A new compound [Yb3(C9H6NO)8⋅ (CH3COO)]⋅3CHCl3 (I) has been synthesized. The complex crystallizes in the monoclinic syngony, space group P21/n: a=18.971(4); b=19.473(4); c=20.914(4) Å; β=100.68(3)°; V=7592(3) Å3; Z=4. The structure of compound I has been determined using the automatic X-ray diffractometer CAD-4 (λMoKα radiation). The structure model has been established by the heavy atom method. Coordinates of itterbium, oxygen, nitrogen, carbon and chlorine atoms have been refined by the least squares method in anisotropic approximation up to the final R factor values R1=0.0397; wR2=0.1024. Three crystallographically independent Yb atoms have distorted antiprism (Yb(1)) and dodecahedral(Yb(2) and Yb(3)) coordination. The Yb(1) atom is coordinated with two oxygen atoms of the acetate anions and with six oxygen atoms of the 8-hydroxyquinolinate anion. The Yb(2) and Yb(3) atoms each are bidentally coordinated with four O atoms and four N atoms from four 8-hydroxyquinolinate anions. Six from eight oxygen atoms of 8-hydroxyquinoline ligand possess both the complexing and bridge atom functions. The neighbouring Yb atoms are bonded with three O atoms from three 8-hydroxyquinolinate anions. The interatomic distances of Yb(2)…Yb(1)…Yb(3) are 3.450(2) and 3.439(2) Å respectively.