The reaction of [Fe2S2（CO）6] with one equiv.of o-OCH3C6H4CH2Br under the re-duction of LiBHEt3 in dry THF afforded a tetranuclear cluster [（μ4-S）{（μ-SCH2（o-OCH3）Ph）Fe2（CO）6}2]（1）.Complex 1 crystallizes i...The reaction of [Fe2S2（CO）6] with one equiv.of o-OCH3C6H4CH2Br under the re-duction of LiBHEt3 in dry THF afforded a tetranuclear cluster [（μ4-S）{（μ-SCH2（o-OCH3）Ph）Fe2（CO）6}2]（1）.Complex 1 crystallizes in monoclinic,space group P21/n with a = 16.5623（6）,b = 12.8265（5）,c = 18.2702（7） ,β = 115.95（1）o,V = 3489.9（4） 3,Z = 4,μ = 1.87 mm-1,Dc = 1.709 Mg/m3,T = 296（2） K,C28H18Fe4O14S3,Mr = 898.03,F（000） = 1800,S = 1.10,R = 0.032 and wR = 0.058.Complex 1 consists of two diiron fragments possessing a {Fe2（CO）6} core.The two diiron units are bridged by an inorganic sulfide in a μ4-S binding mode and the sulfide is in a distorted tetrahedral geometry with the four iron atoms at each corner of the distorted tetrahedral.In its solid state,two types of non-classic intermolecular hydrogen bonding interactions plus a weak π-π stacking interaction led to a 2-D network.展开更多
The title complex,（μ-pdt）Fe_2（CO）_5（Ph_2PCH_3）（pdt = SCH_2CH_2CH_2S）,was obtained by the reaction of the parent complex（μ-pdt）Fe_2（CO）_6 with Ph_2PCH_3 and Me_3NO·2H_2O in good yield（90%）. The tit...The title complex,（μ-pdt）Fe_2（CO）_5（Ph_2PCH_3）（pdt = SCH_2CH_2CH_2S）,was obtained by the reaction of the parent complex（μ-pdt）Fe_2（CO）_6 with Ph_2PCH_3 and Me_3NO·2H_2O in good yield（90%）. The title complex was characterized by IR,~1H NMR,^（31）P{~1H} NMR and ^（13）C{~1H} NMR spectroscopy as well as by single-crystal X-ray diffraction analysis. The molecular structure shows that the title complex contains a butterfly diiron propanedithiolate cluster with five terminal carbonyls and a monophosphine ligand Ph_2PCH_3. The crystal packing diagram reveals that intermolecular C H···O hydrogen bonds between CH_2 and carbonyls,π-π stacking interactions and van der Waals＇ interactions stabilize the solid state to form a three-dimensional network.展开更多
基金supported by the Education Department of Jiangxi Province (GJJ11033)
文摘The reaction of [Fe2S2（CO）6] with one equiv.of o-OCH3C6H4CH2Br under the re-duction of LiBHEt3 in dry THF afforded a tetranuclear cluster [（μ4-S）{（μ-SCH2（o-OCH3）Ph）Fe2（CO）6}2]（1）.Complex 1 crystallizes in monoclinic,space group P21/n with a = 16.5623（6）,b = 12.8265（5）,c = 18.2702（7） ,β = 115.95（1）o,V = 3489.9（4） 3,Z = 4,μ = 1.87 mm-1,Dc = 1.709 Mg/m3,T = 296（2） K,C28H18Fe4O14S3,Mr = 898.03,F（000） = 1800,S = 1.10,R = 0.032 and wR = 0.058.Complex 1 consists of two diiron fragments possessing a {Fe2（CO）6} core.The two diiron units are bridged by an inorganic sulfide in a μ4-S binding mode and the sulfide is in a distorted tetrahedral geometry with the four iron atoms at each corner of the distorted tetrahedral.In its solid state,two types of non-classic intermolecular hydrogen bonding interactions plus a weak π-π stacking interaction led to a 2-D network.
基金Supported by the Natural Science Foundation of Zhejiang Province(No.LY16B020009)K.C.Wong Education Foundation
文摘The title complex,（μ-pdt）Fe_2（CO）_5（Ph_2PCH_3）（pdt = SCH_2CH_2CH_2S）,was obtained by the reaction of the parent complex（μ-pdt）Fe_2（CO）_6 with Ph_2PCH_3 and Me_3NO·2H_2O in good yield（90%）. The title complex was characterized by IR,~1H NMR,^（31）P{~1H} NMR and ^（13）C{~1H} NMR spectroscopy as well as by single-crystal X-ray diffraction analysis. The molecular structure shows that the title complex contains a butterfly diiron propanedithiolate cluster with five terminal carbonyls and a monophosphine ligand Ph_2PCH_3. The crystal packing diagram reveals that intermolecular C H···O hydrogen bonds between CH_2 and carbonyls,π-π stacking interactions and van der Waals＇ interactions stabilize the solid state to form a three-dimensional network.
