Structure and polarity of the Si C single crystal have been analyzed with the four- circle X- ray diffraction method by a double- crystal diffractom eter.The hexagonal{ 10 15 } pole figure shows that this Si C sam pl...Structure and polarity of the Si C single crystal have been analyzed with the four- circle X- ray diffraction method by a double- crystal diffractom eter.The hexagonal{ 10 15 } pole figure shows that this Si C sam ple has a6 H modification.The difference between the integrated intensities m easured byω scan in the triple- axis diffraction set- up finds some convincing evidence that the surface is either a Si- terminated face or C- terminated face.The experi- mental ratios of| F( 0 0 0 L) | 2 / | F( 0 0 0 L) | 2 are in good agreem entwith the calculated ones after the dispersion cor- rections to the atomic scattering factors( L=6 ,12 and18,respectively) .Thus,this m easurem ent technique is con- venient for the application of the materials with remarkable surface polarity.展开更多
A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, ...A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, Zr4＋, Ti4＋and Pb4＋cations are incorporated into the lattice of tetragonal rutile SnO2 to form a solid solution structure. As a consequence, the surface area and thermal stability of the catalysts are improved. Moreover, the oxygen species of the modified catalysts become easier to be reduced. Therefore, the oxidation activity over the catalysts was improved, except for the one modified by Pb oxide. Manganese oxide demonstrates the best promotional effects for SnO2. Using an X‐ray diffraction extrapolation method, the lattice capacity of SnO2 for Mn2O3 was 0.135 g Mn2O3/g SnO2, which indicates that to form stable solid solution, only 21%Sn4＋cations in the lattice can be maximally replaced by Mn3＋. If the amount of Mn3＋cations is over the capacity, Mn2O3 will be formed, which is not favorable for the activity of the catalysts. The Sn rich samples with only Sn‐Mn solid solution phase show higher activity than the ones with excess Mn2O3 species.展开更多
New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebip...New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebipy = 4,5-dimethyl-2,2＇-bipyridine） were synthesized and characterized by IH NMR and elemental analysis. The crystal structure of bis（4-methylpyridine）-4,5- dimethyl-2,2＇-bipyridinepalladium（II）perchlorate [Pd（4,5-dmbipy）（4-pic）2]（CIO4）2 was also determined by single crystal X-ray diffraction. This complex crystallized in the triclinic crystal system and space group PI with a = 9.562 （2）, b = 11.326 （4）, c = 15.0120 （10） A°; α = 70.940°, β= 77.60 （2）, γ= 67.86 （2） and z = 4. The Pd （II） in square planar environment showed a small distortion towards tetrahedral through one coordinated bipyridine ring twisting with respect to the other.展开更多
8β-hydroxyeremophil-7（11）-ene-12,8α（4β,6α）-diolide was isolated from the Ligularia intermedia and characterized by MS, multi NMR and X-ray single crystal diffraction. Its crystal structure was determined as in...8β-hydroxyeremophil-7（11）-ene-12,8α（4β,6α）-diolide was isolated from the Ligularia intermedia and characterized by MS, multi NMR and X-ray single crystal diffraction. Its crystal structure was determined as in a orthorhombic type, with space group P212121 with a=6.8519（5）, b=10.7191（8）, c=18.5942（14） A, V=1365.67（18） A,^3 Z=4, and the calculated density is 1.354 mg/m^3. F（000）=592, μ=0.101 mm^-1.展开更多
