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Acta Cryst. (2007). E63, m1751-m1752    [ doi:10.1107/S160053680702394X ]

2,2',2''-Nitrilotris(ethylammonium) tetrathioantimonate

M. Poisot, C. Näther and W. Bensch

Abstract top

The crystal structure of the title compound, (C6H21N4)[SbS4], consists of discrete tetrahedral [SbS4]3- anions and discrete tris(2-ethylammonium)amine cations. There are two crystallographically independent cations and anions in the asymmetric unit, all of them located in general positions. The cations and anions are connected by N-H...S hydrogen bonding.

Comment top

During the last decade numerous thioantimonate(III) compounds were synthesized under solvothermal conditions. An intriguing observation is that in the overwhelming cases Sb(III)Sx (x = 3 - 6) are observed and the number of compounds containing Sb(V)S4 is comparably low. Some examples for thioantimonate(V) compounds are (C3H10N)[NiSbS4(C6H18N4)] (Stähler & Bensch, 2002), K3SbS4 (Graf & Schäfer, 1976), (NH4)3SbS4 (Graf et al., 1969), Na3SbS4 × 9 H2O (Mereiter et al., 1979), KAg2SbS4 (Schimek et al., 1996), Rb3SbS4 (Bensch & Dürichen, 1996), Cr(en)3SbS4 (Schur et al., 1998), [Ni(en)3]2SbS4NO3 (en = ethylenediamine) (Schur & Bensch, 2000), [Mn(C6H14N2)3]2[Mn(C6H14N2)2(SbS4)2] × 6 H2O and [Mn(tren)(trenH)]SbS4 (tren = tris(2-ethyl)amine)(Schaefer et al., 2003), [Ni(en)3(enH)]SbS4 (Jia et al., 2004), [Sm(en)4]SbS4 × 0.5 en (Jia, Zhu et al., 2005), [Ln(en)3(H2O)x(µ3 - xSbS4)] (Ln = La, x = 0; Ln = Nd, x = 1) and [Ln(en)4]SbS4 × 0.5en (Ln = Eu, Dy, Yb) (Jia, Zhao et al., 2005. There is also one example where Sb(III) and Sb(V) species coexist in a common anion, i.e., in [Ni(dien)2]2Sb4S9 (R. Stähler et al., 2002). During our ongoing work in the field of solvothermal syntheses of new thioantimonates the title compound was prepared. In the crystal structure of (C6H21N4)SbS4, discrete tetrathioantimonate anions and tris(2-ethylammonium)amine cations coexist. There are two crystallographically independent cations and anions in the asymmetric unit, all of them located in general positions (Fig. 1). The tetrathioantimonate anions show slightly distorted tetrahedral geometry (Table 1), but the values are in the range reported for the above mentioned compounds containing this anion. The tetrathioantimonate anions and the organic cations are arranged in layers, which are parallel to the a b plane (Fig. 2). These layers are interconnected by intermolecular N—H···S hydrogen bonding (Table 2). The Sb(1)S4 anion has two such S···H contacts to the first and four contacts to the second crystallographically independent cation, whereas for the Sb(2)S4 anion it is the other way around.

Related literature top

For structures of related compounds, see: Stähler & Bensch (2002); Graf & Schäfer (1976); Graf et al. (1969); Mereiter et al. (1979); Schimek et al. (1996); Bensch & Dürichen (1996); Schur et al. (1998); Schur & Bensch (2000); Schaefer et al. (2003); Jia et al. (2004); Jia, Zhao et al. (2005); Jia, Zhu et al. (2005); Stähler et al. (2002); Alyea et al. (1995).

Experimental top

A mixture of 0.5 mmol MnSb2S4, 0.5 mmol (NH4)2MoS4, 3 mmol S and 5 ml concentrated tris(2-aminoethyl)amine were heated at 413 K for 7 d followed by cooling to room temperature. The product was identified by X-ray powder diffraction and contained two different phases in approximately equivalent amount: red crystals of [Mn(tren)(trenH)]SbS4 (tren = tris(2-ethyl)amine)(Schaefer et al., 2003), and yellow crystals of the title compound.

