Crystal structure of aminoguanidinium hexahydro-closo-hexaborate dihydrate, (CN4H7)2B6H6 · 2H2O

The (HAgu)₂B₆H₆ · 2H₂O compound was synthesized and its crystal structure was determined [R = 0.0385 for 2018 reflections with I > 2σ(I)]. The structure consists of HAgu ⁺ cations, centrosymmetric B₆H ₆ ^2? anions, and water molecules. The anions have an almost regular octahedral structure. The bond lengths and angles lie within the following narrow ranges: B-B, 1.715–1.726(2) Å; B-H, 1.08–1.14(2) Å; B-B-B, 59.72°–60.29(9)° and 89.63°–90.20(11)°; and B-B-H, 133.2°–137.0(9)°. The HAgu ⁺ cations and water molecules are involved in the O-H?O, N-H?O, and N-N?N hydrogen bonds and participate in numerous (N, O)-H?H-B specific interactions with the B₆H ₆ ^2? anions, which results in splitting and high-frequency shift of the band of B-H stretching vibrations in the IR spectrum.     

Synthesis,crystal structure and spectral studies of the complex [Ni(C3H4N2)4(H2O)2]·(C6H4COSO2N)2

The title compound has been synthesized and its crystal structure determined at room temperature.M _r =731.39, triclinic, space groupP¯1,a=9.020(3),b=11.280(7),c=7.784(2)Å,=97.05(4),=97.08(2), =105.32(4)°, U=748(1)ų,Z=1,D _calc.=1.624 g/cm³. The finalR is 0.030 for 3095 independent observed reflections withI3(I). The crystal structure consists of repeated [Ni(im)₄(H₂O)₂]²⁺ cations and noncoordinated saccharin anions. In the complex cation [Ni(im)₄(H₂O)₂]²⁺, Ni² is bonded to four N atoms from four imidazole molecules and two O atoms from two water molecules forming an approximately square octahedral stereochemistry. The d-d transition spectrum of the title compound is also reported and is explained perfectly with the scaling radial theory which was proposed by us.     

Crystal structure of dicesium thorium trisulfate dihydrate,Cs2Th(SO4)3·2H2O

Dicesium Di--sulfatosulphatobisaquothorate(IV), H₄O₁₄S₃Cs₂Th, (M _r =821.8) crystallized from water in the monoclinic space groupP2₁/c (No. 14), witha=6.415(2),b=15.95(1),c=13.078(8) Å,=90.88(4)°,V=1338(14) ų,Z=4,D _x =4.08 g cm^–3, MoK (=0.71069 Å),=195.8 cm^–1,F(000)=1407.3, room temperature, finalR=0.086 for 1699 unique observed reflexions. Two of the sulfate groups are tridentate (chelating and bridging) and the other is bidentate chelating. As the waters are both coordinated the thorium is 10-coordinate. It shows an unusual 2/4/2/2 geometry.     

Structure,magnetic and IR studies of copper(II) diphenylphosphate dihydrate,Cu(DPhP)2·(H2O)2

The title compound has been synthesized, and characterized by means of X-ray, magnetic, and IR-spectroscopic measurements.The crystals of Cu(DPhP)₂(H₂O)₂(DPhP=diphenylphosphate) are monoclinic, space groupI2/c witha=24.126(6),b=8.510(2),c=12.333(3) Å,=90.73(5)° andZ=4. The structure was solved by the heavy-atom technique, and refined by full-matrix least-squares calculations to a finalR of 0.040 for 1494 reflections.The complex is centrosymmetric, and the Cu atom at a center of symmetry is four-fold coordinated with two oxygen atoms from two phosphate groups and two water molecules. The coordination about the Cu atom is square-planar, with Cu-O and Cu-O(W) distances 1.926(3) and 1.912(3) Å, respectively.The O(2) phosphate oxygen is an acceptor of two H bonds; one of them is an intramolecular O(W)-H(2)O(2) of 2.714(4) Å, and the other is an intermolecularO(W)-H(1)O(2ⁱ) of 2.667(4) Å. Their presence is also deduced from the IR spectrum of this compound at 3250 and 3000 cm^–1, respectively.The calculated magnetic moment value of 1.92 B.M. corresponds to that of the monomeric copper(II) complexes including those of some alkyl phosphates.     

