Crystal structure of tris(N-nitroso-N-oxyanilino-κ² O, O′) oxidoniobium(V), C₁₈H₁₅N₆O₇Nb

Abstract

CCDC no.: 1447423The crystal structure is shown in the gure. Tables 1-3 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters. Source of materialUnder atmospheric conditions, NbCl5 (0.27 g, 1 mmol) was dissolved in acetonitrile (10 mL), and treated with tetraethylammonium chloride (0.165 g, 1 mmol). The mixture was re uxed overnight at 90-100°C and the solvent was removed under vacuum. (0.2604 g, 1.68 mmol) at room temperature. The resulting mixture was stirred for 4 h, and then the volatile material was removed in vacuo. The resulting residue was washed with diethyl ether (2 × 10 mL), giving a grey solid and the solution was left to stand at 255 K for a few days after which red crystals were obtained. Atom Site Experimental detailsThe H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with C-H = 0.98 Å and Uiso(H) = 1.2Ueq(C), respectively. The highest peak (2.37 e. Å −3 ) is located 1.07 Å from O4 and the deepest hole (−0.65 e. Å −3 ) is situated 0.69 Å from Nb1. DiscussionThe ammonium salt of N-nitroso-N-phenylhydroxylamine, is a well-known analytical reagent (cupferron) and it was very popular especially for analytical separations [1, 2]. The chelate-forming derivatives of this ligand is known to form stable complexes with various metals, but only few of them have been structurally characterized [3][4][5][6][7][8][9][10][11][12]. Also some cupferrates were investigated in our group [13][14][15][16][17][18]. This study forms part of ongoing research to investigate the mechanism of the reactions of O,O′-and N,O-bidentate ligands with transition metals used in nuclear industry, such as Hf, Zr, Nb,.In the title structure the Nb atom is heptacoordinated by six oxygen atoms, of three bidentate cupferron ligands and an oxido group. The cupferrate ligand forms a ve-membered ring with a small bite angle (see the gure). The Nb-O distances are between 1.7107 (5) and 2.2267 (7) Å, and the O-Nb-O angles vary between 68.36(2)°and 158.51(2)°. All the bond distances and angles are similar to other relevant niobium(V) structures [27,28].Acknowledgements: Financial assistance from the faculty

Crystal structure of 4-(dimethylamino)pyridin-1-ium-2,5-dichloro-3,6-dioxocyclohexa-1,4-diene-1,4-bis(olate) 4-dimethylaminopyridine (2:1) water undeca-solvate

“…This analysis forms part of ongoing research to investigate the mechanism of the reactions of O,O'-and N,O-bidentate ligands with transition metals used in the nuclear industry, such as Hf, Zr, Nb, Ta and some other applications [10][11][12][13]. Previously, we have reported on the novel bidentate ligand system, chloranilic acid (caH2), a good proton donor as well as acceptor known to form complexes and co-crystals [14].…”