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_7132744
_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         314.11
_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                90.762(2)
_cell_angle_beta                 100.271(2)
_cell_angle_gamma                94.709(2)
_cell_formula_units_Z            4
_cell_length_a                   8.3590(2)
_cell_length_b                   11.6452(2)
_cell_length_c                   16.1214(3)
_cell_measurement_reflns_used    22048
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      79.4220
_cell_measurement_theta_min      3.7830
_cell_volume                     1538.31(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      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_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     63.00 118.00   0.50    0.40    --  111.50   0.00 -60.00  110
  2  \w    108.00 178.00   0.50    0.40    --  111.50  30.00 -90.00  140
  3  \w    108.00 178.00   0.50    0.40    --  111.50  30.00  30.00  140
  4  \w    108.00 178.00   0.50    0.40    --  111.50  30.00  60.00  140
  5  \w     98.00 178.00   0.50    0.40    --  111.50  61.00 120.00  160
  6  \w     63.00 118.00   0.50    0.40    --  111.50   0.00  60.00  110
  7  \w    -99.00 -44.00   0.50    0.30    --  -50.49   0.00-180.00  110
  8  \w   -101.00 -24.00   0.50    0.40    --  -90.00 146.00  60.00  154
  9  \w   -101.00 -24.00   0.50    0.30    --  -50.49 146.00  60.00  154
 10  \w    -85.00 -18.00   0.50    0.40    --  -90.00 125.00-105.00  134
 11  \w    -86.00 -13.00   0.50    0.30    --  -50.49 125.00-105.00  146
 12  \w    -55.00  21.00   0.50    0.30    --  -50.49  19.00-150.00  152
 13  \w     41.00  76.00   0.50    0.40    --  111.50 -45.00 150.00   70
 14  \w     41.00  76.00   0.50    0.40    --  111.50 -45.00 120.00   70
 15  \w     40.00  66.00   0.50    0.40    --  111.50 -30.00 -30.00   52
 16  \w     40.00  66.00   0.50    0.40    --  111.50 -30.00-150.00   52
 17  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00-120.00  130
 18  \w     46.00 107.00   0.50    0.30    --   50.49-146.00  10.00  122
 19  \w     46.00 127.00   0.50    0.40    --  111.50-146.00  10.00  162
 20  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00-180.00  130
 21  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00  60.00  130
 22  \w     41.00 106.00   0.50    0.40    --  111.50 -94.00  90.00  130
 23  \w     41.00 111.00   0.50    0.40    --  111.50-125.00 176.00  140
 24  \w     34.00  95.00   0.50    0.30    --   50.49-125.00 176.00  122
 25  \w     81.00 169.00   0.50    0.40    --  111.50 146.00  60.00  176
 26  \w     95.00 178.00   0.50    0.40    --  111.50 125.00 120.00  166
 27  \w     95.00 178.00   0.50    0.40    --  111.50 125.00-105.00  166
 28  \w   -122.00 -73.00   0.50    0.30    --  -50.49-125.00 176.00   98
 29  \w   -161.00 -73.00   0.50    0.40    --  -90.00-125.00 176.00  176
 30  \w   -122.00 -59.00   0.50    0.30    --  -50.49-146.00  10.00  126
 31  \w   -152.00 -59.00   0.50    0.40    --  -90.00-146.00  10.00  186
 32  \w   -122.00 -31.00   0.50    0.30    --  -50.49 -77.00  60.00  182
 33  \w   -161.00 -70.00   0.50    0.40    --  -90.00 -77.00   0.00  182
 34  \w   -122.00 -31.00   0.50    0.30    --  -50.49 -77.00 -30.00  182
 35  \w   -122.00 -31.00   0.50    0.30    --  -50.49 -77.00-120.00  182
 36  \w   -161.00 -70.00   0.50    0.40    --  -90.00 -77.00-150.00  182
 37  \w   -161.00 -80.00   0.50    0.40    --  -90.00 -77.00 -90.00  162
 38  \w   -122.00 -39.00   0.50    0.30    --  -50.49 -57.00  90.00  166
 39  \w   -122.00 -39.00   0.50    0.30    --  -50.49 -57.00 150.00  166
;
_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      -0.0651231000
_diffrn_orient_matrix_UB_12      -0.0421406000
_diffrn_orient_matrix_UB_13      0.0788687000
_diffrn_orient_matrix_UB_21      0.1598088000
_diffrn_orient_matrix_UB_22      0.0501478000
_diffrn_orient_matrix_UB_23      0.0562327000
_diffrn_orient_matrix_UB_31      -0.0745829000
_diffrn_orient_matrix_UB_32      0.1155138000
_diffrn_orient_matrix_UB_33      0.0075410000
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31801
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.332
_diffrn_reflns_theta_min         3.810
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87940
_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    1.356
_exptl_crystal_description       irregular
_exptl_crystal_F_000             648
_exptl_crystal_preparation       oil
_exptl_crystal_recrystallization_method DCM
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0020(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   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.6760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5698
_reflns_number_total             6368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05996k2.cif
_cod_data_source_block           pm3_20_dcm_test_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               7132744
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H14N2F3B
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.815
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C1(H1), C2(H2), C5(H5), C22(H22), C21(H21), C30(H30),
 C4(H4), C28(H28), C13(H13), C24(H24), C31(H31), C7(H7), C34(H34), C11(H11),
 C14(H14), C17(H17), C32(H32), C25(H25), C27(H27), C8(H8), C10(H10), C26(H26),
 C9(H9), C33(H33), C16(H16), C15(H15)
;
_shelx_res_checksum              84315
_shelx_hkl_checksum              43776
_olex2_exptl_crystal_mounting_method oil
_olex2_submission_original_sample_id PM3_20_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 1.170
_oxdiff_exptl_absorpt_empirical_full_min 0.833