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_7118120
_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         'C46 H62 Cl12 N2 S2 Sb2'
_chemical_formula_sum            'C46 H62 Cl12 N2 S2 Sb2'
_chemical_formula_weight         1376.07
_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
_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                103.1816(19)
_cell_angle_beta                 91.496(2)
_cell_angle_gamma                112.2261(18)
_cell_formula_units_Z            4
_cell_length_a                   16.3370(12)
_cell_length_b                   20.1317(13)
_cell_length_c                   20.3767(14)
_cell_measurement_reflns_used    20540
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.02
_cell_volume                     5993.2(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2003
_diffrn_reflns_laue_measured_fraction_full 0.000
_diffrn_reflns_laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53692
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.460
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_min         3.019
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.536
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2760.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.97
_refine_diff_density_min         -1.68
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1070
_refine_ls_number_reflns         25930
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3148
_refine_ls_R_factor_gt           0.1484
_refine_ls_shift/su_max          0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1578P)^2^+53.9206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3031
_refine_ls_wR_factor_ref         0.3957
_reflns_number_gt                9337
_reflns_number_total             25930
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5cc07680c2.cif
_cod_data_source_block           20150508Sakamaki
_cod_database_code               7118120