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A Hexanuclear Niobium Cluster Compound Crystallizing as Macroscopic Tubes.

ABSTRACT: Compounds with ordered structures in one or two dimensions are exciting materials and investigated intensively in many different areas of science. Many activities have been put into the preparation of low-dimensional nano-scaled structures and many compounds in this size regime are known. Contrary, the number of known compounds that have low-dimensional macroscopic sized structures that form directly in a chemical reaction is very limited. Here, we present the synthesis of the niobium cluster compound [(Et₂ O)₂ H]₂ [Nb₆ Cl₁₈ ], crystals of which grow in form of large hexagonal empty tubes of several centimeter length and diameters in the range of 2?mm. The single-crystal X-ray structure of this compound has been refined. Under warming, the compound readily eliminates diethyl ether molecules and decomposes. From a closer look at the crystallization process a step-by-step scheme of the procedure of the tube growth is proposed. The overall conclusion from this proposal is that a crucial balance between the cluster solution concentration, the crystal growth speed and the ether diffusion speed results in the formation of macroscopic crystal tubes.

SUBMITTER: Konig J

PROVIDER: S-EPMC6900163 | biostudies-literature | 2019 Nov

REPOSITORIES: biostudies-literature

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A Hexanuclear Niobium Cluster Compound Crystallizing as Macroscopic Tubes.

König Jonas J Köckerling Martin M

Chemistry (Weinheim an der Bergstrasse, Germany) 20190930 61

Compounds with ordered structures in one or two dimensions are exciting materials and investigated intensively in many different areas of science. Many activities have been put into the preparation of low-dimensional nano-scaled structures and many compounds in this size regime are known. Contrary, the number of known compounds that have low-dimensional macroscopic sized structures that form directly in a chemical reaction is very limited. Here, we present the synthesis of the niobium cluster co ...[more]

PMID: 31298438

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Project description:A new hexanuclear iron-selenium nitrosyl cluster, [(n-Bu)(4)N](2)[Fe(6)Se(6)(NO)(6)] (1), and a hexanuclear iron-sulfur nitrosyl cluster, [(n-Bu)(4)N](2)[Fe(6)S(6)(NO)(6)] (2), were synthesized by the solvent-thermal reactions of [(n-Bu)(4)N][Fe(CO)(3)NO] with selenium or sulfur in methanol, while a tetranuclear iron-sulfur nitrosyl cluster, (Me(4)N)[Fe(4)S(3)(NO)(7)] (3), was also prepared by the solvent-thermal reaction of FeCl(2).4H(2)O with thiourea in the presence of (CH(3))(4)NCl, NaNO(2), and methanol. Complexes 1-3 were characterized by IR, UV-vis, (1)H NMR, electrochemistry, and single-crystal X-ray diffraction analysis. IR spectra of complexes 1 and 2 show the characteristic NO stretching frequencies at 1694 and 1698 cm(-1), respectively, while the absorptions of complex 3 appear at 1799, 1744, and 1710 cm(-1). The UV-vis spectra of complexes 1-3 show different bands in the range of 259-562 nm, which are assigned to the transitions between orbitals delocalized over the Fe-S cluster, the ligand-to-metal charge transfer, pi*(NO)-d(Fe), and the metal-to-ligand charge transfer, d(Fe)-pi*(NO). Single-crystal X-ray structural analysis reveals that complex 1 crystallizes in the monoclinic P2(1)/n space group with two molecules per unit cell. Two parallel "chair-shaped" structures, consisting of three iron and three selenium atoms, are connected by Fe-Se bonds with an average distance of 2.341 A; each iron center is bonded to three selenium atoms and a nitrogen atom from the nitrosyl ligand with a pseudotetrahedral center geometry. Cyclic voltammograms of complexes 1 and 2 display two cathodic and three anodic current peaks with an unusually strong cathodic peak. Further electrochemical investigations demonstrated that the intensity of the unusually strong peak is a result of at least three processes. One is the quasi-reversible reduction, and the other two are from an irreversible electrochemical process, in which the compound goes through a typical electron transfer and chemical reaction mechanism. Compound 3 shows three quasi-reversible reductions.

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A Hexanuclear Niobium Cluster Compound Crystallizing as Macroscopic Tubes.

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A Hexanuclear Niobium Cluster Compound Crystallizing as Macroscopic Tubes.

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