A tetra­gonal polymorph of bis­[hydro­tris­(pyrazol-1-yl)borato]iron(II)

Ni, Z.-H.; Li, G.-L.; Ma, R.; Nie, J.

doi:10.1107/S1600536811025839

Volume 67
Part 8
Page m1033
August 2011

Received 22 June 2011
Accepted 30 June 2011
Online 6 July 2011

Key indicators
Single-crystal X-ray study
T = 123 K
Mean (C-C) = 0.003 Å
R = 0.037
wR = 0.123
Data-to-parameter ratio = 12.6
Details

A tetragonal polymorph of bis[hydrotris(pyrazol-1-yl)borato]iron(II)

Zhong-Hai Ni,^a ^* Guo-Ling Li,^a Rui Ma ^a and Jing Nie ^a

^aSchool of Chemical Engineering and Technology, China University of Mining and Technology, Xuzhou 221116, Jiangsu Province, People's Republic of China
Correspondence e-mail: nizhonghai@cumt.edu.cn

The title compound, [Fe(C₉H₁₀BN₆)₂], is a polymorph of a compound reported previously [Oliver et al. (1980). Inorg. Chem. 19, 165-168]. In the previous report, the compound crystallized in the monoclinic space group P2₁/c (Z = 4), whereas the crystal symmetry of the compound reported here is tetragonal (P4₂/ncm, Z = 4). The molecular structure is comprised of two hydrotris(1-pyrazolyl)borate ligands (Tp^-) and a central Fe^II ion, which is coordinated by six pyrazole N atoms from two two Tp^- ligands, yielding a distorted bipyramidal FeN₆ geometry. The complete molecule exhibits symmetry 2/m.

Related literature

For the crystal structure of the other polymorph measured at room temperature, see: Oliver et al. (1980). For iron(II) complexes with the Tp^- derivative ligands, see: Janiak et al. (2000); Reger et al. (2005).

Experimental

Crystal data

[Fe(C₉H₁₀BN₆)₂]
M_r = 481.93
Tetragonal, P 4₂ /n c m
a = 17.017 (3) Å
c = 7.4099 (15) Å
V = 2145.7 (7) Å³
Z = 4
Mo K radiation
= 0.74 mm^-1
T = 123 K
0.20 × 0.15 × 0.12 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) T_min = 0.867, T_max = 0.916
14091 measured reflections
1099 independent reflections
1095 reflections with I > 2(I)
R_int = 0.034

Refinement

R[F² > 2(F²)] = 0.037
wR(F²) = 0.123
S = 0.95
1099 reflections
87 parameters
H-atom parameters not refined
_max = 0.43 e Å^-3
_min = -0.39 e Å^-3

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP (Sheldrick, 1998); software used to prepare material for publication: XP.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HG5058 ).

Acknowledgements

This work was supported by the Fundamental Research Funds for the Central Universities (China University of Mining and Technology). The authors thank Professors Hui-Zhong Kou and Seik Weng Ng for helpful comments and assistance in the preparation of this paper.

References

Bruker (2001). SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2004). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Janiak, C., Temizdemir, S., Dechert, S., Deck, W., Girgsdies, F., Heinze, J., Kolm, M., Scharmann, T. G. & Zipffel, O. M. (2000). Eur. J. Inorg. Chem. pp. 1229-1236.
Oliver, J. D., Mullica, D. F., Hutchinson, B. B. & Milligan, W. O. (1980). Inorg. Chem. 19, 165-168.
Reger, D. L., Gardinier, J. R., Smith, M. D., Shahin, A. M., Long, G. J., Rebbouh, L. & Grandjean, F. (2005). Inorg. Chem. 44, 1852-1856.
Sheldrick, G. M. (1998). XP. Bruker AXS Inc., Madison, Wisconsin, USA.
Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds