Solvothermal Synthesis, Crystal Structure, and Characterization of a Heterometallic Iodoplumbate
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials and Measurements
2.2. Preparation of [PbCu2I4(bipy)]n (1)
2.3. X-ray Crystallography
3. Results and Discussion
3.1. Synthesis
3.2. Structure Description
3.3. Thermal Stability
3.4. Diffuse Reflectance Spectroscopy
3.5. Luminescence Property
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Conflicts of Interest
References
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Molecular Formula | C10H8Cu2I4N2Pb |
---|---|
Formula weight | 998.05 |
Temperature (K) | 293(2) |
Wavelength (Å) | 0.71073 |
Crystal system | Triclinic |
Space group | P |
a (Å) | 4.2520(4) |
b (Å) | 13.1554(8) |
c (Å) | 16.4353(15) |
α (°) | 98.231(6) |
β (°) | 94.171(8) |
γ (°) | 96.090(7) |
V (Å3) | 901.11(13) |
Z | 2 |
Dcalc (g·cm−3) | 3.678 |
μ (mm−1) | 18.497 |
F (000) | 868 |
Crystal size (mm) | 0.3 × 0.15 × 0.15 |
Index range | −5 ≤ h ≤ 5, −16 ≤ k ≤ 17, −19 ≤ l ≤ 22 |
Reflections collected | 7013 |
Independent reflections | 4124 |
Rint | 0.0388 |
θ range (°) | 2.76 to 29.31 |
Data/restraints/parameters | 172/0/3056 |
Goodness–of–fit on F2 | 1.028 |
Final R1, wR2 indices | R1 = 0.0444, wR2 = 0.0855 |
R1a, wR2b indices (all data) | R1 = 0.0674, wR2 = 0.0999 |
Largest differences peak and hole (e Å–3) | 1.038 and −1.780 |
Bond | Lengths | Bond | Lengths | Bond | Lengths |
Pb1–I2 | 3.0679(8) | Pb1–I1 | 3.1217(9) | Pb1–I2A | 3.1679(9) |
Pb1–I4 | 3.2279(9) | Pb1–I4A | 3.3514(9) | Pb1–I3 | 3.3515(9) |
Cu1–N1 | 2.026(9) | Cu1–N2 | 2.076(11) | Cu1–I1B | 2.5635(17) |
Cu1–I1 | 2.6713(19) | Cu2–I4 | 2.6012(17) | Cu2–I3C | 2.6557(19) |
Cu2–I3 | 2.6603(18) | Cu2–I3B | 2.6807(16) | ||
Bond | Angles | Bond | Angles | Bond | Angles |
I2–Pb1–I1 | 87.33(2) | I4–Pb1–I4A | 80.50(2) | N1–Cu1–I1 | 98.7(3) |
I2–Pb1–I2A | 85.96(2) | I2–Pb1–I3 | 84.58(2) | N2–Cu1–I1 | 128.4(3) |
I1–Pb1–I2A | 104.78(3) | I1–Pb1–I3 | 167.95(2) | I1B–Cu1–I1 | 108.62(6) |
I2–Pb1–I4 | 97.23(2) | I2A–Pb1–I3 | 83.59(2) | I4–Cu2–I3B | 108.63(6) |
I1–Pb1–I4 | 89.98(2) | I4–Pb1–I3 | 82.20(2) | I4–Cu2–I3 | 110.62(6) |
I2A–Pb1–I4 | 165.06(3) | I4A–Pb1–I3 | 81.38(2) | I3C–Cu2–I3 | 114.96(6) |
I2–Pb1–I4A | 165.96(3) | N1–Cu1–N2 | 81.1(4) | I4–Cu2–I3B | 111.65(6) |
I1–Pb1–I4A | 106.46(2) | N1–Cu1–I1B | 130.6(3) | I3C–Cu2–I3B | 105.35(6) |
I2A–Pb1–I4A | 92.85(2) | N2–Cu1–I1B | 109.8(3) | I3–Cu2–I3B | 105.52(6) |
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Fan, L.-Q.; Zhu, X.-T. Solvothermal Synthesis, Crystal Structure, and Characterization of a Heterometallic Iodoplumbate. Crystals 2018, 8, 305. https://doi.org/10.3390/cryst8080305
Fan L-Q, Zhu X-T. Solvothermal Synthesis, Crystal Structure, and Characterization of a Heterometallic Iodoplumbate. Crystals. 2018; 8(8):305. https://doi.org/10.3390/cryst8080305
Chicago/Turabian StyleFan, Le-Qing, and Xiao-Tong Zhu. 2018. "Solvothermal Synthesis, Crystal Structure, and Characterization of a Heterometallic Iodoplumbate" Crystals 8, no. 8: 305. https://doi.org/10.3390/cryst8080305