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Acta Crystallogr Sect E Struct Rep Online. 2008 August 1; 64(Pt 8): m989.
Published online 2008 July 5. doi:  10.1107/S1600536808019806
PMCID: PMC2961916

Hexa-μ2-acetato-triaqua-μ3-oxido-triiron(III) nitrate acetic acid solvate

Abstract

The asymmetric unit of the title compound, [Fe3(CH3COO)6O(H2O)3]NO3·CH3COOH, consists of a hexa-μ2-acetato-triaqua-μ3-oxo-triiron(III) macrocation, a nitrate ion and an acetic acid solvent mol­ecule. In the cation, each Fe3+ ion is coordinated by four carboxyl­ate O atoms, one central bridged O atom and one water mol­ecule, resulting in distorted FeO6 octa­hedra. A network of O—H(...)O hydrogen bonds helps to establish the packing.

Related literature

For related literature, see: Fujihara et al. (1998 [triangle]); Ren et al. (2004 [triangle]); Thirumurugan & Natarajan (2004 [triangle]); Vrubel et al. (2006 [triangle]); Zhang et al. (2005 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m989-scheme1.jpg

Experimental

Crystal data

  • [Fe3(C2H3O2)6O(H2O)3]NO3·C2H4O2
  • M r = 713.92
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m989-efi1.jpg
  • a = 11.835 (3) Å
  • b = 14.755 (4) Å
  • c = 15.250 (4) Å
  • β = 90.851 (5)°
  • V = 2662.8 (12) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.71 mm−1
  • T = 296 (2) K
  • 0.18 × 0.13 × 0.10 mm

Data collection

  • Bruker SMART CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 2001 [triangle]) T min = 0.750, T max = 0.848
  • 14072 measured reflections
  • 4953 independent reflections
  • 3355 reflections with I > 2σ(I)
  • R int = 0.054

Refinement

  • R[F 2 > 2σ(F 2)] = 0.044
  • wR(F 2) = 0.106
  • S = 1.00
  • 4953 reflections
  • 378 parameters
  • 9 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.51 e Å−3
  • Δρmin = −0.41 e Å−3

Data collection: SMART (Bruker, 2001 [triangle]); cell refinement and data reduction: SAINT-Plus (Bruker, 2001 [triangle]); structure solution: SHELXS97 (Sheldrick, 2008 [triangle]); structure refinement: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: PLATON (Spek, 2003 [triangle]); software used to prepare material for publication: PLATON.

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808019806/hb2740sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808019806/hb2740Isup2.hkl

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

Acknowledgments

This work was supported by the Basic Research Foundation for Natural Science of Henan University.

supplementary crystallographic information

Comment

Transiton-metal coordination complexes based on carboxylates have been attracting chemist's interests and constitutes one of the widest families of research (Thirumurugan & Natarajan, 2004). During the past years, lots of novel carboxylates compounds have been reported (Zhang et al., 2005), in which carboxlate-supported Cr3(/m3-O) (Fujihara et al., 1998) and Fe3(/m3-O) core (Ren et al., 2004; Vrubel et al., 2006), present two large kinds of widely investigated transtion-metal complexes. Herein, we report the title compound (I).

The title compound, (I), presents a macrocation of [Fe3O(CH3COO)6(H2O)3]+, in which Fe3+ is coordinated by four oxygen atoms from four carboxylates of four acetate anions, one central bridged oxygen atom, and one water molecule. The environment of all the Fe ions are distorted octahedral geometry (Fig. 1). The three Fe atoms approximatively reside in an equilateral triangle with an oxide ion in the center [Fe3O]. The Fe—O distances range from 1.897 (2) to 2.126 (3) Å (Table 1).

In the crystal, the components are linked by O—H···O hydrogen bonds generating a three-dimensional framework (Fig. 2 and Table 2).

Experimental

Fe(NO3)3.9H2O (1 mmol, 0.404 g) was suspended in 5 ml water and 3 ml (1 mol/L) NaOH solution was added dropwise to produce a brown precipitate, then 25 ml acetic acid were added to the mixture. It was stirred under reflux for 3 h. The solution was filtered, and the filtrate was kept at the room temperature. After one weeks, xxx blocks of (I) were obtained.

