Crystal structure,infrared and raman spectra of tripotassium trisaccha-rinate dihydrate,K<Subscript>3</Subscript>(C<Subscript>7</Subscript>H<Subscript>4</Subscript>NO<Subscript>3</Subscript>S)<Subscript>3</Subscript>·2H<Subscript>2</Subscript>O

The crystal structure of tripotassium trisaccharinate dihydrate, K₃(C₇H₄NO₃S)₃·2H₂O, is triclic, space group\(P \bar 1, Z = 2\). It consists of three crystallographically independent potassium and saccharinato ions as well as two structurally different water molecules. Potassium coordination polyhedra are irregular, with K1 and K3 six-coordinated and the third one K2 seven-coordinated. The K?O distances range from 2.652(9) to 3.100(2) Å(mean: 2.790 Å) whereas the K?N distance is 3.025(3) Å. The water molecules W2 is disordered over three positions with occupancies of approximately 0.6, 0.2 and 0.2. The hydrogen atom (H1W1) of the ordered water molecule (O1W) is hydrogen bonded to the sulfonyl oxygen atom (O11) (R(O...O)=2.976(3) Å), whereas the other hydrogen atom (H2W1) is bifurcated to the carbonyl oxygen atom (O13) (R(O...O)=2.851(3) Å) and the disordered water molecules (O23W) (R(O...O)=3.067(12) Å). The carbonyl oxygens (O13, O23 and O33) and one of the disordered water molecules (O22W) are involved in C?H...O hydrogen bonds (R(C?H...O)=3.027(4)–3.304(9) Å). Structural characteristics of the studied compound are compared with the analogous trisodium trisaccharinate dihydrate and dipotassium sodium trisaccharinate monohydrate. Infrared and Raman spectra of the title compound have been analyzed in relation to the structure, and compared with the spectra of trisodium trisaccharinate dihydrate.     

Röntgenstrukturanalyse von N-((E)-2-Methyl-2-butenyl)-N-(4-methylphenylsulfonyl)-N′-(4-nitrophenyl)schwefeldiamid

X-Ray Structure Analysis of N-((E)-2-Methyl-2-butenyl)-N-(4-methylphenylsulfonyl)-N′-(4-nitrophenyl)sulfurdiamide The title compound crystallizes in the monoclinic space group P2₁/n with a = 16.893(3), b = 14.285(2), c = 18.422(4), β = 114.765(5)°, V = 4037 ų, Z = 8. The formal S? N single bonds of the diaminosulfane moiety are shortened and differ in length (1.700 and 1.644 Å). The bonds of the N? S? N group to the p-nitrophenyl and tosyl rest are also a bit shorter than single bonds. The hybridization of the N atoms of the N? S? N moiety is sp² with a tendency in the direction of sp³. Analogously to open chained sulfur diimides with respect to the N? S? N moiety an E/Z configuration can be derived. In the crystal structure the molecules are connected to one-dimensional polymers via hydrogen bridges between the nitrogen of the secondary amino group as a donor and an oxygen of the nitro group as an acceptor.     

Kristallstrukturen von Säurehydraten und Oxoniumsalzen. XX. Die Oxoniumtetrafluoroborate H3OBF4, [H5O2]BF4 und [H(CH3OH)2]BF4

Crystal Structures of Acid Hydrates and Oxonium Salts. XX. Oxonium Tetrafluoroborates H₃OBF₄, [H₅O₂]BF₄, and [H(CH₃OH)₂]BF₄ The crystal structures of three oxonium tetrafluoroborates were determined. H₃OBF₄, oxonium tetrafluoroborate proper, is triclinic with space group P1 , Z = 2 and the unit cell dimensions a = 4.758, b = 6.047, c = 6.352 Å and α = 80.40, β = 79.48, γ = 88.25° at ?26°C. Cations H₃O⁺ and anions BF₄^? are linked by hydrogen bonds O? H…?F into ribbons of condensed rings. In [H₅O₂]BF₄ (diaquohydrogen tetrafluoroborate, monoclinic, P2₁/c, Z = 4, a = 6.584, b = 9.725, c = 7.084 Å, β = 95.15° at ?100°C) the hydrogen bond in the cation H₅O₂⁺ is 2.412 Å short, asymmetric and approximately centered and the linking of cations and anions three-dimensional. In [H(CH₃OH)₂]BF₄ (Bis(methanol)hydrogen tetrafluoroborate, monoclinic, P2₁/c, Z = 4, a = 5.197, b = 14.458, c = 9.318 Å, β = 94.61° at ?50°C) the cation [H(CH₃OH)₂]⁺ is characterized for the first time in a crystal structure with an again very short (2.394 Å), asymmetric and effectively centered hydrogen bond. By further hydrogen bonds cations and anions form only dimers of the formula unit of centrosymmetric cyclic structure.     

