Thia[<i>n</i>]helicenes with long persistent phosphorescence.
Sun, Zhen; Xu, Wan; Qiu, Shuai; Ma, Zhiying; Li, Chunli; Zhang, Sheng; Wang, Hua; Chemical science 15 (2024) 1077–1087; doi:10.1039/d3sc05480b

data_1570531
_publ_section_title
;
 Thia[<i>n</i>]helicenes with long persistent phosphorescence.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1077
_journal_page_last               1087
_journal_paper_doi               10.1039/d3sc05480b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C27 H20 S3 Si'
_chemical_formula_sum            'C27 H20 S3 Si'
_chemical_formula_weight         468.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-28
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2022-12-11 deposited with the CCDC.	2023-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.9100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2989(3)
_cell_length_b                   12.2575(2)
_cell_length_c                   12.9384(2)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.302
_cell_measurement_theta_min      2.808
_cell_volume                     2251.23(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.98
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25550
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         2.195
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1063 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.8853. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0402P)^2^+1.0204P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4925
_reflns_number_total             5583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05480b2.cif
_cod_data_source_block           TB[7]H
_cod_depositor_comments
'Adding full bibliography for 1570529--1570532.cif.'
_cod_database_code               1570531
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.921
_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: 
 C2(H2), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), 
 C21(H21), C26(H26), C27(H27) 
2.b Idealised Me refined as rotating group: 
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C) 
;
_olex2_submission_special_instructions 'No special instructions were received'