Synthesis and characterization of four ethylenediamine-templated iron arsenates.
Synthesis and characterization of four ethylenediamine-templated iron arsenates.
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DOI：
10.1021/ic991367b
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发表时间：
2000-04
影响因子：
4.6
通讯作者：
S. Ekambaram;S. C. Sevov
中科院分区：
文献类型：
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作者：
S. Ekambaram;S. C. Sevov
以金属铁、氢氟酸和砷酸以及乙二胺为原料，水热合成了四种新型乙二胺模板化砷酸铁和氟砷酸铁。铁(H2AsO4) (HAsO4) 2. enh2。H2O(1)是一维的，包含链，FeIIIFeIIF2(HAsO4)(AsO4), enh2.2 H2O(2)是层状氟砷酸盐，Fe3(HAsO4)6.enH2.NH3。NH4(3)和Fe2F2(AsO4)2（H2O）。enH2(4)分别为砷酸盐和氟砷酸盐，具有三维开框架型结构。化合物1、3和4只含有Fe(III)，而2是Fe（III）和Fe（II）的混价化合物。通过单晶x射线衍射测定其结构。晶体数据：(1)P2(1), a = 4.762(1) a, b = 16.086(3) a, c = 8.698(2) a, beta = 90.65(3)度，Z = 2；(2) P-1, a = 5.289(1) a, b = 7.573 (1) a, c = 8.888(2) a, alpha = 67.32(3)度，beta = 82.77(3)度，gamma = 69.76(3)度，Z = 1；(3) C2/c, a = 18.384(3) a, b = 8.785(1) a, c = 16.052(2) a, β = 111.11(1)度，Z = 4；(4) Pbca, a = 10.490(2) a, b = 10.090(2) a, c = 20.540(4) a, Z = 8。在1和2的链和层之间，以及在二质子化乙二胺和1、2和4结构的无机部分之间存在强氢键。3中的乙二胺没有氢键，因此它是无序的。这些化合物还通过热重分析、红外光谱、元素分析和磁测量进行了表征。
Four new ethylenediamine-templated iron arsenates and fluoroarsenates have been hydrothermally synthesized from iron metal, hydrofluoric and arsenic acids, and ethylenediamine. Fe(H2AsO4)(HAsO4)2.enH2.H2O (1) is one-dimensional and contains chains, FeIIIFeIIF2(HAsO4)(AsO4).enH2.2H2O (2) is a layered fluoroarsenate, and Fe3(HAsO4)6.enH2.NH3.NH4 (3) and Fe2F2(AsO4)2(H2O).enH2 (4) are an arsenate and a fluoroarsenate, respectively, with three-dimensional open-framework type structures. Compounds 1, 3, and 4 contain Fe(III) only, while 2 is a mixed-valence compound of Fe(III) and Fe(II). The structures were determined from single-crystal X-ray diffraction. Crystal data: (1) P2(1), a = 4.762(1) A, b = 16.086(3) A, c = 8.698(2) A, beta = 90.65(3) degrees, Z = 2; (2) P-1, a = 5.289(1) A, b = 7.573 (1) A, c = 8.888(2) A, alpha = 67.32(3) degrees, beta = 82.77(3) degrees, gamma = 69.76(3) degrees, Z = 1; (3) C2/c, a = 18.384(3) A, b = 8.785(1) A, c = 16.052(2) A, beta = 111.11(1) degrees, Z = 4; (4) Pbca, a = 10.490(2) A, b = 10.090(2) A, c = 20.540(4) A, Z = 8. Strong hydrogen bonding exists between the chains and the layers in 1 and 2, and between the diprotonated ethylenediamine and the inorganic part of the structures of 1, 2, and 4. The ethylenediamine in 3 is not hydrogen bonded, and as a result it is disordered. The compounds are characterized also by thermogravimetric analysis, infrared spectroscopy, elemental analysis, and magnetic measurements.