Crystal structure determination of 2-acetylamino-4-benzoyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazolin,C13H15N3O2S

Thiosemicarbazone is receiving increasing interest because of the biological activity of some of its derivatives. Mr = 277.35, space group P2₁2₁2₁, Z = 4, a = 9.290(3), b = = 11.512(2), c = 13.286(2) Å, V = 1421 (1) ų, D_m = 1.29(1) Mg m⁻³, D_x = 1.296 Mg m⁻³, λ(MoK_α) = 0.71062 Å, μ = 0.230 mm⁻¹, F(000) = 584, T = 296 K, final R = 0.028 for 1255 reflections. All hydrogen atoms were located. The structure determed by X-ray analysis confirms the chemical results. The structure analysis of the title compound is described and its molecular and crystal structure discussed.     

Crystal and molecular structures of N-alkyl-N,N-dimethyl-3-(heptamethyltrisiloxan-3-yl) propylammonium bromides

C₁₆H₄₂NO₂Si₃Br: M_r = 444.76, monoclinic space group P 2₁/c, a = 23.300(8), b = 8.918(4), c = 13.403(2) Å, β = 101.69(4)°, V = 2727(1) ų, D_x = 1.08 Mgm⁻³, D_exp = 1.06 Mgm⁻³, Z = 4, F(000) = 932, λ(MoKα) = 0.71069 Å, μ = 16.3 cm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.117. C₁₅H₄₀NO₂ Si₃Br: M_r = 430.34, monoclinic space group P2₁/c, a = 23.460(4), b = 8.518(2), c = 13.403(2) Å, β = 102.03(2)°, V = 2619(1) ų, D_x = 1.09 Mgm⁻³, D_exp = 1.07 Mg⁻³, Z = 4, F (000) = 920, λ(MoKα) = 0.71069 Å, μ = 33.9 cm⁻¹. The crystal structure was determined by least-squares refinement of the structure model derived from structure determination of C₁₆H₄₂NO₂·Si₃Br to the discrepancy factor R = 0.099. C₁₆H₄₂NO₂Si₃Br: Daten siehe oben. C₁₅H₄₀NO₂Si₃Br: Daten siehe oben.     

Crystal structure investigation of [Mn(3-CH3C5H4N)2(N3)2(H2O)2]

The crystal structure of the title compound has been determined by single crystal X-ray diffraction methods. [Mn(3-CH₃C₅H₄N)₂(N₃)₂(H₂O)₂] crystallizes in the space group P 1 with a = 7.444(2) Å, b = 7.691(2) Å, c = 8.926(3) Å, α = 99.82(3)°, β = 108.80(2)°, γ = 114.99(2)° and Z = 1. Least squares refinement gave a R value of R_w = 0.046 for 1414 observed reflections. The manganese atom in the title complex is octahedrally coordinated by two oxygen atoms of the water molecules and four nitrogen atoms; two N-atoms are the end atoms of azide groups and the other two nitrogen atoms belong to the 3-methylpyridine molecules. The polyhedra are linked via hydrogen bonds between the water molecules and the azide groups.     

Synthesis and crystal structure of di(2-aminopyrimidinium) trichlorodimethyl(2-aminopyrimidine)stannate(IV) chloride (H-2APY)2[SnMe2Cl3(2APY)]Cl

The synthesis and molecular structure of di(2-aminopyrimidinium) trichlorodimethyl(2-aminopyrimidine)stannate(IV) chloride (H-2APY)₂[SnMe₂Cl₃(2APY)]Cl is reported. The compound crystallized in the orthorhombic space group Pnma with a = 20.524(1) Å, b = 10.822(1) Å, c = 10.472(1) Å and V = 2325.9(3) ų, Z = 4. The structure consists of three fragments: the hexacoordinated organotin anionic complex [SnMe₂Cl₃(2APY)]⁻, which exhibits distorted octahedral geometry; two protonated 2-aminopyrimidinium cations (H-2APY)⁺, and one chloride anion.

     

Crystal and Molecular Structure of Tosyl Pyrrolidine-2-Methanol (C12H17SO3N)

C₁₂H₁₇SO₃N, M_r = 255.33, Orthorhombic, P2₁2₁2₁, a = 11.703(1) Å, b = 14.797(3) Å, c = 14.971(2) Å, V = 2592.52 ų, Z = 8, D_m = 1.309 Mgm⁻³, D_c = 1.308 Mgm⁻³, mμ = 21.57 cm⁻¹, F(000) = 1088, T = 290 K, final R = 0.080 for 2416 unique reflections. There are two crystallographically independent molecules in the unit cell of the title compound.     

