Crystal Structures of Two 1,4-Diamino-1,2,4-triazolium Salts
Abstract
:1. Introduction
2. Results and Discussion
Compound | 1 | 2 |
---|---|---|
CCDC No. | 1441522 | 1441523 |
Empirical formula | 2(C2H6N5)·O4S | 2(C2H6N5)·C2N10 |
Formula weight | 296.30 | 364.36 |
Crystal system | Monoclinic | Monoclinic |
Space group | Pc | P21/c |
a/Å | 11.0114(3) | 3.5735(3) |
b/Å | 8.4671(2) | 14.8270(12) |
c/Å | 12.8156(5) | 13.4559(11) |
β/° | 92.356(3) | 95.664(3) |
Volume/Å3 | 1193.85(6) | 709.47(10) |
Z | 4 | 2 |
Dx/g·cm−3 | 1.648 | 1.706 |
μ/mm−1 | 0.31 | 0.13 |
F(000) | 616 | 376 |
T/K | 173 | 183 |
Crystal size/mm3 | 0.54 × 0.20 × 0.16 | 0.18 × 0.04 × 0.03 |
θmax/° | 25.4 | 25.0 |
Index ranges | –13 ≤ h ≤ 11, –10 ≤ k ≤ 10, –14 ≤ l ≤ 15 | –4 ≤ h≤ 3, –17 ≤ k ≤ 17, –15 ≤ l ≤ 15 |
Reflections collected | 7080 | 9515 |
Independent reflections (Rint) | 3571 (0.028) | 1250 (0.060) |
Observed reflections [I > 2σ(I)] | 3428 | 1001 |
Absorption correction | multi-scan | multi-scan |
Restraints/parameters | 18/392 | 4/135 |
Goodness-of-fit on F2 | 1.09 | 1.06 |
R1/wR2 [I > 2σ(I)] | 0.026/0.077 | 0.037/0.092 |
R1/wR2 (all data) | 0.029/0.079 | 0.052/0.098 |
Δρmax/Δρmin/e.Å−3 | 0.23/–0.25 | 0.54/–0.22 |
2.1. Bis(1,4-diamino-1,2,4-triazolium) Sulfate (1)
Compound | Interaction | H···A | D···A | D–H···A | Symmetry Operation A |
---|---|---|---|---|---|
1 | N5A–H51A···O5 | 2.04(2) | 2.913(3) | 160(3) | x, y, z |
N5A–H52A···O3 | 2.04(2) | 2.946(3) | 173(3) | x, y, z | |
N3C–H31C···O1 | 2.11(3) | 3.008(3) | 169(3) | x, y, z | |
N3C–H31C···O3 | 2.48(3) | 3.115(3) | 128(3) | x, y, z | |
N3C–H32C···O5 | 2.19(3) | 2.962(4) | 144(3) | x, −y, −1/2 + z | |
N3B–H31B···O2 | 2.15(2) | 2.932(3) | 145(3) | x, 1 + y, z | |
N3B–H32B···O7 | 2.07(2) | 2.951(3) | 172(3) | 1 + x, y, z | |
N5D–H51D···O8 | 2.06(3) | 2.871(3) | 151(3) | x, y, z | |
N5D–H52D···O2 | 2.16(2) | 2.996(3) | 155(3) | −1 + x, y, z | |
N3D–H31D···O1 | 2.00(2) | 2.889(3) | 163(3) | x, y, z | |
N3D–H32D···O5 | 2.16(2) | 3.042(4) | 170(3) | x, −1 + y, z | |
N5B–H51B···O4 | 2.14(2) | 2.989(4) | 162(3) | x, −y, −1/2 + z | |
N5B–H52B···N3A | 2.26(2) | 3.108(4) | 159(3) | x, −y, −1/2 + z | |
N5C–H52C···O5 | 2.11(3) | 2.922(4) | 152(3) | x, 1 − y, −1/2 + z | |
N3A–H31A···O6 | 2.03(2) | 2.874(3) | 157(3) | 1 + x, y, z | |
N3A–H32A···O2 | 1.98(2) | 2.856(3) | 166(3) | x, −y, 1/2 + z | |
N3B–H32B···O8 | 2.54(3) | 3.123(3) | 124(2) | 1 + x, y, z | |
N5C–H51C···O1 | 2.56(3) | 3.353(3) | 150(3) | x, 1 + y, z | |
N5C–H51C···N3D | 2.68(3) | 3.301(4) | 129(2) | x, 1 + y, z | |
2 | N10–HA···N3 | 2.12(2) | 3.018(2) | 169(2) | x, y, z |
N10–HB···N1 | 2.16(2) | 3.048(2) | 167(2) | x, 3/2 – y, –1/2 + z | |
N8–HA···N2 | 2.38(2) | 3.152(2) | 146(2) | 1 – x, 1 – y, 1 – z | |
N8–HB···N4 | 2.64(3) | 3.221(2) | 125(2) | –x, –1/2 + y, 1/2 – z |
2.2. Bis(1,4-diamino-1,2,4-triazolium) 5,5′-Azotetrazolate (2)
2.3. Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA)
3. Experimental Section
3.1. Bis(1,4-diamino-1,2,4-triazolium) Sulfate (1)
3.2. Bis(1,4-diamino-1,2,4-triazolium) 5,5′-Azotetrazolate (2)
4. Conclusions
Author Contributions
Conflicts of Interest
References
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Laus, G.; Wurst, K.; Kahlenberg, V.; Schottenberger, H. Crystal Structures of Two 1,4-Diamino-1,2,4-triazolium Salts. Crystals 2016, 6, 13. https://doi.org/10.3390/cryst6010013
Laus G, Wurst K, Kahlenberg V, Schottenberger H. Crystal Structures of Two 1,4-Diamino-1,2,4-triazolium Salts. Crystals. 2016; 6(1):13. https://doi.org/10.3390/cryst6010013
Chicago/Turabian StyleLaus, Gerhard, Klaus Wurst, Volker Kahlenberg, and Herwig Schottenberger. 2016. "Crystal Structures of Two 1,4-Diamino-1,2,4-triazolium Salts" Crystals 6, no. 1: 13. https://doi.org/10.3390/cryst6010013
APA StyleLaus, G., Wurst, K., Kahlenberg, V., & Schottenberger, H. (2016). Crystal Structures of Two 1,4-Diamino-1,2,4-triazolium Salts. Crystals, 6(1), 13. https://doi.org/10.3390/cryst6010013