Dalius S. Sagatys
Queensland University of Technology
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Polyhedron | 1993
Dalius S. Sagatys; Graham Smith; Raymond C. Bott; Daniel E. Lynch; Colin H. L. Kennard
Abstract The polymeric silver(I) citrate complex {NH4[Ag2(C6H5O7)(H2O)]}n has been synthesized and its structure determined by X-ray diffraction methods and refined to R = 0.046 for 2520 observed reflections. This compound represents the first reported complexes of a silver(I) citrate. In the structural repeating unit there are two independent but different carboxylato(O,O′) bridged silver dimers [AgAg, 2.845, 2.846(1) A] linked into infinite linear chains by the terminal carboxyl groups of the citrato(3 −) ligands. With one dimer, the AgO (axial) bonds are to oxygens from the sub-terminal carboxylate groups of two independent silver citrate chains. The second silver dimer also forms links with adjacent chains via axial AgO(carboxylate) bonds, while in the remaining axial sites are water molecules. The mean AgO distance is 2.377(4) A. The result is a novel convoluted anionic chain sheet structure.
Polyhedron | 1987
Thomas C. W. Mak; Colin H. L. Kennard; Graham Smith; Eric J. O'Reilly; Dalius S. Sagatys; Janelle C. Fulwood
Abstract The crystal structures of three copper(II) complexes with phenoxyisobutyric acid (PIBAH) and p-chlorophenoxyisobutyric acid (PCIBAH) have been determined by X-ray diffraction. Tetra-μ-[2-methyl-2-(4-chlorophenoxy)-propanoato-O,O′]-bis[2-amino-pyrimidine)copper(II)], [Cu2(PCIBA)4(2-aminopyrimidine)2]2 (1) is a centrosymmetric tetracar☐ylate bridged dimer [Cu⋯Cu, 2.689(2)A] with the nitrogens of the 2-aminopyrimidine molecules occupying the axial positions [Cu N, 2.198(7)A]. Tetraaquacopper(II) tri-μ-[2-methyl-2-phenoxypropanoato-O,O′]-bis[(2-methyl-2-phenoxypropanoato(copper(II)], [Cu(H2O)4]2+] {[Cu2(PIBA)5]−}2, (2), is a disordered precursor of the stable structure (3), [Cu(H2O)5]2+ {[Cu2(PIBA)5]−·4H2O, consisting of centrosymmetric square planar [Cu(H2O)4]2+ cations and tris(car☐ylate)-bridged dimer anions [Cu⋯Cu, 2.85(1)A] (2). The fourth position of each square planar dimer ‘end’ is occupied by a car☐ylate oxygen of a PIBA molecule which also provides the ether oxygen capping each axial dimer site [Cu O, 2.15(4), 2.19(5)A]. This completes a five-membered chelate ring. A symmetrical array of eight hydrogen bonds link the four waters of the [Cu(H2O)4]2+ cation to the car☐yl oxygens of both the capping PIBA ligands of the two dimeric anions. Structure (3) has essentially identical [Cu2(PIBA)5]− dimer anions [Cu⋯Cu, 2.929(1)A] and hydrogen-bonding interactions with the tetraaquacopper(II) cations. However, water molecules partially occupy the octahedral sites of these cations [Cu O, 2.46(1)A], as well as a number of lattice sites in the crystal.
Polyhedron | 1992
Dalius S. Sagatys; Raymond C. Bott; Graham Smith; Karl A. Byriel; Colin H. L. Kennard
Abstract The complex (1 : 1) silver nitrate-urea adduct [AgNO3) 2(urea)2]n 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) A], and one to a urea oxygen [AgO, 2.333(7) A]. The second silver is distorted tetrahedral, also with two bonds to separate nitrates [AgO, 2.464(7), 2.467(8) A], one to a urea oxygen [AgO, 2.322(6) A] and one to a urea nitrogen [AgN, 2.405(9) A]. The nitrate groups and one of the urea molecules form bridges between the silver centres, giving a polymeric layer structure.
Australian Journal of Chemistry | 2001
Raymond C. Bott; Graham Smith; Dalius S. Sagatys; Daniel E. Lynch; Colin H. L. Kennard
The structures of sodium (+)-tartrato arsenate(III),[Na8As10(C4H2O6)8(C4H3O6)2(H2O)19]n(1), silver (+)-tartrato arsenate(III),[Ag9As10(C4H2O6)9(C4H3O6)(H4As2O5)(H2O)10](2) and rubidium citrato antimonate(III)[Rb2Sb4(C6H6O7)6(C6H7O7)2(H2O)2](3) have been determined by X-ray methods and refined to residuals of 0.085(1), 0.072 (2) and 0.065 (3) for 5018, 4487 and 8207 observed reflections,respectively. The (+)-tartrato complexes (1) and (2) are similar instructure to the two known isomorphous silver(I) (+)-tartratoarsenate(III) complexes in that independent anionic[As2(tartrate)2] dimericcages are linked to the sodium or silver counter-cations, respectively,through free carboxyl oxygen atoms. However, the structures are made morecomplex by the presence of labile water molecules in the lattice, resulting insome disorder. Furthermore, charge balance in both (1) and (2) requires thepresence of two and one tri-negative tartrato units, respectively, among theten independent tartrate units in each structure, an unusual feature for Asand Sb complexes with this ligand species. Bond distances within the fivearsenic(III)-(+)-tartrate dimers in each structure are: As–O(hydroxy), 1.75(2)–1.84(2) A (1); 1.75(3)–1.83(2) A(2) and As–O (carboxy), 1.94(2)–2.13(3) A (1);1.95(2)–2.14(2) A (2). In addition, the structure of (2) has twoshort Ag–As bonds [2.500, 2.524(3) A] in the terminalsites of two of the f ive independent dimers, as well as an additionalAg–As bond [2.613(4) A] to an unusual dimeric arseniousacid residue(H4As2O5),part of an As2AgO3 hetero-ringforming the polymeric network structure. The antimony(III) citrate complex (3)is isomorphous and isostructural with the previously reported potassiumanalogue which involves mixed-valence citrato ligands in conventionalbis-chelate four-coordination about the antimony centres, linked by bothseven- and eight-coordinate rubidium ions [Rb–O,2.743(10)–3.102(9) A]. The arsenic and antimony atoms in allcompounds have typical distorted pseudo-trigonal bipyramidal stereochemistry.
Australian Journal of Chemistry | 2000
Dalius S. Sagatys; Cathrine Dahlgren; Graham Smith; Raymond C. Bott; Anthony C. Willis
A series of the Group 2 metal complexes with the herbicide N-(phosphonomethyl)glycine (glyphosate, H3L) with general formula [M(HL)·2H2O] has been prepared and characterized by using infrared spectroscopy and in the case of the Ba analogue, by single-crystal X-ray diffraction. Crystals are monoclinic, space group P21/n, with four molecules in a cell having dimensionsa 9.516(3), b 7.609(2), c 12.826(5) A, b 103.00(3)˚, and the structure was refined to a residual R 0.057 for 1655 observed reflections. The polymer structure is based on a centrosymmetric dimeric {[Ba(HL)(H2O)2]2} repeating unit with each irregular BaO8 centre bridged by bisglyphosate [O(phosphonate), O(carboxylate)] ligands, with the carboxylate groups also bidentate and bridging. The two water molecules, together with further interdimer bridges, complete the coordination about Ba [Ba–O range: 2.656–2.947(8) A; mean, 2.774 A]. Infrared spectroscopy has been used to show that the Ba and Sr complexes are similar but both are significantly different from the previously reported calcium analogue with the same general formula {[Ca(HL)(H2O)2]2}n, while all are significantly different from the magnesium analogue which has the probable formula [Mg4(3-OH)4(H2O)12] [Mg2(L)2(-HL)(H2O)2].
Polyhedron | 1994
Raymond C. Bott; Dalius S. Sagatys; Graham Smith; Karl A. Byriel; Colin H. L. Kennard
Abstract 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) A]. 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) A. 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) A]. 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) A]. 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).
Polyhedron | 1992
Graham Smith; Dalius S. Sagatys; Raymond C. Bott; Daniel E. Lynch; Colin H. L. Kennard
Abstract The mixed-metal (CuII/SbIII) complex with citric acid, {[CuSb(C6H6O7)(C6H5 O7)(H2O)2]·2.5H2O}n, 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) A; SbO(carboxyl): 2.177, 2.230(6) A]. The second carboxyl oxygens of these groups are bonded to the axial sites of trigonal bipyramidal copper centres [CuO, 1.924, 1.928(7) A], forming a linear polymer chain. In the equatorial sites of the trigonal bipyramid are two waters [CuO, 2.088, 2.096(6) A] and the carboxylato oxygen of a citrato(3−) residue of an adjacent polymer chain [CuO, 2.015(5) A]. The result is a duplex chain structure involving both citrato(2 −) and citrato(3 −) species.
Journal of The Chemical Society-dalton Transactions | 1991
David W. Hartley; Graham Smith; Dalius S. Sagatys; Colin H. L. Kennard
The antimony(III)–silver(I) and –sodium(I) complexes with citric acid (C6H8O7), [Sb2Ag2(C6H6O7)4]1 and [SbNa(C6H6O7)2(H2O)2]·H2O 2, have been prepared and their crystal structures determined by X-ray diffraction and refined to residuals of R= 0.023 and 0.017 for 2403 and 2969 observed reflections respectively. Crystals are monoclinic, space group P21/n, and P21/a Complex 1 has two dimers in a cell of dimensions a= 6.557(4), b= 12.149(2), c= 20.50(1)A and β= 98.12(3)°, while there are four monomers of 2 in a cell with a= 14.470(5), b= 7.193(3), c= 18.747(6)A and β= 92.22(2)°. In each structure antimony is bonded to two oxygens of two crystallographically independent citrate(2–) residues in classic pseudo-trigonal-bipyramidal antimony(III) four-co-ordination [Sb–O 2.007(2)–2.218(2), 1; 1.988(1)–2.164(1)A, 2]. These oxygens are from the α-hydroxycarboxylate groups giving five-membered chelate rings. In 1 each antimony centre is in turn linked through one of these carboxylate groups to two silver(I) ions in an asymmetric bis(carboxylato-O,O′) bridge [Ag–O 2.314(2) and 2.661(2)A]. Hydroxyl groups complete the angular three-co-ordination about each silver [Ag–O 2.323(2)A], giving a centrosymmetric cyclic dimer structure. In contrast, complex 2 is monomeric with the sodium and two co-ordinated waters [Na–Ow 2.404(2) and 2.512(2)A] forming a tris(oxo)-bridged complex unit (two oxygens from the α-hydroxycarboxy groups), with a Na–O range of 2.413(2)–2.562(2)A[Na ⋯ Sb 3.665(1)A].
Polyhedron | 1993
Graham Smith; Dalius S. Sagatys; Raymond C. Bott; Daniel E. Lynch; Colin H. L. Kennard
Abstract Potassium antimony(III) citrate, {[K2Sb4(citrate)8(H2O)2} (1), and lithium antimony(III) citrate, {[LiSb(citrate)2(H2O)]·2H2O} (2), have been prepared and their structures determined by X-ray diffraction. With 1 each of the two independent centrosymmetric tetramers in the repeating unit of the complex comprises four independent antimony ions and eight citrate residues interlinked by two potassium centres [K—O range 2.62–3.06(1) A]. The difference between the two tetramers is that potassium is seven-coordinate in one and eight-coordinate in the other. The water molecules are coordinated to the potassium ions. Each antimony forms the usual distorted pseudo-trigonal bipyramidal four-coordinate complex through the α-hydroxy carboxylate oxygens of two citrate residues. A feature of the structure is the presence of three differently charged citrate species (1-, 2-, 3-), giving the formula {K2[Sb(C6H6O7)2]2[Sb(C6J7O7)(C6H5O7)]2(H2O)2}. The coordination about antimony in 2 is similar, but the lithium links the two citrate residues together via carboxyl and a hydroxyl oxygen from one ligand and a carboxyl oxygen from the second. A water completes the tetrahedral coordination sphere [mean LiO, 1.942(5) A]. Except for the four-coordination about lithium, the complex is similar to the analogous sodium complex {[NaSb(citrate)2(H2O)2]·H2O}.
Australian Journal of Chemistry | 2003
Dalius S. Sagatys; Graham Smith; Raymond C. Bott; Peter Conrad Healy
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]·2 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) A) with the Bi–O(carboxylate) distances less regular (2.715, 2.741, 2.785(15) A). The network polymeric structure is stabilized by hydrogen-bonding associations through both the ammonium counter ions and the lattice water molecules.