#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/46/7204637.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_7204637
loop_
_publ_author_name
'Zou, Lei'
'Xu, Wei'
'Jia, Chunyang'
'Zhang, Deqing'
'Wang, Quanrui'
'Zhu, Daoben'
_publ_section_title
;
 Cation radical salts of ethylenedisulfanyl-bridged dimeric
 ethylenedithiotetrathiafulvalene with
 2,3,5,6-tetrafluoro-7,7,8,8-tetracyanoquinodimethane (TCNQF4), PF6?,
 AsF6?and BF4?: synthesis, structure and conducting properties
;
_journal_issue                   7
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1646
_journal_paper_doi               10.1039/b303102k
_journal_volume                  13
_journal_year                    2003
_chemical_formula_sum            'C18.5 H15 Cl F6 P S14'
_chemical_formula_weight         866.58
_chemical_name_systematic
;
?
;
_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                97.76(3)
_cell_angle_beta                 96.96(3)
_cell_angle_gamma                101.04(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6200(15)
_cell_length_b                   13.024(3)
_cell_length_c                   15.709(3)
_cell_measurement_temperature    123(2)
_cell_volume                     1498.7(6)
_computing_cell_refinement       'RAPID AUTO (Riogaku, 2001)'
_computing_data_collection       'RAPID AUTO (Riogaku, 2001)'
_computing_data_reduction        'RAPID AUTO (Riogaku, 2001)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10527
_diffrn_reflns_theta_full        27.36
_diffrn_reflns_theta_max         27.36
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  1.1792
_exptl_absorpt_correction_T_min  0.8054
_exptl_absorpt_correction_type   T.Higashi
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                4169
_reflns_number_total             6655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303102k.txt
_cod_data_source_block           1-PF6
_cod_original_cell_volume        1498.7(5)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18.50 H15 Cl F6 P S14'
_cod_database_code               7204637
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
P1 P 0.18711(16) 0.29656(10) 0.99750(7) 0.0226(3) Uani 1 1 d . . .
S1 S -0.25241(16) 0.26293(9) 0.24467(7) 0.0250(3) Uani 1 1 d . . .
S2 S -0.07726(15) 0.53297(9) 0.25813(7) 0.0213(3) Uani 1 1 d . . .
S3 S -0.31385(15) 0.32349(8) 0.42701(7) 0.0198(2) Uani 1 1 d . . .
S4 S -0.17220(15) 0.55100(8) 0.43316(7) 0.0184(2) Uani 1 1 d . . .
S5 S -0.26641(15) 0.59912(8) 0.62714(7) 0.0193(2) Uani 1 1 d . . .
S6 S -0.41247(15) 0.37218(8) 0.62124(7) 0.0187(2) Uani 1 1 d . . .
S7 S -0.50968(15) 0.40420(9) 0.80225(7) 0.0207(3) Uani 1 1 d . . .
S8 S -0.46276(15) 0.14981(9) 0.73777(7) 0.0216(3) Uani 1 1 d . . .
S9 S 0.06469(14) 0.20096(8) 0.65190(6) 0.0166(2) Uani 1 1 d . . .
S10 S -0.31381(14) 0.10667(9) 0.57652(6) 0.0177(2) Uani 1 1 d . . .
S11 S 0.18430(14) 0.15518(8) 0.46271(6) 0.0185(2) Uani 1 1 d . . .
S12 S -0.19243(14) 0.05444(9) 0.38929(6) 0.0185(2) Uani 1 1 d . . .
S13 S 0.32611(16) 0.13668(10) 0.29784(7) 0.0268(3) Uani 1 1 d . . .
S14 S -0.12036(16) 0.00200(9) 0.21030(7) 0.0234(3) Uani 1 1 d . . .
F1 F 0.1277(5) 0.3103(3) 0.90074(19) 0.0785(13) Uani 1 1 d . . .
F2 F 0.2438(5) 0.2819(3) 1.09536(18) 0.0646(11) Uani 1 1 d . . .
F3 F 0.1600(6) 0.1732(3) 0.9679(2) 0.0796(12) Uani 1 1 d . . .
F4 F 0.2064(5) 0.4181(2) 1.0292(2) 0.0628(10) Uani 1 1 d . . .
F5 F -0.0180(4) 0.2750(3) 1.0118(2) 0.0688(11) Uani 1 1 d . . .
F6 F 0.3903(4) 0.3167(3) 0.9846(2) 0.0656(11) Uani 1 1 d . . .
C1 C -0.1153(7) 0.4310(4) 0.1633(3) 0.0297(11) Uani 1 1 d . . .
H1A H -0.1303 0.4638 0.1117 0.036 Uiso 1 1 calc R . .
