The hydrogen bonding in 2-amino-3-cyano-4-(3-nitrophenyl)-4,6-dihydro-5H-pyrano[3,2-c]quinolin-5-one N,N-dimethylformamide solvate monohydrate

The crystal structure of 2-amino-3-cyano-4,6-dihydro-4-(3-nitrophenyl)-5H-pyrano[3,2-c]quinolin-5-one N,N-dimethylformamide solvate monohydrate is determined by room temperature X-ray diffraction. The title compound 1, C₂₂H₂₁N₅O₆, is triclinic, space group P-1, a=9.109(2) ?, b=11.340(2) ?, c=12.485(2) ?, α=70.02(1)°, β=69.36(1)°, γ=67.32(1)°, Z=2, V=1081.4(4) ?³. It is interesting that a bridge-like hydrogen bond O–H···O is formed between the title compound and solvent molecules of water with molecular ratio of 2:2 building a bi-layer framework. In addition, there are two other types of classical hydrogen bonds N–H···N and N–H···O in the crystal structure.Supplementary material Crystallographic data for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CCDC-275001. Copies of available material can be obtained, free of charge, on application to the Director, CCDC, 12 Union Road, Cambridge CB2 1EZ, UK, (fax: +44-(0) 1223–336033 or e-mail: deposit@ccdc.cam.ac.uk).     

Hydrogen bonding patterns in bis(pyrimethamine hydrogen sulfate) monohydrate

The crystal structure of the compound bis [2,4-diamino-5-(p-chlorophenyl)-6-ethyl pyrimidinium hydrogen sulfate] monohydrate was studied by X-ray diffraction methods. The compound crystallises in orthorhombic system, space group P2₁2₁2₁, a=18.531(2) ?, b=16.190(2) ?, c=10.777(2) ?, V=3233.3(8), Z=4. The asymmetric unit shows the presence of two crystallographically independent pyrimethamine molecules, two hydrogen sulfate anions, and a water molecule. The hydrogen sulfate anions form a cyclic hydrogen bonded motif R₂ ²(8) with the 2-amino pyrimidine of the respective protonated pyrimethamine cations, through N–H···O hydrogen bonds. Thus the sulfate anions mimic the role of carboxylate anions observed in many aminopyrimidine-carboxylate interactions. This motif self assembles through DDAA array of quadruple hydrogen bonds, N–H···Cl, O–H···O and C–H···O hydrogen bonds.Supplementary material CCDC-293607 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at www.ccdc.cam.ac.uk/conts/retrieving.html [or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 IEZ, UK; fax: C44 (0) 1223-336033; e-mail: deposit@ccdc.cam.ac.uk].     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

Crystal and molecular structure of the β-anomer of 6,7-dideoxy-1,2;3,4;9,10-tris-O-(1-methylethylidene)- d-erythro-α-d-galacto-undecopyranosid-8-ulose

6,7-dideoxy-1,2;3,4;9,10-tris-O-(1-methylethylidene)-d-erythro-α-d-galacto-undecopy- ranosid-8-ulose, 3, was formed by adding a D-galactose-derived dithiane nucleophile to a protected erythronolactone followed by reductive removal of the dithioacetal group. Its β-anomer crystallizes in the chiral trigonal space group P3₂21 with a=b=12.2649(19) Å, c=24.675(8) Å, and Z=6. The molecule is composed of an erythrofuranose and a galactopyranose moiety, linked by a flexible ethylene bridge. The pyranose part of the molecule is disordered over two positions with equal occupancy. The configuration of the two disordered moieties is the same and they are converted into each other by a slight rotation of 6 degrees around one of the C–C single bonds of the ethylene bridge. The disorder allows for a more effective packing in the solid state.Supplementary material CCDC-602051 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, by e-mailing data_request@ccdc.cam.ac.uk or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033.     

Synthesis and crystal structure of 3-[2-oxo-2-(4-methyloxyphenylsulfonamidophenyl)ethylidene]-3,4-dihydro-1H-quinoxalin-2-one

3-[2-Oxo-2-(4-methyloxyphenylsulfonamidophenyl)ethylidene]-3,4-dihydro-1H-quinox-alin-2-one (4) was synthesized and characterized by ¹H NMR,¹³C NMR, IR, and single-crystal X-ray diffraction techniques. The crystallographic results show that the composition of the title compound is C₂₃H₁₉N₃O₅S. It belongs to triclinic crystal system and P-1 space group, with a=7.273(6) ?, b=9.092(7) ?, c=15.928(13) ?; α=85.135(11)°, β=78.297(10)°, γ=84.619(11)°, V=1024.4(14) ?³, Z=2, D _c=1.457 mg/m³, μ = 0.201 mm⁻¹, F(000)=468, R=0.0597, wR=0.1438. Supplementary material CCDC-281953 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at www.ccdc.cam.ac.uk/retrieving.html or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44-1223-336033; e-mail: deposit@ccdc.cam.ac.uk.     

