Norbornadiene as a Building Block for the Synthesis of Linked Benzazocinones and Benzazocinium Salts through Tetranuclear Carbopalladated Intermediates
García-López, José Antonio; Frutos-Pedreño, Roberto; Bautista, Delia; Saura-Llamas, Isabel; Vicente, José; Organometallics 36 (2017) 372–; doi:10.1021/acs.organomet.6b00795

data_4086885
_publ_section_title
;
 Norbornadiene as a Building Block for the Synthesis of Linked
 Benzazocinones and Benzazocinium Salts through Tetranuclear
 Carbopalladated Intermediates
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              372
_journal_paper_doi               10.1021/acs.organomet.6b00795
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C26.5 H32 Cl2 N2 Pd'
_chemical_formula_weight         555.84
_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                88.334(2)
_cell_angle_beta                 75.903(2)
_cell_angle_gamma                84.385(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9593(9)
_cell_length_b                   10.9676(11)
_cell_length_c                   13.2131(13)
_cell_measurement_reflns_used    5093
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.35
_cell_volume                     1253.2(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.921
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15663
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.9264
_exptl_absorpt_correction_T_min  0.8035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment
'NH2 free with SADI, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5924
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0274P)^2^+1.7530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                5764
_reflns_number_total             5924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00795_si_002.cif
_cod_data_source_block           jag513s
_cod_depositor_comments
'Adding full bibliography for 4086885--4086890.cif.'
_cod_original_formula_sum        'C26.50 H32 Cl2 N2 Pd'
_cod_database_code               4086885