Kirik Sergei D, Mulagaleev Ruslan F, Blokhin Alexander I
Institute of Chemistry and Chemical Technology, 660049 Krasnoyarsk, Russian Federation.
Acta Crystallogr C. 2005 Oct;61(Pt 10):m445-7. doi: 10.1107/S0108270105027095. Epub 2005 Sep 10.
The water-insoluble title compound, octakis(mu-acetato-kappa2O:O)octakis(mu-nitroso-kappa2N:O)octapalladium(II), [Pd8(CH3COO)8(NO)8], was precipitated as a yellow powder from a solution of palladium nitrate in nitric acid by adding acetic acid. Ab initio crystal structure determination was carried out using X-ray powder diffraction techniques. Patterson and Fourier syntheses were used for atom locations, and the Rietveld technique was used for the final structure refinement. The crystal structure is of a molecular type. The skeleton of the [Pd8(CH3COO)8(NO)8] molecule is constructed as a tetragonal prism with Pd atoms at the vertices. The eight NO- groups are in bridging positions along the horizontal edges of the prism. The N and O atoms of each nitroso group coordinate two different Pd atoms. The vertical edges present PdPd contacts with a short distance of 2.865 (1) A. These Pd atoms are bridged by a pair of acetate groups in a cis orientation with respect to each other. The complex has crystallographically imposed 4/m symmetry; all C atoms of the acetate groups are on mirror planes. The unique Pd atom lies in a general position and has square-planar coordination, consisting of three O and one N atom.
水不溶性标题化合物八（μ-乙酸根-κ²O:O）八（μ-亚硝基-κ²N:O）八钯（II），[Pd₈(CH₃COO)₈(NO)₈]，通过向硝酸钯在硝酸中的溶液中加入乙酸而沉淀为黄色粉末。使用X射线粉末衍射技术进行了从头晶体结构测定。帕特森合成和傅里叶合成用于原子定位，里特韦尔德技术用于最终的结构精修。晶体结构为分子型。[Pd₈(CH₃COO)₈(NO)₈]分子的骨架构建为一个四方棱柱，钯原子位于顶点。八个NO⁻基团沿棱柱的水平棱处于桥连位置。每个亚硝基的N和O原子与两个不同的钯原子配位。垂直棱上的钯原子之间存在短距离为2.865(1) Å的Pd-Pd接触。这些钯原子由一对彼此呈顺式取向的乙酸根基团桥连。该配合物具有晶体学上赋予的4/m对称性；乙酸根基团的所有C原子都在镜面上。唯一的钯原子处于一般位置，具有由三个O原子和一个N原子组成的平面正方形配位。
