The Synthesis and Crystal Structure Determination of Phenyl 2-(3,4-dihydro-1(2<Emphasis Type="Italic">H</Emphasis>)naphthalenylidine)hydrazinecarboxylate and Phenyl (2,4-dichlorophenyl-methylene)hydrazinecarboxylate

Abstract  

(E)-Phenyl 2-(3,4-dihydro-1(2H)-naphthalenylidine)hydrazinecarboxylate and (E)-phenyl (2,4-dichlorophenylmethylene)hydrazinecarboxylate were prepared by the condensation of 1-tetralone or 2,4-dichlorobenzaldehyde with phenyl hydrazinecarboxylate. Crystals of C₁₇H₁₆N₂O₂ 3 are monoclinic, C2/c, a = 17.763(4) ?, b = 8.353(2) ?, c = 40.233(8) ?, Z = 16, V = 5,839(2) ?³, R ₁ = 0.0448 and wR ₂ = 0.1104 for reflections with I > 2σ(I). Crystals of C₁₄H₁₀N₂O₂Cl₂ 5 are orthorhombic, P2₁2₁2₁, a = 8.288(3) ?, b = 14.082(2) ?, c = 23.788(5) ?, Z = 8, V = 2,777(1) ?³, R ₁ = 0.0815 and wR ₂ = 0.2006 for reflections with I > 2σ(I). The molecular packing in the crystal for both compounds is the result of N–H···O hydrogen bonding.     

Crystal structures of substituted imidazolidine derivatives

The crystal structures of isoxazole, 3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]methyl-5-phenyl-,N-oxide] (C₁₃H₁₃N₅O₃) (I), isoxazole,3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]-methyl-5-(4-methylphenyl)-,N-oxide] (C₁₄H₁₅N₅O₃) (II) and isoxazole, 3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]-methyl-5-(2-methoxyphenyl)-,N-oxide] (C₁₄H₁₅N₅O₄) (III) have been determined by X-ray diffraction studies. The compound I, crystallized in triclinic space group with unit cell dimensions a = 7.2405(7) ?, b = 7.9936(8) ?, c = 11.6573(11) ?, α = 97.801(2)°, β = 90.884(2)°, γ = 96.250(2)° and Z = 2. Compound II crystallized in orthorhombic space group Pna2₁ with unit cell dimensions a = 10.1778(10) ?, b = 28.228(3) ?, c = 5.1206(5) ?, and Z = 4. Compound III crystallized in monoclinic space group P2₁/n with unit cell dimensions a = 7.8439(9) ?, b = 7.8544(9) ?, c = 23.534(3) ?, β = 99.464(2)° and Z = 4. For all three compounds, the five-membered imidazolidine ring adopts an envelope conformation. The crystal structures are stabilized by both the intramolecular N–H···O and intermolecular N–H···N hydrogen bonding.     

Synthesis and molecular structure of 4,4,5,5-tetramethyl-2-(1-(phenylsulfonyl)propan-2-yl)-1,3,2-dioxaborolane

The compound 4,4,5,5-tetramethyl-2-(1-(phenylsulfonyl)propan-2-yl)-1,3,2-dioxabo- rolane has been prepared by the rhodium catalyzed hydroboration of allyl phenyl sulfone and characterized by a single crystal X-ray diffraction study. The title compound crystallized in the monoclinic space group P2₁/c, with cell parameters a=16.0728(8) ?, b=9.8884(5) ?, and c=10.1926(5) ?, β=92.067(1)°, Z=4, and V=1618.90(14) ?³. The structure was solved by direct methods and refined to a final R=0.0449 for 3627 reflections with I>2σ(I). No significant intramolecular or intermolecular interaction is observed with the Lewis acidic boron atom.     

