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The title compound, μ-oxo-bis­[bispicMe2enFeCl](ClO4)2·0.751H2O [bispicMe2en = N,N′-di­methyl-N,N′-bis(2-pyridyl­methyl)­ethane-1,2-di­amine] or [Fe2Cl2O(C16H22N4)2](ClO4)2·0.751H2O, contains a complex dinuclear cation in which two Fe atoms are linked by a μ-oxo bridge. Each Fe atom is octahedrally coordinated by the bridging O atom, four N atoms of the bispicMe2en ligand and a Cl atom. The Fe...Fe distance is 3.623 (1) Å; the Fe—O distances are 1.811 (1) and 1.814 (1) Å; the Fe—Npyridine distances vary between 2.156 (2) and 2.169 (2) Å (mean value 2.163 Å) and are considerably shorter than the Fe—Namine distances which fall into two categories, viz. Fe—N = 2.284 (2) and 2.296 (2) Å for the N atoms trans to the bridging O atom, and 2.219 (2) and 2.227 (2) Å for those trans to Cl. The Fe—Cl distances are 2.324 (1) and 2.334 (1) Å. The geometry is compared to that in related complexes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801020542/ya6079sup1.cif
Contains datablocks rune2, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801020542/ya6079Isup2.hkl
Contains datablock I

CCDC reference: 180514

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.003 Å
  • Disorder in solvent or counterion
  • R factor = 0.032
  • wR factor = 0.034
  • Data-to-parameter ratio = 16.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
PLAT_420 Alert B D-H Without Acceptor >O10 - >HO10A ?
Yellow Alert Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 36.00 Perc.
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

The structure of the title complex dinuclear cation (Fig. 1) shows that the two Fe atoms are linked by a µ-oxo bridge; each Fe atom is octahedrally coordinated by the bridging O atom, four N atoms of the bispicMe2en ligand and a Cl atom. The Fe···Fe distance is 3.623 (1) Å; the Fe—O distances are 1.811 (1) and 1.814 (1) Å; Fe—Npyridine distances vary between 2.156 (2) and 2.169 (2) Å (mean 2.163 Å) and are considerably shorter than the Fe—Namine distances which fall into two categories, viz. Fe—N = 2.284 (2) and 2.296 (2) Å for the N atoms trans to the bridging O atom, and 2.219 (2) and 2.227 (2) Å for those trans to Cl. The Fe—Cl distances are 2.324 (1) and 2.334 (1) Å. These distances are similar to those found in the corresponding bispicen complex (2) (see Scheme; Arulsamy et al., 1993) and in the bispicMeen (3) and the trispicMeen (4) complexes (Nivorozhkin et al., 1997). The main differences in the geometries of these compounds are in the angle at the bridging O atom and the orientation of the ligands about the Fe—Fe axis. The Fe—O—Fe angles are 176.43 (8)° in (1), 180.0° in (2) (the O atom is in a special position in the inversion centre), 152.3 (3)° in (3) (the O atom is on a twofold axis) and 177.4 (7)° in (4). The Cl—Fe···Fe—Cl pseudo-torsion angles are 128.21 (2)° in (1), 180.0° in (2), 110.2° in (3) and 141.0° in (4).

The crystals pack with the cations lying in the xy planes at z 0 or 1/2 which accounts for the crystals growing as needles parallel to the c axis.

The near linearity of the Fe—O—Fe angle in (1) is in agreement with the prediction based on the observed νsym(Fe—O—Fe) in the resonance-Raman spectrum (Hazell et al., 1995). However, this resonance Raman result was not entirely corroborated by magnetic susceptibility measurements (Hazell et al., 1995). Usually strong magnetic exchange coupling is observed for oxo-bridged diiron(III) complexes. The structural characterization now reported sheds some light on this apparent inconsistency. The Fe—O distances in (1) are significantly longer than those found in most singly bridged µ-oxo-diiron(III) units, the mean Fe—O distance, from the Cambridge Structural database (April 2001 release; Allen & Kennard, 1993) is 1.775 Å with an s.u. of 0.001 Å, the three longest Fe—O distances, out of 162 entries are between 1.811 and 1.815 Å, cf. 1.811 and 1.814 Å found for (1). Thus, a markedly weaker exchange coupling for this particular group is consistent with the observed geometry. The electronegative chloride ions cis to the µ-oxo group and the Cl—Fe···Fe—Cl pseudo-torsion angle will influence the Fe—O bond length and consequent overlap integral of the magnetic orbitals.

Experimental top

Red crystals of the title compound (1) were prepared by the method described by Hazell et al. (1995).

