#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/41/7204136.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_7204136
loop_
_publ_author_name
'Faulmann, C.'
'Doublet, M.-L.'
'Granier, F.'
'Garreau de Bonneval, B.'
'Malfant, I.'
'Legros, J.-P.'
'Togonidze, T.'
'Cassoux, P.'
_publ_section_title
;
 Synthesis, electrical behaviour, and crystal and electronic band
 structures of two different phases of the (SMeEt2)[Pd(dmit)2]2 salt.
 Consequences of cationic disorder on the electrical properties
;
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2205
_journal_paper_doi               10.1039/b102133h
_journal_volume                  11
_journal_year                    2001
_chemical_formula_moiety         'C5 H13 S, 2(C6 Pd S10)'
_chemical_formula_sum            'C17 H13 Pd2 S21'
_chemical_formula_weight         1103.58
_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                91.68(4)
_cell_angle_beta                 112.08(4)
_cell_angle_gamma                88.79(5)
_cell_formula_units_Z            2
_cell_length_a                   7.804(4)
_cell_length_b                   36.171(18)
_cell_length_c                   6.284(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      6.0
_cell_volume                     1642.9(14)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Cameron (Watkin, 1996)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.215
_diffrn_measured_fraction_theta_max 0.215
_diffrn_measurement_device_type  'CAD4 Enraf-Nonius'
_diffrn_measurement_method       'non-profiled 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  0.2488
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4698
_diffrn_reflns_theta_full        22.5
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.5116
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   4
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4305
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.164
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0791P)²+30.8852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1987
_reflns_number_gt                3071
_reflns_number_total             4305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102133h.txt
_cod_data_source_block           pd36_ta
_cod_original_cell_volume        1642.9(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204136
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.4510(11) 0.2526(2) 0.7682(12) 0.106(2) Uani 1 1 d DU . .
C1A C 0.336(5) 0.2331(11) 0.506(3) 0.078(8) Uani 0.50 1 d PDU A 1
H1A1 H 0.3891 0.2411 0.4002 0.118 Uiso 0.50 1 calc PR A 1
H1A2 H 0.2082 0.2404 0.4532 0.118 Uiso 0.50 1 calc PR A 1
H1A3 H 0.3459 0.2066 0.5168 0.118 Uiso 0.50 1 calc PR A 1
C1B C 0.441(5) 0.2081(7) 0.637(5) 0.068(8) Uani 0.50 1 d PDU A 2
H1B1 H 0.3151 0.2023 0.5449 0.103 Uiso 0.50 1 calc PR A 2
H1B2 H 0.4911 0.1900 0.7535 0.103 Uiso 0.50 1 calc PR A 2
H1B3 H 0.5126 0.2080 0.5411 0.103 Uiso 0.50 1 calc PR A 2
C2 C 0.483(4) 0.2838(9) 0.567(5) 0.130(9) Uani 1 1 d DU A .
H2A H 0.3778 0.2818 0.4224 0.156 Uiso 1 1 calc R B 1
H2B H 0.4854 0.3090 0.6256 0.156 Uiso 1 1 calc R B 1
C3A C 0.659(9) 0.276(2) 0.525(17) 0.13(2) Uani 0.50 1 d PDU A 1
H3A1 H 0.7624 0.2854 0.6519 0.190 Uiso 0.50 1 calc PR A 1
H3A2 H 0.6513 0.2877 0.3865 0.190 Uiso 0.50 1 calc PR A 1
H3A3 H 0.6737 0.2497 0.5087 0.190 Uiso 0.50 1 calc PR A 1
C3B C 0.611(12) 0.262(2) 0.48(2) 0.16(2) Uani 0.50 1 d PDU A 2
H3B1 H 0.6244 0.2370 0.5351 0.236 Uiso 0.50 1 calc PR A 2
H3B2 H 0.7300 0.2733 0.5330 0.236 Uiso 0.50 1 calc PR A 2
H3B3 H 0.5604 0.2611 0.3145 0.236 Uiso 0.50 1 calc PR A 2
C4 C 0.211(4) 0.2618(8) 0.727(4) 0.112(8) Uani 1 1 d DU A .
