Synthesis and Crystal Structure of (5-Methyl-3-phenyl-1<Emphasis Type="Italic">H</Emphasis>-pyrazol-1-yl)-[5-(<Emphasis Type="Italic">p</Emphasis>-tolylamino)-2<Emphasis Type="Italic">H</Emphasis>-1,2,3-triazol-4-yl]methanone

Abstract  

(5-Methyl-3-phenyl-1H-pyrazol-1-yl)-[5-(p-tolylamino)-2H-1,2,3-triazol-4-yl]methanone was synthesized and characterized by ¹H NMR, MS and IR spectra data. The structure of title compound was identified by X-ray diffraction. Compound, C₂₀H₁₈N₆O, Mr = 358.40, crystallizes in the triclinic space group P-1 with unit cell parameters a = 10.303(6), b = 12.489(7), c = 15.305(9) ?, α = 108.489(12), β = 101.920(11), γ = 96.971(13)°, V = 1790.0(17) ?³, Z = 4, Dx = 1.330 mg/cm³. The final R was 0.0520.     

Crystal Structure and Conformational Analysis of 4-[(<Emphasis Type="Italic">p</Emphasis>-<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>-Dimethylamino)Benzylidene]-2-Phenyloxazole-5-One

Abstract  

Molecular and crystal structure of 4-[(p-N,N-dimethylamino)benzylidene]-2-phenyloxazol-5-one, C₁₈H₁₆N₂O₂, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a = 12.1704(23) ?, b = 3.9810(5) ?, c = 30.9603(56) ?, β = 101.176(15)°, Z = 4, D _x = 1.32 g/cm³, μ(Mo Kα) = 0.087 mm⁻¹, and space group is P12₁/c1. The structure was solved by direct methods and refined to a final R = 0.047 for 3166 reflections with I > 2σ(I). The crystal structure is stabilized by C–H⋯O and C–H⋯N type intra-molecular, C–H⋯O type inter-molecular interactions. To enlighten the flexibility and the geometric isomerism (E or Z) of the title compound, the selected torsion angle is varied from −180 to 180° in every 10° separately and molecular energy profile is calculated and analyzed.     

An X-ray Crystallographic Study of 1,4-Di[(<Emphasis Type="Italic">E</Emphasis>)-2-(<Emphasis Type="Italic">p</Emphasis>-tolyl)-1-diazenyl]piperazine

Abstract  

The crystal structure of methyl 1,4-di[(E)-2-(p-tolyl)-1-diazenyl]piperazine (4) has been determined by single crystal X-ray diffraction analysis. The bis-triazene (4) adopts a normal chair conformation in the piperazine ring, with puckering parameters : φ₂ = −29(5)°, Q_T = 0.534(2) ? and θ₂ = 177.0(2)°. The crystal structure of 4 is compared with the structure of the triazene (2a) and the closely related bis-triazenes (3 and 5a). The piperazine ring of 2a and 4 adopt a typical chair conformation, whereas the piperazine ring of 3 adopts an unusual pseudo-boat conformation. Crystal data: 4 C₁₈H₂₂N₆, triclinic, space group P[`1] P\overline{1} , a = 6.8925(2) ?, b = 7.8574(3) ?, c = 16.8856(8) ?, α = 103.103(2)°, β = 90.528(2)°, γ = 101.776(2)° and V = 870.44 (6) ?³, for Z = 2.     

