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000824943 1001_ $$0P:(DE-HGF)0$$aGörne, Arno L.$$b0$$eCorresponding author
000824943 245__ $$aAmmonothermal Synthesis, Crystal Structure, and Properties of the Ytterbium(II) and Ytterbium(III) Amides and the First Two Rare-Earth-Metal Guanidinates, YbC(NH)$_{3}$ and Yb(CN$_{3}$ H$_{4}$)$_{3}$
000824943 260__ $$aWashington, DC$$bAmerican Chemical Society$$c2016
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000824943 520__ $$aWe report the oxidation-controlled synthesis of the ytterbium amides Yb(NH2)2 and Yb(NH2)3 and the first rare-earth-metal guanidinates YbC(NH)3 and Yb(CN3H4)3 from liquid ammonia. For Yb(NH2)2, we present experimental atomic displacement parameters from powder X-ray diffraction (PXRD) and density functional theory (DFT)-derived hydrogen positions for the first time. For Yb(NH2)3, the indexing proposal based on PXRD arrives at R3̅, a = 6.2477(2) Å, c = 17.132(1) Å, V = 579.15(4) Å3, and Z = 6. The oxidation-controlled synthesis was also applied to make the first rare-earth guanidinates, namely, the doubly deprotonated YbC(NH)3 and the singly deprotonated Yb(CN3H4)3. YbC(NH)3 is isostructural with SrC(NH)3, as derived from PXRD (P63/m, a = 5.2596(2) Å, c = 6.6704(2) Å, V = 159.81(1) Å3, and Z = 2). Yb(CN3H4)3 crystallizes in a structure derived from the [ReO3] type, as studied by powder neutron diffraction (Pn3̅, a = 13.5307(3) Å, V = 2477.22(8) Å3, and Z = 8 at 10 K). Electrostatic and hydrogen-bonding interactions cooperate to stabilize the structure with wide and empty channels. The IR spectra of the guanidinates are compared with DFT-calculated phonon spectra to identify the vibrational modes. SQUID magnetometry shows that Yb(CN3H4)3 is a paramagnet with isolated Yb3+ (4f13) ions. A CONDON 2.0 fit was used to extract all relevant parameters.
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000824943 7001_ $$0P:(DE-HGF)0$$aGeorge, Janine$$b1
000824943 7001_ $$0P:(DE-HGF)0$$avan Leusen, Jan$$b2
000824943 7001_ $$0P:(DE-HGF)0$$aDück, Gerald$$b3
000824943 7001_ $$0P:(DE-HGF)0$$aJacobs, Philipp$$b4
000824943 7001_ $$0P:(DE-Juel1)130778$$aKumar, Naveen$$b5
000824943 7001_ $$0P:(DE-HGF)0$$aDronskowski, Richard$$b6$$eCorresponding author
000824943 773__ $$0PERI:(DE-600)1484438-2$$a10.1021/acs.inorgchem.6b00736$$gVol. 55, no. 12, p. 6161 - 6168$$n12$$p6161 - 6168$$tInorganic chemistry$$v55$$x1520-510X$$y2016
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