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1.
Abstract  The crystal structures for two of the ligands C6H5CH2SOCH2CONHCH2C6H5 (1) and C6H5SOCH2CON(iC3H7)2 (2) have been determined by X-ray diffraction. These compounds crystallize in orthorhombic system with space groups and cell parameters, Pca21(no. 29), a = 8.4600(5) ?, b = 5.3534(5) ?, c = 32.136(2) ?, V = 1455.42(15) ?3 and Pna21(no. 33) a = 17.5563(11) ?, b = 5.7902(4) ?, c = 14.2866(9) ?, V = 1452.30(16) ?3, respectively. These molecules are stabilized in solid state by various intra and intermolecular hydrogen bonding interactions to give polymeric structures. The reported IR spectra of these compounds in solid state could be explained on the basis of the observed intermolecular hydrogen bonding interactions. Index Abstract  The title compounds C6H5CH2SOCH2CONHCH2C6H5 (1) and C6H5SOCH2CON(iC3H7)2 (2) were prepared by the oxidation of corresponding sulfides with H2O2/SeO2 in methanol and their structures were determined. The structures show that the SO and CO groups are having “anti” configuration in 1 and “syn” configuration in 2. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.  相似文献   

2.
The crystal structures consist of organoammonium cations hydrogen bonded to tetrahedral CoCl4 2– anions. In the 4-dimethylaminopyridinium salt, [(CH3)2NC5H5NH]2CoCl4, pairs of cations hydrogen bond in an asymmetric fashion to two of the chlorines in each anion. The planar cations form two sets of – stacks, first parallel to the a axis and the second parallel to the b axis. The anions lie between these two nonintersecting sets of stacks. In contrast, for the second compound, [C6H4(CH2NH3)2]CoCl4, the tetrahedral CoCl4 2– anions form layers lying parallel to the bc plane. The 1,3-di(ammoniummethyl)benzene cations crosslink adjacent anionic layers, forming a lamellar structure of alternating organic and inorganic layers.  相似文献   

3.
The bis(benzylammonium)tetrahalogenochromate(II), (C6H5CH2NH3)2CrBr3. 3Cl0. 7, has been synthesized and characterized. The crystal structure is related to that of K2NiF4. The compound is ferromagnetic and the Curie temperature TC (TC= 49 K) has been measured by a mutual inductance technique. The susceptibility increases sharply at TC and then shows a drop-off below TC, typical of a single-domain powder sample. The compound is found to behave as a typical 2D easy plane ferromagnet.  相似文献   

4.
Abstract The X-ray crystal structures of two lamotrigine derivatives (I) 2-methyl, 3-amino, 5-imino-6-(2, 3-dichlorophenyl)-1,2,4-triazine, C10H9Cl2N5, as the hemi hydrate and (II) 2-methyl,3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazine, C10H10Cl2N5, as the isethionate-water solvate, have been carried out at liquid nitrogen temperature. A detailed comparison of the two structures is given. Both are monoclinic and centrosymmetric, with (I) in space group C2/c, and (II) in space group P21/n. For (I) the unit cell dimensions are a = 19.5466(10), b = 7.5483(4), c = 15.7861(8) ?, β = 91.458(3)°, volume = 2328.4(2) ?3, Z = 8, density = 1.590 Mg/m3; for (II). For (II) the unit cell dimensions are a = 6.0566(2), b = 11.0084(4) c = 23.9973(9) ?, β = 92.587(3)°, volume = 1598.35(10) ?3, Z = 4, density = 1.597 Mg/m3. For (I) final R indices [I > 2sigma(I)] are R1 = 0.0356, wR2 = 0.0782 and R indices (all data) are R1 = 0.0424, wR2 = 0.0817. For (II) final R indices [I > 2sigma(I)] are R1 = 0.0380, wR2 = 0.0871 and R indices (all data) R1 = 0.0558, wR2 = 0.0949. Both structures have a molecule of water of crystallization and (II) also includes a solvated CH3SO3. Comparisons are made between the two structures. Structure (I) is very unusual in having a = NH group at position C5′ on the triazine ring. No other examples of this particular substitution, which is usually −NH2, have been reported. Index Abstract Rex A. Palmer, Brian S. Potter, Michael J Leach and Babur Z. Chowdhry The crystal structures of (I) 2-methyl,3-amino, 5-imino-6-(2, 3-dichlorophenyl)-1, 2, 4-triazine, water solvate and (II) 2-methyl,3, 5-diamino-6-(2, 3-dichlorophenyl)-1, 2, 4-triazine isethionate water solvate are presented. The relative orientation of the two rings is shown to vary. Lamotrigine and analogues have been investigated for some time for their effects on the central nervous system. For example both lamotrigine and 5-(2,3,5-trichlorophenyl)-2,4-diaminopyrimidine (code name BW 1003C87) are voltage-gated sodium channel blockers as well as blocking the release of the neurotransmitter glutamate [D. R. Riddall, M. J. Leach, J. Garthwaite, Mol. Pharmacol. 2006, 69 (1), 278.3], BW10003C87 (like lamotrigine) has been shown to exhibit excitatory amino acid antagonist activity similar to that of three conventional antiepileptic drugs phenytoin, carbamazepine and phenobarbital [R. Lingamaneni, H. C. Hemmings Jr., Epilepsy Res. 1993, 15, 101.]. BW 1003C87 has also been shown [B. S. Meldrum, J. H. Swan, M. J. Leach, M. H. Millan, R. Gwinn, K. Kadota, S. H Graham, J. Chen, R. P. Simon , Brain Res., 1992, 593, 1.] to reduce the release of glutamate evoked by veratrine in brain tissue, providing a therapeutic approach in both cerebral ischemia and epilepsy. This is one of a series of papers on the structures of lamotrigine analogues.   相似文献   

