#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/33/2203309.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_2203309 loop_ _publ_author_name 'Sakai, Ken' 'Sakai, Itsuki' 'Draper, Neil D.' 'Leznoff, Daniel B.' _publ_section_title ; Di-\m-\a-pyrrolidinonato-bis[cis-diammineplatinum(II)] sulfate hydrate in a head-to-head isomerism ; _journal_issue 3 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m273 _journal_page_last m276 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Pt2 (C4 H6 N O)2 (N H3)4] (S O4), H2 O' _chemical_formula_moiety 'C8 H24 N6 O2 Pt2 2+, S O4 2-, H2 O' _chemical_formula_sum 'C8 H26 N6 O7 Pt2 S' _chemical_formula_weight 740.59 _chemical_name_systematic ; Di-\m-\a-pyrrolidinonato-bis[cis-diammineplatinum(II)] sulfate hydrate ; _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 99.569(10) _cell_angle_beta 93.538(10) _cell_angle_gamma 95.146(10) _cell_formula_units_Z 2 _cell_length_a 6.859(2) _cell_length_b 10.229(2) _cell_length_c 12.896(2) _cell_measurement_reflns_used 1567 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 68.24 _cell_measurement_theta_min 5.13 _cell_volume 885.8(3) _computing_cell_refinement PROCESS-AUTO _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction PROCESS-AUTO _computing_molecular_graphics 'KENX (Sakai, 2002)' _computing_publication_material ; SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEPII (Johnson, 1976) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.928 _diffrn_measured_fraction_theta_max 0.928 _diffrn_measurement_device 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54180 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3014 _diffrn_reflns_theta_full 68.24 _diffrn_reflns_theta_max 68.24 _diffrn_reflns_theta_min 5.13 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 30.633 _exptl_absorpt_correction_T_max 0.465 _exptl_absorpt_correction_T_min 0.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.777 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 688 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.025 _refine_diff_density_max 2.520 _refine_diff_density_min -2.148 _refine_ls_extinction_coef 0.00037(8) _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 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 222 _refine_ls_number_reflns 3014 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0537 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0513P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1170 _refine_ls_wR_factor_ref 0.1265 _reflns_number_gt 2176 _reflns_number_total 3014 _reflns_threshold_expression I>2\s(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2203309 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 0.36898(10) 0.27545(7) 0.11499(5) 0.0357(2) Uani d . 