A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- ...A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- (phen)(μ-L)3/3]?H2O (H2L = pyrazine-2,3-dicarboxylic acid) has been hydrothermally synthesized, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group P21/n with a = 11.480(2), b = 11.885(2), c = 12.939(3) ?, β = 110.55(3)°, V = 1653.1(6) ?3, Mr = 423.25, Dc = 0.425 g/cm3, Z = 4, R = 0.0361 and wR = 0.1011. The title complex consists of 2D 2 ∞ [Co(phen)(μ-L)3/3] layers and crystal water molecules. Each Co atom is octahedrally coordinated by three N atoms and three O atoms to form 2D 2 ∞ [Co(phen)(μ-L)3/3] polymeric layers. Furthermore, such 2D layers are stacked into 3D supramolecular frameworks via Van der Waals’ intermolecular forces, strong and weak hydrogen-bond interactions. The coordination phen and crystal water molecules are resided into cavities of the frameworks.展开更多
The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkali...The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkaline hydrolysis and nitrosation reactions. The yield of DMNNDO was increased from 37% to 45%. The structure of DMNNDO was characterized by IR,^1H NMR,^13 C NMR,and elemental analysis. Also the thermal decomposition of DMNNDO was studied by using DSC and TG-DTG to find that there are primarily two exothermic decomposition processes between 90 and 300 oC. The crystal structure of DMNNDO was studied by X-ray single-crystal diffraction for the first time. The molecular structure exists as a dimeric form due to the presence of nitroso group. The crystal belongs to monoclinic system,space group C2/c with a = 14.515(3),b = 9.955(2),c = 11.897(2) °,β = 98.500(3)°,V = 1.6998(2) nm^3,Z = 8,D_c = 1.486 g×cm^-3,μ = 0.128 mm^-1,F(000) = 800,S = 1.055,R = 0.0358 and wR = 0.0917. In particular,DMNNDO could be easily hydrolyzed in hydrous systems and the hydrolysis mechanism in CDCl_3 was revealed by means of NMR monitoring.展开更多
A new coordination compound of cis-bis(1,10-phenanthroline)glycinecobalt(Ⅲ) chloridate tetrahydrate,cis-[Co(phen)_2gly]Cl_2.4H_2O,has been prepared by glycine reacted with cis-[Co(phen)_2Cl_2]Cl,then isolated by SP-S...A new coordination compound of cis-bis(1,10-phenanthroline)glycinecobalt(Ⅲ) chloridate tetrahydrate,cis-[Co(phen)_2gly]Cl_2.4H_2O,has been prepared by glycine reacted with cis-[Co(phen)_2Cl_2]Cl,then isolated by SP-Sephadex C-25 H^+ form column. The crystal and molecular structure of the new compound has been determined by RIGAKU AFC5R four circle diffractometer,5032 independent reflections were collected of which 3781 observable reflections were used for structure refinement.The crystal is monoclinic,space group C2/c,with a=35.13(1),b=9.637(3)(,c=17.485(6),β= 115.08(Z)~,V=5362(3),Z=8.The structure was refined by full matrix least-squares procedure to a final R=0.041 and R_=0.060.The molecular formula was CoC_(28)H_(28)N_5O_8Cl_2. with molecular weight M_r=636.38,D_c=1.58g/cm^3,μ=8.88cm^(-1)and F_((000))=2624.展开更多
The title complex i-C_4H_9Co(salen)(Py) (Py=pyridine. salen=dianion of disalicylideneethylenediamine) has been first synthesized. Its crystal structure has been determined by X-ray diffraction method. The crystsis are...The title complex i-C_4H_9Co(salen)(Py) (Py=pyridine. salen=dianion of disalicylideneethylenediamine) has been first synthesized. Its crystal structure has been determined by X-ray diffraction method. The crystsis are monoclinic with space group P2_1/ C. The unit cell parametes are presented. The structure has been refined to a final R of 0.038.展开更多
