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Solution Dynamics and Crystal Structure of $CpMoOs_{3}(CO)_{10}(mu-H)_{2}[mu_{3}-eta^{2}-C(O)CH_{2}Tol]$
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  • Solution Dynamics and Crystal Structure of $CpMoOs_{3}(CO)_{10}(mu-H)_{2}[mu_{3}-eta^{2}-C(O)CH_{2}Tol]$
저자명
Park. Joon T.,Cho. Jeong-Ju,Chun. Kang-Moon,Yun. Sock-Sung,Kim. SangSoo
간행물명
Bulletin of the Korean Chemical Society
권/호정보
1993년|14권 1호|pp.137-143 (7 pages)
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이 논문은 한국과학기술정보연구원과 논문 연계를 통해 무료로 제공되는 원문입니다.
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기타언어초록

The tetranuclear heterometallic complex CpMo$Os_3(CO)_{10}({mu]-H)2[{mu}3-{eta}^2-C(O)CH_2Tol];(1,;Cp={eta}^5-C_5H_5,;Tol=p-C_6H_4Me)$ has been examined by variable-temperature $^{13}$C-NMR spectroscopy and by a full three-dimensional X-ray structual analysis. Complex 1 crystallizes in the orthorhombic space group Pna2$_1$ with a = 12.960(1) ${AA}$, b = 11.255(l) ${AA}$, c = 38.569(10)${AA}$, V = 5626(2) ${AA}^3$ and ${ ho}$(calcd) = 2.71 gcm$^{-3}$ for Z = 8 and molecular weight 1146.9. Diffraction data were collectedon a CAD4 diffractometer, and the structure was refined to $R_F$ = 9.7% and $R_{W^F}$ = 9.9% for 2530 data (MoK${alpha}$ radiation). There are two essentially equivalent molecules in the crystallographic asymmetric unit. The tetranuclear molecule contains a triangulated rhomboidal arrangement of metal atoms with Os(2) and Mo at the two bridgehead positions. The metal framework is planar; the dihedral angle between Os(l)-Os(2)-Mo and Os(3)-Os(2)-Mo planes is 180$^{circ}$. A triply bridging (${mu}_3,;{eta}^2$) acyl ligand lies above the Os(l)-Os(2)-Mo plane; the oxygen atom spans the two bridgehead positions, while the carbon atom spans one bridgehead position and an acute apical position. The molecular architecture is completed by an ${eta}^5$-cyclopentadienyl ligand and a semi-triply bridging carbonyl ligand on the molybdenum atom, and nine terminal carbonyl ligands-four on Os(3), three on Os(l), and two on Os(2). The two hydride ligands are inferred to occupy the Os(l)-Os(2) and Mo-Os(3) edges from structural and NMR data.