Crystal structure, thermal analysis, and IR spectrometric investigation of 1,2-diammonium-2-methyl propane sulfate monohydrate

Chemical preparation, X-ray single crystal, thermal analysis, and IR spectrometric investigation of C₄H₁₄N₂SO₄·H₂O (denoted DAMPS) are described. DAMPS crystallizes in the orthorhombic system with P2₁2₁2₁ space group, a = 9.2726(4) Å, b = 9.5227(2) Å, c = 10.3807(4) Å, V = 916.62(6) ų, and Z = 4. The DAMPS structure is built up from inorganic chains parallel to the b axis and linked via Ow–H···O hydrogen bonds. These chains are interconnected by organic groups so as to build a three-dimensional arrangement.     

Structure, thermal behavior, and IR investigation of bis(3-amino-1,2,4-triazolium)monohydrogen monophosphate

Chemical preparation, calorimetric studies, crystal structure, and IR spectrometric investigation of (C₂H₅N₄)₂HPO₄, denoted ATZP, are described. The compound crystallizes in the monoclinic system with C2/c space group. Its unit cell dimensions are a = 13.589(2) Å b = 11.105(2) Å c = 15.734(3) Å = 104.68(2)°, V = 2296.8(7) ų, and Z = 8. The structure of the title compound consists of a three dimensional network of H-bonds connecting all its components. The IR spectrum of ATZP is reported and discussed on the basis of group theoretical analysis.     

Structure, thermal behavior, and IR investigation of a new organic sulfate

[1-(2-ammoniumethyl) piperazinium] sulfate denoted PIPS has a monoclinic unit cell. The parameters are: a = 6.6521(3), b = 7.8756(5), c = 19.197(1) Å, = 94.43(1)° and the space group is P2₁/n. The preparation, thermal analysis, and IR spectrometric investigation are described. The PIPS structure exhibits a complex three-dimensional network of H-bonds connecting all its components.     

Crystal structure and thermal analysis of 1,5-diammonium-2-methyl pentane sulfate monohydrate

Chemical preparation, x-ray single crystal, and thermal analysis of C₆H₁₈N₂SO₄·H₂O (denoted DMPS) are described. The compound crystallizes in the triclinic system with P space group. Its unit cell dimensions are a = 5.826(1) Å, b = 10.014(1) Å, c = 11.221(1) Å, = 66.716(1)°, = 84.395(1)°, = 83.759(1)°, V = 596.7(1) ų, and Z = 2. The DMPS structure is built up from inorganic chains parallel to the a axis and linked via O(W)-H···O hydrogen bonds. These chains are interconnected by organic groups. Thermal analysis reveals the presence of one water molecule in the structure and shows a reversible weak phase transition.     

Crystal structure,thermal analysis and IR spectroscopy investigations of N,N‐dimethyl‐1,3‐propanediammonium monohydrogenmonophosphate trihydrate

A new organic monohydrogenmonophosphate (C₅H₁₆N₂)HPO₄.3H₂O (abbreviate as MPAP) is prepared by reacting H3PO4 with N, N‐dimethyl‐1,3‐propanediamine. This compound crystallizes in the orthorhombic crystal system, space group Pca2₁. Unit cell parameters are a % 8.1445(1) Å, b % 11.7734(2) Å, c % 12.9021(2) Å, with, Z % 4 and ρ_m % 1.31 g cm⁻³. The structure was solved, using the direct methods and refined against F² to a reliability R factor of 0.0257. Three types of hydrogen bonds participate to the structural cohesion: O(P)—H…O, O(W)—H…O and N—H…O. The first one connects HPO₄ groups in infinite chains. This organization of the phosphoric groups creates voids in which are located the water molecules which are themselves connected by the second type of hydrogen bonds to the adjacent phosphoric groups that lead to a typical layer organization of a polyanion [HPO₄.(H₂O)₃ ]²ⁿ⁻_n. The third hydrogen bond type is responsible for the cohesion between the two‐dimensional polyanions. Thus, a framework in a threedimensional way is then created. The thermal decomposition of MPAP shows a large endothermic effect corresponding to the elimination of the water molecules and a set of endotherms which are probably due to the evolution of ammonia from the structure and the decomposition. The title compound was also characterized by IR spectroscopy, the interpretation of the spectra is based on theoretical analyses and literature data. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure,thermal behavior and IR investigation of 1,6‐diammonium hexan dihydrogenodiphosphate dihydrate

