# # Title: # High-Temperature, High-Pressure Hydrothermal Synthesis, Crystal Structure, and # Solid-State NMR Spectroscopy of Cs2(UO2)(Si2O6) and Variable-Temperature Powder # X-ray Diffraction Study of the Hydrate Phase Cs2(UO2)(Si2O6).0.5H2O # # Authors: # Chih-Shan Chen, Ray-Kuang Chiang, and Kwang-Hwa Lii # E-mail: liikh@cc.ncu.edu.tw # data_csu16 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Cs2(UO2)(Si2O6) _chemical_formula_sum 'Cs2 O8 Si2 U' _chemical_formula_weight 688.03 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M Ibca (No. 73) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' _cell_length_a 15.1372(10) _cell_length_b 15.2949(10) _cell_length_c 16.4010(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3797.2(8) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polygon _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.22 mm _exptl_crystal_size_mid 0.20 mm _exptl_crystal_size_min 0.12 mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 24.919 _exptl_absorpt_correction_type SADABS program (All reflections with I>5sigma are used to create an absorption curve by trying to make equivalent reflections have the same intensity.) _exptl_absorpt_correction_T_min 0.329 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details ? _exptl_special_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 Siemens Smart CCD _diffrn_measurement_method omega scans with narrow frames _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11278 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2279 _reflns_number_gt 2036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0147P)^2^+167.3439P] 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 0.000572(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2279 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.285 _refine_ls_restrained_S_all 1.285 _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 Cs1 Cs -0.10478(6) -0.5000 -0.2500 0.01781(19) Uani 1 2 d S . . Cs2 Cs -0.2500 -0.63015(7) -0.5000 0.0246(2) Uani 1 2 d S . . Cs3 Cs 0.0000 -0.2500 -0.35022(6) 0.0296(3) Uani 1 2 d S . . Cs4 Cs 0.0000 -0.7500 -0.40110(6) 0.0280(2) Uani 1 2 d S . . U1 U -0.2500 -0.2500 -0.2500 0.00981(13) Uani 1 2 d S . . U2 U 0.0000 -0.5000 -0.5000 0.00638(13) Uani 1 2 d S . . Si1 Si -0.37082(15) -0.43047(15) -0.32275(14) 0.0086(4) Uani 1 1 d . . . Si2 Si -0.20527(15) -0.39025(15) -0.41700(14) 0.0094(5) Uani 1 1 d . . . O1 O -0.3826(7) -0.5000 -0.2500 0.035(3) Uani 1 2 d S . . O2 O -0.2786(4) -0.4521(4) -0.3707(4) 0.0139(13) Uani 1 1 d . . . O3 O -0.4538(4) -0.4411(4) -0.3828(4) 0.0136(13) Uani 1 1 d . . . O4 O -0.3667(4) -0.3328(5) -0.2852(4) 0.0180(14) Uani 1 1 d . . . O5 O -0.2500 -0.3493(6) -0.5000 0.020(2) Uani 1 2 d S . . O6 O -0.1222(4) -0.4510(5) -0.4382(4) 0.0214(15) Uani 1 1 d . . . O7 O -0.1822(5) -0.3084(5) -0.3583(4) 0.0242(16) Uani 1 1 d . . . O8 O 0.0539(5) -0.3965(4) -0.4771(4) 0.0163(13) Uani 1 1 d . . . O9 O -0.2016(5) -0.3352(5) -0.1876(4) 0.0253(16) Uani 1 1 d . . . 