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Volume 64 
Part 11 
Pages m1370-m1371  
November 2008  

Received 24 September 2008
Accepted 30 September 2008
Online 9 October 2008

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Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.003 Å
R = 0.021
wR = 0.054
Data-to-parameter ratio = 15.7
Details
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Di-[mu]3-oxido-di-[mu]2-oxido-tetraoxidobis(1,1,2,2-tetramethylethylenedicyclopentadienyl)dimolybdenum(IV)dimolybdenum(VI) hexahydrate

Takiya J. Ahmed,a Lev N. Zakharova and David R. Tylera*

aDepartment of Chemistry, 1253 University of Oregon, Eugene, Oregon 97403-1253, USA
Correspondence e-mail: dtyler@uoregon.edu

The title compound, [Mo4(C16H20)2O8]·6H2O, is a centrosymmetric ansa-molybdocene complex in which two dinuclear [C2Me4([eta]5-C5H4)2]Mo([mu]2-O)2MoO2 units dimerize by forming two [mu]3-O bridges between three Mo atoms. The ansa-molybdocene [C2Me4([eta]5-C5H4)2]Mo unit has a typical bent-sandwich metallocene structure with an inter-ring angle of 127.98 (8)°. The Mo atom in the bridging ([mu]2-O)([mu]3-O)2MoO2 group has a distorted trigonal-bipyramidal coordination. The Mo-([mu]3-O) and Mo-([mu]2-O) bond distances inside the units [2.0869 (14) and 2.1014 (15) Å, respectively] are slightly longer than the Mo(-x + 1, -y + 1, -z)-([mu]3-O) bond distance between the units [1.9986 (14) Å]. The solvent water molecules together with complex O atoms form a network of O-H...O hydrogen bonds.

Related literature

For related structures, see: Prout & Daran (1978[Prout, K. & Daran, J.-C. (1978). Acta Cryst. B34, 3586-3591.]); Adam & Green (1981[Adam, G. J. S. & Green, M. L. H. (1981). J. Organomet. Chem. 208, 299-308.]); Daran & Prout (1977[Daran, J. C., Prout, K., Adam, G. J. S., Green, M. L. H. & Sala-Pala, J. (1977). J. Organomet. Chem. 131, C40-C42.]); Prout et al. (1974[Prout, K., Cameron, T. S., Forder, R. A., Critchley, S. R., Denton, B. & Rees, G. V. (1974). Acta Cryst. B30, 2290-2304.]). For general synthesis and reactivity information on related tetramethylethylene-bridged ansa-molybdocene complexes, see: Ahmed et al. (2007[Ahmed, T. J., Zakharov, L. N. & Tyler, D. R. (2007). Organometallics, 26, 5179-5187.]).

[Scheme 1]

Experimental

Crystal data

  • [Mo4(C16H20)2O8]·6H2O

  • Mr = 1044.50

  • Triclinic, [P \overline 1]

  • a = 7.4106 (7) Å

  • b = 9.3518 (8) Å

  • c = 13.5735 (12) Å

  • [alpha] = 93.365 (1)°

  • [beta] = 98.604 (1)°

  • [gamma] = 103.175 (1)°

  • V = 901.39 (14) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 1.43 mm-1

  • T = 173 (2) K

  • 0.30 × 0.09 × 0.07 mm
Data collection

  • Bruker APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.673, Tmax = 0.907

  • 10175 measured reflections

  • 3916 independent reflections

  • 3621 reflections with I > 2[sigma](I)

  • Rint = 0.014
Refinement

  • R[F2 > 2[sigma](F2)] = 0.021

  • wR(F2) = 0.054

  • S = 1.09

  • 3916 reflections

  • 250 parameters

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

  • [Delta][rho]max = 0.46 e Å-3

  • [Delta][rho]min = -0.41 e Å-3

Table 1
Selected bond lengths (Å)

Mo1-O1 2.0869 (14)
Mo1-O2 2.1014 (15)
Mo2-O4 1.7217 (16)
Mo2-O3 1.7237 (16)
Mo2-O2 1.8385 (15)
Mo2-O1i 1.9986 (14)
Mo2-O1 2.0481 (15)
Symmetry code: (i) -x+1, -y+1, -z.

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1S-H2S...O3Sii 0.76 (4) 2.02 (4) 2.771 (3) 169 (4)
O3S-H6S...O2S 0.80 (4) 1.99 (4) 2.792 (3) 175 (3)
O2S-H4S...O4i 0.76 (4) 2.16 (4) 2.908 (3) 167 (4)
O3S-H5S...O1Siii 0.81 (4) 2.06 (4) 2.850 (3) 163 (3)
O2S-H3S...O1S 0.76 (4) 2.12 (4) 2.865 (3) 165 (4)
O1S-H1S...O3i 0.82 (3) 2.01 (3) 2.816 (3) 167 (3)
Symmetry codes: (i) -x+1, -y+1, -z; (ii) x+1, y, z; (iii) -x+1, -y+1, -z+1.

Data collection: SMART (Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB2806 ).

Acknowledgements

We thank the NSF for funding.

References

Adam, G. J. S. & Green, M. L. H. (1981). J. Organomet. Chem. 208, 299-308.  [CrossRef] [ChemPort]
Ahmed, T. J., Zakharov, L. N. & Tyler, D. R. (2007). Organometallics, 26, 5179-5187.  [CrossRef] [ChemPort]
Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Daran, J. C., Prout, K., Adam, G. J. S., Green, M. L. H. & Sala-Pala, J. (1977). J. Organomet. Chem. 131, C40-C42.  [CrossRef] [ChemPort]
Prout, K., Cameron, T. S., Forder, R. A., Critchley, S. R., Denton, B. & Rees, G. V. (1974). Acta Cryst. B30, 2290-2304.  [CrossRef] [details]
Prout, K. & Daran, J.-C. (1978). Acta Cryst. B34, 3586-3591.  [CrossRef] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]

Acta Cryst (2008). E64, m1370-m1371   [ doi:10.1107/S1600536808031668 ]

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