3.2.2 化合物 Cs3K4H2[(Si2W18Ta6O78)FeCl2(H2O)2]·15H2O 的合成
化合物 2 的合成方法与化合物 1 的合成方法差不多,只是 Cr(NO3)3·9H2O 被
FeCl3·6H2O 所代替,最终可以得到黄色块状晶体,其产率为 57%。
3.3 化合物的晶体数据
( 1 ) H24Cs5K2CrSi2Ta6W18O90, Mr = 6709, Triclinic, P -1, a =13.066(5) Å, b
=19.265(5), c = 20.892(5) Å, α =97.447°, β = 101.774°, γ = 99.064°, V = 5012(3) Å3,
Z = 4, ρcalcd= 5.749 g cm−3, final R1 = 0.0832 and wR2 = 0.2594 (Rint = 0.0577) for 26084 independent reflections (I > 2σ(I)).
(2)H36Cs3K4FeSi2Ta6W18O95Cl2, Mr = 6689, Monoclinic, C 2/m, a =34.419(5) Å, b
= 16.271(5) Å, c = 21.596(5) Å, α =γ = 90°, β = 114.928°, V = 10968(5) Å3, Z = 4,
ρcalcd= 4.092 g cm−3, final R1 = 0.0473 and wR2 = 0.1407 (Rint = 0.0641) for 28802 independent reflections (I > 2σ(I)).