Synthesis,Characterization and Crystal Structure of Tetraphenylphosphonium Bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-Nickelate Acetone Solvate Crystal

Abstract  

A new crystal of tetraphenylphosphonium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-nickelate acetone solvate (BPNI) has been prepared at room temperature and characterized by elemental analysis, UV–Vis–NIR absorption spectrum and X-ray single crystal determination. The complex crystallized in monoclinic space group P2/c with unit cell dimensions a = 24.5350 (6) ?, b = 7.3097 (2) ?, c = 23.1141 (6) ?, β = 115.585 (2)°, V = 3738.89 (17) ?³, Z = 4, D _x .= 1.5081 (1) g cm⁻³. The X-ray structure determination revealed that the crystal is centro-symmetrical and there are two halves of independent cations in the molecule.     

Synthesis and Crystal Structure of 2-Amino-4-(4-hydroxyphenyl)-5-propylthiazole Ethanol Solvate 0.25 Hydrate

Abstract  

2-Amino-4-(4-hydroxyphenyl)-5-propylthiazole was synthesized by the reaction of α-bromo-1-(4-hydroxyphenyl)-1-pentone with thiourea. The crystal structure of its ethanol solvate 0.25 hydrate, C₁₂H₁₄N₂OS···C₂H₅OH···0.25·H₂O, was determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with a = 20.9046(10), b = 10.1057(5), c = 30.0017(15) ?, β = 105.5850(10)°, Z = 8, M _r = 569.77, V = 6105.0(5) ?³, D _c = 1.240 g/cm³, μ = 0.214 mm⁻¹, F(000) = 2440, the final R = 0.0598 and wR = 0.1825 for 5,911 observed reflections [I > 2σ(I)]. Compound (1) is composed by two non-coplanar ring systems of phenol and thiazole. The structure displays extensive O–H···N, N–H···O and O–H···O intermolecular hydrogen bonds.     

Structure of the Antiplasmodial Compound 7,9-Dinitrocryptolepine Hydrochloride Methanol Solvate

Abstract  The structure of C₁₆H₁₀N₄O₄[HCl,1.5CH₃OH], M_r = 406.80, has been determined from X-ray diffraction data. The crystals are monoclinic, space group C2/c, with eight molecules per unit cell and a = 21.482(4), b = 7.131(1), c = 24.495(5) ?, β = 111.01(3)°, crystal density D_c = 1.546 g/cm³. The material was difficult to crystallize and crystals produced were found to be poor diffractors. Intensity data were measured at liquid nitrogen temperature using a weakly diffracting crystal typical of the batch. However the X-ray analysis has finally enabled the chemical constitution of this cryptolepine derivative, which was previously incorrectly assigned, to be unequivocally established. Direct methods were used to solve the structure which was refined by full-matrix least squares to a conventional R-index of 0.0798 for 2,861 reflections and 268 parameters. The 7,9-dinitrocryptolepine molecule is highly planar with a strong intramolecular hydrogen bond between N(10) in ring C and O(92) of a nitro group. There are a number of intermolecular hydrogen bonds involving the cryptolepine derivative the hydrochloride and both solvated methanols. One of the methanol solvate molecules (methanol 2) is unusually disordered with its C atom lying exactly on a crystallographic twofold axis. Consequently the methanol OH and H₃ groups are at 0.5 occupancy and repeated by the twofold symmetry. Graphical Abstract  Cryptolepine (5-methyl, 10H-indolo[3,2-b]quinoline) the principal constituent of Cryptolepis sanguinolenta (Periplocaceae) is currently of interest as a lead compound for the development of both antimalarial and anticancer agents. Cryptolepine has potent activity against malaria parasites in vitro, but it is also cytotoxic on account of its abilities to intercalate into DNA, inhibit DNA synthesis and inhibit topoisomerase II. The 7,9-dinitroanalogue of cryptolepine was synthesised as part of a program designed to discover new antimalarial and anticancer agents. The X-ray structure of this compound will help to determine whether or not 7,9-dinitrocryptolepine is able to intercalate into DNA and facilitate the design of new cryptolepine analogues with DNA binding properties appropriate for antimalarial (with no DNA intercalation) or anticancer (sequence-specific binding) applications.      

