Structure of 4,4′-butane-(1,4,7-three-p-tolylsulphonyl-1,4,7-three amine) diphthalonitrile

Abstract

The crystal structure of the title compound, C₄₁ H₃₅ N₇ O₆ S₃ was determined as monoclinic by single crystal X-Ray diffraction technique. The molecular structure was identified by IR, ¹H-NMR, ¹³C-NMR and elemental analysis. The crystal parameters of this compound are as follows: monoclinic P 2 1/n, a = 12.694(2) Å, b = 26.204(2) Å, c = 13.005(2) Å, β = 102.95(2)°, V = 4216.02(1) Å.³, Z = 4, Dx = 1.289 g/cm³, F(000) = 1704, λ (MoKα) = 0.71070 Å, μ = 0.2 mm^?1. The structure was solved by SHELXS-97 and refined by SHELXL-97. R = 0.06 for 3178 observed reflections with I > 2σ (I).     

Structure of Quinoline-4-Carboxaldehyde-2,4-Dinitrophenyl-N Methylhydrazone

Abstract

The crystal structure of the title compound, C₁₇H₁₃N₅O₄, has been determined by single crystal x-ray diffraction at room temperature. The molecule is not planar, with dihedral angles of 7.2(1)° between the quinoline ring and N-methylhydrazone group, and 17.45(2)° between the N-methylhydrazone group and the phenyl ring. The crystal parameters of this compound are as follows: monoclinic P 21/n, a=9.525(2)Å, b = 15.192(2) Å, c = 11.302(2) A, β = 94.722(3)°, V = 1629.8(6) ų, Z = 4, Dx = 1.432 g/cm³, F(000) = 728, λ (MoKα) = 0.71070 Å, μ = 0.106 mm^?1, R_int = 0.017. The structure was solved by SHELXS-86 and refined by SHELXL-93. R = 0.07 for 2438 observed reflections with I > 2σ (I).     

Structure of 5-Allyl-2-hydroxy-3-methoxyazobenzene

Abstract

5-allyl-2-hydroxy-3-methoxyazobenzene was preperad by the reaction of 4-allyl-2-methoxyfenol and benzenediazoniumchloride and crystallized from dimethylsulphoxide to yield crystals suitable for analysis. The molecular structure was identified by UV-VIS, IR, ¹H-NMR, ¹³C-NMR and elemental analysis. The crystal structure of the title compound was determined as monoclinic by by single crystal X-Ray diffraction technique. The crystal parameters of this compound are as follows: monoclinic P 2 1/n, a=5.559(2) Å,b=14.900(2) Å, c= 17.573(29 Å, P = 98.58(1)?, V = 1439.3(2) ų, Z = 2, Dx = 0.610 g/cm³, F(OOO) = 284, λ (MoKα) = 0.71070 Å, μ = 0.041 mm^?1. The structure was solved by SHELXS-86 and refined by SHELXL-93. R = 0.09 for 1107 observed reflections with I > 2σ (I).     

Crystal Structures of Tetrakis‐(4‐chlorophenylthio)‐butatriene and Tetrakis‐(tert‐butylthio)‐butatriene

Tetrakis‐(4‐chlorophenylthio)‐butatriene (3a) and tetrakis‐(tert‐butylthio)‐butatriene (3b) were synthesized, and their crystal structures were determined. The compound 3a is monoclinic, space group P2₁/c, a=6.9785(8), b=8.6803(9), c=22.884(2) Å, β=93.887(6)^o, V=1383.0(3) ų, Z=2. The compound 3b is monoclinic, space group P2₁/n, a=11.0615(6), b=10.8507(4), c=11.2717(6) Å, β =116.427(2)^o, V=1211.5(1) ų, Z=4. The title compounds 3a and 3b reside on an inversion center so that only half of the molecule is crystallographically unique. Both compounds are not planar. The crystal structures of 3a and 3b have cumulated double bonds. The C7–C8–C8ⁱ and C5–C6–C6ⁱ angles that show the linearity in both structures, respectively, are 176.4(3)° in 3a and 175.6(2)° in 3b.     

