Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807049665/is2216sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807049665/is2216Isup2.hkl |
CCDC reference: 1271179
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.029
- wR factor = 0.107
- Data-to-parameter ratio = 13.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 3000 Deg. PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - Cl1 .. 5.19 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P1
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Fe1 (3) 2.97
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
A mixture of iron(III) trichloride (1 mmol) and tris(2-pyridylmethyl)amine (1 mmol) in 20 ml me thanol was refluxed for 2 h. The cooled solution was filterated and the filtrate was evaporated naturally at room temperature. Two days later, brown blocks of (I) were obtained with a yield of 10%. Anal. Calc. for C36H36Cl2F12Fe2N8OP2: C 40.41, H 3.37, N 10.48%; Found: C 40.37, H 3.39, N 10.43%.
All H atoms were placed in calculated positions (C—H = 0.93 or 0.97 Å) and refined as riding, with Uiso(H) = 1.2Ueq(C).
In recent years, N-heterocycle ligands have been widely used as polydentate ligands which show various metal chelation reactions (Scapin et al., 1997; Okabe & Oya, 2000; Serre et al., 2005). In this paper, we report the structure of the title compound, (I).
As shown in Fig. 1, the FeIII atom is chelated by the tetradentate ligand of tris(2-pyridylmethyl)amine via four N atoms, and further bonded by one chloride ion and one bridging oxygen atom. Along the axial site, two FeIII atoms are linked into dimer via one oxygen atom (Fig. 2).
For related literature, see: Scapin et al. (1997); Okabe & Oya (2000); Serre et al. (2005).
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).
[Fe2Cl2O(C18H18N4)2](PF6)2 | Z = 1 |
Mr = 1069.27 | F(000) = 540 |
Triclinic, P1 | Dx = 1.695 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.5480 (17) Å | Cell parameters from 3903 reflections |
b = 11.280 (2) Å | θ = 3.0–25.5° |
c = 12.829 (3) Å | µ = 0.99 mm−1 |
α = 115.49 (3)° | T = 293 K |
β = 107.44 (3)° | Block, brown |
γ = 91.52 (3)° | 0.43 × 0.28 × 0.22 mm |
V = 1047.7 (4) Å3 |
Bruker APEXII CCD area-detector diffractometer | 3903 independent reflections |
Radiation source: fine-focus sealed tube | 3622 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
φ and ω scans | θmax = 25.5°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −8→10 |
Tmin = 0.675, Tmax = 0.811 | k = −13→13 |
8741 measured reflections | l = −15→15 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0834P)2 + 0.2007P] where P = (Fo2 + 2Fc2)/3 |
3903 reflections | (Δ/σ)max < 0.001 |
287 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.26 e Å−3 |
[Fe2Cl2O(C18H18N4)2](PF6)2 | γ = 91.52 (3)° |
Mr = 1069.27 | V = 1047.7 (4) Å3 |
Triclinic, P1 | Z = 1 |
a = 8.5480 (17) Å | Mo Kα radiation |
b = 11.280 (2) Å | µ = 0.99 mm−1 |
c = 12.829 (3) Å | T = 293 K |
α = 115.49 (3)° | 0.43 × 0.28 × 0.22 mm |
β = 107.44 (3)° |
Bruker APEXII CCD area-detector diffractometer | 3903 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 3622 reflections with I > 2σ(I) |
Tmin = 0.675, Tmax = 0.811 | Rint = 0.021 |
8741 measured reflections |
R[F2 > 2σ(F2)] = 0.029 | 0 restraints |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.00 | Δρmax = 0.35 e Å−3 |
3903 reflections | Δρmin = −0.26 e Å−3 |
287 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 | ||
Fe1 | 1.03741 (3) | 0.34679 (3) | 0.39270 (2) | 0.03262 (13) | |
C1 | 0.9133 (4) | 0.5294 (2) | 0.1545 (2) | 0.0555 (6) | |
H1 | 0.8141 | 0.5476 | 0.1144 | 0.067* | |
C2 | 1.0635 (4) | 0.5737 (3) | 0.1516 (2) | 0.0667 (8) | |
H2 | 1.0659 | 0.6246 | 0.1109 | 0.080* | |
C3 | 0.7462 (3) | 0.1753 (2) | 0.1448 (2) | 0.0520 (6) | |
H3A | 0.7443 | 0.2011 | 0.0815 | 0.062* | |
H3B | 0.6367 | 0.1253 | 0.1211 | 0.062* | |
C4 | 1.2074 (4) | 0.5439 (3) | 0.2073 (3) | 0.0668 (7) | |
H4 | 1.3081 | 0.5725 | 0.2041 | 0.080* | |
C5 | 1.2014 (3) | 0.4705 (3) | 0.2686 (2) | 0.0558 (6) | |
H5 | 1.2994 | 0.4493 | 0.3069 | 0.067* | |
C6 | 0.9542 (4) | −0.1238 (2) | 0.0605 (2) | 0.0563 (6) | |
H6 | 0.9321 | −0.2120 | 0.0001 | 0.068* | |
C7 | 1.1346 (3) | 0.0609 (2) | 0.2407 (2) | 0.0483 (5) | |
H7 | 1.2380 | 0.0967 | 0.3031 | 0.058* | |
C8 | 0.8350 (3) | −0.0449 (2) | 0.0586 (2) | 0.0479 (5) | |
H8 | 0.7308 | −0.0793 | −0.0031 | 0.057* | |
C9 | 1.1065 (3) | −0.0703 (2) | 0.1529 (2) | 0.0559 (6) | |
H9 | 1.1894 | −0.1217 | 0.1563 | 0.067* | |
C10 | 0.6720 (3) | 0.2875 (2) | 0.3311 (2) | 0.0448 (5) | |
H10A | 0.5634 | 0.2354 | 0.2732 | 0.054* | |
H10B | 0.6561 | 0.3761 | 0.3820 | 0.054* | |
C11 | 0.7289 (3) | 0.1177 (3) | 0.5343 (2) | 0.0550 (6) | |
H11 | 0.6661 | 0.0789 | 0.5631 | 0.066* | |
C12 | 0.9878 (3) | 0.1900 (2) | 0.53063 (19) | 0.0408 (4) | |
H12 | 1.1033 | 0.1989 | 0.5572 | 0.049* | |
C13 | 0.9147 (3) | 0.4569 (2) | 0.21892 (17) | 0.0419 (5) | |
C14 | 0.8988 (3) | 0.1304 (2) | 0.5744 (2) | 0.0490 (5) | |
H14 | 0.9529 | 0.0995 | 0.6297 | 0.059* | |
C15 | 0.6513 (3) | 0.1628 (2) | 0.4510 (2) | 0.0507 (5) | |
H15 | 0.5357 | 0.1526 | 0.4218 | 0.061* | |
C16 | 0.7606 (3) | 0.4151 (2) | 0.23721 (19) | 0.0426 (5) | |
H16A | 0.7431 | 0.4888 | 0.3056 | 0.051* | |
H16B | 0.6645 | 0.3919 | 0.1640 | 0.051* | |
C17 | 0.7467 (2) | 0.22294 (19) | 0.41166 (19) | 0.0376 (4) | |
C18 | 0.8712 (3) | 0.0858 (2) | 0.14890 (18) | 0.0376 (4) | |
Cl1 | 1.31395 (6) | 0.35084 (6) | 0.48437 (5) | 0.05048 (18) | |
F1 | 0.5830 (3) | 0.6609 (2) | 0.1918 (2) | 0.1015 (7) | |
F2 | 0.6042 (3) | 0.7201 (2) | 0.04869 (17) | 0.0865 (6) | |
F3 | 0.4872 (2) | 0.8487 (2) | 0.27954 (15) | 0.0822 (5) | |
