Cation tuning in anionic framework hydroborates: tailored deep-ultraviolet optical crystals with large birefringence
Jiang, Yansheng; Jia, Hangwei; Wang, Wenhu; Arif, Muhammad; Yan, Xiuling; Hou, Xueling; New Journal of Chemistry 49 (2025) 8908–8913; doi:10.1039/D5NJ01198A

data_7063793
_publ_section_title
;
 Cation tuning in anionic framework hydroborates: tailored
 deep-ultraviolet optical crystals with large birefringence
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8908
_journal_page_last               8913
_journal_paper_doi               10.1039/D5NJ01198A
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'B10 H8 K1.5 N0.5 O19'
_chemical_formula_sum            'B10 H8 K1.5 N0.5 O19'
_chemical_formula_weight         485.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-16 deposited with the CCDC.	2025-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                98.805(18)
_cell_angle_beta                 106.617(19)
_cell_angle_gamma                91.53(2)
_cell_formula_units_Z            2
_cell_length_a                   7.601(4)
_cell_length_b                   9.211(4)
_cell_length_c                   11.809(6)
_cell_measurement_reflns_used    3076
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.64
_cell_volume                     780.7(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17143
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_min         1.826
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.041
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0671P)^2^+0.9825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2806
_reflns_number_total             3558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01198a2.cif
_cod_data_source_block           dddd
_cod_depositor_comments
'Adding full bibliography for 7063791--7063794.cif.'
_cod_original_formula_sum        'B10 H8 K1.50 N0.50 O19'
_cod_database_code               7063793
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups, H1 of O1
 At 1.5 times of:
  All O(H,H) groups, H11 of O11, H8 of O8
2. Shared sites
{K2, N1}
3. Uiso/Uaniso restraints and constraints
Uanis(K2) = Uanis(N1)
4. Others
 Fixed Sof: K2(0.5) N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C,H1D)
5.b Rotating group:
 O19(H19A,H19B)
5.c Aromatic/amide H refined with riding coordinates:
 O1(H1)
5.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O11(H11)
;
_shelx_res_checksum              69518
_shelx_hkl_checksum              5849
_olex2_submission_special_instructions 'No special instructions were received'