Reaction of an ethylenediamine (en) solution of the Zintl phase precursor K(4)Ge(9) with FeAr(2) (Ar = 2,6-Mes(2)C(6)H(3)) in the presence of 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) yielded the endohedral Zintl ion [Fe@Ge(10)](3-) (1) which was crystallographically characterized as a [K(2,2,2-crypt)](+) salt in [K(2,2,2-crypt)](3)[Fe@Ge(10)]*2en. This unprecedented Zintl ion exhibits a pentagonal prismatic 10-atom germanium cage with an interstitial iron atom in the central cavity. Confirmation of the existence of the cluster anion in solution was corroborated by positive and negative ion mode electrospray mass spectrometry.
Reactions between ethylenediamine (en) solutions of the intermetallic Zintl phases K(3)E(7) (E = P, As) and a series of homoleptic post-transition metal organometallics such as Cu(5)(Mes)(5), M(C(6)H(5))(2) (M = Zn, Cd) and In(C(6)H(5))(3) have yielded a family of novel bimetallic cluster anions. These new species were isolated as [K(2, 2,2-crypt)](+) salts in [K(2,2,2-crypt)](4)Cu(2)E(14) (E = P (1), As (2)), [K(2,2,2-crypt)](4)ZnE(14) (E = P (3), As (4)), [K(2,2,2-crypt)](4)CdP(14) x 6py (5) and [K(2,2,2-crypt)](2)E(7)InPh(2) (E = P (6), As (7)). Species 2, 3, 5 and 6 were crystallographically characterised by single-crystal X-ray diffraction. The stability of all of the cluster anions in solution was confirmed by electrospray mass-spectrometry and by (1)H, (13)C{(1)H} and (31)P{(1)H} NMR spectroscopy when possible.
Covalent organic framework (COF) membranes used for selective removal of CO were believed as an efficient and low-cost solution to energy and environmental sustainability. In this study, the amide modified COF nanosheet cluster with a 2D structure was facilely prepared through solid reaction, exhibiting good adsorption-based CO selectivity (223 at 273 K and 90 at 298 K) toward N. Remarkably, the mixed matrix membrane (MMM) that consists of a lesser amount of COF filler (1 wt %) shows promising CO/N gas selectivity (∼64). In addition, the competitive adsorption prompts the selectivity to ∼72 under an equimolar CO/N mixture, which surpasses the values of all reported COF membranes. It is worth to note that the binary gas separation is stable during 120 h.
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