#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/84/1508468.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_1508468
loop_
_publ_author_name
'Kato, Reizo'
'Hengbo, Cui'
_publ_section_title
;
 Cation Dependence of Crystal Structure and Band Parameters in a Series of
 Molecular Conductors, beta'-(Cation)[Pd(dmit)2]2 (dmit =
 1,3-dithiole-2-thione-4,5-dithiolate)
;
_journal_issue                   3
_journal_name_full               Crystals
_journal_page_first              861
_journal_page_last               874
_journal_paper_doi               10.3390/cryst2030861
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         '(C6 H16 Sb), 2(C3 Pd S10)'
_chemical_formula_sum            'C18 H16 Pd2 S20 Sb'
_chemical_formula_weight         1208.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 97.577(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.628(4)
_cell_length_b                   6.4235(15)
_cell_length_c                   37.577(9)
_cell_measurement_reflns_used    3451
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3500.0(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            11993
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.994
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.589
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0337P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                3119
_reflns_number_total             3854
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file
C18H16Pd2S20Sb_C2_c_Et2Me2SbPddmit22_crystals-02-00861-s001_DC203.cif
_cod_data_source_block           783_Et2Me2Sb_110429_chateigner_1508469
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1508468
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Pd1 Pd 0.84904(2) 0.18273(4) 0.517171(8) 0.02500(11) Uani 1 1 d .
S1 S 0.86215(8) 0.48773(16) 0.54951(3) 0.0306(3) Uani 1 1 d .
S2 S 0.79043(8) 0.01672(16) 0.56381(3) 0.0316(3) Uani 1 1 d .
S3 S 0.91713(8) 0.34832(17) 0.47345(3) 0.0322(3) Uani 1 1 d .
S4 S 0.84673(8) -0.12372(16) 0.48518(3) 0.0319(3) Uani 1 1 d .
S5 S 0.82691(9) 0.58411(17) 0.62450(3) 0.0369(3) Uani 1 1 d .
S6 S 0.76152(8) 0.17026(18) 0.63681(3) 0.0381(3) Uani 1 1 d .
S7 S 0.97214(8) 0.19800(18) 0.40427(3) 0.0364(3) Uani 1 1 d .
S8 S 0.91163(9) -0.22387(17) 0.41455(3) 0.0378(3) Uani 1 1 d .
S9 S 0.77033(11) 0.4851(2) 0.69536(4) 0.0591(4) Uani 1 1 d .
S10 S 0.99054(10) -0.1178(2) 0.34809(4) 0.0524(4) Uani 1 1 d .
C1 C 0.8260(3) 0.4108(6) 0.58871(11) 0.0267(9) Uani 1 1 d .
C2 C 0.7952(3) 0.2131(6) 0.59445(12) 0.0288(10) Uani 1 1 d .
C3 C 0.9243(3) 0.1527(6) 0.44364(11) 0.0260(9) Uani 1 1 d .
C4 C 0.8945(3) -0.0475(6) 0.44861(11) 0.0274(9) Uani 1 1 d .
C5 C 0.7851(3) 0.4154(7) 0.65441(13) 0.0364(11) Uani 1 1 d .
C6 C 0.9593(3) -0.0500(7) 0.38670(12) 0.0323(10) Uani 1 1 d .
Sb1 Sb 1.0000 0.78021(7) 0.7500 0.05196(17) Uani 1 2 d S
C7 C 0.8879(4) 0.9726(8) 0.73179(17) 0.0689(18) Uani 1 1 d .
H7A H 0.8709 1.0520 0.7515 0.083 Uiso 1 1 calc R
H7B H 0.8367 0.8885 0.7218 0.083 Uiso 1 1 calc R
H7C H 0.9049 1.0655 0.7138 0.083 Uiso 1 1 calc R
C8 C 1.0342(5) 0.5980(11) 0.7067(2) 0.104(3) Uani 1 1 d .
H8A H 0.9903 0.4845 0.7029 0.125 Uiso 1 1 calc R
H8B H 1.0261 0.6835 0.6853 0.125 Uiso 1 1 calc R
C9 C 1.1237(4) 0.5127(11) 0.71040(18) 0.084(2) Uani 1 1 d .
H9A H 1.1683 0.6220 0.7155 0.101 Uiso 1 1 calc R
H9B H 1.1333 0.4443 0.6885 0.101 Uiso 1 1 calc R
H9C H 1.1305 0.4138 0.7297 0.101 Uiso 1 1 calc R
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'
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
S3 Pd1 S1 88.26(4) . .
S3 Pd1 S4 90.02(4) . .
S1 Pd1 S4 176.09(4) . .
S3 Pd1 S2 175.92(4) . .
S1 Pd1 S2 90.33(4) . .
S4 Pd1 S2 91.15(4) . .
S3 Pd1 Pd1 92.43(4) . 7_656
S1 Pd1 Pd1 89.47(3) . 7_656
S4 Pd1 Pd1 94.11(3) . 7_656
S2 Pd1 Pd1 91.39(3) . 7_656
C1 S1 Pd1 101.32(14) . .
C2 S2 Pd1 100.66(15) . .
C3 S3 Pd1 101.56(15) . .
C4 S4 Pd1 101.35(14) . .
C5 S5 C1 97.7(2) . .
C5 S6 C2 98.0(2) . .
C6 S7 C3 97.8(2) . .
