Chem. J. Chinese Universities ›› 2018, Vol. 39 ›› Issue (12): 2611.doi: 10.7503/cjcu20180009
• Inorganic Chemistry • Previous Articles Next Articles
ZHANG Dechun1,2, XU Qiwei2, LI Xia2,*()
Received:
2018-01-03
Online:
2018-09-10
Published:
2018-09-10
Contact:
LI Xia
E-mail:xiali@cnu.edu.cn
Supported by:
CLC Number:
TrendMD:
ZHANG Dechun,XU Qiwei,LI Xia. Lanthanide Complexes Constructed by 2,2'-Oxybis(benzoic acid) and 1H-Imidazo[4,5-f][1,10]-phenanthroline: Fluorescence and Fluorescent Sensing for NH3†[J]. Chem. J. Chinese Universities, 2018, 39(12): 2611.
Complex | 1 | 2 | 3 | 4 | 5 |
---|---|---|---|---|---|
Empirical formula | C110H70N8O30Eu2 | C110H70N8O30Tb2 | C55H32N4O15Eu2 | C55H32N4O15Tb2 | C66H38N6O16Eu2 |
Formula weight | 2287.66 | 2301.58 | 1292.77 | 1306.69 | 1474.94 |
Crystal system | Triclinic | Triclinic | Triclinic | Triclinic | Monoclinic, |
Space group | P | P | P | P | C2/c |
a/nm | 1.15131(5) | 1.14885(5) | 1.31535(12) | 1.28091(10) | 2.84806(10) |
b/nm | 1.38342(6) | 1.38288(6) | 1.39415(13) | 1.42179(11) | 1.40143(5) |
c/nm | 1.70498(8) | 1.70231(8) | 1.45396(13) | 1.49624(11) | 2.97567(10) |
α/(°) | 113.4990(10) | 113.4240(10) | 73.313(2) | 74.132(2) | 90 |
β/(°) | 93.4370(10) | 93.4800(10) | 72.018(3) | 67.660(2) | 108.9160(10) |
γ/(°) | 93.1820(10) | 92.9840(10) | 84.328(3) | 81.947(2) | 90 |
V/nm3 | 2.47653(19) | 2.46845(19) | 2.4291(4) | 2.4224(3) | 11.2355(7) |
Z | 1 | 1 | 2 | 2 | 8 |
Dc/(Mg·m-3) | 1.534 | 1.548 | 1.767 | 1.791 | 1.744 |
μ/mm-1 | 1.342 | 1.509 | 2.636 | 2.974 | 2.294 |
F(000) | 1152 | 1156 | 1272 | 1280 | 5840 |
Crystal size/mm3 | 0.234×0.139× 0.132 | 0.211×0.107× 0.067 | 0.391×0.232× 0.063 | 0.227×0.126× 0.101 | 0.300×0.204× 0.152 |
θ Range for data collection/(°) | 2.95—25.01 | 2.95—25.01 | 2.97—25.01 | 2.90—25.01 | 2.91—27.55 |
Limiting indices | -13≤h≤13, -16≤k≤16, -20≤l≤20 | -13≤h≤13, -16≤k≤16, -20≤l≤20 | -15≤h≤15, -16≤k≤16, -17≤l≤17 | -15≤h≤15, -16≤k≤16, -17≤l≤17 | -36≤h≤36, -17≤k≤18, -38≤l≤38 |
Reflections collected/unique | 44087/8720 [R(int)=0.0650] | 43696/8696 [R(int)=0.0822] | 40881/8573 [R(int)=0.0930] | 39331/8520 [R(int)=0.1195] | 85920/12923 [R(int)=0.0974] |
Data/restraints/parameters | 8720/108/718 | 8696/127/675 | 8573/0/685 | 8520/0/685 | 12923/0/812 |
Largest difference peak and hole/(e·nm-3) | 1356 and -883 | 1353 and -779 | 1416 and -1360 | 1527 and -1000 | 1568 and -883 |
Goodness-of-fit on F2 | 1.045 | 1.082 | 1.066 | 1.069 | 1.043 |
Final R indices[I>2σ(I)] | R1=0.0447, wR2=0.1190 | R1=0.0522, wR2=0.1210 | R1=0.0370, wR2=0.0906 | R1=0.0462, wR2=0.0996 | R1=0.0415, wR2=0.0996 |
R indices(all data) | R1=0.0571, wR2=0.1321 | R1=0.0780, wR2=0.1385 | R1=0.0504, wR2=0.1073 | R1=0.0794, wR2=0.1178 | R1=0.0585, wR2=0.1066 |
CCDC No. | 1587904 | 1587905 | 1587906 | 1587909 | 1587910 |
Table 1 Crystal data and structural refinement for complexes 1—5
Complex | 1 | 2 | 3 | 4 | 5 |
---|---|---|---|---|---|
Empirical formula | C110H70N8O30Eu2 | C110H70N8O30Tb2 | C55H32N4O15Eu2 | C55H32N4O15Tb2 | C66H38N6O16Eu2 |
Formula weight | 2287.66 | 2301.58 | 1292.77 | 1306.69 | 1474.94 |
Crystal system | Triclinic | Triclinic | Triclinic | Triclinic | Monoclinic, |
Space group | P | P | P | P | C2/c |
a/nm | 1.15131(5) | 1.14885(5) | 1.31535(12) | 1.28091(10) | 2.84806(10) |
