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2014 Volume 33 Issue 7
2014, 33(7): 959-970
Abstract:
Systematic study on the electronic/geometrical structures and the parity alternation effect of silicon-doped ternary cationic clusters HCnSi2+(n=1~9) have been carried out at the coupled cluster level. The ground-state (G-S) isomers of the clusters have been defined. The Cn chains of the G-S isomers display polyacetylene-like structures. The even-n cations are more stable than the odd-n ones. Such a trend of even/odd alternation has been elaborated based on concepts of the bond character, atomic charge, incremental binding energy, ionization potential, proton affinity and fragmentation energies of the systems. The findings accord with the relative intensities of HCnSi2+ species recorded in the related mass spectrometric experiments.
Systematic study on the electronic/geometrical structures and the parity alternation effect of silicon-doped ternary cationic clusters HCnSi2+(n=1~9) have been carried out at the coupled cluster level. The ground-state (G-S) isomers of the clusters have been defined. The Cn chains of the G-S isomers display polyacetylene-like structures. The even-n cations are more stable than the odd-n ones. Such a trend of even/odd alternation has been elaborated based on concepts of the bond character, atomic charge, incremental binding energy, ionization potential, proton affinity and fragmentation energies of the systems. The findings accord with the relative intensities of HCnSi2+ species recorded in the related mass spectrometric experiments.
2014, 33(7): 971-977
Abstract:
[Pb(HL)(phen)]n (1) and [Cd3L2(phen)]n (2), where phen=1,10-phenanthroline and L=4,4'-(2-carboxylatopropane-1,3-diyl)dibenzoate, were hydrothermally prepared and fully characterized by X-ray single-crystal diffraction, infrared spectroscopy and thermogravimetric analyses. The decomposition temperature of 1 and 2 was measured to be ca. 304 and 416℃, respectively. The charge transfer transition based absorption of 1 and 2 was also verified by the powder scattering spectra and theoretical analyses.
[Pb(HL)(phen)]n (1) and [Cd3L2(phen)]n (2), where phen=1,10-phenanthroline and L=4,4'-(2-carboxylatopropane-1,3-diyl)dibenzoate, were hydrothermally prepared and fully characterized by X-ray single-crystal diffraction, infrared spectroscopy and thermogravimetric analyses. The decomposition temperature of 1 and 2 was measured to be ca. 304 and 416℃, respectively. The charge transfer transition based absorption of 1 and 2 was also verified by the powder scattering spectra and theoretical analyses.
2014, 33(7): 978-984
Abstract:
A new clip molecule 1 based on diethoxycarbonyl glycoluril, C46H34Cl4N4O8, has been synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a=11.3674(8), b=11.3674(8), c=16.9704(12) Å, α=70.0690(10), β=72.2310(10), γ=78.0880(10)°, V=1993.2(2) Å3, Z=2, Dc=1.521 g/cm3, μ(MoKα)=0.361 mm-1, F(000)=940, the final R=0.0422 and wR=0.1144 for 22997 observed reflections with I>2σ(I). The crystal structural analysis shows that C-H…O and C-H…Cl hydrogen bonds, C-H…π, C-Cl…π supramolecular interactions, and π-π packing interaction stabilized the whole crystal structure. The binding study by fluorescence spectroscope titration showed that the title molecule can selectively recognize Fe3+ with fluorescence quenching.
A new clip molecule 1 based on diethoxycarbonyl glycoluril, C46H34Cl4N4O8, has been synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a=11.3674(8), b=11.3674(8), c=16.9704(12) Å, α=70.0690(10), β=72.2310(10), γ=78.0880(10)°, V=1993.2(2) Å3, Z=2, Dc=1.521 g/cm3, μ(MoKα)=0.361 mm-1, F(000)=940, the final R=0.0422 and wR=0.1144 for 22997 observed reflections with I>2σ(I). The crystal structural analysis shows that C-H…O and C-H…Cl hydrogen bonds, C-H…π, C-Cl…π supramolecular interactions, and π-π packing interaction stabilized the whole crystal structure. The binding study by fluorescence spectroscope titration showed that the title molecule can selectively recognize Fe3+ with fluorescence quenching.
2014, 33(7): 985-989
Abstract:
A new crystal of 2-methylpropan-2-aminium methyl ((4-fluorobenzamido)(4-fluorophenyl)methyl)phosphonate has been prepared at room temperature and characterized by 1HNMR, 13C NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic space group C2/c with a=20.719(2), b=11.8559(13), c=18.176(2) Å, β=94.434(2)°, V=4451.4(9) Å3, Dc=1.317 Mg/m3, Z=8, F(000)=1864 and μ=0.174 mm-1. The crystal packing is stabilized by intermolecular N-H…O and O-H…O hydrogen bonds, as well as by weak π-π stacking interactions.
