Two compounds 3,3’-(9,10-anthrylene)bis-pentane-2,4-dione 1 and 3-(2-methoxy-1-naphthalenyl)-pentane-2,4-dione 2 were synthesized by the direct arylation of pentane-2,4-diones in the presence of Mn(OAc)3 and H3PO4. Their crystal structures were determined by X-ray diffraction method. Compound 1, C24H22O4, Mr = 374.4, crystallized in the monoclinic system, space group P21/a with a = 7.393(4), b = 14.308(5), c = 10.099(5) ? = 110.8(4)? V = 999.0 (9) 3, Z = 2, Dc = 2.49g/cm3, F(000) = 392, ?= 0.78cm-1, final R = 0.050 and Rw = 0.057 for 1144 observed reflections with I≥3.00 ?(I). The molecular backbone is the anthracene ring, and two acetoacetone groups are perpendicular to the anthracene ring at 9,10 positions. Compound 2, C16H16O3, Mr = 256.3, crystallized in monoclinic system, space group C2 with a = 14.369(3), b = 7.480 (1), c = 15.878 (2) ? = 128.46(1)? V = 1336.3(4) ?, Z = 4, Dc = 1.27g/cm3, F(000) = 544, ?= 0.81cm-1. The structure was solved by direct methods and refined by full-matrix least-squares method, final R = 0.044 and Rw = 0.040 for 764 observed reflections with I ≥3.00(I). The acetoacetone group in compound 2 is also vertical to the naphthalene ring.
