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_4125756
_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 H16 F3 N3 O3 Pd S, C2 H3 N'
_chemical_formula_sum            'C26 H19 F3 N4 O3 Pd S'
_chemical_formula_weight         630.91
_chemical_name_common            Pd-complex
_chemical_name_systematic
;
Pd-complex
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2012 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 100.943(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.534(2)
_cell_length_b                   9.1331(13)
_cell_length_c                   18.096(3)
_cell_measurement_reflns_used    22678
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4
_cell_measurement_theta_min      2.3
_cell_volume                     2520.7(6)
_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, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2012 (Sheldrick, 2012)'
_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 diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0347370
_diffrn_orient_matrix_UB_12      -0.0691169
_diffrn_orient_matrix_UB_13      -0.0369452
_diffrn_orient_matrix_UB_21      0.0445088
_diffrn_orient_matrix_UB_22      0.0092146
_diffrn_orient_matrix_UB_23      -0.0330540
_diffrn_orient_matrix_UB_31      0.0333323
_diffrn_orient_matrix_UB_32      -0.0844156
_diffrn_orient_matrix_UB_33      0.0266522
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41473
_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         29.998
_diffrn_reflns_theta_min         1.918
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0210
_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^+2.5500P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6641
_reflns_number_total             7352
_reflns_threshold_expression     'I > 2\s(I)'
_iucr_refine_instructions_details 'Available on request'
_cod_data_source_file            2535.cif
_cod_data_source_block           2535
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2520.6(6)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4125756
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.894
_iucr_refine_reflections_details 'Available on request'
_diffrn_measurement_frame_width-ccd 512