The Crystal Structures of Some 1-Aryl-5-methyl-1,2,3-triazole Derivatives

Abstract  The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C₉H₈BrN₃, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2) ?, α = 90.00, β = 116.01(3), γ = 90.00o. V = 949.6(3) ?³, Z = 4, Dx = 1.665 Mg m⁻³. The final R was 0.0477. Compound 4b, C₁₃H₁₁N₃, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?³, Z = 8, D _m = 1.304 Mg m⁻³. The final R was 0.0565. Index Abstract  The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C9H8BrN3, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2)  ?, α = 90.00, β = 116.01(3), γ =90.00o. V = 949.6(3) ?³, Z = 4, Dx = 1.665 Mg m⁻³. The final R was 0.0477. Compound 4b, C13H11N3, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?³, Z = 8, D _m = 1.304 Mg m⁻³. The final R was 0.0565.      

Structure of 2-(1-phenylimidiazolidin-2-ylidene)- malononitrile and 2-(hexahydropyrimidinyl-2-ylidene)- malononitrile

The crystal structure of 2-(1-phenylimidazolidin-2-ylidene)-malononitrile, I, and 2-(hexahydropyrimidin-2-ylidene)-malononitrile, II, were determined with crystal data (I: Monoclinic, P2₁/n, a=8.116(3) ?, b=7.650(3) ?, c=17.399(7) ?, β=93.065(6)°, R _all=0.0980; II: Monoclinic, P2₁/n, a=9.169(2) ?, b=8.103(2) ?, c=10.337(3) ?, β=99.853(4)°, R _all=0.0877). N−H···N hydrogen bonds were responsible for the formation of centrosymmetric dimers of I and one-dimensional zigzag molecular chains of II.     

Synthesis and Crystal Structure of a New Cobalt(II) Complex: Bis(pyridine)bis(4,4,4-trifluoro-1-(6-methoxynaphthalen-2-yl)butane-1,3-dione) Cobalt(II)

Abstract  

A new Co(II) complex 2 with ligand 4,4,4-trifluoro-1-(6-methoxynaphthalen-2-yl) butane-1,3-dione 1 and pyridine are prepared and crystallized from an acetone solution. The obtained red and transparent crystal conforms to the empirical formula of Co(C₁₅H₁₀O₃F₃)₂·(C₅H₅N)₂. It crystallizes in monoclinic, space group C2/c with a = 23.3152(14), b = 12.0225(7), c = 15.3950(10) ?, β = 124.1360(10)°, V = 3571.8(4) ?³, Z = 4, C₄₀H₃₀CoF₆N₂O₆, Mr = 807.59, F(000) = 1652, Dc = 1.502 g/cm³, μ = 0.564 mm⁻¹, the final R = 0.0466 and wR = 0.1043 for 3901 observed reflections with I > 2σ(I). X-ray structural analysis revealed that the Co(II) atom is coordinated by two oxygen atoms of 1,3-dione ligands 1 and two nitrogen atoms of pyridines, forming a distorted octahedron coordination geometry.     

Synthesis and structure of ytterbium (III) complex containing tetrachlorophthalate dianions

A novel tetrachlorophthalato-Yb(III) complex [Yb(tcph)(H₂O)₇]Htcph·H₂tcph·H₂O (1) (H₂tcph=tetrachlorophthalic acid) has been synthesized and characterized by the single crystal X-ray diffraction analysis. Colorless crystals of 1 crystallize in the triclinic space group P-1, with a=6.8504(5) ?, b=16.1921(12) ?, c=19.0123(14) ? and α=67.4470(10)°, β=86.5290(10)°, γ=81.6480(10)°, V=2.113 g/cm³ and Z=2. Unique reflections with I > 2σ(I) on refinement afford values of R ₁=0.0219 and wR ₂=0.0565.     

The Synthesis and Crystal Structure of 5-(4-Bromophenylamino)-2-methylsulfanylmethyl-2<Emphasis Type="Italic">H</Emphasis>-1,2,3-triazol-4-carboxylic Acid Ethyl Ester

