STEREOCHEMISTRY OF DISCRETE 8-COORDINATION .3. TETRASODIUM TETRAKISOXALATOZIRCONATE(IV) TRIHYDRATE
STEREOCHEMISTRY OF DISCRETE 8-COORDINATION .3. TETRASODIUM TETRAKISOXALATOZIRCONATE(IV) TRIHYDRATE
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DOI：
10.1021/ic50006a003
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发表时间：
1963-01-01
影响因子：
4.6
通讯作者：
SILVERTON, JV
中科院分区：
文献类型：
--
作者：
GLEN, GL;HOARD, JL;SILVERTON, JV
来自Na 4 Zr（C2 O 4）4·3 H2O的正交晶体的在0<（sin 0）/< 0.95范围内的三维[hkl] X射线数据产生结构的确定性确定。[1][2][3][4][5][6][7][8][10][11]复杂的晶体排列主要由钠离子与气态氧的直接相互作用决定（水分子被归入填料的角色），并且Zr（C2 O 4）4 - 4离子显著偏离42 m对称性。这种扭曲是有限的，以及在可能的实验精度，内部的协调组，即化学上最不稳定和结构上最不刚性的复杂的一部分。结构上不等价的平行四边形是平坦的，并且除了Zr-0键长的一些变化之外，几乎是等维的。键参数，包括平均Zr-0键长2.199 A.，与其他报告数据的合成非常一致。0.06 μ m的结构显著差异。- 和Zr-Os类型的平均键长之间（参见，HS）覆盖了内部协调组的扭曲。
Three-dimensional [hkl] X-ray data in the range 0<(sin 0)/< 0.95 from orthorhombic crystals of Na4Zr (C204) 4-3H20 yield a definitive determination of structure. The'tetrakisoxalatozirconate (IV) ion, required by the space group (B22i2) to have a single twofold axis, belongs in fact to the dodecahedral (Mo (CN) t~ 4) stereoisomeric type having D2ci-42m ideal symmetry and designated mmmm in the first paper (HS) of this series. The complicated crystalline arrangement is determined primarily by direct interaction of sodium ions with oxalatooxygen (water molecules are relegated to the role of filler), and the Zr (C204) 4 “4 ion departs significantly from 42m symmetry. Thisdistortion is limited, well within the probable experimental accuracy, to the inner coordination group, ie, to thechemically least stable and structurally least rigid part of the complex. The structurally non-equivalent oxalatorings are flat and, barring some variation in Zr-0 bond lengths, are virtually isodimensional. Bond parameters, including an averaged Zr-0 bond length of 2.199 A., are in excellent agreement with a composite of other reported data. A structurally significant difference of 0.06 Á. between averaged bond lengths for- and Zr-Os types (cf., HS) overlies the distortion of the inner coordination group.