b/nm | 1.38342(6) | 1.38288(6) | 1.39415(13) | 1.42179(11) | 1.40143(5) |
c/nm | 1.70498(8) | 1.70231(8) | 1.45396(13) | 1.49624(11) | 2.97567(10) |
α/(°) | 113.4990(10) | 113.4240(10) | 73.313(2) | 74.132(2) | 90 |
β/(°) | 93.4370(10) | 93.4800(10) | 72.018(3) | 67.660(2) | 108.9160(10) |
γ/(°) | 93.1820(10) | 92.9840(10) | 84.328(3) | 81.947(2) | 90 |
V/nm3 | 2.47653(19) | 2.46845(19) | 2.4291(4) | 2.4224(3) | 11.2355(7) |
Z | 1 | 1 | 2 | 2 | 8 |
Dc/(Mg·m-3) | 1.534 | 1.548 | 1.767 | 1.791 | 1.744 |
μ/mm-1 | 1.342 | 1.509 | 2.636 | 2.974 | 2.294 |
F(000) | 1152 | 1156 | 1272 | 1280 | 5840 |
Crystal size/mm3 | 0.234×0.139× 0.132 | 0.211×0.107× 0.067 | 0.391×0.232× 0.063 | 0.227×0.126× 0.101 | 0.300×0.204× 0.152 |
θ Range for data collection/(°) | 2.95—25.01 | 2.95—25.01 | 2.97—25.01 | 2.90—25.01 | 2.91—27.55 |
Limiting indices | -13≤h≤13, -16≤k≤16, -20≤l≤20 | -13≤h≤13, -16≤k≤16, -20≤l≤20 | -15≤h≤15, -16≤k≤16, -17≤l≤17 | -15≤h≤15, -16≤k≤16, -17≤l≤17 | -36≤h≤36, -17≤k≤18, -38≤l≤38 |
Reflections collected/unique | 44087/8720 [R(int)=0.0650] | 43696/8696 [R(int)=0.0822] | 40881/8573 [R(int)=0.0930] | 39331/8520 [R(int)=0.1195] | 85920/12923 [R(int)=0.0974] |
Data/restraints/parameters | 8720/108/718 | 8696/127/675 | 8573/0/685 | 8520/0/685 | 12923/0/812 |
Largest difference peak and hole/(e·nm-3) | 1356 and -883 | 1353 and -779 | 1416 and -1360 | 1527 and -1000 | 1568 and -883 |
Goodness-of-fit on F2 | 1.045 | 1.082 | 1.066 | 1.069 | 1.043 |
Final R indices[I>2σ(I)] | R1=0.0447, wR2=0.1190 | R1=0.0522, wR2=0.1210 | R1=0.0370, wR2=0.0906 | R1=0.0462, wR2=0.0996 | R1=0.0415, wR2=0.0996 |
R indices(all data) | R1=0.0571, wR2=0.1321 | R1=0.0780, wR2=0.1385 | R1=0.0504, wR2=0.1073 | R1=0.0794, wR2=0.1178 | R1=0.0585, wR2=0.1066 |
CCDC No. | 1587904 | 1587905 | 1587906 | 1587909 | 1587910 |
Fig.6 Fluorescence intensity(5D0→7F2 or 5D4→7F5) changes(A) and the quenching rate(B) of complexes 1—5 upon addition of NH3 at room temperaturec(NH3)=10 mmol/L, m(complex)=10 mg, V(NH3)=10 mL. (A) a. complex 1; b. complex 1+NH3; c. complex 2; d. complex 2+NH3; e. complex 3; f. compound 3+NH3; g. complex 4; h. complex 4+NH3; i. complex 5; j. complex 5+NH3.
Fig.7 Fluorescence spectra changes of complex 1 upon addition of NH3 and mental ions at room temperaturec(NH3)=c(metal ion)=5 mmol/L, V=10 mL, m(complex 1)=10 mg. λex=368 nm, λem=618 nm.
Fig.8 Effect of NH3 on the fluorescence spectra of complex 1(A), histogram of fluorescence intensity and NH3 concentration(B)c(NH3)=0, 0.1, 0.5, 1.0, 5.0, 10, 50 mmol/L(a—g), V(NH3)=10 mL, m(complex 1)=10 mg, T=25 ℃, λex=368 nm, λem=618 nm.
Fig.10 Emission spectra of complex 1-NH3 in the presence of different metal ionsc(NH3)=c(metal ion)=5 mmol/L, V=10 mL, m(complex 1)=10 mg, T=25 ℃, λex=368 nm, λem=618 nm.
Fig.11 Effect of Zn2+ on the fluorescence spectra of complex 1-NH3c(Zn2+)=0—50 mmol/L, c(NH3)=20 mmol/L, V(Zn2+)=10 mL, m(complex 1)=10 mg, T=25 ℃, λex=368 nm, λem=618 nm.
Fig.12 Effect of Al3+ on the fluorescence spectra of complex 1-NH3 c(Al3+)=0—50 mmol/L, c(NH3)=5 mmol/L, V=10 mL, m(complex 1)=10 mg, T=25 ℃, λex=368 nm, λem=618 nm.
Fig.13 Effect of Cr3+ on the fluorescence spectra of complex 1-NH3c(Cr3+)=0—50 mmol/L, c(NH3)=5 mmol/L, V=10 mL, m(complex 1)=10 mg, T=25 ℃, λex=368 nm, λem=618 nm.
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