Search

The preparation, X-ray crystal structure, Fourier Transform infrared (FTIR) spectroscopy, and elemental analysis of the three complexes (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (2,6-dichlorobenzoic acid)2: H2O [(tp)· (Hbza)2 · H2O, Hdcba = 2,6-dichlorobenzoic acid] (1) (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (2-pyrazinecarboxylic acid) [(tp) · (Hpyca), Hpyca = 2-pyrazinecarboxylic acid] (2) and (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (3-nitrophthalic acid) [(tp) · (Hntpa)] (3) based on 1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione, 2,6-dichlorobenzoic acid 2-pyrazinecarboxylic acid, and 3-nitrophthalic acid are reported. XRD and FTIR analysis indicated that they are all co-crystal. 1 crystallizes in the monoclinic, space group P21/n, with a = 7.1019(7) Å, b = 12.9494(12) Å, c = 26.253(3) Å, β = 93.536(3)°, V = 2409.8(4) Å3, Z = 4. 2 crystallizes in the monoclinic, space group P21/c, with a = 6.9863(7) Å, b = 25.437(3) Å, c = 7.3987(7) Å, β = 95.152(2)°, V = 1309.5(2) Å3, Z = 4. 3 crystallizes in the monoclinic, space group P21/n, with a = 14.2133(15) Å, b = 8.2333(9) Å, c = 15.3860(17) Å, β = 117.236(5)º, V = 1600.9(3) Å3, Z = 4. The imidazole-carboxylic acid synthon of the CO2H···N type is observed in all the co-crystal. The imidazole H–N also donated the N–H···O hydrogen bonds in all cases. Apart from the classical hydrogen bonds, the auxiliary expanding interactions as CH···O, CH3···O, CH···Cl, O···O, Cl···O, Cl···Cl, Cl···π, O···π, and π···π also play important roles in the structure extension. For the coexistence of the various weak interactions these structures adopted the most common R22(7) supramolecular synthon. In conclusion, we have shown that 2D–3D connections can be constructed by the collective non-covalent interactions. In the three prepared supramolecular assemblies there are plenty of weak nonbonding interactions such as directional hydrogen bonds of O–H···N, N-H···O, O–H···O, intra- and interchain CH···O, CH3···O, CH···Cl, O···O, Cl···O, Cl···Cl, Cl···π, O···π, and π···π interactions, on account of these collective weak interactions, these compounds displayed the 2D–3D framework structures. [ABSTRACT FROM AUTHOR]

Seven organic-inorganic hybrids [(H2L1)3(Bi2Br9)(BiBr6)(H2O)] (1) (L1 = N,N,N′,N′-tetramethylethylenediamine), [(HL2)3(SbCl5)] · Cl (2) (L2 = 4-chlorobenzylamine), [(HL3)3(SbCl4)] · Cl2 (3) (L3 = 2,6-dimethylaniline), [(HL3)2(ZnCl4)] · 2H2O (4), [(HL4)4(Bi2Br10)] (5) (L4 = 2-methylquinoline), [(HL4)2(SbCl5)] (6) and [(H2L5)2(SbCl5)2] · H2O (7) (L5 = bis(N-imidazolyl)methane) were prepared and characterized by IR, XRD, EA and TG analysis. XRD analysis told that all complexes were built from non-covalent bonds between the cations and the perhalometallates anions. The lattice H2O also played crucial role in structure extension in the respective hybrids. Extensive intermolecular interactions have been used in the self-assembly of diverse motifs, ranging from strong X-H···Y (X = O, N; Y = Br, Cl, O) H-bonds to weak CH-M (M = Cl, Br), CH2-M (M = Cl, Br), CH3-M (M = O, Cl, Br), CH3-CH3/CH3-CH/CH2-CH/CH-CH, Cl-Cl, CH3-π and π-π associations. Among them, 3 D architectures are found in 1–2 and 4–7, but only 2 D motif is appeared in 3. The arrangements of the anions and cations in the solid mode are ruled not only by the size and symmetry of the cations, but also by the non-covalent bonds in the crystals. Seven organic-inorganic hybrid salts of Bi, Sb and Zn were prepared by using N-Brønsted bases in HX (Cl, Br), and their structures were characterized through X-ray diffraction. The compounds exhibit 2D sheet and 3D net. The thermal properties were also studied. [ABSTRACT FROM AUTHOR]

C18H17NO3S, monoclinic, Cc (no. 9), a = 32.036(3) Å, b = 7.2154(7) Å, c = 7.4283(8) Å, β = 99.943(2)∘, V = 1691.3(3) Å3, Z = 4, Rgt(F) = 0.0343, wRref(F2) = 0.0821, T = 298 K. [ABSTRACT FROM AUTHOR]

C10H5N5O5, monoclinic, P21/c (no. 14), a = 10.9546(11) Å, b = 7.3433(8) Å, c = 13.2567(15) Å, β = 102.972 (5) ∘ , V = 1039.19(19) Å3, Z = 4, R g t (F) = 0.0630, w R r e f (F2) = 0.1622, T = 298 K. [ABSTRACT FROM AUTHOR]

Eight organic-inorganic hybrid salts [(HL1)(SbCl4)] (1) (L1 = N,N-dimethylbenzylamine), [(HL2)2(ZnCl4)] (2) (L2 = 4-chlorobenzylamine), [(HL2)(L2)(CuCl3)(H2O)2] (3), [(HL3)2(Sb2OCl6)] (4) (L3 = quinoline), [(HL4)4(Bi2Cl10)] (5) (L4 = 2-methylquinoline), [(HL5)(SbCl4)] (6) (L5 = 5,7-dimethyl-1,8-naphthyridine-2-amine), [(H2L6)(SbCl5)] (7) (L6 = 3,6-bis(imidazol-1-yl)pyridazine) and [(H2L7)2(CuBr4)2] · 7H2O (8) (L7 = di(2-benzimidazol-1-ylethyl)ether) were prepared and characterized by IR, XRD, EA and TG analysis. XRD analysis told that all of the complexes were 3 D net built from non-covalent bonds from the cations and the halometallates. The aryl rings of the cations in all of the compounds are essentially planar. The H2O also had crucial role in structure extension in 3 and 8. Extensive intermolecular interactions have been used in the self-assembly of diverse motifs, ranging from strong N-H···X (X = Br, Cl), N-H···O, N-H···N, O-H···O, O-H···Br H-bonds to weak CH2···O, CH3-Cl/CH2-Cl/CH-Cl, Cl-Cl, O-Br, CH3-π, CH2-π, Cl-π and π-π associations. The arrangements of the anions and cations in the solid are ruled not only by the size and symmetry of the cations, but also by the non-covalent bonds in the crystal structures. [ABSTRACT FROM AUTHOR]

