Zusammenfassung
The compound [NH4(NH3)(4)][B(C6H5)(4)].NH3 (1) was prepared by the reaction of NaB(C6H5)(4) with a proton-charged ion-exchange resin in liquid ammonia. [NH4(NH3)(4)][Ca(NH3)(7)]As3S6.2NH(3) (2) and [NH4(NH3)(4)][Ba(NH3)(8)]As3S6.NH3 (3) were synthesized by reduction of As4S4 with Ca and Ba in liquid ammonia. All ammoniates were characterized by low-temperature single-crystal X-ray structure ...
Zusammenfassung
The compound [NH4(NH3)(4)][B(C6H5)(4)].NH3 (1) was prepared by the reaction of NaB(C6H5)(4) with a proton-charged ion-exchange resin in liquid ammonia. [NH4(NH3)(4)][Ca(NH3)(7)]As3S6.2NH(3) (2) and [NH4(NH3)(4)][Ba(NH3)(8)]As3S6.NH3 (3) were synthesized by reduction of As4S4 with Ca and Ba in liquid ammonia. All ammoniates were characterized by low-temperature single-crystal X-ray structure analysis. They were found to contain the ammine-ammonium complex with the maximal possible number of coordinating ammonia molecules, the [NH4(NH3)(4)](+) ion. 1 contains a special dimer, the [{NH4(NH3)(4)}(2)(mu-NH3)(2)](2+) ion, which is formed by two [NH4(NH3)(4)](+) ions linked by two ammonia molecules. The H3N-(HN)-N-... hydrogen bonds in all three compounds range from 1.82 to 2.20 Angstrom (DHA = Donor-H(...)Acceptor angles: 156-178degrees). In 2 and 3, additional H2N-(HS)-S-... bonds to the thioanions are observed, ranging between 2.49 and 3.00 Angstrom (DHA angles: 120-175degrees). Two parallel phenyl rings of the [B(C6H5)(4)](-) anion in 1 form a pi(...)pi hydrogen bond ((CC)-C-... distance, 3.38 Angstrom; DHA angles, 82degrees), leading to a dimeric [B(C6H5)(4)](2)(2-) ion.