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Volume 67 
Part 7 
Pages m824-m825  
July 2011  

Received 19 May 2011
Accepted 25 May 2011
Online 4 June 2011

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Key indicators
Single-crystal X-ray study
T = 90 K
Mean [sigma](C-C) = 0.006 Å
Disorder in main residue
R = 0.061
wR = 0.173
Data-to-parameter ratio = 14.1
Details
Open access

Di-[mu]-oxido-bis[(1,4,8,11-tetraazacyclotetradecane-[kappa]4N,N',N'',N''')dimanganese(III,IV)] bis(tetraphenylborate) chloride acetonitrile disolvate

Marilyn M. Olmstead,a* David W. Boycea and Lauren E. Briaa

aDepartment of Chemistry, University of California, One Shields Avenue, Davis, CA 95616, USA
Correspondence e-mail: olmstead@chem.ucdavis.edu

The title compound, [Mn2O2(C10H24N4)2](C24H20B)2Cl·2CH3CN, is a mixed-valent MnIII/MnIV oxide-bridged manganese dimer with one chloride and two tetraphenylborate counter-anions. There are two non-coordinated molecules of acetonitrile in the formula unit. A center of inversion is present between the two metal atoms, and, consequently, there is no distinction between MnIII and MnIV metal centers. In the Mn2O2 core, the Mn-O distances are 1.817 (3) and 1.821 (3) Å. The cyclam ligand is in the cis configuration. The chloride counter-anion resides on a center of symmetry, whereas the tetraphenylborate counter-anion is in a general position. The cyclam ligand is hydrogen bonded to the acetonitrile as well as to the chloride anion. One of the phenyl rings of the anion and the acetonitrile solvent molecule are each disordered over two sets of sites.

Related literature

For structures of different salts containing the disordered mixed-valent {[(cyclam)MnO]2}3+ cation, see: Goodson et al. (1990[Goodson, P. A., Hodgson, D. J. & Michelsen, K. (1990). Inorg. Chim. Acta, 172, 49-57.]); Lu et al. (2001[Lu, Y.-H., Fun, H.-K., Chantrapromma, S., Razak, I. A., Shen, Z., Zuo, J.-L. & You, X.-Z. (2001). Acta Cryst. C57, 911-913.]). For structures of the non-disordered MnIII-MnIVO2 core, see: Brewer et al. (1989[Brewer, K. J., Calvin, M., Lumpkin, R. S., Otvos, J. W. & Spreer, L. O. (1989). Inorg. Chem. 28, 4446-4451.]); Levaton & Olmstead (2010[Levaton, B. B. & Olmstead, M. M. (2010). Acta Cryst. E66, m1226-m1227.]). For cyclam configurations, see: Bosnich et al. (1965[Bosnich, B., Poon, C. K. & Tobe, M. L. (1965). Inorg. Chem. 4, 1102-1108.]).

[Scheme 1]

Experimental

Crystal data

  • [Mn2O2(C10H24N4)2](C24H20B)2Cl·2C2H3N

  • Mr = 1298.52

  • Triclinic, [P \overline 1]

  • a = 11.437 (2) Å

  • b = 11.713 (2) Å

  • c = 13.967 (3) Å

  • [alpha] = 104.136 (3)°

  • [beta] = 97.697 (3)°

  • [gamma] = 107.627 (3)°

  • V = 1684.9 (6) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 0.47 mm-1

  • T = 90 K

  • 0.15 × 0.11 × 0.08 mm
Data collection

  • Bruker SMART APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.952, Tmax = 0.972

  • 17931 measured reflections

  • 6092 independent reflections

  • 4083 reflections with I > 2[sigma](I)

  • Rint = 0.064
Refinement

  • R[F2 > 2[sigma](F2)] = 0.061

  • wR(F2) = 0.173

  • S = 1.03

  • 6092 reflections

  • 433 parameters

  • 258 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.54 e Å-3

  • [Delta][rho]min = -0.81 e Å-3

Table 1
Selected bond lengths (Å)

Mn1-O1 1.817 (3)
Mn1-O1i 1.821 (3)
Mn1-N1 2.187 (5)
Mn1-N2 2.092 (3)
Mn1-N3 2.178 (3)
Mn1-N4 2.116 (3)
Symmetry code: (i) -x, -y+1, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1...N5 0.93 2.42 3.313 (11) 160
N1-H1...N5B 0.93 1.98 2.832 (10) 151
N2-H2...Cl1 0.93 2.37 3.289 (4) 169
N3-H3...N5i 0.93 2.22 3.034 (9) 146
N3-H3...N5Bi 0.93 2.23 3.120 (9) 160
N4-H4...Cl1 0.93 2.42 3.330 (4) 168
Symmetry code: (i) -x, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HG5039 ).

Acknowledgements

The authors thank the University of California, Davis, for acquisition of the Bruker SMART APEXII diffractometer and the support of the Summer Undergraduate Research Program of the University of California, Davis.

References

Bosnich, B., Poon, C. K. & Tobe, M. L. (1965). Inorg. Chem. 4, 1102-1108.  [CrossRef] [ChemPort] [ISI]
Brewer, K. J., Calvin, M., Lumpkin, R. S., Otvos, J. W. & Spreer, L. O. (1989). Inorg. Chem. 28, 4446-4451.
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Goodson, P. A., Hodgson, D. J. & Michelsen, K. (1990). Inorg. Chim. Acta, 172, 49-57.  [ChemPort]
Levaton, B. B. & Olmstead, M. M. (2010). Acta Cryst. E66, m1226-m1227.  [CrossRef] [details]
Lu, Y.-H., Fun, H.-K., Chantrapromma, S., Razak, I. A., Shen, Z., Zuo, J.-L. & You, X.-Z. (2001). Acta Cryst. C57, 911-913.  [CSD] [CrossRef] [ChemPort] [details]
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]

Acta Cryst (2011). E67, m824-m825   [ doi:10.1107/S1600536811019829 ]

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