Polynuclear chloromercurate(II) systems in their chloropyridinium salts

1999 ◽  
Vol 55 (3) ◽  
pp. 396-409 ◽  
Author(s):  
Anthony Linden ◽  
Bruce D. James ◽  
John Liesegang ◽  
Nick Gonis

The chloromercurate(II) salts of 2-, 3- and 4-chloropyridine display a variety of anion stoichiometries and structures, including the rare [Hg3Cl10]4− stoichiometry. 2-Chloropyridinium trichloromercurate(II), (I), (C5H5ClN)[HgCl3], monoclinic, P21/n, a = 9.094 (8), b = 18.143 (4), c = 12.902 (3) Å, β = 106.13 (4)° with Z = 8, has the [HgCl3]− stoichiometry, but the anions are infinite chains composed of [HgCl3]−, HgCl2 and Cl− moieties linked by longer Hg...Cl contacts. Hydrogen bonds link the cations to the formal Cl− ions. Tetrakis(3-chloropyridinium) decachlorotrimercurate(II), (II), (C5H5ClN)4[Hg3Cl10], monoclinic, P21/n, a = 7.522 (2), b = 28.046 (3), c = 9.165 (2) Å, β = 105.78 (2)° with Z = 2, has the rare [Hg3Cl10]4− stoichiometry and contains infinite one-dimensional double-stranded {([HgCl4]2−)2 [HgCl2]} n anionic chains made up of linear HgCl2 and distorted [HgCl4]2− entities linked together by longer Hg...Cl contacts. The HgCl2 moieties are joined by double [HgCl4]2− bridges. Hydrogen bonds link the cations to the sides of the anionic columns. Tetrakis(4-chloropyridinium) decachlorotrimercurate(II), (III), (C5H5ClN)4[Hg3Cl10], triclinic, P1¯, a = 9.907 (3), b = 13.226 (2), c = 7.282 (2) Å, α = 84.41 (2), β = 74.81 (2), γ = 87.34 (2)° with Z = 1, also has the [Hg3Cl10]4− stoichiometry and the same type of {([HgCl4]2−)2[HgCl2]} n anionic chains that were found in compound (II), but the formal HgCl2 and [HgCl4]2− moieties are more discrete with much weaker contacts linking the individual units. Bifurcated hydrogen bonds with the cations cross-link the anionic chains to form an infinite two-dimensional network. Second forms of the 3- and 4-chloropyridinium salts were also obtained. 3-Chloropyridinium trichloromercurate(II), (IV), (C5H5ClN)[HgCl3], monoclinic, P21/c, a = 7.243 (5), b = 22.145 (8), c = 12.320 (3) Å, β = 99.52 (3)° with Z = 8, has the [HgCl3]− stoichiometry, but the anions are infinite chains composed of distorted [Hg2Cl6]2− moieties. Bifurcated hydrogen bonds from the cations cross-link the anionic chains to form infinite two-dimensional layers. Bis(4-chloropyridinium) hexachlorodimercurate(II), (V), (C5H5ClN)2[Hg2Cl6], monoclinic, C2/m, a = 13.447 (3), b = 7.534 (2), c = 9.939 (2) Å, β = 97.48 (2)° with Z = 2, contains highly symmetrical discrete [Hg2Cl6]2−anions. Bifurcated hydrogen bonds from the cations interconnect the anions to form infinite one-dimensional chains.

2012 ◽  
Vol 68 (5) ◽  
pp. o188-o194 ◽  
Author(s):  
Andreas Lemmerer ◽  
Manuel A. Fernandes

