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A more convenient synthesis of the [closo-1-CB9H10]- anion, from the reaction of 6-(NMe3)-nido-6-CB9H11] with piperidine in THF, is reported. Reaction of [NMe4]+[1-CB9H10]- and [(η5-C5Me5)IrCl2]2 gives the ionic species [(η5-C5Me5)2Ir2Cl3]+ [closo-1-CB9H10]- as a yellow crystalline compound. Crystals are orthorhombic, space group Pnma, with a = 2505.9(6), b = 1223.6(3), c = 1029.8(3) ppm, and Z = 4. The structure was refined for 2329 reflections F > 4.0σ(F) to R = 0.0439. Both cation and anion possess crystallographic mirror-plane symmetry. Comparison of the structure of the anion with other formally closo ten-vertex structures reveals a previously unrecognised general opening.

In order to establish the suggestion arising from the assignment of the cluster 11B and 1H NMR shielding behavior, namely, that the title compound (I) is not a closo species, a single‐crystal X‐ray diffraction analysis is carried out (space group P21/c, Z=4).

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