J. H. Noordik

Reactions of gold–phosphine cluster compounds. Preparation and X-ray structure determination of octakis(triphenylphosphine)octa-gold bis(hexafluorophosphate)

[Au9L8]3+(L = PPh3) reacts with L to form [Au8L8]2+ and [AuL2]+; preliminary X-ray structural results are reported for [Au8L8][PF6]2.2CH2Cl2(1).

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.

Paramagnetic alkali-aromatic ion-pair structures. The crystal structure of bis[1,2-bis(2-methoxyethoxy)ethane]sodium biphenylide

[Na(CsH 1804)2 ] C 12Hi0, (C 16H36NaOs)+C 12Hi0, M r = 533.7, monoclinic, P21, a = 11.721(2), b = 13.425 (2), c = 9.555 (2) A, fl = 103.08 (4) ° 12(Mo Ka) = 0.71069/~1, V= 1464.5/~3, Dx (150 K) = 1.21 Mg m -3, Z = 2. The structure was solved by MULTAN and refined to R(F o) = 0.032 and Rw(Fo) = 0.041 for 2059 reflections measured with graphite-monochromated Mo K~t radiation. The complex belongs to the category of solvent-separated ion-pair structures. The biphenyl anion is significantly non-planar. The local symmetry of the sodium-triglyme part of the structure is close to twofold and nearly 222.

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-di-n-butyldithiocarbamato)-gold(III) bis(1,2-dicyanoethene-1,2-dithiolato)aurate(III)

The crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)gold(III) bis(1,2-dicyanoethene-1,2-dithiolato)aurate(III), Au[S2CN(C4H9)2]2Au[S2C2(CN)2]2, has been determined from a single-crystal X-ray diffraction study. The monoclinic cell, space groupP21,/c, witha = 9·930(3),b = 12·517(3),c = 15·632(3) Å and β = 110·46(3) °, contains two formula units. Three-dimensional intensity data, up to θ = 35 ° were collected on an automatic diffractometer. Atomic parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·04 for 1874 independent non-zero reflections. The structure consists of bis(di-n-butyldithiocarbamato)gold(III) cations and bis(l,2-dicyanoethene-l,2-dithiolato)aurate(III) anions. In both ions, the gold atom is in planar coordination with four sulphur atoms, the Au-S bond lengths being 2·333(4) and 2·337(4) Å in the cation and 2·312(4) and 2·306(5) Å in the anion.

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.

Synthesis of a new heteronuclear gold–cobalt cluster. Preparation and X-ray structure determination of tetrakis (triphenylphosphine)-bis(tetracarbonylcobalt)hexagold

The reaction of [AU8L7]2+(L = PPh3) with an excess of Li[Co(CO)4] in tetrahydrofuran results in the formation of Au6L4[Co(CO)4]2, the structure of which has been determined by X-ray crystallography.

STRUCTURE AND PROPERTIES OF N,N-DI-n-BUTYLDITHIOCARBAMATO-1, 2-DICYANOETHENE-1, 2-DITHIOLATO-GOLD(III)

Abstract The crystal and molecular structure and some spectral data of the compound N,N-di-n-butyldithiocarbamato-1, 2-dicyanoethene-1, 2-dithiolato-gold(III), AuS2CN(C4H9)2S2C2(CN)2, are reported. The crystal structure has been determined from a three-dimensional single-crystal X-ray diffraction study. The orthorombic cell, space group Pbca, with a=14.066(3), b=28.980(2) and c=9.192(2) A, contains eight formula units. Intensity data were collected on an automatic diffractometer. The structural parameters were refined by full-matrix least-squares methods to a conventional R-factor of 0.047 for 1587 independent non-zero reflections. The structure determination proved the compound to be a mixed dithiocarbamato-dithiolato complex, Au(dtc)(mnt), (dtc=N,N-di-n-butyl-dithiocarbamate, mnt=maleonitriledithiolate ≡ 1, 2-dicyanoethene-1, 2-dithiolate), as expected from spectral data. The gold atom is in approximately square-planar coordination, however, deviations from mm2 (C2#) symmetry are considerable. Au-S bond...

Synthesis and X-ray crystal structure determination of the cationic gold cluster compound [Au8(PPh3)7](NO3)2

The reaction of [Au8L8](NO3)2(L = PPh3) with the phosphine scavenger [RhCl(C8H14)2]2 yields [Au8L7]-(NO3)2, X-ray analysis of which reveals the Au skeleton to be a fragment of the centred icosahedron; the cluster to be a fragment; the cluster is an intermediate in the reactions of [Au9L8]3+, and its 197 Au Mossbauer spectrum lacks, like that of [Au9L8]3+, a separate resonance for the central Au atom.

Crystal and molecular structure of cis- dibenzobicyclo(3.3.0) octa-2,7-diene, C16H14

AbstractThe structure of the title compound, C16H14, was determined by X-rays:Mr=206.29, monoclinic, space groupP21/n,a=5.002(1),b=23.972(5),c=9.505(2) Å,β=102.56(2)°,Vc=1112.4 Å3,Z=4,Dx=1.23 Mg m−3, MoKα radiation (graphite crystal monochromator,