Two zinc(Ⅱ) compounds, [Zn(L)(H2O)2]n 1 and [Zn(4,4'-bpy)(H2O)4](L) 2 (H2L = trans,trans-1,3 butadiene 1,4-dicarboxylic acid), were synthesized by hydrothermal methods and characterized by single-cryst...Two zinc(Ⅱ) compounds, [Zn(L)(H2O)2]n 1 and [Zn(4,4'-bpy)(H2O)4](L) 2 (H2L = trans,trans-1,3 butadiene 1,4-dicarboxylic acid), were synthesized by hydrothermal methods and characterized by single-crystal X-ray diffraction analyses. Compound 1 crystallizes in monoclinic, space group C2/c with a=15.4970(16), b = 5.4976(6), c = 10.7113(12) A, β=96.298(6)°, C6H8O6Zn, Mr = 241.50, V = 907.06(17) A^3, Z = 4, D, = 1.768 g/cm^3, F(000) = 488,μ = 2.703 mm^-1, S = 1.060, the final R = 0.0256 and wR = 0.0660 for 968 observed reflections with Ⅰ 〉 2σ(Ⅰ). Compound 2 crystallizes in triclinic, space group P1^- with a = 6.915(2), b = 7.166(2), c = 10.363(3) A, α = 73.250(4), β = 84.429(4), γ = 61.605(3)°, C16H2ON2O8Zn, Mr = 433.70, V = 432.1 (2) A^3, Z = 1, D, = 1.667 g/cm^3, F(000) = 224 and μ= 1.471 mm^-1, S = 1.118, the final R = 0.0486 and wR = 0.1077 for 1352 observed reflections with Ⅰ〉 2σ(Ⅰ). Upon using the assembly strategy of combination of coordination polymer chains with intermolecular hydrogen bonds, three-dimensional frameworks of complexes 1 and 2 were formed.展开更多
A zinc complex, [Zn(iso)_2(H_2O)_4](iso=C_6H_4NO_2^-), was synthesized and characterized by elemental analysis, thermal analysis and IR spectrum studies. The crystal structure of the complex was determined by X-ray di...A zinc complex, [Zn(iso)_2(H_2O)_4](iso=C_6H_4NO_2^-), was synthesized and characterized by elemental analysis, thermal analysis and IR spectrum studies. The crystal structure of the complex was determined by X-ray diffraction. The crystal crystallizes in the triclinic system, molecular formula ZnC12H16N2O8, Mr=381.64, space group P with a = 6.338(1), b =6.919(1), c=9.277(1), α=96.28(1), β=104.91(1), γ=112.85(1)°, V=352.12(9)?3, Z=1, Dc=1.80g?cm-3 and F(000)=196, μ =1.791mm-1. The crystal structure was solved by direct methods for final R=0.0204 and Rw=0.0542 for 1258 observed reflections with [Fo>4σ(Fo)]. The crystal structure reveals that zinc ion is trans-octahedral with two pyridyl nitrogens and two aque oxygens at the equational positions and two aqua oxygens at the axial positions. The complex forms a three-dimensional network through intermolecular hydrogen bonds.展开更多
The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H...The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H2O](bdc)}n which has been characterized by single- crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group P2/n with a = 7.0001(2), b = 11.5540(3), c = 11.4192(1) ? = 101.754(2)? V = 904.21(4) 3, Z = 2, C18H20MnN2O8, Mr = 447.30, Dc = 1.643 g/cm3, F(000) = 462 and m(MoK? = 0.783 mm-1. The final R and wR are 0.0499 and 0.1301, respectively for 1335 observed reflections with I ≥ 2(I). The Mn (Ⅱ) is six-coordinated in a distorted octahedral geometry. 4,4?Bipyridine in a m-bridge mode links [Mn(H2O)4]2+ into a linear cation chain. bdc acts as a counter anion and links the linear chains into a three-dimensional structure through hydrogen bonds.展开更多
Two novel polymeric complexes, [Gd(HsTCAS)(H2O)7]·4H2O 1 and [Gd(HsTCAS) (CH3COCH3)(H2O)6]·6H2O 2 (H4TCAS = p-sulfonatothiacalix[4]arene), have been synthesized and characterized by single-crysta...Two novel polymeric complexes, [Gd(HsTCAS)(H2O)7]·4H2O 1 and [Gd(HsTCAS) (CH3COCH3)(H2O)6]·6H2O 2 (H4TCAS = p-sulfonatothiacalix[4]arene), have been synthesized and characterized by single-crystal X-ray diffraction analyses. Complex 1 crystallizes in monoclinic, space group C2/m with a = 20.2308(12), b = 19.0894(10), c = 12.2448(7)A, β = 101.847(3)°, V = 4628.1(5)A^3, C24H43GdO27S8, Mr = 1169.25, Z = 4, Dc = 1.690 g/cm^3, F(000) = 2380,μ = 1.879 mm^-1, the final R = 0.0404 and wR = 0.1038 for 5127 observed reflections with I 〉 2σ(I). Complex 2 is pseudo-isostructural with complex 1.展开更多
A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·2C3H7OH·2H2O 1 (abo = R(-)-2-amino-1-butanol) has been synthesized from VO2^+ in organic solvents and its crystal structure was rep...A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·2C3H7OH·2H2O 1 (abo = R(-)-2-amino-1-butanol) has been synthesized from VO2^+ in organic solvents and its crystal structure was reported as follows: monoclinic, space group P21/n, a = 11.419(9), b = 16.811(16), c = 15.521(12) A, β= 102.98(2)°, V= 2903(4) A^3, Z = 4, C15H46N3O19V5, Mr = 827.25, Dc = 1.893 g/cm^3, 2(MoKα) = 0.71073 A, μ = 1.636 mm^-1, F(000) = 1696, the final R = 0.0696 and wR = 0.1361 for 4641 observed reflections with I 〉 2σ(I). The compound is based on decavanadate clusters [V10O28]^6-. The hydrogen bonding interactions among Habo^+ cations, solvents and decavanadate clusters extend 1 into a three-dimensional supramolecular architecture.展开更多
