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1.

Abstract  

4-((1,3-Dioxoisoindolin-2-yl)methyl)-1-methoxypyridinium tetrafluoroborate, C15H13BF4N2O3, 1, was obtained by alkylation of the corresponding N-oxide and has been characterized by 1H and 13C NMR, IR, UV spectroscopy and by X-ray crystallography. The crystal undergoes a reversible phase transition between 173 and 293 K. At room temperature, crystals are orthorhombic, space group Pna21 with a = 7.2487(3) ?, b = 17.8359 (8) ?, c = 12.4077(6) ?, V = 1604.16(12) ?3, and Z = 4. At 173 K, cations adopt four conformations in monoclinic space group Cc with a = 24.7076(29) ?, b = 14.4145(9) ?, c = 21.8765(25) ?, β = 126.249(17)°, V = 6283.3(7) ?3, and Z = 16. The compound is photostable in the crystal and does not undergo homolytic N–O bond cleavage as observed in solution.  相似文献   

2.
Abstract  The compound, 7-chloro-5-cyclopropyl-9-methyl-10-(2-piperidin-1-yl-ethyl)-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one, C22H26N5ClO, crystallizes in the triclinic space group Pī with cell parameters a = 8.918(7) ?, b = 9.297(7) ?, c = 14.184(8) ?, V = 1095.98(1) ?3 and Z = 2. The final residual factor R 1 = 0.0451. The structure exhibits intermolecular hydrogen bonds. The 2-piperidin-1-yl-ethyl ring adopts a chair conformation. The starting material used to synthesize the title compound is the intermediate compound of well known anti-HIV drug Nevirapine hence the title compound is having biological importance and hence this crystal structure will helps to structural characterization of the molecule and also for the molecular modeling it will helps for biological study. Graphical Abstract  The title compound 7-chloro-5-cyclopropyl-9-methyl-10-(2-piperidin-1-yl-ethyl)-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one was synthesized by condensation of 7-chloro-5-cyclopropyl-9-methyl-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one with 1-(2-chloro-ethyl)-piperidine hydrochloride in presence of anhydrous powdered potassium carbonate as base using N,N-dimethyl formamide as solvent and its crystal structure determined. The title compound derived from bioactive molecule and it is also having biological importance hence this crystal structure will helps for the structural characterization and the biological study of the novel molecule.   相似文献   

3.

Abstract  

The title compound, a salt of C15H13N4 2+2Cl, was synthesized and determined by X-ray crystallography. It crystallizes in the orthorhombic system, space group Pbcn, with lattice parameters a = 9.973(2) ?, b = 9.5012(19) ?, c = 15.574(3) ?, V = 1475.8(5) ?3, Z = 4, C15H13Cl2N4, Mr = 320.19, Dc = 1.441 g/cm3. In the crystal structure, the Cl anion interact with the same benzimidzaole through two kinds of hydrogen bonds forming a 1D hydrogen-bonded chain, two 1D hydrogen-bonded chain cross with each other and form 2D layer structure. The EA, UV, IR and TG-DTG were studied and the possible structures of the title compound were speculated. Moreover, the fluorescence of the title compound was studied. The results reveal that it can emit purple fluorescence in DMF solvent.  相似文献   

4.

Abstract  

Crystal structures of two bis-phenols namely bis-(3,5-dimethyl-2-hydroxyphenyl)(3-amino phenyl)methane 1 and bis-(3,5-dimethyl-4-hydroxyphenyl)(3-aminophenyl) methane 2 are determined. The compound 1 crystallises in monoclinic P21/c with a = 12.2579(16) ?, b = 16.0906(19) ?, c = 10.6664(13) ?, β = 115.417(7)°, V = 1900.2(4) ?3 whereas 2 crystallizes in monoclinic C2/c, a = 9.2538(2) ?, b = 18.6579(4) ?, c = 23.2725(5) ?, β = 98.796(2)°, V = 3970.89(15) ?3. The crystal lattice of both the compounds shows presence of N–H···π interactions but no O–H···π interactions.  相似文献   

5.

