# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ? _publ_contact_author_email kukushkin@VK2100.spb.edu _publ_contact_author_phone ? _publ_contact_author_name 'Kukushkin, Vadim' _publ_author_name 'Vadim Kukushkin' data_[PtCl2(EtCN)2] _database_code_depnum_ccdc_archive 'CCDC 881311' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H10 Cl4 N2 Pt' _chemical_formula_sum 'C6 H10 Cl4 N2 Pt' _chemical_formula_weight 447.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.9682(2) _cell_length_b 8.8714(5) _cell_length_c 11.9058(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.931(3) _cell_angle_gamma 90.00 _cell_volume 611.83(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15209 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 28.70 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 12.300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2421 _exptl_absorpt_correction_T_max 0.6198 _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008)' _publ_section_exptl_refinement ; The Pt atom is located on a center of symmetry (inversion centre) and is coordinated by two Cl atoms and two N atoms in a slightly distorted square planar geometry. Hydrogen atoms were positioned geometrically and were constrained to ride on their parent atoms, with C---H = 0.98-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.72 \%A from atom Cl2 and the deepest hole is located 0.79 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11915 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 28.73 _reflns_number_total 1570 _reflns_number_gt 1347 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystaMaker (CrystalMaker Software ltd., 2011)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+1.0161P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1570 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.0000 0.01287(8) Uani 1 2 d S . . Cl1 Cl 0.13974(16) 0.16747(10) -0.11672(8) 0.0213(2) Uani 1 1 d . . . Cl2 Cl -0.19225(16) 0.19633(10) 0.06471(8) 0.02023(19) Uani 1 1 d . . . N1 N 0.2684(6) 0.0378(4) 0.1295(3) 0.0179(6) Uani 1 1 d . . . C1 C 0.4137(6) 0.0627(4) 0.2072(3) 0.0188(7) Uani 1 1 d . . . C2 C 0.5958(6) 0.0956(4) 0.3101(3) 0.0197(8) Uani 1 1 d . . . H2A H 0.5402 0.1734 0.3565 0.024 Uiso 1 1 calc R . . H2B H 0.7308 0.1373 0.2861 0.024 Uiso 1 1 calc R . . C3 C 0.6717(8) -0.0439(5) 0.3858(4) 0.0257(8) Uani 1 1 d . . . H3A H 0.5362 -0.0917 0.4035 0.039 Uiso 1 1 calc R . . H3B H 0.7798 -0.0136 0.4580 0.039 Uiso 1 1 calc R . . H3C H 0.7476 -0.1155 0.3444 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00977(12) 0.01563(12) 0.01170(12) 0.00059(6) -0.00038(8) -0.00026(6) Cl1 0.0195(4) 0.0230(4) 0.0213(5) 0.0058(4) 0.0046(4) -0.0022(3) Cl2 0.0192(4) 0.0209(4) 0.0200(4) -0.0016(4) 0.0035(3) 0.0034(3) N1 0.0148(16) 0.0214(14) 0.0161(16) -0.0006(13) 0.0009(13) -0.0017(13) C1 0.0197(19) 0.0151(17) 0.0206(19) 0.0016(15) 0.0029(16) 0.0004(14) C2 0.0195(18) 0.0201(17) 0.0151(18) -0.0003(14) -0.0044(15) -0.0016(14) C3 0.028(2) 0.0237(18) 0.021(2) -0.0023(18) -0.0040(17) -0.0021(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 1.966(3) 3 ? Pt1 N1 1.966(3) . yes Pt1 Cl2 2.3172(9) . yes Pt1 Cl2 2.3172(9) 3 ? Pt1 Cl1 2.3221(9) 3 ? Pt1 Cl1 2.3221(9) . yes N1 C1 1.127(5) . yes C1 C2 1.458(5) . ? C2 C3 1.533(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 180.0 3 . ? N1 Pt1 Cl2 90.79(10) 3 . ? N1 Pt1 Cl2 89.21(10) . . yes N1 Pt1 Cl2 89.21(10) 3 3 ? N1 Pt1 Cl2 90.79(10) . 3 ? Cl2 Pt1 Cl2 180.0 . 3 ? N1 Pt1 Cl1 91.03(10) 3 3 ? N1 Pt1 Cl1 88.97(10) . 3 ? Cl2 Pt1 Cl1 90.23(3) . 3 ? Cl2 Pt1 Cl1 89.77(3) 3 3 ? N1 Pt1 Cl1 88.97(10) 3 . ? N1 Pt1 Cl1 91.03(10) . . ? Cl2 Pt1 Cl1 89.77(3) . . yes Cl2 Pt1 Cl1 90.23(3) 3 . ? Cl1 Pt1 Cl1 180.0 3 . ? C1 N1 Pt1 176.0(3) . . yes N1 C1 C2 178.0(4) . . ? C1 C2 C3 112.8(3) . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.215 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.180 #===END======================================================================== data_trans-1 _database_code_depnum_ccdc_archive 'CCDC 881312' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Cl4 N4 O4 Pt' _chemical_formula_sum 'C12 H12 Cl4 N4 O4 Pt' _chemical_formula_weight 613.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6189(2) _cell_length_b 8.7091(2) _cell_length_c 11.1019(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.029(2) _cell_angle_gamma 90.00 _cell_volume 849.43(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27697 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 30.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 8.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1797 _exptl_absorpt_correction_T_max 0.4928 _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008)' _publ_section_exptl_refinement ; The NH~2~O hydrogen atoms were located from the difference Fourier map and refined isotropically. Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95 \%A, and U~iso~ = 1.2 U~eq~(parent atom). The highest peak is located 0.72 \%A from atom Pt1 and the deepest hole is located 0.78 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27697 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2477 _reflns_number_gt 2069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystaMaker (CrystalMaker Software ltd., 2011)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+0.9658P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2477 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0162 _refine_ls_wR_factor_ref 0.0372 _refine_ls_wR_factor_gt 0.0345 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.0000 0.0000 0.01101(4) Uani 1 2 d S . . Cl1 Cl 0.65417(7) -0.21481(6) 0.06211(6) 0.01865(11) Uani 1 1 d . . . Cl2 Cl 0.43646(7) -0.03232(7) 0.17839(6) 0.01822(11) Uani 1 1 d . . . O1 O 0.8940(2) -0.0332(2) 0.30084(19) 0.0249(4) Uani 1 1 d . . . O2 O 1.0873(2) -0.0860(2) 0.2569(2) 0.0385(5) Uani 1 1 d . . . N1 N 0.6695(2) 0.1411(2) 0.1308(2) 0.0146(4) Uani 1 1 d . . . N2 N 0.9737(3) -0.0103(2) 0.2391(2) 0.0219(4) Uani 1 1 d . . . H2N H 0.623(3) 0.216(4) 0.137(3) 0.023(8) Uiso 1 1 d . . . H2M H 0.703(3) 0.094(3) 0.204(3) 0.025(8) Uiso 1 1 d . . . C1 C 0.7916(3) 0.1859(3) 0.0958(2) 0.0173(5) Uani 1 1 d . . . C2 C 0.7643(3) 0.3069(3) 0.0064(2) 0.0216(5) Uani 1 1 d . . . H2 H 0.6698 0.3597 -0.0239 0.026 Uiso 1 1 calc R . . C3 C 0.8718(3) 0.3503(3) -0.0379(3) 0.0260(6) Uani 1 1 d . . . H3 H 0.8510 0.4316 -0.0999 0.031 Uiso 1 1 calc R . . C4 C 1.0115(3) 0.2756(3) 0.0077(3) 0.0283(6) Uani 1 1 d . . . H4 H 1.0860 0.3062 -0.0231 0.034 Uiso 1 1 calc R . . C5 C 1.0426(3) 0.1578(3) 0.0969(3) 0.0256(6) Uani 1 1 d . . . H5 H 1.1384 0.1073 0.1282 0.031 Uiso 1 1 calc R . . C6 C 0.9325(3) 0.1129(3) 0.1413(2) 0.0194(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01057(6) 0.01188(6) 0.00969(6) 0.00042(4) 0.00321(4) -0.00049(4) Cl1 0.0179(3) 0.0158(2) 0.0175(3) 0.0000(2) 0.0023(2) 0.0037(2) Cl2 0.0197(3) 0.0230(3) 0.0135(2) -0.00034(19) 0.0084(2) -0.0032(2) O1 0.0257(10) 0.0236(9) 0.0196(9) 0.0023(7) 0.0034(8) 0.0003(7) O2 0.0341(12) 0.0387(12) 0.0378(12) 0.0041(10) 0.0098(10) 0.0180(10) N1 0.0138(9) 0.0158(9) 0.0125(9) -0.0015(7) 0.0034(7) -0.0015(8) N2 0.0211(10) 0.0207(10) 0.0185(10) -0.0040(8) 0.0023(8) -0.0002(9) C1 0.0170(11) 0.0195(11) 0.0154(11) -0.0068(8) 0.0065(9) -0.0067(9) C2 0.0213(12) 0.0192(11) 0.0205(12) -0.0018(9) 0.0045(10) -0.0042(9) C3 0.0335(15) 0.0211(12) 0.0234(13) -0.0028(10) 0.0114(11) -0.0091(11) C4 0.0314(14) 0.0278(13) 0.0335(15) -0.0108(11) 0.0211(12) -0.0139(12) C5 0.0177(12) 0.0280(13) 0.0322(14) -0.0140(11) 0.0112(11) -0.0046(10) C6 0.0205(12) 0.0160(11) 0.0197(12) -0.0059(9) 0.0061(10) -0.0024(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.0856(19) 3_655 ? Pt1 N1 2.0856(19) . yes Pt1 Cl1 2.3112(5) 3_655 ? Pt1 Cl1 2.3112(5) . yes Pt1 Cl2 2.3153(6) 3_655 ? Pt1 Cl2 2.3153(6) . yes O1 N2 1.236(3) . ? O2 N2 1.221(3) . ? N1 C1 1.433(3) . yes N1 H2N 0.81(3) . ? N1 H2M 0.85(3) . ? N2 C6 1.462(3) . yes C1 C6 1.392(3) . ? C1 C2 1.397(3) . ? C2 C3 1.367(4) . ? C2 H2 0.9500 . ? C3 C4 1.390(4) . ? C3 H3 0.9500 . ? C4 C5 1.371(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(4) . ? C5 H5 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 180.0 3_655 . ? N1 Pt1 Cl1 92.55(6) 3_655 3_655 ? N1 Pt1 Cl1 87.45(6) . 3_655 ? N1 Pt1 Cl1 87.45(6) 3_655 . ? N1 Pt1 Cl1 92.55(6) . . yes Cl1 Pt1 Cl1 180.0 3_655 . ? N1 Pt1 Cl2 83.11(6) 3_655 3_655 ? N1 Pt1 Cl2 96.89(6) . 