Reductive C(sp(2))-N Elimination from Isolated Pd(IV) Amido Aryl Complexes Prepared Using H2O2 as Oxidant.
Abada, Elikplim; Zavalij, Peter Y.; Vedernikov, Andrei N.; Journal of the American Chemical Society 139 (2017) 643–646; doi:10.1021/jacs.6b12648

data_4125753
_publ_section_title
;
 Reductive C(sp(2))-N Elimination from Isolated Pd(IV) Amido Aryl
 Complexes Prepared Using H2O2 as Oxidant.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              643
_journal_page_last               646
_journal_paper_doi               10.1021/jacs.6b12648
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C24 H18 F3 N3 O5 Pd S, C2 H3 N'
_chemical_formula_sum            'C26 H21 F3 N4 O5 Pd S'
_chemical_formula_weight         664.93
_chemical_name_systematic        Pd-complx
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 101.7876(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1494(7)
_cell_length_b                   12.7371(7)
_cell_length_c                   31.5681(16)
_cell_measurement_reflns_used    19038
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.2
_cell_volume                     5175.7(5)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0505369
_diffrn_orient_matrix_UB_12      -0.0009697
_diffrn_orient_matrix_UB_13      0.0283560
_diffrn_orient_matrix_UB_21      0.0589948
_diffrn_orient_matrix_UB_22      0.0021633
_diffrn_orient_matrix_UB_23      -0.0155723
_diffrn_orient_matrix_UB_31      -0.0009974
_diffrn_orient_matrix_UB_32      0.0784750
_diffrn_orient_matrix_UB_33      0.0007793
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            84561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         15081
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+3.9800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11922
_reflns_number_total             15081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2761.cif
_cod_data_source_block           2761
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4125753
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.781
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              77899
_shelx_hkl_checksum              2330