To improve the oxidation resistance and corrosion resistance of Zr-4 alloy, titanium nitride （TIN） coatings were prepared on the Zr-4 alloy with a TiN ceramic target with different ratios of N2. Microstructure and h...To improve the oxidation resistance and corrosion resistance of Zr-4 alloy, titanium nitride （TIN） coatings were prepared on the Zr-4 alloy with a TiN ceramic target with different ratios of N2. Microstructure and high-temperature properties of the TiN coated samples were studied by scanning electron microscopy （SEM）, energy dispersive spectrometer （EDS）, X-ray diffraction meter （XRD）, X-ray photoelectron spectroscopy （XPS）, heat treatment furnace and autoclaves, respectively. The x value of the TiN coatings （TiN） ranges from 0.96 to 1.33. After the introduction of N2, TiN coating exhibits a weak （200） plane and a preferred （111） orientation. The coating prepared with an N2 flow ratio of 15% shows an optimal oxidation resistance in the atmospheric environment at 800 ℃. In either 1 200 ℃ steam environment for one hour, or deionized water at 360 ℃ and a pressure of 18.6 Mpa for 16 d, the opitimized TiN coated samples have no delamination or spallation; and the gains in the masses of samples are much smaller than Zr-4 alloy. These results demonstrate the effectiveness of the optimized TiN coating as the protective coating on the Zr-4 alloy under extreme conditons.展开更多
Semiconductor photocatalysis has been considered as a potential technology for the removal of organic dyes from wastewater.The development of photocatalysts with high stability and strong catalytic activity is the mos...Semiconductor photocatalysis has been considered as a potential technology for the removal of organic dyes from wastewater.The development of photocatalysts with high stability and strong catalytic activity is the most important in application.Visible-light-induced NiCo_(2)O_(4)@Co_(3)O_(4) core/shell heterojunctions were synthesized via a sol-gel method in this paper.Compared to bare NiCo_(2)O_(4) and Co_(3)O_(4),NiCo_(2)O_(4)@Co_(3)O_(4) showed a remarkably enhanced removal rate towards congo red(CR)degradation with 98.4%of the removal rate to CR at 120 min under irradiation.The excellent performance of NiCo_(2)O_(4)@Co_(3)O_(4) benefits from the effective separation of photogenerated electron-holes by forming a heterojunction,and the rapid transfer efficiency of photo-generated charge carriers results from the core/shell architectures.A mechanism that NiCo_(2)O_(4)@Co_(3)O_(4) degrades CR to harmless inorganic substances by h^(+),•O-2 and•OH during the photocatalytic process was proposed.展开更多
Hierarchical porous Co_(3)O_(4)spheres were synthesized by a solvothermal method followed by high-temperature calcination.XRD,SEM,TEM and electrochemical tests were used to study the structure and performance of the h...Hierarchical porous Co_(3)O_(4)spheres were synthesized by a solvothermal method followed by high-temperature calcination.XRD,SEM,TEM and electrochemical tests were used to study the structure and performance of the hierarchical porous Co_(3)O_(4)spheres.The results show that the Co_(3)O_(4)synthesized at a calcination temperature of 700°C(Co_(3)O_(4)-700)is micro-sized spheres(1-2μm)consisting of plentiful nanoparticles(50-200 nm)and numerous pores(~100 nm).Due to its numerous porous morphology,the Co_(3)O_(4)-700 anode exhibits the highest cycling performance with excellent reversible discharge and charge specific capacities of 745 and 755 m A·h/g at the current density of 100 m A/g after 100 charge-discharge cycles,respectively.展开更多