An inorganic-organic hybrid lanthanide selenidostannate [{Tb(en)3}2(μ-OH)2]Sn2Se6(1) was synthesized by the solvothermal method.1 crystallizes in the monoclinic system,space group P21/n with a=10.120(2),b=11....An inorganic-organic hybrid lanthanide selenidostannate [{Tb(en)3}2(μ-OH)2]Sn2Se6(1) was synthesized by the solvothermal method.1 crystallizes in the monoclinic system,space group P21/n with a=10.120(2),b=11.781(3),c=15.403(3),β=99.534(5)°,V=1811.1(7)3,Mr=1423.62,Z=2,Dc=2.611 g/cm3,μ=11.281 mm-1,F(000)=1312,S=1.101,the final R= 0.0400 and wR=0.0853 for 3242 observed reflections with Ⅰ 〉2σ(Ⅰ).1 consists of a [Sn2Se6]4-and a [{Tb(en)3}2(μ-OH)2]4+ ions.The [Sn2Se6]4-anion is constructed by two SnSe4 tetrahedra sharing a common edge.The binuclear [{Tb(en)3}2(μ-OH)2]4+ complex is composed of two [Tb(en)3]3+ ions joined by two μ-OH bridging ligands.The Tb3+ ion lies in an eight-coordinated bicapped trigonal prism.In 1,the [Sn2Se6]4-and [{Tb(en)3}2(μ-OH)2]4+ moieties are connected into a 3-D network via N-H···Se and O-H···Se H-bonds.展开更多
The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/...The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/cm3, μ(MoKa) = 0.081 cm-1 and F(000) = 536.00. The final R and wR are 0.0527 and 0.1285, respectively for 3058 observed reflections (I > 2σ(I)). In the title molecule, two phenyl rings are rotated oppositely with respect to the central part C(1)–C(2)=C(3)– C(4) (plane 3) and the dihedral angle between them is 14.8o. The phenone O(1) atom deviates from plane 3 by 0.291 ?. In the crystal the molecules form H-bond chains of R2 (6) and R2 (5) types 1 1 along [001]. The molecule chains interacted through three cooperative C–H…O H-bonds (R3 (11)) 1 in the ‘bay area’ (Fig. 3), extending along [010] and forming layer (100). Between the layers, there exist C–H/π interactions along [101]. Studies on the cooperative C–H…O H-bonds R3 (11) in the 1 similar crystals are also presented.展开更多
The title compound, 2-pyridinecarboxamide, C6H6N2O, crystallize in the monoclinic system with space group P21/n (No14), Z = 4, and unit cell parameters a = 5.2074(1) , b = 7.1004(1) , c = 16.2531(3) , = 100.260(1)o. T...The title compound, 2-pyridinecarboxamide, C6H6N2O, crystallize in the monoclinic system with space group P21/n (No14), Z = 4, and unit cell parameters a = 5.2074(1) , b = 7.1004(1) , c = 16.2531(3) , = 100.260(1)o. The crystal structure of the title compound, was reported previously from Weissenberg photographic data with R = 0.127. It has now been redetermined, providing a significant increase in the precision of the derived geometric parameters. The crystal packing is governed by N--HO hydrogen bond-type intermolecular interactions, forming infinite one-dimensional chains with graph-set notation C(4), R22(8) and R24(8).展开更多
The title compound [ClC6H4COCH2(C2H2N3)] has been prepared and characterized by elemental analysis, IR spectrum and X-ray studies. It crystallizes in the monoclinic system, space group P21/c with Mr = 221.64 (C10H8ClN...The title compound [ClC6H4COCH2(C2H2N3)] has been prepared and characterized by elemental analysis, IR spectrum and X-ray studies. It crystallizes in the monoclinic system, space group P21/c with Mr = 221.64 (C10H8ClN3O), a = 13.420(3), b = 9.720(2), c = 7.900(2) ? b = 92.00(3)? V = 1029.9(4) 3, Z = 4, Dc = 1.429 g/cm3, F(000) = 456, m = 0.345 mm-1, R = 0.0435 and wR=0.0894. The total reflections were 1949 and the independent ones were 1805 (Rint=0.0340), of which 800 were observed with I > 2s(I). The crystal structure consists of a-(1,2,4-triazol-1H- yl)-r-chloro-acetophenone. The existence of p conjugated systems in the molecule affects partly the bond lengths. The triazole and phenyl rings form the dihedral angle of 77.34. The molecules of the title compound connect to each other through extensive hydrogen bonds to form a two-dimensional structure. Elemental analysis and IR spectra are in good agreement with the structure data.展开更多
Bis(azidoacetamino)furazan (DAZAF) was synthesized and characterized by elemental analysis, IR, 1H NMR and MS as an energetic compound. The crystal structure of the title compound was determined by single-crystal X-ra...Bis(azidoacetamino)furazan (DAZAF) was synthesized and characterized by elemental analysis, IR, 1H NMR and MS as an energetic compound. The crystal structure of the title compound was determined by single-crystal X-ray diffraction with the following data: C6H6N10O3, monoclinic, P21/n, Z = 4, a = 8.402(3), b = 15.146(3), c = 9.247(3) ? ?= 111.09(2)? V = 1098.0(6) 3, Mr = 266.18, Dc = 1.610 g/cm3, F(000) = 544, ?=1.34 cm-1, R = 0.037 and wR = 0.044 for 2136 observed reflections (I > 2(I)). Intra- and inter-molecular hydrogen bonds were identified between the O and H atoms of two intramolecular acetylamino groups and two intermolecular acetylamino groups, respectively.展开更多
