#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100737.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_1100737 _chemical_formula_sum 'H46 Cl2 K2 Na2 Nd0.50 O81 P2 W17' _chemical_formula_weight 4796.96 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M C2/c 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' 'H' 'H' 0.0000 0.0000 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Nd' 'Nd' -0.1943 3.0179 '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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? 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 41.072(8) _cell_length_b 16.152(3) _cell_length_c 24.933(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.63(3) _cell_angle_gamma 90.00 _cell_volume 16004(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 16848 _exptl_absorpt_coefficient_mu 24.980 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.0314 _exptl_absorpt_correction_T_max 0.1890 _exptl_absorpt_process_details 'Numerical absorption correction from indexed c' _diffrn_ambient_temperature 100(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 59874 _diffrn_reflns_av_R_equivalents 0.2791 _diffrn_reflns_av_sigmaI/netI 0.2139 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.32 _reflns_number_total 17288 _reflns_number_gt 10779 _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^)+(0.1544P)^2^+9812.2217P] 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 SHELXL _refine_ls_extinction_coef 0.000070(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 17288 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1846 _refine_ls_R_factor_gt 0.1221 _refine_ls_wR_factor_ref 0.3469 _refine_ls_wR_factor_gt 0.2982 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _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 W2 W 0.02270(4) 0.56841(11) 0.40168(7) 0.0096(4) Uani 1 1 d . . . W3 W 0.09232(4) 0.59860(11) 0.53174(8) 0.0116(4) Uani 1 1 d . . . W4 W 0.15712(4) 0.72008(11) 0.52242(8) 0.0131(4) Uani 1 1 d . . . W5 W 0.15760(4) 0.81552(11) 0.38859(8) 0.0151(4) Uani 1 1 d . . . W6 W 0.09019(4) 0.77867(11) 0.27754(8) 0.0128(4) Uani 1 1 d . . . W7 W 0.03437(4) 0.76844(12) 0.47874(8) 0.0150(4) Uani 1 1 d . . . W8 W 0.09838(5) 0.89270(12) 0.46842(9) 0.0191(4) Uani 1 1 d . . . W9 W 0.03186(4) 0.85611(11) 0.35282(9) 0.0161(4) Uani 1 1 d . . . W11 W 0.06532(4) 0.46914(11) 0.25318(8) 0.0102(4) Uani 1 1 d . . . W12 W 0.06768(4) 0.37699(11) 0.37328(8) 0.0108(4) Uani 1 1 d . . . W13 W 0.13763(4) 0.41360(11) 0.49766(8) 0.0120(4) Uani 1 1 d . . . W14 W 0.20245(4) 