Crystal Structure and Characterization of [Ni(RPOEt)<Subscript>2</Subscript>(C<Subscript>2</Subscript>H<Subscript>5</Subscript>OH)<Subscript>2</Subscript>](ClO<Subscript>4</Subscript>)<Subscript>2</Subscript> [RPOEt = bis{(diphenylphosphinyl)methyl}ethyl phosphinate]

Abstract  

The compound [Ni(RPOEt)₂(C₂H₅OH)₂](ClO₄)₂ (1) [RPOEt = bis{(diphenylphosphinyl)methyl}ethyl phosphinate] has been prepared in the form of single crystals and characterized by elemental and thermal analyses, IR spectroscopy and by a single crystal X-ray diffraction study. The complex crystallizes in the triclinic P[`1] P\bar{1} space group with a = 9.8773(5), b = 13.741(1), c = 14.287(1) ?, α = 64.313(9), β = 70.280(5), γ = 89.973(7)o, V = 1620.5(2) ?³, and Z = 1. The nickel(II) atom in 1, situated at the centre of symmetry, is coordinated by four oxygen atoms from two RPOEt ligands and two oxygen atoms from two ethanol molecules in a slightly distorted octahedral environment. The third phosphoryl-oxygen atom from the phosphinate ligand is hydrogen bonded to the oxygen atom of the ethanol molecule coordinated to nickel(II). The complex [Ni(RPOEt)₂(C₂H₅OH)₂]²⁺ cations are linked by the C–H···O hydrogen bonds into one-dimensional chains and by the composite π···π and C–H···π phenyl interactions into a final three-dimensional structure.     

Structural and Spectroscopic Study of Cu(II) Pyridine-2,6-dicarboxylate Complex with 2-Ethylimidazole

Abstract  

A mononuclear copper(II) complex, [Cu(pydca)(2-Etlm)(H₂O)] (1) (H₂pydca = pyridine-2,6-dicarboxylic acid, 2-Etlm = 2-ethylimidazole), has been synthesized and characterized by elemental analyses, IR, UV–Vis, TG-DTA and single crystal X-ray diffraction. The complex 1 is in the orthorhombic crystal system, space group Pbca and Z = 8. The structural analysis indicated that Cu(II) center is five coordinated in a slightly distorted square pyramidal geometry by one N and two O atoms from a 2,6-pyridine dicarboxylate dianion, one N atom from a 2-ethylimidazole ligand, and one O atom from a aqua molecule. This mononuclear motif of 1 is further assembled to 3D supramolecular framework through strong O–H···O and N–H···O hydrogen bonding interactions.     

5-Pyridine 4-yl-3H-(1,3,4) Oxadiazole-2 Thione Hydrochloride Monohydrate, (I), and 4 [5-Ethylsulfanyl)-(1,3,4) Thiadiazole-2-yl]-Pyridinium Perchlorate, (II)

Abstract  

The title compounds C₇H₈ClN₃O₂S, (I), and C₉H₁₀ClN₃O₄S_2, (II), both crystallize in monoclinic space group P2₁ /c with unit cell parameters (I) a = 7.9402(7), b = 10.6312(9), c = 11.7626(10), ?, β = 99.271(5)°, Z = 4 and (II) a = 5.1439(2), b = 9.0636(4), c = 27.1814 (7), ?, β = 95.116(2)°, Z = 4. In (I) the molecule consists of a 5-pyridine-4-yl group bonded to the carbon atom at the 5 position of (1, 3, 4) oxadiazole-2 thione hydrochloride monohydrate. The angle between the mean planes of the oxadiazole and pyridine rings is 9.6(6)°. Crystal packing in (I) is stabilized by strong N–H···O hydrogen bonds in concert with a solvent water molecule and weak O–H···Cl, O–H···S, N–H···Cl intermolecular interactions. The crystal structure of compound (II) consists of 4 [5-ethylsulfanyl)-(1, 3, 4) thiadiazole-2-yl]-pyridinium perchlorate, (C₉H₁₀N₃S₂)⁺(ClO₄)⁻, cation–anion pairs, containing strong intermolecular N–H···O hydrogen bonds and weak C–H···O and N–H···O intermolecular interactions operating between the ionic species that form a cooperative hydrogen-bonded, infinite chain O–H···O–H···O–H network which generates a sheet motif structure in the unit cell. It is also supported by weak intermolecular Cg···Cg π–π and Cl–O···Cg π-ring interactions which gives additional support to molecular packing stability in the unit cell. Geometry optimized MOPAC AM1 computational calculations on each compound provides support to the structural features in their respective crystal structures.     

