Facile Reductive Elimination of Ethane from Strained Dimethylpalladium(II) Complexes
Steven M. Reid; Joel T. Mague; Mark J. Fink; Journal of the American Chemical Society 123 (2001) 4081–4082; doi:10.1021/ja0056062

data_4115489
_publ_section_title
;
 Facile Reductive Elimination of Ethane from Strained
 Dimethylpalladium(II) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4081
_journal_page_last               4082
_journal_paper_doi               10.1021/ja0056062
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         '(C H3)2 (((C6 H11)2 P)2 C H2) Pd'
_chemical_formula_sum            'C27 H52 P2 Pd'
_chemical_formula_weight         545.03
_chemical_name_systematic
; 
 cis-Dimethyl(bis(dicyclohexylphosphino)methane)palladium(II) 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_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                   16.633(2)
_cell_length_b                   14.7594(14)
_cell_length_c                   23.571(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.70
_cell_measurement_theta_min      17.40
_cell_volume                     5786.5(10)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1987)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1997)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\q/2\q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5144
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        2.1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.6988
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scan (North, et al., 1968)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00138(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+3.9991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                3184
_reflns_number_total             5144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0056062_1.cif
_cod_data_source_block           mjf222
_cod_database_code               4115489