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_7132742
_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         'C17 H14 B F3 N2'
_chemical_formula_sum            'C17 H14 B F3 N2'
_chemical_formula_weight         628.22
_chemical_name_systematic        (4-(diphenylamino)pyridin-1-ium)trifluoroborate
_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             2023-11-29
_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                90.7320(10)
_cell_angle_beta                 99.9450(10)
_cell_angle_gamma                95.1060(10)
_cell_formula_units_Z            4
_cell_length_a                   8.48980(10)
_cell_length_b                   11.7179(2)
_cell_length_c                   16.2792(2)
_cell_measurement_reflns_used    14514
_cell_measurement_temperature    293
_cell_measurement_theta_max      79.5450
_cell_measurement_theta_min      3.7710
_cell_volume                     1588.18(4)
_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      air
_diffrn_ambient_temperature      293
_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 0.977
_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   -121.00 -38.00   0.50    1.01    --  -50.51 -58.00 103.00  166
  2  \w    -62.00  21.00   0.50    1.01    --  -50.51  58.00-116.00  166
  3  \w   -161.00 -78.00   0.50    5.00    --  -90.00 -58.00 103.00  166
  4  \w   -102.00 -18.00   0.50    5.00    --  -90.00  58.00-116.00  168
  5  \w    100.00 178.00   0.50    5.00    --  111.50  58.00-116.00  156
  6  \w     41.00 103.00   0.50    5.00    --  111.50 -58.00 103.00  124
  7  \w    -99.00 -44.00   0.50    1.01    --  -50.51   0.00 120.00  110
  8  \w   -121.00 -73.00   0.50    1.01    --  -50.51-125.00-180.00   96
  9  \w    -86.00 -13.00   0.50    1.01    --  -50.51 125.00  90.00  146
 10  \w      2.00  57.00   0.50    1.01    --   50.51   0.00  60.00  110
 11  \w    -20.00  63.00   0.50    1.01    --   50.51 -58.00 103.00  166
 12  \w     39.00 121.00   0.50    1.01    --   50.51  58.00-116.00  164
 13  \w    -20.00  62.00   0.50    1.01    --   50.51 -57.00  30.00  164
 14  \w    -68.00 -17.00   0.50    5.00    --  -90.00  30.00  90.00  102
 15  \w    -85.00 -18.00   0.50    5.00    --  -90.00 125.00 -60.00  134
 16  \w     40.00 116.00   0.50    5.00    --  111.50 -15.00 -60.00  152
 17  \w     41.00 131.00   0.50    5.00    --  111.50 -77.00-150.00  180
 18  \w     41.00 111.00   0.50    5.00    --  111.50-125.00 -90.00  140
 19  \w     40.00  66.00   0.50    5.00    --  111.50 -30.00   0.00   52
 20  \w     40.00  66.00   0.50    5.00    --  111.50 -30.00 150.00   52
 21  \w     40.00  66.00   0.50    5.00    --  111.50 -30.00 -90.00   52
 22  \w     41.00 106.00   0.50    5.00    --  111.50 -94.00  90.00  130
 23  \w     41.00  76.00   0.50    5.00    --  111.50 -45.00 -90.00   70
 24  \w     41.00  76.00   0.50    5.00    --  111.50 -45.00  90.00   70
 25  \w     41.00  76.00   0.50    5.00    --  111.50 -45.00  30.00   70
 26  \w     41.00 106.00   0.50    5.00    --  111.50 -94.00 120.00  130
 27  \w     41.00 106.00   0.50    5.00    --  111.50 -94.00-120.00  130
 28  \w     40.00  66.00   0.50    5.00    --  111.50 -30.00  90.00   52
 29  \w     95.00 178.00   0.50    5.00    --  111.50 125.00 150.00  166
 30  \w     41.00  76.00   0.50    5.00    --  111.50 -45.00-120.00   70
 31  \w    108.00 178.00   0.50    5.00    --  111.50  30.00 -90.00  140
 32  \w     41.00 106.00   0.50    5.00    --  111.50 -94.00   0.00  130
 33  \w     41.00 111.00   0.50    5.00    --  111.50-125.00-120.00  140
 34  \w     41.00 106.00   0.50    5.00    --  111.50 -94.00 -60.00  130
 35  \w     40.00  66.00   0.50    5.00    --  111.50 -30.00 120.00   52
 36  \w     41.00 106.00   0.50    5.00    --  111.50 -94.00 150.00  130
 37  \w     41.00 111.00   0.50    5.00    --  111.50-125.00  30.00  140
 38  \w     41.00 106.00   0.50    5.00    --  111.50 -94.00  60.00  130
 39  \w     41.00  76.00   0.50    5.00    --  111.50 -45.00 -60.00   70
 40  \w     40.00  66.00   0.50    5.00    --  111.50 -30.00-180.00   52
 41  \w     40.00  66.00   0.50    5.00    --  111.50 -30.00-150.00   52
 42  \w     40.00  66.00   0.50    5.00    --  111.50 -30.00  30.00   52
 43  \w     41.00 131.00   0.50    5.00    --  111.50 -77.00-120.00  180
 44  \w     92.00 178.00   0.50    5.00    --  111.50  77.00 150.00  172
 45  \w     63.00 118.00   0.50    5.00    --  111.50   0.00  30.00  110
 46  \w     43.00 106.00   0.50    5.00    --  111.50 -94.00 -90.00  126
 47  \w     68.00  99.00   0.50    5.00    --  111.50 -94.00 -30.00   62
 48  \w     45.00 106.00   0.50    5.00    --  111.50 -94.00  30.00  122
;
_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      0.0787312000
_diffrn_orient_matrix_UB_12      0.0637196000
_diffrn_orient_matrix_UB_13      -0.0668892000
_diffrn_orient_matrix_UB_21      0.1261689000
_diffrn_orient_matrix_UB_22      -0.0876567000
_diffrn_orient_matrix_UB_23      0.0063802000
_diffrn_orient_matrix_UB_31      -0.1100762000
_diffrn_orient_matrix_UB_32      -0.0754514000
_diffrn_orient_matrix_UB_33      -0.0687281000
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33396
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.400
_diffrn_reflns_theta_min         3.789
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86281
_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    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_preparation       oil
_exptl_crystal_recrystallization_method DCM
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0015(2)
_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   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.6708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5651
_reflns_number_total             6797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05996k2.cif
_cod_data_source_block           pm3_42_280k_auto
_cod_depositor_comments
;
Adding full bibliography for 7132742--7132744.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H28 B2 F6 N4'
_cod_original_formula_weight         628.22
_cod_original_formula_moiety         '2(C17 H14 B F3 N2)'
_cod_original_formula_units_Z            2
_cod_database_code               7132742
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C17H14N2BF3
_chemical_oxdiff_usercomment     'Clear colourless irregular block'
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C19(H19), C2(H2), C18(H18), C4(H4), C5(H5), C22(H22), C34(H34),
 C21(H21), C17(H17), C24(H24), C11(H11), C7(H7), C33(H33), C13(H13), C28(H28),
 C30(H30), C16(H16), C9(H9), C32(H32), C10(H10), C8(H8), C15(H15), C25(H25),
 C31(H31), C27(H27), C14(H14), C26(H26)
;
_shelx_res_checksum              66354
_shelx_hkl_checksum              63441
_olex2_exptl_crystal_mounting_method oil
_olex2_submission_original_sample_id PM3_42_DCM
_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 1.958
_oxdiff_exptl_absorpt_empirical_full_min 0.299