Synthesis,Characterization and Antibacterial Activity of <Emphasis Type="Italic">N</Emphasis>-(<Emphasis Type="Italic">N</Emphasis>-Acetic Acid-yl-Phthalimide-5-yl) Maleamic Acid Dihydrate

Abstract  

The compound N-(N-acetic acid-yl-phthalimide-5-yl) maleamic acid (C₁₄H₁₀N₂O₇, M _r  = 318) was synthesized and its structure was characterized by elemental analysis, ¹H NMR and IR spectra. The single crystal of the title compound (C₁₄H₁₄N₂O₉, M _r  = 354.27) was cultured and its structure was determined by single crystal X-ray diffraction. The crystal belongs to monoclinic system, space group P21/c with a = 14.3859(19), b = 12.5835(18), c = 8.6934(15) ?, β = 102.824(2)°, V = 1534.5(4) ?³, Z = 4, D _c  = 1.534 g cm⁻³, μ(Mo Kα) = 0.131 mm⁻¹, F(000) = 736. The final refinement gave R = 0.0652, wR(F ²) = 0.1239 for 2,703 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the asymmetric unit of the title compound contains one N-(N-acetic acid-yl-phthalimide-5-yl) maleamic acid molecule and two water molecules. One of the two water molecules is disordered. The phthalimide group is essentially planar. The crystal structure of the title compound is stabilized by N–H…O and O–H…O hydrogen bonds interactions. The compound N-(N-acetic acid-yl-phthalimide-5-yl) maleamic acid possesses moderate antibacterial activity.     

Synthesis,Characterization and Antibacterial Activity of <Emphasis Type="Italic">N</Emphasis>-(2,3,4-Trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine

Abstract  The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C₁₈H₂₁NO₃, M _r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2₁/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) ?, β = 92.056(2)°, V = 1,632.4(3) ?³, Z = 4, D _c = 1.218 g cm⁻³, λ = 0.71073 ?, μ(Mo Kα) = 0.083 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0497, wR(F ²) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity. Graphical Abstract  The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C₁₈H₂₁NO₃, M _r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2₁/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) ?, β = 92.056(2)°, V = 1,632.4(3) ?³, Z = 4, D _c = 1.218 g cm⁻³, λ = 0.71073 ?, μ(Mo Kα) = 0.083 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0497, wR(F ²) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity.      

Synthesis and Crystal Structure Determination of 3-Phenyl-2-(2-phenylhydrazino)-4<Emphasis Type="Italic">H</Emphasis>-1-benzothiopyran-4-one

Abstract  

A new type of substituted benzothiopyranone, 3-phenyl-2-(2-phenylhydrazino)-4H-1-benzothiopyran-4-one, has been prepared by the condensation-acid cyclization of polylithiated phenylacetic acid phenylhydrazide with lithiated methyl thiosalicylate. Absorption spectra, especially ¹³C NMR, provided good indication of its structure, which was conclusively established with X-ray crystal structure analysis. In comparison to the few benzothiopyran X-ray reports documented, the benzothiopyranone ring of the molecule was found to be essentially planar, with the 3-phenyl ring nearly perpendicular to the benzothiopyranone fused-ring system. Crystals of C₂₁H₁₆N₂OS are orthorhombic, P2₁2₁2₁, a = 10.140(4) ?, b = 10.432(4) ?, c = 16.228(7) ?, Z = 4, V = 1717(1) ?³, R ₁ = 0.0267 and wR ₂ = 0.0725 for reflections with I > 2σ(I). The molecular packing in the crystal is the result of N–H···O hydrogen bonding.     

Structure and Antibacterial Activity of 3-(3,4-Dimethoxyphenyl)furan-2(5<Emphasis Type="Italic">H</Emphasis>)-ones

Abstract  

Crystalline hydrate of the title compound (5), C₁₉H₂₆N₂O₅·2(H₂O), was structurally characterized by single crystal X-ray diffraction. It crystallizes in monoclinic system space group P 21/c with a = 7.3987(7) ?, b = 17.8691(16) ?, c = 17.0022(13) ?, β = 112.944(3)°, V = 2070.0(3) ?³, Z = 4, R ₁ = 0.0592, wR ₂ = 0.1016, and T = 298(2) K. The X-ray structure determination revealed that the center furanone ring is nearly coplanar with 3,4-dimethoxybenzene ring, making a dihedral angle of 0.860(69)°. Two kinds of centrosymmetric tetramers characterized by graph-set motifs of R ₇⁸(36) and R ₄⁶(32) are formed through O–H···O, O–H···N and C–H···O hydrogen bonding interactions, which generate a sheet of edge-fused rings parallel to the (011) plane. These sheets are further linked into a three dimensional network by C–H···π interactions. Nine 3-(3,4-dimethoxyphenyl)furan-2(5H)-ones were synthesized and fully characterized by elemental analysis, MS and ¹H NMR. All of them were evaluated for antimicrobial activities against three Gram-positive organisms and a Gram-negative organism, and compound 5 was the most active against Staphylococcus aureus ATCC 25923.     