H4A H 0.1851 0.2881 0.7321 0.135 Uiso 1 1 calc R C 1
H4B H 0.1265 0.2511 0.5835 0.135 Uiso 1 1 calc R C 1
C5A C 0.202(11) 0.2427(19) 0.930(9) 0.121(18) Uani 0.50 1 d PDU A 1
H5A1 H 0.1138 0.2230 0.8789 0.182 Uiso 0.50 1 calc PR A 1
H5A2 H 0.1637 0.2601 1.0230 0.182 Uiso 0.50 1 calc PR A 1
H5A3 H 0.3213 0.2328 1.0198 0.182 Uiso 0.50 1 calc PR A 1
C5B C 0.135(9) 0.2319(18) 0.825(9) 0.107(17) Uani 0.50 1 d PDU A 2
H5B1 H 0.2352 0.2186 0.9357 0.160 Uiso 0.50 1 calc PR A 2
H5B2 H 0.0635 0.2152 0.7041 0.160 Uiso 0.50 1 calc PR A 2
H5B3 H 0.0575 0.2427 0.8988 0.160 Uiso 0.50 1 calc PR A 2
Pd1 Pd 0.18800(15) 0.48157(3) 1.01782(18) 0.0310(3) Uani 1 1 d . . .
S11 S 0.0370(6) 0.43437(10) 0.7701(6) 0.0368(9) Uani 1 1 d . . .
S12 S 0.1981(6) 0.44737(10) 1.3228(6) 0.0372(9) Uani 1 1 d . . .
S13 S -0.0659(6) 0.35916(11) 0.8588(7) 0.0451(10) Uani 1 1 d . . .
S14 S 0.0787(6) 0.37004(11) 1.3484(7) 0.0447(10) Uani 1 1 d . . .
S15 S -0.0893(8) 0.29828(13) 1.1517(9) 0.0688(14) Uani 1 1 d . . .
S16 S 0.3559(6) 0.52614(10) 1.2691(6) 0.0384(9) Uani 1 1 d . . .
S17 S 0.1974(6) 0.51506(10) 0.7178(6) 0.0379(9) Uani 1 1 d . . .
S18 S 0.5042(6) 0.59777(11) 1.1968(7) 0.0425(10) Uani 1 1 d . . .
S19 S 0.3638(6) 0.58794(11) 0.7048(7) 0.0422(10) Uani 1 1 d . . .
S20 S 0.5617(7) 0.65656(12) 0.9137(9) 0.0595(12) Uani 1 1 d . . .
C11 C 0.0279(18) 0.4024(4) 0.957(3) 0.033(3) Uani 1 1 d . . .
C12 C 0.100(2) 0.4075(4) 1.194(2) 0.033(3) Uani 1 1 d . . .
C13 C -0.030(3) 0.3396(4) 1.123(3) 0.050(4) Uani 1 1 d . . .
C14 C 0.3823(19) 0.5565(4) 1.092(3) 0.035(4) Uani 1 1 d . . .
C15 C 0.316(2) 0.5530(4) 0.858(2) 0.035(4) Uani 1 1 d . . .
C16 C 0.481(2) 0.6171(4) 0.940(3) 0.038(4) Uani 1 1 d . . .
Pd2 Pd 0.18507(15) 0.01893(3) 1.02142(18) 0.0309(3) Uani 1 1 d . . .
S21 S 0.1970(5) -0.01440(10) 0.7116(6) 0.0370(9) Uani 1 1 d . . .
S22 S 0.3587(5) -0.02574(10) 1.2604(6) 0.0382(9) Uani 1 1 d . . .
S23 S 0.3729(6) -0.08723(11) 0.6780(7) 0.0419(10) Uani 1 1 d . . .
S24 S 0.5151(6) -0.09717(11) 1.1667(7) 0.0409(10) Uani 1 1 d . . .
