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_7062694
_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_absolute_configuration unk
_chemical_formula_moiety         'C41 H24 B F10 N3 O, 0.5[CHCl3]'
_chemical_formula_sum            'C41 H24 B F10 N3 O'
_chemical_formula_weight         775.475
_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'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-19
_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                90
_cell_angle_beta                 107.763(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4589(13)
_cell_length_b                   12.9868(10)
_cell_length_c                   12.6311(11)
_cell_measurement_reflns_used    11938
_cell_measurement_temperature    113(18)
_cell_measurement_theta_max      29.5490
_cell_measurement_theta_min      3.5510
_cell_volume                     1946.3(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      113(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9884
_diffrn_measured_fraction_theta_max 0.9797
_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     -3.00  43.00   0.50   50.06    --    1.32  20.00 153.00   92
  2  \w    -36.00   7.00   0.50   50.06    --    1.32 -20.00 -13.00   86
  3  \w     -7.00  59.00   0.50   50.06    --   -1.94  20.00 153.00  132
  4  \w    -68.00 -39.00   0.50   50.06    --   -1.94 -20.00 -13.00   58
  5  \w      0.00  54.00   0.50   50.06    --    1.32  37.00-180.00  108
  6  \w     23.00  58.00   0.50   50.06    --    1.32-133.00 -72.85   70
  7  \w    -10.00  19.00   0.50   50.06    --    1.32 -99.00 120.00   58
  8  \w    -52.00   4.00   0.50   50.06    --    1.32 -37.00 -30.00  112
  9  \w    -69.00 -44.00   0.50   50.06    --   -1.94 149.00-163.82   50
 10  \w    -68.00 -43.00   0.50   50.06    --   -1.94 148.00 135.39   50
 11  \w    -14.00  32.00   0.50   50.06    --   -1.94 -99.00  90.00   92
 12  \w    -52.00 -27.00   0.50   50.06    --   -1.94 123.00 125.42   50
 13  \w    -53.00 -28.00   0.50   50.06    --   -1.94 125.00-128.90   50
 14  \w    -49.00 -24.00   0.50   50.06    --   -1.94 118.00 173.04   50
 15  \w    -48.00 -23.00   0.50   50.06    --   -1.94 117.00-115.52   50
 16  \w    -15.00  34.00   0.50   50.06    --   -1.94 -99.00 150.00   98
;
_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      -0.0596151000
_diffrn_orient_matrix_UB_12      0.0035089000
_diffrn_orient_matrix_UB_13      -0.0215933000
_diffrn_orient_matrix_UB_21      0.0047122000
_diffrn_orient_matrix_UB_22      0.0132894000
_diffrn_orient_matrix_UB_23      -0.0528249000
_diffrn_orient_matrix_UB_31      -0.0029670000
_diffrn_orient_matrix_UB_32      -0.0528233000
_diffrn_orient_matrix_UB_33      -0.0147199000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.9884
_diffrn_reflns_Laue_measured_fraction_max 0.9797
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34168
_diffrn_reflns_point_group_measured_fraction_full 0.9838
_diffrn_reflns_point_group_measured_fraction_max 0.9600
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51080
_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_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             788.707
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.5086
_refine_diff_density_min         -0.3827
_refine_diff_density_rms         0.0835
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.6(3)
_refine_ls_d_res_high            0.8002
_refine_ls_d_res_low             6.1114
_refine_ls_goodness_of_fit_ref   1.0403
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7671
_refine_ls_number_restraints     1483
_refine_ls_restrained_S_all      0.9455
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+4.0750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2032
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.938
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                6829
_reflns_number_total             7671
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj03025c2.cif
_cod_data_source_block           KV-ACM-SHA-2
_cod_depositor_comments
'Adding full bibliography for 7062692--7062694.cif.'
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_original_formula_sum        'C41 H24 B1 F10 N3 O1'
_cod_database_code               7062694
_chemical_oxdiff_formula         'C84 H48 B4 F24 N4 O6 Cl1 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3A-C25 \\sim N3-C25
 with sigma of 0.02
 N3A-C28A \\sim N3-C28
 with sigma of 0.02
 N3A-C29A \\sim N3-C29
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N3 \\sim C25 \\sim C29 \\sim C28 \\sim C28A \\sim N3A \\sim C29A: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.01 within 1.7A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C25, C29, C28, C28A, N3A, C29A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C28A)=Sof(H28d)=Sof(H28e)=Sof(H28f)=Sof(N3A)=Sof(C29A)=Sof(H29d)=
 Sof(H29e)=Sof(H29f)=1-FVAR(1)
 Sof(N3)=Sof(C29)=Sof(H29a)=Sof(H29b)=Sof(H29c)=Sof(C28)=Sof(H28a)=Sof(H28b)=
 Sof(H28c)=FVAR(1)
 Fixed X: N3(0.79158) C25(0.699301) C29(0.7975) C28(0.84428) C28A(0.84554)
 N3A(0.81341) C29A(0.837029)
 Fixed Y: N3(0.351311) C25(0.4234) C29(0.237629) C28(0.39709) C28A(0.39689)
 N3A(0.39915) C29A(0.29427)
 Fixed Z: N3(0.433749) C25(0.40734) C29(0.42697) C28(0.553741) C28A(0.60239)
 N3A(0.473049) C29A(0.440189)
7.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C4(H4), C5(H5), C19(H19), C11(H11), C17(H17), C27(H27),
 C15(H15), C26(H26), C20(H20), C21(H21), C14(H14), C12(H12), C18(H18), C13(H13),
  C3(H3), C2(H2)
7.b Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C28(H28a,H28b,H28c), C28A(H28d,H28e,H28f), C29A(H29d,
 H29e,H29f)
;
_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 2.550
_oxdiff_exptl_absorpt_empirical_full_min 0.434