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 (Et4N) [VFe3S4Cl3 (CH3CN)(3)] (1) has been obtained from (NH4)(3) VS4/FeCl2/NaHS/Et-4 NCl reaction system in CH3CN 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) Angstrom, V = 2865.6(10) Angstrom (3), Z = 4, M-r = 706.49, D-c =1.638g/cm(3), F(000)=1428, mu (MoK alpha)=2.385 cm(-1) and T = 293(2)K. With use of 1467 observed reflections (I >2 sigma (I)) the structure was refined to R = 0.0874 and wR = 0.2065. Complex 1 contains a VFe3S4 cuboidal core with average V - Fe distance of 2.759(4) Angstrom, which is a little longer than Fe - Fe of 2.716(3) Angstrom,. Around the core, each Fe atom is coordinated by one Cl atom and V atom by three N atoms of CH3CN 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.
Six model compounds have been synthesized and used for probing the structural features of the Mn cluster in oxygen_evolving complex (OEC) of photosystem Ⅱ (PSⅡ). The model compounds contain Mn 2(μ_O) 2 and μ_O_μ_carboxylato di_manganese structural units, which offer Mn—Mn, Mn……Mn, and Mn—O(N) structural parameters consistent with the corresponding data of the OEC in PSⅡ, implying that the Mn cluster in OEC may possess similar structural features. Two model compounds containing halide anion have been used for discussing the binding of Cl - to Mn in PSⅡ. It is suggested that in the five S states, ligand exchange would lead to the ligation of chloride to Mn in the S states with Mn of higher valence.
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(H_2O)_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.
