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The title compound, [Fe(C10H8N2)3][FeCl4]2, consists of a pseudo-octahedral tris(2,2'-bipyridyl)­iron(II) cation and two pseudo-tetrahedral tetra­chloro­ferrate(III) anions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802021773/ac6021sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802021773/ac6021Isup2.hkl
Contains datablock I

CCDC reference: 202310

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.043
  • wR factor = 0.072
  • Data-to-parameter ratio = 14.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 27 N1 -FE1 -N6 -C26 -44.00 1.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 28 N1 -FE1 -N6 -C30 143.00 1.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 37 N2 -FE1 -N4 -C16 -70.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 38 N2 -FE1 -N4 -C20 116.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 52 N3 -FE1 -N5 -C21 126.30 0.80 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 53 N3 -FE1 -N5 -C25 -52.10 0.90 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 62 N4 -FE1 -N2 -C6 -23.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 63 N4 -FE1 -N2 -C10 164.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 77 N5 -FE1 -N3 -C11 154.60 0.70 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 78 N5 -FE1 -N3 -C15 -28.90 0.90 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 87 N6 -FE1 -N1 -C1 131.00 1.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 88 N6 -FE1 -N1 -C5 -52.00 1.00 1.555 1.555 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
12 Alert Level C = Please check

Comment top

We are currently interested in the relationship between the structure of paramagnetic metal complexes and the paramagnetically shifted nuclear magnetic resonance spectra of these complexes (Ariyananda, L. M. D. & Norman, R. E., unpublished results). During an attempt to synthesize a bis(2,2'-bipyridyl)dichloroiron(III) complex as an example of a d5 cationic species, the title complex, (I), was produced.

The title complex consists of a pseudo-octahedral low-spin iron(II) complex and two tetrachloroferrate(III) anions. Given the eight chlorides charge neutrality requires the presence of one iron(II) and two iron(III) centers. The metrical parameters within the tris(2,2'-bipyridyl)iron(II) cation are typical for iron(II), with an average Fe—N distance of 1.964 (2) Å and an average `bite' angle of 81.75 (5)° (Batten et al., 2000; Decurtins et al., 1993). The metrical parameters within the 2,2'-bipyridyl unit are unremarkable. The identity as iron(II) is confirmed by the Fe—N distances and by the NMR spectrum (see Experimental), since the resonances, while broadened, are not paramagnetically shifted. The metrical parameters within the approximately tetrahedral tetrachloroferrate(III) ions are also typical, with an average Fe—Cl distance of 2.1946 (1) Å; the reported average for 97 structures is 2.18 (1) Å (Cotton et al., 1998, and references therein). Fe—Cl distances for [FeCl4]2− anions are typically longer than 2.3 Å (Alcock et al., 1999).

Experimental top

2,2'-Bipyridiyl (0.0625 g, 0.400 mmol) was dissolved in 10 ml of methanol. FeCl3·6H2O (0.0915 g, 0.202 mmol) was dissolved in another 10 ml of methanol. The iron solution was slowly added to the bipyridyl solution. The resultant solution was deep red, and was allowed to stand for one week before the volume was reduced by half via rotoevaporation. This solution was then placed in an ethyl acetate bath yielding dark red crystals after five days. Proton NMR on a D2O solution of the crystals gave four broadened peaks at 7.11, 7.26, 7.85 and 8.31 p.p.m..

Computing details top

Data collection: COLLECT (Nonius 2000); cell refinement: DENZO and SCALEPACK; data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: TEXSAN for Windows (Molecular Structure Corporation, 1997-1999); software used to prepare material for publication: TEXSAN for Windows.

