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,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.      

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 and Crystal Structures of 4-Chloro-<Emphasis Type="Italic">N′</Emphasis>-(4-hydroxy-3-nitrobenzylidene)benzohydrazide monohydrate and 4-Chloro-<Emphasis Type="Italic">N′</Emphasis>-(4-hydroxy-3-methoxybenzylidene)benzohydrazide monohydrate

Abstract  

Two new hydrazone compounds, 4-chloro-N′-(4-hydroxy-3-nitrobenzylidene)benzohydrazide monohydrate (1) and 4-chloro-N′-(4-hydroxy-3-methoxybenzylidene)benzohydrazide monohydrate (2), were synthesized and characterized by physico-chemical methods and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 23.257(3) ?, b = 4.829(1) ?, c = 12.763(2) ?, β = 96.017(2)°, V = 1425.5(5) ?³, Z = 4, R ₁ = 0.0525, and wR ₂ = 0.1120. Compound 2 crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 8.103(3) ?, b = 21.321(3) ?, c = 10.594(3) ?, β = 120.281(2)°, V = 1580.5(8) ?³, Z = 4, R ₁ = 0.0480, and wR ₂ = 0.1078. Both compounds contains a hydrazone molecule and a water molecule. The crystals of the compounds are stabilized by N–H···O, O–H···O, and O–H···N hydrogen bonds.     

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.     

Synthesis and Crystal Structure of <Emphasis Type="Italic">N-</Emphasis>(1-Methyl-3-ethyl-4-chloropyrazol-5-yl)acyl<Emphasis Type="Italic">-N′</Emphasis>-(4-fluorophenyl)thiourea

Abstract  

The title compound was synthesized by reaction of 1-methyl-3-ethyl-4-chloro-5-pyzolyl formaic isothiocyanate with 4-fluoroaniline and its crystal structure was determined by X-ray diffraction method. The compound crystallizes in the triclinic space group P [`1] \bar{1} with a = 7.8510 (10), b = 8.2731 (11), c = 11.9373 (15) ?, α = 78.484 (2), β = 88.938 (2), γ = 88.779 (2)°, V = 759.49 (17) ?³, M _r = 340.80, D _c  = 1.490 mg/m³, and Z = 2. In the title molecule, atoms in the acylthiourea moiety are able to form a plane due to the intramolecular hydrogen-bond N1–H1–O1, and makes a dihedral angle of 3.0° with the benzene ring, while the acylthiourea makes a dihedral angle of 7.6° with the pyrazole ring. The preliminary biological test shows that the title compound has some acaricidal activity.     

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.     

Syntheses and Crystal Structures of the Compounds Na<Emphasis Type="Italic">Ln</Emphasis>TiO<Subscript>4</Subscript> (<Emphasis Type="Italic">Ln</Emphasis> = La,Pr, Nd)

Abstract  

Single crystals of the NaLnTiO₄ (Ln = La, Pr, Nd) phases were grown out of reactive sodium hydroxide melts. These layered materials crystallize in space group P4/nmm of the tetragonal system, with unit cell dimensions of a = 3.7998(5) ? and c = 13.273(3) ? (La), a = 3.7686(5) ? and c = 12.940(3) ? (Pr), and a = 3.7551(5) ? and c = 12.848(3) ? (Nd). These compounds possess a layered structure that is a variant of K₂NiF₄ with ordering of the Na and Ln ions.     

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 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.      

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.      

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.     

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.     

