Syntheses and Crystal Structures of Two Apigenin Alkylation Derivatives

Abstract Two apigenin alkylation derivatives, 4′,7-dimethoxyl-5-hydroxyflavone (I) and 4′,7-diethoxyl-5-hydroxyflavone (II), have been synthesized and their crystal structures were determined by ¹H NMR and single crystal X-ray diffraction study. (I) is triclinic, space group P−1 with a = 7.120(5) ?, b = 7.297(5) ?, c = 13.559(10) ?, α = 89.313(12)°, β = 86.298(12)°, γ = 83.999(13)° and Z = 2. (II) is monoclinic, space group P 2₁ /c with a = 16. 309(4) ?, b = 7.303(2) ?, c = 15.185(4) ?, α = 90.00°, β = 115.70(2)°, γ = 90.00° and Z = 4. They have the same flavone skeleton which is composed of a benzopyranone moiety and a phenyl moiety. Molecules of (I) are linked into a two-dimensional network by a combination of C–H···O hydrogen bond and π–π stacking interactions. (II) shows some discrepancies with (I) and the molecules are linked into a column by π–π stacking interaction. Graphical Abstract Two apigenin alkylation derivatives, 4′,7-dimethoxyl-5-hydroxyflavone (I) and 4′,7-diethoxyl-5-hydroxyflavone (II) were synthesized and their crystal structures were determined by single-crystal X-ray diffraction. Hydrogen bonding and π–π stacking interactions assemble (I) into a two-dimensional network, and in the crystal structure of (II), π–π stacking interaction leads to the formation of a column.      

Syntheses and Crystal Structures of New Unsymmetrical Tetrathiafulvalene-Based Amidoquinline Derivatives

Abstract  

Two new unsymmetrical tetrathiafulvalene-based amidoquinline derivatives of 8-amide quinline of PDT-TTF and BTTF (PDT = propylenedithio, TTF = tetrathiafulvalene, BTTF = benzotetrathiafulavalene) (6, 11) have been synthesized and characterized by ¹H NMR, MS, and X-ray crystal structural determination. The crystal structures determination shows that they have completely different solid-state constructs due to the different functional group on the side of tetrathiafulvalene group. The molecules of compound 6 are assembled into 1D helical chain along c-axis via hydrogen bond interactions; these helical chains are further connected by the transverse S⋯S van der Waals interactions, thus, resulting to form a layered architecture. The molecules of compound 11 are assembled into 1D chain along c-axis via hydrogen bond and the S⋯S van der Waals interactions. Structures analysis indicate that compound 6 belong to orthorhombic system, space group P2(1)2(1)2(1), with crystal data a = 6.140(7) ?, b = 12.628(14) ?, c = 23.707(3) ?, V = 1838.0(4) ?³, Z = 4, F(000) = 872, R ₁ = 0.0570, wR ₂ = 0.0910. Compound 11 belong to triclinic system, space group P-1, with crystal data a = 9.532 (2) ?, b = 10.194(2) ?, c = 10.848(3) ?, α = 79.980(5)°, β = 89.342(4)°, γ = 75.226(5)°, V = 1003.1(4) ?³, Z = 2, F(000) = 492, R ₁ = 0.0686, wR ₂ = 0.1656.     

Syntheses, Crystal Structures and Antibacterial Activities of Two Antipyrine Derivatives

Abstract  

Two new antipyrine derivatives, 4-{[1-(5-bromo-2-methoxyphenyl)methylidene]amino}-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one (C₁₉H₁₈BrN₃O₂, 1) and 4-{[1-(2-hydroxy-3-ethoxyphenyl)methylidene]amino}-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one (C₂₀H₂₁N₃O₃, 2), were synthesized and structurally characterized by elemental analysis, IR and single crystal X-ray diffractions. Compound 1 crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a = 6.987(1) ?, b = 27.930(2) ?, c = 9.483(1) ?, β = 109.36(2)°, V = 1745.9(4) ?³, Z = 4, R ₁ = 0.0430, and wR ₂ = 0.0870. Compound 2 crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a = 19.523(2) ?, b = 7.466(1) ?, c = 12.954(2) ?, β = 108.797(1)°, V = 1787.5(4) ?³, Z = 4, R ₁ = 0.0421, and wR ₂ = 0.1032. X-ray structure determinations revealed that the molecules of both compounds display trans configurations about the C=N double bonds. In the crystal structures, molecules are linked together by intermolecular C–H···O hydrogen bonds. Both compounds show strong antibacterial activities.     

Syntheses and Crystal Structures of Three Pyrrole-2-Carboxylate with C3-Symmetry

Journal of Chemical Crystallography - The reaction of three equivalents of 2-(trifluoroacetyl)pyrrole with triols [RC(CH2OH)3, R=H, CH3, CH2OH] produce triesters of pyrrole-2-carboxylic acid...     

