#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/45/4114592.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_4114592
loop_
_publ_author_name
'Hiroyuki Nishikawa'
'Takanobu Morimoto'
'Takeshi Kodama'
'Isao Ikemoto'
'Koichi Kikuchi'
'Jun-ichi Yamada'
'Harukazu Yoshino'
'Keizo Murata'
_publ_contact_author_address
;
Department of Chemistry, Faculty of Science, Tokyo Metroplitan University, 
Hachioji, Tokyo 192-0397, Japan  
;
_publ_contact_author_email       hiron@comp.metro-u.ac.jp
_publ_contact_author_fax         81-426-77-2525
_publ_contact_author_name        'Hiroyuki Nishikawa'
_publ_contact_author_phone       81-426-77-2530
_publ_section_title
;
 New Organic Superconductors Consisting of an Unprecedented π-Electron
 Donor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              730
_journal_page_last               731
_journal_paper_doi               10.1021/ja011114t
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C20 H20 As F6 O4 S12'
_chemical_formula_weight         898.00
_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                101.720(2)
_cell_angle_beta                 98.150(2)
_cell_angle_gamma                107.282(2)
_cell_formula_units_Z            1
_cell_length_a                   5.7518(5)
_cell_length_b                   9.4285(8)
_cell_length_c                   15.8745(14)
_cell_measurement_reflns_used    2620
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.34
_cell_volume                     785.85(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.705
_diffrn_measured_fraction_theta_max 0.705
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3257
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0.35
_diffrn_standards_number         80
_exptl_absorpt_coefficient_mu    1.95
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       plate
_exptl_crystal_F_000             451.00
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0450
_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)+(0.0605P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                1926
_reflns_number_total             2741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011114t_1.cif
_cod_data_source_block           (DODHT)2AsF6
_cod_original_formula_sum        'C20 H20 S12 O4 As1 F6'
_cod_database_code               4114592
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
S1 S 1.2536(3) 1.00457(13) 1.13913(9) 0.0561(4) Uani 1 1 d .
S2 S 0.7604(2) 0.78984(14) 1.13700(8) 0.0501(3) Uani 1 1 d .
S3 S 1.2510(2) 0.79905(12) 0.95025(7) 0.0427(3) Uani 1 1 d .
S4 S 0.7614(2) 0.58015(12) 0.94783(7) 0.0397(3) Uani 1 1 d .
S5 S 1.3162(2) 0.61787(13) 0.78554(7) 0.0406(3) Uani 1 1 d .
S6 S 0.7399(2) 0.36763(11) 0.77628(8) 0.0418(3) Uani 1 1 d .
O1 O 1.1593(6) 0.5370(3) 0.61100(19) 0.0411(8) Uani 1 1 d .
O2 O 0.7387(5) 0.5618(3) 0.67759(18) 0.0389(8) Uani 1 1 d .
C1 C 1.1328(12) 1.0475(6) 1.2341(4) 0.0753(18) Uani 1 1 d .
H1A H 1.2537 1.0535 1.2851 0.090 Uiso 1 1 calc R
H1B H 1.1171 1.1485 1.2404 0.090 Uiso 1 1 calc R
C2 C 0.8979(14) 0.9420(8) 1.2355(4) 0.100(2) Uani 1 1 d .
H2A H 0.7837 0.9983 1.2454 0.120 Uiso 1 1 calc R
H2B H 0.9198 0.8975 1.2848 0.120 Uiso 1 1 calc R
C3 C 1.0067(8) 0.8358(4) 1.0852(3) 0.0339(10) Uani 1 1 d .
C4 C 1.0103(8) 0.7475(4) 1.0058(3) 0.0319(9) Uani 1 1 d .
C5 C 1.1296(8) 0.6341(4) 0.8611(3) 0.0316(9) Uani 1 1 d .
C6 C 0.9041(8) 0.5348(4) 0.8609(3) 0.0322(9) Uani 1 1 d .
C7 C 1.1012(8) 0.4789(4) 0.6830(3) 0.0348(10) Uani 1 1 d .
H7 H 1.1402 0.3835 0.6764 0.042 Uiso 1 1 calc R
C8 C 0.8269(8) 0.4377(4) 0.6830(3) 0.0326(10) Uani 1 1 d .