Trissarcosine barium(2 + ) dibromide—a new complex of N‐methylglycine

We obtained a new complex containing sarcosine (CH₃NH₂⁺CH₂COO⁻) and barium(2 + ) dibromide (TSBB) in 3:1 molar ratio, as well as its deuterated analog. Single‐crystal X‐ray diffraction measurements show that TSBB crystallizes in the monoclinic system, space group P2(1)/c. The unit cell parameters are as follows: a = 18.345(4) Å, b = 10.668(2) Å, c = 8.9212(18) Å, β = 91.86(3)°, and Z = 4. The structure was determined with final R₁ = 0.0396 (for I > 2σI). The crystal possesses a pseudohexagonal symmetry down c axis showing the resemblance to the crystal structure of trissarcosine calcium chloride (TSCC). There are N HBr hydrogen bonds (HB) of six types. TSBB crystal undergoes a phase transition at 416 K (heating)–415 K (cooling) of continuous nature. The spectroscopic [Infrared (IR) and Raman] investigation of the crystal was performed at room temperature. The results are discussed with respect to the crystallographic data, as well as the results obtained for TSCC crystal. Copyright © 2008 John Wiley & Sons, Ltd.     

Precious Metals - Part 2 - The Spectroscopic Characterisation and X-Ray Crystal Structure of Pd2(Pph3)3Cl5O

This work is on the synthesis and characterisation of a new phosphine stabilised palladium compound. the compound was first obtained from the rejects of cluster syntheses stored in the laboratory. Later on, it was prepared from PdCl₂ and triphenyl phosphine. the compound was characterised by ³¹P {¹H} NMR, UV/visible spectroscopy and elemental analysis. the crystal and molecular structure of Pd₂(PPh₃)₃Cl₅O was determined by X-ray analysis. the compound crystallizes in orthorhombic space group Pbca, N° 61, a = 19.009(2)Å, b=22.283(2)Å, c=23.726(2)Å, V=10050(20)ų, Z=8 residuals R[I>2σ(I)]=0.0457 and R(all) = 0.0636, MoKα radiation, 20 °C.     

Synthesis,crystal structure and electrical properties of (C5H13NCl)2 SnCl6

In this work, a novel compound Bis(2-chloropropyl-N,N-dimethyl-1-ammonium) hexachloridostannate(IV) was synthesized and characterized by; single X-ray diffraction, Hirshfeld surface analysis, differential scanning calorimetric and dielectric measurement. The crystal structure refinement at room temperature reveled that this later belongs to the monoclinic compound with P2₁/n space group with the following unit cell parameters a = 7.2894(7) Å, b = 12.9351(12) Å, c = 12.2302(13) Å and β = 93.423 (6) °. The structure consists of isolated (SnCl₆)^2? octahedral anions connected together into layers via hydrogen bonds N–H….Cl between the chlorine atoms of the anions and the hydrogen atoms of the NH groups of the [C₅H₁₃NCl]⁺ cations. Hirschfeld surface analysis has been performed to gain insight into the behavior of these interactions. The differential scanning calorimetry spectrum discloses phase transitions at 367 and 376.7 K. The electrical properties of this compound have been measured in the temperature range 300–420 K and the frequency range 209 Hz–5 MHz. The Cole–Cole (Z′ versus Z″) plots are well fitted to an equivalent circuit model. The transition phase observed in the calorimetric study is confirmed by the change as function of temperature of electrical parameter such as the conductivity of grain (σ_g) and the σ_dc.     

