The optimized synthesis of a phospho-vanadyl compound, [Cu(VO)(2)(PO4)(2)(H2O)(4)](n), is presented and its structural analysis is performed and discussed in relation to magnetic properties. The structure consists of a 2-D skeleton parallel to (100), made up by two independent VO6 octahedra linked by phosphates. Neighboring 2-D structures stack along [100] and are connected by aqua-mediated H-bonds. The spatial disposition of paramagnetic ions gives rise to weak antiferromagnetic behavior, with J= -17 cm(-1), which is consistent with a model of three paramagnetic centers in an irregular triangular arrangement. An optimization of the synthesis process, looking for a response surface with optimum experimental values, was performed using a multivariate analysis.