A two-wavelength method for the distinction of elements of similar ato
mic numbers in generally solved crystal structures, called delta-synth
esis, and its application to structures with no center of symmetry is
discussed. As an example the determination of the distribution of copp
er and nickel in the mineral muckeite (CuNiBiS3) is presented. Copper
occupies a tetrahedrally coordinated and nickel a tetragonal planar co
ordinated site. During these studies delta-synthesis proved to be a me
thod which is very robust against specimen-dependent errors of measure
ment.