Abstract  The 5-(4-bromophenylamino)-2-methylsulfanylmethyl-2H-1,2,3-triazol-4-carboxylic acid ethyl ester 6 was synthesized from p-bromoaniline. The yielded product 6 was investigated with X-ray crystallographic, NMR, MS, and IR techniques. Compound 6, C₁₃H₁₅BrN₄O₂S, Mr = 371.26, crystallizes in the monoclinic space group P2₁/n with unit cell parameters a = 5.5220(1), b = 26.996(5), c = 10.596(2) ?, β = 103.83(3). V = 1533.8(5) ?³, Z = 4, Dx = 1.608 mg m⁻³. The final R ₁ was 0.0844; wR ₂ was 0.1560. H-bond is discussed. Index Abstract  The structure of 5-(4-bromophenylamino)-2-methylsulfanylmethyl-2H-1,2,3-triazol-4-carboxylic acid ethyl ester from 5-amino-1-(4-bromophenyl)-1,2,3-triazol-4-carboxylic acid ethyl ester is studied. H-bond is discussed.      

Molecular Association of Almotriptan with Oxalate and Terephthalate Anions

Abstract  

Crystal structures of anti-migraine drug almotriptan were crystallized with oxalic acid (I) and with terephthalic acid (II) and their crystal structures and molecular associations were determined using X-ray diffraction methods. Crystals of both (I) and (II) are monoclinic, space group P2₁/c, with a = 5.6270(4) ?, b = 27.6419(19) ?, c = 13.6228(9) ?, β = 93.057(1)°, V = 2115.9(3) ?³, Z = 4 (I) and a = 13.3756(15) ?, b = 15.6065(17) ?, c = 10.7238(12) ?, β = 98.017(2)°, V = 2216.7(4) ?³, Z = 4 (II). In almotriptan oxalate {systematic name: N,N-dimethyl-2-[5-(pyrrolidin-1-ylsulfonyl-methyl)-1H-indol-3-yl]-ethanaminium semioxalate}, C₁₇H₂₆N₃O₂S⁺, C₂HO₄ ⁻, (I) and in almotriptan hemi terephthalate hydrate {systematic name: N,N-dimethyl-2-[5-(pyrrolidin-1-ylsulfonyl-methyl)-1H-indol-3-yl]-ethanaminium hemi terephthalate monohydrate}, C₁₇H₂₆N₃O₂S⁺, 0.5(C₈H₄O₄ ²⁻), H₂O, (II), both the almotriptan cations form a trimer with the corresponding anions via N–H···O hydrogen bonds. In (I), the oxalate salt is monoprotonated and in (II), the terephthalic acid is located across the inversion centre and exists as doubly protonated anion. In (I), the cation and anion are interlinked by the N–H···O and O–H···O hydrogen bonds into continuous two-dimensional layers generate an R₆⁶(34) hydrogen-bonded motif tetramers running parallel to the (0 0 1) plane. In (II), the cation and water form a centrosymmetric tetramer of R₄⁴(22) hydrogen-bonded motif via N–H···O and O–H···O hydrogen bonds and further cross-linked by centrosymmetric anions to form an infinite three-dimensional supramolecular hydrogen-bonded networks.     

Structures and Characterization of [Zn(n-chlorosalicylato)2(N-methylnicotinamide)2(H2O)2] (n?=?4 or 5) Ligand Isomers

Abstract  

Two ligand isomers [Zn{4-ClC₆H₃-2-(OH)COO}₂(Menia)₂(H₂O)₂] (I) and [Zn{5-ClC₆H₃-2-(OH)COO}₂(Menia)₂(H₂O)₂] (II) (Menia = N-methylnicotinamide) were prepared and characterized by elemental analysis, IR spectroscopy and thermal analysis. The X-ray crystal structures of complexes (I) and (II) were determined. Compound (I) crystallizes in the triclinic space group P[`1] P\bar{1} with a = 8.105(1) ?, b = 10.036(2) ?, c = 10.545(2) ?, α = 109.088(9)°, β = 91.416(8)°, γ = 102.757(9)°, V = 786.2(2) ?<sup>3</sup>, Z = 1. Compound (II) crystallizes in the triclinic space group P[`1] P\bar{1} . Its cell parameters are: a = 8.133(1) ?, b = 10.119(2) ?, c = 10.428(1) ?, α = 66.44(1)°, β = 74.32(1)°, γ = 80.16(1)°, V = 755.5(2) ?³, Z = 1. The molecular structure of both isomers is monomeric. Each Zn(II) atom is hexacoordinated by three pairs of unidentate ligands in trans-positions (ZnO₄N₂). The 5-Clsal complex is somewhat less distorted than 4-Clsal complex (Cl-sal = chlorosalicylate). The structural data are compared with those found in similar [Zn(RCOO)₂(NL)₂(H₂O)₂].     