Refinement top

The H atoms of the ligand were constrained to have C—H = 0.95 Å and Uiso = 1.2Ueq for the atom to which they are attached. The H atoms of the water molecules O10 were obtained from a difference map and kept fixed. One of the perchlorate ions (with the central Cl4 atom) was disordered, appearing on the Fourier map as a very anisotropic heavy atom surrounded by six light atoms, and was modelled as two interpenetrating perchlorate ions which were constrained to have regular tetrahedral geometry with all Cl—O distances the same. Site-occupation factors for the two ions were set, arbitrarily, to be 0.5. The site-occupation factor for the water molecule was refined and found to be 0.751 (5).

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1997) and KRYSTAL (Hazell, 1995); program(s) used to refine structure: modified ORFLS (Busing et al., 1962) and KRYSTAL; molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and KRYSTAL; software used to prepare material for publication: KRYSTAL.

Figures top
[Figure 1] Fig. 1. View of the title cation showing the labelling of the non-H atoms. Displacement ellipsoids are shown at 50% probability levels; H atoms have been omitted.
(I) top
Crystal data top
[Fe2Cl2O(C16H22N4)2](ClO4)2·0.751H2OF(000) = 1966.04
Mr = 951.83Dx = 1.572 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ycCell parameters from 8666 reflections
a = 13.632 (3) Åθ = 2.3–30.5°
b = 17.956 (4) ŵ = 1.05 mm1
c = 16.489 (3) ÅT = 120 K
β = 94.938 (4)°Needle, red
V = 4021 (1) Å30.50 × 0.13 × 0.12 mm
Z = 4
Data collection top
Siemens SMART CCD
diffractometer
12123 independent reflections
Radiation source: x-ray tube8461 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.042
ω rotation scans with narrow framesθmax = 30.5°, θmin = 2.3°
Absorption correction: integration
(XPREP; Siemens, 1995)
h = 1918
Tmin = 0.647, Tmax = 0.899k = 2524
45381 measured reflectionsl = 2223
Refinement top
Refinement on F0 restraints
Least-squares matrix: full1 constraint
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.034 w = 1/{[σcs(F2) + B + (1 + A)F2]1/2-|F|}2,
where A = 0.03, B = 0.10
S = 0.88(Δ/σ)max = 0.001
8461 reflectionsΔρmax = 0.72 (8) e Å3
521 parametersΔρmin = 0.51 (8) e Å3
Crystal data top
[Fe2Cl2O(C16H22N4)2](ClO4)2·0.751H2OV = 4021 (1) Å3
Mr = 951.83Z = 4
Monoclinic, P21/cMo Kα radiation
a = 13.632 (3) ŵ = 1.05 mm1
b = 17.956 (4) ÅT = 120 K
c = 16.489 (3) Å0.50 × 0.13 × 0.12 mm
β = 94.938 (4)°
Data collection top
Siemens SMART CCD
diffractometer
12123 independent reflections
Absorption correction: integration
(XPREP; Siemens, 1995)
8461 reflections with I > 3σ(I)
Tmin = 0.647, Tmax = 0.899Rint = 0.042
