A nonlinear optical crystal with deep-ultraviolet transparency and appropriate birefringence achieved using π-conjugated confined [B3O3F4(OH)]2−
Ouyang, Tao; Chen, Xu; Chen, Shanshan; Li, Yanqiang; Shang, Xiaoying; Bai, Zhiyong; Jiang, Ningtao; Yan, Zhishuo; Luo, Junhua; Zhao, Sangen; New Journal of Chemistry 48 (2024) 15281–15286; doi:10.1039/D4NJ02834A

data_7063421
_publ_section_title
;
 A nonlinear optical crystal with deep-ultraviolet transparency and
 appropriate birefringence achieved using \p-conjugated confined
 [B3O3F4(OH)]2&#x2212;
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15281
_journal_page_last               15286
_journal_paper_doi               10.1039/D4NJ02834A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'B3 F4 H K2 O4'
_chemical_formula_sum            'B3 F4 H K2 O4'
_chemical_formula_weight         251.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           40
_space_group_name_Hall           'A 2 -2a'
_space_group_name_H-M_alt        'A m a 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-06 deposited with the CCDC.	2024-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   25.9308(5)
_cell_length_b                   22.5853(4)
_cell_length_c                   7.46320(10)
_cell_measurement_reflns_used    4670
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.3290
_cell_measurement_theta_min      3.9090
_cell_volume                     4370.86(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -97.00 -37.00   0.50    2.11    -- -106.00 114.00  -1.00  120
  2  \w    -61.00 -35.00   0.50    0.53    --  -46.49 114.00  -1.00   52
  3  \w   -177.00-140.00   0.50    2.11    -- -106.00 -15.00 -30.00   74
  4  \w   -134.00 -89.00   0.50    2.11    -- -106.00 -15.00 -30.00   90
  5  \w    -70.00 -44.00   0.50    2.11    -- -106.00  61.00-120.00   52
  6  \w    -68.00 -34.00   0.50    2.11    -- -106.00  61.00-150.00   68
  7  \w    -68.00 -34.00   0.50    2.11    -- -106.00  61.00-180.00   68
  8  \w    -27.00  29.00   0.50    0.53    --  -46.49  19.00-180.00  112
  9  \w      5.00  80.00   0.50    0.53    --   46.49-114.00 -91.00  150
 10  \w     39.00  80.00   0.50    2.11    --  107.95-114.00 -91.00   82
 11  \w     35.00  70.00   0.50    2.11    --  107.95 -61.00 -30.00   70
 12  \w     35.00  71.00   0.50    2.11    --  107.95 -61.00 -60.00   72
 13  \w    104.00 130.00   0.50    2.11    --  107.95 114.00  -1.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1310817000
_diffrn_orient_matrix_UB_12      0.0252029000
_diffrn_orient_matrix_UB_13      0.0403013000
_diffrn_orient_matrix_UB_21      0.1421401000
_diffrn_orient_matrix_UB_22      0.0085330000
_diffrn_orient_matrix_UB_23      -0.0424146000
_diffrn_orient_matrix_UB_31      -0.0721043000
_diffrn_orient_matrix_UB_32      0.0628023000
_diffrn_orient_matrix_UB_33      -0.0104383000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7457
_diffrn_reflns_point_group_measured_fraction_full 0.734
_diffrn_reflns_point_group_measured_fraction_max 0.697
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.598
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    2.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             2928
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.076(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         3271
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+2.1329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.344
_reflns_Friedel_fraction_full    0.432
_reflns_Friedel_fraction_max     0.388
_reflns_number_gt                2987
_reflns_number_total             3271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02834a2.cif
_cod_data_source_block           Compound
_cod_depositor_comments          'Adding full bibliography for 7063421.cif.'
_cod_original_formula_sum        'B3 H F4 K2 O4'
_cod_database_code               7063421
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K B O F'
_chemical_oxdiff_usercomment     'K B O F'
_reflns_odcompleteness_completeness 98.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.924(19)
 0.076(19)
2. Restrained distances
 O15-H4
 0.85 with sigma of 0.02
 H2-O7
 0.85 with sigma of 0.02
 O11-H3
 0.85 with sigma of 0.02
 H1-O3
 0.85 with sigma of 0.02
 H3_$1-O16_$1
 1.85 with sigma of 0.02
 H1_$2-O6_$2
 1.85 with sigma of 0.02
 F10-B8
 1.6 with sigma of 0.02
3. Rigid bond restraints
 B8, B7, B9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F5, F6, F2, F1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: F10(0.5) B8(0.5)
 Fixed Uiso: H1(0.06)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.658
_oxdiff_exptl_absorpt_empirical_full_min 0.656