• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-12-14
Ren-Tao Wu, Ji-Kun Li, Chuan-Ping Wei, Xian Ma

The copper coordination complex [CuCl(2-OHNA)H2O]·H2O (1) was synthesized by the reaction of CuCl2·2H2O with in situ generated 2-hydroxynicotinic acid and its crystal structure was determined by single X-ray diffraction methods. It was further characterized by FT-IR spectroscopy, elemental analyses, and thermogravimetric analysis. Complex 1 crystallizes in monoclinic space group P21/c with a = 8.9797(13), b = 14.196(2), c = 7.0738(11) Å, β = 96.897(2), V = 895.2(2) Å3, Mr = 273.12, Dc = 2.027 g/cm3, and Z = 4. In the structure, complex 1 is linked into 2D sheets via intermolecular hydrogen bonding [N1–H1···O2 (−x+1, y − 1/2, − z+1/2); O5–H10···O2 (− x+1, y + 1/2, − z+1/2); O4–H9···O5 (x, y − 1, z); O4–H8···O5 (− x+2, y + 1, − z)]. The catalytic property of 1 was also investigated in the selective oxidation of benzyl-alkanes using TBHP as oxidant. Under optimized conditions, 1 exhibited high catalytic activity and selectivity toward the corresponding aryl ketones.

更新日期：2019-12-17
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-12-13
Mickey Vinodh, Talal F. Al-Azemi

Crystal structures of two resorcinarene units, namely, a cavitand type upper periphery in which the upper rims are functionalized with hydroxyl groups (RCOH4) and a similarly substituted resorcinarene analogue with non-rigid and flexible upper portion (ROOH4)—are discussed. The functionalization is symmetrical with all of the four upper rim positions being derivatized. The molecular structure of RCOH4 obtained from single crystal diffraction is consistent with the cone conformation, whereas that of ROOH4 possesses a boat conformation at the head position. The boat conformation of ROOH4 is further confirmed by low temperature NMR analysis. The presence of four OH functional groups in the head position enable these resorcinarene units to form efficient H-bonds with neighboring resorcinarene moieties or solvent molecules. The alkyl groups at the tail portions are also involved in C–H···C or C–H···O type weak hydrophobic intermolecular interactions. Hirshfeld surface analysis mapped with dnorm plots and the related 2D fingerprint diagrams also indicate the presence of H···O and H···C intermolecular interactions within these crystals. The supramolecular interactions in RCOH4 have resulted in an ordered bilayer type of packing with separated polar and non-polar parts in its crystal. However, the packing pattern in the ROOH4 crystals is quite different from that of RCOH4 in which each row is aligned with resorcinarenes of alternating upper and lower rims.

更新日期：2019-12-13
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-12-06
Florencia Luzardo, Natalia Álvarez, Karolina Soca Rosas, Carlos Kremer, Andrea S. Stucchi de Camargo, Jorge S. Gancheff

A new crystal structure for complex [Cu2Cl2(bipy)2(μ-Cl)(μ-CH3O)] was obtained. X-ray diffraction data showed dinuclear complexes with metal-ions seated on two symmetrically related pentacoordinated environment, in which, a trigonal bipyramidal (TBPY-5) coordination polyhedra was observed. While chloride was detected as monodentate and as a bridging-ligand, the diimine unit and a bridging oxygen from methoxide occupied the remaining positions. The crystal structure accounted for dinuclear complexes interacting to each other via H-bonds involving C–H groups of bipy and monodentate chloride anions of an adjacent molecule. Theoretical studies were conducted by DFT methods employing B3LYP in combination with 6-31G(d). Larger basis sets (6-311G(d) and cc-pVDZ) were taken into account to assess the performance of B3LYP/6-31G(d) in dealing with equilibrium geometry and population analysis. This standard methodology showed to be a reasonable performer to reproduce geometric parameters keeping the computational cost very low.

更新日期：2019-12-06
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-11-23
Hai-Tao Wu, Jun-Ru Wang, Yu-Chen Zhu, Yong Wang, Wen-Yu Yin, Hong-Jian Cheng, Rong-Xin Yuan

Solvothermal reactions of Zn(NO3)2·6H2O or Cd(NO3)2·4H2O with 1,3-bis(4-imidazolylphenoxy)propane (popmz) and benzophenone-4,4-dicarboxylic acid (H2bpda) afforded two coordination polymers [Zn(bpda)(popmz)]n (1) and {[Cd(bpda)(popmz)]·0.5H2O}n (2), respectively. Both compounds were characterized by elemental analysis, IR and single crystal X-ray diffraction. Compound 1 has a 3D supramolecular structure consisting of two-fold parallel interwoven layers featuring hydrogen-bonding and π···π interactions. Compound 2 possess an extended 3D supramolecular architecture based on 2D layers through hydrogen-bonding interactions and the π···π stacking interactions. A comparative study on their photocatalytic activity toward the degradation of methyl orange in polluted water was explored.

更新日期：2019-11-26
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-11-22
Chloe J. Pugh, Craig M. Robertson, Alexander Steiner

In the solid state diallylamine forms supramolecular helices with four molecules per pitch that are held together by hydrogen bonding. The helical structure is the result of competing length scales at which hydrogen bonding and second-neighbour Van-der-Waals interactions occur. The structure features two crystallographically independent helices and four unique molecules in the asymmetric unit (Z′ = 4). The high Z′ value is partly a consequence of the centrosymmetric pseudo-hexagonal packing of helical columns, which is incompatible with helical spacegroup symmetries.

