Dioxygen activation by an organometallic Pd(II) precursor: formation of a Pd(IV)-OH complex and its C-O bond formation reactivity
Fengrui Qu; Julia R. Khusnutdinova; Nigam P. Rath; Liviu M. Mirica; Chem.Commun. 50 (2014) 3036–; doi:10.1039/c3cc49387c

data_7112074
_publ_section_title
;
 Dioxygen activation by an organometallic Pd(II) precursor: formation of a
 Pd(IV)-OH complex and its C-O bond formation reactivity
;
_journal_name_full               Chem.Commun.
_journal_page_first              3036
_journal_paper_doi               10.1039/c3cc49387c
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C19 H33 Cl N3 Pd, Cl O4'
_chemical_formula_sum            'C19 H33 Cl2 N3 O4 Pd'
_chemical_formula_weight         544.78
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5967(7)
_cell_length_b                   8.3780(4)
_cell_length_c                   15.0330(6)
_cell_measurement_reflns_used    9729
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.99
_cell_measurement_theta_min      2.43
_cell_volume                     2090.30(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            79064
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.999
_diffrn_reflns_theta_min         2.431
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.8032
_exptl_absorpt_correction_T_min  0.7252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2012/1'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.251
_refine_diff_density_max         1.843
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
; 
 Flack x determined using 4730 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.002(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         11727
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.6938P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                10814
_reflns_number_total             11727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc49387c.txt
_cod_data_source_block           l5513
_cod_database_code               7112074
_shelx_estimated_absorpt_t_min   0.751
_shelx_estimated_absorpt_t_max   0.757
_shelxl_version_number           2012-9
_shelx_res_checksum              79105
_shelx_hkl_checksum              66304