#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/08/4000869.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_4000869
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                   29.313(12)
_cell_length_b                   12.572(7)
_cell_length_c                   6.8180(19)
_cell_measurement_temperature    110(2)
_cell_volume                     2512.6(19)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.831
_diffrn_measured_fraction_theta_max 0.831
_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    0.1213
_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            2084
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.840
_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         0.450
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.0640
_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)+(0.0945P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.2030
_reflns_number_gt                880
_reflns_number_total             2084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm100051b_si_002.cif
_cod_data_source_block           x=0.94_110K
_cod_database_code               4000869
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 0.22237(7) 0.2014(2) 0.1766(3) 0.0417(6) Uani 1 1 d .
S4 S 0.33090(7) 0.1862(2) 0.1560(4) 0.0420(6) Uani 1 1 d .
S5 S 0.21511(7) -0.0351(2) 0.1798(3) 0.0402(6) Uani 1 1 d .
S6 S 0.32697(7) -0.0481(2) 0.1565(3) 0.0402(6) Uani 1 1 d .
O11 O 0.13187(17) 0.2148(5) 0.1991(8) 0.0423(16) Uani 1 1 d .
O12 O 0.12453(18) -0.0175(5) 0.1978(8) 0.0421(16) Uani 1 1 d .
C1 C 0.2496(3) 0.0768(8) 0.1686(13) 0.041(2) Uani 1 1 d .
C2 C 0.2966(3) 0.0737(8) 0.1591(11) 0.038(2) Uani 1 1 d .
C7 C 0.1682(3) 0.1453(8) 0.1872(12) 0.037(2) Uani 1 1 d .
C8 C 0.3822(3) 0.1166(8) 0.1390(12) 0.044(2) Uani 1 1 d .
H8 H 0.4118 0.1556 0.1300 0.052 Uiso 1 1 calc R
C9 C 0.1645(3) 0.0406(8) 0.1917(13) 0.040(2) Uani 1 1 d .
C10 C 0.3813(3) 0.0107(8) 0.1383(12) 0.039(2) Uani 1 1 d .
C13 C 0.0913(3) 0.1585(8) 0.2660(13) 0.043(2) Uani 1 1 d .
H13A H 0.0637 0.2037 0.2429 0.052 Uiso 1 1 calc R
H13B H 0.0937 0.1448 0.4101 0.052 Uiso 1 1 calc R
C14 C 0.0859(3) 0.0528(8) 0.1574(14) 0.048(2) Uani 1 1 d .
H14A H 0.0569 0.0175 0.1998 0.058 Uiso 1 1 calc R
H14B H 0.0839 0.0664 0.0131 0.058 Uiso 1 1 calc R
C15 C 0.4231(3) -0.0593(8) 0.1299(13) 0.047(2) Uani 1 1 d .
H15A H 0.4136 -0.1356 0.1335 0.056 Uiso 1 1 calc R
H15B H 0.4432 -0.0436 0.2449 0.056 Uiso 1 1 calc R
H15C H 0.4402 -0.0449 0.0058 0.056 Uiso 1 1 calc R
P16 P 0.0000 0.2100(4) -0.2500 0.0503(10) Uani 1 2 d S
F17 F 0.0070(2) 0.2997(6) -0.4119(11) 0.092(2) Uani 1 1 d .
F18 F -0.05405(15) 0.2095(5) -0.2933(8) 0.0587(16) Uani 1 1 d .
F19 F 0.00625(19) 0.1212(6) -0.4137(8) 0.0697(19) 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 93.1(4) . .
C2 S4 C8 95.2(4) . .
C1 S5 C9 93.2(4) . .
C10 S6 C2 95.3(4) . .
C7 O11 C13 109.9(7) . .
C9 O12 C14 109.4(7) . .
C2 C1 S5 124.2(7) . .
C2 C1 S3 118.7(7) . .
S5 C1 S3 117.1(5) . .
C1 C2 S4 123.8(7) . .
C1 C2 S6 121.7(7) . .
S4 C2 S6 114.5(5) . .
C9 C7 O11 124.4(8) . .
C9 C7 S3 118.8(7) . .
O11 C7 S3 116.7(7) . .
C10 C8 S4 119.0(7) . .
C10 C8 H8 120.5 . .
S4 C8 H8 120.5 . .
C7 C9 O12 126.8(8) . .
C7 C9 S5 117.7(6) . .
O12 C9 S5 115.4(7) . .
C8 C10 C15 124.5(8) . .
C8 C10 S6 115.9(7) . .
C15 C10 S6 119.5(7) . .
O11 C13 C14 110.8(7) . .
O11 C13 H13A 109.5 . .
C14 C13 H13A 109.5 . .
O11 C13 H13B 109.5 . .
C14 C13 H13B 109.5 . .
H13A C13 H13B 108.1 . .
O12 C14 C13 110.7(7) . .
O12 C14 H14A 109.5 . .
C13 C14 H14A 109.5 . .
O12 C14 H14B 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 108.1 . .
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 . .
F19 P16 F19 90.7(6) . 4_554
F19 P16 F17 179.0(4) . 4_554
F19 P16 F17 89.8(4) 4_554 4_554
F19 P16 F17 89.8(4) . .
F19 P16 F17 179.0(4) 4_554 .
F17 P16 F17 89.8(7) 4_554 .
F19 P16 F18 90.7(3) . 4_554
F19 P16 F18 89.0(3) 4_554 4_554
F17 P16 F18 90.2(3) 4_554 4_554
F17 P16 F18 90.2(3) . 4_554
F19 P16 F18 89.0(3) . .
F19 P16 F18 90.7(3) 4_554 .
F17 P16 F18 90.2(3) 4_554 .
F17 P16 F18 90.2(3) . .
F18 P16 F18 179.5(6) 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 1.738(8) .
S3 C1 1.760(9) .
S4 C2 1.734(10) .
S4 C8 1.743(9) .
S5 C1 1.735(10) .
S5 C9 1.765(9) .
S6 C10 1.760(9) .
S6 C2 1.771(9) .
O11 C7 1.381(10) .
O11 C13 1.458(10) .
O12 C9 1.380(9) .
O12 C14 1.464(10) .
C1 C2 1.380(11) .
C7 C9 1.321(13) .
C8 C10 1.332(13) .
C8 H8 1.0000 .
C10 C15 1.509(12) .
C13 C14 1.529(13) .
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 F19 1.589(7) .
P16 F19 1.589(7) 4_554
P16 F17 1.591(7) 4_554
P16 F17 1.591(7) .
P16 F18 1.612(5) 4_554
P16 F18 1.612(4) .
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 179.0(8)
C9 S5 C1 S3 0.8(6)
C7 S3 C1 C2 -179.8(8)
C7 S3 C1 S5 -1.5(6)
S5 C1 C2 S4 -177.8(5)
S3 C1 C2 S4 0.4(11)
S5 C1 C2 S6 0.3(11)
S3 C1 C2 S6 178.4(4)
C8 S4 C2 C1 -179.0(8)
C8 S4 C2 S6 2.8(5)
C10 S6 C2 C1 178.8(7)
C10 S6 C2 S4 -3.0(5)
C13 O11 C7 C9 14.3(12)
C13 O11 C7 S3 -162.8(6)
C1 S3 C7 C9 1.9(8)
C1 S3 C7 O11 179.1(7)
C2 S4 C8 C10 -1.5(8)
O11 C7 C9 O12 3.8(16)
S3 C7 C9 O12 -179.2(7)
O11 C7 C9 S5 -178.7(6)
S3 C7 C9 S5 -1.7(11)
C14 O12 C9 C7 11.8(13)
C14 O12 C9 S5 -165.8(6)
C1 S5 C9 C7 0.5(9)
C1 S5 C9 O12 178.3(7)
S4 C8 C10 C15 -178.2(6)
S4 C8 C10 S6 -0.4(10)
C2 S6 C10 C8 2.0(8)
C2 S6 C10 C15 180.0(7)
C7 O11 C13 C14 -45.2(10)
C9 O12 C14 C13 -42.6(9)
O11 C13 C14 O12 62.4(10)
