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_4086888
_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            'C38 H61 Cl5 N4 O3'
_chemical_formula_weight         799.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                70.643(2)
_cell_angle_beta                 81.038(2)
_cell_angle_gamma                82.093(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5722(8)
_cell_length_b                   14.7572(12)
_cell_length_c                   15.5993(13)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.32
_cell_volume                     2044.8(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2011)'
_computing_data_collection       'APEX2 2014.1-1 (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'w-scans and phi-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1182
_diffrn_reflns_av_unetI/netI     0.1075
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69452
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.366
_diffrn_reflns_theta_min         2.163
_diffrn_source                   'high brilliance microfocus sealed tube '
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       lath
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.591
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9914
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+7.3710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6354
_reflns_number_total             9914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00795_si_002.cif
_cod_data_source_block           rfi35e_1_0msp
_cod_depositor_comments
'Adding full bibliography for 4086885--4086890.cif.'
_cod_database_code               4086888
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              42637
_shelx_hkl_checksum              23914