Regulating KBBF-like structures via a charge-assisted hydrogen-bonded framework to enable easily grown ultraviolet nonlinear optical crystals
Zhang, Mingshu; Zhao, Shuya; Wu, Zhen-Cheng; Yin, Yue; Zhang, Zheyu; Chen, Jiafeng; Guo, Sheng-Ping; Zhou, Yan; Chemical Science  (2026) –; doi:10.1039/D5SC09306F

data_1577091
_publ_section_title
;
 Regulating KBBF-like structures <i>via</i> a charge-assisted
 hydrogen-bonded framework to enable easily grown ultraviolet nonlinear
 optical crystals.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              9930
_journal_page_last               9937
_journal_paper_doi               10.1039/d5sc09306f
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         (C6H9N2SO2)(NO3)
_chemical_formula_sum            'C6 H9 N3 O5 S'
_chemical_formula_weight         235.22
_chemical_name_common            (C6H9N2SO2)(NO3)
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
;
2025-11-12 deposited with the CCDC.	2026-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.039(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1524(8)
_cell_length_b                   8.1924(4)
_cell_length_c                   8.6986(5)
_cell_measurement_reflns_used    8505
_cell_measurement_temperature    300.5(7)
_cell_measurement_theta_max      30.6050
_cell_measurement_theta_min      2.8850
_cell_volume                     964.27(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.5(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.883
_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     -9.00  20.00   0.50    0.30    --    6.50  19.00 150.00   58
  2  \w    -18.00  40.00   0.50    0.30    --    6.50 -99.00 150.00  116
  3  \w    -18.00  40.00   0.50    0.30    --    6.50 -99.00  90.00  116
  4  \w    -18.00  40.00   0.50    0.30    --    6.50 -99.00-120.00  116
  5  \w     -8.00  80.00   0.50    0.30    --    6.50  38.00-150.00  176
  6  \w    -20.00  68.00   0.50    0.30    --   -5.57  38.00 -60.00  176
  7  \w    -79.00   9.00   0.50    0.30    --   -5.57 -38.00 -30.00  176
  8  \w    -78.00  18.00   0.50    0.30    --   -5.57 -77.00 -90.00  192
  9  \w    -27.50  11.00   0.50    0.30    --   -5.57 -57.00-180.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0126501000
_diffrn_orient_matrix_UB_12      -0.0164829000
_diffrn_orient_matrix_UB_13      0.0715555000
_diffrn_orient_matrix_UB_21      0.0490276000
_diffrn_orient_matrix_UB_22      -0.0265803000
_diffrn_orient_matrix_UB_23      0.0377579000
_diffrn_orient_matrix_UB_31      0.0135698000
_diffrn_orient_matrix_UB_32      0.0807299000
_diffrn_orient_matrix_UB_33      0.0270164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9771
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.749
_diffrn_reflns_theta_min         2.907
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_description       bulk
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 1101 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.006(19)
_refine_ls_extinction_coef       0.0236(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2501
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0373P)^2^+0.1468P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.774
_reflns_number_gt                2425
_reflns_number_total             2501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc09306f2.cif
_cod_data_source_block           C6H9N2SO2-NO3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1577091.cif.
;
_cod_original_cell_volume        964.26(10)
_cod_database_code               1577091
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All N(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C2(H2), C6(H6)
2.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_shelx_res_checksum              49643
_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 1.215
_oxdiff_exptl_absorpt_empirical_full_min 0.781