Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101017036/ta1352sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101017036/ta1352Isup2.hkl |
CCDC reference: 180137
Preparation of (I). A methanol solution of phen (36.02 mg, 0.2 mmol) was slowly added to a methanol solution of FeCl3·6H2O (54.06 mg, 0.2 mmol), followed by a water solution of Na[N(CH2COO)3] (51.42 mg, 0.2 mmol). Well shaped red polyhedral crystals of (I) were separated from the mother liquor by slow evaporation at room temperature after three weeks. They were filtered of, washed with a small amount of water, and dried in air. The yield is 25%. Anal. Calcd for C18H20N3O8Fe: C, 46.77; H, 4.36; N, 9.09%. Found: C, 46.93; H, 4.62; N, 9.35%.
All H atoms were located in difference maps and refined isotropically [C—H = 0.81 (3)–1.02 (3) Å)].
Data collection: KappaCCD (Nonius B. V., 1998); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Bruker SHELXTL V5.1 (Sheldrick, 1998); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Fig. 1. An ORTEP diagram of (I) and atom labelling, showing 50% probability displacement ellipsoids. H atoms have been omitted for clarity. |
[Fe(C6H6NO6)(C12H8N2)(H2O)].H2O | F(000) = 948 |
Mr = 460.20 | Dx = 1.637 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.7051 (5) Å | Cell parameters from 24260 reflections |
b = 8.0381 (3) Å | θ = 3.5–27.9° |
c = 19.8739 (7) Å | µ = 0.86 mm−1 |
β = 92.879 (2)° | T = 293 K |
V = 1867.51 (12) Å3 | Polyhedron, red |
Z = 4 | 0.27 × 0.16 × 0.11 mm |
NONIUS KappaCCD diffractometer | 4467 independent reflections |
Radiation source: fine-focus sealed tube | 3086 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.066 |
Detector resolution: 0.76 pixels mm-1 | θmax = 27.9°, θmin = 3.5° |
ω scans | h = −15→15 |
Absorption correction: empirical (using intensity measurements) (Blessing, 1995, 1997) | k = −10→10 |
Tmin = 0.789, Tmax = 0.909 | l = −25→26 |
24260 measured reflections |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | All H-atom parameters refined |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0476P)2 + 0.1433P] where P = (Fo2 + 2Fc2)/3 |
4467 reflections | (Δ/σ)max = 0.001 |
343 parameters | Δρmax = 0.50 e Å−3 |
0 restraints | Δρmin = −0.42 e Å−3 |
[Fe(C6H6NO6)(C12H8N2)(H2O)].H2O | V = 1867.51 (12) Å3 |
Mr = 460.20 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.7051 (5) Å | µ = 0.86 mm−1 |
b = 8.0381 (3) Å | T = 293 K |
c = 19.8739 (7) Å | 0.27 × 0.16 × 0.11 mm |
β = 92.879 (2)° |
NONIUS KappaCCD diffractometer | 4467 independent reflections |
Absorption correction: empirical (using intensity measurements) (Blessing, 1995, 1997) | 3086 reflections with I > 2σ(I) |
Tmin = 0.789, Tmax = 0.909 | Rint = 0.066 |