3_655 ? Cl1 Pt1 Cl2 90.41(2) 3_655 3_655 ? Cl1 Pt1 Cl2 89.59(2) . 3_655 ? N1 Pt1 Cl2 96.89(6) 3_655 . ? N1 Pt1 Cl2 83.11(6) . . yes Cl1 Pt1 Cl2 89.59(2) 3_655 . ? Cl1 Pt1 Cl2 90.41(2) . . yes Cl2 Pt1 Cl2 180.0 3_655 . ? C1 N1 Pt1 117.78(15) . . ? C1 N1 H2N 110(2) . . ? Pt1 N1 H2N 104(2) . . ? C1 N1 H2M 111(2) . . ? Pt1 N1 H2M 105(2) . . ? H2N N1 H2M 109(3) . . ? O2 N2 O1 122.7(2) . . ? O2 N2 C6 118.1(2) . . ? O1 N2 C6 119.2(2) . . ? C6 C1 C2 118.4(2) . . ? C6 C1 N1 124.2(2) . . ? C2 C1 N1 117.4(2) . . ? C3 C2 C1 120.9(2) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.5(2) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 120.7(2) . . ? C1 C6 N2 122.3(2) . . ? C5 C6 N2 117.0(2) . . ? 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 Cl1 Pt1 N1 C1 -104.19(17) 3_655 . . . ? Cl1 Pt1 N1 C1 75.81(17) . . . . ? Cl2 Pt1 N1 C1 -14.09(17) 3_655 . . . ? Cl2 Pt1 N1 C1 165.91(17) . . . . ? Pt1 N1 C1 C6 -97.2(2) . . . . ? Pt1 N1 C1 C2 80.3(2) . . . . ? C6 C1 C2 C3 1.6(3) . . . . ? N1 C1 C2 C3 -176.1(2) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C2 C1 C6 C5 -1.1(3) . . . . ? N1 C1 C6 C5 176.4(2) . . . . ? C2 C1 C6 N2 177.3(2) . . . . ? N1 C1 C6 N2 -5.2(3) . . . . ? C4 C5 C6 C1 0.2(4) . . . . ? C4 C5 C6 N2 -178.3(2) . . . . ? O2 N2 C6 C1 167.5(2) . . . . ? O1 N2 C6 C1 -13.0(3) . . . . ? O2 N2 C6 C5 -14.0(3) . . . . ? O1 N2 C6 C5 165.5(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H2N O1 0.81(3) 2.32(3) 3.062(3) 154(3) 2_655 yes N1 H2M O1 0.85(3) 2.03(3) 2.685(3) 133(3) . yes _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.745 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.119 #===END======================================================================== data_trans-2 _database_code_depnum_ccdc_archive 'CCDC 881313' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Cl4 N4 O4 Pt, 2(H2 O)' _chemical_formula_sum 'C12 H16 Cl4 N4 O6 Pt' _chemical_formula_weight 649.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.8898(2) _cell_length_b 18.3306(7) _cell_length_c 8.9748(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.3540(10) _cell_angle_gamma 90.00 _cell_volume 958.67(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9993 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 32.88 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 7.914 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3641 _exptl_absorpt_correction_T_max 0.4764 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; The H~2~O hydrogen atoms were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95 \%A, N---H = 0.92 \%A, and U~iso~ = 1.2 U~eq~(parent atom). The highest peak is located 0.79 \%A from atom Pt1 and the deepest hole is located 0.88 \%A from atom C1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 16 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21370 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 32.01 _reflns_number_total 3256 _reflns_number_gt 2885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2e (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+2.8776P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3256 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 1.294 _refine_ls_restrained_S_all 1.294 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.5000 0.5000 0.01149(5) Uani 1 2 d S . . Cl1 Cl 0.68934(13) 0.39558(4) 0.59273(9) 0.01555(14) Uani 1 1 d . . . Cl2 Cl 0.24841(13) 0.48529(4) 0.67241(9) 0.01593(14) Uani 1 1 d . . . O1S O 0.7278(6) 0.48835(16) 0.9451(3) 0.0378(7) Uani 1 1 d . . . H1SA H 0.7575 0.4473 0.9363 0.057 Uiso 1 1 d R . . H1SB H 0.7544 0.5075 1.0281 0.057 Uiso 1 1 d R . . O1 O 0.0426(6) 0.13334(15) 0.4257(4) 0.0339(7) Uani 1 1 d . . . O2 O -0.1191(5) 0.22545(16) 0.5152(4) 0.0354(7) Uani 1 1 d . . . N1 N 0.2685(4) 0.44608(14) 0.3397(3) 0.0148(5) Uani 1 1 d . . . H1N H 0.1232 0.4559 0.3605 0.018 Uiso 1 1 calc R . . H1M H 0.2798 0.4666 0.2475 0.018 Uiso 1 1 calc R . . N2 N 0.0190(5) 0.19918(17) 0.4420(4) 0.0212(6) Uani 1 1 d . . . C1 C 0.2875(5) 0.36843(17) 0.3244(3) 0.0145(6) Uani 1 1 d . . . C2 C 0.1454(6) 0.32294(18) 0.3916(4) 0.0168(6) Uani 1 1 d . . . H2 H 0.0356 0.3419 0.4490 0.020 Uiso 1 1 calc R . . C3 C 0.1693(6) 0.24842(18) 0.3718(4) 0.0163(6) Uani 1 1 d . . . C4 C 0.3257(6) 0.21828(18) 0.2888(4) 0.0187(6) Uani 1 1 d . . . H4 H 0.3368 0.1670 0.2771 0.022 Uiso 1 1 calc R . . C5 C 0.4659(6) 0.26562(19) 0.2231(4) 0.0196(6) Uani 1 1 d . . . H5 H 0.5761 0.2465 0.1661 0.023 Uiso 1 1 calc R . . C6 C 0.4474(6) 0.34030(18) 0.2396(4) 0.0180(6) Uani 1 1 d . . . H6 H 0.5432 0.3723 0.1933 0.022 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01201(7) 0.00908(7) 0.01444(7) 0.00008(6) 0.00550(5) 0.00077(6) Cl1 0.0149(3) 0.0122(3) 0.0199(3) 0.0023(3) 0.0039(2) 0.0025(3) Cl2 0.0147(3) 0.0171(3) 0.0174(3) 0.0024(2) 0.0072(2) 0.0014(3) O1S 0.064(2) 0.0271(16) 0.0223(13) -0.0001(11) 0.0054(13) 0.0144(14) O1 0.0463(18) 0.0169(13) 0.0424(17) -0.0049(11) 0.0198(14) -0.0085(12) O2 0.0324(15) 0.0288(15) 0.0515(19) 0.0041(13) 0.0279(14) 0.0005(12) N1 0.0140(12) 0.0142(12) 0.0163(12) -0.0008(10) 0.0031(9) 0.0029(10) N2 0.0211(14) 0.0198(14) 0.0235(14) 0.0002(11) 0.0053(11) -0.0042(11) C1 0.0126(13) 0.0165(14) 0.0142(13) 0.0007(11) 0.0014(10) 0.0014(11) C2 0.0163(14) 0.0168(14) 0.0181(15) -0.0034(11) 0.0054(11) 0.0005(12) C3 0.0175(14) 0.0165(14) 0.0156(14) -0.0009(11) 0.0044(11) -0.0026(12) C4 0.0226(15) 0.0143(14) 0.0199(15) -0.0037(11) 0.0056(12) -0.0001(12) C5 0.0204(16) 0.0186(15) 0.0216(16) -0.0046(12) 0.0094(12) 0.0020(12) C6 0.0183(15) 0.0183(15) 0.0191(15) -0.0022(12) 0.0088(12) -0.0001(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.082(3) . yes Pt1 N1 2.082(3) 3_666 ? Pt1 Cl2 2.3084(7) 3_666 ? Pt1 Cl2 2.3085(7) . yes Pt1 Cl1 2.3087(7) 3_666 ? Pt1 Cl1 2.3087(7) . yes O1S H1SA 0.7794 . ? O1S H1SB 0.8181 . ? O1 N2 1.226(4) . ? O2 N2 1.217(4) . ? N1 C1 1.436(4) . ? N1 H1N 0.9200 . ? N1 H1M 0.9200 . ? N2 C3 1.469(4) . ? C1 C2 1.380(4) . ? C1 C6 1.393(4) . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.381(5) . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C6 1.383(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 179.998(1) . 3_666 ? N1 Pt1 Cl2 90.69(8) . 3_666 ? N1 Pt1 Cl2 89.31(8) 3_666 3_666 ? N1 Pt1 Cl2 89.31(8) . . ? N1 Pt1 Cl2 90.69(8) 3_666 . ? Cl2 Pt1 Cl2 180.00(2) 3_666 . ? N1 Pt1 Cl1 84.89(7) . 3_666 ? N1 Pt1 Cl1 95.11(7) 3_666 3_666 ? Cl2 Pt1 Cl1 89.14(3) 3_666 3_666 ? Cl2 Pt1 Cl1 90.86(3) . 3_666 ? N1 Pt1 Cl1 95.11(7) . . ? N1 Pt1 Cl1 84.89(7) 3_666 . ? Cl2 Pt1 Cl1 90.86(3) 3_666 . ? Cl2 Pt1 Cl1 89.14(3) . . ? Cl1 Pt1 Cl1 180.0 3_666 . ? H1SA O1S H1SB 119.5 . . ? C1 N1 Pt1 119.0(2) . . ? C1 N1 H1N 107.6 . . ? Pt1 N1 H1N 107.6 . . ? C1 N1 H1M 107.6 . . ? Pt1 N1 H1M 107.6 . . ? H1N N1 H1M 107.0 . . ? O2 N2 O1 123.4(3) . . ? O2 N2 C3 118.7(3) . . ? O1 N2 C3 117.9(3) . . ? C2 C1 C6 121.1(3) . . ? C2 C1 N1 119.8(3) . . ? C6 C1 N1 119.2(3) . . ? C1 C2 C3 117.4(3) . . ? C1 C2 H2 121.3 . . ? C3 C2 H2 121.3 . . ? C4 C3 C2 123.4(3) . . ? C4 C3 N2 118.4(3) . . ? C2 C3 N2 118.1(3) . . ? C3 C4 C5 117.6(3) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? C6 C5 C4 120.8(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 119.7(3) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1S H1SA O1 0.78 2.25 2.922(4) 144.9 4_666 yes O1S H1SB O1 0.82 2.60 3.128(4) 123.3 2_656 yes O1S H1SB Cl2 0.82 2.69 3.449(3) 154.4 3_667 yes N1 H1N Cl2 0.92 2.42 3.281(3) 156.2 3_566 yes N1 H1M O1S 0.92 1.91 2.827(4) 174.4 3_666 yes _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 32.01 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.904 _refine_diff_density_min -1.385 _refine_diff_density_rms 0.140 #===END======================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 881314' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H15 Cl4 N4 O2 Pt' _chemical_formula_sum 'C12 H15 Cl4 N4 O2 Pt' _chemical_formula_weight 584.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0633(8) _cell_length_b 8.5041(4) _cell_length_c 14.8670(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.787(3) _cell_angle_gamma 90.00 _cell_volume 1841.39(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 58668 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 8.