Abstract
A new orthorhombic polymorph of silver malonate ( II) has been synthesized and structurally characterized. Compound II crystallizes in space group Pnma, with a = 12.8180(11), b = 9.2479(8), c = 4.0219(3) Å; V = 476.75(7) Å 3; Z = 4; ρ calc = 4.427 g cm −3. Full-matrix least-squares refinement converged to R 1 = 0.0099 ( I > 2 σ( I), 765 data) and w R 2 = 0.0264 ( F 2, 785 data, 51 parameters). The familiar eight-membered Ag 2(RCO 2) 2 ring, characteristic of most silver(I) carboxylate complexes, has a Ag–Ag distance of 2.977(1) Å. Puckered sheets in the crystal ab plane are connected along c to form a three-dimensional coordination polymer. The density of II is >30% higher than that of the monoclinic polymorph ( I), first characterized in 1981. A survey of the density ratios of polymorphs in the Cambridge Structural Database indicates that virtually all of the pairs of entries having a density ratio >1.2 involve at least one form with significant void volume, as estimated using PLATON. However, neither I nor II have significant void volume, which suggests that the silver malonate polymorphs represent one of the largest density differences observed to date for a polymorphic pair. To date, it has not been possible to prepare I in our laboratories.
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