Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4...Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4 )3· 5H2O (complex3) and [Ni3 (BZT ) (Nphen )6] (ClO4 )3 (complex 4 ) (BZT = 1, 3, 5-benzenetricarboxylato, Phen = 1, 10-phenthroline, Nphen = 5-nitro-1, 10-phenanthroline )have been synthesized. The complexes were characterized using elemental analysis,IR and electronic reflection spectra. These complexes are proposed to have extended 1, 3, 5-benzenetricarboxylato-bridged structure and to consist of three manganese (Ⅱ) or three nickel(Ⅱ). The X-band ESR spectra of the complex 1 and complex 2were recorded at room temperature. The variable-temperature magnetic susceptibilities of complex 1 and complex 3 were measured over 4. 2-300 K. According to experimental results of the variable-temperature magnetic susceptibility, the magnetic interaction between the paramagnetic centers is too weak to be detected using the usual magnetic susceptibility technique.展开更多
A novel complex, [Mn(2-NCP)(H2BTC)(H2O)]n(1, 1,3,5-H3BTC = 1,3,5-benzenetricarboxylic acid, 2-HNCP = 2-(2-carboxyphenyl)-1 H-imidazo(4,5-f)-(1,10)phenanthroline), was hydrothermally synthesized and struc...A novel complex, [Mn(2-NCP)(H2BTC)(H2O)]n(1, 1,3,5-H3BTC = 1,3,5-benzenetricarboxylic acid, 2-HNCP = 2-(2-carboxyphenyl)-1 H-imidazo(4,5-f)-(1,10)phenanthroline), was hydrothermally synthesized and structurally characterized by elemental analysis, IR, XRD and single-crystal X-ray diffraction. Structural analyses reveal that complex 1 exhibits a(6, 6)-connected topology network with a Schl?fli symbol of(63). The adjacent 2 D layers are further stacked via strong hydrogen-bonding interactions, giving a 3 D supramolecular framework. In addition, the structure of complex 1 was calculated by the B3LYP/LANL2 DZ method by Gaussian program. The results from natural bond orbital(NBO) analysis shows obvious covalent interaction between the coordinated atoms and Mn(Ⅱ) ion.展开更多
A homochrial manganese(Ⅱ) complex derived from chiral salen ligand (1R,2R)-(-)diaminocyclohexane-N,N-biscarboxyl-salicylidene) (1) has been synthesized through solvothermal procedure and characterized by IR,...A homochrial manganese(Ⅱ) complex derived from chiral salen ligand (1R,2R)-(-)diaminocyclohexane-N,N-biscarboxyl-salicylidene) (1) has been synthesized through solvothermal procedure and characterized by IR,elemental analysis,TGA,circular dichroism (CD),powder and single-crystal X-ray crystallography.It crystallizes in monoclinic,space group C2 with a=32.987(7),b=7.4662(15),c=17.931(4),β=97.82(3)°,V=4375.0(15) 3,Z=8,D c=1.544 g/cm 3,F(000)=2096,M r=508.36,μ=0.658 mm-1,the final GOOF=0.975,R=0.0676 and wR=0.2068 for 6357 observed reflections with I 2σ(Ⅰ).The coordination polymer 1 possesses a 1D infinite zigzag chain architecture constructed by the dicarboxyl-functionalized metallosalen ligand (MnSalen),and the polymeric chains are further assembled into a 2D supramolecular network structure via strong intermolecular hydrogen bonding interactions between the adjacent zigzag chains.展开更多
A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)- benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrotherrnally synthesized and structurally characterized by single-crysta...A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)- benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrotherrnally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with α = 12.154(5), b = 18.166(7), c = 31.197(13) A, V = 6887(5) A^3, C80H48Cl4Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm^3, μ(MoKα) = 0.591 mm^-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I 〉 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions.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
