#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2211653.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_2211653 loop_ _publ_author_name 'Lee, Uk' 'Joo, Hea-Chung' _publ_section_title ; Dipotassium hexahydrogen hexamolybdoplatinate(IV) hexahydrate ; _journal_coeditor_code WM2064 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i241 _journal_page_last i243 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac 'K2 [H6 Pt Mo6 O24], 6H2 O' _chemical_formula_moiety '2(K +), H6 Pt Mo6 O24 2-, 6(H2 O)' _chemical_formula_structural 'K2 [H6 Pt Mo6 O24] (H2 O)6' _chemical_formula_sum 'H18 K2 Mo6 O30 Pt' _chemical_formula_weight 1347.07 _chemical_name_systematic ; Dipotassium hexahydrogen hexamolybdoplatinate(IV) hexahydrate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 105.770(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 21.178(3) _cell_length_b 12.940(2) _cell_length_c 10.110(2) _cell_measurement_reflns_used 30 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 10.4 _cell_measurement_theta_min 9.5 _cell_volume 2666.3(8) _computing_cell_refinement STADI4 _computing_data_collection 'STADI4 (Stoe & Cie, 1996)' _computing_data_reduction 'X-RED (Stoe & Cie, 1996)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Stoe Stadi-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0097 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3078 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 1.86 _diffrn_standards_decay_% 3.2 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 8.384 _exptl_absorpt_correction_T_max 0.3762 _exptl_absorpt_correction_T_min 0.2290 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE; Stoe & Cie, 1996)' _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 3.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'hexagonal block' _exptl_crystal_F_000 2504 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.973 _refine_diff_density_min -1.270 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 3056 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.159 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0328 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+9.1413P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.0814 _reflns_number_gt 2608 _reflns_number_total 3056 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm2064.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 2211653 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 Pt 0.2500 0.2500 0.0000 0.01349(9) Uani d S 1 Mo Mo1 0.40336(3) 0.34274(4) 0.06449(6) 0.02157(14) Uani d . 1 Mo Mo2 0.34798(3) 0.26249(4) 0.32760(6) 0.01849(13) Uani d . 1 Mo Mo3 0.19606(3) 0.16989(4) 0.26248(6) 0.01903(13) Uani d . 