Pyrazine-assisted dimerization of molybdenum(V): Synthesis and structural characterization of novel dinuclear and tetranuclear complexes

European Journal of Inorganic Chemistry

Volumn , Issue 4, 2010, Pages 542-553

  Modec, Barbara ^a   Šala, Martin ^a   Clérac, Rodolphe ^b,c  

^a UNIVERSITY OF LJUBLJANA   (Slovenia)

^b CNRS   (France)

^c CENTRE DE RECHERCHE PAUL PASCAL   (France)

Author keywords

Magnetic properties; Molecular building units; Molybdenum; N ligands; Polynuclear complexes

Indexed keywords

CHELATION; CHLORINE COMPOUNDS; DIMERIZATION; DIMERS; MAGNETIC PROPERTIES; METAL IONS; MOLYBDENUM COMPOUNDS; POSITIVE IONS; SINGLE CRYSTALS; SYNTHESIS (CHEMICAL); X RAY CRYSTALLOGRAPHY;

BUILDING UNITS; DIMERIZATIONS; DINUCLEAR; DINUCLEAR COMPLEX; MOLECULAR BUILDING UNIT; N LIGANDS; N-LIGANDS; POLYNUCLEAR COMPLEXES; PYRAZINES; STRUCTURAL CHARACTERIZATION;

LIGANDS;

EID: 75749153216     PISSN: 14341948     EISSN: 10990682     Source Type: Journal    
DOI: 10.1002/ejic.200900758     Document Type: Article

References (88)

