Diaqua­hexa-μ2-dichloro­acetato-μ3-oxido-tetra­hydro­furan­diiron(III)manganese(II)

Omid Sadeghi; Mostafa M Amini; Seik Weng Ng

doi:10.1107/S1600536809054518

. 2009 Dec 24;66(Pt 1):m101. doi: 10.1107/S1600536809054518

Diaquahexa-μ₂-dichloroacetato-μ₃-oxido-tetrahydrofurandiiron(III)manganese(II)

Omid Sadeghi ^a, Mostafa M Amini ^a, Seik Weng Ng ^b,^*

PMCID: PMC2980185 PMID: 21579910

Abstract

In the oxido-centered title compound, [Fe₂Mn(C₂HCl₂O₂)₆O(C₄H₈O)(H₂O)₂], the central O atom is linked to three metal atoms, which are themselves each linked to four dichloroacetate anions, and is in a triangular configuration. Two of the metal atoms are each coordinated by a water molecule, whereas the third is coordinated by a tetrahydrofuran molecule. In the crystal, adjacent molecules are linked by O—H⋯O and O—H⋯Cl hydrogen bonds across centers of inversion, generating a hydrogen-bonded chain along the c axis. The Mn^II atoms are disordered with respect to the Fe^III atoms, and the same metal site is occupied by 1/3Mn + 2/3Fe.

Related literature

For aquabis(tetrahydrofuran)hexakis(trifluoroacetato)(μ ₃-oxido)M(II)diiron(III) (M = copper, zinc), see: Amini et al. (2004a ▶,b ▶).

Experimental

Crystal data

[Fe₂Mn(C₂HCl₂O₂)₆O(C₄H₈O)(H₂O)₂]
M _r = 1058.34
Triclinic,
a = 9.380 (1) Å
b = 13.316 (1) Å
c = 15.432 (1) Å
α = 90.131 (1)°
β = 100.067 (1)°
γ = 97.677 (1)°
V = 1880.1 (2) Å³
Z = 2
Mo Kα radiation
μ = 2.01 mm⁻¹
T = 295 K
0.35 × 0.15 × 0.15 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.540, T _max = 0.753
15425 measured reflections
8543 independent reflections
5788 reflections with I > 2σ(I)
R _int = 0.025

Refinement

R[F ² > 2σ(F ²)] = 0.063
wR(F ²) = 0.207
S = 1.03
8543 reflections
440 parameters
35 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.64 e Å⁻³
Δρ_min = −0.90 e Å⁻³

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809054518/ci2991sup1.cif

e-66-0m101-sup1.cif^{(27.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809054518/ci2991Isup2.hkl

e-66-0m101-Isup2.hkl^{(417.8KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H11⋯O3ⁱ	0.85 (1)	2.01 (3)	2.809 (6)	158 (5)
O2w—H22⋯O8ⁱⁱ	0.85 (1)	2.06 (4)	2.821 (5)	149 (7)
O2W—H21⋯O10ⁱⁱ	0.84 (6)	2.19 (7)	2.950 (6)	150 (6)
O1W—H12⋯Cl1ⁱ	0.85 (3)	2.47 (4)	3.288 (4)	160 (6)

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Symmetry codes: (i) Inline graphic ; (ii) .

Acknowledgments

The authors thank Shahid Beheshti University and the University of Malaya for supporting this study.

supplementary crystallographic information

Experimental

Sodium bicarbonate (4.12 g, 49 mmol) was dissolved in water (50 ml) and this was mixed with dichloroacetic acid (6.19 g, 48 mmol), ferric nitrate nonahydrate (6.46 g, 16 mmol) dissolved in water (30 ml) along with manganese nitrate hexahydrate (2.36 g, 8 mmol) dissolved in water (5 ml). The mixture was stirred for 24 h. The water was removed under reduced pressure and the residue dissolved in a tetrahydrofuran and hexane mixture. The solvent was removed to give an oily residue. This was treated with hexane to remove the oil; the pure compound was obtained by recrystallization from hexane to which several drops of tetrahydrofuran were added. The brown compound melts at 435–436 K.