Synthesis and Characterization of Proximal Dinuclear Complexes of Palladium Supported by 2,6-Bis(arylimino)phenoxy (aryl = 2,6-diisopropylphenyl and 2,4,6-tri-tert-butylphenyl) and 3,6-Bis(imino(2,6-diisopropylphenyl))pyridazine Ligands
Ohno, Kouji; Arima, Kenji; Tanaka, Shinji; Yamagata, Tsuneaki; Tsurugi, Hayato; Mashima, Kazushi; Organometallics 28 (2009) 3256–; doi:10.1021/om900043u

data_4069131
_publ_section_title
;
 Synthesis and Characterization of Proximal Dinuclear Complexes of
 Palladium Supported by 2,6-Bis(arylimino)phenoxy (aryl =
 2,6-diisopropylphenyl and 2,4,6-tri-tert-butylphenyl) and
 3,6-Bis(imino(2,6-diisopropylphenyl))pyridazine Ligands
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3256
_journal_paper_doi               10.1021/om900043u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C66 H82 N4 Ni O2'
_chemical_formula_sum            'C66 H82 N4 Ni O2'
_chemical_formula_weight         1022.07
_chemical_name_common            8
_chemical_temperature_decomposition_gt 524
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.178(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7649(16)
_cell_length_b                   12.158(2)
_cell_length_c                   24.055(4)
_cell_measurement_reflns_used    27959
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.04
_cell_volume                     2833.5(8)
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_details
;
RAPID: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_collimation    ' 0.5 mm double pinhole '
_diffrn_radiation_detector       'imaging plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1373
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            56135
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_diffrn_source_current           40
_diffrn_source_power             50
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_correction_T_min  0.3890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). ABSCOR - Program for Absorption Correction, Rigaku
        Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            ' green '
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             1100
_exptl_crystal_preparation
'mounted on the CryoLoop with mineral oil and placed in N2 stream at 120(1) K'
_exptl_crystal_recrystallization_method
'slow evaporation of toluene/hexsans at ambient temperature'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+5.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                5088
_reflns_number_total             6472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900043u_si_001.cif
_cod_data_source_block           8
_cod_original_cell_volume        2833.4(9)
_cod_original_sg_symbol_Hall     ' -P 2ybc '
_cod_original_sg_symbol_H-M      ' P21/c '
_cod_database_code               4069131