更新日期：2019-11-22
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-11-16
K. L. Jyothi, Mahesha, N. K. Lokanath

Creatinine, an aliphatic hetero monocyclic compound, plays an important role in the protein metabolism and change in its physiological normal concentration leads to diabetic nephropathy, renal failure and muscle disorder. In this work, a novel molecular salt form (ionic cocrystal) of creatinine (CR) with gallic acid (GA) has been obtained and preliminarily characterized by PXRD, FTIR and the crystal structure was confirmed by X-ray diffraction method. The presence of a single C–O stretching band in the place of two stretching bands [C=O and C–O] in the infrared spectrum confirms the formation of molecular salt. The asymmetric unit of GA–CR ionic cocrystal [(C7H5O5)− (C4H8N3O)+ 3(H2O)] comprises of a molecule of gallic acid, a molecule of creatinine and three water molecules. The structural analysis reveals the strong hydrogen bond DDAA environment of water molecules which confirms the presence of different supramolecular architectures. Thermal gravimetric analysis was carried out to investigate the presence of water/solvent molecules in the molecular salt. Further, the intermolecular interactions in stabilizing the molecular salt were analyzed using Hirshfeld surfaces. Furthermore, the coordinates of molecular salt were optimized by DFT calculations using APFD hybrid functional with 6-311 + G(d,p) level basis set. Frontier molecular orbitals, energy gap and related molecular properties were also analyzed. GA–CR pharmaceutical molecular salt form is found to be more reactive than CR and therefore offers an innovative approach for the futuristic drug design.

更新日期：2019-11-17
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-11-16
Javeed A. Ganaie, Neha Sen, Ray J. Butcher, Jerry P. Jasinski, Sushil K. Gupta

Two new phenol-based metal-free macrocyclic Schiff bases, cyclo-bis{2-[benz(N-propan-1,3-diyl)imidoyl][6-benzimidoyl][4-methyl]phenol} and cyclo-bis{2-[benz(N-butan-1,4-diyl)imidoyl][6-benzimidoyl][4-tert-butyl]phenol} have been synthesized and their structures determined by single crystal X-ray crystallography. The DFT geometry optimization calculations were performed to compare experimental and theoretical results. A comparison of the dihedral angles between mean planes of the central phenolato rings and peripheral phenyl rings in the crystal with the DFT theoretical calculations has been included for each molecule. Electronic transitions have been predicted by DFT molecular orbital calculations and compared with experimental absorption spectral data.

更新日期：2019-11-17
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-11-14
Truc-Vi H. Duong, Todd S. Carroll, Daniel S. Bejan, Edward J. Valente

In the solid state, some 3-substituted 4-hydroxycoumarins β-ketoester enols form infinite translational hydrogen-bonded β-chains with varying degrees of alignment between adjacent delocalized systems. Nine related structures have been studied. At the strongest, intermolecular associations are polar, purely translation neighbors interact essentially along a 717 pm crystallographic repeat with shortened 260 pm intermolecular O·OH-bond contacts. Four distinctive features characterize these structures: (1) moderately delocalized β-ketoester enol structures, (2) translational misalignment angles between oxygen donors and acceptors less than 10°, (3) buttressing intermolecular C–H·O contacts co-planar with and near the intermolecular O–H·O interactions, and (4) fully extended ketoester enol hydrogen-bond (ap-anti-anti) geometries. For non-polar β-chains in related coumarin systems, β-ketoester enol alignments are typically poorer, involve hydrogen-bonding between glide relatives, ap-syn-(anti) geometry, and the intermolecular O·OH-bond contacts are longer.

更新日期：2019-11-14
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-11-07
Gui-Mei Tang, Yong-Tao Wang, Yu-Song Wu

The crystal structure of 2-(3-ethoxy-4-(methoxycarbonyl)phenyl) acetic acid (RGA), an important intermediate in the preparation of Repaglinide, has been carried out. Hydrogen bonds between the carboxylate groups link the molecules into dimers while weak C–H···π interactions link these dimers into a one-dimensional chain lying along the crystallographic b axis. 4-(Carboxymethyl)-2-ethoxybenzoic acid (RGAA), an impurity observed in the preparation of Repaglinide, has been simply synthesized by the hydrolysis of RGA under basic conditions. Hydrogen bonds between the carboxylate groups link the molecules into dimers while weak C–H···O interactions connect these dimers into a one-dimensional chain lying along the crystallographic c axis. The compound RGAA has also been characterized by FT-IR and UV–Vis spectra, and by 1H NMR analysis. RGA: monoclinic, P21/n, a = 12.848(3) Å, b = 4.5539(10) Å, c = 22.328(5) Å, α = 90°, β = 101.703(5)°, γ = 90°, V = 1279.2(5) Å3. RGAA: monoclinic, P21/n, a = 14.0877(11) Å, b = 5.1814(3) Å, c = 14.5857(11) Å, α = 90°, β = 91.578(3)°, γ = 90°, V = 1064.26(13) Å3. The thermal behaviors and fluorescence properties of RGAA were also investigated.

更新日期：2019-11-07
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-01-18
Zuoran Xie, Yuan Lu, Shouwen Jin, Haomiao Ye, Zhong Wang, Bin Liu, Daqi Wang