As a new organic conjugated semiconductor,graphitic carbon nitride(g-C_(3)N_(4))is emerging as a fascinating material for various photocatalytic applications due to its adjustable electronic structure,outstanding ther...As a new organic conjugated semiconductor,graphitic carbon nitride(g-C_(3)N_(4))is emerging as a fascinating material for various photocatalytic applications due to its adjustable electronic structure,outstanding thermal endurance,appealing chemical stability,low cost,and environmental friendliness.Nevertheless,unmodified bulk g-C_(3)N_(4) possesses some intrinsic limitations related to poor crystallinity,marginal visible-light harvesting,easy recombination of charge pairs,small surface area,and slow charge migration,which give rise to the low quantum efficiency of photocatalytic reactions.One efficient strategy to overcome these shortcomings is the manipulation of the microstructures of g-C_(3)N_(4).Other than the traditional structure control,mimicking the structures of creatures in nature to design and construct bio-inspired structures is a promising approach to improve the photocatalytic performance of g-C_(3)N_(4) and even g-C_(3)N_(4)-based systems.This review summarizes the recent advances of the traditional structure-control of g-C_(3)N_(4)-based systems,and bio-inspired synthesis of g-C_(3)N_(4)-based systems from two aspects of structural bionics and functional bionics.Furthermore,the fundamentals of bio-inspired design and fabrication of g-C_(3)N_(4)-based systems are introduced in detail.Additionally,the different theoretical calculations,diverse photocatalytic applications and various modification strategies of bio-inspired structured g-C_(3)N_(4)-based systems are recapped.We believe that this work will be a guiding star for future research in the new field of biomimetic photocatalysis.展开更多
The hydrothermal reaction of isonicotinic acid (4-C5H4N-COOH), Cu(ClO4)(2). 6H(2)O and water at 170 degreesC gave the title compound, [Cu(OH)(2)(H2O)(2)(4-C5H4N-COOH)(2)] (1), which was analyzed by single-crystal X-ra...The hydrothermal reaction of isonicotinic acid (4-C5H4N-COOH), Cu(ClO4)(2). 6H(2)O and water at 170 degreesC gave the title compound, [Cu(OH)(2)(H2O)(2)(4-C5H4N-COOH)(2)] (1), which was analyzed by single-crystal X-ray diffraction, The complex crystallizes in triclinic space group PY with unit cell parameters: a = 6.337(2), b = 6.894(3), c = 9.178(3). alpha = 99.40(3), beta = 105.26(3), gamma 108.17(5)degrees, V = 354.1(2)Angstrom (3), Z = 1, C12H16CuN2O8, M-r = 379.81, D-c = 1.791 Mg/m(3), F(000) 197, mu (MoK alpha) = 1.589 mm(-1). The final R and wR are 0.068 and 0.170 for 1249 observed reflections with I greater than or equal to2 sigma (I). The central copper ion is in a distorted octahedron geometry completed by two nitrogen atoms from carboxylic ligand, two oxygen atoms from hydroxyl groups and two oxygen atoms from coordinated water molecules. The intermolecular hydrogen bonding leads to the formation of a three-dimensional supramolecular structure.展开更多
C9H6N2O5S2 is monoclinic, space group P21/n, for 1278 observed reflections . The result indicates clearly the sul-fonylation takes place at oxygen. According to the data of bond lengths, the isothiazole ring displays ...C9H6N2O5S2 is monoclinic, space group P21/n, for 1278 observed reflections . The result indicates clearly the sul-fonylation takes place at oxygen. According to the data of bond lengths, the isothiazole ring displays aromaticity in some way.展开更多
A new enone (CH 3CO C( p NO 2C 6H 4COO)=CH S C 6H 4( p Br) 5, C 17 H 12 NBrO 5S, M r =422.25) was synthesized and its crystal structure was determined by X ray diffraction method. The crystal belongs to the monoclinic...A new enone (CH 3CO C( p NO 2C 6H 4COO)=CH S C 6H 4( p Br) 5, C 17 H 12 NBrO 5S, M r =422.25) was synthesized and its crystal structure was determined by X ray diffraction method. The crystal belongs to the monoclinic system, space group P2 1/c with a=6.4121(9), b=12.804(1), c=20.998(2) , β=94.884(9)°, V=1717.1(3) 3, Z=4, D c =1.633 g/cm 3, μ (Mo Kα )=2.542 mm -1 , F( 000)=848. Final R =0.0428 and wR =0.0916 for 3335 reflections with I>2σ(I) . The title compound exists as Z isomer with p bromothiophenolate and o nitrobenzoate groups cis arranged around asymmetrical centre. This observation suggests that the substitution of thiophenolate for bromine is a stereoselective step.展开更多
