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     

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.     

Crystal and Molecular Structure of the 1:2 Salt Formed Between 1,2-(4-Pyridyl)Ethane and 2-(4-Hydroxyphenylazo)Benzoic Acid

Abstract  Proton transfer occurred during co-crystallization of 1,2-(4-pyridyl)ethane with 2-(4-hydroxyphenylazo)benzoic acid to yield a salt comprising a 1:2 ratio of 1,2-bis(4-pyridinium)ethane dications and 2-(4-hydroxyphenylazo)benzoate anions. Centrosymmetrically related anions associate by charge-assisted O–H···O hydrogen bonds to form 24-membered {···OC₃N₂C₄OH}₂ synthons. These are connected into a supramolecular polymer via charge-assisted N–H···O hydrogen bonds involving the 1,2-bis(4-pyridinium)ethane dications. The compound crystallizes in the triclinic space group P−1 with a = 8.517(4) ?, b = 9.110(5) ?, c = 10.477(5) ?, α = 96.850(13)°, β = 94.446(12)°, γ = 104.946(10)° and Z = 1 {two anions and a dication}. Index Abstract  Supramolecular chains mediated by charge-assisted O–H···O and N–H···O hydrogen bonding are found in the salt containing a 1:2 ratio of 1,2-bis(4-pyridinium)ethane dications and 2-(4-hydroxyphenylazo)benzoate anions.      

Structural studies of a novel bioactive benzophenone derivative: (4-Chloro-2-hydroxy-phenyl)-phenyl-methanone

The title compound (4-Chloro-2-hydroxy-phenyl)-phenyl-methanone was synthesized and the product obtained was characterized by spectroscopic techniques, and finally the structure was confirmed by X-ray diffraction studies. The compound crystallizes in the orthorhombic crystal system with the space group Pbca with unit cell parameters, a = 14.0359(5) Å, b = 6.8084(3) Å, c = 23.1097(8) Å, and Z = 4. The structure exhibits an intramolecular hydrogen bond which closes an S(6) ring. No directional interactions beyond the van der Waals packing contacts were identified in the crystal structure.     

Growth kinetics of zinc(tris)thiourea sulphate (ZTS) crystals

Growth kinetics of zinc (tris) thiourea sulphate (ZTS) crystals investigated as a function of supersaturation is reported in this communication. Crystal growth rates were investigated normal to the (100), (010) and (001) faces under growth conditions employed for bulk crystal growth. The growth rates normal to (010) and (100) were found to follow the continuous growth model (R_G = Cσ) with respect to the supersaturation whereas the growth rates normal to (001) was found to satisfy birth and spread (B+S) model (R_G = Aσ^5/6 exp(‐B/σ)). The growth rates observed normal to the studied face are in agreement with the growth mechanism predicted from the estimated α (Jackson) factor. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of di(1-pyrazolyl)methane,CH2(C3N2H3)2

The title compound consists of two planar pyrazolyl fragments oriented at 73.0° to each other and linked to a common carbon atom. All hydrogen atoms were located unambiguously and their positions were refined.     

Hydrothermal synthesis of [Mn(HTPO)(BIPY)] (H3TPO = tris-(4-carboxylphenyl)phosphine oxide): a crosslinked coordination polymer

The hydrothermal synthesis and crystal structure of the title compound is reported. The structure consists of 1-D looped chains with the HTPO ligand binding through the phosphoryl and two carboxylate oxygens to manganese atoms. The carboxylic acid group is hydrogen bonded to adjacent chains forming a 2-D hydrogen bonded network. The crystals are triclinic and the space group isP-1 with a = 11.6767(8) Å, b = 10.8680(8) Å and c = 11.4232(87rpar; Å = 92.301(2)°, = 106.932(2)° and = 103.2390(10)° V = 1341.02(16) ų; Z = 2.     

Synthesis,Characterization and Crystal Structure of Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate

Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate was synthesized from ethyl 6-(4-bromophenyl)-4-(4-fluorophenyl)-2-oxocyclohex-3-ene-1-carboxylate and ammonium acetate in glacial acetic acid. The synthesized compound was characterized by elemental analysis, FT-IR, thermogravimetric analysis (TGA), differential thermal analysis (DTA), UV-Visible, and single-crystal X-ray diffraction. The title compound, ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate, C₂₁H₂OFNO₂, crystallizes in the orthorhombic space group Pbca with the following unit-cell parameters: a = 17.417(2), b = 9.7287(9), c = 21.014(2) Å, and Z = 8. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0644 for 1616 observed reflections. An intramolecular N–H…O hydrogen bond generates an S(6) graph-set motif. In the crystal, molecules are linked by N–H…O hydrogen bonds, forming a two-dimensional network.     

