The title compound, [Mn4O2（O2CMe）6（MeOH）2（dbm）2]·2MeCOOH·2CH2Cl2 （Hdbm = dibenzoylmethane）, has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs t...The title compound, [Mn4O2（O2CMe）6（MeOH）2（dbm）2]·2MeCOOH·2CH2Cl2 （Hdbm = dibenzoylmethane）, has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P/, with a = 10.729（3）, b = 12.269（3）, c = 13.085（4） A, a = 106.367（3）,β = 107.643（2）, γ = 94.771（2）°, V = 1547.9（7） A^3, Z = 1, C50H64Cl4Mn4O24, Mr= 1410.57, Dc= 1.513 g/cm^3, F（000） = 724, Rint = 0.0147, T= 293（2） K and p = 1.046 mm ^-1. The final R = 0.0359 and wR = 0.0938 for 5791 observed reflections with 1 〉 2σ（/）. The structure of the complex consists of one [Mn4（μ3-O）2]^8＋ core with four coplanar Mn atoms disposed in an extended ＂butterfly-like＂ arrangement and two O atoms triply bridging each ＂wing＂, and the peripheral ligation is provided by six by-MeCO2^-, two terminal ,μ2-dbm- groups at the two ends of the molecule, and two MeOH molecules on the central Mn atoms, lntermolecular O…H-O hydrogen bonding interactions are found within the structure of the compound.展开更多
A new one-dimensional azido-bridged manganese compound has been prepared and structurally characterized by X-ray diffraction. The complex [Mn（N3）2（H2O）3·C6H12N4]n crystallizes in space group Pnma with a = 6.5...A new one-dimensional azido-bridged manganese compound has been prepared and structurally characterized by X-ray diffraction. The complex [Mn（N3）2（H2O）3·C6H12N4]n crystallizes in space group Pnma with a = 6.5252 （5）, b = 9.3226（7）, c = 22.2070（15） ,A°, V= 1350.89（17） ,A°^3, Z = 4, Mr = 333.24, Dc = 1.639 g/cm^3, μ = 1.005 mm^-1 and F（000） = 692. The final refinement gave R = 0.0328 and wR = 0.0777 for 1085 observed reflections with I 〉 2σ（I）. The structure contains [Mn（N3）2（H2O）3]n polymeric chains and uncoordinated hexamethylenetetramine （HMTA） molecules with Mn/HMTA molar ratio of 1：1. The Mn atoms are bridged by end-to-end azido ligands to construct one-dimensional zig-zag infinite chains. Each Mn atom is six-coordinated by three N atoms of three azido ligands and three water O atoms, resulting in an octahedral geometry. Extending hydrogenbonding interactions involving water O atoms, azido and HMTA N atoms link the chains and HMTA molecules into a three-dimensional network.展开更多
Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group ...Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group C2/c with a=24. 825(8) . b=14.716(5) , c=18. 419(10)A,β=94. 57(3)°, V=6707. 54 A￣3;Z=4, Dc=1. 248 g/cm￣3. μ= 5. 002 cm￣(-1). F(000)=2664. The structure was solved by direct methods and refined to final R(Rω)=0.059(0.059) for 3183 observed reflections with I≥2.5σ(I). The centrosymmetric anion of the title compound contains two [V(mp)_3]￣(2-) fragments linked by a sodium ion, the crystallographic center of symmetry , through the μ2-O bridges. The Ⅴ(Ⅳ) atom is in a coordination environment intermediate between a trigonal prism and an ideal octahedron.展开更多
A two-dimensional coordination polymer, [Cd（AIP）（Bpy）]n.nBpy, was hydrothermally synthesized by the reaction of hydrate cadmium acetate with 5-aminoisophthalic acid, lithium hydroxide, vanadiumpentoxide, sodium ch...A two-dimensional coordination polymer, [Cd（AIP）（Bpy）]n.nBpy, was hydrothermally synthesized by the reaction of hydrate cadmium acetate with 5-aminoisophthalic acid, lithium hydroxide, vanadiumpentoxide, sodium chloride and 2,2′-bipyridyl in water solution. It crystallizes in orthorhombic, space group C222 1, absolute structure parameter 0.00（7）, with a = 15.336（4）, b = 22.390（6）, c = 14.257（3）A, V = 4896（2）/~3, C28H21CdNsO4, Mr = 603.90, Z = 8, F（000） = 2432, Dc = 1.639 g/cm^3, μ = 0.939 mm^-1, T= 298（2） K, S = 1.001, R = 0.0296 and wR = 0.0813 for 5522 observed reflections （I 〉 2a（/））. In the title complex, each 5-aminoisophthalate ligand bridges three cadmium（Ⅱ） ions to form a two-dimensional layer structure.展开更多
