#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:35:58 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289434 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/05/1570529.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1570529
loop_
_publ_author_name
'Sun, Zhen'
'Xu, Wan'
'Qiu, Shuai'
'Ma, Zhiying'
'Li, Chunli'
'Zhang, Sheng'
'Wang, Hua'
_publ_section_title
;
 Thia[n]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         'C19 H16 S3 Si'
_chemical_formula_sum            'C19 H16 S3 Si'
_chemical_formula_weight         368.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-15
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.8509(2)
_cell_length_b                   12.4040(2)
_cell_length_c                   21.8020(4)
_cell_measurement_reflns_used    9470
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.313
_cell_measurement_theta_min      2.950
_cell_volume                     3475.29(10)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26331
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         2.450
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0964 before and 0.0619 after correction. The Ratio of minimum to maximum transmission is 0.9193. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0304
_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/[σ²(Fo²)+(0.0319P)²+1.8476P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3678
_reflns_number_total             4321
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc05480b2.cif
_cod_data_source_block           TB[5]H
_cod_depositor_comments
'Adding full bibliography for 1570529--1570532.cif.'
_cod_database_code               1570529
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.930
_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), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16) 
2.b Idealised Me refined as rotating group: 
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C) 
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.56063(3) 0.12926(3) 0.31204(2) 0.02439(10) Uani 1 1 d . . . . .
S2 S 0.44329(3) 0.08218(3) 0.43505(2) 0.02424(10) Uani 1 1 d . . . . .
S3 S 0.40961(3) 0.19280(3) 0.56127(2) 0.02458(10) Uani 1 1 d . . . . .
Si1 Si 0.70652(3) 0.29050(3) 0.23988(2) 0.02050(10) Uani 1 1 d . . . . .
C1 C 0.63577(11) 0.29492(12) 0.36674(7) 0.0202(3) Uani 1 1 d . . . . .
H1 H 0.673379 0.359312 0.374799 0.024 Uiso 1 1 calc R . . . .
C2 C 0.63797(12) 0.24457(12) 0.31114(7) 0.0217(3) Uani 1 1 d . . . . .
C3 C 0.57219(11) 0.24303(11) 0.41215(7) 0.0180(3) Uani 1 1 d . . . . .
C4 C 0.52671(12) 0.15146(12) 0.38704(7) 0.0207(3) Uani 1 1 d . . . . .
C5 C 0.53780(11) 0.25840(11) 0.47511(7) 0.0188(3) Uani 1 1 d . . . . .
C6 C 0.46830(12) 0.17763(12) 0.49091(7) 0.0210(3) Uani 1 1 d . . . . .
C7 C 0.54601(11) 0.33725(12) 0.52441(7) 0.0183(3) Uani 1 1 d . . . . .
C8 C 0.47773(12) 0.31272(12) 0.57247(7) 0.0212(3) Uani 1 1 d . . . . .
C9 C 0.46273(12) 0.37998(13) 0.62373(8) 0.0252(3) Uani 1 1 d . . . . .
H9 H 0.415718 0.360109 0.655395 0.030 Uiso 1 1 calc R . . . .
C10 C 0.51707(12) 0.47420(13) 0.62698(8) 0.0252(3) Uani 1 1 d . . . . .
H10 H 0.505253 0.521902 0.660355 0.030 Uiso 1 1 calc R . . . .
C11 C 0.59110(12) 0.50222(12) 0.58125(7) 0.0216(3) Uani 1 1 d . . . . .
C12 C 0.60865(11) 0.43275(11) 0.53014(7) 0.0191(3) Uani 1 1 d . . . . .
C13 C 0.68758(11) 0.46085(12) 0.48827(7) 0.0231(3) Uani 1 1 d . . . . .
H13 H 0.702206 0.413902 0.454939 0.028 Uiso 1 1 calc R . . . .
C14 C 0.74395(13) 0.55425(13) 0.49434(8) 0.0269(3) Uani 1 1 d . . . . .
H14 H 0.796780 0.571119 0.465405 0.032 Uiso 1 1 calc R . . . .
C15 C 0.72366(13) 0.62495(13) 0.54326(8) 0.0270(3) Uani 1 1 d . . . . .
H15 H 0.761276 0.690584 0.546826 0.032 Uiso 1 1 calc R . . . .
C16 C 0.64958(13) 0.59881(12) 0.58565(8) 0.0254(3) Uani 1 1 d . . . . .
H16 H 0.636939 0.646539 0.618899 0.030 Uiso 1 1 calc R . . . .