S25 S 0.5770(7) -0.15608(12) 0.8651(9) 0.0592(13) Uani 1 1 d . . .
S26 S 0.1909(5) 0.05337(10) 1.3351(6) 0.0369(9) Uani 1 1 d . . .
S27 S 0.0295(6) 0.06601(10) 0.7861(6) 0.0384(9) Uani 1 1 d . . .
S28 S 0.0602(6) 0.13061(11) 1.3803(7) 0.0472(11) Uani 1 1 d . . .
S29 S -0.0848(6) 0.14117(11) 0.8923(7) 0.0488(11) Uani 1 1 d . . .
S30 S -0.1167(8) 0.20230(13) 1.2012(10) 0.0767(16) Uani 1 1 d . . .
C21 C 0.325(2) -0.0517(4) 0.844(2) 0.033(3) Uani 1 1 d . . .
C22 C 0.3879(17) -0.0567(4) 1.071(2) 0.031(3) Uani 1 1 d . . .
C23 C 0.489(2) -0.1159(4) 0.902(3) 0.042(4) Uani 1 1 d . . .
C24 C 0.0813(18) 0.0929(4) 1.212(2) 0.032(3) Uani 1 1 d . . .
C25 C 0.0169(19) 0.0981(4) 0.983(2) 0.035(4) Uani 1 1 d . . .
C26 C -0.055(2) 0.1602(4) 1.158(3) 0.048(4) Uani 1 1 d . . .
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'
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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1A S1 C1B 43.6(17) . . ?
C1A S1 C2 75.0(15) . . ?
C1B S1 C2 104.3(15) . . ?
C1A S1 C4 77.7(16) . . ?
C1B S1 C4 102.7(15) . . ?
C2 S1 C4 101.4(13) . . ?
C3B C2 C3A 24(6) . . ?
C3B C2 S1 102(5) . . ?
C3A C2 S1 113(4) . . ?
C5A C4 C5B 30(3) . . ?
C5A C4 S1 100(4) . . ?
C5B C4 S1 111(3) . . ?
S16 Pd1 S12 89.12(14) . . ?
S16 Pd1 S17 89.73(14) . . ?
S12 Pd1 S17 176.37(16) . . ?
S16 Pd1 S11 176.11(15) . . ?
S12 Pd1 S11 90.01(14) . . ?
S17 Pd1 S11 90.91(14) . . ?
S16 Pd1 Pd1 92.50(12) . 2_567 ?
S12 Pd1 Pd1 91.55(12) . 2_567 ?
S17 Pd1 Pd1 91.94(12) . 2_567 ?
S11 Pd1 Pd1 91.31(12) . 2_567 ?
C11 S11 Pd1 101.0(5) . . ?
C12 S12 Pd1 102.3(5) . . ?
C11 S13 C13 98.7(8) . . ?
C13 S14 C12 99.4(8) . . ?
C14 S16 Pd1 101.4(6) . . ?
C15 S17 Pd1 101.5(5) . . ?
C16 S18 C14 99.3(7) . . ?
C15 S19 C16 97.3(7) . . ?
C12 C11 S11 124.0(11) . . ?
C12 C11 S13 115.4(11) . . ?
S11 C11 S13 120.5(9) . . ?
C11 C12 S12 122.5(10) . . ?
C11 C12 S14 115.0(11) . . ?
S12 C12 S14 122.5(8) . . ?
S15 C13 S14 124.6(10) . . ?
S15 C13 S13 123.9(10) . . ?
S14 C13 S13 111.5(9) . . ?
C15 C14 S16 125.6(12) . . ?
C15 C14 S18 113.4(11) . . ?
S16 C14 S18 121.0(9) . . ?
C14 C15 S17 121.8(11) . . ?
C14 C15 S19 117.9(12) . . ?
S17 C15 S19 120.3(8) . . ?
S20 C16 S18 125.1(10) . . ?
S20 C16 S19 122.9(9) . . ?
S18 C16 S19 111.9(8) . . ?
S22 Pd2 S26 89.42(14) . . ?
