Crystal structure of calcium adipate monohydrate

The crystal structure of calcium adipate monohydrate, Ca(C₆H₈O₄)·H₂O, has been determined by single crystal X-ray diffraction study. The crystals are triclinic witha=5.8990(3),b=6.7985(5),c=10.8212(6)Å,=78.999(5),=81.831(5), and =82.971(5)°, space group P¯1,Z=2,V=419.65(8)ų,d _m=1.59,d _c=1.600 Mg m^–3. The structure was refined by full-matrix least-squares techniques toR=0.040,R _w=0.058 for 1283 reflections withI3(I). Ca is coordinated to seven oxygen atoms and the coordination polyhedron is best described as pentagonal bipyramid. The coordinations of the two carboxylate groups in adipate ion are quite different. One carboxylate group binds three different Ca ions forming a four-membered chelate ring with one Ca ion and unidentate bridge bonds to two other Ca ions. The other carboxylate group links to two Ca ions through unidentate bonds. The structure is highly polymeric, but with a layertype structure parallel to (001) with the hydrocarbon chains sandwiched between the polar regions consisting of Ca, carboxylate and water molecules.Certain commercial materials and equipment are identified in this paper to specify the experimental procedure. In no instance does such identification imply recommendation or endorsement by the National Institute of Standards and Technology or the ADA Health Foundation or that the material or equipment identified is necessarily the best available for the purpose.     

Synthesis,crystal and molecular structure and vibrational characterization of N,N-dimethyl-oxathioamidate monohydrate

The title compound (SO₂NC₄H₆) has been prepared and characterized by X-ray diffraction and infra-red and Raman spectra. The structure has been refined using single-crystal X-ray diffraction data measured at 295K [MoK-radiation with =0.71073 Å]. The crystals are monoclinic, space groupP2₁/n,Z=4,a=6.240(2),b=6.786(2),c=19.988(1)Å, =108.47(2)°,V=802.8(7)ų.D _calc.=1.566 Mg m^–3,F(000)=392, =8.582 cm^–1. The final agreement factors for 1906 observed refections [I>3(I)] were:R=0.030 andR _w=0.043. The dihedral angle between de C–C–S–N plane and the C–C–O–O plane is 88.31(4). The potassium atom within the title compound structure has a slightly distorted trigonal bipyramidal coordination. Infrared and Raman spectra of the normal CH₃/CD₃ and H₂O/D₂O isotopes and the waterfree compounds at different temperatures made it possible to perform isotopes complete vibrational analysis and clearly shows the very special hydrogen bonded water molecule in the crystal.     

Synthesis and structure of 4,7,13,16-tetraoxa-1,10-diaza-5,6-benzocyclooctadeca-11,18-dione monohydrate

4,7,13,16-tetraoxa-1,10-diaza-5,6-benzocyclooctadeca-11,18-dione, C₁₆H₂₂N₂O₆·H₂O, (3) was synthesized under thermal conditions, starting from ,-diamine (1) and ,-diester (2). The hydrate of compound (3) was investigated in the solid state by X-ray structural analysis. Crystal data: monoclinic system, space group P2₁/c,a=12.342(4) Å,b=15.978(7) Å,c=8.960(3) Å, =96.72(3)°,Z=4. The structure was solved by direct methods and refined to finalR=0.056,R _w=0.069 for 1962 observed reflections. The structure exhibits internal hydrogen bonds between the etheral O(16) atom and the neighboring amide group. The water molecule connects diamide molecules by one strong hydrogen bond with carbonyl oxygen, and four weak hydrogen bonds with the amide groups and etheral oxygen atoms.     

Crystal structure and spectroscopy of a new dmg2−-bridged dinuclear cobalt(III) compound

A new dinuclear complex of formula [Co₂(dien)₂(dmg)₂](ClO₄)₂4.5H₂O (dien = diethlyenetriamine, dmg^2– = dianion of dimethylglyoxime) has been synthesized and characterized by single crystal X-ray diffraction analysis. It crystallizes in the monoclinic space group c2/c, with a = 20.868(7) Å, b = 11.408(4) Å, c = 15.816(4) Å, = 116.97(2), V = 3355.8(17) ų, Z = 4, F(000) = 1732. The structure consists of a dmg^2–-bridged Co(III) dimer. The coordination environments of two Co(III) ions are identical. Each cobalt(III) ion is coordinated by five nitrogen of one dien molecule and one dmg^2– ligand, and the coordination sphere is completed by an oxygen atom of the bridging dmg^2–. The compound is characterized by means of room temperature magnetic susceptibility measurement and infrared spectroscopy.     

