Crystal and molecular structure of nitrito-bis(1,3-propanediamine) nickel(II) tetraphenylborate

The title compound is orthorhombic,M _r =590.2,P2₁2₁2₁ (No. 19),a=9.865(2),b=9.924(2),c=31.202(7) Å,V=3055(2) ų,Z=4,D _x =1.283 g cm^–3, (MoK );F(000)=1256; (MoK )=6.76 cm^–1, finalR=0.052 for 1441 reflections I2.5(I). The nitrite group is chelated via the two oxygen atoms; the two six-membered rings resulting from the coordination of the 1,3-propanediamine ligands to the nickel(II) atom are in the chair conformation. The Ni-N and Ni-O distances average 2.07(1) and 2.14(2) Å respectively. The two Ni-O distances are nearly equivalent.     

Crystal structure of tylophorine methiodide monohydrate,C25H30NO 4 + I−·H2O

The crystal structure of tylophorine (Chemical name 2,3,6,7 tetramethoxy phenanthro [9,10:6, 7] indolizidine. Contribution No. 0871.) methiodide monohydrate has been determined. C₂₅H₃₀NO ₄ ⁺ I^–·H₂0, triclinic, P,a=8.831(1)Å, b=10.842(2),c=13.902(2), =105.0(1)^o, =104.7(1), =97.3(1),V=1210.22ų, Z=2,D _x =1.428 g./cm^–3, (CuK)=1.54184Å, (CUK)=107.2 cm^–1, F(000)=544,T=295^oK,R=0.038,Rw=0.046, for 2331 observed reflections withI2(I). Apart from van der Waals forces, the structure is stabilized by two hydrogen bonds of the type Ow(H) ... O and Ow(H) ... I^– involving the water molecule as the donor and atom O4 of the methoxy group and I^– as acceptors.     

Cl⋯π(Ar), Cl⋯Cl,and other intermolecular interactions in the crystal structure of 8-nitro-6-methyl-2-trichloromethyl-4-dichloromethylene-1,3-benzodioxin

Crystals of the title compound are monoclinic,P2₁,a=9.791(4),b=7.129(3),c=10.428(3)Å,=91.84(3)°,V=727.50ų,Z=2. The structure was solved by direct methods, from data collected at room temperature on an Enraf-Nonius CAD4 diffractometer, and refined by full matrix least squares to a finalR value of 0.045 using 2466 reflections. The molecules form stacks along theb axis of the formA, B, A, B(A=dichloromethylene group; B=aromatic ring in the molecule at –x, 1/2+y, –z to the molecule atx, y, z containing A). Cl(Ar),, ClCl, ClO(N), (Cl₃C)HO intermolecular interactions are also present. An inverse correlation between the (C)ClCl(C) distance and the difference in the corresponding pairs of C-ClCl angles is observed and is interpreted in terms of incipient nucleophile: electrophile attack.     

Crystal and molecular structure of 3-(4-chlorobenzoylimino)-5,6-dihydro-3H-imidazo[2,1-c]-1,2,4-dithiazole

Crystal structure of the title compound belonging to the group of-acylimino derivatives of sulfur(II) compounds has been determined by X-ray structure analysis. The crystals are monoclinic, P2₁/c,a=11.210(2),b=8.197(1),c=13.659(2) Å,=102.36(2)°,V=1226.0(3) ų,Z=4,D _x =1.61 g cm^–3, (MoK)=0.71069 Å,=6.3 cm^–1. The structure has been refined to a finalR value of 0.035 for 1401 observed reflexions.The molecule is nearly planar with symmetrym. The title compound contains a very short intramolecular C=OS contact of 2.328(3) Å, suggesting a bond-non-bond resonance interaction.     

