化工技术与开发
化工技術與開髮
화공기술여개발
TECHNOLOGY & DVELOPMENT OF CHEMICAL INDUSTRY
2013年
8期
6-9,13
,共5页
配合物%晶体结构%热稳定性
配閤物%晶體結構%熱穩定性
배합물%정체결구%열은정성
complex%crystal structure%thermal stability
采用水热法和自然挥发法,邻羟基苯乙酮苯甲酰腙与过渡金属Ni(Ⅱ)、Cr(Ⅲ)反应,合成2种新型配合物。通过X射线单晶衍射对配合物结构进行了表征。配合物1:晶体为单斜晶系,C2/c空间群,晶胞参数a=1.5853(3) nm,b=1.16643(19)nm,c=1.8928(3)nm,β=90.00°,V=3.5000(10) nm3,Z=8,Dc=1.484g·cm-3。配合物2:晶体为四方晶系,I4122空间群,晶胞参数a=1.2272(4)nm,b=1.1098(4)nm,c=1.8849(6)nm,β=90.00°,V=2.5671(15)nm3,Z=4, Dc=1.445g·cm-3。配合物1的中心金属离子Ni(Ⅱ)与周围2个氧原子和2个氮原子形成平面几何构型。配合物2的中心金属离子Cr(Ⅲ)与周围4个氧原子和2个氮原子配位形成畸变的八面体配位构型。并利用热失重法分析研究了配合物的热稳定性。
採用水熱法和自然揮髮法,鄰羥基苯乙酮苯甲酰腙與過渡金屬Ni(Ⅱ)、Cr(Ⅲ)反應,閤成2種新型配閤物。通過X射線單晶衍射對配閤物結構進行瞭錶徵。配閤物1:晶體為單斜晶繫,C2/c空間群,晶胞參數a=1.5853(3) nm,b=1.16643(19)nm,c=1.8928(3)nm,β=90.00°,V=3.5000(10) nm3,Z=8,Dc=1.484g·cm-3。配閤物2:晶體為四方晶繫,I4122空間群,晶胞參數a=1.2272(4)nm,b=1.1098(4)nm,c=1.8849(6)nm,β=90.00°,V=2.5671(15)nm3,Z=4, Dc=1.445g·cm-3。配閤物1的中心金屬離子Ni(Ⅱ)與週圍2箇氧原子和2箇氮原子形成平麵幾何構型。配閤物2的中心金屬離子Cr(Ⅲ)與週圍4箇氧原子和2箇氮原子配位形成畸變的八麵體配位構型。併利用熱失重法分析研究瞭配閤物的熱穩定性。
채용수열법화자연휘발법,린간기분을동분갑선종여과도금속Ni(Ⅱ)、Cr(Ⅲ)반응,합성2충신형배합물。통과X사선단정연사대배합물결구진행료표정。배합물1:정체위단사정계,C2/c공간군,정포삼수a=1.5853(3) nm,b=1.16643(19)nm,c=1.8928(3)nm,β=90.00°,V=3.5000(10) nm3,Z=8,Dc=1.484g·cm-3。배합물2:정체위사방정계,I4122공간군,정포삼수a=1.2272(4)nm,b=1.1098(4)nm,c=1.8849(6)nm,β=90.00°,V=2.5671(15)nm3,Z=4, Dc=1.445g·cm-3。배합물1적중심금속리자Ni(Ⅱ)여주위2개양원자화2개담원자형성평면궤하구형。배합물2적중심금속리자Cr(Ⅲ)여주위4개양원자화2개담원자배위형성기변적팔면체배위구형。병이용열실중법분석연구료배합물적열은정성。
Two transition metal complexes as 2’-Hydroxyacetophenone benzoyl hydrazone with Ni( Ⅱ ), Cr( Ⅲ ) were synthesized by hydrothermal method and solvent evaporation technique and charactered by singal crystal X-ray diffraction analysis and thermogravi-metric analysis .The result showed that the complex 1 crystal structure belonged to monoclinic, space group C2/c with a=1.5853(3)nm, b=1.16643(19)nm, c=1.8928(3)nm,β=90.00 °, V=3.5000(10)nm3,Z=8,Dc=1.484g/cm3. The complex 2 crystallized in the tetragonal space group I4122 with a=1.2272(4) nm,b=1.1098(4)nm,c=1.8849(6)nm,β=90.00° ,V=2.5671(15) nm3,Z=4,Dc=1.445g/cm3. The complex 1 Ni(Ⅱ) ions existed in a four-coordinated environment in which one tridentate ligand in the two oxygen atoms and one nitrogen, one pyridine nitrogen atoms.The complex 2 Cr(Ⅲ) ions in complex 2 were octahedrally coordinated by four oxygen atoms and two ni-trogen atoms from two tridentate ligands.