Journal
DALTON TRANSACTIONS
Volume 47, Issue 16, Pages 5843-5849Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/c8dt00381e
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Funding
- Swiss National Science Foundation
- NCN project [2015/17/B/ST3/02478]
- CPU allocation at PL-Grid
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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)(6)B12H12 crystallizing in two different deformation variants of a complex centred closo-dodecaborate cube, and a heteroleptic octahedral complex in Ni(H2O)(4)B12H12 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 H-5 square pyramid.
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