Efficient Enantioselective Synthesis of Oxahelicenes Using Redox/Acid Cooperative Catalysts.
Sako, Makoto; Takeuchi, Yoshiki; Tsujihara, Tetsuya; Kodera, Junpei; Kawano, Tomikazu; Takizawa, Shinobu; Sasai, Hiroaki; Journal of the American Chemical Society 138 (2016) 11481–11484; doi:10.1021/jacs.6b07424

data_4130846
_publ_section_title
;
 Efficient Enantioselective Synthesis of Oxahelicenes Using Redox/Acid
 Cooperative Catalysts.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11481
_journal_page_last               11484
_journal_paper_doi               10.1021/jacs.6b07424
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C36.5 H21 Cl O'
_chemical_formula_sum            'C36.5 H21 Cl O'
_chemical_formula_weight         511.02
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   '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                 105.568(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.0088(4)
_cell_length_b                   10.2881(3)
_cell_length_c                   16.7851(12)
_cell_measurement_reflns_used    11155
_cell_measurement_temperature    123
_cell_measurement_theta_max      67.73
_cell_measurement_theta_min      3.06
_cell_volume                     2496.7(2)
_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  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID 191R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48716
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1060.00
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.630
_refine_diff_density_min         -1.700
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  4231 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.003(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     737
_refine_ls_number_reflns         9074
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0033Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1567
_reflns_number_gt                8132
_reflns_number_total             9074
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja6b07424_si_002.cif
_cod_data_source_block           54(5)
_cod_depositor_comments
;

2020-04-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2496.7(3)
_cod_original_formula_moiety     'C73 H42 Cl2 O2'
_cod_original_formula_sum        'C73 H42 Cl2 O2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1022.04
_cod_database_code               4130846