1.00 . . . C26 C -0.045(2) 0.1245(4) 0.751(1) 0.060(3) Uani 1.00 . . . H1 H 0.2470 0.0422 0.6668 0.0717 Uiso 1.00 . . . H2 H 0.4463 0.0386 0.6329 0.0717 Uiso 1.00 . . . H3 H 0.0745 0.0399 0.5073 0.0855 Uiso 1.00 . . . H4 H 0.2459 0.0130 0.5003 0.0855 Uiso 1.00 . . . H5 H 0.1935 0.0587 0.3682 0.0795 Uiso 1.00 . . . H6 H 0.4080 0.0590 0.4336 0.0795 Uiso 1.00 . . . H7 H 0.3198 0.1185 0.4316 0.0608 Uiso 1.00 . . . H8 H 0.1117 0.1087 0.4485 0.0608 Uiso 1.00 . . . H9 H 0.2747 0.1810 0.4906 0.0571 Uiso 1.00 . . . H10 H 0.3067 0.2433 0.5267 0.0698 Uiso 1.00 . . . H11 H 0.4291 0.2644 0.6944 0.0641 Uiso 1.00 . . . H12 H 0.5615 0.2459 0.8833 0.0719 Uiso 1.00 . . . H13 H 0.6511 0.2012 1.0090 0.0700 Uiso 1.00 . . . H14 H 0.6740 0.1310 1.0549 0.0700 Uiso 1.00 . . . H15 H 0.6264 0.0704 0.9936 0.0700 Uiso 1.00 . . . H16 H 0.4893 0.0585 0.8213 0.0563 Uiso 1.00 . . . H17 H -0.2234 0.1149 0.5116 0.0748 Uiso 1.00 . . . H18 H -0.2109 0.1806 0.5155 0.0871 Uiso 1.00 . . . H19 H -0.0919 0.2115 0.6718 0.0869 Uiso 1.00 . . . H20 H 0.0279 0.2080 0.8625 0.0762 Uiso 1.00 . . . H21 H 0.1348 0.1727 1.0079 0.0791 Uiso 1.00 . . . H22 H 0.1837 0.1099 1.0938 0.0817 Uiso 1.00 . . . H23 H 0.1686 0.0451 1.0757 0.0895 Uiso 1.00 . . . H24 H 0.0822 0.0201 0.9115 0.0922 Uiso 1.00 . . . H25 H 0.8337 0.0496 0.6771 0.1003 Uiso 1.00 . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt1 0.0410(2) 0.0532(3) 0.0495(2) -0.0002(3) 0.0106(2) -0.0008(3) P1 0.090(3) 0.079(3) 0.063(2) 0.016(2) 0.020(2) 0.016(2) P2 0.084(3) 0.059(2) 0.050(2) 0.000(2) 0.004(2) 0.004(2) F1 0.140(8) 0.082(6) 0.080(6) -0.005(5) -0.002(5) 0.030(5) F2 0.19(1) 0.138(9) 0.129(9) -0.041(9) -0.026(8) 0.070(7) F3 0.29(2) 0.15(1) 0.17(1) 0.10(1) 0.10(1) -0.021(9) F4 0.15(1) 0.25(1) 0.121(9) -0.12(1) -0.033(7) 0.060(9) F5 0.35(2) 0.19(1) 0.135(10) 0.09(1) 0.14(1) -0.009(9) F6 0.15(1) 0.20(1) 0.128(9) -0.064(10) -0.052(8) 0.057(9) F7 0.123(8) 0.082(6) 0.113(7) 0.028(6) 0.010(6) 0.010(5) F8 0.124(8) 0.125(8) 0.123(8) 0.050(7) -0.007(6) 0.021(6) F9 0.18(1) 0.19(1) 0.117(8) 0.087(10) -0.049(8) -0.071(8) F10 0.18(1) 0.26(2) 0.23(2) 0.06(1) 0.12(1) 0.15(1) F11 0.16(1) 0.22(1) 0.19(1) 0.06(1) -0.058(10) -0.12(1) F12 0.16(1) 0.17(1) 0.28(2) 0.036(10) 0.13(1) 0.09(1) O1 0.093(8) 0.138(10) 0.101(8) -0.016(7) 0.023(6) 0.015(7) O2 0.071(7) 0.075(7) 0.147(10) -0.001(5) 0.004(6) -0.031(6) N1 0.060(7) 0.076(7) 0.072(7) 0.004(6) -0.001(6) 0.007(6) N2 0.069(6) 0.063(7) 0.052(6) -0.001(6) 0.015(5) -0.006(5) N3 0.043(5) 0.049(5) 0.058(6) 0.005(5) 0.021(5) -0.001(5) N4 0.034(4) 0.056(6) 0.058(6) -0.004(5) 0.013(4) 0.005(5) N5 0.045(5) 0.067(7) 0.081(7) -0.002(6) 0.018(5) 0.001(7) N6 0.059(7) 0.064(8) 0.085(8) -0.004(6) 0.021(6) 0.009(6) C1 0.08(1) 0.069(10) 0.10(1) -0.011(8) 0.012(9) -0.013(9) C2 0.09(1) 0.071(10) 0.075(9) 0.000(8) 0.013(8) -0.019(8) C3 0.053(7) 0.058(8) 0.063(8) 0.001(6) 0.017(6) 0.008(7) C4 0.072(9) 0.060(9) 0.082(9) 0.005(7) 0.027(8) 0.006(8) C5 0.063(8) 0.054(8) 0.077(9) 0.001(7) 0.019(7) -0.007(7) C6 0.041(6) 0.086(10) 0.051(7) -0.013(7) 0.012(6) -0.003(7) C7 0.055(8) 0.081(10) 0.09(1) 0.004(8) 0.030(8) -0.013(8) C8 0.060(8) 0.10(1) 0.057(8) 0.000(8) 0.019(7) -0.021(8) C9 0.037(6) 0.079(9) 0.053(7) 0.000(6) 0.005(5) -0.001(7) C10 0.053(8) 0.11(1) 0.046(8) 0.008(8) 0.002(6) -0.006(8) C11 0.063(9) 0.09(1) 0.054(9) 0.010(8) 0.016(7) 0.031(8) C12 0.058(8) 0.043(7) 0.068(8) 0.008(6) 0.013(6) 0.018(6) C13 0.037(6) 0.064(8) 0.042(6) -0.001(6) 0.011(5) -0.009(6) C14 0.040(6) 0.051(7) 0.050(7) -0.008(6) 0.014(5) -0.003(6) C15 0.043(7) 0.10(1) 0.081(10) 0.008(8) 0.021(7) 0.002(9) C16 0.053(9) 0.11(1) 0.11(1) 0.014(9) 0.031(9) 0.05(1) C17 0.061(9) 0.08(1) 0.13(1) 0.003(8) 0.032(9) 0.00(1) C18 0.044(7) 0.08(1) 0.083(10) -0.002(7) 0.024(7) 0.004(8) C19 0.056(8) 0.069(9) 0.11(1) -0.003(8) 0.043(9) -0.026(10) C20 0.07(1) 0.09(1) 0.08(1) -0.026(9) 0.022(8) -0.040(9) C21 0.047(7) 0.09(1) 0.071(9) -0.005(7) 0.016(7) -0.002(8) C22 0.069(9) 0.10(1) 0.076(10) 0.010(9) 0.019(8) -0.004(9) C23 0.08(1) 0.10(1) 0.09(1) 0.00(1) 0.033(9) 0.03(1) C24 0.10(1) 0.08(1) 0.10(1) -0.008(10) 0.04(1) 0.00(1) C25 0.046(6) 0.060(8) 0.083(9) 0.008(7) 0.026(6) -0.010(8) C26 0.042(7) 0.063(8) 0.086(10) -0.006(6) 0.036(7) -0.005(8) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on 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 calculated 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. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor 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 'w = 1/[\s^2^(Fo^2^) + (0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7384 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2332 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1517 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.0120 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -1.82 _refine_diff_density_max 0.83 _refine_diff_density_rms 0.16 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PT1 N1 2.05(1) 1_555 1_555 yes PT1 N2 2.034(9) 1_555 1_555 yes PT1 N3 2.029(9) 1_555 1_555 yes PT1 N4 2.022(9) 1_555 1_555 yes P1 F7 1.587(9) 1_555 1_555 yes P1 F8 1.58(1) 1_555 1_555 yes P1 F9 1.55(1) 1_555 1_555 yes P1 F10 1.49(2) 1_555 1_555 yes P1 F11 1.55(1) 1_555 1_555 yes P1 F12 1.51(2) 1_555 1_555 yes P2 F1 1.561(9) 1_555 1_555 yes P2 F2 1.57(1) 1_555 1_555 yes P2 F3 1.51(2) 1_555 1_555 yes P2 F4 1.53(1) 1_555 1_555 yes P2 F5 1.49(2) 1_555 1_555 yes P2 F6 1.54(1) 1_555 1_555 yes O2 H25 0.988 1_555 1_555 no N1 C1 1.50(2) 1_555 1_555 yes N1 H1 0.952 1_555 1_555 no N1 H2 0.957 1_555 1_555 no N2 C2 1.48(2) 1_555 1_555 yes N2 H7 0.953 1_555 1_555 no N2 H8 0.958 1_555 1_555 no N3 C3 1.32(1) 1_555 1_555 yes N3 C14 1.35(1) 1_555 1_555 yes N4 C12 1.33(1) 1_555 1_555 yes N4 C13 1.34(2) 1_555 1_555 yes N5 C15 1.31(2) 1_555 1_555 yes N5 C26 1.35(2) 1_555 1_555 yes N6 C24 1.32(2) 1_555 1_555 yes N6 C25 1.36(2) 1_555 1_555 yes C1 C2 1.48(2) 1_555 1_555 yes C1 H3 0.953 1_555 1_555 no C1 H4 0.950 1_555 1_555 no C2 H5 0.955 1_555 1_555 no C2 H6 0.945 1_555 1_555 no C3 C4 1.37(2) 1_555 1_555 yes C3 H9 0.957 1_555 1_555 no C4 C5 1.37(2) 1_555 1_555 yes C4 H10 0.955 1_555 1_555 no C5 C6 1.43(2) 1_555 1_555 yes C5 H11 0.940 1_555 1_555 no C6 C7 1.40(2) 1_555 1_555 yes C6 C14 1.40(2) 1_555 1_555 yes C7 C8 1.37(2) 1_555 1_555 yes C7 H12 0.937 1_555 1_555 no C8 C9 1.41(2) 1_555 1_555 yes C8 H13 0.949 1_555 1_555 no C9 C10 1.40(2) 1_555 1_555 yes C9 C13 1.43(2) 1_555 1_555 yes C10 C11 1.37(2) 1_555 1_555 yes C10 H14 0.965 1_555 1_555 no C11 C12 1.37(2) 1_555 1_555 yes C11 H15 0.955 1_555 1_555 no C12 H16 0.958 1_555 1_555 no C13 C14 1.38(2) 1_555 1_555 yes C15 C16 1.40(3) 1_555 1_555 yes C15 H17 0.975 1_555 1_555 no C16 C17 1.39(2) 1_555 1_555 yes C16 H18 0.940 1_555 1_555 no C17 C18 1.40(2) 1_555 1_555 yes C17 H19 0.947 1_555 1_555 no C18 C19 1.39(2) 1_555 1_555 yes C18 C26 1.43(2) 1_555 1_555 yes C19 C20 1.35(2) 1_555 1_555 yes C19 H20 0.970 1_555 1_555 no C20 C21 1.44(2) 1_555 1_555 yes C20 H21 0.956 1_555 1_555 no C21 C22 1.40(2) 1_555 1_555 yes C21 C25 1.39(2) 1_555 1_555 yes C22 C23 1.36(2) 1_555 1_555 yes C22 H22 0.957 1_555 1_555 no C23 C24 1.39(2) 1_555 1_555 yes C23 H23 0.955 1_555 1_555 no C24 H24 0.940 1_555 1_555 no C25 C26 1.42(2) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 PT1 N2 82.7(4) 1_555 1_555 1_555 yes N1 PT1 N3 176.7(4) 1_555 1_555 1_555 yes N1 PT1 N4 96.9(4) 1_555 1_555 1_555 yes N2 PT1 N3 99.6(4) 1_555 1_555 1_555 yes N2 PT1 N4 177.7(4) 1_555 1_555 1_555 yes N3 PT1 N4 80.8(4) 1_555 1_555 1_555 yes F7 P1 F8 179.0(5) 1_555 1_555 1_555 yes F7 P1 F9 89.5(6) 1_555 1_555 1_555 yes F7 P1 F10 88.4(7) 1_555 1_555 1_555 yes F7 P1 F11 90.7(6) 1_555 1_555 1_555 yes F7 P1 F12 91.7(6) 1_555 1_555 1_555 yes F8 P1 F9 89.5(6) 1_555 1_555 1_555 yes F8 P1 F10 91.6(7) 1_555 1_555 1_555 yes F8 P1 F11 90.3(6) 1_555 1_555 1_555 yes F8 P1 F12 88.4(7) 1_555 1_555 1_555 yes F9 P1 F10 92.4(8) 1_555 1_555 1_555 yes F9 P1 F11 178.3(8) 1_555 1_555 1_555 yes F9 P1 F12 91.0(8) 1_555 1_555 1_555 yes F10 P1 F11 89.2(8) 1_555 1_555 1_555 yes F10 P1 F12 176.5(8) 1_555 1_555 1_555 yes F11 P1 F12 87.3(8) 1_555 1_555 1_555 yes F1 P2 F2 179.8(5) 1_555 1_555 1_555 yes F1 P2 F3 89.0(6) 1_555 1_555 1_555 yes F1 P2 F4 90.2(6) 1_555 1_555 1_555 yes F1 P2 F5 90.7(6) 1_555 1_555 1_555 yes F1 P2 F6 90.5(6) 1_555 1_555 1_555 yes F2 P2 F3 90.9(7) 1_555 1_555 1_555 yes F2 P2 F4 89.6(7) 1_555 1_555 1_555 yes F2 P2 F5 89.5(7) 1_555 1_555 1_555 yes F2 P2 F6 89.7(7) 1_555 1_555 1_555 yes F3 P2 F4 88.3(8) 1_555 1_555 1_555 yes F3 P2 F5 179.1(9) 1_555 1_555 1_555 yes F3 P2 F6 89.4(8) 1_555 1_555 1_555 yes F4 P2 F5 92.5(8) 1_555 1_555 1_555 yes F4 P2 F6 177.6(8) 1_555 1_555 1_555 yes F5 P2 F6 89.8(8) 1_555 1_555 1_555 yes PT1 N1 C1 109.9(8) 1_555 1_555 1_555 yes PT1 N1 H1 110.1(8) 1_555 1_555 1_555 no PT1 N1 H2 109.9(8) 1_555 1_555 1_555 no C1 N1 H1 109(1) 1_555 1_555 1_555 no C1 N1 H2 108(1) 1_555 1_555 1_555 no H1 N1 H2 108(1) 1_555 1_555 1_555 