Syntheses, structures, and one- and two-photon excited fluorescence of dimesitylboryl-ended quadrupolar hybrid oligothiophenes
Zhou, Senhao; Zhang, Shiqian; Li, Jinsong; Liu, Zhiqiang; Yu, Xiaoqiang; New Journal of Chemistry 45 (2021) 15035–15042; doi:10.1039/D1NJ00694K

data_7060508
_publ_section_title
;
 Syntheses, structures, and one- and two-photon excited fluorescence of
 dimesitylboryl-ended quadrupolar hybrid oligothiophenes
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15035
_journal_page_last               15042
_journal_paper_doi               10.1039/D1NJ00694K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C54 H52 B2 S4'
_chemical_formula_sum            'C54 H52 B2 S4'
_chemical_formula_weight         850.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-19 deposited with the CCDC.	2021-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.305(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   42.4881(14)
_cell_length_b                   15.1359(5)
_cell_length_c                   8.0769(2)
_cell_measurement_reflns_used    5206
_cell_measurement_temperature    297.15
_cell_measurement_theta_max      74.6720
_cell_measurement_theta_min      4.1380
_cell_volume                     5190.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      297.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.932
_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     94.00 174.00   1.00   11.02    --  106.49  19.00  30.00   80
  2  \w     95.00 178.00   1.00   11.02    --  106.49 125.00 -90.00   83
  3  \w    153.00 178.00   1.00   11.02    --  106.49  96.00-161.00   25
  4  \w    153.00 178.00   1.00   11.02    --  106.49  38.00-150.00   25
  5  \w    115.00 141.00   1.00   11.02    --  106.49  96.00-161.00   26
  6  \w     93.00 139.00   1.00   11.02    --  106.49  38.00-150.00   46
  7  \w     34.00 105.00   1.00   11.02    --  106.49 -77.00 -30.00   71
  8  \w     39.00  99.00   1.00   11.02    --  106.49 -96.00  89.00   60
  9  \w     46.00 102.00   1.00   11.02    --  106.49 -77.00 150.00   56
 10  \w     35.00  65.00   1.00   11.02    --  106.49 -57.00   0.00   30
 11  \w     37.00  66.00   1.00   11.02    --  106.49 -57.00 -90.00   29
 12  \w     16.00  65.00   1.00    0.70    --   48.45 -96.00  89.00   49
 13  \w    -26.00  27.00   1.00    0.70    --  -48.45  19.00 -60.00   53
 14  \w     -5.00  24.00   1.00    0.70    --  -48.45  96.00-161.00   29
 15  \w    -43.00 -13.00   1.00   11.02    --  -86.25  38.00-150.00   30
 16  \w    -49.00 -24.00   1.00   11.02    --  -86.25  96.00-161.00   25
 17  \w    -74.00 -10.00   1.00    0.70    --  -48.45  96.00-161.00   64
 18  \w    -40.00 -14.00   1.00   11.02    --  -86.25  38.00  30.00   26
 19  \w    -66.00 -14.00   1.00   11.02    --  -86.25  57.00 150.00   52
 20  \w   -146.00-121.00   1.00   11.02    --  -86.25 -96.00  89.00   25
 21  \w   -120.00 -73.00   1.00    0.70    --  -48.45-125.00-150.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            16352
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.736
_diffrn_reflns_theta_min         4.165
_exptl_absorpt_coefficient_mu    1.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5105
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0839
_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^)+15.9222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.1977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4218
_reflns_number_total             5105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00694k2.cif
_cod_data_source_block           210125h_sq
_cod_depositor_comments
'Adding full bibliography for 7060505--7060508.cif.'
_cod_database_code               7060508
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.789
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H10A,H10B,H10C} of C10, {H13A,H13B,H13C} of C13, {H15A,
  H15B,H15C} of C15
 At 1.5 times of:
  {H2A,H2B,H2C} of C2, {H3A,H3B,H3C} of C3, {H24A,H24B,H24C} of C24
2. Restrained distances
 S2-C1 \\sim S2A-C1
 with sigma of 0.02
 S2-C7 \\sim S2A-C7A
 with sigma of 0.02
 C7-C11 \\sim C7A-C11A
 with sigma of 0.04
 C8-C17 \\sim C8A-C17A
 with sigma of 0.04
 C1-C7 \\sim C1-C7A
 with sigma of 0.04
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C7-C17 \\sim C7A-C17A
 with sigma of 0.02
 C1-C11 \\sim C1-C11A
 with sigma of 0.02
 C1-C8 \\sim C1-C8A
 with sigma of 0.04
 C8-C11 \\sim C8A-C11A
 with sigma of 0.02
 S2-C8 \\sim S2A-C8A
 with sigma of 0.04
 S2-C17 \\sim S2A-C17A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C8A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(S2A)=Sof(C7A)=Sof(C8A)=Sof(C11A)=Sof(H11A)=Sof(C17A)=Sof(H17A)=1-FVAR(1)
 Sof(S2)=Sof(C7)=Sof(C8)=Sof(C11)=Sof(H11)=Sof(C17)=Sof(H17)=FVAR(1)
6.a Riding coordinates:
 C6(H6), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C),
 C19(H19), C21(H21), C25(H25), C27(H27)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C11A(H11A), C17(H17), C17A(H17A), C20(H20)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              70205
_shelx_fab_checksum              48743
_platon_squeeze_void_probe_radius 1.20
_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
;