Transition metal carboxylates with O- and N-donor ligands are interesting for their structural features. Seven novel isonicotinamide(inic)-based metal complexes of [Cd(inic)2(L1)2(H2O)2] · 2H2O (1) (L1 = 2-chloronicotinate), [Cd(inic)2(L2)2(H2O)2] (2) (L2 = 2,4-dichlorobenzoate), [Cu(inic)2(L3)2] (3) (L3 = 4-chlorophenoxyacetate), [Cu3(inic)6(L4)2(HL4)2(H2O)2] · 2H2O (4) (L4 = azelate), [Zn(inic)2(L1)2(H2O)2] · (inic) · H2O (5), [Zn(inic)(L5)(H2O)4] (6) (L5 = 3-nitrophthalate) and [Zn2(inic)2(L6)2] · 5H2O (7) (L6 = 1,4-cyclohexanedicarboxylate) have been obtained by the introduction of the carboxylates by the common solution method and are structurally featured by different techniques of EA, IR spectra, TG and SCXRD analysis. The X-ray studies told that these complexes display mononuclear to trinuclear structures with octahedral/square-pyramidal geometry around the Zn2+, trigonal bipyramidal/octahedral at the Cu2+ and octahedral for the Cd2+. The inic in 1–7 are coordinated only in monodentate fashion with its ring N, while 5 has the lattice inic. The carboxylates coordinated to the metal in monodentate, chelating bidentate and bridging bidentate fashions. The pair of complementary N-H···O H-bonds from the CONH2 of the inic were found in all compounds except 7. Except 1 and 2, all other compounds bear the CH-O contacts from the pyridine CH of the inic. The intricate intra- and intermolecular classical H-bonds, CH-N, CH-O, CH-Cl, CH2-O, O-N, O-O, Cl-O, Cl-Cl, CH-π, CH2-π, C-π, N-π, Cl-π and π-π associations are elucidated by the X-ray crystallographic studies, which push the discrete complexes into high-dimensional ordered supramolecular structures. [ABSTRACT FROM AUTHOR]

Six organic-inorganic hybrid salts, ([(HL1)2(CdCl4)(H2O)] (1) (L1 = 2-(imidazol-1-yl)-1-phenylethanone), [(HL2)2(ZnCl4)(H2O)] (2) (L2 = 6-bromobenzo[d]thiazol-2-amine), [(H2L3)2(CdCl4)2(CH3OH)] (3) (L3 = bis(N-imidazolyl)methane), [(H2L4)(ZnCl4)(H2O)2] (4) (L4 = bis(N-imidazolyl)butane), [(H2L5)2(CuCl4)2]·7H2O (5) (L5 = di(2-benzimidazol-1-ylethyl)ether) and [(H2L6)4(ZnCl4)4]·7H2O (6) (L6 = 1,2-bis(2-benzimidazolyl)-1,2-ethanediol)), were prepared and characterized by IR, XRD, EA and TG analyses. The aryl rings of the cations in all salts are essentially planar. XRD analysis indicated that all of the complexes are built from non-covalent bonds between the cations and the tetrachlorometallate anions. The lattice solvent (H2O/CH3OH) molecules also played crucial roles in structure extension of all salts. Extensive intermolecular interactions have been used in the self-assembly of motifs, ranging from strong X-H···Y (X = O, N; Y = Cl, O) H-bonds to weak CH···A (A = O, Cl, Br), CH2···A (A = O, Cl), O···O, Cl···O, Cl···S, Cl···π, Br···Cl, CH3···π and π···π associations. 3 D architectures are found in 1 and 3-6, but only a 2 D architecture appeared in 2. The arrangements of the anions and cations in the solid are governed not only by the size and symmetry of the cations, but also by the non-covalent bonds in the crystal structures. [ABSTRACT FROM AUTHOR]

Five crystalline organic acid-base salts [(HL)·(dnsa−), L = 2,6-dimethylaniline, dnsa− = 3,5-dinitrosalicylate] (1), [(HL+)·(4-Hnpta−), 4-Hnpta− = 4-nitrophthalate] (2), [(HL)2·(nds)·(H2O)2, nds = 1,5-naphthalenedisulfonate] (3), [(HL)·(dnb)·(Hdnb), dnb = 3,5-dinitrobenzoate, Hdnb = 3,5-dinitrobenzoic acid] (4) and [(HL)·(dca), dca = dichloroacetate] (5) from 2,6-dimethylaniline and organic acids were prepared and characterized by XRD analysis, IR, mp and elemental analysis. Compound 1 adopts the triclinic, space group Pī, with a = 7.6261(6) Å, b = 8.3429(8) Å, c = 13.1147(12) Å, α = 91.3610(10)º, β = 102.755(2)º, γ = 102.597(2)º, V = 791.96(12) Å3, Z = 2. Compound 2 belongs to the monoclinic, space group P2(1)/c, with a = 14.2552(15) Å, b = 8.1436(8) Å, c = 14.5708(13) Å, α = 90°, β = 113.795(2)º, γ = 90°, V = 1547.7(3) Å3, Z = 4. Compound 3 crystallizes in the monoclinic, space group P2(1)/c, with a = 8.4784(7) Å, b = 17.4798(15) Å, c = 9.1119(8) Å, α = 90°, β = 99.742(2)º, γ = 90°, V = 1330.9(2) Å3, Z = 2. Compound 4 has orthorhombic, space group Pna2(1), with a = 24.5029(19) Å, b = 7.5322(9) Å, c = 26.665(2) Å, α = 90°, β = 90°, γ = 90°, V = 4921.3(8) Å3, Z = 8. Compound 5 crystallizes in the monoclinic, space group C2/c, with a = 19.8970(17) Å, b = 11.1850(11) Å, c = 13.1590(12) Å, α = 90°, β = 123.408(3)º, γ = 90°, V = 2444.6(4) Å3, Z = 8. For 1 it was the relatively weak phenol that has ionized, different from 2 to 5. All supramolecular architectures of 1–5 involve N–H⋯O H-bonds as well as CH3⋯O interactions. The other noncovalent interactions (CH⋯O, CH⋯Cl, O⋯C, O⋯N, O⋯O, Cl⋯Cl, C⋯π, O⋯π, CH3⋯π and π⋯π) in the crystal packing were also ascertained. These weak interactions combined, all compounds displayed 3D framework structures. In the five prepared supramolecular assemblies there are plenty of weak bonding interactions such as directional H-bonds of N–H⋯O, O–H⋯O, O–H⋯S, O–H⋯N and noncovalent bonds of CH⋯O, CH3⋯O, CH⋯Cl, O⋯C, O⋯N, O⋯O, Cl–Cl, C⋯π, O⋯π, CH3⋯π, and aryl⋯aryl interactions. All compounds displayed the 3D framework structures [ABSTRACT FROM AUTHOR]

