The title compound ttris-(diisopropyldithiophosphato)tris-μ-disulfidoμ3,-sulfido-cvclo-trimolybdenumj (3Mo-Mo) [diisopropyldithiophosphate], [Mo3S7 (S2P(iprO)2)3] [S2P(iprO)2] (Mr=1365. 39) is an ionic species which...The title compound ttris-(diisopropyldithiophosphato)tris-μ-disulfidoμ3,-sulfido-cvclo-trimolybdenumj (3Mo-Mo) [diisopropyldithiophosphate], [Mo3S7 (S2P(iprO)2)3] [S2P(iprO)2] (Mr=1365. 39) is an ionic species which consists of a discretecluster cation [Mo3S7 (S2P (iprO)2)3] + (ipr = isopropyl) and an anion [S2P (iprO)2]-It was synthesized from the reaction of (NH4)2MoS4 with HS2P (iprO)2. Crystallo-graphic data for its crystal: space group for 7356 independent reflec-'tions with The structure analysis reveals that the cation contains a typical(Mo3 (μ3,-S) (μ-S2)3]+ cluster core in which three molybdenum atoms form an isoscelestriangle;the structure of the free diisopropyldithiophosphate anion [S2P (iprO)2]- isdifferent obviously from the coordinated one.展开更多
The lsolobal displacement reaction between the dianion {M(CO)3[(h5-C5H4) C(O)C6H4C(O)(h5-C5H4)](CO)3M}2- and two molecules of [(m3-C)CO2Et]Co3(CO)9 gave rise to the formation of terephthaloyl(biscyclopentadienyl)-brid...The lsolobal displacement reaction between the dianion {M(CO)3[(h5-C5H4) C(O)C6H4C(O)(h5-C5H4)](CO)3M}2- and two molecules of [(m3-C)CO2Et]Co3(CO)9 gave rise to the formation of terephthaloyl(biscyclopentadienyl)-bridged double cluster complexes [(h5-C5H4)C(O)C6H4C(O)(h5-C5H4)]{[(m3-C)CO2Et]Co2M(CO)8}2 (M = Mo 1, M = W, 2). In the reaction, single cluster complexes[(m3-C)CO2Et]-Co2M(CO)8[h5-C5H4C(O)C6H4CO2CH3] ( M = Mo 3, M = W, 4) were yielded as by-products. All the cluster complexes were characterized by C/H analysis, IR and 1H NMR spectroscopy, and the structure of 3 has been determined by single-crystal X-ray diffraction method. Crystal data: Mr = 750.19, monoclinic, space group P21/c, a = 22.652(5), b = 8.954 (2), c = 14.530(3) ? b = 104.00(3), V = 2859.6(10) 懦, Z = 4, Dc = 1.743 mg/m? F(000) = 1488, m = 1.644 mm-1, the final R = 0.0555 and wR = 0.1353 for 5519 observations with I > 2s(I).展开更多
The new binuclear tungsten compound (Et4N)2W2S4(tdt)2 (H2tdt=H2S2C6H3CH3) (I) with Mr=1067. 97 has been prepared and characterized by IR andX-ray single crystal analysis. Compound (I) has been synthesized by two route...The new binuclear tungsten compound (Et4N)2W2S4(tdt)2 (H2tdt=H2S2C6H3CH3) (I) with Mr=1067. 97 has been prepared and characterized by IR andX-ray single crystal analysis. Compound (I) has been synthesized by two routes, ofwhich one was from the reaction of (NH4)WS4 with H2tdt, and the other is from lig-and substitution reaction of W2S4 (dip)2 by H2tdt. The compound contains a typical[W2S4j2+ moiety with a W-W bond of 2. 862(2) A. Its crystallographic data are: or-thorhombic, space group Pbca, a=23. 995 (9), b=31. 496 (7), c=10. 537 (5) A, V=7950(8) A3, Z=8, Dc= 1. 78 g·cm-3, p(MoKa)= 63. 37 cm-1 and R=0. 062 for1926 reflections with I≥3d(I). Synthesis, structure and reaction of the compound arediscussed in this paper.展开更多
The crystal structures of two new trinuclear Mo-S cluster compounds[Mo3S7(TDT)3](Et4N)2·DMF1 and[Mo3S3(O)2(TDT)3](Et4N)2 2 with bianion TDT(S2C6H3CH32-) as ligands are reported in this paper.There is a weak inter...The crystal structures of two new trinuclear Mo-S cluster compounds[Mo3S7(TDT)3](Et4N)2·DMF1 and[Mo3S3(O)2(TDT)3](Et4N)2 2 with bianion TDT(S2C6H3CH32-) as ligands are reported in this paper.There is a weak interaction between the cluster anions through S atoms(μ-S or S of TDT ligands) in each unit cell of these two compounds.Moreover,the mutual transformation between these two compounds by the cluster reaction is discussed.Crystal data:for 1 space group=P1,a=12.996(4),b=18.100(8),c=12.530(4),α=91.57(3),β=97.42(3),γ=69.04(3)°,Z=2,5309 reflections,R=0.052;for 2 space group C2/c,a=26.504(9),b=22.177(5),c=17.355(9),β=108.43(9)°,Z=8,2999 reflections,R=0.079.展开更多
