Hyperlipidemia, a major pathological condition associated with disrupted lipid levels and physiological redox homeostasis. The excessive release of reactive oxygen species (ROS) leads to enhanced lipid peroxidation, aggravated atherosclerosis and oxidative stress. Integration of natural antioxidant blends in alone or with conventional treatments can alleviate these issues synergistically contributing least side effects. Published literature reported the efficacy of natural antioxidants as individual and in combinations in various conditions but less data is available on their evaluation in low dose ratio blends particularly in hypercholesterolemic diet.n = 6) weighing 1.2–1.6 kg, supplemented with high cholesterol diet (400 mg/kg) for 12 weeks were used in the experiment. Antioxidants were administered individual high (100 mg/kg) and in low dose combinations . Student’s t test and one way analysis of variance (ANOVA) followed by Dunnet’s test were used as statistical tools for evaluation.Antihyperlipidemic effects of selected natural antioxidants; the phenolic oligomeric proanthocyanidins (OPC) and pterostilbene (PT) with niacin (NA) were investigated in current study. Their effects on lipid profile, lipid peroxidation and their aptitude to establish redox state between oxidants and antioxidants in body were evaluated in high cholesterol diet fed animal model. Male albino rabbits (p >0.001) observed in 50:30:20 ratios of OPC, NA and PT, compared to individual therapies 37 and 18 % max respectively. Moreover the results were also in close proximity with the statin therapy .The results showed synergistic effects of low dose antioxidant blends. Therapies retarded elevation in blood lipid levels, lipid peroxidation and blood antioxidant depletion and consequently contributed in reestablishing redox homeostasis. The LDL/HDL ratio and atherogenic index were suppressed significantly in blend therapies with maximum effects of 59.3 and 25 % (This study provides an evidence for natural antioxidants blends superiority over individual therapy in chronic diseases like hyperlipidemia. Such therapies in human equivalent doses can help in mitigating chronic illnesses in general populations. Their oxidation leads to severe endothelial cell injury and atherosclerosis [Hyperlipidemia is a major pathological condition associated with mortality and disability in both developed and developing countries . Chronicclerosis –6. The sclerosis . Howeverclerosis . The antclerosis , 10. In clerosis , 11, 12.clerosis –16.Natural antioxidants were evaluated in individual and in combinations for lipid lowering and free radical scavenging properties and were found effective in depressing the disease progression –22. In cOligomeric proanthocyanidins (OPC) is a polyphenolic compound belongs to flavonoids class, widely distributed in plants and posses potent antioxidant  and lipit test was applied to evaluate the difference statistically. Lipid profiles are calculated as mean ± SEM (n = 6) along with p-values in Table Acute rise in lipid profiles were observed in rabbits administered with cholesterol for 2 weeks compared to healthy group. Almost two to four time rise was observed in every parameter. Student’s p <0.001), 20.26 ± 0.94 (p <0.001) and 19.19 ± 0.91 (p <0.01) and AI values 0.893 ± 0.033 (p <0.01), 0.896 ± 0.053 (p <0.01), 0.971 ± 0.073 (p <0.05) respectively. The atorvastatin therapy showed 14.0 ± 0.99 (p <0.001) and 0.785 ± 0.061 (p <0.001) compared to disease control 30.50 ± 0.69, 1.096 ± 0.040. In combination therapies the results were even more significant and synergism were observed by improving blood lipid profile depending on dose ratio in particular combination. Among combinations of OPC with NA the 70:30 ratio delivered significant effects by suppressing LDL/HDL ratio to 15.36 ± 0.98 (p <0.001) while differ nonsignificantly from other two ratios 16.77 ± 0.69 (p <0.001) and 17.33 ± 0.75 (p <0.001). AI was significantly reduced to 0.843 ± 0.041 (p <0.001), 0.837 ± 0.045 (p <0.001) and 0.887 ± 0.037 (p <0.01) in 70:30, 30:70 and 50:50 respectively. Similarly in OPC with PT combinations all the ratios provided significant effects compared to disease control but no significant differences were observed between the groups. The LDL/HDL and AI were 14.60 ± 0.98 (p <0.001) and 0.851 ± 0.041 (p <0.001) in 70:30 ratio, 15.19 ± 0.42 (p <0.001), 0.929 ± 0.057 (p <0.05) in 30:70 and 16.33 ± 0.75 (p <0.001), 0.906 ± 0.037 (p <0.01) in 50:50 respectively. In NA and PT, the 70:30 and 50:50 combinations induced similar effects on LDL/HDL ratios 15.16 ± 0.89 and 15.16 ± 0.84 (p <0.001) respectively, while comparing AI values results were more profound in 70:30 (0.858 ± 0.053) (p <0.001) compared to other groups 0.919 ± 0.037 (p <0.05) and 0.868 ± 0.037 (p <0.01) respectively. In general the two drug combinations showed synergism, evident from significant outcome however differ less from one another [Single drug therapies showed significant effects in reducing lipid levels, confirmed by LDL/HDL ratio and atherogenic index (AI). The OPC, NA and PT maintained LDL/HDL ratios by 19.49 ± 0.87 (p <0.001) comparable with the statin outcome 52.66, 26.28 % (p <0.001) respectively. Though there were minor differences among the groups but differ significantly from the disease control. The high dose single drug therapies suppressed LDL/HDL by 37 % and AI by 18.5 % maximum, which are much less as compared to low dose blend therapies confirmed the superiority of combinational therapies. Lipid profiles in mean ± SEM and %change in blood lipids at 95 % confidence interval are summarized in Tables The ratios with optimum lipid lowering effects in above therapies were subsequently molded in to three drug combinations to evaluate the extent of synergism of antioxidants acting through various mechanisms. The antioxidant with highest ratio (70 %) was reduced by 20 mg and this amount was replaced with third candidate. All three drug combinations showed more significant results as compared to two drug combinations. Most significant effects were observed in 50:30:20 ratio of OPC, NA and PT which suppressed LDL/HDL ratio by 59.3 % and AI by 25 %  respectively in combination therapies compared to disease control 19.30 ± 1.18, 3.01 ± 0.28 and 3.73 ± 0.412 μmol/L. Although in individual therapies the raised levels of methionine, GSH and NAC (24.73 ± 1.04 μmol/L (p <0.05), 3.38 ± 0.42 μmol/L (p <0.01) and 3.86 ± 0.404 μmol/L (p <0.05)) were less significant compared to combination therapies. The all-trans retinoic acid showed opposite results and increased parallel with the lipid levels from 1.80 ± 0.10 μmol/L (blank control) to 4.48 ± 0.24 μmol/L (disease control) while in treatment groups its elevation was retarded down to 3.26 ± 0.12 μmol/L (p <0.001) max; observed on 70:30 ratio of OPC and PT.Significant up-regulation was observed in levels of methionine, GSH and NAC upto 35.08 ± 1.60, 3.82 ± 0.47 and 4.21 ± 0.425 μmol/L (p <0.01) among individual therapies and more in combinational therapies ranging 2.51 ± 0.092 to 3.40 ± 0.097 (p <0.001), compared to disease control 2.12 ± 0.058. Homocysteine level was significantly controlled down to 10.09 ± 1.39 μmol/L (p <0.01), although nonsignificant variations were observed among treatment groups. Almost half of groups delivered nonsignificant effects on ascorbic acid levels with maximum effect of 5.29 ± 0.51 μmol/L (p <0.001) observed in 50:30:20 ratio of OPC, NA and PT compared to disease control 4.90 ± 0.59 μmol/L. The natural antioxidants were able to correct the antioxidant levels in blood and are more effective when used in blend therapies rather than individual as summarized in mean ± SEM in Tables The improvement in GSH/GSSG ratios was significant in OPC (2.83 ± 0.065)  (≥99 % pure). Cholesterol