Abstract  

The reaction of cobalt (II) chloride hexahydrate and N-tert-butyl-2-thioimidazole (tmt-Bu) yielded products [k2-(tmt-Bu)2]CoCl2 (1) and [(tmt-Bu)2Co2(μ-tmt-Bu)2Cl2]·CH3CN (2) at different reaction time. The single crystal X-ray diffraction analysis was carried out for 1 and 2 {Bruker Kappa Apex-II CCD diffractometer, MoKα radiation}. Crystal data for 1: orthorhombic P212121 unit cell a = 8.195(6) ?, b = 13.778(10) ?, c = 17.354(11) ? and V = 1960(2) ?3 whereas the compound 2 crystallizes in monoclinic system P21/c with unit cell a = 10.069(7) ?, b = 11.181(7) ?, c = 18.156 ?, β = 95.322(4)° and V = 2035.4(2) ?3. The complex 1 contains one dimensional chain running along the a-axis and the complex 2 contains one dimensional chain running along the b-axis due to existence of different types of intermolecular interaction. The change in structure of the product is directly related to the reaction time i.e. reaction for lesser time produces mononuclear product and for longer time produces binuclear compound.  相似文献   

6.

Abstract  

Reactions of 4-chlorobenzohydrazide with 3-bromo-5-chloro-2-hydroxybenzaldehyde and 3,5-dichloro-2-hydroxybenzaldehyde, respectively, afforded two isostructural hydrazone compounds, C14H9BrCl2N2O2·CH3OH (1) and C14H9Cl3N2O2·CH3OH (2). Both compounds were structurally characterized by X-ray determination. Compound 1 crystallizes in the triclinic space group P − 1 with unit cell dimensions a = 7.462(1) ?, b = 9.281(2) ?, c = 12.626(1) ?, α = 98.451(2)°, β = 98.630(2)°, γ = 100.025(2)°, V = 837.8(2) ?3, Z = 2, R 1 = 0.0394 and wR 2 = 0.0967. Compound 2 crystallizes in the monoclinic space group P21/n with unit cell dimensions a = 7.485(1) ?, b = 13.389(2) ?, c = 16.693(2) ?, β = 99.754(2)°, V = 1648.7(4) ?3, Z = 4, R 1 = 0.0375 and wR 2 = 0.0900. X-ray structural determination revealed that each compound consists of a hydrazone molecule and a methanol molecule of crystallization. In the crystal structures of both compounds, the adjacent molecules are linked by methanol molecules through N–H···O and O–H···O hydrogen bonds, forming dimers.  相似文献   

7.

Abstract  

The structures of four spirobisnaphthalenes based monomers 1, 2, 3a and 3b are reported. Each compound represents a methoxylated precursor which after deprotection led to the formation of a monomer successfully used for the synthesis of Polymers of intrinsic microporosity. The spiro-centre represents the site of contortion that, since its rigidity, leads to inefficient packing in the solid state inducing microporosity in the final polymer. Compound 1 crystallized in the monoclinic P2/c space group with unit cell parameters a = 8.1659(19) ?, b = 7.5298(18) ?, c = 19.130(5) ?, β = 97.935(4)°, V = 1165.0(5) ?3, Z = 2, D = 1.210 Mg m−3. Compound 2 crystallized in the monoclinic P21/n space group with unit cell parameters a = 12.6940(9) ?, b = 7.7267(6) ?, c = 19.9754(15) ?, β = 97.220(1)°, V = 1943.7(3) ?3, Z = 4, D = 1.355 Mg m−3. Compound 3a crystallized in the monoclinic P21/c space group with unit cell parameters a = 16.8137(14) ?, b = 10.5577(9) ?, c = 31.344(3) ?, β = 103.618(1)°, V = 5407.5(8) ?3, Z = 8, D = 1.308 Mg m−3. Compound 3b crystallized in the monoclinic Pc space group with unit cell parameters a = 15.594 ?, b = 12.564 ?, c = 18.339 ?, β = 90.224(1)°, V = 3593.0 ?3, Z = 4, D = 1.236 Mg m−3.  相似文献   

8.

Abstract  

Two Br?nsted acid task specific ionic liquids based on the benizimidazolium cation (1-ethylbenzimidazolium tetrafluoroborate {[H-eBim]BF4 (1)} and 1-propylbenzimidazolium tetrafluoroborate {[H-pBim]BF4 (2)}) were synthesized and characterized. The crystal of 1 is in orthorhombic system with space group Pnma, and the unit cell parameters as follows: a = 9.9308(16), b = 6.8813(11), c = 15.345(3) ?, V = 1048.6(3) ?3, Z = 4, Dc = 1.482 g/cm3. Structure 2 crystallizes in the monoclinic space group P21/c, with unit cell a = 4.9688(14), b = 13.684(4), c = 17.295(5) ?, β = 92.090(6)°, V = 1175.2(6) ?3, Z = 4, Dc = 1.402 g/cm3. These molecules are stabilized in solid state by various intra and intermolecular hydrogen bonding interactions to give polymeric structures.  相似文献   

9.

