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Volume 69 
Part 10 
Page m527  
October 2013  

Received 7 August 2013
Accepted 30 August 2013
Online 4 September 2013

Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](C-C) = 0.005 Å
R = 0.027
wR = 0.051
Data-to-parameter ratio = 21.6
Details
Open access

Tricarbonylchlorido(6',7'-dihydro-5'H-spiro[cyclohexane-1,6'-dipyrido[3,2-d:2',3'-f][1,3]diazepine]-[kappa]2N1,N11)rhenium(I)

aDepartment of Chemical & Biological Sciences, University of Huddersfield, Queensgate, Huddersfield HD1 3DH, England
Correspondence e-mail: l.p.harding@hud.ac.uk

In the title compound, [ReCl(C16H18N4)(CO)3], the ReI ion is coordinated in a distorted octahedral geometry by one Cl atom, two N atoms of the bidentate ligand and three carbonyl groups. The cyclohexane group is orientated in a transoid fashion with respect to the chloride ligand. In the crystal, N-H...Cl hydrogen bonds link complex molecules, forming a two-dimensional network parallel to (100).

Related literature

For a review of the photophysical properties of Re-polypyridyl complexes, see: Coleman et al. (2008[Coleman, A., Brennan, C., Vos, J. G. & Pryce, M. T. (2008). Coord. Chem. Rev. 252, 2585-2595.]). For the synthesis of [Re(3,3'-diamino-2,2'-bipyridine)(CO)3Cl] and for the preparation of oxo-steroid derivatives of [Re(3,3'-diamino-2,2'-bipyridine)(CO)3Cl], see: Bullock et al. (2012[Bullock, S., Hallett, A. J., Harding, L. P., Higginson, J. J., Piela, S. A. F., Pope, S. J. A. & Rice, C. R. (2012). Dalton Trans. 41, 14690-14696.]). For the reaction of [Re(3,3'-diamino-2,2'-bipyridine)(CO)3Cl] with ketones, see: Clayton et al. (2008[Clayton, H. J., Harding, L. P., Irvine, J. P., Jeffery, J. C., Riis-Johannessen, T., Laws, A. P., Rice, C. R. & Whitehead, M. (2008). Chem. Commun. pp. 108-110.]). For the structure of the cyclopentane analogue of the title compound, see: Clegg et al. (2013[Clegg, O. R., Harding, L. P., Miller, J. W. & Rice, C. R. (2013). Acta Cryst. E69, m526.]).

[Scheme 1]

Experimental

Crystal data
  • [ReCl(C16H18N4)(CO)3]

  • Mr = 572.02

  • Monoclinic, P 21 /c

  • a = 12.6794 (6) Å

  • b = 11.9040 (6) Å

  • c = 12.7732 (6) Å

  • [beta] = 97.066 (1)°

  • V = 1913.29 (16) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 6.52 mm-1

  • T = 150 K

  • 0.10 × 0.10 × 0.03 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS . Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.562, Tmax = 0.828

  • 22579 measured reflections

  • 5590 independent reflections

  • 4543 reflections with I > 2[sigma](I)

  • Rint = 0.039

Refinement
  • R[F2 > 2[sigma](F2)] = 0.027

  • wR(F2) = 0.051

  • S = 1.04

  • 5590 reflections

  • 259 parameters

  • 2 restraints

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

  • [Delta][rho]max = 1.08 e Å-3

  • [Delta][rho]min = -0.74 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N3-H3...Cl1i 0.89 (3) 2.64 (2) 3.417 (3) 146 (3)
N4-H4...Cl1ii 0.89 (3) 2.46 (3) 3.334 (3) 171 (3)
Symmetry codes: (i) [x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]; (ii) -x+1, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS . Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS . 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: OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]); software used to prepare material for publication: OLEX2.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: LH5645 ).


Acknowledgements

The authors wish to thank the University of Huddersfield for financial support.

References

Bruker (2009). APEX2, SAINT and SADABS . Bruker AXS Inc., Madison, Wisconsin, USA.
Bullock, S., Hallett, A. J., Harding, L. P., Higginson, J. J., Piela, S. A. F., Pope, S. J. A. & Rice, C. R. (2012). Dalton Trans. 41, 14690-14696.  [CSD] [CrossRef] [ChemPort] [PubMed]
Clayton, H. J., Harding, L. P., Irvine, J. P., Jeffery, J. C., Riis-Johannessen, T., Laws, A. P., Rice, C. R. & Whitehead, M. (2008). Chem. Commun. pp. 108-110.  [CSD] [CrossRef]
Clegg, O. R., Harding, L. P., Miller, J. W. & Rice, C. R. (2013). Acta Cryst. E69, m526.  [CrossRef] [IUCr Journals]
Coleman, A., Brennan, C., Vos, J. G. & Pryce, M. T. (2008). Coord. Chem. Rev. 252, 2585-2595.  [Web of Science] [CrossRef] [ChemPort]
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m527  [ doi:10.1107/S1600536813024288 ]

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