Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807021721/bx2082sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807021721/bx2082Isup2.hkl |
CCDC reference: 1233188
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%.
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).
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.
[Fe(C7H5O2)2] | F(000) = 304 |
Mr = 298.07 | Dx = 1.642 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 658 reflections |
a = 8.801 (5) Å | θ = 3.6–26.1° |
b = 6.236 (3) Å | µ = 1.26 mm−1 |
c = 11.408 (6) Å | T = 298 K |
β = 105.642 (7)° | Prism, red |
V = 602.9 (5) Å3 | 0.35 × 0.30 × 0.13 mm |
Z = 2 |
Bruker SMART CCD diffractometer | 1068 independent reflections |
Radiation source: fine-focus sealed tube | 841 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
φ and ω scans | θmax = 25.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→10 |
Tmin = 0.668, Tmax = 0.854 | k = −6→7 |
3023 measured reflections | l = −13→7 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.100 | H-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 parameters | Δρmax = 0.37 e Å−3 |
0 restraints | Δρmin = −0.29 e Å−3 |
[Fe(C7H5O2)2] | V = 602.9 (5) Å3 |
Mr = 298.07 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.801 (5) Å | µ = 1.26 mm−1 |
b = 6.236 (3) Å | T = 298 K |
c = 11.408 (6) Å | 0.35 × 0.30 × 0.13 mm |
β = 105.642 (7)° |
Bruker SMART CCD diffractometer | 1068 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 841 reflections with I > 2σ(I) |
Tmin = 0.668, Tmax = 0.854 | Rint = 0.026 |
3023 measured reflections |
R[F2 > 2σ(F2)] = 0.035 | 0 restraints |
wR(F2) = 0.100 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.37 e Å−3 |
1068 reflections | Δρmin = −0.29 e Å−3 |
88 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Fe | 0.5000 | 0.0000 | 1.0000 | 0.0375 (2) | |
O1 | 0.3768 (2) | 0.1172 (3) | 0.8467 (2) | 0.0613 (6) | |
O2 | 0.6619 (2) | 0.2057 (3) | 1.01596 (19) | 0.0577 (6) | |
C1 | 0.4067 (4) | 0.2879 (5) | 0.7994 (3) | 0.0566 (8) | |
H1A | 0.3347 | 0.3292 | 0.7272 | 0.068* | |
C2 | 0.5378 (4) | 0.4246 (5) | 0.8436 (3) | 0.0480 (7) | |
C3 | 0.6593 (3) | 0.3772 (5) | 0.9496 (3) | 0.0478 (7) | |
C4 | 0.7849 (4) | 0.5252 (5) | 0.9844 (4) | 0.0629 (10) | |
H4A | 0.8673 | 0.4982 | 1.0533 | 0.075* | |
C5 | 0.7869 (4) | 0.7082 (5) | 0.9180 (4) | 0.0694 (10) | |
H5A | 0.8708 | 0.8033 | 0.9433 | 0.083* | |
C6 | 0.6667 (4) | 0.7555 (5) | 0.8137 (4) | 0.0682 (10) | |
H6A | 0.6696 | 0.8802 | 0.7696 | 0.082* | |
C7 | 0.5447 (4) | 0.6140 (5) | 0.7779 (3) | 0.0619 (9) | |
H7A | 0.4639 | 0.6435 | 0.7084 | 0.074* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe | 0.0355 (3) | 0.0346 (3) | 0.0344 (4) | −0.0034 (2) | −0.0043 (2) | 0.0028 (2) |
O1 | 0.0597 (13) | 0.0552 (14) | 0.0568 (14) | −0.0066 (11) | −0.0052 (11) | 0.0086 (12) |
O2 | 0.0571 (13) | 0.0556 (13) | 0.0498 (13) | −0.0091 (10) | −0.0039 (10) | 0.0068 (11) |
C1 | 0.0536 (19) | 0.0568 (19) | 0.052 (2) | 0.0065 (15) | 0.0010 (15) | 0.0093 (16) |