Refinement

H atoms were treated as riding, with C—H distances in the range of 0.93–0.98 Å and O—H distances of 0.82 Å, and were refined as riding with Uiso(H)=1.2Ueq(Cmethylene and Cmethylidyne) and Uiso(H)=1.5Ueq(O or Cmethyl).

Figures

Fig. 1.
The molecular structure of (I), with displacement ellipsoids for the non-hydrogen atoms drawn at the 50% probability level.
Fig. 2.
Three-dimensional structure of (I), with hydrogen bonds shown as dashed lines.

Crystal data

[Fe3(C2H3O2)6O(H2O)3]NO3·C2H4O2F000 = 1460
Mr = 713.92Dx = 1.781 Mg m3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2092 reflections
a = 11.835 (3) Åθ = 2.2–23.2º
b = 14.755 (4) ŵ = 1.71 mm1
c = 15.250 (4) ÅT = 296 (2) K
β = 90.851 (5)ºBlock, yellow
V = 2662.8 (12) Å30.18 × 0.13 × 0.10 mm
Z = 4

Data collection

Bruker SMART CCD diffractometer4953 independent reflections
Radiation source: fine-focus sealed tube3355 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.054
T = 296(2) Kθmax = 25.5º
ω scansθmin = 1.7º
Absorption correction: multi-scan(SADABS; Sheldrick, 2001)h = −14→11
Tmin = 0.750, Tmax = 0.848k = −17→17
14072 measured reflectionsl = −18→17

