inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

Hexa­aqua­iron(II) bis­­[fac-tri­bromido­tri­carbonyl­ferrate(II)]

aInstitute of Applied Synthetic Chemistry, Vienna University of Technology, Getreidemarkt 9/163, A-1060 Vienna, Austria, and bInstitute of Chemical Technologies and Analytics, Vienna University of Technology, Getreidemarkt 9/164SC, A-1060 Vienna, Austria
*Correspondence e-mail: kurt.mereiter@tuwien.ac.at

(Received 3 September 2009; accepted 7 September 2009; online 12 September 2009)

In the title compound, [Fe(H2O)6][FeBr3(CO)3]2, both Fe atoms have an octa­hedral coordination and the bromide carbonyl complex has a fac-stereochemistry. The [Fe(H2O)6]2+ octa­hedron has point symmetry [\overline{1}] and is slightly compressed along one O—Fe—O axis. The [FeBr3(CO)3] anion has point symmetry 1 and mean bond lengths of Fe—Br = 2.455 (5) Å and Fe—C = 1.809 (2) Å. The cation and anion complexes are mutually linked via O—H⋯Br hydrogen bonds with O⋯Br distances of 3.340 (3) to 3.388 (3) Å.

Related literature

For the chemistry of FeBr2(CO)4, see: Hieber & Bader (1928[Hieber, W. & Bader, G. (1928). Chem. Ber. 61, 1717-1722.]); Robertson et al. (2000[Robertson, E. W., Wilkin, O. M. & Young, N. A. (2000). Polyhedron, 19, 1493-1502.]). For the syntheses and crystal structures of anologous compounds with [(Fe/Co/Ru)(H2O)6]2+ cations and [(Ru/Os)(Cl/I)3(CO)3] complexes, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]); Taimisto et al. (2003[Taimisto, M., Oilunkaniemi, R., Laitinen, R. S. & Ahlgren, M. (2003). Z. Naturforsch. Teil B, 58, 959-964.]); Haukka et al. (2006[Haukka, M., Jakonen, M., Nivajarvi, T. & Kallinen, M. (2006). Dalton Trans., pp. 3212-3220.]); Jakonen et al. (2007[Jakonen, M., Hirva, P., Nivajarvi, T., Kallinen, M. & Haukka, M. (2007). Eur. J. Inorg. Chem. 2007, 3497-3508.]).

[Scheme 1]

Experimental

Crystal data
  • [Fe(H2O)6][FeBr3(CO)3]2

  • Mr = 923.17

  • Orthorhombic, P b c a

  • a = 11.9334 (8) Å

  • b = 9.3394 (6) Å

  • c = 20.5775 (14) Å

  • V = 2293.4 (3) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 12.37 mm−1

  • T = 100 K

  • 0.26 × 0.10 × 0.08 mm

Data collection
  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2003[Bruker (2003). SMART, SAINT, SADABS and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.15, Tmax = 0.37

  • 24075 measured reflections

  • 3316 independent reflections

  • 2674 reflections with I > 2σ(I)

  • Rint = 0.061

Refinement
  • R[F2 > 2σ(F2)] = 0.034

  • wR(F2) = 0.070

  • S = 1.04

  • 3316 reflections

  • 145 parameters

  • 18 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.98 e Å−3

  • Δρmin = −0.68 e Å−3

Table 1
Selected bond lengths (Å)

Fe1—O1W 2.137 (3)
Fe1—O2W 2.128 (3)
Fe1—O3W 2.098 (3)
Fe2—C1 1.812 (4)
Fe2—C2 1.807 (4)
Fe2—C3 1.808 (4)
Fe2—Br1 2.4479 (6)
Fe2—Br2 2.4605 (6)
Fe2—Br3 2.4558 (6)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O1W—H1A⋯Br1 0.821 (19) 2.52 (2) 3.340 (3) 174 (4)
O1W—H1B⋯Br2i 0.821 (19) 2.69 (2) 3.475 (3) 162 (5)
O2W—H2A⋯Br2ii 0.821 (19) 2.55 (2) 3.373 (3) 177 (5)
O2W—H2B⋯Br2i 0.821 (19) 2.56 (2) 3.341 (3) 160 (5)
O3W—H3A⋯Br3 0.821 (19) 2.58 (2) 3.388 (3) 169 (5)
O3W—H3B⋯Br3iii 0.821 (19) 2.53 (2) 3.346 (3) 177 (4)
Symmetry codes: (i) -x, -y+1, -z; (ii) [x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]; (iii) [-x+{\script{1\over 2}}, y-{\script{1\over 2}}, z].

