Crystal and molecular structure of 7-hydroxyflavone monohydrate, C14H10O3·H2O

The X-ray crystal structure of 7-hydroxyflavone monohydrate, C₁₄H₁₀O₃ · H₂O, is determined. The compound crystallizes in the monoclinic space group, P2₁/n with a = 3.801(3), b = 19.665(4), c = 16. 039(6), = 93.69(3)°, and = 0.68 mm^–1 for Z = 4. The phenyl ring of the flavone moiety is rotated 18.6(1)° out of the penzopyran plane, which is a typical value for flavones. In the crystal lattice, there are wide channels which are lined mainly by C–H groups. The water molecules enclosed in these channels are severely disordered.     

Crystal structure of aminoguanidinium hexahydro-closo-hexaborate dihydrate, (CN4H7)2B6H6 · 2H2O

The (HAgu)₂B₆H₆ · 2H₂O compound was synthesized and its crystal structure was determined [R = 0.0385 for 2018 reflections with I > 2σ(I)]. The structure consists of HAgu ⁺ cations, centrosymmetric B₆H ₆ ^2? anions, and water molecules. The anions have an almost regular octahedral structure. The bond lengths and angles lie within the following narrow ranges: B-B, 1.715–1.726(2) Å; B-H, 1.08–1.14(2) Å; B-B-B, 59.72°–60.29(9)° and 89.63°–90.20(11)°; and B-B-H, 133.2°–137.0(9)°. The HAgu ⁺ cations and water molecules are involved in the O-H?O, N-H?O, and N-N?N hydrogen bonds and participate in numerous (N, O)-H?H-B specific interactions with the B₆H ₆ ^2? anions, which results in splitting and high-frequency shift of the band of B-H stretching vibrations in the IR spectrum.     

Structural studies on molecular complexes,I: Crystal and molecular structure of 9-aminoacridine-sulfamethoxypyridazine (1∶1), C13H10N2·C11H12N4O3S

The crystal structure of the molecular complex of the antiseptic 9-aminoacridme and the sulfa drug sulfamethoxypyridazine (11), C₁₃H₁₀N₂·C₁₁H₁₂N₄O₃S, has been determined by X-ray diffraction methods. The crystals are orthorhombic: Pbca (No. 61),a=16.321(1),b=16.951(1),c=16.331(1) Å,Z=8,F(000)=1984, andV _c =4518.1(5) ų. The structural parameters have been refined to a finalR value of 0.046 for 3134 observed reflections. The results of X-ray analysis show that the structure contains an acridinium-sulfanilamidate ion pair. A hydrogen atom is transferred from the sulfonamide nitrogen atom to the nitrogen atom of the acridine ring, and an N(acridinium)-HN(sulfonamide) hydrogen bond is formed. A slight folding of the acridine moiety is observed.     

Crystal structure of triaquamaleatostrontium(II) monohydrate, [Sr(C4H2O4)(OH2)3]·H2O

[Sr(C₄H₂O₄)(OH₂)₃]·H₂O is monoclinic, P2₁/n, witha=11.476(2),b=7.027(1),c=12.344(2) Å, =115.74(3)°,V=896.67 ų,Z=4. The Sr atom is surrounded by nine oxygen atoms which come from four different maleate anions and three water molecules. The Sr–O distances range from 2.546(2) to 2.808(2) Å. The C–O distances are equal within the standard deviation 1.263(3) to 1.258(3) Å). In the maleate anion, the planes that contain the carboxylate groups form an angle of 74.44(9)°. Both carboxylate groups deviate significantly from planarity. The different coordination modes of the carboxylate group and the extensive hydrogen bonding present are responsible for the polymeric nature of the structure.     

