Palladium(II)-Mediated Addition of Benzenediamines to Isocyanides: Generation of Three Types of Diaminocarbene Ligands Depending on the Isomeric Structure of the Nucleophile
Kinzhalov, Mikhail A.; Timofeeva, Svetlana A.; Luzyanin, Konstantin V.; Boyarskiy, Vadim P.; Yakimanskiy, Anton A.; Haukka, Matti; Kukushkin, Vadim Yu.; Organometallics 35 (2016) 218–; doi:10.1021/acs.organomet.5b00936

data_4088217
_publ_section_title
;
 Palladium(II)-Mediated Addition of Benzenediamines to Isocyanides:
 Generation of Three Types of Diaminocarbene Ligands Depending on the
 Isomeric Structure of the Nucleophile
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              218
_journal_paper_doi               10.1021/acs.organomet.5b00936
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C24 H24 Cl4 N4 Pd, 3(C2 H3 N)'
_chemical_formula_sum            'C30 H33 Cl4 N7 Pd'
_chemical_formula_weight         739.83
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                92.557(4)
_cell_angle_beta                 96.674(4)
_cell_angle_gamma                99.141(4)
_cell_formula_units_Z            4
_cell_length_a                   11.6073(11)
_cell_length_b                   14.5694(14)
_cell_length_c                   20.3773(19)
_cell_measurement_reflns_used    9129
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.58
_cell_measurement_theta_min      2.39
_cell_volume                     3372.2(6)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics
'CrystaMaker (CrystalMaker Software ltd., 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'curved graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41573
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.9076
_exptl_absorpt_correction_T_min  0.7806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.106
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         12081
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0755
_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^)+(0.0245P)^2^+41.4871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1641
_reflns_number_gt                10058
_reflns_number_total             12081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00936_si_005.cif
_cod_data_source_block           km338c
_cod_database_code               4088217