Physicochemical properties of (C₆H₁₈N₂)H₂P₂O₇·2H₂O denoted DHDP are discussed on the basis of X‐ray crystal structure investigation. The compound crystallises in the triclinic system with P space group. Its unit cell dimensions are a = 13.719(1) Å, b = 14.188(3) Å, c = 9.177(1) Å, α = 108.50(1)°, β = 91.11(1)°, γ = 115.47(1)°, V = 1503.8(4) ų and Z = 4. The structure has been solved using direct methods and refined to a reliability R factor 0.0401 for 4778 reflections. The main feature of the atomic arrangement of DHDP is the existence of infinite rows, parallel to the c direction of the unit cell, composed of H₂P₂O₇ groups. These phosphoric rows are organised to create, with the help of the organic cation, large rectangular channels in which the unstable water molecule are located since they have high thermal parameters. Phosphoric anions and organic cations have no internal symmetry. DSC and TG‐DTA show that dehydration occurs in one step. Such dehydration process may be related to the similar environments on the water molecules residing in the channel. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure,thermal analysis and IR spectrometric investigation of bis (2‐amino‐6‐methyl) pyridinium sulfate

The synthesis method, crystal structure determination, phase transitions studied by thermal analysis and IR spectrometric investigation of 2C₆H₉N₂⁺.SO₄^2– are reported. The compound crystallizes in the monoclinic space group C2/c (no. 15) with a = 10.5068(4) Å, b = 10.2225(5) Å, c = 14.0422(7) Å, and β = 104.489(3)°. The atomic arrangement can be described by layers built by all the components of the structure and centered by planes z = 1/4 and 3/4. The organic molecules form channels parallel to the c direction with dimensions of 4.163(1)Å and 5.148(4)Å. Thermal analysis shows that the anhydrous compound presents an irreversible weak phase transition. The IR study, based on theoretical analyses and on the literature data allows the interpretation of the IR spectrum. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure,thermal analysis,and IR spectroscopic investigation of bis(2-amino-6-methyl) pyridinium sulfate

Synthesis, crystal structure refinement, phase transitions studied by thermal analysis, and IR spectroscopic investigation of 2C₆H₉N₂ < eqid2 > ⋅SO₄²⁻ are reported. The title compound crystallizes in the monoclinic space group C2/c (no. 15) with a = 10.5068(4) Å, b = 10.2225(5) Å, c = 14.0422(7) Å, and β = 104.489(3)^∘. A crystal packing diagram shows layers built by all the components of the structure and centered by planes z = 1/4 and 3/4. The pyridine substituents stack forming channels parallel to the c direction with dimensions of 4.163(1) Å and 5.148(4) Å. Thermal analysis shows that the anhydrous compound possesses an irreversible weak phase transition.     

Crystal structure of a novel bis(guanidiniums) compound incorporated by sulfate anion

Crystal structure of a novel bis(guanidiniums) compound 1 by sulfate anion and water, C₁₁H₂₀N₆OSO₄H₂O, was measured by X-ray crystallographic analysis with an imaging plate method. It possesses space group P2₁/c, with a = 7.6433(15), b = 19.447(4), c = 12.115(2) Å, = 107.81(3)°, and _calc = 1.420 mg/m³ for Z = 4. Crystal data indicate that the architecture network is formed through hydrogen bonds, electrostatic interactions, and arene–arene stacking interaction among the bis(guanidiniums) compound, the sulfate anion and water molecule.     

Synthesis,structure and IR characterization of disodium tetra(9,10-dihydro-9-oxo-10-acridineacetato)zincate(II) bis(ethanol) heptahydrate