Refinement top

All hydrogen atoms were positioned with idealized geometry (amine H atoms allowed to rotate but not to tip) and were refined with fixed isotropic displacement parameters (Uiso(H) = 1.2 Ueq(C)) or 1.5 Ueq(N)) using a riding model with d(C—H) = 0.97 Å and d(N—H) = 0.89 Å. In this structure a pseudo mirror plane and a pseudo center of symmetry are found, but refinement of the structure in the centrosymmetric space group Pnma was not successful and leads to pronounced disorder. The absolue structure was determined on the basis of 544 Friedel pairs.

Computing details top

Data collection: DIF4 (Stoe & Cie, 1992); cell refinement: DIF4; data reduction: REDU4 (Stoe & Cie, 1992); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998) and Diamond (Brandenburg, 1999); software used to prepare material for publication: CIFTAB in SHELXL97.

Figures top
[Figure 1] Fig. 1. : Crystal structure of the title compound with labelling and displacement ellipsoids drawn at the 50% probability level.
[Figure 2] Fig. 2. Crystal structure of the title compound with view along the c axis (hydrogen bonding is not shown for clarity).
2,2',2''-Nitrilotris(ethylammonium) tetrathioantimonate top
Crystal data top
(C6H21N4)[SbS4]F(000) = 1600
Mr = 399.26Dx = 1.828 Mg m−3
Orthorhombic, Pca21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2acCell parameters from 132 reflections
a = 19.7872 (13) Åθ = 13–20°
b = 10.8571 (10) ŵ = 2.46 mm−1
c = 13.5055 (8) ÅT = 293 K
V = 2901.4 (4) Å3Block, orange
Z = 80.2 × 0.1 × 0.1 mm
Data collection top
Stoe AEDII
diffractometer		2898 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.023
graphiteθmax = 27.0°, θmin = 1.9°
Phi scansh = −25→14
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)		k = −13→1
Tmin = 0.738, Tmax = 0.772l = −17→1
6750 measured reflections4 standard reflections every 2 h min
3571 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0261P)2 + 3.7053P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
3571 reflectionsΔρmax = 0.88 e Å−3
277 parametersΔρmin = −0.55 e Å−3
1 restraintAbsolute structure: Flack (1983), 544 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.04 (5)
Crystal data top
(C6H21N4)[SbS4]V = 2901.4 (4) Å3
Mr = 399.26Z = 8
Orthorhombic, Pca21Mo Kα radiation
a = 19.7872 (13) ŵ = 2.46 mm−1
b = 10.8571 (10) ÅT = 293 K
c = 13.5055 (8) Å0.2 × 0.1 × 0.1 mm
Data collection top
Stoe AEDII
diffractometer		2898 reflections with I > 2σ(I)
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)		Rint = 0.023