Synthesis and structure determination of 7a-Aza-B-homostigmast-5-eno [7a, 7-d] tetrazole-3β-yl chloride (C29H47N4Cl)

7a-Aza-B-homostigmast-5-eno [7a, 7-d] tetrazole-3β-yl chloride (C₂₉H₄₇N₄Cl) was synthesized for its crystallographic analysis and to investigate the role of intra- and intermolecular interactions in steroids. It crystallizes in the monoclinic space group C2 with unit cell parameters: a = 38.481(2), b = 6.661(3), c = 11.111 (6) ?, β = 94.49 (4)^o; λ( MoKα) = 0.71069 ?, V = 2839(2) ?³, and Z = 4. The structure has been solved by direct methods using X-ray diffraction techniques. The final reliability index for the computed structure is 0.0597 for 1252 observed reflections. Except the five-membered ring, all other rings of the steroid nucleus exist in non-planar conformations. The structure is stabilized by C–H···N intermolecular interaction.Supplementary material CCDC-267926 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at www.ccdc.cam.an.uk/uk/conts/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, United Kingdom; Fax: $+$44(0) 1223-336033; e-mail: deposit@ccdc.cam.ac.uk.     

Crystallographic and conformational analysis of 1,3-bis(2,4-dimethoxyphenyl)imidazolidine-2-thione

The molecular and crystal structures of the title compound, C₁₉H₂₂N₂O₄S, were determined by single crystal X-ray diffraction technique. The title compound crystallizes in space group F d d 2, with a = 30.785(3) ?, b = 10.6455(9) ?, c = 11.0036(8) ?, Z = 8, D _calc = 1.379(2) g cm⁻³, μ(Mo-K_α) = 0.207 mm⁻¹, and its crystal system is orthorhombic. The structure was solved by direct methods and refined to a final R = 0.042 for 1530 reflections with I > 2σ (I). There is a half-independent molecule in the asymmetric unit. The title molecule has twofold rotational symmetry along with the C–S bond. Classically no hydrogen bond is found in the crystal structure. The crystal structure is stabilized by π–π stacking and edge to face (C–H…π-ring) interactions. To elucidate conformational features and steric hindrances of the title molecule, selected torsion angle is varied from −180° to +180° in every 10° and thus molecular energy profile is calculated by PM3 semi-empirical method.Supplementary materials CCDC 261789 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, by emailing data_request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge CB2 1EZ, UK; fax: $+$44 1223 336033.     

Br···HN, N···HC, Br···HC, and Br···Br intermolecular interactions as supramolecular synthons: Synthesis and crystal structure of bis(2-amino-5-methylpyridinium) tetrabromomercurate(II)

The bis(2-amino-5-methylpyridinium) tetrabromomercurate(II) (C₆H₉N₂)₂[HgBr₄] salt is triclinic, P1, with the following cell parameters: a=8.060(8) ?, b=9.035(9) ?, c=14.964(10) ?, α=96.032(19)°, β=90.317(15)°, γ=113.32(2)°, V=993.8(15) ?³, with Z=2 formula units. The crystal structure consists of alternating stacks of inorganic HgBr₄ ²⁻ anions and organic layers of 2-amino-5-methylpyridinium cations parallel to c-axis. The cohesion forces that connect molecules in the organic layers are N···HC hydrogen bonding and π–π stacking. The HgBr₄ ²⁻ units in the inorganic stacks are attracted via Br···Br intermolecular interactions.Supplementary material CCDC 270395 contains the supplementary crystallographic data. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, or by e-mailing at data_request@ccdc.cam.ac.uk, or by contacting the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: + 44(0)1223-336033.     

