Crystal structure of cis-[Rh(biq)2Cl2]Cl·3H2O: Solid-state characterization and crystal packing analysis

The title compound, cis-[Rh(biq)₂Cl₂]Cl·3H₂O (biq = 2,2′-biquinoline) crystallized in the monoclinic space group P2 ₁ /n with a = 11.231(2) Å, b = 20.895(4) Å, c = 14.081(3) Å, β = 94.76(3)°, V = 3293.0(11) ų, D _c = 1.565 g cm⁻³, μ = 0.806 mm⁻¹, F(000) = 1576 and Z = 4. It contains a monomeric [Rh(biq)₂Cl₂]⁺ cation, a chloride ion and three molecules of H₂O. The rhodium(III) ion is hexa coordinated forming a distorted octahedral arrangement. The mean Rh(III)–N distance for the four Rh(III)–N bonds is 2.0625 Å. The two chloride atoms are bonded in a cis configuration [Rh(III)–Cl bond distances are 2.329(3) and 2.341(4) Å]. The structure shows a curling stacks of cationic complexes interacting via offset-face-to-face (OFF) π–π aryl interaction motif. Water molecules and chloride ions are hydrogen bonded (H₂O···H–OH and Cl···H–OH) and links the curling stacks by hydrogen bonding via Rh–Cl···H–OH interactions.     

Synthesis and characterization of a lead(II) complex [Pb(phen)(H<Subscript>2</Subscript>O)(NO<Subscript>3</Subscript>)<Subscript>2</Subscript>] (phen = 1,10-phenanthroline)

The monomeric lead(II) complex, [Pb(phen)(H₂O)(NO₃)₂] was prepared by a hydrothermal reaction of Pb(NO₃)₂, nitrilotriacetic acid, NaOH, 1,10-phenanthroline, and H₂O. The structure was determined by X-ray crystallography. It crystallizes in monoclinic P2(1)/n space group with the crystal cell parameters of a = 6.3568(6), b = 20.2345(19), c = 11.2722(9) Å, β = 98.337(4)^°, V = 1434.6(2) ų, and Z = 4. The crystal X-ray analysis shows that the lead atom is six-coordinated by two N atoms of phen ligand, three oxygen atoms of nitrate anions and one water molecule. Owing to the presence of a lone pair of electrons of lead atom, a significant gap occurs in the coordination geometry around Pb ion. A 3D architecture is formed through the strong hydrogen bonding and π–π stacking interactions.     

Synthesis and crystal structure of 2-benzoyl-4-methyl phenyl benzoate

The crystal structure of the title compound, C₂₁H₁₆O₃, has been determined. The compound crystallizes in triclinic space group PĪ with cell parameters a = 9.2240(9) Å, b = 9.8050(8) Å, c = 10.1610(11) Å, α = 94.749(6)^∘, β = 112.544(4)^∘, γ = 102.145(6)^∘ and Z = 2. The structure exhibits both intra and intermolecular interactions of the type C–H ⋅s O. The intermolecular interaction between the molecules form centrosymmetric dimers.     

Synthesis and crystal structure of anhydrous copper suberate: [Cu<Subscript>2</Subscript>(OOC-(CH<Subscript>2</Subscript>)<Subscript>6</Subscript> -COO)<Subscript>2</Subscript>]

The title compound [Cu₂(OOC-(CH₂)₆-COO)₂] was synthesized and its crystal structure has been determined by single crystal X-ray diffraction methods. The complex crystallizes in the triclinic space group P-1 with a=5.1077(5) ?, b=8.362(2) ?, c=11.378(2) ?, α=93.773(6)°, β=97.587(9)°, γ=90.493(’9)° and D _cal=1.629 mg/m³ for Z=1.  The structure is polymeric and consists of discrete anhydrous centrosymmetric binuclear units [Cu₂(OOC-(CH₂)₆-COO)₂]. The two copper(II) centres bridged by the suberate groups in a syn-syn conformation, are in pentacoordinated distorted square-pyramidal coordination environment, with an intramolecular Cu–Cu distance of 2.5793(10) ?. Each binuclear unit, related to the next through μ_oxo bridges with a Cuμ_oxo–Cuμ_oxo separation of 3.2326(10)?, defines infinite chains of one-edge sharing CuO₅ square pyramid.     

