Investigation of the interaction between the 4.4'-bipyridinium(2+) cation (4.4'-H,bipyz+) and the octacyanometalates(1v) [M (CN),I4-(Mo or W) led to the isolation of [4,4'-H2bipy],[W(CN,)]-4.5H,0 and its isomorphous molybdenum analogue. The spectroscopic properties of both and the X-ray structural characterization of the former [monoclinic, space group P2,/c, a = 11.281 (5). b = 9.1 98(5), c = 30.1 13(24) 8, p = 91.21 (5)O. Z = 4 1 are described. The [W(CN),I4-anion has an approximate square-antiprismatic D, configuration with average dimensions W-C 2.1 68, C-N 1.1 36

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