Facile intramolecular C(sp3)-H bond activation with PdII.
Bröring, Martin; Kleeberg, Christian; Chemical communications (Cambridge, England)  (2008) 2777–2778; doi:10.1039/b802185f

data_7103174
_publ_section_title
;
 Facile intramolecular C(sp3)-H bond activation with PdII.
;
_journal_issue                   24
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2777
_journal_page_last               2778
_journal_paper_doi               10.1039/b802185f
_journal_year                    2008
_chemical_formula_moiety         'C22 H23 N5 Pd S2'
_chemical_formula_sum            'C22 H23 N5 Pd S2'
_chemical_formula_weight         527.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.23(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0131(16)
_cell_length_b                   15.444(6)
_cell_length_c                   25.514(7)
_cell_measurement_reflns_used    5918
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      11.54
_cell_volume                     2368.8(13)
_computing_cell_refinement       'STOE Wincell (X-Area, Ver. 1.38)'
_computing_data_collection       'STOE WinXpose (X-Area, Ver. 1.38)'
_computing_data_reduction        'STOE WinIntegrate (X-Area, Ver. 1.38)'
_computing_publication_material  'WinGX v1.70.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1992)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'IPDS-2 (Stoe)'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4079
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_recrystallization_method
'Diffusion of n-Hexane into a sol. in CHCl3/C6F6'
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                3005
_reflns_number_total             4079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802185f.txt
_cod_data_source_block           nh4ck
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7103174