Kunchur Harish S, Mondal Dipanjan, Rao Sowmya, Mague Joel T, Balakrishna Maravanji S
Phosphorus Laboratory, Department of Chemistry, Indian Institute of Technology Bombay, Powai, Mumbai 400076, India.
Department of Chemistry, Tulane University, New Orleans, Louisiana 70118, USA.
Acta Crystallogr C Struct Chem. 2021 Nov 1;77(Pt 11):725-733. doi: 10.1107/S205322962101072X. Epub 2021 Oct 27.
The novel hemilabile ferrocenylbisphosphane 1,1'-bis(bis{2-[(dimethylamino)methyl]phenyl}phosphanyl)ferrocene, [Fe{CHP(CHCHNMe-o)}] (1), was synthesized by reacting bis(dichlorophosphanyl)ferrocene, [Fe{CH(PCl)}] with LiCHCHNMe-o. Treatment of 1 with gray selenium and anhydrous ZnCl yielded, respectively, the bisselenide (ferrocene-1,1'-diyl)bis(bis{2-[(dimethylamino)methyl]phenyl}phosphine selenide), [Fe(CHNPSe)] (2), and the dizinc complex [μ-1,1'-bis(bis{2-[(dimethylamino)methyl]phenyl}phosphanyl)ferrocene-κN,P:κN',P']bis[dichloridozinc(II)] dichloromethane monosolvate, [FeZnCl(CHNP)]·CHCl (3), and both have been structurally characterized. Both compounds crystallized with the asymmetric unit containing half a molecule and with the Fe atom on an inversion centre. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of 2 are from H...H (76.7%), C...H/H...C (13.2%) and Se...H/H...Se (7.1%) contacts, while those for 3 are from H...H (62.3%), Cl...H/H...Cl (24.4%) and C...H/H...C (10.9%) contacts.
新型半不稳定二茂铁基双膦1,1'-双（双{2-[(二甲氨基)甲基]苯基}膦基）二茂铁，[Fe{CHP(CHCHNMe-o)}] (1)，通过双（二氯膦基）二茂铁，[Fe{CH(PCl)}] 与LiCHCHNMe-o反应合成。用灰色硒和无水ZnCl分别处理1，得到双硒化物（二茂铁-1,1'-二基）双（双{2-[(二甲氨基)甲基]苯基}膦硒化物），[Fe(CHNPSe)] (2)，以及二锌配合物 [μ-1,1'-双（双{2-[(二甲氨基)甲基]苯基}膦基）二茂铁-κN,P:κN',P']双[二氯锌（II）]二氯甲烷单溶剂化物，[FeZnCl(CHNP)]·CHCl (3)，并且两者都已通过结构表征。两种化合物结晶时不对称单元包含半个分子，且Fe原子位于对称中心上。Hirshfeld表面分析表明，对2的晶体堆积贡献最大的是H...H（76.7%）、C...H/H...C（13.2%）和Se...H/H...Se（7.1%）接触，而对3的贡献最大的是H...H（62.3%）、Cl...H/H...Cl（24.4%）和C...H/H...C（10.9%）接触。