Data collection: SMART (Bruker, 2003[Bruker (2003). SMART, SAINT, SADABS and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2003[Bruker (2003). SMART, SAINT, SADABS and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT and XPREP (Bruker, 2003[Bruker (2003). SMART, SAINT, SADABS and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

FeBr2(CO)4, easily accessible by reaction of Fe(CO)5 with bromine (Hieber & Bader, 1928; Robertson et al., 2000), is stable under dry conditions but reacts readily with various protic or coordinating solvents and thus turned out to be an interesting precursor for iron complexes which are otherwise difficult to obtain. By treatment of FeBr2(CO)4 with wet benzene the title compound was obtained according to the equation: 3 FeBr2(CO)4 + 6H2O Fe(H2O)6 + 2 FeBr3(CO)3 + 6 CO. The structure (Fig. 1) contains a [Fe(H2O)6]2+ octahedron with point symmetry 1 and a [FeBr3(CO)3]- octahedron with iron with point symmetry 1 (Fig. 1). The Fe—O bond lengths in [Fe(H2O)6]2+ (Table 1) correspond well with high-spin iron(II) in an axially weakly compressed octahedron. The [FeBr3(CO)3]- anion has a facial disposition of the bromide and carbonyl ligands and shows each three very uniform Fe—Br and Fe—C bond distances with mean values of Fe—Br = 2.455 (5) Å and Fe—C = 1.809 (2) Å (Table 1) consistent with a low-spin state. The bond angles about this iron deviate up to 5.6° from 90 and 180°. C—O bond lengths average to 1.128 (1) Å, and Fe—C—O angles 177.9 (10)°. Each of the three independent water molecules is coordinated by Fe1 and by pair of bromine atoms as hydrogen bond acceptors. Their coordination environments are pyramidal to flat pyramidal (O2w). The six independent O—H···Br bonds (Table 2) are quite uniform in distances and angles, all being essentially linear. The structure has various architectural aspects, but is best regarded as consisting of double layers of [FeBr3(CO)3] octahedra held together by interactions between the mainly inward-oriented CO groups whereas the bromine atoms define their outer surfaces (Fig. 2). These double layers are oriented parallel to (100) and centered at y = 1/4 and 3/4. Intercalated between these double layers are single layers of [Fe(H2O)6]2+ octahedra at z = 0, 1/2 and 1, which bridge the double layers via the O—H···Br hydrogen bonds. The title compound has no precedents in iron structural chemistry, but a few analogous [MX3(CO)3]- complexes are known for M = Ru, Os, Re, and X = Cl, Br, I (Cambridge Structural Database - CSD; Version 5.30 of November 2008; Allen, 2002). Most related to the title compound is [Ru(H2O)6]2+[RuCl3(CO)3]-2.2H2O (Taimisto et al., 2003), obtained from [RuCl2(CO)3]2 in wet CH2Cl2. It has, despite being triclinic (title compound is orthorhombic), an additional uncoordinated H2O, a structural architecture analogous to the title compound. More recently, this formerly unique compound was expanded into three isomorphous series of type 1, [(Fe/Co)(H2O)6]2+[(Ru/Os)Cl3(CO)3]-2, triclinic, space group P1, of type 2, [(Ru/Fe/Co)(H2O)6]2+[(Ru/Os)Cl3(CO)3]-2.2H2O, triclinic, space group P1, and of type 3, [(Fe/Co)(H2O)6]2+[RuI3(CO)3]-2.2H2O, monoclinic, space group P21/c (Haukka et al., 2006; Jakonen et al., 2007). All these compounds share the [MX3(CO)3]- (X = Cl, Br, I) double layer plus [M(H2O)6]2+ single layer architecture of the title compound with additional non-coordinated water molecules (structure types 2 and 3) being involved in the [M(H2O)6]2+ layers.

Related literature top

For the chemistry of FeBr2(CO)4, see: Hieber & Bader (1928); Robertson et al. (2000). For the syntheses and crystal structures of anologous compounds with [(Fe/Co/Ru)(H2O)6]2+ cations and [(Ru/Os)(Cl/I)3(CO)3]- complexes, see: Allen (2002); Taimisto et al. (2003); Haukka et al. (2006); Jakonen et al. (2007).