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,Structural and Thermal Studies of a New Nickel Complex Containing 2-Aminopyrimidine and Thiocyanate Mixed Ligands with a Three-Dimensional Network Structure

Abstract  

A new nickel(II) complex formulated as, trans-[Ni(amp)₂(SCN)₂(H₂O)₂]·2H₂O (1), (amp = 2-aminopyrimidine) has been synthesized and characterized by elemental analysis, IR spectroscopy, its molecular and crystal structures were determined by X-ray crystal structure analysis and its thermal stability by TGA/DTA methods. 1 is a neutral complex and the central atom sits on an inversion center and is coordinated by two endocyclic nitrogen atoms of two 2-aminopyrimidine heterocycles, two oxygen atoms of two water molecules and two nitrogen atoms of SCN⁻ ions. 2-aminopyrimidine molecules, thiocyanate ions and water molecules are in trans position. Thermal methods confirm two co-crystallized water molecules in 1. π–π stacking interactions and extensive O–H···O, O–H···N, O–H···S and N–H···N hydrogen bonds contribute to the formation of a three-dimensional supramolecular structure. Crystal data for complex at 120 K: triclinic, space group P-1, a = 7.2026(14), b = 7.8332(15), c = 9.0270(17) ?, α = 67.694(3), β = 72.732(4), γ = 77.012(4), Z = 1, R ₁ = 0.0323.     

Synthesis,Characterziation and SOD Activity of Manganese(II) Complexes with Aza-Macrocyclic Ligand

Abstract  

Two manganese(II) complexes, [Mn₂(L)(H₂O)₄]Cl₂·6H₂O(1) and [Mn₂L(NCS)₂(H₂O)₂]·3H₂O(2) (L is 1,2,4-triazolato)-4,12,17,25-tetramethyl-1,2,5,8,11,14,15,18,21,24-decaza-4,11,17,24-cyclohexaeicosatetraene) have been prepared by template synthesis method. They are characterized by elemental analysis and IR. Single-crystal X-ray analysis reveals that complex (1) crystallizes in space group P 2₁/c with a = 8.710(3), b = 14.720(5), c = 14.301(5) ?, α = 90, β = 105.801(14), γ = 90°. The complex [Mn₂(L)(H₂O)₄]Cl₂·6H₂O consists of two manganese(II) macrocyclic complexes in which two Mn(II) centers are linked by two triazolate units of the macrocyclic framework. Each manganese(II) ion is coordinated by five nitrogen atoms from the macrocycle and two oxygen atoms of the coordinated water. The manganese(II) center is in an approximately pentagonal-bipyramidal environment. The SOD activities of both complexes have also been investigated.     

Synthesis,Crystal Structure and Luminescent Properties of One Coordination Polymer of Copper(II) Achieved from Pyridine-3,5-dicarboxylate

Abstract  

A new Cu(II) coordination polymer [Cu(3,5-pdc)(H₂O)₄·H₂O] _n 1 (3,5-pdc=3,5-pyridinedicarboxylic acid) has been synthesized by hydrothermal method and characterized by IR, elemental analysis, TG technique and X-ray crystallography. The crystallographic data for the compound 1: monoclinic P2₁/n, a = 11.361(5) ?, b = 7.095(3) ?, c = 14.575(6) ?, β = 107.630(4)°, V = 1,119.7(8) ?³, Z = 4, Dc = 1.891 Mg/m³, F(000) = 652, R ₁ = 0.0374, wR ₂ = 0.1083. Cu(II) atom has an distorted octahedral environment with N₂O₄ donor set of Cu(1) and O₆ donor set of Cu(2), respectively. Each ligand is bound to two Cu(II) ions and each copper atom is coordinated by two ligands thereby generating a 1D zigzag chain. The 1D chain was interacted each other feathering three-dimensional supramolecular network through π···π interactions and multiform intermolecular hydrogen bonds. The luminescent properties of the title complex in the solid state were investigated.     

