# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Manuel Almeida'
_publ_contact_author_address     
;
Departamento Quimica
Instituto Técnologico e Nuclear / CFMCUL
Sacavem Codex
P-2686-953
PORTUGAL
;

_publ_contact_author_email       MALMEIDA@ITN.PT

_publ_section_title              
;
Cation and ligand roles in the coordination
of FeIII bisdithiolene complexes; The crystal structures of
BrBzPy [Fe(qdt)2] and [Fe(alpha-tpdt)2] salts
;
loop_
_publ_author_name
'Manuel Almeida'
'Dulce Belo'
'Isabel Cordeiro Santos'
'Ana Isabel Soares Neves'
# end Validation Reply Form

# Attachment 'ANeves__n-Bu4N_2[Fe_alpha-tpdt_2]2.cif'

data_tbafea
_database_code_depnum_ccdc_archive 'CCDC 695832'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H36 N), C16 H8 Fe2 S12'
_chemical_formula_sum            'C48 H80 Fe2 N2 S12'
_chemical_formula_weight         1181.56

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'
N N 0.0061 0.0033 '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'
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   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.593(3)
_cell_length_b                   13.734(3)
_cell_length_c                   17.690(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.430(11)
_cell_angle_gamma                90.00
_cell_volume                     3033.8(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2154
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      19.28

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1252
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_T_max  0.9133
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18378
_diffrn_reflns_av_R_equivalents  0.1777
_diffrn_reflns_av_sigmaI/netI    0.1942
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         23.43
_reflns_number_total             4339
_reflns_number_gt                1637
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The poor quality of the crystal results in a weak data set which is
responsible for the low ratio Observed/Unique reflections (38%), a hight
Rint (0.18) and a low resolution data collection (θ-23.43).
The terminal thiophenic rings in the anion units showed evidence of
disorder in the displacement parameters of C and S atoms. However,
this could not be successfully modelled.
Due to problems with severe anisotropy and disorder, restraints to anisotropic
parameters were used (ISOR and DFIX instructions of SHELX).
All non-H atoms were refined ANIS with the exception of the severe
disordered carbon atoms of cation which were left isotropic.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4339
_refine_ls_number_parameters     264
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.3038
_refine_ls_R_factor_gt           0.1322
_refine_ls_wR_factor_ref         0.3878
_refine_ls_wR_factor_gt          0.3258
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 0.52455(18) 0.60470(16) 0.03343(11) 0.0532(8) Uani 1 1 d . . .
S1 S 0.4392(3) 0.4814(3) 0.0828(2) 0.0543(12) Uani 1 1 d . . .
S2 S 0.3667(3) 0.6778(3) -0.0058(2) 0.0581(12) Uani 1 1 d . . .
S3 S 0.1414(4) 0.6181(4) 0.0209(3) 0.0896(18) Uani 1 1 d . . .
S4 S 0.6004(4) 0.7468(4) 0.0142(4) 0.0917(18) Uani 1 1 d . . .
S5 S 0.6687(4) 0.5633(3) 0.1133(2) 0.0660(14) Uani 1 1 d . . .
S6 S 0.8956(6) 0.6499(7) 0.1197(4) 0.148(3) Uani 1 1 d D . .
N1 N 0.6434(18) 0.2619(16) 0.2538(10) 0.122(7) Uani 1 1 d . . .
C1 C 0.2770(13) 0.5996(13) 0.0292(9) 0.061(5) Uani 1 1 d . . .
C2 C 0.3069(12) 0.5162(12) 0.0655(8) 0.050(4) Uani 1 1 d . . .
C3 C 0.2158(13) 0.4628(13) 0.0865(8) 0.061(5) Uani 1 1 d . . .
H3 H 0.2191 0.4026 0.1107 0.073 Uiso 1 1 calc R . .
C4 C 0.1280(18) 0.5128(16) 0.0661(9) 0.090(7) Uani 1 1 d . . .
H4 H 0.0614 0.4908 0.0762 0.108 Uiso 1 1 calc R . .
C5 C 0.7589(14) 0.6471(14) 0.0944(10) 0.070(5) Uani 1 1 d U . .
C6 C 0.7368(13) 0.7218(15) 0.0540(11) 0.084(7) Uani 1 1 d . . .
C7 C 0.8266(11) 0.7964(11) 0.0376(10) 0.061(5) Uani 1 1 d D . .
H7 H 0.8218 0.8534 0.0090 0.074 Uiso 1 1 calc R . .
C8 C 0.9106(18) 0.7533(15) 0.0766(14) 0.146(10) Uani 1 1 d DU . .
H8 H 0.9780 0.7818 0.0794 0.175 Uiso 1 1 calc R . .
C10 C 0.534(3) 0.2796(19) 0.2098(14) 0.159(12) Uani 1 1 d . . .
H10A H 0.5376 0.2629 0.1569 0.191 Uiso 1 1 calc R . .
H10B H 0.5194 0.3489 0.2115 0.191 Uiso 1 1 calc R . .
C11 C 0.435(2) 0.224(2) 0.2357(12) 0.152(12) Uani 1 1 d . . .
H11A H 0.4504 0.1551 0.2390 0.183 Uiso 1 1 calc R . .
H11B H 0.4234 0.2469 0.2859 0.183 Uiso 1 1 calc R . .
C12 C 0.338(2) 0.241(2) 0.1817(19) 0.176(14) Uani 1 1 d . . .
H12A H 0.3259 0.3105 0.1764 0.211 Uiso 1 1 calc R . .
H12B H 0.3496 0.2158 0.1322 0.211 Uiso 1 1 calc R . .
C13 C 0.248(2) 0.198(2) 0.2032(15) 0.146(10) Uani 1 1 d . . .
H13A H 0.1871 0.2133 0.1665 0.218 Uiso 1 1 calc R . .
H13B H 0.2360 0.2220 0.2523 0.218 Uiso 1 1 calc R . .
H13C H 0.2575 0.1286 0.2056 0.218 Uiso 1 1 calc R . .
C20 C 0.673(2) 0.159(2) 0.2672(14) 0.164(12) Uani 1 1 d . . .
H20A H 0.6292 0.1320 0.3030 0.197 Uiso 1 1 calc R . .
H20B H 0.7472 0.1563 0.2907 0.197 Uiso 1 1 calc R . .
C21 C 0.661(3) 0.093(2) 0.1920(17) 0.192(15) Uani 1 1 d D . .
H21A H 0.5887 0.1046 0.1665 0.230 Uiso 1 1 calc R . .
H21B H 0.7092 0.1200 0.1590 0.230 Uiso 1 1 calc R . .
C22 C 0.678(3) -0.017(2) 0.194(2) 0.231(17) Uiso 1 1 d D . .
H22A H 0.6537 -0.0466 0.2383 0.277 Uiso 1 1 calc R . .
H22B H 0.6408 -0.0482 0.1482 0.277 Uiso 1 1 calc R . .
C23 C 0.796(3) -0.024(4) 0.196(4) 0.42(4) Uiso 1 1 d D . .
H23A H 0.8176 -0.0908 0.2037 0.626 Uiso 1 1 calc R . .
H23B H 0.8296 0.0149 0.2372 0.626 Uiso 1 1 calc R . .
H23C H 0.8161 -0.0011 0.1487 0.626 Uiso 1 1 calc R . .
C30 C 0.727(2) 0.3158(19) 0.2133(13) 0.132(9) Uani 1 1 d . . .
H30A H 0.7269 0.2874 0.1630 0.158 Uiso 1 1 calc R . .
H30B H 0.7048 0.3831 0.2062 0.158 Uiso 1 1 calc R . .
C31 C 0.836(2) 0.315(3) 0.2515(13) 0.173(14) Uani 1 1 d D . .
H31A H 0.8587 0.2473 0.2594 0.208 Uiso 1 1 calc R . .
H31B H 0.8372 0.3444 0.3013 0.208 Uiso 1 1 calc R . .
C32 C 0.917(3) 0.367(3) 0.209(3) 0.28(2) Uiso 1 1 d D . .
H32A H 0.8839 0.4182 0.1758 0.340 Uiso 1 1 calc R . .
H32B H 0.9762 0.3939 0.2429 0.340 Uiso 1 1 calc R . .
C33 C 0.952(4) 0.281(4) 0.163(4) 0.40(3) Uiso 1 1 d D . .
H33A H 1.0021 0.3031 0.1299 0.601 Uiso 1 1 calc R . .
H33B H 0.8906 0.2532 0.1328 0.601 Uiso 1 1 calc R . .
H33C H 0.9857 0.2327 0.1972 0.601 Uiso 1 1 calc R . .
C40 C 0.654(2) 0.3024(19) 0.3371(12) 0.133(10) Uani 1 1 d . . .
H40A H 0.6057 0.2682 0.3660 0.160 Uiso 1 1 calc R . .
H40B H 0.7269 0.2922 0.3619 0.160 Uiso 1 1 calc R . .
C41 C 0.628(3) 0.411(2) 0.3349(15) 0.196(17) Uani 1 1 d D . .
H41A H 0.6841 0.4469 0.3137 0.235 Uiso 1 1 calc R . .
H41B H 0.5611 0.4225 0.3029 0.235 Uiso 1 1 calc R . .
C42 C 0.621(3) 0.446(2) 0.416(2) 0.230(19) Uani 1 1 d D . .
H42A H 0.5966 0.5133 0.4163 0.276 Uiso 1 1 calc R . .
H42B H 0.5730 0.4054 0.4409 0.276 Uiso 1 1 calc R . .
C43 C 0.733(3) 0.436(3) 0.452(3) 0.27(2) Uiso 1 1 d . . .
H43A H 0.7391 0.4577 0.5036 0.412 Uiso 1 1 calc R . .
H43B H 0.7786 0.4754 0.4243 0.412 Uiso 1 1 calc R . .
H43C H 0.7546 0.3693 0.4500 0.412 Uiso 1 1 calc R . .


