#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:21:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180334 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/03/7200333.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_7200333
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         '2(C16 H36 N), C16 H8 Fe2 S12'
_chemical_formula_sum            'C48 H80 Fe2 N2 S12'
_chemical_formula_weight         1181.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.430(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.593(3)
_cell_length_b                   13.734(3)
_cell_length_c                   17.690(3)
_cell_measurement_reflns_used    2154
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.28
_cell_measurement_theta_min      2.59
_cell_volume                     3033.8(11)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.1777
_diffrn_reflns_av_sigmaI/netI    0.1942
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18378
_diffrn_reflns_theta_full        23.43
_diffrn_reflns_theta_max         23.43
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.9133
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.3038
_refine_ls_R_factor_gt           0.1322
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3258
_refine_ls_wR_factor_ref         0.3878
_reflns_number_gt                1637
_reflns_number_total             4339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813242a.txt
_cod_data_source_block           tbafea
_cod_original_cell_volume        3033.8(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7200333
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'
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 . .
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'
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) . . ?
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) . ?