no PT1 N2 C2 109.1(7) 1_555 1_555 1_555 yes PT1 N2 H7 109.6(7) 1_555 1_555 1_555 no PT1 N2 H8 109.3(8) 1_555 1_555 1_555 no C2 N2 H7 110(1) 1_555 1_555 1_555 no C2 N2 H8 110.0(10) 1_555 1_555 1_555 no H7 N2 H8 108.6(9) 1_555 1_555 1_555 no PT1 N3 C3 129.1(8) 1_555 1_555 1_555 yes PT1 N3 C14 111.6(7) 1_555 1_555 1_555 yes C3 N3 C14 119.3(10) 1_555 1_555 1_555 yes PT1 N4 C12 127.9(8) 1_555 1_555 1_555 yes PT1 N4 C13 112.6(7) 1_555 1_555 1_555 yes C12 N4 C13 119.4(9) 1_555 1_555 1_555 yes C15 N5 C26 118(1) 1_555 1_555 1_555 yes C24 N6 C25 116(1) 1_555 1_555 1_555 yes N1 C1 C2 107(1) 1_555 1_555 1_555 yes N1 C1 H3 108(1) 1_555 1_555 1_555 no N1 C1 H4 109(1) 1_555 1_555 1_555 no C2 C1 H3 110(1) 1_555 1_555 1_555 no C2 C1 H4 110(1) 1_555 1_555 1_555 no H3 C1 H4 109(1) 1_555 1_555 1_555 no N2 C2 C1 108(1) 1_555 1_555 1_555 yes N2 C2 H5 109(1) 1_555 1_555 1_555 no N2 C2 H6 109(1) 1_555 1_555 1_555 no C1 C2 H5 109(1) 1_555 1_555 1_555 no C1 C2 H6 110(1) 1_555 1_555 1_555 no H5 C2 H6 109(1) 1_555 1_555 1_555 no N3 C3 C4 121(1) 1_555 1_555 1_555 yes N3 C3 H9 119(1) 1_555 1_555 1_555 no C4 C3 H9 118(1) 1_555 1_555 1_555 no C3 C4 C5 121(1) 1_555 1_555 1_555 yes C3 C4 H10 118(1) 1_555 1_555 1_555 no C5 C4 H10 119(1) 1_555 1_555 1_555 no C4 C5 C6 117(1) 1_555 1_555 1_555 yes C4 C5 H11 121(1) 1_555 1_555 1_555 no C6 C5 H11 121(1) 1_555 1_555 1_555 no C5 C6 C7 123(1) 1_555 1_555 1_555 yes C5 C6 C14 117(1) 1_555 1_555 1_555 yes C7 C6 C14 118(1) 1_555 1_555 1_555 yes C6 C7 C8 122(1) 1_555 1_555 1_555 yes C6 C7 H12 119(1) 1_555 1_555 1_555 no C8 C7 H12 118(1) 1_555 1_555 1_555 no C7 C8 C9 119(1) 1_555 1_555 1_555 yes C7 C8 H13 120(1) 1_555 1_555 1_555 no C9 C8 H13 119(1) 1_555 1_555 1_555 no C8 C9 C10 125(1) 1_555 1_555 1_555 yes C8 C9 C13 118(1) 1_555 1_555 1_555 yes C10 C9 C13 116(1) 1_555 1_555 1_555 yes C9 C10 C11 119(1) 1_555 1_555 1_555 yes C9 C10 H14 121(1) 1_555 1_555 1_555 no C11 C10 H14 119(1) 1_555 1_555 1_555 no C10 C11 C12 120(1) 1_555 1_555 1_555 yes C10 C11 H15 119(1) 1_555 1_555 1_555 no C12 C11 H15 120(1) 1_555 1_555 1_555 no N4 C12 C11 122(1) 1_555 1_555 1_555 yes N4 C12 H16 119(1) 1_555 1_555 1_555 no C11 C12 H16 118(1) 1_555 1_555 1_555 no N4 C13 C9 121(1) 1_555 1_555 1_555 yes N4 C13 C14 117.1(9) 1_555 1_555 1_555 yes C9 C13 C14 120(1) 1_555 1_555 1_555 yes N3 C14 C6 122(1) 1_555 1_555 1_555 yes N3 C14 C13 117(1) 1_555 1_555 1_555 yes C6 C14 C13 120.0(10) 1_555 1_555 1_555 yes N5 C15 C16 123(1) 1_555 1_555 1_555 yes N5 C15 H17 118(1) 1_555 1_555 1_555 no C16 C15 H17 118(1) 1_555 1_555 1_555 no C15 C16 C17 118(1) 1_555 1_555 1_555 yes C15 C16 H18 122(1) 1_555 1_555 1_555 no C17 C16 H18 119(1) 1_555 1_555 1_555 no C16 C17 C18 118(1) 1_555 1_555 1_555 yes C16 C17 H19 120(1) 1_555 1_555 1_555 no C18 C17 H19 120(1) 1_555 1_555 1_555 no C17 C18 C19 121(1) 1_555 1_555 1_555 yes C17 C18 C26 118(1) 1_555 1_555 1_555 yes C19 C18 C26 120(1) 1_555 1_555 1_555 yes C18 C19 C20 121(1) 1_555 1_555 1_555 yes C18 C19 H20 120(1) 1_555 1_555 1_555 no C20 C19 H20 118(1) 1_555 1_555 1_555 no C19 C20 C21 120(1) 1_555 1_555 1_555 yes C19 C20 H21 119(1) 1_555 1_555 1_555 no C21 C20 H21 119(1) 1_555 1_555 1_555 no C20 C21 C22 121(1) 1_555 1_555 1_555 yes C20 C21 C25 118(1) 1_555 1_555 1_555 yes C22 C21 C25 119(1) 1_555 1_555 1_555 yes C21 C22 C23 118(1) 1_555 1_555 1_555 yes C21 C22 H22 120(1) 1_555 1_555 1_555 no C23 C22 H22 120(1) 1_555 1_555 1_555 no C22 C23 C24 118(1) 1_555 1_555 1_555 yes C22 C23 H23 120(1) 1_555 1_555 1_555 no C24 C23 H23 120(1) 1_555 1_555 1_555 no N6 C24 C23 125(1) 1_555 1_555 1_555 yes N6 C24 H24 117(1) 1_555 1_555 1_555 no C23 C24 H24 116(1) 1_555 1_555 1_555 no N6 C25 C21 121(1) 1_555 1_555 1_555 yes N6 C25 C26 117(1) 1_555 1_555 1_555 yes C21 C25 C26 121(1) 1_555 1_555 1_555 yes N5 C26 C18 121(1) 1_555 1_555 1_555 yes N5 C26 C25 120(1) 1_555 1_555 1_555 yes C18 C26 C25 118(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag PT1 N5 3.39(1) 1_555 1_555 ? F1 N2 3.08(1) 1_555 3_556 ? F1 C3 3.37(1) 1_555 3_556 ? F1 C16 3.40(2) 1_555 3_556 ? F1 O1 3.56(2) 1_555 3_656 ? F1 O1 3.56(2) 1_555 3_556 ? F2 C17 3.31(2) 1_555 2_546 ? F2 C8 3.57(2) 1_555 3_657 ? F3 C7 3.21(2) 1_555 2_646 ? F4 O1 3.30(2) 1_555 3_556 ? F4 C5 3.30(2) 1_555 2_546 ? F4 C3 3.36(2) 1_555 3_556 ? F4 C4 3.59(2) 1_555 3_556 ? F5 O1 3.35(2) 1_555 3_556 ? F5 C20 3.45(2) 1_555 3_557 ? F5 C22 3.49(2) 1_555 3_557 ? F6 O1 3.13(2) 1_555 3_656 ? F6 C10 3.48(2) 1_555 3_657 ? F6 C8 3.58(2) 1_555 3_657 ? F7 O2 3.18(1) 1_555 1_455 ? F7 C1 3.40(2) 1_555 3_556 ? F7 C2 3.45(2) 1_555 3_556 ? F8 O1 3.07(2) 1_555 3_656 ? F8 C22 3.40(2) 1_555 3_657 ? F8 C23 3.48(2) 1_555 3_657 ? F8 C11 3.53(2) 1_555 3_657 ? F8 C10 3.54(2) 1_555 3_657 ? F9 C2 3.32(2) 1_555 3_556 ? F9 O1 3.36(2) 1_555 3_656 ? F9 N2 3.43(2) 1_555 3_556 ? F9 C1 3.44(2) 1_555 3_556 ? F10 C23 3.37(2) 1_555 3_557 ? F10 C22 3.50(2) 1_555 3_557 ? F10 C11 3.57(2) 1_555 3_657 ? F11 C11 3.58(2) 1_555 3_657 ? F12 C2 3.26(2) 1_555 3_656 ? O1 C15 3.47(2) 1_555 1_655 ? O1 C16 3.56(2) 1_555 1_655 ? O2 N5 2.90(1) 1_555 1_655 ? O2 N6 3.09(1) 1_555 1_655 ? O2 C1 3.34(2) 1_555 3_656 ? O2 C2 3.56(2) 1_555 3_656 ? N3 C16 3.44(2) 1_555 1_655 ? N4 C26 3.55(2) 1_555 1_655 ? N4 N5 3.59(1) 1_555 1_655 ? C3 C16 3.58(2) 1_555 1_655 ? C8 C19 3.45(2) 1_555 1_655 ? C9 C19 3.52(2) 1_555 1_655 ? C9 C20 3.53(2) 1_555 1_655 ? C10 C21 3.41(2) 1_555 1_655 ? C11 C25 3.57(2) 1_555 1_655 ? C13 C18 3.53(2) 1_555 1_655 ? C13 C26 3.54(2) 1_555 1_655 ? C14 C17 3.49(2) 1_555 1_655 ? C14 C18 3.58(2) 1_555 1_655 ? O1 N2 2.88(2) 1_555 1_555 ? O2 N1 2.87(1) 1_555 1_555 ? O2 N5 2.90(1) 1_555 1_655 ? O2 N6 3.09(1) 1_555 1_655 ? N1 N2 2.70(1) 1_555 1_555 ? N1 O2 2.87(1) 1_555 1_555 ? N1 N4 3.05(1) 1_555 1_555 ? N2 N1 2.70(1) 1_555 1_555 ? N2 O1 2.88(2) 1_555 1_555 ? N2 N3 3.10(1) 1_555 1_555 ? N3 N4 2.62(1) 1_555 1_555 ? N3 C5 2.79(2) 1_555 1_555 ? N3 N2 3.10(1) 1_555 1_555 ? N4 N3 2.62(1) 1_555 1_555 ? N4 C10 2.78(1) 1_555 1_555 ? N4 N1 3.05(1) 1_555 1_555 ? N5 N6 2.72(2) 1_555 1_555 ? N5 C17 2.80(2) 1_555 1_555 ? N5 O2 2.90(1) 1_555 1_455 ? N6 N5 2.72(2) 1_555 1_555 ? N6 C22 2.80(2) 1_555 1_555 ? N6 O2 3.09(1) 1_555 1_455 ? C3 C6 2.74(2) 1_555 1_555 ? C4 C14 2.71(2) 1_555 1_555 ? C5 N3 2.79(2) 1_555 1_555 ? C6 C3 2.74(2) 1_555 1_555 ? C6 C9 2.81(2) 1_555 1_555 ? C7 C13 2.77(2) 1_555 1_555 ? C8 C14 2.81(2) 1_555 1_555 ? C9 C12 2.76(2) 1_555 1_555 ? C9 C6 2.81(2) 1_555 1_555 ? C10 N4 2.78(1) 1_555 1_555 ? C11 C13 2.72(2) 1_555 1_555 ? C12 C9 2.76(2) 1_555 1_555 ? C13 C11 2.72(2) 1_555 1_555 ? C13 C7 2.77(2) 1_555 1_555 ? C14 C4 2.71(2) 1_555 1_555 ? C14 C8 2.81(2) 1_555 1_555 ? C15 C18 2.74(2) 1_555 1_555 ? C16 C26 2.75(2) 1_555 1_555 ? C17 N5 2.80(2) 1_555 1_555 ? C18 C15 2.74(2) 1_555 1_555 ? C18 C21 2.81(2) 1_555 1_555 ? C19 C25 2.80(2) 1_555 1_555 ? C20 C26 2.82(2) 1_555 1_555 ? C21 C24 2.68(2) 1_555 1_555 ? C21 C18 2.81(2) 1_555 1_555 ? C22 N6 2.80(2) 1_555 1_555 ? C23 C25 2.73(2) 1_555 1_555 ? C24 C21 2.68(2) 1_555 1_555 ? C25 C23 2.73(2) 1_555 1_555 ? C25 C19 2.80(2) 1_555 1_555 ? C26 C16 2.75(2) 1_555 1_555 ? C26 C20 2.82(2) 1_555 1_555 ? #----------------------------------------------------------------------------- loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 F7 1_555 1_555 1_555 3.08(1) 0.952 2.347 133.752 yes N1 H1 F12 1_555 1_555 1_555 3.08(1) 0.958 2.842 95.249 yes N1 H2 O2 1_555 1_555 1_555 2.87(1) 0.957 1.955 159.824 yes N2 H7 O1 1_555 1_555 1_555 2.88(1) 0.953 1.943 167.182 yes N2 H7 F1 1_555 1_555 2_556 3.08(1) 0.953 2.865 93.872 yes N2 H8 F9 1_555 1_555 2_556 3.43(1) 0.958 2.719 131.149 yes O2 H25 N5 1_555 1_555 1_655 2.90(1) 0.988 2.12 ? yes O2 H25 N6 1_555 1_555 1_655 3.09(1) 0.988 2.26 ? yes #------------------------------------------------------------------------------ #===END data_[Pt(en)(bpy)](PF6)2.phe(3) #------------------------------------------------------------------------------ _audit_creation_date 'Wed Aug 24 11:38:45 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'SHELXL93' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 879.54 _chemical_formula_analytical ? _chemical_formula_sum 'C26 H26 F12 N4 P2 Pt ' _chemical_formula_moiety 'C26 H26 F12 N4 P2 Pt ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.762(4) _cell_length_b 19.455(8) _cell_length_c 6.903(3) _cell_angle_alpha 97.21(4) _cell_angle_beta 105.97(3) _cell_angle_gamma 86.52(3) _cell_volume 1505(1) _cell_formula_units_Z 2 _cell_measurement_temperature 294.5 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.920 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.060 _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852.00 _exptl_absorpt_coefficient_mu 4.846 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa_analytical _exptl_absorpt_correction_T_min 0.645 _exptl_absorpt_correction_T_max 0.769 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294.5 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.82 