Synthesis, characterization and crystal structure of a mononuclear zinc(II) complex derived from 2-methoxy- 6-[(3-cyclohexylaminopropylimino)methyl]phenol

Colourless block-shaped crystals of Dichloro{2-methoxy-6-[(3-cyclohexylaminopropy-limino)methyl]phenolato}zinc(II) methanol, [Zn(C₁₇H₂₆N₂O₂)Cl₂].CH₃OH, have been obtained and characterized by elemental analysis, IR and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a=12.980(3) ?, b=13.139(3) ?, c=13.277(3) ?, β=107.00(3)°, V=2165.4(8) ?³, Z=4, R ₁=0.0631 and wR2=0.1110. X-ray structure determination revealed that the complex consists of a [Zn(C₁₇H₂₆N₂O)Cl₂] moiety and a lattice MeOH molecule. In the crystal structure, molecules are linked through intermolecular N–HO, C–HCl and O–HCl hydrogen bonds, forming chains. It is the first complex derived from the Schiff base ligand 2-methoxy-6-[(3-cyclohexylaminopropylimino)methyl]phenol.Supplementary materialCCDC-606067 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam.ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Synthesis,characterization and crystal structure of a mononuclear iron(III) complex derived from 4-bromo-2-[(pyridin-2-ylmethylimino)methyl]phenol

A nitrate salt of bis[4-bromo-2-(pyridin-2-ylmethyliminomethyl)phenolato]iron(III), [Fe(C₁₃H₁₀BrN₂O)₂].NO₃, has been obtained and characterized by elemental analysis and X-ray single crystal determination. The complex crystallizes in the tetragonal space group P4₂/n with unit cell dimensions a = b = 17.608(3) ?, c = 17.199(3) ?, V = 5332.4(15) ?³, Z = 8, R ₁ = 0.0444 and wR2 = 0.0902. The complex consists of a [Fe(C₁₃H₁₀BrN₂O)₂]⁺ cation and a nitrate anion. The Fe atom in the cation is six-coordinated in an octahedral geometry. In the crystal structure, molecules are linked through weak C–H⋯O intermolecular hydrogen bonds, forming chains running along the c axis. Supplementary material CCDC-607149 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam.ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Intermolecular interactions involved in the crystal structure of 2-amino-5-methylpyridinium hexabromostannate (IV), (C<Subscript>6</Subscript>H<Subscript>9</Subscript>N<Subscript>2</Subscript>)<Subscript>2</Subscript>[SnBr<Subscript>6</Subscript>]

The salt bis(2-amino-5-methylpyridinium) hexabromostannate(IV) (C₆H₉N₂)₂[SnBr₆] is monoclinic, P2 ₁ /c, with the following cell parameters: a=9.1636(18) ?, b=28.767(7) ?, c=16.956(17) ?, β=101.008(5)°, V=4387.5(17) ?³, Z=8, formula units. X-ray crystallography revealed that the structure can be regarded as a semi-regular three-dimensional array of anions, with pairs of cations forming layers perpendicular to b axis in the cavities between the anions. The cohesion forces that connects molecules in the organic layers are hydrophilic N⋯HCH₂ and HN⋯HN hydrogen bonding as well as hydrophobic π-π stacking and CH₃⋯π interactions. Cations and anions are connected via strong Br⋯H hydrogen bonding. Supplementary material CCDC 276493 contains the supplementary crystallographic data. These data can be obtained free of charge via www.ccdc. cam.ac.uk/data_request/cif, by e-mailing data_ request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033.     

Reaction of 1,2-bis(2,6-dicarboxypyridin-4-yl)ethyne with Co(II) generates coordination monomers not polymers: Crystal structure of 4-(2,6-dicarboxypyridin-4-yl)ethynylpyridine-2,6-dicarboxylatotriaqua cobalt(II) monohydrate

Reaction and crystallization of 1,2-bis(2,6-dicarboxypyridin-4-yl)ethyne with Co(II) produces crystals containing monomers of 4-(2,6-dicarboxypyridin-4-yl)ethynylpyridine-2,6-dicarboxylatotriaqua cobalt(II) monohydrate complex (1), [Co(C₁₆H₆N₂O₈)(H₂O)₃]·H₂O, instead of a rigid 1-D metal–organic framework consisting of a linear coordination polymer. This complex crystallizes in the monoclinic space group C2/c with a=6.8028(9) ?, b=36.781(5) ?, c=7.5135(9) 2.474(2)° and Z=4. The complex sits on a symmetry axis such that the two halves of the molecule are related by two-fold rotation symmetry. The molecules form layers in which the molecules are joined by intermolecular O–H⋯O interactions involving hydrogen bonds between CO₂H⋯CO₂ ⁻, H₂O⋯CO₂ ⁻, H₂O⋯CO₂H and H₂O⋯H₂O groups.Supplementary material CCDC-289569 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data request/cif, by e-mailing data request@ccdc.cam.ac.uk or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 IEZ, UK; fax: +44(0)1223-336033.     