Synthesis,crystal structure and dielectric properties of C6H18N2SbCl5

The result of the X‐ray diffraction, differential scanning calorimetry and dielectric studies on a new crystal material C₆H₁₈N₂SbCl₅ is presented. The new organic–inorganic compound has been synthesized and characterized by the X‐ray diffraction method at 296(2) K. It crystallizes in the monoclinic P21/n space group. The cell dimensions are: a = 5.8617(1) Å, b = 15.7069(2) Å, c = 16.6693(2) Å, β = 97.627(1)° and Z = 4. The crystal structure consists of a discrete ionic layer of (C₆H₁₈N₂)²⁺ cations and [SbCl₅]^2? anions linked via simple and bifurcated N―H · · · Cl hydrogen bonds. DSC analysis shows that this compound undergoes a phase transition at about (384 ± 2) K. AC and DC conductivities, complex dielectric permittivity ε*(ω) and complex electrical modulus M*(ω) were respectively studied as temperature and frequency functions. The combined data support each other and confirm the existence of a structural phase transition at about 384 K. Moreover, the temperature dependence of the DC conductivity and relaxation frequency followed the Arrhenius relation. The frequency dependence of the real part of the AC conductivity in both phases follows the Jonscher's universal dynamic law: . The behavior of s(T) with temperature suggests that the hopping over barrier model (CBH) and the small polaron tunneling mechanism (SPTM) prevail in phases I and II, respectively. Copyright © 2016 John Wiley & Sons, Ltd.     

Mössbauer spectra and molecular structure of spin-crossover iron (III) complexes of monoclinic form with hexadentate ligands derived form triethylenetetramine and salicylaldehyde [Fe(sal2trien)]BPh4·acetone

Iron (III) complexes of [FeL]BPh₄·acetone containing the hexadentate ligand derived from triethylenetetramine and salicylaldehyde have been synthesized. These complexes were grown in two crystalline forms; monoclinic and twin crystals. The spin-state interconversion rate of the monoclinic form is as fast as the inverse of the Mössbauer lifetime (1×10^?7 s) above 200 K. The crystal structure of the monoclinic form (complex a) was determined at 290 K and to be of space group P2₁/a, with a=27.418 (4), b=10.097 (2), c=14.726 (3) Å, β=98.00 (1)°, and Z=4. The average bond distances of Fe?O (1.875 Å), Fe?N_imine (1.988 Å) and Fe?N_amine (2.069 Å) are in good agreement with the expected values for the transition spin-state between high- and low-spin states. Twin crystals are in a high-spin state over the temperature range 78–320 K.     

Structural characterization,spectroscopic, thermal,AC conductivity and dielectric properties and antimicrobial studies of (C8H12N)2[SnCl6]

A new inorganic-organic hybrid material produced from 2,6-dimethylanilinium cations and tin halide (SnCl₆)^2? has been synthesized and structurally determined by X-ray diffraction method. The title compound crystallizes in the monoclinic system, space group C2/m with a = 19.8772(4), b = 6.9879(1), c = 8.3001(2) Å, β = 98.487(2)° and V = 1140.26(4) ų. The crystal structure is built up of sheets of (SnCl₆)^2? octahedral anions and 2,6-xylidinium cations. The optical band gap was calculated and found to be 4.11 eV. At high temperature this compound exhibits a structural phase transition at 338 K. This has been characterized by differential scanning calorimetric and dielectric studies. Measurements of AC conductivity as a function of frequency at different temperatures indicated the hopping conduction mechanism. The bioassay results showed that the structure exhibits significant antibacterial activity.     

Crystal structure of the high-pressure modification of LaNbO4

Abstract

The crystal structure of the metastable LaNbO₄ high-pressure modification (HPM) has been studied by X-ray powder diffraction. It was found that the crystal structure of HPM LaNbO₄ belongs to- the room temperature BaMCF₄ -type structure (space group Cmc2₁, a = 3,941(1)Å, b= 14,460(4) Å, c = 5,681(2) Å, Z = 4).     

