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Heterobimetallic Complexes with Phenylcyclopentadienyl Ligand: Syntheses and Structures of Tricarbonylchromium−η6,η5-Phenylcyclopentadienyl−Transition Metal Complexes1
dataset
posted on 1997-03-26, 00:00 authored by Changtao Qian, Jianhua Guo, Jie Sun, Jian Chen, Peiju ZhengA new synthetic method of heterobimetallic complexes bridging with
a π,π-phenylcyclopentadienyl ligand,
tricarbonylchromium−η6,η5-phenylcyclopentadienyl−transition
metal complexes, was developed through the
reactions of
(η6-C6H5C5H5)Cr(CO)3
or its sodium salt with transition metal complexes. The method is
suitable
for most transition metal elements with the advantages of easy
manipulation, mild reaction conditions, and moderate
to high yields. As indicated by 1H NMR spectra, the
interactions between the two π systems of phenyl and
cyclopentadienyl rings were weak. X-ray crystal structures of
seven complexes were studied. Compound 23,
[η6-C6H5Cr(CO)3]2C10H10,
crystallizes in orthorhombic space group Pbca with cell
constants a = 29.616(8) Å,
b = 12.861(5) Å, c = 12.397(7) Å,
V = 4721(6) Å3, Z = 8,
R = 0.045, and Rw = 0.045.
Compound 3, (η6-C6H5C9H7)Cr(CO)3,
crystallizes in monoclinic space group
P21/c with cell constants
a = 7.901(3) Å, b =
14.799(2) Å, c = 12.917(2) Å, β = 99.72(2)°,
V = 1488.7(4) Å3, Z = 4,
R = 0.044, and Rw = 0.051.
Compound 7,
Cr(CO)3(η6,η5-C6H5C5H4)Ti(CO)2(η5-C5H5),
crystallizes in monoclinic space group
P21/c with cell constants
a
= 12.361(4) Å, b = 12.487(6) Å, c
= 12.531(7) Å, β = 93.48(4)°, V = 1930
Å3, Z = 4, R = 0.047, and
Rw =
0.048. Compound 13,
Cr(CO)3(η6,η5-C6H5C5H4)Mo(CO)3Br,
crystallizes in monoclinic space group
P21/c with
cell constants a = 14.685(2) Å, b =
8.509(3) Å, c = 14.960(3) Å, β =
104.46(1)°, V = 1810.0(7) Å3,
Z = 4, R
= 0.037, and Rw = 0.037. Compound
19,
Cr(CO)3(η6,η5-C6H5C9H6)Mn(CO)3,
crystallizes in triclinic space group
P-1 with cell constants
a = 11.660(4) Å, b = 12.578(5) Å,
c = 6.987(2) Å, α = 100.03(3)°, β =
104.19(2)°, γ
= 71.99(3)°, V = 939.3(6) Å3,
Z = 2, R = 0.048, and
Rw = 0.065. Compound 21,
Cr(CO)3(η6,η5-C6H5C5H4)Ru(PPh3)2Cl,
crystallizes with one molecule of EtOH in triclinic space group
P-1 with cell
constants
a = 14.033(4) Å, b = 16.163(6) Å,
c = 10.411(3) Å, α = 104.22(3)°, β =
103.50(2)°, γ = 90.81(3)°, V
=
2219(1) Å3, Z = 2, R =
0.081, and Rw = 0.096. Compound
22,
Cr(CO)3(η6,η5-C6H5C5H4)Co(CO)2,
crystallizes
in orthorhombic space group
P212121 with cell
constants a = 15.083(5) Å, b =
16.391(5) Å, c = 6.351(4) Å,
V
= 1570(1) Å3, Z = 4, R =
0.036, and Rw = 0.039. The
trans configurations of the two metal atoms in
these
molecules were found as expected; the phenyl and cyclopentadienyl or
indenyl rings in the molecules were found
to be not coplanar.
