Bis (2-pyrimidinyl) disulfide dihydrate: a redetermination

The crystal structure of bis(2-pyrimidinyl) disul®de dihydrate, C8H6N4S22H2O, has been redetermined using CCD diffractometer data. This has allowed for a more precise location of the water H atoms and shows the water molecules forming unusual spiral hydrogen-bonded aqua columns, as well as giving inter-column crosslinks through the pyrimidine N-atom acceptors of the disul®de molecules. The structural chemistry of aromatic disul®des has also been reviewed

Unusual hydrate stabilization in the two-dimensional layered structure of quinacrinium bis(2-carboxy-4,5-dichlorobenzoate) tetrahydrate, a proton-transfer compound of the drug quinacrine

The crystal structure of the hydrated proton-transfer compound of the drug quinacrine [rac-N'-(6-chloro-2-methoxyacridin-9-yl)-N,N-diethylpentane-1,4-diamine] with 4,5-dichlorophthalic acid, C23H32ClN3O2+ . 2(C8H3Cl2O4-).4H2O (I), has been determined at 200 K. The four labile water molecules of solvation form discrete ...O--H...O--H... hydrogen-bonded chains parallel to the quinacrine side chain, the two N--H groups of which act as hydrogen-bond donors for two of the water acceptor molecules. The other water molecules, as well as the acridinium H atom, also form hydrogen bonds with the two anion species and extend the structure into two-dimensional sheets. Between these sheets there are also weak cation--anion and anion--anion pi-pi aromatic ring interactions. This structure represents only the third example of a simple quinacrine derivative for which structural data are available but differs from the other two in that it is unstable in the X-ray beam due to efflorescence, probably associated with the destruction of the unusual four-membered water chain structures

Hydrogen bonding in proton-transfer compounds of 5-sulfosalicylic acid with a series of aliphatic nitrogen Lewis bases

The crystal structures of the proton-transfer compounds of 5-sulfosalicylic acid (3-carboxy-4-hydroxybenzenesulfonic acid) with the aliphatic nitrogen Lewis bases, hydroxylamine, triethylamine, pyrrolidine, morpholine, N-methylmorpholine and piperazine, viz. hydroxyammonium 3-carboxy-4-hydroxybenzenesulfonate (1), triethylaminium 3-carboxy-4-hydroxybenzenesulfonate (2), pyrrolidinium 3-carboxy-4-hydroxybenzenesulfonate monohydrate (3), morpholinium 3-carboxy-4-hydroxybenzenesulfonate monohydrate (4), N-methylmorpholinium 3-carboxy-4-hydroxybenzenesulfonate monohydrate (5) and piperazine-1,4-diium bis(3-carboxy-4-hydroxybenzenesulfonate) hexahydrate (6) have been determined and their comparative structural features and hydrogen-bonding patterns described. Crystals of 4 are triclinic, space group P-1 while the remainder are monoclinic with space group either P21/c (1 - 3) or P21/n (5, 6). Unit cell dimensions and contents are: for 1, a = 5.0156(3), b = 10.5738(6), c = 18.4785(9) Å, β = 96.412(5)o, Z = 4; for 2, a = 8.4998(4), b = 12.3832(6), c = 15.4875(9) Å, β = 102.411(5)o, Z = 4; for 3, a = 6.8755(2), b = 15.5217(4), c = 12.8335(3) Å, β = 92.074(2)o, Z = 4; for 4, a = 6.8397(2), b = 12.9756(5), c = 15.8216(6) Å, α = 90.833(3), β = 95.949(3), γ = 92.505(3)o, Z = 4; for 5, a = 7.0529(3), b = 13.8487(7), c = 15.6448(6) Å, β = 90.190(6)o, Z = 4; for 6, a = 7.0561(2), b = 15.9311(4), c = 12.2102(3) Å, β = 100.858(3)o, Z = 2. The hydrogen bonding generates structures which are either two-dimensional (2 and 5) or three-dimensional (1, 3, 4 and 6). Compound 6 represents the third reported structure of a salt of 5-sulfosalicylic acid having a dicationic piperazine species. \u

The Preparation and Crystal Structure of Ammonium Bismuth (III) Thiosalicylate Dihydrate

The bismuth(III) complex of thiosalicylic acid (2-mercaptobenzoic acid; H2L), ammonium tris(2-mercaptobenzoato-O,S) bismuth(III) dihydrate, {(NH4)3[Bi(L)3]粠H2O}, has been prepared and its crystal structure determined. The distorted octahedral tris-bidentate complex unit has pseudo-C3 symmetry with the facially related thiolate sulfur donors providing a regular facial cap to the octahedron (Bi-S 2.595, 2.596, 2.596(5) ũ with the Bi-O(carboxylate) distances less regular (2.715, 2.741, 2.785(15) ũ. The network polymeric structure is stabilized by hydrogen-bonding associations through both the ammonium counter ions and the lattice water molecules.No Full Tex

