Functionalized 1,1-Ethene Dithiolates as Ligands, V [1]. Synthesis and Crystal Structure of Palladium(II) and Platinum(II) Complexes with Dithioylidene Barbituric Acid Ligands. Molecular Structure of a 2,6-Diaminopyridine-Platinum(II) Barbiturate Complex

1998 ◽  
Vol 53 (10) ◽  
pp. 1135-1143 ◽  
Author(s):  
Wolfgang Weigand ◽  
Veronika Plener ◽  
Heinrich Nöth ◽  
Ingo Krossing ◽  
Jörg Knizek ◽  
...  

AbstractThe 1,1-ethene dithiolato ligands (dithioylidene barbituric acids) 2a-f react with palladium(II) and platinum(II) compounds L2MCI2 [M = Pd, Pt; L = PEt3, PBu3, PPh3, 1/2 dppe, 1/2 (-)-DIOP, 1/2 2,9-dimethyl phenanthroline] to give the 1,1-ethene dithiolato metal complexes . Compound 4a forms a 1:1 adduct (8) with 2,6-diaminopyridine. The compounds were characterised on the basis of their IR and NMR (1H, 13C, 31P) spectra. Complexes 4a, 4c, and 5a were further studied by X-ray structural analysis. The barbituric unit in 4a undergoes self-assembly through multiple hydrogen-bonding with complementary 2 ,6-diaminopyridine yielding the supramolecular complex 8

2013 ◽  
Vol 785-786 ◽  
pp. 424-427
Author(s):  
Hai Xing Liu ◽  
Qing Hua Zhang ◽  
Zhang Xue Yu ◽  
Quan Hua Fan ◽  
Ting Ting Huang ◽  
...  

The Y complex C4H10O10Y has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Y atom is coordinated by nine O atoms. The molecular structure stabilized by the O-H…O hydrogen-bonding interactions.


1998 ◽  
Vol 53 (10) ◽  
pp. 1144-1148 ◽  
Author(s):  
Frank Wendland ◽  
Christian Näther ◽  
Michael Schur ◽  
Wolfgang Bensch

AbstractThe title compound has been synthesized under solvothermal conditions by the reaction of elemental chromium, antimony and selenium in a solution of 40% 1,2-ethanediamine (en) in methanol. The crystal structure consists of tetrahedral SbSe43- anions which are connected by monoprotonated 1,2-ethanediamine (enH+) cations via N-H--Se hydrogen bonding. The enH+ cations are joined via strong N-H -N hydrogen bonds between the ammonium hydrogen and the amino nitrogen atom forming four distinct chains, each built up of three crystallographically independent enH+ cations. Two of these chains are running parallel to [100], the other two are parallel to [010]. Based on this arrangement different centrosymmetric or non-centrosymmetric hydrogen bonding patterns are possible, but only in one chain the sequence of NH2 and NH3+ groups was determined by X-ray diffraction


2004 ◽  
Vol 82 (5) ◽  
pp. 616-621 ◽  
Author(s):  
Xian-Ming Zhang ◽  
Chan-Juan Bai ◽  
Yan-Li Zhang ◽  
Hai-Shun Wu

A novel organic-templated zincophosphate, namely (C6H16N2)[Zn(HPO4)2], was hydrothermally synthesized and X-ray single-crystal structural analysis reveals that the anions [Zn(HPO4)2]2–, which have square-twisted chains containing corner-sharing four-rings of alternating ZnO4 and PO4 tetrahedra, are assemblied via self-complementary strong and symmetrical hydrogen-bonding R22(8) synthons between the phosphate groups into three-dimensional hydrogen bond frameworks featuring three-dimensional intersecting pseudochannels. The doubly protonated 2,5-dimethylpiperazinium cations are attached to the three-dimensional inorganic framework via N-H···O hydrogen bonds to strengthen the 3-D network.


2021 ◽  
Vol 252 ◽  
pp. 02069
Author(s):  
Xiaoyan Ren ◽  
Haixing Liu ◽  
Yanfang Huo

A novel complex Ni(C12H12N2)3●(C7H5O3)2●(H3BO3) has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. Triclinic, P-1. a= 12.5380(13) Å, b = 13.0100(15) Å, c = 15.1490(18) Å, α= 102.760(3)°, β= 94.480(2)°, γ= 94.540(2)°. V=2390.9(5) Å3. Z=2. R1 =0.0661, wR2 = 0.2128, T=293(2) K. The Ni atom is coordinated by six N atoms from three 4,4′-dimethyl-2,2′-dipyridyl molecular. The molecular structure stabilized by the O-H…O hydrogen-bonding interactions.


1980 ◽  
Vol 45 (8) ◽  
pp. 2147-2151 ◽  
Author(s):  
Jan Lokaj ◽  
Ján Garaj ◽  
Viktor Kettmann ◽  
Viktor Vrábel

Crystal and molecular structure of nickel(II) dimethyldithiocarbamate, Ni[S2CN(CH3)2]2 was solved by X-ray structural analysis and refined by the least squares method to R = 0.06 for 1065 reflections. The compound crystallizes in a space group P I and the triclinic unit cell has the dimensions: a = 6.521 (7), b = 6.798 (9), c = 7.633 (4), α = 67.21 (8)°, β = 67.34 (6)° γ =85.59 (9)°. The experimentally observed density is 1.75 g cm-3 and the calculated value for Z = 1 is 1.73 g cm-3. In the structure , the Ni atom occupies a special position in the centre of symmetry and is coordinated by four sulphur atoms in a plane: Ni-S 0.2218 (4) and 0.2198 nm S1-Ni-S2 angle 79.62 (8)°. The ligand S2CNC2 is nearly planar.


