Collect. Czech. Chem. Commun. 2010, 75, 807-812
https://doi.org/10.1135/cccc2010053
Published online 2010-08-12 09:56:50

Macropolyhedral boron-containing cluster chemistry [S2B16H17]–. A new eighteen-vertex thiaborane anion

Michael J. Carra,b, William Cleggc, John D. Kennedyb,*, Michael G. S. Londesborougha and Colin A. Kilnerb

a Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic, 250 68 Řež near Prague, Czech Republic
b The School of Chemistry of the University of Leeds, Leeds, UK LS2 9JT, England
c The School of Natural Sciences (Chemistry), The University of Newcastle-upon-Tyne, UK NE1 7RU, England

References

1. Kennedy J. D. in: Advances in Boron Chemistry (W. Siebert, Ed.), p. 451. Royal Society of Chemistry, Cambridge 1997.
2. Bould J., Clegg W., Teat S. J., Barton L., Rath N. P., Thornton-Pett M., Kennedy J. D.: Boron Chemistry at the Millennium, special edition of Inorg. Chim. Acta 1999, 289, 95. <https://doi.org/10.1016/S0020-1693(99)00071-7>
3. Bould J., Ormsby D. L., Yao H.-J., Hu C.-H., Sun J., Jin R.-S., Shea S. L., Clegg W., Jelínek T., Rath N. P., Thornton-Pett M., Greatrex R., Zheng P-J., Barton L., Štíbr B., Kennedy J. D. in: Contemporary Boron Chemistry (M. Davidson, A. K. Hughes, T. B. Marder and K. Wade, Eds), p. 171. Royal Society of Chemistry, Cambridge 2000.
4. Jelínek T., Kennedy J. D., Barrett S. A., Thornton-Pett M., Císařová I. in: Contemporary Boron Chemistry (M. Davidson, A. K. Hughes, T. B. Marder and K. Wade, Eds), p. 175. Royal Society of Chemistry, Cambridge 2000.
5. Shea S. L., Bould J., Londesborough M. G. S., Perera S. D., Franken A., Ormsby D. L., Jelínek T., Štíbr B., Holub J., Kilner C. A., Thornton-Pett M., Kennedy J. D.: Pure Appl. Chem. 2003, 75, 1239. <https://doi.org/10.1351/pac200375091239>
6. Londesborough M. G. S., MacLean E. J., Teat S. J., Bould J., Kilner C. A., Thornton-Pett M., Kennedy J. D.: Boron Chemistry at the Beginning of the 21st Century (Yu. Bubnov, Ed.), p. 248. Editorial URSS, Moscow 2003.
7. Shea S. L., Perera S. D., Bould J., Franken A., Jelínek T., Kennedy J. D., Kilner C. A., Londesborough M. G. S., Thornton-Pett. M.: Boron Chemistry at the Beginning of the 21st Century (Yu. Bubnov, Ed.), p. 27. Editorial URSS, Moscow 2003.
8. Jelínek T., Kennedy J. D., Štíbr B.: J. Chem. Soc., Chem. Commun. 1994, 1415. <https://doi.org/10.1039/c39940001415>
9. Dosangh P. K., Bould J., Londesborough M. G. S., Jelínek T., Thornton-Pett M., Štíbr B., Kennedy J. D.: J. Organomet. Chem. 2003, 680, 312. <https://doi.org/10.1016/S0022-328X(03)00467-4>
10. Kaur P., Thornton-Pett M., Clegg W., Kennedy J. D.: J. Chem. Soc., Dalton Trans. 1996, 4155. <https://doi.org/10.1039/dt9960004155>
11. Jelínek T., Kilner C., Thornton-Pett M., Kennedy J. D.: Chem. Commun. 1999, 1905. <https://doi.org/10.1039/a905473a>
12. Kaur P., Holub J., Rath N. P., Bould J., Barton L., Štíbr B., Kennedy J. D.: Chem. Commun. 1996, 273. <https://doi.org/10.1039/cc9960000273>
13. Jelínek T., Kennedy J. D., Štíbr B., Thornton-Pett M.: Inorg. Chem. Commun. 1998, 1, 179. <https://doi.org/10.1016/S1387-7003(98)00049-5>
