#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2204093.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_2204093 _space_group_IT_number 224 _symmetry_space_group_name_Hall '-P 4bc 2bc 3' _symmetry_space_group_name_H-M 'P n -3 m :2' _[local]_cod_cif_authors_sg_H-M 'P n -3 m' _[local]_cod_cif_authors_sg_Hall '-P 4bc 2bc' loop_ _publ_author_name 'Youjun Kang' 'Manrong Li' 'Jingtai Zhao ' 'Shaoyu Mao' _publ_section_title ; The Keggin-type potassium/hydronium 12-tungstophosphate, K~2.4~(H~3~O)~0.6~PO~4~W~12~O~36~ ; _journal_issue 8 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i97 _journal_page_last i99 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'K2.4 (H3 O)0.6 P O4 W12 O36' _chemical_formula_sum 'H1.62 K2.46 O40.54 P W12' _chemical_formula_weight 2983.48 _chemical_name_common 'Potassium/hydronium 12-Tungstophosphate' _chemical_name_systematic ; ; _symmetry_cell_setting cubic _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.5621(8) _cell_length_b 11.5621(8) _cell_length_c 11.5621(8) _cell_measurement_reflns_used 390 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.850 _cell_measurement_theta_min 3.626 _cell_volume 1545.65(19) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics 'DIAMOND (Brandenburg, 1996-2001)' _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 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker SMART APEX 2000' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1245 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12441 _diffrn_reflns_theta_full 28.30 _diffrn_reflns_theta_max 28.30 _diffrn_reflns_theta_min 2.49 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 44.965 _exptl_absorpt_correction_T_max 0.217 _exptl_absorpt_correction_T_min 0.173 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 6.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2551 _exptl_crystal_size_max 0.043 _exptl_crystal_size_mid 0.037 _exptl_crystal_size_min 0.034 _refine_diff_density_max 2.218 _refine_diff_density_min -2.738 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 31 _refine_ls_number_reflns 390 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.149 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0377 _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^)+(0.0408P)^2^+49.5098P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.0915 _reflns_number_gt 360 _reflns_number_total 390 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm6022.