# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety H4F1.5Na1.5O5U _chemical_formula_sum 'C0 H0 F1.50 N0 Na1.50 O5 U' _chemical_formula_weight 381.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 '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' 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 15.125(3) _cell_length_b 6.9410(10) _cell_length_c 11.257(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.76(3) _cell_angle_gamma 90.00 _cell_volume 1177.7(4) _cell_formula_units_Z 8 _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 4.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 27.656 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _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 6477 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 28.11 _reflns_number_total 1401 _reflns_number_gt 1308 _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 ? _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^)+(0.0182P)^2^+9.1641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00117(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1401 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0470 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.001 _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 U1 U -0.179667(12) 0.02588(3) 0.441839(16) 0.01205(10) Uani 1 1 d . . . Na1 Na 0.0000 -0.0504(5) 0.2500 0.0215(7) Uani 1 2 d S . . Na2 Na -0.11156(17) -0.5098(3) 0.3095(2) 0.0224(5) Uani 1 1 d . . . F1 F -0.3063(2) 0.1293(5) 0.5380(3) 0.0198(7) Uani 1 1 d . . . F2 F -0.2500 -0.2500 0.5000 0.0333(13) Uani 1 2 d S . . O1 O -0.2500(3) 0.0310(6) 0.3076(4) 0.0257(10) Uani 1 1 d . . . O2 O -0.1121(3) 0.0277(6) 0.5788(4) 0.0279(10) Uani 1 1 d . . . O3 O -0.0749(2) 0.1760(5) 0.3475(3) 0.0113(7) Uani 1 1 d . . . O4 O -0.0980(2) -0.2080(5) 0.3696(3) 0.0148(8) Uani 1 1 d . . . O5 O 0.0524(3) -0.5351(7) 0.3787(4) 0.0312(11) 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 U1 0.01061(13) 0.01109(13) 0.01481(12) 0.00002(7) 0.00325(7) -0.00011(7) Na1 0.0177(17) 0.0258(17) 0.0218(16) 0.000 0.0064(13) 0.000 Na2 0.0265(14) 0.0186(11) 0.0227(12) 0.0005(9) 0.0055(10) -0.0008(9) F1 0.0192(17) 0.0145(16) 0.0275(18) -0.0005(13) 0.0126(14) -0.0013(12) F2 0.033(3) 0.021(3) 0.048(3) -0.002(2) 0.020(3) -0.002(2) O1 0.020(2) 0.033(2) 0.023(2) -0.0022(18) -0.0040(18) 0.0023(17) O2 0.024(2) 0.035(3) 0.024(2) 