The title compound 2-(4-fluorophenylamino)-2-thiomethyl acetophe-none (C15H14FNOS, M. = 275. 34 ) was synthesized by the reaction of 2-hydroxy-2-thiomethyl acetohenone (abenzoylhemithioacetal ) with 4-fluoroaniline. T...The title compound 2-(4-fluorophenylamino)-2-thiomethyl acetophe-none (C15H14FNOS, M. = 275. 34 ) was synthesized by the reaction of 2-hydroxy-2-thiomethyl acetohenone (abenzoylhemithioacetal ) with 4-fluoroaniline. The crystal ismonoclinic, space group P21/n. with unit cell constants a = 12. 434 (4 ), b = 6. 00l2(6), c=l8. 49l(2) A, β=100. 87(l)° Z = 4, V = 1355. O(5) A, D'= 1. 350g/cm3, μ(MoKa) = 2. 41 cm-l, F(000) = 576, R=0. 029, Rw.= 0. 041 for 14l2 ob-served reflections (I> 3σ(I) ). X-ray analysis reveals that the dihedral angle betweenplane l (C(l)~C(6), F, N ) and plane 2 (C(8)~C(14), O ) is 4. l8° and theC(7) -S bond is longer than normal single C-S bond.展开更多
The title compound (C20H15ClN4O, Mr = 362.81) was synthesized by the reaction of ethyl 2-cyano-3-(2-chlorophenyl)-1-acylate with 5-amino-3-methyl-1-phenylpyrazole under microwave irradiation and its structure was dete...The title compound (C20H15ClN4O, Mr = 362.81) was synthesized by the reaction of ethyl 2-cyano-3-(2-chlorophenyl)-1-acylate with 5-amino-3-methyl-1-phenylpyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 8.8192(19), b = 15.976(3), c = 13.094(3) ? = 103.074(4), V = 1797.1(7) ?, Z = 4, Dc = 1.341 g/cm3, = 0.229 mm-1, F(000) = 752, R = 0.0632 and wR = 0.1278. X-ray analysis reveals that the pyridine ring adopts an envelope conformation. The dihedral angle between the pyrazole and pyridine planes is 2.19, and inter- molecular hydrogen bonds are also observed in the molecule.展开更多
A novel compound [(CH 3CH 2) 4N] 4[(La 12 (OH) 12 MoO 29 )] was synthesized by hydrothermal reaction. The single crystal X ray diffraction shows that the compound crystallized in the monoclinic space group C2/c ; a =2...A novel compound [(CH 3CH 2) 4N] 4[(La 12 (OH) 12 MoO 29 )] was synthesized by hydrothermal reaction. The single crystal X ray diffraction shows that the compound crystallized in the monoclinic space group C2/c ; a =2 5729(4) nm, b =1 4318(1) nm, c =2 1217(4) nm, β =111 56(1)°, V =6 8235(7) nm 3, Z =4, R =0 0751. The basic building blocks of the crystal structure included one MoO 5 hexahedron and twelve LaO 6 octahedra which shared a common edge to form a [(La 12 (OH) 12 MoO 29 )] 4- unit. These units were held together by the [(CH 3CH 2) 4N] + ions.展开更多
The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amin...The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amine with 2-methoxylcarbonylbenzene-sulfonylisocya- nate. The crystal is of monoclinic, space group P21/c with a =11.169(3), b = 9.508(3), c = 17.690(5) ? b = 91.593(5), Z = 4, V = 1877.9(10) 3, Dc = 1.459 g/cm3, F(000) = 856, m(MoKa) = 0.324 mm-1, R = 0.0690 and wR = 0.1368 for 3301 observed reflections (I > 2s(I)). The N(1)H…N(3) and N(2)H…O(4) hydrogen bonds can be observed. In the molecule the phenyl plane(I), pyrimi- din-2-yl-urea bridge plane(Ⅱ) and ester plane(Ⅲ) form three conjugated systems.展开更多
The crystal structure of crown ether-hydrogen bonded complex,[La(NO3)3 (12-crown-4) ( H2O)] (12-crown-4) has been determined by X-ray method. The title complex C16H34LaN3O18 (Mr=695. 5) crystallized in orthorhombic ...The crystal structure of crown ether-hydrogen bonded complex,[La(NO3)3 (12-crown-4) ( H2O)] (12-crown-4) has been determined by X-ray method. The title complex C16H34LaN3O18 (Mr=695. 5) crystallized in orthorhombic Pnma with a=23. 495(8), b=13. 603(5),c=8. 474(3); V=2706(1); Z=4 ; Dc=1. 71 g/cm3; F(000)=1408, μ=17. 0 cm-1 (MOKα). The final R=0. 052 and Rw= 0. 054(unit weight) for 1367 observed reflections. The La( Ⅲ) ion is 11-coordinated by three nitrale anions, four oxygen atoms from a crown ligand and one O atom of a water molecule. The other crown molecule is hydrogen bonded wilh the coordinated water molecule. The imposed mirror plane in the structure made both crown ligands and one of nitrate groups severely disordered.展开更多