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3426 _exptl_absorpt_correction_T_max 0.5650 _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008)' _publ_section_exptl_refinement ; The large residual electron density on special position 0.5000 1.0000 0.0000 is due to the pseudosymmetry. The sructure could be solved in space group C2/c but the refinedment was not satisfactory. Also, no acceptable twinning model was found. No satisfactory twinning model was found. The anisotropic displacement parameters of adjacent N1 and C1 were restrained to be similar. The NH hydrogen atoma was located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 1.66 \%A from atom N4 (at 0.5000 1.0000 0.0000) and the deepest hole is located 0.76 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31328 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3235 _reflns_number_gt 2376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.1f (Brandenburg, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+35.5039P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3235 _refine_ls_number_parameters 211 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.16974(2) 0.50062(6) 0.14749(2) 0.02603(15) Uani 1 1 d . . . Cl1 Cl 0.28233(19) 0.6930(3) 0.18549(17) 0.0365(6) Uani 1 1 d . . . Cl2 Cl 0.28231(18) 0.3097(3) 0.15701(17) 0.0335(6) Uani 1 1 d . . . Cl3 Cl 0.05793(18) 0.3076(3) 0.10883(17) 0.0318(6) Uani 1 1 d . . . Cl4 Cl 0.05720(19) 0.6878(3) 0.14376(17) 0.0344(6) Uani 1 1 d . . . O1 O 0.4013(8) 1.0698(15) -0.0732(8) 0.079(3) Uani 1 1 d . . . O2 O 0.5126(9) 1.0261(17) -0.1475(9) 0.099(5) Uani 1 1 d . . . N2 N 0.1784(6) 0.4676(10) 0.2819(5) 0.0316(17) Uani 1 1 d U . . N1 N 0.1520(6) 0.5447(11) 0.0118(6) 0.033(2) Uani 1 1 d . . . H1 H 0.0970 0.5610 -0.0134 0.00(2) Uiso 1 1 d R . . N3 N 0.2975(6) 0.5315(13) -0.0095(6) 0.044(3) Uani 1 1 d . . . N4 N 0.4512(10) 0.9773(18) -0.1126(7) 0.074(4) Uani 1 1 d . . . C10 C 0.1752(8) 0.4316(14) 0.3563(6) 0.0321(17) Uani 1 1 d U . . C11 C 0.1752(9) 0.3894(15) 0.4508(7) 0.043(3) Uani 1 1 d . . . H11A H 0.2382 0.3587 0.4851 0.051 Uiso 1 1 calc R . . H11B H 0.1346 0.2975 0.4495 0.051 Uiso 1 1 calc R . . C12 C 0.1437(11) 0.5207(15) 0.5003(8) 0.055(4) Uani 1 1 d . . . H12A H 0.1847 0.6110 0.5032 0.082 Uiso 1 1 calc R . . H12B H 0.1444 0.4873 0.5636 0.082 Uiso 1 1 calc R . . H12C H 0.0811 0.5505 0.4670 0.082 Uiso 1 1 calc R . . C1 C 0.2081(8) 0.5610(15) -0.0400(7) 0.040(3) Uani 1 1 d . . . C2 C 0.1695(8) 0.6086(13) -0.1413(7) 0.033(3) Uani 1 1 d . . . H2A H 0.2091 0.6910 -0.1578 0.039 Uiso 1 1 calc R . . H2B H 0.1074 0.6538 -0.1491 0.039 Uiso 1 1 calc R . . C3 C 0.1638(9) 0.4688(15) -0.2074(7) 0.047(3) Uani 1 1 d . . . H3A H 0.2255 0.4265 -0.2017 0.070 Uiso 1 1 calc R . . H3B H 0.1375 0.5035 -0.2716 0.070 Uiso 1 1 calc R . . H3C H 0.1247 0.3870 -0.1913 0.070 Uiso 1 1 calc R . . C4 C 0.3643(8) 0.5914(19) -0.0557(8) 0.048(3) Uani 1 1 d . . . C5 C 0.3788(9) 0.750(2) -0.0564(9) 0.059(4) Uani 1 1 d . . . H5 H 0.3473 0.8192 -0.0252 0.070 Uiso 1 1 calc R . . C6 C 0.4418(9) 0.808(2) -0.1048(9) 0.059(4) Uani 1 1 d . . . C7 C 0.4895(10) 0.711(2) -0.1463(10) 0.068(5) Uani 1 1 d . . . H7 H 0.5327 0.7535 -0.1765 0.081 Uiso 1 1 calc R . . C8 C 0.4755(10) 0.549(2) -0.1452(9) 0.068(5) Uani 1 1 d . . . H8 H 0.5084 0.4801 -0.1755 0.082 Uiso 1 1 calc R . . C9 C 0.4125(9) 0.487(2) -0.0990(9) 0.060(4) Uani 1 1 d . . . H9 H 0.4027 0.3771 -0.0972 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0306(2) 0.0317(2) 0.0168(2) -0.00037(16) 0.00773(14) 0.0002(2) Cl1 0.0379(15) 0.0392(16) 0.0312(13) -0.0039(12) 0.0068(11) -0.0063(13) Cl2 0.0339(15) 0.0372(16) 0.0293(13) 0.0022(11) 0.0082(11) 0.0056(12) Cl3 0.0325(14) 0.0347(15) 0.0287(12) 0.0008(11) 0.0085(10) -0.0007(12) Cl4 0.0402(15) 0.0367(16) 0.0277(12) -0.0005(11) 0.0112(11) 0.0053(13) O1 0.083(8) 0.090(9) 0.060(7) -0.015(6) 0.011(6) -0.010(7) O2 0.093(9) 0.118(11) 0.086(8) 0.035(8) 0.022(7) -0.045(8) N2 0.052(4) 0.033(4) 0.014(3) -0.012(3) 0.018(3) -0.002(3) N1 0.025(5) 0.037(6) 0.034(5) 0.014(4) 0.002(4) 0.007(4) N3 0.032(5) 0.075(8) 0.027(5) 0.002(5) 0.010(4) 0.006(5) N4 0.090(10) 0.100(12) 0.020(5) 0.008(6) -0.007(6) -0.033(9) C10 0.053(4) 0.033(4) 0.015(3) -0.011(3) 0.017(3) -0.003(3) C11 0.068(9) 0.042(7) 0.020(5) -0.001(5) 0.016(5) 0.004(6) C12 0.115(12) 0.037(8) 0.026(6) 0.009(5) 0.042(7) 0.004(8) C1 0.048(7) 0.047(7) 0.025(5) -0.002(5) 0.011(5) -0.001(6) C2 0.045(7) 0.032(6) 0.025(5) 0.004(5) 0.016(5) 0.003(5) C3 0.060(8) 0.057(9) 0.024(5) -0.005(5) 0.011(5) -0.005(6) C4 0.038(7) 0.076(11) 0.032(6) 0.014(6) 0.010(5) 0.006(7) C5 0.044(8) 0.096(13) 0.036(7) 0.016(7) 0.011(6) 0.006(8) C6 0.045(8) 0.093(12) 0.038(7) 0.011(8) 0.009(6) -0.012(8) C7 0.044(8) 0.115(16) 0.050(8) 0.013(9) 0.022(7) -0.001(9) C8 0.050(8) 0.119(16) 0.040(7) 0.005(8) 0.019(6) 0.016(9) C9 0.048(7) 0.094(12) 0.039(7) 0.000(8) 0.014(6) 0.007(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 1.989(8) . yes Pt1 N1 2.001(8) . yes Pt1 Cl4 2.316(3) . yes Pt1 Cl3 2.317(3) . yes Pt1 Cl1 2.320(3) . yes Pt1 Cl2 2.326(3) . yes O1 N4 1.323(18) . ? O2 N4 1.241(17) . ? N2 C10 1.160(12) . yes N1 C1 1.288(14) . yes N1 H1 0.8300 . ? N3 C1 1.330(15) . yes N3 C4 1.449(15) . ? N4 C6 1.45(2) . ? C10 C11 1.449(14) . ? C11 C12 1.481(16) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C1 C2 1.525(14) . ? C2 C3 1.531(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.36(2) . ? C4 C9 1.400(19) . ? C5 C6 1.419(18) . ? C5 H5 0.9500 . ? C6 C7 1.34(2) . ? C7 C8 1.40(2) . ? C7 H7 0.9500 . ? C8 C9 1.41(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N1 175.4(4) . . yes N2 Pt1 Cl4 88.9(3) . . ? N1 Pt1 Cl4 86.5(3) . . ? N2 Pt1 Cl3 90.4(3) . . ? N1 Pt1 Cl3 88.9(3) . . ? Cl4 Pt1 Cl3 89.98(9) . . ? N2 Pt1 Cl1 89.9(3) . . ? N1 Pt1 Cl1 90.8(3) . . ? Cl4 Pt1 Cl1 90.36(11) . . ? Cl3 Pt1 Cl1 179.56(10) . . yes N2 Pt1 Cl2 88.9(3) . . ? N1 Pt1 Cl2 95.7(3) . . ? Cl4 Pt1 Cl2 177.75(9) . . yes Cl3 Pt1 Cl2 89.60(10) . . ? Cl1 Pt1 Cl2 90.07(10) . . ? C10 N2 Pt1 170.7(9) . . ? C1 N1 Pt1 133.1(8) . . ? C1 N1 H1 116.4 . . ? Pt1 N1 H1 110.3 . . ? C1 N3 C4 122.5(10) . . ? O2 N4 O1 123.6(16) . . ? O2 N4 C6 117.5(16) . . ? O1 N4 C6 118.4(13) . . ? N2 C10 C11 177.5(13) . . ? C10 C11 C12 112.0(10) . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C1 N3 122.5(10) . . ? N1 C1 C2 118.4(10) . . ? N3 C1 C2 119.0(10) . . ? C1 C2 C3 111.9(9) . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 121.2(13) . . ? C5 C4 N3 118.8(12) . . ? C9 C4 N3 120.0(14) . . ? C4 C5 C6 118.5(15) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C7 C6 C5 121.7(16) . . ? C7 C6 N4 119.7(14) . . ? C5 C6 N4 118.6(15) . . ? C6 C7 C8 120.0(14) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 119.6(15) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C4 C9 C8 118.9(16) . . ? C4 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl3 0.83 2.65 3.450(9) 162.7 3_565 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.186 _refine_diff_density_min -1.376 _refine_diff_density_rms 0.217 # start Validation Reply Form _vrf_PUBL971_GLOBAL ; PROBLEM: Large Calcd. Non-Metal Positive Residual Density RESPONSE: The large residual electron density on special position 0.5000 1.0000 0.0000 is due to the pseudosymmetry. The sructure could be solved in space group C2/c but the refinedment was not satisfactory. Also, no acceptable twinning model was found. ; # end Validation Reply Form #===END======================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 881315' #TrackingRef '- all.cif' _audit_creation_date 2012-03-14 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H22 Cl4 N6 O4 Pt' _chemical_formula_sum 'C18 H22 Cl4 N6 O4 Pt' _chemical_formula_weight 723.31 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 6.59770(10) _cell_length_b 7.9991(2) _cell_length_c 11.9255(2) _cell_angle_alpha 73.9520(10) _cell_angle_beta 82.1570(10) _cell_angle_gamma 75.8260(10) _cell_volume 584.84(2) _cell_formula_units_Z 1 _cell_measurement_reflns_used 8872 _cell_measurement_temperature 100 _cell_measurement_theta_max 33.074 _cell_measurement_theta_min 2.715 _exptl_absorpt_coefficient_mu 6.494 _exptl_absorpt_correction_T_max 0.5843 _exptl_absorpt_correction_T_min 0.3862 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0690 before and 0.0429 after correction. The Ratio of minimum to maximum transmission is 0.6610. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.054 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 350 _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _publ_section_exptl_refinement ; The hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.98 \%A and N---H = 0.88 \%A, and U~iso~ = 1.2 U~eq~(parent atom). The highest peak is located 0.77 \%A from atom Pt1 and the deepest hole is located 0.77 \%A from atom Pt1. _exptl_special_details ; _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0356 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 15751 _diffrn_reflns_theta_full 33.19 _diffrn_reflns_theta_max 33.19 _diffrn_reflns_theta_min 1.78 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on three-circle goniostat' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'flat graphite crystal' _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4418 _reflns_number_total 4457 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics 'CrystaMaker (CrystalMaker Software ltd., 2011)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 1.154 _refine_diff_density_min -1.720 _refine_diff_density_rms 0.127 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 152 _refine_ls_number_reflns 4457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0206 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0411 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.0000 0.5000 0.01221(3) Uani 1 2 d S . . Cl1 Cl 0.63318(8) 0.25185(6) 0.47483(4) 0.01907(9) Uani 1 1 d . . . Cl2 Cl 0.66906(8) -0.12586(6) 0.67142(4) 0.02022(9) Uani 1 1 d . . . N1 N 0.2287(3) 0.0979(2) 0.58540(14) 0.0166(3) Uani 1 1 d . . . H1 H 0.1174 0.0823 0.5598 0.020 Uiso 1 1 calc R . . C9 C 0.2957(3) 0.1562(2) 0.92021(18) 0.0183(4) Uani 1 1 d . . . H9 H 0.3068 0.0363 0.9183 0.022 Uiso 1 1 calc R . . N2 N 0.3254(3) 0.2395(2) 0.70730(15) 0.0175(3) Uani 1 1 d . . . H2 H 0.4413 0.2508 0.6625 0.021 Uiso 1 1 calc R . . C7 C 0.2584(3) 0.3739(3) 1.03052(17) 0.0173(3) Uani 1 1 d . . . H7 H 0.2455 0.4049 1.1029 0.021 Uiso 1 1 calc R . . C2 C -0.0398(3) 0.2154(3) 0.72038(18) 0.0192(4) Uani 1 1 d . . . H2A H -0.0418 0.1845 0.8068 0.023 Uiso 1 1 calc R . . H2B H -0.1190 0.1400 0.6987 0.023 Uiso 1 1 calc R . . C3 C -0.1458(3) 0.4123(3) 0.6756(2) 0.0274(5) Uani 1 1 d . . . H3A H -0.1487 0.4418 0.5904 0.041 Uiso 1 1 calc R . . H3B H -0.0670 0.4870 0.6966 0.041 Uiso 1 1 calc R . . H3C H -0.2895 0.4339 0.7113 0.041 Uiso 1 1 calc R . . C8 C 0.2745(3) 0.1994(3) 1.02704(17) 0.0190(4) Uani 1 1 d . . . H8 H 0.2710 0.1090 1.0979 0.023 Uiso 1 1 calc R . . C4 C 0.3007(3) 0.2875(2) 0.81633(17) 0.0153(3) Uani 1 1 d . . . C1 C 0.1820(3) 0.1785(2) 0.66954(16) 0.0154(3) Uani 1 1 d . . . C6 C 0.2618(3) 0.5015(2) 0.92539(17) 0.0152(3) Uani 1 1 d . . . C5 C 0.2835(3) 0.4637(2) 0.81714(16) 0.0149(3) Uani 1 1 d . . . H5 H 0.2864 0.5546 0.7465 0.018 Uiso 1 1 calc R . . O2 O 0.2374(2) 0.7203(2) 1.02284(14) 0.0249(3) Uani 1 1 d . . . O1 O 0.2046(3) 0.8032(2) 0.83630(14) 0.0296(4) Uani 1 1 d . . . N3 N 0.2336(3) 0.6883(2) 0.92823(15) 0.0187(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01824(5) 0.01102(4) 0.00807(5) -0.00456(3) -0.00115(3) -0.00193(3) Cl1 0.0295(2) 0.01657(19) 0.0142(2) -0.00655(16) 0.00157(17) -0.00941(17) Cl2 0.0294(2) 0.01777(19) 0.0130(2) -0.00493(16) -0.00778(17) 0.00032(17) N1 0.0192(7) 0.0183(7) 0.0148(7) -0.0089(6) -0.0018(6) -0.0032(6) C9 0.0225(9) 0.0149(8) 0.0190(9) -0.0066(7) -0.0034(7) -0.0035(7) N2 0.0183(7) 0.0215(7) 0.0166(8) -0.0121(6) 0.0030(6) -0.0055(6) C7 0.0178(8) 0.0213(8) 0.0142(9) -0.0074(7) -0.0014(7) -0.0039(7) C2 0.0176(8) 0.0231(9) 0.0188(9) -0.0105(7) 0.0010(7) -0.0037(7) C3 0.0227(10) 0.0248(10) 0.0368(13) -0.0153(9) -0.0064(9) 0.0017(8) C8 0.0227(9) 0.0185(8) 0.0148(9) -0.0029(7) -0.0021(7) -0.0042(7) C4 0.0160(8) 0.0180(8) 0.0147(8) -0.0096(7) -0.0005(6) -0.0030(6) C1 0.0196(8) 0.0130(7) 0.0128(8) -0.0035(6) -0.0013(6) -0.0016(6) C6 0.0159(8) 0.0148(7) 0.0173(9) -0.0079(7) 0.0003(7) -0.0042(6) C5 0.0160(8) 0.0161(8) 0.0132(8) -0.0052(6) 0.0009(6) -0.0042(6) O2 0.0304(8) 0.0261(7) 0.0242(8) -0.0169(6) 0.0011(6) -0.0071(6) O1 0.0484(10) 0.0160(7) 0.0240(8) -0.0047(6) 0.0008(7) -0.0083(7) N3 0.0197(8) 0.0174(7) 0.0223(9) -0.0106(6) 0.0027(6) -0.0060(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Cl1 2.3197(4) . yes Pt1 Cl1 2.3197(4) 2_656 ? Pt1 Cl2 2.3176(4) 2_656 ? Pt1 Cl2 2.3176(4) . yes Pt1 N1 2.0278(16) . yes Pt1 N1 2.0278(16) 2_656 ? N1 C1 1.301(2) . yes C9 C8 1.390(3) . ? C9 C4 1.387(3) . ? N2 C4 1.432(2) . ? N2 C1 1.342(2) . yes C7 C8 1.386(3) . ? C7 C6 1.382(3) . ? C2 C3 1.533(3) . ? C2 C1 1.498(3) . ? C4 C5 1.389(2) . ? C6 C5 1.386(3) . ? C6 N3 1.469(2) . ? O2 N3 1.229(2) . ? O1 N3 1.224(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pt1 Cl1 180.0 . 2_656 ? Cl2 Pt1 Cl1 90.996(17) . 2_656 ? Cl2 Pt1 Cl1 89.005(17) 2_656 2_656 ? Cl2 Pt1 Cl1 89.004(17) . . yes Cl2 Pt1 Cl1 90.995(17) 2_656 . ? Cl2 Pt1 Cl2 180.0 2_656 . ? N1 Pt1 Cl1 93.88(5) . . yes N1 Pt1 Cl1 86.12(5) 2_656 . ? N1 Pt1 Cl1 93.88(5) 2_656 2_656 ? N1 Pt1 Cl1 86.12(5) . 2_656 ? N1 Pt1 Cl2 92.84(5) . . ? N1 Pt1 Cl2 87.15(5) 2_656 . ? N1 Pt1 Cl2 87.16(5) . 2_656 ? N1 Pt1 Cl2 92.85(5) 2_656 2_656 ? N1 Pt1 N1 180.0 2_656 . ? C1 N1 Pt1 134.41(14) . . ? C4 C9 C8 120.28(17) . . ? C1 N2 C4 123.81(16) . . ? C6 C7 C8 117.93(17) . . ? C1 C2 C3 110.92(17) . . ? C7 C8 C9 120.22(18) . . ? C9 C4 N2 119.32(16) . . ? C9 C4 C5 120.77(17) . . ? C5 C4 N2 119.91(17) . . ? N1 C1 N2 121.59(17) . . ? N1 C1 C2 119.53(17) . . ? N2 C1 C2 118.75(16) . . ? C7 C6 C5 123.59(17) . . ? C7 C6 N3 118.32(16) . . ? C5 C6 N3 118.06(17) . . ? C6 C5 C4 117.20(17) . . ? O2 N3 C6 118.22(17) . . ? O1 N3 C6 117.96(16) . . ? O1 N3 O2 123.81(17) . . ? #===END======================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 881316' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 Cl4 N4 O2 Pt' _chemical_formula_sum 'C12 H16 Cl4 N4 O2 Pt' _chemical_formula_weight 585.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_Hall 'P 32' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 7.8439(3) _cell_length_b 7.8439(3) _cell_length_c 25.4480(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1355.96(8) _cell_formula_units_Z 3 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 8.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4335 _exptl_absorpt_correction_T_max 0.5198 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8574 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2958 _reflns_number_gt 2884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystaMaker (CrystalMaker Software ltd., 2011)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.3938P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(6) _chemical_absolute_configuration unk _refine_ls_number_reflns 2958 _refine_ls_number_parameters 210 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0513 _refine_ls_wR_factor_gt 0.0506 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.55541(3) 0.86764(3) 0.500000(6) 0.01508(7) Uani 1 1 d . . . Cl1 Cl 0.6219(2) 0.9651(2) 0.58721(6) 0.0224(3) Uani 1 1 d . . . Cl2 Cl 0.4843(2) 0.7644(2) 0.41329(6) 0.0238(3) Uani 1 1 d . . . Cl3 Cl 0.8117(2) 0.7984(2) 0.50102(6) 0.0197(3) Uani 1 1 d . . . Cl4 Cl 0.2970(2) 0.9292(3) 0.50095(5) 0.0231(4) Uani 1 1 d . . . O1 O 1.5859(7) 1.1875(7) 0.26353(19) 0.0316(11) Uani 1 1 d . . . O2 O 1.5309(7) 1.4069(7) 0.22739(18) 0.0263(10) Uani 1 1 d . . . N1 N 0.7255(7) 1.1493(7) 0.47763(19) 0.0159(11) Uani 1 1 d . . . H1 H 0.7029 1.2326 0.4952 0.019 Uiso 1 1 calc R . . N2 N 0.3739(7) 0.5919(8) 0.5247(2) 0.0219(11) Uani 1 1 d . . . N3 N 0.9302(7) 1.1278(7) 0.4171(2) 0.0203(11) Uani 1 1 d . . . H3 H 0.8740 1.0036 0.4267 0.024 Uiso 1 1 calc R . . N4 N 1.4993(7) 1.2827(8) 0.2613(2) 0.0220(12) Uani 1 1 d . . . C1 C 0.8629(8) 1.2326(8) 0.4422(2) 0.0169(12) Uani 1 1 d . . . C2 C 0.9414(9) 1.4478(9) 0.4308(2) 0.0194(13) Uani 1 1 d . . . H2A H 1.0726 1.5038 0.4141 0.023 Uiso 1 1 calc R . . H2B H 0.9572 1.5187 0.4643 0.023 Uiso 1 1 calc R . . C3 C 0.8025(10) 1.4784(10) 0.3942(3) 0.0269(15) Uani 1 1 d . . . H3A H 0.7813 1.4029 0.3618 0.040 Uiso 1 1 calc R . . H3B H 0.8617 1.6185 0.3857 0.040 Uiso 1 1 calc R . . H3C H 0.6761 1.4333 0.4119 0.040 Uiso 1 1 calc R . . C4 C 1.0760(9) 1.1822(9) 0.3776(2) 0.0184(13) Uani 1 1 d . . . C5 C 1.1064(9) 1.3096(9) 0.3364(2) 0.0211(13) Uani 1 1 d . . . H5 H 1.0306 1.3732 0.3341 0.025 Uiso 1 1 calc R . . C6 C 1.2474(9) 1.3444(9) 0.2986(2) 0.0197(13) Uani 1 1 d . . . H6 H 1.2718 1.4341 0.2707 0.024 Uiso 1 1 calc R . . C7 C 1.3518(8) 1.2455(8) 0.3024(2) 0.0150(12) Uani 1 1 d . . . C8 C 1.3216(8) 1.1143(9) 0.3417(3) 0.0206(13) Uani 1 1 d . . . H8 H 1.3933 1.0462 0.3428 0.025 Uiso 1 1 calc R . . C9 C 1.1830(10) 1.0837(9) 