#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:34:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180343 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/12/7201236.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_7201236
loop_
_publ_author_name
'Zorina, Leokadiya'
'Simonov, Sergey'
'Mézière, Cécile'
'Canadell, Enric'
'Suh, Steve'
'Brown, Stuart E.'
'Foury-Leylekian, Pascale'
'Fertey, Pierre'
'Pouget, Jean-Paul'
'Batail, Patrick'
_publ_section_title
;
 Charge ordering, symmetry and electronic structure issues and Wigner
 crystal structure of the quarter-filled band Mott insulators and high
 pressure metals δ-(EDT-TTF-CONMe2)2X, X = Br and AsF6
;
_journal_issue                   38
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              6980
_journal_paper_doi               10.1039/b906287d
_journal_volume                  19
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C11 H11 N O S6), As F6'
_chemical_formula_sum            'C22 H22 As F6 N2 O2 S12'
_chemical_formula_weight         920.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ac'
_symmetry_space_group_name_H-M   'P 1 1 21/a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED (Oxford Diffraction Ltd.),
SHELXL-97 and WinGX routine-INITIALISE
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                92.255(13)
_cell_formula_units_Z            2
_cell_length_a                   7.0157(8)
_cell_length_b                   6.4219(13)
_cell_length_c                   35.465(5)
_cell_measurement_reflns_used    90
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     1596.6(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Direct methods (Sir92,Altomare et al.,1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       'combined φ and ω-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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0876
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            46120
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         32.07
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.915
_exptl_absorpt_correction_T_max  0.9152
_exptl_absorpt_correction_T_min  0.7476
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'see N.W. Alcock (1970). Cryst. Computing, p.271'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.747
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         46120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1073P)²+4.8322P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.2160
_reflns_number_gt                28241
_reflns_number_total             46120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906287d.txt
_cod_data_source_block           delta-(EDT-TTF-CONMe2)2AsF6_(P21/a,100K)
_cod_database_code               7201236
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.0000 0.0000 0.0000 0.01978(8) Uani 1 2 d S . .
F1 F 0.0181(3) -0.1357(2) 0.04074(4) 0.0766(6) Uani 1 1 d . . .
F3 F 0.1746(2) 0.1698(3) 0.01559(5) 0.0610(5) Uani 1 1 d . . .
F2 F -0.1644(2) 0.1492(3) 0.02092(5) 0.0681(6) Uani 1 1 d . . .
S3 S 0.00277(7) 0.48789(8) 0.310099(13) 0.01624(11) Uani 1 1 d . . .
S6 S 0.01141(7) 0.69112(8) 0.116931(13) 0.01704(11) Uani 1 1 d . . .
S2 S 0.03535(7) 0.77584(8) 0.198809(14) 0.01701(11) Uani 1 1 d . . .
S1 S -0.00318(7) 0.33910(8) 0.222154(14) 0.01902(12) Uani 1 1 d . . .
S4 S 0.03564(7) 0.92270(8) 0.285259(14) 0.01893(12) Uani 1 1 d . . .
S5 S -0.03912(8) 0.16903(8) 0.145438(14) 0.02190(13) Uani 1 1 d . . .
C2 C 0.0174(2) 0.6600(3) 0.27251(5) 0.0134(4) Uani 1 1 d . . .
O1 O 0.00520(18) 0.3842(2) 0.38225(4) 0.0201(3) Uani 1 1 d . . .
C4 C 0.0071(2) 0.5902(3) 0.16273(5) 0.0136(4) Uani 1 1 d . . .
C3 C -0.0104(3) 0.3896(3) 0.17386(5) 0.0161(4) Uani 1 1 d . . .
C7 C 0.0589(3) 0.2683(3) 0.10199(6) 0.0192(4) Uani 1 1 d . . .
H7A H 0.1939 0.3009 0.1055 0.023 Uiso 1 1 calc R . .
H7B H 0.0461 0.1607 0.0829 0.023 Uiso 1 1 calc R . .
C8 C -0.0362(3) 0.4606(3) 0.08817(6) 0.0187(4) Uani 1 1 d . . .
H8A H -0.1730 0.4319 0.0873 0.022 Uiso 1 1 calc R . .
H8B H 0.0063 0.4900 0.0626 0.022 Uiso 1 1 calc R . .
N1 N 0.0026(2) 0.6874(3) 0.41527(4) 0.0179(4) Uani 1 1 d . . .
C1 C 0.0154(2) 0.5990(3) 0.23580(5) 0.0158(4) Uani 1 1 d . . .
C9 C 0.0052(2) 0.5779(3) 0.38312(5) 0.0146(4) Uani 1 1 d . . .
C5 C 0.0121(3) 0.6812(3) 0.34532(5) 0.0154(4) Uani 1 1 d . . .