Synthesis and Crystal Structures of <Emphasis Type="Italic">o</Emphasis>-[(Phenyl/<Emphasis Type="Italic">p</Emphasis>-methoxyphenyl)carbamoyl]benzene Sulfonamides

Abstract  

o-[(Phenyl/p-methoxyphenyl)carbamoyl]benzene sulfonamides were synthesized in a straightforward manner utilizing directly saccharin and aniline/p-anisidine as starting material and their crystal structures have been determined. (C₁₃H₁₂N₂O₃S): Mr = 276.31, monoclinic, P2₁/c, a = 10.277(6), b = 7.501(2), c = 16.261(10) ?, β = 96.37(2)°, V = 1,245.8(11) ?³, Z = 4. (C₁₄ H₁₄ N₂ O₄ S): Mr = 306.33, monoclinic, P2₁/c, a = 10.381(5), b = 7.861(2), c = 16.837(9) ?, β = 93.43(2)°, V = 1,371.5(10) ?³, Z = 4. In both structures the phenyl rings are inclined at 47.09(7) and 39.88(5)° with respect to each other and the structures are characterized by extensive inter and intramolecular hydrogen bonds.     

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.     

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 Structures of Di-1-Adamantylthiophosphinic Chloride, <Emphasis Type="Italic">P</Emphasis>,<Emphasis Type="Italic">P</Emphasis>-Diphenyl-<Emphasis Type="Italic">N</Emphasis>-Benzyl Phosphinothioic- and Selenoic- Amides

Abstract  Synthesis and X-ray structural determination of three phosphorus compounds are reported. (3b) is monoclinic P2(1)/c with a = 11.852(1), b = 12.825(1), c = 12.445(1) ?, β = 103.693(1)o; (4a) and (4b) are monoclinic P2(1)/n with a = 12.1422(16), b = 9.0860(12), c = 14.845(2) ?, β = 96.498(3)o for (4a), and a = 12.2714(16), b = 9.2812(12), c = 14.800(2) ?, β = 97.176(2)o for (4b). They all exhibit distorted tetrahedral geometry about the P atom. Ph₂P(X)NHC₇H₇ (X=S (4a) and X=Se (4b)) show typical P–S and P–Se double bond distances and P–N single bonds, while P–S bond in 1-Ad₂P(S)Cl (3b) is comparable to P–S single bonded probably due to the largeness of 1-adamantyl groups. Graphical Abstract  Synthesis and X-ray structural determination of 1-Ad₂P(S)Cl (3b), Ph₂P(S)NHC₇H₇ (4a) and Ph₂P(Se)NHC₇H₇ (4b) are reported.      

Synthesis and Crystal Structure of Bis[<Emphasis Type="Italic">N</Emphasis>-{(<Emphasis Type="Italic">S</Emphasis>)-1-Phenylethyl}-<Emphasis Type="Italic">N</Emphasis>-{1-(2-Pyridinyl)Methyl}Amine] Zinc(II) Perchlorate

Abstract  

The reaction of N-[(S)-1-phenylethyl]-N-[1-(2-pyridinyl)methyl]amine (PEPMA) with Zn(ClO₄)₂ affords (PEPMA)₂Zn(ClO₄)₂ at room temperature. The complex is characterized by elemental analysis, ¹H-MNR and X-ray crystallography. The crystal system is orthorhombic with space group of P2₁2₁2₁ and unit cell parameters: a = 8.6911(4), b = 9.7755(7), c = 37.275(2) ?, V = 3166.9(3) ?³, Z = 4, D _x  = 1.445 Mg/m³. The crystal structure reveals that zinc metal is ligated by two PEPMA ligands in a distorted tetrahedral fashion. Interestingly, both nitrogen atoms of amine at PEPMA to the central zinc metal exhibit (R)-configuration.     

