The title complex was synthesized in an aqueous solution at pH=3. 5,and its crystal structure was determined by X-ray diffraction methods. The com-plex is triclinic with space group P1, formula C30H66O42N6Cl6ErY, Mr,=...The title complex was synthesized in an aqueous solution at pH=3. 5,and its crystal structure was determined by X-ray diffraction methods. The com-plex is triclinic with space group P1, formula C30H66O42N6Cl6ErY, Mr,= 1651. 76, a=9. 860(2), b=13. 020(5), c= 13. 632(5) A ; a= 109. 32(3), β=110. 19(2), γ=100. 96(2)°, V= 1456(1 ) A3, Dc= 1. 884 g/cm3, Z= 1, F(000) =833, P= 2. 812mm-1 ;R=0. 046, wR(F2) =0. 123 for 4897 reflections with I>2(I). The complexis of an infinite chain structure with the neibouring metal ions connected by two bridging carboxyl groups from two different proline molecules. The erbium ion and the yttrium ion statistically lies at the position of the metal ion with M=1/2(Er+Y).展开更多
The crystat structure of {[Er;(L—Glu);(H;O);](ClO;);·3H;O);has been studied by X-ray diffraction. The crystal is monoctinic with space group P2;and cell parameters a=19.987(3) , b=16.505(3) , c=11.040...The crystat structure of {[Er;(L—Glu);(H;O);](ClO;);·3H;O);has been studied by X-ray diffraction. The crystal is monoctinic with space group P2;and cell parameters a=19.987(3) , b=16.505(3) , c=11.040(2) , β=104.69(1);, V=3538(1) , Z=2, Dc=2.29 g. cm;, μ=53.2 cm;, F(000)=2384. The asymmetric unit contains two complex motecules and four centre ions. Each erbium (Ⅲ) is coordinated by five oxygen donors from four different glutamates and four oxygen donors from the aqua ligand to form a nine coordination potyhedron. The mean distances of Er—0 (carboxylate) and Er—Ow are 2.439 and 2.41 respectivety. The finat R and Rw are 0.043 and 0. 058, respectivety.展开更多
The formation of ( t BuCp) 2ErOEt was discussed. Its single crystal structure was determined by X ray diffraction. The crystal is monoclinic, P 2(1)/ c space group, a =1.0191(2), b =1.6203(5), c ...The formation of ( t BuCp) 2ErOEt was discussed. Its single crystal structure was determined by X ray diffraction. The crystal is monoclinic, P 2(1)/ c space group, a =1.0191(2), b =1.6203(5), c =1.2118(3) nm, β =102.960(10)°, V =1.9500 (nm 3), Z =2, D c=1.566 mg·m -3 , R =0.0450, R w=0.1363. The complex is monomeric and solvent free in the solid state. The erbium ion is coordinated by two tert butyl cyclopentadienyl rings and one oxygen atom of ethoxy group to form a seven coordinated complex.展开更多
Two new polymeric erbium(Ⅲ) complexes of two flexible double betaine ligands have been synthesized and characterized by X-ray analysis. In {[Er(L1)(H2O)4)Cl3 H2O}n (1) (L1 = 4, 4’ -trimethylenedipyridinio-N, N’-dia...Two new polymeric erbium(Ⅲ) complexes of two flexible double betaine ligands have been synthesized and characterized by X-ray analysis. In {[Er(L1)(H2O)4)Cl3 H2O}n (1) (L1 = 4, 4’ -trimethylenedipyridinio-N, N’-diacetate ), the erbium(Ⅲ) ions form a two-dimensional metal carboxylate layer in which each pair of Er(Ⅲ) atoms is bridged by two syn-anti μ-carboxylato-o,o’ groups, Adjacent layers arecross-linked through hydrogen bonds among aqua ligands, lattice water molecules andchloride ions to form a three-dimensional network. Complex l, C17 H28 N2 O9 ErC13 (Mr =676.0) is monoclinic, space group C2, with a= 27. 408(4), b= 9. 645 (3), c= 9. 423(2) A, p=1loo. 85(1)’, V=2446. 2(9) A’, Z=4, D=l. 836 g/cm’, F(OOO) =1332, μ(MoKa) = 38.06 cm-1, R=0. 048 for 2451 reflections with I>2σ(I). { [Er(L2 ) (H2O)4]Cl3. 5H2O}. (2) (L2=1, 3-bis (pyridinio-4-carboxylato) propane) comprises lanthanide carboxylate chains built from centrosymmetric dimeric units crosslinked by a pair of L2 ligands, discrete anions and lattice water molecules. In the dimeric unit of complex 2, each pair of metal ions is bridged by four syn-syn μ-carboxylatoO, O’ groups that are oriented nearly perpendicular to each other about the metal-metalaxis. The metal carboxylate chains of complex 2 are further cross-linked by hydrogenbonds to form a three-dimensional network. Complex 2, C15 H32 N2O13 ErCl3 (Mr=722.0) belongs to the monoclinic space group C2/m with a=16. 564 (3), b=15. 839(3), c=11. 792(4) , β=122. 27(1)°, V=2616(1), Z=4, Dc=1.833 g/cm3,F(000) =1436, μ (MoKa) = 35. 75 cm-1, R =0.043 for 2436 observed reflectionswithI>2σ(I).展开更多
The title complex was synthesized in an aqueous solution and its crystal structure was determined by Xray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a= 1.306 3(2) nm , b=1....The title complex was synthesized in an aqueous solution and its crystal structure was determined by Xray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a= 1.306 3(2) nm , b=1.319 4(4) nm, c=1.950 2(4) nm, α=90.597(14)°, β= 93.998(11)° , γ=94.093(13)°, V=3.344 1(12) nm3, Z=2, the final R indices are R 1= 0.065 4 , wR 2=0.126 2 respectively. The complex contains a novel tetranuclear cluster cation with four Er 3+ ions connected by four μ 3OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ 3OH, three carboxylic oxygen atoms from three αalanine and two oxygen atoms from water molecules, forming a squareantiprismatic coordination polyhedron.展开更多
The title complex was synthesized in aqueous solution, and its crystal structure was determined by X ray diffraction. The crystal is triclinic space group P 1 with a =1 00935(9) nm, b =1 20190(2) nm, c ...The title complex was synthesized in aqueous solution, and its crystal structure was determined by X ray diffraction. The crystal is triclinic space group P 1 with a =1 00935(9) nm, b =1 20190(2) nm, c =1 28432(8) nm, α =95 013(9)°, β =102 814(5)°, γ =113 368(9)°, V =1 3676(3) nm 3, Z =1, D c=1 962 g/cm 3. The complex is a dimeric molecule with four bridging carboxyl groups from four valine molecules between two erbium ions. Each erbium ion is coordinated by four oxygen atoms from four carboxyl groups and four oxygen atoms of four water molecules with the coordination number 8, taking a square antiprism arrangement.展开更多
The title complex [Er_2 (His·H ̄+)_4 (H_2O)_8] (ClO_4)_(10)·4H_2O was synthesized in aqueous solution and its crystal structure was determined by X ray diffraction method. The crystal is triclinic, space gro...The title complex [Er_2 (His·H ̄+)_4 (H_2O)_8] (ClO_4)_(10)·4H_2O was synthesized in aqueous solution and its crystal structure was determined by X ray diffraction method. The crystal is triclinic, space group P1 with a=1.1726(2) nm, b=1.2660(3) nm, c=1.3142(3) nm, a=82. 92(3)°,β=70. 86(3)°, γ=83.06(3)°, V=1. 8223(7) nm ̄3, Z=1, Dc=1.977g/cm ̄3. The complex was a binuclear molecule, and each erbium ion is coordinated by four carboxylic oxygen atoms from four histidine and four oxygen atoms from H_2O, forming a coordination polyhedron of square antiprism. The structure analysis and specific rotation determination shows that the crystal contains enantiomers.展开更多
The title complex [ErY(Gly)_6(H_2O)4](ClO_4)_6·51H_2O has been synthesized.Its crystal structure has been determined by X-ray diffraction method.The crystal is triclinic with space group P.The unit cell parameter...The title complex [ErY(Gly)_6(H_2O)4](ClO_4)_6·51H_2O has been synthesized.Its crystal structure has been determined by X-ray diffraction method.The crystal is triclinic with space group P.The unit cell parameters are as follows:a=1.1518(4) nm,b=1.4105(7) nm,c=1.5530(6) nm,α=96.61(3)°,β=102.74(3)°, γ=105.70(3)°,V=2.3277(17) nm^3,Z=2,D_(calc)=2.091 g/cm^3.The structure has been refined to a final R of 0.0785.The crystal-is an infinite chain complex,in which four carboxyl groups from glycine molecules bridge the Er^(3+) and Y^(3+) ions,and the other two carboxyl groups bridge two adjacent Er^(3+) or Y^(3+) ions.展开更多