S22 Pd2 S21 89.87(14) . . ?
S26 Pd2 S21 176.55(15) . . ?
S22 Pd2 S27 175.97(16) . . ?
S26 Pd2 S27 89.98(14) . . ?
S21 Pd2 S27 90.49(13) . . ?
S22 Pd2 Pd2 91.84(12) . 2_557 ?
S26 Pd2 Pd2 91.68(12) . 2_557 ?
S21 Pd2 Pd2 91.71(12) . 2_557 ?
S27 Pd2 Pd2 92.16(12) . 2_557 ?
C21 S21 Pd2 100.7(5) . . ?
C22 S22 Pd2 101.4(5) . . ?
C23 S23 C21 96.7(7) . . ?
C23 S24 C22 97.5(7) . . ?
C24 S26 Pd2 101.8(5) . . ?
C25 S27 Pd2 100.9(5) . . ?
C26 S28 C24 97.5(7) . . ?
C26 S29 C25 98.0(7) . . ?
C22 C21 S21 124.0(10) . . ?
C22 C21 S23 116.5(10) . . ?
S21 C21 S23 119.4(8) . . ?
C21 C22 S22 123.9(11) . . ?
C21 C22 S24 115.7(10) . . ?
S22 C22 S24 120.4(8) . . ?
S25 C23 S24 123.6(9) . . ?
S25 C23 S23 122.9(9) . . ?
S24 C23 S23 113.4(8) . . ?
C25 C24 S26 122.8(11) . . ?
C25 C24 S28 116.1(11) . . ?
S26 C24 S28 120.9(9) . . ?
C24 C25 S27 124.5(11) . . ?
C24 C25 S29 115.7(11) . . ?
S27 C25 S29 119.8(8) . . ?
S30 C26 S29 124.3(11) . . ?
S30 C26 S28 123.0(11) . . ?
S29 C26 S28 112.6(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1A 1.692(19) . ?
S1 C1B 1.777(18) . ?
S1 C2 1.81(3) . ?
S1 C4 1.82(3) . ?
C2 C3B 1.52(2) . ?
C2 C3A 1.51(2) . ?
C4 C5A 1.50(2) . ?
C4 C5B 1.50(2) . ?
Pd1 S16 2.279(4) . ?
Pd1 S12 2.287(4) . ?
Pd1 S17 2.295(4) . ?
Pd1 S11 2.297(4) . ?
Pd1 Pd1 3.130(3) 2_567 ?
S11 C11 1.694(15) . ?
S12 C12 1.681(15) . ?
S13 C11 1.736(14) . ?
S13 C13 1.747(16) . ?
S14 C13 1.724(17) . ?
S14 C12 1.736(13) . ?
S15 C13 1.610(17) . ?
S16 C14 1.659(15) . ?
S17 C15 1.697(16) . ?
S18 C16 1.724(15) . ?
S18 C14 1.760(15) . ?
S19 C15 1.738(14) . ?
S19 C16 1.751(16) . ?
S20 C16 1.609(15) . ?
C11 C12 1.39(2) . ?
C14 C15 1.37(2) . ?
Pd2 S22 2.285(4) . ?
Pd2 S26 2.287(4) . ?
Pd2 S21 2.290(4) . ?
Pd2 S27 2.296(4) . ?
Pd2 Pd2 3.139(3) 2_557 ?
S21 C21 1.701(13) . ?
S22 C22 1.684(14) . ?
S23 C23 1.722(15) . ?
S23 C21 1.754(12) . ?
S24 C23 1.721(15) . ?
S24 C22 1.740(14) . ?
S25 C23 1.640(15) . ?
S26 C24 1.701(14) . ?
S27 C25 1.700(15) . ?
S28 C26 1.733(17) . ?
S28 C24 1.742(14) . ?
S29 C26 1.723(18) . ?
S29 C25 1.743(14) . ?
S30 C26 1.633(16) . ?
C21 C22 1.340(19) . ?
C24 C25 1.35(2) . ?
