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.     

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 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,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)     

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)     

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 and molecular structure of the chiral compound 4–(2–methylbutyloxy)phenyl–4–(2-propenyloxy)-benzoate,C21H24O4

The enantiomeric [(S)-(–)-MBP3B] and the racemic form [(±)-MBP3B] of the title compound with the formula C₃H₅O–C₆H₄–CO₂–C₆H₄–OC₅H₁₁ were studied by single crystal analysis at room temperature. (S)-(–)-MBP3B crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 7.835(3) Å, b = 11.093(6) Å, c = 44.820(3) Å and 8 molecules per unit cell. The structure was determined from 966 reflections with intensities > 3σ. The refinement with isotropic temperature factors leads to R = 0.094. The crystals of the racemic form are monoclinic, space group P2₁/a with a = 7.899(5) Å, b = 11.046(6) Å, c = 22.845(12) Å, β = 99.28(3)°, Z = 4.1236 diffractometer data (I > 3σ) were refined by least-squares methods with anisotropic temperature factors for the non-H atoms to R = 0.070. The packing arrangement for both forms shows a layer-like structure with very similar packing coefficients, k = 0.7085 for the pure enantiomer and k = 0.7014 for the racemic form.     

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 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 4-(2-hydroxyethyl)-4-aza-5α-androstan-17β-ol “HS-478”

The crystal structure of HS-478 (aqueous solvate) has been determined by direct method and refined by block diagonal least squares to R₀ = 0.043. The intensity was measured in a four-circle diffractometer in the ω/2θ scanning mode, CuKα radiation. The crystals are triclinic P1, a = 6.721(3), b = 66.532(3), c = 12.188(5) Å, α = 96.86(2)°, β = 82.82(2)°, and γ = 114.68(2)°. Rings A, B, C are chair whereas ring D is envelope. Rings A/B and B/C are trans fused, whereas rings C/D are quasi trans. The hydroxyethyl side chain connected to N(4) has conformation of (−t, t).     

The Crystal and Molecular Structure of 2-(2′-Cyano-2′-amido-ethylenyl)-pyridine

The title compound (C₉H₇N₃O) has been determined from three dimensional X-ray diffraction data. The crystals are monoclinic, a = 4.858(3) Å, b = 15.008(7) Å, c = 11.787(2) Å, ß = 94.107(2)°, V= 857.2(4) ų, z = 4, D_calc = 1.342 g. cm⁻³, space group P2_1/c. The structure was solved by direct methods and refined by full-matrix least-squares method (γ MoK_α′, R = 0.0766).     

The Crystal Structure of 3-Methoxy-estra-1,3,5(10)-triene-16α Br,17β OH

The steroid 3-Methoxy-estra-1,3,5(10)-triene-16αBr,17βOH crystallizes in the tetragonal space group P 4₁ with the lattice constants a = b = 10,358(2) Å, c = 32,591(5) Å. The crystal structure contains two symmetry independent molecules. Significant differences for the two molecules occur in all the four rings of the steroid sceleton. The molecules are linked by hydrogen bridges and Br…︁ Br contacts. The differences between the two symmetry independent molecules are interpreted as due to different intermolecular interaction.     

Crystal structure of R(–)–1–Tosyl–2–methylpyrrolidine

The crystal structure of R(–)-1-tosyl-2-methylpyrrolidine has been determined by X-ray structure analysis. The compound crystallizes in the monoclinic space group P2₁ with cell parameters a = 7.858(1), b = 14.929(6), c = 11.128(1) Å, β = 105.42(1)°. The structure has been solved by direct methods and refined to R = 0.046. There are two crystallographically independent molecules A and B in the asymmetric unit. The pyrrolidine ring of molecule A is disordered with atom C4 occupying two possible sites. The S atom has a distorted tetrahedral coordination in both the molecules. Two bifurcated hydrogen bonds are observed. Molecules are held together by hydrogen bonds.     

Structure and conformation of a nickel complex: {2‐Hydroxo‐3‐piperidine‐1‐yl‐methyl‐N,N′(bis‐5‐bromobenzylpropylenediimine)nickel(II)perchlorate}

The title compound, a nickel complex [C₂₃H₂₆N₃O₂Br₂Ni.(ClO₄)] (CCDC 199520) crystallizes in triclinic space group P with the cell parameters a = 10.2560(4), b = 10.8231(4), c = 12.0888(5)Å, α = 99.404(1), β = 99.780(1), γ = 92.252(1)° and V = 1301.49(9)ų. The structure was solved by Patterson method and refined by full‐matrix least‐squares procedures to a final R = 0.0497 using 6287 observed reflections. In the complex, the piperidine ring takes chair conformation and the geometry around the Ni ion is slightly distorted square planar. The dihedral angle between the planes [N‐Ni‐N and O‐Ni‐O] is 9.4(1)°. The chelate ring containing both the nitrogen atoms adopts twisted boat conformation. The molecules in the crystal are stabilized by N‐H…O and C‐H…O types of hydrogen bonds in addition to a C‐H…π interaction. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a novel 3‐D copper(II) polymer with bent N‐containing ligand

