Hydrogen-Bonded Molecular Ladders and Interlaced Networks in Complexes Built of V-Shaped Molecules 4,4′-Isopropylidenediphenol or 4,4′-Oxydibenzoic Acid with 4,4′-Bipyridine

Abstract  

The title compounds, C₁₀H₈N₂·C₁₅H₁₆O₂ (1) and C₁₀H₈N₂·C₁₄H₁₀O₅ (2), were synthesized by 4,4′-bipyridyl and two similar V-shaped molecules. The two complexes both crystallized in the same space group P2₁/n with the crystal cell parameters: a = 16.0536(3) ?, b = 6.42730(1) ?, c = 21.2717(4) ?, β = 102.330°, V = 2144.21(7) ?³, Z = 4 in compound 1 and a = 7.45020(10) ?, b = 10.0784(2) ?, c = 26.9430(5) ?, β = 92.1140(10)°, V = 2021.67(6) ?³, Z = 4 in compound 2. Compound 1 forms regular molecular chains containing alternative 4,4′-bipyridyl and 4,4′-isopropylidenediphenol units; the molecular components are linked by two types of O–H···N hydrogen bonds. Additionally, every two neighboring chains are connected to be a ladder structure by means of weak C–H···O interactions. In compound 2, 4,4′-bipyridyl and 4,4′-oxydibenzoic acid first construct one-dimensional architecture by strong O–H···N hydrogen bonds, which are similar with the interactions in compound 1. Secondly, two types of weak C–H···O contacts formed between 4,4′-bipyridyl and the acid link one-dimensional chains to be interlaced three-dimensional hydrogen-bonded networks.     

Crystal structures of four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium

Herein four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium, 2(CH₃)₄N⁺·C₁₄H₈O₄S₂^2?·H₂O (1), (C₂H₅)₄N⁺·C₁₄H₉O₄S₂^?·0.25H₂O(2), (n-C₃H₇)₄N⁺·C₁₄H₉O₄S₂^? (3) and (n-C₄H₉)₄N⁺·C₁₄H₉O₄S₂^?(4) are prepared and characterized by X-ray single crystal diffraction. As shown in the results, compounds 1 and 3 belong to orthorhombic crystal system with different space groups of P2₁2₁2₁ and Pca2₁, and 2 and 4 are monoclinic system with similar groups of P2₁/n and P2₁/c. The crystallography data are displayed below: 1: a = 10.5903(7) Å, b = 10.6651(7) Å, c = 21.9476(13) Å, V = 2478.9(3) ų, Z = 4, R₁ = 0.0359; 2: a = 8.13340(1) Å, b = 22.0741(3)Å, c = 13.2143(2)Å, β = 101.6360(1) °, V = 2323.70(6) ų, Z = 1, R₁ = 0.0385; 3: a = 15.7857(2) Å, b = 8.24830(1) Å, c = 20.2599(2) Å, V = 2637.94(5) ų, Z = 4, R₁ = 0.0308_degree4: a = 11.7476(2) Å, b = 17.1346(1) Å, c = 16.3583(3)Å, β = 109.4560(1) °, V = 3104.74(9)ų, Z = 4, R₁ = 0.0562. Interestingly, although the carbon chains of the guest templates vary from methyl group to butyl group, the host molecules of 2,2′-dithiosalicylic acid all construct the similar 2D hydrogen-bonded host layers with or without the existence of water molecules to contain the guest templates to yield analogous sandwich-like inclusion compounds. Obviously, although the guest templates will have certain effects on the ultimate formation of these crystal structures, the host molecule of 2,2′-dithiosalicylic acid is a controlling factor to form these four inclusion compounds.     

