Treatment of [Fe₂(CO)₆(μ-S₂C₃H₆)] (1) with triphenylstibine in a 1:1 molar ratio at room temperature in presence of Me₃NO resulted compound [Fe₂(CO)₅(SbPh₃)(μ-S₂C₃H₆)] (2) in 88% yield as red crystals. When the reaction was carried out under a 1:5 molar ratio in presence of Me₃NO, it resulted a monosubstituted compound [Fe₂(CO)₅(SbPh₃)(μ-S₂C₃H₆)] (2) in 63% yield along with a disubstituted compound [Fe₂(CO)₄(SbPh₃)₂(μ-S₂C₃H₆)] (3) in low yield (8%) as red crystals. Reaction of 2 with triphenylstibine in a 1:5 molar ratio under same condition resulted 3 in moderate yield (46%). Compounds 2 and 3 were characterized by elemental analyses, IR, ¹H NMR and ¹³C NMR spectroscopic data. Crystal structures of the compounds were unambiguously determined by single crystal X-Ray diffraction studies. Compound 2 crystalized as monoclinic crystal system with the space group P2₁/c, a = 9.464(4) Å, b = 16.902(7) Å, c = 17.081(7) Å, β = 101.216(13)° and Z = 4. Compound 3 was triclinic, space group P-1, a = 9.552(3) Å, b = 13.985(5) Å, c = 16.487(6) Å, α = 78.372(16)°, β = 89.976(14)°, γ = 71.638(11)° and Z = 2.

Graphic Abstract

Two new diiron propane-1,3-dithiolate complexes, [Fe₂(CO)₅(SbPh₃)(μ-S₂C₃H₆)] (2) and [Fe₂(CO)₄(SbPh₃)₂(μ-S₂C₃H₆)] (3), were synthesized by the displacement of carbonyl groups from [Fe₂(CO)₆(μ-S2C₃H₆)] (1) with triphenylstibine, and the resulting complexes were structurally characterized.

Solid state molecular structure of compound 2 (left) and compound 3 (right)

中文翻译：

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三苯基锡在二铁丙烷-二硫代磺酸盐络合物中的羰基置换反应：[Fe 2（CO）6-n（SbPh 3）n（μ-S2 C 3 H 6）]的晶体结构（n = 1和2）

的治疗的[Fe ₂（CO）₆（μ-S ₂ C ^ ₃ ħ ₆）]（1）在一个1三苯：在我的存在下，在室温下1摩尔比₃ NO导致化合物的[Fe ₂（CO）₅（灰飞虱₃）（μ-S ₂ C ^ ₃ ħ ₆）]（2）以88％产率，为红色晶体。当反应在1下进行：在我的存在5摩尔比₃ NO，它导致单取代的化合物的[Fe ₂（CO）₅（灰飞虱₃）（μ-S ₂ Ç₃ ħ ₆）]（2）在63产量与二取代的化合物的[Fe沿％₂（CO）₄（灰飞虱₃）₂（μ-S ₂ C ^ ₃ ħ ₆）]（3），产率较低（8％）为红色晶体。在相同条件下，2与三苯基二b啶的摩尔比为1：5的反应产生3的中等收率（46％）。化合物2和3通过元素分析，IR，¹ H NMR和¹³进行表征13 C NMR光谱数据。通过单晶X射线衍射研究明确地确定了化合物的晶体结构。以空间组P 2 ₁ / c结晶为单斜晶系的化合物2，a  = 9.464（4）Å，b  = 16.902（7）Å，c  = 17.081（7）Å，β  = 101.216（13）°和Z  = 4.化合物3为三斜晶系，空间群为P -1，a  = 9.552（3）Å，b  = 13.985（5）Å，c  = 16.487（6）Å，α  = 78.372（16）°，β  = 89.976（ 14）°，γ = 71.638（11）°和Z  = 2。

图形摘要

两个新的二铁丙烷-1,3-二硫醇盐复合物，的[Fe ₂（CO）₅（灰飞虱₃）（μ-S ₂ C ^ ₃ ħ ₆）]（2）和的[Fe ₂（CO）₄（灰飞虱₃）₂（μ-S ₂ C ^ ₃ ħ ₆）]（3）中，通过羰基的离的[Fe位移合成₂（CO）₆（μ-S2C ₃ ħ ₆）]（1）用三苯基，将所得复合体进行了结构表征。

化合物2（左）和化合物3（右）的固态分子结构