Synthesis and crystal structure of copper halide complexes with triethylallylammonium (teaa) chloride: [(teaa)Cu3ICl4], [(teaa)Cu3IBr3.86Cl0.14], and (teaa)2CuIICl4

The results of X-ray diffraction analysis of novel triethylallylammonium chloride compounds with copper(I) chloride, copper(I) bromide, and copper(II) chloride are reported. The [(CH₃CH₂)₃(CH₂=CHCH₂xN]Cu ₃ ^I Cl₄ and [(CH₃CH₂)₃(CH₂=CHCH₂Cu ₃ ^I Br_3.86)Cl_0.14 -complexes are isostructural: space group P2₁/a; a= 17.58(1) Å, b = 12.059(8)Å, c = 7.184(4) Å, = 98.37(5)° and a = 17.972(9) Å, b=12.479(8) Å, c = 7.290(5) Å, = 98.81(5)°, respectively. ²-Coordination of the copper atom by the olefinic bond plays a key role in the structural ordering of the tetraalkylammonium cation. In contrast, the structure of {(CH₃CH₂)₃x(CH₂=CHCH₂)N}₂Cu^IICl₄ (P4₂/nmc; a = 8.839(3) Å, c =15.660(9) Å) follows the ionic salt pattern.Original Russian Text Copyright © 2004 by L. M. Babkov, I. I. Gnatyuk, G. A. Puchkovskaya, and S. V. TrukhachevTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 3, pp. 398–405, May–June, 2004.     

The structures of 1-(2′-hydroxybenzoyl)piperidine and 4-(2′-hydroxybenzoyl)morpholine

1-(2-hydroxybenzoyl)piperidine, C₁₂H₁₅NO₂, orthorhombic, Pbc2₁-C _2v ⁵ ;a=9.529 (1),b=10.001 (1),c=11.652 (1) Å;Z=4. The structure was determined from 1 510 single crystal X-ray data by direct methods and the refinement of the structure parameters yieldedR=0.040. There is one molecule in the asymmetric unit.4-(2-hydroxybenzoyl)morpholine, C₁₁H₁₃NO₃, orthorhombic, P2₁2₁2₁-D ₂ ⁴ ;a=13.006 (1),b=17.258 (2),c=9.125 (1) Å;Z=8. The structure parameters of the isotypic compound 4-(2-hydroxythiobenzoyl)morpholine were used in a starting set of refinement; finallyR=0.054 was obtained for 1 900 single crystal X-ray data. There are two molecules in the asymmetric unit.In both compounds the hydrogen atoms could be located by means of differenceFourier summations. The intermolecular hydrogen bonds with O ... O distances of 2.649 (2) Å for the piperidine derivate and 2.688 (3) resp. 2.754 (3) Å for the morpholine derivate are typical for intermediate bond strengths.

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Die Strukturen von 1-(2-hydroxybenzoyl)piperidin und 4-(2-hydroxybenzoyl)morpholin

Zusammenfassung 1-(2-hydroxybenzoyl)piperidin, C₁₂H₁₅NO₂, orthorhombisch, Pbc2₁-C _2v ⁵ ;a=9.529 (1),b=10.001 (1),c=11.652 (1) Å;Z=4. Die Struktur wurde aus 1 510 Einkristallröntgendaten mittels direkter Methoden bestimmt; die Strukturverfeinerung ergabR=0.040. Es ist ein Molekül in der asymmetrischen Einheit.4-(2-hydroxybenzoyl)morpholin, C₁₁H₁₃NO₃, orthorhombisch, P2₁2₁2₁-D ₂ ⁴ ;a=13.006 (1),b=17.258 (2),c=9.125 (1) Å;Z=8. Die Strukturparameter der isotypen Verbindung 4-(2-hydroxythiobenzoyl)morpholin wurden als Startsatz für die Strukturverfeinerung benutzt. Es wurdeR=0.054 aus 1 900 Einkristallröntgendaten erreicht. Es befinden sich zwei Moleküle in der asymmetrischen Einheit.In beiden Verbindungen konnten mittels Differenz-Fourier-Summierungen die Wasserstoffatome lokalisiert werden. Die intermolekularen Wasserstoffbrükken mit O ... O-Distanzen von 2.649 (2) Å für das Piperidinderivat und 2.688 (3) bzw. 2.754 (3) Å für das Morpholinderivat sind typisch für mittlere Bindungsstärken.

