#==================================================================== ========== data_global #==================================================================== ========== _audit_creation_date 14-03-96 _audit_creation_method from_MolEN_master_file_using_cif_in _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; P.E. Fanwick Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; _publ_contact_author_email 'fanwick@.xray.chem.purdue.edu' _publ_contact_author_fax '(317) 494 0239' _publ_contact_author_phone '(317) 494 4572' _publ_requested_journal ? _publ_requested_coeditor_name ? # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Fanwick, Phillip E.' #<--'Last name, first name' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 'Burla, M.C., Polidori, G., & Camalli, M.,(1994). SIR. J. Appl. Cryst. 27, 435-442. Enraf-Nonius, CAD4 Operations Manual, Delft, 1977. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. International Tables for X-Ray Crystallography, Vol. IV, The Kynoch Press, Birmingham, England, 1974 Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158-166. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ;? ; data_DPKPHE # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C23 H18 Cl4 N4 O2 Pt1' _chemical_formula_structural ? _chemical_formula_weight 719.33 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p_-1 _cell_length_a 8.2320(11) _cell_length_b 8.7139(14) _cell_length_c 19.097(2) _cell_angle_alpha 100.346(12) _cell_angle_beta 95.190(10) _cell_angle_gamma 115.117(13) _cell_volume 1198.6(7) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19 _cell_measurement_theta_max 21 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.99 _exptl_crystal_density_meas ? _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 6.393 _cell_measurement_temperature 295 _exptl_crystal_F_000 692 # 6. DATA COLLECTION _diffrn_ambient_temperature 295 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method Enraf_Nonius_CAD4 _exptl_absorpt_correction_type refined_empirical_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.2458 _exptl_absorpt_correction_T_max 0.3752 _diffrn_reflns_number 6061 _reflns_number_total 5669 _reflns_number_observed 4767 _reflns_observed_criterion >3.0\s(I) _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.82 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 83 # 7. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all 0.044 _refine_ls_R_factor_obs 0.031 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.038 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others not refined, U=1.3*Ueq of bonding atom ; _refine_ls_number_reflns 4767 _refine_ls_number_parameters 315 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.190 _refine_ls_weighting_scheme '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_shift/esd_max 0.011 _refine_diff_density_max 1.91 _refine_diff_density_min -0.26 _refine_ls_extinction_method none _atom_type_scat_source International_Tables_for_Xray_Crystallography # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Pt 0.59436(2) 0.81849(2) 0.351733(10) 0.02863(4) Uani ? Cl(1) 0.41952(16) 0.96800(15) 0.35791(7) 0.0428(3) Uani ? Cl(2) 0.76400(19) 0.97499(16) 0.27705(8) 0.0504(4) Uani ? Cl(3) 0.80018(18) 1.01741(18) 0.45431(8) 0.0500(4) Uani ? Cl(10) 0.4136(2) 0.28688(17) 0.11000(8) 0.0581(4) Uani ? O(1) 0.4134(4) 0.6217(4) 0.27035(17) 0.0334(9) Uani ? O(2) 0.2820(5) 0.3200(4) 0.24833(18) 0.0399(10) Uani ? N(12) 0.7235(5) 0.6645(5) 0.3387(2) 0.0337(11) Uani ? N(22) 0.4366(5) 0.6548(5) 0.4088(2) 0.0306(10) Uani ? N(101) 0.1326(6) 0.2644(5) -0.0711(3) 0.0486(14) Uani ? N(112) 0.3468(5) 0.5510(5) 0.0420(2) 0.0419(12) Uani ? C(1) 0.4078(6) 0.4750(5) 0.2945(2) 0.0315(12) Uani ? C(11) 0.6055(6) 0.4991(5) 0.3062(2) 0.0312(12) Uani ? C(13) 0.9041(6) 0.7165(6) 0.3552(3) 0.0413(14) Uani ? C(14) 0.9690(7) 0.5954(7) 0.3383(3) 0.0501(16) Uani ? C(15) 0.8504(7) 0.4240(6) 0.3055(3) 0.0472(15) Uani ? C(16) 0.6636(7) 0.3714(6) 0.2889(3) 0.0393(14) Uani ? C(21) 0.3554(6) 0.4888(6) 0.3687(3) 0.0322(12) Uani ? C(23) 0.4063(7) 0.6980(7) 0.4758(3) 0.0405(14) Uani ? C(24) 0.2920(8) 0.5698(8) 0.5049(3) 0.0505(18) Uani ? C(25) 0.2079(8) 0.4005(8) 0.4663(3) 0.0560(19) Uani ? C(26) 0.2370(7) 0.3561(7) 0.3960(3) 0.0438(15) Uani ? C(102) 0.0266(9) 0.1310(8) -0.1255(4) 0.0588(19) Uani ? C(103) -0.0908(8) 0.1372(9) -0.1818(4) 0.060(2) Uani ? C(104) -0.0940(8) 0.2898(9) -0.1823(3) 0.0589(19) Uani ? C(105) 0.0171(7) 0.4387(7) -0.1267(3) 0.0489(16) Uani ? C(106) 0.0217(8) 0.6047(8) -0.1219(4) 0.0602(18) Uani ? C(107) 0.1299(8) 0.7437(7) -0.0678(4) 0.0651(19) Uani ? C(108) 0.2465(7) 0.7305(7) -0.0103(3) 0.0508(16) Uani ? C(109) 0.3617(8) 0.8691(7) 0.0476(4) 0.0604(18) Uani ? C(110) 0.4676(9) 0.8459(8) 0.1009(4) 0.062(2) Uani ? C(111) 0.4552(8) 0.6813(8) 0.0974(3) 0.0533(18) Uani ? C(113) 0.2414(6) 0.5666(6) -0.0130(3) 0.0380(13) Uani ? C(114) 0.1285(6) 0.4184(6) -0.0722(3) 0.0430(14) Uani ? H(1) 0.329(8) 0.441(8) 0.041(3) 0.07(2) Uiso ? H(2) 0.318(8) 0.315(8) 0.214(4) 0.07(2) Uiso ? H(131) 0.9864 0.8371 0.3788 0.0532 Uiso calc H(141) 1.0981 0.6309 0.3491 0.0639 Uiso calc H(151) 0.8969 0.3396 0.2944 0.0604 Uiso calc H(161) 0.5776 0.2516 0.2659 0.0513 Uiso calc H(231) 0.4644 0.8190 0.5025 0.0535 Uiso calc H(241) 0.2703 0.5993 0.5528 0.0657 Uiso calc H(251) 0.1280 0.3104 0.4873 0.0722 Uiso calc H(261) 0.1762 0.2375 0.3668 0.0578 Uiso calc H(1021) 0.0285 0.0189 -0.1266 0.0749 Uiso calc H(1031) -0.1667 0.0346 -0.2198 0.0779 Uiso calc H(1041) -0.1728 0.2975 -0.2205 0.0758 Uiso calc H(1061) -0.0561 0.6179 -0.1591 0.0769 Uiso calc H(1071) 0.1286 0.8529 -0.0672 0.0841 Uiso calc H(1091) 0.3678 0.9827 0.0503 0.0783 Uiso calc H(1101) 0.5471 0.9429 0.1404 0.0803 Uiso calc H(1111) 0.5267 0.6625 0.1349 0.0705 Uiso calc 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 0.02824(6) 0.02569(6) 0.03092(7) 0.01138(4) 0.00463(5) 0.00676(5) Cl(1) 0.0451(5) 0.0383(4) 0.0486(6) 0.0245(3) 0.0050(5) 0.0063(4) Cl(2) 0.0580(6) 0.0405(5) 0.0573(7) 0.0193(4) 0.0252(5) 0.0231(5) Cl(3) 0.0386(6) 0.0419(6) 0.0509(7) 0.0088(5) -0.0041(5) -0.0028(5) Cl(10) 0.0911(7) 0.0557(5) 0.0462(7) 0.0470(4) 0.0226(6) 0.0157(5) O(1) 0.0351(13) 0.0303(12) 0.0334(15) 0.0145(10) -0.0001(12) 0.0082(11) O(2) 0.0400(15) 0.0352(14) 0.0350(16) 0.0116(12) 0.0049(13) 0.0007(13) N(12) 0.0315(15) 0.0292(14) 0.042(2) 0.0138(11) 0.0088(15) 0.0120(14) N(22) 0.0250(15) 0.0320(15) 0.0295(17) 0.0089(12) 0.0023(13) 0.0064(13) N(101) 0.058(2) 0.0459(18) 0.048(2) 0.0299(14) 0.0065(19) 0.0116(17) N(112) 0.0452(18) 0.0439(17) 0.045(2) 0.0248(13) 0.0142(16) 0.0147(16) C(1) 0.0326(18) 0.0266(17) 0.032(2) 0.0114(13) 0.0025(16) 0.0055(15) C(11) 0.0341(18) 0.0328(17) 0.0297(19) 0.0157(13) 0.0079(16) 0.0118(15) C(13) 0.0288(19) 0.044(2) 0.053(3) 0.0154(15) 0.0060(19) 0.0182(19) C(14) 0.036(2) 0.054(2) 0.068(3) 0.0239(16) 0.011(2) 0.023(2) C(15) 0.048(2) 0.0495(19) 0.065(3) 0.0344(14) 0.022(2) 0.025(2) C(16) 0.048(2) 0.0363(18) 0.041(2) 0.0235(14) 0.0104(19) 0.0135(17) C(21) 0.0272(17) 0.0353(18) 0.035(2) 0.0147(13) 0.0018(16) 0.0098(16) C(23) 0.040(2) 0.050(2) 0.032(2) 0.0215(16) 0.0051(18) 0.0063(19) C(24) 0.050(3) 0.065(3) 0.034(2) 0.021(2) 0.014(2) 0.016(2) C(25) 0.050(3) 0.066(3) 0.048(3) 0.014(2) 0.015(2) 0.030(2) C(26) 0.040(2) 0.039(2) 0.047(3) 0.0109(18) 0.008(2) 0.0148(19) C(102) 0.069(3) 0.057(3) 0.055(3) 0.035(2) 0.006(3) 0.010(2) C(103) 0.056(3) 0.069(3) 0.049(3) 0.026(2) 0.009(3) 0.007(3) C(104) 0.055(3) 0.088(3) 0.045(3) 0.038(2) 0.012(2) 0.027(2) C(105) 0.051(2) 0.068(2) 0.047(3) 0.0365(17) 0.019(2) 0.027(2) C(106) 0.068(3) 0.074(3) 0.063(3) 0.0458(19) 0.016(2) 0.035(2) C(107) 0.083(3) 0.064(2) 0.086(4) 0.0530(18) 0.039(3) 0.045(2) C(108) 0.062(2) 0.051(2) 0.061(3) 0.0365(16) 0.032(2) 0.026(2) C(109) 0.086(3) 0.043(2) 0.070(3) 0.0396(18) 0.037(3) 0.016(2) C(110) 0.077(3) 0.047(3) 0.058(3) 0.025(2) 0.025(3) 0.008(3) C(111) 0.059(3) 0.057(3) 0.046(3) 0.028(2) 0.014(2) 0.010(2) C(113) 0.0436(19) 0.0481(19) 0.037(2) 0.0296(14) 0.0167(17) 0.0175(17) C(114) 0.044(2) 0.056(2) 0.046(2) 0.0321(15) 0.0190(18) 0.0220(19) # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Pt Cl(1) 2.3130(11) ? Pt Cl(2) 2.2992(12) ? Pt Cl(3) 2.3236(11) ? Pt O(1) 2.008(3) ? Pt N(12) 2.033(3) ? Pt N(22) 2.037(3) ? Cl(10) H(1) 2.29(6) ? Cl(10) H(2) 2.22(6) ? O(1) C(1) 1.419(5) ? O(2) C(1) 1.376(5) ? O(2) H(2) 0.74(6) ? N(12) C(11) 