X-ray structure analysis of 1-(4-bromophenyl)-3-(4-chlorophenyl)-prop-2-en-1-one

The title compound crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 15.6239(15) ?, b = 14.0537(14) ?, c = 5.8396(5) ?, β = 92.666(3)°, V = 1280.8 (2) ?³, and Z = 4. The final reliability index is 0.0538 for 2921 observed reflections. Two phenyl rings of the title molecule are not coplanar, with a dihedral angle of 46.3(0)°. The molecular planarity of this substituted chalcone is strongly affected by the 4′-bromo group. The crystal cohesion is accentuated by π···π, C–H···Br interactions and R₃ ¹ (11) hydrogen bond.     

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.     

Variable Ag—O bonding patterns in silver cyclic amide tri-aryl-phosphine complexes

The solid-state structures of five new tri-arylphosphine silver cyclic amide complexes having a systematic variation in the ring structures have been resolved. Normal Ag—N bonding and variable, weaker Ag—O bonding interactions, which can be attributed to the ring modifications, form the basis of the bonding patterns. Reported here are the solid-state structures of silver complexes of tri-arylphosphine derivatives of silver 1(2H)-phthalazinone, silver phthalimide, silver 1,2,3-benzotriazin-4(3H)-one, silver 2H-1,3-benzoxazine-2,4(3H)-dione and silver 2,3-dihydro-1,4-phthalazine- dione. The unit cell parameters are: P-1, a = 11.179(2) ?, b = 15.508(3) ?, c = 22.636(5) ?, α = 104.30(3)°, β = 95.39(3)°, γ = 94.62(3)°; C2/c, a = 17.3600(8) ?, b = 15.4930(8) ?, c = 15.0760(7) ?, β = 113.911(2)°; P-1, a = 11.0656(2) ?, b = 11.9447(2) ?, c = 17.4764(3) ?, α = 79.5254(9)°, β = 80.2877(9)°, γ = 68.9136(7)°; P-1, a = 10.5743(4) ?, b = 11.8439(4) ?, c = 19.0110(8) ?, α = 102.4280(13)°, β = 104.0330(12)°, γ = 100.2520(18)°, P-1, a = 13.6908(3) ?, b = 16.2230(4) ?, c = 18.3678(7) ?, α = 86.8920(10)°, β = 69.5290(10)°, γ = 70.7840(10)°, respectively. Four of the complexes include ligand chelation by Ag—O bonding to the adjacent carbonyl in addition to the main Ag—N connection.     

Complexation with diol host compounds. Part 36: inclusion compounds of 1,1,6,6-tetraphenylhexa-2,4-diyne-1,6-diol with benzene, toluene and mesitylene

The title compound 1,1,6,6-tetraphenylhexa-2,4-diyne-1,6-diol (H) forms inclusion compounds with benzene, toluene and mesitylene. H·C₆H₆ (1) and H·C₇H₈ (2) crystallize in the triclinic space group P(-1) with unit cell dimensions for 1: a = 13.001(3) ?, b = 15.284(3) ?, c = 16.744(3) ?, α = 99.26(3)°, β = 74.78(3)°, γ = 64.96(3)°, Z = 4 and for 2: a = 12.922(3) ?, b = 15.159(3) ?, c = 16.562(3) ?, α = 68.12(3)°, β = 73.99(3)°, γ = 66.00(3)°, Z = 4. The hydroxyl groups of adjacent host molecules are involved in hydrogen bonding. H·C₉H₁₂ (3) exhibits a different packing arrangement with weak hydrogen bonding between the hydroxyl hydrogen of the host and the phenyl ring of the guest. The crystal system of compound 3 is monoclinic with space group C2/c, a = 23.750(5) ?, b = 8.4746(17) ?, c = 17.760(4) ?, α = 90°, β = 123.40(3)°, γ = 90°, Z = 4. The thermal behaviour of these compounds has also been studied.     

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.     

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.     

Group 6 metal carbonyl complexes of a bulky phosphine: The crystal structures of tris(trimethylsilyl)phosphine-M(0)pentacarbonyl, M = chromium, molybdenum, and tungsten

The crystal structures of M(P{Si(CH₃)₃}₃)(CO)₅, M = Cr (1), Mo (2), and W (3), have been determined. Crystal data for 1, trigonal crystal system, space group = P3₁, a, b = 9.2118(6) ?, c = 22.416(3) ?, V = 1647.3(2) ?³, Z = 3; for 2, trigonal crystal system, space group = P3₂, a, b = 9.3394(3) ?, c = 22.7375(12) ?, V = 1717.56(12) ?³, Z = 3; trigonal crystal system, space group = P3₂, a, b = 9.3147(5) ?, c = 22.6955(16) ?, V = 1705.33(18) ?³, Z = 3. All three structures show distorted octahedral coordination environments around the metal center and exhibit especially long M–P bond distances, illustrating the unique steric and electronic properties of this bulky phosphine ligand. The ³¹P{¹H} NMR spectra of the compounds are also reported.     