A new Schiff base compound, C13H9Br2N3O2CH3OH, isonicotinic acid [1-(3,5- dibromo-2-hydroxyphenyl)methylidene]hydrazide methanol, has been synthesized and characterized by elemental analysis, IR spectra, and single-...A new Schiff base compound, C13H9Br2N3O2CH3OH, isonicotinic acid [1-(3,5- dibromo-2-hydroxyphenyl)methylidene]hydrazide methanol, has been synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The compound comprises a Schiff base moiety isonicotinic acid [1-(3,5-dibromo-2-hydroxyphenyl) methylidene]hydrazide and a methanol molecule. The crystal belongs to the triclinic system, space group P1 with a = 8.464(1), b = 9.511(2), c = 10.901(2)A, a = 92.940(2), β = 110.456(2), y = 96.040(2)°, Z= 2, V= 814.0(2)A^3, Dc = 1.759 g/cm^3, Mr = 431.09, λ(MoKa) = 0.71073A, μ = 4.994 mm^-1, F(000) = 424, R = 0.0440 and wR = 0.1061. A total of 3284 unique reflections were collected, of which 2197 with I 〉 20(I) were observed. The molecule adopts a trans configuration about the C=N double bond. The dihedral angle between the benzene and pyridine rings is 22.0(4)°. The crystal structure is stabilized by intermolecular O-H…N and C-H…O hydrogen bonds, forming layers parallel to the ac plane. The preliminary biological tests show that the compound has potential antibacterial activities.展开更多
A new Zn(Ⅱ) complex,[Zn(1,2,3-HBTC)(L)]2(1,L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline and 1,2,3-H3 BTC = 1,2,3-benzentricarboxylic acid),was synthesized under hydrothermal conditi...A new Zn(Ⅱ) complex,[Zn(1,2,3-HBTC)(L)]2(1,L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline and 1,2,3-H3 BTC = 1,2,3-benzentricarboxylic acid),was synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction.It crystallizes in triclinic,space group P1 with a = 10.455(2),b = 11.533(2),c = 12.499(3) A,α = 116.97(3),β = 94.08(3),γ = 103.29(3)o,V = 1280.2(4) A^3,Z = 1,C56H28Cl2F2N8O12Zn2,Mr = 1244.50,Dc = 1.614 g/cm^3,F(000) = 628,μ(Mo Ka) = 1.124 mm^-1,R = 0.0502 and w R = 0.1417.In compound 1,two 1,2,3-HBTC anions bridge two Zn(Ⅱ) atoms to give a dimeric structure with Zn···Zn distance of 3.15 A.Adjacent dimers interact through π-π stackings between two L ligands to result in a supramolecular layer.Moreover,N–H···O and O–H···N hydrogen bonds further stabilize the 2D supramolecular architecture of 1.In addition,the luminescent property of 1 has been studied.展开更多
A new Cu(Ⅱ) complex [Cu(4-cba)(1,10-phen)(H2O)2](NO3) (4-Hcba = 4-cyanobenzoic acid) has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characteriz...A new Cu(Ⅱ) complex [Cu(4-cba)(1,10-phen)(H2O)2](NO3) (4-Hcba = 4-cyanobenzoic acid) has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single-crystal X-ray diffraction. Crystallographic data: C20H16CuN4O7, Mr= 487.91, triclinic, space group PI, a = 7.8420(2), b = 9.1070(2), c = 15.1140(6) A, a = 76.889(9), β = 81.332(11), γ = 74.844( 11)°, V = 1009.89(5) A^3, Z = 2, Dc = 1.605 g/cm^3, F(000) = 498, μ = 1.134 mm^-1, the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with 1 〉 2σ(Ⅰ). The Cu(Ⅱ) atom is coordinated by two terminal water molecules, one chelating 1,10-phen molecule and one monodentate 4-cba ligand to form a slightly distorted square pyramid. The title complex molecules are connected through hydrogen bonds and π-π stacking interactions to generate a 2D layered network. The thermogravimetric analysis of the title complex has also been discussed.展开更多
A new one-dimensional copper coordination polymer chain has been prepared and fully characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound { [Cu2(C2O4)2(inta)4](i...A new one-dimensional copper coordination polymer chain has been prepared and fully characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound { [Cu2(C2O4)2(inta)4](inta)}n 1 crystallizes in the triclinic system, space group P1, with a = 8.4722(5), b = 10.9825(6), c = 11.6128(6)A, α= 104.8050(10),β = 102.5740(10), γ= 109.6890(10)°, V= 927.18(9) A3, Mr = 929.79, Z = 1, Dc = 1.665 g/cm^3, F(000) = 475, μ = 1.231 mm^-1, R = 0.0453 and wR = 0.1185 for 3290 observed reflections (Ⅰ 〉 2σ(Ⅰ)). Of the compound, the Cu center is octahedrally coordinated with oxalate acting as a tetra-dentate ligand coordinated to the copper atom and each inta serving as a terminal ligand by employing only one N-donor to coordinate with the Cu center. An infinite {Cu2(C2O4)2}∞ chain is formed along the c axis. Furthermore, the 1D chains are held together via extensive hydrogen-bonding interactions to generate a three-dimensional network with 1D channels (ca. 5.491A×11.507A) where inta molecules are filled.展开更多
