Synthesis, structural, and photophysical properties of pyrazolyl bis(pentafluorophenyl)boron complexes
Murali, Anna Chandrasekar; Pratakshya, Preeta; Patel, Pratiksha; Nayak, Prakash; Peruncheralathan, Saravanan; Venkatasubbaiah, Krishnan; New Journal of Chemistry 47 (2023) 17835–17842; doi:10.1039/D3NJ03025C

data_7062693
_publ_section_title
;
 Synthesis, structural, and photophysical properties of pyrazolyl
 bis(pentafluorophenyl)boron complexes
;
_journal_issue                   38
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17835
_journal_page_last               17842
_journal_paper_doi               10.1039/D3NJ03025C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C39 H19 B F10 N2 O, 1[CHCl3]'
_chemical_formula_sum            'C39 H19 B F10 N2 O'
_chemical_formula_weight         732.406
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-19 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                75.6912(15)
_cell_angle_beta                 81.6746(17)
_cell_angle_gamma                78.4570(18)
_cell_formula_units_Z            2
_cell_length_a                   8.8800(2)
_cell_length_b                   14.0601(3)
_cell_length_c                   16.9083(3)
_cell_measurement_reflns_used    18212
_cell_measurement_temperature    299.6(9)
_cell_measurement_theta_max      75.0590
_cell_measurement_theta_min      3.7900
_cell_volume                     1994.07(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.6(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9925
_diffrn_measured_fraction_theta_max 0.9385
_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   -102.00 -30.00   0.50    2.10    --  -38.50 -52.00-161.00  144
  2  \w    -46.00  25.00   0.50    2.10    --  -38.50  52.00 -16.00  142
  3  \w     41.00 113.00   0.50    2.10    --   49.31  52.00 -16.00  144
  4  \w    -14.00  57.00   0.50    2.10    --   49.31 -52.00-161.00  142
  5  \w     95.00 166.00   0.50    8.44    --  102.63  52.00 -16.00  142
  6  \w     39.00 111.00   0.50    8.44    --  102.63 -52.00-161.00  144
  7  \w    -44.00  31.00   0.50    2.10    --  -38.50  19.00  60.00  150
  8  \w   -108.00 -33.00   0.50    2.10    --  -38.50 -19.00-150.00  150
  9  \w   -101.00 -26.00   0.50    2.10    --  -38.50 -60.00 112.94  150
 10  \w     28.00 100.00   0.50    2.10    --   49.31-125.00  60.00  144
 11  \w     28.00 100.00   0.50    2.10    --   49.31-125.00-120.00  144
 12  \w     34.00 107.00   0.50    8.44    --  102.63 -94.00-150.00  146
 13  \w     38.00 112.00   0.50    8.44    --  102.63-125.00-150.00  148
 14  \w     34.00 107.00   0.50    8.44    --  102.63 -94.00   0.00  146
 15  \w     98.00 167.00   0.50    8.44    --  102.63  45.00 -30.00  138
 16  \w     38.00 112.00   0.50    8.44    --  102.63-125.00-180.00  148
 17  \w    103.00 167.00   0.50    8.44    --  102.63  77.00   0.00  128
 18  \w     38.00 112.00   0.50    8.44    --  102.63-125.00 -30.00  148
 19  \w     38.00 107.00   0.50    8.44    --  102.63 -45.00  60.00  138
 20  \w     38.00 107.00   0.50    8.44    --  102.63 -45.00 -90.00  138
 21  \w     92.00 166.00   0.50    8.44    --  102.63  56.00  73.90  148
 22  \w    103.00 167.00   0.50    8.44    --  102.63  77.00-120.00  128
 23  \w     38.00 126.00   0.50    8.44    --  102.63 -77.00-150.00  176
 24  \w     98.00 167.00   0.50    8.44    --  102.63  45.00-150.00  138
 25  \w    103.00 167.00   0.50    8.44    --  102.63  77.00 150.00  128
 26  \w     38.00 107.00   0.50    8.44    --  102.63 -45.00 -30.00  138
 27  \w     34.00 107.00   0.50    8.44    --  102.63 -94.00  60.00  146
 28  \w    103.00 167.00   0.50    8.44    --  102.63  77.00 -90.00  128
 29  \w     34.00 107.00   0.50    8.44    --  102.63 -94.00 120.00  146
 30  \w    103.00 167.00   0.50    8.44    --  102.63  77.00  90.00  128
 31  \w     99.00 171.00   0.50    8.44    --  102.63  30.00-120.00  144
 32  \w     34.00 107.00   0.50    8.44    --  102.63 -94.00-120.00  146
 33  \w     34.00 108.00   0.50    8.44    --  102.63-106.00  28.93  148
 34  \w     38.00 126.00   0.50    8.44    --  102.63 -77.00   0.00  176
 35  \w   -102.00 -17.00   0.50    2.10    --  -38.50 -74.00 -38.50  170
 36  \w   -102.00 -42.00   0.50    2.10    --  -38.50 -73.00  54.06  120
 37  \w     38.00 112.00   0.50    2.10    --   49.31  57.00-180.00  148
 38  \w     38.00 112.00   0.50    2.10    --   49.31  57.00 120.00  148
 39  \w     38.00 112.00   0.50    2.10    --   49.31  57.00-120.00  148
 40  \w     38.00 112.00   0.50    2.10    --   49.31  57.00  30.00  148
 41  \w     38.00 112.00   0.50    2.10    --   49.31  57.00 -60.00  148
 42  \w     38.00 112.00   0.50    2.10    --   49.31  57.00  60.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1223874000
_diffrn_orient_matrix_UB_12      -0.0954098000
_diffrn_orient_matrix_UB_13      0.0055454000
_diffrn_orient_matrix_UB_21      -0.0814577000
_diffrn_orient_matrix_UB_22      -0.0335849000
_diffrn_orient_matrix_UB_23      -0.0602845000
_diffrn_orient_matrix_UB_31      0.1002920000
_diffrn_orient_matrix_UB_32      0.0542458000
_diffrn_orient_matrix_UB_33      -0.0725719000
_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  0.0632
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.9925
_diffrn_reflns_Laue_measured_fraction_max 0.9385
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37626
_diffrn_reflns_point_group_measured_fraction_full 0.9925
_diffrn_reflns_point_group_measured_fraction_max 0.9385
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         78.42
_diffrn_reflns_theta_min         3.77
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       plate
_exptl_crystal_F_000             743.263
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.2442
_refine_diff_density_min         -0.3934
_refine_diff_density_rms         0.0560
_refine_ls_d_res_high            0.7869
_refine_ls_d_res_low             11.7389
_refine_ls_goodness_of_fit_ref   1.0312
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    38
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0312
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          -0.0023
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1005P)^2^+0.3123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1767
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6455
_reflns_number_total             8039
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj03025c2.cif
_cod_data_source_block           KV-ACM-TPPPF
_cod_depositor_comments
'Adding full bibliography for 7062692--7062694.cif.'
_cod_original_formula_sum        'C39 H19 B1 F10 N2 O1'
_cod_database_code               7062693
_chemical_oxdiff_formula         'C23 H23 B23 N23 O23 F23 Cl1 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C2(H2), C5(H5), C17(H17), C18(H18), C27(H27), C3(H3), C11(H11),
 C4(H4), C19(H19), C23(H23), C20(H20), C12(H12), C15(H15), C13(H13), C26(H26),
 C14(H14), C25(H25), C24(H24)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.239
_oxdiff_exptl_absorpt_empirical_full_min 0.331