#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/08/4000866.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_4000866
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         'C17.88 H15.76 O4 S8, F6 P1'
_chemical_formula_sum            'C17.88 H15.76 F6 O4 P S8'
_chemical_formula_weight         696.07
_chemical_name_common            (Me0.94EDO-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                   29.662(3)
_cell_length_b                   12.6150(13)
_cell_length_c                   6.9940(5)
_cell_measurement_temperature    300(2)
_cell_volume                     2617.1(4)
_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      300(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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    0.0262
_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            1447
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.30
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.813
_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             1408
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0696
_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)+(0.1195P)²+7.7959P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2183
_reflns_number_gt                1072
_reflns_number_total             1447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm100051b_si_002.cif
_cod_data_source_block           x=0.94_300K
_cod_database_code               4000866
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 0.27705(6) 0.70145(13) 0.2500 0.0600(6) Uani 1 2 d S
S4 S 0.17031(6) 0.68780(14) 0.2500 0.0649(6) Uani 1 2 d S
S5 S 0.28366(6) 0.46660(12) 0.2500 0.0516(5) Uani 1 2 d S
S6 S 0.17371(6) 0.45548(13) 0.2500 0.0543(5) Uani 1 2 d S
O11 O 0.36614(16) 0.7129(4) 0.2500 0.0708(14) Uani 1 2 d S
O12 O 0.37277(15) 0.4838(4) 0.2500 0.0648(13) Uani 1 2 d S
C1 C 0.2496(2) 0.5793(4) 0.2500 0.0486(14) Uani 1 2 d S
C2 C 0.2034(2) 0.5746(5) 0.2500 0.0490(14) Uani 1 2 d S
C7 C 0.3307(2) 0.6457(5) 0.2500 0.0540(15) Uani 1 2 d S
C8 C 0.1198(2) 0.6201(6) 0.2500 0.071(2) Uani 1 2 d S
H8 H 0.0905 0.6595 0.2500 0.085 Uiso 1 2 calc SR
C9 C 0.3337(2) 0.5399(5) 0.2500 0.0539(15) Uani 1 2 d S
C10 C 0.1204(2) 0.5139(6) 0.2500 0.0651(18) Uani 1 2 d S
C13 C 0.4060(3) 0.6558(9) 0.3294(17) 0.079(4) Uani 0.50 1 d P
C14 C 0.4111(3) 0.5559(7) 0.2500 0.097(3) Uani 1 2 d S
C15 C 0.0792(3) 0.4437(7) 0.2500 0.085(3) Uani 1 2 d S
H15A H 0.0887 0.3677 0.2500 0.102 Uiso 1 2 calc SR
H15B H 0.0607 0.4585 0.1333 0.102 Uiso 0.50 1 calc PR
H15C H 0.0607 0.4585 0.3667 0.102 Uiso 0.50 1 calc PR
P16 P 0.5000 0.2931(4) 0.2500 0.224(6) Uani 1 4 d S
F17 F 0.5000 0.3903(10) 0.0999(18) 0.216(5) Uani 1 2 d S
F20 F 0.5000 0.1824(10) 0.2500 0.253(11) Uani 1 4 d S
F18 F 0.4488(2) 0.3015(7) 0.2500 0.238(7) Uani 1 2 d S
F19 F 0.5000 0.2339(16) 0.030(4) 0.38(2) 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(3) . .
C8 S4 C2 94.8(3) . .
C1 S5 C9 93.5(3) . .
C2 S6 C10 95.4(3) . .
C7 O11 C13 108.3(6) . .
C7 O11 C13 108.3(6) . 10_556
C13 O11 C13 43.7(9) . 10_556
C9 O12 C14 109.9(6) . .
C2 C1 S3 120.3(4) . .
C2 C1 S5 122.9(5) . .
S3 C1 S5 116.7(4) . .
C1 C2 S4 122.0(5) . .
C1 C2 S6 122.8(5) . .
S4 C2 S6 115.2(4) . .
C9 C7 O11 125.0(6) . .
C9 C7 S3 117.7(5) . .
O11 C7 S3 117.3(5) . .
C10 C8 S4 118.9(5) . .
C10 C8 H8 120.5 . .
S4 C8 H8 120.5 . .
C7 C9 O12 125.3(6) . .
C7 C9 S5 118.1(5) . .
O12 C9 S5 116.6(5) . .
C8 C10 C15 125.1(7) . .
C8 C10 S6 115.7(5) . .
C15 C10 S6 119.1(6) . .
