Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Vadim Kukushkin' 'Dmitrii A. Garnovskii' 'Matti Haukka' 'Armando J. L. Pombeiro' 'Piotr Sobota' _publ_contact_author_name 'ProfD Vadim Kukushkin' _publ_contact_author_address ; Department of Chemistry St.Petersburg State University St. Petersburg 198904 RUSSIAN FEDERATION ; _publ_contact_author_email KUKUSHKIN@VK2100.SPB.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Regioselective HON-Addition of Bifunctional Hydrazone Oximes to Pt(IV)-Bound Nitriles ; data_structure_3 _database_code_depnum_ccdc_archive 'CCDC 231143' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-[PtCl4{NHC(Et)ONC(Me)C(Ph)NNH2}2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 Cl4 N8 O2 Pt' _chemical_formula_weight 801.47 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.40350(10) _cell_length_b 9.54080(10) _cell_length_c 10.0344(2) _cell_angle_alpha 67.3988(6) _cell_angle_beta 68.9532(6) _cell_angle_gamma 82.5980(10) _cell_volume 775.628(19) _cell_formula_units_Z 1 _cell_measurement_temperature 150(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 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 394 _exptl_absorpt_coefficient_mu 4.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.24824 _exptl_absorpt_correction_T_max 0.30984 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method phi/omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11281 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 27.10 _reflns_number_total 3345 _reflns_number_gt 3345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material SHELXL-97 _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. NH2 and NH hydrogens were located from the difference Fourien map and refined isotropically. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0000P)^2^+0.2985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3345 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0173 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0401 _refine_ls_wR_factor_gt 0.0401 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 C1 C 0.2295(2) -0.1697(2) -0.1865(2) 0.0158(4) Uani 1 1 d . . . C2 C 0.2416(3) -0.3112(2) -0.0580(3) 0.0193(5) Uani 1 1 d . . . H2A H 0.1616 -0.3112 0.0384 0.023 Uiso 1 1 calc R . . H2B H 0.3418 -0.3117 -0.0461 0.023 Uiso 1 1 calc R . . C3 C 0.2252(3) -0.4546(3) -0.0835(3) 0.0292(6) Uani 1 1 d . . . H3A H 0.1299 -0.4510 -0.1035 0.044 Uiso 1 1 calc R . . H3B H 0.2236 -0.5435 0.0082 0.044 Uiso 1 1 calc R . . H3C H 0.3114 -0.4616 -0.1716 0.044 Uiso 1 1 calc R . . C4 C 0.3788(2) -0.0602(2) -0.5779(2) 0.0175(4) Uani 1 1 d . . . C5 C 0.4732(3) -0.1954(3) -0.5948(3) 0.0287(6) Uani 1 1 d . . . H5A H 0.5162 -0.2386 -0.5119 0.043 Uiso 1 1 calc R . . H5B H 0.5560 -0.1642 -0.6939 0.043 Uiso 1 1 calc R . . H5C H 0.4091 -0.2719 -0.5896 0.043 Uiso 1 1 calc R . . C6 C 0.3654(2) 0.0673(2) -0.7138(2) 0.0175(4) Uani 1 1 d . . . C7 C 0.2632(3) 0.1968(3) -0.6947(2) 0.0181(4) Uani 1 1 d . . . C8 C 0.1066(3) 0.1845(3) -0.6581(3) 0.0265(5) Uani 1 1 d . . . H8 H 0.0639 0.0934 -0.6456 0.032 Uiso 1 1 calc R . . C9 C 0.0128(3) 0.3057(3) -0.6399(3) 0.0311(6) Uani 1 1 d . . . H9 H -0.0940 0.2966 -0.6143 0.037 Uiso 1 1 calc R . . C10 C 0.0734(3) 0.4396(3) -0.6587(3) 0.0309(6) Uani 1 1 d . . . H10 H 0.0087 0.5223 -0.6471 0.037 Uiso 1 1 calc R . . C11 C 0.2286(3) 0.4521(3) -0.6945(3) 0.0302(6) Uani 1 1 d . . . H11 H 0.2706 0.5433 -0.7065 0.036 Uiso 1 1 calc R . . C12 C 0.3234(3) 0.3316(3) -0.7129(3) 0.0258(5) Uani 