The reaction of tetraethylammonium metavanadate, （Et4N）VO3, with isovanillin semithiocarbazone（VSTC）, HOC6H3（OCH3）CH=NNHCSNH2, in a mixed solvent of ethanol, water and DMSO yields the mononuclear dioxovanadate（...The reaction of tetraethylammonium metavanadate, （Et4N）VO3, with isovanillin semithiocarbazone（VSTC）, HOC6H3（OCH3）CH=NNHCSNH2, in a mixed solvent of ethanol, water and DMSO yields the mononuclear dioxovanadate（V） complex, [（C2H5）4N][V（V）O2 （OC6H3- （OCH3）CHNNCSNH2）](H2O （C17H31N4O5SV, Mr = 454.5） and its single-crystal structure has been determined by X-ray diffraction. The crystal belongs to orthorhombic space group P212121 with unit cell parameters a = 12.940（3）, b= 15.414（3）, c = 10.703（2） ?, V = 2134.8（11） ?3, Z=4, Dcalc = 1.414 Kg/m3, ( = 0.597 mm-1, and F（000） = 960. The final agreement factors are R = 0.076 and Rw=0.096 for 1600 observed independent reflections with F ≥4.0(（F）. The structure revealed that the vanadium atom is bound to two terminal oxygen atoms and one tridentate donor ligand in a distorted square pyramidal arrangement. The sulphur-nitrogen-oxygen donor Schiff-base ligand in the thiol form rather than the thione form is coordinated to the vanadium via the mercapto sulphur, the (-nitrogen and the hydroxylate oxygen.展开更多
This paper focused on the crystal structures of two new ternary phases,Ti(Cu,Pt)2 and Ti(Cu,Pt)3,which were studied by X-ray powder diffraction data using Rietveld method.Electron probe microanalysis was used for samp...This paper focused on the crystal structures of two new ternary phases,Ti(Cu,Pt)2 and Ti(Cu,Pt)3,which were studied by X-ray powder diffraction data using Rietveld method.Electron probe microanalysis was used for sample composition examination.Elastic properties of these phases were further measured by nano-indentation,and meanwhile calculated with first-principle(FP)calculations.It is found that the crystal structure of Ti(Cu,Pt)2 is of orthorhombic cell space group Amm2(No.38)with structural prototype of VAu2.The resolved structure of Ti(Cu,Pt)3 is of tetragonal Al Pt3 type,belonging to the space group P4/mmm(No.123).The nano-indentation measurement and FP calculations show that the elastic modulus of Ti(Cu,Pt)2 increases firstly then decreases with Pt content,whereas that of Ti(Cu,Pt)3almost linearly increases with Pt content.展开更多
Grain growth of nanostructured Al6061produced by cryorolling and aging process was investigated during isothermalheat treatment in100?500°C temperature range.Transmission electron microscopy(TEM)observations demo...Grain growth of nanostructured Al6061produced by cryorolling and aging process was investigated during isothermalheat treatment in100?500°C temperature range.Transmission electron microscopy(TEM)observations demonstrate that aftercryorolling and aging at130°C for30h,the microstructure contains61nm grains with dispersed50?150nm precipitates and0.248%lattice strain.In addition,an increase in tensile strength up to362MPa because of formation of fine strengtheningprecipitation and nano-sized grains was observed.Thermal stability investigation within100?500°C temperature range showedrelease of lattice strain,dissolution of precipitates and grain growth.According to the X-ray diffraction(XRD)analysis,Mg2Siprecipitates disappeared after annealing at temperatures higher than300°C.According to the results,due to the limited grain growthup to200°C,there would be little decrease in mechanical properties,but within300?500°C range,the grain growth,dissolution ofstrengthening precipitates and decrease in mechanical properties are remarkable.The activation energies for grain growth werecalculated to be203.3kJ/mol for annealing at100?200°C and166.34kJ/mol for annealing at300?500°C.The effect ofprecipitation dissolution on Al lattice parameter,displacement of Al6061(111)XRD peak and Portevin?LeChatelier(PLC)effect onstress?strain curves is also discussed.展开更多