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot of the tris-(2,2'-bipyridyl)iron(II) cation, with ellipsoids at the 50% probability level.
(I) top
Crystal data top
[Fe(C10H8N2)3][FeCl4]2F(000) = 1840.0
Mr = 919.72Dx = 1.668 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 13360 reflections
a = 18.6108 (4) Åθ = 2.5–30.0°
b = 10.7729 (2) ŵ = 1.79 mm1
c = 18.5661 (6) ÅT = 100 K
β = 100.381 (2)°Prism, dark red
V = 3661.43 (14) Å30.35 × 0.22 × 0.20 mm
Z = 4
Data collection top
Nonius KappaCCD (with Oxford Cryosystems Cryostream cooler)
diffractometer
10556 independent reflections
Radiation source: fine-focus sealed tube6113 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.054
ω scans with κ offsetsθmax = 30.0°, θmin = 2.5°
Absorption correction: multi-scan
HKL SCALEPACK (Otwinowski & Minor, 1997)
h = 2326
Tmin = 0.600, Tmax = 0.699k = 1315
50254 measured reflectionsl = 2326
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.072Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo) + 0.0004|Fo|2]
S = 0.92(Δ/σ)max < 0.001
6113 reflectionsΔρmax = 0.72 e Å3
424 parametersΔρmin = 0.55 e Å3
Crystal data top
[Fe(C10H8N2)3][FeCl4]2V = 3661.43 (14) Å3
Mr = 919.72Z = 4
Monoclinic, P21/cMo Kα radiation
a = 18.6108 (4) ŵ = 1.79 mm1
b = 10.7729 (2) ÅT = 100 K
c = 18.5661 (6) Å0.35 × 0.22 × 0.20 mm
β = 100.381 (2)°
Data collection top
Nonius KappaCCD (with Oxford Cryosystems Cryostream cooler)
diffractometer
10556 independent reflections
Absorption correction: multi-scan
HKL SCALEPACK (Otwinowski & Minor, 1997)
6113 reflections with I > 3σ(I)
Tmin = 0.600, Tmax = 0.699Rint = 0.054
50254 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0430 restraints
wR(F2) = 0.072H-atom parameters constrained
S = 0.92Δρmax = 0.72 e Å3
6113 reflectionsΔρmin = 0.55 e Å3
424 parameters
Special details top

