# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 loop_ _publ_author_name 'Alan Sargeson' 'Kylie N. Brown' 'Rodney J. Geue' 'T. Hambley' 'David C. R. Hockless' 'A. David Rae' _publ_contact_author_name 'Prof Alan Sargeson' _publ_contact_author_address ; Research School of Chemistry Australian National University RSChem,ANU School of Chemistry,University of S Canberra ACT 0200 AUSTRALIA ; _publ_contact_author_email SARGESON@RSC.ANU.EDU.AU _publ_section_title ; Specificity inTemplate Syntheses of Hexa-aza-macrobicyclic Cages and Electrochemistry of [Pt(Me5-tricosatrieneN6)]4+ and [Pt(Me5-tricosaneN6)]4+ ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. Coppens, P., Leiserowitz, L., and Rabinovich, D., (1965) Acta Cryst., 18, 1035-1038. Rae, A.D. RAELS96 Australian National University, Canberra, ACT 0200, Australia. Rae, A.D. (1975). Acta Crystallographica, A31, 560-570. Rae, A.D. (1975). Acta Crystallographica, A31, 570-574. ; data_kb6 _database_code_CSD 202905 #------------------------------------------------------------------------------ _audit_creation_date 1999-09-23 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 23.502(9) _cell_length_b 15.453(3) _cell_length_c 13.680(4) _cell_angle_alpha 90 _cell_angle_beta 118.66(2) _cell_angle_gamma 90 _cell_volume 4360(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.0 _cell_measurement_theta_max 22.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c ' _symmetry_Int_Tables_number 9 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' 1/2+x, 1/2+y, +z' ' +x, -y, 1/2+z' ' 1/2+x, 1/2-y, 1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1194.20 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H54.123 Cl9.877 N6 O3.123 Pt Zn3 ' _chemical_formula_moiety ; (C22 H48 N6 Pt 4+)0.877, (C22 H47 N6 Pt 3+)0.123, (Cl3 H2 O Zn 1-)2.123, (Cl4 Zn 2-)0.877, (H2 O) ; _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2356.06 _exptl_absorpt_coefficient_mu 5.454 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.245 _exptl_absorpt_correction_T_min 0.153 _exptl_special_details ; The scan width was (0.80+0.34tan\q)\% with an \w scan speed of 4\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.66 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 0 0 0 2 0 1 1 3 _diffrn_reflns_number 4111 _reflns_number_total 4007 _reflns_number_gt 3276 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01522 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04404 _diffrn_orient_matrix_UB_12 -0.01263 _diffrn_orient_matrix_UB_13 -0.00921 _diffrn_orient_matrix_UB_21 -0.00578 _diffrn_orient_matrix_UB_22 0.06268 _diffrn_orient_matrix_UB_23 0.01120 _diffrn_orient_matrix_UB_31 -0.01947 _diffrn_orient_matrix_UB_32 0.00998 _diffrn_orient_matrix_UB_33 -0.08204 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 88 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 216 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 39 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 24 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 12 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 4 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Zn 0 12 0.222 1.431 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.5000 0.25005(2) 0.2500 0.03030(6) 1.000 . Uani d ? Zn(1) 0.68662(6) 0.08466(9) 0.6568(1) 0.0529(4) 0.877(6) . Uani d ? Zn(1') 0.6800(5) 0.1572(6) 0.6933(8) 0.053(3) 0.123 . Uiso d ? Zn(2) 0.30418(6) 0.04219(7) -0.0653(1) 0.0506(3) 1.000 . Uani d ? Zn(3) 0.42122(7) 0.60177(7) 0.2072(1) 0.0551(3) 1.000 . Uani d ? Cl(11) 0.7066(1) 0.1672(2) 0.5382(2) 0.0555(7) 1.000 . Uani d ? Cl(12) 0.5805(1) 0.1126(2) 0.6069(2) 0.0684(8) 1.000 . Uani d ? CL(13') 0.691(1) 0.300(1) 0.761(2) 0.079(7) 0.123 . Uiso d ? Cl(13) 0.7072(2) -0.0541(2) 0.6346(3) 0.084(1) 0.877 . Uani d ? Cl(14) 0.7460(2) 0.1266(4) 0.8346(3) 0.120(2) 0.877 . Uani d ? Cl(21) 0.4072(1) 0.0439(2) -0.0410(2) 0.0571(6) 1.000 . Uani d ? Cl(22) 0.3037(1) 0.1008(2) 0.0852(2) 0.0637(7) 1.000 . Uani d ? Cl(23) 0.2397(1) 0.1050(2) -0.2257(2) 0.0811(9) 1.000 . Uani d ? Cl(31) 0.4276(1) 0.5156(2) 0.3434(2) 0.0579(7) 1.000 . Uani d ? Cl(32) 0.4863(1) 0.5468(2) 0.1414(2) 0.0615(8) 1.000 . Uani d ? Cl(33) 0.4415(2) 0.7402(2) 0.2484(2) 0.085(1) 1.000 . Uani d ? O(1') 0.738(3) 0.063(3) 0.813(4) 0.063 0.123 PD Uiso d ? O(2) 0.2740(4) -0.0754(5) -0.0676(7) 0.084(2) 1.000 . Uani d ? O(3) 0.3263(4) 0.5814(6) 0.0881(6) 0.089(2) 1.000 . Uani d ? O(4) 0.3065(7) 0.1557(9) 0.623(1) 0.165(6) 1.000 . Uani d ? N(1) 0.5472(4) 0.3589(5) 0.2283(6) 0.043(2) 1.000 . Uani d ? N(2) 0.5361(4) 0.2697(5) 0.4226(6) 0.038(2) 1.000 . Uani d ? N(3) 0.4664(4) 0.2193(5) 0.0814(6) 0.036(2) 1.000 . Uani d ? N(4) 0.4222(4) 0.3271(5) 0.2227(6) 0.040(2) 1.000 . Uani d ? N(5) 0.5863(4) 0.1760(4) 0.2895(6) 0.039(2) 1.000 . Uani d ? N(6) 0.4498(3) 0.1428(5) 0.2606(6) 0.039(2) 1.000 . Uani d ? C(1) 0.6234(8) 0.2613(7) 0.057(1) 0.054(4) 1.000 . Uani d ? C(2) 0.5846(6) 0.2570(5) 0.126(1) 0.043(3) 1.000 . Uani d ? C(3) 0.5694(5) 0.3485(6) 0.1414(7) 0.043(2) 1.000 . Uani d ? C(4) 0.6019(4) 0.4009(6) 0.3336(8) 0.053(2) 1.000 . Uani d ? C(5) 0.5858(4) 0.4131(6) 0.4252(7) 0.048(2) 1.000 . Uani d ? C(6) 0.6342(6) 0.4815(7) 0.508(1) 0.073(4) 1.000 . Uani d ? C(7) 0.5903(4) 0.3293(6) 0.4832(7) 0.046(2) 1.000 . Uani d ? C(8) 0.4829(5) 0.2914(7) 0.4500(7) 0.048(3) 1.000 . Uani d ? C(9) 0.4227(8) 0.2422(6) 0.379(1) 0.048(3) 1.000 . Uani d ? C(10) 0.3859(8) 0.2372(8) 0.443(1) 0.061(4) 1.000 . Uani d ? C(11) 0.5182(4) 0.2077(6) 0.0490(7) 0.040(2) 1.000 . Uani d ? C(12) 