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  • 1
    ISSN: 0044-2313
    Keywords: Cobalt(III) complexes functionalized N2S2-macrocyclic ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Cobalt(III) Complexes of 14-Membered cis- and trans-N2S2 Dibenzo Macrocycles with two Pendant Acetato GroupsThe isomeric fourteen membered macrocyclic ligands 6,7,9,15,16,18-hexahydrodibenzo[f,m][1,8]dithia[4,11]diazacyclotetradecine-8,17-diacetic acid-0.5-hydrate (H2L3), C22H26N2O4S2 · 0.5 H2O and 6,7,13,15,16,18-hexahydrodibenzo-[e,m][1,4]dithia[8,11]diazacyclotetradecine-14,17-diacetic acid-1.5-hydrate (H2L6), C22H26N2O4S2 · 1.5 H2O with cis- and trans-N2S2 donorsets and two pendant acetato groups form the stable complexes [Co(L3)]ClO4 · 2 H2O (1) and [Co(L6)]ClO4 · H2O (2). Co(III) is octahedrally coordinated herein to all six donor centers of the respective ligand. The macrocyclic rings are folded. The metal ions are located outside the macrocyclic cavity. The mean Co—N, Co—O and Co—S distances are 196, 190 and 224 pm, respectively.Crystal data: 1, monoclinic, space group 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 reflections, R(Rw) = 0.072(0.070); 2, monoclinic, space group C2/c, a = 3 197.1(6), b = 880.4(2), c = 1 890.6(4) pm, β = 112,19(3)°, Z = 8, 4 415 reflections, R(Rw) = 0.062(0.064).
    Notes: 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).
    Additional Material: 3 Ill.
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  • 2
    ISSN: 0009-2940
    Keywords: Copper complexes ; Macrocyclic ligands, N-functionalized ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: trans-N2S2-Macrocyclic Ligands with Pendant Carboxylic Groups. - Synthesis of 6,7,8,9,15,16,17,18-Octahydrodibenzo[f,m][1,8,4,11]dithiadiazacyclotetradecine-8,17-diacetic Acid (H2L1); Structures of Corresponding Copper ComplexesThe macrocyclic ligand with pendant carboxylic groups 6,7,8,9,15,16,17,18-octahydrodibenzo[f,m][1,8,4,11]dithiadiazacyclotetradecine-8,17-diacetic acid (H2L1) and its Ni(II) and Cu(II) complexes, [NiL1]3(H3O·ClO4)4·H2O (1) and [Cu(HL1)]ClO4·1.5 H2O (2), have been prepared. The coordination properties of H2L1 towards Ni(II) and Cu(II) in aqueous solutions are independent on the pH according to UV/Vis-spectral measurements. The structures of 2 and of [CuL2]ClO4 (3) with HL2 = 6,7,8,9,15,16,17,18-octahydrodibenzo[f,m][1,8,4,11]dithiadiazacyclodetradecine-8-acetic acid have been determined by X-ray crystallography. In 2, all six donor atoms of the ligand are coordinated, forming an octahedron. Due to their size the metal atoms are not incorporated in the ligand cavity. The ligand is folded in such a way, that the N-donor atoms are in trans, and the S-(and O-)donor atoms in cis positions. In 3, the five donor atoms form a rather regular bipyramid with the N atoms in the axial positions. The stereochemistry of the ligands in the complexes 2 and 3 is discussed.
    Additional Material: 2 Ill.
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