基金Funded by the National Science and Technology Major Project of the Ministry of Science and Technology of China(2015ZX06004001-002)the Postgraduate Research and Innovation Project of the University of South China(2017XCX11)
文摘To improve the oxidation resistance and corrosion resistance of Zr-4 alloy, titanium nitride （TIN） coatings were prepared on the Zr-4 alloy with a TiN ceramic target with different ratios of N2. Microstructure and high-temperature properties of the TiN coated samples were studied by scanning electron microscopy （SEM）, energy dispersive spectrometer （EDS）, X-ray diffraction meter （XRD）, X-ray photoelectron spectroscopy （XPS）, heat treatment furnace and autoclaves, respectively. The x value of the TiN coatings （TiN） ranges from 0.96 to 1.33. After the introduction of N2, TiN coating exhibits a weak （200） plane and a preferred （111） orientation. The coating prepared with an N2 flow ratio of 15% shows an optimal oxidation resistance in the atmospheric environment at 800 ℃. In either 1 200 ℃ steam environment for one hour, or deionized water at 360 ℃ and a pressure of 18.6 Mpa for 16 d, the opitimized TiN coated samples have no delamination or spallation; and the gains in the masses of samples are much smaller than Zr-4 alloy. These results demonstrate the effectiveness of the optimized TiN coating as the protective coating on the Zr-4 alloy under extreme conditons.
基金Project(2017TP1031)supported by the Hunan Key Laboratory for Rare Earth Functional Materials,ChinaProject(2020JJ4735)supported by the Natural Science Foundation of Hunan Province,China+1 种基金Project(2018GK4001)supported by Science and Technology Department of Hunan Province Tackling Key Scientific and Technological Problems and Transformation of Major Scientific and Technological Achievements,ChinaProject(CSUZC202126)supported by the Open Sharing Fund for the Large-scale Instruments and Equipments of Central South University,China。
文摘Semiconductor photocatalysis has been considered as a potential technology for the removal of organic dyes from wastewater.The development of photocatalysts with high stability and strong catalytic activity is the most important in application.Visible-light-induced NiCo_(2)O_(4)@Co_(3)O_(4) core/shell heterojunctions were synthesized via a sol-gel method in this paper.Compared to bare NiCo_(2)O_(4) and Co_(3)O_(4),NiCo_(2)O_(4)@Co_(3)O_(4) showed a remarkably enhanced removal rate towards congo red(CR)degradation with 98.4%of the removal rate to CR at 120 min under irradiation.The excellent performance of NiCo_(2)O_(4)@Co_(3)O_(4) benefits from the effective separation of photogenerated electron-holes by forming a heterojunction,and the rapid transfer efficiency of photo-generated charge carriers results from the core/shell architectures.A mechanism that NiCo_(2)O_(4)@Co_(3)O_(4) degrades CR to harmless inorganic substances by h^(+),•O-2 and•OH during the photocatalytic process was proposed.
基金funded by the Natural Science Foundation of Hunan Province,China(No.2020JJ4729)。
文摘Hierarchical porous Co_(3)O_(4)spheres were synthesized by a solvothermal method followed by high-temperature calcination.XRD,SEM,TEM and electrochemical tests were used to study the structure and performance of the hierarchical porous Co_(3)O_(4)spheres.The results show that the Co_(3)O_(4)synthesized at a calcination temperature of 700°C(Co_(3)O_(4)-700)is micro-sized spheres(1-2μm)consisting of plentiful nanoparticles(50-200 nm)and numerous pores(~100 nm).Due to its numerous porous morphology,the Co_(3)O_(4)-700 anode exhibits the highest cycling performance with excellent reversible discharge and charge specific capacities of 745 and 755 m A·h/g at the current density of 100 m A/g after 100 charge-discharge cycles,respectively.