0.53280(11) 0.48785(8) 0.0114(4) Uani 1 1 d . . . W15 W 0.20360(4) 0.63112(11) 0.35479(8) 0.0126(4) Uani 1 1 d . . . W16 W 0.13873(4) 0.59932(11) 0.24381(8) 0.0107(4) Uani 1 1 d . . . W17 W 0.15184(4) 0.28391(11) 0.38250(8) 0.0150(4) Uani 1 1 d . . . W18 W 0.21669(4) 0.40525(12) 0.37114(8) 0.0148(4) Uani 1 1 d . . . W19 W 0.15010(4) 0.37458(12) 0.25831(8) 0.0140(4) Uani 1 1 d . . . Nd Nd 0.0000 0.6565(2) 0.2500 0.0097(6) Uani 1 2 d S . . P1 P 0.0898(2) 0.6937(7) 0.4060(5) 0.008(2) Uiso 1 1 d . . . P2 P 0.1377(3) 0.4969(7) 0.3676(5) 0.010(2) Uiso 1 1 d . . . O2 O -0.0053(7) 0.5210(19) 0.4334(13) 0.013(6) Uiso 1 1 d . . . O3 O 0.0822(8) 0.562(2) 0.5893(15) 0.021(7) Uiso 1 1 d . . . O4 O 0.1908(8) 0.759(2) 0.5755(15) 0.019(7) Uiso 1 1 d . . . O5 O 0.1894(9) 0.882(2) 0.4008(16) 0.027(8) Uiso 1 1 d . . . O6 O 0.0848(8) 0.836(2) 0.2184(15) 0.024(8) Uiso 1 1 d . . . O7 O 0.0067(8) 0.780(2) 0.5196(15) 0.024(8) Uiso 1 1 d . . . O8 O 0.1147(11) 0.984(3) 0.503(2) 0.046(11) Uiso 1 1 d . . . O9 O 0.0089(7) 0.940(2) 0.3245(14) 0.017(7) Uiso 1 1 d . . . O11 O 0.0435(6) 0.4426(16) 0.1862(11) 0.002(5) Uiso 1 1 d . . . O12 O 0.0430(8) 0.302(2) 0.3902(16) 0.024(8) Uiso 1 1 d . . . O13 O 0.1341(8) 0.344(2) 0.5457(16) 0.026(8) Uiso 1 1 d . . . O14 O 0.2415(7) 0.5451(19) 0.5349(13) 0.013(6) Uiso 1 1 d . . . O15 O 0.2406(7) 0.6717(19) 0.3558(13) 0.013(6) Uiso 1 1 d . . . O16 O 0.1358(8) 0.620(2) 0.1768(15) 0.021(7) Uiso 1 1 d . . . O17 O 0.1511(10) 0.180(3) 0.3978(18) 0.036(9) Uiso 1 1 d . . . O18 O 0.2578(8) 0.379(2) 0.3796(16) 0.026(8) Uiso 1 1 d . . . O19 O 0.1525(9) 0.327(2) 0.1970(16) 0.027(8) Uiso 1 1 d . . . O2N O -0.0041(7) 0.5988(19) 0.3397(13) 0.012(6) Uiso 1 1 d . . . O6N O 0.0575(7) 0.7073(19) 0.2620(13) 0.013(6) Uiso 1 1 d . . . O9N O 0.0124(6) 0.7712(17) 0.3180(12) 0.006(5) Uiso 1 1 d . . . O11N O 0.0382(9) 0.544(3) 0.2721(18) 0.033(9) Uiso 1 1 d . . . O2P O 0.0629(6) 0.6290(16) 0.3775(11) 0.003(5) Uiso 1 1 d . . . O3P O 0.1121(7) 0.6625(18) 0.4584(12) 0.009(6) Uiso 1 1 d . . . O5P O 0.1101(7) 0.7266(18) 0.3645(13) 0.011(6) Uiso 1 1 d . . . O7P O 0.0704(8) 0.771(2) 0.4219(15) 0.024(8) Uiso 1 1 d . . . O11P O 0.1000(7) 0.4811(19) 0.3462(14) 0.015(7) Uiso 1 1 d . . . O13P O 0.1483(8) 0.506(2) 0.4296(14) 0.019(7) Uiso 1 1 d . . . O15P O 0.1481(6) 0.5740(17) 0.3374(12) 0.006(5) Uiso 1 1 d . . . O17P O 0.1563(7) 0.4192(19) 0.3524(13) 0.012(6) Uiso 1 1 d . . . O112 O 0.0525(7) 0.3819(19) 0.2940(13) 0.012(6) Uiso 1 1 d . . . O116 O 0.0967(7) 0.552(2) 0.2378(14) 0.016(7) Uiso 1 1 d . . . O119 O 0.1057(9) 0.395(2) 0.2497(17) 