Synthesis, crystal structure, and thermal analyses of triaqua-(1,10-phenanthroline-N,N′) succinatomanganese(II) dihydrate, [Mn(H2O)3(phen)(C4H4O4)]·2H2O

[Mn(H₂O)₃(phen)(C₄H₄O₄)]·2H₂O was obtained by reaction of freshly prepared MnCO₃, phen and succinic acid in CH₃OH/H₂O (1:1 v/v), and its crystal structure has been determined by single crystal X-ray diffraction methods. The title mixed ligand complex crystallizes in the triclinic space group with cell dimensions a = 7.590(1) Å, b = 9.324(1) Å, c = 13.917(1) Å, = 85.64(1)°, = 74.56(1)°, = 77.10(1)°, and D _calc = 1.584 g/cm³ for Z = 2. The crystal structure consists of the [Mn(H₂O)₃(phen)(C₄H₄O₄)] complex molecules and lattice H₂O molecules. The Mn atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of three H₂O molecules and one succinato ligand with d(Mn—N) = 2.271 and 2.299 Å, and d(Mn—O) = 2.133–2.239 Å. Through intermolecular hydrogen bondings, the complex molecules are interlinked to form 2D layers, which are assembled by – stacking interactions into 3D framework with tunnels occupied by the lattice H₂O molecules. Thermal analyses showed that the title compound decomposes in two steps over the range 25–600°C upon heating in flowing Ar.     

Crystal and molecular structure of bis(o-phenylenethiourea)selenium(II)chloride dihydrate,C14H12N4S2Cl2Se·2H2O

The synthesis and crystal structure ofbis(o-phenylenethiourea)selenium(II)-chloride dihydrate, Se(C₇H₆N₂S)₂Cl₂·2H₂O are reported. The compound crystallizes in the monoclinic space group, P2₁/n, with four molecules per unit cell, the dimensions of which area=10.243(3),b=13.341(4),c=14.273(4) Å,=93.00(3)°,U=1947.76 ų. The structure was solved by direct methods and refined by full-matrix least-squares toR=0.039 andR _w =0.040 for 3314 unique reflections. Selenium displays two strong coordinations arising from the two sulfurs, Se-S(1)=2.191(1), Se-S(2)=2.206(1) Å, and S(1)-Se-S(2)=101.0(1)°, and four secondary interactions involving three chlorines and one sulfur. The complex occurs as a dimer with two sets of very weakly interacting bridging pairs S(2), S(2)^a; and Cl(2), Cl(2)^a, where a denotes the inversion related atom. Lattice stabilization is ensured by the extensive network of hydrogen bonds involving chlorines, water oxygens, and nitrogens of phenylenethiourea ligands.     

Crystal structure of aqua[S-prolinato-N-monoacetato)copper(II) dihydrate [Cu(Proma)H2O] ⋅ 2H2O

The crystal structure of [Cu(C₇H₉NO₄)H₂O] ? 2H₂O is determined by X-ray diffraction (λMo, R = 0.0316 for 857 reflections). The crystals are tetragonal, a = 8.219(1) Å, c = 17.449(3) Å, Z = 4, ρ_calcd = 1.627 g cm^?3, and space group P4₃. The coordination polyhedron of the Cu atom is a tetragonal pyramid with the O atom of the acetate arm of the prolinatomonoacetate ion (Proma) in the apical position [Cu-O 2.312(6) Å]. The O atom of the water molecule and the N and O atoms of the prolinate group of the Proma ligand lie in the basal plane. The Cu-N bond length is 2.044(6) Å, and the Cu-O bond lengths are 1.932(7) and 1.927(6) Å. The O atom of the acetate arm of the neighboring Proma ion completes the basal plane [Cu-O 1.951(6) Å], thus linking the copper complexes into infinite chains.     