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -3 -1 1 -3 0 2 1 -1 _diffrn_reflns_number 7462 _reflns_number_total 6885 _reflns_number_gt 5043 _reflns_threshold_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.066 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.07879 _diffrn_orient_matrix_UB_12 -0.02458 _diffrn_orient_matrix_UB_13 0.01880 _diffrn_orient_matrix_UB_21 -0.02814 _diffrn_orient_matrix_UB_22 -0.03681 _diffrn_orient_matrix_UB_23 0.06328 _diffrn_orient_matrix_UB_31 -0.02873 _diffrn_orient_matrix_UB_32 -0.02697 _diffrn_orient_matrix_UB_33 -0.13655 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pt' 'Pt' -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ 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_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.11632(3) 0.23534(2) 0.40686(5) 0.0417(1) Uani 1.00 . . . P1 P 0.8274(3) 0.3503(2) 0.7858(6) 0.0662(8) Uani 1.00 . . . P2 P 0.7997(3) 0.0526(2) 0.6234(6) 0.0631(7) Uani 1.00 . . . F1 F 0.711(1) 0.3941(7) 0.700(2) 0.144(5) Uani 1.00 . . . F2 F 0.761(1) 0.3212(9) 0.920(2) 0.156(6) Uani 1.00 . . . F3 F 0.774(1) 0.2921(8) 0.623(3) 0.164(6) Uani 1.00 . . . F4 F 0.9393(10) 0.3064(9) 0.879(3) 0.155(6) Uani 1.00 . . . F5 F 0.892(2) 0.3738(8) 0.638(3) 0.164(6) Uani 1.00 . . . F6 F 0.876(2) 0.412(1) 0.930(3) 0.25(1) Uani 1.00 . . . F7 F 0.9110(8) 0.0992(7) 0.658(2) 0.114(4) Uani 1.00 . . . F8 F 0.7564(8) 0.1008(5) 0.792(1) 0.097(3) Uani 1.00 . . . F9 F 0.7248(7) 0.0966(5) 0.453(1) 0.087(2) Uani 1.00 . . . F10 F 0.686(1) 0.0071(6) 0.590(2) 0.129(4) Uani 1.00 . . . F11 F 0.839(1) 0.0011(7) 0.459(2) 0.132(5) Uani 1.00 . . . F12 F 0.874(1) 0.0071(5) 0.796(2) 0.109(4) Uani 1.00 . . . N1 N -0.0609(8) 0.2576(5) 0.294(2) 0.057(2) Uani 1.00 . . . N2 N 0.0599(9) 0.1351(5) 0.359(1) 0.057(2) Uani 1.00 . . . N3 N 0.2899(7) 0.2149(5) 0.512(1) 0.048(2) Uani 1.00 . . . N4 N 0.1733(8) 0.3328(5) 0.449(1) 0.049(2) Uani 1.00 . . . C1 C -0.131(1) 0.1942(8) 0.260(2) 0.073(4) Uani 1.00 . . . C2 C -0.057(1) 0.1306(8) 0.208(2) 0.076(4) Uani 1.00 . . . C3 C 0.3430(10) 0.1548(7) 0.542(2) 0.058(3) Uani 1.00 . . . C4 C 0.466(1) 0.1456(7) 0.616(2) 0.064(3) Uani 1.00 . . . C5 C 0.535(1) 0.2041(9) 0.655(2) 0.075(4) Uani 1.00 . . . C6 C 0.482(1) 0.2683(8) 0.628(2) 0.065(3) Uani 1.00 . . . C7 C 0.3584(9) 0.2736(6) 0.555(1) 0.048(2) Uani 1.00 . . . C8 C 0.2932(10) 0.3391(6) 0.518(2) 0.050(2) Uani 1.00 . . . C9 C 0.344(1) 0.4030(7) 0.547(2) 0.062(3) Uani 1.00 . . . C10 C 0.272(1) 0.4619(7) 0.506(2) 0.070(3) Uani 1.00 . . . C11 C 0.154(1) 0.4542(7) 0.436(2) 0.076(4) Uani 1.00 . . . C12 C 0.105(1) 0.3908(7) 0.411(2) 0.064(3) Uani 1.00 . . . C13 C 0.211(1) 0.195(1) 0.953(2) 0.087(5) Uani 1.00 . . . C14 C 0.201(2) 0.127(1) 0.937(2) 0.087(5) Uani 1.00 . . . C15 C 0.302(2) 0.085(1) 1.006(3) 0.096(5) Uani 1.00 . . . C16 C 0.410(2) 0.111(1) 1.074(3) 0.098(5) Uani 1.00 . . . C17 C 0.420(1) 0.1862(9) 1.088(2) 0.072(4) Uani 1.00 . . . C18 C 0.536(1) 0.216(1) 1.164(2) 0.087(5) Uani 1.00 . . . C19 C 0.548(1) 0.286(1) 1.167(2) 0.094(6) Uani 1.00 . . . C20 C 0.453(1) 0.3282(9) 1.112(2) 0.075(4) Uani 1.00 . . . C21 C 0.465(2) 0.402(1) 1.117(3) 0.103(6) Uani 1.00 . . . C22 C 0.368(3) 0.444(1) 1.066(3) 0.121(8) Uani 1.00 . . . C23 C 0.255(2) 0.421(1) 1.002(3) 0.111(7) Uani 1.00 . . . C24 C 0.237(2) 0.350(1) 0.983(2) 0.092(5) Uani 1.00 . . . C25 C 0.333(1) 0.3044(8) 1.039(2) 0.064(3) Uani 1.00 . . . C26 C 0.319(1) 0.2306(8) 1.026(2) 0.066(3) Uani 1.00 . . . H1 H -0.0838 0.2887 0.3828 0.0575 Uiso 1.00 . . . H2 H -0.0725 0.2763 0.1817 0.0575 Uiso 1.00 . . . H3 H 0.1104 0.1075 0.3131 0.0574 Uiso 1.00 . . . H4 H 0.0546 0.1222 0.4723 0.0574 Uiso 1.00 . . . H5 H -0.1482 0.1836 0.3836 0.0729 Uiso 1.00 . . . H6 H -0.1997 0.1932 0.1559 0.0729 Uiso 1.00 . . . H7 H -0.0490 0.1326 0.0758 0.0758 Uiso 1.00 . . . H8 H -0.0940 0.0890 0.2116 0.0758 Uiso 1.00 . . . H9 H 0.2949 0.1139 0.5171 0.0575 Uiso 1.00 . . . H10 H 0.4987 0.0985 0.6361 0.0636 Uiso 1.00 . . . H11 H 0.6169 0.1946 0.6990 0.0745 Uiso 1.00 . . . H12 H 0.5281 0.3110 0.6564 0.0646 Uiso 1.00 . . . H13 H 0.4268 0.4104 0.5973 0.0623 Uiso 1.00 . . . H14 H 0.3048 0.5067 0.5217 0.0705 Uiso 1.00 . . . H15 H 0.1050 0.4949 0.4067 0.0763 Uiso 1.00 . . . H16 H 0.0205 0.3896 0.3676 0.0635 Uiso 1.00 . . . H17 H 0.1420 0.2173 0.9149 0.0865 Uiso 1.00 . . . H18 H 0.1237 0.1079 0.8802 0.0873 Uiso 1.00 . . . H19 H 0.2924 0.0406 1.0032 0.0961 Uiso 1.00 . . . H20 H 0.4783 0.0845 1.1107 0.0982 Uiso 1.00 . . . H21 H 0.6035 0.1821 1.2023 0.0866 Uiso 1.00 . . . H22 H 0.6226 0.3082 1.2115 0.0935 Uiso 1.00 . . . H23 H 0.5361 0.4291 1.1625 0.1025 Uiso 1.00 . . . H24 H 0.3785 0.4930 1.0680 0.1211 Uiso 1.00 . . . H25 H 0.1942 0.4618 0.9724 0.1112 Uiso 1.00 . . . H26 H 0.1594 0.3359 0.9345 0.0919 Uiso 1.00 . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt1 0.0384(2) 0.0431(2) 0.0449(2) 0.0029(1) 0.0137(1) 0.0061(1) P1 0.057(2) 0.067(2) 0.075(2) -0.001(1) 0.015(2) 0.018(2) P2 0.063(2) 0.049(2) 0.073(2) 0.007(1) 0.013(1) 0.008(1) F1 0.127(10) 0.14(1) 0.18(1) 0.064(8) 0.048(9) 0.074(10) F2 0.108(9) 0.22(2) 0.18(1) 0.041(9) 0.078(9) 0.13(1) F3 0.14(1) 0.12(1) 0.20(2) -0.015(9) 0.02(1) -0.03(1) F4 0.074(7) 0.18(1) 0.23(2) 0.040(7) 0.045(8) 0.12(1) F5 0.20(1) 0.15(1) 0.20(1) 0.03(1) 0.14(1) 0.07(1) F6 0.20(2) 0.23(2) 0.26(2) -0.08(2) 0.05(2) -0.15(2) F7 0.059(5) 0.142(10) 0.136(9) -0.026(5) 0.003(5) 0.036(7) F8 0.086(6) 0.092(7) 0.099(6) 0.034(5) 0.017(5) -0.004(5) F9 0.071(5) 0.087(6) 0.095(6) 0.015(4) 0.002(4) 0.029(5) F10 0.15(1) 0.103(9) 0.142(10) -0.058(8) 0.035(8) 0.015(7) F11 0.17(1) 0.13(1) 0.081(6) 0.076(8) 0.035(7) 0.006(6) F12 0.141(9) 0.084(6) 0.094(6) 0.063(6) 0.025(6) 0.026(5) N1 0.045(5) 0.054(6) 0.075(6) 0.004(4) 0.015(4) 0.017(5) N2 0.051(5) 0.057(6) 0.058(5) 0.002(4) 0.008(4) 0.000(4) N3 0.046(4) 0.055(5) 0.045(4) 0.005(4) 0.017(3) 0.006(4) N4 0.057(5) 0.042(4) 0.053(5) 0.002(4) 0.025(4) 0.005(4) C1 0.045(6) 0.070(9) 0.10(1) -0.007(6) 0.020(6) -0.005(7) C2 0.066(8) 0.070(9) 0.091(10) -0.013(6) 0.026(7) -0.011(7) C3 0.043(5) 0.067(7) 0.057(6) 0.002(5) 0.011(5) -0.002(5) C4 0.047(6) 0.064(7) 0.078(8) 0.016(5) 0.014(5) 0.015(6) C5 0.040(6) 0.11(1) 0.072(8) 0.006(6) 0.015(5) 0.007(7) C6 0.049(6) 0.087(9) 0.057(6) -0.006(6) 0.018(5) -0.001(6) C7 0.044(5) 0.065(7) 0.038(5) -0.008(4) 0.016(4) -0.003(4) C8 0.054(6) 0.055(6) 0.044(5) -0.007(5) 0.019(4) -0.003(4) C9 0.063(7) 0.068(8) 0.057(6) -0.014(6) 0.018(5) 0.000(5) C10 0.088(9) 0.051(7) 0.074(8) -0.008(6) 0.026(7) 0.003(6) C11 0.10(1) 0.054(7) 0.088(9) 0.016(7) 0.037(8) 0.022(7) C12 0.064(7) 0.055(7) 0.075(8) 0.011(5) 0.026(6) 0.010(6) C13 0.071(8) 0.15(2) 0.050(7) -0.034(9) 0.029(6) -0.005(8) C14 0.09(1) 0.11(1) 0.069(9) -0.04(1) 0.030(8) 0.000(8) C15 0.12(2) 0.08(1) 0.09(1) -0.02(1) 0.04(1) 0.003(9) C16 0.12(2) 0.11(2) 0.067(9) 0.00(1) 0.037(10) 0.009(9) C17 0.068(8) 0.10(1) 0.050(6) -0.010(7) 0.023(6) 0.004(7) C18 0.049(7) 0.15(2) 0.066(8) 0.001(8) 0.020(6) 0.009(9) C19 0.049(7) 0.17(2) 0.062(8) -0.022(9) 0.003(6) 0.03(1) C20 0.077(9) 0.10(1) 0.058(7) -0.013(8) 0.032(7) 0.001(7) C21 0.12(2) 0.13(2) 0.08(1) -0.03(1) 0.05(1) -0.01(1) C22 0.18(3) 0.11(2) 0.10(1) 0.00(2) 0.09(2) 0.00(1) C23 0.13(2) 0.12(2) 0.11(1) 0.03(1) 0.06(1) 0.03(1) C24 0.09(1) 0.13(2) 0.058(8) 0.01(1) 0.035(7) -0.001(9) C25 0.065(7) 0.094(10) 0.040(5) -0.002(6) 0.026(5) 0.002(6) C26 0.054(6) 0.10(1) 0.043(5) -0.016(6) 0.021(5) -0.005(6) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on 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 calculated 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. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor 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 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6885 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.2271 _refine_ls_goodness_of_fit_ref 1.282 _refine_ls_restrained_S_all 1.282 _refine_ls_shift/su_max 0.0690 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -2.22 _refine_diff_density_max 4.88 _refine_diff_density_rms 0.28 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PT1 N1 2.054(9) 1_555 1_555 yes PT1 N2 2.06(1) 1_555 1_555 yes PT1 N3 2.003(8) 1_555 1_555 yes PT1 N4 2.009(9) 1_555 1_555 yes P1 F1 1.58(1) 1_555 1_555 yes P1 F2 1.54(2) 1_555 1_555 yes P1 F3 1.52(1) 1_555 1_555 yes P1 F4 1.55(1) 1_555 1_555 yes P1 F5 1.56(2) 1_555 1_555 yes P1 F6 1.50(2) 1_555 1_555 yes P2 F7 1.58(1) 1_555 1_555 yes P2 F8 1.57(1) 1_555 1_555 yes P2 F9 1.577(10) 1_555 1_555 yes P2 F10 1.59(1) 1_555 1_555 yes P2 F11 1.57(1) 1_555 1_555 yes P2 F12 1.60(1) 1_555 1_555 yes N1 C1 1.49(2) 1_555 1_555 yes N1 H1 0.889 1_555 1_555 no N1 H2 0.874 1_555 1_555 no N2 C2 1.48(2) 1_555 1_555 yes N2 H3 0.874 1_555 1_555 no N2 H4 0.869 1_555 1_555 no N3 C3 1.31(2) 1_555 1_555 yes N3 C7 1.39(1) 1_555 1_555 yes N4 C8 1.37(1) 1_555 1_555 yes N4 C12 1.36(2) 1_555 1_555 yes C1 C2 1.53(2) 1_555 1_555 yes C1 H5 0.974 1_555 1_555 no C1 H6 0.921 1_555 1_555 no C2 H7 0.950 