0.0004(18) -0.0045(19) -0.0009(18) O3 0.0109(18) 0.0054(15) 0.0196(18) 0.0021(13) 0.0128(14) 0.0002(13) O4 0.0148(19) 0.0053(16) 0.026(2) -0.0017(14) 0.0120(16) 0.0006(13) O5 0.027(3) 0.043(3) 0.024(2) -0.0045(19) 0.000(2) -0.004(2) _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 U1 O1 1.774(4) . ? U1 O2 1.778(5) . ? U1 O4 2.234(3) . ? U1 O3 2.237(3) . ? U1 F2 2.3114(3) . ? U1 F1 2.387(3) . ? U1 F1 2.415(3) 7_456 ? U1 Na1 3.6472(11) . ? U1 Na2 3.731(2) 1_565 ? U1 U1 4.0476(7) 7_456 ? U1 Na2 4.069(3) 4_455 ? Na1 O3 2.272(4) 2 ? Na1 O3 2.272(4) . ? Na1 O4 2.353(4) 2 ? Na1 O4 2.353(4) . ? Na1 O2 2.464(5) 5_556 ? Na1 O2 2.464(5) 6 ? Na1 U1 3.6472(11) 2 ? Na1 Na2 3.695(4) 2 ? Na1 Na2 3.695(4) . ? Na1 Na2 4.191(4) 2_565 ? Na1 Na2 4.191(4) 1_565 ? Na2 O4 2.205(4) . ? Na2 O3 2.282(4) 1_545 ? Na2 F1 2.352(4) 7_446 ? Na2 O5 2.375(5) 2 ? Na2 O1 2.398(5) 4_445 ? Na2 O5 2.543(6) . ? Na2 U1 3.731(2) 1_545 ? Na2 Na2 3.733(5) 2 ? Na2 U1 4.069(3) 4_445 ? Na2 Na1 4.191(4) 1_545 ? F1 Na2 2.352(4) 7_446 ? F1 U1 2.415(3) 7_456 ? F2 U1 2.3114(3) 7_446 ? O1 Na2 2.398(5) 4_455 ? O2 Na1 2.464(5) 5_556 ? O3 Na2 2.282(4) 1_565 ? O5 Na2 2.375(5) 2 ? 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 O1 U1 O2 177.7(2) . . ? O1 U1 O4 90.86(17) . . ? O2 U1 O4 91.47(18) . . ? O1 U1 O3 89.12(18) . . ? O2 U1 O3 91.67(18) . . ? O4 U1 O3 74.38(12) . . ? O1 U1 F2 90.03(15) . . ? O2 U1 F2 90.31(15) . . ? O4 U1 F2 77.43(9) . . ? O3 U1 F2 151.79(8) . . ? O1 U1 F1 86.18(17) . . ? O2 U1 F1 91.70(18) . . ? O4 U1 F1 150.73(12) . . ? O3 U1 F1 134.56(12) . . ? F2 U1 F1 73.47(8) . . ? O1 U1 F1 90.50(16) . 7_456 ? O2 U1 F1 87.71(16) . 7_456 ? O4 U1 F1 144.12(11) . 7_456 ? O3 U1 F1 69.79(11) . 7_456 ? F2 U1 F1 138.43(7) . 7_456 ? F1 U1 F1 65.10(13) . 7_456 ? O1 U1 Na1 85.53(16) . . ? O2 U1 Na1 96.40(16) . . ? O4 U1 Na1 38.49(10) . . ? O3 U1 Na1 36.35(10) . . ? F2 U1 Na1 115.50(5) . . ? F1 U1 Na1 167.77(9) . . ? F1 U1 Na1 105.98(9) 7_456 . ? O1 U1 Na2 78.96(15) . 1_565 ? O2 U1 Na2 100.48(15) . 1_565 ? O4 U1 Na2 107.65(10) . 1_565 ? O3 U1 Na2 34.74(9) . 1_565 ? F2 U1 Na2 167.82(4) . 1_565 ? F1 U1 Na2 100.34(9) . 1_565 ? F1 U1 Na2 37.90(8) 7_456 1_565 ? Na1 U1 Na2 69.21(6) . 1_565 ? O1 U1 U1 88.05(14) . 7_456 ? O2 U1 U1 89.64(15) . 7_456 ? O4 U1 U1 176.23(9) . 7_456 ? O3 U1 U1 101.98(9) . 7_456 ? F2 U1 U1 106.173(18) . 7_456 ? F1 U1 U1 32.76(8) . 