Synthesis and crystal structure of trans-bis(O, O′-diisopropylthiophosphoryl-1H-imidazole-N3) bis(O,O′-diisopropyldithiophosphato) nickel(II) complex: Ni[N3-ImSP(OiPr)2]2[S2P(OiPr)2]2 (Im = imidazole; iPr = isopropyl)

The mononuclear complex, Ni[N³-ImSP(OiPr)₂]₂[S₂P(OiPr)₂]₂ (Im = imidazole; iPr = isopropyl), was unexpectedly obtained in a reaction of bis(O,O-diisopropyl-dithiophosphato) nickel(II) complex with imidazole ligand, and its structure was determined by X-ray crystallography. It crystallizes in the triclinic system, space group P , with lattice parameters a = 12.437(3) Å, b = 13.181(3) Å, c = 8.4580(17) Å, = 93.16(3)°, = 101.93(3)°, = 65.26(3)°, and Z = 1. The Ni atom has almost perfect octahedral coordination geometry and is coordinated by two N atoms of imidazole from two O,O-diisopropylthiophosphoryl-1H-imidazole ligands in axial positions and four S atoms from two (O,O-diisopropyldithiophosphato) anions which act as bidentate ligands forming a four-membered chelate ring in the equatorial plane. The Ni—S bond distances are 2.469(1) and 2.507(1) Å, and the Ni—N bond distances are 2.097(2) Å. The IR spectra data are in agreement with the structural data.     

Molecular structure ofrac-(4R*,4aS*,10aS*)-4-nitro-1,2,3,4,4a,9,10,10a-octahydrophenanthren-4a-ol,an unusual by-product of nitration of a crude 9,10-dihydrophenanthrene

A new nitro-octahydrophenanthrenol has been isolated by nitration of a crude 9,10-dihydrophenanthrene, which was identified by nmr and X-ray diffraction analysis. Crystallographic and molecular structure confirmed the compound as therac-(4R^*,4aS^*,10aS^*)-4-Nitro-1,2,3,4,4a,9,10,10a-octahydrophenanthren-4a-ol. The crystal was triclinic, ,a=10.549(3),b=8.530(3),c=7.131(1)Å, =107.07(3), =91.62(3), =96.27(4)°. Cyclohexane and cyclohexene rings aretrans-fused and have chair and half-chair conformations, respectively. The molecules are associated by hydrogen bridge between the hydroxyl oxygen and both nitro oxygens.     

Preparation,spectral studies and X-ray crystal structure of 1,3,5-triphenyl-1,5-pentanedione,C23H20O2

1,3,5-triphenyl-1,5-pentanedione, C₂₃H₂₀O₂, has been prepared and characterized by spectroscopic methods and single crystal X-ray analysis. Crystals are monoclinic, space groupP2₁/n, a=28.124(4),b=5.997(1),c=10.434(1)Å, -98.42(1)Å,Z=4. The structure has been refined to a finalR-value of 0.040 for 1625 reflections withF _o>3(F _o). The compound contains the two carbonyl groups in a mutuallycis arrangement.     

Redetermination of the crystal structure of [Na4(H2O)14]SnS4: a compound containing a novel chain of aquated sodium ions

[Na₄(H₂O)₁₄]SnS₄ is obtained by the reaction of Na₂S·9H₂O with SnCl₄·5H₂O in aqueous solution at 21°C. It crystallizes in the space group Cc with a = 8.621(2) Å, b = 23.543(5) Å, c = 11.358(2) Å, = 110.58(3)° and V = 2158.2 ų with Z = 2. Refinement of 3826 unique reflections from a racemically twinned crystal yielded a final value of R₁ = 0.0464 (|F| > 4) and wR₂ = 0.104 and a goodness of fit of 1.125. The structure consists of a Na⁺/H₂O network supporting the tetrahedral SnS₄ ^4– anions. Water molecules or sulfide ions octahedrally coordinate each of the four crystallographically independent Na⁺ ions. The dominant feature of the structure is the existence of zigzag chains of edgeshared Na octahedra. These chains are tied together into a three-dimensional network by bridging Na(H₂O)₆ octahedra and individual H₂O molecules.     

