Molecular and crystal structure of 4′-cyanobenzo-15-crown-5

The crystal structure of 4′-cyanobenzo-15-crown-5 is determined by X-ray diffraction. The crystallographic parameters of single crystals are as follows: a = 40.479(6) Å, b = 8.821(2) Å, c = 8.484(2) Å, β = 93.94(2)°, V = 3022.2 ų, Z = 8, d _calcd = 1.27 g/cm³, and space group C2/c. The structure is solved by the direct method and refined by the least-squares procedure to R = 0.068. The conformation of the macrocycle in 4′-cyano-B15C5 is described by the a-a-g ^? -a-a-g-g ^? -a-a-g-a-g-a-a-s sequence of torsion angles.     

The crystal and molecular structure of spiro[1-(S)-Br-3-(S)-H-4-(R)-l-(1′ R,2′ S,5′R)-menthyloxy-5-oxo-6-oxa-bicyclo[3.1.0]hexane-2,3′-(R)-(4′-(R)-diphenylmethoxy-5′-l-(1′ R,2′ S,5′ R)-menthyloxy-butyrolactone)]

Crystal structure of C₄₁H₅₃O₇Br has been determined by single-crystal X-ray diffraction. The compound crystalline in the orthorhombic space group P2₁2₁2₁, with a = 11.264(2), b = 12.058(2), c = 29.337(6) Å, Z = 4. The bond angles of cyclopropane moiety in the molecule are approximate to 60° and agree with theoretic values of the internal angles in a cyclopropane, and two chiral menthyloxy groups are located above and under the whole chiral molecule, respectively. The configuration of the pentacyclic lactone is shown as envelope form.     

Synthesis and crystal structure of (S, S, S, S)-N, N′-bis[N-(P-toluenesulfonamido)-1,2-diphenylethyl]ethylenediamine

(S, S, S, S)-N,N′-bis[N-(p-toluenesulfonamido)-1,2-diphenylethyl] ethylenediamine (C₄₄H₄₆N₄O₄S₂), has been synthesized and structurally characterized by elemental analysis, ¹H-NMR, MS, IR and single-crystal X-ray diffraction. The title compound contains four chiral centers with C atoms in S configuration. Molecules are connected to one another by hydrogen bonds between sulfonamide nitrogen and sulfonyl oxygen to form chains alone a axis.     

The crystal structure of 2-amino-5,5′-bis(β-cyanoethyl)-1,2-pyrrolenineN-oxide monohydrate

2-Amino-5,5-di(-cyanoethyl)-1,2-pyrrolenineN-oxide monohydrate, C₁₀H₁₄N₄O·H₂O, crystallizes from MeCN in space group P2₁2₁2₁ witha=7.0007(5),b=8.2998(6),c=20.8418(13) Å,V=1211.0(2) ų,Z=4. The structure was refined toR=0.034 andR _w=0.044 for 2325 observed reflections. The pyrrolenine ring adopts a nearly planar conformation, with maximum deviation from planarity 0.089(2) Å. The N–O distance is 1.345(2) Å. The water molecule bridges two pyrrolenine molecules via hydrogen bonds to theirN-oxide oxygen atoms, and also accepts a hydrogen bond from the NH₂ group of another pyrrolenine molecule.     

Synthesis and crystal structure of (1R,2R)-N,N′-bis(4-toluenesulfonyl)-1, 2-di(4-methoxylphenyl)ethylenediamine

The reaction of (1R,2R)-1,2-di(4-methoxylphenyl)ethylenediamine with p-toluene sulfonyl chloride affords the title compound C₃₀H₃₂N₂O₆S₂, the structure of which is ascertained by X-ray diffraction. The title compound contains two chiral centre with each C atom in R configuration. Two adjacent molecules are linked by intermolecular hydrogen bonds through sulfonamide nitrogen and sulfonyl oxygen to form a one-dimensional chain alone a axis.     

Synthesis and crystal structure of (+)-(2R,3R)-N, N′-bis-trityl-2,3-bis-aziridine

A new C₂ symmetric bis-aziridine derivative was synthesized starting from L-(+)-tartaric acid. The molecular structure of (+)-(2R, 3R)-N, N-bis-trityl-2,3-bis-aziridine 4, was determined by ¹H, ¹³C NMR and elemental analysis and was confirmed by single-crystal X-ray diffraction. Crystal data for 4: C₄₂H₃₆N₂, orthorhombic, space group: P2₁2₁2₁, a = 12.7633(14), b = 14.5661(6), c = 17.4184(14) Å, and Z = 4.     