The synthesis, crystal structure and IR data are reported for Na₂[Zn(CMA)₄]·2EtOH·7H₂O, where CMA^– is the 9,10-dihydro-9-oxo-10-acridinacetate ion. The complex crystallizes in the monoclinic space group P2/n, with cell dimensionsa=17.335(9),b=8.440(5),c=21.875(12) Å, =91.94(5)°,Z=2. The structure was solved by direct methods and refined to a finalR value of 0.0363 for 3022 non-zero reflections. The Zn²⁺ ion occupies twofold axis and is coordinated to four carboxylate ligands, the ZnO₄ tetrahedron is considerably distorted with Zn–O distances of 1.978(3) and 1.961(3)Å. Each Na⁺ cation interacts with two water, one ethanol, and three carboxylate O atoms comprising distorted octahedron. The Zn²⁺ and Na⁺ cations are linked through monooxygen and syn-syn carboxylate bridges forming a trinuclear, mixed-metal cluster. The Zn...Na separation is 3.267(2)Å and Na...Na distance equals 3.520(2)Å. All oxygen bonded H-atoms are utilized in hydrogen bonds. The acridone rings overlap in the crystal with the 3.5 Å interlayer separations. The compound has been characterized by IR spectroscopy.     

Tris-(thiocyanato)-bis-(hexamethylenetetramine)-nona-(aquo) lanthanum(III): synthesis, crystal structure, IR and Raman characterization

The title compound (LaC₁₅H₄₂N₁₁O₉S₃) was prepared and characterized by means of X-ray, IR and Raman measurements. The crystals are orthorhombic: Pnma (No. 62), a = 21.117(2), b = 14.736(2), c = 10.082(1) Å, and Z = 4. The structure consists of polyhedra with a La(III) ion in the center of them and hexamethylene molecules, which link these polyhedra. Each La(III) ion coordinates seven molecules of water and two thiocyanate ions via nitrogen atoms. The IR and Raman spectra, which have been obtained and interpreted, are in good agreement with X-ray results.     

Synthesis, Crystal Structure, Thermal Behavior and IR Characterization of Pentacarbonyl(4-methylpyridine)chromium(0) Complex

Abstract  Pentacarbonyl(4-methylpyridine)chromium(0) complex was isolated from n-hexane solution as yellow plate-like crystals and characterized by using X-ray crystallography. It crystallizes in the orthorhombic system with the space group Cmcm and Z = 4. The unit cell parameters are a = 11.737(1) ?, b = 12.857(2) ?, c = 8.465(1) ?. The single crystal X-ray structure of the complex shows that the coordination sphere around the chromium central atom is slightly distorted octahedron, involving the 4-methylpyridine (4-mp), ligand as a monodentate N-donor ligand and five carbonyl groups. The four equatorial CO groups in the complex, with the Cr–C2 distance of 1.886 Ǻ, are slightly bent away from the 4-methylpyridine ligand with the N–Cr–C2 angle of 91.69°. The pyridine ring plane makes an angle of 135.17° with the Cr–N–CO bond axis. The thermal analysis (differential thermal analysis and thermal gravimetry) and IR spectra of the complex indicated that the compound undergoes complete decomposition to form the Cr₂O₃ as the final decomposition product. Index Abstract  The crystal structure of pentacarbonyl(4-methylpyridine)chromium(0) complex has been determined and its thermal behavior has also been studied.      

Crystal structure and spectroscopic characterization of bis(N-phenylthiourea)

Bis(N-phenylthiourea) (BPTU) has been synthesized and characterized by means of X-ray, IR, Raman, UV-Vis, ¹H NMR, and FAB mass spectra. The BPTU crystal belongs to the monoclinic C2/c space group with the cell constants a = 26.992(8) Å, b = 6.336(3) Å, c = 9.463(3) Å, = = 90°, = 105.97(7)°, Z = 4. The compound has been found to exist in the thione form, with cis configuration of the thiosemicarbazone moiety and skew conformation of the molecule.     

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 structure and EPR spectra of glycilglycilglycinocopper(II)bromide sesquihydrate

