Catalytic Enantioselective Addition of Cyclic β-Keto Esters with Activated Olefins and N-Boc Imines Using ChiralC2-Symmetric Cationic Pd2+N-Heterocyclic Carbene (NHC) Diaqua Complexes
Liu, Zhen; Shi, Min; Organometallics 29 (2010) 2831–; doi:10.1021/om100331z

data_4066166
_publ_section_title
;
 Catalytic Enantioselective Addition of Cyclic \b-Keto Esters with
 Activated Olefins and N-Boc Imines Using ChiralC2-Symmetric Cationic
 Pd2+N-Heterocyclic Carbene (NHC) Diaqua Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2831
_journal_paper_doi               10.1021/om100331z
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_sum            'C22 H30 Br N O5'
_chemical_formula_weight         468.38
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 109.586(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9053(17)
_cell_length_b                   11.2911(18)
_cell_length_c                   11.0981(19)
_cell_measurement_reflns_used    1088
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.098
_cell_measurement_theta_min      4.365
_cell_volume                     1169.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6167
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.788
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75495
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.245
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3660
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1978
_reflns_number_gt                1790
_reflns_number_total             3660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100331z_si_001.cif
_cod_data_source_block           cd29379
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4066166