Crystal structure of bis(potassium hydrogenl-malate)·malic acid, 2[K+(C4H5O5)]·C4H6O5

The crystal structure of bis(potassium hydrogenl-malate)·malic acid, 2[K⁺(C₄H₅O₅)^–]·C₄H₆O₅, has been determined: C₁₂H₁₆K₂O₁₅, M _r =1913.9, orthorhombic, space groupP2₁2₁2₁ a=7.719(5),b=7.916(5),c=29.863(20) Å,V _c=1824.7 ų,Z=4. The structure was determined by a new application of theDirdif procedure using MoK automatic diffractometer X-ray data, and refined by full-matrix least squares toR=0.059 for 962 reflections. A question on space-group assignment and composition was resolved only after the structure had been determined. The conformation of the central carbon skeleton of all three crystallographic independent malate moieties isanti. The potassium ions are coordinated by eight oxygen atoms, forming face-sharing distorted square antiprisms.     

Crystal structure of mixed-ligand copper(II) complexes. Bis(2,2′-bipyridyl)monophenylphos-phatocopper(II)monophenylphosphate monohydrate, [Cu(C10H8N2)2(C6H5OPO3)]-(C6H5OPO3H2)(H2O)

The title mixed-ligand copper(II) complex has been synthesized and its crystal structure at room temperature solved. The crystals are monoclinic:P2₁/c,a=12.004(3),b=19.402(5),c=14.192(4) Å,=108.80(3)°,Z=4. The structure was solved by direct methods, and refined to anR value of 0.041 for 4457 nonzero independent reflections. The crystal structure consists of discrete [Cu(bipy) (MPhP)] units, noncoordinated MPhPH₂, and H₂O molecules. Each [Cu(bipy)₂(MPhP)] unit involves a five coordinate CuN₄O chromophore with a distorted trigonal-bipyramidal stereochemistry. The phosphate groups are linked together by short hydrogen bonds of (P)-O-H--O-P type.     

The structure of 2R-(3′S-benzyloxy-5′S-hydroxy-2′R-hydroxymethyl-1′-oxacyclohexan-6′S-yl)-propionic acid-1,5′-lactone,C16H20O5

The title compound is C₁₆H₂₀O₅, MW=292.3, orthorhombic,P2₁2₁2₁,a=9.741(2),b=29.391(7),c=5.354(1) Å from diffractometer measurements,V=1532.8 ų,Z=4,D _c =1.267 g cm^?3,D _o =1.271 g cm^?3 (ether/1,1,2,2-tetrabromoethane), λ(Mo Kα)=0.71069 Å,F(000)=624,μ=1.02 cm^?1, crystal dimensions 0.23×0.23×0.40 mm,R=0.049 for 1164 observed reflections. The molecule contains a possibly significant asymmetric ether linkage between the oxacyclohexane ring and the highly anisotropic benzyl ring. The packing consists of zigzagged chains parallel to thea-axis formed by hydrogen bonds. The chains are separated by van der Waals contacts.     

Synthesis and crystal structure of [(η5-C5H5)2HfO]3·C6H5Me

The crystal structure of [(⁵-C₅H₅)₂HfO]₃·C₆H₅Me has shown that the compound is not isostructural with its zirconium analog. The title compound crystallizes in the orthorhombic space groupCmcm with well-refined parameters associated with the organometallic moiety and the toluene molecule, whereas [(⁵-C₅H₅)₂ZrO]₃·C₆H₅Me has been reported to belong to the monoclinic space groupP2₁/c with a badly disordered molecule of crystallization. The hafnium derivative exhibits unit cell constantsa=12.322(3),b=17.473(4),c=17.836(4) Å, andZ=4 forD _c =1.84 g cm^–3. Full-matrix least-squares refinement gave a finalR value of 0.062 for 1243 independent observed reflections. The trimer resides on a site of crystallo-graphicmm symmetry. The (⁵-C₅H₅)₂Hf units are bridged together by oxygen atoms at an average Hf-O distance of 1.95(2) Å.     

