scholarly journals Metallkomplexe mit 1,4,7-Trithiacyclononan: Kristallstrukturen von [CdI2 · C6H12S3]2 und [Hg(C6H12S3)2](HgI3)2 / Metal Complexes with 1,4,7-Trithiacyclononane: Crystal Structures of [CdI2 · C6H12S3]2 and [Hg(C6H12S3)2](HgI3)2

1993 ◽  
Vol 48 (7) ◽  
pp. 969-972 ◽  
Author(s):  
Joachim Pickardt ◽  
Jing Shen

Crystals of the complexes [CdI2 · C6H12S3]2 (1) and [Hg(C6H12S3)2](HgI3)2 (2) were obtained by diffusion of 1,4,7-trithiacyclononane (9 S 3) in ethanol into aqueous solutions of cadmium iodide and mercuric iodide/potassium iodide, resp. Both compounds crystallize monoclinically,1: space group P21/n, Z = 4, a = 1207.1(5), b = 909.9(2), c = 1240.3(7) pm, β = 92.59(9)°; 2: P21/c, Z = 2, a = 804.7(6), b = 934.0(6), c = 2167.9(4) pm, β = 94.34(7)°. 1 is dimeric, consisting of two [CdI2 · 9S3] units, connected via iodine bridges. Crystals of 2 contain sandwich-like cations [Hg(9S3)2]2+ and [HgI3]- anions, forming chains via Hg ··· S and Hg ··· I bridges.

1981 ◽  
Vol 36 (10) ◽  
pp. 1225-1227 ◽  
Author(s):  
Joachim Pickardt

Abstract The reaction of aqueous solutions of cadmium iodide and hexamethylenetetramine yields crystals of an adduct 3CdI2 • 2CeH12N4 • 4H2O. The crystals are monoclinic, space group P 21/n, Z = 2, a = 811.5(2), b = 1049.2(4), c = 1849.5(6) pm, β = 97.73(2)°. The adduct is polymeric and may be regarded as built up from groups of two tetrahedrally and one octahedrally coordinated Cd(II) ions in which the tetrahedra and the octahedron are sharing common iodine atoms at the corners; neighbourirg Cd3 units are interlinked by hexamethylenetetramine molecules.


1989 ◽  
Vol 44 (5) ◽  
pp. 519-525 ◽  
Author(s):  
Hans-Jürgen Meyer ◽  
Joachim Pickardt

By reaction of methanolic solutions of hexamethylenetetramine with aqueous solutions of hexacyanoferrates(III) of strontium and barium resp., crystals of the compounds were obtained. Sr3[Fe(CN)6]2 · 3 C6H12N4 · 18 H2O, tetragonal, space group P42/nmc, Z = 4, a = 1931.8(4), c = 1579.9(4) pm, 1358 reflections. R = 0.066. Ba3[Fe(CN)6]2 · 2 C6H12N4 · 11 Η2Ο. monoclinic. space group P21/n, Ζ = 2, a = 1148.0(4), b = 1369.7(4), c = 1584.5(4) pm, γ = 95.79(3)°, 2583 reflections, R = 0.057. The crystal structures of these adducts are compared with those of other hexamethylenetetramine adducts of alkaline and alkaline earth metal hexacyanoferrates of the general formula M,[Fe(CN)6]y · zC6H12N4 · vH2O recently investigated by us. A structural model for the adducts is presented.


1985 ◽  
Vol 38 (9) ◽  
pp. 1381 ◽  
Author(s):  
CHL Kennard ◽  
EJ O'Reilly ◽  
G Smith ◽  
TCW Mak