     

Molecular and crystal structure of 2-phenoxy-2λ5-2,2′(3H,3′H)-spirobi[1,3,2-benzoxazaphosphole]

The crystal and molecular structure of 2-phenoxy-2⁵-2,2(3H,3H)-spirobi[1,3,2-benzoxazaphosphole] has been determined using X-ray diffraction structure analysis. The P atom in the molecule in question has a distorted trigonal bipyramidal coordination, with the bond lengths P-O_ax=1.701(1) and 1.700(1) Å, P-O_eq (Ph)=1.625 Å, P-N_eq=1.654(2) and 1.645(1) Å, and bond angles (O-P-O)_ax=175.69(7)° and (N-P-N)_eq = 132.38(7)°.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 876–879, May, 1993.     

The polyiodide salts: Pyridinium pentaiodide;β-naphthylammonium pentaiodide; andN-methyl-γ-picolinium heptaiodide. Structures with channel inclusion features

The crystal structures of three polyiodode salts are reported (pyridinium pentaiodide, monoclinic,P2 ₁/m,a=9.221(5),b=12.918(5),c=6.026(4) Å, =103.60(7)^o,Z=2,R _F=0.087 for 1187 intensities; -naphthyl-ammonium pentaiodide, triclinic,173-1,a=10.390(5),b=9.502(5),c=4.462(3) Å, =99.19(7), =90.40(7),=108.49(8)^o,Z=2,R _F=0.059 for 1319 intensities;N-methyl--picolinium heptaiodide, monoclinic,C2/c,a=19.315(7),b=12.714(5),c=8.442(4) Å, =107.26(7)^o,Z=4,R _F=0.065 for 1336 intensities). All three structures can be described as having channel inclusion features; the cations are contained in channels in polyiodide frameworks based on different arrangements of I₂ molecules and I ₃ ^– anions. This structural type is the converse of the more widespread kind where polyiodide anions are contained in an organic matrix (e.g., cyclodextrin polyiodides). Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82016 (30 pages).Part X of Crystal Structures of Polyiodide Salts and Complexes. For Part IX, see F. H. Herbstein, G. M. Reisner, and W. Schwotzer,Acta Crystallogr. C, accepted for publication, 1984     

Synthesis of Co3(CO)7(μ-η3-Allyl)(μ3-X) Complexes (X=S, Se) and Structure of the Selenium Derivative

The complexes Co₃(CO)₉( ₃-X) (X=S, Se) can be reduced to the corresponding anionic species [Co₃(CO)₉( ₃-X)]^–, which react with allyl bromide to give Co₃(CO)₇(- ³-C₃H₅)( ₃-X) (X=S, Se). These are the first two cobalt complexes containing the bridging - ³-allyl ligand. The structure of the selenium complex was determined by X-ray crystallography. Crystal data for Co₃(CO)₇(- ³-C₃H₅)( ₃-Se) are as follows: space group P2₁/c, a=9.051(2) Å, b=8.102(2) Å, c=21.27(4) Å, =93.82(3)°, Z=4, and R=0.0565 for 2491 observed reflections.     

Synthesis and Crystal Structure of a New Copper–PMIDA Compound (H4PMIDA=H2O3PCH2N(CH2CO2H)2)

A new Cu(II)PMIDA compound [Cu(H₂PMIDA)(phen)] 3H₂O (1) (H₄PMIDA = H₂O₃PCH₂N (CH₂CO₂H)₂,phen = 1,10-phenanthroline) has been successfully synthesized and structurally characterized. In complex 1, Cu (II) is six coordinated by chelation in a tetradentate fashion by a PMIDA ligand and by two N atoms of a phen ligand. Every phen–Cu(II)–PMIDA group connects with each other via a hydrogen bond and the edge-to-face -stacking interaction. Complex 1 crystallized in triclinic P-1 with cell dimensions of a = 7.5817(6) Å, b = 10.6980(8) Å, c = 13.1852(10) Å, =82.350(2)°, = 84.151(2)°, =78.4250(2), V= 1035.25(14) ų, Z = 2, Dc = 1.677 Mg/m³.     

