Crystal Structure of the Phase Pd32S14.

Synthesis, characterization, and structural properties of mercury(II), cadmium(II) and zinc(II) tripiperidinophosphine chalcogenide complexes

“…The smaller shifts of the selenides compared to that in the sulfides are consistent with the difference observed between P=O and P=S absorptions upon coordination [24] in related complexes and are reasonable since the vibrations involving the relatively heavy selenium atom would be less sensitive to coordination than those with the lighter oxygen or sulfur atoms. There is an increase in the frequency of the P-N vibration upon complexation (960-980 vs. 900-955 cm -1 in the free ligands) as observed in related systems [22], indicating that the nitrogen atoms are not involved in coordination. The 31 P NMR spectra show that the resonances of bound ligands are shifted to lower frequencies compared with those of the free ligand.…”

“…The tripiperidinohosphine chalcogenides (Pip3PE) were prepared using previously reported methods [22,23].…”

Virgidivarine, a sparteine-type alkaloid

“…Moreover, the Cambridge Crystallographic Data Base system displays a bewildering variety of single-bond C-C distances between 1.483 and 1.532 A, with an average of 1.517 A for 12 selected piperidine and piperidinium compounds published in the last decade (Kashino, Sumida & Haisa, 1972;Kashino, 1973 N(l')-C(2')-C(3') 107.3 (4) N(l)-C(2)-C(3) 110.5 (4) C(2')-C(3')-C(4') 111.6 (4) C(2)-C(3)-C(4) l I1.0 (4) C(3')-C(4')-C(5') 110.3 (4) C(3)-C(4)-C(5) 111.0 (4) C(4')-C(5')-C(6') 110.9 (5) C(4)-C(5)-C(6) I08.4 (4) C(5')-C(6')-N(I') 110.6 (4) C(5)-C(6)-N(1) 112.2 (4) C(6')-N(1')-C(2') 112.9 (4) C(6)-N(1)-C(2) 109.0 (4) N(I')-C(2')-C(5) 108.4 (4) C(2)-C(3)-C(11) 114.1 (4) C(3')-C(2')-C(5) 116.8 (4) C(4)-C(3)-C(1 l) 108.8 (4) C(2')-C(5)-C(6) 109.7 (4) C(2)-N(1)-C(7) 108.7 (4) C(2')-C(5)-C(4) 112.8 (4) C(6)-N(1)-C(7) 111.2 (4) O(12)-C(11)-O(13) 126.6 (5) N(1)-C(7)-C(8) 113.5 (4) O( 12)-C(1 I)-C(3) 115.7 (5) C(7)-C(8)-C(9) 112.7 (5) O(13)-C(11)-C(3) 117.6 (5) C(8)-C(9)-C(10) 126.3 (6) VIRGIDIVARINE, A SPARTEINE-TYPE ALKALOID Endocyclic N(1')-C(2')-C(3')-C(4') 57-5 (5) N(1)-C(2)-C(3)-C(4) 57.2 (5) C(2')-C(3')-C(4')-C(5') -57.5 (5) C(2)-C(3)-C(4)-C(5) -53.0 (5) C(3')-C(4')-C(5')-C(6') 55.2 (5) C(3)-C(4)-C(5)-C(6) 52.5 (5) C(4')-C(5')-C(6')-N(1') -55.6 (6) C(4)-C(5)-C(6)-N(1) 58.4 (5) C(5')-C(6')-N(1')-C(2') 58.6 (6) C(5)-C(6)-N(1)-C(2) 63.3 (5) C(6')-N(1')-C(2')-C(3') -58.5 (5) C(6)-N(1)-C(2)-C(3) -61.2 (5) Exocyclic N(1')-C(2')-C(5)-C(6) -77.7 (4) C(2)-N(1)-C(7)-C(8) -171.5 (4) C(3')-C(2')-C(5)-C(6) 161. I (4) C(6)-N(1)-C(7)-C(8) 68.5 (5) C(3')-C(2')-C(5)-C(4) 40.1 (5) N(1)-C(7)-C(8)-C(9) 175.2 (4) C( 12)-C(I 1)-C(3)-C(4) -85.3 (5) C(7)-C(8)-C(9)-C(10) 127.6 (7) O( 13)-C( I 1)-C(3)-C(4) 94.1 (5) Boucherle, 1974;Ducruix & Pascard-Billy, 1974;Bhattacharjee & Chacko, 1977;Jask61ski, Gdaniec & Kosturkiewicz, 1977;Minshall & Sheldrick, 1977;Arte, Feneau-Dupont, Declercq, Germain & Van Meerssche, 1977;Romming & Songstad, 1978;Jask61ski, Kosturkiewicz, Mickiewicz-Wicklacz & Wiewiorowski, 1979). The bond lengths of C(11)-O(12) and C(11)-O(13) do not differ significantly: Al and cr(Al) being 0.010 and 0.0085 ,/t respectively.…”

(2S,4S,5R)-2-Chloro-3,4-dimethyl-5-phenyl-1,3,2-oxazaphospholidine 2-sulphide, C10H13ClNOPS

“…This interaction probably causes a shortening of the P-N single bond, 1.622 (3)/~, which is significantly shorter than in the four structures cited above: 1.640 (3)A in (I), mean 1.653 (5)/~, in (IV), mean 1.654 (3) ,/~ in (II) and mean 1.693 (10) A. in (III). It is also shorter than the P-N bond in 2-phenyl-l,3di-p-tolyl-1,3,2-diaz apho spholidine (V) (Clardy, Kolpa & Verkade, 1974), 1.700(5).A, and shorter than the shortest P--N distances 1.65-1.66/~, found by Romming & Songstad (1979) in tris-(morpholino), tris(piperidino) and tris(dimethylamino)phosphine selenides. Only P-N bonds in some cyclophosphazenes are shorter, e.g.…”