Asymmetric systematic synthesis, structures, and (chir)optical properties of a series of dihetero[8]helicenes
Yanagi, Tomoyuki; Tanaka, Takayuki; Yorimitsu, Hideki; Chemical Science 12 (2021) 2784–2793; doi:10.1039/D1SC00044F

data_1560217
_publ_section_title
;
 Asymmetric systematic synthesis, structures, and (chir)optical properties
 of a series of dihetero[8]helicenes
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2784
_journal_page_last               2793
_journal_paper_doi               10.1039/D1SC00044F
_journal_volume                  12
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H16 O, C0.50 H0.50 Cl1.50'
_chemical_formula_sum            'C28.5 H16.5 Cl1.5 O'
_chemical_formula_weight         428.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           91
_space_group_name_Hall           'P 4w 2c'
_space_group_name_H-M_alt        'P 41 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-12-01 deposited with the CCDC.	2021-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.0201(9)
_cell_length_b                   9.0201(9)
_cell_length_c                   49.382(7)
_cell_measurement_reflns_used    3290
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      72.9
_cell_measurement_theta_min      30.7
_cell_volume                     4017.8(8)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            53658
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.995
_diffrn_reflns_theta_max         65.995
_diffrn_reflns_theta_min         3.580
_exptl_absorpt_coefficient_mu    2.437
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 1131 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.478(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3507
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0853
_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^)+(0.1412P)^2^+7.1101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2422
_refine_ls_wR_factor_ref         0.2449
_reflns_Friedel_coverage         0.614
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3284
_reflns_number_total             3507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00044f2.cif
_cod_data_source_block           423yan
_cod_depositor_comments
'Adding full bibliography for 1560212--1560217.cif.'
_cod_original_cell_volume        4017.8(10)
_cod_original_formula_sum        'C28.50 H16.50 Cl1.50 O'
_cod_database_code               1560217
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.528
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              21720
_shelx_hkl_checksum              1002