[PdS2C2(COOMe)2]6n (n = 0, -1, -2, -3, -4): Hexanuclear Homoleptic Palladium Dithiolene Complexes
Colin L. Beswick; Raquel Terroba; Mark A. Greaney; Edward I. Stiefel; Journal of the American Chemical Society 124 (2002) 9664–9665; doi:10.1021/ja026079k

data_4115048
_publ_contact_author
;
  Edward I. Stiefel
  101 Hoyt Laboratory
  Department of Chemistry
  Princeton, NJ 08544
;
_publ_contact_author_email       estiefel@princeton.edu
_publ_contact_author_fax         '609 258 6746'
_publ_contact_author_phone       '609 258 2065'
_publ_section_title
;
 [PdS2C2(COOMe)2]6n (n = 0, -1, -2, -3, -4): Hexanuclear Homoleptic
 Palladium Dithiolene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9664
_journal_page_last               9665
_journal_paper_doi               10.1021/ja026079k
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C57 H60 O24 Pd6 S12'
_chemical_formula_weight         2152.17
_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                105.8390(10)
_cell_angle_beta                 109.0640(10)
_cell_angle_gamma                106.8990(10)
_cell_formula_units_Z            1
_cell_length_a                   12.4637(6)
_cell_length_b                   12.6975(6)
_cell_length_c                   14.6816(7)
_cell_measurement_temperature    233(2)
_cell_volume                     1919.50(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13371
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.772
_exptl_absorpt_correction_T_max  0.8427
_exptl_absorpt_correction_T_min  0.7182
_exptl_absorpt_correction_type   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_F_000             1062
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00075(9)
_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   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8302
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.276
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.0880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                7165
_reflns_number_total             8302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026079k_s1.cif
_cod_data_source_block           1_pds10
_cod_database_code               4115048