Synthesis and Crystal Structure of Bis (<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′,<Emphasis Type="Italic">N</Emphasis>′-tetramethylethylendiammonium) Octaiodo Pentachloroantimonate (III)

Abstract  

The synthesis and Crystal structure are given for the bis (N,N,N′,N′-tetramethylethylendiammonium) octaiodo pentachloroantimonate (III) salt. An X-ray investigation has shown that the title compound crystallizes in a monoclinic system, space group P2₁/m with the following lattice parameters a = 9.786(2) Ǻ, b = 14.024(5) Ǻ, c = 14.336(3) Ǻ, β = 91.35(2)° and Z = 2. The structure was solved from 3085 independent reflections with R ₁ = 0.0402 and wR ₂ = 0.0952 and refined with 152 parameters. The structure shows a layer arrangement perpendicular to the [(b)\vec] \vec{b} -axis: planes of [SbCl₅]²⁻, I₃ ⁻ and I₅ ⁻ anions alternate with planes of [(CH₂)₂(NH(CH₃)₂)₂]²⁺ cations. The [SbCl₅]²⁻ square pyramids present an active lone electron pair (LEP) on the Sb atoms and they are interconnected by means of N–H···Cl hydrogen bond originating from [(CH₂)₂(NH(CH₃)₂)₂]²⁺ entities. The polyiodides (I₃ ⁻ and I₅ ⁻) anions form a planer zigzag polymeric chains via I···I linking interactions. These chains are linked to the [SbCl₅]²⁻ anions by a long range contact.     

Synthesis and Crystal Structure of <Emphasis Type="Italic">Tris</Emphasis>-(<Emphasis Type="Italic">N</Emphasis>–<Emphasis Type="Italic">N</Emphasis> dimethyl benzylammonium)-hexachlorobismuthate(III)

Abstract  The salt tris-(N–N dimethyl benzylammonium)-hexachlorobismuthate(III) crystallizes in the triclinic system P1 with unit cell parameters: a = 9.0300(12), b = 9.9220(3), c = 19.575(2) ?, α = 79.955(5), β = 89.952(2), γ = 88.108(6)°, V = 1726.0(3) ?³, Z = 2. The examination of the structure shows an alternate stacking of inorganic layers of hexachlorobismuthate(III) anions and organic layers of [C₆H₅CH₂NH(CH₃)₂]⁺ cations parallel to the a-axis. The cohesion forces of the packing of N–N dimethyl benzylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N–H⋯Cl) and van der Waals contacts. Index Abstract  The examination of the structure shows a layer arrangement parallel to the a-axis: planes of octahedral anions [BiCl₆]³⁻ alternate with planes of [C₆H₅CH₂NH(CH₃)₂]⁺ cations (Fig. 3). The cohesion forces of the packing of the N–N dimethyl benzylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N–H⋯Cl) and van der Waals contacts. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis,Characterization, and Crystal Structure of <Emphasis Type="Italic">N</Emphasis>-<Emphasis Type="Italic">p</Emphasis>-Bromophenyl-<Emphasis Type="Italic">N</Emphasis>′-Phenylacetylthiourea

Abstract   N-p-bromophenyl-N′-phenylacetylthiourea was characterized by elemental analysis, IR and ¹H NMR etc. Single crystal structure of the title compound was determined on X-ray diffraction instrument. The title compound crystallizes in monoclinic space group c2/c, with a = 21.442(5) ?, b = 12.208(2) ?, c = 11.955(2) ?, β = 109.375(4)°, and D _calc = 1.571 g/cm³ for Z = 8. An intermolecular hydrogen bond N–H···S which links two thiourea molecules as a dimer and an offset face-to-face π–π stacking interaction were observed in the title compound. The strong non-covalent interaction influences the conformation and property of thiourea derivatives. Index Abstract  The title compound, N-p-bromophenyl-N′-phenylacetylthiourea, was synthesized by the treatment of phenylacetyl chloride with 4-bromoaniline and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that hydrogen bonds and face-to-face π–π stacking interactions have strong influence on the conformation and molecular stacking of the title compound.      

