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Inorganic Chemistry
Volumn 47, Issue 7, 2008, Pages 2246-2248
Water-soluble 3,7-dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane (dmoPTA) as a polydentate ligand: Synthesis of [RuClCp(PPh3)-μ- dmoPTA-1κP:2κ2N,N′-Co(acac-κ2O, O′)2]·H2O
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EID: 42449132966     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic702239w     Document Type: Article
Times cited : (38)
References (42)
  • 23
    • 42449113623 scopus 로고    scopus 로고
    • Co(acac)2 (0.0858 g, 0.33 mmol) was introduced into a solution of 1 (0.075 g, 0.0095 mmol) in 6 mL of MeOH. The mixture was first stirred at room temperature until dissolution of the reactants was completed and then refluxed for 3.5 h. The solvent was removed until 0.5 mL, and then 5 mL of pentane was added. The obtained pale-brown precipitated was filtered and washed with water (2 x 5 mL, The wet powder was recrystallized in EtOH. Yield: 47.7 mg (∼ 55, S25°C,H2O < 1 mg/mL. Elem anal. Calcd for C40H52N3ClO5P2RuCo (MW, 912.25 g/mol, C, 52.66; H, 5.70; N, 4.60. Found: C, 52.42; H, 5.81; N, 4.47. 13C{1H} NMR (CD3OD, δ (ppm) 88.24 (s, Cp, 127.8-136.22 (m, aromatic, PPh3, 31P{ 1H} NMR (CD3OD, δ (ppm) 52.71 (d, 2JPP, 41.6 Hz, PPh3, 51.56 dd, 2
    • PP = 41.6 Hz, dmoPTA).
  • 27
    • 42449140047 scopus 로고    scopus 로고
    • Magnetic susceptibility measurements on polycrystalline samples were carried out in the temperature range 1.9-300 K by means of a Quantum Design SQUID magnetometer operating at 10 000 Oe. Diamagnetic corrections of the constituent atoms were estimated from Pascal's constants. Experimental susceptibilities were also corrected for the magnetization of the sample holder
    • Magnetic susceptibility measurements on polycrystalline samples were carried out in the temperature range 1.9-300 K by means of a Quantum Design SQUID magnetometer operating at 10 000 Oe. Diamagnetic corrections of the constituent atoms were estimated from Pascal's constants. Experimental susceptibilities were also corrected for the magnetization of the sample holder.
  • 28
    • 42449103803 scopus 로고    scopus 로고
    • 2. (a) Altamore, A.; Cascarano, G.; Giacovazzo, C.; Guagliardi, A.; Moliterni, G.; Burla, M. C.; Polidori, G.; Camalli, M.; Spagna, R. Sir 97 Package Program; 1997.
    • 2. (a) Altamore, A.; Cascarano, G.; Giacovazzo, C.; Guagliardi, A.; Moliterni, G.; Burla, M. C.; Polidori, G.; Camalli, M.; Spagna, R. Sir 97 Package Program; 1997.
  • 29
    • 42449117862 scopus 로고    scopus 로고
    • Sheldrick, G. M. SHELXL, version 6.14; Bruker-AXS: Madison, WI, 2003. Crystallographic data were collected at 293(2) K on a Bruker APEX CCD diffractometer (XDIFRACT service of the University of Almería) with Mo Kα radiation (λ, 0.710 69 Å, Crystal data for 2 (CCDC 667604, 0.07 x 0.05 x 0.04 mm3, monoclinic P2 1/c, Z, 4, a, 12.154(5) Å, b, 35.492(5) Å, c, 9.884(5) Å, α, 90°, V, 4082(3) Å3, 14 ≤ h ≤ 13, 35 ≤ k ≤ 41, 11 ≤ l ≤ 11. Of the 6733 measured independent reflections in the θ range 1.75-24.44°, 3414 have I0 > 2σ(I0, R1, 0.0810, wR2, 0.1468. The function minimized during the refinement was w, 1/[σ 2(Fo2, 0.0631P)2, 0.0000P, where P, max
    • 3.
  • 42
    • 42449109761 scopus 로고    scopus 로고
    • 1H NMR. At 65°C, complex 2 catalyzed the isomerization of the substrate to give 3-butanone in 2.5 h, while 1 is not active. The addition of 2.5% water to the reaction increased the activity of 1, but the reactivity of 2 was even lower.
    • 1H NMR. At 65°C, complex 2 catalyzed the isomerization of the substrate to give 3-butanone in 2.5 h, while 1 is not active. The addition of 2.5% water to the reaction increased the activity of 1, but the reactivity of 2 was even lower.

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