Structures of Two (<Emphasis Type="Italic">E</Emphasis>)-3-Substituted Cinnamoylbenzotriazole 1-Oxides

Abstract  

The molecule of (E)-3-(3-MeOC₆H₄CH=CHCO)-benzotriazole 1-oxide, 2, has a very near planar structure, while the 2-nitrophenyl ring is rotated out of the plane of the remaining atoms in (E)-3-(2-O₂NC₆H₄CH=CHCO)-benzotriazole 1-oxide, 1. The nitrogen oxide bond lengths in 1 and 2 are 1.258 (6) and 1.2683 (15) ?, respectively, and are in the region found for related compounds. There are no strong intermolecular hydrogen-bonds in either compound, instead there are weak C–H···O intermolecular hydrogen-bonds and π···π stacking interactions in 1, and C–H···O, C–H···π, and π···π stacking interactions in 2. Different three-dimensional arrays are generated in each case. Compound 1 crystallises in the orthorhombic space group Pna2₁, with a = 25.061 (2) ?, b = 3.6997 (2) ?, c = 14.2623 (12) ? and Z = 4. Compound 2 crystallises in the triclinic space group P-1, with a = 5.7297 (3) ?, b = 10.8440 (6) ?, c = 11.4965 (6) ?, α = 89.689 (3)°, β = 76.019 (3)°, γ = 75.047 (3)°, Z = 2.     

Synthesis, Structural Characterization and Spectroscopic Properties of 1,2-Bis[4-(3,5-dimethyl-1H-pyrazol-1-yl)-2-oxobutyl]benzene

Abstract  

The crystal structure of the title compound C₂₂H₃₀N₄O₂·H₂O (L), has been determined using X-ray diffraction at 293 K. The crystal of 1,2-bis[4-(3,5-dimethyl-1H-pyrazol-1-yl)-2-oxobutyl]benzene is in triclinic crystal system with space group P(−1) (Z = 2), lattice parameters a = 8.225(6) ?, b = 10.967(6) ?, c = 12.903(6) ?, V = 1119.1(11) ?³. Analyses of single crystals of L, crystallized from dichloromethane/diethyl ether (1:1), revealed that the molecules are arranged in couples, which adopt a pseudo chair conformation, by means of intermolecular O–H···N hydrogen bonding interactions. Moreover, the extended structure revealed a 1D chain caused by several C–H···N intermolecular interactions.     

Synthesis and Structural Characterization of <Emphasis Type="Italic">N</Emphasis>-(2-Pyridylmethyl)-3-Methoxysalicylaldiminato Copper(II) Chloride

Abstract  The copper(II) complex [Cu(C₅H₄NCH₂−N=CH–C₆H₃OCH₃–O)Cl], (1) containing a new tridentate Schiff base ligand (LH), which is the 1:1 condensation product of 2-(aminomethyl)pyridine and o-vaniline, has been synthesised and characterized by IR and UV–Vis spectra. Structural investigation shows that 1 crystallizes to a monoclinic system, having space group P2(1)/c, a = 6.9634(7), b = 18.1209(19), c = 10.3448(11) ?, α = 90°, β = 103.97(2)°, γ = 90° and Z = 4. The coordination geometry around the copper atom is slightly distorted square planar, formed by the N₂O donor set of the Schiff base and one Cl atom. The Cu–N(1), Cu–N(2), Cu–O(1) and Cu–Cl bond distances are 2.0114(14), 1.9414(14), 1.9147(12) and 2.2520(5) ?, respectively. Index Abstract  The copper(II) complex [Cu(C₅H₄NCH₂−N=CH–C₆H₃OCH₃–O)Cl], (1) containing a tridentate Schiff base ligand (LH), synthesised and characterized by IR and UV–Vis spectra. The central copper ion possesses a distorted square-planar geometry.      