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y, -x, -z' 'y+1/2, -x, z+1/2' '-y, x+1/2, z+1/2' 'x+1/2, z+1/2, -y' '-x, z+1/2, y+1/2' '-x, -z, -y' 'x+1/2, -z, y+1/2' 'z+1/2, y+1/2, -x' 'z+1/2, -y, x+1/2' '-z, y+1/2, x+1/2' '-z, -y, -x' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y-1/2, -x-1/2, z' 'y, x, z' '-y-1/2, x, -z-1/2' 'y, -x-1/2, -z-1/2' '-x-1/2, -z-1/2, y' 'x, -z-1/2, -y-1/2' 'x, z, y' '-x-1/2, z, -y-1/2' '-z-1/2, -y-1/2, x' '-z-1/2, y, -x-1/2' 'z, -y-1/2, -x-1/2' 'z, y, x' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 W1 0.46708(4) 0.46708(4) 0.25851(5) 0.0101(3) Uani d S 1 W P1 0.2500 0.2500 0.2500 0.016(3) Uani d S 1 P O1 0.6521(6) 0.6521(6) 0.0044(10) 0.015(2) Uani d S 1 O O2 0.0690(7) 0.0690(7) 0.7681(9) 0.015(2) Uani d S 1 O O3 0.1228(6) 0.1228(6) 0.5380(9) 0.014(2) Uani d S 1 O O4 0.3268(9) 0.3268(9) 0.3268(9) 0.010(4) Uiso d S 1 O K1 0.2500 0.7500 0.7500 0.035(4) Uani d SP 0.82(7) K O5 0.2500 0.7500 0.7500 0.035(4) Uani d SP 0.18(7) 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 0.0103(3) 0.0103(3) 0.0098(4) -0.0021(2) -0.00013(14) -0.00013(14) P1 0.016(3) 0.016(3) 0.016(3) 0.000 0.000 0.000 O1 0.015(3) 0.015(3) 0.014(5) 0.004(4) 0.005(3) 0.005(3) O2 0.014(3) 0.014(3) 0.016(6) -0.008(4) 0.002(3) 0.002(3) O3 0.018(3) 0.018(3) 0.007(5) -0.007(5) 0.000(3) 0.000(3) K1 0.035(7) 0.036(5) 0.036(5) 0.000 0.000 0.000 O5 0.035(7) 0.036(5) 0.036(5) 0.000 0.000 0.000 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 O2 26_666 1.695(11) Y W1 O1 35_665 1.897(3) Y W1 O1 32_665 1.897(3) Y W1 O3 6 1.907(4) Y W1 O3 10 1.907(4) Y W1 O4 . 2.426(10) Y W1 K1 29_666 4.1243(3) ? W1 K1 25_666 4.1243(3) ? P1 O4 . 1.537(18) Y P1 O4 3 1.537(18) ? P1 O4 4 1.537(18) ? P1 O4 2 1.537(18) ? O1 W1 35_665 1.897(3) ? O1 W1 32_665 1.897(3) ? O1 K1 9 3.260(11) ? O2 W1 26_556 1.695(11) ? O2 K1 33_666 2.966(11) ? O3 W1 12 1.907(4) ? O3 W1 7 1.907(4) ? O3 K1 33_666 3.215(10) ? O4 W1 9 2.426(10) ? O4 W1 5 2.426(10) ? K1 O2 30_666 2.966(11) ? K1 O2 29_666 2.966(11) ? K1 O2 32_566 2.966(11) ? K1 O2 31_566 2.966(11) ? K1 O3 29_666 3.215(11) ? K1 O3 30_666 3.215(11) ? K1 O3 32_566 3.215(11) ? K1 O3 31_566 3.215(11) ? K1 O1 5 3.260(11) ? K1 O1 7_565 3.260(11) ? K1 O1 8_556 3.260(11) ? K1 O1 6_566 3.260(11) ? 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 O2 W1 O1 26_666 35_665 103.2(4) Y O2 W1 O1 26_666 32_665 103.2(4) ? O1 W1 O1 35_665 32_665 84.8(7) Y O2 W1 O3 26_666 6 102.2(4) Y O1 W1 O3 35_665 6 154.6(4) Y O1 W1 O3 32_665 6 88.5(5) Y O2 W1 O3 26_666 10 102.2(4) ? O1 W1 O3 35_665 10 88.5(5) ? O1 W1 O3 32_665 10 154.6(4) ? O3 W1 O3 6 10 87.2(6) Y O2 W1 O4 26_666 . 171.5(5) Y O1 W1 O4 35_665 . 83.0(4) Y O1 W1 O4 32_665 . 83.0(4) ? O3 W1 O4 6 . 71.9(3) Y O3 W1 O4 10 . 71.9(3) ? O2 W1 K1 26_666 29_666 82.375(8) ? O1 W1 K1 35_665 29_666 50.4(3) ? O1 W1 K1 32_665 29_666 134.3(3) ? O3 W1 K1 6 29_666 135.3(3) ? O3 W1 K1 10 29_666 49.0(3) ? O4 W1 K1 . 29_666 97.538(11) ? O2 W1 K1 26_666 25_666 82.375(8) ? O1 W1 K1 35_665 25_666 134.3(3) ? O1 W1 K1 32_665 25_666 50.4(3) ? O3 W1 K1 6 25_666 49.0(3) ? O3 W1 K1 10 25_666 135.3(3) ? O4 W1 K1 . 