1 1 d . . . H12 H 0.4301 0.3412 -0.7382 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.14370(6) -0.10161(6) 0.16104(6) 0.02119(12) Uani 1 1 d . . . Cl2 Cl 0.13406(6) 0.22723(6) -0.10871(6) 0.02142(12) Uani 1 1 d . . . N1 N 0.1492(2) -0.0539(2) -0.1765(2) 0.0173(4) Uani 1 1 d . . . N2 N 0.3018(2) -0.0436(2) -0.4505(2) 0.0184(4) Uani 1 1 d . . . N3 N 0.4453(2) 0.0555(2) -0.8444(2) 0.0196(4) Uani 1 1 d . . . N4 N 0.4379(3) 0.1689(2) -0.9750(2) 0.0247(4) Uani 1 1 d . . . O1 O 0.31738(18) -0.17626(17) -0.32391(17) 0.0197(3) Uani 1 1 d . . . Pt1 Pt 0.0000 0.0000 0.0000 0.01388(5) Uani 1 2 d S . . H1 H 0.151(3) 0.009(3) -0.257(3) 0.018(7) Uiso 1 1 d . . . H42 H 0.475(3) 0.137(3) -1.056(3) 0.026(7) Uiso 1 1 d . . . H41 H 0.354(3) 0.217(3) -0.966(3) 0.029(8) Uiso 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 C1 0.0165(11) 0.0176(11) 0.0148(10) -0.0088(9) -0.0039(9) 0.0004(8) C2 0.0235(12) 0.0150(11) 0.0169(11) -0.0054(9) -0.0051(9) 0.0024(8) C3 0.0444(16) 0.0165(12) 0.0243(12) -0.0053(10) -0.0107(11) -0.0010(10) C4 0.0170(11) 0.0200(11) 0.0178(11) -0.0093(9) -0.0060(9) 0.0010(8) C5 0.0365(15) 0.0260(13) 0.0187(12) -0.0097(10) -0.0058(11) 0.0103(10) C6 0.0177(11) 0.0204(11) 0.0162(10) -0.0085(9) -0.0061(9) 0.0015(8) C7 0.0241(12) 0.0197(11) 0.0110(10) -0.0062(9) -0.0071(9) 0.0040(9) C8 0.0250(13) 0.0265(13) 0.0287(13) -0.0126(11) -0.0078(11) 0.0023(10) C9 0.0247(13) 0.0368(15) 0.0319(14) -0.0150(12) -0.0099(11) 0.0085(11) C10 0.0401(16) 0.0294(14) 0.0244(13) -0.0140(11) -0.0143(12) 0.0192(11) C11 0.0442(16) 0.0212(13) 0.0304(13) -0.0131(11) -0.0160(12) 0.0048(11) C12 0.0249(13) 0.0271(13) 0.0269(13) -0.0116(11) -0.0096(10) 0.0031(10) Cl1 0.0257(3) 0.0212(3) 0.0216(3) -0.0104(2) -0.0127(2) 0.0063(2) Cl2 0.0230(3) 0.0142(3) 0.0246(3) -0.0061(2) -0.0054(2) -0.0028(2) N1 0.0211(10) 0.0155(9) 0.0142(9) -0.0044(8) -0.0061(8) 0.0010(7) N2 0.0214(10) 0.0165(9) 0.0152(9) -0.0035(8) -0.0071(8) 0.0028(7) N3 0.0226(10) 0.0204(10) 0.0159(9) -0.0067(8) -0.0071(8) 0.0016(7) N4 0.0308(13) 0.0276(11) 0.0141(10) -0.0088(9) -0.0073(9) 0.0081(9) O1 0.0251(9) 0.0160(8) 0.0137(7) -0.0045(6) -0.0048(6) 0.0066(6) Pt1 0.01631(7) 0.01239(7) 0.01252(7) -0.00601(5) -0.00322(5) 0.00130(4) _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 C1 N1 1.271(3) . ? C1 O1 1.350(3) . ? C1 C2 1.492(3) . ? C2 C3 1.521(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N2 1.283(3) . ? C4 C6 1.471(3) . ? C4 C5 1.498(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N3 1.295(3) . ? C6 C7 1.494(3) . ? C7 C12 1.393(3) . ? C7 C8 1.393(3) . ? C8 C9 1.390(4) . ? C8 H8 0.9500 . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 C11 1.382(4) . ? C10 H10 0.9500 . ? C11 C12 1.390(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? Cl1 Pt1 2.3246(5) . ? Cl2 Pt1 2.3191(5) . ? N1 Pt1 2.0242(19) . ? N1 H1 0.79(3) . ? N2 O1 1.444(2) . ? N3 N4 1.360(3) . ? N4 H42 0.91(3) . ? N4 H41 0.86(3) . ? Pt1 N1 2.0242(19) 2 ? Pt1 Cl2 2.3191(5) 2 ? Pt1 Cl1 2.3246(5) 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 N1 C1 O1 121.32(19) . . ? N1 C1 C2 127.4(2) . . ? O1 C1 C2 111.32(18) . . ? C1 C2 C3 112.81(19) . . ? 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 . . ? N2 C4 C6 113.9(2) . . ? N2 C4 C5 125.6(2) . . ? C6 C4 C5 120.52(19) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C4 115.3(2) . . ? N3 C6 C7 124.79(19) . . ? C4 C6 C7 119.95(19) . . ? C12 C7 C8 119.1(2) . . ? C12 C7 C6 120.3(2) . . ? C8 C7 C6 120.6(2) . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.7(2) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 119.6(2) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.5(2) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C1 N1 Pt1 134.26(16) . . ? C1 N1 H1 114.3(19) . . ? Pt1 N1 H1 111.2(19) . . ? C4 N2 O1 109.88(17) . . ? C6 N3 N4 118.5(2) . . ? N3 N4 H42 110.6(17) . . ? N3 N4 H41 115.4(19) . . ? H42 N4 H41 116(3) . . ? C1 O1 N2 112.35(16) . . ? N1 Pt1 N1 180.00(17) 2 . ? N1 Pt1 Cl2 93.46(6) 2 . ? N1 Pt1 Cl2 86.54(6) . . ? N1 Pt1 Cl2 86.54(6) 2 2 ? N1 Pt1 Cl2 93.46(6) . 2 ? Cl2 Pt1 Cl2 180.000(16) . 2 ? N1 Pt1 Cl1 95.33(6) 2 2 ? N1 Pt1 Cl1 84.67(6) . 2 ? Cl2 Pt1 Cl1 90.148(19) . 2 ? Cl2 Pt1 Cl1 89.852(19) 2 2 ? N1 Pt1 Cl1 84.67(6) 2 . ? N1 Pt1 Cl1 95.33(6) . . ? Cl2 Pt1 Cl1 89.852(19) . . ? Cl2 Pt1 Cl1 90.148(19) 2 . ? Cl1 Pt1 Cl1 180.00(4) 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 N1 C1 C2 C3 132.2(2) . . . . ? O1 C1 C2 C3 -47.7(3) . . . . ? N2 C4 C6 N3 178.2(2) . . . . ? C5 C4 C6 N3 -3.1(3) . . . . ? N2 C4 C6 C7 -2.6(3) . . . . ? C5 C4 C6 C7 176.1(2) . . . . ? N3 C6 C7 C12 -80.9(3) . . . . ? C4 C6 C7 C12 99.9(3) . . . . ? N3 C6 C7 C8 99.3(3) . . . . ? C4 C6 C7 C8 -79.8(3) . . . . ? C12 C7 C8 C9 -0.2(3) . . . . ? C6 C7 C8 C9 179.6(2) . . . . ? C7 C8 C9 C10 0.4(4) . . . . ? C8 C9 C10 C11 -0.6(4) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C10 C11 C12 C7 -0.4(4) . . . . ? C8 C7 C12 C11 0.2(3) . . . . ? C6 C7 C12 C11 -179.6(2) . . . . ? O1 C1 N1 Pt1 177.60(15) . . . . ? C2 C1 N1 Pt1 -2.3(4) . . . . ? C6 C4 N2 O1 177.84(17) . . . . ? C5 C4 N2 O1 -0.8(3) . . . . ? C4 C6 N3 N4 179.69(19) . . . . ? C7 C6 N3 N4 0.5(3) . . . . ? N1 C1 O1 N2 -2.7(3) . . . . ? C2 C1 O1 N2 177.17(17) . . . . ? C4 N2 O1 C1 -175.40(18) . . . . ? C1 N1 Pt1 N1 -44(83) . . . 2 ? C1 N1 Pt1 Cl2 131.2(2) . . . . ? C1 N1 Pt1 Cl2 -48.8(2) . . . 2 ? C1 N1 Pt1 Cl1 -138.3(2) . . . 2 ? C1 N1 Pt1 Cl1 41.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.534 _refine_diff_density_min -1.321 _refine_diff_density_rms 0.095 #===END======================================================================== data_structure_4 _database_code_depnum_ccdc_archive 'CCDC 231144' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-[PtCl2{NHC(Et)ONC(Me)C(ph)CCH2}2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 Cl2 N8 O2 Pt' _chemical_formula_weight 730.57 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0753(2) _cell_length_b 8.6907(3) _cell_length_c 10.6485(4) _cell_angle_alpha 97.9160(10) _cell_angle_beta 104.1450(10) _cell_angle_gamma 98.463(2) _cell_volume 704.913(40) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13568 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.022 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 5.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.19314 _exptl_absorpt_correction_T_max 0.26538 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally 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 CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10837 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.01 _reflns_number_total 2761 _reflns_number_gt 2697 _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-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material SHELXL-97 _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. NH and NH2 hydrogens were located from the difference Fourien map and refined isotropically. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0180P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2761 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.5000 0.5000 0.0000 0.02948(8) Uani 1 2 d S . . Cl1 Cl 0.25928(11) 0.31998(11) 0.00027(9) 0.0397(2) Uani 1 1 d . . . N1 N 0.3444(4) 0.6299(3) -0.0995(3) 0.0309(7) Uani 1 1 d . . . N2 N 0.1568(3) 0.7750(3) -0.2648(3) 0.0269(6) Uani 1 1 d . . . N3 N -0.1429(4) 0.8084(4) -0.5460(3) 0.0375(7) Uani 1 1 d . . . N4 N -0.1877(5) 0.7619(6) -0.6786(3) 0.0582(11) Uani 1 1 d . . . O1 O 0.1651(3) 0.8142(3) -0.1271(2) 0.0290(5) Uani 1 1 d . . . C1 C 0.2673(4) 0.7323(4) -0.0531(3) 0.0261(7) Uani 1 1 d . . . C2 C 0.2808(5) 0.7802(4) 0.0890(3) 0.0335(8) Uani 1 1 d . . . H2A H 0.3174 0.6956 0.1368 0.040 Uiso 1 1 calc R . . H2B H 0.1655 0.7946 0.1000 0.040 Uiso 1 1 calc R . . C3 C 0.4121(5) 0.9341(5) 0.1475(4) 0.0419(9) Uani 1 1 d . . . H3A H 0.5261 0.9200 0.1362 0.063 Uiso 1 1 calc R . . H3B H 0.4209 0.9623 0.2416 0.063 Uiso 1 1 calc R . . H3C H 0.3736 1.0188 0.1024 0.063 Uiso 1 1 calc R . . C4 C 0.0332(4) 0.8304(4) -0.3324(3) 0.0276(7) Uani 1 1 d . . . C5 C -0.0842(5) 0.9213(5) -0.2757(4) 0.0389(9) Uani 1 1 d . . . H5A H -0.1639 0.8491 -0.2446 0.058 Uiso 1 1 calc R . . H5B H -0.1512 0.9703 -0.3437 0.058 Uiso 1 1 calc R . . H5C H -0.0140 1.0037 -0.2019 0.058 Uiso 1 1 calc R . . C6 C 0.0057(4) 0.7898(4) -0.4762(3) 0.0278(7) Uani 1 1 d . . . C7 C 0.1423(4) 0.7267(4) -0.5283(3) 0.0278(7) Uani 1 1 d . . . C8 C 0.1039(5) 0.5832(4) -0.6152(4) 0.0389(9) Uani 1 1 d . . . H8 H -0.0117 0.5245 -0.6430 0.047 Uiso 1 1 calc R . . C9 C 0.2328(6) 0.5250(5) -0.6615(4) 0.0495(11) Uani 1 1 d . . . H9 H 0.2048 0.4275 -0.7216 0.059 Uiso 1 1 calc R . . C10 C 0.4009(6) 0.6078(5) -0.6207(4) 0.0466(10) Uani 1 1 d . . . H10 H 0.4894 0.5666 -0.6513 0.056 Uiso 1 1 calc R . . C11 C 0.4413(5) 0.7517(5) -0.5349(4) 0.0414(9) Uani 1 1 d . . . H11 H 0.5571 0.8099 -0.5072 0.050 Uiso 1 1 calc R . . C12 C 0.3122(4) 0.8096(4) -0.4901(3) 0.0351(8) Uani 1 1 d . . . H12 H 0.3402 0.9084 -0.4318 0.042 Uiso 1 1 calc R . . H1 H 0.320(5) 0.617(4) -0.188(4) 0.038(10) Uiso 1 1 d . . . H4A H -0.097(6) 0.746(6) -0.718(5) 0.069(15) Uiso 1 1 d . . . H4B H -0.286(6) 0.797(6) -0.725(5) 0.067(14) Uiso 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 0.03457(12) 0.03517(12) 0.01943(11) 0.00326(8) 0.00292(7) 0.01779(8) Cl1 0.0391(5) 0.0450(5) 0.0345(5) 0.0073(4) 0.0061(4) 0.0124(4) N1 0.0342(16) 0.0383(17) 0.0198(15) 0.0016(13) 0.0032(12) 0.0155(13) N2 0.0328(15) 0.0311(15) 0.0171(13) 0.0031(11) 0.0045(11) 0.0121(12) N3 0.0331(16) 0.053(2) 0.0275(16) 0.0143(14) 0.0033(13) 0.0116(14) N4 0.040(2) 0.108(3) 0.0258(18) 0.0180(19) -0.0013(15) 0.022(2) O1 0.0357(12) 0.0344(13) 0.0199(12) 0.0056(10) 0.0058(10) 0.0181(10) C1 0.0258(16) 0.0293(17) 0.0237(17) 0.0075(14) 0.0044(13) 0.0081(14) C2 0.043(2) 0.038(2) 0.0248(18) 0.0092(15) 0.0093(15) 0.0202(16) C3 0.046(2) 0.051(2) 0.0237(19) -0.0037(17) 0.0025(16) 0.0166(18) C4 0.0277(17) 0.0288(18) 0.0272(18) 0.0071(14) 0.0064(14) 0.0083(14) C5 0.042(2) 0.044(2) 0.039(2) 0.0117(17) 0.0137(17) 0.0252(18) C6 0.0286(17) 0.0303(18) 0.0256(18) 0.0099(14) 0.0038(14) 0.0102(14) C7 0.0325(18) 0.0312(18) 0.0209(17) 0.0088(14) 0.0054(14) 0.0091(15) C8 0.047(2) 0.034(2) 0.037(2) 0.0021(16) 0.0192(17) 0.0011(17) C9 0.079(3) 0.036(2) 0.045(2) 0.0056(18) 0.034(2) 0.015(2) C10 0.063(3) 0.054(3) 0.047(2) 0.026(2) 0.035(2) 0.034(2) C11 0.0317(19) 0.058(3) 0.039(2) 0.0161(19) 0.0096(17) 0.0152(18) C12 0.0340(19) 0.043(2) 0.0273(19) 0.0051(16) 0.0048(15) 0.0105(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.018(3) 