1 K K1 0.5000 0.62888(19) 0.2500 0.0426(6) Uani d S 1 K K2 0.4913(2) 0.0638(3) 0.5596(5) 0.0566(12) Uani d P 0.50 O O1C 0.3295(2) 0.2475(3) -0.0723(5) 0.0187(9) Uani d . 1 O O2C 0.3026(2) 0.3565(3) 0.1270(5) 0.0186(9) Uani d D 1 H H2 0.284(4) 0.416(5) 0.131(9) 0.03(2) Uiso d D 1 O O3C 0.2827(2) 0.1571(3) 0.1616(4) 0.0160(9) Uani d D 1 H H3 0.298(4) 0.096(5) 0.130(8) 0.03(2) Uiso d D 1 O O4B 0.3522(3) 0.4257(4) -0.1024(5) 0.0261(11) Uani d D 1 H H4 0.361(7) 0.486(7) -0.103(14) 0.11(5) Uiso d D 1 O O5B 0.4045(2) 0.2459(3) 0.2076(5) 0.0216(10) Uani d . 1 O O6B 0.2581(2) 0.2735(4) 0.3417(5) 0.0231(10) Uani d . 1 O O7T 0.4670(3) 0.3023(5) 0.0061(6) 0.0430(14) Uani d . 1 O O8T 0.4277(3) 0.4548(4) 0.1523(6) 0.0377(14) Uani d . 1 O O9T 0.3787(3) 0.3731(4) 0.4121(5) 0.0281(11) Uani d . 1 O O10T 0.3775(3) 0.1636(4) 0.4370(5) 0.0298(12) Uani d . 1 O O11T 0.2256(3) 0.0603(4) 0.3558(5) 0.0305(12) Uani d . 1 O O12T 0.1295(3) 0.2088(4) 0.3103(5) 0.0313(12) Uani d . 1 O O13W 0.5000 0.0853(8) 0.2500 0.064(3) Uani d SD 1 H H13 0.477(5) 0.120(7) 0.273(12) 0.05(3) Uiso d D 1 O O14W 0.6168(5) 0.0610(6) 0.5963(9) 0.068(2) Uani d D 1 H H14A 0.626(7) 0.131(7) 0.575(13) 0.098 Uiso d D 1 H H14B 0.587(5) 0.086(8) 0.616(12) 0.050 Uiso d D 1 O O15W 0.4892(7) 0.1583(9) 0.6918(13) 0.055(4) Uani d PD 0.50 H H15A 0.5064 0.2208 0.6617 0.082 Uiso calc PRD 0.50 H H15B 0.4428 0.1713 0.6790 0.082 Uiso calc PRD 0.50 O O16W 0.3233(3) -0.0263(4) 0.1255(6) 0.0439(15) Uani d . 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 Pt 0.01563(16) 0.01233(15) 0.01243(16) -0.00035(12) 0.00369(12) 0.00013(11) Mo1 0.0183(3) 0.0239(3) 0.0210(3) -0.0040(2) 0.0028(2) 0.0030(2) Mo2 0.0229(3) 0.0161(3) 0.0147(3) -0.0011(2) 0.0021(2) 0.00053(19) Mo3 0.0220(3) 0.0196(3) 0.0166(3) -0.0013(2) 0.0072(2) 0.0029(2) K1 0.0304(13) 0.0294(12) 0.072(2) 0.000 0.0213(13) 0.000 K2 0.042(2) 0.053(2) 0.064(3) -0.0027(19) -0.004(2) 0.007(2) O1C 0.016(2) 0.019(2) 0.021(2) -0.0012(17) 0.0055(18) 0.0020(17) O2C 0.021(2) 0.0119(19) 0.021(2) -0.0014(17) 0.0015(19) -0.0028(17) O3C 0.021(2) 0.014(2) 0.012(2) -0.0010(17) 0.0030(17) 0.0017(16) O4B 0.032(3) 0.022(2) 0.019(2) -0.009(2) -0.001(2) 0.0025(19) O5B 0.019(2) 0.021(2) 0.023(2) 0.0008(18) 0.0020(19) 0.0019(18) O6B 0.028(3) 0.024(2) 0.018(2) -0.0044(19) 0.008(2) -0.0049(18) O7T 0.026(3) 0.058(4) 0.047(4) 0.001(3) 0.014(3) 0.010(3) O8T 0.040(3) 0.028(3) 0.037(3) -0.016(2) -0.004(3) 0.006(2) O9T 0.030(3) 0.022(2) 0.027(3) -0.002(2) -0.002(2) -0.004(2) O10T 0.036(3) 0.026(2) 0.024(3) 0.005(2) 0.003(2) 0.005(2) O11T 0.037(3) 0.024(2) 0.029(3) -0.006(2) 0.007(2) 0.009(2) O12T 0.030(3) 0.038(3) 0.028(3) -0.001(2) 0.012(2) 0.000(2) O13W 0.040(6) 0.033(5) 0.109(10) 0.000 0.001(6) 0.000 O14W 0.094(7) 0.037(4) 0.071(5) -0.019(4) 0.022(5) 0.006(4) O15W 0.056(9) 0.048(7) 0.050(8) 0.017(6) -0.004(7) 0.002(6) O16W 0.057(4) 0.035(3) 0.035(3) 0.011(3) 0.004(3) -0.004(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Mo3 O1C Mo1 7 . 