Structures of Three Chalcones Derived from 6-Methoxy-2-naphthaldehyde

Abstract  In the molecular structures of three new structurally related chalcone derivatives, namely (2E)-1-(2-hydroxyphenyl)-3-(6-methoxy-2-naphthyl)prop-2-en-1-one, C₂₀H₁₆O₃, I, (2E)-1-(2-chloropyridin-4-yl)-3-(6-methoxy-2-naphthyl)prop-2-en-1-one, C₁₉H₁₄ClNO₂, II, and (2E)-3-(6-methoxy-2-naphthyl)-1-pyridin-4-ylprop-2-en-1-one, III, C₁₉H₁₅NO₂, the configuration of the keto group is syn with respect to the olefinic double bond. In all three structures the molecules pack with weak intermolecular C–H···O interactions utilizing both the methoxy and keto oxygen’s in I, the methoxy oxygen in II and the keto oxygen in III. These interactions link the molecules into chains diagonally along the (011) plane of the unit cell in I and III and along the (010) plane in II. The dihedral angle between the phenyl and 2-napthyl rings in I is 31.7(3)°. In II and III the dihedral angle between the pyridyl and 2-naphthyl rings is 14.4(9)° and 1.8(9)°, respectively. C–H···O hydrogen bonding interactions influence these twist angles of these rings in I–III while weak π–π stacking interactions between naphthyl rings in I and III and also between pyridyl and naphthyl rings in II help stabilize crystal packing. [I: P2 ₁ /c, a = 7.6635(4) ?, b = 11.8047(6) ?, c = 16.7584(7) ?, β = 99.271(5)°, V = 1496.25(13) ?³; II: Pbca, a = 14.1424(4) ?, b = 6.0957(2) ?, c = 33.1458(11) ?, V = 2857.43(16) ?³; III: P2 ₁ /c, a = 11.5155(4) ?, b = 6.0020(2) ?, c = 22.4645(8) ?, β = 103.002(4)°, V = 1512.85(9) ?³]. Index Abstract  Crystal structures from three Chalcones derived from 6-methoxy-2-naphthaldehyde are reported and their geometric and packing parameters described.     

Synthesis,Crystal Structure and Thermal Properties of <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline and <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline

Abstract  

Two novel ferrocenyl substituted N-acetyl-2-pyrazolines, N-acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline (3) and N-acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline (4), have been synthesized and characterized by FTIR, ¹H-NMR, ¹³C-NMR techniques, elemental analysis and X-ray structure analysis. Thermal properties of these compounds have been determined by TGA, DTA and DSC analysis. Compound 3 (C₁₉H₁₈N₂O₂Fe) crystallizes in the monoclinic space group P21/c and Z = 4, with a = 8.6970(4) ?, b = 18.4725(9) ?, c = 11.0041(5) ?, β = 110.942(3)°. Compound 4 (C₁₉H₁₈N₂OSFe) crystallizes in the orthorhombic space group Fdd2 and Z = 16, with a = 84.242(2) ?, b = 13.5416(5) ?, c = 5.9405(2) ?, β = 90°. In terms of crystal packing, each compound shows different molecular arrangement, which are stabilized by C–H···O intermolecular weak hydrogen bonds, and/or C–H···π interactions.     

Synthesis and Crystal Structure of 2-Amino-4-(4-hydroxyphenyl)-5-propylthiazole Ethanol Solvate 0.25 Hydrate

Abstract  

2-Amino-4-(4-hydroxyphenyl)-5-propylthiazole was synthesized by the reaction of α-bromo-1-(4-hydroxyphenyl)-1-pentone with thiourea. The crystal structure of its ethanol solvate 0.25 hydrate, C₁₂H₁₄N₂OS···C₂H₅OH···0.25·H₂O, was determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with a = 20.9046(10), b = 10.1057(5), c = 30.0017(15) ?, β = 105.5850(10)°, Z = 8, M _r = 569.77, V = 6105.0(5) ?³, D _c = 1.240 g/cm³, μ = 0.214 mm⁻¹, F(000) = 2440, the final R = 0.0598 and wR = 0.1825 for 5,911 observed reflections [I > 2σ(I)]. Compound (1) is composed by two non-coplanar ring systems of phenol and thiazole. The structure displays extensive O–H···N, N–H···O and O–H···O intermolecular hydrogen bonds.     

