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_4111456
_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            'C30.5 H45.5 N3 O Pd'
_chemical_formula_weight         576.60
_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                93.220(4)
_cell_angle_beta                 110.871(3)
_cell_angle_gamma                98.433(3)
_cell_formula_units_Z            4
_cell_length_a                   13.9617(12)
_cell_length_b                   14.0737(11)
_cell_length_c                   17.2592(14)
_cell_measurement_temperature    153(2)
_cell_volume                     3112.9(4)
_computing_cell_refinement       'Bruker SAINT program Vers. 5.0'
_computing_data_collection       'Bruker SMART CCD area detector system'
_computing_data_reduction        'Bruker SAINT program Vers. 5.0'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            'Smart 1000 CCD area detector'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'four-circle diffractometer Bruker P4'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans,
 in omega at 0.3 deg scan width, three runs with 98, 67 and 67 frames, phi=0 deg
 in phi at 0.3 deg scan width, two runs with 1207 frames, omega=-32 deg
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_sigmaI/netI    0.2159
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46750
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.47
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           250
_diffrn_source_power             47
_diffrn_source_size              '10 mm x 0.5 mm fine focus'
_diffrn_source_type              'MACScience Co. M18X-HF'
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.670673
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Siemens SADABS program multi-scan
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       needle
_exptl_crystal_F_000             1214
_exptl_crystal_preparation
;
 Slow evaporation of dichloromethane under inert conditions
;
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.544
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.773
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         18397
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.772
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0281P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                8089
_reflns_number_total             18397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0441192Bsi20040927_052928.cif
_cod_data_source_block           1a-NCCH3
_cod_original_formula_sum        'C30.50 H45.50 N3 O Pd'
_cod_database_code               4111456