Tmin = 0.738, Tmax = 0.772θmax = 27.0°
6750 measured reflections4 standard reflections every 2 h min
3571 independent reflections intensity decay: none
Refinement top
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.065Δρmax = 0.88 e Å−3
S = 1.03Δρmin = −0.55 e Å−3
3571 reflectionsAbsolute structure: Flack (1983), 544 Friedel pairs
277 parametersFlack parameter: 0.04 (5)
1 restraint
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. 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 > σ(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sb10.72266 (4)0.49351 (4)0.64960 (3)0.0204 (2)
S10.75959 (10)0.6794 (2)0.7180 (2)0.0305 (5)
S20.7352 (2)0.50371 (16)0.4781 (4)0.0289 (9)
S30.78342 (12)0.3293 (3)0.7154 (3)0.0388 (6)
S40.60811 (12)0.4725 (2)0.6887 (3)0.0318 (5)
Sb20.52627 (4)0.00637 (4)0.83030 (3)0.0196 (2)
S50.48991 (11)−0.1799 (2)0.7655 (3)0.0338 (5)
S60.5162 (2)−0.00107 (17)1.0015 (4)0.0319 (10)
S70.46215 (11)0.1664 (2)0.7672 (2)0.0366 (6)
S80.64036 (11)0.0315 (2)0.7919 (3)0.0338 (5)
N10.2974 (6)−0.0028 (5)1.0178 (10)0.023 (3)
C10.2972 (4)0.1250 (6)0.9832 (6)0.0345 (17)
H1A0.28980.12590.91220.041*
H1B0.25990.16841.01400.041*
C20.3586 (5)0.1882 (9)1.0049 (9)0.034 (3)
H2A0.35480.27320.98330.040*
H2B0.39540.15030.96860.040*
N20.3745 (4)0.1851 (7)1.1154 (6)0.0354 (18)
H1N0.34630.23501.14750.053*
H2N0.41690.20991.12520.053*
H3N0.36970.10861.13790.053*
C30.3304 (4)−0.0849 (7)0.9525 (7)0.0362 (18)
H3A0.3690−0.04250.92420.043*
H3B0.2997−0.10380.89870.043*
C40.3538 (5)−0.1994 (9)0.9943 (10)0.035 (3)
H4A0.3803−0.24220.94460.042*
H4B0.3148−0.25021.00910.042*
N30.3965 (4)−0.1871 (7)1.0885 (7)0.039 (2)
H4N0.4338−0.14441.07510.059*
H5N0.4078−0.26171.11020.059*
H6N0.3727−0.14821.13480.059*
C50.2287 (4)−0.0471 (7)1.0443 (6)0.0316 (16)
H5A0.1979−0.02780.99050.038*
H5B0.2299−0.13591.05150.038*
C60.2022 (8)0.0076 (8)1.1366 (16)0.045 (4)
H6A0.2329−0.01161.19040.054*
H6B0.20100.09641.12940.054*
N40.1343 (4)−0.0365 (7)1.1625 (8)0.0404 (17)
H7N0.1091−0.04111.10800.061*
H8N0.11530.01561.20510.061*
H9N0.1373−0.11081.19010.061*
N110.5448 (7)0.5007 (4)0.9564 (11)0.024 (3)
C110.4766 (4)0.4589 (7)0.9377 (6)0.0307 (15)
H11A0.44660.49050.98850.037*
H11B0.47500.36960.93990.037*
C120.4534 (6)0.5041 (5)0.8357 (12)0.021 (2)
H12A0.45780.59300.83220.025*
H12B0.48180.46830.78470.025*
N120.3826 (4)0.4685 (7)0.8190 (8)0.0431 (18)
H11N0.38110.39360.79240.065*
H12N0.36320.52220.77800.065*
H13N0.36050.46830.87640.065*
C130.5806 (4)0.4188 (7)1.0288 (6)0.0324 (17)
H13A0.55050.39941.08330.039*
