#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/20/2202099.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_2202099 loop_ _publ_author_name 'Matsushita, Nobuyuki' _publ_section_title ;A one-dimensional Cl-bridged Pt^II/IV^ mixed-valence complex, catena-poly[[bis(ethylenediamine)platinum(II)-\m-chloro-bis(ethylenediamine)platinum(IV)-\m-chloro] tetrakis(hydrogensulfate)] ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m26 _journal_page_last m28 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Pt2 Cl2 (C2 H8 N2)4] (H S O4)4' _chemical_formula_moiety 'C4 H16 N4 Pt 2+, C4 H16 Cl2 N4 Pt 2+, 4(H O4 S 1-)' _chemical_formula_sum 'C8 H36 Cl2 N8 O16 Pt2 S4' _chemical_formula_weight 1089.77 _chemical_name_systematic ;catena-Poly[bis(ethylenediamine)platinum(II,IV)-\m-chloro bis(hydrogensulfate)] ; _space_group_IT_number 72 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-I 2 2c' _symmetry_space_group_name_H-M 'I b a m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.2610(10) _cell_length_b 14.422(2) _cell_length_c 10.9290(10) _cell_measurement_reflns_used 50 _cell_measurement_temperature 295 _cell_measurement_theta_max 14.64 _cell_measurement_theta_min 10.01 _cell_volume 1459.7(3) _computing_cell_refinement 'AFC Diffractometer Control Software' _computing_data_collection 'AFC Diffractometer Control Software (Rigaku, 1987)' _computing_data_reduction 'a handmade program' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'UNICS3 (Sakurai & Kobayashi, 1979)' _diffrn_ambient_temperature 295 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku AFC-5S' _diffrn_measurement_method \q/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 0.0289 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 3059 _diffrn_reflns_theta_full 32.50 _diffrn_reflns_theta_max 32.50 _diffrn_reflns_theta_min 1.5 _diffrn_standards_decay_% none _diffrn_standards_interval_count 50 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 10.12 _exptl_absorpt_correction_T_max 0.7017 _exptl_absorpt_correction_T_min 0.1868 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details '(Coppens et al., 1965)' _exptl_crystal_colour 'intense red' _exptl_crystal_density_diffrn 2.48 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1044 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.506 _refine_diff_density_min -1.185 _refine_ls_extinction_coef 0.0054(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 68 _refine_ls_number_reflns 975 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0236 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0266P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.0479 _reflns_number_gt 975 _reflns_number_total 1387 _reflns_threshold_expression F>3\s(F) _[local]_cod_data_source_file ob6201.