文摘The title compound ttris-(diisopropyldithiophosphato)tris-μ-disulfidoμ3,-sulfido-cvclo-trimolybdenumj (3Mo-Mo) [diisopropyldithiophosphate], [Mo3S7 (S2P(iprO)2)3] [S2P(iprO)2] (Mr=1365. 39) is an ionic species which consists of a discretecluster cation [Mo3S7 (S2P (iprO)2)3] + (ipr = isopropyl) and an anion [S2P (iprO)2]-It was synthesized from the reaction of (NH4)2MoS4 with HS2P (iprO)2. Crystallo-graphic data for its crystal: space group for 7356 independent reflec-'tions with The structure analysis reveals that the cation contains a typical(Mo3 (μ3,-S) (μ-S2)3]+ cluster core in which three molybdenum atoms form an isoscelestriangle;the structure of the free diisopropyldithiophosphate anion [S2P (iprO)2]- isdifferent obviously from the coordinated one.
基金This work is supported by Natural Science Foundation of China
文摘The lsolobal displacement reaction between the dianion {M(CO)3[(h5-C5H4) C(O)C6H4C(O)(h5-C5H4)](CO)3M}2- and two molecules of [(m3-C)CO2Et]Co3(CO)9 gave rise to the formation of terephthaloyl(biscyclopentadienyl)-bridged double cluster complexes [(h5-C5H4)C(O)C6H4C(O)(h5-C5H4)]{[(m3-C)CO2Et]Co2M(CO)8}2 (M = Mo 1, M = W, 2). In the reaction, single cluster complexes[(m3-C)CO2Et]-Co2M(CO)8[h5-C5H4C(O)C6H4CO2CH3] ( M = Mo 3, M = W, 4) were yielded as by-products. All the cluster complexes were characterized by C/H analysis, IR and 1H NMR spectroscopy, and the structure of 3 has been determined by single-crystal X-ray diffraction method. Crystal data: Mr = 750.19, monoclinic, space group P21/c, a = 22.652(5), b = 8.954 (2), c = 14.530(3) ? b = 104.00(3), V = 2859.6(10) 懦, Z = 4, Dc = 1.743 mg/m? F(000) = 1488, m = 1.644 mm-1, the final R = 0.0555 and wR = 0.1353 for 5519 observations with I > 2s(I).
文摘The new binuclear tungsten compound (Et4N)2W2S4(tdt)2 (H2tdt=H2S2C6H3CH3) (I) with Mr=1067. 97 has been prepared and characterized by IR andX-ray single crystal analysis. Compound (I) has been synthesized by two routes, ofwhich one was from the reaction of (NH4)WS4 with H2tdt, and the other is from lig-and substitution reaction of W2S4 (dip)2 by H2tdt. The compound contains a typical[W2S4j2+ moiety with a W-W bond of 2. 862(2) A. Its crystallographic data are: or-thorhombic, space group Pbca, a=23. 995 (9), b=31. 496 (7), c=10. 537 (5) A, V=7950(8) A3, Z=8, Dc= 1. 78 g·cm-3, p(MoKa)= 63. 37 cm-1 and R=0. 062 for1926 reflections with I≥3d(I). Synthesis, structure and reaction of the compound arediscussed in this paper.
文摘The crystal structures of two new trinuclear Mo-S cluster compounds[Mo3S7(TDT)3](Et4N)2·DMF1 and[Mo3S3(O)2(TDT)3](Et4N)2 2 with bianion TDT(S2C6H3CH32-) as ligands are reported in this paper.There is a weak interaction between the cluster anions through S atoms(μ-S or S of TDT ligands) in each unit cell of these two compounds.Moreover,the mutual transformation between these two compounds by the cluster reaction is discussed.Crystal data:for 1 space group=P1,a=12.996(4),b=18.100(8),c=12.530(4),α=91.57(3),β=97.42(3),γ=69.04(3)°,Z=2,5309 reflections,R=0.052;for 2 space group C2/c,a=26.504(9),b=22.177(5),c=17.355(9),β=108.43(9)°,Z=8,2999 reflections,R=0.079.
