#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/08/4000870.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_4000870
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         'C17.94 H15.88 O4 S8,'F6 P1'
_chemical_formula_sum            'C17.94 H15.88 F6 O4 P S8'
_chemical_formula_weight         696.92
_chemical_name_common            (Me0.97EDO-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                   29.672(3)
_cell_length_b                   12.6090(14)
_cell_length_c                   6.9920(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2615.9(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      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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    0.0235
_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            1392
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_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    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.123
_refine_diff_density_min         -1.548
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0789
_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)+(0.1611P)²+8.3262P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2347
_refine_ls_wR_factor_ref         0.2596
_reflns_number_gt                1083
_reflns_number_total             1392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm100051b_si_002.cif
_cod_data_source_block           x=0.97
_cod_database_code               4000870
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 0.27708(6) 0.70159(15) 0.2500 0.0576(6) Uani 1 2 d S
S4 S 0.17036(7) 0.68820(16) 0.2500 0.0626(7) Uani 1 2 d S
S5 S 0.28360(6) 0.46655(14) 0.2500 0.0494(6) Uani 1 2 d S
S6 S 0.17366(6) 0.45568(15) 0.2500 0.0517(6) Uani 1 2 d S
O11 O 0.36635(19) 0.7126(4) 0.2500 0.0697(16) Uani 1 2 d S
O12 O 0.37252(17) 0.4837(5) 0.2500 0.0637(14) Uani 1 2 d S
C1 C 0.2497(2) 0.5792(5) 0.2500 0.0479(16) Uani 1 2 d S
C2 C 0.2034(3) 0.5748(5) 0.2500 0.0477(16) Uani 1 2 d S
C7 C 0.3307(2) 0.6461(6) 0.2500 0.0530(17) Uani 1 2 d S
C8 C 0.1195(3) 0.6207(7) 0.2500 0.067(2) Uani 1 2 d S
H8 H 0.0902 0.6600 0.2500 0.080 Uiso 1 2 calc SR
C9 C 0.3337(2) 0.5396(6) 0.2500 0.0517(17) Uani 1 2 d S
C10 C 0.1204(2) 0.5145(7) 0.2500 0.062(2) Uani 1 2 d S
C13 C 0.4061(4) 0.6544(10) 0.3285(17) 0.073(3) Uani 0.50 1 d P
C14 C 0.4107(3) 0.5553(8) 0.2500 0.092(3) Uani 1 2 d S
C15 C 0.0791(3) 0.4441(8) 0.2500 0.083(3) Uani 1 2 d S
H15A H 0.0887 0.3680 0.2500 0.100 Uiso 1 2 calc SR
H15B H 0.0607 0.4588 0.1332 0.100 Uiso 0.50 1 calc PR
H15C H 0.0607 0.4588 0.3668 0.100 Uiso 0.50 1 calc PR
P16 P 0.5000 0.2925(4) 0.2500 0.237(7) Uani 1 4 d S
F17 F 0.5000 0.3902(11) 0.100(2) 0.216(5) Uani 1 2 d S
F18 F 0.4489(3) 0.3013(7) 0.2500 0.243(8) Uani 1 2 d S
F19 F 0.5000 0.2296(17) 0.025(4) 0.37(3) Uani 0.50 2 d SP
F20 F 0.5000 0.1822(11) 0.2500 0.227(11) Uani 1 4 d S
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 94.1(3) . .
C8 S4 C2 95.0(4) . .
C1 S5 C9 93.5(3) . .
C2 S6 C10 95.3(4) . .
C7 O11 C13 108.3(6) . .
C7 O11 C13 108.3(6) . 10_556
C13 O11 C13 43.1(10) . 10_556
C9 O12 C14 110.0(6) . .
C2 C1 S5 123.0(5) . .
C2 C1 S3 120.2(5) . .
S5 C1 S3 116.9(4) . .
C1 C2 S4 122.1(5) . .
C1 C2 S6 122.8(5) . .
S4 C2 S6 115.2(4) . .
C9 C7 O11 124.7(6) . .
C9 C7 S3 117.5(5) . .
O11 C7 S3 117.9(6) . .
C10 C8 S4 118.3(6) . .
C10 C8 H8 120.9 . .
S4 C8 H8 120.9 . .
C7 C9 O12 125.1(7) . .
C7 C9 S5 118.1(5) . .
O12 C9 S5 116.8(6) . .
