Abstract
C8H10N4O6Mn, monoclinic, P21/c (no. 14), a = 5.1531(5) Å, b = 11.7052(11) Å, c = 9.4154(7) Å, β = 95.1540(10)°, V = 565.62(9) Å3, Z = 2, Rgt(F) = 0.0227, wRref(F2) = 0.0611, T = 298 K.
The crystal structure is shown in the figure. The asymmetric unit of the title structure is labelled. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.
Source of material
A mixture of 1H-pyrazole-3-carboxylic acid (0.0224 g, 0.2 mmol), Mn(OAc)2⋅4H2O (0.0245 g, 0.1 mmol), and distilled water (10 mL) was heated under reflux at 180 °C for 72 h, and then cooled to room temperature. The resulting block crystals of the title compound were obtained and washed with distilled water. The yield is ca. 55% based on Mn.
Data collection and handling.
| Crystal: | Colorless block |
| Size: | 0.38 × 0.35 × 0.30 mm |
| Wavelength: | Mo Kα radiation (0.71073 Å) |
| μ: | 1.20 mm−1 |
| Diffractometer, scan mode: | Bruker SMART, φ and ω-scans |
| 2θmax, completeness: | 25°, >99% |
| N(hkl)measured, N(hkl)unique, Rint: | 2751, 1001, 0.021 |
| Criterion for Iobs, N(hkl)gt: | Iobs > 2 σ(Iobs), 900 |
| N(param)refined: | 89 |
| Programs: | Bruker programs [1], SHELX [2, 3] |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).
| Atom | x | y | z | Uiso*/Ueq |
|---|---|---|---|---|
| Mn1 | 0.5000 | 0.5000 | 0.5000 | 0.02409(19) |
| N1 | 0.3875(3) | 0.68580(12) | 0.50559(15) | 0.0237(4) |
| N2 | 0.2305(3) | 0.76013(13) | 0.56490(16) | 0.0259(4) |
| H2 | 0.1274 | 0.7417 | 0.6281 | 0.031* |
| O1 | 0.7423(2) | 0.58436(11) | 0.35255(14) | 0.0277(3) |
| O2 | 0.8443(2) | 0.75116(11) | 0.25642(14) | 0.0296(3) |
| O3 | 0.1991(3) | 0.47570(12) | 0.32306(15) | 0.0322(3) |
| H3C | 0.0513 | 0.5061 | 0.3310 | 0.039* |
| H3D | 0.1757 | 0.4063 | 0.2984 | 0.039* |
| C1 | 0.7152(3) | 0.69161(15) | 0.33378(18) | 0.0213(4) |
| C2 | 0.5139(3) | 0.74888(15) | 0.41438(17) | 0.0211(4) |
| C3 | 0.4345(4) | 0.86296(16) | 0.4160(2) | 0.0297(4) |
| H3 | 0.4916 | 0.9232 | 0.3624 | 0.036* |
| C4 | 0.2531(4) | 0.86614(16) | 0.5143(2) | 0.0317(5) |
| H4 | 0.1626 | 0.9303 | 0.5408 | 0.038* |
Experimental details
H atoms attached to C atoms were placed in geometrically idealized positions (C—H 0.93 Å) and treated as riding on their parent atoms, with Uiso(H) = 1.2Ueq(C). The water H-atoms were located in a difference Fourier map, and were included riding on the O3 atom.
Discussion
Many mononuclear complexes containing the 1H-pyrazole-3-carboxylate ligand have been reported, for example: mononuclear cobalt(II), nickel(II) and zinc complexes with the 1H-pyrazole-3-carboxylate ligand [4, 5] , but manganese complex based on 3-carboxy-pyrazole have not been reported.
There is one half of a Mn2+ cation, one Hpca− anion and one water molecule in the asymmetric unit of the title crystal structure. The Mn2+ center shows a distorted {MnO4N2} octahedral coordination geometry with two nitrogen atoms from two separate Hpca− anions, two chelate oxygen atoms from two water molecules and two carboxylic oxygen atoms (O1, O3) from two separate Hpca− anions. In the title compound, the equatorial plane is formed by two N,O-bidentate 1H-pyrazole-3-carboxylate ligands in a trans configuration. The axial positions are occupied by two water molecules. The mononuclear complex molecules are arranged in layers parallel to the ab plane. The distances of the Mn—O and Mn—N are 2.185(2) Å and 2.253(3) Å, respectively, for the organic ligand, and 2.190(2) Å for the water ligand, which is larger than the homologous Zn complex [5]. The bond angles around the Mn2+ ion are in the range of 73.2(1)–167.5(1)°.
Acknowledgements
Authors thank the Doctor Fund of Shanxi Normal University (0505/02070298).
References
SMART and SAINT for Windows NT Software Reference Manuals, Version 5.0, Bruker Analytical X-Ray Systems, Madison, WI, USA (1997).Search in Google Scholar
Sheldrick, G. M.: SADABS, A Software for Empirical Absorption Correction, University of Göttingen: Göttingen, Germany (1997).Search in Google Scholar
SHELXL Reference Manual, version 5.1; Bruker Analytical X-Ray Systems: Madison, WI, USA (1997).Search in Google Scholar
López-Viseras, M. E.; Fernández, B.; Hilfiker, S.; González, C. S.; González, J. L.; Calahorro, A. J.; Colacio, E.; Rodríguez-Diéguez, A.: In vivo potential antidiabetic activity of a novel zinc coordination compound based on 3-carboxy-pyrazole. J. Inorg. Biochem. 131 (2014) 64–67.10.1016/j.jinorgbio.2013.10.019Search in Google Scholar PubMed
Artetxe, B.; Reinoso, S.; Felices, L. S.; Vitoria, P.; Pache, A.; Martín-Caballero, J.; Gutiérrez-Zorrill, J. M.: Functionalization of krebs-type polyoxometalates with N, O chelating ligands: A systematic study. Inorg. Chem. 54 (2015) 241–252.10.1021/ic502232vSearch in Google Scholar PubMed
©2018 Hui Wang et al., published by De Gruyter, Berlin/Boston
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.
