Syntheses, Structures, and Properties of the Bis(cyclopentadienyl) Rare-Earth Imidodiphosphinochalcogenido Compounds Cp2Ln[N(QPPh2)2] (Ln = La, Gd, Er, or Yb for Q = S
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- 作者：Christopher G. Pernin and James A. Ibers
- 刊名：Inorganic Chemistry
- 出版年：2000
- 出版时间：March 20, 2000
- 年：2000
- 卷：39
- 期：6
- 页码：1216 - 1221
- 全文大小：112K
- 年卷期：v.39,no.6(March 20, 2000)
- ISSN：1520-510X
文摘
The compounds Cp2Ln[N(QPPh2)2] (Ln = La (1), Gd (2), Er (3), or Yb (4) for Q = Se, Ln = Yb (5) for Q =S) have been synthesized from the corresponding rare-earth tris(cyclopentadienyl) compound and H[N(QPPh2)2].The structures of compounds 1, 2, 3, and 5, as determined by X-ray crystallography, consist of a Cp2Ln fragment,coordinated 
3 through two chalcogen atoms and an N atom of the imidodiphosphinochalcogenido ligand[N(QPPh2)2]-. In compound 4, the Cp2Yb moiety is coordinated 2 through the two Se atoms of the [N(SePPh2)2]-ligand. 31P and 77Se (for 1) NMR spectroscopies lend insight into the solution nature of these species. Crystaldata: 1, C34H30LaNP2Se2, triclinic, P
, a = 9.7959(10) Å, b = 12.4134(13) Å, c = 13.9077(14) Å, 
= 88.106(2)
,
= 88.327(2), 
= 68.481(2), V = 1572.2(3) Å3, T = 153 K, Z = 2, and R1(F) = 0.0257 for the 5947reflections with I > 2
(I); 2, C34H30GdNP2Se2, triclinic, P, a = 9.7130(14) Å, b = 12.2659(17) Å, c = 13.953(2)Å, = 88.062(2), = 87.613(2), = 69.041(2), V = 1550.7(4) Å3, T = 153 K, Z = 2, and R1(F) = 0.0323for the 5064 reflections with I > 2(I); 3, C34H30ErNP2Se2, triclinic, P, a = 9.704(2) Å, b = 12.222(3) Å, c =13.980(4) Å, = 88.230(4), = 87.487(4), = 69.107(4), V = 1547.4(7) Å3, T = 153 K, Z = 2, and R1(F)= 0.0278 for the 6377 reflections with I > 2(I); 4, C34H30NP2Se2Yb·C4H8O, triclinic, P, a = 12.087(4) Å, b= 12.429(4) Å, c = 23.990(7) Å, = 89.406(5), = 86.368(5), = 81.664(5), V = 3558.8(18) Å3, T = 153K, Z = 4, and R1(F) = 0.0321 for the 11 883 reflections with I > 2(I); and 5, C34H30NP2S2Yb, monoclinic,P21/n, a = 13.8799(18) Å, b = 12.6747(16) Å, c = 17.180(2) Å, = 91.102(3), V = 3021.8(7) Å3, T = 153K, Z = 4, and R1(F) = 0.0218 for the 6698 reflections with I > 2(I).
3 through two chalcogen atoms and an N atom of the imidodiphosphinochalcogenido ligand[N(QPPh2)2]-. In compound 4, the Cp2Yb moiety is coordinated 2 through the two Se atoms of the [N(SePPh2)2]-ligand. 31P and 77Se (for 1) NMR spectroscopies lend insight into the solution nature of these species. Crystaldata: 1, C34H30LaNP2Se2, triclinic, P, a = 9.7959(10) Å, b = 12.4134(13) Å, c = 13.9077(14) Å, = 88.106(2), = 88.327(2), = 68.481(2), V = 1572.2(3) Å3, T = 153 K, Z = 2, and R1(F) = 0.0257 for the 5947reflections with I > 2(I); 2, C34H30GdNP2Se2, triclinic, P, a = 9.7130(14) Å, b = 12.2659(17) Å, c = 13.953(2)Å, = 88.062(2), = 87.613(2), = 69.041(2), V = 1550.7(4) Å3, T = 153 K, Z = 2, and R1(F) = 0.0323for the 5064 reflections with I > 2(I); 3, C34H30ErNP2Se2, triclinic, P, a = 9.704(2) Å, b = 12.222(3) Å, c =13.980(4) Å, = 88.230(4), = 87.487(4), = 69.107(4), V = 1547.4(7) Å3, T = 153 K, Z = 2, and R1(F)= 0.0278 for the 6377 reflections with I > 2(I); 4, C34H30NP2Se2Yb·C4H8O, triclinic, P, a = 12.087(4) Å, b= 12.429(4) Å, c = 23.990(7) Å, = 89.406(5), = 86.368(5), = 81.664(5), V = 3558.8(18) Å3, T = 153K, Z = 4, and R1(F) = 0.0321 for the 11 883 reflections with I > 2(I); and 5, C34H30NP2S2Yb, monoclinic,P21/n, a = 13.8799(18) Å, b = 12.6747(16) Å, c = 17.180(2) Å, = 91.102(3), V = 3021.8(7) Å3, T = 153K, Z = 4, and R1(F) = 0.0218 for the 6698 reflections with I > 2(I).