Ag-induced homochiral <i>versus</i> heterochiral double helicates based on cyclooctatetrathiophene-bipyridine.
Wang, Chenglong; Yang, Jie; Miao, Guanfeng; Ma, Zhiying; Wang, Guangxia; Wang, Hua; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13048–13052; doi:10.1039/d5dt01584g

data_1575480
_publ_section_title
;
 Ag-induced homochiral <i>versus</i> heterochiral double helicates based
 on cyclooctatetrathiophene-bipyridine.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13048
_journal_page_last               13052
_journal_paper_doi               10.1039/d5dt01584g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C42 H36 N4 S4 Si2'
_chemical_formula_sum            'C42 H36 N4 S4 Si2'
_chemical_formula_weight         781.17
_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             2021-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-04-08 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                102.507(5)
_cell_angle_beta                 97.552(5)
_cell_angle_gamma                110.270(5)
_cell_formula_units_Z            4
_cell_length_a                   13.7578(13)
_cell_length_b                   15.9691(16)
_cell_length_c                   20.936(2)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      68.293
_cell_measurement_theta_min      3.245
_cell_volume                     4104.0(7)
_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      296.29
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49797
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.507
_diffrn_reflns_theta_min         2.219
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1029 before and 0.0709 after correction. The Ratio of minimum to maximum transmission is 0.7606. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         15019
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0576P)^2^+0.8420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11622
_reflns_number_total             15019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01584g2.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 1575480--1575481.cif.'
_cod_database_code               1575480
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.514
_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. Restrained distances
 Si1'-C39' = C1A-Si2A
 1.84 with sigma of 0.02
 Si2A-C1C
 1.84 with sigma of 0.02
 C1B-Si2A
 1.84 with sigma of 0.02
 C1B-C1C
 3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41') \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C42')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40') \\sim Ueq, Uanis(C1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C41') = Uanis(C1A)
Uanis(C40') = Uanis(C1B)
Uanis(C42') = Uanis(C1C)
Uanis(Si2') = Uanis(Si2A)
4. Others
 Sof(Si2A)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=
 Sof(H1AC)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(1)
 Sof(Si2')=Sof(C40')=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41')=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=Sof(C42')=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C7'(H7'), C10'(H10'), C15'(H15'), C18'(H18'), C19'(H19'),
 C20'(H20'), C23'(H23'), C24'(H24'), C25'(H25'), C26'(H26'), C28'(H28'),
 C29'(H29'), C30'(H30'), C33'(H33'), C34'(H34'), C35'(H35'), C36'(H36'), C2(H2),
  C7(H7), C10(H10), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24),
 C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35),
  C36(H36)
5.b Idealised Me refined as rotating group:
 C1C(H1CA,H1CB,H1CC), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C37'(H37A,H37B,
 H37C), C38'(H38A,H38B,H38C), C39'(H39A,H39B,H39C), C40'(H40A,H40B,H40C),
 C41'(H41A,H41B,H41C), C42'(H42A,H42B,H42C), C37(H37D,H37E,H37F), C38(H38D,H38E,
 H38F), C39(H39D,H39E,H39F), C40(H40D,H40E,H40F), C41(H41D,H41E,H41F), C42(H42D,
 H42E,H42F)
;
_shelx_res_checksum              73870
_shelx_hkl_checksum              88344
_olex2_submission_special_instructions 'No special instructions were received'