A new Mn2Ni2 cubane complex has been synthesized and characterized by single-crystal X-ray diffraction,FT IR spectra and elemental analysis.The title compound [MnIII2NiII2(hmp)4(N3)4(O2CR)2](hmp-is the anion of...A new Mn2Ni2 cubane complex has been synthesized and characterized by single-crystal X-ray diffraction,FT IR spectra and elemental analysis.The title compound [MnIII2NiII2(hmp)4(N3)4(O2CR)2](hmp-is the anion of 2-pyridinemethanol and O2CR-is α-na-phthaleneacetate)crystallizes in the monoclinic system,space group P21/c with a = 10.519(5),b = 22.109(10),c = 23.235(9),β = 106.096(17)o,C48H42Mn2N16Ni2O8,Mr = 1198.28,V = 5192(4)3,Dc = 1.533 g/cm3,F(000)= 2448,μ = 1.258 cm1,Z = 4,the final R = 0.0875 and wR = 0.2020 for 3398 reflections with I 2σ(I).X-ray diffraction analysis reveals that each Mn(III)center is octahedrally coordinated by two nitrogen atoms of azide anions and three oxygen atoms from three 2-pyridinemethanol anion ligands together with one oxygen atom from naphthaleneacetate.Each Ni(II)is octahedrally coordinated by two nitrogen atoms of 2-pyridinemethanol anion ligands as well as three oxygen atoms from three 2-pyridinemethanol anion ligands and one oxygen atom from naphthaleneacetate.展开更多
A cubane-type molybdenum cluster compound Mo4S4(DTP)4[-SOP(OEt)2]2 A (DTP = diethyl dithiophosphate) was obtained from the reaction of cation [Mo3O2S2(H2O)9]4+ B with metal tin as well as HDTP. The crystal structure h...A cubane-type molybdenum cluster compound Mo4S4(DTP)4[-SOP(OEt)2]2 A (DTP = diethyl dithiophosphate) was obtained from the reaction of cation [Mo3O2S2(H2O)9]4+ B with metal tin as well as HDTP. The crystal structure has been determined by X-ray crystallography and the data for the title compound: Mo4S14P6O14C24H60, triclinic P , Mr = 1591.14, a = 12.5596(5), b = 14.3441(5), c = 18.0005(6) ? = 85.318(1), = 70.495(1), = 78.415(2)? V = 2994.2(2) ?, Z = 2, Dc = 1.765 g/cm3, (MoK? = 1.515 mm-1, F(000) = 1596, R = 0.0918 and wR = 0.1908 for 3546 reflections (I > 2(I)). X-ray analysis reveals that two weak CH贩稯 hydrogen bonds exist in the packing diagram with C贩稯 distance 3.22(5) ? The structure of A is similar to that of -Mo4S4(DTP)6 except that one sulfur of each bridging DTPs has been replaced by oxygen during the reaction, resulting in two bridging [SOP(OEt2)2] - ligands.展开更多
The synthesis, X-ray crystal structure, thermal properties and electrochemistry of the new complex formulated as {Er(DMSO)7}PW12O40 are reported. The single-crystal X-ray analysis reveals that the crystal crystalliz...The synthesis, X-ray crystal structure, thermal properties and electrochemistry of the new complex formulated as {Er(DMSO)7}PW12O40 are reported. The single-crystal X-ray analysis reveals that the crystal crystallizes in the monoclinic system, space group P21/c with a=11.767(2), b=14.909(3), c=34.905(7)A, β=98.97(3)°, Mr=3591.33, V=6049(2)A^3, Dc=3.944g/cm^3, Z=4, GOOF=1.098, F(000)=6340, R=0.0490 and wR=0.1202. Crystal structure analysis indicates that the Er(Ⅲ) is seven-coordinate with a distorted pentagonal bipyramid and combines to the anion [PW12O40]3- via static electric force.展开更多
The title complex was synthesized in an aqueous solution and its crystal structure was determined by Xray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a= 1.306 3(2) nm , b=1....The title complex was synthesized in an aqueous solution and its crystal structure was determined by Xray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a= 1.306 3(2) nm , b=1.319 4(4) nm, c=1.950 2(4) nm, α=90.597(14)°, β= 93.998(11)° , γ=94.093(13)°, V=3.344 1(12) nm3, Z=2, the final R indices are R 1= 0.065 4 , wR 2=0.126 2 respectively. The complex contains a novel tetranuclear cluster cation with four Er 3+ ions connected by four μ 3OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ 3OH, three carboxylic oxygen atoms from three αalanine and two oxygen atoms from water molecules, forming a squareantiprismatic coordination polyhedron.展开更多
