{2-I-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)} | 147104-97-0

• 英文名称: {2-I-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)}
• CAS: 147104-97-0
• 化学式: C₃₆H₃₉B₁₀IP₂PdTe
• 分子量: 1002.69
• InChiKey: QLDPMUYRZKKMOD-UHFFFAOYSA-M

计算性质

• 辛醇/水分配系数(LogP)：
  None
• 重原子数：
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• 可旋转键数：
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• 环数：
  None
• sp3杂化的碳原子比例：
  None
• 拓扑面积：
  None
• 氢给体数：
  None
• 氢受体数：
  None

反应信息

• 作为反应物：
  描述：

  {2-I-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)} 在 CH₂Cl₂ 、 AgBF₄ 作用下， 以 甲苯 为溶剂， 以94.3%的产率得到{2-(H2O)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)}{BF4} * 0.89 CH2Cl2
  参考文献：
  名称：

  Metallaheteroborane chemistry. Part 12. Synthesis of cationic metallaheteroboranes [2-L-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4]; molecular structures of the compounds with L = H2O or CO

  摘要：

  The reaction of Ag[BF4] and [2-1-2-(PPh3)-closo-2,1 -PdTeB10H9(PPh3)] 1 in toluene for 30 min at room temperature and subsequent isolation of the product under aerobic conditions afforded [2-(H2O)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4] 2 in excellent yield. This complex has been characterised by (IR and B-11 NMR)spectroscopy and X-ray crystallography. Crystals of 2-0.89 CH,Cl,are monoclinic, space group P2(1)/c, with cell dimensions a = 14.073(3), b = 15.640(2), c = 20.262(6) angstrom and beta = 94.80(2)-degrees. A final R factor of 0.038 was calculated for 5595 observed reflections. The Pd-OH2 distance is 2.208(4) angstrom and Pd-P(1) is 2.3544(14) angstrom. Cage interatomic distances include Pd-Te 2.6958(6) and ranges for Pd-B of 2.192(6) 2.299(6)and Te-B of 2.287(6)-2.403(6)angstrom. The exo-cage B(7)-P(2) distance is 1.950(6) angstrom. The water molecule in 2 can be displaced by a variety of ligands to produce the cationic palladatelluraborane complexes [2-L-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4][L = CO, CNBu(t), CNC6H11, NCMe, MeCH(Ph)NH2, OC4H8 or SC4H8) in yields ranging from 39 to 93%. Reaction between 2 and a ten-fold excess of PMe2Ph affords [2,2-(PMe2Ph)2-closo-2,1-PdTeB10H9(PPh3)][BF4] in 75% yield. All complexes have been characterised spectroscopically (IR and B-11 NMR) and in the case of [2-(CO)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4] 3 by X-ray crystallography. The 3.C6H5Me solvate crystallises in the monoclinic space group P2(1)/c with Z = 4, a = 14.509(3), b = 10.732(l ), c = 31.377(8) A and beta = 97.49(2)-degrees. The final R factor of 0.054 was calculated from 5439 observed reflections. Principal interatomic distances include Pd-Te 2.6897(9), Pd-B 2.195(10)-2.307(9), Te-B 2.262(11)-2.389(9), Pd-P(2) 2.367(2), B(11)-P(1) 1.941 (9) and Pd-C(1) 2.003(9) angstrom.

  DOI：

  10.1039/dt9930000035
• 作为产物：
  描述：

  diiodobis(triphenylphosphino)palladium(II) 、 [nido-7-TeB10H11](1-) caesium salt 以 甲苯 为溶剂， 以95.4%的产率得到{2-I-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)}
  参考文献：
  名称：

  Metallaheteroborane chemistry. Part 11. Selective syntheses of the palladium heteroborane complexes [2,2-(PR3)2-closo-2,1-PdEB10H10](R3= Ph3, MePh2 or Me2Ph; E = Se or Te) and [2-X-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)](X = Cl, Br, I, CN, SCN or O2CMe)

  摘要：

  Reaction of [PdCl2(PR3)2] (R3 = Ph3, MePh2 or Me2Ph) with the nido-[7-EB10H11]- anions (E = Se or Te) in tetrahydrofuran (thf) at ambient temperature affords twelve-vertex [2,2-(PR3)2-closo-2,1-PdEB10H10] complexes selectively in yields ranging from 16 (E = Se, R = Ph) to 82% (E = Te, R, = Me2Ph). In contrast, the reaction between [PdX2(PPh3)2] (X = Cl or 1) and [7-TeB10H11]- in refluxing toluene affords only [2-X-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)] in 39 and 95% yields respectively. Further reactions of [2-1-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)] with Hg(II) salts in thf produce [2-X-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)] complexes (X = Cl, Br, CN, SCN or O2CMe) in yields from 19 (X = O2CMe) to 96% (X = CN). All complexes were characterised by infrared and NMR spectroscopies. Variable-temperature H-1-{P-31} NMR spectroscopy of [2,2-(PMePh)2-closo-2,1-PdSeB10H10] shows a metal-to-selenaborane rotational bonding fluxionality with DELTAG(double-dagger)293 = 44.5 kJ mol-1. An X-ray diffraction study of [2,2-(PMe2Ph)2-closo-2,1-PdTeB10H10] 6 reveals the crystals to be monoclinic, space group P2(1)/n, with a = 13.110(3), b = 10.498(3), c = 19.561(3) angstrom, beta = 105.44(1)-degrees and Z = 4. A final R factor of 0.023 was calculated for 4579 observed reflections. Principal interatomic distances include Pd-Te 2.6833(2), Pd-B 2.234(3)-2.301(3), Te-B 2.294(4)-2.374(3) and Pd-P 2.3301(7) and 2.3354(8) angstrom. An X-ray diffraction study of [2-(O2CMe)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)] 14 recrystallised from CH2Cl2-n-C7H14 as 14. 0.79CH2Cl2 shows the crystals to be triclinic, space group P1BAR with a = 10.416(2), b = 12.409(2), c = 18.720(4) angstrom, alpha = 75.59(2), beta = 84.10(2), gamma = 70.98(1)-degrees and Z = 2. The final R factor is 0.035 for 6472 observed reflections. The acetate ligand is monodentate with Pd-O(1) 2.121(3) A. Other interatomic distances include Pd-Te 2.6903(4), Pd-P(2) 2.355(1), Pd-B(7) 2.201(5), Pd-B(6) 2.268(4) and B(11)-P(1) 1.942(4) angstrom.

  DOI：

  10.1039/dt9930000027

文献信息

• An alternative route to cationic metallaheteroboranes
  作者：George Ferguson、John F. Gallagher、James P. Sheehan、Trevor R. Spalding、John D. Kennedy、Ramón Maciás

  DOI：10.1039/dt9930003147

  日期：——

  The reaction between [2-I-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)] and excess of phosphine (PR3 = PMe3 or PMe2Ph) afforded air-stable cationic palladatelluraboranes [2,2-(PR3)2-closo-2,1-PdTeB10H9(PPh3)]I 1 (PR3 = PMe3) or 2 (PR3 = PMe2Ph) which were characterised spectroscopically (IR and B-11 NMR) and by an X-ray diffraction study of 1.