Crystal structure of 4,5-dihydro-6-(2-thienyl)-3(2H) pyridazinone azine, (C16H16N16S2)

M_r = 484, monoclinic, P 2₁/c, a = 5.567(1), b = 7.857(2), c = 19.194(10) Å, β = 99.97(3)°, V = 826.9 ų, Z′ = 2, D_x = 1.43 g · cm⁻³, F(000) = 372, MoKα, λ = 0.71069 Å, μ = 0.328 mm⁻¹, final R = 0.055 for 889 observed reflections, T = 293 K. The compound was prepared from a direct unusual reaction of 6-(2-thienyl)-2,3,4,5-tetrahydropyridazine-3-one with hydrazine hydrate. The structure was solved by direct methods and refined by full-matrix least squares. The molecule in the solid state consists of a dimer with its two equivalent halves related by a center of symmetry at the middle of the N N bond. Each molecular fragment is nearly planar and the N N bond between the two halves is 1.296(5) Å indicating that it is a partial double bond.     

The Structure of 4-n-Hexyle-6-(4-cyanophenyl)-1,5-diazobicyclo [3.1.0]-hexanone-(2), C17H21N3O

M_r = 283.2; monoclinic, P 2₁/c, a = 9.631(7), b = 21.268(16), c = 8.488(8) Å, β = 107.13(9)°, Z = 4, V = 1661.8(9) ų, D_x = 1.42 Mg m⁻³, final R = 0.134 for 605 independent reflections excluding those with |F_o| < 3σ|F_o|). Intensities were measured with an automatic diffractometer. The compound is a product of a photoreaction. The five membered ring and the three membered ring of the bicyclic diaziridine group and the six membered ring of the 4-cyanophenyl group are nearly perpendicular one to another. The 4-cyanophenyl group is in exo-position to the five membered ring of the bicyclic diaziridine group. The C(4) atom and the aliphatic hexyle group are in respect to the five ring in trans-position.     

Structural and spectroscopic study of Mg13.4(OH)6(HVO4)2(H0.2VO4)6

Single‐crystals of the polar compound magnesium hydrogen vanadate(V), Mg_13.4(OH)₆(HVO₄)₂(H_0.2VO₄)₆, were synthesized hydrothermally. It represents the first hydrogen vanadate(V) among inorganic compounds. Its structure was determined by single‐crystal X‐ray diffraction [space group P 6₃mc, a = 12.9096(2), c = 5.0755(1) Å, V = 732.55(2) ų, Z = 1]. The crystal structure of Mg_13.4(OH)₆(HVO₄)₂(H_0.2VO₄)₆ consists of well separated, vacancy‐interrupted chains of face sharing Mg2O₆ octahedra, with short Mg2—Mg2 distances of 2.537(1) Å, embedded in a porous magnesium vanadate 3D framework having the topology of the zeolite cancrinite. All three hydrogen positions in the structure were confirmed by FTIR spectroscopy. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 1-diazo-2,3,4,5-tetraphenylcyclopentadiene

M_r = 396.30, monoclinic space group P 2₁/c, a = 10.145(2), b = 18.523(4), c = 12.443(2) Å, β = 110.31(2)°, V = 2193(1) ų, Z = 4, D_x = 1.201 Mg m⁻³, F(000) = 832, λ(MoKα) = 0.71069 Å, μ = 0.7 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.039.     

Crystal and molecular structure of 1-(p-nitrophenyl)-2-acetylamino-3-brom-propen-2-on-1, C11H9BrN2O4

M_r = 313.11, orthorhombic space group Pbca, a = 8.165(1), b = 9.491(2), c = 32.207(5) Å V = 2496(1) ų, D_X = 1.667 Mgm⁻³, Z = 8, F(000) = 1248, λ(MoKα) = 0.71069 Å, μ = 32.7 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.065. Positions of hydrogen atoms were calculated. The structure determined by x-ray analysis confirms the chemical results.     

