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_4021965
_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_sum            'C29 H26 Cl8 N P Pd'
_chemical_formula_weight         809.53
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Wed Apr 16 11:50:00 2003'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                92.460(4)
_cell_angle_beta                 97.8730(4)
_cell_angle_gamma                106.201(4)
_cell_formula_units_Z            2
_cell_length_a                   8.652(3)
_cell_length_b                   10.517(3)
_cell_length_c                   18.683(6)
_cell_measurement_temperature    100.2
_cell_volume                     1611.3(8)
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_measured_fraction_theta_full 0.8709
_diffrn_measured_fraction_theta_max 0.8709
_diffrn_measurement_device_type  'Quantum CCD/Rigaku AFC7'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9766
_diffrn_reflns_theta_full        28.60
_diffrn_reflns_theta_max         28.60
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.88
_refine_diff_density_min         -1.93
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6427
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.2163
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                3392
_reflns_number_total             7176
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo061261fsi20060619_091401.cif
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C29 H26 Cl8 N P Pd '
_cod_database_code               4021965