Journal of Synthetic Crystals ›› 2025, Vol. 54 ›› Issue (8): 1463-1469.DOI: 10.16553/j.cnki.issn1000-985x.2025.0026
• Research Articles • Previous Articles Next Articles
LIANG Yinong1(
), ZHANG Kaixin1, XU Yarong1, SUN Zan1,2(
)
Received:2025-02-14
Online:2025-08-20
Published:2025-09-01
CLC Number:
LIANG Yinong, ZHANG Kaixin, XU Yarong, SUN Zan. Synthesis, Crystal Structure and Fluorescent Properties of a Lead-Based Coordination Polymer[J]. Journal of Synthetic Crystals, 2025, 54(8): 1463-1469.
| Parameter | Value | Parameter | Value |
|---|---|---|---|
| Empirical formula | C40H28N8O7Pb | Formula weight | 939.90 |
| Temperature/K | 273(2) | Crystal system | Triclinic |
| Space group | $P \overline{1}$ | a/nm | 1.162 15(2) |
| b/nm | 1.197 45(2) | c/nm | 1.504 68(2) |
| α/(°) | 109.007 0(10) | β/(°) | 90.487 0(10) |
| γ/(°) | 115.910 0(10) | V/nm3 | 1.752 54(5) |
| Z | 2 | Dc/(g·cm-3) | 1.781 |
| µ/mm-1 | 4.880 | θ/(°) | 2.020~24.999 |
| Unique reflns,Rint | 6 168[R(int)=0.046 9] | GOF | 1.032 |
| R1, wR2 [I > 2σ(I)] | R1=0.032 7, wR2=0.081 1 | R1, wR2(all data) | R1=0.034 6, wR2=0.081 9 |
Table 1 Crystallographic data and structure refinement parameters of 1
| Parameter | Value | Parameter | Value |
|---|---|---|---|
| Empirical formula | C40H28N8O7Pb | Formula weight | 939.90 |
| Temperature/K | 273(2) | Crystal system | Triclinic |
| Space group | $P \overline{1}$ | a/nm | 1.162 15(2) |
| b/nm | 1.197 45(2) | c/nm | 1.504 68(2) |
| α/(°) | 109.007 0(10) | β/(°) | 90.487 0(10) |
| γ/(°) | 115.910 0(10) | V/nm3 | 1.752 54(5) |
| Z | 2 | Dc/(g·cm-3) | 1.781 |
| µ/mm-1 | 4.880 | θ/(°) | 2.020~24.999 |
| Unique reflns,Rint | 6 168[R(int)=0.046 9] | GOF | 1.032 |
| R1, wR2 [I > 2σ(I)] | R1=0.032 7, wR2=0.081 1 | R1, wR2(all data) | R1=0.034 6, wR2=0.081 9 |
| Bond | Length/nm | Bond | Length/nm | Bond | Length/nm |
|---|---|---|---|---|---|
| Pb(1)—O(1W) | 0.229 1(3) | Pb(1)—O(2) | 0.257 6(3) | Pb(1)—O(4) | 0.282 1(7) |
| Pb(1)—O(5)#1 | 0.240 3(3) | Pb(1)—N(5)#2 | 0.253 2(4) | Pb(1)—N(1) | 0.271 9(4) |
| Bond | Angle/(°) | Bond | Angle/(°) | Bond | Angle/(°) |
| O(1W)—Pb(1)—O(5)#1 | 75.19(12) | N(5)#2—Pb(1)—O(2) | 82.95(12) | O(1W)—Pb(1)—N(1) | 77.85(12) |
| O(1W)—Pb(1)—N(5)#2 | 78.46(13) | N(5)#2—Pb(1)—N(1) | 155.12(13) | O(1W)—Pb(1)—O(2) | 71.21(12) |
| O(5)#1—Pb(1)—N(5)#2 | 89.77(12) | O(5)#1—Pb(1)—O(2) | 146.40(11) | O(2)—Pb(1)—N(1) | 96.47(12) |
| O(5)#1—Pb(1)—N(1) | 76.94(12) | O(4)#1—Pb(1)—N(5)#2 | 79.22(13) | O(4)#1—Pb(1)—N(1) | 106.36(13) |
| O(4)#1—Pb(1)—O(1W) | 119.98(99) | O(4)#1—Pb(1)—O(5)#1 | 45.60(12) | O(4)#1—Pb(1)—O(2) | 156.16(10) |
Table 2 Selected bond lengths and angles of 1
| Bond | Length/nm | Bond | Length/nm | Bond | Length/nm |
|---|---|---|---|---|---|
| Pb(1)—O(1W) | 0.229 1(3) | Pb(1)—O(2) | 0.257 6(3) | Pb(1)—O(4) | 0.282 1(7) |
| Pb(1)—O(5)#1 | 0.240 3(3) | Pb(1)—N(5)#2 | 0.253 2(4) | Pb(1)—N(1) | 0.271 9(4) |
| Bond | Angle/(°) | Bond | Angle/(°) | Bond | Angle/(°) |
| O(1W)—Pb(1)—O(5)#1 | 75.19(12) | N(5)#2—Pb(1)—O(2) | 82.95(12) | O(1W)—Pb(1)—N(1) | 77.85(12) |
| O(1W)—Pb(1)—N(5)#2 | 78.46(13) | N(5)#2—Pb(1)—N(1) | 155.12(13) | O(1W)—Pb(1)—O(2) | 71.21(12) |
| O(5)#1—Pb(1)—N(5)#2 | 89.77(12) | O(5)#1—Pb(1)—O(2) | 146.40(11) | O(2)—Pb(1)—N(1) | 96.47(12) |
| O(5)#1—Pb(1)—N(1) | 76.94(12) | O(4)#1—Pb(1)—N(5)#2 | 79.22(13) | O(4)#1—Pb(1)—N(1) | 106.36(13) |
| O(4)#1—Pb(1)—O(1W) | 119.98(99) | O(4)#1—Pb(1)—O(5)#1 | 45.60(12) | O(4)#1—Pb(1)—O(2) | 156.16(10) |
Fig.1 Structure of 1. (a) Coordination environment of Pb(II) ion; (b) geometry of the Pb(II) ions; (c) 1D chain structure; (d) 3D supramolecular structure (symmetry codes: #1 -x-1,-y-1, -z+1;#2 -x+1, -y+2, -z+2)
Fig.4 Fluorescence-sensing properties of 1. (a) Fluorescence spectra in different solvents; (b) fluorescence intensity bar plots at 550 nm; (c) fluorescence spectra in nitroaromatic compound solutions; (d) fluorescence titration plots towards p-NA; (e) fitting curve of p-NA fluorescence titration; (f) fluorescence intensity plot of 5 cycles of p-NA experiments in CH2Cl2 solution
Fig.5 Fluorescence-quenching mechanism of 1. (a) PXRD patterns before and after immersion in solution of p-NA; (b) excitation and emission spectra and UV-visible absorption spectra of p-NA
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