An X-ray study of single crystals extracted from an arc-melted Yb-Fe-Ga alloy showed that the diffraction pattern can be modeled by an intergrown crystal that has three sorts of domains: one hexagonal (1, LuFe(9.5) type) and two rhombohedral (2 a and 2 b, PrFe(7) type), the last two twinned by reticular merohedry. Crystals 1 and 2 are essentially polytypes with maximum degree of order (MDO polytypes), built up of nearly identical slabs that are stacked along [001] in ABAB em leader (1). and ABCABC em leader (2). sequences. Structure refinement was performed by a newly developed program that allowed us to refine several structures on a single data set. We found that the hexagonal and rhombohedral domains differ in chemical composition: while 1 shows a higher rate of Yb substitution by Fe(2) dumbbells, 2 shows partial substitution of Fe by Ga. Our observation of the nanoscale phase segregation is supported by latest finding of nonrandom distribution of stacking faults in a similar 2:17 alloy. An unequal distribution of chemical substitutions in 1 and 2 apparently compensates the inherent mismatch of basal plane dimensions of the individual MDO polytypes and thus constrains their cell parameters within the syntaxy. According to our knowledge this is the first example of two chemically distinct polytypes constituting a single crystal, refined on a single set of diffraction data.