文摘As a new organic conjugated semiconductor,graphitic carbon nitride(g-C_(3)N_(4))is emerging as a fascinating material for various photocatalytic applications due to its adjustable electronic structure,outstanding thermal endurance,appealing chemical stability,low cost,and environmental friendliness.Nevertheless,unmodified bulk g-C_(3)N_(4) possesses some intrinsic limitations related to poor crystallinity,marginal visible-light harvesting,easy recombination of charge pairs,small surface area,and slow charge migration,which give rise to the low quantum efficiency of photocatalytic reactions.One efficient strategy to overcome these shortcomings is the manipulation of the microstructures of g-C_(3)N_(4).Other than the traditional structure control,mimicking the structures of creatures in nature to design and construct bio-inspired structures is a promising approach to improve the photocatalytic performance of g-C_(3)N_(4) and even g-C_(3)N_(4)-based systems.This review summarizes the recent advances of the traditional structure-control of g-C_(3)N_(4)-based systems,and bio-inspired synthesis of g-C_(3)N_(4)-based systems from two aspects of structural bionics and functional bionics.Furthermore,the fundamentals of bio-inspired design and fabrication of g-C_(3)N_(4)-based systems are introduced in detail.Additionally,the different theoretical calculations,diverse photocatalytic applications and various modification strategies of bio-inspired structured g-C_(3)N_(4)-based systems are recapped.We believe that this work will be a guiding star for future research in the new field of biomimetic photocatalysis.
文摘The hydrothermal reaction of isonicotinic acid (4-C5H4N-COOH), Cu(ClO4)(2). 6H(2)O and water at 170 degreesC gave the title compound, [Cu(OH)(2)(H2O)(2)(4-C5H4N-COOH)(2)] (1), which was analyzed by single-crystal X-ray diffraction, The complex crystallizes in triclinic space group PY with unit cell parameters: a = 6.337(2), b = 6.894(3), c = 9.178(3). alpha = 99.40(3), beta = 105.26(3), gamma 108.17(5)degrees, V = 354.1(2)Angstrom (3), Z = 1, C12H16CuN2O8, M-r = 379.81, D-c = 1.791 Mg/m(3), F(000) 197, mu (MoK alpha) = 1.589 mm(-1). The final R and wR are 0.068 and 0.170 for 1249 observed reflections with I greater than or equal to2 sigma (I). The central copper ion is in a distorted octahedron geometry completed by two nitrogen atoms from carboxylic ligand, two oxygen atoms from hydroxyl groups and two oxygen atoms from coordinated water molecules. The intermolecular hydrogen bonding leads to the formation of a three-dimensional supramolecular structure.
文摘C9H6N2O5S2 is monoclinic, space group P21/n, for 1278 observed reflections . The result indicates clearly the sul-fonylation takes place at oxygen. According to the data of bond lengths, the isothiazole ring displays aromaticity in some way.
文摘A new enone (CH 3CO C( p NO 2C 6H 4COO)=CH S C 6H 4( p Br) 5, C 17 H 12 NBrO 5S, M r =422.25) was synthesized and its crystal structure was determined by X ray diffraction method. The crystal belongs to the monoclinic system, space group P2 1/c with a=6.4121(9), b=12.804(1), c=20.998(2) , β=94.884(9)°, V=1717.1(3) 3, Z=4, D c =1.633 g/cm 3, μ (Mo Kα )=2.542 mm -1 , F( 000)=848. Final R =0.0428 and wR =0.0916 for 3335 reflections with I>2σ(I) . The title compound exists as Z isomer with p bromothiophenolate and o nitrobenzoate groups cis arranged around asymmetrical centre. This observation suggests that the substitution of thiophenolate for bromine is a stereoselective step.