5.
A single crystal X-ray investigation of the purple nickel (II) complex Ni[L(en)](NO3)2, produced by condensation of 1,2-diaminoethane (en) with the thiodiketone S(CH2COCH3)2 in the presence of nickel (II) nitrate (L is NH2(CH2)2N=C(CH3)CH2SCH2COCH3), shows that the metal ions are six coordinate. The new ligand L is tetradentate, with the N,N and S donor atoms arranged meridionally, and the coordination shell completed by the carbonyl oxygen atom of L and the nitrogen atoms of 1,2-diaminoethane. Metal-ligand bond distances are Ni-N: 2.08 av. (en), 2.10 and 2.05 (NH2 and N=C respectively of L); Ni-O, 2.16; Ni-S, 2.45 Å. There is considerable angular distortion from regular octahedral values of the bond angles at nickel. The crystals are monoclinic,P21/c (No. 14),a=12.433(2),b=11.709(1),c=13.150(2) Å,=103.93(1)°,V c=1858.2(4) Å3. The structure was solved by the heavy-atom method and refined by full-matrix least squares to anR value of 0.055 for 3633 reflections.  相似文献   

6.
The title compound is (μ-H)Ru3(CO)7(μ-As(C6H5)CH2As(C6H5)2)((C6H5)2 AsCH2As(C6H5)2)·CH2C12. Crystal data: monoclinic,P21/n, cell parameters (X-ray)a=12.82(2) Å,b=22.91(2) Å,c=17.83(2) Å, β=99.1(3)°; (neutron)a=12.94(1) Å, β=22.95(2)Å,c=17.93(3)Å,β=99.55(5)°. The structure was solved from X-ray data. FinalR indices areR(F)=0.051,R w (F)=0.049 (X-ray);R(F)=0.064,R w (F)=0.048,R(F 2)=0.072,R w (F2)=0.088 (neutron). The complex is derived from Ru3(CO)8(dpam)2 through reaction with hydrogen. The structure consists of a triangular array of metal atoms involving three metal-metal bonds[Ru(1)?Ru(2)=2.912(7)Å;Ru(1)?Ru(3)=2.829(3) A; Ru(2)?Ru(3)=2.845(6) Å]. The metal-metal edge Ru(1)?Ru(2) is supported by a bridging bis(diphenylarsino)methane ligand which lies in the equatorial plane. Activation of the second dpam ligand has generated the new face-bridging ligand unit μ-As(C6H5)CH2As(C6H5)2. In this unit, the bridgehead As atom spans over the Ru(1)?Ru(2) bond, while the second As atom is only bonded to Ru(3). The metal environment is achieved by CO ligands. The hydride ligand is bridging the Ru(1)?Ru(2) vector [Ru(1)?H=1.791(10) Å; Ru(2)?H=1.818(8) Å]. Geometric features of the dibridged Ru(μ-H)(μ-As)Ru bond are discussed.  相似文献   

