Tensimetric study of [ClSb{Cr(CO) 5}2]2 and its reaction with pyridine

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Аннотация

Thermal stability of [ClSb{Cr(CO)5}2]2 and its reaction with pyridine was studied by static tensimetry method with membrane null-manometer. [ClSb{Cr(CO)5}2]2 is thermally unstable and decomposes at 50–80°C with the formation of carbon monooxide and chromium hexacarbonyl. Upon reaction with pyridine on heating instead of the expected ClSb{Cr(CO)5}2∙Py formation of СO, Cr(CO)6, Cr(CO)5∙Py, antimony and supposedly complex of chromium dichloride with pyridine are formed.

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Авторлар туралы

A. Schevchenko

St. Petersburg State University

Email: a.y.timoshkin@spbu.ru
Ресей, St. Petersburg, 199034

I. Kazakov

St. Petersburg State University

Email: a.y.timoshkin@spbu.ru
ORCID iD: 0000-0003-1078-960X
Ресей, St. Petersburg, 199034

L. Rummel

Universität Regensburg

Email: a.y.timoshkin@spbu.ru

Institut für Anorganische Chemie

Германия, Regensburg, 93053

M. Seidl

Universität Regensburg

Email: a.y.timoshkin@spbu.ru

Institut für Anorganische Chemie

Германия, Regensburg, 93053

A. Timoshkin

St. Petersburg State University

Хат алмасуға жауапты Автор.
Email: a.y.timoshkin@spbu.ru
ORCID iD: 0000-0002-1932-6647
Ресей, St. Petersburg, 199034

Әдебиет тізімі

  1. Weber U., Zsolnai L., Huttner G. // J. Organomet. Chem. 1984. Vol. 260. P. 281. doi: 10.1016/S0022-328X(00)99477-4
  2. Sigwarth B., Weber U., Zsolnai L., Huttner G. // Chem. Ber. 1985. Vol. 118. N 8. P. 3114. doi: 10.1002/cber.19851180810
  3. Rummel L., Seidl M., Timoshkin A.Y., Scheer M. // Z. anorg. allg. Chem. 2022. Vol. 648. P. e202200014. doi: 10.1002/zaac.202200014
  4. Дойников Д.А., Казаков И.В., Краснова И.С., Тимошкин А.Ю. // ЖФХ. 2017. Т. 91. С. 1429; Doinikov D.A., Kazakov I.V., Krasnova I.S., Timoshkin A.Y. // Russ. J. Phys. Chem. (A). 2017. Vol. 91. P. 1603. doi: 10.1134/S0036024417080088
  5. Давыдова Е.И., Дойников Д.А., Казаков И.В., Краснова И.С., Севастьянова Т.Н., Суворов А.В., Тимошкин А.Ю. // ЖОХ. 2019. Т. 89. N 6. С. 843; Davydova E.I., Doinikov D.A., Kazakov I.V., Krasnova I.S., Sevast’yanova T.N., Suvorov A.V., Timoshkin A.Yu. // Russ. J. Gen. Chem. 2019. Vol. 89. N 6. P. 1069. doi: 10.1134/S1070363219060021
  6. Linstrom P.J., Mallard W.G. // NIST Chemistry WebBook, NIST Standard Reference Database Number 69, National Institute of Standards and Technology, Gaithersburg MD, 20899, March 24, 2025. doi: 10.18434/T4D303
  7. Meulen P.V.D., Mann R.F. // J. Am. Chem. Soc. 1931. Vol. 53. N 2. P. 451. doi: 10.1021/ja01353a006
  8. Stull D.R. // Ind. Eng. Chem. 1947. Vol. 39. N 4. P. 517. doi: 10.1021/ie50448a022
  9. Ries W., Bernal I., Quast M., Albright T.A. // Inorg. Chim. Acta. 1984. Vol. 83. P. 5. doi: 10.1016/S0020-1693(00)82357-9
  10. Lux H., Eberle L., Sarre D. // Chem. Ber. 1964. Vol. 97. P. 503. doi: 10.1002/cber.19640970228
  11. Holah D.G., Fackler J.P. // Inorg. Chem. 1965. Vol. 4. N 8. P. 1112. doi: 10.1021/ic50030a005
  12. Cotton F.A., Daniels L.M., Feng X., Maloney D.J., Murillo C.A., Zúñiga L.A. // Inorg. Chim. Acta. 1995. Vol. 235. P. 21. doi: 10.1016/0020-1693(95)90041-4
  13. Weber U., Huttner G., Scheidsteger O., Zsolnai L. // J. Organomet. Chem. 1985. Vol. 289. P. 357. doi: 10.1016/0022-328X(85)87412-X

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2. Fig. 1. Dependence of the signal intensity in the mass spectrum on the temperature in the vapor above [ClSb{Cr(CO)5}2]2. 1 – Cr(CO)6+, 2 – ClSb{Cr(CO)5}2+ (the intensity of signal 2 is increased by 100 times).

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3. Fig. 2. Dependence of the vapor pressure over [ClSb{Cr(CO)5}2]2 on temperature during heating-thermostat series at 50°C (1), 70°C (2), 80°C (3).

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4. Fig. 3. Dependence of the amount of substance in the gas phase over [ClSb{Cr(CO)5}2]2 on time during thermostatting at 50 (1), 70 (2) and 80°C (3).

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5. Fig. 4. IR spectra of crystals from the membrane chamber (1) and Cr(CO)6 (Sigma-Aldrich, 99.9%) (2).

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6. Fig. 5. Calculation of the number of components in steam. 1 – measured Pо/T, 2 – P[Cr(CO)6]/T based on the difference between Pо/T and PCO/T, 3 – saturated steam pressure P[Cr(CO)6]/T based on data from [6].

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7. Fig. 6. Dependence of the vapor pressure in the [ClSb{Cr(CO)5}2]2–Py system on the temperature during defrosting from the temperature of liquid nitrogen in a series of sequential experiments. 1–3 – measured total pressure Pо in the first, fourth and seventh series; 4 – difference Pо(3) – PCO, 5 – saturated vapor pressure of dioxane according to data from [8].

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