Synthesis,Crystal Structure and Characterization of (Z)-2-N′-hydroxyisonicotinamidine

The compound (Z)-2-N′-hydroxyisonicotinamidine, (2) was synthesized and characterized by ¹H NMR, FT-IR, FAB-Mass, UV-Visible Spectra, and elemental Analysis. Its molecular structure was solved by single crystal X-ray diffraction method. The title molecule, C₆H₇N₃O is crystallized in the orthorhombic crystal system with the space group Pna2₁ and with unit cell parameters a = 12.5664(8) Å, b = 8.8622(6) Å, c = 5.7953(4) Å, α = 90°, β = 90°, γ = 90°, and Z = 4. The molecular and crystal structure of the title molecule is stabilized by an intramolecular interaction of the type N—H···O, and the intermolecular interactions of types N—H···N and O—H···N.     

Synthesis,Characterization and Structural Conformation Studies of 2-Amino-3-ethoxycarbonyl-4-(4′-methoxy Phenyl)-4H-pyrano-[3,2-c]-chromene-6-methyl-5-one

2-amino-3-ethoxycarbonyl-4-(4′-methoxy Phenyl)-4H-pyrano-[3,2-c]-chromene-6-methyl-5-one was synthesized by the two-component reaction of 6-methyl-4-hydroxy coumarin with 4′-methoxy-2-cyano cinnamate, which was synthesized by Knoevenagel reaction with 88% yield. The compound obtained was characterized by spectroscopic techniques and confirmed by X-ray crystallographic studies. The crystallographic data analysis reveals that the title compound crystallizes in the triclinic space group \(P\overline{1}\) with cell parameters a = 7.7750(8) Å, b = 9.0310(6) Å, c = 15.6120(17) Å, α = 77.249(7)°, β = 115.860(3)°, γ = 70.139(7)°, V = 1,003.0(16) Å³ for Z = 4. The structure has been solved by direct methods and refined to R1 = 0.0552 for 3,164 observed reflections with I > 2 σ(I). The pyran ring is in a flattened boat conformation. The carbonyl group is oriented in a -synperiplanar(cis) conformation.

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Synthesis and structure analysis of 2-(2′-propanonylthio)-3-(o-methyl phenyl) quinazol-4(3H)-one

The three-dimensional molecular and crystal structure of 2-(2'-propanonylthio)3-(o-methyl phenyl)quinazol-4(3H)-one has been determined by X-ray crystallographic methods. This compound crystallizes in the orthorhombic space group P_bca with unit cell parameters: a=9.649(5), b=30.102(10), c=11.403(9)Å. It has been solved by direct methods and refined to a residual index of 0.054. The magnitude of torsion along C16— C11— N3— C4 bond is 93.5(4)°. The dihedral angle between the plane comprising all the ring atoms of quinazoline moiety and the atoms of the methyl substituted phenyl ring is 94.12(1)°. The crystal structure is stabilized by one intramolecular C— HsO interaction and three intermolecular C— HsN contacts.     

Synthesis,crystal structure and spectral studies of the complex [Ni(C3H4N2)4(H2O)2]·(C6H4COSO2N)2

The title compound has been synthesized and its crystal structure determined at room temperature.M _r =731.39, triclinic, space groupP¯1,a=9.020(3),b=11.280(7),c=7.784(2)Å,=97.05(4),=97.08(2), =105.32(4)°, U=748(1)ų,Z=1,D _calc.=1.624 g/cm³. The finalR is 0.030 for 3095 independent observed reflections withI3(I). The crystal structure consists of repeated [Ni(im)₄(H₂O)₂]²⁺ cations and noncoordinated saccharin anions. In the complex cation [Ni(im)₄(H₂O)₂]²⁺, Ni² is bonded to four N atoms from four imidazole molecules and two O atoms from two water molecules forming an approximately square octahedral stereochemistry. The d-d transition spectrum of the title compound is also reported and is explained perfectly with the scaling radial theory which was proposed by us.     

Synthesis and structure of (NH4)3[UO2(C3H2O4)2(NCS)] · 2H2O

Malonate-thiocyanate complex (NH₄)₃[UO₂(C₃H₂O₄)₂(NCS)] · 2H₂O is synthesized and studied by X-ray diffraction. The compound crystallizes in the monoclinic system: a = 13.9983(4) Å, b = 8.1947(2) Å, c = 16.4678(4) Å, β = 100.846(1)°, space group Cc, Z = 4, and R = 0.0158. The main structural units of the crystal are mononuclear [UO₂(C₃H₂O₄)₂(NCS)]^3? groups belonging to the AB ₂ ⁰¹ M ₁ crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ , B ⁰¹ = C₃H₂O ₄ ^2? , M ¹ = NCS^?). Discrete uranium-containing groups are connected by electrostatic interactions with ammonium ions and by hydrogen bonds. Some specific structural features of crystals containing [UO₂(L)₂(NCS)]^3? complexes, where L is the oxalate or malonate ion, are discussed.     

Synthesis and Structural Characterization of (2,4-Diamino-5-(3′,4′,5′-Trimethoxybenzyl)Pyrimidine Copper (II)) Complex

Abstract  The reaction of Cu(OOCCH₃)₂·H₂O with (2,4-diamino-5-(3′,4′,5′-trimethoxybenzyl) pyrimidine (trimethoprim) in ethanolic solution at 80 °C affords the title complex which has been characterized by elemental, IR, and NMR (¹H and ¹³C).The crystal structure has been determined by single crystal X-ray diffraction. Compound 1 (C₃₆H₄₈Cu₂N₈O₁₄) is triclinic, space group P-1 with a = 7.2676(4) ?, b = 11.6721(7) ?, c = 12.8279(8) ?, α = 95.839(1)°, β = 93.456(1)°, γ = 105.541(1)°, Z = 1. Two copper atoms are coordinated directly to each other as well as are held together by four bridging aceto groups. Each copper atom is also bonded opposite the Cu–Cu vector to a trimethoprim molecule through the N(1) atom of the pyrimidine ring. Trimethoprim acts as a monodentate ligand through the pyrimidine nitrogen N(1) atom. The complex was screened for the activity against several bacteria, showing more activity against bacteria as compared to trimethoprim. Graphical Abstract  To enhance the activity of trimethoprim, its derivative was prepared and there bacterial activity against several bacteria was analyzed.      

Synthesis and Structural Characterization of [2-(2-1H-Imidazoly)-1H-imidazolium nitrate] and [2-(2-1H-Imidazoly)-2H-imidazolium phthalyl glycinate] Based on the 2,2′-bi-1H-Imidazole Molecule

Abstract  

Two new compounds (H₃biim)(NO₃)(1) and (H₄biim)(phthgly)₂ (2) (H₂biim=biimidazole; Hphthgly=N-phthaloylglycine) have been synthesized and characterized by luminescence and single crystal X-ray diffraction study. Compound 1 crystallizes in the monoclinic space group C2/c, where a = 14.8078(15), b = 5.9233(6), c = 20.028(2) ?, β = 92.7910(10)°, V = 1754.6(3) ?³ and Z = 8. Compound 2 crystallizes in the monoclinic space group P2(1)/n, where a = 15.3775(14), b = 5.3200(6), c = 6.4689(18)?, β = 115.418(2)° V = 1216.9(2)?³ and Z = 4. In 1, the N–H groups of H₃biim⁺ and the oxygen atoms of NO₃ ⁻ are linked by hydrogen bonds leading to H₃biim⁺(N,N)–R₂²(10) and N–H···O interactions forming infinite 1D helical chains along the b-axis. Compound 2 consists of a planar diprotonated biimidazole moiety and two phthgly anions which connect to the dication by hydrogen bonds phthgly⁻(O,O)–R₂²(9).     

Synthesis and crystal structure of 2-trifluoromethyl-1-[(2′-1H-tetrazole-5-yl-biphenyl-4-yl) methyl]benzimidazole

The crystal structure of 2-trifluoromethyl-1-[(2'-1H-tetrazle-5-yl-biphenyl-4-yl) methyl]-benzimidazole and a methylene chloride have been determined by X-ray crystallography. The compound crystallizes in the monoclinic space group, P2 ₁/n with cell dimensions a = 10.931(2) Å, b = 12.31(3) Å, c = 17.901(4) Å, = 102.45(3)°, V = 2352.9(8) ų, D _calc = 1.427 g/cm³, Z = 4, = 0.324 mm^–1, and F(000) = 1032, and its structure was refined to R ₁ = 0.0663 and wR ₂ = 0.1668 for 1910 observed reflections I > 2(I)). Intermolecular hydrogen bonds were identified between the N and H atoms of intermolecular benzimidazole group and tetrazole group.     

Keto–enol tautomerism, conformations, and structure of 1-[N-(4-chlorophenyl)]aminomethylidene-2(1H)naphthalenone

1-[N-(4-chlorophenyl)]aminomethylidene-2(1H)naphthalenone (C₁₇H₁₂NOCl) (1) was synthesized and the crystal structure was determined. Compound 1 crystallizes in the monoclinic space group P2₁/n with a = 4.761(3) Å, b = 20.347(1) Å, c = 13.773(2) Å, = 92.89(3)°, V = 1332.4(3) ų, Z = 4, D _c = 1.404 g cm^–3, (Mo K) = 0.28 mm^–1, and R = 0.036 for 2680 reflections [I > 2(I)]. Molecule 1 is not planar, and the dihedral angle between the naphthaldeyde plane A [C1–C11, 01] and the 4-chloroaniline plane B [C12–C17, C11, N1] is 20.1(3)°. An intramolecular hydrogen bond occurs between the hydroxyl oxygen and imine nitrogen atoms [2.528(3) Å]. IR, ¹H NMR, and UV measurements and AM1 semiempirical quantum mechanical calculations support the keto form found in the X-ray structure.     

