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_4511978
_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         'C42 H64 P4 Pd2 S4, C4 H10 O'
_chemical_formula_sum            'C46 H74 O P4 Pd2 S4'
_chemical_formula_weight         1108.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90
_cell_angle_beta                 113.610(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0562(8)
_cell_length_b                   14.0451(7)
_cell_length_c                   22.0832(9)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.46
_cell_measurement_wavelength     0.71073
_cell_volume                     5131.5(4)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            77988
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.9603
_exptl_absorpt_correction_T_min  0.9070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.954
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         9358
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.1
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+3.7313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.104
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                7686
_reflns_number_total             9358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs5010322_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4511978--4511979.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4511978