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This manuscript details the construction and demonstration of the first known microwave three-wave mixing (M3WM) experiment utilizing multiple arbitrary waveform generators (AWGs) completely operable in the 6–18 GHz frequency range for use in chirality determination and quantification. Many M3WM techniques, which involve two orthogonal, subsequent Rabi π/2 and π microwave pulses, suffer from flexibility in pulse types and timings as well as frequency due to most instruments only using one, one-channel AWG and the M3WM probability decreasing with an increasing quantum number, J. In this work, we presented an M3WM instrument that allows that flexibility by introducing multiple, synchronized AWGs and adheres to the high probability transition loop pathways in carvone. The functionality and reliability of the instrument were demonstrated using a series of experiments and mixtures of the R and S enantiomers and determined to be of similar accuracy to other reported M3WM setups with the additional benefit of flexibility in pulsing schemes. 

The molecules 1,1-difluorosilacyclopent-3-ene (3SiCPF 2 ) and silacyclopent-3-ene (3SiCP) have been synthesized and studied using chirped pulse, Fourier transform microwave (CP-FTMW) spectroscopy. For 3SiCP this is the first ever microwave study of the molecule and, for 3SiCPF 2 , the spectra reported in this work have been combined with that of previous work in a global fit. The spectra of each contain splitting which has been fit using a Hamiltonian consisting of semirigid and Coriolis coupling parameters. A refit of the original 3SiCPF 2 work was also carried out. All fits and approaches are reported. Analyses of the spectra provide evidence that the molecule is planar which is in agreement with the high-level calculations, but the source of the splitting in the spectra has not been determined.