metal-organic compounds
Acta Crystallographica Section C
Crystal Structure
Communications
bility in aromatic solvents compared with [Mo(phen)(CO)4]. It
could be the precursor for further reaction with fullerenes to
obtain complexes which are expected to have good solubility.
The structure determination of (I) indicated that the Mo-
atom coordination is distorted octahedral, with two CO
groups cis to each other, but each trans to an N atom of
dpphen (Fig. 1). The C2ÐMo1ÐN2 and C3ÐMo1ÐN1 bond
angles are 170.52 (87) and 170.97 (7)ꢁ, respectively. Atoms C2,
C3, N1, N2 and Mo1 are in the equatorial plane, coplanar to
ISSN 0108-2701
A molybdenum complex with
4,7-diphenyl-1,10-phenanthroline
Ê
within 0.07 A. The dihedral angle between the phen and C2/
Ê
Xiang-Jin Xie, Xiang-Lin Jin and Ka-Luo Tang*
C3/N1/N2/Mo1 planes is 10.70 (8) A and the two phenyl
groups make angles of 42.45 (7) and 54.05 (5)ꢁ with the phen
plane. The other two CO groups are trans to each other and on
the axis position of the distorted octahedron.
Institute of Physical Chemistry, Peking University, Beijing 100871, People's Republic
of China
Correspondence e-mail: jt1939@pku.edu.cn
Received 2 January 2001
Accepted 7 March 2001
In the title compound, tetracarbonyl(4,7-diphenyl-1,10-phen-
anthroline-N,N0)molybdenum(0), [Mo(C24H16N2)(CO)4], the
Mo-atom coordination is distorted octahedral, with two CO
groups cis to each other, but each trans to an N atom of the
4,7-diphenyl-1,10-phenanthroline (dpphen) ligand, and with
the other two CO groups trans to each other and on the axis
position. The complex has better solubility than
[Mo(phen)(CO)4], where phen is 1,10-phenanthroline.
Comment
As a precursor, [M(L±L)(CO)4] [M = Mo or W, L±L = 1,10-
phenanthroline (phen) or 2,20-bipyridine (bipy); Stiddard,
1962] was reacted with fullerene to form stable molybdenum
or tungsten complexes of fullerene [M(ꢀ2-C60)(L±L)(CO)3]
(Tang et al., 1996). These complexes are only sparingly soluble
in chlorobenzene and o-dichlorobenzene, and crystals suitable
for X-ray diffraction have not been obtained. However, when
one carbonyl group of [M(ꢀ2-C60)(phen)(CO)3] was displaced
by dibutyl maleate (dbm), the resulting [M(ꢀ2-C60)(phen)-
(dbm)(CO)2] complexes have good solubilities in a number of
organic solvents and their crystal structures were determined
Figure 1
The molecular structure of (I) shown with 50% probability displacement
ellipsoids.
Experimental
The title compound was prepared by the reaction of Mo(CO)6 and
dpphen (in a 1:1 molar ratio) in toluene under a nitrogen atmosphere
using Schlenk techniques, followed by chromatography over silica
gel. Red crystals were formed by diffusion of n-pentane into a
benzene solution of the title complex.
by X-ray diffraction (Tang et al., 1997). If dbm is replaced by
another C60 ligand, we can obtain dumb-bell [M(ꢀ2-C60)2-
(L±L)(CO)2] complexes, which are expected to have better
optical or electric properties than [M(ꢀ2-C60)(phen)(dbm)-
(CO)2] (Zhang et al., 1998). But the key problem is still the
poor solubility of the dumb-bell complex, making them dif®-
cult to analyse and use in applications. However, when two
phenyl groups were introduced into 1,10-phenanthroline, we
obtained the title complex, (I), which has much better solu-
Crystal data
3
[Mo(C24H16N2)(CO)4]
Mr = 540.37
Monoclinic, P21/c
Dx = 1.555 Mg m
Mo Kꢂ radiation
Cell parameters from 39 842
re¯ections
Ê
a = 9.8354 (1) A
b = 7.5648 (1) A
ꢃ = 2.4±27.5ꢁ
ꢄ = 0.61 mm
T = 123 (2) K
Ê
1
Ê
c = 31.1172 (4) A
ꢁ = 94.4628 (4)ꢁ
V = 2308.19 (5) A
Z = 4
3
Ê
Block, red
0.60 Â 0.40 Â 0.20 mm
ꢀ
696 # 2001 International Union of Crystallography
Printed in Great Britain ± all rights reserved
Acta Cryst. (2001). C57, 696±697
Xie
