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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100009185/qa0337sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100009185/qa0337Isup2.hkl
Contains datablock I

CCDC reference: 150375

Comment top

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.

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)2F(000) = 1480
Mr = 723.30Dx = 1.670 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 17.0545 (10) ÅCell parameters from 10435 reflections
b = 10.5812 (6) Åθ = 3.4–28.3°
c = 15.9456 (7) ŵ = 0.78 mm1
β = 91.332 (6)°T = 150 K
V = 2876.7 (3) Å3Cube, dark red
Z = 40.5 × 0.5 × 0.38 mm
Data collection top
Nonius KappaCCD
diffractometer
1935 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.140
Graphite monochromatorθmax = 28.3°, θmin = 3.4°
Detector resolution: 9 pixels mm-1h = 2210
ϕ and ω scansk = 1113
5238 measured reflectionsl = 1919
3049 independent reflections
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)] = 0.061Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.137H-atom parameters constrained
S = 1.06Calculated w = 1/[σ2(Fo2) + (0.0497P)2 + 1.9714P]
where P = (Fo2 + 2Fc2)/3
3049 reflections(Δ/σ)max = 0.001
213 parametersΔρmax = 0.66 e Å3
0 restraintsΔρmin = 0.41 e Å3
Crystal data top
[Fe(C10H8N2)3](ClO4)2V = 2876.7 (3) Å3
Mr = 723.30Z = 4
Monoclinic, C2/cMo Kα radiation
a = 17.0545 (10) ŵ = 0.78 mm1
b = 10.5812 (6) ÅT = 150 K
c = 15.9456 (7) Å0.5 × 0.5 × 0.38 mm
β = 91.332 (6)°
Data collection top
Nonius KappaCCD
diffractometer
1935 reflections with I > 2σ(I)
5238 measured reflectionsRint = 0.140
3049 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0610 restraints
wR(F2) = 0.137H-atom parameters constrained
S = 1.06Δρmax = 0.66 e Å3
3049 reflectionsΔρmin = 0.41 e Å3
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
xyzUiso*/Ueq
Fe10.50000.52947 (7)0.75000.0155 (2)
N110.40526 (19)0.5175 (3)0.81819 (17)0.0162 (7)
C100.3858 (2)0.5909 (4)0.8836 (2)0.0220 (9)
H10A0.41450.66650.89380.026*
C110.3253 (2)0.5602 (4)0.9367 (2)0.0234 (10)
H11A0.31330.61370.98250.028*
C120.2831 (2)0.4517 (4)0.9223 (2)0.0227 (9)
H12A0.24360.42640.95980.027*
C130.2989 (2)0.3794 (4)0.8519 (2)0.0204 (9)
H13A0.26860.30620.83920.024*
C140.3594 (2)0.4156 (3)0.8007 (2)0.0172 (8)
C150.3813 (2)0.3473 (3)0.7242 (2)0.0170 (8)
C160.3387 (3)0.2459 (4)0.6921 (2)0.0227 (9)
H16A0.29360.21580.71970.027*
C170.3635 (3)0.1895 (4)0.6191 (2)0.0251 (9)
H17A0.33540.12000.59560.030*
C180.4297 (3)0.2355 (4)0.5809 (2)0.0226 (9)
H18A0.44770.19800.53070.027*
C190.4690 (2)0.3359 (3)0.6163 (2)0.0202 (9)
H19A0.51470.36640.59000.024*
N120.4452 (2)0.3937 (3)0.68763 (17)0.0161 (7)
N210.45714 (19)0.6687 (3)0.68294 (18)0.0166 (7)
C200.4166 (2)0.6593 (4)0.6096 (2)0.0198 (8)
H20A0.39720.57890.59260.024*
C210.4022 (3)0.7624 (4)0.5583 (2)0.0224 (9)
H21A0.37430.75250.50650.027*
C220.4287 (3)0.8797 (4)0.5833 (2)0.0236 (9)
H22A0.42150.95100.54780.028*
C230.4658 (3)0.8922 (4)0.6608 (2)0.0214 (9)
H23A0.48170.97310.68070.026*
C240.4793 (2)0.7857 (3)0.7090 (2)0.0165 (8)
Cl10.32544 (6)0.00662 (9)0.86473 (5)0.0257 (3)
O10.2490 (2)0.0520 (3)0.8632 (2)0.0462 (9)
O20.3324 (2)0.0892 (3)0.93560 (18)0.0494 (10)
O30.3849 (2)0.0900 (3)0.8729 (2)0.0468 (9)
