Synthesis, Crystal Structure and Characterization of Two Rare Earth Substituted Keggin-Type Germanotungstates

摘要

Two germanotungstates based on the dysprosium cations and monovacant Keggin anions [GeW11O39]8-, [(CH3)4N]1.5H3.5[Dy(H2O)2(GeW11O39)]·1.5H2O (1) and [Cu(Hen)(en)]2[Cu(H2O)3]0.5{[Cu(H2en)(Hen)]-[Cu(H2O)3]0.5[Dy(GeW11O39)2]}·1.25H2O (2), have been synthesized and characterized by elemental analysis, inductively coupled plasma (ICP) analysis, IR spectroscopy, thermal analysis, and single-crystal X-ray diffraction. Crystal data for 1: monoclinic, space group C2/c with cell dimensions of a=2.8201(5) nm, b=2.2885(3) nm, c=2.4033(4) nm, =123.875(2)°, V=12.878(4) nm3, Z=8, µ=21.239 mm-1; and for 2: monoclinic, space group P21 with cell dimensions of a=2.12808(5) nm, b=1.63834(4) nm, c=3.18074(4) nm, =93.760(2)°, V=11.0658(5) nm3, Z=4, µ=24.803 mm-1. The Dy3+/[GeW11O39]8- ratio of compound 1 is 1:1, and it displays an interesting one dimensional chainlike arrangement. And the Dy3+/[GeW11O39]8- ratio of compound 2 is 1:2 , and it shows a typical dimeric structure.