Crystal and molecular structure and vibrational spectra of 2,6-bis(diphenylphosphorylmethyl)-4-methylphenol and its complex with cerium(III) nitrate

The structure of 2,6-bis(diphenylphosphorylmethyl)-4-methylphenol 2,6-[Ph₂P(O)CH₂]₂-4-MeC₆H₂OH(L¹) and its 1: 1 complex with cerium(III) nitrate were studied by X-ray diffraction. A rather strong intramolecular hydrogen bond P=O…H-O (O…O, 2.646(1) Å) exists in the L¹ molecules. In the crystal, the molecules are combined into centrosymmetric dimers through the stacking interaction between the central phenol rings; the distance between the ring planes is 3.39 Å. In the complex molecule, [Ce(L¹)(NO₃)₃ · Me₂C(O)], the neutral ligand L¹ is tridentate and the three nitrate ions are bidentate, and the tenth coordination site is occupied by acetone oxygen. No intramolecular H-bonds are present. In the crystal, the complex molecules are combined into centrosymmetric dimers through intermolecular hydrogen bonds O-H…O-NO₂ (O…O, 2.713(8) Å). The vibrational (IR, Raman) spectra of the ligand and the complex were studied and the principal bands were assigned. According to IR spectroscopy, the P=O…H-O intramolecular hydrogen bond is retained in both the ligand and the complex molecules.     

Darstellung und Kristallstruktur von Tetraphenylphosphonium-Hexathiocyanatorhodat(III), [P(C6H5)4]3[Rh(SCN)6]

Preparation and Crystal Structure of Tetraphenylphosphonium Hexathiocyanatorhodate(III), [P(C₆H₅)₄]₃[Rh(SCN)₆] By treatment of RhCl₃ · n H₂O with KSCN in water a mixture of the linkage isomers [Rh(NCS)_n(SCN)_6–n]^3?, n = 0–2 is formed which is separated by ion exchange chromatography on diethylaminoethyl cellulose. The X-ray structure determination on a single crystal of [P(C₆H₅)₄]₃[Rh(SCN)₆] (monoclinic, space group C1c1, a = 13.620(5), b = 22.929(13), c = 22.899(9) Å, β = 98.55(3)°, Z = 4) confirms the coordination of all ligands via S with the middle Rh? S distance of 2.372 Å and Rh? S? C angles of 109°. The SCN groups are nearly linear with 175° and averaged bondlengths S? C 1.63 and C? N 1.14 Å. The crystal lattice is build up by layers of complex anions and voluminous cations with no specific interactions but which are closely connected by thiocyanate ligands and phenyl rings.     

Kaliumamidotrioxogermanate(IV) – Wasserstoff-Brückenbindungen in K3GeO3NH2 und K3GeO3NH2 · KNH2

Potassium Amido Trioxo Germanates(IV) – Hydrogen Bridge Bonds in K₃GeO₃NH₂ and K₃GeO₃NH₂ · KNH₂ Colorless crystals of K₃GeO₃NH₂ and of K₃GeO₃NH₂ · KNH₂ were obtained by the reaction of KNH₂ with GeO₂ in supercritical ammonia at 450°C and p = 6 kbar in high-pressure autoclaves within 15 resp. 5 days. The crystal structures of both compounds were solved by X-ray single crystal methods. K₃GeO₃NH₂: P1 , a = 6.390(1) Å, b = 6.684(1) Å, c = 7.206(1) Å, α = 96.47(1)°, β = 101.66(1)°, γ = 91.66(1)°, Z = 2, R/R_w = 0.020/0.022, N(I) ≥ 2σ(I) = 3023, N(Var.) = 82 K₃GeO₃NH₂ · KNH₂: P2₁/c, a = 10.982(6) Å, b = 6.429(1) Å, c = 12.256(8) Å, β = 106.12(1)°, Z = 4, R/R_w = 0.022/0.029, N(F) ≥ 3σ(F) = 1745, N(Var.) = 107. In K₃GeO₃NH₂ tetrahedral ions GeO₃NH₂^3? are connected to chains by N? H …? O bridge bonds with 2.18 Å ≤ d(H …? O) ≤ 2.40 Å for d(N? H) ? 1.0 Å and by potassium ions while in K₃GeO₃NH₂ · KNH₂ bridge bonds between NH₂ groups of GeO₃NH₂^3? and NH₂^? ions as acceptors occur with 2.41 Å ≤ d((N? )H …? NH₂^?) ≤ 2.61 Å for d(N? H) ? 1.0 Å.     