A new molecular C60 complex with bis(methylenedithio)tetrathiafulvalene (BMDT-TTF): Synthesis, crystal structure, and properties

A new molecular C₆₀ complex of the composition (BMDT-TTF) · C₆₀ · 2CS₂ (I) with the bis(methylenedithio)tetrathiafulvalene (BMDT-TTF) organic donor is synthesized. The molecular and crystal structures of this complex are determined by x-ray diffraction. The (BMDT-TTF) · C₆₀ · 2CS₂ (I) compound crystallizes in a monoclinic crystal system. The main crystal data are as follows: a=13.550(5) Å, b=9.964(7) Å, c=17.125(8) Å, β=99.52(4)°, V=2280(2) ų, M=1229.45, and space group P2₁/m. Crystals of I have a layered structure: layers consisting of C₆₀ molecules alternate with layers composed of BMDT-TTF and CS₂ molecules. It is found that, in complex I, the donor and C₆₀ molecules are linked through the shortest contacts, which leads to a change in the molecular geometry of BMDT-TTF. The donor molecules in a crystal layer are characterized by the shortest S...S contacts. The IR data indicate the electroneutrality of the fullerene molecule. The electrical conductivity of (BMDT-TTF) · C₆₀ · 2CS₂ single crystals is measured using the four-point probe method at room temperature: σ_RT=2×10^?5 Ω^?1 cm^?1.     

Pressure-dependent phase transition in the ordered BaBi0.7Nb0.3O3 perovskite

BaBi_0.7Nb_0.3O₃, an ordered perovskite, crystallizes in a centrosymmetric rhombohedral structure with the space group R3¯. The refined cell parameters obtained from synchrotron powder X-ray diffraction data for the rhombohedral phase at ambient pressure are a=6.109 (2) Å and α=60.3 (1)°. The pressure-dependent synchrotron powder X-ray diffraction studies show a phase transition around 8.44±1 GPa, where it transforms from rhombohedral structure to a monoclinic structure. The lattice parameters obtained for the monoclinic phase at a pressure of 15±1 GPa are a=5.91 (2) Å, b=6.25 (3) Å and c=8.22 (1) Å with monoclinic angle, β=88 (1)°.     

X-ray structure analysis of trans-1,4-polybutadiene

The crystal structure of trans-1,4-polybutadiene has been reported by Natta et al. to be pseudo-hexagonal below its solid-phase transition temperature. In the present X-ray structure analysis, it is revealed that the crystal belongs to the monoclinic system with the space group P2¹/a. The unit cell, with the lattice constants a = 8.63 Å, b = 9.11 Å, c = 4.83 Å, and β = 114°, includes four molecular segments.     

Crystal structure,spectroscopy and magnetism of binuclear complexes of mercury and lanthanides; the Ln(NCS)(HMPA)4(μ-SCN)2HgCl(SCN) type

A series of lanthanide compounds of type Ln(NCS)(HMPA)₄,(μ-SCN)₂HgCl(SCN) (Ln = Pr, Nd, Eu) were synthesized and grown in the form of single crystals.

The crystal structure of the neodymium complex was determined by X-ray diffraction. Its space group is Cc, with the following unit cell parameters; a = 17.338(3) Å, b = 15.795(3) Å, c = 21.828(4) Å, β = 107.65(3)°. The structure has an unexpected architecture in which one Cl^? ion, four SCN^? ions, and four oxygen atoms of HMPA groups are engaged in the metal ion coordination.

The binuclear complex is composed of two types of subunits; seven coordinated Nd (III) and four coordinated Hg (II). The results obtained were compared with the earlier published data on the crystal structures of polynuclear complexes with ions of the IIa group (Zn or Cd). Luminescence, excitation of luminescence and absorption spectra of lanthanide (Pr, Nd, Eu) single crystals, as well as vibrational IR and Raman spectra at 293, 77 and 4K, were recorded. Non-trivial results of reabsorption of the d-level of Pr(III) emission by ³H₄ → ³ P_J, ₁D² transitions were observed with simultaneous detection of emission from the ³P₀ level after excitation in the UV region. The experimental oscillator strengths of the transitions were determined from the absorption spectra and parametrized in terms of the Judd-Ofelt intensity parameters Ω_λ (λ = 2, 4, 6).