Syntheses,Crystal Structures and Physical Properties of Cd(II) and Mn(II) Complexes with <Emphasis Type="Italic">Trans</Emphasis>-1,2-di(4-pyrindyl)ethylene and <Emphasis Type="Italic">P</Emphasis>-(carboxyl-methyloxy)-benzenecarboxylic Acid

Abstract  

Two complexes [Cd₂(dpe)₃(H₂O)₈]·(dpe)·(hssal)₂·(H₂O)₂ 1, [Mn(dpe)₂(Hpcmb)₂·(H₂O)₂] 2, (dpe = trans-1,2-di(4-pyrindyl)ethylene; H₂hssal = sulphosalicylic acid; H₂pcmb = p-(carboxyl-methyloxy)-benzenecarboxylic acid) has been prepared, and was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. Structure indicates in complex 1 that Cd(II) is a distorted octahedral coordination geometry. The hssal²⁻ anions are localized between 2-D sheets {[Cd(dpe)₂(H₂O)₄]²⁺(dpe)}n and {{[Cd(dpe)₂(H₂O)₄]²⁺}n as count anions and bridge to further connect these 2-D sheets through hydrogen bond O–H···O to form 3-D structure. The complex 2 is a single molecule structure. In 2, Each Mn(II) atom is six-coordinated with a distorted octahedral coordination geometry. The single molecule units are extended into three-dimensional structure via π–π, hydrogen bonding interactions. The thermogravimetric behavior and luminescent property of complex 1 were investigated.     

Experimental and Semi-Empirical and DFT Calculational Studies on (<Emphasis Type="Italic">E</Emphasis>)-2-[(2,4-Dichlorophenylimino) methyl]-<Emphasis Type="Italic">p</Emphasis>-cresol

Abstract  

The molecular and crystal structure of the title compound, C₁₄H₁₁Cl₂NO, has been determined by X-ray single crystal diffraction technique. The compound crystallizes in the orthorhombic, space group Pbca with unit cell dimensions a = 7.5537(10) ?, b = 11.5518(13) ?, c = 29.760(4) ?, M _r  = 280.14, V = 2596.8(6) ?³, Z = 8, R ₁ = 0.065 and wR ₂ = 0.191. The title compound exists in the enol–imine tautomeric form with a strong intramolecular O–H···N hydrogen bond. The dihedral angle between the two benzene rings is 37.66(15)°. The asymmetric unit in the crystal structure contains only one neutral molecule. Calculational studies were performed by using AM1, PM3, PM6 semi-empirical and DFT methods. Geometry optimizations of compound have been carried out by using three semi-empirical methods and DFT method and bond lengths, bond and torsion angles of title compound have been determined. Dipole moments (Debye) and the energy parameters of compound (kcal/mol) were calculated by using above mentioned calculation methods. Atomic charge distribution has been obtained from AM1, PM3, PM6 and DFT. In order to determine conformational flexibility on the molecule, molecular energy profile of the title compound was obtained with respect to the selected torsion angle T(N1–C7–C1–C2), which is varied from −180° to +180° in every 10 via PM3 semi-empirical method.     

