The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a=...The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a= 1.41999(2)nm, b=1.43467(2)nm, c=1.694610(10)nm, α=95.7250(10)°, β=92.2110(10)°, γ=92.6060(10)°, V=3.42829(7)nm3, Z=2, Dc=2.388g·cm-3, Mr=2465.10g·mol-1, μ=2.489mm-1, F(000)=2388, R1=0.0584, wR2=0.1461, S=1.164. The heteropolyanion is a bi capped pseudo Keggin complex. CCDC: 186645.展开更多
The reactions of [(h5-C5Me5)Mo(StBu)3] with equimolar FeBr3 in THF afforded a neutral tetranuclear cluster [(h5-C5Me5)2Mo2Fe2S4Br2] 1. The structure of 1 was determined by single-crystal X-ray diffraction analysis. 1 ...The reactions of [(h5-C5Me5)Mo(StBu)3] with equimolar FeBr3 in THF afforded a neutral tetranuclear cluster [(h5-C5Me5)2Mo2Fe2S4Br2] 1. The structure of 1 was determined by single-crystal X-ray diffraction analysis. 1 crystallizes in the monoclinic space group P21/n (No. 14) with a = 9.691(2), b = 15.204(2), c = 18.850(2) ? b = 96.44(1), V = 2759.8(7) ?, Z = 4, Mr = 862.08, Dc = 2.075 g/cm3, F(000) = 1680, m (MoKa) = 51.31 cm-1 and T = 296.2 K. With the use of 3667 observed reflections (I > 3.0s(I)), the structure was refined to R = 0.041 and Rw = 0.051. 1 is composed of a distorted Mo2Fe2S4 cubane core with two Br atoms and two h5-C5Me5 groups coordinating at the Fe and Mo sites, respectively. The lengths of MoMo and FeFe bonds are 2.826 and 2.773 ? respectively the mean length of MoFe bond is 2.751 ?展开更多
The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）O...The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）OCH3]M（CO）3Na （M = Mo or W） in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (（3-S）CoFeMo（CO）8[(5-C5H4C（NR）Me] [R = NHC6H3-2,4-（NO2）2] 3. All the compounds were characterized by elemental analyses, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P, a = 8.148（2）, b = 10.685（3）, c = 13.410（4） ?, ( = 100.077（5）, ( = 102.452（5）, ( = 91.108（6）(, V = 1120.4（5） ?3, Z = 2, Dc = 1.915 g/cm3, F（000） = 636, ( = 2.071 mm(1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I > 2（（I））.展开更多
文摘The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a= 1.41999(2)nm, b=1.43467(2)nm, c=1.694610(10)nm, α=95.7250(10)°, β=92.2110(10)°, γ=92.6060(10)°, V=3.42829(7)nm3, Z=2, Dc=2.388g·cm-3, Mr=2465.10g·mol-1, μ=2.489mm-1, F(000)=2388, R1=0.0584, wR2=0.1461, S=1.164. The heteropolyanion is a bi capped pseudo Keggin complex. CCDC: 186645.
基金This work was supported by the Key Laboratory of Organic Chemistry of Jiangsu Province at Suzhou University.
文摘The reactions of [(h5-C5Me5)Mo(StBu)3] with equimolar FeBr3 in THF afforded a neutral tetranuclear cluster [(h5-C5Me5)2Mo2Fe2S4Br2] 1. The structure of 1 was determined by single-crystal X-ray diffraction analysis. 1 crystallizes in the monoclinic space group P21/n (No. 14) with a = 9.691(2), b = 15.204(2), c = 18.850(2) ? b = 96.44(1), V = 2759.8(7) ?, Z = 4, Mr = 862.08, Dc = 2.075 g/cm3, F(000) = 1680, m (MoKa) = 51.31 cm-1 and T = 296.2 K. With the use of 3667 observed reflections (I > 3.0s(I)), the structure was refined to R = 0.041 and Rw = 0.051. 1 is composed of a distorted Mo2Fe2S4 cubane core with two Br atoms and two h5-C5Me5 groups coordinating at the Fe and Mo sites, respectively. The lengths of MoMo and FeFe bonds are 2.826 and 2.773 ? respectively the mean length of MoFe bond is 2.751 ?
基金the National Natural Science Foundation of China.
文摘The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）OCH3]M（CO）3Na （M = Mo or W） in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (（3-S）CoFeMo（CO）8[(5-C5H4C（NR）Me] [R = NHC6H3-2,4-（NO2）2] 3. All the compounds were characterized by elemental analyses, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P, a = 8.148（2）, b = 10.685（3）, c = 13.410（4） ?, ( = 100.077（5）, ( = 102.452（5）, ( = 91.108（6）(, V = 1120.4（5） ?3, Z = 2, Dc = 1.915 g/cm3, F（000） = 636, ( = 2.071 mm(1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I > 2（（I））.