_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 S4 2.218(5) . ?
Fe1 S5 2.226(5) . ?
Fe1 S1 2.242(5) . ?
Fe1 S2 2.255(4) . ?
Fe1 S1 2.466(4) 3_665 ?
S1 C2 1.722(16) . ?
S1 Fe1 2.466(4) 3_665 ?
S2 C1 1.731(17) . ?
S3 C4 1.67(2) . ?
S3 C1 1.713(17) . ?
S4 C6 1.80(2) . ?
S5 C5 1.681(19) . ?
S6 C8 1.634(16) . ?
S6 C5 1.721(18) . ?
N1 C20 1.47(3) . ?
N1 C10 1.51(3) . ?
N1 C30 1.54(3) . ?
N1 C40 1.56(3) . ?
C1 C2 1.34(2) . ?
C2 C3 1.45(2) . ?
C3 C4 1.31(2) . ?
C5 C6 1.26(2) . ?
C6 C7 1.58(2) . ?
C7 C8 1.326(16) . ?
C10 C11 1.57(3) . ?
C11 C12 1.47(3) . ?
C12 C13 1.38(3) . ?
C20 C21 1.60(3) . ?
C21 C22 1.538(18) . ?
C22 C23 1.485(19) . ?
C30 C31 1.45(3) . ?
C31 C32 1.529(19) . ?
C32 C33 1.53(2) . ?
C40 C41 1.53(3) . ?
C41 C42 1.525(19) . ?
C42 C43 1.48(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
S4 Fe1 S5 89.4(2) . . ?
S4 Fe1 S1 164.1(2) . . ?
S5 Fe1 S1 87.26(18) . . ?
S4 Fe1 S2 86.64(19) . . ?
S5 Fe1 S2 157.44(17) . . ?
S1 Fe1 S2 90.47(17) . . ?
S4 Fe1 S1 99.5(2) . 3_665 ?
S5 Fe1 S1 100.58(16) . 3_665 ?
S1 Fe1 S1 96.47(14) . 3_665 ?
S2 Fe1 S1 101.98(16) . 3_665 ?
C2 S1 Fe1 102.9(6) . . ?
C2 S1 Fe1 105.3(5) . 3_665 ?
Fe1 S1 Fe1 83.53(14) . 3_665 ?
C1 S2 Fe1 101.7(6) . . ?
C4 S3 C1 89.5(10) . . ?
C6 S4 Fe1 100.4(7) . . ?
C5 S5 Fe1 102.4(7) . . ?
C8 S6 C5 94.0(11) . . ?
C20 N1 C10 116(2) . . ?
C20 N1 C30 111(2) . . ?
C10 N1 C30 108.5(17) . . ?
C20 N1 C40 101.5(18) . . ?
C10 N1 C40 113(2) . . ?
C30 N1 C40 106.6(19) . . ?
C2 C1 S3 112.5(13) . . ?
C2 C1 S2 123.0(13) . . ?
S3 C1 S2 124.5(12) . . ?
C1 C2 C3 111.8(15) . . ?
C1 C2 S1 121.8(12) . . ?
C3 C2 S1 126.4(14) . . ?
C4 C3 C2 109.4(18) . . ?
C3 C4 S3 116.8(16) . . ?
C6 C5 S5 124.4(15) . . ?
C6 C5 S6 105.6(15) . . ?
S5 C5 S6 130.0(12) . . ?
C5 C6 C7 121.4(18) . . ?
C5 C6 S4 120.4(14) . . ?
C7 C6 S4 118.2(16) . . ?
C8 C7 C6 99.0(17) . . ?
C7 C8 S6 119.9(18) . . ?
N1 C10 C11 118.3(18) . . ?
C12 C11 C10 111(2) . . ?
C13 C12 C11 114(3) . . ?
N1 C20 C21 114.3(19) . . ?
C22 C21 C20 123(3) . . ?
C23 C22 C21 102(3) . . ?
C31 C30 N1 116(2) . . ?
C30 C31 C32 114(3) . . ?
C33 C32 C31 99(3) . . ?
C41 C40 N1 109.3(19) . . ?
C42 C41 C40 109(2) . . ?
C43 C42 C41 101(3) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        23.43
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.178

# start Validation Reply Form
_vrf_PLAT242_tbafea              
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C22
RESPONSE: Due to problems with severe anisotropy and disorder,
restraints to anisotropic parameters were used (ISOR and DFIX instructions
of SHELX).
All non-H atoms were refined ANIS with the exception of the severe
disordered carbon atoms of cation which were left isotropic.
The poor quality of the crystal results in a weak data set which is
responsible for the low ratio Observed/Unique reflections (38%), a hight
Rint (0.18) and a low resolution data collection (\q-23.43).

