[(C<sub>5</sub>H<sub>6</sub>N<sub>2</sub>)<sub>2</sub>H](Sb<sub>4</sub>F<sub>13</sub>): a polyfluoroantimonite with a strong second harmonic generation effect.
Wu, Jia-Hang; Hu, Chun-Li; Li, Ya-Feng; Mao, Jiang-Gao; Kong, Fang; Chemical science 15 (2024) 8071–8079; doi:10.1039/d4sc01716a

data_1571506
_publ_section_title
;
 [(C<sub>5</sub>H<sub>6</sub>N<sub>2</sub>)<sub>2</sub>H](Sb<sub>4</sub>F<sub>13</sub>):
 a polyfluoroantimonite with a strong second harmonic generation effect.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              8071
_journal_page_last               8079
_journal_paper_doi               10.1039/d4sc01716a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'F13 Sb4, C5 H7 N2, C5 H6 N2'
_chemical_formula_sum            'C10 H13 F13 N4 Sb4'
_chemical_formula_weight         923.24
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-12-04 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                101.002(4)
_cell_angle_beta                 105.247(4)
_cell_angle_gamma                106.829(4)
_cell_formula_units_Z            1
_cell_length_a                   7.2222(3)
_cell_length_b                   8.1293(4)
_cell_length_c                   10.3779(4)
_cell_measurement_reflns_used    6384
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      28.5020
_cell_measurement_theta_min      3.7820
_cell_volume                     538.65(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -12.00  65.00   1.00    1.00    --    6.30  58.00 -48.00   77
  2  \w     -9.00  32.00   1.00    1.00    --    6.30 -58.00 170.00   41
  3  \w    -33.00  61.00   1.00    1.00    --   -7.31  58.00 -48.00   94
  4  \w    -76.00 -23.00   1.00    1.00    --   -7.31 -58.00 170.00   53
  5  \w    -49.00  -5.00   1.00    1.00    --   -7.31 104.00  53.78   44
  6  \w    -66.00 -28.00   1.00    1.00    --   -7.31 132.00-155.59   38
  7  \w    -66.00 -31.00   1.00    1.00    --   -7.31 132.00 -47.32   35
  8  \w    -41.00  69.00   1.00    1.00    --   -7.31  19.00-180.00  110
  9  \w    -27.00  14.00   1.00    1.00    --   -7.31  57.00  30.00   41
 10  \w     36.00  61.00   1.00    1.00    --   -7.31  57.00  30.00   25
 11  \w    -78.00  13.00   1.00    1.00    --   -7.31 -38.00   0.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1071935000
_diffrn_orient_matrix_UB_12      0.0179129000
_diffrn_orient_matrix_UB_13      0.0258723000
_diffrn_orient_matrix_UB_21      0.0150510000
_diffrn_orient_matrix_UB_22      0.0843196000
_diffrn_orient_matrix_UB_23      0.0442656000
_diffrn_orient_matrix_UB_31      -0.0132357000
_diffrn_orient_matrix_UB_32      -0.0404546000
_diffrn_orient_matrix_UB_33      0.0533606000
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9297
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         3.338
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.846
_exptl_crystal_description       needle
_exptl_crystal_F_000             422
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 1680 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3745
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0207P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0504
_reflns_Friedel_coverage         0.974
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                3613
_reflns_number_total             3745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01716a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1571505--1571506.cif.'
_cod_original_cell_volume        538.65(4)
_cod_database_code               1571506
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), N1(H1), C2(H2), C5(H5), C9(H9), C7(H7), C10(H10), C4(H4), C8(H8)
2.b X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N2(H2A,H2B)
;
_shelx_res_checksum              2368
_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 1.793
_oxdiff_exptl_absorpt_empirical_full_min 0.802