F4 | 0.7327 (2) | 0.8614 (2) | 0.24929 (18) | 0.0928 (7) | |
F5 | 0.5110 (2) | 0.90780 (17) | 0.13816 (17) | 0.0758 (5) | |
F6 | 0.36000 (19) | 0.71100 (16) | 0.08030 (14) | 0.0660 (4) | |
N1 | 1.0560 (2) | 0.42830 (18) | 0.27430 (16) | 0.0430 (4) | |
N2 | 0.7779 (2) | 0.29828 (16) | 0.26251 (15) | 0.0373 (4) | |
N3 | 1.0195 (2) | 0.13923 (16) | 0.23996 (15) | 0.0388 (4) | |
N4 | 0.9131 (2) | 0.23558 (16) | 0.45116 (15) | 0.0359 (4) | |
O1 | 1.0000 | 0.5000 | 0.5000 | 0.0375 (4) | |
P1 | 0.54888 (7) | 0.78429 (6) | 0.16556 (5) | 0.04801 (18) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.02598 (19) | 0.03690 (19) | 0.03504 (19) | 0.00687 (11) | 0.00891 (12) | 0.01758 (13) |
C1 | 0.0802 (18) | 0.0457 (12) | 0.0422 (12) | 0.0145 (11) | 0.0187 (11) | 0.0230 (10) |
C2 | 0.105 (2) | 0.0507 (13) | 0.0512 (14) | 0.0005 (14) | 0.0321 (14) | 0.0270 (11) |
C3 | 0.0475 (13) | 0.0445 (11) | 0.0411 (11) | 0.0094 (10) | −0.0014 (9) | 0.0106 (9) |
C4 | 0.081 (2) | 0.0650 (16) | 0.0624 (15) | −0.0025 (14) | 0.0340 (14) | 0.0309 (13) |
C5 | 0.0541 (14) | 0.0630 (15) | 0.0572 (14) | 0.0042 (11) | 0.0247 (11) | 0.0303 (12) |
C6 | 0.0718 (17) | 0.0396 (11) | 0.0564 (13) | 0.0117 (10) | 0.0302 (12) | 0.0155 (10) |
C7 | 0.0428 (12) | 0.0498 (12) | 0.0541 (13) | 0.0145 (9) | 0.0183 (10) | 0.0241 (10) |
C8 | 0.0520 (13) | 0.0426 (11) | 0.0436 (11) | 0.0015 (9) | 0.0160 (9) | 0.0159 (9) |
C9 | 0.0580 (15) | 0.0516 (13) | 0.0672 (15) | 0.0246 (11) | 0.0326 (12) | 0.0273 (11) |
C10 | 0.0268 (9) | 0.0536 (12) | 0.0556 (12) | 0.0086 (8) | 0.0088 (8) | 0.0301 (10) |
C11 | 0.0557 (14) | 0.0597 (14) | 0.0606 (14) | 0.0039 (11) | 0.0261 (11) | 0.0336 (12) |
C12 | 0.0378 (11) | 0.0424 (10) | 0.0424 (10) | 0.0088 (8) | 0.0112 (8) | 0.0212 (8) |
C13 | 0.0544 (13) | 0.0383 (10) | 0.0302 (9) | 0.0091 (9) | 0.0141 (8) | 0.0136 (8) |
C14 | 0.0553 (14) | 0.0507 (12) | 0.0479 (12) | 0.0100 (10) | 0.0176 (10) | 0.0289 (10) |
C15 | 0.0356 (12) | 0.0546 (13) | 0.0648 (14) | 0.0052 (9) | 0.0182 (10) | 0.0294 (11) |
C16 | 0.0445 (11) | 0.0442 (11) | 0.0380 (10) | 0.0153 (9) | 0.0083 (8) | 0.0214 (9) |
C17 | 0.0293 (9) | 0.0367 (9) | 0.0429 (10) | 0.0050 (7) | 0.0115 (8) | 0.0157 (8) |
C18 | 0.0387 (10) | 0.0392 (10) | 0.0361 (9) | 0.0050 (8) | 0.0134 (8) | 0.0181 (8) |
Cl1 | 0.0289 (3) | 0.0560 (3) | 0.0553 (3) | 0.0120 (2) | 0.0086 (2) | 0.0194 (3) |
F1 | 0.0956 (15) | 0.1158 (16) | 0.158 (2) | 0.0535 (13) | 0.0633 (15) | 0.1043 (16) |
F2 | 0.0924 (13) | 0.0893 (12) | 0.0793 (11) | 0.0075 (10) | 0.0537 (10) | 0.0245 (10) |
F3 | 0.0766 (12) | 0.1077 (14) | 0.0562 (9) | 0.0051 (10) | 0.0312 (8) | 0.0274 (9) |
F4 | 0.0410 (9) | 0.1444 (19) | 0.0804 (12) | −0.0076 (10) | 0.0008 (8) | 0.0552 (12) |
F5 | 0.0739 (11) | 0.0658 (10) | 0.0922 (12) | 0.0048 (8) | 0.0181 (9) | 0.0476 (9) |