O40.3354 (2)0.0767 (3)0.78951 (17)0.0460 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0145 (4)0.0171 (4)0.0150 (4)0.0000.0015 (3)0.000
N110.0166 (17)0.0192 (16)0.0127 (14)0.0024 (15)0.0002 (12)0.0015 (12)
C100.018 (2)0.024 (2)0.024 (2)0.0003 (18)0.0008 (17)0.0041 (16)
C110.020 (3)0.031 (2)0.0192 (19)0.0045 (18)0.0017 (17)0.0077 (16)
C120.015 (2)0.032 (2)0.0208 (18)0.0021 (18)0.0079 (16)0.0019 (17)
C130.015 (2)0.021 (2)0.025 (2)0.0019 (18)0.0010 (16)0.0023 (16)
C140.017 (2)0.0184 (19)0.0163 (17)0.0059 (17)0.0024 (15)0.0017 (14)
C150.013 (2)0.021 (2)0.0172 (18)0.0010 (17)0.0028 (15)0.0024 (15)
C160.021 (2)0.024 (2)0.0233 (19)0.0053 (18)0.0046 (16)0.0006 (16)
C170.026 (2)0.024 (2)0.026 (2)0.0075 (19)0.0040 (18)0.0088 (17)
C180.027 (3)0.021 (2)0.0197 (19)0.0027 (18)0.0022 (17)0.0025 (16)
C190.022 (2)0.020 (2)0.0187 (19)0.0018 (18)0.0014 (17)0.0015 (15)
N120.0143 (18)0.0196 (16)0.0146 (15)0.0027 (14)0.0024 (13)0.0008 (12)
N210.0106 (17)0.0201 (16)0.0192 (15)0.0001 (14)0.0006 (13)0.0009 (13)
C200.015 (2)0.022 (2)0.0220 (19)0.0014 (17)0.0033 (16)0.0024 (15)
C210.024 (3)0.027 (2)0.0164 (18)0.0038 (19)0.0009 (17)0.0010 (16)
C220.024 (2)0.028 (2)0.0188 (19)0.0055 (19)0.0008 (17)0.0055 (16)
C230.021 (2)0.019 (2)0.0235 (19)0.0023 (18)0.0027 (17)0.0027 (16)
C240.013 (2)0.020 (2)0.0169 (18)0.0019 (16)0.0010 (16)0.0042 (14)
Cl10.0245 (6)0.0344 (6)0.0182 (5)0.0051 (5)0.0017 (4)0.0019 (4)
O10.025 (2)0.053 (2)0.061 (2)0.0138 (18)0.0049 (16)0.0003 (17)
O20.065 (3)0.053 (2)0.0299 (17)0.014 (2)0.0026 (17)0.0145 (15)
O30.039 (2)0.0397 (19)0.062 (2)0.0065 (17)0.0058 (18)0.0068 (17)
O40.041 (2)0.073 (2)0.0237 (15)0.0004 (19)0.0061 (15)0.0210 (16)
Geometric parameters (Å, º) top
Fe1—N211.953 (3)C16—C171.383 (5)
Fe1—N21i1.953 (3)C17—C181.385 (6)
Fe1—N121.970 (3)C18—C191.371 (5)
Fe1—N12i1.970 (3)C19—N121.362 (4)
Fe1—N111.972 (3)N21—C201.348 (5)
Fe1—N11i1.972 (3)N21—C241.356 (5)
N11—C101.348 (5)C20—C211.383 (5)
N11—C141.357 (5)C21—C221.376 (6)
C10—C111.389 (5)C22—C231.381 (6)
C11—C121.372 (5)C23—C241.381 (5)
C12—C131.390 (5)C24—C24i1.471 (7)
C13—C141.386 (5)Cl1—O41.424 (3)
C14—C151.473 (5)Cl1—O21.431 (3)
C15—N121.342 (5)Cl1—O11.443 (3)
C15—C161.386 (5)Cl1—O31.444 (4)
N21—Fe1—N21i82.01 (18)N12—C15—C14113.8 (3)
N21—Fe1—N1296.12 (12)C16—C15—C14123.0 (3)
N21i—Fe1—N12173.55 (13)C17—C16—C15118.5 (4)
N21—Fe1—N12i173.55 (13)C16—C17—C18119.1 (4)
N21i—Fe1—N12i96.12 (12)C19—C18—C17119.2 (3)
N12—Fe1—N12i86.40 (18)N12—C19—C18122.7 (4)
N21—Fe1—N1192.82 (13)C15—N12—C19117.3 (3)
N21i—Fe1—N1192.72 (12)C15—N12—Fe1115.4 (2)
N12—Fe1—N1181.18 (13)C19—N12—Fe1127.0 (3)
N12i—Fe1—N1193.43 (13)C20—N21—C24117.9 (3)
N21—Fe1—N11i92.72 (12)C20—N21—Fe1126.6 (3)
N21i—Fe1—N11i92.82 (13)C24—N21—Fe1115.0 (2)
N12—Fe1—N11i93.43 (13)N21—C20—C21122.4 (4)
N12i—Fe1—N11i81.18 (12)C22—C21—C20119.2 (4)
N11—Fe1—N11i172.65 (18)C21—C22—C23119.1 (4)
C10—N11—C14117.8 (3)C24—C23—C22119.1 (4)
C10—N11—Fe1127.5 (3)N21—C24—C23122.2 (3)
C14—N11—Fe1114.4 (2)N21—C24—C24i113.39 (19)
N11—C10—C11122.5 (4)C23—C24—C24i124.4 (2)
C12—C11—C10119.2 (3)O4—Cl1—O2109.7 (2)
C11—C12—C13119.1 (4)O4—Cl1—O1109.6 (2)
C14—C13—C12119.0 (4)O2—Cl1—O1109.5 (2)
N11—C14—C13122.1 (3)O4—Cl1—O3110.3 (2)
N11—C14—C15113.9 (3)O2—Cl1—O3108.4 (2)
C13—C14—C15124.0 (3)O1—Cl1—O3109.2 (2)
N12—C15—C16123.2 (3)
Symmetry code: (i) x+1, y, z+3/2.

