Synthesis, Characterization And Structural Study Of Yetterocene(â…¡) And Polymer Of Indenyl Potassium Salt With (Me₂Si)₂NSiMe₂ Side-Chains

Under the protection of purified, water-free, oxygen-free argon,using standard Schlenk techniques, We synthesized oneorganolanthanide complex and potassium salt polymer. Synthesis ,characterization and structure study of the two compound have beendiscussed in this paper. (1)Synthesis , characterization and structures t u d y o f [ η 5 - C5 H 4 S i M e 2 N ( S i M e 3 ) 2 ]2 Y b ( Ⅱ ) · 2 T H F :After reaction of two molar (Me3Si)2NSiMe2 CpLi with oneequivalent YbCl3 and Na in solvent, we get the complex[η5-C5H4SiMe2N(SiMe3)2]2Yb( Ⅱ ) ·2THF. The new complex[η5-C5H4SiMe2N(SiMe3)2]2Yb( Ⅱ ) ·2THF has been prepared in aconvenient three-step synthesis. Its crystal structure was characterized byX-ray diffraction. It crystallizes in the monoclinic system, space groupP21/C with a=16.4687(12), b=9.0770(6), c=30.494(3)?, β=93.642(4)0,V=4549.3(6) ?3, Z=2, C34H72N2O2Si6Yb, Mr=882.51, Dc=1.288g/cm3,F(000)=1840.00 and μ(MoKα)=22.42cm-1(λ=0.71070 ?). The final R andRw are 0.039,0.050, respectively with 7814 observed reflections withI>3.00σ(1). The ytterbium atom is coordinated to the oxygen atoms oftwo tetrahydrofuran molecules and to two cyclopentadienyl rings.(2)Synthesis , characterization and structure study of polymer of indenylpotassium salt with (Me3Si)2NSiMe2 side chain: After reaction of twomolar (Me3Si)2NSiMe2IndLi with one equivalent YbCl3 and K/Na in 5solvent, we hope get the complex [IndSiMe2N(SiMe3)2]2Yb(Ⅱ) ·2THF,but we get the unexpected polymeric complex {K[IndSiMe2N(SiMe3)2]}n.The new complex unit K[IndSiMe2N(SiMe3)2] has been prepared in aconvenient three-step synthesis. Its crystal structure was alsocharacterized by X-ray diffraction. It crystallizes in the monoclinicsystem, space group P21/n with a=13.853(6), b=10.243(4), c=16.754(7)?,β=109.284(6)0, V=2244.1(16) ?3, Z=4, C17H25NSi3K, Mr=366.75,Dc=1.086g/cm3, F(000)=780 and μ(MoKα)=22.42cm-1(λ=0.71073 ?).The final R and Rw are 0.0842,0.2162, respectively with 2056 observedreflections with I>2.00σ(1). The potassium atom is coordinated to thecarbon atoms of two methylenes and to two indene. Two complexes werecharacterized by elemental analysis, IR,X-ray diffraction.