45381 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0320 restraints
wR(F2) = 0.034H-atom parameters constrained
S = 0.88Δρmax = 0.72 (8) e Å3
8461 reflectionsΔρmin = 0.51 (8) e Å3
521 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Fe10.61790 (2)0.23117 (1)0.47934 (2)0.0142 (1)
Fe20.88440 (2)0.22588 (1)0.50562 (2)0.0137 (1)
Cl10.57692 (4)0.18339 (3)0.60298 (3)0.0222 (2)
Cl20.91849 (3)0.16269 (3)0.38755 (3)0.0189 (2)
O10.7513 (1)0.23165 (7)0.49289 (7)0.0156 (6)
N10.5972 (1)0.34514 (9)0.51623 (10)0.0195 (8)
N20.6143 (1)0.29613 (9)0.36461 (9)0.0181 (8)
N30.4553 (1)0.22114 (9)0.43131 (10)0.0200 (8)
N40.6020 (1)0.12359 (9)0.42168 (10)0.0206 (8)
N50.9157 (1)0.33305 (9)0.45299 (10)0.0179 (8)
N60.8967 (1)0.30488 (9)0.61008 (9)0.0193 (8)
N71.0454 (1)0.21039 (9)0.55344 (10)0.0189 (8)
N80.8897 (1)0.12447 (9)0.57680 (9)0.0186 (8)
C10.5687 (1)0.3677 (1)0.5888 (1)0.025 (1)
C20.5748 (2)0.4411 (1)0.6133 (1)0.033 (1)
C30.6104 (2)0.4933 (1)0.5620 (2)0.033 (1)
C40.6367 (1)0.4715 (1)0.4866 (1)0.028 (1)
C50.6296 (1)0.3967 (1)0.4652 (1)0.021 (1)
C60.6623 (1)0.3679 (1)0.3869 (1)0.023 (1)
C70.6699 (2)0.2586 (1)0.3034 (1)0.026 (1)
C80.5103 (1)0.3098 (1)0.3317 (1)0.022 (1)
C90.4488 (1)0.2416 (1)0.3436 (1)0.023 (1)
C100.3853 (1)0.2670 (1)0.4736 (1)0.027 (1)
C110.4292 (1)0.1419 (1)0.4387 (1)0.027 (1)
C120.5114 (1)0.0932 (1)0.4141 (1)0.024 (1)
C130.4961 (2)0.0212 (1)0.3856 (2)0.034 (1)
C140.5749 (2)0.0204 (1)0.3638 (2)0.038 (1)
C150.6678 (2)0.0112 (1)0.3708 (1)0.033 (1)
C160.6791 (2)0.0831 (1)0.4005 (1)0.025 (1)
C170.9439 (1)0.3439 (1)0.3777 (1)0.021 (1)
C180.9427 (2)0.4131 (1)0.3415 (1)0.026 (1)
C190.9122 (2)0.4740 (1)0.3846 (1)0.028 (1)
C200.8868 (1)0.4641 (1)0.4630 (1)0.025 (1)
C210.8888 (1)0.3927 (1)0.4958 (1)0.019 (1)
C220.8556 (1)0.3764 (1)0.5786 (1)0.022 (1)
C230.8390 (2)0.2794 (1)0.6768 (1)0.026 (1)
C241.0026 (1)0.3147 (1)0.6395 (1)0.023 (1)
C251.0562 (1)0.2412 (1)0.6376 (1)0.022 (1)
C261.1193 (1)0.2450 (1)0.5041 (1)0.026 (1)
C271.0634 (1)0.1292 (1)0.5567 (1)0.022 (1)
C280.9771 (1)0.0888 (1)0.5869 (1)0.020 (1)
C290.9859 (2)0.0184 (1)0.6214 (1)0.025 (1)
C300.9033 (2)0.0159 (1)0.6468 (1)0.026 (1)
C310.8136 (2)0.0212 (1)0.6385 (1)0.026 (1)
C320.8095 (1)0.0908 (1)0.6027 (1)0.023 (1)
Cl30.70397 (4)0.61278 (3)0.31004 (3)0.0273 (3)
O20.6623 (2)0.5405 (1)0.2916 (1)0.056 (1)
O30.6259 (1)0.6647 (1)0.3194 (1)0.047 (1)
O40.7602 (1)0.6359 (1)0.2452 (1)0.054 (1)
O50.7650 (1)0.6092 (1)0.3850 (1)0.052 (1)
Cl4a0.7985 (2)0.8915 (1)0.1886 (1)0.027 (1)0.5
O6a0.6968 (2)0.8895 (3)0.2056 (1)0.032 (1)0.5
O7a0.8075 (2)0.9313 (2)0.1139 (2)0.040 (3)0.5
O8a0.8556 (2)0.9286 (2)0.2541 (2)0.045 (2)0.5
O9a0.8343 (3)0.8167 (1)0.1809 (2)0.045 (2)0.5
Cl4b0.8017 (2)0.9086 (1)0.1822 (1)0.027 (1)0.5
