#------------------------------------------------------------------------------ #$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/33/2013340.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_2013340 loop_ _publ_author_name 'Lee, Uk' 'Joo, Hea-Chung' 'Park, Ki-Min' 'Ozeki, Tomoji' _publ_section_title ; Synchrotron structure determination of an \a-Keggin doubly Pt^IV^-substituted silicotungstate, (CH~6~N~3~)~8~[\a-SiPt~2~W~10~O~40~]·6H~2~O ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m152 _journal_page_last m155 _journal_paper_doi 10.1107/S0108270103004517 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '(C1 H6 N3)8 [O40 Pt2 Si1 W10], 6H2 O1' _chemical_formula_moiety '8C1 H6 N3 1+, O40 Pt2 Si1 W10 8-, 6H2 O1' _chemical_formula_sum 'C8 H60 N24 O46 Pt2 Si W10' _chemical_formula_weight 3485.57 _chemical_name_systematic ; Octaguanidinium \a-silicodiplatinodecatungstate hexahydrate ; _space_group_IT_number 82 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4' _symmetry_space_group_name_H-M 'I -4' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 13.2760(10) _cell_length_b 13.2760(10) _cell_length_c 18.9590(10) _cell_measurement_reflns_used 12596 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.80 _cell_measurement_theta_min 2.00 _cell_volume 3341.6(4) _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'DIP Xpress (MAC Science, 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'MAC Science DIP LABO' _diffrn_measurement_method 'oscillation method' _diffrn_radiation_monochromator Si(111) _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.3282 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 42373 _diffrn_reflns_theta_full 15.80 _diffrn_reflns_theta_max 15.80 _diffrn_reflns_theta_min 2.00 _exptl_absorpt_coefficient_mu 2.857 _exptl_absorpt_correction_T_max 0.5548 _exptl_absorpt_correction_T_min 0.5220 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(PLATON MULABS; Spek, 2003)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 3.464 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description truncated-tetrahedron _exptl_crystal_F_000 3108 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 2.091 _refine_diff_density_min -2.549 _refine_ls_abs_structure_details '(Flack, 1983), 3878 Friedel pairs' _refine_ls_abs_structure_Flack 0.08(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.259 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 207 _refine_ls_number_reflns 7980 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.259 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0293 _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^) + 65.1125P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.0679 _reflns_number_gt 7961 _reflns_number_total 7980 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ob1100.