| 146911-74-2

• CAS: 146911-74-2
• 化学式: C₁₇H₃₀B₉OP₂RhS
• 分子量: 544.643
• InChiKey: IXCDDCLTDHHVCP-UHFFFAOYSA-N

反应信息

• 作为产物：
  描述：

  、 二甲基苯基磷 以 苯 为溶剂， 以25%的产率得到
  参考文献：
  名称：

  Metallaheteroborane chemistry. Part 10. Synthesis and characterisation of closo-structured rhodathiaborane complexes [1-(CO)-1-L-3-L′-1,2-RhSB₉H₈](L = L′= PPh₃; L = PMe₂Ph, L′= PMe₂Ph or PPh₃)

  摘要：

  The reaction of CO with [8,8-(PPh3)2-8,7-RhSB9H10] 1 in benzene yields [8-(CO)-8,8-(PPh3)2-nido-8,7-RhSB9H10] 3 in 98% yield. Refluxing a benzene solution of 3 produces [1-(CO)-1,3-(PPh3)2-closo-1,2-RhSB9H8] 4 in 46% yield. The reaction between 4 and excess of PMe2Ph in refluxing benzene affords [1-(CO)-1-(PMe2Ph)-3-L-closo-1,2-RhSB9H8] [L= PMe2Ph 5 (25%) or PPh3 6 (46%)]. NMR data (H-1, B-11 and P-31) confirm the nido nature of 3 and the closo structures of compounds 4-6. X-Ray diffraction studies of 4, 4' (= 4.1.5C6H5Me), and 5 showed that there was conformational disorder in all three cases. The structure of 5 was solved in space group P2(1)/n with unit cell dimensions of a = 9.626(2), b = 23.714(5), c = 11.595(2) angstrom, beta = 109.00(2)-degrees, and Z = 4. The final R factor was 0.027 for 4472 observed reflections. Principal interatomic distances are Rh(1)-S(2) 2.3736(7), Rh(1)-P(1) 2.3090(7), Rh(1)-C(1) 1.855(3), Rh(1)-B(3) 2.101(3), Rh(1)-B (4, 5, 6, 7) 2.380(3)-2.444(3), S(2)-B 1.923(3)-1.989(4), B-B 1.719(4)-1.897(4) and B(3)-P(2) 1.895(3) angstrom. The geometry of the RhSB9 cage in 5 was used as a template in the final refinement of the structures of 4 and 4' which were more disordered: 4, space group C2/c, a = 37.529(l 1), b = 10.749(5), c = 19.536(5) angstrom, beta = 101.96(2)-degrees, Z = 8, R 0.051 for 3970 observed reflections; 4', space group P1BAR, a = 11.933(2), b = 14.157(2), c = 14.190(2) angstrom, alpha = 79.25(1), beta = 83.27(1), gamma = 87.32(1)-degrees, Z = 2, R 0.041 for 6959 observed reflections.

  DOI：

  10.1039/dt9920002865