1_555 1_555 no C2 H8 0.947 1_555 1_555 no C3 C4 1.40(2) 1_555 1_555 yes C3 H9 0.975 1_555 1_555 no C4 C5 1.39(2) 1_555 1_555 yes C4 H10 0.986 1_555 1_555 no C5 C6 1.37(2) 1_555 1_555 yes C5 H11 0.946 1_555 1_555 no C6 C7 1.40(2) 1_555 1_555 yes C6 H12 0.991 1_555 1_555 no C7 C8 1.46(2) 1_555 1_555 yes C8 C9 1.38(2) 1_555 1_555 yes C9 C10 1.39(2) 1_555 1_555 yes C9 H13 0.948 1_555 1_555 no C10 C11 1.36(2) 1_555 1_555 yes C10 H14 0.953 1_555 1_555 no C11 C12 1.36(2) 1_555 1_555 yes C11 H15 0.958 1_555 1_555 no C12 H16 0.952 1_555 1_555 no C13 C14 1.34(3) 1_555 1_555 yes C13 C26 1.41(2) 1_555 1_555 yes C13 H17 0.884 1_555 1_555 no C14 C15 1.40(3) 1_555 1_555 yes C14 H18 0.962 1_555 1_555 no C15 C16 1.33(3) 1_555 1_555 yes C15 H19 0.881 1_555 1_555 no C16 C17 1.46(3) 1_555 1_555 yes C16 H20 0.924 1_555 1_555 no C17 C18 1.44(2) 1_555 1_555 yes C17 C26 1.42(2) 1_555 1_555 yes C18 C19 1.38(3) 1_555 1_555 yes C18 H21 0.997 1_555 1_555 no C19 C20 1.35(2) 1_555 1_555 yes C19 H22 0.958 1_555 1_555 no C20 C21 1.44(3) 1_555 1_555 yes C20 C25 1.44(2) 1_555 1_555 yes C21 C22 1.36(4) 1_555 1_555 yes C21 H23 0.976 1_555 1_555 no C22 C23 1.36(4) 1_555 1_555 yes C22 H24 0.961 1_555 1_555 no C23 C24 1.41(3) 1_555 1_555 yes C23 H25 1.030 1_555 1_555 no C24 C25 1.38(2) 1_555 1_555 yes C24 H26 0.927 1_555 1_555 no C25 C26 1.44(2) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 PT1 N2 82.9(4) 1_555 1_555 1_555 yes N1 PT1 N3 178.7(4) 1_555 1_555 1_555 yes N1 PT1 N4 97.6(4) 1_555 1_555 1_555 yes N2 PT1 N3 97.9(4) 1_555 1_555 1_555 yes N2 PT1 N4 178.8(4) 1_555 1_555 1_555 yes N3 PT1 N4 81.6(4) 1_555 1_555 1_555 yes F1 P1 F2 87.0(8) 1_555 1_555 1_555 yes F1 P1 F3 86.8(8) 1_555 1_555 1_555 yes F1 P1 F4 177.0(10) 1_555 1_555 1_555 yes F1 P1 F5 93.9(9) 1_555 1_555 1_555 yes F1 P1 F6 89.2(10) 1_555 1_555 1_555 yes F2 P1 F3 86.6(9) 1_555 1_555 1_555 yes F2 P1 F4 90.0(9) 1_555 1_555 1_555 yes F2 P1 F5 175.1(9) 1_555 1_555 1_555 yes F2 P1 F6 97(1) 1_555 1_555 1_555 yes F3 P1 F4 93.7(8) 1_555 1_555 1_555 yes F3 P1 F5 88.6(9) 1_555 1_555 1_555 yes F3 P1 F6 174(1) 1_555 1_555 1_555 yes F4 P1 F5 89.1(9) 1_555 1_555 1_555 yes F4 P1 F6 90.6(10) 1_555 1_555 1_555 yes F5 P1 F6 87(1) 1_555 1_555 1_555 yes F7 P2 F8 90.8(6) 1_555 1_555 1_555 yes F7 P2 F9 91.1(6) 1_555 1_555 1_555 yes F7 P2 F10 178.7(7) 1_555 1_555 1_555 yes F7 P2 F11 92.2(7) 1_555 1_555 1_555 yes F7 P2 F12 89.9(6) 1_555 1_555 1_555 yes F8 P2 F9 91.4(5) 1_555 1_555 1_555 yes F8 P2 F10 88.1(6) 1_555 1_555 1_555 yes F8 P2 F11 176.6(7) 1_555 1_555 1_555 yes F8 P2 F12 88.5(6) 1_555 1_555 1_555 yes F9 P2 F10 88.3(6) 1_555 1_555 1_555 yes F9 P2 F11 90.0(6) 1_555 1_555 1_555 yes F9 P2 F12 179.0(6) 1_555 1_555 1_555 yes F10 P2 F11 88.9(7) 1_555 1_555 1_555 yes F10 P2 F12 90.7(7) 1_555 1_555 1_555 yes F11 P2 F12 90.0(6) 1_555 1_555 1_555 yes PT1 N1 C1 110.9(7) 1_555 1_555 1_555 yes PT1 N1 H1 108.7(7) 1_555 1_555 1_555 no PT1 N1 H2 109.5(9) 1_555 1_555 1_555 no C1 N1 H1 109(1) 1_555 1_555 1_555 no C1 N1 H2 110.6(10) 1_555 1_555 1_555 no H1 N1 H2 107(1) 1_555 1_555 1_555 no PT1 N2 C2 109.5(8) 1_555 1_555 1_555 yes PT1 N2 H3 109.6(9) 1_555 1_555 1_555 no PT1 N2 H4 109.9(8) 1_555 1_555 1_555 no C2 N2 H3 109(1) 1_555 1_555 1_555 no C2 N2 H4 109(1) 1_555 1_555 1_555 no H3 N2 H4 109(1) 1_555 1_555 1_555 no PT1 N3 C3 127.9(8) 1_555 1_555 1_555 yes PT1 N3 C7 113.5(7) 1_555 1_555 1_555 yes C3 N3 C7 118.6(9) 1_555 1_555 1_555 yes PT1 N4 C8 115.1(7) 1_555 1_555 1_555 yes PT1 N4 C12 126.2(8) 1_555 1_555 1_555 yes C8 N4 C12 118.7(10) 1_555 1_555 1_555 yes N1 C1 C2 109(1) 1_555 1_555 1_555 yes N1 C1 H5 112(1) 1_555 1_555 1_555 no N1 C1 H6 115(1) 1_555 1_555 1_555 no C2 C1 H5 102(1) 1_555 1_555 1_555 no C2 C1 H6 105(1) 1_555 1_555 1_555 no H5 C1 H6 109(1) 1_555 1_555 1_555 no N2 C2 C1 107(1) 1_555 1_555 1_555 yes N2 C2 H7 110(1) 1_555 1_555 1_555 no N2 C2 H8 110(1) 1_555 1_555 1_555 no C1 C2 H7 107(1) 1_555 1_555 1_555 no C1 C2 H8 111(1) 1_555 1_555 1_555 no H7 C2 H8 109(1) 1_555 1_555 1_555 no N3 C3 C4 123(1) 1_555 1_555 1_555 yes N3 C3 H9 118(1) 1_555 1_555 1_555 no C4 C3 H9 117(1) 1_555 1_555 1_555 no C3 C4 C5 117(1) 1_555 1_555 1_555 yes C3 C4 H10 118(1) 1_555 1_555 1_555 no C5 C4 H10 123(1) 1_555 1_555 1_555 no C4 C5 C6 119(1) 1_555 1_555 1_555 yes C4 C5 H11 114(1) 1_555 1_555 1_555 no C6 C5 H11 125(1) 1_555 1_555 1_555 no C5 C6 C7 119(1) 1_555 1_555 1_555 yes C5 C6 H12 121(1) 1_555 1_555 1_555 no C7 C6 H12 118(1) 1_555 1_555 1_555 no N3 C7 C6 120(1) 1_555 