2_665 ? Pt1 N1 2.018(3) . ? Pt1 Cl1 2.3098(9) 2_665 ? Pt1 Cl1 2.3098(9) . ? N1 C1 1.271(4) . ? N1 H1 0.90(4) . ? N2 C4 1.278(4) . ? N2 O1 1.442(3) . ? N3 C6 1.293(4) . ? N3 N4 1.355(4) . ? N4 H4A 0.94(5) . ? N4 H4B 0.94(5) . ? O1 C1 1.348(4) . ? C1 C2 1.486(5) . ? C2 C3 1.527(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.476(5) . ? C4 C5 1.502(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.489(5) . ? C7 C12 1.386(5) . ? C7 C8 1.392(5) . ? C8 C9 1.385(5) . ? C8 H8 0.9500 . ? C9 C10 1.374(6) . ? C9 H9 0.9500 . ? C10 C11 1.387(6) . ? C10 H10 0.9500 . ? C11 C12 1.378(5) . ? C11 H11 0.9500 . ? C12 H12 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 2_665 . ? N1 Pt1 Cl1 90.30(9) 2_665 2_665 ? N1 Pt1 Cl1 89.70(9) . 2_665 ? N1 Pt1 Cl1 89.70(9) 2_665 . ? N1 Pt1 Cl1 90.30(9) . . ? Cl1 Pt1 Cl1 180.00(4) 2_665 . ? C1 N1 Pt1 127.9(2) . . ? C1 N1 H1 112(2) . . ? Pt1 N1 H1 121(2) . . ? C4 N2 O1 109.2(2) . . ? C6 N3 N4 119.6(3) . . ? N3 N4 H4A 117(3) . . ? N3 N4 H4B 115(3) . . ? H4A N4 H4B 120(4) . . ? C1 O1 N2 112.1(2) . . ? N1 C1 O1 124.1(3) . . ? N1 C1 C2 124.8(3) . . ? O1 C1 C2 111.2(3) . . ? C1 C2 C3 110.8(3) . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? 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 . . ? N2 C4 C6 114.1(3) . . ? N2 C4 C5 124.8(3) . . ? C6 C4 C5 121.0(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C4 114.8(3) . . ? N3 C6 C7 125.9(3) . . ? C4 C6 C7 119.3(3) . . ? C12 C7 C8 118.2(3) . . ? C12 C7 C6 120.6(3) . . ? C8 C7 C6 121.2(3) . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 120.2(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 119.5(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 121.5(3) . . ? C11 C12 H12 119.3 . . ? C7 C12 H12 119.3 . . ? 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 N1 Pt1 N1 C1 79(80) 2_665 . . . ? Cl1 Pt1 N1 C1 -97.0(3) 2_665 . . . ? Cl1 Pt1 N1 C1 83.0(3) . . . . ? C4 N2 O1 C1 167.1(3) . . . . ? Pt1 N1 C1 O1 180.0(2) . . . . ? Pt1 N1 C1 C2 1.5(5) . . . . ? N2 O1 C1 N1 -1.4(4) . . . . ? N2 O1 C1 C2 177.3(2) . . . . ? N1 C1 C2 C3 98.8(4) . . . . ? O1 C1 C2 C3 -79.9(4) . . . . ? O1 N2 C4 C6 -176.7(2) . . . . ? O1 N2 C4 C5 -0.3(4) . . . . ? N4 N3 C6 C4 -174.4(3) . . . . ? N4 N3 C6 C7 3.1(6) . . . . ? N2 C4 C6 N3 163.0(3) . . . . ? C5 C4 C6 N3 -13.6(5) . . . . ? N2 C4 C6 C7 -14.7(5) . . . . ? C5 C4 C6 C7 168.7(3) . . . . ? N3 C6 C7 C12 128.0(4) . . . . ? C4 C6 C7 C12 -54.6(5) . . . . ? N3 C6 C7 C8 -52.6(5) . . . . ? C4 C6 C7 C8 124.8(4) . . . . ? C12 C7 C8 C9 0.2(6) . . . . ? C6 C7 C8 C9 -179.2(4) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? C8 C9 C10 C11 -1.2(6) . . . . ? C9 C10 C11 C12 0.6(6) . . . . ? C10 C11 C12 C7 0.4(6) . . . . ? C8 C7 C12 C11 -0.8(5) . . . . ? C6 C7 C12 C11 178.6(3) . . . . ? 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 N2 0.90(4) 2.14(4) 2.618(4) 112(3) . C5 H5B N3 0.98 2.43 2.809(5) 102.6 . C11 H11 N3 0.95 2.56 3.355(5) 141.8 1_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.469 _refine_diff_density_min -1.162 _refine_diff_density_rms 0.103 #===END====================================================== data_structure_5 _database_code_depnum_ccdc_archive 'CCDC 231145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-[PtCl2{NHC(Et)ONC(Me)C(Ph)NNCH(C6H3-2-OH-5-NO2}2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H38 Cl2 N10 O8 Pt' _chemical_formula_weight 1028.77 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7209(2) _cell_length_b 10.9317(2) _cell_length_c 11.9651(2) _cell_angle_alpha 109.4880(10) _cell_angle_beta 101.5020(10) _cell_angle_gamma 100.2610(10) _cell_volume 1016.11(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(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 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 3.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.31969 _exptl_absorpt_correction_T_max 0.37318 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 6.12 (Bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally 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 CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16718 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3974 _reflns_number_gt 3878 _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 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.6.12 (Bruker AXS, 2001)' _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. OH hydrogens was located from the difference Fourien map but not refined. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0181P)^2^+0.9555P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3974 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 1.0000 1.0000 1.0000 0.02264(8) Uani 1 2 d S . . Cl1 Cl 0.91517(12) 1.12819(10) 1.16033(8) 0.0331(2) Uani 1 1 d . . . O1 O 0.5128(3) 0.7522(3) 0.8262(2) 0.0271(6) Uani 1 1 d . . . O2 O 0.4023(3) 0.6095(3) 0.1284(2) 0.0372(7) Uani 1 1 d . . . O3 O -0.2030(4) 0.1288(3) -0.2053(3) 0.0420(7) Uani 1 1 d . . . O4 O -0.1162(4) 0.1871(3) -0.3419(2) 0.0443(8) Uani 1 1 d . . . N1 N 0.7738(4) 0.8931(3) 0.8956(3) 0.0257(7) Uani 1 1 d . . . H1 H 0.7540 0.8892 0.8193 0.031 Uiso 1 1 calc R . . N2 N 0.5237(4) 0.7486(3) 0.7081(3) 0.0282(7) Uani 1 1 d . . . N3 N 0.2744(4) 0.5702(3) 0.4114(3) 0.0309(7) Uani 1 1 d . . . N4 N 0.2848(4) 0.5531(3) 0.2919(3) 0.0301(7) Uani 1 1 d . . . N5 N -0.1075(4) 0.2005(3) -0.2347(3) 0.0310(7) Uani 1 1 d . . . C1 C 0.6543(4) 0.8304(4) 0.9174(3) 0.0231(8) Uani 1 1 d . . . C2 C 0.6391(5) 0.8251(4) 1.0382(3) 0.0258(8) Uani 1 1 d . . . H2A H 0.7453 0.8708 1.1011 0.031 Uiso 1 1 calc R . . H2B H 0.6105 0.7299 1.0295 0.031 Uiso 1 1 calc R . . C3 C 0.5108(5) 0.8917(4) 1.0828(3) 0.0324(9) Uani 1 1 d . . . H3A H 0.5514 0.9897 1.1116 0.049 Uiso 1 1 calc R . . H3B H 0.4873 0.8678 1.1508 0.049 Uiso 1 1 calc R . . H3C H 0.4113 0.8604 1.0147 0.049 Uiso 1 1 calc R . . C4 C 0.3922(5) 0.6734(4) 0.6251(3) 0.0262(8) Uani 1 1 d . . . C5 C 0.2448(5) 0.6037(4) 0.6479(4) 0.0391(10) Uani 1 1 d . . . H5A H 0.2635 0.5242 0.6630 0.059 Uiso 1 1 calc R . . H5B H 0.1516 0.5761 0.5754 0.059 Uiso 1 1 calc R . . H5C H 0.2227 0.6653 0.7200 0.059 Uiso 1 1 calc R . . C6 C 0.3982(5) 0.6586(4) 0.4980(3) 0.0264(8) Uani 1 1 d . . . C7 C 0.5389(5) 0.7394(4) 0.4782(3) 0.0278(8) Uani 1 1 d . . . C8 C 0.5161(5) 0.8340(4) 0.4256(3) 0.0319(9) Uani 1 1 d . . . H8 H 0.4116 0.8483 0.4051 0.038 Uiso 1 1 calc R . . C9 C 0.6450(5) 0.9064(4) 0.4035(3) 0.0363(10) Uani 1 1 d . . . H9 H 0.6288 0.9707 0.3682 0.044 Uiso 1 1 calc R . . C10 C 0.7960(6) 0.8864(5) 0.4319(4) 0.0428(11) Uani 1 1 d . . . H10 H 0.8834 0.9347 0.4139 0.051 Uiso 1 1 calc R . . C11 C 0.8217(5) 0.7953(4) 0.4872(4) 0.0391(10) Uani 1 1 d . . . H11 H 0.9270 0.7827 0.5083 0.047 Uiso 1 1 calc R . . C12 C 0.6946(5) 0.7234(4) 0.5113(4) 0.0328(9) Uani 1 1 d . . . H12 H 0.7130 0.6627 0.5506 0.039 Uiso 1 1 calc R . . C13 C 0.1679(5) 0.4600(4) 0.2067(3) 0.0270(8) Uani 1 1 d . . . H13 H 0.0866 0.4085 0.2274 0.032 Uiso 1 1 calc R . . C14 C 0.1604(4) 0.4337(3) 0.0781(3) 