在加热条件下,发现氯化铵可以使季戊四醇单侧修饰的Anderson型铬钼酸盐发生结构变异,Anderson型多酸母体上的季戊四醇配体由正中心位置异构到非正中心位置(季戊四醇配体的一个烷氧基从取代多酸骨架中的μ3-O桥氧原子异构为取代骨架中的μ2-O桥氧原子),得到其χ同分异构体(NH4)3{χ-[Cr(OH)3Mo6O(18)(OCH2)3CCH2OH]},并通过电喷雾质谱ESI、红外光谱IR和单晶X射线衍射的方法确定了该化合物的结构.晶体测定及分析结果表明,该化合物属单斜晶系,P21/n空间群,晶胞参数a=1.053 68(4)nm,b=2.911 72(6)nm,c=1.124 70(7)nm,α=90°,β=117.45(6)°,γ=90°,Z=4,V=3.062 1(3)nm3.
On heating,ammonium chloride can promote a structural transformation of the single-side pentaerythritol-modified Anderson-type chromohexamolybdate,(NH4)3{δ-[Cr(OH)3Mo6O(18)(OCH2)3 CCH2OH]},to form itsχisomer,(NH4)3{χ-[Cr(OH)3Mo6O(18)(OCH2)3 CCH2OH]},in which the pentaerythritol ligand on the Anderson polyoxometalate precursor isomerizes from the center position to a non-center position(One of its three alkoxy groups of the pentaerythritol ligand substitutes a μ2-O bridging oxygen atom instead of μ3-O bridging oxygen atom in commonδisomers).The structure of theχisomer compound was determined by electrospray ionization mass spectrometry ESI,IR spectroscopy and single crystal X-ray diffraction technique.The results of crystal structure determination and analysis show that theχisomer compound is crystallized in monoclinic space group,P21/n,with unit cell parameter a=1.053 68(4)nm,b=2.911 72(6),c=1.124 70(7)nm,α=90°,β=117.452(6)°,γ=90°,Z=4,V=3.062 1(3)nm~3.