#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/47/2004778.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_2004778 loop_ _publ_author_name 'Sakai, K.' 'Ishikura, A.' 'Tsubomura, T.' 'Matsumoto, K.' _publ_section_title ; Two Different Crystal Forms of cis-diamminebis(pyrazole)platinum(II) Nitrate ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 779 _journal_page_last 783 _journal_paper_doi 10.1107/S0108270195013461 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Pt1 (N H3)2 (C3 H4 N2)2](N1 O3)2' _chemical_formula_moiety 'C6 H14 N6 Pt1, (N O3)2' _chemical_formula_structural '(Pt (N H3)2 (C3 H4 N2)2) (N O3)2' _chemical_formula_sum 'C6 H14 N8 O6 Pt' _chemical_formula_weight 489.32 _chemical_name_systematic ; cis-Diammine-bis(pyrazole)platinum(II) nitrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method 'teXsan (modified by Ken Sakai)' _cell_angle_alpha 90 _cell_angle_beta 90.530(10) _cell_angle_gamma 90 _cell_formula_units_Z 4.00 _cell_length_a 8.9430(10) _cell_length_b 9.222(2) _cell_length_c 17.184(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296.0 _cell_measurement_theta_max 29.89 _cell_measurement_theta_min 25.16 _cell_volume 1417.1(4) _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' _computing_structure_refinement 'teXsan: LS (MSC)' _computing_structure_solution 'SAPI91 (Fan, 1991)' _diffrn_ambient_temperature 296 _diffrn_measurement_device 'Rigaku AFC-5S' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 3675 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.2 _diffrn_standards_decay_% 0.73 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 9.944 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_type 'empirical via \y scan' _exptl_absorpt_process_details psi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.2934 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 928.00 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.81 _refine_diff_density_min -1.61 _refine_ls_extinction_coef 2.96793 _refine_ls_extinction_method 'Zachariasen type II, Gaussian isotropic' _refine_ls_goodness_of_fit_obs 3.18 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 191 _refine_ls_number_reflns 2458 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0391 _refine_ls_shift/esd_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'sigma; w = 1/\s^2^(F)' _refine_ls_wR_factor_obs 0.0377 _reflns_number_observed 2458 _reflns_number_total 3461 _reflns_observed_criterion I_>_3.0_sigma(I) _[local]_cod_data_source_file kh1060.cif _[local]_cod_data_source_block ptpz1 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _[local]_cod_chemical_formula_sum_orig 'C6 H14 N8 O6 Pt1' _cod_database_code 2004778 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt 0.0231(2) 0.0283(2) 