A new 3-D nickel(Ⅱ) metal-organic framework(MOFs) with formula [Ni(bib)_2(SO_4)]_n(1), where bib = 1,4-bis(imidazol-1-yl)benzene, has been synthesized and characterized by single-crystal X-ray diffraction...A new 3-D nickel(Ⅱ) metal-organic framework(MOFs) with formula [Ni(bib)_2(SO_4)]_n(1), where bib = 1,4-bis(imidazol-1-yl)benzene, has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and surface photovoltage spectroscopy(SPS). Complex 1 crystallizes in monoclinic system, space group C2/c with a = 19.5988(6), b = 9.7531(3), c = 11.8146(4) ?, β = 96.185(3)°, V = 2245.20(12) ?~3, C_(24)H_(20)N_8NiO_4S, M_r = 575.25, D_c = 1.702 g/cm^3, Z = 4, F(000) = 1184, μ = 1.011 mm-1, the final R = 0.0293 and w R = 0.0702. X-ray diffraction analyses indicated that the center Ni^(2+) ion is six-coordinated with an O_2N_4 donor set of two μ_2-SO_4^(2–) and four bib ligands, resulting in an ideal octahedral geometry. Topological analysis on complex 1 considers each Ni^(2+) as a 6-connected node, while bib and sulfate ion as linkers, giving an α-Po topology with short Schl?fli symbol 412·63. In the crystal packing, the components interact with pairs of intermolecular C–H×××O hydrogen bonds. The SPS of 1 indicates that there are positive response bands in the range of 300~600 nm showing photo-electric conversion properties.展开更多
Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3...Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.展开更多
[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15c...[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .展开更多
A metal-organic coordination polymer [ZnE.s(phen)(BDC)2(OH)]2 (phen = 1,10- phenanthroline, BDC = benzene-1,4-dicarboxylic acid) 1 has been hydrothermally synthesized and structurally characterized by single-c...A metal-organic coordination polymer [ZnE.s(phen)(BDC)2(OH)]2 (phen = 1,10- phenanthroline, BDC = benzene-1,4-dicarboxylic acid) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The complex crystallizes in the triclinic system, space group PI with a = 11.199(2), b = 11.593(2), c = 11.865(3)/A, α= 99.330(1), β = 111.506(1), γ = 104.804(1)^o, V= 1328.4(5)A^3, Dc= 1.722 g/cm^3, Z = 1, Mr = 1377.82, F(000) = 692,μ(MoKa) = 2.306 mm^-1, S = 1.093, R= 0.0281 and wR = 0.0756 for 4179 observed reflections (I 〉 2σ(/)). The coordination polyhedron around Zn(II) can be described as a tetrahedron, trigonal bipyramid and octahedron. It is worth noting that the crystal structure of 1 is composed of tetranuclear zinc clusters linked by {ZnO6} units.展开更多
A metal-organic coordination polymer {[Zn(Pht)(4,4'-bipy)(H2O)2]·2H2O}n (Pht = phthalate, 4,4'-bipy = 4,4'-bipyridine) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR,...A metal-organic coordination polymer {[Zn(Pht)(4,4'-bipy)(H2O)2]·2H2O}n (Pht = phthalate, 4,4'-bipy = 4,4'-bipyridine) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Yellow crystals crystallize in the monoclinic system, space group P2/n, a = 7.6346(14), b = 11.316(2), c = 10.8133(19) ,A, β = 92.A.A,A.(3)°, V = 933.3(3) A^3, C18H20N2O8Zn, Mr = 457.73, Dc = 1.629 g/cm^3, F(000) = 472, Z = 2,μ(MoKa) = 1.367 mm^-1, the final R = 0.0323 and wR = 0.0821 for 1859 observed reflections (Ⅰ〉 2σ(Ⅰ)). The structure of 1 exhibits a two-dimensional bilayer framework formed by hydrogen bonding interactions. Furthermore, 1 shows yellow photoluminescent property at room temperature.展开更多
A new metal-organic coordination polymer [Zn(ipt)(im)2]2n·3nH2O 1 has been obtained by using hydrothermal synthesis and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-...A new metal-organic coordination polymer [Zn(ipt)(im)2]2n·3nH2O 1 has been obtained by using hydrothermal synthesis and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P2(1/n) with a = 10.653(3), b = 17.891(6), c = 10.743(4)A^°,β= 117.093(5)°, V= 1822.9(10) A^°3, Mr= 413.65, Dc = 1.507 g/cm^3,/t(MoKa) = 1.390 mm^-1, F(000) = 840, Z = 4, the final R = 0.0444 and wR = 0.1066 for 2434 observed reflections (I〉 2σ(I)). Furthermore, compound 1 shows blue photoluminescent property at room temperature.展开更多
