RESUMO
The neutral metalloligand [CpFe(CO)2P(Se)(O(i)Pr)2] (Cp = η(5)-C5H5), which contains the rare secondary phosphite selenide moiety, reacts with different metal complex precursors to form six new heterobimetallic complexes containing M-Se-P-Fe(Cp) bond connectivity. The complexes [M(CO)5{CpFe(CO)2P(Se)(O(i)Pr)2}] (M = Cr, 1; M = W, 2), [MCl2{CpFe(CO)2P(Se)(O(i)Pr)2}2] (M = Pd, 3; M = Pt, 4), [Au4Cl4{CpFe(CO)2P(Se)(O(i)Pr)2}2], 5, and [AuI{CpFe(CO)2P(Se)(O(i)Pr)2}], 6, are all heterometallic, neutral, dinuclear (1, 2, 6), trinuclear (3, 4), and hexanuclear (5) complexes. The complexes were all prepared from straightforward substitution reactions (1-5) or as an adduct, 6. All new complexes were characterized by (1)H, (31)P, (77)Se NMR, infrared spectroscopy, elemental analysis and single crystal X-ray diffraction.
RESUMO
Novel lead pseudo polymorphs supported by diselenophosphate (dsep) ligands, [Pb{Se(2)P(O(i)Pr)(2)}(2)](n) (1alpha and 1beta), were synthesized and structurally characterized. The two structures differed in the binding modes of the dsep ligand. Each repeating unit in 1alpha was composed of a lead atom coordinated by two dsep ligands, one in a chelating mode and the other in a bridging-dangling mode. By contrast, the dsep ligands in 1beta adopted a bimetallic-biconnective (mu(1)-S, mu(1)-S) binding pattern. The bridging-dangling mode observed in 1alpha is the first example of this mode for the dsep ligand. [Pb{Se(2)P(O(i)Pr)(2)}(2)](n) could be successfully utilized as a single source precursor (SSP) for growing lead selenide (PbSe) nanostructures with different shapes via the solvothermal process. The morphologies of the as-grown PbSe structures were controlled by capping agents, poly(vinyl pyrrolidone) (PVP) and ethylenediamine, both bind on the {200} plane and enhance the growth rate of the <111> direction of the PbSe crystals, resulting in the formation of cubes and eight-horned rod dendrites, respectively. Raman spectroscopy was utilized to investigate the phonon vibration behaviour of the as-grown eight-horned rod dendrites. All peaks in the Raman spectra can be attributed to longitudinal (LO) and transverse (TO) optical phonon modes of the PbSe rod dendrites.