electronic reprint
Acta Crystallographica Section E
Structure Reports
Online
ISSN 1600-5368
Editors: W. Clegg and D. G. Watson
A cofacial binuclear copper(II) complex with a bridging 1,4-dithiane
ligand
Sylvester Burton, Frank R. Fronczek and Andrew W. Maverick
Copyright © International Union of Crystallography
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Acta Cryst. (2007). E63, m1977–m1978
Burton et al.
¯
[Cu2 (C22 H22 O4 )(C4 H8 S2 )]
metal-organic compounds
Acta Crystallographica Section E
Structure Reports
Online
ISSN 1600-5368
A cofacial binuclear copper(II) complex
with a bridging 1,4-dithiane ligand
Sylvester Burton,‡ Frank R. Fronczek* and Andrew W.
Maverick
Department of Chemistry, Louisiana State University, Baton Rouge, LA 70803-1804,
USA
Correspondence e-mail: [email protected]
Received 30 May 2007; accepted 15 June 2007
Key indicators: single-crystal X-ray study; T = 120 K; mean (C–C) = 0.005 Å;
R factor = 0.050; wR factor = 0.110; data-to-parameter ratio = 12.7.
The molecule of (-1,4-dithiane-2S:S0 )bis{-3,30 -[naphthalene-2,7-diylbis(methylene)]bis(pentane-2,4-dionato)-4O,O0 :O00 ,O000 }dicopper(II), [Cu2(C22H22O4)(C4H8S2)], lies on an
inversion center, with a Cu Cu distance of 8.130 (1) Å.
The CuII centers have square-pyramidal coordination
geometry, with Cu—O distances in the range 1.905 (2)–
1.925 (2) Å and a Cu—S distance of 2.8088 (10) Å. The host
binuclear complex is distorted from a rectangular shape. The
inversion symmetry of the molecule requires that the two
coordination planes be parallel. However, they are ‘slipped’:
the normals to the two coordination planes at the Cu atoms
are 1.865 (1) Å apart. Another measure of this ‘slipping’ is
provided by the four CH2 groups, whose C atoms form a
parallelogram with interior angles of 87.2 (3) and 92.8 (3) .
The two chelate rings tilt differently from the coordination
plane, with one Cu atom lying only 0.0131 (5) Å out of one
C3O2 mean plane, but 0.4416 (5) Å out of the other. Those two
chelate planes form a dihedral angle of 11.2 (4) . This
relatively large deviation is believed to be due to the large
size of the 1,4-dithiane guest.
Related literature
Cu2(NBA)2 {NBAH2 is 3,30 -[naphthalene-2,7-diylbis(methylene)]bis(pentane-2,4-dione)} forms a crystalline solvate with
two CHCl3 molecules, in which the Cu Cu distance is
7.349 (1) Å at room temperature (Maverick et al., 1986) and
7.298 (1) Å at 100 K (Burton et al., 2002). With -Dabco (1,4diazabicyclo[2.2.2]octane), the Cu Cu distance is 7.403 (4) Å
(Maverick et al., 1986), with -2,5-dimethylpyrazine it is
7.559 (2) and 7.596 (2) Å (Maverick et al., 1990), and with -2methylpyrazine it is 7.4801 (8) Å (Maverick et al., 2001). For
related literature, see: Martin et al. (1959).
‡ Current address: Department of Chemistry, Southern University, Baton
Rouge, LA 70813, USA.
Acta Cryst. (2007). E63, m1977–m1978
Experimental
Crystal data
[Cu2(C22H22O4)(C4H8S2)]
Mr = 948.10
Monoclinic, P21 =c
a = 7.758 (2) Å
b = 28.981 (7) Å
c = 9.640 (3) Å
= 97.840 (15)
V = 2147.1 (10) Å3
Z=2
Mo K radiation
= 1.14 mm1
T = 120 K
0.15 0.08 0.07 mm
Data collection
Nonius KappaCCD diffractometer
with an Oxford Cryosystems
Cryostream cooler
Absorption correction: multi-scan
(SCALEPACK; Otwinowski &
Minor, 1997)
Tmin = 0.878, Tmax = 0.924
10982 measured reflections
3491 independent reflections
2598 reflections with I > 2(I)
Rint = 0.046
Refinement
R[F 2 > 2(F 2)] = 0.050
wR(F 2) = 0.110
S = 1.06
3491 reflections
275 parameters
H-atom parameters constrained
max = 0.30 e Å3
min = 0.44 e Å3
Data collection: COLLECT (Nonius, 2000); cell refinement:
SCALEPACK (Otwinowski & Minor, 1997); data reduction:
SCALEPACK and DENZO (Otwinowski & Minor, 1997);
program(s) used to solve structure: SIR97 (Altomare et al., 1999);
program(s) used to refine structure: SHELXL97 (Sheldrick, 1997);
molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
This research was supported by the Petroleum Research
Fund (American Chemical Society) and by the US Department of Energy. The purchase of the diffractometer was made
possible by grant No. LEQSF(1999–2000)-ENH-TR-13,
administered by the Louisiana Board of Regents.
Supplementary data and figures for this paper are available from the
IUCr electronic archives (Reference: FJ2036).
References
Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C.,
Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J.
Appl. Cryst. 32, 115–119.
Burton, S., Maverick, A. W. & Fronczek, F. R. (2002). Private communication
(refcode FAGKED01). CCDC, Union Road, Cambridge, England.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
doi:10.1107/S1600536807029583
electronic reprint
# 2007 International Union of Crystallography
m1977
metal-organic compounds
Martin, D. F., Fernelius, W. C. & Shamma, M. (1959). J. Am. Chem. Soc. 81,
130–133.
Maverick, A. W., Billodeaux, D. R., Ivie, M. L., Fronczek, F. R. & Maverick, E.
F. (2001). J. Incl. Phenom. Macrocyclic Chem. 39, 19–26.
Maverick, A. W., Buckingham, S. C., Yao, Q., Bradbury, J. R. & Stanley, G. G.
(1986). J. Am. Chem. Soc. 108, 7430–7431.
m1978
Burton et al.
[Cu2(C22H22O4)(C4H8S2)]
Maverick, A. W., Ivie, M. L., Waggenspack, J. H. & Fronczek, F. R. (1990).
Inorg. Chem. 29, 2403–2409.
Nonius (2000). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M.
Sweet, pp. 307–326. New York: Academic Press.
Sheldrick, G. M. (1997). SHELXL97. University of Göttingen, Germany.
electronic reprint
Acta Cryst. (2007). E63, m1977–m1978
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