Intermolecular Hydrogen Bonds and the Supramolecular Structure of <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis(<Emphasis Type="Italic">p</Emphasis>-tolylsulfonyl)diethylenetriamine

Abstract  The title compound N,N′-bis(p-tolylsulfonyl)diethylenetriamine (1) was synthesized and its crystal structure determined by X-ray diffraction. Adjacent molecules of 1, symmetrically related through a c-glide, are linked by alternating hydrogen bonds that form molecular chains along [0 0 1]. Two molecular chains occur in each unit cell and pack to form alternating layers in a three-dimensional supramolecular structure. The compound crystallizes in the Pca2₁ space group stabilized by the inclusion of solvent dichloromethane molecules in structural voids between molecules of 1. The dichloromethane molecules are related through a twofold screw rotation axis and are not disordered. Index Abstract  Intermolecular hydrogen bonds involving sulfonamide moieties of title compound afford a supramoleular structure that accommodates the inclusion of dichloromethane in alternating layers.      

Crystal Structure of Unsymmetrically <Emphasis Type="Italic">N</Emphasis>-nor-dehydroabietyl-<Emphasis Type="Italic">N</Emphasis>′-isopropyl Urea

Abstract  

The title compound (C₄₆H₇₂N₄O₂, M _r  = 713.08) [systematic name: 1-isopropyl-3-((1R,4aS,10aR)-7-isopropyl-1, 4a-dimethyl-1,2,3,4,4a,9,10,10a-octahydrophenanthren-1-yl)urea] is a new derivative of dehydroabietic acid. It crystallized in the orthorhombic system, space group P2₁2₁ 2₁ with cell dimensions of a = 9.5950(19) ?, b = 18.740(4) ?, c = 24.654(5) ?, V = 4,433.0(16) ?³, Z = 4, D _c  = 1.068 g/cm³, λ = 0.71073 ?, μ = 0.07 mm⁻¹, F(000) = 1,568, final R = 0.0777 and wR = 0.1731 for 2,048 observed reflections with I > 2σ(I). Two crystallorgraphically independent molecules with different conformations co-exist in the structure. Each molecule exhibit classic tricyclic hydrophenanthrene structure, the two cyclohexane rings form a trans ring junction with chair and half-chair conformations, respectively. The crystal is stabilized by intermolecule hydrogen bonds and the molecules are in a head–tail zigzag arrangement.     

Synthesis,spectroscopic and structural studies of <Emphasis Type="Italic">N</Emphasis>-(1<Emphasis Type="Italic">H</Emphasis>-benzimidazol-2-yl)-<Emphasis Type="Italic">N</Emphasis>′-benzyl propionamidine

N-(1H-Benzimidazol-2-yl) propionimidic acid ethyl ester (1) reacts with benzylamine to yield the corresponding N-(1H-Benzimidazol-2-yl)-N′-benzyl proponamidine (2). The structure and conformation of the amidine 2 were determined by ¹H and ¹³C NMR and X-ray diffraction. The product crystallizes in monoclinic system with space group P2₁/c, a = 10.7913 ?, b = 15.5164 ?, c = 9.1130 ?, β = 108.378° and Z = 4. In the crystal there are two N–HN hydrogen bonds, the first is intramolecular H-Bond links H4 to N1; the second one is intermolecular and it links H2 to N3 of a second molecule leading to inversion-related dimers. The X-ray results were compared with those obtained by semi-empirical and ab-initio calculations.     

Synthesis and Crystal Structure of <Emphasis Type="Italic">N</Emphasis>′-(6-Chloropyridin-3-formyl)-<Emphasis Type="Italic">N</Emphasis>-<Emphasis Type="Italic">t</Emphasis>-Butyl Urea

Abstract The crystal structure of N′-(6-chloropyridin-3-formyl)-N-t-butyl urea, C₁₁H₁₄ClN₃O₂, has been established, and which belongs to monoclinic crystal system, space group Pn with unit cell dimensions a = 9.335(3) ?, b = 12.715(3) ?, c = 21.813(6) ?, β = 95.417(6)°, V = 2577.6(12) ?³ and Z = 8. An intramolecular N–H···O hydrogen bond forms a six-membered ring in the central part of the molecule. Both two N–H atoms of single unit participate in intermolecular hydrogen bonds and an intramolecular hydrogen bond, respectively. Index Abstract The crystal structure ofN′-(6-chloropyridin-3-formyl)-N-t-butyl urea, C₁₁H₁₄ClN₃O₂, has been established, and which belongs to monoclinic crystal system withZ = 8, space group Pn.      