The title compound (2S,2'S,4'R)-2-(1-hydroxy-1-ethylpropyl)-1-[(1'-p-tosyl-4'- hydroxypyrolidin-2'-yl)methyl]pyrrolidine synthesized by using (2S,4R)-4-hydroxy-L-proline and L-proline as the main material...The title compound (2S,2'S,4'R)-2-(1-hydroxy-1-ethylpropyl)-1-[(1'-p-tosyl-4'- hydroxypyrolidin-2'-yl)methyl]pyrrolidine synthesized by using (2S,4R)-4-hydroxy-L-proline and L-proline as the main materials was characterized through IR, ^1H NMR, ^13C NMR and HRMS spectra as well as single-crystal X-ray diffraction analysis. There is one equivalent ethanol involved in the crystal (C23H40N2O5S, Mr = 456.63). The crystal belongs to the triclinic system, space group P1, a = 6.5628(13), b = 8.4228(17), c = 11.957(2)°A, α= 80.54(3),β= 83.19(3), γ= 89.89(3)°, V= 647.3(2) °A^3, Z = 1, D, = 1.171 g/cm^3, λ(MoKα) = 0.71073°A,β = 0.158 mm^-1, F(000) = 248, the final R = 0.0465 and wR = 0.1336 for 1769 observed reflections with I〉 2σ(I). The adjacent molecules of compound 5 are linked through intermolecular hydrogen bonds formed by the secondary hydroxy group of one molecule with the tertiary hydroxy group of another one, and the molecular chains are further linked by ethanol through two kinds of hydrogen bonds with two molecules from different chains respectively to form a supramolecular structure.展开更多
The title compound 1-(N-tert-butyloxycarbonyl-L-prolyl)-1,3-dicyclohexylurea formed in the coupling reaction of N-Boc-L-proline and n-butyl amine activated by DCC as an unexpected product was characterized through I...The title compound 1-(N-tert-butyloxycarbonyl-L-prolyl)-1,3-dicyclohexylurea formed in the coupling reaction of N-Boc-L-proline and n-butyl amine activated by DCC as an unexpected product was characterized through IR,1H NMR,13C NMR and HRMS spectra as well as single-crystal X-ray diffraction analysis.The crystal(C23H39N3O4,Mr = 421.57) belongs to the orthorhombic system,space group P212121,a = 10.8990(5),b = 12.2153(6),c = 18.8102(9) ,V = 2504.3(2) 3,Z = 4,Dc = 1.118 g/cm3,λ(MoKα) = 0.71073 ,μ = 0.076 mm-1,F(000) = 920,the final R = 0.0572 and wR = 0.1521 for 3564 observed reflections with I 〉 2σ(I).An intramolecular hydrogen bond N(3)-H…O(2) is observed.展开更多
The title compound(C25H16Cl2N3O3S),as a thiopyran derivative,has been synthe-sized by the cyclization of an organic intermediate obtained from Baylis-Hillman adducts with a β-aroylthioamide using copper(I) salt a...The title compound(C25H16Cl2N3O3S),as a thiopyran derivative,has been synthe-sized by the cyclization of an organic intermediate obtained from Baylis-Hillman adducts with a β-aroylthioamide using copper(I) salt as the catalyst.The crystal belongs to the monoclinic system,space group P21/c with a = 13.668(3),b = 8.4803(17) c = 21.999(4) ,β = 113.57(3)°,V = 2337.2(10) 3,Z = 4,Mr = 510.38,Dc = 1.451 g/cm3,μ = 0.401 mm-1,F(000) = 1048,the final R = 0.0487 and wR = 0.1079 for 3678 observed reflections with I〉 2σ(I).展开更多
A nutritional fortifier N-(1-(phenylacetyl)-L-prolyl)glycine ethyl ester(4)was successfully synthesized through two synthetic schemes and characterized by IR,^1H-NMR,^13C-NMR,elemental analysis and X-ray single-crysta...A nutritional fortifier N-(1-(phenylacetyl)-L-prolyl)glycine ethyl ester(4)was successfully synthesized through two synthetic schemes and characterized by IR,^1H-NMR,^13C-NMR,elemental analysis and X-ray single-crystal diffraction.The intermediate N-phenylacetyl-L-proline(2)was synthesized by the solid-liquid reaction of L-proline and phenylacetyl chloride directly.Compound 2(C13 H15 NO3,Mr=233.26)belongs to the orthorhombic system,space group P212121 with a=8.9468(3),b=9.3190(3),c=14.0453(4)A,V=1171.03(6)A^3,Z=4,Dc=1.323 g/cm^3,μ=0.773 mm^-1,F(000)=496.0,the final R=0.0313 and wR=0.0797 for all data.Compound 4(C17 H22 N2 O4,Mr=318.36)is of orthorhombic system,space group P212121 with a=6.5831(2),b=8.5536(2),c=28.9138(9)A,V=1628.11(8)A^3,Z=4,Dc=1.299 g/cm3,μ=0.763 mm-1,F(000)=680.0,the final R=0.0353 and wR=0.0816 for all data.展开更多