Two salicylate containing mononuclear manganese complexes formulated as [Mnand characterized by elemental analysis, IR and single-crystal X-ray diffraction analyses. Crystal data for compound 1： monoclinic, space gro...Two salicylate containing mononuclear manganese complexes formulated as [Mnand characterized by elemental analysis, IR and single-crystal X-ray diffraction analyses. Crystal data for compound 1： monoclinic, space group C2/c, a=30.748（6）, b=8.1933（13）, c=21.137（4） A, β=126.772（4）°, V=4265.5（13）A^3, Z=8, Mr=471.34, Dc=1.468 g/cm^3, μ=0.667 mm^-1, F（000）=1952,the final R=0.0637, wR=0.1783 （I 〉 2σ（I）） and GOOF=1.073; and those for compound 2： monoclinic,space group C2/c, a=14.505（5）, b=11.048（4）, c=20.711 （7）（A）, β=103.603（6）°, V=3225.6 （18）A^3, Z=4, Mr=668.65, Dc=1.377 g/cm^3, μ=0.466 mm^-1, F（000）=1416, the final R=0.0373, wR=0.1125 （I 〉2σ（I））, and GOOF=1.000. The Mn atoms of both complexes are six-coordinated in an axially elongated octahedral geometry for 1 and an axially compressed octahedral geometry for 2, and their oxidation states have been determined to be trivalent by bond valence sum calculation.展开更多
Dinuclear palladium complex (Et_4N)_2[Pd_2(mp)_2 (mpH)_2 (mpH=_2-SC_6H_4OH ) (M_r = 971. 95 ) is prepared in a reaction of sodium 2-mercaptophenolate (Na_2mp) with PdCl_2. It crystallizes in monoclinic with space grou...Dinuclear palladium complex (Et_4N)_2[Pd_2(mp)_2 (mpH)_2 (mpH=_2-SC_6H_4OH ) (M_r = 971. 95 ) is prepared in a reaction of sodium 2-mercaptophenolate (Na_2mp) with PdCl_2. It crystallizes in monoclinic with space group P2_1/n, a=9. 088(1),b=17. 851 (4), c=12. 932(2) , β= 93. 21 (1)°, V=2094. 7(7), D_c=1. 54 g/cm￣3, F(000) = 1000, Z=2, and final R= 0. 044 and R_w= 0. 055 for 3090 reflections (I≥3σ(I)). Structure analysis revealed the multifunction chelating character of mp functions as S_tO_t(t for terminal) and S_bOH (b for bridging) in the complex.展开更多
This paper presents the synthetic and structure studies of molybdenum（tungsten）-copper-sulphur-dialkyldithiocarbamate cluster compounds.The reactions of（M=Mo,W;n=0,2）,CuCl,and R<sub>2</sub>dtc￣-（R<...This paper presents the synthetic and structure studies of molybdenum（tungsten）-copper-sulphur-dialkyldithiocarbamate cluster compounds.The reactions of（M=Mo,W;n=0,2）,CuCl,and R<sub>2</sub>dtc￣-（R<sub>2</sub>=Me<sub>2</sub>,Et<sub>2</sub>,C<sub>4</sub>H<sub>8</sub>,C<sub>5</sub>H<sub>1</sub>0） yield a series of tetra-,hexa-,and heptanuclear cluster compounds.Their spectroscopic properties and the synthetic reaction mechanism are discussed.展开更多