0.0228(7) Uani 1 1 d . . . C15 C 0.0335(4) 0.3312(4) -0.0152(3) 0.0255(8) Uani 1 1 d . . . H15 H -0.0466 0.2778 0.0050 0.031 Uiso 1 1 calc R . . C16 C 0.0260(4) 0.3086(4) -0.1373(3) 0.0265(8) Uani 1 1 d . . . C17 C 0.1381(5) 0.3839(4) -0.1703(3) 0.0287(8) Uani 1 1 d . . . H17 H 0.1296 0.3657 -0.2550 0.034 Uiso 1 1 calc R . . C18 C 0.2634(5) 0.4866(4) -0.0798(3) 0.0307(9) Uani 1 1 d . . . H18 H 0.3401 0.5405 -0.1022 0.037 Uiso 1 1 calc R . . C19 C 0.2773(5) 0.5113(4) 0.0447(3) 0.0283(8) Uani 1 1 d . . . H02 H 0.4029 0.6194 0.2132 0.050 Uiso 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 0.02196(12) 0.02503(12) 0.01835(11) 0.00727(8) 0.00452(8) 0.00325(8) Cl1 0.0314(5) 0.0319(5) 0.0278(5) 0.0020(4) 0.0118(4) 0.0026(4) O1 0.0260(14) 0.0336(15) 0.0159(12) 0.0076(11) 0.0038(10) -0.0001(11) O2 0.0386(16) 0.0349(16) 0.0233(13) 0.0056(12) 0.0039(12) -0.0097(13) O3 0.0367(17) 0.0428(18) 0.0341(15) 0.0109(14) 0.0038(13) -0.0048(14) O4 0.0384(17) 0.063(2) 0.0169(13) 0.0037(14) 0.0034(12) 0.0051(15) N1 0.0300(17) 0.0296(17) 0.0163(14) 0.0073(13) 0.0081(13) 0.0061(14) N2 0.0300(18) 0.0328(18) 0.0164(14) 0.0067(13) 0.0054(13) 0.0022(14) N3 0.0371(19) 0.0309(18) 0.0176(15) 0.0071(14) 0.0032(14) 0.0014(15) N4 0.0339(18) 0.0315(18) 0.0189(15) 0.0080(14) 0.0043(13) 0.0013(15) N5 0.0266(18) 0.0378(19) 0.0232(16) 0.0061(15) 0.0051(14) 0.0085(15) C1 0.0210(18) 0.0223(19) 0.0196(17) 0.0029(15) 0.0034(14) 0.0025(15) C2 0.028(2) 0.026(2) 0.0205(17) 0.0083(15) 0.0032(15) 0.0061(16) C3 0.033(2) 0.043(2) 0.0266(19) 0.0164(18) 0.0135(17) 0.0140(19) C4 0.030(2) 0.027(2) 0.0190(17) 0.0063(16) 0.0065(15) 0.0057(16) C5 0.037(2) 0.044(3) 0.0234(19) 0.0057(19) 0.0093(17) -0.007(2) C6 0.027(2) 0.0244(19) 0.0205(17) 0.0042(16) 0.0018(15) 0.0038(16) C7 0.030(2) 0.030(2) 0.0185(17) 0.0052(16) 0.0059(15) 0.0038(17) C8 0.033(2) 0.032(2) 0.0230(19) 0.0066(17) -0.0001(16) 0.0058(18) C9 0.042(3) 0.030(2) 0.026(2) 0.0081(18) 0.0041(18) -0.0038(19) C10 0.042(3) 0.041(3) 0.033(2) 0.005(2) 0.014(2) -0.005(2) C11 0.029(2) 0.049(3) 0.036(2) 0.012(2) 0.0104(18) 0.007(2) C12 0.036(2) 0.035(2) 0.029(2) 0.0120(18) 0.0099(17) 0.0125(18) C13 0.028(2) 0.027(2) 0.0233(18) 0.0091(16) 0.0038(16) 0.0058(16) C14 0.0261(19) 0.0211(18) 0.0206(17) 0.0080(15) 0.0045(15) 0.0070(15) C15 0.0218(19) 0.030(2) 0.0225(18) 0.0089(16) 0.0043(15) 0.0065(16) C16 0.026(2) 0.027(2) 0.0203(17) 0.0035(16) 0.0014(15) 0.0091(16) C17 0.035(2) 0.034(2) 0.0189(17) 0.0103(16) 0.0074(16) 0.0129(18) C18 0.032(2) 0.033(2) 0.0281(19) 0.0125(17) 0.0114(17) 0.0051(18) C19 0.030(2) 0.026(2) 0.0250(19) 0.0080(16) 0.0052(16) 0.0051(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.009(3) 2_777 ? Pt1 N1 2.009(3) . ? Pt1 Cl1 2.3092(9) . ? Pt1 Cl1 2.3092(9) 2_777 ? O1 C1 1.381(4) . ? O1 N2 1.423(4) . ? O2 C19 1.332(4) . ? O2 H02 0.9827 . ? O3 N5 1.225(4) . ? O4 N5 1.225(4) . ? N1 C1 1.264(5) . ? N1 H1 0.8800 . ? N2 C4 1.282(5) . ? N3 C6 1.299(5) . ? N3 N4 1.402(4) . ? N4 C13 1.280(5) . ? N5 C16 1.470(5) . ? C1 C2 1.497(5) . ? C2 C3 1.529(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.488(5) . ? C4 C5 1.495(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.487(5) . ? C7 C12 1.396(6) . ? C7 C8 1.401(5) . ? C8 C9 1.379(6) . ? C8 H8 0.9500 . ? C9 C10 1.368(6) . ? C9 H9 0.9500 . ? C10 C11 1.393(6) . ? C10 H10 0.9500 . ? C11 C12 1.377(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.453(5) . ? C13 H13 0.9500 . ? C14 C15 1.399(5) . ? C14 C19 1.414(5) . ? C15 C16 1.383(5) . ? C15 H15 0.9500 . ? C16 C17 1.369(5) . ? C17 C18 1.381(5) . ? C17 H17 0.9500 . ? C18 C19 1.399(5) . ? C18 H18 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 2_777 . ? N1 Pt1 Cl1 85.88(9) 2_777 . ? N1 Pt1 Cl1 94.12(9) . . ? N1 Pt1 Cl1 94.12(9) 2_777 2_777 ? N1 Pt1 Cl1 85.88(9) . 