Two crystalline compounds N-(5-chloro-2-hydroxy-phenyl)-acetamide [L] (1), and (N-(5-chloro-2-hydroxy-phenyl)-acetamide): (3,5-dinitrobenzoic acid) [(L) · (3,5-Hdns), 3,5-Hdns = 3,5-dinitrobenzoic acid] (2) were prepared and characterized by X-ray diffraction analysis, IR, mp, and elemental analysis. Compound 1 crystallizes in the monoclinic, space group C2/c, with a = 9.9833(7) Å, b = 10.7789(8) Å, c = 16.1622(14) Å, β = 92.8010(10)°, V = 1737.1(2) Å3, Z = 8. Compound 2 crystallizes in the monoclinic, space group C2/c, with a = 32.818(3) Å, b = 6.9900(5) Å, c = 14.8431(12) Å, β = 90.5340(10)°, V = 3404.8(5) Å3, Z = 8. Both supramolecular architectures of the compounds 1–2 involve N–H···O/O–H···O/C–H···O hydrogen bonds as well as other non-covalent association. The role of these non-covalent interactions in the crystal packing is ascertained. These weak interactions combined, the compounds displayed 1D–3D structures. The crystal structures of the N-(5-chloro-2-hydroxy-phenyl)-acetamide and its co-crystal with 3,5-dinitrobenzoic acid show the classical hydrogen bonding as well as CH–O, CH3–O, and π···π interactions, giving higher dimensional networks. [ABSTRACT FROM AUTHOR]

Three organic adducts of N-benzyladenine have been prepared with trichloroacetic acid, 3-nitrophthalic acid, and citric acid. The three crystalline complexes were characterized by X-ray diffraction analysis, IR, mp, and elemental analysis. Compound 1 crystallizes in the triclinic, space group P-1, with a = 5.4634(4) Å, b = 9.7180(7) Å, c = 15.9707(12) Å, α = 84.2100(10)°, β = 86.633(2)°, γ = 78.0640(10)°, V = 824.75(10) Å, Z = 2. Compound 2 crystallizes in the triclinic, space group P-1, with a = 7.4065(7) Å, b = 8.1151(8) Å, c = 18.4782(15) Å, α = 95.3190(10)°, β = 90.7750(10)°, γ = 115.063(2)°, V = 1000.00(16) Å, Z = 2. Compound 3 crystallizes in the triclinic, space group P-1, with a = 5.0883(5) Å, b = 13.0295(11) Å, c = 16.4332(14) Å, α = 69.1550(10)°, β = 83.900(3)°, γ = 79.244(2)°, V = 999.35(15) Å, Z = 2. In 1, the N atom was protonated, thus 1 is a salt. For 2 and 3, all carboxyl groups remain protonated, so 2 and 3 are both cocrystal. These structures adopted homo or hetero supramolecular synthons or both. Analysis of the crystal packing of 1- 3 displays that there are O-H···O, O-H···N, N-H···O, and N-H···N hydrogen bonds as well as C-H···O, CH···O, C-H···Cl, O-O, O-N, Cl···N, Cl···O, Cl···π, CH···π, and π···π interactions, giving 2D/3D framework structures. Graphical Abstract: The crystal structures of the N-benzyladenine adducts with trichloroacetic acid, 3-nitrophthalic acid, and citric acid show extensive classical hydrogen bonding as well as C-H···O, CH···O, C-H···Cl, O-O, O-N, Cl···N, Cl···O, Cl···π, CH···π, and π···π interactions, giving 2D/3D framework structures. [ABSTRACT FROM AUTHOR]

Two anhydrous salts of piperidine have been prepared with naphthalene-1,5-disulfonic acid, and 4-nitrophthalic acid by slow evaporation technique, and their structures were fully characterized. These two structures adopted homo or hetero supramolecular synthons. Compound 1 crystallizes in the triclinic, space group P-1, with a = 7.728(3) Å, b = 8.042(3) Å, c = 9.150(3) Å, α = 80.631(4)°, β = 79.433(4)°, γ = 86.531(4)°, V = 551.3(3) Å, Z = 1. Compound 2 crystallizes in the monoclinic, space group P2(1)/c, with a = 6.3466(5) Å, b = 24.008(2) Å, c = 9.0390(7) Å, α = 90°, β = 97.0050(10)°, γ = 90°, V = 1367.01(19) Å, Z = 4. Analysis of the crystal packing of 1, 2 suggests that there are N-H···O hydrogen bonds between the acids and the piperidine in both compounds. Except the classical hydrogen bonds, the secondary propagating interactions including CH···O, O···C, and CH···π interactions also play important roles in structure extension. In conclusion, we have shown that 3D structures can be constructed by collective non-covalent interactions. Graphical Abstract: The crystal structures of the salts from piperidine, naphthalene-1,5-disulfonic acid, and 4-nitrophthalic acid are predominantly stabilized by classical hydrogen bonds as well as CH···O, O···C, and CH···π interactions.[Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

