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_7063791
_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 H4 O18, 2(H4 N), H2 O'
_chemical_formula_sum            'B10 H14 N2 O19'
_chemical_formula_weight         454.23
_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     iterative
_audit_creation_date             2025-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.02.27 svn.r83f5de26 for OlexSys, GUI svn.r7172)
;
_audit_update_record
;
2025-03-04 deposited with the CCDC.	2025-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                99.468(12)
_cell_angle_beta                 105.940(11)
_cell_angle_gamma                91.566(13)
_cell_formula_units_Z            2
_cell_length_a                   7.644(2)
_cell_length_b                   9.249(3)
_cell_length_c                   11.944(3)
_cell_measurement_reflns_used    3010
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.24
_cell_volume                     798.6(4)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7992
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.802
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6834
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0667 before and 0.0434 after correction.
The Ratio of minimum to maximum transmission is 0.9166.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         2909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0537P)^2^+0.4848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2419
_reflns_number_total             2909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01198a2.cif
_cod_data_source_block           NHBO
_cod_depositor_comments
'Adding full bibliography for 7063791--7063794.cif.'
_cod_database_code               7063791
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Others
 Sof(O19B)=1-FVAR(1)
 Sof(O19A)=FVAR(1)
2.a Riding coordinates:
 N1(H1A,H1B,H1C), N2(H2A,H2B), N2(H2C,H2D)
2.b Idealised tetrahedral OH refined as rotating group:
 O12(H12), O18(H18), O7(H7)
;
_shelx_res_checksum              50850
_shelx_hkl_checksum              81681
_olex2_submission_special_instructions 'No special instructions were received'