Bis(benzo)triazinethionoaza-14-crown-4 ether and its complex with CoBr2: Synthesis and crystal structures

• Published in: Russian journal of coordination chemistry Vol. 36; no. 11; pp. 838 - 843
• Main Authors: Mazur, V. M., Kolyadina, N. M., Sokol, V. I., Soro, Siaka, Sergienko, V. S., Davydov, V. V.
• Format: Journal Article
• Language: English
• Published: Dordrecht SP MAIK Nauka/Interperiodica 01-11-2010
• Subjects: Chemistry; Chemistry and Materials Science; Inorganic Chemistry; Physical Chemistry; Azacrown Ether; Triazine Ring; Macrocyclic Cavity; Crown Ether; Macrocycle
• ISSN: 1070-3284; 1608-3318
• DOI: 10.1134/S1070328410110096

8,11,14-Trioxa-22,24,25-triazatetracyclo[19.3.1.0
2,7
.0
15,20
]pentacosa-2,4,6,15(20),16,18-hexaene-23-thione (L) containing a symmetric triazinethione subunit in its macrocycle and its complex with cobalt(II) bromide of the formula [CoL
2
Br
2
] · 0.5CHCl
3
(
I
) were obtained and examined by X-ray diffraction, IR and NMR spectroscopy, and mass spectrometry. It was found that the thiourea fragment in compound L is attached to the nitrogen macrocycle through the C(2) and C(19) atoms, thus forming a substantially nonplanar six-membered triazine ring in a slightly distorted sofa conformation. Its mean-square plane is nearly perpendicular to the mean-square plane of the macrocycle (the dihedral angle between them is 83.3°). Structure L is stabilized by two bifurcate endocyclic hydrogen bonds between the N(1) atom of the triazine ring and the O(1) and O(3) atoms. The size of the macrocyclic cavity is 4.07 Å. The coordination polyhedron of the Co atom is a distorted tetrahedron made up of the sulfur atoms of two monodentate terminal molecules L and two bromine atoms.