Polymorphism of Inclusion Complexes and Unsolvated Hosts. IV. Dimorphism of the Acetone Host–Guest Complex of Dianilinegossypol. Structures of the α- and β-Phase Complexes

Crystal structures of the - and -phase inclusion complexes of dianilinegossypol with acetone obtained at 20° and 30 °C, respectively, have been determined by X-ray structure analysis. Crystal data of the -phase complex are: C₄₂H₄₀O₆N₂2C₃H₆O, orthorhombic, space group Pccn, a = 29.501(9), b = 10.866(2), c = 13.756(3) Å, V = 4409(1) ų, Z = 4, D _x = 1.18 g cm^-3. The structure has been refined to a final R value of 0.117 for 1401 observed reflections. The host–guest ratio for the -phase complex is the same (1 : 2) and the crystals are monoclinic, space group C2/c, a = 28.352(6), b = 11.836(2), c = 13.196(1) Å, = 93.05(1)°, V = 4422(2) Å3, Z = 4, D _x =1.18 g cm^-3. The structure has been refined to a final R value of 0.077 for 1414 observed reflections.In both phases molecules of dianilinegossypol form hydrogen-bondedribbons by O(4)–-HO(3) H-bonds. Phases are determined by the same structural motif. In the -phase complex the cages are in the form of prisms but in the -phase clathrate they undergo a modification by shrinking in two directions and widening in one. Molecules of acetone are hydrogen bonded to the host molecules via aO(1)–-HO(G) bond and are accommodated in cavities for both complexes, i.e. both phases are cryptate-type inclusion complexes.Supplementary data relevant to this publicationhave been deposited with the British Library,No. SUP 82227 (24 pages).     

X-ray structure and thermal analysis of a 1∶1 complex between sulfathiazole andβ-cyclodextrin

An inclusion complex with the formula (-cyclodextrin) (sulfathiazole) 8.3 H₂O has been crystallized and characterized by physicochemical methods including single crystal X-ray analysis. The complex crystallizes in the monoclinic system, space group P2₁, witha=15.264(4),b= 16.500(6),c=15.559(5) Å,=117.29(3)^o andZ=2. The structure was solved using published co-ordinates for-cyclodextrin in an isomorphous complex. Refinement by block-diagonal leastsquares yieldedR=0.061 for 4706 unique observed reflections. Inclusion of sulfathiazole produces a slight ellipticity in the host conformation, but the guest adopts a conformation similar to that observed in its polymorphs. The guest is held in the macrocyclic cavity predominantly by hydrophobic forces, with the phenyl ring near the host primary hydroxyl side and the thiazole ring near the secondary hydroxyl side. The complex packs in layers parallel to theac-plane. Layers are linked by hydrogen bonding to water molecules which are located outside the cyclodextrin cavity. An extensive network of hydrogen bonds mediated chiefly by water molecules stabilizes the crystal structure.     

Structure and Energetics of β-Diketonates. XII. Structure of Lanthanide tris-Dipivaloylmethanates for Er(thd)3 Used as an Example

A simultaneous electron diffraction and mass spectroscopic study of saturated vapors of erbium tris-dipivalylmethanate has revealed that at 136(5)°C, the vapor consists solely of Er(thd)₃ molecules. Electron diffraction data may be described by two alternative models (of C_3 and D_3 symmetry), for which r_a, r_g, and r structural parameters have been determined. D₃ symmetry is recognized to be preferable for free Er(thd)₃ molecules. The main structural parameters of the model are r (Er – O) 2.218(5), r (O – C) 1.279(5), r (C – C_r) 1.404(6), r (C – C_t) 1.512(3), r(C_t – C_m) 1.542(5), r (rm C_m– H) 1.804(4) , The ErO 75.0(0.4)°. The ErO₆ coordination polyhedron has a structure close to an antiprism. A rotational angle of the O–O–O trigonal face relative to the position in a regular prism is 20.7(0.8)°. Possible reasons for the differences in the structure of Er(thd)₃ molecules in the gas phase and crystal are discussed.     

2,2′-Diphenyl-Δ3,3′-bi-3H-indole-1,1′-dioxide: Molecular interactions and crystal structure

The Dinitrone 2,2-diphenyl-^3,3-bi-3H-indole-1,1-dioxide acts as a demethylating and dehydrogenating agent. The mechanism of interaction of the dinitrone with donors and acceptors does not involve intermediate charge-transfer complexes probably due to a self association between dinitrone molecules (as supported by X-ray determinations). The crystal structure of the dinitrone was obtained by direct methods;a=9.967 (2),b=19.817 (3),c=10.875 (2) Å, =111.2 (2)°, space group P2₁/n. The finalR andR _w were 0.089 and 0.063 for all measured reflexes.