C6 S8 C4 97.6(2) . .
C2 C1 S1 123.3(3) . .
C2 C1 S5 116.0(3) . .
S1 C1 S5 120.7(2) . .
C1 C2 S2 124.3(3) . .
C1 C2 S6 115.2(3) . .
S2 C2 S6 120.5(2) . .
C4 C3 S3 123.6(3) . .
C4 C3 S7 116.1(3) . .
S3 C3 S7 120.3(2) . .
C3 C4 S4 123.5(3) . .
C3 C4 S8 115.2(3) . .
S4 C4 S8 121.3(2) . .
S9 C5 S6 124.3(3) . .
S9 C5 S5 122.6(3) . .
S6 C5 S5 113.1(3) . .
S10 C6 S7 123.8(3) . .
S10 C6 S8 123.0(3) . .
S7 C6 S8 113.2(2) . .
C7 Sb1 C7 107.7(3) . 2_756
C7 Sb1 C8 109.2(3) . .
C7 Sb1 C8 108.9(3) 2_756 .
C7 Sb1 C8 108.9(3) . 2_756
C7 Sb1 C8 109.2(3) 2_756 2_756
C8 Sb1 C8 112.8(5) . 2_756
Sb1 C7 H7A 109.5 . .
Sb1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Sb1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 Sb1 116.8(5) . .
C9 C8 H8A 108.1 . .
Sb1 C8 H8A 108.1 . .
C9 C8 H8B 108.1 . .
Sb1 C8 H8B 108.1 . .
H8A C8 H8B 107.3 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 S3 2.2923(12) .
Pd1 S1 2.3002(11) .
Pd1 S4 2.3044(11) .
Pd1 S2 2.3109(12) .
Pd1 Pd1 3.1339(9) 7_656
S1 C1 1.702(4) .
S2 C2 1.703(4) .
S3 C3 1.696(4) .
S4 C4 1.694(4) .
S5 C5 1.730(5) .
S5 C1 1.744(4) .
S6 C5 1.725(5) .
S6 C2 1.749(4) .
S7 C6 1.725(4) .
S7 C3 1.742(4) .
S8 C6 1.738(5) .
S8 C4 1.752(4) .
S9 C5 1.644(5) .
S10 C6 1.636(4) .
C1 C2 1.375(5) .
C3 C4 1.379(5) .
Sb1 C7 2.094(5) .
Sb1 C7 2.094(5) 2_756
Sb1 C8 2.116(6) .
Sb1 C8 2.116(6) 2_756
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.409(7) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
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_1
S3 Pd1 S1 C1 -173.90(15) .
S4 Pd1 S1 C1 -110.0(6) .
S2 Pd1 S1 C1 2.27(15) .
Pd1 Pd1 S1 C1 93.65(15) 7_656
S3 Pd1 S2 C2 67.9(6) .
S1 Pd1 S2 C2 -1.84(15) .
S4 Pd1 S2 C2 174.54(15) .
Pd1 Pd1 S2 C2 -91.32(15) 7_656
S1 Pd1 S3 C3 177.19(15) .
S4 Pd1 S3 C3 0.70(15) .
S2 Pd1 S3 C3 107.3(5) .
Pd1 Pd1 S3 C3 -93.41(14) 7_656
S3 Pd1 S4 C4 -0.68(15) .
S1 Pd1 S4 C4 -64.6(6) .
S2 Pd1 S4 C4 -176.77(15) .
Pd1 Pd1 S4 C4 91.76(15) 7_656
Pd1 S1 C1 C2 -2.5(4) .
Pd1 S1 C1 S5 177.2(2) .
C5 S5 C1 C2 0.2(4) .
C5 S5 C1 S1 -179.5(3) .
S1 C1 C2 S2 1.2(6) .
S5 C1 C2 S2 -178.6(2) .
S1 C1 C2 S6 -179.9(2) .
S5 C1 C2 S6 0.3(5) .
Pd1 S2 C2 C1 1.0(4) .
Pd1 S2 C2 S6 -177.9(2) .
C5 S6 C2 C1 -0.7(4) .
C5 S6 C2 S2 178.3(3) .
Pd1 S3 C3 C4 -0.6(4) .
Pd1 S3 C3 S7 179.9(2) .
C6 S7 C3 C4 0.6(4) .
C6 S7 C3 S3 -179.9(3) .
S3 C3 C4 S4 0.0(6) .
S7 C3 C4 S4 179.6(2) .
S3 C3 C4 S8 -178.6(2) .
S7 C3 C4 S8 1.0(5) .
Pd1 S4 C4 C3 0.6(4) .
Pd1 S4 C4 S8 179.1(2) .
C6 S8 C4 C3 -2.0(4) .
C6 S8 C4 S4 179.4(3) .
C2 S6 C5 S9 -179.0(3) .
C2 S6 C5 S5 0.8(3) .
C1 S5 C5 S9 179.1(3) .
C1 S5 C5 S6 -0.7(3) .
C3 S7 C6 S10 179.3(3) .
C3 S7 C6 S8 -1.9(3) .
C4 S8 C6 S10 -178.8(3) .
C4 S8 C6 S7 2.3(3) .
C7 Sb1 C8 C9 159.6(6) .
C7 Sb1 C8 C9 42.2(7) 2_756
C8 Sb1 C8 C9 -79.2(6) 2_756
