Three complexes, (PBT)W(CO)5 (1), (3,5-Me2PBT)W(CO)5 (2) and (3,5- Pri2PBT)W(CO)5 (3) (PBT = 1H-(pyrazol-1-ylmethyl)-1,2,3-benzotriazole), were synthesized, and two of them were structurally characterized by X-ray crystallography. Complex 1 crystallizes in monoclinic with space group P21/c, a = 1.0828(2), b = 2.1655(4), c = 0.6982(1) nm, β = 93.39(3)º, V = 1.6343(6) nm3, Z = 4, Dc = 2.126 g/cm3, F(000) = 992, μ = 7.107 mm-1, S = 0.990, the final R = 0.0301 and wR = 0.0685. Complex 2 crystallizes in triclinic with space group P, a = 0.95021(8), b = 0.98391(6), c = 1.1433(1) nm, = 68.792(7), β = 77.860(8), = 75.533(6)º, V = 0.9563(1) nm3, Z = 2, Dc = 1.914 g/cm3, F(000) = 528, μ = 6.078 mm-1, S = 1.042, the final R = 0.0253 and wR = 0.0549. 1H-(Pyrazol-1-ylmethyl)-1,2,3-benzotriazoles acted as monodentate ligands through the 3-position nitrogen of the triazolyl group, and the pyrazolyl nitrogen did not participate in coordinating to the metal centers in these complexes. Their UV and fluorescence properties have been studied.
Three complexes, (PBT)W(CO)5 (1), (3,5-Me2PBT)W(CO)5 (2) and (3,5- Pri2PBT)W(CO)5 (3) (PBT = 1H-(pyrazol-1-ylmethyl)-1,2,3-benzotriazole), were synthesized, and two of them were structurally characterized by X-ray crystallography. Complex 1 crystallizes in monoclinic with space group P21/c, a = 1.0828(2), b = 2.1655(4), c = 0.6982(1) nm, β = 93.39(3)º, V = 1.6343(6) nm3, Z = 4, Dc = 2.126 g/cm3, F(000) = 992, μ = 7.107 mm-1, S = 0.990, the final R = 0.0301 and wR = 0.0685. Complex 2 crystallizes in triclinic with space group P, a = 0.95021(8), b = 0.98391(6), c = 1.1433(1) nm, = 68.792(7), β = 77.860(8), = 75.533(6)º, V = 0.9563(1) nm3, Z = 2, Dc = 1.914 g/cm3, F(000) = 528, μ = 6.078 mm-1, S = 1.042, the final R = 0.0253 and wR = 0.0549. 1H-(Pyrazol-1-ylmethyl)-1,2,3-benzotriazoles acted as monodentate ligands through the 3-position nitrogen of the triazolyl group, and the pyrazolyl nitrogen did not participate in coordinating to the metal centers in these complexes. Their UV and fluorescence properties have been studied.
杨焕;刘沛野;宋海斌;唐良富. Synthesis and Property of Tungsten Carbonyl Derivatives Based on 1H-(Pyrazol-1-ylmethyl)-1,2,3-benzotriazoles[J]. 结构化学, 2015, 34(11): 1742-1748.
YANG Huan; LIU Pei-Ye;SONG Hai-Bin;TANG Liang-Fu. Synthesis and Property of Tungsten Carbonyl Derivatives Based on 1H-(Pyrazol-1-ylmethyl)-1,2,3-benzotriazoles. CHINESE JOURNAL OF STRUCTURAL CHEMISTRY, 2015, 34(11): 1742-1748.
REFERENCES
(1)Otero, A.; Fernández-Baeza, J.; Lara-Sánchez, A.; Sánchez-Barba, L. F. Metal complexes with heteroscorpionate ligands based on the bis(pyrazol-1-yl)methane moiety: catalytic chemistry. Coord. Chem. Rev. 2013, 257, 1806–1868.
(2)Pettinari, C.; Pettinari, R. Metal derivatives of poly(pyrazolyl)alkanes II. Bis(pyrazolyl)alkanes and related systems. Coord. Chem. Rev. 2005, 249, 663–691.
(3)Ding, K.; Sun, Z. M.; Li, H. Q.; Tang, L. F. Reaction of tungsten carbonyl with bis(pyrazol-1-yl)methanes functionalized by azaaryl groups. Chin. J. Inorg. Chem. 2015, 31, 345–352.
(4)Safa, M.; Puddephatt, R. J. Chelating imidazole ligands promote oxidative addition in dimethylplatinum(II) complexes. J. Organomet. Chem. 2014, 761, 42–50.