F6 | 0.0484 (8) | 0.0654 (9) | 0.0676 (9) | −0.0062 (7) | 0.0112 (7) | 0.0228 (7) |
N1 | 0.0468 (10) | 0.0444 (9) | 0.0411 (9) | 0.0069 (8) | 0.0173 (7) | 0.0214 (7) |
N2 | 0.0316 (8) | 0.0391 (8) | 0.0376 (8) | 0.0087 (7) | 0.0065 (6) | 0.0178 (7) |
N3 | 0.0356 (9) | 0.0411 (9) | 0.0406 (9) | 0.0097 (7) | 0.0135 (7) | 0.0191 (7) |
N4 | 0.0304 (8) | 0.0377 (8) | 0.0397 (8) | 0.0072 (6) | 0.0109 (7) | 0.0187 (7) |
O1 | 0.0333 (10) | 0.0385 (10) | 0.0382 (10) | 0.0076 (8) | 0.0095 (8) | 0.0172 (8) |
P1 | 0.0379 (3) | 0.0613 (4) | 0.0485 (3) | 0.0062 (3) | 0.0134 (2) | 0.0296 (3) |
Fe1—O1 | 1.7969 (7) | C10—N2 | 1.474 (3) |
Fe1—N4 | 2.1173 (18) | C10—C17 | 1.511 (3) |
Fe1—N1 | 2.1254 (19) | C10—H10A | 0.9700 |
Fe1—N2 | 2.2223 (19) | C10—H10B | 0.9700 |
Fe1—N3 | 2.2798 (19) | C11—C14 | 1.368 (4) |
Fe1—Cl1 | 2.2923 (9) | C11—C15 | 1.379 (4) |
C1—C2 | 1.382 (4) | C11—H11 | 0.9300 |
C1—C13 | 1.388 (3) | C12—N4 | 1.338 (3) |
C1—H1 | 0.9300 | C12—C14 | 1.378 (3) |
C2—C4 | 1.356 (5) | C12—H12 | 0.9300 |
C2—H2 | 0.9300 | C13—N1 | 1.331 (3) |
C3—N2 | 1.487 (3) | C13—C16 | 1.503 (3) |
C3—C18 | 1.494 (3) | C14—H14 | 0.9300 |
C3—H3A | 0.9700 | C15—C17 | 1.376 (3) |
C3—H3B | 0.9700 | C15—H15 | 0.9300 |
C4—C5 | 1.374 (4) | C16—N2 | 1.488 (3) |
C4—H4 | 0.9300 | C16—H16A | 0.9700 |
C5—N1 | 1.352 (3) | C16—H16B | 0.9700 |
C5—H5 | 0.9300 | C17—N4 | 1.340 (3) |
C6—C9 | 1.372 (4) | C18—N3 | 1.343 (3) |
C6—C8 | 1.372 (4) | F1—P1 | 1.581 (2) |
C6—H6 | 0.9300 | F2—P1 | 1.5824 (18) |
C7—N3 | 1.340 (3) | F3—P1 | 1.5847 (18) |
C7—C9 | 1.379 (3) | F4—P1 | 1.5782 (19) |
C7—H7 | 0.9300 | F5—P1 | 1.5959 (17) |
C8—C18 | 1.380 (3) | F6—P1 | 1.6059 (17) |
C8—H8 | 0.9300 | O1—Fe1i | 1.7969 (7) |
C9—H9 | 0.9300 | ||
O1—Fe1—N4 | 90.93 (5) | N4—C12—H12 | 119.0 |
O1—Fe1—N1 | 92.68 (5) | C14—C12—H12 | 119.0 |
N4—Fe1—N1 | 154.66 (7) | N1—C13—C1 | 121.1 (2) |
O1—Fe1—N2 | 91.68 (6) | N1—C13—C16 | 116.61 (18) |
N4—Fe1—N2 | 78.42 (7) | C1—C13—C16 | 122.2 (2) |
N1—Fe1—N2 | 76.41 (7) | C11—C14—C12 | 118.3 (2) |
O1—Fe1—N3 | 166.76 (5) | C11—C14—H14 | 120.8 |
N4—Fe1—N3 | 82.06 (7) | C12—C14—H14 | 120.8 |
N1—Fe1—N3 | 89.03 (7) | C17—C15—C11 | 119.2 (2) |
N2—Fe1—N3 | 75.96 (7) | C17—C15—H15 | 120.4 |
O1—Fe1—Cl1 | 103.05 (5) | C11—C15—H15 | 120.4 |
N4—Fe1—Cl1 | 103.64 (5) | N2—C16—C13 | 110.29 (17) |
N1—Fe1—Cl1 | 99.94 (6) | N2—C16—H16A | 109.6 |
N2—Fe1—Cl1 | 165.03 (5) | C13—C16—H16A | 109.6 |
N3—Fe1—Cl1 | 89.56 (6) | N2—C16—H16B | 109.6 |
C2—C1—C13 | 118.2 (3) | C13—C16—H16B | 109.6 |
C2—C1—H1 | 120.9 | H16A—C16—H16B | 108.1 |
C13—C1—H1 | 120.9 | N4—C17—C15 | 120.9 (2) |
C1—C2—C4 | 120.7 (2) | N4—C17—C10 | 116.74 (18) |
C1—C2—H2 | 119.6 | C15—C17—C10 | 122.17 (19) |
C4—C2—H2 | 119.6 | N3—C18—C8 | 122.3 (2) |
N2—C3—C18 | 114.64 (17) | N3—C18—C3 | 117.46 (18) |
N2—C3—H3A | 108.6 | C8—C18—C3 | 120.20 (19) |