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 Cs1 0.0160(4) 0.0229(4) 0.0146(4) 0.0033(3) 0.000 0.000 Cs2 0.0124(4) 0.0298(5) 0.0315(5) 0.000 -0.0012(4) 0.000 Cs3 0.0091(4) 0.0547(6) 0.0249(5) 0.000 0.000 -0.0077(4) Cs4 0.0484(6) 0.0134(4) 0.0221(5) 0.000 0.000 -0.0088(4) U1 0.0056(2) 0.0135(2) 0.0104(2) -0.00461(17) -0.00019(17) -0.00098(16) U2 0.0024(2) 0.0094(2) 0.0073(2) -0.00003(15) -0.00004(15) 0.00108(15) Si1 0.0050(10) 0.0143(11) 0.0065(10) -0.0002(8) 0.0007(8) -0.0019(9) Si2 0.0041(10) 0.0151(11) 0.0088(10) -0.0021(8) 0.0008(9) 0.0010(9) O1 0.015(5) 0.055(8) 0.034(6) 0.023(6) 0.000 0.000 O2 0.008(3) 0.014(3) 0.020(3) 0.003(2) 0.004(3) 0.000(2) O3 0.011(3) 0.019(3) 0.011(3) -0.002(2) -0.005(2) 0.001(3) O4 0.011(3) 0.025(3) 0.018(3) -0.010(3) 0.002(3) -0.004(3) O5 0.017(5) 0.014(4) 0.028(5) 0.000 -0.007(4) 0.000 O6 0.009(3) 0.035(4) 0.020(3) 0.000(3) 0.002(3) 0.010(3) O7 0.014(3) 0.039(4) 0.019(3) -0.014(3) 0.001(3) -0.010(3) O8 0.018(3) 0.011(3) 0.019(3) -0.001(2) -0.006(3) -0.004(3) O9 0.036(4) 0.021(3) 0.019(3) 0.002(3) -0.006(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cs1 O9 3.089(7) 8_434 ? Cs1 O9 3.089(7) . ? Cs1 O6 3.188(7) 8_434 ? Cs1 O6 3.188(7) . ? Cs1 O3 3.283(6) 10_655 ? Cs1 O3 3.283(6) 15_545 ? Cs1 O1 3.363(11) 10_655 ? Cs1 O2 3.373(7) . ? Cs1 O2 3.373(7) 8_434 ? Cs1 Si2 3.554(2) . ? Cs1 Si2 3.554(2) 8_434 ? Cs1 O7 3.622(8) 8_434 ? Cs2 O8 3.019(7) 9_544 ? Cs2 O8 3.019(7) 15_445 ? Cs2 O9 3.208(7) 2_444 ? Cs2 O9 3.208(7) 8_434 ? Cs2 O5 3.351(10) 14_544 ? Cs2 O2 3.479(6) . ? Cs2 O2 3.479(6) 7_443 ? Cs2 O6 3.504(8) . ? Cs2 O6 3.504(8) 7_443 ? Cs2 O7 3.726(8) 14_544 ? Cs2 O7 3.726(8) 12 ? Cs2 Si2 3.972(3) . ? Cs3 O7 2.901(7) . ? Cs3 O7 2.901(7) 6_444 ? Cs3 O8 3.165(7) . ? Cs3 O8 3.165(6) 6_444 ? Cs3 O4 3.258(6) 10_655 ? Cs3 O4 3.258(6) 13_444 ? Cs3 Si2 3.931(2) . ? Cs3 Si2 3.931(2) 6_444 ? Cs3 Cs4 4.0785(15) 9_544 ? Cs3 Cs4 4.1220(15) 3_554 ? Cs3 U1 4.1259(5) 6_444 ? Cs3 U1 4.1259(5) . ? Cs4 O3 3.020(6) 15_545 ? Cs4 O3 3.020(6) 12 ? Cs4 O4 3.048(7) 15_545 ? Cs4 O4 3.048(7) 12 ? Cs4 O8 3.111(6) 14_544 ? Cs4 O8 3.111(6) 9_544 ? Cs4 Si1 3.619(2) 15_545 ? Cs4 Si1 3.619(2) 12 ? Cs4 O9 3.623(8) 3_544 ? Cs4 O9 3.623(8) 8_434 ? Cs4 Cs3 4.0785(15) 9_544 ? Cs4 Cs3 4.1220(15) 3_544 ? U1 O9 1.812(7) . ? U1 O9 1.812(7) 13_444 ? U1 O7 2.238(7) . ? U1 O7 2.238(7) 13_444 ? U1 O4 2.249(6) . ? U1 O4 2.249(6) 13_444 ? U1 Cs3 4.1259(5) 13_444 ? U1 Cs1 4.4106(5) 13_444 ? U1 Cs2 4.4914(5) 14_554 ? U1 Cs2 4.4914(5) 2_445 ? U2 O8 1.820(6) 9_544 ? U2 O8 1.820(6) . ? U2 O3 2.235(6) 15_545 ? U2 O3 2.235(6) 7_443 ? U2 O6 2.239(6) . ? U2 O6 2.239(6) 9_544 ? U2 Cs4 4.1535(5) 9_544 ? U2 Cs2 4.2759(5) 9_544 ? U2 Cs1 4.3963(4) 9_544 ? Si1 O3 1.604(6) . ? Si1 O1 1.608(3) . ? Si1 O4 1.617(7) . ? Si1 O2 1.635(7) . ? Si1 Cs4 3.619(2) 15_445 ? Si1 Cs1 3.885(2) 10 ? Si2 O6 1.601(7) . ? Si2 O7 1.618(7) . ? Si2 O5 1.645(4) . ? Si2 O2 1.645(7) . ? Si2 Cs2 4.259(3) 14_554 ? O1 Si1 1.608(3) 8_434 ? O1 Cs1 3.363(11) 10 ? O3 U2 2.235(6) 7_443 ? O3 Cs4 3.020(6) 15_445 ? O3 Cs1 3.283(6) 10 ? O4 Cs4 3.048(7) 15_445 ? O4 Cs3 3.258(6) 13_444 ? O5 Si2 1.645(4) 7_443 ? O5 Cs2 3.351(10) 14_554 ? O7 Cs2 3.726(8) 14_554 ? O8 Cs2 3.019(7) 9_544 ? O8 Cs4 3.111(6) 9_544 ? O9 Cs2 3.208(7) 2_445 ? O9 Cs4 3.623(8) 3_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Cs1 O9 123.4(3) 8_434 . ? O9 Cs1 O6 95.12(18) 8_434 8_434 ? O9 Cs1 O6 80.33(19) . 8_434 ? O9 Cs1 O6 80.33(19) 8_434 . ? O9 Cs1 O6 95.12(18) . . ? O6 Cs1 O6 170.5(2) 8_434 . ? O9 Cs1 O3 140.69(18) 8_434 10_655 ? O9 Cs1 O3 83.49(18) . 10_655 ? O6 Cs1 O3 58.66(16) 8_434 10_655 ? O6 Cs1 O3 129.46(17) . 10_655 ? O9 Cs1 O3 83.49(18) 8_434 15_545 ? O9 Cs1 O3 140.69(18) . 15_545 ? O6 Cs1 O3 129.46(17) 8_434 15_545 ? O6 Cs1 O3 58.66(16) . 15_545 ? O3 Cs1 O3 91.8(2) 10_655 15_545 ? O9 Cs1 O1 118.31(15) 8_434 10_655 ? O9 Cs1 O1 118.31(15) . 10_655 ? O6 Cs1 O1 94.76(12) 8_434 10_655 ? O6 Cs1 O1 94.76(12) . 10_655 ? O3 Cs1 O1 45.89(11) 10_655 10_655 ? O3 Cs1 O1 45.89(11) 15_545 10_655 ? O9 Cs1 O2 67.22(18) 8_434 . ? O9 Cs1 O2 69.34(18) . . ? O6 Cs1 O2 123.67(16) 8_434 . ? O6 Cs1 O2 46.85(16) . . ? O3 Cs1 O2 150.77(15) 10_655 . ? O3 Cs1 O2 102.32(15) 15_545 . ? O1 Cs1 O2 141.28(11) 10_655 . ? O9 Cs1 O2 69.34(18) 8_434 8_434 ? O9 Cs1 O2 67.22(18) . 8_434 ? O6 Cs1 O2 46.85(16) 8_434 8_434 ? O6 Cs1 O2 123.67(16) . 8_434 ? O3 Cs1 O2 102.32(15) 10_655 8_434 ? O3 Cs1 O2 150.77(16) 15_545 8_434 ? O1 Cs1 O2 141.28(11) 10_655 8_434 ? O2 Cs1 O2 77.4(2) . 8_434 ? O9 Cs1 Si2 85.82(14) 8_434 . ? O9 Cs1 Si2 70.54(14) . . ? O6 Cs1 Si2 145.27(13) 8_434 . ? O6 Cs1 Si2 26.77(12) . . ? O3 Cs1 Si2 132.80(12) 10_655 . ? O3 Cs1 Si2 85.20(11) 15_545 . ? O1 Cs1 Si2 115.34(4) 10_655 . ? O2 Cs1 Si2 27.32(11) . . ? O2 Cs1 Si2 102.75(11) 8_434 . ? O9 Cs1 Si2 70.54(14) 8_434 8_434 ? O9 Cs1 Si2 85.83(14) . 8_434 ? O6 Cs1 Si2 26.77(12) 8_434 8_434 ? O6 Cs1 Si2 145.27(13) . 8_434 ? O3 Cs1 Si2 85.20(11) 10_655 8_434 ? O3 Cs1 Si2 132.80(12) 15_545 8_434 ? O1 Cs1 Si2 115.34(4) 10_655 8_434 ? O2 Cs1 Si2 102.75(12) . 8_434 ? O2 Cs1 Si2 27.32(11) 8_434 8_434 ? Si2 Cs1 Si2 129.32(8) . 8_434 ? O9 Cs1 O7 49.37(17) 8_434 8_434 ? O9 Cs1 O7 110.14(18) . 8_434 ? O6 Cs1 O7 46.19(17) 8_434 8_434 ? O6 Cs1 O7 129.69(18) . 