The synthesis and crystal structure of one novel ternary complex of 2,2′-bipyridine N-salicylidenetyrosinatocopper(II)

The crystal structure of copper(II)—salicylidene-aminoacidate Schiff base—nitrogen-donor chelating ligand, [Cu(sal-tyr)(bipy)] (sal-tyr: N-salicylidenetyrosinato; bipy: 2,2-bipyridine) which is obtained by means of one-step synthesis, is presented. It crystallizes in space group P2₁2₁2₁ with a = 9.0356(18) Å, b = 11.992(2) Å, c = 20.618(4) Å. The Cu^II ion is five coordinated by one oxygen atom of carboxylate, the imine nitrogen atom, and the hydroxyl oxygen atom of the salicylidene in the Schiff base anion as well as two nitrogen atoms of bipy, resulting in a seriously distorted square pyramid coordination polyhedron. The phenol group and the apical coordination bond Cu(1)–N(2) are in the same side of the Schiff base chelating plane which could be attributed to the intramolecular C–H s interaction between the H(17) of the bipy and the benzene ring of the phenol. The hydrogen bond between the hydroxyl hydrogen atom of the phenol group and the coordinated oxygen atom of the carboxylate from neighboring molecule is helpful to stabilize the crystal.     

Molecular and crystal structure of [NO2Py]2[Ni(mnt)2](NO2Py=1-(4-nitrobenzyl)pyridinium, mnt2−=maleonitriledithiolate)

The structure of [NO₂Py]₂[Ni(mnt)₂], as determined by x-ray single crystal analysis, consists of two 1-(4-nitrobenzyl)pyridinium cations and one [Ni(mnt)₂]^2– anion. The crystallographic data for the complex:monoclinic P2₁/n, a = 9.913(2) Å, b = 11.968(2) Å, c = 14.566(3) Å, = 100.36(3)°, V = 1699.9(6) ų, Z = 2. The [Ni(mnt)₂]^2– anion has a crystallographically imposed center of symmetry and exhibits a relatively planar structure. The cation, [NO₂Py]⁺, adopts a conformation where both the aromatic rings are twisted to the C11-C10-N3 reference plane. The anions (A) and the cations (C) consist of alternating layers (i.e., of type ···C₁A₁C₂A₂C₁A₁C₂···) along the c axis of the crystallographic unit cell.     

Synthesis and crystal structure of 1-(1′,3′-dimethyl-5′-chloropyrazol-4′-carbonyl′-3-(2′-chlorophenyl)-5-amino-4-cyanopyrazole

The title compound 1-(1,3-dimethyl-5-chloropyrazol-4-carbonyl)-3-(2-chlorophenyl)-5-amino-4-cyanopyrazole (C₁₆H₁₂Cl₂N₆O) has been synthesized and characterized by X-ray diffraction: Triclinic, space group P1, with a = 8.6712(8) Å, b = 9.5091(10) Å, c = 11.2170(11) Å = 71.531(2)°, = 84.683(2)°, = 74.099(2)° Z = 2; V = 843.7(14) ų. C(10), O(1), C(11), and N(2) atoms are coplanar with the average deviation of 0.0071 Å, which form 11.03° and 43.93° dihedral angles with pyrazole planes (I) and (II), respectively.     

Synthesis and crystal structure of Nd(III)–Zn(II) complex

A novel heteronuclear complex, [NdZn₂L₆(NO ₃)(phen)₂] (HL = -methylacrylic acid, phen = 1,10-phenanthroline), was synthesized and characterized by elemental analysis, infrared absorption spectra (IR) and its molecular structure was also determined by X-ray structure analysis. The title complex contains a discrete trinuclear ZnNdZn molecule bridged by carboxylate groups between Zn and Nd ions and crystallizes in space group P¯1 with the cell dimensions: a = 13.601(3) Å, b = 16.859(2) Å, c = 12.575(2) Å, = 110.09(1), = 112.21(1), = 81.10(2).     

Molecular structure and absolute configuration of (+)-(1R, 2S, 6R, 7S, 1′R)-5-(1′-phenylethylamino)-endo-tricyclo[5.2.1.02,6]deca-4,8-dien-3-one

The crystal and molecular structure of (+)-(1R, 2S, 6R, 7S, 1R)-5-(1-phenylethylamino)-endo-tricyclo[5.2.1.0^2,6]deca-4,8-dien-3-one is described. Based on the known absolute configuration (R) of the -phenylethylamine moiety the X-ray analysis revealed the absolute configuration of the title compound. The structure was refined to R ₁ = 0.0298 for 1950 reflections (with I > 2(I)). Crystal data: C₁₈H₁₉NO, monoclinic, space group P2₁, a = 6.7406(4), b = 9.959(2), c = 11.3123(8)Å, = 102.969(5), V = 740.0(2)ų, and Z = 2.     