A Neutral Four-Coordinate Mononuclear Cobalt(II) Complex with Biphenyl Appended N-Bidendate Ligand: Synthesis, Structure and Spectral Properties

Abstract  

A mononuclear cobalt(II) complex [Co(BP)(Cl₂)], 1 with a new N,N-bidentate ligand, BP ([N,N-(1,1′-biphenyl-2,2′-dimethylene)]-2-aminomethyl) pyridine) was synthesized and characterized by elemental analysis, UV–Vis, paramagnetic NMR, magnetic moment and single crystal XRD. The air and moisture stable Co(II) title complex is a 15 electron species which crystallizes in the monoclinic space group P2₁/n with cell dimensions a = 10.406(3), b = 12.873(4), c = 13.859(7) ?, β = 96.30(3)˚ and Z = 4. The cobalt atom has distorted tetrahedral (td) geometry with coordination provided by an amine and pyridyl nitrogen donors of BP and two terminal chloride ions. The packing is stabilized through C–H···π and van der Waals interactions.     

Low-Dimensional Compounds Containing Cyanido Groups. XX. Synthesis,Crystal Structure and Spectroscopic Properties of Polymeric 1,10-Phenanthroline-<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Copper(II) Tetracyanidoplatinate(II)

Abstract  

Polymeric {[Cu(phen)][Pt(CN)₄]} _n compound (phen = 1,10-phenanthroline) has been prepared under hydrothermal conditions using CuSO₄ · 5H₂O, phen and K₂[Pt(CN)₄] · 3H₂O, and characterized by chemical analysis and IR spectroscopy. The X-ray structure analysis [C2/c, a = 6.6057(7), b = 19.747(2), c = 11.5891(13) ?, β = 91.723(10)°] has revealed that the coordination geometry of the Cu(II) atom, situated on a two-fold rotation axis, is tetragonally distorted octahedral. Two nitrogen donor atoms originate from one blocking phen ligand, chelate coordinated in the equatorial plane at the distance of 2.026(4) ? (2×). The remaining four coordination sites are occupied by the nitrogen atoms [Cu–N = 1.975(5) (2×) and 2.574(5) ? (2×)] of two pairs symmetrically related bridging cyanido groups. These link Cu(II) with Pt(II) atoms, which lie on symmetry centers and are coordinated by four C-bonded cyanido ligands in the square planar form. Thus infinite 2D wave-like net is formed in the ac plane stabilized by π–π interactions between the phen molecules.     

Three New Complexes Based on a Flexible Bis(benzimidazole) Ligand and Rigid/Flexible Organic Carboxylates

Abstract  

Three new polymeric frameworks, [Ni(bbbm)(L1)₂] _n (1), [Ni(bbbm)(L2)₂] _n (2), and {[Co(bbbm)(L3)]·H₂O} _n (3) (bbbm = 1,4-bis(N-benzimidazolyl) butane, HL1 = 4-bromobenzoic acid, HL2 = 3-methylbenzoic acid, and H₂L3 = glutaric acid) have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Complex 1 features a one-dimensional (1D) linear chain structure bridged by bbbm ligands, which is further connected into a supramolecular double chain structure through intermolecular π–π stacking interactions. Complex 2 contains 1D zigzag chain, which is further arranged into a 2D supramolecular architecture by hydrogen bonding and π–π stacking interactions. In the structure of 3, there are infinite 1D zigzag Co(II)-bbbm chains linked together by L3 ligands to generate an undulated 2D (4,4) sheet, which is further connected by intermolecular π–π stacking interactions to form a 3D supramolecular network. Furthermore, thermal stability and luminescent property of 1–3 were investigated.     