A new cyanide-bridged bimetallic assembly [Mn(3-meosalpn)(H2O)]2[Fe(CN)5NO](1) was obtained by the reaction of [Fe(CN)5NO]2-with [Mn(3-meosalpn)]+,and characterized by elemental analysis,IR and single-cry...A new cyanide-bridged bimetallic assembly [Mn(3-meosalpn)(H2O)]2[Fe(CN)5NO](1) was obtained by the reaction of [Fe(CN)5NO]2-with [Mn(3-meosalpn)]+,and characterized by elemental analysis,IR and single-crystal X-ray structure analysis.The complex crystallizes in the monoclinic system,space group P21/c with a = 12.992(5),b = 13.274(6),c = 14.644(6) ,β = 115.198(4)o,V = 2285.2(16)3,Z = 2,C43H44FeMn2N10O11,Mr = 1042.61,Dc = 1.515 g/cm3,F(000) = 1072,μ = 0.928 mm-1,S = 1.052,the final R = 0.0347 and wR = 0.0957 for 17377 observed reflections(Ⅰ 〉 2σ(Ⅰ)).X-ray single-crystal diffraction analysis reveals that 1 has a trinuclear molecular structure,in which the two [Mn(3-meosalpn)(H2O)]+ cations are linked by the central [Fe(CN)5NO]2-anion via two trans CN-groups.Furthermore,the two [Mn(3-meo-salpn)(H2O)]+ cations and [Fe(CN)5NO]2-anion are connected into a one-dimensional zigzag chain through hydrogen bonding interactions.展开更多
A novel metal-organic coordination polymer [Mn3(2,2′-dipha)3(phen)6]n·3nH2O (2,2′-dipha = 2,2′-diphenic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characteri...A novel metal-organic coordination polymer [Mn3(2,2′-dipha)3(phen)6]n·3nH2O (2,2′-dipha = 2,2′-diphenic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and magnetic susceptibility measurements. The crystal crystallizes in triclinic, space group P1 with a = 16.921(5), b = 18.307(5), c = 18.450(5)A , α = 113.369(5), β = 108.529(5), γ = 102.984(5)°, V = 4553(2)A^ 3, C114H72Mn3N12O14.25, Mr = 2002.66, Dc = 1.461 g/cm^3, μ(MoKα) = 0.488 mm^-1, the final F(000) = 2058, Z = 2, R = 0.0491 and wR = 0.0980 for 9087 observed reflections (I 〉 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with two carboxylate oxygen atoms from different carboxylate groups of the same dipha and four nitrogen atoms from two different phen ligands, showing a slightly distorted octahedral geometry. Fur- thermore, it exhibits a zero-dimensional structure with dipha-Mn-phen- as building units. Variable- temperature magnetic measure shows an overall anti-ferromagnetic behavior for compound 1.展开更多
A new metal-organic complex [Mn2(PDC)2(bipy)2(H2O)2] (H2PDC = 2,4-pyridine-dicarboxylic acid, bipy = 2,2′-bipyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis...A new metal-organic complex [Mn2(PDC)2(bipy)2(H2O)2] (H2PDC = 2,4-pyridine-dicarboxylic acid, bipy = 2,2′-bipyridine) 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 P ^-1 with a = 7.376(3), b = 9.990(4), c = 11.950(5) A^°, α= 75.217(5), β = 78.052(5), γ = 70.655(5)°, V = 796.0(5)A^°3, C34HE6Mn2N6O10, Mr = 788.49, De = 1.645 g/cm^3,μ(MoKa) = 0.866 mm^-1, F(000) = 235, Z = 1, the final R = 0.0425 and wR = 0.0700 for 1971 observed reflections (I 〉 2σ(I)). In the crystal structure, the manganese atom is six-coordinated by two carboxylate oxygen atoms from two different PDC ligands, one aqua ligand, and three nitrogen atoms from 2,2′-bipy and PDC ligands, giving a distorted octahedral geometry. It exhibits a three-dimensional supramolecular network defined by O-H…O hydrogen-bonding interactions.展开更多
A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure...A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1^-, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5)A, a = 101.5310(10), β = 90.2610(10), γ = 116.4600( 10)% V = 1459.44(8)A^3, Z = 2, Dc = 1.619 g/cm^3,μ = 0.539 mm^-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the Mnn atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D'…A' H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O, N-H…O and N-H…N hydrogen bonds between (tataH)^+, [Mn(pydc)2]^2- and crystal water.展开更多
