Synthesis and crystal structures of the five-coordinate diorganotin(IV) complex [Ph_2Sn(L)]·DMF and its 5-hydroxypyrazoline ligand (H_2L)

De Sousa G.F.; Marques D.R.; Resck I.S.; Sabino J.R.

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Synthesis and crystal structures of the five-coordinate diorganotin(IV) complex [Ph_2Sn(L)]·DMF and its 5-hydroxypyrazoline ligand (H_2L)

机译：五配位二有机锡（IV）配合物[Ph_2Sn（L）]·DMF及其5-羟基吡唑啉配体（H_2L）的合成和晶体结构

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A five-coordinate diorganotin(IV) complex [Ph_2Sn(L)]·DMF and its ligand, 5-hydroxy-3-methyl-5-phenyl-(N_4- phenylthiosemicarbazone)pyrazoline (H_2L), were synthesized and characterized by elemental analysis, IR, NMR (1H, 13C) spectroscopies and X-ray crystallography techniques. Our studies revealed that H_2L has formed as 5-hydroxy-4,5-dihydropyrazoline derivative in orthorhombic, Pbca space group with a = 15.4330(3) ?, b = 11.5427(2) ?, c = 18.1440(3) ?whereas [Ph_2Sn(L)]·DMF crystallizes with two independent molecules (a and b) in the asymmetric unit in triclinic system, P? space group with a = 9.2795(1) ?, b = 15.8315(2) ?, c = 19.9895(3) ?, α = 100.855(1)°,β = 92.985(1)°, γ = 102.243(1)°. In molecule a, the central Sn(IV) atom adopts a distorted tetragonal-pyramidal (TTP) geometry with N2 atom at apical position, while in molecule b the Sn(IV) occupies the centre of a trigonal-bipyramid (TBP) with N2 atom of the ONS-tridentate ligand and both Ph groups occupying equatorial positions. One molecule of DMF (crystallization solvent) helps in stabilizing the crystal structure.

机译：合成了五配位的二有机锡（IV）配合物[Ph_2Sn（L）]·DMF及其配体5-羟基-3-甲基-5-苯基-（N_4-苯基硫代半碳emi酮）吡唑啉（H_2L），并通过元素分析进行了表征，IR，NMR（1H，13C）光谱学和X射线晶体学技术。我们的研究表明，H_2L已形成为正交的Pbca空间群中的5-羟基-4,5-二氢吡唑啉衍生物，其中a = 15.4330（3）？，b = 11.5427（2）？，c = 18.1440（3）？ Ph_2Sn（L）]·DMF在三斜晶系的不对称单元中以两个独立的分子（a和b）结晶。 a = 9.2795（1）？，b = 15.8315（2）？，c = 19.9895（3）？，α= 100.855（1）°，β= 92.985（1）°，γ= 102.243（1）°的空间群。在分子a中，中心的Sn（IV）原子采用畸变的四角锥（TTP）几何结构，其N2原子位于顶端位置，而在分子b中，Sn（IV）占据具有N2的三角双锥体（TBP）的中心ONS-三齿配体的原子和两个Ph基团均占据赤道位置。一分子DMF（结晶溶剂）有助于稳定晶体结构。

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《Journal of chemical crystallography》 |2011年第4期|共5页
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De Sousa G.F.; Marques D.R.; Resck I.S.; Sabino J.R.;
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正文语种 eng
中图分类晶体学;
关键词
Complex Pyrazoline derivative; Crystal structures; Diorganotin(IV);

机译：吡唑啉配合物衍生物;晶体结构;二有机锡（IV）;

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1. Synthesis and crystal structures of the five-coordinate diorganotin(IV) complex [Ph_2Sn(L)]·DMF and its 5-hydroxypyrazoline ligand (H_2L) [J] . De Sousa G.F., Marques D.R., Resck I.S., Journal of chemical crystallography . 2011,第4期

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2. Synthesis, spectroscopic characterization and X-ray structures of five-coordinate diorganotin(IV) complexes containing 5-hydroxypyrazoline derivatives as ligands [J] . Sousa G.F.D., Garcia E., Gatto C.C., Journal of Molecular Structure . 2010,第1a3期

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Synthesis and crystal structures of the five-coordinate diorganotin(IV) complex [Ph_2Sn(L)]·DMF and its 5-hydroxypyrazoline ligand (H_2L)

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