Hexathioalkyl sumanenes: An electron-donating buckybowl as a building block for supramolecular materials
Shoji, Yoshiaki; Kajitani, Takashi; Ishiwari, Fumitaka; Ding, Qiang; Sato, Hiroyasu; Anetai, Hayato; Akutagawa, Tomoyuki; Sakurai, Hidehiro; Fukushima, Takanori; Chem. Sci.  (2017) –; doi:10.1039/C7SC03860G

data_1547731
_publ_section_title
;
 Hexathioalkyl sumanenes: An electron-donating buckybowl as a building
 block for supramolecular materials
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03860G
_journal_year                    2017
_chemical_formula_sum            'C117 H24 S6'
_chemical_formula_weight         1621.72
_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-2014/6
_audit_update_record
;
2017-09-04 deposited with the CCDC.
2017-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                98.3340(10)
_cell_angle_beta                 113.3320(10)
_cell_angle_gamma                112.8910(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7708(11)
_cell_length_b                   16.9234(14)
_cell_length_c                   17.1467(14)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.28
_cell_volume                     3162.1(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHELL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.968
_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       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23130
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         1.383
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1125
_refine_ls_number_reflns         11101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0398P)^2^+4.4247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10001
_reflns_number_total             11101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03860g2.cif
_cod_data_source_block           SumS_C60_0m_a
_cod_database_code               1547731
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2014/6
_shelx_res_checksum              62914