A new 3d-4fheterometallic polymer {[Sm2Cu(PDC)2(SO4)2(H20)6]·2H2O}n 1 has been synthesized by Sm2O3, Cu(SO4)2·5H2O and pyridine-3,5-dicarboxylic acid under hydrothermal conditions. The compound cryst...A new 3d-4fheterometallic polymer {[Sm2Cu(PDC)2(SO4)2(H20)6]·2H2O}n 1 has been synthesized by Sm2O3, Cu(SO4)2·5H2O and pyridine-3,5-dicarboxylic acid under hydrothermal conditions. The compound crystallizes in triclinic system, space group Pi, with a = 6.352(7), b = 10.040(10), c = 10.315(11) A, α = 94.958(14), β = 95.556(7), γ = 99.747(14)°, V = 641.7(12)A3, Z = 1, M, = 1030.63, Dc= 2.651 Mg/m3,μ = 5.615 mm-1, F(000) = 491, the final R = 0.0491 and wR = 0.1345 for 2098 observed reflections with I 〉 2σ(I). The compound is a three-dimensional network structure in which infinite lanthanide-carboxylate chains are linked by [Cu($04)2]2- metalloligands to form a mixed-metal coordination network.展开更多
A metal-organic coordination polymer [Ni(PDB)(bix)(H20)]n (H2PDB = 3,4-pyri- dinedicarboxylic acid, bix = 1,4-bis(imidazol-l-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elem...A metal-organic coordination polymer [Ni(PDB)(bix)(H20)]n (H2PDB = 3,4-pyri- dinedicarboxylic acid, bix = 1,4-bis(imidazol-l-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. Blue crystals crystallize in the triclinic system, space group PI with a = 9.1849(8), b = 9.2065(9), c = 12.9308(12) °, a = 103.3070(10), β = 104.7160(10), y = 90.5900(10)°, V = 1026.42(16)/k3, C21H19NsNiOs, Mr = 480.12, Dc = 1.553 g/cm3, F(000) = 496, Z = 2,/l(MoKa) = 0.991 mm-1, the final R = 0.0325 and wR = 0.0799 for 3561 observed reflections (I 〉 2σ(I)). The structure of 1 exhibits a two-dimensional network structure.展开更多
A new two-dimensional cobalt coordination polymer has been prepared and fully characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The compound [Co(C2O4)(bix)]n 1 crystallizes in the m...A new two-dimensional cobalt coordination polymer has been prepared and fully characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The compound [Co(C2O4)(bix)]n 1 crystallizes in the monoclinic system, space group C2/c, with a = 11.549(3), b = 15.700(3), c = 9.260(2) A, β = 102.984(3)°, V = 1636.0(6) A^3, C16HIaCON4O4, Mr= 383.23, Dc = 1.556 g/cm^3, μ(MoKa) = 1.078 mm^-1, F(000) = 780, Z = 4, the final R = 0.0455 and wR = 0.1286 for 1483 observed reflections (I 〉 2σ(I)). Of the compound, the Co center is octahedrally coordinated with oxalate acting as a tetra-dentate ligand coordinated to the cobalt atom and each bix serving as a bridging ligand by employing two N-donors to coordinate with the Co center. An infinite {Co2(C2O4)2}∞ chain is formed along the α axis. Furthermore, the 1D chains are held together via bix ligands to generate a two-dimensional network structure with 1D coronal-like channels (ca. 5.691A × 15.700A).展开更多
A novel metal-organic coordination polymer [Cu2(phen)(ipt)2]2n-nH2O 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic,...A novel metal-organic coordination polymer [Cu2(phen)(ipt)2]2n-nH2O 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 12.338(3), b = 12.167(3), c = 18.167(4)A, β= 111.686(14)°, V = 2534.1(10)A^3, C28H18Cu2N2O9, Mr = 653.52, Dc = 1.713 g/cm^3,μ(MoKα) = 1.740 mm^-1, F(000) = 1320, Z = 4, the final R = 0.0443 and wR = 0.0853 for 3543 observed reflections (1 〉 2σ(I)). It exhibits a novel two-dimensional network with tetra-Cu-ipt-as building units.展开更多
A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by el...A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The title complex crystallizes in monoclinic,space group P21/c with a = 13.302(4),b = 10.981(3),c = 13.804(4) ,β = 93.587(5)°,V = 2012.3(10) 3,C20H14N2O5F6Zn,Mr = 541.72,Z = 4,Dc = 0.447 g/cm3, = 0.328 mm-1,F(000) = 272,R = 0.0340 and wR = 0.1107 for 4528 observed reflections(I 〉2σ(I)).In the structure of compound 1,two Zn(Ⅱ) ions are bridged by two carboxylate groups from two hfipbb ligands to form a dinuclear unit,and each dinuclear Zn(Ⅱ) unit is linked with its two adjacent dinuclear units through four hfipbb ligands into an infinite one-dimensional double-chain.The interesting structural feature of compound 1 is that the one-D double-chains are self-interconnected into a three-D supramolecular structure through hydrogen bonds between the coordinated e-urea molecules and carboxylate oxygen atoms(N1 and O2,N2 and O4).展开更多
