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Synthesis, crystal structure, and spectroscopy of (azido-N1)bis(2,2 '-bi-imidazoline)copper(II) perchlorate

机译:(叠氮基-N1)双(2,2'-双咪唑啉)高氯酸铜(II)的合成,晶体结构和光谱

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The compound [Cu(biz)(2)(N-3)](ClO4) (biz=2,2'-bi-imidazoline) has been synthesized and characterized by X-ray crystallography and infrared spectroscopy. In addition, EPR and magnetic measurements have been performed. The compound crystallizes in the monoclinic space group P2(1)/c, with a=9.2716(2), b=27.6454(4), c=7.4285(1)Angstrom, beta=102.1417(6)degrees, V=1861.46(5)Angstrom(3), and Z=4. The coordination geometry around the Cu(II) ion is distorted square pyrimidal, with 4 nitrogen atoms of 2 bis-chelating ligand molecules in the basal plane and one nitrogen of the azide molecule in the apical position. The perchlorate ion is noncoordinating. In the infrared the vibrations of the coordinated azide anion are observed at 2050, 1286, and 620 cm(-1), while the vibrations of the free perchlorate anion are observed at 1071, 1035, and 919 cm(-1); Cu-N vibrations are observed at 418 and 336 cm(-1). The molecules are connected in the lattice via relatively strong hydrogen bonding between the N-H groups at the back of the biz ligand and the N1 and N3 atoms of the azide ligand forming layers. No intermolecular magnetic interaction was observed for this compound. [References: 21]
机译:合成了化合物[Cu(biz)(2)(N-3)](ClO4)(biz = 2,2'-双咪唑啉),并通过X射线晶体学和红外光谱对其进行了表征。另外,已经进行了EPR和磁测量。该化合物在单斜空间群P2(1)/ c中结晶,a = 9.2716(2),b = 27.6454(4),c = 7.4285(1)埃,beta = 102.1417(6)度,V = 1861.46( 5)埃(3),Z = 4。 Cu(II)离子周围的配位几何结构扭曲成方形的嘧啶亚砜,在基面上具有2个双螯合配体分子的4个氮原子,在顶位具有叠氮分子的1个氮。高氯酸根离子是非配位的。在红外中,在2050、1286和620 cm(-1)处观察到配位叠氮化物阴离子的振动,而在1071、1035和919 cm(-1)处观察到游离高氯酸根阴离子的振动。在418和336 cm(-1)处观察到Cu-N振动。分子通过biz配体背面的N-H基团与叠氮化物配体形成层的N1和N3原子之间相对较强的氢键在晶格中连接。没有观察到该化合物的分子间磁性相互作用。 [参考:21]

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