#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100736.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100736 _chemical_formula_sum 'K14 La O158 P4 W34' _chemical_formula_weight 9589.09 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' 'La' 'La' -0.2871 2.4523 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M C2/c 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' _cell_length_a 41.339(8) _cell_length_b 15.636(3) _cell_length_c 24.988(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.53(3) _cell_angle_gamma 90.00 _cell_volume 15635(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 16652 _exptl_absorpt_coefficient_mu 25.692 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34400 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.57 _reflns_number_total 17934 _reflns_number_gt 12594 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1104P)^2^+2917.2334P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17934 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1162 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.1953 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.09244(2) 0.10038(7) 1.03130(4) 0.0233(2) Uani 1 1 d . . . W2 W 0.02275(2) 0.07338(7) 0.90275(3) 0.0202(2) Uani 1 1 d . . . W3 W 0.03694(3) 0.28133(7) 0.97872(4) 0.0289(2) Uani 1 1 d . . . W4 W 0.15812(2) 0.22013(8) 1.02124(4) 0.0311(3) Uani 1 1 d . . . W5 W 0.06439(2) -0.03596(7) 0.75190(4) 0.0252(2) Uani 1 1 d . . . W6 W 0.06519(3) -0.12746(7) 0.87213(4) 0.0271(2) Uani 1 1 d . . . W7 W 0.09266(2) 0.28184(8) 0.77711(4) 0.0315(3) Uani 1 1 d . . . W8 W 0.13867(2) 0.09160(9) 0.74297(4) 0.0372(3) Uani 1 1 d . . . W9 W 0.13498(3) -0.09488(8) 0.99606(4) 0.0323(3) Uani 1 1 d . . . W10 W 0.16004(3) 0.31633(10) 0.88759(5) 0.0441(3) Uani 1 1 d . . . W11 W 0.20082(2) 0.02205(10) 0.98638(4) 0.0391(3) Uani 1 1 d . . . W12 W 0.10232(3) 0.40277(8) 0.96772(5) 0.0387(3) Uani 1 1 d . . . La1 La 0.0000 0.16333(13) 0.7500 0.0197(4) Uani 1 2 d S . . W14 W 0.03575(3) 0.36980(7) 0.85322(4) 0.0320(3) Uani 1 1 d . . . W15 W 0.20337(3) 0.12006(11) 0.85343(4) 0.0494(4) Uani 1 1 d . . . W16 W 0.21317(3) -0.11506(12) 0.87055(5) 0.0591(5) Uani 1 1 d . . . W17 W 0.14704(4) -0.23373(10) 0.88149(5) 0.0518(4) Uani 1 1 d . . . W18 W 0.14724(3) -0.14194(11) 0.75775(4) 0.0486(4) Uani 1 1 d . . . P1 P 0.13602(15) -0.0126(5) 0.8656(3) 0.0307(16) Uani 1 1 d . . . P2 P 0.09041(14) 0.1969(5) 0.9054(2) 0.0263(14) Uani 1 1 d . . . O21 O -0.0048(4) 0.1044(11) 0.8395(7) 0.023(3) Uiso 1 1 d . . . O35 O 0.0602(4) 0.0551(10) 0.9748(6) 0.021(3) Uiso 1 1 d . . . O39 O 0.0589(4) 0.2124(11) 0.7603(7) 0.025(3) Uiso 1 1 d . . . O17 O -0.0058(4) 0.0241(11) 0.9329(7) 0.025(3) Uiso 1 1 d . . . O16 O 0.0400(5) -0.2065(13) 0.8863(8) 0.037(4) Uiso 1 1 d . . . O43 O 0.1854(5) 0.1209(13) 0.7764(8) 0.037(4) Uiso 1 1 d . . . O5 O 0.0688(4) 0.2066(10) 1.0255(6) 0.020(3) Uiso 1 1 d . . . O9 O 0.0131(4) 0.2807(12) 0.8188(7) 0.031(4) Uiso 1 1 d . . . O50 O 0.0429(4) -0.0623(11) 0.6854(6) 0.022(3) Uiso 1 1 d . . . O40 O 0.0933(4) -0.1055(11) 0.9437(7) 0.024(3) Uiso 1 1 d . . . O41 O 0.0508(4) -0.1264(11) 0.7948(7) 0.023(3) Uiso 1 1 d . . . O8 O 0.0703(5) 0.3612(13) 0.8156(8) 0.035(4) Uiso 1 1 d . . . O42 O 0.0963(4) 0.0448(11) 0.7369(7) 0.026(4) Uiso 1 1 d . . . O32 O 0.0634(4) 0.1337(11) 0.8793(7) 0.024(3) Uiso 1 1 d . . . O11 O 0.0396(4) -0.0307(10) 0.8802(6) 0.021(3) Uiso 1 1 d . . . O19 O 0.0888(5) 0.3408(13) 0.7176(8) 0.035(4) Uiso 1 1 d . . . O52 O 0.1913(5) 0.2581(14) 1.0725(8) 0.039(5) Uiso 1 1 d . . . O18 O 0.0816(4) 0.0637(12) 1.0891(7) 0.031(4) Uiso 1 1 d . . . O14 O 0.1790(5) 0.1102(12) 1.0139(7) 0.032(4) Uiso 1 1 d . . . O46 O 0.0703(5) 0.4456(14) 0.9106(8) 0.040(5) Uiso 1 1 d . . . O47 O 0.0169(5) 0.3567(12) 0.9177(8) 0.034(4) Uiso 1 1 d . . . O4 O 0.0190(4) 0.1843(11) 0.9380(7) 0.027(4) Uiso 1 1 d . . . O37 O 0.1707(5) 0.2593(13) 0.9584(8) 0.037(4) Uiso 1 1 d . . . O51 O 0.2396(5) 0.0314(13) 1.0324(8) 0.038(4) Uiso 1 1 d . . . O26 O 0.0731(4) 0.2796(11) 0.9198(7) 0.025(4) Uiso 1 1 d . . . O53 O 0.1032(5) -0.1214(13) 0.7497(8) 0.034(4) Uiso 1 1 d . . . O1 O 0.0097(5) 0.2954(13) 1.0207(8) 0.035(4) Uiso 1 1 d . . . O33 O 0.1809(5) -0.0612(13) 1.0242(8) 0.035(4) Uiso 1 1 d . . . O13 O 0.1218(4) 0.0040(11) 1.0240(7) 0.026(4) Uiso 1 1 d . . . O36 O 0.1339(4) 0.1638(11) 1.0656(7) 0.024(3) Uiso 1 1 d . . . O45 O 0.0691(5) 0.3725(12) 1.0055(8) 0.033(4) Uiso 1 1 d . . . O34 O 0.2538(6) -0.1484(17) 0.8816(10) 0.058(6) Uiso 1 1 d . . . O44 O 0.2065(5) 0.0948(14) 0.9282(9) 0.043(5) Uiso 1 1 d . . . O49 O 0.1369(5) 0.1113(13) 0.6753(8) 0.039(5) Uiso 1 1 d . . . O29 O 0.1480(4) 0.0661(12) 0.8374(7) 0.030(4) Uiso 1 1 d . . . O15 O 0.1304(5) -0.1652(14) 1.0469(8) 0.041(5) Uiso 1 1 d . . . O54 O 0.1014(4) -0.2024(12) 0.8656(7) 0.032(4) Uiso 1 1 d . . . O27 O 0.1463(4) -0.0035(12) 0.9291(7) 0.029(4) Uiso 1 1 d . . . O20 O 0.1937(6) 0.3872(16) 0.8973(10) 0.052(6) Uiso 1 1 d . . . O38 O 0.1360(5) 0.3427(13) 0.8179(8) 0.033(4) Uiso 1 1 d . . . O12 O 0.1813(5) 0.2223(13) 0.8581(8) 0.040(5) Uiso 1 1 d . . . O2 O 0.0128(5) 0.4567(14) 0.8208(9) 0.042(5) Uiso 1 1 d . . . O6 O 0.1307(5) 0.3143(13) 1.0149(8) 0.035(4) Uiso 1 1 d . . . O23 O 0.1552(5) -0.0281(13) 0.7430(8) 0.038(5) Uiso 1 1 d . . . O28 O 0.0982(4) -0.0272(11) 0.8441(7) 0.024(3) Uiso 1 1 d . . . O22 O 0.1503(5) -0.1801(13) 0.9506(8) 0.036(4) Uiso 1 1 d . . . O24 O 0.1446(5) -0.2442(15) 0.8041(9) 0.045(5) Uiso 1 1 d . . . O30 O 0.1117(4) 0.2258(11) 0.8660(7) 0.024(3) Uiso 1 1 d . . . O48 O 0.2431(6) 0.1622(15) 0.8559(9) 0.049(5) Uiso 1 1 d . . . O31 O 0.1129(4) 0.1614(11) 0.9598(6) 0.023(3) Uiso 1 1 d . . . O7 O 0.1328(5) 0.3846(13) 0.9209(8) 0.040(5) Uiso 1 1 d . . . O25 O 0.1542(5) -0.0965(13) 0.8502(8) 0.039(5) Uiso 1 1 d . . . O3 O 0.1191(6) 0.4937(16) 1.0031(9) 0.050(5) Uiso 1 1 d . . . O59 O 0.2123(5) -0.0685(14) 0.9412(9) 0.043(5) Uiso 1 1 d . . . O55 O 0.1963(5) -0.1496(14) 0.7968(8) 0.042(5) Uiso 1 1 d . . . O57 O 0.1501(6) -0.1955(16) 0.6986(10) 0.052(6) Uiso 1 1 d . . . O56 O 0.1948(6) -0.2188(15) 0.8936(9) 0.049(5) Uiso 1 1 d . . . O58 O 0.1460(7) -0.3443(18) 0.8982(11) 0.063(7) Uiso 1 1 d . . . O60 O 0.2137(5) -0.0011(14) 0.8475(9) 0.044(5) Uiso 1 1 d . . . O10 O 0.1239(4) 0.1967(12) 0.7620(7) 0.028(4) Uiso 1 1 d . . . K2 K 0.2436(2) 0.1565(9) 1.1188(4) 0.088(3) Uani 1 1 d . . . K1 K -0.0623(3) 0.2823(9) 0.9856(6) 0.106(4) Uani 1 1 d . . . O61 O 0.0384(4) 0.0418(10) 0.7702(6) 0.019(3) Uiso 1 1 d . . . K4 K 0.06700(13) -0.0891(4) 1.1265(2) 0.0320(13) Uani 1 1 d . . . K5 K 0.01881(15) -0.1464(5) 0.5904(2) 0.0368(14) Uani 1 1 d . . . K6 K 0.1119(5) 0.3179(12) 1.1200(7) 0.139(6) Uani 1 1 d . . . O62 O 0.0507(5) -0.2599(15) 1.1214(9) 0.045(5) Uiso 1 1 d . . . O63 O -0.0414(5) 0.1166(13) 0.9937(8) 0.039(5) Uiso 1 1 d . . . O64 O 0.1840(5) 0.0467(14) 1.1366(9) 0.042(5) Uiso 1 1 d . . . O65 O 0.1954(7) 0.3404(18) 1.1778(11) 0.064(7) Uiso 1 1 d . . . O66 O 0.2869(9) -0.084(2) 1.0962(14) 0.090(10) Uiso 1 1 d . . . O67 O 0.0019(10) -0.362(3) 0.8537(16) 0.104(11) Uiso 1 1 d . . . O68 O 0.3079(9) -0.022(2) 1.0385(15) 0.094(10) Uiso 1 1 d . . . O69 O 0.2199(9) -0.224(2) 1.0195(14) 0.092(10) Uiso 1 1 d . . . K7 K 0.0000 -0.254(3) 0.7500 0.29(2) Uani 1 2 d S . . O71 O -0.0533(7) 0.507(2) 0.7726(12) 0.074(8) Uiso 1 1 d . . . O72 O 0.2279(7) -0.002(2) 1.2333(12) 0.069(7) Uiso 1 1 d . . . K8 K 0.2500 0.2500 1.0000 0.28(3) Uani 1 2 d S . . O74 O 0.0595(11) -0.262(3) 0.6599(18) 0.125(14) Uiso 1 1 d . . . O75 O 0.2383(16) 0.198(4) 1.234(2) 0.16(2) Uiso 1 1 d . . . O76 O 0.2145(19) 0.221(5) 1.192(3) 0.20(3) Uiso 1 1 d . . . O77 O 0.1086(11) 0.521(3) 0.8208(17) 0.114(13) Uiso 1 1 d . . . O78 O 0.212(2) -0.115(6) 1.144(4) 0.26(4) Uiso 1 1 d . . . O79 O 0.272(2) 0.012(6) 1.172(3) 0.24(3) Uiso 1 1 d . . . O80 O 0.264(4) 0.141(11) 1.217(6) 0.39(8) Uiso 1 1 d . . . O81 O -0.043(3) 0.436(7) 0.941(4) 0.30(5) Uiso 1 1 d . . . K3 K 0.267(5) 0.406(10) 0.809(8) 0.72(16) Uani 0.63(3) 1 d P . 1 K3 K 0.2815(4) 0.1007(14) 0.9733(7) 0.043(7) Uani 0.37(3) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0148(4) 0.0402(6) 0.0132(4) -0.0011(4) 0.0003(3) -0.0023(4) W2 0.0118(4) 0.0338(6) 0.0140(4) -0.0007(4) 0.0012(3) -0.0019(4) W3 0.0262(5) 0.0362(6) 0.0210(5) -0.0073(4) -0.0006(4) 0.0049(4) W4 0.0165(4) 0.0534(7) 0.0191(5) 0.0008(4) -0.0037(3) -0.0087(4) W5 0.0187(4) 0.0425(6) 0.0134(4) 0.0012(4) 0.0021(3) 0.0091(4) W6 0.0321(5) 0.0317(6) 0.0156(4) 0.0005(4) 0.0024(4) 0.0060(4) W7 0.0205(5) 0.0476(7) 0.0217(5) 0.0067(4) -0.0031(4) -0.0122(4) W8 0.0134(4) 0.0818(9) 0.0154(5) 0.0047(5) 0.0020(3) 0.0019(5) W9 0.0311(5) 0.0481(7) 0.0148(4) 0.0029(4) 0.0006(4) 0.0132(5) W10 0.0244(5) 0.0769(10) 0.0247(5) 0.0098(5) -0.0058(4) -0.0224(6) W11 0.0179(5) 0.0794(9) 0.0169(5) 0.0028(5) -0.0018(4) 0.0137(5) W12 0.0411(6) 0.0364(7) 0.0288(6) -0.0015(5) -0.0098(5) -0.0090(5) La1 0.0107(7) 0.0303(11) 0.0162(8) 0.000 -0.0004(6) 0.000 W14 0.0339(5) 0.0294(6) 0.0255(5) -0.0015(4) -0.0061(4) 0.0002(4) W15 0.0125(4) 0.1140(13) 0.0197(5) 0.0064(6) 0.0004(4) -0.0033(6) W16 0.0304(6) 0.1203(14) 0.0227(6) -0.0038(7) -0.0009(4) 0.0421(8) W17 0.0607(8) 0.0671(10) 0.0212(5) -0.0017(5) -0.0015(5) 0.0435(7) W18 0.0357(6) 0.0883(11) 0.0189(5) -0.0038(6) 0.0016(4) 0.0370(7) P1 0.016(3) 0.056(5) 0.018(3) -0.001(3) 0.000(2) 0.013(3) P2 0.015(3) 0.049(4) 0.013(3) -0.003(3) -0.001(2) -0.006(3) K2 0.045(5) 0.146(11) 0.066(6) -0.010(6) 0.004(4) -0.012(6) K1 0.063(6) 0.129(11) 0.123(10) -0.049(8) 0.018(6) 0.017(7) K4 0.020(2) 0.053(4) 0.019(2) 0.001(2) -0.0013(19) -0.003(2) K5 0.030(3) 0.055(4) 0.025(3) -0.005(3) 0.005(2) 0.003(3) K6 0.140(14) 0.139(14) 0.135(13) -0.016(11) 0.032(11) 0.010(11) K7 0.34(7) 0.21(4) 0.31(6) 0.000 0.07(5) 0.000 K8 0.16(3) 0.19(4) 0.47(8) -0.08(5) 0.03(4) -0.04(3) K3 0.7(3) 0.5(2) 1.0(4) -0.4(2) 0.5(3) -0.3(2) K3 0.018(8) 0.077(15) 0.027(9) 0.015(8) -0.006(6) -0.025(8)