#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/70/2207043.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2207043 loop_ _publ_author_name 'Khripun, Anatoly V.' 'Haukka, Matti' 'Nikolaeva, Dina N.' 'Kukushkin, Vadim Yu.' _publ_section_title ; fac-Trichloro(pyrazolato)bis(pyrazole)platinum(IV) ; _journal_coeditor_code OB6588 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m2069 _journal_page_last m2071 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Pt Cl3 (C3 H3 N2) (C3 H4 N2)2]' _chemical_formula_moiety 'C9 H11 Cl3 N6 Pt' _chemical_formula_sum 'C9 H11 Cl3 N6 Pt' _chemical_formula_weight 504.68 _chemical_name_systematic ; fac-Trichloro(pyrazolato)bis(pyrazole)platinum(IV) ; _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 94.888(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.8307(6) _cell_length_b 13.5005(7) _cell_length_c 7.6421(7) _cell_measurement_reflns_used 4975 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.43 _cell_measurement_theta_min 2.99 _cell_volume 702.18(10) _computing_cell_refinement 'DENZO and SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_data_reduction 'DENZO and SCALEPACK' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2005)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\f scans, and \w scans with \k offset' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 4975 _diffrn_reflns_theta_full 27.43 _diffrn_reflns_theta_max 27.43 _diffrn_reflns_theta_min 2.99 _exptl_absorpt_coefficient_mu 10.556 _exptl_absorpt_correction_T_max 0.6312 _exptl_absorpt_correction_T_min 0.1887 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(de Meulenaer & Tompa, 1965)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 472 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.821 _refine_diff_density_min -2.944 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 1645 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0307 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0542P)^2^+1.4982P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.0808 _reflns_number_gt 1522 _reflns_number_total 1645 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ob6588.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/m' _cod_database_code 2207043 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Pt1 0.31554(3) 0.2500 1.01373(3) 0.01119(12) Uani d S 1 Pt Cl1 0.49671(18) 0.12879(9) 0.89008(18) 0.0156(3) Uani d . 1 Cl Cl2 0.5399(3) 0.2500 1.2607(3) 0.0188(4) Uani d S 1 Cl N1 0.1595(6) 0.1404(3) 1.1278(6) 0.0123(8) Uani d . 1 N N2 -0.0356(6) 0.1266(3) 1.0947(6) 0.0150(9) Uani d . 1 N H2N -0.099(10) 0.155(5) 1.014(9) 0.016(16) Uiso d . 1 H N3 0.1260(8) 0.2500 0.7924(8) 0.0113(12) Uani d S 1 N N4 -0.0686(8) 0.2500 0.8079(8) 0.0127(12) Uani d S 1 N C1 -0.0928(8) 0.0486(4) 1.1857(7) 0.0178(11) Uani d . 1 C H1 -0.2229 0.0235 1.1843 0.021 Uiso calc R 1 H C2 0.0693(8) 0.0115(4) 1.2809(8) 0.0191(11) Uani d . 1 C H2 0.0742 -0.0439 1.3577 0.023 Uiso calc R 1 H C3 0.2252(8) 0.0713(4) 1.2424(7) 0.0178(11) Uani d . 