Development of inhomogeneous deformation is an interest matter in material engineering. Synchrotron radiation tomography provides 3D distribution map of local strain in polycrystalline aluminum alloy by tracking micro...Development of inhomogeneous deformation is an interest matter in material engineering. Synchrotron radiation tomography provides 3D distribution map of local strain in polycrystalline aluminum alloy by tracking microstructural features. To perform further deep analysis on development of inhomogeneous deformation, crystallographic grain orientation is necessary. Three-dimensional X-ray diffraction technique was developed. A new crystallographic orientation measurement method was described in 3D space, utilizing grain boundary tracking （GBT） information.展开更多
CaCO3 was chosen as main raw material and Solid State method was used to prepare the sample. The precursor was directly sintered at 1100 ℃ with reducing atmosphere for 3 h to obtain new green CaO：Tb^3＋, Li^＋ Phosp...CaCO3 was chosen as main raw material and Solid State method was used to prepare the sample. The precursor was directly sintered at 1100 ℃ with reducing atmosphere for 3 h to obtain new green CaO：Tb^3＋, Li^＋ Phosphors. The effects of the content of the doping ions Tb^3＋ on the luminescent properties have been studied. The structure, morphology and luminescent properties of the phosphors were characterized by XRD, SEM, UV and PL-PLE spectra respectively. The results showed that the CaO：Tb^3＋, Li^＋ was a single face-centered cubic crystals, the phosphor particle distributed uniformly. The phosphor has a strong absorptive capacity excited by 282 nm ultraviolet ray, and could emit the strong green light with the wavelength of 543 nm （^5D4→^7F5）. The CaO：Tb^3＋, Li^＋ is a new type of green fluorescent material.展开更多
Organic semiconductoe 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA) has been synthetized with 1,8-naphthalic anhydride using chemical method.X-ray diffraction spectrum shows that it is monoclinic.Visible absorp...Organic semiconductoe 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA) has been synthetized with 1,8-naphthalic anhydride using chemical method.X-ray diffraction spectrum shows that it is monoclinic.Visible absorption spectrum shows that its gap band is 2.2 eV with singlet exciton bandwidth of 0.9 eV.展开更多
A new compound containing discrete cationic and anionic complexes, [Cu(pyr)3]Hg2I6 (C30H24CuHg2I6N6), where pyr = 2,2-bipyridine, was prepared by the reaction of CuBr with pyr and HgI2 in a mixed solvent of acetone, m...A new compound containing discrete cationic and anionic complexes, [Cu(pyr)3]Hg2I6 (C30H24CuHg2I6N6), where pyr = 2,2-bipyridine, was prepared by the reaction of CuBr with pyr and HgI2 in a mixed solvent of acetone, methanol and acetonitrile. Single-crystal X-ray diffraction analysis indicates that it crystallizes in an orthorhombic system, Pna21 (No. 33), a = 33.1595(7), b = 9.4605(1), c = 13.0899(2) ? V = 4106.4(1) 3, Mr = 1694.67, Dc = 2.741 g/cm3, Z = 4, F(000) = 3012, m(MoKa) = 12.511 mm-1, R = 0.0736, wR = 0.1360 (I > 2(I)) and S = 1.218. The structure consists of discrete [Hg2I6]2- anions and [Cu(bipyridine)3]2+ cations. The double tetrahedral [Hg2I6]2- unit is formed by sharing one tetrahedral edge and possesses approximate D2h symmetry. The mononuclear Cu2+ ion is coordinated by six N atoms from three pyr molecules to form a slightly disordered octahedral geometry.展开更多
The crystal of Nd(0.06)Y(0.94)S(r)6Sc(BO3)(6) with the dimensions up to 35 mm x 28 mm x 13 mm was grown by a top-seeded solution growth method from Li6B4O9 flux. The grown crystal was characterized by X-ray powder dif...The crystal of Nd(0.06)Y(0.94)S(r)6Sc(BO3)(6) with the dimensions up to 35 mm x 28 mm x 13 mm was grown by a top-seeded solution growth method from Li6B4O9 flux. The grown crystal was characterized by X-ray powder diffraction. The optical absorption of the crystal shows that it has a strong absorption band at 8070 Angstrom, and the absorption coefficient is 2.17cm(-1) with a FWHM of 41 Angstrom, which can match with the wavelength of the diode-laser (LD) and is suitable for the LD pumping. Based on the Judd-Ofelt theory, the three parameters of line oscillator strength Omega((lambda)) (lambda = 2, 4 and 6) of the Nd3+ ion in the crystal were calculated as follows: Omega(2) = 1.194 x 10(-20), Omega(4) = 4.186 x 10(-20) and Omega(6) = 3.351 x 10(-20) cm(2), Which are relatively larger. The results indicate that the crystal Nd0.06Y0.94Sr6Sc(BO3)(6) may be a kind of high-efficient laser material for diode-pumped.展开更多
