Cyclometalated 2-Phenylimidazole Palladium Carbene Complexes in the Catalytic Suzuki‒Miyaura Cross-Coupling Reaction
Micksch, Maik; Tenne, Mario; Strassner, Thomas; Organometallics 33 (2014) 3966–; doi:10.1021/om5004336

data_4084077
_publ_section_title
;
 Cyclometalated 2-Phenylimidazole Palladium Carbene Complexes in the
 Catalytic Suzuki--Miyaura Cross-Coupling Reaction
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3966
_journal_paper_doi               10.1021/om5004336
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C50 H62 N4 O2 Pd'
_chemical_formula_sum            'C50 H62 N4 O2 Pd'
_chemical_formula_weight         857.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.818(12)
_cell_angle_beta                 92.665(10)
_cell_angle_gamma                90.906(9)
_cell_formula_units_Z            2
_cell_length_a                   9.7670(6)
_cell_length_b                   13.1080(17)
_cell_length_c                   17.632(3)
_cell_measurement_reflns_used    995
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      20.339
_cell_measurement_theta_min      4.137
_cell_volume                     2242.8(5)
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius BV, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'ORTEP-3 (Ferrugia, 2012)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SIR97 (Altomare et al., 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       \f
_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  0.0791
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42190
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.9644
_exptl_absorpt_correction_T_min  0.8906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+2.2309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                5133
_reflns_number_total             6406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5004336_si_001.cif
_cod_data_source_block           compound21
_cod_depositor_comments
'Adding full bibliography for 4084075--4084077.cif.'
_cod_database_code               4084077