Asymmetric Synthesis of Diphosphine Ligands Containing Phosphorus and Carbon Stereogenic Centers by Means of a Chiral Palladium Complex Promoted Hydrophosphination Reaction
Zhang, Yi; Pullarkat, Sumod A.; Li, Yongxin; Leung, Pak-Hing; Inorganic chemistry 48 (2009) 5535–5539; doi:10.1021/ic900461t

data_4302377
_publ_section_title
;
 Asymmetric Synthesis of Diphosphine Ligands Containing Phosphorus and
 Carbon Stereogenic Centers by Means of a Chiral Palladium Complex
 Promoted Hydrophosphination Reaction
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5535
_journal_page_last               5539
_journal_paper_doi               10.1021/ic900461t
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H42 N P2 Pd, C H2 Cl2, Cl O4'
_chemical_formula_sum            'C39 H44 Cl3 N O4 P2 Pd'
_chemical_formula_weight         865.44
_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                 92.841(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3975(5)
_cell_length_b                   9.8036(6)
_cell_length_c                   20.7827(11)
_cell_measurement_reflns_used    6669
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.71
_cell_measurement_theta_min      2.43
_cell_volume                     1912.34(19)
_computing_cell_refinement       'Bruker SMART'
_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, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37064
_diffrn_reflns_theta_full        33.39
_diffrn_reflns_theta_max         33.39
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.9225
_exptl_absorpt_correction_T_min  0.8275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         13784
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.0378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                12117
_reflns_number_total             13784
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338548
_cod_data_source_file            ic900461t_si_001_1.cif
_cod_data_source_block           leung314
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4302377