#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/84/1508463.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_1508463
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         '(C4 H12 P), 2(C3 Pd S10)'
_chemical_formula_sum            'C16 H12 P Pd2 S20'
_chemical_formula_weight         1089.24
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.070(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.379(3)
_cell_length_b                   6.3539(12)
_cell_length_c                   36.496(7)
_cell_measurement_reflns_used    4322
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      2.3
_cell_volume                     3301.4(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            16301
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_exptl_absorpt_coefficient_mu    2.419
_exptl_absorpt_correction_T_max  0.6434
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2140.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.10
_refine_diff_density_min         -1.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4699
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0440P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                4043
_reflns_number_total             4699
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file
C16H12PPd2S20_C2_c_Me4PPddmit22_crystals-02-00861-s001_DC198.cif
_cod_data_source_block           '__621_Me4P_110729'
_cod_original_cell_volume        3301.5(11)
_cod_original_formula_sum        'C16 H12 P Pd2 S20 '
_cod_database_code               1508463
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-Y,1/2+Z
5 1/2+X,1/2+Y,+Z
6 1/2-X,1/2+Y,1/2-Z
7 1/2-X,1/2-Y,-Z
8 1/2+X,1/2-Y,1/2+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
Pd(1) Pd 0.350898(14) 0.32730(3) 0.018721(5) 0.02356(7) Uani 1.00 1 d .
S(1) S 0.29226(5) 0.50178(11) 0.065727(19) 0.03004(15) Uani 1.00 1 d .
S(2) S 0.36469(5) 0.02375(11) 0.053625(19) 0.02860(15) Uani 1.00 1 d .
S(3) S 0.34572(6) 0.63602(11) -0.01407(2) 0.02990(15) Uani 1.00 1 d .
S(4) S 0.41886(6) 0.16295(11) -0.02703(2) 0.03037(15) Uani 1.00 1 d .
S(5) S 0.26399(6) 0.36483(14) 0.14168(2) 0.03618(17) Uani 1.00 1 d .
S(6) S 0.32671(6) -0.05947(13) 0.13134(2) 0.03637(17) Uani 1.00 1 d .
S(7) S 0.40427(6) 0.74355(12) -0.08720(2) 0.03208(16) Uani 1.00 1 d .
S(8) S 0.46621(6) 0.32007(12) -0.09962(2) 0.03418(17) Uani 1.00 1 d .
S(9) S 0.26910(7) 0.06250(18) 0.20375(2) 0.0526(2) Uani 1.00 1 d .
S(10) S 0.47105(7) 0.64608(16) -0.15798(2) 0.0487(2) Uani 1.00 1 d .
P(1) P 0.5000 0.7171(2) 0.2500 0.0386(2) Uani 1.00 2 d S
C(1) C 0.2974(2) 0.3107(4) 0.09856(8) 0.0274(5) Uani 1.00 1 d .
C(2) C 0.32735(19) 0.1078(4) 0.09347(8) 0.0271(5) Uani 1.00 1 d .
C(3) C 0.39191(19) 0.5636(4) -0.05234(7) 0.0247(5) Uani 1.00 1 d .
C(4) C 0.42225(19) 0.3598(4) -0.05794(7) 0.0249(5) Uani 1.00 1 d .
C(5) C 0.2858(2) 0.1201(5) 0.16087(8) 0.0337(6) Uani 1.00 1 d .
C(6) C 0.44799(19) 0.5724(4) -0.11698(8) 0.0292(5) Uani 1.00 1 d .
C(7) C 0.5325(2) 0.8764(6) 0.21379(10) 0.0543(9) Uani 1.00 1 d .
C(8) C 0.4027(2) 0.5561(6) 0.23261(11) 0.0576(10) Uani 1.00 1 d .
H(1) H 0.5778 0.8029 0.2016 0.065 Uiso 1.00 1 c R
H(2) H 0.5592 1.0058 0.2239 0.065 Uiso 1.00 1 c R
H(3) H 0.4779 0.9063 0.1962 0.065 Uiso 1.00 1 c R
H(4) H 0.3453 0.6291 0.2350 0.069 Uiso 1.00 1 c R
H(5) H 0.4052 0.4273 0.2465 0.069 Uiso 1.00 1 c R
H(6) H 0.4050 0.5250 0.2070 0.069 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.125 0.123
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Pd Pd -0.999 1.007
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.102 0.094
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S(1) Pd(1) S(2) 90.18(2) yes . .
S(1) Pd(1) S(3) 89.34(2) yes . .
S(1) Pd(1) S(4) 176.26(2) yes . .
S(2) Pd(1) S(3) 176.51(2) yes . .
S(2) Pd(1) S(4) 90.51(2) yes . .
S(3) Pd(1) S(4) 89.74(2) yes . .
Pd(1) S(1) C(1) 101.37(10) yes . .
