MethylSulfate Complex (Bu4N)2[Мo6I8(O3SOCH3)6]: Synthesis, Structure, Lability of Ligands, and Phosphorescence

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New methylsulfate complex (Bu4N)2[Мо6I8(O3SOCH3)6] (I) is synthesized by the reaction of (Bu4N)2[Mo6I8(C≡C–C(O)OCH3)6] with dimethyl sulfate (CH3)2SO4. According to the XRD data, the molybdenum atoms are coordinated by the monodentate methylsulfate ligands. In a DMSO solution, the complex undergoes solvolysis accompanied by the complete substitution of the methylsulfate ligands by the solvent molecules. A powder sample of cluster I luminesces (phosphorescence) with the emission maximum at a wavelength of 620 nm (77 K). Increasing temperature to 300 K results in the shift of the emission maximum to 650 nm and a decrease in the integral intensity by 1.6 times.

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作者简介

M. Mikhaylov

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

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Email: mikhajlovmaks@yandex.ru
俄罗斯联邦, Novosibirsk

T. Sukhikh

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Email: mikhajlovmaks@yandex.ru
俄罗斯联邦, Novosibirsk

D. Sheven

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Email: mikhajlovmaks@yandex.ru
俄罗斯联邦, Novosibirsk

A. Berezin

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Email: mikhajlovmaks@yandex.ru
俄罗斯联邦, Novosibirsk

M. Sokolov

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences; Novosibirsk State University

Email: mikhajlovmaks@yandex.ru
俄罗斯联邦, Novosibirsk; Novosibirsk

N. Kompankov

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Email: mikhajlovmaks@yandex.ru
俄罗斯联邦, Novosibirsk

参考

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2. Fig. 1. Fragment of the crystal structure of cluster complex I, hydrogen atoms are not shown) (a); fragment of cluster anion I, the crystallographically equivalent atoms Mo, I, O are indicated in brackets, the upper index above the brackets denotes the corresponding centrally symmetric atom (b)

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3. Fig. 2. Found and calculated isotopic distributions in the negative m/z region corresponding to [Mo6I8(O3SOCH3)6]2- and {(Bu4N)[Mo6I8(O3SOCH3)6]}-

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4. Fig. 3. PMR spectra of I in DMSO-d6 at different temperatures. Chemical shifts of signals from protons of Bu4N+ cations and DMSO (2.5 m.d.) are marked by rectangles; the red oval inside the rectangle is from methyl protons of methanol molecules; the orange oval is from protons of free methyl sulfate anions; the red oval is from protons of coordinated methyl sulfate anions; the migrating (in the range 3. 31-3.74 m.d.) broadened signal marked with a red dot is attributed to protons of H2O

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5. Fig. 4. Temperature dependence of luminescence of powder sample I at excitation λex = 440 nm

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6. Fig. 5. Temperature dependence of the excitation spectrum of cluster complex I powder with luminescence maximum at λem = 620 nm

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7. Fig. 6. Temperature dependence of luminescence intensity I at excitation λex = 440 nm

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