#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:46:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179127 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308947.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_4308947
loop_
_publ_author_name
'Junichi Nishijo'
'Akira Miyazaki'
'Toshiaki Enoki'
'Ryoji Watanabe'
'Yoshiyuki Kuwatani'
'Masahiko Iyoda'
_publ_contact_author             'Toshiaki Enoki'
_publ_contact_author_email       tenoki@chem.titech.ac.jp
_publ_section_title
;
d-Electron-Induced Negative Magnetoresistance of a π-d Interaction System
Based on a Brominated-TTF Donor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2493
_journal_page_last               2506
_journal_paper_doi               10.1021/ic048548k
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C16 H8 Br8 Fe S12'
_chemical_formula_weight         1280.07
_chemical_name_common
; 
(4,5-dibromo-4',5'-ethylenedithiotetrathiafulvalene)2(tetrabromo iron)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2xb'
_symmetry_space_group_name_H-M   'I 2/b 1 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.26(16)
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.066(10)
_cell_length_b                   13.10(2)
_cell_length_c                   35.65(9)
_cell_measurement_temperature    293(2)
_cell_volume                     3300(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.621
_diffrn_measured_fraction_theta_max 0.621
_diffrn_measurement_device_type  'Rigaku AFC7R with CCD detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            7286
_diffrn_reflns_theta_full        30.76
_diffrn_reflns_theta_max         30.76
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    10.915
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          1mm
_exptl_crystal_size_mid          0.1mm
_exptl_crystal_size_min          0.05mm
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0262P)²+2.2377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                2287
_reflns_number_total             3205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048548ksi20041016_122440_1.cif
_cod_data_source_block           (EDT-TTFBr2)2FeBr4
_cod_database_code               4308947
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1, z+1/2'
'-x, -y, -z'
'x, -y-1/2, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.04663(16) 0.2500 0.5000 0.0307(3) Uani 1 2 d S . .
Br1 Br 0.24164(12) 0.35100(7) 0.46231(3) 0.0555(3) Uani 1 1 d . . .
Br2 Br -0.14426(11) 0.15203(7) 0.46164(3) 0.0590(3) Uani 1 1 d . . .
Br3 Br 0.32338(9) 0.12945(6) 0.13917(2) 0.0392(2) Uani 1 1 d . . .
Br4 Br 0.32895(9) -0.13594(5) 0.14111(2) 0.0391(2) Uani 1 1 d . . .
C1 C 0.3306(7) -0.0531(5) 0.18279(19) 0.0253(12) Uani 1 1 d . . .
C2 C 0.3312(7) 0.0495(5) 0.18213(18) 0.0237(12) Uani 1 1 d . . .
C3 C 0.3337(7) 0.0001(5) 0.2519(2) 0.0265(13) Uani 1 1 d . . .
C4 C 0.3333(7) -0.0003(4) 0.29010(19) 0.0249(12) Uani 1 1 d . . .
C5 C 0.3259(7) -0.0500(5) 0.3605(2) 0.0273(13) Uani 1 1 d . . .
C6 C 0.3292(7) 0.0532(4) 0.35953(18) 0.0223(12) Uani 1 1 d . . .
C7 C 0.3859(10) 0.0486(5) 0.4353(2) 0.0382(15) Uani 1 1 d . . .
H7A H 0.5178 0.0287 0.4333 0.046 Uiso 1 1 calc R . .
H7B H 0.3700 0.0842 0.4590 0.046 Uiso 1 1 calc R . .
C8 C 0.2662(10) -0.0457(6) 0.4356(2) 0.0428(17) Uani 1 1 d . . .
H8A H 0.1342 -0.0260 0.4336 0.051 Uiso 1 1 calc R . .
H8B H 0.2827 -0.0799 0.4595 0.051 Uiso 1 1 calc R . .
S1 S 0.3351(2) -0.11346(12) 0.22653(5) 0.0317(4) Uani 1 1 d . . .
S2 S 0.3335(2) 0.11175(12) 0.22497(5) 0.0312(4) Uani 1 1 d . . .
S3 S 0.3290(2) -0.11072(12) 0.31698(5) 0.0296(3) Uani 1 1 d . . .
S4 S 0.3341(2) 0.11247(11) 0.31579(5) 0.0286(3) Uani 1 1 d . . .
S5 S 0.3314(2) 0.13592(13) 0.39757(6) 0.0360(4) Uani 1 1 d . . .
S6 S 0.3207(2) -0.13282(13) 0.39881(5) 0.0344(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
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
Br2 Fe1 Br2 108.43(15) 6_566 . ?
Br2 Fe1 Br1 111.71(13) 6_566 . ?
Br2 Fe1 Br1 108.60(15) . . ?
Br2 Fe1 Br1 108.60(15) 6_566 6_566 ?
Br2 Fe1 Br1 111.72(13) . 6_566 ?
Br1 Fe1 Br1 107.82(15) . 6_566 ?
C2 C1 S1 118.1(5) . . ?
C2 C1 Br4 125.0(6) . . ?
S1 C1 Br4 116.9(4) . . ?
C1 C2 S2 116.9(5) . . ?
C1 C2 Br3 125.5(5) . . ?
S2 C2 Br3 117.6(4) . . ?
C4 C3 S1 120.8(5) . . ?
C4 C3 S2 123.7(5) . . ?
S1 C3 S2 115.5(4) . . ?
C3 C4 S4 121.3(5) . . ?
C3 C4 S3 124.0(5) . . ?
S4 C4 S3 114.7(4) . . ?
C6 C5 S3 115.4(6) . . ?
C6 C5 S6 130.2(6) . . ?
S3 C5 S6 114.4(4) . . ?
C5 C6 S5 126.9(6) . . ?
C5 C6 S4 118.2(5) . . ?
S5 C6 S4 114.8(4) . . ?
C8 C7 S5 114.1(5) . . ?
C7 C8 S6 113.5(5) . . ?
C3 S1 C1 94.2(4) . . ?
C2 S2 C3 95.3(3) . . ?
C4 S3 C5 96.5(3) . . ?
C4 S4 C6 95.2(3) . . ?
C6 S5 C7 100.9(4) . . ?
C5 S6 C8 100.4(4) . . ?
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
Fe1 Br2 2.307(4) 6_566 ?
Fe1 Br2 2.307(4) . ?
Fe1 Br1 2.339(4) . ?
Fe1 Br1 2.339(4) 6_566 ?
Br3 C2 1.860(7) . ?
Br4 C1 1.836(7) . ?
C1 C2 1.345(9) . ?
C1 S1 1.752(8) . ?
C2 S2 1.728(7) . ?
C3 C4 1.362(10) . ?
C3 S1 1.738(7) . ?
C3 S2 1.753(8) . ?
C4 S4 1.735(7) . ?
C4 S3 1.739(7) . ?
C5 C6 1.353(9) . ?
C5 S3 1.742(8) . ?
C5 S6 1.748(8) . ?
C6 S5 1.732(7) . ?
C6 S4 1.745(8) . ?
C7 C8 1.498(10) . ?
C7 S5 1.811(8) . ?
C8 S6 1.778(9) . ?
