Preparation,Structure,and Properties of a New Giant Manganese Oxo-Alkoxide Wheel,[Mn_(19)O_(12)(OC_2H_4OCH_3)_(14)(HOC_2H_4OCH-3)_(10)]·HOC_2H_4OCH_3

Annika M.Pohl; L.Gunnar Westin; Mikael Kritikos

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Preparation,Structure,and Properties of a New Giant Manganese Oxo-Alkoxide Wheel,[Mn_(19)O_(12)(OC_2H_4OCH_3)_(14)(HOC_2H_4OCH-3)_(10)]·HOC_2H_4OCH_3

机译：[Mn_（19）O_（12）（OC_2H_4OCH_3）_（14）（HOC_2H_4OCH-3）_（10）]·HOC_2H_4OCH_3新型巨型氧化锰锰氧化物轮的制备，结构和性能

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Alkoxides are of great interest as precursors for sol-gel processing of advanced ceramic materials,but there isvery little general knowledge about the low-valent 3d-element alkoxides.The novel oxo-alkoxide,[Mn_(19)O_(12)(moe)_(14)-(moeH)_(10)]·MOEH (MOE=OC_2H_2-OCH_3),was prepared,by metathesis and auto-decomposition,from MnCl_2 and potassium methoxyethoxide in toluene/MOEH,and the solid-state structure was determined from single-crystal X-ray diffraction data: trigonal cell,space group R3(no.148),#alpha#=27.560(3),c=19.294(2)A,Z=3,R1=0.0737,wR2=0.1609.The individual molecules are shaped as flat discs and all Mn atoms are divalent and octahedrally coordinated by oxygen atoms in a CdI_2-type layer structure.The central Mn aton is coordinated by six #mu#_3-oxo atoms and four MOE(H) groups,while the peripheral ring contains twelve Mn atoms coordinated by one #mu#_3-oxo atom and five MOE(H) groups.Differential scanning calorimetry studies showed that the first and irreversible changes start at about 100 deg C.The continuous decrease of X_M T with decreasing temperature below 150 K in the magnetic susceptibility measurements is probably due to amtiferromagnetic interactions.FTIR and UV/Vis spectroscopy of solid and dissolved samples showed that the solid-state structure changes at least to some extemt on dissolution in toluene/MOEH.

机译：烷氧化物作为高级陶瓷材料的溶胶-凝胶加工的前驱物备受关注，但对低价3d元素醇盐的常识知之甚少。新型的氧代醇盐[Mn_（19）O_（12）（moe））_（14）-（moeH）_（10）]·MOEH（MOE = OC_2H_2-OCH_3）是由MnCl_2和甲氧基乙氧基钾在甲苯/ MOEH中经易位和自分解制得的，并具有固态结构由单晶X射线衍射数据确定：三角晶胞，空间群R3（148号），＃alpha＃= 27.560（3），c = 19.294（2）A，Z = 3，R1 = 0.0737，wR2 = 0.1609.CdI_2型层结构中的单个分子形状为圆盘状，所有Mn原子都是二价且由氧原子八面体配位的。中心Mn原子由六个＃mu＃_3-oxo原子和四个MOE（ H）组，而外围环包含由一个＃mu＃_3-oxo原子配位的12个Mn原子和5个MOE（H）基团。差示扫描量热研究表明，第一个和不可逆的变化是星形在大约100摄氏度时t。在磁化率测量中X_M T随温度降低至150 K以下而连续降低可能是由于铁磁相互作用引起的。固相和溶解样品的FTIR和UV / Vis光谱表明，固态结构发生了变化至少在溶解于甲苯/ MOEH中有一些例子。

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《Chemistry: A European journal》 |2001年第16期|共7页
作者
Annika M.Pohl; L.Gunnar Westin; Mikael Kritikos;
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正文语种 eng
中图分类化学;应用化学;
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alkoxides; ir spectroscopy; manganese; structural elucidation; uv/vis spectroscopy;

机译：醇盐;红外光谱;锰;结构解析;紫外/可见光谱;

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Preparation,Structure,and Properties of a New Giant Manganese Oxo-Alkoxide Wheel,[Mn_(19)O_(12)(OC_2H_4OCH_3)_(14)(HOC_2H_4OCH-3)_(10)]·HOC_2H_4OCH_3

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