;
# end Validation Reply Form

# end Validation Reply Form

# Attachment 'ANeves__BrBzPy]2[Fe_qdt_2]2.cif'

data_brfqdt
_database_code_depnum_ccdc_archive 'CCDC 695833'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H16 Fe2 N8 S8, 2(C12 H11 Br N)'
_chemical_formula_sum            'C56 H38 Br2 Fe2 N10 S8'
_chemical_formula_weight         1378.96

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'
N N 0.0061 0.0033 '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'
Fe Fe 0.3463 0.8444 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3129(4)
_cell_length_b                   11.4865(7)
_cell_length_c                   17.0461(11)
_cell_angle_alpha                100.625(3)
_cell_angle_beta                 98.672(3)
_cell_angle_gamma                106.991(3)
_cell_volume                     1313.60(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1662
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      25.40

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             694
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5691
_exptl_absorpt_correction_T_max  0.9528
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11335
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         25.68
_reflns_number_total             4957
_reflns_number_gt                3157
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0302P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4957
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.0812
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_restrained_S_all      0.903
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Br1 Br 0.38841(7) 0.32367(5) 0.13913(3) 0.03094(15) Uani 1 1 d . . .
Fe1 Fe 0.71996(8) 0.03868(6) 0.55216(3) 0.01376(15) Uani 1 1 d . . .
S1 S 0.93239(14) 0.19923(10) 0.64799(6) 0.0157(2) Uani 1 1 d . . .
S2 S 0.65311(15) -0.06762(10) 0.64698(6) 0.0161(2) Uani 1 1 d . . .
S3 S 0.87005(14) 0.10426(10) 0.45593(6) 0.0162(2) Uani 1 1 d . . .
S4 S 0.54207(14) -0.14081(10) 0.46206(6) 0.0143(2) Uani 1 1 d . . .
N1 N 0.9471(5) 0.2585(3) 0.80719(19) 0.0155(8) Uani 1 1 d . . .
N2 N 0.7101(5) 0.0140(3) 0.8070(2) 0.0189(8) Uani 1 1 d . . .
N3 N 0.8080(5) 0.0015(3) 0.2974(2) 0.0170(8) Uani 1 1 d . . .
N4 N 0.5372(5) -0.2259(3) 0.3070(2) 0.0162(8) Uani 1 1 d . . .
N5 N 1.2395(4) 0.4482(3) 0.4148(2) 0.0146(8) Uani 1 1 d . . .
C1 C 0.8759(5) 0.1684(4) 0.7402(2) 0.0136(10) Uani 1 1 d . . .
C2 C 0.7520(5) 0.0447(4) 0.7400(2) 0.0134(9) Uani 1 1 d . . .
C3 C 0.9008(6) 0.2280(4) 0.8777(3) 0.0189(10) Uani 1 1 d . . .
C4 C 0.7836(6) 0.1070(4) 0.8774(2) 0.0169(10) Uani 1 1 d . . .
C5 C 0.9712(6) 0.3218(4) 0.9518(3) 0.0262(11) Uani 1 1 d . . .
H5 H 1.0488 0.4043 0.9523 0.031 Uiso 1 1 calc R . .
C6 C 0.7427(6) 0.0807(5) 0.9518(3) 0.0284(12) Uani 1 1 d . . .
H6 H 0.6665 -0.0015 0.9525 0.034 Uiso 1 1 calc R . .
C7 C 0.9277(6) 0.2940(5) 1.0223(3) 0.0280(12) Uani 1 1 d . . .
H7 H 0.9762 0.3573 1.0720 0.034 Uiso 1 1 calc R . .
C8 C 0.8118(6) 0.1727(5) 1.0228(3) 0.0281(12) Uani 1 1 d . . .
H8 H 0.7815 0.1546 1.0724 0.034 Uiso 1 1 calc R . .
C9 C 0.7584(5) -0.0146(4) 0.3667(2) 0.0142(9) Uani 1 1 d . . .
C10 C 0.6173(5) -0.1291(4) 0.3699(2) 0.0127(9) Uani 1 1 d . . .
C11 C 0.7214(6) -0.0941(4) 0.2297(2) 0.0166(10) Uani 1 1 d . . .
C12 C 0.5882(6) -0.2088(4) 0.2339(2) 0.0170(10) Uani 1 1 d . . .
C13 C 0.7655(6) -0.0799(4) 0.1537(3) 0.0229(11) Uani 1 1 d . . .
H13 H 0.8532 -0.0029 0.1497 0.027 Uiso 1 1 calc R . .
C14 C 0.5085(6) -0.3073(4) 0.1633(3) 0.0231(11) Uani 1 1 d . . .
H14 H 0.4232 -0.3858 0.1661 0.028 Uiso 1 1 calc R . .
C15 C 0.6831(7) -0.1757(5) 0.0863(3) 0.0304(12) Uani 1 1 d . . .
H15 H 0.7137 -0.1650 0.0353 0.036 Uiso 1 1 calc R . .
C16 C 0.5538(6) -0.2901(5) 0.0904(3) 0.0279(12) Uani 1 1 d . . .
H16 H 0.4971 -0.3562 0.0424 0.033 Uiso 1 1 calc R . .
C17 C 1.2483(5) 0.3654(4) 0.4602(2) 0.0164(10) Uani 1 1 d . . .
H17 H 1.2473 0.2840 0.4352 0.020 Uiso 1 1 calc R . .
C18 C 1.2587(5) 0.3986(4) 0.5433(3) 0.0202(10) Uani 1 1 d . . .
H18 H 1.2651 0.3404 0.5758 0.024 Uiso 1 1 calc R . .
C19 C 1.2597(5) 0.5158(4) 0.5785(3) 0.0192(10) Uani 1 1 d . . .
H19 H 1.2667 0.5395 0.6356 0.023 Uiso 1 1 calc R . .
C20 C 1.2506(6) 0.5992(4) 0.5313(3) 0.0204(10) Uani 1 1 d . . .
H20 H 1.2523 0.6810 0.5554 0.024 Uiso 1 1 calc R . .
C21 C 1.2391(5) 0.5638(4) 0.4490(3) 0.0186(10) Uani 1 1 d . . .
H21 H 1.2308 0.6209 0.4159 0.022 Uiso 1 1 calc R . .
C22 C 1.2258(6) 0.4122(4) 0.3248(2) 0.0231(11) Uani 1 1 d . . .
H22A H 1.2614 0.3352 0.3112 0.028 Uiso 1 1 calc R . .
H22B H 1.3206 0.4800 0.3088 0.028 Uiso 1 1 calc R . .
C23 C 1.0243(6) 0.3893(4) 0.2771(2) 0.0155(10) Uani 1 1 d . . .
C24 C 0.8758(6) 0.2767(4) 0.2695(2) 0.0231(11) Uani 1 1 d . . .
H24 H 0.9042 0.2132 0.2928 0.028 Uiso 1 1 calc R . .
C25 C 0.6872(6) 0.2570(4) 0.2282(2) 0.0220(10) Uani 1 1 d . . .
H25 H 0.5859 0.1800 0.2223 0.026 Uiso 1 1 calc R . .
C26 C 0.6493(6) 0.3503(4) 0.1960(2) 0.0185(10) Uani 1 1 d . . .
C27 C 0.7917(6) 0.4630(4) 0.2019(2) 0.0208(10) Uani 1 1 d . . .
H27 H 0.7615 0.5258 0.1784 0.025 Uiso 1 1 calc R . .
C28 C 0.9803(6) 0.4819(4) 0.2433(2) 0.0196(10) Uani 1 1 d . . .
H28 H 1.0808 0.5591 0.2487 0.023 Uiso 1 1 calc R . .