H1B H -0.0085 0.4009 0.1622 0.036 Uiso 1 1 calc R . .
C2 C -0.2775(6) 0.3422(4) 0.1589(3) 0.0280(11) Uani 1 1 d . . .
H2A H -0.2962 0.2965 0.1030 0.034 Uiso 1 1 calc R . .
H2B H -0.3840 0.3720 0.1630 0.034 Uiso 1 1 calc R . .
C3 C -0.2337(5) 0.3617(3) 0.3343(3) 0.0171(9) Uani 1 1 d . . .
C4 C -0.1660(5) 0.4662(3) 0.3374(3) 0.0175(9) Uani 1 1 d . . .
C5 C -0.2670(5) 0.4499(3) 0.4865(3) 0.0162(9) Uani 1 1 d . . .
C6 C -0.3080(5) 0.4713(3) 0.5688(3) 0.0155(9) Uani 1 1 d . . .
C7 C -0.4166(5) 0.4583(3) 0.7174(2) 0.0187(10) Uani 1 1 d . . .
C8 C -0.3489(6) 0.5611(3) 0.7186(3) 0.0215(10) Uani 1 1 d . . .
H8A H -0.3461 0.6109 0.7674 0.026 Uiso 1 1 calc R . .
C9 C -0.3244(6) 0.3465(3) 0.8469(3) 0.0202(10) Uani 1 1 d . . .
H9A H -0.2250 0.3609 0.8140 0.024 Uiso 1 1 calc R . .
H9B H -0.2815 0.3805 0.9066 0.024 Uiso 1 1 calc R . .
C10 C -0.3799(6) 0.2269(3) 0.8443(3) 0.0204(10) Uani 1 1 d . . .
H10A H -0.4733 0.2135 0.8807 0.024 Uiso 1 1 calc R . .
H10B H -0.2764 0.2020 0.8696 0.024 Uiso 1 1 calc R . .
C11 C -0.0949(6) 0.1982(3) 0.7221(3) 0.0180(9) Uani 1 1 d . . .
H11A H -0.0615 0.2241 0.7811 0.022 Uiso 1 1 calc R . .
C12 C -0.2686(6) 0.1572(3) 0.6878(2) 0.0165(9) Uani 1 1 d . . .
C13 C -0.0892(5) 0.1378(3) 0.5602(2) 0.0143(9) Uani 1 1 d . . .
C14 C -0.0378(5) 0.1170(3) 0.4804(2) 0.0145(9) Uani 1 1 d . . .
C15 C 0.1390(6) 0.1091(3) 0.3508(3) 0.0168(9) Uani 1 1 d . . .
C16 C -0.0344(6) 0.0607(3) 0.3170(3) 0.0181(9) Uani 1 1 d . . .
C17 C 0.2415(6) 0.0645(4) 0.1896(3) 0.0296(11) Uani 1 1 d . . .
H17A H 0.3206 0.0919 0.1502 0.035 Uiso 1 1 calc R . .
H17B H 0.2468 -0.0094 0.1893 0.035 Uiso 1 1 calc R . .
C18 C 0.0505(7) 0.0707(4) 0.1558(3) 0.0316(12) Uani 1 1 d . . .
H18A H 0.0243 0.0414 0.0944 0.038 Uiso 1 1 calc R . .
H18B H 0.0426 0.1447 0.1615 0.038 Uiso 1 1 calc R . .
Cl1 Cl -0.3249(2) 0.07493(11) 1.01445(9) 0.0491(4) Uani 1 1 d . . .
C19 C -0.5535(13) 0.0325(8) 0.9575(7) 0.036(2) Uani 0.50 1 d P . .
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'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
F6 P1 F4 90.0(2) . . ?
F6 P1 F1 91.0(2) . . ?
F4 P1 F1 90.9(2) . . ?
F6 P1 F3 92.5(2) . . ?
F4 P1 F3 177.3(2) . . ?
F1 P1 F3 90.1(2) . . ?
F6 P1 F5 179.0(2) . . ?
F4 P1 F5 90.44(19) . . ?
F1 P1 F5 89.8(2) . . ?
F3 P1 F5 87.1(2) . . ?
F6 P1 F2 89.9(2) . . ?
F4 P1 F2 89.26(19) . . ?
F1 P1 F2 179.1(2) . . ?
F3 P1 F2 89.7(2) . . ?
F5 P1 F2 89.2(2) . . ?
C3 S1 C2 98.8(2) . . ?
C4 S2 C1 103.8(2) . . ?
C5 S3 C3 95.6(2) . . ?
C5 S4 C4 94.9(2) . . ?
