Crystal structure of (Z)-1-(sec-butyl)-3-(4-dimethylaminophenyl)-2-(1H-1,2,4-triazol-1-yl)propen-2-one

The crystal structure of the title compound is determined by X-ray diffraction studies. The structure is solved by the direct method. The experimental data are obtained on a DAR-UMB diffractometer by the θ-θ/2θ scan technique using MoK _α radiation. The crystal is monoclinic, a = 17.913(3) Å, b = 17.239(3) Å, c = 5.501(5) Å, γ = 74.4(3)°, space group P2₁/a, Z = 4 for C₁₇H₂₂N₄O, and ρ_calcd = 1.211 g/cm³. The molecule consists of the phenyl and triazole rings and the dimethylamino, carbonyl, and isopropyl groups attached to the rings. The dihedral angle between the rings is 67.4°. The carbonyl oxygen atom and the triazole ring are in the trans position relative to each other. The N-C-C-O torsion angle is 172.8°. The molecule is in the Z isomeric form.     

Crystal and molecular structures of 2′-nitro-4-aminobiphenyl and 2-amino-7-nitrofluorene

2′-nitro-4-aminobiphenyl (5), C₁₂H₁₀N₂O₂, crystallizes in the monoclinic space groupP2₁/c:a = 6.043(2),b =15.795(3),c = 11.577(2) Å, β = 103.42(8) °;D _c = 1.324 g cm^?3 forZ = 4. 2-amino-7-nitrofluorene (3), C₁₃H₁₀N₂O₂, crystallizes in the monoclinic space groupP2₁ n:a = 10.765(2),b = 7.454(4),c = 12.959(2) Å, β = 95.44(1) °;D _c = 1.451 g cm^?3 forZ = 4. Three-dimensional CuKα intensity data were measured with a computer-controlled diffractometer, and the initial phases were obtained by direct methods. The two structures were refined by the full-matrix least-squares method, which gave finalR values for 5 and 3 of 0.045 and 0.043, respectively. Bond lengths in the compounds are normal, apart from slight shortening of the phenyl-phenyl C-C bond and some distortion of the phenyl rings caused by the amino and nitro groups. In 5, the two phenyl rings are twisted by 57.1 °, and the nitro group is twisted by 34.6 ° from the plane of its phenyl group. The carbon backbone of 3 is nearly planar with the two phenyl groups tilted by 4.0 ° to each other. The nitro group in 3 is twisted 5.7 ° from the plane of its phenyl group. There is amino hydrogen to nitro oxygen intermolecular hydrogen bonding in each structure.     

Crystallographic analysis of Royline monohydrate [C25H41NO7 · H2O]

The crystal and molecular structures of the alkaloid Royline {(1α,6β,14α, 16β)-20-ethyl-4-hydroxymethyl)-1,6,14,16-tetramethoxyaconitane-7,8-diol} with a water molecule has been determined by X-ray diffraction analysis. The compound crystallizes in the space group P2₁ with the unit cell parameters a = 10.985(1) Å, b = 7.898(1) Å, c = 14.956(1) Å, β = 102.96(1)°, V = 1264.52 ų, Z = 2, λMoK _α = 0.71073 Å, and R = 0.033 for 2067 observed reflections. Rings A, B, and C adopt a chair conformation, ring D is a half-boat, ring E is a half-chair, and ring F is in an envelope conformation with C(14) at the flap. Molecules are linked together in the crystal by hydrogen bonds.     

Crystal structure of 4-phenyl-3,5-dioxacyclohexyl-1, 1′-cyclopentane-2′,3″-(1,5,8,11-tetraoxacyclotridecane)

The structure of the title compound is determined by X-ray diffraction (DAR-UMB diffractometer, θ-θ/2θ scan mode, MoK _α radiation, direct method). The crystal is monoclinic, a = 24.582(6) Å, b = 22.812(8) Å, c = 8.647(3) Å, γ = 60.64(2)°, ρ _calcd = 1.232 g/cm³ space group A2/a, and Z = 8 for C₂₂H₃₂O₆. The molecule consists of four fragments: 13-crown-4 (A), 1,3-dioxane (B), a five-membered ring (C) acting as a bridge between fragments A and B, and a phenyl ring (D). Introduction of the bulky ring C as a bridge into the molecule results in significant deviations (up to ±0.014 Å) of the ether O atoms from planarity. The conformation of the macrocyclic fragment is [3433] according to the Dale notation. The C—H?O 1,4-interactions, which are energetically favorable occur in the propylene part of 13-crown-4: the C(2)?O(5) and C(4)?O(1) distances are 2.82 Å. The molecules in the structure form planar networks parallel to the xy plane. The intermolecular contacts correspond to the van der Waals interactions.     