O6b0.7000 (2)0.8971 (2)0.1960 (2)0.032 (1)0.5
O7b0.8346 (3)0.9787 (2)0.2170 (2)0.066 (3)0.5
O8b0.8603 (3)0.8492 (2)0.2197 (3)0.084 (4)0.5
O9b0.8118 (3)0.9092 (2)0.0960 (1)0.042 (3)0.5
O100.6891 (2)0.8185 (1)0.3539 (1)0.035 (1)0.751 (5)
HO10a0.69890.83710.30400.050*0.751 (5)
HO10b0.66820.77140.34070.050*0.751 (5)
H10.54360.33190.62400.030*
H20.55480.45550.66480.040*
H30.61680.54390.57840.040*
H40.65930.50710.44990.034*
H6a0.64570.40310.34500.028*
H6b0.73170.36090.39270.028*
H7a0.63900.21240.28900.031*
H7b0.73560.24990.32550.031*
H7c0.67050.28910.25640.031*
H8a0.50870.32090.27530.027*
H8b0.48450.35070.35960.027*
H9a0.38210.25170.32530.028*
H9b0.47220.20150.31310.028*
H10a0.38950.25400.52970.032*
H10b0.32030.25840.45010.032*
H10c0.40130.31820.46840.032*
H11a0.37120.13180.40430.032*
H11b0.41760.13150.49360.032*
H130.43170.00060.38110.041*
H140.56550.06990.34430.046*
H150.72310.01600.35550.040*
H160.74300.10450.40610.030*
H170.96540.30230.34840.025*
H180.96240.41900.28800.032*
H190.90880.52200.36030.034*
H200.86820.50550.49420.031*
H22a0.87730.41520.61500.026*
H22b0.78580.37380.57480.026*
H23a0.86550.23340.69700.031*
H23b0.77210.27280.65680.031*
H23c0.84300.31540.71920.031*
H24a1.00710.33310.69370.028*
H24b1.03200.34930.60530.028*
H25a1.12410.24860.65400.027*
H25b1.02910.20720.67380.027*
H26a1.11240.22540.45040.031*
H26b1.18360.23460.52830.031*
H26c1.10940.29740.50210.031*
H27a1.12030.11950.59240.027*
H27b1.07360.11180.50370.027*
H291.04800.00590.62740.030*
H300.90770.06440.66990.032*
H310.75630.00090.65700.031*
H320.74800.11590.59600.028*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0126 (1)0.0166 (1)0.0130 (1)0.0005 (1)0.0006 (1)0.0002 (1)
Fe20.0127 (1)0.0145 (1)0.0138 (1)0.0002 (1)0.0006 (1)0.0016 (1)
Cl10.0197 (2)0.0305 (2)0.0164 (2)0.0041 (2)0.0011 (2)0.0047 (2)
Cl20.0205 (2)0.0186 (2)0.0175 (2)0.0040 (2)0.0005 (2)0.0018 (2)
O10.0143 (5)0.0162 (6)0.0160 (6)0.0004 (5)0.0002 (4)0.0005 (5)
N10.0159 (8)0.0220 (8)0.0204 (8)0.0018 (6)0.0001 (6)0.0029 (6)
N20.0149 (7)0.0232 (8)0.0162 (7)0.0038 (6)0.0012 (6)0.0014 (6)
N30.0162 (8)0.0241 (8)0.0194 (7)0.0004 (6)0.0003 (6)0.0007 (6)
N40.0188 (8)0.0201 (8)0.0221 (8)0.0019 (6)0.0034 (6)0.0017 (6)
N50.0161 (7)0.0175 (7)0.0199 (8)0.0003 (6)0.0009 (6)0.0005 (6)
N60.0168 (7)0.0238 (8)0.0170 (7)0.0033 (6)0.0001 (6)0.0009 (6)
N70.0153 (7)0.0211 (8)0.0201 (8)0.0006 (6)0.0004 (6)0.0032 (6)
N80.0170 (8)0.0187 (8)0.0195 (8)0.0010 (6)0.0018 (6)0.0040 (6)
C10.019 (1)0.033 (1)0.024 (1)0.004 (1)0.001 (1)0.007 (1)
C20.026 (1)0.039 (1)0.033 (1)0.009 (1)0.005 (1)0.017 (1)
C30.024 (1)0.024 (1)0.050 (1)0.005 (1)0.010 (1)0.013 (1)
C40.017 (1)0.022 (1)0.044 (1)0.002 (1)0.004 (1)0.001 (1)
C50.013 (1)0.022 (1)0.027 (1)0.002 (1)0.002 (1)0.000 (1)
