Crystal structure of penthylenediammonium pentachlorothallate(III)

The penthylenediammonium pentachlorothallate(III) salt is orthorhombic with the following unit cell dimensions: a = 7.696(3) Å, b = 13.2890(17) Å, and c = 13.503(18) Å, space group P2₁2₁2₁ with Z = 4. The structure was solved by Patterson methods and refined to a final R value of 0.0387 for 1991 observed reflections. The structure consists of penthylenediammonium cations and polynuclear anions in which slightly distorted [TlCl₆]^3– octahedral sharing two vertices are interconnected into chains. These chains are themselves interconnected by means of the N–HCl bonds originating from the [NH₃(CH₂)₅NH₃]²⁺ entities forming a three-dimensional network.     

Synthesis and Crystal Structure of 2-(2,3,4-Trimethoxy-6-Methylbenzylideneamino)phenol

Abstract  The title compound 2-(2,3,4-trimethoxy-6-methylbenzylideneamino)phenol (C₁₇H₁₉NO₄, M _r = 301.33) was synthesised and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 10.4458(14), b = 8.3870(10), c = 17.780(2) ?, β = 91.102(2)^°, V = 1557.4(3) ?³, Z = 4, D _c = 1.285 g/cm³, λ = 0.71073 ?, μ(Mo Kα) = 0.092 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0452, wR(F ²) = 0.1065 for 2,743 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the molecule adopts an E configuration at the C=N functional bond. The dihedral angle between the two phenyl rings is 38.3(3)°. The crystal structure is stabilized by C–H···O, O–H···O and O–H···N hydrogen bonds and π–π stacking interactions. Graphical Abstract  The title compound 2-(2,3,4-trimethoxy-6-methylbenzylideneamino)phenol (C₁₇H₁₉NO₄, M _r = 301.33) was synthesised and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 10.4458(14), b = 8.387(1), c = 17.780(2) ?, β = 91.102(2)°, V = 1557.4(3) ?³, Z = 4, D _c = 1.285 g/cm³, λ = 0.71073 ?, μ(Mo Kα) = 0.092 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0452, wR(F ²) = 0.1065 for 2,743 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the molecule adopts an E configuration at the C=N functional bond. The dihedral angle between the two phenyl rings is 38.3(3)°. The crystal structure is stabilized by C–H···O and O–H···O hydrogen bonds and π–π stacking interactions.      

Crystal structure of a macrocyclic tetraamine isocyanato zinc(II) complex

The complex, [Zn(L)(NCO)]Cl · 3H₂O (1) (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^1.18,0^7.12]docosane), has been synthesized and structurally characterized. 1 crystallizes in the monoclinic system, space group P2₁/n with a = 10.530(3), b = 9.315(2), c = 27.188(3) Å, = 92.58(1)°, V = 2664.1(9)ų, and Z = 4. The zinc atom is in a distorted squarepyramidal environment with the four nitrogen atoms of the macrocycle and one nitrogen atom of the isocyanate ligand.     

Crystal structure of a nickel(II) complex with macrocyclic tetraamine

A new compound [Ni(cyclen)(²-CH₃CO₂)]BF₄ (cyclen = 1,4,7,10-tetraazacyclodode- cane) has been synthesized and characterized structurally. It crystallizes in the orthorhombic system, space group Pnnm with a =12.045(5), b =14.906(6), c =8.913(4) Å, V =1600.4(12) ų, and Z =4. The nickel(II) ion has a distorted octahedral geometry with four secondary amines of the macrocycle and two oxygen atoms of the bidentate acetate group. TGA curve shows its thermal stability is up to 280°C.     

Crystal structure of tris (phenylammonium) chloride pentachloroantimonate (III) monohydrate

The tris (phenylammonium) chloride pentachloroantimonate (III) monohydrate salt is triclinic with the following cell parameters: a = 9.4283(3), b = 11.4482(3), c = 13.1748(3)Å, = 113.493(2), = 90.381(2), = 97.331(1)°, V = 1290.86(6)ų, with Z = 2 formula units. The structure consists of [C₆H₅NH₃]⁺ cations, water molecules, Cl^– anions, and SbCl₅ square pyramids. Hydrogen bonds, established through water molecule, link the anions [SbCl₅]^2– and Cl^– and make an infinite chain in the [011] direction. Chains are linked together via another hydrogen bond network originating from the ammonium groups. A distortion of the SbCl₅ square pyramid can be attributed to the stereo activity of the Sb(III) lone electron pair.     