8_434 ? O3 Cs1 O7 97.00(15) 10_655 8_434 ? O3 Cs1 O7 109.17(15) 15_545 8_434 ? O1 Cs1 O7 108.87(11) 10_655 8_434 ? O2 Cs1 O7 102.18(15) . 8_434 ? O2 Cs1 O7 44.30(15) 8_434 8_434 ? Si2 Cs1 O7 128.44(12) . 8_434 ? Si2 Cs1 O7 26.03(11) 8_434 8_434 ? O8 Cs2 O8 164.5(2) 9_544 15_445 ? O8 Cs2 O9 97.33(19) 9_544 2_444 ? O8 Cs2 O9 85.24(19) 15_445 2_444 ? O8 Cs2 O9 85.24(19) 9_544 8_434 ? O8 Cs2 O9 97.33(19) 15_445 8_434 ? O9 Cs2 O9 161.0(3) 2_444 8_434 ? O8 Cs2 O5 97.77(12) 9_544 14_544 ? O8 Cs2 O5 97.77(12) 15_445 14_544 ? O9 Cs2 O5 80.50(13) 2_444 14_544 ? O9 Cs2 O5 80.50(13) 8_434 14_544 ? O8 Cs2 O2 95.32(16) 9_544 . ? O8 Cs2 O2 72.29(16) 15_445 . ? O9 Cs2 O2 133.29(17) 2_444 . ? O9 Cs2 O2 64.70(16) 8_434 . ? O5 Cs2 O2 141.51(10) 14_544 . ? O8 Cs2 O2 72.29(16) 9_544 7_443 ? O8 Cs2 O2 95.32(16) 15_445 7_443 ? O9 Cs2 O2 64.70(16) 2_444 7_443 ? O9 Cs2 O2 133.29(17) 8_434 7_443 ? O5 Cs2 O2 141.51(10) 14_544 7_443 ? O2 Cs2 O2 77.0(2) . 7_443 ? O8 Cs2 O6 52.25(16) 9_544 . ? O8 Cs2 O6 113.63(16) 15_445 . ? O9 Cs2 O6 122.19(18) 2_444 . ? O9 Cs2 O6 74.07(17) 8_434 . ? O5 Cs2 O6 141.46(11) 14_544 . ? O2 Cs2 O6 43.97(15) . . ? O2 Cs2 O6 59.69(16) 7_443 . ? O8 Cs2 O6 113.63(16) 9_544 7_443 ? O8 Cs2 O6 52.25(16) 15_445 7_443 ? O9 Cs2 O6 74.07(17) 2_444 7_443 ? O9 Cs2 O6 122.19(18) 8_434 7_443 ? O5 Cs2 O6 141.46(11) 14_544 7_443 ? O2 Cs2 O6 59.69(16) . 7_443 ? O2 Cs2 O6 43.97(15) 7_443 7_443 ? O6 Cs2 O6 77.1(2) . 7_443 ? O8 Cs2 O7 75.54(16) 9_544 14_544 ? O8 Cs2 O7 116.57(16) 15_445 14_544 ? O9 Cs2 O7 49.00(17) 2_444 14_544 ? O9 Cs2 O7 114.49(17) 8_434 14_544 ? O5 Cs2 O7 42.98(10) 14_544 14_544 ? O2 Cs2 O7 170.83(15) . 14_544 ? O2 Cs2 O7 99.09(15) 7_443 14_544 ? O6 Cs2 O7 126.90(15) . 14_544 ? O6 Cs2 O7 122.95(16) 7_443 14_544 ? O8 Cs2 O7 116.57(16) 9_544 12 ? O8 Cs2 O7 75.54(16) 15_445 12 ? O9 Cs2 O7 114.49(17) 2_444 12 ? O9 Cs2 O7 49.00(17) 8_434 12 ? O5 Cs2 O7 42.98(11) 14_544 12 ? O2 Cs2 O7 99.09(15) . 12 ? O2 Cs2 O7 170.83(15) 7_443 12 ? O6 Cs2 O7 122.95(16) . 12 ? O6 Cs2 O7 126.90(15) 7_443 12 ? O7 Cs2 O7 86.0(2) 14_544 12 ? O8 Cs2 Si2 75.54(12) 9_544 . ? O8 Cs2 Si2 90.01(12) 15_445 . ? O9 Cs2 Si2 121.35(13) 2_444 . ? O9 Cs2 Si2 77.57(13) 8_434 . ? O5 Cs2 Si2 157.49(3) 14_544 . ? O2 Cs2 Si2 24.38(11) . . ? O2 Cs2 Si2 57.63(11) 7_443 . ? O6 Cs2 Si2 23.68(11) . . ? O6 Cs2 Si2 58.04(12) 7_443 . ? O7 Cs2 Si2 147.41(11) 14_544 . ? O7 Cs2 Si2 120.60(11) 12 . ? O7 Cs3 O7 174.8(3) . 6_444 ? O7 Cs3 O8 89.83(19) . . ? O7 Cs3 O8 86.7(2) 6_444 . ? O7 Cs3 O8 86.7(2) . 6_444 ? O7 Cs3 O8 89.83(19) 6_444 6_444 ? O8 Cs3 O8 97.8(2) . 6_444 ? O7 Cs3 O4 120.0(2) . 10_655 ? O7 Cs3 O4 64.03(18) 6_444 10_655 ? O8 Cs3 O4 90.76(17) . 10_655 ? O8 Cs3 O4 152.04(17) 6_444 10_655 ? O7 Cs3 O4 64.03(18) . 