Advanced
A Linear Trinuclear Cobalt(II) Complex with Acetate Bridging Ligang:Hexakisacetatodiphenanthrolinetricobalt(II)
A Linear Trinuclear Cobalt(II) Complex with Acetate Bridging Ligang:Hexakisacetatodiphenanthrolinetricobalt(II)
Journal of the Korean Chemical Society. 2003. Dec, 47(6): 667-670
Copyright © 2003, The Korean Chemical Society
  • Received : September 15, 2003
  • Published : December 20, 2003
Download
PDF
e-PUB
PubReader
PPT
Export by style
Article
Author
Metrics
Cited by
TagCloud
About the Authors
본권 구
욱 이

Abstract
Keywords
PPT Slide
Lager Image
PPT Slide
Lager Image
PPT Slide
Lager Image
EXPERIMENTAL
To a stirred solution of Co(O 2 CCH 3 ) 2 ·4H 2 O (2.04 mmol, 0.508 g) in 20 ml of DMF was added a solution of 1,10-phenanthroline (1.36 mmol, 0.27 g) in 10 ml of DMF. The resulting solution was allowed to stir for 10 min. and then pink solid began to precipitate. After stirring for further 10 min, the reaction mixture was filtered off and washed with several aliquots of DMF, followed by several aliquots of acetone, and then diethyl ether. The solid was dried in vacuo. Data for (1): Yield 0.38 g (62%). mp=297 ℃ (dec.). λ M (mmho cm 2 mol -1 , in DMSO at 25 ℃): 28. Anal. Calc. for C 36 H 34 N 4 O 12 Co 3 : C, 48.50; H, 3.84; N, 6.28; Co, 20.95. Found: C, 48.07; H, 3.86; N, 6.39; Co, 20.60. FAB-MS, m/z: [M+2H] + , 893; [M-OAc+H] + , 833; [M-phen+ 2H] + , 713. FT-IR (KBr, cm -1 ): 3069, 2923, 1592 ( v asym. COO - ), 1515, 1419 ( v sym. COO - ), 1339, 1018, 849, 728, 669.
Pink crystals of (1) suitable for X-ray diffraction study were grown by diffusive mixing of DMF solutions of 1,10-phenanthroline and Co(O 2 CCH 3 ) 2 ·4H 2 O.
Crystal Structure Determination of 1 . X-ray quality crystals were obtained as described above. A crystal size 0.50×0.25×0.13 mm was used for data collection on a STOE STAD14 four-circlediffractometer 11 with graphite-monochromatized Mo- Kα radiation (λ=0.71069 Å) at room temperature. Cell parameters and orientation matrix for data collection were determined by least-squares refinement, using 34 reflections in the range of 9.5°<θ< 10.5°. Data were collected using the ω-2θ scan technique. Three standard reflections monitored every 1h and decayed 4.4% over the course of the data collection. The intensity data were corrected for Lorentz and polarization effects. The structure was solved by direct method 12 and refined by fullmatrix least-squares methods. 13 All non-hydrogen atoms were refined anisotropically. The positions of hydrogen atoms were idealized ( d (C-H)=0.93 or 0.96 Å) and included in the calculations of the structure factors as fixed contributions. Each hydrogen atom was assigned an isotropic thermal parameter of 1.2 times that of attached atom. The data collection and structure solution parameters are listed in 1 , together with standard discrepancy discrepancy indicies R and wR .
Crystal Data and Structure Refinement for Compound 1
PPT Slide
Lager Image
aw= 1/[σ2(Fo2)+(0.0451P)2+17.2917P] where P=(Fo2+2Fc2)/3|
Selected geometric parameters (Å, º).
PPT Slide
Lager Image
Symmetry transformations of i: 1-x, y, -z+1/2
This work was partially supported by the 2003 research fund of Catholic University of Daegu, Korea.
Supporting information available . Crystallographic data for the structure reported here have been deposited with the Cambridge Crystallographic Data Centre (Deposition No. CCDC-216817). The data can be obtained free of charge via www.ccdc.cam.ac.uk/conts/retrieving.html (or from the CCDC, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336033; e-mail: deposit@ccdc.cam.ac.uk ).
References
Christmas C. , Vincent J. B. , Chang H. R. , Huffman J. C. , Christou G. , Hendrickson D. N 1988 J. Am. Chem. Soc. 10 823 -    DOI : 10.1021/ja00211a022
Adams H. , Clunas S. , Fenton D. E. , Gregson T. J. , McHugh P. E. , Spey S. E. 2002 Inorg. Chem. Comm. 5 211 -    DOI : 10.1016/S1387-7003(02)00327-1
Pal S. , Olmstead M. A. , Armstrong W. H. 1995 Inorg. Chem. 34 4708 -    DOI : 10.1021/ic00123a002
Birkelbach F. , Florke U. , Haupt H.-J. , Butzlaff C. , Trautwein A. X. , Wieghardt K. , Chaudhuri P. 1998 Inorg. Chem. 37 2000 -    DOI : 10.1021/ic970362g
Nakamoto T. , Wang Q. , Miyazaki Y. , Sorai M 2002 Polyhedron 21 1299 -    DOI : 10.1016/S0277-5387(02)00976-2
Beattie J. K. , Klepetko J. A. , Masters A. F. , Turner P. 2003 Polyhedron 22 947 -    DOI : 10.1016/S0277-5387(02)01437-7
Rardin R. L. , Poganiuch P. , Bino A. , Goldberg D. P. , Tolman W. B. , Liu S. , Lippard S. J. 1992 J. Am. Chem. Soc. 114 5240 -    DOI : 10.1021/ja00039a041
Billson T. S. , Crane J. D. , Fox O. D. , Heath S. L. 2000 Inorg. Chem. Comm. 3 718 -    DOI : 10.1016/S1387-7003(00)00171-4
Perlepes S. P. , Libby E. , Streib W. E. , Folting K. , Christou G. 1992 Polyhedron 11 923 -    DOI : 10.1016/S0277-5387(00)83342-2
Clegg W. , Little I. R. , Straughan B. P. 1988 Inorg. Chem. 27 1916 -    DOI : 10.1021/ic00284a020
STOE (1996) STADI4, X-RED, & X-SHAPE. X-Ray structure evalutation package. STOE-Cie Gmbh, Hilpertstrase 10, D64295 Darmstadt Germany
Sheldrick G. M. 1990 Acta Cryst. A46 467 -    DOI : 10.1107/S0108767390000277
Sheldrick G. M. (1997) SHELXS97-2 and SHELXL97-2. University of Göttingen Göttingen, Germany
Farrugia L. J. 1997 J. Appl. Cryst. 30 565 -    DOI : 10.1107/S0021889897003117
Heinze K. , Huttner G. , Zsolnai L. , Schober P. 1997 Inorg. Chem. 36 5457 -    DOI : 10.1021/ic9705352