#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:21:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180334 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/03/7200334.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_7200334
loop_
_publ_author_name
'Neves, Ana Isabel Soares'
'Santos, Isabel Cordeiro'
'Belo, Dulce'
'Almeida, Manuel'
_publ_section_title
;
 Cation and ligand roles in the coordination of FeIII bisdithiolene
 complexes; the crystal structures of (BrBzPy)2[Fe(qdt)2]2 and
 [Fe(α-tpdt)2]22− salts
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1046
_journal_paper_doi               10.1039/b813242a
_journal_volume                  11
_journal_year                    2009
_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
_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                100.625(3)
_cell_angle_beta                 98.672(3)
_cell_angle_gamma                106.991(3)
_cell_formula_units_Z            1
_cell_length_a                   7.3129(4)
_cell_length_b                   11.4865(7)
_cell_length_c                   17.0461(11)
_cell_measurement_reflns_used    1662
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.52
_cell_volume                     1313.60(14)
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11335
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_T_max  0.9528
_exptl_absorpt_correction_T_min  0.5691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0424
_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)+(0.0302P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                3157
_reflns_number_total             4957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813242a.txt
_cod_data_source_block           brfqdt
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7200334
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
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 . .
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'
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 . . ?
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 . ?
