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Synthesis and characterization of the lead borate Pb6B12O21(OH)(6)

机译:硼酸铅Pb6B12O21(OH)(6)的合成与表征

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摘要

A lead borate with the composition Pb6B12O21(OH)(6) was synthesized through a hydrothermal synthesis, using lead metaborate in combination with sodium nitrate and potassium nitrate. The compound crystallizes in the trigonal, non-centrosymmetric space group P3(2) (no. 145) with the lattice parameters a = 1176.0( 4), c = 1333.0( 4) pm, and V = 0.1596( 2) nm(3). Interestingly, the data of Pb6B12O21(OH)(6) correct the structure of a literature known lead borate with the composition "Pb6B11O18(OH)(9)". For the latter compound, nearly identical lattice parameters of a = 1176.91(7) and c = 1333.62(12) pm were reported, possessing a crystal structure, in which the localization and refinement of one boron atom was obviously overlooked. The structure of Pb6B12O21(OH)(6) is built up from trigonal planar BO3 and tetrahedral BO4 groups forming complex chains. The Pb2+ cations are located between neighboring poly-borate chains. The here reported compound Pb6B12O21(OH)(6) and "Pb6B11O18(OH)(9)" were, however, produced under different synthesis conditions. While "Pb6B11O18(OH)(9)" was synthesized via a hydrothermal synthesis including ethylenediamine and acetic acid, the here reported lead borate Pb6B12O21(OH)(6) could be obtained under moderate hydrothermal conditions (240 degrees C) without the addition of organic reagents.
机译:使用偏硼酸铅结合硝酸钠和硝酸钾,通过水热合成法合成了组成为Pb6B12O21(OH)(6)的硼酸铅。该化合物在晶格参数为a = 1176.0(4),c = 1333.0(4)pm和V = 0.1596(2)nm(3)的三角形非中心对称空间群P3(2)(编号145)中结晶。 )。有趣的是,Pb6B12O21(OH)(6)的数据校正了组成为“ Pb6B11O18(OH)(9)”的文献中已知的硼酸铅的结构。对于后一种化合物,据报道具有几乎相同的晶格参数a = 1176.91(7)和c = 1333.62(12)pm,具有晶格结构,其中明显忽略了一个硼原子的定位和细化。 Pb6B12O21(OH)(6)的结构由形成复杂链的三角形平面BO3和四面体BO4组构建。 Pb2 +阳离子位于相邻的多硼酸盐链之间。然而,本文报道的化合物Pb6B12O21(OH)(6)和“ Pb6B11O18(OH)(9)”是在不同的合成条件下生产的。虽然通过水热合成包括乙二胺和乙酸合成了“ Pb6B11O18(OH)(9)”,但此处报道的硼酸铅Pb6B12O21(OH)(6)可以在中等水热条件下(240摄氏度)获得,而无需添加有机试剂。

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