kit; TC, TG and HDL (Human diagnostics GmbH Germany). Oligomeric proanthocyanidins (OPC) , pterostilbene (PT)  (≥99 % pure) and niacin (NA) (Scharlau Chemie SA) (≥98 % pure).HPLC system  linked with a DECADE II Electrochemical Detector , HPLC column Discovery HS C18 RP chromatographic column . Lambda-25 UV/Visible spectrophotometer (Perkin Elmer). Centrifuge machine (Centurion scientific Ltd) and Incubator (Incucell Med Center GmbH Germany) were used in the analysis.n = 6. Three groups were treated with OPC, PT and NA individually in 100 mg/kg doses along with cholesterol doses. In 09 groups, low dose combinatorial blends of all the three drugs in 30:70, 50:50 and 70:30 ratios were administered and most effective combination in each two drug combinations was further incorporated in three drug combinations  were used in the experiment. The experimental protocol for our study was approved by ethical committee of Department of Pharmacy University of Peshawar under reference number: 04/EC-15/Pharm. After 7 days of acclimatization in animal house and bio assay center, hyperlipidemia was developed according to the previous reported protocol . AnimalsPlasma lipid profiling was performed on commercial kits. Base line levels were recorded and samples were taken at every 2 weeks interval after overnight fasting to evaluate the effect of therapies on blood lipid levels sequentially. Total cholesterol (TC), teiglyceride (TG) and high density lipoproteins (HDL-C) were calculated enzymatically, while low density lipoproteins (LDL-C), very low density lipoproteins (VLDL-C) and atherogenic index (AI) were calculated according to the following formulae –65.1\doctrans retinol (ATR) were determined simultaneously using HPLC-UV [Serum levels of water soluble thiol antioxidants; glutathione (GSH) its oxidized form (GSSG), GSH/GSSG ratio, cystine, cysteine (cys), Homocysteine (Hcy), methionine (meth), N-acetylcysteine (NAC) long with ascorbic acid (AA) and lipid peroxidation were determined simultaneously at the end of study using RP-HPLC- electro chemical detection (ECD) method . Fat sol HPLC-UV .t test for pair analysis and one way analysis of variance (ANOVA) followed by Dunnett’s test for comparison of lipid lowering effect in all treatment groups with respect to the disease control (with no treatment). Data is presented in mean ± standard error of mean (SEM) at level of significance p <0.05 %.Data analysis was performed by applying student’s


II complex containing an σ-dimerized TCNQ–TCNQ unit is presented, with a C—C bond length of 1.653 (11) Å. In addition, the σ-dimerized TCNQ–TCNQ unit (refined 75% occupancy) is disordered, forming also a less populated pair of TCNQ molecules (25% occupancy) with tightly π-stacked dicyanomethanide groups.The first example of an Ni 3)2, 2,2′-bipyridine (bpy) and LiTCNQ  in a 1:3:2 molar ratio yielded single crystals of bis[trisnickel(II)] bis bi hexahydrate, [Ni(C10H8N2)3]2(C24H8N8)(C12H4N4)2·6H2O or [Ni(bpy)3]2(TCNQ–TCNQ)(TCNQ)2·6H2O. The crystal structure comprises [Ni(bpy)3]2+ complex cations, two centrosymmetric crystallographically independent TCNQ·− anion radicals with π-stacked exo groups, and an additional dimeric TCNQ–TCNQ unit which comprises 75.3 (9)% of a σ-dimerized (TCNQ–TCNQ)2− dianion and 24.7 (9)% of two TCNQ·− anion radicals with tightly π-stacked exo groups. The title complex represents the first example of an NiII complex containing a σ-dimerized (TCNQ–TCNQ)2− dianion. Disordered solvent water molecules present in the crystal structure participate in hydrogen-bonding interactions.Crystallization from an aqueous methanol system composed of Ni(NO Several complexes of NiII-containing TCNQ species have been reported previously, e.g. [Ni(terpy)2](TCNQ)2  with non-coordinating π-dimerized anion radicals  with σ-coordinating anion radicals 4·(CH3)2CO was reported, along with the results of its crystal structure analysis 3]2(TCNQ–TCNQ)(TCNQ)2·6H2O (1) and report here its crystal structure.In the quest for new promising molecular magnetic materials besides the complexes of 31, comprises two [Ni(bpy)3]2+ complex cations, a centrosymmetric TCNQ–TCNQ dimeric unit, two centrosymmetric crystallographically independent TCNQ·− anion radicals, and three crystallographically independent disordered solvent water molecules 8]·6H2O :0.247 (9)  1 − x, 1 − y, 2 − z] dimerization bond length is 1.653 (11) Å and this value is within the usual range (see Database survey section). At the same time, this value is longer than a usual single C—C bond and, consequently, the corresponding bond angles around the C37A atom range from 105.6 (4) to 113.6 (3)°, displaying significant deviations from the ideal tetrahedral angle. In the less populated pair of anion radicals within TCNQA, the distance between the C37B atom and its symmetry-related counterpart C37Biii is 3.06 (2) Å; the interplanar distance between the least-squares plane P1 formed by atoms C31B, C37B, C38B and C39B and the least-squares plane P2 formed by their symmetry-related counterparts through a centre of symmetry at  is 3.03 Å. The distance of the C37iii atom from the plane P1 is 2.90 Å and the slippage between atoms C37B and C37Biii is 0.98 Å. These geometric parameters suggest a very strong π-interaction between the less populated pair of anion radicals in TCNQA, and they are pre-positioned for σ-dimerization with little structural rearrangement required upon formation of the covalent bond. This could be seen as an indication of σ-bond formation in the solid state upon crystallization rather than pre-formation of the σ-dimers in solution.The unit cell of the title complex, s Figs. 1 ▸ ▸ ▸·− anion radicals, TCNQB and TCNQC, in the crystal structure of 1 ’ by Ballester et al. (1999Biii and N10vii  is, however, much longer than for the ‘front-end’ dicyanomethanide group. It is outside the usually observed range for strong π-stacking interactions in analogous systems  1 − x, 1 − y, 1 − z] and the second shortest contact is 3.479 (4) Å between atoms C46 and C53ii; the latter distance is already somewhat longer due to the noncoplanarity of the two anion radicals. These observed distances are at the upper border for stacking arrangements reported for similar compounds  hydrogen-bonded bridges involving TCNQA dianions and TCNQC anion radicals, yielding a supramolecular layer within the bc plane  form an additional hydrogen-bonded bridging path, N⋯H—O2A⋯H—O3B—H⋯O1B—H⋯N, between the supramolecular layers. On the other hand, the least-occupied position (O2B) of water molecule O2 seems to be hydrogen bonded only to the nitrile N atom and so partially occupies the void in the structure in alternation with its symmetry-related atom O2Bxi  (bipy)]·p-xy (TCNQ–TCNQ)]  Å, which is in line with the observed range in the published crystal structures.A search of the CSD (Groom 3)2·6H2O  and bpy  in methanol (2 ml) at the same temperature. The dark-green solution that resulted was immediately enclosed in a 5 ml vial and cooled to room temperature (8.75 K h−1) in a programmable drying oven. The dark-green crystalline solid that resulted was filtered off, washed with a small amount of methanol and ether, and dried in air. The solid was mainly of microcrystalline character, with a few single crystals suitable for X-ray study (yield 63%). IR : 3341 (m), 3382 (m), 3074 (vw), 3033 (vw), 2200 (s), 2175 (vs), 2152ssh, 1598 (m), 1581 (s), 1504 (s), 1471 (m), 1441 (m), 1359 (s), 1182 (m), 1020 (w), 987 (w), 826 (w), 779 (m), 765 (m), 737 (w), 653 (w), 483 (w). CNH : C 65.54/67.00, H 3.87/3.98, N 19.81/19.80.A solution of LiTCNQ  in methanol (2 ml) heated to 323 K was added dropwise to a mixture of Ni2− dianion is positionally disordered  were considered to be exactly one half, while the refined site-occupation factors for atoms O2A and O2B are 0.908 (3) and 0.092 (3), respectively. Some of the water H atoms were resolved in difference maps and all H-atom positions were refined assuming idealized geometric parameters of O—H = 0.85 (1) Å and H⋯H = 1.344 (1) Å. For the H atoms of the O2B water molecule (the least-occupied water molecule), a riding model was used. The Uiso parameters for water H atoms were set at 1.5 times the Ueq value of the parent O atom.