Satisfactory results for the calculation with low errors of estimation of the parameters were obtained for a crystal of the Nd-Hg compound, which reproduced the intensities of the electronic transitions well. Positive values of Ω_λ were evaluated for Pr(III) after including the ³H₄ → ³F₂ hypersensitive transition (obeying selection rules δJ = 2, δL = 2) in the calculations.

Based on the above results, the radiative rate constant can be determined. Strong vibronic components were found in the low temperature spectra for both types of ligands involved in metal ion coordination. The vibronic transitions are mainly associated with modes of groups directly coordinated to the metal ions. Electron-phonon coupling including the resonant vibronic effect was analysed based on IR and Raman data.

Magnetic susceptibility measurements were carried out down to 1.7 K. Correlation of the spectra and magnetic properties with details of the structure of the title compound was studied.     

Syntheses and structure characterization of inorganic/organic coordination polymers: Ag(dpa), Co(O3PH)(4,4′-bpy)(H2O), Zn(O3PH)(4,4′-bpy)0.5 and Mn[O2PH(C6H5)]2(4,4′-bpy) (dpa=2,2′-dipyridylamine; 4,4′-bpy=4,4′-bipyridine)

Four novel coordination polymers: Ag(dpa) I, Co(O₃PH)(4,4′-bpy)(H₂O) II, Zn(O₃PH)(4,4′-bpy)_0.5 III and Mn[O₂PH(C₆H₅)]₂(4,4′-bpy) IV (dpa=2,2′-dipyridylamine; 4,4′-bpy=4,4′-bipyridine), were synthesized by microwave heating and characterized by X-ray crystallography. I crystallizes in monoclinic space group P21/n with a=11.576(2) Å, b=5.585(2) Å, c=15.243(4) Å, β=109.00(2)°, V=931.8(3) ų. II crystallizes in monoclinic Cc space group with a=22.477(7) Å, b=5.280(1) Å, c=10.404(4) Å, β=96.08(3)°, V=1227.8(7) ų. III crystallizes in monoclinic P21/c space group with a=9.758(2) Å, b=7.449(3) Å, c=10.277(2) Å, β=100.02(2)°, V=735.6(4) ų. IV crystallizes in monoclinic space group P2/c with a=10.174(1) Å, b=11.817(3) Å, c=18.784(4) Å, β=102.14(1)°, V=2207.8(8) ų. I consists of linear metal–metal chains wrapped by dpa ligands. II and III consist of two-dimensional M^II(O₃PH) inorganic sheets cross-linked by 4,4′-bpy ligands, while IV is formed by Mn[O₂PH(C₆H₅)]₂ sheets cross-linked by 4,4′-bpy ligands. I exhibits two-step thermal decomposition at ~200 and ~250°C, resulting in the reduction of Ag⁺ to Ag metal. II loses its coordination water at ~100°C, leaving vacant coordination sites at Co²⁺ ions, while the original framework remains intact. The removal of 4,4′-bpy in II–IV occurs at elevated temperatures above 250, 200 and 400°C respectively.     