1 Pt Pt2 0.04202(10) 0.32841(6) 0.25238(5) 0.0320(2) Uani d . 1 Pt S1 -0.2172(6) 0.2402(4) -0.1152(3) 0.0352(9) Uani d . 1 S O1 0.4881(18) 0.4458(12) 0.2083(9) 0.047(3) Uani d . 1 O O2 0.4409(17) 0.1671(12) 0.2256(10) 0.048(3) Uani d . 1 O O3 -0.422(2) 0.2011(19) -0.1427(13) 0.090(6) Uani d . 1 O O4 -0.136(2) 0.1445(13) -0.0575(11) 0.066(4) Uani d . 1 O O5 -0.108(2) 0.2489(13) -0.2066(11) 0.062(4) Uani d . 1 O O6 -0.197(3) 0.3696(13) -0.0458(11) 0.081(5) Uani d . 1 O O7 0.202(2) 0.0886(14) -0.2468(12) 0.065(4) Uani d . 1 O N1 0.238(2) 0.4775(13) 0.3212(10) 0.037(3) Uani d . 1 N N2 0.174(2) 0.2013(14) 0.3256(11) 0.039(3) Uani d . 1 N N3 0.315(2) 0.3740(12) -0.0046(11) 0.042(3) Uani d . 1 N H3A 0.4071 0.3624 -0.0498 0.062 Uiso calc R 1 H H3B 0.3150 0.4605 0.0207 0.062 Uiso calc R 1 H H3C 0.1978 0.3427 -0.0376 0.062 Uiso calc R 1 H N4 0.277(2) 0.1081(14) 0.0149(11) 0.048(4) Uani d . 1 N H4A 0.3661 0.0910 -0.0317 0.072 Uiso calc R 1 H H4B 0.1635 0.1176 -0.0189 0.072 Uiso calc R 1 H H4C 0.2607 0.0409 0.0504 0.072 Uiso calc R 1 H N5 -0.0889(17) 0.4588(14) 0.1751(11) 0.037(3) Uani d . 1 N H5A -0.0036 0.5292 0.1735 0.056 Uiso calc R 1 H H5B -0.1921 0.4851 0.2084 0.056 Uiso calc R 1 H H5C -0.1283 0.4191 0.1094 0.056 Uiso calc R 1 H N6 -0.1564(19) 0.1773(14) 0.1783(12) 0.042(3) Uani d . 1 N H6A -0.1353 0.1594 0.1102 0.063 Uiso calc R 1 H H6B -0.2772 0.2012 0.1849 0.063 Uiso calc R 1 H H6C -0.1436 0.1051 0.2072 0.063 Uiso calc R 1 H C1 0.413(2) 0.5057(16) 0.2883(13) 0.038(4) Uani d . 1 C C2 0.522(3) 0.6238(18) 0.3557(15) 0.058(6) Uani d . 1 C H2A 0.5483 0.6952 0.3160 0.069 Uiso calc R 1 H H2B 0.6455 0.6017 0.3858 0.069 Uiso calc R 1 H C3 0.384(3) 0.663(2) 0.4410(17) 0.072(6) Uani d . 1 C H3D 0.4441 0.6542 0.5094 0.086 Uiso calc R 1 H H3E 0.3566 0.7543 0.4431 0.086 Uiso calc R 1 H C4 0.198(3) 0.571(2) 0.4151(16) 0.061(6) Uani d . 1 C H4D 0.1702 0.5242 0.4730 0.073 Uiso calc R 1 H H4E 0.0881 0.6197 0.4001 0.073 Uiso calc R 1 H C5 0.331(2) 0.1455(16) 0.2985(13) 0.036(4) Uani d . 1 C C6 0.389(3) 0.0468(16) 0.3669(13) 0.043(4) Uani d . 1 C H6D 0.5144 0.0758 0.4064 0.052 Uiso calc R 1 H H6E 0.3927 -0.0413 0.3258 0.052 Uiso calc R 1 H C7 0.217(3) 0.051(2) 0.4399(15) 0.065(6) Uani d . 1 C H7A 0.1442 -0.0368 0.4304 0.078 Uiso calc R 1 H H7B 0.2690 0.0742 0.5130 0.078 Uiso calc R 1 H C8 0.084(3) 0.1494(18) 0.4150(13) 0.043(4) Uani d . 