2_777 ? Cl1 Pt1 Cl1 180.0 . 2_777 ? C1 O1 N2 111.5(3) . . ? C19 O2 H02 112.2 . . ? C1 N1 Pt1 133.0(2) . . ? C1 N1 H1 113.5 . . ? Pt1 N1 H1 113.5 . . ? C4 N2 O1 110.1(3) . . ? C6 N3 N4 113.6(3) . . ? C13 N4 N3 113.5(3) . . ? O3 N5 O4 123.6(3) . . ? O3 N5 C16 118.8(3) . . ? O4 N5 C16 117.5(3) . . ? N1 C1 O1 122.6(3) . . ? N1 C1 C2 128.2(3) . . ? O1 C1 C2 109.2(3) . . ? C1 C2 C3 112.6(3) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? 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 . . ? N2 C4 C6 113.2(3) . . ? N2 C4 C5 125.6(3) . . ? C6 C4 C5 121.2(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 125.5(3) . . ? N3 C6 C4 114.1(3) . . ? C7 C6 C4 120.4(3) . . ? C12 C7 C8 118.9(4) . . ? C12 C7 C6 121.3(3) . . ? C8 C7 C6 119.8(3) . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 120.2(4) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? N4 C13 C14 119.6(3) . . ? N4 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C19 118.9(3) . . ? C15 C14 C13 119.7(3) . . ? C19 C14 C13 121.4(3) . . ? C16 C15 C14 119.2(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 122.2(3) . . ? C17 C16 N5 118.9(3) . . ? C15 C16 N5 118.8(3) . . ? C16 C17 C18 119.6(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? O2 C19 C18 117.7(3) . . ? O2 C19 C14 122.3(3) . . ? C18 C19 C14 120.0(3) . . ? 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 N1 Pt1 N1 C1 -161(100) 2_777 . . . ? Cl1 Pt1 N1 C1 -49.7(4) . . . . ? Cl1 Pt1 N1 C1 130.3(4) 2_777 . . . ? C1 O1 N2 C4 178.8(3) . . . . ? C6 N3 N4 C13 175.8(3) . . . . ? Pt1 N1 C1 O1 -173.7(2) . . . . ? Pt1 N1 C1 C2 5.7(6) . . . . ? N2 O1 C1 N1 2.2(5) . . . . ? N2 O1 C1 C2 -177.2(3) . . . . ? N1 C1 C2 C3 114.2(4) . . . . ? O1 C1 C2 C3 -66.4(4) . . . . ? O1 N2 C4 C6 -176.8(3) . . . . ? O1 N2 C4 C5 2.5(5) . . . . ? N4 N3 C6 C7 1.5(6) . . . . ? N4 N3 C6 C4 -177.4(3) . . . . ? N2 C4 C6 N3 172.0(3) . . . . ? C5 C4 C6 N3 -7.3(5) . . . . ? N2 C4 C6 C7 -6.9(5) . . . . ? C5 C4 C6 C7 173.8(4) . . . . ? N3 C6 C7 C12 -114.7(4) . . . . ? C4 C6 C7 C12 64.1(5) . . . . ? N3 C6 C7 C8 65.5(5) . . . . ? C4 C6 C7 C8 -115.7(4) . . . . ? C12 C7 C8 C9 2.1(5) . . . . ? C6 C7 C8 C9 -178.0(3) . . . . ? C7 C8 C9 C10 0.3(6) . . . . ? C8 C9 C10 C11 -2.0(6) . . . . ? C9 C10 C11 C12 1.2(6) . . . . ? C10 C11 C12 C7 1.3(6) . . . . ? C8 C7 C12 C11 -2.9(6) . . . . ? C6 C7 C12 C11 177.2(3) . . . . ? N3 N4 C13 C14 178.2(3) . . . . ? N4 C13 C14 C15 179.4(4) . . . . ? N4 C13 C14 C19 -1.8(6) . . . . ? C19 C14 C15 C16 0.1(5) . . . . ? C13 C14 C15 C16 178.9(3) . . . . ? C14 C15 C16 C17 -0.6(6) . . . . ? C14 C15 C16 N5 179.8(3) . . . . ? O3 N5 C16 C17 176.4(3) . . . . ? O4 N5 C16 C17 -3.3(5) . . . . ? O3 N5 C16 C15 -4.0(5) . . . . ? O4 N5 C16 C15 176.2(3) . . . . ? C15 C16 C17 C18 -0.1(6) . . . . ? N5 C16 C17 C18 179.4(3) . . . . ? C16 C17 C18 C19 1.4(6) . . . . ? C17 C18 C19 O2 178.6(4) . . . . ? C17 C18 C19 C14 -1.9(6) . . . . ? C15 C14 C19 O2 -179.3(4) . . . . ? C13 C14 C19 O2 1.9(6) . . . . ? C15 C14 C19 C18 1.1(6) . . . . ? C13 C14 C19 C18 -177.7(4) . . . . ? 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 O2 H02 N4 0.98 1.75 2.576(4) 139.8 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.614 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.108