The intercalation reaction of n-alkylamines from methyl- to hexadecylamine into alpha-tin (IV) bis(hydrogenphosphate) has been investigated. The reaction was conducted by mixing the phosphate and solutions of the amines dissolved in water or benzene. The amine/phosphate molar ratios in the reaction mixtures were 0.43, 0.85, 1.71 and 3.41. The nitrogen/phosphorus atomic ratio in the intercalation compound was not changed by the amine/phosphate molar ratio. The interlayer distances of the intercalates obtained in the reaction mixtures with molar ratios of 3.41 and 1.71 increased with an increase in the number of carbon atoms in the alkyl chain of the amine. The slope of the straight line obtained in plot of interlayer distance versus number of carbon atoms in the alkyl chain of the amine indicates that the amine molecules form a double layer in the interlayer space of the phosphate and are inclined at an approximate angle of 67.7 degrees to the phosphate layer. The interlayer distances of the intercalates of butyl- to nonylamines obtained at the molar ratio of 0.85 are smaller than those of the corresponding compounds from the molar ratios of 3.41 and 1.71, while those of decyl- to hexadecylamine intercalates lie on the previously discussed line. This behaviour is interpreted by assuming kink formation in the short alkyl chains between the phosphate layers.