Insertion of Acrylonitrile into Palladium Methyl Bonds in Neutral and Anionic Pd(II) Complexes
Laurent F. Groux; Thomas Weiss; Dastigiri N. Reddy; Preston A. Chase; Warren E. Piers; Tom Ziegler; Masood Parvez; Jordi Benet-Buchholz; Journal of the American Chemical Society 127 (2005) 1854–1869; doi:10.1021/ja044119+

data_4111458
_publ_contact_author
;
    Masood Parvez
    Department of Chemistry
    University of Calgary
    2500 University Drive N.W.
    Calgary, Alberta, Canada T2N 1N4
;
_publ_contact_author_email       parvez@ucalgary.ca
_publ_contact_author_fax         (403)289-9488
_publ_contact_author_phone       (403)220-5348
_publ_section_title
;
 Insertion of Acrylonitrile into Palladium Methyl Bonds in Neutral and
 Anionic Pd(II) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1854
_journal_page_last               1869
_journal_paper_doi               10.1021/ja044119+
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C42 H69.5 B F3 K N2.5 O7 P Pd'
_chemical_formula_weight         965.78
_space_group_IT_number           2
_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                85.573(17)
_cell_angle_beta                 80.042(16)
_cell_angle_gamma                88.58(2)
_cell_formula_units_Z            4
_cell_length_a                   14.004(4)
_cell_length_b                   16.841(5)
_cell_length_c                   21.172(6)
_cell_measurement_reflns_used    40813
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     4903(2)
_computing_cell_refinement       'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \w and \f '
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40813
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_correction_T_min  0.9265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       prism
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1094
_refine_ls_number_reflns         21810
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.367
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+13.1100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                13472
_reflns_number_total             21810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0441192Bsi20040927_052959.cif
_cod_data_source_block           Compound_1c-PMe3
_cod_original_formula_sum        'C42 H69.50 B F3 K N2.50 O7 P Pd'
_cod_database_code               4111458