A metal-organic coordination compound formulated as [Zn(pzdc)(phen)]n·nH2O 1 (H2pzdc = pyrazine-2,3-dicarboxylic acid, phen = 1,10-phenanthroline) has been hydrothermally synthesized and structurally charac...A metal-organic coordination compound formulated as [Zn(pzdc)(phen)]n·nH2O 1 (H2pzdc = pyrazine-2,3-dicarboxylic acid, phen = 1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 11.607(2), b = 11.719(2), c = 13.140(3)A^°, β = 110.707(3)°, V= 1671.9(6)A^°3, C18H12ZnN4O5, Mr= 429.69, De = 1.707 g/cm^3,μ(MoKa) = 1.511 mm^-1, F(000) = 872, Z = 4, the final R = 0.0356 and wR = 0.0853 for 2713 observed reflections (I 〉 2σ(I)). It exhibits an interesting two-dimensional layer structure and shows yellow photoluminescent property at room temperature.展开更多
A metal-organic coordination polymer [Cd(bpy)(BDC)]n·nbpy (bpy = 2,2-bipyri-dine, H2BDC = terephthalic acid) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spec...A metal-organic coordination polymer [Cd(bpy)(BDC)]n·nbpy (bpy = 2,2-bipyri-dine, H2BDC = terephthalic acid) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group C2/c with a = 15.723(5), b = 21.695(5), c = 7.576(5) A, β = 116.171(7)°, V = 2319.3(18)A^3, C28H20CdN4O4, Mr = 588.88, Dc = 1.686 g/cm^3, μ(MoKα) = 0.987 mm^-1, F(000) = 1184, Z = 4, the final R = 0.0464 and wR = 0.0831 for 1882 observed reflections (Ⅰ〉 2σ(Ⅰ)). It exhibits a three-dimensional network with channels constructed from one-dimensional coordination chains via C–H…O hydrogen bonds and significant aromatic π-π stacking interactions.展开更多
A new metal-organic complex [Pb2(PDB)2(phen)]n·nH2O (H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis...A new metal-organic complex [Pb2(PDB)2(phen)]n·nH2O (H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,TG and single-crystal X-ray diffraction.The compound crystallizes in triclinic,space group P1 with a=7.2472(5),b=10.6966(8),c=16.2376(12),α=98.2960(10),β=91.6430(10),γ=97.4810(10)o,V=1233.53(16)3,C26H16O9N4Pb2,Mr=942.81,Dc=2.538 g/cm3,μ(MoKα)=13.697 mm-1,F(000)=872,Z=2,the final R=0.0247 and wR=0.0654 for 3886 observed reflections (I 〉 2σ(I)).In the crystal structure,the Pb(1) atom is six-coordinated with four carboxylate oxygen atoms from three different PDB ligands and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry;the Pb(2) atom is four-coordinated with four carboxylate oxygen atoms from four different PDB ligands,showing a distorted tetrahedral geometry.It exhibits a three-dimensional supramolecular network structure formed by hydrogen bonds and π-π interactions.展开更多
A new complex [Cd(H2biim)2(H2O)2]·(ino)2·4H2O (H2biim = 2,2'-biimidazole, ino = isonicotinate-N-oxide) has been prepared and characterized by single-crystal X-ray diffraction analysis, IR and fluore...A new complex [Cd(H2biim)2(H2O)2]·(ino)2·4H2O (H2biim = 2,2'-biimidazole, ino = isonicotinate-N-oxide) has been prepared and characterized by single-crystal X-ray diffraction analysis, IR and fluorescence spectra analysis. The crystal is of triclinic system, space group P1 with a = 7.5380(6), b = 8.0402(7), c = 13.5094(11) , α = 104.269(1), β = 93.604(1), γ = 98.349(1)°, V = 780.93(11) 3, Mr = 765.00, Dc = 1.627 g/cm3, F(000) = 390, μ = 0.776 mm-1 and Z = 1. The final R = 0.0322 and wR = 0.0825 for 7038 observed reflections with I 2σ(I) and R = 0.0341 and wR = 0.0832 for all data. The title complex exhibits an infinite chain-like structure through bridging isonicotinate-N-oxide. Strong interchain hydrogen bonds between isonicotinate-N-oxide and H2biim result in the robust 3-D supramolecular architecture. Moreover, the complex shows strong photoluminescence with emission maximum at λ = 401 nm upon λex = 330 nm.展开更多
