Synthesis, Spectroscopic Characterization and Crystal Structure of a New Acetyl phosphorylamidate P(O)[NHC(O)C6H4(4-NO2)][N(CH(CH3)2)(CH2C6H5)]2

Abstract  

A new acetyl phosphorylamidate P(O)[NHC(O)C₆H₄(4-NO₂)][N(CH(CH₃)₂)(CH₂C₆H₅)]₂ has been synthesized and characterized by elemental analysis, ¹H, ¹³C and ³¹P NMR, IR and single crystal X-ray diffraction. Single crystal X-ray analysis shows that it belongs to triclinic system, space group P[`1] P\bar{1} , with a = 10.5868(16) Å, b = 11.8058(18) Å, c = 12.4364(19) Å, α = 65.410(3)°, β = 67.492(4)°, γ = 85.879(3)°, V = 1,298.6(3) Å³, and Z = 2. The intermolecular PO···HN hydrogen bond makes H-bonded dimer of molecule with Ci symmetry. In the crystal network, the dimers are aggregated in the chain arrays through π-stacking between p-NO₂–C₆H₄–C(O)–NH– moieties. Moreover, weak C–H···O and C–H···π interactions exist in the crystal network.     

Synthesis and Crystal Structure Analysis of Methyl 2-Hydroxyimino-3-phenyl-propionate

Abstract  

As precursors of α-amino acids, methyl 2-hydroxyimino-3-phenyl-propionate (F.W. 193.20) was synthesized, characterized by ¹H NMR, IR, element analysis and confirmed by X-ray crystal structure analysis. This compound crystallizes in monoclinic class under the space group P2₁/c with cell parameters, a = 8.6435(17) Å, b = 5.4957(11) Å, c = 21.146(4) Å; β = 97.12(3)°, and Z = 4. The structure exhibits inter-molecular hydrogen bonds of the type O–H···N, O–H···O, C–H···O.     

Synthesis,Crystal Structure and Optical Properties of a Three-Dimensional Supramolecule Assembled by a Dinuclear Neodymium Cluster

Abstract  

The reaction of isonicotinic acid (IN), sodium hydroxide, 1,10-phenanthroline (phen) and neodymium nitrate leads to the formation of a novel complex [Nd(phen)(IN)₂(NO₃)(H₂O)₂]₂ 1, which has been characterized by single crystal X-ray diffraction analysis: monoclinic, space group C2/c, with a = 24.93(2) Å, b = 9.452(3) Å, c = 21.406(5) Å, β = 97.87(2)°, and Z = 4. Complex 1 consists of a centrosymmetric dinclear molecule, and neodymium atoms are bridged by two carboxyl groups of two IN ligands. The dinuclear clusters of 1 are connected each other into a three-dimensional (3D) supramolecular framework, which is stabilized by O–H···O, O–H···N hydrogen bonds as well as π–π stacking interactions. Its electronic absorption and luminescence properties have also been investigated.     

Structures of Three New (Phenylsulfonyl)Indole Derivatives

Abstract  

Three new 1-(phenylsulfonyl)indole derivatives, 3-acetyl-2-ethyl-1-(phenylsulfonyl)indole, (I), 2-benzyl-1-(phenylsulfonyl)indole, (II), and 3-trimethylsilylethynyl-1-(phenylsulfonyl)indole, (III), have been synthesized and their crystal structures determined by single crystal X-ray crystallography. (I), C₁₈H₁₇NO₃S, is triclinic with space group P-1 and cell constants: a = 8.6129(2) Å, b = 8.8366(2) Å, c = 11.0108(2) Å, α = 72.7920(1)°, β = 75.0120(1)°, γ = 77.2550(1)°, V = 763.79(3) ų and Z = 2. (II), C₂₁H₁₇NO₂S, is monoclinic with space group P21/n and cell constants: a = 10.8355(18) Å, b = 10.6987(19) Å, c = 14.472(3) Å, β = 75.0120(1), V = 1675.2(5) ų and Z = 4. (III), C₁₉H₁₉NO₂SSi, is monoclinic with, space group P21/c and cell constants: a = 12.9596(1) Å, b = 10.543(3) Å, c = 13.543(2) Å, β = 93.58°, V = 1846.8(6)ų and Z = 4. All three have the same (phenylsulfonyl)indole skeleton with different ligands attached to the 2- and 3-sites of the indole ring. The angle between the mean planes of the indole and benzyl groups is 76.9(6)° (I), 82.9(3)° (II), 89.6(2)° (III) and between the sulfonyl group with the indole and benzyl rings is 61.2(9)° (I), 59.0((5)° (II), 51.5(6)°, 42.5(8)° (III) and 51.5(6)°(I), 44.3(8)° (II), 47.2(8)° (III), respectively. In addition to the ligand substitutions, weak intermolecular C–H···O hydrogen bond interactions and π stacking interactions between the π orbitals of nearby indole and phenyl rings influence these twist angles. Comparison to a MOPAC AM1 computational calculation supports these observations.     

