#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/08/4000868.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_4000868
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           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   29.396(3)
_cell_length_b                   12.5640(18)
_cell_length_c                   6.9060(5)
_cell_measurement_temperature    200(2)
_cell_volume                     2550.6(5)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.873
_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    0.0345
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2254
_diffrn_reflns_theta_full        26.23
_diffrn_reflns_theta_max         26.23
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.813
_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         0.667
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0501
_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)+(0.0808P)²+2.4190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                1664
_reflns_number_total             2254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm100051b_si_002.cif
_cod_data_source_block           x=0.94_200K
_cod_database_code               4000868
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
S3 S 0.22276(3) 0.20134(10) 0.16557(17) 0.0398(3) Uani 1 1 d .
S4 S 0.33062(4) 0.18736(10) 0.14898(16) 0.0413(3) Uani 1 1 d .
S5 S 0.21609(3) -0.03488(9) 0.16611(15) 0.0355(3) Uani 1 1 d .
S6 S 0.32698(3) -0.04611(9) 0.14784(15) 0.0363(3) Uani 1 1 d .
O11 O 0.13282(9) 0.2133(3) 0.1862(4) 0.0439(8) Uani 1 1 d .
O12 O 0.12611(9) -0.0179(3) 0.1796(4) 0.0416(7) Uani 1 1 d .
C1 C 0.25049(13) 0.0782(4) 0.1597(6) 0.0344(9) Uani 1 1 d .
C2 C 0.29699(14) 0.0736(4) 0.1523(5) 0.0341(9) Uani 1 1 d .
C7 C 0.16882(13) 0.1448(4) 0.1742(6) 0.0369(10) Uani 1 1 d .
C8 C 0.38148(14) 0.1193(4) 0.1351(6) 0.0431(11) Uani 1 1 d .
H8 H 0.4109 0.1590 0.1266 0.052 Uiso 1 1 calc R
C9 C 0.16564(13) 0.0385(4) 0.1750(6) 0.0361(10) Uani 1 1 d .
C10 C 0.38107(13) 0.0131(4) 0.1360(6) 0.0381(10) Uani 1 1 d .
C13 C 0.09250(14) 0.1558(4) 0.2506(7) 0.0460(11) Uani 1 1 d .
H13A H 0.0648 0.2006 0.2291 0.055 Uiso 1 1 calc R
H13B H 0.0949 0.1404 0.3922 0.055 Uiso 1 1 calc R
C14 C 0.08807(14) 0.0532(4) 0.1400(7) 0.0462(11) Uani 1 1 d .
H14A H 0.0590 0.0173 0.1769 0.055 Uiso 1 1 calc R
H14B H 0.0869 0.0689 -0.0019 0.055 Uiso 1 1 calc R
C15 C 0.42235(16) -0.0576(4) 0.1316(7) 0.0512(12) Uani 1 1 d .
H15A H 0.4126 -0.1338 0.1331 0.061 Uiso 1 1 calc R
H15B H 0.4417 -0.0428 0.2476 0.061 Uiso 1 1 calc R
H15C H 0.4402 -0.0432 0.0112 0.061 Uiso 1 1 calc R
P16 P 0.0000 0.21104(18) -0.2500 0.0546(5) Uani 1 2 d S
F17 F 0.00612(16) 0.2959(5) -0.4053(10) 0.204(4) Uani 1 1 d .
F18 F -0.05327(9) 0.2097(3) -0.2901(5) 0.0833(12) Uani 1 1 d .
F19 F 0.00508(14) 0.1231(5) -0.4050(7) 0.154(3) Uani 1 1 d .
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 93.7(2) . .
C8 S4 C2 94.9(2) . .
C1 S5 C9 93.6(2) . .
C2 S6 C10 95.3(2) . .
C7 O11 C13 109.6(4) . .
C9 O12 C14 109.3(4) . .
C2 C1 S5 123.0(3) . .
C2 C1 S3 120.3(3) . .
S5 C1 S3 116.7(2) . .
C1 C2 S4 122.2(3) . .
C1 C2 S6 122.8(3) . .
S4 C2 S6 114.9(2) . .
C9 C7 O11 125.1(4) . .
C9 C7 S3 118.1(3) . .
O11 C7 S3 116.8(4) . .
C10 C8 S4 119.2(3) . .
C10 C8 H8 120.4 . .