Refinement. Refinement of F2. The weighted R-factor wR and goodness of fit are based on F2, conventional R-factors R are based on F. R-factors based on F2 are statistically about twice as large as those based on F.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.75386 (2)0.05888 (3)0.99014 (2)0.01572 (9)
Fe20.61693 (2)0.03489 (4)0.66489 (2)0.02168 (10)
Fe30.88302 (2)0.54248 (4)0.82609 (2)0.02373 (10)
Cl10.55849 (4)0.13717 (7)0.57039 (4)0.0372 (2)
Cl20.66129 (5)0.13581 (7)0.62506 (4)0.0356 (2)
Cl30.54023 (4)0.00386 (7)0.74024 (4)0.0305 (2)
Cl40.70593 (4)0.14879 (7)0.72311 (4)0.0301 (2)
Cl50.90394 (6)0.48621 (7)0.94071 (4)0.0448 (2)
Cl60.89092 (5)0.74431 (6)0.81280 (4)0.0337 (2)
Cl70.96732 (4)0.45352 (6)0.77338 (4)0.0266 (2)
Cl80.77522 (5)0.47679 (7)0.77280 (5)0.0443 (2)
N10.69408 (11)0.1980 (2)0.94529 (10)0.0165 (5)
N20.79939 (11)0.1919 (2)1.05526 (10)0.0162 (5)
N30.67552 (12)0.0184 (2)1.04435 (11)0.0192 (6)
N40.70384 (12)0.0695 (2)0.92338 (11)0.0188 (6)
N50.83083 (12)0.0819 (2)0.93264 (10)0.0175 (5)
N60.81968 (12)0.0745 (2)1.03467 (11)0.0182 (5)
C10.6372 (1)0.1907 (2)0.88873 (13)0.0202 (7)
C20.5957 (2)0.2930 (3)0.8629 (1)0.0250 (7)
C30.6126 (2)0.4066 (2)0.8955 (2)0.0268 (7)
C40.6712 (2)0.4162 (2)0.9524 (1)0.0233 (7)
C50.7106 (1)0.3107 (2)0.97675 (13)0.0177 (6)
C60.7731 (1)0.3080 (2)1.03804 (13)0.0172 (6)
C70.8041 (2)0.4122 (2)1.0744 (1)0.0215 (7)
C80.8643 (2)0.3993 (2)1.1293 (1)0.0238 (7)
C90.8920 (2)0.2818 (2)1.14680 (13)0.0221 (7)
C100.8577 (1)0.1810 (2)1.10958 (13)0.0194 (7)
C110.6630 (2)0.0736 (2)1.1059 (1)0.0231 (7)
C120.6048 (2)0.0420 (3)1.1388 (2)0.0277 (8)
C130.5569 (2)0.0489 (3)1.1072 (2)0.0308 (8)
C140.5684 (2)0.1058 (3)1.0441 (2)0.0273 (8)
C150.6275 (2)0.0711 (2)1.01319 (13)0.0206 (7)
C160.6463 (1)0.1245 (2)0.94602 (13)0.0206 (7)
C170.6087 (2)0.2223 (3)0.9075 (2)0.0313 (8)
C180.6304 (2)0.2648 (3)0.8448 (2)0.0359 (9)
C190.6896 (2)0.2113 (2)0.8221 (1)0.0257 (7)
C200.7248 (2)0.1132 (2)0.86242 (13)0.0214 (7)
C210.8338 (2)0.1714 (2)0.88278 (13)0.0209 (7)
C220.8894 (2)0.1781 (3)0.8428 (1)0.0265 (8)
C230.9449 (2)0.0921 (3)0.8546 (1)0.0263 (8)
C240.9425 (2)0.0009 (2)0.9062 (1)0.0236 (7)
C250.8854 (1)0.0038 (2)0.94384 (13)0.0175 (6)
C260.8768 (1)0.0970 (2)0.99965 (13)0.0180 (6)
C270.9215 (2)0.1997 (2)1.0167 (1)0.0225 (7)
C280.9107 (2)0.2784 (2)1.0729 (2)0.0256 (7)
C290.8549 (2)0.2517 (2)1.1103 (1)0.0253 (7)
C300.8105 (2)0.1507 (2)1.08964 (13)0.0220 (7)
H10.59770.08221.18250.033*
H20.55590.28510.82320.030*
H30.58410.47770.87900.032*
H40.68440.49440.97470.028*
H50.78410.49211.06170.026*
H60.88640.47001.15470.029*
H70.93390.27071.18380.026*
H80.87600.10031.12290.023*
H90.69550.13671.12750.028*
