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_4105610
_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_moiety         'C54 H72 N4 O4 Pd,(C6 H14)0.5'
_chemical_formula_sum            'C57 H79 N4 O4 Pd'
_chemical_formula_weight         990.64
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.647(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.766(4)
_cell_length_b                   15.624(4)
_cell_length_c                   25.915(8)
_cell_measurement_reflns_used    13739
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.0
_cell_volume                     5416(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1201
_diffrn_reflns_av_sigmaI/netI    0.1264
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31509
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.9488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.271
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.1261
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+100.3336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2906
_refine_ls_wR_factor_ref         0.3092
_reflns_number_gt                6664
_reflns_number_total             9637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1103348_si_002.cif
_cod_data_source_block           sngf27
_cod_database_code               4105610