Molecular structure of isopropyl 1-phenyl-4-phenylhydrazono-5-oxo-3-pyrazolecarboxylate

The new azopyrazolone dye has been synthesized and its crystal structure has been investigated. Crystals of C₁₉H₁₈N₄O₃ are triclinic: ,a=7.484(1),b=10.646 (1),c=11.897(1) Å, =82.28(1), =72.86(1), =86.83(1)°,Z=2. The structure has been solved by direct methods and refined by full-matrix least-squares techniques toR=0.050 for 2622 unique reflections. The tautomeric form of the molecules has been determined as a hydrazo form. Delocalization of the C5=O3 and C4=N3 -electrons and delocalization of the lone-pair electrons of N1, N3, and N4 atoms has been observed. The intramolecular N–H...O hydrogen bond forms the six-membered ring C₂N₂H...O condensed with the pyrazolone ring. The molecules are connected by intramolecular C–H...O hydrogen bonds.     

Crystal structure oftrans-tetrachlorobis[2-(2-1H-imidazolyl)-1H-imidazolium]cadmium(II), [Cd(H3biim)2Cl4]

The reaction between cadmium(II) chloride and 2,2'-bi-1H-imidazole (H₂biim) in an acidic solution affords [Cd(H₃biim)₂Cl₄] (H₃biim=2-(2-1H-imidazolyl)-1H-imidazolium) in 63% yield. The compound crystallizes in the triclinic space groupP1, wherea=8.072(2),b=8.100(2),c=8.593(2) Å, =75.89(2), =62.94(2), =63.29(1)°,V=446.4(2) ų, andZ=1. The central Cd atom exhibits an octahedral geometry composed of a Cl₄N₂ core. The Cd-N bond distance is 2.392(2) Å. Cd–Cl distances are 2.5919(9) and 2.671(1) Å.     

The crystal and molecular structure of bis(melamine)silver(I) perchlorate, Ag(C3H6N6)2ClO4

The crystal structure of the title compound, Ag(mela)₂ClO₄ (mela = melamine), has been investigated by X-ray diffraction techniques, the crystals are triclinic, space group P1¯, with a = 5.236(2), b = 7.5385(9) c = 19.063(3) Å, = 99.91(1), = 90.53(2), = 108.32(2)° and Z = 2. The Ag atom has a coordination geometry with two strong bonds (2.162(2) and 2.179(4) Å) to the nitrogen of the melamines and two weak bonds (2.776(4) and 2.785(4) Å) to oxygen atoms of the ClO^– ₄anions. The N—Ag—N vector is markedly nonlinear (angle at Ag 167.7(2)°).     

Properties and structural characterization of a complex salt, 2[C12H18N4OS]·[Sb2Cl10], obtained by the reaction of thiamine (vitamin B1) with antimony trichloride

Thiamine hydrochloride (vitamin B₁) reacts with antimony trichloride in methanol to produce a crystalline compound which has been characterized as the salt 2[C₁₂H₁₈N₄OS]·[Sb₂Cl₁₀] by X-ray crystallography. The compound crystallizes in the triclinic space group ,b=11.029(2),c=12.234(2) Å, =108.75(2), =102.67(2), =103.59(2)°,U=1041.52 ų,D _c=1.80 g cm^–3,Z=1. The crystal structure consists of discrete [C₁₂H₁₈N₄OS]²⁺ cations and chloro bridged [Cl₄Sb(-Cl)₂SbCl₄]^4- anions in 2:1 ratio, held together by hydrogen bonds and electrostatic forces.     