Crystal and molecular structure of bis-(1-<Emphasis Type="Italic">tert-</Emphasis>butyl-1,2-dibenzoylhydrazine)-<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-sulfide

The structure of the title compound bis-(1-tert-butyl-1,2-dibenzoylhydrazine)-N,N- sulfide was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2(1)/c with the following crystallographic parameters: a = 14.681(7) Å, b = 14.501(7) Å, c = 16.535(8) Å, = 90°, = 109.173(9)°, = 90°, V = 3325(3) Å ³, z = 4, Dx = 1.244 mg/m³, F(000) = 1320, T = 293(2) K, 1.47° 25.00°, the final R factor: R₁ = 0.0584, wR₂ = 0.1111. The bond distances and angles in the tert-butyl groups are different, that can interpret its ¹H NMR spectra, which are very unusual for the absorption of –CMe₃ being multiple.     

Synthesis and crystal structure of <Emphasis Type="Italic">N</Emphasis>-(6methoxylbenzothiazol-2-yl)-1-(4-fluorophenyl)<Emphasis Type="Italic">O</Emphasis>,<Emphasis Type="Italic">O</Emphasis>-dipropyl-<Emphasis Type="Italic">α</Emphasis>-aminophosphonate

Molecular and crystal structure of N-(6-methoxybenzothiazol-2-yl)-1-(4-fluorophenyl)-O,O-dipropyl-α-aminophosphonate, C₂₁H₂₆FN₂O₄PS, have been determined by single-crystal X-ray diffraction study. The title compound is tetragonal, with a = 21.35(3) Å, c = 20.16(5) Å, Z = 16, D _x = 1.308 Mg/m³, μ(MoKα) = 0.247 mm^?1, and space group is I4₁/a. The structure was solved by direct method and refined to a final R = 0.0687 for 2370 reflections with I > 2σ(I). The compound shows a fully delocalized benzothiazole system with a sp² hybridization of the N(2). There is a strong intermolecular hydrogen bond between P=O and NH. The crystal structure is stabilized by a strong intermolecular N–H?sO hydrogen bond.     

2,4-Pentane <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis(2,6-Diisopropylphenyl) ketiminato cobalt (II) (trimethylsilyl)methylene

Abstract  

The title compound [^MeL^iPrCoCH₂Si(CH₃)₃ ^MeL^iPr = 2,4-pentane-N,N′-bis(2,6-diisopropylphenyl) ketiminato] possesses trigonal planar geometry and crystallizes in monoclinic space group P2₁/n with crystal cell parameters a = 10.6155(14) ?, b = 21.279(3) ?, c = 14.8057(19) ?, β = 97.196(2)°, V = 3,318.1(7) ?³, and Z = 4. The title compound is the second reported three coordinated 13 valence electron Co(II) alkyl complex and the first such complex reported with an asymmetrically bonded alkyl group. The steric effects are discussed in comparison of known similar structures of Fe, Co, and Zn.     

Crystal Study of <Emphasis Type="Italic">N,N</Emphasis>′-diphenyl-<Emphasis Type="Italic">N,N</Emphasis>′-bis(1-naphthyl)-1,1′-biphenyl-4,4′-diamine

Abstract  

The structure of N,N′-diphenyl-N,N′-bis(1-naphthyl)-1,1′-biphenyl-4,4′-diamine (NPB) with two molecules in the asymmetric unit, was solved and refined to a final R factor of 0.0434. The compound crystallized in the triclinic crystal system, space group P − 1, Z = 2, V = 1597.0(3) ?³ with unit cell parameters a = 10.3077(10) ?, b = 11.3545(11) ?, c = 14.4778(14) ?, α = 82.339(2)°, β = 77.657(2)°, and γ = 75.526(2)°. The two molecules in the asymmetric unit differed in the orientation of their triarylamino groups. The biphenyl group in the central structure is coplanar, and the angle between the least-square planes of the two six-carbon rings of the biphenyl moiety is zero degree. The packing of the molecules in the lattice is mainly due to the naphthyl-to-naphthyl π–π interaction with a distance of 3.861 ?.     

