Crystal Structure of 6,6′-dimethoxy-2,2′-diphenyl-19-crown-5 Hg(SCN)2

The crystal structure of 6,6′-dimethoxy-2,2′-diphenyl-19-crown-5 Hg(SCN)₂ has been determined from three-dimensional X-ray diffraction data. The compound crystallizes in the triclinic space group P1 (no 2) with unit cell parameters α = 9.712(6) Å, β = 11.137(7) Å, c = 14.768(12) Å, α = 86.04(5), β = 80.36(4), γ = 65.70(4), Z = 2, V= 1435(2) ų. The structure was determined by direct methods which on refinement yielded a final value of R(F) index as 0.068.     

Synthesis,crystal structure and photophysical studies on a ruthenium(II) carbonyl hydrido compound based on 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid (H2bpdc)

A novel complex, namely [Ru^II(PPh₃)(CO)(H)(Hbpdc)]·2MeOH ( 1 ) (H₂bpdc = 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid), has been synthesized from the reaction of H₂bpdc with [Ru^II(PPh₃)₃(CO)(H)₂] in methanol under mild condition and characterized by elemental analysis, IR spectrum, ESI mass spectrometry, and single crystal X‐ray diffraction. The structure shows that the complex crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 11.8984(13) Å, b = 16.5180(18) Å, c = 25.5322(19) Å, β = 115.302(4)°, V = 4536.6(8) ų, Z = 4. This compound features a 1‐D supramolecular chain constructed via hydrogen bonds. Its photophysical properties have been investigated in MeOH solution and in the solid state at room temperature.     

Crystal structure of 2‐(2'‐hydroxyphenyl)‐6‐tributylstannyl‐4‐(3H )‐quinazolinone and 2‐(2'‐hydroxyphenyl)‐6‐iodo‐4‐(3H)‐quinazolinone

The structures of the title compounds C₂₆H₃₇N₂O₂Sn ( I ) and C₁₄H₉IN₂O₂ ( II ) were determined by single‐crystal X‐ray diffraction technique. Compound I crystallizes in the triclinic space group P1 with a = 9.560(3) Å, b = 16.899(6) Å, c = 17.872(5) Å, α = 65.957(7)°, β = 83.603(5)°, γ ( = 75.242(5)°, V = 2549.8(13) ų, Z = 4, and D =1.374 g/cm³. The compound consists of a quinazolinone ring with phenol and tributylstannyl moieties. Compound II crystallizes in the monoclinic space group P2₁/c with a = 7.6454(12) Å, b = 5.9270(9) Å, c = 27.975(4) Å; α = 90°, β = 95.081(3)°, γ = 90°, V = 1262.7(3) ų, Z = 4, and D = 1.915 g/cm³. The compound consists of a quinazolinone ring with phenol and iodine substituents. For both I and II , the short intramolecular O–H…N and two long intermolecular N–H…O hydrogen bonds are highly effective in holding the molecular system in a stable state. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

2′-Methyl-3′-nitroflavone

The crystal and molecular structure of the title compound has been determined by direct methods and refined to a final R of 0.044. The compound crystallizes in space group P2₁/n with cell dimensions a = 16.681(2), b = 3.838(1), c = 20.550(4) Å, and β = 104.21(2)°. The phenyl and benzene rings of the title molecule are quite planar. The γ-pyrone ring exhibits maximum deviation 0.032(4) Å from planarity and makes a dihedral angle of 139.8(2)° with the 2-phenyl substituent.     

Crystal and molecular structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione

The crystal structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione (C₂₂H₂₀N₂OS) has been determined from three dimensional single crystal X‐ray diffraction data. The title compound crystallizes in the monoclinic space group P 2₁/c, with a = 10.6674(13), b = 10.1077(7), c = 17.9467(19) Å, β = 98.460(9)°, V = 1914.0(3) ų, D_calc = 1.251 g cm^–3, Z = 4. In the title compound, the allyl group shows positional disorder. Molecules are linked by C‐H···O, C‐H···N and C‐H···S intermolecular interactions forming two‐dimensional network. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 2,6‐bis(4‐chlorophenyl)‐3‐phenylpiperidin‐4‐one

The crystal structure of the title compound is described. The chemical formula of the compound is C₂₃H₁₉Cl₂NO. The compound is found to crystallize in monoclinic system with space group P2₁/c, Z = 4. The unit cell dimensions are a = 15.137(3) Å, b = 8.9171(18) Å, c = 14.779(3) Å, β = 91.461(4)° and V = 1994.2(7) ų, D_calc = 1.320 gcm^‐3. The final R factor is 4.4%. The central piperidone ring of the molecule adopts a slightly distorted chair conformation, the mean torsion angle being 52.3°; the phenyl rings are planar. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal and Molecular Structure of 4-Hydroxy-4′-nitro- biphenyl and its Potassium Salt

