Synthesis of Tetrathia-Oligothiophene Macrocycles.
Press, David J.; Gendy, Chris; Pasalkar, Samruddhi; Schechtel, Shauna; Heyne, Belinda; Sutherland, Todd C.; ACS omega 4 (2019) 3405–3408; doi:10.1021/acsomega.8b03444

data_4515131
_publ_section_title
;
 Synthesis of Tetrathia-Oligothiophene Macrocycles.
;
_journal_issue                   2
_journal_name_full               'ACS omega'
_journal_page_first              3405
_journal_page_last               3408
_journal_paper_doi               10.1021/acsomega.8b03444
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C32 H28 S10'
_chemical_formula_sum            'C32 H28 S10'
_chemical_formula_weight         733.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                100.16
_cell_angle_beta                 92.47
_cell_angle_gamma                98.58
_cell_formula_units_Z            6
_cell_length_a                   8.1710(3)
_cell_length_b                   18.1630(8)
_cell_length_c                   33.5750(4)
_cell_measurement_reflns_used    15561
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4837.5(3)
_computing_cell_refinement       'DENZO & ScalePACK (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo and ScalePACK'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            33008
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         1.154
_diffrn_source                   'Fine focused sealed X-Ray tube'
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ScalePACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         20732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0047P)^2^+25.1065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16523
_reflns_number_total             20732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            C4terTh.cif
_cod_data_source_block           DPIII30
_cod_database_code               4515131
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              86221
_shelx_hkl_checksum              18421