Crystal and molecular structure of diphenyl sulphone, 4,4′-difluorodiphenyl sulphone and 3,3′-dinitro-4,4′-difluorodiphenyl sulphone

The crystal and molecular structures of diphenyl sulphone (A), 4,4′-difluorodiphenyl sulphone (B) and 3,3′-dinitro-4,4′-difluorodiphenyl sulphone (C) have been determined from three-dimensional MoKα diffractometer data. Each molecule crystallizes in the monoclinic space groupP2₁/c with cell dimensionsa = 12.225(4),b = 7.830(2),c = 11.328(2) Å, β = 98 °19′(2);a = 8.255(3),b= 13.062(3),c = 10.135(2) Å, β = 99 ° 31′(2) anda = 14.736 (4),b = 8.145(2),c= 14.626(3) Å, β= 129°8′(2), respectively. The structures were solved by Patterson and Fourier techniques and refined by the method of least squares toR-factors of 3.8% over 1798 reflections, 6.3% over 1834 reflections and 5.4% over 2185 reflections forA,B andC, respectively. The dimensions of the sulphone group are similar in each molecule; the S—C bond lengths range from 1.764(3) to 1.775(3) Å, and the S—O bond lengths from 1.432(3) to 1.439(3) Å. The dihedral angles between the aromatic rings and the S—S—C planes lie between 72,6 and 88.9 °, compared with the value of 90 ° predicted for maximum conjugation between the sulphone group and the aromatic ring. Intermolecular H―O contacts of 2.37 Å suggest possible C—H—O type hydrogen bonds joining the molecules of 4,4′-difluorodiphenyl sulphone into dimers and the molecules of 3,3′-dinitro-4,4′-difluorodiphenyl sulphone into chains.     

Stereochemical studies of oligomers. IV: structure of bis-3,3,5-trimethylcyclohexyl phthalate

C₂₆H₃₈O₄,Mr=414.6, is monoclinic,P2₁/c, witha=15.059(2),b=7.348(2),c=23.164(3) Å,β=90.35(16)°,V _c =2563.13(85) ų,D _x =1.07(4) g cm^?3,μ(CuKα)=5.28 cm^?1. The structure was determined by direct methods and refined by full-matrix least squares toR=0.074 for 2479 observed reflections. The two cyclohexane rings both adopt a chair conformation.     

Structure of zinc tetraphenylporphyrin dimethyl formamide-methylene chloride

C₄₈H₃₇N₅ZnOCl₂,M _r+836.13, triclinic, $P\bar 1$ ,a+11.2231(15),b+12.5155(18),c+14.6013(19)Å, α=99.001(7), β=94.600(8), γ=103.221(7)^o,V+1957.6(5)ų,Z+2, D_x+1.419 gcm^?3, MoKα (λ=0.7107Å), µ_cale,F(000)=1670,T+173±1K, final discrepancy factor 2.8% for 5274 unique reflections above 2.5σ(I) in the range 3<2θ<48^o. The metal is coordinated to the four nitrogen atoms of the porphyrin ring and the oxygen of the dimethyl formamide moiety. The geometry of this porphyrin is nonplanar with respect to the overall structure, although the pyrrole rings are nearly coplanar with the zine metal pulled out of the plane in the familiar domed-shaped geometry.     