H13B0.61950.46171.05550.039*
C140.6045 (5)0.2953 (9)0.9772 (11)0.037 (3)
H14A0.62900.24531.02480.044*
H14B0.56530.24900.95560.044*
N130.6473 (3)0.3202 (7)0.8936 (6)0.0348 (18)
H14N0.62400.36140.84800.052*
H15N0.66190.24950.86810.052*
H16N0.68250.36530.91300.052*
C150.5440 (4)0.6289 (6)0.9983 (6)0.0311 (16)
H15A0.53660.62471.06920.037*
H15B0.50690.67470.96920.037*
C160.6113 (4)0.6975 (10)0.9776 (10)0.032 (3)
H16A0.60690.78400.99420.039*
H16B0.64740.66261.01720.039*
N140.6263 (4)0.6837 (8)0.8743 (7)0.051 (2)
H17N0.61680.60710.85530.077*
H18N0.66990.69910.86390.077*
H19N0.60140.73650.83940.077*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.0172 (4)0.0241 (4)0.0197 (5)0.00031 (15)0.0006 (4)−0.0019 (3)
S10.0332 (10)0.0250 (9)0.0333 (11)−0.0025 (9)−0.0050 (12)−0.0036 (9)
S20.0218 (15)0.042 (2)0.023 (2)0.0020 (7)0.0040 (17)0.0018 (7)
S30.0500 (13)0.0341 (11)0.0321 (12)0.0173 (10)−0.0011 (14)0.0031 (10)
S40.0169 (10)0.0494 (9)0.0290 (12)−0.0009 (10)0.0043 (8)−0.0011 (14)
Sb20.0160 (4)0.0236 (4)0.0192 (5)−0.00037 (14)−0.0011 (4)0.0003 (3)
S50.0403 (12)0.0253 (9)0.0357 (12)−0.0075 (10)−0.0061 (13)−0.0007 (10)
S60.0282 (17)0.050 (2)0.017 (2)−0.0088 (8)−0.0049 (17)0.0021 (7)
S70.0477 (12)0.0282 (10)0.0340 (12)0.0110 (10)−0.0064 (15)−0.0007 (9)
S80.0183 (10)0.0532 (10)0.0298 (12)−0.0053 (11)0.0017 (9)−0.0123 (14)
N10.008 (4)0.041 (6)0.020 (6)0.000 (2)−0.004 (4)0.000 (2)
C10.038 (4)0.038 (4)0.028 (4)−0.008 (4)−0.009 (4)0.014 (3)
C20.045 (5)0.019 (4)0.036 (6)0.004 (4)0.021 (5)0.011 (4)
N20.039 (4)0.028 (3)0.039 (5)0.001 (3)−0.006 (3)−0.001 (3)
C30.027 (4)0.048 (5)0.033 (5)0.003 (3)0.003 (4)−0.008 (4)
C40.041 (5)0.029 (5)0.034 (6)0.001 (4)0.002 (5)−0.008 (4)
N30.043 (4)0.024 (3)0.051 (5)0.008 (3)−0.007 (4)−0.001 (3)
C50.023 (4)0.042 (4)0.030 (4)−0.012 (4)0.000 (4)−0.004 (4)
C60.020 (6)0.069 (9)0.047 (10)−0.004 (4)−0.001 (7)−0.006 (5)
N40.029 (4)0.063 (4)0.029 (4)−0.005 (4)0.000 (3)0.004 (5)
N110.028 (5)0.017 (5)0.029 (6)0.0012 (19)−0.012 (5)−0.001 (2)
C110.020 (4)0.045 (4)0.028 (4)0.000 (4)−0.001 (3)0.000 (4)
C120.018 (5)0.025 (4)0.019 (5)−0.005 (2)−0.007 (5)0.006 (3)
N120.020 (3)0.083 (4)0.027 (4)−0.009 (4)−0.006 (3)0.003 (5)
C130.036 (4)0.039 (4)0.022 (4)−0.003 (3)−0.004 (4)0.000 (3)
C140.037 (5)0.023 (5)0.051 (7)0.001 (4)−0.003 (5)0.006 (4)
N130.037 (4)0.033 (3)0.035 (4)0.000 (3)−0.010 (3)−0.007 (3)
C150.024 (4)0.038 (4)0.031 (4)0.011 (3)−0.007 (3)−0.006 (3)
C160.018 (4)0.037 (5)0.042 (7)0.000 (4)−0.005 (4)−0.001 (5)
N140.050 (5)0.036 (4)0.068 (6)0.000 (4)0.024 (4)−0.001 (4)
