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Volumn 48, Issue 5, 2009, Pages 1805-1807

Unprecedented linking of two polyoxometalate units with a metal-metal multiple bond

(6) Sokolov, Maxim N a,b Korenev, Vladimir S a Izarova, Natalya V a Peresypkina, Eugenia V a Vicent, Cristian c Fedin, Vladimir P a,b

a NIKOLAEV INSTITUTE OF INORGANIC CHEMISTRY (Russian Federation)

b NOVOSIBIRSK STATE UNIVERSITY (Russian Federation)

c UNIVERSITAT JAUME I (Spain)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 64549131319 PISSN: 00201669 EISSN: None Source Type: Journal
DOI: 10.1021/ic802373j Document Type: Article

Times cited : (16)

References (27)

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6
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- J. Mol. Catal. A: Chem. 2007, 262(special issue Polyoxometalates in Catalysis; Hill, C. L., Ed.).
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- (1999) Metal Clusters in Chemistry , vol.1 , pp. 444
- Cavaleiro, A.M.V.¹ Pedrosa de Jesus, J.D.² Noguera, H.I.S.³

8
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- Meiklejohn, P.T.¹ Pope, M.T.² Prados, R.A.³

9
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- (b) Ortega, F.; Pope, M. T.; Ewans, H. T., Jr Inorg. Chem. 1997, 36, 2166.
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- Ortega, F.¹ Pope, M.T.² Ewans Jr, H.T.³

10
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11
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14
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- Wei, X.; Bachman, R. E.; Pope, M. T. J. Chem. Soc. 1998, 120, 10248.
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15
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16
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- Catalytic applications of dimolybdenum and ditungsten complexes containing multiple metal-metal bonds
- Adams, R. D, Cotton, F. A, Eds, Wiley-VCH Inc, New York
- Mc Cann, M. Catalytic applications of dimolybdenum and ditungsten complexes containing multiple metal-metal bonds. In Catalysis by di- and polynuclear metal cluster complexes; Adams, R. D., Cotton, F. A., Eds.; Wiley-VCH Inc.: New York, 1998; pp 145-166.
- (1998) Catalysis by di- and polynuclear metal cluster complexes , pp. 145-166
- Mc Cann, M.¹

17
- 64549161398
- A total of 1.00 g (0.31 mmo1) of K7[PW11O 39]• 14H2O was dissolved in 30 mL of water while stirring and heating gently (50 °C, then 0.18 g (0.16 mmol) of [Bu 4[Re2Cl8] was added, and the pH was adjusted to 1 with 2 M HC1. The mixture was stirred for 12 h at room temperature, during which time it became brown. Then it was heated at 80 °C for 30 min and filtered to remove a brown precipitate. The filtrate was added to an aqueous solution of 1 g (3.10 mmol) of [N(C4H9)4]Br, the precipitate was collected by filtration and dissolved in acetonitrile, and the solution was allowed to evaporate slowly in an open vial to give brown needlelike crystals of 1. Repeated recrystallization gave pure compound 1. Yield: 0.12 g 11% based on {PW11, Anal. Calcd for C 99H222.5N7.5O78P2Re 2W22: C
- 3-O-W). 754 s, 593 s, 516 s, 486 s.

18
- 0003989668
- 2nd ed, Clarendon Press: Oxford, U.K
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- (1993) Multiple Bonds between Metal Atoms
- Cotton, F.A.¹ Walton, R.A.²

19
- 64549159629
- The diffraction data for 1 and 2 were collected on a Bruker X8APEX CCD diffractometer with Mo Kα radiation (λ, 0.710 73 Å) using combined φ and ω scans of narrow (0.5°) frames. The structure was solved by direct methods and refined by a full-matrix least-squares method against F2in an anisotropic approximation using the SHELKTL program set.12 Absorption corrections were applied empirically using the SADABS program.13 Crystal data for 1: C99H222. 5N7.5O78P 2Re2W22, monoclinic. space group P2 1lc, a, 14.2256(4) Å b, 31.3989(11) Å, c, 18.8250(6) Å,β, 93.8180(10)°, T, 150.0(2) K, Z, 2, V, 8389.9(5) Å3, ρcalc, 2.868 g/cm3, 2θ max, 54.96°, μ, 16.548 mm-1, 55 012 reflections collected within -18 ≥
- max= 0.332/0.610.

20
- 64549141417
- SHELXTL, version 6.22; Bruker AXS Inc, Madison, WI, 2003
- SHELXTL, version 6.22; Bruker AXS Inc.: Madison, WI, 2003.

21
- 26944459109
- Bruker-Nonius: Dordrecht, The Netherlands
- Sheldrick, G. M. SADABS, Program for empirical X-ray absorption correction; Bruker-Nonius: Dordrecht, The Netherlands, 1990.
- (1990) SADABS, Program for empirical X-ray absorption correction
- Sheldrick, G.M.¹

22
- 64549139586
- In one of the preparations with different amounts of Bu4NBr, crystals of (Bu4N)7(H)[Re2(PW 11O39)2]•nH2O and (Bu 4N)4(H)4[Re2-(PW11O 39)2]•H2O were obtained together with 1. The overall composition was confirmed by X-ray data, but severe disorder and the poor quality of the single crystals have so far precluded satisfactory refinement
- 2O were obtained together with 1. The overall composition was confirmed by X-ray data, but severe disorder and the poor quality of the single crystals have so far precluded satisfactory refinement.

