Chiral Amino Alcohol Derived Bis-phosphoramidite Pincer Palladium Complexes and Their Applications in Asymmetric Allylation of Aldimines
Li, Jie; Lutz, Martin; Spek, Anthony L.; van Klink, Gerard P. M.; van Koten, Gerard; Klein Gebbink, Robertus J. M.; Organometallics 29 (2010) 1379–; doi:10.1021/om100021p

data_4065606
_publ_section_title
;
 Chiral Amino Alcohol Derived Bis-phosphoramidite Pincer Palladium
 Complexes and Their Applications in Asymmetric Allylation of Aldimines
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1379
_journal_paper_doi               10.1021/om100021p
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H37 I N2 O4 P2 Pd, 0.85(C4 H10 O)'
_chemical_formula_sum            'C43.4 H45.5 I N2 O4.85 P2 Pd'
_chemical_formula_weight         967.96
_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                 108.878(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.5613(5)
_cell_length_b                   9.5680(2)
_cell_length_c                   17.5560(9)
_cell_measurement_reflns_used    18879
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.59
_cell_volume                     2155.44(15)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40685
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             975
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.027(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         9826
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0268P)^2^+1.0403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                8492
_reflns_number_total             9826
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om100021p_si_001.cif
_cod_data_source_block           s3840a
_cod_original_cell_volume        2155.43(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C43.40 H45.50 I N2 O4.85 P2 Pd'
_cod_database_code               4065606