Structure of N-5-Anilino-pentadien-(2,4)-ylidenaniliniumperchlorate,C17H17N2O4Cl

M_r=348.65, monoclinic, P2₁/n, a=11.088(2), b=17.521(3), c=8.845(2) Å, β=98.87(3)⁰, Z=4, V=1697.8(8) ų, D_x=1.368(1) Mgm⁻³, μ(MoKα)=0.256 mm⁻¹, λ(MoKα)=0.71069 Å, T=296 K. Final R=0.040 for 2454 independent reflections excluding those with |F₀|<4σ(|F₀|). Intensities were measured with an automatic diffractometer. The structure belongs to the openchained cyanines. Characteristic for this class of compounds is their nearly ideal polymethinic electron structure with its main geometrical features: equalisation of bond lengths, alternation of bond angles, planarity of the polymethinic chain. All three features are significantly to be observed in the structure. The bond angle alternation determines essentially the shape of the molecules and the molecular packing.     

Crystal Structure Determination of Nickel (2,2-Dipyridyl) Sulphate Hexahydrate [Ni(C10H8N2) · 4 H2O]SO4 · 2H2O

[Ni(C₁₀H₈N₂) · 4 H₂O]SO₄ · 2 H₂O, Mr = 418.7, monoclinic, P1 , a = 7.781(3), b = 9.421(3), c = 11.457(4) Å, α = 87.54(2)º, β = 96.40(2)º, γ = 102.58(2)º, ν = 814.5 Å, D_x = 1.26 g/cm³, Z = 2, (MoKx) = 0.71073 Å, μ = 7.0 cm⁻¹: T = 23 °C, R = 0.047 for 2139 reflections having intensities greater than 36. The structure was solved using the Patterson heavy-atom method and the remaining atoms were located in succeeding difference Fourier syntheses. The structure was then refined by full matrix least-squares using anisotropic temperature factors. Hydrogen atoms were located and their positions and isotropic parameters were refined.     

Crystal and molecular structure of 2-diazo-5-phenyl-cyclohexan-1,3-dione

M_r = 214.24, monoclinic space group P 2₁, a = 10.964(2), b = 5.870(2), c = 8.574(2) Å, β = 98.09(2)°, V = 546(1) ų, Z = 2, D_x = 1.302 Mg m⁻³, F(000) = 224, λ (MoKα) = 0.71069 Å, μ = 0.8 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.034. M_r = 214.24, monokline Raumgruppe P 2₁, a = 10.964(2), b = 5.870(2), c = 8.574(2) Å, β = 98.09(2)°, V = 546(1) ų, Z = 2, D_x = 1.302 Mg m⁻³, F(000) = 224, λ(MoKα) = 0.71069 Å, μ = 0.8 mm⁻¹.     

Structures of Azomethine Imines of the Pyrazolidone-(3)-type, (III) The Structure of 1-[Anthryl-(9)-methylene]-pyrazolidone-(3)-betaine

C₁₈H₁₄N₂O, Pbca, a = 19.541(4) Å, b = 14.800(2) Å, c = 9.572(3) Å, Z = 8, U = 2768.3 ų, D_x = 1.32 g cm⁻³, μ(MoKα) = 0.93 cm⁻⁻¹, crystal size 0.5 × 0.2 × 0.1 mm, colourless. Final R = 0.077 for 1177 independent reflections excluded those with |F₀| < 8 σ(F₀). The intensities were measured with an automatic diffractometer. The azomethine imine unit of the molecule has a geometry in approximate agreement with a polymethinic electron structure. The conjugation of the azomethine imine unit with the anthryl unit is only small. The anthryl ring and the five membered pyrazolidone ring include a dihedral angle of 65.4°. The main intermolecular forces are C–H … N hydrogen bridges.     

Structure of monoclinic acridine orange hydrochloride monohydrate,C17H19N3 · HCl · H2O

M_r = 319.82, monoclinic P2₁/a, Z = 4, a = 14.545(5), b = 15.562(6), c = 8.538(4) Å, β = 120.66(3)°, V = 1662(1) ų, D_m = 1.27 Mgm⁻³, D_x = 1.278 Mgm⁻³, λ(MoKα) = 0.71069 Å, μ(MoKα) = 0.24 mm⁻¹, T = 297 K. Final R = 0.049 for 1485 observed reflections. All hydrogen atoms were located and refined isotropically. Bond lengths (σ = 0.004 Å) and angles (σ = 0.3°) are normal. The substance is a derivative of acridine. The structure consists of chloride anions, bisdimethylaminoacridinium cations and water molecules. In the solid state the molecules are approximately planar. Pairs of cations form dimers with parallel planes connected by an I inversion centre and plane distances of 3.474 Å. They overlap with partial areas of all three six membered rings.     