_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
Br1 C26 1.914(4) . ?
Fe1 S1 2.2208(11) . ?
Fe1 S2 2.2271(12) . ?
Fe1 S4 2.2280(12) . ?
Fe1 S3 2.2312(12) . ?
Fe1 S4 2.5270(12) 2_656 ?
S1 C1 1.755(4) . ?
S2 C2 1.748(4) . ?
S3 C9 1.747(4) . ?
S4 C10 1.756(4) . ?
S4 Fe1 2.5270(12) 2_656 ?
N1 C1 1.310(5) . ?
N1 C3 1.376(5) . ?
N2 C2 1.309(5) . ?
N2 C4 1.367(5) . ?
N3 C9 1.317(5) . ?
N3 C11 1.357(5) . ?
N4 C10 1.311(5) . ?
N4 C12 1.385(5) . ?
N5 C17 1.342(5) . ?
N5 C21 1.350(5) . ?
N5 C22 1.494(5) . ?
C1 C2 1.444(5) . ?
C3 C4 1.402(6) . ?
C3 C5 1.415(6) . ?
C4 C6 1.411(6) . ?
C5 C7 1.358(6) . ?
C5 H5 0.9500 . ?
C6 C8 1.366(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.406(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.431(5) . ?
C11 C13 1.409(6) . ?
C11 C12 1.413(6) . ?
C12 C14 1.403(5) . ?
C13 C15 1.353(6) . ?
C13 H13 0.9500 . ?
C14 C16 1.366(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.399(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.382(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.367(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.369(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.368(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.494(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C28 1.392(6) . ?
C23 C24 1.395(6) . ?
C24 C25 1.384(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.369(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.380(6) . ?
C27 C28 1.387(5) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?

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
S1 Fe1 S2 89.92(4) . . ?
S1 Fe1 S4 169.91(5) . . ?
S2 Fe1 S4 85.55(4) . . ?
S1 Fe1 S3 90.86(4) . . ?
S2 Fe1 S3 157.50(5) . . ?
S4 Fe1 S3 89.91(4) . . ?
S1 Fe1 S4 94.61(4) . 2_656 ?
S2 Fe1 S4 103.97(4) . 2_656 ?
S4 Fe1 S4 95.23(4) . 2_656 ?
S3 Fe1 S4 98.38(4) . 2_656 ?
C1 S1 Fe1 104.29(14) . . ?
C2 S2 Fe1 104.73(14) . . ?
C9 S3 Fe1 105.40(15) . . ?
C10 S4 Fe1 105.76(14) . . ?
C10 S4 Fe1 99.30(12) . 2_656 ?
Fe1 S4 Fe1 84.77(4) . 2_656 ?
C1 N1 C3 116.3(4) . . ?
C2 N2 C4 116.4(4) . . ?
C9 N3 C11 117.7(4) . . ?
C10 N4 C12 115.7(4) . . ?
C17 N5 C21 120.9(4) . . ?
C17 N5 C22 120.1(3) . . ?
C21 N5 C22 119.0(3) . . ?
N1 C1 C2 121.9(4) . . ?
N1 C1 S1 119.0(3) . . ?
C2 C1 S1 119.1(3) . . ?
N2 C2 C1 122.3(4) . . ?
N2 C2 S2 118.9(3) . . ?
C1 C2 S2 118.8(3) . . ?
N1 C3 C4 121.6(4) . . ?
N1 C3 C5 118.9(4) . . ?
C4 C3 C5 119.6(4) . . ?
N2 C4 C3 121.5(4) . . ?
N2 C4 C6 119.4(4) . . ?
C3 C4 C6 119.0(4) . . ?
C7 C5 C3 120.0(5) . . ?
C7 C5 H5 120.0 . . ?
C3 C5 H5 120.0 . . ?
C8 C6 C4 120.5(5) . . ?
C8 C6 H6 119.7 . . ?
C4 C6 H6 119.7 . . ?
C5 C7 C8 120.8(4) . . ?
C5 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C6 C8 C7 120.0(4) . . ?
C6 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
N3 C9 C10 120.7(4) . . ?
N3 C9 S3 119.4(3) . . ?
C10 C9 S3 119.9(3) . . ?
N4 C10 C9 123.6(4) . . ?
N4 C10 S4 117.7(3) . . ?
C9 C10 S4 118.7(3) . . ?
N3 C11 C13 119.8(4) . . ?
N3 C11 C12 121.3(4) . . ?
C13 C11 C12 118.9(4) . . ?
N4 C12 C14 119.6(4) . . ?
N4 C12 C11 120.8(4) . . ?
C14 C12 C11 119.5(4) . . ?
C15 C13 C11 120.2(4) . . ?
C15 C13 H13 119.9 . . ?
C11 C13 H13 119.9 . . ?
C16 C14 C12 120.0(4) . . ?
C16 C14 H14 120.0 . . ?
C12 C14 H14 120.0 . . ?
C13 C15 C16 121.1(4) . . ?
C13 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C14 C16 C15 120.3(4) . . ?
C14 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
N5 C17 C18 119.9(4) . . ?
N5 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 119.5(4) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 119.9(4) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 119.6(4) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
N5 C21 C20 120.3(4) . . ?
N5 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
N5 C22 C23 111.8(3) . . ?
N5 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
N5 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
C28 C23 C24 119.3(4) . . ?
C28 C23 C22 120.6(4) . . ?
C24 C23 C22 120.0(4) . . ?
C25 C24 C23 120.3(4) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 118.8(4) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
C25 C26 C27 122.8(4) . . ?
C25 C26 Br1 118.9(3) . . ?
C27 C26 Br1 118.2(3) . . ?
C26 C27 C28 117.9(4) . . ?
C26 C27 H27 121.0 . . ?
C28 C27 H27 121.0 . . ?
C27 C28 C23 120.8(4) . . ?
C27 C28 H28 119.6 . . ?
C23 C28 H28 119.6 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.109