Six ammonium carboxylate salts, namely cyclopentylammonium cinnamate, C5H12N+·C9H7O2−, (I), cyclohexylammonium cinnamate, C6H14N+·C9H7O2−, (II), cycloheptylammonium cinnamate form I, C7H16N+·C9H7O2−, (IIIa), and form II, (IIIb), cyclooctylammonium cinnamate, C8H18N+·C9H7O2−, (IV), and cyclododecylammonium cinnamate, C12H26N+·C9H7O2−, (V), are reported. Salts (II)–(V) all have a 1:1 ratio of cation to anion and feature three N+—H...O−hydrogen bonds forming one-dimensional hydrogen-bonded columns consisting of repeatingR43(10) rings, while salt (I) has a two-dimensional network made up of alternatingR44(12) andR68(20) rings. Salt (III) consists of two polymorphic forms,viz.form I havingZ′ = 1 and form II withZ′ = 2. The latter polymorph has disorder of the cycloheptane rings in the two cations, as well as whole-molecule disorder of one of the cinnamate anions. A similar, but ordered,Z′ = 2 structure is seen in salt (IV).


2006 ◽  
Vol 62 (4) ◽  
pp. o1529-o1531 ◽  
Author(s):  
Li-Ping Zhang ◽  
Long-Guan Zhu

In the crystal structure of the title organic proton-transfer complex, 2C12H11N2 +·C7H4O5S2−·3H2O, the cations form one-dimensional chains via intermolecular N—H...N hydrogen bonds and these chains, in turn, form a two-dimensional network through π–π stacking interactions. In addition, the anions and water molecules are connected into a two-dimensional hydrogen-bonded network through intermolecular O—H...O hydrogen bonds. The two motifs result in sheets of cations and anions stacked alternately.


2006 ◽  
Vol 62 (4) ◽  
pp. o1490-o1491
Author(s):  
Xin-Biao Mao ◽  
Tie-Han Li ◽  
Chun-An Ma ◽  
Qing-Bao Song

The title compound, C5H4ClNO3S, was obtained by hydrolysis of 4-chloropyridine-3-sulfonamide in dilute hydrochloric acid. In the crystal structure, one-dimensional chains are formed via N—H...O hydrogen bonds. In addition, weak C—H...Cl hydrogen bonds link these chains into a two-dimensional network


2007 ◽  
Vol 63 (11) ◽  
pp. m2734-m2735
Author(s):  
Hai-Yan Liu ◽  
Ji-Cheng Ma ◽  
Jin Yang

In the title compound, {[Ag(C6H8N2)(H2O)](C6H4Cl2NO3S)} n , the AgI ion is three-coordinated by two N atoms from two symmetry-related 2,3-dimethylpyrazine (dmp) ligands, and one water O atom in a distorted trigonal–planar geometry. The dmp ligands bridge AgI ions to form a one-dimensional chain structure with charge-balancing 4-amino-2,5-dichlorobenzenesulfonate anions. In the crystal structure, intermolecular O—H...O and N—H...O hydrogen bonds form a two-dimensional network.


2011 ◽  
Vol 66 (5) ◽  
pp. 459-464 ◽  
Author(s):  
Chao Xu ◽  
Sheng-Bo Liu ◽  
Taike Duan ◽  
Qun Chen ◽  
Qian-Feng Zhang

Two novel cadmium coordination polymers, [Cd(pydc)2(tu)]n (1) and [Cd2(SO4)(nic)2(tu)1.5 - (H2O)2]n (2) (pydc = pyridine-2,3-dicarboxylate, nic = nicotinate, tu = thiourea), have been synthesized under hydrothermal conditions and structurally characterized by X-ray diffraction analysis. 1 is a one-dimensional ladder coordination polymer in a two-dimensional network formed by hydrogen bonds. 2 consists of two kinds of Cd(II) centers in different coordination environments connected via nicotinate and sulfate to form a two-dimensional grid network integrated in a three-dimensional framework generated by hydrogen bonds. 2 shows intense fluorescent emission in the solid state at room temperature


2015 ◽  
Vol 71 (8) ◽  
pp. 667-672
Author(s):  
Guang-Kui Shao ◽  
Mei Zhao ◽  
Zheng Wei ◽  
Jian-Ping Ma ◽  
Dian-Shun Guo

