10.1002/ejic.202000720
European Journal of Inorganic Chemistry
FULL PAPER
1223-336-033;
http://www.ccdc.cam.ac.uk).
E-Mail:
deposit@ccdc.cam.ac.uk,
Acknowledgements
This work was supported by the Julius-Maximilians-Universität
Würzburg and the Deutsche Forschungsgemeinschaft (Ra
720/13).
Crystal Data of (Me2ImMe)∙AlH2I 7 C13H20AlIN2, Mr = 358.19, colorless
block, 0.20 x 0.17 x 0.14 mm, orthorhombic group Pbca, a = 24.6229(3) Å,
b = 8.35440(10) Å, c = 15.6920(2) Å, α = 90°, b = 64.043(5)°, γ = 101.
37770(10)°, V = 3164.57(7) Å3, T = 100(10) K, Z = 8, ρcalcd. = 1.504 g·cm–
3, μ = 16.292, F(000) = 1424, 15990 reflections, in h(–30/31), k(-10/10), l(-
19/19) measured in the range 3.6850 ° < θ < 76.9390°, completeness
98.0 %, 3012 independent reflections, 2946 observed reflections (I > 2σ(I)),
168 parameters, 0 restraints; all data: R1 = 0.0297 and wR2 = 0.0758, I >
2σ(I): R1 = 0.0301 and wR2 = 0.00761, Goof 1.097, largest difference
Keywords: N-Heterocyclic Carbenes • Aluminium • Gallium •
Cations • Main Group Element Hydrides
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(a) R. Brückner, Chapter 14: Oxidations and Reductions. In Advanced
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(c) F. A. Carey, R. J. Sundberg, Reduction of Carbonyl and Other
Functional Groups. In Advanced Organic Chemistry, Part B: Reactions
and Synthesis, Springer US, 1990; pp 219-281.
peak/hole 1.379 /-0.697 e·Å–3
.
Crystal Data of (iPr2ImMe)∙AlH2I 9 C11H22AlIN2, Mr = 336.18, colorless
block, 0.22 x 0.22 x 0.12 mm, monoclinic group C2/c, a = 15.7664(3) Å, b
= 10.9910(2) Å, c = 17.1308(4) Å, α = 90°, b = 90°, b = 90°, V = 3164.57(7)
Å3, T = 99.99(10) K, Z = 8, ρcalcd. = 1.504 g·cm–3, μ = 17.320, F(000) =
1344, 15340 reflections, in h(-13/19), k(-13/13), l(-21/21) measured in the
range 5.5540 ° < θ < 76.4870°, completeness 98.0 %, 2714 independent
reflections, 2434 observed reflections (I > 2σ(I)), 150 parameters, 0
restraints; all data: R1 = 0.0355 and wR2 = 0.0939, I > 2σ(I): R1 = 0.0392
and wR2 = 0.0967, Goof 1.070, largest difference peak/hole 1.735 /-0.892
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43, 7284-7293; (f) R. J. Wehmschulte, P. P. Power, Polyhedron 2000,
19, 1649-1661.
e·Å–3
.
Crystal Data of (Me2ImMe)∙GaH2I 10 C7H14N2GaI, Mr = 322.83, colorless
block, 0.17 x 0.13 x 0.06 mm, monoclinic group P21/n, a = 9.1674(3) Å, b
= 9.9889(2) Å, c = 12.4319(3) Å, α = 90°, b = 108.739(3)°, γ = 90°, V =
1078.07(5) Å3, T = 100.0(5) K, Z = 4, ρcalcd. = 1.989 g·cm–3, μ = 25.555,
F(000) = 616, 5683 reflections, in h(–8/11), k(-12/11), l(-15/11) measured
in the range 3.270 ° < θ < 70.075°, completeness 100.0 %, 2049
independent reflections, 1968 observed reflections (I > 2σ(I)), 112
parameters, 0 restraints; all data: R1 = 0.0444 and wR2 = 0.0456, I > 2σ(I):
R1 = 0.1148 and wR2 = 0.1161, Goof 1.030, largest difference peak/hole
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A. Schneemann, J. L. White, S. Kang, S. Jeong, L. F. Wan, E. S. Cho, T.
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Chem. 2005, 44, 7143-7150.
2.28 /-1.62 e·Å–3
.
H. Schneider, A. Hock, R. Bertermann, U. Radius, Chem. Eur. J. 2017,
23, 12387-12398.