Synthesis,spectroscopic and structural studies of <Emphasis Type="Italic">N</Emphasis>-(1<Emphasis Type="Italic">H</Emphasis>-benzimidazol-2-yl)-<Emphasis Type="Italic">N</Emphasis>′-benzyl propionamidine

N-(1H-Benzimidazol-2-yl) propionimidic acid ethyl ester (1) reacts with benzylamine to yield the corresponding N-(1H-Benzimidazol-2-yl)-N′-benzyl proponamidine (2). The structure and conformation of the amidine 2 were determined by ¹H and ¹³C NMR and X-ray diffraction. The product crystallizes in monoclinic system with space group P2₁/c, a = 10.7913 ?, b = 15.5164 ?, c = 9.1130 ?, β = 108.378° and Z = 4. In the crystal there are two N–HN hydrogen bonds, the first is intramolecular H-Bond links H4 to N1; the second one is intermolecular and it links H2 to N3 of a second molecule leading to inversion-related dimers. The X-ray results were compared with those obtained by semi-empirical and ab-initio calculations.     

Synthesis and structural characterization of the dinuclear bis(glutarato)bis(urea)copper(II)complex, dihydrate

The complex [Cu(OOC-(CH₂)₃-COO)(O=C(NH₂)₂]₂·2H₂O has been synthesized and characterized by X-ray crystallography. It crystallizes in the triclinic system P-1 with a = 8.003(2) ?, b = 8.611(2) ?, c = 8.620(2) ?, α = 96.14(3)°, β = 116.66(2)°, γ = 105.66(4)° and V = 492.9(3) ?³. The structure consists of discrete centrosymmetric binuclear units and water molecules. The Cu(II) ions adopt a square-pyramidal coordination with four oxygen atoms of four bridging carboxylate and one carbonyl oxygen of the monodentate urea ligand. There is a very strong interaction between the two copper centers in binuclear entities (CuCu: 2.6266(15) ?).     

Syntheses and crystal structures of two N-substituted thio-imidazoles

The syntheses and structures of two N-substituted thio-imidazoles are reported. The geometrical parameters for both compounds, including essentially planar imidazole rings, are consistent with previous structural studies of related materials. The only possible non-van der Waals’ interactions influencing the molecular packing are weak C–H⋯π bonds. Crystal data: C₁₂H₁₄N₂S (N-methyl-N′-2-phenylethyl-imidazol-2-thione), M _r = 218.31, monoclinic, P2₁/n, (No. 14), a = 6.8441(2) ?, b = 12.9960(4) ?, c = 13.4703(4) ?, β = 97.7729(16)°, V = 1187.12(6) ?³, Z = 4, R(F) = 0.039, wR(F ²) = 0.104. C₁₉H₂₀N₂S (N,N′-bis((s)-1-phenylethyl)imidazol-2-thione), M _r = 308.43, orthorhombic, P2₁2₁2₁ (No. 19), a = 10.4060(3) ?, b = 10.6712(3) ?, c = 14.8932(3) ?, V = 1653.81(7) ?³, Z = 4, R(F) = 0.038, wR(F ²) = 0.085.     

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).     

Crystal structure of irisolidone from the flowers of Pueraia lobata

Irisolidone (5,7-dihydroxy-6,4′-dimethoxyisoflavone) was isolated from the flowers of Pueraia lobata and its crystal structure was examined by X-ray single crystal diffraction. The crystal structure of irisolidone is monoclinic, space group P2₁/c with a = 15.491(9) ?, b = 7.895(4) ?, c = 13.321(7) ?, β = 110.546(9)° and Z = 4. Hydrogen bonding and aromatic π–π stacking assemble the title compound into a three-dimensional networking structure.     

