Acyclic Diaminocarbene Platinum(IV) Complexes Synthesized by the Oxidative Addition of MeI and I2

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The oxidative addition of methyl iodide or molecular iodine to the bis(С,N-chelate) deprotonated diaminocarbene platinum(II) complexes [Pt{C(N(H)Ar)(NC(N(H)Ph)N(Ph)}2] (Ar = C6H3-2,6-Me2 (Xyl), C6H2-2,4,6-Me3 (Mes), and C6H4-4-Me (pTol)) affords the corresponding platinum(IV) derivatives in a yield of 89–99%. The addition of CF3CO2H is accompanied by the protonation of the nitrogen atoms of the diaminocarbene fragment to form the cationic complexes [[PtI(X)-{C(N(H)Ar)(NC(N(H)Ph)N(Ph)}2]CF3CO2H (X = Me, I). The structures of the compounds are determined by elemental analysis; high resolution mass spectrometry with electrospray ionization (ESI HRMS); IR spectroscopy; 1H, 13C{1H}, 19F{1H}, and 195Pt{1H} NMR spectroscopy; 2D NMR spectroscopy (1H,1Н COSY, 1H,1Н NOESY, 1H,13C HSQC, 1H,13C HMBC, 1H,15N HSQC, 1H,15N HMBC), and X-ray diffraction

(XRD) and thermogravimetric analyses. The synthesized platinum(IV) complexes are thermally stable to 200–260°C and are electroneutral molecules with the octahedral coordination sphere formed by two deprotonated diaminocarbene C,N-chelate substituents and iodine and methyl or two iodine atoms localized in the apical positions.

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作者简介

A. Karchevsky

Saint Petersburg State University

Email: s.katkova@spbu.ru
俄罗斯联邦, Saint Petersburg

M. Kinzhalov

Saint Petersburg State University

Email: s.katkova@spbu.ru
俄罗斯联邦, Saint Petersburg

S. Katkova

Saint Petersburg State University

编辑信件的主要联系方式.
Email: s.katkova@spbu.ru
俄罗斯联邦, Saint Petersburg

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2. Scheme 1

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3. Fig. 1. Fragment of the 1H,13C-HMBC IIa ∙ CF3CO2H NMR spectrum

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4. Fig. 2. Molecular structures of IIa ∙ (CH3)2CO (a) and IIIa ∙ CH2Cl2 (b) in thermal ellipsoids of 50% probability. The solvent molecules are hidden

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5. Fig. 3. Supramolecular structure of IIIv in thermal ellipsoids of 50% probability

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