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_4125754
_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 H21 N3 O5 Pd S, C4 H8 O'
_chemical_formula_sum            'C28 H29 N3 O6 Pd S'
_chemical_formula_weight         642.00
_chemical_name_common            Pd-complex
_chemical_name_systematic
;
Pd-complex
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 118.7580(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.3195(17)
_cell_length_b                   11.3339(6)
_cell_length_c                   17.6574(10)
_cell_measurement_reflns_used    14739
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.5
_cell_volume                     5319.4(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      -0.0188162
_diffrn_orient_matrix_UB_12      -0.0754556
_diffrn_orient_matrix_UB_13      -0.0078589
_diffrn_orient_matrix_UB_21      -0.0118629
_diffrn_orient_matrix_UB_22      0.0030053
_diffrn_orient_matrix_UB_23      -0.0635105
_diffrn_orient_matrix_UB_31      0.0303429
_diffrn_orient_matrix_UB_32      -0.0456301
_diffrn_orient_matrix_UB_33      0.0088338
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42529
_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         29.999
_diffrn_reflns_theta_min         1.953
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.387
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7749
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.387
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+4.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6443
_reflns_number_total             7749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2578.cif
_cod_data_source_block           2578
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4125754
_shelx_estimated_absorpt_t_min   0.846
_shelx_estimated_absorpt_t_max   0.922
_shelxl_version_number           2014-3
_shelx_res_checksum              66170
_shelx_hkl_checksum              6017