Crystal structures of the pyrazinamide–p‐aminobenzoic acid (1/1) cocrystal and the transamidation reaction product 4‐(pyrazine‐2‐carboxamido)benzoic acid in the molten state

The synthesis of pharmaceutical cocrystals is a strategy to enhance the performance of active pharmaceutical ingredients (APIs) without affecting their therapeutic efficiency. The 1:1 pharmaceutical cocrystal of the antituberculosis drug pyrazinamide (PZA) and the cocrystal former p‐aminobenzoic acid (p‐ABA), C₇H₇NO₂·C₅H₅N₃O, (1), was synthesized successfully and characterized by relevant solid‐state characterization methods. The cocrystal crystallizes in the monoclinic space group P2₁/n containing one molecule of each component. Both molecules associate via intermolecular O—H...O and N—H...O hydrogen bonds [O...O = 2.6102 (15) Å and O—H...O = 168.3 (19)°; N...O = 2.9259 (18) Å and N—H...O = 167.7 (16)°] to generate a dimeric acid–amide synthon. Neighbouring dimers are linked centrosymmetrically through N—H...O interactions [N...O = 3.1201 (18) Å and N—H...O = 136.9 (14)°] to form a tetrameric assembly supplemented by C—H...N interactions [C...N = 3.5277 (19) Å and C—H...N = 147°]. Linking of these tetrameric assemblies through N—H...O [N...O = 3.3026 (19) Å and N—H...O = 143.1 (17)°], N—H...N [N...N = 3.221 (2) Å and N—H...N = 177.9 (17)°] and C—H...O [C...O = 3.5354 (18) Å and C—H...O = 152°] interactions creates the two‐dimensional packing. Recrystallization of the cocrystals from the molten state revealed the formation of 4‐(pyrazine‐2‐carboxamido)benzoic acid, C₁₂H₉N₃O₃, (2), through a transamidation reaction between PZA and p‐ABA. Carboxamide (2) crystallizes in the triclinic space group P with one molecule in the asymmetric unit. Molecules of (2) form a centrosymmetric dimeric homosynthon through an acid–acid O—H...O hydrogen bond [O...O = 2.666 (3) Å and O—H...O = 178 (4)°]. Neighbouring assemblies are connected centrosymmetrically via a C—H...N interaction [C...N = 3.365 (3) Å and C—H...N = 142°] engaging the pyrazine groups to generate a linear chain. Adjacent chains are connected loosely via C—H...O interactions [C...O = 3.212 (3) Å and C—H...O = 149°] to generate a two‐dimensional sheet structure. Closely associated two‐dimensional sheets in both compounds are stacked via aromatic π‐stacking interactions engaging the pyrazine and benzene rings to create a three‐dimensional multi‐stack structure.     

Darstellung und Kristallstruktur von (n-Bu4N)3[Ir(NCS)(SCN)5]

Preparation and Crystal Structure of (n-Bu₄N)₃[Ir(NCS)(SCN)₅] The evaporated ethanolic extrakt of the reaction product of K₃[IrCl₆] and HNO₃, refluxed with an aqueous KSCN solution yields a mixture of the linkage isomers [Ir(NCS)_n(SCN)_6?-n]^3?, n = 0? 2, and small amounts of linkage isomeric chloropentarhodanoiridates(III), from which [Ir(NCS)(SCN)₅]^3? has been isolated by ion exchange chromatography on DEAE-cellulose. The X-Ray structure determination on a single crystal of (n-Bu₄N)₃[Ir(NCS)(SCN)₅] (monoclinic, space group P 2₁/a, a = 17.513(5), b = 32.607(5), c = 23.661(5) Å, β = 94.757(5)°, Z = 8) confirms the existance of a heteroleptic hexakis(thiocyanato(N)-thiocyanato(S))iridate(III) with an Ir? N distance of 2.03 Å and Ir? S bond lengths between 2.29 and 2.38 Å. The SCN groups with angles between 166 and 175° are nearly linear with Ir? S? C angles from 99.9 to 109.4°. The Ir? N? C angles of the two crystallographic independent anions are 166 and 174°.     