Pd(1) S(2) C(2) 101.33(10) yes . .
Pd(1) S(3) C(3) 102.13(9) yes . .
Pd(1) S(4) C(4) 101.75(10) yes . .
C(1) S(5) C(5) 97.56(14) yes . .
C(2) S(6) C(5) 97.58(14) yes . .
C(3) S(7) C(6) 97.50(14) yes . .
C(4) S(8) C(6) 97.50(14) yes . .
C(7) P(1) C(7) 110.6(2) yes . 2_655
C(7) P(1) C(8) 109.75(17) yes . .
C(7) P(1) C(8) 108.50(18) yes . 2_655
C(7) P(1) C(8) 108.50(18) yes 2_655 .
C(7) P(1) C(8) 109.75(17) yes 2_655 2_655
C(8) P(1) C(8) 109.72(19) yes . 2_655
S(1) C(1) S(5) 120.33(17) yes . .
S(1) C(1) C(2) 123.8(2) yes . .
S(5) C(1) C(2) 115.9(2) yes . .
S(2) C(2) S(6) 121.48(17) yes . .
S(2) C(2) C(1) 123.3(2) yes . .
S(6) C(2) C(1) 115.2(2) yes . .
S(3) C(3) S(7) 121.15(16) yes . .
S(3) C(3) C(4) 122.8(2) yes . .
S(7) C(3) C(4) 116.0(2) yes . .
S(4) C(4) S(8) 121.52(17) yes . .
S(4) C(4) C(3) 123.5(2) yes . .
S(8) C(4) C(3) 115.0(2) yes . .
S(5) C(5) S(6) 113.74(17) yes . .
S(5) C(5) S(9) 122.9(2) yes . .
S(6) C(5) S(9) 123.4(2) yes . .
S(7) C(6) S(8) 113.89(17) yes . .
S(7) C(6) S(10) 122.23(18) yes . .
S(8) C(6) S(10) 123.87(18) yes . .
P(1) C(7) H(1) 109.5 no . .
P(1) C(7) H(2) 109.5 no . .
P(1) C(7) H(3) 109.5 no . .
H(1) C(7) H(2) 109.5 no . .
H(1) C(7) H(3) 109.5 no . .
H(2) C(7) H(3) 109.5 no . .
P(1) C(8) H(4) 109.5 no . .
P(1) C(8) H(5) 109.5 no . .
P(1) C(8) H(6) 109.5 no . .
H(4) C(8) H(5) 109.5 no . .
H(4) C(8) H(6) 109.5 no . .
H(5) C(8) H(6) 109.5 no . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Pd(1) S(1) 2.2998(7) yes .
Pd(1) S(2) 2.3046(7) yes .
Pd(1) S(3) 2.2936(7) yes .
Pd(1) S(4) 2.3004(8) yes .
S(1) C(1) 1.700(2) yes .
S(2) C(2) 1.705(3) yes .
S(3) C(3) 1.692(2) yes .
S(4) C(4) 1.690(2) yes .
S(5) C(1) 1.743(3) yes .
S(5) C(5) 1.716(3) yes .
S(6) C(2) 1.744(3) yes .
S(6) C(5) 1.728(3) yes .
S(7) C(3) 1.738(2) yes .
S(7) C(6) 1.718(3) yes .
S(8) C(4) 1.746(2) yes .
S(8) C(6) 1.730(3) yes .
S(9) C(5) 1.657(3) yes .
S(10) C(6) 1.646(3) yes .
P(1) C(7) 1.778(4) yes .
P(1) C(7) 1.778(4) yes 2_655
P(1) C(8) 1.777(3) yes .
P(1) C(8) 1.777(3) yes 2_655
C(1) C(2) 1.380(4) yes .
C(3) C(4) 1.390(4) yes .
C(7) H(1) 0.960 no .
C(7) H(2) 0.960 no .
C(7) H(3) 0.960 no .
C(8) H(4) 0.960 no .
C(8) H(5) 0.960 no .
C(8) H(6) 0.960 no .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Pd(1) Pd(1) 3.1842(2) 7_555
S(1) S(2) 3.5226(9) 1_565
S(1) S(3) 3.4259(9) 7_565
S(1) S(4) 3.3320(10) 7_555
S(1) S(7) 3.4410(11) 7_565
S(2) S(1) 3.5226(9) 1_545
S(2) S(3) 3.4725(9) 1_545
S(2) S(3) 3.3230(10) 7_555
S(2) S(4) 3.5895(11) 3_655
S(2) S(8) 3.5152(10) 3_655
S(3) S(1) 3.4259(9) 7_565
S(3) S(2) 3.4725(9) 1_565
S(3) S(2) 3.3230(10) 7_555
S(3) S(3) 3.3948(12) 7_565
S(3) S(4) 3.5608(10) 1_565
S(4) S(1) 3.3320(10) 7_555
S(4) S(2) 3.5895(11) 3_655
S(4) S(3) 3.5608(10) 1_545
S(4) S(4) 3.5119(10) 3_655
S(4) S(7) 3.4407(10) 1_545
S(7) S(1) 3.4410(11) 7_565
S(7) S(4) 3.4407(10) 1_565
S(8) S(2) 3.5152(10) 3_655
C(1) C(4) 3.469(3) 7_555
C(2) C(3) 3.471(3) 7_555
C(3) C(2) 3.471(3) 7_555
C(4) C(1) 3.469(3) 7_555
S(5) H(6) 3.078 .
