1400
S. Schulz et al. · Studies on a β-Diketiminate Zinc Hydride Complex
˚
T = 233 K: δ = 1.40 (s, 6 H, C(CH3)), 1.97 (s, 12 H, o- tometer for 1b (MoKα radiation, λ = 0.71073 A). The
CH3), 2.29 (s, 6 H, p-CH3), 4.78 (s, 1 H, ZnH), 4.76 (s, 1 H, structures were solved by Direct Methods (SHELXS-97
CH), 6.65 (s, 4 H, Ar-H).
[16]) and refined by full-matrix least-squares on F2. Semi-
T = 253 K: δ = 1.43 (s, 6 H, C(CH3)), 1.98 (s, 12 H, o- empirical absorption corrections were applied. All non-
CH3), 2.27 (s, 6 H, p-CH3), 4.69 (s, 1 H, ZnH), 4.79 (s, 1 H, hydrogen atoms were refined anisotropically and hydro-
CH), 6.67 (s, 4 H, Ar-H).
gen atoms by a riding model except for Zn-H, which were
T = 273 K: δ = 1.47 (s, 6 H, C(CH3)), 2.01 (s, 12 H, o- found from the difference fourier maps and refined freely
CH3), 2.23 (s, 6 H, p-CH3), 4.57 (s, 1 H, ZnH), 4.84 (s, 1 H, (SHELXL-97 [17]). Crystal data and parameters pertinent to
CH), 6.70 (s, 4 H, Ar-H).
T = 298 K: δ = 1.53 (s, 6 H, C(CH3)), 2.04 (s, 12 H, o- Table 1.
CH3), 2.19 (s, 6 H, p-CH3), 4.43 (s, 1 H, ZnH), 4.88 (s, 1 H,
the structure determination of 1a and 1b are summarized in
CCDC 745610 (1a) and 745612 (1b) contain the supple-
mentary crystallographic data for this paper. These data can
CH), 6.73 (s, 4 H, Ar-H).
T = 313 K: δ = 1.56 (s, 6 H, C(CH3)), 2.05 (s, 12 H, o- be obtained free of charge from The Cambridge Crystallo-
CH), 6.74 (s, 4 H, Ar-H).
cif.
T = 333 K: δ = 1.58 (s, 6 H, C(CH3)), 2.06 (s, 12 H, o-
CH3), 2.15 (s, 6 H, p-CH3), 4.27 (s, 1 H, ZnH), 4.93 (s, 1 H,
CH), 6.75 (s, 4 H, Ar-H).
T = 353 K: δ = 1.60 (s, 6 H, C(CH3)), 2.07 (s, 12 H, o-
CH3), 2.14 (s, 6 H, p-CH3), 4.21 (s, 1 H, ZnH), 4.94 (s, 1 H,
CH), 6.75 (s, 4 H, Ar-H).
Acknowledgements
S. Schulz and S. Harder like to thank the German Science
Foundation (DFG) for financial support. D. Schuchmann is
grateful to the Fonds der Chemischen Industrie for a doctoral
fellowship.
Crystal structure determination
Data were collected on a Bruker AXS SMART APEX
CCD diffractometer for 1a and on a Stoe IPDS-II diffrac-
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