Black single crystals of (OLi2Ca4)(3)[ReN4](4) were prepared from the eleme
nts (molar ratio Li:Ca:Re = 6:1:1) by reaction with molecular nitrogen at 9
00 degreesC; oxygen content results from a leak in the gas supply. The nitr
idorhenal(VI)-oxide is an isotype of (OLi2Ca4)(3)[MN4](4) (M = Mo-VI, W-VI)
. These compounds are obtained under similar reaction conditions in the pre
sence of small amounts of oxygen containing impurities (Li-/Ga-hydroxides).
The crystal structure of (OLi2Ca4)3[ReN4]4 was determined by single crysta
l methods (cubic; 143d (#220); a=1315.X8(9) pm; Z=4) and can be derived fro
m the Th3P4 type structure by hierarchical replacements: Th <(<boolean AND>
)double under bar> (OLi2Ca4)(8+)-tetragonal bipyramids and P <(<boolean AND
>)double under bar> [(ReN4)-N-VI] "-tetrahedra.