The title complex [Mn(phen)2(H2O)2](OAc)26H2O (phen = 1,10-phenanthroline, C12H8N2, OAc = acetate, C2H3O2) with formula C28H38MnN4O12 and Mr = 677.56 has been syn- thesized and structurally characterized by X-ray diff...The title complex [Mn(phen)2(H2O)2](OAc)26H2O (phen = 1,10-phenanthroline, C12H8N2, OAc = acetate, C2H3O2) with formula C28H38MnN4O12 and Mr = 677.56 has been syn- thesized and structurally characterized by X-ray diffraction. The crystal is of triclinic, space group P ?with a = 9.6201(5), b = 13.4663(7), c = 14.5375(8) , a = 108.428(1), b =93.898(1), g = 110.492(1), V = 1639.5(2) ?, Dc = 1.373 g/cm3, F(000) = 710, = 0.468 cm-1 and Z = 2. The final refinement gave R = 0.0522 and wR = 0.1259 for 4714 observed reflections with I > 2s(I). It consists of discrete [Mn(phen)2(H2O)2]2+ cation, two acetate anions and six lattice water molecules. The MnII ion coordinated by four nitrogen atoms from two chelating phen and two oxygen atoms from two cis-related water molecules is in a distorted octahedral coordination environment. Two OAc- anions and six water molecules exist outside the [Mn(phen)2(H2O)2]2+ cation as counter ions and solvate molecules, respectively. The cations and anions are interconnected by the solvate water molecules which are hydrogen bonded to both aqua ligands and acetate oxygen atoms, building up the crystals of this compound to be a supramolecule-like aggregate.展开更多
The crystal of the title compound [Ni(dsen)]. EtOH, C32H32NiN2O5,Mr= 583. 33, (dsen = N, N'-disalicylidene-1, 2-dirnethoxyphenylethylenediamine) has been prepared and determined by X-ray single crystal diffraction...The crystal of the title compound [Ni(dsen)]. EtOH, C32H32NiN2O5,Mr= 583. 33, (dsen = N, N'-disalicylidene-1, 2-dirnethoxyphenylethylenediamine) has been prepared and determined by X-ray single crystal diffraction. The crystal belongs to the orthorhombic space group Pbca with parameters: observab1e reflections.The result reveals that nickel ion is coordinated by two nitrogen atoms of azomethene and two phenoxy atoms of the ligand. The coordination geometry around the Ni(II) is close to a Square plane (D4h).展开更多
The reaction of Ru (DMSO)_4Cl_2 with Dipheny1-[(pyrid-2-y1 ) amino]phosphine (pap) (1:2) gives the title compound Ru(PAP)_2Cl_2· 4EtoH. The crystallographic data for C_(24)H_(54)C_(12)N_4O_4P_2Ru: monoclinic,spac...The reaction of Ru (DMSO)_4Cl_2 with Dipheny1-[(pyrid-2-y1 ) amino]phosphine (pap) (1:2) gives the title compound Ru(PAP)_2Cl_2· 4EtoH. The crystallographic data for C_(24)H_(54)C_(12)N_4O_4P_2Ru: monoclinic,space group C2/c .α= 20. 47 (1) . b = 15. 431(9), c=15. 958(8) A , β=16. 82(4)°, V=4509(9) A3￣, Z=4, M_r= 912. 85, D_c= 1. 35 g/cm￣3,μ(MoKα) = 5. 71 cm￣(-1), F(000) =1092, R= 0. 073 and R_w = 0. 081 for 1700 observed reflections. The Ru atom is coordinated by two P atoms, two N atoms and two Cl atoms, forming octahedral coordination geomery.展开更多
基金the NNSFC (No. 20471061)the Science & Technology Innovation Foundation for the Young Scholar of Fujian Province (No. 2005J059)
文摘The title compound, [Mn4O2（O2CMe）6（MeOH）2（dbm）2]·2MeCOOH·2CH2Cl2 （Hdbm = dibenzoylmethane）, has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P/, with a = 10.729（3）, b = 12.269（3）, c = 13.085（4） A, a = 106.367（3）,β = 107.643（2）, γ = 94.771（2）°, V = 1547.9（7） A^3, Z = 1, C50H64Cl4Mn4O24, Mr= 1410.57, Dc= 1.513 g/cm^3, F（000） = 724, Rint = 0.0147, T= 293（2） K and p = 1.046 mm ^-1. The final R = 0.0359 and wR = 0.0938 for 5791 observed reflections with 1 〉 2σ（/）. The structure of the complex consists of one [Mn4（μ3-O）2]^8＋ core with four coplanar Mn atoms disposed in an extended ＂butterfly-like＂ arrangement and two O atoms triply bridging each ＂wing＂, and the peripheral ligation is provided by six by-MeCO2^-, two terminal ,μ2-dbm- groups at the two ends of the molecule, and two MeOH molecules on the central Mn atoms, lntermolecular O…H-O hydrogen bonding interactions are found within the structure of the compound.