Syntheses,Structures and Optical Properties of a Series of Lanthanide Complexes with Chelidamic Acid and 4,4′-Bipyridyl

Abstract  

The title complexes, (C₁₀H₈N₂)·[Y(C₇H₃NO₅)(C₇H₄NO₅)·2H₂O]·3H₂O (1), (C₁₀H₈N₂)·[Er(C₇H₃NO₅)(C₇H₄NO₅)·2H₂O]·3H₂O (2), (C₁₀H₈N₂)·[La(C₇H₃NO₅)(C₇H₄NO₅)·2H₂O]·4.5H₂O (3), (C₁₀H₈N₂)·[Sm(C₇H₃NO₅)(C₇H₄NO₅)·2H₂O]·4.75H₂O (4), (C₁₀H₈N₂)·[Pr(C₇H₃NO₅)(C₇H₄NO₅)·2H₂O]·4.75H₂O (5) were synthesized and characterized by X-ray single-crystal diffraction. The crystal structures of 1–2 reveal that they are isomorphous, among which the metal atoms are all eight-coordinate with a distorted dodecahedron coordination geometry. The structures of 3–5 are isomorphic, among which the metal atoms are all nine-coordinate with distorted tricapped trigonal prismatic coordination geometries by two chelidamic acid ligands. Complexes 1–5 are formed into 3D networks by H-bonds. The optical properties of 1–5 were investigated in terms of fluorescent spectra, which all exhibit strong luminescence.     

Molecular Association of Almotriptan with Oxalate and Terephthalate Anions

Abstract  

Crystal structures of anti-migraine drug almotriptan were crystallized with oxalic acid (I) and with terephthalic acid (II) and their crystal structures and molecular associations were determined using X-ray diffraction methods. Crystals of both (I) and (II) are monoclinic, space group P2₁/c, with a = 5.6270(4) ?, b = 27.6419(19) ?, c = 13.6228(9) ?, β = 93.057(1)°, V = 2115.9(3) ?³, Z = 4 (I) and a = 13.3756(15) ?, b = 15.6065(17) ?, c = 10.7238(12) ?, β = 98.017(2)°, V = 2216.7(4) ?³, Z = 4 (II). In almotriptan oxalate {systematic name: N,N-dimethyl-2-[5-(pyrrolidin-1-ylsulfonyl-methyl)-1H-indol-3-yl]-ethanaminium semioxalate}, C₁₇H₂₆N₃O₂S⁺, C₂HO₄ ⁻, (I) and in almotriptan hemi terephthalate hydrate {systematic name: N,N-dimethyl-2-[5-(pyrrolidin-1-ylsulfonyl-methyl)-1H-indol-3-yl]-ethanaminium hemi terephthalate monohydrate}, C₁₇H₂₆N₃O₂S⁺, 0.5(C₈H₄O₄ ²⁻), H₂O, (II), both the almotriptan cations form a trimer with the corresponding anions via N–H···O hydrogen bonds. In (I), the oxalate salt is monoprotonated and in (II), the terephthalic acid is located across the inversion centre and exists as doubly protonated anion. In (I), the cation and anion are interlinked by the N–H···O and O–H···O hydrogen bonds into continuous two-dimensional layers generate an R₆⁶(34) hydrogen-bonded motif tetramers running parallel to the (0 0 1) plane. In (II), the cation and water form a centrosymmetric tetramer of R₄⁴(22) hydrogen-bonded motif via N–H···O and O–H···O hydrogen bonds and further cross-linked by centrosymmetric anions to form an infinite three-dimensional supramolecular hydrogen-bonded networks.     

The Zolmitriptan-Pyridine (1:1) and Zolmitriptan-Propiophenone (3:2) Inclusion Complex

Abstract  

The crystal structures of zolmitriptan with pyridine (I) and propiophenone (II) solvates have been determined by single crystal X-ray diffraction studies. Compound (I) crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 8.5610(5) ?, b = 12.2709(7) ?, c = 19.6201(12) ?, V = 2061.1(2) ?³, and Z = 4, while compound (II) crystallizes in the monoclinic space group P2₁ with a = 15.085(1) ?, b = 19.656(12) ?, c = 21.0860(13) ?, β = 92.068(1)°, V = 6248(4) ?³ and Z = 4. The asymmetric unit of (I), C₁₆H₂₁N₃O₂·C₅H₅N, contains one zolmitriptan molecule and one pyridine solvate, while the asymmetric unit of (II), 3(C₁₆H₂₁N₃O₂)·2(C₉H₁₀O) comprises six zolmitriptan molecules and four propiophenone solvates. In both structures, the N–H···N hydrogen bonds, form an infinite helical chain and generate a C(11)-type motif in (I) and a D₂²(13)-type motif in (II). Both the complexes have layer structures, the layers being constructed from rings (cavity) of four zolmitriptan molecules, hydrogen bonded through N–H···N and N–H···O bonds, where the pyridine (I) and propiophenone (II) solvates are included in an R₄⁴(33) ring.     