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.044H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.106  w = 1/[σ2(Fo2) + (0.048P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
4953 reflectionsΔρmax = 0.51 e Å3
378 parametersΔρmin = −0.41 e Å3
9 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Fe10.40305 (4)0.89656 (3)0.62790 (3)0.02692 (12)
Fe20.17864 (4)0.76827 (3)0.59152 (3)0.02751 (12)
Fe30.16879 (4)0.93399 (3)0.73634 (3)0.02779 (13)
O1W0.5730 (2)0.92274 (16)0.59831 (17)0.0390 (7)
O2W0.1067 (2)0.66185 (17)0.51505 (18)0.0536 (8)
O3W0.0853 (2)1.01043 (16)0.82684 (16)0.0414 (7)
O10.4549 (2)0.76906 (16)0.61642 (19)0.0505 (8)
O20.30533 (19)0.67883 (15)0.61664 (16)0.0373 (6)
O30.3729 (2)0.90801 (17)0.49476 (15)0.0433 (7)
O40.2469 (2)0.79746 (15)0.47350 (15)0.0375 (6)
O50.0995 (2)0.71685 (15)0.69403 (15)0.0379 (6)
O60.0942 (2)0.82725 (15)0.79378 (16)0.0461 (7)
O70.0395 (2)0.84025 (16)0.55730 (15)0.0387 (7)
O80.03183 (19)0.94965 (16)0.65798 (16)0.0406 (7)
O90.2290 (2)1.05548 (15)0.69826 (17)0.0430 (7)
O100.38902 (19)1.03126 (16)0.62901 (17)0.0456 (7)
O110.2928 (2)0.92041 (18)0.82695 (16)0.0492 (8)
O120.4514 (2)0.89345 (18)0.75438 (16)0.0481 (7)
O130.25047 (17)0.86634 (13)0.65078 (14)0.0254 (5)
O170.1754 (3)0.16154 (19)0.9058 (2)0.0782 (11)
O180.2920 (3)0.26869 (19)0.9325 (2)0.0674 (9)
O140.7459 (2)0.9001 (2)0.9425 (2)0.0738 (10)
H140.76980.87980.98930.111*
O150.9248 (2)0.9381 (2)0.92925 (19)0.0637 (9)
C10.4856 (3)0.6134 (2)0.6411 (3)0.0472 (11)
H1A0.44140.55900.64450.071*
H1B0.52580.62240.69560.071*
H1C0.53860.60800.59430.071*
C20.4094 (3)0.6923 (2)0.6240 (2)0.0302 (8)
C30.3290 (3)0.8632 (3)0.3488 (2)0.0479 (11)
H3A0.38370.90930.33610.072*
H3B0.25760.87920.32250.072*
H3C0.35390.80630.32560.072*
C40.3164 (3)0.8553 (2)0.4464 (2)0.0305 (9)
C50.0056 (3)0.6886 (3)0.8275 (2)0.0458 (11)
H5A−0.00750.63070.80040.069*
H5B−0.06550.71670.84000.069*
H5C0.04780.68030.88110.069*
C60.0711 (3)0.7479 (2)0.7666 (2)0.0317 (9)
C7−0.1126 (3)0.9443 (3)0.5496 (3)0.0476 (11)
H7A−0.13800.99600.58200.071*
H7B−0.16960.89800.55040.071*
H7C−0.09870.96180.49010.071*
C8−0.0058 (3)0.9087 (2)0.5905 (2)0.0317 (9)
C90.3287 (3)1.1823 (2)0.6455 (3)0.0512 (12)
H9A0.39751.19350.61470.077*
H9B0.33221.21180.70160.077*
H9C0.26591.20560.61200.077*
C100.3142 (3)1.0824 (2)0.6584 (2)0.0303 (9)
C110.4539 (3)0.8788 (3)0.9092 (2)0.0487 (11)
H11A0.40250.88650.95670.073*
H11B0.51680.91930.91680.073*
H11C0.48070.81740.90840.073*
C120.3942 (3)0.8995 (2)0.8241 (2)0.0324 (9)
O160.1840 (3)0.2745 (2)0.8165 (2)0.0802 (11)
N10.2187 (3)0.2358 (2)0.8830 (2)0.0534 (10)
C130.7984 (4)0.9702 (3)0.8110 (3)0.0624 (13)
H13A0.76941.03060.81630.094*
H13B0.74150.93180.78510.094*
H13C0.86370.97070.77440.094*
C140.8301 (3)0.9353 (3)0.8986 (3)0.0470 (11)
H3AW0.0417 (12)0.9921 (13)0.8637 (11)0.083 (16)*
H1AW0.6123 (14)0.8779 (8)0.5921 (16)0.048 (12)*
