Composition Space of the (CuO, 1/2Nb2O5)/(HF)x·pyridine/H2O System. Structure and Synthesis of [pyH+]2[CuNb2(py)4O2F10]2- and CuNb(py)4OF5
dataset
posted on 1996-02-28, 00:00 authored by Paramasivan Halasyamani, Michael J. Willis, Charlotte L. Stern, Paul M. Lundquist, George K. Wong, Kenneth R. PoeppelmeierSingle 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.