The Ugi four-component reaction, a powerful method for the synthesis of diverse dipeptide-like derivatives in combinatorial chemistry, was used to synthesize (S)-1′-{N-[1-(anthracen-9-yl)-2-(tert-butylamino)-2-oxoethyl]-N-(4-methoxyphenyl)carbamoyl}ferrocene-1-carboxylic acid dichloromethane disolvate, [Fe(C6H5O2)(C33H31N2O3)]·2CH2Cl2, (I), and (S)-2-(anthracen-9-yl)-N-tert-butyl-2-[N-(4-methylphenyl)ferrocenylformamido]acetamide, [Fe(C5H5)(C33H31N2O2)], (II). They adopt broadly similar molecular conformations, with near-eclipsed cyclopentadienyl rings and near-perpendicular amide planes in their dipeptide-like chains, one of which is almost coplanar with its attached cyclopentadienyl ring but perpendicular to the aromatic ring bound to the N atom. In the supramolecular structure of (I), a two-dimensional network is constructed based on molecular dimers and a combination of intermolecular O—H...O, N—H...O and C—H...O hydrogen bonds, formingR22(11),R22(16),R22(22) andC(9) motifs. These two-dimensional networks are connected by C—H...O and C—H...Cl contacts to create a three-dimensional framework, where one dichloromethane solvent molecule acts as a bridge between two neighbouring networks. In the packing of (II), classical hydrogen bonds are absent and an infinite one-dimensional chain is generatedviaa combination of C—H...O hydrogen bonds and C—H...π interactions, producing aC(7) motif. This work describes a simple synthesis and the supramolecuar structures of ferrocenyl dipeptide-like compounds and is significant in the development of redox-active receptors.


2013 ◽  
Vol 69 (12) ◽  
pp. 1488-1493 ◽  
Author(s):  
Yan-Fei Liu ◽  
Chao-Wei Zhao ◽  
Jian-Ping Ma ◽  
Qi-Kui Liu ◽  
Yu-Bin Dong

Two novel symmetric fluorene-based ligands, namely, 2,7-bis(1H-imidazol-1-yl)-9,9-dimethyl-9H-fluorene [L1 or (I), C21H18N4] and 2,7-bis(1H-imidazol-1-yl)-9,9-dipropyl-9H-fluorene (L2), have been used to construct the coordination polymerscatena-poly[[dichloridodicopper(I)(Cu—Cu)]-μ-2,7-bis(1H-imidazol-1-yl)-9,9-dimethyl-9H-fluorene], [Cu2Cl2(C21H18N4)]n, (II), andcatena-poly[[tetra-μ2-chlorido-tetracopper(I)]-bis[μ-2,7-bis(1H-imidazol-1-yl)-9,9-dipropyl-9H-fluorene]], [Cu4Cl4(C25H26N4)2]n, (III). There are three types of C—H...N hydrogen bonds in (I), resulting a two-dimensional network in theabplane, including a chiral helical chain along thebaxis. Compounds (II) and (III) are related one-dimensional polymers. In both, CuIatoms connect the symmetric ligands (L1 orL2) into a one-dimensional chain. In (II), the {[CuICl2]−} unit, acting as a co-anion, adheres to the one-dimensional chain through a weak Cu...Cu interaction. However, in (III), the {[CuI2Cl4]2−} unit links two different chains into a one-dimensional rope-ladder-type chain. In addition, there are C—H...Cl hydrogen bonds and π–π interactions in the extended structures of (II) and (III), the difference is that the chains in (II) are linked into a two-dimensional network while the chains in (III) are stacked into a three-dimensional framework.


2015 ◽  
Vol 71 (4) ◽  
pp. 242-246 ◽  
Author(s):  
Hao Guo ◽  
Jinfeng Wu

Two inclusion compounds of dithiobiurea and tetrapropylammonium and tetrabutylammonium are characterized and reported, namely tetrapropylammonium carbamothioyl(carbamothioylamino)azanide, C12H28N+·C2H5N4S2−, (1), and tetrabutylammonium carbamothioyl(carbamothioylamino)azanide, C16H36N+·C2H5N4S2−, (2). The results show that in (1), the dithiobiurea anion forms a dimerviaN—H...N hydrogen bonds and the dimers are connected into wide hydrogen-bonded ribbons. The guest tetrapropylammonium cation changes its character to become the host molecule, generating pseudo-channels containing the aforementioned ribbons by C—H...S contacts, yielding the three-dimensional network structure. In comparison, in (2), the dithiobiurea anions are linkedviaN—H...S interactions, producing one-dimensional chains which pack to generate two-dimensional hydrogen-bonded layers. These layers accommodate the guest tetrabutylammonium cations, resulting in a sandwich-like layer structure with host–guest C—H...S contacts.


