A new metal-organic complex Co2(cbba)4(phen)2(μ2-OH2)(H2cbba=2-(4'-chlorine-benzoyl)benzoic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and struc-turally characterized by single-cr...A new metal-organic complex Co2(cbba)4(phen)2(μ2-OH2)(H2cbba=2-(4'-chlorine-benzoyl)benzoic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and struc-turally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.7659(7),b=17.1856(11),c=19.2022(13),α=83.8120(10),β=84.9930(10),γ=87.2070(10)°,V=3515.8(4)3,C80H50Cl4Co2N4O13,Mr=1534.90,Dc=1.450 g/cm3,μ(MoKα)=0.693 mm-1,F(000)=1568,Z=2,the final R=0.0490 and wR=0.1092 for 8216 observed reflections(Ⅰ 〉2σ(Ⅰ)).In the crystal structure,the cobalt atom is six-coordinated with three carboxylate oxygen atoms from three different cbba ligands,one oxygen atom from coordinated water molecule and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry.Furthermore,it exhibits a 3D supramolecular network through π-π and hydrogen bonding interactions.展开更多
A novel layered mixed metal vanadium-cobadt complex, (py)5Co2(H2O)3[V4O12] 1 (py = pyridine), was hydro(solvo)thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in ort...A novel layered mixed metal vanadium-cobadt complex, (py)5Co2(H2O)3[V4O12] 1 (py = pyridine), was hydro(solvo)thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pca21 with a = 17.473(4), b = 11.447(2), c = 17.509(4)A^°, V = 5005.3(7)A^°3, Z = 4, Mr = 3502.1(12), Z = 4, Dc = 1.827 g/cm^3,μ(MoKα) = 2.023 mm^-1, F(000) = 1928, S = 1.020, the final R = 0.0400 and wR= 0.1063 for 6035 observed reflections with I 〉 2σ(I) and 460 variables. Complex 1 consists of tetrahedral VO4 groups to form the large layers which are alternately bonded by two cobalt complex species Co(py)2(H2O)2 and Co(py)3(H2O).展开更多
A new metal-organic coordination polymer [Co(2-pya)2(4,4'-bipy)]2n-[(4,4'- bipy)0.5· H2O]2n (2-pya = 2-pyridinecarboxylic acid, 4,4'-bipy = 4,4'-bipyridine) 1 has been hydrothermally synthesized and s...A new metal-organic coordination polymer [Co(2-pya)2(4,4'-bipy)]2n-[(4,4'- bipy)0.5· H2O]2n (2-pya = 2-pyridinecarboxylic acid, 4,4'-bipy = 4,4'-bipyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I41/a with a = b = 22.719(2), c = 10.710(2)/k, V = 5527.8(14) A3, C54H46N10Co2O10, Mr= 1112.87, Dc = 1.337 g/cm3,μ(MoKa) = 0.665 mm-1, F(000) = 2296, Z = 4, the final R = 0.0633 and wR = 0.1096 for 1261 observed reflections (I 〉 2σ(I)). It exhibits a one-dimensional chain-like structure constructed by mixed ligands of 2-pyridinedicarboxylic acid and 4,4'-bipyridine.展开更多
A novel dinuclear complex with an empirical formula [Co2(1H-benzimidazole)4(1, 4-bdoa)2] (1,4-bdoa2– = benzene-1,4-dioxyacetate dianion) has been synthesized and characterized by elemental analysis, IR and single-cry...A novel dinuclear complex with an empirical formula [Co2(1H-benzimidazole)4(1, 4-bdoa)2] (1,4-bdoa2– = benzene-1,4-dioxyacetate dianion) has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 11.000(2), b = 19.385(4), c = 11.417(2) ?, β = 95.49(3)o, V = 2423.3(8) ?3, Z = 2, Mr = 1074.77, Dc = 1.473 g/cm3, μ = 0.760 mm–1, F(000) = 1108, the final R = 0.0645 and wR = 0.0714 for 3273 observed reflections (I > 2σ(I)). Two octahedrally coordinated Co(II) atoms are bridged by two 1,4-bdoa2– groups, generating a macrocyclic ring complex. The Co…Co separa- tion is 7.677(3) ?. An extended 3-D supramolecular network is formed through hydrogen bonds and weak π-π stacking interactions.展开更多
A new mononuclear cobalt(Ⅲ) complex [Co(dpa)2(Gly)](ClO4)2-4H2O was synthesized by the reaction of Co^2+, glycine (gly) and 2,2"-dipyridylamine (dpa) in a methanol-water solution, and its structure was ...A new mononuclear cobalt(Ⅲ) complex [Co(dpa)2(Gly)](ClO4)2-4H2O was synthesized by the reaction of Co^2+, glycine (gly) and 2,2"-dipyridylamine (dpa) in a methanol-water solution, and its structure was characterized by IR, EA, ES-MS and X-ray structure analysis. The compound crystallizes in the monoclinic system, space group P21/n with a = 12.8795(2), b = 13.2904(2), c = 19.1104(2)A, β= 109.378(1)°, V = 3085.89(8)A^3, Z = 4, Mr = 746.36, Dc = 1.606 g/cm^3, μ= 0.808 mm^-1, F(000) = 1536, the final R = 0.0543 and wR = 0.1306 for 5393 independent reflections. The magnetic measurement of the compound at room temperature shows that it is diamagnetic and the cobalt ion is in low spin +3 oxidation state. ES-MS experiments show that the [Co(dpa)E(Gly)]^2+ cation is very stable in the methanol solution.展开更多