The two title complexes, [Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5- (NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal = 3,5-dinitrosalicylate, 2,2'-bipy = 2,2′-bipyridine), were synthesized by the hydrother...The two title complexes, [Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5- (NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal = 3,5-dinitrosalicylate, 2,2'-bipy = 2,2′-bipyridine), were synthesized by the hydrothermal reaction and structurally characterized. Complex 1 crystallizes in triclinic, space group P1, a = 5.581(4), b = 12.071(8), c = 12.88(1)A, α= 92.10(3),β= 96.73(3), γ = 102.02(2)°, C17H10N407Cd, Mr = 494.69, V= 841(1)A3, Z = 2, Dc = 1.954 g/cm3, F(000) = 488, μ= 1.353 mm^-1, R = 0.0248 and wR = 0.0761. Complex 2 crystallizes in monoclinic with space group P21/c, a = 8.604(3), b = 23.88(1), c = 8.894(3) A, β = 102.45(1)°, C17H10N407Mn, Mr = 437.23, V= 1785(1) A3, Z=.4, Dc = 1.627 g/cm3, F(000) = 884, μ = 0.791 mm^-1, R = 0.0471 and wR = 0.1250. Complex 1 possesses an infinite 1D polymeric chain structure consisting of the repeated basic four-membered ring units (Cd2O2) and eight-membered ring units (CdOCO)2. Compound 2displays a linear 1D chain through Mn(Ⅱ) atoms and bridging carboxylate groups of 3,5-dinitrosalicylic acid ligands with the Mn…Mn separation of 4.472(2)A. The fluorescence properties and cyclic voltammetric behaviors of the complexes are also reported.展开更多
文摘Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4 )3· 5H2O (complex3) and [Ni3 (BZT ) (Nphen )6] (ClO4 )3 (complex 4 ) (BZT = 1, 3, 5-benzenetricarboxylato, Phen = 1, 10-phenthroline, Nphen = 5-nitro-1, 10-phenanthroline )have been synthesized. The complexes were characterized using elemental analysis,IR and electronic reflection spectra. These complexes are proposed to have extended 1, 3, 5-benzenetricarboxylato-bridged structure and to consist of three manganese (Ⅱ) or three nickel(Ⅱ). The X-band ESR spectra of the complex 1 and complex 2were recorded at room temperature. The variable-temperature magnetic susceptibilities of complex 1 and complex 3 were measured over 4. 2-300 K. According to experimental results of the variable-temperature magnetic susceptibility, the magnetic interaction between the paramagnetic centers is too weak to be detected using the usual magnetic susceptibility technique.
基金supported by the National Natural Science Foundation of China(No.21576112)the Project of Department of Science&Technology of Jilin Province(No.20180623042TC)+3 种基金Natural Science Foundation Project of Jilin Province(No.20170520143JH)the China Postdoctoral Science Foundation(No.2017M611732)the Science and Technology Research Projects of the Education Department of Jilin Province(No.JJKH20180791KJ)the Science and Technology Development Plan of Siping City(2017056)
文摘A novel complex, [Mn(2-NCP)(H2BTC)(H2O)]n(1, 1,3,5-H3BTC = 1,3,5-benzenetricarboxylic acid, 2-HNCP = 2-(2-carboxyphenyl)-1 H-imidazo(4,5-f)-(1,10)phenanthroline), was hydrothermally synthesized and structurally characterized by elemental analysis, IR, XRD and single-crystal X-ray diffraction. Structural analyses reveal that complex 1 exhibits a(6, 6)-connected topology network with a Schl?fli symbol of(63). The adjacent 2 D layers are further stacked via strong hydrogen-bonding interactions, giving a 3 D supramolecular framework. In addition, the structure of complex 1 was calculated by the B3LYP/LANL2 DZ method by Gaussian program. The results from natural bond orbital(NBO) analysis shows obvious covalent interaction between the coordinated atoms and Mn(Ⅱ) ion.
