Die Molekül- und Kristallstruktur des N-Methyl-piperidinium-acet-para-brom-anilid-jodid

N-Methyl-piperidinium-acet-para-bromo-anilide-iodide crystallizes in the triclinic space group P 1 with two formula units C₁₄H₂₀N₂OBrJ and two H₂O molecules in the unit cell. The lattice constants are a = 8.950 Å, b = 14.721 Å, c = 7.440 Å, α = 80.19°, β = 112.57° and γ = 106.82°. The molecular structure of the compound was determined by the X-ray structure analysis and the interaction between the molecules in the crystal was investigated. Especially the influence of the water in the crystal on the form of the molecule was analysed.     

Crystal and Molecular Structure of Non-hydrated and Hydrated Piperidinium-acet-o-Cl-anilide-chloride

Crystallizations from water and alcoholic solution respectively yield different crystal and molecular structures of Piperidinium-acet-o-Cl-anilide-chloride. The non-hydrated compound crystallizes from alcoholic solution in the space group P 2₁/c with 4 formula units C₁₃H₁₈N₂OCl₂ in the unit cell of dimensions a = 12.352 Å, b = 6.864 Å, c = 19.018 Å and β = 113.98°. The hydrated modification has the space group C 2/c with 8 formula units C₁₃H₁₈N₂OCl₂ and 8 H₂O molecules in the unit cell. The lattice constants are a = = 24.159 Å, b = 8.966 Å, c = 14.179 Å and β = 90.50°. The X-ray structure analyses were carried out to investigate the hydrogen bonds and the change of the molecular conformation caused by linking of water molecules to the drug molecules.     

The Crystal and Molecular Structure of the Complex Diaquatetrakis(imidazole)copper(II) Terephthalate Crystal Structure Containing Cu(II) Him and TA

The title compound has been synthesized and its crystals structure determined at room temperature. MW = 536.01, monoclinic, space group C2/c, Z = 4, a = 22.193(5) Å, b = 8.038(2) Å, c = 15.699(4) Å, β = 119.64(2)°. The crystal structure consists of repeated [Cu(Him)₄(H₂O)₂] (Him = imidazole) cations and non-coordinated terephthalato dianions. The copper(II) ion displays an elongated octahedral coordination being linked to the four nitrogen atoms of the four imidazole ligands and to the two oxygen atoms of the two water molecules. The terephthalato dianions are hydrogen bonded to the four water molecules and four imidazole groups.     

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.     

Crystal and molecular structure of N-(Diethylaminothiocarbonyl)-N′-phenyl-benzamidine

The crystal structure of the title compound has been determined by X-ray diffractometer data collected on a CAD-4 diffractometer. C₁₈H₂₁N₃S crystallizes monoclinic, space group P 2₁/n with a = 8.939(1) Å, b = 18.992(3) Å, c = 10.416(2) Å, β = 97.29(2) Å and Z = 4. Least-squares refinement gave a value of R = 0.107 for 2647 observed reflections. The molecule has a configuration which can be described best by Z, E′ and exists in the tautomeric enamine form. The molecules form infinite chains connected by intermolecular N—H … S interactions, with H … S distances of 2.46 Å.     

Crystal and molecular structure of the chiral compound 4–(2–methylbutyloxy)phenyl–4–(2-propenyloxy)-benzoate,C21H24O4

The enantiomeric [(S)-(–)-MBP3B] and the racemic form [(±)-MBP3B] of the title compound with the formula C₃H₅O–C₆H₄–CO₂–C₆H₄–OC₅H₁₁ were studied by single crystal analysis at room temperature. (S)-(–)-MBP3B crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 7.835(3) Å, b = 11.093(6) Å, c = 44.820(3) Å and 8 molecules per unit cell. The structure was determined from 966 reflections with intensities > 3σ. The refinement with isotropic temperature factors leads to R = 0.094. The crystals of the racemic form are monoclinic, space group P2₁/a with a = 7.899(5) Å, b = 11.046(6) Å, c = 22.845(12) Å, β = 99.28(3)°, Z = 4.1236 diffractometer data (I > 3σ) were refined by least-squares methods with anisotropic temperature factors for the non-H atoms to R = 0.070. The packing arrangement for both forms shows a layer-like structure with very similar packing coefficients, k = 0.7085 for the pure enantiomer and k = 0.7014 for the racemic form.     