A dinuclear cobalt(II) complex [Co2(a-furacrylato)4(Phen)2(H20)]'C2HsOH has been synthesized with a-furacrylic acid and 1,10-phenanthroline as the ligands, and its crystal structure was determined. The crysta...A dinuclear cobalt(II) complex [Co2(a-furacrylato)4(Phen)2(H20)]'C2HsOH has been synthesized with a-furacrylic acid and 1,10-phenanthroline as the ligands, and its crystal structure was determined. The crystal is of monoclinic system, space group C2/c with a = 1.07388(8), b = 2.4300(2), c = 1.86708(14) nm, β= 104.3830(10)°, V= 4.719.4(7) nm3, Dc = 1.503 g/cm3, Z = 2, F(000) = 2196, GOOF = 1.053, the final R = 0.0343 and wR = 0.0883. The crystal structure shows that two neighboring cobalt(II) ions are linked by the bridging coordination of two a-furacrylic acid anions and one water molecule, and their end positions are respectively coordinated with two 1,10-phenanthroline molecules and two a-furacrylic acid anions, forming a dinuclear structure. Both cobalt(II) ions adopt hexa-coordinated distorted octahedral geometry. The electrochemical and fluorescence properties of the title complex are also discussed.展开更多
A new cobalt complex Co(C10H8N2)(H2O)3[C9H11O2(COO)] with methy-5-norbor- nene-2,3-dicarboxylic anhydride acid (MNA) and 2,2'-bipyridine as ligands has been synthesized in the mixed solvents of ethanol and wa...A new cobalt complex Co(C10H8N2)(H2O)3[C9H11O2(COO)] with methy-5-norbor- nene-2,3-dicarboxylic anhydride acid (MNA) and 2,2'-bipyridine as ligands has been synthesized in the mixed solvents of ethanol and water. It crystallizes in monoclinic, space group P21/c with α = 13.0430(13), b = 21.014(2), c = 7.5151(7) ?, β = 102.319(2)o, V = 2012.4(3) A3, Dc = 1.529 g/cm3, Z = 4, F(000) = 964, GOOF = 1.051, the final R= 0.0457 and wR= 0.0974. The crystal structure shows that the cobalt ion is coordinated with four oxygen atoms from one MNA molecule and three water molecules together with two nitrogen atoms from the 2,2'-bipyridine molecule, forming a distorted octahedral coordination geometry. The thermal stabilityand electrochemical properties have studied in this paper.展开更多
Two new cobalt(Ⅱ)complexes[Co2(2,2?-bipy)2(dpa)2(H2O)5]·4H2O(1)and Co(2,2?-bipy)3(SO4)]·7.5H2O(2)have been synthesized with diaphonic acid(H2dpa)and 2,2?-bipyridine(2,2?-bipy)as ligands.In 1,two neighboring...Two new cobalt(Ⅱ)complexes[Co2(2,2?-bipy)2(dpa)2(H2O)5]·4H2O(1)and Co(2,2?-bipy)3(SO4)]·7.5H2O(2)have been synthesized with diaphonic acid(H2dpa)and 2,2?-bipyridine(2,2?-bipy)as ligands.In 1,two neighboring cobalt(Ⅱ)ions are linked together by one bridging diaphonic acid group,forming an asymmetric dinuclear structure.1 crystallizes in triclinic,space group P1 with a=9.825(6),b=13.007(8),c=19.586(1)A,α=80.773(1)o,β=77.065(1)o,γ=85.902(1)o,Mr=431.4,V=2406.5(3)A^3,Dc=1.48 g/cm^3,Z=2,μ(Mo Kα)=0.767 mm-1,F(000)=1112,the final R=0.0379 and wR=0.0862.The central cobalt(Ⅱ)ions in 1 and 2 are coordinated with six atoms,forming distorted octahedral coordination geometry.The fluorescence and thermal stability properties of 1 and 2 are also reported.展开更多
The reaction of Co(OAc)2 with bpe and 4,4?-dpdo in an aqueous-alcohol solution affords the formation of red crystals of [Co(H2O)2(bpe)(OAc)2]?4,4?-dpdo (bpe = trans-1,2-bis(4- pyridyl)ethylene, 4,4?-dpdo = 4,4?-dipyri...The reaction of Co(OAc)2 with bpe and 4,4?-dpdo in an aqueous-alcohol solution affords the formation of red crystals of [Co(H2O)2(bpe)(OAc)2]?4,4?-dpdo (bpe = trans-1,2-bis(4- pyridyl)ethylene, 4,4?-dpdo = 4,4?-dipyridyl N,N?-oxide). The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 7.6146(9), b = 8.6691(11), c = 10.3440(11) ?, α = 88.311(3), β = 76.992(3), γ = 75.809(3)°, V = 644.76(13) ?3, Z = 1, C26H28CoN4O8, Mr = 583.45, Dc = 1.503 g/cm3, μ = 0.724 mm-1, F(000) = 303, T = 223(2) K, the final R = 0.0477 and wR = 0.1177 for 3199 observed reflections with I > 2σ(I). In the crystal the cobalt atom is six-coordinated by oxygen atoms from two carboxylic molecules, two nitrogen atoms from the bpe ligands and two water molecules, completing an octahedral geometry. The structure of the title complex consists of neutral chains containing cobalt(II) ions bridged by mutually trans bpe molecules. The adjacent chains are connected through weak hydrogen bonds to form a two-dimensional structure.展开更多