Crystal structure of bis(2-butyl-4-chloro-imidazole)5-iminoethane

The title compound (C₁₈H₂₆N₆Cl₂) crystallizes in monoclinic space group P2₁/c with a = 14.867(4) Å}, b = 7.758(2) Å}, c = 9.671(3) Å}, = 108.78(1), V = 1056.0(5) Å}³, Z = 2, D_cal = 1.250 Mg/m³ at T = 293 K. The structure was solved by direct methods and refined by full-matrix least-squares procedures to final R = 0.0650 and wR = 0.1719 using 2493 reflections. The imidazole ring is planar and the n-butyl chain adopts an extended conformation. The molecules in the crystal are stabilized by N–H s N type of intermolecular hydrogen bondings in addition to van der Waals forces.     

Crystal structures of N1, N5‐dibenzoyltetrahydro‐4‐methyl‐1, 5‐benzodiazepin‐2‐one (DBTBO) and tetrahydro‐4‐methyl‐1, 5‐benzodiazepin‐2‐one (TBO)

Adducing structural analogies between the two fused systems, N1, N5‐Dibenzoyltetrahydro‐4‐methyl‐1,5‐benzodiazepin‐2‐one, C₂₄H₂₀N₂O₃ (DBTBO CCDC 200341) and Tetrahydro‐4‐methyl‐1,5‐benzodiazepin‐2‐one, C₁₀H₁₂ N₂O (TBO CCDC 200342) helps to find the pharmacological differences from the view point of variant hetero atom substitutions in the hetero cycle. Both the diazepines crystallized in identical monoclinic space group P2₁/n with a = 14.1134(1) Å, b = 9.2444(1) Å, c = 16.3812(1) Å; β = 107.11(1)º, V = 2042.7(3) ų for DBTBO and a = 9.3363(7) Å, b = 10.4895(8) Å, c = 9.9852(7) Å, β = 91.314(1)º, V = 977.62(1) ų for TBO, respectively. The two structures were solved by direct methods and refined by full‐matrix least‐squares procedure to final R‐values of R1 = 0.0575(DBTBO) and R1 = 0.0984(TBO). Structural differences include non‐identical boat conformations of these seven‐membered rings and the different non‐bonding interactions in the benzodiazepine pair.     

Structural and spectroscopic study of Mg13.4(OH)6(HVO4)2(H0.2VO4)6

Single‐crystals of the polar compound magnesium hydrogen vanadate(V), Mg_13.4(OH)₆(HVO₄)₂(H_0.2VO₄)₆, were synthesized hydrothermally. It represents the first hydrogen vanadate(V) among inorganic compounds. Its structure was determined by single‐crystal X‐ray diffraction [space group P 6₃mc, a = 12.9096(2), c = 5.0755(1) Å, V = 732.55(2) ų, Z = 1]. The crystal structure of Mg_13.4(OH)₆(HVO₄)₂(H_0.2VO₄)₆ consists of well separated, vacancy‐interrupted chains of face sharing Mg2O₆ octahedra, with short Mg2—Mg2 distances of 2.537(1) Å, embedded in a porous magnesium vanadate 3D framework having the topology of the zeolite cancrinite. All three hydrogen positions in the structure were confirmed by FTIR spectroscopy. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Thermal and phase behaviour studies of hydrogen-bonded compounds (SA:nOBA) using POM,DSC and image-processing techniques

A novel series of hydrogen-bonded liquid crystals are synthesised. The hydrogen bond is formed between non-mesogenic salicylic acid and the mesogenic p-n-alkoxy benzoic acids with n = 4–8, 10–12 and 16. The formation of hydrogen bond is confirmed from infrared studies. The transition temperatures and the phase identification are made with the use of polarising microscope (POM) attached with a hot stage. Further, the heats of transition and enthalpies are obtained by employing the differential scanning calorimeter (DSC). Along with POM and DSC, textural image analysis is done by image-processing techniques using MATLAB software and transition temperatures are identified. The results reveal that the compounds with the chain number n = 7, 8, 10–12 show the manifestation of smectic-B phase by quenching smectic-C phase.     

Crystal structure of [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2] (Hdmpa = N,N-dimethyl-3-amino-1-propanol)

The copper complex, [Cu₂(II)(dmpa)₂(p-Cl-C₆H₅COO)₂], has been prepared and its structure determined using X-ray crystallography. The dimer is a di-₂-alkoxo complex which is a five-coordinate copper dimer with unsupported alkoxo bridges. The complex crystallizes in the triclinic space group P-1 with a = 11.384(2), b = 14.636(5), c = 9.609(2) Å, = 100.07(2), = 104.33(3), = 72.79(2)°, V = 1471.8(7) ų, and Z = 2. The structure is comprised of discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the dmpa^– ligands. The Cu-O and Cu-N distances are in good agreement with those found for other copper(II) aminoalcoholato complexes. The Cu···Cu distance is 2.9765(6) Å. In the crystal, every two dimeric coordination molecules are combined together by the recognition through intermolecular hydrogen-bonding interactions between the apical water molecule and the non-coordinated O atom from the p-chlorobenzoato ligand, forminga tetramer.     