Synthesis,Crystal Structure and Fluorescent Study of Bis(2-(2-hydroxyphenyl)benzimidazolate)zinc with Ethanol Solvate

Abstract  The zinc(II) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Zn(2-(2-hydroxyphenyl)benzimidazolate)₂]·C₂H₅OH (1 · C₂H₅OH) has been synthesized and characterized by X-ray crystallography and photoluminescent analysis. The complex crystallizes in monoclinic space group P2₁/c with cell parameters a = 10.156(1) ?, b = 25.771(3) ?, c = 9.674(1) ?, α = 90°, β = 103.641(2)°, γ = 90°, Z = 4, V = 2460.4(4) ?³. The central Zn(II) is four-coordinate and has a tetrahedral geometry. The steady-state and time-resolved photoluminescent spectra for the title compound have also been studied. The emission property can be ascribed to ligand-centered charge-transfer transition (LCCT) with π → π* property. Index Abstract   A new co-crystal of Zn(II) complex of 2-(2-hydroxylphenyl)benzimidazole with ethanol solvate has been prepared, characterized by X-ray crystallography and fluorescent studies.      

The Molecular and Crystal Structure of p-methyl-phenyl-glyoxyacid-p-chloranilide

Using X-ray crystal structure analysis of the title compound the positions of all the atoms (including all H atoms) in the monoclinic unit cell with the parameters a = 13.90₀ Å, b = 5.13₈ Å, c = 17.95₆ Å and β = 91.05° and the space group P 2₁/n were localized. The existence of an intramolecular N—H(N)…︁ O(1)-bridge was inferred, whose H-bridge acceptor predominantly is the π-electron density of the carbonyl group. At the same time the H(N) atom participates in the intermolecular bridge N H(N)…︁ O′(1) to the symmetry-equivalent neighbouring molecule. H-bridge-like interactions of the two phenyl hydrogen atoms H(6) and H(15) to the carbonyl oxygen O(2) have also been inferred from the torsion angles.     

Synthesis,Crystal Structure and Antibacterial Activity of 5-Bromonicotinic Acid [1-(4-Chlorophenyl)methylidene]hydrazide Monohydrate Methanol Solvate

Abstract  The compound 5-bromonicotinic acid [1-(4-chlorophenyl)methylidene]hydrazide monohydrate methanol solvate, derived from the condensation reaction of 5-bromonicotinic acid hydrazide with 4-chlorobenzaldehyde in a methanol solution, was synthesized and characterized by elemental analysis, IR spectrum, ¹H NMR and X-ray single crystal determination. The compound crystallizes in the triclinic space group P − 1 with unit cell dimensions a = 6.9360(14) ?, b = 10.070(2) ?, c = 12.267(3) ?, α = 84.39(3)°, β = 86.10(3)°, γ = 80.50(3)°, V = 839.8(3) Ǻ³, Z = 2, R ₁ = 0.0724, and wR ₂ = 0.1720. X-ray structure determination reveals that the compound has a trans configuration with respect to the C=N double bond or C–N single bond. In the crystal structure, molecules are linked through intermolecular O–H···N, O–H···O, and C–H···O hydrogen bonds, forming layers parallel to the ab plane. The preliminary biological tests show that the compound has excellent antibacterial activity. Index Abstract  The compound 5-bromonicotinic acid [1-(4-chlorophenyl)methylidene]hydrazide monohydrate methanol solvate, derived from the condensation reaction of 5-bromonicotinic acid hydrazide with 4-chlorobenzaldehyde in a methanol solution, was synthesized and characterized by elemental analysis, IR spectrum, ¹H NMR and X-ray single crystal determination. The molecule of the compound has a trans configuration with respect to the C=N double bond or C–N single bond. In the crystal structure, molecules are linked through intermolecular O–H···N, O–H···O, and C–H···O hydrogen bonds, forming layers parallel to the ab plane. The preliminary biological tests show that the compound has excellent antibacterial activity.      