13_444 ? O7 Cs3 O4 120.0(2) 6_444 13_444 ? O8 Cs3 O4 152.04(17) . 13_444 ? O8 Cs3 O4 90.76(17) 6_444 13_444 ? O4 Cs3 O4 94.0(2) 10_655 13_444 ? O7 Cs3 Si2 21.28(14) . . ? O7 Cs3 Si2 155.00(17) 6_444 . ? O8 Cs3 Si2 68.55(13) . . ? O8 Cs3 Si2 89.97(13) 6_444 . ? O4 Cs3 Si2 117.88(12) 10_655 . ? O4 Cs3 Si2 84.98(12) 13_444 . ? O7 Cs3 Si2 155.00(17) . 6_444 ? O7 Cs3 Si2 21.28(14) 6_444 6_444 ? O8 Cs3 Si2 89.97(13) . 6_444 ? O8 Cs3 Si2 68.55(13) 6_444 6_444 ? O4 Cs3 Si2 84.98(12) 10_655 6_444 ? O4 Cs3 Si2 117.88(12) 13_444 6_444 ? Si2 Cs3 Si2 147.65(7) . 6_444 ? O7 Cs3 Cs4 87.38(14) . 9_544 ? O7 Cs3 Cs4 87.38(14) 6_444 9_544 ? O8 Cs3 Cs4 48.90(12) . 9_544 ? O8 Cs3 Cs4 48.90(12) 6_444 9_544 ? O4 Cs3 Cs4 133.00(12) 10_655 9_544 ? O4 Cs3 Cs4 133.00(12) 13_444 9_544 ? Si2 Cs3 Cs4 73.82(4) . 9_544 ? Si2 Cs3 Cs4 73.82(4) 6_444 9_544 ? O7 Cs3 Cs4 92.62(14) . 3_554 ? O7 Cs3 Cs4 92.62(14) 6_444 3_554 ? O8 Cs3 Cs4 131.10(12) . 3_554 ? O8 Cs3 Cs4 131.10(12) 6_444 3_554 ? O4 Cs3 Cs4 47.00(12) 10_655 3_554 ? O4 Cs3 Cs4 47.00(12) 13_444 3_554 ? Si2 Cs3 Cs4 106.18(4) . 3_554 ? Si2 Cs3 Cs4 106.18(4) 6_444 3_554 ? Cs4 Cs3 Cs4 180.0 9_544 3_554 ? O7 Cs3 U1 152.86(16) . 6_444 ? O7 Cs3 U1 31.41(14) 6_444 6_444 ? O8 Cs3 U1 91.45(12) . 6_444 ? O8 Cs3 U1 119.90(12) 6_444 6_444 ? O4 Cs3 U1 32.87(11) 10_655 6_444 ? O4 Cs3 U1 107.25(12) 13_444 6_444 ? Si2 Cs3 U1 146.71(3) . 6_444 ? Si2 Cs3 U1 52.13(3) 6_444 6_444 ? Cs4 Cs3 U1 113.478(14) 9_544 6_444 ? Cs4 Cs3 U1 66.522(14) 3_554 6_444 ? O7 Cs3 U1 31.41(14) . . ? O7 Cs3 U1 152.86(16) 6_444 . ? O8 Cs3 U1 119.90(12) . . ? O8 Cs3 U1 91.45(12) 6_444 . ? O4 Cs3 U1 107.25(12) 10_655 . ? O4 Cs3 U1 32.87(11) 13_444 . ? Si2 Cs3 U1 52.13(3) . . ? Si2 Cs3 U1 146.71(3) 6_444 . ? Cs4 Cs3 U1 113.478(14) 9_544 . ? Cs4 Cs3 U1 66.522(14) 3_554 . ? U1 Cs3 U1 133.04(3) 6_444 . ? O3 Cs4 O3 168.6(2) 15_545 12 ? O3 Cs4 O4 51.87(17) 15_545 15_545 ? O3 Cs4 O4 119.57(17) 12 15_545 ? O3 Cs4 O4 119.57(17) 15_545 12 ? O3 Cs4 O4 51.87(17) 12 12 ? O4 Cs4 O4 102.8(2) 15_545 12 ? O3 Cs4 O8 134.44(17) 15_545 14_544 ? O3 Cs4 O8 55.07(16) 12 14_544 ? O4 Cs4 O8 121.73(18) 15_545 14_544 ? O4 Cs4 O8 105.95(17) 12 14_544 ? O3 Cs4 O8 55.07(16) 15_545 9_544 ? O3 Cs4 O8 134.44(17) 12 9_544 ? O4 Cs4 O8 105.95(17) 15_545 9_544 ? O4 Cs4 O8 121.73(18) 12 9_544 ? O8 Cs4 O8 100.1(2) 14_544 9_544 ? O3 Cs4 Si1 26.02(12) 15_545 15_545 ? O3 Cs4 Si1 145.90(13) 12 15_545 ? O4 Cs4 Si1 26.33(13) 15_545 15_545 ? O4 Cs4 Si1 116.96(13) 12 15_545 ? O8 Cs4 Si1 129.48(13) 14_544 15_545 ? O8 Cs4 Si1 79.65(12) 9_544 15_545 ? O3 Cs4 Si1 145.90(13) 15_545 12 ? O3 Cs4 Si1 26.02(12) 12 12 ? O4 Cs4 Si1 116.96(13) 15_545 12 ? O4 Cs4 Si1 26.33(13) 12 12 ? O8 Cs4 Si1 79.65(12) 14_544 12 ? O8 Cs4 Si1 129.48(13) 