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_1572681
_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 H23 B O2 S'
_chemical_formula_sum            'C28 H23 B O2 S'
_chemical_formula_weight         434.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 98.258(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3139(2)
_cell_length_b                   19.4235(6)
_cell_length_c                   13.8886(4)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.8730
_cell_measurement_theta_min      3.9160
_cell_volume                     2219.55(11)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(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 0.976
_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    -71.00  22.00   0.50    5.98    --  -38.50  93.00  68.00  186
  2  \w      0.00  82.00   0.50    5.98    --   49.56 -93.00 -43.00  164
  3  \w     39.00 106.00   0.50   10.95    --  107.46 -93.00 -43.00  134
  4  \w    104.00 176.00   0.50   10.95    --  107.46  93.00  68.00  144
  5  \w   -105.00 -35.00   0.50    5.98    --  -38.50 -37.00 -30.00  140
  6  \w    -42.00  28.00   0.50    5.98    --  -38.50  37.00-180.00  140
  7  \w     38.00 113.00   0.50    5.98    --   49.56  57.00 150.00  150
  8  \w     39.00 107.00   0.50   10.95    --  107.46 -94.00 150.00  136
  9  \w     39.00 111.00   0.50   10.95    --  107.46 -30.00 150.00  144
 10  \w     39.00 107.00   0.50   10.95    --  107.46 -94.00 120.00  136
 11  \w     45.00 121.00   0.50   10.95    --  107.46 -61.00 -60.00  152
 12  \w     97.00 170.00   0.50   10.95    --  107.46 125.00-180.00  146
 13  \w    103.00 172.00   0.50   10.95    --  107.46  77.00  60.00  138
 14  \w     45.00 113.00   0.50   10.95    --  107.46-125.00  60.00  136
 15  \w     96.00 164.00   0.50   10.95    --  107.46  61.00 -30.00  136
 16  \w     44.00 102.00   0.50   10.95    --  107.46 -45.00  30.00  116
 17  \w     51.00 105.00   0.50   10.95    --  107.46 -94.00 -90.00  108
 18  \w    100.00 174.00   0.50   10.95    --  107.46  15.00-180.00  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      0.0813676000
_diffrn_orient_matrix_UB_12      0.0714050000
_diffrn_orient_matrix_UB_13      0.0083561000
_diffrn_orient_matrix_UB_21      -0.0836543000
_diffrn_orient_matrix_UB_22      0.0161814000
_diffrn_orient_matrix_UB_23      0.0894877000
_diffrn_orient_matrix_UB_31      0.1463150000
_diffrn_orient_matrix_UB_32      -0.0305145000
_diffrn_orient_matrix_UB_33      0.0670283000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17918
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.246
_diffrn_reflns_theta_min         3.940
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48783
_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    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_preparation       Dichlormethane/n-hexane
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0508P)^2^+0.8209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4048
_reflns_number_total             4652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02471k2.cif
_cod_data_source_block           kv_acm_ar_09_auto
_cod_depositor_comments
'Adding full bibliography for 1572679--1572683.cif.'
_cod_database_code               1572681
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N B F O S'
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.843
_diffrn_oxdiff_digest_frames
;
01b5f0287aec1942ae91e18c1c6a40164a000253374
;
_diffrn_oxdiff_digest_hkl
;
01999fe90f613e267f9bcd6aa28422bfb26cb7
;
_reflns_odcompleteness_completeness 99.95
_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:
 C2(H2), C19(H19), C9(H9), C22(H22), C25(H25), C8(H8), C20(H20), C21(H21),
 C5(H5), C15(H15), C28(H28), C11(H11), C6(H6), C24(H24), C18(H18), C13(H13),
 C27(H27), C26(H26), C14(H14), C12(H12)
2.b Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c)
;
_shelx_res_checksum              24750
_shelx_hkl_checksum              12694
_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 1.818
_oxdiff_exptl_absorpt_empirical_full_min 0.495