#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:04:03 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180058 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/04/7050448.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_7050448
loop_
_publ_author_name
'Bouguessa, Sabrina'
'Hervé, Katel'
'Golhen, Stéphane'
'Ouahab, Lahcène'
'Fabre, Jean-Marc'
_publ_section_title
;
 Synthesis, redox behaviour and X-ray structure of bis-TTF containing a
 pyridine unit as a potential building block in the construction of
 conducting magnetic materials
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              560
_journal_paper_doi               10.1039/b208624g
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C29 H27 N3 S16'
_chemical_formula_weight         930.50
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 100.367(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   43.3630(16)
_cell_length_b                   5.8730(2)
_cell_length_c                   16.1730(8)
_cell_measurement_reflns_used    3772
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.998
_cell_volume                     4051.6(3)
_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      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6207
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.881
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0647
_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)+(0.0942P)²+8.0160P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.2141
_reflns_number_gt                2107
_reflns_number_total             3700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208624g.txt
_cod_data_source_block           calcul
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050448
loop_
_symmetry_equiv_pos_as_xyz
'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, -y, -z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.0000 0.5946(8) 0.2500 0.0536(14) Uani 1 2 d S . .
C11 C 0.01699(12) 0.4794(8) 0.2032(3) 0.0620(13) Uani 1 1 d . . .
C10 C 0.03526(12) 0.6153(9) 0.1503(3) 0.0651(14) Uani 1 1 d . . .
H10A H 0.0217 0.7316 0.1207 0.078 Uiso 1 1 calc R . .
H10B H 0.0416 0.5157 0.1086 0.078 Uiso 1 1 calc R . .
C12 C 0.01755(19) 0.2459(9) 0.2015(5) 0.106(3) Uani 1 1 d . . .
H12 H 0.0295 0.1684 0.1684 0.127 Uiso 1 1 calc R . .
C7 C 0.0761(2) 0.275(3) 0.4487(5) 0.219(8) Uani 1 1 d . . .
H7A H 0.0910 0.1519 0.4477 0.262 Uiso 1 1 calc R . .
H7B H 0.0752 0.3020 0.5073 0.262 Uiso 1 1 calc R . .
C13 C 0.0000 0.1300(14) 0.2500 0.170(7) Uani 1 2 d S . .
H13 H 0.0000 -0.0283 0.2500 0.204 Uiso 1 2 calc SR . .
N2 N 0.0350(2) -0.1352(14) 0.4973(5) 0.135(3) Uani 1 1 d . . .
C9 C 0.0486(3) -0.0069(16) 0.4714(5) 0.125(3) Uani 1 1 d . . .
C15 C 0.21272(19) -0.0198(15) -0.0202(5) 0.127(3) Uani 1 1 d . . .
H15A H 0.2225 -0.0476 -0.0681 0.190 Uiso 1 1 calc R . .
H15B H 0.2274 0.0529 0.0231 0.190 Uiso 1 1 calc R . .
H15C H 0.1948 0.0771 -0.0364 0.190 Uiso 1 1 calc R . .
C14 C 0.225119(14) -0.50570(11) 0.31548(4) 0.148(4) Uani 1 1 d . . .
H14A H 0.2400 -0.6232 0.3356 0.221 Uiso 1 1 calc R . .
H14B H 0.2059 -0.5340 0.3351 0.221 Uiso 1 1 calc R . .
H14C H 0.2334 -0.3607 0.3360 0.221 Uiso 1 1 calc R . .
C8 C 0.048111(14) 0.19309(11) 0.41348(4) 0.368(19) Uani 1 1 d R . .
H8A H 0.0473 0.1477 0.3555 0.442 Uiso 1 1 calc R . .
H8B H 0.0312 0.2984 0.4174 0.442 Uiso 1 1 calc R . .
S1 S 0.069808(14) 0.75080(11) 0.20969(4) 0.0796(5) Uani 1 1 d R . .
S2 S 0.109750(14) 0.38502(11) 0.15522(4) 0.0845(5) Uani 1 1 d R . .
S3 S 0.170570(14) -0.18069(11) 0.25533(4) 0.0926(6) Uani 1 1 d R . .