X-ray Crystallographic Structure of the Potent Antiplasmodial Compound 2,7-Dibromocryptolepine Acetic Acid Solvate

Abstract  The structure of 2,7-dibromocryptolepine acetic acid solvate, C₁₆H₁₁N₂Br₂ [1.5(C₂H₄O₂)][C₂H₃O₂⁻][0.5H₂O], M_r = 460.17, has been determined from X-ray diffraction data. The crystals are monoclinic, space group P2₁/c with Z = 4 molecules per unit cell and a = 7.3243(3), b = 18.7804(6), c = 15.8306(7) ?, β = 94.279(1)°, V_c = 2171.5(2) ?, crystal density D_c = 1.667 g/cm³. The structure was determined using direct methods and refined by full-matrix least-squares to a conventional R-index of 0.0496 for 4,908 reflections and 258 parameters. The cryptolepine nucleus of the 2,7-dibromocryptolepine molecule is highly planar and the two Br atoms are in this plane within 0.06 and 0.01 ?, respectively. The crystal structure is maintained via hydrogen bonding between N(10) in the cryptolepine nucleus and the oxygen of one of the three solvated acetic acid molecules. The acetic acid molecules also form hydrogen bonded chains. Acetic acid B is deprotonated and its two C–O bond lengths are equivalent, unlike those in A and C. Acetic acid C lies very close to a crystallographic centre of symmetry. To avoid overlap the two repeats cannot exist together and are subject to 50% statistical disorder. O(1C) of this methanol is furthest from the two-fold axis and its occupancy refines to a value of 1.0 and is assumed to exist alternately as a water oxygen hydrogen bonding to methanol O(1C) across the two-fold axis at a distance of 2.775 ?. Index Abstract  The antiplasmodial activity of the analogue 2,7-dibromocryptolepine is nine times greater than that of cryptolepine itself against chloroquine-resistant Plasmodium falciparum (multi-drug resistant strain K1) with IC₅₀ values = 0.44 and 0.049 μM, respectively. This analogue also showed promising in vivo activity against P. berghei in mice. Parasitaemia was suppressed by 91.4% compared to untreated infected control animals at a dose of 25 mg/kg given daily by i.p. injection with no apparent toxicity to the mice, in contrast to cryptolepine which was toxic to mice when given i.p. at 20 mg/kg. Further experiments showed a dose-dependent relationship with ED₅₀ and ED₉₀ values of 6.92 and 21.46 mg/kg/day, respectively. Although 2,7-dibromocryptolepine was not toxic to the mice its cytotoxic activity is similar to that of cryptolepine, but unlike cryptolepine it does not appear to intercalate into DNA as assessed using thermodenaturation techniques (ΔTm values = 3 and 9 °C, respectively). Like cryptolepine, 2,7-dibromocryptolepine inhibits the formation of haemozoin, but its increased antiplasmodial potency does not appear to be due to more potent inhibition of haemozoin formation, nor to increased accumulation into the acidic parasite food vacuole suggesting that 2,7-dibromocryptolepine has additional modes of action compared to cryptolepine. The X-ray structure of this compound will help to determine whether or not 2,7-dibromocryptolepine is able to intercalate into DNA and facilitate the design of new cryptolepine analogues with DNA binding properties appropriate for antimalarial (with no DNA intercalation) or anticancer (sequence-specific binding) applications.      

