(Di-2-pyridyl­amine)­(methanol)sulfato­copper(II)

DeBurgomaster, P.; Zubieta, J.

doi:10.1107/S1600536810038675

Volume 66
Part 11
Pages m1350-m1351
November 2010

Received 20 September 2010
Accepted 27 September 2010
Online 2 October 2010

Key indicators
Single-crystal X-ray study
T = 90 K
Mean (C-C) = 0.005 Å
R = 0.052
wR = 0.109
Data-to-parameter ratio = 17.2
Details

(Di-2-pyridylamine)(methanol)sulfatocopper(II)

Paul DeBurgomaster ^a and Jon Zubieta ^a ^*

^aDepartment of Chemistry, Syracuse University, Syracuse, New York 13244, USA
Correspondence e-mail: jazubiet@syr.edu

The title complex, [Cu(SO₄)(C₁₀H₉N₃)(CH₃OH)], is a mononuclear species with the Cu^II ion in a Jahn-Teller-distorted `4 + 1' square-pyramidal geometry. The basal plane is defined by the pyridyl N-atom donors of the bipyridylamine (bpa) ligand and two O-atom donors of the sulfate ligand. The coordination geometry is completed by the axial coordination of a methanol O-atom donor. The axial bond length displays the usual elongation: Cu-O(axial) = 2.168 (2), Cu-O(basal) = 2.016 (2) (average) and Cu-N(basal) = 1.951 (3) Å (average). In the crystal structure, the complex molecules are linked through N-HO and O-HO hydrogen bonds into chains along [100].

Related literature

For structures of other copper-bis(2-pyridyl)amine complexes, see: Fischer & Bau (1977); Kavounis et al. (1999); Youngme et al. (2005). For solvatothermal chemistry of compounds containing copper-bis(2-pyridyl)amine subunits, see: DeBurgomaster et al. (2010). For structural chemistry of the related tridentate ligand bis(2-pyridylmethyl)amine, see: Bartholomä et al. (2010a, b,c,d,e). For copper-pyridyl subunits in the design of organic-inorganic hybrid materials, see: Armatas et al. (2005); Chesnut et al. (1999); Hagrman et al. (1999).

Experimental

Crystal data

[Cu(SO₄)(C₁₀H₉N₃)(CH₄O)]
M_r = 362.84
Monoclinic, P 2₁ /n
a = 7.1403 (10) Å
b = 10.7361 (15) Å
c = 17.798 (3) Å
= 92.185 (3)°
V = 1363.4 (3) Å³
Z = 4
Mo K radiation
= 1.78 mm^-1
T = 90 K
0.30 × 0.15 × 0.07 mm

Data collection

Bruker APEX CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1998) T_min = 0.617, T_max = 0.886
13215 measured reflections
3308 independent reflections
3119 reflections with I > 2(I)
R_int = 0.033

Refinement

R[F² > 2(F²)] = 0.052
wR(F²) = 0.109
S = 1.26
3308 reflections
192 parameters
H-atom parameters constrained
_max = 0.79 e Å^-3
_min = -0.75 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-HN2O3ⁱ	0.90	1.97	2.854 (3)	169
O5-HO5O3ⁱⁱ	0.89	1.82	2.700 (3)	168
Symmetry codes: (i) -x+1, -y+1, -z; (ii) x+1, y, z.

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalMaker (Palmer, 2006); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HG2716 ).

Acknowledgements

This work was supported by a grant from the National Science Foundation, CHE-0907787.

References

Armatas, G. N., Burkholder, E. & Zubieta, J. (2005). J. Solid State Chem. 718, 2430-2435.
Bartholomä, M., Cheung, H., Darling, K. & Zubieta, J. (2010e). Acta Cryst. E66, m1201-m1202.
Bartholomä, M., Cheung, H. & Zubieta, J. (2010a). Acta Cryst. E66, m1195-m1196.
Bartholomä, M., Cheung, H. & Zubieta, J. (2010b). Acta Cryst. E66, m1197.
Bartholomä, M., Cheung, H. & Zubieta, J. (2010c). Acta Cryst. E66, m1198.
Bartholomä, M., Cheung, H. & Zubieta, J. (2010d). Acta Cryst. E66, m1199-m1200.
Bruker (1998). SMART, SAINT and SADABS. Bruker AXS Inc. Madison, Wisconsin, USA.
Chesnut, D. J., Hagrman, D., Zapf, P. J., Hammond, R. P., LaDuca, R., Haushalter, R. C. & Zubieta, J. (1999). Coord. Chem. Rev. 190-192, 737-769.
DeBurgomaster, P., Bartholoma, M., Raffel, R., Ouellette, W., Muller, A. & Zubieta, J. (2010). Inorg. Chim. Acta, 63, 1386-1394.
Fischer, B. E. & Bau, R. (1977). J. Chem. Soc. Chem. Commun. pp. 272-273.
Hagrman, P. J., Hagrman, D. & Zubieta, J. (1999). Angew. Chem. Int. Ed. 38, 2638-2684.
Kavounis, C. A., Tzavellas, C., Cardin, C. J. & Zubavichus, Y. (1999). Struct. Chem. 10, 411-417.
Palmer, D. (2006). Crystal Maker. Crystal Maker Software Ltd, Yarnton, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Youngme, S., Phuengphai, P., Pakawatchai, C., Van Albada, G. A. & Reedijk, J. (2005). Inorg. Chim. Acta, 358, 2125-2128.

metal-organic compounds