Hydrothermal Synthesis and Characterization of Four Oxalatotitanates with Ti4O4(C2O4)8 Tetramers as Basic Building Blocks

作者: Yunlong Fu , Yunling Liu , Zhan Shi , Baozong Li , Wenqin Pang

DOI: 10.1006/JSSC.2001.9422

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摘要: Abstract Four oxalatotitanates have been prepared hydrothermally in the presence of organic amine and their structures solved by means single-crystal X-ray diffraction. The compound Ti4O4(C2O4)8·4C2N2H10·4H2O 1 crystallizes triclinic space group P with a=10.7587(7) A, b=11.3180(7) c=11.5940(8) α=114.8650(10)°, β=109.2980(10)°, γ=95.7160(10)°, V=1161.07(13) A3, Z=1, R=0.0357, wR=0.1019. Ti4O4(C2O4)8·4C4N2H12·8H2O 2 tetragonal I4(1)/a a=13.2270(10) b=13.2270(10) c=32.799(4) V=5738.2(9) Z=4, R=0.0529, wR=0.1496. Ti4O4(C2O4)8·4C6N2H14·10H2O 3 monoclinic P2(1)/c a=13.1613(7) b=18.2394(11) c=13.8579(7) α=90°, β=104.8600(10)°, γ=90°, V=3215.4(3) Z=2, R=0.0445, wR=0.1188. These compounds are all composed Ti4O4(C2O4)8 tetramer anions protonated cations. fourth Ti4O4(C2O4)7·3C4N2H12·2H2O 4 (No. 2) a=9.5187(13) b=11.4926(15) c=11.6349(15) α=67.405(3)°, β=81.407(3)°, γ=66.906(3)°, V=1080.9(2) R=0.0356, wR=0.0932. For 4, tetramers connected sharing oxalates as bridging ligands form a one-dimensional chain negative charges which neutralized piperazine as-synthesized products characterized powder diffraction, IR spectroscopy, inductively coupled plasma analysis, thermogravimetric differential thermal analysis.

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