Three aliphatic amine derived supramolecular complexes were synthesized and structurally characterized by X-ray crystallography. All these structures adopted the hetero supramolecular synthons. Compound 1 crystallizes in the monoclinic, space group C2/c, with a = 40.328(7) Å, b = 7.2054(14) Å, c = 7.6464(17) Å, α = 90º, β = 97.364(16)º, γ = 90º, V = 2203.6(8) Å, Z = 8. Compound 2 crystallizes in the monoclinic, space group P2(1)/n, with a = 7.4134(4) Å, b = 18.3749(14) Å, c = 12.1456(12) Å, α = 90º, β = 104.227(2)º, γ = 90º, V = 1603.7(2) Å, Z = 4. Compound 3 crystallizes in the monoclinic, space group P2(1)/c, with a = 9.8804(7) Å, b = 10.5061(8) Å, c = 11.8262(9) Å, α = 90º, β = 104.674(2)º, γ = 90º, V = 1187.57(15) Å, Z = 2. Analysis of the crystal packing of 1- 3 suggests that there are N-H···O hydrogen bonds between the acids and the aliphatic amines in all of the compounds. Except the classical hydrogen bonds, the secondary propagating interactions including CH···O, CH···O, CH···Cl, CH···π, and π···π interactions also play important roles in the structure extension. In conclusion, we have shown that 2D-3D structures can be constructed by the collective non-covalent interactions. Graphical Abstract: The crystal structures of the salts from aliphatic amines, (2,4-dichlorophenoxy)-acetic acid, 4-nitrophthalic acid, and 1,5-naphthalenedisulfonic acid are predominantly stabilized by the classical hydrogen bonds as well as CH···O, CH···O, CH···Cl, CH···π, and π···π interactions.[Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

The crystalline compounds quinolin-8-ol ( 1) and its two salts 2, and 3 have been prepared and structurally characterized. Compound 1 crystallizes in the triclinic, space group P-1, with a = 6.5775(5) Å, b = 7.8285(6) Å, c = 14.4617(13) Å, α = 96.099(2), β = 92.4700(10)°, γ = 106.171(3), V = 709.09(10) Å, Z = 4. Compound 1 is a new polymorph of quinolin-8-ol, and displays as dimer. Compound 2 crystallizes in the monoclinic, space group P2(1)/n, with a = 7.4815(11) Å, b = 18.844(3) Å, c = 8.0396(8) Å, β = 94.069(10), V = 1130.5(3) Å, Z = 4. Compound 3 crystallizes in the triclinic, space group P-1, with a = 7.0968(6) Å, b = 8.6854(7) Å, c = 11.0494(11) Å, α = 105.169(2), β = 90.3700(10)°, γ = 106.031(2), V = 629.50(10) Å, Z = 1. In the compound 3, the middle two COOH groups were ionized. In the compounds 2 and 3, as predicted on the basis of p Ka differences, proton transfer from the COOH group to the hetero-nitrogen of the quinolin-8-ol molecule occurs, resulting in the formation of the hydrogen or dihydrogen salts. In neither of the compounds ( 2 and 3) the primary cyclic hydrogen-bonded R(8) A-B heterodimer was formed, involving the second oxygen of the anion and the 8-hydroxy substituent of quinolin-8-ol. Instead, this molecule acts in a bridging mode to link the associated molecular units into chain polymers via combination of hydrogen bonds and other nonbonding interactions. The role of these non-covalent interactions in the crystal packing is analyzed. Under these weak interactions, compounds 2 and 3 displayed 3D framework structures. Graphical Abstract: The crystal structures of quinolin-8-ol and its two salts from acetylenedicarboxylic acid, and butane-1,2,3,4-tetracarboxylic acid display extensive classical hydrogen bonding as well as other non-covalent CH-O, CH-O, O-C, CH-C, and π···π interactions, giving 0/3D framework structures.[Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

Four salts benzylammonium (4-chloro-phenoxy)-acetate monhydrate ( 1), benzylammonium 3,5-dinitrosalicylate ( 2), benzylammonium 2,5-bis-benzylcarbamoyl-terephthalate ( 3), and benzylammonium 4-nitro-phthalate monohydrate ( 4) were obtained from self-assembly of the corresponding carboxylic acids with the benzylamine, and their structures were fully characterized. All four compounds are ionic, with proton transfer occurring to the NH of the benzylamine moiety. Compound 1 crystallizes in the Monoclinic, space group P2(1)/ n, with a = 6.7577(5) Å, b = 8.3490(7) Å, c = 28.658(2) Å, β = 95.765(2)°, V = 1608.7(2) Å, Z = 4. Compound 2 crystallizes in the Triclinic, space group P-1, with a = 9.7082(11) Å, b = 10.9970(11) Å, c = 15.9915(17) Å, α = 98.2230(10)°, β = 102.6500(10)°, γ = 114.105(2)°, V = 1467.9(3) Å, Z = 4. Compound 3 crystallizes in the Monoclinic, space group P2(1)/ c, with a = 15.8100(12) Å, b = 5.6638(3) Å, c = 20.1245(17) Å, β = 106.857(2)°, V = 1724.6(2) Å, Z = 2. Compound 4 crystallizes in the Monoclinic, space group Pc, with a = 17.3360(19) Å, b = 9.4133(8) Å, c = 14.5066(16) Å, β = 112.104(2)°, V = 2193.3(4) Å, Z = 4. Supramolecular architectures of the compounds 1- 4 involve O-H···O/N-H···O/N-H···N hydrogen bonds as well as other non-covalent associations. These salts displayed 2D-3D framework structures for the synergistic effect of the various non-covalent interactions. Graphical Abstract: The crystal structures of the benzylamine salts with (4-chloro-phenoxy)-acetic acid, 3,5-dinitrosalicylic acid, 2,5-bis-benzylcarbamoyl-terephthalic acid, and 4-nitro-phthalic acid show extensive hydrogen bonding as well as other noncovalent interactions, linking discrete components into higher-dimensional networks.[Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