# Attachment 'ANeves__Et4]2[Fe_alpha-tpdt_2]2.cif'

data_featpdt
_database_code_depnum_ccdc_archive 'CCDC 695834'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H8 Fe2 S12, 2(C8 H20 N)'
_chemical_formula_sum            'C32 H48 Fe2 N2 S12'
_chemical_formula_weight         957.14

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'
N N 0.0061 0.0033 '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'
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   P21/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.5925(6)
_cell_length_b                   11.0890(5)
_cell_length_c                   16.2457(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.464(3)
_cell_angle_gamma                90.00
_cell_volume                     2175.51(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1935
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      21.88

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             996
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7854
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_process_details   'SADABS - Sheldrick 2004'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15151
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_sigmaI/netI    0.1007
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.73
_reflns_number_total             4132
_reflns_number_gt                2219
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SCHAKAL(Keller,1989),Ortep3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The crystals obtained were of poor quality, which results in a weak data set.
Due to slight anisotropy in the CH3 atoms of TEA cation, restraints to
anisotropic parameters were used (ISOR instructions in SHELX97
(Sheldrick,1997).
The terminal thiophenic rings in the anion units showed evidence of disorder in
the displacement parameters of C and S atoms. They were successfully modelled
over two positions with sof 70:30 for S3-C3-C4, and sof 61:39 for S6-C7-C8
and restraints
were used (ISOR and DFIX instructions in SHELX97 (Sheldrick,1997).

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0949P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4132
_refine_ls_number_parameters     273
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1794
_refine_ls_wR_factor_gt          0.1547
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 0.47083(6) 0.05928(8) 0.57955(5) 0.0325(3) Uani 1 1 d . . .
S1 S 0.63433(12) 0.04907(14) 0.54983(10) 0.0368(4) Uani 1 1 d . . .
S2 S 0.45372(15) 0.25288(15) 0.53984(11) 0.0474(5) Uani 1 1 d . A .
S4 S 0.53214(16) -0.08883(15) 0.67414(11) 0.0512(5) Uani 1 1 d . B .
S5 S 0.32970(14) 0.09429(19) 0.63391(11) 0.0553(5) Uani 1 1 d . . .
C1 C 0.5701(7) 0.2768(6) 0.5047(4) 0.054(2) Uani 1 1 d D . .
C2 C 0.6496(6) 0.1899(6) 0.5088(4) 0.0479(17) Uani 1 1 d D A .
S3 S 0.5993(5) 0.4030(4) 0.4541(3) 0.092(2) Uani 0.698(10) 1 d PD A 1
C3 C 0.739(2) 0.226(2) 0.4752(19) 0.084(11) Uani 0.698(10) 1 d PDU A 1
H3 H 0.8016 0.1782 0.4758 0.101 Uiso 0.698(10) 1 calc PR A 1
C4 C 0.7203(15) 0.3364(13) 0.4435(12) 0.110(8) Uani 0.698(10) 1 d PD A 1
H4 H 0.7690 0.3762 0.4171 0.132 Uiso 0.698(10) 1 calc PR A 1
C3A C 0.616(2) 0.389(2) 0.473(2) 0.032(8) Uani 0.302(10) 1 d PDU A 2
H3A H 0.5821 0.4649 0.4762 0.038 Uiso 0.302(10) 1 calc PR A 2
S3A S 0.7459(12) 0.2449(14) 0.4649(10) 0.078(6) Uani 0.302(10) 1 d PD A 2
C4A C 0.703(3) 0.383(2) 0.441(3) 0.0742(2) Uani 0.302(10) 1 d PDU A 2
H4A H 0.7320 0.4440 0.4128 0.089 Uiso 0.302(10) 1 calc PR A 2
C5 C 0.4243(7) -0.1003(7) 0.7229(4) 0.066(2) Uani 1 1 d D . .
C6 C 0.3375(7) -0.0203(8) 0.7068(5) 0.062(2) Uani 1 1 d D B .
C7 C 0.254(2) -0.0300(18) 0.7497(17) 0.051(6) Uani 0.609(14) 1 d PD B 1
H7 H 0.1904 0.0186 0.7427 0.062 Uiso 0.609(14) 1 calc PR B 1
S6 S 0.3992(5) -0.2017(5) 0.7961(3) 0.064(2) Uani 0.609(14) 1 d P B 1
C8 C 0.2884(15) -0.1259(14) 0.8034(10) 0.054(6) Uani 0.609(14) 1 d PDU B 1
H8 H 0.2500 -0.1486 0.8436 0.065 Uiso 0.609(14) 1 calc PR B 1
S6A S 0.2688(8) -0.0822(14) 0.7717(8) 0.106(7) Uani 0.391(14) 1 d PD B 2
C7A C 0.451(2) -0.204(2) 0.7896(18) 0.058(10) Uani 0.391(14) 1 d PD B 2
H7A H 0.5113 -0.2594 0.8058 0.070 Uiso 0.391(14) 1 calc PR B 2
C8A C 0.3606(19) -0.188(2) 0.8164(16) 0.055(9) Uani 0.391(14) 1 d PDU B 2
H8A H 0.3489 -0.2376 0.8609 0.066 Uiso 0.391(14) 1 calc PR B 2
N1 N 0.6095(4) 0.2642(5) 0.8511(3) 0.0448(14) Uani 1 1 d . . .
C10 C 0.5507(7) 0.1451(7) 0.8458(5) 0.066(2) Uani 1 1 d . . .
H10A H 0.5373 0.1123 0.7870 0.079 Uiso 1 1 calc R . .
H10B H 0.4778 0.1583 0.8561 0.079 Uiso 1 1 calc R . .
C11 C 0.6161(10) 0.0516(12) 0.9106(9) 0.149(5) Uani 1 1 d U . .
H11A H 0.6955 0.0690 0.9240 0.223 Uiso 1 1 calc R . .
H11B H 0.6014 -0.0293 0.8858 0.223 Uiso 1 1 calc R . .
H11C H 0.5930 0.0557 0.9633 0.223 Uiso 1 1 calc R . .
C20 C 0.7217(6) 0.2557(9) 0.8407(6) 0.091(3) Uani 1 1 d . . .
H20A H 0.7672 0.2028 0.8862 0.109 Uiso 1 1 calc R . .
H20B H 0.7558 0.3369 0.8488 0.109 Uiso 1 1 calc R . .
C21 C 0.7251(8) 0.2065(9) 0.7527(6) 0.102(3) Uani 1 1 d U . .
H21A H 0.6898 0.1269 0.7433 0.153 Uiso 1 1 calc R . .
H21B H 0.8023 0.1994 0.7516 0.153 Uiso 1 1 calc R . .
H21C H 0.6854 0.2618 0.7073 0.153 Uiso 1 1 calc R . .
C30 C 0.5329(7) 0.3380(8) 0.7823(5) 0.076(3) Uani 1 1 d . . .
H30A H 0.4589 0.3383 0.7923 0.091 Uiso 1 1 calc R . .
H30B H 0.5252 0.2981 0.7264 0.091 Uiso 1 1 calc R . .
C31 C 0.5695(9) 0.4706(11) 0.7761(8) 0.125(4) Uani 1 1 d U . .
H31A H 0.5860 0.5085 0.8328 0.188 Uiso 1 1 calc R . .
H31B H 0.5096 0.5150 0.7357 0.188 Uiso 1 1 calc R . .
H31C H 0.6358 0.4721 0.7559 0.188 Uiso 1 1 calc R . .
C40 C 0.6279(6) 0.3252(8) 0.9351(5) 0.066(2) Uani 1 1 d . . .
H40A H 0.6551 0.4079 0.9303 0.079 Uiso 1 1 calc R . .
H40B H 0.6870 0.2816 0.9781 0.079 Uiso 1 1 calc R . .
C41 C 0.5278(8) 0.3332(9) 0.9678(7) 0.101(3) Uani 1 1 d U . .
H41A H 0.4734 0.3879 0.9311 0.152 Uiso 1 1 calc R . .
H41B H 0.5497 0.3640 1.0268 0.152 Uiso 1 1 calc R . .
H41C H 0.4949 0.2529 0.9668 0.152 Uiso 1 1 calc R . .