Crystal and molecular structure of the bidentate ligand 2,2-di(1-pyrazolyl)propane,CH3C(C3N2H3)2CH3

The title compound lies on a site of C₂ symmetry, with the two planar pyrazolyl moieties oriented at 86.1° to one another. The hydrogen atoms were located and refined.     

Synthesis and crystal structure of bis(benzimidazolium) tetrahalocobaltate(II)

The crystal structures of benzimidazolium tetrahalocobaltates (HBz)₂[CoX₄] (X = Cl and Br) have been determined. The chloride salt is triclinic, P-1, with a = 7.670(3) Å, b = 8.307(3) Å, c = 15.730(2) Å, and = 87.37(3)°, = 84.99(3)°, = 67.72(2)°. The bromide salt is monoclinic, C2/c, with a = 15.568(2) Å, b = 8.063(3) Å, c = 5.762(2) Å and = 91.36(3)°. The structures of the two salts are closely related. Both the compounds contain isolated tetrahedral CoX₄ ^2– anions and benzimidazolium cations. In the chloride salt, three chloride ions are involved in strong hydrogen bonding while only two bromide ions participate in the bromide salt. The greater deviation from the ideal tetrahedral geometry in CoBr₄ ^2– can be related to the less extensive hydrogen-bonding network compared to the chloro complex.     

Crystal and molecular structure of the triflate salt of diprotonated 1,4,8,11-tetrakis(2-hydroxyethyl)-1,4,8,11-tetraazacyclotetradecane, [C10H22N4(CH2CH2OH)4 2+]−[CF3SO3 −]2: geometry of a diprotonated octadenate ligand

The title complex crystallizes in the centrosymmetric monoclinic space group P2₁/n with Z=2. The cation is the diprotonated derivative of the neutral octadentate macrocyclic ligand C₁₀H₂₀N₄(CH₂CH₂OH)₄; the two protonated nitrogen atoms are as far apart as is possible in the 14-membered ring (1-and 8-positions) so as to minimize electrostatic repulsions. Each of the [C₁₀H₂₂N₄(CH₂CH₂OH)₄ ²⁺] cations is involved in hydrogen bonding (through the four hydroxy groups) to oxygen atoms on four different peripheral [CF₃SO₃ ⁻] anions.     

Synthesis,spectroscopic and X-ray structural study of [<Emphasis Type="Italic">trans</Emphasis>-di(4-aminobenzoato)bis(ethylenediamine) cobalt(III)] 4-aminobenzoate tetrahydrate

The title compound was synthesized by mixing the separately dissolved trans-dichlorobis(ethylenediamine)cobalt(III) chloride and sodium 4-aminobenzoate in aqueous medium in 1:3 molar ratio and recrystallizing the product obtained, from hot water. Elemental analyses and spectroscopic techniques (IR, UV/visible, ¹H and ¹³C NMR) were used for characterizing the complex salt. X-ray structure determination revealed an ionic structure consisting of [Co(en)₂(C₇H₆NO₂)₂]⁺ cation, (C₇H₆NO₂)⁻ anion and four lattice water molecules. The complex salt crystallizes in the triclinic space group P with cell dimensions a = 9.985(1) Å, b = 11.522(1) Å, c = 14.233(1) Å, α = 80.20(1)^∘, β = 72.80(1)^∘, γ = 86.43(1)^∘, Z = 2, V = 1541.3(2) ų, R₁ = 0.0291, and wR₂ = 0.0751.     

Strain Energy and Structural Property of Methyl Substituted Imogolite

Aluminosilicate mineral, imogolite, with chemical composition [(OH)₃Al₂O₃SiOH] has high monodispersity of diameter originated by the arrangements of inner hydroxyl (OH) groups that induced the strain energy minimum due to hydrogen bond networks. We have successfully synthesized substituted imogolite with methyl groups (Me-imo) instead of inner hydroxyl groups. While imogolite prefers zigzag chirality, Me-imo prefers armchair chirality which was confirmed by the simulation and the x-ray diffraction (XRD) pattern. Me-imo has larger specific surface area and less hydrogen bond contribution than that of imogolite, which was confirmed by the Barrett-Joyner-Halenda (BJH) pore size distribution.     

Synthesis and crystal structure of bis(2-methylbenzimidazolium) tetrahalocuprate(II)

The crystal structures of 2-methylbenzimidazolium tetrahalocuprates (H2-mebz)₂[CuX₄] (X = Cl and Br) have been detemined. The chloride salt is monoclinic, P2₁/c, with a = 8.540(2) Å, b = 16.591(2) Å, c = 14.303(3) Å, and = 98.69(2)°. The bromide salt is also monoclinic, P2₁/c, with a = 8.316(3) Å, b = 17.436(3) Å, c = 14.747(3) Å, and = 98.82(3)°. Both the compounds contain discrete distorted tetrahedral CuX₄ ^2– anions and almost planar 2-methylbenzimidazolium cations. In the chloride salt, three chloride ions are involved in hydrogen bonding instead of two bromide ions in the bromide salt.