C60.018 (1)0.025 (1)0.025 (1)0.000 (1)0.001 (1)0.007 (1)
C70.023 (1)0.038 (1)0.017 (1)0.010 (1)0.004 (1)0.002 (1)
C80.018 (1)0.031 (1)0.018 (1)0.007 (1)0.002 (1)0.003 (1)
C90.018 (1)0.031 (1)0.019 (1)0.004 (1)0.005 (1)0.003 (1)
C100.016 (1)0.037 (1)0.026 (1)0.002 (1)0.003 (1)0.000 (1)
C110.017 (1)0.030 (1)0.032 (1)0.006 (1)0.002 (1)0.000 (1)
C120.020 (1)0.024 (1)0.026 (1)0.005 (1)0.006 (1)0.001 (1)
C130.027 (1)0.027 (1)0.046 (1)0.009 (1)0.006 (1)0.004 (1)
C140.038 (1)0.022 (1)0.052 (2)0.005 (1)0.010 (1)0.010 (1)
C150.032 (1)0.023 (1)0.043 (1)0.003 (1)0.003 (1)0.008 (1)
C160.022 (1)0.023 (1)0.030 (1)0.001 (1)0.002 (1)0.004 (1)
C170.019 (1)0.023 (1)0.022 (1)0.000 (1)0.004 (1)0.004 (1)
C180.022 (1)0.030 (1)0.028 (1)0.001 (1)0.004 (1)0.011 (1)
C190.025 (1)0.020 (1)0.039 (1)0.003 (1)0.001 (1)0.010 (1)
C200.021 (1)0.019 (1)0.037 (1)0.001 (1)0.002 (1)0.002 (1)
C210.015 (1)0.018 (1)0.024 (1)0.001 (1)0.001 (1)0.001 (1)
C220.021 (1)0.022 (1)0.022 (1)0.001 (1)0.000 (1)0.004 (1)
C230.025 (1)0.036 (1)0.017 (1)0.004 (1)0.004 (1)0.002 (1)
C240.018 (1)0.027 (1)0.024 (1)0.004 (1)0.003 (1)0.003 (1)
C250.018 (1)0.028 (1)0.020 (1)0.004 (1)0.005 (1)0.001 (1)
C260.016 (1)0.034 (1)0.028 (1)0.002 (1)0.003 (1)0.005 (1)
C270.018 (1)0.024 (1)0.024 (1)0.005 (1)0.001 (1)0.004 (1)
C280.022 (1)0.021 (1)0.018 (1)0.001 (1)0.003 (1)0.000 (1)
C290.026 (1)0.022 (1)0.025 (1)0.006 (1)0.003 (1)0.003 (1)
C300.033 (1)0.019 (1)0.026 (1)0.000 (1)0.003 (1)0.006 (1)
C310.025 (1)0.025 (1)0.027 (1)0.004 (1)0.001 (1)0.006 (1)
C320.019 (1)0.024 (1)0.025 (1)0.002 (1)0.001 (1)0.005 (1)
Cl30.0260 (3)0.0258 (3)0.0297 (3)0.0036 (2)0.0003 (2)0.0038 (2)
O20.072 (1)0.047 (1)0.050 (1)0.027 (1)0.002 (1)0.008 (1)
O30.042 (1)0.060 (1)0.039 (1)0.025 (1)0.010 (1)0.014 (1)
O40.059 (1)0.043 (1)0.067 (1)0.001 (1)0.039 (1)0.002 (1)
O50.049 (1)0.043 (1)0.058 (1)0.006 (1)0.029 (1)0.000 (1)
O6a0.021 (1)0.046 (1)0.030 (1)0.006 (1)0.002 (1)0.016 (1)
Cl4a0.0215 (3)0.0366 (10)0.027 (4)0.0057 (5)0.0018 (3)0.0128 (5)
O7a0.033 (2)0.060 (3)0.030 (2)0.017 (2)0.018 (2)0.021 (2)
O8a0.025 (2)0.068 (3)0.041 (2)0.005 (2)0.007 (1)0.019 (2)
O9a0.047 (3)0.042 (2)0.047 (2)0.012 (2)0.004 (2)0.001 (2)
O6b0.021 (1)0.046 (1)0.030 (1)0.006 (1)0.002 (1)0.016 (1)
Cl4b0.0215 (3)0.0366 (10)0.027 (4)0.0057 (5)0.0018 (3)0.0128 (5)
O7b0.063 (3)0.078 (3)0.057 (3)0.035 (3)0.012 (2)0.015 (2)
O8b0.034 (2)0.108 (5)0.108 (5)0.018 (3)0.006 (3)0.091 (4)
O9b0.044 (3)0.059 (3)0.026 (2)0.024 (2)0.017 (2)0.003 (2)
O100.039 (1)0.036 (1)0.031 (1)0.000 (1)0.005 (1)0.006 (1)
Geometric parameters (Å, º) top
Fe1—Fe23.623 (1)Cl3—O41.430 (2)
Fe1—Cl12.324 (1)Cl3—O51.432 (2)
Fe1—O11.814 (1)Cl4a—O6a1.439 (1)
Fe1—N12.161 (2)Cl4a—O7a1.439
Fe1—N22.219 (2)Cl4a—O8a1.439