0.3800(3) 0.0226(14) Uani 1 1 d . . . H9 H 1.1608 0.9951 0.4081 0.027 Uiso 1 1 calc R . . C10 C 0.2771(9) 0.4413(9) 0.5421(3) 0.0219(14) Uani 1 1 d . . . C11 C 0.1518(10) 0.2534(9) 0.5676(3) 0.0247(14) Uani 1 1 d . . . H11A H 0.2095 0.1673 0.5630 0.030 Uiso 1 1 calc R . . H11B H 0.0206 0.1883 0.5507 0.030 Uiso 1 1 calc R . . C12 C 0.1293(10) 0.2790(10) 0.6252(3) 0.0276(15) Uani 1 1 d . . . H12A H 0.2577 0.3338 0.6425 0.041 Uiso 1 1 calc R . . H12B H 0.0377 0.1510 0.6408 0.041 Uiso 1 1 calc R . . H12C H 0.0778 0.3690 0.6298 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01287(11) 0.01636(12) 0.01557(11) 0.00198(9) 0.00221(9) 0.00699(10) Cl1 0.0213(8) 0.0266(8) 0.0166(8) 0.0006(6) 0.0012(6) 0.0100(7) Cl2 0.0214(8) 0.0259(8) 0.0166(8) -0.0028(6) 0.0001(6) 0.0062(7) Cl3 0.0165(7) 0.0200(8) 0.0259(9) 0.0049(6) 0.0044(6) 0.0117(6) Cl4 0.0180(7) 0.0298(9) 0.0263(10) 0.0038(7) 0.0021(6) 0.0155(6) O1 0.029(3) 0.035(3) 0.038(3) 0.003(2) 0.010(2) 0.021(2) O2 0.029(2) 0.025(2) 0.019(2) 0.004(2) 0.005(2) 0.009(2) N1 0.014(2) 0.018(3) 0.014(3) 0.003(2) 0.003(2) 0.007(2) N2 0.018(3) 0.022(3) 0.026(3) 0.006(2) 0.003(2) 0.010(2) N3 0.022(3) 0.012(2) 0.025(3) 0.005(2) 0.010(2) 0.007(2) N4 0.019(3) 0.025(3) 0.021(3) -0.002(2) 0.000(2) 0.011(2) C1 0.015(3) 0.011(3) 0.018(3) -0.002(2) -0.002(2) 0.002(2) C2 0.019(3) 0.015(3) 0.017(3) -0.002(3) 0.001(3) 0.004(3) C3 0.030(4) 0.023(3) 0.030(4) 0.002(3) 0.000(3) 0.015(3) C4 0.019(3) 0.019(3) 0.011(3) 0.002(2) 0.004(3) 0.006(3) C5 0.021(3) 0.021(3) 0.021(3) 0.004(3) 0.003(3) 0.011(3) C6 0.020(3) 0.015(3) 0.017(3) 0.005(3) -0.001(3) 0.004(3) C7 0.012(3) 0.011(3) 0.018(3) -0.003(2) 0.001(2) 0.003(2) C8 0.014(3) 0.020(3) 0.029(4) 0.000(3) -0.004(3) 0.009(3) C9 0.026(3) 0.025(3) 0.017(3) 0.003(3) 0.001(3) 0.013(3) C10 0.017(3) 0.022(3) 0.026(4) 0.000(3) 0.002(3) 0.009(3) C11 0.021(3) 0.015(3) 0.031(4) 0.005(3) 0.002(3) 0.004(3) C12 0.027(4) 0.032(4) 0.023(3) 0.002(3) 0.001(3) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.005(5) . yes Pt1 N1 2.009(5) . yes Pt1 Cl4 2.3064(15) . yes Pt1 Cl1 2.3202(15) . yes Pt1 Cl2 2.3205(15) . yes Pt1 Cl3 2.3297(14) . yes O1 N4 1.236(7) . ? O2 N4 1.230(7) . ? N1 C1 1.303(7) . yes N1 H1 0.8800 . ? N2 C10 1.128(8) . yes N3 C1 1.340(8) . yes N3 C4 1.418(8) . ? N3 H3 0.8800 . ? N4 C7 1.476(8) . ? C1 C2 1.507(8) . ? C2 C3 1.541(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.384(9) . ? C4 C9 1.398(9) . ? C5 C6 1.387(9) . ? C5 H5 0.9500 . ? C6 C7 1.385(9) . ? C6 H6 0.9500 . ? C7 C8 1.368(9) . ? C8 C9 1.389(9) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.452(9) . ? C11 C12 1.501(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N1 176.2(2) . . yes N2 Pt1 Cl4 89.89(15) . . ? N1 Pt1 Cl4 86.72(15) . . ? N2 Pt1 Cl1 88.66(16) . . ? N1 Pt1 Cl1 89.56(14) . . ? Cl4 Pt1 Cl1 89.85(5) . . ? N2 Pt1 Cl2 90.28(16) . . ? N1 Pt1 Cl2 91.49(14) . . ? Cl4 Pt1 Cl2 89.99(5) . . ? Cl1 Pt1 Cl2 178.93(6) . . yes N2 Pt1 Cl3 88.59(15) . . ? N1 Pt1 Cl3 94.78(15) . . ? Cl4 Pt1 Cl3 178.28(6) . . yes Cl1 Pt1 Cl3 89.32(5) . . ? Cl2 Pt1 Cl3 90.82(5) . . ? C1 N1 Pt1 132.5(4) . . ? C1 N1 H1 113.8 . . ? Pt1 N1 H1 113.8 . . ? C10 N2 Pt1 175.1(6) . . ? C1 N3 C4 131.2(5) . . ? C1 N3 H3 114.4 . . ? C4 N3 H3 114.4 . . ? O2 N4 O1 123.8(5) . . ? O2 N4 C7 118.8(5) . . ? O1 N4 C7 117.4(5) . . ? N1 C1 N3 120.2(5) . . ? N1 C1 C2 117.8(5) . . ? N3 C1 C2 122.0(5) . . ? C1 C2 C3 111.4(5) . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 119.9(5) . . ? C5 C4 N3 125.1(6) . . ? C9 C4 N3 114.8(5) . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 118.6(5) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C8 C7 C6 122.9(6) . . ? C8 C7 N4 119.4(5) . . ? C6 C7 N4 117.7(5) . . ? C7 C8 C9 118.0(5) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? C8 C9 C4 120.5(6) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? N2 C10 C11 176.3(7) . . ? C10 C11 C12 111.4(6) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.88 2.36 3.032(7) 133.9 3_685 N1 H1 N4 0.88 3.15 3.926(7) 149.0 3_685 N3 H3 Cl3 0.88 2.37 3.115(5) 142.5 . N3 H3 Cl2 0.88 2.69 3.225(5) 120.1 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.042 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.119 #===END======================================================================== data_8 _database_code_depnum_ccdc_archive 'CCDC 881317' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Cl3 N6 O4 Pt, H2 O' _chemical_formula_sum 'C18 H22 Cl3 N6 O5 Pt' _chemical_formula_weight 703.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9646(7) _cell_length_b 11.9025(5) _cell_length_c 13.2546(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.4980(10) _cell_angle_gamma 90.00 _cell_volume 2513.93(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6746 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 30.43 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 5.940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4229 _exptl_absorpt_correction_T_max 0.5908 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; The H~2~O molecules and CH~3~ group (C12 and C12B) were disordered over two sites with occupancy ratio 0.58/0.42 and 0.79/0.21 respectively. The C---C distances C11-C12 and C11-C12B were set to be similar. The aniosotropic displacement parameters of the disordered oxygens were restrained so that their U~ij~ components approximate to isotropic behavior. The anisotropic displacement parameters of the disordered carbons were set to be similar. The H~2~O and NH hydrogen atoms were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.98 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 1.54 \%A from atom H12D and the deepest hole is located 1.56 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19613 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5771 _reflns_number_gt 4885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystaMaker (CrystalMaker Software ltd., 2011)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+9.5552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5771 _refine_ls_number_parameters 315 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.201317(11) 0.033010(15) 0.073475(14) 0.01856(6) Uani 1 1 d . . . Cl1 Cl 0.21128(8) 0.15944(10) -0.05663(9) 0.0270(3) Uani 1 1 d . . . Cl2 Cl 0.10345(8) -0.08127(11) -0.03330(10) 0.0274(3) Uani 1 1 d . . . Cl3 Cl 0.18863(10) -0.08905(11) 0.20730(10) 0.0371(3) Uani 1 1 d . . . O1 O 0.4854(3) -0.5442(4) 0.1161(4) 0.0430(11) Uani 1 1 d . . . O2 O 0.4379(3) -0.6821(3) 0.0224(3) 0.0422(11) Uani 1 1 d . . . O3 O 0.5263(2) 0.3006(3) 0.3473(3) 0.0287(8) Uani 1 1 d . . . O4 O 0.4298(2) 0.4255(3) 0.3569(3) 0.0388(10) Uani 1 1 d . . . N1 N 0.3005(3) -0.0463(3) 0.0140(3) 0.0231(9) Uani 1 1 d D . . H1 H 0.3310 0.0010 -0.0197 0.035 Uiso 1 1 d RD . . N3 N 0.2768(3) -0.2320(4) 0.0416(3) 0.0291(10) Uani 1 1 d D . . H3 H 0.2325 -0.2261 0.0771 0.044 Uiso 1 1 d RD . . N5 N 0.4319(3) -0.5869(4) 0.0570(4) 0.0323(10) Uani 1 1 d . . . N2 N 0.1037(3) 0.1213(4) 0.1190(3) 0.0244(9) Uani 1 1 d D . . H2 H 0.0529 0.0945 0.1094 0.037 Uiso 1 1 d RD . . N4 N 0.1773(2) 0.2812(4) 0.1756(3) 0.0230(9) Uani 1 1 d . . . N6 N 0.4545(3) 0.3341(4) 0.3288(3) 0.0250(9) Uani 1 1 d . . . C1 C 0.3184(3) -0.1511(4) -0.0019(4) 0.0218(10) Uani 1 1 d . . . C2 C 0.3841(3) -0.1793(4) -0.0753(4) 0.0253(11) Uani 1 1 d . . . H2A H 0.4129 -0.2501 -0.0547 0.030 Uiso 1 1 calc R . . H2B H 0.4265 -0.1187 -0.0754 0.030 Uiso 1 1 calc R . . C3 C 0.3415(4) -0.1924(6) -0.1809(4) 0.0389(14) Uani 1 1 d . . . H3A H 0.2998 -0.2527 -0.1804 0.058 Uiso 1 1 calc R . . H3B H 0.3837 -0.2109 -0.2289 0.058 Uiso 1 1 calc R . . H3C H 0.3137 -0.1218 -0.2012 0.058 Uiso 1 1 calc R . . C4 C 0.2832(3) -0.3498(4) 0.0202(4) 0.0275(11) Uani 1 1 d . . . C5 C 0.3543(3) -0.4100(4) 0.0517(4) 0.0269(11) Uani 1 1 d . . . H5 H 0.3998 -0.3752 0.0894 0.032 Uiso 1 1 calc R . . C6 C 0.3566(3) -0.5226(4) 0.0261(4) 0.0265(11) Uani 1 1 d . . . C7 C 0.2927(4) -0.5765(5) -0.0259(4) 0.0324(12) Uani 1 1 d . . . H7 H 0.2972 -0.6539 -0.0426 0.039 Uiso 1 1 calc R . . C8 C 0.2211(4) -0.5166(5) -0.0540(5) 0.0370(14) Uani 1 1 d . . . H8 H 0.1748 -0.5533 -0.0883 0.044 Uiso 1 1 calc R . . C9 C 0.2166(4) -0.4019(5) -0.0322(5) 0.0352(13) Uani 1 1 d . . . H9 H 0.1680 -0.3601 -0.0532 0.042 Uiso 1 1 calc R . . C10 C 0.1058(3) 0.2251(4) 0.1495(4) 0.0251(11) Uani 1 1 d . A . C11 C 0.0265(4) 0.2922(5) 0.1590(6) 0.0485(19) Uani 1 1 d D . . C12 C 0.0145(7) 0.3675(11) 0.0569(9) 