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_4078281
_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            'C47.66 H51.96 Cl0.34 F6 N5 O6.88 Pd S2'
_chemical_formula_weight         1101.67
_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                71.603(2)
_cell_angle_beta                 78.117(2)
_cell_angle_gamma                74.951(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2499(5)
_cell_length_b                   14.6931(7)
_cell_length_c                   17.9342(9)
_cell_measurement_reflns_used    5697
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.24
_cell_volume                     2452.3(2)
_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 0.984
_diffrn_measured_fraction_theta_max 0.908
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28552
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.9566
_exptl_absorpt_correction_T_min  0.8645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment
'NH free with SADIn rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10993
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0415P)^2^+1.5547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                9990
_reflns_number_total             10993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300201s_si_002.cif
_cod_data_source_block           ajd202bs
_cod_database_code               4078281