Bifunctional Photocatalysts for Enantioselective Aerobic Oxidation of β-Ketoesters.
Ding, Wei; Lu, Liang-Qiu; Zhou, Quan-Quan; Wei, Yi; Chen, Jia-Rong; Xiao, Wen-Jing; Journal of the American Chemical Society 139 (2017) 63–66; doi:10.1021/jacs.6b11418

data_4125637
_publ_section_title
;
 Bifunctional Photocatalysts for Enantioselective Aerobic Oxidation of
 \b-Ketoesters.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              63
_journal_page_last               66
_journal_paper_doi               10.1021/jacs.6b11418
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H38 O5'
_chemical_formula_sum            'C30 H38 O5'
_chemical_formula_weight         478.60
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                68.5180(10)
_cell_angle_beta                 89.2290(10)
_cell_angle_gamma                77.5010(10)
_cell_formula_units_Z            2
_cell_length_a                   6.3690(3)
_cell_length_b                   14.0432(6)
_cell_length_c                   15.4534(6)
_cell_measurement_reflns_used    9178
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      3.08
_cell_volume                     1252.37(9)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30062
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.358
_diffrn_reflns_theta_min         3.081
_exptl_absorpt_coefficient_mu    0.677
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 4149 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+0.1899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                8711
_reflns_number_total             8804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11418_si_001.cif
_cod_data_source_block           t
_cod_database_code               4125637
_shelx_estimated_absorpt_t_min   0.823
_shelx_estimated_absorpt_t_max   0.876
_shelxl_version_number           2014-3
_shelx_res_checksum              12
_shelx_hkl_checksum              90070