0.057(4) Uani 0.580(14) 1 d PDU A 1 H12A H 0.0648 0.4131 0.0494 0.086 Uiso 0.580(14) 1 calc PR A 1 H12B H -0.0343 0.4169 0.0614 0.086 Uiso 0.580(14) 1 calc PR A 1 H12C H 0.0055 0.3179 -0.0018 0.086 Uiso 0.580(14) 1 calc PR A 1 H11A H 0.0319 0.3428 0.2165 0.068 Uiso 0.58 1 d P A 1 H11B H -0.0219 0.2431 0.1627 0.068 Uiso 0.58 1 d P A 1 C12B C 0.0160(18) 0.287(3) 0.2823(9) 0.119(11) Uani 0.420(14) 1 d PDU A 2 H12D H -0.0027 0.2119 0.3009 0.179 Uiso 0.420(14) 1 calc PR A 2 H12E H -0.0255 0.3428 0.3008 0.179 Uiso 0.420(14) 1 calc PR A 2 H12F H 0.0701 0.3035 0.3182 0.179 Uiso 0.420(14) 1 calc PR A 2 H11C H -0.0221 0.2617 0.1167 0.143 Uiso 0.42 1 d P A 2 H11D H 0.0344 0.3736 0.1370 0.143 Uiso 0.42 1 d P A 2 C13 C 0.2579(3) 0.2349(4) 0.1910(4) 0.0198(10) Uani 1 1 d . . . C14 C 0.3166(3) 0.3031(4) 0.2442(4) 0.0223(10) Uani 1 1 d . . . H14 H 0.3022 0.3776 0.2621 0.027 Uiso 1 1 calc R . . C15 C 0.3947(3) 0.2617(4) 0.2703(4) 0.0212(10) Uani 1 1 d . . . C16 C 0.4186(3) 0.1533(4) 0.2462(4) 0.0244(11) Uani 1 1 d . . . H16 H 0.4726 0.1253 0.2669 0.029 Uiso 1 1 calc R . . C17 C 0.3610(3) 0.0876(4) 0.1910(4) 0.0245(11) Uani 1 1 d . . . H17 H 0.3762 0.0135 0.1729 0.029 Uiso 1 1 calc R . . C18 C 0.2811(3) 0.1274(4) 0.1612(4) 0.0198(10) Uani 1 1 d . . . O5 O -0.1614(3) 0.0048(4) 0.2570(3) 0.0259(10) Uani 0.795(6) 1 d P B 3 H5A H -0.1442 0.0009 0.1988 0.039 Uiso 0.795(6) 1 d PR B 3 H5B H -0.1652 -0.0652 0.2807 0.039 Uiso 0.795(6) 1 d PR B 3 O5B O -0.1205(11) 0.0890(13) 0.2949(12) 0.0259(10) Uani 0.205(6) 1 d P B 4 H5BA H -0.1487 0.0306 0.2904 0.039 Uiso 0.205(6) 1 d PR B 4 H5BB H -0.0796 0.0831 0.2560 0.039 Uiso 0.205(6) 1 d PR B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02007(10) 0.01307(9) 0.02227(10) -0.00342(8) -0.00073(6) 0.00080(8) Cl1 0.0346(7) 0.0193(6) 0.0267(6) 0.0017(5) -0.0007(5) -0.0024(5) Cl2 0.0239(6) 0.0210(6) 0.0368(7) -0.0091(5) -0.0018(5) -0.0040(5) Cl3 0.0600(10) 0.0227(6) 0.0292(7) 0.0034(6) 0.0070(6) -0.0009(7) O1 0.036(2) 0.036(2) 0.056(3) -0.003(2) -0.011(2) 0.001(2) O2 0.044(3) 0.022(2) 0.061(3) -0.006(2) 0.004(2) 0.0096(19) O3 0.0213(18) 0.030(2) 0.034(2) -0.0054(17) -0.0074(15) 0.0022(16) O4 0.027(2) 0.029(2) 0.060(3) -0.022(2) -0.0075(19) 0.0023(18) N1 0.023(2) 0.017(2) 0.029(2) -0.0078(17) -0.0030(17) 0.0030(17) N3 0.029(2) 0.020(2) 0.038(3) -0.002(2) 0.007(2) 0.0043(19) N5 0.034(3) 0.024(2) 0.040(3) 0.001(2) 0.005(2) 0.003(2) N2 0.0131(19) 0.021(2) 0.039(2) -0.0074(19) -0.0003(17) -0.0012(17) N4 0.015(2) 0.021(2) 0.032(2) -0.0063(18) -0.0018(17) 0.0035(17) N6 0.025(2) 0.022(2) 0.027(2) -0.0066(18) -0.0012(17) 0.0004(19) C1 0.023(2) 0.021(2) 0.021(2) -0.005(2) -0.0046(19) 0.001(2) C2 0.025(3) 0.019(2) 0.032(3) 0.001(2) 0.002(2) 0.002(2) C3 0.043(4) 0.046(4) 0.028(3) -0.007(3) 0.008(2) -0.005(3) C4 0.032(3) 0.018(2) 0.033(3) 0.000(2) 0.007(2) 0.000(2) C5 0.030(3) 0.023(3) 0.028(3) 0.000(2) 0.000(2) -0.001(2) C6 0.028(3) 0.023(3) 0.029(3) 0.003(2) 0.004(2) 0.001(2) C7 0.038(3) 0.017(2) 0.042(3) -0.004(2) 0.001(2) 0.000(2) C8 0.038(3) 0.024(3) 0.048(4) 0.000(3) -0.003(3) -0.004(3) C9 0.031(3) 0.029(3) 0.046(3) 0.003(3) -0.003(2) 0.001(3) C10 0.021(2) 0.022(3) 0.032(3) -0.006(2) 0.003(2) 0.002(2) C11 0.018(3) 0.039(4) 0.089(5) -0.032(4) 0.000(3) 0.006(3) C12 0.034(6) 0.053(7) 0.084(8) 0.016(6) 0.000(5) 0.009(5) C12B 0.098(13) 0.130(14) 0.131(14) -0.017(9) 0.014(9) 0.015(9) C13 0.024(2) 0.016(2) 0.020(2) -0.0016(19) 0.0023(18) 0.004(2) C14 0.023(2) 0.017(2) 0.026(2) -0.006(2) -0.0002(19) 0.002(2) C15 0.024(2) 0.019(2) 0.020(2) -0.004(2) -0.0011(19) -0.001(2) C16 0.024(3) 0.023(3) 0.026(3) -0.004(2) -0.005(2) 0.005(2) C17 0.024(3) 0.019(2) 0.030(3) -0.006(2) -0.006(2) 0.006(2) C18 0.024(2) 0.014(2) 0.021(2) -0.0057(18) -0.0026(18) -0.0005(19) O5 0.038(3) 0.0115(19) 0.028(2) 0.0073(17) -0.0006(19) -0.0081(18) O5B 0.038(3) 0.0115(19) 0.028(2) 0.0073(17) -0.0006(19) -0.0081(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.003(4) . yes Pt1 C18 2.014(5) . yes Pt1 N1 2.043(4) . yes Pt1 Cl1 2.3015(12) . yes Pt1 Cl3 2.3113(13) . yes Pt1 Cl2 2.4545(12) . yes O1 N5 1.232(6) . ? O2 N5 1.228(6) . ? O3 N6 1.223(5) . ? O4 N6 1.224(6) . ? N1 C1 1.299(6) . yes N1 H1 0.8831 . ? N3 C1 1.323(7) . yes N3 C4 1.435(6) . ? N3 H3 0.8752 . ? N5 C6 1.462(7) . ? N2 C10 1.299(6) . yes N2 H2 0.8739 . ? N4 C10 1.349(6) . yes N4 C13 1.402(6) . ? N6 C15 1.472(6) . ? C1 C2 1.512(7) . ? C2 C3 1.526(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C9 1.381(8) . ? C4 C5 1.385(7) . ? C5 C6 1.385(7) . ? C5 H5 0.9500 . ? C6 C7 1.358(8) . ? C7 C8 1.379(8) . ? C7 H7 0.9500 . ? C8 C9 1.398(8) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.510(7) . ? C11 C12 1.626(8) . ? C11 C12B 1.653(9) . ? C11 H11A 0.9703 . ? C11 H11B 0.9730 . ? C11 H11C 0.9971 . ? C11 H11D 1.0217 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 H11D 1.0921 . ? C12B H11A 1.1360 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13 C18 1.396(6) . ? C13 C14 1.397(7) . ? C14 C15 1.367(7) . ? C14 H14 0.9500 . ? C15 C16 1.388(7) . ? C16 C17 1.382(7) . ? C16 H16 0.9500 . ? C17 C18 1.394(7) . ? C17 H17 0.9500 . ? O5 H5A 0.8352 . ? O5 H5B 0.8944 . ? O5 H5BA 0.5672 . ? O5B H5BA 0.8288 . ? O5B H5BB 0.8594 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 C18 90.57(18) . . yes N2 Pt1 N1 173.98(18) . . yes C18 Pt1 N1 90.14(18) . . ? N2 Pt1 Cl1 88.47(13) . . ? C18 Pt1 Cl1 89.85(14) . . ? N1 Pt1 Cl1 85.56(13) . . ? N2 Pt1 Cl3 89.56(13) . . ? C18 Pt1 Cl3 89.42(14) . . ? N1 Pt1 Cl3 96.42(13) . . ? Cl1 Pt1 Cl3 177.89(5) . . yes N2 Pt1 Cl2 89.13(12) . . ? C18 Pt1 Cl2 179.69(15) . . ? N1 Pt1 Cl2 90.14(12) . . ? Cl1 Pt1 Cl2 90.06(4) . . yes Cl3 Pt1 Cl2 90.67(5) . . ? C1 N1 Pt1 133.6(4) . . ? C1 N1 H1 113.3 . . ? Pt1 N1 H1 111.4 . . ? C1 N3 C4 125.5(5) . . ? C1 N3 H3 128.2 . . ? C4 N3 H3 104.8 . . ? O2 N5 O1 123.4(5) . . ? O2 N5 C6 117.3(5) . . ? O1 N5 C6 119.2(5) . . ? C10 N2 Pt1 125.9(4) . . ? C10 N2 H2 113.5 . . ? Pt1 N2 H2 119.8 . . ? C10 N4 C13 126.7(4) . . ? O3 N6 O4 123.0(4) . . ? O3 N6 C15 119.0(4) . . ? O4 N6 C15 118.0(4) . . ? N1 C1 N3 120.5(5) . . ? N1 C1 C2 119.1(5) . . ? N3 C1 C2 120.4(4) . . ? C1 C2 C3 109.0(4) . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 120.7(5) . . ? C9 C4 N3 118.4(5) . . ? C5 C4 N3 120.9(5) . . ? C6 C5 C4 117.4(5) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? C7 C6 C5 123.5(5) . . ? C7 C6 N5 118.4(5) . . ? C5 C6 N5 118.1(5) . . ? C6 C7 C8 118.5(5) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C7 C8 C9 120.0(5) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C4 C9 C8 119.7(5) . . ? C4 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 N4 123.8(5) . . ? N2 C10 C11 121.5(5) . . ? N4 C10 C11 114.7(5) . . ? C10 C11 C12 106.2(6) . . ? C10 C11 C12B 101.5(11) . . ? C12 C11 C12B 146.1(13) . . ? C10 C11 H11A 111.1 . . ? C12 C11 H11A 108.2 . . ? C12B C11 H11A 42.0 . . ? C10 C11 H11B 111.1 . . ? C12 C11 H11B 108.6 . . ? C12B C11 H11B 78.4 . . ? H11A C11 H11B 111.5 . . ? C10 C11 H11C 112.8 . . ? C12 C11 H11C 71.6 . . ? C12B C11 H11C 114.9 . . ? H11A C11 H11C 134.1 . . ? H11B C11 H11C 38.5 . . ? C10 C11 H11D 111.0 . . ? C12 C11 H11D 41.3 . . ? C12B C11 H11D 109.9 . . ? H11A C11 H11D 68.3 . . ? H11B C11 H11D 134.2 . . ? H11C C11 H11D 106.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? C11 C12 H11D 38.2 . . ? H12A C12 H11D 82.5 . . ? H12B C12 H11D 94.9 . . ? H12C C12 H11D 146.2 . . ? C11 C12B H11A 34.9 . . ? C11 C12B H12D 109.5 . . ? C11 C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11 C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C18 C13 C14 119.5(4) . . ? C18 C13 N4 125.2(4) . . ? C14 C13 N4 115.2(4) . . ? C15 C14 C13 119.5(4) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 122.4(5) . . ? C14 C15 N6 118.4(4) . . ? C16 C15 N6 119.1(4) . . ? C17 C16 C15 117.7(5) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C16 C17 C18 121.7(5) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C13 119.0(4) . . ? C17 C18 Pt1 120.6(3) . . ? C13 C18 Pt1 120.3(4) . . ? H5A O5 H5B 107.8 . . ? H5A O5 H5BA 129.0 . . ? H5B O5 H5BA 105.0 . . ? H5BA O5B H5BB 108.