C8 C10 C15 124.8(7) . .
C8 C10 S6 116.3(6) . .
C15 C10 S6 118.9(6) . .
C13 C13 C14 66.4(5) 10_556 .
C13 C13 O11 68.4(5) 10_556 .
C14 C13 O11 112.2(8) . .
C13 C14 C13 47.2(11) 10_556 .
C13 C14 O12 119.4(8) 10_556 .
C13 C14 O12 119.4(8) . .
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 94.2(4) . 11_655
F20 P16 F18 94.2(4) . .
F18 P16 F18 171.6(8) 11_655 .
F20 P16 F17 139.5(5) . 10_556
F18 P16 F17 86.8(3) 11_655 10_556
F18 P16 F17 86.8(3) . 10_556
F20 P16 F17 139.5(5) . .
F18 P16 F17 86.8(3) 11_655 .
F18 P16 F17 86.8(3) . .
F17 P16 F17 80.9(10) 10_556 .
F20 P16 F19 63.3(9) . .
F18 P16 F19 91.89(18) 11_655 .
F18 P16 F19 91.89(18) . .
F17 P16 F19 157.2(9) 10_556 .
F17 P16 F19 76.3(10) . .
F20 P16 F19 63.3(9) . 10_556
F18 P16 F19 91.89(18) 11_655 10_556
F18 P16 F19 91.89(18) . 10_556
F17 P16 F19 76.3(10) 10_556 10_556
F17 P16 F19 157.2(9) . 10_556
F19 P16 F19 126.5(17) . 10_556
F20 F19 P16 47.6(9) . .
P16 F20 F19 69.2(8) . 10_556
P16 F20 F19 69.2(8) . .
F19 F20 F19 138.4(16) 10_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S3 C7 1.738(7) .
S3 C1 1.744(7) .
S4 C8 1.732(8) .
S4 C2 1.733(7) .
S5 C1 1.742(7) .
S5 C9 1.748(8) .
S6 C2 1.741(7) .
S6 C10 1.745(8) .
O11 C7 1.350(9) .
O11 C13 1.494(12) .
O11 C13 1.494(12) 10_556
O12 C9 1.352(9) .
O12 C14 1.448(10) .
C1 C2 1.375(11) .
C7 C9 1.345(11) .
C8 C10 1.339(12) .
C8 H8 1.0000 .
C10 C15 1.514(11) .
C13 C13 1.10(2) 10_556
C13 C14 1.372(14) .
C14 C13 1.372(14) 10_556
C15 H15A 1.0000 .
C15 H15B 1.0000 .
C15 H15C 1.0000 .
P16 F20 1.391(14) .
P16 F18 1.521(8) 11_655
P16 F18 1.521(8) .
P16 F17 1.619(15) 10_556
P16 F17 1.619(15) .
P16 F19 1.76(2) .
P16 F19 1.76(2) 10_556
F19 F20 1.68(3) .
F20 F19 1.68(3) 10_556
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
C9 S5 C1 C2 180.0 . .
C9 S5 C1 S3 0.0 . .
C7 S3 C1 C2 180.0 . .
C7 S3 C1 S5 0.0 . .
S5 C1 C2 S4 180.0 . .
S3 C1 C2 S4 0.0 . .
S5 C1 C2 S6 0.0 . .
S3 C1 C2 S6 180.0 . .
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 -22.8(5) . .
C13 O11 C7 C9 22.8(5) 10_556 .
C13 O11 C7 S3 157.2(5) . .
C13 O11 C7 S3 -157.2(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 97.5(3) . 10_556
C7 O11 C13 C14 46.3(9) . .
C13 O11 C13 C14 -51.2(9) 10_556 .
O11 C13 C14 C13 52.3(9) . 10_556
C13 C13 C14 O12 -104.2(6) 10_556 .
O11 C13 C14 O12 -51.9(10) . .
C9 O12 C14 C13 -27.3(7) . 10_556
C9 O12 C14 C13 27.3(7) . .
F18 P16 F19 F20 93.8(3) 11_655 .
F18 P16 F19 F20 -93.8(3) . .
F17 P16 F19 F20 180.000(5) 10_556 .
F17 P16 F19 F20 180.000(2) . .
F19 P16 F19 F20 0.0 10_556 .
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(2) 11_655 .
F18 P16 F20 F19 90.000(2) . .
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 .
P16 F19 F20 F19 0.000(9) . 10_556