A new crystal of 2-methylpropan-2-aminium methyl ((4-fluorobenzamido)(4-fluorophenyl)methyl)phosphonate has been prepared at room temperature and characterized by 1HNMR, 13C NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic space group C2/c with a=20.719(2), b=11.8559(13), c=18.176(2) Å, β=94.434(2)°, V=4451.4(9) Å3, Dc=1.317 Mg/m3, Z=8, F(000)=1864 and μ=0.174 mm-1. The crystal packing is stabilized by intermolecular N-H…O and O-H…O hydrogen bonds, as well as by weak π-π stacking interactions.
2014, 33(7): 990-994
Abstract:
A novel heterobimetallic coordination polymer, {(NH4)2[Cd(H2O)Fe(CN)6]}n 1, has been synthesized by using the slow diffusion method and structurally characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group P21/n, a=7.4202(16), b=14.939(3), c=10.868(2) Å and β=91.660(3)°. For 1, five CN groups of Fe(CN)6]4- are involved in bridging. The polymer displays a 3D open microporous framework with 5-connected uninodal (46.64) topology.
A novel heterobimetallic coordination polymer, {(NH4)2[Cd(H2O)Fe(CN)6]}n 1, has been synthesized by using the slow diffusion method and structurally characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group P21/n, a=7.4202(16), b=14.939(3), c=10.868(2) Å and β=91.660(3)°. For 1, five CN groups of Fe(CN)6]4- are involved in bridging. The polymer displays a 3D open microporous framework with 5-connected uninodal (46.64) topology.
2014, 33(7): 995-1000
Abstract:
A new complex K0.5[K(18-crown-6)]1.5Ge9·1.5en (1) which contains unprecedented "up" and "down" chain arrangement of unit [-(Ge9-K-Ge9)3--] has been prepared by the reaction of K4Ge9 with HgS in ethylenediamine (en) in the presence of 18-crown-6(1,4,7,10,13,16-hexaoxacyclooctadecane), and characterized by X-ray structure analysis. The color of the title crystals (black), which is darker than that of the reported three compounds with chains of germanium clusters, may result from the naked K+ and their interactions with the chain. And the structure differences between 1 and the reported three compounds with chains of germanium have also been discussed.
A new complex K0.5[K(18-crown-6)]1.5Ge9·1.5en (1) which contains unprecedented "up" and "down" chain arrangement of unit [-(Ge9-K-Ge9)3--] has been prepared by the reaction of K4Ge9 with HgS in ethylenediamine (en) in the presence of 18-crown-6(1,4,7,10,13,16-hexaoxacyclooctadecane), and characterized by X-ray structure analysis. The color of the title crystals (black), which is darker than that of the reported three compounds with chains of germanium clusters, may result from the naked K+ and their interactions with the chain. And the structure differences between 1 and the reported three compounds with chains of germanium have also been discussed.
2014, 33(7): 1001-1006
Abstract:
A novel metal-organic complex [La(o-NCP)3]n (o-HNCP=2-(2-carboxyphenyl)imidazo(4,5-f)(1,10)-phenanthroline) has been hydrothermally synthesized and characterized by elemental analysis, infrared analysis and X-ray single-crystal diffraction. The complex crystallizes in triclinic, space group P1 with a=9.898(2), b=16.193(3), c=16.909(3) Å, α=67.68(3), β=80.85(3), γ=78.78(3)°, V=2448.2(8) Å3, Z=2, Mr=1156.9, Dc=1.569 g/cm3, μ=0.71073 Å, F(000)=1164, GOOF=1.065, the final R=0.051 and wR=0.123 for 8539 observed reflections with I>2σ(I). The complex exhibits a one-dimensional double chain structure. The adjacent chains are further connected by N-H…N hydrogen bonds which help to form a two-dimensional supramolecular architecture. Furthermore, the complex exhibits excellent thermal stability and luminescent property.
A novel metal-organic complex [La(o-NCP)3]n (o-HNCP=2-(2-carboxyphenyl)imidazo(4,5-f)(1,10)-phenanthroline) has been hydrothermally synthesized and characterized by elemental analysis, infrared analysis and X-ray single-crystal diffraction. The complex crystallizes in triclinic, space group P1 with a=9.898(2), b=16.193(3), c=16.909(3) Å, α=67.68(3), β=80.85(3), γ=78.78(3)°, V=2448.2(8) Å3, Z=2, Mr=1156.9, Dc=1.569 g/cm3, μ=0.71073 Å, F(000)=1164, GOOF=1.065, the final R=0.051 and wR=0.123 for 8539 observed reflections with I>2σ(I). The complex exhibits a one-dimensional double chain structure. The adjacent chains are further connected by N-H…N hydrogen bonds which help to form a two-dimensional supramolecular architecture. Furthermore, the complex exhibits excellent thermal stability and luminescent property.