Structure of Diaqua 1,10-Phenanthroline Cobalt (II) 2,5-Pyridinedicarboxylate Monohydrate

Abstract  

The coordination complex namely diaqua 1,10-phenanthroline cobalt (II) 2,5-pyridine dicarboxylate monohydrate that is formulated as [Co(H₂O)₂(PHEN)(PDC)] H₂O, (PHEN is the abbreviation of 1,10-phenanthroline and PDC is the abbreviation of 2,5-pyridinedicarboxylate), has been hydrothermally synthesized and characterized via single crystal X-ray diffraction techniques. This compound is monoclinic, space group P21/c, with Z = 4 in a unit cell with dimensions a = 11.7840(5) ?, b = 7.5298(3) ?, c = 21.5238(9) ?, β = 93.124(3)°. The structure contains one crystallographic unique Co atom, two coordinate water molecules, one PHEN species, one PDC fragment and one lattice water molecule. Extensive water O–H···O hydrogen bonding interaction among the adjacent discrete molecules leads to a two dimensional framework. This structure represents the first of cobalt compound in the system of PDC and PHEN that has been reported.     

Synthesis and Crystal Structures of Methyl 3-(Benzoylamino)-6-methyl-2-oxo-2<Emphasis Type="Italic">H</Emphasis>-pyran-5-carboxylate and <Emphasis Type="Italic">N</Emphasis>-[5-(3,4-Dimethoxyphenyl)-6-methyl-2-oxo-2<Emphasis Type="Italic">H</Emphasis>-pyran-3-yl]benzamide

Abstract  

The compounds methyl 3-(benzoylamino)-6-methyl-2-oxo-2H-pyran-5-carboxylate (1), C₁₅H₁₃NO₅, and N-[5-(3,4-dimethoxyphenyl)-6-methyl-2-oxo-2H-pyran-3-yl]benzamide (2), C₂₁H₁₉NO₅, crystallize as a centrosymmetric hydrogen-bonded dimer facilitated by N–H···O interactions involving the amide and carbonyl moiety of the lactone group of adjacent molecules. Supramolecular aggregation in 1 is controlled by a combination of π–π interactions [centroid–centroid distance = 4.0745(11) ?] and weak C–H···O hydrogen bonding between the phenyl ring of the benzoylamino group and the carbonyl atom of the methoxycarbonyl group and in 2 by a combination of π–π interactions [centroid–centroid distance = 4.0699(8) and 4.1556(10) ?], weak C–H···O interactions between the methoxy substituents of the adjacent dimethoxyphenyl group and weak C–H··· π interactions.     

Synthesis, Crystal Structure and Properties of the Binuclear Complex [Sm2(C10H9N2O4)2(C10H8N2O4)2(H2O)4]

Abstract  A novel binuclear Smarium (III) complex with N-(2-propionic acid)-salicyloyl hydrazone (C₁₀H₁₀N₂O₄, H₃L) was prepared and characterized. The crystal structure of [Sm₂(H₂L)₂(HL)₂(H₂O)₄] (1) was determined by X-ray single crystal diffractometry. 1 crystallizes in the monoclinic systerm, space group P2(1)/c, with a = 0.10229(2), c = 31.549(7), b = 0.70599(15) nm, and Z = 4. In the structure, Sm(III) is nine-coordinated by carboxyl O and acyl O atoms and imido N atoms of two ligands (H₂L and HL forms) and O atoms from two water molecules. H₂L and HL act as tridentate ligands which form two stable five-numbered chelating rings sharing one edge in the keto form for each ligand, and the carboxyl groups of two ligands were coordinated via bidentated bridging form. The coordination polyhedron around Sm (III) was described as a monocapped square antiprism. The inter- and intramolecular hydrogen bonds resulted in a three-dimensional network and provided extra stability for the structure. The complex was researched the interaction with calf thymus DNA by electronic absorption titration and emission titration. The results show that the complex is bound to calf thymus DNA mainly by intercalation .The complex also shows good fluorescence property. Index Abstract  The title compound, [Sm₂(H₂L)₂(HL)₂(H₂O)₄] was synthesized by the treatment of N-(2-propionic acid)-salicyloyl hydrazone (C₁₀H₁₀N₂O₄, H₃L) and Sm(NO₃) · 4H₂O and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that Sm (III) is nine-coordinated by carboxyl O and acyl O atoms and imido N atoms of two ligands (H₂L and HL forms) and O atoms from two water molecules. The carboxyl groups of two ligands were coordinated via bidentated bridging form. The coordination polyhedron around Sm (III) was described as a monocapped square antiprism. The inter- and intramolecular hydrogen bonds resulted in a three-dimensional network and provided extra stability for the structure.      

