## Abstract The preparation of a macrocyclic diphosphine ligand 5 incorporating a binaphthyl unit and its Ni^II^ and Pd^II^ complexes, 6 and 7, is described. A complete assignment of ^1^H,‐ ^13^C‐, and ^31^P‐NMR data on the basis of 2D NMR spectroscopy (^1^H, ^1^H‐, ^13^C, ^1^H‐, ^31^P, ^1^H‐, ^31^
Synthesis, spectroscopic and structural investigation of two nickel(II) thiocyanate complexes with isonicotinic acid
✍ Scribed by Marijana Đaković; Zora Popović; Neven Smrečki-Lolić
- Publisher
- Elsevier Science
- Year
- 2008
- Tongue
- English
- Weight
- 487 KB
- Volume
- 888
- Category
- Article
- ISSN
- 0022-2860
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✦ Synopsis
Two co-crystals of trans-[Ni(NCS) 2 (H 2 O) 2 (isonicH) 2 ] with isonicotinic acid and water molecules (isonicH = isonicotinic acid, i.e., pyridine-4-carboxylic acid) were obtained by reaction of Ni(NO 3 ) 2 Á6H 2 O, isonicH and KSCN in 1:2:2 molar ratio in aqueous media. One cocrystal 2), is obtained from reaction which has been performed at room temperature while the other one, 1), was obtained by refluxing the reaction mixture for a few hours. The complexes are characterized by IR-spectroscopy and thermal and X-ray crystallographic methods. The compounds crystallize in monoclinic C2/c (1) and P2 1 /c (2) space groups and in both complexes N 4 O 2 nearly perfect octahedron around nickel is established. In both compounds molecules are linked into three-dimensional framework by O-HÁ Á ÁO, N-HÁ Á ÁO and O-HÁ Á ÁS hydrogen bonds. The co-crystallized isonicotinic acid molecules are mutually linked forming C 2 1 (7)[R 2 1 (4)] (1) and in C(7) (2) hydrogen-bond motifs along b axis. The IR and thermal data correlate with the structures of the complexes in the solid state.
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