2014, 33(7): 1007-1012
Abstract:
A novel 1,2,3-triazolyl-containing ligand (H2L) with long donor arms extending from the central pyridyl linker was synthesized by click cycloaddition of 2,6-bis(azidomethyl)pyridine and 2-((prop-2-yn-1-yl(pyridin-2-ylmethyl)amino)methyl)phenol. Further treatment of the ligand H2L with zinc(Ⅱ) perchlorate in the presence of triethylamine, followed by anion exchange with Na[BPh4], provided a dinuclear zinc(Ⅱ) complex [Zn2L][BPh4]2·2DMF (1). Complex 1 crystallizes in monoclinic, space group P21 with a=10.4873(4), b=14.9078(5), c=25.8620(9) Å, β=94.566(2)°, V=4030.5(2) Å3, Z=2, μ=0.657 mm-1, Dc=1.324 Mg/m3, T=296(2) K, C93H91N13B2O4Zn2, Mr=1607.19, F(000)=1684, S=0.958, R=0.0271 and wR=0.0607. In the structure of cation, the phenolate oxygen atoms of ligand act as the bridging nodes to form a rhombic Zn2(OAr)2 core.
A novel 1,2,3-triazolyl-containing ligand (H2L) with long donor arms extending from the central pyridyl linker was synthesized by click cycloaddition of 2,6-bis(azidomethyl)pyridine and 2-((prop-2-yn-1-yl(pyridin-2-ylmethyl)amino)methyl)phenol. Further treatment of the ligand H2L with zinc(Ⅱ) perchlorate in the presence of triethylamine, followed by anion exchange with Na[BPh4], provided a dinuclear zinc(Ⅱ) complex [Zn2L][BPh4]2·2DMF (1). Complex 1 crystallizes in monoclinic, space group P21 with a=10.4873(4), b=14.9078(5), c=25.8620(9) Å, β=94.566(2)°, V=4030.5(2) Å3, Z=2, μ=0.657 mm-1, Dc=1.324 Mg/m3, T=296(2) K, C93H91N13B2O4Zn2, Mr=1607.19, F(000)=1684, S=0.958, R=0.0271 and wR=0.0607. In the structure of cation, the phenolate oxygen atoms of ligand act as the bridging nodes to form a rhombic Zn2(OAr)2 core.
2014, 33(7): 1013-1018
Abstract:
A new coordination compound with formula [Tb(2-TC)3(DMF)]n (1, 2-TC=2-thiophenecarboxylic ligand and DMF=dimethylformamide) was synthesized by solvothermal method. The structure of compound 1 was determined by single-crystal X-ray diffraction analyses, and characterized by elemental analyses, IR and powder X-ray diffraction. Structure analysis reveals compound 1, exhibiting a one-dimensional chain structure, crystallizes in triclinic space group P21/c, with a=9.2751(19), b=16.490(3), c=15.865(5) Å, β=118.98(2)°, V=2122.7(9) Å3, Dc=1.916 g/cm3, Mr=612.45 (C18H15NO7S3Tb), F(000)=1196, μ(MoKα)=3.67 mm-1, Z=4, R=0.0616 and wR=0.0962 for 3865 observed reflections (I>2σ(I)), and R=0.1092 for all data. Meanwhile, the photoluminescent properties of compound 1 were also investigated in the solid state at room temperature.
A new coordination compound with formula [Tb(2-TC)3(DMF)]n (1, 2-TC=2-thiophenecarboxylic ligand and DMF=dimethylformamide) was synthesized by solvothermal method. The structure of compound 1 was determined by single-crystal X-ray diffraction analyses, and characterized by elemental analyses, IR and powder X-ray diffraction. Structure analysis reveals compound 1, exhibiting a one-dimensional chain structure, crystallizes in triclinic space group P21/c, with a=9.2751(19), b=16.490(3), c=15.865(5) Å, β=118.98(2)°, V=2122.7(9) Å3, Dc=1.916 g/cm3, Mr=612.45 (C18H15NO7S3Tb), F(000)=1196, μ(MoKα)=3.67 mm-1, Z=4, R=0.0616 and wR=0.0962 for 3865 observed reflections (I>2σ(I)), and R=0.1092 for all data. Meanwhile, the photoluminescent properties of compound 1 were also investigated in the solid state at room temperature.
2014, 33(7): 1019-1024
Abstract:
The title complex [Zn8Ⅱ(4-APha)8(CH3COO)8(CH3CH2OH)2]n (1, 4-APha=4-aminophenylhydroxamic acid) has been prepared under solvothermal conditions. It has been characterized by X-ray single-crystal diffraction, IR and elemental analysis. The crystal belongs to the monoclinic system, space group C2/c with a=39.074(4), b=9.9645(8), c=38.846(3) Å, β=136.438°, V=10423.1(14) Å3, C84H118N16O39Zn8, Mr=2498.90, Z=4, Dc=1.592 g/cm3, μ=1.900 mm-1, F(000)=5144, the final R=0.1036 and wR=0.2953. This complex possesses a 3-D structure which is constructed from 1-D chain motifs linked by the 4-APha- ligands. The luminescent property of the title complex has been investigated.