C13 C13 C14 66.4(5) 10_556 .
C13 C13 O11 68.2(5) 10_556 .
C14 C13 O11 112.1(8) . .
C13 C14 C13 47.2(10) 10_556 .
C13 C14 O12 118.9(7) 10_556 .
C13 C14 O12 118.9(7) . .
C10 C15 H15A 109.5 . .
C10 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C10 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
F20 P16 F18 94.0(4) . 11_655
F20 P16 F18 94.0(4) . .
F18 P16 F18 172.0(7) 11_655 .
F20 P16 F17 139.4(4) . 10_556
F18 P16 F17 87.0(3) 11_655 10_556
F18 P16 F17 87.0(3) . 10_556
F20 P16 F17 139.4(4) . .
F18 P16 F17 87.0(3) 11_655 .
F18 P16 F17 87.0(3) . .
F17 P16 F17 81.1(9) 10_556 .
F20 P16 F19 64.1(8) . .
F18 P16 F19 91.74(16) 11_655 .
F18 P16 F19 91.74(16) . .
F17 P16 F19 156.5(9) 10_556 .
F17 P16 F19 75.3(9) . .
F20 P16 F19 64.1(8) . 10_556
F18 P16 F19 91.74(16) 11_655 10_556
F18 P16 F19 91.74(16) . 10_556
F17 P16 F19 75.3(9) 10_556 10_556
F17 P16 F19 156.5(9) . 10_556
F19 P16 F19 128.2(16) . 10_556
P16 F20 F19 67.1(8) . 10_556
P16 F20 F19 67.1(8) . .
F19 F20 F19 134.3(15) 10_556 .
F20 F19 P16 48.8(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S3 C7 1.739(6) .
S3 C1 1.743(6) .
S4 C8 1.725(8) .
S4 C2 1.732(6) .
S5 C1 1.744(6) .
S5 C9 1.749(7) .
S6 C2 1.742(6) .
S6 C10 1.745(7) .
O11 C7 1.351(8) .
O11 C13 1.492(11) .
O11 C13 1.492(11) 10_556
O12 C9 1.358(8) .
O12 C14 1.457(9) .
C1 C2 1.372(10) .
C7 C9 1.338(9) .
C8 C10 1.340(11) .
C8 H8 1.0000 .
C10 C15 1.509(10) .
C13 C13 1.11(2) 10_556
C13 C14 1.386(13) .
C14 C13 1.386(13) 10_556
C15 H15A 1.0000 .
C15 H15B 1.0000 .
C15 H15C 1.0000 .
P16 F20 1.396(13) .
P16 F18 1.522(7) 11_655
P16 F18 1.522(7) .
P16 F17 1.614(13) 10_556
P16 F17 1.614(13) .
P16 F19 1.71(3) .
P16 F19 1.71(3) 10_556
F20 F19 1.67(3) 10_556
F20 F19 1.67(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 -23.1(5) . .
C13 O11 C7 C9 23.1(5) 10_556 .
C13 O11 C7 S3 156.9(5) . .
C13 O11 C7 S3 -156.9(5) 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 97.6(3) . 10_556
C7 O11 C13 C14 46.6(9) . .
C13 O11 C13 C14 -51.1(8) 10_556 .
O11 C13 C14 C13 52.0(8) . 10_556
C13 C13 C14 O12 -104.0(5) 10_556 .
O11 C13 C14 O12 -52.0(9) . .
C9 O12 C14 C13 -27.2(6) . 10_556
C9 O12 C14 C13 27.2(6) . .
F18 P16 F20 F19 90.000(3) 11_655 10_556
F18 P16 F20 F19 -90.000(3) . 10_556
F17 P16 F20 F19 0.000(4) 10_556 10_556
F17 P16 F20 F19 180.000(4) . 10_556
F19 P16 F20 F19 180.000(4) . 10_556
F18 P16 F20 F19 -90.000(3) 11_655 .
F18 P16 F20 F19 90.000(3) . .
F17 P16 F20 F19 180.000(2) 10_556 .
F17 P16 F20 F19 0.000(2) . .
F19 P16 F20 F19 180.000(2) 10_556 .
F19 F20 F19 P16 0.000(1) 10_556 .
F18 P16 F19 F20 93.6(3) 11_655 .
F18 P16 F19 F20 -93.6(3) . .
F17 P16 F19 F20 180.000(7) 10_556 .
F17 P16 F19 F20 180.000(2) . .
F19 P16 F19 F20 0.0 10_556 .
