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New X-ray powder diffraction data for heterometallic complexes with unsaturated organic ligands Cp(CO)2MnPt(μ-C=CHPh)(η2-dppm), [Cp(CO)2MnCu(μ-C=CHPh)]2(μ-Cl)2, CpMnFe2(μ3-C=CHPh)(CO)8 and η4-[Cp(CO)2MnC(CO)CHPh]Fe(CO)3(Cp=η5-C5H5;dppm=Ph2PCH2PPh2)

Published online by Cambridge University Press:  01 March 2012

Alla B. Antonova
Affiliation:
Institute of Chemistry and Chemical Technology, Siberian Branch of the Russian Academy of Sciences, K. Marx str., 42, Krasnoyarsk 660049, Russian Federation
Oleg S. Chudin
Affiliation:
Institute of Chemistry and Chemical Technology, Siberian Branch of the Russian Academy of Sciences, K. Marx str., 42, Krasnoyarsk 660049, Russian Federation
Sergei D. Kirik
Affiliation:
Institute of Chemistry and Chemical Technology, Siberian Branch of the Russian Academy of Sciences, K. Marx str., 42, Krasnoyarsk 660049, Russian Federation

Abstract

Four heterometallic carbonyl complexes: (1) Cp(CO)2MnPt(μ-C=CHPh)dppm) (2) [Cp(CO)2MnCu(μ-C=CHPh)(μ-Cl)]2, (3) CpMnFe2(μ3-C=CHPh)(CO)8, and (4) η4-[Cp(CO)2MnC(CO)CHPh]Fe(CO)3 have been studied by X-ray powder diffraction and their unit cell parameters are reported. Orthorhombic cell parameters for complex (1) are a=18.5719(14) Å, b=18.6092(14) Å, c=23.8117(18) Å, Z=8, space group Pbca. Monoclinic cell parameters found for complex (2) are a=11.5816(5) Å, b=7.9784(5) Å, c=16.7819(7) Å, β=105.460(2)°, Z=2, space group P21∕n. Orthorhombic cell parameters for complex (3) are a=13.5260(9) Å, b=15.1487(10) Å, c=10.3330(6) Å, Z=4, space group Pna21. Monoclinic cell parameters for complex (4) are a=10.3545(45) Å, b=8.0002(43) Å, c=21.8355(95) Å, β=102.89(2), Z=4, space group P21∕c. Parameters found for complexes (1–4) are in good agreement with those obtained from single crystal X-ray diffractometry.

