Angewandte
Chemie
J. H. Teuben, G. Helgesson, M. Hµkansson, S. Jagner, A. L.
Spek, Organometallics 1993, 12, 2268 – 2276.
[4] J.-K. F. Buijink, J. H. Teuben, H. Kooijman, A. L. Spek, Organo-
metallics 1994, 13, 2922 – 2924.
disordered diethyl ether solvent molecule was located in the cell
at an inversion center. All non-hydrogen atoms were refined
with anisotropic displacement parameters. The residual peak
and hole electron densities were 0.267 and À0.374 eAÀ3
,
respectively. The absorption coefficient was 0.260 mmÀ1. The
least-squares refinement converged normally with residuals of
R(F) = 0.0461, wR(F2) = 0.0839 and a GOF = 0.835 (I > 2s(I)).
C55H66N2O0.5V, space group P2(1)/n, monoclinic, a =
11.5823(11), b = 15.0376(15), c = 26.496(2) , b = 101.522(3)8,
[5] a) B. Hessen, A. Meetsma, F. van Bolhuis, J. H. Teuben, G.
Helgesson, S. Jagner, Organometallics 1990, 9, 1925 – 1936; b) M.
Moore, S. Gambarotta, G. Yap, L. M. Liable-Sands, A. L.
Rheingold, Chem. Commun. 1997, 643 – 644; c) R. Milczarek,
W. Russeler, P. Binger, K. Jonas, K. Angermund, C. Kruger, M.
Regitz, Angew. Chem. 1987, 99, 957 – 958; Angew. Chem. Int. Ed.
Engl. 1987, 26, 908 – 909.
[6] For examples of vanadium(i) carbenes see: a) G. Erker, R. Lecht,
R. Schlund, K. Angermund, C. Kruger, Angew. Chem. 1987, 26,
708 – 710; Angew. Chem. Int. Ed. Engl. 1987, 26, 666 – 668; b) G.
Erker, R. Lecht, R. Schlund, K. Angermund, C. Kruger, 1987,
99, 708 – 709; c) M. Berlekamp, G. Erker, J. L. Petersen, J.
Organomet. Chem. 1993, 458, 97 – 103; d) M. Grehl, M. Berle-
kamp, G. Erker, Acta Crystallogr. Sect. C 1995, 51, 1772– 1774.
[7] F. Basuli, B. C. Bailey, J. Tomaszewski, J. C. Huffman, D. J.
Mindiola, J. Am. Chem. Soc. 2003, 125, 6052– 6053.
[8] P. H. M. Budzelaar, A. B. von Oort, A. G. Orpen, Eur. J. Inorg.
Chem. 1998, 1485 – 1494.
[9] See Supporting Information for complete experimental, spec-
tral, and crystallographic details.
[10] Crystallographic details for 2·2THF : A dark crystal of approx-
imate dimensions 0.30 0.30 0.06 mm3 was selected and
mounted on a glass fiber. A total of 88763 reflections (À54 ꢀ
h ꢀ 52, À20 ꢀ k ꢀ 20, À24 ꢀ l ꢀ 24) was collected at T= 136(2) K
in the range of 2.27 to 27.468, of which 8308 were observed
(Rint = 0.0957); MoKa radiation (l = 0.71073 ). A direct-meth-
ods solution was calculated which provided most non-hydrogen
atoms from the E-map. All non-hydrogen atoms were refined
with anisotropic displacement parameters. The residual peak
V= 4521.8(7) A3, Z = 4, 1calcd = 1.212 mgmÀ3 [17]
.
[14] Crystallographic details for 6: A crystal of approximate dimen-
sions 0.30 0.30 0.24 mm3 was selected and mounted on a glass
fiber. A total of 21477 reflections (À12 ꢀ h ꢀ 12, À13 ꢀ k ꢀ 15,
À23 ꢀ l ꢀ 23) was collected at T= 130(2) K in the range of 2.03
to 30.028, of which 7739 were observed (Rint = 0.0320); MoKa
radiation (l = 0.71073 ). A direct-methods solution was calcu-
lated which provided most non-hydrogen atoms from the E-map.
