Synthesis and Reactivity of Ortho-Palladated Phenylacetamides. Intramolecular C−N vs C−O Reductive Coupling after CO or XyNC Insertion into the Pd−C Bond. Synthesis of Isoquinoline- and Isocoumarin-Based Heterocycles
Vicente, José; González-Herrero, Pablo; Frutos-Pedreño, Roberto; Chicote, María-Teresa; Jones, Peter G.; Bautista, Delia; Organometallics 30 (2011) 1079–; doi:10.1021/om101110s

data_4064054
_publ_section_title
;
 Synthesis and Reactivity of Ortho-Palladated Phenylacetamides.
 Intramolecular C&#x2212;N vs C&#x2212;O Reductive Coupling after CO or
 XyNC Insertion into the Pd&#x2212;C Bond. Synthesis of Isoquinoline- and
 Isocoumarin-Based Heterocycles
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1079
_journal_paper_doi               10.1021/om101110s
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C27.5 H34 Cl N3 O Pd'
_chemical_formula_weight         564.43
_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                95.000(2)
_cell_angle_beta                 99.522(2)
_cell_angle_gamma                105.510(2)
_cell_formula_units_Z            4
_cell_length_a                   12.1373(5)
_cell_length_b                   13.4080(6)
_cell_length_c                   16.7547(7)
_cell_measurement_reflns_used    7140
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.36
_cell_volume                     2566.23(19)
_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 0.914
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29868
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.9350
_exptl_absorpt_correction_T_min  0.7744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    'ordered methyls rigid, other riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         11505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0359P)^2^+3.9498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                9754
_reflns_number_total             11505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101110s_si_003.cif
_cod_data_source_block           rfa23bs
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C27.50 H34 Cl N3 O Pd'
_cod_database_code               4064054