A metal-organic coordination polymer [Cd2(PDC)2(bix)(H2O)2]n·nH2O (H2PDC = 2,4-pyridinedicarboxylic acid, bix = 1,4-bis(imidazol-l-ylmethyl)-benzene) 1 has been hydrother- mally synthesized and characte...A metal-organic coordination polymer [Cd2(PDC)2(bix)(H2O)2]n·nH2O (H2PDC = 2,4-pyridinedicarboxylic acid, bix = 1,4-bis(imidazol-l-ylmethyl)-benzene) 1 has been hydrother- mally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Brown crystals crystallize in the orthorhombic system, space group P212121 with a = 11.741(3), b = 14.190(4), c = 18.963(5) A, V= 3159.4(14) A3, C28H26Cd2N6O11, Mr= 847.35, Dc = 1.781 g/cm3, F(000) = 1680, Z = 4,μ(MoKa) = 1.415 mm-1, the final R = 0.0381 and wR = 0.0882 for 5472 observed reflections (1 〉 2σ(I)). The structure of 1 exhibits a threedimensional network structure.展开更多
基金This work was supported by the Science and Technology Bureau of Jinhua City (No 2003-01-179)
文摘A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- (phen)(μ-L)3/3]?H2O (H2L = pyrazine-2,3-dicarboxylic acid) has been hydrothermally synthesized, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group P21/n with a = 11.480(2), b = 11.885(2), c = 12.939(3) ?, β = 110.55(3)°, V = 1653.1(6) ?3, Mr = 423.25, Dc = 0.425 g/cm3, Z = 4, R = 0.0361 and wR = 0.1011. The title complex consists of 2D 2 ∞ [Co(phen)(μ-L)3/3] layers and crystal water molecules. Each Co atom is octahedrally coordinated by three N atoms and three O atoms to form 2D 2 ∞ [Co(phen)(μ-L)3/3] polymeric layers. Furthermore, such 2D layers are stacked into 3D supramolecular frameworks via Van der Waals’ intermolecular forces, strong and weak hydrogen-bond interactions. The coordination phen and crystal water molecules are resided into cavities of the frameworks.
文摘The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkaline hydrolysis and nitrosation reactions. The yield of DMNNDO was increased from 37% to 45%. The structure of DMNNDO was characterized by IR,^1H NMR,^13 C NMR,and elemental analysis. Also the thermal decomposition of DMNNDO was studied by using DSC and TG-DTG to find that there are primarily two exothermic decomposition processes between 90 and 300 oC. The crystal structure of DMNNDO was studied by X-ray single-crystal diffraction for the first time. The molecular structure exists as a dimeric form due to the presence of nitroso group. The crystal belongs to monoclinic system,space group C2/c with a = 14.515(3),b = 9.955(2),c = 11.897(2) °,β = 98.500(3)°,V = 1.6998(2) nm^3,Z = 8,D_c = 1.486 g×cm^-3,μ = 0.128 mm^-1,F(000) = 800,S = 1.055,R = 0.0358 and wR = 0.0917. In particular,DMNNDO could be easily hydrolyzed in hydrous systems and the hydrolysis mechanism in CDCl_3 was revealed by means of NMR monitoring.
基金This project was supported by the National Science Foundation of China and Research Found 1991 of Royal Society of Chemistry(London).
文摘A new coordination compound of cis-bis(1,10-phenanthroline)glycinecobalt(Ⅲ) chloridate tetrahydrate,cis-[Co(phen)_2gly]Cl_2.4H_2O,has been prepared by glycine reacted with cis-[Co(phen)_2Cl_2]Cl,then isolated by SP-Sephadex C-25 H^+ form column. The crystal and molecular structure of the new compound has been determined by RIGAKU AFC5R four circle diffractometer,5032 independent reflections were collected of which 3781 observable reflections were used for structure refinement.The crystal is monoclinic,space group C2/c,with a=35.13(1),b=9.637(3)(,c=17.485(6),β= 115.08(Z)~,V=5362(3),Z=8.The structure was refined by full matrix least-squares procedure to a final R=0.041 and R_=0.060.The molecular formula was CoC_(28)H_(28)N_5O_8Cl_2. with molecular weight M_r=636.38,D_c=1.58g/cm^3,μ=8.88cm^(-1)and F_((000))=2624.
文摘The title complex i-C_4H_9Co(salen)(Py) (Py=pyridine. salen=dianion of disalicylideneethylenediamine) has been first synthesized. Its crystal structure has been determined by X-ray diffraction method. The crystsis are monoclinic with space group P2_1/ C. The unit cell parametes are presented. The structure has been refined to a final R of 0.038.