Abstract  

The title compounds, C10H8N2·C15H16O2 (1) and C10H8N2·C14H10O5 (2), were synthesized by 4,4′-bipyridyl and two similar V-shaped molecules. The two complexes both crystallized in the same space group P21/n with the crystal cell parameters: a = 16.0536(3) ?, b = 6.42730(1) ?, c = 21.2717(4) ?, β = 102.330°, V = 2144.21(7) ?3, Z = 4 in compound 1 and a = 7.45020(10) ?, b = 10.0784(2) ?, c = 26.9430(5) ?, β = 92.1140(10)°, V = 2021.67(6) ?3, Z = 4 in compound 2. Compound 1 forms regular molecular chains containing alternative 4,4′-bipyridyl and 4,4′-isopropylidenediphenol units; the molecular components are linked by two types of O–H···N hydrogen bonds. Additionally, every two neighboring chains are connected to be a ladder structure by means of weak C–H···O interactions. In compound 2, 4,4′-bipyridyl and 4,4′-oxydibenzoic acid first construct one-dimensional architecture by strong O–H···N hydrogen bonds, which are similar with the interactions in compound 1. Secondly, two types of weak C–H···O contacts formed between 4,4′-bipyridyl and the acid link one-dimensional chains to be interlaced three-dimensional hydrogen-bonded networks.  相似文献   

10.

Abstract  

The synthesis and molecular structure of (phenoxathiin-4,6-dithiolate)tellurium(II) is described. [Te{S(C6H3S)2O}] was synthesized from the reaction of 4,6-dimercaptophenoxatiin and TeCl4 in 36% yield. The crystal structure was determined by single crystal X-ray diffraction analysis. Crystal data: [Te{S(C6H3S)2O}], formula weight = 389.95, crystallized in monoclinic system, space group P2(1)/n with a = 7.7898(10) ?, b = 18.513(2) ?, c = 8.9898(11) ?, β = 105.974(2)°, V = 1246.4(3) ?3 and Z = 4. The tetracyclic compound is non-planar with a di-coordinate TeII atom. The eight-membered central ring is in a boat–chair conformation. The title compound displays weak intermolecular contacts Te–S, S–S and C–H⋯S.  相似文献   

11.

Abstract  

The title compound [MeLiPrCoCH2Si(CH3)3 MeLiPr = 2,4-pentane-N,N′-bis(2,6-diisopropylphenyl) ketiminato] possesses trigonal planar geometry and crystallizes in monoclinic space group P21/n with crystal cell parameters a = 10.6155(14) ?, b = 21.279(3) ?, c = 14.8057(19) ?, β = 97.196(2)°, V = 3,318.1(7) ?3, and Z = 4. The title compound is the second reported three coordinated 13 valence electron Co(II) alkyl complex and the first such complex reported with an asymmetrically bonded alkyl group. The steric effects are discussed in comparison of known similar structures of Fe, Co, and Zn.  相似文献   

12.

Abstract  

The synthesis and characterization of some pyrazoline compounds of 1,3-diketones with hydrazine derivatives, namely, 1-(S-benzyldithiocarbazate)-3-methyl-5-phenyl-5-hydroxypyrazoline (1); 1-(2-thiophenecarboxylic)-3-methyl-5-phenyl-5-hydroxypyrazoline (2); 1-(2-thiophenecarboxylic)-3,5-dimethyl-5-hydroxypyrazoline (3); 1-(S-benzyldithiocarbazato)-3-methyl-5-phenylpyrazole (4); 1-(2-thiophenecarboxylic)-3-methyl-5-phenylpyrazole (5) and 1-(S-benzyldithiocarbazate)-3,5-dimethylpyrazole (6) are reported. Studies by IR, (1H, 13C)-NMR spectroscopies and single crystal X-ray diffraction revealed that compounds (1), (2) and (3) are formed as pyrazoline, whereas (4) and (5) are formed as pyrazole derivatives only under acidic conditions. Compound (1) crystallizes in orthorhombic P212121, a = 6.38960(10) ?, b = 12.9176(3) ?, c = 21.2552(5) ?, (2) crystallizes in monoclinic, P21/n, a = 11.3617(2) ?, b = 8.4988(2) ?, c = 92.8900(10) ? and β = 92.8900(5)°, (3) crystallizes in monoclinic, C2/c, a = 15.9500(5) ?, b = 9.3766(3) ?, c = 16.6910(5) ? and β = 113.825(2)°, (4) crystallizes in monoclinic, P21/c, a = 15.228(4) ?, b = 5.5714(13) ?, c = 19.956(5) ? and β = 91.575(7)° and (6) crystallizes in orthorhombic, P212121, a = 5.3920(2) ?, b = 11.2074(5) ?, c = 21.885(1) ?. The (3) derivative represents the first pyrazoline compound prepared from 2,4-pentanedione and characterized crystallographically.  相似文献   

13.

