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Volume 69 
Part 10 
Pages m534-m535  
October 2013  

Received 22 August 2013
Accepted 26 August 2013
Online 7 September 2013

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.010 Å
Disorder in main residue
R = 0.048
wR = 0.112
Data-to-parameter ratio = 15.5
Details
Open access

[[mu]-3,3'-Bis(trihydroboryl)[3]ferrocenophane]bis(chloridozirconocene)

aInstitut für Anorganische Chemie, J. W. Goethe-Universität Frankfurt, Max-von-Laue-Strasse 7, 60438 Frankfurt/Main, Germany
Correspondence e-mail: bolte@chemie.uni-frankfurt.de

The title compound, [FeZr2(C5H5)4Cl2(C13H18B2)], is a heteronuclear complex that consists of a [3]ferrocenophane moiety substituted at each cyclopentadienyl (Cp) ring by a BH3 group; the BH3 group is bonded via two H atoms to the Zr atom of the zirconocene chloride moiety in a bidentate fashion. The two Cp rings of the [3]ferrocenophane moiety are aligned at a dihedral angle of 8.9 (4)° arising from the strain of the propane-1,3-diyl bridge linking the two Cp rings. [One methylene group is disordered over two positions with a site-occupation factor of 0.552 (18) for the major occupied site.] The dihedral angles between the Cp rings at the two Zr atoms are 50.0 (3) and 51.7 (3)°. The bonding Zr...H distances are in the range 1.89 (7)-2.14 (7) Å. As the two Cp rings of the ferrocene unit are connected by an ansa bridge, the two Zr atoms approach each other at 6.485 (1) Å. The crystal packing features C-H...Cl interactions.

Related literature

For Zr...B distances, see: Edelstein (1981[Edelstein, N. (1981). Inorg. Chem. 20, 297-299.]). For information about the coordination behaviour of mono- and ditopic ferrocenylhydroborates toward [Cp2ZrCl]-, see: Reichert et al. (2013a[Reichert, A., Bolte, M., Lerner, H.-W. & Wagner, M. (2013a). Dalton Trans. 42, 688-694.]). For synthetic details, see: Reichert (2013[Reichert, A. (2013). PhD thesis, University of Frankfurt, Germany.]); Reichert et al. (2013b[Reichert, A., Bolte, M., Lerner, H.-W. & Wagner, M. (2013b). J. Organomet. Chem. 744, 15-23.]).

[Scheme 1]

Experimental

Crystal data
  • [FeZr2(C5H5)4Cl2(C13H18B2)]

  • Mr = 765.44

  • Monoclinic, P 21 /c

  • a = 18.2954 (9) Å

  • b = 11.6004 (6) Å

  • c = 15.3351 (6) Å

  • [beta] = 104.963 (3)°

  • V = 3144.3 (3) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.30 mm-1

  • T = 173 K

  • 0.19 × 0.14 × 0.13 mm

Data collection
  • Stoe IPDS II two-circle diffractometer

  • Absorption correction: multi-scan (MULABS; Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]; Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.791, Tmax = 0.849

  • 29348 measured reflections

  • 5885 independent reflections

  • 3926 reflections with I > 2[sigma](I)

  • Rint = 0.102

Refinement
  • R[F2 > 2[sigma](F2)] = 0.048

  • wR(F2) = 0.112

  • S = 0.94

  • 5885 reflections

  • 379 parameters

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

  • [Delta][rho]max = 0.60 e Å-3

  • [Delta][rho]min = -1.22 e Å-3

Table 1
Selected bond lengths (Å)

Zr1-Cl1 2.506 (2)
Zr1-B1 2.551 (6)
Zr2-Cl2 2.4616 (17)
Zr2-B2 2.593 (7)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C25-H25...Cl1i 0.95 2.75 3.466 (7) 133
C28-H28...Cl1ii 0.95 2.80 3.496 (8) 131
C30-H30...Cl2 0.95 2.82 3.623 (7) 143
Symmetry codes: (i) [-x+2, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]; (ii) -x+2, -y, -z+1.

Data collection: X-AREA (Stoe & Cie, 2001[Stoe & Cie (2001). X-AREA. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; 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 and publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG5341 ).


References

Blessing, R. H. (1995). Acta Cryst. A51, 33-38.  [CrossRef] [IUCr Journals]
Edelstein, N. (1981). Inorg. Chem. 20, 297-299.  [CrossRef] [ChemPort] [Web of Science]
Reichert, A. (2013). PhD thesis, University of Frankfurt, Germany.
Reichert, A., Bolte, M., Lerner, H.-W. & Wagner, M. (2013a). Dalton Trans. 42, 688-694.  [CSD] [CrossRef] [ChemPort] [PubMed]
Reichert, A., Bolte, M., Lerner, H.-W. & Wagner, M. (2013b). J. Organomet. Chem. 744, 15-23.  [CSD] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Stoe & Cie (2001). X-AREA. Stoe & Cie, Darmstadt, Germany.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m534-m535   [ doi:10.1107/S1600536813023933 ]

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