Kristall‐ und Molekülstruktur von Bis(1,1‐diethyl‐3‐thiobenzoyl‐thioureato)nickel(II)

Abstract

Bis(1, 1‐diethyl‐3‐thiobenzoyl‐thioureato)nickel(II) bildet zwei Modifikationen, deren Strukturen mittels Röntgenkristallstrukturanalyse ermittelt wurden. Die monokline Modifikation kristallisiert in der Raumgruppe P21/n mit den Gitterkonstanten a = 13,709, b = 8,571, c = 12,803 Å, β = 68,10° und Z = 2. Die trikline Modifikation kristallisiert in der Raumgruppe I1 mit den Gitterkonstanten a = 14,406, b = 7,761, c = 11,734 Å, α = 86,10, β = 97,39, γ = 90,18° und Z = 2. Die Molekülstrukturen beider Modifikationen sind nahezu identisch (Packungspolymorphie). Die Koordination ist exakt planar, die Liganden sind in trans‐Stellung angeordnet. Die mittlere NiS‐Bindungslänge beträgt 2,153 Å für die monokline und 2,163 Å für die trikline Form. Die Chelatringe weichen von der Planarität ab.

Structure of (cis,trans,cis-η-1,5,9-cyclotridecatriene)nitratosilver(I)

“…However, in some derivatives of the sesquiterpene humulene, a trans, trans,trans-l,4,8-cycloundecatriene, angles of 8 to 23 ° were obtained (MacPhail & Sim, 1966;Hall, Nimgirawath, Raston, Sittatrakul, Thadaniti, Thirasasana & White, 1981;Russell, Sim & White, 1982;MacAlpine, Porte & Sim, 1982;Khan, MacAlpine, Porte & Sire, 1983). In a trans-oxacycloundecene derivative we found 10 °, while in a related cis-oxacycloundecene a value of only 3 ° was obtained (Sieler, Richter, Haufe, Lindqvist, Andersen & Faure, 1985;Sim & Haufe, 1984, unpublished results). In the cis,trans-l,5-cyclodecatriene-AgNO 3 complex the cis double bond is also nearly planar, while the trans-double-bond torsion is 22 ° (Rogers & Smart, 1969).…”

Structure of two modifications of 1,1-diethyl-3-thiobenzoylthiourea

“…The molecules in modification (II) do not show any major structural differences from those in (I). Table 3 gives a comparison of selected bond distances and angles of the free ligand in both modifications with those of the nickel chelate, which also exists in two polymorphic modifications (Sieler et aL, 1985).…”

“…1.404 C(8)--C(9) 1.391 (10) C(81)-C(91) 1.399 C(9)-C(10) 1.377 (12) C(91)-C(I01) 1.347 C(10)-C(ll) 1.364(11) C(101)-C(III) 1.368 C(11)-C(12) 1.371 (9) C(111)-C(121) 1.356 C(7)-C(12) 1.396 (8) (Sieler et al, 1985) CI2HI6N2S2 [Ni(CI2HtsN2S2)2] (I) (II)* (I) (II) S(1)-C(2) 1-675 (6) ,1.675 (8) 1.75 (2) 1.73 (I) S(2)--C(I) 1.639 (6) 1.635 (8) 1.71 (2) 1.71 (1) N(I)--C(2) 1.408 (7) 1-430 (10) 1.29 (3) 1.34 (2) N(I)--C(I) 1.365 (7) 1.359 (9) 1.27 (3) 1.29 (2) N(2)--C (2) 1.335 (7) 1.310 (10) 1.41 (3) 1.35 (2) S(I)--C(2)--N(1) 119.0 (4) 117.8 (7) 129 (2) 130 (1) As in (I), C(1)-S(2) is about 0.04 A shorter than C(2)-S(1) which corresponds to distances in thioureas (Kunchur & Truter, 1958;Elcombe & Taylor, 1968;Dias & Truter, 1964) and thioamides (Truter, 1960;Walter, Harto & Voss, 1976).…”

“…N-Chalcogenoacylthioureas are of great interest as chelating ligands in complex chemistry. Whereas the structures of N-chalcogenoacylthiourea complexes of transition-metal ions (Fitzl, Beyer, Sieler, Richter, Kaiser & Hoyer, 1977;Knuuttila, Knuuttila, Hennig & Beyer, 1982;Sieler, Richter, Braun, Beyer, Lindqvist & Andersen, 1985) have been described, the structures of the corresponding ligands are generally unknown. We now report the crystal structure of the title compound (R 1 = R 2 --C2H5, R a = C6H5, X = S).…”