A ladder type structure: Rubidium diphenylacetate diphenylacetic acid

A new rubidium complex, rubidium diphenylacetate diphenylacetic acid has been synthesised and characterised by single-crystal X-ray diffraction: triclinic, P with a=7.437(3) ?, b=12.377(4) ?, c=14.384(3) ?, α=107.08(2)°, β=103.67(2)°, γ=96.95(3)°, Mr=508.93, V=1203.6(6) ?³, Z=2. The diphenylacetic molecules bridge the metallic ions forming an infinite ladder structure. Two strong hydrogen bonds link the organic moieties. Supplementary materials Crystallographic data for structural analysis have been deposited with the Cambridge Crystallographic Data Center, CCDC No. 602647. Copies of this information may be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: +44 1223 336 033; e-mail: deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk).     

Synthesis and crystal structure of a copper coordination polymer [(Cu(btapo)2BrCH3OH)+Br−]n (btapo=1,3-bis(benzotriazol-1-yl) propan-2-ol)

A new coordination polymer [(Cu(btapo)₂BrCH₃OH)⁺Br⁻]_n (btapo = 1,3-bis(benzotria- zol-1-yl) propan-2-ol) was synthesized by the reaction of CuBr₂ and btapo, a new ligand synthesized in our laboratory, in THF. Its structure was determined by single-crystal X-ray crystallography. It crystallizes in tetragonal I4(1)/a space group with the crystal cell parameters of a=11.987(9) ?, c=54.24(4) ?, V=7794(10) ?³, and Z=8. The crystal X-ray analysis shows that each copper atom is five-coordinated with a bromine atom and four nitrogen atoms from four ligands to form a slightly distorted square pyramid. Each ligand bridges two copper atoms to form a two-strand helical chain. The chains are further extended to a three-dimensional network by the hydrogen bonds between the hydroxyl groups and the bromine anions. Supplementary material Crystallographic data for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Center as supplementary publication no. CCDC 600471. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (Fax;(+44) 1223–336-033; e-mail: deposit@ccdc.cam.ac.uk).     

Synthesis,Characterization and Antibacterial Activity of <Emphasis Type="Italic">N</Emphasis>-(2,3,4-Trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine

Abstract  The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C₁₈H₂₁NO₃, M _r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2₁/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) ?, β = 92.056(2)°, V = 1,632.4(3) ?³, Z = 4, D _c = 1.218 g cm⁻³, λ = 0.71073 ?, μ(Mo Kα) = 0.083 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0497, wR(F ²) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity. Graphical Abstract  The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C₁₈H₂₁NO₃, M _r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2₁/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) ?, β = 92.056(2)°, V = 1,632.4(3) ?³, Z = 4, D _c = 1.218 g cm⁻³, λ = 0.71073 ?, μ(Mo Kα) = 0.083 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0497, wR(F ²) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity.      

A novel stable CuI complex based on an unconjugated bisanthryl-tethered diimine ligand with tri-coordinate mode

The first air-stable mononuclear Cu^I complex (1) based on an unconjugated bisanthryl-tethered diimine ligand has been synthesized and characterized by elemental analysis, ESI-MS, UV-vis, FT-IR spectra and TGA analysis. X-ray diffraction analysis at room temperature reveals that complex 1 crystallizes in a monoclinic system, space group P2₁/c with a=15.611(3) ?, b=24.412 (5) ?, c=15.430 (6) ?, β=114.49 (3)°, V=5351.3 (19) ?³, ρ _calc=1.359 g cm⁻³, μ=0.472 mm⁻¹ and Z=4. The crystal structure of 1 features a mononuclear tricoordinated complex with a distorted triagonal planar geometry. The Cu^I center is coordinated to three imine N atoms of two Schiff base ligands, while the remaining one imine N atom keeps uncoordinated. UV-vis absorption and emission spectra indicate that the complexation of metal ion has slight influence on the electronic structure of the ligand. TGA analysis confirms that complex 1 is stable up to 253°C.Supplementary materials Crystallographic data reported in this paper have been deposited with Cambridge Crystallographic Data center (CCDC no.282672). Copies of the data can be obtained free of charge from www.ccdc.cam.ac.uk/conts/retrieving.html (or from the Cambridge Crystallographic Data Center, 12, Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336033; or deposit@ccdc. cam. ac.uk).     

