The crystal structure of 1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane nickel(II) bisperchlorate at 155 K

Autor: Peter A. Tregloan, Ian S. Crick, Robert W. Gable, Bernard F. Hoskins
Rok vydání: 1986
Předmět:
Zdroj: Inorganica Chimica Acta. 111:35-38
ISSN: 0020-1693
DOI: 10.1016/s0020-1693(00)82213-6
Popis: The crystal structure of the complex 1, 4, 8, 11-tetramethyl-1,4,8,11-tetraazacyclotetradecane nickel(II) bisperchlorate has been determined by an X-ray diffraction study conducted at 155 K. The monoclinic crystals have the space group Cc with a = 16.960(5), b = 36.651(8), c =18.681(5) A, β = 112.06° and Z = 20. A combination of Patterson and direct methods were used to solve the structure which was refined by a least squares procedure with R = 0.078 and Rw = 0.079, employing 7242 unique reflections with I ⩾ 2.5 σ(I). The asymmetric unit consists of five independent complex nickel cations and ten independent perchlorate anions. Of the five nickel centres, three are well resolved and of these, two exhibit a marginal tetrahedral distortion of the square planar arrangement of nitrogen atoms around each nickel centre, whilst the third possesses a slight pyramidally distorted square planar character. An average NiN bond length of 1.96 A has been observed. This study unambiguously establishes that for each of these cations, the ligand possesses the R, S, R, S conformation with all four methyl groups on the same side of the NiN4 plane.
Databáze: OpenAIRE