Inorganic Chemistry
ARTICLE
tube with the reaction mixture in liquid nitrogen. The polymer formed
was diluted with CHCl3 (ca. 5 mL) and precipitated with an excess of
n-hexane. This procedure was repeated one more time, and the polymer
obtained was dried at 50 °C under vacuum to the constant weight.
Monomer conversion was determined gravimetrically. All polymers
obtained by this method were then analyzed by SEC on a Knauer
instrument equipped with two polystyrene gel columns (Phenomenex,
pore size 103À105 Å) and an RI Detector K-2301 differential refract-
ometer as the detector. THF was used as the eluent. The columns
were calibrated against 8 standard poly(methyl methacrylate) samples
received from Waters (the Mn varies from 2580 to 9.81 Â 105).
X-ray Diffraction Studies of Complexes 3À7. Single-crystal
X-ray diffraction experiment in all cases was carried out with a Bruker
SMART APEX II diffractometer (graphite monochromated Mo KR
radiation, λ = 0.710 73 Å, ω-scan technique, T = 100 K). The APEX II
software23 was used for collecting frames of data, indexing reflections,
determination of lattice constants, integration of intensities of reflec-
tions, scaling, and absorption correction, and SHELXTL24 was used for
space group and structure determination, refinements, graphics, and
structure reporting. The structures were solved by direct methods and
refined by the full-matrix least-squares technique against F2 with the
anisotropic temperature factors for all non-hydrogen atoms. The hydro-
gen atoms of carborane moieties in structures 3À7 as well as the hydride
ligand in complex 3 were located from difference Fourier maps and
refined isotropically. The H(C) atoms were placed geometrically and
included in the structure factors calculation in the riding motion
approximation. The principal experimental and crystallographic para-
meters are presented in Tables 4 and 5.
Noels, A. F. Can. J. Chem. 2001, 79, 529. (g) Delaude, L.; Delfosse, S.;
Richel, A; Demonceau, A.; Noels, A. F. Chem. Commun. 2003, 1526.
(h) Richel, A; Delfosse, S.; Cremasco, C.; Delaude, L.; Demonceau, A.;
Noels, A. F. Tetrahedron Lett. 2003, 44, 6011. (i) Borguet, Y.; Sauvage,
X.; Bicchielli, D.; Delfosse, S.; Delaude, L.; Demonceau, A.; Bareille, L.
Controlled/Living Radical Polymerization: Progress in ATRP; ACS Sym-
posium Series; American Chemical Society: Washington, DC, 2009;
Vol. 1023, Chapter 7, p 97. (j) Kato, M.; Kamigaito, M.; Sawamoto, M.;
Higashimura, T. Macromolecules 1995, 28, 1721. (k) Ando, T.; Kato, M.;
Kamigaito, M.; Sawamoto, M. Macromolecules 1996, 29, 1070. (l) Simal,
F.; Demonceau, A.; Noels, A. F. Tetrahedron Lett. 1999, 40, 5689.
(m) Simal, F.; Sebille, S.; Demonceau, A.; Noels, A. F.; Nun~ez, R.; Abad,
M.; Teixidor, F.; Vinas, C. Tetrahedron Lett. 2000, 41, 5347. (n) Tutusaus,
O.; Nu~nez, R.; Vinas, C.; Teixidor, F.; Mata, I.; Molins, E. Inorg. Chem.
2004, 43, 6067.
(4) (a) Hawthorne, M. F. Acc. Chem. Res. 1968, 1, 281. (b) Callahan,
K. P.; Hawthorne, M. F. Adv. Organomet. Chem. 1976, 145. (c) Hanusa,
T. P. Polyhedron 1982, 1, 663. (d) Warren, L. F.; Hawthorne, M. F. J. Am.
Chem. Soc. 1970, 92, 1157. (e) Clair, D. S.; Zalkin, A.; Templeton, D. H.
J. Am. Chem. Soc. 1970, 92, 1173.
(5) (a) Wong, E. H. S.; Hawthorne, M. F. J. Chem. Soc., Chem. Commun.
1976, 257. (b) Wong, E. H. S.; Hawthorne, M. F. Inorg. Chem. 1978,
17, 2863. (c) Chizhevsky, I. T.; Lobanova, I. A.; Bregadze, V. I.; Petrovskii,
P. V.; Polyakov, A. V.; Yanovsky, A. I.; Struchkov, Yu. T. Organomet. Chem.
USSR (Engl. Transl.) 1991, 4, 469. (d) Cheredilin, D. N.; Dolgushin, F. M.;
Grishin, I. D.; Kolyakina, E. V.; Nikiforov, A. S.; Solodovnikov, S. P.; Il’in,
M. M.; Davankov, V. A.; Chizhevsky, I. T.; Grishin, D. F. Russ. Chem. Bull.
2006, 55, 1163. (e) Ellis, D. D.; Couchman, S. M.; Jeffery, J. C.; Malget,
J. M.; Stone, F. G. A. Inorg. Chem. 1999, 38, 2981.
(6) Cheredilin, D. N.; Balagurova, E. V.; Godovikov, I. A.; Solodovnikov,
S. P.; Chizhevsky, I. T. Russ. Chem. Bull. 2005, 54, 2535.
(7) (a) Kolyakina, E. V.; Grishin, I. D.; Cheredilin, D. N.; Dolgushin,
F. M.; Chizhevsky, I. T.; Grishin, D. F. Russ. Chem. Bull. 2006, 55, 89.
(b) Grishin, I. D.; Kolyakina, E. V.; Cheredilin, D. N.; Chizhevsky, I. T.;
Grishin, D. F. Polym. Sci. A 2007, 49, 1079. (c) Grishin, I. D.;
Chizhevsky, I. T.; Grishin, D. F. Dokl. Chem. 2008, 423, 290. (d) Grishin,
I. D.; Chizhevsky, I. T.; Grishin, D. F. Kinet. Catal. 2009, 50, 550.
(e) Grishin, D. F.; Grishin, I. D.; Chizhevsky, I. T. Controlled/Living Radical
Polymerization: Progress in ATRP; ACS Symposium Series; American Chemical
Society: Washington, DC, 2009; Vol. 1023, Chapter 8, p 115.
