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The title compound, [Fe(C10H8N2)3](ClO4)2, is isomorphous with the ZnII and RuII analogues. A twofold axis passes through the metal atom and the midpoint of the C-C bond joining the two pyridine rings of one of the bipyridyl ligands.
Supporting information
 | Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100009185/qa0337sup1.cif |
 | Structure factor file (CIF format) https://doi.org/10.1107/S0108270100009185/qa0337Isup2.hkl |
CCDC reference: 150375
S2. Experimental top
Crystals of the title compound were obtained inadvertently by slow evaporation of an ethanolic solution containing [Fe(bpm)2(H2O)2](ClO4)2 [bpm is bis(1-pyrazolyl)methane], 2,2'-bipyridine and sodium dicyanamide (yield 75%); satisfactory elemental analysis obtained.
Computing details top
Data collection: COLLECT (Hooft, 1998); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.
Tris(2,2'-bipyridyl-N,N')iron(II) diperchlorate top
Crystal data top
| [Fe(C10H8N2)3](ClO4)2 | F(000) = 1480 |
| Mr = 723.30 | Dx = 1.670 Mg m−3 |
| Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
| a = 17.0545 (10) Å | Cell parameters from 10435 reflections |
| b = 10.5812 (6) Å | θ = 3.4–28.3° |
| c = 15.9456 (7) Å | µ = 0.78 mm−1 |
| β = 91.332 (6)° | T = 150 K |
| V = 2876.7 (3) Å3 | Cube, dark red |
| Z = 4 | 0.5 × 0.5 × 0.38 mm |
Data collection top
| Nonius KappaCCD diffractometer | 1935 reflections with I > 2σ(I) |
| Radiation source: fine-focus sealed tube | Rint = 0.140 |
| Graphite monochromator | θmax = 28.3°, θmin = 3.4° |
| Detector resolution: 9 pixels mm-1 | h = −22→10 |
| ϕ and ω scans | k = −11→13 |
| 5238 measured reflections | l = −19→19 |
| 3049 independent reflections |
Refinement top
| 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)] = 0.061 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.137 | H-atom parameters constrained |
| S = 1.06 | Calculated w = 1/[σ2(Fo2) + (0.0497P)2 + 1.9714P] where P = (Fo2 + 2Fc2)/3 |
| 3049 reflections | (Δ/σ)max = 0.001 |
| 213 parameters | Δρmax = 0.66 e Å−3 |
| 0 restraints | Δρmin = −0.41 e Å−3 |
Crystal data top
| [Fe(C10H8N2)3](ClO4)2 | V = 2876.7 (3) Å3 |
| Mr = 723.30 | Z = 4 |
| Monoclinic, C2/c | Mo Kα radiation |
| a = 17.0545 (10) Å | µ = 0.78 mm−1 |
| b = 10.5812 (6) Å | T = 150 K |
| c = 15.9456 (7) Å | 0.5 × 0.5 × 0.38 mm |
| β = 91.332 (6)° |
Data collection top
| Nonius KappaCCD diffractometer | 1935 reflections with I > 2σ(I) |
| 5238 measured reflections | Rint = 0.140 |
| 3049 independent reflections |
Refinement top
| R[F2 > 2σ(F2)] = 0.061 | 0 restraints |
| wR(F2) = 0.137 | H-atom parameters constrained |
| S = 1.06 | Δρmax = 0.66 e Å−3 |
| 3049 reflections | Δρmin = −0.41 e Å−3 |
| 213 parameters |
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
| x | y | z | Uiso*/Ueq | ||
| Fe1 | 0.5000 | 0.52947 (7) | 0.7500 | 0.0155 (2) | |
