A multi-chromic boron trifluoride-pyridyl Lewis adduct.
McDonald, Peter W.; Ritchie, Chris; Chemical communications (Cambridge, England) 60 (2024) 3051–3054; doi:10.1039/d3cc05996k

data_7132743
_publ_section_title
;
 A multi-chromic boron trifluoride-pyridyl Lewis adduct.
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3051
_journal_page_last               3054
_journal_paper_doi               10.1039/d3cc05996k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'B F4, C17 H15 N2'
_chemical_formula_sum            'C17 H15 B F4 N2'
_chemical_formula_weight         334.12
_chemical_name_systematic
'4-(diphenylamino)pyridin-1-ium tetrafluoroborate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-29 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.30620(10)
_cell_length_b                   7.70180(10)
_cell_length_c                   10.32470(10)
_cell_measurement_reflns_used    10156
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      78.3540
_cell_measurement_theta_min      4.3380
_cell_volume                     804.326(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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     41.00  76.00   0.50    0.10    --  111.50 -45.00   0.00   70
  2  \w     41.00  76.00   0.50    0.10    --  111.50 -45.00-150.00   70
  3  \w     41.00  76.00   0.50    0.10    --  111.50 -45.00 -90.00   70
  4  \w     41.00  76.00   0.50    0.10    --  111.50 -45.00 -30.00   70
  5  \w     41.00  76.00   0.50    0.10    --  111.50 -45.00 120.00   70
  6  \w     41.00  76.00   0.50    0.10    --  111.50 -45.00  60.00   70
  7  \w     41.00  76.00   0.50    0.10    --  111.50 -45.00  90.00   70
  8  \w     41.00  76.00   0.50    0.10    --  111.50 -45.00  30.00   70
  9  \w     40.00  66.00   0.50    0.10    --  111.50 -30.00 120.00   52
 10  \w     40.00  66.00   0.50    0.10    --  111.50 -30.00  30.00   52
 11  \w     40.00  66.00   0.50    0.10    --  111.50 -30.00  60.00   52
 12  \w     41.00  76.00   0.50    0.10    --  111.50 -45.00-180.00   70
 13  \w     40.00  66.00   0.50    0.10    --  111.50 -30.00-180.00   52
 14  \w     40.00  66.00   0.50    0.10    --  111.50 -30.00 -90.00   52
 15  \w     40.00  66.00   0.50    0.10    --  111.50 -30.00   0.00   52
 16  \w    104.00 178.00   0.50    0.10    --  111.50 109.00 -27.00  148
 17  \w     95.00 178.00   0.50    0.10    --  111.50 125.00 120.00  166
 18  \w     22.00  86.00   0.50    0.10    --   50.49-109.00-123.00  128
 19  \w     41.00 111.00   0.50    0.10    --  111.50-125.00   0.00  140
 20  \w     41.00 111.00   0.50    0.10    --  111.50-125.00 -30.00  140
 21  \w     41.00 111.00   0.50    0.10    --  111.50-125.00 -60.00  140
 22  \w     41.00 107.00   0.50    0.10    --  111.50-109.00-123.00  132
 23  \w    -82.00  -1.00   0.50    0.10    --  -50.49 109.00 -27.00  162
 24  \w    -68.00 -17.00   0.50    0.10    --  -90.00  30.00-180.00  102
 25  \w    -82.00 -18.00   0.50    0.10    --  -90.00 109.00 -27.00  128
 26  \w    -99.00 -44.00   0.50    0.10    --  -50.49   0.00   0.00  110
 27  \w   -122.00 -64.00   0.50    0.10    --  -50.49 -57.00 -30.00  116
 28  \w   -122.00 -73.00   0.50    0.10    --  -50.49-125.00  90.00   98
 29  \w   -161.00 -82.00   0.50    0.10    --  -90.00-109.00-123.00  158
 30  \w   -122.00 -31.00   0.50    0.10    --  -50.49 -77.00-180.00  182
 31  \w   -146.00-121.00   0.50    0.10    --  -90.00-109.00-123.00   50
 32  \w     68.00 112.00   0.50    0.10    --  111.50-128.00 156.00   88
 33  \w     -9.00  17.00   0.50    0.10    --  -50.49  38.00 120.00   52