The Double Salts Cd(C6H5COO)2 · CdCl2 and Cd(C6H5COO)2 · CdBr2

The systems Cd(C₆H₅COO)₂ CdCl₂ H₂O and Cd(C₆H₅COO) ₂ CdBr₂ H₂O have been studied at 25 °C. Formation of the double salts Cd(C₆H₅COO)₂ · CdCl₂ and Cd(C₆H₅COO)₂ · CdBr₂(1:1:0) has been established and their chemical individuality has been confirmed by chemical, X-ray, and DT-analyses. Proceeding from data on the structure of Cd(C₆H₅COO)₂ · 2 H₂O and the composition of the 1:1:0 double salts as well as using Pauling's rules for the most probable spacial disposition of the ions, the crystal structure type of the double salts obtained are predicted.     

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 of Zn[Cl2Ti(C5H5)2]2·2C6H6

The structure of crystals of the composition Zn[Cl₂Ti(C₅H₅)₂]₂·2C₆H₆ has been determined from Patterson and Fourier syntheses of two projections, and refined toR = 0·117 by full-matrix three-dimensional least-squares methods. The crystals are orthorhombic:Pbcn,a = 18·45(5),b = 15·40(6),c = 11·35(3) Å,Z= 4. The complex consists of a central distorted ZnCl ₄ ^2– tetrahedron linked along the Cl—Cl edges to two distorted TiCl₂(C₅H₅)₂ ⁺ tetrahedra in such a way that their centres are nearly collinear The two C₆H₆ molecules in the formulae unit may be regarded as benzene of crystallization.     

The X-ray crystal structure of Hg(C6H4OMe-4) (C6F5): an unexpected twist

The X-ray crystal structure of Hg(C₆H₄OMe-4)(C₆F₅) reveals the first example of perpendicular rings in a diarylmercurial complex. Hg(C₆H₄OMe-4) (C₆F₅) crystallizes in monoclinic space group P2₁/c with a = 11.4004(14), b = 7.5683(9), c = 15.0247(18) Å, = 104.849 (2)° with calculated density 2.517 g cm^–3 for Z = 4.     

Molecular structure and crystal packing of uncomplexed 1,6-bis(N-cyano-p-methoxy-anilino)-2,4-hexadiyne, C22H18N4O2

The X-ray crystal structure of 1,6-bis(N-cyano-p-methoxy-anilino)-2,4-hexadiyne, C₂₂H₁₈N₄O₂, is determined. The crystal packing is dominated by phenyl stacking interactions. Weak C–H···N hydrogen bonds help align the molecules. C–H··· hydrogen bonding is not apparent.     

Crystal growth,crystal structure and pyroelectric properties of the polar hexagonal antimony tartrates MII[Sb2(C4H2O6)2]·2H2O (MII = Ca,Sr, Pb)

Single crystal growth of lead antimony tartrate dihydrate, Pb[Sb₂((+)C₄H₂O₆)₂]·2H₂O, was successfully performed. The determined polar hexagonal crystal structure is isomorphous to the corresponding calcium and strontium antimony tartrates dihydrates. New results of crystal growth and the redetermination of the crystal structures of the nonlinear optical crystal Sr[Sb₂((+)C₄H₂O₆)₂]·2H₂O and its calcium analogue are reported, together with investigations of the thermal stability and the pyroelectric properties of these polar crystals.

     

Crystal structure of protogenkwanin,C16H14O6

The crystal structure of protogenkwanin, C₁₆H₁₄O₆, has been determined by single-crystal diffraction methods. The compound crystallizes in the monoclinic space groupP2₁/c witha=6.804(4),b=7.457(3),c=26.234(3)Å,=95.66(2)° andZ=4. A total of 3275 unique reflection intensities were recorded on a Rigaku AFC6R diffractometer (MoK radiation) at room temperature. The structure was solved by direct methods and electron density calculations. Full-matrix least-squares refinement gaveR=0.058 for 1257 observed [I>3(I)] reflections. Thecrystal structure confirms results from earlier studies on protogenkwanin and elucidates the steric orientation of the hydroxyl substituents of the cyclohexadiene ring: the hydroxyl groups aretrans orientated.     