7.
A new organic-inorganic hybrid γ-octamolybdate complex, (NH4)4[(C3H7NO)2Mo8O26]·2CH3CH2OH·2H2O was synthesized from the mixture of ethanol, DMF, 4-aminobenzoic acid, (NH4)6Mo7O24·4H2O, HCl and H2O. The structure was determined by X-ray crystallography. It crystallizes in monoclinic P21/n space group with the crystal cell parameters of a = 8.8825(4), b = 21.1608(10), c = 11.1343(6) ?, β = 104.7720(10)°, V = 2023.64(17) ?3 and Z = 2. The crystal X-ray analysis shows that two DMF molecules are bound to γ-octamolybdate anion. The molecular structure is stabilized by the complex hydrogen bonding.  相似文献   

8.
W(CO)5(C8H14) and W(CO)4(C8H14)2 were synthesized photochemically from W(CO)6 andcis-cyclooctene with a respective yield of 71% and 18%. The compounds were characterized by NMR, IR and single X-ray crystallography. The IR spectra of the two compounds exhibited characteristic bands for the mono- and bis-substituted metal carbonyl complexes. In W(CO)4(C8H14)2, thecis-cyclooctene ligands are in atrans configuration with the double bonds perpendicular to each other. The two crystal structures were refined toR=0.040 for W(CO)5(C8H14) and 0.025 for W(CO)4(C8H14)2. Although the tungsten-carbon (of the carbonyl groups) distances are very similar in both structures, the distances between the tungsten atom and the olefinic carbons are shorter in W(CO)4(C8H14)2, 2.36 Å, than in W(CO)5(C8H14), 2.51 Å.  相似文献   

9.

Abstract  

Two 16 electron titanacyclobutanes of the formula Ti(C5H4R)22-CH2)2C(CH3)(i-C3H7) (R=H, CH3) have been prepared from the reaction of Ti(C5H5)22-CH2)(μ2-Cl)Al(CH3)2 or Ti(C5H4CH3)22-CH2)(μ2-Cl)Al(CH3)2 with H2C=C(CH3)(i-C3H7). Structural parameters, most notably lengthened C–C bonds in the titanacyclobutane ring, for both complexes reveal the expected presence of (C–C)→Ti agostic interactions. The complexes are isomorphous, crystallizing in the monoclinic space group Cc. For Ti(C5H5)22-CH2)2C(CH3)(i-C3H7), a = 11.3459(3) ?, b = 16.2108(4) ?, c = 8.1646(2) ?, β = 105.5276(16)°, V = 1446.87(6)°, Dcalc = 1.268 at 150(1) K. For Ti(C5H4CH3)22-CH2)2C(CH3)(i-C3H7), a = 12.6591(2) ?, b = 16.2795(4) ?, c = 8.2462(2) ?, β = 107.2421(14)°, V = 1623.04(6) ?3, Dcalc = 1.245 at 150(1) K.  相似文献   

10.
New crystals of the composition Er2(SO4)3 ? 8H2O have been synthesized by the method similar to that used for synthesis of (CH3)2NH2Al(SO4)2 ? 6H2O. The synthesized crystals were studied by the X-ray diffraction method. The crystals are monoclinic C2/c) and contain no (CH3)2NH2 ions. It is established that, contrary to DMAAS crystals, Er2(SO4)3 ? 8H2O crystals undergo no phase transitions and possess neither ferroelectric nor ferroelastic properties.  相似文献   

11.
The crystal structures of 1,4,7,10,13,16-hexaoxa-cyclooctadecane dicyano mercury(II) monohydrate, C14H24HgN2O6·H2O, 1, and 2,5,8,11,18,21,24,27-octaoxa-tricyclo[26.4.0.012,17]-dotriconta-1(28),12,14,16,29,31-hexaene dicyano mercury(II) monohydrate, C26H32HgN2O8·H2O, 2, were determined: 1 crystallizes in the trigonal space group R3¯ with cell dimensions a = 11.7842(1) and c = 12.0316(1) Å. 2 crystallizes in the monoclinic space group P21/c with cell dimensions a = 11.156(3) Å, b = 8.417(2), c = 30.901(8) Å, and = 93.279°. In spite of the different cyclic systems, similar complexes are formed where the Hg atom is coordinated by two CN groups and six oxygen atoms of the crown ether. The structure of 1 is isostructural with the crystal structures of 18C6—HgCl2, 18C6—CdBr2, 18C6—Sr(BH4)2, and 18C6—Ba(BH4)2. Furthermore, 1 is very similar to other 18C6—HgX2 complexes.  相似文献   