基金supported by NSFC-20971085"973" programs (2007CB209701 and 2009CB930403)+1 种基金the Major Fundamental Research of Shanghai Science and Technology Committee (10dj1400102)the key project of State Education Ministry
文摘A homochrial manganese(Ⅱ) complex derived from chiral salen ligand (1R,2R)-(-)diaminocyclohexane-N,N-biscarboxyl-salicylidene) (1) has been synthesized through solvothermal procedure and characterized by IR,elemental analysis,TGA,circular dichroism (CD),powder and single-crystal X-ray crystallography.It crystallizes in monoclinic,space group C2 with a=32.987(7),b=7.4662(15),c=17.931(4),β=97.82(3)°,V=4375.0(15) 3,Z=8,D c=1.544 g/cm 3,F(000)=2096,M r=508.36,μ=0.658 mm-1,the final GOOF=0.975,R=0.0676 and wR=0.2068 for 6357 observed reflections with I 2σ(Ⅰ).The coordination polymer 1 possesses a 1D infinite zigzag chain architecture constructed by the dicarboxyl-functionalized metallosalen ligand (MnSalen),and the polymeric chains are further assembled into a 2D supramolecular network structure via strong intermolecular hydrogen bonding interactions between the adjacent zigzag chains.
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No. 2007. 213)
文摘A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)- benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrotherrnally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with α = 12.154(5), b = 18.166(7), c = 31.197(13) A, V = 6887(5) A^3, C80H48Cl4Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm^3, μ(MoKα) = 0.591 mm^-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I 〉 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions.
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supported by Industry High Technology Foundation of Jiangsu (BG2007025)Doctoral Fund from National Ministry of Education (20093227110009),China
文摘A new cyanide-bridged bimetallic assembly [Mn(3-meosalpn)(H2O)]2[Fe(CN)5NO](1) was obtained by the reaction of [Fe(CN)5NO]2-with [Mn(3-meosalpn)]+,and characterized by elemental analysis,IR and single-crystal X-ray structure analysis.The complex crystallizes in the monoclinic system,space group P21/c with a = 12.992(5),b = 13.274(6),c = 14.644(6) ,β = 115.198(4)o,V = 2285.2(16)3,Z = 2,C43H44FeMn2N10O11,Mr = 1042.61,Dc = 1.515 g/cm3,F(000) = 1072,μ = 0.928 mm-1,S = 1.052,the final R = 0.0347 and wR = 0.0957 for 17377 observed reflections(Ⅰ 〉 2σ(Ⅰ)).X-ray single-crystal diffraction analysis reveals that 1 has a trinuclear molecular structure,in which the two [Mn(3-meosalpn)(H2O)]+ cations are linked by the central [Fe(CN)5NO]2-anion via two trans CN-groups.Furthermore,the two [Mn(3-meo-salpn)(H2O)]+ cations and [Fe(CN)5NO]2-anion are connected into a one-dimensional zigzag chain through hydrogen bonding interactions.