Six salts, ([(H2L1)(ZnCl4)] (1) (L1 = 1,1′-bis(benzimidazolyl)methane), [(H2L1)(CuCl4)]·H2O (2), [(H2L2)(ZnCl4)] (3) (L2 = 1-(3-(1H-benzimidazol-1-yl)propyl)-1H-benzimidazole), [( H2L2)(CuCl4)] (4), [(H2L3)(CuCl4)]·H2O (5) (L3 = 1- (4-(1H-benzimidazol-1-yl)butyl)-1H-benzimidazole), and [(H2L4)(ZnCl4)]·H2O (6) (L4 = 3,6-bis(imidazol-1-yl)pyridazine)), derived from bis(benzimidazole)/bis(imidazole) and metal(II) chloride dihydrate (zinc(II) chloride and copper(II) chloride dihydrate) were prepared and characterized by IR, X-ray structure analysis, elemental analysis, and TG analysis. The aromatic rings of the cations in all of the compounds are planar. X-ray diffraction analysis revealed that all the complexes have 3-D layer network structures built from hydrogen bonds between the cations and chlorometallate anions. Water molecules also play an important role in structure extension in2,5,and6. The arrangements of the anions and cations in their solid state are dominated not only by size and symmetry of the cations, but also by the non-covalent interactions existing in the crystal structures. Due to the weak interactions, the compound displays 3-D layer structure. [ABSTRACT FROM AUTHOR]

Five imidazole/benzimidazole-based metal complexes, Cd(bim)2(L1)2 ( 1) [L1 = 2-methyl-2-phenoxypropionate, bim = benzimidazole], Zn(im)2(L2)2 ( 2) [L2 = 3-(4-methoxyphenyl)acrylate, im = imidazole], Zn(im)2(L3)2 ( 3) [L3 = 3,4-(methylenedioxy)benzoate], [Cd(im)2(L3)2]2 ·4H2O ( 4), and Cd(Bim)2(L4) ·CH3CH2OH ·H2O ( 5) (L4 = 1,4-cyclohexanedicarboxylate), were obtained by the introduction of the carboxylates as coligands and are structurally characterized by different techniques including elemental analysis, IR spectra, TG, and single-crystal X-ray diffraction analysis. The X-ray crystal structure analyses reveal that these complexes display mononuclear to dinuclear structures with tetrahedral coordination spheres around each central zinc atom, and octahedral coordination sphere around each central cadmium atom. The imidazole ligands in all compounds are coordinated only in a monodentate fashion with their neutral nitrogen groups. The carboxylates coordinate to the metal in monodentate, chelating bidentate, and bridging bidentate fashions. The N-H ···O hydrogen bonds from the NH donor of the neutral imidazole were found in all compounds. On the basis of X-ray crystallographic study the rich intra- and intermolecular noncovalent interactions (including classical hydrogen bonds, C-H ···O, CH2 ···O, CH3 ···O, CH2-N, C-H ···π, CH3-π, O-H ···π, and π-π interactions) are analyzed. The various nonbonding interactions in these compounds are responsible for different structures such as 3D network, 3D prismatic layer network, and 3D layer network structure. [ABSTRACT FROM AUTHOR]

Four zinc(II) complexes, namely, Zn(Hdmpz)2(L1)2 ( 1) (Hdmpz = 3, 5-dimethylpyrazole, HL1 = trichloroacetic acid), Zn(Hdmpz)2(L2)2 ( 2) (HL2 = 2, 4-dichlorophenoxyacetic acid), [Zn2(μ-dmpz)2(Hdmpz)2(L3)2] ( 3) (HL3 = 1-naphthylacetic acid), and [Zn(Hdmpz)2(L4)2] ·H2O ( 4) (HL4 = indole-3-acetic acid) were prepared and structurally characterized by different techniques including elemental analysis, IR spectroscopy, TG, and single-crystal X-ray diffraction analysis. The complexes display 2D to 3D structures with tetrahedral to pentagonal coordination around the central zinc atom. The X-ray studies suggested that 1, 2, and 4 are mononuclear complexes, whereas 3 is a centrosymmetric dinuclear complex. The pyrazole ligand is coordinated in both terminal as well as a bridging fashion in the dinuclear moiety but the pyrazole ligand in the mononuclear complexes is coordinated only in monodentate terminal fashion with its neutral N group. The carboxylate groups behave as monodentate ligands in 1- 3, whereas the carboxylate in 4 functioned as both monodentate and chelating bidentate ligand. On the basis of X-ray crystallographic study the rich intra- and intermolecular weak interactions such as classical hydrogen bonds, C-H ···O, CH3 ···O, CH-Cl, Cl-Cl, C-H ···π, CH2-π, CH3-π, O-π, and π-π are analyzed. All these noncovalent interactions help to assemble the discrete complexes into high-dimensional ordered superamolecular structures. [ABSTRACT FROM AUTHOR]

Highlights: [•] Eight organic acid–base adducts with 3D structure have been prepared and structurally characterized. [•] The classical hydrogen bonds in the eight supramolecules containing the OH⋯bzim synthons have been discussed. [•] The secondary interactions in the solid-state packing of the final structure have also been discussed. [Copyright &y& Elsevier]

Highlights: [•] Six mixed-ligand complexes were prepared and characterized. [•] These complexes display mononuclear to trinuclear structures. [•] The pyrazole is coordinated only in monodentate fashion with its neutral N group. [•] There exist intramolecular N–H⋯O hydrogen bonds from the NH of the pyrazole. [Copyright &y& Elsevier]