1. a) E. I. Stiefel, Prog. Inorg. Chem. 1977, 22, 1-223;
2. b) F. A. Cotton, J. Less-Common Met. 1974, 36, 13-22.
3. a) A. B. Blake, F. A. Cotton, J. S. Wood, J. Am. Chem. Soc. 1964, 86, 3024-3031;
4. b) F. A. Cotton, S. M. Morehouse, Inorg. Chem. 1965, 4, 1377-1381;
5. c) P. C. H. Mitchell, Q. Rev., Chem. Soc. 1966, 20, 103-118.
6. 2+ core are very rare. See for example: K. Wieghardt, M. Hahn, W. Swiridoff, J. Weiss, Angew. Chem. Int. Ed. Engl. 1983, 22, 491-492.
7. J. Bernholc, N. A. W. Holzwarth, J. Chem. Phys. 1984, 81, 3987-3995.
8. a) T. Chandler, D. L. Lichtenberger, J. H. Enemark, Inorg. Chem. 1981, 20, 75-77;
9. b) P. Rabe, J. E. Guerchais, J. Sala Pala, M. El Khalifa, J.-Y. Saillard, L. Toupet, Polyhedron 1993, 12, 1215-1225.
10. 2+ structural unit we refer to the more common syn isomer.
11. a) H. K. Chae, W. G. Klemperer, T. A. Marquart, Coord. Chem. Rev. 1993, 128, 209-224;
12. b) B. Modec, J. V. Brenčič, J. Cluster Sci. 2002, 13, 279-302.
13. a) F. A. Cotton, L. M. Daniels, C. Lin, C. A. Murillo, Chem, Commun. 1999, 841-842;
14. b) F. A. Cotton, L. M. Daniels, C. Lin, C. A. Murillo, J. Am, Chem. Soc. 1999, 121, 4538-4539;
15. c) F. A. Cotton, C. Lin, C. A. Murillo, Acc. Chem. Res. 2001, 34, 759-771;
16. d) F. A. Cotton, J. P. Donahue, C. A. Murillo, J. Am. Chem. Soc. 2003, 125, 5436-5450;
17. e) M. H. Chisholm, A. M. Macintosh, Chem. Rev. 2005, 105, 2949-2976;
18. f) J. P. Donahue, C. A. Murillo, Dalton Trans. 2008, 1547-1551.
19. a) M. H. Chisholm, K. Foiltng, J. C. Huffman, C. C. Kirkpatrick, Inorg. Chem. 1984, 23, 1021-1037;
20. b) S. Lincoln, S. A. Koch, Inorg Chem. 1986, 25, 1594-1602;
21. c) B. Modec, D. Dolenc, J. V. Brenčič, Inorg. Chim. Acta 2007, 360, 663-678.
22. a) M. F. Belicchi, G. G. Fava, C. Pelizzi, J. Chem. Soc., Dalton Trans. 1983, 65-69;
23. b) H. Kang, S. Liu, S. N. Shaikh, T. Nicholson, J. Zubieta, Inorg. Chem. 1989, 28, 920-933;
24. c) B. Modec, J.V. Brenčič, J. Zubieta, J. Chem. Soc., Dalton Trans. 2002,1500-1507;
25. d) M. D. Meienberger, B. Morgenstern, S. Stucky, K. Hegetschweiler, Eur. J. Inorg. Chem, 2008, 129-137.
26. a) R. Mattes, K. Mühlsiepen, Z. Naturforsch, Teil B 1980, 35, 265-268;
27. b) W Schirmer, U. Flörke, H. J. Haupt, Z. Anorg. AlLg. Chem. 1989, 574, 239-255;
28. c) G. S. Kim, D. A. Keszler, C. W. DeKock, Inorg. Chem. 1991, 30, 574-577;
29. d) B. Modec, J. V. Brenčič, E. M. Burkholder, J. Zubieta, Dalton Trans. 2003, 4618-4625.
30. B. Modec, J. V. Brenčič, Eur. J. Inorg. Chem. 2005, 4325-4334.
31. B. Modec, J. V Brenčič, J. Koller, Eur. J. Inorg. Chem. 2004, 1611-1620.
32. a) M. J. Manos, A. D. Keramidas, J. D. Woollins, A. M. Z. Slawin, TA. Kabanos, J. Chem. Soc., Dalton Trans. 2001, 3419-3420;
33. b) E. Dumas, C. Sassoye, K. D. Smith, S. C. Sevov, Inorg. Chem. 2002, 41, 4029-4032;
34. c) C. du Peloux, A. Dolbecq, P. Mialane, J. Marrot, F. Secheresse, Dalton Trans. 2004, 1259-1263;
35. d) M. J. Manos, J. D. Woollins, A. M. Z. Slawin, T. A. Kabanos, Angew. Chem, Int. Ed. 2002, 41, 2801-2805;
36. e) D. Liu, P. Zhang, J. Xu, S. Feng, Z. Shi, Solid State Sci. 2007, 9, 16-20;
37. f) M. Y. Lee, S.L. Wang, Chem, Mater. 1999, 11, 3588-3594.
38. M. K. Ehlert, S. J. Rettig, A. Storr, R. C. Thompson. J. Trotter, Inorg. Chem, 1993, 32, 5176-5182.
39. Selected examples from recent literature include dinuclear species: a) M. Willermann, C. Mulcahy, R. K. O. Sigel, M. M. Cerda, E. Freisinger, P. J. S. Miguel, M. Roitzsch, B. Lippert, Inorg. Chem. 2006, 45, 2093-2099;
40. b) D. Matoga, J. Szklarzewicz, J. Fawcett, Polyhedron 2005, 24, 1533-1539; trinuclear species:
41. c) X.Y. Yu, M. Maekawa, M. Kondo, S. Kitagawa, G.X. Jin, Chem. Lett. 2001, 168-169;
42. d) M. Schweiger, S. R. Seidel, A. M. Arif, P. J. Stang, Angew. Chem. Int. Ed. 2001, 40, 3467-3469; tetranuclear species:
43. e) J. K. Clegg, L. F. Lindoy, J. C. McMurtrie, D. Schilter, Dalton Trans. 2005, 857-864;
44. f) B. Manimaran, T. Rajendran, Y.L. Lu, G.H. Lee, S.M. Peng, K.L. Lu, J. Chem. Soc., Dalton Trans. 2001, 515-517;
45. g) T. Fujimura, H. Seino, M. Hidai, Y Mizobe, Inorg. Chim. Acta 2005, 358, 2449-2453;
46. h) P. H. Dinolfo, M. E. Williams, C. L. Stern, J. T. Hupp, J. Am Chem. Soc 2004, 126, 12989-13001; polymeric species:
47. i) S. Takamizawa, E. Nakata, T. Saito, T. Akatsuka, Inorg. Chem. 2005, 44, 1362-1366;
48. j) S. A. Barnett, A. J. Blake, N. R. Champness, C. Wilson, Dalton Trans. 2005, 3852-3861.
49. 2+ species: B. Modec, J. V. Brenčič, Eur. J. Inorg. Chem. 2005, 1698-1709.
50. 2O. The addition of an excess amount of pyridinium chloride (115 mg, 1.0 mmol) to the reaction mixture, described for the preparation of 1, leads to a better yield. On average, 420 mg of 1 was isolated. Yield: 79%.
51. 2+-containing products: B. Modec, Inorg. Chem. Commun. 2009, 12, 328-331.
52. D. Dolenc, B. Modec, Acta Chim. Slov. 2008, 55, 752-756.
53. S. Parsons, X. Liu, L. Yellowlees, P. Wood, Private communication to the Cambridge Structural Database, 2004. Deposition number CCDC-247870.
54. 3·2Pyz [W. M. Carmichael, D. A. Edwards, J. Inorg. Nucl. Chem. 1970, 32, 1199-1207], are not included in Table 2. The lack of X-ray structural data precludes unambiguous conclusions about the true identity of either of the two compounds.
55. D. Matoga, J. Szklarzewicz, A. Samotus, K. Lewinski, J. Chem. Soc, Dalton Trans. 2002, 3587-3592.
56. Y. Liang, M. Hong, R. Cao, D. Sun, J. Weng, Acta Crystallogr., Sect. E 2001, 57, m159-ml61.
57. a) M. M. El-Essawi, F. Weiler, K. Stahl, M. Kersting, K. Dehnicke, Z. Anorg. Allg. Chem. 1986, 542, 175-181;
58. b) A. A. Eagle, M., F. Mackay, C. G. Young, Inorg. Chem. 1991, 30, 1425-1428;
59. c) L.Z. Cai, L.I. Song, H.Y. Zeng, Z.C. Dong, G.C. Guo, J.S. Huang, Inorg. Chim, Acta 2003, 344, 61-64.
60. The sum of the corresponding van derWaals radii is 3.10 Å. Data were taken, from B. Douglas, D. McDaniel, J. Alexander, Concepts and Models of Inorganic Chemistry, 3rd ed., Wiley, New York, 1994, p. 102.
61. B. Modec, D. Dolenc, M. Kasunič, Inorg. Chem. 2008, 47, 3625-3633.
62. The distance between the centroids is given.
63. C. Janiak, J. Chem, Soc., Dalton Trans. 2000, 3885-3896.
64. B. Bleaney, K. D. Bowers, Proc. K Soc London, Ser. A 1952, 214, 451-465.
65. 4] following a published procedure (A. Bino, F. A. Cotton, Inorg. Chem. 1979, 18, 2710-2713).
66. This is supported with the CV of DMF, to which a small amount of hydrochloric acid was added, which also revealed a strong reduction wave at this potential.
67. -1) = 365 (sh., 350), 455 (20), 745 (15) nm.
68. The UV/Vis data for 2, 3 and 4, listed in the Experimental part, pertain to the species present in solution.
69. a) J. A. Craig, E. W Harlan, B. S. Snyder, M. A. Whitener, R. H. Holm, Inorg. Chem, 1989, 28, 2082-2091;
70. b) S. A. Roberts, C. G. Young, C. A. Kipke, W. E. Cleland Jr., K. Yamanouchi, M. D. Carducci, J. H. Enemark, Inorg. Chem, 1990, 29, 3650-3656.
71. The choice of DMF as a solvent was necessitated by the low solubility of 5 in other solvents.
72. a) W. E. Newton, J. L. Corbin, D. C. Bravard, J. E. Searles, J. W. McDonald, Inorg. Chem. 1974, 13, 1100-1104;
73. b) L. J. De Hayes, H. C. Faulkner, W. H. Doub, D. T. Sawyer, Inorg. Chem, 1975, 14, 2110-2116;
74. c) T. Matsuda, K. Tanaka, T. Tanaka, Inorg. Chem. 1979, 18, 454-457;
75. d) K. F. Miller, R. A. D. Wentworth, Inorg. Chem. 1980, 19, 1818-1821.
76. C. G. Barraclough, J. Lewis, R. S. Nyholm, J. Chem. Soc. 1959, 3552-3555.
77. a) W. E. Newton, J. W. McDonald, J. Less-Common Met. 1977, 54, 51-62;
78. b) S. E. Lincoln, T. M, Loehr, Inorg Chem. 1990, 29, 1907-1915;
79. c) Z Xiao, J. H. Enemark, A. G. Wedd, C. G. Young, Inorg. Chem. 1994, 33, 3438-3441;
80. d) K. R. Barnard, M. Bruck, S. Huber, C. Grittini, J. H. Enemark, R. W. Gable, A. G. Wedd, Inorg. Chem. 1997, 36, 637-649.
81. N. B. Colthup, L. H. Daly, S. E. Wiberley, Introduction to Infrared and Raman Spectroscopy, Academic Press, 1964, p. 202.
82. F. A. Cotton, D. M. L. Goodgame, M. Goodgame, A. Sacco, J. Am, Chem. Soc. 1961, 83, 4157-4161.
83. Z. Otwinowski, W Minor, Methods Enzymol. 1997, 276,307-326.
84. G. M. Sheldrick, SHELXS-97 and SHELXL-97, University of Göttingen, 1997.
85. WinGX: L. J. Farrugia, J. Appl. Crystallogr. 1999, 32, 837-838.
86. ORTEP3 for Windows: L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
87. SHELXTL, version 5.03, Siemens Analytical X-ray Instrument Division, Madison, WI, 1994.
88. CrystalMaker for Windows, version 2.15, CrystalMaker Software Ltd., Oxfordshire, UK, 2008.