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 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.     

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.     

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.     

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.     

An X-ray diffraction refinement of the crystal structure of natural apophyllite

The crystal structure of apophyllite (Andersberg — GDR), with a = 8.966(2), c = = 15.767(1) Å, P4/mnc, z = 2, Q = 2.35 gm · cm⁻³, has been refined (R = 0.035) by least squares with 976 reflections collected with a diffractometer. Apophyllite is a sheet structure with the bringing Si O bond lengths 1.6236 Å, while the non-bridging bond length Si O(3) is 1.5843 Å. The two independent Si O Si angles are 140.09, 140.76 degrees. The mean Si O bond length is 1.6138 Å. As it was not possible to locate unequivocally the H-atoms with the X-ray data, the interpretation of the of water in the structure was based on the charge balance approach of DONNAY and ALLMAN . Assuming that the fluorine ion is bonded to calcium ion (Ca-F = = 2.416 Å) and to H3 atom (F-H3 = 0.9145(1) Å) and water molecule hydrogen bonded to silicate framework. The average bond distances O-H are 0.962(2) Å and angle 105.24(1)°.     

The Crystal and Molecular Structure of 2-(2′-Cyano-2′-amido-ethylenyl)-pyridine

The title compound (C₉H₇N₃O) has been determined from three dimensional X-ray diffraction data. The crystals are monoclinic, a = 4.858(3) Å, b = 15.008(7) Å, c = 11.787(2) Å, ß = 94.107(2)°, V= 857.2(4) ų, z = 4, D_calc = 1.342 g. cm⁻³, space group P2_1/c. The structure was solved by direct methods and refined by full-matrix least-squares method (γ MoK_α′, R = 0.0766).     

Crystal and Molecular Structure of an Oligomeric 1:2 Complex of Copper (II) Azide with 4-Methylpyridine

A 1:2 complex of copper (II) azide with 4-methylpyridine has been synthesized and the crystal structure has been determined by X-ray methods. The compound crystallizes in space group P2₁/a with a = 11,062(3), b = 19.310(6), c = 20.547(5) Å, β = 90.83(2)°, V = 4389(1) ų, Z = 12 and R = 0.048 for 959 observed MoKα data. The structure is built up by oligomeric edge-sharing chains of polyhedra. With the exception of a single coordinated azido group, all other azido ligands serve to bridge neighbouring copper centers [at Cu  N bond distances of 1.94(2) to 2.76(2) Å] in the μ(1,1) fashion.     

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.     

A Novel Coordination Structure of Dichromates Bonding to Copper (II): [Cu(bipy)2(Cr2O7)] · 2 H2O

Dark-green multimetal compound crystal [Cu(bipy)₂(Cr₂O₇)]· 2 H₂O was obtained from aqueous solution of Cu(NO₃)₂, K₂Cr₂O₇ and bipyridine. The crystal structure was determined by X-ray crystallography: triclinic P1 , a = 7.716(3) Å, b = 9.656(3) Å, c = 15.517(5)Å, α = 77.41(3)°, β = 81.04(3)°, γ = 82.33(3)°, Z = 2. In this compound, two chromium atoms and a copper atom are linked by two oxo bridges (Cu(II) O Cr(VI) O Cr(VI)). The copper coordination polyhedron corresponds to a five-coordinated distorted trigonal bipyramid.     

The structure of Tetraphenyl Imidodiphosphate,C24H21NO6P2

M_r = 481.24, monoclinic, P 2₁/c, a = 12.009(3), b = 12.305(5), c = 18.993(7) Å, β = = 122.1(1)⁰, V = 2377.2(6) ų, D_x = 1.349 Mgm⁻³, Z = 4. Final R = 0.051 for 2690 independent reflections excluding those with |F₀| < 4 σ(F₀). Intensities were measured with an automatic diffractometer. The two phosphoryl oxygen atoms are in trans position. The acidic hydrogen atom is bonded at the nittogen atom. The molecules form dimers connected by N H … O intermolecular hydrogen bonds. Results are compared with those of the structure of tris(tetraphenylimidodiphosphato)ytterbium (III).     