The crystal and molecular structures of the title compounds have been solved by single crystal X-ray analysis. 4-Hydroxy-4′-nitro-biphenyl (NBO) crystallizes in the centrosymmetric, monoclinic space group P2₁/n with a = 6.036(4) Å, b = 12.392(3) Å, c = 13.346(8) Å, β = 96.46(3)° and 4 molecules in the unit cell. Its potassium salt (NBOK) similarly belongs to P2₁/a with a = 11.277(2) Å, b = 7.3606(6) Å, c = 14.383(3) Å, β = 107.804(7)° and also 4 molecules in the unit cell. The structure of NBO was refined by full matrix least-squares calculation to R = 0.043 for 1105 observed reflections, the structure of NBOK to R = 0.041 for 2288 observed reflections, respectively. NBO and NBOK crystallize in layer-like structures. The biphenyl molecules of NBO are arranged as corrugated ribbons in layers. The ionic and polar moiety of NBOK (potassium, oxygen, and crystal water) are separated by biphenyl units to form layers. The almost planar biphenyl units of NBOK are arranged in pairs and exhibit a short molecular distance of 3.08 Å within one pair.     

Crystal structure of N‐(2‐methoxyphenyl)‐3,6‐diphenyl‐1,4‐dihydro‐1,2,4,5‐tetrazine‐1‐carbonamide

The title compound, C₂₂H₁₉N₅O₂, was prepared and its structure was determined by X‐ray diffraction [CCDC 216074]. The compound crystallizes from ethanol in the orthorhombic system, space group P2₁2₁2₁, with unit cell parameters: a =10.048(1) Å, b = 13.935 (2) Å, c =14.607(2) Å, Z =4, and V=2045.3(5) ų. The crystal structure was solved by direct methods and refined by full‐matrix least‐squares to a final R‐value of 0.0516 with 3621 unique reflections. The central six‐membered ring of the compound has a boat conformation and is not homoaromatic, in which adjacent atoms N1 and N4 deviate from the plane of the ring by 0.4546(33) Å and 0.3786(33) Å, respectively. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a novel Ni(II) coordination polymer with dipyrido[3,2‐a:2′,3′‐c]phenazine and 4,4′‐oxy(bisbenzoate)

A novel coordination polymer, [Ni(dppz)(oba)(H₂O)]·0.5H₂O (dppz = dipyrido[3,2‐a:2′,3′‐c]phenazine and oba = 4,4′‐oxy(bisbenzoate)) has been synthesized through hydrothermal method and characterized by IR, and single‐crystal X‐ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 23.163(5), b = 18.211(4), c = 14.460(3) Å, α = γ = 90°, β = 100.45(3)°, V = 5998(2) ų, Z = 2. The structure was solved by direct methods and refined to R = 0.0866 (wR₂ = 0.1836). The compound exhibits interesting one‐dimensional chain structures, which are further stacked through π‐π interactions to form supramolecular double chains. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The crystal and molecular structure of three homologue 1,4-terephthalylidene-bis-N-(4′-alkylanilines) (TBAA-n)

The three homologue compounds with the general formula (TBAA-n) crystallize in the following space groups: TBAA-0 : monoclinic, P 2₁ c. a = 7.656(3), b = 6.073(1), c = 16.403(7) Å, β = 91.60(2)°; TBAA-1 : monoclinic, P 2₁ c. a = 7.656(3), b = 6.073(1), c = 16.403(7) Å, β = 91.60(2)°; TBAA-1 : monoklin, P 2₁/n, a = 6.0426(11), b = 7.84171(4), c = 18.2147(31) Å, β = 92.32(1)°; TBAA-2 : orthorhombic, P ben, a = 20.9390(8), b = 14.8876(7), c = 6.2069(1) Å. The structures have been solved by direct methods and refined to R = 0.029, 0.044, and 0.049, respectively. Despite the different conformation of the terminal phenyl rings relative to the central core of the coplanar azomethine groups and the phenyl ring, the molecular packing of the three compounds obeys the same principles in forming the crystal structure.     

