The crystal structures of p-halo-N-(p-cyanobenzylidene)aniline and p-cyano-N-(p-halobenzylidene)aniline (halo = bromo and chloro)

p-Bromo-N-(p-cyanobenzylidene)aniline is triclinic, has space group P , at 173 K, with a = 7.3892(15), b = 12.087(2), c = 7.0283(14) Å, = 105.24(2), = 98.11(2), = 98.89(2)°, Z = 2, V = 587.4(2) ų. p-Chloro-N-(p-cyanobenzylidene)aniline is triclinic, space group P , at 173 K, with a = 7.317(2), b = 12.165(3), c = 6.990(2) Å, = 104.02(2), = 100.96(2), = 100.76(2)°, Z = 2, V = 574.7(3) ų. p-Cyano-N-(p-bromobenzylidene)aniline is orthorhombic, has space group P2₁2₁2₁, at 173 K, with a = 10.333(3), b = 4.732(3), c = 23.526(5) Å, Z = 4, V = 1150.3(8) ų. p-Cyano-N-(p-chlorobenzylidene)aniline is orthorhombic, has space group P2₁2₁2₁, at 173 K, with a = 10.161(2), b = 4.713(2), c = 23.509(5) Å, Z = 4, V = 1125.8(4) ų. In the two cyanobenzylidene compounds there are chains of molecules held together by CN······X interactions. The chains form two-dimensional sheets similar to those in the iodo analog, but with a different stacking arrangement between the sheets. In the two halobenzylidene compounds there are no CN······X contacts; rather there are short X······X and C–H······NC contacts.     

Crystal structures of 1,1-di(p-substituted phenyl)-2,2-dinitroethylenes

The X-ray crystal structures of 1,1-di(p-methylphenyl)-2,2-dinitroethylene (2), 1,1-di(p-methoxylphenyl)-2,2-dinitroethylene (3), 1,1-di(p-fluorophenyl)-2,2- dinitroethylene (4), 1,1-di(p-chlorophenyl)-2,2-dinitroethylene (5), and 1-phenyl-1- (p-nitrophenyl)-2,2-dinitroethylene (6) are reported and compared with that of 1,1-diphenyl-2,2-dinitroethylene (1). Owing to steric repulsion between the aryl rings, the single bond lengths between C(1) and the two ring carbons atoms are longer than the normal sp²–sp² bond distance of 1.46 Å. For 4–6 in which the aryl rings contain electron-withdrawing substituents (F, Cl, NO₂), the double bonds between C(1) and C(2) are shorter than those in 2 and 3, whose aryl rings containing electron-donating substituents. Furthermore, the steric repulsion between the aryl rings and C NO₂ fragments results in an appreciable twist about the central double bond. The two aryl rings of compounds 1–6 make dihedral angles of 77.7, 66.6, 62.8, 80.9, 82.0, and 71.2°, and the two C NO₂ fragments make dihedral angles of 68.5, 67.8, 65.9, 76.9, 73.0, and 71.9°, respectively.     

Synthesis and crystal structure of Bi(mpo)3 (Hmpo = 2-mercaptopyridine N-oxide)

The synthesis as well as crystal and molecular structure of [Bi(C₅H₄NOS)₃] are reported. The complex crystallizes in the monoclinic system, space group P2₁/n with lattice parameters a = 9.6521(3) Å, b = 10.0659(4) Å, c = 18.4484(7) Å, = 102.13(6)°, and D _calc = 2.227 Mg · m^–3 for Z = 4. It is clear from the packing diagram that the title compound is a dimer via the secondary coordination. Surrounding Bi atom, three five-membered ring planes (Bi,O,N,C,S) make a dihedral angle of 55.91, 54.72, and 26.13° respectively. The whole crystal presents a three-dimensional network structure as each molecule produces four weak C–H O hydrogen bonds and a weak C–H S hydrogen bond.     

Preparation,spectral studies,and X-ray crystal structures of (16S, 17R, 20S)-3-oxo-16-hydroxy-25-nor-lanostan-24-oic lactone (II) and (16S, 17R, 20S)-4,16-dihydroxy-25-nor-3,4-seco-lanostan-3,24-dioic acid dilactone (III)

The crystal and molecular structures of the title compounds have been determined by direct methods, and refined to a finalR of 0.059 forII and 0.046 forIII. Both molecules crystallize in space group P2₁2₁2₁. The cell dimensions forII area=10.096(5),b=11.255(3),c=20.300(7) Å;Z=4,D _x=1.188 g cm^–3, (MoK)=0.70 cm^–1, while the cell dimensions forIII area=7.346(1),b=10.470(3),c=30.546(5) Å;Z=4,D _x=1.212 g cm^–3, (MoK)=0.74 cm^–1. The rings of the triterpene skeletons aretrans-cis-trans-cis connected. The conformations of both molecules are discussed. Also the preparation and the spectral data of (17R, 20S)-3,16-dioxo-25-nor-lanostan-24-oic acid (V) and (17R, 20S)-3,16,24-trioxo-25-hydroxy-16,24-seco-lanostan-25-acetate (VI) are given.     

Structure and characterization of hexakis(imidazole) cobalt(II) complexes: [Co(Im)6(OBz)2] and [Co(Im)6(mB)2] (Im = imidazole, OBz = benzoate, mB = p-methoxybenzoate)

The crystal and molecular structures of the complexes of [Co(Im)₆(OBz)₂] and [Co(Im)₆(mB)₂] (Im = imidazole, OBz = benzoate, mB = p-methoxybenzoate) have been determined by X-ray crystallography. The crystal structures are very similar and consist of discrete molecules of [Co(Im)₆(OBz)₂] and [Co(Im)₆(mB)₂], respectively. They both crystallize in the triclinic system, space group the former with lattice parameters a = 7.6934(3), b = 10.4518(5), c = 11.6088(5) Å, = 73.920(1), = 79.023(1), = 73.681(1)°, and Z = 1; the latter with a = 9.8336(3), b = 10.5509(2), c = 10.8889(3) Å, = 61.450(1), = 76.832(1), = 71.157(1)°, and Z = 1. The cobalt(II) ions have octahedral geometry with a CoN₆ chromophore. In the solid state, the complexes all form a three-dimensional network through N—H···O hydrogen bonds. The electronic spectra and IR spectra data are in agreement with the structural data.     

The structures of N-(t-butoxycarbonyl)-3-methylbenz[f]indole and N-benzenesulfonyl-4-bromo-3-methylbenz[f]indole

N-(t-butoxycarbonyl)-3-methylbenz[f]indole,1, C₁₈H₁₉NO₂, crystallizes in orthorhombic space groupPna2₁ witha=6.0338(2),b=24.839(4),c=10.2481(7) Å,V=1535.9(3) ų,Z=4. The structure was refined toR=0.051 for 2007 observed reflections. The benz[f]indole ring system is nearly planar, exhibiting mean deviation of 0.048 Å. The ester plane of thet-butoxycarbonyl substituent is nearly coplanar with the benz[f]indole ring system, forming a C?N?C=O torsion angle with magnitude 10.6(5)⁰.N-benzenesulfonyl-4-bromo-3-methyl-benz[f]indole,2, C₁₉H₁₄BrNO₂S crystallizes in triclinic space groupP?1 witha=8.1400(5),b=10.0587(8),c=10.8863(7) Å, α=89.927(7), β=110.495(5), γ=96.846(6)⁰,V=828.2(3) ų,Z=2. The structure was refined toR=0.050 for 2653 observed reflections. The benz[f]indole ring system is nearly planar, with mean deviation 0.016 Å, and forms a dihedral angle of 80.93(9)⁰ with the phenyl plane.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

The crystal and molecular structure of (−)—Crinine (C16H17NO3)

(–)—Crinine, C₁₆H₁₇NO₃, is an alkaloid extracted from the bulbs of Pancratium maritimum L. (Amaryllidaceae). The compound crystallizes in the space group P2₁2₁2₁ with cell dimensions a = 6.040(1), b = 12.382(1), c = 17.861(2) Å, with Z = 4. The molecule has five rings and an OH group. The N-containing, five-membered ring and the D ring have envelope conformations. The A and B rings have distorted chair and half-chair conformations, respectively.     

Synthesis and structural characterization of fac-BrMn(CO)3{PH(C6H5)2}2

In attempts to find appropriated methods for preparation of unstable sulfinyl and sulfonylphosphane complexes we have synthesized the diphenylphosphine complexes of Mn(I), BrMn(CO)₄PHPh₂, (1) and BrMn(CO)₃(PHPh₂)₂ (2). Both should undergo electrophilic substitution in the presence of an adequated base. Parallel to the reactions of stabilization of phosphanes we have studied by means of x-ray analysis the structure of fac-BrMn(CO)₃(PHPh₂)₂ (2). The compound crystallizes in the triclinic space group P, a = 9.840(2), b = 11.207(2), c = 13.083(3) Å, = 72.00(3), = 69.59(3), = 81.41(3)°, U = 1284.7(4) ų, and Z = 2. In this complex the manganese atom shows an octahedral coordination geometry, with three carbonyl ligands in a fac arrangement, and one bromide and two diphenylphosphine ligands cis to each other.     

Syntheses and crystal structures of two soybean isoflavone derivatives

Two soybean isoflavone derivatives, 7-methoxy-4′-hydroxyisoflavone (1) and 4′, 7-diethoxyl-5-hydroxyisoflavone (2) were synthesized and their crystal structures were determined by single-crystal X-ray diffraction. Two derivatives crystallize in the monoclinic crystal system, space group P2₁/c. The cell dimensions of 1 are a = 8.696(4) Å, b = 11.947(5) Å, c = 12.078(5) Å, β = 93.594(7)^∘, D_c = 1.423 Mg/m³, V = 1252.3(10) ų, Z = 4, and those of 2 are a = 37.672(12) Å, b = 11.228(4) Å, c = 7.582 (3) Å, β = 94.150(6)^∘, D_c = 1.355 Mg/m³, V = 3198.6(18) ų and Z = 8. They have the same isoflavone skeleton which is composed of a benzopyranone moiety and a phenyl moiety. Hydrogen bonding and π < eqid1 > π stacking interactions assemble 1 into supramolecule with a three-dimensional network. And in the crystal structure of 2, hydrogen bonding and C–H ⋅s π stacking interactions lead to the formation of a two-dimensional network.     

Synthesis and crystal structures of the bis-Schiff bases of 2-(methylthio)aniline with isophthaldehyde, terephthaldehyde, and para-diacetylbenzene

The crystal structures of the new compounds 1,3-bis(((2-methylthio)phenylimino)methyl)benzene (1), 1,4-bis(((2-methylthio)phenylimino)methyl)benzene (2), and 1,4-bis(1-((2-methylthio)phenylimino)ethyl)benzene (3) were obtained by single crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic space group Pna2₁ with a=16.8250(13) ?, b=18.1068(13) ?, c=6.3086(5) ?; and Z=4. Compound 2 crystallizes in the triclinic space group with a=6.7532(7) ?, b=9.4433(9) ?, c=15.2473(15) ?; and α=86.339(2)°, β=80.609(2)°, γ=80.962(2)°; and Z=2. Compound 3 crystallizes in the triclinic space group with a=6.787(3) ?, b=7.517(3) ?, c=10.653(4) ?; and α=89.998(7)°, β=72.341(7)°, γ=75.998(7)°; and Z=1. Details of the synthesis, structures, and spectroscopic results are discussed.     

The crystal structure of a novel product from the acid-catalyzed condensation of 1-benzylindole with acetone

The acid-catalyzed condensation of 1-benzylindole with acetone in the presence of N-phenylmaleimide gave a tetrahydrocarbazole, (4,5,10,10b-tetrahydro-5-methyl-2-phenyl-10-(phenylmethyl)pyrrolo[3,4-a]carbazole-1,3[2H, 3aH]-dione (1), as the major product and a novel spiro compound, 1,3,4,4-tetrahydro-1,1,3,3-tetramethyl-4,4-bis(phenylmethyl)-1,3(2H, 2H)-spiro[cyclopent[b]indole] (2), as the minor product. The structure of the spiro compound was determined by an X-ray crystallographic determination. The acid-catalyzed condensation of 1-benzylindole with acetone in the absence of N-phenylmaleimide gave a bisindole, (1,1-bis(phenylmethyl)-3,3-(1-methylethylidene)diindole (3), as the major product and the spiro-compound as the minor product.     

The crystallographic structure of 4-hydroxy-3-methylene-4-(p-nitrophenyl)butan-2-one

The crystallographic structure of 4-hydroxy-3-methylene-4-(p-nitrophenyl)butan-2-one 1 is disclosed by x-ray analysis. It crystallized in the space group C2/c (#15) with a = 19.958(4), b = 10.486(3), c = 15.009(3) Å, = 137.553(6)°, V = 2120.0(9) Å,³ Dcalc = 1.386 g/cm³, and Z = 8.     

X-ray crystal structure and spectroscopy of a pseudo-square pyramidal Cu(II) complex, trans-dinitratotetrakis (trans-4-styrylpyridine)copper(II)

Single crystals of the title Cu(II) complex, [Cu(stpy)₄(ONO₂)(ONO₂)] [stpy = trans-4-styryl-pyridine] have been prepared and characterized by elemental and thermal analyses, IR, electronic and EPR spectral measurements, and X-ray crystal structure determination. The complex crystallizes in the monoclinic space group P2₁/c with unit-cell parameters, a = 12.985(2), b = 22.865(8), c = 17.024(10) Å, = 112.29(3)°, and Z = 4. The structure consists of discrete monomeric units of [Cu(stpy)₄(ONO₂)(ONO₂)]. The equatorial positions of the Cu(II) polyhedron are occupied by nitrogen atoms of the four stpy ligands and the axial positions by the oxygens of two unidentate nitrate anions. One of these oxygens is at rather longer distance [2.609(3) Å] and may be considered to be semicoordinated. If this semibond is ignored, the coordination geometry lies closer to an idealized square pyramid than to the trigonal bipyramid geometry. IR spectra reveal nitrogen coordination from stpy and asymmetry in the monodentate oxygen binding of the two nitrate ligands. The optical reflectance band at 600 nm suggests pseudo-square-based pyramidal geometry around Cu(II). Well-resolved Cu(II) hyperfine features in the EPR spectra reveal the absence of exchange interactions between adjacent copper centers. Optical and EPR spectra of a methanolic solution of the complex indicate solvent interactions. Thermogravimetric analysis shows the complex to be stable up to 175°C.     

The crystal and molecular structure of bis(melamine)silver(I) perchlorate, Ag(C3H6N6)2ClO4

The crystal structure of the title compound, Ag(mela)₂ClO₄ (mela = melamine), has been investigated by X-ray diffraction techniques, the crystals are triclinic, space group P1¯, with a = 5.236(2), b = 7.5385(9) c = 19.063(3) Å, = 99.91(1), = 90.53(2), = 108.32(2)° and Z = 2. The Ag atom has a coordination geometry with two strong bonds (2.162(2) and 2.179(4) Å) to the nitrogen of the melamines and two weak bonds (2.776(4) and 2.785(4) Å) to oxygen atoms of the ClO^– ₄anions. The N—Ag—N vector is markedly nonlinear (angle at Ag 167.7(2)°).     

Synthesis and crystal structure of cobalt(III) complex with a Schiff base and azide

The cobalt(III) complex, [Co(L)₂(N₃)₂]₂(ClO₄)₂, L being a Schiff base N-[phenyl(pyridin-2-yl)methylene]aniline has been synthesized and the crystal structure determined using X-ray crystallography. The complex crystallizes in triclinic system, space group P-1 with unit cell parameters a=10.9367(9) ?, b=18.0817(17) ?, c=20.1629(16) ?, α=111.341(2)°, β=91.622(2)°, γ=107.5030(10)°, V=3499.1(5) ?³ and Z=2. It crystallizes with two independent molecules in the asymmetric unit. The two cobalt atoms are hexa-coordinate and have a distorted octahedral geometry, satisfied by four nitrogen atoms from two molecules of the Schiff base and two nitrogen atoms from the monodentate azide group. The perchlorate ions are non-coordinating.     

Synthesis and X-ray crystal structure investigation of a potential boronate affinity chromatography ligando-boronobenzalmethoxyamine

A potential boronate affinity chromatography ligando-boronobenzalmethoxyamine (IV) and its precursor [o-formylbenzeneboronic acid (III)] were synthesized and characterized by three-dimensional single-crystal X-ray diffractometry. Both compounds contained no bonding between the boron atoms and the oxygen atoms [O(3)] of the distinguishing functional group. In addition,¹¹B NMR data confirmed the lack of any coordination between the boron and oxygen atoms in the boronic acid compoundsIII andIV and the catachol ester derivative (V) ofIV.o-Formylbenzeneboronic acid (III) crystallizes in space groupP2₁/n witha=3.883(1),b= 13.225(1),c=14.029(2) Å, =92.16(1)^o, and four molecules per unit cell.o-Boronobenzalmethoxyamine (IV) crystallizes in space group Pcen witha=14.158(2),b=17.156(1),c=7.734(2)Å, and eight molecules per unit cell. Selected bond distances and angles are tabularized.     

Synthesis, characterization, and structural analysis of ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate

Ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate was prepared by reacting the lithium salt of ethyl cyanoacetate with (Z)-O-methyl-4-chloroben-zohydroximoyl fluoride. This compound crystallizes in space group Pbca,with lattice constants a=7.5740(15) ?, b=11.337(2) ?, and c=30.424(5) ? at 110 K. Characterizations include spectrometric identifications employing IR, UV, and ¹H and ¹³C NMR. The compound exists in the solid as the enamine tautomer, with the cyano group cis to the 4-chlorophenyl group (the Z configuration). The C=C and C–N bond distances are 1.3930(16) ? and 1.3278(16) ?, respectively. The N–H group forms a bifurcated hydrogen bond with acceptors C=O (intramolecular) and C≡N (intermolecular).Supplementary material CCDC-289444 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, by e-mailing data_request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; Fax: +44(0)1223-336033.     

The X-ray crystal structures of three bis(cyclopentadienyl)titanium(IV) derivatives

The X-ray crystal structures of (aqua)bis(cyclopentadienyl)chlorotitanium(IV) trifluoromethanesulfonate, bis(aqua)bis(cyclopentadienyl)titanium(IV) bis(trifluoromethanesul-fonate) and bis(cyclopentadienyl)bis(trifluoromethanesulfonato)titanium(IV) show a pseudo-tetrahedral array of Cp ring centroids and oxygen or oxygen and chloride donors around titanium, and varied long-range packing motifs dependent on the availability of hydrogen bond acceptors within the lattice.     

Crystal structures of mollugin and lucidin

Mollugin was isolated from the extract of Rubia tinctorum roots. Lucidin was obtained by semisynthesis from xanthopurpurin. Mollugin crystallises in space group P-1 (No. 2), a = 8.5857(7), b = 11.473(4), c = 15.024(1) Å, α = 77.64(2)^∘, β = 89.36(1)^∘, γ = 89.71(2)^∘, and V = 1445.5(5) ų, lucidin crystallises in space group P2₁/c (No.14), a = 16.800(6), b = 9.637(2), c = 7.073(7) Å, β = 98.01(5)^∘, and V = 1134(1) ų.