Five crystalline organic acid-base salts [(HL)·(dnsa−), L = 2,6-dimethylaniline, dnsa− = 3,5-dinitrosalicylate] (1), [(HL+)·(4-Hnpta−), 4-Hnpta− = 4-nitrophthalate] (2), [(HL)2·(nds)·(H2O)2, nds = 1,5-naphthalenedisulfonate] (3), [(HL)·(dnb)·(Hdnb), dnb = 3,5-dinitrobenzoate, Hdnb = 3,5-dinitrobenzoic acid] (4) and [(HL)·(dca), dca = dichloroacetate] (5) from 2,6-dimethylaniline and organic acids were prepared and characterized by XRD analysis, IR, mp and elemental analysis. Compound 1 adopts the triclinic, space group Pī, with a = 7.6261(6) Å, b = 8.3429(8) Å, c = 13.1147(12) Å, α = 91.3610(10)º, β = 102.755(2)º, γ = 102.597(2)º, V = 791.96(12) Å3, Z = 2. Compound 2 belongs to the monoclinic, space group P2(1)/c, with a = 14.2552(15) Å, b = 8.1436(8) Å, c = 14.5708(13) Å, α = 90°, β = 113.795(2)º, γ = 90°, V = 1547.7(3) Å3, Z = 4. Compound 3 crystallizes in the monoclinic, space group P2(1)/c, with a = 8.4784(7) Å, b = 17.4798(15) Å, c = 9.1119(8) Å, α = 90°, β = 99.742(2)º, γ = 90°, V = 1330.9(2) Å3, Z = 2. Compound 4 has orthorhombic, space group Pna2(1), with a = 24.5029(19) Å, b = 7.5322(9) Å, c = 26.665(2) Å, α = 90°, β = 90°, γ = 90°, V = 4921.3(8) Å3, Z = 8. Compound 5 crystallizes in the monoclinic, space group C2/c, with a = 19.8970(17) Å, b = 11.1850(11) Å, c = 13.1590(12) Å, α = 90°, β = 123.408(3)º, γ = 90°, V = 2444.6(4) Å3, Z = 8. For 1 it was the relatively weak phenol that has ionized, different from 2 to 5. All supramolecular architectures of 1–5 involve N–H⋯O H-bonds as well as CH3⋯O interactions. The other noncovalent interactions (CH⋯O, CH⋯Cl, O⋯C, O⋯N, O⋯O, Cl⋯Cl, C⋯π, O⋯π, CH3⋯π and π⋯π) in the crystal packing were also ascertained. These weak interactions combined, all compounds displayed 3D framework structures.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2018-12-15
Lai-Jun Zhang, Li Qi, Xiu-Ying Chen, Feng Liu, Li-Juan Liu, Wen-Li Ding, De-Lin Li, Guo-Cai Yuan, Ji-Zao Tong, Fa-Yun Chen, Hai-Jin Huang, Yong-Hua Wang

Two reduced Schiff bases, namely 5-[(2-hydroxybenzyl)amino]isophthalic acid (1) and 5-[(pyridin-4-ylmethyl)amino]isophthalic acid (2), were synthesized in two-step method using 5-aminoisophthalic acid as the starting material, and were characterized by single-crystal X-ray diffraction, elemental analysis, infrared, 1H NMR, mass, absorption and fluorescence spectra. Both 1 and 2 crystallize in monoclinic system with space groups P21/c for 1 and P21/n for 2. Photophysical properties of both 1 and 2 are significantly different from those of raw material 5-aminoisophthalic acid due to stronger p → π conjugation when one amino hydrogen atom in 5-aminoisophthalic acid is substituted with electron-donor group. 1 displays a very strong narrow-band blue fluorescence with the maximum peak at 439 nm, a high quantum efficiency up to 64%, and a narrow full width at half maximum of 35 nm, while 2 has a broader and weaker fluorescence with the peak at 418 nm and FHWM of about 50 nm.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2018-12-14
Hüseyin Ünver, Celal Tuğrul Zeyrek, Bahadir Boyacioglu, Mustafa Yıldız, Neslihan Demir, Ayhan Elmali

We report the synthesis and characterization, colorimetric anion sensors properties, density functional theory (DFT) calculation studies of a Schiff base (E)-2-[(3,5-bis(trifluoromethyl)phenylimino)methyl]-4-chlorophenol. The molecular structure of the title compound was experimentally determined using X-ray single-crystal data and was compared to the structure predicted by theoretical calculations using DFT. The experimental and calculated data (using DFT) of the title compound have been compared. To investigate the tautomeric stability, some properties such as total energy, HOMO and LUMO energies, the chemical hardness (η), the ionization potential, the electron affinity, the absolute electronegativity (χ), the absolute softness (σ) of the compound were obtained at B3LYP/6–311++G(d,p) level in the gas phase and solvent phase. The calculated results showed that the enol-imine form of the compound was more favorite than keto-amine form. The colorimetric response of the Schiff base receptors in DMSO was investigated.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-09-23
Rahul P. Dubey, Urmila H. Patel

The cadmium complex of picoline and sulfadiazine, a constituent of the triple sulfa drug, was synthesized and characterized by IR, NMR, and PL. It crystallizes in the orthorhombic space group Pca21 with the lattice parameters a = 13.73(10) Å, b = 17.0800(13) Å and c = 14.0558(11) Å. The experimental geometric data of the crystalline compound were compared with theoretical data in gaseous phase (B3LYP data). The HOMO and LUMO energy of the title molecule were calculated to get better knowledge of the reactivity and charge transfer properties. In addition, charge distributions from a Mullikan population, natural population, and NBO analysis were performed using the B3LYP method.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-04-22
Vitthal A. Kawade, Satish S. Bhat, Ray J. Butcher

Coordination polymer {[Cu(bpy)(bpe)(NO3)2]·(H2O)4}n (CP1) has been synthesized using [Cu(bpy)(NO3)2] (where bpy = 2,2′-bipyridine) and bpe (bpe = 1,2-bis(4-pyridyl)ethane as a spacer in equimolar ratio. CP1 was characterized by using Infrared spectroscopy, elemental analysis, and single crystal X-ray diffraction. The crystal structure confirms that the CP1 is formed with a bridging bpe linker giving rise to helical chain in one-dimensional (1D) structure. Copper ion is connected to two nitrogen atoms from bpy, two oxygen atoms from nitrate anions (major component) and two nitrogen atoms from two bpe ligands. There is an additional minor component which is five coordinate. The hydrogen bonding links the helical chains to generate a three dimensional (3D) network structure.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2018-11-01
E. K. Voinkov, R. A. Drokin, E. N. Ulomskiy, P. A. Slepukhin, V. L. Rusinov, O. N. Chupakhin

