A trinuclear linear Mo-Fe-Mo dialkyldithiocarbamate complex [Et4N] { [ Me2dtcMoO (μ-S)2 ]2Fe} has been obtained and structurally characterized, which contains two Me2dtcMoO-(μ-S)2 units coordinated to a central tetrahedral Fe atom. A comparison of the structural parameters indicates the metal oxidation states of 2Mo(v) + Fe(III). The 1H NMR shows chemical shifts of Me2dtc ligands at 5 10.14 and 8 9.40 with the intensity ratio of 1:1. The cyclic voltammogram displays a reversible couple at - 1.41 V/ - 1.36 V responsible for 1-/2-anions of the complex and an irreversible oxidation at 0.5 V, which seems to show the apparent lack of stability for its neutral species (Me2dtcMoOS2)2Fe.
Complex (Et 4N)[VFe 3S 4Cl 3(CH 3CN) 3] (1) has been obtained from (NH 4) 3VS 4/FeCl 2/NaHS/Et 4NCl reaction system in CH 3CN solvent and structurally characterized by X ray diffraction analysis. It crystallizes in orthorhombic space group Pnma (No. 62) with a=8.851(2), b=16.447(3), c=19.448(4) , V=2865.6(10) 3, Z=4, M r=706.49, D c =1.638g/cm 3 , F(000)=1428, μ (Mo Kα )=2\^385 cm -1 and T= 293(2)K. With use of 1467 observed reflections ( I>2σ(I )) the structure was refined to R =0.0874 and wR= 0.2065. Complex 1 contains a VFe 3S 4 cuboidal core with average V-Fe distance of 2.759(4) , which is a little longer than Fe-Fe of 2.716(3). Around the core, each Fe atom is coordinated by one Cl atom and V atom by three N atoms of CH 3CN ligands.
The title compound (C6H5NH2)2PdCl2 was prepared by the reaction of N-phenylbenzaldimine with dichlorobis(benzonitrile) palladium (Ⅱ) in methanol and its structure was characterized by single-crystal X-ray diffraction. The title complex crystallizes in monoclinic system, space group P21/c, C12H14Cl2N2Pd, Mr = 363.55, a = 6.0668(7), b = 4.7691(5), c = 23.006(3) ? b = 95.118(2)? V = 662.99(13) ?, Z = 2, Dc = 1.821 g/cm3, m = 1.780 mm-1, F(000) = 360, the final R = 0.0624 and wR = 0.1271 for 850 observed reflections. Two bifurcated intermolecular NH…Cl hydrogen bonds are observed, forming a strip structure.
A cubane-type molybdenum cluster compound Mo4S4(DTP)4[-SOP(OEt)2]2 A (DTP = diethyl dithiophosphate) was obtained from the reaction of cation [Mo3O2S2(H2O)9]4+ B with metal tin as well as HDTP. The crystal structure has been determined by X-ray crystallography and the data for the title compound: Mo4S14P6O14C24H60, triclinic P , Mr = 1591.14, a = 12.5596(5), b = 14.3441(5), c = 18.0005(6) ? = 85.318(1), = 70.495(1), = 78.415(2)? V = 2994.2(2) ?, Z = 2, Dc = 1.765 g/cm3, (MoK? = 1.515 mm-1, F(000) = 1596, R = 0.0918 and wR = 0.1908 for 3546 reflections (I > 2(I)). X-ray analysis reveals that two weak CH贩稯 hydrogen bonds exist in the packing diagram with C贩稯 distance 3.22(5) ? The structure of A is similar to that of -Mo4S4(DTP)6 except that one sulfur of each bridging DTPs has been replaced by oxygen during the reaction, resulting in two bridging [SOP(OEt2)2] - ligands.
A novel supramolecular compound, [Co(IN)2(H2O)4](1), was synthesized by means of the hydrothermal method and its structure was characterized with elemental analysis, FT-IR spectrum, TGA and X-ray diffraction. Though the unit cell structure of the title compound is only monomeric, all these units as building blocks are assembled into a novel three-dimensional supramolecular network via the widely hydrogen-bonding and π-π stacking interactions.