The Crystal and Molecular Structure of Mesogenic Malonates

The crystal and molecular structures of diethylene-6-[4-(4′-nitrophenylazo)phenoxy]dodecylmalonate (12 PhNO₂) and -propylmalonate (3 PhNO₂) were determined with CuK_α to a = 19.235(5) Å, b = 7.620(1) Å, c = 22.400(4) Å; α = 90°, β = 103.27(1)°, γ = 90°; space group P2₁/c for 12 PhNO₂ and a = 6.797 (6) Å, b = 7.756 (8) Å, c = 22.74(2) Å; α = 81.48(7)°, β = 88.29(7)°, γ = 68.10(9)°; space group P1 for 3 PhNO₂. Refinement with 1130 observed reflections (> 3σ) for 12 PhNO₂ and 1615 for 3 PhNO₂ leads to R (12 PhNO₂) = 5.8% and R(3 PhNO₂) = 4.4%. The molecular conformation in the crystalline state is the most extended trans conformation for both compounds. On rapidly cooling from the isotropic melt, 12 PhNO₂ shows a smectic A-phase. In agreement with prior investigations on polar mesogens, the molecules arrange in an antiparallel packing. The azo-mesogen is nearly coplanar with the alkoxy spacer up to the branching atom. The low molecular weight malonates investigated may serve as model compounds for side-group liquid crystalline polymers.     

The Preparation and Crystal Structure of MgP4

In the systematical study of the A¹¹B^V semiconducting compounds the Mg-P system has been examined. Among the products of crystallization from Bi Pb Sn alloy the crystals of a new compound MgP₄ have been identified. It has been found that these crystals are isostructural with CdP₄. The crystal structure refinement from X-ray data has been performed. The lattice constants are: a = 5.141 Å, b = 5.079 Å, c = 7.518 Å, β = 98.64°; Z = 2; space group P2₁/c.     

The Crystal Structure of Hydrated Barium Copper Oxalate

BaCu(C₂O₄₂.6 H₂O is triclinic, P1 , with a = 6.5405(9), b = 9.202(3), c = 10.939(1) Å, α = 85.46(2), β = 79.22(1), γ = 80.45(2), V = 636.99(1) ų, Z = 2, D₀ = 2.14, D_c = 2.465 g. cm⁻³, R = 0.074, wR = 0.0746 for 2219 significant reflections |F₀|≧ 6.0σF₀. The barium has eleven coordinations and the coordination polyhedra is a capped antiprism. Six water oxygen atoms are coordinated whereas the other five are coming from the oxalate group. In the unit cell the molecules form a polymeric network. One lattice water molecule belongs to the coordinating water. The barium oxygen distances vary from 2.75 Å to 3.15 Å.     

The Crystal and Molecular Structure of 1,18-dibromooctadecane

The crystal and molecular structures of 1,18-dibromooctadecane are determined precisely by X-ray diffraction method. The results obtained are as follows: empirical formula, C₁₈H₃₆Br₂, formula weight Mr = 412.27, crystal system, monoclinic, space group, P2₁/n, lattice parameters, a = 5.496(1), b = 5.403(1), c = 34.374(4) Å, β = 94.50(1)°, volume of unit cell, V = 1017.6(3) ų, Z value, Z = 2, calculated density, D_x = 1.346 g/cm³, wave length of X-ray, λ(CuKα) = 1.5418 Å, absorption coefficient, μ(CuKα) = 49.64 cm⁻¹, F(000) = 428.00, temperature, T = 293 ± 1 K, R factor, R = 0.052, weighted R factor, R_w = 0.078 for 1019 unique observed reflection [I > 3σ (I)]. There are no unusual bond distances or angles. The structure obtained here is quite similar to that of 1,12-dibromododecane.     

The Crystal Structure and Conformational Studies of Acridinedione Derivatives

Abstract  

Two crystal structures of acridinediones namely, TMHAD and MPHAD were studied by X-ray crystallographic method in view of their occurrence in numerous commercial products including pharmaceuticals, fragrances and dyes. Crystal data of TMHAD are: C₁₇H₂₃NO₂, orthorhombic, Fdd2, with cell parameters a = 40.417(6) ?, b = 5.744(1) ?, c = 12.979(2) ?, V = 3013.1(7) ?³, Z = 8, D_cal = 1.205 Mg/m³, μ = 0.078 mm⁻¹. Crystal data of MPHAD are: C₂₀H₁₈NO₃; monoclinic, P2₁/c with cell parameters a = 10.182(9) ?, b = 17.105(14) ?, c = 10.895(9) ?, β = 117.857(1)°, V = 1678(2) ?³, Z = 4, D_cal = 1.268 Mg/m³, μ = 0.085 mm⁻¹. Both data were collected using λ (MoK_α) = 0.71073 ?. The central ring in the acridinedione moieties tends to be planar while the outer two rings adopt sofa conformations. Intermolecular interactions of C–H···O type of hydrogen bond help the molecules to stabilize into the crystal packing. Interestingly, a week forces of C–H···π interactions also helps the molecules for stabilization.     