Crystal structure of N‐(3,4‐dichlorophenyl)‐N′‐hydroxy‐2‐oxo‐2‐phenylacetamidine

The title compound (C₁₄H₁₀N₂O₂Cl₂) crystallizes in the monoclinic space group P2₁/a with a=10.042(1) Å, b=10.317(1) Å, c=13.877(2) Å, β=97.36(2)°, V=1425.8(3) ų, Z=4, D_x=1.44 g.cm^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R = 0.0457). The title molecule consists of 3,4‐dichlorophenylamino and 2‐phenyl‐1,2‐ethanedione‐1‐oxime groups. The intermolecular O‐H…N and N‐H…O hydrogen bonds [O…N 2.760(6) and 3.087(5) Å] are highly effective in forming the polymeric chains. The oxime group has an E configuration. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of an ammonium thiocyanate complex of 18–crown–6

The title compound (C₁₃H₃₀N₂O₇S) has been determined from three‐dimensional X‐ray diffraction data. The crystals are monoclinic, a = 22.654(8) Å, b = 8.652(4) Å, c = 23.925(9) Å, β = 123.880(9)°, V = 3893(3) ų, Z = 8, D_calc = 1.192 g/cm³, space group C2/c. The structure was solved by direct methods and refined by full‐matrix least squares method (R = 0.051). The ammonium cation is displaced by 1.08 Å from the mean plane of the ligand causing hydrogen bonding with the macrocyclic O atoms in a perching arrangement. The thiocyanate anion forms an extended hydrogen bonded chain with the cation via the occluded water molecule. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Solvothermal syntheses and crystal structures of two 4‐heterocyclic acylpyrazolone complexes

Many explorations of transition metal (M)‐L system under solvothermal condition, have led to the syntheses of two new 4‐heterocyclic acylpyrazolone complexes [Co(L)₂(CH₃OH)₂] (HL = 1‐phenyl‐3‐methyl‐4‐(2‐furoyl)‐5‐pyrazolone) ( 1 ) and [Cr(L)₃] ( 2 ). Single‐crystal X‐ray analyses reveal that crystal structures of compound 1 and 2 are respectively orthorhombic, Pbca, a = 15.0378(6) Å, b = 9.8405(4) Å, c = 20.7321(8) Å, V = 3067.9(2) ų, Z = 8 and triclinic, P‐1, a = 10.7966(18) Å, b = 13.023(2) Å, c = 15.520(3) Å, α = 73.011(4)°, β = 84.884(4)°, γ = 70.267(4)°, V = 1964.3(6) ų, Z = 2. Complex 1 has a two‐dimensional (2D) network structure that is formed by O–H···N H‐bonding interactions. Complex 2 makes a one‐dimensional (1D) zigzag chain structure by intermolecular π···π interactions, which is further interlinked via C–H···N H‐bonding interactions to generate a 2D sheet, and then a three‐dimensional (3D) supramolecular network structure is further linked by intermolecular C–H···π interactions. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal Structure of 3‐(4′‐Methoxyphenyl)propanoyl pyrrole of Piper lolot C.DC from Vietnam

C₁₄H₁₅NO₂ (293 K): monoclinic space group P2₁/n, a = 24.580(10), b = 5.536(2), c = 9.037(3) Å, β = 91.18(4)°, V = 1229.4(8) ų, D_x = 1.239 g · cm^‐3, Z = 4, F(000) = 488, λ(CuKα) = 1.5418 Å, μ = 0.667 mm^‐1. The title compound which was isolated from the rhizomes of Piper lolot C.DC has antibacterial activity. Its chemical identity was established by this X‐ray analysis. The molecule consists of a planar propanoyl pyrrole and a methoxyphenyl fragment with an interplanar angle of 93.8(3)° which is by 30° larger than the corresponding angle reported in the literature for the comparable dimethoxy derivative, which was also derived from Piper species.     

The Molecular and Crystal Structure of 3β-O-(2′,3′ -O-isoropylidene-α-L-rhamnopyranosyl) — digitoxigenin

3β-O-(2′,3′ -O-isoropylidene-α-L-rhamnopyranosyl) — digitoxigenin crystallizes in the monoclinic space group P 2₁ with two molecules C₃₂H₄₈O₈ per unit cell and the lattice constants a = 7.865, b = 6.470, c = 29.803 Å, β = 93.95°. The structure was solved by direct methods of phases determination and subsequently refined by least squares technique to the final R-value 0.06. The position of the lactone ring is disordered in the crystal.     

Crystal Structure of Diethyl 2‐[2,2,2‐ trifluoro‐1‐(indole‐3‐yl)‐ethyl]‐2‐acetamidomalonate

The title compound (C₁₉H₂₁F₃N₂O₅) has been determined from three dimensional X‐ray diffraction data. The crystals are monoclinic, a = 7.626(4)Å, b = 17.515(4)Å, c = 15.066(3)Å, β = 101.02(3)°, V = 1975(1)ų, Z = 4, D_calc = 1.393g cm^‐3, space group P2₁/c. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R = 0.039).     

