Cationic Dinuclear Pd−Allyl−Halide Complexes with N-Heterocyclic Carbenes
Ding, Yuqiang; Goddard, Richard; Pörschke, Klaus-Richard; Organometallics 24 (2005) 439–; doi:10.1021/om049317o

data_4075758
_publ_section_title
;
 Cationic Dinuclear Pd&#x2212;Allyl&#x2212;Halide Complexes with
 N-Heterocyclic Carbenes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              439
_journal_paper_doi               10.1021/om049317o
_journal_volume                  24
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_compound_source        diethylether/dichloromethane
_chemical_formula_moiety
'2(C28 H50 Cl N4 Pd2 1+), 2(P F6 1-), C4 H10 O, C H2 Cl2'
_chemical_formula_sum            'C61 H112 Cl4 F12 N8 O P2 Pd4'
_chemical_formula_weight         1830.93
_chemical_melting_point          293
_chemical_name_systematic
; 
(\m~2~-chloro)-bis[(\h^3^-allyl)-(1,3-tert-butyl-imidazol-
 2-ylidene)-palladium] hexafluorophosphate 
 demi-diethylether demi-dichloromethane solvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.7460(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7790(1)
_cell_length_b                   16.7882(1)
_cell_length_c                   19.3921(1)
_cell_measurement_reflns_used    126025
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      2.91
_cell_volume                     3834.43(4)
_computing_cell_refinement       'Denzo / Scalepack (Otwinowski 1997)'
_computing_data_collection       'Collect software (Nonius, 1998)'
_computing_data_reduction        'Denzo / Scalepack (Otwinowski 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD \w-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.3 mm focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            87312
_diffrn_reflns_theta_full        31.49
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.93686
_exptl_absorpt_correction_T_min  0.78976
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XPREP, Siemens (1995)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         23159
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0409P)^2^+4.0849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                22074
_reflns_number_total             23159
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om049317osi20040901_093929.cif
_cod_data_source_block           3a.0.5(C4H10O).0.5(CH2Cl2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4075758