Crystal Structure of Rabdoternin A

Abstract  

Rabdoternin A is a natural diterpenoid isolated from Rabdosia rubescen and its crystal structure was determined by X-ray single crystal diffraction. The compound compactly packs in an orthorhombic unit cell in the P2₁2₁2₁ space group with unit cell dimensions a = 7.9200(10) ?, b = 11.2411(14) ?, c = 20.474(2) ?, V = 1822.8(4) ?³ and Z = 4. Two intermolecular hydrogen bonds assemble the title compound into infinite two-dimensional networks along (001) plane.     

The Crystal and Molecular Structure of 4'-Cyanophenyl-4-n-Pentylbenzoate

The crystal and molecular structure of the title compound with the formula C₅H¹¹—C₆H₄—COO—C₆H₄—CN (CPPB) has been determined by X-ray diffraction methods. CPPB crystallizes in the monoclinic space group P2₁/n with eight molecules in a unit cell of dimensions a = 15.268(2) Å, b = 9.165(1) Å, c = 24.031(3) Å, β = 94.67(1)°. The structure has been solved by direct methods and refined to an R value of 0.070.

The CPPB molecules adopt a stretched form and are packed in an approximate parallel imbricated mode, the molecular long axes making an angle of about 5° with the crystal c axis. The molecular geometry and packing are discussed in relation to the mesomorphic behavior of CPPB.     

Synthesis, Crystal Structure and Electrochemical Property of New Rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene)bis(azido)cobalt(III) Nitrate Methanol Solvate Complex

Abstract  

The new cobalt compound, [Co(C₁₆H₃₅N₁₀]⁺(NO₃)⁻·CH₃OH (1), have been synthesized and characterized. It’s structure and electrochemical property were investigated using single-crystal X-ray diffraction and cyclic voltammetry in solutions of dimethyl sulfoxide (DMSO) and methanol (CH₃OH). The X-ray diffraction analysis reveals that 1 crystallizes in the monoclinic space group P2₁/c with a = 9.8339 (10) ?, b = 16.4048 (17) ?, c = 15.3628 (16) ?, β = 104.96 (9)° and Z = 4. The complex 1 consists of one [Co(C₁₆H₃₅N₁₀)]⁺ cation, one NO₃ ⁻ anions and one solvent CH₃OH molecule. The metal center of complex 1 is six-coordinated, with the four nitrogens of the macrocycle defining an equatorial plane and two axially ligated [N₃]⁻ ions completing the cobalt coordination sphere. Moreover, hydrogen bonds of O–H⋯N, O–H⋯O and N–H⋯O and static force connect two components of the compound and maintain the crystal structure. Additionally, in situ spectro-electrochemical measurements support Co(III)/Co(II) reversible reduction processes with the observation of the corresponding spectral changes with the applied potentials E _app = −1.5 and 0.5 V. The results obtained by the method are in agreement with those by the CV methods.     

Crystal Structure of Microclusters of Silver

Finding the crystallographic structure of clusters is a crucial and challenging problem. The properties like lattice concentration, unusual crystal symmetries etc. of metal clusters have been studied recently. We report here a 15% lattice concentration for silver clusters produced by Bredig's method.     

Crystal Structure of Glycinium Dicitratoborate Monohydrate

Crystallography Reports - Crystals of glycinium dicitratoborate monohydrate H3NCH2COOH[B(C6H6O7)2] · Н2О have been synthesized and selected for the first time. Their structure is...