Helical mesoscopic crystals based on an achiral charge-transfer complex with controllable untwisting/breaking.
Yang, Canglei; Luo, Lixing; Chen, Jinqiu; Yang, Bo; Wang, Wei; Wang, Hebin; Long, Guankui; Liu, Guangfeng; Zhang, Jing; Huang, Wei; Chemical communications (Cambridge, England) 57 (2021) 10031–10034; doi:10.1039/d1cc03767f

data_7129050
_publ_section_title
;
 Helical mesoscopic crystals based on an achiral charge-transfer complex
 with controllable untwisting/breaking.
;
_journal_issue                   78
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10031
_journal_page_last               10034
_journal_paper_doi               10.1039/d1cc03767f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C16 H4 N4 S2, C16 H10'
_chemical_formula_sum            'C32 H14 N4 S2'
_chemical_formula_weight         518.59
_chemical_melting_point          300
_chemical_name_systematic        'Form 1'
_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
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-08-16 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                112.930(2)
_cell_angle_beta                 109.052(2)
_cell_angle_gamma                90.147(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4924(4)
_cell_length_b                   9.4682(5)
_cell_length_c                   9.6821(5)
_cell_measurement_reflns_used    7251
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      68.40
_cell_measurement_theta_min      5.13
_cell_volume                     591.24(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.0538
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12390
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.644
_diffrn_reflns_theta_min         5.129
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             266
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         2181
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0606
_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^)+(0.1317P)^2^+0.0583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.2071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1784
_reflns_number_total             2181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03767f4.cif
_cod_data_source_block           a_b
_cod_original_cell_volume        591.24(5)
_cod_database_code               7129050
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.658
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Others
 Fixed Sof: C1(0.5) C2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5)
 C6(0.5) S1A(0.5) C1A(0.5) H1A(0.5) C1B(0.5) H1B(0.5) S1B(0.5) C7(0.5) H7(0.5)
 C8(0.5) H8(0.5) C9B(0.5) H9B(0.5) C16(0.5) C2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5)
 H4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5)
 C9A(0.5) H9A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C1A(H1A), C1B(H1B), C7(H7), C8(H8), C9B(H9B),
 C3A(H3A), C4A(H4A), C5A(H5A), C7A(H7A), C8A(H8A), C9A(H9A)
4.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C16(C2A,C3A,C4A,C5A,C6A)
;
_shelx_res_checksum              92369
_olex2_submission_special_instructions 'No special instructions were received'