Synthesis and Crystal Structures of Unsymmetrical Wave-shaped Heptathienoacenes
Wu, Zhiping; Xu, Wan; Li, Chunli; Ma, Zhiying; Wang, Guangxia; Wang, Hua; Organic & Biomolecular Chemistry  (2022) –; doi:10.1039/D2OB00800A

data_7158729
_publ_section_title
;
 Synthesis and Crystal Structures of Unsymmetrical Wave-shaped
 Heptathienoacenes
;
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB00800A
_journal_year                    2022
_chemical_formula_moiety         'C19 H12 S7 Si'
_chemical_formula_sum            'C19 H12 S7 Si'
_chemical_formula_weight         492.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           46
_space_group_name_Hall           'I 2 -2a'
_space_group_name_H-M_alt        'I m a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-14 deposited with the CCDC.	2022-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0326(3)
_cell_length_b                   30.5918(13)
_cell_length_c                   10.3680(4)
_cell_measurement_reflns_used    5398
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.273
_cell_measurement_theta_min      3.501
_cell_volume                     2230.57(16)
_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      149.99
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5150
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.338
_diffrn_reflns_theta_min         2.663
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1644 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.6812.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 962 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2278
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.3589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    0.851
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                2257
_reflns_number_total             2278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob00800a2.cif
_cod_data_source_block           a_CCDC2
_cod_database_code               7158729
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.868
_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. Uiso/Uaniso restraints and constraints
Uanis(S4) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.08
3. Others
 Fixed Sof: H18A(0.5) H18B(0.5) H18C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C15(H15)
4.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'