Experimental top

The title compound was synthesized as follows: FeBr2(CO)4 (200 mg, 0.610 mmol; Hieber & Bader, 1928) was dissolved in wet benzene (20 ml, containing 1.67 mmol water) resulting in significant CO gas evolution. The solution was allowed to stand for 15 minutes until no further gas evolution was observed. The solution was set aside for about 1 h to give orange crystals of the title copound. Yield: 75 mg (40%).

Refinement top

All H atoms belong to H2O molecules. They were refined in x,y,z using hard SADI restraints of program SHELXL97 (Sheldrick, 2008) to make all O—H bond lengths and all intramolecular H—H distances equal. Moreover, pairs of identical Uiso(H) values were refined for each water molecule.

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003) and XPREP (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL ((Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Perspective view of the title compound with the atom numbering scheme. Atoms with primed labels are generated by inversion (-x,-y,-z). Displacement ellipsoids are at the 50% probability level.
[Figure 2] Fig. 2. Packing diagram of the title compound viewed down the a axis. [Fe(H2O)6] octahedra in green and stick bond representation, [FeBr3(CO)3] in ball-and-stick representation, hydrogen bonds shown as red broken lines.
Hexaaquairon(II) bis[fac-tribromidotricarbonylferrate(II)] top
Crystal data top
[Fe(H2O)6][FeBr3(CO)3]2F(000) = 1728
Mr = 923.17Dx = 2.674 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 4102 reflections
a = 11.9334 (8) Åθ = 2.6–29.5°
b = 9.3394 (6) ŵ = 12.37 mm1
c = 20.5775 (14) ÅT = 100 K
V = 2293.4 (3) Å3Prism, brown
Z = 40.26 × 0.10 × 0.08 mm
Data collection top
Bruker SMART APEX CCD
diffractometer
3316 independent reflections
Radiation source: fine-focus sealed tube2674 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
ω and ϕ scansθmax = 30.0°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2003)
h = 1616
Tmin = 0.15, Tmax = 0.37k = 1212
24075 measured reflectionsl = 2828
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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.070H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0343P)2]
where P = (Fo2 + 2Fc2)/3
3316 reflections(Δ/σ)max = 0.001
145 parametersΔρmax = 0.98 e Å3
18 restraintsΔρmin = 0.68 e Å3
Crystal data top
[Fe(H2O)6][FeBr3(CO)3]2V = 2293.4 (3) Å3
Mr = 923.17Z = 4
Orthorhombic, PbcaMo Kα radiation
a = 11.9334 (8) ŵ = 12.37 mm1
b = 9.3394 (6) ÅT = 100 K
c = 20.5775 (14) Å0.26 × 0.10 × 0.08 mm
Data collection top
Bruker SMART APEX CCD
diffractometer
3316 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2003)
2674 reflections with I > 2σ(I)
Tmin = 0.15, Tmax = 0.37Rint = 0.061
24075 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03418 restraints
wR(F2) = 0.070H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.98 e Å3
3316 reflectionsΔρmin = 0.68 e Å3
145 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
Fe10.00000.00000.00000.01291 (15)
O1W0.0694 (2)0.2102 (3)0.00795 (12)0.0182 (5)
O2W0.1316 (2)0.0750 (3)0.06090 (15)0.0232 (6)
O3W0.0994 (2)0.0389 (3)0.08220 (14)0.0215 (6)
H1A0.077 (4)0.227 (5)0.0468 (10)0.054 (12)*
H1B0.037 (4)0.277 (4)0.010 (2)0.054 (12)*
H2A0.194 (2)0.039 (4)0.067 (2)0.052 (12)*