Synthesis and crystal structure of bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl)copper(II)

The title compound, bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl) copper(II), [Cu(C₁₇H₁₁NOCl)₂] (1) was synthesized and its crystal structure was determined. The Compound 1 is monoclinic, space group P2 ₁/c with a = 9.146(3) Å, b = 18.724(3) Å, c = 16.230(2) Å, β = 96.46(1)°, V = 2761.8(11) ų, Z = 4, D _c = 1.503 g cm^?3, μ(Mo Kα) = 1.020 mm^?1, R = 0.0606 for 2361 reflections [I > 2σ(I)]. In the title compound, the Cu atom is coordinated by an N₂O₂ donor set from the imine-phenol ligand in a slightly distorted square planar coordination geometry, with the two phenolate O atoms being deprotonated. The Cu–O bond lengths are 1.878(4) and 1.889(4) Å, the Cu–N bond lengths are 1.980(5) and 1.985(5) Å. The angles O1–Cu–N1 and O2–Cu–N2 are 90.96(19) and 90.72(19)°, respectively.     

Crystal and molecular structure of 5,6-diphenyl-2-(α-formyl-benzyliden)-2H-thiopyranes

The crystal and molecular structure of the title compound has been determined by X-ray diffraction techniques. It crystallizes in the monoclinic space group P2₁/n with cell parameters a = 6.101(3) Å, b = 14.365(6) Å, c = 21.888(7) Å, β = 90.20(4)°, Z = 4. The structure was solved by direct methods and refined by least-squares calculations to an R value of 0.074. The molecule exists in solid state in the Z configuration. The very short intramolecular O S distance of 2.654(8) Å can be explained with polar interactions between the O and S atoms.     

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 mer-Co(4-CH3C5H4N)3(N3)3

The crystal structure of mer-Co(4-CH₃C₅H₄N)₃(N₃)₃has been determined by single crystal X-ray methods at 300 K. The compound crystallizes in the monoclinic space group C 2/c, a = 19.087(6), b = 16.769(4), c = 15.845(4) Å, β = 119.04(2)°, V = 4434(2) ų, M_r = 464.42. Z = 8, D_x = 1.391 Mgm⁻³, F(000) = 1920, λ (MoKα) = 0.71069 Å, μ = 0.802 mm⁻¹. The cobalt(III) ions are octahedrally coordinated to three azide groups and to three 4-methyl-pyridine molecules to form isolated coordination polyhedra.     

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.     

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 Structure of Sarcosine Cadmium Chloride

Single crystals of sarcosine cadmium chloride were crystallised from a saturated aqueous solution containing stoichiomeric amounts of sarcosine and cadmium chloride, in 1:1 proportion. The intensity data were collected using a CAD-4 diffractometer with graphite monochromated MoK_α, radiation. The crystal data are as follows: a = 6.916(1) Å, b = 13.855(3) Å, c = 7.981(1) Å, V = 764.1 Å · F.W. = 272.4, d_expt = 2.39 g · cm⁻³, d_calc = 2.368 g · cm⁻³, Z = 4 and the space group is P2₁/n. The structure has been solved to an R value of 0.023 for all the 1323 reflections with I > 2σ(I). The sarcosine molecule exists as zwitterion in the structure. The conformation of the sarcosine molecule is significantly changed due to the complexation of the molecule with cadmium chloride. The cadmium ion is found to have an octahedral coordination with both the oxygens of the carboxyl group of the amino acid and chlorines taking part in it. Since the complex has no water of hydration, only two hydrogen bonds of the types N H ‥ O and N H ‥ Cl are found.     

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 and molecular structure of 7-[1-(2-carbomethoxyanilino)-1-(phenyl)-methyl]-quinolin-8-ol(CMAB-Oxine) and comparising consideration to CMAP-Oxine

C₂₄H₂₀N₂O₃, Pbc2₁, a = 11.338(4), b = 7.786(3), c = 44.381(6) Å, D_x = 1.29 Mg · m⁻³, V = 3.82053 · 10⁻²⁷ m³. There are eight molecules in the unit cell (two molecules, A and B, in the asymmetric unit). The substitution of N (CMAP-Oxine) by CH(CMAB-Oxine) in the aldehyde participant of reactants creates differences both in intermolecular contacts and orientation phenomenons of ring planes. A high degree of selectivity of the substitution position for both compounds is given. The reactions to the synthesis of both compounds are difficult to agree upon with the characteristic feature of the Mannichreaction and corresponded more to the character of the electrophilic substitution of aromatics.