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_4105801
_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_moiety         'C28 H42 F2 N1 O3 P2 Pd1'
_chemical_formula_sum            'C28 H42 F2 N O3 P2 Pd'
_chemical_formula_weight         646.99
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-04-11
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 106.5060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9685(4)
_cell_length_b                   11.7323(3)
_cell_length_c                   14.7031(3)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2971.85(12)
_computing_cell_refinement       'Apex2, (Bruker AXS, 2006)'
_computing_data_collection       'Apex2, (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2, (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59805
_diffrn_reflns_theta_full        30.122
_diffrn_reflns_theta_max         30.122
_diffrn_reflns_theta_min         1.182
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker AXS, 2006)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.73
_refine_diff_density_min         -1.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         8753
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.93P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0733
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0733
_reflns_limit_h_max              24
_reflns_limit_h_min              -25
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7014
_reflns_number_total             8753
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0356
_oxford_refine_ls_scale          0.097449(16)
_oxford_reflns_number_all        8753
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ152_0ma in P2(1)/c'
_cod_data_source_file            ja200346a_si_001.cif
_cod_data_source_block           OZ152
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C28 H42 F2 N1 O3 P2 Pd1'
_cod_database_code               4105801