The Crystal and Molecular Structure of 4-Hydroxy-4′-nitro- biphenyl and its Potassium Salt

The crystal and molecular structures of the title compounds have been solved by single crystal X-ray analysis. 4-Hydroxy-4′-nitro-biphenyl (NBO) crystallizes in the centrosymmetric, monoclinic space group P2₁/n with a = 6.036(4) Å, b = 12.392(3) Å, c = 13.346(8) Å, β = 96.46(3)° and 4 molecules in the unit cell. Its potassium salt (NBOK) similarly belongs to P2₁/a with a = 11.277(2) Å, b = 7.3606(6) Å, c = 14.383(3) Å, β = 107.804(7)° and also 4 molecules in the unit cell. The structure of NBO was refined by full matrix least-squares calculation to R = 0.043 for 1105 observed reflections, the structure of NBOK to R = 0.041 for 2288 observed reflections, respectively. NBO and NBOK crystallize in layer-like structures. The biphenyl molecules of NBO are arranged as corrugated ribbons in layers. The ionic and polar moiety of NBOK (potassium, oxygen, and crystal water) are separated by biphenyl units to form layers. The almost planar biphenyl units of NBOK are arranged in pairs and exhibit a short molecular distance of 3.08 Å within one pair.     

Crystal structures of four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium

Herein four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium, 2(CH₃)₄N⁺·C₁₄H₈O₄S₂^2?·H₂O (1), (C₂H₅)₄N⁺·C₁₄H₉O₄S₂^?·0.25H₂O(2), (n-C₃H₇)₄N⁺·C₁₄H₉O₄S₂^? (3) and (n-C₄H₉)₄N⁺·C₁₄H₉O₄S₂^?(4) are prepared and characterized by X-ray single crystal diffraction. As shown in the results, compounds 1 and 3 belong to orthorhombic crystal system with different space groups of P2₁2₁2₁ and Pca2₁, and 2 and 4 are monoclinic system with similar groups of P2₁/n and P2₁/c. The crystallography data are displayed below: 1: a = 10.5903(7) Å, b = 10.6651(7) Å, c = 21.9476(13) Å, V = 2478.9(3) ų, Z = 4, R₁ = 0.0359; 2: a = 8.13340(1) Å, b = 22.0741(3)Å, c = 13.2143(2)Å, β = 101.6360(1) °, V = 2323.70(6) ų, Z = 1, R₁ = 0.0385; 3: a = 15.7857(2) Å, b = 8.24830(1) Å, c = 20.2599(2) Å, V = 2637.94(5) ų, Z = 4, R₁ = 0.0308_degree4: a = 11.7476(2) Å, b = 17.1346(1) Å, c = 16.3583(3)Å, β = 109.4560(1) °, V = 3104.74(9)ų, Z = 4, R₁ = 0.0562. Interestingly, although the carbon chains of the guest templates vary from methyl group to butyl group, the host molecules of 2,2′-dithiosalicylic acid all construct the similar 2D hydrogen-bonded host layers with or without the existence of water molecules to contain the guest templates to yield analogous sandwich-like inclusion compounds. Obviously, although the guest templates will have certain effects on the ultimate formation of these crystal structures, the host molecule of 2,2′-dithiosalicylic acid is a controlling factor to form these four inclusion compounds.     

The Crystal and Molecular Structure of the Smectogenic Compound 5-Hexyl-2-(4-bromophenyl)-1,3-dioxane

The title compound with the formula C₆H₁₃ C₄O₂H₆ C₆H ₄Br (HBPD) crystallizes in the monoclinic space group C 2/c with lattice parameters a = 28.48 Å, b = 5.71 Å, c = 20.19 Å, β = 97.4° and molecules per unit cell. The structure has been solved by the heavy atom method and refined to a final R value of 0.094. – The HBPD molecules adopt a fully stretched form, both the alkyl and phenyl substituent are in equatorial position with respect to the chair-shaped dioxane ring. The orientation of the phenyl group is an intermediate between the perpendicular and parallel conformation. The molecules show a nearly perfect parallel arrangement in the crystal lattice.     

Synthesis and characterization of single crystals of the layered copper hydroxide acetate Cu2(OH)3(CH3COO)·H2O

