Vitaly K. Belsky

Crystal and molecular structures of bis(1,3-di-tert-butylcyclopentadienyl)cerium chloride and borohydride. First example of the bridging tetradentate BH4-group with two μ3-hydrogens: μ : η4-[(μ3-H)2B(μ2-H)2]

Abstract Interaction between CeCl 3 and two equivalents of (C 5 H 3 Bu t 2 ) Na leads to the complex [(η 5 -C 5 H 3 Bu t 2 ) 2 Ce(μ 2 -Cl)] 2 . ( I ). Crystals of 1 are rhombic, a = 13.032(3), b = 24.629(5), c = 17.044(3) A, space group Pbnb , Z = 4, d = 1.630 g cm −3 . Complex I reacts with one equivalent of LiBH 4 to afford {(η 5 -C 5 H 3 Bu t 2 ) 2 Ce[μ: η 4 -(η 3 -H) 2 B(μ 2 -H) 2 ]} 2 ( II ) which is isostructural to I. Two BH 4 groups in complex II are tetradentate and contain two μ 3 - and two μ 2 -bridging hydrogens. Cerium has a 20e environment.

Template synthesis, structure and unusual series of phase transitions in clathrochelate iron(II) α-dioximates and oximehydrazonates formed by capping with functionalized boron-containing agents

Abstract A series of clathrochelate α-dioximates and oximehydrazonates with apical long-chain paraffin and allyl substituents has been synthesized and characterized by X-ray analysis. For the hexadecylboronic FeNx3(BHd)2 complex (where Nx2− is the cyclohexanedion-1,2-dioxime dianion) in the temperature range 100–305 K, two structural phase transitions have been detected by X-ray diffractometry and 57Fe Mossbauer spectroscopy.

Structure analysis of triaryl derivatives of the group V elements. crystal and molecular structure of tri-p-tolylantimony, C21H21Sb

Abstract An X-ray structure analysis of tri-p-tolylantimony has been made. Crystals are rhombohedral, a 9.988 A, α 79.77°, Z = 2, space group R 3 . Final value of R is 0.024 after full-matrix least squares refinement. The valence angle CSbC, 97.3°, is in good accordance with values for triaryl derivatives of other Group V elements

THE SYNTHESIS AND STRUCTURE OF A MACROBICYCLIC HEXAHALOGENIDE TRISDIOXIMATE AS A PROMISING PRECURSOR OF FUNCTIONALIZED CLATHROCHELATES

The reactive hexachloride precursor of functionalized α-dioximate clathrochelates and the product of their reaction with thiophenol have been prepared and structurally characterized by single-crystal X-ray diffraction.

Bis(acetato‐O)bis(pyridine‐N)palladium(II) Monohydrate and Bis(acetato‐O)bis(diethylamine‐N)palladium(II)

The title complexes, [Pd(C 2 H 3 O 2 ) 2 (C 5 H 5 N) 2 ].H 2 O, (I), and [Pd(C 2 H 3 O 2 ) 2 (C 4 H 11 N) 2 ], (II), are typical of metal acetates with additional N-donor coordination. In both structures, the central Pd atom has a centrosymmetric square-planar environment. In the pyridine complex (I), carbonyl O atoms are involved in intermolecular O-H...O hydrogen bonds with water molecules and in the amine complex (II), they participate in intramolecular N-H...O hydrogen bonds. Owing to the latter, the Pd-N bond lengths are different with values of 2.010 (4) for complex (I) and 2.066 (2) A for complex (II).

Structure and reactivity of [PtX2 (ketoxime) 2] compounds. Cis-trans isomerization and X-ray structures of cis- [PtBr2 (Me2C=NOH) 2] and trans- [PtBr2 (Me2C=NOH) 2] · 2MeC (=O) NMe2

Abstract The solid state thermal isomerization of cis- [PtX2 (ketoxime) 2] (X = Cl, ketoxime = Me2C=NOH, (CH2) 4C = NOH, (CH2) 5C=NOH ; X = Br, ketoxime = Me2C=NOH) gives the corresponding trans-isomers in almost quantitative yields, thus showing that solid state isomerization is a general and convenient procedure for the synthesis of trans- [PtX2 (ketoxime) 2] complexes. X-ray structure analyses were performed for both cis- [PtBr2 (Me2C=NOH) 2] and the bis-dimethylacetamide solvate of trans- [PtBr2 (Me2C=NOH) 2] . The former compound crystallizes in the orthorhombic space group Pbca with a = 9.593 (1) , b = 14.827 (2) , c = 17.218 (2) A ; V = 2449.0 (8) A3, Z = 8, and ρcalcd = 2.718 cm−3. The latter complex crystallizes in the orthorhombic space group Pbca with a = 10.543 (2) , b = 17.676 (4) , c = 12.398 (2) A ; V = 2310.5 (8) A3, Z = 4, and ρcalcd = 1.941 g cm−3. These two compounds are the first structurally characterized representatives of neutral Pt complexes with ‘‘simple’’ oximes.

SYNTHESIS AND STRUCTURE OF SOME STABLE PHOSPHOLANE-PHOSPHOLANES

Abstract Bicyclophosphites based on linear 1,2,3-triols with terminal substituents were found to be stable. Thus a series of hitherto unknown phospholane-phospholane esters, including optically active ones, was synthesized and their promise for synthetic use was demonstrated. The structure of the new compounds was proved by 1H, 13C and 31P NMR spectroscopy and, for one of them, by X-ray analysis.

STRUCTURAL INVESTIGATION ON 1-AMINO-ARYL-METHYLPHOSPHONATE ESTERS. X-RAY STRUCTURE OF O,O-DIETHYL-N-N′-ETHYLENE-BIS-PHENYLMETHYLPHOSPHONATE

Abstract The crystal and molecular structure of the title compound has been determined by single crystal x-ray analysis. C24H38N2O6P2 has a meso configuration, its crystal is triclinic, space group P1, with a = 11.795(2), b = 8.616(2), c = 7.694(2), α = 112.72(2), β = 94.42(2), γ = 104.91(2), and Z = 1. The refinement had a R-value of 0.036 for 1580 reflections.

Structure analysis of triaryl derivatives of the group V elements III. Molecular Structure and Spectra of Tris(2,6-Dimethylphenyl)Stibine, C24H27Sb

X-Ray structure analysis, dipole moment measurement and electronic spectra investigation have been carried out on tris(2,6-dimethylphenyl)stibine. Crystals are monoclinic, a 15.873 A, b 16.204 A, c 8.246 A, γ 103.29°, Z = 4, space group P 2 1 / b . The mean value of valence angle CSbC is 104.7°; that of the SbC bonds 2.190 A. The molecular conformation is governed by steric effects due to the methyl groups. The dipole moment is 0.62 D.

THE SYNTHESIS AND STRUCTURE OF THE FIRST REPRESENTATIVES OF OLIGOARYLENEPHOSPHOCYCLANES

Abstract Based on phenylphosphonous acid tetraethyldiamide and 2,2-di(p-oxyphenyl)propane diarylenecyclo-phenylphosphonite is synthesized. Its oxidation and sulfurization is investigated. It is shown that these reactions are stereospecific and lead to cis-isomers. The compounds obtained are the first representatives of oligoarylenephosphocyclanes. The structure of these compounds is confirmed by an X-ray structure analysis.