Reaction of cobalt carbonate, pivalic acid and quinoline in a refluxing ethanol solvent yielded the dicobalt(Ⅱ) compound, Co 2(O 2CCMe 3) 4(C 9H 7N) 2 (1) (C 9H 7N is quinoline), which has been characterised...Reaction of cobalt carbonate, pivalic acid and quinoline in a refluxing ethanol solvent yielded the dicobalt(Ⅱ) compound, Co 2(O 2CCMe 3) 4(C 9H 7N) 2 (1) (C 9H 7N is quinoline), which has been characterised by elemental analysis, IR and X ray diffraction method. Crystallographic data: monoclinic, P2 1/a, a=9.341(2), b=18.591(4), c=11.822(2) , β=97.71(2), V=2034(1) 3, Z=2, M r=918.19, D c =1.27 g/cm -3 , F(000)=820, μ (Mo Kα )=8.60 cm -1 , T =293K, final R=0 049, R w =0.060 for 2715 observed reflections with I】3.0 σ(I) . The centrosymmetric molecule comprises a pair of cobalt(Ⅱ) atoms connected by four pivalate ligands in syn syn bridging modes. Square pyramidal five coordination of cobalt(Ⅱ) is further completed by a quimoline molecule. The Co Ⅱ-Co Ⅱ distance is 2.784(1) .展开更多
Two new coordination polymers [Co(oba)(mbix)]2n·nH2O (1) and [Mn(Hoba)2(H2O)2]n (2) (H2oba = 4,4'-oxydibenzoic acid, mbix = 1,3-bis(imidazol-1-ylmethyl)benzene) have been successfully synthesized...Two new coordination polymers [Co(oba)(mbix)]2n·nH2O (1) and [Mn(Hoba)2(H2O)2]n (2) (H2oba = 4,4'-oxydibenzoic acid, mbix = 1,3-bis(imidazol-1-ylmethyl)benzene) have been successfully synthesized under hydrothermal conditions. Their structures have been determined by elemental analyses, IR spectroscopy, UV and single-crystal X-ray diffraction analysis. The intermolecular hydrogen bonding and π-π stacking interactions extend the complexes into a 3D supramolecular structure.展开更多
A novel cuprous azide complex with the formula of [Cu2(dmpz)(N3)2]n(1, dmpz: 2,6-dimethylpyrazine) has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characteriz...A novel cuprous azide complex with the formula of [Cu2(dmpz)(N3)2]n(1, dmpz: 2,6-dimethylpyrazine) has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characterized by single-crystal X-ray diffraction method. Single-crystal X-ray diffraction analysis reveals the title complex represents a three-dimensional network structure featuring 2D [Cu N3]n plane units bridged by bridging dmpz ligands to form a 3D network. Research results reveal that 1 has lower impact sensitivity and friction sensitivity, which may be expected to become insensitive energetic material and have potential applications. Crystal data: monoclinic, space group C2/c, a = 17.8599(15), b = 8.2889(5), c = 14.8076(14) A, β = 113.2580(10)o, V = 2014.0(3) A3, Z = 8, S = 1.025, the final R = 0.0303, w R = 0.0825 for 1460 observed reflections with I 2σ(I) and R = 0.0386, wR = 0.0870 for all reflections. In addition, elemental analysis, IR, and sensitivity characterization are presented.展开更多
A novel cobalt complex,[Co2(bptc)(bix)1.5](1,H4bptc=3,3',4,4'-biphenyltetra-carboxylic acid,bix = 1,4-bis(imidazol-1-ylmethyl)benzene),has been hydrothermally prepared and characterized by IR spectroscopy,el...A novel cobalt complex,[Co2(bptc)(bix)1.5](1,H4bptc=3,3',4,4'-biphenyltetra-carboxylic acid,bix = 1,4-bis(imidazol-1-ylmethyl)benzene),has been hydrothermally prepared and characterized by IR spectroscopy,elemental analysis and single-crystal X-ray diffraction.The crystal is of triclinic system,space group P1 with a=10.770(7),b=12.245(8),c=13.514(9),α=102.829(8),β=107.734(8),γ=98.833(9)°,C37H27N6O8Co2,Mr=801.51,V=1607.5(18)3,Dc=1.656g/cm3,F(000)=818,μ=1.100mm-1,Z=2,the final R = 0.0694 and wR = 0.1543 for 3034 observed reflections(I2σ(I)).In the title complex,the two Co(Ⅱ) ions are in different coordination environments with distorted octahedral and trigonal bipyramidal geometries,respectively.The Co atoms are linked together through hexadentate bptc ligands,giving rise to 2D layers which are bridged by the bix ligands into a 3-D supramolecular network.Magnetic susceptibilities of 1 reveal weak antiferromagnetic exchange interactions between the adjacent Co(Ⅱ) ions.展开更多