104.58(18) yes Mo2 O2C Mo1 . . 90.27(16) yes Mo2 O3C Mo3 . . 91.55(15) yes Mo1 O4B Mo3 . 7 111.7(2) yes Mo1 O5B Mo2 . . 121.3(2) yes Mo3 O6B Mo2 . . 119.7(2) yes Pt O1C Mo3 . 7 106.7(2) ? Pt O1C Mo1 . . 106.8(2) ? Pt O2C Mo2 . . 102.93(18) ? Pt O2C Mo1 . . 99.22(18) ? Pt O3C Mo2 . . 104.20(17) ? Pt O3C Mo3 . . 100.13(19) ? H14A O14W H14B . . 83(10) ? O15W O15W H15B 2_656 . 104.1 ? H15A O15W H15B . . 105.5 ? Mo3 Mo2 Mo1 . . 118.87(2) ? Mo2 Mo1 Mo3 . 7 119.88(2) ? O3C Pt O3C . 7 180.0(3) ? O3C Pt O2C . 7 96.84(18) ? O3C Pt O2C 7 7 83.16(18) ? O3C Pt O2C . . 83.16(18) ? O3C Pt O2C 7 . 96.84(18) ? O2C Pt O2C 7 . 180.0(4) ? O3C Pt O1C . . 98.60(18) ? O3C Pt O1C 7 . 81.40(18) ? O2C Pt O1C 7 . 97.51(19) ? O2C Pt O1C . . 82.49(19) ? O3C Pt O1C . 7 81.40(18) ? O3C Pt O1C 7 7 98.60(18) ? O2C Pt O1C 7 7 82.49(19) ? O2C Pt O1C . 7 97.51(19) ? O1C Pt O1C . 7 180.00(9) ? O7T Mo1 O8T . . 106.7(3) ? O7T Mo1 O5B . . 102.3(3) ? O8T Mo1 O5B . . 102.9(2) ? O7T Mo1 O4B . . 99.6(3) ? O8T Mo1 O4B . . 90.0(2) ? O5B Mo1 O4B . . 149.9(2) ? O7T Mo1 O1C . . 96.1(2) ? O8T Mo1 O1C . . 151.5(2) ? O5B Mo1 O1C . . 88.19(18) ? O4B Mo1 O1C . . 69.13(18) ? O7T Mo1 O2C . . 165.1(2) ? O8T Mo1 O2C . . 87.9(2) ? O5B Mo1 O2C . . 71.16(18) ? O4B Mo1 O2C . . 82.45(19) ? O1C Mo1 O2C . . 70.74(16) ? O10T Mo2 O9T . . 106.5(2) ? O10T Mo2 O5B . . 98.3(2) ? O9T Mo2 O5B . . 101.0(2) ? O10T Mo2 O6B . . 101.6(2) ? O9T Mo2 O6B . . 98.6(2) ? O5B Mo2 O6B . . 146.69(19) ? O10T Mo2 O3C . . 94.0(2) ? O9T Mo2 O3C . . 159.0(2) ? O5B Mo2 O3C . . 80.14(18) ? O6B Mo2 O3C . . 72.11(18) ? O10T Mo2 O2C . . 162.0(2) ? O9T Mo2 O2C . . 90.5(2) ? O5B Mo2 O2C . . 72.04(18) ? O6B Mo2 O2C . . 81.16(18) ? O3C Mo2 O2C . . 69.69(15) ? O12T Mo3 O11T . . 107.2(3) ? O12T Mo3 O6B . . 101.8(2) ? O11T Mo3 O6B . . 104.1(2) ? O12T Mo3 O4B . 7 97.4(2) ? O11T Mo3 O4B . 7 88.0(2) ? O6B Mo3 O4B . 7 152.9(2) ? O12T Mo3 O1C . 7 94.7(2) ? O11T Mo3 O1C . 7 150.4(2) ? O6B Mo3 O1C . 7 90.18(19) ? O4B Mo3 O1C 7 7 69.25(18) ? O12T Mo3 O3C . . 164.5(2) ? O11T Mo3 O3C . . 88.2(2) ? O6B Mo3 O3C . . 72.43(18) ? O4B Mo3 O3C 7 . 84.05(19) ? O1C Mo3 O3C 7 . 71.31(16) ? O8T K1 O8T . 2_655 70.1(2) ? O8T K1 O15W . 5_666 151.9(3) ? O8T K1 O15W 2_655 5_666 136.1(3) ? O8T K1 O15W . 6_565 136.1(3) ? O8T K1 O15W 2_655 6_565 151.9(3) ? O15W K1 O15W 5_666 6_565 23.4(5) ? O8T K1 O12T . 