Crystal Data of [(iPr2ImMe)2∙AlH2]I 15 C14H26N4AlI, Mr = 404.28, colorless
block, 0.17 x 0.01 x 0.06 mm, triclinic group P¯1, a = 10.1308(3) Å, b =
13.0257(4) Å, c = 13.5023(5) Å, α = 76.396(3)°, b = 82.890(3)°, b =
79.406(3)°, V = 1696.21(1) Å3, T = 100.01(1) K, Z = 2, ρcalcd. = 1.241 g·cm–
3, μ = 7.833, F(000) = 662, 14143 reflections, in h(-12/12), k(-15/19), l(-
16/16) measured in the range 3.380 ° < θ < 72.101°, completeness 99.7 %,
6674 independent reflections, 6226 observed reflections (I > 2σ(I)), 354
parameters, 0 restraints; all data: R1 = 0.0377 and wR2 = 0.0400, I > 2σ(I):
R1 = 0.0994 and wR2 = 0.1007, Goof 1.090, largest difference peak/hole
L. L. Cao, E. Daley, T. C. Johnstone, D. W. Stephan, Chem. Comm. 2016,
52, 5305-7.
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Int. Ed. 2013, 52, 4941-4944; Angew. Chem. 2013, 125, 5041-5044.
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2018, 644, 1243-1251; (b) H. Schneider, A. Hock, A. D. Jaeger, D. Lentz,
U. Radius, Eur. J. Inorg. Chem. 2018, 2018, 4031-4043.
1.40 /-1.08 e·Å–3
.
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2014, 275, 63-86; (b) V. Nesterov, D. Reiter, P. Bag, P. Frisch, R. Holzner,
A. Porzelt, S. Inoue, Chem. Rev. 2018, 118, 9678-9842; (c) A. J.
Arduengo III, H. R. Dias, J. C. Calabrese, F. Davidson, J. Am. Chem.
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C. Jones, M. Kloth, J. Organomet. Chem. 2002, 656, 203-210; (f) A. R.
Leverett, M. L. Cole, A. I. McKay, Dalton Trans. 2019, 48, 1591-1594.
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P. Bag, A. Porzelt, P. J. Altmann, S. Inoue, J. Am. Chem. Soc. 2017, 139,
14384-14387.
Crystal Data of [(Me2ImMe)2∙GaH2]I 16 C14H26N4GaI, Mr = 447.02,
colorless block, 0.15 x 0.09 x 0.06 mm, monoclinic group P21/n, a =
11.8570(4) Å, b = 11.7644(3) Å, c = 13.5361(5) Å, α = 90°, b = 90.219(3)°,
b = 90°, V = 1888.14(11) Å3, T = 99.99(10) K, Z = 4, ρcalcd. = 1.572 g·cm–3
,
μ = 14.799, F(000) = 888, 4267 reflections, in h(-11/14), k(-16/6), l(-16/16)
measured in the range 4.968 ° < θ < 68.230°, completeness 95.9 %, 3314
independent reflections, 2923 observed reflections (I > 2σ(I)), 197
parameters, 0 restraints; all data: R1 = 0.0381 and wR2 = 0.0428, I > 2σ(I):
R1 = 0.0994 and wR2 = 0.1031, Goof 1.029, largest difference peak/hole
1.60 /-0.60 e·Å–3
.
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4852-4857; (b) S. J. Bonyhady, D. Collis, G. Frenking, N. Holzmann, C.
Jones, A. Stasch, Nat. Chem. 2010, 2, 865-9.
Crystal Data of [(Dipp2Im)∙GaH2(aDipp2Im)]I 18 C54H74N4GaI, Mr
=
975.79, colorless block, 0.24 x 0.15 x 0.13 mm, monoclinic group P21/n, a
= 10.86080(10) Å, b = 22.4035(3) Å, c = 21.5667(2) Å, α = 90°, b =
92.6500(10)°, b = 90°, V = 5242.00(10) Å3, T = 100.00(10) K, Z = 4, ρcalcd.
= 1.236 g·cm–3, μ = 5.607, F(000) = 2040, 27454 reflections, in h(-12/13),
k(-28/27), l(--26/23) measured in the range 2.846 ° < θ < 77.506°,
completeness 97.6 %, 10888 independent reflections, 10009 observed
reflections (I > 2σ(I)), 565 parameters, 0 restraints; all data: R1 = 0.0383
and wR2 = 0.0417, I > 2σ(I): R1 = 0.1017 and wR2 = 0.1036, Goof 1.059,
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2009, 16, 2909-2911; (b) S. G. Alexander, M. L. Cole, C. M. Forsyth,
Chem. Eur. J. 2009, 15, 9201-14; (c) S. G. Alexander, M. L. Cole, M.
Hilder, J. C. Morris, J. B. Patrick, Dalton Trans. 2008, 45, 6361-6363.; (d)
G. E. Ball, M. L. Cole, A. I. McKay, Dalton Trans. 2012, 41, 946-952; (e)
A. K. Swarnakar, M. J. Ferguson, R. McDonald, E. Rivard, , Dalton Trans.
2017, 46, 1046-1412; R. J. Wehmschulte, R. Peverati, D. R. Powell,
largest difference peak/hole 1.19 /-1.68 e·Å–3
.
8
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