0.031(9) Uiso 1 1 d . . . O123 O 0.0946(7) 0.3987(19) 0.4455(14) 0.014(6) Uiso 1 1 d . . . O127 O 0.1063(7) 0.3134(18) 0.3637(12) 0.009(6) Uiso 1 1 d . . . O134 O 0.1839(7) 0.449(2) 0.5254(14) 0.018(7) Uiso 1 1 d . . . O137 O 0.1542(7) 0.334(2) 0.4525(14) 0.016(7) Uiso 1 1 d . . . O145 O 0.2070(8) 0.608(2) 0.4297(15) 0.020(7) Uiso 1 1 d . . . O148 O 0.2133(6) 0.4486(17) 0.4424(12) 0.005(5) Uiso 1 1 d . . . O156 O 0.1853(8) 0.630(2) 0.2758(14) 0.018(7) Uiso 1 1 d . . . O158 O 0.2160(7) 0.5215(19) 0.3461(14) 0.014(6) Uiso 1 1 d . . . O169 O 0.1563(8) 0.486(2) 0.2435(15) 0.019(7) Uiso 1 1 d . . . O178 O 0.2003(7) 0.3031(19) 0.3926(13) 0.012(6) Uiso 1 1 d . . . O179 O 0.1475(8) 0.274(2) 0.3053(14) 0.019(7) Uiso 1 1 d . . . O189 O 0.1999(8) 0.376(2) 0.2969(15) 0.022(7) Uiso 1 1 d . . . O212 O 0.0409(7) 0.4702(19) 0.3800(14) 0.013(6) Uiso 1 1 d . . . O230 O 0.0602(6) 0.5533(16) 0.4748(12) 0.004(5) Uiso 1 1 d . . . O270 O 0.0171(7) 0.6762(19) 0.4370(13) 0.013(6) Uiso 1 1 d . . . O313 O 0.1227(7) 0.5104(18) 0.5256(12) 0.008(6) Uiso 1 1 d . . . O340 O 0.1330(8) 0.662(2) 0.5675(16) 0.025(8) Uiso 1 1 d . . . O370 O 0.0677(8) 0.699(2) 0.5239(14) 0.018(7) Uiso 1 1 d . . . O414 O 0.1796(6) 0.6170(17) 0.5140(12) 0.007(6) Uiso 1 1 d . . . O450 O 0.1692(7) 0.7544(19) 0.4583(13) 0.012(6) Uiso 1 1 d . . . O480 O 0.1281(9) 0.814(2) 0.5137(17) 0.029(8) Uiso 1 1 d . . . O515 O 0.1792(7) 0.7267(19) 0.3604(13) 0.012(6) Uiso 1 1 d . . . O560 O 0.1331(6) 0.8446(17) 0.3206(12) 0.005(5) Uiso 1 1 d . . . O580 O 0.1292(8) 0.876(2) 0.4231(15) 0.020(7) Uiso 1 1 d . . . O616 O 0.1227(7) 0.7007(18) 0.2618(13) 0.010(6) Uiso 1 1 d . . . O690 O 0.0687(7) 0.853(2) 0.3177(14) 0.015(6) Uiso 1 1 d . . . O780 O 0.0640(8) 0.861(2) 0.5048(15) 0.022(7) Uiso 1 1 d . . . O790 O 0.0142(7) 0.8388(18) 0.4181(12) 0.009(6) Uiso 1 1 d . . . O890 O 0.0661(8) 0.932(2) 0.4064(15) 0.023(7) Uiso 1 1 d . . . K1 K 0.0673(2) 0.5830(7) 0.1269(4) 0.019(2) Uani 1 1 d . . . K2 K -0.0180(2) 0.3552(7) 0.4069(5) 0.019(2) Uani 1 1 d . . . Cl1 Cl 0.2444(3) 0.6557(8) 0.6211(5) 0.022(2) Uani 1 1 d . . . Cl2 Cl 0.0661(4) 0.7675(12) 0.0149(8) 0.050(5) Uani 1 1 d . . . Na1 Na 0.2838(6) 0.6131(14) 0.4717(12) 0.042(6) Uani 1 1 d . . . Na2 Na 0.1995(6) 1.0495(15) 0.3964(11) 0.038(5) Uiso 1 1 d . . . O901 O 0.1998(8) 0.386(2) 0.6391(15) 0.020(7) Uiso 1 1 d . . . O902 O 0.1138(11) 0.188(3) 0.125(2) 0.043(11) Uiso 1 1 d . . . O903 O 0.0517(8) 0.745(2) 0.1230(15) 0.021(7) Uiso 1 1 d . . . O904 O 0.2258(10) 0.480(3) 0.7283(19) 0.039(10) Uiso 1 1 d . . . O905 O 0.1873(9) 0.557(3) 