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989016019162/zl2686sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989016019162/zl2686Isup2.hklStructure factors: contains datablock(s) I. DOI: 1520298CCDC reference: crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the crystal, complex and DMF solvate molecules build up a one-dimensional hydrogen-bonded polymer along [010].The homoleptic nickel–thiosemicarbazonate complex shows structural features including an unusual  II acetate tetrahydrate with 4-methyl-2-hydrazinecarbothioamide in a 2:1 molar ratio and recrystallization from dimethylformamide yielded the title compound, [Ni(C12H14N3S)2]·C3H7NO. The ligands act as monoanionic κ2N1,S-donors, forming five-membered metallarings. The NiII ion is fourfold coordinated in a distorted square-planar cis-configuration, which is rather uncommon for monothiosemicarbazone complexes. Intramolecular H⋯Ni trans-interactions are observed [H⋯Ni distances are 2.50 and 2.57 Å] and thus anagostic interactions can be suggested. The Hirshfeld surface analysis indicates that the major contributions for the crystal packing are H⋯H (66.6%), H⋯S (12.3%) and H⋯C (10.9%) interactions. In the crystal, the complex molecules are linked by dimethylformamide solvent molecules through N—H⋯O interactions into one-dimensional hydrogen-bonded polymers along [010].The reaction of Ni The hydrazinic H atom can be easily removed and the negative charge is then delocalized over the C—N—N—C—S backbone, which enables chemical bonding with many different metal ions hydrazinecarbothiamide as ligand  Å for C3 and of 0.3685 (15) Å for C15. The two ligands are deprotonated with the negative charge delocalized over the C—N—N—C—S entity, as suggested by their intermediate bond lengths and supported by the sp2-hybridization for C1, C13, N1, C11, C23 and N4. The imine and thioamide C—N distances indicate considerable double-bond character, while the C—S distance is consistent with mainly single-bond character. The change of the bond lengths is a key feature to distinguish free, i.e. non-coordinating, and coordinating thiosemicarbazones. For the title compound these distances  are C1—N1 = 1.306 (2), N1—N2 = 1.408 (2), N2—C11 = 1.307 (2) and C11—S1 = 1.752 (2) for one ligand and C13—N4 = 1.303 (2), N4—N5 = 1.409 (2), N5—C23 = 1.303 (2) and C23—S2 = 1.7573 (19) for the other one.One molecule of the title complex and one dimethylformamide solvate comprise the asymmetric unit. The Nids Fig. 1. The maxcis coordination mode, which is rather uncommon for mono-thiosemicarbazone ligands, as well as two positioned trans H⋯Ni anagostic interactions  −x + 1, y − z + In the crystal, the coordination entities are linked by DMF solvate molecules through N—H⋯O interactions. The DMF-oxygen atoms are hydrogen-bond acceptors, forming a bridging structure between two N—H⋯O arrangements: N6—H6⋯O1 and N3—H3⋯O10] Fig. 3. Additio0] Fig. 3.et al., 2012de (y axis) and di (x axis) values are the closest external and internal distances  from given points on the Hirshfeld surface contacts -4-phenyl-hydrazinecarbothioamidate-κ2N1,S)}nickel(II) monohydrate bis(tetrahydrofurane) solvate  = 1.2Ueq(C and N) for the sp2–hybridized DMF C atom, the aromatic and the secondary C atoms, and for all N atoms, and with Uiso(H) = 1.5Ueq(C) for the methyl C atoms. The bond lengths  are: C—H = 0.99 for –CH2– fragments, C—H = 0.98 for CH3– fragments, C—H = 0.95 for aromatic groups and the sp2-hybridized DMF C atom; N—H = 0.88 for all N atoms.