H3BW0.1149 (16)1.0579 (9)0.8427 (17)0.085 (16)*
H2AW0.0434 (9)0.6407 (19)0.5202 (14)0.106 (19)*
H2BW0.122 (2)0.667 (3)0.4630 (7)0.16 (3)*
H1BW0.584 (3)0.9594 (9)0.5594 (11)0.079 (16)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Fe10.0246 (3)0.0245 (2)0.0317 (3)−0.0017 (2)0.0026 (2)−0.0008 (2)
Fe20.0289 (3)0.0224 (2)0.0313 (3)−0.0028 (2)0.0011 (2)0.0004 (2)
Fe30.0276 (3)0.0232 (2)0.0327 (3)−0.0019 (2)0.0055 (2)−0.0002 (2)
O1W0.0293 (13)0.0336 (13)0.0542 (16)0.0006 (11)0.0079 (12)0.0048 (12)
O2W0.0598 (18)0.0415 (16)0.0590 (19)−0.0159 (14)−0.0129 (15)−0.0030 (14)
O3W0.0436 (15)0.0338 (14)0.0472 (15)−0.0071 (12)0.0163 (13)−0.0110 (12)
O10.0332 (14)0.0288 (13)0.090 (2)0.0000 (12)0.0072 (14)−0.0050 (14)
O20.0375 (14)0.0235 (12)0.0506 (15)0.0018 (11)−0.0025 (12)−0.0014 (11)
O30.0430 (15)0.0563 (16)0.0306 (13)−0.0180 (13)0.0012 (12)0.0004 (12)
O40.0425 (14)0.0368 (13)0.0333 (13)−0.0113 (12)0.0046 (11)−0.0004 (11)
O50.0445 (15)0.0337 (13)0.0356 (14)−0.0096 (12)0.0077 (12)0.0040 (11)
O60.0565 (16)0.0293 (14)0.0530 (16)−0.0106 (12)0.0223 (13)0.0000 (12)
O70.0382 (14)0.0376 (14)0.0399 (14)0.0067 (12)−0.0069 (12)−0.0032 (12)
O80.0323 (14)0.0413 (14)0.0482 (16)0.0094 (12)−0.0028 (12)−0.0082 (12)
O90.0410 (15)0.0247 (13)0.0638 (17)−0.0030 (11)0.0204 (13)0.0019 (12)
O100.0341 (14)0.0250 (13)0.0784 (19)−0.0050 (11)0.0198 (14)−0.0003 (13)
O110.0411 (15)0.0685 (18)0.0376 (15)0.0119 (14)−0.0061 (13)−0.0085 (13)
O120.0355 (14)0.0763 (19)0.0324 (14)−0.0086 (14)−0.0018 (12)0.0012 (14)
O130.0236 (12)0.0226 (11)0.0303 (12)−0.0007 (9)0.0018 (10)−0.0004 (10)
O170.116 (3)0.0492 (18)0.069 (2)−0.0405 (18)−0.019 (2)0.0065 (16)
O180.0604 (19)0.0547 (18)0.087 (2)−0.0155 (16)−0.0065 (18)0.0070 (17)
O140.0485 (18)0.096 (2)0.076 (2)−0.0236 (18)−0.0037 (16)0.0325 (19)
O150.0425 (17)0.089 (2)0.0599 (19)−0.0098 (16)0.0070 (15)0.0113 (17)
C10.050 (2)0.038 (2)0.053 (2)0.0169 (19)0.000 (2)0.0056 (19)
C20.034 (2)0.0310 (18)0.0254 (18)0.0068 (17)0.0036 (15)−0.0009 (15)
C30.053 (2)0.060 (3)0.031 (2)−0.006 (2)0.0001 (19)0.0040 (19)
C40.0294 (19)0.0318 (19)0.0305 (19)0.0023 (16)0.0027 (16)0.0025 (16)
C50.047 (2)0.047 (2)0.043 (2)−0.017 (2)0.0054 (19)0.0111 (19)
C60.0297 (19)0.0257 (19)0.040 (2)−0.0044 (15)−0.0030 (16)0.0085 (15)
C70.039 (2)0.049 (2)0.054 (3)0.0014 (19)−0.008 (2)0.010 (2)
C80.0255 (18)0.035 (2)0.035 (2)−0.0030 (16)0.0037 (16)0.0117 (17)
C90.046 (2)0.032 (2)0.076 (3)−0.0016 (19)0.013 (2)0.010 (2)
C100.0274 (19)0.0260 (18)0.038 (2)−0.0042 (15)0.0007 (16)0.0009 (15)
C110.054 (3)0.050 (2)0.041 (2)−0.005 (2)−0.008 (2)0.0116 (19)
C120.040 (2)0.0230 (17)0.034 (2)−0.0067 (16)−0.0057 (17)0.0055 (16)
O160.120 (3)0.070 (2)0.0502 (19)−0.002 (2)0.002 (2)0.0049 (17)
N10.063 (2)0.045 (2)0.053 (2)−0.0038 (19)0.0088 (19)−0.0055 (18)
C130.063 (3)0.066 (3)0.058 (3)0.007 (3)−0.001 (2)0.006 (2)
C140.039 (2)0.042 (2)0.061 (3)0.0000 (19)0.005 (2)0.001 (2)