0.0256(2) 0.0013(3) 0.0011(2) -0.0019(3) O(1) 0.036(6) 0.084(8) 0.057(7) -0.032(5) -0.016(5) 0.030(6) O(2) 0.037(6) 0.073(7) 0.043(6) 0.002(5) -0.013(5) 0.017(5) O(3) 0.056(7) 0.053(7) 0.075(8) -0.001(6) 0.006(6) 0.004(6) O(4) 0.037(6) 0.072(7) 0.059(7) -0.024(5) -0.005(5) 0.008(6) O(5) 0.045(6) 0.058(7) 0.073(8) 0.004(5) -0.007(6) -0.009(6) O(6) 0.071(7) 0.027(6) 0.079(8) 0.001(5) -0.016(6) 0.011(5) N(1) 0.021(6) 0.051(8) 0.039(7) -0.003(5) 0.000(5) -0.004(5) N(2) 0.041(7) 0.031(6) 0.058(8) 0.001(5) 0.020(6) -0.013(6) N(3) 0.032(6) 0.024(6) 0.029(6) -0.001(5) 0.009(5) -0.007(5) N(4) 0.041(6) 0.028(6) 0.038(6) 0.010(6) 0.000(5) 0.003(6) N(5) 0.020(5) 0.045(7) 0.019(5) 0.006(5) -0.005(4) -0.002(5) N(6) 0.028(6) 0.081(9) 0.014(5) 0.003(6) -0.004(4) -0.004(5) N(7) 0.040(8) 0.046(8) 0.034(7) -0.001(7) 0.014(6) 0.009(6) N(8) 0.045(7) 0.053(8) 0.028(6) 0.006(8) 0.002(5) -0.003(7) C(1) 0.050(10) 0.033(8) 0.060(10) -0.015(7) -0.008(8) -0.003(7) C(2) 0.041(8) 0.048(8) 0.042(8) -0.014(9) 0.001(6) -0.008(9) C(3) 0.021(7) 0.044(8) 0.047(9) 0.010(6) -0.001(6) -0.002(7) C(4) 0.039(8) 0.070(10) 0.018(7) -0.001(7) 0.007(6) -0.001(7) C(5) 0.052(9) 0.046(9) 0.018(7) -0.004(7) 0.004(6) -0.007(6) C(6) 0.046(8) 0.043(9) 0.021(6) 0.006(7) -0.012(6) -0.004(6) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt .56356(5) .39010(5) .65321(3) .02570(10) Uani d . O(1) .9386(10) .2570(10) .7088(5) .059(3) Uani d . O(2) 1.1457(9) .2590(10) .7742(5) .051(3) Uani d . O(3) 1.0680(10) .4560(10) .7204(6) .061(4) Uani d . O(4) .6285(10) .3070(10) .8794(5) .056(3) Uani d . O(5) .8640(10) .3180(10) .9009(5) .059(3) Uani d . O(6) .7430(10) .5130(10) .8743(6) .059(3) Uani d . N(1) .4370(10) .4300(10) .7506(6) .037(3) Uani d . N(2) .7100(10) .5440(10) .6907(6) .043(3) Uani d . N(3) .4170(10) .2383(10) .6142(5) .028(3) Uani d . N(4) .4550(10) .1010(10) .6032(5) .036(3) Uani d . N(5) .6896(9) .3580(10) .5580(5) .028(3) Uani d . N(6) .8370(10) .3340(10) .5601(5) .041(3) Uani d . N(7) 1.0500(10) .3260(10) .7354(7) .040(4) Uani d . N(8) .7450(10) .3820(10) .8846(5) .042(3) Uani d . C(1) .335(2) .0210(10) .5806(8) .047(5) Uani d . C(2) .2160(10) .111(2) .5771(7) .044(4) Uani d . C(3) .2700(10) .2450(10) .5954(7) .037(4) Uani d . C(4) .8980(10) .327(2) .4916(7) .043(4) Uani d . C(5) .7860(10) .3470(10) .4397(7) .039(4) Uani d . C(6) .6580(10) .3650(10) .4838(6) .037(4) Uani d . H(1) .3673 .3640 .7541 .0377 Uiso calc N(1) H(2) .3960 .5149 .7468 .0377 Uiso calc N(1) H(3) .4939 .4264 .7918 .0197 Uiso calc N(1) H(4) .6680 .5972 .7261 .0441 Uiso calc N(2) H(5) .7891 .5023 .7104 .0441 Uiso calc N(2) H(6) .7360 .5984 .6517 .0197 Uiso calc N(2) H(7) .5446 .0666 .6097 .0404 Uiso calc N(4) H(8) .3351 -0.0796 .5693 .0545 Uiso calc C(1) H(9) .1157 .0856 .5644 .0532 Uiso calc