The title complex [Zn8Ⅱ(4-APha)8(CH3COO)8(CH3CH2OH)2]n (1, 4-APha=4-aminophenylhydroxamic acid) has been prepared under solvothermal conditions. It has been characterized by X-ray single-crystal diffraction, IR and elemental analysis. The crystal belongs to the monoclinic system, space group C2/c with a=39.074(4), b=9.9645(8), c=38.846(3) Å, β=136.438°, V=10423.1(14) Å3, C84H118N16O39Zn8, Mr=2498.90, Z=4, Dc=1.592 g/cm3, μ=1.900 mm-1, F(000)=5144, the final R=0.1036 and wR=0.2953. This complex possesses a 3-D structure which is constructed from 1-D chain motifs linked by the 4-APha- ligands. The luminescent property of the title complex has been investigated.
2014, 33(7): 1025-1030
Abstract:
A new 3D copper(I) iodide hybrid, [Cu4I4(TMEDA)2]n (1, TMEDA=N,N,N',N'-tetramethylethylenediamine), has been solvothermally synthesized and characterized by singlecrystal X-ray diffraction, IR spectroscopy, elemental analysis, powder X-ray diffractions and thermogravimetric analysis. Compound 1 crystallizes in tetragonal space group P42/n with a=b=11.5663(7) Å, c=9.2456(11) Å, V=1236.87(18) Å3, Z=8, C3H8CuIN, Mr=248.54, Dc=3.507 g/cm3, F(000)=920, μ(MoKα)=8.388 mm-1, the final R=0.0244 and wR=0.0573 for 1118 observed reflections (I>2σ(I)). The hybrid framework is built up from cubane-like Cu4I4 cluster and flexible acyclic aliphatic diamine TMEDA, which can be simplified into a twofold interpenetrating dia network. The solid state luminescence spectrum displays a strong yellow emission band at room temperature (λex=340 nm, λem=530 nm). Results reveal that steric effect of N-substituted methyl groups in TMEDA have obvious influence on the structure and photoluminescent property of compound 1.
A new 3D copper(I) iodide hybrid, [Cu4I4(TMEDA)2]n (1, TMEDA=N,N,N',N'-tetramethylethylenediamine), has been solvothermally synthesized and characterized by singlecrystal X-ray diffraction, IR spectroscopy, elemental analysis, powder X-ray diffractions and thermogravimetric analysis. Compound 1 crystallizes in tetragonal space group P42/n with a=b=11.5663(7) Å, c=9.2456(11) Å, V=1236.87(18) Å3, Z=8, C3H8CuIN, Mr=248.54, Dc=3.507 g/cm3, F(000)=920, μ(MoKα)=8.388 mm-1, the final R=0.0244 and wR=0.0573 for 1118 observed reflections (I>2σ(I)). The hybrid framework is built up from cubane-like Cu4I4 cluster and flexible acyclic aliphatic diamine TMEDA, which can be simplified into a twofold interpenetrating dia network. The solid state luminescence spectrum displays a strong yellow emission band at room temperature (λex=340 nm, λem=530 nm). Results reveal that steric effect of N-substituted methyl groups in TMEDA have obvious influence on the structure and photoluminescent property of compound 1.
2014, 33(7): 1031-1036
Abstract:
Three homoleptic lanthanide complexes, [C6H5COCHC(CH3)N(p-ClC6H4)]3Ln(THF)n (n=0, Ln=Yb (1); n=0, Ln=Y (2); n=1, Ln=Nd (3)), were synthesized by amine elimination reaction of Ln[N(SiMe3)2]3 with 1-phenyl-3-N-(p-chlorophenylimino)-1-butanone. These complexes crystallize in triclinic, space group P1 with a=9.805(3), b=14.831(6), c=16.075(6) Å, α=111.996(9), β=91.570(7), γ=93.744(6)°, V=2159.4(13) Å3, Z=2, Dc=1.515 g/cm3, F(000)=986, μ(MoKα)=2.396 mm-1, R=0.0360 and wR=0.0850 for 9548 observed reflections with I>2σ(I) for complex 1; a=9.861(5), b=14.852(9), c=16.111(9) Å, α=112.362(13), β=91.949(11), γ=93.678(14)°, V=2173(2) Å3, Z=2, Dc=1.377 g/cm3, F(000)=924, μ(MoKα)=1.570 mm-1, R=0.0735 and wR=0.1389 for 8015 observed reflections with I>2σ(I) for complex 2; and a=9.308(3), b=15.357(3), c=17.419(4) Å, α=66.493(13), β=88.61(2), γ=86.664(19)°, V=2279.4(9) Å3, Z=2, Dc=1.499 g/cm3, F(000)=1046, μ(MoKα)=1.364 mm-1, R=0.0843 and wR=0.2280 for 8433 observed reflections with I>2σ(I) for complex 3. Each central metal in complexes 1 and 2 is six-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands to give a distorted octahedral geometry, while the central metal in 3 is seven-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands and one oxygen atom from the solvated THF molecule to complete a distorted monocapped trigonal prism.
