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_4334646
_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         K15(UO2)18(BO3)7O15
_chemical_formula_sum            'B7 K15 O72 U18'
_chemical_formula_weight         6098.71
_chemical_name_common            'Potassium uranyl borate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           10
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 1'
_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                 107.586(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   13.438(7)
_cell_length_b                   6.850(4)
_cell_length_c                   22.238(12)
_cell_measurement_reflns_used    4497
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      0.96
_cell_volume                     1951.3(19)
_computing_cell_refinement       'smart saint'
_computing_data_collection       smart
_computing_data_reduction        sanit
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1384
_diffrn_reflns_av_sigmaI/netI    0.1133
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22221
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    38.103
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    5.190
_exptl_crystal_description       Tablet
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.012
_refine_diff_density_max         9.199
_refine_diff_density_min         -7.252
_refine_diff_density_rms         0.650
_refine_ls_extinction_coef       0.000063(18)
_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   1.070
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                1894
_reflns_number_total             4497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400016z_si_001_3.cif
_cod_data_source_block           new
_cod_original_cell_volume        1951.3(18)
_cod_original_sg_symbol_H-M      'P 2/m'
_cod_database_code               4334646