Crystal structure of C11H18N2O2·HBr: Corrigendum

Contribution No. 7919 from the Arthur A. Noyes Laboratory of Chemical Physics     

Crystal and molecular structure of (2E,4S,10R)-4-hydroxy-2-undecen-10-olide (nor-patulolide C), C11H18O3

The stereogeometry and absolute configuration of the title compound has been proved by an X-ray diffraction analysis. Crystal data: monoclinic, P2₁,a=7.7976(2),b=7.8288(2),c=8.9791(4) Å, =90.331(4)^o, Z=2. The crystal structure has been solved by vector search methods and refined toR=0.042 for 1798 observed reflections.     

Crystal and molecular structure of 1,4,10-trioxa-7,13-diaza-cyclopentadecane-7,13-diacetatocopper (II) dihydrate,C114H24N2O7Cu · 2H2O

l,4,10-Trioxa-7,13-diazacyclopentadecane-7,13-diacetatocopper(II) dihydrate: space groupP4₃, witha=b=7.217(1),c=34.553(7) Å, andZ=4. The structure was solved by direct methods, and refined by full-matrix least-squares toR=0.039 andR _w=0.043. The Cu(II) atom is seven-coordinated (deformed pentagonal bipyramidal coordination) by the two nitrogens and three oxygens of the 15-membered ring and by two oxygens from acetato groups. These groups form 5-membered chelate rings positioned on opposite sides of the macrocycle.     

Crystal and molecular structures of 1-(2-methyloxycarbonylo-propan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol hydrochloride (1) (C18H24NO4Cl) and 1-(2-methylcarbamoylpropan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (2) (C18H24N2O3)

The crystal structures of two new-adrenergic antagonists, derivatives of propranolol, are reported in this paper. The space groups and unit-cell parameters are: compound1 (C₁₈H₂₄NO₄Cl), monoclinic,P2₁,a=7.215(1),b=8.591(1),c=15.017(1)Å,=95.64(1)°; compound2 (C₁₈H₂₄N₂O₃), monoclinic,P2₁/c,a=10.218(3),b=21.616(5),c=8.124(2)Å,=101.28(2)°. The structures were solved with direct methods and refined by full-matrix least-squares techniques toR indices of 0.036 and 0.066, respectively. The molecule of compound1 has an extended external chain, and thus its structure is linear, whereas the molecule of compound2 is compact, and its external chain is twisted in a characteristic way, as is the case of peptides.     

Crystal structure of di(ethyleneglycol)di(para-methylbenzoate), C20H22O5

The crystal structure of di(ethyleneglycol)di(para-methylbenzoate), C₂₀H₂₂O₅, has been determined by direct methods from 1400 observed reflections collected on a Nonius CAD-4 automatic diffractometer. The crystals have a monoclinic unit cell of dimensionsa=11.408(2),b=5.808(3),c=8.542(4) Å and=109.50(2)° and belong to theP2¹/c space group (No. 14). The finalR value is 0.049. The benzene rings are planar and show the usual distortions due topara-substitutions. The carboxylate planes are inclined by 2.2(4) and 4.7(4)° from their respective benzene ring planes. The conformation of the di(ethyleneglycol) moiety,tg ^– gtg ^– g ^– (t=trans, g=gauche), differs considerably from that of the methylenic sequences in pentamethyleneglycoldi(para-nitrobenzoate) which is alltrans, or in pentamethyleneglycoldi(para-chlorobenzoate) which isg t t t t g.     

Crystal and molecular structure of 1-(2-isopropylcarbamoylpropan-2-ylamino) 3-(1-naphthyloxy)propan-2-ol (C20H28N2O3)

The crystal structure of the title compound has been determined with three-dimensional MoK X-ray diffraction data. The space group and unit-cell parameters are:P2₁/c,a=8.610(3) Å,b=13.516(5) Å,c=16.818(5) Å,=94.95(3)° andV=1950.0(7) ų. The structure was solved by direct methods, and refined by full-matrix least-squares techniques toR=0.0608 andR _w=0.0648. The compound is a derivative of the popular-adrenolytic propranolol, and in the propanol part of the side chain shows the typicalgauche conformation.     

