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A series of novel composite inorganic-organic materials from the copper-cyanide-triazolate-organoamine system have been isolated and structurally characterized. An unusual interpenetrating layered structure type composed of fused and flattened "slinkies", [Cu(6)(CN)(5)(trz)] (1) (trz = triazolate, C(2)N(3)H(2)(-)), a complex corrugated layer structure, [Cu(5)(CN)(3)(trz)(2)(bpy)] (2), and a series of increasingly intricate one-dimensional ribbons, [Cu(3)(CN)(2)(trz)(bpy)], [Cu(3)(CN)(2)(trz)(phen)], and [Cu(4)(CN)(3)(trz)(phen)] (3-5), have been isolated from hydrothermal media. All trz ligands are deprotonated and participate in &mgr;(3)-bridging of Cu sites. An anionic layered compound, [Cu(OH(2))(4)][Cu(4)(CN)(6)] (6), composed of {Cu(6)(CN)(6)} rings with tetraaquacupric dications intercalated into alternate interlamellar spaces, has also been characterized upon the slow evaporation of the mother liquor of 1. The syntheses and structural characterizations of compounds 1-6 by single-crystal X-ray diffraction and FTIR microscopy are discussed in relation to the supramolecular chemistry of other copper cyanide solid-state materials. Crystal data: C(7)H(2)Cu(6)N(8) (1), orthorhombic, Pcca, a = 11.108(2) Å, b = 8.886(2) Å, c = 15.397(3) Å, Z = 4; C(34)H(24)Cu(10)N(22) (2), triclinic, P&onemacr;, a = 9.1183(5) Å, b = 9.9838(6) Å, c = 12.7545(8) Å, alpha = 94.206(1) degrees, beta = 90.492(1) degrees, gamma = 112.534(1) degrees, Z = 1; C(28)H(20)Cu(6)N(14) (3), monoclinic, P2(1)/c, a = 9.7582(1) Å, b = 17.1622(2) Å, c = 9.901(1) Å, beta = 106.869(1) degrees, Z = 2; C(17)H(10)Cu(4)N(8) (4), monoclinic, P2(1)/c, a = 11.590(3) Å, b = 20.555(4) Å, c = 16.158(3) Å, beta = 103.865(5) degrees, Z = 8; C(16)H(10)Cu(3)N(7) (5), triclinic, P&onemacr;, a = 8.542(2) Å, b = 9.802(2) Å, c = 20.439(4) Å, alpha = 82.468(5) degrees, beta = 83.126(5) degrees, gamma = 79.832(5) degrees, Z = 4; C(6)Cu(5)N(6)O(4) (6), monoclinic, P2(1)/n, a = 7.466(1) Å, b = 8.952(2) Å, c = 11.116(2) Å, beta = 92.816(5) degrees, Z = 4.

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The compounds [Cu3Cl3(bipypy)] (1), [CuBr(bipypy)]2 (2), [Cu2Br2(bipypy)] (3), and [Cu3(CN)3(bipypy)] (4) were prepared from mixtures of the copper halide salts and the ligand bis-2,3-(2-pyridyl)pyrazine (bipypy) in hydrothermal media. The series of compounds includes molecular, one- and two-dimensional species and demonstrates a trend in increasing complexity. The synthetic conditions, methods of structural characterization and descriptions of the structures of compounds 1−4 are presented. Crystal data for C14H10Cl3Cu3N4 (1), orthorhombic, Pna21, a = 18.6778(5) Å, b = 5.1046(2) Å, c = 16.6257(2) Å, Z = 4; for C28H20Br2Cu2N8O2 (2), triclinic, P1̄, a = 7.795(1) Å, b = 8.857(1) Å, c = 11.1268(2) Å, α = 72.2(1)°, β = 83.050(1)°, γ = 73.832(1)°, Z = 1; for C14H10Br2Cu2N4 (3), monoclinic C2/c, a = 10.884(2) Å, b =16.713(4) Å, c = 9.307(2) Å, β = 113.199(5)°, Z = 4; and for C17H10Cu3N7 (4), monoclinic, P21/n, a = 12.8549(2) Å, b = 9.0875(1) Å, c = 16.0023(2) Å, Z = 4.

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