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2,2-Diphenyl-^3,3-bi-3H-indol-1,1-dioxid: Molekulare Wechselwirkungen und Kristallstruktur

Zusammenfassung Das Dinitron 2,2-Diphenyl-^3,3-bi-3H-indol-1,1-dioxid wirkt als Demethylierungs- und Oxydationsmittel. Die Wechselwirkung des Dinitrons mit Elektronen-Acceptoren und Elektronen-Donatoren geht wegen der Selbstassoziation zwischen den Dinitron-Molekülen ohne die dazwischenliegende Bildung eines Charge-Transfer-Komplexes vor sich; das wird auch von Röntgenstrukturuntersuchungen gestützt. Die Kristallstruktur wurde mit direkten Methoden ermittelt:a=9.967 (2),b=19.817 (3),c=10.875 (2) Å; =111.2 (2)°. P2₁/n. Die endgültigen WerteR undR _w waren 0.089 und 0.063 für alle gemessenen Reflexe.

     

SCF-CI studies on the electronic ground state of water: Potential energy hypersurface and spectroscopic constants

Large-scale Hartree-Fock self-consistent field calculations, employing extended Gaussian basis sets, and configuration interaction studies are performed to calculate the energy hypersurface of the electronic ground state of the water molecule and to investigate the accuracy requirements in view of the determination of molecular spectroscopic constants. From the calculated points on the hypersurface the theoretical equilibrium geometry, the force field through fourth order, the spectroscopic constants _i, x_ij, _i as well as the Darling-Dennison and Fermi resonance constants are evaluated. The CI surface yields an equilibrium structure for H₂O withr _e = 0.9501 Å and _e=105.33 ° (r _exp = 0.9572 Å and _exp = 104.52 °). The vibrational levels are obtained with a systematic error of about 2 percent and the rotational constants to about 1 percent compared to spectroscopic data. The relative energy maximum corresponding to the linear structure with = is calculated to be 11890cm^–1, within the error limits of the values deduced from experimental measurements.     

Influence of conjugated nitrogenous bases on the spectra and structure of mixed-ligand nickel(II) chelates containing β-diones

The infrared and electronic excitation spectra of a series of new nickel(II) chelates containing an-diimine (or nitrogenous base, enR) and the anion of a-dione (1,3-ketoenol or 1,3-ketoester,H) were obtained in the solid state and in solution. The composition and the overall structure of the new chelates in the solid state depends on ligand concentration, the substituents within the-dionato moiety and the counterion present. The IR and electronic excitation spectra of [Ni(enR)₂ ]NO₃ and [Ni(enR)(O₂NO)] indicate, in conjunction with other physicochemical measurements, bidentate coordination of the ligands, while the spectral shifts reveal replacement of the (O,O)nitrato group by basic solvents. The existence of the nickel(II) in an octahedral environment is confirmed by an X-ray structure analysis of [Ni(dpamH)₂acac]NO₃ · CH₃OH (monoclinic, space groupP2_l/n, a=17.296(1),b=7.462(1),c=21.604(3) å,=95.65(1),Z=4, R=0.0534,Rw=0.0600), where dpamH denotes the 2,2-dipyridylamine.     

Synthesis and crystal structure ofN,N′-DicyclohexylpiperazineN,N′-dioxide octahydrate

N,N-DicyclohexylpiperazineN,N-dioxide octahydrate, C₁₆H₄₆N₂O₁₀,M _r=426.55, monoclinic, space groupC2/m (No. 12),a=12.961(4),b=11.533(4),c=7.907(1) Å, =98.37(2)^o,V=1169.3(6) ų,Z=2. The structure was solved by the direct method and refined toR=0.045 for 1192 observed MoK reflections. TheN,N-dioxide molecule occupies a site of symmetry 2/m. The piperazine ring takes the chair form with the two N–O bonds oriented axially in atrans configuration. Hydrogen bonding between the water molecules, as well as between theN-oxide groups and water molecules, gives rise to a puckered layer composed of edge-sharing four-membered, five-membered, six-membered, and eight-membered rings. Adjacent layers are cross-linked by theN,N-dicyclohexylpiperazine moieties lying between them, thereby generating a sandwich structure consolidated by covalent and hydrogen bonding. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82062 (8 pages).     

