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_4076602
_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            'C20 H23 Cl N2 O7 Pd'
_chemical_formula_weight         545.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.108(2)
_cell_angle_beta                 78.096(2)
_cell_angle_gamma                78.395(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6119(6)
_cell_length_b                   8.7766(6)
_cell_length_c                   14.8426(12)
_cell_measurement_reflns_used    8101
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.38
_cell_volume                     1069.90(14)
_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 0.993
_diffrn_measured_fraction_theta_max 0.912
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12439
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_correction_T_min  0.7754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0310P)^2^+0.8601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                4553
_reflns_number_total             4803
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4078290
_cod_data_source_file            om300217k_si_002.cif
_cod_data_source_block           fjd211s
_cod_database_code               4076602