Two new inclusion 1,4-butylenediphosphonates with three-dimensional hydrogen- bonded frameworks have been synthesized and determined by single-crystal X-ray diffraction. In compound 1, the two-dimensional cationic sub...Two new inclusion 1,4-butylenediphosphonates with three-dimensional hydrogen- bonded frameworks have been synthesized and determined by single-crystal X-ray diffraction. In compound 1, the two-dimensional cationic substructures interpenetrate into the anionic framework, and in compound 2, the cations are encapsulated in the three-dimensional framework. Crystal 1 (C14H24N2O8P2) belongs to triclinic, space group P?with a = 9.4645(2), b = 9.6490(2), c = 11.9479(3) ? = 79.7420(10), b = 73.5650(10), = 63.8420(10), V = 937.55(4) 3, Z = 2, Mr = 410.29, Dc = 1.453 g/cm3, m(MoKa) = 0.276 mm-1, F(000) = 432, the final R = 0.0465 and wR = 0.1304 for 3274 independent reflections. Crystal 2 (C18H26N2O10P2) is of monoclinic, space group P21/c with a = 9.7069(12), b = 16.227(2), c = 6.9339(9) ? b = 98.834(3), V = 1079.2(2) ?, Z = 2, Mr = 492.35, Dc = 1.515 g/cm3, m(MoKa) = 0.261 mm-1, F(000) = 516, the final R = 0.0611 and wR = 0.1162 for 1871 independent reflections.展开更多
A new ligand 1,4-bis(2-hydroxymethylphenyl)-1,4-dioxabutane was synthesized by reducing 1,4-bis(2-formylphenyl)-1,4-dioxabutane with NaBH4 in absolute methanol solution. The crystal structure of the title compound C16...A new ligand 1,4-bis(2-hydroxymethylphenyl)-1,4-dioxabutane was synthesized by reducing 1,4-bis(2-formylphenyl)-1,4-dioxabutane with NaBH4 in absolute methanol solution. The crystal structure of the title compound C16H18O4 has been determined by single-crystal X-ray diffraction. The ligand crystallizes in the orthorhombic system, space group Pbcn with a = 13.777(1), b = 11.731(1), c = 9.076(8) ? V = 1466.8(2) ?, Mr = 274.30, Z = 4, F(000) = 548, Dc = 1.24 g/cm3, T = 293 K, m = 8.9 cm-1 and l = 0.71073 ? The structure was refined to R = 0.0324 and wR = 0.1025 for 1112 observed reflections with I > 2s(I). The two benzene rings are not on the same plane, and the dihedral angle between them is 60.6? The ligand has C2 symmetry axis which passes through the center of C(8)C(8a). The molecules are linked to each other by hydrogen bonding network to form supramolecular chain. The ligands connect to each other through the hydrogen bonds to form one-dimensional chains which further connect through the hydrogen bonds to form two- and three-dimensional structures.展开更多
文摘Structure and polarity of the Si C single crystal have been analyzed with the four- circle X- ray diffraction method by a double- crystal diffractom eter.The hexagonal{ 10 15 } pole figure shows that this Si C sam ple has a6 H modification.The difference between the integrated intensities m easured byω scan in the triple- axis diffraction set- up finds some convincing evidence that the surface is either a Si- terminated face or C- terminated face.The experi- mental ratios of| F( 0 0 0 L) | 2 / | F( 0 0 0 L) | 2 are in good agreem entwith the calculated ones after the dispersion cor- rections to the atomic scattering factors( L=6 ,12 and18,respectively) .Thus,this m easurem ent technique is con- venient for the application of the materials with remarkable surface polarity.