Crystal structure of complexes of bivalent Co,Ni, and Cd with anions of benzoic and 2-(acetylamino)-5-nitrobenzoic acids

The structure of three complexes of bivalent metals (cobalt, nickel, and cadmium) with anions of benzoic (HL ¹) and 2-(acetylamino)-5-nitrobenzoic (HL ²) acids, namely, [Co₂¹ (H₂O)₂(μ-C₄H₄N₂)] _n (I), [NiL²(H₂O)₅]L² · 2H₂O (II), and [Cd(μ-L ²)₂(H₂O)₂] _n · 2nH₂O (III), is determined. In chainlike structure I, cobalt atoms are connected by bridging pyrazine molecules; structure II contains isolated complexes. In structure III, centrosymmetric (CdOCO)₂ cycles and polymeric ribbons are formed due to the coordination of the carboxylate group of the L ² ligand to two cadmium atoms.     

Structures of two N-methylated tricyclic quinolones with antimalarial activity

The crystal structures of two N-methylated tricyclic quinolones were determined. 3-amino-6-methoxy-9-methyl-(1H)pyrazolo[3,4-b]-4-quinolone hydrate, C₁₂H₁₂N₄O₂ · H₂O (1) crystallizes in P-1 with a=11.5078(18) ?, b=13.0614(19) ?, c=9.0860(15) ?, α=106.229(4)°, β=108.378(3)°, γ=71.118(3)° and Z=4, while 2,4-diamino-10-methyl-9-methoxypyrimido[4,5-b]-5-quinolone, C₁₃H₁₃N₅O₂ (2) crystallizes in P2₁/n with a=10.6643(17) ?, b=10.1114(17) ?, c=11.3185(18) ?, β=99.351(4)° and Z=4. Both molecules are essentially planar, including the exocyclic groups. 1 and 2 have moderate antimalarial activity which seems to be related to the formation of intramolecular N – H · · · O=C hydrogen bonds; 1 does not form these bonds and has approximately twice the activity of 2. In both crystal structures there are extensive networks of N–H · · · O and N–H · · · N hydrogen bonds, and in 1 the water molecules of solvation form N–H · · · Ow, Ow–H · · · O=C and Ow–H · · · Ow bonds.     

Synthesis, structure and characterization of a new inorganic-organic hybrid complex (C3H5N2)2[Cd(C3H4N2)2Nb2O3F8]·2H2O

(C₃H₅N₂)₂[Cd(C₃H₄N₂)₂Nb₂O₃F₈]·2H₂O (C₃H₄N₂=imidazole) (1) was prepared from the hydrothermal reaction of Nb₂O₅, 3CdSO₄·8H₂O, C₃H₄N₂, HF and H₂O at 403 K, and characterized by single crystal X-ray diffraction and IR spectra. 1 crystallizes in the orthorhombic system, space group Pba2, with a=11.0192(9), b=16.8012(14), c=6.8717(6) ?, and Z=2. The crystal is made up of [Cd(C₃H₄N₂)₂Nb₂O₃F₈]²⁻ anions, [C₃H₅N₂]⁺ complex cations and H₂O molecules of crystallization. And the backbone of the compound is a one dimension coordination polymeric chain containing the anions. The complex cations and anions are linked through hydrogen bonding interactions. Co-crystallized water molecules fill in the pores and hydrogen bond to the host. Bond valence sums show that O1, O3 and F3 have much more negative charge, which are in agreement with the crystal structure that they act as bridging atoms.Supplementary material CCDC-606794 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdc.cam.ac.uk/ const/retrieving.html or from the Cambridge Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Supramolecular Network via Hydrogen Bonding and π–π Stacking in 4,4′-Bipyridin-1-ium Perchlorate Dihydrate