Synthesis and structure of (H2O·HBF4)2(18-crown-6)

The title compound has been prepared by the addition of fluoroboric acid to 18-crown-6 in toluene. The compound crystallizes in the triclinic space group P¯1 witha=7.341(2),b=8.364(2),c=10.631(3)Å,=71.48(2),=67.91(2), =67.94(2)°, andD _c =1.44 g cm^–3 forZ=1. The final conventionalR value was 0.079 based on 1575 observed reflections. The molecule resides on a center of inversion. The (H₂O·HBF₄) moieties are best viewed as fluoroboric acid monohydrate molecules hydrogen bonded to the crown ether, one above and one below the plane of the crown. The FO(water) hydrogen bond separation is 2.474(5)Å, and the O(crown)O(water) separations are 2.834(5) and 2.841(6) Å. The oxygen atoms of the crown ether are planar to 0.23 Å.     

Caging the mercurous ion: a tetradentate tripodal nitrogen ligand enhances stability and J(1H199Hg)

The dimeric mercurous ion has been encapsulated by a pair of the tetradentate tripodal nitrogen ligands tris[(2-(6-methylpyridyl))methyl]amine (TLA). The complex [Hg₂(TLA)₂](ClO₄)₂ (1) was isolated directly from an acetonitrile solution of Hg(ClO₄)₂ 3H₂O and TLA. Complex 1 crystallizes in the triclinic space group with a = 10.537(2) Å, b = 10.751(2) Å, c = 10.907(2) Å, = 75.20(3), = 73.73(3), = 75.73(3), and Z = 1. The cation is located an inversion center. The Hg–Hg and Hg–N_amine bond distances are 2.5469(8) and 2.297(6) Å, respectively, and the average Hg–N_pyridyl bond length is 2.75(7) Å. Complex 1 was stable indefinitely in acetonitrile-d ₃ solution, permitting detection of 13 and 22 Hz heteronuclear couplings between the Hg(I) ions and the methylene protons of the ligand. Comparisons with the structures and spectroscopic properties of related mercuric and mercurous complexes are made.     

Identification of a new family of diphosphate compounds, AI2BII3(P2O7)2: Structures of Ag2Co3(P2O7)2, Ag2Mn3(P2O7)2, and Na2Cd3(P2O7)2

Syntheses and single-crystal X-ray structural results are reported for three new mixed diphosphates of the family A^I ₂B^II ₃(P₂O₇)₂; Ag₂Co₃(P₂O₇)₂ (I), Ag₂Mn₃(P₂O₇)₂ (II), and Na₂Cd₃(P₂O₇)₂ (III). All crystallize in the triclinic system, space group P1 bar: (I) a = 5.351(4), b = 6.375(4), c = 16.532(4) Å, = 80.83(6) = 81.45(4), = 72.87(5)°, V = 528.9(6) ų, Z = 2, D _calc = 4.649 mg/m³, R/Rw = 0.0428/0.0548 for 3949 obs. reflns; (II) a = 5.432(7), b = 6.619(6), c = 16.51(3) Å, = 80.78(8) = 82.43(9), = 72.82(7)°, V = 557.7(13) ų, Z = 2, D _calc = 4.338 mg/m³, R/Rw = 0.0679/0.1303 for 2100 obs. reflns and (III) a = 5.67(3), b = 7.08(4), c = 7.90(4) Å, = 77.0(2), = 82.5(2), = 67.8(2)°, V = 286(3) ų, Z = 2, D _calc = 4.249 mg/m³, R/Rw = 0.0307/0.0342 for 1945 obs. reflns. (I) and (II) are isostructural but (III) is of a different type. All three structures are characterized by layers of P₂O₇ groups alternating with layers of mixed metal atoms. Differences are seen in the conglomerate bonding patterns of B atoms and in the irregular geometry of Ag in (I) and (II) compared to the octahedral bonding seen for Na in (III). The differences in structure may be understood in terms of the ratios of the ionic radii of A and B atoms.     

