Crystal form F of [2S, 4R, 5R, 8R, 9S, 10S, 11R, 12R]-9-[(2,6-dideoxy-3-C--
methyl-3-O-methyl-.alpha.-L-ribo-hexopyranosyl)oxy]-5-ethyl-4-methoxy-2,4,-
8,10,12,14-hexamethyl-11-[[3,4,6-trideoxy-3-(isopropylmethylamino)-.beta.--
D-xylo-hexopyranosyl]oxy]-6,15-dioxabicyclo[10.2.1]pentadec-14(1)-ene-3,7--
dione (E)-2-butenedioic acid salt (2:1) showing strong X-ray diffraction
peaks at diffraction angles 2.theta.=6.6.degree. and 8.5.degree., Crystal
form D anhydrate of said compound showing strong X-ray diffraction peaks
at diffraction angles 2.theta.=7.1.degree., 13.5.degree. and
14.2.degree., Crystal form D X-hydrate of said compound showing strong
X-ray diffraction peaks at diffraction angles 2.theta.=7.1.degree. and
14.2.degree. but not showing a strong X-ray diffraction peak at a
diffraction angle 2.theta.=13.5.degree., Solvate Crystal forms G1, G2 and
G3 of said compound characterized by 2-theta angle positions in the
powder X-ray diffraction pattern of 5.4.degree., 10.4.degree.,
10.7.degree. and 12.1.degree.. Crystal form D X-hydrate of said compound
has more preferred properties for use as a pharmaceutical material such
as higher stability as compared with Crystal form D anhydrate of said
compound.