Crystal structure of [<Emphasis Type="Italic">N</Emphasis>-(2-aminoethyl)iminodiacetato](1,10-phenanthroline)copper(II) tetrahydrate, [Cu(<Emphasis Type="Italic">Aeida</Emphasis>)(<Emphasis Type="Italic">Phen</Emphasis>)] · 4H<Subscript>2</Subscript>O

Crystals of [N-(2-aminoethyl)iminodiacetato](1,10-phenanthroline)copper(II) tetrahydrate, [Cu(Aeida)(Phen)] · 4H₂O (I), are obtained, and their structure is determined. Crystals I are triclinic, and the unit cell parameters are as follows: a = 8.341(1) Å, b = 9.424(1) Å, c = 13.864(2) Å, α = 74.23(1)°, β = 79.25(1)°, γ = 82.67(1)°, Z = 2, and space group P1. The structural units of the crystal are [Cu(Aeida)(Phen)] molecular complexes and crystallization water molecules. The coordination polyhedron of the copper atom is a tetragonal bipyramid with four nitrogen atoms in the equatorial plane (mean Cu-N, 2.05 Å) and two oxygen atoms of the acetate groups in axial positions (Cu-O, 2.264 and 2.426 Å; O-Cu-O angle, 148.8°). The Aeida and Phen ligands fulfill the tetradentate (2N + 2O) chelate and bidentate (2N) chelate functions, respectively. The complexes are joined into dimer associates in which the interplanar spacing between Phen molecules is equal to 3.54 Å and the Cu?Cu distance is 7.02 Å.     

Synthesis,Spectroscopic Studies and Crystal Structure of <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-bis((thiophene-2-carboxamido)propyl)piperazine

Abstract  A new multidentate ligand N,N′-bis((thiophene-2-carboxamide)propyl)piperazine has been synthesized from the reaction of thiophene-2-carbonylchloride and 1,4-bis(3-aminopropyl)piperazine. The title compound has been characterized by elemental analysis, FT-IR, ¹H-NMR and ¹³C-NMR spectroscopic techniques. The crystal structure of the title compound (C₂₀H₃₀N₄O₂S₂Cl₂) has also been determined by X-ray analysis. The title compound crystallize in the monoclinic space group P2₁/c with a = 9.768(1), b = 12.895(1), c = 10.083(1) ?, β = 115.12(1)°, V = 1149.9(2) ?³, D _x = 1.425 g cm⁻³ and Z = 2. The crystal structure was solved by direct methods and refined by full-matrix least squares to a find R = 0.039 [I > 2σ (I)] for 2,786 observed reflections. Graphical Abstract  The (N,N’–bis((thiophene-2- carboxamido)propyl)piperazine) molecule has been synthesized and its molecule structure has been investigated by using , FT-IR, 13C NMR and 1H-NMR spectroscopic and crystallographic techniques.

Synthesis and Crystal Structure of Di-μ-chlorido-bis{chlorido[4-ethyl-<Emphasis Type="Italic">N</Emphasis>-(pyridin-2-ylmethylidene-κ<Emphasis Type="Italic">N</Emphasis>)aniline-κ<Emphasis Type="Italic">N</Emphasis>]mercury(II)}

The centrosymmetric dinuclear title complex [Hg₂Cl₄(dip)₂] was synthesized using the Schiff base bidentate ligand (E)-4-ethyl-N-(pyridine-2-ylmethylene)benzeneamine (dip) and mercury(II) chloride salts. It has been characterized by elemental analysis, X-ray diffraction, and UV-Visible and infrared spectroscopic techniques. The X-ray analysis shows that the title compound crystallizes in the monoclinic sp. gr. P2₁/n, Z = 2 with a = 7.8233(17) Å, b = 15.178(3) Å, c = 12.559(3) Å, β = 97.021(3)°. The Hg(II) ion has a distorted trigonal–bipyramidal coordination environment formed by the bischelating N-heterocyclic ligands, two bridging Cl atoms and one terminal Cl atom.     

Crystal Structure of Trinuclear Nickel(II) Complex with Schiff Base Ligand of <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis(Salicylidene)-1,3-Diiminopropane

Abstract  

A linear trinuclear nickel complex containing the ligand, N,N′-bis(salicylidene)-1,3-diiminopropane(H₂Salpn), is synthesized and characterized by elemental analysis, thermogravimetric analysis, IR spectroscopy and X-ray diffraction techniques. The title complex contains two different molecules, [Ni₃(Salpn)₂(CH₃COO)₂(DMF)₂](1) and [Ni₃(Salpn)₂(CH₃COO)₂(CH₃OH)₂]·2CH₃OH(2). Both molecules are constructed by two mononuclear NiSalpn units linked by a central Ni(II) ion and two bridging acetate anions, the difference between them is: molecule (1) contains two coordinated DMF molecules, while molecule (2) contains two coordinated methanol molecules and two hydrogen bond linked methanol molecules. All the Ni(II) ions are coordinated in disorted octahedral geometry. The crystal of the title complex(formula C₈₆H₁₀₆N₁₀Ni₆O₂₂, M _r 1,984.07) belongs to triclinic system, space group Pī(2) with the following crystallographic parameters: a = 12.1506(11) Å, b = 13.3601(12) Å, c = 14.8600(13) Å, α = 84.894(2)°, β = 70.101(2)°, γ = 81.899(2)°, V = 2243.9(3) ų, Z = 1, Dc = 1.468 g cm⁻³, μ = 1.310 mm⁻¹, F(000) = 1,036, and the final R indices[[I > 2σ(I)]: R ₁ = 0.0545, wR ₂ = 0.1052.     