1 C H8A 0.0811 0.2202 0.4749 0.052 Uiso calc R 1 H H8B -0.0479 0.1077 0.3942 0.052 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 Pt1 0.0335(5) 0.0343(4) 0.0410(4) 0.0056(3) 0.0039(3) 0.0096(3) Pt2 0.0297(5) 0.0340(4) 0.0342(4) 0.0050(3) -0.0005(3) 0.0112(3) S1 0.039(3) 0.034(2) 0.0329(18) 0.0071(17) 0.0009(17) 0.0064(15) O1 0.043(8) 0.046(7) 0.050(7) 0.007(6) 0.000(6) -0.003(6) O2 0.045(8) 0.054(8) 0.051(7) 0.019(6) 0.009(6) 0.025(6) O3 0.035(9) 0.146(16) 0.077(11) -0.001(9) 0.006(8) -0.010(10) O4 0.095(12) 0.050(8) 0.060(8) 0.017(8) 0.000(8) 0.027(7) O5 0.078(10) 0.053(8) 0.063(8) 0.026(7) 0.023(8) 0.022(7) O6 0.140(15) 0.039(8) 0.061(9) 0.008(9) 0.002(10) 0.001(7) O7 0.055(9) 0.061(9) 0.077(10) 0.011(7) 0.014(7) -0.002(7) N1 0.032(9) 0.042(8) 0.037(7) 0.005(6) -0.003(6) 0.007(6) N2 0.030(9) 0.043(8) 0.044(8) 0.009(6) 0.001(6) 0.003(6) N3 0.056(10) 0.026(7) 0.045(8) 0.011(6) 0.010(7) 0.006(6) N4 0.065(11) 0.045(9) 0.038(7) 0.007(7) -0.002(7) 0.017(6) N5 0.009(7) 0.061(9) 0.049(8) 0.010(6) 0.000(6) 0.024(7) N6 0.023(8) 0.051(9) 0.056(9) 0.003(6) -0.002(6) 0.020(7) C1 0.023(10) 0.043(10) 0.046(9) 0.000(7) -0.016(8) 0.011(8) C2 0.068(15) 0.041(10) 0.053(11) -0.027(9) -0.017(10) 0.001(9) C3 0.083(17) 0.063(14) 0.058(12) -0.004(12) -0.003(12) -0.014(11) C4 0.072(15) 0.051(12) 0.062(12) 0.029(11) 0.014(11) -0.004(10) C5 0.026(10) 0.035(9) 0.048(9) 0.005(7) -0.009(8) 0.012(7) C6 0.059(13) 0.030(9) 0.041(9) 0.013(8) -0.015(8) 0.008(7) C7 0.075(15) 0.090(16) 0.045(10) 0.016(12) 0.021(10) 0.049(11) C8 0.043(11) 0.055(11) 0.038(9) 0.013(9) 0.012(8) 0.017(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' 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 N4 Pt1 O2 89.7(5) yes N4 Pt1 N3 87.3(5) yes O2 Pt1 N3 174.4(5) yes N4 Pt1 O1 174.0(5) yes O2 Pt1 O1 91.5(5) yes N3 Pt1 O1 91.0(5) yes N2 Pt2 N1 91.0(5) yes N2 Pt2 N5 178.8(5) yes N1 Pt2 N5 88.7(5) yes N2 Pt2 N6 89.8(5) yes N1 Pt2 N6 178.4(5) yes N5 Pt2 N6 90.4(5) yes N4 Pt1 Pt2 105.7(4) yes O2 Pt1 Pt2 81.2(3) yes N3 Pt1 Pt2 104.1(4) yes O1 Pt1 Pt2 80.3(4) yes N2 Pt2 Pt1 79.9(4) yes N1 Pt2 Pt1 80.9(4) yes N5 Pt2 Pt1 98.9(4) yes N6 Pt2 Pt1 97.9(4) yes O3 S1 O5 112.5(9) ? O3 S1 O4 109.3(10) ? O5 S1 O4 109.0(8) ? O3 S1 O6 108.2(10) ? O5 S1 O6 109.6(9) ? O4 S1 O6 108.1(8) ? C1 O1 Pt1 125.3(11) ? C5 O2 Pt1 123.3(10) ? C1 N1 C4 112.8(15) ? C1 N1 Pt2 125.2(11) ? C4 N1 Pt2 122.0(13) ? C5 N2 C8 112.8(13) ? C5 N2 Pt2 126.4(12) ? C8 N2 Pt2 120.6(10) ? Pt1 N3 H3A 109.5 ? Pt1 N3 H3B 109.5 ? H3A N3 H3B 109.5 ? Pt1 N3 H3C 109.5 ? H3A N3 H3C 109.5 ? H3B N3 H3C 109.5 ? Pt1 N4 H4A 109.5 ? Pt1 N4 H4B 109.5 ? H4A N4 H4B 109.5 ? Pt1 N4 H4C 109.5 ? H4A N4 H4C 109.5 ? H4B N4 H4C 109.5 ? Pt2 N5 H5A 109.5 ? Pt2 N5 H5B 109.5 ? H5A N5 H5B 109.5 ? Pt2 N5 H5C 109.5 ? H5A N5 H5C 109.5 ? H5B N5 H5C 109.5 ? Pt2 N6 H6A 109.5 ? Pt2 N6 H6B 109.5 ? H6A N6 H6B 109.5 ? Pt2 N6 H6C 109.5 ? H6A N6 H6C 109.5 ? H6B N6 H6C 109.5 ? O1 C1 N1 127.8(15) ? O1 C1 C2 120.2(16) ? N1 C1 C2 112.0(16) ? C1 C2 C3 103.4(16) ? C1 C2 H2A 111.1 ? C3 C2 H2A 111.1 ? C1 C2 H2B 111.1 ? C3 C2 H2B 111.1 ? H2A C2 H2B 109.0 ? C4 C3 C2 