Synthesis, Structures, and Properties of Hexapole Helicenes: Assembling Six [5]Helicene Substructures into Highly Twisted Aromatic Systems.
Hosokawa, Tomoka; Takahashi, Yusuke; Matsushima, Tomoya; Watanabe, Soichiro; Kikkawa, Shoko; Azumaya, Isao; Tsurusaki, Akihiro; Kamikawa, Ken; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07113

data_4126562
_publ_section_title
;
 Synthesis, Structures, and Properties of Hexapole Helicenes: Assembling
 Six [5]Helicene Substructures into Highly Twisted Aromatic Systems.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07113
_journal_year                    2017
_chemical_formula_moiety         'C94.33 H48 Cl2'
_chemical_formula_sum            'C94.33 H48 Cl2'
_chemical_formula_weight         1252.28
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-09
_audit_creation_method           'by CrystalStructure 4.2.2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            18
_cell_length_a                   30.50240(10)
_cell_length_b                   30.50240(10)
_cell_length_c                   35.1637(2)
_cell_measurement_reflns_used    73377
_cell_measurement_temperature    93
_cell_measurement_theta_max      71.33
_cell_measurement_theta_min      2.22
_cell_volume                     28333.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            120942
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         5.023
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11663.64
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.69
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         11513
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1674P)^2^+107.1730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2636
_refine_ls_wR_factor_ref         0.2641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11273
_reflns_number_total             11513
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja7b07113_si_002.cif
_cod_data_source_block           HH-2
_cod_database_code               4126562
_shelx_res_checksum              37917
_shelx_hkl_checksum              80491