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Volume 69 
Part 10 
Page m526  
October 2013  

Received 7 August 2013
Accepted 16 August 2013
Online 4 September 2013

Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](C-C) = 0.004 Å
R = 0.037
wR = 0.075
Data-to-parameter ratio = 44.1
Details
Open access

Tricarbonylchlorido(6',7'-dihydro-5'H-spiro[cyclopentane-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(C15H16N4)(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 cyclopentane group is orientated in a transoid fashion with respect to the chloride ligand. The dihedral angle between the pryridine rings is 10.91 (12)°. In the crystal, N-H...Cl hydrogen bonds link complex molecules, forming a two-dimensional network parallel to (001).

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 cyclohexane analog 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, m527.]).

[Scheme 1]

Experimental

Crystal data
  • [ReCl(C15H16N4)(CO)3]

  • Mr = 558.00

  • Orthorhombic, P b c a

  • a = 12.1162 (5) Å

  • b = 11.9638 (5) Å

  • c = 24.9181 (9) Å

  • V = 3612.0 (2) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 6.90 mm-1

  • T = 150 K

  • 0.50 × 0.50 × 0.20 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 = 0.16, Tmax = 0.34

  • 45382 measured reflections

  • 10757 independent reflections

  • 7941 reflections with I > 2[sigma](I)

  • Rint = 0.053

Refinement
  • R[F2 > 2[sigma](F2)] = 0.037

  • wR(F2) = 0.075

  • S = 1.04

  • 10757 reflections

  • 244 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 2.28 e Å-3

  • [Delta][rho]min = -5.29 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N3-H3A...Cl1i 0.88 2.53 3.363 (3) 158
N4-H4...Cl1ii 0.88 2.65 3.419 (2) 147
Symmetry codes: (i) -x+1, -y+1, -z; (ii) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z].

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: LH5644 ).


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, m527. [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, m526  [ doi:10.1107/S1600536813023076 ]

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