Molecular and crystal structure of 2-para-toluimido-4,4-dimethyl-(4H)-1,3-thiazine

The imino structure of 2-p-toluimido-4,4-dimethyl-(4H)-1,3-thiazine (I) was demonstrated by x-ray diffraction structural analysis. Molecules of I in the crystal are linked by N-HO hydrogen bonds in infinite chains. A shortened SO intramolecular contact was found which corresponds to a secondary interaction. A mechanism was proposed for the thiazoline-thiazine rearrangement.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 12, pp. 1638–1643, December, 1984.     

Synthesis of 2-methyl-1,3-cyclopentanedione monoethylene ketal

Direct ketalization of 2-methyl-1,3-cyclopentanedione 3 led to the corresponding diethylene ketal 2. Carefully controlled hydrolysis of compound 2 afforded the monoethylene ketal 1 in high yield.     

Crystal structure of 2-Se-(2-methyl-2-propenyl)-1-benzoic acid.

C11H12O2Se is triclinic, P1. Unit-cell dimensions at 293 K are a = 5.8450(10), b = 8.1490(10), c = 11.4620(10)A, alpha = 97.050(10), beta = 90.140(10), gamma = 90.120(10) degrees, V = 541.81(12)A3, Dx = 1.564 g/cm3, and Z = 2. The R value is 0.047 for 1388 observed reflections. The dihedral angle between the phenyl ring and the isobutenyl group is 72.3(2) degrees. There is an intermolecular hydrogen bond between two symmetry-related carbonyl groups with an O1...O2 distance of 2.669(6)A. The molecules in the crystal are packed at normal van der Waals distances.     

Molecular and crystal structure of 3,7-di(2-propenyl)-1,5-diphenyl-3,7-diazabicyclo[3.3.1]-nonan-9-one complexed with copper(II) chloride

We have investigated the molecular and crystal structure of 3, 7-di(2-propenyl)-1, 5-diphenyl-3, 7-diazabicyclo[3.3.1]nonan-9-one complexed with copper(II) chloride. We have shown for the first time that the reason for the distortion of the coordination polyhedron of the metal is the interaction of the substituents at the nitrogen atoms with the halogen atoms.Communication 2 in the series Complexing properties of 3,7-diazabicyclo[3.3.1]nonanes.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 770–774, June, 1996. Original article submitted April 13, 1996.Deceased.     

Molecular and crystal structure of 2-(N-benzyl-N-phenylhydrazinoethylidene)-3-(2H)-benzo[b]-thiophenone

X-ray structural analysis was used to determine the molecular and crystal structure of 2-(N-benzyl-N-phenylhydrazinoethylidene)-3-(2H)-benzo[b]thiophenone. The crystals are monoclinic, the space group isC2/c,a=16.022(6),b=11.202(3),c=22.111(4) Å, =81.08(3)°, and andZ=8. It was shown that the ability of hydrazones of a similar class to exhibit photochromic properties is a function of the steric stresses in the molecules and their confirmation.Institute of Chemical Physics in Chernogolovka, Russian Academy of Sciences, 142432 Chernogolovka. Translated fromIzvestiya Akademii Nauk, Seriya Khimicheskaya, No. 12, pp. 2805–2809, December, 1992.     

硫氰酸铀铣(18-冠-6)铵(或钾)配合物的合成, 特性和结构

本文报导了硫氰酸铀铣(18-冠-6)铵和硫氰酸铀酰(18-冠-6)钾两种固体配合物的合成。由测定其物理常数及谱学数据, 确定了配合物的组成为[(C12H24O6)M]2UO2(NCS)4H2O(M=NH4, K)。X射线结构分析确定了二种单晶的结构。铵配合物属正交晶素, 空间群为Fdd2, 钾配合物属单斜晶系, 空间群为C2/c。     

Molecular structure of 1-methyl-1-fluoroquasisilatrane (2-methyl-2-fluoro-1,3-dioxa-6-aza-2-silacyclooctane)

The molecular structure of 1-methyl-1-fluoroquasisilatrane (2-methyl-2-fluoro-1,3-dioxa-6-aza-2-silacyclooctane) MeFSi(OCH₂CH₂)₂NH (I) is determined by single crystal X-ray diffraction at 100 K. The coordination polyhedron of the silicon atom in this molecule is a slightly distorted trigonal bipyramid with an NH group and a strongly electron-withdrawing fluorine atom in the axial positions, and two endocyclic oxygen atoms and a CH₃ group in three vertices of the equatorial plane. The axial angle N→SiF is 171°. The length of the transannular donor-acceptor bond N→Si (2.058 Å) is as small as in 1-fluorosilatrane. The axial bond F-Si (1.660 Å) is longer than that in 1-fluorosilatrane and tetrahedral silicon compounds.