H100.62540.11260.86600.024*
H110.51640.07191.12900.037*
H120.53600.16861.02190.033*
H130.56840.25950.92420.038*
H140.60470.33070.81750.043*
H150.70600.24080.77960.031*
H160.76530.07540.84640.026*
H170.79620.23220.87480.025*
H180.88940.24180.80740.032*
H190.98400.09610.82820.032*
H200.98000.06180.91520.028*
H210.95950.21610.98990.027*
H220.94100.34901.08530.031*
H230.84720.30261.14990.030*
H240.77180.13421.11540.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0161 (2)0.0149 (2)0.0161 (2)0.0007 (2)0.0026 (1)0.00080 (13)
Fe20.0190 (2)0.0237 (2)0.0219 (2)0.0002 (2)0.0025 (2)0.0031 (2)
Fe30.0264 (2)0.0220 (2)0.0231 (2)0.0056 (2)0.0053 (2)0.0041 (2)
Cl10.0308 (4)0.0520 (5)0.0279 (4)0.0155 (4)0.0028 (3)0.0044 (3)
Cl20.0449 (5)0.0256 (4)0.0382 (4)0.0047 (4)0.0126 (4)0.0049 (3)
Cl30.0241 (4)0.0422 (4)0.0258 (3)0.0091 (3)0.0064 (3)0.0065 (3)
Cl40.0274 (4)0.0343 (4)0.0277 (4)0.0101 (3)0.0028 (3)0.0032 (3)
Cl50.0758 (7)0.0377 (4)0.0232 (4)0.0105 (4)0.0151 (4)0.0027 (3)
Cl60.0428 (5)0.0223 (4)0.0350 (4)0.0034 (3)0.0039 (3)0.0040 (3)
Cl70.0280 (4)0.0259 (4)0.0272 (3)0.0053 (3)0.0088 (3)0.0016 (3)
Cl80.0273 (4)0.0395 (5)0.0630 (6)0.0069 (4)0.0005 (4)0.0151 (4)
N10.0168 (12)0.0163 (10)0.0171 (10)0.0021 (9)0.0048 (9)0.0008 (8)
N20.0169 (12)0.0169 (10)0.0157 (10)0.0001 (9)0.0049 (9)0.0011 (8)
N30.0185 (12)0.0172 (11)0.0221 (11)0.0015 (9)0.0043 (9)0.0028 (8)
N40.0189 (12)0.0163 (10)0.0204 (11)0.0002 (10)0.0015 (9)0.0015 (8)
N50.0190 (12)0.0171 (10)0.0162 (10)0.0025 (9)0.0028 (9)0.0030 (8)
N60.0206 (12)0.0145 (10)0.0193 (10)0.0016 (9)0.0025 (9)0.0015 (8)
C10.020 (1)0.0205 (13)0.0201 (12)0.0040 (11)0.0025 (11)0.0001 (10)
C20.022 (2)0.028 (2)0.0234 (13)0.0016 (13)0.0019 (11)0.0039 (11)
C30.027 (2)0.022 (1)0.029 (1)0.0041 (13)0.0004 (12)0.0058 (11)
C40.027 (2)0.0180 (13)0.0242 (13)0.0010 (12)0.0037 (12)0.0019 (10)
C50.018 (1)0.0172 (12)0.0189 (12)0.0006 (11)0.0051 (11)0.0015 (9)
C60.017 (1)0.0188 (13)0.0170 (12)0.0010 (11)0.0056 (10)0.0025 (10)
C70.025 (2)0.0175 (13)0.0225 (13)0.0018 (12)0.0061 (11)0.0002 (10)
C80.027 (2)0.021 (1)0.0233 (13)0.0049 (12)0.0034 (12)0.0034 (10)
C90.021 (2)0.027 (1)0.0177 (12)0.0027 (12)0.0004 (11)0.0006 (10)
C100.020 (1)0.0216 (13)0.0176 (12)0.0024 (11)0.0044 (11)0.0006 (10)
C110.026 (2)0.0209 (13)0.0239 (13)0.0009 (12)0.0077 (12)0.0015 (11)
C120.030 (2)0.029 (2)0.028 (1)0.002 (1)0.0128 (13)0.0017 (12)
C130.024 (2)0.034 (2)0.037 (2)0.001 (1)0.0123 (13)0.0100 (13)
C140.024 (2)0.028 (2)0.031 (2)0.0038 (13)0.0060 (13)0.0036 (12)
C150.022 (1)0.0179 (13)0.0224 (13)0.0002 (11)0.0046 (11)0.0044 (10)
C160.021 (2)0.0187 (13)0.0217 (13)0.0033 (11)0.0018 (11)0.0023 (10)
C170.030 (2)0.028 (2)0.037 (2)0.013 (1)0.0092 (13)0.0007 (13)
