Key Mechanistic Features of Enantioselective C-H Bond Activation Reactions Catalyzed by [(Chiral Mono-N-Protected Amino Acid)-Pd(II)] Complexes
Djamaladdin G. Musaev; Alexey Kaledin; Bing-Feng Shi; Jin-Quan Yu; Journal of the American Chemical Society 134 (2012) 1690–1698; doi:10.1021/ja208661v

data_4117327
_publ_section_title
;
 Key Mechanistic Features of Enantioselective C-H Bond Activation
 Reactions Catalyzed by [(Chiral Mono-N-Protected Amino Acid)-Pd(II)]
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1690
_journal_page_last               1698
_journal_paper_doi               10.1021/ja208661v
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C41 H36 Cl2 N2 O4 Pd2'
_chemical_formula_weight         904.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.632(10)
_cell_length_b                   11.154(2)
_cell_length_c                   14.125(3)
_cell_measurement_reflns_used    7026
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.23
_cell_volume                     7504(3)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53475
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  0.9665
_exptl_absorpt_correction_T_min  0.7868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      0
_exptl_crystal_description       Plate-like
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(6)
_refine_ls_extinction_coef       0.00000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         13227
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+32.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                10020
_reflns_number_total             13227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208661v_si_001.cif
_cod_data_source_block           bing
_cod_original_cell_volume        7505(3)
_cod_database_code               4117327