TY  - JOUR
A1  - Sperlich, Eric
A1  - Köckerling, Martin
T1  - Cluster salts [Nb6Cl12(HIm)(6)]A(n) (with HIm=1H-imidazole and A=Mineral Acid Anion, n=1 or 2) made in and with Bronsted-basic ionic liquids and liquid mixtures
JF  - ChemistryOpen
N2  - Four new hexanuclear niobium cluster compounds of the general formula [Nb6Cl12(HIm)(6)](A)(n) . x(solvent molecule) (HIm=1H-imidazole, A=mineral acid anion, Cl- (n=2) (1), (SO4)(2-) (n=1) (2), (CrO4)(2-) (n=1) (3), and (HAsO4)(2-) (n=1) (4)) were prepared. Their synthesis can be done in basic ionic liquids, which form on the addition of a mineral acid, which also delivers the counter anion for the final cluster compound, to an excess of the 1H-imidazole. Some addition of an auxiliary solvent, like methanol, improves the speed of crystallisation. The cluster unit comprises a hexanuclear Nb-6 unit of octahedral shape with the edges bridged by Cl atoms and the exo sites being occupied by N-bonded 1H-imidazole ligands. The cluster cation carries sixteen cluster-based electrons. Between the NH groups of the ligands of the cluster unit, the anions and the co-crystallised water (1), or 1H-imidazole and methanol molecules (2, 3, and 4) a network of hydrogen bonds exists.
KW  - cluster
KW  - ionic liquid
KW  - structure elucidation
KW  - heterocyclic ligand
KW  - Niobium
Y1  - 2021
U6  - https://doi.org/10.1002/open.202000266
SN  - 2191-1363
VL  - 10
IS  - 2
SP  - 248
EP  - 254
PB  - Wiley-VCH
CY  - Weinheim
ER  - 
TY  - JOUR
A1  - Sperlich, Eric
A1  - Köckerling, Martin
T1  - [Nb6Cl12(CH3OH)4(OCH3)2] ⋅ DABCO ⋅ 1.66 CH2Cl2
BT  - cluster units wrapped in a network of hydrogen bonds
JF  - Zeitschrift für anorganische und allgemeine Chemie : ZAAC = Journal of inorganic and general chemistry
N2  - An easy-to-do synthesis for the hexanuclear niobium cluster compound [Nb6Cl12(CH3OH)(4)(OCH3)(2)] . DABCO . 1.66 CH2Cl2 has been developed. An one-pot reaction between the cluster precursor [Nb6Cl14(H2O)(4)] . 4H(2)O and methanol with the addition of DABCO leads to the crystallization of the title compound in high yield within a few minutes. The single-crystal X-ray structure of this cluster compound has been determined. Very strong, nearly symmetric intercluster hydrogen bonds Nb-6-MeO...H...OMe-Nb-6 are present between the cluster units. A bridging co-crystalline DABCO molecule is also involved in a three-dimensional hydrogen-bonding network.
KW  - Niobium
KW  - Cluster
KW  - Hydrogen Bonds
KW  - Synthesis
KW  - Structure Determination
Y1  - 2021
U6  - https://doi.org/10.1002/zaac.202100138
SN  - 0044-2313
SN  - 1521-3749
VL  - 647
IS  - 18
SP  - 1759
EP  - 1763
PB  - Wiley-VCH
CY  - Weinheim
ER  -