C(2) H(10) .2120 .3310 .5950 .0435 Uiso calc C(3) H(11) .8876 .3237 .6033 .0414 Uiso calc N(6) H(12) 1.0008 .3117 .4804 .0492 Uiso calc C(4) H(13) .7925 .3494 .3846 .0433 Uiso calc C(5) H(14) .5603 .3798 .4629 .0440 Uiso calc C(6) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables for X-ray Crystallography (1974, Vol. IV)' H 0.000 0.000 'International Tables for X-ray Crystallography (1974, Vol. IV)' N 0.006 0.003 'International Tables for X-ray Crystallography (1974, Vol. IV)' Pt -1.703 8.390 'International Tables for X-ray Crystallography (1974, Vol. IV)' O 0.011 0.006 'International Tables for X-ray Crystallography (1974, Vol. IV)' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 -1 -2 -1 1 -1 -1 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N(1) Pt N(2) 88.7(4) yes N(1) Pt N(3) 91.8(4) yes N(1) Pt N(5) 178.3(4) yes N(2) Pt N(3) 179.1(4) yes N(2) Pt N(5) 89.9(4) yes N(3) Pt N(5) 89.7(3) yes N(4) N(3) C(3) 104.9(9) yes N(3) N(4) C(1) 110.0(10) yes N(6) N(5) C(6) 104.0(9) yes N(5) N(6) C(4) 113.8(9) yes N(4) C(1) C(2) 107.0(10) yes C(1) C(2) C(3) 105.0(10) yes N(3) C(3) C(2) 110.0(10) yes N(6) C(4) C(5) 105.0(10) yes C(4) C(5) C(6) 105.0(10) yes N(5) C(6) C(5) 110.0(10) yes Pt N(3) N(4) 122.7(8) no Pt N(3) C(3) 132.4(8) no Pt N(5) N(6) 124.1(7) no Pt N(5) C(6) 131.8(8) no O(1) N(7) O(2) 119.0(10) no O(1) N(7) O(3) 120.0(10) no O(2) N(7) O(3) 120.0(10) no O(4) N(8) O(5) 117.0(10) no O(4) N(8) O(6) 122.0(10) no O(5) N(8) O(6) 120.0(10) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Pt N(1) 2.061(9) yes Pt N(2) 2.033(10) yes Pt N(3) 2.029(9) yes Pt N(5) 2.018(9) yes N(3) N(4) 1.330(10) yes N(3) C(3) 1.350(10) yes N(4) C(1) 1.350(10) yes N(5) N(6) 1.340(10) yes N(5) C(6) 1.310(10) yes N(6) C(4) 1.300(10) yes C(1) C(2) 1.35(2) yes C(2) C(3) 1.36(2) yes C(4) C(5) 1.35(2) yes C(5) C(6) 1.39(2) yes O(1) N(7) 1.260(10) no O(2) N(7) 1.240(10) no O(3) N(7) 1.240(10) no O(4) N(8) 1.250(10) no O(5) N(8) 1.250(10) no O(6) N(8) 1.220(10) no N(1) H(1) 0.8700 no N(1) H(2) 0.8700 no N(1) H(3) 0.8700 no N(2) H(4) 0.8700 no N(2) H(5) 0.8700 no N(2) H(6) 0.8700 no N(4) H(7) 0.8700 no N(6) H(11) 0.8700 no C(1) H(8) 0.9500 no C(2) H(9) 0.9500 no C(3) H(10) 0.9500 no C(4) H(12) 0.9500 no C(5) H(13) 0.9500 no C(6) H(14) 0.9500 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) N(6) 2.790(10) . yes O(1) N(2) 2.940(10) 2_646 yes O(2) N(1) 3.070(10) 1_655 yes O(4) N(1) 3.010(10) . yes O(4) N(2) 3.070(10) 2_646 yes O(5) N(2) 3.050(10) 2_646 yes O(5) N(4) 3.070(10) 2_656 yes O(6) N(4) 2.840(10) 2_656 yes O(1) N(1) 3.290(10) 2_646 no O(1) N(2) 3.360(10) . no O(2) N(1) 3.160(10) 2_646 no O(3) N(4) 3.320(10) 2_656 no O(3) N(2) 3.330(10) . no O(3) N(1) 3.350(10) 1_655 no O(6) N(2) 3.180(10) . no O(6) N(6) 3.250(10) 2_656 no