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_4115490
_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         '(((C6 H11)2 P)2 C H2)2 Pd2'
_chemical_formula_sum            'C50 H92 P4 Pd2'
_chemical_formula_weight         1029.92
_chemical_name_systematic
; 
 Mu-bis(bis(dicyclohexylphosphino)methane)dipalladium(Pd-Pd) 
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.713(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3049(14)
_cell_length_b                   19.636(2)
_cell_length_c                   16.8965(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.69
_cell_measurement_theta_min      19.07
_cell_volume                     5207.5(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9590
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        17.6
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.6081
_exptl_absorpt_correction_T_min  0.5511
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scans (Northe, et al., 1968)'
_exptl_crystal_colour            'Dark orange-red'
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       Block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                5309
_reflns_number_total             9245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0056062_2.cif
_cod_data_source_block           mjf225
_cod_database_code               4115490