S(6) H(3) 2.989 1_545
S(9) H(1) 3.137 5_445
S(9) H(2) 3.370 2_645
S(9) H(3) 3.210 1_545
S(9) H(4) 3.120 1_545
S(9) H(4) 2.987 6_545
S(9) H(5) 3.283 .
S(9) H(5) 3.405 6_545
S(9) H(6) 3.522 .
S(10) H(1) 3.295 3_665
S(10) H(2) 3.253 3_675
S(10) H(3) 3.296 3_675
S(10) H(5) 3.514 4_564
S(10) H(6) 2.908 3_665
C(5) H(3) 3.183 1_545
C(5) H(6) 3.403 .
H(1) S(9) 3.137 5_555
H(1) S(10) 3.295 3_665
H(2) S(9) 3.370 2_665
H(2) S(10) 3.253 3_675
H(2) H(5) 2.906 2_665
H(3) S(6) 2.989 1_565
H(3) S(9) 3.210 1_565
H(3) S(10) 3.296 3_675
H(3) C(5) 3.183 1_565
H(4) S(9) 3.120 1_565
H(4) S(9) 2.987 6_555
H(5) S(9) 3.283 .
H(5) S(9) 3.405 6_555
H(5) S(10) 3.514 4_565
H(5) H(2) 2.906 2_645
H(6) S(5) 3.078 .
H(6) S(9) 3.522 .
H(6) S(10) 2.908 3_665
H(6) C(5) 3.403 .
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
S(1) Pd(1) S(2) C(2) -1.67(9)
S(2) Pd(1) S(1) C(1) 1.94(9)
S(1) Pd(1) S(3) C(3) 177.41(9)
S(3) Pd(1) S(1) C(1) -174.60(9)
S(1) Pd(1) S(4) C(4) -77.2(4)
S(4) Pd(1) S(1) C(1) -98.9(4)
S(2) Pd(1) S(3) C(3) 95.0(4)
S(3) Pd(1) S(2) C(2) 80.7(4)
S(2) Pd(1) S(4) C(4) -178.05(9)
S(4) Pd(1) S(2) C(2) 174.66(9)
S(3) Pd(1) S(4) C(4) -1.54(9)
S(4) Pd(1) S(3) C(3) 1.03(9)
Pd(1) S(1) C(1) S(5) 177.55(13)
Pd(1) S(1) C(1) C(2) -2.0(2)
Pd(1) S(2) C(2) S(6) -177.80(13)
Pd(1) S(2) C(2) C(1) 1.0(2)
Pd(1) S(3) C(3) S(7) 179.97(13)
Pd(1) S(3) C(3) C(4) -0.15(19)
Pd(1) S(4) C(4) S(12) -178.71(13)
Pd(1) S(4) C(4) C(3) 2.0(2)
C(1) S(5) C(5) S(6) -0.68(18)
C(1) S(5) C(5) S(9) 179.50(19)
C(5) S(5) C(1) S(1) -179.23(17)
C(5) S(5) C(1) C(2) 0.4(2)
C(2) S(6) C(5) S(5) 0.70(18)
C(2) S(6) C(5) S(9) -179.48(18)
C(5) S(6) C(2) S(2) 178.46(17)
C(5) S(6) C(2) C(1) -0.4(2)
C(3) S(7) C(6) S(10) 177.09(17)
C(3) S(7) C(6) S(12) -3.50(16)
C(6) S(7) C(3) S(3) -177.50(16)
C(6) S(7) C(3) C(4) 2.6(2)
C(4) S(12) C(6) S(7) 3.15(16)
C(4) S(12) C(6) S(10) -177.45(17)
C(6) S(12) C(4) S(4) 179.27(16)
C(6) S(12) C(4) C(3) -1.4(2)
S(1) C(1) C(2) S(2) 0.8(3)
S(1) C(1) C(2) S(6) 179.65(15)
S(5) C(1) C(2) S(2) -178.85(14)
S(5) C(1) C(2) S(6) 0.0(2)
S(3) C(3) C(4) S(4) -1.4(3)
S(3) C(3) C(4) S(12) 179.31(14)
S(7) C(3) C(4) S(4) 178.49(14)
S(7) C(3) C(4) S(12) -0.8(2)
