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
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
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
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.
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.