Reaction of [(ButCp)2Er(μ-Cl)]2 with ButLi in 1:1 molar ratio in THF at –78℃, after work-up, afforded the trimetallic erbium tetrahydride complex [Li(THF)4][{(ButCp)2Er(μ-H)}3 (μ3-H)] (1) by [β-hydrogen eliminat...Reaction of [(ButCp)2Er(μ-Cl)]2 with ButLi in 1:1 molar ratio in THF at –78℃, after work-up, afforded the trimetallic erbium tetrahydride complex [Li(THF)4][{(ButCp)2Er(μ-H)}3 (μ3-H)] (1) by [β-hydrogen elimination reaction. Crystal structure determination reveals that complex 1 has discrete ion pair structure. The anion is composed of three (ButCp)2Er units to form a triangle array connected by three bridged hydrogen atoms, and the fourth hydrogen atom coordinated to three Er3+ ions. The coordination num-ber for each Er3+ ion is 9.展开更多
A new tripodal ligand, N, N, N′, N′, N″, N″ hexaisopropyl 2, 2′, 2″ nitrilotris (2,1 ethoxy) triacetamide (L) and its new erbium picrate complex were prepared. The structure of the complex was determined by...A new tripodal ligand, N, N, N′, N′, N″, N″ hexaisopropyl 2, 2′, 2″ nitrilotris (2,1 ethoxy) triacetamide (L) and its new erbium picrate complex were prepared. The structure of the complex was determined by X ray crystal structure analysis. The result reveals that the Er 3+ is encapsulated by the three arms of the tripodal ligand, and nine coordinated by the bridged head nitrogen atom, all ether oxygen atoms and carbonyl oxygen atoms of the ligand, and two oxygen atoms of the bidentate picrate. The coordination polyhedron is a distorted mono-capped square antiprism.展开更多
The tetranuclear cubane-like complex, [NiL(EtOH)]4·0.5EtOH (1) with tridentate Schiff base ligand (H2L= 2-Hydroxymethyl-N-salicylideneaniline) has been synthesized and its crystal structure and spectroscopi...The tetranuclear cubane-like complex, [NiL(EtOH)]4·0.5EtOH (1) with tridentate Schiff base ligand (H2L= 2-Hydroxymethyl-N-salicylideneaniline) has been synthesized and its crystal structure and spectroscopic properties have been studied. The complex consists of a tetranuclear (NiO)4 cubane core, of which four nickel(Ⅱ) ions are bridged by μ3-alkoxide group and each nickel(Ⅱ) ion is coordinated to three μ3-alkoxide oxygen atoms, one imino nitrogen atom and one phenoxide oxygen atom from Schiff base ligand, and further ligated by one EtOH molecule, completing a distorted octahedral geometry.展开更多
文摘The title complex was synthesized in an aqueous solution at pH=3. 5,and its crystal structure was determined by X-ray diffraction methods. The com-plex is triclinic with space group P1, formula C30H66O42N6Cl6ErY, Mr,= 1651. 76, a=9. 860(2), b=13. 020(5), c= 13. 632(5) A ; a= 109. 32(3), β=110. 19(2), γ=100. 96(2)°, V= 1456(1 ) A3, Dc= 1. 884 g/cm3, Z= 1, F(000) =833, P= 2. 812mm-1 ;R=0. 046, wR(F2) =0. 123 for 4897 reflections with I>2(I). The complexis of an infinite chain structure with the neibouring metal ions connected by two bridging carboxyl groups from two different proline molecules. The erbium ion and the yttrium ion statistically lies at the position of the metal ion with M=1/2(Er+Y).
文摘The crystat structure of {[Er;(L—Glu);(H;O);](ClO;);·3H;O);has been studied by X-ray diffraction. The crystal is monoctinic with space group P2;and cell parameters a=19.987(3) , b=16.505(3) , c=11.040(2) , β=104.69(1);, V=3538(1) , Z=2, Dc=2.29 g. cm;, μ=53.2 cm;, F(000)=2384. The asymmetric unit contains two complex motecules and four centre ions. Each erbium (Ⅲ) is coordinated by five oxygen donors from four different glutamates and four oxygen donors from the aqua ligand to form a nine coordination potyhedron. The mean distances of Er—0 (carboxylate) and Er—Ow are 2.439 and 2.41 respectivety. The finat R and Rw are 0.043 and 0. 058, respectivety.
文摘The formation of ( t BuCp) 2ErOEt was discussed. Its single crystal structure was determined by X ray diffraction. The crystal is monoclinic, P 2(1)/ c space group, a =1.0191(2), b =1.6203(5), c =1.2118(3) nm, β =102.960(10)°, V =1.9500 (nm 3), Z =2, D c=1.566 mg·m -3 , R =0.0450, R w=0.1363. The complex is monomeric and solvent free in the solid state. The erbium ion is coordinated by two tert butyl cyclopentadienyl rings and one oxygen atom of ethoxy group to form a seven coordinated complex.