基金supported by the National Natural Science Foundation of China (21263015,21567016 and 21503106)the Education Department Foundation of Jiangxi Province (KJLD14005 and GJJ150016)the Natural Science Foundation of Jiangxi Province (20142BAB213013 and 20151BBE50006),which are greatly acknowledged by the authors~~
文摘A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, Zr4＋, Ti4＋and Pb4＋cations are incorporated into the lattice of tetragonal rutile SnO2 to form a solid solution structure. As a consequence, the surface area and thermal stability of the catalysts are improved. Moreover, the oxygen species of the modified catalysts become easier to be reduced. Therefore, the oxidation activity over the catalysts was improved, except for the one modified by Pb oxide. Manganese oxide demonstrates the best promotional effects for SnO2. Using an X‐ray diffraction extrapolation method, the lattice capacity of SnO2 for Mn2O3 was 0.135 g Mn2O3/g SnO2, which indicates that to form stable solid solution, only 21%Sn4＋cations in the lattice can be maximally replaced by Mn3＋. If the amount of Mn3＋cations is over the capacity, Mn2O3 will be formed, which is not favorable for the activity of the catalysts. The Sn rich samples with only Sn‐Mn solid solution phase show higher activity than the ones with excess Mn2O3 species.
文摘New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebipy = 4,5-dimethyl-2,2＇-bipyridine） were synthesized and characterized by IH NMR and elemental analysis. The crystal structure of bis（4-methylpyridine）-4,5- dimethyl-2,2＇-bipyridinepalladium（II）perchlorate [Pd（4,5-dmbipy）（4-pic）2]（CIO4）2 was also determined by single crystal X-ray diffraction. This complex crystallized in the triclinic crystal system and space group PI with a = 9.562 （2）, b = 11.326 （4）, c = 15.0120 （10） A°; α = 70.940°, β= 77.60 （2）, γ= 67.86 （2） and z = 4. The Pd （II） in square planar environment showed a small distortion towards tetrahedral through one coordinated bipyridine ring twisting with respect to the other.
文摘8β-hydroxyeremophil-7（11）-ene-12,8α（4β,6α）-diolide was isolated from the Ligularia intermedia and characterized by MS, multi NMR and X-ray single crystal diffraction. Its crystal structure was determined as in a orthorhombic type, with space group P212121 with a=6.8519（5）, b=10.7191（8）, c=18.5942（14） A, V=1365.67（18） A,^3 Z=4, and the calculated density is 1.354 mg/m^3. F（000）=592, μ=0.101 mm^-1.
文摘The reaction of tetraethylammonium metavanadate, （Et4N）VO3, with isovanillin semithiocarbazone（VSTC）, HOC6H3（OCH3）CH=NNHCSNH2, in a mixed solvent of ethanol, water and DMSO yields the mononuclear dioxovanadate（V） complex, [（C2H5）4N][V（V）O2 （OC6H3- （OCH3）CHNNCSNH2）](H2O （C17H31N4O5SV, Mr = 454.5） and its single-crystal structure has been determined by X-ray diffraction. The crystal belongs to orthorhombic space group P212121 with unit cell parameters a = 12.940（3）, b= 15.414（3）, c = 10.703（2） ?, V = 2134.8（11） ?3, Z=4, Dcalc = 1.414 Kg/m3, ( = 0.597 mm-1, and F（000） = 960. The final agreement factors are R = 0.076 and Rw=0.096 for 1600 observed independent reflections with F ≥4.0(（F）. The structure revealed that the vanadium atom is bound to two terminal oxygen atoms and one tridentate donor ligand in a distorted square pyramidal arrangement. The sulphur-nitrogen-oxygen donor Schiff-base ligand in the thiol form rather than the thione form is coordinated to the vanadium via the mercapto sulphur, the (-nitrogen and the hydroxylate oxygen.
基金Projects(2016YFB07014042016YFB0701301)supported by the National Key Research and Development Program of China。
文摘This paper focused on the crystal structures of two new ternary phases,Ti(Cu,Pt)2 and Ti(Cu,Pt)3,which were studied by X-ray powder diffraction data using Rietveld method.Electron probe microanalysis was used for sample composition examination.Elastic properties of these phases were further measured by nano-indentation,and meanwhile calculated with first-principle(FP)calculations.It is found that the crystal structure of Ti(Cu,Pt)2 is of orthorhombic cell space group Amm2(No.38)with structural prototype of VAu2.The resolved structure of Ti(Cu,Pt)3 is of tetragonal Al Pt3 type,belonging to the space group P4/mmm(No.123).The nano-indentation measurement and FP calculations show that the elastic modulus of Ti(Cu,Pt)2 increases firstly then decreases with Pt content,whereas that of Ti(Cu,Pt)3almost linearly increases with Pt content.
