Synthesis and Crystal Structure of O,O-Dimethyl-N-(β-triphenylgermanyl)propionyl-α- aminobenzylphosphonates

The title compound (C30H32NO4PGe), O,O-dimethyl-N-(β-triphenylgermanyl) propionyl-α-aminobenzylphosphonates was synthesized by a convenient method, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is triclinic, space group P-1 with parameters: a=9.7753(5), b=11.5773(5), c=13.5059(6) ?, α=104.185(1),β= 95.971(1), γ =96.727(1)°, V=1457.63(12) ?3, Z=2, Mr=574.13, Dc=1.308 g/cm3, λ=0.71073 ?, μ = 1.139mm-1, and F(000)=596. The structure was solved by direct methods. The structure was refined to R=0.0257, wR=0.0705 for 5080 observed reflections with I >2σ(I).The result of structure analysis indicates that atom Ge is sp3 hydridized because the arrangement of the four carbon atoms bonded to it is a distorted tetrahedron. The geometry of the three phenyl groups linking with the Ge atom looks like a propeller form.

N-取代氨乙基膦酸为配位中心的Keggin型杂多酸

用Ｎ－取代的β－氨乙基磷酸Ｒ２Ｒ’Ｎ＋ＣＨ２ＣＨ２ＰＯ３Ｈ－（Ｒ＝Ｒ’＝Ｈ；Ｒ＝Ｍｅ，Ｒ’＝Ｈ；Ｒ＝Ｒ’＝Ｍｅ；Ｒ＝Ｈ，Ｒ’＝Ｍｅ２ＣＨ；Ｒ＝Ｈ，Ｒ’＝ＣＨ３（ＣＨ２）２ＣＨ２）为配位中心合成了系列Ｐ：Ｗ比为 １：１２的有机膦－钨杂多酸，用元素分析、红外、紫外光谱、ＴＧ和ＤＳＣ热分析对其进行了结构表征．结果表明，这些有机膦杂多酸具有Ｋｅｇｇｉｎ型结构，可表示为Ｎ＋ＣＨ２ＣＨ２ＰＯ３Ｈ－·Ｗ１２Ｏ３６·ｎＨ２Ｏ．其中铵离子有机侧链Ｒ２Ｒ’Ｎ＋ＣＨ２ＣＨ２与磷酸根ＰＯ３Ｈ一起参与构成杂多阴离子的一级结构，即整个有机磷酸一体作为了杂多阴离子的核心或配位中心．有机磷酸的取代基对杂多酸的结晶水量有显著影响．