Synthesis and Hydrolysis of Cationic Palladium(II) 2,6-Diacetylpyridine Dimethyl Ketal Complexes. Cyclopalladation of 2,6-Diacetylpyridine. Palladium-Catalyzed Synthesis of a 1,5-Benzodiazepine†
Juliá-Hernández, Francisco; Arcas, Aurelia; Bautista, Delia; Vicente, José; Organometallics 31 (2012) 3736–; doi:10.1021/om300217k

data_4076603
_publ_section_title
;
 Synthesis and Hydrolysis of Cationic Palladium(II)
 2,6-Diacetylpyridine Dimethyl Ketal Complexes. Cyclopalladation of
 2,6-Diacetylpyridine. Palladium-Catalyzed Synthesis of a
 1,5-Benzodiazepine&#x2020;
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3736
_journal_paper_doi               10.1021/om300217k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C11 H11 Cl N2 O6 Pd'
_chemical_formula_weight         409.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.965(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6698(4)
_cell_length_b                   23.7216(12)
_cell_length_c                   7.8644(4)
_cell_measurement_reflns_used    5718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.81
_cell_volume                     1382.32(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15633
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  0.8468
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       neddle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    'rigid methyls, other riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0277P)^2^+1.2715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0565
_reflns_number_gt                3097
_reflns_number_total             3197
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4078291
_cod_data_source_file            om300217k_si_002.cif
_cod_data_source_block           fjd871s
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               4076603