Fe1—N32.296 (2)Cl4a—O9a1.439
Fe1—N42.156 (2)Cl4b—O6b1.439
Fe2—Cl22.334 (1)Cl4b—O7b1.439
Fe2—O11.811 (1)Cl4b—O8b1.439
Fe2—N52.169 (2)Cl4b—O9b1.439
Fe2—N62.227 (2)C1—H10.950
Fe2—N72.284 (2)C2—H20.950
Fe2—N82.164 (2)C3—H30.950
N1—C11.351 (2)C4—H40.950
N1—C51.350 (2)C6—H6a0.950
N2—C61.477 (3)C6—H6b0.950
N2—C71.477 (2)C7—H7a0.950
N2—C81.493 (2)C7—H7b0.950
N3—C91.488 (2)C7—H7c0.950
N3—C101.480 (2)C8—H8a0.950
N3—C111.475 (3)C8—H8b0.950
N4—C121.346 (2)C9—H9a0.950
N4—C161.349 (3)C9—H9b0.950
N5—C171.345 (2)C10—H10a0.950
N5—C211.351 (2)C10—H10b0.950
N6—C221.477 (2)C10—H10c0.950
N6—C231.479 (2)C11—H11a0.950
N6—C241.493 (2)C11—H11b0.950
N7—C271.479 (2)C13—H130.950
N7—C251.490 (2)C14—H140.950
N7—C261.485 (2)C15—H150.950
N8—C281.350 (2)C16—H160.950
N8—C321.349 (2)C17—H170.950
C1—C21.380 (3)C18—H180.950
C2—C31.378 (4)C19—H190.950
C3—C41.379 (3)C20—H200.950
C4—C51.391 (3)C22—H22a0.950
C5—C61.495 (3)C22—H22b0.950
C8—C91.507 (3)C23—H23a0.950
C11—C121.505 (3)C23—H23b0.950
C12—C131.385 (3)C23—H23c0.950
C13—C141.382 (3)C24—H24a0.950
C14—C151.384 (3)C24—H24b0.950
C15—C161.383 (3)C25—H25a0.950
C17—C181.378 (3)C25—H25b0.950
C18—C191.386 (3)C26—H26a0.950
C19—C201.379 (3)C26—H26b0.950
C20—C211.391 (3)C26—H26c0.950
C21—C221.504 (3)C27—H27a0.950
C24—C251.510 (3)C27—H27b0.950
C27—C281.502 (3)C29—H290.950
C28—C291.387 (3)C30—H300.950
C29—C301.381 (3)C31—H310.950
C30—C311.388 (3)C32—H320.950
C31—C321.382 (3)O10—HO10a0.909
Cl3—O21.438 (2)O10—HO10b0.914
Cl3—O31.433 (2)
O1—Fe1—N196.59 (6)O6a—Cl4a—O7a109.47
O1—Fe1—N292.93 (6)O6a—Cl4a—O8a109.47
O1—Fe1—N3166.23 (6)O6a—Cl4a—O9a109.47
O1—Fe1—N496.91 (6)O7a—Cl4a—O8a109.47
O1—Fe1—Cl1102.00 (4)O7a—Cl4a—O9a109.47
N1—Fe1—N275.42 (6)O8a—Cl4a—O9a109.47
N1—Fe1—N391.48 (6)O6b—Cl4b—O7b109.47
N1—Fe1—N4164.24 (6)O6b—Cl4b—O8b109.47
N1—Fe1—Cl193.19 (5)O6b—Cl4b—O9b109.47
N2—Fe1—N378.29 (6)O7b—Cl4b—O8b109.47
N2—Fe1—N495.80 (6)O7b—Cl4b—O9b109.47
N2—Fe1—Cl1162.25 (4)O8b—Cl4b—O9b109.47
N3—Fe1—N473.75 (6)N1—C1—H1119.0
N3—Fe1—Cl188.62 (4)C2—C1—H1119.0
N4—Fe1—Cl191.92 (5)C3—C2—H2120.4
O1—Fe2—N597.62 (6)C1—C2—H2120.4
O1—Fe2—N693.51 (6)C2—C3—H3120.3
O1—Fe2—N7165.92 (6)C4—C3—H3120.3
O1—Fe2—N895.58 (6)C3—C4—H4120.5
O1—Fe2—Cl2101.56 (4)C5—C4—H4120.5
N5—Fe2—N674.92 (6)H6a—C6—H6b109.5
N5—Fe2—N791.71 (6)N2—C6—H6a109.1
N5—Fe2—N8164.83 (6)C5—C6—H6a109.1
N5—Fe2—Cl292.15 (5)N2—C6—H6b109.1
N6—Fe2—N778.71 (6)C5—C6—H6b109.1
N6—Fe2—N896.87 (6)H7a—C7—H7b109.6
N6—Fe2—Cl2161.39 (4)H7a—C7—H7c109.6
N7—Fe2—N873.99 (6)N2—C7—H7a109.0
N7—Fe2—Cl288.54 (4)H7b—C7—H7c109.5
N8—Fe2—Cl292.50 (5)N2—C7—H7b109.6
Fe1—O1—Fe2176.43 (8)N2—C7—H7c109.6
Fe1—N1—C1126.0 (1)H8a—C8—H8b109.5
Fe1—N1—C5114.6 (1)N2—C8—H8a109.4
Fe1—N2—C6105.6 (1)C9—C8—H8a109.4
Fe1—N2—C7111.6 (1)N2—C8—H8b109.4
