Hybrid Organic-Inorganic Frameworks (MIL-n). Hydrothermal Synthesis of a Series of Pillared Lanthanide Carboxyethylphosphonates and X-ray Powder ab Initio Structure Determination of MIL-19, Pr[O(3)P(CH(2))(2)CO(2)].
Hybrid Organic-Inorganic Frameworks (MIL-n). Hydrothermal Synthesis of a Series of Pillared Lanthanide Carboxyethylphosphonates and X-ray Powder ab Initio Structure Determination of MIL-19, Pr[O(3)P(CH(2))(2)CO(2)].
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DOI：
10.1021/ic981440i
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发表时间：
1999-10
影响因子：
4.6
通讯作者：
F. Serpaggi;G. Férey
中科院分区：
文献类型：
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作者：
F. Serpaggi;G. Férey
由羧乙基膦酸和金属氯化物的1：1混合物水热（200 ℃，4天）制备了一系列镧系元素和钇羧乙基膦酸盐。用X-射线粉末衍射法从头算确定了镨配合物Pr（III）[O（3）P（CH（2））（2）CO（2）]的晶体结构，并用Rietveld方法进行了修正。该化合物在单斜晶系空间群P2（1）/m（No.11）中结晶，晶胞参数为20 ℃ a = 8.3617（2）° C，B = 7.1899（2）° C，c = 5.4586（2）° C，β = 103.784（2）° C，Z = 2。最终的一致性因子收敛到值R（p）= 0.139，R（wp）= 0.177，Bragg R = 0.123，R（F）= 0.055和chi（2）= 3.50。杂化骨架由有机基团连接的无机Pr/O/P/C层组成，层间距约为8.36 μ m。在这种柱撑层状结构中，praesoorphins原子是7重配位的。钇和整个系列的镧系元素的同构化合物制备。
A series of lanthanide and yttrium carboxyethylphosphonates has been hydrothermally prepared (200 degrees C, 4 days) from the 1:1 mixture of carboxyethylphosphonic acid and the metal chlorides. The crystal structure of the praesodymium compound Pr(III)[O(3)P(CH(2))(2)CO(2)] has been determined ab initio from X-ray powder diffraction data and refined by the Rietveld method. The compound crystallizes in the monoclinic space group P2(1)/m (No. 11) with cell parameters at 20 degrees C a = 8.3617(2) Å, b = 7.1899(2) Å, c = 5.4586(2) Å, beta = 103.784(2) degrees, and Z = 2. The final agreement factors converged to the values R(p) = 0.139, R(wp) = 0.177, Bragg R = 0.123, R(F) = 0.055, and chi(2) = 3.50. The hybrid framework consists of inorganic Pr/O/P/C layers connected by organic groups, with an interlayer spacing of approximately 8.36 Å. The praesodymium atoms are 7-fold coordinated in this pillared layered structure. Isostructural compounds were prepared for yttrium and the entire series of the lanthanide elements.