The Endless Chain [AcOHg]nn+ Cation. Crystal Structure of Acetatomercury(II) Nitrate - Mercury(II) Acetate (1/1)

Acetatomercury(II) nitrate-mercury(II) acetate (llI), (AcOHg) N03 • Hg(AOch, not described so far in the chemical literature,\u27 was obtained by the reaction of mercury(II) nit rate hydrate with acetic anhydride. Orthorhombic-disphenoidal crystals, as shown by threedimensional X-ray diffraction analysis, are built of polymeric [AcOHg]nn+cations, nitrate anions and mercury(II)-acetate molecules. The mercury ions in the cation are bridged over by the acetate ion through both oxygen atom s separately at the Hg-O distances of 213(3) and 212(2) pm under the O-Hg-O arigle of 167(1)°. The mercury(II)-acetate molecule is in syn. conformation with the Hg-O distances of 204(3) and 209(3) pm and the O-Hg-O angle of 173(1)°. Crystal structure, determined from 1330 intensity data, was refined by full-rnatrix least-squares method to R = 0.076 and Rw = 0.090

Mercuration of Some Aliphatic Aldehydes. The Crystal Structure of 2,2-Bis(chloromercuri)butyraldehyde

Tris ( chloromercuri)acetaldehyde (1), 2,2-bis( chloromercuri)propionaldehyde (II) and 2,2-bis(chloromercuri)butyraldehyde (III) were obtained by mercuration of the corresponding aldehyde in an aqueous mercury(II) chloride solution containing sodium acetate. The mercurated aldehydes (II) and (III) are described for the first time. The crystal structure of (III) was determined by means of Patterson and Fourier syntheses based on threedimensional X-ray diffractometer intensity data and refined by the full-matrix least- squares method to an R value of 0.049. Crystals are orthorhombic, space group Pna21 with z = 4 formula units in the unit cell of the dimensions : a= 1114.6(6), b = 1121.3(5), c = 657.3(3) pm, Dots= 4.51and Deale = 4.38 Mg m-3• The structure consists of discrete moleculesof 2,2-bis(chloromercuri)butyraldehyde. The Hg-C bond lengthsare 216(2) and 209(2) pm. The Hg-C-Hg bond angle is 103(1) 0 and the C-Hg-Cl bond angles are 173(2)0 and 172(2)0 , respectively

Synthesis of Two Novel Tetranuclear Molybdenum(V) Complexes. Crystal Structure of Hexa-μ-propionato-dichlorodi-μ3-oxotetraoxotetramolybdenum(V)

In the reaction of MoO2Cl2 and MoO22Br2 with propionic anhydride, new complexes of molybdenum(V), and Mo4O6Br2(OCOC2H5)6, respectively, have been prepared. The crystal structure of the former was determined from single crystal diffractometer data and refined to the final R value of 0.046. The complex crystallizes in the monoclinic space group P2!n with cell dimensions a = 11.713(2) Å, b = 9.292(3) Å, c = 30.957(6) Å, f = 96.71(2)°, Z)caic = 1.963 g cm-3, Z = 4. The tetranuclear complex molecule contains four molybdenum atoms bridged through two oxo- oxygen atoms and six bidentate propionato-ligands. Two of the four molybdenum atoms form a Mo-Mo bond at 2.592(3) A

Synthesis of Two Novel Tetranuclear Molybdenum(V) Complexes. Crystal Structure of Hexa-μ-propionato-dichlorodi-μ3-oxotetraoxotetramolybdenum(V)

In the reaction of MoO2Cl2 and MoO22Br2 with propionic anhydride, new complexes of molybdenum(V), and Mo4O6Br2(OCOC2H5)6, respectively, have been prepared. The crystal structure of the former was determined from single crystal diffractometer data and refined to the final R value of 0.046. The complex crystallizes in the monoclinic space group P2!n with cell dimensions a = 11.713(2) Å, b = 9.292(3) Å, c = 30.957(6) Å, f = 96.71(2)°, Z)caic = 1.963 g cm-3, Z = 4. The tetranuclear complex molecule contains four molybdenum atoms bridged through two oxo- oxygen atoms and six bidentate propionato-ligands. Two of the four molybdenum atoms form a Mo-Mo bond at 2.592(3) A