Synthesis, Crystal Structure and Thermal Stability of 1D Linear Silver(I) Coordination Polymers with 1,1,2,2-Tetra(pyrazol-1-yl)ethane
Abstract
:1. Introduction
2. Results and Discussion
2.1. Synthesis of Coordination Polymers
2.2. Crystal Structures
2.3. Thermal and XRD Analyses
2.4. Solid-State Luminescence Studies
3. Experimental Section
3.1. Materials and Methods
3.2. Synthesis of Compounds
3.2.1. Synthesis of {[Ag(µ2‑Pz4)(NO3)]·DMF}n (1)
3.2.2. Synthesis of [{Ag(µ2‑Pz4)(NO3)}n] (2)
4. Conclusions
Supplementary Materials
Acknowledgments
Author Contributions
Conflicts of Interest
Appendix A
References
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Parameter | Compound 1 | Compound 2 |
---|---|---|
ν3, cm−1 | 1390 1294 | 1393 1309 |
Δν3, cm−1 | 96 | 84 |
ν4, cm−1 | 770 | 755 |
l2-l1, Å 1 | 0.699 | 0.932 |
A1-A2, ° 1 | 33.49 | 47.72 |
l3-l2, Å 1 | 0.006 | −0.085 |
Parameter | Compound 1 | Compound 2 |
---|---|---|
Empirical formula | C17H21AgN10O4 | C14H14AgN9O3 |
Formula weight | 537.31 | 464.21 |
Crystal system | Monoclinic | Triclinic |
Space group | P21/n | P-1 |
Unit cell dimensions a, Å | 9.394(2) | 7.8650(9) |
b, Å | 14.299(4) | 8.8031(10) |
c, Å | 15.793(4) | 13.2418(15) |
α, ° | 90 | 74.380(4) |
β, ° | 94.173(7) | 76.990(3) |
γ, ° | 90 | 83.647(4) |
Volume, Å3 | 2115.7(9) | 859.07(17) |
Z | 4 | 2 |
Density (calcd.), g·cm−3 | 1.687 | 1.795 |
F(000) | 1088 | 464 |
Abs. coefficient, mm-1 | 1.001 | 1.211 |
Crystal size, mm3 | 0.8 × 0.15 × 0.15 | 0.32 × 0.08 × 0.08 |
2θmax, ° | 51.38 | 53.58 |
Index range | −11 ≤ h ≤11 −17 ≤ k ≤17 −19 ≤ l ≤11 | −9 ≤ h ≤ 9 −10 ≤ k ≤ 8 −16 ≤ l ≤ 16 |
Reflections collected | 14199 | 7730 |
Independent reflections | 3967 [R(int) = 0.0215] | 3239 [R(int) = 0.0549] |
Completness to 2θ = 51.38, % | 98.7 | 99.4 |
Reflections, I ≥ 2σ(I) | 3786 | 2328 |
Parameters | 291 | 250 |
Final R indices [I > 2σ(I)] | R1 = 0.0665 wR2 = 0.1958 | R1 = 0.0681 wR2 = 0.1577 |
R indices (all data) | R1 = 0.0679 wR2 = 0.1962 | R1 = 0.0924 wR2 = 0.1771 |
GoF | 1.277 | 1.037 |
Residual electron density (min/max, e/Å3) | −0.931/2.534 | −2.227/1.646 |
Parameter | {[Ag(µ2‑Pz4)(NO3)]DMF}n (1) | [{Ag(µ2‑Pz4)(NO3)}n] (2) |
---|---|---|
α (°) | 128.0 | 141.5 |
β (°) | 166.8 | 178.0 |
τ5 = (β – α)/60 | 0.64 | 0.61 |
Parameter | {[Ag(µ2‑Pz4)(NO3)]DMF}n (1) | [{Ag(µ2‑Pz4)(NO3)}n] (2) |
---|---|---|
Ag–N12 | 2.41 | 2.30 |
Ag–N14 | 2.40 | 2.63 |
Ag–N22 | 2.54 | 2.49 |
Ag–N24 | 2.40 | 2.31 |
Ag–O1 | 2.58 | 2.60 |
Parameter | Nmn–C1–C1’–Nmn | C1–C1’–Nmn–Nmn |
---|---|---|
{[Ag(µ2‑Pz4)(NO3)]DMF}n (1) | ±55.5; ±54.8 | ±57.9; ±53.8; ±50.4; ±54.8 |
[{Ag(µ2‑Pz4)(NO3)}n] (2) | ±54.8; ±54.0 | ±57.6; ±58.1; ±50.5; ±58.2 |
[Cu2(µ2‑Pz4)(H2O)2(NO3)4] [21] | −58.9; 56.1; −57.3; 55.4 | 60.8; −70.4; 69.1; −61.7 70.4; −61.5; 63.2; −67.0 |
[Cu2(µ2‑Pz4)(H2O)6(NO3)4] [22] | 52.6; −61.7 | 59.5; −74.9; 67.7; −61.0. |
[Cu(Pz4)(NO3)2]n [22] | ±56.0 | ±72.2; ±61.5; |
[{Cu(Pz4)(H2O)(NO3)2}2]n [22] | ±55.3 | ±70.0; ±72.5 |
Thermolysis Conditions (T, Annealing Time) | Crystallite Size Range for Different Atmospheres (nm) | |
---|---|---|
He | H2/He (7.2%) | |
400 °C, 0 h | 12–23 | 11–20 |
400 °C, 3 h | - | 9–20 |
400 °C, 10 h | 17–30 | 10–20 |
600 °C, 0 h | - | 10–21 |
800 °C, 0 h | 26–53 | - |
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Semitut, E.; Komarov, V.; Sukhikh, T.; Filatov, E.; Potapov, A. Synthesis, Crystal Structure and Thermal Stability of 1D Linear Silver(I) Coordination Polymers with 1,1,2,2-Tetra(pyrazol-1-yl)ethane. Crystals 2016, 6, 138. https://doi.org/10.3390/cryst6110138
Semitut E, Komarov V, Sukhikh T, Filatov E, Potapov A. Synthesis, Crystal Structure and Thermal Stability of 1D Linear Silver(I) Coordination Polymers with 1,1,2,2-Tetra(pyrazol-1-yl)ethane. Crystals. 2016; 6(11):138. https://doi.org/10.3390/cryst6110138
Chicago/Turabian StyleSemitut, Evgeny, Vladislav Komarov, Taisiya Sukhikh, Evgeny Filatov, and Andrei Potapov. 2016. "Synthesis, Crystal Structure and Thermal Stability of 1D Linear Silver(I) Coordination Polymers with 1,1,2,2-Tetra(pyrazol-1-yl)ethane" Crystals 6, no. 11: 138. https://doi.org/10.3390/cryst6110138
APA StyleSemitut, E., Komarov, V., Sukhikh, T., Filatov, E., & Potapov, A. (2016). Synthesis, Crystal Structure and Thermal Stability of 1D Linear Silver(I) Coordination Polymers with 1,1,2,2-Tetra(pyrazol-1-yl)ethane. Crystals, 6(11), 138. https://doi.org/10.3390/cryst6110138