Bis(triphenylphosphoranylidene)ammonium tetraethylborate, (Ph3P)32N+BEt34-: preparation and structure

The compound (Ph₃P)₃2N,⁺BEt₄ ^- is readily prepared from (Ph₃P)₂N⁺Cl^– and LiBHEt₃. The NMR spectrum (¹H, ¹³C. ¹¹B, ³³P) are reported. C₄₄H₅₀NBP₂ M = 665.64, Triclinic, P (#2), a = 11.530(4), b = 15.397(9), c = 11.497(9) Å, = 102.94(6), = 102.87(4), = 89.34(4)°, V = 1938(4) ų, and Z= 2.     

Single-crystal structure determination of a new polymorph (ε-Alq<Subscript>3</Subscript>) of the electroluminescence OLED (organic light-emitting diode) material,tris(8-hydroxyquinoline)aluminum (Alq<Subscript>3</Subscript>)

Tris(8-hydroxyquinoline) aluminum, Alq₃, is the most widely used electroluminescent material in organic light-emitting diode (OLED), chemistry. Single-crystal structure determination of a new polymorph of Alq₃, designated as -Alq₃, is described. There are three molecules of Alq₃ in the asymmetric unit. This octahedrally coordinated complex crystallizes in the triclinic space group P-1, lattice parameters a = 13.5190(5) Å, b = 15.8550(6)~Å, c = 18.7110(8) Å, = 95.4940(19), = 109.774(2), = 114.6270(16), Volume = 3296.8(2) ų, Z = 6, Z = 3.     

X-ray structure and NMR assignment of 4-methoxy-4′-methylthio-3,3′-diquinolinyl sulfidea

The title compound (C₂₀H₁₆N₂OS₂) is monoclinic, witha=7.786(3).,b=13.252(3),c=17.162(4) Å, =99.16(3)° and space groupP2₁/n. Two quinoline moieties are nearly perpendicular to each other (112.9(2)°). Both methoxy and methylthio groups are trans-orientated with the respect to the C(3)–S(1)–C(13) plane. Two pairs of the heteroatoms in ortho-positions are in very close contact. The conformation of the molecule explains an unusual¹H NMR spectrum     

Crystal and molecular structure of aquabis(2,2′-bipyridine)nitratomanganese(II) nitrate monohydrate

A new monomeric manganese(II) nitrate complex with 2,2-bipyridine (bpy), [Mn(bpy)₂(NO₃)(H₂O)](NO₃)·H₂O, has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space group witha=9.721(3),b=14.691(5),c=8.578(3) Å, =106.79(3), =96.05(3), =82.55(3)°,V=1159.9 ų andZ=2. The structure comprises discrete cation [Mn(bpy)₂(NO₃)(H₂O)]⁺ in which the metal atom is coordinated by a pair of bidentate bpy ligands [Mn–N=2.261(4)–2.299(4) Å], a unidentate nitrato [Mn–O=2.284(4) Å] and aqua [Mn–O=2.160(3) Å] ligands in a highly distorted octahedral arrangement.     

Hydrogen-bond networks in the mono- and diprotonated cyclic diamine [9]aneN2S

The hydrogen-bond networks in the mono- and diprotonated cyclic diamine, 1-thia-4,7-diazacyclononane, [9]aneN₂S, have been examined. Crystals of the monoprotonated, form [9]aneN₂S HCl, contain a ribbon-like network of alternating strong and weak intermolecular N H Cl hydrogen bonds and weak intramolecular N H N hydrogen bonds. Crystal data for [9]aneN₂S HCl: monoclinic, a = 6.6640(6) Å, b = 10.3493(9) Å, c = 6.9807(6) Å, = 108.847(1)°, V = 455.63(7) ų, space group P2₁, Z = 2. In the di-protonated form, [9]aneN₂S 2HBr, the ribbon-like network comprises strong intermolecular and weak intramolecular N H Br hydrogen bonds. Crystal data for [9]aneN₂S 2HBr: orthorhombic, a = 12.5918(13) Å, b = 8.0753(9) Å, c = 10.6856(11) Å, V = 1086.5(2) ų, space group Pnma, Z = 4. The chloride anions of [9]aneN₂S HCl align in interlocking columns in the a- and c-direction whereas the bromide anions in [9]aneN₂S 2HBr occupy channels in the b-direction.