Geometric parameters (Å, °)

Fe1—O131.897 (2)O12—C121.272 (4)
Fe1—O11.987 (2)O17—N11.260 (4)
Fe1—O101.995 (2)O18—N11.240 (4)
Fe1—O122.005 (3)O14—C141.316 (4)
Fe1—O32.063 (2)O14—H140.8200
Fe1—O1W2.104 (2)O15—C141.209 (5)
Fe2—O131.900 (2)C1—C21.494 (5)
Fe2—O51.985 (2)C1—H1A0.9600
Fe2—O72.021 (2)C1—H1B0.9600
Fe2—O22.030 (2)C1—H1C0.9600
Fe2—O42.030 (2)C3—C41.501 (5)
Fe2—O2W2.126 (3)C3—H3A0.9600
Fe3—O131.916 (2)C3—H3B0.9600
Fe3—O112.011 (3)C3—H3C0.9600
Fe3—O62.013 (2)C5—C61.500 (5)
Fe3—O82.013 (2)C5—H5A0.9600
Fe3—O92.017 (2)C5—H5B0.9600
Fe3—O3W2.048 (2)C5—H5C0.9600
O1W—H1AW0.815 (9)C7—C81.497 (5)
O1W—H1BW0.814 (9)C7—H7A0.9600
O2W—H2AW0.816 (9)C7—H7B0.9600
O2W—H2BW0.819 (9)C7—H7C0.9600
O3W—H3AW0.816 (9)C9—C101.497 (5)
O3W—H3BW0.818 (9)C9—H9A0.9600
O1—C21.260 (4)C9—H9B0.9600
O2—C21.251 (4)C9—H9C0.9600
O3—C41.258 (4)C11—C121.499 (5)
O4—C41.260 (4)C11—H11A0.9600
O5—C61.249 (4)C11—H11B0.9600
O6—C61.270 (4)C11—H11C0.9600
O7—C81.254 (4)O16—N11.229 (5)
O8—C81.268 (4)C13—C141.475 (6)
O9—C101.251 (4)C13—H13A0.9600
O10—C101.251 (4)C13—H13B0.9600
O11—C121.241 (4)C13—H13C0.9600
O13—Fe1—O195.13 (10)Fe2—O13—Fe3119.60 (11)
O13—Fe1—O1098.80 (9)C14—O14—H14109.5
O1—Fe1—O10165.92 (10)C2—C1—H1A109.5
O13—Fe1—O1294.40 (10)C2—C1—H1B109.5
O1—Fe1—O1288.79 (12)H1A—C1—H1B109.5
O10—Fe1—O1292.13 (11)C2—C1—H1C109.5
O13—Fe1—O392.81 (9)H1A—C1—H1C109.5
O1—Fe1—O392.29 (11)H1B—C1—H1C109.5
O10—Fe1—O385.04 (11)O2—C2—O1123.8 (3)
O12—Fe1—O3172.58 (10)O2—C2—C1118.9 (3)
O13—Fe1—O1W176.56 (9)O1—C2—C1117.4 (3)
O1—Fe1—O1W81.82 (10)C4—C3—H3A109.5
O10—Fe1—O1W84.19 (9)C4—C3—H3B109.5
O12—Fe1—O1W87.14 (10)H3A—C3—H3B109.5
O3—Fe1—O1W85.75 (10)C4—C3—H3C109.5
O13—Fe2—O597.45 (9)H3A—C3—H3C109.5
O13—Fe2—O794.56 (9)H3B—C3—H3C109.5
O5—Fe2—O790.68 (10)O3—C4—O4124.8 (3)
O13—Fe2—O294.67 (9)O3—C4—C3118.2 (3)
O5—Fe2—O287.64 (10)O4—C4—C3117.0 (3)
O7—Fe2—O2170.76 (10)C6—C5—H5A109.5
O13—Fe2—O494.54 (9)C6—C5—H5B109.5
O5—Fe2—O4167.95 (10)H5A—C5—H5B109.5
O7—Fe2—O489.59 (10)C6—C5—H5C109.5
O2—Fe2—O490.17 (10)H5A—C5—H5C109.5
O13—Fe2—O2W174.84 (10)H5B—C5—H5C109.5
O5—Fe2—O2W87.69 (11)O5—C6—O6124.6 (3)
O7—Fe2—O2W85.90 (10)O5—C6—C5118.9 (3)
O2—Fe2—O2W84.95 (10)O6—C6—C5116.5 (3)
O4—Fe2—O2W80.32 (10)C8—C7—H7A109.5
O13—Fe3—O1192.62 (10)C8—C7—H7B109.5
O13—Fe3—O696.76 (9)H7A—C7—H7B109.5
O11—Fe3—O686.74 (11)C8—C7—H7C109.5
O13—Fe3—O893.76 (10)H7A—C7—H7C109.5
O11—Fe3—O8173.00 (10)H7B—C7—H7C109.5
O6—Fe3—O889.64 (11)O7—C8—O8124.4 (3)
O13—Fe3—O994.77 (9)O7—C8—C7118.5 (3)
O11—Fe3—O991.68 (11)O8—C8—C7117.1 (3)