1.337(5) ? N(12) C(13) 1.344(5) ? N(22) C(21) 1.347(5) ? N(22) C(23) 1.344(5) ? N(101) C(102) 1.316(7) ? N(101) C(114) 1.361(6) ? N(112) C(111) 1.320(7) ? N(112) C(113) 1.364(6) ? N(112) H(1) 0.91(6) ? C(1) C(11) 1.539(6) ? C(1) C(21) 1.518(6) ? C(11) C(16) 1.387(6) ? C(13) C(14) 1.375(7) ? C(14) C(15) 1.376(7) ? C(15) C(16) 1.391(7) ? C(21) C(26) 1.382(6) ? C(23) C(24) 1.366(7) ? C(24) C(25) 1.360(8) ? C(25) C(26) 1.400(7) ? C(102) C(103) 1.404(8) ? C(103) C(104) 1.343(9) ? C(104) C(105) 1.403(8) ? C(105) C(106) 1.417(8) ? C(105) C(114) 1.410(7) ? C(106) C(107) 1.340(9) ? C(107) C(108) 1.446(8) ? C(108) C(109) 1.391(8) ? C(108) C(113) 1.403(6) ? C(109) C(110) 1.378(9) ? C(110) C(111) 1.383(8) ? C(113) C(114) 1.440(7) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl(1) Pt Cl(2) 92.55(5) ? Cl(1) Pt Cl(3) 90.91(4) ? Cl(1) Pt O(1) 93.50(9) ? Cl(1) Pt N(12) 173.62(10) ? Cl(1) Pt N(22) 91.00(10) ? Cl(2) Pt Cl(3) 91.46(5) ? Cl(2) Pt O(1) 94.70(9) ? Cl(2) Pt N(12) 89.07(10) ? Cl(2) Pt N(22) 173.43(10) ? Cl(3) Pt O(1) 172.25(8) ? Cl(3) Pt N(12) 95.23(11) ? Cl(3) Pt N(22) 94.01(10) ? O(1) Pt N(12) 80.21(13) ? O(1) Pt N(22) 79.56(12) ? N(12) Pt N(22) 86.81(14) ? H(1) Cl(10) H(2) 108(2) ? Pt O(1) C(1) 101.0(2) ? C(1) O(2) H(2) 106(5) ? Pt N(12) C(11) 111.0(3) ? Pt N(12) C(13) 126.7(3) ? C(11) N(12) C(13) 122.1(4) ? Pt N(22) C(21) 110.4(3) ? Pt N(22) C(23) 127.5(3) ? C(21) N(22) C(23) 122.0(4) ? C(102) N(101) C(114) 116.1(5) ? C(111) N(112) C(113) 124.0(5) ? C(111) N(112) H(1) 120(4) ? C(113) N(112) H(1) 115(4) ? O(1) C(1) O(2) 111.9(3) ? O(1) C(1) C(11) 106.3(3) ? O(1) C(1) C(21) 107.0(3) ? O(2) C(1) C(11) 115.2(3) ? O(2) C(1) C(21) 109.5(3) ? C(11) C(1) C(21) 106.5(3) ? N(12) C(11) C(1) 111.3(3) ? N(12) C(11) C(16) 121.4(4) ? C(1) C(11) C(16) 127.3(4) ? N(12) C(13) C(14) 118.8(4) ? C(13) C(14) C(15) 120.3(4) ? C(14) C(15) C(16) 120.3(4) ? C(11) C(16) C(15) 117.0(4) ? N(22) C(21) C(1) 111.8(3) ? N(22) C(21) C(26) 120.3(4) ? C(1) C(21) C(26) 127.8(4) ? N(22) C(23) C(24) 119.2(4) ? C(23) C(24) C(25) 120.6(5) ? C(24) C(25) C(26) 120.1(5) ? C(21) C(26) C(25) 117.7(4) ? N(101) C(102) C(103) 124.7(5) ? C(102) C(103) C(104) 118.7(5) ? C(103) C(104) C(105) 120.0(5) ? C(104) C(105) C(106) 124.2(5) ? C(104) C(105) C(114) 116.9(5) ? C(106) C(105) C(114) 118.9(5) ? C(105) C(106) C(107) 122.3(5) ? C(106) C(107) C(108) 121.2(5) ? C(107) C(108) C(109) 124.3(5) ? C(107) C(108) C(113) 117.5(5) ? C(109) C(108) C(113) 118.2(5) ? C(108) C(109) C(110) 121.0(5) ? C(109) C(110) C(111) 119.2(5) ? N(112) C(111) C(110) 119.4(5) ? N(112) C(113) C(108) 118.2(5) ? N(112) C(113) C(114) 120.7(4) ? C(108) C(113) C(114) 121.2(4) ? N(101) C(114) C(105) 123.6(5) ? N(101) C(114) C(113) 117.5(4) ? C(105) C(114) C(113) 118.9(5) ? Cl(10) H(1) N(112) 141(5) ? Cl(10) H(2) O(2) 177(10) ?