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Acta Cryst. (2007). E63, m1613    [ doi:10.1107/S1600536807021721 ]

Bis(2-formylphenolato-[kappa]2O,O')iron(II)

Y.-M. Yang, P.-C. Lu, T.-T. Zhu and C.-H. Liu

Abstract top

The title complex, [Fe(C7H5O2)2], is a mononuclear iron(II) complex with a distorted square planar coordination geometry and has the central Fe2+ ion located on an inversion centre, with four O atoms from two 2-formylphenolate ligands.

Experimental top

Equimolar iron(II) acetate and salicylaldehyde were put into a Teflon vessel, and aqueous ethanol solution (H2O: EtOH = 1: 1 v/v) was added. The vessel was then put in a stainless steel tank to make hydrothermal treatment. The tank was heated to 140°C for 48 h. After the autoclave was cooled to room temperature, red crystals were formed. They were filtered, washed with aqueous ethanol solution for three times, and dried in a vacuo using CaCl2, yield 71%.

Refinement top

C-bound H atoms were included in the riding model approximation with C—H = 0.93 - 0.97 Å, and with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 1996); cell refinement: SAINT (Bruker, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1996); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. A view of the molecular structure of (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability label and H atoms are shown as small spheres of arbitrary radii. Unlabeled atoms are related to labeled atoms by the symmetry code (-x + 1,-y,-z + 2).
Bis(2-formylphenolato-κ2O,O')iron(II) top
Crystal data top
[Fe(C7H5O2)2]F(000) = 304
Mr = 298.07Dx = 1.642 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 658 reflections
a = 8.801 (5) Åθ = 3.6–26.1°
b = 6.236 (3) ŵ = 1.26 mm−1
c = 11.408 (6) ÅT = 298 K
β = 105.642 (7)°Prism, red
V = 602.9 (5) Å30.35 × 0.30 × 0.13 mm
Z = 2
Data collection top
Bruker SMART CCD
diffractometer		1068 independent reflections
Radiation source: fine-focus sealed tube841 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
φ and ω scansθmax = 25.0°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −9→10
Tmin = 0.668, Tmax = 0.854k = −6→7
3023 measured reflectionsl = −13→7
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.100H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0643P)2]
where P = (Fo2 + 2Fc2)/3
1068 reflections(Δ/σ)max = 0.009
88 parametersΔρmax = 0.37 e Å−3
0 restraintsΔρmin = −0.29 e Å−3
Crystal data top
[Fe(C7H5O2)2]V = 602.9 (5) Å3
Mr = 298.07Z = 2
Monoclinic, P21/nMo Kα radiation
a = 8.801 (5) ŵ = 1.26 mm−1
b = 6.236 (3) ÅT = 298 K
c = 11.408 (6) Å0.35 × 0.30 × 0.13 mm
β = 105.642 (7)°
Data collection top
Bruker SMART CCD
diffractometer		1068 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		841 reflections with I > 2σ(I)
Tmin = 0.668, Tmax = 0.854Rint = 0.026
3023 measured reflectionsθmax = 25.0°
Refinement top
R[F2 > 2σ(F2)] = 0.035H-atom parameters constrained
wR(F2) = 0.100Δρmax = 0.37 e Å−3
S = 1.02Δρmin = −0.29 e Å−3
1068 reflectionsAbsolute structure: ?
88 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Special details top

