[(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_1571505
_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         'F7 Sb2, C6 H7 N2 O'
_chemical_formula_sum            'C6 H7 F7 N2 O Sb2'
_chemical_formula_weight         499.64
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-04 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                75.512(13)
_cell_angle_beta                 83.357(11)
_cell_angle_gamma                85.846(13)
_cell_formula_units_Z            2
_cell_length_a                   7.3227(10)
_cell_length_b                   7.4727(12)
_cell_length_c                   11.1037(16)
_cell_measurement_reflns_used    2485
_cell_measurement_temperature    295.68(10)
_cell_measurement_theta_max      29.4210
_cell_measurement_theta_min      4.2460
_cell_volume                     583.73(15)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.68(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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    -85.00   4.00   1.00    1.00    --  -12.30 -44.00-112.00   89
  2  \w    -27.00  61.00   1.00    1.00    --  -12.30  44.00  38.00   88
  3  \w     35.00  91.00   1.00    1.00    --   12.15 178.00 -60.00   56
  4  \w     36.00  99.00   1.00    1.00    --   12.15-178.00-150.00   63
  5  \w    -18.00  24.00   1.00    1.00    --  -12.30 -99.00-150.00   42
;
_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      0.0241948000
_diffrn_orient_matrix_UB_12      -0.0924305000
_diffrn_orient_matrix_UB_13      0.0307017000
_diffrn_orient_matrix_UB_21      -0.0767736000
_diffrn_orient_matrix_UB_22      -0.0311885000
_diffrn_orient_matrix_UB_23      -0.0212335000
_diffrn_orient_matrix_UB_31      0.0552235000
_diffrn_orient_matrix_UB_32      -0.0107110000
_diffrn_orient_matrix_UB_33      -0.0548130000
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5198
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.710
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40961
_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    2.843
_exptl_crystal_description       plate
_exptl_crystal_F_000             460
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       0.0192(6)
_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   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0172P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2035
_reflns_number_total             2558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01716a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1571505--1571506.cif.'
_cod_database_code               1571505
_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:
 N1(H1), C6(H6), C5(H5), C4(H4), C3(H3)
2.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_shelx_res_checksum              13005
_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 2.186
_oxdiff_exptl_absorpt_empirical_full_min 0.659