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Vol 49, No 6 (2023)
Articles
New 5-n-C4H9-C2B9-Carborane Ligand and Its Ruthenium Complexes
Abstract
The reaction of 9-iodo-ortho-carborane with n-butylmagnesium bromide affords 9-n-butyl-ortho-carborane. The reaction of the latter with alkali in boiling ethanol gives new nido-carborane [5-Bu-7,8-C2B9H11]– (I) containing the n-butyl substituent at the lower rim of the basket. The reaction of compound I with RuCl2(PPh3)(Ph2P(CH2)4PPh2) results in the formation of the corresponding ruthenium(IV) closo complex 3,3-(Ph2P(CH2)4PPh2)-3-H-3-Cl-9-Bu-closo-3,1,2-RuC2B9H10 (II) characterized by 2D NMR spectroscopy. On heating compound II can react with carbon tetrachloride to form the 17-electron complex 3,3-(Ph2P(CH2)4PPh2)-3-Cl-9-Bu-closo-3,1,2-RuC2B9H10 (III). The structure of complex III is solved by X-ray diffraction (XRD) (CIF file CCDC no. 2180761). The electrochemical studies show that complex III undergoes the reversible transition Ru(II) → Ru(III) similarly to the earlier studied ruthenacarboranes.
323-332
Ligand Metathesis in Nickel(II) Complexation with closo-Decaborate Anion
Abstract
Nickel(II) complexation with the closo-decaborate anion in water and acetonitrile is studied. Complexes [Ni(solv)6][B10H10] (solv = H2O (I) or CH3CN (II)) are isolated. The complexes are characterized by elemental analysis and IR spectroscopy. Complex [Ni(CH3CN)5(H2O)]0.75[Ni(CH3CN)4(H2O)2]0.25[B10H10]·0.5H2O (III) is isolated from an acetonitrile–water system. The structure of complex III is solved by X-ray diffraction (XRD) (CIF file CCDС no. 2224702). A mechanism of ligand metathesis in the complexation of nickel(II) is proposed.
333-340
Bromoantimonates(III) vs. Bromobismuthates(III): Differences in the Tendency for the Formation of Polynuclear Complexes
Abstract
Pyridine-based Sb(III) bromide complexes with doubly charged cations, (PyC3)3[Sb2Br9]2 (I), (PyC4)[Sb2Br8] (II), (PyC5)2[α-Sb4Br16] (III), (PyC6)2[Sb2Br10] (IV), (4-MePyC2)2[Sb2Br10] (V), (4‑MePyC3)2[α-Sb4Br16] (VI), and (4-MePyC5)2[α-Sb4Br16] (VII), were synthesized and characterized by X-ray diffraction (CCDC nos. 2204718–2204724). The structures of these compounds were compared with the structures of related bromobismuthates(III).
341-346
Structure of Copper(II) N-Methylbenzoylhydroxamate in the Crystalline State and in Solution
Abstract
The geometrical structure of CuL2 (I), where L = R1N(O)–(O)CR2, R1 = Me, R2 = Ph, was studied by X-ray diffraction in the crystalline state and by stationary ESR spectroscopy in solution. In the crystalline state, I is a chain polynuclear complex. According to ESR data, in frozen solutions, complex I exists as three species, two being mononuclear and one being binuclear. The magnetic resonance parameters and concentrations of the species in frozen solutions were determined. The electronic structure of the complex with full geometry optimization of all systems was calculated in terms of the unrestricted density functional theory (DFT) method.
347-353
Adducts of Sterically Hindered Tellurium Catecholate with Ethers
Abstract
Adducts of tellurium(IV) 3,6-di-tert-butyl catecholate (Te(Cat36)2) with 1,2-dimethoxyethane (Dme), bis(2-methoxy)ethyl ether (diglyme), and crown ether 18-crown-6 (18c6) ([Te(Cat36)2(Dme)]2 (I), [Te(Cat36)2(diglyme)] (II), and [Te2(Cat36)4(18c6)] (III), respectively) are synthesized and characterized by X-ray diffraction (XRD) (CIF files CCDC nos. 2208717 (I), 2208718 (II), and 2208719 (III)). The complexes are also characterized by NMR (1H, 125Te) and IR spectroscopy.
354-359
Template Synthesis of the Trinuclear Cobalt(III) Complex with Diarylimidazole-Based Ligands: Synthesis and Properties
Abstract
The trinuclear cobalt(III) complex [(Bipy)5Co3(L)2](Cl)3 (I) is synthesized by the template reaction of 2,2'-(1H-imidazole-4,5-diyl)bis(4-ethylphenol) (L) and bis(2,2-bipyridine)cobalt(II) dichloride in the presence of diazabicycloundecene. The complex is isolated in the individual state and characterized by elemental analysis, cyclic voltammetry, UV-VIS spectroscopy, and X-ray diffraction (XRD) (CIF file СCDC no. 2201135). According to the obtained data, the cobalt ions in trinuclear complex I have the oxidation state +3, and the complex formation occurs with the oxidation of the initial cobalt(II) ions.
360-366
Lutetium Cyclopentadienyl Complex with the 2,6-Di-tert-Butylanthracene Dianion
Abstract
The reaction of 2,6-di(tert-butyl)anthracene with potassium graphite and monocyclopentadienyllutetium dichloride tetrahydrofuranate in THF gave the anthracenide complex [(η5-C5H5)Lu(η2-2,6-tBu2C14H8)(THF)2] (I), which was studied by X-ray diffraction (CCDC no. 2215512). Complex I crystallizes in the orthorhombic space group P212121. The structural rigidity of the Lu(O)2Cp(anthracene) crystallographic node was demonstrated. The retention of the structure of complex I in solution was confirmed by NMR techniques.
367-374
New Uranyl Succinate-Containing Polymers: Synthesis and Structure
Abstract
Two uranyl succinate polymers, NH4[UO2(Suc)(HSuc)]∙H2O (I) and [UO2(Suc)(H2O)2] (II), where Suc = succinate ion (C4H4O2−4
), were synthesized and studied by X-ray diffraction, IR spectroscopy, and thermography (CCDC nos. 2202634 and 2202635, respectively). The main structural units in the crystals of I are infinite zigzag chains [UO2(Suc)(HSuc)]–, corresponding to the AQ02B01 crystal chemical formula (A = UO2+2,
Q02 = C4H4O2−4,
B01 = C4H5O−4
). It was established that in structure II, the electrically neutral [UO2(Suc)(H2O)2] chains correspond to the AQ02M12
crystal chemical formula (A = UO2+2,
Q02 = C4H4O2−4,
M1 = H2O). The intermolecular interactions in structures I and II were analyzed using the method of molecular Voronoi–Dirichlet polyhedra.
375-382
К пятидесятилетию Константина Юрьевича Жижина
383-384