Modellkomplexe mit Hydrazonchelaten von (S)- und (R)-1-Amino-2-methoxymethylpyrrolidin („SAMP”︁ und „RAMP”︁) und Dimethylhydrazin - Struktur des Pyridinaldehyd-RAMP-hydrazon-tetracarbonyl-molybdäns

Model Complexes with Hydrazone Chelates of (S)- and (R)-1-Amino-2-methoxymethylpyrrolidine (?SAMP”? and ?RAMP”?) and Dimethylhydrazine — Structure of (Pyridine-2-aldehyde-RAMP-hydrazone)tetracarbonyl-molybdenum The hydrazones of glyoxal, biacetyl, pyridine-2-aldehyde and 2-acetylpyridine with N,N-dimethylhydrazine and (R)- and (S)-1-amino-2-methoxymethylpyrrolidine are synthesized and reacted with hexacarbonylmolybdenum to give the chelate hydrazone tetracarbonylmolybdenum complexes. In contrast to the pure electronic effect of methyl groups complexes derived from biacetyl (relativ to glyoxal) or from acetylpyridine (rel to the aldehyde) show a long-wavelength shift of the characteristic MLCT absorption band in their electric spectra, indicativ of a dominant steric effect. A single crystal x-ray diffraction study on (pyridine-2-aldehyde-RAMP-hydrazone)tetracarbonylmolybdenum 12 proves the conjugative interaction of the sp²-hybridized amino nitrogen with the chelate π-system. Orthorhombic 12 crystallizes in space group P2₁2₁2 with 4 molecules in the unit cell: a = 14.689(4), b = 15.699(1) and c = 7.866(6) Å, V = 1814 ų. Complete ¹H and ¹³C nmr parameter are given for the ligands and the complexes.     

Darstellung und Struktur eines Ammoniumdiamidodioxophosphats(V), NH4PO2(NH2)2

Synthesis and Structure of an Ammonium Diamidodioxophosphate(V), NH₄PO₂(NH₂)₂ The ammonolysis of P₃N₅ under ammonothermal conditions (T = 400°C, p(NH₃) = 6 kbar, 14 d in autoclaves) in the presence of small definite amounts of water leads to the formation of NH₄PO₂(NH₂)₂. The structure was solved by single crystal X-ray methods. NH₄PO₂(NH₂)₂: P2₁/c (Nr. 14), a = 6.886(1) Å, b = 8.366(2) Å, c = 9.151(2) Å, β = 111.78(3)°, Z = 4, R₁/wR₂ = 0.026/0.072, Z(F > 2σ(F)) = 1183, N(variables) = 87. In NH₄PO₂(NH₂)₂ the anions [PO₂(NH₂)₂]^? are linked to chains by N? H …? N and N? H …? O bridge bonds. The ammonium ions are located between these chains and are donors for N? H …? O bridge bonds which connect the chains three-dimensionally.     

Contributions to the Chemistry of Silicon—Sulphur Compounds. 66. Synthesis,crystal and molecular structure of bis(tri-tert-butoxysilanethiolato)(acetonitrile)cobalt(II)[(t-C4H9O)3SiS]2Co(NCCH3)

The title compound [(t-C₄H₉O)₃SiS]₂Co(NCCH₃)] 1 was obtained by reaction of anhydrous cobalt(II) chloride with tri-tert-butoxysilanethiol and triethylamine in acetonitrile as a solvent. The compound crystallizes as deep-blue orthorhombic plates with a = 17.779(4), b = 45.363(9), c = 9.096(2) Å, space group Fdd2 and Z = 8. The structure was solved by Patterson synthesis and refined to the R value of 0.0343. The crystal consists of mononuclear complexes in which the cobalt atom is five-fold coordinated to two sulphurs, two oxygens and one nitrogen in a distorted trigonal bipyramidal arrangement. The relevant bond distances and angles are: Co? S, 2.2680(7); Co? N, 2.065(4); Co? O1, 2.283(2); S? Si, 2.0666(8) Å; S? Co? S′, 119.14(4); N? Co? S, 120.43(2); O1? Co? O1′, 178.81(10)°.     

