#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/41/7204137.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_7204137
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                92.112(11)
_cell_angle_beta                 112.169(12)
_cell_angle_gamma                88.740(12)
_cell_formula_units_Z            2
_cell_length_a                   7.7888(9)
_cell_length_b                   36.181(3)
_cell_length_c                   6.2573(6)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      21.0
_cell_measurement_theta_min      2.8
_cell_volume                     1631.8(3)
_computing_cell_refinement       'IPDS software (Stoe, 1996)'
_computing_data_collection       'IPDS software (Stoe, 1996)'
_computing_data_reduction        'IPDS software (Stoe, 1996)'
_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      160(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'STOE Imaging Plate Diffraction System'
_diffrn_measurement_method       'φ scan '
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9065
_diffrn_reflns_theta_full        21.03
_diffrn_reflns_theta_max         21.03
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.463
_exptl_absorpt_correction_T_max  0.5464
_exptl_absorpt_correction_T_min  0.2078
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.757
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         3336
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0262P)²+81.7913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.2292
_reflns_number_gt                2890
_reflns_number_total             3336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102133h.txt
_cod_data_source_block           pd36_bt
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204137
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 0.4437(12) 0.2531(3) 0.7689(15) 0.091(2) Uani 1 1 d U . .
C1 C 0.433(6) 0.2097(11) 0.633(7) 0.132(14) Uani 1 1 d U . .
H1A H 0.3994 0.1911 0.7204 0.197 Uiso 1 1 calc R . .
H1B H 0.5542 0.2034 0.6275 0.197 Uiso 1 1 calc R . .
H1C H 0.3394 0.2102 0.4760 0.197 Uiso 1 1 calc R . .
C2 C 0.472(5) 0.2843(12) 0.558(6) 0.114(10) Uani 1 1 d U . .
H2A H 0.3594 0.2838 0.4141 0.137 Uiso 1 1 calc R . .
H2B H 0.4896 0.3100 0.6218 0.137 Uiso 1 1 calc R . .
C3 C 0.639(5) 0.2717(12) 0.505(6) 0.123(13) Uani 1 1 d U . .
H3A H 0.7371 0.2634 0.6473 0.184 Uiso 1 1 calc R . .
H3B H 0.6846 0.2924 0.4449 0.184 Uiso 1 1 calc R . .
H3C H 0.6039 0.2513 0.3903 0.184 Uiso 1 1 calc R . .
C4 C 0.208(4) 0.2623(10) 0.728(6) 0.096(8) Uani 1 1 d U . .
H4A H 0.1940 0.2883 0.7749 0.115 Uiso 1 1 calc R . .
H4B H 0.1282 0.2587 0.5625 0.115 Uiso 1 1 calc R . .
C5 C 0.150(5) 0.2360(11) 0.873(6) 0.110(11) Uani 1 1 d U . .
H5A H 0.2535 0.2191 0.9507 0.165 Uiso 1 1 calc R . .
H5B H 0.0429 0.2217 0.7729 0.165 Uiso 1 1 calc R . .
H5C H 0.1180 0.2502 0.9888 0.165 Uiso 1 1 calc R . .
Pd1 Pd 0.1882(2) 0.48155(5) 1.0166(3) 0.0474(6) Uani 1 1 d . . .
S11 S 0.0361(8) 0.43429(17) 0.7638(10) 0.0492(15) Uani 1 1 d . . .
S12 S 0.1991(8) 0.44738(17) 1.3227(10) 0.0493(15) Uani 1 1 d . . .
S13 S -0.0697(9) 0.35876(18) 0.8493(11) 0.0556(16) Uani 1 1 d . . .
S14 S 0.0774(9) 0.36966(18) 1.3461(11) 0.0575(17) Uani 1 1 d . . .
S15 S -0.0942(10) 0.2980(2) 1.1453(12) 0.070(2) Uani 1 1 d . . .
S16 S 0.3583(9) 0.52657(18) 1.2734(10) 0.0515(15) Uani 1 1 d . . .
S17 S 0.1977(8) 0.51461(17) 0.7164(10) 0.0488(15) Uani 1 1 d . . .
S18 S 0.5077(9) 0.59822(18) 1.2049(10) 0.0543(16) Uani 1 1 d . . .
S19 S 0.3661(9) 0.58830(18) 0.7070(11) 0.0539(16) Uani 1 1 d . . .
S20 S 0.5637(10) 0.65747(19) 0.9209(12) 0.0649(18) Uani 1 1 d . . .
