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#$Date: 2016-03-22 12:37:16 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178956 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/85/4118506.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_4118506
loop_
_publ_author_name
'Takashi Shirahata'
'Keita Shiratori'
'Shouhei Kumeta'
'Tadashi Kawamoto'
'Tadahiko Ishikawa'
'Shin-ya Koshihara'
'Yoshiaki Nakano'
'Hideki Yamochi'
'Misaki, Yohji'
'Takehiko Mori'
_publ_contact_author_address
;
Department of Applied Chemistry, 
Graduate School of Science and Engineering, 
Ehime University, 
3 Bunkyo-cho, Matsuyama 790-8577, Japan
;
_publ_contact_author_email       shirahata.takashi.mj@ehime-u.ac.jp
_publ_contact_author_fax         +81-89-927-9922
_publ_contact_author_name        'Dr Takashi Shirahata'
_publ_contact_author_phone       +81-89-927-8537
_publ_section_title
;
 Structural Transitions from Triangular to Square Molecular Arrangements
 in the Quasi-One-Dimensional Molecular Conductors (DMEDO-TTF)2XF6 (X = P,
 As, and Sb)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13330
_journal_page_last               13340
_journal_paper_doi               10.1021/ja303435n
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C20 H20 F6 O4 S8 Sb'
_chemical_formula_weight         816.59
_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                94.22(3)
_cell_angle_beta                 110.72(3)
_cell_angle_gamma                78.956(19)
_cell_formula_units_Z            1
_cell_length_a                   7.488(2)
_cell_length_b                   14.543(3)
_cell_length_c                   7.182(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    373
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      12.7
_cell_volume                     718.0(6)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      373
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4503
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  0.9685
_exptl_absorpt_correction_T_min  0.7827
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North, Phillips & Mathews, 1968 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       plate
_exptl_crystal_F_000             405
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         6.437
_refine_diff_density_min         -1.840
_refine_diff_density_rms         0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.278
_refine_ls_R_factor_all          0.1639
_refine_ls_R_factor_gt           0.1164
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2924
_refine_ls_wR_factor_ref         0.3462
_reflns_number_gt                2511
_reflns_number_total             4195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303435n_si_002_7.cif
_cod_data_source_block           DMEDO-TTF_2_SbF_6_HT
_cod_original_cell_volume        718.0(5)
_cod_database_code               4118506
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 0.3305(3) 0.60940(15) 0.6951(4) 0.0609(5) Uani 1 1 d . . .
S2 S 0.7372(3) 0.52097(14) 0.8348(3) 0.0577(5) Uani 1 1 d . . .
S3 S 0.1983(3) 0.41078(15) 0.6339(4) 0.0609(5) Uani 1 1 d . . .
S4 S 0.6096(3) 0.31704(15) 0.7730(4) 0.0602(5) Uani 1 1 d . . .
O1 O 0.0913(10) 0.2456(5) 0.5732(12) 0.079(2) Uani 1 1 d . . .
O2 O 0.4933(12) 0.1542(5) 0.7071(14) 0.086(2) Uani 1 1 d . . .
C1 C 0.4987(11) 0.5069(5) 0.7483(12) 0.0521(16) Uani 1 1 d . . .
C2 C 0.4434(11) 0.4204(5) 0.7196(12) 0.0517(15) Uani 1 1 d . . .
C3 C 0.5052(12) 0.6850(6) 0.7687(12) 0.0563(17) Uani 1 1 d . . .
C4 C 0.6887(12) 0.6438(6) 0.8303(13) 0.0551(16) Uani 1 1 d . . .
C5 C 0.2463(12) 0.2889(6) 0.6348(14) 0.0614(19) Uani 1 1 d . A .
C6 C 0.4348(14) 0.2467(6) 0.6960(14) 0.0623(19) Uani 1 1 d . A .
C7 C 0.4215(17) 0.7874(6) 0.747(2) 0.078(3) Uani 1 1 d . . .
H7A H 0.5234 0.8231 0.8063 0.117 Uiso 1 1 calc R . .
H7B H 0.3281 0.8022 0.8132 0.117 Uiso 1 1 calc R . .
H7C H 0.3593 0.8025 0.6087 0.117 Uiso 1 1 calc R . .
C8 C 0.8609(16) 0.6908(7) 0.8994(17) 0.074(2) Uani 1 1 d . . .
H8A H 0.8196 0.7571 0.9101 0.112 Uiso 1 1 calc R . .
H8B H 0.9276 0.6790 0.8056 0.112 Uiso 1 1 calc R . .
H8C H 0.9466 0.6667 1.0272 0.112 Uiso 1 1 calc R . .
C9A C 0.163(5) 0.144(2) 0.628(9) 0.072(9) Uani 0.49(7) 1 d P A 1
H9A1 H 0.1808 0.1387 0.7673 0.086 Uiso 0.49(7) 1 calc PR A 1
H9A2 H 0.0620 0.1098 0.5519 0.086 Uiso 0.49(7) 1 calc PR A 1
C10A C 0.328(5) 0.102(2) 0.602(9) 0.098(12) Uani 0.49(7) 1 d P A 1
H10A H 0.3082 0.0985 0.4604 0.117 Uiso 0.49(7) 1 calc PR A 1
H10B H 0.3625 0.0386 0.6520 0.117 Uiso 0.49(7) 1 calc PR A 1
C9B C 0.146(4) 0.146(2) 0.536(7) 0.073(8) Uani 0.51(7) 1 d P A 2
H9B1 H 0.1534 0.1370 0.4033 0.088 Uiso 0.51(7) 1 calc PR A 2
H9B2 H 0.0501 0.1120 0.5446 0.088 Uiso 0.51(7) 1 calc PR A 2
C10B C 0.356(5) 0.1079(18) 0.701(10) 0.110(15) Uani 0.51(7) 1 d P A 2
H10C H 0.3427 0.1117 0.8312 0.132 Uiso 0.51(7) 1 calc PR A 2
H10D H 0.3958 0.0424 0.6736 0.132 Uiso 0.51(7) 1 calc PR A 2
Sb1 Sb 0.0000 0.0000 0.0000 0.0720(4) Uani 1 2 d S . 2
F1 F -0.007(3) -0.0003(9) -0.2547(17) 0.211(8) Uani 1 1 d . B 2
F2 F -0.2469(14) -0.0283(8) -0.091(2) 0.170(5) Uani 1 1 d . C 2
F3 F 0.074(2) -0.1239(7) 0.017(3) 0.196(7) Uani 1 1 d . D 2
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'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 '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
C1 S1 C3 95.3(4) . .
C1 S2 C4 95.9(4) . .
C5 S3 C2 93.8(4) . .
C6 S4 C2 94.2(4) . .
C5 O1 C9B 111.5(15) . .
C5 O1 C9A 107.4(15) . .
C9B O1 C9A 24.6(12) . .
C10B O2 C6 113.3(16) . .
C10B O2 C10A 26(3) . .
C6 O2 C10A 112.0(15) . .
C2 C1 S2 123.0(6) . .
C2 C1 S1 121.8(6) . .
S2 C1 S1 115.3(4) . .
C1 C2 S4 122.4(6) . .
C1 C2 S3 120.8(6) . .
S4 C2 S3 116.8(4) . .
C4 C3 C7 129.0(8) . .
C4 C3 S1 116.2(6) . .
C7 C3 S1 114.8(7) . .
C3 C4 C8 126.7(8) . .
C3 C4 S2 117.3(7) . .
C8 C4 S2 116.0(7) . .
O1 C5 C6 126.3(8) . .
O1 C5 S3 116.6(7) . .
C6 C5 S3 117.1(7) . .
O2 C6 C5 123.8(9) . .
O2 C6 S4 118.1(7) . .
C5 C6 S4 118.0(7) . .
C3 C7 H7A 109.5 . .
C3 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C3 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C4 C8 H8A 109.5 . .
C4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10A C9A O1 118(3) . .
C10A C9A H9A1 107.8 . .
O1 C9A H9A1 107.8 . .
C10A C9A H9A2 107.8 . .
O1 C9A H9A2 107.8 . .
H9A1 C9A H9A2 107.1 . .
C9A C10A O2 112(4) . .
C9A C10A H10A 109.3 . .
O2 C10A H10A 109.3 . .
C9A C10A H10B 109.3 . .
O2 C10A H10B 109.3 . .
H10A C10A H10B 108.0 . .
O1 C9B C10B 108(3) . .
O1 C9B H9B1 110.0 . .
C10B C9B H9B1 110.0 . .
O1 C9B H9B2 110.0 . .
C10B C9B H9B2 110.0 . .
H9B1 C9B H9B2 108.4 . .
O2 C10B C9B 114(4) . .
O2 C10B H10C 108.8 . .
C9B C10B H10C 108.8 . .
O2 C10B H10D 108.8 . .
C9B C10B H10D 108.8 . .
H10C C10B H10D 107.6 . .
F3 Sb1 F3 180.000(1) . 2
F3 Sb1 F1 92.0(8) . .
F3 Sb1 F1 88.0(8) 2 .
F3 Sb1 F1 88.0(8) . 2
F3 Sb1 F1 92.0(8) 2 2
F1 Sb1 F1 180.000(1) . 2
F3 Sb1 F2 96.1(6) . 2
F3 Sb1 F2 83.9(6) 2 2
F1 Sb1 F2 90.6(7) . 2
F1 Sb1 F2 89.4(7) 2 2
F3 Sb1 F2 83.9(6) . .
F3 Sb1 F2 96.1(6) 2 .
F1 Sb1 F2 89.4(7) . .
F1 Sb1 F2 90.6(7) 2 .
F2 Sb1 F2 180.0 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C1 1.725(8) .
S1 C3 1.782(9) .
S2 C1 1.719(8) .
S2 C4 1.754(8) .
S3 C5 1.741(9) .
S3 C2 1.747(8) .
S4 C6 1.727(9) .
S4 C2 1.728(8) .
O1 C5 1.347(10) .
O1 C9B 1.46(3) .
O1 C9A 1.50(3) .
O2 C10B 1.32(3) .
O2 C6 1.331(11) .
O2 C10A 1.51(4) .
C1 C2 1.378(11) .
C3 C4 1.317(12) .
C3 C7 1.497(12) .
C4 C8 1.487(13) .
C5 C6 1.353(13) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9A C10A 1.34(6) .
C9A H9A1 0.9700 .
C9A H9A2 0.9700 .
C10A H10A 0.9700 .
C10A H10B 0.9700 .
C9B C10B 1.62(7) .
C9B H9B1 0.9700 .
C9B H9B2 0.9700 .
C10B H10C 0.9700 .
C10B H10D 0.9700 .
Sb1 F3 1.782(10) .
Sb1 F3 1.782(10) 2
Sb1 F1 1.810(11) .
Sb1 F1 1.810(11) 2
Sb1 F2 1.847(9) 2
Sb1 F2 1.847(9) .
