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Hydrothermal synthesis and characterization of new hybrid open-framework indium phosphate-oxalates

机译：新型混合开放骨架磷酸铟草酸酯的水热合成与表征

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摘要

Three new hybrid open-framework indium phosphate-oxalates, I, Na[InPO_4(C_2O_4)_(0.5)] centre dot H_2O II, [C_2N_2-H_(10)]_(0.5)[InPO_4(C_2O_4)_(0.5)] III, [C_3N_2H_(12)]_(0.5)[In_2(PO_4)(HPO_4)(C_2-O_4)] centre dot H_2O have been hydrothermally synthesized by using organic amines such as ethylamine, 1,3-diaminopropane and alkali metal ions such as Na~+ as structure-directing agents (SDA). The structures of these compounds were characterized by single crystal X-ray diffraction. The structure of I consists of InO_6 octahedra that are linked by phosphate and oxalate groups to generate a three-dimensional framework with intersecting 8-membered ring (MR) channels parallel to the [100] and [010] directions. The structure of II is similar to that of I except that its guest species are protonated ethylamines. III is built from indiumphosphate double-six-rings second building units linked by oxalate units, resulting in large circular 16 MR channels. Single crystal X-ray diffraction measurements show that the SDA of I-III are located in their channels. Crystal data for these three indium phosphate-oxalates are as follows: I, triclinic, space group: P-1 (No. 2), a = 5.5662(17)A, b = 6.454(2)A, c = 8.966(3)A, alpha = 102.609(4) deg, beta=107.319(3) deg, gamma= 94.426(4) deg, V = 296.56(16)A~3, Z = 2, M = 294.81, rho_(calcu) = 3.301 g/cm~3, R1 = 0.0275, wR2 = 0.0731. II, triclinic, space group: P-1 (No. 2), a = 5.653(4)A, b = 6.627(4)A, c = 9.391(8)A, alpha = 70.788(8) deg, beta=75.836(12) deg, gamma= 89.681(9) deg, V = 321.1(4)A~3, Z = 2, M = 283.85, rho_(calcu) = 2.936 g/cm~3, R1= 0.0664, wR2 = 0.1572. III, orthorhombic, space group: Pccm (No. 49), a = 10.350(2) A, b = 12.190(2)A, c = 13.000(3)A, V = 1640.2(6)A~3, Z = 4, M =272.32, rho_(calcu) = 2.206 g/cm~3, R1=0.0691, wR2 = 0.1831.
机译：三种新的杂化开放骨架磷酸铟草酸酯，I，Na [InPO_4（C_2O_4）_（0.5）]中心点H_2O II，[C_2N_2-H_（10）] _（0.5）[InPO_4（C_2O_4）_（0.5） ] III，通过使用有机胺如乙胺，1，3-二氨基丙烷和碱金属水热合成[C_3N_2H_（12）] _（0.5）[In_2（PO_4）（HPO_4）（C_2-O_4）]中心点H_2O Na +等离子作为结构导向剂（SDA）。这些化合物的结构通过单晶X射线衍射表征。 I的结构由InO_6八面体组成，这些八面体通过磷酸酯基团和草酸酯基团连接以生成三维结构，该结构具有相交的平行于[100]和[010]方向的8元环（MR）通道。 II的结构类似于I的结构，除了其客体是质子化的乙胺。 III是由磷酸铟双六环第二建筑单元（由草酸酯单元连接）构建而成的，形成了大型环形16 MR通道。单晶X射线衍射测量表明，I-III的SDA位于它们的通道中。这三种磷酸草酸铟的晶体数据如下：I，三斜晶系，空间群：P-1（2号），a = 5.5662（17）A，b = 6.454（2）A，c = 8.966（3） A），alpha = 102.609（4）度，beta = 107.319（3）度，γ= 94.426（4）度，V = 296.56（16）A〜3，Z = 2，M = 294.81，rho_（calcu）= 3.301 g / cm〜3，R1 = 0.0275，wR2 = 0.0731。 II，三斜线，空间群：P-1（2号），a = 5.653（4）A，b = 6.627（4）A，c = 9.391（8）A，alpha = 70.788（8）度，beta = 75.836（12）度，γ= 89.681（9）度，V = 321.1（4）A〜3，Z = 2，M = 283.85，rho_（calcu）= 2.936 g / cm〜3，R1 = 0.0664，wR2 = 0.1572。 III，正交，空间群：Pccm（No. 49），a = 10.350（2）A，b = 12.190（2）A，c = 13.000（3）A，V = 1640.2（6）A〜3，Z =在图4中，M ＝ 272.32，rho_（计算）＝ 2.206g / cm〜3，R1 ＝ 0.0691，wR2 ＝ 0.1831。

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