#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:46:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179708 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/11/7001194.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_7001194
loop_
_publ_author_name
'Cosquer, Goulven'
'Pointillart, Fabrice'
'Le Gal, Yann'
'Golhen, Stéphane'
'Cador, Olivier'
'Ouahab, Lahcène'
_publ_section_title
;
 Coordination complexes with the redox active tetrathiafulvalene based
 imino-pyrazine ligand: syntheses, a radical cation salt, crystal
 structures and electrochemistry
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3495
_journal_page_last               3502
_journal_paper_doi               10.1039/b815865g
_journal_year                    2009
_chemical_formula_sum            'C11 H7 F6 N3 P S4'
_chemical_formula_weight         454.41
_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                115.373(4)
_cell_angle_beta                 101.960(4)
_cell_angle_gamma                98.581(5)
_cell_formula_units_Z            2
_cell_length_a                   8.7948(6)
_cell_length_b                   10.0620(6)
_cell_length_c                   11.1148(10)
_cell_measurement_reflns_used    3623
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     837.30(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare al, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6610
_diffrn_reflns_theta_full        27.69
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.041(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         6610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0804
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1981P)²+1.0348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.2997
_reflns_number_gt                4067
_reflns_number_total             6610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815865g.txt
_cod_data_source_block           1.PF6
_cod_original_cell_volume        837.30(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001194
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 0.7682(8) 0.2126(7) 0.8941(7) 0.0616(16) Uani 1 1 d . . .
H2 H 0.8639 0.2831 0.9593 0.074 Uiso 1 1 calc R . .
C2 C 0.7271(7) 0.0706(8) 0.8762(7) 0.0598(16) Uani 1 1 d . . .
H1 H 0.7930 0.0382 0.9288 0.072 Uiso 1 1 calc R . .
C3 C 0.5020(6) 0.0808(6) 0.6996(6) 0.0438(12) Uani 1 1 d . . .
C4 C 0.3666(6) 0.0482(6) 0.5908(6) 0.0425(11) Uani 1 1 d . . .
C5 C 0.1080(6) -0.0794(6) 0.3901(6) 0.0438(12) Uani 1 1 d . . .
H5 H 0.0151 -0.1496 0.3200 0.053 Uiso 1 1 calc R . .
C6 C 0.1480(6) 0.0654(6) 0.4141(6) 0.0414(11) Uani 1 1 d . . .
C7 C 0.0527(7) 0.1338(6) 0.3446(6) 0.0442(12) Uani 1 1 d . . .
H7 H -0.0423 0.0759 0.2715 0.053 Uiso 1 1 calc R . .
C8 C 0.0059(6) 0.3473(6) 0.3328(5) 0.0438(12) Uani 1 1 d . . .
C9 C 0.0785(8) 0.4880(7) 0.3442(7) 0.0574(15) Uani 1 1 d . . .
H9 H 0.1895 0.5285 0.3849 0.069 Uiso 1 1 calc R . .
C10 C -0.1634(8) 0.5024(7) 0.2426(7) 0.0585(15) Uani 1 1 d . . .
H10 H -0.2271 0.5512 0.2072 0.070 Uiso 1 1 calc R . .
C11 C -0.2361(8) 0.3646(7) 0.2354(7) 0.0615(16) Uani 1 1 d . . .
H11 H -0.3477 0.3265 0.1986 0.074 Uiso 1 1 calc R . .
F1 F 1.3717(5) 0.1505(5) 0.9989(6) 0.0862(14) Uani 1 1 d . . .
F2 F 1.1165(5) 0.1524(6) 0.9958(6) 0.0996(17) Uani 1 1 d . . .
F3 F 1.1701(5) 0.3955(5) 1.0410(6) 0.0910(15) Uani 1 1 d . . .
F4 F 1.2199(7) 0.2189(6) 0.8574(5) 0.1029(17) Uani 1 1 d . . .
F5 F 1.4245(5) 0.3918(5) 1.0413(6) 0.0930(15) Uani 1 1 d . . .
F6 F 1.3225(7) 0.3248(8) 1.1802(5) 0.122(2) Uani 1 1 d . . .
