Chem. J. Chinese Universities ›› 2017, Vol. 38 ›› Issue (7): 1125.doi: 10.7503/cjcu20160958
• Articles: Inorganic Chemistry • Previous Articles Next Articles
WANG Qiushuang, ZHENG Xiaoli, QU Xianglong, LI Rui, LI Xia*()
Received:
2016-12-29
Online:
2017-07-10
Published:
2017-05-02
Contact:
LI Xia
E-mail:xiali@cnu.edu.cn
Supported by:
TrendMD:
WANG Qiushuang, ZHENG Xiaoli, QU Xianglong, LI Rui, LI Xia. Synthesis, Structure and Luminescence Property of Transition Metal Complexes with 1,3-Di(4-pyridyl)-propane and 1,2-Benzenedicarboxylic Acid†[J]. Chem. J. Chinese Universities, 2017, 38(7): 1125.
Complex | 1 | 2 | 3 |
---|---|---|---|
Empirical formula | C42H40N4O10Co2 | C42H40N4O10Ni2 | C21H20N2O5Cd |
Formula weight | 878.64 | 878.20 | 492.79 |
Temperature/K | 120(2) | 120(2) | 120(2) |
Crystal system | Monoclinic | Monoclinic | Monoclinic |
Space group | P21 | P21 | P21/c |
a/nm | 1.16755(2) | 1.1609(3) | 1.04635(8) |
b/nm | 1.4003(2) | 1.3986(3) | 1.01448(8) |
c/nm | 1.18421(2) | 1.1847(3) | 1.87662(1) |
β/(°) | 96.298(2) | 96.632(3) | 109.661(3) |
V/nm3 | 1.9244(5) | 1.9107(7) | 1.8759(2) |
Z | 2 | 2 | 4 |
Dc/(g·cm-3) | 1.516 | 1.526 | 1.745 |
Absorption coefficient/mm-1 | 0.928 | 1.052 | 1.202 |
F(000) | 908 | 912 | 992 |
Crystal size/mm | 0.38×0.34×0.30 | 0.42×0.15×0.10 | 0.15×0.10×0.07 |
θ range for data collection/(°) | 1.730—25.249 | 2.26—25.25 | 2.07—27.63 |
Limiting indices | -14≤h≤10, -16≤k≤16, | -13≤h≤13, -16≤k≤8, | -13≤h≤12, -13≤k≤13, |
-12≤l≤14 | -14≤l≤13 | -24≤l≤20 | |
Reflections collected | 9762 | 9035 | 10882 |
Rint | 0.0220 | 0.0322 | 0.0311 |
Data/restraints/parameters | 6637/7/535 | 4556/31/554 | 4307/39/280 |
Goodness-of-fit on F2 | 1.028 | 1.062 | 1.025 |
Final R indices[I>2σ(I)] | R1=0.0373, wR2=0.0887 | R1=0.0501, wR2= 0.1463 | R1=0.0284, wR2= 0.0604 |
R indices(all data) | R1=0.0405, wR2=0.0907 | R1=0.0525, wR2=0.1478 | R1=0.0358, wR2= 0.0636 |
CCDC No. | 1522654 | 1522656 | 1522655 |
Table 1 Crystallographic data of complexes 1—3
Complex | 1 | 2 | 3 |
---|---|---|---|
Empirical formula | C42H40N4O10Co2 | C42H40N4O10Ni2 | C21H20N2O5Cd |
Formula weight | 878.64 | 878.20 | 492.79 |
Temperature/K | 120(2) | 120(2) | 120(2) |
Crystal system | Monoclinic | Monoclinic | Monoclinic |
Space group | P21 | P21 | P21/c |
a/nm | 1.16755(2) | 1.1609(3) | 1.04635(8) |
b/nm | 1.4003(2) | 1.3986(3) | 1.01448(8) |
c/nm | 1.18421(2) | 1.1847(3) | 1.87662(1) |
β/(°) | 96.298(2) | 96.632(3) | 109.661(3) |
V/nm3 | 1.9244(5) | 1.9107(7) | 1.8759(2) |
Z | 2 | 2 | 4 |
Dc/(g·cm-3) | 1.516 | 1.526 | 1.745 |
Absorption coefficient/mm-1 | 0.928 | 1.052 | 1.202 |
F(000) | 908 | 912 | 992 |
Crystal size/mm | 0.38×0.34×0.30 | 0.42×0.15×0.10 | 0.15×0.10×0.07 |
θ range for data collection/(°) | 1.730—25.249 | 2.26—25.25 | 2.07—27.63 |
Limiting indices | -14≤h≤10, -16≤k≤16, | -13≤h≤13, -16≤k≤8, | -13≤h≤12, -13≤k≤13, |
-12≤l≤14 | -14≤l≤13 | -24≤l≤20 | |
Reflections collected | 9762 | 9035 | 10882 |
Rint | 0.0220 | 0.0322 | 0.0311 |
Data/restraints/parameters | 6637/7/535 | 4556/31/554 | 4307/39/280 |
Goodness-of-fit on F2 | 1.028 | 1.062 | 1.025 |
Final R indices[I>2σ(I)] | R1=0.0373, wR2=0.0887 | R1=0.0501, wR2= 0.1463 | R1=0.0284, wR2= 0.0604 |
R indices(all data) | R1=0.0405, wR2=0.0907 | R1=0.0525, wR2=0.1478 | R1=0.0358, wR2= 0.0636 |
CCDC No. | 1522654 | 1522656 | 1522655 |
Co1—O6 | 0.2020(4) | Co1—O1 | 0.2153(4) | Co2—O8 | 0.2102(4) |
---|---|---|---|---|---|
Co1—N2A | 0.2105(5) | Co1—O2 | 0.2212(4) | Co2—N3 | 0.2112(5) |
Co1—N1 | 0.2110(5) | Co2—O4B | 0.1987(4) | Co2—O10 | 0.2185(4) |
Co1—O5 | 0.2152(4) | Co2—N4C | 0.2095(5) | Co2—O9 | 0.2237(4) |
O6—Co1—N2A | 100.21(18) | O6—Co1—O2 | 94.71(16) | O8—Co2—N3 | 94.64(16) |
O6—Co1—N1 | 92.04(17) | N2A—Co1—O2 | 164.30(16) | O4B—Co2—O10 | 89.72(16) |
N2A—Co1—N1 | 92.14(18) | N1—Co1—O2 | 92.18(17) | N4C—Co2—O10 | 84.56(17) |
O6—Co1—O5 | 90.58(16) | O5—Co1—O2 | 89.73(16) | O8—Co2—O10 | 85.50(15) |
N2A—Co1—O5 | 85.30(17) | O1—Co1—O2 | 60.59(14) | N3—Co2—O10 | 179.62(18) |
N1—Co1—O5 | 176.63(18) | O4B—Co2—N4C | 100.76(18) | O4B—Co2—O9 | 97.62(15) |
O6—Co1—O1 | 154.37(16) | O4B—Co2—O8 | 158.35(16) | N4C—Co2—O9 | 159.14(16) |
N2A—Co1—O1 | 103.95(17) | N4C—Co2—O8 | 99.79(17) | O8—Co2—O9 | 61.00(14) |
N1—Co1—O1 | 95.45(17) | O4B—Co2—N3 | 90.28(17) | N3—Co2—O9 | 94.61(16) |
O5—Co1—O1 | 83.07(15) | N4C—Co2—N3 | 95.07(18) | O10—Co2—O9 | 85.76(15) |
Table 2 Selected bond lengths(nm) and bond angles(°) for complex 1*
Co1—O6 | 0.2020(4) | Co1—O1 | 0.2153(4) | Co2—O8 | 0.2102(4) |
---|---|---|---|---|---|
Co1—N2A | 0.2105(5) | Co1—O2 | 0.2212(4) | Co2—N3 | 0.2112(5) |
Co1—N1 | 0.2110(5) | Co2—O4B | 0.1987(4) | Co2—O10 | 0.2185(4) |
Co1—O5 | 0.2152(4) | Co2—N4C | 0.2095(5) | Co2—O9 | 0.2237(4) |
O6—Co1—N2A | 100.21(18) | O6—Co1—O2 | 94.71(16) | O8—Co2—N3 | 94.64(16) |
O6—Co1—N1 | 92.04(17) | N2A—Co1—O2 | 164.30(16) | O4B—Co2—O10 | 89.72(16) |
N2A—Co1—N1 | 92.14(18) | N1—Co1—O2 | 92.18(17) | N4C—Co2—O10 | 84.56(17) |
O6—Co1—O5 | 90.58(16) | O5—Co1—O2 | 89.73(16) | O8—Co2—O10 | 85.50(15) |
N2A—Co1—O5 | 85.30(17) | O1—Co1—O2 | 60.59(14) | N3—Co2—O10 | 179.62(18) |
N1—Co1—O5 | 176.63(18) | O4B—Co2—N4C | 100.76(18) | O4B—Co2—O9 | 97.62(15) |
O6—Co1—O1 | 154.37(16) | O4B—Co2—O8 | 158.35(16) | N4C—Co2—O9 | 159.14(16) |
N2A—Co1—O1 | 103.95(17) | N4C—Co2—O8 | 99.79(17) | O8—Co2—O9 | 61.00(14) |
N1—Co1—O1 | 95.45(17) | O4B—Co2—N3 | 90.28(17) | N3—Co2—O9 | 94.61(16) |
O5—Co1—O1 | 83.07(15) | N4C—Co2—N3 | 95.07(18) | O10—Co2—O9 | 85.76(15) |
Ni1—O6 | 0.2009(6) | Ni1—O1 | 0.2128(5) | Ni2—N3 | 0.2075(6) |
---|---|---|---|---|---|
Ni1—N2A | 0.2053(7) | Ni1—O2 | 0.2145(5) | Ni2—O8 | 0.2080(5) |
Ni1—N1 | 0.2066(6) | Ni2—O4B | 0.1985(5) | Ni2—O10 | 0.2117(5) |
Ni1—O5 | 0.2108(6) | Ni2—N4C | 0.2048(7) | Ni2—O9 | 0.2178(5) |
O6—Ni1—N2A | 98.3(2) | O6—Ni1—O2 | 96.6(2) | N3—Ni2—O8 | 93.5(2) |
O6—Ni1—N1 | 91.6(2) | N2A—Ni1—O2 | 164.2(2) | O4B—Ni2—O10 | 89.8(2) |
N2A—Ni1—N1 | 91.5(3) | N1—Ni1—O2 | 93.2(2) | N4C—Ni2—O10 | 85.0(2) |
O6—Ni1—O5 | 90.5(2) | O5—Ni1—O2 | 88.8(2) | N3—Ni2—O10 | 179.6(3) |
N2A—Ni1—O5 | 85.9(2) | O1—Ni1—O2 | 62.2(2) | O8—Ni2—O10 | 86.6(2) |
N1—Ni1—O5 | 176.9(3) | O4B—Ni2—N4C | 97.6(2) | O4B—Ni2—O9 | 100.1(2) |
O6—Ni1—O1 | 158.1(2) | O4B—Ni2—N3 | 90.3(2) | N4C—Ni2—O9 | 160.3(2) |
N2A—Ni1—O1 | 102.4(2) | N4C—Ni2—N3 | 94.6(3) | N3—Ni2—O9 | 94.0(2) |
N1—Ni1—O1 | 94.8(2) | O4B—Ni2—O8 | 162.1(2) | O8—Ni2—O9 | 62.2(2) |
O5—Ni1—O1 | 84.0(2) | N4C—Ni2—O8 | 99.5(2) | O10—Ni2—O9 | 86.4(2) |
Table 3 Selected bond lengths(nm) and bond angles(°) for complex 2*
Ni1—O6 | 0.2009(6) | Ni1—O1 | 0.2128(5) | Ni2—N3 | 0.2075(6) |
---|---|---|---|---|---|
Ni1—N2A | 0.2053(7) | Ni1—O2 | 0.2145(5) | Ni2—O8 | 0.2080(5) |
Ni1—N1 | 0.2066(6) | Ni2—O4B | 0.1985(5) | Ni2—O10 | 0.2117(5) |
Ni1—O5 | 0.2108(6) | Ni2—N4C | 0.2048(7) | Ni2—O9 | 0.2178(5) |
O6—Ni1—N2A | 98.3(2) | O6—Ni1—O2 | 96.6(2) | N3—Ni2—O8 | 93.5(2) |
O6—Ni1—N1 | 91.6(2) | N2A—Ni1—O2 | 164.2(2) | O4B—Ni2—O10 | 89.8(2) |
N2A—Ni1—N1 | 91.5(3) | N1—Ni1—O2 | 93.2(2) | N4C—Ni2—O10 | 85.0(2) |
O6—Ni1—O5 | 90.5(2) | O5—Ni1—O2 | 88.8(2) | N3—Ni2—O10 | 179.6(3) |
N2A—Ni1—O5 | 85.9(2) | O1—Ni1—O2 | 62.2(2) | O8—Ni2—O10 | 86.6(2) |
N1—Ni1—O5 | 176.9(3) | O4B—Ni2—N4C | 97.6(2) | O4B—Ni2—O9 | 100.1(2) |
O6—Ni1—O1 | 158.1(2) | O4B—Ni2—N3 | 90.3(2) | N4C—Ni2—O9 | 160.3(2) |
N2A—Ni1—O1 | 102.4(2) | N4C—Ni2—N3 | 94.6(3) | N3—Ni2—O9 | 94.0(2) |
N1—Ni1—O1 | 94.8(2) | O4B—Ni2—O8 | 162.1(2) | O8—Ni2—O9 | 62.2(2) |
O5—Ni1—O1 | 84.0(2) | N4C—Ni2—O8 | 99.5(2) | O10—Ni2—O9 | 86.4(2) |
Cd1—N1 | 0.2331(2) | Cd1—O3 | 0.2352(7) | Cd1—O5 | 0.2448(2) |
---|---|---|---|---|---|
Cd1—N2A | 0.2351(2) | Cd1—O1B | 0.2421(2) | Cd1—O4 | 0.2467(1) |
Cd1—O2B | 0.2352(4) | ||||
N1—Cd1—N2A | 161.86(7) | N2A—Cd1—O1B | 85.12(7) | O1B—Cd1—O5 | 95.46(6) |
N1—Cd1—O2B | 95.12(7) | O2B—Cd1—O1B | 54.97(6) | N1—Cd1—O4 | 87.61(7) |
N2A—Cd1—O2B | 97.82(6) | O3—Cd1—O1B | 139.52(6) | N2A—Cd1—O4 | 90.69(7) |
N1—Cd1—O3 | 101.52(7) | N1—Cd1—O5 | 82.41(7) | O2B—Cd1—O4 | 139.69(6) |
N2A—Cd1—O3 | 92.11(7) | N2A—Cd1—O5 | 80.05(7) | O3—Cd1—O4 | 54.56(6) |
O2B—Cd1—O3 | 85.67(6) | O2B—Cd1—O5 | 150.34(6) | O1B—Cd1—O4 | 165.32(6) |
N1—Cd1—O1B | 92.00(7) | O3—Cd1—O5 | 123.87(6) | O5—Cd1—O4 | 69.93(6) |
Table 4 Selected bond lengths(nm) and bond angles(°) for complex 3*
Cd1—N1 | 0.2331(2) | Cd1—O3 | 0.2352(7) | Cd1—O5 | 0.2448(2) |
---|---|---|---|---|---|
Cd1—N2A | 0.2351(2) | Cd1—O1B | 0.2421(2) | Cd1—O4 | 0.2467(1) |
Cd1—O2B | 0.2352(4) | ||||
N1—Cd1—N2A | 161.86(7) | N2A—Cd1—O1B | 85.12(7) | O1B—Cd1—O5 | 95.46(6) |
N1—Cd1—O2B | 95.12(7) | O2B—Cd1—O1B | 54.97(6) | N1—Cd1—O4 | 87.61(7) |
N2A—Cd1—O2B | 97.82(6) | O3—Cd1—O1B | 139.52(6) | N2A—Cd1—O4 | 90.69(7) |
N1—Cd1—O3 | 101.52(7) | N1—Cd1—O5 | 82.41(7) | O2B—Cd1—O4 | 139.69(6) |
N2A—Cd1—O3 | 92.11(7) | N2A—Cd1—O5 | 80.05(7) | O3—Cd1—O4 | 54.56(6) |
O2B—Cd1—O3 | 85.67(6) | O2B—Cd1—O5 | 150.34(6) | O1B—Cd1—O4 | 165.32(6) |
N1—Cd1—O1B | 92.00(7) | O3—Cd1—O5 | 123.87(6) | O5—Cd1—O4 | 69.93(6) |
Fig.1 Asymmetric unit(A), coordination environment of Co(Ⅱ)(B), Co1-(1,2-bdc)-Co2 helix chain(C), Co2-(bpp)-Co2 chain(D), three-dimensional structure(E) and topological structure(F) of complex 1All hydrogen atoms in (A)—(E) are omitted; symmetry codes: A. x, y, z+1; B. -x, y-1/2, -z+2; C. x-1, y, z.
Fig.2 Asymmetric unit(A), coordination environment of Cd(Ⅱ)(B), two-dimensional network(C), three-dimensional structure by hydrogen bonds(D) and L-, R-helical chains(E) of complex 3All hydrogen atoms in (A)—(E) are omitted; symmetry codes: A. x+1, y-1, z; B. -x+2, y+1/2, -z+1/2; C. x, 1/2-y, -1/2+z.
Fig.4 Emission spectra(A) and peak intensity at 408 nm(B) of complex 3 in different solvents Solvent: a. DMF; b. ethyl acetate; c. DMSO; d. dichloromethane; e. benzene; f. methanol; g. etanol; h. acetonitrile; i. hexane; j. formaldehyde; k. acetone; l. isopropanol; m. triethylamine; n. water; o. xylene; p. tetrahydrofuran; q. aniline.
Fig.5 Emission spectra of complex 3 dispersed in ethanol solvent containing aniline with different concentrations(λex=314 nm)c(Aniline)/(mol·L-1): a. 0; b. 10-6; c. 10-5; d. 10-4. Inset shows peak intensity at 408 nm.
Fig.6 Emission spectra of complex 3 dispersed in ethanol solvent containing tetrahydrofuran with different concentrations(λex=314 nm)c(THF)/(mol·L-1): a. 0; b. 10-6; c. 10-5; d. 10-4; e. 10-3; f. 10-2; g. 10-1. Inset shows peak intensity at 345 nm.
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