Synthese und Kristallstruktur von TesO10(PO4)4

Synthese und Kristallstruktur von TesO10(PO4)4
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DOI:
10.1524/zkri.1977.145.16.321
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发表时间:
1977
期刊:
--
影响因子:
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通讯作者:
H. Mayer;G. Pupp
H. Mayer;G. Pupp
中科院分区:
其他
文献类型:
--
作者:
H. Mayer;G. Pupp

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首次合成了十氧四正磷酸钠(IV) TegOiofPO^。以TeOi和p2o5氧化物为原料,在550℃下通过化学传递反应得到了该化合物的单晶。晶体为单斜晶,空间群为P2i /n, a = 20.076, b = 4.650, c = 11.220 Α, β = 92.99°,Ζ = 2。用三维x射线衍射数据直接测定了晶体结构,并用最小二乘法将其细化为R = 4.9°/o。晶体结构包括“Zweier-Dreifachketten”(三链)30 [,[TeeOio]4+(平均Te -Ο距离1.954 Ä),在末端氧原子(Te -Ο = 1.896 A)上与另一个碲原子连接。碲原子本身通过共价Te-0 (->P)键与3个正磷酸盐基团紧密相连(1.945,2.092,2.104 Ä)。这导致了带状结构单元[Te«Oio] [Te(P04> - p)]2,它们在正磷酸盐基团的非键氧原子上相互连接,从而形成褶皱层[Te - 0(->- p) = 2.201, 2.288 A]。这些层本身是由正磷酸盐基团的氧原子与相邻层的碲原子之间的弱相互作用维系在一起的[Te··0 (* P) = 2.653, 2.870 A]。
Oetatellurium(IV)decaoxide tetraorthophosphate, TegOiofPO^, has been synthesized for the first time. Single crystals of the compound have been obtained from the oxides TeOi and P 2 O 5 by chemical transport reaction at 550 °C. The crystals are monoclinic, space group P2i /n , with a = 20.076, b = 4.650, c = 11.220 Α, β = 92.99° and Ζ = 2. The crystal structure has been determined by direct methods using three-dimensional x-ray diffraction data and refined by a least-squares method to R = 4.9°/o. The crystal structure comprises "Zweier-Dreifachketten" (triple chain) 3o[,[TeeOio]4+ (average Te—Ο distances 1.954 Ä) which are connected with an other tellurium atom over the terminal oxygen atoms (Te—Ο = 1.896 A). The tellurium atom, itself, is strongly bonded to three orthophosphate groups by covalent Te—0(->P) bonds (1.945, 2.092, 2.104 Ä). This leads to band-like structural units [Te«Oio] [Te(P04>2]2, which are connected with each other over the non-bonded oxygen atoms of the orthophosphat groups thus forming puckered layers [Te—0(->-P) = 2.201, 2.288 A]. The layers themselves are held together by weak interaction between the oxygen atoms of the orthophosphate groups and the tellurium atoms of the adjacent layer [Te· · 0 ( * P ) = 2.653, 2.870 A].