172295-53-3Relevant articles and documents
Polysulfonyl Amines. LXIX. Novel Pnictogen Disulfonylamides: Synthesis of Bismuth Dimesylamides and Crystal Structures of the Twelve-Membered Cyclodimer [Ph2BiN(SO2Me)2]2 and of the Ionic Complex [H(OAsPh3)2](1+)(MeSO2)2N(1-)
Weitze, Achim,Henschel, Dagmar,Blaschette, Armand,Jones, Peter G.
, (2008/10/08)
The novel bismuth(III or V) disulfonylamides Ph2BiN(SO2Me)2 (1), PhBi[N(SO2Me)2]2 (2), PhBi[N(SO2Me)2]Br (3), Bi[N(SO2Me)2]2Cl (4), Bi[N(SO2Me)2]Cl2*12-crown-4 (5) and Ph3Bi[N(SO2Me)2]Cl (6) were obtained by acidolysis of Ph3Bi with HN(SO2Me)2 (-1), by metathesis of AgN(SO2Me)2 with Ph2BiCl (-1) or PhBiBr2 (-2,3), by condensation of BiCl3 with Me3SiN(SO2Me)2(-4; in presence of 12-crown-4: -5), or by oxidative addition of ClN(SO 2Me)2 to Ph3Bi (-6). Independently of the molar ratio employed, triphenylarsane oxide and dimesylamine form the crystalline 2/1 complex [H(OAsPh3)](1+)(MeSO2)2N(1-) (7). The crystal packing of 7 (monoclinic, space group C2/C) consists of discrete cations displaying crystallographic Ci symmetry and a strong O...H...O hydrogen bond (H atom located on a centre of symmetry, O...O' 241.2 pm, As-O...O' 120°, As-O 168.3 pm), andchiral anions with crystallographic C2 symmetry (N-S 157.3 pm, S-N-S 12 2.9°). In the solid state, the bismuth(III) compound (1) (triclinic, space group P1-) is a cyclodimer with crystallographic Ci symmetry, in which two Ph2Bi(1+) cations are connected through two (α-O, ω-O)-donating dimesylamide ligands to form a roughly twelve-membered [BiOSNSO]2 ring (Bi-O 239.7 and 246.6, O-S 148.0 and 145.4, S-N 157.7 and 159.2 pm, Bi-O-S 126.6 and 127.5°). The bismuth atom adopts a pseudo-trigonal bipyramidal geometry (O-Bi-O 165.4, C-Bi-C 93.0, O-Bi-C 83.8 to 86.5°). The essentially similar conformations of the discrete anion in 7 and of the bidentate bridging lignad in 1 are discussed in detail.