Iron-catalysed asymmetric tandem spiro-cyclization using dioxygen in air as the hydrogen acceptor
Takuya Oguma; Tsutomu Katsuki; Chem.Commun. 50 (2014) 5053–; doi:10.1039/C4CC01555J

data_7112618
_publ_section_title
;
 Iron-catalysed asymmetric tandem spiro-cyclization using dioxygen in air
 as the hydrogen acceptor
;
_journal_name_full               Chem.Commun.
_journal_page_first              5053
_journal_paper_doi               10.1039/C4CC01555J
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H13 Br O2'
_chemical_formula_sum            'C18 H13 Br O2'
_chemical_formula_weight         341.20
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   5.42559(13)
_cell_length_b                   12.7257(3)
_cell_length_c                   21.3576(5)
_cell_measurement_reflns_used    11750
_cell_measurement_temperature    296
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      3.48
_cell_volume                     1474.62(6)
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0787
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15195
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.810
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             688.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.750
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1093 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.04(7)
_refine_ls_extinction_coef       0.0083(13)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2693
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1442P)^2^+1.6815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2344
_reflns_number_gt                1985
_reflns_number_total             2693
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc01555j2.cif
_cod_data_source_block           130517
_cod_database_code               7112618