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

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Abstract

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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About the authors

A. V. Schevchenko

St. Petersburg State University

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

I. V. Kazakov

St. Petersburg State University

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

L. Rummel

Universität Regensburg

Email: a.y.timoshkin@spbu.ru

Institut für Anorganische Chemie

Germany, Regensburg, 93053

M. Seidl

Universität Regensburg

Email: a.y.timoshkin@spbu.ru

Institut für Anorganische Chemie

Germany, Regensburg, 93053

A. Y. Timoshkin

St. Petersburg State University

Author for correspondence.
Email: a.y.timoshkin@spbu.ru
ORCID iD: 0000-0002-1932-6647
Russian Federation, St. Petersburg, 199034

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Supplementary files

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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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