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_7109390
_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            'C52 H49 B2 Cl F8 N4 P2 Pd'
_chemical_formula_weight         1107.36
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 92.807(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8013(7)
_cell_length_b                   9.4307(6)
_cell_length_c                   44.208(3)
_cell_measurement_reflns_used    8826
_cell_measurement_temperature    103.1500
_cell_measurement_theta_max      25.3476
_cell_measurement_theta_min      3.0552
_cell_volume                     4914.2(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Saturn70 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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            50454
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.8947
_exptl_absorpt_correction_T_min  0.8947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         8608
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+8.6869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                8159
_reflns_number_total             8608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc42655f.cif
_cod_data_source_block           mono
_cod_original_cell_volume        4914.3(5)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7109390