H2B0.132 (4)0.157 (3)0.075 (2)0.052 (12)*
H3A0.104 (4)0.124 (2)0.091 (2)0.043 (11)*
H3B0.161 (2)0.001 (4)0.086 (2)0.043 (11)*
Fe20.00342 (4)0.48304 (5)0.17284 (2)0.01109 (11)
Br10.09906 (3)0.25138 (4)0.168259 (17)0.01518 (9)
Br20.11162 (3)0.57039 (4)0.079096 (17)0.01582 (9)
Br30.14630 (3)0.39406 (4)0.101623 (18)0.01610 (9)
C10.0671 (3)0.6547 (4)0.17014 (16)0.0147 (7)
O10.1100 (2)0.7616 (3)0.16509 (13)0.0217 (6)
C20.0777 (3)0.4172 (4)0.24072 (18)0.0146 (7)
O20.1272 (2)0.3740 (3)0.28314 (13)0.0205 (6)
C30.1149 (3)0.5406 (3)0.22633 (18)0.0147 (7)
O30.1840 (2)0.5739 (3)0.26062 (13)0.0194 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0130 (4)0.0108 (3)0.0149 (3)0.0008 (3)0.0008 (3)0.0007 (3)
O1W0.0231 (15)0.0132 (12)0.0182 (14)0.0015 (11)0.0009 (11)0.0008 (10)
O2W0.0206 (15)0.0173 (13)0.0317 (16)0.0026 (12)0.0083 (13)0.0042 (12)
O3W0.0220 (15)0.0165 (13)0.0260 (15)0.0059 (11)0.0072 (12)0.0062 (11)
Fe20.0113 (2)0.0102 (2)0.0117 (2)0.00088 (19)0.00038 (19)0.00026 (17)
Br10.01807 (18)0.01203 (17)0.01544 (17)0.00387 (13)0.00183 (14)0.00048 (12)
Br20.01585 (18)0.01523 (17)0.01639 (17)0.00118 (13)0.00296 (14)0.00300 (13)
Br30.01316 (18)0.01727 (17)0.01787 (18)0.00097 (14)0.00263 (14)0.00377 (13)
C10.0114 (17)0.0197 (18)0.0131 (17)0.0020 (14)0.0001 (13)0.0008 (13)
O10.0247 (15)0.0175 (14)0.0229 (14)0.0057 (11)0.0047 (11)0.0014 (10)
C20.0141 (18)0.0108 (15)0.0188 (18)0.0040 (13)0.0031 (14)0.0023 (13)
O20.0209 (14)0.0191 (13)0.0216 (14)0.0000 (11)0.0051 (12)0.0006 (10)
C30.0187 (19)0.0087 (15)0.0167 (18)0.0036 (13)0.0032 (14)0.0016 (12)
O30.0188 (14)0.0184 (13)0.0209 (13)0.0018 (11)0.0031 (11)0.0011 (10)
Geometric parameters (Å, º) top
Fe1—O1W2.137 (3)O3W—H3B0.821 (19)
Fe1—O2W2.128 (3)Fe2—C11.812 (4)
Fe1—O3W2.098 (3)Fe2—C21.807 (4)
Fe1—O1Wi2.137 (3)Fe2—C31.808 (4)
Fe1—O2Wi2.128 (3)Fe2—Br12.4479 (6)
Fe1—O3Wi2.098 (3)Fe2—Br22.4605 (6)
O1W—H1A0.821 (19)Fe2—Br32.4558 (6)
O1W—H1B0.821 (19)C1—O11.126 (4)
O2W—H2A0.821 (19)C2—O21.128 (4)
O2W—H2B0.821 (19)C3—O31.129 (4)
O3W—H3A0.821 (19)
O3W—Fe1—O3Wi180.00 (18)Fe1—O3W—H3A113 (3)
O3W—Fe1—O2Wi89.97 (12)Fe1—O3W—H3B121 (3)
O3Wi—Fe1—O2Wi90.03 (12)H3A—O3W—H3B109 (3)
O3W—Fe1—O2W90.03 (12)C2—Fe2—C391.43 (16)
O3Wi—Fe1—O2W89.97 (12)C2—Fe2—C194.35 (15)
O2Wi—Fe1—O2W180.00 (16)C3—Fe2—C195.59 (15)
O3W—Fe1—O1W89.91 (10)C2—Fe2—Br188.80 (11)
O3Wi—Fe1—O1W90.09 (10)C3—Fe2—Br186.75 (11)
O2Wi—Fe1—O1W88.35 (10)C1—Fe2—Br1176.03 (11)
O2W—Fe1—O1W91.65 (10)C2—Fe2—Br387.49 (11)
O3W—Fe1—O1Wi90.09 (10)C3—Fe2—Br3177.51 (11)
O3Wi—Fe1—O1Wi89.91 (10)C1—Fe2—Br386.74 (11)
O2Wi—Fe1—O1Wi91.65 (10)Br1—Fe2—Br390.981 (19)
O2W—Fe1—O1Wi88.35 (10)C2—Fe2—Br2178.97 (12)
O1W—Fe1—O1Wi180.00 (14)C3—Fe2—Br289.57 (11)
Fe1—O1W—H1A107 (3)C1—Fe2—Br285.77 (11)
Fe1—O1W—H1B119 (4)Br1—Fe2—Br291.04 (2)
H1A—O1W—H1B109 (3)Br3—Fe2—Br291.50 (2)
Fe1—O2W—H2A128 (3)O1—C1—Fe2176.4 (3)
Fe1—O2W—H2B121 (3)O2—C2—Fe2178.8 (3)
H2A—O2W—H2B109 (3)O3—C3—Fe2178.4 (3)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1A···Br10.82 (2)2.52 (2)3.340 (3)174 (4)
O1W—H1B···Br2ii0.82 (2)2.69 (2)3.475 (3)162 (5)
O2W—H2A···Br2iii0.82 (2)2.55 (2)3.373 (3)177 (5)
O2W—H2B···Br2ii0.82 (2)2.56 (2)3.341 (3)160 (5)
O3W—H3A···Br30.82 (2)2.58 (2)3.388 (3)169 (5)
O3W—H3B···Br3iv0.82 (2)2.53 (2)3.346 (3)177 (4)
Symmetry codes: (ii) x, y+1, z; (iii) x+1/2, y+1/2, z; (iv) x+1/2, y1/2, z.