0.4160(4) 0.2761(6) -0.0047(7) 0.041(2) 1.000 . Uani d ? C(13) 0.3600(4) 0.3032(6) 0.0138(7) 0.043(2) 1.000 . Uani d ? C(14) 0.3087(4) 0.3461(7) -0.0913(7) 0.055(3) 1.000 . Uani d ? C(15) 0.3807(4) 0.3670(6) 0.1070(7) 0.042(2) 1.000 . Uani d ? C(16) 0.3801(5) 0.2901(7) 0.2667(7) 0.044(3) 1.000 . Uani d ? C(17) 0.6235(5) 0.2078(6) 0.2320(8) 0.041(3) 1.000 . Uani d ? C(18) 0.5822(4) 0.0798(5) 0.2825(7) 0.046(2) 1.000 . Uani d ? C(19) 0.5443(5) 0.0420(6) 0.3321(7) 0.048(2) 1.000 . Uani d ? C(20) 0.5588(6) -0.0591(6) 0.346(1) 0.071(4) 1.000 . Uani d ? C(21) 0.4722(5) 0.0567(5) 0.2563(7) 0.047(2) 1.000 . Uani d ? C(22) 0.4329(5) 0.1504(6) 0.3520(8) 0.045(2) 1.000 . Uani d ? H(91) 0.5145 0.4020 0.1983 0.051 1.000 . Uiso c ? H(92) 0.5517 0.2147 0.4556 0.046 1.000 . Uiso c ? H(93) 0.4464 0.1641 0.0712 0.044 1.000 . Uiso c ? H(94) 0.4418 0.3758 0.2691 0.048 1.000 . Uiso c ? H(95) 0.6142 0.1875 0.3662 0.047 1.000 . Uiso c ? H(96) 0.4090 0.1464 0.1949 0.047 1.000 . Uiso c ? H(1a) 0.6321 0.2042 0.0418 0.065 1.000 . Uiso c ? H(1b) 0.5982 0.2910 -0.0112 0.065 1.000 . Uiso c ? H(1c) 0.6632 0.2911 0.0995 0.065 1.000 . Uiso c ? H(3a) 0.6073 0.3824 0.1635 0.052 1.000 . Uiso c ? H(3b) 0.5359 0.3692 0.0722 0.052 1.000 . Uiso c ? H(4a) 0.6392 0.3651 0.3601 0.063 1.000 . Uiso c ? H(4b) 0.6112 0.4559 0.3138 0.063 1.000 . Uiso c ? H(5) 0.5428 0.4349 0.3951 0.058 1.000 . Uiso c ? H(6a) 0.6773 0.4600 0.5381 0.088 1.000 . Uiso c ? H(6b) 0.6306 0.5339 0.4689 0.088 1.000 . Uiso c ? H(6c) 0.6242 0.4920 0.5662 0.088 1.000 . Uiso c ? H(7a) 0.6290 0.3009 0.4953 0.055 1.000 . Uiso c ? H(7b) 0.5925 0.3419 0.5529 0.055 1.000 . Uiso c ? H(8a) 0.4971 0.2776 0.5260 0.057 1.000 . Uiso c ? H(8b) 0.4738 0.3515 0.4385 0.057 1.000 . Uiso c ? H(10a) 0.3764 0.2940 0.4569 0.073 1.000 . Uiso c ? H(10b) 0.3467 0.2064 0.4000 0.073 1.000 . Uiso c ? H(10c) 0.4114 0.2081 0.5112 0.073 1.000 . Uiso c ? H(11a) 0.5020 0.2282 -0.0252 0.048 1.000 . Uiso c ? H(11b) 0.5274 0.1477 0.0515 0.048 1.000 . Uiso c ? H(12a) 0.3984 0.2462 -0.0738 0.049 1.000 . Uiso c ? H(12b) 0.4371 0.3273 -0.0092 0.049 1.000 . Uiso c ? H(13) 0.3421 0.2536 0.0300 0.051 1.000 . Uiso c ? H(14a) 0.3263 0.3964 -0.1065 0.066 1.000 . Uiso c ? H(14b) 0.2948 0.3069 -0.1519 0.066 1.000 . Uiso c ? H(14c) 0.2728 0.3619 -0.0812 0.066 1.000 . Uiso c ? H(15a) 0.4052 0.4112 0.0962 0.051 1.000 . Uiso c ? H(15b) 0.3430 0.3914 0.1046 0.051 1.000 . Uiso c ? H(16a) 0.3503 0.2503 0.2141 0.053 1.000 . Uiso c ? H(16b) 0.3569 0.3355 0.2787 0.053 1.000 . Uiso c ? H(17a) 0.6419 0.1589 0.2155 0.049 1.000 . Uiso c ? H(17b) 0.6572 0.2447 0.2824 0.049 1.000 . Uiso c ? H(18a) 0.5624 0.0636 0.2062 0.056 1.000 . Uiso c ? H(18b) 0.6249 0.0570 0.3203 0.056 1.000 . Uiso c ? H(19) 0.5572 0.0675 0.4029 0.057 1.000 . Uiso c ? H(20a) 0.5336 -0.0856 0.3753 0.085 1.000 . Uiso c ? H(20b) 0.5480 -0.0838 0.2758 0.085 1.000 . Uiso c ? H(20c) 0.6036 -0.0683 0.3960 0.085 1.000 . Uiso c ? H(21a) 0.4628 0.0455 0.1818 0.056 1.000 . Uiso c ? H(21b) 0.4490 0.0170 0.2771 0.056 1.000 . Uiso c ? H(22a) 0.4671 0.1255 0.4173 0.054 1.000 . Uiso c ? H(22b) 0.3940 0.1190 0.3311 0.054 1.000 . Uiso c ? 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 Pt(1) 0.0329(1) 0.0309(1) 0.0238(1) -0.0014(1) 0.01094(9) -0.0011(1) Zn(1) 0.0439(7) 0.0638(8) 0.0408(6) -0.0059(6) 0.0121(5) 0.0091(6) Zn(2) 0.0427(5) 0.0488(6) 0.0499(6) -0.0015(5) 0.0138(5) -0.0063(5) Zn(3) 0.0720(7) 0.0508(6) 0.0381(6) 0.0136(6) 0.0228(5) 0.0052(5) Cl(11) 0.050(1) 0.069(2) 0.047(1) 0.007(1) 0.022(1) 0.013(1) Cl(12) 0.049(1) 0.110(2) 0.043(1) 0.007(1) 0.019(1) 0.016(1) Cl(13) 0.087(2) 0.060(2) 0.103(3) 0.001(2) 0.044(2) 0.012(2) Cl(14) 0.103(3) 0.178(5) 0.035(1) -0.040(3) -0.003(2) 0.003(2) Cl(21) 0.046(1) 0.061(1) 0.060(1) -0.005(1) 0.021(1) -0.025(1) Cl(22) 0.057(1) 0.070(2) 0.068(2) -0.017(1) 0.033(1) -0.026(1) Cl(23) 0.057(2) 0.113(2) 0.062(2) 0.026(2) 0.019(1) 0.027(2) Cl(31) 0.076(2) 0.057(1) 0.048(1) 0.020(1) 0.036(1) 0.012(1) Cl(32) 0.088(2) 0.049(1) 0.064(1) 0.010(1) 0.049(1) 0.008(1) Cl(33) 0.140(3) 0.054(1) 0.053(2) 0.003(2) 0.040(2) -0.007(1) O(2) 0.114(7) 0.049(3) 0.079(5) -0.025(4) 0.039(5) -0.011(4) O(3) 0.070(3) 0.118(7) 0.058(5) 0.010(5) 0.014(3) 0.017(5) O(4) 0.22(1) 0.20(1) 0.123(9) -0.10(1) 0.12(1) -0.057(9) N(1) 0.055(5) 0.040(4) 0.034(4) -0.016(3) 0.021(3) -0.001(3) N(2) 0.051(4) 0.032(3) 0.021(2) 0.004(3) 0.009(3) 0.005(3) N(3) 0.039(4) 0.042(4) 0.026(2) -0.001(3) 0.014(3) -0.007(3) N(4) 0.036(4) 0.051(5) 0.028(3) 0.014(3) 0.013(3) 0.004(3) N(5) 0.036(4) 0.037(3) 0.035(4) 0.012(3) 0.010(3) 0.002(3) N(6) 0.037(4) 0.036(3) 0.033(4) -0.007(2) 0.008(3) 0.003(3) C(1) 0.064(8) 0.070(8) 0.047(8) -0.015(6) 0.042(7) -0.004(5) C(2) 0.034(5) 0.046(5) 0.045(6) -0.006(3) 0.015(4) -0.005(3) C(3) 0.042(5) 0.046(4) 0.035(5) 0.005(5) 0.013(4) 0.005(4) C(4) 0.039(5) 0.059(6) 0.053(5) -0.014(4) 0.016(4) -0.027(4) C(5) 0.038(4) 0.047(4) 0.050(5) 0.007(4) 0.013(4) 0.001(3) C(6) 0.077(7) 0.064(7) 0.088(8) -0.034(6) 0.047(7) -0.048(6) C(7) 0.042(5) 0.050(4) 0.032(4) 0.001(4) 0.005(4) -0.006(3) C(8) 0.058(5) 0.054(6) 0.033(5) 0.007(5) 0.024(4) -0.005(4) C(9) 0.066(7) 0.049(5) 0.025(5) -0.002(4) 0.018(4) 0.002(3) C(10) 0.056(8) 0.080(9) 0.062(9) 0.013(6) 0.042(7) 0.006(6) C(11) 0.039(5) 0.048(5) 0.033(5) -0.011(4) 0.018(4) -0.010(4) C(12) 0.042(4) 0.047(5) 0.026(4) -0.001(3) 0.011(3) 0.001(3) C(13) 0.040(4) 0.054(5) 0.034(4) -0.007(4) 0.018(3) 0.005(3) C(14) 0.036(5) 0.083(7) 0.035(5) 0.004(5) 0.008(4) 0.008(4) C(15) 0.042(5) 0.047(5) 0.031(3) 0.001(4) 0.012(3) 0.012(3) C(16) 0.041(5) 0.063(6) 0.030(5) 0.011(5) 0.019(4) 0.010(4) C(17) 0.044(5) 0.034(5) 0.049(5) -0.007(4) 0.026(4) -0.009(4) C(18) 0.054(5) 0.035(3) 0.045(5) 0.010(4) 0.021(4) -0.001(4) C(19) 0.062(4) 0.043(4) 0.031(4) 0.007(4) 0.017(3) 0.000(4) C(20) 0.106(9) 0.042(4) 0.086(8) 0.006(5) 0.064(8) 0.018(5) C(21) 0.060(4) 0.033(4) 0.043(5) -0.006(4) 0.021(4) 0.001(4) C(22) 0.052(6) 0.048(4) 0.034(5) -0.014(5) 0.020(4) -0.003(4) #------------------------------------------------------------------------------ _refine_special_details ; H atoms of the cation were placed at geometrically determined positions. H atoms of anions and solvate molecules were not located. Refinement of a model with all coordinates transformed by (-x,-y,-z) gave almost identical agreement factors. The first anion appears to be disordered ZnCl4(2-) (occ = p) and ZnCl3(H2O)- (occ = 1-p) with Cl11 and Cl12 common to both species. The relative occupancies were refined and restraints placed on Zn1'-Cl13' and Zn1'-O1' distances. The disorder above infers p(cation)4+ and (1-p)(cation)3+; the latter being attained by deprotonation of a N atom. The (cation)3+ species is consistant with the orange colour of the bulk sample. All N's in the structure are tetrahedral and a H of occ 1.0 is attached to each in our model. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.0004|Fo|^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 3276 _refine_ls_number_parameters 416 _refine_ls_number_restraints 2 _refine_ls_number_constraints 5 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_all 0.0379 _refine_ls_wR_factor_ref 0.0364 _refine_ls_goodness_of_fit_all 1.619 _refine_ls_goodness_of_fit_ref 1.704 _refine_ls_shift/su_max 0.0500 _refine_ls_shift/su_mean 0.0560 _refine_diff_density_min -0.56 _refine_diff_density_max 0.86 #------------------------------------------------------------------------------ _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 Pt(1) N(1) 2.113(9) . . yes Pt(1) N(2) 2.11(1) . . yes Pt(1) N(3) 2.102(9) . . yes Pt(1) N(4) 2.059(9) . . yes Pt(1) N(5) 2.159(9) . . yes Pt(1) N(6) 2.079(9) . . yes Zn(1) Zn(1') 1.27(1) . . yes Zn(1) Cl(11) 2.282(3) . . yes Zn(1) Cl(12) 2.288(4) . . yes Zn(1) Cl(13) 2.252(5) . . yes Zn(1) Cl(14) 2.242(5) . . yes Zn(1) O(1') 1.91(5) . . yes Zn(1') Cl(11) 2.49(1) . . yes Zn(1') Cl(12) 2.16(1) . . yes Zn(1') CL(13') 2.36(2) . . yes Zn(1') Cl(14) 1.87(1) . . yes Zn(1') O(1') 2.12(2) . . yes Zn(2) Cl(21) 2.280(4) . . yes Zn(2) Cl(22) 2.254(4) . . yes Zn(2) Cl(23) 2.205(4) . . yes Zn(2) O(2) 1.945(9) . . yes Zn(3) Cl(31) 2.235(3) . . yes Zn(3) Cl(32) 2.278(4) . . yes Zn(3) Cl(33) 2.205(4) . . yes Zn(3) O(3) 2.06(1) . . yes Cl(14) O(1') 1.01(7) . . yes N(1) C(3) 1.52(2) . . yes N(1) C(4) 1.54(1) . . yes N(1) H(91) 0.95 . . no N(2) C(7) 1.47(1) . . yes N(2) C(8) 1.50(2) . . yes N(2) H(92) 0.95 . . no N(3) C(11) 1.50(1) . . yes N(3) C(12) 1.49(1) . . yes N(3) H(93) 0.95 . . no N(4) C(15) 1.53(1) . . yes N(4) C(16) 1.50(2) . . yes N(4) H(94) 0.95 . . no N(5) C(17) 1.51(2) . . yes N(5) C(18) 1.49(1) . . yes N(5) H(95) 0.95 . . no N(6) C(21) 1.44(1) . . yes N(6) C(22) 1.49(1) . . yes N(6) H(96) 0.95 . . no C(1) C(2) 1.59(2) . . yes C(1) H(1c) 0.95 . . no C(1) H(1a) 0.95 . . no C(1) H(1b) 0.95 . . no C(2) C(3) 1.50(2) . . yes C(2) C(11) 1.59(2) . . yes C(2) C(17) 1.50(2) . . yes C(3) H(3a) 0.95 . . no C(3) H(3b) 0.95 . . no C(4) C(5) 1.48(2) . . yes C(4) H(4a) 0.95 . . no C(4) H(4b) 0.95 . . no C(5) C(6) 1.57(2) . . yes C(5) C(7) 1.50(2) . . yes C(5) H(5) 0.95 . . no C(6) H(6c) 0.95 . . no C(6) H(6a) 0.95 . . no C(6) H(6b) 0.95 . . no C(7) H(7b) 0.95 . . no C(7) H(7a) 0.95 . . no C(8) C(9) 1.48(2) . . yes C(8) H(8a) 0.95 . . no C(8) H(8b) 0.95 . . no C(9) C(10) 1.49(3) . . yes C(9) C(16) 1.56(2) . . yes C(9) C(22) 1.51(2) . . yes C(10) H(10a) 0.95 . . no C(10) H(10b) 0.95 . . no C(10) H(10c) 0.95 . . no C(11) H(11b) 0.95 . . no C(11) H(11a) 0.95 . . no C(12) C(13) 1.51(2) . . yes C(12) H(12a) 0.95 . . no C(12) H(12b) 0.95 . . no C(13) C(14) 1.52(2) . . yes C(13) C(15) 1.50(2) . . yes C(13) H(13) 0.95 . . no C(14) H(14a) 0.95 . . no C(14) H(14b) 0.95 . . no C(14) H(14c) 0.95 . . no C(15) H(15b) 0.95 . . no C(15) H(15a) 0.95 . . no C(16) H(16a) 0.95 . . no C(16) H(16b) 0.95 . . no C(17) H(17a) 0.95 . . no C(17) H(17b) 0.95 . . no C(18) C(19) 1.47(2) . . yes C(18) H(18b) 0.95 . . no C(18) H(18a) 0.95 . . no C(19) C(20) 1.59(2) . . yes C(19) C(21) 1.52(2) . . yes C(19) H(19) 0.95 . . no C(20) H(20a) 0.95 . . no C(20) H(20b) 0.95 . . no C(20) H(20c) 0.95 . . no C(21) H(21a) 0.95 . . no C(21) H(21b) 0.95 . . no C(22) H(22b) 0.95 . . no C(22) H(22a) 0.95 . . no #------------------------------------------------------------------------------ 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 N(1) Pt(1) N(2) 95.0(4) . . . yes N(1) Pt(1) N(3) 88.4(4) . . . yes N(1) Pt(1) N(4) 89.7(4) . . . yes N(1) Pt(1) N(5) 87.9(4) . . . yes N(1) Pt(1) N(6) 176.4(4) . . . yes N(2) Pt(1) N(3) 175.1(5) . . . yes N(2) Pt(1) N(4) 88.0(4) . . . yes N(2) Pt(1) N(5) 88.3(4) . . . yes N(2) Pt(1) N(6) 88.5(4) . . . yes N(3) Pt(1) N(4) 95.6(4) . . . yes N(3) Pt(1) N(5) 88.2(4) . . . yes N(3) Pt(1) N(6) 88.2(4) . . . yes N(4) Pt(1) N(5) 175.4(5) . . . yes N(4) Pt(1) N(6) 89.4(4) . . . yes N(5) Pt(1) N(6) 93.2(4) . . . yes Zn(1') Zn(1) Cl(11) 83.8(5) . . . yes Zn(1') Zn(1) Cl(12) 68.2(6) . . . yes Zn(1') Zn(1) Cl(13) 166.2(6) . . . yes Zn(1') Zn(1) Cl(14) 56.4(6) . . . yes Zn(1') Zn(1) O(1') 81(2) . . . yes Cl(11) Zn(1) Cl(12) 104.4(1) . . . yes Cl(11) Zn(1) Cl(13) 