Synthesis and Optical Resolution of Aminophosphines with Axially Chiral C(aryl)-N(amine) Bonds for Use as Ligands in Asymmetric Catalysis
Takashi Mino; Youichi Tanaka; Youtaro Hattori; Toshihiro Yabusaki; Hiroaki Saotome; Masami Sakamoto; Tsutomu Fujita; Journal of Organic Chemistry 71 (2006) 7346–7353; doi:10.1021/jo061261f

data_4021963
_publ_section_title
;
 Synthesis and Optical Resolution of Aminophosphines with Axially
 Chiral C(aryl)-N(amine) Bonds for Use as Ligands in Asymmetric
 Catalysis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7346
_journal_page_last               7353
_journal_paper_doi               10.1021/jo061261f
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C40 H38 Cl N2 P Pd '
_chemical_formula_sum            'C40 H38 Cl N2 P Pd'
_chemical_formula_weight         719.58
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             2005-03-01
_audit_creation_method           'by CrystalStructure v3.5.1'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4700(13)
_cell_length_b                   15.561(2)
_cell_length_c                   22.835(3)
_cell_measurement_reflns_used    15294
_cell_measurement_temperature    293.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     3720.3(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.5.1'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.9895
_diffrn_measured_fraction_theta_max 0.9895
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71302
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480.00
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.26
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   5.223
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     444
_refine_ls_number_reflns         4346
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.0040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1.0'
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                4346
_reflns_number_total             4728
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo061261fsi20060619_091316.cif
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C40 H38 Cl N2 P Pd '
_cod_database_code               4021963