2016 ◽  
Vol 72 (6) ◽  
pp. 498-503 ◽  
Author(s):  
Yang-Rong Xu ◽  
Jing-Jing Yang ◽  
Juan Liu ◽  
Gui-Ge Hou ◽  
Qing-Guo Meng

Ocotillol-type saponins have a wide spectrum of biological activities. Previous studies indicated that the configuration at the C24 position may be responsible for their stereoselectivity in pharmacological action and pharmacokinetics. Natural ocotillol-type saponins share a 20(S)-form but it has been found that the 20(R)-stereoisomers have different pharmacological effects. The semisynthesis of 20(R)-ocotillol-type saponins has not been reported and it is therefore worthwhile clarifying their crystal structures. Two C24 epimeric 20(R)-ocotillol-type saponins, namely (20R,24S)-20,24-epoxydammarane-3β,12β,25-triol, C30H52O4, (III), and (20R,24R)-20,24-epoxydammarane-3β,12β,25-triol monohydrate, C30H52O4·H2O, (IV), were synthesized, and their structures were elucidated by spectral studies and finally confirmed by single-crystal X-ray diffraction. The (Me)C—O—C—C(OH) torsion angle of (III) is 146.41 (14)°, whereas the corresponding torsion angle of (IV) is −146.4 (7)°, indicating a different conformation at the C24 position. The crystal stacking in (III) generates anR44(8) motif, through which the molecules are linked into a one-dimensional double chain. The chains are linkedvianonclassical C—H...O hydrogen bonds into a two-dimensional network, and further stacked into a three-dimensional structure. In contrast to (III), epimer (IV) crystallizes as a hydrate, in which the water molecules act as hydrogen-bond donors linking one-dimensional chains into a two-dimensional network through intermolecular O—H...O hydrogen bonds. The hydrogen-bonded chains extend helically along the crystallographicaaxis and generate aC44(8) motif.


2017 ◽  
Vol 73 (7) ◽  
pp. 1056-1061 ◽  
Author(s):  
Lauren A. Mitchell ◽  
Gregory H. Imler ◽  
Damon A. Parrish ◽  
Jeffrey R. Deschamps ◽  
Philip W. Leonard ◽  
...  

In the molecule of neutral bis[(1H-tetrazol-5-yl)methyl]nitramide, (I), C4H6N10O2, there are two intramolecular N—H...O hydrogen bonds. In the crystal, N—H...N hydrogen bonds link molecules, forming a two-dimensional network parallel to (-201) and weak C—H...O, C—H...N hydrogen bonds, and intermolecular π–π stacking completes the three-dimensional network. The anion in the molecular salt, triaminoguanidinium 5-({[(1H-tetrazol-5-yl)methyl](nitro)amino}methyl)tetrazol-1-ide, (II), CH9N6+·C4H5N10O2−, displays intramolecular π–π stacking and in the crystal, N—H...N and N—H...O hydrogen bonds link the components of the structure, forming a three-dimensional network. In the crystal of diammonium bis[(tetrazol-1-id-5-yl)methyl]nitramide monohydrate, (III), 2NH4+·C4H4N10O22−·H2O, O—H...N, N—H...N, and N—H...O hydrogen bonds link the components of the structure into a three-dimensional network. In addition, there is intermolecular π–π stacking. In all three structures, the central N atom of the nitramide is mainlysp2-hybridized. Bond lengths indicate delocalization of charges on the tetrazole rings for all three compounds. Compound (II) was found to be a non-merohedral twin and was solved and refined in the major component.


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