Crystal Structure of 1,3-Diphenyl-2,3-dihydro-1<i>H</i>-benzo[<i>d</i>][1,3]dithiole-1,3-dinium Bis(tetrafluoroborate) Acetonitrile Solvate
FUJII, Takayoshi; KURIBAYASHI, Megumi; KUBO, Kanji; X-ray Structure Analysis Online 37 (2021) 21–23; doi:10.2116/xraystruct.37.21

data_1563170
_publ_section_title
;
 Crystal Structure of
 1,3-Diphenyl-2,3-dihydro-1&lt;i&gt;H&lt;/i&gt;-benzo[&lt;i&gt;d&lt;/i&gt;][1,3]dithiole-1,3-dinium
 Bis(tetrafluoroborate) Acetonitrile Solvate
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              21
_journal_page_last               23
_journal_paper_doi               10.2116/xraystruct.37.21
_journal_volume                  37
_journal_year                    2021
_chemical_formula_moiety         'C19 H16 S2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C21 H19 B2 F8 N S2'
_chemical_formula_weight         523.11
_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             2020-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                79.659(2)
_cell_angle_beta                 77.822(2)
_cell_angle_gamma                78.551(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3368(2)
_cell_length_b                   8.9193(2)
_cell_length_c                   16.7407(4)
_cell_measurement_reflns_used    7432
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.5830
_cell_measurement_theta_min      2.3480
_cell_volume                     1180.22(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Rigaku HyPix-3000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.945
_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     25.00  94.00   0.50   16.70    --   20.00  54.00   0.00  138
  2  \w    -73.00 109.00   0.50   16.70    --   20.00  54.00-150.00  364
  3  \w    -72.00 -45.00   0.50   16.70    --   20.00  54.00 120.00   54
  4  \w     -5.00  54.00   0.50   16.70    --   20.00  54.00 120.00  118
  5  \w    -69.00  14.00   0.50   16.70    --   20.00  54.00 -90.00  166
  6  \w    -67.00  34.00   0.50   16.70    --   20.00  54.00 -30.00  202
  7  \w     38.00  63.00   0.50   16.70    --   20.00  54.00 -30.00   50
  8  \w    -73.00 -18.00   0.50   16.70    --   20.00  54.00  60.00  110
  9  \w     23.00  70.00   0.50   16.70    --   20.00  54.00  60.00   94
 10  \w    -68.00 -43.00   0.50   16.70    --   20.00  54.00  90.00   50
 11  \w    -23.00   2.00   0.50   16.70    --   20.00  54.00  90.00   50
 12  \w     44.00  69.00   0.50   16.70    --   20.00  54.00  90.00   50
 13  \w    -65.00 -40.00   0.50   16.70    --   20.00  54.00-120.00   50
 14  \w     45.00 103.00   0.50   16.70    --   20.00  54.00-120.00  116
 15  \w    -62.00  66.00   0.50   16.70    --   20.00  54.00 150.00  256
 16  \w     -7.00  20.00   0.50   16.70    --   20.00  54.00  30.00   54
 17  \w    -64.00 -37.00   0.50   16.70    --   20.00  54.00   0.00   54
;
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0139061000
_diffrn_orient_matrix_UB_12      -0.0819093000
_diffrn_orient_matrix_UB_13      0.0082009000
_diffrn_orient_matrix_UB_21      0.0115011000
_diffrn_orient_matrix_UB_22      0.0033946000
_diffrn_orient_matrix_UB_23      0.0403879000
_diffrn_orient_matrix_UB_31      -0.0864160000
_diffrn_orient_matrix_UB_32      0.0012620000
_diffrn_orient_matrix_UB_33      0.0148309000
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20814
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.448
_diffrn_reflns_theta_min         2.354
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.532
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1498P)^2^+0.6670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2373
_refine_ls_wR_factor_ref         0.2579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4830
_reflns_number_total             6773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            37_21_1.txt
_cod_data_source_block           exp_129
_cod_database_code               1563170
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         ku
_chemical_oxdiff_usercomment     'C19 H16 F8 S4 B2'
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.903
_reflns_odcompleteness_completeness 98.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1,H2)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H11), C3(H3), C9(H7), C15(H12), C6(H6), C5(H5), C10(H8), C4(H4), C17(H14),
  C11(H9), C19(H16), C12(H10), C16(H13), C18(H15)
2.c Idealised Me refined as rotating group:
 C20(H19,H18,H17)
;
_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 1.044
_oxdiff_exptl_absorpt_empirical_full_min 0.938