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Acta Crystallogr Sect E Struct Rep Online. 2008 November 1; 64(Pt 11): i76.
Published online 2008 October 18. doi:  10.1107/S1600536808032881
PMCID: PMC2959719

Hexaamminecobalt(III) hexa­cyanido­manganate(III)

Abstract

The asymmetric unit of the title compound, [Co(NH3)6][Mn(CN)6], contains one Co and one Mn atom, both lying on threefold inversion axes, and one NH3 and one CN group. The octa­hedral environments around CoII and MnII are generated by symmetry and show very slight deviations from ideal geometry. A three-dimensional network is created by N—H(...)N hydrogen bonds.

Related literature

For related structures, see: Buschmann et al. (1999 [triangle]). For the construction of clusters and networks with adjustable magnetic properties, see: Przychodzen et al. (2006 [triangle]); Withers et al. (2005 [triangle]).

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Object name is e-64-00i76-scheme1.jpg

Experimental

Crystal data

  • [Co(NH3)6][Mn(CN)6]
  • M r = 372.19
  • Trigonal, An external file that holds a picture, illustration, etc.
Object name is e-64-00i76-efi1.jpg
  • a = 10.963 (5) Å
  • c = 10.779 (5) Å
  • V = 1121.9 (9) Å3
  • Z = 3
  • Mo Kα radiation
  • μ = 1.96 mm−1
  • T = 100 (2) K
  • 0.35 × 0.26 × 0.25 mm

Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2004 [triangle]) T min = 0.546, T max = 0.614
  • 3602 measured reflections
  • 628 independent reflections
  • 497 reflections with I > 2σ(I)
  • R int = 0.038

Refinement

  • R[F 2 > 2σ(F 2)] = 0.025
  • wR(F 2) = 0.071
  • S = 0.93
  • 628 reflections
  • 32 parameters
  • H-atom parameters constrained
  • Δρmax = 0.29 e Å−3
  • Δρmin = −0.43 e Å−3

Data collection: APEX2 (Bruker, 2005 [triangle]); cell refinement: SAINT-Plus (Bruker, 2004 [triangle]); data reduction: SAINT-Plus and XPREP (Bruker, 2004 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 [triangle]); software used to prepare material for publication: SHELXL97 and WinGX (Farrugia, 1999 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808032881/pk2122sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808032881/pk2122Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The University of the Free State is gratefully acknowledged for financial support. Dr A. J. Muller and Mr Leo Kirsten are acknowledged for help with the data collection.

supplementary crystallographic information

Comment

Our interest is in the use of cyanometalates as molecular building blocks for potentially constructing clusters and networks with adjustable magnetic properties [Przychodzen et al., (2006), Withers et al., (2005)].

The title compound crystallizes in the trigonal R-3 space group with Z = 3. The main part of the asymmetric unit contains one Co and one Mn atom, both lying on threefold rotational axes.

The octahedral environments around CoII and MnII are generated by symmetry and shows very slight deviation from ideal geometry as illustrated by the C—Mn—C angles of 180.00 (7), 89.80 (7) and 90.20 (7) and N—Co—N angles of 180.00 (7), 89.47 (6) and 90.53 (6) ° respectively.

A three dimensional network is created by hydrogen bonds of the type N—H—N.

Experimental

Equimolar amounts of K3[Mn(CN)6] and [Co(NH3)6]Cl3 were dissolved in water, added together and allowed to stand. Orange crystals separated out after a few days.

Figures

Fig. 1.
An ellipsoid plot of the title compound (50% probability displacement ellipsoids).

Crystal data

[Co(NH3)6][Mn(CN)6]Dx = 1.653 Mg m3
Mr = 372.19Mo Kα radiation, λ = 0.71069 Å
Trigonal, R3Cell parameters from 1532 reflections
Hall symbol: -R 3θ = 2.9–28.3°
a = 10.963 (5) ŵ = 1.96 mm1
c = 10.779 (5) ÅT = 100 K
V = 1121.9 (9) Å3Cuboid, orange
Z = 30.35 × 0.26 × 0.25 mm
F(000) = 570

Data collection

Bruker SMART APEXII CCD area-detector diffractometer497 reflections with I > 2σ(I)
[var phi] and ω scansRint = 0.038
Absorption correction: multi-scan (SADABS; Bruker, 2004)θmax = 28.3°, θmin = 2.9°
Tmin = 0.546, Tmax = 0.614h = −12→14
3602 measured reflectionsk = −14→9
628 independent reflectionsl = −10→14

Refinement

Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.025w = 1/[σ2(Fo2) + (0.0379P)2 + 3.8029P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.071(Δ/σ)max < 0.001
S = 0.93Δρmax = 0.29 e Å3
628 reflectionsΔρmin = −0.42 e Å3
32 parameters