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_Hall I-4 _cod_original_sg_symbol_H-M I-4 _cod_database_code 2013340 _cod_database_fobs_code 2013340 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -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 W1 0.344386(19) 0.393810(19) 0.368398(16) 0.01991(5) Uani d P 0.83 . . W Pt1 0.344386(19) 0.393810(19) 0.368398(16) 0.01991(5) Uani d P 0.17 . . Pt W2 0.235962(16) 0.53609(2) 0.493510(13) 0.01951(4) Uani d P 0.83 . . W Pt2 0.235962(16) 0.53609(2) 0.493510(13) 0.01951(4) Uani d P 0.17 . . Pt W3 0.379342(19) 0.644708(18) 0.368059(15) 0.01938(5) Uani d P 0.83 . . W Pt3 0.379342(19) 0.644708(18) 0.368059(15) 0.01938(5) Uani d P 0.17 . . Pt Si 0.5000 0.5000 0.5000 0.0159(5) Uani d S 1 . . Si Ot1 0.2879(4) 0.3198(4) 0.3053(3) 0.0253(10) Uani d . 1 . . O Ot2 0.1101(3) 0.5536(4) 0.5119(3) 0.0269(10) Uani d . 1 . . O Ot3 0.3467(4) 0.7334(4) 0.3056(3) 0.0266(10) Uani d . 1 . . O Oe4 0.2242(4) 0.4345(4) 0.4209(3) 0.0221(8) Uani d . 1 . . O Oe5 0.2528(4) 0.6362(4) 0.4194(2) 0.0215(8) Uani d . 1 . . O Oe6 0.3409(4) 0.5223(4) 0.3188(2) 0.0217(8) Uani d . 1 . . O Oc7 0.5156(4) 0.6181(4) 0.3418(3) 0.0212(8) Uani d . 1 . . O Oc8 0.2960(4) 0.6277(4) 0.5595(3) 0.0212(8) Uani d . 1 . . O Oc9 0.4309(4) 0.7311(4) 0.4408(3) 0.0207(8) Uani d . 1 . . O Od10 0.3999(3) 0.5142(3) 0.4497(2) 0.0151(7) Uani d . 1 . . O C1 0.1961(12) 0.5002(7) 0.1541(6) 0.059(4) Uani d . 1 . . C N1 0.1385(11) 0.5230(7) 0.0980(6) 0.068(4) Uani d . 1 . . N H1A 0.1200 0.5842 0.0910 0.081 Uiso calc R 1 . . H H1B 0.1203 0.4764 0.0693 0.081 Uiso calc R 1 . . H N2 0.2231(12) 0.4051(7) 0.1638(7) 0.075(4) Uani d . 1 . . N H2A 0.2596 0.3890 0.1995 0.090 Uiso calc R 1 . . H H2B 0.2040 0.3596 0.1344 0.090 Uiso calc R 1 . . H N3 0.2222(14) 0.5701(8) 0.1959(7) 0.095(6) Uani d . 1 . . N H3A 0.2587 0.5566 0.2321 0.114 Uiso calc R 1 . . H H3B 0.2033 0.6310 0.1880 0.114 Uiso calc R 1 . . H C2 0.3198(13) 1.0004(10) 0.3410(9) 0.065(4) Uani d . 1 . . C N4 0.2758(14) 0.9461(8) 0.2898(7) 0.089(5) Uani d . 