24260 measured reflections |
R[F2 > 2σ(F2)] = 0.040 | 0 restraints |
wR(F2) = 0.098 | All H-atom parameters refined |
S = 1.02 | Δρmax = 0.50 e Å−3 |
4467 reflections | Δρmin = −0.42 e Å−3 |
343 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 | 0.20451 (3) | 0.26301 (3) | 0.123392 (15) | 0.02161 (11) | |
O1 | 0.28839 (13) | 0.05034 (18) | 0.15071 (8) | 0.0283 (4) | |
O2 | 0.28711 (15) | −0.22592 (19) | 0.14949 (10) | 0.0388 (4) | |
O3 | 0.08277 (13) | 0.23425 (17) | 0.04966 (7) | 0.0267 (4) | |
O4 | −0.09738 (15) | 0.1759 (2) | 0.01638 (8) | 0.0418 (4) | |
O5 | 0.16469 (15) | 0.3437 (2) | 0.21563 (8) | 0.0353 (4) | |
O6 | 0.14334 (16) | 0.2722 (2) | 0.32247 (8) | 0.0413 (5) | |
O7 | 0.17502 (19) | 0.5088 (2) | 0.09580 (9) | 0.0337 (4) | |
O8 | 0.05410 (18) | 0.0701 (2) | 0.42309 (12) | 0.0444 (5) | |
N1 | 0.37406 (17) | 0.3730 (2) | 0.15566 (9) | 0.0287 (5) | |
N2 | 0.31620 (16) | 0.2314 (2) | 0.03656 (9) | 0.0262 (4) | |
N3 | 0.06959 (16) | 0.0781 (2) | 0.16354 (9) | 0.0251 (4) | |
H1 | 0.340 (2) | 0.454 (3) | 0.2449 (13) | 0.045 (8)* | |
H2 | 0.529 (3) | 0.553 (4) | 0.2748 (15) | 0.071 (10)* | |
H3 | 0.672 (3) | 0.527 (4) | 0.1961 (15) | 0.073 (10)* | |
H5 | 0.717 (3) | 0.418 (3) | 0.0848 (13) | 0.047 (9)* | |
H6 | 0.681 (2) | 0.292 (3) | −0.0165 (13) | 0.043 (8)* | |
H8 | 0.529 (2) | 0.160 (3) | −0.0955 (13) | 0.050 (8)* | |
H9 | 0.340 (2) | 0.079 (3) | −0.1116 (14) | 0.053 (8)* | |
H10 | 0.211 (2) | 0.117 (3) | −0.0263 (12) | 0.042 (8)* | |
H13A | 0.091 (2) | −0.094 (3) | 0.0944 (13) | 0.040 (7)* | |
H13B | 0.076 (2) | −0.178 (4) | 0.1637 (13) | 0.049 (8)* | |
H15A | −0.069 (2) | 0.232 (3) | 0.1548 (12) | 0.036 (7)* | |
H15B | −0.098 (2) | 0.047 (3) | 0.1334 (11) | 0.032 (7)* | |
H17B | 0.001 (2) | 0.080 (3) | 0.2557 (12) | 0.043 (7)* | |
H17A | 0.122 (2) | −0.011 (3) | 0.2557 (12) | 0.040 (7)* | |
H20 | 0.083 (3) | 0.129 (4) | 0.3952 (14) | 0.051 (10)* | |
H21 | 0.069 (3) | 0.109 (4) | 0.4611 (17) | 0.073 (12)* | |
H22 | 0.214 (3) | 0.591 (4) | 0.1193 (15) | 0.079 (11)* | |
H23 | 0.110 (3) | 0.531 (4) | 0.0908 (16) | 0.069 (12)* | |
C1 | 0.4008 (3) | 0.4463 (3) | 0.21448 (14) | 0.0402 (6) | |
C2 | 0.5106 (3) | 0.5040 (4) | 0.23225 (17) | 0.0526 (8) | |
C3 | 0.5943 (3) | 0.4867 (4) | 0.18794 (17) | 0.0554 (9) | |
C4 | 0.5701 (2) | 0.4103 (3) | 0.12480 (14) | 0.0418 (7) | |
C5 | 0.6526 (3) | 0.3853 (4) | 0.07545 (18) | 0.0547 (9) | |
C6 | 0.6247 (3) | 0.3126 (4) | 0.01623 (18) | 0.0532 (8) | |
C7 | 0.5102 (2) | 0.2566 (3) | 0.00021 (13) | 0.0379 (6) | |
C8 | 0.4760 (3) | 0.1794 (4) | −0.06066 (14) | 0.0461 (7) | |
C9 | 0.3655 (3) | 0.1299 (4) | −0.07095 (14) | 0.0441 (7) | |
C10 | 0.2876 (2) | 0.1575 (3) | −0.02136 (12) | 0.0354 (6) | |
