摘要
本文报道MoCl3·3H2O与乙酸作用生成三核钼簇合物H[HO]3[Mo3O(OAc)3Cl6]的反应,并用X射线单晶结构分析方法测定了簇合物的晶体结构,结晶学参数为:α=17.468(4),b=9.948(2),c=13.035(2)A.β=148.83(2)°,V=1172(1)A3,Z=2,Do=2.109g/cm3.空间群为Pc.非权重偏离因子是R=0.057.结构分析结果表明该化合物阴离子为单氧帽等边三角形三核钼簇合阴离子,Mo—Mo平均距离2.569A.对簇骼单元[Mo3O(μ-Cl)3Cl3]2+进行简正坐标分析.从理论上对振动光谱谱带进行了归属.10条IR谱带的观测和计算频率的平均偏差为1.15%.本文讨论了特征谱带(包括金属键)的归属和力常数的合理性.
The synthesis of trinuclear molybdenum cluster H[H2O]3[Mo3O(OAc)3Cl6]by reacting of MoCl3·3H2O with acetic acid is reported.The crystal structure of cluster has been determined by X-ray single crystal structure analysis.Crystallographic parameters are as followingα=17.468(4),b=9.948(2),c=13.035(2)A,β=148.83(2)°,V=1172(1)A~3,Z=2,Dc=2.109g/cm~3,space group is Pc.Unweighted factor R=0.057.Result of structure determination reveals that anion of title compound is an anion cluster of oxygen monocapped equilateral triangle trinuclear molybdenum,average distance of Mo-Mo is 2.569A.The assignment of vibrational spectra has been carried out using normal coordinate analysis of cluster unit[Mo3O(μ-Cl)3Cl3]2+.The average error between observed and calculated frequencies of ten IR bands is 1.15%.The rationality of assignment of feature bands(including metal bond)and force constants has been discussed.
出处
《化学学报》
SCIE
CAS
1988年第5期439-444,共6页
Acta Chimica Sinica