Molecular structure of N-(2-phenylethyl)amide of α-(1,1-ethylenedioxy)-ethyl γ-hydroxybutyric acid (I) and1H NMR spectra of (I) and N-(p-methoxybenzyl)derivative (III)

The spectroscopic and X-ray investigation of the N-(2-phenylethyl) amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid are reported. The¹H NMR spectra for the title structure and for the N-(p-methoxybenzyl) amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid are given. The N-(2-phenylethyl)amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid, C₁₆H₂₃O₄N, crustallizes in the monoclinic space groupP2 ₁/c witha=21.547(5),b=6.333(2),c=11.822(3) Å and =101.01(2)°. The dioxolane ring has a half-chair conformation with C₂(O3)=2.4° and ||_av=18.2°. The inconsiderable deviations from planarity of the six atoms of the amide group are caused mainly by twist around the C4–N1 bond and out-of-plane bending at the N1 atom ((C4–N1)=4°, X_N =7°, X_c =0.4° ). The amide group plane is nearly coplanar with the phenyl ring. The molecules are connected by two intermolecular hydrogen bonds.     

Crystal and molecular structure of [rac-1S,2S,-3S,4R]methyl 2-benzoyl-3,4-dimethyl-4-phenylcyclobutane-1-carboxylate,C21H22O3

The structure of the title compound C₂₁H₂₂O₃, was determined by X-rays.Minr=322.4, monoclinic, space groupP2₁/a,a=11.960(2),b=14.275(3),c=10.858(2) Å,=103.20(2)°,V _c =1804.8 ų,Z=4,D _x =1.223 Mg m^–3. CuK radiation (graphite crystal monochromator,=1.54184 Å),(CuK)=6.53 cm^–1,F(000)=688, T=290 K. Final conventionalR factor=0.050,R _w =0.069 for 1679 unique reflections and 284 variables. The structure was solved usingMultan.     

The structure of 20 oximo-5α-pregnano-16-eno[3,4-C]-1′,2′,5′-oxadiazole (HS976)

The crystal and the molecular structure of the steroidal oxadiazole 20-oximo-5-pregnano-16-eno[3,4-C]-1,2,5-oxadiazole (C₂₁H₂₈N₂O₃) has been determined by direct methods, and refined to a finalR of 0.086 for 3100 observed reflections. The compound crystallizes in space groupP2₁, with cell dimensionsa=18.284(6),b=13.992(4),c=7.370(3)Å,=96.97(3)°;V=1885 ų,Z=4,D _x =1.27 g cm^–3, =1.5418 Å, (CuK =5.95 cm^–1. The two independent molecules are related by a pseudo twofold axis. Both molecules exhibit similar overall topography, rings A, B, C, and D adopting distorted sofa, chair, chair, and distorted envelope conformations, respectively.     

Crystal structures of 1-(2-hydroxyphenyl)-3-phenyl-1,3-propanedione and 1-(1,3-benzodioxol-5-yl)-3-(2,4-dimethoxyphenyl)-1,3-propanedione

1-(2-Hydroxyphenyl)-3-phenyl-1,3-propanedione crystallizes in the triclinic space group (a=5.4233(5),b=13.910(1),c=17.036(1) Å, =68.311(6), =80.854(7), =78.760(8)°) as two independent enolic tautomers in which the hydroxyl and phenolic protons are hydrogen bonded to the ketonic oxygen atom. The structure was refined toR=0.039 for 2085I3(I) reflections. 1-(1,3-Benzodioxol-5-yl)-3-(2,4-dimethoxyphenyl)-1,3-propanedione, which belongs to the triclinic space group (a=7.3990(7),b=8.1239(5),c=14.004(1) Å, =86.673(6). =88.574(7), =64.885(7)°) also exists in the enolic form. The structure was refined toR=0.040 for 1564I3(I) reflections.     

Structure of bis(2-pyridine-N-oxide) diselenide and its formation from tetraphenylantimony(V)selenopyridine-N-oxide

The structure of bis(2-pyridine-N-oxide) diselenide was determined by single crystal X-ray diffraction. The compound crystallized in the triclinic system and the structure was solved in the space group . The lattice constants were determined to bea=7.174(2),b=7.176(2),c=11.070(2) , =87.67(2)°, =73.68(2)°, and =89.57(2)°;Z=2,D _x=1.906 Mg m^–3. The final least squares refinement based on 1942 independent observed reflections yieldedR=0.033,wR=0.044. The Se–Se bond length is 2.326(1) and each Se is coordinated to the O atom of the corresponding N-oxide moiety at a distance of about 2.6 .     

Synthesis and structure of (η5-C5H5)2Hf(η1-NC4H4)2

The crystal structure of (⁵-C₅H₅)₂Hf(¹-NC₄H₄)₂ has been determined from X-ray data measured by counter methods. The title compound is isostructural with (⁵-C₅H₅)₂Zr(¹-NC₄H₄)₂, and crystallizes in the monoclinic space groupP2₁/c (C _2h ⁵ , No. 14) with unit cell constantsa=9.605(3),b=8.174(3),c=19.487(4) Å, =90.85(3)°, andZ=4 forD _c=1.91 gcm^–3. Full-matrix least-squares refinement gave a finalR value of 0.068 for 2154 independent observed reflections. The two cyclopentadienyl rings are ⁵-coordinated to the hafnium atom at an average Hf-C(⁵–) distance of 2.51(1) Å. The Hf-N-centroid (-pyrrolyl) angles average 166°.     

Structure of a binuclear silver(I) complex [Ph3PAg(O2CCH2Ph)]2

The reaction of [Ph₃PAgI]₄ with sodium phenylacetate in MeOH and CH₂Cl₂ at room temperature gave rise to a binuclear silver complex with triphenylphosphine and phenylacetate mixed ligands, [Ph₃PAg(O₂CCH₂Ph)]₂. The crystal and molecular structure of the complex has been determined by single crystal X-ray diffraction analysis. The space group is witha=9.198(2),b=9.516(2),c=13.842(3) Å, =102.00(3), =108.34(3), =93.58(3)°,Z=1, andDc=1.506 g cm^–3. The silver atoms are each coordinated by one phosphorus atom from triphenylphosphine and two oxygen atoms from the carboxylate groups in a T-shape. The complex is further characterized by its IR,¹H, and³¹P NMR spectra.     

Crystal structure of a nucleoside analog: 2′,3′-dideoxy-3′-fluoro-5-bromocytidine

The title compound crystallizes in the orthorhombic space groupP2₁2₁2₁ witha=5.084(1),b=14.322(3),c=16.065(2)Å,Z=4. The structure was solved by the heavy atom method and refined by full-matrix least-squares calculations to a finalR value of 0.033 for 1106 unique observed reflections. The N-glycosidic torsion anglex has a value of –153.7(4)°, in the anti-range. The sugar pucker is²T₃ withP=175(1)° and=30(1)°. The C4-C5 conformation is + sc with =46.7(7)°. The structure is stabilized by N-HN, N-HO and O-HO hydrogen bonds and C-HO close contacts.     

Structure oftrans-dichlorooxobis(triphenylphosphine)rhenium(V), ReCl2O(OEt)(Ph3P)2

C₃₈H₃₅Cl₂O₂P₂Re,M _r=842, triclinic,P¯1,a=17.71(2),b=11.33(1),c=9.82(1) Å,=114.60(3),=90.84(3), =78.05(3),V=1747(2) ų,D _m(flotation)=1.60,D _x=1.60 Mg m^–3 forZ=2, MoK, =0.7107 Å,=41.6 cm^–1,F(000)=836, room temperature. The structure was solved by standard methods from diffractometer data and refined to a conventionalR of 3.4% for 5412 observed reflections. The Re atom is six coordinate octahedral withtrans-Cl atoms andtrans-Ph₃P groups. Relevant bond distances are: Re-P 2.533(1) and 2.535(1) Å, Re-O(ethoxo) 1.888(4) Å, and Re-O(oxide) 1.699(4) Å. The ethyl chain is partially disordered.     

Crystal structure of 1,2,4,6-tetraphenylpyridinium tetrabromoferrate(III)

The title structure, which belongs to the triclinicP¯1 space group witha=13.901(4),b=10.732(1),c=10.570(8)Å=109.14(4),=96.17(4), =90.34(2)°, is refined toR=0.052 for 2985I3(I) reflections. The structure consists of a non-interacting 1,2,4,6-tetraphenylpyridinium and tetrahedral tetrabromoferrate (III) ions.     

Crystal structure of 6-nitrobenzo(a)pyrene

In 6-nitrobenzo(a)pyrene, an environmental pollutant, the nitro substituent lies at 69.5(1) to the mean plane of the aromatic moiety. The C–C bond distances range from 1.341(3) to 1.443(3) Å. The crystal is in the monoclinic space group, P2₁/c, with a = 8.3239(3) Å, b = 8.9530(3) Å, c = 18.0678(5) Å, = 99.264(2) and Z = 4. Molecules are assembled in sheets in the unit cell through stacking and alternating C–H O interactions.     