Deprotonierte Dithiocarbaminsäureester als Thiolat-S-Donor-Liganden. Strukturen von Ph(H)NC(S)SMe,Co(PhNC(S)SMe)3 und Cu6(PhNC(S)SMe)6

Deprotonated Dithiocarbamic Acid Esters as Thiolate S-Donor Ligands. Structures of Ph(H)NC(S)SMe, Co(PhNC(S)SMe)₃, and Cu₆(PhNC(S)SMe)₆ The reaction of N-phenyl-S-methyldithiocarbamate, PhN(H)C(?S)SMe, ( 1 ) with cobalt(II) and copper(II) salts yields the monomeric compound Co^III(PhNC(S)SMe)₃ ( 2 ) and the hexameric compound Cu₆^I(PhNC(S)SMe)₆ ( 3 ). These complexes contain the negatively charged imino-thiolate ligand PhN?C(? S)SMe, which has been formed by deprotonation of 1 . The crystal structures of 1 – 3 have been determined. 1 forms centrosymmetrical dimers through N? H …? S bridge bonds, the conformation in the solid state and in solution is Z,E′. Co^III shows in 2 a trigonal-antiprismatic coordination, with the ligands acting as N,S-chelates. 3 contains an octahedral Cu₆-core with Cu …? Cu-distances ranging from 276.3(5) to 305.7(4) pm. Each copper center is trigonally coordinated to one nitrogen and two sulfur atoms of three different ligands. Crystal data: 1 , triclinic, space group P1 , a = 590.5(6), b = 869.0(1), c = 968.5(9) pm, α = 67.29(8), β = 78.44(8), γ = 81.64(9)°, Z = 2, 1 775 reflections, R(R_w) = 0.0317(0.032). 2 , orthorhombic, space group Pbca, a = 978.0(2), b = 1 842.9(4), c = 3 059.7(6) pm, Z = 8, 1 129 reflections, R(R_w) = 0.0997(0.0886). 3 , monoclinic, space group P2₁/c, a = 1 363.1(3), b = 1 342.8(3), c = 1 671.9(3) pm, β = 103.48°, Z = 2, 1 374 reflections, R(R_w) = 0.0708(0.0617).     

Synthesis,crystal structure and luminescence of a 3-D coordination polymer based on 4-(1H-tetrazol-5-yl) benzoic acid

A cobalt(II) coordination polymer [Co(4-TZBA^2?)(H₂O)₂] (1) was obtained by treatment of Co(ClO₄)₂ · 6H₂O with 4-(1H-tetrazol-5-yl)benzoic acid [H₂(4-TZBA)] under hydrothermal conditions. The X-ray single crystal diffraction analysis reveals that 1 crystallizes in monoclinic P2₁/c, with a = 10.503(2) Å, b = 9.0860(18) Å, c = 10.179(2) Å, β = 96.75(3)° and Z = 4. In 1, adjacent cobalt(II) atoms are bridged by two 4-TZBA^2? ligands to form a dimer, which is linked with six dimers to result in a 3-D structure. 1 exhibits strong luminescence at room temperature in the solid state.     

Preparation,X-ray crystal structure and 13C- and 1H-NMR study of 1-methyl-2-(N-methyl-N-phenylglycyl)-3-(N-methylanilino)indole

Reaction of N-methylaniline with 40% glyoxal yields 1-methyl-2-(N-methyl-N-phenylglycyl)-3-(N-methylanilino)indole ( 1a ) as the main product together with 1-methyl-3-(N-methylanilino)indole ( 1b ). The reaction appears to be general for aromatic secondary amines since N-ethylaniline and N-phenylbenzylamine yield the corresponding indoles. The structure of 1a has been verified by single crystal X-ray diffraction. Compound 1a (C₂₅H₂₅N₃O) crystallized in the triclinic space group Pl? with cell dimensions a = 10.085(3)Å, b = 10.371(3)Å, c = 11.908(5)Å, α = 74.2(3)°, β = 74.7(3)° and γ = 60.7(2)° with Z = 2. The complete ¹H and ¹³C nmr assignment of indoles 1a and 1b was achieved from two-dimensional HETCOR and COSY spectra with the aid of homonuclear and heteronuclear double resonance experiments.     