Fe1—N2—C8110.3 (1)C9—C8—H8b109.4
Fe1—N3—C9106.9 (1)H9a—C9—H9b109.5
Fe1—N3—C10115.8 (1)N3—C9—H9a109.4
Fe1—N3—C11106.3 (1)C8—C9—H9a109.4
Fe1—N4—C12117.4 (1)N3—C9—H9b109.4
Fe1—N4—C16123.2 (1)C8—C9—H9b109.4
Fe2—N5—C17125.4 (1)H10a—C10—H10b109.5
Fe2—N5—C21115.0 (1)H10a—C10—H10c109.5
Fe2—N6—C22106.3 (1)N3—C10—H10a109.5
Fe2—N6—C23111.6 (1)H10b—C10—H10c109.5
Fe2—N6—C24109.4 (1)N3—C10—H10b109.5
Fe2—N7—C25107.0 (1)N3—C10—H10c109.5
Fe2—N7—C26115.9 (1)H11a—C11—H11b109.5
Fe2—N7—C27106.5 (1)N3—C11—H11a109.3
Fe2—N8—C28116.9 (1)C12—C11—H11a109.3
Fe2—N8—C32123.9 (1)N3—C11—H11b109.3
C1—N1—C5118.7 (2)C12—C11—H11b109.3
C6—N2—C7109.0 (2)C14—C13—H13120.2
C6—N2—C8109.5 (1)C12—C13—H13120.2
C7—N2—C8110.7 (1)C13—C14—H14120.5
C9—N3—C11108.9 (2)C15—C14—H14120.5
C10—N3—C11109.2 (2)C16—C15—H15120.5
C9—N3—C10109.5 (1)C14—C15—H15120.5
C12—N4—C16119.1 (2)N4—C16—H16119.0
C17—N5—C21118.6 (2)C15—C16—H16119.0
C22—N6—C23108.7 (2)N5—C17—H17118.8
C22—N6—C24109.8 (1)C18—C17—H17118.8
C23—N6—C24110.9 (1)C17—C18—H18120.6
C26—N7—C27108.3 (2)C19—C18—H18120.6
C25—N7—C27109.2 (1)C20—C19—H19120.3
C25—N7—C26109.7 (1)C18—C19—H19120.3
C28—N8—C32118.6 (2)C19—C20—H20120.5
N1—C1—C2122.0 (2)C21—C20—H20120.5
C1—C2—C3119.1 (2)H22a—C22—H22b109.5
C2—C3—C4119.5 (2)N6—C22—H22a109.2
C3—C4—C5119.0 (2)C21—C22—H22a109.2
N1—C5—C4121.6 (2)N6—C22—H22b109.2
N1—C5—C6116.0 (2)C21—C22—H22b109.2
C4—C5—C6122.3 (2)H23a—C23—H23b109.7
N2—C6—C5111.0 (2)H23a—C23—H23c109.7
N2—C8—C9109.9 (2)N6—C23—H23a108.7
N3—C9—C8109.9 (2)H23b—C23—H23c109.5
N3—C11—C12110.3 (2)N6—C23—H23b109.7
N4—C12—C13121.4 (2)N6—C23—H23c109.7
N4—C12—C11116.0 (2)H24a—C24—H24b109.5
C11—C12—C13122.6 (2)N6—C24—H24a109.3
C12—C13—C14119.6 (2)C25—C24—H24a109.3
C13—C14—C15118.9 (2)N6—C24—H24b109.3
C14—C15—C16119.0 (2)C25—C24—H24b109.3
N4—C16—C15122.0 (2)H25a—C25—H25b109.5
N5—C17—C18122.5 (2)N7—C25—H25a109.5
C17—C18—C19118.8 (2)C24—C25—H25a109.5
C18—C19—C20119.4 (2)N7—C25—H25b109.5
C19—C20—C21119.0 (2)C24—C25—H25b109.5
N5—C21—C20121.7 (2)H26a—C26—H26b109.4
N5—C21—C22115.9 (2)H26a—C26—H26c109.4
C20—C21—C22122.3 (2)N7—C26—H26a109.7
N6—C22—C21110.7 (2)H26b—C26—H26c109.5
N6—C24—C25110.3 (2)N7—C26—H26b109.4
N7—C25—C24109.5 (2)N7—C26—H26c109.4
N7—C27—C28110.8 (2)H27a—C27—H27b109.5
N8—C28—C29121.8 (2)N7—C27—H27a109.1
N8—C28—C27116.0 (2)C28—C27—H27a109.1
C27—C28—C29122.2 (2)N7—C27—H27b109.1
C28—C29—C30119.2 (2)C28—C27—H27b109.1
C29—C30—C31119.4 (2)C30—C29—H29120.4
C30—C31—C32118.6 (2)C28—C29—H29120.4
N8—C32—C31122.4 (2)C29—C30—H30120.3
O2—Cl3—O3109.0 (1)C31—C30—H30120.3
O2—Cl3—O4109.3 (1)C32—C31—H31120.7
O2—Cl3—O5109.4 (1)C30—C31—H31120.7
O3—Cl3—O4110.0 (1)N8—C32—H32118.8
O3—Cl3—O5108.6 (1)C31—C32—H32118.8
O4—Cl3—O5110.5 (1)HO10a—O10—HO10b101.0
Cl1—Fe1—Fe2—Cl2128.21 (2)