Four compounds, [(HL) · (cba)·2HO] ( 1, cba = o-chlorobenzoate), [(HL)·(NSA)] ( 2, NSA = 5-nitrosalicylate), [(HL)·(3,5-dns)] ( 3, 3,5-dns = 3,5-dinitrosalicylate), and [(HL)·(nda)] ( 4, nda = 1,5-naphthalenedisulfonate) were obtained from self-assembly of the corresponding acids with the cyclohexylamine, and their structures were fully characterized. All four compounds are organic salts, with proton transfer occurring to the NH of the cyclohexylamine moiety. All structures adopted hetero supramolecular synthons. Compound 1 crystallizes in the triclinic, space group P-1, with a = 10.151(3) Å, b = 13.160(4) Å, c = 17.172(5) Å, α = 72.159(4)°, β = 79.546(4)°, γ = 78.285(4)°, V = 2120.5(11) Å, Z = 2. Compound 2 crystallizes in the monoclinic, space group P2(1)/c, with a = 13.501(2) Å, b = 6.3144(15) Å, c = 19.601(3) Å, β = 123.900(13)°, V = 1386.9(4) Å, Z = 4. Compound 3 crystallizes in the monoclinic, space group P2(1)/n, with a = 14.6439(11) Å, b = 6.9231(4) Å, c = 21.3012(18) Å, β = 96.4800(10)°, V = 2145.7(3) Å, Z = 4. Compound 4 crystallizes in the monoclinic, space group P2(1)/n, with a = 5.3477(5) Å, b = 19.9238(16) Å, c = 11.1761(9) Å, β = 95.7230(10)°, V = 1184.84(17) Å, Z = 2. Analysis of the crystal packing of 1- 4 displays that there are extensive N-H···O hydrogen bonds between the acids and the cyclohexylamine in all of the salts. Except the classical hydrogen bonding interactions, the secondary propagating interactions also play significant roles in structure extension. The four salts displayed 2D/3D framework structures for the synergistic effect of the various noncovalent interactions. Graphical Abstract: The crystal structures of the cyclohexylamine salts with o-chlorobenzoic acid, 5-nitrosalicylic acid, 3,5-dinitrosalicylic acid, and 1,5-naphthalenedisulfonic acid show extensive classical hydrogen bonding as well as C-H···O, CH···O, Cl···O, NH···π, CH···π, and π···π interactions, giving 2D sheets or 3D networks.[Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

Three compounds (benzylamine): (2,4,6-trinitrophenol) ( 1) [(HL)·(pic), pic = picrate], (benzylamine): (3,5-dinitrobenzoic acid) ( 2) [(HL)·(dna), dna = 3,5-dinitrobenzoate], and (benzylamine): (oxalic acid): HO ( 3) [(HL)·(Hoxa)·HO, Hoxa = hydrogenoxalate] were obtained from self-assembly of the corresponding acidic components with the benzylamine, and their structures were fully characterized. All three compounds are ionic, with proton transfer occurring to the NH of the benzylamine moiety. These structures adopted homo or hetero supramolecular synthons or both. Compound 1 crystallizes in the triclinic, space group P− 1, with a = 7.9195(8) Å, b = 9.7316(9) Å, c = 10.7905(11) Å, α = 108.300(2), β = 109.386(2)°, γ = 94.3360(10), V = 729.62(12) Å, Z = 2. Compound 2 crystallizes in the monoclinic, space group P2( 1), with a = 10.8635(11) Å, b = 6.2690(7) Å, c = 11.5810(14) Å, β = 106.9180(10)°, V = 754.57(15) Å, Z = 2. Compound 3 crystallizes in the monoclinic, space group C2/ c, with a = 22.011(2) Å, b = 5.6418(2) Å, c = 16.5081(13) Å, β = 97.1680(10)°, V = 2,034.0(3) Å, Z = 4. Supramolecular architectures of the compounds 1- 3 involve O-H···O/N-H···O hydrogen bonds as well as other noncovalent associations. The role of these noncovalent interactions in the crystal packing is analysed. These salts displayed 3D framework structure for the synergistic effect of the various noncovalent interactions. Graphical Abstract: Due to the weak interactions, the compound displays 3D framework structure. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

Five organic-inorganic hybrid complexes [(HL1)2(CdCl4)] · H2O (1), (L1 = 2-methylquinoline); [(HL1)2(CoCl4)] · H2O (2), [(HL2)2(CuCl4)] (3), (L2 = 6-bromobenzo[d]thiazol-2-amine), [(HL3)2(ZnCl4)] · 2H2O, (4), (L3 = 5,7-dimethyl-1,8-naphthyri- dine-2-amine), and [(H2L4)(Cu2Cl8)0.5], and (5) (L4 = 3,6-bis(imidazol-1-yl)pyridazine) derived from N-containing aromatic Brønsted bases and metal(II) chloride (cadmium(II) chloride dihydrate, cobalt(II) chloride hexahydrate, copper(II) chloride dihydrate, and zinc(II) chloride) were prepared and characterized by IR, X-ray structure analysis, elemental analysis, and TG analysis. The aromatic rings of the cations in all of the compounds are essentially planar. On the structural level, the atomic arrangement of the title hybrid crystals can be described as built up by the perchlorometallates of Cd2+, Co2+, Cu2+,andZn2+associated to the organic cations through the multiple noncovalent associations. X-ray diffraction analysis revealed that complexes 1, 2, 4, and 5 have 3D network structures built from hydrogen bonds between the cations and chlorometallate anions, while 3 displays 2D doublesheet structure. The water molecules also played important role in structure extension in compounds 1, 2, and 4. The arrangements of the anions and cations in their solid state are dominated not only by the shape, size, and symmetry of the cations, but also by the different structure type of the chlorometallate anions as well as the hydrogen-bonded interactions existing in the crystal structures. [ABSTRACT FROM AUTHOR]

Abstract: Studies concentrating on hydrogen bonding between the base of 2-aminophenol, 2-amino-4-chlorophenol, and acidic compounds have led to an increased understanding of the role 2-aminophenol, and 2-amino-4-chlorophenol have in binding with acidic compounds. Here anhydrous and hydrated multicomponent crystals of 2-aminophenol, and 2-amino-4-chlorophenol have been prepared with 2,4,6-trinitrophenol, p-nitrobenzoic acid, 3,5-dinitrobenzoic acid, 5-nitrosalicylic acid, 3,5-dinitrosalicylic acid, and fumaric acid. The crystals and complexes of the seven organic acid–base adducts were characterized by X-ray diffraction analysis, IR, mp, and elemental analysis. The seven crystalline forms reported are organic salts except 2. All of the adducts were formed in solution and obtained by the slow evaporation technique. All supramolecular architectures involve extensive NO, OO, and CH⋯O hydrogen bonds as well as other nonbonding interactions. The role of weak and strong hydrogen bonding in the crystal packing is ascertained. [Copyright &y& Elsevier]

