F. G. Moers

Crystal structure of 3-methylrhodaninecopper(I) iodide

The crystal structure of the copper(I) complex has been determined by a three-dimensional X-ray analysis. The monoclinic unit cell, space groupP21/c,a = 4·195(1),b = 15·581(2),c = 13·885(2) Å and β = 114·9(1) °, contains four formula-units. Intensities were collected on an automatic diffractometer. The structural parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·07 for 1809 non-zero observed reflexions.In this complex, the copper atom is in tetrahedral coordination with three iodine atoms and the sulphur atom of the thiocarbonyl group of the ligand. The iodine atom is coordinated with three copper atoms. The distances are 2·683(2), 2·627(2) and 2·665(2) Å. The distances between neighbouring copper atoms are 3·008(3) and 2·960(3) Å and the corresponding angles are 68·44(6) and 68·02(6) °, suggesting weak copper-copper interactions in this complex.

Hydrogen-deuterium exchange in tricyclohexylphosphine complexes

SummaryThe reactions of D2 with OsHCl(CO)(PCy3)2 and the deuteriation reaction with C2H5OD have been studied. The deuteriation ratios in the PCy3 ligand have been calculated. The reaction mechanism for the deuteriation in C2H5OD is discussed.

Crystal and Molecular Structure of (3ar,8bs,5'r)3-[(2,5-Dihydro-3-Methyl-2-Oxo-5-Furanyl)Oxymethylene]-3,3a, 4,8b-Tetrahydroindeno[1,2-B]Furan-2-One

The stereogeometry and absolute configuration of the title compound has been proved by an X-ray diffraction analysis. Crystal data: monoclinic, C2,a=20.2528(4),b=6.7254(2),c=10.6748(2) A, β=94.699(3),Z=4. The crystal structure has been solved by vector search methods and refined toR1=0.053 for 2043 observed reflections.

Menthol mediated optical resolution of 10-oxatricyclodecadienones. Application in the enantioselective synthesis of cyclopentenoids

Abstract The efficient conversion of 5-ethoxy-4-p-tolylsulphonylmhetyl-exo-10-oxatricyclo[5.2.1.02,6]deca-4,8-dien-3-one 6 into a diastereomeric mixture of the (-)menthyl ethers, 9a and 9b, is described. Separation of these ethers, followed by reduction with DIBAL and trans-etherification with NaOMe affords the enantio-merically pure methoxymethyl substituted 10-oxatricyclodecadienones (+)14 and (-)14. These tricyclodeca-dienones are enantiospecifically converted into the cyclopentadienone epoxides (-)16 and (+)16, respectively, by successive alkaline epoxidation and Flash Vacuum Thermolysis. The absolute configurations of all compounds, from 9a, 9b up to (-)16, (+)16 were established by means of X-Ray diffraction analyses.

Crystal structure of bis-(rhodanine)copper(I) iodide, C6H6CuIN2O2S4

The structure of the polymeric rhodanine compound Cul(HN-CO-CH/sub 2/-S-CS)/sub 2/, C/sub 6/H/sub 6/CuIN/sub 2/O/sub 2/S/sub 4/, was determined by X-rays. M /SUB r/ = 456.8, monoclinic, space group P2/sub 1//c, a = 4.1947(7), b = 17.6999(12), C = 17.1048(8) A, ..beta.. = 96.15(1)/sup 0/, V /SUB c/ = 1262.6 A/sup 3/, Z = 4, D /SUB c/ = 2.40Mg m/sup -3/, Cu K..cap alpha.. radiation (graphite crystal monochromator, lambda = 1.54056 A), ..mu..(Cu K..cap alpha..) = 278.9 cm/sup -1/, F(000) = 872, T = 290 K. Final conventional R - factor = 0.029, and R /SUB w/ = 0.044 for 2384 unique reflections and 153 variables. The structure was solved using Patterson methods and DIRDIF, and refined by full-matrix least-squares methods. The compound forms zigzag chains (..-Cu-I-Cu-..) along a. The copper atom is in trigonal pyramidal coordination, with two sulfur atoms of the thiocarbonyl group and two bridging iodine atoms. The copper-sulfur distances are 2.278(1) and 2.299(1) A, and the copper-iodine distances are 2.657(1) and 2.814(1) A.The structure of the polymeric rhodanine compound, C6H6CuIN2O2S4, was determined by X-rays.Mr=456.8, monoclinic, space groupP21/c,a=4.1947(7),b=17.6999(12),c=17.1048(8) Å,β=96.15(1)°,Vc=1262.6 Å3,Z=4,Dc=2.40Mg m−3, CuKα radiation (graphite crystal monochromator, λ=1.54056 Å),μ(CuKα)=278.9 cms-1,F(000)=872,T=290 K. Final conventionalR-factor=0.029, andRw=0.044 for 2384 unique reflections and 153 variables. The structure was solved using Patterson methods andDirdif, and refined by full-matrix least-squares methods. The compound forms zigzag chains alonga. The copper atom is in trigonal pyramidal coordination, with two sulfur atoms of the thiocarbonyl group and two bridging iodine atoms. The copper-sulfur distances are 2.278(1) and 2.299(1) Å, and the copper-iodine distances are 2.657(1) and 2.814(1) Å.

Crystal and molecular structure of 1-vinyl-3-methyl-imidazolium iodide, C6H9N2I

The title compound crystallizes with two independent molecules in the unit cell. The two molecules arecis-trans isomers. Crystal data: orthorhombic, P212121,a=7.0417(6),b=9.5341(9),c=25.411(2) Å,Z=8. The crystal structure has been solved by automated Patterson methods and refined toR=0.024 for 1843 observed reflections.

Crystal structure of di-μchlorobis{[bis(3-methylrhodanine)]copper(I)}-3-methylrhodanine

The crystal structure of has been determined by X-ray analysis. The monoclinic cell, space groupC2/c witha=12.956(2),b=15.873(2),c=17.437(2) Å,β=105.90(1)° contains eight formula units. The structure was determined using MoKα. automatic diffractometer X-ray data and refined by full-matrix least squares toR=0.039 for 3025 reflections. Two crystallographically independent 3-memylrhodanines are coordinated to copper, and another 3-methylrhodanine is not bonded to copper and is in a disordered position around the crystallographic two-fold axis. In the dimeric structure with bridging chlorine atoms, the copper is in tetrahedral coordination with two chlorine and two sulfur atoms. The copper-copper distance is 2.906(1) Å.

Crystal structure of 2-{(R)-1-hydroxy-1-[(2S)-1-tritylaziridin-2-yl] methyl}acrylate and spectroscopic properties of the (R,S) and (S,S) stereoisomers

The crystal and molecular structure of 2-{(R)-1-Hydroxy-1-[(2S)-1-tritylaziridin-2-y1] methy1}acrylate is described. Crystal data: C26H25NO3, orthorhombic, space group P212121, a = 9.6954(5), b = 13.1458(5), c = 16.7885(7) Å, V = 2139.8(2) Å3, Z = 4. The (R,S) diastereomer shows an intramolecular hydrogen bonding N···H—O under formation of a five-membered ring with N···O distance of 2.664 Å. IR, 1H NMR and 13C NMR data are discussed. The 1H NMR of the (R,S) diastereomer shows a singlet- whereas the (S,S) diastereomer exhibits a doublet-pattern for the hydroxyl proton.

endo-5-Methyl-exo-6-phenylseleno-endo-tricyclo[5.2.1.02,6]dec-8-en-3-one

Structural analysis of the title compound, C 17 H 18 OSe, confirms the endo configuration of the C5-methyl group.