Crystal structure of bis[dihydrobis(3,5-dimethy-1-pyrazolyl)borato]cadmium(II)

The structure of [H₂B(3,5-Me₂pz)₂]₂Cd shows the four nitrogen donor atoms form a pseudotetrahedral arrangement about the cadmium(II). The intraligand N—Cd—N angles are restricted to an average of 91.4° by the chelate rings forcing the interligand N—Cd—N bond angles to average 119.4°. The Cd—N bond distances average 2.21 Å with a range of 0.04 Å. The crystal is in the triclinic space group, P with a = 7.6793(2) Å, b = 8.5992(2) Å, c = 25.0874(4) Å, = 91.0791(2)°, = 97.9769(4)°, = 110.2344(6)°, and Z = 2.     

Crystal structure of [Pb(cis-anti-cis-dicyclohexyl-18-crown-6)(OH2)2][ClO4]2

[Pb(cis-anti-cis-dicyclohexyl-18-crown-6)(OH₂)₂][ClO₄]₂ was crystallized using a slightly modified literature method for the separation of dicyclohexyl-18-crown-6 isomers. It crystallizes in the monoclinic space groupP2₁/n witha=8.415(5),b=20.993(9),c=8.973(5) Å, β=111.56(6)^o, andD _calc=1.84 g/cm³ for Z=2. The Pb²⁺ ion resides on a crystallographic center of inversion and is coordinated to the six crown ether donors and two axial water molecules in a hexagonal bipyramidal geometry. The Pb-O(etheric) distances range from 2.694(4) to 2.743(4) Å while the Pb?OH₂ distance is 2.522(6) Å.     

Crystal structure of di(N-benzyl piperidinium) pentachloroantimonate(III) dihydrate

The salt di(N-benzyl piperidinium) pentachloroantimonate(III) dihydrate crystallizes in the orthorhombic system with space group Cmc2₁, the unit cell dimensions are: a = 29.383(1), b = 10.509(2), c = 9.941(1) Å, with Z = 8. The structure shows a layer arrangement perpendicular to the a axis: planes of SbCl₆ octahedra alternate with planes of [C₁₂H₁₇N]⁺ cations. The SbCl₆ octahedra are connected through a O(W)–HCl hydrogen bonds and a chlorine bridge, so that infinite unidimensional chains of composition [SbCl₅(H₂O)₂]^2n– _n are formed in the structure along the c direction. These chains are connected to [C₁₂H₁₇N]⁺ entities by N–HCl and N–HO(W) hydrogen bonds, forming a three-dimensional network. It was found that lengths of Sb–Cl bonds may differ from each other. The differences shown as a distortion of the SbCl₆ octahedra were attributed to the Sb(III) lone electron pair stereoactivity.     

Crystal structure of tetrakisdiphenylammonium hexadecachlorotetrabismuthate(III)

[(C₆H₅)₂NH₂]₄ ⁺[Bi₄Cl₁₆]^4– crystallizes in the triclinic space group witha=11.835(2),b=12.393(2),c=12.625(3)Å, =108.37(3), =108.69(3), =96.00(3)° andD _c=2.135 g cm^–3 forZ=1. The [Bi₄Cl₁₆]^4– anion is a centrosymmetric cluster of four distorted edge-sharing BiCl₆ octahedra. The ranges of the Bi–Cl bonds are 2.484(4)–2.606(3)Å for Bi–Cl(terminal), 2.691(3)–2.956(4)Å for Bi-Cl(µ₂), and 2.960(3)–3.120(4)Å for Bi-Cl(µ₃). The cations and anions are held in place by weak hydrogen bonds.     