Experimental details

Crystal data
Chemical formula[Fe(H2O)6][FeBr3(CO)3]2
Mr923.17
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)100
a, b, c (Å)11.9334 (8), 9.3394 (6), 20.5775 (14)
V3)2293.4 (3)
Z4
Radiation typeMo Kα
µ (mm1)12.37
Crystal size (mm)0.26 × 0.10 × 0.08
Data collection
DiffractometerBruker SMART APEX CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2003)
Tmin, Tmax0.15, 0.37
No. of measured, independent and
observed [I > 2σ(I)] reflections
24075, 3316, 2674
Rint0.061
(sin θ/λ)max1)0.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.070, 1.04
No. of reflections3316
No. of parameters145
No. of restraints18
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.98, 0.68

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003) and XPREP (Bruker, 2003), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL ((Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Fe1—O1W2.137 (3)Fe2—C31.808 (4)
Fe1—O2W2.128 (3)Fe2—Br12.4479 (6)
Fe1—O3W2.098 (3)Fe2—Br22.4605 (6)
Fe2—C11.812 (4)Fe2—Br32.4558 (6)
Fe2—C21.807 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1A···Br10.821 (19)2.52 (2)3.340 (3)174 (4)
O1W—H1B···Br2i0.821 (19)2.69 (2)3.475 (3)162 (5)
O2W—H2A···Br2ii0.821 (19)2.55 (2)3.373 (3)177 (5)
O2W—H2B···Br2i0.821 (19)2.56 (2)3.341 (3)160 (5)
O3W—H3A···Br30.821 (19)2.58 (2)3.388 (3)169 (5)
O3W—H3B···Br3iii0.821 (19)2.53 (2)3.346 (3)177 (4)
Symmetry codes: (i) x, y+1, z; (ii) x+1/2, y+1/2, z; (iii) x+1/2, y1/2, z.
 

Acknowledgements

Financial support by the FWF Austrian Science Fund (project No. P16600-N11) is gratefully acknowledged.

References

First citationAllen, F. H. (2002). Acta Cryst. B58, 380–388.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationBruker (2003). SMART, SAINT, SADABS and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationHaukka, M., Jakonen, M., Nivajarvi, T. & Kallinen, M. (2006). Dalton Trans., pp. 3212–3220.  Google Scholar
First citationHieber, W. & Bader, G. (1928). Chem. Ber. 61, 1717–1722.  CrossRef Google Scholar
First citationJakonen, M., Hirva, P., Nivajarvi, T., Kallinen, M. & Haukka, M. (2007). Eur. J. Inorg. Chem. 2007, 3497–3508.  Web of Science CSD CrossRef Google Scholar
First citationRobertson, E. W., Wilkin, O. M. & Young, N. A. (2000). Polyhedron, 19, 1493–1502.  Web of Science CrossRef CAS Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationTaimisto, M., Oilunkaniemi, R., Laitinen, R. S. & Ahlgren, M. (2003). Z. Naturforsch. Teil B, 58, 959–964.  CAS Google Scholar

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