C2 | 0.0500 (18) | 0.0448 (14) | 0.0499 (19) | 0.0071 (14) | 0.0146 (14) | 0.0032 (15) |
C3 | 0.0527 (19) | 0.0456 (17) | 0.0448 (17) | 0.0001 (14) | 0.0125 (14) | −0.0028 (15) |
C4 | 0.065 (2) | 0.063 (2) | 0.056 (2) | −0.0143 (16) | 0.0078 (17) | −0.0014 (17) |
C5 | 0.075 (2) | 0.061 (2) | 0.078 (3) | −0.0172 (19) | 0.030 (2) | −0.005 (2) |
C6 | 0.076 (2) | 0.0538 (19) | 0.082 (3) | 0.0027 (18) | 0.034 (2) | 0.0130 (19) |
C7 | 0.062 (2) | 0.059 (2) | 0.067 (2) | 0.0129 (18) | 0.0206 (17) | 0.0132 (19) |
Fe—O2i | 1.889 (2) | C2—C3 | 1.413 (4) |
Fe—O2 | 1.889 (2) | C3—C4 | 1.412 (4) |
Fe—O1i | 1.936 (2) | C4—C5 | 1.373 (4) |
Fe—O1 | 1.936 (2) | C4—H4A | 0.9300 |
O1—C1 | 1.253 (3) | C5—C6 | 1.394 (5) |
O2—C3 | 1.307 (3) | C5—H5A | 0.9300 |
C1—C2 | 1.413 (4) | C6—C7 | 1.365 (5) |
C1—H1A | 0.9300 | C6—H6A | 0.9300 |
C2—C7 | 1.409 (5) | C7—H7A | 0.9300 |
O2i—Fe—O2 | 180.0 | O2—C3—C2 | 123.9 (3) |
O2i—Fe—O1i | 93.15 (9) | C4—C3—C2 | 117.3 (3) |
O2—Fe—O1i | 86.85 (9) | C5—C4—C3 | 120.9 (3) |
O2i—Fe—O1 | 86.85 (9) | C5—C4—H4A | 119.5 |
O2—Fe—O1 | 93.15 (9) | C3—C4—H4A | 119.5 |
O1i—Fe—O1 | 180.000 (1) | C4—C5—C6 | 121.8 (3) |
C1—O1—Fe | 125.3 (2) | C4—C5—H5A | 119.1 |
C3—O2—Fe | 127.21 (19) | C6—C5—H5A | 119.1 |
O1—C1—C2 | 127.2 (3) | C7—C6—C5 | 118.3 (3) |
O1—C1—H1A | 116.4 | C7—C6—H6A | 120.9 |
C2—C1—H1A | 116.4 | C5—C6—H6A | 120.9 |
C7—C2—C3 | 120.0 (3) | C6—C7—C2 | 121.8 (3) |
C7—C2—C1 | 117.7 (3) | C6—C7—H7A | 119.1 |
C3—C2—C1 | 122.4 (3) | C2—C7—H7A | 119.1 |
O2—C3—C4 | 118.8 (3) | ||
O2i—Fe—O1—C1 | 172.5 (3) | C7—C2—C3—O2 | 179.8 (3) |
O2—Fe—O1—C1 | −7.5 (3) | C1—C2—C3—O2 | −0.1 (5) |
O1i—Fe—O1—C1 | 33 (100) | C7—C2—C3—C4 | −0.5 (5) |
O2i—Fe—O2—C3 | 0 (100) | C1—C2—C3—C4 | 179.6 (3) |
O1i—Fe—O2—C3 | −170.2 (2) | O2—C3—C4—C5 | −179.7 (3) |
O1—Fe—O2—C3 | 9.8 (2) | C2—C3—C4—C5 | 0.7 (5) |
Fe—O1—C1—C2 | 3.0 (5) | C3—C4—C5—C6 | −0.4 (5) |
O1—C1—C2—C7 | −177.5 (3) | C4—C5—C6—C7 | 0.0 (6) |
O1—C1—C2—C3 | 2.5 (5) | C5—C6—C7—C2 | 0.2 (5) |
Fe—O2—C3—C4 | 172.7 (2) | C3—C2—C7—C6 | 0.1 (5) |
Fe—O2—C3—C2 | −7.6 (4) | C1—C2—C7—C6 | −180.0 (3) |
Symmetry code: (i) −x+1, −y, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Fe(C7H5O2)2] |
Mr | 298.07 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 298 |
a, b, c (Å) | 8.801 (5), 6.236 (3), 11.408 (6) |
β (°) | 105.642 (7) |
V (Å3) | 602.9 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.26 |
Crystal size (mm) | 0.35 × 0.30 × 0.13 |
Data collection | |
Diffractometer | Bruker SMART CCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.668, 0.854 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3023, 1068, 841 |
Rint | 0.026 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.100, 1.02 |
No. of reflections | 1068 |
No. of parameters | 88 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.37, −0.29 |
Computer programs: SMART (Bruker, 1996), SAINT (Bruker, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1996), SHELXTL.