Die Molekül- und Kristallstruktur von 1.1′-Bis-[phenyl-glyoxyloyl]-ferrocen

The 1.1′-Bis-[phenylglyoxyloyl]-ferrocen (PGF) crystallizes within the monoclinic space group P₁/c with the lattice constants a = 7,338 Å, b = 16,872 Å, c = 8,046 Å, β = 87,0°. The PGF belongs to metal-π-complexes. With the iron atom in the center of symmetry, both the heavy atom ligands are centrosymmetric-to each other. The two cyclopentadinyl rings linked to the iron atom are arranged in the sandwichtype with staggered conformation. The mean planes are separated by 3,32 Å. In a single phenyl-glyoxyloyl molecule exists an expanded Csp²–Csp² bondlength (1,528 Å). The two plane parts of the molecule are twisted around this bond. These two plane parts consist on the one hand of the carbon-5-ring and a C  O group and on the other hand of the carbon-6-ring and a C  O group. The dihedral angle is 62,5°. The expanded bond length mentioned is explained by Coulomb repelling forces of partially charged atoms. The packing of the molecules in the crystal lattice is discussed in detail.     

Crystal structure,thermal and compositional deformations of β‐CsB5O8

The crystal structure of β‐CsB₅O₈ has been determined from X‐ray powder diffraction data using synchrotron radiation: Pbca, a = 7.8131(3) Å, b = 12.0652(4) Å, c = 14.9582(4) Å, Z = 8, ρ_calc = 2.967 g/cm³, R‐p = 0.076, R‐wp = 0.094. β‐CsB₅O₈ was found to be isostructural with β‐KB₅O₈ and β‐RbB₅O₈. The crystal structure consists of a double interlocking framework built up from B‐O pentaborate groups. The crystal structure exhibits a highly anisotropic thermal expansion: α_a = 53, α_b = 16, α_c = 14 · 10^‐6/K; the anisotropy may be caused by partial straightening of the screw chains of the pentaborate groups. The similarity of the thermal and compositional (Cs‐Rb‐K substitution) deformations of CsB₅O₈ is revealed: increasing the radius of the metal by 0.01 Å leads to the same deformations of the crystal structure as increasing the temperature by 35°C. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structures of N1, N5‐dibenzoyltetrahydro‐4‐methyl‐1, 5‐benzodiazepin‐2‐one (DBTBO) and tetrahydro‐4‐methyl‐1, 5‐benzodiazepin‐2‐one (TBO)

Adducing structural analogies between the two fused systems, N1, N5‐Dibenzoyltetrahydro‐4‐methyl‐1,5‐benzodiazepin‐2‐one, C₂₄H₂₀N₂O₃ (DBTBO CCDC 200341) and Tetrahydro‐4‐methyl‐1,5‐benzodiazepin‐2‐one, C₁₀H₁₂ N₂O (TBO CCDC 200342) helps to find the pharmacological differences from the view point of variant hetero atom substitutions in the hetero cycle. Both the diazepines crystallized in identical monoclinic space group P2₁/n with a = 14.1134(1) Å, b = 9.2444(1) Å, c = 16.3812(1) Å; β = 107.11(1)º, V = 2042.7(3) ų for DBTBO and a = 9.3363(7) Å, b = 10.4895(8) Å, c = 9.9852(7) Å, β = 91.314(1)º, V = 977.62(1) ų for TBO, respectively. The two structures were solved by direct methods and refined by full‐matrix least‐squares procedure to final R‐values of R1 = 0.0575(DBTBO) and R1 = 0.0984(TBO). Structural differences include non‐identical boat conformations of these seven‐membered rings and the different non‐bonding interactions in the benzodiazepine pair.     

Crystal structure and optical properties of 4‐nitrophenyl 4‐butoxybenzoate

The title compound, C₁₇H₁₇N₁O₅, has been synthesized and characterized by single crystal X‐ray analysis and UV‐Vis spectra. The crystals are monoclinic, P 2₁/c, a = 17.994 (5) Å, b = 4.0592 (9) Å, c = 21.625 (5) Å, β = 99.634 (5)°, V = 1557.2 (6) ų and Z = 4. The molecule has an almost stretched form with a molecular length of 17.505 Å and an imbricated structure known for liquid crystals. The structure contains no direction‐specific intermolecular interactions like aromatic π‐π stacking and C‐H… π(arene) other than two weak C‐H…O hydrogen bonds. Good optical transmittance in the entire visible region of the UV‐Vis spectrum suggests that it is a potential candidate for optoelectronic applications. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)