<Emphasis Type="Italic">Mangifera indica</Emphasis>: Crystal Structures of Two Cycloartane Type Triterpenoids Present in the Bark

Abstract  

Cycloart-23-ene-3-oxo-26-oic acid or Mangiferolic acid (C₃₀H₄₈O₃), compound 1 and Cycloart-23-ene-3β,25-diol (C₃₀H₅₀O₂) compound 2, were isolated from the bark of Mangifera indica. The structures of both compounds 1 and 2 were established by spectral and X-ray diffraction studies. Compound 1 crystallizes in the monoclinic space group P2₁ with unit cell parameters a = 8.416(1), b = 20.638(2), c = 17.203(2) Å, β = 91.779(2)°, Z = 2. Compound 2 crystallizes in the monoclinic space group C 2 with unit cell parameters a = 33.824(9), b = 7.413(2), c = 11.136(3) Å, β = 98.347(4)°, Z = 4. Both structures (1 and 2) were solved by direct methods and refined to R = 0.0511 and 0.0588, respectively. For compound 1, there are two independent molecules (1A and 1B) per asymmetric unit and one disordered trichloride methane molecule. For compound 2, there is positional disorder of the side chain at C17 beginning from C23 up to C27. All the rings of both steroid skeletons are trans connected. For structures 1A, 1B and 2, the six-membered rings A, B and C have a deformed chair, deformed chair and sofa conformations. The five-membered rings D adopt a half-chair conformation. In structure 1, there are two types of hydrogen bonds, the first type, the molecules 1A and 1B are linked by pairs of O(3A)–H···O(1B) and O3B H3B···O1A hydrogen bonds. In addition, both O(1A)–H and O(1B)–H hydroxyl groups participate in a second type of hydrogen bond involving the atoms O(2A) and O(2B) of adjacent molecules, respectively. In structure 2, there is a characteristic pattern observed in packing diagram is that both hydroxyl groups (O1–H and O2–H) participate as hydrogen bond donors and acceptors. In both structures 1 and 2, the hydrophobic part of the steroid nucleus is stabilized by C–H···O interactions and van der Waals forces.     

Co-crystal Structure of 11-Hydroxy-2,3,9-trimethoxy-6<Emphasis Type="Italic">H</Emphasis>-chromeno[3,4-<Emphasis Type="Italic">b</Emphasis>]chromen-12-one and 11-Hydroxy-2,3,9-trimethoxy-chromeno[3,4-<Emphasis Type="Italic">b</Emphasis>]chromene-6,12-dione

Abstract  

A 1:1 co-crystal structure of 11-hydroxy-2,3,9-trimethoxy-6H-chromeno[3,4-b]chromen-12-one and 11-hydroxy-2,3,9-trimethoxy-chromeno[3,4-b]chromene-6,12-dione (stemonone) was crystallized from the reaction mixture of 6-deoxyclitoriacetal and methanesulfonyl chloride, and its structure was characterized by X-ray diffraction. This co-crystal crystallizes in a triclinic crystal system, space group P(−1) with unit cell parameters of a = 8.1317(3) Å, b = 9.8224(4) Å, c = 10.7268(3) Å, α = 78.116(1)°, β = 77.463(1)°, γ = 77.140(1)°, Z = 2 and V = 804.11(3) Å³. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F ² to final values of R ₁ = 0.0501 and wR ₂ = 0.1520.     

Synthesis and Characterization of <Emphasis Type="Italic">N,N</Emphasis>-di(prop-2-ynyl)-<Emphasis Type="Italic">p</Emphasis>-toluidine

