Enhanced Catalytic Performance of Indenediide Palladium Pincer Complexes for Cycloisomerization: Efficient Synthesis of Alkylidene Lactams
Espinosa-Jalapa, Noel Ángel; Ke, Diandian; Nebra, Noel; Le Goanvic, Lucas; Mallet-Ladeira, Sonia; Monot, Julien; Martin-Vaca, Blanca; Bourissou, Didier; ACS Catalysis 4 (2014) 3605–; doi:10.1021/cs5010322

data_4511979
_publ_section_title
;
 Enhanced Catalytic Performance of Indenediide Palladium Pincer Complexes
 for Cycloisomerization: Efficient Synthesis of Alkylidene Lactams
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              3605
_journal_paper_doi               10.1021/cs5010322
_journal_volume                  4
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'2(C21 H32 Cl P2 Pd S2), 2(C16 H36 N), C H2 Cl2'
_chemical_formula_sum            'C75 H138 Cl4 N2 P4 Pd2 S4'
_chemical_formula_weight         1674.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                91.6030(10)
_cell_angle_beta                 90.239(2)
_cell_angle_gamma                103.7250(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2156(3)
_cell_length_b                   16.2747(5)
_cell_length_c                   26.6821(8)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.25
_cell_measurement_wavelength     0.71073
_cell_volume                     4307.4(2)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0237
_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       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            85271
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.9706
_exptl_absorpt_correction_T_min  0.8402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         15749
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.031
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+4.4350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                13571
_reflns_number_total             15749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs5010322_si_002.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 4511978--4511979.cif.'
_cod_database_code               4511979