The X-ray data of 2-methylsulfanyl-6-nitro-1,2,4-triazolo [5,1-c][1,2,4]triazin-7-one sodium salt dihydrate (triazavirin) is reported. The compound crystallizes in the form binuclear complex шт triclinic space group P-1 with unit cell parameters: a = 7.2616 (6) Å, b = 9.3036 (5) Å, c = 9.5237 (7) Å, α = 110.968 (6), β = 92.600 (6)°, γ = 102.990 (6)° and Z = 1.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2018-12-04
T. M. Asha, M. R. P. Kurup

Cis-dioxidomolybdenum(VI) complexes [MoO2L1(DMSO)] (1), [MoO2L2(H2O)]·DMF (2) and [MoO2L3(DMF)] (3) were synthesized by solution based reactions of aroylhydrazones (H2L1 = 5-chloro-2-hydroxybenzaldehyde nicotinoylhydrazone, H2L2 = 2-hydroxy-5-iodobenzaldehyde nicotinoylhydrazone and H2L3 = 3,5-dichloro-2-hydroxybenzaldehyde nicotinoylhydrazone) with bis(acetylacetonato)dioxidomolybdenum(VI) complex, [MoO2(acac)2] in presence of DMSO or DMF. The synthesized aroylhydrazones and their molybdenum complexes were characterized by elemental analysis, spectroscopic techniques (FT-IR, UV–Vis, 1H NMR) and conductivity measurements. Finally the three dimensional structures of the complexes were confirmed by single crystal X-ray diffraction studies. Crystal structures of 1, 2 and 3 were solved by direct methods and refined with full-matrix least-squares calculations using the SHELXS97 and SHELXL2014 software programs respectively. Complex 1 got crystallized in monoclinic space group, P21/c with Z = 4, whereas complexes 2 and 3 in triclinic space group, P$$\overline {1}$$ with Z = 2. The ligands, H2L1−3 showed coordination to the metal ion in a dibasic tridentate manner through deprotonated phenolate oxygen, azomethine nitrogen and enolate oxygen.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-01-02
Yubo Xing, Yuqi Liu, Binfang Meng, Xiaofei Xue, Xinying Wang, Wei Li

Two novel transition-metal coordination polymers with the formulas [Co(L1)(bbi)(H2O)]n (1) and {[Co(L2)(phen)]·H2O}n (2) (H2L1 = 1,4-naphthalenedi- carboxylic acid, H2L2 = 5-OH-1,3-benzenedicarboxylic acid, bbi = 1,1′-(1,4-butanediyl)bis(imidazole), phen = 1,10-phenanthroline) have been hydrothermally synthesized and characterized by techniques of single crystal X-ray diffraction, infrared spectra, elemental analysis, powder X-ray diffraction, and variable-temperature magnetic susceptibility measurements. X-ray crystal structure analyses reveal that complex 1 exhibits 2D framework with 4-connected sql topology and is further extended into a 3D supramolecular architecture via strong O–H···O and weak C–H···O hydrogen-bonding interactions, while complex 2 features a 1D ladder-like chain with a 3-connected (42·6) topological structure. Magnetic studies showed the presence of an antiferromagnetic interaction between adjacent Co(II) ions in both complexes.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-10-17
Mária Šimuneková, Peter Schwendt, Róbert Gyepes, Lukáš Krivosudský

Two new 1D polymeric heterometallic copper–vanadium compounds were prepared. The polymers are constructed from [Cu(im)4]2+ cations that are coordinated to two terminal oxido ligands of [V2O4(mand)2]2− anions. The stronger coordination in [Cu(im)4V2O4(mand)2]n (1) that contains the racemic mandelato ligand is manifested by a shorter Cu‒O bond distance 2.4095(12) Å, while the weaker interaction in [Cu(im)4(V2O4((S)-mand)2)]n·2nH2O (2) is exhibited by Cu‒O bond distances 2.4547(16) Å and 2.5413(16) Å. The vanadate anion in compound 2 carries only the (S)-enantiomer of the initial mandelic acid and differs from the anion in 1 in parallel cis orientation of the phenyl groups of the mandelato ligand. FT-IR spectroscopy was used for the confirmation of the coordination mode of mandelato ligand. Strong bands corresponding to the vibrations of carboxyl groups can be observed around 1650 and at 1344 cm−1. The stretching vibration of deprotonated hydroxyl group in the mandelato ligand occurs at 1045 and 1065 cm−1 for 1 and 2, respectively. In addition, the very strong, characteristic band corresponding to ν(V=O) vibration can be observed at 931 cm−1 for 1 and 925 cm−1 for 2, as well as in Raman spectrum.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-10-16
Owen J. Curnow, Chaminda D. Jayasinghe, Matthew I. J. Polson, Ruhamah Yunis

The crystal structures of tris(ethylmethylamino)cyclopropenium bromide and tris(allylmethylamino)cyclopropenium chloride are found to contain weak dimers of the cyclopropenium cation whereas the structure of the mixed salt of tris(dimethylamino)cyclopropenium chloride and dimethylammonium chloride reveals half of the cyclopropenium cations to have formed dimers and the other not to have formed dimers. These structures are compared to three related triiodide salts ([C3(NMeEt)3]I3, [C3(NEt2)3]I3 and [C3(NBu2)3]I3) as well as the previously-reported salts [C3(NEtMe)3]Cl, [C3(NH2)3]Cl, [C3(NH2)3]I and [C3(NEt2)3]I. The distances between the C3 centroids of the staggered dimers are at the short end of those normally found in π-stacked neutral arenes, let alone charged aromatic rings. Factors leading to the formation of dimers and the effect of dimer formation on the cyclopropenium structures are investigated.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-10-09
Shampa Chakraborty, Shyamaprosad Goswami, Annada C. Maity, Ching Kheng Quah, Sandipan Halder

