Mechanistic Studies of the Insertion of CO2into Palladium(I) Bridging Allyl Dimers
Hruszkewycz, Damian P.; Wu, Jianguo; Green, Jennifer C.; Hazari, Nilay; Schmeier, Timothy J.; Organometallics 31 (2012) 470–; doi:10.1021/om201163k

data_4068169
_publ_section_title
;
 Mechanistic Studies of the Insertion of CO2into Palladium(I) Bridging
 Allyl Dimers
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              470
_journal_paper_doi               10.1021/om201163k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'Pd2 O2 C61 H86 N4'
_chemical_formula_sum            'C61 H86 N4 O2 Pd2'
_chemical_formula_weight         1120.18
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.576(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.2110(5)
_cell_length_b                   18.5314(6)
_cell_length_c                   22.6888(16)
_cell_measurement_reflns_used    20846
_cell_measurement_temperature    93
_cell_measurement_theta_max      63.70
_cell_measurement_theta_min      2.02
_cell_volume                     5755.7(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46501
_diffrn_reflns_theta_full        63.69
_diffrn_reflns_theta_max         63.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.362
_exptl_absorpt_correction_T_max  0.342
_exptl_absorpt_correction_T_min  0.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2352.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.940
_refine_diff_density_min         -1.420
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     622
_refine_ls_number_reflns         9430
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0892P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                5766
_reflns_number_total             9754
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om201163k_si_002.cif
_cod_data_source_block           '_II-SIPr-A'
_cod_original_formula_sum        'Pd2 O2 C61 H86 N4'
_cod_database_code               4068169