N1 N 0.1059(6) 0.2769(5) 0.3887(5) 0.0466(11) Uani 1 1 d . . .
N2 N -0.0055(7) 0.5649(6) 0.2990(7) 0.0632(14) Uani 1 1 d . . .
N3 N -0.1523(6) 0.2862(5) 0.2789(6) 0.0566(13) Uani 1 1 d . . .
P1 P 1.27188(18) 0.27402(18) 1.02036(18) 0.0530(4) Uani 1 1 d . . .
S1 S 0.63652(18) 0.25905(16) 0.79134(17) 0.0537(4) Uani 1 1 d . . .
S2 S 0.54894(17) -0.04903(17) 0.75288(16) 0.0512(4) Uani 1 1 d . . .
S3 S 0.32444(17) 0.18606(14) 0.54688(15) 0.0466(4) Uani 1 1 d . . .
S4 S 0.23322(16) -0.13155(15) 0.49263(15) 0.0446(4) 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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
C2 C1 S1 116.9(5) . . ?
C1 C2 S2 117.4(5) . . ?
C4 C3 S1 121.0(4) . . ?
C4 C3 S2 124.0(4) . . ?
S1 C3 S2 115.0(3) . . ?
C3 C4 S3 121.3(4) . . ?
C3 C4 S4 122.1(4) . . ?
S3 C4 S4 116.6(3) . . ?
C6 C5 S4 118.0(4) . . ?
C5 C6 C7 126.2(5) . . ?
C5 C6 S3 117.0(4) . . ?
C7 C6 S3 116.7(4) . . ?
N1 C7 C6 116.9(5) . . ?
N3 C8 N1 120.8(4) . . ?
N3 C8 C9 121.4(5) . . ?
N1 C8 C9 117.8(5) . . ?
N2 C9 C8 122.3(6) . . ?
N2 C10 C11 121.2(5) . . ?
N3 C11 C10 122.6(6) . . ?
C7 N1 C8 117.3(5) . . ?
C9 N2 C10 116.4(5) . . ?
C8 N3 C11 116.1(5) . . ?
F5 P1 F6 90.8(3) . . ?
F5 P1 F2 178.8(3) . . ?
F6 P1 F2 90.3(3) . . ?
F5 P1 F3 91.0(3) . . ?
F6 P1 F3 91.2(3) . . ?
F2 P1 F3 89.4(3) . . ?
F5 P1 F1 89.7(3) . . ?
F6 P1 F1 89.0(3) . . ?
F2 P1 F1 89.9(3) . . ?
F3 P1 F1 179.2(2) . . ?
F5 P1 F4 90.0(3) . . ?
F6 P1 F4 178.8(3) . . ?
F2 P1 F4 88.9(3) . . ?
F3 P1 F4 89.7(3) . . ?
F1 P1 F4 90.2(3) . . ?
C3 S1 C1 95.3(3) . . ?
C2 S2 C3 95.3(3) . . ?
C4 S3 C6 94.2(2) . . ?
C5 S4 C4 94.2(3) . . ?
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 1.336(9) . ?
C1 S1 1.713(7) . ?
C2 S2 1.708(6) . ?
C3 C4 1.391(7) . ?
C3 S1 1.719(5) . ?
C3 S2 1.717(5) . ?
C4 S3 1.720(5) . ?
C4 S4 1.727(5) . ?
C5 C6 1.338(7) . ?
C5 S4 1.719(5) . ?
C6 C7 1.462(7) . ?
C6 S3 1.736(5) . ?
C7 N1 1.277(7) . ?
C8 N3 1.325(7) . ?
C8 N1 1.412(6) . ?
C8 C9 1.405(7) . ?
C9 N2 1.321(7) . ?
C10 N2 1.325(8) . ?
C10 C11 1.400(8) . ?
C11 N3 1.323(7) . ?
F1 P1 1.590(4) . ?
F2 P1 1.581(4) . ?
F3 P1 1.587(4) . ?
F4 P1 1.587(5) . ?
F5 P1 1.556(4) . ?
F6 P1 1.562(5) . ?