Structure of 2-(1-phenylimidiazolidin-2-ylidene)- malononitrile and 2-(hexahydropyrimidinyl-2-ylidene)- malononitrile

The crystal structure of 2-(1-phenylimidazolidin-2-ylidene)-malononitrile, I, and 2-(hexahydropyrimidin-2-ylidene)-malononitrile, II, were determined with crystal data (I: Monoclinic, P2₁/n, a=8.116(3) ?, b=7.650(3) ?, c=17.399(7) ?, β=93.065(6)°, R _all=0.0980; II: Monoclinic, P2₁/n, a=9.169(2) ?, b=8.103(2) ?, c=10.337(3) ?, β=99.853(4)°, R _all=0.0877). N−H···N hydrogen bonds were responsible for the formation of centrosymmetric dimers of I and one-dimensional zigzag molecular chains of II.     

A microporous coordination polymer with 1-D channels constructed from a basic reaction system

A ytterbium coordination polymer, {[Yb₂(OH)₂(atpt)₂]·0.5H₂O} _n , (atpt = 2-aminoterephthalate) was synthesized by using the reaction of YbCl₃·6H₂O with 2-aminoterephthalic acid under hydrothermal condition and structurally characterized by single-crystal X-ray diffraction method. The Yb(III) complex crystallizes in the monoclinic system P2/c with a = 13.1306(9) ?, b = 7.8049(5) ?, c = 21.5601(12) ?, β = 111.481(3)°, V = 2056.1(2) ?³, Z = 4. There are two crystallographically independent Yb³⁺ ions in the crystal, in which one is seven-coordinate, the other is eight-coordinate, and both of them are in oxygen environments. The ligand atpt adopts two coordination modes, bis(bridging bidentate) and bis(chelating and bridging tridentate). In addition, every hydroxyl group adopts μ₃-O mode linking three Yb³⁺ ions. It is through the linkage of atpt and hydroxyl group that ytterbium ions are linked together to form a 3-D structure with an open metal–organic framework.     

PM3 semiempirical study and its comparison with X-ray crystal structure of 4-[2-Methyl-4-(4-methoxyphenylazo)] phenoxyphtalonitrile

  The molecular and crystal structures of the title compound, C₂₂H₁₆N₄O₂, were determined by single crystal X-ray diffraction technique. The title compound crystallizes in monoclinic space group P1 2 ₁ /n1, with a=12.7811(9) ?, b=8.2002(4) ?, c=17.8772(14) ?, Z=4, D _calc=1.3112(1) g/cm³, μ (Mo-K_α)=0.087 mm⁻¹. The structure was solved by direct methods and refined to a final R=0.056 for 1891 reflections with I > 2σ (I). The asymmetric unit in the crystal structure contains only one neutral molecule. The positions of nitrogen atoms in the azo groups were disordered. There is no classic hydrogen bond in the crystal structure. The molecules in the crystal structure are stacked by π–π stacking and one edge-to-face interactions. In order to determine conformational flexibility and crystal packing effects on the molecules, molecular energy profile of the title compound was obtained with respect to the selected torsion angle, which is varied from −180° to +180° in every 10° via PM3 semi-empirical method.     

Synthesis and crystal structure of 3,5,9,11-tetraacetyl-14-oxo-1,3,5,7,9,11-hexaazapentacyclo[5.5.3.02,6.04,10.08,12]pentadecane

Crystals of 3,5,9,11-tetraacetyl-14-oxo-1,3,5,7,9,11-hexaazapentacyclo[5.5.3.0^2,6.0^4,10 .0^8,12]pentadecane, a new hexaazaisowurtzitane derivative, were obtained from a condensation reaction of 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0^5,9.0^3,11] dodecane with aqueous formaldehyde and subsequent crystallization of the product from aqueous acetone. X-ray diffraction analysis at room temperature indicates that the compound crystallizes in monoclinic system, space group P2₁/n with a = 9.4564(15), b = 14.184(2), c = 13.334(2) ?, β = 107.671(4)°, V = 1704.1(5) ?³, Z = 4, D _calc = 1.475 g/cm³, F(000) = 800, μ(MoK) = 0.112 mm⁻¹, and final R ₁ = 0.0505, wR ₂ = 0.1215 for observed reflections 2641 (I > 2σ(I)). The ether link (C–O–C) forms two heptacyclic rings with the N, C atoms in the cage respectively. The results of elemental analysis, IR and NMR spectroscopy are included.     

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.      

