Reactivity of a Pd(I)-Pd(I) Dimer with O2: Monohapto Pd Superoxide and Dipalladium Peroxide in Equilibrium
Rafael Huacuja; Daniel J. Graham; Claudia M. Fafard; Chun-Hsing Chen; Bruce M. Foxman; David E. Herbert; Glen Alliger; Christine M. Thomas; Oleg V. Ozerov; Journal of the American Chemical Society 133 (2011) 3820–3823; doi:10.1021/ja200346a

data_4105802
_publ_section_title
;
 Reactivity of a Pd(I)-Pd(I) Dimer with O2: Monohapto Pd Superoxide and
 Dipalladium Peroxide in Equilibrium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3820
_journal_page_last               3823
_journal_paper_doi               10.1021/ja200346a
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C24 H34 F2 N O P2 Pd'
_chemical_formula_weight         558.86
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.419(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.58(2)
_cell_length_b                   20.65(2)
_cell_length_c                   13.762(14)
_cell_measurement_reflns_used    6130
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      2.32
_cell_volume                     4998(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22047
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.162
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.582
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.314
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4367
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.311
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+207.2796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2289
_reflns_number_gt                4062
_reflns_number_total             4367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200346a_si_002.cif
_cod_data_source_block           oz234_ii_sad_tri
_cod_original_cell_volume        4997(9)
_cod_database_code               4105802