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. '_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2202099 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pt 0.0000 0.0000 0.2500 0.02543(10) Uani d S 1 . . Pt Cl 0.0000 0.0000 0.0375(2) 0.0377(5) Uani d SP .5 . . Cl S 0.38104(19) 0.21958(12) 0.0000 0.0435(3) Uani d S 1 . . S O1 0.5028(13) 0.2396(9) 0.0858(10) 0.073(3) Uani d P .5 . . O O2 0.3372(9) 0.1267(4) 0.0000 0.100(3) Uani d S 1 . . O O3 0.2708(9) 0.2814(6) 0.0389(13) 0.117(7) Uani d P .5 . . O O4 0.4300(15) 0.2442(8) -0.1248(9) 0.080(4) Uani d P .5 . . O N 0.1654(4) 0.0935(2) 0.2484(4) 0.0416(7) Uani d . 1 . . N C 0.3014(5) 0.0456(4) 0.2821(6) 0.0607(15) Uani d . 1 . . C H1O 0.5787 0.2419 0.0473 0.109 Uiso calc PR .5 . . H H1N 0.1740 0.1186 0.1733 0.062 Uiso calc R 1 . . H H2N 0.1472 0.1394 0.3020 0.062 Uiso calc R 1 . . H H1C 0.3060 0.0365 0.3700 0.091 Uiso calc R 1 . . H H2C 0.3841 0.0822 0.2571 0.091 Uiso calc R 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 Pt 0.02861(14) 0.02775(13) 0.01993(12) 0.000 0.000 0.000 Cl 0.0447(12) 0.0469(12) 0.0215(8) 0.0042(15) 0.000 0.000 S 0.0386(8) 0.0427(7) 0.0492(9) -0.0082(7) 0.000 0.000 O1 0.057(5) 0.090(7) 0.071(7) -0.010(7) -0.032(6) -0.019(6) O2 0.163(8) 0.052(3) 0.086(4) -0.056(4) 0.000 0.000 O3 0.041(4) 0.130(6) 0.18(2) 0.005(4) -0.007(6) -0.095(11) O4 0.135(14) 0.059(5) 0.048(5) 0.012(7) -0.001(6) 0.005(4) N 0.0401(16) 0.0415(15) 0.0431(17) -0.0098(13) 0.005(2) -0.003(2) C 0.034(2) 0.078(4) 0.070(4) -0.013(2) -0.006(2) 0.006(3) 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 Pt Cl . 2.323(2) yes Pt Cl 9 3.142(2) yes Cl Cl 9 0.819(5) no Pt N . 2.041(3) yes S O1 . 1.494(10) yes S O2 . 1.400(5) yes S O3 . 1.420(8) yes S O4 . 1.480(11) yes N C . 1.483(7) yes C C 8_445 1.491(12) yes O1 H1O . 0.8200 no N H1N . 0.9000 no N H2N . 0.9000 no C H1C . 0.9700 no C H2C . 0.9700 no 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' S S 0.1246 0.1234 '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_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 4 0 4 0 4 2 0 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 N Pt N 2 . 179.0(2) no N Pt N . 7_445 97.3(2) no N Pt N . 8_445 82.7(2) yes N Pt Cl . . 89.50(11) yes N Pt Cl . 7_445 90.50(11) no Cl Pt Cl . 7_445 180.0 no Cl Pt Cl . 9 0.0 no Cl Pt Cl 9 7_445 180.0 no Cl Cl Pt 9 . 180.0 no O1 S O2 . . 113.8(6) yes O1 S O3 . . 103.5(6) yes O1 S O4 . . 107.5(8) yes O2 S O3 . . 113.1(5) yes O2 S O4 . . 108.6(5) yes O3 S O4 . . 110.2(8) yes O2 S O3 . 10 113.1(5) no O3 S O3 10 . 34.8(12) no O2 S O4 . 10 108.6(5) no O3 S O4 10 10 110.2(8) no O3 S O4 . 10 78.1(7) no O3 S O4 10 . 78.1(7) no O4 S O4 10 . 134.2(10) no O3 S O1 10 . 127.4(7) no O4 S O1 10 . 31.2(6) no O2 S O1 . 10 113.8(6) no O3 S O1 10 10 103.5(6) no O3 S O1 . 10 127.4(7) no O4 S O1 10 10 107.5(8) no O4 S O1 . 10 31.2(6) no O1 S O1 . 10 77.7(10) no C N Pt . . 109.1(3) yes N C C . 8_445 107.1(4) yes S O1 H1O . . 109.5 no C N H1N . . 109.9 no Pt N H1N . . 109.9 no C N H2N . . 109.9 no Pt N H2N . . 109.9 no H1N N H2N . . 108.3 no N C H1C . . 110.3 no C C H1C 8_445 . 110.3 no N C H2C . . 110.3 no C C H2C 8_445 . 110.3 no H1C C H2C . . 108.6 no 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 N H2N O4 6 0.90 1.99 2.860(11) 162 yes N H2N O3 13 0.90 2.22 3.002(12) 146 yes N H1N O2 . 0.90 2.43 3.182(5) 142 yes O1 H1O O3 4 0.82 2.04 2.848(14) 168 yes