Abstract  

Erbium (III) coordination compound with the formula [Er(IN)3(H2O)2]n 1 (HIN = isonicotinic acid) was synthesized by mixing Er2O3 with isonicotinic acid under hydrothermal condition. The structure of the title compound was determined by single crystal X-ray diffraction analysis, which reveals that the 1-D chain-like structure is formed by the erbium polyhedra through the carboxyl groups of IN. It crystallizes in the monoclinic system, possesses space group C2/c, with lattice parameters: a = 20.229(10) ?, b = 11.594(6) ?, c = 9.871(5) ?, α = γ=90°, β = 115.509(6)°, V = 2089.3(18) ?3, and D calc = 1.811 mg/cm3 for Z = 4, F(000) = 1108, GOF = 1.109, R1 = 0.0675. Compound 1 has been characterized by IR absorption spectroscopy, ultraviolet excitation and emission spectrum.  相似文献   

14.

Abstract  

Synthesis and characterization of single crystals of a new organic Schiff-base derivative, N,N′-bis(2,3-dimethoxybenzylidene)-1,2-diaminoethane is reported. Good quality single crystals with size 10 mm × 1 mm × 1 mm were grown by slow evaporation technique from a methanol solution at room temperature. The grown crystals have been characterized by elemental analyses and functional groups were identified using FT-IR and 1H-NMR spectroscopy. Crystal structure of the title compound has been determined by single crystal X-ray diffraction. The title compound has a monoclinic symmetry, space group P21/c, lattice parameters are a = 4.4159(3) ?, b = 14.2333(9) ?, c = 15.0601(10) ?, β = 97.755(5)°, Z = 2, V = 937.91(11) ?3.  相似文献   

15.

Abstract  

A pair of novel isostructural azido-bridged polynuclear zinc(II) complexes, [Zn2(L1)21,1-N3)(μ1,3-N3)] n (1) and [Zn2(L2)21,1-N3)(μ1,3-N3)] n (2) (HL1 = 2-bromo-4-chloro-6-[(2-isopropylaminoethylimino)methyl]phenol, HL2 = 2,4-dibromo-6-[(2-isopropylaminoethylimino)methyl]phenol), have been synthesized and structurally characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. Both complexes crystallize in the orthorhombic space group Pcca. Crystal data for (1): a = 22.567(4) ?, b = 8.414(2) ?, c = 17.268(3) ?, V = 3279.0(11) ?3, Z = 8, R 1 = 0.0441, and wR 2 = 0.0846. Crystal data for (2): a = 22.536(4) ?, b = 8.409(2) ?, c = 17.531(3) ?, V = 3322.2(11) ?3, Z = 8, R 1 = 0.0538, and wR 2 = 0.0906. X-ray structure determination revealed that each zinc(II) atom in the complexes is in a trigonal–bipyramidal coordination, with one imine N atom of a Schiff base ligand and two N atoms from two bridging azide ligands defining the basal plane, and one phenolate O and one amine N atoms of the Schiff base ligand occupying the two axial positions.  相似文献   

16.

Abstract  

The coordination compound {[Cu(NAP)2](4,4′-bpy)1/2}·DMF (1) was prepared by the reaction of α-naphthoic acid, 4,4′-bipyridine and Copper(II) acetate hydrate in basic solution, and was fully characterized by X-ray diffraction, element analysis, FTIR and TG analysis. Crystals of compound 1 belongs to the monoclinic crystal system, space group C2/c; a = 17.460(4) ?, b = 13.928(3) ?, c = 21.240(4) ?, β = 93.83(3), V = 5153.7 ?3, Z = 8. The structure analyses of 1 show a one-dimensional chain structure where the binuclear structural units [Cu2(NAP)4] are bridged by 4,4′-bipyridine molecules. Furthermore, the 1D chains are assembled to form 2D supramolecular sheet by intermolecular π···π stacking interactions between naphthalene rings.  相似文献   

17.