Experimental details

Crystal data
Chemical formula[Fe(C10H8N2)3](ClO4)2
Mr723.30
Crystal system, space groupMonoclinic, C2/c
Temperature (K)150
a, b, c (Å)17.0545 (10), 10.5812 (6), 15.9456 (7)
β (°) 91.332 (6)
V3)2876.7 (3)
Z4
Radiation typeMo Kα
µ (mm1)0.78
Crystal size (mm)0.5 × 0.5 × 0.38
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
5238, 3049, 1935
Rint0.140
(sin θ/λ)max1)0.666
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.061, 0.137, 1.06
No. of reflections3049
No. of parameters213
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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—N211.953 (3)Cl1—O21.431 (3)
Fe1—N121.970 (3)Cl1—O11.443 (3)
Fe1—N111.972 (3)Cl1—O31.444 (4)
Cl1—O41.424 (3)
N21—Fe1—N21i82.01 (18)N12—Fe1—N1181.18 (13)
N21—Fe1—N1296.12 (12)N12i—Fe1—N1193.43 (13)
N21i—Fe1—N12173.55 (13)N21—Fe1—N11i92.72 (12)
N21—Fe1—N12i173.55 (13)N21i—Fe1—N11i92.82 (13)
N21i—Fe1—N12i96.12 (12)N12—Fe1—N11i93.43 (13)
N12—Fe1—N12i86.40 (18)N12i—Fe1—N11i81.18 (12)
N21—Fe1—N1192.82 (13)N11—Fe1—N11i172.65 (18)
N21i—Fe1—N1192.72 (12)
Symmetry code: (i) x+1, y, z+3/2.
 

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