Extension of the Alkane Bridge in BisNHC−Palladium−Chloride Complexes. Synthesis, Structure, and Catalytic Activity
Ahrens, Sebastian; Zeller, Alexander; Taige, Maria; Strassner, Thomas; Organometallics 25 (2006) 5409–; doi:10.1021/om060577a

data_4074363
_publ_section_title
;
 Extension of the Alkane Bridge in BisNHC&#x2212;Palladium&#x2212;Chloride
 Complexes. Synthesis, Structure, and Catalytic Activity
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5409
_journal_paper_doi               10.1021/om060577a
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C12 H18 Cl2 N4 Pd, C2 H6 O S'
_chemical_formula_sum            'C14 H24 Cl2 N4 O Pd S'
_chemical_formula_weight         473.76
_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                75.813(7)
_cell_angle_beta                 84.518(9)
_cell_angle_gamma                78.738(6)
_cell_formula_units_Z            2
_cell_length_a                   8.7180(8)
_cell_length_b                   9.0560(6)
_cell_length_c                   12.9660(16)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      22.094
_cell_measurement_theta_min      7.635
_cell_volume                     972.11(17)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep III 1.0.3 (Burnett,Johnson,2000)'
_computing_publication_material  'XCIF 6.12 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21422
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_correction_T_min  0.8728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2.03.(Sheldrick,Bruker AXS Inc.,2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0292P)^2^+0.9769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                3619
_reflns_number_total             3988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060577asi20060629_122036.cif
_cod_data_source_block           str-197
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074363