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.     

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.     

The structure of [Co(H-tptz)Cl3]·H2O (tptz=2,4,6-tri(2-pyridyl)-1,3,5-triazine) prepared by crystallization from the ionic liquid, N-butyl-N-methyl-pyrrolidinium bis(trifluoromethanesulfonyl)imide

The structure of tris-chloro[2,6-bis(2′-pyridyl)-4-(2′-pyridinium)-1,3,5-triazine]cobalt(II) monohydrate, [Co(C₁₈H₁₃N₆)Cl₃]·H₂O (C2/c (No. 15), a=7.783(11), b=22.42(3), c=11.001(15) ?, β=90.05(2)°), crystallized from the open air reaction of CoCl₂ and 2,4,6-tri(2-pyridyl)-1,3,5-triazine in the ionic liquid, N-butyl-N-methyl-pyrrolidinium bis(trifluoromethanesulfonyl)imide is reported. The structure consists of six coordinate cobalt in an octahedral geometry bonded to the tridentate tptz ligand and three chlorines. The non-coordinating pyridyl group in the tptz ligand is protonated (with the protonated nitrogen crystallographically disordered over two possible sites), providing overall charge neutrality for the complex.     

Synthesis, Crystal Structure and Cytotoxic Property of Bis(4-chlorobenzoato)bis[1-(2-aminoethyl)piperidine]disilver(I)

Abstract  

4-Chlorobenzoic acid reacts with silver oxide and 1-(2-aminoethyl)piperidine to give a dinuclear silver(I) complex, [Ag₂(C₇H₄ClO₂)₂(C₇H₁₆N₂)₂]. The complex was characterized by elemental analysis and X-ray diffraction. The complex crystallizes in the triclinic space group P−1 with unit cell dimensions a = 6.8550(10), b = 8.7370(10), c = 13.859(2) ?, α = 73.213(3), β = 87.945(3), γ = 77.050(3)°, V = 774.09(18) ?³, Z = 1, R ₁ = 0.0386, and wR ₂ = 0.0791. The dimeric Ag complex is located on an inversion center. The Ag atom in the complex is three-coordinated by two N atoms from two 1-(2-aminoethyl)piperidine ligands and by one O atom of a 4-chlorobenzoate ligand, forming a triangular coordination. In the crystal structure, the molecules are linked through intermolecular N–H···O hydrogen bonds, forming chains running along the a axis. The complex shows high cytotoxic property to both normal and carcinoma cells.     

Synthesis and Structural Studies of [Na(C7H6O4)(H2O)3](C7H5O4)?·?2H2O

Abstract  The mononuclear complex [Na(C₇H₆O₄)(H₂O)₃](C₇H₅O₄) · 2H₂O has been synthesized and characterized by IR, single crystal X-ray and thermal analysis. The compound crystallizes in the monoclinic space group P2₁ with a = 3.623(2) ?, b = 15.872(6) ?, c = 15.650(5) ?, β = 93.13(4)°, V = 896.6(7) ?³ and Z = 2. The central sodium ion is six coordinated with distorted octahedral geometry by two oxygen atoms from two bridging 3,5-dihydroxybenzoate ligands and four ones from different water molecules. The notable feature of the title complex is the formation of a three-dimensional network, through the combination of coordination bonds, hydrogen bonds and π···π interactions. There are one-dimensional channels in the structure, filled in by water molecules. The compound dehydrates in the temperature range of 70–125 °C and then is stable up to 230 °C. Index Abstract  The mononuclear complex [Na(C₇H₆O₄)(H₂O)₃](C₇H₅O₄) · 2H₂O has been synthesized and characterized by IR, single crystal X-ray and thermal analysis.      

