data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca O4 U' _chemical_formula_weight 342.11 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' 'Ca' 'Ca' 0.2262 0.3064 '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 ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'y, -x+1/2, z+1/2' '-y, x+1/2, z+1/2' 'x, z+1/2, -y+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'x, -z+1/2, y+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' '-z, y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, -z+1/2' '-y+1/2, -x, -z+1/2' 'y+1/2, -x, z+1/2' '-y+1/2, x, z+1/2' 'x+1/2, z, -y+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' 'y+1/2, -x+1/2, z' '-y+1/2, x+1/2, z' 'x+1/2, z+1/2, -y' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'x+1/2, -z+1/2, y' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' '-z+1/2, y+1/2, x' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-z, -x+1/2, -y+1/2' '-z, x+1/2, y+1/2' 'z, x+1/2, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' '-y, -x+1/2, z+1/2' 'y, x+1/2, z+1/2' '-y, x+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' '-x, -z+1/2, y+1/2' 'x, -z+1/2, -y+1/2' 'x, z+1/2, y+1/2' '-x, z+1/2, -y+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' 'z, -y+1/2, -x+1/2' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' '-z+1/2, -x, -y+1/2' '-z+1/2, x, y+1/2' 'z+1/2, x, -y+1/2' 'z+1/2, -x, y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/2, -z, x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' '-y+1/2, -x, z+1/2' 'y+1/2, x, z+1/2' '-y+1/2, x, -z+1/2' 'y+1/2, -x, -z+1/2' '-x+1/2, -z, y+1/2' 'x+1/2, -z, -y+1/2' 'x+1/2, z, y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' 'z+1/2, -y, -x+1/2' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/2, y' 'z+1/2, x+1/2, -y' 'z+1/2, -x+1/2, y' '-y+1/2, -z+1/2, -x' 'y+1/2, -z+1/2, x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' '-y+1/2, x+1/2, -z' 'y+1/2, -x+1/2, -z' '-x+1/2, -z+1/2, y' 'x+1/2, -z+1/2, -y' 'x+1/2, z+1/2, y' '-x+1/2, z+1/2, -y' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, -x' 'z+1/2, y+1/2, x' _cell_length_a 5.3813(2) _cell_length_b 5.3813(2) _cell_length_c 5.3813(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 155.834(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 53.544 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.1749 _exptl_absorpt_correction_T_max 0.6165 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 1548 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0071 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 6.57 _diffrn_reflns_theta_max 32.99 _reflns_number_total 29 _reflns_number_gt 29 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0114P)^2^+0.0000P] 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 29 _refine_ls_number_parameters 4 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0083 _refine_ls_R_factor_gt 0.0083 _refine_ls_wR_factor_ref 0.0190 _refine_ls_wR_factor_gt 0.0190 _refine_ls_goodness_of_fit_ref 1.322 _refine_ls_restrained_S_all 1.322 _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 U1 U 0.0000 0.5000 0.0000 0.01790(17) Uani 0.471(18) 48 d SP . . Ca1 Ca 0.0000 0.5000 0.0000 0.01790(17) Uani 0.529(18) 48 d SP . . O1 O 0.2500 0.2500 0.2500 0.057(3) Uani 1 24 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 U1 0.01790(17) 0.01790(17) 0.01790(17) 0.000 0.000 0.000 Ca1 0.01790(17) 0.01790(17) 0.01790(17) 0.000 0.000 0.000 O1 0.057(3) 0.057(3) 0.057(3) 0.000 0.000 0.000 _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 2.3302 145_565 ? U1 O1 2.3302 49_454 ? U1 O1 2.3302 169 ? U1 O1 2.3302 . ? U1 O1 2.3302 121 ? U1 O1 2.3302 97_565 ? U1 O1 2.3302 73_455 ? U1 O1 2.3302 25_554 ? U1 U1 3.80515(14) 25 ? U1 U1 3.80515(14) 49 ? U1 U1 3.80515(14) 73_445 ? U1 U1 3.80515(14) 49_454 ? Ca1 O1 2.3302 145_565 ? Ca1 O1 2.3302 49_454 ? Ca1 O1 2.3302 169 ? Ca1 O1 2.3302 . ? Ca1 O1 2.3302 121 ? Ca1 O1 2.3302 97_565 ? Ca1 O1 2.3302 73_455 ? Ca1 O1 2.3302 25_554 ? Ca1 U1 3.80515(14) 25 ? Ca1 U1 3.80515(14) 49 ? Ca1 U1 3.80515(14) 73_445 ? Ca1 U1 3.80515(14) 49_454 ? O1 Ca1 2.3302 49 ? O1 U1 2.3302 49 ? O1 Ca1 2.3302 73_545 ? O1 U1 2.3302 25_545 ? O1 U1 2.3302 73_545 ? O1 Ca1 2.3302 25_545 ? 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 O1 180.0 145_565 49_454 ? O1 U1 O1 109.5 145_565 169 ? O1 U1 O1 70.5 49_454 169 ? O1 U1 O1 70.5 145_565 . ? O1 U1 O1 109.5 49_454 . ? O1 U1 O1 70.5 169 . ? O1 U1 O1 109.5 145_565 121 ? O1 U1 O1 70.5 49_454 121 ? O1 U1 O1 109.5 169 121 ? O1 U1 O1 70.5 . 121 ? O1 U1 O1 109.5 145_565 97_565 ? O1 U1 O1 70.5 49_454 97_565 ? O1 U1 O1 109.5 169 97_565 ? O1 U1 O1 180.0 . 97_565 ? O1 U1 O1 109.5 121 97_565 ? O1 U1 O1 70.5 145_565 73_455 ? O1 U1 O1 109.5 49_454 73_455 ? O1 U1 O1 180.0 169 73_455 ? O1 U1 O1 109.5 . 73_455 ? O1 U1 O1 70.5 121 73_455 ? O1 U1 O1 70.5 97_565 73_455 ? O1 U1 O1 70.5 145_565 25_554 ? O1 U1 O1 109.5 49_454 25_554 ? O1 U1 O1 70.5 169 25_554 ? O1 U1 O1 109.5 . 25_554 ? O1 U1 O1 180.0 121 25_554 ? O1 U1 O1 70.5 97_565 25_554 ? O1 U1 O1 109.5 73_455 25_554 ? O1 U1 U1 35.3 145_565 25 ? O1 U1 U1 144.7 49_454 25 ? O1 U1 U1 144.7 169 25 ? O1 U1 U1 90.0 . 25 ? O1 U1 U1 90.0 121 25 ? O1 U1 U1 90.0 97_565 25 ? O1 U1 U1 35.3 73_455 25 ? O1 U1 U1 90.0 25_554 25 ? O1 U1 U1 35.3 145_565 49 ? O1 U1 U1 144.7 49_454 49 ? O1 U1 U1 90.0 169 49 ? O1 U1 U1 35.3 . 49 ? O1 U1 U1 90.0 121 49 ? O1 U1 U1 144.7 97_565 49 ? O1 U1 U1 90.0 73_455 49 ? O1 U1 U1 90.0 25_554 49 ? U1 U1 U1 60.0 25 49 ? O1 U1 U1 144.7 145_565 73_445 ? O1 U1 U1 35.3 49_454 73_445 ? O1 U1 U1 90.0 169 73_445 ? O1 U1 U1 90.0 . 73_445 ? O1 U1 U1 35.3 121 73_445 ? O1 U1 U1 90.0 97_565 73_445 ? O1 U1 U1 90.0 73_455 73_445 ? O1 U1 U1 144.7 25_554 73_445 ? U1 U1 U1 120.0 25 73_445 ? U1 U1 U1 120.0 49 73_445 ? O1 U1 U1 144.7 145_565 49_454 ? O1 U1 U1 35.3 49_454 49_454 ? O1 U1 U1 90.0 169 49_454 ? O1 U1 U1 144.7 . 