Synthesis, crystal structure, and spectroscopy of (azido-N1)bis(2,2′-bi-imidazoline)copper(II) perchlorate

The compound [Cu(biz)₂(N₃)](ClO₄) (biz = 2,2-bi-imidazoline) has been synthesized and characterized by X-ray crystallography and infrared spectroscopy. In addition, EPR and magnetic measurements have been performed. The compound crystallizes in the monoclinic space group P2₁/c, with a = 9.2716(2), b = 27.6454(4), c = 7.4285(1) Å, = 102.1417(6)°, V = 1861.46(5) ų, and Z = 4. The coordination geometry around the Cu(II) ion is distorted square pyrimidal, with 4 nitrogen atoms of 2 bis-chelating ligand molecules in the basal plane and one nitrogen of the azide molecule in the apical position. The perchlorate ion is noncoordinating. In the infrared the vibrations of the coordinated azide anion are observed at 2050, 1286, and 620 cm^–1, while the vibrations of the free perchlorate anion are observed at 1071, 1035, and 919 cm^–1; Cu—N vibrations are observed at 418 and 336 cm^–1. The molecules are connected in the lattice via relatively strong hydrogen bonding between the N—H groups at the back of the biz ligand and the N1 and N3 atoms of the azide ligand forming layers. No intermolecular magnetic interaction was observed for this compound.     

Synthesis and crystal structure of 1,1′-di(ethylpropionato)-2,2′-biimidazole, a macromolecular precursor

1,1,-Di(ethylpropionato)-2,2-biimidazole, C₁₆H₂₂N₄O₄, crystallizes from ice-cold ethanol in the space group P , with a = 4.6742(9), b = 9.1119(13), c = 10.175(2) Å, = 96.22(1), = 96.29(2), = 97.53(1)°, and Z = 1. The molecule crystallizes with coplanar rings and the substituents assume a trans conformation with a center of inversion between the bridging carbon atoms.     

Synthesis and crystal structure of N-(1-phenyl-3-methyl-4-benzal-pyrazolone-5)- N′-salicylidene hydrazine

A novel Schiff base compound, N-(1-phenyl-3-methyl-4-benzal-pyrazolone-5)-salicylidene hydrazine (PMBP-SAH), has been synthesized and characterized by X-ray diffraction: monoclinic, space group C2/c with a = 21.796(5) Å, b = 18.370(3) Å, c = 20.843(3) Å, = 95.440(10)°, V = 8308(3) ų, and Z = 16. The title compound contains two kinds of tautomers: the red compound is the keto form and the other is the enol form. Changes in color are due to the isomerization of the enol and keto forms by the intramolecular proton transfer.     

5(2′Carboxy)phenylazo barbiturate diaqua copper(II) trihydrate: Characterization and crystal structure

The title compound has been synthesized and characterized by standard spectroscopic techniques and magnetic susceptibility measurements and its structure has been determined by monocrystal X-ray diffraction. The complex crystallizes in the monoclinic space groupP2₁/c in a cell of dimensionsa=11.432(3),b=6.927(2),c=21.289(8)Å,=106.54(4)°,V=1616.1(9)ų,D _c =1.758 Mg m^–3,D(flotation)=1.76 Mg m^–3,M _w =427.8, (CuK)=2.47 mm^–1,F(000)=876. The structure refined to a finalR of 0.041 for 1290 observed independent reflections. The copper atom is coordinated by the nitrogen atom of the azo group next to the phenyl ring, the oxygen atom of one of the carbonyl groups of the barbituric moiety and one of the oxygen atoms of the carboxylate, closing two six-member chelate rings. Two water molecules complete a typical 4+1 square-based pyramidal environment.     