Type
New Diffraction Data
Copyright
Copyright © Cambridge University Press 2005

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References

Andrianov, V. G., Struchkov, Yu. T., Kolobova, N. E., Antonova, A. B., and Obezyuk, N. S. (1976). “The unusual iron complex with a trimethylenemethane type ligand, (η 5-cyclopentadienyl-dicarbonylmanganese)(phenylmethylene)carbomethane iron tricarbonyl [Cp(CO)2MnC(CO)CHPh]Fe(CO)3,” J. Organomet. Chem.JORCAI10.1016/S0022-328X(00)89700-4 110, C36–C38.Google Scholar
Antonova, A. B. and Ioganson, A. A. (1989a). “Transition metal complexes of unsaturated carbenes: Synthesis, structure and reactivity,” Usp. Khim.USKHAB0042-1308 58, 11971229;Antonova, A. B. and Ioganson, A. A.Russ. Chem. Rev.RCRVAB0036-021X 58, 693710 (Engl. Transl.).CrossRefGoogle Scholar
Antonova, A. B., Kovalenko, S. V., Ioganson, A. A., Deikhina, N. A., Korniets, E. D., Struchkov, Yu. T., and Yanovskii, A. I. (1989b). “The chemistry of vinylidene complexes. VIII. Dinuclear phenylvinylidene complexes with a Mn-Rh bond. The crystal and molecular structures of (η 5−Cp)(CO)2MnRh(μ−C=CHPh)(C5H7O2)(CO),” Metalloorganich. Khim. 2, 10141023; Antonova, A. B., Kovalenko, S. V., Ioganson, A. A., Deikhina, N. A., Korniets, E. D., Struchkov, Yu. T., and Yanovskii, A. I.Organomet. Chem. in the USSR 2, 530535 (Engl. Transl.).Google Scholar
Antonova, A. B., Kovalenko, S. V., Johansson, A. A., Kornyets, E. D., Sukhina, I. A., Ginzburg, A. G., and Petrovskii, P. V. (1991). “Chemistry of vinylidene complexes. X. Synthesis and characterization of the vinylidene bridged complexes Cp(CO)2MnPt(μ−C=CHPh)(P−P) with chelating diphosphine ligands P−P=dppm, dppe or dppp at the platinum atom,” Inorg. Chim. ActaICHAA3 182, 4954.CrossRefGoogle Scholar
Antonova, A. B., Pogrebnyakov, D. A., Deykhina, N. A., Starikova, Z. A., Dolgushin, F. M., and Belokon’, A. I. (2000). “Chemistry of vinylidene complexes. 15. Transmetallation of μ-vinylidene MnPd complexes. Synthesis, X-ray diffraction analysis, and mass spectrometric study of the (η 5−C5H5)MnFe2(μ 3−C=CHPh(CO)8 cluster,” Izv. Akad. Nauk. SSR, Ser. Khi.,IASKA6523529; Antonova, A. B., Pogrebnyakov, D. A., Deykhina, N. A., Starikova, Z. A., Dolgushin, F. M., and Belokon’, A. I.Russ. Chem. Bull.RCBUEY1066-5285 49, 526532.Google Scholar
Antonova, A. B., Chudin, O. S., and Kirik, S. D. (2004). “New X-ray powder diffraction data for the series CpMn(CO)3, Cp(CO)2Mn=C=CHPh, [Cp(CO)2Mn]2(μ−C=CHPh), and [Cp(CO)2Mn]2(μ−C4Ph2) complexes (Cp=η 5−C5H5),” Powder Diffr.PODIE210.1154/1.1707038 19(2), 165171.CrossRefGoogle Scholar
Bruce, M. I. (1991). “Organometallic chemistry of vinylidene and related unsaturated carbenes,” Chem. Rev. (Washington, D.C.)CHREAY 91, 197257.CrossRefGoogle Scholar
Bruce, M. I. (1998). “Transition metal complexes containing allenylidene, cumulenylidene, and related ligands,” Chem. Rev. (Washington, D.C.)CHREAY10.1021/cr970473x 98, 27972858.CrossRefGoogle ScholarPubMed
Dolgushin, F. M., Deykhina, N. A., Pogrebnyakov, D. A., and Antonova, A. B. (2001). “The binuclear μ-phenylvinylidene complex (η 5−C5H5)(CO)(μ−CO)MnPt(μ−C=CHPPh)−(η 2−Ph2PCH2PPh2)Et 2O,” Acta Crystallograph. E57, m541–m542.Google Scholar
Ioganson, A. A., Antonova, A. B., Deikhina, N. A., Pogrebnyakov, D. A., Pavlenko, N. I., Burmakina, G. V., Rubailo, A. I., Petrovski, P. V., and Ginzburg, A. G. (1999). “Chemistry of vinylidene complexes: XIV. Synthesis and NMR and IR study of heterometallic PdMn, PdFe 2, and PdFe 3 complexes with Ph2PCH2CH2PPh2 chelating ligand,” Zh. Obshch. Khim.ZOKHA4 69, 881889; Ioganson, A. A., Antonova, A. B., Deikhina, N. A., Pogrebnyakov, D. A., Pavlenko, N. I., Burmakina, G. V., Rubailo, A. I., Petrovski, P. V., and Ginzburg, A. G.Russ. J. Gen. Chem. 69, 847855 (Engl. Transl.).Google Scholar
Kirik, S. D., Borisov, S. V., and Fedorov, V. E. (1979). “Symmetry independent algorithm for indexing of X-ray powder pattern,” Zh. Strukt. Khim.ZSTKAI 20, 359362.Google Scholar
Kolobova, N. E., Derunov, V. V., Khitrova, O. M., Lusenkova, M. A., Batsanov, A. S., Struchkov, Yu. T., and Petrovsky, P. V. (1988). “The reactions of η 2-coordinated alkynes in the presence of heteronuclear systems with Mn-Fe bonds,” Metalloorganich. Khim. 1, 400406; Kolobova, N. E., Derunov, V. V., Khitrova, O. M., Lusenkova, M. A., Batsanov, A. S., Struchkov, Yu. T., and Petrovsky, P. V.Organomet. Chem. in the USSR 1, 220223 (Engl. Transl.).Google Scholar
Pogrebnyakov, D. A., Starikova, Z. A., Pavlenko, N. I., Rubaylo, A. I., Sokolenko, V. A., Chudin, O. S., and Antonova, A. B. (2002). “Synthesis and molecular structure of the first vinylidene complex with the Mn-Cu bond [Cp(CO)(2MnCu(μ-C=CHPh)(μCl)]2,” Izv. Akad. Nauk. Ser. Khim. 12351236; Pogrebnyakov, D. A., Starikova, Z. A., Pavlenko, N. I., Rubaylo, A. I., Sokolenko, V. A., Chudin, O. S., and Antonova, A. B.Russ. Chem. Bull., Int. Ed. 51, 13391340.Google Scholar
Visser, J. W. (1969). “A fully automatic program for finding the unit cell from powder data,” J. Appl. Crystallogr.JACGAR10.1107/S0021889869006649 2, 8995.CrossRefGoogle Scholar