Double Heterohelicenes Composed of Benzo[<i>b</i>]- and Dibenzo[<i>b</i>,<i>i</i>]phenoxazine: A Comprehensive Comparison of Their Electronic and Chiroptical Properties.
Sakamaki, Daisuke; Tanaka, Shunya; Tanaka, Katsuki; Takino, Mayu; Gon, Masayuki; Tanaka, Kazuo; Hirose, Takashi; Hirobe, Daichi; Yamamoto, Hiroshi M.; Fujiwara, Hideki; The journal of physical chemistry letters 12 (2021) 9283–9292; doi:10.1021/acs.jpclett.1c02896

data_8000549
_publ_section_title
;
 Double Heterohelicenes Composed of Benzo[<i>b</i>]- and
 Dibenzo[<i>b</i>,<i>i</i>]phenoxazine: A Comprehensive Comparison of
 Their Electronic and Chiroptical Properties.
;
_journal_issue                   38
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              9283
_journal_page_last               9292
_journal_paper_doi               10.1021/acs.jpclett.1c02896
_journal_volume                  12
_journal_year                    2021
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C32 H18 N2 O2, 0.5(C6 H14)'
_chemical_formula_sum            'C35 H25 N2 O2'
_chemical_formula_weight         505.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.931(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.7291(2)
_cell_length_b                   12.2843(3)
_cell_length_c                   19.3087(4)
_cell_measurement_reflns_used    14129
_cell_measurement_temperature    296
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      2.19
_cell_volume                     2538.89(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Rigaku XtaLAB PRO'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36471
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.364
_diffrn_reflns_theta_min         2.239
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1060.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details
;
 Flack x determined using 3708 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13299
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0642P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.821
_reflns_number_gt                9915
_reflns_number_total             13299
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jz1c02896_si_004.cif
_cod_data_source_block           xcalibur
_cod_depositor_comments
;

2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C70 H50 N4 O4'
_cod_original_formula_weight         1011.19
_cod_original_formula_moiety         'C70 H50 N4 O4'
_cod_original_formula_units_Z            2
_cod_database_code               8000549
_shelx_res_checksum              12756
_shelx_hkl_checksum              75997