1 . . N H4A 0.2429 0.9759 0.2568 0.107 Uiso calc R 1 . . H H4B 0.2805 0.8814 0.2901 0.107 Uiso calc R 1 . . H N5 0.3745(12) 0.9507(9) 0.3893(6) 0.076(4) Uani d . 1 . . N H5A 0.4064 0.9835 0.4214 0.091 Uiso calc R 1 . . H H5B 0.3777 0.8860 0.3881 0.091 Uiso calc R 1 . . H N6 0.3125(15) 1.0986(9) 0.3405(8) 0.100(7) Uani d . 1 . . N H6A 0.3435 1.1337 0.3719 0.120 Uiso calc R 1 . . H H6B 0.2768 1.1281 0.3088 0.120 Uiso calc R 1 . . H Ow1 0.5000 0.5000 0.1949(8) 0.126(8) Uani d S 1 . . O Ow2 0.2007(16) 0.8262(10) 0.5015(17) 0.178(8) Uani d . 1 . . O 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 W1 0.02067(10) 0.02074(10) 0.01833(10) -0.00228(7) -0.00428(9) -0.00320(9) Pt1 0.02067(10) 0.02074(10) 0.01833(10) -0.00228(7) -0.00428(9) -0.00320(9) W2 0.01312(9) 0.02381(11) 0.02159(9) 0.00160(8) 0.00118(8) 0.00019(9) Pt2 0.01312(9) 0.02381(11) 0.02159(9) 0.00160(8) 0.00118(8) 0.00019(9) W3 0.02164(10) 0.01865(9) 0.01785(10) 0.00119(7) -0.00220(9) 0.00483(8) Pt3 0.02164(10) 0.01865(9) 0.01785(10) 0.00119(7) -0.00220(9) 0.00483(8) Si 0.0162(7) 0.0162(7) 0.0152(11) 0.000 0.000 0.000 Ot1 0.025(2) 0.024(2) 0.027(2) -0.0004(18) -0.0076(18) -0.0086(18) Ot2 0.0139(17) 0.038(3) 0.028(3) 0.0043(17) 0.0027(16) 0.002(2) Ot3 0.028(2) 0.025(2) 0.027(2) 0.0033(18) -0.0083(19) 0.0071(18) Oe4 0.021(2) 0.024(2) 0.022(2) -0.0039(16) -0.0021(16) -0.0025(16) Oe5 0.0201(19) 0.024(2) 0.0203(19) 0.0019(16) 0.0016(15) 0.0039(16) Oe6 0.025(2) 0.022(2) 0.0188(19) -0.0011(16) -0.0035(16) -0.0017(15) Oc7 0.0184(19) 0.0210(19) 0.024(2) -0.0006(15) -0.0005(16) -0.0034(16) Oc8 0.023(2) 0.0198(19) 0.0207(19) -0.0020(16) -0.0015(16) -0.0015(15) Oc9 0.0195(19) 0.022(2) 0.0205(19) -0.0008(16) -0.0023(15) -0.0015(15) Od10 0.0135(15) 0.0174(17) 0.0145(16) 0.0004(13) -0.0045(12) -0.0007(13) C1 0.106(10) 0.019(3) 0.053(6) 0.007(4) -0.052(7) -0.003(3) N1 0.118(10) 0.028(4) 0.057(6) 0.017(5) -0.059(6) -0.010(4) N2 0.134(12) 0.025(4) 0.066(7) 0.019(5) -0.047(8) -0.003(4) N3 0.160(15) 0.035(5) 0.091(9) 0.027(7) -0.097(10) -0.025(5) C2 0.080(10) 0.039(6) 0.076(9) 0.004(6) -0.027(8) -0.013(6) N4 0.153(13) 0.037(5) 0.078(7) 0.028(6) -0.089(9) -0.012(5) N5 0.126(12) 0.053(6) 0.050(6) 0.000(7) -0.047(7) -0.003(5) N6 0.186(18) 0.031(5) 0.084(9) 0.012(7) -0.081(10) -0.012(5) Ow1 0.095(17) 0.22(3) 0.062(9) -0.03(2) 0.000 0.000 Ow2 0.25(2) 0.078(9) 0.210(19) 0.070(11) -0.06(2) -0.064(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W W -1.4577 1.8630 'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)' O O 0.0032 