Synthesis and Crystal Structures of 4-(3-Nitropyridin-2-ylamino)phenol and 4-(3-Aminopyridin-2-ylamino)phenol

Abstract  

The title compounds, 4-(3-nitropyridin-2-ylamino)phenol (I) and 4-(3-aminopyridin-2-ylamino)phenol (II), are two intermediates for the synthesis of a potential antitumor agent ABT-751. The reaction of 4-aminophenol with 2-chloro-3-nitropyridine yielded I which was converted into II by reduction. Instead of the Pd/C catalytic hydrogenation described in many literature, reduction with cheap sodium sulfide in aqueous media was utilized for shorting the reaction time and simplifying the operation. The crystal structures of the resultant compounds were determined by single-crystal X-ray diffraction. The compound I is crystallized in P2₁/c space group of monoclinic system, with a = 11.5236(19) ?, b = 8.7389(17) ?, c = 10.684(3) ? and α = 90.00°, β = 107.76(3)°, γ = 90.00°. The compound II is crystallized in Cc space group of monoclinic system, with a = 10.688(2) ?, b = 14.2181(18) ?, c = 7.9836(15) ? and α = 90.00°, β = 125.801(7)°, γ = 90.00°. In both crystal structures, the intermolecular N–H–O and O–H–N hydrogen bonds link the molecules, which effectively stabilize the structures.     

Crystal and molecular structures oftrans-dichloro-(ethylene) (4-methylpyridine)platinum(II) andtrans-dichloro(ethylene) (2,4,6-trimethylpyridine)platinum(II)

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.     

Crystal Structure of [Zn(2-Bromobenzoato)<Subscript>2</Subscript>]<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript> and [Zn(2-Bromobenzoato)<Subscript>2</Subscript>(<Emphasis Type="Italic">N</Emphasis>-Methylnicotinamide)]<Subscript>2</Subscript>

Abstract  

The syntheses and structural characterizations of two novel 2-bromobenzoatozinc(II) complexes—[Zn(2-BrC₆H₄COO)₂] _n (I) and [Zn(2-BrC₆H₄COO)₂(mnad)]₂ (II), where mnad is N-methylnicotinamide are reported. Compound (I) crystallized with a monoclinic lattice (space group P2₁/c) and is polymeric in solid state. Its cell parameters are: a = 7.37220(10) Å, b = 19.9639(3) Å, c = 30.2756(5) Å, β = 94.7510(7)°, V = 4440.59(12) ų, Z = 4. The coordination environments of all zinc atoms are distorted tetrahedra built from four carboxylate oxygen atoms coming from four 2-bromobenzoato ligands. Compound (II) crystallized with a monoclinic lattice (space group P2₁/c) with a = 11.7488(2) Å, b = 20.3683(3) Å, c = 9.30130(10) Å, β = 100.3941(11)°, V = 2189.30(5) ų, Z = 2. This dimeric molecule features a paddle-wheel [Zn₂O₈] cage in solid state; the coordination environment of the central atom is square pyramidal consisting of four carboxylate oxygen atoms and the pyridine N atom of the mnad ligand.     

Crystal and molecular structure of (Z)-2-(1,3-benzothiazol-2-yl)-2-(6,7,8,9-tetrahydro-5H-benzocyclohepten-5-ylidene)ethanonitrile

The title compound C₂₀H₁₆N₂S is crystallized in the monoclinic space groupP2₁/c with cell parametersa=10.663(4),b=17.585(9),c=9.418(5)Å,=115.23°(4),V=1598(3)ų,Z=4. The structure was refined by full-matrix least-squares methods using X-ray data set collected at room temperature. A finalR _F =0.033 andR _w =0.048 for 2225 unique reflections withI> 3(I) and 272 variables was obtained. The X-ray crystallographic study establishes theZ stereochemistry of the title compound.