Et4N)2pd(i-mnt)2.fw = 647. 04, monoclinic,space group P21/c;a =9.511(1), b = 11.612(2), c=14.820(3)A,g= 94.38(1)',I'= 1631.9(5)A;7=2' D.=1.32g.cnl-;F (000)=672, R=0 0324, R. = 0'0298.Tills is a new e,\...Et4N)2pd(i-mnt)2.fw = 647. 04, monoclinic,space group P21/c;a =9.511(1), b = 11.612(2), c=14.820(3)A,g= 94.38(1)',I'= 1631.9(5)A;7=2' D.=1.32g.cnl-;F (000)=672, R=0 0324, R. = 0'0298.Tills is a new e,\alil[)le ot' X-raycharacterized Pd colllplexes with bivalent anion l,1 -dithiolato ligands an(i IIis reactioll witll(Et'N)zWS# gives (Et4N)ZWS4Pd(i-1lint).展开更多
A hexamolybdenum complex, [Et_4N]_2[Mo_6O_(19)H_4] crystal, with pentavalent and hexavalent molybdenum has been obtained in the solution of DMF and CH_3OH as organic solvents using MoCl_5 as a starting material. The c...A hexamolybdenum complex, [Et_4N]_2[Mo_6O_(19)H_4] crystal, with pentavalent and hexavalent molybdenum has been obtained in the solution of DMF and CH_3OH as organic solvents using MoCl_5 as a starting material. The crystallographic parameters obtained by X-ray diffraction analysis are: crthorhombic, a=10. 757(3), b=10. 763(2), c=14. 238(4)A, =1648. 9A^3; Z=2; space group Pnnm; final R=0. 047; final Rw=0. 051^(**)展开更多
A new trithiocarbonato Mo complex(Et_4N)_2[(S_2)Mo2O_2(μ-S)_2(CS_3)]was obtained from a system containing MoO_4^(2-),S_x^(2-),and CS_2 and characterized by IR and X-ray structural analysis. The complex crystallizes i...A new trithiocarbonato Mo complex(Et_4N)_2[(S_2)Mo2O_2(μ-S)_2(CS_3)]was obtained from a system containing MoO_4^(2-),S_x^(2-),and CS_2 and characterized by IR and X-ray structural analysis. The complex crystallizes in the (?)onoclinic space group P2_1/c with a=9.539(3)(?), b=20.745(2)(?),c=15.452(2)(?),β=94.58(2)°,and Z=4.The structure was solved by direct and difference Fourier synthesis methods.Least squares refinement using 2910 reflections with I>3σ(I)converged to R=0.054.The CS_3^(2-) iigand in the complex chelates to Mo atom and values of the C-S bond distances in the CS_3^(2-) ligend indicate a substantial contribution of three resonance forms.展开更多
The crystal structures of two isomorphic cluster compounds, (C5H7S2)[Mo3-(μ3-O)(μ-Cl)3 (μ-OAc)3Cl3] and (C5H2S2)[Mo3 (μ3-O)(μ-Br)3 (μ-OAc)3Cl3] have been investigated. The compounds have been pre...The crystal structures of two isomorphic cluster compounds, (C5H7S2)[Mo3-(μ3-O)(μ-Cl)3 (μ-OAc)3Cl3] and (C5H2S2)[Mo3 (μ3-O)(μ-Br)3 (μ-OAc)3Cl3] have been investigated. The compounds have been prepared by similar procedures, with the exception that the former has used MoCl3 as the starting material,展开更多
The title compound was prepared by dissolving 1.3g MoCl3·3H2O into 20 ml anhydrous formic acid. The solution was then heated and refluxed for half an hour. After cooling a bit, 20ml anhydrous ethanol saturated wi...The title compound was prepared by dissolving 1.3g MoCl3·3H2O into 20 ml anhydrous formic acid. The solution was then heated and refluxed for half an hour. After cooling a bit, 20ml anhydrous ethanol saturated with HCl and 0.5g (Et4N)I were added to the solution. The brown twin crystals were crystallized in three days. The formula of the product was confirmed by elemental chemical analysis. Found: Mo, 36.09; Cl, 26.84; C, 15.19; H, 3.54; N, 1.76. Calcd: Mo, 36.82; Cl, 27.21; C, 16.90; H, 2.97; N, 1.79. Diffraction work of a selected twin展开更多
文摘A hexamolybdenum complex, [Et_4N]_2[Mo_6O_(19)H_4] crystal, with pentavalent and hexavalent molybdenum has been obtained in the solution of DMF and CH_3OH as organic solvents using MoCl_5 as a starting material. The crystallographic parameters obtained by X-ray diffraction analysis are: crthorhombic, a=10. 757(3), b=10. 763(2), c=14. 238(4)A, =1648. 9A^3; Z=2; space group Pnnm; final R=0. 047; final Rw=0. 051^(**)
文摘A new trithiocarbonato Mo complex(Et_4N)_2[(S_2)Mo2O_2(μ-S)_2(CS_3)]was obtained from a system containing MoO_4^(2-),S_x^(2-),and CS_2 and characterized by IR and X-ray structural analysis. The complex crystallizes in the (?)onoclinic space group P2_1/c with a=9.539(3)(?), b=20.745(2)(?),c=15.452(2)(?),β=94.58(2)°,and Z=4.The structure was solved by direct and difference Fourier synthesis methods.Least squares refinement using 2910 reflections with I>3σ(I)converged to R=0.054.The CS_3^(2-) iigand in the complex chelates to Mo atom and values of the C-S bond distances in the CS_3^(2-) ligend indicate a substantial contribution of three resonance forms.
文摘The crystal structures of two isomorphic cluster compounds, (C5H7S2)[Mo3-(μ3-O)(μ-Cl)3 (μ-OAc)3Cl3] and (C5H2S2)[Mo3 (μ3-O)(μ-Br)3 (μ-OAc)3Cl3] have been investigated. The compounds have been prepared by similar procedures, with the exception that the former has used MoCl3 as the starting material,
文摘The title compound was prepared by dissolving 1.3g MoCl3·3H2O into 20 ml anhydrous formic acid. The solution was then heated and refluxed for half an hour. After cooling a bit, 20ml anhydrous ethanol saturated with HCl and 0.5g (Et4N)I were added to the solution. The brown twin crystals were crystallized in three days. The formula of the product was confirmed by elemental chemical analysis. Found: Mo, 36.09; Cl, 26.84; C, 15.19; H, 3.54; N, 1.76. Calcd: Mo, 36.82; Cl, 27.21; C, 16.90; H, 2.97; N, 1.79. Diffraction work of a selected twin