μ-(Acetic acid)-di-μ-chlorido-bis[tri­phenyl­tellurium(IV)] monohydrate

Feng Hu; Chao Xu; Hua-Tian Shi; Qun Chen; Qian-Feng Zhang

doi:10.1107/S160053681301739X

. 2013 Jun 29;69(Pt 7):o1171. doi: 10.1107/S160053681301739X

μ-(Acetic acid)-di-μ-chlorido-bis[triphenyltellurium(IV)] monohydrate

Feng Hu ^a, Chao Xu ^a, Hua-Tian Shi ^a, Qun Chen ^b, Qian-Feng Zhang ^a,^b,^*

PMCID: PMC3770430 PMID: 24046715

Abstract

The asymmetric unit of the title compound, C₃₈H₃₄Cl₂O₂Te₂·H₂O, contains two independent Te^IV cations, each coordinated by three phenyl ligands, two Cl⁻ anions and one acetic acid molecule in a distorted octahedral C₃Cl₂O geometry; the longer Te⋯Cl distances ranging from 3.2007 (11) to 3.4407 (11) Å and the longer Te⋯O distances of 3.067 (3) and 3.113 (3) Å indicate the weak bridge coordination. The Cl⁻ anion and acetic acid molecule bridge the two independent Te^IV cations, forming the dimeric complex molecule, in which the Te⋯Te separation is 3.7314 (4) Å. In the crystal, the water molecules of crystallization link the Te^IV complex molecules into chains running along the b-axis direction via O—H⋯O and O—H⋯Cl hydrogen bonds.

Related literature

For background to organotelluronium salts: see: Collins et al. (1988 ▶); Oilunkaniemi et al. (2001 ▶); Ziolo & Extine (1980 ▶); Ziolo & Troup (1979 ▶); Zhou et al. (1994 ▶). For related structures, see: Jeske et al. (1996 ▶); Oilunkaniemi et al. (2001 ▶). For a description of the Cambridge Structural Database, see: Allen (2002 ▶).

Experimental

Crystal data

C₃₈H₃₄Cl₂O₂Te₂·H₂O
M _r = 866.77
Monoclinic,
a = 13.9469 (6) Å
b = 9.3616 (4) Å
c = 27.7941 (12) Å
β = 96.584 (1)°
V = 3605.0 (3) Å³
Z = 4
Mo Kα radiation
μ = 1.80 mm⁻¹
T = 296 K
0.22 × 0.15 × 0.12 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.692, T _max = 0.813
23122 measured reflections
8145 independent reflections
6494 reflections with I > 2σ(I)
R _int = 0.033

Refinement

R[F ² > 2σ(F ²)] = 0.032
wR(F ²) = 0.078
S = 1.08
8145 reflections
407 parameters
H-atom parameters constrained
Δρ_max = 0.85 e Å⁻³
Δρ_min = −0.51 e Å⁻³

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S160053681301739X/xu5713sup1.cif

e-69-o1171-sup1.cif^{(25.2KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681301739X/xu5713Isup2.hkl

e-69-o1171-Isup2.hkl^{(398.5KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Te1—C11	2.129 (3)
Te1—C21	2.124 (3)
Te1—C31	2.116 (3)
Te1—Cl1	3.2366 (9)
Te1—Cl2	3.4407 (11)
Te1—O1	3.067 (3)
Te2—C41	2.129 (4)
Te2—C51	2.126 (4)
Te2—C61	2.118 (4)
Te2—Cl1	3.2802 (9)
Te2—Cl2	3.2007 (11)
Te2—O1	3.113 (3)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2A⋯O1W	0.84	2.13	2.972 (5)	174
O1W—H1W⋯Cl2ⁱ	0.88	2.38	3.205 (4)	155
O1W—H2W⋯Cl2ⁱⁱ	0.87	2.41	3.200 (4)	152

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Symmetry codes: (i) Inline graphic ; (ii) .