Crystal and molecular structure of (exo)-2-methoxycarbonyl-5-ethoxycarbonyl-4,5,6,11b-tetrahydroisoxazolidino-[2,3-a]-β-carboline,C18H20N2O5

The structure of the title compound, C₁₈H₂₀N₂O₅, was determined by X-rays atT=290 K.M _r =344.366, monoclinic, space groupP2₁/c,a=13.7850(8),b=8.8951(7),c=15.1603(11) Å, =111.410(6)°,V _c =1730.7 ų,Z=4,D _x =1.322 Mgm^–3. Cu K radiation (graphite crystal monochromator, =1.54178 Å),(Cu K)=7.69 cm^–1. Final conventionalR-factor=0.057,R _w =0.076 for 2160 observed reflections and 271 variables. The structure was solved usingMultan.     

Crystal and molecular structure of dimethanolbis(salicylaldehydato)cobalt(II), C16H18CoO6

The structure of dimethanolbis(salicylaldehydato)cobalt(II) has been determined by three-dimensional X-ray diffraction methods. The crystals are monoclinic, space groupP2₁/c,a = 5.099(7),b = 19.446(9),c = 8.889(7) Å, = 111.85(10) °, andZ = 2. The structure consists of discrete centro-symmetric molecules of C₁₆H₁₈CoO₆ in which the oxygen atoms form a distorted octahedron about the cobalt atom, with cobalt-oxygen distances of 2.010(4), 2.076(4) Å (salicylaldehyde) and 2.115(4) Å (methanol). The molecules are linked together along thea-axis by intermolecular hydrogen bonds from the hydrogen atoms of the methanol groups to phenolic oxygen atoms of neighboring molecules. The final conventionalR-factor for 1232 observed reflections is 0.058.     

Crystal and molecular structure of methylene bis(piperidine-dithiocarbamate), C13H22N2S4

Reaction of anhydrous sodium piperidine dithiocarbamate with methylene chloride yields methylene bis(piperidine dithiocarbamate). The crystals, C₁₃H₂₂N₂S₄ (M=334.57), are monoclinic with space group ,a=6.421(3),b=29.321(7),c=9.022(4)Å,=109.05(3)°,V=1605.6 ų,Z=4,D _c =1.384 g cm^–3,F(000)=712,T=295°K (Mo-K)=0.71069 Å,=5.62 cm^–1 andR=0.032 for 1734 reflections. The molecular structure shows that the methylenic group is bonded to two planar moieties at distances of 1.782(3) and 1.803(3)Å with an S-CH₂-S angle of 114.7(2)°. The configuration about each N atom is planar rather than pyramidal. The two C-N bond lengths adjacent to the C=S bonds are both very short 1.330(4) and 1.336(4) Å indicating the influence of the C=S bond on C-N bond lengths. The six-membered piperidine ring has a classical chair conformation with average C-C distance of 1.511 (5)Å.     

Crystal and molecular structure of (exo)-1-carboxymethyl-5-ethoxycarbonyl-4,5,6,11b-tetrahydroisoxazolidmo-[2,3-a]-β-carboline,C18H20N2O5

The structure of the title compound C₁₈H₂₀N₂O₅, was determined by X-rays atT=290 K.M _r =344.366, monoclinic, space groupP2₁/c,a=15.589(4),b=7.619(1),c=16.792(4) Å, =111.47(2)°,V=1856.1 ų,Z=4,D _x =1.23 Mg m^–3. CuK radiation (graphite crystal monochromator, =1.54178 Å),(CuK)=7.17 cm^–1,F(000)=728. Final conventionalR-factor=0.075,R _w =0.106 for 2266 observed reflections and 274 variables. The structure was solved usingMultan.     

