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Issue 16, 2018
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Synthesis and crystal structure of solvent-free dodecahydro closo-dodecaborate of nickel, NiB12H12

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Abstract

Nickel closo-dodecaborate NiB12H12 was prepared by mechanosynthesis (ball milling) of mixtures of Na2B12H12 + NiCl2 followed by hydration and drying under dynamic vacuum. The crystal structures of hydrated and anhydrous closo-dodecaborates were characterized by temperature dependent synchrotron radiation X-ray powder diffraction, ab initio calculations, thermal analysis and infrared spectroscopy. Three different water containing complexes were found: a homoleptic octahedral complex in Ni(H2O)6B12H12 crystallizing in two different deformation variants of a complex centred closo-dodecaborate cube, and a heteroleptic octahedral complex in Ni(H2O)4B12H12 containing four water molecules and two hydrogens and centring also a deformed closo-dodecaborate cube. Anhydrous nickel closo-dodecaborate was obtained by drying the hydrated sample under dynamic vacuum. It crystallizes with bcc packing of B12H122− anions and Ni2+ is disordered close to the triangular face of the tetrahedral interstice coordinated by a H5 square pyramid.

Graphical abstract: Synthesis and crystal structure of solvent-free dodecahydro closo-dodecaborate of nickel, NiB12H12

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Article information


Submitted
29 Jan 2018
Accepted
18 Mar 2018
First published
27 Mar 2018

Dalton Trans., 2018,47, 5843-5849
Article type
Paper

Synthesis and crystal structure of solvent-free dodecahydro closo-dodecaborate of nickel, NiB12H12

Y. Sadikin, E. Didelot, Z. Łodziana and R. Černý, Dalton Trans., 2018, 47, 5843
DOI: 10.1039/C8DT00381E

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