A new quinolyl substituted 1,2,4-triazole, 3-(p-methylphenyl)-4-phenyl-5-(2- quinolyl)-1,2,4-triazole (L) and its iron(II) complex cis-[FeLE(NCS)2] (1), have been successfully synthesized and characterized...A new quinolyl substituted 1,2,4-triazole, 3-(p-methylphenyl)-4-phenyl-5-(2- quinolyl)-1,2,4-triazole (L) and its iron(II) complex cis-[FeLE(NCS)2] (1), have been successfully synthesized and characterized by single-crystal X-ray diffraction. Both L and 1.Me2CO crystallize in monoclinic system but with different space groups: P21/c for L and C2/c for I.Me2CO. The L molecule is nonplanar and intermolecular C-H...N hydrogen bonds link two L molecules to form a dimer, which is further connected by intermolecular C-H...π interactions to produce 1D chains along the c axis. In complex 1-Me2CO, the iron(II) cation lies in a distorted octahedral environment with two cis-disposed NCS- ions. The L ligand coordinates via one triazole nitrogen and the quinolyl nitrogen. There is an intermolecular offset face-to-face π...π stacking interaction in the crystal packing of 1-Me2CO. 1 is the first complex with a quinolyl substituted 1,2,4-triazole.展开更多
The title compound, 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.05,9.03,11] dodecane (TAIW, C14H20N6O4, Mr = 336.36), has been synthesized by hydrogenolysis debenzylation of tetraacetyldibenzylhexaaza...The title compound, 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.05,9.03,11] dodecane (TAIW, C14H20N6O4, Mr = 336.36), has been synthesized by hydrogenolysis debenzylation of tetraacetyldibenzylhexaazaisowurtzitane (TADB) and its crystal structure was determined to be monoclinic, space group C2/c with a = 28.193(6), b = 12.139(2), c = 17.678(4) ?, β = 97.44(3)o, V = 5999(2) ?3, Z = 16, Dc = 1.490 g/cm3, F(000) = 2848, μ(MoKα) = 0.112 mm-1, R = 0.0631 and wR = 0.1586. X-ray investigations indicate that the molecule has different isomers and there exist intermolecular C–H…O hydrogen bonds in the crystal structure. The results of elemental analysis, IR and NMR spectroscopy are included.展开更多
A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and d...A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490(15), b = 7.0847(16), c = 30.845(3)A, β= 95.33(3)°, V = 1599.0(5)A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F(000) = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones (I 〉2σ(I)). In the crystal structure, mononuclear units [Cu(naphdien)]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.展开更多
2,9-Diformyl-l, 10-phenanthrolinebis(2,6-dimethylanil)cobalt(Ⅱ) perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space grou...2,9-Diformyl-l, 10-phenanthrolinebis(2,6-dimethylanil)cobalt(Ⅱ) perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group C2/c with a = 22.294(4), b = 15.122(3), c = 20.640(4) A, β = 119.618(4)°, V = 6048.9(19) A^3, C63H52Cl2CoN9O9, Mr= 1208.97, F(000) = 2504, De= 1.328g/cm^3, Z = 4, μ= 0.436, the final R = 0.0712 and wR = 0.1718 for 1734 observed reflections (I 〉 2σ(I)). In its solid state the helical polymeric chains are supramolecularly associated through intermolecular and interionic hydrogen bonding interactions.展开更多
A novel binuclear complex ([Cu^2(μ2-shed)(hshed)].(CIO4),H2O, h2shed = N-salicylidene-N'-(2-hydroxyethyl)ethylenediamine) has been synthesized and structurally characterized by X-ray diffraction analysis. ...A novel binuclear complex ([Cu^2(μ2-shed)(hshed)].(CIO4),H2O, h2shed = N-salicylidene-N'-(2-hydroxyethyl)ethylenediamine) has been synthesized and structurally characterized by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 12.511(10), b = 15.750(12), c = 14.281 (12) A, β = 100.564(14)°, C22H31CIN4O9Cu2, Mr = 658.04, V = 2766(4) A^3, Z = 4, Dc = 1.580 g/cm^3,μ(MoKα = 1.689 mm^-1, F(000) = 1352, the final R = 0.0528 and wR = 0.1433 for 4880 independent reflections with Rint = 0.0577. The complex is a binuclear copper compound, and two Cu(Ⅱ) ions in the binuclear cation are in different coordination environments. The Cu(1) ion adopts a distorted square pyramidal geometry (x = 0.22) with four donor atoms (N2O2) of the ligand in the basal plane, and one hydroxyl oxygen atom with protonated form occupying the apical position. The Cu(2) ion assumes the geometry of a distorted square plane with four donor atoms (N2O2) of the ligand. The Cu...Cu separation is 3.103 A,. In addition, N-H…O and C-H…O intermolecular hydrogen bonding interactions link these binuclear cations into a quasi one-dimensional chain along the a axis.展开更多
