Pyridine-based dicarbene ligand; synthesis and structure of a bis-2-pyridylidene palladium complex
Tetsushi Yoshidomi; Yasutomo Segawa; Kenichiro Itami; Chem.Commun. 49 (2013) 5648–; doi:10.1039/c3cc42655f

data_7109389
_publ_section_title
;
 Pyridine-based dicarbene ligand; synthesis and structure of a
 bis-2-pyridylidene palladium complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              5648
_journal_paper_doi               10.1039/c3cc42655f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C26 H24 B F4 N4 Na O6 Pd2'
_chemical_formula_weight         811.09
_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                89.999(13)
_cell_angle_beta                 86.530(16)
_cell_angle_gamma                86.072(14)
_cell_formula_units_Z            2
_cell_length_a                   6.894(4)
_cell_length_b                   10.276(6)
_cell_length_c                   18.762(11)
_cell_measurement_reflns_used    3307
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.3415
_cell_measurement_theta_min      3.0977
_cell_volume                     1323.6(13)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Saturn724 CCD (4x4 bin mode) with MicroMax-007
;
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18004
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  0.9856
_exptl_absorpt_correction_T_min  0.7594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.864
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         4651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0561P)^2^+3.7021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                3953
_reflns_number_total             4651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc42655f.cif
_cod_data_source_block           bi
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7109389