The crystal structures of 2-formylphenoxyacetic acid ( ofpaH ), tetraaquabis (2-formylphenoxyacetato)-cobalt(II) (1) and tetraaquabis (2- formylphenoxyacetato )zinc(II) (2) have been determined by X-ray diffraction and refined to residuals R 0.039, 0.058 and 0.045 for 1197, 1178 and 1230 observed reflections respectively. 2-Formylphenoxyacetic acid crystallizes in a monoclinic cell, space group P21/n with a 8.066(2), b 7.375(1), c 14.206(2) Ǻ, β 98.12(1)° and Z 4. The planar molecules form unusual hydrogen-bonded chain polymers (O…O 2.694(3)Ǻ] linked through the carboxyl groups. The complexes (1) and (2) are isomorphous, the comparative cells being a 5.036(1), b 13.463(3), c 15.083(4) Ǻ, β 96.88(2)° for (1), and a 5.044(1), b 13.481(3), c 15.055(4) Ǻ, β 96.95(2)° for (2), with Z 2 and space group P21. The complexes have four waters and two trans-related carboxyl oxygens [mean M-O distances 2.129(5) and 2.117(3) Ǻ respectively] completing almost regular octahedral stereochemistries . The nickel(II) complex [Ni( ofpa )(H2O)4] is probably not isostructural with (1) and (2), and the copper(II) complex is also different, with formula [Cu( ofpa )2(H2O)2].


1996 ◽  
Vol 51 (10) ◽  
pp. 1469-1472 ◽  
Author(s):  
Joachim Pickardt ◽  
Britta Kühn

Crystals of |Zn(cnge)2(SCN)2]-2H2O (1) were obtained by evaporation of an aqueous solution of Z n(SO4)·7H2O , KSCN, and cyanoguanidine. Crystals of Zn(eoge)Br2 (2) were obtained by reaction of ZnBr2 and cyanoguanidine in ethanol/water. Both compounds are monoclinic, space group C2/c, 1: Z = 4, a = 1919.6(7), b = 467.3(2), c = 1838.5(6) pm, β = 112.99(3)°, 2: Z = 8, a = 1799.5(6), b = 878.7(2), c = 1367.2(5) pm, β = 101.52(3)°. In 1 each Zn is bonded to two cyanoguanidine molecules and via the N atoms to two NCS groups. Intermolecular hydrogen bonds lead to chains along the a-axis, and these chains are again connected via hydrogen bonds to the two crystal water molecules. In the course of the formation of 2, the cyanoguanidine reacted with the ethanol to form 1-ethoxyiminomethylguanidine. This ligand forms chelate rings with the Zn atoms, which are tetrahedrally coordinated by the two imino N atoms of the ligand and by two bromine atoms.


1985 ◽  
Vol 40 (12) ◽  
pp. 1756-1758 ◽  
Author(s):  
Joachim Pickardt ◽  
Pamela Droas

Abstract By reaction of zinc chloride and zinc bromide with hexamethylenetetramine in water/methanol crystals of the adducts ZnCl2 • C6H12N4 and ZnBr2 • C6H12N4, resp. were obtained. The compounds are isotypic, they crystallize in the orthorhombic space group P21am (non-standard setting of space group Pmc21, No. 26), Z = 2. The lattice parameters of the zinc chloride adduct are a = 1168.0(4), b = 685.7(4), and c = 601.1(4) pm, of the zinc bromide adduct a - 1188.9(6), b = 721.5(5), and c = 602.3(4) pm. The adducts are polymeric, they form parallel chains in the crystal. The zinc atoms are bonded to two halogen atoms and, via nitrogen atoms, to two hexamethylenetetramine molecules, which act as bidentate ligands. The coordination of the zinc atoms is approximately tetrahedral


1993 ◽  
Vol 48 (7) ◽  
pp. 991-999 ◽  
Author(s):  
Mathias O. Senge ◽  
Kevin M. Smith

The crystal structures of two zinc(II) 5,15-dioxo-porphyrins (porphodimethenes) have been determined to investigate the coordination chemistry of porphyrins with interrupted conjugation system. Both compounds have a five-coordinated zinc center with pyridine as axial ligand and show overall structural parameters very similar to porphyrins. The oxidized meso-positions are, however, easily identified by longer Cm–Ca bond lengths and smaller Ca–Cm–Ca angles. The macrocycles exhibit a small degree of conformational distortion, and the etioporphyrin I derivative shows evidence for π-stacking in the crystal. Crystal data: 1 – C41H47N5O2Zn. Triclinic, a = 10.052(3) Å, b = 14.139(4) Å, c = 14.635(5) Å, α = 105.17(2)°, β = 108.62(3)°, γ = 106.29(2)°, V = 1745.3(9) Å3, CuKα radiation, λ = 1.54178 Å, space group P1̅, Z = 2. R = 0.089. 2 – C37H39N5O2Zn. Triclinic, a = 12.122(3) Å, b = 12.383(3) Å, c = 12.759(4) Å, α = 61.77(2)°, β = 72.19(2)°, γ = 70.32(2)°, V = 1563.8(8) Å3, CuKa radiation, λ = 1.54178 A, space group PĪ, Z = 2, R = 0.076.