Molecular structure and hydrogen bonding of 4-dimethylaminopyridinioacetate in its crystalline dihydrate and hydrochloride trihydrate,L·2H2O and [L2H]Cl·3H2O (L=p-Me2NC5H4N+CH2CO2 −)

The crystalline dihydrate and hydrochloride trihydrate of a new betaine, namely, L·2H₂O (1) and [L₂H]Cl·3H₂O(2) (L=p-Me₂NC₅H₄N⁺CH₂CO₂), have been synthesized and characterized by X-ray crystallography. Molecule L in compound1 [space groupPbcn, witha=15.732(3),b=7.894(2),c=18.304(4) Å, andZ=8] possesses approximateC _s symmetry. The formation of hydrogen bonds by water molecules bridging neighboring carboxy oxygen atoms leads to an infinite two-dimensional network composed of a packing of two different kinds of 12-membered rings. In compound2 [space group PT witha=7.341(2),b=9.543(2),c=17.010(4) Å, =82.43(2)°, =80.34(2)°, =74.05(2)°, andZ=2], the carboxylate groups of a pair of betaine molecules are bridged by a proton to form a dimeric cation L₂H⁺ with a very strong asymmetric hydrogen bond of length 2.464(7) Å. The crystal structure features a hydrogen-bonded corrugated ribbon comprising an alternate arrangement of edge-sharing centrosymmetric (H₂O)₄(Cl^–)₂ and (H₂O)₄ rings running parallel to thea axis.     

A comparison of the crystal structures of (dabcoH2)CuCl4 and (dabcoH2)CuCl4⋅H2O

The crystal structures of the anhydrous and monohydrated (dabcoH₂)CuCl₄nH₂O salts (n = 0,1) have been determined and a comparison of their crystal structures has been reported. The anhydrous salt is monoclinic P2₁/c with a = 9.045(2) Å, b = 6.9270(10) Å, c = 18.767(4) Å and = 90.07(3)° with V = 1175.8(4) ų. The hydrated salt is also monoclinic P2₁/c with a = 9.266(2) Å, b = 9.395(2) Å, c = 14.386(3) Å and = 93.32(3)° with V = 1250.3(5) ų. The structures of the two salts are closely related. Both compounds contain isolated distorted (compressed) tetrahedral CuCl₄ ^2– anions, diprotonated dabco cations, and in the case of the hydrated salt, lattice H₂O molecules. In the anhydrous salt, each of the two N–H⁺ groups of the dabcoH₂ ²⁺ dications form bifurcated hydrogen bonds to chloride ions on adjacent CuCl₄ ^2– anions along the c axis, thus forming chains running parallel to the c axis. In the hydrated salt, a water molecule is inserted into one of the pair of bifurcated hydrogen bonds, forming instead N–H O–H CuCl₄ ^2– linkages. The chains thus formed are cross-linked by O–H Cl hydrogen bonds between the chains. Because of this additional hydrogen bonding, the CuCl₄ ^2– anions in the hydrated salt are distorted further from tetrahedral geometry.     

Synthesis, crystal structure, and thermal property of a novel supramolecular assembly: (NH4)2(C8H10N4O2)4 [H4V10O28]·2H2O, constructed from decavanadate and caffeine

A novel 3D supramolecular assembly constructed from decavanadate and caffeine building blocks, (NH₄)₂(C₈H₁₀N₄O₂)₄[H₄V₁₀O₂₈]·2H₂O (1), has been synthesized in aqueous solution and characterized by elemental analysis, IR, ¹H NMR, ⁵¹V NMR, TG-DTA, and single crystal X-Ray diffraction. The compound 1 crystallizes in monoclinic system, space groupP2 ₁/n, a = 15.801(1) Å, b = 12.914(1) Å, c = 15.913(2) Å, = 113.55°,V = 2976.4 (5)ų, Z = 2, R = 0.0498 with 6818 reflections. Water molecules, ammonium ions, and caffeine act as cement linking the polyanions into 1D chain along the c-axis by hydrogen bonding. In compound 1, extensive hydrogen-bond contacts and strong – interactions lead to an ordered 3D supramolecular framework. TG-DTA curves indicate that the weight loss of the complex can be divided into three stages.     

Structure of a Cu(II)-containing peptide,diaquo-gly-l-tyr Cu(II) dihydrate, [Cu(C11N2O4H13)(H2O)2·2H2O

The structure of the Cu(II) complex of gly-l-tyr [Cu(C₁₁N₂O₄H₁₃) (H₂O)₂]·2H₂O has been solved by X-ray diffraction methods. The compound crystallizes in the orthorhombic space groupP2₁2₁2₁ witha=11.970(2) Å,b=12.485(2) Å andc=10.418(3) Å, respectively, (MoK)=0.710 Å,D _c =1.59 Mgm^–3,D _m =1.59 Mgm^–3, finalR=0.04. The structure was solved by heavy atom (Cu) phased Fourier and refined by full-matrix least squares methods. The coordination geometry of the ligand around the Cu(II) ion has been established as a distorted tetragonal pyramid. The peptide molecule behaves as a tridentate ligand via its amino (N2), amido (N1) nitrogens and carboxyl (O2) oxygens. The peptide nitrogen is found to be deprotonated.     