A crystallographic study of 2-hydroxyacetophenone N(4)-cyclohexyl thiosemicarbazone

The crystal structure of 2-hydroxyacetophenone N(4)-cyclohexyl thiosemicarbazone is described. The compound crystallizes in the triclinic crystal system, space group , Z = 4, V = 1569.6(3) ?³ with unit cell parameters a = 6.9436(8) ?, b = 12.4762(15) ?, c = 18.588(2) ?, α = 100.187(2)°, β = 97.069(2)° and γ = 92.340(2)°. There are two independent molecules in the asymmetric unit. The crystal structure reveals that the compound exists in the thione form and S1 and N1 are at E configuration to each other with respect to N2-C8 bond. Similarly, S2 and N4 are trans to each other with respect to N5-C23 bond in the second molecule of the asymmetric unit. The packing of the molecules in the crystal lattice is stabilized by intermolecular hydrogen bonds.     

The synthesis and crystal structure of a new coordination polymeric adduct containing mercury iodide

A new organic-inorganic hybrid adduct, [HgI₂(dps)] _n (dps=4,4′-dipyridylsulfide), has been synthesized by the reaction of HgI₂ with dps in THF at room temperature. The structure characterization was performed by means of IR, elemental analyses and single crystal X-ray analysis. It crystallizes in space group P2(1)/c with a=5.5522(1) ?, b=12.127(2) ?, c=21.508(4) ?, β=91.84(3)°. The structure consists of distorted tetrahedral Hg(II) centers bridged by dps ligands to form one-dimensional linear chains with C–H···I interaction. Comparison of transition metal assemblies with dps showed that the dimensionality and structure of self-assembled supramolecule depend on the coordination preferences of metal ions, the geometry, bulk, and rigidity of ligands, the number and size of anions, and the supramolecular weak interactions.Supplementary material Crystallographic data for the structure reported in this article has been deposited in the Cambridge Crystallographic Data Center, CCDC No. 285579 for compound 1. The information may be obtained free of charge from the Director, CCDC, 12 Union Road, Cambridge, CB2 1EZ, UK (fax: +44-1223-336033; e-mail: deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk).     

Syntheses,characterization and crystal structures of two structurally similar Schiff bases isonicotinic acid [1-(3-methoxy-2-hydroxyphenyl)methylidene]hydrazide and isonicotinic acid [1-(4-dimethylaminophenyl)methylidene]hydrazide monohydrate

The Schiff base compounds, isonicotinic acid [1-(3-methoxy-2-hydroxyphenyl) methylidene]hydrazide (C₁₄H₁₃N₃O₃, 1) and isonicotinic acid [1-(4-dimethylaminophenyl) methylidene]hydrazide monohydrate (C₁₅H₁₆N₄O·H₂O, 2) have been synthesized by the condensation of equimolar 3-methoxysalicylaldehyde or 4-dimethylaminobenzaldehyde with isonicotinic acid hydrazide in MeOH or EtOH. The compounds were characterized by elemental analysis, IR, ¹HNMR spectra, and single crystal X-ray diffractions. Compound 1 crystallizes in the monoclinic space group P-1 with unit cell dimensions a = 7.662(1) ?, b = 16.249(2) , c = 10.874(2) ?, β = 110.426(3)°, V = 1268.7(3) ′³, Z = 4, R ₁ = 0.0644, and wR ₂ = 0.1283. Compound 2 crystallizes in the orthorhombic space group P2₁2₁2₁ with unit cell dimensions a = 7.388(1) ?, b = 11.812(1) ?, c = 17.197(2) ?, V = 1500.7(2) ′³, Z = 4, R ₁ = 0.0585, and wR ₂ = 0.1143. X-ray structure determinations revealed that the molecules of both compounds display trans configurations with respect to the C=N double bonds. In the crystal structure of 1, molecules are linked through N–H···N intermolecular hydrogen bonds, forming layers parallel to the bc plane, while in the crystal structure of 2, molecules are linked through N–H···O, O–H···O, and O–H···N intermolecular hydrogen bonds, forming a network. Supplementary material CCDC-615072 and 620235 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam. ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223–336033 or e-mail: deposit@ccdc.cam.ac.uk.     

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.