文摘The title compound 2-(4-fluorophenylamino)-2-thiomethyl acetophe-none (C15H14FNOS, M. = 275. 34 ) was synthesized by the reaction of 2-hydroxy-2-thiomethyl acetohenone (abenzoylhemithioacetal ) with 4-fluoroaniline. The crystal ismonoclinic, space group P21/n. with unit cell constants a = 12. 434 (4 ), b = 6. 00l2(6), c=l8. 49l(2) A, β=100. 87(l)° Z = 4, V = 1355. O(5) A, D'= 1. 350g/cm3, μ(MoKa) = 2. 41 cm-l, F(000) = 576, R=0. 029, Rw.= 0. 041 for 14l2 ob-served reflections (I> 3σ(I) ). X-ray analysis reveals that the dihedral angle betweenplane l (C(l)~C(6), F, N ) and plane 2 (C(8)~C(14), O ) is 4. l8° and theC(7) -S bond is longer than normal single C-S bond.
基金This work was supported by the NNSFC (No. 20372057) the NSF of Jiangsu Province (No. BK2001142)+2 种基金 the Open Foundation of Key Laboratory of Organic Synthesis of Jiangsu Province College of Chemistry and Chemical Engineering Suzhou University (No. S
文摘The title compound (C20H15ClN4O, Mr = 362.81) was synthesized by the reaction of ethyl 2-cyano-3-(2-chlorophenyl)-1-acylate with 5-amino-3-methyl-1-phenylpyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 8.8192(19), b = 15.976(3), c = 13.094(3) ? = 103.074(4), V = 1797.1(7) ?, Z = 4, Dc = 1.341 g/cm3, = 0.229 mm-1, F(000) = 752, R = 0.0632 and wR = 0.1278. X-ray analysis reveals that the pyridine ring adopts an envelope conformation. The dihedral angle between the pyrazole and pyridine planes is 2.19, and inter- molecular hydrogen bonds are also observed in the molecule.
基金Supported by the National Natural Science Foundation of China(No.2 0 1710 10 )
文摘A novel compound [(CH 3CH 2) 4N] 4[(La 12 (OH) 12 MoO 29 )] was synthesized by hydrothermal reaction. The single crystal X ray diffraction shows that the compound crystallized in the monoclinic space group C2/c ; a =2 5729(4) nm, b =1 4318(1) nm, c =2 1217(4) nm, β =111 56(1)°, V =6 8235(7) nm 3, Z =4, R =0 0751. The basic building blocks of the crystal structure included one MoO 5 hexahedron and twelve LaO 6 octahedra which shared a common edge to form a [(La 12 (OH) 12 MoO 29 )] 4- unit. These units were held together by the [(CH 3CH 2) 4N] + ions.
基金The project was supported by the National Natural Science Foundation of China (20372021) and Natural Science Foundation of Hunan Province (03JJY3018)
文摘The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amine with 2-methoxylcarbonylbenzene-sulfonylisocya- nate. The crystal is of monoclinic, space group P21/c with a =11.169(3), b = 9.508(3), c = 17.690(5) ? b = 91.593(5), Z = 4, V = 1877.9(10) 3, Dc = 1.459 g/cm3, F(000) = 856, m(MoKa) = 0.324 mm-1, R = 0.0690 and wR = 0.1368 for 3301 observed reflections (I > 2s(I)). The N(1)H…N(3) and N(2)H…O(4) hydrogen bonds can be observed. In the molecule the phenyl plane(I), pyrimi- din-2-yl-urea bridge plane(Ⅱ) and ester plane(Ⅲ) form three conjugated systems.
文摘The crystal structure of crown ether-hydrogen bonded complex,[La(NO3)3 (12-crown-4) ( H2O)] (12-crown-4) has been determined by X-ray method. The title complex C16H34LaN3O18 (Mr=695. 5) crystallized in orthorhombic Pnma with a=23. 495(8), b=13. 603(5),c=8. 474(3); V=2706(1); Z=4 ; Dc=1. 71 g/cm3; F(000)=1408, μ=17. 0 cm-1 (MOKα). The final R=0. 052 and Rw= 0. 054(unit weight) for 1367 observed reflections. The La( Ⅲ) ion is 11-coordinated by three nitrale anions, four oxygen atoms from a crown ligand and one O atom of a water molecule. The other crown molecule is hydrogen bonded wilh the coordinated water molecule. The imposed mirror plane in the structure made both crown ligands and one of nitrate groups severely disordered.
