The compound [NH4(NH3)4][B(C6H5)4].NH3 (1) was prepared by the reaction of NaB(C(6)H(5))(4) with a proton-charged ion-exchange resin in liquid ammonia. [NH(4)(NH(3))(4)][Ca(NH(3))(7)]As(3)S(6).2NH(3) (2) and [NH4(NH3)4][Ba(NH3)8]As3S6.NH3 (3) were synthesized by reduction of As(4)S(4) 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 H(3)N-H...N hydrogen bonds in all three compounds range from 1.82 to 2.20 A (DHA = Donor-H... Acceptor angles: 156-178 degrees). In 2 and 3, additional H(2)N-H...S bonds to the thioanions are observed, ranging between 2.49 and 3.00 A (DHA angles: 120-175 degrees). Two parallel phenyl rings of the [B(C(6)H(5))(4)](-) anion in 1 form a pi...pi hydrogen bond (C...C distance, 3.38 A; DHA angles, 82 degrees), leading to a dimeric [B(C6H5)4]2(2-) ion.
Supramolecular chemistry / Hydrogen bond / Low temperature crystal structure analysis / Ammonia / Crown ether / Cryptand / X-ray diffraction / Single crystal structure analysis Abstract. The crystal structures of the new polyether ligand-ammoniates C 12 H 24 O 6 Á 2 NH 3 (1) and C 18 H 36 O 6 N 2 Á 2 NH 3 (2) have been elucidated at 123 K by single crystal X-ray structure analysis. Compound 1 crystallizes as yellow plate-like crystals in the monoclinic space group P2 1 /c (no. 14) with unit cell parameters a ¼ 7.572(4) A, b ¼ 7.724(4) A and c ¼ 14.448(7) A with an angle b ¼ 91.79(6) . It consists of a molecule of [18]-crown-6 to which two ammonia molecules of crystallisation are bound by three hydrogen bonds each. The ammonia molecules reside below and above the plane of the crown ether oxygen atoms. Compound 2 crystallizes as colourless isometric crystals in the space group P6 3 22 (no. 182) with unit cell parameters a ¼ 8.2568(5) A and c ¼ 18.992(2) A. It consists of molecules of cryptand [2.2.2] which are connected by hydrogen bonds via ammonia molecules of crystallisation, resulting in two-dimensional layers parallel to the ab-plane.
NH4)3AsS4·5NH3 (I) and (NH4)3SbS4·8NH3 (II) are prepared by the reaction of Na3ES4 (E: As, Sb) with a proton-charged ion exchange material (Amberlyst 15) in liq. NH3 and characterized by single crystal XRD at 123 K. (I) crystallizes in the orthorhombic space group Pna2 1 with Z = 4 and (II) in the monoclinic space group P12 1 1 with Z = 2. The compounds show H 3 N-H···N hydrogen bonds and H 3 N-H···S bonds. The former interaction is responsible for the formation of [(NH3)2H] + , [(NH3)3H] + , and [(NH3)4H] + complexes, the last two of which are characterized by X-ray analysis for the first time. -(ROSSMEIER, T.; KORBER, N.
The compound [NH4(NH3)4][Co(C2B9H11)2] · 2 NH3 (1) was prepared by the reaction of Na[Co(C2B9H11)2] with a proton‐charged ion‐exchange resin in liquid ammonia. The ammoniate 1 was characterized by low temperature single‐crystal X‐ray structure analysis. The anionic part of the structure consists of [Co(C2B9H11)2]‐ complexes, which are connected via C‐H···H‐B dihydrogen bonds. Furthermore, 1 contains an infinite ∞1[{NH4(NH3)4}+(μ‐NH3)2] cationic chain, which is formed by [NH4(NH3)4]+ ions linked by two ammonia molecules. The N‐H···N hydrogen bonds range from 1.92 to 2.71Å (DHA = Donor···Acceptor angles: 136‐176°). Additional N‐H···H‐B dihydrogen bonds are observed (H···H: 2.3‐2.4Å).
The compound NH4HCN2 (1) was prepared by the reaction of H2CN2 with liquid ammonia. The ammonium salt 1 was characterized by a low temperature single‐crystal X‐ray structure analysis. The anionic part of the structure consists of HCN2− anions, which are connected via N–H···N bonds (H···N distance: 2.47Å, DHA: 165°). The N–H···N hydrogen bonds of the ammonium ion to the anions range from 2.00 to 2.14Å (DHA = Donor···Acceptor angles: 165–176°), all N–H···N interactions together give rise to a three‐dimensional network. 1 decomposes quantitatively to dicyandiamide at room temperature.
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