The recent increased availability of additional wavelengths in the telecommunications window of about 1300-1600 nm has generated an interest in new optical materials and devices that can operate outside the normally used regions of 840 nm, 1310 nm, and 1550 nm. Specifically, methods to amplify fiber optical data transmission in the regions where there is limited or no existing methods to achieve amplification is of interest in the chemistry and photonic communities. Raman gain is one method that has been proposed to passively amplify optical data transmission through a distributed process. Amplification is obtained through a nonlinear light scattering process where an optical wave is amplified at the expense of a higher frequency pump wave. Multiple wavelengths can be evenly amplified simultaneously in a desired region by specific selection of one or more pump wavelengths. Herein, the synthesis and characterization of new hybrid inorganic/organic sol-gels and monomers capable of producing broad wavelength Raman scattering over a spectral range of 1200-1670 nm are presented. The synthetic methodology developed facilitates the systematic approach to produce sol-gel derivatives with functional groups known to be strongly Raman scattering. Additionally, a method to synthesize and characterize a large number of different compounds using a combinatorial approach was demonstrated. Thio based derivatives of sulfonyldiphenol, isopropylidenediphenol, and triallyloxy triazine were synthesized in addition to thio derivatives of poly(hydroxystyrene). Micro-Raman spectra of the hybrid sol-gels, thiobased derivatives, and IR spectra of select sol-gel monomers were obtained.