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二甲基双[2,4-戊二酮基(1-)-κ,]锡(IV)晶体结构的重新测定

Redetermination of the crystal structure of di-methyl-bis-[2,4-penta-nedionato(1-)-κ,]tin(IV).

作者信息

Reuter Hans, Reichelt Martin

机构信息

Institute of Chemistry of New Materials, University of Osnabrück, Barbarastrasse 7, 49069 Osnabrück, Germany.

出版信息

Acta Crystallogr E Crystallogr Commun. 2017 Mar 3;73(Pt 4):472-475. doi: 10.1107/S2056989017003206. eCollection 2017 Apr 1.

Abstract

The redetermination of the title compound, [Sn(CH)(CHO)] or SnMe(acac), from CCD data recorded at 100 K basically confirms the previous study based on integrated film data recorded at room temperature [Miller & Schlemper (1972 ▸). , 677-681], but reveals a remarkable shrinkage of the axis [7.12 (1) > 6.7694 (4) Å]. The mol-ecule belongs to point group with the Sn atom on a centre of inversion. The Sn atom shows a slightly distorted octa-hedral coordination sphere with the methyl groups in positions and a Sn-C bond length of 2.115 (2) Å which may serve as a standard value for an Sn-CH bond of an octa-hedrally coordinated Sn atom. The Sn-O bonds involving the two carbonyl groups of the acetyl-acetonate ligand are of equal length [2.180 (1) and 2.183 (1) Å], as are the C=O [1.273 (1) and 1.274 (1) Å] and C-C bond lengths [1.393 (2) and 1.400 (2) Å]. The acetyl-acetonate ligand deviates considerably from planarity, with a dihedral angle of 5.57 (9)° between the least-squares planes of the two acetone moieties. The four O atoms of the two symmetry-related acetyl-acetonate ligands are arranged in a nearly quadratic rectangle. Weak C-H⋯O inter-actions consolidate the crystal packing.

摘要

通过在100K下记录的电荷耦合器件(CCD)数据对标题化合物[Sn(CH)(CHO)]或SnMe(acac)进行重新测定,基本上证实了之前基于室温下记录的积分胶片数据所做的研究[米勒和施伦珀(1972▸),677 - 681],但揭示出a轴有显著收缩[7.12 (1) > 6.7694 (4) Å]。该分子属于点群,Sn原子位于对称中心。Sn原子呈现出略微扭曲的八面体配位环境,甲基处于特定位置,Sn - C键长为2.115 (2) Å,这可作为八面体配位Sn原子的Sn - CH键的标准值。涉及乙酰丙酮配体两个羰基的Sn - O键长度相等[2.180 (1)和2.183 (1) Å],C = O键长[1.273 (1)和1.274 (1) Å]以及C - C键长[1.393 (2)和1.400 (2) Å]也相等。乙酰丙酮配体显著偏离平面性,两个丙酮部分的最小二乘平面之间的二面角为5.57 (9)°。两个对称相关的乙酰丙酮配体的四个O原子排列成近似矩形。弱的C - H⋯O相互作用巩固了晶体堆积。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a511/5382601/f21c8f258354/e-73-00472-fig1.jpg

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