C11 | 0.4272 (2) | 0.2796 (3) | 0.04767 (12) | 0.0289 (5) | |
C12 | 0.4576 (2) | 0.3564 (3) | 0.11131 (12) | 0.0287 (5) | |
C13 | 0.1083 (2) | −0.0849 (3) | 0.13960 (13) | 0.0274 (5) | |
C14 | 0.2375 (2) | −0.0907 (3) | 0.14758 (11) | 0.0251 (5) | |
C15 | −0.0399 (2) | 0.1308 (3) | 0.13152 (12) | 0.0309 (5) | |
C16 | −0.0208 (2) | 0.1821 (3) | 0.05961 (11) | 0.0287 (5) | |
C17 | 0.0738 (2) | 0.0869 (3) | 0.23721 (11) | 0.0302 (5) | |
C18 | 0.1315 (2) | 0.2460 (3) | 0.26142 (11) | 0.0270 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe | 0.01980 (18) | 0.02124 (17) | 0.02356 (17) | −0.00200 (13) | −0.00100 (12) | −0.00070 (13) |
O1 | 0.0219 (9) | 0.0247 (8) | 0.0378 (9) | −0.0034 (7) | −0.0044 (7) | 0.0022 (7) |
O2 | 0.0304 (10) | 0.0242 (8) | 0.0614 (11) | 0.0027 (7) | −0.0021 (9) | −0.0012 (8) |
O3 | 0.0219 (9) | 0.0320 (8) | 0.0259 (8) | −0.0017 (7) | −0.0017 (6) | −0.0010 (7) |
O4 | 0.0270 (10) | 0.0580 (11) | 0.0392 (10) | −0.0019 (9) | −0.0103 (8) | −0.0049 (9) |
O5 | 0.0426 (11) | 0.0290 (9) | 0.0349 (9) | −0.0087 (8) | 0.0087 (8) | −0.0085 (8) |
O6 | 0.0451 (12) | 0.0517 (11) | 0.0272 (9) | −0.0026 (9) | 0.0037 (8) | −0.0091 (8) |
O7 | 0.0324 (12) | 0.0230 (8) | 0.0449 (10) | 0.0016 (8) | −0.0073 (9) | 0.0018 (8) |
O8 | 0.0452 (13) | 0.0447 (11) | 0.0427 (12) | −0.0076 (9) | −0.0034 (10) | 0.0027 (11) |
N1 | 0.0270 (12) | 0.0257 (10) | 0.0328 (11) | −0.0036 (8) | −0.0061 (9) | 0.0014 (9) |
N2 | 0.0208 (10) | 0.0289 (10) | 0.0287 (10) | 0.0004 (8) | −0.0006 (8) | 0.0021 (8) |
N3 | 0.0229 (11) | 0.0258 (9) | 0.0264 (9) | 0.0015 (8) | 0.0006 (8) | −0.0030 (8) |
C1 | 0.0395 (17) | 0.0394 (14) | 0.0404 (15) | −0.0066 (13) | −0.0106 (13) | −0.0018 (13) |
C2 | 0.047 (2) | 0.0532 (18) | 0.0554 (18) | −0.0122 (15) | −0.0236 (17) | −0.0089 (16) |
C3 | 0.0316 (18) | 0.0586 (19) | 0.073 (2) | −0.0156 (15) | −0.0228 (17) | 0.0024 (16) |
C4 | 0.0233 (15) | 0.0418 (15) | 0.0594 (17) | −0.0060 (12) | −0.0079 (13) | 0.0111 (13) |
C5 | 0.0227 (17) | 0.064 (2) | 0.077 (2) | −0.0097 (15) | −0.0028 (16) | 0.0150 (18) |
C6 | 0.0267 (17) | 0.066 (2) | 0.068 (2) | 0.0020 (15) | 0.0142 (16) | 0.0162 (18) |
C7 | 0.0254 (14) | 0.0427 (15) | 0.0462 (15) | 0.0035 (12) | 0.0061 (11) | 0.0107 (12) |
C8 | 0.0363 (18) | 0.0581 (17) | 0.0455 (16) | 0.0122 (14) | 0.0171 (14) | 0.0024 (15) |
C9 | 0.0404 (19) | 0.0567 (17) | 0.0355 (14) | 0.0045 (14) | 0.0063 (13) | −0.0085 (14) |
C10 | 0.0300 (16) | 0.0430 (14) | 0.0334 (13) | 0.0010 (12) | 0.0024 (12) | −0.0045 (12) |
C11 | 0.0218 (13) | 0.0271 (11) | 0.0377 (13) | 0.0013 (10) | −0.0003 (10) | 0.0096 (10) |
C12 | 0.0203 (13) | 0.0269 (11) | 0.0383 (13) | −0.0015 (10) | −0.0053 (10) | 0.0074 (11) |
C13 | 0.0251 (14) | 0.0238 (12) | 0.0332 (13) | −0.0031 (10) | −0.0012 (11) | −0.0050 (11) |
