A double hetero[4]helicene composed of two phenothiazines: synthesis, structural properties, and cationic states
Daisuke Sakamaki; Daisuke Kumano; Eiji Yashim; Shu Seki; Chem.Commun. 51 (2015) 17237–; doi:10.1039/C5cc07680C

data_7118119
_publ_section_title
;
 A double hetero[4]helicene composed of two phenothiazines: synthesis,
 structural properties, and cationic states
;
_journal_name_full               Chem.Commun.
_journal_page_first              17237
_journal_paper_doi               10.1039/C5cc07680C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C41 H52 N2 O S2'
_chemical_formula_sum            'C41 H52 N2 O S2'
_chemical_formula_weight         652.99
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-07-24 deposited with the CCDC.
2015-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 104.7159(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            16
_cell_length_a                   23.0126(5)
_cell_length_b                   29.0068(6)
_cell_length_c                   22.0641(4)
_cell_measurement_reflns_used    92289
_cell_measurement_temperature    123
_cell_measurement_theta_max      71.74
_cell_measurement_theta_min      3.04
_cell_volume                     14245.1(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            123850
_diffrn_reflns_theta_full        71.74
_diffrn_reflns_theta_max         71.74
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5632.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.380
_refine_diff_density_min         -1.980
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     806
_refine_ls_number_reflns         13775
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.1064
_refine_ls_shift/su_max          0.060
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1714P)^2^+82.7027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3091
_reflns_number_gt                11137
_reflns_number_total             13775
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5cc07680c2.cif
_cod_data_source_block           150128_pt2
_cod_database_code               7118119