Three homoleptic lanthanide complexes, [C6H5COCHC(CH3)N(p-ClC6H4)]3Ln(THF)n (n=0, Ln=Yb (1); n=0, Ln=Y (2); n=1, Ln=Nd (3)), were synthesized by amine elimination reaction of Ln[N(SiMe3)2]3 with 1-phenyl-3-N-(p-chlorophenylimino)-1-butanone. These complexes crystallize in triclinic, space group P1 with a=9.805(3), b=14.831(6), c=16.075(6) Å, α=111.996(9), β=91.570(7), γ=93.744(6)°, V=2159.4(13) Å3, Z=2, Dc=1.515 g/cm3, F(000)=986, μ(MoKα)=2.396 mm-1, R=0.0360 and wR=0.0850 for 9548 observed reflections with I>2σ(I) for complex 1; a=9.861(5), b=14.852(9), c=16.111(9) Å, α=112.362(13), β=91.949(11), γ=93.678(14)°, V=2173(2) Å3, Z=2, Dc=1.377 g/cm3, F(000)=924, μ(MoKα)=1.570 mm-1, R=0.0735 and wR=0.1389 for 8015 observed reflections with I>2σ(I) for complex 2; and a=9.308(3), b=15.357(3), c=17.419(4) Å, α=66.493(13), β=88.61(2), γ=86.664(19)°, V=2279.4(9) Å3, Z=2, Dc=1.499 g/cm3, F(000)=1046, μ(MoKα)=1.364 mm-1, R=0.0843 and wR=0.2280 for 8433 observed reflections with I>2σ(I) for complex 3. Each central metal in complexes 1 and 2 is six-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands to give a distorted octahedral geometry, while the central metal in 3 is seven-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands and one oxygen atom from the solvated THF molecule to complete a distorted monocapped trigonal prism.
2014, 33(7): 1037-1042
Abstract:
One compound with N-(4-pyridylmethyl)imidazole liand, [Co(pyim)2(N3)2]n 1 (pyim=N-(4-pyridylmethyl)imidazole), was synthesized and structurally characterized. Compound 1 crystallizes in triclinic, space group P21/c with a=8.090(3), b=16.109(3), c=8.590(3), β=117.800(12)°, V=990.3(5) Å3, Z=2, Mr=461.37, Dc=1.547 g/cm3, F(000)=474, μ=0.901 mm-1, the final R=0.0381 and wR=0.0950 for 1581 observed reflections with I>2σ(I). In this compound, the unique Co(Ⅱ) resides at a crystallographic inversion center and exhibits an octahedral coordination geometry. The adjacent Co(Ⅱ) ions are connected by the pyim ligands to form a 2D layer structure. The layers are stacked in an ABAB mode and reinforced by the weak interlayer C-H…N hydrogen bonds and π-π stacking to give a 3D architecture. The thermal property and electrochemical property of compound 1 have also been studied.
One compound with N-(4-pyridylmethyl)imidazole liand, [Co(pyim)2(N3)2]n 1 (pyim=N-(4-pyridylmethyl)imidazole), was synthesized and structurally characterized. Compound 1 crystallizes in triclinic, space group P21/c with a=8.090(3), b=16.109(3), c=8.590(3), β=117.800(12)°, V=990.3(5) Å3, Z=2, Mr=461.37, Dc=1.547 g/cm3, F(000)=474, μ=0.901 mm-1, the final R=0.0381 and wR=0.0950 for 1581 observed reflections with I>2σ(I). In this compound, the unique Co(Ⅱ) resides at a crystallographic inversion center and exhibits an octahedral coordination geometry. The adjacent Co(Ⅱ) ions are connected by the pyim ligands to form a 2D layer structure. The layers are stacked in an ABAB mode and reinforced by the weak interlayer C-H…N hydrogen bonds and π-π stacking to give a 3D architecture. The thermal property and electrochemical property of compound 1 have also been studied.
2014, 33(7): 1043-1049
Abstract:
A new sulfate inorganic framework, {(C2H8N)9[Nd5(SO4)12]·2H2O}n (1) templated by organic amine, has been solvothermally synthesized and characterized by TGA, PXRD and single-crystal X-ray diffraction. Compound 1 crystalizes in monoclinic, space group C2/c with a=20.570(5), b=35.815(8), c=10.106(2) Å, C18H72N9Nd5O50S12, Mr=2315.73, V=6765(3) Å3, Z=4, Dc=2.274 g·cm-3, μ=4.253 mm-1, F(000)=4520, 2.52 < θ < 25°, λ(MoKα)=0.71073 Å, T=273(2) K, the final R=0.0401, wR=0.1022 and S=1.042. X-ray diffraction analysis reveals that complex 1 possesses a 3D inorganic sulfate framework with large 20-membered ring (20 MR) and 10-membered ring (10 MR) channels constructed by two kinds of SBUs. Moreover, the UV-vis and luminescent properties of complex 1 were also investigated.
