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_4328131
_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         'Pd C12 H24 S6, 6(Cl O4), 3(H3 O), H2O'
_chemical_formula_sum            'C12 H35 Cl6 O28 Pd S6'
_chemical_formula_weight         1138.86
_chemical_name_common            '[Pd(III)([9]aneS3)2]3+'
_chemical_name_systematic
; 
 Palladium(III) bis 1,4,7-trithiacyclononane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL-97 created file'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.787(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5602(11)
_cell_length_b                   9.1932(10)
_cell_length_c                   19.079(2)
_cell_measurement_reflns_used    3078
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_cell_volume                     1848.2(3)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4205
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1150
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4205
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0300P)^2^+3.5792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                3517
_reflns_number_total             4205
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2017006_si_002_3.cif
_cod_data_source_block           '[Pd([9]aneS3)2]3+'
_cod_original_cell_volume        1848.1(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328131