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End date: 2019 × Start date: 2016 × DDC: 540 × Type: article × Publisher: Chester : International Union of Crystallography ×

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    A second polymorph of 3,4-bis­­(6-bromo­pyridin-3-yl)-1,2,5-thia­diazole
    (Chester : International Union of Crystallography, 2016) Becker, Lisanne; Altenburger, Kai; Spannenberg, Anke; Arndt, Perdita; Rosenthal, Uwe
    The title compound, C12H6Br2N4S, a second polymorph in the triclinic space group P-1, is presented. As in the earlier reported monoclinic polymorph in the space group C2/c [Becker et al. (2016[Becker, L., Reiss, F., Altenburger, K., Spannenberg, A., Arndt, P., Jiao, H. & Rosenthal, U. (2016). Chem. Eur. J. In the press. doi: 10.1002/chem.201601337.]). Chem. Eur. J. In the press], the thia­diazole ring is planar with an r.m.s. deviation of 0.004 Å. The five-membered ring is tilted with respect to the two pyridyl substituents by 23.16 (7) and 49.47 (9)°. In the crystal, mol­ecules are linked by a weak non-bonding Br⋯N inter­action [3.056 (3) Å]. Furthermore, a column of mol­ecules is established along the b axis by π–π stacking inter­actions between the pyridine rings [centroid–centroid distances = 3.7014 (16) and 3.5934 (15) Å]. Additionally, a short inter­molecular Br⋯Br contact [3.3791 (6) Å] and Br⋯π-aryl contacts [3.6815 (11)–3.7659 (12) Å] towards the thia­diazole and pyridine rings are found.
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    1,1-Bis(di­phenyl­phosphor­yl)hydrazine
    (Chester : International Union of Crystallography, 2018) Höhne, Martha; Aluri, Bhaskar R.; Spannenberg, Anke; Müller, Bernd H.; Peulecke, Normen; Rosenthal, Uwe
    The title compound, C24H22N2O2P2, contains a diphosphazane backbone, as well as a hydrazine entity. The P—N—P diphosphazane unit and the N-amine N atom are almost coplanar, and the O atoms of the Ph2P(O) units are oriented trans to each other with respect to the P...P axis. In the crystal, centrosymmetrically related mol­ecules are linked into dimers by pairs of N—H...O hydrogen bonds, forming rings of graph-set motif R22(10).
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    Di-μ-chlorido-bis­­({4-[bis­(tri­methylsilyl)amino]-6-chloro-2,2,8,8-tetra­methyl-5,7-bis­(tri­methylsilyl)-3,5,7-tri­aza-4,6-diphospha-2,8-disilanon-3-en-4-ido-κ2P,P′}palladium(II)) di­ethyl ether disolvate
    (Chester : International Union of Crystallography, 2016) Höhne, Martha; Müller, Bernd H.; Spannenberg, Anke; Rosenthal, Uwe
    The title compound, [Pd2(C18H54Cl2N4P2Si6)2Cl2]·2C4H10O, features a dinuclear chloride-bridged palladium complex bearing two equivalents of the novel monoanionic mixed valent (λ3-P)—N—(λ5-P) ligand. A metal catalyzed coupling of two amino­imino­phosphines and a shift of one chlorine from the metal to the phospho­rus results in the (λ3-P)—N—(λ5-P) ligand. The mol­ecule contains a planar bimetallic Pd2Cl2 core with a crystallographic centre of inversion at the mid-point of the Pd⋯Pd line. The Pd atoms are in a distorted square-planar arrangement, where the P/Pd/P and Cl/Pd/Cl planes are twisted with respect to each other by a dihedral angle of 7.57 (4)°. The P—Pd—P bite angle is 71.380 (18)°. Intra­molecular C—H⋯Cl inter­actions are observed. In the crystal, the diethyl ether solvent mol­ecule is disordered over two sites, with an occupancy ratio of 0.788 (5):0.212 (5).
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    Tris(tetrahydrofuran-kO)tris[tris(thio-phen-2-yl)methanolato-kO]terbium(III)tetrahydrofuran monosolvate
    (Chester : International Union of Crystallography, 2011) Veith, Michael; Belot, Celine; Huch, Volker
    In the mononuclear title compound, [Tb(C13H9OS3)3(C4H8O)3]·C4H8O, the lanthanide cation is located on a threefold rotation axis and is surrounded by electron-rich ligands in an approximately octahedral geometry. One of the thienyl groups and the bound THF are disordered with 0.5:0.5 occupancy. The free THF is disordered around the threefold axis.