14. Jelínek T., Kennedy J. D., Štíbr B., Thornton-Pett M.: Angew. Chem., Int. Ed. Engl. 1994, 33, 1599. <https://doi.org/10.1002/anie.199415991>
15. Ormsby D. L., Greatrex R., Kennedy J. D.: Dalton Trans. (K. Wade Special Edition) 2008, 1625. <https://doi.org/10.1039/b715915c>
16. Jelínek T., Císařová, Štíbr B., Kennedy J. D., Thornton-Pett. M.: J. Chem. Soc., Dalton Trans. (Dalton Commun.) 1998, 2965. <https://doi.org/10.1039/a805791e>
17. X-ray data. Compound 1a: C14H36B16N2S3: M = 469.53, triclinic (0.2 × 0.02 × 0.01 mm, yellow needle from CH3(CH2)3CH3/CD2Cl2CH2Cl2), space group P1, a = 8.9490(15) Å, b = 12.665 (2) Å, c = 13.190(2) Å, α = 71.430(2)°, β = 89.683(2)°, γ = 69.523(2)°, U = 1318.1(4) Å3, Dcalc = 1.183 mg m–3, Z = 2, λ = 0.6814 Å (synchrotron, wiggler-generated, Station 9.8, UK National SRS facility, Daresbury)18, μ = 0.211 mm–1, T = 150(2) K, R1 = 0.0722 for 2805 reflections with I > 2σ(I), and wR2 = 0.2152 for all data. Methods and programs were standard (Sheldrick G. M.: SHELX97. Acta Crystallogr., Sect. A 2008, 64, 112; Sheldrick G. M.: SHELXTL Manual. Bruker AXS Inc., Madison (WI) 1994 and 1998; Farrugia L. J.: ORTEP-3 J. Appl. Crystallogr. 1997, 30, 565). CCDC deposition number 779102.
18. Cernik R. J., Clegg W., Catlow C. R. A., Bushnell-Wye G., Flaherty J. V., Greaves G. N., Burrows I., Taylor D. J., Teat S. J., Hamichi M.: J. Synchrotron Radiat. 1997, 4, 279. <https://doi.org/10.1107/S090904959701008X>
19. NMR data. 11B and 1H NMR chemical shifts for the [S2B16H17]– anion 1, measured as its [tmndH]+ salt in CD2Cl2 at 300 K; ordered as assignment, δ(11B) in ppm relative to [BF3(OEt2)] (δ(1H) in ppm relative to TMS of directly attached exo-hydrogen atoms in square brackets): BH(2) +16.7 [+4.48], B(6) +8.8 [conjuncto position, no exo-H], BH(3′) +4.7 [+1.40], BH(8) +2.9 [+3.33], BH(4) +1.5 [+3.23], BH(1′) –5.0 [+2.78], BH(6′) –8.2 [+2.54], BH(5′) –11.2 [+2.35], BH(10) –17.9 [+1.69], BH(1) –19.0 [+1.56], B(7) –25.3 [exo-sulfur-bound position, no exo-H], BH(3) –26.9 [+1.03], BH(5) –30.9 [+1.45], BH(2′) –32.6 [+1.21], BH(7′) –32.6 [+ 0.71] and BH(4′) –34.3 [+ 0.80], with δ(1H) for μH(3′,4′) –0.38, μH(6′,7′) –1.08 and μH(5,10) –1.62 ppm. Assignments by [11B-11B]-{1H(broadband)}-COSY, [1H-1H]-{11B(broadband)}-COSY and 1H-{11B (selective)} multiple resonance experiments.
20. Carr M. J., Londesborough M. G. S., Hamilton Mcleod A. R., Kennedy J. D.: Dalton Trans. (Dalton Commun.) 2006, 3624.
21. Bould J., Clegg W., Kennedy J. D., Teat S. J.: J. Chem. Soc., Dalton Trans. 1998, 2777. <https://doi.org/10.1039/a803817a>
22. Cheek Y. M., Greenwood N. N., Kennedy J. D., McDonald W. S.: J. Chem. Soc., Chem. Commun. 1982, 80. <https://doi.org/10.1039/c39820000080>
23. McGrath T. D., Kennedy J. D., McInnes Y. M., Thornton-Pett M. in: Advances in Boron Chemistry (W. Siebert, Ed.), p. 480. Royal Society of Chemistry, Cambridge 1997.
24. Carr M. J., Londesborough M. G. S., Bould J., Císařová I., Kennedy J. D.: Collect. Czech. Chem. Commun. 2005, 70, 430. <https://doi.org/10.1135/cccc20050430>