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Summary form only given. Recent experiments on As-S, As-S-Se and related compounds have demonstrated flexibility in forming fiber and film devices such as narrowband spectral Bragg filters, lens-arrays as well as couplers and self-written planar waveguides made from single and multilayer film structures. Efforts to optimize film properties and device performance have focused on identifying the chemical and structural origin of the linear and nonlinear response in terms of the material processing conditions used in creating the optical element. High molecular specificity in the microstructural analysis of samples, which strongly absorb in the visible is achieved by near-infrared Raman spectroscopy. Sub-components of the broad bands are compared with spectral signatures of possible structural units predicted by molecular modelling. We further discuss spatially resolved Raman spectra to directly probe the microstructure of multilayers and integrated optical devices.