Co(II)(C7H7O2N)2(C12H12N2)2微晶粉体的水热合成及表征

本文以对氨基苯甲酸和联苯胺为配体,通过水热合成制备Co(II)的配合物,得到Co(II)(C7H7O2N)2(C12H12N2)2(C7H7O2N= p-aminobenzoic acid, p-abza, C12H12N2= Benzidine)深蓝色微晶颗粒.通过元素分析、IR等方法对配合物进行了表征,并通过TG分析对该配合物的热稳定性及热分解机理做了初步探讨.     

Crystal and molecular structure of inner-chelatetrans-1,4,10,13-tetraoxa-7,16-diazacyclooctadecane-7,16-diacetatozinc(II), C16H28N2O8Zn

The molecular structure of trans-1,4,10,13-tetraoxa-7,16-diazacyclooctadecane-7,16-diacetatozinc(II), complex (I), has been investigated by X-ray diffraction methods. It crystallizes in the monoclinic space groupP2₁/c, witha=16.229(2),b=12.001(1),c=9.778(1) Å,=95.59(1)°, andZ=4. The structure was solved by direct methods, and refined by full-matrix least-squares toR=0.048. The zinc cation, placed asymmetrically in the macro-ring cavity, is six-coordinated to 2 N- and 2 O-atoms of the macrocycle, and to 2 O-atoms of two acetate groups, thus forming an irregular octahedral coordination sphere. The 18-diaza-crown-6 ring reveals approximate twofold symmetry (s=0.1 Å), with the axis through C2-C3 and C11-C12 midpoints.     

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.     

双核Cu(II)-5-溴水杨醛缩氨基甲磺酸席夫碱4,4'-联吡啶三元配合物的合成及晶体结构

采用Cu(II)盐和氨基甲磺酸缩-5-溴水杨醛席夫碱(H2L)以及4,4'-联吡啶(bpy)在乙醇和水溶液中合成了三元配合物,通过元素分析、红外光谱对配合物进行了表征,并用X射线衍射测定了其结构.结构解析表明,该标题配合物属单斜晶系,空间群P21/c,晶胞参数为: a=0.9509(2) nm,b=1.8783(2) nm,c=1.0514(2) nm;β= 98.48 (1)°,V=1.8575(3) nm3, Z=2,Dc=1.812 g·cm-3, F(000)=1016, μ=3.473,最终偏差因子(对I＞2σ(I)的衍射点)R1=0.0459, wR2=0.0739,对全部衍射点R1=0.1205, wR2=0.0887, ω-1= [σ2(Fo)2+0.0345P],P=(Fo2+2Fc2)/3.邻近配合物分子间存在着大量的氢键, 席夫碱三元配合物通过氢键作用堆积成2D网状结构.     

Crystal structure and vibrational spectra of hydrazinium(2+) aquatetrafluoroindate(III), N2H6(InF4H2O)2

The crystal structure of hydrazinium(2+) aquatetrafluoroindate(III), N₂H₆(InF₄H₂O)₂, has been determined by X-ray diffraction. The compound crystallizes in the triclinic space group (C _i ¹) with a = 6.759(2) Å, b = 6.228(1) Å, c = 5.7854(7) Å, = 80.28(2)°, = 88.79(1)°, = 69.96(2)°, V = 225.3(1) ų, and Z = 1. The structure comprises hydrazinium(2+) cations and InF₂F_4/2O^– anions in which In appears to be seven-coordinated in the form of a pentagonal bipyramid by four bridging fluorine atoms, two terminal fluorine atoms, and one oxygen atom. Pentagonal bipyramids are interconnected and form chains along a axis. Bands in vibrational spectra were assigned to the vibrations in N₂H₆ ²⁺ cations and anionic InF₂F_4/2O^– entities. The rather intensive band appearing at 1042 cm^–1 in Raman spectrum, which is absent from infrared, is characteristic of the N₂H₆ ²⁺ cation, in line with the predictions of the unit-cell group analysis for the studied system.     