文摘Grain growth of nanostructured Al6061produced by cryorolling and aging process was investigated during isothermalheat treatment in100?500°C temperature range.Transmission electron microscopy(TEM)observations demonstrate that aftercryorolling and aging at130°C for30h,the microstructure contains61nm grains with dispersed50?150nm precipitates and0.248%lattice strain.In addition,an increase in tensile strength up to362MPa because of formation of fine strengtheningprecipitation and nano-sized grains was observed.Thermal stability investigation within100?500°C temperature range showedrelease of lattice strain,dissolution of precipitates and grain growth.According to the X-ray diffraction(XRD)analysis,Mg2Siprecipitates disappeared after annealing at temperatures higher than300°C.According to the results,due to the limited grain growthup to200°C,there would be little decrease in mechanical properties,but within300?500°C range,the grain growth,dissolution ofstrengthening precipitates and decrease in mechanical properties are remarkable.The activation energies for grain growth werecalculated to be203.3kJ/mol for annealing at100?200°C and166.34kJ/mol for annealing at300?500°C.The effect ofprecipitation dissolution on Al lattice parameter,displacement of Al6061(111)XRD peak and Portevin?LeChatelier(PLC)effect onstress?strain curves is also discussed.
文摘Development of inhomogeneous deformation is an interest matter in material engineering. Synchrotron radiation tomography provides 3D distribution map of local strain in polycrystalline aluminum alloy by tracking microstructural features. To perform further deep analysis on development of inhomogeneous deformation, crystallographic grain orientation is necessary. Three-dimensional X-ray diffraction technique was developed. A new crystallographic orientation measurement method was described in 3D space, utilizing grain boundary tracking （GBT） information.
文摘CaCO3 was chosen as main raw material and Solid State method was used to prepare the sample. The precursor was directly sintered at 1100 ℃ with reducing atmosphere for 3 h to obtain new green CaO：Tb^3＋, Li^＋ Phosphors. The effects of the content of the doping ions Tb^3＋ on the luminescent properties have been studied. The structure, morphology and luminescent properties of the phosphors were characterized by XRD, SEM, UV and PL-PLE spectra respectively. The results showed that the CaO：Tb^3＋, Li^＋ was a single face-centered cubic crystals, the phosphor particle distributed uniformly. The phosphor has a strong absorptive capacity excited by 282 nm ultraviolet ray, and could emit the strong green light with the wavelength of 543 nm （^5D4→^7F5）. The CaO：Tb^3＋, Li^＋ is a new type of green fluorescent material.
文摘Organic semiconductoe 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA) has been synthetized with 1,8-naphthalic anhydride using chemical method.X-ray diffraction spectrum shows that it is monoclinic.Visible absorption spectrum shows that its gap band is 2.2 eV with singlet exciton bandwidth of 0.9 eV.
基金the Innovative Project (No.IP01007), the Introduction of Overseas Elitists Program (No. IB990168) and the Chinese Academy of Sciences
文摘A new compound containing discrete cationic and anionic complexes, [Cu(pyr)3]Hg2I6 (C30H24CuHg2I6N6), where pyr = 2,2-bipyridine, was prepared by the reaction of CuBr with pyr and HgI2 in a mixed solvent of acetone, methanol and acetonitrile. Single-crystal X-ray diffraction analysis indicates that it crystallizes in an orthorhombic system, Pna21 (No. 33), a = 33.1595(7), b = 9.4605(1), c = 13.0899(2) ? V = 4106.4(1) 3, Mr = 1694.67, Dc = 2.741 g/cm3, Z = 4, F(000) = 3012, m(MoKa) = 12.511 mm-1, R = 0.0736, wR = 0.1360 (I > 2(I)) and S = 1.218. The structure consists of discrete [Hg2I6]2- anions and [Cu(bipyridine)3]2+ cations. The double tetrahedral [Hg2I6]2- unit is formed by sharing one tetrahedral edge and possesses approximate D2h symmetry. The mononuclear Cu2+ ion is coordinated by six N atoms from three pyr molecules to form a slightly disordered octahedral geometry.