The title compound, 4-salicylimine-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole, was obtained by the condensation reaction of 4-amino-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole with salicylaldehyde in methanol. The crys...The title compound, 4-salicylimine-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole, was obtained by the condensation reaction of 4-amino-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole with salicylaldehyde in methanol. The crystal structure (C21H16N4O3, Mr = 372.38) belongs to monoclinic system, space group P21/n with a = 10.507(2), b = 16.878(3), c = 11.199(2) ? = 110.86(3), V = 1855.9(6) ?, Z = 4, Dc = 1.333 g/cm3, F(000) = 776, (MoK? = 0.092 mm-1, R = 0.0552 and wR = 0.1095 for 1920 reflections ( I > 2.0(I) ). The analytical results of crystal structure show that there are two different non-covalent interactions in the compound. One is hydrogen bond, and the other p-p stacking interaction. These two types of non-covalent interactions play an important role in the packing of crystal.展开更多
基金This work was supported by the National Natural Science Foundation of China (No. 20231020)
文摘Two zinc(Ⅱ) compounds, [Zn(L)(H2O)2]n 1 and [Zn(4,4'-bpy)(H2O)4](L) 2 (H2L = trans,trans-1,3 butadiene 1,4-dicarboxylic acid), were synthesized by hydrothermal methods and characterized by single-crystal X-ray diffraction analyses. Compound 1 crystallizes in monoclinic, space group C2/c with a=15.4970(16), b = 5.4976(6), c = 10.7113(12) A, β=96.298(6)°, C6H8O6Zn, Mr = 241.50, V = 907.06(17) A^3, Z = 4, D, = 1.768 g/cm^3, F(000) = 488,μ = 2.703 mm^-1, S = 1.060, the final R = 0.0256 and wR = 0.0660 for 968 observed reflections with Ⅰ 〉 2σ(Ⅰ). Compound 2 crystallizes in triclinic, space group P1^- with a = 6.915(2), b = 7.166(2), c = 10.363(3) A, α = 73.250(4), β = 84.429(4), γ = 61.605(3)°, C16H2ON2O8Zn, Mr = 433.70, V = 432.1 (2) A^3, Z = 1, D, = 1.667 g/cm^3, F(000) = 224 and μ= 1.471 mm^-1, S = 1.118, the final R = 0.0486 and wR = 0.1077 for 1352 observed reflections with Ⅰ〉 2σ(Ⅰ). Upon using the assembly strategy of combination of coordination polymer chains with intermolecular hydrogen bonds, three-dimensional frameworks of complexes 1 and 2 were formed.
文摘A zinc complex, [Zn(iso)_2(H_2O)_4](iso=C_6H_4NO_2^-), was synthesized and characterized by elemental analysis, thermal analysis and IR spectrum studies. The crystal structure of the complex was determined by X-ray diffraction. The crystal crystallizes in the triclinic system, molecular formula ZnC12H16N2O8, Mr=381.64, space group P with a = 6.338(1), b =6.919(1), c=9.277(1), α=96.28(1), β=104.91(1), γ=112.85(1)°, V=352.12(9)?3, Z=1, Dc=1.80g?cm-3 and F(000)=196, μ =1.791mm-1. The crystal structure was solved by direct methods for final R=0.0204 and Rw=0.0542 for 1258 observed reflections with [Fo>4σ(Fo)]. The crystal structure reveals that zinc ion is trans-octahedral with two pyridyl nitrogens and two aque oxygens at the equational positions and two aqua oxygens at the axial positions. The complex forms a three-dimensional network through intermolecular hydrogen bonds.
基金supported by the National Natural Science Foundation of China (No. 29890210) and the Key Project of the Chinese Academy of Sciences (KJCX2-H3)
文摘The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H2O](bdc)}n which has been characterized by single- crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group P2/n with a = 7.0001(2), b = 11.5540(3), c = 11.4192(1) ? = 101.754(2)? V = 904.21(4) 3, Z = 2, C18H20MnN2O8, Mr = 447.30, Dc = 1.643 g/cm3, F(000) = 462 and m(MoK? = 0.783 mm-1. The final R and wR are 0.0499 and 0.1301, respectively for 1335 observed reflections with I ≥ 2(I). The Mn (Ⅱ) is six-coordinated in a distorted octahedral geometry. 4,4?Bipyridine in a m-bridge mode links [Mn(H2O)4]2+ into a linear cation chain. bdc acts as a counter anion and links the linear chains into a three-dimensional structure through hydrogen bonds.
基金This work was supported by the National Natural Science Foundation of China,Natural Science Foundation of Fujian Province,and the Young Scientist Funds of Fujian Province (No. 2006F3130)
文摘Two novel polymeric complexes, [Gd(HsTCAS)(H2O)7]·4H2O 1 and [Gd(HsTCAS) (CH3COCH3)(H2O)6]·6H2O 2 (H4TCAS = p-sulfonatothiacalix[4]arene), have been synthesized and characterized by single-crystal X-ray diffraction analyses. Complex 1 crystallizes in monoclinic, space group C2/m with a = 20.2308(12), b = 19.0894(10), c = 12.2448(7)A, β = 101.847(3)°, V = 4628.1(5)A^3, C24H43GdO27S8, Mr = 1169.25, Z = 4, Dc = 1.690 g/cm^3, F(000) = 2380,μ = 1.879 mm^-1, the final R = 0.0404 and wR = 0.1038 for 5127 observed reflections with I 〉 2σ(I). Complex 2 is pseudo-isostructural with complex 1.