12.
The crystal and molecular structures oftrans-[PtCl2(C2H4)(4-MeC5H4N)] (I) andtrans-[PtCl2(C2H4)(2,4,6-Me3C5H2N)] (II) have been determined by single-crystal x-ray methods.I crystallizes in space groupP21/c witha= 4.991(1), b=21.658(3), c=10.675(3) Å, =110.17(2) °,Z=4;II is orthorhombic (Pbca) witha=10.295(6),b=12.393(8),c=20.370(10) Å,Z=8.Full-matrix least-squares refinements have given finalR factors of 0.053 (1520 reflections) forI and 0.042. (1412 reflections) forII. The intensities were recorded by counter methods, and only those reflections havingI>3(I) were used in the analyses.In both complexes, platinum is four-coordinate with the two chlorine atoms, the double bond of the ethylene, and the nitrogen atom of the substituted pyridine. The two structures are discussed in terms of the arrangement of the pyridine ligand with respect to the PtCl2(C2H4) moiety.  相似文献   

13.
The cobalt(III) complex salt [(C4H9)4N][trans-Co(NH3)2(NO2)4] has been synthesized in high yield by reacting equimolar quantities of [(C4H9)4N]Br and K[trans-Co(NH3)2(NO2)4] in aqueous medium at room temperature. The product thus formed has been re-crystallised from acetone-water mixture, in the monoclinic space group P 21/n, with cell dimensions a=11.651(3) ?, b=19.005(4) ?, c=11.733(5) ?, β=90.28(3)°. The X-ray structure determination revealed the presence of discrete ions, [(C4H9)4N]+ and [trans-Co(NH3)2(NO2)4]. The central metal ion cobalt(III) in the anion is found in octahedral environment, in trans geometry, while the organic counterion is a quaternary alkylammonium cation. The crystal lattice is stabilized by electrostatic interactions between the cations and anions.Supplementary material Crystallographic data (excluding structure factors) for the structure(s) reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CCDC 291300. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: (44) 1223 336-033; e-mail: deposit@ccdc.cam.ac.uk.  相似文献   

14.
The new compound [Pd(NH2CH2CH2OH)4][Pd6(NH2CH2CH2S)8]Cl6 · 5H2O (I) is synthesized and its crystal structure is determined. The crystals are monoclinic, a = 25.625(6) Å, b = 9.633(5) Å, c = 24.847(7) Å, β = 91.47(2)°, Z = 4, and space group C2/c. The structural units of crystals I are the centrosymmetric hexanuclear [Pd6(NH2CH2CH2S)8]4+ cations, the mononuclear [Pd(NH2CH2CH2OH)4]2+ cations with C 2 symmetry, the Cl? anions, and crystallization water molecules. In the hexanuclear cation, the interaction between the Pd atoms occurs through the S atoms of the mercaptoethylaminate ligands. The Pd(2) and Pd(3) atoms and the ligands form two metallochelate fragments in which the N and S atoms are located in cis positions. The average lengths of the Pd-S and Pd-N bonds are equal to 2.274(1) and 2.074(6) Å, respectively. The metallochelate fragments are joined to each other and to their centrosymmetric analogues through the Pd(1) atom, which coordinates four S atoms [the average Pd-Sav bond length is 2.332(1) Å]. In the mononuclear cation, the Pd(4) atom coordinates four N atoms of the monoethylaminate ligands [the Pd-N bond lengths are 2.045(6) and 2.056(6) Å]. The shortest Pd?Pd distance is equal to 3.207(1) Å. The bonding in the structure is provided by numerous hydrogen bonds with the participation of all the H2O molecules, NH2 groups, and Cl? anions.  相似文献   

15.
Two crystalline adducts of triethylenediamine with hydroquinone [N(CH2CH2)3N·C6H4(OH)2,I] and phenol [N(CH2CH2)3N·2C6H5OH,II] have been isolated and characterized by X-ray analysis. ComplexI crystallizes in the monoclinic space groupC2/c, witha=11.944(2),b=9.491(2),c=11.986(2) Å,=121.70(1)°, andZ=4. Both molecular components occupy sites of symmetry 2, and are linked alternately by N H-O hydrogen bonds to form infinite zigzag chains. Crystals ofII are also monoclinic, with space groupP21/c,a=12.987(2),b=6.376(1),c=21.350(3) Å,=106.94(1)°, andZ=4. The structure is composed of discrete hydrogen-bonded molecular aggregates corresponding to the stoichiometric formula. The triethylenediamine moieties in both adducts closely approximate to the idealizedD 3 h conformation. The structures have been refined toR values of 0.097 (I) and 0.092 (II) using, respectively, 479 and 1580 observed MoK data.  相似文献   