Synthesis,Separation and Crystal Structures of <Emphasis Type="Italic">E</Emphasis> and <Emphasis Type="Italic">Z</Emphasis> Isomers of 3-(2,5-Dimethoxyphenyl)-2-(4-Methoxyphenyl)Acrylic Acid

Abstract Synthesis, separation and X-ray crystal structures of E and Z isomers of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylic acid are reported. Separation of E and Z isomers from a 1:1 mixture has been carried out by selective acidification of their sodium salts carefully controlling the pH of the solution. The structures of E and Z isomers were confirmed by determining crystal structures of these isomers using single crystal X-ray diffraction. The E isomer crystallizes in the P2₁/c space group with a = 11.493(2) ?, b = 5.5456(11) ?, c = 24.900(5) ?, α = 90°, β = 92.36(3)°, γ = 90°, Z = 4. The Z isomer crystallizes in the P2₁/c space group with a = 10.192(2) ?, b = 12.893(3) ?, c = 13.948(3) ?, α = 90°, β = 92.18(3)°, γ = 90°, Z = 4. Details of the synthesis and structural characterization and X-ray crystal structure determination of the title compounds are presented. Index Abstract Synthesis, Separation and Crystal Structures of E and Z Isomers of 3-(2,5-Dimethoxyphenyl)-2-(4-Methoxyphenyl)Acrylic Acid Balachandra Chenna, Bidhan A. Shinkre, Shweta Patel, Samuel B. Owens Jr., Gary M. Gray, Sadanandan E. Velu* Separation of E and Z isomers of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylic acid from a 1:1 mixture has been carried out by selective acidification of their sodium salts and the structures of the individual isomers have been determined by X-ray single crystal diffraction.      

Two-dimensional crown ether complex. Synthesis and crystal structure of [Na(N15C5)]<Subscript>2</Subscript>[Cu(mnt)<Subscript>2</Subscript>]

A novel crown ether complex [Na(N15C5)]₂[Cu(mnt)₂] (1) (where N15C5 = 2,3-naphtho-15-crown-5 and mnt = maleonitriledithiolate, [C₂S₂(CN)₂]^2–) was synthesized and characterized by elemental analysis, FT-IR spectra, UV-visible spectra and single crystal X-ray diffraction. Structural analysis reveals that the complex 1 consists of two [Na(N15C5)]⁺ complex cations and one [Cu(mnt)₂]^2– complex anion and the complex molecules are assembled into a novel 2D network by Na–N interactions. In the network, there are 34-member macrocycles formed by four sodium ions of complex cations and four complex anions through Na–N bonds. In each macrocycle, – stacking interactions occurred between two parallel naphthylene moieties of N15C5. It is interesting that the 2D network displays an open-capped wave-like sheet viewed along the crystallographic a axis.     

Synthesis of <Emphasis Type="Italic">E</Emphasis> Isomer and Crystal Structures of <Emphasis Type="Italic">E</Emphasis> and <Emphasis Type="Italic">Z</Emphasis> Isomers of 3-(2,5-Dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile

Abstract Details of the synthesis of the E isomer of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile, and the X-ray crystal structures of both the E and Z isomers of this compound are presented. The E isomer crystallizes in the P2₁/c space group with cell parameters, a = 8.5659(17) ?, b = 16.399(3) ?, c = 11.224(2) ?, α = 90°, β = 95.27(3)°, γ = 90°and Z = 4. The Z isomer crystallizes in the Pca2₁ space group with cell parameters, a = 4.1223(8) ?, b = 19.113(4) ?, c = 19.453(4) ?, α = 90°, β = 90°, γ = 90° and Z = 4. Index Abstract Synthesis of E isomer and X-ray crystal structure determination of both E and Z isomers of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile are presented.      