Abstract The crystal structure of 4,4′-bipyridin-1-ium perchlorate dihydrate, [C₁₀H₉N₂](ClO₄) · 2H₂O, is determined by room temperature X-ray diffraction. The compound crystallizes in the triclinic space group P-1 with a = 8.122(3) ?, b = 9.726(3) ?, c = 17.648(6) ?, α = 78.181(4)°, β = 82.797(5)°, γ = 67.439(4)°, Z = 2, V = 1258.4(7) ?³. In the compound, monoprotonated 4,4′-bipyridin-1-ium cations are self-assembled into supramolecular chains along the a-axis through N–H···N hydrogen bonds in a head-to-tail fashion. The chains are stacked via π–π stacking interactions to create two-dimensional sheets. The interlayer space is occupied by the hydrogen-bonded water chains that are linked to the organic sheets via C–H···O interactions and the perchlorate anions that are linked to the water chains and the organic sheets via O–H···O and C–H···O hydrogen bonds, respectively, thus generating a three-dimensional supramolecular architecture. Index Abstract Supramolecular Network via Hydrogen Bonding and π–π Stacking in 4,4′-Bipyridin-1-ium perchlorate dihydrate Jian-Yong Zhang, Ai-Ling Cheng and En-Qing Gao* Monoprotonated 4,4′-bipyridin-1-ium cations are self-assembled into supramolecular chains along the a-axis through N–H···N hydrogen bonds, and these chains are stacked via π–π stacking and hydrogen bond interactions involving water molecules and perchlorate anions.      

The Crystal Structures of Bis(2-amino-5-methylpyridinium) Tetrabromometallate(II): Intermolecular Interactions in (C<Subscript>6</Subscript>H<Subscript>9</Subscript>N<Subscript>2</Subscript>)<Subscript>2</Subscript>[MBr<Subscript>4</Subscript>]; M = Cd and Co

Abstract The crystallization and structures of a triclinic (henceforth T) (C₆H₉N₂)₂[CdBr₄] and a monoclinic (henceforth M) of (C₆H₉N₂)₂[CoBr₄] are reported. The crystal packing of both solids is analyzed and compared: both contain parallel chains of cations and stacks of anions. In both T and M, each [MBr₄]²⁻ is hydrogen bonded non-symmetrically to surrounding cations in a ladder chains that run along b axis, with planar cations in both structures falling in parallel to the planes to anions. In T the cation chains are further involved in classical π···π stacking, while in M the cation chains show less significant stacking, with longer repeat distance. Index Abstract Extensive N–H···Br hydrogen bonds link both anions and cations into chains of the ladder type parallel to the crystallographic b axis. The crystal structures of bis(2-amino-5-methylpyridinium) tetrabromometallate(II): Intermolecular interactions in (C6H9N2)2[MBr4]; M = Cd and Co Rawhi Al-Far and Basem Fares Ali      

Hydrogen Bonding Patterns of Coordinated Ligands in Hybrid Materials: Crystal Structures of Hydronium Tetra(Thiocyanato-κN)-Zinc(II): Tris(2-Amino-4,6-Dimethylpyrimidinium) (2-amino-4,6-dimethylpyrimidine) Dinitrate and Bis(2-Amino-4,6-Dimethylpyrimidinium) Tetrachlorocobaltate(II) Monohydrate

Abstract  

Hydronium tetra(thiocyanato-κN)-zinc (II) tri (2-amino-4,6-dimethylpyrimidinium) 2-amino-4,6-dimethylpyrimidine dinitrate [H₃O⁺ Zn(NCS)₄ 3(C₆H₁₀N₃ ⁺) C₆H₉N₃ 2(NO₃)⁻] and bis(2-amino-4,6-dimethylpyrimidinium) tetrachlorocobaltate(II) monohydrate [2(C₆H₁₀N₃ ⁺)] CoCl₄ H₂O have been synthesized and characterized by X-ray diffraction analysis and spectroscopic studies. In compound 1, the coordination geometry around zinc is distorted tetrahedral, Zn being bonded to four N atoms from the thiocyanate anions. In compound 2, the anion [CoCl₄]²⁻ displays distortion from ideal tetrahedral geometry. The 2-amino-4,6-dimethylpyrimidine cations are not directly coordinated to zinc/cobalt, but are hydrogen bonded to the thiocyanate/chloride ions. In both the compounds the protonated nitrogen N1 and the 2-amino group are hydrogen bonded to the nitro group/chloride ions/water molecule through N–H···O and N–H···Cl hydrogen bonds to form R₂²(8) motifs. In both the compounds, the pyrimidine cations also form base pairs via a pair of N–H···N hydrogen bonds involving the amino group and the unprotonated ring N atom. The crystal structures are further stabilized by N–H···S, O–H···O, C–H···O and C–H···Cl hydrogen bonds.     