Abstract  

The new ligand 2,4-N,N′-bis(napthylamino)-pent-2-ene (Lnapth) (1) has been synthesized and crystallizes in space group P212121 with crystal cell parameters a = 8.196(3) ?, b = 9.119(3) ?, c = 25.746(10) ?, V = 1924.3(12) ?3 and Z = 4. The complexes bis[2,4-pentane-N,N′-bis(napthyl)ketiminato] chromium(II) (2), bis[2,4-pentane-N,N′-bis(isopropylphenyl)ketiminato] chromium(II) (3), and bis[2,4-pentane-N,N′-bis(tertbutylphenyl)ketiminato] chromium(II) (4) were synthesized and structurally characterized. Complex 2, the first complex reported with a bis(napthyl) β-diketiminate ligand, crystallizes in space group P − 1 with crystal cell parameters a = 12.0824(15) ?, b = 12.2462(16) ?, c = 14.8975(19) ?, α = 87.035(2)°, β = 80.615(2)°, γ = 62.756(2)°, V = 1932.9(4) ?3 and Z = 2. Complex 3 crystallizes in space group P21/n with crystal cell parameters a = 13.088(3) ?, b = 22.222(5) ?, c = 14.206(3) ?, β = 102.310(4)°, V = 4036.6(17) ?3 and Z = 4. Complex 4 crystallizes in space group P21/n with crystal cell parameters a = 20.831(6) ?, b = 11.575(4) ?, c = 21.373(7) ?, β = 107.241(5)°, V = 4922(3) ?3 and Z = 4. The degree of twist between the ligand planes is dependent on the steric bulk of the ligand.  相似文献   

18.

Abstract  

The hydrazone compounds, N′-(5-chloro-2-hydroxybenzylidene)-4-dimethylaminobenzohydrazide (1) and N′-(2,4-dichlorobenzylidene)-4-dimethylaminobenzohydrazide (2), have been synthesized by the condensation reaction of equimolar quantities of 4-dimethylaminobenzohydrazide with 5-chlorosalicylaldehyde and 2,4-dichlorobenzaldehyde, respectively, in methanol. The compounds were characterized by elemental analysis, IR, 1HNMR spectra, and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 35.014(3) ?, b = 10.407(2) ?, c = 18.505(2) ?, β = 112.046(2)°, V = 6250.0(15) Ǻ3, Z = 16, R 1 = 0.0624, and wR 2 = 0.1187. Compound 2 crystallizes in the triclinic space group P-1 with unit cell dimensions a = 12.625(2) ?, b = 12.688(3) ?, c = 13.005(2) ?, α = 101.271(2)°, β = 112.945(1)°, γ = 104.966(2)°, V = 1747.6(6) Ǻ3, Z = 2, R 1 = 0.0523, and wR 2 = 0.1138. In the asymmetric unit of each compound, there exists two hydrazone molecules linking together by an N–H⋯O hydrogen bond. Furthermore, compound (2) contains one methanol molecule and one water molecule of crystallization.  相似文献   

19.

Abstract  

The crystal structure together with unambiguous assignation of 1H and 13C NMR signals of 3-epismilagenin acetate 4 and 23-oxo-3-epismilagenin acetate 5 are described. Compound 4, crystallized as orthorhombic system a = 10.535(1) ?, b = 13.775 (1) ?, c = 18.347 (1) ?, α = β = γ = 90°; with space group P2 1 2 1 2 1 ; while compound 5 crystallized as a monoclinic system a = 10.380(1) ?, b = 7.327(1) ?, c = 17.881(1) ?, α = γ = 90°, β = 99.56(1)°, with a space group P2 1 . The presence a carbonyl group at C(23) in compound 5 produces a significant deviation from the chair conformation observed in compound 4. The effects of the side chain modifications on the puckering parameters derived from are discussed.  相似文献   

20.

Abstract  

Evaporation of the mixture solution of Cu(ClO4)2·6H2O, KOH and (S)-2-hydroxy-3-phenylpropanoic acid affords a Cu(II)–K(I) coordination compound 1. Single-crystal X-ray diffraction analysis reveals that 1 is a one-dimensional comb-like coordination polymer in the P212121 space group with crystal cell parameters a = 10.989(2) ?, b = 15.939(3) ?, c = 22.511(5) ?, V = 3943(1) ?3 and Z = 4.  相似文献   

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