7_456 ? F1 U1 U1 32.34(7) 7_456 7_456 ? Na1 U1 U1 137.78(5) . 7_456 ? Na2 U1 U1 68.60(4) 1_565 7_456 ? O1 U1 Na2 14.84(16) . 4_455 ? O2 U1 Na2 163.89(16) . 4_455 ? O4 U1 Na2 97.07(11) . 4_455 ? O3 U1 Na2 103.75(10) . 4_455 ? F2 U1 Na2 78.33(3) . 4_455 ? F1 U1 Na2 74.23(9) . 4_455 ? F1 U1 Na2 93.23(9) 7_456 4_455 ? Na1 U1 Na2 98.78(4) . 4_455 ? Na2 U1 Na2 89.94(5) 1_565 4_455 ? U1 U1 Na2 82.72(3) 7_456 4_455 ? O3 Na1 O3 92.5(2) 2 . ? O3 Na1 O4 71.48(12) 2 2 ? O3 Na1 O4 163.89(17) . 2 ? O3 Na1 O4 163.89(17) 2 . ? O3 Na1 O4 71.48(12) . . ? O4 Na1 O4 124.6(2) 2 . ? O3 Na1 O2 89.75(15) 2 5_556 ? O3 Na1 O2 85.19(15) . 5_556 ? O4 Na1 O2 92.97(15) 2 5_556 ? O4 Na1 O2 90.43(15) . 5_556 ? O3 Na1 O2 85.19(15) 2 6 ? O3 Na1 O2 89.75(15) . 6 ? O4 Na1 O2 90.43(15) 2 6 ? O4 Na1 O2 92.97(15) . 6 ? O2 Na1 O2 172.7(3) 5_556 6 ? O3 Na1 U1 35.70(8) 2 2 ? O3 Na1 U1 127.68(14) . 2 ? O4 Na1 U1 36.21(8) 2 2 ? O4 Na1 U1 160.36(14) . 2 ? O2 Na1 U1 87.46(12) 5_556 2 ? O2 Na1 U1 91.47(12) 6 2 ? O3 Na1 U1 127.68(14) 2 . ? O3 Na1 U1 35.70(8) . . ? O4 Na1 U1 160.36(14) 2 . ? O4 Na1 U1 36.21(8) . . ? O2 Na1 U1 91.47(12) 5_556 . ? O2 Na1 U1 87.46(12) 6 . ? U1 Na1 U1 163.31(10) 2 . ? O3 Na1 Na2 104.82(10) 2 2 ? O3 Na1 Na2 159.70(11) . 2 ? O4 Na1 Na2 34.53(10) 2 2 ? O4 Na1 Na2 91.23(13) . 2 ? O2 Na1 Na2 84.38(13) 5_556 2 ? O2 Na1 Na2 102.01(13) 6 2 ? U1 Na1 Na2 69.14(5) 2 2 ? U1 Na1 Na2 127.34(8) . 2 ? O3 Na1 Na2 159.70(11) 2 . ? O3 Na1 Na2 104.82(10) . . ? O4 Na1 Na2 91.23(13) 2 . ? O4 Na1 Na2 34.53(10) . . ? O2 Na1 Na2 102.01(13) 5_556 . ? O2 Na1 Na2 84.38(13) 6 . ? U1 Na1 Na2 127.34(8) 2 . ? U1 Na1 Na2 69.14(5) . . ? Na2 Na1 Na2 60.69(9) 2 . ? O3 Na1 Na2 23.09(10) 2 2_565 ? O3 Na1 Na2 71.42(12) . 2_565 ? O4 Na1 Na2 92.50(10) 2 2_565 ? O4 Na1 Na2 142.08(12) . 2_565 ? O2 Na1 Na2 78.93(13) 5_556 2_565 ? O2 Na1 Na2 94.46(13) 6 2_565 ? U1 Na1 Na2 56.34(4) 2 2_565 ? U1 Na1 Na2 107.12(8) . 2_565 ? Na2 Na1 Na2 123.21(7) 2 2_565 ? Na2 Na1 Na2 176.10(5) . 2_565 ? O3 Na1 Na2 71.42(12) 2 1_565 ? O3 Na1 Na2 23.09(10) . 1_565 ? O4 Na1 Na2 142.08(12) 2 1_565 ? O4 Na1 Na2 92.50(10) . 1_565 ? O2 Na1 Na2 94.46(13) 5_556 1_565 ? O2 Na1 Na2 78.93(13) 6 1_565 ? U1 Na1 Na2 107.12(8) 2 1_565 ? U1 Na1 Na2 56.34(4) . 1_565 ? Na2 Na1 Na2 176.10(5) 2 1_565 ? Na2 Na1 Na2 123.21(7) . 1_565 ? Na2 Na1 Na2 52.89(8) 2_565 1_565 ? O4 Na2 O3 146.66(19) . 1_545 ? O4 Na2 F1 98.79(15) . 7_446 ? O3 Na2 F1 70.20(13) 1_545 7_446 ? O4 Na2 O5 108.15(17) . 