#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:37:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179193 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/34/4313408.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_4313408
loop_
_publ_author_name
'Fatima Setifi'
'Lahcène Ouahab'
'Stéphane Golhen'
'Yukihiro Yoshida'
'Gunzi Saito'
_publ_section_title
;
 First Radical Cation Salt of Paramagnetic Transition Metal Complex
 Containing TTF as Ligand, [CuII(hfac)2(TTF-py)2](PF6).2CH2Cl2 (hfac =
 Hexafluoroacetylacetonate and TTF-py =
 4-(2-Tetrathiafulvalenyl-ethenyl)pyridine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1791
_journal_page_last               1793
_journal_paper_doi               10.1021/ic026211h
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C38 H26 Cl4 Cu F18 N2 O4 P S8'
_chemical_formula_weight         1409.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.695(2)
_cell_angle_beta                 91.419(2)
_cell_angle_gamma                97.7194(19)
_cell_formula_units_Z            1
_cell_length_a                   9.6998(5)
_cell_length_b                   10.2050(5)
_cell_length_c                   14.4317(8)
_cell_measurement_reflns_used    5794
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1360.02(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0889
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10692
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             702
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0819
_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)+(0.1429P)²+0.4696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2708
_reflns_number_gt                3245
_reflns_number_total             6199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026211hsi20030110_053742.cif
_cod_data_source_block           val
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1789(7) 0.1867(6) -0.0532(4) 0.0630(15) Uani 1 1 d . . .
H1 H -0.1698 0.2315 0.0140 0.076 Uiso 1 1 calc R . .
C2 C -0.2579(7) 0.2347(6) -0.1107(4) 0.0644(15) Uani 1 1 d . . .
H2 H -0.3026 0.3123 -0.0834 0.077 Uiso 1 1 calc R . .
C3 C -0.2758(6) 0.1719(6) -0.2108(4) 0.0572(14) Uani 1 1 d . . .
C4 C -0.2042(6) 0.0594(6) -0.2446(4) 0.0596(14) Uani 1 1 d . . .
H4 H -0.2111 0.0121 -0.3113 0.071 Uiso 1 1 calc R . .
C5 C -0.1258(6) 0.0186(6) -0.1825(4) 0.0614(15) Uani 1 1 d . . .
H5 H -0.0773 -0.0569 -0.2081 0.074 Uiso 1 1 calc R . .
C6 C -0.3634(7) 0.2226(6) -0.2737(4) 0.0614(15) Uani 1 1 d . . .
H6 H -0.4155 0.2935 -0.2440 0.074 Uiso 1 1 calc R . .
C7 C -0.3753(6) 0.1759(6) -0.3702(4) 0.0576(14) Uani 1 1 d . . .
H7 H -0.3228 0.1052 -0.3992 0.069 Uiso 1 1 calc R . .
C8 C -0.4601(6) 0.2234(6) -0.4333(4) 0.0559(13) Uani 1 1 d . . .
C9 C -0.4672(6) 0.1782(6) -0.5295(4) 0.0603(14) Uani 1 1 d . . .
H9 H -0.4156 0.1079 -0.5610 0.072 Uiso 1 1 calc R . .
C10 C -0.6277(6) 0.3607(6) -0.4962(4) 0.0582(14) Uani 1 1 d . . .
C11 C -0.7186(6) 0.4500(6) -0.5028(4) 0.0571(13) Uani 1 1 d . . .
C12 C -0.8694(7) 0.6037(7) -0.5575(7) 0.082(2) Uani 1 1 d . . .
H12 H -0.9199 0.6463 -0.5955 0.099 Uiso 1 1 calc R . .
C13 C -0.8616(7) 0.6481(7) -0.4643(6) 0.0770(19) Uani 1 1 d . . .
H13 H -0.9050 0.7244 -0.4319 0.092 Uiso 1 1 calc R . .
C14 C -0.2542(7) -0.0055(6) 0.1046(4) 0.0619(15) Uani 1 1 d . . .
C15 C -0.3284(8) -0.1224(7) 0.0418(5) 0.0798(19) Uani 1 1 d . . .
H15A H -0.4077 -0.0921 0.0128 0.096 Uiso 1 1 calc R . .
H15B H -0.3690 -0.1805 0.0821 0.096 Uiso 1 1 calc R . .
C16 C -0.2698(8) -0.2097(6) -0.0343(5) 0.0653(16) Uani 1 1 d . . .
