J. A. Cras

Crystal and molecular structure of 3,5-bis(N,N-diethylimonium)-1,2,4-trithiolane-tetraiododi-μ-iododiinercurate(II)

The crystal and molecular structure of 3,5-bis(N,N-diethylimonium)-1,2,4-trithiolane-tetraiododi-μ-iododimercurate(II), (S3C2N2(C2H5)4)Hg2I6, has been determined from a single-crystal X-ray diffraction study. The monoclinic unit cell, space groupP21/c, witha = 12·574(3),b = 15·777(4),c = 14·560(4) Å, and β = 90·83(4) °, contains four formula-units. Three-dimensional intensity data were collected on an automatic diffractometer. Atomic parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·05 for 1380 independent non-zero reflexions. The structure consists of (3,5-bis(N,N-diethyl-imonium)-1,2,4-trithiolane)2+ and Hg2I62− ions. The cation contains a five-membered ring, S-S-C-S-C, which can be formed by oxidation of dithiocarbamato and thiuramdisulfide complexes.

Crystal and molecular structure of diiodo-N,N,N′,N′-tetramethylthiuramdisulphidemercury(II)

The crystal and molecular structure of diiodo-N,N,N′,N′-tetramethylthiuramdisulphidemercury(II), HgI2(S2CN(CH3)2)2, has been determined by a three-dimensional X-ray analysis. The compound crystallizes in the monoclinic space groupP21/c with the unit cell dimensionsa = 7·957 ± 4,b = 22·639 ± 7,c = 9·956 ± 6 Å and β = 112·14 ± 5 °;Z = 4. Intensities were obtained with an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·044 for 1294 non-zero observed reflexions. The mercury is in distorted tetrahedral coordination with two iodine and two sulphur atoms. The Hg-I distances are 2.654 ± 2 and 2·661 ± 2 Å; the Hg-S distances are 2·651 ± 7 and 2·882 ± 7 Å. The thiuramdisulphide ligand consists of two planar units S2CNC2, nearly perpendicular to each other. Bond distances of the ligand are compared with distances in tetraalkylthiuram disulphide molecules and agree with infrared observations.

Crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)gold(III) dibromoargentate(I)

The crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)gold(III)dibromoargentate(I), Au(S2CN(C4H9)2)2AgBr2, has been determined by three-dimensional X-ray methods. The compound crystallizes in the monoclinic space groupC2/c with unit cell dimensions:a= 17·39(1)b = 18·65(1);c = 9·199(6) Å; β = 93·9(1)°;Z=4. Intensities were collected on an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·048 for 854 non-zero observed reflexions. The structure consists of Au(S2CN(C4H9)2)2+ and AgBr2− ions. The gold is in planar coordination with four sulphur atoms, the two crystallographically non-equivalent Au-S bond lengths being 2·357(8) and 2·324(8) Å. The silver is linearly coordinated, the Ag-Br bond lengths being 2·450(5) Å. The ionic packing in the structure differs from that in the analogous Au(S2CN(C4H9)2)2AuBr2 complex.

Crystal and molecular structure of bis(N,N-diethyldithiocarbamato)palladium(II)

The crystal and molecular structure of bis(N,N-diethyldithiocarbamato)palladium(II), Pd(S2CN(C2H5)2)2, has been determined by a three-dimensional X-ray analysis. The compound crystallizes in the tetragonal space groupP42/n with unit cell dimensionsa = 16·439(8) Å andc = 6·247(3) Å. The crystals are isomorphous with bis(N,N-diethyldithiocarbamato)platinum(II). Intensities were obtained with an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·038 for 600 non-zero observed reflections. The palladium is in planar coordination with four sulphur atoms, the two non-equivalent Pd-S bond lengths being 2·317(3) and 2·315(3) Å.

Structure analysis of twinned crystals of tris(N,N-di-n-butyldiselenocarbamato)nickel(IV) bromide

The crystal structure of tris(N,N-di-n-butyldiselenocarbamato)nickel(IV) bromide, Ni(Se2CN-(C4H9)2)3Br, has been determined by three-dimensional X-ray methods. The Laue symmetry is 6/mmm, but the structure could be solved only in space groupP¯31c. The crystals were, therefore, regarded as being microtwinned on (001). The unit cell dimensions area =b = 14·69(3) andc = 10·91(3) Å. From integrated Weissenberg photographs, 307 non-zero symmetry-independent reflexions were measured photometrically. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·10. The quadrivalent nickel atom is octahedrally coordinated by six selenium atoms. The Ni-Se distance is 2·391(5) Å; the Se-Se distance within one diselenocarbamate ligand is 3·00(1) Å; Se-Se distances between different ligands are 3·51(1), 3·52(1) and 3·55(1) Å.