Methyl Levamisolium Triflate as a Precursor to a Chiral Bifunctional N-Heterocyclic Carbene-Thiolate Ligand: Palladium(II) Complexes†
Cabeza, Javier A.; del Río, Ignacio; Sánchez-Vega, M. Gabriela; Suárez, Marta; Organometallics 25 (2006) 1831–; doi:10.1021/om060042h

data_4089347
_publ_section_title
;
 Methyl Levamisolium Triflate as a Precursor to a Chiral Bifunctional
 N-Heterocyclic Carbene-Thiolate Ligand:&#x00A0; Palladium(II)
 Complexes&#x2020;
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1831
_journal_paper_doi               10.1021/om060042h
_journal_volume                  25
_journal_year                    2006
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C60 H60 N4 P2 Pd2 S2, 2(B F4)'
_chemical_formula_sum            'C60 H60 B2 F8 N4 P2 Pd2 S2'
_chemical_formula_weight         1349.69
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_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                81.075(4)
_cell_angle_beta                 88.287(5)
_cell_angle_gamma                63.849(4)
_cell_formula_units_Z            2
_cell_length_a                   13.3185(9)
_cell_length_b                   13.5907(11)
_cell_length_c                   20.5690(19)
_cell_measurement_temperature    200(2)
_cell_volume                     3298.5(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20312
_diffrn_reflns_theta_full        68.72
_diffrn_reflns_theta_max         68.72
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    5.960
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'off white'
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.022
_refine_diff_density_min         -1.565
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.039(15)
_refine_ls_extinction_coef       0.0080(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1442
_refine_ls_number_reflns         20312
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.1281
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
  [1.00000+-1.00000exp(-2.50(sin\q/\l)^2^)]/
    [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.2000P)^2^+0.0000sin\q/\l]
  where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3591
_refine_ls_wR_factor_ref         0.4123
_reflns_number_gt                17608
_reflns_number_total             20312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060042hsi20060116_074422.cif
_cod_data_source_block           m46
_cod_database_code               4089347