#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/52/2015266.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_2015266 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _publ_author_name ' Odoko, Mamiko' ' Okabe, Nobuo' _publ_section_title ;\ Dichloro(propane-1,3-diamine-\k^2^N,N')platinum(II), dichloro(propane-1,3-diamine-\k^2^N,N')palladium(II) and \m-4,9-diazadodecane-1,12-diamine-\k^2^N^1^,N^4^;\ \k^2^N^9^,N^12^-- bis[dichlorodiplatinum(II)] ; _journal_coeditor_code OB1247 _journal_issue 4 _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first m136 _journal_page_last m139 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Pt2 Cl4 (C10 H26 N4)]' _chemical_formula_moiety 'C10 H26 Cl4 N4 Pt2' _chemical_formula_sum 'C10 H26 Cl4 N4 Pt2' _chemical_formula_weight 734.31 _chemical_name_systematic ; \m-4,9-diazadodecane-1,12-diamine-\k^2^N^1^,N^4^;\k^2^N^9^,N^12^- bis[dichlorodiplatinum(II)] ; _symmetry_cell_setting monoclinic _cell_angle_alpha 90 _cell_angle_beta 92.09(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.860(10) _cell_length_b 8.018(6) _cell_length_c 12.930(10) _cell_measurement_reflns_used 8101 _cell_measurement_temperature 123 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.1 _cell_volume 917.9(14) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2005) and CRYSTALS (Watkin et al., 1996)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material CrystalStructure _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 0.9960 _diffrn_measured_fraction_theta_max 0.9960 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9030 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 15.802 _exptl_absorpt_correction_T_max 0.455 _exptl_absorpt_correction_T_min 0.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 676.00 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_diff_density_max 2.61 _refine_diff_density_min -2.71 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 92 _refine_ls_number_reflns 2105 _refine_ls_R_factor_gt 0.0290 _refine_ls_shift/su_max 0.0010 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.3492P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0760 _reflns_number_gt 1725 _reflns_number_total 2105 _reflns_threshold_expression F^2^>2.0\s(F^2^) _[local]_cod_data_source_file ob1247.cif loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-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 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pt Pt -1.703 8.390 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _atom_site_type_symbol _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 Pt Pt1 0.19858(2) 0.16739(2) 0.825909(16) 0.02137(10) Uani d . 1 Cl Cl1 0.45049(17) 0.16947(15) 0.78547(15) 0.0351(4) Uani d . 1 Cl Cl2 0.24417(15) 0.03880(16) 0.98396(11) 0.0291(3) Uani d . 1 N N1 0.1493(5) 0.2662(6) 0.6856(4) 0.0283(10) Uani d . 1 H H1A 0.1190 0.3724 0.6939 0.034 Uiso calc R 1 H H1B 0.2339 0.2682 0.6492 0.034 Uiso calc R 1 N N2 -0.0242(5) 0.1749(5) 0.8627(4) 0.0226(10) Uani d . 1 H H2 -0.0321 0.1075 0.9188 0.027 Uiso calc R 1 C C1 0.0288(8) 0.1737(7) 0.6241(5) 0.0353(15) Uani d . 1 H H1C 0.0578 0.0576 0.6175 0.042 Uiso calc R 1 H H1D 0.0184 0.2211 0.5552 0.042 Uiso calc R 1 C C2 -0.1197(7) 0.1848(7) 0.6765(5) 0.0331(14) Uani d . 1 H H2A -0.1440 0.3017 0.6857 0.040 Uiso calc R 1 H H2B -0.1974 0.1372 0.6307 0.040 Uiso calc R 1 C C3 -0.1262(6) 0.0997(7) 0.7794(5) 0.0287(12) Uani d . 