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_1572679
_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 O2 S'
_chemical_formula_sum            'C28 H13 B F10 O2 S'
_chemical_formula_weight         614.25
_chemical_name_systematic        ACM-AR-05
_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             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                71.659(2)
_cell_angle_beta                 81.2320(10)
_cell_angle_gamma                76.3720(10)
_cell_formula_units_Z            2
_cell_length_a                   8.88200(10)
_cell_length_b                   11.7045(2)
_cell_length_c                   14.6627(3)
_cell_measurement_reflns_used    16641
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.8230
_cell_measurement_theta_min      4.0520
_cell_volume                     1401.08(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.977
_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   -108.00 -28.00   0.50    0.23    --  -38.50 164.00 -50.00  160
  2  \w    -81.00   1.00   0.50    0.23    --  -38.50 116.00 160.00  164
  3  \w   -105.00 -50.00   0.50    0.23    --  -38.50-164.00 -75.00  110
  4  \w     49.00 119.00   0.50    0.23    --   49.56-164.00 -75.00  140
  5  \w     20.00  92.00   0.50    0.23    --   49.56-116.00  72.00  144
  6  \w    102.00 172.00   0.50    0.92    --  107.46 116.00 160.00  140
  7  \w     43.00 110.00   0.50    0.92    --  107.46-116.00  72.00  134
  8  \w     49.00 139.00   0.50    0.92    --  107.46-164.00 -75.00  180
  9  \w     72.00 156.00   0.50    0.92    --  107.46 164.00 -50.00  168
 10  \w   -101.00 -21.00   0.50    0.23    --  -38.50 -68.00 -56.98  160
 11  \w   -101.00 -26.00   0.50    0.23    --  -38.50 -60.00  25.57  150
 12  \w   -101.00 -23.00   0.50    0.23    --  -38.50 -64.00 -94.17  156
 13  \w     46.00 116.00   0.50    0.23    --   49.56  37.00 120.00  140
 14  \w    -17.00  53.00   0.50    0.23    --   49.56 -37.00 -30.00  140
 15  \w     46.00 116.00   0.50    0.23    --   49.56  37.00 -90.00  140
 16  \w     39.00 107.00   0.50    0.92    --  107.46 -94.00 -60.00  136
 17  \w     95.00 170.00   0.50    0.92    --  107.46  61.00  30.00  150
 18  \w     43.00 112.00   0.50    0.92    --  107.46 -45.00  30.00  138
 19  \w     45.00 121.00   0.50    0.92    --  107.46 -61.00  60.00  152
 20  \w     39.00 107.00   0.50    0.92    --  107.46 -94.00-180.00  136
 21  \w     39.00 107.00   0.50    0.92    --  107.46 -94.00   0.00  136
 22  \w     45.00 121.00   0.50    0.92    --  107.46 -61.00 -30.00  152
 23  \w     45.00 113.00   0.50    0.92    --  107.46-125.00 -90.00  136
 24  \w     39.00 111.00   0.50    0.92    --  107.46 -30.00  90.00  144
 25  \w     45.00 113.00   0.50    0.92    --  107.46-125.00 150.00  136
 26  \w    103.00 172.00   0.50    0.92    --  107.46  45.00-180.00  138
 27  \w     39.00 107.00   0.50    0.92    --  107.46 -94.00 -30.00  136
 28  \w     39.00 116.00   0.50    0.92    --  107.46 -15.00  30.00  154
 29  \w     39.00 116.00   0.50    0.92    --  107.46 -15.00-120.00  154
 30  \w    103.00 172.00   0.50    0.92    --  107.46  45.00  60.00  138
 31  \w     39.00 111.00   0.50    0.92    --  107.46 -30.00-180.00  144
 32  \w     97.00 170.00   0.50    0.92    --  107.46 125.00  30.00  146
 33  \w     66.00 107.00   0.50    0.92    --  107.46 -94.00 -90.00   82
 34  \w     77.00 107.00   0.50    0.92    --  107.46 -94.00  90.00   60
 35  \w     43.00 111.00   0.50    0.92    --  107.46 -30.00-120.00  136
 36  \w    141.00 175.00   0.50    0.92    --  107.46  15.00  90.00   68
;
_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      0.0945926000
_diffrn_orient_matrix_UB_12      -0.0957816000
_diffrn_orient_matrix_UB_13      -0.0495545000
_diffrn_orient_matrix_UB_21      0.0055070000
_diffrn_orient_matrix_UB_22      -0.0998178000
_diffrn_orient_matrix_UB_23      0.0981016000
_diffrn_orient_matrix_UB_31      -0.1520039000
_diffrn_orient_matrix_UB_32      -0.0298625000
_diffrn_orient_matrix_UB_33      -0.0161736000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.112
_diffrn_reflns_theta_min         4.061
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69197
_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    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_preparation       Dichloromethane/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         0.369
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0692P)^2^+0.4777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5556
_reflns_number_total             5864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02471k2.cif
_cod_data_source_block           kv_acm_ar_05_auto
_cod_depositor_comments
'Adding full bibliography for 1572679--1572683.cif.'
_cod_database_code               1572679
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N B F O S'
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.806
_diffrn_oxdiff_digest_frames
;
01815593c009dac805c37f77a8f7d26bc5000330c16
;
_diffrn_oxdiff_digest_hkl
;
011eb8aa40eb687a3de05a45b390032021cd57
;
_reflns_odcompleteness_completeness 99.86
_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:
 C4(H4), C9(H9), C3(H3), C7(H7), C6(H6), C12(H12), C13(H13), C16(H16),
 C15(H15), C14(H14)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12497
_shelx_hkl_checksum              27769
_shelx_fab_checksum              72013
_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 1.481
_oxdiff_exptl_absorpt_empirical_full_min 0.711