The reaction of Ph3SnCl, (R4N)(2)[Mo6O19] and (R4N)OH in a molar ratio of 6:1:10 leads to the formation of (R4N)[(Ph3Sn)MoO4] (R = Pr-n (1), Bu-n (2)). Compounds 1 center dot CH3CN and 2 have been charactarized by IR spectroscopy and single crystal X-ray diffraction. 1 center dot CH3CN forms orthorhombic crystals, space group P2(1)2(1)2(1) with a = 1339.9(2), b = 1508.9(2), c = 1733.2(3) pm. 2 crystallizes in the monoclinic space group P2(1) with a = 1342.6(2), b = 2280.3(4), c = 1344.0(2) pm, beta = 118.34(1). Both compounds 1 and 2 consist of isolated R4N+ cations and polymeric (1)(infinity)[(Ph3Sn)MoO4](-) chains with an alternating arrangement of Ph3Sn+ and MoO42- groups. Treatment of (Ph3Sn)(2)MoO4 with bis(ethylenediamine)copper(II) succinate yields [Cu(en)(2)(Ph(3)Sn())2(MoO4)(2)] (3). The zinc derivative [Zn(en)(2)(Ph3Sn)(2)(MoO4)(2)] (4) is obtained similarly by reaction of (Ph3Sn)(2)MoO4 with bis(ethylenediamine)zinc(II) formiate. Compounds 3 center dot 2DMF center dot EtOH and 4 center dot 2DMF center dot EtOH crystallize in the monoclinic space group P2(1)/n with a = 1998.0(2), b = 1313.3(1), c = 2181.6(2) pm, beta = 90.97(1)degrees for 3 and a = 2015.4(1), b = 1316.7(1), c = 2157.0(1) pm, beta = 90.40(1)degrees for 4. Like in the cases of 1 and 2, polymeric (1)(infinity)(Ph3Sn)MoO4] chains are observed. The [M(en)(2)](2+) units (M = Cu, Zn) act as linkers between the (1)(infinity)[(Ph3Sn)MoO4] chains to give 2D layer structures with (6, 3) net topology.