Structure of the [5S,15S] isomer of the macrocyclic complex, [La(NCS)3(C24H30N6)]

The crystal and molecular structure of the [5S,15S] isomer of the [LaL(NCS)₃] complex (L=C₂₆H₃₀N₆) was determined by single crystal X-ray diffraction analysis. The compound crystallizes in the orthorhombic space group P2₁2₁2₁ witha=13.647(4),b=19.504(4),c=11.606(4)Å. The 9-coordinate La(III) is bound to the N atoms of three monodentate isothiocyanates and to the six N atoms of the macrocycle ligand L, which has an 18-membered, six-nitrogen donor cavity and two peripheral –CH₃ substituents.     

Hydrothermal synthesis and structure of a novel terbium coordination polymer with packing cavities, {[Tb(TCB)1/2(H2TCB)1/2(H2O)](H2O)2}n (H2TCB = 1, 2, 4, 5‐benzenetetracarboxylic acid)

A novel terbium coordination polymer {[Tb(TCB)_1/2(H₂TCB)_1/2(H₂O)](H₂O)₂}_n (H₂TCB = 1, 2, 4, 5‐benzenetetracarboxylic acid) ( 1 ) has been hydrothermally synthesized and determined by single crystal X‐ray diffraction method, which features a very interesting three‐dimensional framework with large packing cavities. It crystallizes in the monoclinic space group P2₁/n with a = 1.0723(4) nm, b = 0.7168(3) nm, c = 1.7155(6) nm, β = 97.079(4)°, V = 1.3086(8) nm³, Z = 4, and final R₁ = 0.0203, wR₂ = 0.0404. In 1, the protonated carboxylate groups are free, the other carboxylate groups are bonded to Tb³⁺ ion in three modes: the chelating bidentate, the bridging bidentate and bridging tridentate. Moreover each Tb³⁺ ion is coordinated by nine oxygen atoms from six carboxylate groups and one water molecule respectively to complete a deformed tricapped trigonal prismatic geometry. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystal structure of N-benzylmethy- lammonium pentachlorothallate (III), [C6H5CH2NH2CH3]2TlCl5

N-Benzylmethylammonium pentachlorothallate (III) salt crystallizes in the monoclinic system P2₁/c with the following unit cell dimensions: a = 10.9540 (8), b = 12.559(1), c = 18.099(2)Å, = 112.1(3)° and Z = 4. The examination of the structure shows an alternate stacking of inorganic layers of pentachlorothallate (III) anions and organic layers of [C₆H₅CH₂NH₂CH₃]⁺ cations parallel to the c axis. The cohesion forces of the packing of N-benzylmethylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N—HsCl) and van der Waals contacts.     

Study on the crystal and molecular structure of triphenyl tin methacrylate: (C6H5)3SnOCOCCH2CH3

The crystal and molecular structure of (C₆H₅)₃SnOCOCCH₂CH₃ has been determined by a single crystal X-ray diffraction study. The crystal is monoclinic with space group P2₁/c,a=11.902(3),b=10.104(4),c=16.721(2) Å,=97.56(1)°,V=1930.4 ų,Z=4 andD _c =1.495 g/ cm³,F(0,0,0)=872,(CuK)=1.5418 Å. The structure was solved by the heavy-atom method and refined by full-matrix least-squares procedures to anR factor of 0.060 based on 2157 independent reflections. The results showed that the Sn-O bond distance is 2.064(4) Å. The average Sn-C bond distance is 2.126 Å. There is a weak coordination through the O of the CO group of the methacrylate residue (Sn-O(2) 2.774(5) Å) except for four normal coordinations. The coordination number at the Sn⁴⁺ is 5.     

Crystal and molecular structure of 1-vinyl-3-methyl-imidazolium iodide,C6H9N2I

The title compound crystallizes with two independent molecules in the unit cell. The two molecules arecis-trans isomers. Crystal data: orthorhombic, P2₁2₁2₁,a=7.0417(6),b=9.5341(9),c=25.411(2) Å,Z=8. The crystal structure has been solved by automated Patterson methods and refined toR=0.024 for 1843 observed reflections.     