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 a Mixed-Ligand Cobalt(II) Complex with 2-Aminobenzimidazole

Abstract  The cobalt(II) complex, [Co(abz)₂(SCN)₂] 1, has been synthesized by the reaction of cobalt(II) nitrate with ammonium thiocyanate and abz ligands (abz = 2-aminobenzimidazole), and was fully structurally characterized by elemental analysis, IR spectra, X-ray diffraction and thermogravimetric experiments. It crystallizes in the triclinic P-1 space group with a = 8.6316(10), b = 9.3426(10), c = 13.254(2) ?, α = 95.793(2), β = 95.870(2), γ = 115.7380(10), V = 945.1(2) ?³, and Z = 2. The central cobalt(II) atom is four-coordinated to nitrogen donors from two neutral abz ligands and two isothiocyanate anions respectively, adopting a slightly distorted tetrahedral geometry. In addition, the intermolecular N–H···N and N–H···S hydrogen bonds interactions link the discrete mononuclear units into infinite three-dimensional networks. Index Abstract  The essence sentence of the paper: In the mixed-ligand mononuclear complex, [Co(abz)₂(SCN)₂], the four coordinated cobalt(II) atom exhibits a slightly distort tetrahedron, which is further assembled into 3D infinite network by intermolecular hydrogen interactions.      

Crystal structure of Pt(S2COEt)2

The crystals of Pt(S₂COEt)₂ are orthorhombic, Pbca, with (at 20°C)a=7.799(3),b=7.368(6),c=20.588(7) Å.D _cale=2.46g cm^–3 forZ=4. The platinum atom resides on a crystallographic center of inversion and is bound to the four sulfur atoms of the xanthato ligand in a square planar geometry. The Pt–S distances are 2.313(6) and 2.320(7)Å with an intraligand S–Pt–S angle of 75.1(2)°.     

Crystal Structure of a Metallohybrid Acid of 1,3,5-Benzenetricarboxylic Acid of Copper(II)

Abstract The crystal structure of a metallohybrid carboxylic acid obtained from the reaction of 1,3,5-benzenetricarboxylic acid (TCAH3) with copper(II)acetate monohydrate in the presence of pyridine (py) having composition Cu(py)₂(TCAH2)₂(H₂O)₂ [1] is reported. It crystallizes in triclinic space group P-1 and with a = 7.0110(3)?, b = 8.9523(5)?, c = 11.5370(5) ?, α = 79.776(3) °, β = 82.881(3)°, γ = 83.628(3)°, and V = 704.18(6)?³. The hydrogen bond in 1 is compared with the hydrogen bond pattern in the structure of 1,3-dicarbomethoxy 4,6-benzenedicarboxylic acid, which crystallizes in mononclinic space group P21/c and has unit cell parameters of a = 6.9549(16)?, b = 8.7676(15)?, c = 20.111(4)?; β = 92.585(17) ° and V = 1225.1(4) ?³. Index Abstract Crystal structure of a metallohybrid carboxylic acid obtained from the reaction of 1,3,5-benzenetricarboxylic acid with copper(II)acetate monohydrate in the presence of pyridine is determined and compared with hydrogen bond pattern present in the structure of 1,3-dicarbomethoxy 4,6-benzenedicarboxylic acid. Crystal structure of a metallohybrid acid of 1,3,5-benzenetricarboxylic acid of copper(II). Kusum Bania, Nilotpal Barooah, Rupam Sarma, Jubaraj B. Baruah     

Crystal structure of a novel tertiary phosphine coordination complex: dichlorobis(tribenzylphosphine)nickel(II)

The title compound dichlorobis(tribenzylphosphine)nickel(II), Ni[P(CH₂C₆H₅)₃]₂Cl₂, belongs to a type of tertiary phosphine coordination complex, M(PR₃)₂X₂. There are two molecules in the unit cell which do not appear to interact chemically. Both molecules have a trans-square planar configuration with each nickel atom on a center of symmetry. Three benzyl groups are bonded to each phosphorus atom as rotors in a propeller, and the threefold axis is along the P—Ni bond, which has a mean length of 2.23(1) Å. Crystal data: C₄₂H₄₂Cl₂NiP₂, Triclinic, space group , a = 10.4892(15) b = 10.5249(12) c = 19.453(2) Å, = 83.872(8), = 76.839(9), = 62.241(8)°, V = 1850.5(4) ų, Z = 2. There is an intramolecular hydrogen bond between the C3 and C11 atoms.     

Crystal structure,thermal analysis,and IR spectroscopic investigation of bis(2-amino-6-methyl) pyridinium sulfate

Synthesis, crystal structure refinement, phase transitions studied by thermal analysis, and IR spectroscopic investigation of 2C₆H₉N₂ < eqid2 > ⋅SO₄²⁻ are reported. The title compound crystallizes in the monoclinic space group C2/c (no. 15) with a = 10.5068(4) Å, b = 10.2225(5) Å, c = 14.0422(7) Å, and β = 104.489(3)^∘. A crystal packing diagram shows layers built by all the components of the structure and centered by planes z = 1/4 and 3/4. The pyridine substituents stack forming channels parallel to the c direction with dimensions of 4.163(1) Å and 5.148(4) Å. Thermal analysis shows that the anhydrous compound possesses an irreversible weak phase transition.     