Four organic–inorganic crystals, [(HL1)2(ZnCl4)]·H2O (1) (L1 = 2-methylquinoline), [(HL1)2(CuCl4)] (2), [(HL2)2SnCl6] (3) (L2 = 6-bromobenzo[d]thiazol-2-amine), and [(HL3)FeCl4] (4) (L3 = 5,7-dimethyl-1,8-naphthyridine-2-amine), derived from N-containing aromatic Brønsted bases and metal(II) chlorides (zinc(II) chloride, copper(II) chloride dihydrate, tin(II) chloride dihydrate, and iron(III) chloride hexahydrate) were prepared at room temperature and characterized by IR, X-ray structure analysis, elemental analysis, and TG analysis. The crystals are built up by perchlorometallates (Zn, Cu, Sn, and Fe) associated with organic cations through multiple non-covalent associations. X-ray diffraction analysis reveals that 1 and 2 have 3-D network structures built from hydrogen bonds between the cations and chlorometallates. Water molecules play an important role in structure extension in 1. Anhydrous 3 and 4 produced from 2-aminoheterocyclic derivatives display 2-D sheet structures. Arrangements of anions and cations are dominated by shape and size of cations, and also by the different structures of the chlorometallates as well as non-bonding interactions in the crystal structures. Except for 1, the other compounds are thermally stable below 240°C. [ABSTRACT FROM PUBLISHER]

Abstract: Studies concentrating on noncovalent weak interactions between the organic base of 2-methylquinoline, and carboxylic acid derivatives have led to an increased understanding of the role 2-methylquinoline has in binding with carboxylic acid derivatives. Here anhydrous and hydrous multicomponent organic acid–base adducts of 2-methylquinoline have been prepared with carboxylic acids that ranged from monocarboxylic acid to tricarboxylic acid such as 3,5-dinitrobenzoic acid, 3-hydroxy-2-naphthoic acid, oxalic acid, fumaric acid, and citric acid. The five crystalline complexes were characterized by X-ray diffraction analysis, IR, mp, and elemental analysis. These structures adopted homo or heterosupramolecular synthons or both. Analysis of the crystal packing of 1–5 suggests that there are NO, ON, and OO hydrogen bonds (charge assisted or neutral) between acid and base components in the studied compounds. Except the classical hydrogen bonding interactions, the secondary propagating interactions also play an important role in structure extension. These weak interactions are responsible for the formation of 1D–3D frameworks. [Copyright &y& Elsevier]

Four organic–inorganic hybrid complexes ([(HL1)2SnCl6] · 2H2O (1) (L1 = 2-methylquinoline), [(HL2)2(CdCl4)] · 2H2O (2) (L2 = 5,7-dimethyl-1,8-naphthyridine-2-amine), [(H2L2)2SnCl6] · 2(Cl) (3), and [(H2L3)SnCl6] · 2H2O (4) (L3 = 3,6-bis(imidazol-1-yl)pyridazine)) derived from N-containing aromatic Brønsted bases and metal(II) chloride dihydrate (tin(II) chloride dihydrate and cadmium(II) chloride dihydrate) were prepared and characterized by IR, X-ray structure analysis, elemental analysis, and TG analysis. The aromatic rings of the cations in all of the compounds are essentially planar. X-ray diffraction analysis revealed that 2–4 have 3-D network structures built from hydrogen bonds between the cations and chlorometallates. Water molecules also play important roles in structure extension in 1, 2, and 4. The arrangements of the anions and cations in their solid state are dominated by shape, size, and symmetry of the cations and the different structures of the chlorometallates as well as by hydrogen-bond interactions. [ABSTRACT FROM AUTHOR]

Six organic-inorganic complexes derived from bis-imidazole derivatives ([(H2L1)(CdCl3 ⋅ H2O)2] (1), L1 = 1-(3-(1H-benzimidazol-1-yl)propyl)-1H-benzimidazole; [(H2L2)CdCl4] (2), L2 = 1,1'-bis(benzimidazolyl)methane; [(H2L3)CdCl4] (3), L3 = 1-(2-(1H-benzimidazol-1-yl)ethyl)-1H-benzimidazole; [(H2L4)4(CdCl4)4] ⋅ 13H2O (4), L4 = 1,5-bis(1-benzimidazolyl)-3-oxapentane; [(H2L5)CdCl4] (5), L5 = 1-(4-(1H-benzimidazol-1-yl)butyl)-1H-benzimidazole; [(H2L6)(Cd2Cl8)0.5] ⋅ H2O (6), L6 = 3,6-bis(imidazol-1-yl)pyridazine), and cadmium(II) chloride dihydrate were prepared and characterized by IR, X-ray structure analysis, elemental analysis, and TG analysis. The imidazolyl moieties in all six compounds are essentially planar. X-ray diffraction analysis revealed that complexes 1-6 have 3-D network structures built from hydrogen bonds between imidazolium cations, chlorocadmate anions, and water. The arrangements of the anions and cations in their solid state are dominated not only by the size and symmetry of the imidazolium cations, but also by the different structure types of the chlorocadmate anions as well as the hydrogen-bonded interactions existing in the crystal structures. All of the complexes are thermally stable. [ABSTRACT FROM AUTHOR]

In this work, [Cu3I2(PPh3)6(L1)2]∙2DMSO∙Cl2 ( 1) (L1 = bis( N-imidazolyl)methane) complex was synthesized by solvothermal method. The crystal and complexes were characterized by X-ray diffraction (XRD) analysis, Fourier Transform infrared (FTIR) spectroscopy, elemental analysis and photoluminescence (PL) measurements. XRD and FTIR analysis indicated that the complex 1 is a trinuclear compound, in the compound there are two kinds of copper atoms, i.e. monovalent, and divalent copper cations. For the copper(I) center, it is surrounded by two P, one N, and one iodide atoms to complete its tetrahedron geometry. While the copper(II) center is surrounded by two P and two nitrogen atoms, the chloride anions existed as free counter anions. The copper(II) atom and the copper(I) atoms were bridged by exobidentate L1 ligand. The PL spectrum showed that the complex displays intense blue emission related to shallow holes. [ABSTRACT FROM AUTHOR]