| N11 | 0.40526 (19) | 0.5175 (3) | 0.81819 (17) | 0.0162 (7) | |
| C10 | 0.3858 (2) | 0.5909 (4) | 0.8836 (2) | 0.0220 (9) | |
| H10A | 0.4145 | 0.6665 | 0.8938 | 0.026* | |
| C11 | 0.3253 (2) | 0.5602 (4) | 0.9367 (2) | 0.0234 (10) | |
| H11A | 0.3133 | 0.6137 | 0.9825 | 0.028* | |
| C12 | 0.2831 (2) | 0.4517 (4) | 0.9223 (2) | 0.0227 (9) | |
| H12A | 0.2436 | 0.4264 | 0.9598 | 0.027* | |
| C13 | 0.2989 (2) | 0.3794 (4) | 0.8519 (2) | 0.0204 (9) | |
| H13A | 0.2686 | 0.3062 | 0.8392 | 0.024* | |
| C14 | 0.3594 (2) | 0.4156 (3) | 0.8007 (2) | 0.0172 (8) | |
| C15 | 0.3813 (2) | 0.3473 (3) | 0.7242 (2) | 0.0170 (8) | |
| C16 | 0.3387 (3) | 0.2459 (4) | 0.6921 (2) | 0.0227 (9) | |
| H16A | 0.2936 | 0.2158 | 0.7197 | 0.027* | |
| C17 | 0.3635 (3) | 0.1895 (4) | 0.6191 (2) | 0.0251 (9) | |
| H17A | 0.3354 | 0.1200 | 0.5956 | 0.030* | |
| C18 | 0.4297 (3) | 0.2355 (4) | 0.5809 (2) | 0.0226 (9) | |
| H18A | 0.4477 | 0.1980 | 0.5307 | 0.027* | |
| C19 | 0.4690 (2) | 0.3359 (3) | 0.6163 (2) | 0.0202 (9) | |
| H19A | 0.5147 | 0.3664 | 0.5900 | 0.024* | |
| N12 | 0.4452 (2) | 0.3937 (3) | 0.68763 (17) | 0.0161 (7) | |
| N21 | 0.45714 (19) | 0.6687 (3) | 0.68294 (18) | 0.0166 (7) | |
| C20 | 0.4166 (2) | 0.6593 (4) | 0.6096 (2) | 0.0198 (8) | |
| H20A | 0.3972 | 0.5789 | 0.5926 | 0.024* | |
| C21 | 0.4022 (3) | 0.7624 (4) | 0.5583 (2) | 0.0224 (9) | |
| H21A | 0.3743 | 0.7525 | 0.5065 | 0.027* | |
| C22 | 0.4287 (3) | 0.8797 (4) | 0.5833 (2) | 0.0236 (9) | |
| H22A | 0.4215 | 0.9510 | 0.5478 | 0.028* | |
| C23 | 0.4658 (3) | 0.8922 (4) | 0.6608 (2) | 0.0214 (9) | |
| H23A | 0.4817 | 0.9731 | 0.6807 | 0.026* | |
| C24 | 0.4793 (2) | 0.7857 (3) | 0.7090 (2) | 0.0165 (8) | |
| Cl1 | 0.32544 (6) | −0.00662 (9) | 0.86473 (5) | 0.0257 (3) | |
| O1 | 0.2490 (2) | 0.0520 (3) | 0.8632 (2) | 0.0462 (9) | |
| O2 | 0.3324 (2) | −0.0892 (3) | 0.93560 (18) | 0.0494 (10) | |
| O3 | 0.3849 (2) | 0.0900 (3) | 0.8729 (2) | 0.0468 (9) | |
| O4 | 0.3354 (2) | −0.0767 (3) | 0.78951 (17) | 0.0460 (9) |
Atomic displacement parameters (Å2) top
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Fe1 | 0.0145 (4) | 0.0171 (4) | 0.0150 (4) | 0.000 | 0.0015 (3) | 0.000 |
| N11 | 0.0166 (17) | 0.0192 (16) | 0.0127 (14) | 0.0024 (15) | 0.0002 (12) | −0.0015 (12) |
| C10 | 0.018 (2) | 0.024 (2) | 0.024 (2) | 0.0003 (18) | 0.0008 (17) | −0.0041 (16) |
| C11 | 0.020 (3) | 0.031 (2) | 0.0192 (19) | 0.0045 (18) | 0.0017 (17) | −0.0077 (16) |
| C12 | 0.015 (2) | 0.032 (2) | 0.0208 (18) | 0.0021 (18) | 0.0079 (16) | 0.0019 (17) |
| C13 | 0.015 (2) | 0.021 (2) | 0.025 (2) | −0.0019 (18) | 0.0010 (16) | 0.0023 (16) |
| C14 | 0.017 (2) | 0.0184 (19) | 0.0163 (17) | 0.0059 (17) | −0.0024 (15) | 0.0017 (14) |
| C15 | 0.013 (2) | 0.021 (2) | 0.0172 (18) | 0.0010 (17) | 0.0028 (15) | 0.0024 (15) |
| C16 | 0.021 (2) | 0.024 (2) | 0.0233 (19) | −0.0053 (18) | 0.0046 (16) | −0.0006 (16) |
| C17 | 0.026 (2) | 0.024 (2) | 0.026 (2) | −0.0075 (19) | 0.0040 (18) | −0.0088 (17) |
| C18 | 0.027 (3) | 0.021 (2) | 0.0197 (19) | 0.0027 (18) | −0.0022 (17) | −0.0025 (16) |
| C19 | 0.022 (2) | 0.020 (2) | 0.0187 (19) | 0.0018 (18) | 0.0014 (17) | −0.0015 (15) |
| N12 | 0.0143 (18) | 0.0196 (16) | 0.0146 (15) | 0.0027 (14) | 0.0024 (13) | 0.0008 (12) |
| N21 | 0.0106 (17) | 0.0201 (16) | 0.0192 (15) | −0.0001 (14) | 0.0006 (13) | −0.0009 (13) |
| C20 | 0.015 (2) | 0.022 (2) | 0.0220 (19) | −0.0014 (17) | −0.0033 (16) | −0.0024 (15) |
| C21 | 0.024 (3) | 0.027 (2) | 0.0164 (18) | 0.0038 (19) | −0.0009 (17) | 0.0010 (16) |
| C22 | 0.024 (2) | 0.028 (2) | 0.0188 (19) | 0.0055 (19) | 0.0008 (17) | 0.0055 (16) |
| C23 | 0.021 (2) | 0.019 (2) | 0.0235 (19) | 0.0023 (18) | 0.0027 (17) | 0.0027 (16) |
| C24 | 0.013 (2) | 0.020 (2) | 0.0169 (18) | −0.0019 (16) | 0.0010 (16) | −0.0042 (14) |
| Cl1 | 0.0245 (6) | 0.0344 (6) | 0.0182 (5) | 0.0051 (5) | 0.0017 (4) | −0.0019 (4) |
| O1 | 0.025 (2) | 0.053 (2) | 0.061 (2) | 0.0138 (18) | 0.0049 (16) | −0.0003 (17) |
| O2 | 0.065 (3) | 0.053 (2) | 0.0299 (17) | 0.014 (2) | 0.0026 (17) | 0.0145 (15) |
| O3 | 0.039 (2) | 0.0397 (19) | 0.062 (2) | −0.0065 (17) | −0.0058 (18) | −0.0068 (17) |
| O4 | 0.041 (2) | 0.073 (2) | 0.0237 (15) | 0.0004 (19) | 0.0061 (15) | −0.0210 (16) |
Geometric parameters (Å, º) top
| Fe1—N21 | 1.953 (3) | C16—C17 | 1.383 (5) |
| Fe1—N21i | 1.953 (3) | C17—C18 | 1.385 (6) |
| Fe1—N12 | 1.970 (3) | C18—C19 | 1.371 (5) |
| Fe1—N12i | 1.970 (3) | C19—N12 | 1.362 (4) |
| Fe1—N11 | 1.972 (3) | N21—C20 | 1.348 (5) |
| Fe1—N11i | 1.972 (3) | N21—C24 | 1.356 (5) |
| N11—C10 | 1.348 (5) | C20—C21 | 1.383 (5) |
| N11—C14 | 1.357 (5) | C21—C22 | 1.376 (6) |
| C10—C11 | 1.389 (5) | C22—C23 | 1.381 (6) |
| C11—C12 | 1.372 (5) | C23—C24 | 1.381 (5) |
| C12—C13 | 1.390 (5) | C24—C24i | 1.471 (7) |
| C13—C14 | 1.386 (5) | Cl1—O4 | 1.424 (3) |
| C14—C15 | 1.473 (5) | Cl1—O2 | 1.431 (3) |
| C15—N12 | 1.342 (5) | Cl1—O1 | 1.443 (3) |
| C15—C16 | 1.386 (5) | Cl1—O3 | 1.444 (4) |
| N21—Fe1—N21i | 82.01 (18) | N12—C15—C14 | 113.8 (3) |
| N21—Fe1—N12 | 96.12 (12) | C16—C15—C14 | 123.0 (3) |
| N21i—Fe1—N12 | 173.55 (13) | C17—C16—C15 | 118.5 (4) |
| N21—Fe1—N12i | 173.55 (13) | C16—C17—C18 | 119.1 (4) |
| N21i—Fe1—N12i | 96.12 (12) | C19—C18—C17 | 119.2 (3) |
| N12—Fe1—N12i | 86.40 (18) | N12—C19—C18 | 122.7 (4) |
| N21—Fe1—N11 | 92.82 (13) | C15—N12—C19 | 117.3 (3) |
| N21i—Fe1—N11 | 92.72 (12) | C15—N12—Fe1 | 115.4 (2) |
| N12—Fe1—N11 | 81.18 (13) | C19—N12—Fe1 | 127.0 (3) |
| N12i—Fe1—N11 | 93.43 (13) | C20—N21—C24 | 117.9 (3) |
| N21—Fe1—N11i | 92.72 (12) | C20—N21—Fe1 | 126.6 (3) |
| N21i—Fe1—N11i | 92.82 (13) | C24—N21—Fe1 | 115.0 (2) |
| N12—Fe1—N11i | 93.43 (13) | N21—C20—C21 | 122.4 (4) |