An exploration of the mixed‐ligand system under hydrothermal condition, has led to the isolation of a 3‐D novel framework {[Cu₂(mp)L₂)(H₂O)₂]·6H₂O}_n ( 1 ) (mp = benzene‐1,2,4,5‐ tetracarboxylate tetraanion, L = 4‐(5‐(pyridin‐4‐yl)‐1,3,4‐thiadiazol‐2yl)pyridine). Single‐crystal X‐ray analyses reveal that it crystallizes in the triclinic space group P‐1, a = 8.807(4) Å, b =11.139(6) Å, c = 11.291(5) Å, α=75.337(7), β = 73.584(5), γ= 66.795(5)°. The Cu^II ions are linked into an extended 2‐D grid net via mp molecules. Further these layers are united together through the bridging L to form a 3‐D structure, which exhibits a new 4‐connected topological network. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of N‐[(1Z)‐1‐(3‐methyl‐3‐phenylcyclobutyl)‐2‐thiomorpholin‐4‐ylethylidene] thiourea

The crystal structure of N‐[(1Z)‐1‐(3‐methyl‐3‐phenylcyclobutyl)‐2‐thiomorpholin‐4‐ylethylidene] thiourea (C₁₈H₂₆N₄S₂) has been determined by X‐ray crystallographic techniques. The compound crystallizes in the orthorhombic space group Pbca, with unit cell parameters: a = 15.692(3), b = 20.803(8), c = 11.979(6)Å, Z = 8, V = 3911(7)ų. The crystal structure was solved by direct methods and refined by full‐matrix least squares to a final R‐value of 0.084 for 1447 observed reflections [I > 2σ ( I ) ]. In the thiosemicarbazide moiety, the S = C bond length is 1.656(6), N‐C‐N angle is 115.6(5)°. The crystal structure is stabilized by the intermolecular N‐H...S hydrogen bonds. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of marmesin,C14H14O4, 2-(β-hydroxyisopropyl)-2,3-dihydro-6,7-furano-coumarin

The unit cell parameters of this compound were determined by least-squares calculations from the adjusted angular setting of 25 general reflections. The crystals are monoclinic with the following crystallographic data: a = 5.718(1), b = 13.794(4), c = 7.861(1) Å, β = 100.53(2)°, Z = 2 and D_x = 1.34 g · cm⁻³. The space group according to the systematic absences is P2₁. The structure of this compound was solved by direct methods and refined by full matrix least-squares with anisotropic temperature factors to R = 0.04. The refined atomic positions indicate a considerable strain within the molecule. The structure is built up from molecules connected by H-atoms forming infinite chains along b-axis.     

Synthesis and crystal structure investigation of pyridine‐2‐(3′‐mercaptopropanoic acid)‐N ‐oxide

Pyridine‐2‐(3′‐mercaptopropanoic acid)‐N ‐oxide (I), is a higher homologue of 1‐oxopyridinium‐2‐thioacetic acid (II) [1]. It crystallizes in monoclinic space group P2₁ with a = 9.2168(2) Å, b = 4.1423(2) Å, c = 11.3904(4) Å, β = 98.65(2)°, V = 429.93(3) ų and Z = 2. The least‐squares refinement gave residual index R = 0.024 for 1070 observed reflections. The introduction of an additional methylene group in (II) causes a flip in the carboxylic acid group of (I) that facilitates the molecules to align infinite antiparallel chains through strong C–H···O interactions. The molecules are interlinked by O–H···O hydrogen bonding across the chains and forming an infinite screw chain along y‐direction. The molecular packing is stabilized by O–H···O and C–H···O hydrogen bonding and π‐π electron interactions. This is an important facet of the crystal packing. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallographic investigation of single crystals of the mesogen compound 4′-nitrophenyl-4-n-octyloxybenzoate

X-ray investigations of single crystals of 4′-nitrophenyl-4-n-octyloxybenzoate (NPOB) have been performed for the determination of the space group P2₁/c and the lattice constants (a₀ = 16.77 ± 0.02 Å, b₀ = 9.207 ± 0.005 Å, c₀ = 16.72 ± 0.01 Å, β = 128.0 ± 0.5°). Furthermore powder patterns after Debye-Scherrer method have been taken to estimate the d-values together with the indexing. On the basis of small Miller indices the crystal angles yielded a discrepancy between axis ratios determined from optical measurements and X-ray methods. It can be shown that these differences appear with many molecular crystals.     

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.