C180.048 (2)0.025 (2)0.033 (2)0.012 (2)0.004 (2)0.0071 (12)
C190.032 (2)0.0207 (13)0.0230 (13)0.0006 (13)0.0008 (12)0.0025 (11)
C200.022 (2)0.0228 (13)0.0184 (12)0.0010 (12)0.0015 (11)0.0005 (10)
C210.024 (2)0.0185 (13)0.0203 (13)0.0040 (12)0.0049 (11)0.0003 (10)
C220.034 (2)0.024 (1)0.023 (1)0.0100 (13)0.0098 (13)0.0023 (11)
C230.026 (2)0.028 (2)0.028 (1)0.0116 (13)0.0142 (12)0.0105 (11)
C240.021 (2)0.023 (1)0.028 (1)0.0027 (12)0.0062 (12)0.0077 (11)
C250.016 (1)0.0186 (13)0.0174 (12)0.0032 (11)0.0013 (11)0.0061 (10)
C260.017 (1)0.0185 (13)0.0174 (12)0.0015 (11)0.0005 (11)0.0046 (10)
C270.020 (2)0.0205 (13)0.026 (1)0.0024 (12)0.0014 (11)0.0046 (11)
C280.026 (2)0.0179 (13)0.028 (1)0.0041 (12)0.0057 (12)0.0033 (11)
C290.033 (2)0.0176 (13)0.0234 (13)0.0017 (13)0.0007 (13)0.0004 (10)
C300.026 (2)0.0211 (13)0.0181 (12)0.0007 (12)0.0015 (11)0.0022 (10)
Geometric parameters (Å, º) top
Fe1—N11.960 (2)C8—H60.95
Fe1—N21.966 (2)C9—C101.380 (3)
Fe1—N31.964 (2)C9—H70.95
Fe1—N41.975 (2)C10—H80.95
Fe1—N51.950 (2)C11—C121.378 (4)
Fe1—N61.971 (2)C11—H90.95
FE2—CL12.1880 (8)C12—C131.382 (4)
FE2—CL22.1978 (8)C12—H10.95
FE2—CL32.2109 (8)C13—C141.373 (4)
FE2—CL42.1847 (7)C13—H110.95
FE3—CL52.1793 (8)C14—C151.379 (4)
FE3—CL62.1962 (8)C14—H120.95
FE3—CL72.2116 (8)C15—C161.472 (4)
FE3—CL82.1884 (9)C16—C171.390 (4)
N1—C11.353 (3)C17—C181.377 (4)
N1—C51.358 (3)C17—H130.95
N2—C61.360 (3)C18—C191.375 (4)
N2—C101.347 (3)C18—H140.95
N3—C111.345 (3)C19—C201.390 (4)
N3—C151.370 (3)C19—H150.95
N4—C161.355 (3)C20—H160.95
N4—C201.347 (3)C21—C221.380 (4)
N5—C211.345 (3)C21—H170.95
N5—C251.361 (3)C22—C231.375 (4)
N6—C261.363 (4)C22—H180.95
N6—C301.344 (3)C23—C241.392 (4)
C1—C21.381 (4)C23—H190.95
C1—H100.95C24—C251.373 (4)
C2—C31.376 (4)C24—H200.95
C2—H20.95C25—C261.472 (4)
C3—C41.380 (4)C26—C271.387 (4)
C3—H30.95C27—C281.387 (4)
C4—C51.384 (3)C27—H210.95
C4—H40.95C28—C291.378 (4)
C5—C61.473 (3)C28—H220.95
C6—C71.382 (3)C29—C301.379 (4)
C7—C81.379 (4)C29—H230.95
C7—H50.95C30—H240.95
C8—C91.383 (4)
Cl1···C4i3.345 (3)Cl6···C24v3.295 (3)
Cl1···C17ii3.549 (3)Cl7···C23vi3.457 (3)
Cl1···C3i3.599 (3)Cl7···C9i3.568 (3)
Cl2···C14iii3.472 (3)Cl8···C11i3.454 (3)
Cl3···C3iv3.576 (3)C14···C14vii3.587 (6)
Cl4···C213.459 (3)C23···C27viii3.331 (4)
Cl4···C13.566 (3)C23···C28viii3.430 (4)
Cl5···C73.452 (3)C24···C27viii3.438 (4)
Cl5···C28v3.515 (3)
N1—Fe1—N281.53 (8)C9—C8—H6120.5
N1—Fe1—N388.31 (9)C8—C9—C10118.9 (2)
N1—Fe1—N495.82 (8)C8—C9—H7120.6
N1—Fe1—N594.98 (9)C10—C9—H7120.6
N1—Fe1—N6176.24 (9)N2—C10—C9123.0 (2)
N2—Fe1—N397.13 (9)N2—C10—H8118.5
N2—Fe1—N4177.18 (9)C9—C10—H8118.5
N2—Fe1—N588.07 (9)N3—C11—C12122.5 (3)