Abstract  

In order to investigate the intramolecular [4 + 2] cycloaddition, we prepared some new tertiary N-(5-substituted-2-furfuryl)-N-prop-2-ynyl-p-toluidines [Hergold-Brundić et al., Acta Cryst C56:e520, 2000; Mance and Jakopčić, Mol Divers 9:229, 2005; Mance, “unpublished results”] by the alkylation of secondary N-(5-substituted-2-furfuryl)-p-toluidines with the propargyl-bromide [Mance and Šindler-Kulyk, Synth Commun 26:923, 1996]. In the course of preparation of N-(5-methoxy-2-furfuryl)-N-prop-2-ynyl-p-toluidine [Mance, “unpublished results”], besides the main product (compound 1) (Scheme 1) we obtained N,N-di(prop-2-ynyl)-p-toluidine (compound 2) as the colourless crystals. The title compound 2, N,N-di(prop-2-ynyl)-p-toluidine, C₁₃H₁₃N, crystallizes in monoclinic C 2/c space group with unit cell parameters: a = 19.5319(9) ?, b = 7.5230(3) ?, c = 15.9000(7) ?, β = 112.554(5)°, V = 2157.64(18) ?³, Z = 8. The crystal structure is dominated by van der Waals forces only. The bond distances around amine N atom correspond to σ dominated bonds (1.467(2), 1.462(2) and 1.419(2) ?). The angles sum around amine N atom is in accord with sp³ hybridization (343°).     

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 One Trinuclear di-<Emphasis Type="Italic">n</Emphasis>-butyltin(IV) Complex with Salicylaldoxime

Abstract   One trinuclear di-n-butyltin(IV) complex with salicylaldoxime (o-HON=CHC₆H₄OH=HONZOH), (Bu₂Sn)(Bu₂SnO)(Bu₂SnOH)(ONZOH)(ONZO), has been synthesized and characterized by elemental analyses, IR spectrum, and single crystal X-ray diffraction. This complex is a small cluster displaying two unequivalent salicylaldoximate with one seven-coordinate pentagonal–bipyramidal tin atom linked two five-coordinate trigonal–bipyramidal tin atoms via a network of oxygen atoms by Sn–O–Sn bridges. The hydrogen bonds (o-HON=CHC₆H₄–O…H–O) are observed in the complex. These hydrogen bonds include intramolecular hydrogen bonds and intermolecular hydrogen bonds. (Bu₂Sn)(Bu₂SnO)(Bu₂SnOH)(ONZOH)(ONZO) belongs to monoclinic: space group P2₁/n, with a = 12.2307(15) ?, b = 17.361(2) ?, c = 20.976(3) ?, β = 94.424(2)°, V = 4440.5(10) ?³, Z = 4, D _c  = 1.500 g/cm³, μ(MoKα) = 1.715 mm⁻¹, F(000) = 2024, and final R ₁ = 0.0426, wR ₂ = 0.1064 for observed reflections 7779(I > 2σ(I)). Index abstract  The title compound, di-n-butyltin(IV) complex with salicylaldoxime, was synthesized and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the molecular structure of the title compound is trinuclear. The complex is a small cluster displaying two unequivalent salicylaldoximate with one seven-coordinate pentagonal–bipyramidal tin atom linked two five-coordinate trigonal–bipyramidal tin atoms via a network of oxygen atoms by Sn–O–Sn bridges.      

Synthesis and Crystal Structure of Bis(<Emphasis Type="Italic">N</Emphasis>-alkyl-<Emphasis Type="Italic">N</Emphasis>-phenyl dithiocarbamato)mercury(II)

Abstract  

The mixed ligand dithiocarbamate complex was synthesized by the reaction between the ammonium salt of the dithiocarbamate ligands with mercury salt. There are two mercury complexes in the asymmetric unit with a compositional disorder between an ethyl group and a methyl group. A distorted tetrahedral geometry is found for each mercury atom defined by four sulphur atoms derived from two asymmetrically chelating dithiocarbamate ligands. IR spectra show thioureide υ(C–N) bands at 1491 cm⁻¹ which is higher than observed in the simple complexes of the same ligands. The effect of alkyl substituents were observed in the magnetic unequivalence of the thioureide and phenyl units in the NMR spectroscopy. The molecules are related to each other by virtue of the compositional disorder which exists at three positions in the alkyl group across the unit. The compound crystallizes in the triclinic space group P-1 with a = 10.4764(10) ?, b = 11.0433(10) ?, c = 18.5566(17) ?, α = 97.8980(10)^°, β = 95.3340(10)^°, γ = 110.3010(10)^°, and Z = 2.