Insights into mechanistic interpretation of crystalline-state reddish phosphorescence of non-planar π-conjugated organoboron compounds.
Adachi, Yohei; Kurihara, Maho; Yamada, Kohei; Arai, Fuka; Hattori, Yuto; Yamana, Keita; Kawasaki, Riku; Ohshita, Joji; Chemical science 15 (2024) 8127–8136; doi:10.1039/d4sc01184h

data_1571484
_publ_section_title
;
 Insights into mechanistic interpretation of crystalline-state reddish
 phosphorescence of non-planar &#x3c0;-conjugated organoboron compounds.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              8127
_journal_page_last               8136
_journal_paper_doi               10.1039/d4sc01184h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C35 H43 B O2 S2'
_chemical_formula_sum            'C35 H43 B O2 S2'
_chemical_formula_weight         570.62
_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             2023-11-21
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2024-01-10 deposited with the CCDC.	2024-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                79.288(5)
_cell_angle_beta                 79.038(5)
_cell_angle_gamma                79.944(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0896(4)
_cell_length_b                   11.2795(6)
_cell_length_c                   15.8838(10)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.9740
_cell_measurement_theta_min      2.1620
_cell_volume                     1554.47(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.27a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.27a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.27a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.827
_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    -25.00  18.00   0.50   21.00    --   -6.02  90.00 143.00   86
  2  \w    -35.00   7.00   0.50   21.00    --   -6.02 -90.00  28.00   84
  3  \w      1.00  32.00   0.50   21.00    --    6.80 -90.00  28.00   62
  4  \w    -77.00   7.00   0.50   21.00    --   -6.02 -57.00 150.00  168
  5  \w    -71.00  -4.00   0.50   21.00    --   -6.02 -38.00  30.00  134
  6  \w     19.00  69.00   0.50   21.00    --    6.80  38.00 -60.00  100
  7  \w      4.00  36.00   0.50   21.00    --    6.80 -99.00   0.00   64
  8  \w    -62.00  13.00   0.50   21.00    --    6.80 -19.00 120.00  150
  9  \w     53.00  78.00   0.50   21.00    --    6.80  38.00-180.00   50
 10  \w    -17.00   8.00   0.50   21.00    --    6.80 -99.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0607131000
_diffrn_orient_matrix_UB_12      -0.0299006000
_diffrn_orient_matrix_UB_13      -0.0032279000
_diffrn_orient_matrix_UB_21      0.0367820000
_diffrn_orient_matrix_UB_22      -0.0125503000
_diffrn_orient_matrix_UB_23      -0.0416227000
_diffrn_orient_matrix_UB_31      0.0375934000
_diffrn_orient_matrix_UB_32      -0.0559601000
_diffrn_orient_matrix_UB_33      0.0194673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28350
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.038
_diffrn_reflns_theta_min         2.103
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.27a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         8964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0447P)^2^+0.7354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6689
_reflns_number_total             8964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01184h3.cif
_cod_data_source_block           exp_2973
_cod_depositor_comments
'Adding full bibliography for 1571483--1571487.cif.'
_cod_database_code               1571484
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C35H43B1O2S2
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.981
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,
 H28B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C29(H29A,H29B,H29C),
 C35(H35A,H35B,H35C)
;
_shelx_res_checksum              89874
_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 1.140
_oxdiff_exptl_absorpt_empirical_full_min 0.869