Synthesis,Structure and Property of Oxo-Bridged Binuclear Iron(III) Complex [Fe(phen)(H<Subscript>2</Subscript>O)<Subscript>3</Subscript>]<Subscript>2</Subscript>O⋅2SO<Subscript>4</Subscript>

An oxo-bridged binuclear iron(III) complex, [Fe(phen)(H₂O)₃]₂O2SO₄, has been synthesized and structurally characterized by elemental analysis (EA), IR, TG-DSC and X-ray. Its crystal structure has been determined by X-ray crystallography. It crystallizes in the orthorhombic system, space group P2₁2₁2, with lattice parameters a = 17.650(4), b = 8.5133(17), c = 9.971(2) Å; V = 1498.2(5) ų, _calcd = 1.763 g/cm³ and Z = 4 for R₁ = 0.0601. The crystal structure indicated that two octahedrally coordinated iron(III) ions bridged with oxygen atoms formed a non-linear complex. The bond angle of Fe–O–Fe is 163.9(4). The data of EA and IR are in good agreement with the crystal structure. The thermal gravity (TG) data indicate that there are four decomposition steps with three endothermic peaks. The final product of the thermal decomposition may be Fe(C₂H₈N₂)SO₄.     

Crystal structure of copper(II) bis-hexafluoroacetylacetonate

An X-ray diffraction investigation has performed for copper(II) bis-hexafluoroacetylacetonate (Bruker AXS P4 automatic diffractometer, MoK radiation, t = –25°C). Crystal data for C₁₀H₂CuF₁₂O₄: a = 5.530(1) Å, b = 6.038(1) Å, c = 11.266(2) Å, = 95.948(3)°, = 101.743(3)°, = 92.298(3)°, space group; P1, V = 365.6(1) ų, Z = 1, d _calc = 2.169 g/cm³. The square-planar environment of the copper atom (Cu-O_av 1.912 Å, O-Cu-O_av 93°) is completed to bipyramidal by two fluorine atoms of the neighboring molecules, Cu...F 2.71 Å and 2.75 Å.Original Russian Text Copyright © 2004 by S. A. Gromilov, I. A. Baidina, P. A. Stabnikov, and G. V. RomanenkoTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 3, pp. 502–507, May–June 2004.     

Structure and Spectroscopic Characteristics of N,N′-bis(2-Hydroxy-3-methoxyphenylmethylidene)2,6-pyridinediamine

The Schiff base N,N-bis(2-hydroxy-3-methoxyphenylmethylidene)-2,6-pyridinediamine has been synthesized and characterized in the solid state and in solution using X-ray analysis, IR, UV/Vis, and NMR spectroscopy. Crystal data: C₂₁H₁₉N₃O₄, M _r = 377.39, orthorhombic, space group Pnc2, a = 4.9288(8), b = 8.8873(19), c = 20.870(5) Å, V = 914.19(20) ų, Z = 2, R = 0.0387, R _w = 0.0530, 1845 independent reflections, 778 with I > 2(I). There are two intramolecular hydrogen bonds O—H-N between the hydroxyl and imino groups of 2.622(3) Å. The enolimine form is found in the solid state and is also the predominant tautomeric form in solution. Comparison of the title compound with the structurally related N,N-bis(salicylidene)-2,6-pyridinediamine and N,N-bis(salicylidene)-2,3-pyridinediamine is given.     

Inclusion of ibuprofen by heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin: An X-ray diffraction and thermal analysis study

Inclusion of the non-steroidal anti-inflammatory drug ibuprofen by permethylated-cyclodextrin (TRIMEB) was investigated by thermal analysis and X-ray diffraction. Reaction between racemic ibuprofen and TRIMEB yielded a mixture of isomorphous crystals of TRIMEB - (R)-ibuprofen and TRIMEB — (S)-ibuprofen. The single crystal chosen for X-ray analysis was found to contain the (S)-isomer of the drug. The crystal is orthorhombic, space groupP2₁2₁2₁, witha = 15. 232(7) Å,b = 21.327(7) Å,c = 27.597(7) Å andZ = 4. The structure was solved using the coordinates for the rigid portion of the cyclodextrin molecule of the isomorphous complex with (S)-naproxen. Refinement by full-matrix least-squares techniques gave a finalR factor of 0.079 for 7473 unique observed reflections. The isobutyl group of (S)-ibuprofen is included in the cyclodextrin cavity through hydrophobic forces, with the propionic acid group protruding from theO(2),O(3) face. The lack of chiral discrimination of the host TRIMEB towards ibuprofen as guest was confirmed by a combination of X-ray diffraction methods, thermal analysis and polarimetry.     