N2—Fe1—N696.14 (8)N3—C11—H9118.7
N3—Fe1—N481.76 (9)C12—C11—H9118.7
N3—Fe1—N5174.21 (9)C11—C12—C13119.0 (3)
N3—Fe1—N694.92 (9)C11—C12—H1120.5
N4—Fe1—N593.16 (9)C13—C12—H1120.5
N4—Fe1—N686.55 (8)C12—C13—C14119.4 (3)
N5—Fe1—N681.95 (9)C12—C13—H11120.3
CL1—FE2—CL2108.31 (3)C14—C13—H11120.3
CL1—FE2—CL3108.55 (3)C13—C14—C15119.5 (3)
CL1—FE2—CL4109.69 (3)C13—C14—H12120.2
CL2—FE2—CL3112.29 (3)C15—C14—H12120.2
CL2—FE2—CL4109.82 (3)N3—C15—C14121.5 (3)
CL3—FE2—CL4108.14 (3)N3—C15—C16113.3 (2)
CL5—FE3—CL6112.41 (3)C14—C15—C16125.1 (2)
CL5—FE3—CL7107.18 (4)N4—C16—C15114.4 (2)
CL5—FE3—CL8109.84 (4)N4—C16—C17121.7 (3)
CL6—FE3—CL7108.19 (3)C15—C16—C17123.9 (3)
CL6—FE3—CL8110.11 (4)C16—C17—C18119.3 (3)
CL7—FE3—CL8109.00 (3)C16—C17—H13120.4
Fe1—N1—C1126.2 (2)C18—C17—H13120.4
Fe1—N1—C5115.7 (2)C17—C18—C19119.6 (3)
C1—N1—C5118.1 (2)C17—C18—H14120.2
Fe1—N2—C6115.4 (2)C19—C18—H14120.2
Fe1—N2—C10126.7 (2)C18—C19—C20118.6 (3)
C6—N2—C10117.6 (2)C18—C19—H15120.7
Fe1—N3—C11126.6 (2)C20—C19—H15120.7
Fe1—N3—C15115.3 (2)N4—C20—C19122.6 (3)
C11—N3—C15118.0 (2)N4—C20—H16118.7
Fe1—N4—C16114.9 (2)C19—C20—H16118.7
Fe1—N4—C20126.7 (2)N5—C21—C22122.4 (3)
C16—N4—C20118.2 (2)N5—C21—H17118.8
Fe1—N5—C21126.4 (2)C22—C21—H17118.8
Fe1—N5—C25115.6 (2)C21—C22—C23119.5 (3)
C21—N5—C25118.0 (2)C21—C22—H18120.2
Fe1—N6—C26114.1 (2)C23—C22—H18120.2
Fe1—N6—C30127.5 (2)C22—C23—C24118.6 (3)
C26—N6—C30118.1 (2)C22—C23—H19120.7
N1—C1—C2122.3 (2)C24—C23—H19120.7
N1—C1—H10118.9C23—C24—C25119.3 (3)
C2—C1—H10118.9C23—C24—H20120.3
C1—C2—C3119.2 (2)C25—C24—H20120.3
C1—C2—H2120.4N5—C25—C24122.1 (2)
C3—C2—H2120.4N5—C25—C26113.4 (2)
C2—C3—C4119.4 (2)C24—C25—C26124.5 (2)
C2—C3—H3120.3N6—C26—C25114.1 (2)
C4—C3—H3120.3N6—C26—C27121.4 (2)
C3—C4—C5119.2 (2)C25—C26—C27124.5 (3)
C3—C4—H4120.4C26—C27—C28119.8 (3)
C5—C4—H4120.4C26—C27—H21120.1
N1—C5—C4121.9 (2)C28—C27—H21120.1
N1—C5—C6113.6 (2)C27—C28—C29118.4 (3)
C4—C5—C6124.5 (2)C27—C28—H22120.8
N2—C6—C5113.6 (2)C29—C28—H22120.8
N2—C6—C7122.1 (2)C28—C29—C30119.5 (3)
C5—C6—C7124.3 (2)C28—C29—H23120.2
C6—C7—C8119.4 (2)C30—C29—H23120.2
C6—C7—H5120.3N6—C30—C29122.7 (3)
C8—C7—H5120.3N6—C30—H24118.6
C7—C8—C9119.0 (2)C29—C30—H24118.6
C7—C8—H6120.5
Fe1—N1—C1—C2176.6 (2)N4—C16—C15—C14175.6 (2)
Fe1—N1—C5—C4177.7 (2)N4—C16—C17—C180.2 (4)
Fe1—N1—C5—C62.0 (3)N4—C20—C19—C180.8 (4)
Fe1—N2—C6—C54.8 (3)N5—Fe1—N1—C195.8 (2)
Fe1—N2—C6—C7173.8 (2)N5—Fe1—N1—C586.9 (2)
Fe1—N2—C10—C9171.6 (2)N5—Fe1—N2—C692.4 (2)
Fe1—N3—C11—C12177.5 (2)N5—Fe1—N2—C1080.6 (2)
Fe1—N3—C15—C14177.9 (2)N5—Fe1—N3—C11154.6 (7)
Fe1—N3—C15—C162.8 (3)N5—Fe1—N3—C1528.9 (9)
Fe1—N4—C16—C155.0 (3)N5—Fe1—N4—C16174.4 (2)
Fe1—N4—C16—C17175.6 (2)N5—Fe1—N4—C200.2 (2)