基金supported by the Guangxi Provincial Department of Education(No.KY2015ZD130,YB2014414)the Natural Science Foundation of Guangxi Province(No.2014GXNSFBA118040)+2 种基金The supports of the National Natural Science Foundation of China(No.51402158)are gratefully acknowledgedthe financial support by the Opening Project of Guangxi Colleges and Universities Key Laboratory of Beibu Gulf Oil and Natural Gas Resource Effective Utilization(No.2015KLOG09)the financial support from the Natural Science Foundation of Qinzhou University(No.2014PY-GJ05)
文摘A new 3-D nickel(Ⅱ) metal-organic framework(MOFs) with formula [Ni(bib)_2(SO_4)]_n(1), where bib = 1,4-bis(imidazol-1-yl)benzene, has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and surface photovoltage spectroscopy(SPS). Complex 1 crystallizes in monoclinic system, space group C2/c with a = 19.5988(6), b = 9.7531(3), c = 11.8146(4) ?, β = 96.185(3)°, V = 2245.20(12) ?~3, C_(24)H_(20)N_8NiO_4S, M_r = 575.25, D_c = 1.702 g/cm^3, Z = 4, F(000) = 1184, μ = 1.011 mm-1, the final R = 0.0293 and w R = 0.0702. X-ray diffraction analyses indicated that the center Ni^(2+) ion is six-coordinated with an O_2N_4 donor set of two μ_2-SO_4^(2–) and four bib ligands, resulting in an ideal octahedral geometry. Topological analysis on complex 1 considers each Ni^(2+) as a 6-connected node, while bib and sulfate ion as linkers, giving an α-Po topology with short Schl?fli symbol 412·63. In the crystal packing, the components interact with pairs of intermolecular C–H×××O hydrogen bonds. The SPS of 1 indicates that there are positive response bands in the range of 300~600 nm showing photo-electric conversion properties.
基金Project supported by China National Climbing plan and National Nature Science Foundation
文摘Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.
基金Project supported by the National Natural Science Foundation of China
文摘[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .
基金The project was supported by the Education Office of Jilin Province (No. 0047)
文摘A metal-organic coordination polymer [ZnE.s(phen)(BDC)2(OH)]2 (phen = 1,10- phenanthroline, BDC = benzene-1,4-dicarboxylic acid) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The complex crystallizes in the triclinic system, space group PI with a = 11.199(2), b = 11.593(2), c = 11.865(3)/A, α= 99.330(1), β = 111.506(1), γ = 104.804(1)^o, V= 1328.4(5)A^3, Dc= 1.722 g/cm^3, Z = 1, Mr = 1377.82, F(000) = 692,μ(MoKa) = 2.306 mm^-1, S = 1.093, R= 0.0281 and wR = 0.0756 for 4179 observed reflections (I 〉 2σ(/)). The coordination polyhedron around Zn(II) can be described as a tetrahedron, trigonal bipyramid and octahedron. It is worth noting that the crystal structure of 1 is composed of tetranuclear zinc clusters linked by {ZnO6} units.
基金The project was supported by the Education Office of Jilin Province (No. 0047)
文摘A metal-organic coordination polymer {[Zn(Pht)(4,4'-bipy)(H2O)2]·2H2O}n (Pht = phthalate, 4,4'-bipy = 4,4'-bipyridine) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Yellow crystals crystallize in the monoclinic system, space group P2/n, a = 7.6346(14), b = 11.316(2), c = 10.8133(19) ,A, β = 92.A.A,A.(3)°, V = 933.3(3) A^3, C18H20N2O8Zn, Mr = 457.73, Dc = 1.629 g/cm^3, F(000) = 472, Z = 2,μ(MoKa) = 1.367 mm^-1, the final R = 0.0323 and wR = 0.0821 for 1859 observed reflections (Ⅰ〉 2σ(Ⅰ)). The structure of 1 exhibits a two-dimensional bilayer framework formed by hydrogen bonding interactions. Furthermore, 1 shows yellow photoluminescent property at room temperature.
基金The project was supported by the Education Office of Jilin Province (No. 0047)
文摘A new metal-organic coordination polymer [Zn(ipt)(im)2]2n·3nH2O 1 has been obtained by using hydrothermal synthesis and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P2(1/n) with a = 10.653(3), b = 17.891(6), c = 10.743(4)A^°,β= 117.093(5)°, V= 1822.9(10) A^°3, Mr= 413.65, Dc = 1.507 g/cm^3,/t(MoKa) = 1.390 mm^-1, F(000) = 840, Z = 4, the final R = 0.0444 and wR = 0.1066 for 2434 observed reflections (I〉 2σ(I)). Furthermore, compound 1 shows blue photoluminescent property at room temperature.
