The First Example of Simple Oxidative Addition of an Aryl Chloride to a Discrete Palladium N-Heterocyclic Carbene Amination Precatalyst
Caddick, Stephen; Cloke, F. Geoffrey N.; Hitchcock, Peter B.; Leonard, John; Lewis, Alexandra K. de K.; McKerrecher, Darren; Titcomb, Lisa R.; Organometallics 21 (2002) 4318–; doi:10.1021/om020552l

data_4077071
_publ_section_title
;
 The First Example of Simple Oxidative Addition of an Aryl Chloride to a
 Discrete Palladium N-Heterocyclic Carbene Amination Precatalyst
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4318
_journal_paper_doi               10.1021/om020552l
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H47 Cl1 N4 Pd1).2(C6 D6)'
_chemical_formula_sum            'C41 H49 Cl D12 N4 Pd'
_chemical_formula_weight         761.8
_chemical_name_common            '[PdCl(C6H4Me)(C3H2N2tBu2)2].2(C6D6)'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-12-03T09:14:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.785(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5279(6)
_cell_length_b                   13.7541(3)
_cell_length_c                   23.2188(11)
_cell_measurement_reflns_used    21248
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.076
_cell_measurement_wavelength     0.71073
_cell_volume                     3964.0(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20601
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         4.17
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.28
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6950
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+6.7663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                5357
_reflns_number_total             6950
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020552l.cif
_cod_data_source_block           nov2301
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C41 H49 D12 Cl N4 Pd'
_cod_database_code               4077071