Geometric parameters (Å, °) top
Sb1—S32.326 (3)C6—H6B0.9700
Sb1—S22.333 (5)N4—H7N0.8900
Sb1—S12.337 (3)N4—H8N0.8900
Sb1—S42.338 (3)N4—H9N0.8900
Sb2—S72.314 (3)N11—C111.445 (14)
Sb2—S52.319 (3)N11—C131.499 (13)
Sb2—S62.323 (5)N11—C151.503 (9)
Sb2—S82.332 (3)C11—C121.532 (17)
N1—C31.414 (13)C11—H11A0.9700
N1—C11.463 (9)C11—H11B0.9700
N1—C51.486 (13)C12—N121.472 (13)
C1—C21.427 (13)C12—H12A0.9700
C1—H1A0.9700C12—H12B0.9700
C1—H1B0.9700N12—H11N0.8900
C2—N21.525 (14)N12—H12N0.8900
C2—H2A0.9700N12—H13N0.8900
C2—H2B0.9700C13—C141.583 (12)
N2—H1N0.8900C13—H13A0.9700
N2—H2N0.8900C13—H13B0.9700
N2—H3N0.8900C14—N131.437 (15)
C3—C41.441 (13)C14—H14A0.9700
C3—H3A0.9700C14—H14B0.9700
C3—H3B0.9700N13—H14N0.8900
C4—N31.534 (15)N13—H15N0.8900
C4—H4A0.9700N13—H16N0.8900
C4—H4B0.9700C15—C161.551 (12)
N3—H4N0.8900C15—H15A0.9700
N3—H5N0.8900C15—H15B0.9700
N3—H6N0.8900C16—N141.434 (16)
C5—C61.48 (2)C16—H16A0.9700
C5—H5A0.9700C16—H16B0.9700
C5—H5B0.9700N14—H17N0.8900
C6—N41.469 (16)N14—H18N0.8900
C6—H6A0.9700N14—H19N0.8900
S3—Sb1—S2111.14 (11)C6—N4—H7N109.5
S3—Sb1—S1110.43 (13)C6—N4—H8N109.5
S2—Sb1—S1108.56 (10)H7N—N4—H8N109.5
S3—Sb1—S4109.88 (11)C6—N4—H9N109.5
S2—Sb1—S4109.39 (14)H7N—N4—H9N109.5
S1—Sb1—S4107.34 (10)H8N—N4—H9N109.5
S7—Sb2—S5110.24 (12)C11—N11—C13111.6 (7)
S7—Sb2—S6110.23 (12)C11—N11—C15110.3 (9)
S5—Sb2—S6108.60 (11)C13—N11—C15107.9 (9)
S7—Sb2—S8111.17 (11)N11—C11—C12109.6 (9)
S5—Sb2—S8108.58 (10)N11—C11—H11A109.8
S6—Sb2—S8107.95 (14)C12—C11—H11A109.8
C3—N1—C1113.5 (10)N11—C11—H11B109.8
C3—N1—C5111.7 (7)C12—C11—H11B109.8
C1—N1—C5112.4 (8)H11A—C11—H11B108.2
C2—C1—N1112.9 (8)N12—C12—C11109.8 (10)
C2—C1—H1A109.0N12—C12—H12A109.7
N1—C1—H1A109.0C11—C12—H12A109.7
C2—C1—H1B109.0N12—C12—H12B109.7
N1—C1—H1B109.0C11—C12—H12B109.7
H1A—C1—H1B107.8H12A—C12—H12B108.2
C1—C2—N2111.5 (8)C12—N12—H11N109.5
C1—C2—H2A109.3C12—N12—H12N109.5
N2—C2—H2A109.3H11N—N12—H12N109.5
C1—C2—H2B109.3C12—N12—H13N109.5
N2—C2—H2B109.3H11N—N12—H13N109.5
H2A—C2—H2B108.0H12N—N12—H13N109.5
C2—N2—H1N109.5N11—C13—C14110.9 (8)
C2—N2—H2N109.5N11—C13—H13A109.5
H1N—N2—H2N109.5C14—C13—H13A109.5
C2—N2—H3N109.5N11—C13—H13B109.5
H1N—N2—H3N109.5C14—C13—H13B109.5
H2N—N2—H3N109.5H13A—C13—H13B108.1
N1—C3—C4116.6 (9)N13—C14—C13111.2 (7)
N1—C3—H3A108.1N13—C14—H14A109.4
C4—C3—H3A108.1C13—C14—H14A109.4
N1—C3—H3B108.1N13—C14—H14B109.4
C4—C3—H3B108.1C13—C14—H14B109.4
H3A—C3—H3B107.3H14A—C14—H14B108.0
C3—C4—N3115.2 (8)C14—N13—H14N109.5
C3—C4—H4A108.5C14—N13—H15N109.5
N3—C4—H4A108.5H14N—N13—H15N109.5
C3—C4—H4B108.5C14—N13—H16N109.5
N3—C4—H4B108.5H14N—N13—H16N109.5
