PyBidine-NiCl2-Catalyzed Asymmetric Addition of Alcohols and Peroxides to Isatin-Derived Ketimines.
Arai, Takayoshi; Tsuchiya, Kento; Matsumura, Eri; Organic letters 17 (2015) 2416–2419; doi:10.1021/acs.orglett.5b00928

data_1555011
_publ_section_title
;
 PyBidine-NiCl2-Catalyzed Asymmetric Addition of Alcohols and Peroxides to
 Isatin-Derived Ketimines.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              2416
_journal_page_last               2419
_journal_paper_doi               10.1021/acs.orglett.5b00928
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C23 H27 Br N2 O5'
_chemical_formula_weight         491.37
_chemical_name_common            arai20150110
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 91.1454(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3956(8)
_cell_length_b                   11.6027(11)
_cell_length_c                   23.715(2)
_cell_measurement_temperature    173
_cell_volume                     2309.7(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13148
_diffrn_reflns_theta_full        27.627
_diffrn_reflns_theta_max         27.627
_diffrn_reflns_theta_min         1.718
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.609
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                3849
_reflns_number_total             5283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b00928_si_001.cif
_cod_data_source_block           I
_cod_database_code               1555011