2 ? O3 Na2 O5 89.58(16) 1_545 2 ? F1 Na2 O5 152.40(17) 7_446 2 ? O4 Na2 O1 96.38(17) . 4_445 ? O3 Na2 O1 113.81(17) 1_545 4_445 ? F1 Na2 O1 87.29(16) 7_446 4_445 ? O5 Na2 O1 83.93(18) 2 4_445 ? O4 Na2 O5 84.74(16) . . ? O3 Na2 O5 70.17(15) 1_545 . ? F1 Na2 O5 108.25(17) 7_446 . ? O5 Na2 O5 80.69(18) 2 . ? O1 Na2 O5 164.12(19) 4_445 . ? O4 Na2 Na1 37.22(10) . . ? O3 Na2 Na1 138.69(13) 1_545 . ? F1 Na2 Na1 135.54(12) 7_446 . ? O5 Na2 Na1 71.97(13) 2 . ? O1 Na2 Na1 100.92(12) 4_445 . ? O5 Na2 Na1 70.54(12) . . ? O4 Na2 U1 136.04(13) . 1_545 ? O3 Na2 U1 33.96(9) 1_545 1_545 ? F1 Na2 U1 39.10(8) 7_446 1_545 ? O5 Na2 U1 115.42(13) 2 1_545 ? O1 Na2 U1 93.68(12) 4_445 1_545 ? O5 Na2 U1 96.46(13) . 1_545 ? Na1 Na2 U1 164.42(8) . 1_545 ? O4 Na2 Na2 92.65(12) . 2 ? O3 Na2 Na2 81.62(11) 1_545 2 ? F1 Na2 Na2 144.12(14) 7_446 2 ? O5 Na2 Na2 42.33(13) 2 2 ? O1 Na2 Na2 125.23(16) 4_445 2 ? O5 Na2 Na2 38.96(12) . 2 ? Na1 Na2 Na2 59.66(5) . 2 ? U1 Na2 Na2 115.54(5) 1_545 2 ? O4 Na2 U1 101.67(13) . 4_445 ? O3 Na2 U1 110.55(12) 1_545 4_445 ? F1 Na2 U1 95.87(11) 7_446 4_445 ? O5 Na2 U1 73.25(13) 2 4_445 ? O1 Na2 U1 10.92(12) 4_445 4_445 ? O5 Na2 U1 153.89(14) . 4_445 ? Na1 Na2 U1 99.27(6) . 4_445 ? U1 Na2 U1 96.09(6) 1_545 4_445 ? Na2 Na2 U1 115.00(10) 2 4_445 ? O4 Na2 Na1 150.58(14) . 1_545 ? O3 Na2 Na1 22.99(9) 1_545 1_545 ? F1 Na2 Na1 92.58(10) 7_446 1_545 ? O5 Na2 Na1 66.70(12) 2 1_545 ? O1 Na2 Na1 111.27(13) 4_445 1_545 ? O5 Na2 Na1 65.91(12) . 1_545 ? Na1 Na2 Na1 123.21(7) . 1_545 ? U1 Na2 Na1 54.45(4) 1_545 1_545 ? Na2 Na2 Na1 63.55(4) 2 1_545 ? U1 Na2 Na1 104.05(5) 4_445 1_545 ? Na2 F1 U1 135.82(16) 7_446 . ? Na2 F1 U1 103.00(13) 7_446 7_456 ? U1 F1 U1 114.90(13) . 7_456 ? U1 F2 U1 180.000(10) . 7_446 ? U1 O1 Na2 154.2(3) . 4_455 ? U1 O2 Na1 171.0(3) . 5_556 ? U1 O3 Na1 107.95(15) . . ? U1 O3 Na2 111.30(15) . 1_565 ? Na1 O3 Na2 133.92(18) . 1_565 ? Na2 O4 U1 139.63(19) . . ? Na2 O4 Na1 108.25(17) . . ? U1 O4 Na1 105.31(15) . . ? Na2 O5 Na2 98.72(18) 2 . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.11 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.021 _refine_diff_density_min -1.343 _refine_diff_density_rms 0.214 _database_code_depnum_ccdc_archive 'CCDC 947896' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'F5 O4 U2, Cs' _chemical_formula_sum 'Cs F5 O4 U2' _chemical_formula_weight 767.97 