Oxygen Binding to [Pd(L)(L')] (L= NHC, L' = NHC or PR3, NHC = N-Heterocyclic Carbene). Synthesis and Structure of a Paramagnetic trans-[Pd(NHC)2(η1-O2)2] Complex
Xiaochen Cai; Subhojit Majumdar; George C. Fortman; Catherine S. J. Cazin; Alexandra M. Z. Slawin; Charles Lhermitte; Rajeev Prabhakar; Meaghan E. Germain; Taryn Palluccio; Steven P. Nolan; Elena V. Rybak-Akimova; Manuel Temprado; Burjor Captain; Carl D. Hoff; Journal of the American Chemical Society 133 (2011) 1290–1293; doi:10.1021/ja1103348

data_4105611
_publ_section_title
;
 Oxygen Binding to [Pd(L)(L')] (L= NHC, L' = NHC or PR3, NHC =
 N-Heterocyclic Carbene). Synthesis and Structure of a Paramagnetic
 trans-[Pd(NHC)2(\h1-O2)2] Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1290
_journal_page_last               1293
_journal_paper_doi               10.1021/ja1103348
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C54 H78 N4 O4 Pd'
_chemical_formula_weight         953.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.982(1)
_cell_angle_beta                 87.966(1)
_cell_angle_gamma                89.015(1)
_cell_formula_units_Z            2
_cell_length_a                   12.2884(5)
_cell_length_b                   12.3340(5)
_cell_length_c                   17.2479(7)
_cell_measurement_reflns_used    8624
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.16
_cell_measurement_theta_min      2.33
_cell_volume                     2592.74(18)
_computing_cell_refinement       'SAINT+  V7.46A (Bruker, 2007)'
_computing_data_collection       'APEX2 v2.2-0 (Bruker, 2007)'
_computing_data_reduction        'SAINT+  V7.46A (Bruker, 2007)'
_computing_molecular_graphics    'XSHELL v4.02 (Bruker, 2000)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27560
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/4 Bruker)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         13057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.6079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                10468
_reflns_number_total             13057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1103348_si_003.cif
_cod_data_source_block           collect_0m
_cod_database_code               4105611