Crystal structure determination of (triethyleneglycol)bis(3,5-dinitrobenzoate) strontium(II) monohydrate

The complex {[Sr(C₇H₃N₂O₆)₂(C₆H₁₄O₄)]·H₂O}₂ is a centrosymmetric dimer. Each Sr^{2 +} in the cluster is nine coordinated by four oxygens of triethyleneglycol and the carboxylate oxygens of 3,5-dinitrobenzoate (DNB) anions. One of the DNBs behaves as a symmetrical bidentate chelating ligand whereas the other acts as a highly unsymmetrical, tridentate, chelating-cum-bridging ligand. The crystal is triclinic with a space group P1. The unit cell dimensions are a = 14.955(2), b = 12.730(2), c = 7.389(2) Å, = 73.06(1)°, = 99.56(1)°, = 80.02(2)° , V = 1289.84 ų, = 0.71070 Å, Z = 2. The centrosymmetrically related Sr^{2 +} is separated by a short distance of 4.565(1) Å, which results in a closely packed cluster of monomers. Both the alcoholic oxygens are H-bond donors toward the carboxylate oxygens of one of the DNB anion. The water molecule occupies intermolecular spaces.     

Crystal structure of the addition compound of [Ni(meso-cth)][Cr(ox)2(bpy)](H2O)(ClO4) with weak coordination bonds and hydrogen bonds

A new ionic complex [Ni(meso-cth)][Cr(ox)₂(bpy)](H₂O)(ClO₄) [meso-cth = meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane, ox = oxalato ainon, bpy = 2,2-bipyridine] was prepared and its structure was determined. The complex was found to crystallized in monoclinic space group P2(1)/n, with a = 13.6000(4) Å, b = 18.763(5) Å, c = 14.995(4) Å, =106.958(5)°, V = 3659.9(17) ų, and Z = 4. The structure consisted of cationic [Ni(meso-cth)]²⁺, anionic [Cr(ox)₂(bpy)]^–, and perchlorate anions; the cationic [Ni(meso-cth)]²⁺ and anionic [Cr(ox)₂(bpy)]^– units were related by weak coordination bonds and hydrogen bonds.     

Crystal and molecular structure of 6-0-acetylgrayanotoxin III

The crystal and molecular structure of a grayanotoxin III derivative, 6-0-acetylgrayanotoxin III is presented. The crystal is orthorhombic, space group P2₁2₁2₁, witha=15.582(3),b=21.304(3),c=6.339(3)Å,V=2104(1) ų Z=4. The structure was solved by direct methods and refined by full matrix least-squares methods to a finalR=0.047 for 1763 independent reflections withF ₀>3 (F ₀) The molecule is based on a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered ring with various conformations.     

Synthesis and crystal structure of a novel polymeric silver(I) complex

The complex of [Ag₂(μ–L)₂(μ–NO₃)₂]_n, where L?=?2–methyl–5–(2–pyridyl)–1,3,4–oxadiazole, has been synthesized and characterized by single–crystal X–ray diffraction analysis. The crystals are in triclinic system with space group P–1. Complex [Ag₂(μ–L)₂(μ–NO₃)₂]_n is a polymeric silver(I) complex bridged through the 1,3,4–oxadiazole rings and the nitrate ions, and the center Ag1(I) atoms have distorted trigonal bipyramidal geometries [AgN₃O₂].     

X-ray crystal structure of a macrocyclic tetraamine nitrito nickel(II) complex

The compound [Ni(L)(²-NO₂)]ClO₄ (L = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) has been synthesized and structurally characterized. It crystallizes in the monoclinic system, space group P2₁/c with a = 26.899(5), b = 8.476(2), c = 23.633(5) Å, = 115.12(13)°, V = 4878.6(17) ų, and Z = 4. Each nickel(II) ion has a six-coordinated bicapped square-pyramidal geometry with four secondary amines of the macrocycle and two oxygen atoms of the bidentate nitrito group. Electronic spectra and effective magnetic moment of the complex also exhibit a high-spin six-coordinated geometry.