Clidinium bromide is an anticholinergic drug which may help symptoms of cramping and abdominal stomach pain by decreasing stomach acid and slowing the intestines. It is commonly prescribed in combination with chlordiazepoxide by the name of clidinium-c. Accurate, simple, and selective stability-indicating reversed phase HPLC and TLC-densitometric methods with UV detection have been developed and validated for simultaneous determination of chlordiazepoxide and clidinium bromide in the presence of its alkaline induced degradation product. Successful separation of the drugs from the degradation product was achieved. The spectroscopic and structural morphology properties of the charge transfer complex of the anticholinergic drug clidinium bromide with picric acid have been studied in three polar solvents acetonitrile, methanol, and ethanol at room temperature. The formed transfer complex complex in each solvent was characterized in both solution and solid state using electronic, IR, and 1H and 13CNMR spectroscopies and XRD, SEM, TEM, and CHN elemental analyses. The outcome suggests that the formation of the CT complex is high in less polar solvent and that its spectroscopic and morphologic characteristics are markedly affected by the variation in solvent polarity. The United States Pharmacopeia (USP) stated the nonaqueous titration method for the assay of clidinium bromide and chlordiazepoxide[3,4,5,6]. Few methods for the determination of clidinium bromide and chlordiazepoxide in combined dosage forms including HPLC[7,8,9], derivative spectrophotometry[10,11], spectrophotometry using multivariate calibration techniques, and capillary SFC have been reported. The present article reports studies on interactions between clidinium bromide drug and some of divalent transition metal ions like (Mn(Ⅱ), Ni(Ⅱ), and Hg(Ⅱ)). The elemental analysis, conductivity, IR and, 1H-NMR, electronic spectral studies of these complexes were assignments and deduced the suggested structure via deprotonation of the hydroxyl —OH group.