The structure of Dimethylaminomethanediphosphonic Acid,C3H11NO6P2

M_r = 218.9, monoclinic, P 2₁/c, a = 6.870(1), b = 10.824(2), c = 11.337(2) Å, β = = 94.59(2)⁰, Z = 4, V = 840.5(3) ų, D_x = 1.73 Mgm⁻³. Final R = 0.033 for 2648 independent reflections, excluding those with |F₀| < 3σ(F₀). Intensities were measured with an automatic diffractometer. This organophosphorous compound is characterized by two P C bonds. Four symmetrically independent intermolecular hydrogen bonds determine the threedimensional packing of the molecules and the unique chemical properties of the campound.     

Crystal Structure Investigation of 2-Pheny limidazo [f]1,10-phenanthroline

The crystal structure of the title compound (PIP) has been determined by single crystal X-ray diffraction methods. C₁₉H₁₂N₄. C₂H₅OH crystallizes in the monoclinic space group P2₁/n with a = 11.4414(8), b = 12.6052(9), c = 12.4627(8) Å, β = 100.345(2)°, Z = 4, V = 1768.17 ų, D_cal = 1.286 Mg. m⁻³, μ (MoKα) = 0.80 cm^-1, F(000) = 720. The structure was solved by the direct methods and refined by full-matrix least-squares method to a final R = 0.0337 and R_w = 0.0332 for 2306 reflections with F₀ > 4σ(F₀). The phenl ring and the imidazo[f]1,10-phenanthroline moiety are coplanar in the crystal. The packing of the molecules involves hydrogen bonded association of the hydroxyl group of ethanol both with the N H of the imidazole moiety of one PIP and one nitrogen atom of the phenanthroline moiety of another PIP.     

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.     

The structure of N-Pyrid-4-yl-iminotriphenylphosphorane,C23H19N2P

M_r = 353.9, monoclinic, P 2₁/c, a = 11.248(2), b = 11.323(2), c = 14.845(4) Å, β = = 95.87(2)⁰, Z = 4, V = 1880.8(3) ų, D_x = 1.28 Mgm⁻³, final R = 0.049 for 1995 independent reflections excluding those with |F₀| < 5 σ(F₀). Intensities were measured with an automatic diffractometer. The PN C-group of the molecule is nearly coplanar with the pyridine ring (dihedral angle 4.1°). The P atom and the C(2) atom of the pyridine ring overlap with their van der Waals spheres and have nearly the position with the maximum of steric hindrance. This conformation is the consequence of a conjugation between the Ph₃PN group and the N-standing pyridine ring as well as of an attraction between the P atom and the C(2) atom. A similar conformation has been observed in the molecule of N-pyrid-2-yliminotriphenylphosphorane.     

The molecular and crystal structure of 2-oxo-1-pyrrolidine-acetamide

C₆H₁₀N₂O₂, P1 , a = 6,607(2) Å, b = 8,538(2) Å, c = 6,392(2) Å, α = 102,43(2)°, β = 91,11(2)°, y = 79,82(2)°, V = 349,1 ų, Z = 2, D_m = 1,36 g × cm⁻³, D_x = 1,35 g × × cm⁻³, MoKα radiation, λ = 1.71069 Å, μ(MoKα) = 1.11 cm⁻¹. The structure was solved by direct methods. The parameters were refined by full matrix least squares technique to a final R = 0.088 for 834 reflections with ∥F₀∥ > 4σ(F₀). The dihedral angle between the least-squares plane through the pyrrolidine ring and that through the acetamide group is 90.4°. The N H … O hydrogen bonds connect molecules to form bands parallel to the z axis.     

The structure of N-Pyrid-2-yl-iminotriphenylphosphorane,C23H19N2P

M_r = 353.9, monoclinic, P 2₁/c, a = 11.371(4), b = 11.391(5), c = 14.699(11) Å, β = = 97.78(2)⁰, Z = 4, V = 1888.6(6) ų, D_x = 1.28 Mgm⁻³, final R = 0.052 for 2360 independent reflections excluding those with |F₀| < 5 σ(F₀). Intensities were measured with an automatic diffractometer. The PN C- part of the molecule is nearly coplanar with the pyridinring (torsion angle 6.4°). The P atom and the N(2) atom of the pyridinring overlap with their van der Waals spheres and have nearly the position with the maximum of steric hindrance. This conformation of the molecule is the consequence of a conjugation between the Ph₃P=N-group and the N-standing pyridine ring as well as of an attraction between the P atom and the N(2) atom.     