(5)Li, H. J.; Liu, X. L.; Ding, K.; Song, H. B.; Tang, L. F. Functionalized bis(1-methylimidazol-2-yl)methane and
1-(1-methylimidazol-2-yl)methyl-3,5-dimethylpyrazole and their reactions. J. Organomet. Chem. 2014, 757, 8–13.
(6)Rumble, S. L.; Page, M. J.; Field, L. D.; Messerle, B. A. In situ catalysts for the intramolecular hydroamination of aminoalkynes–What ligand properties determine catalyst activity? Eur. J. Inorg. Chem. 2012, 2226–2231.
(7)Burns, C. T.; Jordan, R. F. Ethylene polymerization by sterically crowded palladium(II) complexes that contain bis(heterocycle)methane ligands. Organometallics 2007, 26, 6737–6749.
(8)Abuskhuna, S.; Briody, J.; McCann, M.; Devereux, M.; Kavanagh, K.; Fontecha, J. B.; McKee, V. Synthesis, structure and anti-fungal activity of dimeric Ag(I) complexes containing bis-imidazole ligands. Polyhedron 2004, 23, 1249–1255.
(9)Rüther, T.; Braussaud, N.; Cavell, K. J. Novel chromium(III) complexes containing imidazole-based chelate ligands with varying donor sets: synthesis and reactivity. Organometallics 2001, 20, 1247–1250.
(10)Braussaud, N.; Rüther, T.; Cavell, K. J.; Skelton, B. W.; White, A. H. Bridged 1-methylbisimidazoles as building blocks for mixed donor bi- and tridentate chelating ligands. Synthesis 2001, 626–632.
(11)Mautner, F. A.; Berger, C.; Dartez, M. J.; Nguyen, Q. L.; Favreau, J.; Massoud, S. S. Cadmium(II) and zinc(II) azido complexes with different nuclearity and dimensionality. Polyhedron 2014, 69, 48–54.
(12)Ojwach, S. O.; Nyamato, G. S.; Omondi, B.; Darkwa, J. Chelating (pyrazolylmethyl)pyridine ligands: coordination chemistry and binding properties with zinc(II) and cadmium(II) cations. Inorg. Chim. Acta 2012, 392, 141–147.
(13)Lu, J. T.; Chen, D. F.; Song, H. B.; Tang, L. F. Synthesis and structure of carbonyl molybdenum and tungsten derivatives containing 2-(pyrazol-1-ylmethyl)pyridine. Chin. J. Inorg. Chem. 2011, 27, 1830–1836.
(14)Ojwach, S. O.; Guzei, I. A.; Darkwa, J. (Pyrazol-1-ylmethyl)pyridine palladium complexes: synthesis, molecular structures, and activation of small molecules. J. Organomet. Chem. 2009, 694, 1393–1399.
(15)Álvarez-Boo, P.; Casas, J. S.; Castiñeiras, A.; Couce, M. D.; Freijanes, E.; Novoa, E.; Sordo, J. Dihalodimethyltin(IV) complexes of 2-(pyrazol-1-ylmethyl)pyridine. Appl. Organometal. Chem. 2003, 17, 725–729.
(16)Katritzky, A. R.; Drewniak-Dyrup, M.; Lan, X.; Brunner, F. Preparation, lithiation and transformation of N-(benzotriazol-1-ylmethyl)heterocycles. J. Heterocyclic Chem. 1989, 26, 829–836.
(17)Burckhalter, J. H.; Stephens, V. C.; Hall, L. A. R. Proof of structures derived from the hydroxy- and aminomethylation of benzotriazole. J. Am. Chem. Soc. 1952, 74, 3868–3870.
(18)Sheldrick, G. M. A short history of SHELX. Acta Crystallogr. 2008, A64, 112–122.
(19)Kraihanzel, C. S.; Cotton, F. A. Vibrational spectra and bonding in metal carbonyls. Amine-substituted group VI carbonyls in the CO stretching region. Inorg. Chem. 1963, 2, 533–540.
(20)Chen, D. F.; Pan, A. Q.; Lu, J. T.; Tang, L. F. Synthesis and related reactivity of organometallic complexes based on 1-(2-pyridylmethyl)-1,2,4-triazole. Chin. J. Inorg. Chem. 2014, 30, 1685–1693.
(21)Kelly, J. M.; Long, C.; Vos, J. G.; Haasnoot, J. G.; Vos, G. Group vi metal pentacarbonyl complexes of 1,2,4-triazoles. J. Organomet. Chem. 1981, 221, 165–176.