Synthesis,Crystal Structure and Characterizations of New 3,4,7,8-Tetrachloro-1,10-Phenanthroline Zn(II) Complex

Abstract  

A novel 3,4,7,8-tetrachloro-1,10-phenanthroline (Cl₄phen) Zn(II) complex has been synthesized. The complex, [Zn(Cl₄phen)₂(H₂O)₂](NO₃)₂·CH₃CH₂OH (1), has been identified and characterized by single crystal X-ray diffraction, elemental analysis, FT-IR, thermogravimetric analysis and photoluminescence studies. Single crystal X-ray diffraction analysis reveals that complex (1) belongs to the monoclinic system, space group P2(1)/c, a = 10.061(2) Å, b = 18.924(4) Å, c = 18.189(4) Å, β = 100.94(3)°, and Z = 4. Complex (1) consists of cationic species [Zn(Cl₄phen)₂(H₂O)₂]²⁺, NO₃ ⁻ and CH₃CH₂OH. The zinc atom displays a distorted cis-N₄O₂ octahedral geometry. Via extended Zn–O–H···O–N–O···H–O–Zn bridge, every mononuclear unit is linked with other ones to form one-dimensional (1D) infinite chain of hydrogen bond system. Three-dimensional (3D) polymeric network arrangement was built via weak C–H···O and π-stacking interactions between Cl₄phen moieties. A solvent-dependency effect of complex (1) was observed in spectroscopic properties.     

Synthesis and Structural Characterization of Bis[(cyclohexylamino)pent-2-en-4-onato]-Chromium(II)

Abstract  Addition of one equivalent of CrI₂ to two equivalents of lithium cyclohexylamino-pent-2-en-4-onate results in bis[(cyclohexylamino)pent-2-en-4-onato]-chromium(II). Crystallization in diethylether reaction solvent forms the hemi-etherate A with the asymmetric unit showing two target compounds and one molecule of cocrystallized diethylether in the P-1 space group with crystal cell parameters a = 12.931(4) Å, b = 13.207(4) Å, c = 16.104(5) Å, α = 66.559(5)°, β = 77.670(5)°, γ = 81.562(5)°, V = 2,459.1(14) Å³ and Z = 4. Drying A in vacuo and recrystallization in pentane yields a nonsolvated crystalline phase B with an asymmetric unit displaying only one molecule of the target compound in the P2₁/c space group with crystal cell parameters a = 14.290(7) Å, b = 14.082(7) Å, c = 11.246(6) Å, β = 94.807(8)°, V = 2,255.1(19) Å³ and Z = 4. Graphical Abstract  A Cr(II) complex supported by two β-enaminoketiminato ligands, bis[(cyclohexylamino)pent-2-en-4-onato]-chromium(II), has been synthesized and has been structurally characterized in two different crystal phases.      

A New 3-D Gd(III) Coordination Polymer Constructed with Mixed Aromatic Acid: Synthesis,Structural Characterization and Magnetic Characterization

Abstract  

Using pyridine-2,5-dicarboxylic acid (2,5-pdcH₂) and Gd₂O₃, a new three-dimensional (3D) polymeric complex, [Gd(2,5-pdc)(nic)·H₂O] _n (1) was synthesized under hydrothermal conditions, in which nic (nicotinate; also named as pyridine-2-carboxylic acid) might have been formed from the 2,5-pdc ligands through the C–C bond cleavage and release of CO₂ molecules. The complex crystallizes in monoclinic system, space group P2₁/c with unit cell parameters a = 9.221(9) Å, b = 14.179(14) Å, c = 10.516(10) Å, β = 95.658(14)°, V = 1,368(2) Å³ and Z = 2. 2,5-pdc ligands bridge gadolinium centers to form the three-dimensional framework featuring hexagonal channels along the axis a which are occupied by bridging nic anions and mono-coordinated water molecules. Magnetic properties have been investigated in the range of 2–300 K reveal that t there is very weak antiferromagnetic exchange between the Gd(III) ions (J = −0.017 cm⁻¹).     