Crystal and molecular structure of 6,13-Di(ethoxycarbonyl)-7,12-dimethyl-dibenzo [b.i.]-1,4,8,11-tetraaza[14]annulenato(2-) nitrosocobaltat [C26H26O5N5Co] and the neutral ligand [C26H28O4N4]

Both title compounds crystallize in the orthorhombic space group Pnma with 4 formular units in the unit cell. The lattice parameters are: [C₂₆H₂₆O₅N₅Co], a = 8.589(4), b = 19.395(3), and c = 14.850(3) Å;[C₂₆H₂₈O₄N₄], a = 8.413(7), b = 19.166(4), and c = 14.807(28) Å. The crystal structures have been determined by direct methods and refined by full-matrix least square calculations. The ligands have a pronounced saddle-shaped conformation in each structure because of interactions of the methyl groups with the benzene rings. The overall conformations of the neutral ligand and the cobalt complex are remarkably similar.     

Crystal and molecular structure of p-Toluquinone-monoguanylhydrazone,C8H10N4O

The crystal structure of p-toluquinone-monoguanylhydrazone is orthorhombic, space group Pna2₁ with 4 formula units C₈H₁₀N₄O in the unit cell. The lattice constants are a = 7.589, b = 20.117, and c = 5.699 Å. The structure was refined to the conventional R = 0.05. The configuration and conformation of the molecule as well as the unusual hydrogen bridge system are discussed.     

Synthesis and Single Crystal X-Ray Structure of [Na(H2O)2(C18H15O6SO3)]2

Abstract  [Na(H₂O)₂(C₁₈H₁₅O₆SO₃)]₂ was synthesized by sulfated 5-hydroxy-6,7,4′-trimethoxyisoflavone with concentrated sulfuric acid. Single-crystal X-ray diffraction study indicates that it is a dimeric centrosymmetric species. The coordination polyhedron of each Na(I) atom exhibits a distorted trigonal bipyramidal geometry. The dimeric units are linked by intermolecular hydrogen bonds C–H⋯π, C–H⋯O and O–H⋯O to result in a three-dimensional framework. Graphical Abstract  [Na(H₂O)₂(C₁₈H₁₅O₆SO₃)]₂ was synthesized by sulfated 5-hydroxy-6,7,4′-trimethoxyisoflavone with concentrated sulfuric acid. The coordination polyhedron of each Na(I) atom exhibits a distorted trigonal bipyramidal geometry. The dimeric centrosymmetric units are linked by intermolecular hydrogen bonds C–H⋯π, C–H⋯O and O–H⋯O to result in a three-dimensional framework. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal and molecular structure of tetrakis-(phenylenethiourea)tellurium(II) perchlorate hexahydrate,C28H24N8O8S4Cl2Te·6H2O

The synthesis and structural characterization of the title compound, C₂₈H₂₄N₈O₈S₄Cl₂Te·6H₂O are reported. The crystals are triclinic, space group P¯1 (No. 2), withZ=1 in a unit cell of dimensionsa=10.312(7),b=7.144(6),c=14.256(7) Å,=83.04(5),=92.15(5), and=101.25(6)°,V _c =1022 ų. The structure was solved by Fourier methods, and refined by full-matrix least squares toR=0.073 andR _w =0.077 for 1305 unique reflections. The tellurium atom in the molecule lies at a crystallographic center of symmetry, and is bonded to four phenylenethiourea sulfur atoms in a near square-planar arrangement with Te-S(1)=2.666(5), Te-S(2)=2.675(6) Å, and S(1)-Te-S(2)=88.7(3)°. The ligands behave as thiones. The crystal packing is stabilized by the extensive hydrogen bonding involving oxygen and nitrogen atoms. The Cl-O bond lengths are 1.29-1.36 Å and the O-Cl-O angles are 90–130° in the ClO₄ ^– moiety, and differ considerably from the normal values of 1.44 Å and 109°, respectively.