Nickel(II)-Catalyzed Highly Enantioselective Hydrophosphination of Methacrylonitrile
Aaron D. Sadow; Isabelle Haller; Luca Fadini; Antonio Togni; Journal of the American Chemical Society 126 (2004) 14704–14705; doi:10.1021/ja0449574

data_4113156
_publ_section_title
;
 Nickel(II)-Catalyzed Highly Enantioselective Hydrophosphination of
 Methacrylonitrile
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14704
_journal_page_last               14705
_journal_paper_doi               10.1021/ja0449574
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration rm
_chemical_formula_sum            'C44 H57 Cl N2 P Pd'
_chemical_formula_weight         786.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.440(2)
_cell_length_b                   16.326(3)
_cell_length_c                   41.174(8)
_cell_measurement_temperature    273(2)
_cell_volume                     7690(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1659
_diffrn_reflns_av_sigmaI/netI    0.2274
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            50377
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.9285
_exptl_absorpt_correction_T_min  0.6338
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         19097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1526
_refine_ls_R_factor_gt           0.0900
_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^)+(0.0219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1431
_reflns_number_gt                11494
_reflns_number_total             19097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0449574si20041008_034853_3.cif
_cod_data_source_block           Compound_S4
_cod_original_cell_volume        7690(3)
_cod_database_code               4113156