9_544 12 ? Si1 Cs4 Si1 138.40(8) 15_545 12 ? O3 Cs4 O9 96.50(16) 15_545 3_544 ? O3 Cs4 O9 78.87(17) 12 3_544 ? O4 Cs4 O9 48.80(17) 15_545 3_544 ? O4 Cs4 O9 99.07(17) 12 3_544 ? O8 Cs4 O9 77.16(17) 14_544 3_544 ? O8 Cs4 O9 137.57(18) 9_544 3_544 ? Si1 Cs4 O9 71.14(12) 15_545 3_544 ? Si1 Cs4 O9 92.17(12) 12 3_544 ? O3 Cs4 O9 78.87(17) 15_545 8_434 ? O3 Cs4 O9 96.50(16) 12 8_434 ? O4 Cs4 O9 99.07(17) 15_545 8_434 ? O4 Cs4 O9 48.80(17) 12 8_434 ? O8 Cs4 O9 137.57(18) 14_544 8_434 ? O8 Cs4 O9 77.16(17) 9_544 8_434 ? Si1 Cs4 O9 92.17(12) 15_545 8_434 ? Si1 Cs4 O9 71.14(12) 12 8_434 ? O9 Cs4 O9 132.6(2) 3_544 8_434 ? O3 Cs4 Cs3 95.70(12) 15_545 9_544 ? O3 Cs4 Cs3 95.70(12) 12 9_544 ? O4 Cs4 Cs3 128.58(12) 15_545 9_544 ? O4 Cs4 Cs3 128.58(12) 12 9_544 ? O8 Cs4 Cs3 50.05(12) 14_544 9_544 ? O8 Cs4 Cs3 50.05(12) 9_544 9_544 ? Si1 Cs4 Cs3 110.80(4) 15_545 9_544 ? Si1 Cs4 Cs3 110.80(4) 12 9_544 ? O9 Cs4 Cs3 113.69(12) 3_544 9_544 ? O9 Cs4 Cs3 113.69(12) 8_434 9_544 ? O3 Cs4 Cs3 84.30(12) 15_545 3_544 ? O3 Cs4 Cs3 84.30(12) 12 3_544 ? O4 Cs4 Cs3 51.42(12) 15_545 3_544 ? O4 Cs4 Cs3 51.42(12) 12 3_544 ? O8 Cs4 Cs3 129.95(12) 14_544 3_544 ? O8 Cs4 Cs3 129.95(12) 9_544 3_544 ? Si1 Cs4 Cs3 69.20(4) 15_545 3_544 ? Si1 Cs4 Cs3 69.20(4) 12 3_544 ? O9 Cs4 Cs3 66.31(12) 3_544 3_544 ? O9 Cs4 Cs3 66.31(12) 8_434 3_544 ? Cs3 Cs4 Cs3 180.0 9_544 3_544 ? O9 U1 O9 180.0(4) . 13_444 ? O9 U1 O7 88.6(3) . . ? O9 U1 O7 91.4(3) 13_444 . ? O9 U1 O7 91.4(3) . 13_444 ? O9 U1 O7 88.6(3) 13_444 13_444 ? O7 U1 O7 180.0(2) . 13_444 ? O9 U1 O4 93.3(3) . . ? O9 U1 O4 86.7(3) 13_444 . ? O7 U1 O4 86.1(2) . . ? O7 U1 O4 93.9(2) 13_444 . ? O9 U1 O4 86.7(3) . 13_444 ? O9 U1 O4 93.3(3) 13_444 13_444 ? O7 U1 O4 93.9(2) . 13_444 ? O7 U1 O4 86.1(2) 13_444 13_444 ? O4 U1 O4 180.0(3) . 13_444 ? O9 U1 Cs3 98.4(3) . 13_444 ? O9 U1 Cs3 81.6(3) 13_444 13_444 ? O7 U1 Cs3 137.49(17) . 13_444 ? O7 U1 Cs3 42.51(17) 13_444 13_444 ? O4 U1 Cs3 51.83(16) . 13_444 ? O4 U1 Cs3 128.17(16) 13_444 13_444 ? O9 U1 Cs3 81.6(3) . . ? O9 U1 Cs3 98.4(3) 13_444 . ? O7 U1 Cs3 42.51(17) . . ? O7 U1 Cs3 137.49(17) 13_444 . ? O4 U1 Cs3 128.17(16) . . ? O4 U1 Cs3 51.83(16) 13_444 . ? Cs3 U1 Cs3 180.0 13_444 . ? O9 U1 Cs1 34.4(2) . . ? O9 U1 Cs1 145.6(2) 13_444 . ? O7 U1 Cs1 54.9(2) . . ? O7 U1 Cs1 125.1(2) 13_444 . ? O4 U1 Cs1 84.45(18) . . ? O4 U1 Cs1 95.55(18) 13_444 . ? Cs3 U1 Cs1 117.203(10) 13_444 . ? Cs3 U1 Cs1 62.797(10) . . ? O9 U1 Cs1 145.6(2) . 13_444 ? O9 U1 Cs1 34.4(2) 13_444 13_444 ? O7 U1 Cs1 125.1(2) . 13_444 ? O7 U1 Cs1 54.9(2) 13_444 13_444 ? O4 U1 Cs1 95.55(18) . 13_444 ? O4 U1 Cs1 84.45(18) 13_444 13_444 ? Cs3 U1 Cs1 62.797(10) 13_444 13_444 ? Cs3 U1 Cs1 117.203(10) . 13_444 ? Cs1 U1 Cs1 180.0 . 13_444 ? O9 U1 Cs2 144.0(2) . 