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_7103173
_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         'C27 H28 N6 Pd S2'
_chemical_formula_sum            'C27 H28 N6 Pd S2'
_chemical_formula_weight         607.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.311(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3605(8)
_cell_length_b                   23.687(3)
_cell_length_c                   11.4803(9)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.95
_cell_measurement_theta_min      1.85
_cell_volume                     2752.6(5)
_computing_cell_refinement       'Stoe Cell'
_computing_data_collection       'Stoe Expose'
_computing_data_reduction        'Stoe Integrate'
_computing_publication_material  'WinGX v1.64.05'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1992)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'IPDS 1 (Stoe)'
_diffrn_measurement_method       phi-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21357
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.8562
_exptl_absorpt_correction_T_min  0.7657
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of 8 x 8 x 8 = 512 sampling points was used
PLATON-ABSGAUSS (1980-2003 A.L.Spek) was used for abs. correction.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_recrystallization_method
'Cryst. of (4-tBuBTI)Pd from sol. in pyridine layered by n-hexane.'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                4332
_reflns_number_total             5282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802185f.txt
_cod_data_source_block           ck30ck
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7103173