Crystal and molecular structure of a diradical, 1,3-dinitro-4,6-di[3-(2,2,5,5-tetramethyl)-pyrrolidinyl-N-oxide]aminobenzene monohydrate

The crystal structure of 1,3-dinitro-4,6-di[3-(2,2,5,5-tetramethyl)pyrrolidinyl-N-oxide] aminobenzene monohydrate has been determined by single-crystal X-ray diffraction methods using the 1793 unique reflections for which 3 ° < 2θ < 40 ° andI > 3σ(I), and refined to a conventionalR index of 0.032. Counter methods using MoKα radiation were employed. Crystals form in the triclinic space groupP¯1 (No. 2) witha = 16.160(10),b = 11.686(6),c = 7.211(5) Å, α = 95.87(5) °, β = 98.67(5) °, and γ = 107.74(4) °. All hydrogen atom positions were determined. Intramolecular hydrogen-bonding between the nitro and amino groups has, in part, caused the central 20 atoms of the molecule, counting hydrogen atoms, to lie in an approximate plane. The benzene ring is distorted by its substituents to the symmetrymm2(C _2v ). The internal angles of the benzene ring range from 116.1 ° to 124.7 ° (esd = 0.3 °), and its bonds are between 1.368 Å and 1.436 Å (esd = 0.004 Å) in length. Four of the five atoms in each pyrrolidine ring are nearly coplanar; the remaining atom, the carbon bonded to the amine nitrogen in each case, lies approximately 0.53 Å from the corresponding plane. The best four-atom planes of the two pyrrolidine rings are each near to perpendicular to the central plane, giving the molecule a lobster-like appearance; they are each rotated approximately 15 °, in opposite senses, from perpendicular. The intramolecular distance between the two pyrrolidine nitrogen atoms, to which the unpaired charges can be assigned, is 7.68 Å. One of the nitroso oxygen atoms is hydrogen-bonded by two symmetry-equivalent water molecules. The inversion center necessitates that the remaining hydrogen atoms of these water molecules both hydrogen-bond to a symmetry-equivalent nitroso oxygen atom to give a hydrogen-bonded four-oxygen ring.     

N-isopropyl-2-(isopropylamino)troponiminate complexes of lithium and calcium

The synthesis and structures of [(i-Pr)₂ATI]Li₂(thf)(I)(1) and [(i-Pr)₂ATI]Ca(thf)₂(I)₂Li₂(thf)₂-[(i-Pr)₂ATI] (2) (where [(i-Pr)₂ATI]=N-isopropyl-2-(isopropylamino)troponiminate) have been described. The lithium atoms in compounds1 and2 occupy positions above and below the plane of the aminotroponiminate ligand. The calcium atom in2 adopts a pseudo-octahedral geometry with two tetrahydrofurans occupying thetrans-positions. Compound1 crystallizes as dimeric units. Crystal data with MoKα at 193 K:1, C₁₇H₂₇ILi₂N₂O,a=13.217(2)Å,b=9.875(2)Å,c=16.410(4)Å, B=111.41(1)^o,V=1993.4(6)ų, a monoclinic space groupP2₁/n,Z=4,R=0.029;2, C₄₂H₇₀CaI₂Li₂N₄O₄,a=911.390(2)Å,b=30.880(4)Å,c=13,465(2)Å, B=93.85(1)^o,V=4724(1)ų, monoclinic space groupC2/c,Z=4,R=0.027.     

Molecular and crystal structure of mesomorphic para-n-hexyloxybenzoic acid

The triclinic modification of para-n-hexyloxybenzoic acid is studied using X-ray diffraction analysis (MoK _α radiation) at 120 K. The crystallographic parameters of the compound are as follows: space group, $P\overline 1 $ a = 7.8854(4) Å, b = 14.3021(7) Å, c = 33.0513(16) Å, α = 88.738(1)°, β = 85.701(1)°, γ = 78.331(1)°, and Z = 12. The asymmetric unit of the crystal contains six molecules of the acid with different orientations of the aliphatic chain. In the crystal, the molecules are joined into dimers by hydrogen bonds between the carboxyl groups. The crystal packing is built on the principle of the separation of aromatic and aliphatic regions.     

