Iron-Catalyzed Asymmetric Epoxidation of β,β-Disubstituted Enones
Yasuhiro Nishikawa; Hisashi Yamamoto; Journal of the American Chemical Society 133 (2011) 8432–8435; doi:10.1021/ja201873d

data_4106194
_publ_section_title
;
 Iron-Catalyzed Asymmetric Epoxidation of \b,\b-Disubstituted Enones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8432
_journal_page_last               8435
_journal_paper_doi               10.1021/ja201873d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C94 H62 F6 Fe N6 O7 S2'
_chemical_formula_weight         1621.47
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                108.511(3)
_cell_angle_beta                 90.726(3)
_cell_angle_gamma                112.000(3)
_cell_formula_units_Z            2
_cell_length_a                   12.581(2)
_cell_length_b                   16.682(3)
_cell_length_c                   21.338(4)
_cell_measurement_temperature    100(2)
_cell_volume                     3893.1(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.1120
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47447
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.9498
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         18748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.102
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                10808
_reflns_number_total             18748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201873d_si_001.cif
_cod_data_source_block           nish02s
_cod_original_cell_volume        3892.9(12)
_cod_database_code               4106194