 34  \w    -78.00 -52.00   0.50    0.10    --  -50.49   0.00 -60.00   52
 35  \w    -42.00 -11.00   0.50    0.10    --  -50.49  38.00 120.00   62
 36  \w    111.00 144.00   0.50    0.10    --  111.50  30.00  60.00   66
 37  \w     48.00  76.00   0.50    0.10    --  111.50 -45.00 -60.00   56
 38  \w     79.00 105.00   0.50    0.10    --  111.50 -94.00   0.00   52
 39  \w     83.00 109.00   0.50    0.10    --  111.50-125.00-180.00   52
 40  \w     66.00 106.00   0.50    0.10    --  111.50   0.00 -60.00   80
 41  \w    109.00 135.00   0.50    0.10    --  111.50  45.00 120.00   52
 42  \w    140.00 172.00   0.50    0.10    --  111.50  45.00 120.00   64
 43  \w     61.00 107.00   0.50    0.10    --  111.50-125.00 120.00   92
 44  \w     47.00  73.00   0.50    0.10    --  111.50 -94.00-180.00   52
 45  \w     79.00 105.00   0.50    0.10    --  111.50 -94.00 -60.00   52
 46  \w     40.00  65.00   0.50    0.10    --  111.50 -30.00-150.00   50
 47  \w    150.00 177.00   0.50    0.10    --  111.50  30.00  60.00   54
 48  \w     71.00  97.00   0.50    0.10    --  111.50 -94.00  30.00   52
 49  \w     49.00  75.00   0.50    0.10    --  111.50 -94.00 150.00   52
 50  \w     81.00 106.00   0.50    0.10    --  111.50 -94.00 150.00   50
 51  \w     65.00  91.00   0.50    0.10    --  111.50   0.00-120.00   52
 52  \w     76.00 110.00   0.50    0.10    --  111.50   0.00   0.00   68
 53  \w    -77.00 -52.00   0.50    0.10    --  -90.00 129.00-129.00   50
 54  \w     43.00  68.00   0.50    0.10    --   50.49-129.00 156.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0299621000
_diffrn_orient_matrix_UB_12      0.0482056000
_diffrn_orient_matrix_UB_13      0.1475652000
_diffrn_orient_matrix_UB_21      -0.0271751000
_diffrn_orient_matrix_UB_22      -0.1889472000
_diffrn_orient_matrix_UB_23      0.0360702000
_diffrn_orient_matrix_UB_31      0.1467765000
_diffrn_orient_matrix_UB_32      -0.0447702000
_diffrn_orient_matrix_UB_33      0.0068517000
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13391
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.960
_diffrn_reflns_theta_min         4.363
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80354
_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_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       irregular
_exptl_crystal_F_000             344
_exptl_crystal_preparation       oil
_exptl_crystal_recrystallization_method THF
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 1452 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_coef       0.0072(11)
_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   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0404P)^2^+0.1883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                3311
_reflns_number_total             3393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05996k2.cif
_cod_data_source_block           pm3_18_thf_1_auto
_cod_depositor_comments
'Adding full bibliography for 7132742--7132744.cif.'
_cod_database_code               7132743
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H14N2BF3
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.746
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C2(H2A), C7(H7), C15(H15), C13(H13), C4(H4), C11(H11), C16(H16),
 C1(H1), C5(H5), C8(H8), C10(H10), C9(H9), C14(H14)
;
_shelx_res_checksum              33783
_shelx_hkl_checksum              11013
_olex2_exptl_crystal_mounting_method oil
_olex2_submission_original_sample_id PM3_18_THF
_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 1.739
_oxdiff_exptl_absorpt_empirical_full_min 0.626