Hydrothermal Synthesis and Structural Investigation of a Crystalline Uranyl Borosilicate
Pace, Kristen A.; Klepov, Vladislav V.; Smith, Mark D.; Williams, Travis; Morrison, Gregory; Lauterbach, Jochen A.; Misture, Scott T.; zur Loye, Hans-Conrad; Inorganics 9 (2021) 25–; doi:10.3390/inorganics9040025

data_1562365
_publ_section_title
;
 Hydrothermal Synthesis and Structural Investigation of a Crystalline
 Uranyl Borosilicate
;
_journal_issue                   4
_journal_name_full               Inorganics
_journal_page_first              25
_journal_paper_doi               10.3390/inorganics9040025
_journal_volume                  9
_journal_year                    2021
_chemical_formula_moiety         'B K1.78 Na1.22 O14 Si4 U'
_chemical_formula_sum            'B K1.78 Na1.22 O14 Si4 U'
_chemical_formula_weight         682.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_primary     dual-space
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5471(19)
_cell_length_b                   14.3403(17)
_cell_length_c                   11.7315(15)
_cell_measurement_reflns_used    9730
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      34.952
_cell_measurement_theta_min      2.597
_cell_volume                     2615.5(6)
_computing_cell_refinement       'SAINT+ Ver. 8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX3 v2019.1-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT+ Ver. 8.40A (Bruker, 2019)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      301(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            72412
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.003
_diffrn_reflns_theta_min         2.598
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    13.460
_exptl_absorpt_correction_T_max  0.1637
_exptl_absorpt_correction_T_min  0.1143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.468
_exptl_crystal_description       plate
_exptl_crystal_F_000             2498
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         4.154
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2963
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+41.1625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2822
_reflns_number_total             2963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            KAP1150B_MDS.cif
_cod_data_source_block           kap1150b
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               1562365
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.615
_shelx_estimated_absorpt_t_max   0.775
_shelx_res_checksum              78028
_shelx_hkl_checksum              66469