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' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_space_group_name_Hall '-C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 12.1485(12) _cell_length_b 11.8621(13) _cell_length_c 12.3655(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1782.0(3) _cell_formula_units_Z 8 _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 5.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 40.391 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _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 5789 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.09 _reflns_number_total 976 _reflns_number_gt 887 _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 ? _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^)+(0.0400P)^2^+38.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00062(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 976 _refine_ls_number_parameters 69 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _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 0.27237(8) 0.0000 0.5000 0.0226(3) Uani 1 2 d S . . U2 U 0.0000 0.22326(4) 0.57102(4) 0.00637(18) Uani 1 2 d S . . U1 U 0.17846(4) 0.22427(4) 0.2500 0.00900(19) Uani 1 2 d S . . F1 F 0.0000 0.1687(9) 0.2500 0.015(2) Uani 1 4 d S . . F2 F 0.1798(5) 0.2285(6) 0.6335(5) 0.0310(17) Uani 1 1 d U . . F3 F 0.1192(5) 0.1998(6) 0.4273(4) 0.0205(13) Uani 1 1 d . . . F4 F 0.0000 0.2647(9) 0.7500 0.018(2) Uani 1 4 d SU . . O3 O 0.0000 0.0785(8) 0.5949(8) 0.023(2) Uani 1 2 d S . . O1 O 0.2242(9) 0.0830(9) 0.2500 0.023(2) Uani 1 2 d S . . O8 O 0.0000 0.3704(8) 0.5441(8) 0.023(2) Uani 1 2 d S . . O2 O 0.1352(10) 0.3658(8) 0.2500 0.027(2) Uani 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 Cs1 0.0287(5) 0.0156(4) 0.0235(5) 0.0095(4) 0.000 0.000 U2 0.0074(3) 0.0109(3) 0.0008(3) 0.00005(15) 0.000 0.000 U1 0.0057(3) 0.0196(3) 0.0016(3) 0.000 0.000 0.00088(18) F1 0.014(5) 0.019(6) 0.012(5) 0.000 0.000 0.000 F2 0.016(3) 0.069(5) 0.008(3) -0.003(3) -0.003(2) -0.012(3) F3 0.010(3) 0.046(4) 0.005(3) -0.001(2) -0.003(2) -0.006(3) F4 0.024(6) 0.025(5) 0.005(5) 0.000 0.000 0.000 O3 0.039(6) 0.014(5) 0.015(5) -0.002(4) 0.000 0.000 O1 0.027(6) 0.030(6) 0.012(5) 0.000 0.000 0.015(5) O8 0.037(6) 0.012(5) 0.020(5) 0.007(4) 0.000 0.000 O2 0.040(7) 0.014(5) 0.028(6) 0.000 0.000 -0.002(5) _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 F3 3.144(6) 4_556 ? Cs1 F3 3.144(6) . ? Cs1 O8 3.211(5) 13_556 ? Cs1 O8 3.211(5) 5_545 ? Cs1 O1 3.297(3) . ? Cs1 O1 3.297(3) 11_556 ? Cs1 F2 3.367(7) 4_556 ? Cs1 F2 3.367(7) . ? Cs1 O3 3.632(4) 9_556 ? Cs1 O3 3.632(4) . ? Cs1 O2 3.654(5) 13_556 ? Cs1 O2 3.654(5) 7_545 ? U2 O3 1.742(9) . ? U2 O8 1.776(9) . ? U2 F4 2.267(2) . ? U2 F3 2.309(5) 12 ? U2 F3 2.309(5) . ? U2 F2 2.317(6) . ? U2 F2 2.317(6) 12 ? U2 Cs1 4.3283(8) 9_556 ? U2 Cs1 4.3811(8) 13_556 ? U2 Cs1 4.3811(8) 5_455 ? U1 O2 1.759(10) . ? U1 O1 1.766(10) . ? U1 F1 2.266(3) . ? U1 F2 2.314(6) 13_556 ? U1 F2 2.314(6) 6_554 ? U1 F3 2.326(5) 10_556 ? U1 F3 2.326(5) . ? U1 Cs1 4.2351(5) 10_556 ? U1 Cs1 4.5399(5) 13_556 ? U1 Cs1 4.5399(5) 6_554 ? F1 U1 2.266(3) 3 ? F2 U1 2.314(6) 13_556 ? F2 Cs1 3.666(7) 13_556 ? F4 U2 2.267(2) 10_557 ? O3 Cs1 3.632(4) 9_556 ? O1 Cs1 3.297(3) 10_556 ? O8 Cs1 3.211(5) 5_455 ? O8 Cs1 3.211(5) 13_556 ? O2 Cs1 3.654(5) 13_556 ? O2 Cs1 3.654(5) 6_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 F3 Cs1 F3 107.4(2) 4_556 . ? F3 Cs1 O8 156.82(18) 4_556 13_556 ? F3 Cs1 O8 95.75(18) . 13_556 ? F3 Cs1 O8 95.75(18) 4_556 5_545 ? F3 Cs1 O8 156.82(18) . 5_545 ? O8 Cs1 O8 61.1(3) 13_556 5_545 ? F3 Cs1 O1 112.8(2) 4_556 . ? F3 Cs1 O1 53.27(18) . . ? O8 Cs1 O1 81.4(2) 13_556 . ? O8 Cs1 O1 117.1(2) 5_545 . ? F3 Cs1 O1 53.27(18) 4_556 11_556 ? F3 Cs1 O1 112.8(2) . 11_556 ? O8 Cs1 O1 117.1(2) 13_556 11_556 ? O8 Cs1 O1 81.4(2) 5_545 11_556 ? O1 Cs1 O1 159.6(4) . 11_556 ? F3 Cs1 F2 48.37(15) 4_556 4_556 ? F3 Cs1 F2 105.59(16) . 4_556 ? O8 Cs1 F2 126.2(2) 13_556 4_556 ? O8 Cs1 F2 89.2(2) 5_545 4_556 ? O1 Cs1 F2 73.8(2) . 4_556 ? O1 Cs1 F2 99.2(2) 11_556 4_556 ? F3 Cs1 F2 105.59(16) 4_556 . ? F3 Cs1 F2 48.37(15) . . ? O8 Cs1 F2 89.2(2) 13_556 . ? O8 Cs1 F2 126.2(2) 5_545 . ? O1 Cs1 F2 99.2(2) . . ? O1 Cs1 F2 73.8(2) 11_556 . ? F2 Cs1 F2 141.0(2) 4_556 . ? F3 Cs1 O3 50.20(18) 4_556 9_556 ? F3 Cs1 O3 64.01(18) . 9_556 ? O8 Cs1 O3 148.5(2) 13_556 9_556 ? O8 Cs1 O3 135.8(2) 5_545 9_556 ? O1 Cs1 O3 67.2(2) . 9_556 ? O1 Cs1 O3 93.7(2) 11_556 9_556 ? F2 Cs1 O3 47.99(17) 4_556 9_556 ? F2 Cs1 O3 93.46(17) . 9_556 ? F3 Cs1 O3 64.01(18) 4_556 . ? F3 Cs1 O3 50.20(18) . . ? O8 Cs1 O3 135.8(2) 13_556 . ? O8 Cs1 O3 148.5(2) 5_545 . ? O1 Cs1 O3 93.7(2) . . ? O1 Cs1 O3 67.2(2) 11_556 . ? F2 Cs1 O3 93.46(17) 4_556 . ? F2 Cs1 O3 47.99(17) . . ? O3 Cs1 O3 48.7(3) 9_556 . ? F3 Cs1 O2 105.56(17) 4_556 13_556 ? F3 Cs1 O2 95.48(19) . 