Synthesis and crystal structure of catena-μ-chloro-bis(acetonitrile)copper(I) [(H3CCN)2CuCl]∞

The new crystalline compound of catena--chloro-bis(acetonitrile)copper(I) [(H₃CCN)₂ CuCl] has been synthesized and structurally characterized by X-ray crystallography. The compound is an infinite polymeric chain in which chlorides bridge the coppers. Copper exhibits tetrahedral coordination geometry with two acetonitrile molecules acting as coordinating ligands. The compound crystallizes in the orthorhombic Pbcm space group with a = 12.585(3) Å, b = 7.496(2) Å, and c = 7.275(2) Å.     

Synthesis, Characterization, and Crystal Structures of 3-bromo-N′-(2-methoxybenzylidene)benzohydrazide and N′-(2-methoxybenzylidene)-3,4-methylenedioxybenzohydrazide

Abstract  

Two new hydrazone compounds, 3-bromo-N′-(2-methoxybenzylidene)benzohydrazide (1) and N′-(2-methoxybenzylidene)-3,4-methylenedioxybenzohydrazide (2), have been synthesized and characterized by elemental analysis, IR, and single crystal X-ray diffractions. Compound (1) crystallizes in the triclinic space group P1 with unit cell dimensions a = 8.4088(5) ?, b = 8.5398(5) ?, c = 10.6572(6) ?, α = 90.356(3)°, β = 102.868(3)°, γ = 97.987(3)°, V = 738.28(7) Ǻ³, Z = 2, R ₁ = 0.0406, and wR ₂ = 0.0804. Compound (2) crystallizes in the tetragonal space group P4₁ with unit cell dimensions a = b = 9.792(4) ?, c = 15.788(6) ?, V = 1513.8(10) Ǻ³, Z = 4, R ₁ = 0.0415, and wR ₂ = 0.0818. The molecules of both compounds display E configurations with respect to the C=N double bonds. In the crystal structure of (1), molecules are linked through N–H···O hydrogen bonds, forming chains running along the b axis. In the crystal structure of (2), molecules are linked through N–H···O hydrogen bonds, forming chains running along the c axis.     

Crystal Structure of 3′-(4-Methoxyphenyl)-2-Phenyl-4′-(4-Ethoxyphenyl)-1,2-Dihydro-4H,4′H-Spiro [Isoquinoline-3,5′-Isoxazol]-4-One

The title compound, 3′-(4-methoxyphenyl)-2-phenyl-4′-(4-ethoxyphenyl)-1,2-dihydro-4H,4′H-spiro[isoquinoline-3,5′-isoxazol]-4-one was synthesized from the reaction of dipolarophile with p-methoxybenzadoxime in the presence of sodium hypochlorite in chloroform solution. The structure of the synthesized compound was determined by IR, ¹H NMR, mass spectroscopic data, ¹³C NMR spectroscopy, elemental analysis and X-ray crystallography. The structure was solved in monoclinic, space group C2/c with a = 21.941 (4), b = 17.233 (3), c = 15.404 (3) Å, β = 122.193 (2), V = 4928.9 (16) Å³, Z = 8 and with R_int = 0.154. The geometry of the title compound showed that the piperidine ring adopts a half-chair conformation. In the crystal structure, molecules are linked by C–H···O and C–H···N contacts. Weak C–H···π interactions plays an important role in stabilizing the supramolecular structure.     

Reinvestigation of the reaction of [Ru3(CO)12] with 2-mercaptobenzothiazole: X-ray structure of [(μ-H)2Ru3 (μ-η2-C7H4NS2)(μ3-η2-C7H4NS2)(CO)7]

Treatment of Ru₃(CO)₁₂ with 2-mercaptobenzothiazole at 68°C gave the known compound [(-H)Ru₃(₃-²-C₇H₄NS₂)(CO)₉] 1 and the new compound [(-H)₂Ru₃(-²-C ₇H₄NS₂) (₃-²-C₇H₄NS₂)(CO)₇] 2 in 15 and 10% yields respectively. Compound 2 has been characterized by elemental analysis, infrared, ¹H NMR and mass spectroscopic data together with single crystal X-ray crystallography. It crystallizes in the monoclinic space group C2/c with a = 31.662(6), b = 14.577(3), c = 11.602(2) Å, = 104.15(3)°, Z = 8, and V = 5192.4(2) ų. The compound consists of a Ru₃ triangle with three different Ru-Ru bond lengths [2.75264, 2.79084, 2.97604 Å] and the two 2-mercaptobenzothiazole ligands are differently attached to the metal atoms. Compound 2 is also obtained by the reaction of 1 with excess 2-mercaptobenzothiazole at 68°C.     