Single crystal X-ray structures of new perchlorate salts of 6-carboxylic acid 5-deaza pterin perchlorates (cdpt) and 6-carboxylic acid 5-deaza pterin tetrahydro perchlorates (cdtpt) and chloropterin (cpt) are reported.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-10-09
Cheng-Hu Xie, Yong-Mei Cui, Dan-Hui Jin, Yan-Ru Xiao, Hai-Xia Lin

Two novel taxoids were synthesized from 1-deoxybacctin VI (5) and their crystal structures were determined by X-ray crystallographic techniques. The influence of C(10) substituents of the cyclooctane ring B on molecular conformations were investigated. A larger effect on the conformation of the diterpenoid core is observed when the hydroxyl group is oxidized at the C(9) position and the hydroxyl group is acylated at the C(10) position compared to other baccatin analogs. Compounds 12a and 12c crystallize in the orthorhombic space group P212121. In the structures, the six-membered A ring exhibits a 1, 4-di-planar conformation, the eight-membered B ring adopts boat–chair conformation, and the six-membered C ring exhibits a slightly distorted half-chair conformation.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-09-27
Xiu-Guang Yi, Xiao-Niu Fang, Yin-Feng Wang, Jin Guo, Jia Li

A novel copper complex [CuL(bipy)(H2O)]·H2O was synthesized by solvothermal reaction and its crystal structure was determined by single-crystal X-ray diffraction technique. (HL = 3-hydroxy-2-methylquinoline4-carboxylic acid; bipy = 2,2′-bipyrdine) The title complex (1) crystallizes in the orthorhombic system of the Pbca space group, and exists as an isolated mononuclear structure. The intermolecular hydrogen bonds and the strong π···π stacking interactions yield a three-dimensional (3-D) supramolecular network. Solid-state photoluminescence spectrum uncovers that it shows an emission in the pale blue region of the light spectrum. It has remarkable CIE (Commission Internationale de I’Éclairage) chromaticity coordinates of (0.2656, 0.3162), so it may be a very promising color lighting and display converter. Time-dependent density functional theory (TDDFT) calculation reveals that this emission is caused by to the ligand-to-ligand charge transfer (LLCT). Solid-state diffuse reflectance data shows that there is a narrow optical band gap of 1.38 eV. Therefore, it could be probably a candidate for narrow band gap semiconductors.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-09-26
Xiu-Mei Li, Zhi-Tao Wang, Valentin Valtchev, Qian-Rong Fang, Ya-Ru Pan

Two new Zn(II) coordination polymers based on bis(imidazol), namely, [Zn(hba)2(bib)]n(1) and [Zn(NAA)(bib)1.5]n·nNO3−·3nH2O (2) (Hhba = 3-hydroxybenzoic acid, HNAA = 1-naphthyl acetic acid, bib = 1,4-bis(imidazol-1-yl)-butane) have been successfully synthesized under hydrothermal conditions. Their structures have been determined by single crystal X-ray diffraction analyses, elemental analyses, IR, TG and fluorescence spectrums. Complex 1 shows a one-dimensional zigzag chain structure. Complex 2 exhibits two-dimensional network structure. The intermolecular hydrogen bonding and π–π stacking interactions extend the complexes 1 and 2 into supramolecular architectures and play an important role in stabilizing complexes 1 and 2. Furthermore, complex 1 exhibits intense blue luminescence and appears to be a good candidate for novel hybrid inorganic–organic photoactive materials, while no photoluminescent response was observed for complex 2. In addition, we analyzed the Natural Bond Orbitals (NBO) of 1 and 2 using the PBE0/LANL2DZ method in the Gaussian 09 Program. The calculations showed the obvious covalent interaction between the coordinated atoms and Zn(II) ion.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-09-26
Daniel E. Lynch, Emily M. Harcourt, James T. Engle, Joshua R. Farrell, Christopher J. Ziegler, Darren G. Hamilton

The crystal structures of six cobalt sandwich complexes—four in the η5-cyclopentadienyl/η4-cyclobutadiene family, two from the related η5-cyclopentadienyl/η4-cyclopentadienone family—are presented and discussed alongside related structural precedents. In each of the complexes an undecorated cyclopentadienyl ligand is present whereas the partner cyclobutadiene or cyclopentadienone ligand bears four identical aromatic substituents (phenyl, p-tolyl, p-fluorophenyl, 2-thienyl or 2,2′-bithienyl). This range of substituents allows for detailed structural comparison between members of the families of sandwich complexes presented here, and with previously reported structures.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-01-05
Wulan Zeng, Xia Wang

The original version of this article unfortunately contains the error in reaction Scheme 1 Graphical Abstract and inside text.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2018-10-31
Wulan Zeng, Xia Wang

A new intermediate, C22H30N2O8 (J0) was attained by reaction of 6,10-dioxaspiro[4.5]decane-7,9-dione with 1,1-dimethoxy-n,n-dimethyl-methanamin in ethanol. The two oxaspirocyclic compounds C16H17NO4 (J1) and C16H17NO4 (J2) were prepared by adding 2-methylbenzenamine and 3-methylbenzenamine into to the ethanol solution of J0, respectively. Two crystals (J0 and J1) were determined by single-crystal X-ray diffraction. The compound of J0 includes one (C5 H13 N2)+ cation and one (C17 H17 O8)− anion, which indicates it is a salt. There is no classical hydrogen bonds in J0. However, there is one kind of N–H⋅⋅⋅O intramolecular interactions and one kind of C–H⋅⋅⋅O intermolecular interactions in J1. In addition, the fluorescence spectra of J1 and J2 in dilute ethanol were studied, which they exhibit purplish red emission and reddish purple emission, respectively.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-04-23
Július Sivý, Štefan Marchalín, Peter Šafář

