SYNTHESIS AND MOLECULAR STRUCTURE OF PLATINUM(II) COMPLEXES
1879
(973.6). Calculated, %: C 44.39; H 3.28; N 7.19; Pt
20.04.
N 5.67. C36H31Cl2N4O6P3Pt (974.56). Calculated, %:
C 44.37; H 3.21; N 5.75.
Dichloro[pentaphenoxy(3-pyridylmethylamino)-
cyclotriphosphazene]platinum, [PtL2Cl2]. A pre-
heated solution of 0.743 g of pentaphenoxy(3-pyri-
dylmethylamino)cyclotriphosphazene in 15 ml of
acetonitrile was added to a solution of 0.360 g of
[Pt(MeCN)2Cl2] in 10 ml of acetonitrile. The mixture
was heated for 4 h, after which it was evaporated and
the resulting oil was recrystallized from acetone
toluene, 1 : 1. Yield 56 mg (17%). Found, %: C 44.01;
H 3.45; N 7.64. C36H32Cl2N5O5P3Pt. Calculated, %:
C 44.39; H 3.28; N 7.19.
ACKNOWLEDGMENTS
The study was financially supported by the Depart-
mental Target Program Development of the Scientif-
ic Potential of Higher School (grant RNP.2.1.1.1277).
REFERENCES
1. Diefenbach, U., Phosphazenes: A Worldwide Insight,
Gleria, M. and DeJaeger, R., Eds., New York: Nova
Science, 2004, p. 853.
2. Allcock, H.R., Allen, R.W., and O’Brien, J.P., J. Am.
Chem. Soc., 1977, vol. 99, no. 12, p. 3984.
Dichloro{pentaphenoxy[2-(2-pyridyl)ethylami-
no]cyclotriphosphazene}platinum, [PtL3Cl2]. An
0.300-g portion of [Pt(MeCN)2Cl2] was dissolved
with slight heating ( 30 C) in 10 ml of acetonitrile,
and a solution of 0.762 g of pentaphenoxy[2-(2-py-
ridyl)ethyl- amino]cyclotriphosphazene in 20 ml of
acetonitrile, heated to 40 C, was added dropwise. The
mixture was heated for approximately 0.5 h at 60 C;
in so doing, the color of the reaction mixture changed
from pale yellow to bright yellow. After that, the
solvent was evaporated to a minimal volume. The
mixture was separated on a column packed with silica
gel L 40/100 m (Chemapol), eluent acetone chloro-
form, 1 : 5. The crystals were grown from the middle
fraction, Rf 0.8, acetone chloroform, 1 : 5. Yield
194 mg (22.8%), mp 145 C. Mass spectrum [M
987.1]; m/z: 988 [M + H], 951 [M HCl], 915 [M
2 HCl], 722, 600, 307, 217, 154, 136, 107, 89, 77.
Found, %: C 45.15; H 3.50; N 6.94; Pt 19.60. C37H34
Cl2N5O5P3Pt (973.6). Calculated, %: C 45.00; H 3.47;
N 7.09; Pt 19.75.
3. Allen, R.W., O’Brien, J.P., and Allcock, H.R., J. Am.
Chem. Soc., 1977, vol. 99, no. 12, p. 3987.
4. Diefenbach, U., Kretschmann, M., and Stromburg, B.,
Chem. Ber., 1996, vol. 129, no. 12, p. 1573.
5. Justin Thomas, K.R., Chandrasekhar, V., Zanello, P.,
and Laschi, F., Polyhedron, 1997, vol. 16, no. 7,
p. 1003.
6. Chandrasekhar, V. and Nagendran, S., Chem. Soc.
Rev., 2001, vol. 30, no. 3, p. 193.
7. Diefenbach, U., Multifunktionelle Cyclo- und Poly-
phosphazene.
Synthese,
Koordinationschemie,
Eigenschaften, Berlin: Wissenschaft und Technik,
1999, 1st ed.
8. Bloy, M., Kretschmann, M., Scholz, S., Teichert, M.,
and Diefenbach, U., Z. Anorg. Allg. Chem., 2000,
vol. 626, no. 9, p. 1946.
9. Diefenbach, U., Kretschmann, M., and Cavdarci, O.,
Monatsh. Chem., 1996, vol. 127, no. 10, p. 989.
10. Diefenbach, U., Adamaszek, P., and Bloy, M.,
Heteroatom Chem., 1999, no. 10, p. 9; Chem. Ber.,
1996, vol. 129, no. 12, p. 1573.
Dichloro[pentaphenoxy(2-pyridylmethoxy)cyclo-
triphosphazene]platinum, [PtL4Cl2]. Weighed por-
tions of [Pt(EtCN)2Cl4] (0.1 g) and pentaphenoxy(2-
pyridylmethoxy)cyclotriphosphazene (L4, 0.189 g)
were mixed in a chloroform solution (3 ml). The re-
sulting mixture was thoroughly stirred until the com-
ponents dissolved completely, after which it was
heated at 50 C for 1.5 h. Then the solvent was re-
moved, and the oily residue was crystallized from di-
chloromethane acetone chloroform toluene CCl4,
1 : 1 : 1 : 1 :1. Rf 0.75, acetone chloroform, 1 : 3.
11. Simanova, S.A., Kuznetsova, T.V., Diefenbach, U.,
and Demidov, V.N., Zh. Obshch. Khim., 2006, vol. 76,
no. 4, p. 565.
12. Simanova, S.A., Kuznetsova, T.V., Diefenbach, U.,
and Demidov, V.N., Abstracts of Papers, XXI Mezh-
dunarodnaya konferentsiya po koordinatsionnoi
khimii (XXI Int. Conf. on Coordination Chemistry),
Kiev, 2003, p. 363.
13. Herbis, R.H., Croft, M., Coyer, M.J., Bilash, B., and
Sahiner, A., Inorg. Chem., 1994, vol. 33, no. 11,
p. 2422.
Yield 48 mg (18.5%), mp 161 C. Mass spectrum
(EI/70 eV) [M 974.6]; m/z: 1969 [2M 2H + Na, 9%],
1911 [2M HCl, 27%], 1875 [2M 2HCl, 4%], 1801
[2M 4HCl, 2%], 1459 [2M 4 HCl L4, 15%],
1097 [2M 4HCl 2L4, 4%], 996 [M H + Na,
21%], 974 [M, 8%], 938 [M HCl, 39%], 902 [M
2HCl, 100%], 808 [25%]. Found, %: C 44.28; H 3.23;
14. Sintez kompleksnykh soedinenii metallov platinovoi
gruppy (Synthesis of Coordination Compounds of
Platinum Group Metals), Chernyaev, I.I., Ed.,
Moscow: Nauka, 1964.
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 77 No. 11 2007