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2017 Volume 33 Issue 9
2017, 33(9): 1505-1509
doi: 10.11862/CJIC.2017.204
Abstract:
Er3+-Yb3+ co-doped transparent oxyfluoride glass ceramics containing SrF2 crystals were successfully synthesized using a high temperature melting quenching method. The structure, morphology and luminescent properties of the samples were measured and characterized by DSC, XRD, SEM and fluorescence spectra. The results show that the optimum heat treatment temperature is 620℃, and the optimum heat treatment tine is 2 h. The effect of Er3+-Yb3+ co-doped glass ceramics with different doping concentrations of Yb3+ on the up-conversion luminescence properties was discussed. The optimum doping concentration ratio of Er3+-Yb3+ is 1:7. Bright green light (522, 540 nm) and weak red light (656 nm) were observed in the luminescence spectra. The energy transfer process between Er3+ and Yb3+ was discussed.
Er3+-Yb3+ co-doped transparent oxyfluoride glass ceramics containing SrF2 crystals were successfully synthesized using a high temperature melting quenching method. The structure, morphology and luminescent properties of the samples were measured and characterized by DSC, XRD, SEM and fluorescence spectra. The results show that the optimum heat treatment temperature is 620℃, and the optimum heat treatment tine is 2 h. The effect of Er3+-Yb3+ co-doped glass ceramics with different doping concentrations of Yb3+ on the up-conversion luminescence properties was discussed. The optimum doping concentration ratio of Er3+-Yb3+ is 1:7. Bright green light (522, 540 nm) and weak red light (656 nm) were observed in the luminescence spectra. The energy transfer process between Er3+ and Yb3+ was discussed.
2017, 33(9): 1521-1526
doi: 10.11862/CJIC.2017.201
Abstract:
A simple but useful hydrothermal method is developed to prepare molybdenum disulfide (MoS2) flower-like spheres by sodium molybdate dehydrate (Na2MoO4·2H2O) and thiocarbamide (CS(NH2)2). In this work, the appropriate hydrothermal condition is at 180℃ reaction temperature for 48 h and the atomic ratio of S and Mo is 1:4 in 0.001 mol·L-1 aqueous solution. The morphologies and microstructures of as-prepared MoS2 are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area test method (BET). Results indicate that the average diameter of as-prepared products is about 1 μm with good crystallinity and dispersibility, and their specific surface area is about 87 m2·g-1. In order to character the electrical properties of MoS2, the electrochemical performance was studied by cyclic voltammetry (CV), galvanostatic charge-discharge cycling (GCD) and electrochemical impedance spectroscopy (EIS). Analysis results show that in 3 mol·L-1 KOH electrolyte, the specific capacitance of single electrode is 130.6 F·g-1 at 5 mV·s-1 scan rate and 110.9 F·g-1 at 0.1 A·g-1 current density. The charge-transfer resistance (Rct) is of 0.33 Ω. The loss of specific capacitance is 14.7% after 1 000 cycles. These electric properties illustrate the MoS2 prepared by hydrothermal processing can act as an ideal material for supercapacitor electrode.
A simple but useful hydrothermal method is developed to prepare molybdenum disulfide (MoS2) flower-like spheres by sodium molybdate dehydrate (Na2MoO4·2H2O) and thiocarbamide (CS(NH2)2). In this work, the appropriate hydrothermal condition is at 180℃ reaction temperature for 48 h and the atomic ratio of S and Mo is 1:4 in 0.001 mol·L-1 aqueous solution. The morphologies and microstructures of as-prepared MoS2 are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area test method (BET). Results indicate that the average diameter of as-prepared products is about 1 μm with good crystallinity and dispersibility, and their specific surface area is about 87 m2·g-1. In order to character the electrical properties of MoS2, the electrochemical performance was studied by cyclic voltammetry (CV), galvanostatic charge-discharge cycling (GCD) and electrochemical impedance spectroscopy (EIS). Analysis results show that in 3 mol·L-1 KOH electrolyte, the specific capacitance of single electrode is 130.6 F·g-1 at 5 mV·s-1 scan rate and 110.9 F·g-1 at 0.1 A·g-1 current density. The charge-transfer resistance (Rct) is of 0.33 Ω. The loss of specific capacitance is 14.7% after 1 000 cycles. These electric properties illustrate the MoS2 prepared by hydrothermal processing can act as an ideal material for supercapacitor electrode.
2017, 33(9): 1527-1536
doi: 10.11862/CJIC.2017.211
Abstract:
MoS2/WO3 composite photocatalyst was synthesized by a hydrothermal method. The morphology and structure of samples were respectively characterized by SEM, TEM, XRD, Raman, BET and DRS. Compared with pure WO3 and flaky MoS2/WO3, the results show that spherical MoS2/WO3 photocatalysts possess higher photocatalytic efficiency for RhB. For the spherical MoS2/WO3 composite semiconductor, the effect of MoS2 loading content (0.5%, 1%, 2%, 5%, 10%) on the photocatalytic degradation of RhB was investigated. The results show that the catalytic effect is the best when the content of MoS2 is 2%. At the same time, the effect of pH (pH=1, 3, 7, 11) on the photocatalytic activity was studied. The results show that the degradation rate is the highest at pH=6. When the amount of catalyst is 1 g·L-1, the degradation rate of RhB reaches 96.6% after 30 min. The transient photocurrent of spherical MoS2/WO3 is 0.050 6 mA·cm-2, which is increased by a factor of 2.4 compared with that of WO3. After five cycles of stability test, the spherical MoS2/WO3 composite semiconductor catalyst can maintain a high degradation rate of 90%.
MoS2/WO3 composite photocatalyst was synthesized by a hydrothermal method. The morphology and structure of samples were respectively characterized by SEM, TEM, XRD, Raman, BET and DRS. Compared with pure WO3 and flaky MoS2/WO3, the results show that spherical MoS2/WO3 photocatalysts possess higher photocatalytic efficiency for RhB. For the spherical MoS2/WO3 composite semiconductor, the effect of MoS2 loading content (0.5%, 1%, 2%, 5%, 10%) on the photocatalytic degradation of RhB was investigated. The results show that the catalytic effect is the best when the content of MoS2 is 2%. At the same time, the effect of pH (pH=1, 3, 7, 11) on the photocatalytic activity was studied. The results show that the degradation rate is the highest at pH=6. When the amount of catalyst is 1 g·L-1, the degradation rate of RhB reaches 96.6% after 30 min. The transient photocurrent of spherical MoS2/WO3 is 0.050 6 mA·cm-2, which is increased by a factor of 2.4 compared with that of WO3. After five cycles of stability test, the spherical MoS2/WO3 composite semiconductor catalyst can maintain a high degradation rate of 90%.
2017, 33(9): 1555-1560
doi: 10.11862/CJIC.2017.176
Abstract:
Zirconia nanorods were prepared via molten salt route, using zirconia dry gel powder as precursor synthesized by non-hydrolytic sol-gel (NHSG) method. Differential thermal analysis and thermogravimetric analysis (DTA-TG), X-ray diffraction analysis (XRD), transmission electron microscope (TEM) and field emission scanning electron microscopy (FE-SEM) were employed to characterize the phase transformation process of zirconia, the influences of the type, amount of molten salt and the role of fluoride on the formation of zirconia nanorods. The results show that the optimized molten salt type and dosage are NaVO3 and 1:1(mmolten salt:mxerogel mass ratio), respectively, and the monoclinic zirconia nanorods grow preferentially along the [010] direction in the presence of sodium fluoride. It is found that the F- in the flux plays a vital role in formation of zirconia nanorods:on one hand, the fluoride ions accelerate the mass transfer of Zr4+ ions and the dissolution of zirconia xerogel in molten salt system; on the other hand, fluoride ions adsorb on high-energy facets of the zirconia to block the growth along these facets. The interaction of two aspects promotes the formation of zirconia nanorods in large scale.
Zirconia nanorods were prepared via molten salt route, using zirconia dry gel powder as precursor synthesized by non-hydrolytic sol-gel (NHSG) method. Differential thermal analysis and thermogravimetric analysis (DTA-TG), X-ray diffraction analysis (XRD), transmission electron microscope (TEM) and field emission scanning electron microscopy (FE-SEM) were employed to characterize the phase transformation process of zirconia, the influences of the type, amount of molten salt and the role of fluoride on the formation of zirconia nanorods. The results show that the optimized molten salt type and dosage are NaVO3 and 1:1(mmolten salt:mxerogel mass ratio), respectively, and the monoclinic zirconia nanorods grow preferentially along the [010] direction in the presence of sodium fluoride. It is found that the F- in the flux plays a vital role in formation of zirconia nanorods:on one hand, the fluoride ions accelerate the mass transfer of Zr4+ ions and the dissolution of zirconia xerogel in molten salt system; on the other hand, fluoride ions adsorb on high-energy facets of the zirconia to block the growth along these facets. The interaction of two aspects promotes the formation of zirconia nanorods in large scale.
2017, 33(9): 1561-1567
doi: 10.11862/CJIC.2017.210
Abstract:
Two lanthanide-organic frameworks[Dy2(MH)6]n·0.5DMF (1) and[Eu2(MH)6]n (2) (MH=maleichydrazide and DMF=N, N-dimethylformamide) have been synthesized and characterized by X-ray single-crystal diffraction and X-ray powder diffraction. Two complexes are both Triclinic P1 space group. Ln(Ⅲ)ions adopt same coordination environments, and seven-coordinated Ln(Ⅲ)atom form feature isostructural 3D structures, topological type:tsi. The luminescence properties of 1 and 2 were investigated. Under the excitation of 375 nm, the emission spectrum of complex 2 shows five peaks at 581, 593, 616, 652 and 705 nm, corresponding to 5D0→7FJ (J=0~4) transitions of Eu3+. The emission spectrum of complex 1 shows a peak at 618 nm, which plausibly arises from π*-π transition of ligands.CCDC: 1473814, 1; 1473816, 2.
Two lanthanide-organic frameworks[Dy2(MH)6]n·0.5DMF (1) and[Eu2(MH)6]n (2) (MH=maleichydrazide and DMF=N, N-dimethylformamide) have been synthesized and characterized by X-ray single-crystal diffraction and X-ray powder diffraction. Two complexes are both Triclinic P1 space group. Ln(Ⅲ)ions adopt same coordination environments, and seven-coordinated Ln(Ⅲ)atom form feature isostructural 3D structures, topological type:tsi. The luminescence properties of 1 and 2 were investigated. Under the excitation of 375 nm, the emission spectrum of complex 2 shows five peaks at 581, 593, 616, 652 and 705 nm, corresponding to 5D0→7FJ (J=0~4) transitions of Eu3+. The emission spectrum of complex 1 shows a peak at 618 nm, which plausibly arises from π*-π transition of ligands.CCDC: 1473814, 1; 1473816, 2.
2017, 33(9): 1568-1572
doi: 10.11862/CJIC.2017.195
Abstract:
A novel organic-inorganic hybrid material containing diammonium cations, (NH3C6H12NH3)CuCl4 with perovskite structure, was synthesized by low-temperature solution method and characterized by elemental analysis, FT-IR, XRD and UV-Vis absorption spectra techniques. The result shows that the UV-visible absorption peak of this material is located at 285 and 387 nm, with a layer spacing of 1.18 nm. The organic layer +NH3C6H12NH3+ and two inorganic frameworks, CuCl42-, are bound together by strong hydrogen bonds, so more orderly arrangement and good heat stability are obtained. The resistance of (NH3C6H12NH3)CuCl4 is about 1.36×105Ω·cm, three orders of magnitude less than hybrid perovskite that contain single ammonium cation, just because there is no weaker van der Waals force between two layers of organic molecules.
A novel organic-inorganic hybrid material containing diammonium cations, (NH3C6H12NH3)CuCl4 with perovskite structure, was synthesized by low-temperature solution method and characterized by elemental analysis, FT-IR, XRD and UV-Vis absorption spectra techniques. The result shows that the UV-visible absorption peak of this material is located at 285 and 387 nm, with a layer spacing of 1.18 nm. The organic layer +NH3C6H12NH3+ and two inorganic frameworks, CuCl42-, are bound together by strong hydrogen bonds, so more orderly arrangement and good heat stability are obtained. The resistance of (NH3C6H12NH3)CuCl4 is about 1.36×105Ω·cm, three orders of magnitude less than hybrid perovskite that contain single ammonium cation, just because there is no weaker van der Waals force between two layers of organic molecules.
2017, 33(9): 1573-1578
doi: 10.11862/CJIC.2017.209
Abstract:
The hydrothermal-coprecipitation method was successfully used to prepare Sn6O4(OH)4 coated on the surface of zinc oxide. The modified ZnO material was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive spectrometer (EDS) analysis. The results show:Sn6O4(OH)4 was coated on the surface of ZnO and the crystallinity was well at pH=12, and the coating composition is including Zn, Sn, O. The electrochemical performances of Sn6O4(OH)4-coated ZnO was investigated by cyclic voltammetry (CV), electro-chemical impedance spectroscopy (EIS) and charge-discharge technology. Compared with pure ZnO, The CV curves and the electrochemical impedance spectroscopy show that Sn6O4(OH)4-coated ZnO can improve the corrosion resistance and increase charge transfer resistance (Rct), Sn6O4(OH)4-coated ZnO electrode has best charge-discharge efficiency when the Sn6O4(OH)4 content is 3%, and the capacity retention ratio of the coated ZnO is about 70% after over 40 cycles with the rate of 0.2C, which is much higher than that of the pure ZnO.
The hydrothermal-coprecipitation method was successfully used to prepare Sn6O4(OH)4 coated on the surface of zinc oxide. The modified ZnO material was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive spectrometer (EDS) analysis. The results show:Sn6O4(OH)4 was coated on the surface of ZnO and the crystallinity was well at pH=12, and the coating composition is including Zn, Sn, O. The electrochemical performances of Sn6O4(OH)4-coated ZnO was investigated by cyclic voltammetry (CV), electro-chemical impedance spectroscopy (EIS) and charge-discharge technology. Compared with pure ZnO, The CV curves and the electrochemical impedance spectroscopy show that Sn6O4(OH)4-coated ZnO can improve the corrosion resistance and increase charge transfer resistance (Rct), Sn6O4(OH)4-coated ZnO electrode has best charge-discharge efficiency when the Sn6O4(OH)4 content is 3%, and the capacity retention ratio of the coated ZnO is about 70% after over 40 cycles with the rate of 0.2C, which is much higher than that of the pure ZnO.
2017, 33(9): 1579-1586
doi: 10.11862/CJIC.2017.179
Abstract:
Properties of Cp4An and COT2An (Cp-=C5H5-, COT2-=C8H82-, An=U(Ⅳ), Pu(Ⅳ)) species both in gas phase and tetrahydrofuran (THF) solution are systematically studied by DFT (density functional theory). The solvent effect of THF is simulated by a conductor-like polarized continuum model (CPCM). Theoretical calculations show that the binding energies of the complexes are in the order of COT2Pu>COT2U>Cp4Pu>Cp4U. Solvent effects decreased binding energies of the structures. The optimized geometry structures and the IR spectra for the complexes in gas and aqueous phase are in accordance to the available experimental data very well. Detail studies on MO energy levels for Cp4An and COT2An with An=U(Ⅳ), Pu(Ⅳ)calculated with rsc ecp indicate that COT2U and CP4U favors triplets fφ2 and fσ2 configuration respectively, meanwhile, COT2Pu and Cp4Pu favor quintets fσ1fπ1fφ1 and fσ3fδ1 configuration respectively.
Properties of Cp4An and COT2An (Cp-=C5H5-, COT2-=C8H82-, An=U(Ⅳ), Pu(Ⅳ)) species both in gas phase and tetrahydrofuran (THF) solution are systematically studied by DFT (density functional theory). The solvent effect of THF is simulated by a conductor-like polarized continuum model (CPCM). Theoretical calculations show that the binding energies of the complexes are in the order of COT2Pu>COT2U>Cp4Pu>Cp4U. Solvent effects decreased binding energies of the structures. The optimized geometry structures and the IR spectra for the complexes in gas and aqueous phase are in accordance to the available experimental data very well. Detail studies on MO energy levels for Cp4An and COT2An with An=U(Ⅳ), Pu(Ⅳ)calculated with rsc ecp indicate that COT2U and CP4U favors triplets fφ2 and fσ2 configuration respectively, meanwhile, COT2Pu and Cp4Pu favor quintets fσ1fπ1fφ1 and fσ3fδ1 configuration respectively.
2017, 33(9): 1595-1602
doi: 10.11862/CJIC.2017.208
Abstract:
The structure-directing effect of dipropylamine isomers, i.e., di-n-propylamine (DPA) and diisopro-pylamine (D-iPA), was investigated. By heating the initial gels with certain composition at 200℃ for 24 h, highly crystalline aluminophosphate molecular sieve AlPO4-11 was obtained. The crystallization processes were investigated using X-ray diffraction, elemental analysis and pH value measurement. For the crystallization process of the initial gel with nAL2O3:nP2O5:nDPA/D-iPA:nH2O=1.0:1.0:1.2:75, no intermediate phase was formed when the DPA was used as the structure-directing agent, whereas intermediate phase of aluminophosphate molecular sieve AlPO4-5 was observed when the D-iPA was used as the structure-directing agent. For the crystallization process of the initial gel with nAL2O3:nP2O5:nDPA/D-iPA:nH2O=1.0:1.0:1.0:75, intermediate phase of aluminophosphate molecular sieve VPI-5 was formed when the DPA was used as the structure-directing agent, whereas intermediate phases of both VPI-5 and AlPO4-5 were observed when the D-iPA was used as the structure-directing agent. Theoretical calculation showed that the charge on the N of the protonated DPA was different with that on the N of the protonated D-iPA. The results indicate that the structure-directing effect of amine can be affected by the composition of the initial gel and the fine-tuning of the structure of amine can influence its structure-directing effect. However, such influence is affected by the composition of the initial gel.
The structure-directing effect of dipropylamine isomers, i.e., di-n-propylamine (DPA) and diisopro-pylamine (D-iPA), was investigated. By heating the initial gels with certain composition at 200℃ for 24 h, highly crystalline aluminophosphate molecular sieve AlPO4-11 was obtained. The crystallization processes were investigated using X-ray diffraction, elemental analysis and pH value measurement. For the crystallization process of the initial gel with nAL2O3:nP2O5:nDPA/D-iPA:nH2O=1.0:1.0:1.2:75, no intermediate phase was formed when the DPA was used as the structure-directing agent, whereas intermediate phase of aluminophosphate molecular sieve AlPO4-5 was observed when the D-iPA was used as the structure-directing agent. For the crystallization process of the initial gel with nAL2O3:nP2O5:nDPA/D-iPA:nH2O=1.0:1.0:1.0:75, intermediate phase of aluminophosphate molecular sieve VPI-5 was formed when the DPA was used as the structure-directing agent, whereas intermediate phases of both VPI-5 and AlPO4-5 were observed when the D-iPA was used as the structure-directing agent. Theoretical calculation showed that the charge on the N of the protonated DPA was different with that on the N of the protonated D-iPA. The results indicate that the structure-directing effect of amine can be affected by the composition of the initial gel and the fine-tuning of the structure of amine can influence its structure-directing effect. However, such influence is affected by the composition of the initial gel.
2017, 33(9): 1603-1610
doi: 10.11862/CJIC.2017.198
Abstract:
Two substituted benzyltin complexes (C1, C2) has been synthesized via the reaction of N-(2-propionic acid)-aroyl hydrazone with di-p-methylbenzytin dichloride. The complexes C1 and C2 have been characterized by IR, UV-Vis, 1H NMR, 13C NMR 119Sn NMR spectra, elemental analysis and the crystal structures have been determined by X-ray diffraction. In vitro antitumor activities of both complexes were evaluated by the 3-(4, 5-dimethylthiazoly-2-yl)-2, 5-diphenyltetrazolium bromide (MTT) assay against three human cancer cell lines(H460, HepG2, MCF7) and a human cell line(HL7702). Two complexes exhibit strong antitumor activity, moreover, C2 is less toxic than C1. The result of EB fluorescent probe shows the interaction between complexes and calf thymus DNA is intercalation. CCDC: 1457502, C1; 1547503, C2.
Two substituted benzyltin complexes (C1, C2) has been synthesized via the reaction of N-(2-propionic acid)-aroyl hydrazone with di-p-methylbenzytin dichloride. The complexes C1 and C2 have been characterized by IR, UV-Vis, 1H NMR, 13C NMR 119Sn NMR spectra, elemental analysis and the crystal structures have been determined by X-ray diffraction. In vitro antitumor activities of both complexes were evaluated by the 3-(4, 5-dimethylthiazoly-2-yl)-2, 5-diphenyltetrazolium bromide (MTT) assay against three human cancer cell lines(H460, HepG2, MCF7) and a human cell line(HL7702). Two complexes exhibit strong antitumor activity, moreover, C2 is less toxic than C1. The result of EB fluorescent probe shows the interaction between complexes and calf thymus DNA is intercalation. CCDC: 1457502, C1; 1547503, C2.
2017, 33(9): 1611-1617
doi: 10.11862/CJIC.2017.206
Abstract:
Amine molecule plays a role of improving selectivity on the CO2 capture. Small size ethylenediamine molecules were selected to modify the light metal Al-based metal-organic framework (MOFs) MIL-100Al with unsaturated metal sites in this work, the structure of the materials was characterized by XRD, N2 adsorption and FT-IR. The adsorption properties of MIL-100Al modified with different concentrations of ethylenediamine on CO2 and CH4 were tested. Compared with the original MIL-100Al sample, the amount of CO2 adsorbed by MIL-100Al modified with ethylenediamine is significantly improved, while CH4 adsorption decreases. The CO2/CH4 adsorption selectivity of the material therefor is further improved, and the performance of adsorption separation is enhanced.
Amine molecule plays a role of improving selectivity on the CO2 capture. Small size ethylenediamine molecules were selected to modify the light metal Al-based metal-organic framework (MOFs) MIL-100Al with unsaturated metal sites in this work, the structure of the materials was characterized by XRD, N2 adsorption and FT-IR. The adsorption properties of MIL-100Al modified with different concentrations of ethylenediamine on CO2 and CH4 were tested. Compared with the original MIL-100Al sample, the amount of CO2 adsorbed by MIL-100Al modified with ethylenediamine is significantly improved, while CH4 adsorption decreases. The CO2/CH4 adsorption selectivity of the material therefor is further improved, and the performance of adsorption separation is enhanced.
2017, 33(9): 1510-1520
doi: 10.11862/CJIC.2017.191
Abstract:
Bi2Fe4O9/g-C3N4/UiO-66 ternary composites synthesized by a facile hydrothermal method possess synergistically enhanced visible-light photocatalytic performance for degradation of both RhodamineB dye and colorless phenol solutions as compared with purity materials of g-C3N4, Bi2Fe4O9 and UiO-66. The ternary composite materials show increased visible light absorption, efficient separation of charge carriers, strong redox capability via Z-scheme Bi2Fe4O9/g-C3N4 heterojunction and high adsorption ability.
Bi2Fe4O9/g-C3N4/UiO-66 ternary composites synthesized by a facile hydrothermal method possess synergistically enhanced visible-light photocatalytic performance for degradation of both RhodamineB dye and colorless phenol solutions as compared with purity materials of g-C3N4, Bi2Fe4O9 and UiO-66. The ternary composite materials show increased visible light absorption, efficient separation of charge carriers, strong redox capability via Z-scheme Bi2Fe4O9/g-C3N4 heterojunction and high adsorption ability.
2017, 33(9): 1537-1546
doi: 10.11862/CJIC.2017.203
Abstract:
Spherical Ni0.7Co0.15Mn0.15(OH)2 precursor with a full concentration gradient (FCG) of Ni, Co and Mn elements was obtained via co-precipitation method. The precursor was evenly mixed with LiOH·H2O and then sintered at 750~900℃ for 12 h in oxygen to synthesize FCG-LiNi0.7Co0.15Mn0.15O2 cathode material with the Ni rich in core and Mn rich in the outer layer. The diffusion of Ni, Co, and Mn under different calcination temperatures led to various elements homogeneity, and was analyzed by energy-dispersive X-ray spectroscopy (EDXS). Then, the electrochemical properties of samples were investigated by the charge-discharge test and electrochemical impedance spectroscopy (EIS) test. The results indicate that the cathode material sintered at 800℃ has an obvious concentration-gradient distribution with a shell of LiNi0.52Co0.24Mn0.24O2 and exhibits the optimal electrochemical performance. Under the voltage range 2.8~4.3 V, it deliveres an initial discharge of 186.1 mAh·g-1 at a charge-discharge rate of 0.2C, and shows an excellent capacity retention of 90.1% after 200 cycles at a high rate of 2C.
Spherical Ni0.7Co0.15Mn0.15(OH)2 precursor with a full concentration gradient (FCG) of Ni, Co and Mn elements was obtained via co-precipitation method. The precursor was evenly mixed with LiOH·H2O and then sintered at 750~900℃ for 12 h in oxygen to synthesize FCG-LiNi0.7Co0.15Mn0.15O2 cathode material with the Ni rich in core and Mn rich in the outer layer. The diffusion of Ni, Co, and Mn under different calcination temperatures led to various elements homogeneity, and was analyzed by energy-dispersive X-ray spectroscopy (EDXS). Then, the electrochemical properties of samples were investigated by the charge-discharge test and electrochemical impedance spectroscopy (EIS) test. The results indicate that the cathode material sintered at 800℃ has an obvious concentration-gradient distribution with a shell of LiNi0.52Co0.24Mn0.24O2 and exhibits the optimal electrochemical performance. Under the voltage range 2.8~4.3 V, it deliveres an initial discharge of 186.1 mAh·g-1 at a charge-discharge rate of 0.2C, and shows an excellent capacity retention of 90.1% after 200 cycles at a high rate of 2C.
2017, 33(9): 1547-1554
doi: 10.11862/CJIC.2017.192
Abstract:
Reaction of isopropylthiobenzene with n-BuLi, and subsequently with iron carbonyl and iodine gave a dimeric ortho-isopropylthiobenzoyl iron derivative[(o-iPrS)C6H4COFe(CO)2I]2 through two iodide bridges, while similar reaction of thioanisole only yielded mononuclear phenylthiomethyl iron complex C6H5SCH2Fe(CO)3I. These two complexes show significantly different reactivities upon treatment with various nucleophiles. For example, reaction of[(o-iPrS)C6H4COFe(CO)2I]2 with sodium 2-pyridinethiolate (PySNa) give mononuclear complex (o-iPrS)C6H4COFe(CO)2(SPy), while reaction of C6H5SCH2Fe(CO)3I with PySNa results in the decomposition of the starting material. On the other hand, reaction of C6H5SCH2Fe(CO)3I with PPh3 give complex C6H5SCH2Fe(CO)2(PPh3)I, but no characterizable product is obtained from the similar reaction of[(o-iPrS)C6H4COFe(CO)2I]2. All these newly synthesized compounds have been characterized by physico-chemical and spectroscopic methods, and their structures were unambiguously determined by X-ray crystallography.CCDC: 1545834, 1; 1545835, 2A; 1545836, 3; 1545837, 4.
Reaction of isopropylthiobenzene with n-BuLi, and subsequently with iron carbonyl and iodine gave a dimeric ortho-isopropylthiobenzoyl iron derivative[(o-iPrS)C6H4COFe(CO)2I]2 through two iodide bridges, while similar reaction of thioanisole only yielded mononuclear phenylthiomethyl iron complex C6H5SCH2Fe(CO)3I. These two complexes show significantly different reactivities upon treatment with various nucleophiles. For example, reaction of[(o-iPrS)C6H4COFe(CO)2I]2 with sodium 2-pyridinethiolate (PySNa) give mononuclear complex (o-iPrS)C6H4COFe(CO)2(SPy), while reaction of C6H5SCH2Fe(CO)3I with PySNa results in the decomposition of the starting material. On the other hand, reaction of C6H5SCH2Fe(CO)3I with PPh3 give complex C6H5SCH2Fe(CO)2(PPh3)I, but no characterizable product is obtained from the similar reaction of[(o-iPrS)C6H4COFe(CO)2I]2. All these newly synthesized compounds have been characterized by physico-chemical and spectroscopic methods, and their structures were unambiguously determined by X-ray crystallography.CCDC: 1545834, 1; 1545835, 2A; 1545836, 3; 1545837, 4.
2017, 33(9): 1618-1624
doi: 10.11862/CJIC.2017.186
Abstract:
A highly-uniform nanofiber of Ag-graphene-TiO2 was successfully fabricated by the electrospinning technique, which exhibited significantly increased visible light absorption (λ > 420 nm) and improved photocurrent response. The Ag nanoparticles (AgNPs) and graphenes located in TiO2 fibers induced an increase in the visible-light photocurrent response. The photocurrent density of Ag-graphene-TiO2 fibers is 4-fold higher than the pristine TiO2 fibers under visible light. The increased photocurrent response in visible light region is resulted from the strong interaction between TiO2 fibers and graphene sheets, as well as the localized surface plasmon resonance of AgNPs.
A highly-uniform nanofiber of Ag-graphene-TiO2 was successfully fabricated by the electrospinning technique, which exhibited significantly increased visible light absorption (λ > 420 nm) and improved photocurrent response. The Ag nanoparticles (AgNPs) and graphenes located in TiO2 fibers induced an increase in the visible-light photocurrent response. The photocurrent density of Ag-graphene-TiO2 fibers is 4-fold higher than the pristine TiO2 fibers under visible light. The increased photocurrent response in visible light region is resulted from the strong interaction between TiO2 fibers and graphene sheets, as well as the localized surface plasmon resonance of AgNPs.
2017, 33(9): 1625-1630
Abstract:
Solvothermal reactions of 1, 1, 1-tris(hydroxymethyl)propane (H3tmp) and FeCl3 by using different counter ions resulted in three hexanuclear iron(Ⅲ)clusters (C5N2H14)[Fe6(μ6-O)Cl6(tmp)4]·2H2O·CH3OH (1), (C3N2H5)2[Fe6(μ6-O)Cl6(tmp)4] (2), and (C4N3H8)3(C2N3H4)[Fe12(μ6-O)2Cl12(tmp)8]·3CH3OH (3), whose structures were characterized. The tripodal alcohols ligands are very useful in constructing high-nuclearity metal clusters. In all cases, similar anionic cluster[Fe6(μ6-O)Cl6(tmp)4]2- is formed by six Fe(Ⅲ)ions, four tmp3- ligands, one center O2- ion, and six Cl- ions. Within the system of compounds 1 and 3, the nitrogen-containing heterocyclic ligands experience N-and C-alkylation reactions, which is validated by the crystallographic parameters, elemental analyses, and IR. CCDC: 980726, 1; 980727, 2; 980728, 3.
Solvothermal reactions of 1, 1, 1-tris(hydroxymethyl)propane (H3tmp) and FeCl3 by using different counter ions resulted in three hexanuclear iron(Ⅲ)clusters (C5N2H14)[Fe6(μ6-O)Cl6(tmp)4]·2H2O·CH3OH (1), (C3N2H5)2[Fe6(μ6-O)Cl6(tmp)4] (2), and (C4N3H8)3(C2N3H4)[Fe12(μ6-O)2Cl12(tmp)8]·3CH3OH (3), whose structures were characterized. The tripodal alcohols ligands are very useful in constructing high-nuclearity metal clusters. In all cases, similar anionic cluster[Fe6(μ6-O)Cl6(tmp)4]2- is formed by six Fe(Ⅲ)ions, four tmp3- ligands, one center O2- ion, and six Cl- ions. Within the system of compounds 1 and 3, the nitrogen-containing heterocyclic ligands experience N-and C-alkylation reactions, which is validated by the crystallographic parameters, elemental analyses, and IR. CCDC: 980726, 1; 980727, 2; 980728, 3.
2017, 33(9): 1631-1638
doi: 10.11862/CJIC.2017.190
Abstract:
Two coordination polymers with 3D supramolecular network, {[Zn(L)(bpa)0.5(H2O)2]·2.25H2O}n (1) and {[Cd(L)(H2O)]·2H2O}n (2) (H3LCl=5-(4-hydroxypyridinium-1-ylmethyl) isophthalic acid chloride, bpa=1, 2-bis(4-pyridyl)ethane) were hydrothermally synthesized and structurally characterized by X-ray diffraction analyses and further characterized by infrared spectra (IR), elemental analyses, and thermogravimetric (TG) analyses. Compound 1 exhibits a ladder-like chain structure, and such chains are further united together to generate a 3D supramolecular structure through the hydrogen bonding interactions. Compound 2 possesses a 2D coordination network with a 1D channel that run parallel to the coordination layers. Meanwhile, their luminescent properties have also been investigated in detail.CCDC:908522,1;908526,2.
Two coordination polymers with 3D supramolecular network, {[Zn(L)(bpa)0.5(H2O)2]·2.25H2O}n (1) and {[Cd(L)(H2O)]·2H2O}n (2) (H3LCl=5-(4-hydroxypyridinium-1-ylmethyl) isophthalic acid chloride, bpa=1, 2-bis(4-pyridyl)ethane) were hydrothermally synthesized and structurally characterized by X-ray diffraction analyses and further characterized by infrared spectra (IR), elemental analyses, and thermogravimetric (TG) analyses. Compound 1 exhibits a ladder-like chain structure, and such chains are further united together to generate a 3D supramolecular structure through the hydrogen bonding interactions. Compound 2 possesses a 2D coordination network with a 1D channel that run parallel to the coordination layers. Meanwhile, their luminescent properties have also been investigated in detail.CCDC:908522,1;908526,2.
2017, 33(9): 1639-1648
doi: 10.11862/CJIC.2017.174
Abstract:
An azido-Cu(Ⅱ)compound with substituted benzoate derivative, [Cu(4-Fb)(N3)(H2O)]n (1) (4-Fb=4-form-ylbenzoate), has been successfully synthesized, and then structurally and magnetically characterized. Single crystal structure analysis demonstrates that the asymmetric unit of compound 1 possesses one crystallographically independent Cu(Ⅱ)ion that exhibits distorted tetragonal pyramid geometry. Adjacent Cu(Ⅱ)ions are linked by alternating mixed-bridges of μ-1, 1(end-on, EO) azido and syn, syn-carboxylate, forming a linear 1D Cu(Ⅱ)chain-like motif. Magnetic measurements reveal that the dominant ferromagnetic coupling between adjacent Cu(Ⅱ)ions within each chain due to the counter-complementarity of the dual superexchange pathway is observed in the resulting compounds. However, the interesting plots of magnetic ordering and slow magnetic relaxation are absent in the compound. The critical structural parameter, Cu-N-Cu angle of 113.34°, is corresponding to that of known ferromangetic copper systems containing mixed carboxylate/EO-azido connectors. Magneto-structural correlations are also investigated. Moreover, density functional theory (DFT) calculations (using different methods and basis sets) have been performed on title compound to offer qualitatively theoretical explanation for the ferromagnetic coupling between two Cu(Ⅱ)centers.CCDC:1496426.
An azido-Cu(Ⅱ)compound with substituted benzoate derivative, [Cu(4-Fb)(N3)(H2O)]n (1) (4-Fb=4-form-ylbenzoate), has been successfully synthesized, and then structurally and magnetically characterized. Single crystal structure analysis demonstrates that the asymmetric unit of compound 1 possesses one crystallographically independent Cu(Ⅱ)ion that exhibits distorted tetragonal pyramid geometry. Adjacent Cu(Ⅱ)ions are linked by alternating mixed-bridges of μ-1, 1(end-on, EO) azido and syn, syn-carboxylate, forming a linear 1D Cu(Ⅱ)chain-like motif. Magnetic measurements reveal that the dominant ferromagnetic coupling between adjacent Cu(Ⅱ)ions within each chain due to the counter-complementarity of the dual superexchange pathway is observed in the resulting compounds. However, the interesting plots of magnetic ordering and slow magnetic relaxation are absent in the compound. The critical structural parameter, Cu-N-Cu angle of 113.34°, is corresponding to that of known ferromangetic copper systems containing mixed carboxylate/EO-azido connectors. Magneto-structural correlations are also investigated. Moreover, density functional theory (DFT) calculations (using different methods and basis sets) have been performed on title compound to offer qualitatively theoretical explanation for the ferromagnetic coupling between two Cu(Ⅱ)centers.CCDC:1496426.
2017, 33(9): 1649-1655
doi: 10.11862/CJIC.2017.171
Abstract:
Two new inorganic-organic hybrids[(3-F-4-MeAnis)(DB[18]crown-6)]2[Mo6O19]·2CH3CN (1) and[(2-F-4-MeAnis)([18]crown-6)]2[SMo12O40]·2CH3CN (2) (3-F-4-MeAnis=3-fluoro-4-methylanilinium, DB[18]crown-6=dibenzo[18]crown-6, 2-F-4-MeAnis=2-fluoro-4-methylanilinium) have been synthesized and characterized by infrared spectrum (IR), elemental analysis (EA), thermosgravimetric analysis (TGA) and X-ray diffraction. Compounds 1 and 2 are constructed through noncovalent bonding interaction and the polyoxometalates (POMs) and supramolecular cation arrange alternately. Supramolecular cation forms through the N-H…O hydrogen bonding interaction between the nitrogen atom of anilinium and oxygen atoms of crown ether derivatives. In the crystals of 1 and 2, each polyoxoanion is surrounded by six supramolecular cations and forms hexagonal arrangement viewed along the a axis. Crystalline structure and TGA indicated that phenyl rings in DB[18]crown-6 plays an important role in maintaining the stability of compound 1.CCDC:1540103,1;1540105,2.
Two new inorganic-organic hybrids[(3-F-4-MeAnis)(DB[18]crown-6)]2[Mo6O19]·2CH3CN (1) and[(2-F-4-MeAnis)([18]crown-6)]2[SMo12O40]·2CH3CN (2) (3-F-4-MeAnis=3-fluoro-4-methylanilinium, DB[18]crown-6=dibenzo[18]crown-6, 2-F-4-MeAnis=2-fluoro-4-methylanilinium) have been synthesized and characterized by infrared spectrum (IR), elemental analysis (EA), thermosgravimetric analysis (TGA) and X-ray diffraction. Compounds 1 and 2 are constructed through noncovalent bonding interaction and the polyoxometalates (POMs) and supramolecular cation arrange alternately. Supramolecular cation forms through the N-H…O hydrogen bonding interaction between the nitrogen atom of anilinium and oxygen atoms of crown ether derivatives. In the crystals of 1 and 2, each polyoxoanion is surrounded by six supramolecular cations and forms hexagonal arrangement viewed along the a axis. Crystalline structure and TGA indicated that phenyl rings in DB[18]crown-6 plays an important role in maintaining the stability of compound 1.CCDC:1540103,1;1540105,2.
2017, 33(9): 1656-1666
doi: 10.11862/CJIC.2017.199
Abstract:
Bi2WO6/TiO2 nanotubes (Bi2WO6/TiO2-NTs) heterostructures composite were synthesized by multicom-ponent assembly approach combined with hydrothermal treatment employed TiO2 nanotubes as template. Multiple techniques such as X-ray powder diffraction (XRD), X-ray photo-electron spectroscopy (XPS), N2 adsorption-desorption, scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), and UV-Vis diffused absorption spectra (UV-Vis DRS) were applied to investigate the composition, structures, morphologies, optical and electronic properties of as-prepared samples. The heterostructures were formed with Bi2WO6 nanoflakes or nanoparticles attached on the surface of TiO2 nanotubes. The photocatalytic activity of Bi2WO6/TiO2-NTs heterostructures was evaluated sufficiently by photodegradation of rhodamine B (RhB) under multimode including UV, visible and microwave-assisted photocatalysis. Compared to TiO2 nanotubes and Bi2WO6, Bi2WO6/TiO2-NTs-35 shows the highest photocatalytic activity under multimode. In contrast with UV, visible mode, the Bi2WO6/TiO2-NTs-35 shows the highest activity toward RhB degradation under microwave-assisted photocatalytic mode. This enhanced photocatalytic activity is due to the more efficient separation of the e--h+ pairs, originating from the introduction of Bi2WO6 modified TiO2-NTs, the nanotubular geometries, and degradation mode. The main active species of the degradation process are proven to be h+, ·OH, and ·O2- radicals. Moreover, more ·OH and ·O2- radicals were generated under microwave-assisted photocatalytic mode.
Bi2WO6/TiO2 nanotubes (Bi2WO6/TiO2-NTs) heterostructures composite were synthesized by multicom-ponent assembly approach combined with hydrothermal treatment employed TiO2 nanotubes as template. Multiple techniques such as X-ray powder diffraction (XRD), X-ray photo-electron spectroscopy (XPS), N2 adsorption-desorption, scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), and UV-Vis diffused absorption spectra (UV-Vis DRS) were applied to investigate the composition, structures, morphologies, optical and electronic properties of as-prepared samples. The heterostructures were formed with Bi2WO6 nanoflakes or nanoparticles attached on the surface of TiO2 nanotubes. The photocatalytic activity of Bi2WO6/TiO2-NTs heterostructures was evaluated sufficiently by photodegradation of rhodamine B (RhB) under multimode including UV, visible and microwave-assisted photocatalysis. Compared to TiO2 nanotubes and Bi2WO6, Bi2WO6/TiO2-NTs-35 shows the highest photocatalytic activity under multimode. In contrast with UV, visible mode, the Bi2WO6/TiO2-NTs-35 shows the highest activity toward RhB degradation under microwave-assisted photocatalytic mode. This enhanced photocatalytic activity is due to the more efficient separation of the e--h+ pairs, originating from the introduction of Bi2WO6 modified TiO2-NTs, the nanotubular geometries, and degradation mode. The main active species of the degradation process are proven to be h+, ·OH, and ·O2- radicals. Moreover, more ·OH and ·O2- radicals were generated under microwave-assisted photocatalytic mode.
2017, 33(9): 1667-1677
doi: 10.11862/CJIC.2017.202
Abstract:
A series of 2-hydroxy-4-trifluoromethylbenzoic acid(h2tba)-copper complexes:[Cu(htba)2(pz)2] (1), [Cu(htba)(2, 2'-bipy)](htba) (2) and[Cu(htba)2(4, 4'-bipy)] (3) (h2tba=2-hydroxy-4-trifluoromethylbenzoic acid, pz=pyrazole, 2, 2'-bipy=2, 2'-bipyridine, 4, 4'-bipy=4, 4'-bipyridine) have been synthesized and characterized by elemental analysis, IR spectra, UV-Vis, spectroscopy, powder X-ray diffraction, single-crystal X-ray diffraction and thermal gravimetric analysis (TG). The complexes which catalyzed phenol red bromination in the presence of H2O2 and bromide, exhibited high catalytic bromination activity.CCDC:1041787,1;1041788,2;1041789,3.
A series of 2-hydroxy-4-trifluoromethylbenzoic acid(h2tba)-copper complexes:[Cu(htba)2(pz)2] (1), [Cu(htba)(2, 2'-bipy)](htba) (2) and[Cu(htba)2(4, 4'-bipy)] (3) (h2tba=2-hydroxy-4-trifluoromethylbenzoic acid, pz=pyrazole, 2, 2'-bipy=2, 2'-bipyridine, 4, 4'-bipy=4, 4'-bipyridine) have been synthesized and characterized by elemental analysis, IR spectra, UV-Vis, spectroscopy, powder X-ray diffraction, single-crystal X-ray diffraction and thermal gravimetric analysis (TG). The complexes which catalyzed phenol red bromination in the presence of H2O2 and bromide, exhibited high catalytic bromination activity.CCDC:1041787,1;1041788,2;1041789,3.
2017, 33(9): 1678-1684
doi: 10.11862/CJIC.2017.207
Abstract:
Two coordination compounds[Zn(mtyaa)2(H2O)4]·4H2O (1) and[Zn(bpe)(mtyaa)2(H2O)2]n (2) (Hmtyaa=2-(5-methyl-1, 3, 4-thiadiazol-2-ylthio) acetic acid, bpe=1, 2-bis(4-pridyl)ethane) have been synthesized and they were structurally characterized by single-crystal X-ray diffraction, and then were characterized by elemental analysis, FTIR spectra, thermal analysis and powder X-ray diffraction. Compounds 1 and 2 crystallize in the triclinic and monoclinic, space group P1 and C2/c, respectively. Face-to-face π-π interactions and hydrogen bonds between coordinated and free water molecules with carboxylate oxygen atoms connect single molecules in compound 1 into three dimensional network. Compound 2 is connected into three dimensional structure by hydrogen bonds between coordinated water molecules and carboxylate oxygen atoms or nitrogen atoms.CCDC:653462,1;653467,2.
Two coordination compounds[Zn(mtyaa)2(H2O)4]·4H2O (1) and[Zn(bpe)(mtyaa)2(H2O)2]n (2) (Hmtyaa=2-(5-methyl-1, 3, 4-thiadiazol-2-ylthio) acetic acid, bpe=1, 2-bis(4-pridyl)ethane) have been synthesized and they were structurally characterized by single-crystal X-ray diffraction, and then were characterized by elemental analysis, FTIR spectra, thermal analysis and powder X-ray diffraction. Compounds 1 and 2 crystallize in the triclinic and monoclinic, space group P1 and C2/c, respectively. Face-to-face π-π interactions and hydrogen bonds between coordinated and free water molecules with carboxylate oxygen atoms connect single molecules in compound 1 into three dimensional network. Compound 2 is connected into three dimensional structure by hydrogen bonds between coordinated water molecules and carboxylate oxygen atoms or nitrogen atoms.CCDC:653462,1;653467,2.
2017, 33(9): 1685-1696
doi: 10.11862/CJIC.2017.194
Abstract:
Five complexes[Co(HL)2(H2O)2](NO3)2(1), [Cu2(L)2(NO3)2(H2O)4] (2), [Cu2(L)2(AcO)2(H2O)2]·6H2O (3), [Cu2(L)2(HL)2(ClO4)2]·2CH3CN (4) and[Cd2(L)2(HL)2(NO3)2]·2H2O (5) utilizing 3-(2-pyridyl)-1, 2, 4-triazole ligand(HL) as well as different metal salts have been synthesized and structurally characterized by single crystal X-ray diffraction, infrared spectroscopy (IR), elemental analysis, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The structural analyses reveal that complex 1 has a mononuclear structure and forms a 2D supramolecular structure via hydrogen bonding interactions. Complexes 2~5 have dinuclear structures. Complexes 2 and 5 are arranged into 2D supramolecular structurs by the corresponding hydrogen bonding interactions, and complex 3 is also arranged into a 3D supramolecular structure through hydrogen bonding interactions. The coordination modes of HL ligand in the complexes were studied. Moreover, the fluorescent properties and fluorescence lifetimes of ligand HL, complexes 1 and 5 were investigated in the solid at room temperature.CCDC:1054520,1;1054521, 2; 1054522, 3;1054523, 4;1054524, 5
Five complexes[Co(HL)2(H2O)2](NO3)2(1), [Cu2(L)2(NO3)2(H2O)4] (2), [Cu2(L)2(AcO)2(H2O)2]·6H2O (3), [Cu2(L)2(HL)2(ClO4)2]·2CH3CN (4) and[Cd2(L)2(HL)2(NO3)2]·2H2O (5) utilizing 3-(2-pyridyl)-1, 2, 4-triazole ligand(HL) as well as different metal salts have been synthesized and structurally characterized by single crystal X-ray diffraction, infrared spectroscopy (IR), elemental analysis, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The structural analyses reveal that complex 1 has a mononuclear structure and forms a 2D supramolecular structure via hydrogen bonding interactions. Complexes 2~5 have dinuclear structures. Complexes 2 and 5 are arranged into 2D supramolecular structurs by the corresponding hydrogen bonding interactions, and complex 3 is also arranged into a 3D supramolecular structure through hydrogen bonding interactions. The coordination modes of HL ligand in the complexes were studied. Moreover, the fluorescent properties and fluorescence lifetimes of ligand HL, complexes 1 and 5 were investigated in the solid at room temperature.CCDC:1054520,1;1054521, 2; 1054522, 3;1054523, 4;1054524, 5
2017, 33(9): 1697-1704
doi: 10.11862/CJIC.2017.165
Abstract:
Two Cu4I4 coordination polymers, {[Cu2(aadmtrz)I2]·CH3CN}n (1) and[Cu2(dptrz)I]n (2) (aadmtrz=4-((1-aminoethylidene)-amino)-3, 5-dimethyl-1, 2, 4-triazole, dptrz=3, 5-dipropyl-1, 2, 4-triazole), have been synthesized by the solvothermal reactions of CuI and 3, 5-dialkyl-4-amino-1, 2, 4-triazole ligands in mixed H2O/MeCN solution and characterized using elemental analysis, IR, PXRD and single-crystal X-ray diffraction. The structures of the Cu4I4 units in the polymers are different. The Cu4I4 cluster in complex 1 is an inorganic 8-membered ring with a chair-chair conformation, while the one in complex 2 is a distorted cube. Complex 1 exhibits 2D 4, 4-connected rhombic-grid. Complex 2 is a (3, 4)-connected framework with 19.5% porosity. In addition, the luminescent properties of the complexes in the solid state were also investigated.CCDC:1437794,1;1437795,2.
Two Cu4I4 coordination polymers, {[Cu2(aadmtrz)I2]·CH3CN}n (1) and[Cu2(dptrz)I]n (2) (aadmtrz=4-((1-aminoethylidene)-amino)-3, 5-dimethyl-1, 2, 4-triazole, dptrz=3, 5-dipropyl-1, 2, 4-triazole), have been synthesized by the solvothermal reactions of CuI and 3, 5-dialkyl-4-amino-1, 2, 4-triazole ligands in mixed H2O/MeCN solution and characterized using elemental analysis, IR, PXRD and single-crystal X-ray diffraction. The structures of the Cu4I4 units in the polymers are different. The Cu4I4 cluster in complex 1 is an inorganic 8-membered ring with a chair-chair conformation, while the one in complex 2 is a distorted cube. Complex 1 exhibits 2D 4, 4-connected rhombic-grid. Complex 2 is a (3, 4)-connected framework with 19.5% porosity. In addition, the luminescent properties of the complexes in the solid state were also investigated.CCDC:1437794,1;1437795,2.
