Optically active triptycenes containing hexa-peri-hexabenzocoronene units
Wada, Yuya; Shinohara, Ken-ichi; Ikai, Tomoyuki; Chemical Communications  (2019) –; doi:10.1039/C9CC06025A

data_7124073
_publ_section_title
;
 Optically active triptycenes containing hexa-peri-hexabenzocoronene units
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06025A
_journal_year                    2019
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C132 H118'
_chemical_formula_sum            'C132 H118'
_chemical_formula_weight         1704.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-07-24 deposited with the CCDC.    2019-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 108.140(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   56.145(2)
_cell_length_b                   7.4648(2)
_cell_length_c                   17.3511(12)
_cell_measurement_reflns_used    13274
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      3.10
_cell_volume                     6910.6(7)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       72
_diffrn_reflns_limit_h_min       -72
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38345
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.303
_diffrn_reflns_theta_min         3.054
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.046
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1820.00
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.38
_refine_ls_abs_structure_details
;
 Flack x determined using 2668 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   3.9(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     595
_refine_ls_number_reflns         14531
_refine_ls_number_restraints     1078
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0907
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1374P)^2^+4.5596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.2684
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                9205
_reflns_number_total             14531
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9cc06025a3.cif
_cod_data_source_block           489_1018a_FS
_cod_database_code               7124073
_shelx_res_checksum              73852
_shelx_fab_checksum              41220