23
- 64549143252
- Bond distances (Å) and angles (deg) in 1: W-μ4-O 2.425(8)-2.464(8, W-μ2-Ow 1.868(9)-1.952(9, W-μ2-ORe 1.865(8)-1.918(8, W-Oterm 1.688(8)-1.710(9, P-Ow 1.525(8)-1.537(8, W-μ4-O-W 89.1(3)-90.4(3, W-μ4-O-P 123.9(4)-127.6(5, Re-μ4- O-W 88.4(3)-88.7(3, Re-μ4-O-P123.4(4, W-μ2-O-W125. 3(4)-128.2(4) and 150.0(5)-151.7(5, W-μ-O-Re 124.9(4, 126.0(4) and 147.6(4, 148.4(5, O-Re-O 72.4(3)-91.6(4) and 160.3(3, 160.7(3, O-P-O 108.7(5)-110.25
- 2-O-W125. 3(4)-128.2(4) and 150.0(5)-151.7(5), W-μ-O-Re 124.9(4), 126.0(4) and 147.6(4). 148.4(5), O-Re-O 72.4(3)-91.6(4) and 160.3(3), 160.7(3), O-P-O 108.7(5)-110.2(5).

24
- 64549098029
- Bond distances (Å) and angles (deg) in 2: W-μ4-O 2.405(10)-2.486(10, W-μ2-Ow 1.864(10)-1.949(11, W-μ2-ORe 1.891(10)-1.934(10, W-Oterm, 1.678(10)-1.716(11, P-Ow 1.519(10)-1.525(10) Å; W-μ4-O-W 88.3(3)-90.0(3, W-μ4-O-P 125.5(6)-128.4(6, Re-μ4-O-W 87.4(3, 88.2(3, Re-μ4-O-P 122.1(5, W-μ2-O-W 125.1(6)-129.1(6) and 149.9(5)-153.3(6, W-μ2-O-Re 123.8(5, 125.1(6) and 147.9(5, 149.9(6, O-Re-O 86.0(4)-92.0(4) and 160.6(4, 161.2(4, O-P-O 108.0(6)-110.56
- 2-O-Re 123.8(5), 125.1(6) and 147.9(5), 149.9(6), O-Re-O 86.0(4)-92.0(4) and 160.6(4), 161.2(4), O-P-O 108.0(6)-110.5(6).

25
- 64549154301
- Polyoxometalates. Molecular Science
- Borras-Almenar, J. J, Coronado, E, Muller, A, Pope, M, Eds, Kluwer Academic Publishers: Dordrecht, The Netherlands, 98; pp
- Pope, M. T. In Polyoxometalates. Molecular Science; Borras-Almenar, J. J., Coronado, E., Muller, A., Pope, M., Eds.; NATO Science Series II; Kluwer Academic Publishers: Dordrecht, The Netherlands, 2001; Vol. 98; pp 3-31.
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- Pope, M.T.¹

26
- 64549158705
- A Q-TOF premier mass spectrometer with an orthogonal Z-spray electrospray source (Waters, Manchester, U.K, was used. The temperature of the source block was set to 80 °C and the desolvation temperature to 100 °C. A capillary voltage of 3.0 kV was used in the negative scan mode, and the cone voltage was set to 10 V to control the extent of fragmentation. Time-of-flight mass spectra were acquired in the V-mode operating at a resolution of ca. 10 000 (full width at half-maximum) at mlz 2000. Mass calibration was performed using a solution of sodium iodide in isopropyl alcohol/water (50:50) from mlz 100 to 2800. Acetonitrile/acetone (5:1) sample solutions were infused via a syringe pump directly connected to the ESI-MS source at a flow rate of 10 μL/min. The observed isotopic pattern of each compound perfectly matched the theoretical isotopic pattern calculated from their elemental composition using the MassLynx 4.1 program
- A Q-TOF premier mass spectrometer with an orthogonal Z-spray electrospray source (Waters, Manchester, U.K.) was used. The temperature of the source block was set to 80 °C and the desolvation temperature to 100 °C. A capillary voltage of 3.0 kV was used in the negative scan mode, and the cone voltage was set to 10 V to control the extent of fragmentation. Time-of-flight mass spectra were acquired in the V-mode operating at a resolution of ca. 10 000 (full width at half-maximum) at mlz 2000. Mass calibration was performed using a solution of sodium iodide in isopropyl alcohol/water (50:50) from mlz 100 to 2800. Acetonitrile/acetone (5:1) sample solutions were infused via a syringe pump directly connected to the ESI-MS source at a flow rate of 10 μL/min. The observed isotopic pattern of each compound perfectly matched the theoretical isotopic pattern calculated from their elemental composition using the MassLynx 4.1 program.

27
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- Long, D. L.; Streb, C.; Song, Y. F.; Mitchell, S.; Cronin, L. J. Am. Chem. Soc. 2008, 130, 1830.
- (2008) J. Am. Chem. Soc , vol.130 , pp. 1830
- Long, D.L.¹ Streb, C.² Song, Y.F.³ Mitchell, S.⁴ Cronin, L.⁵

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