1977 ◽  
Vol 32 (11) ◽  
pp. 1239-1243 ◽  
Author(s):  
Gerhard Thiele ◽  
Peter Hilfrich

By mixing aqueous solutions of Hg(CH3COO)2 and KOCN the white precipitate K2Hg3(NCO)8 is formed. When recrystallised from CH3OH colorless crystals of the compound KHg(NCO)3 are obtained. The crystal structure analysis (space group Pnma; α = 1015.2(6) pm, b = 399.3(3) pm, c = 1772.9(9) pm) shows a distorted KCdCl3 arrangement with isolated Hg(NCO)2 molecules, K+ and NCO- ions. The vibrational spectra in the range of 250-3000 cm-1 are discussed. The rubidium compound is isotypous (a = 1019.0(6) pm, b = 411.6(4) pm, c = 1820.5(8) pm).


1989 ◽  
Vol 44 (4) ◽  
pp. 383-388 ◽  
Author(s):  
Martin Hilbers ◽  
Manfred Leimkühler ◽  
Rainer Mattes

From aqueous HF solutions the following fluorooxo complexes have been crystallized and characterized: AI(NMe4)2[V3O3F12] (1), AI = Na. K; K2(NMe4)[V2O2F9]·H2O (2); Cs(NMe4)[V2O2F8(H2O)] (3) and NMe4[VOF4] (4). The structures of 1 and 3 have been determined.Crystal data: 1c, hexagonal, space group P63/m . a = 1695.0(9), c = 1248.1(5) pm. Z = 6: 1803 reflections. R = 0.045. 3, orthorhombic. space group Pnma, a = 2152.8(7), b = 751.5(2), c = 850.7(2) pm, Z = 4; 1379 reflections, R = 0.030. 1 contains a trimeric, cyclic anion with asymmetrically bonded μ-fluoroligands and terminal V = O groups in the same plane; the anion of 3 is a fluorobridged dimer with unequally coordinated vanadium atoms with terminal V = O groups. The preparation of these com pounds establishes the presence of VOF4(H2O)- species in aqueous solutions.


1996 ◽  
Vol 51 (12) ◽  
pp. 1701-1706 ◽  
Author(s):  
Joachim Pickardt ◽  
Britta Kühn

Crystals of [Cd(cnge)2F2]·3H2O (1), Cd(cnge)2Br2 (2) and Hg(cnge)Cl2 (3) (cnge = cyanoguanidine) were obtained by crystallisation from solutions of CdF2, CdBr2 or HgCl2 and cyanoguanidine in water/ethanol or methanol. 1 crystallizes monoclinically, space group C2, Z = 2,a = 1629.2(4), b = 1056.6(4), c = 353.9( 1) pm, β = 101.05(2)°; 2 is monoclinic, space group P21/n, Z = 2, a = 391.9(1), b = 850.7(2), c = 1722.1(4) pm, β = 94.06(2)°, 3 is triclinic, space group P1, Z = 1, a = 686.7( 1), b = 693.0(5), c = 387.2(4) pm, α = 94.45(5)°, β = 95.05(4)°, γ = 78.58(5)°. In 1 and 2 each Cd atom is bonded to four halogen atoms to form polymeric (CdF2)n and (CdBr2)n chains, resp., and to two cyanoguanidine molecules. In 3 each Hg atom is bonded to four chlorine atoms also forming (HgCl2)n chains, which are connected via cyanoguanidine molecules acting as a bidentate bridging ligands to form a network.


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