data_(EDT-TTFBr2)2FeBr4
loop_
_publ_author_name
      'Junichi Nishijo'
      'Akira Miyazaki'
      'Toshiaki Enoki'
      'Ryoji Watanabe'
      'Yoshiyuki Kuwatani'
      'Masahiko Iyoda'
_publ_section_title
;
d-Electron-Induced Negative Magnetoresistance of a \p-d Interaction System
Based on a Brominated-TTF Donor
;
_journal_name_full
   'Inorganic Chemistry'
_journal_volume          44
_journal_page_first      2493
_journal_page_last       2506
_journal_year            2005
 
_publ_contact_author              'Toshiaki Enoki' 
_publ_contact_author_email        tenoki@chem.titech.ac.jp 
 

_chemical_name_common 
; 
(4,5-dibromo-4',5'-ethylenedithiotetrathiafulvalene)2(tetrabromo iron)
; 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C16 H8 Br8 Fe S12' 
_chemical_formula_weight          1280.07 
 
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' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M 'I 2/b 1 1'
 
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' 
 
_cell_length_a                    7.066(10) 
_cell_length_b                    13.10(2) 
_cell_length_c                    35.65(9) 
_cell_angle_alpha                 90.26(16) 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3300(11) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        'Needle' 
_exptl_crystal_colour             'Black' 
_exptl_crystal_size_max           1mm 
_exptl_crystal_size_mid           0.1mm 
_exptl_crystal_size_min           0.05mm 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.576 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2408 
_exptl_absorpt_coefficient_mu     10.915 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku AFC7R with CCD detector'  
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7286 
_diffrn_reflns_av_R_equivalents   0.0693 
_diffrn_reflns_av_sigmaI/netI     0.1091 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -46 
_diffrn_reflns_limit_l_max        48 
_diffrn_reflns_theta_min          2.29 
_diffrn_reflns_theta_max          30.76 
_reflns_number_total              3205 
_reflns_number_gt                 2287 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+2.2377P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3205 
_refine_ls_number_parameters      168 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0900 
_refine_ls_R_factor_gt            0.0579 
_refine_ls_wR_factor_ref          0.1321 
_refine_ls_wR_factor_gt           0.1198 
_refine_ls_goodness_of_fit_ref    1.053 
_refine_ls_restrained_S_all       1.053 
_refine_ls_shift/su_max           0.005 
_refine_ls_shift/su_mean          0.001 
 
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_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Fe1 0.0368(6) 0.0325(7) 0.0228(8) -0.0014(5) 0.000 0.000 
Br1 0.0680(5) 0.0569(5) 0.0417(6) 0.0075(4) 0.0111(4) -0.0182(4) 
Br2 0.0665(5) 0.0687(6) 0.0416(6) -0.0126(4) -0.0094(4) -0.0227(4) 
Br3 0.0429(4) 0.0474(4) 0.0274(4) 0.0132(3) 0.0003(3) -0.0009(3) 
Br4 0.0430(4) 0.0461(4) 0.0281(5) -0.0150(3) 0.0003(3) 0.0009(2) 
C1 0.028(3) 0.034(3) 0.015(3) -0.005(3) -0.001(2) 0.002(2) 
C2 0.029(3) 0.034(3) 0.008(3) -0.001(2) 0.002(2) -0.002(2) 
C3 0.029(3) 0.027(3) 0.023(4) -0.005(3) -0.003(2) 0.0039(19) 
C4 0.030(3) 0.028(3) 0.017(4) -0.002(3) -0.002(2) 0.000(2) 
C5 0.026(3) 0.033(3) 0.022(4) 0.002(3) -0.002(2) 0.003(2) 
C6 0.029(3) 0.028(3) 0.010(3) 0.000(2) -0.004(2) 0.004(2) 
C7 0.059(4) 0.037(4) 0.019(4) -0.002(3) -0.014(3) -0.002(3) 
C8 0.055(4) 0.053(5) 0.021(4) 0.003(3) 0.008(3) 0.003(3) 
S1 0.0478(9) 0.0256(8) 0.0216(10) -0.0011(7) 0.0001(6) 0.0001(6) 
S2 0.0464(9) 0.0240(8) 0.0233(10) 0.0000(7) 0.0006(6) -0.0009(5) 
S3 0.0431(8) 0.0243(8) 0.0212(10) -0.0008(6) -0.0006(6) -0.0002(5) 
S4 0.0411(8) 0.0245(8) 0.0202(9) -0.0004(6) -0.0009(6) 0.0002(5) 
S5 0.0522(10) 0.0312(9) 0.0247(11) -0.0065(7) -0.0011(7) 0.0020(6) 
S6 0.0518(9) 0.0313(9) 0.0201(10) 0.0040(7) -0.0015(6) -0.0007(6) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
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) . ? 
 
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) . . ? 
 
_diffrn_measured_fraction_theta_max    0.621 
_diffrn_reflns_theta_full              30.76 
_diffrn_measured_fraction_theta_full   0.621 
_refine_diff_density_max    0.675 
_refine_diff_density_min   -0.814 
_refine_diff_density_rms    0.142 

#===END

 