Crystal structures of 1,1′-di(methylacetato)- and 1,1′-di(chloroethoxyethyl)-2,2′-biimidazole

1,1′-Di(methylacetato)-2,2′-biimidazole, C₁₂H₁₄N₄O₄, crystallizes from methanol in the space groupP2 ₁/c, wherea=9.535(2),b=13.385(2),c=5.1208(8) Å,V=652.2(2) ų, andZ=4.1,1′-Di(chloroethoxyethyl)-2,2′-biimidazole, C₁₄H₂₀Cl₂N₄O₂, crystallizes from cyclohexane in the space groupPbca, wherea=12.372(2),b=8.959(2),c=14.840(2) Å,V=1644.9(5) ų, andZ=8. The structures were refined toR=0.041 (1380 observed reflections) andR=0.043 (3243 observed reflections), respectively. Both molecules crystallize with coplanar rings and the substituents assume atrans configuration with a center of inversion between the bridging carbon atoms.     

Crystal structure of (2,2′-bipyrimidine)-dinitratopalladium(II) acetone solvate

(2,2′-bipyrimidine)dinitratopalladium(II) forms a triclinic crystal in space groupP?1 witha=7.605(5) Å,b=8.791(4) Å,c=12.632(5) Å, α=85.11(3)⁰, β=78.79(4)⁰, γ=77.45(4)⁰,V=807.7(7) ų, andZ=2. The Pd atom exhibits square planar coordination geometry with mean Pd?O=2.206(7) Å, Pd?N=1.990(5) Å, O?Pd?O=92.0(2)⁰, and N?Pd?N=81.0(2)⁰. The complexes associate across an inversion center with Pd...Pd=3.190(2) Å. The bipyrimidine ligand is bowed with a 5.9(2)⁰ dihedral angle between the C₄N₂ rings. The nitrate ions are on the same side of the N₂O₂ donor atoms plane and make 60.4(2)⁰ and 66.6(2)⁰ dihedral angles with that plane.     

Molecular and crystal structures of 3-methyl-3-[1,7-dicarba-closo-dodecaborane(12)-1-oyl-peroxy]-but-1-yne

The crystal and molecular structures of 3-methyl-3-[1,7-dicarba-closo-dodecaborane(12)-1-oylperoxy]-but-1-yne (I) are determined by X-ray diffraction analysis (Nicolet R3m automated diffractometer, MoK _α radiation, θ/2θ scan mode). It is found that the compound crystallizes in the orthorhombic crystal system, space group P2₁2₁2₁. The unit cell parameters are as follows: a = 7.355(2) Å, b = 9.773(3) Å, c = 21.938(7) Å, and Z = 4. The structure is solved by the direct method and refined to R = 0.0658. The structural features of the molecule and the C-H?O contacts in the structure are discussed.     

Synthesis and crystal structure of 3-ammonium-4-hydroxyphenyl sulfonate hemihydrate

The crystal structure of 3-ammonium-4-hydroxyphenyl sulfonate hemihydrate C₆H₃(NH₃)(OH)SO₃ · 0.5H₂O is determined by single-crystal X-ray diffraction. The unit cell parameters are as follows: a = 11.2395(3), b = 10.3814(3), c = 13.7509(4) Å, β = 100.326(1)°, V = 1578.49(8) ų, space group P2₁/n, Z = 4. The crystal structure can be described us a succession of infinite corrugated layers parallel to ab plane. These layers consist of rings formed by four sulfonate molecules located around a center of symmetry. The rings are connected to each other and to water molecules via O-H...O hydrogen bonds. The structure is further stabilized by π-π interactions between phenyl rings of organic entities of successive layers.     

Crystal and molecular structure of di(perchlorato)(1,4,8,11-tetraazacyclotetradecane)copper (II). Cu(cyclam) (ClO4)2

The title compound, Cu(C₁₀H₂₄N₄)(ClO₄)₂, crystallizes in the triclinic system with unit cell dimensionsa= 8.744,b= 8.022,c= 8.677 Å, α = 118.7, β = 56.9, γ = 113.5 °,Z= 1, space group P¯1. The structure was solved by Fourier methods and refined by least-squares techniques using the 1545 nonzero three-dimensional counter-diffraction intensity data (CuKα) to give a conventionalR factor of 0.056. The coordination sphere of the copper ion is defined by a planar arrangement of the four nitrogen donors in the macrocyclic ligand with oxygen atoms from the perchlorate groups lying above and below this plane. The resulting tetragonally distorted octahedron of donor atoms gives interatomic distances Cu?N = 2.02(4) Å and 2.02(3) Å, and Cu?N = 2.57(4) Å.     