C11 C 0.030(3) 0.4007(6) 0.955(4) 0.038(5) Uani 1 1 d . . .
C12 C 0.096(3) 0.4074(6) 1.183(4) 0.049(6) Uani 1 1 d . . .
C13 C -0.030(3) 0.3398(6) 1.118(4) 0.049(6) Uani 1 1 d . . .
C14 C 0.386(3) 0.5581(6) 1.081(5) 0.053(7) Uani 1 1 d . . .
C15 C 0.315(3) 0.5535(6) 0.858(4) 0.037(5) Uani 1 1 d . . .
C16 C 0.479(3) 0.6174(7) 0.941(4) 0.053(6) Uani 1 1 d . . .
Pd2 Pd 0.1850(2) 0.01911(5) 1.0218(3) 0.0477(6) Uani 1 1 d . . .
S21 S 0.1973(8) -0.01421(17) 0.7086(10) 0.0502(15) Uani 1 1 d . . .
S22 S 0.3596(9) -0.02569(18) 1.2625(10) 0.0510(15) Uani 1 1 d . . .
S23 S 0.3748(9) -0.08752(18) 0.6712(10) 0.0528(16) Uani 1 1 d . . .
S24 S 0.5180(9) -0.09763(18) 1.1650(10) 0.0543(16) Uani 1 1 d . . .
S25 S 0.5795(10) -0.1564(2) 0.8587(12) 0.0657(18) Uani 1 1 d . . .
S26 S 0.1911(8) 0.05370(17) 1.3405(10) 0.0512(15) Uani 1 1 d . . .
S27 S 0.0286(8) 0.06611(17) 0.7857(10) 0.0501(15) Uani 1 1 d . . .
S28 S 0.0567(9) 0.13113(18) 1.3876(11) 0.0574(17) Uani 1 1 d . . .
S29 S -0.0903(9) 0.14154(18) 0.8924(11) 0.0588(17) Uani 1 1 d . . .
S30 S -0.1233(11) 0.2026(2) 1.2088(14) 0.072(2) Uani 1 1 d . . .
C21 C 0.321(3) -0.0528(6) 0.839(4) 0.043(6) Uani 1 1 d . . .
C22 C 0.391(3) -0.0578(7) 1.059(5) 0.055(6) Uani 1 1 d . . .
C23 C 0.492(3) -0.1168(7) 0.892(4) 0.058(7) Uani 1 1 d . . .
C24 C 0.083(3) 0.0937(6) 1.213(5) 0.055(7) Uani 1 1 d . . .
C25 C 0.016(3) 0.0990(6) 0.983(4) 0.043(6) Uani 1 1 d . . .
C26 C -0.054(3) 0.1613(7) 1.171(4) 0.056(6) 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
C1 S1 C4 102.9(17) . . ?
C1 S1 C2 102(2) . . ?
C4 S1 C2 100.4(17) . . ?
C3 C2 S1 109(3) . . ?
C5 C4 S1 109(2) . . ?
S17 Pd1 S12 176.1(2) . . ?
S17 Pd1 S16 90.0(2) . . ?
S12 Pd1 S16 89.0(2) . . ?
S17 Pd1 S11 90.4(2) . . ?
S12 Pd1 S11 90.4(2) . . ?
S16 Pd1 S11 176.1(2) . . ?
S17 Pd1 Pd1 92.19(18) . 2_567 ?
S12 Pd1 Pd1 91.57(17) . 2_567 ?
S16 Pd1 Pd1 92.35(18) . 2_567 ?
S11 Pd1 Pd1 91.47(17) . 2_567 ?
C11 S11 Pd1 101.3(7) . . ?
C12 S12 Pd1 100.9(9) . . ?
C11 S13 C13 96.5(11) . . ?
C13 S14 C12 97.2(12) . . ?
C14 S16 Pd1 100.4(9) . . ?
C15 S17 Pd1 101.7(7) . . ?
C14 S18 C16 94.6(12) . . ?
C16 S19 C15 97.5(11) . . ?
C12 C11 S13 118.6(17) . . ?
C12 C11 S11 121.5(17) . . ?
S13 C11 S11 119.9(12) . . ?
C11 C12 S12 125.9(18) . . ?
C11 C12 S14 114.4(17) . . ?
S12 C12 S14 119.7(15) . . ?
S15 C13 S14 123.8(14) . . ?
S15 C13 S13 122.9(13) . . ?