ESR and Theoretical Studies of Bis-Benzene-1, 2-Diselenolate Nickel and Related Complexes

Abstract

ESR and theoretical studies of the transition metal complexes of [Co and Ni (Se₂C₆H₄)₂]^? (n-C₄H₉)₄N⁺ are reported and compared with closely related systems. Room temperature single crystal X-ray studies reveal the Nickel complex is orthorhombic. ESR studies of the polycrystalline powders of the Ni complex as a function of temperature from 108 K to room temperature show a series of spectral envelopes which can arise only from a paramagnetic site which possesses axial symmetry. At ca 160 K, there is an abrupt change in the value of the principal components of the anisotropic g-tensor of the Ni complex which is discussed. Low temperature ESR studies of polycrystalline samples of the ground state triplet Cobalt complex which is isomorphous with the Nickel complex reveal an orthorhombic g-tensor. From the field position of the half-field resonance, it is possible to calculate a mean separation, of the two electrons which make up the triplet state, of 4.3 (±0.5) A.     

Inclusion Compounds of the Host 9-(4-Methylphenyl)-9<Emphasis Type="Italic">H</Emphasis>-xanthen-9-ol with a Series of Organic Guests

Abstract  The host 9-(4-methylphenyl)-9H-xanthen-9-ol (H) forms inclusion compounds with the guests cyclohexane (H · ?CHEX), benzene (H · ?BENZ), 1,4-dioxane (H · ?DIOX), cyclohexanone (H · CYONE), N,N-dimethylformamide (H · DMF) and N,N-dimethylacetamide (H · DMA). For those guest molecules possessing electron acceptor atoms/functionalities hydrogen bonding with the host is the prominent mode of interaction and presents itself in the form of (Host)–OH···O(Guest) linkages. The cyclohexane and benzene guests however, occupy voids created by neighbouring host molecules which form hydrogen bonded dimers of the form (Host)–OH···O(Host). The structures of the inclusion compounds were investigated and their thermal stabilities determined. Selectivity experiments were also conducted. Graphical Abstract  The host 9-(4-methylphenyl)-9H-xanthen-9-ol (H) forms inclusion compounds with the guests cyclohexane (H · ?CHEX), benzene (H · ?BENZ), 1,4-dioxane (H · ?DIOX), cyclohexanone (H · CYONE), N,N-dimethylformamide (H · DMF) and N,N-dimethylacetamide (H · DMA). Crystal structures and thermal stabilities were determined. The host selectivity was also investigated.      

One Novel Three-dimensional Network Constructed from [Mn(4,4′-bip)<Subscript>2</Subscript>(OH<Subscript>2</Subscript>)<Subscript>4</Subscript>]<Superscript>2+</Superscript> Cations and DBA<Superscript>2−</Superscript> Anions via Hydrogen-bonding and π–π Interactions

Abstract One new mononuclear manganese complex of [Mn(4,4′-bip)₂(OH₂)₄](DBA) · 4H₂O (1) (4,4′-bipyridine, 4,4′-bip; H₂DBA, benzene-1,3-dicarboxylic acid) has been obtained from the hydrothermal reaction of MnCl₂ · 4H₂O, 4,4′-bipyridine and H₂DBA in the solvent of H₂O at 140 °C for 3 days, characterized by X-ray analysis, spectroscopic methods, and thermal analysis. Packing diagram shows that the three-dimensional network was formed via hydrogen bonds and strong π–π interactions. Graphical abstract One Novel Three-dimensional Network Constructed from [Mn(4,4′-bip) ₂ (OH ₂ ) ₄ ] ²⁺ Cations and DBA ²⁻ Anions via Hydrogen-bonding and π–π Interactions Ying Liu, Bao Zhang, Jian-min Dou, Da-qi Wang, Da-cheng Li, Lei Zhou One new mononuclear manganese complex of [Mn(4,4’-bip)₂(OH₂)₄](DBA) · 4H₂O (1) (4,4’-bipyridine, 4,4’-bip; H₂DBA, benzene-1, 3-dicarboxylic acid) has been obtained and haracterized by X-ray analysis, spectroscopic methods, and thermal analysis. Packing diagram shows that the three-dimensional network was formed via hydrogen bonds and strong π-π interactions.      