3 141.86(18) ? O8T K1 O12T 2_655 3 79.05(17) ? O15W K1 O12T 5_666 3 65.1(3) ? O8T K1 O7T . 5_665 99.85(18) ? O8T K1 O7T 2_655 5_665 108.43(18) ? O15W K1 O7T 5_666 5_665 82.2(3) ? O15W K1 O7T 6_565 5_665 63.4(3) ? O15W K1 O7T 5_666 6_566 63.4(3) ? O15W K1 O7T 6_565 6_566 82.2(3) ? O15W K2 O14W . . 97.7(6) ? K2 K2 O14W 5_656 . 75.0(3) ? O15W K2 O13W . 5_656 88.1(5) ? O14W K2 O13W . 5_656 91.1(2) ? O15W K2 O10T . . 79.7(5) ? O14W K2 O10T . . 145.4(3) ? O13W K2 O10T 5_656 . 123.1(2) ? O15W K2 O15W . 2_656 18.0(5) ? O14W K2 O15W . 2_656 89.0(4) ? O13W K2 O15W 5_656 2_656 72.5(3) ? O10T K2 O15W . 2_656 95.8(4) ? O15W K2 O14W . 5_656 127.0(6) ? O14W K2 O14W . 5_656 134.5(2) ? O15W K2 O13W . . 132.8(5) ? O14W K2 O13W . . 79.1(2) ? O13W K2 O13W 5_656 . 138.60(18) ? O10T K2 O13W . . 78.00(18) ? O15W K2 O13W 2_656 . 146.1(4) ? O14W K2 O13W 5_656 . 76.3(2) ? O15W K2 O7T . 2_655 65.4(5) ? K2 K2 O7T 5_656 2_655 120.6(3) ? O14W K2 O7T . 2_655 73.9(2) ? O13W K2 O7T 5_656 2_655 146.8(2) ? O10T K2 O7T . 2_655 73.66(18) ? O15W K2 O7T 2_656 2_655 77.6(3) ? O14W K2 O7T 5_656 2_655 128.5(2) ? O13W K2 O7T . 2_655 68.6(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 Mo1 Mo2 . 3.3503(10) ? Mo1 Mo3 7 3.4065(10) ? Mo2 Mo3 . 3.3269(9) ? Pt O1C . 2.010(4) yes Pt O2C . 2.003(4) yes Pt O3C . 1.995(4) yes Pt O3C 7 1.995(4) ? Pt O2C 7 2.003(4) ? Pt O1C 7 2.010(4) ? Mo1 O1C . 2.169(4) yes Mo1 O2C . 2.391(5) yes Mo1 O4B . 2.044(5) yes Mo1 O5B . 1.909(5) yes Mo1 O7T . 1.696(6) yes Mo1 O8T . 1.706(5) yes Mo2 O2C . 2.336(5) yes Mo2 O3C . 2.308(4) yes Mo2 O5B . 1.934(5) yes Mo2 O6B . 1.953(5) yes Mo2 O9T . 1.702(5) yes Mo2 O10T . 1.695(5) yes Mo3 O1C 7 2.137(4) yes Mo3 O3C . 2.335(5) yes Mo3 O4B 7 2.073(5) yes Mo3 O6B . 1.895(5) yes Mo3 O11T . 1.724(5) yes Mo3 O12T . 1.688(5) yes K1 O7T 5_665 2.994(6) ? K1 O7T 6_566 2.994(6) ? K1 O8T . 2.751(5) ? K1 O8T 2_655 2.751(5) ? K1 O15W 5_666 2.813(13) ? K1 O15W 6_565 2.813(13) ? K1 O12T 3 2.837(5) ? K1 O12T 4 2.837(5) ? K2 O10T . 2.719(7) ? K2 O7T 2_655 3.325(8) ? K2 O13W . 3.198(5) ? K2 O13W 5_656 2.696(9) ? K2 O14W . 2.583(11) ? K2 O14W 5_656 2.894(10) ? K2 O15W . 1.820(14) ? K2 O15W 2_656 2.723(14) ? O2C H2 . 0.86(7) ? O3C H3 . 0.93(6) ? O4B H4 . 0.81(8) ? O13W H13 . 0.75(7) ? O14W H14A . 0.96(8) ? O14W H14B . 0.78(7) ? O15W H15A . 0.9700 ? O15W H15B . 0.9700 ? 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 O2C H2 O11T 4 0.86(7) 1.89(7) 2.720(6) 160(8) O4B H4 O9T 6_565 0.81(8) 1.86(9) 2.659(7) 174(14) O13W H13 O5B . 0.75(7) 2.21(8) 2.850(9) 144(11) O14W H14A O1C 2_655 0.96(8) 1.79(9) 2.707(8) 159(12) O15W H15B O12T 7_556 0.97 2.20 3.041(15) 143.8 O15W H15B O10T . 0.97 2.46 2.988(14) 113.6 O15W H15A O7T 2_655 0.97 2.20 3.056(16) 147.1