Redox Non-innocence of Thioether Crowns: Elucidation of the Electronic Structure of the Mononuclear Pd(III) Complexes [Pd([9]aneS~3~)~2~]^3+^ and [Pd([18]aneS~6~)]^3+^
Emma Stephen; Alexander J. Blake; Emma Carter; David Collison; E. Stephen Davies; Ruth Edge; William Lewis; Damien M. Murphy; Claire Wilson; Robert O. Gould; Alan J. Holder; Jonathan McMaster; Martin Schröder; Inorganic Chemistry 51 (2012) 1450–1461; doi:10.1021/ic2017006

data_4328129
_publ_contact_author_address
;
  School of Chemistry
  The University of Nottingham
  University Park
  Nottingham  NG7 2RD
  England UK
;
_publ_contact_author_email       M.Schroder@nottingham.ac.uk
_publ_contact_author_fax         '0115 951 3563'
_publ_contact_author_name        'Martin Schr\"oder'
_publ_contact_author_phone       '0115 951 3490'
_publ_section_title
;
 Redox Non-innocence of Thioether Crowns: Elucidation of the Electronic
 Structure of the Mononuclear Pd(III) Complexes [Pd([9]aneS~3~)~2~]^3+^
 and [Pd([18]aneS~6~)]^3+^
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1450
_journal_page_last               1461
_journal_paper_doi               10.1021/ic2017006
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C12 H24 Pd1 S6 2+, 2(P F6 -)'
_chemical_formula_sum            'C12 H24 F12 P2 Pd S6'
_chemical_formula_weight         757.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELX
_cell_angle_alpha                90
_cell_angle_beta                 92.922(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.613(4)
_cell_length_b                   10.861(3)
_cell_length_c                   5.7978(12)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      21.8
_cell_measurement_theta_min      11.8
_cell_volume                     1233.4(5)
_computing_cell_refinement       'Local program'
_computing_data_collection       'Local program'
_computing_data_reduction        'Local program'
_computing_publication_material
'enCIFer (Allen et al., 2004; PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELX (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe Stadi-2 two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1256
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.5
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Local program'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.039
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.65
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         913
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo) + 0.000513F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_reflns_number_gt                913
_reflns_number_total             1137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2017006_si_002_1.cif
_cod_data_source_block           '[Pd([18]aneS6)]_2PF6'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C12 H24 F12 P2 Pd1 S6'
_cod_database_code               4328129