Two crystals of quinolizidine compounds; systematic name: (rac)-(7,8,9,9a)-tetrahydro-4H-thieno[2,3-b]quinolizine-6,10-dione, (I), and (rac)-(9a,10)-10-hydroxy-8,9,9a,10-tetrahydro-4H-thieno[2,3-b]quinolizin-6(7H)-one, (II), have been compared and characterized by single-crystal X-ray diffraction and electronic analysis. N-heterocyclic rings in both structures are not planar and adopt a half-chair conformation. The molecules of (I) are linked via weak C–H···O hydrogen bonds into chains along c axis. While the crystal stacks in compound (II) are formed by strong O–H···O hydrogen bonds the molecules link into infinite zig-zag chains along the b axis. In both crystal structures, π–π stacking and C–H···π interactions are also observed. Calculation of the net atomic charges shows that O atoms in both compounds carry a relatively large negative charges, in comparison with the corresponding H atoms. Crystal, molecular and electronic structures of these compounds, which are influenced by hydrogen-bonded assemblies in the molecular crystals, are discussed in detail.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2018-11-19
Xinchen Chi, Lanqing Wang, Shouwen Jin, Daqi Wang, Ying Zhao, Zhaohui Tao

Two crystalline compounds N-(5-chloro-2-hydroxy-phenyl)-acetamide [L] (1), and (N-(5-chloro-2-hydroxy-phenyl)-acetamide): (3,5-dinitrobenzoic acid) [(L) · (3,5-Hdns), 3,5-Hdns = 3,5-dinitrobenzoic acid] (2) were prepared and characterized by X-ray diffraction analysis, IR, mp, and elemental analysis. Compound 1 crystallizes in the monoclinic, space group C2/c, with a = 9.9833(7) Å, b = 10.7789(8) Å, c = 16.1622(14) Å, β = 92.8010(10)°, V = 1737.1(2) Å3, Z = 8. Compound 2 crystallizes in the monoclinic, space group C2/c, with a = 32.818(3) Å, b = 6.9900(5) Å, c = 14.8431(12) Å, β = 90.5340(10)°, V = 3404.8(5) Å3, Z = 8. Both supramolecular architectures of the compounds 1–2 involve N–H···O/O–H···O/C–H···O hydrogen bonds as well as other non-covalent association. The role of these non-covalent interactions in the crystal packing is ascertained. These weak interactions combined, the compounds displayed 1D–3D structures.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2019-07-11
Emily O’Loughlin, Edward J. Valente

Three methods for producing anhydrides of arylfuran and arylpyran pseudoacids were explored. These included thermal dehydration, phosgene or thionly chloride activation and decomposition, and dicyclohexylcarbodiimide activation and coupling. Derivatives of the cyclic forms of o-formylbenzoic acid, o-acetylbenzoic acid, 2-carboxyphenylacetaldehyde and of 4,4-dimethyl-3,4-dihydro-3-hydroxy-[1H]-isobenzopyran-1-one were formed including dipseudoanhydides and normal-pseudo anhydrides. Crystal and molecular structures for meso and (R,R/S,S)-bis(1[3H]-isobenzofuranone-3-yl)ether, (R,R/S,S)-bis(3-methyl-1[3H]-isobenzofuranone-3yl)ether, meso (3,4-dihydro-[1H]-isobenzopyran-1-one-3-yl)ether, 3-benzoyloxy-1[3H]-isobenzofuranone, 3-benzoyloxy-3-methyl-1[3H]isobenzofuranone, 3-(4′-nitrobenzoyloxy)-4,4-dimethyl-3,4-dihydro-[1H]-isobenzopyran-1-one, and (1[3H]-isobenzofuranone-3-yl)(4,4,dimethyl-3,4-dihydro-[1H]-isobenzopyran-1-one-3-yl)ether are reported. Endocyclic pseudoacyl C–O bonds are always longer than the exocyclic pseudoacyl C–O bonds. It is possible to refine the previously established C–O bond length dependencies on the pKa (of the conjugate acids) of the leaving groups for 3-substituted 1-[3H]-isobenzofuranones. Of six dipseudoanhydrides studied, conformations are found with exocyclic C–O(ether) linkages synclinal to the endocyclic C–O and away from the ring (exo conformation) in two meso structures, two of three RR/SS forms and in a chiral unsymmetrical form. An endo conformation is observed in one of the RR/SS forms. In three normal-pseudo anhydrides, both endo and exo conformations are observed.

更新日期：2019-11-04
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2010-06-08
Rong Fan,Qiu-Ping Zhou,Guo-Fang Zhang,Mei-Yu Cai,Ping Li,Li-Hua Gan,Feng-Qi Zhao,Ji-Zhen Li,Xue-Zhong Fan,Seik Weng Ng