Synthesis and Crystal Structure of a Depside Derivative 2-(2-Methoxy-2-oxoethyl)phenyl 2-(3,4-Dimethoxyphenyl)acetate

Abstract  

A depside derivative, 2-(2-methoxy-2-oxoethyl)phenyl 2-(3,4-dimethoxyphenyl)acetate (3), was synthesized through a facile approach in high yields. Its structure was confirmed by ¹H NMR, ¹³C NMR, ESI mass spectra, elemental analyses and X-ray single crystal diffraction study. Crystal structure analysis revealed that compound 3 crystallized in the monoclinic, space group P2₁/c with the following unit cell parameters: a = 10.173(2) Å, b = 10.459(2) Å, c = 16.516(3) Å, α = 90°, β = 102.30(3)°, γ = 90°, V = 1717.0(6) Å³, Z = 4.     

Synthesis,Characterization and Crystal Structure Determination of a Hepta-coordinated Cadmium(II) Complex with Thiocyanato-bridges

Abstract  A new cadmium(II) complex [(C₂₈H₂₄N₆)Cd(SCN)₂]₂(CH₃OH)₂ (1) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single crystal X-ray diffraction analysis. The crystallographic data for compound 1: triclinic P1ˉ, a = 9.630(2) Å, b = 11.123(3) Å, c = 15.396(4) Å, α = 106.93(1)°, β = 91.60(1)°, γ = 99.99(1)°, V = 1,548.5(6) Å³, Z = 1, Dc = 1.512 mg/m³, F(000) = 716, R ₁ = 0.0332, wR ₂ = 0.0907. The molecule contains a symmetrical dinuclear unit in which two Cd(II) ions are double bridged by two di-μ-1,3-SCN⁻ anoins with a cadmium–cadmium separation of 6.48 Å. Each Cd(II) ion is seven-coordinated with six nitrogen atoms and a sulfur atom to form a monocapped trigonal prism coordination geometry. In addition, the molecule is further connected by multiform intermolecular C–H···π, π···π interactions and hydrogen bonds to form a three-dimensional supramolecular structure. Graphical Abstract  A hepta-coordinated Cd(II) complex which exhibits a distorted a monocapped trigonal prism coordination geometry has been achieved by using bisbidentate Schiff-base ligand and thiocyanate anion.      

Synthesis and Crystal Structure of 3-Methyl-4-phenyl-5-(2-pyridyl)-1,2,4-triazole

Abstract  

The title compound, 3-methyl-4-phenyl-5-(2-pyridyl)-1,2,4-triazole was synthesized by reaction of diphenylphosphazoanilide with N-acetyl-N′-(2-pyridoyl)hydrazine. Crystals suitable for X-ray analysis were obtained from a mixed solution of water and ethanol in a one-to-one volume ratio. The crystal is orthorhombic, space group P2₁2₁2₁ with crystallographic parameters: a = 19.414(4) Å, b = 17.172(3) Å, c = 7.4850(15) Å, β = 90.00°, μ = 0.079 mm⁻¹, V = 2495.3(8) Å³, Z = 8, Dc = 1.258 g/cm³, F(000) = 992, T = 295(2) K. The X-ray results showed that in the crystal structure of the title compound, the 1,2,4-triazole, pyridine and benzene rings are not coplanar.     