文摘Two new polymeric erbium(Ⅲ) complexes of two flexible double betaine ligands have been synthesized and characterized by X-ray analysis. In {[Er(L1)(H2O)4)Cl3 H2O}n (1) (L1 = 4, 4’ -trimethylenedipyridinio-N, N’-diacetate ), the erbium(Ⅲ) ions form a two-dimensional metal carboxylate layer in which each pair of Er(Ⅲ) atoms is bridged by two syn-anti μ-carboxylato-o,o’ groups, Adjacent layers arecross-linked through hydrogen bonds among aqua ligands, lattice water molecules andchloride ions to form a three-dimensional network. Complex l, C17 H28 N2 O9 ErC13 (Mr =676.0) is monoclinic, space group C2, with a= 27. 408(4), b= 9. 645 (3), c= 9. 423(2) A, p=1loo. 85(1)’, V=2446. 2(9) A’, Z=4, D=l. 836 g/cm’, F(OOO) =1332, μ(MoKa) = 38.06 cm-1, R=0. 048 for 2451 reflections with I>2σ(I). { [Er(L2 ) (H2O)4]Cl3. 5H2O}. (2) (L2=1, 3-bis (pyridinio-4-carboxylato) propane) comprises lanthanide carboxylate chains built from centrosymmetric dimeric units crosslinked by a pair of L2 ligands, discrete anions and lattice water molecules. In the dimeric unit of complex 2, each pair of metal ions is bridged by four syn-syn μ-carboxylatoO, O’ groups that are oriented nearly perpendicular to each other about the metal-metalaxis. The metal carboxylate chains of complex 2 are further cross-linked by hydrogenbonds to form a three-dimensional network. Complex 2, C15 H32 N2O13 ErCl3 (Mr=722.0) belongs to the monoclinic space group C2/m with a=16. 564 (3), b=15. 839(3), c=11. 792(4) , β=122. 27(1)°, V=2616(1), Z=4, Dc=1.833 g/cm3,F(000) =1436, μ (MoKa) = 35. 75 cm-1, R =0.043 for 2436 observed reflectionswithI>2σ(I).
基金Supported by the National Key Project of Fundamental Research and the National Natural Science Foundation ofChina(No.29771001,
文摘The title complex was synthesized in an aqueous solution and its crystal structure was determined by Xray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a= 1.306 3(2) nm , b=1.319 4(4) nm, c=1.950 2(4) nm, α=90.597(14)°, β= 93.998(11)° , γ=94.093(13)°, V=3.344 1(12) nm3, Z=2, the final R indices are R 1= 0.065 4 , wR 2=0.126 2 respectively. The complex contains a novel tetranuclear cluster cation with four Er 3+ ions connected by four μ 3OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ 3OH, three carboxylic oxygen atoms from three αalanine and two oxygen atoms from water molecules, forming a squareantiprismatic coordination polyhedron.
文摘The title complex was synthesized in aqueous solution, and its crystal structure was determined by X ray diffraction. The crystal is triclinic space group P 1 with a =1 00935(9) nm, b =1 20190(2) nm, c =1 28432(8) nm, α =95 013(9)°, β =102 814(5)°, γ =113 368(9)°, V =1 3676(3) nm 3, Z =1, D c=1 962 g/cm 3. The complex is a dimeric molecule with four bridging carboxyl groups from four valine molecules between two erbium ions. Each erbium ion is coordinated by four oxygen atoms from four carboxyl groups and four oxygen atoms of four water molecules with the coordination number 8, taking a square antiprism arrangement.
文摘The title complex [Er_2 (His·H ̄+)_4 (H_2O)_8] (ClO_4)_(10)·4H_2O was synthesized in aqueous solution and its crystal structure was determined by X ray diffraction method. The crystal is triclinic, space group P1 with a=1.1726(2) nm, b=1.2660(3) nm, c=1.3142(3) nm, a=82. 92(3)°,β=70. 86(3)°, γ=83.06(3)°, V=1. 8223(7) nm ̄3, Z=1, Dc=1.977g/cm ̄3. The complex was a binuclear molecule, and each erbium ion is coordinated by four carboxylic oxygen atoms from four histidine and four oxygen atoms from H_2O, forming a coordination polyhedron of square antiprism. The structure analysis and specific rotation determination shows that the crystal contains enantiomers.
基金The Project supported by the National Natural Science Foundation of China
文摘The title complex [ErY(Gly)_6(H_2O)4](ClO_4)_6·51H_2O has been synthesized.Its crystal structure has been determined by X-ray diffraction method.The crystal is triclinic with space group P.The unit cell parameters are as follows:a=1.1518(4) nm,b=1.4105(7) nm,c=1.5530(6) nm,α=96.61(3)°,β=102.74(3)°, γ=105.70(3)°,V=2.3277(17) nm^3,Z=2,D_(calc)=2.091 g/cm^3.The structure has been refined to a final R of 0.0785.The crystal-is an infinite chain complex,in which four carboxyl groups from glycine molecules bridge the Er^(3+) and Y^(3+) ions,and the other two carboxyl groups bridge two adjacent Er^(3+) or Y^(3+) ions.
基金Financially supported by the National Natural Science Foundation of China (No.20971063)
文摘A new Mn2Ni2 cubane complex has been synthesized and characterized by single-crystal X-ray diffraction,FT IR spectra and elemental analysis.The title compound [MnIII2NiII2(hmp)4(N3)4(O2CR)2](hmp-is the anion of 2-pyridinemethanol and O2CR-is α-na-phthaleneacetate)crystallizes in the monoclinic system,space group P21/c with a = 10.519(5),b = 22.109(10),c = 23.235(9),β = 106.096(17)o,C48H42Mn2N16Ni2O8,Mr = 1198.28,V = 5192(4)3,Dc = 1.533 g/cm3,F(000)= 2448,μ = 1.258 cm1,Z = 4,the final R = 0.0875 and wR = 0.2020 for 3398 reflections with I 2σ(I).X-ray diffraction analysis reveals that each Mn(III)center is octahedrally coordinated by two nitrogen atoms of azide anions and three oxygen atoms from three 2-pyridinemethanol anion ligands together with one oxygen atom from naphthaleneacetate.Each Ni(II)is octahedrally coordinated by two nitrogen atoms of 2-pyridinemethanol anion ligands as well as three oxygen atoms from three 2-pyridinemethanol anion ligands and one oxygen atom from naphthaleneacetate.