基金This work was supported by the National Natural Science Foundation of China and Natural Science Foundation of Fujian Province
文摘A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·2C3H7OH·2H2O 1 (abo = R(-)-2-amino-1-butanol) has been synthesized from VO2^+ in organic solvents and its crystal structure was reported as follows: monoclinic, space group P21/n, a = 11.419(9), b = 16.811(16), c = 15.521(12) A, β= 102.98(2)°, V= 2903(4) A^3, Z = 4, C15H46N3O19V5, Mr = 827.25, Dc = 1.893 g/cm^3, 2(MoKα) = 0.71073 A, μ = 1.636 mm^-1, F(000) = 1696, the final R = 0.0696 and wR = 0.1361 for 4641 observed reflections with I 〉 2σ(I). The compound is based on decavanadate clusters [V10O28]^6-. The hydrogen bonding interactions among Habo^+ cations, solvents and decavanadate clusters extend 1 into a three-dimensional supramolecular architecture.
基金Supported by the National Natural Science Foundation of China (No. 20771077)
文摘An inorganic-organic hybrid lanthanide selenidostannate [{Tb(en)3}2(μ-OH)2]Sn2Se6(1) was synthesized by the solvothermal method.1 crystallizes in the monoclinic system,space group P21/n with a=10.120(2),b=11.781(3),c=15.403(3),β=99.534(5)°,V=1811.1(7)3,Mr=1423.62,Z=2,Dc=2.611 g/cm3,μ=11.281 mm-1,F(000)=1312,S=1.101,the final R= 0.0400 and wR=0.0853 for 3242 observed reflections with Ⅰ 〉2σ(Ⅰ).1 consists of a [Sn2Se6]4-and a [{Tb(en)3}2(μ-OH)2]4+ ions.The [Sn2Se6]4-anion is constructed by two SnSe4 tetrahedra sharing a common edge.The binuclear [{Tb(en)3}2(μ-OH)2]4+ complex is composed of two [Tb(en)3]3+ ions joined by two μ-OH bridging ligands.The Tb3+ ion lies in an eight-coordinated bicapped trigonal prism.In 1,the [Sn2Se6]4-and [{Tb(en)3}2(μ-OH)2]4+ moieties are connected into a 3-D network via N-H···Se and O-H···Se H-bonds.
基金This research was supported by the Key Subject Foundation of Jiangsu Province(S1109001)
文摘The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/cm3, μ(MoKa) = 0.081 cm-1 and F(000) = 536.00. The final R and wR are 0.0527 and 0.1285, respectively for 3058 observed reflections (I > 2σ(I)). In the title molecule, two phenyl rings are rotated oppositely with respect to the central part C(1)–C(2)=C(3)– C(4) (plane 3) and the dihedral angle between them is 14.8o. The phenone O(1) atom deviates from plane 3 by 0.291 ?. In the crystal the molecules form H-bond chains of R2 (6) and R2 (5) types 1 1 along [001]. The molecule chains interacted through three cooperative C–H…O H-bonds (R3 (11)) 1 in the ‘bay area’ (Fig. 3), extending along [010] and forming layer (100). Between the layers, there exist C–H/π interactions along [101]. Studies on the cooperative C–H…O H-bonds R3 (11) in the 1 similar crystals are also presented.
文摘The title compound, 2-pyridinecarboxamide, C6H6N2O, crystallize in the monoclinic system with space group P21/n (No14), Z = 4, and unit cell parameters a = 5.2074(1) , b = 7.1004(1) , c = 16.2531(3) , = 100.260(1)o. The crystal structure of the title compound, was reported previously from Weissenberg photographic data with R = 0.127. It has now been redetermined, providing a significant increase in the precision of the derived geometric parameters. The crystal packing is governed by N--HO hydrogen bond-type intermolecular interactions, forming infinite one-dimensional chains with graph-set notation C(4), R22(8) and R24(8).
基金This work was supported by the Educational Administration Key Project of Shandong province (No.J01C05) and Natural Science Foundation of Shandong province (No.Y2002B06)
文摘The title compound [ClC6H4COCH2(C2H2N3)] has been prepared and characterized by elemental analysis, IR spectrum and X-ray studies. It crystallizes in the monoclinic system, space group P21/c with Mr = 221.64 (C10H8ClN3O), a = 13.420(3), b = 9.720(2), c = 7.900(2) ? b = 92.00(3)? V = 1029.9(4) 3, Z = 4, Dc = 1.429 g/cm3, F(000) = 456, m = 0.345 mm-1, R = 0.0435 and wR=0.0894. The total reflections were 1949 and the independent ones were 1805 (Rint=0.0340), of which 800 were observed with I > 2s(I). The crystal structure consists of a-(1,2,4-triazol-1H- yl)-r-chloro-acetophenone. The existence of p conjugated systems in the molecule affects partly the bond lengths. The triazole and phenyl rings form the dihedral angle of 77.34. The molecules of the title compound connect to each other through extensive hydrogen bonds to form a two-dimensional structure. Elemental analysis and IR spectra are in good agreement with the structure data.