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O4 0.88 2.50 3.345(6) 160.7 4_565 N3 H3 Cl3 0.88 2.51 3.174(5) 133.7 . N2 H2 Cl2 0.87 2.64 3.463(4) 157.8 3 O5 H5A Cl2 0.84 2.52 3.288(5) 154.3 3 O5 H5A Cl1 0.84 2.85 3.354(5) 121.1 3 O5 H5B N4 0.89 1.93 2.824(6) 176.4 2_545 O5B H5BB Cl2 0.86 2.95 3.496(17) 123.0 3 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.148 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.145 # start Validation Reply Form _vrf_PUBL220_GLOBAL ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.01 Ratio RESPONSE: Large ratio is due to the disordered CH~3~ group. ; # end Validation Reply Form #===END======================================================================== data_10 _database_code_depnum_ccdc_archive 'CCDC 881318' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H13 Cl4 N3 O3 Pt, 2(H2 O)' _chemical_formula_sum 'C9 H17 Cl4 N3 O5 Pt' _chemical_formula_weight 584.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7248(7) _cell_length_b 8.0570(5) _cell_length_c 16.8733(13) _cell_angle_alpha 79.899(6) _cell_angle_beta 81.282(7) _cell_angle_gamma 72.243(6) _cell_volume 852.47(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11610 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 32.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 8.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1726 _exptl_absorpt_correction_T_max 0.6134 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The OH, NH, and NH~2~ hydrogen atoms were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 1.18 \%A from atom Pt1 and the deepest hole is located 0.77 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16984 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 32.00 _reflns_number_total 5811 _reflns_number_gt 5068 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'EvalCCD (Duisenberg, 2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 2003)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1f (Brandenburg, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.7426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5811 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.989303(17) 0.760250(14) 0.259139(7) 0.00929(3) Uani 1 1 d . . . Cl1 Cl 1.15125(11) 0.49972(9) 0.20523(4) 0.01461(14) Uani 1 1 d . . . Cl2 Cl 1.28215(11) 0.70978(9) 0.32691(4) 0.01466(14) Uani 1 1 d . . . Cl3 Cl 0.83325(11) 0.60465(9) 0.36720(4) 0.01412(14) Uani 1 1 d . . . Cl4 Cl 1.13615(12) 0.91696(10) 0.15041(4) 0.01737(15) Uani 1 1 d . . . O1 O 0.5302(3) 0.9959(3) 0.32633(13) 0.0171(5) Uani 1 1 d . . . H1O H 0.4119 1.0611 0.3322 0.026 Uiso 1 1 d R . . O2 O 0.6285(4) 0.2293(3) 0.17026(14) 0.0195(5) Uani 1 1 d . . . O3 O 0.7127(4) 0.2084(3) 0.04242(15) 0.0250(5) Uani 1 1 d . . . O4 O 0.9693(4) 0.7935(4) 0.49490(15) 0.0355(7) Uani 1 1 d . . . H4O H 0.9238 0.7267 0.4670 0.053 Uiso 1 1 d R . . H4P H 1.0802 0.8044 0.4716 0.053 Uiso 1 1 d R . . O5 O 0.8518(3) 0.8156(3) 0.65278(13) 0.0169(4) Uani 1 1 d . . . H5O H 0.8740 0.8218 0.5968 0.025 Uiso 1 1 d R . . H5P H 0.8731 0.7128 0.6762 0.025 Uiso 1 1 d R . . N1 N 0.8666(4) 0.9883(3) 0.30778(15) 0.0118(5) Uani 1 1 d . . . H1N H 0.9577 1.0394 0.3138 0.018 Uiso 1 1 d R . . N2 N 0.7195(4) 0.8159(3) 0.19796(15) 0.0119(5) Uani 1 1 d . . . H2N H 0.6797 0.9264 0.1873 0.018 Uiso 1 1 d R . . H2M H 0.6398 0.7890 0.2413 0.018 Uiso 1 1 d R . . N3 N 0.6794(4) 0.2896(3) 0.10036(16) 0.0151(5) Uani 1 1 d . . . C1 C 0.6775(5) 1.0686(4) 0.33049(18) 0.0135(6) Uani 1 1 d . . . C2 C 0.6180(5) 1.2419(4) 0.36222(19) 0.0167(6) Uani 1 1 d . . . H2A H 0.5024 1.3258 0.3331 0.020 Uiso 1 1 calc R . . H2B H 0.7398 1.2903 0.3513 0.020 Uiso 1 1 calc R . . C3 C 0.5480(6) 1.2246(5) 0.4536(2) 0.0286(8) Uani 1 1 d . . . H3A H 0.4252 1.1796 0.4645 0.043 Uiso 1 1 calc R . . H3B H 0.5114 1.3402 0.4718 0.043 Uiso 1 1 calc R . . H3C H 0.6627 1.1431 0.4826 0.043 Uiso 1 1 calc R . . C4 C 0.7248(5) 0.7204(4) 0.13195(18) 0.0122(6) Uani 1 1 d . . . C5 C 0.7649(5) 0.7946(4) 0.05282(18) 0.0143(6) Uani 1 1 d . . . H5 H 0.7890 0.9070 0.0420 0.017 Uiso 1 1 calc R . . C6 C 0.7696(5) 0.7040(4) -0.01059(19) 0.0162(6) Uani 1 1 d . . . H6 H 0.7930 0.7561 -0.0649 0.019 Uiso 1 1 calc R . . C7 C 0.7405(5) 0.5383(4) 0.00484(18) 0.0136(6) Uani 1 1 d . . . H7 H 0.7461 0.4743 -0.0381 0.016 Uiso 1 1 calc R . . C8 C 0.7028(4) 0.4685(4) 0.08470(18) 0.0124(6) Uani 1 1 d . . . C9 C 0.6911(4) 0.5561(4) 0.14960(18) 0.0117(5) Uani 1 1 d . . . H9 H 0.6613 0.5059 0.2037 0.014 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00963(5) 0.00750(5) 0.01059(5) -0.00203(3) 0.00017(4) -0.00235(4) Cl1 0.0163(3) 0.0119(3) 0.0138(3) -0.0050(3) 0.0001(3) -0.0003(3) Cl2 0.0118(3) 0.0142(3) 0.0181(3) -0.0033(3) -0.0027(3) -0.0027(3) Cl3 0.0162(3) 0.0115(3) 0.0143(3) -0.0019(3) 0.0021(3) -0.0051(3) Cl4 0.0171(3) 0.0167(4) 0.0165(3) 0.0015(3) 0.0024(3) -0.0063(3) O1 0.0113(10) 0.0157(11) 0.0252(12) -0.0090(9) 0.0015(9) -0.0033(9) O2 0.0228(12) 0.0138(11) 0.0209(12) 0.0022(9) -0.0003(9) -0.0073(10) O3 0.0415(15) 0.0121(11) 0.0248(13) -0.0080(10) -0.0083(11) -0.0074(11) O4 0.0313(14) 0.0554(19) 0.0239(14) -0.0095(13) 0.0015(11) -0.0182(14) O5 0.0173(11) 0.0144(11) 0.0184(11) -0.0013(9) -0.0026(9) -0.0040(9) N1 0.0139(12) 0.0090(11) 0.0154(12) -0.0037(10) -0.0042(10) -0.0051(10) N2 0.0136(12) 0.0086(11) 0.0132(12) -0.0052(9) -0.0013(9) -0.0008(10) N3 0.0154(12) 0.0097(12) 0.0203(13) -0.0017(10) -0.0058(10) -0.0018(10) C1 0.0180(14) 0.0118(14) 0.0129(13) -0.0022(11) -0.0033(11) -0.0066(12) C2 0.0168(15) 0.0125(14) 0.0215(16) -0.0073(12) -0.0007(12) -0.0032(12) C3 0.0316(19) 0.036(2) 0.0223(18) -0.0166(16) 0.0022(15) -0.0113(17) C4 0.0114(13) 0.0122(14) 0.0144(14) -0.0050(11) 0.0002(11) -0.0042(11) C5 0.0179(14) 0.0097(13) 0.0158(14) 0.0010(11) -0.0023(12) -0.0061(12) C6 0.0194(15) 0.0156(15) 0.0131(14) -0.0023(12) -0.0003(12) -0.0050(13) C7 0.0154(14) 0.0129(14) 0.0124(13) -0.0039(11) -0.0024(11) -0.0022(12) C8 0.0117(13) 0.0085(13) 0.0167(14) -0.0025(11) -0.0009(11) -0.0024(11) C9 0.0114(13) 0.0091(13) 0.0139(13) -0.0008(11) -0.0026(11) -0.0017(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.032(2) . yes Pt1 N2 2.114(2) . yes Pt1 Cl4 2.3095(8) . yes Pt1 Cl2 2.3200(8) . yes Pt1 Cl1 2.3226(7) . yes Pt1 Cl3 2.3276(7) . yes O1 C1 1.311(4) . ? O1 H1O 0.8115 . ? O2 N3 1.234(3) . ? O3 N3 1.226(3) . ? O4 H4O 0.9159 . ? O4 H4P 0.8108 . ? O5 H5O 0.9283 . ? O5 H5P 0.8332 . ? N1 C1 1.273(4) . ? N1 H1N 0.8619 . ? N2 C4 1.451(4) . ? N2 H2N 0.8427 . ? N2 H2M 0.8744 . ? N3 C8 1.471(4) . ? C1 C2 1.501(4) . ? C2 C3 1.537(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C9 1.384(4) . ? C4 C5 1.386(4) . ? C5 C6 1.389(4) . ? C5 H5 0.9500 . ? C6 C7 1.382(4) . ? C6 H6 0.9500 . ? C7 C8 1.383(4) . ? C7 H7 0.9500 . ? C8 C9 1.384(4) . ? C9 H9 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N2 90.29(9) . . ? N1 Pt1 Cl4 87.83(7) . . ? N2 Pt1 Cl4 89.05(7) . . ? N1 Pt1 Cl2 87.76(7) . . ? N2 Pt1 Cl2 177.94(7) . . ? Cl4 Pt1 Cl2 90.25(3) . . ? N1 Pt1 Cl1 176.21(7) . . ? N2 Pt1 Cl1 93.25(7) . . ? Cl4 Pt1 Cl1 90.90(3) . . ? Cl2 Pt1 Cl1 88.69(3) . . ? N1 Pt1 Cl3 92.00(7) . . ? N2 Pt1 Cl3 89.49(7) . . ? Cl4 Pt1 Cl3 178.53(3) . . ? Cl2 Pt1 Cl3 91.21(3) . . ? Cl1 Pt1 Cl3 89.37(3) . . ? C1 O1 H1O 114.0 . . ? H4O O4 H4P 107.7 . . ? H5O O5 H5P 112.8 . . ? C1 N1 Pt1 130.7(2) . . ? C1 N1 H1N 114.6 . . ? Pt1 N1 H1N 114.7 . . ? C4 N2 Pt1 119.80(18) . . ? C4 N2 H2N 115.5 . . ? Pt1 N2 H2N 104.9 . . ? C4 N2 H2M 113.5 . . ? Pt1 N2 H2M 94.6 . . ? H2N N2 H2M 106.0 . . ? O3 N3 O2 123.7(3) . . ? O3 N3 C8 117.4(2) . . ? O2 N3 C8 118.9(2) . . ? N1 C1 O1 118.4(3) . . ? N1 C1 C2 122.5(3) . . ? O1 C1 C2 119.1(3) . . ? C1 C2 C3 112.1(3) . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 121.5(3) . . ? C9 C4 N2 119.1(3) . . ? C5 C4 N2 119.5(3) . . ? C4 C5 C6 119.7(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 118.0(3) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? C7 C8 C9 123.5(3) . . ? C7 C8 N3 117.4(3) . . ? C9 C8 N3 119.1(3) . . ? C4 C9 C8 116.9(3) . . ? C4 C9 H9 121.6 . . ? C8 C9 H9 121.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O5 H5P Cl1 0.83 2.41 3.175(2) 152.1 2_766 yes O5 H5P Cl3 0.83 2.85 3.446(2) 130.2 2_766 yes O5 H5O O4 0.93 1.77 2.682(3) 166.8 . yes O4 H4O Cl3 0.92 2.33 3.224(3) 165.2 . yes O4 H4P Cl2 0.81 2.72 3.304(3) 130.4 . yes N1 H1N O5 0.86 2.16 3.016(3) 169.8 2_776 yes N2 H2N O2 0.84 2.33 3.161(3) 168.4 1_565 yes N2 H2M O1 0.87 2.27 2.749(3) 114.4 . yes N2 H2M Cl3 0.87 2.64 3.130(3) 116.6 . yes N2 H2M Cl2 0.87 2.80 3.613(3) 155.4 1_455 yes O1 H1O O5 0.81 1.75 2.562(3) 174.6 2_676 yes _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.991 _refine_diff_density_min -1.832 _refine_diff_density_rms 0.208 #===END======================================================================== data_11 _database_code_depnum_ccdc_archive 'CCDC 881319' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H20 Cl4 N4 O3 Pt' _chemical_formula_sum 'C13 H20 Cl4 N4 O3 Pt' _chemical_formula_weight 617.