Structures of azomethine imines of the pyrazolid-3-one-type (V). The structure of 1-[pyrenyl-(1)-methylene]-5,5-dimethyl-pyrazolid-3-one-betaine.

C₂₂H₁₈N₂O, P2₁, a = 7.473(2), b = 13.563(3), c = 18.264(3) Å, β = 115.49(4)°, Z = 4, U = 1670.9(6) ų, D_x = 1.295 Mg m⁻³, μ(MoKα) = 0.855 cm⁻¹, crystal size: 0.3 × 0.2 × 0.2 mm, colour: yellow. Final R = 0.086 for 1973 independent reflections excluding those with |F₀ < 3σ(F₀). The intensities were measured with an automatic diffractometer. There are two symmetrically independent molecules in the unit cell. The azomethine imine parts of the molecules are similar to those of four other relevant structures determined by X-ray analysis. A polymethinic part of a molecule is linked with an aromatic part via the bond C(4)–C(5). The mean pyrenyl plains and the mean plains of the five membered rings include dihedral angles of 29.6° for molecule A and 23.7° for molecule B.     

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.     

The Crystal Structure of Hydrated Barium Copper Oxalate

BaCu(C₂O₄₂.6 H₂O is triclinic, P1 , with a = 6.5405(9), b = 9.202(3), c = 10.939(1) Å, α = 85.46(2), β = 79.22(1), γ = 80.45(2), V = 636.99(1) ų, Z = 2, D₀ = 2.14, D_c = 2.465 g. cm⁻³, R = 0.074, wR = 0.0746 for 2219 significant reflections |F₀|≧ 6.0σF₀. The barium has eleven coordinations and the coordination polyhedra is a capped antiprism. Six water oxygen atoms are coordinated whereas the other five are coming from the oxalate group. In the unit cell the molecules form a polymeric network. One lattice water molecule belongs to the coordinating water. The barium oxygen distances vary from 2.75 Å to 3.15 Å.     

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 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 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.     

Static Disorder in Hexagonal Crystal Structures of C60 at 100 K and 20 K

C₆₀ · 2C₈H₁₀ (100 K): hexagonal space group P6₃, a = 23.694(4), c = 10.046(2) Å, V = 4884(2) ų, D_x = 1.903 g cm⁻³, Z = 6, F(000) = 2856, γ(CuKa) = 1.54178 Å, μ = 0.84 mm⁻¹. C₆₀ · 2C₈H₁₀ (20 K): hexagonal space group P6₃, a = 23.67(1), c = 10.02(1) Å, V = 4862(6) ų, D_x = 1.912 g cm⁻³, Z = 6, F(000) = 2856, γ(CuKa) = 1.54178 Å, μ = 0.84 mm⁻¹. The structures were determined by Patterson syntheses and rigid-body refinements. The C₆₀ molecules show two orientations with one molecular centre in common. The solvent molecules are disordered too. Static disorder could not be overcome or influenced by cooling down. A coordination number of 10 was found for the fullerene molecules.     

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.     

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.     

Synthesis,crystal and molecular structure of trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II)

Trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II), [Ni(sac)₂(pypr)₂], where sac and pypr are the saccharinate anion and the 2‐pyridinepropanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 8.1981(8), b = 9.9680(10), c = 10.4956(10) Å, α = 90.740(3)° β = 108.142(3)°, γ = 111.025(3)°, Z = 1, V = 1.537 ų. The structure of the nickel(II) complex consists of neutral molecules in which the nickel(II) ion sits on a center of symmetry and is octahedrally coordinated by two sac ligands, and two neutral pypr ligands. The pypr acts as a bidentate N‐ and O‐donor ligand forming a seven‐membered chelate ring, while sac behaves as a monodentate O‐donor ligand via the carbonyl O atom. The Ni‐N bond distance is 2.1016(15) Å, whereas the Ni‐O_pypr and Ni‐O_sac bond distances are 2.1280(12) and 2.0792(11) Å, respectively. The individual molecules are held together with a strong hydrogen bond between the hydroxyl O atom of pypr and N atom of sac and the C‐H…O type weak hydrogen bonds between some ring hydrogen atoms of pypr and sac, and the carbonyl and sulfonyl O atoms of sac in the neighbouring molecules. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