Synthesis,crystal structure and conformation of N-acetyl-Cα,α-diethylglycine-N′-methylamide

Summary Synthesis and X-ray structure analysis of N-acetyl-^,-diethylglycine-N-methylamide [CH₃-Co-NH-C(C₂H₅)₂-CO-NHCH₃] are described. The compound was obtained from the corresponding N-acetyl derivative [CH₃-CO-NH-C(C₂H₅)₂-COOH] through the mixed anhydride procedure. It crystallizes as monohydrate (C₉H₁₈N₂O₂·H₂O) in space group P2₁/c,a=7.139(1),b=11.823(2),c=15.778(3) Å, =122.23(1)°,V=1126.53 ų,D _m=1.20 Mgm^–3 (room temperature),R=0.046 for 1523 reflections. The crystal packing is dominated by two strong hydrogen bonds between the water molecule and two carbonyl oxygen atoms and two weak H-bonds to two amide-N-atoms of symmetry-equivalent molecules. The molecular conformation is closer to a 3₁₀-helix then ana-helix.

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Synthese, Kristallstruktur und Konformation von N-Acetyl-^,-diethylglycin-N-methylamid

Zusammenfassung Es wird über Synthese und die röntgenographische Strukturbestimmung von N-Acetyl-^,-diethylglycin-N-methyl-amid [CH₃-CO-NH-C(C₂H₅)₂-CO-NH-CH₃] berichtet. Die Verbindung wurde unter Anwendung der Methode der gemischten Anhydride aus dem entsprechenden N-Acetylderivat [CH₃-CO-NH-C(C₂H₅)₂-COOH] erhalten. Sie kristallisiert als Monohydrat (C₉H₁₈N₂O₂·H₂O) in der Raumgruppe P2₁/c mita=7.139(1),b=11.823(2),c=15.778(3) Å, =122.23(1)°,V=1126.53 ų,D _m=1.20 Mgm^–3,D _x=1.204 Mgm^–3 (Raumtemperatur).R=0.046 für 1523 Reflexe. Die Kristallpackung ist dominiert durch zwei starke H-Brücken vom Wassermolekül zu zwei Carbonylsauerstoffatomen sowie zwei schwachen H-Brücken zu zwei Amid-N-atomen symmetrieequivalenter Moleküle. Die Konformation des Peptidgerüstes ist näher einer 3₁₀ als einera-Helix.

     

Crystal structure and spectra of the Ni(II) complex of pyridine-2,6-dithio-carbomethylamide

The crystal structure of the paramagnetic bis(pyridine-2,6-dithiocarbomethylamide) nickel(II) nitrate (NiPDTA) is described: C₁₈H₂₂N₆S₄·(NO₃)₂·(H₂O)_1,5, monoclinic, C2/c,Z=4,a=14.705 (3) Å,b=23.254 (8) Å,c=8.383 (3) A, =98.18 (2)°,d _x=1.55 gcm^–3,d _m=1.53 gcm^–3. The structure was solved withPatterson and differenceFourier techniques and refined to a residual ofR=0.053. The nickel is surrounded by a square bipyramidal coordination of four thioamide sulfur atoms and two pyridine nitrogen atoms. Vibrational and electronic band positions for this compound are discussed.

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Kristallstruktur und Spektren des Pyridin-2,6-dithiocarbomethylamid Nickel(II)-Komplexes

Zusammenfassung Die Kristallstruktur des paramagnetischen bis(Pyridin-2,6-dithiocarbomethylamid) Nickel(II)-nitrats (NiPDTA) wurde bestimmt. C₁₈H₂₂N₆S₄Ni·(NO₃)₂·(H₂O)_1,5, monoklin, C2/c,Z=4,a=14,705 (3) Å,b=23,254 (8) Å,c=8,383 (3) A, =98,18 (2)°,d _x=1,55gcm^–3,d _m=1,53gcm^–3. Das Phasenproblem wurde mittelsPatterson-und Differenz-Fourier-Synthese bestimmt und die Struktur bis zu einem kristallographischenR-Faktor vonR=0.053 verfeinert. Das Nickel-Atom ist von vier Thioamid-Schwefelatomen und zwei Pyridin-Stickstoffatomen in quadratisch-bipyramidaler Anordnung umgeben. Schwingungsspektren und Anregungsspektren des Komplexes werden diskutiert.

     

Molecular structure of 1′,3′,3′-trimethyl-6-trifluoromethylsulfonyl-spiro-(indoline-2,2′-benzo[b]pyran)

Photochromic 1, 3, 3 -trimethyl-6-trifluoromethylsulfonyl-spiro(indoline-2,2-ben-zo[b]pyran) (1) was studied by X-ray diffraction analysis. In compound1, the C_spiro-O bond (1.49(1) Å (average)), broken on photoexcitation, is the longest of all the indoline spiropyrans studied.Translated fromIzyestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 1969–1971, November, 1994.