Reactions of aromatic nitro compounds with acetophenone in the presence of alkali. Crystal structure of (E)-1,2-dibenzoyl-o-tolylaminoethylene

Methyl and methoxy substituted nitroarenes were reacted with acethophenone in the presence of sodium ethoxide in ethanol giving arylamino-conjugated diketo derivatives. A case ofipso-substitution of a methoxy group is discussed. The title compound C₂₃H₁₉NO₂ (M _r =341.4) crystallizes in the monoclinic system, space groupP2₁/n witha=21.579(4),b=8.526(2),c=9.983(2) Å;=92.3(1)°;V=1835.2(7) ų,Z=4,D _c =1.24 g cm^–3,(Cu-K )=5.9 cm^–1, =1.5418 Å,F(000)=720. The molecule adopts theE configuration with the C=O carbonyl groupstrans with respect to the ethylenic double bond.     

Crystallographic and IR spectral study ofcis-bis(creatinine-N)dinitro platinum(II)

Acis-Pt(creat)₂(NO₂)₂ complex was synthesized stereoselectively in a high yield (65%) and characterized by IR spectral and X-ray diffraction analysis. Crystal data: Pt(C₄H₇N₃O)₂(NO₂)₂,M _r=767.55, monoclinic, space groupP2₁/n,a=9.736(1),b=13.433(1),c=12.098(1) Å,=110.55(1)°,V _c=1482(1) ų,Z=2,D _x=3.441 g cm^–3,(MoK)=0.71073 Å,=97.0 cm^–1,F(000)=1504,T=292 K,R=0.026 andR _w=0.028 for 2061 observed reflections with I>2(I). The structure consists of Pt(creat)₂(NO₂)₂ molecules disposed in general positions and joined by N-HO and N-HN hydrogen bonds. The platinum atom has square-planar PtN₄ coordination of twocis disposed pairs of nitro [Pt-N_av 2.023(7) Å] and creatinine [Pt-N(endo)_av 1.991(8) Å] ligands. The creatinine moieties are planar and tilted to the equatorial plane by ~80°.     

The molecular structure of dibutylbis(2-pyridinethiolato-5-ethyl ester)tin(IV), [SnBu2(TNEE)2]

The crystal structure of [SnBu₂(TNEE)₂], (HTNEE=5-ethyl ester of 2-mercaptopyridine-5-carboxylic acid) has been determined by X-ray single crystal diffraction study. The crystal is triclinic, space groupP,a=10.042(1),b=18.421(2),c=7.979(1) Å, =98.7(1), =107.3(1), =87.7(1)^o,V=1393(1) ų, and Z=2 The tin center is coordinated to two butyl groups and to the nitrogen and the sulfur atoms of two ligand molecules in a very distorted trapezoidal bipyramid.     

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.     

The crystal structure of 5-methyl-1-(octahydro-1-iodo-1H-1-inden-4-yl)-1H-tetrazole

The title compound is C₁₁H₁₇N₄I, F.W.=330.20, monoclinic, space groupP2₁/a,a=11.586(2),b=10.617(1),c=10.417(1) Å, =94.567(2)°,Z=4,F(000)=652, (MoK)=0.7107 Å, (MoK)=2.31 mm^–1,V=1277.31 Å₃,D _C=1.71 gcm^–3,D _m=1.70 gcm^–3. The structurewassolved by Patterson and Fourier methods and refined to anR value 0.031 for 1620 observed reflections. The connectivity and conformation of the addition product ofcis-1,5-cyclononadiene and iodine azide was determined by X-ray analysis. The reaction product contains a chair-conformation cyclohexane ring that iscis fused to a cyclopentane ring. The cyclopentane ring has an envelope conformation and an equatorially oriented iodine substituent. A planar tetrazole ring is axially substituted on the cyclohexane ring. The plane of the tetrazole ring makes a dihedral angle of 69.6° with the average plane of the carbon atoms of the cyclohexane ring.