Synthesis and crystal structure of bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl)copper(II)

The title compound, bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl) copper(II), [Cu(C₁₇H₁₁NOCl)₂] (1) was synthesized and its crystal structure was determined. The Compound 1 is monoclinic, space group P2 ₁/c with a = 9.146(3) Å, b = 18.724(3) Å, c = 16.230(2) Å, β = 96.46(1)°, V = 2761.8(11) ų, Z = 4, D _c = 1.503 g cm^?3, μ(Mo Kα) = 1.020 mm^?1, R = 0.0606 for 2361 reflections [I > 2σ(I)]. In the title compound, the Cu atom is coordinated by an N₂O₂ donor set from the imine-phenol ligand in a slightly distorted square planar coordination geometry, with the two phenolate O atoms being deprotonated. The Cu–O bond lengths are 1.878(4) and 1.889(4) Å, the Cu–N bond lengths are 1.980(5) and 1.985(5) Å. The angles O1–Cu–N1 and O2–Cu–N2 are 90.96(19) and 90.72(19)°, respectively.     

X-ray crystal structure of dichloropicric acid

Dichloropicric acid is orthorhombic, space groupP2₁2₁2₁; at 24°a=5.672(3),b=8.044(3),c=22.491(7) Å,D _x=1.929(2) g-cm^?3,V=1026(1) ų,Z=4. The phenolic OH group is intramolecularly hydrogen bonded to one of theortho nitro groups with an O...O distance of 2.524(5) Å. As a consequence, this nitro group is twisted out of the plane of the benzene ring by only 20.1° in spite of crowding by the adjacent chlorine atom which is only 2.764(3) Å from the O atom in the nitro group. The two non-hydrogen bonded nitro groups have twist angles of 73.9 and 84.1°. There is no evidence of intermolecular hydrogen bonding with any adjacent dichloropicric acid molecule.     

Molecular conformation and electronic structure. II: Crystal and molecular structure ofN-(p-bromobenzylidene)-p-bromoaniline

The structure of the title compound C₁₃H₉Br₂N has been determined with MoKα₁ diffractometer data, and refined by full-matrix least squares toR = 0.061 for 888 observed reflections. The crystals are monoclinic: space groupP2₁/a,a = 24.912(13),b = 5.877(1),c = 4.046(1) Å,β = 92.42(3) °Z = 2. The uv absorption spectrum indicates a nonplanar conformation in solution. In the solid, the molecule is disordered about a crystallographic inversion center and is planar to within 0.045 Å.     

Crystal structure of zirconium-rich seidozerite

The crystal structure of seidozerite was refined (a Siemens P4 diffractometer, MoK _α radiation, 1180 independent reflections, anisotropic refinement, R = 0.053). The monoclinic unit-cell parameters are a = 5.627(1) Å, b = 7.134(1) Å, c = 18.590(4) Å, β = 102.68(1)°, sp. gr. P2/c, Z = 4. The structural formula, Na_1.6Ca_0.275Mn_0.425Ti_0.575Zr_0.925[Si₂O₇]OF, agrees well with the results of the electron probe analysis. Seidozerite is demonstrated to belong to the meroplesiotype polysomatic series including the structures of more than 30 titano-and zirconosilicates.     

Crystal structure of 5-(2′-aminophenyl)-2-dimethylamino-1,3,4-thiadiazole

The crystal structure of 5-(2′-Aminophenyl)-2-dimethylamino-1,3,4-thiazole is determined by X-ray diffraction. The compound is prepared by an unusual recyclization of 3-N, N-dimethylthioureidoquinazolin-4(3H)-one. The crystal is monoclinic, space group P2₁/c, a = 7.420(2) Å, b = 10.466(5) Å, c = 14.752(9) Å, β = 109.2(4)°, ρ_calcd = 1.359 g/cm³, and Z = 4 for the C₁₀H₁₂N₄S composition. The molecule consists of the thiadiazole and phenyl rings and the dimethylamine N(CH₃)₂ and amine NH₂ groups attached to the rings. The molecule as a whole is planar. The dihedral angle between the rings is 8.9°. The N(1) and N(4) atoms in the molecule are bound through the intramolecular interaction (2.76 Å). Molecules, which are linked in pairs by antiparallel hydrogen bonds, form a framework structure.