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Co10000.00732 (17)
Mn10.33330.66670.16670.00607 (17)
N1−0.02748 (15)0.13048 (15)−0.10659 (13)0.0107 (3)
H1A0.02380.2179−0.07770.016*
H1B−0.11810.1061−0.10650.016*
H1C−0.00060.1264−0.18370.016*
C20.31385 (18)0.80238 (18)0.06080 (16)0.0119 (3)
N20.30018 (17)0.87891 (17)−0.00283 (15)0.0184 (4)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.0076 (2)0.0076 (2)0.0067 (3)0.00381 (10)00
Mn10.0064 (2)0.0064 (2)0.0055 (3)0.00318 (10)00
N10.0117 (7)0.0099 (7)0.0111 (7)0.0058 (6)0.0007 (5)0.0010 (5)
C20.0108 (8)0.0144 (8)0.0115 (8)0.0070 (7)0.0001 (6)−0.0026 (6)
N20.0200 (8)0.0248 (9)0.0159 (7)0.0152 (7)0.0014 (6)0.0013 (6)

Geometric parameters (Å, °)

Co1—N1i1.9718 (16)Mn1—C2vii1.9696 (19)
Co1—N1ii1.9718 (16)Mn1—C2viii1.9696 (19)
Co1—N1iii1.9718 (15)Mn1—C2ix1.9696 (19)
Co1—N1iv1.9718 (15)Mn1—C2x1.9696 (19)
Co1—N11.9718 (15)N1—H1A0.89
Co1—N1v1.9718 (15)N1—H1B0.89
Mn1—C2vi1.9696 (19)N1—H1C0.89
Mn1—C21.9696 (19)C2—N21.150 (2)
N1i—Co1—N1ii180.00 (7)C2—Mn1—C2viii89.80 (7)
N1i—Co1—N1iii89.47 (6)C2vii—Mn1—C2viii89.80 (7)
N1ii—Co1—N1iii90.53 (6)C2vi—Mn1—C2ix89.80 (7)
N1i—Co1—N1iv89.47 (6)C2—Mn1—C2ix90.20 (7)
N1ii—Co1—N1iv90.53 (6)C2vii—Mn1—C2ix180
N1iii—Co1—N1iv89.47 (6)C2viii—Mn1—C2ix90.20 (7)
N1i—Co1—N190.53 (6)C2vi—Mn1—C2x89.80 (7)
N1ii—Co1—N189.47 (6)C2—Mn1—C2x90.20 (7)
N1iii—Co1—N1180.00 (10)C2vii—Mn1—C2x90.20 (7)
N1iv—Co1—N190.53 (6)C2viii—Mn1—C2x180.00 (7)
N1i—Co1—N1v90.53 (6)C2ix—Mn1—C2x89.80 (7)
N1ii—Co1—N1v89.47 (6)Co1—N1—H1A109.5
N1iii—Co1—N1v90.53 (6)Co1—N1—H1B109.5
N1iv—Co1—N1v180.00 (10)H1A—N1—H1B109.5
N1—Co1—N1v89.47 (6)Co1—N1—H1C109.5
C2vi—Mn1—C2180H1A—N1—H1C109.5
C2vi—Mn1—C2vii90.20 (7)H1B—N1—H1C109.5
C2—Mn1—C2vii89.80 (7)N2—C2—Mn1178.31 (17)
C2vi—Mn1—C2viii90.20 (7)

Symmetry codes: (i) y, −x+y, −z; (ii) −y, xy, z; (iii) −x, −y, −z; (iv) xy, x, −z; (v) −x+y, −x, z; (vi) −x+2/3, −y+4/3, −z+1/3; (vii) −y+1, xy+1, z; (viii) −x+y, −x+1, z; (ix) y−1/3, −x+y+1/3, −z+1/3; (x) xy+2/3, x+1/3, −z+1/3.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N1—H1A···N2vii0.892.092.979 (2)173

Symmetry codes: (vii) −y+1, xy+1, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PK2122).

References

  • Brandenburg, K. & Putz, H. (2005). DIAMOND Crystal Impact GbR, Bonn, Germany.
  • Bruker (2004). SAINT-Plus, XPREP and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Bruker (2005). APEX2 Bruker AXS Inc., Madison, Wisconsin, USA.
  • Buschmann, W. E., Liable-Sands, L., Rheingold, A. L. & Miller, J. S. (1999). Inorg. Chim. Acta, 284, 175–179.
  • Farrugia, L. J. (1999). J. Appl. Cryst.32, 837–838.
  • Przychodzen, P., Korzeniak, T., Podgajny, R. & Sieklucka, B. (2006). Coord. Chem. Rev.250, 2234–2260.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Withers, J. R., Ruschmann, C., Bojang, P., Parkin, S. & Holmes, S. M. (2005). Inorg. Chem.44, 352–358. [PubMed]

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography