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 and molecular structure of a naphthalene-tolan photoadduct: 1,8-Diphenyl-1a,2,7,7a-tetrahydro-1,2,7-metheno-1H-cyclopropa[b]naphthalene

The title compound, C₂₄H₁₈, crystallizes in the monoclinic space groupP2₁/c with cell parametersa=16.382(10),b=6.360(3),c=18.051(11) Å, =116.6(1) °,Z=4,V=1695.6 ų. The structure was solved by direct methods and refined using least-squares procedures to a finalR of 0.097 for 811 observed (I>2₁) structure magnitudes. The variables refined were the fractional coordinates of all atoms and the individual isotropic temperature factors of the nonhydrogen atoms. The highly strained molecule has single carbon-carbon bond distances of 1.47–1.59 Å, and bond angles between 59 and 136 °.     

The crystal structures of NaAlR4, R=methyl,ethyl, and n-propyl

The crystal structures of the title compounds have been determined from diffractometer data and refined by full-matrix least squares. NaAlMe₄ is orthorhombic,Cmcm,a=9.234(3),b=9.221(3),c=8.303(2) Å,Z=4,D _c=1.03 g cm^–3,R=0.029 for 278 data. NaAlEt₄ is monoclinic,P2₁/c (No. 14),a=13.900(2),b=13.207(2),c=14.443(1) Å,=117.43(1)°,Z=8,D _c=0.94 g cm^–3,R=0.056 for 2747 data. NaAl(n-Pr)₄ is monoclinic,C2/c,a=9.802(5),b=15.336(4),c=21.611(10) A,=98.34(4)°,Z=8,D _c=0.92 g cm^–3,R=0.072 for 899 data. Coordination of Al is essentially tetrahedral in all structures, and closest contacts to Na⁺ involve-carbon atoms of alkyl groups.     

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.     

Structural and spectral studies of N-trans-cinnamylidene-m-toluidine and N-trans-cinnamylidene-m-chloroaniline

N-trans-cinnamylidene-m-toluidine (1) C₁₆H₁₅N, and N-trans-cinnamylidene-m-chloroaniline (2) C₁₅H₁₂NCl form isomorphous crystals which are monoclinic, space group P2_l/c, with unit cell dimensionsa=5.967(2),b=13.793(3),c=15.048(5) Å, =91.97(3)° anda=5.868(2),b=13.788(4),c=15.191(4) Å, =91.87(3)°, respectively. The single-crystal X-ray structure determinations of the title compounds revealtrans structures. Ring (A) C_10–15 and ring (B) C_1–6, are practically planar in both structures with dihedral angels of 61.3(3) and 63.6(2)°, respectively.¹H nmr, u.v. and i.r. spectra are also reported.     

The crystal structure of a N-(2-thiophenyl)-salicylaldiminopiperidino nickel(II) complex

The crystal and molecular structure of the title complex, C₁₈H₁₉N₂OSNi, has been determined by direct methods. The compound crystallizes in monoclinic crystal system witha=11.968(1),b=12.182(1),c=12.399(1) Å, =115.23(1)°, space group P2₁/n. Nickel is in a slightly distorted square-planar environment of two nitrogens [1.881(2) and 1.952(2) Å] and one oxygen [1.856(3) Å] and one sulphur [2.138(2) Å] atom. Ni is 0.005 Å out of the plane of its ligands.     

Crystal and molecular structure of 1,4-S,S′-bis-isothiosemicarbazidebutane dihydrobromide

The synthesis and crystal structure of 1,4-S,S-isothiosemicarbazidebutane dihydrobromide have been presented. The crystals are monoclinic:P2₁/n, a=7.9910(10),b=10.979(2),c=8.9240(10)Å, =111.450(10)°,Z=2, room temp. The structure was solved by direct methods. and refined to R=0.0297 for 846 reflections. The title compound consists of the centrosymmetric [C₆H₁₈N₆S₂]²⁺ dication and two Br^– anions. Intramolecular N–H...N and intermolecular N–H...Br hydrogen bonds stabilizetrans conformation of the thiosemicarbazide moiety.     

The crystal and molecular structure of [K·DB-18-C-6][AlMe3NO3]·0.5C6H6

The use of dibenzo-18-crown-6 in the synthesis of trimethylaluminum adducts of KNO₃ results in the formation of a 1/1 adduct, [K·DB-18-C-6]-[AIMe₃NO₃]. The crystal structure of [K·DB-18-C-6][AlMe₃NO₃]-has been determined from single-crystal X-ray diffraction data collected by counter methods. The title compound crystallizes in the monoclinic space groupP2₁/c (No. 14) with unit cell parametersa=11.804(3),b=28.828(4),c=9.118(3) Å, =96.61(3)°, andD _calc=1.23 forZ=4. Least-squares refinement gave a final conventionalR value of 0.045 for 983 independent observed reflactions. The potassium atom is centered among the six oxygen atoms of the crown at an average KO contact of 2.74(2) Å. Its environment is completed by an oxygen atom of a nitrate anion (2.88 Å) and a benzo group (>3.44 Å) of a neighboring crown ether. The trimethylaluminum moeity is coordinated to the nitrate anion by an oxygen atom at an Al-O bond distance of 1.92(1) Å.     

Properties and structural characterization of a complex salt, 2[C12H18N4OS]·[Sb2Cl10], obtained by the reaction of thiamine (vitamin B1) with antimony trichloride

Thiamine hydrochloride (vitamin B₁) reacts with antimony trichloride in methanol to produce a crystalline compound which has been characterized as the salt 2[C₁₂H₁₈N₄OS]·[Sb₂Cl₁₀] by X-ray crystallography. The compound crystallizes in the triclinic space group ,b=11.029(2),c=12.234(2) Å, =108.75(2), =102.67(2), =103.59(2)°,U=1041.52 ų,D _c=1.80 g cm^–3,Z=1. The crystal structure consists of discrete [C₁₂H₁₈N₄OS]²⁺ cations and chloro bridged [Cl₄Sb(-Cl)₂SbCl₄]^4- anions in 2:1 ratio, held together by hydrogen bonds and electrostatic forces.     

Crystal and molecular structures of two polymorphic forms of dimethyl-N-(2-ethylphenyl)-phosphoramidate (I) and dimethyl-N-(2,6-dimethylphenyl)-phosphoramidate (II)

The crystal structures of the phosphoric amides dimethyl-N-(2-ethylphenyl)-phosphoramidate (I) and dimethyl-N-(2,6-dimethylphenyl)-phosphoramidate (II) have been determined by direct methods and refined by full-matrix least squares. Compound (I) crystallizes in two polymorphic forms, both monoclinicP2₁/c, but with different cell parameters. Parameters for compound (I) are: FormA:a=10.878(5),b=8.890(4),c=25.11(1) Å,=92.18(2)°; FormB:a=7.071(4),b=17.059(9),c=10.221(5) Å,=97.07(2)°. Compound (II) is also monoclinicP2₁/c witha=8.453(4),b=14.231(7),c=10.283(5) Å,=108.95(2)°. Compound (I) exists as a hydrogen-bonded dimer, whereas compound (II) exists as a hydrogen-bonded polymeric species.     

Crystal and molecular structures of the 4-(1H)-pyridone (=L) lanthanide complexes {[GdL(NO3)3(H2O)]·CH3OH}2 and [DyL4(NO3)2](NO3) and of L2HNO3

The crystal structures of the title compounds have been determined by single crystal diffraction methods. Crystals of the dysprosium compound are monoclinic, space groupP2₁/c witha=14.133(4),b=13.438(5),c=14.401 (4)Å,=103.98(2)°,V=2654(1)ų,Z=4,D _c =1.82 g cm^–3, finalR=0.035. The Dy atom is eight-coordinate with a distorted dodecahedral coordination geometry involving two bidentate nitrate groups and four pyridone oxygen atoms. An erbium complex with analogous stoichiometry was also prepared but not structurally characterized. Crystals of the Gd compound are monoclinic, space groupP2₁/n, witha=11.226(2),b=9.075(2),c=16.737(3)Å,=93.88(3)°,V=1701(1)ų,Z=2,D _c =1.91 g cm^–3, finalR=0.042. Each Gd atom is bonded to one pyridone oxygen atom, a water molecule and three bidentate nitrate groups. An oxygen atom of one of the bidentate nitrates additionally serves to bridge pairs of Gd atoms so as to form a dinuclear complex in which each Gd atom is nine-coordinate with a tricapped trigonal prismatic geometry. Crystals of L₂HNO₃ are monoclinic, space groupI2/a witha=12.479(4),b=6.535(2),c=14.297(6)Å,=96.07(3)°,V=1159(1)ų,Z=4,D _c =1.45 g cm^–3, finalR=0.057. The pyridones are linked in pairs by very short (2.44 Å) symmetrical OHO hydrogen bonds. Each pair is further linked via a nitrate ion by means of N-HO(nitrate)H-N hydrogen bonds, so as to form an extended chevron-like pyridone-pyridone-nitrate-pyridone-pyridone array. Adjacent chains are linked via weak C-HO(NO₃) interactions.     

Crystal structure of bis-(rhodanine)copper(I) iodide,C6H6CuIN2O2S4

The structure of the polymeric rhodanine compound, C₆H₆CuIN₂O₂S₄, was determined by X-rays.M _r =456.8, monoclinic, space groupP2₁/c,a=4.1947(7),b=17.6999(12),c=17.1048(8) Å,=96.15(1)°,V _c =1262.6 ų,Z=4,D _c =2.40Mg m^–3, CuK radiation (graphite crystal monochromator, =1.54056 Å),(CuK)=278.9 cm^s-1,F(000)=872,T=290 K. Final conventionalR-factor=0.029, andR _w =0.044 for 2384 unique reflections and 153 variables. The structure was solved using Patterson methods andDirdif, and refined by full-matrix least-squares methods. The compound forms zigzag chains alonga. The copper atom is in trigonal pyramidal coordination, with two sulfur atoms of the thiocarbonyl group and two bridging iodine atoms. The copper-sulfur distances are 2.278(1) and 2.299(1) Å, and the copper-iodine distances are 2.657(1) and 2.814(1) Å.     

Structure of 9-oxa-2,3-(4′-methoxy)-benzo bicyclo[4,3,0]non-1(6)-ene-7,8-dione: C13H10O4

The crystal and molecular structure of the title compound: C₁₃H₁₀O₄,M _r=230.22, determined by single crystal X-ray diffraction is reported. Crystals are monoclinic, space groupP2_l/c,a=3.991(3),b=21.381(4),c=12.289(4)Å,b=91.15(1)°,V=1048(1)Å₃,z=4,D _x=1.46Mg m^–3, (MoK)=0.7107 Å,m=0.87 mm^–1,F(000)=480,T=298 K. The structure was solved by direct methods and the finalR value is 0.071 (wR=0.055) for 795 independent observed reflections. The cyclohexadienic moiety of the molecule adopt a twist conformation.     

Synthesis and crystal structure of cis-1-benzylidene-1,2,3,4-tetrahydronaphthalene,containing an unexpected conformation of the cyclohexenylidene ring

Two isomers of 1-benzylidene-1,2,3,4-tetrahydronaphthalene have been synthesized by the Wittig reaction, and the crystal structure of the cis-isomer has been solved. The compound C₁₇H₁₆ crystallizes in the monoclinic space groupP2₁/n witha=9.796(2),b=5.490(5),c=23.215(3)Å,=95.11(2)°, andZ=4. The structure was determined by direct methods, and refined by fullmatrix least squares toR=0.047 for 1104 reflections. The cyclohexenylidene ring has the unusual envelopec _s ^{2, 10} conformation.     

Synthesis and crystal structure of 1-vinyl-cis-2,3-diphenylaziridine

1-Vinyl-cis-2,3-diphenylaziridine, C₁₆H₁₅N, has been synthesized and characterized by spectroscopic methods and single crystal X-ray analysis. The structure was studied at room temperature (2a) (18°C) and at low temperature (2b) (–70°C). The title compound crystallizes in the space group Cm with Z=2 showing no phase transformation between the two temperatures. The cell parameters area=8.258(3),b=15.880(3),c=5.827(2)Å, =122.32(2)° for (2a) anda=8.188(2),b=15.762(3),c=5.724(1)Å, =121.57(2)° for (2b). Both the studies show nearly the same conformation. With the exception of the vinyl group, the molecule hasm symmetry, so, the asymmetric unit is half a molecule. The mirror plane of the space group cuts the aziridine ring through the N atom. The vinyl group is distributed on two symmetrical positions by means of the same mirror plane. In this way, the crystal is built with the two diastereoisomers of the title compound.     

Crystal and molecular structures of trichloro (π-cis-but-2-en- 1,4-diammonium) platinum(II) chloride and trichloro(π-cis-pent-2-enylammonium) platinum(II)

The structures of the olefinic complexes of platinum(II) withcis-but-2-en-1,4-diammonium, [PtCl₃(C₄H₁₂N₂)]⁺, and withcis-pent-2-enylammonium, [PtCl₃(C₅H₁₂N)], the first one as its chloride, have been determined by single-crystal X-ray methods. The compounds form yellow monoclinic crystals, witha=11.238(3),b=12.234(4),c=7.769(1) Å, = 112.99(2) ° anda= 11.530(3),b=9.037(3),c= 10.067(3) Å, =105.50(2) °, respectively; both crystallize in the space groupP2₁/c withZ=4. The structures, solved by standard methods, have been refined anisotropically by full-matrix least-squares methods, both toR=0.040, on, respectively, 1808 and 1849 independent reflections collected by counter methods.In both complexes, platinum is four-coordinate to the three chlorine atoms and the double bond of the olefinic ligand. The structures are discussed, and comparison with the analogous platinum(II)-olefin complexes with the trans isomers of the olefinic ligands is made.     

