Hostname: page-component-cd9895bd7-dk4vv Total loading time: 0 Render date: 2024-12-28T19:48:39.120Z Has data issue: false hasContentIssue false
  • English
  • Français

Crystal and molecular structures of the organometallic species [Rh2(bim)2(cod)2]Cl2∙2H2O [bim=bis-(1-imidazolyl)methane; cod=1, 5-cyclooctadiene]

Published online by Cambridge University Press:  01 March 2012

Norberto Masciocchi ,
Alessandro Figini Albisetti ,
Angelo Sironi ,
Claudio Pettinari  and
Alessandro Marinelli
Norberto Masciocchi
Affiliation:
Dipartimento di Scienze Chimiche e Ambientali, Università dell’Insubria, via Valleggio 11, 22100 Como, Italy
Alessandro Figini Albisetti
Affiliation:
Dipartimento di Chimica Strutturale e Stereochimica Inorganica, Università di Milano, via Venezian 21, 20133 Milano, Italy
Angelo Sironi
Affiliation:
Dipartimento di Chimica Strutturale e Stereochimica Inorganica, Università di Milano, via Venezian 21, 20133 Milano, Italy
Claudio Pettinari
Affiliation:
Dipartimento di Chimica, Università di Camerino, via S.Agostino 1, 62032 Camerino (MC), Italy
Alessandro Marinelli
Affiliation:
Dipartimento di Chimica, Università di Camerino, via S.Agostino 1, 62032 Camerino (MC), Italy
Get access Rights & Permissions [Opens in a new window]

Abstract

The synthesis and X-ray powder diffraction data for the organometallic [Rh2(bim)2(cod)2]Cl2∙2H2O species are reported. Its crystal and molecular structures were determined by simulated annealing and full-profile Rietveld refinement methods. [Rh2(bim)2(cod)2]Cl2∙2H2O was found to crystallize in the orthorhombic Cmca space group. The lattice parameters were determined to be a=21.3574(6), b=10.7764(3), c=14.2795(4) Å, V=3286.5(2) Å3, for Z=4. The crystal structure was found to contain dimeric [Rh2(bim)2(cod)2]2+ cations, in which the bim ligands bridge Rh(cod) fragments with an intermetallic separation of ca. 8.90 Å. The crystal structure is completed by chloride ions and hydrogen-bonded water molecules, situated in the small cavities of the large cation substructure. The conformation of the bim ligand, lying on a crystallographic mirror plane, is rigorously Cs.

Keywords

powder diffractionrhodiumcyclooctadieneRietveld refinement
Type
Technical Articles
Information
Powder Diffraction , Volume 22 , Issue 3 , September 2007 , pp. 236 - 240
Copyright
Copyright © Cambridge University Press 2007