N,N′-Dihydrogenpiperazonium dichloridobis(dimethylglyoximato-k2N,N′)cobaltate(III) Dihydrate

Abstract  

The title complex: C₄H₁₂N₂[Co(C₄H₇N₂O₂)₂Cl₂]₂·2H₂O, viz., PpH₂[Co(dmgH)₂Cl₂]₂·2H₂O, where, dmgH⁻ = dimethylglyoximate and Pp = piperazine was synthesized and analyzed by single crystal XRD studies. The complex was grown as brown crystals by the slow evaporation method in ethanol. The complex crystallizes as triclinic with the space group p[`1] p\overline{1} and unit cell parameters a = 8.4521 (10) Å, b = 10.0999 (11) Å, c = 10.8952(13) Å; α = 94.066(6)°, β = 106.047(6)° and γ = 100.901(6)°. There are two complex molecules present in the unit cell. The short intra molecular O–H···O hydrogen bonds link the glyoximate moieties in the crystal.     

Rapid Eco-Friendly Synthesis and Structure of 3-Hydroxy-3-nitromethyl-1,3-dihydro-indol-2-one

Abstract  

3-Hydroxy-3-nitromethyl-1,3-dihydro-indol-2-one was synthesized from isatin by Henry reaction using an eco-friendly method and characterized by NMR and MS. The crystal structure was determined from single-crystal X-ray diffraction data. It crystallizes in the orthorhombic space group, Pbca, with unit cell dimensions a = 10.515 (2) Å, b = 7.3736 (14) Å, and c = 23.261 (4) Å. The two rings are coplanar and the angle between hydroxyl group and nitromethyl group is 109.07(9)°. In the crystal structure, intermolecular N–H···O and O–H···O hydrogen bonds are responsible for the formation of a 3-dimensional network. No intramolecular hydrogen bond exists.     

Synthesis,Crystal Structures and Physicochemical Properties of Poly[bis(<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>-Dimethylformamide)tetra(thiocyanato)metal(II) Mercury(II)] (Metal = Cadmium and Manganese)

Abstract  

Two novel single crystals, poly[bis(N,N-dimethylformamide)tetra(thiocyanato)metal(II)mercury(II)] (metal = cadmium and manganese, abbreviated as DTCM and DTMM, respectively) were prepared. The characterizations of DTCM and DTMM were performed by elemental analyses, infrared, X-ray single crystal diffraction. The two title complexes crystallized in the same monoclinic crystallographic system and P2₁/n space group with unit cell parameters: a = 9.2515(2) Å, b = 14.1670(3) Å, c = 16.5898(3) Å, β = 93.0320(10)°, z = 4, D _x  = 2.115 g/cm³ for DTCM, and a = 9.24580(10) Å, b = 14.1110(2) Å, c = 16.4937(2) Å, β = 92.9120(10)°, z = 4, D _x  = 1.960 g/cm³ for DTMM, respectively. The two structures are isostructural. The thermal decomposition processes of the two crystals were investigated by means of thermogravimetric analysis and differential thermal analysis measurements in air.     

Structure of Triammonium <Emphasis Type="Italic">fac</Emphasis>-Trichloridotrioxidorhenate(VII) Chloride with <Emphasis Type="Italic">C</Emphasis><Subscript>3<Emphasis Type="Italic">v</Emphasis></Subscript> Crystallographic Symmetry of the Complex Anion

Abstract  

The unstable crystals of triammonium fac-trichloridotrioxidorhenate(VII) chloride have been obtained from ammonium rhenate(VII) solution in concentrated hydrochloric acid. The crystal structure consists of fac-trichloridotrioxidorhenate(VII) anions, chloride anions and ammonium cations. Each fac-trichloridotrioxidorhenate(VII) anion and each chloride anion lies in special position of 3m site symmetry (cell parameters: a = 9.026(3) Å; c = 7.690(4) Å; space group: P6₃ mc). The ammonium cation lies in special position of m site symmetry. The following anion geometrical parameters of the fac-trichloridotrioxidorhenate(VII) anion have been obtained: Re–O bond length of 1.720(2) Å, Re–Cl bond length of 2.5428(9) Å, the bond angles: O–Re–O of 103.5(1)° and Cl–Re–Cl of 79.8(1)°.     

Bis[(2,3,4-Trimethoxy-Benzylidenepropylideneamino)Phenyl]Ether: Synthesis,Characterization and Crystal Structure

Abstract  

New Schiff base compound bis[(2,3,4-trimethoxy-benzylidenepropylideneamino)phenyl]-ether (1) was synthesized and characterized by elemental analyses (CHN), FT-IR and ¹H-NMR spectroscopy and single-crystal X-ray diffraction. The title compound 1 crystallizes in triclinic system, space group P-1, with a = 6.8255(4) Å, b = 10.4346(4) Å, c = 19.4166(8) Å, α = 86.588(3)°, β = 85.019(4)°, γ = 89.042(4)°, V = 1375.12(11) Å³ and Z = 2. It displays a trans configuration about the C=N double bonds.     