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) top
xyzUiso*/Ueq
Fe0.50000.00001.00000.0375 (2)
O10.3768 (2)0.1172 (3)0.8467 (2)0.0613 (6)
O20.6619 (2)0.2057 (3)1.01596 (19)0.0577 (6)
C10.4067 (4)0.2879 (5)0.7994 (3)0.0566 (8)
H1A0.33470.32920.72720.068*
C20.5378 (4)0.4246 (5)0.8436 (3)0.0480 (7)
C30.6593 (3)0.3772 (5)0.9496 (3)0.0478 (7)
C40.7849 (4)0.5252 (5)0.9844 (4)0.0629 (10)
H4A0.86730.49821.05330.075*
C50.7869 (4)0.7082 (5)0.9180 (4)0.0694 (10)
H5A0.87080.80330.94330.083*
C60.6667 (4)0.7555 (5)0.8137 (4)0.0682 (10)
H6A0.66960.88020.76960.082*
C70.5447 (4)0.6140 (5)0.7779 (3)0.0619 (9)
H7A0.46390.64350.70840.074*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.0355 (3)0.0346 (3)0.0344 (4)−0.0034 (2)−0.0043 (2)0.0028 (2)
O10.0597 (13)0.0552 (14)0.0568 (14)−0.0066 (11)−0.0052 (11)0.0086 (12)
O20.0571 (13)0.0556 (13)0.0498 (13)−0.0091 (10)−0.0039 (10)0.0068 (11)
C10.0536 (19)0.0568 (19)0.052 (2)0.0065 (15)0.0010 (15)0.0093 (16)
C20.0500 (18)0.0448 (14)0.0499 (19)0.0071 (14)0.0146 (14)0.0032 (15)
C30.0527 (19)0.0456 (17)0.0448 (17)0.0001 (14)0.0125 (14)−0.0028 (15)
C40.065 (2)0.063 (2)0.056 (2)−0.0143 (16)0.0078 (17)−0.0014 (17)
C50.075 (2)0.061 (2)0.078 (3)−0.0172 (19)0.030 (2)−0.005 (2)
C60.076 (2)0.0538 (19)0.082 (3)0.0027 (18)0.034 (2)0.0130 (19)
C70.062 (2)0.059 (2)0.067 (2)0.0129 (18)0.0206 (17)0.0132 (19)
Geometric parameters (Å, º) top
Fe—O2i1.889 (2)C2—C31.413 (4)
Fe—O21.889 (2)C3—C41.412 (4)
Fe—O1i1.936 (2)C4—C51.373 (4)
Fe—O11.936 (2)C4—H4A0.9300
O1—C11.253 (3)C5—C61.394 (5)
O2—C31.307 (3)C5—H5A0.9300
C1—C21.413 (4)C6—C71.365 (5)
C1—H1A0.9300C6—H6A0.9300
C2—C71.409 (5)C7—H7A0.9300
O2i—Fe—O2180.0O2—C3—C2123.9 (3)
O2i—Fe—O1i93.15 (9)C4—C3—C2117.3 (3)
O2—Fe—O1i86.85 (9)C5—C4—C3120.9 (3)
O2i—Fe—O186.85 (9)C5—C4—H4A119.5
O2—Fe—O193.15 (9)C3—C4—H4A119.5
O1i—Fe—O1180.000 (1)C4—C5—C6121.8 (3)
C1—O1—Fe125.3 (2)C4—C5—H5A119.1
C3—O2—Fe127.21 (19)C6—C5—H5A119.1
O1—C1—C2127.2 (3)C7—C6—C5118.3 (3)
O1—C1—H1A116.4C7—C6—H6A120.9
C2—C1—H1A116.4C5—C6—H6A120.9
C7—C2—C3120.0 (3)C6—C7—C2121.8 (3)
C7—C2—C1117.7 (3)C6—C7—H7A119.1
C3—C2—C1122.4 (3)C2—C7—H7A119.1
O2—C3—C4118.8 (3)
O2i—Fe—O1—C1172.5 (3)C7—C2—C3—O2179.8 (3)
O2—Fe—O1—C1−7.5 (3)C1—C2—C3—O2−0.1 (5)
O1i—Fe—O1—C133 (100)C7—C2—C3—C4−0.5 (5)
O2i—Fe—O2—C30 (100)C1—C2—C3—C4179.6 (3)
O1i—Fe—O2—C3−170.2 (2)O2—C3—C4—C5−179.7 (3)
O1—Fe—O2—C39.8 (2)C2—C3—C4—C50.7 (5)
Fe—O1—C1—C23.0 (5)C3—C4—C5—C6−0.4 (5)
O1—C1—C2—C7−177.5 (3)C4—C5—C6—C70.0 (6)
O1—C1—C2—C32.5 (5)C5—C6—C7—C20.2 (5)
Fe—O2—C3—C4172.7 (2)C3—C2—C7—C60.1 (5)
Fe—O2—C3—C2−7.6 (4)C1—C2—C7—C6−180.0 (3)
Symmetry code: (i) −x+1, −y, −z+2.
Acknowledgements top

The work was supported by the Analytical Test Fund of Nanjing University awarded to Dr Chang-Hong Liu.

references
References top

Bruker (1996). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXTL. Version 5.1. Bruker AXS Inc., Madison, Wisconsin, USA.