107.8(2) . . . yes Cl(11) Zn(1) Cl(14) 112.1(2) . . . yes Cl(11) Zn(1) O(1') 131(3) . . . yes Cl(12) Zn(1) Cl(13) 114.5(2) . . . yes Cl(12) Zn(1) Cl(14) 106.9(2) . . . yes Cl(12) Zn(1) O(1') 113(2) . . . yes Cl(13) Zn(1) Cl(14) 111.1(3) . . . yes Cl(13) Zn(1) O(1') 86(2) . . . yes Cl(14) Zn(1) O(1') 27(2) . . . yes Zn(1) Zn(1') Cl(11) 65.8(5) . . . yes Zn(1) Zn(1') Cl(12) 78.9(6) . . . yes Zn(1) Zn(1') CL(13') 166(1) . . . yes Zn(1) Zn(1') Cl(14) 89.2(7) . . . yes Zn(1) Zn(1') O(1') 63(2) . . . yes Cl(11) Zn(1') Cl(12) 101.6(5) . . . yes Cl(11) Zn(1') CL(13') 104.5(9) . . . yes Cl(11) Zn(1') Cl(14) 118.3(6) . . . yes Cl(11) Zn(1') O(1') 111(2) . . . yes Cl(12) Zn(1') CL(13') 113.5(9) . . . yes Cl(12) Zn(1') Cl(14) 128.9(6) . . . yes Cl(12) Zn(1') O(1') 109(2) . . . yes CL(13') Zn(1') Cl(14) 87(1) . . . yes CL(13') Zn(1') O(1') 115(3) . . . yes Cl(14) Zn(1') O(1') 29(2) . . . yes Cl(21) Zn(2) Cl(22) 109.4(1) . . . yes Cl(21) Zn(2) Cl(23) 108.4(2) . . . yes Cl(21) Zn(2) O(2) 111.5(4) . . . yes Cl(22) Zn(2) Cl(23) 115.5(2) . . . yes Cl(22) Zn(2) O(2) 103.2(3) . . . yes Cl(23) Zn(2) O(2) 108.9(4) . . . yes Cl(31) Zn(3) Cl(32) 108.5(1) . . . yes Cl(31) Zn(3) Cl(33) 116.4(1) . . . yes Cl(31) Zn(3) O(3) 100.5(3) . . . yes Cl(32) Zn(3) Cl(33) 111.0(2) . . . yes Cl(32) Zn(3) O(3) 108.0(3) . . . yes Cl(33) Zn(3) O(3) 111.7(4) . . . yes Zn(1) Cl(11) Zn(1') 30.4(3) . . . yes Zn(1) Cl(12) Zn(1') 32.9(3) . . . yes Zn(1) Cl(14) Zn(1') 34.4(4) . . . yes Zn(1) Cl(14) O(1') 58(3) . . . yes Zn(1') Cl(14) O(1') 90(3) . . . yes Zn(1) O(1') Zn(1') 36.1(6) . . . yes Zn(1) O(1') Cl(14) 95(2) . . . yes Zn(1') O(1') Cl(14) 62(1) . . . yes Pt(1) N(1) C(3) 115.3(7) . . . yes Pt(1) N(1) C(4) 117.6(7) . . . yes Pt(1) N(1) H(91) 104.3 . . . no C(3) N(1) C(4) 109.4(9) . . . yes C(3) N(1) H(91) 104.3 . . . no C(4) N(1) H(91) 104.3 . . . no Pt(1) N(2) C(7) 119.7(8) . . . yes Pt(1) N(2) C(8) 112.0(8) . . . yes Pt(1) N(2) H(92) 105.0 . . . no C(7) N(2) C(8) 108.7(9) . . . yes C(7) N(2) H(92) 105.0 . . . no C(8) N(2) H(92) 105.0 . . . no Pt(1) N(3) C(11) 114.9(7) . . . yes Pt(1) N(3) C(12) 118.2(7) . . . yes Pt(1) N(3) H(93) 105.3 . . . no C(11) N(3) C(12) 106.7(9) . . . yes C(11) N(3) H(93) 105.3 . . . no C(12) N(3) H(93) 105.3 . . . no Pt(1) N(4) C(15) 119.3(7) . . . yes Pt(1) N(4) C(16) 114.0(7) . . . yes Pt(1) N(4) H(94) 103.6 . . . no C(15) N(4) C(16) 110.6(9) . . . yes C(15) N(4) H(94) 103.6 . . . no C(16) N(4) H(94) 103.6 . . . no Pt(1) N(5) C(17) 113.9(7) . . . yes Pt(1) N(5) C(18) 119.3(8) . . . yes Pt(1) N(5) H(95) 104.3 . . . no C(17) N(5) C(18) 109.0(9) . . . yes C(17) N(5) H(95) 104.3 . . . no C(18) N(5) H(95) 104.3 . . . no Pt(1) N(6) C(21) 120.1(7) . . . yes Pt(1) N(6) C(22) 112.7(7) . . . yes Pt(1) N(6) H(96) 103.7 . . . no C(21) N(6) C(22) 110.9(9) . . . yes C(21) N(6) H(96) 103.7 . . . no C(22) N(6) H(96) 103.7 . . . no C(2) C(1) H(1c) 109.5 . . . no C(2) C(1) H(1a) 109.5 . . . no C(2) C(1) H(1b) 109.5 . . . no H(1c) C(1) H(1a) 109.5 . . . no H(1c) C(1) H(1b) 109.5 . . . no H(1a) C(1) H(1b) 109.5 . . . no C(1) C(2) C(3) 107(1) . . . yes C(1) C(2) C(11) 107(1) . . . yes C(1) C(2) C(17) 110(1) . . . yes C(3) C(2) C(11) 109(1) . . . yes C(3) C(2) C(17) 114(1) . . . yes C(11) C(2) C(17) 110(1) . . . yes N(1) C(3) C(2) 114(1) . . . yes N(1) C(3) H(3a) 108.3 . . . no N(1) C(3) H(3b) 108.3 . . . no C(2) C(3) H(3a) 108.3 . . . no C(2) C(3) H(3b) 108.3 . . . no H(3a) C(3) H(3b) 109.5 . . . no N(1) C(4) C(5) 114(1) . . . yes N(1) C(4) H(4a) 108.3 . . . no N(1) C(4) H(4b) 108.3 . . . no C(5) C(4) H(4a) 108.3 . . . no C(5) C(4) H(4b) 108.3 . . . no H(4a) C(4) H(4b) 109.5 . . . no C(4) C(5) C(6) 108(1) . . . yes C(4) C(5) C(7) 111(1) . . . yes C(4) C(5) H(5) 109.1 . . . no C(6) C(5) C(7) 111(1) . . . yes C(6) C(5) H(5) 109.1 . . . no C(7) C(5) H(5) 109.1 . . . no C(5) C(6) H(6c) 109.5 . . . no C(5) C(6) H(6a) 109.5 . . . no C(5) C(6) H(6b) 109.5 . . . no H(6c) C(6) H(6a) 109.5 . . . no H(6c) C(6) H(6b) 109.5 . . . no H(6a) C(6) H(6b) 109.5 . . . no N(2) C(7) C(5) 115.0(9) . . . yes N(2) C(7) H(7b) 108.1 . . . no N(2) C(7) H(7a) 108.1 . . . no C(5) C(7) H(7b) 108.1 . . . no C(5) C(7) H(7a) 108.1 . . . no H(7b) C(7) H(7a) 109.5 . . . no N(2) C(8) C(9) 112(1) . . . yes N(2) C(8) H(8a) 108.9 . . . no N(2) C(8) H(8b) 108.9 . . . no C(9) C(8) H(8a) 109.0 . . . no C(9) C(8) H(8b) 108.9 . . . no H(8a) C(8) H(8b) 109.5 . . . no C(8) C(9) C(10) 106(1) . . . yes C(8) C(9) C(16) 111(1) . . . yes C(8) C(9) C(22) 115(2) . . . yes C(10) C(9) C(16) 109(2) . . . yes C(10) C(9) C(22) 107(1) . . . yes C(16) C(9) C(22) 108(1) . . . yes C(9) C(10) H(10a) 109.5 . . . no C(9) C(10) H(10b) 109.5 . . . no C(9) C(10) H(10c) 109.5 . . . no H(10a) C(10) H(10b) 109.5 . . . no H(10a) C(10) H(10c) 109.5 . . . no H(10b) C(10) H(10c) 109.5 . . . no N(3) C(11) C(2) 115(1) . . . yes N(3) C(11) H(11b) 108.0 . . . no N(3) C(11) H(11a) 108.0 . . . no C(2) C(11) H(11b) 108.0 . . . no C(2) C(11) H(11a) 108.0 . . . no H(11b) C(11) H(11a) 109.5 . . . no N(3) C(12) C(13) 117.0(9) . . . yes N(3) C(12) H(12a) 107.6 . . . no N(3) C(12) H(12b) 107.6 . . . no C(13) C(12) H(12a) 107.6 . . . no C(13) C(12) H(12b) 107.6 . . . no H(12a) C(12) H(12b) 109.5 . . . no C(12) C(13) C(14) 108.8(9) . . . yes C(12) C(13) C(15) 111.8(9) . . . yes C(12) C(13) H(13) 109.5 . . . no C(14) C(13) C(15) 108(1) . . . yes C(14) C(13) H(13) 109.5 . . . no C(15) C(13) H(13) 109.5 . . . no C(13) C(14) H(14a) 109.5 . . . no C(13) C(14) H(14b) 109.5 . . . no C(13) C(14) H(14c) 109.5 . . . no H(14a) C(14) H(14b) 109.5 . . . no H(14a) C(14) H(14c) 109.5 . . . no H(14b) C(14) H(14c) 109.5 . . . no N(4) C(15) C(13) 113.6(9) . . . yes N(4) C(15) H(15b) 108.4 . . . no N(4) C(15) H(15a) 108.4 . . . no C(13) C(15) H(15b) 108.4 . . . no C(13) C(15) H(15a) 108.4 . . . no H(15b) C(15) H(15a) 109.5 . . . no N(4) C(16) C(9) 110(1) . . . yes N(4) C(16) H(16a) 109.4 . . . no N(4) C(16) H(16b) 109.4 . . . no C(9) C(16) H(16a) 109.3 . . . no C(9) C(16) H(16b) 109.4 . . . no H(16a) C(16) H(16b) 109.5 . . . no N(5) C(17) C(2) 116(1) . . . yes N(5) C(17) H(17a) 107.9 . . . no N(5) C(17) H(17b) 107.9 . . . no C(2) C(17) H(17a) 107.9 . . . no C(2) C(17) H(17b) 107.9 . . . no H(17a) C(17) H(17b) 109.5 . . . no N(5) C(18) C(19) 113.6(9) . . . yes N(5) C(18) H(18b) 108.4 . . . no N(5) C(18) H(18a) 108.4 . . . no C(19) C(18) H(18b) 108.4 . . . no C(19) C(18) H(18a) 108.4 . . . no H(18b) C(18) H(18a) 109.5 . . . no C(18) C(19) C(20) 108(1) . . . yes C(18) C(19) C(21) 110.4(9) . . . yes C(18) C(19) H(19) 109.8 . . . no C(20) C(19) C(21) 109(1) . . . yes C(20) C(19) H(19) 109.8 . . . no C(21) C(19) H(19) 109.8 . . . no C(19) C(20) H(20a) 109.5 . . . no C(19) C(20) H(20b) 109.5 . . . no C(19) C(20) H(20c) 109.5 . . . no H(20a) C(20) H(20b) 109.5 . . . no H(20a) C(20) H(20c) 109.5 . . . no H(20b) C(20) H(20c) 109.5 . . . no N(6) C(21) C(19) 114.8(9) . . . yes N(6) C(21) H(21a) 108.1 . . . no N(6) C(21) H(21b) 108.1 . . . no C(19) C(21) H(21a) 108.1 . . . no C(19) C(21) H(21b) 108.1 . . . no H(21a) C(21) H(21b) 109.5 . . . no N(6) C(22) C(9) 115(1) . . . yes N(6) C(22) H(22b) 108.2 . . . no N(6) C(22) H(22a) 108.2 . . . no C(9) C(22) H(22b) 108.2 . . . no C(9) C(22) H(22a) 108.2 . . . no H(22b) C(22) H(22a) 109.5 . . . no #------------------------------------------------------------------------------ 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 Cl(11) N(5) 3.22(1) . . no Cl(11) C(7) 3.51(1) . . no Cl(11) C(18) 3.58(1) . . no Cl(12) N(2) 3.29(1) . . no Cl(12) C(8) 3.57(1) . . no Cl(12) C(22) 3.60(1) . . no CL(13') O(2) 2.93(3) . 2_556 no CL(13') C(7) 3.41(3) . . no Cl(13) O(3) 3.18(1) . 4 no Cl(14) O(3) 3.13(1) . 2_546 no Cl(14) C(10) 3.57(2) . 4 no Cl(21) N(3) 3.14(1) . . no Cl(21) C(11) 3.41(1) . . no Cl(21) C(22) 3.52(1) . 3_554 no Cl(21) C(21) 3.60(1) . . no Cl(22) N(6) 3.17(1) . . no Cl(22) C(22) 3.54(1) . . no Cl(22) C(21) 3.57(1) . . no Cl(23) O(4) 3.24(1) . 1_554 no Cl(23) C(1) 3.57(2) . 4_454 no Cl(23) C(3) 3.59(1) . 4_454 no Cl(31) N(4) 3.32(1) . . no Cl(32) N(1) 3.20(1) . . no Cl(32) C(4) 3.54(1) . . no Cl(32) C(8) 3.59(1) . 3_564 no Cl(33) O(4) 3.22(2) . 3_564 no O(1') O(3) 3.33(7) . 2_546 no O(2) O(4) 2.64(2) . 3_554 no O(2) C(10) 3.58(2) . 3_554 no O(3) C(15) 3.52(2) . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pt(1) N(1) C(3) C(2) . . . . -28(1) no Pt(1) N(1) C(4) C(5) . . . . -45(1) no Pt(1) N(2) C(7) C(5) . . . . 44(1) no Pt(1) N(2) C(8) C(9) . . . . 37(1) no Pt(1) N(3) C(11) C(2) . . . . -25(1) no Pt(1) N(3) C(12) C(13) . . . . -44(1) no Pt(1) N(4) C(15) C(13) . . . . 49(1) no Pt(1) N(4) C(16) C(9) . . . . 37(1) no Pt(1) N(5) C(17) C(2) . . . . -25(1) no Pt(1) N(5) C(18) C(19) . . . . -44(1) no Pt(1) N(6) C(21) C(19) . . . . 48(1) no Pt(1) N(6) C(22) C(9) . . . . 30(1) no Zn(1) Zn(1') Cl(14) O(1') . . . . -21(5) no Zn(1) Zn(1') O(1') Cl(14) . . . . 156(5) no Zn(1) Cl(11) Zn(1') Cl(12) . . . . -72.1(5) no Zn(1) Cl(11) Zn(1') CL(13') . . . . 170(1) no Zn(1) Cl(11) Zn(1') Cl(14) . . . . 74.9(7) no Zn(1) Cl(11) Zn(1') O(1') . . . . 44(3) no Zn(1) Cl(12) Zn(1') Cl(11) . . . . 62.2(5) no Zn(1) Cl(12) Zn(1') CL(13') . . . . 174(1) no Zn(1) Cl(12) Zn(1') Cl(14) . . . . -79.8(9) no Zn(1) Cl(12) Zn(1') O(1') . . . . -56(2) no Zn(1) Cl(14) Zn(1') Cl(11) . . . . -61.7(6) no Zn(1) Cl(14) Zn(1') Cl(12) . . . . 75.0(8) no Zn(1) Cl(14) Zn(1') CL(13') . . . . -167(1) no Zn(1) Cl(14) Zn(1') O(1') . . . . 21(5) no Zn(1) Cl(14) O(1') Zn(1') . . . . -14(3) no Zn(1) O(1') Zn(1') Cl(11) . . . . -46(2) no Zn(1) O(1') Zn(1') Cl(12) . . . . 66(2) no Zn(1) O(1') Zn(1') CL(13') . . . . -165(1) no Zn(1) O(1') Zn(1') Cl(14) . . . . -156(5) no Zn(1) O(1') Cl(14) Zn(1') . . . . 14(3) no Zn(1') Zn(1) Cl(14) O(1') . . . . 155(5) no Zn(1') Zn(1) O(1') Cl(14) . . . . -21(4) no Zn(1') Cl(11) Zn(1) Cl(12) . . . . 65.5(6) no Zn(1') Cl(11) Zn(1) Cl(13) . . . . -172.4(6) no Zn(1') Cl(11) Zn(1) Cl(14) . . . . -49.9(6) no Zn(1') Cl(11) Zn(1) O(1') . . . . -73(3) no Zn(1') Cl(12) Zn(1) Cl(11) . . . . -77.1(6) no Zn(1') Cl(12) Zn(1) Cl(13) . . . . 165.3(6) no Zn(1') Cl(12) Zn(1) Cl(14) . . . . 41.8(6) no Zn(1') Cl(12) Zn(1) O(1') . . . . 70(3) no Zn(1') Cl(14) Zn(1) Cl(11) . . . . 65.8(7) no Zn(1') Cl(14) Zn(1) Cl(12) . . . . -48.0(7) no Zn(1') Cl(14) Zn(1) Cl(13) . . . . -173.5(7) no Zn(1') Cl(14) Zn(1) O(1') . . . . -155(5) no Zn(1') O(1') Zn(1) Cl(11) . . . . 74(2) no Zn(1') O(1') Zn(1) Cl(12) . . . . -62(1) no Zn(1') O(1') Zn(1) Cl(13) . . . . -176.4(8) no Zn(1') O(1') Zn(1) Cl(14) . . . . 21(4) no Cl(11) Zn(1) Zn(1') Cl(12) . . . . 108.2(3) no Cl(11) Zn(1) Zn(1') CL(13') . . . . -47(5) no Cl(11) Zn(1) Zn(1') Cl(14) . . . . -121.8(4) no Cl(11) Zn(1) Zn(1') O(1') . . . . -133(3) no Cl(11) Zn(1) Cl(14) O(1') . . . . -139(5) no Cl(11) Zn(1) O(1') Cl(14) . . . . 53(6) no Cl(11) Zn(1') Zn(1) Cl(12) . . . . -108.2(3) no Cl(11) Zn(1') Zn(1) Cl(13) . . . . 148(2) no Cl(11) Zn(1') Zn(1) Cl(14) . . . . 121.8(4) no Cl(11) Zn(1') Zn(1) O(1') . . . . 133(3) no Cl(11) Zn(1') Cl(14) O(1') . . . . -83(5) no Cl(11) Zn(1') O(1') Cl(14) . . . . 