Preparation and reactivity towards hydrazines of bis(cyanamide) and bis(cyanoguanidine) complexes of the iron triad

Gabriele Albertin; Stefano Antoniutti; Alfonso Caia; Jesús Castro

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Preparation and reactivity towards hydrazines of bis(cyanamide) and bis(cyanoguanidine) complexes of the iron triad

机译：三合一铁的双（氰酰胺）和双（氰基胍）配合物的制备及其对肼的反应性

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Bis(diethylcyanamide) [Fe(N≡CNEt_2)_2L_4](BPh_4)_2 1a and bis(cyanoguanidine) [Fe{N≡CN(H)C(NH_2)v NH}_2L_4](BPh_4)_2 1b [L = P(OEt)_3] complexes were prepared by allowing iron(II) chloride to react first with an excess of P(OEt)3 and then of the appropriate cyanamide, followed by addition of an excess of NaBPh4. Instead, bis(complexes) of ruthenium and osmium [M(N≡CNEt_2)_2L_4](BPh_4)_2 2a, 3a and [M{N≡CN(H)C- (NH_2)vNH}_2L_4](BPh_4)_2 2b, 3b (M = Ru 2, Os 3) were prepared by reacting hydrides MH2L4 first with either triflic acid HOTf or methyltriflate MeOTf and then with an excess of the appropriate cyanamide. Hydridediethylcyanamide [MH(N≡CNEt_2)L_4]BPh_4 4a, 5a and hydride-cyanoguanidine complexes [MH{N≡CN(H)- C(NH_2)vNH}L_4](BPh_4)_2 4b, 5b (M = Ru 4, Os 5) were also obtained by reacting MH_2L_4 first with one equivalent of HOTf or MeOTf and then with the appropriate cyanamide. Treatment of bis(cyanamide) and bis- (cyanoguanidine) complexes 1–3 with hydrazines RNHNH_2 afforded hydrazinecarboximidamide derivatives [M{η~2-N(H)vC(NEt_2)N(R)NH_2}L_4](BPh_4)_2 6a–12a and [M{η~2-N(H)vC[NvC(NH_2)_2]N(R)NH_2}L_4](BPh_4)_2 6b–12b (M = Fe 6–8, Ru 9, 10, Os 11, 12; R = H 6, 9, 11, Me 7, 10, 12, Ph 8). A reaction path involving nucleophilic attack by hydrazine on the cyanamide carbon atom is proposed. All the complexes were characterised by spectroscopy and X-ray crystal structure determination of [Os{η~2-NHvC[NvC(NH_2)_2]- N(CH_3)NH_2}{P(OEt)_3}_4](BPh_4)_2 12b.

机译：双（二乙基氰酰胺）[Fe（N≡CNEt_2）_2L_4]（BPh_4）_2 1a和双（氰基胍）[Fe {N≡CN（H）C（NH_2）v NH} _2L_4]（BPh_4）_2 1b [L = P （OEt）_3]配合物的制备方法是，先使氯化铁（II）与过量的P（OEt）3，然后与适当的氰胺反应，然后加入过量的NaBPh4。取而代之的是钌和的双（络合物）[M（N≡CNEt_2）_2L_4]（BPh_4）_2 2a，3a和[M {N≡CN（H）C-（NH_2）vNH} _2L_4]（BPh_4）_2 2b通过使氢化物MH2L4首先与三氟甲磺酸HOTf或三氟甲磺酸甲酯MeOTf反应，然后与过量的适当氰胺反应，制备3b（M = Ru 2，Os 3）。氢化二乙基氰酰胺[MH（N≡CNEt_2）L_4] BPh_4 4a，5a和氢化物-氰基胍络合物[MH {N≡CN（H）-C（NH_2）vNH} L_4]（BPh_4）_2 4b，5b（M = Ru 4， Os 5）也通过首先使MH_2L_4与一当量的HOTf或MeOTf反应，然后与适当的氰胺反应而获得。用肼RNHNH_2处理双（氰胺）和双-（氰基胍）配合物1-3，得到肼甲酰亚胺酰胺衍生物[M {η〜2-N（H）vC（NEt_2）N（R）NH_2} L_4]（BPh_4）_2 6a –12a和[M {η〜2-N（H）vC [NvC（NH_2）_2] N（R）NH_2} L_4]（BPh_4）_2 6b-12b（M = Fe 6-8，Ru 9，10， Os 11、12; R = H 6、9、11，Me 7、10、12，Ph 8）。提出了涉及肼对氰胺碳原子的亲核进攻的反应路径。通过[Os {η〜2-NHvC [NvC（NH_2）_2]-N（CH_3）NH_2} {P（OEt）_3} _4]（BPh_4）_2的光谱学和X射线晶体结构测定来表征所有配合物12b。

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《Dalton transactions: An international journal of inorganic chemistry》 |2014年第19期|共10页
作者
Gabriele Albertin; Stefano Antoniutti; Alfonso Caia; Jesús Castro;
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Preparation; reactivity towards hydrazines; bis(cyanamide);

机译：制备;对肼的反应性;双氰胺;

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1. Preparation and reactivity towards hydrazines of bis(cyanamide) and bis(cyanoguanidine) complexes of the iron triad [J] . Gabriele Albertin, Stefano Antoniutti, Alfonso Caia, Dalton transactions: An international journal of inorganic chemistry . 2014,第19期

机译：三合一铁的双（氰酰胺）和双（氰基胍）配合物的制备及其对肼的反应性
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4. Synthesis of Metal-Bis(N-(3-Ethylphenyl))-Pyridine-2-Acetyl-Hydrazine Complexes and Evaluation of their Magnetic and Antimicrobial Activity [C] . Jagvir Singh, Kamelesh Kumari, Prashant Singh, International Workshop on Functional Materials . 2012

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5. New chemistry of organoplatinum complexes. Preparation and reactivity studies of 3-oxaplatinacyclobutane complexes and platinum bis(phosphonium ylide) complexes [D] . Hoover, James Franklin 1989

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Preparation and reactivity towards hydrazines of bis(cyanamide) and bis(cyanoguanidine) complexes of the iron triad

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