The 8,17-bis(2-pyridylmethyI) -functionalised derivative ( Lz) of a 14-membered trans-N,S, dibenzo macrocycle 6,7,8,9,15,16,17,18-octahydrodibenzo[ f,m] E1.8.4.11 ]dithiadiazacyclotetradecine has been prepared and its crystal structure determined. The ligand Lz forms stable complexes with nickel(l1) 1, copper(ii) 2 and cobalt(i1) 3. The complexes have been isolated in the solid state and characterised by standard methods and single-crystal X-ray diffraction. Crystal data for L2: space group P2,lc. a = 945.6(1), b = 1467.9(2), c = 1041.1 (2) pm, p = 115.67(1)", Z = 2, R(R') = 0.035(0.040) for 2183 observed reflections. Complex 1: space group P2,/n, a = 1418.8(3), b = 1288.8(3).c = 1867.0(4) pm, p = 109.20(3)", Z = 4, R ( R ' ) = 0.067(0.068) for 4124 observed reflections. The nickel atom lies outside the macrocyclic cavity and is in a distorted octahedral cis-N,S, environment. Complex 2: space group P r , a = 787.8(2), b = 11 37.5(2), c = 1800.5(4) pm. z = 98.84(3), p = 99.43(3), y = 94.74(3)", Z = 2, R ( R ' ) = 0.082(0.075) for 2165 observed reflections. The copper atom exhibits a highly distorted trigonal-prismatic co-ordination geometry with the following distances: Cu-S, 242.7(4) and 269.8(4), Cu-N(amine) 225.8(11) and 255.2(10) and Cu-N(pyridine) 198.4(11) and 200.2(12) pm, respectively. Complex 3: space group P i , a = 789.3(2), b = 1165.8(2), c = 1806.2(3) pm, a = 98.90(1), p = 98.86(2), y = 94.24(2)", Z = 2, R(R') = 0.066(0.063) for 3039 observed reflections. The geometry about high-spin cobalt(ii) is trigonal prismatic with average Co-S, Co-N(amine) and Co-N (pyridine) bond lengths of 252.5, 229.0 and 213.7 pm, respectively. The stereochemistry of the free and complexed ligand is discussed

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Die beiden isomeren Liganden 6,7,9,15,16,18‐Hexahydrodibenzo[f,m][1,8]dithia[4,11]diazacyclotetradecin‐8,17‐diessigsäure‐0,5‐hydrat (H2L3), C22H26N2O4S2 · 0,5 H2O bzw. 6,7,13,15,16,18‐Hexahydrodibenzo[e,m][1,4]dithia‐[8,11]diazacyclotetradecin‐14,17‐diessigsäure‐1,5‐hydrat (H2L6), C22H26N2O4S2 · 1,5 H2O mit cis‐ bzw. trans‐N2S2‐Donorzentren im vierzehngliedrigen makrocyclischen Ring und zwei Acetat‐Seitenketten bilden die stabilen Komplexe [Co(L3)]ClO4 · 2H2O (1) und [Co(L6)]ClO4 · H2O (2). CoIII ist jeweils von allen 6 Donorzentren der Liganden oktaedrisch umgeben. Die Liganden sind gefaltet. Die Metallatome liegen außerhalb der makrocyclischen Kavität. Kristalldaten: 1, monoklin, Raumgruppe C2/c, a = 3 797,7(9), b = 763,8(3), c = 2 207,0(7) pm, β = 123,17(2)°, Z = 8, 3 445 Reflexe, R(Rw) = 0,072(0,070); 2, monoklin, Raumgruppe C2/c, a = 3 197,1(6), b = 880,4(2), c = 1 890,6(4) pm, β = 112,19(3)°, Z = 8, 4415 Reflexe, R(Rw) = 0,062(0,064).

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