_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 S5 2.2313(19) . ?
Fe1 S4 2.2322(19) . ?
Fe1 S2 2.2344(19) . ?
Fe1 S1 2.2469(17) . ?
Fe1 S1 2.4570(17) 3_656 ?
S1 C2 1.730(7) . ?
S1 Fe1 2.4570(17) 3_656 ?
S2 C1 1.738(8) . ?
S4 C5 1.760(8) . ?
S5 C6 1.720(8) . ?
C1 C2 1.377(10) . ?
C1 C3A 1.520(18) . ?
C1 S3 1.715(8) . ?
C2 C3 1.44(3) . ?
C2 S3A 1.686(15) . ?
S3 C4 1.745(15) . ?
C3 C4 1.321(18) . ?
C3A C4A 1.34(2) . ?
S3A C4A 1.637(19) . ?
C5 C6 1.375(11) . ?
C5 C7A 1.550(18) . ?
C5 S6 1.730(9) . ?
C6 C7 1.42(3) . ?
C6 S6A 1.689(13) . ?
C7 C8 1.366(17) . ?
S6 C8 1.660(18) . ?
S6A C8A 1.665(17) . ?
C7A C8A 1.35(2) . ?
N1 C20 1.473(9) . ?
N1 C40 1.481(8) . ?
N1 C30 1.496(9) . ?
N1 C10 1.505(9) . ?
C10 C11 1.539(14) . ?
C20 C21 1.541(12) . ?
C30 C31 1.553(13) . ?
C40 C41 1.503(11) . ?

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
S5 Fe1 S4 90.82(8) . . ?
S5 Fe1 S2 85.68(8) . . ?
S4 Fe1 S2 153.12(7) . . ?
S5 Fe1 S1 167.15(7) . . ?
S4 Fe1 S1 87.23(7) . . ?
S2 Fe1 S1 90.32(7) . . ?
S5 Fe1 S1 97.30(6) . 3_656 ?
S4 Fe1 S1 103.09(7) . 3_656 ?
S2 Fe1 S1 103.79(6) . 3_656 ?
S1 Fe1 S1 95.51(6) . 3_656 ?
C2 S1 Fe1 104.2(2) . . ?
C2 S1 Fe1 101.7(2) . 3_656 ?
Fe1 S1 Fe1 84.49(6) . 3_656 ?
C1 S2 Fe1 102.7(2) . . ?
C5 S4 Fe1 101.7(3) . . ?
C6 S5 Fe1 104.3(3) . . ?
C2 C1 C3A 104.5(12) . . ?
C2 C1 S3 110.0(6) . . ?
C3A C1 S3 10.6(14) . . ?
C2 C1 S2 123.1(5) . . ?
C3A C1 S2 132.2(12) . . ?
S3 C1 S2 126.7(5) . . ?
C1 C2 C3 114.9(11) . . ?
C1 C2 S3A 109.0(8) . . ?
C3 C2 S3A 6.0(14) . . ?
C1 C2 S1 119.5(5) . . ?
C3 C2 S1 125.6(11) . . ?
S3A C2 S1 131.4(8) . . ?
C1 S3 C4 90.8(6) . . ?
C4 C3 C2 110(2) . . ?
C3 C4 S3 114.6(17) . . ?
C4A C3A C1 121(2) . . ?
C4A S3A C2 101.9(14) . . ?
C3A C4A S3A 102(2) . . ?
C6 C5 C7A 128.2(11) . . ?
C6 C5 S6 105.1(6) . . ?
C7A C5 S6 23.7(8) . . ?
C6 C5 S4 122.7(6) . . ?
C7A C5 S4 108.8(10) . . ?
S6 C5 S4 132.2(6) . . ?
C5 C6 C7 121.0(9) . . ?
C5 C6 S6A 98.0(7) . . ?
C7 C6 S6A 23.2(8) . . ?
C5 C6 S5 119.7(6) . . ?
C7 C6 S5 119.3(9) . . ?
S6A C6 S5 142.3(8) . . ?
C8 C7 C6 103(2) . . ?
C8 S6 C5 92.4(6) . . ?
C7 C8 S6 117.7(18) . . ?
C8A S6A C6 98.3(11) . . ?
C8A C7A C5 95.2(18) . . ?
C7A C8A S6A 120(2) . . ?
C20 N1 C40 103.3(5) . . ?
C20 N1 C30 112.6(7) . . ?
C40 N1 C30 109.8(6) . . ?
C20 N1 C10 114.2(6) . . ?
C40 N1 C10 113.6(6) . . ?
C30 N1 C10 103.5(5) . . ?
N1 C10 C11 113.1(7) . . ?
N1 C20 C21 114.1(6) . . ?
N1 C30 C31 115.2(7) . . ?
N1 C40 C41 115.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.73
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.105

# start Validation Reply Form
_vrf_PLAT860_featpdt             
;
PROBLEM: Number of Least-Squares Restraints ....... 67
RESPONSE: The crystals obtained were of poor quality, which results in
a weak data set.
Due to slight anisotropy in the CH3 atoms of TEA cation, restraints to
anisotropic parameters were used (ISOR instructions in SHELX97
(Sheldrick,1997).
The terminal thiophenic rings in the anion units showed evidence of disorder in
the displacement parameters of C and S atoms. They were successfully modelled
over two positions with sof 70:30 for S3-C3-C4, and sof 61:39 for S6-C7-C8
and restraints
were used (ISOR and DFIX instructions in SHELX97 (Sheldrick,1997).
;
_vrf_PLAT241_featpdt             
;
PROBLEM: Check High Ueq as Compared to Neighbors for S6A
RESPONSE: The crystals obtained were of poor quality, which results in
a weak data set.
The terminal thiophenic rings in the anion units showed evidence of disorder in
the displacement parameters of C and S atoms. They were successfully modelled
over two positions with sof 70:30 for S3-C3-C4, and sof 61:39 for S6-C7-C8
and restraints
were used (ISOR and DFIX instructions in SHELX97 (Sheldrick,1997).
;
_vrf_PLAT242_featpdt             
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C3A
RESPONSE:The crystals obtained were of poor quality, which results in a
weak data set.
The terminal thiophenic rings in the anion units showed evidence of disorder in
the displacement parameters of C and S atoms. They were successfully modelled
over two positions with sof 70:30 for S3-C3-C4, and sof 61:39 for S6-C7-C8
and restraints
were used (ISOR and DFIX instructions in SHELX97 (Sheldrick,1997).
;