Crystal and molecular structure of di-μ-chlorobis[2-[[[(2-hydroxy-1-naphthyl)methyl]-imino]ethanolato]N,O,O′]di-copper(II) dihydrate

The crystal structure of the title compound has been determined from three-dimensional, single crystal X-ray diffraction data. [Cu₂Cl₂(C₁₃H₁₂NO₂)₂]·2H₂O crystallizes in the orthorhombic space group P2₁2₁2₁ with lattice constants,a=11.866(2),b=13.555(3),c=17.380(3) Å. Final full-matrix least-squares refinement of 3735 unique reflections yieldedR=0.054. The structure consists of dimeric C₂₆H₂₄Cl₂Cu₂N₂O₄ molecules and water molecules connected with the dimeric molecules by a hydrogen bond system. Both of the copper(II) centers are five-coordinated by twotrans oxygen atoms and one nitrogen atom from one ligand molecule and two chloride ions. The geometry at each copper(II) center is best described as distorted tetragonal pyramidal. The apical Cu1–Cl2 and Cu2–C11 distances are 2.747(2) and 2.938(3)Å, respectively. The Cu...Cu separation is 3.496(1)Å. The comparison with previously reported crystal structure of [Cu₂Cl₂ (C₁₃H₁₂NO₂)₂]·1/2H₂O is given.     

Crystal structure of triaquamaleatostrontium(II) monohydrate, [Sr(C4H2O4)(OH2)3]·H2O

[Sr(C₄H₂O₄)(OH₂)₃]·H₂O is monoclinic, P2₁/n, witha=11.476(2),b=7.027(1),c=12.344(2) Å, =115.74(3)°,V=896.67 ų,Z=4. The Sr atom is surrounded by nine oxygen atoms which come from four different maleate anions and three water molecules. The Sr–O distances range from 2.546(2) to 2.808(2) Å. The C–O distances are equal within the standard deviation 1.263(3) to 1.258(3) Å). In the maleate anion, the planes that contain the carboxylate groups form an angle of 74.44(9)°. Both carboxylate groups deviate significantly from planarity. The different coordination modes of the carboxylate group and the extensive hydrogen bonding present are responsible for the polymeric nature of the structure.     

Structure of the first homoleptic manganese–phosphine complex, [Mn(Me2PC2H4PMe2)3][BF4]

The crystal structure of the first homoleptic manganese–phosphine complex, [Mn(Me₂ PC₂H₄PMe₂)₃][BF₄], has been determined. This complex, previously synthesized as a PF₆ salt characterized only by NMR spectroscopy, is a by-product of reaction of MnH₃(Me₂PC₂H₄PMe₂)₂ with [Ag(CH₃CN)₄][BF₄]. It crystallizes in the trigonal system, space group P31c and Z = 2. The structure shows 3 chelating diphosphine ligands coordinating to the central manganese cation in octahedral fashion. The Mn—P distances are essentially equivalent within 3: each diphosphine has Mn—P = 2.283(3) and 2.290(3) Å, where the short and long distances are trans to each other. The bite angle for each diphosphine is 83.57(9)°, Lattice parameters: a = 9.954(2) Å, b =9.954(2) Å, c = 16.416(2) Å. Unit cell volume: 1408.6(4) ų.     

The properties,crystal, and molecular structure of catena-[(μ-acetato-) (μ-phthalazine)silver(I)dihydrate]: {[Ag(μ-O2CCH3) (μ-PHZ) (H2O)2]2}n

The crystal and molecular structure of catena-[(-acetato) (-phthalazine)-silver(I)dihydrate], {[Ag(O₂CCH₃) (C₈H₆N₂)(H₂O)₂]₂}_n, has been determined by single crystal X-ray analysis: the space group is P2₁/n,a=16.150(8) Å,b=3.886(5) Å,c=18.716(9) Å, =96.02(5)°,V=1168 ų. Phthalazine (PHZ) bridges the silver atoms to form {Ag--PHZ]₂ dimeric subunits. These dimeric subunits are planar and stack by bridging acetates to form a polymeric lattice. The acetates also form an asymrnetric chelate ring with the silver atoms which result in a distorted, square pyramidal configuration. The complex is further characterized by its IR and thermal properties.     

