Reaction of Co(NCS)2 with 1,2-bis(4-pyridyl)-ethane (bpa) leads to the formation of [Co(NCS)2(bpa)2]n, which, on heating, transforms into the new layered coordination polymer [Co(NCS)2(bpa)]n. This compound can also be prepared in solution, but because no reasonable single crystals are available, its crystal structure was determined from X-ray powder data from scratch. In the crystal structure of [Co(NCS)2(bpa)]n, the cobalt(II) cations are coordinated by two S-bonded and two N-bonded thiocyanato anions and two N atoms of the bpa co-ligands in a distorted octahedral geometry. The cobalt(II) cations are linked into chains by pairs of μ-1,3 bridging thiocyanato anions. These chains are further connected into layers by the 1,2-bis(4-pyridyl)-ethane ligand. The compound was magnetically characterized, and, for comparative purposes, the complementary magnetic study of a known and very similar compound, [Co(NCS)2(bpe)]n (bpe = 1,2-bis(4-pyridyl)-ethylene), was also undertaken. The compounds differ in their interchain interactions, which are antiferromagnetic but significantly greater for [Co(NCS)2(bpe)]n. Magnetic measurements indicate that [Co(NCS)2(bpa)]n is a canted antiferromagnet with Néel temperature TN = 3.1 K and that Co(NCS)2(bpe) is an antiferromagnet with TN = 4.0 K. Both compounds show a metamagnetic transition with a critical field HC ∼ 40 Oe and ∼ 400 Oe, respectively. Magnetic relaxations were studied by means of dc and ac methods and analyzed using the Argand diagrams. Except for the thermally activated single chain and domain wall relaxations observed for both compounds, temperature-independent slow relaxations were observed for [Co(NCS)2(bpa)]n.
The donor-free mesityllithium was prepared from the reaction of MesBr with n-BuLi in diethyl ether at -78 degrees C. The solid-state structure of unsupported mesityllithium consists of C(2)Li(2)-rings composed of two LiMes units, which interact with adjacent dimers [LiMes](2), forming a polymeric infinite chain along the crystallographic c-axis (monoclinic space group, P2(1)/n). The structure of donor-free mesityllithium reveals short contacts between the C atoms of the mesityl rings and the lithium atoms of neighbouring [LiMes](2) units. The structure determination of LiMes was performed by X-ray powder diffraction. In addition we have investigated the reaction of LiMes with Me(3)SnCl and P(4) for our understanding of the reactivity of donor-free mesityllithium. The heterogeneous reaction of donor-free mesityllithium with Me(3)SnCl produces conveniently the stannylated mesitylene Me(3)SnMes (triclinic, space group P1). White phosphorus reacts with three equivalents of unsupported mesityllithium in benzene to give Li(3)P(4)Mes(3). In this context it should be noted that a tetraphosphide with an identical LiP-core as in Li(3)P(4)Mes(3) had been formed in the 1:3 reaction of P(4) with the silanide Li[SitBu(3)]. The tetraphosphide Li(3)P(4)Mes(3) was analyzed using X-ray crystallography (monoclinic, space group C2/c).
The reactivity of the neuroleptic drug adamantylamine toward aliphatic carboxylic acids, sulfone derivatives, and aromatic amino acids was screened for the first time using simple mechanochemical methods. Seven new molecular salt structures were reported exhibiting improved physicochemical properties. To carefully characterize these compounds, multiple complementary techniques were combined: single crystal and powder X-ray diffraction, 13 C/ 15 N solid-state NMR, and Fourier transform infrared-attenuated total reflectance spectroscopies, employed to solve cocrystal/salt ambiguities. In all molecular salts, the crystal packing is supported on a common synthon, a N−H + (ADA) •••O − (coformer) charge assisted hydrogen bond. Different supramolecular arrangements were obtained induced by the size of the counterions as well as their complementary functional groups. Two salts, with glutaric and methanesulfonic acids, presented higher solubility than the commercially available pharmaceutical product.
No crystal structure at ambient pressure is known for tetramethylsilane, Si(CH(3))(4), which is used as a standard in NMR spectroscopy. Possible crystal structures were predicted by global lattice-energy minimizations using force-field methods. The lowest-energy structure corresponds to the high-pressure room-temperature phase (Pa3, Z = 8). Low-temperature crystallization at 100 K resulted in a single crystal, and its crystal structure has been determined. The structure corresponds to the predicted structure with the second lowest energy rank. In X-ray powder analyses this is the only observed phase between 80 and 159 K. For tetramethylgermane, Ge(CH(3))(4), no experimental crystal structure is known. Global lattice-energy minimizations resulted in 47 possible crystal structures within an energy range of 5 kJ mol(-1). The lowest-energy structure was found in Pa3, Z = 8.
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