Nine metal compounds of Mn(II), Zn(II) and Cd(II) derived from dinitropyridone ligands (3,5-dinitro-pyrid-2-one, 2HDNP; 3,5-dinitropyrid-4-one, 4HDNP and 3,5-dinitropyrid-4-one-N- hydroxide, 4HDNPO) were characterized by elemental analysis, FT-IR and partly by TG-DSC. Three of which were further structurally characterized by X-ray single-crystal diffraction analysis. The structures of the three compounds, Mn(4DNP)(2)(H(2)O)(4), 4, Zn(4DNPO)(2)(H(2)O)(4), 8, and Cd(4DNPO)(2)(H(2)O)(4), 9, crystallize in the monoclinic space group P2(1)/n and Z = 2, with a = 8.9281(9), b = 9.1053(9), c = 10.6881(11) A, beta = 97.9840(10) degrees for 4; a = 8.4154(7), b = 9.9806(8), c = 10.5695(8) A, beta = 97.3500(10) degrees for 8; a = 8.5072(7), b = 10.2254(8), c = 10.5075(8) A, beta 96.6500(10) degrees for 9. All three complexes are octahedral consisting of four equatorial water molecules, and two nitrogen or oxygen donor ligands (DNP or DNPO). The abundant hydrogen-bonding and pi-pi stacking interactions seem to contribute to stabilization of the crystal structures of the compounds. The TG-DTG results revealed that the complexes showed a weight loss sequence corresponding to all coordinated water molecules, nitro groups, the breaking of the pyridine rings and finally the formation of metal oxides.

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2010-06-08
Guo-Fang Zhang,Mei-Yu Cai,Ping Jing,Chong He,Ping Li,Feng-Qi Zhao,Ji-Zhen Li,Xue-Zhong Fan,Seik Weng Ng

Two transition-metal compounds derived from 2,4-dinitroimidazole, {[Ni(DNI)(2)(H(2)O)(3)][Ni(DNI)(2) (H(2)O)(4)]}.6H(2)O, 1, and Pb(DNI)(2)(H(2)O)(4), 2, were characterized by elemental analysis, FT-IR, TG-DSC and X-ray single-crystal diffraction analysis. Crystal data for 1: monoclinic, space group C2/c, a = 26.826(3), b = 7.7199(10), c = 18.579(2) A, beta = 111.241(2) degrees and Z = 4; 2: monoclinic, space group C2/c, a = 6.5347(6), b = 17.1727(17), c = 14.1011(14) A, beta = 97.7248(10) and Z = 4. Compound 1 contains two isolated nickel centers in its structure, one being six-coordinate and another five-coordinate. The structure of 2 contains a lead (II) center surrounded by two chelating DNI ligands and four water molecules in distorted square-antiprism geometry. The abundant hydrogen bonds in two compounds link the molecules into three-dimensional network and stabilize the molecules. The TG-DSC analysis reveals that the first step is the loss of water molecules and the final residue is the corresponding metal oxides and carbon.

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2010-05-18
Naijue Zhu,Danielle Lightsey,Jiawang Liu,Maryam Foroozesh,Kathleen M Morgan,Edwin D Stevens,Cheryl L Klein Stevens

The single-crystal X-ray structures and in vivo activities of three aryl acetylenic inhibitors of cytochromes P450 1A1, 1A2, 2A6, and 2B1 have been determined and are reported herein. These are 1-ethynylpyrene, 1-propy-nylpyrene, and 4-propynylpyrene. To investigate electronic influences on the mechanism of enzyme inhibition, the experimental electron density distribution of 1-ethynylpy-rene has been determined using low-temperature X-ray diffraction measurements, and the resulting net atomic charges compared with various theoretical calculations. A total of 82,390 reflections were measured with Mo Kα radiation to a (sinθ/λ)(max) = 0.985 Å(-1). Averaging symmetry equivalent reflections yielded 8,889 unique reflections. A least squares refinement procedure was used in which multipole parameters were added to describe the distortions of the atomic electron distributions from spherical symmetry. A map of the model electron density distribution of 1-ethynylpyrene was obtained. Net atomic charges calculated from refined monopole population parameters yielded charges that showed that the terminal acetylenic carbon atom (C18) is more negative than the internal carbon (C17). Net atomic charges calculated by ab initio, density functional theory, and semi-empirical methods are consistent with this trend suggesting that the terminal acetylenic carbon atom is more likely to be the site of oxidation. This is consistent with the inhibition mechanism pathway that results in the formation of a reactive ketene intermediate. This is also consistent with assay results that determined that 1-ethynylpyrene acts as a mechanism-based inhibitor of P450s 1A1 and 1A2 and as a reversible inhibitor of P450 2B1. Crystallographic data: 1-ethynylpyrene, C(18)H(10), P2(1)/c, a = 14.571(2) Å, b = 3.9094(5) Å, c = 20.242(3) Å, β = 105.042(2)°, V = 1,113.5(2) Å(3); 1-propynylpyrene, C(19)H(12), P2(1)/n, a = 8.970(2) Å, b = 10.136(1) Å, c = 14.080(3) Å, β = 99.77(2)°, V = 1,261.5(4) Å(3); 4-propynylpyrene, C(19)H(12), Pbca, a = 9.904(1) Å, b = 13.174(2) Å, c = 19.401(1) Å, V = 2,531.4(5) Å(3).

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2013-10-26
Kejia Ding,Sergey M Dibrov,Thomas Hermann

The preparation and crystal structure of 8-chloro-1H-pyrrolo[2,3-b]phenazine 5-oxide (1) are described. Compound 1 formed dark purple crystals from deeply colored solution in methanol. Crystal plates were in the triclinic system, P-1 space group with unit cell parameters a = 6.9514(8), b = 9.1568(10), c = 10.2067(11), α = 84.509(2), β = 82.936(2), γ = 72.357(2) and a cell volume of 613.25(12) A-3. The title compound which contains the first example of the extensively conjugated pyrrolo-phenazine N-oxide system exhibits strong light absorption in the green to cyan wavelength range which disappears upon protonation.