0.0011 'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)' C C -0.0017 0.0003 'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)' N N -0.0027 0.0006 'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)' Si Si 0.0025 0.0139 'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)' Pt Pt -1.4795 2.3196 'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)' H H 0.0000 0.0000 'International Tables Vol. C Table 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag W3 W1 W2 3_665 4_656 59.974(7) yes W2 W1 W3 . . 60.209(8) yes W1 W2 W3 . . 59.992(8) yes W2 W1 W2 . 4_656 90.149(9) yes W1 W2 W3 . 4_656 90.066(9) yes Od10 Si Od10 4_656 . 109.63(15) yes Od10 Si Od10 . 3_665 109.2(3) yes W1 W3 W2 . . 59.799(8) yes Ot1 W1 Oc8 . 4_656 101.1(2) ? Ot1 W1 Oc7 . 3_665 101.0(2) ? Oc8 W1 Oc7 4_656 3_665 86.8(2) ? Ot1 W1 Oe6 . . 98.9(2) ? Oc8 W1 Oe6 4_656 . 160.0(2) ? Oc7 W1 Oe6 3_665 . 88.2(2) ? Ot1 W1 Oe4 . . 99.0(2) ? Oc8 W1 Oe4 4_656 . 89.0(2) ? Oc7 W1 Oe4 3_665 . 160.0(2) ? Oe6 W1 Oe4 . . 89.1(2) ? Ot1 W1 Od10 . . 170.3(2) ? Oc8 W1 Od10 4_656 . 86.13(18) ? Oc7 W1 Od10 3_665 . 85.67(18) ? Oe6 W1 Od10 . . 74.18(17) ? Oe4 W1 Od10 . . 74.55(17) ? W3 W1 W2 . 4_656 120.118(10) ? Ot2 W2 Oc8 . . 100.7(2) ? Ot2 W2 Oc9 . 4_656 100.8(2) ? Oc8 W2 Oc9 . 4_656 86.8(2) ? Ot2 W2 Oe4 . . 99.2(2) ? Oc8 W2 Oe4 . . 160.1(2) ? Oc9 W2 Oe4 4_656 . 88.4(2) ? Ot2 W2 Oe5 . . 99.5(2) ? Oc8 W2 Oe5 . . 89.5(2) ? Oc9 W2 Oe5 4_656 . 159.7(2) ? Oe4 W2 Oe5 . . 88.4(2) ? Ot2 W2 Od10 . . 171.0(2) ? Oc8 W2 Od10 . . 85.67(18) ? Oc9 W2 Od10 4_656 . 85.87(18) ? Oe4 W2 Od10 . . 74.71(17) ? Oe5 W2 Od10 . . 73.92(17) ? W3 W2 W3 . 4_656 119.912(10) ? Ot3 W3 Oc7 . . 100.7(2) ? Ot3 W3 Oc9 . . 100.1(2) ? Oc7 W3 Oc9 . . 87.7(2) ? Ot3 W3 Oe6 . . 100.1(2) ? Oc7 W3 Oe6 . . 88.2(2) ? Oc9 W3 Oe6 . . 159.8(2) ? Ot3 W3 Oe5 . . 99.5(2) ? Oc7 W3 Oe5 . . 159.8(2) ? Oc9 W3 Oe5 . . 89.0(2) ? Oe6 W3 Oe5 . . 88.0(2) ? Ot3 W3 Od10 . . 171.5(2) ? Oc7 W3 Od10 . . 85.67(18) ? Oc9 W3 Od10 . . 85.73(18) ? Oe6 W3 Od10 . . 74.26(17) ? Oe5 W3 Od10 . . 74.18(17) ? W2 Oe4 W1 . . 119.3(2) ? W3 Oe5 W2 . . 120.0(2) ? W3 Oe5 Ow2 . . 113.8(5) ? W2 Oe5 Ow2 . . 99.8(6) ? W3 Oe6 W1 . . 119.6(2) ? W3 Oe6 Ow1 . . 105.0(2) ? W1 Oe6 Ow1 . . 105.1(2) ? W3 Oc7 W1 . 3_665 149.2(3) ? W3 Oc7 Ow1 . . 104.81(18) ? W1 Oc7 Ow1 3_665 . 104.42(18) ? W2 Oc8 W1 . 2_566 150.1(3) ? W2 Oc8 Ow2 . . 97.9(4) ? W1 Oc8 Ow2 2_566 . 111.2(4) ? W3 Oc9 W2 . 2_566 149.4(3) ? W1 Od10 W3 . . 91.92(14) ? W1 Od10 W2 . . 