Synthesis and crystal structure of 3-ammoniumphenyl sulfone selenate, 3-aminophenyl sulfone [C12H14N2O2S]SeO4 · [C12H12N2O2S]

The crystal structure of [C₁₂H₁₄N₂O₂S]SeO₄ · [C₁₂H₁₂N₂O₂S] was determined by X-ray diffraction on single crystal. Crystals are orthorhombic, space group Pbca, with cell parameters a = 11.545 (1), b = 8.143 (1), c = 55.783(1)Å, V = 5244.2 (8)ų and Z = 8. The structure can be described as organic layers built by [C₁₂H₁₄N₂O₂S]²⁺ cations and [C₁₂H₁₂N₂O₂S] molecules, parallel to ab plane, between which the inorganic groups SeO ₄ ^2? are inserted. In this atomic arrangement, H-bonds between the different species play an important role in the three-dimensional network cohesion.     

Structure of a Cu(II)-containing peptide,diaquo-gly-l-tyr Cu(II) dihydrate, [Cu(C11N2O4H13)(H2O)2·2H2O

The structure of the Cu(II) complex of gly-l-tyr [Cu(C₁₁N₂O₄H₁₃) (H₂O)₂]·2H₂O has been solved by X-ray diffraction methods. The compound crystallizes in the orthorhombic space groupP2₁2₁2₁ witha=11.970(2) Å,b=12.485(2) Å andc=10.418(3) Å, respectively, (MoK)=0.710 Å,D _c =1.59 Mgm^–3,D _m =1.59 Mgm^–3, finalR=0.04. The structure was solved by heavy atom (Cu) phased Fourier and refined by full-matrix least squares methods. The coordination geometry of the ligand around the Cu(II) ion has been established as a distorted tetragonal pyramid. The peptide molecule behaves as a tridentate ligand via its amino (N2), amido (N1) nitrogens and carboxyl (O2) oxygens. The peptide nitrogen is found to be deprotonated.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Crystal structure of tetrabutylammonium nitroprusside dihydrate, [(C4H9)4N]2[Fe(CN)5NO]·2H2O, and vibrational spectra of ground and metastable excited states of the dihydrate and the anhydrate

The crystal structure of tetrabutylammonium nitroprusside dihydrate (TBANPDH, [(C₄H₉)₄N]₂[Fe(CN)₅NO]·2H₂O) was determined by single crystal X-ray diffraction (XRD) and the compound was also studied, as well as the anhydrous salt (TBANP), by room and low temperature Fourier Transform Infra-Red (FTIR) and room temperature Fourier Transform Near Infra-Red Raman (FTNIRR) spectroscopies. In addition to the ground states (GS), the metastable excited states (MSI and MSII) generated by laser excitation (488 nm) at low temperature were IR studied, both of the dihydrate and the anhydrate. TBANPDH crystallizes in the trigonal space group P3₂21, D ⁶ ₃, with a = b = 13.777(2), c = 22.039(2) Å, and Z = 3. The structure was solved employing 1273 independent XR reflections, with I > 2(I), by Patterson and Fourier methods and refined by full-matrix least-squares to R1 = 0.054.     

Crystal structure of aqua[S-prolinato-N-monoacetato)copper(II) dihydrate [Cu(Proma)H2O] ⋅ 2H2O

The crystal structure of [Cu(C₇H₉NO₄)H₂O] ? 2H₂O is determined by X-ray diffraction (λMo, R = 0.0316 for 857 reflections). The crystals are tetragonal, a = 8.219(1) Å, c = 17.449(3) Å, Z = 4, ρ_calcd = 1.627 g cm^?3, and space group P4₃. The coordination polyhedron of the Cu atom is a tetragonal pyramid with the O atom of the acetate arm of the prolinatomonoacetate ion (Proma) in the apical position [Cu-O 2.312(6) Å]. The O atom of the water molecule and the N and O atoms of the prolinate group of the Proma ligand lie in the basal plane. The Cu-N bond length is 2.044(6) Å, and the Cu-O bond lengths are 1.932(7) and 1.927(6) Å. The O atom of the acetate arm of the neighboring Proma ion completes the basal plane [Cu-O 1.951(6) Å], thus linking the copper complexes into infinite chains.     

Crystal structure of dicesium thorium trisulfate dihydrate,Cs2Th(SO4)3·2H2O

Dicesium Di--sulfatosulphatobisaquothorate(IV), H₄O₁₄S₃Cs₂Th, (M _r =821.8) crystallized from water in the monoclinic space groupP2₁/c (No. 14), witha=6.415(2),b=15.95(1),c=13.078(8) Å,=90.88(4)°,V=1338(14) ų,Z=4,D _x =4.08 g cm^–3, MoK (=0.71069 Å),=195.8 cm^–1,F(000)=1407.3, room temperature, finalR=0.086 for 1699 unique observed reflexions. Two of the sulfate groups are tridentate (chelating and bridging) and the other is bidentate chelating. As the waters are both coordinated the thorium is 10-coordinate. It shows an unusual 2/4/2/2 geometry.     

Crystal and molecular structure of tetraiodo (1,8-di-2-pyridyl-3,6-dithiaoctane-N,S,S′,N′)dimercury(II)

Summary The X-ray crystal structure of the title compound, [Hg₂(C₁₆H₂₀N₂S₂)I₄], has been determined. The crystals are monoclinic (space groupP2₁/c), with cell dimensionsa=15.016(2),b=6.201(3),c=15.273(2) Å,=115.18(1)°;V _o =1287.0(7) ų,M _r =1213.266,Z=4,D _x =6.26mg m^–3, MoK radiation (graphite crystal monochromator, ),(MoK)=336 cm^–1,F(000)=4272, andT=290°K. The final conventionalR factor=0.054, andR _w =0.062 for 2799 observed reflections. The structure was solved by Patterson and Fourier methods and refined by block-diagonal least-squares methods. The coordination around the mercury atoms is approximately tetrahedral, although with considerable distortion, with two iodine atoms and the N and S atoms of one-half of the ligand molecule.     

Crystal structures of bis(cyanido)bis(N,N′-diethylthiourea-κS) mercury(II) and bis(cyanido)bis(N,N′-dipropylthiourea-κS) mercury(II)

Two mercury(II) complexes containing cyanide and, N,N′-diethylthiourea (detu) and N,N′-dipropylthiourea (dprtu) ligands, [(detu)₂Hg(CN)₂] (1) and [(dprtu)₂Hg(CN)₂] (2), respectively, have been prepared and characterized by X-ray crystallography. In the both complexes Hg atom lies on a 2-fold rotation axis, and is coordinated to the sulfur atoms of two thiourea ligands and to two cyanide carbon atoms. Both have a distorted tetrahedral environment with bond angles about the Hg atoms in the range of 93.41(4)°–146.75(19)°. In the crystal structures symmetry related molecules are linked via N-H-N hydrogen bonds resulting in the formation of a two-dimensional network in 1, while in 2 a double stranded one-dimensional chain is formed.     

Synthesis, crystal structure, and thermal analyses of triaqua-(1,10-phenanthroline-N,N′) succinatomanganese(II) dihydrate, [Mn(H2O)3(phen)(C4H4O4)]·2H2O

[Mn(H₂O)₃(phen)(C₄H₄O₄)]·2H₂O was obtained by reaction of freshly prepared MnCO₃, phen and succinic acid in CH₃OH/H₂O (1:1 v/v), and its crystal structure has been determined by single crystal X-ray diffraction methods. The title mixed ligand complex crystallizes in the triclinic space group with cell dimensions a = 7.590(1) Å, b = 9.324(1) Å, c = 13.917(1) Å, = 85.64(1)°, = 74.56(1)°, = 77.10(1)°, and D _calc = 1.584 g/cm³ for Z = 2. The crystal structure consists of the [Mn(H₂O)₃(phen)(C₄H₄O₄)] complex molecules and lattice H₂O molecules. The Mn atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of three H₂O molecules and one succinato ligand with d(Mn—N) = 2.271 and 2.299 Å, and d(Mn—O) = 2.133–2.239 Å. Through intermolecular hydrogen bondings, the complex molecules are interlinked to form 2D layers, which are assembled by – stacking interactions into 3D framework with tunnels occupied by the lattice H₂O molecules. Thermal analyses showed that the title compound decomposes in two steps over the range 25–600°C upon heating in flowing Ar.     