Synthesis and crystal structure of a novel 3D supramolecular complex [Na(DC18C6-B)][Ni(mnt)<Subscript>2</Subscript>]

A supramolecular complex [Na(DC18C6-B)][Ni(mnt)₂] (1) (DC18C6-B = cis-anti-cis-dicyclohexyl-18-crown-6, isomer B; mnt = maleonitriledithiolate) has been prepared and characterized by elementary analysis, FT-IR spectroscopy and X-ray single crystal diffraction. It crystallizes in triclinic, space group P1 with crystallographic data: a = 7.974(4) Å, b = 14.343(7) Å, c = 15.559(8) Å, α = 96.230(8)^∘, β = 100.361(8)^∘, γ = 93.849(9)^∘, V = 1733.2(15) ų, Z = 2, D_calcd = 1.408 g/cm³, F(000) = 766, R₁ = 0.0491, wR₂ = 0.1018. The formula unit contains one [Na(DC18C6-B)]⁺ complex cation and one [Ni(mnt)₂]⁻ complex anion, which are constructed into an infinite chain-like structure through Na–N bonds. The resulting chains crisscross on the [Ni(mnt)₂]⁻ complex anions and further assemble into an unusual 3D supramolecular framework via the weak interactions.     

Stereoselective Synthesis and X-Ray Structure Determination of Labeled [1, 2, 3-<Superscript>13</Superscript>C<Subscript>3</Subscript>]-1-(Phenylsulfinyl)-3-Benzyloxyacetone

[1,2,3-¹³C₃]-1-(Phenylsulfinyl)-3-benzyloxyacetone, C₁₆H₁₆O₃S, (3) has been synthesized and its crystal structure has been determined by a single-crystal X-ray diffraction analysis. The X-ray diffraction study revealed that compound 3 crystallizes in the monoclinic crystal system in the acentric space group Pc, with cell constants at T = 100 K: a = 16.073(5), b = 5.5079(16), c = 7.949(2) Å, β = 100.221(4)^°, V = 692.6(3) ų, Z = 2, d _calc = 1.383 g/cm³. Compound 3 contains the chiral tetravalent three-coordinated sulfur atom, which has a distorted tetrahedral configuration with a lone electron pair occupying one of the tetrahedron vertices. In the crystal, the molecules are packed in stacks along the b axis; the stacks consist of the molecules of the same chirality. Furthermore, the stacks of the molecules of the opposite chirality alternate along the c axis. The molecules in neighboring stacks are arranged by head-to-tail orientations. There are no short intermolecular contacts in the crystal of 3.     

Synthesis and crystal structure of bis(malonato)tetra (aqua)barium(II)cobalt(II): [BaCo(C<Subscript>3</Subscript>H<Subscript>2</Subscript>O<Subscript>4</Subscript>)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)<Subscript>4</Subscript>]

The title compound [BaCo(C₃H₂O₄)₂(H₂O)₄] was synthesized and its crystal structure was determined. The compound is orthorhombic, space group Pccn with a = 18.974(3) Å, b = 6.783(2) Å, c = 9.394(4) Å. The structure is polymeric and consists of edge-sharing BaO₈ polyhedra and CoO₆ octahedra linked together by the malonate groups. The geometry around the Ba(II) centres is a slightly distorted square-antiprism with Ba–O distances ranging from 2.789(4) to 2.843(4) Å. Around the Co(II) centres, the coordination forms a distorted octahedron with Co–O bonds between 2.040(3) and 2.238(4) Å.     

Synthesis and Crystal Structure of Complex [Nd(2-FC<Subscript>6</Subscript>H<Subscript>4</Subscript>COO)<Subscript>3</Subscript>·(2-FC<Subscript>6</Subscript>H<Subscript>4</Subscript>COOH)·H<Subscript>2</Subscript>O]<Subscript>2</Subscript>

The neodymium complex with 2-fluorobenzoic acid was synthesized and characterized by X-ray diffraction. The complex crystallizes in the triclinic system with space group Pī, lattice parameters: a = 9.2747(10) Å, b = 11.7594(13) Å, c = 13.5158(14) Å, α = 110.220(2)°, β = 93.930(2)°, γ = 90.894(2)°, V = 1378.8(3) Å³, Z = 1, Dcalc = 1.733 Mg/m³. The complex is a binuclear molecule in which four 2-fluorobenzoato groups act as bidentate and tridentate bridges between the two Nd³⁺ ions. Each Nd³⁺ ion is additionally chelated by one 2-fluorobenzoato group and coordinated by one 2-fluorobenzoic acid and one water molecule.     

