Abstract
Diethyl-2,2′-bipyridine-3,3′-dicarboxylate (3 or L) reacts with RuCl3 · 3H2O to give cis-(Cl)-[Ru(L)2Cl2] · H2O (4) and structure of the complex was determined by spectral (IR, 1H-NMR), and mass spectroscopic data, elemental analyses and X-ray crystallography. The structure is solved in triclinic, space group p-1 with a = 10.658 (2), b = 12.446 (3), c = 14.186 (5) Å, α = 104.856 (3), β = 108.704 (3), γ = 94.973 (2)°, V = 1693.2 (8) Å3, Z = 2 with final R = 0.012. The geometry of the complex is shown to be a distorted octahedral with four nitrogens of two 2,2′-bipyridyl ligands in two different planes with Ru–N distance as 2.021 (2)−2.071 (3) Å. The cis-position is occupied by two chloride atoms with Ru–Cl distance as 2.4156 (12) and 2.4167 (13) Å. The trans-axial Cl2–Ru1–N and Cl1–Ru1–N4 angles are respectively, 172.42 (7) and 174.12 (7)°. A weak hydrogen bonding is observed between the two chlorides and hydrogens of neighbouring molecule [C–H···Cl distance as 2.72, 2.77 (4) Å]. A second type of weak hydrogen bonding is also observed between the oxygens of carboxylate groups and hydrogens of a neighbouring molecule [C–H···O distance as 2.53, 2.56 and 2.34 (4) Å].
Graphical Abstract
The structure of anti-tubercular precursor complexes, cis-(chloro)-[N,N′-bis-(diethyl-2,2′-bipyridine-3,3′-dicarboxylate)]ruthenium(II) monohydrate is solved by single crystal X-ray diffraction analysis which reveals geometry of the complex to be a distorted octahedral with four nitrogens of two 2,2′-bipyridyl ligands in two different planes. The cis-position is occupied by two chloride atoms.
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References
Cole Hamilton DJ (1980) J Chem Soc Chem Commun 1213. doi:10.1039/c39800001213
Choudhury D, Cole Hamilton DJ (1982) J Chem Soc Dalton Trans 1985
Tanaka K, Morimoto M, Tanaka T (1983) Chem Lett 901. doi:10.1246/cl.1983.901
Ishida M, Tanaka K, Morimoto M, Tanaka T (1986) Organometallics 5724
Haasnoot JG, Hinrichs W, Weir O, Vos JG (1986) Inorg Chem 25:1440. doi:10.1021/ic00243a018
Che C-M, Leung W-H (1987) J Chem Soc Chem Commun 1376. doi:10.1039/c39870001376
Goldstein AS, Drago RS (1991) J Chem Soc Chem Commun 21. doi:10.1039/c39910000021
Collomb-Dunand-Sautier N, Deronzier A, Ziessel R (1994) Inorg Chem 33:2961. doi:10.1021/ic00091a040
Ishida M, Fujicki K, Omba T, Ohkubo K, Tanaka K, Terada T, Tanaka T (1990) J Chem Soc Dalton Trans 2155. doi:10.1039/dt9900002155
Ishida M, Tanaka K, Tanaka T (1987) Organometallics 6:181. doi:10.1021/om00144a033
Morgan JL, Buck DP, Turley AG, Collins JG, Keene FR (2006) Inorg Chim Acta 3(359):888. doi:10.1016/j.ica.2005.06.036
Wu B-Y, Gao Li-H, Duan Z-M, Wang K-Z (2005) J Inorg Biochem 3(99):1685. doi:10.1016/j.jinorgbio.2005.05.012
Liu Y-J, Chao H, Tan L-F, Yuan Y-X, Wei W, Ji L-N (2005) J Inorg Biochem 2(99):530. doi:10.1016/j.jinorgbio.2004.10.030
Ju H-X, Ye Y-K, Zha J-H, Zhu Y-L (2003) Anal Biochem 2(313):255. doi:10.1016/S0003-2697(02)00625-5
Mazumder UK, Gupta M, Karki SS, Bhattacharya S, Rathinasamy S, Sivakumar T (2005) Bioorg Med Chem 13(20):5766. doi:10.1016/j.bmc.2005.05.047
Ben Hadda T, Sam N, Le Bozec H, Dixneuf PH (1999) Inorg Chem Commun 2(10):460. doi:10.1016/S1387-7003(99)00112-4
Hadda TB, Akkurt M, Baba MF, Daoudi M, Bennani B, Kerbal A, Chohan ZH (2008) Anti-tubercular Activity of Ruthenium(II) Complexes with Polypyridines. J Enzyme Inhib Med Chem 1–7. doi:10.1080/14756360802188628
Fair CK (1990) MolEN. An interactive intelligent system for crystal structure analysis. Enraf-Nonius, Delft
Spek AL (1997) HELENA. Program for the handling of CAD4-Diffractometer output SHELX(S/L). Utrecht University, Utrecht
Altomare A, Burla MC, Camalli M, Cascarano GL, Giacovazzo C, Guagliardi A, Moliterni AGG, Polidori G, Spagna R (1999) J Appl Cryst 32:115. doi:10.1107/S0021889898007717
Sheldrick GM (1997) SHELXL97. Program for the refinement of crystal structures. University of Göttingen, Germany
Fujihara T, Kobayashi A, Iwai M, Nagasawa A (2004) Acta Crystallogr E60:m1172–m1174
Eckhard IF, Summers LA (1973) Aust J Chem 26:2727
Acknowledgments
N. Sam and M. Daoudi are grateful to the ‘Projet Globale de Recherche de l’Université Mohammed Premier’ and ‘PROTARS I’ project for financial support.
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Toupet, L., Dixneuf, P.H., Akkurt, M. et al. Crystal Structure of Antitubercular Complex: cis-(chloro)-[N,N′-bis-(diethyl-2,2′-bipyridine-3,3′-dicarboxylate)]ruthenium(II) Monohydrate. J Chem Crystallogr 39, 423–427 (2009). https://doi.org/10.1007/s10870-008-9495-7
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DOI: https://doi.org/10.1007/s10870-008-9495-7