FULL PAPER
[Eu(Odpp)3(dme)]). Data collected on the Bruker X8 APEX II
CCD were empirically corrected for absorption (SADABS[27]) then
merged. Data collection and integration on the MX1: Macromolec-
ular Crystallography beamline were carried out using Blu-Ice[28]
and the XDS software package.[29] The structures were solved using
SHELXS[30] and refined by full-matrix least-squares cycles on all
F2 data using SHELX,[30] in conjunction with the X-Seed graphical
user interface.[31] All hydrogen atoms were placed in calculated po-
sitions using the riding model.
Crystal Data for [Eu3(Omes)6(thf)6]: C78H114Eu3O12, Mr = 1699.57,
pale yellow block, 0.04ϫ0.04ϫ0.03 mm , triclinic, space group P1
3
¯
(no. 2), a = 11.790(2) Å, b = 12.180(2) Å, c = 14.270(3) Å, α =
110.07(3)°, β = 98.65(3)°, γ = 96.94(3)°, V = 1869.7(7) Å3, Z = 1,
Dcalcd. = 1.509 gcm–3, F(000) = 867, ADSC Quantum 210r, syn-
chrotron radiation, λ = 0.71080 Å, T = 100 K, 2θmax = 55.0°, 45213
reflections collected, 8552 unique (Rint = 0.0764). Final GOF =
1.118, R1 = 0.0413, wR2 = 0.1091, R indices based on 7838 reflec-
tions with IϾ2σ(I) (refinement on F2), 430 parameters, 0 restraints.
Lp and absorption corrections applied, μ = 2.544 mm–1.
CCDC-967213 (for [La(Odbmp)3(NCMe)2]·2MeCN), -967212 (for
[Eu(Odbmp)2(thf)3]·thf), -967211 (for [Eu(Odpp)2(dme)2]), -967209
(for [Eu(Odpp)3(dme)]) and -967210 (for [Eu3(Omes)6(thf)6]) con-
tain the supplementary crystallographic data for this paper. These
data can be obtained free of charge from The Cambridge Crystallo-
graphic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
Supporting Information (see footnote on the first page of this arti-
cle): Selected bond lengths and angles for [Eu(Odpp)2(dme)2] and
[Yb(Odpp)2(dme)2] and the molecular structure of [Eu3(Omes)6-
(thf)6].
Crystal Data for [La(Odbmp)3(NCMe)2]·2MeCN: C53H81LaN4O3,
Mr = 961.13, colourless block, 0.14ϫ0.12ϫ0.05 mm3, triclinic,
space group P1 (no. 2), a = 11.0333(5) Å, b = 12.4987(6) Å, c =
Acknowledgments
¯
The authors thank the Australian Research Council for support
including a scholarship for S. H. Dean’s Scholarship support for
S. H. and R. P. K. is also acknowledged. Aspects of this research
were undertaken on the MX1 beamline at the Australian Synchro-
tron, Victoria, Australia.
20.9264(9) Å, α = 75.401(2)°, β = 88.544(2)°, γ = 70.837(2)°, V =
2632.7(2) Å3, Z = 2, Dcalcd. = 1.212 gcm–3, F(000) = 1016, Bruker
X8 Apex II CCD, Mo-Kα radiation, λ = 0.71073 Å, T = 123(1) K,
2θmax = 55.0°, 39349 reflections collected, 12030 unique (Rint
=
0.0269). Final GOF = 0.979, R1 = 0.0283, wR2 = 0.0755, R indices
based on 11016 reflections with IϾ2σ(I) (refinement on F2), 575
parameters, 0 restraints. Lorentz polarization (Lp) and absorption
corrections applied, μ = 0.854 mm–1.
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Crystal Data for [Eu(Odbmp)2(thf)3]·thf: C46H78EuO6, Mr = 879.04,
yellow block, 0.20ϫ0.10ϫ0.05 mm3, monoclinic, space group P21
(no. 4), a = 9.7984(6) Å, b = 15.1389(13) Å, c = 15.4681(11) Å, β
= 95.266(4)°, V = 2284.8(3) Å3, Z = 2, Dcalcd. = 1.278 gcm–3, F(000)
= 930, Bruker X8 Apex II CCD, Mo-Kα radiation, λ = 0.71073 Å,
T = 123(1) K, 2θmax = 50.0°, 13981 reflections collected, 7910
unique (Rint = 0.0498). Final GOF = 1.095, R1 = 0.0526, wR2 =
0.1160, R indices based on 6668 reflections with IϾ2σ(I) (refine-
ment on F2), 492 parameters, 19 restraints. Lp and absorption cor-
rections applied, μ = 1.416 mm–1. Absolute structure parameter =
0.09(2).[32]
Crystal Data for [Eu(Odpp)2(dme)2]: C44H46EuO6, Mr = 822.77,
yellow/orange prism, 0.35ϫ0.25ϫ0.06 mm3, triclinic, space group
¯
P1 (no. 2), a = 8.9740(2) Å, b = 10.3834(2) Å, c = 21.1732(5) Å, α
=
95.6390(10)°, β = 91.3230(10)°, γ = 109.0810(10)°, V =
1852.31(7) Å3, Z = 2, Dcalcd. = 1.475 gcm–3, F(000) = 842, Bruker
X8 Apex II CCD, Mo-Kα radiation, λ = 0.71073 Å, T = 123(1) K,
2θmax = 50.0°, 25379 reflections collected, 6374 unique (Rint
=
0.0409). Final GOF = 1.045, R1 = 0.0320, wR2 = 0.0671, R indices
based on 5676 reflections with IϾ2σ(I) (refinement on F2), 464
parameters, 6 restraints. Lp and absorption corrections applied, μ
= 1.742 mm–1.
Crystal Data for [Eu(Odpp)3(dme)]: C58H49EuO5, Mr = 977.93,
orange prism, 0.12ϫ0.06ϫ0.05 mm3, monoclinic, space group
P21/n (no. 14), a = 10.054(2) Å, b = 20.987(4) Å, c = 24.808(5) Å,
β = 94.11(3)°, V = 5221.1(18) Å3, Z = 4, Dcalcd. = 1.244 gcm–3,
F(000) = 2000, ADSC Quantum 210r, synchrotron radiation, λ =
0.71080 Å, T = 100 K, 2θmax = 50.0°, 60244 reflections collected,
11091 unique (Rint = 0.0572). Final GOF = 1.062, R1 = 0.0294,
wR2 = 0.0769, R indices based on 8978 reflections with IϾ2σ(I)
(refinement on F2), 579 parameters, 0 restraints. Lp and absorption
corrections applied, μ = 1.246 mm–1. After refinement of the pri-
mary molecule, attempts to model the residual electron density in
the lattice voids as disordered solvents gave unsatisfactory refine-
ments. Subsequently, the electron density in voids was accounted
for using PLATON/SQUEEZE.
[6] a) K. Mashima, H. Fukumoto, Y. Nakayama, K. Tani, A.
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Eur. J. Inorg. Chem. 2014, 460–468
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