基金The project was supported by the National Natural Science of China(No.59972037)Natural Science Foundation of Fujian province(A0110018)
文摘The crystal of Nd(0.06)Y(0.94)S(r)6Sc(BO3)(6) with the dimensions up to 35 mm x 28 mm x 13 mm was grown by a top-seeded solution growth method from Li6B4O9 flux. The grown crystal was characterized by X-ray powder diffraction. The optical absorption of the crystal shows that it has a strong absorption band at 8070 Angstrom, and the absorption coefficient is 2.17cm(-1) with a FWHM of 41 Angstrom, which can match with the wavelength of the diode-laser (LD) and is suitable for the LD pumping. Based on the Judd-Ofelt theory, the three parameters of line oscillator strength Omega((lambda)) (lambda = 2, 4 and 6) of the Nd3+ ion in the crystal were calculated as follows: Omega(2) = 1.194 x 10(-20), Omega(4) = 4.186 x 10(-20) and Omega(6) = 3.351 x 10(-20) cm(2), Which are relatively larger. The results indicate that the crystal Nd0.06Y0.94Sr6Sc(BO3)(6) may be a kind of high-efficient laser material for diode-pumped.
基金This research was supported by the grants of the State Key Laboratory of Structural Chemistry the National misistry of science and technology of china (001CB1089)+1 种基金 the Chinese academy of sciences(CAS) the national Science Foundation of china (2027
文摘Two new inclusion 1,4-butylenediphosphonates with three-dimensional hydrogen- bonded frameworks have been synthesized and determined by single-crystal X-ray diffraction. In compound 1, the two-dimensional cationic substructures interpenetrate into the anionic framework, and in compound 2, the cations are encapsulated in the three-dimensional framework. Crystal 1 (C14H24N2O8P2) belongs to triclinic, space group P?with a = 9.4645(2), b = 9.6490(2), c = 11.9479(3) ? = 79.7420(10), b = 73.5650(10), = 63.8420(10), V = 937.55(4) 3, Z = 2, Mr = 410.29, Dc = 1.453 g/cm3, m(MoKa) = 0.276 mm-1, F(000) = 432, the final R = 0.0465 and wR = 0.1304 for 3274 independent reflections. Crystal 2 (C18H26N2O10P2) is of monoclinic, space group P21/c with a = 9.7069(12), b = 16.227(2), c = 6.9339(9) ? b = 98.834(3), V = 1079.2(2) ?, Z = 2, Mr = 492.35, Dc = 1.515 g/cm3, m(MoKa) = 0.261 mm-1, F(000) = 516, the final R = 0.0611 and wR = 0.1162 for 1871 independent reflections.
基金The project was supported by the state key laboratory of Suzhou University and the foundation of Science Committee of Jiangsu Province
文摘A new ligand 1,4-bis(2-hydroxymethylphenyl)-1,4-dioxabutane was synthesized by reducing 1,4-bis(2-formylphenyl)-1,4-dioxabutane with NaBH4 in absolute methanol solution. The crystal structure of the title compound C16H18O4 has been determined by single-crystal X-ray diffraction. The ligand crystallizes in the orthorhombic system, space group Pbcn with a = 13.777(1), b = 11.731(1), c = 9.076(8) ? V = 1466.8(2) ?, Mr = 274.30, Z = 4, F(000) = 548, Dc = 1.24 g/cm3, T = 293 K, m = 8.9 cm-1 and l = 0.71073 ? The structure was refined to R = 0.0324 and wR = 0.1025 for 1112 observed reflections with I > 2s(I). The two benzene rings are not on the same plane, and the dihedral angle between them is 60.6? The ligand has C2 symmetry axis which passes through the center of C(8)C(8a). The molecules are linked to each other by hydrogen bonding network to form supramolecular chain. The ligands connect to each other through the hydrogen bonds to form one-dimensional chains which further connect through the hydrogen bonds to form two- and three-dimensional structures.