A new sulfate inorganic framework, {(C2H8N)9[Nd5(SO4)12]·2H2O}n (1) templated by organic amine, has been solvothermally synthesized and characterized by TGA, PXRD and single-crystal X-ray diffraction. Compound 1 crystalizes in monoclinic, space group C2/c with a=20.570(5), b=35.815(8), c=10.106(2) Å, C18H72N9Nd5O50S12, Mr=2315.73, V=6765(3) Å3, Z=4, Dc=2.274 g·cm-3, μ=4.253 mm-1, F(000)=4520, 2.52 < θ < 25°, λ(MoKα)=0.71073 Å, T=273(2) K, the final R=0.0401, wR=0.1022 and S=1.042. X-ray diffraction analysis reveals that complex 1 possesses a 3D inorganic sulfate framework with large 20-membered ring (20 MR) and 10-membered ring (10 MR) channels constructed by two kinds of SBUs. Moreover, the UV-vis and luminescent properties of complex 1 were also investigated.
2014, 33(7): 1050-1056
Abstract:
A new Cd(Ⅱ) coordination polymer, {[Cd(Hnbta)(L)]·H2O}n (L=1,4-bis(5,6-dimethylbenzimidazol-1-yl)butane), H3nbta=5-nitrobenzene-1,2,3-tricarboxylic acid), has been hydro-thermally synthesized and characterized by elemental analyses, IR, XRPD, and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a=17.3056(13), b=11.0114(9), c=17.7484(14) Å, β=117.3640(10)°, V=3003.7(4) Å3, Z=4, C31H31CdN5O9, Mr=730.01, Dc=1.614 g/cm3, μ=0.792 mm-1 and F(000)=1488. The cadmium(Ⅱ) ions are bridged by Hnbta2- to generate a two-dimensional metal organic framework with fes topology. In addition, the thermal stability and fluorescence properties of the complex were also studied.
A new Cd(Ⅱ) coordination polymer, {[Cd(Hnbta)(L)]·H2O}n (L=1,4-bis(5,6-dimethylbenzimidazol-1-yl)butane), H3nbta=5-nitrobenzene-1,2,3-tricarboxylic acid), has been hydro-thermally synthesized and characterized by elemental analyses, IR, XRPD, and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a=17.3056(13), b=11.0114(9), c=17.7484(14) Å, β=117.3640(10)°, V=3003.7(4) Å3, Z=4, C31H31CdN5O9, Mr=730.01, Dc=1.614 g/cm3, μ=0.792 mm-1 and F(000)=1488. The cadmium(Ⅱ) ions are bridged by Hnbta2- to generate a two-dimensional metal organic framework with fes topology. In addition, the thermal stability and fluorescence properties of the complex were also studied.
2014, 33(7): 1057-1062
Abstract:
A novel lanthanum(Ⅲ) complex, [LaL2(NO3)3]·H2O (1) based on L (L=N-(naphthalene-1-yl)-2-(quinolin-8-yloxy)acetamide), was synthesized and characterized by X-ray diffraction. The crystal of 1 belongs to the monoclinic system, space group C2c with Mr=1017.69, a=25.1438(17), b=13.5950(9), c=18.2349(12) Å, β=132.4980(10)°, V=4595.8(5) Å3, Z=4, Dc=1.471 Mg/m3, F(000)=2056, μ=1.004 mm-1, R=0.0588 and wR=0.1402. The central La(Ⅲ) ion is coordinated to four oxygen atoms, two nitrogen atoms from two independent acetamide ligands and six oxygen atoms from three nitrate anions, possessing a distorted icosahedron coordination geometry. In the crystal of 1, intermolecular N-H…O hydrogen bonds linked the molecules into chains along the c axis. In solid state and CH3CN solution, complex 1 exhibits stronger fluorescent emission than the ligand L.
A novel lanthanum(Ⅲ) complex, [LaL2(NO3)3]·H2O (1) based on L (L=N-(naphthalene-1-yl)-2-(quinolin-8-yloxy)acetamide), was synthesized and characterized by X-ray diffraction. The crystal of 1 belongs to the monoclinic system, space group C2c with Mr=1017.69, a=25.1438(17), b=13.5950(9), c=18.2349(12) Å, β=132.4980(10)°, V=4595.8(5) Å3, Z=4, Dc=1.471 Mg/m3, F(000)=2056, μ=1.004 mm-1, R=0.0588 and wR=0.1402. The central La(Ⅲ) ion is coordinated to four oxygen atoms, two nitrogen atoms from two independent acetamide ligands and six oxygen atoms from three nitrate anions, possessing a distorted icosahedron coordination geometry. In the crystal of 1, intermolecular N-H…O hydrogen bonds linked the molecules into chains along the c axis. In solid state and CH3CN solution, complex 1 exhibits stronger fluorescent emission than the ligand L.