14_554 ? O9 U1 Cs2 36.0(2) 13_444 14_554 ? O7 U1 Cs2 55.8(2) . 14_554 ? O7 U1 Cs2 124.2(2) 13_444 14_554 ? O4 U1 Cs2 89.72(18) . 14_554 ? O4 U1 Cs2 90.28(18) 13_444 14_554 ? Cs3 U1 Cs2 111.328(12) 13_444 14_554 ? Cs3 U1 Cs2 68.672(12) . 14_554 ? Cs1 U1 Cs2 110.722(11) . 14_554 ? Cs1 U1 Cs2 69.278(11) 13_444 14_554 ? O9 U1 Cs2 36.0(2) . 2_445 ? O9 U1 Cs2 144.0(2) 13_444 2_445 ? O7 U1 Cs2 124.2(2) . 2_445 ? O7 U1 Cs2 55.8(2) 13_444 2_445 ? O4 U1 Cs2 90.28(18) . 2_445 ? O4 U1 Cs2 89.72(18) 13_444 2_445 ? Cs3 U1 Cs2 68.672(12) 13_444 2_445 ? Cs3 U1 Cs2 111.328(12) . 2_445 ? Cs1 U1 Cs2 69.278(11) . 2_445 ? Cs1 U1 Cs2 110.722(11) 13_444 2_445 ? Cs2 U1 Cs2 180.0 14_554 2_445 ? O8 U2 O8 180.000(1) 9_544 . ? O8 U2 O3 88.1(3) 9_544 15_545 ? O8 U2 O3 91.9(3) . 15_545 ? O8 U2 O3 91.9(3) 9_544 7_443 ? O8 U2 O3 88.1(3) . 7_443 ? O3 U2 O3 180.00(16) 15_545 7_443 ? O8 U2 O6 90.8(3) 9_544 . ? O8 U2 O6 89.2(3) . . ? O3 U2 O6 90.3(2) 15_545 . ? O3 U2 O6 89.7(2) 7_443 . ? O8 U2 O6 89.2(3) 9_544 9_544 ? O8 U2 O6 90.8(3) . 9_544 ? O3 U2 O6 89.7(2) 15_545 9_544 ? O3 U2 O6 90.3(2) 7_443 9_544 ? O6 U2 O6 180.000(1) . 9_544 ? O8 U2 Cs4 44.0(2) 9_544 . ? O8 U2 Cs4 136.0(2) . . ? O3 U2 Cs4 45.00(17) 15_545 . ? O3 U2 Cs4 135.00(17) 7_443 . ? O6 U2 Cs4 97.57(19) . . ? O6 U2 Cs4 82.43(19) 9_544 . ? O8 U2 Cs4 136.0(2) 9_544 9_544 ? O8 U2 Cs4 44.0(2) . 9_544 ? O3 U2 Cs4 135.00(17) 15_545 9_544 ? O3 U2 Cs4 45.00(17) 7_443 9_544 ? O6 U2 Cs4 82.43(19) . 9_544 ? O6 U2 Cs4 97.57(19) 9_544 9_544 ? Cs4 U2 Cs4 180.0 . 9_544 ? O8 U2 Cs2 143.3(2) 9_544 9_544 ? O8 U2 Cs2 36.7(2) . 9_544 ? O3 U2 Cs2 84.88(16) 15_545 9_544 ? O3 U2 Cs2 95.12(16) 7_443 9_544 ? O6 U2 Cs2 125.13(19) . 9_544 ? O6 U2 Cs2 54.87(19) 9_544 9_544 ? Cs4 U2 Cs2 115.377(12) . 9_544 ? Cs4 U2 Cs2 64.623(12) 9_544 9_544 ? O8 U2 Cs2 36.7(2) 9_544 . ? O8 U2 Cs2 143.3(2) . . ? O3 U2 Cs2 95.12(16) 15_545 . ? O3 U2 Cs2 84.88(16) 7_443 . ? O6 U2 Cs2 54.87(19) . . ? O6 U2 Cs2 125.13(19) 9_544 . ? Cs4 U2 Cs2 64.623(12) . . ? Cs4 U2 Cs2 115.377(12) 9_544 . ? Cs2 U2 Cs2 180.00(2) 9_544 . ? O8 U2 Cs1 88.2(2) 9_544 9_544 ? O8 U2 Cs1 91.8(2) . 9_544 ? O3 U2 Cs1 133.56(17) 15_545 9_544 ? O3 U2 Cs1 46.44(17) 7_443 9_544 ? O6 U2 Cs1 136.07(18) . 9_544 ? O6 U2 Cs1 43.93(18) 9_544 9_544 ? Cs4 U2 Cs1 111.359(12) . 9_544 ? Cs4 U2 Cs1 68.641(12) 9_544 9_544 ? Cs2 U2 Cs1 71.380(10) 9_544 9_544 ? Cs2 U2 Cs1 108.620(10) . 9_544 ? O8 U2 Cs1 91.8(2) 9_544 . ? O8 U2 Cs1 88.2(2) . . ? O3 U2 Cs1 46.44(17) 15_545 . ? O3 U2 Cs1 133.56(17) 7_443 . ? O6 U2 Cs1 43.93(18) . . ? O6 U2 Cs1 136.07(18) 9_544 . ? Cs4 U2 Cs1 68.641(12) . . ? Cs4 U2 Cs1 111.359(12) 9_544 . ? Cs2 U2 Cs1 108.620(10) 9_544 . ? Cs2 U2 Cs1 71.380(10) . . ? Cs1 U2 Cs1 180.0 9_544 . ? O3 Si1 O1 107.6(4) . . ? O3 Si1 O4 110.9(4) . . ? O1 Si1 O4 109.5(3) . . ? O3 Si1 O2 110.6(3) . . ? O1 Si1 O2 108.5(4) . . ? O4 Si1 O2 109.7(4) . . ? O3 Si1 Cs4 55.7(2) . 