PREPARATION AND CRYSTAL-STRUCTURE OF TETRAAQUA-BIS(HYDROGENOPYRIDINE-2,3(DI CARBOXYLATE)BIS(PYRIDINE-2,3-DICARBOXYLATE)HEXA SILVER(I) [AG-6(C7H4NO4)(2)(C7H3NO4)(2)(H2O)(4)](N)
F. Jaber et al., PREPARATION AND CRYSTAL-STRUCTURE OF TETRAAQUA-BIS(HYDROGENOPYRIDINE-2,3(DI CARBOXYLATE)BIS(PYRIDINE-2,3-DICARBOXYLATE)HEXA SILVER(I) [AG-6(C7H4NO4)(2)(C7H3NO4)(2)(H2O)(4)](N), Polyhedron, 15(17), 1996, pp. 2909-2913
The title compound was precipitated by the action of freshly prepared
Ag2O on an aqueous solution of pyridine-2,3-dicarboxylic acid. The whi
te compound was redissolved in hot water and crystals suitable for X-r
ay diffraction study were grown. The crystal is a polymeric network; f
ive-membered chelate rings (-C-N-Ag-O-C-) and dimeric units (AgOCO')(2
) sequenced in two types of similar chains linked by Ag-Ag bonds and s
hort intermolecular hydrogen bonds are presented simultaneously. The f
our Ag atoms of the asymmetric unit show two different environments. A
g(1) and Ag(2), sitting on a symmetry centre, are each included in two
chelating rings. So, Ag(1) and Ag(2) are in four-coordinated planar e
nvironments: Ag(1)-N(21) = 2.166(5), Ag(1)-O(24) = 2.705(4), Ag(2)-N(1
1) = 2.172(4), Ag(2)-O(11) = 2.706(5) Angstrom, N(21)-Ag(1)-O(24) = 67
.7(2), N(11)-Ag(2)-O(11) = 68.4(2)degrees. Ag(3) and Ag(4) are include
d in eight-membered rings, (AgOCO')(2) with bipyramidal trigonal arran
gement constituted by two Ag atoms [Ag(3)-Ag(3(ii)) = 2.843(2), Ag(3)-
Ag(4(i)) = 3.090(2), Ag(4)-Ag(4(v)) = 2.894(1) Angstrom, two oxygen ca
rboxylic atoms [Ag(3)-O(23) = 2.271(5), Ag(3)-O(24(ii)) = 2.245(4), Ag
(4)-O(12(v)) = 2.236(6), Ag(4)-O(11) = 2.242(6) Angstrom] and one aque
ous oxygen atom [Ag(3)-O(wl) = 2.329(6), Ag(4)-O(w2) = 2.399(5) Angstr
om]. The H carboxylic hydrogen atoms of the hydrogenopyridine-2,3-dica
rboxylate ligands being split between two carboxylate groups are invol
ved in short intermolecular hydrogen bonds between two carboxylic grou
ps: O(13)...O(22(ii)) = 2.459(4) Angstrom. Copyright (C) 1996 Elsevier
Science Ltd