C14 | 0.0248 (13) | 0.0237 (11) | 0.0266 (11) | −0.0002 (10) | −0.0002 (10) | 0.0003 (9) |
C15 | 0.0178 (13) | 0.0338 (13) | 0.0409 (14) | −0.0008 (11) | 0.0009 (11) | −0.0012 (12) |
C16 | 0.0224 (14) | 0.0292 (12) | 0.0340 (13) | 0.0016 (10) | −0.0030 (10) | −0.0069 (10) |
C17 | 0.0312 (15) | 0.0332 (13) | 0.0263 (12) | −0.0043 (11) | 0.0035 (11) | −0.0017 (10) |
C18 | 0.0218 (12) | 0.0319 (12) | 0.0278 (12) | 0.0043 (10) | 0.0047 (9) | −0.0033 (11) |
Fe—O3 | 2.0054 (15) | C2—H2 | 0.95 (3) |
Fe—O5 | 2.0208 (15) | C3—C4 | 1.413 (4) |
Fe—O1 | 2.0316 (15) | C3—H3 | 0.97 (3) |
Fe—O7 | 2.0744 (16) | C4—C12 | 1.400 (3) |
Fe—N2 | 2.2311 (19) | C4—C5 | 1.424 (4) |
Fe—N1 | 2.2370 (19) | C5—C6 | 1.340 (5) |
Fe—N3 | 2.3381 (19) | C5—H5 | 0.81 (3) |
O1—C14 | 1.281 (3) | C6—C7 | 1.434 (4) |
O2—C14 | 1.232 (3) | C6—H6 | 0.97 (3) |
O3—C16 | 1.307 (3) | C7—C11 | 1.400 (3) |
O4—C16 | 1.211 (3) | C7—C8 | 1.400 (4) |
O5—C18 | 1.277 (3) | C8—C9 | 1.358 (4) |
O6—C18 | 1.232 (3) | C8—H8 | 0.96 (3) |
O7—H22 | 0.92 (4) | C9—C10 | 1.394 (4) |
O7—H23 | 0.79 (4) | C9—H9 | 0.94 (3) |
O8—H20 | 0.81 (3) | C10—H10 | 0.96 (3) |
O8—H21 | 0.83 (3) | C11—C12 | 1.436 (3) |
N1—C1 | 1.332 (3) | C13—C14 | 1.513 (3) |
N1—C12 | 1.355 (3) | C13—H13A | 0.92 (2) |
N2—C10 | 1.324 (3) | C13—H13B | 0.97 (3) |
N2—C11 | 1.363 (3) | C15—C16 | 1.515 (3) |
N3—C17 | 1.464 (3) | C15—H15A | 1.01 (2) |
N3—C15 | 1.465 (3) | C15—H15B | 0.96 (2) |
N3—C13 | 1.473 (3) | C17—C18 | 1.513 (3) |
C1—C2 | 1.395 (4) | C17—H17B | 0.95 (3) |
C1—H1 | 0.96 (3) | C17—H17A | 1.02 (3) |
C2—C3 | 1.357 (5) | ||
O3—Fe—O5 | 120.80 (7) | C6—C5—C4 | 121.5 (3) |
O3—Fe—O1 | 114.48 (6) | C6—C5—H5 | 122 (2) |
O5—Fe—O1 | 99.09 (7) | C4—C5—H5 | 117 (2) |
O3—Fe—O7 | 79.28 (7) | C5—C6—C7 | 121.1 (3) |
O5—Fe—O7 | 83.76 (7) | C5—C6—H6 | 121.3 (16) |
O1—Fe—O7 | 160.68 (8) | C7—C6—H6 | 117.6 (16) |
O3—Fe—N2 | 81.03 (7) | C11—C7—C8 | 117.5 (2) |
O5—Fe—N2 | 155.35 (7) | C11—C7—C6 | 118.8 (3) |
O1—Fe—N2 | 79.45 (7) | C8—C7—C6 | 123.7 (3) |
O7—Fe—N2 | 90.01 (7) | C9—C8—C7 | 119.3 (3) |
O3—Fe—N1 | 147.42 (6) | C9—C8—H8 | 118.9 (16) |
O5—Fe—N1 | 81.66 (7) | C7—C8—H8 | 121.9 (16) |
O1—Fe—N1 | 81.16 (6) | C8—C9—C10 | 119.9 (3) |
O7—Fe—N1 | 80.37 (8) | C8—C9—H9 | 121.3 (18) |
N2—Fe—N1 | 73.79 (7) | C10—C9—H9 | 118.7 (18) |
O3—Fe—N3 | 73.07 (6) | N2—C10—C9 | 122.7 (3) |
O5—Fe—N3 | 72.78 (6) | N2—C10—H10 | 116.0 (15) |
O1—Fe—N3 | 72.51 (6) | C9—C10—H10 | 121.2 (15) |
O7—Fe—N3 | 126.11 (8) | N2—C11—C7 | 122.8 (2) |
N2—Fe—N3 | 128.58 (6) | N2—C11—C12 | 117.1 (2) |
N1—Fe—N3 | 139.31 (6) | C7—C11—C12 | 120.1 (2) |
C14—O1—Fe | 120.96 (14) | N1—C12—C4 | 123.2 (2) |
C16—O3—Fe | 123.84 (14) | N1—C12—C11 | 117.4 (2) |