A new cobalt(II) complex [Co(NO2-salen)2]·1.5H2O containing mono acetalization Schiff base ligand(NO2-salen = N-5-nitro-salicylideneamino ethanato) has been prepared through one-pot template condensation, a...A new cobalt(II) complex [Co(NO2-salen)2]·1.5H2O containing mono acetalization Schiff base ligand(NO2-salen = N-5-nitro-salicylideneamino ethanato) has been prepared through one-pot template condensation, and has been structurally characterized by elemental analysis, IR spectra and X-ray diffraction. It is formulated as C18H23CoN6O7.5, crystallizes in the hexagonal system, space group of R-3c with α = 25.895(18), b = 25.895(18), c = 35.075(6), γ = 120o, V = 20368(3) and Z = 36. The ligand of 5-nitrosalicylaldehyde-ethylene-diamine takes unusual mono asymmetry mode. The Co(II) ion exhibits a coordination number of six, and assumes a distorted octahedral geometry with a N2O4 donor set. The neutral monomeric units of [Co(NO2-salen)2]·1.5H2O are linked into a one-dimensional(1D) structure via the intermolecular hydrogen bonds and weak π-π stacking interactions. Cyclic-voltammetry measurement reveals the oxidation and reduction processes for the complex are irreversible in nature.展开更多
The reaction of [Et4N]2WS4 with 4 equiv of CuCN in pyridine produced a new polymeric complex [WS4Cu4(Py)4(m-CN)2]∞ 1, whose crystal structure has been characterized by single-crystal X-ray analysis. 1 (C22H20Cu4N6S4W...The reaction of [Et4N]2WS4 with 4 equiv of CuCN in pyridine produced a new polymeric complex [WS4Cu4(Py)4(m-CN)2]∞ 1, whose crystal structure has been characterized by single-crystal X-ray analysis. 1 (C22H20Cu4N6S4W, Mr = 934.71) crystallizes in monoclinic, space group P21/m with a = 8.994(2), b = 16.038(3), c = 12.026(3) ? b = 90.85(1)? V = 1734.6(6) ?, Z = 2, Dc = 1.789 g/cm3, F(000) = 896, m(MoKa) = 59.8 cm-1 and T = 193 K. The structure was refined to R = 0.064 and Rw = 0.080 for 2209 observed reflections (I > 3.0s(I)). The X-ray analysis shows that the tetrahedral WS4 core is coordinated by four Cu atoms, forming a saddle-like WS4Cu4 unit. These repeating units are further interconnected by four Cum-CNCu bridges to generate a one-dimensional ladder-shaped structure. The W…Cu bond distances are 2.726(2) and 2.723(2) ? respectively.展开更多
Complex salt Co_2Cl_5(py)_5 (py=pyridine) was obtained by the reaction of CoCl_2·6H_2O with Bu_4NMnO_4 in pyridine in the presence of benzoic acid. It is monoclinic and crystallizes in space group P2_1/n, fw=690....Complex salt Co_2Cl_5(py)_5 (py=pyridine) was obtained by the reaction of CoCl_2·6H_2O with Bu_4NMnO_4 in pyridine in the presence of benzoic acid. It is monoclinic and crystallizes in space group P2_1/n, fw=690.64, a=28.652(5), b=14.108(4), c=7.424(3) ;β=90.09(1); V=3001(2)~3; Z=4, Dc=1.53g/cm^3. Final R factor is 0.041. The structure consists of a discrete cation [Co~ⅢCl_2(py)_4]^+ and an anion [Co~Ⅱ Cl_3(py)]^-. The Co~Ⅲ ion is coordinated by two Cl^- and four pyridine nitrogen atoms to form an octahedral geometry, and Co~Ⅱ is coordinated by three Cl^- and one pyridine nitrogen atom to form the apices of a tetrahedron. The variable-temperature magnetic susceptility measurement shows no magnet-exchange interaction between Co~Ⅲ and Co~Ⅱ ions.展开更多
The complex [Nd(L)(CH_3CN)(CF_3SO_3)_3] has been synthesized, where L=1-methyl-1,4,7,10-tetraazacyclododecane. The crystal structure of the complex has been determined by a fourcircle X-ray diffractometer to a final R...The complex [Nd(L)(CH_3CN)(CF_3SO_3)_3] has been synthesized, where L=1-methyl-1,4,7,10-tetraazacyclododecane. The crystal structure of the complex has been determined by a fourcircle X-ray diffractometer to a final R value of 0.0370 and Rw value of 0.0385 respectively. The crystal is triclinic system, space group P1 with a=8.738(2), b=12.870(3), c=12.900(3), α=85.63(2), β=87.25(2), γ=78.30(2)°, V=1415.71(60)~3, Z=2, Dc=1.92g/cm^3. The neodymiumion is eight-coordinated, forming a distorted square antiprism.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