Experimental details

Crystal data
Chemical formula[Fe2Cl2O(C16H22N4)2](ClO4)2·0.751H2O
Mr951.83
Crystal system, space groupMonoclinic, P21/c
Temperature (K)120
a, b, c (Å)13.632 (3), 17.956 (4), 16.489 (3)
β (°) 94.938 (4)
V3)4021 (1)
Z4
Radiation typeMo Kα
µ (mm1)1.05
Crystal size (mm)0.50 × 0.13 × 0.12
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Absorption correctionIntegration
(XPREP; Siemens, 1995)
Tmin, Tmax0.647, 0.899
No. of measured, independent and
observed [I > 3σ(I)] reflections
45381, 12123, 8461
Rint0.042
(sin θ/λ)max1)0.714
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.034, 0.88
No. of reflections8461
No. of parameters521
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.72 (8), 0.51 (8)

Computer programs: SMART (Siemens, 1995), SAINT (Siemens, 1995), SAINT, SIR97 (Altomare et al., 1997) and KRYSTAL (Hazell, 1995), modified ORFLS (Busing et al., 1962) and KRYSTAL, ORTEPIII (Burnett & Johnson, 1996) and KRYSTAL, KRYSTAL.

Selected geometric parameters (Å, º) top
Fe1—Fe23.623 (1)Fe2—Cl22.334 (1)
Fe1—Cl12.324 (1)Fe2—O11.811 (1)
Fe1—O11.814 (1)Fe2—N52.169 (2)
Fe1—N12.161 (2)Fe2—N62.227 (2)
Fe1—N22.219 (2)Fe2—N72.284 (2)
Fe1—N32.296 (2)Fe2—N82.164 (2)
Fe1—N42.156 (2)
O1—Fe1—N196.59 (6)O1—Fe2—N693.51 (6)
O1—Fe1—N292.93 (6)O1—Fe2—N7165.92 (6)
O1—Fe1—N3166.23 (6)O1—Fe2—N895.58 (6)
O1—Fe1—N496.91 (6)O1—Fe2—Cl2101.56 (4)
O1—Fe1—Cl1102.00 (4)N5—Fe2—N674.92 (6)
N1—Fe1—N275.42 (6)N5—Fe2—N791.71 (6)
N1—Fe1—N391.48 (6)N5—Fe2—N8164.83 (6)
N1—Fe1—N4164.24 (6)N5—Fe2—Cl292.15 (5)
N1—Fe1—Cl193.19 (5)N6—Fe2—N778.71 (6)
N2—Fe1—N378.29 (6)N6—Fe2—N896.87 (6)
N2—Fe1—N495.80 (6)N6—Fe2—Cl2161.39 (4)
N2—Fe1—Cl1162.25 (4)N7—Fe2—N873.99 (6)
N3—Fe1—N473.75 (6)N7—Fe2—Cl288.54 (4)
N3—Fe1—Cl188.62 (4)N8—Fe2—Cl292.50 (5)
N4—Fe1—Cl191.92 (5)Fe1—O1—Fe2176.43 (8)
O1—Fe2—N597.62 (6)
 

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