25_666 97.538(11) ? K1 W1 K1 29_666 25_666 164.750(17) ? O4 P1 O4 . 3 109.471(2) ? O4 P1 O4 . 4 109.471(3) ? O4 P1 O4 3 4 109.4710(10) ? O4 P1 O4 . 2 109.5 ? O4 P1 O4 3 2 109.5 ? O4 P1 O4 4 2 109.4710(10) ? W1 O1 W1 35_665 32_665 152.9(7) ? W1 O1 K1 35_665 9 103.0(3) ? W1 O1 K1 32_665 9 103.0(3) ? W1 O2 K1 26_556 33_666 165.5(5) ? W1 O3 W1 12 7 126.8(5) ? W1 O3 K1 12 33_666 104.4(3) ? W1 O3 K1 7 33_666 104.4(3) ? P1 O4 W1 . . 125.8(3) ? P1 O4 W1 . 9 125.8(3) ? W1 O4 W1 . 9 89.3(5) ? P1 O4 W1 . 5 125.8(3) ? W1 O4 W1 . 5 89.3(5) ? W1 O4 W1 9 5 89.3(5) ? O2 K1 O2 30_666 29_666 171.9(4) ? O2 K1 O2 30_666 32_566 90.29(3) ? O2 K1 O2 29_666 32_566 90.29(3) ? O2 K1 O2 30_666 31_566 90.29(3) ? O2 K1 O2 29_666 31_566 90.29(3) ? O2 K1 O2 32_566 31_566 171.9(4) ? O2 K1 O3 30_666 29_666 134.4(3) ? O2 K1 O3 29_666 29_666 53.7(3) ? O2 K1 O3 32_566 29_666 86.91(15) ? O2 K1 O3 31_566 29_666 86.91(15) ? O2 K1 O3 30_666 30_666 53.7(3) ? O2 K1 O3 29_666 30_666 134.4(3) ? O2 K1 O3 32_566 30_666 86.91(15) ? O2 K1 O3 31_566 30_666 86.91(15) ? O3 K1 O3 29_666 30_666 80.6(3) ? O2 K1 O3 30_666 32_566 86.91(15) ? O2 K1 O3 29_666 32_566 86.91(15) ? O2 K1 O3 32_566 32_566 53.7(3) ? O2 K1 O3 31_566 32_566 134.4(3) ? O3 K1 O3 29_666 32_566 125.5(2) ? O3 K1 O3 30_666 32_566 125.5(2) ? O2 K1 O3 30_666 31_566 86.91(15) ? O2 K1 O3 29_666 31_566 86.91(15) ? O2 K1 O3 32_566 31_566 134.4(3) ? O2 K1 O3 31_566 31_566 53.7(3) ? O3 K1 O3 29_666 31_566 125.5(2) ? O3 K1 O3 30_666 31_566 125.5(2) ? O3 K1 O3 32_566 31_566 80.6(3) ? O2 K1 O1 30_666 5 56.5(3) ? O2 K1 O1 29_666 5 115.4(3) ? O2 K1 O1 32_566 5 93.53(18) ? O2 K1 O1 31_566 5 93.53(18) ? O3 K1 O1 29_666 5 169.1(3) ? O3 K1 O1 30_666 5 110.3(2) ? O3 K1 O1 32_566 5 48.38(15) ? O3 K1 O1 31_566 5 48.38(15) ? O2 K1 O1 30_666 7_565 93.53(18) ? O2 K1 O1 29_666 7_565 93.53(18) ? O2 K1 O1 32_566 7_565 56.5(3) ? O2 K1 O1 31_566 7_565 115.4(3) ? O3 K1 O1 29_666 7_565 48.38(15) ? O3 K1 O1 30_666 7_565 48.38(15) ? O3 K1 O1 32_566 7_565 110.3(2) ? O3 K1 O1 31_566 7_565 169.1(3) ? O1 K1 O1 5 7_565 139.4(2) ? O2 K1 O1 30_666 8_556 93.53(18) ? O2 K1 O1 29_666 8_556 93.53(18) ? O2 K1 O1 32_566 8_556 115.4(3) ? O2 K1 O1 31_566 8_556 56.5(3) ? O3 K1 O1 29_666 8_556 48.38(15) ? O3 K1 O1 30_666 8_556 48.38(15) ? O3 K1 O1 32_566 8_556 169.1(3) ? O3 K1 O1 31_566 8_556 110.3(2) ? O1 K1 O1 5 8_556 139.4(2) ? O1 K1 O1 7_565 8_556 58.8(4) ? O2 K1 O1 30_666 6_566 115.4(3) ? O2 K1 O1 29_666 6_566 56.5(3) ? O2 K1 O1 32_566 6_566 93.53(18) ? O2 K1 O1 31_566 6_566 93.53(18) ? O3 K1 O1 29_666 6_566 110.3(2) ? O3 K1 O1 30_666 6_566 169.1(3) ? O3 K1 O1 32_566 6_566 48.38(15) ? O3 K1 O1 31_566 6_566 48.38(15) ? O1 K1 O1 5 6_566 58.8(4) ? O1 K1 O1 7_565 6_566 139.4(2) ? O1 K1 O1 8_556 6_566 139.4(2) ? _cod_database_code 2204093