91.46(14) ? W3 Od10 W2 . . 91.94(14) ? N3 C1 N2 . . 122.5(10) ? N3 C1 N1 . . 118.9(9) ? N2 C1 N1 . . 118.6(9) ? N6 C2 N5 . . 122.3(13) ? N6 C2 N4 . . 119.9(13) ? N5 C2 N4 . . 117.7(11) ? Oe6 Ow1 Oe6 3_665 . 84.5(4) ? Oe6 Ow1 Oc7 3_665 . 50.1(2) ? Oe6 Ow1 Oc7 . . 49.7(2) ? Oe6 Ow1 Oc7 3_665 3_665 49.7(2) ? Oe6 Ow1 Oc7 . 3_665 50.1(2) ? Oc7 Ow1 Oc7 . 3_665 59.2(3) ? Oe5 Ow2 Oc8 . . 52.4(2) ? C1 N1 H1A . . 120.0 ? C1 N1 H1B . . 120.0 ? H1A N1 H1B . . 120.0 ? C1 N2 H2A . . 120.0 ? C1 N2 H2B . . 120.0 ? H2A N2 H2B . . 120.0 ? C1 N3 H3A . . 120.0 ? C1 N3 H3B . . 120.0 ? H3A N3 H3B . . 120.0 ? C2 N4 H4A . . 120.0 ? C2 N4 H4B . . 120.0 ? H4A N4 H4B . . 120.0 ? C2 N5 H5A . . 120.0 ? C2 N5 H5B . . 120.0 ? H5A N5 H5B . . 120.0 ? C2 N6 H6A . . 120.0 ? C2 N6 H6B . . 120.0 ? H6A N6 H6B . . 120.0 ? 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 W1 W2 . 3.3565(4) yes W1 W3 . 3.3631(4) yes W2 W3 . 3.3704(4) yes W1 W2 4_656 3.7100(4) yes W1 W3 3_665 3.7033(4) yes W2 W3 4_656 3.7051(4) yes W1 Ot1 . 1.721(5) yes W1 Oc8 4_656 1.921(5) yes W1 Oc7 3_665 1.932(5) yes W1 Oe6 . 1.948(5) yes W1 Oe4 . 1.956(5) yes W1 Od10 . 2.339(4) yes W2 Ot2 . 1.722(4) yes W2 Oc8 . 1.919(5) yes W2 Oc9 4_656 1.922(5) yes W2 Oe4 . 1.934(5) yes W2 Oe5 . 1.948(5) yes W2 Od10 . 2.348(4) yes W3 Ot3 . 1.725(5) yes W3 Oc7 . 1.910(5) yes W3 Oc9 . 1.920(5) yes W3 Oe6 . 1.943(5) yes W3 Oe5 . 1.945(5) yes W3 Od10 . 2.339(4) yes Si Od10 . 1.646(4) yes C1 N3 . 1.268(13) yes C1 N2 . 1.324(13) yes C1 N1 . 1.344(12) yes C2 N6 . 1.308(17) yes C2 N5 . 1.342(18) yes C2 N4 . 1.342(17) yes Ow1 Oe6 3_665 3.174(13) yes Ow1 Oc7 . 3.204(14) yes Ow1 Oe6 . 3.174(13) yes Ow1 Oe6 . 3.174(13) yes Ow2 Oe5 . 3.043(17) yes Ow2 Oc8 . 3.123(19) yes N5 Ot2 2_566 3.132(13) yes N1 H1A . 0.8600 ? N1 H1B . 0.8600 ? N2 H2A . 0.8600 ? N2 H2B . 0.8600 ? N3 H3A . 0.8600 ? N3 H3B . 0.8600 ? N4 H4A . 0.8600 ? N4 H4B . 0.8600 ? N5 H5A . 0.8600 ? N5 H5B . 0.8600 ? N6 H6A . 0.8600 ? N6 H6B . 0.8600 ? 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 N1 H1B Ot2 6_455 0.86 2.11 2.957(10) 166.1 N1 H1A Oe4 8 0.86 2.01 2.864(10) 174.9 N2 H2A Ot1 . 0.86 2.24 3.036(12) 154.5 N2 H2B Oe5 6_455 0.86 2.02 2.865(12) 167.9 N3 H3B Ot1 8 0.86 2.11 2.945(11) 163.8 N3 H3A Oe6 . 0.86 2.02 2.884(11) 178.1 N4 H4B Ot1 8 0.86 2.57 3.045(13) 116.2 N4 H4B Ot3 . 0.86 2.17 2.991(12) 158.8 N5 H5A Ot2 4_666 0.86 2.17 2.984(12) 157.8 N6 H6B Ot1 1_565 0.86 2.55 3.029(13) 116.2 N6 H6B Ot3 6_465 0.86 2.27 3.050(14) 151.1