基金This work was supported by 973 Project (001CB108906) and NNSFC (No. 30170229 and 20471061)
文摘A new one-dimensional azido-bridged manganese compound has been prepared and structurally characterized by X-ray diffraction. The complex [Mn（N3）2（H2O）3·C6H12N4]n crystallizes in space group Pnma with a = 6.5252 （5）, b = 9.3226（7）, c = 22.2070（15） ,A°, V= 1350.89（17） ,A°^3, Z = 4, Mr = 333.24, Dc = 1.639 g/cm^3, μ = 1.005 mm^-1 and F（000） = 692. The final refinement gave R = 0.0328 and wR = 0.0777 for 1085 observed reflections with I 〉 2σ（I）. The structure contains [Mn（N3）2（H2O）3]n polymeric chains and uncoordinated hexamethylenetetramine （HMTA） molecules with Mn/HMTA molar ratio of 1：1. The Mn atoms are bridged by end-to-end azido ligands to construct one-dimensional zig-zag infinite chains. Each Mn atom is six-coordinated by three N atoms of three azido ligands and three water O atoms, resulting in an octahedral geometry. Extending hydrogenbonding interactions involving water O atoms, azido and HMTA N atoms link the chains and HMTA molecules into a three-dimensional network.
文摘Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group C2/c with a=24. 825(8) . b=14.716(5) , c=18. 419(10)A,β=94. 57(3)°, V=6707. 54 A￣3;Z=4, Dc=1. 248 g/cm￣3. μ= 5. 002 cm￣(-1). F(000)=2664. The structure was solved by direct methods and refined to final R(Rω)=0.059(0.059) for 3183 observed reflections with I≥2.5σ(I). The centrosymmetric anion of the title compound contains two [V(mp)_3]￣(2-) fragments linked by a sodium ion, the crystallographic center of symmetry , through the μ2-O bridges. The Ⅴ(Ⅳ) atom is in a coordination environment intermediate between a trigonal prism and an ideal octahedron.
基金Supported by the NNSFC (No. 20471061)the Science & Technology Innovation Foundation for the Young Scholars of Fujian Province (No. 2005J059)
文摘A two-dimensional coordination polymer, [Cd（AIP）（Bpy）]n.nBpy, was hydrothermally synthesized by the reaction of hydrate cadmium acetate with 5-aminoisophthalic acid, lithium hydroxide, vanadiumpentoxide, sodium chloride and 2,2′-bipyridyl in water solution. It crystallizes in orthorhombic, space group C222 1, absolute structure parameter 0.00（7）, with a = 15.336（4）, b = 22.390（6）, c = 14.257（3）A, V = 4896（2）/~3, C28H21CdNsO4, Mr = 603.90, Z = 8, F（000） = 2432, Dc = 1.639 g/cm^3, μ = 0.939 mm^-1, T= 298（2） K, S = 1.001, R = 0.0296 and wR = 0.0813 for 5522 observed reflections （I 〉 2a（/））. In the title complex, each 5-aminoisophthalate ligand bridges three cadmium（Ⅱ） ions to form a two-dimensional layer structure.
基金This work was supported by the NNSFC (No. 20471061)the Science & Technology Innovation Foundation for the Young Scholar of Fujian Province (No. 2005J059)
文摘Two salicylate containing mononuclear manganese complexes formulated as [Mnand characterized by elemental analysis, IR and single-crystal X-ray diffraction analyses. Crystal data for compound 1： monoclinic, space group C2/c, a=30.748（6）, b=8.1933（13）, c=21.137（4） A, β=126.772（4）°, V=4265.5（13）A^3, Z=8, Mr=471.34, Dc=1.468 g/cm^3, μ=0.667 mm^-1, F（000）=1952,the final R=0.0637, wR=0.1783 （I 〉 2σ（I）） and GOOF=1.073; and those for compound 2： monoclinic,space group C2/c, a=14.505（5）, b=11.048（4）, c=20.711 （7）（A）, β=103.603（6）°, V=3225.6 （18）A^3, Z=4, Mr=668.65, Dc=1.377 g/cm^3, μ=0.466 mm^-1, F（000）=1416, the final R=0.0373, wR=0.1125 （I 〉2σ（I））, and GOOF=1.000. The Mn atoms of both complexes are six-coordinated in an axially elongated octahedral geometry for 1 and an axially compressed octahedral geometry for 2, and their oxidation states have been determined to be trivalent by bond valence sum calculation.