Crystal and Molecular Structure of the 1:2 Adduct Formed Between <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Butylenebis(imidazole) and Carboxylic Acid Derivatives

Abstract  

Two imidazolyl derived complexes [N,N′-butylenebis(imidazole): (fumaric acid)₂ (1), and N,N′-butylenebis(imidazole): (2,4,6-trinitrophenol)₂ (2)] were prepared and structurally characterized by X-ray crystallography. Compound 1 crystallizes in the triclinic, space group P−1, with a = 5.9990(12) ?, b = 8.1772(16) ?, c = 10.419(2) ?, α = 86.88(2)°, β = 84.73(3)°, γ = 77.03(4)°, V = 495.67(17) ?³, Z = 1. For 1, two dimensional network structure is formed through imidazolium moieties forming hydrogen bonds to di-ionic carboxylate groups of fumarate chains. In the same network layers and adjacent layers, C–H···O contact also accompanies the N⁺–H···O⁻ hydrogen bonds, all these lead the extended architecture to show a three-dimensional lamellar structure. Compound 2 crystallizes in the triclinic, space group P − 1, with a = 7.0236(14) ?, b = 8.2831(17) ?, c = 12.053(2) ?, α = 106.05(4)°, β = 99.13(2)°, γ = 98.84(3)°, V = 650.8(2) ?³, Z = 1. In 2, two parallel imidazolium cations and two antiparallel 2,4,6-trinitrophenolate anions formed 32-membered rings through hydrogen bonding interaction, these rings extended along the c axis direction to form one dimensional railway structure. Adjacent parallel railways connect further through C–H···O hydrogen bonds between the 2-CH of the imidazole ring and the NO₂ group O atoms. These weak interactions combined, the complex showed 3D layer structure.     

Synthesis and Structure Determination of <Emphasis Type="Italic">S</Emphasis>,<Emphasis Type="Italic">S</Emphasis>′-(Naphthalen-2-ylmethyl sulfanyl (1-<Emphasis Type="Italic">p</Emphasis>-tolyl-ethylidene) Hydrazine

Abstract  

S,S′-(Naphthalen-2-ylmethyl sulfanyl (1-p-tolyl-ethylidene) hydrazine (SNM4MA) was prepared by the condensation of S-napthalen-2-ylmethyldithiocarbazate (SNMDTC) and 4-methylacetophenone. Yellow needles of SNM4MA were obtained upon slow evaporation of a 50:50 mixture of acetonitrile and DMSO over a period of weeks. The compound crystallizes in the monoclinic system with the space group C 2/c and Z = 4. The unit cell parameters are a = 7.0221(2) ?, b = 22.8428(6) ?, c = 23.5127(6) ? with β = 94.0222(13)°. Single crystal X-ray analysis shows that the molecule has crystallographic two-fold rotational symmetry coincident with the S–S bond. The title compound exists as a trans–cis conformer in which the naphthalene group is trans with respect to the thione sulfur while the benzyl group adopts a cis geometry. ¹³C and ¹H spectra confirm that the dimeric nature is retained in DMSO solution.     

Synthesis and Crystal Structure of New <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis[1-(4-methoxyphenyl)-5-methyl-1<Emphasis Type="Italic">H</Emphasis>-1,2,3-triazole-4-carbonyl]hydrazide

Abstract  The N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide 6 was synthesized from aryl triazole acids and its structure is established by MS, IR, and ¹H NMR spectral data. Compound 6, C₂₂H₂₂N₈O₄, Mr = 462.48, crystallizes in the monoclinic space group P2(1)/c with unit cell parameters a = 15.3451(8), b = 8.6486(4), c = 16.8502(9) ?, α = 90.00, β = 95.731(2), γ = 90.00o, V = 2225.1(2) ?³, Z = 4, and Dx = 1.381 mg m⁻³. The final R was 0.0450. The four aromatic rings are close to linear because of N···H–N hydrogen bonds. Index Abstract  Synthesis and crystal structures of N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide Heng-Shan Dong, Yan-Fei, Wang, Hong-Ru Dong, Bin, Wang, Bin Quan N,N′-Bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide was synthesized.      