2014, 33(7): 1063-1068
Abstract:
A new coordination polymer, namely [Ca(HOABDC)]n (1, H3OABDC=5-oxyacetateisophthalic acid), has been synthesized through hydrothermal reactions of Ca(NO3)2 and H3OABDC. The title compound crystallizes in monoclinic, space group P21/c with a=4.3043(2), b=21.4959(11), c=10.7450(6) Å, β=91.411(5)°, V=993.88(9) Å3, C10H6O7Ca, Mr=278.23, Z=4, Dc=1.859 g/cm3, F(000)=560, μ=0.659 mm-1, the final R=0.0328 and wR=0.0670 for 1469 observed reflections (I>2σ(I)). Single-crystal X-ray structural analysis reveals that compound 1 features 1D Ca(Ⅱ)-carboxylate chain-shaped subunits, which are further connected together via HOABDC2- ligands into a 3D (6,6)-connected nia-type hybrid framework. Moreover, the luminescent property and thermal stability of 1 were also investigated.
A new coordination polymer, namely [Ca(HOABDC)]n (1, H3OABDC=5-oxyacetateisophthalic acid), has been synthesized through hydrothermal reactions of Ca(NO3)2 and H3OABDC. The title compound crystallizes in monoclinic, space group P21/c with a=4.3043(2), b=21.4959(11), c=10.7450(6) Å, β=91.411(5)°, V=993.88(9) Å3, C10H6O7Ca, Mr=278.23, Z=4, Dc=1.859 g/cm3, F(000)=560, μ=0.659 mm-1, the final R=0.0328 and wR=0.0670 for 1469 observed reflections (I>2σ(I)). Single-crystal X-ray structural analysis reveals that compound 1 features 1D Ca(Ⅱ)-carboxylate chain-shaped subunits, which are further connected together via HOABDC2- ligands into a 3D (6,6)-connected nia-type hybrid framework. Moreover, the luminescent property and thermal stability of 1 were also investigated.
2014, 33(7): 1069-1073
Abstract:
A new 2D Ca(Ⅱ) coordination polymer, [Ca(H2btc)(H2O)2]n (1, H4btc=biphenyl-3,3',5,5'-tetracarboxylic acid), has been synthesized using the hydrothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, IR, thermogravimetric analysis, and photoluminescent analysis. Complex 1 crystallizes in the monoclinic system, space group C2/c with a=17.5676(15), b=11.4496(8), c=7.6197(8) Å, β=102.787(2)°, V=1494.6(2) Å3, Z=4, Dc=1.797 Mg·m-3, μ=0.483 mm-1, F(000)=832, the final R=0.0348 and wR=0.0915 for 1521 observed reflections with I>2σ(I). Complex 1 has a 2D network containing 1D calcium-oxygen chains. These 2D networks are further connected by O-H…O hydrogen bonding interactions to generate a 3D supramolecular structure.
A new 2D Ca(Ⅱ) coordination polymer, [Ca(H2btc)(H2O)2]n (1, H4btc=biphenyl-3,3',5,5'-tetracarboxylic acid), has been synthesized using the hydrothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, IR, thermogravimetric analysis, and photoluminescent analysis. Complex 1 crystallizes in the monoclinic system, space group C2/c with a=17.5676(15), b=11.4496(8), c=7.6197(8) Å, β=102.787(2)°, V=1494.6(2) Å3, Z=4, Dc=1.797 Mg·m-3, μ=0.483 mm-1, F(000)=832, the final R=0.0348 and wR=0.0915 for 1521 observed reflections with I>2σ(I). Complex 1 has a 2D network containing 1D calcium-oxygen chains. These 2D networks are further connected by O-H…O hydrogen bonding interactions to generate a 3D supramolecular structure.
2014, 33(7): 1074-1080
Abstract:
Two coordination polymers constructed from 3,4-thiophenedicarboxylic acid and bis(2-methyl imidazole) ligands, namely, {[Cd2(tdc)2(bip)2]·7H2O}n (1) and [Cd(tdc)(bib)]n (2) (H2tdc=3,4-thiophenedicarboxylic acid, bip=1,3-bis-(imidazol-2-methyl)propane and bib=1,4-bis(imidazol-2-methyl)butane), have been synthesized and structurally characterized by single-crystal X-ray diffraction. Structural analyses reveal that 1 exhibits a two-dimensional (2D) layered network with 3-connected (6,3) topology, which is further connected into a threedimensional (3D) supramolecular structure by intermolecular hydrogen bonds. However, 2 features a 2D network which can be rationalized as a 4-connected sql net. The results indicate the subtle difference of auxiliary bis(imidazol-2-methyl) ligands may lead to diverse architectures. Moreover, they exhibit luminescence emission in the solid state at room temperature.
Two coordination polymers constructed from 3,4-thiophenedicarboxylic acid and bis(2-methyl imidazole) ligands, namely, {[Cd2(tdc)2(bip)2]·7H2O}n (1) and [Cd(tdc)(bib)]n (2) (H2tdc=3,4-thiophenedicarboxylic acid, bip=1,3-bis-(imidazol-2-methyl)propane and bib=1,4-bis(imidazol-2-methyl)butane), have been synthesized and structurally characterized by single-crystal X-ray diffraction. Structural analyses reveal that 1 exhibits a two-dimensional (2D) layered network with 3-connected (6,3) topology, which is further connected into a threedimensional (3D) supramolecular structure by intermolecular hydrogen bonds. However, 2 features a 2D network which can be rationalized as a 4-connected sql net. The results indicate the subtle difference of auxiliary bis(imidazol-2-methyl) ligands may lead to diverse architectures. Moreover, they exhibit luminescence emission in the solid state at room temperature.
