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_1571483
_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         'C29 H35 B S2 Si2'
_chemical_formula_sum            'C29 H35 B S2 Si2'
_chemical_formula_weight         514.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-21
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2574(2)
_cell_length_b                   12.8335(3)
_cell_length_c                   19.7938(4)
_cell_measurement_reflns_used    25597
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.8180
_cell_measurement_theta_min      1.8780
_cell_volume                     2859.65(10)
_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 0.890
_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    -15.00  72.00   0.50    2.00    --    6.38  77.00-180.00  174
  2  \w     32.00  70.00   0.50    2.00    --    6.38  77.00-120.00   76
  3  \w     -8.00  75.00   0.50    2.00    --    6.38  77.00 -60.00  166
  4  \w      3.00  62.00   0.50    2.00    --    6.38  77.00  60.00  118
  5  \w    -30.00  57.00   0.50    2.00    --   -9.04  77.00   0.00  174
  6  \w     26.00  52.00   0.50    2.00    --   -9.04  77.00 120.00   52
  7  \w    -30.00   3.00   0.50    2.00    --   -9.04  77.00 120.00   66
;
_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      0.0465382000
_diffrn_orient_matrix_UB_12      -0.0332826000
_diffrn_orient_matrix_UB_13      -0.0108753000
_diffrn_orient_matrix_UB_21      -0.0403223000
_diffrn_orient_matrix_UB_22      -0.0268080000
_diffrn_orient_matrix_UB_23      -0.0213404000
_diffrn_orient_matrix_UB_31      0.0133383000
_diffrn_orient_matrix_UB_32      0.0350474000
_diffrn_orient_matrix_UB_33      -0.0266557000
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34149
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.827
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98599
_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    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 2562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0328P)^2^+0.4389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                6421
_reflns_number_total             6965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01184h3.cif
_cod_data_source_block           exp_797
_cod_depositor_comments
'Adding full bibliography for 1571483--1571487.cif.'
_cod_database_code               1571483
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H35B1S2Si2
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.969
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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:
 C1(H1), C2(H2), C3(H3), C6(H6), C8(H8), C14(H14), C23(H23), C25(H25)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              12472
_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 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.912