Synthesis, Crystal Structure of catena-poly [[4,4′-bipyridine-N,N′-bis[(triphenylphosphine)-copper(I)]-pyridine-2-carbaldehyde azine-N,N′:N″,N′″] bis(tetrafluoroboride)]

Abstract  

The title complex [Cu₂(C₁₀H₈N₂)(C₁₂H₁₀N₄)(C₁₈H₁₅)₂(BF₄)₂] _n has been synthesized and characterized by single crystal X-ray analysis. The compound crystallizes in the monoclinic space group P2₁/c with a = 10.450(4) Å, b = 14.027(5) Å, c = 18.950(6) Å, β = 100.459(5)°, V = 2,731.7(16) ų. In the title complex, the cation forms a linear chain, which is bridged by 4,4′-bipyridine and pyridine-2-carbaldehyde azine. The crystallographic asymmetry unit could be expanded polymeric structure using symmetry code: x, 1 + y, z; 1 − x, −y, 1 − z. The Cu(I) atom is coordinated by one P atom of PPh₃ ligand, two N atoms of pyridine-2-carbaldehyde azine ligand and one N atom of 4,4′-bipyridine ligand. There is a crystallographic centre of symmetry at the mid-point of the C–C bond between two pyridine rings of 4,4′-bipyridine.     

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.     

A Sodium Supported Borate Ester: Synthesis,Spectral Characterization and Crystal Structure of dimeric Sodium Organoborate Complex [Na(py)][B(hyncaH<Subscript>−2</Subscript>)<Subscript>2</Subscript>]<Subscript>2</Subscript>

Abstract  A dimeric sodium supported borate complex, [Na(py)][B(hyncaH₋₂)₂]₂ (1) (py = pyridine, hynca = 1-hydroxynaphthalene-2-carboxylic acid), has been synthesised by the reaction of NaBH₄ with two equivalents of hynca in anhydrous THF and following crystallization from py/H₂O solution afforded borate ester derivative. The complex has been fully characterized by FT-IR in the solid state and by NMR (¹H and ¹³C) spectroscopy and electrospray ionization mass spectrometry in solution. The molecular structure of the title compound was determined by single crystal X-ray diffraction. Structure analysis of complex 1 confirmed the presence of an anionic complex [B(hyncaH₋₂)₂]⁻ in which boron atom is coordinated simultaneously by two hynca ligands utilising both alkoxide and carboxylate groups for bonding. The Na atom is six- coordinate to five O atoms of hydroxy carboxylic acid and one pyridine N atom. Crystal data: crystal system, monoclinic, a = 10.971(3) Å, b = 6.839(3) Å, c = 30.545(5) Å, β = 92.20(2)°, space group P2₁/c (#14), V = 2,290(1) Å³, Z = 4. Index Abstract  There are limited examples of alkali metal supported borate ester complexes.      

Synthesis,Crystal Structure and Hydrogen-Bonding Patterns in (RS)-1-Carbamoyl Pyrrolidine-2-Carboxylic Acid

Abstract  

The title compound, N-carbamoyl-dl-proline, C₆H₁₀N₂O₃, crystallizes in the triclinic P-1 space group with unit cell parameters a = 7.610 (4) Å, b = 9.259 (5) Å, c = 11.749 (7) Å, α = 110.294 (11)°, β = 101.304 (13)°, γ = 91.391 (16)°, with two crystallographically independent molecules in the asymmetric unit. The ureido and carboxyl groups are equatorial and axial to the pyrrolidine rings, respectively. The pyrrolidine rings adopt envelope and twisted conformations in the residue A and B, respectively. The molecules are joined by N–H···O and O–H···O hydrogen bonds into cyclic structures with graph set R ₂²(8), forming infinite chains parallel to the cb plane with graph set C ₂²(14), that are further connected via N–H···O hydrogen bonds into a three-dimensional network.