Palladium(II) Complexes of Unsymmetrical CNN Pincer Ligands
Martin Bröring; Christian Kleeberg; Silke Köhler; Inorganic Chemistry 47 (2008) 6404–6412; doi:10.1021/ic800507k

data_4305508
_publ_section_title
;
Palladium(II) Complexes of Unsymmetrical CNN Pincer Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6404
_journal_page_last               6412
_journal_paper_doi               10.1021/ic800507k
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C22 H18 N4 O2 Pd1.02, 0.92 (C H Cl3)'
_chemical_formula_sum            'C22.925 H18.925 Cl2.77 N4 O2 Pd1.02'
_chemical_formula_weight         589.34
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.537(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.2418(17)
_cell_length_b                   11.5637(11)
_cell_length_c                   17.9680(12)
_cell_measurement_reflns_used    13435
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      1.98
_cell_volume                     4674.5(7)
_computing_cell_refinement       'STOE Wincell (X-Area)'
_computing_data_collection       'Stoe Expose'
_computing_data_reduction        'STOE WinIntegrate (X-Area)'
_computing_publication_material  'WinGX v1.70.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1992)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'IPDS-1 (Stoe)'
_diffrn_measurement_method       phi-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22437
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  0.8566
_exptl_absorpt_correction_T_min  0.7604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2356.4
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.794
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0668P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                3370
_reflns_number_total             4310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800507k-file003_2.cif
_cod_data_source_block           ck1skck
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4305508