Synthesis and Crystal Structures of Nickel(II) and Copper(II) Complexes of Meso‐3,6,6,9‐Tetramethyl‐4,8‐Diazaundecane‐2,10‐Dione Dioxime

Hoong‐Kun ‐K Fun, Tsong‐Jen ‐J Lee, Tahir Tahirov, Tian‐Huey ‐H Lu, Hung Luh, Chung‐Sun ‐S Chung

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Abstract

The nickel(II) and copper(II) complexes of meso‐3,6,6,9‐tetramethyl‐4,8‐diazaundecane‐2,10‐dione dioxime (meso‐HM‐PAO) have an intramolecular hydrogen bond between cis oxime groups. [Cu(meso‐HM‐PAO‐H)(H2O)](NCS) crystallizes in space group P21/n with a = 7.692(1), b = 12.028(2), c=20.235(3) Å, β=93.03(1)°, Z = 4 and Dc=1.46 g/cm3. The final R value for this complex was 0.034 for 2223 observed reflections with I ≥ 2.5σ (I). The Cu(II) coordination is a distorted square pyramid. The Cu(II) ion is five‐coorinated with the diazadioxime N atoms equatorial and water O atom axial. The Cu(II) is 0.12 Å from the equatorial plane towards the hydrate. The equatorial Cu‐N distances span a narrow range, 1.953(3)‐1.999(3) Å. The axial Cu‐O distance is 2.314(3) Å. The thiocyanate group is almost linear. The intramolecular O ⃛O hydrogen bond length is 2.479(4) Å. [Ni(meso‐HM‐PAO‐H)](ClO4) crystallizes in space group P21/c with a = 14.774(3), b = 12.752(3), c = 20.035(4) Å, β = 92.94(3)°, Z = 8 and Dc = 1.51 g/cm3. The final R value for the complex was 0.053 for 4794 observed reflections with F ≥ 4σ (F). The coordination about Ni(II) is a slightly distorted square plane. The Ni(II) ion is 0.0673(7) Å from the best plane of the four donor nitrogen atoms away from the perchlorate ion. The Ni‐N distances span a narrow range 1.863(4)‐1.927(4) Å. There are two molecules per asymmetrical unit resulting in eight molecules being packed in an unit cell; they are bound together by van der Waals interactions. The O‐H ⃛O bonds of these complexes give characteristic infrared absorptions as well as chemical shift of the 1H NMR signal (Ni complex).

Original languageEnglish (US)
Pages (from-to)429-435
Number of pages7
JournalJournal of the Chinese Chemical Society
Volume40
Issue number5
DOIs
StatePublished - Oct 1993

Keywords

  • Copper(II) complex
  • Hydrogen bonding
  • Nickel(II) complex
  • X‐ray structure
  • meso‐HM‐PAO

ASJC Scopus subject areas

  • Chemistry(all)

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