0.6330(18) 0.034(9) Uiso 1 1 d . . . O906 O 0.0402(8) 0.609(2) 0.0037(15) 0.023(7) Uiso 1 1 d . . . O907 O 0.1952(11) 0.166(3) 0.178(2) 0.050(12) Uiso 1 1 d . . . O908 O 0.2201(12) 0.966(3) 0.311(2) 0.059(14) Uiso 1 1 d . . . O909 O 0.2358(12) 0.301(3) 0.232(2) 0.052(12) Uiso 1 1 d . . . O910 O -0.0673(13) 0.266(4) 0.334(2) 0.064(15) Uiso 1 1 d . . . O911 O 0.1092(14) 0.853(4) -0.028(3) 0.074(17) Uiso 1 1 d . . . O912 O 0.2233(15) 0.289(4) 0.523(3) 0.082(18) Uiso 1 1 d . . . O913 O -0.0371(17) 1.033(5) 0.242(3) 0.09(2) Uiso 1 1 d . . . O914 O 0.0427(15) 0.917(4) 0.047(3) 0.078(18) Uiso 1 1 d . . . O915 O 0.1622(17) 0.888(5) 0.223(3) 0.09(2) Uiso 1 1 d . . . O916 O 0.051(2) 0.928(6) 0.606(4) 0.12(3) Uiso 1 1 d . . . O917 O 0.0255(19) 1.072(5) 0.444(4) 0.11(3) Uiso 1 1 d . . . O918 O 0.118(2) 1.018(6) 0.326(4) 0.14(3) Uiso 1 1 d . . . O919 O 0.0779(19) 0.197(5) 0.266(4) 0.11(2) Uiso 1 1 d . . . O920 O 0.2500 0.7500 0.5000 0.046(16) Uiso 1 2 d S . . O921 O 0.0000 2.272(6) 0.2500 0.08(3) Uiso 1 2 d S . . 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 W2 0.0030(7) 0.0156(9) 0.0081(9) 0.0010(7) -0.0024(6) 0.0006(6) W3 0.0061(7) 0.0175(9) 0.0090(9) -0.0016(7) -0.0022(6) 0.0016(6) W4 0.0077(7) 0.0135(9) 0.0132(10) -0.0055(8) -0.0064(7) 0.0000(6) W5 0.0087(7) 0.0121(8) 0.0182(10) -0.0003(8) -0.0084(7) -0.0028(7) W6 0.0072(7) 0.0119(8) 0.0149(10) 0.0009(7) -0.0052(7) -0.0015(6) W7 0.0115(8) 0.0166(9) 0.0141(10) -0.0043(8) -0.0023(7) 0.0067(7) W8 0.0176(8) 0.0106(9) 0.0230(11) -0.0057(8) -0.0057(8) 0.0027(7) W9 0.0132(8) 0.0104(8) 0.0191(10) -0.0035(8) -0.0061(7) 0.0047(7) W11 0.0055(7) 0.0133(8) 0.0102(9) 0.0006(7) -0.0014(6) -0.0004(6) W12 0.0089(7) 0.0107(8) 0.0116(9) 0.0013(7) 0.0002(7) -0.0005(6) W13 0.0096(7) 0.0132(9) 0.0107(9) 0.0009(7) -0.0020(7) 0.0021(6) W14 0.0056(7) 0.0142(9) 0.0110(9) 0.0003(7) -0.0040(6) 0.0018(6) W15 0.0044(7) 0.0167(9) 0.0141(9) 0.0012(8) -0.0027(7) -0.0016(6) W16 0.0045(7) 0.0157(9) 0.0091(9) 0.0027(7) -0.0036(6) -0.0012(6) W17 0.0177(8) 0.0088(8) 0.0169(10) 0.0016(7) 0.0010(8) 0.0051(7) W18 0.0097(7) 0.0182(9) 0.0152(10) 0.0010(8) 0.0011(7) 0.0071(7) W19 0.0124(8) 0.0147(9) 0.0133(10) -0.0015(8) 0.0005(7) 0.0059(7) Nd 0.0025(12) 0.0142(16) 0.0096(16) 0.000 -0.0036(12) 0.000 K1 0.011(4) 0.030(6) 0.011(5) 0.002(4) -0.007(4) 0.005(4) K2 0.009(4) 0.031(6) 0.020(6) -0.005(5) 0.005(4) 0.001(4) Cl1 0.020(5) 0.021(6) 0.022(6) 0.000(5) 0.001(5) 0.000(5) Cl2 0.039(8) 0.058(11) 0.059(12) -0.015(9) 0.022(8) -0.029(8) Na1 0.033(12) 0.027(12) 0.062(19) 0.007(12) 0.005(12) -0.016(10)