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_1572680
_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         'C31 H13 B F10 O S'
_chemical_formula_sum            'C31 H13 B F10 O S'
_chemical_formula_weight         634.28
_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             2023-05-23
_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                74.848(3)
_cell_angle_beta                 82.963(3)
_cell_angle_gamma                71.503(4)
_cell_formula_units_Z            2
_cell_length_a                   8.9743(4)
_cell_length_b                   11.7030(4)
_cell_length_c                   15.0237(4)
_cell_measurement_reflns_used    15154
_cell_measurement_temperature    109(13)
_cell_measurement_theta_max      75.2180
_cell_measurement_theta_min      3.9880
_cell_volume                     1443.00(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_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      109(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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   -103.00 -34.00   0.50    2.25    --  -38.50 -43.00  78.00  138
  2  \w     45.00 114.00   0.50    2.25    --   49.31  43.00-130.00  138
  3  \w    -16.00  53.00   0.50    2.25    --   49.31 -43.00  78.00  138
  4  \w     99.00 168.00   0.50    9.00    --  102.63  43.00-130.00  138
  5  \w     38.00 107.00   0.50    9.00    --  102.63 -43.00  78.00  138
  6  \w    -62.00  26.00   0.50    2.25    --  -38.50  77.00-120.00  176
  7  \w    -42.00  27.00   0.50    2.25    --  -38.50  43.00-130.00  138
  8  \w   -105.00 -35.00   0.50    2.25    --  -38.50 -37.00 120.00  140
  9  \w   -101.00 -27.00   0.50    2.25    --  -38.50 -57.00  60.00  148
 10  \w     24.00 100.00   0.50    2.25    --   49.31-125.00 -30.00  152
 11  \w     46.00 116.00   0.50    2.25    --   49.31  37.00-150.00  140
 12  \w     80.00 167.00   0.50    9.00    --  102.63  77.00-180.00  174
 13  \w     40.00 116.00   0.50    9.00    --  102.63 -61.00-150.00  152
 14  \w     34.00 110.00   0.50    9.00    --  102.63 -94.00   0.00  152
 15  \w     38.00 118.00   0.50    9.00    --  102.63-125.00   0.00  160
 16  \w     95.00 171.00   0.50    9.00    --  102.63  15.00-180.00  152
 17  \w     40.00 116.00   0.50    9.00    --  102.63 -61.00  90.00  152
 18  \w     40.00 116.00   0.50    9.00    --  102.63 -61.00 -60.00  152
 19  \w     99.00 171.00   0.50    9.00    --  102.63  30.00 120.00  144
 20  \w     40.00 116.00   0.50    9.00    --  102.63 -61.00   0.00  152
 21  \w     98.00 167.00   0.50    9.00    --  102.63  45.00  30.00  138
 22  \w     38.00 107.00   0.50    9.00    --  102.63 -45.00-150.00  138
 23  \w     38.00 118.00   0.50    9.00    --  102.63-125.00-150.00  160
 24  \w     99.00 171.00   0.50    9.00    --  102.63  30.00 -90.00  144
 25  \w     34.00 110.00   0.50    9.00    --  102.63 -94.00-150.00  152
 26  \w     95.00 171.00   0.50    9.00    --  102.63  15.00-150.00  152
 27  \w     98.00 167.00   0.50    9.00    --  102.63  45.00  90.00  138
 28  \w     38.00 107.00   0.50    9.00    --  102.63 -45.00 -90.00  138
 29  \w     38.00 118.00   0.50    9.00    --  102.63-125.00 120.00  160
 30  \w     94.00 168.00   0.50    9.00    --  102.63 125.00 120.00  148
 31  \w     38.00  90.00   0.50    2.25    --   49.31  57.00 -90.00  104
 32  \w     26.00 114.00   0.50    2.25    --   49.31  77.00 -30.00  176
;
_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      -0.0164508000
_diffrn_orient_matrix_UB_12      0.1354512000
_diffrn_orient_matrix_UB_13      -0.0516540000
_diffrn_orient_matrix_UB_21      0.1674050000
_diffrn_orient_matrix_UB_22      -0.0155726000
_diffrn_orient_matrix_UB_23      0.0258524000
_diffrn_orient_matrix_UB_31      0.0673279000
_diffrn_orient_matrix_UB_32      -0.0426508000
_diffrn_orient_matrix_UB_33      -0.0892784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0991
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19128
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.012
_diffrn_reflns_theta_min         4.099
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull light orange'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       needle
_exptl_crystal_F_000             636
_exptl_crystal_preparation       chloroform/hexane
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0893
_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^)+(0.1782P)^2^+1.6255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2742
_refine_ls_wR_factor_ref         0.2816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5135
_reflns_number_total             5833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02471k2.cif
_cod_data_source_block           kv-acm-nap-sobf5
_cod_depositor_comments
'Adding full bibliography for 1572679--1572683.cif.'
_cod_database_code               1572680
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H S  B F O'
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.785
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C43(H43), C3(H3), C40(H40), C2(H2), C5(H5), C8(H8),
 C44(H44), C41(H41), C42(H42), C7(H7), C6(H6)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89139
_shelx_hkl_checksum              10497
_shelx_fab_checksum              96116
_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 4.646
_oxdiff_exptl_absorpt_empirical_full_min 0.145