Synthesis,Crystal and Molecular Structure of Cd2(sacch)4(Im)4

The title compound has been synthesized and its crystal structure determined at room temperature. Cd₂(Sacch)₄(Im)₄ F.W. = 1225.83, monoclinic. Space group: C2/c, Z = 4, a = 20.065(3) Å, b = 11.164(4) Å, c = 20.697(6) Å, β = 94.69(5)°, The coordination polyhedron of Cd(II) correspond to a five-coordinate trigonal-bipyramid. In the title complex, two of the saccharin groups act as monodentate ligands. The other two act as bidentate ligands. The two Cd(II) ions are bridged by the two bidentate saccharin groups and the distance is 4.75 Å.     

Crystal and Molecular Structure of 1-Ethyl-3-[tris(trimethylsiloxanyl)silyl]pyrrolinium Hydrochloride

The crystal and molecular structure of 1-Ethyl-3[tris(trimethylsiloxyl)silyl]pyrrolinium hydro-chloride (C₁₅H₃₈N⁺O₃Si₄ · C¹⁻) has been determined by direct methods. The title compound crystallizes in the monoclinic space group C2/c with a = 20.640(3), b = 19.494(2), c = 27.34(3) Å, β = 90.60(4)°, V = 11000(13) ų, Z = 16, D_x = 1.034 Mg m⁻³. There are two molecules with different conformations in the crystal. The pyrroline rings are non-planar.-The Si O Si angles range from 149(1)° to 163(1)°. Two of the SiMe₃ groups are disordered. All molecules are connected by C¹⁻ – N⁺ contacts and C¹⁻ - HN⁺ hydrogen bonds to form double chains.     

The emission and structure of a new laser crystal Nd3+: NaY(WO4)2

A new laser Nd³⁺ : NaY(WO₄)₂ crystal rod of Φ 2.5 × 5 mm was pumped by a xenon flash lamp, and a 1.06 μm laser output was for the first time obtained in our laboratory, which has a threshold lower than 1 J. The crystal structure of NaY(WO₄)₂ was determined. The crystal is tetragonal, with the space group 14₁/a, a = 5.205(2) Å, c = 11.251(3) Å, V = 304.8(2) ų, Z = 2, D_calc = 6.62 g/cm³, D_obs = 6.51 g/cm³.     

Crystal and molecular structure of 5-diazo-2,2-dimethyl-4,6-dioxo-1,3-dioxane and 5-diazo-1,3-dimethylpyrimidin-2,4,6-trione

C₆N₂O₄H₆: M_r = 170.12, orthorhombic space group Pbca, a = 6.751(2), b = 13.669(4), c = = 16.845(4) Å, V = 1555(1) ų, D_x = 1.248 Mgm⁻³, Z = 8, F(000) = 704, λ(moKα) = 0.71069 Å, μ = 1.1 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.039. C₆N₄O₃H₆: M_r = 182.14, monoclinic space group C2/c, a = 17.726(8), b = 6.191(12), c = 16.062(6) Å, β = 117.59 (3)°, V = 1562 (1) ų, D_x = 1.549 Mgm⁻³, Z = 8, F(000) = 752, λ(MoKα) = 0.71069 Å, μ = 1.2 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.056.     

Structure of the OD-disordered 2-Hydroxy-4-methoxy-2H-1,4-benzoxazin-3-one,C9H9NO4

The X-ray diagrams of the title compound show pronounced maxima on diffuse streaks parallel c* and unusual extinctions. The intensity distribution is compatible with the assumption of a disordered (OD) structure consisting of one kind of layers. The structure contains ordered domains with the crystal data: monoelinic, space group P 2₁/a, lattice parameters a = 15.910(5), b = 8.365(4), c = 15.747(5) Å, β = 120.34(6)°, V = 1809 ų, Z = 8, M_r = 195.1, D_x = 1.432 Mg m⁻³, μ(MoKα) = 0.36 mm⁻¹, final R = 0.129 for 859 observed reflections. The asymmetric unit is constituted of two crystallographically independent molecules related by a pseudo glide plane. The crystal used for X-ray analysis proved to be twinned.