Single‐crystals of the layered copper hydroxide acetate Cu₂(OH)₃(CH₃COO)·H₂O were synthesized by heating copper acetate solution at 60 °C. The standard synthesis of the title compound based on slow titration of copper acetate solution with NaOH yielded materials with worse morphology and an additional phase present. The obtained products were characterized with powder X‐ray diffraction, high temperature powder X‐ray diffraction, scanning electron microscopy and infrared spectroscopy. The crystal structure was determined from single‐crystal X‐ray diffraction data, collected both at 120 K and at 293 K. The title compound crystallizes in the monoclinic botallackite‐type layered structure, space group P 2₁, with the lattice parameters a = 5.5776(3) Å, b = 6.0733(2) Å, c = 18.5134(8) Å, β = 91.802(4)° and a = 5.5875(4)Å, b = 6.0987(4) Å, c = 18.6801(10)Å, β = 91.934(5)° for 120 K and for 293 K, respectively. Acetate groups and water molecules are interlayered between corrugated sheets of edge‐sharing CuO6 octahedra exhibiting strong distortion resulted from the Jahn‐Teller effect. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Three‐Dimensional Structure Constructed via Hydrogen Bonds and π‐π Stacking Interaction. Crystal Structure of [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)

The structure of the title complexes [Cu(AFO)₂(H₂O)₂](ClO₄)₂.2(AFO).2H₂O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R₁ = 0.0595 (wR₂ = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)₂(H₂O)₂]²⁺, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction.     

Double Salt Formation in the Cu(HCOO)2–Sr(HCOO)2–H2O System

The solubility in the Cu(HCOO)₂–Sr(HCOO)₂–H₂O system has been studied by the method of physico-chemical analysis at 25 and 50 °C. It has been established that two double salts are formed in the system: CuSr₂(HCOO)₆ · H₂O at 25 °C and CuSr(HCOO)₄ · 4 H₂O at 50 °C. The latter salt has not yet been described in the literature. It has been characterized by X-ray powder diffraction and DT and TG analysis. CuSr(HCOO)₄ · 4 H₂O crystallizes in the triclinic system with lattice parameters a = 12.376(6) Å, b = 13.394(4) Å, c = 11.508(6) Å, α = 93.38(3)°, β = 94.01(3)°, γ = 75.04(3)°. Dehydration proceeds in two stages.     

Synthesis,characterization and crystal structure of a novel 3‐D copper(II) polymer with bent N‐containing ligand

An exploration of the mixed‐ligand system under hydrothermal condition, has led to the isolation of a 3‐D novel framework {[Cu₂(mp)L₂)(H₂O)₂]·6H₂O}_n ( 1 ) (mp = benzene‐1,2,4,5‐ tetracarboxylate tetraanion, L = 4‐(5‐(pyridin‐4‐yl)‐1,3,4‐thiadiazol‐2yl)pyridine). Single‐crystal X‐ray analyses reveal that it crystallizes in the triclinic space group P‐1, a = 8.807(4) Å, b =11.139(6) Å, c = 11.291(5) Å, α=75.337(7), β = 73.584(5), γ= 66.795(5)°. The Cu^II ions are linked into an extended 2‐D grid net via mp molecules. Further these layers are united together through the bridging L to form a 3‐D structure, which exhibits a new 4‐connected topological network. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural Properties of S-alkylated Dithiolene Chelates (I). Crystal and Molecular Structures of Bis(S-ethyl-ethene-1,2- dithiolato)palladium (II) and Bis(S-ethyl-ethene-1,2-dithiolato) platinum (II)

Bis(S-ethyl-ethene-1,2-dithiolato)palladium(II), Pd(S₂C₄H₇)₂, is monoclinic, P 2₁/n, with a = 7.598(1) Å, b = 10.445(2) Å, c = 8.031(1) Å, β = 95.3(1)° and Z = 2. The structure was determined by 893 independent reflections and refined by the block-diagonal leastsquares method to R = 0.12. The chelate molecule is nearly planar and the palladiumsulfur distances are 2.278(6) Å and 2.403(6) Å. Bis(S-ethyl-ethene-1,2-dithiolato)platinum(II), Pt(S₂C₄H₇)₂, is monoclinic, P 2₁/a, with a 13.114(2) Å, b = 12.873(2) Å, c = 7.446(2) Å, β = 96.1(1)° and Z = 4. The structure was solved from 2040 independent reflections. The compound is not isomorphic with the isomeric palladium complex. In the unit cell there exist two symmetry independent molecules. The platinum-sulfur distance is 2.280 (6) Å.     