Fe1—N4—C20—C19174.4 (2)N5—Fe1—N6—C268.7 (2)
Fe1—N5—C21—C22177.8 (2)N5—Fe1—N6—C30178.1 (2)
Fe1—N5—C25—C24178.7 (2)N5—C21—C22—C231.1 (4)
Fe1—N5—C25—C261.6 (2)N5—C25—C24—C230.2 (4)
Fe1—N6—C26—C2510.1 (3)N5—C25—C26—N65.6 (3)
Fe1—N6—C26—C27169.9 (2)N5—C25—C26—C27174.4 (2)
Fe1—N6—C30—C29171.1 (2)N6—Fe1—N1—C1131 (1)
N1—Fe1—N2—C62.9 (2)N6—Fe1—N1—C552 (1)
N1—Fe1—N2—C10175.9 (2)N6—Fe1—N2—C6174.1 (2)
N1—Fe1—N3—C1180.6 (2)N6—Fe1—N2—C101.1 (2)
N1—Fe1—N3—C1596.0 (2)N6—Fe1—N3—C1197.5 (2)
N1—Fe1—N4—C1690.2 (2)N6—Fe1—N3—C1585.9 (2)
N1—Fe1—N4—C2095.6 (2)N6—Fe1—N4—C1692.7 (2)
N1—Fe1—N5—C211.8 (2)N6—Fe1—N4—C2081.5 (2)
N1—Fe1—N5—C25176.6 (2)N6—Fe1—N5—C21176.1 (2)
N1—Fe1—N6—C2644 (1)N6—Fe1—N5—C255.6 (2)
N1—Fe1—N6—C30143 (1)N6—C26—C25—C24174.1 (2)
N1—C1—C2—C30.2 (4)N6—C26—C27—C283.2 (4)
N1—C5—C4—C31.3 (4)N6—C30—C29—C281.0 (4)
N1—C5—C6—N24.4 (3)C1—N1—C5—C40.1 (4)
N1—C5—C6—C7174.1 (3)C1—N1—C5—C6179.6 (2)
N2—Fe1—N1—C1177.0 (2)C1—C2—C3—C41.0 (5)
N2—Fe1—N1—C50.4 (2)C2—C1—N1—C50.6 (4)
N2—Fe1—N3—C110.7 (2)C2—C3—C4—C51.7 (4)
N2—Fe1—N3—C15177.2 (2)C3—C4—C5—C6178.4 (3)
N2—Fe1—N4—C1670 (2)C4—C5—C6—C76.2 (4)
N2—Fe1—N4—C20116 (2)C5—C6—N2—C10178.4 (2)
N2—Fe1—N5—C2179.6 (2)C5—C6—C7—C8177.5 (3)
N2—Fe1—N5—C25102.0 (2)C6—N2—C10—C91.3 (4)
N2—Fe1—N6—C2695.8 (2)C6—C7—C8—C90.2 (4)
N2—Fe1—N6—C3090.9 (2)C7—C6—N2—C100.2 (4)
N2—C6—C5—C4175.3 (3)C7—C8—C9—C101.1 (4)
N2—C6—C7—C80.9 (4)C11—N3—C15—C141.0 (4)
N2—C10—C9—C81.9 (4)C11—N3—C15—C16179.7 (2)
N3—Fe1—N1—C179.5 (2)C11—C12—C13—C140.1 (4)
N3—Fe1—N1—C597.8 (2)C12—C11—N3—C151.0 (4)
N3—Fe1—N2—C690.1 (2)C12—C13—C14—C150.1 (4)
N3—Fe1—N2—C1096.9 (2)C13—C14—C15—C16179.8 (3)
N3—Fe1—N4—C162.8 (2)C14—C15—C16—C173.8 (4)
N3—Fe1—N4—C20177.0 (2)C15—C16—N4—C20179.8 (2)
N3—Fe1—N5—C21126.3 (8)C15—C16—C17—C18179.5 (3)
N3—Fe1—N5—C2552.1 (9)C16—N4—C20—C190.4 (4)
N3—Fe1—N6—C26166.4 (2)C16—C17—C18—C191.0 (5)
N3—Fe1—N6—C306.8 (2)C17—C16—N4—C200.9 (4)
N3—C11—C12—C130.6 (4)C17—C18—C19—C201.5 (4)
N3—C15—C14—C130.5 (4)C21—N5—C25—C240.2 (3)
N3—C15—C16—N45.1 (3)C21—N5—C25—C26179.8 (2)
N3—C15—C16—C17175.5 (2)C21—C22—C23—C241.0 (4)
N4—Fe1—N1—C12.1 (2)C22—C21—N5—C250.5 (4)
N4—Fe1—N1—C5179.4 (2)C22—C23—C24—C250.3 (4)
N4—Fe1—N2—C623 (2)C23—C24—C25—C26179.9 (2)
N4—Fe1—N2—C10164 (2)C24—C25—C26—C276.0 (4)
N4—Fe1—N3—C11176.7 (2)C25—C26—N6—C30175.9 (2)
N4—Fe1—N3—C150.2 (2)C25—C26—C27—C28176.8 (2)
N4—Fe1—N5—C2197.9 (2)C26—N6—C30—C291.9 (4)
N4—Fe1—N5—C2580.5 (2)C26—C27—C28—C290.2 (4)
N4—Fe1—N6—C2685.0 (2)C27—C26—N6—C304.1 (3)
N4—Fe1—N6—C3088.2 (2)C27—C28—C29—C301.9 (4)
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x+1, y+1/2, z+3/2; (iii) x, y1/2, z1/2; (iv) x+1, y1/2, z+3/2; (v) x, y+1, z; (vi) x+2, y+1/2, z+3/2; (vii) x+1, y, z+2; (viii) x+2, y, z+2.

