Synthesis, structure, and vibrational spectrum of poly-μ-pyrazine(pyrazine)(trifluoromethanesulfonato-O)copper(I)

1989 ◽  
Vol 67 (11) ◽  
pp. 1964-1969 ◽  
Author(s):  
T. Otieno ◽  
S. J. Rettig ◽  
R. C. Thompson ◽  
J. Trotter

Orange–brown crystals of composition Cu(pyz)2(CF3SO3) (pyz = pyrazine, 1,4-diazine) were obtained from methanol solutions containing Cu(CF3SO3)2 and pyrazine in approximate 1:2 mole ratio. Single crystal X-ray diffraction and infrared and Raman spectroscopy studies are reported. Crystals of the title compound are triclinic, a = 8.312(2), b = 10.903(3), c = 8.201(2) Å, α = 92.53(2), β = 113.77(2), γ = 91.40(2)°, Z = 2, space group [Formula: see text] The structure was solved by heavy atom methods and was refined by full-matrix least-squares to R = 0.035 and Rw = 0.044 for 2458 reflections with 1 ≥ 3σ(I). The compound contains chains of copper ions linked by bidentate bridging pyrazine ligands. The coordination around each copper is completed by monodentate pyrazine and trifluoromethanesulfonato groups to produce a distorted tetrahedral CuN3O chromophore. Keywords: crystal structure, μ-pyrazine copper(I) triflate polymer, vibrational spectra.

1990 ◽  
Vol 68 (10) ◽  
pp. 1901-1907 ◽  
Author(s):  
Tom Otieno ◽  
Steven J. Rettig ◽  
Robert C. Thompson ◽  
James Trotter

The complexes CuL2(CF3SO3) where L is pyrazine and 2,5-dimethylpyrazine have been prepared by the reaction of copper(I) triflate with the neutral ligand in methanol. Single crystal X-ray diffraction studies on the 2,5-Me2pyz complex are reported. Crystals of the compound are triclinic, a = 9.424(4), b = 12.103(4), c = 9.113(4) Å, α = 110.97(3), β = 117.20(3), γ = 80.26(3)°, Z = 2, space group [Formula: see text]. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.033 and Rw = 0.039 for 3326 reflections with I ≥ 3σ(1). The structure is similar to that of the pyz analogue involving chains of copper ions linked by bridging 2,5-Me2pyz ligands and monodenate triflate and terminal 2,5-Me2pyz ligands completing a distorted tetrahedral CuN3O chromophore. Mono-pyrazine and -2,5-dimethylpyrazine complexes of the type CuL(CF3SO3) were obtained by thermolysis of the corresponding bis-ligand complexes. These compounds are assigned a polymeric structure involving bridging neutral ligands and monodenate triflate groups on the basis of infrared spectroscopy studies. Electronic spectroscopy and differential scanning calorimetry studies are also reported. Keywords: pyrazine and 2,5-dimethylpyrazine complexes, copper(I) triflate, crystal structure.


1980 ◽  
Vol 33 (11) ◽  
pp. 2369 ◽  
Author(s):  
E Horn ◽  
MR Snow

The complexes Re(CO)5ClO4, Re(CO)5PO2F2, L2(CO)3Re(OClO3) and L2(CO)3Re(PO2F2), where L2 = 2,2?-bipyridyl (bpy), have been synthesized by bromide abstraction reactions from the respective rhenium carbonyl bromide precursors. The complexes were characterized by infrared and mass spectroscopy. The crystal structure of (bpy)(CO)3Re(PO2F2) has been determined from X-ray diffraction data by the heavy-atom technique. The crystals are triclinic, space group Pī with a 8.620(3), b 15.912(5), c 6.466(3) Ǻ, α 102.08(8), β 83.29(8), γ 95.08(4) and Z 2. The structure has been refined by full-matrix least-squares from 2829 reflections to R = 0.084, Rw = 0.088. The coordination geometry about rhenium is that of a distorted octahedron. Difluorophosphate coordinates to the metal centre by one of its oxygen atoms. Formation of the difluorophosphate by hydrolysis of hexafluorophosphate was shown by 31P n.m.r. spectra.


ChemInform ◽  
2009 ◽  
Vol 40 (14) ◽  
Author(s):  
B. Lazic ◽  
V. Kahlenberg ◽  
R. Kaindl ◽  
A. Kremenovic

2006 ◽  
Vol 62 (a1) ◽  
pp. s255-s255
Author(s):  
E. Boldyreva ◽  
T. Drebushchak ◽  
H. Sowa ◽  
S. Goryainov ◽  
V. Chernyshev ◽  
...  

1977 ◽  
Vol 30 (8) ◽  
pp. 1837 ◽  
Author(s):  
DPG Hamon ◽  
CL Raston ◽  
GF Taylor ◽  
JN Varghese ◽  
AH White

The crystal structure of the title compound, C12H18, has been determined at 295 K by X-ray diffraction and refined by full-matrix least squares to a residual of 0.049 for 216 ?observed? reflections; molecular geometry has been corrected for the effects of thermal motion using a rigid body approximation. Crystals are hexagonal, P63/m, a = 6.582(1), c = 11.843(3) Ǻ, Z = 2, the molecules occupying a hexagonal close- packed array.


2015 ◽  
Vol 45 (1) ◽  
pp. 715-721 ◽  
Author(s):  
Jingjing Qu ◽  
Fei Liu ◽  
Xing Wei ◽  
Changlai Yuan ◽  
Xinyu Liu ◽  
...  

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