Metal Complexes with N-(Phosphonomethyl)glycine (Glyphosate): the Preparation and Characterization of the Group 2 Metal Complexes with Glyphosate and the Crystal Structure of Barium Glyphosate Dihydrate

A series of the Group 2 metal complexes with the herbicide N-(phosphonomethyl)glycine (glyphosate, H 3L) with general formula [M(HL)·2H 2O] has been prepared and characterized by using infrared spectroscopy and in the case of the Ba analogue, by single-

Univalent metal ion α-hydroxy and interactions: Part 9. Preparation and crystal structures of lithium hydrogen (+)-tartrate monohydrate, potassium (+)-tartrate hemihydride and thallium(I) (+)-tartrate

The univalent metal ion compounds of (+)-tartaric acid, lithium hydrogen (+)-tartrate monohydrate (1), potassium (+)-tartrate hemihydrate (2) and thallium (+)-tartrate (3) have been prepared and their structures determined by X-ray diffraction methods. All form network polymer structures similar to the other group one metal tartrates. However, (1) is based on a dimeric repeating unit, with two independent but different five-coordinate square pyramidal lithium centres, [LiO, 1.971-2.322(8) Å]. Although both centres involve (+)-tartrate residues in α-hydroxycarboxyl bis-coordinate interactions, one centre has two, the other has one and is also coordinated to both waters (one bridging). The protonated carboxylic acid groups are uncoordinated but hydrogen bonded in both inter- and intra-dimer associations. Potassium (+)-tartrate hemihydrate (2) has two independent and different distorted octahedral potassium centres. About the first, there are five oxygens from (+)-tartrate residues and one from a water which bridges to another symmetry generated potassium. The second potassium has six bonds to (+)-tartrate oxygens, including a β-hydroxycarboxyl chelate ring, with a KO range of 2.711(2)-2.988(3) Å. An unusual feature is a carboxyl oxygen giving a three-centre bonding system to three separate potassium ions. The polymeric structure of thallium(I) (+)-tartrate (3) is based upon two different five-coordinate thallium centres [TlO range, 2.59(3)-2.96(2) Å]. About one, bonds are to three oxygens from one (+)-tartrate residue (one carboxyl, two hydroxyl), and two from a symmetric bidentate-carboxylato-(O,O′) group of a bridging (+)-tartrate. The bonded hydroxyl also bridges to the second Tl [Tl⋯Tl, 3.519(2) Å]. Completing the bonding to this second Tl are oxygens from four different tartrate residues. Crystallographic and analytical data are also provided for silver(I) (+)-tartrate (4)

The preparation and crystal structure of a polymeric (1 : 1)-silver nitrate-urea complex, [(AgNO3)2(CH4N2O)2]n

The complex (1 : 1) silver nitrate-urea adduct [AgNO) (urea)] has been prepared and characterized by X-ray diffraction. The structure contains two independent silver centres which are different, the first being three-coordinate distorted trigonal planar, with two bonds to separate nitrates [AgO, 2.393, 2.486(7) Å], and one to a urea oxygen [AgO, 2.333(7) Å]. The second silver is distorted tetrahedral, also with two bonds to separate nitrates [AgO, 2.464(7), 2.467(8) Å], one to a urea oxygen [AgO, 2.322(6) Å] and one to a urea nitrogen [AgN, 2.405(9) Å]. The nitrate groups and one of the urea molecules form bridges between the silver centres, giving a polymeric layer structure

Crystallographic evidence for the presence of both (2-) and (3-) citrate species in a mixed-metal complex, [CuSb(C6H6O72-)(C6H5O7 3-)(H2O)2]·2.5H2O

The mixed-metal (Cu/Sb) complex with citric acid, {[CuSb(CHO)(CH O)(HO)]·2.5HO}, has been synthesized and its structure determined by X-ray diffraction. Each antimony is bonded to four oxygens from two α-hydroxycarboxyl moieties of two citrate residues [SbO(hydroxyl): 1.974, 2.009(5) Å; SbO(carboxyl): 2.177, 2.230(6) Å]. The second carboxyl oxygens of these groups are bonded to the axial sites of trigonal bipyramidal copper centres [CuO, 1.924, 1.928(7) Å], forming a linear polymer chain. In the equatorial sites of the trigonal bipyramid are two waters [CuO, 2.088, 2.096(6) Å] and the carboxylato oxygen of a citrato(3-) residue of an adjacent polymer chain [CuO, 2.015(5) Å]. The result is a duplex chain structure involving both citrato(2 -) and citrato(3 -) species