# Attachment 'ANeves__BrBzPy]2[Fe_alpha-tpdt_2]2.cif'

data_brbzfe
_database_code_depnum_ccdc_archive 'CCDC 695835'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H8 Fe2 S12, 2(C12 H11 Br N)'
_chemical_formula_sum            'C40 H30 Br2 Fe2 N2 S12'
_chemical_formula_weight         1194.90

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'
N N 0.0061 0.0033 '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'
Fe Fe 0.3463 0.8444 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.3573(5)
_cell_length_b                   25.3284(15)
_cell_length_c                   10.0811(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.854(3)
_cell_angle_gamma                90.00
_cell_volume                     2346.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2076
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      19.25

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1196
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2996
_exptl_absorpt_correction_T_max  0.9445
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19152
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4116
_reflns_number_gt                1904
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The poor quality of the crystal results in a weak data set with great value
of Rint (0.12%) which is responsible for the low ratio Unique/expected
reflections (46 %).
The two terminal thiophenic rings showed evidence of disorder in the
displacement parameters of C and S atoms, witch were successfully modelled
over two positions in the case of C7, C8 and S6 with sof 55:45. Restraints
for displacement parameters were applied for atoms C6, C7 and C8
using DFIX and ISOR instructions in SHELXL97 (Sheldrick,1997).
For the C3, C4 and S3 atoms these could not be successfully modelled.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0851P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4116
_refine_ls_number_parameters     290
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1621
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1604
_refine_ls_wR_factor_gt          0.1346
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_restrained_S_all      0.866
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

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 0.04612(10) 0.50854(4) 0.35762(10) 0.0461(3) Uani 1 1 d . . .
Br1 Br 0.43160(13) 0.24010(4) -0.09711(12) 0.1082(5) Uani 1 1 d . . .
S5 S 0.2368(2) 0.56187(8) 0.42594(19) 0.0571(5) Uani 1 1 d . . .
S1 S -0.0552(2) 0.43787(8) 0.2423(2) 0.0603(6) Uani 1 1 d . . .
S2 S 0.14338(19) 0.45583(7) 0.52976(18) 0.0494(5) Uani 1 1 d . . .
S4 S -0.0167(2) 0.55577(8) 0.16759(19) 0.0578(5) Uani 1 1 d . A .
N1 N 0.4200(6) 0.4746(2) 0.2229(6) 0.0494(15) Uani 1 1 d . . .
C5 C 0.1018(8) 0.6091(3) 0.1945(8) 0.0522(19) Uani 1 1 d D . .
C6 C 0.2091(9) 0.6115(3) 0.3056(8) 0.059(2) Uani 1 1 d D A .
C14 C 0.3954(8) 0.4229(3) 0.2906(8) 0.060(2) Uani 1 1 d . . .
H14A H 0.4685 0.4190 0.3749 0.072 Uiso 1 1 calc R . .
H14B H 0.2977 0.4231 0.3148 0.072 Uiso 1 1 calc R . .
C12 C 0.5711(9) 0.5452(4) 0.1905(9) 0.076(3) Uani 1 1 d . . .
H12 H 0.6625 0.5626 0.2114 0.091 Uiso 1 1 calc R . .
C10 C 0.3309(10) 0.5410(4) 0.0680(8) 0.069(2) Uani 1 1 d . . .
H10 H 0.2538 0.5558 0.0039 0.083 Uiso 1 1 calc R . .
C11 C 0.4625(10) 0.5657(3) 0.0993(8) 0.069(2) Uani 1 1 d . . .
H11 H 0.4774 0.5980 0.0557 0.083 Uiso 1 1 calc R . .
C9 C 0.3128(8) 0.4944(3) 0.1313(8) 0.060(2) Uani 1 1 d . . .
H9 H 0.2229 0.4761 0.1095 0.071 Uiso 1 1 calc R . .
C13 C 0.5483(9) 0.4985(3) 0.2535(8) 0.067(2) Uani 1 1 d . . .
H13 H 0.6240 0.4835 0.3185 0.080 Uiso 1 1 calc R . .
C17 C 0.5457(9) 0.3121(3) 0.1124(8) 0.065(2) Uani 1 1 d . . .
H17 H 0.6364 0.2953 0.1120 0.078 Uiso 1 1 calc R . .
C15 C 0.4071(8) 0.3773(3) 0.1996(7) 0.0502(18) Uani 1 1 d . . .
C18 C 0.4227(10) 0.2955(3) 0.0244(9) 0.067(2) Uani 1 1 d . . .
C16 C 0.5373(9) 0.3527(3) 0.2006(8) 0.060(2) Uani 1 1 d . . .
H16 H 0.6217 0.3638 0.2622 0.072 Uiso 1 1 calc R . .
C20 C 0.2860(9) 0.3609(3) 0.1150(9) 0.076(3) Uani 1 1 d . . .
H20 H 0.1951 0.3770 0.1186 0.091 Uiso 1 1 calc R . .
C19 C 0.2925(9) 0.3206(3) 0.0225(11) 0.085(3) Uani 1 1 d . . .
H19 H 0.2083 0.3106 -0.0408 0.102 Uiso 1 1 calc R . .
C1 C -0.0056(7) 0.3868(3) 0.3536(8) 0.058(2) Uani 1 1 d . . .
C2 C 0.0801(7) 0.3920(3) 0.4770(8) 0.056(2) Uani 1 1 d . . .
S3 S -0.0565(3) 0.32188(11) 0.3276(3) 0.1074(10) Uani 1 1 d . . .
C3 C 0.1113(7) 0.3425(2) 0.5627(7) 0.0391(17) Uani 1 1 d . . .
H3 H 0.1686 0.3388 0.6506 0.047 Uiso 1 1 calc R . .
C4 C 0.0388(12) 0.3061(5) 0.4844(14) 0.127(5) Uani 1 1 d U . .
H4 H 0.0393 0.2707 0.5154 0.152 Uiso 1 1 calc R . .
S6 S 0.1061(10) 0.6603(5) 0.0927(8) 0.078(3) Uani 0.547(14) 1 d P A 1
C8 C 0.248(3) 0.6872(10) 0.191(2) 0.063(7) Uani 0.547(14) 1 d PD A 1
H8 H 0.2897 0.7195 0.1697 0.075 Uiso 0.547(14) 1 calc PR A 1
C7 C 0.301(4) 0.6597(15) 0.306(3) 0.080(18) Uani 0.547(14) 1 d PD A 1
H7 H 0.3821 0.6694 0.3734 0.095 Uiso 0.547(14) 1 calc PR A 1
S6A S 0.3121(18) 0.6671(6) 0.2996(16) 0.086(6) Uani 0.453(14) 1 d P A 2
C8A C 0.204(4) 0.6868(14) 0.133(3) 0.076(10) Uani 0.453(14) 1 d PD A 2
H8A H 0.2206 0.7180 0.0854 0.091 Uiso 0.453(14) 1 calc PR A 2
C7A C 0.097(6) 0.6510(17) 0.086(4) 0.10(2) Uani 0.453(14) 1 d PDU A 2
H7A H 0.0325 0.6520 0.0016 0.124 Uiso 0.453(14) 1 calc PR A 2


_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 S5 2.241(2) . ?
Fe1 S4 2.241(2) . ?
Fe1 S2 2.242(2) . ?
Fe1 S1 2.245(2) . ?
Fe1 S2 2.451(2) 3_566 ?
Br1 C18 1.874(8) . ?
S5 C6 1.733(9) . ?
S1 C1 1.718(8) . ?
S2 C2 1.769(7) . ?
S2 Fe1 2.451(2) 3_566 ?
S4 C5 1.736(7) . ?
N1 C9 1.327(9) . ?
N1 C13 1.328(9) . ?
N1 C14 1.515(9) . ?
C5 C6 1.358(10) . ?
C5 C7A 1.517(17) . ?
C5 S6 1.659(10) . ?
C6 C7 1.49(4) . ?
C6 S6A 1.714(13) . ?
C14 C15 1.492(10) . ?
C12 C11 1.340(11) . ?
C12 C13 1.378(10) . ?
C10 C11 1.364(11) . ?
C10 C9 1.367(10) . ?
C17 C16 1.372(10) . ?
C17 C18 1.380(11) . ?
C15 C20 1.350(10) . ?
C15 C16 1.366(9) . ?
C18 C19 1.371(11) . ?
C20 C19 1.392(11) . ?
C1 C2 1.354(10) . ?
C1 S3 1.718(7) . ?
C2 C3 1.519(9) . ?
S3 C4 1.710(12) . ?
C3 C4 1.316(14) . ?
S6 C8 1.65(3) . ?
C8 C7 1.359(19) . ?
S6A C8A 1.86(3) . ?
C8A C7A 1.36(2) . ?

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
S5 Fe1 S4 90.38(8) . . ?
S5 Fe1 S2 86.41(8) . . ?
S4 Fe1 S2 169.22(8) . . ?
S5 Fe1 S1 150.94(9) . . ?
S4 Fe1 S1 88.04(8) . . ?
S2 Fe1 S1 89.78(8) . . ?
S5 Fe1 S2 103.86(8) . 3_566 ?
S4 Fe1 S2 95.92(8) . 3_566 ?
S2 Fe1 S2 94.84(7) . 3_566 ?
S1 Fe1 S2 105.17(8) . 3_566 ?
C6 S5 Fe1 102.5(3) . . ?
C1 S1 Fe1 103.1(2) . . ?
C2 S2 Fe1 104.3(3) . . ?
C2 S2 Fe1 104.2(2) . 3_566 ?
Fe1 S2 Fe1 85.16(7) . 3_566 ?
C5 S4 Fe1 103.0(3) . . ?
C9 N1 C13 121.4(7) . . ?
C9 N1 C14 118.8(6) . . ?
C13 N1 C14 119.8(6) . . ?
C6 C5 C7A 118.5(14) . . ?
C6 C5 S6 112.0(6) . . ?
C7A C5 S6 7.6(19) . . ?
C6 C5 S4 121.0(6) . . ?
C7A C5 S4 120.1(14) . . ?
S6 C5 S4 127.0(6) . . ?
C5 C6 C7 112.0(11) . . ?
C5 C6 S6A 109.9(8) . . ?
C7 C6 S6A 2.2(13) . . ?
C5 C6 S5 122.3(7) . . ?
C7 C6 S5 125.6(10) . . ?
S6A C6 S5 127.6(7) . . ?
C15 C14 N1 110.9(6) . . ?
C11 C12 C13 119.0(8) . . ?
C11 C10 C9 118.3(7) . . ?
C12 C11 C10 121.0(8) . . ?
N1 C9 C10 120.5(7) . . ?
N1 C13 C12 119.8(7) . . ?
C16 C17 C18 120.2(8) . . ?
C20 C15 C16 120.4(7) . . ?
C20 C15 C14 118.5(7) . . ?
C16 C15 C14 121.1(7) . . ?
C19 C18 C17 119.9(8) . . ?
C19 C18 Br1 119.1(7) . . ?
C17 C18 Br1 120.9(7) . . ?
C15 C16 C17 119.8(7) . . ?
C15 C20 C19 120.8(8) . . ?
C18 C19 C20 118.8(8) . . ?
C2 C1 S3 109.4(6) . . ?
C2 C1 S1 124.5(6) . . ?
S3 C1 S1 126.0(5) . . ?
C1 C2 C3 117.4(6) . . ?
C1 C2 S2 118.2(6) . . ?
C3 C2 S2 124.4(6) . . ?
C4 S3 C1 90.1(5) . . ?
C4 C3 C2 102.4(7) . . ?
C3 C4 S3 120.7(8) . . ?
C8 S6 C5 93.5(8) . . ?
C7 C8 S6 115(2) . . ?
C8 C7 C6 107(3) . . ?
C6 S6A C8A 92.2(13) . . ?
C7A C8A S6A 112(2) . . ?
C8A C7A C5 107(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.100

# start Validation Reply Form

_vrf_PLAT241_brbzfe              
;
PROBLEM: Check High Ueq as Compared to Neighbors for C4
RESPONSE: The two terminal thiophenic rings showed evidence of disorder in the
displacement parameters of C and S atoms, witch were successfully modelled
over two positions in the case of C7, C8 and S6 with sof 55:45. For the
C3, C4 and S3 atoms these could not be successfully modelled.

;
_vrf_PLAT242_brbzfe              
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C3
RESPONSE: The two terminal thiophenic rings showed evidence of disorder in the
displacement parameters of C and S atoms, witch were successfully modelled
over two positions
in the case of C7, C8 and S6 with sof 55:45. For the C3, C4 and S3 atoms
these could not be successfully modelled.
;
_vrf_PLAT860_brbzfe              
;
PROBLEM: Number of Least-Squares Restraints ....... 16
RESPONSE: The two terminal thiophenic rings showed evidence of disorder in the
displacement parameters of C and S atoms, witch were successfully modelled
over two positions in the case of C7, C8 and S6 with sof 55:45.
Restraints for displacement parameters were applied for atoms C6, C7 and C8
using DFIX and ISOR instructions in SHELXL97 (Sheldrick,1997).
For the C3, C4 and S3 atoms
these could not be successfully modelled.
;