Crystal and molecular structure of 2,9-di-(methylnitronato)-3,5,10,12-tetramethyl-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) di-triethylammonium diperchlorate,C16H28N6O4Ni·2(C2H5)3NH·2ClO4

The crystal and molecular structure of 2,9-di-(methylnitronato)-3,5,10,12-tetramethyl-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) di-triethylammonium diperchlorate (2c) has been determined of the basis of X-ray diffraction data. The crystals are monoclinic, space groupP2₁/c,Z=2; cell constants=11.478(3),b=15.177(3),c=11.431(3) Å,=99.34(2)°. The structure was refined (full matrix, least squares) with 3408 unique reflections givingR=0.0616. An octahedral configuration of the Ni(II) coordination sphere was found to consist of the macrocycle N₄ atoms occupying the equatorial plane of the octahedron with the O-atoms of the nitronato groups in the apical positions. The triethylammonium cations are hydrogen-bonded to the remaining O-atoms of the nitronato groups.     

Crystal and molecular structure of 1-chloro-1,2-benziodoxolin-3(1H)-one·tetra-n-butylammonium chloride

The title compound,6, a novel 11 complex of 1-chloro-1,2-benziodoxolin-3(1H)-one (5) andtetra-n-butylammonium chloride, was prepared from tetra-n-butylammoniumo-iodoxybenzoate (7) and acetyl chloride. A single crystal of6 was subjected to X-ray analysis: triclinic, space group a=10.239(2),b=11.518(2),c=11.523(3)Å; =73.20(2); =87.85(2), =87.72(2)°; R1=0.0326. The most notable structural feature of crystalline6 is the existence of a secondary bond [I· ·Cl(2), 2.943(1)Å] between the chloride ion and the iodine atom of the chlorobenziodoxolinone moiety. Further coordination at iodine includes three primary bonds: I–C [2.115(4) Å], I–O [2.145(3) Å], I–Cl(1) [2.454(1) Å]. The entire 1-chlorobenziodoxolinone-chloride sub-structure is planar and exhibits iodine-centered bond angles of 78.8(1)° [C–I–O], 92.0(1)° [C–I–Cl(1)], 97.6(1)° [Cl(2)–I–O] and 91.6(1)° [Cl(2)–I–Cl(1)]. The unit cell of6 contains two loosely packed formula units. The chlorobenziodoxolinone-chloride sub-structures occupy a common plane and exhibit a centrosymmetric relationship, while the tetra-n-butylammonium ions are situated one above and one below the plane. Bonding at the iodine atom in6 is more consistent with a 10-I-3 species electrostatically associated with the chloride ion than a 12-I-4 species such as the tetrachloroiodate ion.     

Crystal and molecular structure of 2,2′-di-N-methylamino-1,1′ -di-p-hydroxyphenyldiethyleneether dihydrobromide, (C9H12ON·HBr)2O

The structure of the title compound (C₉H₁₂ON·HBr)₂O was determined by X-ray diffraction methods. The crystals are monoclinic:C2/c,a=7.645(2),b=19.777(3),c=13.704(3) Å,=98.32(2)°,V _c =2050.2 ų,Z=4,F(000)=968,D _m =1.62,D _c =1.615 Mg m^–3; MoK radiation (graphite crystal monochromator, =0.71073 Å),(MoK)=4.39 mm^–1. FinalR factor=0.061 andR _w =0.045 for 1566 reflections. The structure was solved by the heavy-atom Fourier method and refined by least-squares procedures. Each asymmetric unit in the unit cell contains one-half of the molecule, with oxygen atom O(2) at a special position with half-occupancy. The molecules are protonated at their nitrogen sites. The structure is stabilized by a three-dimensional network of hydrogen bonds. The ethylamine side chain in the molecular fragment in the asymmetric unit exhibits an extended (trans) conformation that is also found in most of the other adrenergic phenylethylamines.     

