#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/08/4000865.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_4000865
loop_
_publ_author_name
'Murata, Tsuyoshi'
'Shao, Xiangfeng'
'Nakano, Yoshiaki'
'Yamochi, Hideki'
'Uruichi, Mikio'
'Yakushi, Kyuya'
'Saito, Gunzi'
'Tanaka, Koichiro'
_publ_section_title
;
 Tuning of Multi-Instabilities in Organic Alloy,
 [(EDO-TTF)1−x(MeEDO-TTF)x]2PF6
;
_journal_issue                   10
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3121
_journal_paper_doi               10.1021/cm100051b
_journal_volume                  22
_journal_year                    2010
_chemical_formula_moiety         'C17.82 H15.64 O4 S8, F6 P1'
_chemical_formula_sum            'C17.82 H15.64 F6 O4 P S8'
_chemical_formula_weight         695.23
_chemical_name_common            (Me0.91EDO-TTF)2PF6
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.658(4)
_cell_length_b                   12.6080(15)
_cell_length_c                   6.9900(12)
_cell_measurement_temperature    293(2)
_cell_volume                     2613.8(6)
_computing_cell_refinement       MAC-DENZO
_computing_data_collection       'DIP software (MAC Science)'
_computing_data_reduction        MAC-DENZO
_computing_molecular_graphics    'ORTEP III'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Mac Science DIP-2020K'
_diffrn_measurement_method       theta/2theta
_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    0.0415
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1412
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0734
_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)+(0.1669P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2129
_refine_ls_wR_factor_ref         0.2552
_reflns_number_gt                779
_reflns_number_total             1412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm100051b_si_002.cif
_cod_data_source_block           x=0.91
_cod_original_cell_volume        2613.8(7)
_cod_database_code               4000865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, 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
S3 S 0.27711(7) 0.70162(16) 0.2500 0.0687(7) Uani 1 2 d S
S4 S 0.17024(8) 0.68803(17) 0.2500 0.0727(8) Uani 1 2 d S
S5 S 0.28374(7) 0.46672(15) 0.2500 0.0596(7) Uani 1 2 d S
S6 S 0.17372(7) 0.45531(16) 0.2500 0.0624(7) Uani 1 2 d S
O11 O 0.36611(19) 0.7130(5) 0.2500 0.0760(17) Uani 1 2 d S
O12 O 0.37273(19) 0.4837(5) 0.2500 0.0721(16) Uani 1 2 d S
C1 C 0.2494(3) 0.5795(6) 0.2500 0.0594(19) Uani 1 2 d S
C2 C 0.2035(3) 0.5745(6) 0.2500 0.0582(19) Uani 1 2 d S
C7 C 0.3307(3) 0.6454(6) 0.2500 0.064(2) Uani 1 2 d S
C8 C 0.1201(3) 0.6191(7) 0.2500 0.081(3) Uani 1 2 d S
H8 H 0.0928 0.6554 0.2500 0.097 Uiso 1 2 calc SR
C9 C 0.3333(3) 0.5403(7) 0.2500 0.063(2) Uani 1 2 d S
C10 C 0.1206(3) 0.5135(7) 0.2500 0.074(2) Uani 1 2 d S
C13 C 0.4058(4) 0.6559(11) 0.328(2) 0.097(7) Uani 0.50 1 d P
C14 C 0.4112(3) 0.5557(8) 0.2500 0.099(4) Uani 1 2 d S
C15 C 0.0793(4) 0.4443(9) 0.2500 0.088(3) Uani 0.91 2 d SP
H15A H 0.0883 0.3711 0.2500 0.105 Uiso 0.91 2 calc SPR
H15B H 0.0617 0.4588 0.1379 0.105 Uiso 0.45 1 calc PR
H15C H 0.0617 0.4588 0.3621 0.105 Uiso 0.45 1 calc PR
P16 P 0.5000 0.2931(5) 0.2500 0.241(7) Uani 1 4 d S
F17 F 0.5000 0.1820(11) 0.2500 0.270(13) Uani 1 4 d S
F18 F 0.5000 0.3903(11) 0.099(2) 0.228(5) Uani 1 2 d S
F19 F 0.4489(3) 0.3020(8) 0.2500 0.246(7) Uani 1 2 d S
F20 F 0.5000 0.2348(17) 0.032(5) 0.42(3) Uani 0.50 2 d SP
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'
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'
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
C7 S3 C1 94.0(4) . .
C8 S4 C2 94.3(4) . .
C9 S5 C1 93.4(4) . .
C10 S6 C2 95.4(4) . .
C7 O11 C13 108.1(7) . .
C7 O11 C13 108.1(7) . 10_556
C13 O11 C13 42.9(12) . 10_556
C9 O12 C14 110.1(7) . .
C2 C1 S3 120.7(6) . .
C2 C1 S5 122.9(6) . .
S3 C1 S5 116.3(5) . .
C1 C2 S4 121.9(6) . .
C1 C2 S6 123.1(6) . .
S4 C2 S6 115.0(5) . .
C9 C7 O11 125.7(8) . .
C9 C7 S3 117.4(6) . .
O11 C7 S3 116.9(6) . .
C10 C8 S4 119.5(7) . .
C7 C9 O12 124.8(8) . .
C7 C9 S5 118.8(6) . .
O12 C9 S5 116.4(6) . .
C8 C10 C15 124.7(9) . .
C8 C10 S6 115.7(7) . .
C15 C10 S6 119.5(7) . .
C13 C13 C14 66.9(6) 10_556 .