’ ASSOCIATED CONTENT
S
Supporting Information. CIF files giving X-ray crystal-
b
lographic data for complexes 3, 4, 5, 6, and 7. Cartesian coor-
dinates of all optimized structures with energies. This material is
’ AUTHOR INFORMATION
(8) Grishin, I. D.; D’iachikhin, D. I.; Dolgushin, F. M.; Grishin, D. F.;
Chizhevsky, I. T. Abstracts of the Fifth European Meeting on Boron
Chemistry (EUROBORON 5); Heriot-Watt University, Edinburgh,
U.K., August 29ÀSeptember 2, 2010; Abstract no. O 18, p 39.
(9) (a) Crook, J. E.; Greenwood, N. N.; Kennedy, J. D.; McDonald,
W. S. J. Chem. Soc., Chem. Commun. 1981, 933. (b) Kukina, G. A.; Sergienko,
V. S.; Porai-Koshits, M. A. Koord. Khim. 1985, 11, 400. (c) McGrath, T. D.;
Franken, A.; Kautz, J. A.; Stone, F. G. A. Inorg. Chem. 2005, 44, 8135.
(10) Cheredilin, D. N.; Kadyrov, R.; Dolgushin, F. M.; Balagurova,
E. V.; Godovikov, I. A.; Solodovnikov, S. P.; Chizhevsky, I. T. Inorg.
Chem. Commun. 2005, 8, 614.
Corresponding Author
*E-mail: chizbor@ineos.ac.ru.
’ ACKNOWLEDGMENT
This work has been supported by Grants 09-03-00211, 10-03-
00505, and 11-03-00074 from the Russian Foundation for Basic
Research. The authors are also grateful to Dr. M. G. Ezernitskaya
for recording IR spectra of complexes 3À7.
(11) (a) Bould, J.; Crook, J. E.; Greenwood, N. N.; Kennedy, J. D.;
McDonald, W. S. J. Chem. Soc., Chem. Commun. 1982, 465. (b) Bould, J.;
Crook, J. E.; Greenwood, N. N.; Kennedy, J. D.; McDonald, W. S.
J. Chem. Soc., Chem. Commun. 1983, 949. (c) Elrinton, M.; Greenwood,
N. N.; Kennedy, J. D.; Thornton-Pett, M. J. Chem. Soc., Dalton Trans.
1986, 2277. (d) Ferguson, G.; Jennings, M. C.; Lough, A. J.; Loughlan,
S.; Spalding, T. R.; Kennedy, J. D.; Fontain, X. R. L J. Chem. Soc., Chem.
Commun. 1990, 891. (e) Bould, J.; Greenwood, N. N.; Kennedy, J. D.
J. Chem. Soc., Dalton Trans. 1990, 1451. (f) Bould, J.; Brint, P.; Kennedy,
J. D.; Thornton-Pett, M. J. Chem. Soc., Dalton Trans. 1993, 2335.
(g) Dou, J.-M.; Hu, C.-H.; Li, W.; Yao, H.-J.; Jin, R.-S.; Zheng, P.-J.
Polyhedron 1997, 16, 2323. (h) Bould, J.; Clegg, W.; Teat, S. J.; Barton,
L.; Rath, N. P.; Thornton-Pett, M.; Kennedy, J. D. Inorg. Chim. Acta
1999, 289, 95.
’ REFERENCES
(1) (a) Kharasch, M. S.; Jensen, E. V.; Urry, W. H. Science 1945,
102, 128. (b) Kharasch, M. S.; Urry, W. H.; Jensen, E. V. J. Am. Chem. Soc.
1945, 67, 1626.
(2) See for the latest reviews: (a) di Lena, F.; Matyjaszewski, K. Prog.
Polym. Sci. 2010, 35, 959. (b) Ouchi, M.; Terashima, T.; Sawamoto, M.
Chem. Rev. 2009, 109, 4963. (c) Grishin, I. D.; Grishin, D. F. Russ. Chem.
Rev. 2008, 77, 633.
(3) (a) Takahashi, H.; Ando, T.; Kamigaito, M.; Sawamoto, M.
Macromolecules 1999, 32, 3820. (b) Ando, T.; Kamigaito, M.; Sawamoto,
M. Macromolecules 2000, 33, 5825. (c) Watanable, Y.; Ando, T.;
Kamigaito, M.; Sawamoto, M. Macromolecules 2001, 34, 4370.
(d) Tutusaus, O.; Delfosse, S.; Simal, F.; Demonceau, A.; Noels, A. F.;
Nu~nez, R.; Vinas, C.; Teixidor, F. Inorg. Chem. Commun. 2002, 941.
(e) Simal, F.; Demonceau, A.; Noels, A. F. Angew. Chem., Int. Ed. 1999,
38, 538. (f) Simal, F.; Jan, D; Delaude, L.; Demonceau, A.; Spirlet, M.-R.;
(12) (a) Lahiri, G. K.; Bhattacharya, S.; Mukherjee, M.; Mukherjee,
A. K.; Chakravorty, A. Inorg. Chem. 1987, 26, 3359. (b) Munshi, P.;
Samanta, R.; Lahiri, G. K. J. Organomet. Chem. 1999, 586, 176.
7584
dx.doi.org/10.1021/ic200487w |Inorg. Chem. 2011, 50, 7574–7585