Three mixed-alkaline-metal borates with {Li@B12Ox(OH)24−x} (x = 18, 22) clusters: from isolated oxoboron cluster to unusual layer
Qiu, Qi-Ming; Yang, Guo-Yu; CrystEngComm 23 (2021) 6518–6525; doi:10.1039/D1CE00910A

data_7243363
_publ_section_title
;
 Three mixed-alkaline-metal borates with {Li@B12Ox(OH)24&#x2212;x} (x =
 18, 22) clusters: from isolated oxoboron cluster to unusual layer
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              6518
_journal_page_last               6525
_journal_paper_doi               10.1039/D1CE00910A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'B12 Cs5 H8 Li O25'
_chemical_formula_weight         1209.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2021-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.316(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3037(19)
_cell_length_b                   10.863(2)
_cell_length_c                   13.007(3)
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.43
_cell_volume                     1306.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3971
_diffrn_reflns_point_group_measured_fraction_full 0.533
_diffrn_reflns_point_group_measured_fraction_max 0.521
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.158
_diffrn_reflns_theta_min         1.875
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.074
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.379
_refine_diff_density_max         2.365
_refine_diff_density_min         -2.190
_refine_diff_density_rms         0.341
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.22(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         2716
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0108P)^2^+99.5817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.098
_reflns_Friedel_fraction_full    0.102
_reflns_Friedel_fraction_max     0.093
_reflns_number_gt                2471
_reflns_number_total             2716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00910a2.cif
_cod_data_source_block           3_a
_cod_depositor_comments
'Adding full bibliography for 7243362--7243364.cif.'
_cod_original_cell_volume        1306.6(4)
_cod_original_sg_symbol_H-M      'P c'
_cod_original_formula_sum        'B12 H8 Cs5 Li O25'
_cod_database_code               7243363
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.721
_shelx_estimated_absorpt_t_max   0.767
_shelx_res_checksum              45424