基金This work was financially supported by the NNSF of China (No. 29733090 and No. 20173063) Key Project in KIP of CAS (KJCX2-H3) and the NNSF of Fujian Province (E0020001)
文摘A cubane-type molybdenum cluster compound Mo4S4(DTP)4[-SOP(OEt)2]2 A (DTP = diethyl dithiophosphate) was obtained from the reaction of cation [Mo3O2S2(H2O)9]4+ B with metal tin as well as HDTP. The crystal structure has been determined by X-ray crystallography and the data for the title compound: Mo4S14P6O14C24H60, triclinic P , Mr = 1591.14, a = 12.5596(5), b = 14.3441(5), c = 18.0005(6) ? = 85.318(1), = 70.495(1), = 78.415(2)? V = 2994.2(2) ?, Z = 2, Dc = 1.765 g/cm3, (MoK? = 1.515 mm-1, F(000) = 1596, R = 0.0918 and wR = 0.1908 for 3546 reflections (I > 2(I)). X-ray analysis reveals that two weak CH贩稯 hydrogen bonds exist in the packing diagram with C贩稯 distance 3.22(5) ? The structure of A is similar to that of -Mo4S4(DTP)6 except that one sulfur of each bridging DTPs has been replaced by oxygen during the reaction, resulting in two bridging [SOP(OEt2)2] - ligands.
基金The project was supported by Henan Innovation Project for University Prominent Research Talentsthe Natural Science Foundation of Henan Province (No.0524480020)Natural Science Foundation of Henan University (No. XK04YBRW057)
文摘The synthesis, X-ray crystal structure, thermal properties and electrochemistry of the new complex formulated as {Er(DMSO)7}PW12O40 are reported. The single-crystal X-ray analysis reveals that the crystal crystallizes in the monoclinic system, space group P21/c with a=11.767(2), b=14.909(3), c=34.905(7)A, β=98.97(3)°, Mr=3591.33, V=6049(2)A^3, Dc=3.944g/cm^3, Z=4, GOOF=1.098, F(000)=6340, R=0.0490 and wR=0.1202. Crystal structure analysis indicates that the Er(Ⅲ) is seven-coordinate with a distorted pentagonal bipyramid and combines to the anion [PW12O40]3- via static electric force.
基金Supported by the National Key Project of Fundamental Research and the National Natural Science Foundation ofChina(No.29771001,
文摘The title complex was synthesized in an aqueous solution and its crystal structure was determined by Xray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a= 1.306 3(2) nm , b=1.319 4(4) nm, c=1.950 2(4) nm, α=90.597(14)°, β= 93.998(11)° , γ=94.093(13)°, V=3.344 1(12) nm3, Z=2, the final R indices are R 1= 0.065 4 , wR 2=0.126 2 respectively. The complex contains a novel tetranuclear cluster cation with four Er 3+ ions connected by four μ 3OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ 3OH, three carboxylic oxygen atoms from three αalanine and two oxygen atoms from water molecules, forming a squareantiprismatic coordination polyhedron.
基金Supported by the National Natural Science Foundation of China (No. 20372059)
文摘The title compound (2S,2'S,4'R)-2-(1-hydroxy-1-ethylpropyl)-1-[(1'-p-tosyl-4'- hydroxypyrolidin-2'-yl)methyl]pyrrolidine synthesized by using (2S,4R)-4-hydroxy-L-proline and L-proline as the main materials was characterized through IR, ^1H NMR, ^13C NMR and HRMS spectra as well as single-crystal X-ray diffraction analysis. There is one equivalent ethanol involved in the crystal (C23H40N2O5S, Mr = 456.63). The crystal belongs to the triclinic system, space group P1, a = 6.5628(13), b = 8.4228(17), c = 11.957(2)°A, α= 80.54(3),β= 83.19(3), γ= 89.89(3)°, V= 647.3(2) °A^3, Z = 1, D, = 1.171 g/cm^3, λ(MoKα) = 0.71073°A,β = 0.158 mm^-1, F(000) = 248, the final R = 0.0465 and wR = 0.1336 for 1769 observed reflections with I〉 2σ(I). The adjacent molecules of compound 5 are linked through intermolecular hydrogen bonds formed by the secondary hydroxy group of one molecule with the tertiary hydroxy group of another one, and the molecular chains are further linked by ethanol through two kinds of hydrogen bonds with two molecules from different chains respectively to form a supramolecular structure.