Synthesis,Characterization and Crystal Structure of <Emphasis Type="Italic">N,N</Emphasis>′-di[(<Emphasis Type="Italic">E</Emphasis>)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide

Abstract  

A new bishydrazone compound, N,N′-di[(E)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide (1), has been prepared by condensation reaction of 2,6-naphthalenedicarbohydrazide with salicylaldehyde in ethanol, and characterized by elemental analysis, FT-IR, ¹H- and ¹³C-NMR, ESI–MS and single-crystal X-ray diffraction analysis. The crystal of 1·2DMF belongs to monoclinic, space group P2(1)/n with a = 10.454(1), b = 7.711(1), c = 18.801(2) ?, β = 93.364(1)°, V = 1512.9(3) ?³, Z = 2, D _c  = 1.314 g cm⁻³, μ = 0.093 mm⁻¹, F(000) = 632, Mr = 598.65, the final R ₁ = 0.0861 and wR ₂ = 0.2279 for 7243 observed reflections with I > 2σ(I). The structural analysis reveals that compound 1·2DMF contains one N,N′-di[(E)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide molecule and two N,N-dimethylformamide solvent molecules. A 2D supramolecular structure of 1·2DMF was constructed by multiple intermolecular N–H···O and C–H···O hydrogen bonds.     

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.      

Synthesis,Crystal Structures,and Antibacterial Activity of Two Hydrazone Derivatives 3-Methoxy-<Emphasis Type="Italic">N</Emphasis>′-(3,5-Dibromo-2-Hydroxybenzylidene)Benzohydrazide Methanol Solvate and 3-Methoxy-<Emphasis Type="Italic">N</Emphasis>′-(2,4-Diclorobenzylidene)Benzohydrazide

Abstract  

Two new hydrazone compounds with the formulae C₁₅H₁₂Br₂N₂O₃·CH₃OH (1) and C₁₅H₁₂Cl₂N₂O₂ (2), were prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray determination. Compound (1) crystallizes in the triclinic space group P-1 with unit cell dimensions a = 7.654(1) ?, b = 13.801(2) ?, c = 16.904(2) ?, α = 90.772(2)^o, β = 101.721(2)^o, γ = 95.891(2)^o, V = 1738.1(4) Ǻ³, Z = 4, R ₁ = 0.0495 and wR ₂ = 0.1161. Compound (2) crystallizes in the triclinic space group P-1 with unit cell dimensions a = 8.296(1) ?, b = 12.987(2) ?, c = 14.121(2) ?, α = 88.922(2)^o, β = 87.960(2)^o, γ = 84.130(2)^o, V = 1512.3(4) Ǻ³, Z = 4, R ₁ = 0.0526 and wR ₂ = 0.1220. The single crystal structure analysis indicates that compound (1) consists of two nearly coplanar hydrazone molecules and two methanol molecules which link to the hydrazone molecules through O–H···O hydrogen bonds, while compound (2) consists of two independent distorted hydrazone molecules. In the crystal structure of (1), adjacent two hydrazone molecules are linked with methanol molecules through intermolecular hydrogen bonds of O–H···O and N–H···O, forming a dimer. In the crystal structure of (2), molecules are linked through intermolecular N–H···O hydrogen bonds, forming chains running along the a axis.     

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.     

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.      

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 Structures of Trinuclear Chlorido(<Emphasis Type="Italic">N,N</Emphasis>′-diethylthiourea)copper(I) and a Second Polymorph of Iodidotris(<Emphasis Type="Italic">N,N</Emphasis>′-diethylthiourea)copper(I)

Abstract  

Reactions of N,N′-diethylthiourea (Detu) with copper(I) cyanide and copper(I) iodide in a 2:1 M ratio in acetonitrile resulted in the formation of [Cu(Detu)Cl]₃·(CH₃CN)_0.5 (1) and [Cu(Detu)₃I] (2), respectively. In compound 1 each copper atom is coordinated with one sulfur atom of Detu and with one chloride ion forming a centrosymmetric trinuclear core (Cu₃S₃Cl₃) that exhibits a Cu–Cu separation of 2.7383(5) Ǻ indicating the existence of cuprophilic interactions. Complex 2 crystallizes with two independent molecules per asymmetric unit. Each copper atom is coordinated with three sulfur atoms of Detu and with one iodide ion in a tetrahedral arrangement.