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_4069132
_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         'C32 H44 Cl N4 Pd2, 2(C H2 Cl2), B F4''
_chemical_formula_sum            'C34 H48 B Cl5 F4 N4 Pd2'
_chemical_formula_weight         989.62
_chemical_name_common            9b
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.966(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2797(15)
_cell_length_b                   31.117(4)
_cell_length_c                   13.3146(18)
_cell_measurement_reflns_used    61588
_cell_measurement_temperature    114(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.0
_cell_volume                     4181.2(10)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      114(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9566
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  0.8872
_exptl_absorpt_correction_T_min  0.5791
_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            orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.606
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         9566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0864P)^2^+5.5525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1917
_reflns_number_gt                6650
_reflns_number_total             9566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900043u_si_001.cif
_cod_data_source_block           9b
_cod_original_cell_volume        4181.3(10)
_cod_database_code               4069132