2370
KATLENOK, BALASHEV
3
3
complexes are characterized by only weak inner ligand
fluorescence.
7.85 d (2Н6', JHH 7.4), 7.55 d.d (2Нm, JHH 7.4, 7.5),
7.45 d. d (2Нp, JHH 7.3, 7.5), 7.32 d. d (2H6, JHH 8.4,
3
3
4JHH 1.5), 7.22 m (6Н5',m',p'), 6.81 d (2Н3', JHH 0.4),
4
Complexes of Pd(II) and Rh(III) were obtained at
refluxing Pd(OOCCH3)2 and RhCl3·3H2O with 2-(4-
biphenyl)-5-phenylbenzoxazole in acetic acid and 2-
methoxyethanol medium, respectively, that led to the
3
4.88 d (2Нα, JHH 10.5), 4.28 m (2Нδ), 2.72 d (2Нβ,
3JHH 10.5), 2.69 d (2Нγ, 3JHH 12.3). IR spectrum (KBr),
ν, cm–1: 3356, 3296 (NH2), 1600 (C=N), 1587 (C2H4),
844, 868 (C6H3, biphenyl metalated ring). Absorption
spectrum (CH3CN), λmax, nm (ε×10–3, mol–1 cm–1): 231
(36.3), 240 sh (31.1), 276 (25.5), 316 (37.1), 337
(33.3), 391 (20.9). Fluorescence spectrum (CH3CN,
λem 337 nm), λmax 423 nm. Fluorescence excitation
spectrum (CH3CN, λlum 420 nm), λmax, 311, 329 nm.
precipitation
of
[Pd(C^N)(μ-OOCCH3)]2
and
[Rh(C^N)2(μ-Cl)]2 dimer complexes. Adding ethylene-
diamine to the solution of [Pd(C^N)(μ-OOCCH3)] in
CH2Cl2 led to the substitution of acetate ligands with
chelating ethylenediamine and formation of [Pd(C^N)En]·
OOCCH3 precipitate in 40% yield. The substitution of
bridging chlorine ligands in the rhodium complex was
performed by adding ethylenediamine to [Rh(C^N)2·
(μ-Cl)]2 suspension in 2-methoxyethanol and pre-
cipitating [Rh(C^N)2En]Cl from the solution with
diethyl ether, yield 56%.
The 1H NMR, absorption, fluorescence and
fluorescence excitation spectra were obtained on JNM-
ECX400A, SF-2000 and Fluorat Panorama spec-
trometers at 293 K in (CD3)SO and CH3CN solu-
tions. The IR spectra of the complexes were taken on a
Shimadzu IR Prestige-21 spectrometer from KBr
pellets.
2-(4-Biphenyl-3-ido)-5-phenylbenzoxazole(ethylene-
1
diamine)palladium(II) acetate. Н NMR spectrum
[(CD3)2SO], δ, ppm (J, Hz): 8.19 s (Н8), 7.84 d (Н5,
3JHH 8.4), 7.77 m (4Нo,o'), 7.67 d (H6', 3JHH 8.2), 7.54 m
(5Н6,m,m'), 7.42 m (2Нp,p'), 7.23 s (H3'), 5.66 s (2Нα),
4.91 s (2Нδ), 2.80 m (4Нβ,γ), 1.18 s (CН3). IR spectrum
(KBr), ν, cm–1: 3370, 3289 (NH2), 1607 (C=N), 1586
(C2H4), 1577, 1449 (СОО), 858, 830 (C6H3, biphenyl
REFERENCES
1. Krasovitskii, B.M. and Bolotov, B.M., Organicheskie
lyuminofory (Organic Luminophors), Moscow: Khimiya,
1984.
2. Brooks, J., Babayan, Y., Lamansky, S., and Thom-
pson, M.E., Inorg. Chem., 2002, vol. 41, no. 12,
p. 3055.
3. Lamansky, S., Djurovich, P., Murphy, D., Abdel-
Razzaq, F., Lee, H.E., Adachi, C., Burrows, P.E.,
Forrest, S.R., and Thomson, M.E., J. Am. Chem. Soc.,
2001, vol. 123, no. 18, p. 4304.
4. Nakanisi, K., Infrared Spectra and Structure of Organic
Compounds, Moscow: Mir, 1965.
metalated ring). Absorption spectrum (CH3СN), λmax
,
nm (ε×10–3, mol–1 cm–1): 230 (15.3), 262.8 (11.9), 302
sh (6.9), 315 sh (8.9), 329 (10.4), 369 (12.4). Fluore-
scence spectrum (CH3CN, λem 337 nm), λmax 419,
432 nm. Fluorescence excitation spectrum (CH3CN,
λlum 420 nm), λmax 312, 326, 338, 343 nm.
Bis[2-(4-biphenyl-3-ido)-5-phenylbenzoxazol]-
1
(ethylenediamine)rhodium(III) chloride. Н NMR
5. Nakamoto, K., Infrared and Raman Spectra of
Inorganic and Coordination Compounds, Moscow: Mir,
1992.
spectrum [(CD3)2SO], δ, ppm (J, Hz): 8.29 d (2H8,
3JHH 1.4), 8.17 d (2Н5, 3JHH 8.3), 7.90 d (2Но, 3JHH 8.0),
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 81 No. 11 2011