Experimental details

Crystal data
Chemical formula[Fe(C10H8N2)3][FeCl4]2
Mr919.72
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)18.6108 (4), 10.7729 (2), 18.5661 (6)
β (°) 100.381 (2)
V3)3661.43 (14)
Z4
Radiation typeMo Kα
µ (mm1)1.79
Crystal size (mm)0.35 × 0.22 × 0.20
Data collection
DiffractometerNonius KappaCCD (with Oxford Cryosystems Cryostream cooler)
diffractometer
Absorption correctionMulti-scan
HKL SCALEPACK (Otwinowski & Minor, 1997)
Tmin, Tmax0.600, 0.699
No. of measured, independent and
observed [I > 3σ(I)] reflections
50254, 10556, 6113
Rint0.054
(sin θ/λ)max1)0.704
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.043, 0.072, 0.92
No. of reflections6113
No. of parameters424
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.72, 0.55

Computer programs: COLLECT (Nonius 2000), DENZO and SCALEPACK (Otwinowski & Minor, 1997), SIR92 (Altomare et al., 1993), TEXSAN for Windows (Molecular Structure Corporation, 1997-1999), TEXSAN for Windows.

Selected geometric parameters (Å, º) top
Fe1—N11.960 (2)FE2—CL22.1978 (8)
Fe1—N21.966 (2)FE2—CL32.2109 (8)
Fe1—N31.964 (2)FE2—CL42.1847 (7)
Fe1—N41.975 (2)FE3—CL52.1793 (8)
Fe1—N51.950 (2)FE3—CL62.1962 (8)
Fe1—N61.971 (2)FE3—CL72.2116 (8)
FE2—CL12.1880 (8)FE3—CL82.1884 (9)
N1—Fe1—N281.53 (8)N2—Fe1—N696.14 (8)
N1—Fe1—N388.31 (9)N3—Fe1—N481.76 (9)
N1—Fe1—N495.82 (8)N3—Fe1—N5174.21 (9)
N1—Fe1—N594.98 (9)N3—Fe1—N694.92 (9)
N1—Fe1—N6176.24 (9)N4—Fe1—N593.16 (9)
N2—Fe1—N397.13 (9)N4—Fe1—N686.55 (8)
N2—Fe1—N4177.18 (9)N5—Fe1—N681.95 (9)
N2—Fe1—N588.07 (9)
 

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