C18—C3—H3A | 108.6 | C13—N1—C5 | 119.9 (2) |
N2—C3—H3B | 108.6 | C13—N1—Fe1 | 114.83 (15) |
C18—C3—H3B | 108.6 | C5—N1—Fe1 | 124.38 (17) |
H3A—C3—H3B | 107.6 | C10—N2—C3 | 112.59 (18) |
C5—C4—C2 | 118.7 (3) | C10—N2—C16 | 112.68 (16) |
C5—C4—H4 | 120.7 | C3—N2—C16 | 109.10 (17) |
C2—C4—H4 | 120.7 | C10—N2—Fe1 | 104.81 (12) |
N1—C5—C4 | 121.4 (3) | C3—N2—Fe1 | 113.27 (13) |
N1—C5—H5 | 119.3 | C16—N2—Fe1 | 104.09 (12) |
C4—C5—H5 | 119.3 | C7—N3—C18 | 117.61 (18) |
C9—C6—C8 | 118.9 (2) | C7—N3—Fe1 | 126.10 (15) |
C9—C6—H6 | 120.5 | C18—N3—Fe1 | 115.74 (14) |
C8—C6—H6 | 120.5 | C12—N4—C17 | 119.66 (18) |
N3—C7—C9 | 123.0 (2) | C12—N4—Fe1 | 125.24 (14) |
N3—C7—H7 | 118.5 | C17—N4—Fe1 | 114.81 (14) |
C9—C7—H7 | 118.5 | Fe1—O1—Fe1i | 180.000 (17) |
C18—C8—C6 | 119.4 (2) | F3—P1—F1 | 90.06 (13) |
C18—C8—H8 | 120.3 | F3—P1—F4 | 91.04 (11) |
C6—C8—H8 | 120.3 | F1—P1—F4 | 91.70 (14) |
C6—C9—C7 | 118.8 (2) | F3—P1—F2 | 177.94 (12) |
C6—C9—H9 | 120.6 | F1—P1—F2 | 91.05 (12) |
C7—C9—H9 | 120.6 | F4—P1—F2 | 90.66 (12) |
N2—C10—C17 | 112.31 (17) | F3—P1—F5 | 89.67 (11) |
N2—C10—H10A | 109.1 | F1—P1—F5 | 178.99 (11) |
C17—C10—H10A | 109.1 | F4—P1—F5 | 89.27 (12) |
N2—C10—H10B | 109.1 | F2—P1—F5 | 89.19 (12) |
C17—C10—H10B | 109.1 | F3—P1—F6 | 88.48 (10) |
H10A—C10—H10B | 107.9 | F1—P1—F6 | 90.43 (12) |
C14—C11—C15 | 119.8 (2) | F4—P1—F6 | 177.81 (12) |
C14—C11—H11 | 120.1 | F2—P1—F6 | 89.78 (10) |
C15—C11—H11 | 120.1 | F5—P1—F6 | 88.59 (10) |
N4—C12—C14 | 122.0 (2) |
Symmetry code: (i) −x+2, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Fe2Cl2O(C18H18N4)2](PF6)2 |
Mr | 1069.27 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 8.5480 (17), 11.280 (2), 12.829 (3) |
α, β, γ (°) | 115.49 (3), 107.44 (3), 91.52 (3) |
V (Å3) | 1047.7 (4) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.99 |
Crystal size (mm) | 0.43 × 0.28 × 0.22 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.675, 0.811 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8741, 3903, 3622 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.606 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.107, 1.00 |
No. of reflections | 3903 |
No. of parameters | 287 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.35, −0.26 |
Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001).
In recent years, N-heterocycle ligands have been widely used as polydentate ligands which show various metal chelation reactions (Scapin et al., 1997; Okabe & Oya, 2000; Serre et al., 2005). In this paper, we report the structure of the title compound, (I).
As shown in Fig. 1, the FeIII atom is chelated by the tetradentate ligand of tris(2-pyridylmethyl)amine via four N atoms, and further bonded by one chloride ion and one bridging oxygen atom. Along the axial site, two FeIII atoms are linked into dimer via one oxygen atom (Fig. 2).