C17 C -0.3702(12) -0.3321(10) -0.0985(7) 0.105(3) Uani 1 1 d . . .
C18 C -0.3300(12) 0.0763(11) 0.1881(8) 0.115(3) Uani 1 1 d . . .
S1 S -0.57045(18) 0.24869(17) -0.59547(11) 0.0660(4) Uani 1 1 d . . .
S2 S -0.56282(18) 0.35165(17) -0.38521(11) 0.0649(4) Uani 1 1 d . . .
S3 S -0.78568(19) 0.46424(19) -0.61196(13) 0.0734(5) Uani 1 1 d . . .
S4 S -0.76962(19) 0.56350(18) -0.40154(13) 0.0732(5) Uani 1 1 d . . .
N1 N -0.1114(5) 0.0770(5) -0.0872(3) 0.0580(12) Uani 1 1 d . . .
O1 O -0.1327(4) 0.0463(4) 0.1037(3) 0.0633(10) Uani 1 1 d . . .
O2 O -0.1503(5) -0.2014(4) -0.0566(3) 0.0751(12) Uani 1 1 d . . .
F1 F -0.2754(12) 0.0749(13) 0.2678(5) 0.243(6) Uani 1 1 d . . .
F2 F -0.4637(7) 0.0425(7) 0.1831(6) 0.197(4) Uani 1 1 d . . .
F3 F -0.3159(8) 0.2056(6) 0.1910(6) 0.169(3) Uani 1 1 d . . .
F4 F -0.4869(9) -0.3548(9) -0.0654(6) 0.237(6) Uani 1 1 d . . .
F5 F -0.3172(10) -0.4442(6) -0.1137(7) 0.219(5) Uani 1 1 d . . .
F6 F -0.3921(9) -0.3185(8) -0.1832(5) 0.175(3) Uani 1 1 d . . .
F7 F 0.0353(10) 0.0905(8) 0.4286(6) 0.195(4) Uani 1 1 d . . .
F8 F 0.0004(9) -0.1323(7) 0.4154(5) 0.174(3) Uani 1 1 d . . .
F9 F -0.1609(9) 0.0014(9) 0.4831(6) 0.184(3) Uani 1 1 d . . .
P P 0.0000 0.0000 0.5000 0.1294(17) Uani 1 2 d S . .
Cu Cu 0.0000 0.0000 0.0000 0.0548(3) Uani 1 2 d S . .
C19 C 0.1159(16) 0.342(2) 0.8025(16) 0.242(11) Uani 1 1 d . . .
H19A H 0.0734 0.2705 0.8322 0.290 Uiso 1 1 calc R . .
H19B H 0.1238 0.2996 0.7329 0.290 Uiso 1 1 calc R . .
Cl1 Cl 0.0054(5) 0.5030(6) 0.8252(4) 0.2040(18) Uani 1 1 d . . .
Cl2 Cl 0.2672(7) 0.4179(8) 0.8567(4) 0.256(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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
C2 C1 N1 122.6(5) . . ?
C1 C2 C3 121.2(6) . . ?
C4 C3 C2 115.3(6) . . ?
C4 C3 C6 123.3(5) . . ?
C2 C3 C6 121.4(5) . . ?
C5 C4 C3 120.0(5) . . ?
N1 C5 C4 124.5(5) . . ?
C7 C6 C3 124.6(5) . . ?
C6 C7 C8 125.8(5) . . ?
C9 C8 C7 124.7(5) . . ?
C9 C8 S2 115.3(5) . . ?
C7 C8 S2 119.9(4) . . ?
C8 C9 S1 119.2(5) . . ?
C11 C10 S1 123.5(5) . . ?
C11 C10 S2 121.4(4) . . ?
S1 C10 S2 115.1(3) . . ?
C10 C11 S4 121.9(5) . . ?
C10 C11 S3 123.3(5) . . ?
S4 C11 S3 114.8(3) . . ?
C13 C12 S3 118.8(6) . . ?
C12 C13 S4 117.3(6) . . ?
O1 C14 C15 129.3(6) . . ?
O1 C14 C18 112.7(6) . . ?
C15 C14 C18 118.0(7) . . ?
C14 C15 C16 123.7(7) . . ?
O2 C16 C15 128.5(6) . . ?
O2 C16 C17 115.4(7) . . ?
C15 C16 C17 116.1(7) . . ?
F4 C17 F5 106.5(10) . . ?
F4 C17 F6 107.5(11) . . ?
F5 C17 F6 104.0(9) . . ?