基金The project was supported by the Education Office of Jilin Province (No. 0047)
文摘A novel metal-organic coordination polymer [Mn3(2,2′-dipha)3(phen)6]n·3nH2O (2,2′-dipha = 2,2′-diphenic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and magnetic susceptibility measurements. The crystal crystallizes in triclinic, space group P1 with a = 16.921(5), b = 18.307(5), c = 18.450(5)A , α = 113.369(5), β = 108.529(5), γ = 102.984(5)°, V = 4553(2)A^ 3, C114H72Mn3N12O14.25, Mr = 2002.66, Dc = 1.461 g/cm^3, μ(MoKα) = 0.488 mm^-1, the final F(000) = 2058, Z = 2, R = 0.0491 and wR = 0.0980 for 9087 observed reflections (I 〉 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with two carboxylate oxygen atoms from different carboxylate groups of the same dipha and four nitrogen atoms from two different phen ligands, showing a slightly distorted octahedral geometry. Fur- thermore, it exhibits a zero-dimensional structure with dipha-Mn-phen- as building units. Variable- temperature magnetic measure shows an overall anti-ferromagnetic behavior for compound 1.
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 [Mn2(PDC)2(bipy)2(H2O)2] (H2PDC = 2,4-pyridine-dicarboxylic acid, bipy = 2,2′-bipyridine) 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 P ^-1 with a = 7.376(3), b = 9.990(4), c = 11.950(5) A^°, α= 75.217(5), β = 78.052(5), γ = 70.655(5)°, V = 796.0(5)A^°3, C34HE6Mn2N6O10, Mr = 788.49, De = 1.645 g/cm^3,μ(MoKa) = 0.866 mm^-1, F(000) = 235, Z = 1, the final R = 0.0425 and wR = 0.0700 for 1971 observed reflections (I 〉 2σ(I)). In the crystal structure, the manganese atom is six-coordinated by two carboxylate oxygen atoms from two different PDC ligands, one aqua ligand, and three nitrogen atoms from 2,2′-bipy and PDC ligands, giving a distorted octahedral geometry. It exhibits a three-dimensional supramolecular network defined by O-H…O hydrogen-bonding interactions.
基金supported by the Postdoctor Foundation of Jiangsu Province (No. 0701001B)the Foundation of Taishan University (No. Y04-2-02)
文摘A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1^-, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5)A, a = 101.5310(10), β = 90.2610(10), γ = 116.4600( 10)% V = 1459.44(8)A^3, Z = 2, Dc = 1.619 g/cm^3,μ = 0.539 mm^-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the Mnn atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D'…A' H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O, N-H…O and N-H…N hydrogen bonds between (tataH)^+, [Mn(pydc)2]^2- and crystal water.
基金the National Natural Science Foundation of China (No. 20431010)
文摘The two title complexes, [Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5- (NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal = 3,5-dinitrosalicylate, 2,2'-bipy = 2,2′-bipyridine), were synthesized by the hydrothermal reaction and structurally characterized. Complex 1 crystallizes in triclinic, space group P1, a = 5.581(4), b = 12.071(8), c = 12.88(1)A, α= 92.10(3),β= 96.73(3), γ = 102.02(2)°, C17H10N407Cd, Mr = 494.69, V= 841(1)A3, Z = 2, Dc = 1.954 g/cm3, F(000) = 488, μ= 1.353 mm^-1, R = 0.0248 and wR = 0.0761. Complex 2 crystallizes in monoclinic with space group P21/c, a = 8.604(3), b = 23.88(1), c = 8.894(3) A, β = 102.45(1)°, C17H10N407Mn, Mr = 437.23, V= 1785(1) A3, Z=.4, Dc = 1.627 g/cm3, F(000) = 884, μ = 0.791 mm^-1, R = 0.0471 and wR = 0.1250. Complex 1 possesses an infinite 1D polymeric chain structure consisting of the repeated basic four-membered ring units (Cd2O2) and eight-membered ring units (CdOCO)2. Compound 2displays a linear 1D chain through Mn(Ⅱ) atoms and bridging carboxylate groups of 3,5-dinitrosalicylic acid ligands with the Mn…Mn separation of 4.472(2)A. The fluorescence properties and cyclic voltammetric behaviors of the complexes are also reported.