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_7062692
_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'
_chemical_formula_sum            'C39 H19 B F10 N2 O'
_chemical_formula_weight         732.37
_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             2023-08-12
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2023-08-19 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                109.877(2)
_cell_angle_beta                 90.082(2)
_cell_angle_gamma                107.239(2)
_cell_formula_units_Z            2
_cell_length_a                   7.88670(10)
_cell_length_b                   13.1605(3)
_cell_length_c                   17.5175(4)
_cell_measurement_reflns_used    14789
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.6750
_cell_measurement_theta_min      3.5910
_cell_volume                     1622.46(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      4.00  51.00   0.50   47.37    --    1.32-122.00-140.00   94
  2  \w     20.00  69.00   0.50   47.37    --    1.32-151.00  58.00   98
  3  \w     26.00  65.00   0.50   47.37    --   -1.94-151.00  58.00   78
  4  \w     -2.00  34.00   0.50   47.37    --    1.32 -99.00  30.00   72
  5  \w    -39.00  12.00   0.50   47.37    --    1.32 -77.00   0.00  102
  6  \w    -37.00 -11.00   0.50   47.37    --    1.32 -77.00-120.00   52
  7  \w    -42.00  -9.00   0.50   47.37    --    1.32 -77.00-150.00   66
  8  \w    -52.00  13.00   0.50   47.37    --    1.32 -57.00  60.00  130
  9  \w    -66.00 -35.00   0.50   47.37    --   -1.94 -37.00 120.00   62
 10  \w    -40.00  19.00   0.50   47.37    --   -1.94 -77.00 -90.00  118
 11  \w    -25.00  16.00   0.50   47.37    --   -1.94  77.00-180.00   82
 12  \w     -1.00  65.00   0.50   47.37    --   -1.94  37.00  30.00  132
;
_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      -0.0459738000
_diffrn_orient_matrix_UB_12      -0.0501748000
_diffrn_orient_matrix_UB_13      0.0075899000
_diffrn_orient_matrix_UB_21      0.0275324000
_diffrn_orient_matrix_UB_22      0.0291949000
_diffrn_orient_matrix_UB_23      0.0424295000
_diffrn_orient_matrix_UB_31      -0.0781785000
_diffrn_orient_matrix_UB_32      0.0166748000
_diffrn_orient_matrix_UB_33      0.0045017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22626
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.470
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
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    1.499
_exptl_crystal_description       needle
_exptl_crystal_F_000             740
_exptl_crystal_preparation       Chloroform/n-hexane
_exptl_crystal_recrystallization_method 'slow evaoporation'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.7555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5241
_reflns_number_total             5704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03025c2.cif
_cod_data_source_block           acm-ta-1_autored
_cod_depositor_comments
'Adding full bibliography for 7062692--7062694.cif.'
_cod_original_cell_volume        1622.45(6)
_cod_database_code               7062692
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C156 H76 B4 F40 N8 O4 '
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.981
_diffrn_oxdiff_digest_frames
;
012d3b8fb4e2e2d4f0cdfd677b431afc1c01086aaf7
;
_diffrn_oxdiff_digest_hkl
;
01b09d5cb496130a59cba2fdb8f32f1d97ba45
;
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C18(H18), C24(H24), C22(H22), C14(H14), C23(H23), C12(H12), C3(H3),
 C6(H6), C4(H4), C21(H21), C5(H5), C8(H8), C11(H11), C17(H17), C9(H9), C15(H15),
  C10(H10), C16(H16)
;
_shelx_res_checksum              67584
_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 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.778