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Kim, Seulgi,Kang, Dong Hee,Ju, Huiyeong,Lee, Eunji,Jung, Jong Hwa,Lee, Shim Sung,Choi, Kyu Seong,Park, In-Hyeok Elsevier Sequoia [etc.] 2018 Inorganica chimica acta Vol.478 No.-
<P><B>Abstract</B></P> <P>The 20-membered N<SUB>3</SUB>O<SUB>2</SUB>-macrocycle <B>L</B> reacts with copper(II) salts (NO<SUB>3</SUB>, ClO<SUB>4</SUB>) in dichloromethane/methanol to yield unexpected isostructural chloro-bridged dinuclear bis(macrocycle) copper(II) complexes of type [<B>L</B>Cu<SUP>II</SUP>-(μ-Cl)<SUB>2</SUB>-Cu<SUP>II</SUP> <B>L</B>]X<SUB>2</SUB> (<B>1</B>: X = NO<SUB>3</SUB>, <B>2</B>: X = ClO<SUB>4</SUB>). Each complex contains two five-coordinate copper(II) ions which are bridged by two chloro-ligands, (μ-Cl)<SUB>2</SUB>, and the remaining coordination sites are completed by three nitrogens from the macrocycle. Notably, the chloro-bridging ligands are derived from the partial decomposition of the dichloromethane solvent molecules. Analogous reaction employing copper(I) chloride also afforded a similar dimer complex, [<B>L</B>Cu<SUP>II</SUP>-(μ-Cl)<SUB>2</SUB>-Cu<SUP>II</SUP> <B>L</B>]Cl<SUB>2</SUB> (<B>3</B>), suggesting such type of the chloro-bridged dicopper(II) complexes are thermodynamically stable under the reaction conditions employed in this work. Considering the τ values (0.45–0.52) for the five-coordinated copper(II) centers, complexes <B>1</B>–<B>3</B> present an intermediate geometry between square planar and trigonal bipyramidal arrangements.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Chloro-bridged bis(macrocycle) dicopper(II) complexes of an N<SUB>3</SUB>O<SUB>2</SUB>-macrocycle. </LI> <LI> Chloro-bridging ligand derived from decomposition of dichloromethane solvent. </LI> <LI> Intermediate geometry of copper(II) between SP and TBP. </LI> </UL> </P> <P><B>Graphical abstract</B></P> <P>The N<SUB>3</SUB>O<SUB>2</SUB>-macrocycle <B>L</B> reacts with copper(II) nitrate to afford an unexpected chloro-bridged dicopper(II) complex in which the chloro-ligands are derived from the decomposition of dichloromethane.</P> <P>[DISPLAY OMISSION]</P>