Synthesis and crystal structure of bis(2,2′-bipyridyl)mononitritozinc(II) perchlorate. An example of a six-coordinate cis-octahedral ZnN4O2 chromophore

The crystal structure of bis(2,2-bipyridyl)mononitritozinc(II) perchlorate, [Zn(bipy)₂ (ONO)][ClO₄] (1) has been determined. The complex is monoclinic, with a = 10.9195(4) Å, b = 12.2320(5) Å, c = 16.5477(8) Å, = 105.6150(10), P2₁/n space group, with final R1 = 0.0657 and wR2 = 0.1630. The complex involves a [Zn(bipy)₂ (ONO)]⁺ cation and a [ClO₄]^– anion. The ZnN₄O₂ chromophore is six-coordinate, with a cis-distortion of the two oxygens of the nitrite, O(1) and O(2), at distances 2.216(5) and 2.197(5) Å from the zinc (Zn– O _mean = 2.206(5) Å, O = 0.019(5) Å) and two out of plane Zn–N bonds, Zn–N(2) and Zn–N(3), at 2.129(4) and 2.135(4) Å (Zn–n _mean/out = 2.132(4) Å, n _2,3 = 0.006(4) Å). The two inplane nitrogens, N(1) and N(4), at distances Zn–N(1) = 2.090(4) and Zn–N(4) = 2.085(4) Å (Zn–n _mean/in = 2.087(4) Å, n _1,4 = 0.005(4) Å) are greater than 2.0 Å, but slightly shorter than the axial bonds. The inplane angles ₁, ₂, and ₃ in 1 have values 150.33(18), 108.98(17), and 99.73(18) respectively. The stereochemistry is cis-distorted octahedral, with an ₃ = 99.37(18), which is lower than ₃ = 103.4(1) observed in [Zn(bipy)₂(ONO)][NO₃] (5). Comparison with the corresponding [Cu(bipy)₂(ONO)][Y] complexes suggested that the cis-distortion of the CuN₄O₂ chromophore in the copper(II) series does not originate in the Jahn–Teller or pseudo-Jahn–Teller effect.     

Heteropolymetallic complexes of 1,1′-bis(diphenylphosphino) ferrocene (dppf). II. Crystal structure of dppf and NiCl2(dppf)

The crystal structures of dppf [dppf=1,1-bis(diphenylphoshino)ferrocene] and (dppf)NiCl₂ were determined by X-ray crystallography and refined toR=0.043 (both). The molecule of dppf is centrosymmetric, with the inversion center at the Fe atom. The ferrocene rings are parallel and staggered. In (dppf)NiCl₂ the coordination around nickel is tetrahedral, with a significantly large Cl-Ni-Cl angle (125°) due to repulsion of the chlorine atoms. The ferrocene ligand exhibits a slightly distorted (9°) eclipsed conformation, very similar to that observed in (dppf)NiBr₂.     

X-ray structure investigation of two polymorphic modifications of 1-acetyl-3-(4-nitrophenyl)-5-(2′-furyl)pyrazoline

Two polymorphic modifications of 1-acetyl-3-(4-nitrophenyl)-5-(2′-furyl)pyrazoline (I) are investigated by X-ray diffraction with the purpose of analyzing the factors responsible for the formation of crystal structures of the optical nonlinear organic compounds. Both modifications crystallize simultaneously upon slow evaporation of a solution of compound I in an isopropanol-acetonitrile (3: 1) mixture. It is found that the molecular geometry of the polymorphic modifications is characterized by the rotation of the furan substituent with respect to the plane of the pyrazoline ring. The molecular hyperpolarizabilities (β) of both conformers are calculated.     

The X-ray crystal structures of bis(l-α-alaninehydroxamato)nickel(II) and bis(l-α-alaninehydroxamato)copper(II)

The structure of twol--alaninehydroxamato (-Alaha) complexes of Ni(II) and Cu(II) have been determined by single-crystal X-ray diffraction methods. The crystals of Ni(-Alaha)₂·2H₂O (I) are monoclinic witha=12.267(4),b=4.798(2),c=10.017(4)Å,=95.48(3)°,Z=2, and space groupP2₁. The crystals of Cu(-Alaha)₂·2H₂O (II) are monoclinic witha=5.073(2),b=11.463(3),c=20.198(5) Å,Z=4 and space groupP2₁2₁2₁. The values of the final residualsR for Ni(-Alaha)₂·2H₂O and Cu(-Alaha)₂·2H₂O are 0.06 and 0.03, respectively. The molecular structures of Ni(-Alaha)₂ and Cu(-Alaha)₂ consist of a square planar and a pentanuclear piramidal, respectively, with the-alaninehydroxamato, (CH₃CH₂(NH₂)CONOH^–), ligands coordinating to metal ion via the N(amino) and the hydroxamic N^– donors.