Copper-Catalyzed anti-Hydrophosphination Reaction of 1-Alkynylphosphines with Diphenylphosphine Providing (Z)-1,2-Diphosphino-1-alkenes
Azusa Kondoh; Hideki Yorimitsu; Koichiro Oshima; Journal of the American Chemical Society 129 (2007) 4099–4104; doi:10.1021/ja070048d

data_4109276
_publ_contact_author             'Hideki Yorimitsu'
_publ_contact_author_email       yori@orgrxn.mbox.media.kyoto-u.ac.jp
_publ_contact_author_fax         +81-75-383-2438
_publ_contact_author_phone       +81-75-383-2441
_publ_section_title
;
 Copper-Catalyzed anti-Hydrophosphination Reaction of 1-Alkynylphosphines
 with Diphenylphosphine Providing (Z)-1,2-Diphosphino-1-alkenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4099
_journal_page_last               4104
_journal_paper_doi               10.1021/ja070048d
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C30 H30 Cl2 Ni P2'
_chemical_formula_weight         582.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.6080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6193(7)
_cell_length_b                   15.4796(9)
_cell_length_c                   16.0015(9)
_cell_measurement_reflns_used    5328
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.466
_cell_volume                     2797.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16920
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        -1.36
_diffrn_standards_interval_time  200
_diffrn_standards_number         387
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' dark red'
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       ' block'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.682
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.682
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1082P)^2^+2.0209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                5305
_reflns_number_total             6085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070048dsi20070104_012939.cif
_cod_data_source_block           1az
_cod_database_code               4109276