1 C H3 0.3574 0.0642 1.2902 0.021 Uiso calc R 1 H C4 -0.1519(10) 0.2500 0.6438(10) 0.0147(14) Uani d S 1 C H4 -0.2897 0.2500 0.6134 0.018 Uiso calc SR 1 H C5 -0.0083(11) 0.2500 0.5202(10) 0.0165(15) Uani d S 1 C H5 -0.0271 0.2500 0.3956 0.020 Uiso calc SR 1 H C6 0.1685(11) 0.2500 0.6281(10) 0.0165(15) Uani d S 1 C H6 0.2968 0.2500 0.5890 0.020 Uiso calc SR 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt1 0.00831(17) 0.01220(18) 0.01306(18) 0.000 0.00093(11) 0.000 Cl1 0.0118(5) 0.0129(6) 0.0224(7) 0.0027(4) 0.0035(5) -0.0013(5) Cl2 0.0134(8) 0.0232(9) 0.0187(10) 0.000 -0.0040(7) 0.000 N1 0.0101(19) 0.012(2) 0.015(2) 0.0000(15) 0.0015(16) 0.0014(17) N2 0.014(2) 0.017(2) 0.014(2) -0.0010(17) 0.0010(18) 0.0014(18) N3 0.011(3) 0.009(3) 0.013(3) 0.000 -0.004(2) 0.000 N4 0.013(3) 0.017(3) 0.009(3) 0.000 0.004(2) 0.000 C1 0.022(3) 0.015(3) 0.018(3) -0.007(2) 0.010(2) -0.001(2) C2 0.028(3) 0.011(2) 0.020(3) 0.001(2) 0.009(2) -0.002(2) C3 0.019(2) 0.013(2) 0.021(3) 0.0032(19) 0.001(2) 0.002(2) C4 0.010(3) 0.014(3) 0.019(4) 0.000 0.001(3) 0.000 C5 0.021(4) 0.018(4) 0.011(4) 0.000 0.004(3) 0.000 C6 0.015(3) 0.023(4) 0.012(4) 0.000 0.005(3) 0.000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 N3 . 2.041(6) yes Pt1 N1 . 2.060(4) yes Pt1 N1 4_565 2.060(4) ? Pt1 Cl1 . 2.3026(12) yes Pt1 Cl1 4_565 2.3026(12) ? Pt1 Cl2 . 2.3274(19) yes N1 C3 . 1.331(7) ? N1 N2 . 1.348(6) ? N2 C1 . 1.339(7) ? N2 H2N . 0.81(7) ? N3 C6 . 1.312(10) ? N3 N4 . 1.344(8) ? N4 C4 . 1.333(10) ? C1 C2 . 1.367(8) ? C1 H1 . 0.9500 ? C2 C3 . 1.388(7) ? C2 H2 . 0.9500 ? C3 H3 . 0.9500 ? C4 C5 . 1.418(10) ? C4 H4 . 0.9500 ? C5 C6 . 1.403(11) ? 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N3 Pt1 N1 . . 92.07(18) yes N3 Pt1 N1 . 4_565 92.07(17) ? N1 Pt1 N1 . 4_565 91.8(2) yes N3 Pt1 Cl1 . . 89.14(13) yes N1 Pt1 Cl1 . . 88.78(13) yes N1 Pt1 Cl1 4_565 . 178.62(12) ? N3 Pt1 Cl1 . 4_565 89.14(13) ? N1 Pt1 Cl1 . 4_565 178.62(12) ? N1 Pt1 Cl1 4_565 4_565 88.77(13) ? Cl1 Pt1 Cl1 . 4_565 90.59(6) yes N3 Pt1 Cl2 . . 178.21(17) yes N1 Pt1 Cl2 . . 89.18(13) yes N1 Pt1 Cl2 4_565 . 89.18(13) ? Cl1 Pt1 Cl2 . . 89.60(5) yes Cl1 Pt1 Cl2 4_565 . 89.60(5) ? C3 N1 N2 . . 107.4(4) ? C3 N1 Pt1 . . 128.6(4) ? N2 N1 Pt1 . . 124.0(3) ? C1 N2 N1 . . 109.8(5) ? C1 N2 H2N . . 127(5) ? N1 N2 H2N . . 122(5) ? C6 N3 N4 . . 112.7(6) ? C6 N3 Pt1 . . 128.0(5) ? N4 N3 Pt1 . . 119.3(5) ? C4 N4 N3 . . 105.2(6) ? N2 C1 C2 . . 107.8(5) ? N2 C1 H1 . . 126.1 ? C2 C1 H1 . . 126.1 ? C1 C2 C3 . . 106.0(5) ? C1 C2 H2 . . 127.0 ? C3 C2 H2 . . 127.0 ? N1 C3 C2 . . 109.0(5) ? N1 C3 H3 . . 125.5 ? C2 C3 H3 . . 125.5 ? N4 C4 C5 . . 111.3(6) ? N4 C4 H4 . . 124.4 ? C5 C4 H4 . . 124.4 ? C6 C5 C4 . . 102.6(7) ? C6 C5 H5 . . 128.7 ? C4 C5 H5 . . 128.7 ? N3 C6 C5 . . 108.2(6) ? N3 C6 H6 . . 125.9 ? C5 C6 H6 . . 125.9 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N2 H2N N4 . 0.81(7) 2.06(7) 2.747(7) 142(6) yes N2 H2N N3 . 0.81(7) 2.71(7) 3.125(7) 114(5) no N2 H2N Cl1 1_455 0.81(7) 2.87(7) 3.435(5) 129(6) no _cod_database_fobs_code 2207043 _journal_paper_doi 10.1107/S1600536805029661