Asymmetric Synthesis of Functionalized 1,3-Diphosphines via Chiral Palladium Complex Promoted Hydrophosphination of Activated Olefins
Mingjun Yuan; Na Zhang; Sumod A. Pullarkat; Yongxin Li; Fengli Liu; Phuong-Tu Pham; Pak-Hing Leung; Inorganic Chemistry 49 (2010) 989–996; doi:10.1021/ic9018053

data_4314666
_publ_section_title
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 Asymmetric Synthesis of Functionalized 1,3-Diphosphines via Chiral
 Palladium Complex Promoted Hydrophosphination of Activated Olefins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              989
_journal_page_last               996
_journal_paper_doi               10.1021/ic9018053
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H30 Cl2 O P2 Pd'
_chemical_formula_sum            'C30 H30 Cl2 O P2 Pd'
_chemical_formula_weight         645.78
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.704(5)
_cell_angle_beta                 99.824(5)
_cell_angle_gamma                107.217(5)
_cell_formula_units_Z            2
_cell_length_a                   8.5973(10)
_cell_length_b                   10.8849(12)
_cell_length_c                   16.260(2)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1404.3(3)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35186
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.9252
_exptl_absorpt_correction_T_min  0.8270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         9991
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0397P)^2^+1.1710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                8868
_reflns_number_total             9991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9018053_si_001_3.cif
_cod_data_source_block           leung274
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314666