S4 C8 H8 120.4 . .
C7 C9 O12 125.4(4) . .
C7 C9 S5 117.9(3) . .
O12 C9 S5 116.7(3) . .
C8 C10 C15 125.7(4) . .
C8 C10 S6 115.6(3) . .
C15 C10 S6 118.7(4) . .
O11 C13 C14 109.9(4) . .
O11 C13 H13A 109.7 . .
C14 C13 H13A 109.7 . .
O11 C13 H13B 109.7 . .
C14 C13 H13B 109.7 . .
H13A C13 H13B 108.2 . .
O12 C14 C13 111.3(4) . .
O12 C14 H14A 109.4 . .
C13 C14 H14A 109.4 . .
O12 C14 H14B 109.4 . .
C13 C14 H14B 109.4 . .
H14A C14 H14B 108.0 . .
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 . .
F17 P16 F17 91.1(7) 4_554 .
F17 P16 F19 178.4(4) 4_554 .
F17 P16 F19 90.1(4) . .
F17 P16 F19 90.1(4) 4_554 4_554
F17 P16 F19 178.4(4) . 4_554
F19 P16 F19 88.7(5) . 4_554
F17 P16 F18 90.1(2) 4_554 4_554
F17 P16 F18 90.8(2) . 4_554
F19 P16 F18 91.0(2) . 4_554
F19 P16 F18 88.1(2) 4_554 4_554
F17 P16 F18 90.8(2) 4_554 .
F17 P16 F18 90.1(2) . .
F19 P16 F18 88.1(2) . .
F19 P16 F18 91.0(2) 4_554 .
F18 P16 F18 178.8(3) 4_554 .
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(4) .
S3 C1 1.749(4) .
S4 C8 1.725(5) .
S4 C2 1.738(4) .
S5 C1 1.745(4) .
S5 C9 1.747(4) .
S6 C2 1.743(5) .
S6 C10 1.758(4) .
O11 C7 1.367(5) .
O11 C13 1.458(5) .
O12 C9 1.362(5) .
O12 C14 1.457(5) .
C1 C2 1.369(6) .
C7 C9 1.338(7) .
C8 C10 1.335(7) .
C8 H8 1.0000 .
C10 C15 1.504(6) .
C13 C14 1.504(7) .
C13 H13A 1.0000 .
C13 H13B 1.0000 .
C14 H14A 1.0000 .
C14 H14B 1.0000 .
C15 H15A 1.0000 .
C15 H15B 1.0000 .
C15 H15C 1.0000 .
P16 F17 1.523(5) 4_554
P16 F17 1.523(5) .
P16 F19 1.546(4) .
P16 F19 1.546(4) 4_554
P16 F18 1.590(3) 4_554
P16 F18 1.590(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
C9 S5 C1 C2 179.7(3)
C9 S5 C1 S3 0.3(3)
C7 S3 C1 C2 -179.9(3)
C7 S3 C1 S5 -0.4(3)
S5 C1 C2 S4 -179.2(2)
S3 C1 C2 S4 0.2(5)
S5 C1 C2 S6 0.1(5)
S3 C1 C2 S6 179.5(2)
C8 S4 C2 C1 -179.0(3)
C8 S4 C2 S6 1.7(3)
C10 S6 C2 C1 179.3(3)
C10 S6 C2 S4 -1.3(3)
C13 O11 C7 C9 14.9(6)
C13 O11 C7 S3 -162.8(3)
C1 S3 C7 C9 0.4(4)
C1 S3 C7 O11 178.3(3)
C2 S4 C8 C10 -1.6(4)
O11 C7 C9 O12 2.9(7)
S3 C7 C9 O12 -179.4(3)
O11 C7 C9 S5 -178.0(3)
S3 C7 C9 S5 -0.3(5)
C14 O12 C9 C7 12.6(6)
C14 O12 C9 S5 -166.5(3)
C1 S5 C9 C7 0.0(4)
C1 S5 C9 O12 179.2(3)
S4 C8 C10 C15 -177.8(3)
S4 C8 C10 S6 0.9(5)
C2 S6 C10 C8 0.2(4)
C2 S6 C10 C15 179.1(3)
C7 O11 C13 C14 -45.7(5)
C9 O12 C14 C13 -44.3(5)
O11 C13 C14 O12 63.8(5)