C6 C 0.0268(2) 0.8795(3) 0.33313(5) 0.0174(4) Uani 1 1 d . . .
H6 H 0.0321 0.9901 0.3501 0.021 Uiso 1 1 calc R . .
C10 C -0.0103(3) 0.5761(4) 0.45113(6) 0.0236(5) Uani 1 1 d . . .
H10A H -0.0082 0.4288 0.4466 0.035 Uiso 1 1 calc R . .
H10B H -0.1271 0.6080 0.4636 0.035 Uiso 1 1 calc R . .
H10C H 0.0960 0.6183 0.4668 0.035 Uiso 1 1 calc R . .
C11 C 0.0028(3) 0.9147(3) 0.41752(6) 0.0275(5) Uani 1 1 d . . .
H11A H 0.1198 0.9727 0.4073 0.041 Uiso 1 1 calc R . .
H11B H -0.0086 0.9564 0.4434 0.041 Uiso 1 1 calc R . .
H11C H -0.1029 0.9645 0.4034 0.041 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'
As As 0.0499 2.0058 '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'
N N 0.0061 0.0033 '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'
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
F1 As1 F1 180.00(10) . 3 ?
F1 As1 F2 89.07(9) . . ?
F1 As1 F2 90.93(9) 3 . ?
F1 As1 F2 90.93(9) . 3 ?
F1 As1 F2 89.07(9) 3 3 ?
F2 As1 F2 180.00(13) . 3 ?
F1 As1 F3 90.80(9) . 3 ?
F1 As1 F3 89.20(9) 3 3 ?
F2 As1 F3 90.89(8) . 3 ?
F2 As1 F3 89.11(8) 3 3 ?
F1 As1 F3 89.20(9) . . ?
F1 As1 F3 90.80(9) 3 . ?
F2 As1 F3 89.11(8) . . ?
F2 As1 F3 90.89(8) 3 . ?
F3 As1 F3 180.00(14) 3 . ?
C2 S3 C5 95.54(9) . . ?
C4 S6 C8 102.69(10) . . ?
C1 S2 C4 95.90(10) . . ?
C1 S1 C3 95.54(10) . . ?
C6 S4 C2 95.68(10) . . ?
C3 S5 C7 100.22(10) . . ?
C1 C2 S3 123.61(16) . . ?
C1 C2 S4 121.72(16) . . ?
S3 C2 S4 114.67(10) . . ?
C3 C4 S6 128.72(15) . . ?
C3 C4 S2 116.05(15) . . ?
S6 C4 S2 115.21(11) . . ?
C4 C3 S5 127.61(15) . . ?
C4 C3 S1 117.57(15) . . ?
S5 C3 S1 114.83(12) . . ?
C8 C7 S5 113.23(14) . . ?
C8 C7 H7A 108.9 . . ?
S5 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
S5 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 S6 114.28(14) . . ?
C7 C8 H8A 108.7 . . ?
S6 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
S6 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C9 N1 C10 119.10(17) . . ?
C9 N1 C11 124.81(17) . . ?
C10 N1 C11 116.02(16) . . ?
C2 C1 S2 122.37(16) . . ?
C2 C1 S1 122.88(15) . . ?
S2 C1 S1 114.75(11) . . ?
O1 C9 N1 123.11(18) . . ?
O1 C9 C5 114.82(17) . . ?
N1 C9 C5 122.06(18) . . ?
C6 C5 C9 135.09(18) . . ?
C6 C5 S3 116.03(15) . . ?
C9 C5 S3 108.87(14) . . ?
C5 C6 S4 118.09(16) . . ?
C5 C6 H6 121.0 . . ?
S4 C6 H6 121.0 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
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
As1 F1 1.6945(15) . ?
As1 F1 1.6945(15) 3 ?
As1 F2 1.6988(15) . ?
As1 F2 1.6988(15) 3 ?
As1 F3 1.7002(14) 3 ?
As1 F3 1.7002(14) . ?
S3 C2 1.732(2) . ?
S3 C5 1.761(2) . ?
S6 C4 1.7483(19) . ?
S6 C8 1.818(2) . ?
S2 C1 1.737(2) . ?
S2 C4 1.755(2) . ?
S1 C1 1.738(2) . ?
S1 C3 1.744(2) . ?
S4 C6 1.7208(19) . ?
S4 C2 1.746(2) . ?
S5 C3 1.744(2) . ?
S5 C7 1.794(2) . ?
C2 C1 1.359(3) . ?
O1 C9 1.244(2) . ?
C4 C3 1.349(3) . ?
C7 C8 1.509(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
N1 C9 1.340(2) . ?
N1 C10 1.460(3) . ?
N1 C11 1.462(3) . ?
C9 C5 1.496(3) . ?
C5 C6 1.345(3) . ?
C6 H6 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