文摘Bis(azidoacetamino)furazan (DAZAF) was synthesized and characterized by elemental analysis, IR, 1H NMR and MS as an energetic compound. The crystal structure of the title compound was determined by single-crystal X-ray diffraction with the following data: C6H6N10O3, monoclinic, P21/n, Z = 4, a = 8.402(3), b = 15.146(3), c = 9.247(3) ? ?= 111.09(2)? V = 1098.0(6) 3, Mr = 266.18, Dc = 1.610 g/cm3, F(000) = 544, ?=1.34 cm-1, R = 0.037 and wR = 0.044 for 2136 observed reflections (I > 2(I)). Intra- and inter-molecular hydrogen bonds were identified between the O and H atoms of two intramolecular acetylamino groups and two intermolecular acetylamino groups, respectively.
文摘A new Schiff base compound, C13H9Br2N3O2CH3OH, isonicotinic acid [1-(3,5- dibromo-2-hydroxyphenyl)methylidene]hydrazide methanol, has been synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The compound comprises a Schiff base moiety isonicotinic acid [1-(3,5-dibromo-2-hydroxyphenyl) methylidene]hydrazide and a methanol molecule. The crystal belongs to the triclinic system, space group P1 with a = 8.464(1), b = 9.511(2), c = 10.901(2)A, a = 92.940(2), β = 110.456(2), y = 96.040(2)°, Z= 2, V= 814.0(2)A^3, Dc = 1.759 g/cm^3, Mr = 431.09, λ(MoKa) = 0.71073A, μ = 4.994 mm^-1, F(000) = 424, R = 0.0440 and wR = 0.1061. A total of 3284 unique reflections were collected, of which 2197 with I 〉 20(I) were observed. The molecule adopts a trans configuration about the C=N double bond. The dihedral angle between the benzene and pyridine rings is 22.0(4)°. The crystal structure is stabilized by intermolecular O-H…N and C-H…O hydrogen bonds, forming layers parallel to the ac plane. The preliminary biological tests show that the compound has potential antibacterial activities.
基金Supported by the Institute Foundation of Siping City(No.2013036)
文摘A new Zn(Ⅱ) complex,[Zn(1,2,3-HBTC)(L)]2(1,L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline and 1,2,3-H3 BTC = 1,2,3-benzentricarboxylic acid),was synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction.It crystallizes in triclinic,space group P1 with a = 10.455(2),b = 11.533(2),c = 12.499(3) A,α = 116.97(3),β = 94.08(3),γ = 103.29(3)o,V = 1280.2(4) A^3,Z = 1,C56H28Cl2F2N8O12Zn2,Mr = 1244.50,Dc = 1.614 g/cm^3,F(000) = 628,μ(Mo Ka) = 1.124 mm^-1,R = 0.0502 and w R = 0.1417.In compound 1,two 1,2,3-HBTC anions bridge two Zn(Ⅱ) atoms to give a dimeric structure with Zn···Zn distance of 3.15 A.Adjacent dimers interact through π-π stackings between two L ligands to result in a supramolecular layer.Moreover,N–H···O and O–H···N hydrogen bonds further stabilize the 2D supramolecular architecture of 1.In addition,the luminescent property of 1 has been studied.
基金This work was supported by the NSF for Distinguished Young Scientist of China (20425104) and the NSF of Fujian Province (A0420002, 2005I017)
文摘A new Cu(Ⅱ) complex [Cu(4-cba)(1,10-phen)(H2O)2](NO3) (4-Hcba = 4-cyanobenzoic acid) has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single-crystal X-ray diffraction. Crystallographic data: C20H16CuN4O7, Mr= 487.91, triclinic, space group PI, a = 7.8420(2), b = 9.1070(2), c = 15.1140(6) A, a = 76.889(9), β = 81.332(11), γ = 74.844( 11)°, V = 1009.89(5) A^3, Z = 2, Dc = 1.605 g/cm^3, F(000) = 498, μ = 1.134 mm^-1, the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with 1 〉 2σ(Ⅰ). The Cu(Ⅱ) atom is coordinated by two terminal water molecules, one chelating 1,10-phen molecule and one monodentate 4-cba ligand to form a slightly distorted square pyramid. The title complex molecules are connected through hydrogen bonds and π-π stacking interactions to generate a 2D layered network. The thermogravimetric analysis of the title complex has also been discussed.
基金the Education Office of Jilin Province (No. 0047)
文摘A new one-dimensional copper coordination polymer chain has been prepared and fully characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound { [Cu2(C2O4)2(inta)4](inta)}n 1 crystallizes in the triclinic system, space group P1, with a = 8.4722(5), b = 10.9825(6), c = 11.6128(6)A, α= 104.8050(10),β = 102.5740(10), γ= 109.6890(10)°, V= 927.18(9) A3, Mr = 929.79, Z = 1, Dc = 1.665 g/cm^3, F(000) = 475, μ = 1.231 mm^-1, R = 0.0453 and wR = 0.1185 for 3290 observed reflections (Ⅰ 〉 2σ(Ⅰ)). Of the compound, the Cu center is octahedrally coordinated with oxalate acting as a tetra-dentate ligand coordinated to the copper atom and each inta serving as a terminal ligand by employing only one N-donor to coordinate with the Cu center. An infinite {Cu2(C2O4)2}∞ chain is formed along the c axis. Furthermore, the 1D chains are held together via extensive hydrogen-bonding interactions to generate a three-dimensional network with 1D channels (ca. 5.491A×11.507A) where inta molecules are filled.