C17 C 0.82223(15) 0.36816(16) 0.26564(9) 0.0373(4) Uani 1 1 d . . . . .
H17A H 0.855484 0.402184 0.230120 0.056 Uiso 1 1 calc GR . . . .
H17B H 0.871752 0.319345 0.285571 0.056 Uiso 1 1 calc GR . . . .
H17C H 0.800473 0.423886 0.294805 0.056 Uiso 1 1 calc GR . . . .
C18 C 0.74534(15) 0.16967(14) 0.19486(9) 0.0347(4) Uani 1 1 d . . . . .
H18A H 0.683779 0.125445 0.186444 0.052 Uiso 1 1 calc GR . . . .
H18B H 0.795901 0.127358 0.218368 0.052 Uiso 1 1 calc GR . . . .
H18C H 0.776795 0.192534 0.156029 0.052 Uiso 1 1 calc GR . . . .
C19 C 0.61805(14) 0.37835(16) 0.19470(9) 0.0348(4) Uani 1 1 d . . . . .
H19A H 0.655948 0.408606 0.159701 0.052 Uiso 1 1 calc GR . . . .
H19B H 0.592509 0.437040 0.220759 0.052 Uiso 1 1 calc GR . . . .
H19C H 0.559000 0.335750 0.179809 0.052 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 S1 C2 91.38(7) . . ?
C4 S2 C6 88.33(7) . . ?
C6 S3 C8 89.89(7) . . ?
C17 Si1 C2 106.45(8) . . ?
C17 Si1 C18 111.26(9) . . ?
C18 Si1 C2 108.57(7) . . ?
C19 Si1 C2 109.28(8) . . ?
C19 Si1 C17 110.24(9) . . ?
C19 Si1 C18 110.92(9) . . ?
C2 C1 C3 114.79(13) . . ?
S1 C2 Si1 121.81(9) . . ?
C1 C2 S1 110.74(11) . . ?
C1 C2 Si1 127.38(11) . . ?
C1 C3 C5 139.88(13) . . ?
C4 C3 C1 109.52(13) . . ?
C4 C3 C5 110.55(13) . . ?
S1 C4 S2 130.99(9) . . ?
C3 C4 S1 113.57(11) . . ?
C3 C4 S2 115.41(12) . . ?
C3 C5 C7 139.65(13) . . ?
C6 C5 C3 109.62(13) . . ?
C6 C5 C7 110.39(13) . . ?
S3 C6 S2 128.46(9) . . ?
C5 C6 S2 116.09(12) . . ?
C5 C6 S3 115.18(12) . . ?
C8 C7 C5 111.15(13) . . ?
C8 C7 C12 117.70(13) . . ?
C12 C7 C5 131.13(14) . . ?
C7 C8 S3 113.28(11) . . ?
C7 C8 C9 123.44(14) . . ?
C9 C8 S3 123.24(12) . . ?
C10 C9 C8 118.64(15) . . ?
C9 C10 C11 121.06(15) . . ?
C10 C11 C12 120.41(14) . . ?
C16 C11 C10 120.94(15) . . ?
C16 C11 C12 118.66(15) . . ?
C11 C12 C7 118.50(14) . . ?
C13 C12 C7 123.42(14) . . ?
C13 C12 C11 118.08(14) . . ?
C14 C13 C12 121.77(15) . . ?
C13 C14 C15 120.13(16) . . ?
C16 C15 C14 119.65(15) . . ?
C15 C16 C11 121.63(15) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C2 1.7418(15) . ?
S1 C4 1.7145(16) . ?
S2 C4 1.7271(15) . ?
S2 C6 1.7287(16) . ?
S3 C6 1.7196(16) . ?
S3 C8 1.7431(16) . ?
Si1 C2 1.8746(16) . ?
Si1 C17 1.8586(17) . ?
Si1 C18 1.8598(17) . ?
Si1 C19 1.8575(18) . ?
C1 C2 1.364(2) . ?
C1 C3 1.436(2) . ?
C3 C4 1.390(2) . ?
C3 C5 1.455(2) . ?
C5 C6 1.386(2) . ?
C5 C7 1.457(2) . ?
C7 C8 1.400(2) . ?
C7 C12 1.438(2) . ?
C8 C9 1.408(2) . ?
C9 C10 1.363(2) . ?
C10 C11 1.421(2) . ?
C11 C12 1.426(2) . ?
C11 C16 1.418(2) . ?
C12 C13 1.408(2) . ?
C13 C14 1.373(2) . ?
C14 C15 1.405(2) . ?
C15 C16 1.366(2) . ?
