Synthesis and Crystal Structures of New 5,5'-Azotetrazolates
Abstract
:1. Introduction
2. Results and Discussion
Compound | 1 | 2 | 3 | 4 | 5 |
CCDC no. | 846911 | 846912 | 846913 | 846914 | 846915 |
Chemical formula | Ag2(NH3)2 (C2N10) | (C3H9S)2 (C2N10) | (C4H12P)2·(C2N10) | (C3H9OS)2·(C2N10) | (C5H14NO)2·(C2N10) |
Mr | 413.89 | 318.43 | 346.31 | 350.42 | 372.43 |
Crystal shape, color | plate, orange | prism, yellow | plate, orange | fragment, yellow | fragment, yellow |
Crystal size/mm3 | 0.1 × 0.1 × 0.06 | 0.44 × 0.36 × 0.24 | 0.36 × 0.32 × 0.12 | 0.2 × 0.2 × 0.2 | 0.40 × 0.24 × 0.24 |
Crystal system | monoclinic | triclinic | monoclinic | monoclinic | triclinic |
Space group | C2/c | P | P21/c | P21/n | P |
a/Å | 18.0338(7) | 5.9032(7) | 5.9035(9) | 5.2452(2) | 5.4900(4) |
b/Å | 3.601(2) | 7.4591(8) | 13.388(2) | 14.0290(4) | 8.4206(6) |
c/Å | 14.906(3) | 9.2538(8) | 11.3173(19) | 10.7735(4) | 10.3003(6) |
α/° | 90 | 113.598(9) | 90 | 90 | 78.564(5) |
β/° | 91.94(1) | 98.370(8) | 93.941(17) | 102.036(3) | 85.796(6) |
γ/° | 90 | 99.017(9) | 90 | 90 | 81.876(6) |
V/Å3 | 967.4(6) | 358.88(7) | 892.4 (2) | 775.34 (5) | 461.53(6) |
Z | 8 | 2 | 4 | 4 | 2 |
Dx/g cm–3 | 2.84 | 1.47 | 1.29 | 1.50 | 1.34 |
µ/mm–1 | 4.04 | 0.38 | 0.26 | 0.37 | 0.10 |
F(000)/e | 784 | 168 | 368 | 368 | 200 |
Diffractometer | Nonius KappaCCD | Gemini Ultra | Gemini-R Ultra | Gemini-R Ultra | Gemini-R Ultra |
Data collection method | φand ω scans | ω scans | ω scans | Ω scans | ω scans |
Temperature/K | 233 | 173 | 173 | 173 | 173 |
θmax/° | 24 | 25.4 | 25 | 28 | 25 |
h, k, l range | –19 ≤ h ≤ 20 | –6 ≤ h ≤ 7 | –5 ≤ h ≤ 7 | –6 ≤ h ≤ 6 | –6 ≤ h ≤ 5 |
–4 ≤ k ≤ 3 | –8 ≤ k ≤ 5 | –14 ≤ k ≤ 16 | –18 ≤ k ≤ 17 | –10 ≤ k ≤ 10 | |
–16 ≤ l ≤ 17 | –10 ≤ l ≤ 11 | –15 ≤ l ≤ 13 | –13 ≤ l ≤ 13 | –12 ≤ l ≤ 10 | |
Absorption correction | none | multi-scan | multi-scan | multi-scan | none |
Measured reflections | 1927 | 2168 | 3626 | 6332 | 3070 |
Independent reflections (Rint) | 739 (0.028) | 1288 (0.024) | 1760 (0.021) | 1723 (0.021) | 1686 (0.030) |
Observed reflections [I≥ 2σ(I)] | 620 | 1162 | 1461 | 1573 | 1449 |
Restraints / parameters | 0/75 | 0/94 | 0/104 | 0/103 | 0/123 |
R1/wR2[I ≥ 2σ(I)] | 0.037/0.097 | 0.030/0.070 | 0.030/0.079 | 0.028/0.070 | 0.035/0.095 |
R1/wR2 (all data) | 0.046/0.104 | 0.035/ 0.073 | 0.039/0.082 | 0.031/0.072 | 0.042/0.098 |
Goodness of fit | 1.09 | 1.06 | 1.08 | 1.05 | 1.03 |
Δρmax/min/e Å–3 | 1.38/–0.81 | 0.24/–0.25 | 0.27/–0.24 | 0.34/0.31 | 0.19/–0.17 |
2.1. Bis(amminsilver(I)) 5,5'-Azotetrazolate (1)
2.2. Bis(trimethylsulfonium) 5,5'-Azotetrazolate (2)
2.3. Bis(tetramethylphosphonium) 5,5'-Azotetrazolate (3)
2.4. Bis(trimethylsulfoxonium) 5,5'-Azotetrazolate (4)
2.5. Bis(2-(hydroxyethyl)trimethylammonium) 5,5'-azotetrazolate (5)
3. Experimental Section
3.1. Bis(amminsilver(I)) 5,5'-Azotetrazolate (1)
3.2. Preparation of 5,5'-Azotetrazolates (2–5) (General Procedure)
3.3. Bis(trimethylsulfonium) 5,5'-Azotetrazolate (2)
3.4. Bis(tetramethylphosphonium) 5,5'-Azotetrazolate (3)
3.5. Bis(trimethylsulfoxonium) 5,5'-Azotetrazolate (4)
3.6. Bis(2-(hydroxyethyl)trimethylammonium) 5,5'-Azotetrazolate (5)
4. Conclusions
References and Notes
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Laus, G.; Kahlenberg, V.; Wurst, K.; Schottenberger, H.; Fischer, N.; Stierstorfer, J.; Klapötke, T.M. Synthesis and Crystal Structures of New 5,5'-Azotetrazolates. Crystals 2012, 2, 127-136. https://doi.org/10.3390/cryst2010127
Laus G, Kahlenberg V, Wurst K, Schottenberger H, Fischer N, Stierstorfer J, Klapötke TM. Synthesis and Crystal Structures of New 5,5'-Azotetrazolates. Crystals. 2012; 2(1):127-136. https://doi.org/10.3390/cryst2010127
Chicago/Turabian StyleLaus, Gerhard, Volker Kahlenberg, Klaus Wurst, Herwig Schottenberger, Niko Fischer, Jörg Stierstorfer, and Thomas M. Klapötke. 2012. "Synthesis and Crystal Structures of New 5,5'-Azotetrazolates" Crystals 2, no. 1: 127-136. https://doi.org/10.3390/cryst2010127
APA StyleLaus, G., Kahlenberg, V., Wurst, K., Schottenberger, H., Fischer, N., Stierstorfer, J., & Klapötke, T. M. (2012). Synthesis and Crystal Structures of New 5,5'-Azotetrazolates. Crystals, 2(1), 127-136. https://doi.org/10.3390/cryst2010127