Synthesis of Palladium(II), -(III), and -(IV) Complexes with Acyclic Diaminocarbene Ligands
Mart\?ínez-Mart\?ínez, Antonio-Jesús; Chicote, María-Teresa; Bautista, Delia; Vicente, José; Organometallics 31 (2012) 3711–; doi:10.1021/om300201s

data_4078280
_publ_section_title
;
 Synthesis of Palladium(II), -(III), and -(IV) Complexes with Acyclic
 Diaminocarbene Ligands
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3711
_journal_paper_doi               10.1021/om300201s
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C24.5 H25.5 Cl3.5 N3 Pd'
_chemical_formula_weight         592.45
_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                77.926(2)
_cell_angle_beta                 87.072(2)
_cell_angle_gamma                67.016(2)
_cell_formula_units_Z            4
_cell_length_a                   12.9318(11)
_cell_length_b                   14.0685(12)
_cell_length_c                   14.8638(13)
_cell_measurement_reflns_used    5307
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.25
_cell_volume                     2433.0(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30288
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.85
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.9659
_exptl_absorpt_correction_T_min  0.8346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.032
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment
'NH free with SADI, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         11519
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0335P)^2^+3.4679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                9951
_reflns_number_total             11519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300201s_si_002.cif
_cod_data_source_block           aje64s
_cod_original_formula_sum        'C24.50 H25.50 Cl3.50 N3 Pd'
_cod_database_code               4078280