Synthesis,Crystal Structure,and Magnetic Properties of the YbFeTi<Subscript>2</Subscript>O<Subscript>7</Subscript> Compound

We report on the synthesis conductions and results of experimental investigations of the crystal structure and magnetic properties of a new magnetic compound YbFeTi₂O₇. According to the X-ray diffractometry data, the crystal structure of the investigated compound is described by the rhombic space group Pcnb with unit cell parameters of a = 9.8115(1) Å, b = 13.5106(2) Å, and c = 7.31302(9) Å and atomic disordering in the distribution of iron ions Fe³⁺ over five structural sites. The magnetic measurements in the lowtemperature region revealed a kink in the temperature dependence of the magnetic moment and its dependence on the sample magnetic prehistory. The experimental results obtained suggest that with a decrease in temperature the sample passes from the paramagnetic state to the spin-glass-like magnetic state characterized by a freezing temperature of T _f = 4.5 K at the preferred antiferromagnetic exchange coupling in the sample spin system. The chemical pressure variation upon replacement of rare-earth ion R by Yb in the RFeTi₂O₇ system does not change the crystal lattice symmetry and magnetic state.     

NdNi2Ge2化合物的结构和电磁输运性质

利用非自耗真空电弧熔炼法制备了NdNi₂Ge₂化合物样品,采用X射线粉末衍射技术和Rietveld全谱拟合分析方法测定了其晶体结构. 结果显示该化合物的空间群为I4/mmm,点阵参数为:a=4.120(1),c=9.835(0),Z=2,Nd原子占据2a晶位,Ni原子占据4d晶位,Ge原子占据4e晶位. NdNi₂Ge₂化合物呈现顺磁性,应用居里-外斯定律拟合计算得到居里-外斯常数为25.8,居里-外斯温度为6.24 K. 有效势磁矩为3.69μ_B,这与理论计算Nd³⁺的磁矩相符,表明磁矩主要源于Nd³⁺. 电阻率变化范围为0.3 Ω ·μm^-1-1 Ω ·μm,电阻曲线拟合显示NdNi₂Ge₂呈半金属性. 关键词： 2Ge₂')" href="#">NdNi₂Ge₂ Rietveld结构精修 电磁输运     

A Rule Governing Crystallization of Configurationally Directional Polymers: The Crystal Structure of the α and β Forms of Polypivalolactone

A “Rule” is proposed for incorporation of polymer chains having directional configuration, e.g. A‐B‐C‐A‐B‐C, into a crystal. Crystallization into a lamella morphology, as in slow crystallization from the melt, will incorporate antiparallel sequences (↑↓↑↓↑↓). Formation of a fiber by drawing the lamellar morphology must produce a different crystal structure containing parallel directional sequences. The drawn fiber must be polymorphic with a disordered aggregation of antiparallel and parallel crystal polymorphs. An example of this rule is found in the crystal structure of polypivalolactone. The melt crystallized α form is monoclinic, P2₁/c with a=9.05Å, b (fiber axis)=5.97Å, c=11.69Å, β=121.4° and consists of planar antiparallel sequences. The molecular conformation is a folded zig‐zag arrangement. On drawing a fiber, a disordered second phase of parallel plus antiparallel sequences is created. The chain conformation is a slightly distorted extended zigzag. The crystal structure of the directionally disordered β form is metrically monoclinic, with a=5.95Å, b=10.32Å, c (fiber axis)=4.94Å, β=101.3°. Examples of several classes of crystalline polymers demonstrating this Rule are presented.     

15N Isotopic Effects on the Raman Spectra of Tribromoacetamide

Abstract

¹⁵N-Tribromoacetamide has been synthesized with an isotopic content of 99, 4%, its Raman spectra have been recorded in the range 4.000–50 cm^?1. The isotopic shifts arising from ¹⁵N have been determined and interpreted. We have assigned the vibrational spectra of Br₃CCONH₂ and some overtones, combinations and difference bands. The molecular structure of tribromoacetamide has been studied employing the Ab Initio teoretical calculations and the Teller - Redlich isotopic product rule has been applied by assuming these geometrical parameters:

rCN = 1.4623 Å, rCC = 1.6014 Å, rBrC = 1.9468 Å, rCO = 1.2144 Å, rNH = 1.0292 Å, C-C-Br = 108.83320, C-C-0:118.2440, C-C-N:120.4137, C-N-H:110.45930