Tris(1,10-phenanthroline-κ2N,N′)iron(II) μ-oxido-bis[trichloridoferrate(III)] ethanol hemisolvate

Li, Z.-X.; Yu, M.-M.; Zhang, Y.-N.; Wei, L.-H.

doi:10.1107/S1600536808035897

Volume 64
Part 12
Page m1514
December 2008

Received 13 October 2008
Accepted 1 November 2008
Online 8 November 2008

Key indicators
Single-crystal X-ray study
T = 294 K
Mean (C-C) = 0.011 Å
Disorder in solvent or counterion
R = 0.064
wR = 0.212
Data-to-parameter ratio = 14.9
Details

Tris(1,10-phenanthroline-²N,N')iron(II) -oxido-bis[trichloridoferrate(III)] ethanol hemisolvate

Zhan-Xian Li,^a Ming-Ming Yu,^a Yu-Na Zhang ^a and Liu-He Wei ^a ^*

^aDepartment of Chemistry, Zhengzhou University, Zhengzhou 450001, People's Republic of China
Correspondence e-mail: weiliuhe@zzu.edu.cn

The title compound, [Fe(C₁₂H₈N₂)₃][Fe₂Cl₆O]·0.5CH₃CH₂OH, consists of one [Fe(phen)₃]²⁺ cation (phen = 1,10-phenanthroline), one [Fe₂Cl₆O]^2- anion and one half-molecule of ethanol. In the cation, the Fe^II atom is coordinated by six N atoms from three phen ligands in a distorted octahedral geometry. In the bent anion, two Fe^III atoms are connected by a bridging oxide O atom [bridging angle = 160.6 (4)°], and each Fe^III atom is also coordinated by three Cl atoms, completing a distorted tetrahedral geometry.

Related literature

For general background, see: Hwang & Ha (2006); Potocnák et al. (2002); Zhou & Guo (2007). For a related structure, see: Aparici Plaza et al. (2007).

Experimental

Crystal data

[Fe(C₁₂H₈N₂)₃][Fe₂Cl₆O]·0.5C₂H₆O
M_r = 959.89
Monoclinic, P 2₁ /c
a = 15.3536 (18) Å
b = 13.1857 (16) Å
c = 20.897 (2) Å
= 94.701 (2)°
V = 4216.4 (8) Å³
Z = 4
Mo K radiation
= 1.44 mm^-1
T = 294 (2) K
0.55 × 0.47 × 0.42 mm

Data collection

Bruker SMART 1K CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.452, T_max = 0.544
20409 measured reflections
7434 independent reflections
4248 reflections with I > 2(I)
R_int = 0.058

Refinement

R[F² > 2(F²)] = 0.064
wR(F²) = 0.212
S = 1.02
7434 reflections
498 parameters
3 restraints
H-atom parameters constrained
_max = 0.84 e Å^-3
_min = -0.39 e Å^-3

Table 1
Selected bond lengths (Å)

Fe1-N4	1.958 (6)
Fe1-N2	1.970 (5)
Fe1-N6	1.979 (5)
Fe1-N1	1.980 (5)
Fe1-N3	1.982 (5)
Fe1-N5	1.985 (5)
Fe2-O1	1.735 (5)
Fe2-Cl4	2.204 (3)
Fe2-Cl6	2.223 (2)
Fe2-Cl5	2.231 (2)
Fe3-O1	1.756 (5)
Fe3-Cl2	2.213 (2)
Fe3-Cl3	2.227 (2)
Fe3-Cl1	2.227 (2)

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2160 ).

Acknowledgements

This work was supported by the Natural Science Foundation of China (grant No. 50873093).

References

Aparici Plaza, L., Baranowska, K. & Becker, B. (2007). Acta Cryst. E63, m1537-m1539.
Bruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Hwang, I.-C. & Ha, K. (2006). Acta Cryst. E62, m376-m378.
Potocnák, I., Pohlová, M., Wagner, C. & Jäger, L. (2002). Acta Cryst. E58, m595-m596.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Zhou, D.-P. & Guo, G.-L. (2007). Acta Cryst. E63, m1122-m1124.

metal-organic compounds

Tris(1,10-phenanthroline-2N,N')iron(II) -oxido-bis[trichloridoferrate(III)] ethanol hemisolvate