110(4) no Cl(12) Zn(1) Zn(1') CL(13') . . . . -155(5) no Cl(12) Zn(1) Zn(1') Cl(14) . . . . 130.0(6) no Cl(12) Zn(1) Zn(1') O(1') . . . . 119(3) no Cl(12) Zn(1) Cl(14) O(1') . . . . 107(5) no Cl(12) Zn(1) O(1') Cl(14) . . . . -83(5) no Cl(12) Zn(1') Zn(1) Cl(13) . . . . -104(2) no Cl(12) Zn(1') Zn(1) Cl(14) . . . . -130.0(6) no Cl(12) Zn(1') Zn(1) O(1') . . . . -119(3) no Cl(12) Zn(1') Cl(14) O(1') . . . . 54(5) no Cl(12) Zn(1') O(1') Cl(14) . . . . -138(4) no CL(13') Zn(1') Zn(1) Cl(13) . . . . 101(5) no CL(13') Zn(1') Zn(1) Cl(14) . . . . 75(5) no CL(13') Zn(1') Zn(1) O(1') . . . . 86(6) no CL(13') Zn(1') Cl(14) O(1') . . . . 172(5) no CL(13') Zn(1') O(1') Cl(14) . . . . -9(5) no Cl(13) Zn(1) Zn(1') Cl(14) . . . . 26(3) no Cl(13) Zn(1) Zn(1') O(1') . . . . 15(4) no Cl(13) Zn(1) Cl(14) O(1') . . . . -19(5) no Cl(13) Zn(1) O(1') Cl(14) . . . . 163(5) no Cl(14) Zn(1) Zn(1') O(1') . . . . -11(3) no Cl(14) Zn(1') Zn(1) O(1') . . . . 11(3) no N(1) Pt(1) N(2) C(7) . . . . -14.7(9) no N(1) Pt(1) N(2) C(8) . . . . 114.3(8) no N(1) Pt(1) N(3) C(11) . . . . 57.0(9) no N(1) Pt(1) N(3) C(12) . . . . -70.4(8) no N(1) Pt(1) N(4) C(15) . . . . 66.7(8) no N(1) Pt(1) N(4) C(16) . . . . -159.5(8) no N(1) Pt(1) N(5) C(17) . . . . -30.0(7) no N(1) Pt(1) N(5) C(18) . . . . -161.1(8) no N(1) Pt(1) N(6) C(21) . . . . 91(8) no N(1) Pt(1) N(6) C(22) . . . . -135(7) no N(1) C(3) C(2) C(1) . . . . -166(1) no N(1) C(3) C(2) C(11) . . . . 79(2) no N(1) C(3) C(2) C(17) . . . . -44(2) no N(1) C(4) C(5) C(6) . . . . -162(1) no N(1) C(4) C(5) C(7) . . . . 77(1) no N(2) Pt(1) N(1) C(3) . . . . 146.2(9) no N(2) Pt(1) N(1) C(4) . . . . 14.9(9) no N(2) Pt(1) N(3) C(11) . . . . -76(6) no N(2) Pt(1) N(3) C(12) . . . . 156(6) no N(2) Pt(1) N(4) C(15) . . . . 161.7(9) no N(2) Pt(1) N(4) C(16) . . . . -64.5(8) no N(2) Pt(1) N(5) C(17) . . . . -125.0(8) no N(2) Pt(1) N(5) C(18) . . . . 103.8(8) no N(2) Pt(1) N(6) C(21) . . . . -105.6(8) no N(2) Pt(1) N(6) C(22) . . . . 27.9(8) no N(2) C(7) C(5) C(4) . . . . -76(1) no N(2) C(7) C(5) C(6) . . . . 164(1) no N(2) C(8) C(9) C(10) . . . . 156(1) no N(2) C(8) C(9) C(16) . . . . -86(1) no N(2) C(8) C(9) C(22) . . . . 37(2) no N(3) Pt(1) N(1) C(3) . . . . -30.2(9) no N(3) Pt(1) N(1) C(4) . . . . -161.5(9) no N(3) Pt(1) N(2) C(7) . . . . 119(6) no N(3) Pt(1) N(2) C(8) . . . . -112(6) no N(3) Pt(1) N(4) C(15) . . . . -21.7(9) no N(3) Pt(1) N(4) C(16) . . . . 112.1(8) no N(3) Pt(1) N(5) C(17) . . . . 58.5(8) no N(3) Pt(1) N(5) C(18) . . . . -72.7(8) no N(3) Pt(1) N(6) C(21) . . . . 70.7(8) no N(3) Pt(1) N(6) C(22) . . . . -155.7(8) no N(3) C(11) C(2) C(1) . . . . -163(1) no N(3) C(11) C(2) C(3) . . . . -48(2) no N(3) C(11) C(2) C(17) . . . . 78(1) no N(3) C(12) C(13) C(14) . . . . -170(1) no N(3) C(12) C(13) C(15) . . . . 71(1) no N(4) Pt(1) N(1) C(3) . . . . -125.8(9) no N(4) Pt(1) N(1) C(4) . . . . 102.9(8) no N(4) Pt(1) N(2) C(7) . . . . -104.2(9) no N(4) Pt(1) N(2) C(8) . . . . 24.8(8) no N(4) Pt(1) N(3) C(11) . . . . 146.6(8) no N(4) Pt(1) N(3) C(12) . . . . 19.2(9) no N(4) Pt(1) N(5) C(17) . . . . -88(5) no N(4) Pt(1) N(5) C(18) . . . . 140(5) no N(4) Pt(1) N(6) C(21) . . . . 166.4(8) no N(4) Pt(1) N(6) C(22) . . . . -60.1(8) no N(4) C(15) C(13) C(12) . . . . -72(1) no N(4) C(15) C(13) C(14) . . . . 168.3(9) no N(4) C(16) C(9) C(8) . . . . 41(2) no N(4) C(16) C(9) C(10) . . . . 158(1) no N(4) C(16) C(9) C(22) . . . . -86(1) no N(5) Pt(1) N(1) C(3) . . . . 58.1(8) no N(5) Pt(1) N(1) C(4) . . . . -73.2(9) no N(5) Pt(1) N(2) C(7) . . . . 73.1(8) no N(5) Pt(1) N(2) C(8) . . . . -157.9(8) no N(5) Pt(1) N(3) C(11) . . . . -30.9(8) no N(5) Pt(1) N(3) C(12) . . . . -158.3(8) no N(5) Pt(1) N(4) C(15) . . . . 125(5) no N(5) Pt(1) N(4) C(16) . . . . -101(5) no N(5) Pt(1) N(6) C(21) . . . . -17.4(8) no N(5) Pt(1) N(6) C(22) . . . . 116.2(8) no N(5) C(17) C(2) C(1) . . . . -163(1) no N(5) C(17) C(2) C(3) . . . . 77(2) no N(5) C(17) C(2) C(11) . . . . -46(2) no N(5) C(18) C(19) C(20) . . . . -166(1) no N(5) C(18) C(19) C(21) . . . . 75(1) no N(6) Pt(1) N(1) C(3) . . . . -51(8) no N(6) Pt(1) N(1) C(4) . . . . 178(7) no N(6) Pt(1) N(2) C(7) . . . . 166.4(9) no N(6) Pt(1) N(2) C(8) . . . . -64.6(8) no N(6) Pt(1) N(3) C(11) . . . . -124.2(9) no N(6) Pt(1) N(3) C(12) . . . . 108.4(8) no N(6) Pt(1) N(4) C(15) . . . . -109.9(9) no N(6) Pt(1) N(4) C(16) . . . . 23.9(8) no N(6) Pt(1) N(5) C(17) . . . . 146.6(8) no N(6) Pt(1) N(5) C(18) . . . . 15.5(8) no N(6) C(21) C(19) C(18) . . . . -78(1) no N(6) C(21) C(19) C(20) . . . . 164(1) no N(6) C(22) C(9) C(8) . . . . -80(2) no N(6) C(22) C(9) C(10) . . . . 162(1) no N(6) C(22) C(9) C(16) . . . . 45(2) no C(2) C(3) N(1) C(4) . . . . 107(1) no C(2) C(11) N(3) C(12) . . . . 108(1) no C(2) C(17) N(5) C(18) . . . . 111(1) no C(3) N(1) C(4) C(5) . . . . -179(1) no C(5) C(7) N(2) C(8) . . . . -86(1) no C(7) N(2) C(8) C(9) . . . . 172(1) no C(9) C(16) N(4) C(15) . . . . 175(1) no C(9) C(22) N(6) C(21) . . . . 168(1) no C(11) N(3) C(12) C(13) . . . . -175.7(9) no C(13) C(15) N(4) C(16) . . . . -86(1) no C(17) N(5) C(18) C(19) . . . . -177.6(9) no C(19) C(21) N(6) C(22) . . . . -87(1) no #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_d _geom_bond_atom_site_label_h _geom_contact_atom_site_label_a _geom_bond_distance_dh _geom_contact_distance_ha _geom_contact_distance_da _geom_angle_dha _geom_contact_site_symmetry_a N(1) H(91) Cl(32) 0.95 2.36 3.21(1) 148.4 . N(2) H(92) Cl(12) 0.95 2.42 3.29(1) 151.0 . N(3) H(93) Cl(21) 0.95 2.30 3.14(1) 146.6 . N(4) H(94) Cl(31) 0.95 2.48 3.32(1) 148.0 . N(5) H(95) Cl(11) 0.95 2.34 3.22(1) 154.7 . N(6) H(96) Cl(22) 0.95 2.31 3.18(1) 151.5 . N(1) H(91) N(4) 0.95 2.62 2.95(1) 100.6 . N(3) H(93) N(6) 0.95 2.58 2.91(1) 101.1 . N(5) H(95) N(2) 0.95 2.63 2.98(1) 101.9 . data_PTTRIIMINE _database_code_CSD 205497 #------------------------------------------------------------------------------ _audit_creation_date 1999-06-03 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'RAELS96, (Rae, 1996)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 14.724(5) _cell_length_b 14.724(5) _cell_length_c 55.80(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 10476(6) _cell_formula_units_Z 12 _cell_measurement_temperature 294.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? #------------------------------------------------------------------------------ _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_Int_Tables_number 167 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 -y,-x,1/2+z 5 x,x-y,1/2+z 6 -x+y,y,1/2+z 7 -x,-y,-z 8 y,-x+y,-z 9 x-y,x,-z 10 y,x,1/2-z 11 -x,-x+y,1/2-z 12 x-y,-y,1/2-z 13 1/3+x,2/3+y,2/3+z 14 1/3-y,2/3+x-y,2/3+z 15 1/3-x+y,2/3-x,2/3+z 16 1/3-y,2/3-x,7/6+z 17 1/3+x,2/3+x-y,7/6+z 18 1/3-x+y,2/3+y,7/6+z 19 1/3-x,2/3-y,2/3-z 20 1/3+y,2/3-x+y,2/3-z 21 1/3+x-y,2/3+x,2/3-z 22 1/3+y,2/3+x,7/6-z 23 1/3-x,2/3-x+y,7/6-z 24 1/3+x-y,2/3-y,7/6-z 25 2/3+x,1/3+y,1/3+z 26 2/3-y,1/3+x-y,1/3+z 27 2/3-x+y,1/3-x,1/3+z 28 2/3-y,1/3-x,5/6+z 29 2/3+x,1/3+x-y,5/6+z 30 2/3-x+y,1/3+y,5/6+z 31 2/3-x,1/3-y,1/3-z 32 2/3+y,1/3-x+y,1/3-z 33 2/3+x-y,1/3+x,1/3-z 34 2/3+y,1/3+x,5/6-z 35 2/3-x,1/3-x+y,5/6-z 36 2/3+x-y,1/3-y,5/6-z #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 967.98 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H46 Cl7 N6 O2 Pt1 Zn1.5 ' _chemical_formula_moiety '(C22 H42 N6 Pt 4+), (Cl4 Zn 2-)1.5, (Cl 1-), 2(H2 O)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 5736.00 _exptl_absorpt_coefficient_mu 5.573 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; Coppens et al (1965) ; _exptl_absorpt_correction_T_max 0.408 _exptl_absorpt_correction_T_min 0.108 #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type Nonius-CAD4 _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_decay_% -8.1 _diffrn_reflns_number 6497 _reflns_number_total 2066 _reflns_number_gt 1480 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 66 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 264 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 552 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 24 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 84 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 72 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 12 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Zn 0 18 0.222 1.431 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt1 0.0000 0.0000 0.36249(1) 0.0256(3) 1.0 . Uani d ? N1 0.1066(6) -0.0081(5) 0.3847(1) 0.033(2) 1.0 . Uani d ? N2 0.1175(5) 0.1100(5) 0.3407(1) 0.031(2) 1.0 . Uani d ? C1 0.0000 0.0000 0.4462(4) 0.063(7) 1.0 . Uani d ? C2 0.0000 0.0000 0.4180(4) 0.040(5) 1.0 . Uani d ? C3 0.0691(7) -0.0439(7) 0.4097(2) 0.038(2) 1.0 . Uani d ? C4 0.2015(6) 0.0207(6) 0.3793(2) 0.039(2) 1.0 . Uani d ? C5 0.2558(7) 0.0720(7) 0.3570(2) 0.041(2) 1.0 . Uani d ? C6 0.3733(8) 0.1252(9) 0.3586(2) 0.065(3) 1.0 . Uani d ? C7 0.2256(7) 0.1542(7) 0.3497(2) 0.045(2) 1.0 . Uani d ? C8 0.1108(8) 0.0746(7) 0.3151(2) 0.036(2) 1.0 . Uani d ? C9 0.0000 0.0000 0.3066(3) 0.032(4) 1.0 . Uani d ? C10 0.0000 0.0000 0.2791(4) 0.047(5) 1.0 . Uani d ? Zn1 0.0326(2) 0.3212(2) 0.2380(1) 0.082(2) 0.5 . Uani d ? Cl1 0.0045(5) 0.4514(3) 0.2471(1) 0.061(2) 0.5 . Uani d ? Cl2 0.1088(7) 0.2874(8) 0.2681(1) 0.205(7) 0.5 . Uani d ? Cl3 0.1399(5) 0.3721(5) 0.2066(1) 0.109(3) 0.5 . Uani d ? Cl4 -0.1121(4) 0.1815(4) 0.2255(1) 0.165(6) 0.5 . Uani d ? Cl5 0.1556(6) 0.3219(6) 0.3226(2) 0.063(3) 0.3333 . Uani d ? O1 0.1472(38) 0.3197(38) 0.3285(13) 0.063(3) 0.1667 . Uani d ? O2 0.2889(10) 0.2566(8) 0.2585(2) 0.084(6) 0.5 . Uani d ? H1(O1) 0.1357 0.3111 0.3108 0.063 0.1667 . Uani c ? H2(O1) 0.2223 0.3719 0.3319 0.063 0.1667 . Uani c ? H1(O2) 0.2224 0.2588 0.2599 0.084 0.5 . Uani c ? H2(O2) 0.2797 0.2027 0.2463 0.084 0.5 . Uani c ? H1(N2) 0.1046 0.1705 0.3400 0.031 1.0 . Uani c ? H1(C1) -0.0449 0.0285 0.4522 0.063 1.0 . Uani c ? H1(C3) 0.1309 -0.0184 0.4207 0.038 1.0 . Uani c ? H2(C3) 0.0278 -0.1222 0.4101 0.038 1.0 . Uani c ? H1(C4) 0.2430 0.0070 0.3915 0.039 1.0 . Uani c ? H1(C5) 0.2319 0.0177 0.3441 0.041 1.0 . Uani c ? H1(C6) 0.4049 0.1583 0.3429 0.065 1.0 . Uani c ? H2(C6) 0.3988 0.1805 0.3713 0.065 1.0 . Uani c ? H3(C6) 0.3944 0.0723 0.3628 0.065 1.0 . Uani c ? H1(C7) 0.2336 0.1982 0.3641 0.045 1.0 . Uani c ? H2(C7) 0.2749 0.1994 0.3369 0.045 1.0 . Uani c ? H1(C8) 0.1527 0.0384 0.3135 0.036 1.0 . Uani c ? H2(C8) 0.1417 0.1380 0.3045 0.036 1.0 . Uani c ? H1(C10) -0.0725 -0.0488 0.2731 0.047 1.0 . Uani c ? 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 0.0212(4) 0.0212(4) 0.0345(5) 0.0106(2) 0.000 0.000 N1 0.033(3) 0.026(3) 0.039(3) 0.013(3) -0.004(3) -0.001(3) N2 0.020(3) 0.028(3) 0.042(3) 0.011(2) 0.001(2) 0.002(3) C1 0.082(9) 0.082(9) 0.026(8) 0.041(5) 0.000 0.000 C2 0.044(7) 0.044(7) 0.033(9) 0.022(3) 0.000 0.000 C3 0.045(5) 0.037(4) 0.035(4) 0.023(4) -0.004(3) 0.000(3) C4 0.032(4) 0.034(4) 0.056(5) 0.021(3) -0.012(4) -0.007(4) C5 0.041(4) 0.051(5) 0.047(5) 0.035(4) 0.007(3) 0.004(4) C6 0.038(5) 0.080(7) 0.078(7) 0.031(5) 0.002(5) 0.005(5) C7 0.032(4) 0.033(5) 0.058(5) 0.008(4) 0.003(4) -0.010(4) C8 0.034(5) 0.033(4) 0.038(5) 0.014(4) 0.000(4) 0.000(3) C9 0.029(5) 0.029(5) 0.038(8) 0.015(3) 0.000 0.000 C10 0.053(7) 0.053(7) 0.036(9) 0.026(3) 0.000 0.000 Zn1 0.069(2) 0.071(2) 0.114(5) 0.040(2) -0.010(1) -0.015(2) Cl1 0.050(2) 0.070(2) 0.064(4) 0.031(2) -0.003(2) -0.015(2) Cl2 0.324(12) 0.165(5) 0.199(8) 0.176(7) -0.083(6) 0.012(4) Cl3 0.081(5) 0.098(3) 0.146(7) 0.043(3) 0.013(3) -0.055(3) Cl4 0.065(3) 0.078(2) 0.334(13) 0.022(2) 0.010(4) -0.072(3) Cl5 0.050(4) 0.023(3) 0.116(6) 0.018(3) 0.044(4) 0.030(4) O1 0.050(4) 0.023(3) 0.116(6) 0.018(3) 0.044(4) 0.030(4) O2 0.070(7) 0.070(7) 0.087(13) 0.017(7) 0.027(4) -0.027(4) H1(O1) 0.050 0.023 0.116 0.018 0.044 0.030 H2(O1) 0.050 0.023 0.116 0.018 0.044 0.030 H1(O2) 0.070 0.070 0.087 0.017 0.027 -0.027 H2(O2) 0.070 0.070 0.087 0.017 0.027 -0.027 H1(N2) 0.020 0.028 0.042 0.011 0.001 0.002 H1(C1) 0.082 0.082 0.026 0.041 0.000 0.000 H1(C3) 0.045 0.037 0.035 0.023 -0.004 0.000 H2(C3) 0.045 0.037 0.035 0.023 -0.004 0.000 H1(C4) 0.032 0.034 0.056 0.021 -0.012 -0.007 H1(C5) 0.041 0.051 0.047 0.035 0.007 0.004 H1(C6) 0.038 0.080 0.078 0.031 0.002 0.005 H2(C6) 0.038 0.080 0.078 0.031 0.002 0.005 H3(C6) 0.038 0.080 0.078 0.031 0.002 0.005 H1(C7) 0.032 0.033 0.058 0.008 0.003 -0.010 H2(C7) 0.032 0.033 0.058 0.008 0.003 -0.010 H1(C8) 0.034 0.033 0.038 0.014 0.000 0.000 H2(C8) 0.034 0.033 0.038 0.014 0.000 0.000 H1(C10) 0.053 0.053 0.036 0.026 0.000 0.000 #------------------------------------------------------------------------------ _refine_special_details ; Hydrogen atoms were given the same thermal parameters as the atoms to which they were attached. They were included in chemically sensible positions which were recalculated each refinement cycle. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.0016|Fo|^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 1480 _refine_ls_number_parameters 137 _refine_ls_number_restraints 7 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_all 0.1020 _refine_ls_wR_factor_ref 0.0880 _refine_ls_goodness_of_fit_all 1.932 _refine_ls_goodness_of_fit_ref 1.964 _refine_ls_shift/esd_max 0.1 _refine_ls_shift/esd_mean 0.04 _refine_diff_density_min -0.8 _refine_diff_density_max 1.2 #------------------------------------------------------------------------------ _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 N1 Pt1 2.050(7) . . yes N2 Pt1 2.072(6) . . yes C2 C1 1.575(27) . . yes C3 N1 1.497(11) . . yes C3 C2 1.525(12) . . yes C4 N1 1.277(10) . . yes C5 C4 1.470(12) . . yes C6 C5 1.503(13) . . yes C7 N2 1.475(11) . . yes C7 C5 1.538(13) . . yes C8 N2 1.508(11) . . yes C9 C8 1.517(11) . . yes C10 C9 1.533(27) . . yes Cl1 Zn1 2.214(4) . . yes Cl2 Zn1 2.210(5) . . yes Cl3 Zn1 2.224(7) . . yes Cl4 Zn1 2.207(5) . . yes Cl5 Cl2 3.106(12) . . yes O1 Cl2 3.414(70) . . yes O2 Cl2 2.954(14) . . yes Cl4 O2 2.840(7) . 2_555 yes O2 Cl4 2.840(7) . 3_555 yes N2 Cl5 3.052(10) . . yes N2 O1 2.972(52) . . yes N2 Cl5 3.115(10) . 19_555 yes N2 O1 3.113(50) . 19_555 yes O1 Cl4 3.049(70) . 11_555 yes Cl4 O1 3.049(70) . 11_555 yes Cl4 Cl5 3.978(12) . 29_454 yes Cl4 O1 3.681(69) . 29_454 yes Cl2 Cl5 4.343(12) . 19_555 yes Cl4 Cl5 2.742(12) . 11_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 92.1(3) . . . yes N1 Pt1 N1 87.2(3) . . 2_555 yes N2 Pt1 N2 89.0(3) . . 2_555 yes N1 Pt1 N2 178.7(2) . . 2_555 yes N1 Pt1 N2 91.7(3) . . 3_555 yes Pt1 N1 C3 115.3(6) . . . yes Pt1 N1 C4 125.5(6) . . . yes C3 N1 C4 119.0(7) . . . yes Pt1 N2 C7 116.0(5) . . . yes Pt1 N2 C8 113.7(5) . . . yes C7 N2 C8 110.3(6) . . . yes C1 C2 C3 107.6(8) . . . yes N1 C3 C2 109.9(10) . . . yes N1 C4 C5 126.4(8) . . . yes C4 C5 C6 113.9(8) . . . yes C4 C5 C7 109.3(6) . . . yes C6 C5 C7 108.5(8) . . . yes N2 C7 C5 114.6(7) . . . yes N2 C8 C9 114.0(9) . . . yes C8 C9 C10 108.2(8) . . . yes Cl1 Zn1 Cl2 110.9(3) . . . yes Cl1 Zn1 Cl3 107.3(3) . . . yes Cl1 Zn1 Cl4 111.6(3) . . . yes Cl2 Zn1 Cl3 108.6(3) . . . yes Cl2 Zn1 Cl4 113.1(3) . . . yes Cl3 Zn1 Cl4 104.9(3) . . . yes Zn1 Cl2 Cl5 143.5(4) . . . yes Zn1 Cl2 O1 141.9(9) . . . yes Zn1 Cl2 O2 119.5(4) . . . yes Cl5 Cl2 O2 93.5(3) . . . yes O1 Cl2 O2 95.8(9) . . . yes Pt1 N2 Cl5 130.4(3) . . . yes C3 N2 Cl5 136.4(3) . . . yes C4 N2 Cl5 139.3(3) . . . yes Pt1 N2 O1 125.3(12) . . . yes C3 N2 O1 130.1(14) . . . yes C4 N2 O1 136.0(12) . . . yes Pt1 N2 Cl5 119.7(3) . . 19_555 yes C3 N2 Cl5 114.0(3) . . 19_555 yes C4 N2 Cl5 118.5(3) . . 19_555 yes Pt1 N2 O1 125.4(12) . . 19_555 yes C3 N2 O1 120.1(13) . . 19_555 yes C4 N2 O1 122.3(11) . . 19_555 yes N2 Cl5 Cl2 104.1(3) . . . yes N2 Cl5 Cl2 99.1(3) . 19_555 19_555 yes N2 O1 Cl2 92.8(16) . 19_555 19_555 yes Cl2 O2 Cl4 126.3(4) . . 3_555 yes Cl4 O2 Cl2 126.3(4) . 2_555 2_555 yes N2 Cl5 Cl4 105.0(3) . . 11_555 yes N2 O1 Cl4 99.6(17) . . 11_555 yes N2 Cl5 Cl4 79.8(3) . 19_555 11_555 yes N2 O1 Cl4 84.8(14) . 19_555 11_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 Pt1 N2 155.7(5) . . . . no C4 N1 Pt1 N2 -19.6(7) . . . . no C7 N2 Pt1 N1 -9.4(6) . . . . no C8 N2 Pt1 N1 120.0(5) . . . . no C2 C3 N1 Pt1 -37.0(8) . . . . no C2 C3 N1 C4 138.6(8) . . . . no C5 C4 N1 Pt1 4.6(12) . . . . no C5 C4 N1 C3 -170.5(8) . . . . no C5 C7 N2 Pt1 52.7(8) . . . . no C5 C7 N2 C8 -78.3(8) . . . . no C9 C8 N2 Pt1 30.4(8) . . . . no C9 C8 N2 C7 162.7(7) . . . . no N1 C3 C2 C1 202.2(5) . . . . no C6 C5 C4 N1 162.5(9) . . . . no C7 C5 C4 N1 41.1(12) . . . . no N2 C7 C5 C4 -72.1(9) . . . . no N2 C7 C5 C6 163.2(8) . . . . no C10 C9 C8 N2 -198.9(5) . . . . no O1 Cl2 Zn1 Cl1 21.1(15) . . . . no O1 Cl2 Zn1 Cl3 138.8(14) . . . . no O1 Cl2 Zn1 Cl4 -105.1(14) . . . . no