Crystal structure of an unusual four-coordinated copper(II) complex containing 1,10-o-phenanthroline and salicyclic acid crystal structure containing Cu(II) o-phen and salicyclic acid

We have synthesized a multi-ligand chelate copper(II) complex [Cu · (C₇H₅O₃] · (C₁₂H₈N₂) · H₂O₁ · (C₇H₆O₃)· NO₃, and determined its structure by X-ray diffraction method. The space group of the title compound is P2₁/a. It is monoclinic, with a = 14.227(4), b = 9.627(4), c = 19.008(7) Å, β = 102.06(3)·, Z = 4. The two salicyclic acid molecules in the cell are in different environments, one inner, the other outer. The geometry around Cu(II) is a four-coordinated distorted plane square. The two coordinating atoms are two nitrogen atoms from phenanthroline, one oxygen atom from salicyclic acid, one oxygen atom from water.     

Crystal Structure of Three Isomorphous Compounds of 2,5-Dibromopyridine with Tetrahalometalate(II) Ions

Abstract  Three salts of 2,5-dibromopyridinium with metal halides, (C₅H₄Br₂N)₂[CuCl₄], (I); (C₅H₄Br₂N)₂[CuBr₄], (II); and (C₅H₄Br₂N)₂[CdBr₄], (III), are isomorphous in C2/c with cell volumes 1864.5(8), 1974.6(4) and 2072.9(7) ?³, respectively. For the Cu cases (I) and (II) the discrete [MX₄]²⁻ anions are strongly distorted with max/min tetrahedral angles of 131.19(8)°/99.67(9)° and 130.24(5)°/99.36(11)°, respectively. For the Cd case (III) the distortion is much less with max/min tetrahedral angles of 115.97(3)°/105.99(4)°. The cations are planar. The short hal···hal contacts are for (I), aryl Br···anionic Cl 3.335(3) ? and 3.430(2) ?; for (II), aryl Br···anionic Br 3.473(2) ? and 3.567(2) ?; and for (III), aryl Br···anionic Br 3.452(1) ? and 3.675(1) ?. Longer aryl Br···aryl Br contacts (3.842(2) ? to 3.967(2) ? are present in the three isomorphs. Bifurcated hydrogen bonding to two anionic halides exist in the three structures with N–H···Cl 3.365(8) ? and 3.379(7) ? in (I), N–H···Br 3.539(11) ? and 3.425(11) ? in (II), and N–H···Br 3.426(5) ? and 3.387(5) ? in (III). Short ring contacts exist with the perpendicular distances between mean cation planes in (I), (II), and (III) of 3.68(6) ?, 3.56(1) ? and 3.72(1) ?, respectively. Index Abstract  An analysis is made of the competition between hydrogen bonding, halogen–halogen and halogen–halide interactions as well as differences between [CuX₄]²⁻ and [CdX_4] ²⁻ polydedra in the structures of the three isomorphs.      

Hydrothermal Synthesis,Crystal Structure,and Luminescence Property of Two Lanthanide Coordination Polymers with Diglycolic Acid

Abstract  Two new coordination polymers {[Tb₂(C₄H₄O₅)₃ · 4H₂O] · 2H₂O} _n (1) and {[La₂(C₄H₄O₅)₃ · 3H₂O] · 3H₂O} _n (2) (C₄H₄O₅ ²⁻ = diglycolato) were prepared by hydrothermal reaction and characterized by X-ray crystallography. The two complexes have different network structures through carboxylate oxygen atoms and ether oxygen atoms from diglycolato ligands linking lanthanide ions. The characteristic transition bands ⁵D₄ → ⁷F_J (J = 6 − 3) of Tb(III) ion are observed in complex 1. Graphical Abstract  Two new coordination polymers {[Tb₂(C₄H₄O₅)₃ · 4H₂O] · 2H₂O} _n (1) and {[La₂(C₄H₄O₅)₃ · 3H₂O] · 3H₂O} _n (2) (C₄H₄O₅ ²⁻ = diglycolato) have network structures through the carboxylate oxygen atoms and ether oxygen atoms from diglycolato ligands. The emission spectrum of complex 1 indicates the ⁵D₄ → ⁷F_J (J = 6 − 3) transitions of Tb(III) ion.      