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.59850(10) _cell_length_b 7.95740(10) _cell_length_c 19.0913(4) _cell_angle_alpha 87.0580(10) _cell_angle_beta 86.2180(10) _cell_angle_gamma 74.5110(10) _cell_volume 963.32(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8637 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 30.45 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 7.858 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2532 _exptl_absorpt_correction_T_max 0.7138 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; The NH hydrogen atoms were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.74 \%A from atom Pt1 and the deepest hole is located 0.74 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'flat graphite crystal' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on three-circle goniostat' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_measurement_method '\f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18919 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 30.61 _reflns_number_total 5860 _reflns_number_gt 5044 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SIR2008 (Burla et al., 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystaMaker (CrystalMaker Software ltd., 2011)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0134P)^2^+2.9253P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5860 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.89381(3) 0.28427(2) 0.301327(9) 0.01241(5) Uani 1 1 d . . . Cl1 Cl 1.02355(17) 0.52485(13) 0.31390(6) 0.0182(2) Uani 1 1 d . . . Cl2 Cl 0.69329(17) 0.33929(14) 0.40550(6) 0.0192(2) Uani 1 1 d . . . Cl3 Cl 0.76917(17) 0.04281(13) 0.28866(6) 0.0200(2) Uani 1 1 d . . . Cl4 Cl 1.09221(17) 0.22992(14) 0.19592(6) 0.0189(2) Uani 1 1 d . . . O1 O 0.6631(5) 1.2411(4) 0.09912(17) 0.0245(7) Uani 1 1 d . . . O2 O 0.7415(5) 1.2367(4) -0.01304(17) 0.0212(7) Uani 1 1 d . . . O3 O 1.3808(5) -0.0389(4) 0.42433(17) 0.0210(7) Uani 1 1 d . . . N1 N 0.6366(5) 0.4233(4) 0.25265(18) 0.0143(7) Uani 1 1 d . . . H1 H 0.5238 0.3892 0.2624 0.021 Uiso 1 1 d R . . N3 N 0.7535(5) 0.6201(4) 0.17855(19) 0.0154(7) Uani 1 1 d . . . H3 H 0.8639 0.6085 0.1985 0.023 Uiso 1 1 d R . . N4 N 0.7148(5) 1.1644(4) 0.04389(19) 0.0157(7) Uani 1 1 d . . . N2 N 1.1427(5) 0.1158(4) 0.34673(19) 0.0157(7) Uani 1 1 d . . . H2 H 1.1840 0.0230 0.3203 0.024 Uiso 1 1 d R . . C1 C 0.6068(6) 0.5375(5) 0.2006(2) 0.0144(8) Uani 1 1 d . . . C2 C 0.3990(6) 0.5882(5) 0.1671(2) 0.0148(8) Uani 1 1 d . . . H2A H 0.3191 0.5018 0.1813 0.018 Uiso 1 1 calc R . . H2B H 0.4233 0.5871 0.1154 0.018 Uiso 1 1 calc R . . C3 C 0.2694(7) 0.7699(6) 0.1885(2) 0.0191(9) Uani 1 1 d . . . H3A H 0.2317 0.7678 0.2390 0.029 Uiso 1 1 calc R . . H3B H 0.1409 0.8042 0.1624 0.029 Uiso 1 1 calc R . . H3C H 0.3527 0.8541 0.1778 0.029 Uiso 1 1 calc R . . C4 C 0.7551(6) 0.7126(5) 0.1126(2) 0.0139(8) Uani 1 1 d . . . C5 C 0.7368(6) 0.8910(5) 0.1113(2) 0.0125(8) Uani 1 1 d . . . H5 H 0.7208 0.9530 0.1535 0.015 Uiso 1 1 calc R . . C6 C 0.7429(6) 0.9745(5) 0.0461(2) 0.0132(8) Uani 1 1 d . . . C7 C 0.7658(6) 0.8906(5) -0.0168(2) 0.0150(8) Uani 1 1 d . . . H7 H 0.7708 0.9524 -0.0605 0.018 Uiso 1 1 calc R . . C8 C 0.7813(6) 0.7139(5) -0.0138(2) 0.0159(8) Uani 1 1 d . . . H8 H 0.7948 0.6528 -0.0561 0.019 Uiso 1 1 calc R . . C9 C 0.7771(6) 0.6248(5) 0.0507(2) 0.0164(8) Uani 1 1 d . . . H9 H 0.7894 0.5030 0.0522 0.020 Uiso 1 1 calc R . . C10 C 1.2341(6) 0.1042(6) 0.4052(2) 0.0169(9) Uani 1 1 d . . . C11 C 1.1913(7) 0.2403(6) 0.4578(2) 0.0203(9) Uani 1 1 d . . . H11A H 1.0902 0.3463 0.4394 0.024 Uiso 1 1 calc R . . H11B H 1.3237 0.2710 0.4657 0.024 Uiso 1 1 calc R . . C12 C 1.1013(8) 0.1817(7) 0.5278(3) 0.0271(10) Uani 1 1 d . . . H12A H 0.9630 0.1629 0.5212 0.041 Uiso 1 1 calc R . . H12B H 1.0864 0.2720 0.5622 0.041 Uiso 1 1 calc R . . H12C H 1.1966 0.0727 0.5448 0.041 Uiso 1 1 calc R . . C13 C 1.4310(7) -0.1901(6) 0.3813(3) 0.0236(10) Uani 1 1 d . . . H13A H 1.3023 -0.2253 0.3746 0.035 Uiso 1 1 calc R . . H13B H 1.5324 -0.2861 0.4046 0.035 Uiso 1 1 calc R . . H13C H 1.4923 -0.1616 0.3356 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01647(7) 0.00787(7) 0.01171(8) 0.00047(5) -0.00002(5) -0.00151(5) Cl1 0.0260(5) 0.0149(5) 0.0151(5) 0.0003(4) -0.0028(4) -0.0078(4) Cl2 0.0212(5) 0.0191(5) 0.0145(5) 0.0010(4) 0.0034(4) -0.0017(4) Cl3 0.0280(5) 0.0141(5) 0.0192(6) 0.0029(4) -0.0041(4) -0.0079(4) Cl4 0.0250(5) 0.0149(5) 0.0134(5) -0.0005(4) 0.0024(4) -0.0004(4) O1 0.0416(19) 0.0106(15) 0.0213(18) -0.0025(13) -0.0031(15) -0.0063(14) O2 0.0258(16) 0.0155(15) 0.0228(18) 0.0064(13) -0.0028(13) -0.0073(13) O3 0.0222(15) 0.0168(16) 0.0214(17) 0.0025(13) -0.0056(13) -0.0002(13) N1 0.0140(16) 0.0108(16) 0.0158(19) 0.0028(14) 0.0011(13) -0.0003(13) N3 0.0164(16) 0.0129(17) 0.0169(19) 0.0062(14) -0.0065(14) -0.0041(14) N4 0.0159(16) 0.0128(17) 0.0182(19) 0.0023(15) -0.0028(14) -0.0033(14) N2 0.0203(17) 0.0105(17) 0.0140(18) -0.0017(14) -0.0002(14) 0.0001(14) C1 0.0169(19) 0.0098(19) 0.015(2) -0.0021(16) 0.0013(16) -0.0016(15) C2 0.0156(18) 0.0125(19) 0.016(2) 0.0002(16) -0.0007(16) -0.0041(16) C3 0.0168(19) 0.016(2) 0.021(2) 0.0010(18) 0.0006(17) -0.0007(17) C4 0.0109(17) 0.0122(19) 0.017(2) 0.0030(16) -0.0018(15) -0.0016(15) C5 0.0124(17) 0.0111(19) 0.013(2) -0.0008(15) -0.0028(15) -0.0009(15) C6 0.0123(17) 0.0091(18) 0.018(2) 0.0003(16) -0.0023(15) -0.0026(14) C7 0.0137(18) 0.017(2) 0.014(2) 0.0036(16) -0.0010(15) -0.0041(16) C8 0.0157(19) 0.015(2) 0.016(2) -0.0029(17) -0.0005(16) -0.0007(16) C9 0.0166(19) 0.012(2) 0.020(2) -0.0004(17) 0.0006(16) -0.0039(16) C10 0.0173(19) 0.016(2) 0.018(2) 0.0057(17) -0.0015(16) -0.0065(16) C11 0.025(2) 0.018(2) 0.019(2) -0.0017(18) 0.0027(18) -0.0069(18) C12 0.032(3) 0.030(3) 0.020(3) -0.003(2) -0.002(2) -0.008(2) C13 0.023(2) 0.015(2) 0.028(3) 0.0013(19) -0.0017(19) 0.0013(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.017(3) . yes Pt1 N2 2.034(3) . yes Pt1 Cl2 2.3089(11) . yes Pt1 Cl3 2.3118(10) . yes Pt1 Cl4 2.3217(11) . yes Pt1 Cl1 2.3249(10) . yes O1 N4 1.228(5) . ? O2 N4 1.228(5) . ? O3 C10 1.334(5) . yes O3 C13 1.444(5) . ? N1 C1 1.299(5) . yes N1 H1 0.8644 . ? N3 C1 1.343(5) . yes N3 C4 1.426(5) . ? N3 H3 0.8252 . ? N4 C6 1.471(5) . ? N2 C10 1.291(5) . yes N2 H2 0.8867 . ? C1 C2 1.499(6) . ? C2 C3 1.531(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C9 1.383(6) . ? C4 C5 1.391(5) . ? C5 C6 1.384(6) . ? C5 H5 0.9500 . ? C6 C7 1.383(6) . ? C7 C8 1.381(6) . ? C7 H7 0.9500 . ? C8 C9 1.391(6) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.475(6) . ? C11 C12 1.528(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N2 172.49(14) . . yes N1 Pt1 Cl2 87.01(10) . . yes N2 Pt1 Cl2 94.25(10) . . yes N1 Pt1 Cl3 86.58(10) . . ? N2 Pt1 Cl3 86.03(10) . . ? Cl2 Pt1 Cl3 89.35(4) . . ? N1 Pt1 Cl4 92.40(10) . . ? N2 Pt1 Cl4 86.32(10) . . ? Cl2 Pt1 Cl4 179.39(5) . . ? Cl3 Pt1 Cl4 90.47(4) . . ? N1 Pt1 Cl1 94.04(10) . . ? N2 Pt1 Cl1 93.34(10) . . ? Cl2 Pt1 Cl1 91.08(4) . . ? Cl3 Pt1 Cl1 179.27(4) . . ? Cl4 Pt1 Cl1 89.11(4) . . ? C10 O3 C13 119.9(4) . . ? C1 N1 Pt1 133.8(3) . . ? C1 N1 H1 110.0 . . ? Pt1 N1 H1 115.1 . . ? C1 N3 C4 124.2(3) . . ? C1 N3 H3 123.2 . . ? C4 N3 H3 111.8 . . ? O2 N4 O1 124.1(4) . . ? O2 N4 C6 118.2(4) . . ? O1 N4 C6 117.8(3) . . ? C10 N2 Pt1 136.4(3) . . ? C10 N2 H2 115.7 . . ? Pt1 N2 H2 107.5 . . ? N1 C1 N3 121.6(4) . . ? N1 C1 C2 119.7(4) . . ? N3 C1 C2 118.5(4) . . ? C1 C2 C3 111.3(3) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 120.6(4) . . ? C9 C4 N3 120.1(4) . . ? C5 C4 N3 119.3(4) . . ? C6 C5 C4 117.2(4) . . ? C6 C5 H5 121.4 . . ? C4 C5 H5 121.4 . . ? C7 C6 C5 123.7(4) . . ? C7 C6 N4 118.5(4) . . ? C5 C6 N4 117.8(4) . . ? C8 C7 C6 117.8(4) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C7 C8 C9 120.3(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C4 C9 C8 120.4(4) . . ? C4 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N2 C10 O3 121.8(4) . . ? N2 C10 C11 125.6(4) . . ? O3 C10 C11 112.6(4) . . ? C10 C11 C12 112.3(4) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 Cl1 0.83 2.49 3.180(4) 142.1 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.61 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.462 _refine_diff_density_min -3.104 _refine_diff_density_rms 0.248