Full-matrix least-squares/difference Fourier cycles were per-
formed which located the remaining non-hydrogen atoms. All
non-hydrogen atoms were refined with anisotropic displacement
parameters. The residual peak and hole electron densities were
1.105 and À0.614 eAÀ3, respectively. The absorption coefficient
was 1.295 mmÀ1. The least-squares refinement converged nor-
mally with residuals of R(F) = 0.0341, wR(F2) = 0.0869 and a
¯
GOF = 1.020 (I > 2s(I)). C34H51IN2V, space group P1, triclinic,
a = 9.0935(4),
102.4790(10)8,
b = 11.0457(5),
c = 17.0793(8) ,
g = 98.7240(10)8,
a =
b = 92.1090(10)8,
V=
1651.30(13) A3, Z = 2, 1calcd = 1.339 mgmÀ3 [17]
.
[15] F. Basuli, J. Tomaszewski, J. C. Huffman, D. J. Mindiola, J. Am.
Chem. Soc. 2003, 125, 10170 – 10171.
[16] For an example of ATRP see: J. F. Lutz, D. Neugebauer, K.
Matyjaszewski, J. Am. Chem. Soc. 2003, 125, 6986 – 6993.
[17] CCDC-222957 (2), CCDC-222958 (3), CCDC-222959 (4),
CCDC-222960 (5), and CCDC-222961 (6) contain the supple-
mentary crystallographic data for this paper. These data can be
ving.html (or from the Cambridge Crystallographic Data Centre,
12, Union Road, Cambridge CB21EZ, UK; fax: (+ 44)1223-
336-033; or deposit@ccdc.cam.ac.uk).
and hole electron densities were 1.692and À0.604 eAÀ3
,
respectively. The absorption coefficient was 0.213 mmÀ1. The
least-squares refinement converged normally with residuals of
R(F) = 0.0733, wR(F2) = 0.2286, and a GOF = 0.934 (I > 2s(I)).
C70H95BN2O3V, space group C2/c, monoclinic, a = 42.3319(19),
b = 15.8991(7), c = 19.1013(9) , b = 110.2890(10)8, V=
12058.3(9) A3, Z = 8, 1calcd = 1.183 mgmÀ3, F(000) = 4648.[17]
[11] W.-K. Kim, M. J. Fevola, L. M. Liable-Sands, A. L. Rheingold,
K. H. Theopold, Organometallics 1998, 17, 4541 – 4543.
[12] Crystallographic details for 4: A crystal of approximate dimen-
sions 0.20 0.20 0.15 mm3 was selected and mounted on a glass
fiber. A total of 29941 reflections (À13 ꢀ h ꢀ 13, À36 ꢀ k ꢀ 36,
À13 ꢀ l ꢀ 15) was collected at T= 112(2) K in the range of 2.92
to 25.35o, of which 5437 were observed (Rint = 0.0804); MoKa
radiation (l = 0.71073 ). A direct-methods solution was calcu-
lated which provided most non-hydrogen atoms from the E-map.
Full-matrix least-squares/difference Fourier cycles were per-
formed which located the remaining non-hydrogen atoms. The
residual peak and hole electron densities were 1.104 and
À0.608 eAÀ3
, respectively. The absorption coefficient was
1.215 mmÀ1. The least-squares refinement converged normally
with residuals of R(F) = 0.0387, wR(F2) = 0.0810 and a GOF =
0.894 (I > 2s(I)). C34H51IN2V, space group P2(1)/n, monoclinic,
a = 10.4492(9), b = 27.924(2), c = 12.3261(10) , b = 107.904(2)8,
V= 3422.4(5) A3, Z = 4, 1calcd = 1.292 mgmÀ3 [17]
.
[13] Crystallographic details for 5·2Et2O: A crystal of approximate
dimensions 0.25 0.25 0.08 mm3 was selected and mounted on
a glass fiber. A total of 43991 reflections (À15 ꢀ h ꢀ 15, À19 ꢀ
k ꢀ 19, À27 ꢀ l ꢀ 34) was collected at T= 111(2) K in the range
of 2.07 to 27.538, of which 5447 were observed (Rint = 0.1258);
MoKa radiation (l = 0.71073 ). A direct-methods solution was
calculated which provided most non-hydrogen atoms from the
E-map. Full-matrix least-squares/difference Fourier cycles were
performed which located the remaining non-hydrogen atoms. A
Angew. Chem. Int. Ed. 2004, 43, 3156 –3159
ꢀ 2004 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
3159