Crystal Forms of the Antiepileptic Lamotrigine: Molecular Salts and Solvates with Fluorobenzoic Acid,Nicotinic Acid, 2-Thiobarbituric Acid, 3-Picoline and Butyl Alcohol

Abstract  

The crystal structures of three salts and two solvated multicomponent crystals of lamotrigine with 4-fluorobenzoic acid, nicotinic acid, 2-thiobarbituric acid, 3-picoline and butyl alcohol are reported. Compound 1a crystallizes in monoclinc system, space group P2₁ with a = 13.3860(5) ?, b = 8.3420(3) ?, c = 15.5200(6) ?, β = 93.524(1)°, V = 1729.78(11) ?³, and Z = 2. Compound 1b crystallizes in monoclinic system, space group P2₁/c with a = 10.6625(7) ?, b = 16.2575(11) ?, c = 13.6346(9) ?, β = 100.904(1)°, V = 2320.8(3) ?³, and Z = 4. Compound 1c crystallizes in triclinic system, space group P[`1] \overline{1} , with a = 10.1309(7) ?, b = 12.0260(8) ?, c = 14.0826(10) ?, α = 71.783(1)°, β = 86.451(1)°, γ = 80.902(1)°, V = 1609.10(19) ?<sup>3</sup>, and Z = 1. Compound 1d crystallizes in monoclinic system, space group P2<sub>1</sub>/c with a = 14.9570(10) ?, b = 8.0230(6) ?, c = 13.8162(10) ?, β = 102.884(1)°, V = 1616.2(2) ?<sup>3</sup>, and Z = 4. Compound 1e crystallizes in triclinic system, space group P[`1] \overline{1} , with a = 7.5710(6) ?, b = 8.5721(7) ?, c = 13.5532(11) ?, α = 85.364(1)°, β = 79.632(1) (1)°, γ = 86.188(1)°, V = 861.19(12) ?³, and Z = 2. Characteristic R₂²(8) dimer is observed in all five structures. A complete hydrogen bonded motif analysis is described. Lamotrigine-lamotrigine base pair is observed in all the structures, except in (1b). In (1c), the R₂²(7) dimer is noticed while, in all other structures R₂²(8) dimer exist between the lamotrigine-lamotrigine base pair. In all the six structures, chlorine atoms of the lamotrigine molecules are not involved in any interactions.     

Synthesis and crystal structure of cobalt(III) complex with a Schiff base and azide

The cobalt(III) complex, [Co(L)₂(N₃)₂]₂(ClO₄)₂, L being a Schiff base N-[phenyl(pyridin-2-yl)methylene]aniline has been synthesized and the crystal structure determined using X-ray crystallography. The complex crystallizes in triclinic system, space group P-1 with unit cell parameters a=10.9367(9) ?, b=18.0817(17) ?, c=20.1629(16) ?, α=111.341(2)°, β=91.622(2)°, γ=107.5030(10)°, V=3499.1(5) ?³ and Z=2. It crystallizes with two independent molecules in the asymmetric unit. The two cobalt atoms are hexa-coordinate and have a distorted octahedral geometry, satisfied by four nitrogen atoms from two molecules of the Schiff base and two nitrogen atoms from the monodentate azide group. The perchlorate ions are non-coordinating.     

Crystal Study of Salicylaldehyde N(4)-Phenylthiosemicarbazone

Abstract The crystal structure of salicylaldehyde N(4)-phenyl thiosemicarbazone is described. The compound crystallizes in the triclinic crystal system, space group P Z = 6, V = 2002.1(5) ?³ with unit cell parameters a = 10.6733(15) ?, b = 13.8856(19) ?, c = 14.052(2) ?, α = 81.851(2)°, β = 77.061(2)° and γ = 83.482(2)°. There are three independent molecules in the asymmetric unit. The crystal structure reveals that the compound exists in the thione form and S1 and N3 are at E configuration to each other with respect to N2–C7 bond. Similarly, S2 and N6 are trans to each other with respect to N5–C21 bond in the second molecule of the asymmetric unit and S3 and N9 are trans to each other with respect to N8–C35 bond in the third molecule of the asymmetric unit. The packing of the molecules in the crystal lattice is stabilized by intermolecular hydrogen bonds. Index Abstract The compound salicylaldehyde N(4)-phenyl thiosemicarbazone crystallizes in the triclinic crystal system, space group P Z = 6, V=2002.1(5) ?³ with unit cell parameters a = 10.6733(15) ?, b = 13.8856(19) ?, c = 14.052(2) ?, α = 81.851(2)°, β = 77.061(2)° and γ = 83.482(2)°. The structure of the compound salicylaldehyde N(4)-phenylthiosemicarbazone