Catalytic Enantioselective O-Nitrosocarbonyl Aldol Reaction of β-Dicarbonyl Compounds
Mahiuddin Baidya; Kimberly A. Griffin; Hisashi Yamamoto; Journal of the American Chemical Society 134 (2012) 18566–18569; doi:10.1021/ja309311z

data_4118908
_publ_section_title
;
 Catalytic Enantioselective O-Nitrosocarbonyl Aldol Reaction of
 \b-Dicarbonyl Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18566
_journal_page_last               18569
_journal_paper_doi               10.1021/ja309311z
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C100 H124 N4 O20 S4'
_chemical_formula_weight         1830.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.581(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   11.688(4)
_cell_length_b                   12.115(4)
_cell_length_c                   19.217(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2389.5(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22894
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9537
_exptl_absorpt_correction_T_min  0.9348
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.721
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.721
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                3117
_reflns_number_total             4307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309311z_si_004.cif
_cod_data_source_block           baid36s
_cod_database_code               4118908