Crystal and molecular structure of [Cu2(3,5-dihydroxybenzoate)4 (acetonitrile)2] ⋅ 8H2O

The crystal and molecular structure of the title compound, [Cu₂(3,5-dihydroxybenzoate)₄ (acetonitrile)₂] 8H₂O 1, is reported. Crystal data for 1: tetragonal, space group I 4/m, a = 11.720(2) Å, c = 15.304(3) Å, V = 2102.4(6), and D _c = 1.53 g/cm³, for Z = 2. The metal and organic components crystallize to form a Cu paddle-wheel complex, of idealized D_4h symmetry, that assembles in the solid-state, along with eight equivalents of water, to form a 3D hydrogen-bonded network held together by O–H O hydrogens bonds. The metal complexes pack to form a 2D layered structure.     

Synthesis,Structure, and Properties of the Tris(ethylendiamine)nickel(II) Dichloride Dihydrate [Ni(H2NCH2CH2NH2)3]Cl2 ⋅ 2H2O Crystals

Crystallography Reports - The conditions for synthesis of [Ni(H2NCH2CH2NH2)3]Cl2 ⋅ 2H2O ([Ni(en)3]Cl2 ⋅ 2H2O) crystals from aqueous solutions have been considered. The synthesized...     

Interferometric study of the growth kinetics of K2Co(SO4)2 · 6H2O and K2Ni(SO4)2 · 6H2O crystals

Crystallography Reports - The growth kinetics of the (001) and (110) faces of K2Co(SO4)2 · 6H2O and K2Ni(SO4)2 · 6H2O crystals in the kinetic mode has been in situ investigated for the...     

Crystal and molecular structure of complex compound [Fe3O(CH3COO)6(H2O)3]2[ZnCl4] ⋅ 2H2O

The X-ray crystal structure of trinuclear iron acetate [Fe₃O(CH₃COO)₆(H₂O)₃]₂ [ZnCl₄] ? 2H₂O was determined. The crystal has a ionic structure. It is monoclinic, a = 25.363(7), b = 14.533(4), c = 15.692(4) Å, β = 103.11(2)°, space group _C2/c, and R = 0.0685. The structure of the cationic complex [Fe₃O(CH₃COO)₆(H₂O)₃]⁺ is typical of trinuclear iron(III) compounds containing a μ₃-O bridge: the iron atoms are situated at the vertices of an almost equilateral triangle with the O atom at the center. Each Fe atom is coordinated by four O atoms of bridging carboxy groups, the μ₃-bridging O atom, and the water molecule in the trans position to the latter O atom. Mössbauer spectroscopy evidence indicates the high-spin state (_S = 5/2) of the iron(III) ions.     

Structure and conformation of the monohydrate of N-t-boctyrosyl-proline (Boc-Tyr-Pro·H2O)

The structure and conformation of the monohydrate of N-t-boc-tyrosyl-proline (Boc-Tyr-Pro·H₂O) (C₁₉H₂₆O₆N₂·H₂O) has been investigated with X-ray crystallographic and spectroscopic methods. Boc-Tyr-Pro crystallized in an extendedtrans conformation in the space group P2₁2₁2₁ with cell dimensionsa=8.566(1),b=9.996(1),c=24.734(1). The conformation of Boc-Tyr-Pro reflex -helix type prolines. Three intermolecular hydrogen bonds are observed. Crystal water is involved in two hydrogen bonds (to the hydroxyl group of the C-terminal of the proline residue; to the carbonyl group of the t-Boc functionality) while the hydroxyl group of the tyrosyl residue (to the carbonyl group of the amide bond) is involved in one hydrogen bond. The puckering mode of the pyrrolidine ring of the proline residue is similar to what has been previously observed for other proline-containing peptides.Cis-trans isomerism is observed in the NMR spectra of Boc-Tyr-Pro with a predominance for the extended side chain for the tyrosyl residue.