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_7063794
_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 Cs1.3 H6 O19, 0.7(H4 N1)'
_chemical_formula_sum            'B10 Cs1.3 H8.8 N0.7 O19'
_chemical_formula_weight         603.56
_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             2024-07-08
_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                98.919(7)
_cell_angle_beta                 106.626(6)
_cell_angle_gamma                91.351(7)
_cell_formula_units_Z            2
_cell_length_a                   7.7386(13)
_cell_length_b                   9.1876(17)
_cell_length_c                   12.178(2)
_cell_measurement_reflns_used    7384
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.25
_cell_volume                     817.5(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0643
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22982
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.771
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.028
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0919 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.8734.
The \l/2 correction factor is Not present.
;
_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    2.452
_exptl_crystal_description       block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.952
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0516P)^2^+3.7429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3414
_reflns_number_total             3729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01198a2.cif
_cod_data_source_block           44444
_cod_depositor_comments
'Adding full bibliography for 7063791--7063794.cif.'
_cod_original_formula_sum        'B10 H8.80 Cs1.30 N0.70 O19'
_cod_database_code               7063794
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Shared sites
{Cs2, N1}
2. Restrained distances
 O9-H9
 0.95 with sigma of 0.01
 H13-O13
 0.95 with sigma of 0.01
 H2-O2
 0.95 with sigma of 0.01
 O19-H19
 0.95 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cs2) = Uanis(N1)
4. Others
 Fixed Sof: Cs2(0.3) N1(0.7) H1C(0.7) H1D(0.7) H1E(0.7) H1F(0.7)
5.a Riding coordinates:
 O13(H13), O2(H2), O1(H1A,H1B), N1(H1C,H1D,H1E,H1F)
5.b Aromatic/amide H refined with riding coordinates:
 O19(H19)
5.c Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'