Trinuclear Triangular Copper(II) Clusters
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We also obtained the analogous pivalate derivative [Cu3(µ3-
OH)(µ-pz)3{(Me3)CCOO}2{(Me3)CCOOH}], whose synthesis,
through a different procedure, as well as its SCXRD crystal
structure has been recently reported, see J.-H. Zhou, Z. Liu,
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2006, 59, 147–153.
H-bonds concerning data and figures reported in the Support-
ing Information have been obtained by using the CIF files sup-
plied as Supporting Information in refs. 5b (compounds 1 and
4) and 5a (compound 2). To these CIF files are also referred
the atom labels used here.
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The Cambridge Structural Database contains 667 crystal struc-
tures where the [Cu2(RCOO)4] paddlewheel moiety is present
but only 19 of them refer to polymeric unsubstituted copper(II)
carboxylates.
¯
Crystal data for C20H36Cu2O4, A: triclinic, space group P1
(No. 2), a = 5.1829(6), b = 11.1982(13), c = 11.8865(14) Å, α
= 65.631(2)°, β = 88.023(2)°, γ = 88.948(2), V = 628.04(13) Å3,
Z = 1, R (Rw) [I Ͼ 2σ(I)] = 0.0448 (0.1388). The X-ray intensity
data for A were recorded on a Bruker SMART Apex II CCD
area detector diffractometer [λ = 0.71073 Å, T = 293(2) K)].
Cell dimensions and the orientation matrix were initially deter-
mined from a least-squares refinement on reflections measured
in three sets of 20 exposures, collected in three different ω re-
gions and eventually refined against all data. For all crystals, a
full sphere of reciprocal space was scanned in 0.3° ω steps. The
software SMART[10] was used for collecting frames of data,
indexing reflections and determining lattice parameters. The
collected frames were then processed for integration by the
SAINT program[10] and an empirical absorption correction was
applied using SADABS.[11] The structure was solved by direct
methods (SIR 97)[12] and subsequent Fourier syntheses and re-
fined by full-matrix least-squares on F2 (SHELXTL)[13] using
anisotropic thermal parameters for all non-hydrogen atoms.
Some disorder in the carboxylate chains was detected and, in
particular, in one of the chains there was a disorder between
the methyl and ethyl chains bound at C(3) and a second posi-
tion for the methyl [bound to C(9) and alternative to C(10)].
Therefore the site occupation factors of the methyls were re-
fined yielding 0.54 for C(10), 0.26 for C(81) and 0.19 for C(91),
respectively. All hydrogen atoms were added in calculated posi-
tions, included in the final stage of refinement with isotropic
thermal parameters, U(H) = 1.2 Ueq(C) [U(H) = 1.5 Ueq(C–
Me)] and allowed to ride on their carrier carbons. Molecular
graphics were generated using Mercury[14] and Schakal[15] soft-
ware. CCDC-697289 contains the supplementary crystallo-
graphic data for this paper. These data can be obtained free of
charge from The Cambridge Crystallographic Data Centre via
www.ccdc.cam.ac.uk/data_request/cif.
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© 2009 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
www.eurjic.org
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