S4 S 0.153758(14) 0.00626(11) 0.08436(4) 0.0888(6) Uani 1 1 d R . .
S5 S 0.131186(14) 0.21176(11) 0.32628(4) 0.1016(7) Uani 1 1 d R . .
S6 S 0.200545(14) -0.28248(11) 0.01781(4) 0.1124(7) Uani 1 1 d R . .
S7 S 0.218061(14) -0.50413(11) 0.20601(4) 0.1090(7) Uani 1 1 d R . .
S8 S 0.095570(14) 0.55468(11) 0.40750(4) 0.1085(7) Uani 1 1 d R . .
C1 C 0.191409(14) -0.28282(11) 0.18016(4) 0.0719(15) Uani 1 1 d R . .
C3 C 0.149663(14) 0.02564(11) 0.18961(4) 0.0714(15) Uani 1 1 d R . .
C6 C 0.094561(14) 0.51557(11) 0.23684(4) 0.0716(15) Uani 1 1 d R . .
C2 C 0.183996(14) -0.19505(11) 0.10275(4) 0.0747(16) Uani 1 1 d R . .
C5 C 0.104151(14) 0.43568(11) 0.31484(4) 0.0820(17) Uani 1 1 d R . .
C4 C 0.132222(14) 0.18305(11) 0.21912(4) 0.0749(16) Uani 1 1 d R . .
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'
S S 0.1246 0.1234 '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'
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
C11 N1 C11 119.0(5) 2 . ?
N1 C11 C12 122.1(5) . . ?
N1 C11 C10 117.3(4) . . ?
C12 C11 C10 120.6(5) . . ?
C11 C10 S1 113.8(4) . . ?
C13 C12 C11 118.2(6) . . ?
C8 C7 S8 123.8(9) . . ?
C12 C13 C12 120.3(8) 2 . ?
N2 C9 C8 146.7(11) . . ?
C7 C8 C9 96.1(8) . . ?
C6 S1 C10 101.35(16) . . ?
C4 S2 C6 95.5 . . ?
C1 S3 C3 95.2 . . ?
C3 S4 C2 94.8 . . ?
C5 S5 C4 96.0 . . ?
C2 S6 C15 102.0(2) . . ?
C1 S7 C14 103.6 . . ?
C5 S8 C7 97.1(3) . . ?
C2 C1 S7 123.4 . . ?
C2 C1 S3 116.8 . . ?
S7 C1 S3 119.6 . . ?
C4 C3 S4 123.8 . . ?
C4 C3 S3 121.7 . . ?
S4 C3 S3 114.4 . . ?
C5 C6 S2 117.4 . . ?
C5 C6 S1 125.7 . . ?
S2 C6 S1 116.8 . . ?
C1 C2 S6 124.2 . . ?
C1 C2 S4 117.7 . . ?
S6 C2 S4 117.9 . . ?
C6 C5 S5 116.8 . . ?
C6 C5 S8 126.0 . . ?
S5 C5 S8 116.8 . . ?
C3 C4 S2 123.3 . . ?
C3 C4 S5 122.5 . . ?
S2 C4 S5 114.1 . . ?
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
N1 C11 1.332(5) 2 ?
N1 C11 1.332(5) . ?
C11 C12 1.372(7) . ?
C11 C10 1.496(6) . ?
C10 S1 1.812(6) . ?
C12 C13 1.368(7) . ?
C7 C8 1.334(10) . ?
C7 S8 2.015(14) . ?
C13 C12 1.368(7) 2 ?
N2 C9 1.087(11) . ?
C9 C8 1.500(9) . ?
C15 S6 1.776(8) . ?
C14 S7 1.7416 . ?
S1 C6 1.7561 . ?
S2 C4 1.7499 . ?
S2 C6 1.7541 . ?
S3 C1 1.7463 . ?
S3 C3 1.7530 . ?
S4 C3 1.7467 . ?
S4 C2 1.7508 . ?
S5 C5 1.7493 . ?
S5 C4 1.7499 . ?
S6 C2 1.7379 . ?
S7 C1 1.7395 . ?
S8 C5 1.7530 . ?
C1 C2 1.3386 . ?
C3 C4 1.3358 . ?
C6 C5 1.3401 . ?
