#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/81/4328129.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4328129
loop_
_publ_author_name
'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'
_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 Schröder'
_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]aneS₃)₂]³⁺
 and [Pd([18]aneS₆)]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       ω
_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/[σ²(Fo) + 0.000513F²]'
_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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-x, y, -z'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0322(6) 0.0287(6) 0.0325(6) 0.0000 -0.0012(4) 0.0000
S1 0.0650(9) 0.0672(20) 0.0402(6) 0.0000 0.0111(14) 0.0000
C2 0.068(6) 0.077(7) 0.076(6) 0.000(5) 0.024(5) -0.023(5)
C3 0.058(5) 0.071(7) 0.109(9) -0.026(6) 0.004(6) -0.020(5)
S4 0.0459(11) 0.0408(11) 0.0452(11) -0.0068(8) -0.0050(9) -0.0027(8)
P1 0.0506(17) 0.0460(7) 0.0444(17) 0.0000 -0.0012(13) 0.0000
F1 0.279(17) 0.156(12) 0.060(6) 0.0000 0.015(8) 0.0000
F2 0.369(25) 0.245(19) 0.042(6) 0.0000 0.015(9) 0.0000
F3 0.174(8) 0.188(9) 0.165(9) 0.009(8) -0.006(7) -0.118(8)
F4 0.144(7) 0.153(8) 0.304(17) 0.002(10) -0.034(9) 0.083(7)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.0000 0.0000 0.0312(6) 1 4 . .
S1 S 0.13050(16) 0.0000 -0.2534(5) 0.0573(19) 1 2 . .
C2 C 0.1692(5) 0.1285(9) -0.0997(19) 0.073(6) 1 1 . .
C3 C 0.1469(4) 0.1558(9) 0.1416(21) 0.079(7) 1 1 . .
S4 S 0.05988(9) 0.15546(17) 0.2012(3) 0.0441(11) 1 1 . .
C5A C 0.0369(9) 0.2949(14) 0.030(3) 0.042(7) 0.5 1 A 2
C5B C 0.0115(12) 0.2843(19) 0.134(5) 0.072(9) 0.5 1 B 1
P1 P 0.15686(15) 0.5000 0.5622(5) 0.0471(17) 1 2 . .
F1 F 0.1565(8) 0.5000 0.2958(19) 0.165(12) 1 2 . .
F2 F 0.1550(11) 0.5000 0.8202(20) 0.219(17) 1 2 . .
F3 F 0.1046(5) 0.3969(9) 0.5376(21) 0.176(9) 1 2 . .
F4 F 0.2124(5) 0.4034(9) 0.582(3) 0.201(11) 1 1 . .
H2A H 0.1592 0.2100 -0.2028 0.0800 1 1 . .
H2B H 0.2235 0.1112 -0.0869 0.0800 1 1 . .
H3A H 0.1712 0.0881 0.2547 0.0800 1 1 . .
H3B H 0.1664 0.2462 0.1859 0.0800 1 1 . .
H5A1 H 0.0652 0.2968 -0.1259 0.0800 0.5 1 A 2
H5A2 H 0.0500 0.3768 0.1319 0.0800 0.5 1 A 2
H5B1 H 0.0416 0.3671 0.1766 0.0800 0.5 1 B 1
H5B2 H -0.0334 0.2859 0.2383 0.0800 0.5 1 B 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
S1 Pd1 S4 79.95(6) .
Pd1 S4 C5A 102.8(5) .
S4 Pd1 S4 87.36(6) 6_555
Pd1 S4 C3 111.8(4) .
Pd1 S4 C5B 102.5(8) .
Pd1 S1 C2 96.0(3) .
C3 S4 C5A 96.0(6) .
C2 S1 C2 101.5(5) .
C3 S4 C5B 118.8(9) .
S1 C2 C3 118.3(7) .
S4 C5A C5A 109.6(12) 6_555
C2 C3 S4 120.6(8) .
S4 C5B C5B 110.2(16) 6_555
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 S1 3.0154(25) .
Pd1 S4 2.3347(18) .
S1 C2 1.802(10) .
C2 C3 1.516(15) .
C3 S4 1.758(11) .
S4 C5A 1.854(17) .
S4 C5B 1.724(24) .
C5A C5A 1.473(24) 6_555
C5B C5B 1.60(3) 6_555
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
_geom_torsion_site_symmetry_3
C2 C3 S4 C5A -68.5(10) . .
C2 C3 S4 C5B -81.3(13) . .
C3 S4 C5A C5A 158.5(12) 6_555 .
C3 S4 C5B C5B 81.0(17) 6_555 .
S4 C5A C5A S4 -59.7(13) 6_555 6_555
S1 C2 C3 S4 -45.8(8) . .
S4 C5B C5B S4 60.3(19) 6_555 6_555
S1 C2 C3 S4 -45.2(11) . .
