O,S-Chelated bis(pentafluorophenyl)boron and diphenylboron-β-thioketonates: synthesis, photophysical, electrochemical and NLO properties.
Murali, Anna Chandrasekar; Panda, Rudrashish; Kannan, Ramkumar; Das, Ritwick; Venkatasubbaiah, Krishnan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17263–17271; doi:10.1039/d4dt02471k

data_1572683
_publ_section_title
;
 O,S-Chelated bis(pentafluorophenyl)boron and
 diphenylboron-&#x3b2;-thioketonates: synthesis, photophysical,
 electrochemical and NLO properties.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17263
_journal_page_last               17271
_journal_paper_doi               10.1039/d4dt02471k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H13 B F10 O S'
_chemical_formula_sum            'C28 H13 B F10 O S'
_chemical_formula_weight         598.25
_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     iterative
_audit_creation_date             2024-04-25
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2024-08-30 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                112.846(3)
_cell_angle_beta                 104.805(4)
_cell_angle_gamma                93.529(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0473(3)
_cell_length_b                   11.9367(3)
_cell_length_c                   12.7968(5)
_cell_measurement_reflns_used    14156
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.9870
_cell_measurement_theta_min      3.9520
_cell_volume                     1211.08(8)
_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    'olex2.solve (Bourhis et al., 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 0.999
_diffrn_measured_fraction_theta_max 0.964
_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    -62.00  26.00   0.50    0.31    --  -38.50  78.00 -37.00  176
  2  \w    103.00 172.00   0.50    1.24    --  107.46  78.00 -37.00  138
  3  \w     43.00 131.00   0.50    1.24    --  107.46 -78.00-162.00  176
  4  \w    -86.00  -6.00   0.50    0.31    --  -38.50 125.00  60.00  160
  5  \w   -102.00 -20.00   0.50    0.31    --  -38.50 -71.00-137.36  164
  6  \w   -101.00 -27.00   0.50    0.31    --  -38.50 -57.00-180.00  148
  7  \w     46.00 116.00   0.50    0.31    --   49.06  37.00   0.00  140
  8  \w    -17.00  52.00   0.50    0.31    --   49.06 -37.00-120.00  138
  9  \w    -16.00  73.00   0.50    0.31    --   49.06 -78.00-162.00  178
 10  \w     34.00 112.00   0.50    0.31    --   49.06  64.00  35.48  156
 11  \w     39.00 107.00   0.50    1.24    --  107.46 -94.00-150.00  136
 12  \w     95.00 170.00   0.50    1.24    --  107.46  61.00 -60.00  150
 13  \w     43.00 112.00   0.50    1.24    --  107.46 -45.00-180.00  138
 14  \w    103.00 172.00   0.50    1.24    --  107.46  45.00 -60.00  138
 15  \w     39.00 107.00   0.50    1.24    --  107.46 -94.00  30.00  136
 16  \w     39.00 107.00   0.50    1.24    --  107.46 -94.00-180.00  136
 17  \w     39.00 107.00   0.50    1.24    --  107.46 -94.00  60.00  136
 18  \w     45.00 113.00   0.50    1.24    --  107.46-125.00-150.00  136
 19  \w    103.00 172.00   0.50    1.24    --  107.46  77.00 -30.00  138
 20  \w     40.00 108.00   0.50    1.24    --  107.46-105.00 -21.44  136
 21  \w    103.00 172.00   0.50    1.24    --  107.46  77.00 -90.00  138
 22  \w     97.00 170.00   0.50    1.24    --  107.46 125.00  30.00  146
 23  \w     39.00 111.00   0.50    1.24    --  107.46 -30.00  30.00  144
 24  \w     39.00 107.00   0.50    1.24    --  107.46 -94.00 -30.00  136
 25  \w     45.00 121.00   0.50    1.24    --  107.46 -61.00   0.00  152
 26  \w     99.00 176.00   0.50    1.24    --  107.46  15.00-120.00  154
 27  \w     43.00 112.00   0.50    1.24    --  107.46 -45.00 -90.00  138
 28  \w     43.00 131.00   0.50    1.24    --  107.46 -77.00  60.00  176
 29  \w     39.00 111.00   0.50    1.24    --  107.46 -30.00 -90.00  144
 30  \w    103.00 172.00   0.50    1.24    --  107.46  77.00-180.00  138
 31  \w     39.00 116.00   0.50    1.24    --  107.46 -15.00 -30.00  154
 32  \w   -101.00 -22.00   0.50    0.31    --  -38.50 -67.00 -64.34  158
 33  \w     31.00 112.00   0.50    0.31    --   49.06  71.00 179.88  162
 34  \w     32.00 112.00   0.50    0.31    --   49.06  68.00 109.69  160
;
_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      0.0052032000
_diffrn_orient_matrix_UB_12      0.1188533000
_diffrn_orient_matrix_UB_13      -0.0206151000
_diffrn_orient_matrix_UB_21      0.0445139000
_diffrn_orient_matrix_UB_22      -0.0672869000
_diffrn_orient_matrix_UB_23      -0.1142383000
_diffrn_orient_matrix_UB_31      -0.1733659000
_diffrn_orient_matrix_UB_32      -0.0402457000
_diffrn_orient_matrix_UB_33      -0.0729734000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18134
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.713
_diffrn_reflns_theta_min         3.934
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44492
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_preparation       Dichloromethane/n-hexane
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.0027(6)
_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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+0.9577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4787
_reflns_number_total             5052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02471k2.cif
_cod_data_source_block           kv_acm_ar_6_auto
_cod_depositor_comments
'Adding full bibliography for 1572679--1572683.cif.'
_cod_database_code               1572683
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H S O B F'
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.785
_diffrn_oxdiff_digest_frames
;
010c848b99ee26b52c71b9611845d65ef3000371241
;
_diffrn_oxdiff_digest_hkl
;
01452ea1f92534b068a45bb8ee9fd999b3481c
;
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C6(H6), C2(H2), C8(H8), C16(H16), C14(H14), C5(H5),
 C9(H9), C15(H15)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              3712
_shelx_hkl_checksum              77376
_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 2.736
_oxdiff_exptl_absorpt_empirical_full_min 0.534