15_445 ? O1 Si1 Cs4 135.1(4) . 15_445 ? O4 Si1 Cs4 56.7(3) . 15_445 ? O2 Si1 Cs4 116.4(2) . 15_445 ? O3 Si1 Cs1 56.5(2) . 10 ? O1 Si1 Cs1 59.4(4) . 10 ? O4 Si1 Cs1 99.9(2) . 10 ? O2 Si1 Cs1 150.4(2) . 10 ? Cs4 Si1 Cs1 79.94(4) 15_445 10 ? O6 Si2 O7 114.1(4) . . ? O6 Si2 O5 111.4(3) . . ? O7 Si2 O5 106.7(4) . . ? O6 Si2 O2 107.3(4) . . ? O7 Si2 O2 108.5(4) . . ? O5 Si2 O2 108.9(3) . . ? O6 Si2 Cs1 63.7(3) . . ? O7 Si2 Cs1 79.3(3) . . ? O5 Si2 Cs1 173.8(3) . . ? O2 Si2 Cs1 70.2(2) . . ? O6 Si2 Cs3 75.9(3) . . ? O7 Si2 Cs3 40.6(3) . . ? O5 Si2 Cs3 110.4(3) . . ? O2 Si2 Cs3 136.0(3) . . ? Cs1 Si2 Cs3 72.83(4) . . ? O6 Si2 Cs2 61.5(3) . . ? O7 Si2 Cs2 162.9(3) . . ? O5 Si2 Cs2 89.9(3) . . ? O2 Si2 Cs2 60.8(2) . . ? Cs1 Si2 Cs2 84.31(5) . . ? Cs3 Si2 Cs2 137.25(6) . . ? O6 Si2 Cs2 126.7(3) . 14_554 ? O7 Si2 Cs2 60.1(3) . 14_554 ? O5 Si2 Cs2 46.7(3) . 14_554 ? O2 Si2 Cs2 125.3(2) . 14_554 ? Cs1 Si2 Cs2 139.07(6) . 14_554 ? Cs3 Si2 Cs2 72.84(4) . 14_554 ? Cs2 Si2 Cs2 136.58(6) . 14_554 ? Si1 O1 Si1 167.3(8) 8_434 . ? Si1 O1 Cs1 96.4(4) 8_434 10 ? Si1 O1 Cs1 96.4(4) . 10 ? Si1 O2 Si2 132.9(4) . . ? Si1 O2 Cs1 115.3(3) . . ? Si2 O2 Cs1 82.5(3) . . ? Si1 O2 Cs2 123.9(3) . . ? Si2 O2 Cs2 94.8(3) . . ? Cs1 O2 Cs2 95.20(16) . . ? Si1 O3 U2 144.5(4) . 7_443 ? Si1 O3 Cs4 98.3(3) . 15_445 ? U2 O3 Cs4 103.4(2) 7_443 15_445 ? Si1 O3 Cs1 99.5(3) . 10 ? U2 O3 Cs1 104.0(2) 7_443 10 ? Cs4 O3 Cs1 99.81(18) 15_445 10 ? Si1 O4 U1 130.4(4) . . ? Si1 O4 Cs4 96.9(3) . 15_445 ? U1 O4 Cs4 116.5(3) . 15_445 ? Si1 O4 Cs3 126.5(3) . 13_444 ? U1 O4 Cs3 95.3(2) . 13_444 ? Cs4 O4 Cs3 81.57(16) 15_445 13_444 ? Si2 O5 Si2 135.2(6) 7_443 . ? Si2 O5 Cs2 112.4(3) 7_443 14_554 ? Si2 O5 Cs2 112.4(3) . 14_554 ? Si2 O6 U2 160.3(5) . . ? Si2 O6 Cs1 89.5(3) . . ? U2 O6 Cs1 106.9(2) . . ? Si2 O6 Cs2 94.8(3) . . ? U2 O6 Cs2 93.6(2) . . ? Cs1 O6 Cs2 98.15(19) . . ? Si2 O7 U1 133.0(4) . . ? Si2 O7 Cs3 118.1(4) . . ? U1 O7 Cs3 106.1(2) . . ? Si2 O7 Cs1 74.7(3) . . ? U1 O7 Cs1 94.7(2) . . ? Cs3 O7 Cs1 85.37(19) . . ? Si2 O7 Cs2 97.8(3) . 14_554 ? U1 O7 Cs2 94.4(3) . 14_554 ? Cs3 O7 Cs2 93.7(2) . 14_554 ? Cs1 O7 Cs2 170.7(2) . 14_554 ? U2 O8 Cs2 122.2(3) . 9_544 ? U2 O8 Cs4 112.1(3) . 9_544 ? Cs2 O8 Cs4 94.62(18) 9_544 9_544 ? U2 O8 Cs3 129.5(3) . . ? Cs2 O8 Cs3 103.86(18) 9_544 . ? Cs4 O8 Cs3 81.05(15) 9_544 . ? U1 O9 Cs1 126.3(3) . . ? U1 O9 Cs2 124.6(3) . 2_445 ? Cs1 O9 Cs2 106.9(2) . 2_445 ? U1 O9 Cs4 108.0(3) . 3_554 ? Cs1 O9 Cs4 91.6(2) . 3_554 ? Cs2 O9 Cs4 82.32(16) 2_445 3_554 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 2.529 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.321