基金supported by the Youth Foundation of Luoyang Normal University(No.10000875)the Foundation of Education Department of Henan Province(No.2011A150021)
文摘A new 3d-4fheterometallic polymer {[Sm2Cu(PDC)2(SO4)2(H20)6]·2H2O}n 1 has been synthesized by Sm2O3, Cu(SO4)2·5H2O and pyridine-3,5-dicarboxylic acid under hydrothermal conditions. The compound crystallizes in triclinic system, space group Pi, with a = 6.352(7), b = 10.040(10), c = 10.315(11) A, α = 94.958(14), β = 95.556(7), γ = 99.747(14)°, V = 641.7(12)A3, Z = 1, M, = 1030.63, Dc= 2.651 Mg/m3,μ = 5.615 mm-1, F(000) = 491, the final R = 0.0491 and wR = 0.1345 for 2098 observed reflections with I 〉 2σ(I). The compound is a three-dimensional network structure in which infinite lanthanide-carboxylate chains are linked by [Cu($04)2]2- metalloligands to form a mixed-metal coordination network.
基金supported by the Science and Technology Development Project of Jilin Provincial Science & Technology Department(201205080)
文摘A metal-organic coordination polymer [Ni(PDB)(bix)(H20)]n (H2PDB = 3,4-pyri- dinedicarboxylic acid, bix = 1,4-bis(imidazol-l-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. Blue crystals crystallize in the triclinic system, space group PI with a = 9.1849(8), b = 9.2065(9), c = 12.9308(12) °, a = 103.3070(10), β = 104.7160(10), y = 90.5900(10)°, V = 1026.42(16)/k3, C21H19NsNiOs, Mr = 480.12, Dc = 1.553 g/cm3, F(000) = 496, Z = 2,/l(MoKa) = 0.991 mm-1, the final R = 0.0325 and wR = 0.0799 for 3561 observed reflections (I 〉 2σ(I)). The structure of 1 exhibits a two-dimensional network structure.
基金supported by the Science and Technology Development Project of Jilin Provincial Science & Technology Department(201205080)the Science and Technology Research Projects of the Education Office of Jilin Province (No. 2012. 358)
文摘A new two-dimensional cobalt coordination polymer has been prepared and fully characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The compound [Co(C2O4)(bix)]n 1 crystallizes in the monoclinic system, space group C2/c, with a = 11.549(3), b = 15.700(3), c = 9.260(2) A, β = 102.984(3)°, V = 1636.0(6) A^3, C16HIaCON4O4, Mr= 383.23, Dc = 1.556 g/cm^3, μ(MoKa) = 1.078 mm^-1, F(000) = 780, Z = 4, the final R = 0.0455 and wR = 0.1286 for 1483 observed reflections (I 〉 2σ(I)). Of the compound, the Co center is octahedrally coordinated with oxalate acting as a tetra-dentate ligand coordinated to the cobalt atom and each bix serving as a bridging ligand by employing two N-donors to coordinate with the Co center. An infinite {Co2(C2O4)2}∞ chain is formed along the α axis. Furthermore, the 1D chains are held together via bix ligands to generate a two-dimensional network structure with 1D coronal-like channels (ca. 5.691A × 15.700A).
文摘A novel metal-organic coordination polymer [Cu2(phen)(ipt)2]2n-nH2O 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 12.338(3), b = 12.167(3), c = 18.167(4)A, β= 111.686(14)°, V = 2534.1(10)A^3, C28H18Cu2N2O9, Mr = 653.52, Dc = 1.713 g/cm^3,μ(MoKα) = 1.740 mm^-1, F(000) = 1320, Z = 4, the final R = 0.0443 and wR = 0.0853 for 3543 observed reflections (1 〉 2σ(I)). It exhibits a novel two-dimensional network with tetra-Cu-ipt-as building units.
基金supported by the Natural Science Foundation of Fujian Province (No.2010J01029)the Foundation of Education Committee of Fujian Province (No.JB11002)
文摘A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The title complex crystallizes in monoclinic,space group P21/c with a = 13.302(4),b = 10.981(3),c = 13.804(4) ,β = 93.587(5)°,V = 2012.3(10) 3,C20H14N2O5F6Zn,Mr = 541.72,Z = 4,Dc = 0.447 g/cm3, = 0.328 mm-1,F(000) = 272,R = 0.0340 and wR = 0.1107 for 4528 observed reflections(I 〉2σ(I)).In the structure of compound 1,two Zn(Ⅱ) ions are bridged by two carboxylate groups from two hfipbb ligands to form a dinuclear unit,and each dinuclear Zn(Ⅱ) unit is linked with its two adjacent dinuclear units through four hfipbb ligands into an infinite one-dimensional double-chain.The interesting structural feature of compound 1 is that the one-D double-chains are self-interconnected into a three-D supramolecular structure through hydrogen bonds between the coordinated e-urea molecules and carboxylate oxygen atoms(N1 and O2,N2 and O4).