The crystal structure of the title complex salt has been determined by single-crystal X-ray structure analysis. The crystal data are as follows; Monoclinic, P21/c, a=15.6480(10)A,b=16.7870(10)A, c=10.347(2)A, β=90.79...The crystal structure of the title complex salt has been determined by single-crystal X-ray structure analysis. The crystal data are as follows; Monoclinic, P21/c, a=15.6480(10)A,b=16.7870(10)A, c=10.347(2)A, β=90.790(10), V=2717.7(6)A3, Z=3, and R=0.0333 for 4789 unique reflections. The complex anion has a pseudo-octahedral structure distorted more than the CrⅢand CoⅢ analogs, in which cach iminodiacetato ligand (ida2-) is coordinated in a facial fashion with the two N atoms in a cis configuration, resulting in an unsyin-fac structure.展开更多
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No. 2009. 272)
文摘A new metal-organic complex Co2(cbba)4(phen)2(μ2-OH2)(H2cbba=2-(4'-chlorine-benzoyl)benzoic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and struc-turally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.7659(7),b=17.1856(11),c=19.2022(13),α=83.8120(10),β=84.9930(10),γ=87.2070(10)°,V=3515.8(4)3,C80H50Cl4Co2N4O13,Mr=1534.90,Dc=1.450 g/cm3,μ(MoKα)=0.693 mm-1,F(000)=1568,Z=2,the final R=0.0490 and wR=0.1092 for 8216 observed reflections(Ⅰ 〉2σ(Ⅰ)).In the crystal structure,the cobalt atom is six-coordinated with three carboxylate oxygen atoms from three different cbba ligands,one oxygen atom from coordinated water molecule and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry.Furthermore,it exhibits a 3D supramolecular network through π-π and hydrogen bonding interactions.
基金supported by the Science and Technological Fund of Anhui Province for Outstanding Youth and the Program for New Century Excellent Talents in University (06046100 and NCET-06-0556)
文摘A novel layered mixed metal vanadium-cobadt complex, (py)5Co2(H2O)3[V4O12] 1 (py = pyridine), was hydro(solvo)thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pca21 with a = 17.473(4), b = 11.447(2), c = 17.509(4)A^°, V = 5005.3(7)A^°3, Z = 4, Mr = 3502.1(12), Z = 4, Dc = 1.827 g/cm^3,μ(MoKα) = 2.023 mm^-1, F(000) = 1928, S = 1.020, the final R = 0.0400 and wR= 0.1063 for 6035 observed reflections with I 〉 2σ(I) and 460 variables. Complex 1 consists of tetrahedral VO4 groups to form the large layers which are alternately bonded by two cobalt complex species Co(py)2(H2O)2 and Co(py)3(H2O).
基金supported by Science and Technology Research Projects of the Education Office of Jilin Province (No. 2007. 213)
文摘A new metal-organic coordination polymer [Co(2-pya)2(4,4'-bipy)]2n-[(4,4'- bipy)0.5· H2O]2n (2-pya = 2-pyridinecarboxylic acid, 4,4'-bipy = 4,4'-bipyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I41/a with a = b = 22.719(2), c = 10.710(2)/k, V = 5527.8(14) A3, C54H46N10Co2O10, Mr= 1112.87, Dc = 1.337 g/cm3,μ(MoKa) = 0.665 mm-1, F(000) = 2296, Z = 4, the final R = 0.0633 and wR = 0.1096 for 1261 observed reflections (I 〉 2σ(I)). It exhibits a one-dimensional chain-like structure constructed by mixed ligands of 2-pyridinedicarboxylic acid and 4,4'-bipyridine.
基金This work was supported by the National Natural Science Foundation of China (No. 20101003), Natural Science Foundation of Heilongjiang Province (No. B0007) and the Scientific Fund of Remarkable Teachers of Heilongjiang Province (1054G036)
文摘A novel dinuclear complex with an empirical formula [Co2(1H-benzimidazole)4(1, 4-bdoa)2] (1,4-bdoa2– = benzene-1,4-dioxyacetate dianion) has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 11.000(2), b = 19.385(4), c = 11.417(2) ?, β = 95.49(3)o, V = 2423.3(8) ?3, Z = 2, Mr = 1074.77, Dc = 1.473 g/cm3, μ = 0.760 mm–1, F(000) = 1108, the final R = 0.0645 and wR = 0.0714 for 3273 observed reflections (I > 2σ(I)). Two octahedrally coordinated Co(II) atoms are bridged by two 1,4-bdoa2– groups, generating a macrocyclic ring complex. The Co…Co separa- tion is 7.677(3) ?. An extended 3-D supramolecular network is formed through hydrogen bonds and weak π-π stacking interactions.
