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_1570530
_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         'C15 H14 S3 Si'
_chemical_formula_sum            'C15 H14 S3 Si'
_chemical_formula_weight         318.53
_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             2023-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-04 deposited with the CCDC.	2023-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                94.58(2)
_cell_angle_beta                 99.657(16)
_cell_angle_gamma                114.95(2)
_cell_formula_units_Z            2
_cell_length_a                   7.373(4)
_cell_length_b                   8.088(5)
_cell_length_c                   14.380(8)
_cell_measurement_reflns_used    8808
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.279
_cell_measurement_theta_min      2.824
_cell_volume                     755.5(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17165
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.818
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_correction_T_min  0.1970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1495 before and 0.0928 after correction. The Ratio of minimum to maximum transmission is 0.7499. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.824
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0999
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2545
_refine_ls_wR_factor_ref         0.2673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2226
_reflns_number_total             2619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05480b2.cif
_cod_data_source_block           TB[4]H
_cod_depositor_comments
'Adding full bibliography for 1570529--1570532.cif.'
_cod_original_cell_volume        755.4(8)
_cod_database_code               1570530
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.942
_diffrn_source_source            'Incoatc Ius 3.0 '
_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:
 C5(H5), C4(H4), C3(H3), C2(H2), C11(H11)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              75340
_shelx_hkl_checksum              11714
_olex2_submission_special_instructions 'No special instructions were received'