O6—Fe3—O9168.42 (10)C10—C9—H9A109.5
O8—Fe3—O990.67 (10)C10—C9—H9B109.5
O13—Fe3—O3W177.83 (10)H9A—C9—H9B109.5
O11—Fe3—O3W86.91 (10)C10—C9—H9C109.5
O6—Fe3—O3W85.33 (10)H9A—C9—H9C109.5
O8—Fe3—O3W86.82 (10)H9B—C9—H9C109.5
O9—Fe3—O3W83.13 (10)O9—C10—O10124.3 (3)
Fe1—O1W—H1AW115.2 (13)O9—C10—C9118.1 (3)
Fe1—O1W—H1BW116 (2)O10—C10—C9117.6 (3)
H1AW—O1W—H1BW111.0 (16)C12—C11—H11A109.5
Fe2—O2W—H2AW126.2 (19)C12—C11—H11B109.5
Fe2—O2W—H2BW112 (3)H11A—C11—H11B109.5
H2AW—O2W—H2BW109.8 (15)C12—C11—H11C109.5
Fe3—O3W—H3AW126.8 (15)H11A—C11—H11C109.5
Fe3—O3W—H3BW117.5 (16)H11B—C11—H11C109.5
H3AW—O3W—H3BW110.7 (16)O11—C12—O12125.1 (3)
C2—O1—Fe1135.3 (2)O11—C12—C11117.6 (3)
C2—O2—Fe2129.6 (2)O12—C12—C11117.3 (3)
C4—O3—Fe1127.6 (2)O16—N1—O18122.8 (4)
C4—O4—Fe2134.9 (2)O16—N1—O17119.9 (4)
C6—O5—Fe2134.0 (2)O18—N1—O17117.2 (4)
C6—O6—Fe3132.3 (2)C14—C13—H13A109.5
C8—O7—Fe2132.1 (2)C14—C13—H13B109.5
C8—O8—Fe3134.2 (2)H13A—C13—H13B109.5
C10—O9—Fe3135.5 (2)C14—C13—H13C109.5
C10—O10—Fe1131.6 (2)H13A—C13—H13C109.5
C12—O11—Fe3134.2 (2)H13B—C13—H13C109.5
C12—O12—Fe1130.9 (2)O15—C14—O14121.4 (4)
Fe1—O13—Fe2120.78 (11)O15—C14—C13124.1 (4)
Fe1—O13—Fe3119.60 (11)O14—C14—C13114.5 (4)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O14—H14···O17i0.821.822.642 (4)178
O3W—H3AW···O15ii0.816 (9)1.894 (9)2.697 (4)168 (2)
O1W—H1AW···O18iii0.815 (9)2.008 (10)2.821 (4)176 (2)
O3W—H3BW···O17iv0.818 (9)1.938 (13)2.742 (4)167 (3)
O2W—H2AW···O15v0.816 (9)2.28 (2)2.904 (4)134 (2)
O1W—H1BW···O3vi0.814 (9)2.188 (12)2.948 (3)155 (2)

Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y, z; (iii) −x+1, y+1/2, −z+3/2; (iv) x, y+1, z; (v) x−1, −y+3/2, z−1/2; (vi) −x+1, −y+2, −z+1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB2740).

References

  • Bruker (2001). SAINT-Plus and SMART Bruker AXS Inc., Madison, Wisconsin, USA.
  • Fujihara, T., Aonahata, J., Kumakura, S., Nagasawa, A., Murakami, K. & Ito, T. (1998). Inorg. Chem.37, 3779–3784. [PubMed]
  • Ren, X. M., Okudera, H. & Kremer, R. K. (2004). Acta Cryst. E60, m14–m16.
  • Sheldrick, G. M. (2001). SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Spek, A. L. (2003). J. Appl. Cryst.36, 7–13.
  • Thirumurugan, A. & Natarajan, S. (2004). Dalton Trans. pp. 2923–2928. [PubMed]
  • Vrubel, H., Hasegawa, T., Oliverira, E. & Nunes, F. S. (2006). Inorg. Chem. Commun.9, 208–211.
  • Zhang, H. T., Li, Y. Z., Wang, H. Q., Nfor, E. N. & You, X. Z. (2005). CrystEngComm, 7, 578–585.

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