13_556 ? O8 Cs1 O2 70.8(3) 13_556 13_556 ? O8 Cs1 O2 78.5(2) 5_545 13_556 ? O1 Cs1 O2 135.9(2) . 13_556 ? O1 Cs1 O2 52.5(2) 11_556 13_556 ? F2 Cs1 O2 150.24(18) 4_556 13_556 ? F2 Cs1 O2 48.5(2) . 13_556 ? O3 Cs1 O2 131.7(2) 9_556 13_556 ? O3 Cs1 O2 84.0(2) . 13_556 ? F3 Cs1 O2 95.48(19) 4_556 7_545 ? F3 Cs1 O2 105.56(17) . 7_545 ? O8 Cs1 O2 78.5(2) 13_556 7_545 ? O8 Cs1 O2 70.8(3) 5_545 7_545 ? O1 Cs1 O2 52.5(2) . 7_545 ? O1 Cs1 O2 135.9(2) 11_556 7_545 ? F2 Cs1 O2 48.5(2) 4_556 7_545 ? F2 Cs1 O2 150.24(18) . 7_545 ? O3 Cs1 O2 84.0(2) 9_556 7_545 ? O3 Cs1 O2 131.7(2) . 7_545 ? O2 Cs1 O2 144.2(4) 13_556 7_545 ? O3 U2 O8 179.0(4) . . ? O3 U2 F4 92.8(4) . . ? O8 U2 F4 88.3(4) . . ? O3 U2 F3 90.7(3) . 12 ? O8 U2 F3 88.5(3) . 12 ? F4 U2 F3 141.03(14) . 12 ? O3 U2 F3 90.7(3) . . ? O8 U2 F3 88.5(3) . . ? F4 U2 F3 141.03(14) . . ? F3 U2 F3 77.7(3) 12 . ? O3 U2 F2 88.3(2) . . ? O8 U2 F2 92.1(2) . . ? F4 U2 F2 70.66(17) . . ? F3 U2 F2 148.3(2) 12 . ? F3 U2 F2 70.7(2) . . ? O3 U2 F2 88.3(2) . 12 ? O8 U2 F2 92.1(2) . 12 ? F4 U2 F2 70.66(17) . 12 ? F3 U2 F2 70.7(2) 12 12 ? F3 U2 F2 148.3(2) . 12 ? F2 U2 F2 140.9(3) . 12 ? O3 U2 Cs1 55.34(12) . 9_556 ? O8 U2 Cs1 124.27(13) . 9_556 ? F4 U2 Cs1 109.30(16) . 9_556 ? F3 U2 Cs1 44.81(16) 12 9_556 ? F3 U2 Cs1 104.44(15) . 9_556 ? F2 U2 Cs1 143.56(18) . 9_556 ? F2 U2 Cs1 50.47(18) 12 9_556 ? O3 U2 Cs1 55.34(12) . . ? O8 U2 Cs1 124.27(13) . . ? F4 U2 Cs1 109.30(16) . . ? F3 U2 Cs1 104.44(15) 12 . ? F3 U2 Cs1 44.81(16) . . ? F2 U2 Cs1 50.47(18) . . ? F2 U2 Cs1 143.56(18) 12 . ? Cs1 U2 Cs1 99.72(2) 9_556 . ? O3 U2 Cs1 140.57(4) . 13_556 ? O8 U2 Cs1 39.33(3) . 13_556 ? F4 U2 Cs1 91.9(2) . 13_556 ? F3 U2 Cs1 109.39(16) 12 13_556 ? F3 U2 Cs1 62.64(16) . 13_556 ? F2 U2 Cs1 56.77(17) . 13_556 ? F2 U2 Cs1 129.91(18) 12 13_556 ? Cs1 U2 Cs1 154.202(13) 9_556 13_556 ? Cs1 U2 Cs1 86.288(9) . 13_556 ? O3 U2 Cs1 140.57(4) . 5_455 ? O8 U2 Cs1 39.33(3) . 5_455 ? F4 U2 Cs1 91.9(2) . 5_455 ? F3 U2 Cs1 62.64(16) 12 5_455 ? F3 U2 Cs1 109.39(16) . 5_455 ? F2 U2 Cs1 129.91(18) . 5_455 ? F2 U2 Cs1 56.77(17) 12 5_455 ? Cs1 U2 Cs1 86.288(9) 9_556 5_455 ? Cs1 U2 Cs1 154.201(13) . 5_455 ? Cs1 U2 Cs1 78.28(2) 13_556 5_455 ? O2 U1 O1 179.0(5) . . ? O2 U1 F1 89.6(5) . . ? O1 U1 F1 91.4(4) . . ? O2 U1 F2 89.5(3) . 13_556 ? O1 U1 F2 89.7(3) . 13_556 ? F1 U1 F2 141.49(17) . 