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_4328132
_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 Pd S6, 6(Cl O4), 3(H5 O2)'
_chemical_formula_sum            'C12 H39 Cl6 O30 Pd S6'
_chemical_formula_weight         1174.89
_chemical_name_common            Pd(III)[18]aneS6
_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                 99.840(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9805(2)
_cell_length_b                   10.62075(17)
_cell_length_c                   18.2038(4)
_cell_measurement_reflns_used    10386
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      73.79
_cell_measurement_theta_min      4.15
_cell_volume                     1901.22(7)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    ' ? '
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'SuperNova, single source, Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12654
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.09
_diffrn_reflns_theta_min         4.50
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.854
_exptl_absorpt_correction_T_max  0.259
_exptl_absorpt_correction_T_min  0.053
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_description       block
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.4283
_exptl_crystal_size_mid          0.3341
_exptl_crystal_size_min          0.2299
_refine_diff_density_max         1.19
_refine_diff_density_min         -1.80
_refine_diff_density_rms         0.12
_refine_ls_extinction_coef       0.00217(12)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3791
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0561P)^2^+2.5219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                3711
_reflns_number_total             3791
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2017006_si_002_4.cif
_cod_data_source_block           '[Pd([18]aneS6)]3+'
_cod_original_cell_volume        1901.22(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328132