4‐Iodo­anilinium 3‐nitro­phthalate(1–): tripartite sheets built from O—H...O and N—H...O hydrogen bonds

In the title compound, 4‐iodoanilinium 2‐carboxy‐6‐nitrobenzoate, C₆H₇IN⁺·C₈H₄NO₆⁻, the anions are linked by an O—H...O hydrogen bond [H...O = 1.78 Å, O...O = 2.614 (3) Å and O—H...O = 171°] into C(7) chains, and these chains are linked by two two‐centre N—H...O hydrogen bonds [H...O = 1.86 and 1.92 Å, N...O = 2.700 (3) and 2.786 (3) Å, and N—H...O = 153 and 158°] and one three‐centre N—H...(O)₂ hydrogen bond [H...O = 2.02 and 2.41 Å, N...O = 2.896 (3) and 2.789 (3) Å, N—H...O = 162 and 105°, and O...H...O = 92°], thus forming sheets con­taining R(6), R(8), R(13) and R(18) rings.     

Über Chalkogenolate. 152. Untersuchungen über Derivate der N-Thioformyldithiocarbamidsäure. 2. Kristallstruktur von Tetra-n-butylammonium-N-thioformyldithiocarbamat

On Chalcogenolates. 152. Studies on Derivatives of N-Thioformyl Dithiocarbamic Acid. 2. Crystal Structure of Tetra-n-butylammonium N-Thioformyl Dithiocarbamate The title compound [N(ⁿC₄H₉)₄][S₂C? NH? CS? H] crystallizes with Z = 2 in the triclinic space group P1 with cell dimensions a = 9.694(2) Å, b = 11.478(3) Å, c = 12.551(6) Å, α = 63.03(3)°, β = 66.42(2)°, γ = 85.60(2)°. The crystal structure has been determined from single crystal X-ray data measured at 20°C and refined to a conventional R of 0.061 for 2249 independent reflections (R_w = 0.042). The structure is built up of dimeric aggregates consisting of 2[N(ⁿC₄H₉)₄]⁺ cations and 2[S₂C? NH? CS? H]^? anions. The two anions are linked together by ? CS? S…?H? N bridges. To make possible a space saving stacking of the dimeric aggregates in the crystal, one methyl group in terminal position of one n-butyl chain in the cation has gauche conformation.     

Supramolecular Assemblies of Mononuclear and Polymeric Nickel(II) Glutarato Complexes via π‐π Stacking Interactions and Hydrogen Bonds: [Ni(H2O)3(phen)(C5H6O4)] · H2O and [Ni(H2O)2(phen)(C5H6O4)]

Syntheses of the sky blue complex compounds [Ni(H₂O)₃(phen)(C₅H₆O₄)] · H₂O ( 1 ) and [Ni(H₂O)₂(phen)(C₅H₆O₄)] ( 2 ) were carried out by the reactions of 1,10‐phenanthroline monohydrate, glutaric acid, NiSO₄ · 6 H₂O and Na₂CO₃ in CH₃OH/H₂O at pH = 6.9 and 7.5, respectively. The crystal structure of 1 (P 1 (no. 2), a = 14.289 Å, b = 15.182 Å, c = 15.913 Å, α = 67.108°, β = 87.27°, γ = 68.216°, V = 2934.2 ų, Z = 2) consists of hydrogen bonded [Ni(H₂O)₃‐ (phen)(C₅H₆O₄)]₂ dimers and H₂O molecules. The Ni atoms are octahedrally coordinated by two N atoms of one phen ligand, three water O atoms and one carboxyl O atom from one monodentate glutarato ligand (d(Ni–N) = 2.086, 2.090 Å; d(Ni–O) = 2.064–2.079 Å). Through the π‐π stacking interactions and intermolecular hydrogen bonds, the dimers are assembled to form 2 D layers parallel to (0 1 1). The crystal structure of 2 (P2₁/n (no. 14), a = 7.574 Å, b = 11.938 Å, c = 18.817 Å, β = 98.48°, V = 1682.8 ų, Z = 4) contains [Ni(H₂O)₂(phen)(C₅H₆O₄)_2/2] supramolecular chains extending along [010]. The Ni atoms are octahedrally coordinated by two N atoms of one phen ligand, two water O atoms and two carboxyl O atoms from different bis‐monodentate glutarato ligands with d(Ni–N) = 2.082, 2.105 Å and d(Ni–O) = 2.059–2.087 Å. The supramolecular chains are assembled into a 3 D network by π‐π stacking interactions and interchain hydrogen bonds. A TG/DTA of 2 shows two endothermic effects at 132 °C and 390 °C corresponding to the complete dehydration and the lost of phen.     