基金Supported by the Natural Science Foundation of China (No. 21072089)
文摘The title compound 1-(N-tert-butyloxycarbonyl-L-prolyl)-1,3-dicyclohexylurea formed in the coupling reaction of N-Boc-L-proline and n-butyl amine activated by DCC as an unexpected product was characterized through IR,1H NMR,13C NMR and HRMS spectra as well as single-crystal X-ray diffraction analysis.The crystal(C23H39N3O4,Mr = 421.57) belongs to the orthorhombic system,space group P212121,a = 10.8990(5),b = 12.2153(6),c = 18.8102(9) ,V = 2504.3(2) 3,Z = 4,Dc = 1.118 g/cm3,λ(MoKα) = 0.71073 ,μ = 0.076 mm-1,F(000) = 920,the final R = 0.0572 and wR = 0.1521 for 3564 observed reflections with I 〉 2σ(I).An intramolecular hydrogen bond N(3)-H…O(2) is observed.
基金supported by the National Natural Science Foundation of China (No. 20872074 and 21072110)the Natural Science Foundation of Shandong Province (No. Z2008B03 and ZR2010BM007)the Doctoral Foundation of Qingdao University of Science and Technology
文摘The title compound(C25H16Cl2N3O3S),as a thiopyran derivative,has been synthe-sized by the cyclization of an organic intermediate obtained from Baylis-Hillman adducts with a β-aroylthioamide using copper(I) salt as the catalyst.The crystal belongs to the monoclinic system,space group P21/c with a = 13.668(3),b = 8.4803(17) c = 21.999(4) ,β = 113.57(3)°,V = 2337.2(10) 3,Z = 4,Mr = 510.38,Dc = 1.451 g/cm3,μ = 0.401 mm-1,F(000) = 1048,the final R = 0.0487 and wR = 0.1079 for 3678 observed reflections with I〉 2σ(I).
文摘A nutritional fortifier N-(1-(phenylacetyl)-L-prolyl)glycine ethyl ester(4)was successfully synthesized through two synthetic schemes and characterized by IR,^1H-NMR,^13C-NMR,elemental analysis and X-ray single-crystal diffraction.The intermediate N-phenylacetyl-L-proline(2)was synthesized by the solid-liquid reaction of L-proline and phenylacetyl chloride directly.Compound 2(C13 H15 NO3,Mr=233.26)belongs to the orthorhombic system,space group P212121 with a=8.9468(3),b=9.3190(3),c=14.0453(4)A,V=1171.03(6)A^3,Z=4,Dc=1.323 g/cm^3,μ=0.773 mm^-1,F(000)=496.0,the final R=0.0313 and wR=0.0797 for all data.Compound 4(C17 H22 N2 O4,Mr=318.36)is of orthorhombic system,space group P212121 with a=6.5831(2),b=8.5536(2),c=28.9138(9)A,V=1628.11(8)A^3,Z=4,Dc=1.299 g/cm3,μ=0.763 mm-1,F(000)=680.0,the final R=0.0353 and wR=0.0816 for all data.
文摘Reaction of [(ButCp)2Er(μ-Cl)]2 with ButLi in 1:1 molar ratio in THF at –78℃, after work-up, afforded the trimetallic erbium tetrahydride complex [Li(THF)4][{(ButCp)2Er(μ-H)}3 (μ3-H)] (1) by [β-hydrogen elimination reaction. Crystal structure determination reveals that complex 1 has discrete ion pair structure. The anion is composed of three (ButCp)2Er units to form a triangle array connected by three bridged hydrogen atoms, and the fourth hydrogen atom coordinated to three Er3+ ions. The coordination num-ber for each Er3+ ion is 9.
文摘A new tripodal ligand, N, N, N′, N′, N″, N″ hexaisopropyl 2, 2′, 2″ nitrilotris (2,1 ethoxy) triacetamide (L) and its new erbium picrate complex were prepared. The structure of the complex was determined by X ray crystal structure analysis. The result reveals that the Er 3+ is encapsulated by the three arms of the tripodal ligand, and nine coordinated by the bridged head nitrogen atom, all ether oxygen atoms and carbonyl oxygen atoms of the ligand, and two oxygen atoms of the bidentate picrate. The coordination polyhedron is a distorted mono-capped square antiprism.
文摘The tetranuclear cubane-like complex, [NiL(EtOH)]4·0.5EtOH (1) with tridentate Schiff base ligand (H2L= 2-Hydroxymethyl-N-salicylideneaniline) has been synthesized and its crystal structure and spectroscopic properties have been studied. The complex consists of a tetranuclear (NiO)4 cubane core, of which four nickel(Ⅱ) ions are bridged by μ3-alkoxide group and each nickel(Ⅱ) ion is coordinated to three μ3-alkoxide oxygen atoms, one imino nitrogen atom and one phenoxide oxygen atom from Schiff base ligand, and further ligated by one EtOH molecule, completing a distorted octahedral geometry.