49_454 ? O1 U1 U1 90.0 121 49_454 ? O1 U1 U1 35.3 97_565 49_454 ? O1 U1 U1 90.0 73_455 49_454 ? O1 U1 U1 90.0 25_554 49_454 ? U1 U1 U1 120.0 25 49_454 ? U1 U1 U1 180.0 49 49_454 ? U1 U1 U1 60.0 73_445 49_454 ? O1 Ca1 O1 180.0 145_565 49_454 ? O1 Ca1 O1 109.5 145_565 169 ? O1 Ca1 O1 70.5 49_454 169 ? O1 Ca1 O1 70.5 145_565 . ? O1 Ca1 O1 109.5 49_454 . ? O1 Ca1 O1 70.5 169 . ? O1 Ca1 O1 109.5 145_565 121 ? O1 Ca1 O1 70.5 49_454 121 ? O1 Ca1 O1 109.5 169 121 ? O1 Ca1 O1 70.5 . 121 ? O1 Ca1 O1 109.5 145_565 97_565 ? O1 Ca1 O1 70.5 49_454 97_565 ? O1 Ca1 O1 109.5 169 97_565 ? O1 Ca1 O1 180.0 . 97_565 ? O1 Ca1 O1 109.5 121 97_565 ? O1 Ca1 O1 70.5 145_565 73_455 ? O1 Ca1 O1 109.5 49_454 73_455 ? O1 Ca1 O1 180.0 169 73_455 ? O1 Ca1 O1 109.5 . 73_455 ? O1 Ca1 O1 70.5 121 73_455 ? O1 Ca1 O1 70.5 97_565 73_455 ? O1 Ca1 O1 70.5 145_565 25_554 ? O1 Ca1 O1 109.5 49_454 25_554 ? O1 Ca1 O1 70.5 169 25_554 ? O1 Ca1 O1 109.5 . 25_554 ? O1 Ca1 O1 180.0 121 25_554 ? O1 Ca1 O1 70.5 97_565 25_554 ? O1 Ca1 O1 109.5 73_455 25_554 ? O1 Ca1 U1 35.3 145_565 25 ? O1 Ca1 U1 144.7 49_454 25 ? O1 Ca1 U1 144.7 169 25 ? O1 Ca1 U1 90.0 . 25 ? O1 Ca1 U1 90.0 121 25 ? O1 Ca1 U1 90.0 97_565 25 ? O1 Ca1 U1 35.3 73_455 25 ? O1 Ca1 U1 90.0 25_554 25 ? O1 Ca1 U1 35.3 145_565 49 ? O1 Ca1 U1 144.7 49_454 49 ? O1 Ca1 U1 90.0 169 49 ? O1 Ca1 U1 35.3 . 49 ? O1 Ca1 U1 90.0 121 49 ? O1 Ca1 U1 144.7 97_565 49 ? O1 Ca1 U1 90.0 73_455 49 ? O1 Ca1 U1 90.0 25_554 49 ? U1 Ca1 U1 60.0 25 49 ? O1 Ca1 U1 144.7 145_565 73_445 ? O1 Ca1 U1 35.3 49_454 73_445 ? O1 Ca1 U1 90.0 169 73_445 ? O1 Ca1 U1 90.0 . 73_445 ? O1 Ca1 U1 35.3 121 73_445 ? O1 Ca1 U1 90.0 97_565 73_445 ? O1 Ca1 U1 90.0 73_455 73_445 ? O1 Ca1 U1 144.7 25_554 73_445 ? U1 Ca1 U1 120.0 25 73_445 ? U1 Ca1 U1 120.0 49 73_445 ? O1 Ca1 U1 144.7 145_565 49_454 ? O1 Ca1 U1 35.3 49_454 49_454 ? O1 Ca1 U1 90.0 169 49_454 ? O1 Ca1 U1 144.7 . 49_454 ? O1 Ca1 U1 90.0 121 49_454 ? O1 Ca1 U1 35.3 97_565 49_454 ? O1 Ca1 U1 90.0 73_455 49_454 ? O1 Ca1 U1 90.0 25_554 49_454 ? U1 Ca1 U1 120.0 25 49_454 ? U1 Ca1 U1 180.0 49 49_454 ? U1 Ca1 U1 60.0 73_445 49_454 ? Ca1 O1 U1 0.0 49 49 ? Ca1 O1 Ca1 109.5 49 73_545 ? U1 O1 Ca1 109.5 49 73_545 ? Ca1 O1 U1 109.5 49 25_545 ? U1 O1 U1 109.5 49 25_545 ? Ca1 O1 U1 109.5 73_545 25_545 ? Ca1 O1 Ca1 109.5 49 . ? U1 O1 Ca1 109.5 49 . ? Ca1 O1 Ca1 109.5 73_545 . ? U1 O1 Ca1 109.5 25_545 . ? Ca1 O1 U1 109.5 49 73_545 ? U1 O1 U1 109.5 49 73_545 ? Ca1 O1 U1 0.0 73_545 73_545 ? U1 O1 U1 109.5 25_545 73_545 ? Ca1 O1 U1 109.5 . 73_545 ? Ca1 O1 Ca1 109.5 49 25_545 ? U1 O1 Ca1 109.5 49 25_545 ? Ca1 O1 Ca1 109.5 73_545 25_545 ? U1 O1 Ca1 0.0 25_545 25_545 ? Ca1 O1 Ca1 109.5 . 25_545 ? U1 O1 Ca1 109.5 73_545 25_545 ? Ca1 O1 U1 109.5 49 . ? U1 O1 U1 109.5 49 . ? Ca1 O1 U1 109.5 73_545 . ? U1 O1 U1 109.5 25_545 . ? Ca1 O1 U1 0.0 . . ? U1 O1 U1 109.5 73_545 . ? Ca1 O1 U1 109.5 25_545 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 32.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.244 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.086