Two new d0 TM fluoroantimonites, namely, Cs8Sb4Nb5O5F35 and Cs6Sb4Mo3O5F26, have
been synthesized by hydrothermal reactions. Cs8Sb4Nb5O5F35 features a new 0D CS structure formed by Nb2Sb and NbSb2 trinuclear clusters. When the d0 TM Nb5+ was changed to
Mo6+, a new NCS compound, Cs6Sb4Mo3O5F26,
was obtained. It exhibits a novel 2D layered structure composed of 2D molybdenum
antimonitelayers separated by isolated Sb(4)F3 groups and cesium
cations, and is the first example of NCS d0 TM fluoroantimonate. SHG
measurements revealed that Cs6Sb4Mo3O5F26 is a phase-matchable NLO material with SHG response of about 0.72 times that of
KDP. The LIDT of Cs6Sb4Mo3O5F26 was evaluated to be 133.5 MW/cm2, about 33.4 times that of AGS. This
work indicated that d0 TM fluoroantimonate is a promising NLO
material system.