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2013-06-12
Sergey M Dibrov,Matthew A Parker,B Mikael Bergdahl,Thomas Hermann

The crystal structure of 8-((dimethylamino)methyl)-1-(3-(dimethylamino)propyl)-1,7,8,9-tetrahydrochromeno[5,6-d]imidazol-2-amine (1), an inhibitor of the hepatitis C virus internal ribosome entry site, is described and compared to the structure of the compound in complex with the viral RNA target. Compound 1 crystallized by pentane vapor diffusion into dichloroethane solution. It crystallized in the monoclinic system, P21/c space group with unit cell parameters a = 15.7950(5) Å, b = 14.0128(4) Å, c = 8.8147(3) Å, β = 94.357(2)° and a cell volume of 1945.34(11) A-3. Packing interactions in the small molecule crystal lattice correspond to key interactions of the compound with the viral RNA target.

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2012-06-02
Dustin W Demoin,Charles L Barnes,Timothy J Hoffman,Silvia S Jurisson

2-[2-benzothiazoylmethyl)thio]-benzenamine, which was first reported in 1898, was isolated from the reaction of bromoacetyl bromide and 2-aminothiophenol [1]. The product crystallized from an aqueous methanol solution of the reaction mixture to which nickel(II) acetate had been added. 2-[(2-benzothiazolylmethyl)thio]-benzenamine crystallized in the monoclinic system, in space group C2/c, with cell dimensions of a = 27.392 (19) Å, b = 4.730 (3) Å, and c = 23.686 (16) Å, β = 122.465 (6)°, V = 2589(3) Å(3), Z = 8 and refined to R = 0.0343 and R(w) = 0.0844. Crystallization from methanol yielded the product as the hydrobromide salt in the monoclinic space group Cc, with cell dimensions of a = 10.488 (3) Å, b = 33.404 (9) Å, c = 5.2578 (14) Å, β = 116.769(2)°, V = 1644.7(8) Å(3), Z = 4 and refined to R = 0.0296 and R(w) = 0.0600. Mass spectral and NMR analyses confirmed that the bulk and crystalline compound were all 2-[(2-benzothiazolylmethyl)thio]-benzenamine.

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2012-02-04
Anuruddha Rajapakse,Charles L Barnes,Kent S Gates

The helicene, pyrido[3,2-f]quinolino[6,5-c]cinnoline 5-oxide, was prepared by treatment of 6-hydroxylaminoquinoline with xanthine oxidase or treatment of 6-nitroquinoline with glucose in 30% NaOH and the product characterized using NMR, high resolution mass spectrometry, and X-ray crystallography. The hydrogens on carbons 7 and 12 of the terminal aromatic rings are separated by 2.495 Å creating an angle of 25.0° between the planes of the two quinoline ring systems. In the crystal, water molecules serve to link the helicenes into a one dimensional chain structure forming a hydrogen bonded bridge between N2 of one molecule and N4 of another. The molecule (C(18)H(10)N(4)O•H(2)O) crystallized in the monoclinic P2(1)/n space group. Unit cell parameters for pyrido[3,2-f]quinolino[6,5-c]cinnoline 5-oxide monohydrate: a = 7.0829(12), b = 18.559(3), c = 11.0985(19) Å, β = 107.736(2)°, and Z = 4.

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2010-07-01
Ujjal Sarkar,Rainer Glaser,Zack D Parsons,Charles L Barnes,Kent S Gates

1,2,4-Benzotriazine 1,4-di-N-oxides are potent antitumor drug candidates that undergo in vivo bioreduction leading to selective DNA damage in the low oxygen (hypoxic) cells found in tumors. Tirapazamine (TPZ) is the lead compound in this family. Here we report on the synthesis, crystal structure, and conformational analysis of a new analog, 3-cyclopropyl-1,2,4-benzotriazine 1,4-di-N-oxide (3). Compound 3 (C(10)H(10)N(3)O(2)) crystallized in the monoclinic space group C2/c. Unit cell parameters for 3: a = 16.6306 (12), b = 7.799 (5), c = 16.0113 (11) Å, α = 90, β = 119.0440 (10), γ = 90, and z = 8.

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2009-05-01
D Michelle Motley,Judith A Walmsley,Julio Zukerman-Schpector,Edward R T Tiekink

The gold(III) atom in [Au(NH2CH2CH2NH2) Cl2]NO3 is chelated by the ethylenediamine (en) ligand and the approximately square planar geometry is completed by two chloride atoms. Weak Au⋯O and Au⋯Cl contacts are noted above and below the square plane leading to a tetragonally distorted octahedron for the gold(III) center. Extensive charge-assisted hydrogen bonding of the type N-H⋯O leads to the formation of a 2-D array and layers are consolidated into a 3-D network via C-H⋯O and C-H⋯Cl contacts. The compound crystallizes in the orthorhombic space group Pbca with a = 10.3380(11) Å, b = 8.2105(7) Å, c = 19.625(2) Å, and Z = 8.

更新日期：2019-11-01
• J. Chem. Crystallogr. (IF 0.63) Pub Date : 2010-11-01
Gary S Nichol,Ruben Vardanyan,Victor J Hruby

As part of a study into new Fentanyl-derived opioid compounds with potent analgesic activity and reduced side effects the starting material title compound, C14H21N3O (1), was synthesized and characterized by NMR spectroscopy and single-crystal X-ray diffraction. The crystal structure is monoclinic Cc with unit cell parameters a = 14.1480(3) Å, b = 14.1720(4) Å, c = 27.6701(7) Å, β = 96.956(1)°, α = γ = 90°. The compound has crystallized with four crystallographically unique molecules in the asymmetric unit; each molecule has a very similar conformation and an analysis of the structure shows that although all four unique molecules overlay very well there is no evidence of pseudo-symmetry which would relate the molecules in the higher symmetry space group C2/c. The crystal packing consists of two separate hydrogen bonded chains which are linked together to form a thick 2D structure in the ab plane.

更新日期：2019-11-01
Contents have been reproduced by permission of the publishers.

down
wechat
bug