F4 C17 C16 115.1(8) . . ?
F5 C17 C16 111.2(9) . . ?
F6 C17 C16 111.8(8) . . ?
F1 C18 F2 111.5(9) . . ?
F1 C18 F3 104.4(10) . . ?
F2 C18 F3 102.7(10) . . ?
F1 C18 C14 110.4(10) . . ?
F2 C18 C14 115.6(8) . . ?
F3 C18 C14 111.3(7) . . ?
C9 S1 C10 95.1(3) . . ?
C10 S2 C8 95.3(3) . . ?
C11 S3 C12 93.6(4) . . ?
C13 S4 C11 95.4(3) . . ?
C5 N1 C1 116.4(5) . . ?
C5 N1 Cu 121.0(4) . . ?
C1 N1 Cu 122.5(4) . . ?
C14 O1 Cu 128.5(4) . . ?
C16 O2 Cu 120.7(4) . . ?
F8 P F8 180.000(1) 2_556 . ?
F8 P F7 89.7(4) 2_556 2_556 ?
F8 P F7 90.3(4) . 2_556 ?
F8 P F7 90.3(4) 2_556 . ?
F8 P F7 89.7(4) . . ?
F7 P F7 180.000(2) 2_556 . ?
F8 P F9 93.3(4) 2_556 2_556 ?
F8 P F9 86.7(4) . 2_556 ?
F7 P F9 91.1(5) 2_556 2_556 ?
F7 P F9 88.9(5) . 2_556 ?
F8 P F9 86.7(4) 2_556 . ?
F8 P F9 93.3(4) . . ?
F7 P F9 88.9(5) 2_556 . ?
F7 P F9 91.1(5) . . ?
F9 P F9 180.000(1) 2_556 . ?
O1 Cu O1 180.0(2) . 2 ?
O1 Cu N1 91.05(18) . . ?
O1 Cu N1 88.95(18) 2 . ?
O1 Cu N1 88.95(18) . 2 ?
O1 Cu N1 91.05(18) 2 2 ?
N1 Cu N1 180.0(3) . 2 ?
O1 Cu O2 94.81(16) . 2 ?
O1 Cu O2 85.19(16) 2 2 ?
N1 Cu O2 93.14(19) . 2 ?
N1 Cu O2 86.86(19) 2 2 ?
O1 Cu O2 85.19(16) . . ?
O1 Cu O2 94.81(16) 2 . ?
N1 Cu O2 86.86(19) . . ?
N1 Cu O2 93.14(19) 2 . ?
O2 Cu O2 180.0(3) 2 . ?
Cl2 C19 Cl1 101.4(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.344(8) . ?
C1 N1 1.356(7) . ?
C2 C3 1.408(8) . ?
C3 C4 1.402(8) . ?
C3 C6 1.466(8) . ?
C4 C5 1.344(8) . ?
C5 N1 1.339(7) . ?
C6 C7 1.341(8) . ?
C7 C8 1.432(8) . ?
C8 C9 1.336(8) . ?
C8 S2 1.755(6) . ?
C9 S1 1.716(6) . ?
C10 C11 1.369(8) . ?
C10 S1 1.730(6) . ?
C10 S2 1.737(6) . ?
C11 S4 1.730(6) . ?
C11 S3 1.739(6) . ?
C12 C13 1.294(11) . ?
C12 S3 1.744(8) . ?
C13 S4 1.718(8) . ?
C14 O1 1.227(7) . ?
C14 C15 1.384(9) . ?
C14 C18 1.534(10) . ?
C15 C16 1.401(9) . ?
C16 O2 1.209(8) . ?
C16 C17 1.539(11) . ?
C17 F4 1.257(11) . ?
C17 F5 1.284(11) . ?
C17 F6 1.284(11) . ?
C18 F1 1.259(13) . ?
C18 F2 1.292(12) . ?
C18 F3 1.297(11) . ?
N1 Cu 2.016(5) . ?
O1 Cu 1.999(4) . ?
O2 Cu 2.290(5) . ?
F7 P 1.575(6) . ?
F8 P 1.557(6) . ?
F9 P 1.577(8) . ?
P F8 1.557(7) 2_556 ?
P F7 1.575(6) 2_556 ?
P F9 1.577(8) 2_556 ?
Cu O1 1.999(4) 2 ?
Cu N1 2.016(5) 2 ?
Cu O2 2.290(5) 2 ?
C19 Cl2 1.635(15) . ?
C19 Cl1 2.04(2) . ?