基金① This project was supported by the Natural Science Foundation of Jiangsu Province (BK2005045)the Key Marine Biotechnology Lab. of HHIT and the Natural Science Foundation of HHIT (Z2005016)
文摘A new mononuclear cobalt(Ⅲ) complex [Co(dpa)2(Gly)](ClO4)2-4H2O was synthesized by the reaction of Co^2+, glycine (gly) and 2,2"-dipyridylamine (dpa) in a methanol-water solution, and its structure was characterized by IR, EA, ES-MS and X-ray structure analysis. The compound crystallizes in the monoclinic system, space group P21/n with a = 12.8795(2), b = 13.2904(2), c = 19.1104(2)A, β= 109.378(1)°, V = 3085.89(8)A^3, Z = 4, Mr = 746.36, Dc = 1.606 g/cm^3, μ= 0.808 mm^-1, F(000) = 1536, the final R = 0.0543 and wR = 0.1306 for 5393 independent reflections. The magnetic measurement of the compound at room temperature shows that it is diamagnetic and the cobalt ion is in low spin +3 oxidation state. ES-MS experiments show that the [Co(dpa)E(Gly)]^2+ cation is very stable in the methanol solution.
基金Supported by the Fund of Science and Technology Committee of Hunan Province(No.2012GK3030)the Scientific Research Fund of Hunan Provincial Education Department(No.B21018)the Hengyang Bureau of Science & Technology(No.2011kG28)
文摘A dinuclear cobalt(II) complex [Co2(a-furacrylato)4(Phen)2(H20)]'C2HsOH has been synthesized with a-furacrylic acid and 1,10-phenanthroline as the ligands, and its crystal structure was determined. The crystal is of monoclinic system, space group C2/c with a = 1.07388(8), b = 2.4300(2), c = 1.86708(14) nm, β= 104.3830(10)°, V= 4.719.4(7) nm3, Dc = 1.503 g/cm3, Z = 2, F(000) = 2196, GOOF = 1.053, the final R = 0.0343 and wR = 0.0883. The crystal structure shows that two neighboring cobalt(II) ions are linked by the bridging coordination of two a-furacrylic acid anions and one water molecule, and their end positions are respectively coordinated with two 1,10-phenanthroline molecules and two a-furacrylic acid anions, forming a dinuclear structure. Both cobalt(II) ions adopt hexa-coordinated distorted octahedral geometry. The electrochemical and fluorescence properties of the title complex are also discussed.
基金Supported by the Natural Science Foundation of Hunan Province(No.11JJ9006)Key Project of Science and Technology Plan of Hunan Province(2012FJ2002)the Construct Program of the Key Discipline in Hunan Province
文摘A new cobalt complex Co(C10H8N2)(H2O)3[C9H11O2(COO)] with methy-5-norbor- nene-2,3-dicarboxylic anhydride acid (MNA) and 2,2'-bipyridine as ligands has been synthesized in the mixed solvents of ethanol and water. It crystallizes in monoclinic, space group P21/c with α = 13.0430(13), b = 21.014(2), c = 7.5151(7) ?, β = 102.319(2)o, V = 2012.4(3) A3, Dc = 1.529 g/cm3, Z = 4, F(000) = 964, GOOF = 1.051, the final R= 0.0457 and wR= 0.0974. The crystal structure shows that the cobalt ion is coordinated with four oxygen atoms from one MNA molecule and three water molecules together with two nitrogen atoms from the 2,2'-bipyridine molecule, forming a distorted octahedral coordination geometry. The thermal stabilityand electrochemical properties have studied in this paper.
基金Supported by Hunan Provincial Natural Science Foundation of China(2019JJ60021)the Scientific Research Found of Hunan Provincial Education Department of China(17A049,17C0226)Industry and Research Key Project of Hengyang City(2018KJ016)
文摘Two new cobalt(Ⅱ)complexes[Co2(2,2?-bipy)2(dpa)2(H2O)5]·4H2O(1)and Co(2,2?-bipy)3(SO4)]·7.5H2O(2)have been synthesized with diaphonic acid(H2dpa)and 2,2?-bipyridine(2,2?-bipy)as ligands.In 1,two neighboring cobalt(Ⅱ)ions are linked together by one bridging diaphonic acid group,forming an asymmetric dinuclear structure.1 crystallizes in triclinic,space group P1 with a=9.825(6),b=13.007(8),c=19.586(1)A,α=80.773(1)o,β=77.065(1)o,γ=85.902(1)o,Mr=431.4,V=2406.5(3)A^3,Dc=1.48 g/cm^3,Z=2,μ(Mo Kα)=0.767 mm-1,F(000)=1112,the final R=0.0379 and wR=0.0862.The central cobalt(Ⅱ)ions in 1 and 2 are coordinated with six atoms,forming distorted octahedral coordination geometry.The fluorescence and thermal stability properties of 1 and 2 are also reported.
