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Volume 69 
Part 5 
Pages m259-m260  
May 2013  

Received 18 March 2013
Accepted 28 March 2013
Online 13 April 2013

Key indicators
Single-crystal X-ray study
T = 295 K
Mean [sigma](C-C) = 0.007 Å
R = 0.038
wR = 0.086
Data-to-parameter ratio = 13.9
Details
Open access

Aquabis(4-methylbenzenesulfonato-[kappa]O)([eta]5-pentamethylcyclopentadienyl)rhodium(III) monohydrate

aDepartment of Chemistry, Virginia Tech, Blacksburg, VA 24061, USA
Correspondence e-mail: jmerola@vt.edu

The title half-sandwich rhodium(III) complex, [Rh(C10H15)(C7H7O3S)2(H2O)]·H2O, consists of a [pi]-bonded pentamethylcyclopentadienyl group, two [sigma]-bonded tosylate groups and an aqua ligand. The structure displays both inter- and intramolecular O-H...O hydrogen bonding. The intermolecular hydrogen bonding results in an extended helical chain along a 21 screw axis parallel to c, due to hydrogen bonding from the coordinating water ligand to the lattice water molecule and then to a sulfonate O atom of a different asymmetric unit.

Related literature

Synthesis details are given in Boyer et al. (1996[Boyer, P. M., Roy, C. P. & Merola, J. S. (1996). Inorg. Chim. Acta, 245, 7-15.]). For the structure of another pentamethylcyclopentadienylmetal bis-tosylate (CCDC: 821138), see: Zaitsev et al. (2008[Zaitsev, A. B., Gruber, S., Pluss, P. A., Pregosin, P. S., Verlos, L. F. & Worle, M. (2008). J. Am. Chem. Soc. 130, 11604-11605.]). For the characterization of other aquo compounds, see: Bergmeister et al. (1990[Bergmeister, J. J., Hanson, B. E. & Merola, J. S. (1990). Inorg. Chem. 29, 4831-4833.]; CCDC: 601561) and Luo et al. (1990[Luo, X. L., Schulte, G. K. & Crabtree, R. H. (1990). Inorg. Chem. 29, 682-686.]; CCDC: 595047). A survey of the geometry and environment of water molecules in crystalline hydrates studied by neutron diffraction can be found in in Ferraris & Franchini-Angela (1972[Ferraris, G. & Franchini-Angela, M. (1972). Acta Cryst. B28, 3572-3583.]).

[Scheme 1]

Experimental

Crystal data
  • [Rh(C10H15)(C7H7O3S)2(H2O)]·H2O

  • Mr = 616.53

  • Orthorhombic, P b c n

  • a = 23.550 (8) Å

  • b = 18.814 (7) Å

  • c = 12.114 (5) Å

  • V = 5367 (3) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 0.84 mm-1

  • T = 295 K

  • 0.4 × 0.4 × 0.4 mm

Data collection
  • Siemens P4 diffractometer

  • Absorption correction: [psi] scan (North et al., 1968[North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.]) Tmin = 0.00, Tmax = 0.881

  • 4738 measured reflections

  • 4738 independent reflections

  • 3297 reflections with I > 2[sigma](I)

  • 3 standard reflections every 200 reflections intensity decay: 0(1)

Refinement
  • R[F2 > 2[sigma](F2)] = 0.038

  • wR(F2) = 0.086

  • S = 1.03

  • 4738 reflections

  • 340 parameters

  • 1 restraint

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

  • [Delta][rho]max = 0.38 e Å-3

  • [Delta][rho]min = -0.29 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O7-H7A...O8 0.85 (5) 1.99 (6) 2.608 (6) 128 (5)
O7-H7B...O3 1.11 (8) 1.64 (8) 2.647 (5) 147 (7)
O8-H8D...O2i 0.77 (8) 2.06 (8) 2.807 (6) 162 (8)
O8-H8E...O5 0.88 (6) 1.91 (6) 2.766 (7) 162 (6)
Symmetry code: (i) [-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}].

Data collection: XSCANS (Siemens, 1994[Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]); cell refinement: XSCANS; data reduction: XSCANS; 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: PK2474 ).


Acknowledgements

We acknowledge the financial support of the NSF (CHE 9214027) and ACS-PRF (23961-ACl). PMB acknowledges an ACS-PRF undergraduate summer fellowship. Funds for the purchase of the diffractometer used in this work were provided by the Commonwealth of Virginia.

References

Bergmeister, J. J., Hanson, B. E. & Merola, J. S. (1990). Inorg. Chem. 29, 4831-4833.  [CrossRef] [ChemPort] [ISI]
Boyer, P. M., Roy, C. P. & Merola, J. S. (1996). Inorg. Chim. Acta, 245, 7-15.  [CrossRef] [ChemPort] [ISI]
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.  [ISI] [CrossRef] [ChemPort] [details]
Ferraris, G. & Franchini-Angela, M. (1972). Acta Cryst. B28, 3572-3583.  [CrossRef] [ChemPort] [details]
Luo, X. L., Schulte, G. K. & Crabtree, R. H. (1990). Inorg. Chem. 29, 682-686.  [CrossRef] [ChemPort] [ISI]
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.  [CrossRef] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
Zaitsev, A. B., Gruber, S., Pluss, P. A., Pregosin, P. S., Verlos, L. F. & Worle, M. (2008). J. Am. Chem. Soc. 130, 11604-11605.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]


Acta Cryst (2013). E69, m259-m260   [ doi:10.1107/S160053681300860X ]

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