C13 C13 O11 68.5(6) 10_556 .
C14 C13 O11 113.1(10) . .
C13 C14 C13 46.1(13) . 10_556
C13 C14 O12 118.5(9) . .
C13 C14 O12 118.5(9) 10_556 .
F17 P16 F19 94.2(4) . .
F17 P16 F19 94.2(4) . 11_655
F19 P16 F19 171.5(8) . 11_655
F17 P16 F18 139.3(5) . 10_556
F19 P16 F18 86.8(3) . 10_556
F19 P16 F18 86.8(3) 11_655 10_556
F17 P16 F18 139.3(5) . .
F19 P16 F18 86.8(3) . .
F19 P16 F18 86.8(3) 11_655 .
F18 P16 F18 81.3(10) 10_556 .
F17 P16 F20 64.2(9) . .
F19 P16 F20 91.84(18) . .
F19 P16 F20 91.84(18) 11_655 .
F18 P16 F20 156.5(9) 10_556 .
F18 P16 F20 75.1(10) . .
F17 P16 F20 64.2(9) . 10_556
F19 P16 F20 91.84(18) . 10_556
F19 P16 F20 91.84(18) 11_655 10_556
F18 P16 F20 75.1(10) 10_556 10_556
F18 P16 F20 156.5(9) . 10_556
F20 P16 F20 128.4(17) . 10_556
P16 F17 F20 66.3(9) . 10_556
P16 F17 F20 66.3(9) . .
F20 F17 F20 132.7(18) 10_556 .
F17 F20 P16 49.5(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S3 C7 1.740(8) .
S3 C1 1.745(8) .
S4 C8 1.723(9) .
S4 C2 1.738(8) .
S5 C9 1.739(9) .
S5 C1 1.749(8) .
S6 C10 1.737(9) .
S6 C2 1.743(8) .
O11 C7 1.352(9) .
O11 C13 1.482(13) .
O11 C13 1.482(13) 10_556
O12 C9 1.368(9) .
O12 C14 1.458(11) .
C1 C2 1.364(13) .
C7 C9 1.328(11) .
C8 C10 1.331(13) .
C10 C15 1.504(13) .
C13 C13 1.08(3) 10_556
C13 C14 1.383(15) .
C14 C13 1.383(15) 10_556
P16 F17 1.402(15) .
P16 F19 1.518(9) .
P16 F19 1.518(9) 11_655
P16 F18 1.615(14) 10_556
P16 F18 1.615(14) .
P16 F20 1.69(3) .
P16 F20 1.69(3) 10_556
F17 F20 1.66(3) 10_556
F17 F20 1.66(3) .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C7 S3 C1 C2 180.0 . .
C7 S3 C1 S5 0.0 . .
C9 S5 C1 C2 180.0 . .
C9 S5 C1 S3 0.0 . .
S3 C1 C2 S4 0.0 . .
S5 C1 C2 S4 180.0 . .
S3 C1 C2 S6 180.0 . .
S5 C1 C2 S6 0.0 . .
C8 S4 C2 C1 180.0 . .
C8 S4 C2 S6 0.0 . .
C10 S6 C2 C1 180.0 . .
C10 S6 C2 S4 0.0 . .
C13 O11 C7 C9 -22.6(6) . .
C13 O11 C7 C9 22.6(6) 10_556 .
C13 O11 C7 S3 157.4(6) . .
C13 O11 C7 S3 -157.4(6) 10_556 .
C1 S3 C7 C9 0.0 . .
C1 S3 C7 O11 180.0 . .
C2 S4 C8 C10 0.0 . .
O11 C7 C9 O12 0.0 . .
S3 C7 C9 O12 180.0 . .
O11 C7 C9 S5 180.0 . .
S3 C7 C9 S5 0.0 . .
C14 O12 C9 C7 0.0 . .
C14 O12 C9 S5 180.0 . .
C1 S5 C9 C7 0.0 . .
C1 S5 C9 O12 180.0 . .
S4 C8 C10 C15 180.0 . .
S4 C8 C10 S6 0.0 . .
C2 S6 C10 C8 0.0 . .
C2 S6 C10 C15 180.0 . .
C7 O11 C13 C13 97.4(4) . 10_556
C7 O11 C13 C14 46.1(11) . .
C13 O11 C13 C14 -51.3(11) 10_556 .
O11 C13 C14 C13 52.1(11) . 10_556
C13 C13 C14 O12 -103.3(6) 10_556 .
O11 C13 C14 O12 -51.2(12) . .
C9 O12 C14 C13 26.5(8) . .
C9 O12 C14 C13 -26.5(8) . 10_556
F19 P16 F17 F20 -90.000(4) . 10_556
F19 P16 F17 F20 90.000(4) 11_655 10_556
F18 P16 F17 F20 0.000(4) 10_556 10_556
F18 P16 F17 F20 180.000(5) . 10_556
F20 P16 F17 F20 180.000(5) . 10_556
F19 P16 F17 F20 90.000(3) . .
F19 P16 F17 F20 -90.000(3) 11_655 .
F18 P16 F17 F20 180.000(3) 10_556 .
F18 P16 F17 F20 0.000(3) . .
F20 P16 F17 F20 180.000(3) 10_556 .
F20 F17 F20 P16 0.000(1) 10_556 .
F19 P16 F20 F17 -93.8(4) . .
F19 P16 F20 F17 93.8(4) 11_655 .
F18 P16 F20 F17 180.000(9) 10_556 .
F18 P16 F20 F17 180.000(2) . .
F20 P16 F20 F17 0.0 10_556 .
