High Structural Complexity of Potassium Uranyl Borates Derived from High-Temperature/High-Pressure Reactions
Shijun Wu; Shuao Wang; Matthew Polinski; Oliver Beermann; Philip Kegler; Thomas Malcherek; Astrid Holzheid; Wulf Depmeier; Dirk Bosbach; Thomas E. Albrecht-Schmitt; Evgeny V. Alekseev; Inorganic Chemistry 52 (2013) 5110–5118; doi:10.1021/ic400016z

data_4334644
_publ_section_title
;
 High Structural Complexity of Potassium Uranyl Borates Derived from
 High-Temperature/High-Pressure Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5110
_journal_page_last               5118
_journal_paper_doi               10.1021/ic400016z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
K12[(UO2)19(UO4)(B2O5)2(BO3)6(BO2OH)O10](H2O)19.5
_chemical_formula_sum            'B22 H20 K24 O185 U40'
_chemical_formula_weight         13677.42
_chemical_name_common            'Potassium uranyl borate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           55
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2'
_symmetry_space_group_name_H-M   'P m c b'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   6.9284(4)
_cell_length_b                   13.3816(16)
_cell_length_c                   49.865(4)
_cell_measurement_reflns_used    5314
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      1.58
_cell_volume                     4623.1(7)
_computing_cell_refinement       'smart saint'
_computing_data_collection       smart
_computing_data_reduction        smart
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            92095
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    35.547
_exptl_absorpt_correction_T_max  0.058
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    4.906
_exptl_crystal_description       Prsim
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.266
_refine_diff_density_min         -2.804
_refine_diff_density_rms         0.337
_refine_ls_extinction_coef       0.000040(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5314
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.622
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+31.6193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                4359
_reflns_number_total             5314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400016z_si_001_1.cif
_cod_data_source_block           sad
_cod_original_formula_sum        'H20 B22 K24 O185 U40'
_cod_database_code               4334644