基金This work was supported by the NSFC (20361004) NSF of Yunnan Province (2003E0012M and 2003RC13) and NSF of Yunnan University (2002Z001GC)
文摘The reaction of Co(OAc)2 with bpe and 4,4?-dpdo in an aqueous-alcohol solution affords the formation of red crystals of [Co(H2O)2(bpe)(OAc)2]?4,4?-dpdo (bpe = trans-1,2-bis(4- pyridyl)ethylene, 4,4?-dpdo = 4,4?-dipyridyl N,N?-oxide). The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 7.6146(9), b = 8.6691(11), c = 10.3440(11) ?, α = 88.311(3), β = 76.992(3), γ = 75.809(3)°, V = 644.76(13) ?3, Z = 1, C26H28CoN4O8, Mr = 583.45, Dc = 1.503 g/cm3, μ = 0.724 mm-1, F(000) = 303, T = 223(2) K, the final R = 0.0477 and wR = 0.1177 for 3199 observed reflections with I > 2σ(I). In the crystal the cobalt atom is six-coordinated by oxygen atoms from two carboxylic molecules, two nitrogen atoms from the bpe ligands and two water molecules, completing an octahedral geometry. The structure of the title complex consists of neutral chains containing cobalt(II) ions bridged by mutually trans bpe molecules. The adjacent chains are connected through weak hydrogen bonds to form a two-dimensional structure.
文摘Reaction of cobalt carbonate, pivalic acid and quinoline in a refluxing ethanol solvent yielded the dicobalt(Ⅱ) compound, Co 2(O 2CCMe 3) 4(C 9H 7N) 2 (1) (C 9H 7N is quinoline), which has been characterised by elemental analysis, IR and X ray diffraction method. Crystallographic data: monoclinic, P2 1/a, a=9.341(2), b=18.591(4), c=11.822(2) , β=97.71(2), V=2034(1) 3, Z=2, M r=918.19, D c =1.27 g/cm -3 , F(000)=820, μ (Mo Kα )=8.60 cm -1 , T =293K, final R=0 049, R w =0.060 for 2715 observed reflections with I】3.0 σ(I) . The centrosymmetric molecule comprises a pair of cobalt(Ⅱ) atoms connected by four pivalate ligands in syn syn bridging modes. Square pyramidal five coordination of cobalt(Ⅱ) is further completed by a quimoline molecule. The Co Ⅱ-Co Ⅱ distance is 2.784(1) .
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.2013.384)
文摘Two new coordination polymers [Co(oba)(mbix)]2n·nH2O (1) and [Mn(Hoba)2(H2O)2]n (2) (H2oba = 4,4'-oxydibenzoic acid, mbix = 1,3-bis(imidazol-1-ylmethyl)benzene) have been successfully synthesized under hydrothermal conditions. Their structures have been determined by elemental analyses, IR spectroscopy, UV and single-crystal X-ray diffraction analysis. The intermolecular hydrogen bonding and π-π stacking interactions extend the complexes into a 3D supramolecular structure.
基金Supported by the National Natural Science Foundation of China(No.21203160)Education Department Foundation of Shaanxi Province(No.12JK0631)+1 种基金Natural Science Foundation of Shaanxi Province(No.2013JM2013)Special Research Fund of Xianyang Normal University(No.11XSYK204,11XSYK205,12XSYK023)
文摘A novel cuprous azide complex with the formula of [Cu2(dmpz)(N3)2]n(1, dmpz: 2,6-dimethylpyrazine) has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characterized by single-crystal X-ray diffraction method. Single-crystal X-ray diffraction analysis reveals the title complex represents a three-dimensional network structure featuring 2D [Cu N3]n plane units bridged by bridging dmpz ligands to form a 3D network. Research results reveal that 1 has lower impact sensitivity and friction sensitivity, which may be expected to become insensitive energetic material and have potential applications. Crystal data: monoclinic, space group C2/c, a = 17.8599(15), b = 8.2889(5), c = 14.8076(14) A, β = 113.2580(10)o, V = 2014.0(3) A3, Z = 8, S = 1.025, the final R = 0.0303, w R = 0.0825 for 1460 observed reflections with I 2σ(I) and R = 0.0386, wR = 0.0870 for all reflections. In addition, elemental analysis, IR, and sensitivity characterization are presented.
基金supported by the National Natural Science Foundation of China (No 20971004)the Outstanding Youth Foundation of Education Commission of Anhui Province (No 2010SQRL108ZD)
文摘A novel cobalt complex,[Co2(bptc)(bix)1.5](1,H4bptc=3,3',4,4'-biphenyltetra-carboxylic acid,bix = 1,4-bis(imidazol-1-ylmethyl)benzene),has been hydrothermally prepared and characterized by IR spectroscopy,elemental analysis and single-crystal X-ray diffraction.The crystal is of triclinic system,space group P1 with a=10.770(7),b=12.245(8),c=13.514(9),α=102.829(8),β=107.734(8),γ=98.833(9)°,C37H27N6O8Co2,Mr=801.51,V=1607.5(18)3,Dc=1.656g/cm3,F(000)=818,μ=1.100mm-1,Z=2,the final R = 0.0694 and wR = 0.1543 for 3034 observed reflections(I2σ(I)).In the title complex,the two Co(Ⅱ) ions are in different coordination environments with distorted octahedral and trigonal bipyramidal geometries,respectively.The Co atoms are linked together through hexadentate bptc ligands,giving rise to 2D layers which are bridged by the bix ligands into a 3-D supramolecular network.Magnetic susceptibilities of 1 reveal weak antiferromagnetic exchange interactions between the adjacent Co(Ⅱ) ions.
