Composition Space of the (CuO, <sup>1</sup>/<sub>2</sub>Nb<sub>2</sub>O<sub>5</sub>)/(HF)<i><sub>x</sub></i>·pyridine/H<sub>2</sub>O System. Structure and Synthesis of [pyH<sup>+</sup>]<sub>2</sub>[CuNb<sub>2</sub>(py)<sub>4</sub>O<sub>2</sub>F<sub>10</sub>]<sup>2-</sup> and CuNb(py)<sub>4</sub>OF<sub>5</sub>
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Single crystals of [pyH+]2[CuNb2(py)4O2F10]2- and CuNb(py)4OF5 were synthesized in a (HF)x·pyridine/pyridine/water solution (150 °C, 24 h, autogeneous pressure) using CuO and Nb2O5 as reagents. The compound [pyH+]2[CuNb2(py)4O2F10]2- contains clusters of [CuNb2(py)4O2F10]2- anions linked through N−H+···F hydrogen bonds to the [pyH+] cations. In contrast CuNb(py)4OF5 is a unidimensional compound consisting only of chains, perpendicular to the c axis, of alternating [Cu(py)4(O/F)2/2]0.5+ and [NbF4(O/F)2/2]0.5- octahedra. The chains change direction between the [110] and [11̄0] every c/2. Crystal data for [pyH+]2[CuNb2(py)4O2F10]2-: tetragonal, space group I4122 (No. 98),with a = 11.408(3) Å, c = 30.36(1) Å, and Z = 4. Crystal data for CuNb(py)4OF5: monoclinic, space group C2/c (No. 15), with a = 10.561(3) Å, b = 13.546(6) Å, c = 16.103(4) Å, β = 97.77(2)°, and Z = 4.