The crystal and molecular structure of 14-β-N-pentylaminomorphinone,C22H28N2O3

The crystal and molecular structure of 14--N-pentylaminomorphinone (14--N-PAM), C₂₂H₂₈N₂O₃, has been determined by analysis of single crystal X-ray diffraction data. The compound crystallized at room temperature in the orthorhombic system, space group P2₁2₁2₁ witha=12.4535(8),b=13.7855(8),c=11.710(1) Å,V _c =2010.3(2) ų,Z=4,D _x =1.22 gm/cm³,(Cu K)=6.58 cm^–1, andF(000)=792. The final refinement yieldedR=0.051,R _w =0.059 for 328 variables with 1133 unique observed reflections. The absolute configuration is established via the synthesis from thebaine by the noninvolvement of certain asymmetric centers. The molecule is found to have as its central structure a T shape similar to that found in morphine and codeine. The distinctive feature of the molecule is the 14--N-pentylamino lipophilic side chain. Molecular modeling studies on the alkylamino chain result in the identification of clusters of conformations based on energy and dihedral angle criteria. Selected conformations are compared to 19-propylthevinol (etorphine), another potent analgesic which contains a lipophilic hydroxyalkyl substituent at C19. The enhanced analgesic activity of 14--N-pentylaminomorphinone is postulated to arise from an overall morphine-like contact with the receptor augmented by the interaction of the aliphatic chain with a lipophilic receptor pocket.     

Crystal and molecular structure of the spin-crossover complex bis(pyridine) [N,N′-ethylenebis (3-carboxysalicylaldimine)] cobalt (II)

The average structure of the title compound, Co(H₂fsa₂en)(py)₂, which has been shown previously to exhibit a thermally induced high-spin low-spin crossover, has been investigated by single-crystal X-ray diffraction. This structure has been solved in the monoclinic space groupC2/c (No. 15), with cell dimensionsa=16.641(5),b=9.496(4),c=16.329(6) Å, and=95.47(3)°;V=2569(3) ų,M _r =571.46,Z=4,D _x =1.478 mg m^–3; MoK radiation (graphite crystal monochromator),=0.71073 Å,(MoK)=7.138 cm^–1;T=295 K andR=0.081 for 681 observed [I>3(I)] independent reflections. The cobalt(II) ion resides on a twofold axis in an elongated octahedral environment, the length of the apical bond (formed with pyridine) being 2.262(12) Å and the mean length of the equatorial bonds (formed with the Schiff base) 2.079(12) Å. These values are consistent with the magnetic behavior, which suggested a distorted surrounding for the metal atom. The packing is essentially governed by the parallelism of the salicylaldimine ligands. The two pyridine rings of the molecule are twisted by ~98° on each side of the basal plane; they are probably affected by orientational disorder or, if ordered, they might be described in a superstructure not yet established.     

Crystal structure of strontium aqua(ethylenediaminetetraacetato)cobaltate(II) tetrahydrate Sr[CoEdta(H2O)] · 4H2O

The complex Sr[Co^II Edta] · 5H₂O (I) (where Edta ^4? is the ethylenediaminetetraacetate ion) has been synthesized. The crystal structure of this compound is determined by X-ray diffraction. Crystals are monoclinic, a = 7.906(2) Å, b = 12.768(2) Å, c = 18.254(3) Å, β = 95.30(3)°, V = 1834.8 ų, space group P2₁/n, Z = 4, and R = 0.036. The structure is built up of the binuclear complex fragments {Sr(H₂O)₃[CoEdta(H₂O)]}, which consist of the anionic [CoEdta(H₂O)]^2? and cationic [Sr(H₂O)₃]²⁺ units linked by the Sr-O bonds into a three-dimensional framework. The coordination polyhedra of the Co and Sr atoms are mono-and bicapped trigonal prisms. The coordination sphere of the Co atom (the coordination number is equal to 6 + 1) involves six donor atoms (2N and 4O) of the Edta ^4? ligand and the O_w atom of water molecule. One of the Co-O distances (2.718 Å) is considerably longer than the other Co-O_lig distances (2.092–2.190 Å) and the Co-O_w(1) distance (2.079 Å). The Sr coordination polyhedron (the coordination number is eight) contains three water molecules, three carbonyl O atoms of the three different anionic complexes, and two O atoms of one acetate group of the fourth anionic complex. The Sr-O distances fall in the range 2.535–2.674 Å. The structural formula of the compound is {Sr(H₂O)₃[CoEdta(H₂O)]}_3∞ · H₂O.