H8 H 0.7377 0.3544 0.6298 0.039 Uiso 1 1 calc R
C9 C 1.0578(10) 0.6575(5) 0.6012(3) 0.0503(14) Uani 1 1 d .
H9A H 1.0889 0.6871 0.5477 0.060 Uiso 1 1 calc R
H9B H 1.1396 0.7470 0.6507 0.060 Uiso 1 1 calc R
C10 C 0.7872(10) 0.6037(5) 0.5972(3) 0.0480(13) Uani 1 1 d .
H10A H 0.7204 0.6845 0.5896 0.058 Uiso 1 1 calc R
H10B H 0.7048 0.5154 0.5471 0.058 Uiso 1 1 calc R
As1 As 0.5000 0.0000 0.5000 0.0438(2) Uani 1 2 d S
F1 F 0.1962(6) -0.1068(3) 0.4529(2) 0.0794(11) Uani 1 1 d .
F2 F 0.4503(7) 0.1626(3) 0.4857(3) 0.0951(14) Uani 1 1 d .
F3 F 0.5707(8) -0.0338(4) 0.3988(2) 0.1028(13) 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'
As As 0.0499 2.0058 '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'
O O 0.0106 0.0060 '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'
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
C3 S1 C1 96.1(2) . .
C3 S2 C2 96.9(3) . .
C4 S3 C5 95.9(2) . .
C6 S4 C4 95.2(2) . .
C5 S5 C7 105.3(2) . .
C6 S6 C8 99.01(19) . .
C7 O1 C9 112.6(4) . .
C8 O2 C10 107.4(4) . .
C2 C1 S1 116.4(4) . .
C1 C2 S2 114.2(5) . .
C4 C3 S2 122.8(3) . .
C4 C3 S1 121.0(3) . .
S2 C3 S1 116.2(3) . .
C3 C4 S3 122.9(3) . .
C3 C4 S4 122.3(3) . .
S3 C4 S4 114.5(2) . .
C6 C5 S5 128.2(3) . .
C6 C5 S3 116.0(3) . .
S5 C5 S3 115.8(2) . .
C5 C6 S6 124.1(4) . .
C5 C6 S4 118.0(3) . .
S6 C6 S4 117.8(2) . .
O1 C7 C8 111.9(3) . .
O1 C7 S5 108.1(3) . .
C8 C7 S5 115.4(3) . .
O2 C8 C7 112.2(3) . .
O2 C8 S6 108.9(3) . .
C7 C8 S6 114.3(3) . .
O1 C9 C10 110.3(3) . .
O2 C10 C9 110.1(3) . .
F2 As1 F2 180.0(3) . 2_656
F2 As1 F3 89.6(2) . 2_656
F2 As1 F3 90.4(2) 2_656 2_656
F2 As1 F3 90.4(2) . .
F2 As1 F3 89.6(2) 2_656 .
F3 As1 F3 180.00(8) 2_656 .
F2 As1 F1 91.30(15) . .
F2 As1 F1 88.70(16) 2_656 .
F3 As1 F1 90.69(19) 2_656 .
F3 As1 F1 89.31(19) . .
F2 As1 F1 88.70(16) . 2_656
F2 As1 F1 91.30(15) 2_656 2_656
F3 As1 F1 89.31(19) 2_656 2_656
F3 As1 F1 90.69(19) . 2_656
F1 As1 F1 180.0(2) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C3 1.744(4) .
S1 C1 1.770(7) .
S2 C3 1.727(5) .
S2 C2 1.787(6) .
S3 C4 1.746(5) .
S3 C5 1.757(4) .
S4 C6 1.746(5) .
S4 C4 1.755(4) .
S5 C5 1.733(5) .
S5 C7 1.870(4) .
S6 C6 1.754(4) .
S6 C8 1.815(4) .
O1 C7 1.404(5) .
O1 C9 1.447(5) .
O2 C8 1.419(4) .
O2 C10 1.450(6) .
C1 C2 1.427(9) .
C3 C4 1.369(6) .
C5 C6 1.355(6) .
C7 C8 1.508(6) .
C9 C10 1.474(7) .
As1 F2 1.693(3) .
As1 F2 1.693(3) 2_656
As1 F3 1.703(4) 2_656
As1 F3 1.703(4) .
As1 F1 1.704(3) .
As1 F1 1.704(3) 2_656
