Constructing highly efficient multiple resonance fluorescence materials by inserting benzothiophene within B/N-skeletons
Zhao, He; Han, Wenkun; Xu, Jianan; Bi, Yan; Li, He; Yang, Tianyu; Ma, Xiaoyu; Su, Chunhui; New Journal of Chemistry 48 (2024) 16119–16126; doi:10.1039/D4NJ01922A

data_7063422
_publ_section_title
;
 Constructing highly efficient multiple resonance fluorescence materials
 by inserting benzothiophene within B/N-skeletons
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16119
_journal_page_last               16126
_journal_paper_doi               10.1039/D4NJ01922A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C75 H78 B N3 O S2, C H2 Cl2, C Cl2'
_chemical_formula_sum            'C77 H80 B Cl4 N3 O S2'
_chemical_formula_weight         1280.17
_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             2023-09-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                105.358(2)
_cell_angle_beta                 95.154(3)
_cell_angle_gamma                116.471(3)
_cell_formula_units_Z            2
_cell_length_a                   13.9094(14)
_cell_length_b                   15.1975(14)
_cell_length_c                   19.4579(16)
_cell_measurement_reflns_used    9477
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      29.770
_cell_measurement_theta_min      2.237
_cell_volume                     3446.0(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            182295
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.150
_diffrn_reflns_theta_min         1.922
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.645
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         20287
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1269P)^2^+3.7523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13394
_reflns_number_total             20287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01922a2.cif
_cod_data_source_block           SBN-2
_cod_depositor_comments
'Adding full bibliography for 7063422--7063423.cif.'
_cod_database_code               7063422
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.946
_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. Restrained distances
 Cl1-C75
 1.78 with sigma of 0.02
 Cl2-C75
 1.77 with sigma of 0.02
 Cl1-C75 = Cl2-C75
 1.771 with sigma of 0.01
 Cl3-Cl4
 2.916 with sigma of 0.03
 Cl1-Cl2
 2.916 with sigma of 0.03
 Cl3-C19
 1.78 with sigma of 0.02
 Cl4-C19
 1.77 with sigma of 0.02
 Cl3-C19 = Cl4-C19
 1.771 with sigma of 0.01
 Cl1-Cl2
 2.92 with sigma of 0.04
 Cl3-Cl4
 2.92 with sigma of 0.04
 Cl4-C19 \\sim Cl5-C19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C75: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Cl3 \\sim Cl4 \\sim C19: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C19) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl1, Cl2, C75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3, Cl4, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, Cl1, C75, H75A, H75B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl5)=1-FVAR(1)
 Sof(Cl4)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C75(H75A,H75B)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C20(H20), C30(H30), C32(H32), C36(H36), C50(H50), C54(H54),
 C56(H56), C58(H58), C60(H60), C64(H64), C66(H66), C68(H68), C70(H70), C74(H74),
  C39(H39), C5(H5), C41(H41), C21(H21), C47(H47), C49(H49), C51(H51), C27(H27),
 C7(H7), C57(H57), C15(H15)
6.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C61(H61A,H61B,
 H61C), C31(H31A,H31B,H31C), C63(H63A,H63B,H63C), C2(H2A,H2B,H2C), C65(H65A,
 H65B,H65C), C33(H33A,H33B,H33C), C67(H67A,H67B,H67C), C17(H17A,H17B,H17C),
 C69(H69A,H69B,H69C), C35(H35A,H35B,H35C), C71(H71A,H71B,H71C), C9(H9A,H9B,H9C),
  C73(H73A,H73B,H73C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              10987
_shelx_hkl_checksum              8293
_olex2_submission_special_instructions 'No special instructions were received'