107.7(16) ? C4 C3 H3D 110.2 ? C2 C3 H3D 110.2 ? C4 C3 H3E 110.2 ? C2 C3 H3E 110.2 ? H3D C3 H3E 108.5 ? N1 C4 C3 104.0(16) ? N1 C4 H4D 111.0 ? C3 C4 H4D 111.0 ? N1 C4 H4E 111.0 ? C3 C4 H4E 111.0 ? H4D C4 H4E 109.0 ? O2 C5 N2 128.5(15) ? O2 C5 C6 117.8(15) ? N2 C5 C6 113.7(16) ? C5 C6 C7 100.0(13) ? C5 C6 H6D 111.8 ? C7 C6 H6D 111.8 ? C5 C6 H6E 111.8 ? C7 C6 H6E 111.8 ? H6D C6 H6E 109.5 ? C8 C7 C6 110.1(13) ? C8 C7 H7A 109.6 ? C6 C7 H7A 109.6 ? C8 C7 H7B 109.6 ? C6 C7 H7B 109.6 ? H7A C7 H7B 108.1 ? C7 C8 N2 103.3(13) ? C7 C8 H8A 111.1 ? N2 C8 H8A 111.1 ? C7 C8 H8B 111.1 ? N2 C8 H8B 111.1 ? H8A C8 H8B 109.1 ? 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 N4 . 1.991(14) yes Pt1 O2 . 2.011(11) yes Pt1 N3 . 2.012(12) yes Pt1 O1 . 2.020(12) yes Pt2 N2 . 1.978(13) yes Pt2 N1 . 1.990(14) yes Pt2 N5 . 2.030(11) yes Pt2 N6 . 2.031(14) yes Pt1 Pt2 . 2.9749(11) yes Pt1 Pt2 1_655 4.7921(16) yes S1 O3 . 1.431(15) ? S1 O5 . 1.444(14) ? S1 O4 . 1.453(12) ? S1 O6 . 1.460(14) ? O1 C1 . 1.27(2) ? O2 C5 . 1.28(2) ? N1 C1 . 1.32(2) ? N1 C4 . 1.47(2) ? N2 C5 . 1.30(2) ? N2 C8 . 1.49(2) ? C1 C2 . 1.48(2) ? C2 C3 . 1.52(3) ? C3 C4 . 1.50(3) ? C5 C6 . 1.510(19) ? C6 C7 . 1.55(3) ? C7 C8 . 1.48(2) ? N3 H3A . 0.8900 ? N3 H3B . 0.8900 ? N3 H3C . 0.8900 ? N4 H4A . 0.8900 ? N4 H4B . 0.8900 ? N4 H4C . 0.8900 ? N5 H5A . 0.8900 ? N5 H5B . 0.8900 ? N5 H5C . 0.8900 ? N6 H6A . 0.8900 ? N6 H6B . 0.8900 ? N6 H6C . 0.8900 ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 H3D . 0.9700 ? C3 H3E . 0.9700 ? C4 H4D . 0.9700 ? C4 H4E . 0.9700 ? C6 H6D . 0.9700 ? C6 H6E . 0.9700 ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? 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 O5 O7 2.820(18) . yes O7 O3 2.88(2) 1_655 yes 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 N4 H4B O4 . 0.89 2.14 3.00(2) 164 yes N5 H5C O6 . 0.89 2.00 2.87(2) 167 yes N6 H6A O4 . 0.89 2.14 3.02(2) 167 yes N3 H3B O6 2_565 0.89 1.97 2.798(18) 154 yes N3 H3A O3 1_655 0.89 2.32 3.08(2) 143 yes N4 H4C O4 2 0.89 2.03 2.829(19) 149 yes N4 H4A O3 1_655 0.89 2.44 3.18(2) 141 yes N5 H5A O5 2_565 0.89 2.29 3.12(2) 155 yes N5 H5A O6 2_565 0.89 2.50 3.23(2) 140 yes N5 H5B O1 1_455 0.89 2.19 2.954(17) 143 yes N6 H6C O7 2 0.89 2.14 2.99(2) 161 yes N6 H6B O2 1_455 0.89 2.05 2.862(18) 151 yes 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_publ_flag O2 Pt1 Pt2 N2 -3.5(5) yes O1 Pt1 Pt2 N1 -3.9(5) yes N3 Pt1 Pt2 N5 -5.2(6) yes N4 Pt1 Pt2 N6 -4.7(5) yes C4 N1 C1 O1 -178.3(16) ? C4 N1 C1 C2 0(2) ? O1 C1 C2 C3 -179.2(16) ? N1 C1 C2 C3 2(2) ? C1 C2 C3 C4 -3(2) ? C1 N1 C4 C3 -3(2) ? C2 C3 C4 N1 4(2) ? C8 N2 C5 O2 -180.0(16) ? C8 N2 C5 C6 -3(2) ? O2 C5 C6 C7 -179.1(16) ? N2 C5 C6 C7 3.2(19) ? C5 C6 C7 C8 -3(2) ? C6 C7 C8 N2 1(2) ? C5 N2 C8 C7 1(2) ?