Characterization crystals synthesized

Shibata, T. Muranushi, Y. Miura, T. Kishi, T. 1991. Electrical characterization of 2H-SnS2 single crystals synthesized by the low temperature chemical vapor transport method. J. Phys. Chem. Solids 52 551-553. 

The first simple sodium phosphide to be structurally characterized was synthesized in 1995 by Raston and co-workers (68). The complex [Na(PHCy)(pmdeta)]2 crystallizes as dimers with a central planar P2Na2 ring and a trans arrangement of the cyclohexyl substituents across the ring [Na-P = 2.884(8), 2.936(7) A Na-P-Na = 86.2(2)°]. 

Crystal syntheses do not differ, in their essence, from classical chemical experiments in which molecules are modelled, synthetic routes devised, products characterized and their properties evaluated. However, this typical chemical approach needs, in a sense, to be repeated twice first, in order to prepare the building blocks (whether molecules or ions), and then to arrange the building blocks in a desired way via nucleation, precipitation and crystallization to attain and/or control crystal properties. Obviously, crystallization invariably implies the need to characterize the solid product, often in the form of a polycrystalline powder, for which routine analytical and spectroscopic laboratory tools are much less useful than in the case of solution chemistry. 

Jing H, Edulji SK, Gibbs JM, Stem CL, Zhou H, Nguytai ST (2004) (Salen)tin complexes syntheses, characterization, crystal stractures, and catalytic activity in the formation of propylene carbonate from CO2 and propylene oxide. hiOTg Chem 43(14) 4315-4327... 

Jing, H. Edulji, S. K. Gibbs, J.M. Stem, C.L. Zhou, H. Nguyen, S. T. (Salen)Tin Complexes Syntheses, Characterization, Crystal Stmctures, and Catalytic Activity in the Formation of Propylene Carbonate from CO and Propylene Oxide. Inorg. Chem. 2004,43,4315 327. 

Syntheses, crystallization, structural identification, and chemical characterization of high nuclearity clusters can be exceedingly difficult. Usually, several different clusters are formed in any given synthetic procedure, and each compound must be extracted and identified. The problem may be compounded by the instabiUty of a particular molecule. In 1962 the stmcture of the first high nuclearity carbide complex formulated as Fe (CO) C [11087-47-1] was characterized (40,41) see stmcture (12). This complex was originally prepared in an extremely low yield of 0.5%. This molecule was the first carbide complex isolated and became the foremnner of a whole family of carbide complexes of square pyramidal stmcture and a total of 74-valence electrons (see also Carbides, survey). 

A comparable compound, (Me2N)2BPPh2-Cr(CO)5, was synthesized by Noth et al. but not structurally characterized by single crystal X-ray diffraction Noth H, Sze SN (1978) Z Naturforsch B Anorg Chem Org Chem 33 1313... 

For ruthenium, special precursors are required to synthesize defined bidentate diphosphine complexes. With Taniaphos for instance, it is possible to synthesize such complexes starting from unusual rathenium(ll) species. The complexes were characterized by NMR and single crystal analysis. 

Goff (54) synthesized an Fe(III) porphyrin with a 2-hydroxyphenyl group at one meso position (35, Fig. 12a). Under basic conditions, the system spontaneously dimerizes due to phenolate-Fe(III) coordination. The complex is very stable and was isolated and fully characterized. In the solid state, the X-ray crystal structure confirmed the structure of the assembly as a macrocyclic head-to-tail dimer with two intermolecu-... 

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