Two organic‐inorganic hybrids with Keggin polyanions

Two new Keggin polyoxometalates [Co(phen)₃]₂[SiW₁₂O₄₀]·6H₂O (1) and (ppy)₆ H₄SiMo₁₂O₄₀·0.4H₂O (2) (phen = 1,10′‐phenanthroline, ppy = 4‐(5‐phenylpyridin‐2‐yl)pyridine) have been synthesized by the hydrothermal method. Single crystal X‐ray analysis revealed that compound 1 crystallizes in the monoclinic crystal system with cell parameters of a = 13.344(2) Å, b = 17.191(3) Å, c = 22.002(4) Å, α = 90.00°, β = 99.566(2)°, γ = 90.00°, V = 4977 ų, Z = 2, and compound 2 crystallizes in the triclinic crystal system with cell parameters of a = 11.297(2) Å, b = 12.341(3) Å, c = 19.354(4) Å, α = 107.60(3)°, β = 95.80(3)°, γ = 94.16(3)°, V = 2543.7(9) ų, Z = 1. Both 1 and 2 represent organic ligand molecules and inorganic Keggin anions, which are further interconnected to a 3D framework by supramolecular interactions. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

X-ray Diffraction Study on MgSeO4. 6 H2O at Elevated Temperatures

The dehydration of MgSeO₄. 6 H₂O has been studied using an X-ray powder diffraction method at elevated temperatures. Five different solid phases have been identified in the temperature interval of 20–450 °C: MgSeO₄. 6 H₂O; MgSeO₄. 5 H₂O (with a small amount of MgSeO₄. 4 H₂O), MgSeO₄. 2 H₂O, amorphous MgSeO₄ and crystalline MgSeO₄. MgSeO₄. 5 H₂O crystallizes in the triclinic system with the lattice parameters: a = 6.403(2) Å, b = 10.576(5) Å, c = 6.196(3) Å, α = 98.63(2)°, β = 110.36(2)°, γ = 75.25(3)°, SG P1 . MgSeO₄. 2 H₂O forms orthorhombic crystals with lattice parameters: a = 10.304(1) Å, b = 10.351(9) Å, c = 9.138(9) Å. The crystalline anhydrous magnesium selenate crystallizes in the orthorhombic system with the lattice parameters: a = 4.925(2) Å, b = 9.026(5) Å, c = 6.816(6) Å. Additionally MgSeO₄. 4 H₂O has been prepared and studied roentgenographically: monoclinic system with the lattice constants: a = 6.064(4) Å, b = 13.773(7) Å, c = 8.062(6) Å, β = 91.82(7)°, SG P2₁/n. According to expectation the magnesium selenate hydrates are isomorphous with the corresponding magnesium sulphate hydrates.     

Synthesis and Structure Study of the Complex [Cu2 (μ–C2O4) (C10H8N2)2(H2O)2] (C6H4COSO2N)2 Crystal Structure Containing Cu (II) Bipy Oxalato and Saccharin

The title compound has been synthesized and its crystal structure determined at room temperature. MW = 927.86, monoclinic, space group P2₁/c, Z = 2, a = 9.283(1) Å, b = 16.239(2) Å, c = 12.209(1) Å, β = 99.848(9)°. The crystal structure consists of repeated [Cu₂(μ–C₂O₄)(C₁₀H₈N₂)₂ · (H₂O)₂]₂ cations and non-coordinated saccharin anions. Each copper ion is in a square pyrimidal environment with two oxalate oxygen and two bipyridine nitrogen atoms as a base and one water molecule at the apex. The two copper ions are bridged by oxalato and the distance is 5.138 Å.     

Crystal structure of an ammonium thiocyanate complex of 18–crown–6

The title compound (C₁₃H₃₀N₂O₇S) has been determined from three‐dimensional X‐ray diffraction data. The crystals are monoclinic, a = 22.654(8) Å, b = 8.652(4) Å, c = 23.925(9) Å, β = 123.880(9)°, V = 3893(3) ų, Z = 8, D_calc = 1.192 g/cm³, space group C2/c. The structure was solved by direct methods and refined by full‐matrix least squares method (R = 0.051). The ammonium cation is displaced by 1.08 Å from the mean plane of the ligand causing hydrogen bonding with the macrocyclic O atoms in a perching arrangement. The thiocyanate anion forms an extended hydrogen bonded chain with the cation via the occluded water molecule. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal and Molecular Structure of 4'-Cyanophenyl-4-n-Pentylbenzoate

The crystal and molecular structure of the title compound with the formula C₅H¹¹—C₆H₄—COO—C₆H₄—CN (CPPB) has been determined by X-ray diffraction methods. CPPB crystallizes in the monoclinic space group P2₁/n with eight molecules in a unit cell of dimensions a = 15.268(2) Å, b = 9.165(1) Å, c = 24.031(3) Å, β = 94.67(1)°. The structure has been solved by direct methods and refined to an R value of 0.070.

The CPPB molecules adopt a stretched form and are packed in an approximate parallel imbricated mode, the molecular long axes making an angle of about 5° with the crystal c axis. The molecular geometry and packing are discussed in relation to the mesomorphic behavior of CPPB.     

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.