1990 ◽  
Vol 45 (8) ◽  
pp. 1210-1212 ◽  
Author(s):  
Dieter Fenske ◽  
Gerhard Baum ◽  
Hans-Walter Swidersky ◽  
Kurt Dehnicke

[OsCl4(CH3CN)2] · 1/2CH3CN has been prepared by the reaction of OsCl5 with acetonitrile in a slow reaction at room temperature, forming red, moisture sensitive crystals. The compound was characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1281 observed unique reflexions, R = 0.031. Lattice dimensions at 20 °C: a = 1032.5(5), b = 1356.0(7), c = 975.9(5) pm. The complex has a molecular structure, in which the osmium atom is octahedrally coordinated by four chlorine atoms and by two N-atoms of the ciscoordinated acetonitrile molecules. The included CH3CN molecules are disordered in two positions.


1997 ◽  
Vol 52 (8) ◽  
pp. 901-905 ◽  
Author(s):  
Vera V Ponomareva ◽  
Victor V Skopenko ◽  
Konstantin V Domasevitch ◽  
Joachim Sieler ◽  
Thomas Gelbrich

Abstract The caesium hydrogen benzoylcyanoximate (L-) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [monoclinic, space group P21/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Å, β = 90.13(1)°, V = 3434.3(9) Å, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of Cs(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}-, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O - - - O ca. 2.456(5)Å]. The caesium atom deviates by 1.492(3) Å from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical “sunrise coordination” [Cs-O (ether) 3.040(9)-3.312(7) Å]. The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (Cs-O ca. 3.040(9), 3.312(7) Å; Cs-N ca. 3.469(5), 3.679(6) Å). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism.


2014 ◽  
Vol 488-489 ◽  
pp. 252-255
Author(s):  
Hai Xing Liu ◽  
Qing Liu ◽  
Huan Mei Guo ◽  
Quan Hua Fan ◽  
Xiao Ping Zhang ◽  
...  

The Eu complex C4H10EuO10has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Eu atom is coordinated by nine O atoms. The molecular structure stabilized by the O-H…O hydrogen-bonding interactions.


1982 ◽  
Vol 47 (10) ◽  
pp. 2623-2632 ◽  
Author(s):  
Viktor Vrábel ◽  
Jan Lokaj ◽  
Ján Garaj ◽  
František Pavelčík

The crystal structure of [Cu(H2O)(en)2][Cu2(CN)3(SeCN)] was solved by single crystal X-ray structural analysis in the triclinic system with a space group of P1 and in the monoclinic system with a space group of C2. In the triclinic system the unit cell has dimensions of a = 0.8445(3), b = 0.7903(3), c = 0.8444(3) nm, α = 119.58(2), β = 118.59(2) and γ = 93.63(3)° and, in the monoclinic system, a = 1.3331(4), b = 0.8670(2), c = 0.8267(3), β = 122.60(2)°. The structure was refined by the least squares method to final value of R = 5.5% in the triclinic system and R = 7.8% in the monoclinic system. The coordination sphere around the Cu(II) atom is square pyramidal, formed of two ethylenediamine molecules and one water molecule. The Cu(I) atoms are tetrahedrally coordinated by bridging SeCN and CN ligands to form infinite three-dimensional chains. The SeCN group is bonded to the Cu(I) atoms through the Se atom at distances of 0.2731(3) and 0.2745(3) nm.


2009 ◽  
Vol 64 (7) ◽  
pp. 821-825 ◽  
Author(s):  
Xiuhong Xu ◽  
Ling Zhang ◽  
Yi Zhang ◽  
Bin Qi ◽  
Fang Luo

The sandwich-type complex Na(H2O)6(C6H16O3N)2[Na2(H2O)7(C6H16O3N)]2[(Na(H2O)2)3- (Cu(H2O))3(BiW9O33)2]・14H2O (1) (C6H16O3N+ = protonated triethanolamine) has been synthesized and structurally characterized by single-crystal X-ray diffraction, IR spectroscopy and TG analysis. The basic framework of 1 is built from a sandwich-type [(Na(H2O)2)3- (Cu(H2O))3(BiW9O33)2]9− anion, two [Na2(H2O)7(C6H16O3N)]3+ cations, a free Na(H2O)6+ cation, and two free C6H16O3N+ units. In compound 1, the [(Na(H2O)2)3(Cu(H2O))3- (BiW9O33)2]9− anion links two bi-nuclear units [Na2(H2O)7(C6H16O3N)]3+ to form a [Na2- (H2O)7(C6H16O3N)]2[(Na(H2O)2)3(Cu(H2O))3(BiW9O33)2]3− cluster, and a new 3D supramolecular structure is further constructed by hydrogen bonding interactions among this cluster, the free Na(H2O)6+ cation, and the free C6H16O3N+ cations. Crystal data: Cu3Na8Bi2W18C24H150O121N4, monoclinic, C2/c, a = 14.5668(13), b = 23.0405(13), c = 37.412(2) Å , β = 91.569(10)° , Z = 4.


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