X-ray diffraction analysis of (Ph2PO)2

The title compound (Ph2PO)2 is analyzed by single crystal X-ray diffraction analysis. The crystals are monoclinic, space group P2(1)/n with a = 9.5112(19) Å, b = 11.161(2) Å, c = 9.5487(19) Å, α = 90°, β = 91.65(3)°, γ = 90°, V = 1013.2(3) ų, Z = 2, F(₀₀₀) = 420, Dc = 1.319 g cm^–3, μ = 0.232 mm^?1, the final R = 0.0818, and wR = 0.2259. A total of 7954 reflections were collected, of which 1758 were independent (R_int = 0.0542). In the crystal packing diagram, intermolecular C—H···O hydrogen bonds stabilize the solid state of the title compound.     

On the stereochemistry of 7-[1(2-carbomethoxyanilino)-1-(pyridyl)-methyl]-quinolin-8-ol (CMAP-oxine)

C₂₃H₁₉N₃O₃, P1 , a = 11,683(3), b = 7.740(2), c = 14.445(3) Å, α = 131.02(8), β = 95.43(8), γ = 95.02(8)°, D_x = 1.328 Mg · m⁻³, V = 0.9614 · 10⁻²⁷ m³, Final R = 0.059 for 2905 symmetrically independent reflections (|F₀| ≧ 3σ(F₀)). The intensities were measured with an automatic diffractometer. There are two molecules in the unit cell. The substance is not tridentat in potentially coordination behaviour; coordination takes place (twodentat) on the oxine group.     

Crystal structure determination of bis-dimethyl heptamethine cyanine chloride,C11N2H19Cl · 4 H2O

Mr = 286.59, monoclinic superposition structure C 121, Z = 4, a = 15.248(3), b = = 6.942 (3), c = 9.074(1) Å, β = 120.1(1)°, V = 827(1) ų, D_m = 1.13(1) Mg m⁻³, D_x = = 1.15 Mg m⁻³, λ(MoK_α) = 0.71069 Å, μ = 0.243 mm⁻¹, F (000) = 312, T = 296 K, final R = 0.061 for 802 reflections. All hydrogen atoms were located. The structure consists of chloride anions, bis-dimethyl heptamethine cyanine cations and water molecules. The structure of bis-dimethyl heptamethine cyanine chloride is disordered, e.g. there exist partial coincidence operations, leading to more than one stacking mode of the bis-dimethyl heptamethin cyanine chains. The crystal structure consists of rows of molecule along the a-axis. The C C bonds show the bond length compensation, typical of polymethines, towards a partial double bond (mean value 1.38 Å) between formally sp²-hybridized C atoms. The C N bond lengths to the methyl carbon atoms (mean value 1.49 Å) correspond to normal C N single bonds. The valence angles at the C atoms of the heptamethine chain clearly alternate and deviate systematically from 120°. This is also observed in other structures of a similar type. The structure determined by X-ray analysis confirms the chemical results.     

Crystal structure of 3‐(3‐nitrophenylhydrazonocarbonyl)‐(1H)‐1,2,4‐triazole

The title compound, C₁₀H₈N₆O₃, was synthesized by the reaction of 3‐(1H)‐1,2,4‐triazole hydrazine with 3‐nitrobenzaldehyde in ethanol. The single crystal structure has been determined by X‐ray analysis. The crystal belongs to monoclinic system, space group p2₁/c with cell constant, a = 8.0214(17) Å, b = 17.334(4) Å, c = 8.9070(18) Å, V= 1179.4(4) ų. An intramolecular N—H...O and N—H…N hydrogen bond are observed between the ‐NH group with O atom of the carbonyl group and the ‐NH group with N atom. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)