2014, 33(7): 1081-1090
Abstract:
The synthesis and in vitro photodynamic anticancer activity of a new photosensitizer, tetra(trifluoroethoxy) germanium phthalocyanine (GePcF), were studied. GePcF was characterized by UV-Vis, IR, MS and elemental analysis. The in vitro photodynamic activity of GePcF was studied by MTT. IC50 of GePcF for SW480 cells of human colonic adenocarcinoma and HeLa cells of cervical cancer were 36.53 and 45.78 μmol/L, respectively. GePcF as a photosensitizer may be used to treat cancers due to its photodynamic anticancer activity.
The synthesis and in vitro photodynamic anticancer activity of a new photosensitizer, tetra(trifluoroethoxy) germanium phthalocyanine (GePcF), were studied. GePcF was characterized by UV-Vis, IR, MS and elemental analysis. The in vitro photodynamic activity of GePcF was studied by MTT. IC50 of GePcF for SW480 cells of human colonic adenocarcinoma and HeLa cells of cervical cancer were 36.53 and 45.78 μmol/L, respectively. GePcF as a photosensitizer may be used to treat cancers due to its photodynamic anticancer activity.
2014, 33(7): 1091-1095
Abstract:
The title compound (zifaxaban 2, C20H16ClN3O4S, Mr=429.87) was synthesized and its crystal structure was determined by single-crystal X-ray diffraction. Zifaxaban crystallizes in monoclinic, space group P21 with a=5.7900(12), b=13.086(3), c=12.889(3) Å, β=100.86(3)°, V=959.1(3) Å3, Z=2, Dc=1.489 g/cm3, F(000)=444, μ=0.342 mm-1, the final R=0.0320 and wR=0.0640 for 2717 observed reflections (I>2σ(I)). The absolute configuration of the stereogenic center in the title compound was confirmed to be S by single-crystal X-ray diffraction. Four existing intermolecular hydrogen bonds help to stabilize the lattice and the molecule in the lattice to adopt an L-shape conformation. Zifaxaban was slightly more active than rivaroxaban 1 in in vitro assay against human FXa and therefore is promising as a drug candidate.
The title compound (zifaxaban 2, C20H16ClN3O4S, Mr=429.87) was synthesized and its crystal structure was determined by single-crystal X-ray diffraction. Zifaxaban crystallizes in monoclinic, space group P21 with a=5.7900(12), b=13.086(3), c=12.889(3) Å, β=100.86(3)°, V=959.1(3) Å3, Z=2, Dc=1.489 g/cm3, F(000)=444, μ=0.342 mm-1, the final R=0.0320 and wR=0.0640 for 2717 observed reflections (I>2σ(I)). The absolute configuration of the stereogenic center in the title compound was confirmed to be S by single-crystal X-ray diffraction. Four existing intermolecular hydrogen bonds help to stabilize the lattice and the molecule in the lattice to adopt an L-shape conformation. Zifaxaban was slightly more active than rivaroxaban 1 in in vitro assay against human FXa and therefore is promising as a drug candidate.
2014, 33(7): 1096-1101
Abstract:
A new phenoxyacetamide derivative, methyl 2-((4-(2-(2-methylphenoxy)acetyl)piperazin-1-yl)methyl)benzoate (C22H26N2O4, Mr=382.45), has been synthesized and characterized by 1H NMR, 13C NMR, H RMS and single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a=11.145(2), b=13.667(3), c=13.998(3) Å, β=112.01(3)°, V=1976.8(7) Å3, Z=4, Dc=1.285 g/cm3, F(000)=816, μ=0.089 mm-1, MoKα radiation (λ=0.71073 Å), the final R=0.0602 and wR=0.1533 for 2343 observed reflections with I>2σ(I). Intramolecular C-H…O interactions as well as intermolecular C-H…O hydrogen bonds help to stabilize the crystal structure. The preliminary bioassay results show that the title compound exhibits potent neuroprotective activity.
A new phenoxyacetamide derivative, methyl 2-((4-(2-(2-methylphenoxy)acetyl)piperazin-1-yl)methyl)benzoate (C22H26N2O4, Mr=382.45), has been synthesized and characterized by 1H NMR, 13C NMR, H RMS and single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a=11.145(2), b=13.667(3), c=13.998(3) Å, β=112.01(3)°, V=1976.8(7) Å3, Z=4, Dc=1.285 g/cm3, F(000)=816, μ=0.089 mm-1, MoKα radiation (λ=0.71073 Å), the final R=0.0602 and wR=0.1533 for 2343 observed reflections with I>2σ(I). Intramolecular C-H…O interactions as well as intermolecular C-H…O hydrogen bonds help to stabilize the crystal structure. The preliminary bioassay results show that the title compound exhibits potent neuroprotective activity.