Synthesis and single crystal structure of a new polymorph of 5, 10, 15, 20-tetrakis-(4-chlorophenyl) porphyrin,H2TTPCl4: Spectroscopic investigation of aggregation of H2TTPCl4

5, 10, 15, 20-tetrakis-(4-chlorophenyl) porphyrin, H₂TTPCl₄, has been isolated as a new polymorph following the modified Adler’s method and its X-ray crystal structure solved. The new polymorph (I) crystallises in the monoclinic space group, P2₁/n with a?=?10.1574(5) Å, b?=?8.9827(4) Å, c?=?20.9350(8) Å, β?=?102.532(4)°, V?=?1864.62(15) ų, Z?=?2. The previously found polymorph, prepared using Lindsay method was crystallised in monoclinic space group, P2₁/a with a?=?15.776 (13) Å, b?=?8.646 (3) Å, c?=?14.087 (5) Å, β?=?96.05 (5)°, V?=?1910.7 (3) ų, Z?=?2. The main difference between the two polymorphs seems to be the different packing arrangement of molecules in their crystal lattices. The dramatic self aggregation property of new polymorph (I) has also been investigated. The investigation reveals that under certain conditions of solute concentration and pH of the media, the compound exhibits a strong tendency to exist in a prominent self aggregated state in head-to-tail type (j-aggregation) molecular alignment. The self association behaviour of (I) was confirmed by UV-Vis absorption spectra, performed in chloroform by varying concentrations and pH changes and ¹H NMR spectra, performed in deuterated chloroform at varying concentrations and their results have been discussed in detail.     

Crystal and molecular structure of 2,2′-bipyridyl-(μ3-1-keto-2,3,4-triphenylcyclobutenyl) dicarbonylbromomolybdenum(1)benzene [(C6H5)3C3CO](C10H8N2)(CO)2MoBr·C6H6

The crystal structure of [(C₆H₅)₃C₃CO](C₁₀H₈N₂)(CO)₂MoBr·C₆H₆ has been determined. The complex crystallizes in the triclinic space groupP ¯1 witha=8.52(1),b=19.42(3),c=10.54(1) Å, =97.4(1), =74.6(1), and =87.5(1)°. There are two formula units per cell. A total of 2924 unique observed reflections was collected photographically using CuK radiation. The structure was refined toR=0.072. The molybdenum atom in this compound can be considered as situated at the center of a very distorted octahedron. The six coordination sites about the metal atom are occupied by two carbonyl groups which share with the bipyridyl the four equatorial positions. The bromine and a -bonded keto-triphenylcyclobutenyl ring take up the two axial positions. There is an ³ interaction between the cyclobutenyl ring and the molybdenum atom. The detailed geometry of the 1-keto-2,3,4-triphenylcyclobutenyl ligand is similar to that found by Coffey (1962) in a cobalt complex. In the present compound the cyclobutenyl ring is slightly puckered with a dihedral angle of 11.05° between the plane which contains the allylic carbon atoms and that containing the ketonic group. Two solvating benzene molecules are centered at the inversion sites in the unit cell.     

Crystal structure and hydrogen bonding of propargylammonium hexafluorosilicate, 2(C3H6N)+ (SiF6)2−

The X-ray crystal structure of propargylammonium hexafluorosilicate, 2(C₃H₆N)⁺ (SiF₆)^2?, is determined. The SiF₆ anion is involved in N?H...F and C?H...F interactions with eight surrounding cations. This involves two-three-and four-center N?H...F hydrogen bonds, and additional C?H...F interactions with C...F distances down to 2.963(6) Å. The alkynyl C?H donors form only C?H...F interactions of unfavorable geometries.     

Synthesis and crystal structure of the N4-oxide of an hydroxybenzo[f]quinoxalin-6(5H)-one obtained by oxidative cleavage of beta-lapachone-quinoxaline

The N4-oxide of the 5-(3-hydroxy-3-methylbutyl)-5-hydroxybenzo[f]quinoxalin-6(5H)-one was synthesized from beta-lapachone-quinoxaline by MCPBA oxidation and the crystal structure has been determined (C₁₇H₁₈N₂O₄), Mr=297.3, a=15.880(5), b=16.998(1), c=5.587(2) ?, V=1508.1(5) ?³, D _x=1.31, space group P2₁2₁2, Z=4, S=1.109 and R _obs=0.06. The central ring of the molecule is in a twisted-boat conformation and the molecular packing is done through two intermolecular hydrogen bonds O–H···O [2.072(6)] and [2.177(5) ?], forming columns along the direction parallel to the c-axis.