C18—O5—Fe | 122.78 (14) | C4—C12—C11 | 119.4 (2) |
Fe—O7—H22 | 119 (2) | N3—C13—C14 | 108.38 (18) |
Fe—O7—H23 | 113 (2) | N3—C13—H13A | 109.4 (16) |
H22—O7—H23 | 111 (3) | C14—C13—H13A | 105.9 (16) |
H20—O8—H21 | 109 (3) | N3—C13—H13B | 112.9 (16) |
C1—N1—C12 | 118.0 (2) | C14—C13—H13B | 109.6 (16) |
C1—N1—Fe | 126.30 (19) | H13A—C13—H13B | 110 (2) |
C12—N1—Fe | 115.67 (14) | O2—C14—O1 | 124.2 (2) |
C10—N2—C11 | 117.7 (2) | O2—C14—C13 | 119.8 (2) |
C10—N2—Fe | 126.26 (17) | O1—C14—C13 | 115.98 (19) |
C11—N2—Fe | 115.68 (15) | N3—C15—C16 | 108.7 (2) |
C17—N3—C15 | 113.89 (19) | N3—C15—H15A | 110.4 (14) |
C17—N3—C13 | 111.76 (18) | C16—C15—H15A | 106.4 (13) |
C15—N3—C13 | 113.18 (18) | N3—C15—H15B | 113.0 (14) |
C17—N3—Fe | 108.72 (13) | C16—C15—H15B | 111.5 (14) |
C15—N3—Fe | 105.03 (13) | H15A—C15—H15B | 106.6 (19) |
C13—N3—Fe | 103.37 (14) | O4—C16—O3 | 124.4 (2) |
N1—C1—C2 | 122.8 (3) | O4—C16—C15 | 121.3 (2) |
N1—C1—H1 | 115.7 (16) | O3—C16—C15 | 114.33 (19) |
C2—C1—H1 | 121.5 (16) | N3—C17—C18 | 110.55 (19) |
C3—C2—C1 | 119.2 (3) | N3—C17—H17B | 113.4 (15) |
C3—C2—H2 | 119 (2) | C18—C17—H17B | 108.9 (16) |
C1—C2—H2 | 122 (2) | N3—C17—H17A | 108.2 (14) |
C2—C3—C4 | 120.2 (3) | C18—C17—H17A | 107.8 (14) |
C2—C3—H3 | 123.8 (19) | H17B—C17—H17A | 108 (2) |
C4—C3—H3 | 116.1 (19) | O6—C18—O5 | 125.0 (2) |
C12—C4—C3 | 116.7 (3) | O6—C18—C17 | 118.9 (2) |
C12—C4—C5 | 119.2 (3) | O5—C18—C17 | 116.09 (19) |
C3—C4—C5 | 124.1 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H20···O6 | 0.82 (3) | 2.00 (3) | 2.818 (3) | 176 (4) |
O8—H21···O3i | 0.83 (3) | 2.16 (3) | 2.971 (3) | 164 (4) |
O7—H22···O2ii | 0.92 (3) | 1.79 (3) | 2.696 (2) | 168 (3) |
O7—H23···O8iii | 0.78 (4) | 1.95 (4) | 2.734 (3) | 176 (4) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, y+1, z; (iii) −x, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Fe(C6H6NO6)(C12H8N2)(H2O)].H2O |
Mr | 460.20 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 11.7051 (5), 8.0381 (3), 19.8739 (7) |
β (°) | 92.879 (2) |
V (Å3) | 1867.51 (12) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.86 |
Crystal size (mm) | 0.27 × 0.16 × 0.11 |
Data collection | |
Diffractometer | NONIUS KappaCCD diffractometer |
Absorption correction | Empirical (using intensity measurements) (Blessing, 1995, 1997) |
Tmin, Tmax | 0.789, 0.909 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 24260, 4467, 3086 |
Rint | 0.066 |
(sin θ/λ)max (Å−1) | 0.659 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.098, 1.02 |
No. of reflections | 4467 |
No. of parameters | 343 |
H-atom treatment | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | 0.50, −0.42 |