Synthesis and structure of (H2O·HBF4)2(18-crown-6)

The title compound has been prepared by the addition of fluoroboric acid to 18-crown-6 in toluene. The compound crystallizes in the triclinic space group P¯1 witha=7.341(2),b=8.364(2),c=10.631(3)Å,=71.48(2),=67.91(2), =67.94(2)°, andD _c =1.44 g cm^–3 forZ=1. The final conventionalR value was 0.079 based on 1575 observed reflections. The molecule resides on a center of inversion. The (H₂O·HBF₄) moieties are best viewed as fluoroboric acid monohydrate molecules hydrogen bonded to the crown ether, one above and one below the plane of the crown. The FO(water) hydrogen bond separation is 2.474(5)Å, and the O(crown)O(water) separations are 2.834(5) and 2.841(6) Å. The oxygen atoms of the crown ether are planar to 0.23 Å.     

三维孔道结构钒磷酸盐[H3N(CH2)3NH3]2[H3N(CH2)3NH2][H2N(CH2)3NH2]-[V(H2O)2(VO)8(OH)4(PO4)4(HPO4)4]·4H2O的水热合成和结构表征

以1,3-丙二胺为模板,水热合成了三维孔道结构钒磷酸盐[H3N(CH2)3NH3]2[H3N(CH2)3NH2][H2N(CH2)3NH2][V(H2O)2(VO)8(OH)4(PO4)4(HPO4)4]·4H2O(DAP-V9P8).用单晶X射线衍射、红外光谱和热重法对该化合物的晶体结构进行了表征.DAP-V9P8的无机骨架由[VO5]、[VO6]、[PO4]和[HPO4]通过共顶点连接而成.孔道中充填的丙二胺分子随所处结晶学位置不同,有三种完全不同的分子构象.其中,位于//b轴直径达1.82nm椭圆形孔道中心的丙二胺分子碳链呈独特的直线状分布.晶体学参数:a=1.4820(9)nm,b=1.0255(4)nm,c=1.8181(9)nm,β=90.391(8)°;P21/n(No.14);R1=0.0772,wR2=0.2004(I＞(2σI)).与等结构的其它化合物进行了系统的结构比较.     

Structural,theoretical, and third-order nonlinear optical investigations of N’-[(E)-(4-bromophenyl)(phenyl)methylidene]–4-methylbenzenesulfonohydrazide

Single crystals of N’-[(E)-(4-bromophenyl) (phenyl) methylidene]–4-methylbenzenesulfonohydrazide (4BBTH), having potential applications in nonlinear electro optic field. The structure is elucidated by single crystal X-ray diffraction analysis. The functional groups are identified by FT-IR analysis. The band gap energy is estimated using diffuse reflectance data by the application of Kubelka–Munk algorithm. Third-order nonlinear optical properties of the grown crystal were derived by employing a single beam Z-scan technique. Theoretical calculations were performed using density functional theory (DFT) method. Estimated large first-order molecular hyperpolarizality of 9.79 times of urea, suggests a charge transfer atmosphere facilitating micro level nonlinearity.GRAPHICAL ABSTRACT     

Synthesis, crystal structure, and thermal analyses of triaqua-(1,10-phenanthroline-N,N′) succinatomanganese(II) dihydrate, [Mn(H2O)3(phen)(C4H4O4)]·2H2O

[Mn(H₂O)₃(phen)(C₄H₄O₄)]·2H₂O was obtained by reaction of freshly prepared MnCO₃, phen and succinic acid in CH₃OH/H₂O (1:1 v/v), and its crystal structure has been determined by single crystal X-ray diffraction methods. The title mixed ligand complex crystallizes in the triclinic space group with cell dimensions a = 7.590(1) Å, b = 9.324(1) Å, c = 13.917(1) Å, = 85.64(1)°, = 74.56(1)°, = 77.10(1)°, and D _calc = 1.584 g/cm³ for Z = 2. The crystal structure consists of the [Mn(H₂O)₃(phen)(C₄H₄O₄)] complex molecules and lattice H₂O molecules. The Mn atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of three H₂O molecules and one succinato ligand with d(Mn—N) = 2.271 and 2.299 Å, and d(Mn—O) = 2.133–2.239 Å. Through intermolecular hydrogen bondings, the complex molecules are interlinked to form 2D layers, which are assembled by – stacking interactions into 3D framework with tunnels occupied by the lattice H₂O molecules. Thermal analyses showed that the title compound decomposes in two steps over the range 25–600°C upon heating in flowing Ar.