Syntheses,Crystal Structures and Fluorescence Properties of Zn(II) Complexes with Pyrazolone Derivatives

Abstract   N-(1,3-Diphenyl-4-benzal-5-pyrazolone)-salicylidene hydrazone(H₂L ¹ ) and its zinc complex Zn(HL ¹ )₂ · 2CH₃OH (1) have been synthesized and characterized by elemental analyses, IR spectra, thermal analyses and single-crystal X-ray diffraction studies. The X-ray diffraction analyses of the complex Zn(HL ¹ )₂ · 2CH₃OH (1) and the known compound Zn₄(L ² )₄ (2) (H₂L ²  = N-(1,3-diphenyl-4-phenylethylene-5-pyrazolone)-salicylidene hydrazone) show that different acyl groups in position 4 of pyrazolones may lead to the different coordination mode of the ligands and distinctive structures of the same central metal Zn(II) complexes, of which 1 is a mononuclear complex while 2 is a tetranuclear complex. Meanwhile, two Zn(II) complexes have different thermal stabilities and fluorescence properties. Graphical Abstract        

Syntheses and Crystal Structures of Two Ferrocenyl Dicarboximides

Abstract  

Reactions of 1,1′-ferrocenedicarboxylic chloride with 2-aminopyrimidine and 2-aminopyrazine produce organometallic dicarboximides I and II, respectively. They crystallize in space groups F dd2 and P2₁/c, respectively. The molecules of I lying on twofold rotation axes are linked into a B-faced sheet by a C–H···O=C hydrogen bond [H····O = 2.46, C···O = 3.163(7) ? and C–H···O = 132°]. The sheets are linked into a layered structure by two types of weak C–H···O=C hydrogen bonds [H···O = 2.71, C···O = 3.340(8) ? and C–H···O = 126°; H···O = 2.69, C···O = 3.303(10) ? and C–H···O = 124°]. The molecules of II are linked into a centrosymmetric R ₂²(12) dimer by a C–H···O hydrogen bond [H···O = 2.40, C···O = 3.321(10) ? and C–H···O = 172°]. The dimers are further packed along the a axis by a C–H···O hydrogen bond [H···O = 2.69, C···O = 3.416(9) ? and C–H···O = 135°] to give an [100] double-chain. The double-chain is packed in the [010] direction by a C–H···O=C hydrogen bond [H···O = 2.69, C···O = 3.532(9) ? and C–H···O = 150°]. Further the intermolecular C–H···N hydrogen bond involving the cyclopentadienyl group as a hydrogen-bond donor and pyrazine N atom as an acceptor [H···O = 2.71, C···N = 3.536(10) ? and C–H···N = 148°] leads to a three-dimensional framework structure.     

The Syntheses and Crystal Structures of Metronidazole-derived Compounds

Abstract Metronidazole (MET-OH), widely used as an antibacterial agent, is found to have some side effects on human bodies. Due to these disadvantages, people have been looking for its modification compounds for substituents. In this article, four MET-OH derivatives were designed, prepared, and structurally characterized by single crystal X-ray diffraction. These compounds are MET-OTs (1), MET-Br (2), MET-Cl (3), and MET-I (4). X-ray structure analyses revealed that, 1 crystallized in the monoclinic system with space group P2 ₁ /c, with a = 16.1178, b = 7.5473, c = 13.4161 ?, V = 1520.3 ?³, β = 111.3210^o and Z = 4. 2 crystallized in the monoclinic system with space group P2 ₁ /c, with a = 12.079, b = 11.089, c = 6.380 ?, V = 847.1 ?³, β = 97.57^o and Z = 4. 3 crystallized in the monoclinic system with space group P2 ₁ /c, with a = 12.098, b = 11.007, c = 6.295 ?, V = 830.3 ?³, β = 97.886^o and Z = 4. 4 crystallized in the triclinic system with space group P1, with a = 6.192, b = 7.740, c = 10.001 ?, V = 457.9 ?³, α = 89.073, β = 86.903, γ = 73.097^o and Z = 2. Index Abstract In this article, metronidazole-derived compounds were prepared and structurally characterized by single crystal X-ray diffraction      

Syntheses and Crystal Structures of Two 2-Aminoisoflavones

Abstract  

2-Amino-7,4′-dimethoxyisoflavone (I), C₁₇H₁₅NO₄ and 2-amino-7-methoxy-4′-hydroxyisoflavone (II), C₁₆H₁₃NO₄ were synthesized and their crystal structures were determined by single-crystal X-ray diffraction. They all crystallize in the monoclinic crystal system, space group P21/c. The cell dimensions of I are a = 15.6673(17) ?, b = 7.3998(8) ?, c = 13.2919(14) ?, β = 111.4460(10)°, D _c = 1.377 mg/mm³, V = 1,434.3(3) A³, Z = 4 and those of II are a = 10.990(7) ?, b = 11.879(7) ?, c = 10.422(6) ?, β = 96.904(11)°, D _c = 1.393 mg/mm³, V = 1,350.8(14) A³, Z = 4. A combination of F-type and T-type aromatic–aromatic interaction and hydrogen bonding links the molecules of I into a tri-dimensional framework structure. In the crystal structure of II, paired tri-centered hydrogen bond generates a R₄²(21) ring and the R₄²(21) rings link the molecules into a sheet.     

Syntheses,Crystal Structures and Fluorescence Properties of Three Complexes Based on 2,2'-Quinoline-4,4'-dicarboxylic Ligands

Crystallography Reports - Three new coordination complexes, [Mn(L)(H2O)4⋅(H2O)3]2 (1), [Mg(L)(H2O)4⋅(H2O)3]2 (2), and [Cu(L)(phen)⋅(H2O)4]2 (3) (H2L =...