基金Supported by the Science and Technology Research Projects of the Education Office of Jilin Province (No. 2007. 213)
文摘A metal-organic coordination compound formulated as [Zn(pzdc)(phen)]n·nH2O 1 (H2pzdc = pyrazine-2,3-dicarboxylic acid, phen = 1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 11.607(2), b = 11.719(2), c = 13.140(3)A^°, β = 110.707(3)°, V= 1671.9(6)A^°3, C18H12ZnN4O5, Mr= 429.69, De = 1.707 g/cm^3,μ(MoKa) = 1.511 mm^-1, F(000) = 872, Z = 4, the final R = 0.0356 and wR = 0.0853 for 2713 observed reflections (I 〉 2σ(I)). It exhibits an interesting two-dimensional layer structure and shows yellow photoluminescent property at room temperature.
基金The project was supported by the Education Office of Jilin Province (No. 0047)
文摘A metal-organic coordination polymer [Cd(bpy)(BDC)]n·nbpy (bpy = 2,2-bipyri-dine, H2BDC = terephthalic acid) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group C2/c with a = 15.723(5), b = 21.695(5), c = 7.576(5) A, β = 116.171(7)°, V = 2319.3(18)A^3, C28H20CdN4O4, Mr = 588.88, Dc = 1.686 g/cm^3, μ(MoKα) = 0.987 mm^-1, F(000) = 1184, Z = 4, the final R = 0.0464 and wR = 0.0831 for 1882 observed reflections (Ⅰ〉 2σ(Ⅰ)). It exhibits a three-dimensional network with channels constructed from one-dimensional coordination chains via C–H…O hydrogen bonds and significant aromatic π-π stacking interactions.
基金Supported by the Science and Technology Research Projects of the Education Office of Jilin Province (No. 2007. 213)
文摘A new metal-organic complex [Pb2(PDB)2(phen)]n·nH2O (H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,TG and single-crystal X-ray diffraction.The compound crystallizes in triclinic,space group P1 with a=7.2472(5),b=10.6966(8),c=16.2376(12),α=98.2960(10),β=91.6430(10),γ=97.4810(10)o,V=1233.53(16)3,C26H16O9N4Pb2,Mr=942.81,Dc=2.538 g/cm3,μ(MoKα)=13.697 mm-1,F(000)=872,Z=2,the final R=0.0247 and wR=0.0654 for 3886 observed reflections (I 〉 2σ(I)).In the crystal structure,the Pb(1) atom is six-coordinated with four carboxylate oxygen atoms from three different PDB ligands and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry;the Pb(2) atom is four-coordinated with four carboxylate oxygen atoms from four different PDB ligands,showing a distorted tetrahedral geometry.It exhibits a three-dimensional supramolecular network structure formed by hydrogen bonds and π-π interactions.
基金supported by the National Natural Science Foundation of China (No. 20772042)
文摘A new complex [Cd(H2biim)2(H2O)2]·(ino)2·4H2O (H2biim = 2,2'-biimidazole, ino = isonicotinate-N-oxide) has been prepared and characterized by single-crystal X-ray diffraction analysis, IR and fluorescence spectra analysis. The crystal is of triclinic system, space group P1 with a = 7.5380(6), b = 8.0402(7), c = 13.5094(11) , α = 104.269(1), β = 93.604(1), γ = 98.349(1)°, V = 780.93(11) 3, Mr = 765.00, Dc = 1.627 g/cm3, F(000) = 390, μ = 0.776 mm-1 and Z = 1. The final R = 0.0322 and wR = 0.0825 for 7038 observed reflections with I 2σ(I) and R = 0.0341 and wR = 0.0832 for all data. The title complex exhibits an infinite chain-like structure through bridging isonicotinate-N-oxide. Strong interchain hydrogen bonds between isonicotinate-N-oxide and H2biim result in the robust 3-D supramolecular architecture. Moreover, the complex shows strong photoluminescence with emission maximum at λ = 401 nm upon λex = 330 nm.
基金supported by the Science and Technology Development Project of Jilin Provincial Science & Technology Department(201205080)
文摘A metal-organic coordination polymer [Cd2(PDC)2(bix)(H2O)2]n·nH2O (H2PDC = 2,4-pyridinedicarboxylic acid, bix = 1,4-bis(imidazol-l-ylmethyl)-benzene) 1 has been hydrother- mally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Brown crystals crystallize in the orthorhombic system, space group P212121 with a = 11.741(3), b = 14.190(4), c = 18.963(5) A, V= 3159.4(14) A3, C28H26Cd2N6O11, Mr= 847.35, Dc = 1.781 g/cm3, F(000) = 1680, Z = 4,μ(MoKa) = 1.415 mm-1, the final R = 0.0381 and wR = 0.0882 for 5472 observed reflections (1 〉 2σ(I)). The structure of 1 exhibits a threedimensional network structure.