Crystal and molecular structure of methyl(±)-2-((1R,3R)-3-{ 2-[(3S)-1-ethyl-3-hydroxy-2-oxo-2,3-dihydro-1H-3-indolyl]acetyl}-2,2-dimethylcyclobutyl) acetate

The structure of methyl (±)-2-((1R,3R)-3-{ 2-[(3S)-1-ethyl-3-hydroxy-2-oxo-2,3-dihydro-1H-3-indolyl]acetyl}-2,2-dimethylcyclobutyl) acetate has been determined by single crystal X-ray diffraction. The crystal belongs to triclinic system; parameters of the unit cell are: a = 6.551(1) Å, b = 11.506(1) Å, c = 14.334(1) Å, α = 101.41(1)°, β = 97.57(1)°, γ = 104.72(1)°; space group P-1, Z = 2, composition C₂₁H₂₇NO₅. The structure of N-ethyloxindole fragment is usual for the present class of compounds. The configuration of the formed asymmetric carbon atom C(3) of the pyrrole ring along with the configuration of C(12) and C(14) atoms of 2,2-dimethylcyclobutane ring form the side chain of the molecule were determined. There is observed the generation of centrosymmetrical dimers in the crystal structure due to realized intermolecular hydrogen bond of O-H...O type, 2.808(2) Å.     

Crystal Structure and Spectroscopic Studies of a New Organic Dihydrogenmonophosphate [2-NH2-6-CH3-C4H3N2O]2(H2PO4)2

Physicochemical properties of a new dihydrogenmonophosphate [2-NH ₂ -6-CH ₃ -C ₄ H ₃ N ₂ O] ₂ (H ₂ PO ₄ ) ₂ are described on the basis of X-ray crystal structure investigation. This compound crystallizes in the triclinic space group P-1. The unit cell parameters are: a = 7.667(3) Å, b = 8.204(5) Å, c = 14.761(6) Å, α = 98.85(4)°, β = 99.23(3)°, γ = 90.50(4)°, V = 905.0 ų, and Z = 2. The crystal structure was solved and refined to R = 0.037, using 4351 independent reflections. The atomic arrangement of this compound is built up by (H ₂ PO ₄ ) _n ^{n ?} chains. Each chain aggregates with organic molecules to form an open framework architecture through hydrogen bond interactions. The structure includes four types of hydrogen bonds. The first one, O─H─O, links the H ₂ PO ₄ groups to form (H ₂ PO ₄ ) _n ^{n ?} infinite inorganic chains parallel to the a axis. The three other types, O─H─O(carbonylic), N─H─O(carbonylic), and N─H─O, assemble the inorganic chains so as to build up a three-dimensional arrangement. This compound has also been investigated by IR, and solid-state ¹³ C and ³¹ P MAS NMR spectroscopies combined to ab initio calculations.     

Crystal structures of bis(AZIDO)bis(2-morpholin-4-ylethylamino)copper(II) and bis{2,4-dibromo-6-[(2-morpholin-4-ylethylimino)methyl] phenolato}copper(II)

Two new copper(II) complexes [Cu(MEA)₂(N₃)₂] (1) and [Cu(BMP)₂] (2), where MEA and BMP are 2-morpholin-4-ylethylamine and 2,4-dibromo-6-[(2-morpholin-4-ylethylimino)methyl]phenolate respectively, are prepared and characterized using elemental analysis, FT-IR spectroscopy, and X-ray single crystal diffraction. The crystal of 1 belongs to the triclinic system, space group P-1, with a = 6.661(2) Å, b = 8.440(3) Å, c = 8.913(3) Å, α = 102.032(3)°, β = 107.899(2)°, γ = 98.242(3)°, V = 454.6(3) ų, Z = 1, D _c = 1.490 g/cm³, R ₁ = 0.0226, and wR ₂ = 0.0564. The crystal of 2 belongs to the monoclinic system, space group P2₁/c, with α = 7.0707(7) Å, b = 15.438(1) Å, c = 14.227(1) Å, β = 96.659(2)°, V = 1542.5(3) ų, Z = 2, D _c = 1.821 g/cm³, R ₁ = 0.0437, and wR ₂ = 0.1041. In each complex, the Cu atom is in a square planar coordination. The molecules of 1 are linked through intermolecular N-H...N and N-H...O hydrogen bonds to form layers parallel to the ab plane. The molecules of 2 are linked through intermolecular C-H...Br hydrogen bonds to form a 3D network.