Synthesis and Structural Features of Thiophene-fused Analogues of Warped Nanographene and Quintuple Helicene
Lin, Hsing-An; Kato, Kenta; Segawa, Yasutomo; Scott, Lawrence T.; Itami, Kenichiro; Chemical Science  (2019) –; doi:10.1039/C8SC04470H

data_1550375
_publ_section_title
;
 Synthesis and Structural Features of Thiophene-fused Analogues of Warped
 Nanographene and Quintuple Helicene
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04470H
_journal_year                    2019
_chemical_formula_sum            'C77 H51.5 Cl6 S5'
_chemical_formula_weight         1349.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-09-01 deposited with the CCDC.
2018-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.893(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7713(6)
_cell_length_b                   21.4590(6)
_cell_length_c                   27.4874(7)
_cell_measurement_reflns_used    18723
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.1230
_cell_measurement_theta_min      2.0600
_cell_volume                     12825.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            57659
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.959
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       Block
_exptl_crystal_F_000             5564
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.908
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     821
_refine_ls_number_reflns         11307
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0899
_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^)+(0.1301P)^2^+80.5408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2491
_refine_ls_wR_factor_ref         0.2702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8280
_reflns_number_total             11307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04470h2.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C77 H51.50 Cl6 S5'
_cod_database_code               1550375
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              99717