1_555 1_555 yes N3 C7 C8 115.7(9) 1_555 1_555 1_555 yes C6 C7 C8 123(1) 1_555 1_555 1_555 yes N4 C8 C7 114.1(10) 1_555 1_555 1_555 yes N4 C8 C9 121(1) 1_555 1_555 1_555 yes C7 C8 C9 124(1) 1_555 1_555 1_555 yes C8 C9 C10 119(1) 1_555 1_555 1_555 yes C8 C9 H13 124(1) 1_555 1_555 1_555 no C10 C9 H13 116(1) 1_555 1_555 1_555 no C9 C10 C11 118(1) 1_555 1_555 1_555 yes C9 C10 H14 121(1) 1_555 1_555 1_555 no C11 C10 H14 119(1) 1_555 1_555 1_555 no C10 C11 C12 121(1) 1_555 1_555 1_555 yes C10 C11 H15 117(1) 1_555 1_555 1_555 no C12 C11 H15 120(1) 1_555 1_555 1_555 no N4 C12 C11 121(1) 1_555 1_555 1_555 yes N4 C12 H16 122(1) 1_555 1_555 1_555 no C11 C12 H16 116(1) 1_555 1_555 1_555 no C14 C13 C26 124(1) 1_555 1_555 1_555 yes C14 C13 H17 112(1) 1_555 1_555 1_555 no C26 C13 H17 122(2) 1_555 1_555 1_555 no C13 C14 C15 119(1) 1_555 1_555 1_555 yes C13 C14 H18 118(1) 1_555 1_555 1_555 no C15 C14 H18 122(2) 1_555 1_555 1_555 no C14 C15 C16 122(1) 1_555 1_555 1_555 yes C14 C15 H19 117(2) 1_555 1_555 1_555 no C16 C15 H19 120(2) 1_555 1_555 1_555 no C15 C16 C17 117(1) 1_555 1_555 1_555 yes C15 C16 H20 123(2) 1_555 1_555 1_555 no C17 C16 H20 118(2) 1_555 1_555 1_555 no C16 C17 C18 118(1) 1_555 1_555 1_555 yes C16 C17 C26 121(1) 1_555 1_555 1_555 yes C18 C17 C26 119(1) 1_555 1_555 1_555 yes C17 C18 C19 119(1) 1_555 1_555 1_555 yes C17 C18 H21 116(2) 1_555 1_555 1_555 no C19 C18 H21 123(1) 1_555 1_555 1_555 no C18 C19 C20 120(1) 1_555 1_555 1_555 yes C18 C19 H22 123(1) 1_555 1_555 1_555 no C20 C19 H22 115(2) 1_555 1_555 1_555 no C19 C20 C21 121(1) 1_555 1_555 1_555 yes C19 C20 C25 123(1) 1_555 1_555 1_555 yes C21 C20 C25 115(1) 1_555 1_555 1_555 yes C20 C21 C22 120(2) 1_555 1_555 1_555 yes C20 C21 H23 129(2) 1_555 1_555 1_555 no C22 C21 H23 110(2) 1_555 1_555 1_555 no C21 C22 C23 123(2) 1_555 1_555 1_555 yes C21 C22 H24 119(3) 1_555 1_555 1_555 no C23 C22 H24 117(2) 1_555 1_555 1_555 no C22 C23 C24 118(2) 1_555 1_555 1_555 yes C22 C23 H25 111(2) 1_555 1_555 1_555 no C24 C23 H25 129(2) 1_555 1_555 1_555 no C23 C24 C25 120(1) 1_555 1_555 1_555 yes C23 C24 H26 116(2) 1_555 1_555 1_555 no C25 C24 H26 123(2) 1_555 1_555 1_555 no C20 C25 C24 121(1) 1_555 1_555 1_555 yes C20 C25 C26 116(1) 1_555 1_555 1_555 yes C24 C25 C26 122(1) 1_555 1_555 1_555 yes C13 C26 C17 113(1) 1_555 1_555 1_555 yes C13 C26 C25 126(1) 1_555 1_555 1_555 yes C17 C26 C25 119(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag PT1 C13 3.59(2) 1_555 1_554 ? PT1 H17 3.46 1_555 1_554 ? F1 C10 3.33(2) 1_555 2_666 ? F1 C22 3.54(3) 1_555 2_667 ? F2 N1 3.18(2) 1_555 1_656 ? F2 C1 3.56(2) 1_555 1_656 ? F3 C1 3.35(2) 1_555 1_655 ? F3 N1 3.36(2) 1_555 1_655 ? F3 C19 3.51(2) 1_555 1_554 ? F4 N1 3.13(2) 1_555 1_656 ? F4 C24 3.51(2) 1_555 1_655 ? F5 N1 3.20(2) 1_555 1_655 ? F5 C12 3.34(3) 1_555 1_655 ? F5 C11 3.44(2) 1_555 2_666 ? F6 C23 3.53(3) 1_555 2_667 ? F7 N2 3.21(2) 1_555 1_655 ? F7 C2 3.36(2) 1_555 1_655 ? F7 C1 3.41(2) 1_555 1_655 ? F7 C14 3.46(2) 1_555 1_655 ? F8 C2 3.11(2) 1_555 1_656 ? F8 C1 3.46(2) 1_555 1_656 ? F9 C1 3.24(2) 1_555 1_655 ? F9 C18 3.52(2) 1_555 1_554 ? F9 C2 3.57(2) 1_555 1_655 ? F10 C3 3.18(2) 1_555 2_656 ? F10 C15 3.47(3) 1_555 2_657 ? F10 C4 3.50(2) 1_555 2_656 ? F11 N2 3.10(2) 1_555 2_656 ? F11 C14 3.41(2) 1_555 2_656 ? F11 C15 3.45(2) 1_555 2_656 ? F12 N2 2.98(1) 1_555 2_656 ? F12 C2 3.34(2) 1_555 2_656 ? F12 C2 3.43(2) 1_555 1_656 ? F12 C15 3.47(3) 1_555 2_657 ? F12 F12 3.51(2) 1_555 2_757 ? N3 C26 3.52(2) 1_555 1_554 ? N4 C24 3.55(2) 1_555 1_554 ? C3 C16 3.52(2) 1_555 1_554 ? C5 C18 3.42(2) 1_555 1_554 ? C6 C18 3.45(2) 1_555 1_554 ? C6 C19 3.54(2) 1_555 1_554 ? C7 C26 3.55(2) 1_555 1_554 ? C8 C25 3.44(2) 1_555 1_554 ? C8 C24 3.59(2) 1_555 1_554 ? C9 C22 3.60(3) 1_555 1_554 ? C10 C23 3.42(3) 1_555 1_554 ? C10 C22 3.49(3) 1_555 1_554 ? C11 C23 3.49(3) 1_555 1_554 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' Masako Kato' _publ_contact_author_address ; Division of Material Science Graduate School of Human Culture Nara Women's Univeristy Nara 630-8506, Japan ; _publ_contact_author_email ' kato@cc.nara-wu.ac.jp ' _publ_contact_author_fax ' +81-742-203393 ' _publ_contact_author_phone ' +81-742-203393' _publ_requested_journal ' J. Chem. Soc. Dalton Trans.' _publ_section_title ; Selective formation of the integrated stacks of (\a-diimine)(ethylenediamine)platinum(II) and neutral \p-systems of the phenanthrene-type ; #---------------------------------------------------------------------