16.
The crystal structures of (i) CH3(C9H6O2)SO2C6H5 and (ii) CH3(C8H8O2)SO2−C6H5 have been determined by X-ray diffraction. (i) crystallizes in the monoclinic space groupP21/c with unit cell parametersa=8.814(1)?,b=10.310(1)?,c=15.841(4)?, β=98.17(1)o, andZ=4, and (ii) crystallizes in the orthorhombic space groupP212121 with unit cell parametersa=6.206(1)?,b=11.752(5)?,c=19.865(3)?, andZ=4. The pyran ring in both of them is in the distorted half-chair conformation with differeing degrees of distortion from the ideal.  相似文献   

17.
The solid-vapor reaction properties of [Zn(p-NH2C6H4SO3)2(H2O)2] n and alkyl monoamines were investigated. Two of the resulting complexes, [Zn(C2H5NH2)4](p-H2NC6H4 SO3)2 and [Zn(n-C3H7NH2)4](p-H2NC6H4SO3)2, grew into single crystals in situ during the solid-vapor reaction process and their structures were characterized by single-crystal structural analysis.  相似文献   

18.
The crystal structures of two Bi tris xanthates are reported, namely [Bi(S2CO-c-C6H11)3 J and [Bi(S2COCH2C6H5)3]. They exist as centrosymmetric dimers, owing to the presence of bridging xanthate ligands, with seven-coordinate Bi atoms. The presence of a stereochemically active lonepair of electrons in each structure distorts the coordination geometry defined by seven S atoms and causes the elongation of some of the Bi-S bond distances. Crystals of both compounds are triclinic, space groupP¯1 with unit cell dimensions for [Bi(S2CO-c-C6H11)3]:a=12.417(3),b=13.571(3),c=9.681(4) Å;=102.30(2),=109.21(2), =66.23(2)° andZ=2; and for [Bi(S2COCH2C6H5)3]:a=14.747(2),b=15.966(2),c=5.991(1) Å;=95.08(1),=98.51(1), =104.92(1)° andZ=2. The structures were refined by a full-matrix least-squares procedure to finalR=0.045 using 4274 reflections for [Bi(S2CO-c-C6H11)3] and toR=0.027 using 3993 reflections for [Bi(S2COCH2C6H5)3].  相似文献   

19.
Complex of iron(II) bis(2,4-dimethylphenyl)dithiophosphate with 4-ethylpyridine [{(2,4- (CH3)2C6H3O)2PS2}2Fe{NC5H4(C2H5)-4}2] is synthesized and characterized by elemental analysis, magnetic moment, IR spectroscopy and single crystal X-ray analysis. Complex crystallizes in the monoclinic sp. gr. P21/n, Z = 2. Crystal structure consists of mononuclear units with Fe(II) ion chelated by four S atoms of the two diphenyldithiophosphate ligands in bidentate manner. N atoms from two 4-ethylpyridine ligands are axially coordinated to the Fe(II) atom leading to an octahedral geometry.  相似文献   

20.
Three N2O4 Schiff. base homologs, H2L1 (n = 8), H2L3 ((n = 9), and H2L4 (n = 10) were obtained from the reactions of 2-HOC6H4CHO with H2N(CH2)8-10NH2, while a derivative of H2L1, namely, H2L2, was obtained from the reaction of 3,5-X2-2-HOC6H2CHO (X = tert-butyl) with H2N(CH2)8NH2. The Schiff bases H2L2 (triclinic; P-1), H2L3 (monoclinic; C2/c), and H2L4 (monoclinic; P21/c) were single crystals with low melting temperatures (less than 100°C). The homologs exhibited mesomorphisms, while the derivative was not mesomorphic and did not reform crystals from its melt. Copper(II) complexes of H2L1, H2L2 and H2L4 were dimeric, while that of H2L3 was dinuclear with chelating CH3COO ligand. These complexes were paramagnetic with insignificant interactions between the copper(II) atoms and have high decomposition temperatures (Tdec = 268–304°C). Their melting temperatures (Tmelt = 138.9–190.2°C) were higher than the corresponding Schiff bases, but they were not mesomorphic.  相似文献   

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