A highly efficient precatalyst for amination of aryl chlorides: synthesis, structure and application of a robust acenaphthoimidazolylidene palladium complex
Tao Tu; Weiwei Fang; Jiang Jian; Chem.Commun. 47 (2011) 12358–; doi:10.1039/c1cc15503b

data_7107060
_publ_section_title
;
 A highly efficient precatalyst for amination of aryl chlorides:
 synthesis, structure and application of a robust
 acenaphthoimidazolylidene palladium complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              12358
_journal_paper_doi               10.1039/c1cc15503b
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C43 H46 Cl5 N3 Pd'
_chemical_formula_weight         888.48
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.962(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.83(2)
_cell_length_b                   12.576(8)
_cell_length_c                   23.076(14)
_cell_measurement_reflns_used    962
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.370
_cell_measurement_theta_min      2.531
_cell_volume                     9124(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18407
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.9305
_exptl_absorpt_correction_T_min  0.8106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1133P)^2^+25.1782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2238
_reflns_number_gt                5580
_reflns_number_total             7994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15503b.txt
_cod_data_source_block           a10426a
_cod_original_cell_volume        9125(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7107060