Crystal and molecular structures of 1-(2-iso butylylcarbamoyl propan-2-ylamino) 3-(1-naphthyloxy)propan-2-ol hydrochloride (1) (C21H31N2O3Cl) and 1-(2-isobutyloxycarbonylo propan-2-ylamino) 3-(1-naphthyloxy)propan-2-ol hydrochloride (2) (C21H30NO4Cl)

This paper shows the crystal structures of two new-adrenergic antagonists, derivatives of propranolol, which were determined with three-dimensional x-ray diffraction data. The space groups and unit-cell parameters are: compound1 (C₂₁H₃₁N₂O₃Cl) monoclinic space groupP2₁/c,a=20.523(4),b=6.909(2),c=15.950(2) Å,=105.03(1)°; compound2 (C₂₁H₃₁NO₄Cl) monoclinic space groupP2₁/c,a=6.364(2),b=36.043(8),c=10.149(1) Å,=104.48(2)°. The structures were solved with direct methods, and refined with full-matrix least-squares techniques toR indices of 0.059 and 0.067, respectively. The-CH(OH)-CH₂-NH-sections of the side chains show the conformation approximate togauche.     

Crystal and molecular structures of 5,7-dimethyl-1,8-naphthyridine-2-ol (=LH) and of its mercury (II) complex HgL2 and synthesis of some lanthanide/HgL2 heterometallic complexes

The crystal structures of the title compounds have been determined by single crystal diffraction methods. Crystals of 5,7-dimethyl-1,8-naphthyridine-2-ol (1) are monoclinic, space groupP2₁/n witha=7.336(2),b=8.989(2),c=13.125(3)Å,=95.72(3)°,V=861.2(4)ų,Z=4,D _c =1.34 g cm^–3, finalR=0.052. The molecules are linked in pairs by two N-HO hydrogen bonds, and these dimers are stacked in a discontinuous, stepped fashion. Crystals of HgL₂ (2) are monoclinic space groupP2₁,/c witha=4.044(2),b=12.147(2),c=18.093(5)Å,=93.32(2)°,V=887.3(4)ų,Z=2,D _c =2.05 g cm^–3, finalR=0.051. In2 the mercury binds to N(1) to form a linear N-Hg-N coordination geometry, and the HgL₂ molecules form a continuous stacked structure. The syntheses of the compounds ML₄(NO₃)₃·H₂O (M=Nd, Gd, and Er), PrHg₂L₄(NO₃)₃, andM ₂Hg₃L₆(NO₃)₆ (M=Gd, Er) are also reported.     

Crystal structures of 3-(4-pyridinyl)-5,6,7,8-tetrahydro-1,2,4-triazolo[4,3-a]pyrimidine and its 6-hydroxy derivative

(1): C₁₀H₁₁N₅,M _r=201.23, from water, P ,a=6.913(1),b=8.198(2),c=9.212(2) Å, =72.36(2), =109.03(2) and =88.13(1)^o,D _x=1.436 g/cm³,Z=2. FinalR=0.043 for 1477 observed reflections. (2): C₁₀H₁₁N₅O,M _r=217.23, from methanol/water solution. P2₁/c,a=9.291(2),b=11.263(3),c=10.454(3) Å, and =114.05(1)^o,D _x=1.444, g/cm³,Z=4. FinalR 0.056 for 1587 observed reflections. The data were collected on a diffractometer at room temperature. Structures were solved by direct methods and refined by anisotropic full-matrix least-squares method. In the solid state both molecules have the same conformation and are packed in similar manner. The planarity of the condensed triazole ring and its electrons conjugation with a lone pair at N8 impose C6 sofa conformation of the saturated diazine rings. Hydroxy group in2 is in an energetically unfavorable axial position. Both in1 and2, N8–H ... N34 hydrogen bonds join molecules into infinite chains, and O6–H ... N1 hydrogen bonds in2 span the chains into two-dimensional net. The molecules in hydrogen bonded chains and sheets have the same chirality.     

Crystal structures of two isomeric oximes. (EE)-2-methyl-3-phenyl-3-thiocyanatopropenaldoxime and (Z)-5-methyl-6-phenyl-1,3-thiazin-2-one oxime

The crystal structure of two isomeric oximes, C₁₁N₁₀N₂OS have been studied by X-ray diffraction. The open-chain thiocyanato derivative is somewhat'less dense and crystallizes with the orthorhombic space group Pbcn;a,b,c=18.718(1), 10.601(3), 11.528(1) Å,Z=8. The heterocyclic isomer occurs as pseudo-orthorhombic (Cmma)twinned crystals of space group P2₁/n, a, b, c, =12.11(1), 7.46(1), 12.12(1) Å, 100.09(1)^o,Z=4. Twinning occurs as a result of the near-equality of the monoclinica andc cell constants.