Hydrogen Bonded 3D Supramolecular Architectures of Two Organic Salts Assembled from 2-Aminoheterocyclic Compounds and Phosphoric Acid

Abstract  

Two phosphate salts (2-aminopyrimidine): (phosphoric acid): H₂O [HL1⁺ (H₂PO₄) ⁻ ]·H₂O (1), and (4-phenylthiazol-2-amine): (phosphoric acid) [HL2⁺·(H₂PO₄)⁻] (2) based on 2-aminoheterocyclic compounds, 2-aminopyrimidine (L1), and 4-phenylthiazol-2-amine (L2) were prepared and structurally characterized by X-ray crystallography. Compound 1 crystallizes in the triclinic, space group P-1, with a = 6.2201(7) Å, b = 8.6139(9) Å, c = 9.4800(10) Å, α = 109.685(2)°, β = 106.3340(10)°, γ = 95.4450(10)°, V = 448.72(8) Å³, Z = 2. For 1, the cations were linked to each other via intermolecular C–H···N hydrogen bonds to form a 1-D chain structure running along the a-axis direction. The anions and the water molecules were connected alternatively along the a-axis direction through O–H···O hydrogen bonds to form a 1-D chain also. The cationic chains and the anionic chains were alternatively connected along the c-axis direction through N–H···O and C–H···O hydrogen bonds to form a 2D corrugated sheet. Adjacent sheets were combined together through π–π interaction to form double sheet. These double sheets were further joined together by O–H···O and N–H···O hydrogen bonds to produce a 3D network structure. Compound 2 crystallizes in the Orthorhombic, space group Pbca, with a = 10.1929(10) Å, b = 8.4406(9) Å, c = 27.589(2) Å, α = 90°, β = 90°, γ = 90°, V = 2373.6(4) Å³, Z = 8. In 2, the phosphates formed 1D chain along the b-axis through two P–O–H···O = P hydrogen bonds. The cations formed 1D zigzag chain along the b-axis direction under the CH–π interaction. The anionic chains were intercalated between two adjacent cationic chains through N–H···O, O–H···O, C–H···O, and O–S contacts. Such stacking repeated along the c-axis direction to form a 3D network structure.     

Synthesis and Crystal Structure of [Na(H<Subscript>2</Subscript>O)<Subscript>1.5</Subscript>][Na(H<Subscript>2</Subscript>O)<Subscript>3.5</Subscript>] X<Subscript>2</Subscript>·2H<Subscript>2</Subscript>O (X = 4′-Methoxy-7-Hydroxyisoflavone-3′-Sulfonate)

Abstract  

Water-soluble derivative of formononetin, [Na(H₂O)_1.5][Na(H₂O)_3.5] X₂·2H₂O(X = 4′-methoxy-7-hydroxyisoflavone-3′-sulfonate) was synthesized by sulfonation reaction. It was characterized by IR, ¹H NMR and single-crystal X-ray diffraction analysis. Single-crystal X-ray diffraction analysis showed that the title compound crystallized in a triclinic space group P-1 with cell parameters a = 6.9642(15) ?, b = 13.343(3) ?, c = 20.634(5) ?, α = 107.115(3)˚, β = 93.121(4)˚, γ = 91.911(3)˚, V = 1827.3(7) ?⁻³, D _c  = 1.575 Mg m ⁻³, Z = 2. There are two conformers of 4′-methoxy-7-hydroxyisoflavone-3′-sulfonate anions, two kinds of sodium cations, five coordinated water molecules and two lattice water molecules in the crystal structure. The sodium atoms coordinated with the oxygen atoms from water molecules, hydroxyl groups and sulfo-groups to form a Na–O coordinated network. Aromatic π···π stacking interactions and hydrogen bonding existed in the crystal structure of title compound, which together with coordinated interactions and electrostatic interactions between sodium cations and anions sulfonates C₁₆H₁₀O₄SO₃ ⁻ lead to the moieties into a three-dimensional network.