Synthesis, characterization, and structural analysis of ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate

Ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate was prepared by reacting the lithium salt of ethyl cyanoacetate with (Z)-O-methyl-4-chloroben-zohydroximoyl fluoride. This compound crystallizes in space group Pbca,with lattice constants a=7.5740(15) ?, b=11.337(2) ?, and c=30.424(5) ? at 110 K. Characterizations include spectrometric identifications employing IR, UV, and ¹H and ¹³C NMR. The compound exists in the solid as the enamine tautomer, with the cyano group cis to the 4-chlorophenyl group (the Z configuration). The C=C and C–N bond distances are 1.3930(16) ? and 1.3278(16) ?, respectively. The N–H group forms a bifurcated hydrogen bond with acceptors C=O (intramolecular) and C≡N (intermolecular).Supplementary material CCDC-289444 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, by e-mailing data_request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; Fax: +44(0)1223-336033.     

Synthesis,characterization and crystal structure of bis{2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenolato}thiocyanatocobalt(III) perchlorate

Brown block-shaped crystals of bis{2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenolato}thiocyanatocobalt(III) perchlorate, the first cobalt(III) complex derived from the Schiff base ligand HL, [Co^III(L)(HL)(NCS)].ClO₄ (HL=2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenol) have been obtained and characterized by elemental analysis and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a=16.087(3) ?, b=12.354(3) ?, c=16.762(3) ?, β=93.77(3)°, V=3324.1(12) ?³, Z=4, R ₁=0.0741 and wR2=0.1366. X-ray structure determination revealed that the complex consists of a [Co^III(L)(HL)(NCS)]⁺ cation and a disordered perchlorate anion. The Co atom in the cation is six-coordinate in an octahedral coordination. In the crystal structure, the perchlorate anions are linked to the cations through intermolecular C–H⋯O hydrogen bonds, forming zigzag chains running along the caxis. It is the first cobalt(III) complex derived from the Schiff base ligand HL.     

Synthesis and crystal structure of a new composite complex between a hepta-coordinate ytterbium(III) and a heteropoly molybdic anion: [Yb(DMSO)<Subscript>7</Subscript>]H[SiMo<Subscript>12</Subscript>O<Subscript>40</Subscript>] (DMSO = dimethyl sulfoxide)

A new composite complex of the general formula [Yb(DMSO)₇]H[SiMo₁₂O₄₀] has been synthesized from H₄SiMo₁₂O₄₀⋅nH₂O, YbCl₃ and DMSO in mixed solvent of acetonitrile and water and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. Singe crystal X-ray structure analysis shows that it belongs to monoclinic system, space group P2₁/c, with a = 11.685(2) Å, b = 14.969(3) Å, c = 35.037(7) Å, β = 98.50(3)^∘, and Z = 4. There is one [Yb(DMSO)₇]³⁺ coordinated cation and one [SiMo₁₂O₄₀]⁴⁻ polyanion in one structure unit. The organic ligands (DMSO) do coordinate directly with ytterbium(III) to form a distorted pentagonal bipyramid complex ion by coordination bond, then combines to the SiMo₁₂O₄₀⁴⁻ anion by static electric force. The results of IR and X-ray diffraction show that there is strong interaction between polyoxometalate and organic donors.     

Synthesis and structural characterization of [Ni(Me2NCH2CH2CH2N=CHC6H4O)2]

The synthesis, properties, and X-ray crystal structure of a Ni(II) complex of the tridentate Schiff base ligand Me₂NCH₂CH₂CH₂N=CHC₆H₄OH(LH) are described. The complex crystallizes in the monoclinic space group P2₁/c, with a = 10.180(2), b = 15.169(3), c = 15.293(4) Å, = 106.69(2)°, and Z = 4. The Ni atom shows a distorted fac-octahedral geometry, with the two Ni—N(Me₂) bonds being significantly longer than the two Ni—N(imino) bonds, 2.284(9), 2.310(9) vs. 2.051(2), 2.055(2) Å.     

Synthesis and structures of two chiral bis(pyrazolyl)borate complexes, [{H<Subscript>2</Subscript>B(4-Mepz)(3,5-Me<Subscript>2</Subscript>pz)}<Subscript>2</Subscript>M], M = Co,Zn

The title compounds are chiral and have similar molecular geometries. The Co complex crystallizes in space group P2₁/c with a = 8.475(4) Å, b = 7.706(8) Å, c = 35.778(9) Å, = 95.779(18) and Z = 4, while the Zn complex crystallizes in space group P2₁/n with a = 8.353(3) Å, b = 20.768(4) Å, c = 13.818(3) Å, = 100.96(2) and Z = 4. The metal atoms are tetrahedrally coordinated to two bidentate ligands with M–N distances in the ranges 1.985(2)–2.018(2) Å (Co) and 1.985(2)–2.008(2) Å (Zn), and N–M–N angles in the ranges 96.07(7)–128.23(7) (Co) and 98.50(8)–125.63(8) (Zn). No agostic bonds are formed. The molecules display C₁ symmetry; geometric considerations indicate that the formation of the other two possible conformers, with C₂ symmetry, is sterically less favorable.     