Acknowledgments

This project was supported by the Natural Science Foundation of China (90922008).

supplementary crystallographic information

Comment

Organotelluronium salts, R₃TeX, have attracted considerable interest because of their application in organic synthetic chemistry (Zhou et al., 1994). In the past several decades, a large number of triorganotelluronium salts have been prepared and many of their structures have been determined. Previous studies on such triorganotelluronium salts have shown that the salts have relatively complex structures due to weak bonding interactions between the tellurium atom and the anion (Ziolo & Extine, 1980). It has become evident that the interactions are sensitive to the nature of both them. Moreover, the structural features are also influenced by the organic groups and the presence or absence of solvent of crystallization (Ziolo & Troup, 1979). The X-ray structure determinations of several (Ph₃Te)X (X = halide, SCN^-, NCO^-, [NO₃]^-, ¹/₂[SO₄]^2-, ¹/₂[Hg₂Cl₆]^2-, ¹/₂[PtCl₆]^2-, ¹/₂[IrCl₆]^2- and [AuCl₄]^-) salts have established that in the solid state the structural features are governed by weak secondary tellurium-anion interactions which may result in the trigonal pyramidal geometry around tellurium into a five- or six-coordinate entity (Collins et al., 1988; Oilunkaniemi et al., 2001; Ziolo & Extine, 1980; Ziolo & Troup, 1979). In this paper, we report the structural characterization of bis(µ₂-chloride)-(µ₂-acetic acid-O)- bis(triphenyltelluronium) hydrate monosolvate which is expected to expand the pool of the known organotelluronium chemistry.

The structure of the title compound, (µ-Cl)₂(µ-CH₃COOH)(Ph₃Te)₂.H₂O (HAc = CH₃COOH), consists of two Ph₃Te⁺ cations, two chloride anions, one acetic acid molecule and one water molecule linked by a complex network of Te···Cl and Te···O secondery bonds and hydrogen bonds into infinate chains. The geometry around the tellurium atom is pseudo-octahedral, with three phenyl groups, two chloride atoms and one oxygen atom from the acetic acid. The two Ph₃Te⁺ cations occupy on the opposite trigonal faces of octahedra, as shown in Fig. 1. The two tellurium atoms form two secondary bonds of 3.068 (4) and 3.113 (4) Å invoving the oxygen atom of the acetic acid molecule, which are longer than those in (Ph₃Te)₂SO₄.5H₂O (av. 2.797 (9) Å) (Collins et al., 1988), but are still shorter than the sum of the van der Waals radii of the tellurium and oxygen atoms. The two bridging Te···Cl distances involving non-hydrogen-bonded Cl(1) atom are almost equal (3.236 (3) and 3.279 (3) Å), while those involving hydrogen-bonded Cl(2) atom are inequal (3.199 (3) and 3.439 (3) Å). The average Te···Cl distances of 3.288 (3) Å in the title compound is in the range of the van der Waals radii of the tellurium and chloride atoms. The Ph₃Te⁺ cation in the title compound has its expected structure as well as normal distances and angles (Allen, 2002), for example, the six Te—C bond lengths in the two cations are normal and have a mean value 2.124 (4) Ph₃Te⁺ (Jeske et al., 1996). The [(µ-Cl)₂(µ-HAc)(Ph₃Te)₂] moieties are further linked by two kinds of the intermolecular hydrogen bonds of (H₂O)O—H···Cl (av. O···Cl = 3.205 (4) Å) and (HAc)O—H···O(H₂O) (O···O = 2.962 (2) Å), forming one-dimensional infinate chains (see Fig. 2).

Experimental

Ph₃TeCl (212 mg, 0.55 mmol) in water (5 mL) was added into a hot aqueous solution (5 mL) containing the acetic acid (69%, 0.025 mL, 0.22 mmol). A pale brown precipitate was obtained almost immediately. The precipitate was filtered, washed with water and Et₂O, and dried. Recrystallization from acetone-water (1:1) at room temperature afforded brown block crystals suitable for X-ray diffraction. Yield: 140 mg (57%).