Solid-state Spectroscopic and Structural Investigation of <Emphasis Type="Italic">cis</Emphasis>-(CH<Subscript>3</Subscript>)<Subscript>2</Subscript>Au(<Emphasis Type="Italic">O</Emphasis>,<Emphasis Type="Italic">O</Emphasis>′-acac)

Abstract  The structure of cis-(CH₃)₂Au(O,O′-acac) was investigated by single-crystal X-ray diffraction. It crystallizes in the orthorhombic space group Cmca with unit cell dimensions a = 6.7831(13) ?, b = 15.080(3) ?, c = 18.073(3) ? and α = β = γ = 90°. The molecule is planar but lacks a C₂ axis in the solid-state, with two Au–C bond lengths that differ by 0.078(21) ? due to crystal packing effects. The inequivalence of the crystallographic carbon positions is evident in the solid-state ¹³C CP-MAS NMR spectrum, which was recorded at low temperature due to the thermal sensitivity of the compound during magic-angle spinning. Head-to-tail stacking, which creates short intermolecular paths, was reproduced computationally in a dimer model. Graphical Abstract   Solid-state Spectroscopic and Structural Investigation of cis -(CH ₃ ) _Au 2 ( O , O ′-acac) Miyako Hisamoto • Swarup Chattopadhyay • Juergen Eckert • Guang Wu • Susannah L. Scott In the solid state, cis-(CH₃)₂Au(O,O′-acac) has no C₂ axis, two different Au–C bond lengths (1.960, 2.038 ?; Δd = 0.078(21) ?) and a close Au–C…C–Au contact; these features give rise to additional features in the ¹³C CP-MAS NMR spectrum.     

Crystal Structure of Antitubercular Complex: <Emphasis Type="Italic">cis</Emphasis>-(chloro)-[<Emphasis Type="Italic">N,N</Emphasis>′-<Emphasis Type="Italic">bis</Emphasis>-(diethyl-2,2′-bipyridine-3,3′-dicarboxylate)]ruthenium(II) Monohydrate

Abstract  Diethyl-2,2′-bipyridine-3,3′-dicarboxylate (3 or L) reacts with RuCl₃ · 3H₂O to give cis-(Cl)-[Ru(L)₂Cl₂] · H₂O (4) and structure of the complex was determined by spectral (IR, ¹H-NMR), and mass spectroscopic data, elemental analyses and X-ray crystallography. The structure is solved in triclinic, space group p-1 with a = 10.658 (2), b = 12.446 (3), c = 14.186 (5) ?, α = 104.856 (3), β = 108.704 (3), γ = 94.973 (2)°, V = 1693.2 (8) ?³, Z = 2 with final R = 0.012. The geometry of the complex is shown to be a distorted octahedral with four nitrogens of two 2,2′-bipyridyl ligands in two different planes with Ru–N distance as 2.021 (2)−2.071 (3) ?. The cis-position is occupied by two chloride atoms with Ru–Cl distance as 2.4156 (12) and 2.4167 (13) ?. The trans-axial Cl2–Ru1–N and Cl1–Ru1–N4 angles are respectively, 172.42 (7) and 174.12 (7)°. A weak hydrogen bonding is observed between the two chlorides and hydrogens of neighbouring molecule [C–H···Cl distance as 2.72, 2.77 (4) ?]. A second type of weak hydrogen bonding is also observed between the oxygens of carboxylate groups and hydrogens of a neighbouring molecule [C–H···O distance as 2.53, 2.56 and 2.34 (4) ?]. Graphical Abstract  The structure of anti-tubercular precursor complexes, cis-(chloro)-[N,N′-bis-(diethyl-2,2′-bipyridine-3,3′-dicarboxylate)]ruthenium(II) monohydrate is solved by single crystal X-ray diffraction analysis which reveals geometry of the complex to be a distorted octahedral with four nitrogens of two 2,2′-bipyridyl ligands in two different planes. The cis-position is occupied by two chloride atoms.