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Bruker AXS (2005). TOPAS-R Version 3, General profile and structure analysis software for powder diffraction data (computer software), Karlsruhe, Germany.Google Scholar
Cingolani, A., Galli, S., Masciocchi, N., Pandolfo, L. Pettinari, C., and Sironi, A. (2005). “Sorption-desorption behavior of bispyrazolato-copper(II) 1D coordination polymers, ” J. Am. Chem. Soc.JACSAT 127, 6144–6145.CrossRefGoogle ScholarPubMed
Coelho, A. A. (2000). “Whole-profile structure solution from powder diffraction data using simulated annealing, ” J. Appl. Crystallogr.JACGAR 22, 899–908.CrossRefGoogle Scholar
Cui, G. H., Li, J. H., Tian, J. L., Bu, X. H., and Batten, S. (2005). “Multidimensional metal-organic frameworks constructed from flexible bis(imidazole) ligands, ” Cryst. Growth Des.CGDEFU 5, 1775–1780.CrossRefGoogle Scholar
Cui, G.-H., Dong, G.-Y., and Ribas, J. (2006). “catena-Poly[[bis(isothiocyanato-κ N) copper(II)] - bis(μ-1, 1′-methylenedi-1H-imidazole-κ N 3:κ N 3)], ” Acta Crystallogr., Sect. E: Struct. Rep. OnlineACSEBH 62, m523–m525.Google Scholar
Dong, G.-Y., Cui, G.-H., and Wang, S.-C. (2006). “μ-1, 1′ -Methylenedi-1H-imidazole-κ 2N 3:N 3′ bis[aqua(pyridine-2, 6-dicarboxylato)copper(II)] tetrahydrate, ” Acta Crystallogr., Sect. E: Struct. Rep. OnlineACSEBH 62, m606–m607.Google Scholar
Hwang, I. C., Chandran, R. P., Singh, J., Khandelwal, M, Thangadurai, D., Lee, J. W., Chang, J. A., and Kim, K. S. (2006). “Organic-inorganic hybrid compounds of Li with benzimidazole derivatives: Li ion binding study and topochemical properties, ” Inorg. Chem.INOCAJ 45, 8062–8069.CrossRefGoogle Scholar
Jin, C. M., Lu, H., Wu, L. W., and Huang, J. (2006). “A new infinite inorganic [n]catenane from silver and bis(2-methylimidazolyl)methane ligand, ” Chem. Commun. (Cambridge)CHCOFS 2006, 5039–5041.CrossRefGoogle Scholar
Kirkpatrick, S., Gelatt, C. D., and Vecchi, M. P. (1983). “Optimization by simulated annealing, ” ScienceSCIEAS10.1126/science.220.4598.671 220, 671–680.CrossRefGoogle ScholarPubMed
Li, J. (2006). “Bis(imidazol-l-yl)methane, ” Acta Crystallogr., Sect. E: Struct. Rep. OnlineACSEBH 62, ol798–ol799.Google Scholar
Lorenzotti, A., Cecchi, P., Pettinari, C., Leonesi, D., and Bonati, F. (1991). “Adduct formation or metalation from 1, 2-bis(N-pyrazolyl)ethane and mercury(II) derivatives, ” Gazz. Chim. Ital.GCITA9 121, 89–91.Google Scholar
Masciocchi, N., Ardizzoia, G. A., La Monica, G., Maspero, A., and Sironi, A. (1998). “The unique formation of a crystal phase containing cyclic oligomers and helical polymers of the same monomeric fragment, ” Angew. Chem., Int. Ed.ACIEF5 37, 3366–3369.Google Scholar
Masciocchi, N., Bruni, S., Cariati, E., Cariati, F., Galli, S., and Sironi, A. (2001). “Extended polymorphism in copper(II) imidazolate polymers: a spectroscopic and XRPD structural study, ” Inorg. Chem.INOCAJ 40, 5897–5905.CrossRefGoogle ScholarPubMed
Masciocchi, N., Galli, S., and Sironi, A. (2005). “X-ray powder diffraction characterization of polymeric metal diazolates, ” Comments Inorg. Chem.COICDZ 26, 1–37.Google Scholar
Masciocchi, N., Galli, S.,Figini, Albisetti A., Sironi, A., Di Nicola, C., and Pettinari, C. (2006). “Polímeros organometálicos de estaño con ligandos nitrogenados puente. Estudios estructurales de difracción de polvo, ” QIES-06, 12a Reunión Científica Plenaria de Química Inorgánica, Barcelona, Spain.Google Scholar
Masciocchi, N., Galli, S., Figini Albisetti, A., Sironi, A., Di Nicola, C., and Pettinari, C. (2007). “Structural and thermodiffractometric analysis of coordination polymers. Part II: zinc and cadmium derivatives of the bim ligand [bim=bis-(1 -imidazolyl)-methane], ” submittedGoogle Scholar
Pettinari, C., Marchetti, F., Lorenzotti, A., Gioia, Lobbia G., Leonesi, D., and Cingolani, A. (1994a). “Zinc, cadmium and mercury derivatives of 1, 2-bis(3, 5-dimethylpyrazol-l-yl)ethane, ” Gazz. Chim. Ital.GCITA9 124, 51–55.Google Scholar
Pettinari, C., Santini, C., Leonesi, D., and Cecchi, P. (1994b). “Synthesis and characterization of some zinc, cadmium and mercury(II) derivatives of bis(4-methylpyrazol-1-yl)alkanes, ” PolyhedronPLYHDE 13, 1553–1562.CrossRefGoogle Scholar