Synthesis, characterization and crystal structure of a mononuclear zinc(II) complex derived from 2-methoxy- 6-[(3-cyclohexylaminopropylimino)methyl]phenol

Colourless block-shaped crystals of Dichloro{2-methoxy-6-[(3-cyclohexylaminopropy-limino)methyl]phenolato}zinc(II) methanol, [Zn(C₁₇H₂₆N₂O₂)Cl₂].CH₃OH, have been obtained and characterized by elemental analysis, IR and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a=12.980(3) ?, b=13.139(3) ?, c=13.277(3) ?, β=107.00(3)°, V=2165.4(8) ?³, Z=4, R ₁=0.0631 and wR2=0.1110. X-ray structure determination revealed that the complex consists of a [Zn(C₁₇H₂₆N₂O)Cl₂] moiety and a lattice MeOH molecule. In the crystal structure, molecules are linked through intermolecular N–HO, C–HCl and O–HCl hydrogen bonds, forming chains. It is the first complex derived from the Schiff base ligand 2-methoxy-6-[(3-cyclohexylaminopropylimino)methyl]phenol.Supplementary materialCCDC-606067 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam.ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Synthesis and characterization of platinum – selenium derivatives: X-ray structure of <Emphasis Type="Italic">trans</Emphasis>-Pt(PEt<Subscript>3</Subscript>)<Subscript>2</Subscript>(SePh)<Subscript>2</Subscript>

The crystal structure of trans-[((bis)triethylphosphine)(bis(phenylselenato))platinum (II)] has been determined by single crystal X-ray diffraction. Crystallization occurs in the triclinic space group P-1 (No. 2) with a = 8.9964(2) ?, b = 11.5103(2) ?, c = 14.9335(3) ?; α = 85.8750(10)°, β = 72.5350(10)°, γ = 68.4450(10)°. Details of the structure and spectroscopic results are presented and discussed and comparisons are made with related square planar platinum (II) structures.     

Separation of 4-aminobenzoic acid by cocrystallization: Crystal structure of the complex of 4-aminobenzoic acid with (2R,3R)-tartaric acid

4-Aminobenzoic acid (PABA) has been successfully separated from a mixture containing 2-aminobenzoic acid and (2R,3R)-tartaric acid. X-ray structure analysis confirms the separating result. The molecular complex formed by PABA and tartaric acid in 1:1 molar ratio crystallizes in the orthorhombic space group P2₁2₁2₁ with cell dimensions of a = 7.329(1) Å, b = 12.095(2) Å, c = 15.231(3) Å, V = 1350.1(4) ų, Z = 4. The crystal structure comprises protonated PABA, monoanion of tartaric acid, and crystalline water. The extensive H-bonding network exists in the crystal structure. H bonding between tartaric acid and both terminal groups on para position of PABA is considered as a possible reason for the successful separation.     

A structural study of copper(II) carboxylates: Crystal structure and physical characterisation of [Cu2(2-bromopropanoato)4(caffeine)2]

Based on the bond-valence sum model the continual transition between the bidentate and monodentate bonding mode of carboxylato group and minimum of Cu–O bond lengths were estimated. The dependence of Cu⋯Cu separation on Cu–N bond length in binuclear Cu(II) carboxylates with caffeine were derived and fitted to the observed data. The crystal structure of [Cu₂(2-bromopropanoato)₄(caffeine)₂] has been determined by X-ray crystallography. The structure consists of centrosymmetric binuclear units where the two Cu atoms are coordinated by four disordered bridging 2-bromopropionates and two caffeine ligands at the apices of a bicapped square prism. Both 2-bromopropionates show disorder of their –Br and –CH₃ substituents. Stacking π·π interactions between the adjacent caffeine molecules link the complex units in 1-D networks. The binuclear structure of the studied compound is consistent with magnetic data and EPR spectrum.