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Preparation and crystal structure of the new ternary niobium polysulfide K4Nb2S14 exhibiting the dimeric complex anion [Nb2S14]4− by W Bensch; P Dürichen is a Chemistry article available to read on EtoBox.

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The new ternary niobium polysulfide K 4 Nb 2 S 14 was prepared at low temperatures via the reactive flux method. It crystallizes in the monoclinic space group P2 1 /c with unit cell dimensions of as21.656(2), bs7.8541(9), cs12.455(1) A ̊, bs99.22(1)8 and Zs4. The crystal structure consists of well-separated K q and [Nb 2 S 14 ] 4y ions. The Nb centers are coordinated by S units, S 2y and S anions. 2y 2y 2 4 The title compound is the first transition metal polysulfide in which an S anion acts as a monodentate ligand. According to the different 2y 4 bridging modes of the ligands [Nb 2 S 14 ] 4y may be described as 4y . The Nb centers are in a six-fold coordination and the polyhedra may be described as distorted pentagonal pyramids. The Nb-S interatomic distances vary from 2.189 to 2.949 A ̊. Bond-valence calculations show that the bond valences for these distances range from 0.1 to 1.5. Within the unit cell the anions are stacked parallel to the crystallographic b-axis, and the K q ions are located between the anions. UV-Vis experiments yield an optical gap of E g s2.11 eV.

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Author

W Bensch; P Dürichen

Publisher

Elsevier Science; Elsevier ; Elsevier BV (ISSN 0020-1693)

Published

1997

Language

EN

Field

Chemistry (Physical Sciences)