| N12i—Fe1—N11i | 81.18 (12) | C22—C21—C20 | 119.2 (4) |
| N11—Fe1—N11i | 172.65 (18) | C21—C22—C23 | 119.1 (4) |
| C10—N11—C14 | 117.8 (3) | C24—C23—C22 | 119.1 (4) |
| C10—N11—Fe1 | 127.5 (3) | N21—C24—C23 | 122.2 (3) |
| C14—N11—Fe1 | 114.4 (2) | N21—C24—C24i | 113.39 (19) |
| N11—C10—C11 | 122.5 (4) | C23—C24—C24i | 124.4 (2) |
| C12—C11—C10 | 119.2 (3) | O4—Cl1—O2 | 109.7 (2) |
| C11—C12—C13 | 119.1 (4) | O4—Cl1—O1 | 109.6 (2) |
| C14—C13—C12 | 119.0 (4) | O2—Cl1—O1 | 109.5 (2) |
| N11—C14—C13 | 122.1 (3) | O4—Cl1—O3 | 110.3 (2) |
| N11—C14—C15 | 113.9 (3) | O2—Cl1—O3 | 108.4 (2) |
| C13—C14—C15 | 124.0 (3) | O1—Cl1—O3 | 109.2 (2) |
| N12—C15—C16 | 123.2 (3) |
| Symmetry code: (i) −x+1, y, −z+3/2. |
Experimental details
| Crystal data | |
| Chemical formula | [Fe(C10H8N2)3](ClO4)2 |
| Mr | 723.30 |
| Crystal system, space group | Monoclinic, C2/c |
| Temperature (K) | 150 |
| a, b, c (Å) | 17.0545 (10), 10.5812 (6), 15.9456 (7) |
| β (°) | 91.332 (6) |
| V (Å3) | 2876.7 (3) |
| Z | 4 |
| Radiation type | Mo Kα |
| µ (mm−1) | 0.78 |
| Crystal size (mm) | 0.5 × 0.5 × 0.38 |
| Data collection | |
| Diffractometer | Nonius KappaCCD diffractometer |
| Absorption correction | – |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 5238, 3049, 1935 |
| Rint | 0.140 |
| (sin θ/λ)max (Å−1) | 0.666 |
| Refinement | |
| R[F2 > 2σ(F2)], wR(F2), S | 0.061, 0.137, 1.06 |
| No. of reflections | 3049 |
| No. of parameters | 213 |
| H-atom treatment | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 0.66, −0.41 |
Computer programs: COLLECT (Hooft, 1998), DENZO-SMN (Otwinowski & Minor, 1997), DENZO-SMN, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97.
Selected geometric parameters (Å, º) top
| Fe1—N21 | 1.953 (3) | Cl1—O2 | 1.431 (3) |
| Fe1—N12 | 1.970 (3) | Cl1—O1 | 1.443 (3) |
| Fe1—N11 | 1.972 (3) | Cl1—O3 | 1.444 (4) |
| Cl1—O4 | 1.424 (3) | ||
| N21—Fe1—N21i | 82.01 (18) | N12—Fe1—N11 | 81.18 (13) |
| N21—Fe1—N12 | 96.12 (12) | N12i—Fe1—N11 | 93.43 (13) |
| N21i—Fe1—N12 | 173.55 (13) | N21—Fe1—N11i | 92.72 (12) |
| N21—Fe1—N12i | 173.55 (13) | N21i—Fe1—N11i | 92.82 (13) |
| N21i—Fe1—N12i | 96.12 (12) | N12—Fe1—N11i | 93.43 (13) |
| N12—Fe1—N12i | 86.40 (18) | N12i—Fe1—N11i | 81.18 (12) |
| N21—Fe1—N11 | 92.82 (13) | N11—Fe1—N11i | 172.65 (18) |
| N21i—Fe1—N11 | 92.72 (12) |
| Symmetry code: (i) −x+1, y, −z+3/2. |
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The structure of [Fe(bipy)3](ClO4)2, (I) is isomorphous with the related RuII (Harrowfield & Sobolev, 1994; Krausz et al., 1995) and ZnII (Chen et al., 1995; Klement et al., 1995; Krausz et al., 1995) analogues. A twofold axis passes through the metal and the midpoint of the C—C bond joining the two pyridine rings of one of the bipyridine ligands. Thus, the asymmetric unit contains one metal on a special position, one perchlorate, and one and a half bipyridine ligands.