13_556 ? O2 U1 F2 89.5(3) . 6_554 ? O1 U1 F2 89.7(3) . 6_554 ? F1 U1 F2 141.49(17) . 6_554 ? F2 U1 F2 77.0(3) 13_556 6_554 ? O2 U1 F3 91.5(2) . 10_556 ? O1 U1 F3 88.8(2) . 10_556 ? F1 U1 F3 70.58(14) . 10_556 ? F2 U1 F3 147.9(2) 13_556 10_556 ? F2 U1 F3 71.0(2) 6_554 10_556 ? O2 U1 F3 91.5(2) . . ? O1 U1 F3 88.8(2) . . ? F1 U1 F3 70.58(14) . . ? F2 U1 F3 71.0(2) 13_556 . ? F2 U1 F3 147.9(2) 6_554 . ? F3 U1 F3 141.0(3) 10_556 . ? O2 U1 Cs1 132.84(4) . 10_556 ? O1 U1 Cs1 47.07(3) . 10_556 ? F1 U1 Cs1 94.29(18) . 10_556 ? F2 U1 Cs1 113.96(18) 13_556 10_556 ? F2 U1 Cs1 59.82(17) 6_554 10_556 ? F3 U1 Cs1 46.90(16) 10_556 10_556 ? F3 U1 Cs1 133.86(16) . 10_556 ? O2 U1 Cs1 132.84(4) . . ? O1 U1 Cs1 47.07(3) . . ? F1 U1 Cs1 94.29(18) . . ? F2 U1 Cs1 59.82(17) 13_556 . ? F2 U1 Cs1 113.96(18) 6_554 . ? F3 U1 Cs1 133.86(16) 10_556 . ? F3 U1 Cs1 46.90(16) . . ? Cs1 U1 Cs1 93.764(14) 10_556 . ? O2 U1 Cs1 49.59(17) . 13_556 ? O1 U1 Cs1 129.97(16) . 13_556 ? F1 U1 Cs1 109.61(18) . 13_556 ? F2 U1 Cs1 45.87(18) 13_556 13_556 ? F2 U1 Cs1 98.71(17) 6_554 13_556 ? F3 U1 Cs1 140.59(16) 10_556 13_556 ? F3 U1 Cs1 59.26(16) . 13_556 ? Cs1 U1 Cs1 156.086(12) 10_556 13_556 ? Cs1 U1 Cs1 85.415(9) . 13_556 ? O2 U1 Cs1 49.59(17) . 6_554 ? O1 U1 Cs1 129.97(16) . 6_554 ? F1 U1 Cs1 109.61(18) . 6_554 ? F2 U1 Cs1 98.71(17) 13_556 6_554 ? F2 U1 Cs1 45.87(18) 6_554 6_554 ? F3 U1 Cs1 59.26(16) 10_556 6_554 ? F3 U1 Cs1 140.59(16) . 6_554 ? Cs1 U1 Cs1 85.415(9) 10_556 6_554 ? Cs1 U1 Cs1 156.086(12) . 6_554 ? Cs1 U1 Cs1 85.833(12) 13_556 6_554 ? U1 F1 U1 146.2(5) . 3 ? U1 F2 U2 156.3(3) 13_556 . ? U1 F2 Cs1 104.6(2) 13_556 . ? U2 F2 Cs1 97.5(2) . . ? U1 F2 Cs1 87.10(19) 13_556 13_556 ? U2 F2 Cs1 91.3(2) . 13_556 ? Cs1 F2 Cs1 115.69(19) . 13_556 ? U2 F3 U1 154.7(3) . . ? U2 F3 Cs1 104.0(2) . . ? U1 F3 Cs1 100.4(2) . . ? U2 F4 U2 155.0(5) . 10_557 ? U2 O3 Cs1 101.4(2) . 9_556 ? U2 O3 Cs1 101.4(2) . . ? Cs1 O3 Cs1 131.3(3) 9_556 . ? U1 O1 Cs1 109.83(17) . 10_556 ? U1 O1 Cs1 109.83(17) . . ? Cs1 O1 Cs1 139.4(3) 10_556 . ? U2 O8 Cs1 120.15(15) . 5_455 ? U2 O8 Cs1 120.15(15) . 13_556 ? Cs1 O8 Cs1 118.9(3) 5_455 13_556 ? U1 O2 Cs1 108.9(3) . 13_556 ? U1 O2 Cs1 108.9(3) . 6_554 ? Cs1 O2 Cs1 115.6(3) 13_556 6_554 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.164 _refine_diff_density_min -1.761 _refine_diff_density_rms 0.389 _database_code_depnum_ccdc_archive 'CCDC 947897'