Abstract: [Cu2Br2L1(PPh3)4]2 · 2CH2Cl2 · 3H2O (1) (L1 =bis(N-imidazolyl)butane) and [Cu3I2(PPh3)6(L2)2] · 2DMSO · Br · H2O (2) (L2 =bis(N-imidazolyl)methane) have been synthesized and characterized by X-ray diffraction analysis and elemental analysis. Compound 1 is a tetracoordinated dinuclear complex, it consists of two Cu(PPh3)2 units bridged by a bis(N-imidazolyl)butane ligand. While compound 2 is a trinuclear copper(I) complex, in the compound copper atoms are located in two kinds of coordination spheres, for the two terminal copper(I) atoms, they are surrounded by two P, one N, and one iodine atoms to complete their tetrahedron geometry. While the middle copper(I) atom is surrounded by two P and two nitrogen atoms, the bromide anion exists as free counter anion. The photoluminescent studies show that the two complexes display intense blue emissions. [Copyright &y& Elsevier]

Six bismuth(III) complexes containing dithio-ligands formulated as (R2NCS2)3Bi [R2NCS2M = Me2NCS2Na, C4H8NCS2Na, Bz2NCS2Na] and [(R2NCS2)2BiI]2 [R2NCS2M = C5H10NCS2Na, nBu2NCS2Na, OC4H8NCS2Na] have been obtained by reactions of bismuth(III) halides with dithiocarbamate ligands in 1 : 2 or 1 : 3 stoichiometry. All compounds were characterized by elemental and IR analyses. The crystal structures of complexes 1 and 4 have been determined by X-ray single crystal diffraction. The structure analyses reveal that BiIII in complex 1 adopts a distorted pentagonal-pyramidal coordination, due to its stereochemically active lone pair of electrons. A long Bi · S contact of 3.218 (3) Å leads to dimeric associations of molecules in the crystal structure. The structure of complex 4 is six-coordination with a distorted octahedral configuration. Intramolecular S · S weak interactions contribute to the stability and lead to a one-dimensional chain structure. [ABSTRACT FROM AUTHOR]

Six diorganotin esters of Schiff-base ligands formulated as [R 2 SnLY] 2 , where L 1 is C 6 H 5 CON 2 C(CH 3 )CO 2 with Y  =  CH 3 CH 2 OH, R  =   m ClC 6 H 4 CH 2 ( 1 ), o FC 6 H 4 CH 2 ( 2 ), p FC 6 H 4 CH 2 ( 3 ) and L 2 is 2-HOC 6 H 4 CON 2 C(CH 3 )CO 2 with Y  =  CH 3 OH, R  =   o FC 6 H 4 CH 2 ( 4 ), p FC 6 H 4 CH 2 ( 5 ), m ClC 6 H 4 CH 2 ( 6 ) have been prepared and characterized by elemental analysis, IR, 1 H and 119 Sn NMR spectra. The crystal structures of complexes 1 and 4 have been determined by X-ray single crystal diffraction. The structure analyses reveal that the Sn atom in both 1 and 4 is seven-coordinate in distorted pentagonal bipyramid geometries with a planar SnO 4 N unit and two apical aryl carbon atoms, thus forming a dimeric molecule, which sits on a crystallographic center of symmetry. Intramolecular or intradimeric hydrogen bonds contribute to the stability and compactness of the crystal structures. [ABSTRACT FROM AUTHOR]

The reaction of [NiCl 2 (PPh 3 ) 2 ] with in i PrOH under solvothermal conditions gives a nickeladodecaborane cluster: H 2 [Cl 2 NiB 11 H 6 -2,3,4,5,6-(O i Pr) 5 ] which was characterized by FT-IR, NMR spectroscopy and elemental analysis. It was also characterized by an X-ray diffraction study of a single crystal. The title cluster belongs to monoclinic, space group P 2(1)/ n , with crystal cell parameters: a   =  12.355(13)  Å, b   =  18.471(19)  Å, c   =  12.956(14)  Å, β  =  93.524(18)°, Z   =  4, D Calcd   =  1.242  Mg  m -3 , F (000)  =  1160, R 1   =  0.0746, wR 2   =  0.1829. The cluster has a closo 12-vertex {NiB 11 } icosahedral skeleton, in which Ni connects with two Cl atoms and five B atoms. O i Pr groups substituted all five H atoms on the boron cage atoms adjacent to Ni. [ABSTRACT FROM AUTHOR]

A novel compound (NH4)2Y(H2O)8[PMo10V2O40]·10H2O has been prepared in an aqueous solution and characterized by elemental analysis, IR, and TG-DTG analysis. X-ray diffraction analysis was carried out on (NH4)2Y(H2O)8 [PMo10V2O40]·10H2O single crystal, which crystallizes in the monoclinic system of a space group P21/c with a=0. 9871 (3) nm, b=1. 5424 (5) nm, c=2.7924(9) nm, β = 94.183(5)° and Z=2. In the compound, a two-dimensional network is constructed by the PMo10V2O anion and the Y(H2O) cation building blocks via hydrogen bonding exhibiting the porous structure. [ABSTRACT FROM AUTHOR]

The heteropolytungstate (NH4)20[Na2(H2O)2Ni(H2O)5{Ni(H2O)}2As4W40O140] · 61H2O is obtained by the reaction of Na27[NaAs4W40O140] · 60H2O with NiCl2 · 6H2O and NH4Cl in pH≈4.0. The structure and chemical composition are determined by X-ray diffraction analysis and element analysis. The crystal data and main structure refinement are: a = 1.33135(18) nm, b = 1.9722(3) nm, c = 3.6430(5) nm, α = 78.010(2)°, β = 82.145(2)δ, γ = 74.385(2)°, V = 8.978(2) nm3, triclinic crystal system, space group: P1, Z = 2, R1 = 0.0512, and wR2 = 0.0684(I >2σ). The four S2 sites of the big cyclic ligand [As4W40O140]28- are occupied by two Na+ and two Ni2+ respectively, and each site supplies four Od coordinating to metal ion. The coordination number of Ni2+ is six, and that of two Na+ is five and six respectively. The third Ni2+ locates outside the cyclic [As4W40O140]28- and connects with one Od, and its coordination number is six. [ABSTRACT FROM AUTHOR]

C10H5N5O5, monoclinic, P21/c (no. 14), a = 10.9546(11) Å, b = 7.3433(8) Å, c = 13.2567(15) Å, β = 102.972 (5) ∘ , V = 1039.19(19) Å3, Z = 4, R g t (F) = 0.0630, w R r e f (F2) = 0.1622, T = 298 K. [ABSTRACT FROM AUTHOR]