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_4314665
_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 O2 P2 Pd'
_chemical_formula_sum            'C30 H30 Cl2 O2 P2 Pd'
_chemical_formula_weight         661.78
_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                96.552(2)
_cell_angle_beta                 99.248(2)
_cell_angle_gamma                106.096(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6202(3)
_cell_length_b                   10.7327(4)
_cell_length_c                   16.3388(6)
_cell_measurement_reflns_used    8179
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1413.29(9)
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31857
_diffrn_reflns_theta_full        30.60
_diffrn_reflns_theta_max         30.60
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.9616
_exptl_absorpt_correction_T_min  0.7837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.391
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         14208
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0583P)^2^+3.8890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                11993
_reflns_number_total             14208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9018053_si_001_2.cif
_cod_data_source_block           leung268
_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               4314665