文摘Dinuclear palladium complex (Et_4N)_2[Pd_2(mp)_2 (mpH)_2 (mpH=_2-SC_6H_4OH ) (M_r = 971. 95 ) is prepared in a reaction of sodium 2-mercaptophenolate (Na_2mp) with PdCl_2. It crystallizes in monoclinic with space group P2_1/n, a=9. 088(1),b=17. 851 (4), c=12. 932(2) , β= 93. 21 (1)°, V=2094. 7(7), D_c=1. 54 g/cm￣3, F(000) = 1000, Z=2, and final R= 0. 044 and R_w= 0. 055 for 3090 reflections (I≥3σ(I)). Structure analysis revealed the multifunction chelating character of mp functions as S_tO_t(t for terminal) and S_bOH (b for bridging) in the complex.
文摘This paper presents the synthetic and structure studies of molybdenum（tungsten）-copper-sulphur-dialkyldithiocarbamate cluster compounds.The reactions of（M=Mo,W;n=0,2）,CuCl,and R<sub>2</sub>dtc￣-（R<sub>2</sub>=Me<sub>2</sub>,Et<sub>2</sub>,C<sub>4</sub>H<sub>8</sub>,C<sub>5</sub>H<sub>1</sub>0） yield a series of tetra-,hexa-,and heptanuclear cluster compounds.Their spectroscopic properties and the synthetic reaction mechanism are discussed.
基金This work was supported by the State Key Basic Research and Development Plan (G1998010100) and NNSFC+5 种基金 (No. 30170229) and Expert Project of Key Basic Research from Ministry of Sci.& Tech.
文摘The title complex [Mn(phen)2(H2O)2](OAc)26H2O (phen = 1,10-phenanthroline, C12H8N2, OAc = acetate, C2H3O2) with formula C28H38MnN4O12 and Mr = 677.56 has been syn- thesized and structurally characterized by X-ray diffraction. The crystal is of triclinic, space group P ?with a = 9.6201(5), b = 13.4663(7), c = 14.5375(8) , a = 108.428(1), b =93.898(1), g = 110.492(1), V = 1639.5(2) ?, Dc = 1.373 g/cm3, F(000) = 710, = 0.468 cm-1 and Z = 2. The final refinement gave R = 0.0522 and wR = 0.1259 for 4714 observed reflections with I > 2s(I). It consists of discrete [Mn(phen)2(H2O)2]2+ cation, two acetate anions and six lattice water molecules. The MnII ion coordinated by four nitrogen atoms from two chelating phen and two oxygen atoms from two cis-related water molecules is in a distorted octahedral coordination environment. Two OAc- anions and six water molecules exist outside the [Mn(phen)2(H2O)2]2+ cation as counter ions and solvate molecules, respectively. The cations and anions are interconnected by the solvate water molecules which are hydrogen bonded to both aqua ligands and acetate oxygen atoms, building up the crystals of this compound to be a supramolecule-like aggregate.
文摘The crystal of the title compound [Ni(dsen)]. EtOH, C32H32NiN2O5,Mr= 583. 33, (dsen = N, N'-disalicylidene-1, 2-dirnethoxyphenylethylenediamine) has been prepared and determined by X-ray single crystal diffraction. The crystal belongs to the orthorhombic space group Pbca with parameters: observab1e reflections.The result reveals that nickel ion is coordinated by two nitrogen atoms of azomethene and two phenoxy atoms of the ligand. The coordination geometry around the Ni(II) is close to a Square plane (D4h).
文摘The reaction of Ru (DMSO)_4Cl_2 with Dipheny1-[(pyrid-2-y1 ) amino]phosphine (pap) (1:2) gives the title compound Ru(PAP)_2Cl_2· 4EtoH. The crystallographic data for C_(24)H_(54)C_(12)N_4O_4P_2Ru: monoclinic,space group C2/c .α= 20. 47 (1) . b = 15. 431(9), c=15. 958(8) A , β=16. 82(4)°, V=4509(9) A3￣, Z=4, M_r= 912. 85, D_c= 1. 35 g/cm￣3,μ(MoKα) = 5. 71 cm￣(-1), F(000) =1092, R= 0. 073 and R_w = 0. 081 for 1700 observed reflections. The Ru atom is coordinated by two P atoms, two N atoms and two Cl atoms, forming octahedral coordination geomery.