Synthesis, Structural Characterization and Crystal Structure of Selenium Bearing 3-(Phenylseleno) Propylammonium Acetate Salt and its Cleavage on Reaction with Mercury(II) and Tin(IV) Salts

Abstract  

3-(Phenylseleno) propylammonium acetate, C₉H₁₄NSe⁺ C₂H₃O₂ ^–, L ¹ , the first example of a selenium bearing acetate salt has been synthesized and characterized by spectroscopic, NMR, DSC and single crystal X-ray crystallographic techniques. L ¹ crystallizes with one cation–anion pair in the asymmetric unit. Reactions of L ¹ with four different metal salts revealed four new selenium bearing compounds (1–4) whose identities are characterized by spectroscopic and NMR techniques. The crystal structure of Compound 1, [C₉H₁₄NSe]₂⁺ [ClO₄]₂^–, whose crystal structure has been confirmed. It crystallizes with two independent cation–anion pairs in the asymmetric unit. Both L ¹ and Compound 1 display strong N–H···O hydrogen bond intermolecular interactions which help stabilize crystal packing in the unit cell.     

Crystal structures of substituted imidazolidine derivatives

The crystal structures of isoxazole, 3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]methyl-5-phenyl-,N-oxide] (C₁₃H₁₃N₅O₃) (I), isoxazole,3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]-methyl-5-(4-methylphenyl)-,N-oxide] (C₁₄H₁₅N₅O₃) (II) and isoxazole, 3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]-methyl-5-(2-methoxyphenyl)-,N-oxide] (C₁₄H₁₅N₅O₄) (III) have been determined by X-ray diffraction studies. The compound I, crystallized in triclinic space group with unit cell dimensions a = 7.2405(7) ?, b = 7.9936(8) ?, c = 11.6573(11) ?, α = 97.801(2)°, β = 90.884(2)°, γ = 96.250(2)° and Z = 2. Compound II crystallized in orthorhombic space group Pna2₁ with unit cell dimensions a = 10.1778(10) ?, b = 28.228(3) ?, c = 5.1206(5) ?, and Z = 4. Compound III crystallized in monoclinic space group P2₁/n with unit cell dimensions a = 7.8439(9) ?, b = 7.8544(9) ?, c = 23.534(3) ?, β = 99.464(2)° and Z = 4. For all three compounds, the five-membered imidazolidine ring adopts an envelope conformation. The crystal structures are stabilized by both the intramolecular N–H···O and intermolecular N–H···N hydrogen bonding.     

Crystal structures of polymeric complexes of zinc(II) bromide and perchlorate with 1,4-diazoniabicyclo [2.2.2]octane-1,4-diacetate

Two zinc(II) complexes containing a flexible double betaine, namely [{Zn(L)Br₂}_n]·nH₂O (1) and [{Zn(L)₂(H₂O)₂}_n](ClO₄)_2n·4nH₂O (2) [L=1,4-diazoniabicyclo [2.2.2]octane-1,4-diacetate,⁻O₂CCH₂N⁺(CH₂CH₂)₃N⁺CH₂CO₂ ⁻], have been prepared and shown to have polymeric structures by single-crystal X-ray analysis. Complex (1) exhibits an infinite zigzag chain in which each zinc(II) atom is coordinated by two unidentate carboxylate oxygen atoms and two bromide ligands in a distorted tetrahedral geometry. Complex (2) consists of an assembly of catonic Zn(L)₂(H₂O)₂ ²⁺ moieties and discrete perchlorate anions as well as lattice water molecules. In (2) each zinc(II) atom is coordinated by two pairs of unidentate carboxylate oxygen atoms and two aqua ligands in a distorted octahedral geometry and cross-linked by skeletons of double betaine ligands to form a corrugated layer structure corresponding to the plane (100).