Room-Temperature Isolation of Palladium(II) Organocarbonyl Intermediates in the Synthesis of Eight-Membered Lactams after Alkyne/CO Sequential Insertions
Garc\?ía-López, José-Antonio; Oliva-Madrid, Mar\?ía-José; Saura-Llamas, Isabel; Bautista, Delia; Vicente, José; Organometallics 32 (2013) 1094–; doi:10.1021/om301241n

data_4080095
_publ_section_title
;
 Room-Temperature Isolation of Palladium(II) Organocarbonyl Intermediates
 in the Synthesis of Eight-Membered Lactams after Alkyne/CO Sequential
 Insertions
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1094
_journal_paper_doi               10.1021/om301241n
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C40 H44 Cl2 N2 O4 Pd2'
_chemical_formula_weight         900.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.861(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5407(10)
_cell_length_b                   12.1740(15)
_cell_length_c                   18.682(2)
_cell_measurement_reflns_used    3159
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.21
_cell_volume                     1919.3(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.978
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12070
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  0.9258
_exptl_absorpt_correction_T_min  0.7902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment
'NH2 free with SADI, rigid methyls, other riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4479
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+2.4715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                3949
_reflns_number_total             4479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301241n_si_002.cif
_cod_data_source_block           jakxs076
_cod_original_cell_volume        1919.2(4)
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               4080095