C8 S5 C6 95.3(2) . . ?
C6 S6 C7 95.1(2) . . ?
C7 S7 C9 100.5(2) . . ?
C12 S8 C10 103.5(2) . . ?
C11 S9 C13 95.16(19) . . ?
C13 S10 C12 94.85(19) . . ?
C14 S11 C15 95.23(19) . . ?
C14 S12 C16 95.3(2) . . ?
C15 S13 C17 102.2(2) . . ?
C16 S14 C18 99.4(2) . . ?
C2 C1 S2 114.8(3) . . ?
C1 C2 S1 112.9(3) . . ?
C4 C3 S3 116.9(3) . . ?
C4 C3 S1 125.6(3) . . ?
S3 C3 S1 117.5(2) . . ?
C3 C4 S2 129.8(3) . . ?
C3 C4 S4 117.0(3) . . ?
S2 C4 S4 113.2(2) . . ?
C6 C5 S3 123.0(3) . . ?
C6 C5 S4 121.4(3) . . ?
S3 C5 S4 115.5(2) . . ?
C5 C6 S5 122.8(3) . . ?
C5 C6 S6 122.1(3) . . ?
S5 C6 S6 115.0(2) . . ?
C8 C7 S7 125.3(3) . . ?
C8 C7 S6 116.2(3) . . ?
S7 C7 S6 118.5(3) . . ?
C7 C8 S5 118.3(3) . . ?
C10 C9 S7 112.9(3) . . ?
C9 C10 S8 115.4(3) . . ?
C12 C11 S9 117.4(3) . . ?
C11 C12 S10 117.1(3) . . ?
C11 C12 S8 129.3(3) . . ?
S10 C12 S8 113.6(2) . . ?
C14 C13 S9 122.3(3) . . ?
C14 C13 S10 122.3(3) . . ?
S9 C13 S10 115.4(2) . . ?
C13 C14 S12 121.9(3) . . ?
C13 C14 S11 122.4(3) . . ?
S12 C14 S11 115.7(2) . . ?
C16 C15 S13 129.2(3) . . ?
C16 C15 S11 117.0(3) . . ?
S13 C15 S11 113.8(2) . . ?
C15 C16 S14 128.1(3) . . ?
C15 C16 S12 116.7(3) . . ?
S14 C16 S12 115.2(2) . . ?
C18 C17 S13 114.3(3) . . ?
C17 C18 S14 114.6(3) . . ?
C19 Cl1 C19 64.7(6) 2_457 . ?
Cl1 C19 Cl1 115.3(6) 2_457 . ?
Cl1 C19 C19 61.2(5) 2_457 2_457 ?
Cl1 C19 C19 54.1(5) . 2_457 ?
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
P1 F6 1.563(3) . ?
P1 F4 1.567(3) . ?
P1 F1 1.576(3) . ?
P1 F3 1.578(3) . ?
P1 F5 1.583(3) . ?
P1 F2 1.592(3) . ?
S1 C3 1.746(4) . ?
S1 C2 1.819(5) . ?
S2 C4 1.742(5) . ?
S2 C1 1.812(4) . ?
S3 C5 1.730(4) . ?
S3 C3 1.743(4) . ?
S4 C5 1.743(4) . ?
S4 C4 1.753(4) . ?
S5 C8 1.731(5) . ?
S5 C6 1.740(4) . ?
S6 C6 1.742(4) . ?
S6 C7 1.763(4) . ?
S7 C7 1.751(5) . ?
S7 C9 1.833(4) . ?
S8 C12 1.750(4) . ?
S8 C10 1.804(4) . ?
S9 C11 1.736(4) . ?
S9 C13 1.740(4) . ?
S10 C13 1.740(4) . ?
S10 C12 1.750(4) . ?
S11 C14 1.737(4) . ?
S11 C15 1.749(4) . ?
S12 C14 1.734(4) . ?
S12 C16 1.751(4) . ?
S13 C15 1.739(4) . ?
S13 C17 1.806(4) . ?
S14 C16 1.737(4) . ?
S14 C18 1.805(5) . ?
C1 C2 1.510(6) . ?
C3 C4 1.352(6) . ?
C5 C6 1.371(5) . ?
C7 C8 1.336(6) . ?
C9 C10 1.528(6) . ?
C11 C12 1.344(6) . ?
C13 C14 1.367(5) . ?
C15 C16 1.358(6) . ?
C17 C18 1.509(6) . ?
Cl1 C19 1.667(10) 2_457 ?
Cl1 C19 1.805(10) . ?
C19 Cl1 1.667(10) 2_457 ?
C19 C19 1.86(2) 2_457 ?