基金supported by the National Natural Science Foundation of China(No.21273101)the Foundation of the Program for Backbone Teachers in Universities of Henan Province(No.2012GGJS158)+1 种基金tackle key problem of science and technology Project of Henan Province(No.142102310483)the Foundation of Education Committee of Henan Province(No.14B150033)
文摘A new cobalt(II) complex [Co(NO2-salen)2]·1.5H2O containing mono acetalization Schiff base ligand(NO2-salen = N-5-nitro-salicylideneamino ethanato) has been prepared through one-pot template condensation, and has been structurally characterized by elemental analysis, IR spectra and X-ray diffraction. It is formulated as C18H23CoN6O7.5, crystallizes in the hexagonal system, space group of R-3c with α = 25.895(18), b = 25.895(18), c = 35.075(6), γ = 120o, V = 20368(3) and Z = 36. The ligand of 5-nitrosalicylaldehyde-ethylene-diamine takes unusual mono asymmetry mode. The Co(II) ion exhibits a coordination number of six, and assumes a distorted octahedral geometry with a N2O4 donor set. The neutral monomeric units of [Co(NO2-salen)2]·1.5H2O are linked into a one-dimensional(1D) structure via the intermolecular hydrogen bonds and weak π-π stacking interactions. Cyclic-voltammetry measurement reveals the oxidation and reduction processes for the complex are irreversible in nature.
基金This work was supported by NNSFC (No. 20271036) the NSF of the Education Committee of Jiangsu province (No. 02KJB150001) and the State Key Laboratory of Structural Chemistry (No. 030066)
文摘The reaction of [Et4N]2WS4 with 4 equiv of CuCN in pyridine produced a new polymeric complex [WS4Cu4(Py)4(m-CN)2]∞ 1, whose crystal structure has been characterized by single-crystal X-ray analysis. 1 (C22H20Cu4N6S4W, Mr = 934.71) crystallizes in monoclinic, space group P21/m with a = 8.994(2), b = 16.038(3), c = 12.026(3) ? b = 90.85(1)? V = 1734.6(6) ?, Z = 2, Dc = 1.789 g/cm3, F(000) = 896, m(MoKa) = 59.8 cm-1 and T = 193 K. The structure was refined to R = 0.064 and Rw = 0.080 for 2209 observed reflections (I > 3.0s(I)). The X-ray analysis shows that the tetrahedral WS4 core is coordinated by four Cu atoms, forming a saddle-like WS4Cu4 unit. These repeating units are further interconnected by four Cum-CNCu bridges to generate a one-dimensional ladder-shaped structure. The W…Cu bond distances are 2.726(2) and 2.723(2) ? respectively.
文摘Complex salt Co_2Cl_5(py)_5 (py=pyridine) was obtained by the reaction of CoCl_2·6H_2O with Bu_4NMnO_4 in pyridine in the presence of benzoic acid. It is monoclinic and crystallizes in space group P2_1/n, fw=690.64, a=28.652(5), b=14.108(4), c=7.424(3) ;β=90.09(1); V=3001(2)~3; Z=4, Dc=1.53g/cm^3. Final R factor is 0.041. The structure consists of a discrete cation [Co~ⅢCl_2(py)_4]^+ and an anion [Co~Ⅱ Cl_3(py)]^-. The Co~Ⅲ ion is coordinated by two Cl^- and four pyridine nitrogen atoms to form an octahedral geometry, and Co~Ⅱ is coordinated by three Cl^- and one pyridine nitrogen atom to form the apices of a tetrahedron. The variable-temperature magnetic susceptility measurement shows no magnet-exchange interaction between Co~Ⅲ and Co~Ⅱ ions.
文摘The complex [Nd(L)(CH_3CN)(CF_3SO_3)_3] has been synthesized, where L=1-methyl-1,4,7,10-tetraazacyclododecane. The crystal structure of the complex has been determined by a fourcircle X-ray diffractometer to a final R value of 0.0370 and Rw value of 0.0385 respectively. The crystal is triclinic system, space group P1 with a=8.738(2), b=12.870(3), c=12.900(3), α=85.63(2), β=87.25(2), γ=78.30(2)°, V=1415.71(60)~3, Z=2, Dc=1.92g/cm^3. The neodymiumion is eight-coordinated, forming a distorted square antiprism.
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.
文摘The crystal structure of the title complex salt has been determined by single-crystal X-ray structure analysis. The crystal data are as follows; Monoclinic, P21/c, a=15.6480(10)A,b=16.7870(10)A, c=10.347(2)A, β=90.790(10), V=2717.7(6)A3, Z=3, and R=0.0333 for 4789 unique reflections. The complex anion has a pseudo-octahedral structure distorted more than the CrⅢand CoⅢ analogs, in which cach iminodiacetato ligand (ida2-) is coordinated in a facial fashion with the two N atoms in a cis configuration, resulting in an unsyin-fac structure.