Abstract
Single crystal XRD is used to determine the structures of the complexes (H2TMEDA)[Mg(ptac)3]2 (1, TMEDA = Me2N(CH2)2NMe2, ptac = tBuCOCHCOCF3) and (H2TMEDA)[Mg(hfac)3](hfac) (2, hfac = CF3COCHCOCF3) at a temperature of 150 K. The crystallographic data for complex 1: a = 10.2919(3) Å, b = 10.9492(4) Å, c = 15.4159(6) Å, α = 87.117(1)°, β = 89.686(1)°, γ = 79,864(1)°, space group \(P\bar 1\) Z = 1, R = 0.0573; for complex 2: a = 12.9446(2) Å, b = 23.0035(4) Å, c = 13.1473(3) Å, β = 98.779(1)°, space group P21/n, Z = 4, R = 0.0605. The structures are ionic; the metal atom coordinates six oxygen atoms of three β-diketonate ligands. The distances Mg-O in complex 1 are in the range 2.036(2)–2.0920(19) Å; the same distances in complex 2 are in the range 2.051(2)–2.076(2) Å. The spatial packing is determined by the system of hydrogen bonds between the (H2TMEDA)2+ cations and [Mg(ptac)3]− (1) or hfac− (2) anions. A thermogravimetric study of complex 1 is carried out.
Similar content being viewed by others
References
L. F. Hatch and G. Sutherland, J. Org. Chem., 13, No. 2, 249 (1948).
Yu-W. Zhao and H. Suhr, Appl. Phys. A, 54, 451 (1992).
E. S. Vikulova, K. V. Zherikova, L. N. Zelenina, et al., Key Eng. Mat., 508, 215 (2012).
A. M. E. Raj, M. Jayachandran, and C. Sanjeeviraja, CIRP J. Manuf. Sci. Techn., 2, 93 (2010).
G. B. Hammond, D. C. Nonhebel, and Ch.-H. S. Wu, Inorg. Chem., 2, No. 1, 73 (1963).
E. Weiss, J. Kopf, T. Gardein, et al., Chem. Ber., 118, 3529 (1985).
T. Hatanpää, J. Ihanus, J. Kansikas, et al., Chem. Mater., 11, No. 7, 1846 (1999).
B. Morosin, Acta Crystallogr., 22, 315 (1967).
N. P. Kuz’mina, M. V. Ryazanov, S. I. Troyuanov, et al., Koordinats. Khim., 25, No. 6, 409 (1999).
N. B. Morozova, G. I. Zharkova, P. A. Stabnikov, et al., Synthesis and Physicochemical Study of β-Diketonates of Alkaline Earth Metals [in Russian], Novosibirsk (1989); (Preprint, Institute of Inorganic Chemistry, Siberian Division, USSR Academy of Sciences, No. 89-08).
T. Hatanpää, J. Kansikas, I. Mutikainen, et al., Inorg. Chem., 40, No. 4, 788 (2001).
M. E. Fragala, R. G. Toro, P. Rossi, et al., Chem. Mater., 21, No. 10, 2062 (2009).
I. E. Soboleva, S. I. Troyanov, and N. P. Kuz’mina, Koordinats. Khim., 22, No. 8, 579 (1996).
J. R. Babcock, D. D. Benson, A. Wang, et al., Chem. Vapor Dep., 6, No. 4, 180 (2000).
L. Wang, Yu. Yang, J. Ni, et al., Chem. Mater., 17, No. 23, 5697 (2005).
M. Maria, J. Selvakumar, V. S. Raghunathan, et al., Surf. Coat. Tech., 204, 222 (2009).
M. R. Truter and B. L. Vickery, J. Chem. Soc., Dalton Trans., 395 (1972).
M. Z. Gurevich, T. M. Sas, N. E. Mazepova, et al., Zh. Neorg. Khim., 20, 735 (1975).
M. Z. Gurevich, B. D. Stepin, and V. V. Zelentsov, Zh. Neorg. Khim., 15, 890 (1970).
S. J. Lippard, J. Am. Chem. Soc., 88, 4800 (1966).
M. Z. Gurevich, T. M. Sas, B. D. Stepin, et al., Zh. Neorg. Khim., 16, 2099 (1971).
V. P. Fadeeva and I. M. Moryakina, Izv. Sib. Otd. Akad. Nauk SSSR, Ser Khim., 6, 113 (1981).
V. P. Fadeeva, V. D. Tikhova, and O. N. Nikulicheva, J. Anal. Chem., 63, 1094 (2008).
J. S. Strukl and J. L. Walter, Spectrochim. Acta A, 27, 209 (1971).
K. Nakamoto, Infrared and Raman Spectra of Inorganic and Organic Compounds, John Wiley & Sons, Inc., New York (1997).
A. Gordon and R. Ford, The Chemist’s Companion, John Wiley & Sons, New York (1972).
T. V. Basova, V. G. Kiselev, E. S. Filatov, et al., Vib. Spectroscop., 61, 219 (2012).
NETZSCH Proteus Thermal Analysis v.4.8.1, Netzsch-Gerätebau, Bayern, Germany (2005).
Bruker: SADABS, SAINT and SHELXTL, Bruker AXS Inc., Madison, Wisconsin, USA (2008).
S. A. Gromilov and I. A. Baidina, J. Struct. Chem., 45, No. 6, 1031–1081 (2004).
K. V. Zherikova, N. V. Kuratieva, I. A. Baidina, et al., J. Struct. Chem., 51, No. 6, 769 (2010).
F. A. Villamena, M. H. Dickman, and D. L.R. Crist, Inorg. Chem., 37, No. 7, 1446 (1998).
H. Mehdi, K. Binnemans, K. Van Hecke, et al., Chem. Commun., 46, 234 (2010).
E. Yu. Fursova, O. V. Kuznetsova, V. I. Ovcharenko, et al., Izv. Akad. Nauk, Ser. Khim., 6, 1175 (2008).
S. J. Coles, J. Granifo, M. B. Hursthouse, et al., Acta Crystallogr., E57, m535 (2001).
T. S. Pochekutova, V. K. Khamylov, G. K. Fukin, et al., Polyhedron, 30, 1945 (2011).
J. A. Darr, S. R. Drake, M. B. Hursthouse, et al., J. Chem. Soc., Dalton Trans., 945 (1997).
F. Marchetti, C. Pettinari, R. Pettinari, et al., Inorg. Chem., 45, No. 7, 3074 (2006).
D. J. Otway and W. S. Rees Jr., Coord. Chem. Rev., 210, 279 (2000).
L. Huang, S. B. Turnipseed, R. C. Haltiwanger, et al., Inorg. Chem., 33, No. 4, 798 (1994).
Author information
Authors and Affiliations
Corresponding author
Additional information
Original Russian Text Copyright © 2013 by E. S. Vikulova, D. A. Piryazev, K. V. Zherikova, N. I. Alferova, N. B. Morozova, I. K. Igumenov
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 54, No. 5, pp. 845–851, September–October, 2013.
Rights and permissions
About this article
Cite this article
Vikulova, E.S., Piryazev, D.A., Zherikova, K.V. et al. Crystal structure of two complexes containing tris-(β-diketonato)magnate anion. J Struct Chem 54, 883–889 (2013). https://doi.org/10.1134/S0022476613050077
Received:
Revised:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0022476613050077