The title compound, Cu(glyglygly)Br·1·5H₂O, crystallizes in the space group C2/c, with a = 21.468(7), b = 6.716(5), c = 16.166(6) Å, = 98.39°, and Z = 8. The tripeptide is bonded to one Cu(II) ion through the nitrogen [Cu–N=1.97(1)Å] and oxygen [Cu–O=2.019(8)Å] atoms of the amino end glycine residue and to another Cu(II) through one oxygen atom [Cu–O=1.931(9)Å] of the terminal carboxyl group. This give rise to covalently bonded and infinite ···–Cu–tripeptide–Cu–··· chains. These chains are linked to one another by a network of H-bonds involving the water molecules and bromide ions. The Cu(II) ion is in a distorted tetragonal pyramidal coordination polyhedron. At the corner of the base of the pyramid are the terminal glycine nitrogen and oxygen atoms of one tripeptide, a carboxylic oxygen of another tripeptide and a bromide ion. The fivefold coordination is completed with a water molecule at the top of the pyramid [Cu–Ow=2.286(9)Å]. For all orientations of the applied magnetic field the single crystal EPR spectra display a single anisotropic exchange collapsed resonance without hyperfine structure. Its position was measured in three perpendicular planes and the crystal g-tensor evaluated from the data. This tensor is interpreted in terms of the contributing Cu(II) complexes in the unit cell to deduce the principal values g₁ = 2.273, g₂ = 2.050 and g₃ = 2.131 for the molecular gyromagnetic tensor. We also discuss the magnitude of the exchange interaction between neighboring copper ions in the lattice on the basis of the features in the EPR spectra and the structural information.     

Crystal and molecular structure of trans-bis(dodecylamine) bis(dimethylglyoximato)cobalt(III) nitrite

An octahedral geometry for the molecule of the title complex with very slight distortions around Co(III) is confirmed by single-crystal X-ray diffraction study. The molecular structure of the complex has been shown to contain two dodecylamine moieties in the trans orientations, two N-bonded dimethylglyoximato (DMG) groups and an uncoordinated nitrite ion.     

The crystal and molecular structure of ammonium-bis(malonato) oxovanadium(IV) dihydrate

The title compound, (NH₄)₂[VO(C₃H₂O₄)₂]·2H₂O, crystallizes in the monoclinic space group P2₁/n, with a=7.1889(7), b=19.254(2), c=9.879(2) Å, β=108.19(1)^o, and Z=4. The VO²⁺ cation is five-fold coordinated with two malonate anions acting as bidentate ligands and a water molecule. Infrared and Raman spectra are also reported to attain a wider insight into the compound characteristics.     

Crystal structure of aluminum sulfate hexadecahydrate and its morphology

A single‐crystal structure of aluminum sulfate hexadecahydrate (Al₂(SO₄)₃·16H₂O) was captured with a polarizing microscope. The structure was similar to a hexagonal plate and consistent with the predicted morphology derived from the modified AE model. An octagonal plate morphology was first obtained in a vacuum but was transformed into hexagonal plate‐like when the effect of the solvent with two disappearing {1 1 0} and {1 0 −1} faces was considered.     

Synthesis, characterization, and crystal structure of 1-(4-chloro-benzoyl)-3-naphthalen-1-yl-thiourea

1-(4-Chloro-benzoyl)-3-naphthalen-1-yl-thiourea has been synthesized and characterized by elemental analysis, IR spectroscopy, and mass spectrometry. The crystal and molecular structure of the title compound has been determined from single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1, with a = 6.962(1) Å, b = 10.770(3) Å, c = 11.738(2) Å, = 65.76(2)°, = 80.03(1)°, = 84.86(2)°, and D _calc= 1.432 g cm^–1 for Z = 2. The thermal behavior of the compound has been studied by DTA and TG. The antibacterial activities of the title compound were investigated for three Gram (+) and two Gram (–) bacteria by employing broth microdilution method and subsequently, inhibitory activity against yeast-like fungi was also determined.     

Crystal growth and characterization of PbI2‐AgI binary system

The crystals of the binary system PbI₂‐AgI (PIAI) were obtained by heating the mixture of individual PbI₂ (PI) and AgI (AI) placed at 30° angle in the horizontal tubular furnace of variable temperature zone. The crystals were characterized by powder XRD, TG/DTA, FT‐IR and SEM. The 3.37% weight loss in the sample after heating at 853 K is due to the presence of water molecules absorbed (3446 cm^–1) by the crystals during sintering and cooling process. The cell parameters of the crystal were determined using the powder X‐ray data. The PbI₂‐AgI crystallizes in monoclinic system a = 10.799 (±0.009), b = 7.492 (±0.004), c = 6.929(±0.004) Å and α = 90°, β = 108.04(±0.073) γ = 90°, V = 533.18 ų. The electrical conductivity measurements of the crystals showed a sudden change in the current value at the temperature range 385–393 K. The activation energy before and after the drift was found to be 0.49 and 0.35 eV respectively. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)