1 H H3A -0.0992 -0.0166 0.7710 0.034 Uiso calc R 1 H H3B -0.2294 0.1034 0.8020 0.034 Uiso calc R 1 C C4 -0.0748(7) 0.3426(6) 0.8963(5) 0.0276(13) Uani d . 1 H H4A -0.1773 0.3347 0.9199 0.033 Uiso calc R 1 H H4B -0.0755 0.4181 0.8377 0.033 Uiso calc R 1 C C5 0.0268(6) 0.4140(7) 0.9830(5) 0.0317(13) Uani d . 1 H H5A 0.1292 0.4226 0.9596 0.038 Uiso calc R 1 H H5B 0.0276 0.3388 1.0418 0.038 Uiso calc R 1 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 0.02145(14) 0.01958(15) 0.02336(16) 0.00114(6) 0.00473(9) -0.00127(7) Cl1 0.0241(7) 0.0303(8) 0.0515(11) -0.0006(4) 0.0121(7) 0.0017(6) Cl2 0.0305(7) 0.0335(7) 0.0232(7) 0.0054(5) 0.0003(5) -0.0003(5) N1 0.033(3) 0.026(2) 0.027(3) 0.0010(18) 0.014(2) 0.006(2) N2 0.027(3) 0.020(2) 0.021(3) 0.0009(15) 0.005(2) 0.0025(17) C1 0.045(4) 0.036(4) 0.024(3) 0.001(2) -0.001(3) 0.000(2) C2 0.033(3) 0.033(3) 0.032(4) 0.001(2) -0.009(3) -0.003(2) C3 0.024(3) 0.028(3) 0.034(3) -0.005(2) 0.001(2) -0.003(3) C4 0.027(3) 0.024(3) 0.032(3) 0.0083(18) 0.005(2) -0.003(2) C5 0.037(3) 0.034(3) 0.024(3) 0.010(2) 0.002(2) -0.005(2) 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 N1 . 2.013(5) yes Pt1 N2 . 2.047(5) yes Pt1 Cl1 . 2.310(3) yes Pt1 Cl2 . 2.312(2) yes N1 C1 . 1.503(8) ? N1 H1A . 0.9000 ? N1 H1B . 0.9000 ? N2 C4 . 1.488(6) ? N2 C3 . 1.506(7) ? N2 H2 . 0.9100 ? C1 C2 . 1.504(10) ? C1 H1C . 0.9700 ? C1 H1D . 0.9700 ? C2 C3 . 1.499(9) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 C5 . 1.524(8) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 C5 3_567 1.527(11) ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? 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 N1 Pt1 N2 . . 91.0(2) yes N1 Pt1 Cl1 . . 88.44(14) yes N2 Pt1 Cl1 . . 177.87(11) ? N1 Pt1 Cl2 . . 176.04(13) ? N2 Pt1 Cl2 . . 86.94(15) yes Cl1 Pt1 Cl2 . . 93.69(7) yes C1 N1 Pt1 . . 114.2(3) ? C1 N1 H1A . . 108.7 ? Pt1 N1 H1A . . 108.7 ? C1 N1 H1B . . 108.7 ? Pt1 N1 H1B . . 108.7 ? H1A N1 H1B . . 107.6 ? C4 N2 C3 . . 113.1(4) ? C4 N2 Pt1 . . 113.4(3) ? C3 N2 Pt1 . . 112.4(4) ? C4 N2 H2 . . 105.7 ? C3 N2 H2 . . 105.7 ? Pt1 N2 H2 . . 105.7 ? N1 C1 C2 . . 110.4(5) ? N1 C1 H1C . . 109.6 ? C2 C1 H1C . . 109.6 ? N1 C1 H1D . . 109.6 ? C2 C1 H1D . . 109.6 ? H1C C1 H1D . . 108.1 ? C3 C2 C1 . . 115.8(5) ? C3 C2 H2A . . 108.3 ? C1 C2 H2A . . 108.3 ? C3 C2 H2B . . 108.3 ? C1 C2 H2B . . 108.3 ? H2A C2 H2B . . 107.4 ? C2 C3 N2 . . 114.3(4) ? C2 C3 H3A . . 108.7 ? N2 C3 H3A . . 108.7 ? C2 C3 H3B . . 108.7 ? N2 C3 H3B . . 108.7 ? H3A C3 H3B . . 107.6 ? N2 C4 C5 . . 112.3(5) ? N2 C4 H4A . . 109.1 ? C5 C4 H4A . . 109.1 ? N2 C4 H4B . . 109.1 ? C5 C4 H4B . . 109.1 ? H4A C4 H4B . . 107.9 ? C4 C5 C5 . 3_567 111.7(6) ? C4 C5 H5A . . 109.3 ? C5 C5 H5A 3_567 . 109.3 ? C4 C5 H5B . . 109.3 ? C5 C5 H5B 3_567 . 109.3 ? H5A C5 H5B . . 107.9 ? 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_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N2 Pt1 N1 C1 . -53.6(4) yes Cl1 Pt1 N1 C1 . 128.5(4) ? N1 Pt1 N2 C4 . -80.2(4) ? Cl2 Pt1 N2 C4 . 103.3(4) ? N1 Pt1 N2 C3 . 49.7(3) yes Cl2 Pt1 N2 C3 . -126.9(3) ? Pt1 N1 C1 C2 . 65.1(5) yes N1 C1 C2 C3 . -65.7(6) ? C1 C2 C3 N2 . 65.1(7) ? C4 N2 C3 C2 . 69.7(6) ? Pt1 N2 C3 C2 . -60.3(5) yes C3 N2 C4 C5 . 178.1(5) ? Pt1 N2 C4 C5 . -52.5(6) ? N2 C4 C5 C5 3_567 -179.9(6) ? 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 N1 H1A Cl1 2_556 0.90 2.48 3.376(5) 177 yes N1 H1B Cl2 2_556 0.90 2.78 3.261(5) 115 yes N2 H2 Cl2 3_557 0.91 2.58 3.309(6) 138 yes _cod_database_code 2015266