Computer programs: KappaCCD (Nonius B. V., 1998), HKL SCALEPACK (Otwinowski & Minor, 1997), HKL DENZO (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), Bruker SHELXTL V5.1 (Sheldrick, 1998).
Fe—O3 | 2.0054 (15) | Fe—N2 | 2.2311 (19) |
Fe—O5 | 2.0208 (15) | Fe—N1 | 2.2370 (19) |
Fe—O1 | 2.0316 (15) | Fe—N3 | 2.3381 (19) |
Fe—O7 | 2.0744 (16) |
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H20···O6 | 0.82 (3) | 2.00 (3) | 2.818 (3) | 176 (4) |
O8—H21···O3i | 0.83 (3) | 2.16 (3) | 2.971 (3) | 164 (4) |
O7—H22···O2ii | 0.92 (3) | 1.79 (3) | 2.696 (2) | 168 (3) |
O7—H23···O8iii | 0.78 (4) | 1.95 (4) | 2.734 (3) | 176 (4) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, y+1, z; (iii) −x, y+1/2, −z+1/2. |
The structures of several iron(III) complexes containing coordinated tetradentate NTA (Clegg et al., 1984; White et al., 1984; Heath et al., 1992; Fujita et al., 1994; Powell et al., 1995) have been reported due to the unique reactivity of Fe(III)-NTA solutions (Awai et al., 1979; Goddard et al., 1986). With the exception of the seven-coordinate [Fe(NTA)2]3- ion (Clegg et al., 1984), the iron atoms in all the known Fe-NTA complexes are six-coordinate. To the best of our knowledge, seven-coordinate iron(III) compounds are also rare (Marlin et al., 2000; Sanchiz et al., 1997; Finnen et al., 1991; Fleischer & Hawkinson, 1967). Herein we report the X-ray structure of a seven-coordinate iron centre compound, [Fe(NTA)(Phen)(H2O)]·H2O (I).
Unlike most seven-coordinate iron(III) complexes which usually have pentagonal bipyramidal geometries, the Fe atom in (I) lies near the centre of a distorted capped trigonal prism: O1, O3 and N2; and O5, O7 and N1 make up the two triangular ends of the distorted trigonal prism, while N3 (of NTA) occupies the capped position (Fig. 1). The Fe—O7 (water) bond length is significantly longer than the Fe—O bond lengths to NTA (Table 1), but the latter are similar to those previously observed in Fe(NTA) complexes (Clegg et al., 1984; White et al., 1984; Heath et al., 1992; Fujita et al., 1994; Powell et al., 1995). The Fe—N3 bond length is significantly longer than the average value of the Fe—N(Phen) bonds [2.2340 (13) Å]. Steric effects due to the constraints on the NTA ligand, required by its tetradentate ligation, may be responsible for the difference in the Fe—N bond lengths. The molecules are packed in such a way that the intermolecular O—H···O hydrogen bonding interconnections [2.696 (2) Å] between the coordinated water molecule and the carboxylate oxygen (O2) in the NTA ligand (Table 2) results in infinite chains of molecules. Each solvent water molecule bridges two iron complex molecules through long-range intermolecular hydrogen bonds O8—H···O and forms the rung of the infinite ladder packing mode.