Oxamato-Bridged Trinuclear Ni<sup>II</sup>Cu<sup>II</sup>Ni<sup>II</sup> Complexes: A New (Ni<sup>II</sup>Cu<sup>II</sup>Ni<sup>II</sup>)<sub>2</sub>\nHexanuclear Complex and Supramolecular Structures. Characterization\nand Magnetic Properties
Javier Tercero (2343754)Carmen Diaz (1556782)Joan Ribas (833748)Miguel Maestro (2030371)José Mahía (2470852)Helen Stoeckli-Evans (2172040)
Abstract
Eight oxamato-bridged heterotrinuclear Ni<sup>II</sup>Cu<sup>II</sup>Ni<sup>II</sup> complexes of formula {[Ni(H<sub>2</sub>O)(dpt)]<sub>2</sub>(μ-Cu(H<sub>2</sub>O)(opba))}(ClO<sub>4</sub>)<sub>2</sub>\n(<b>1</b>), {[Ni(H<sub>2</sub>O)(dien)]<sub>2</sub>(μ-Cu(pba))}(ClO<sub>4</sub>)<sub>2</sub>·6H<sub>2</sub>O (<b>2</b>), {[Ni(H<sub>2</sub>O)(Medpt)]<sub>2</sub>(μ-Cu(OHpba))}(ClO<sub>4</sub>)<sub>2</sub>·4H<sub>2</sub>O (<b>3</b>), {[Ni(H<sub>2</sub>O)(dien)]<sub>2</sub>(μ-Cu(Me<sub>2</sub>pba))}(ClO<sub>4</sub>)<sub>2</sub>·2.5H<sub>2</sub>O (<b>4</b>), {[Ni(H<sub>2</sub>O)(dpt)]<sub>2</sub>(μ-Cu(Me<sub>2</sub>pba))}(ClO<sub>4</sub>)<sub>2</sub>·2H<sub>2</sub>O (<b>5</b>), {[Ni(H<sub>2</sub>O)(dien)]<sub>2</sub>(μ-Cu(OHpba))}(ClO<sub>4</sub>)<sub>2</sub>·4H<sub>2</sub>O (<b>6</b>), {[Ni<sub>2</sub>(dpt)<sub>2</sub>(μ-Cu(H<sub>2</sub>O)(pba))]<sub>2</sub>(μ-N<sub>3</sub>)<sub>2</sub>}Na<sub>2</sub>(ClO<sub>4</sub>)<sub>4</sub>·6H<sub>2</sub>O (<b>7</b>), and {[Cu(H<sub>2</sub>O)<sub>2</sub>(dpt)Ni<sub>2</sub>(H<sub>2</sub>O)(dpt)<sub>2</sub>](μ-H<sub>2</sub>Me<sub>2</sub>pba(2−))}(ClO<sub>4</sub>)<sub>4</sub>·3H<sub>2</sub>O (<b>8</b>) in which opba = <i>o</i>-phenylenbis(oxamato), pba = 1,3-propylenebis(oxamato), OHpba = 2-hydroxy-1,3-propylenebis(oxamato), Me<sub>2</sub>pba = 2,2-dimethyl-1,3-propylenbis(oxamato),\ndpt = 3,3‘-diaminodipropylamine, dien = 2,2‘-diaminodiethylamine, and Medpt = 3,3‘-diamino-<i>N</i>-methyldipropylamine\nwere synthesized and characterized. The crystal structures of <b>1</b>, <b>7</b>, and <b>8</b> were solved. For complex <b>1</b>, the trinuclear\nentities are linked by hydrogen bonds forming a one-dimensional system, and for complex <b>8</b>, the presence of van\nder Waals interactions gives a one-dimensional system, too. For complex <b>7</b>, the trinuclear entities are self-assembled\nby azido ligands, given a hexanuclear system; each of these hexanuclear entities are self-assembled through two\n[Na(O)<sub>3</sub>(H<sub>2</sub>O)<sub>3</sub>] octahedral-sharing one-edge entities, given a one-dimensional system. The magnetic behavior of\ncomplexes <b>2</b>−<b>7 </b>was investigated by variable-temperature magnetic susceptibility measurements. Complexes <b>2</b>−<b>6\n</b>exhibit the minimum characteristic of this kind of polymetallic species with an irregular spin state structure. The <i>J\n</i>value through the oxamato bridge varied between −88 cm<sup>-1</sup> (for <b>6</b>) and −111.2 cm<sup>-1</sup> (for <b>5</b>). For complex <b>7</b>, the\nvalues obtained were <i>J</i><sub>1</sub> = −101.7 cm<sup>-1</sup> (through the oxamato ligand) and <i>J</i><sub>2</sub> = −3.2 cm<sup>-1</sup> (through the azido\nligand).
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