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| 100 | 1 | _ | |a Görne, Arno L. |0 P:(DE-HGF)0 |b 0 |e Corresponding author |
| 245 | _ | _ | |a Ammonothermal 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$_{4}$)$_{3}$ |
| 260 | _ | _ | |a Washington, DC |c 2016 |b American Chemical Society |
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| 520 | _ | _ | |a We 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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| 700 | 1 | _ | |a George, Janine |0 P:(DE-HGF)0 |b 1 |
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| 700 | 1 | _ | |a Dück, Gerald |0 P:(DE-HGF)0 |b 3 |
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| 700 | 1 | _ | |a Dronskowski, Richard |0 P:(DE-HGF)0 |b 6 |e Corresponding author |
| 773 | _ | _ | |a 10.1021/acs.inorgchem.6b00736 |g Vol. 55, no. 12, p. 6161 - 6168 |0 PERI:(DE-600)1484438-2 |n 12 |p 6161 - 6168 |t Inorganic chemistry |v 55 |y 2016 |x 1520-510X |
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