H4A—C4—H4B107.5H15N—N13—H16N109.5
C4—N3—H4N109.5N11—C15—C16111.6 (8)
C4—N3—H5N109.5N11—C15—H15A109.3
H4N—N3—H5N109.5C16—C15—H15A109.3
C4—N3—H6N109.5N11—C15—H15B109.3
H4N—N3—H6N109.5C16—C15—H15B109.3
H5N—N3—H6N109.5H15A—C15—H15B108.0
C6—C5—N1113.4 (8)N14—C16—C15107.6 (9)
C6—C5—H5A108.9N14—C16—H16A110.2
N1—C5—H5A108.9C15—C16—H16A110.2
C6—C5—H5B108.9N14—C16—H16B110.2
N1—C5—H5B108.9C15—C16—H16B110.2
H5A—C5—H5B107.7H16A—C16—H16B108.5
N4—C6—C5113.2 (11)C16—N14—H17N109.5
N4—C6—H6A108.9C16—N14—H18N109.5
C5—C6—H6A108.9H17N—N14—H18N109.5
N4—C6—H6B108.9C16—N14—H19N109.5
C5—C6—H6B108.9H17N—N14—H19N109.5
H6A—C6—H6B107.7H18N—N14—H19N109.5
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N2—H1N···S1i0.892.483.336 (7)161
N3—H4N···S60.892.463.327 (9)164
N3—H5N···S4ii0.892.543.383 (8)158
N3—H6N···S8ii0.892.483.307 (9)154
N4—H7N···S6iii0.892.383.217 (10)157
N4—H8N···S7iv0.892.393.240 (9)159
N12—H12N···S3v0.892.413.259 (9)160
N12—H13N···S2i0.892.363.184 (10)154
N13—H14N···S40.892.493.316 (8)155
N13—H15N···S80.892.623.425 (8)152
N13—H16N···S2vi0.892.383.267 (8)172
N14—H19N···S5vii0.892.593.410 (9)155
Symmetry codes: (i) −x+1, −y+1, z+1/2; (ii) −x+1, −y, z+1/2; (iii) x−1/2, −y, z; (iv) −x+1/2, y, z+1/2; (v) x−1/2, −y+1, z; (vi) −x+3/2, y, z+1/2; (vii) x, y+1, z.
Table 1
Selected geometric parameters (Å, °) top
Sb1—S32.326 (3)Sb2—S72.314 (3)
Sb1—S22.333 (5)Sb2—S52.319 (3)
Sb1—S12.337 (3)Sb2—S62.323 (5)
Sb1—S42.338 (3)Sb2—S82.332 (3)
S3—Sb1—S2111.14 (11)S7—Sb2—S5110.24 (12)
S3—Sb1—S1110.43 (13)S7—Sb2—S6110.23 (12)
S2—Sb1—S1108.56 (10)S5—Sb2—S6108.60 (11)
S3—Sb1—S4109.88 (11)S7—Sb2—S8111.17 (11)
S2—Sb1—S4109.39 (14)S5—Sb2—S8108.58 (10)
S1—Sb1—S4107.34 (10)S6—Sb2—S8107.95 (14)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N2—H1N···S1i0.892.483.336 (7)161
N3—H4N···S60.892.463.327 (9)164
N3—H5N···S4ii0.892.543.383 (8)158
N3—H6N···S8ii0.892.483.307 (9)154
N4—H7N···S6iii0.892.383.217 (10)157
N4—H8N···S7iv0.892.393.240 (9)159
N12—H12N···S3v0.892.413.259 (9)160
N12—H13N···S2i0.892.363.184 (10)154
N13—H14N···S40.892.493.316 (8)155
N13—H15N···S80.892.623.425 (8)152
N13—H16N···S2vi0.892.383.267 (8)172
N14—H19N···S5vii0.892.593.410 (9)155
Symmetry codes: (i) −x+1, −y+1, z+1/2; (ii) −x+1, −y, z+1/2; (iii) x−1/2, −y, z; (iv) −x+1/2, y, z+1/2; (v) x−1/2, −y+1, z; (vi) −x+3/2, y, z+1/2; (vii) x, y+1, z.
Acknowledgements top

This work is supported by the state of Schleswig-Holstein and the Fonds der Chemischen Industrie.

references
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