S14 C13 S13 113.3(13) . . ?
C15 C14 S18 120.1(18) . . ?
C15 C14 S16 123.6(18) . . ?
S18 C14 S16 116.2(16) . . ?
C14 C15 S17 124.2(17) . . ?
C14 C15 S19 114.5(17) . . ?
S17 C15 S19 121.0(12) . . ?
S20 C16 S19 123.9(15) . . ?
S20 C16 S18 123.0(14) . . ?
S19 C16 S18 113.0(14) . . ?
S21 Pd2 S22 90.1(2) . . ?
S21 Pd2 S26 176.4(2) . . ?
S22 Pd2 S26 89.2(2) . . ?
S21 Pd2 S27 90.3(2) . . ?
S22 Pd2 S27 176.1(2) . . ?
S26 Pd2 S27 90.2(2) . . ?
S21 Pd2 Pd2 91.87(18) . 2_557 ?
S22 Pd2 Pd2 91.50(18) . 2_557 ?
S26 Pd2 Pd2 91.63(17) . 2_557 ?
S27 Pd2 Pd2 92.38(17) . 2_557 ?
C21 S21 Pd2 101.2(7) . . ?
C22 S22 Pd2 100.7(9) . . ?
C23 S23 C21 97.6(12) . . ?
C22 S24 C23 95.2(13) . . ?
C24 S26 Pd2 100.8(9) . . ?
C25 S27 Pd2 101.5(8) . . ?
C26 S28 C24 98.0(13) . . ?
C25 S29 C26 97.2(12) . . ?
C22 C21 S21 125.3(17) . . ?
C22 C21 S23 114.7(19) . . ?
S21 C21 S23 119.8(13) . . ?
C21 C22 S24 119.9(19) . . ?
C21 C22 S22 123(2) . . ?
S24 C22 S22 117.4(15) . . ?
S25 C23 S23 124.9(15) . . ?
S25 C23 S24 122.8(16) . . ?
S23 C23 S24 112.3(14) . . ?
C25 C24 S26 124.3(18) . . ?
C25 C24 S28 116.1(19) . . ?
S26 C24 S28 119.6(17) . . ?
C24 C25 S27 123.2(18) . . ?
C24 C25 S29 116.6(18) . . ?
S27 C25 S29 120.3(13) . . ?
S30 C26 S28 125.2(15) . . ?
S30 C26 S29 122.6(15) . . ?
S28 C26 S29 112.1(14) . . ?
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 C1 1.74(3) . ?
S1 C4 1.78(3) . ?
S1 C2 1.85(4) . ?
C2 C3 1.52(5) . ?
C4 C5 1.53(4) . ?
Pd1 S17 2.289(6) . ?
Pd1 S12 2.291(6) . ?
Pd1 S16 2.299(6) . ?
Pd1 S11 2.303(6) . ?
Pd1 Pd1 3.132(4) 2_567 ?
S11 C11 1.75(2) . ?
S12 C12 1.71(2) . ?
S13 C11 1.71(2) . ?
S13 C13 1.75(2) . ?
S14 C13 1.71(2) . ?
S14 C12 1.77(2) . ?
S15 C13 1.64(2) . ?
S16 C14 1.76(2) . ?
S17 C15 1.72(2) . ?
S18 C14 1.74(2) . ?
S18 C16 1.75(2) . ?
S19 C16 1.72(2) . ?
S19 C15 1.74(2) . ?
S20 C16 1.63(3) . ?
C11 C12 1.34(3) . ?
C14 C15 1.30(3) . ?
Pd2 S21 2.295(6) . ?
Pd2 S22 2.299(6) . ?
Pd2 S26 2.300(6) . ?
Pd2 S27 2.301(6) . ?
Pd2 Pd2 3.138(4) 2_557 ?
S21 C21 1.72(2) . ?
S22 C22 1.77(3) . ?
S23 C23 1.73(3) . ?
S23 C21 1.75(2) . ?
S24 C22 1.73(3) . ?
S24 C23 1.76(2) . ?
S25 C23 1.61(3) . ?
S26 C24 1.72(3) . ?
S27 C25 1.71(2) . ?
S28 C26 1.72(3) . ?
S28 C24 1.76(2) . ?
S29 C25 1.74(2) . ?
S29 C26 1.78(2) . ?
S30 C26 1.62(3) . ?
C21 C22 1.30(3) . ?
C24 C25 1.35(3) . ?
