共查询到20条相似文献,搜索用时 31 毫秒
1.
Sema Özturk Şamil Işik Erbil Aguar Selami Şalsmaz H. K. Fun Ahmet Erdönmez 《光谱学快报》2013,46(2):245-254
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). 相似文献
2.
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) Å3, Z = 4, Dx = 1.432 g/cm3, F(000) = 728, λ (MoKα) = 0.71070 Å, μ = 0.106 mm?1, Rint = 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). 相似文献
3.
Şamil IŞlik Muhittin Aygün Selami Işaşmaz Tahir M. Nawaz İsmail E. Gümrükçüoğlu Orhan Büyükgüngör 《光谱学快报》2013,46(8):1525-1549
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) Å3, 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). 相似文献
4.
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) Å3, 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) Å3, 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. 相似文献
5.
Monika Trzebiatowska‐Gusowska Anna Gagor Jan Baran Marek Drozd 《Journal of Raman spectroscopy : JRS》2009,40(3):315-322
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 HBr 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. 相似文献
6.
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)Å3, Z=8 residuals R[I>2σ(I)]=0.0457 and R(all) = 0.0636, MoKα radiation, 20 °C. 相似文献
7.
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 (σg) and the σdc. 相似文献
8.
Houda Kharrat Nizar Elfaleh Slaheddine Kamoun 《Journal of Physical Organic Chemistry》2016,29(10):532-543
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. 相似文献
9.
Yonezo Maeda Hiroki Oshio Yuichi Tanigawa Takayuki Oniki Yoshimasa Takashima 《Hyperfine Interactions》1992,68(1-4):157-160
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?Nimine (1.988 Å) and Fe?Namine (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. 相似文献
10.
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) Å3. 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. 相似文献
11.
Yu. A. Titov A. M. Sych A. N. Sokolov V. Ya. Markiv N. M. Belyavina A. A. Kapshuk 《高压研究》2013,33(3-4):175-181
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). 相似文献
12.
N. G. Spitsina V. V. Gritsenko O. A. D’yachenko É. B. Yagubskii 《Physics of the Solid State》2002,44(3):531-533
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) Å3, 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: σRT=2×10?5 Ω?1 cm?1. 相似文献
13.
BaBi0.7Nb0.3O3, 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)°. 相似文献
14.
Shigeo Iwayanagi Ikuko Sakurai Tosio Sakurai Tsuneo Seto 《Journal of Macromolecular Science: Physics》2013,52(2):163-177
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. 相似文献
15.
E. GAŁDECKA Z. GAŁDECKI J. CYBIŃSKA R. J. WIGLUSZ V. AMIRKHANOV J. LEGENDZIEWICZ 《Molecular physics》2013,111(7):1015-1027
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 PJ, 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 Ωλ (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 Ωλ 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. 相似文献
16.
《Journal of Physics and Chemistry of Solids》2001,62(9-10):1629-1642
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) Å3. 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) Å3. 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) Å3. 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) Å3. I consists of linear metal–metal chains wrapped by dpa ligands. II and III consist of two-dimensional MII(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. 相似文献
17.
T. V. Drokina G. A. Petrakovskii M. S. Molokeev D. A. Velikanov 《Physics of the Solid State》2018,60(3):532-536
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. 相似文献
18.
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3.69μB,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 相似文献
19.
Edward S. Clark 《Journal of Macromolecular Science: Physics》2013,52(6):1179-1189
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. 相似文献
20.
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 相似文献