基金funded by the National Natural Science Foundation of China(Nos.20771059,21171093)the scientific innovation research of college graduate in Jiangsu Province(CXZZ12-0436)the State Key Laboratory of Materials-oriented Chemical Engineering(KL11-03)
文摘A new quinolyl substituted 1,2,4-triazole, 3-(p-methylphenyl)-4-phenyl-5-(2- quinolyl)-1,2,4-triazole (L) and its iron(II) complex cis-[FeLE(NCS)2] (1), have been successfully synthesized and characterized by single-crystal X-ray diffraction. Both L and 1.Me2CO crystallize in monoclinic system but with different space groups: P21/c for L and C2/c for I.Me2CO. The L molecule is nonplanar and intermolecular C-H...N hydrogen bonds link two L molecules to form a dimer, which is further connected by intermolecular C-H...π interactions to produce 1D chains along the c axis. In complex 1-Me2CO, the iron(II) cation lies in a distorted octahedral environment with two cis-disposed NCS- ions. The L ligand coordinates via one triazole nitrogen and the quinolyl nitrogen. There is an intermolecular offset face-to-face π...π stacking interaction in the crystal packing of 1-Me2CO. 1 is the first complex with a quinolyl substituted 1,2,4-triazole.
基金The project was supported by the National DefenceAdvanced Research Foundation of COSTIND (1206045186)
文摘The title compound, 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.05,9.03,11] dodecane (TAIW, C14H20N6O4, Mr = 336.36), has been synthesized by hydrogenolysis debenzylation of tetraacetyldibenzylhexaazaisowurtzitane (TADB) and its crystal structure was determined to be monoclinic, space group C2/c with a = 28.193(6), b = 12.139(2), c = 17.678(4) ?, β = 97.44(3)o, V = 5999(2) ?3, Z = 16, Dc = 1.490 g/cm3, F(000) = 2848, μ(MoKα) = 0.112 mm-1, R = 0.0631 and wR = 0.1586. X-ray investigations indicate that the molecule has different isomers and there exist intermolecular C–H…O hydrogen bonds in the crystal structure. The results of elemental analysis, IR and NMR spectroscopy are included.
基金This work was supported by the National Natural Science Foundation of China (Nos. 20671011, 20331010, 90406002 and 90406024)the 111 Project (B07012) and Key Laboratory of Structural Chemistry Foundation (No. 060017)
文摘A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490(15), b = 7.0847(16), c = 30.845(3)A, β= 95.33(3)°, V = 1599.0(5)A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F(000) = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones (I 〉2σ(I)). In the crystal structure, mononuclear units [Cu(naphdien)]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.
文摘2,9-Diformyl-l, 10-phenanthrolinebis(2,6-dimethylanil)cobalt(Ⅱ) perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group C2/c with a = 22.294(4), b = 15.122(3), c = 20.640(4) A, β = 119.618(4)°, V = 6048.9(19) A^3, C63H52Cl2CoN9O9, Mr= 1208.97, F(000) = 2504, De= 1.328g/cm^3, Z = 4, μ= 0.436, the final R = 0.0712 and wR = 0.1718 for 1734 observed reflections (I 〉 2σ(I)). In its solid state the helical polymeric chains are supramolecularly associated through intermolecular and interionic hydrogen bonding interactions.
文摘A novel binuclear complex ([Cu^2(μ2-shed)(hshed)].(CIO4),H2O, h2shed = N-salicylidene-N'-(2-hydroxyethyl)ethylenediamine) has been synthesized and structurally characterized by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 12.511(10), b = 15.750(12), c = 14.281 (12) A, β = 100.564(14)°, C22H31CIN4O9Cu2, Mr = 658.04, V = 2766(4) A^3, Z = 4, Dc = 1.580 g/cm^3,μ(MoKα = 1.689 mm^-1, F(000) = 1352, the final R = 0.0528 and wR = 0.1433 for 4880 independent reflections with Rint = 0.0577. The complex is a binuclear copper compound, and two Cu(Ⅱ) ions in the binuclear cation are in different coordination environments. The Cu(1) ion adopts a distorted square pyramidal geometry (x = 0.22) with four donor atoms (N2O2) of the ligand in the basal plane, and one hydroxyl oxygen atom with protonated form occupying the apical position. The Cu(2) ion assumes the geometry of a distorted square plane with four donor atoms (N2O2) of the ligand. The Cu...Cu separation is 3.103 A,. In addition, N-H…O and C-H…O intermolecular hydrogen bonding interactions link these binuclear cations into a quasi one-dimensional chain along the a axis.
文摘The title compound, 4-salicylimine-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole, was obtained by the condensation reaction of 4-amino-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole with salicylaldehyde in methanol. The crystal structure (C21H16N4O3, Mr = 372.38) belongs to monoclinic system, space group P21/n with a = 10.507(2), b = 16.878(3), c = 11.199(2) ? = 110.86(3), V = 1855.9(6) ?, Z = 4, Dc = 1.333 g/cm3, F(000) = 776, (MoK? = 0.092 mm-1, R = 0.0552 and wR = 0.1095 for 1920 reflections ( I > 2.0(I) ). The analytical results of crystal structure show that there are two different non-covalent interactions in the compound. One is hydrogen bond, and the other p-p stacking interaction. These two types of non-covalent interactions play an important role in the packing of crystal.