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989017007198/wm5389sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989017007198/wm5389Isup2.hklStructure factors: contains datablock(s) I. DOI: 1550129CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the title benzoylthiourea derivative (MPiCB), the piperidine ring has a chair conformation and its mean plane is inclined to the 4-methoxybenzene ring by 63.0 (3)°. 14H18N2O2S, the piperidine ring has a chair conformation. Its mean plane is twisted with respect to the 4-methoxybenzoyl ring, with a dihedral angle of 63.0 (3)°. The central N—C(=S)—N(H)—C(=O) bridge is twisted with an N—C—N—C torsion angle of 74.8 (6)°. In the crystal, molecules are linked by N—H⋯O and C—H⋯O hydrogen bonds, forming chains along the c-axis direction. Adjacent chains are linked by C—H⋯π interactions, forming layers parallel to the ac plane. The layers are linked by offset π–π interactions [intercentroid distance = 3.927 (3) Å], forming a supramolecular three-dimensional structure.In the title compound, C The central N—C(=S)—N(H)—C(=O) bridge is twisted with an N2—C8—N1—C7 torsion angle of 74.8 (6)°. The methoxy group lies in the plane of the benzene ring, with the C14—O2—C4—C3 torsion angle being 180.0 (4)°.The molecular structure of the title compound, MPiCB, is illustrated in Fig. 1c-axis direction (Table 1ac plane (Table 1Cg⋯Cgi = 3.927 (3) Å; Cg is the centroid of the C1–C6 ring; interplanar distance = 3.517 (2) Å; slippage = 1.747 Å; symmetry code: (i) −x, −y + 2, −z + 2].In the crystal of MPiCB, neighbouring molecules are linked by N—H⋯O and C—H⋯O hydrogen bonds, forming chains along the n Table 1. Adjacene Table 1. The layet al., 2016N-(carbonothioyl)benzamide skeleton gave 37 hits. Two compounds are of particular interest, namely 4-methoxy-N-(pyrrolidin-1-ylcarbonothioyl)benzamide -3,4,5-trimethoxybenzamide benzamide  was added slowly to ammonium thiocyanate (0.01 mol) in acetone and the mixture was stirred for 30 min at room temperature. A white precipitate of ammonium chloride was filtered off and the filtrate was cooled in an ice bath (278–283 K) for about 15 min. A cold solution (278–283 K) of piperidine (0.01 mol) in acetone was added to the benzoyl isothiocyanate and the mixture was left for 3 h at room temperature. A yellowish precipitate was formed, filtered and washed with cold water to give pale-yellow crystals .3) 2900, ν(C=O) 1609, ν(C—Cbenzene) 1460, ν(C—Ostretching) 1327 and v(C=S) 1252 cm−1. The 1H NMR spectrum exhibits the H(N) group at 8.35 Hz, while the 13C NMR signal of the C=S and C=O groups appear at 174.66 and 163.19 Hz, respectively.The infrared spectrum of MPiCB shows the characteristic signals for ν(NH) 3300, ν(O—CHUiso(H) = 1.2Ueq(C).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989017013317/su4162sup1.cifCrystal structure: contains datablock(s) I, Global. DOI: 10.1107/S2056989017013317/su4162Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989017013317/su4162Isup3.cmlSupporting information file. DOI: 1575129CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


II complex molecules are linked by O—H⋯O hydrogen bonds into supramolecular chains propagating along the [110] direction.In the crystal, the title centrosymmetric Zn 8H4NO2)2(C10H14N2O)2(H2O)2], the ZnII cation, located on an inversion centre, is coordinated by two water molecules, two 4-cyanobenzoate (CB) anions and two diethylnicotinamide (DENA) ligands in a distorted N2O4 octahedral geometry. In the molecule, the dihedral angle between the planar carboxylate group and the adjacent benzene ring is 9.50 (14)°, while the benzene and pyridine rings are oriented at a dihedral angle of 56.99 (5)°. The water molecules exhibit both an intramolecular hydrogen bond  and an intermolecular hydrogen bond ; the latter lead to the formation of supramolecular chains propagating along the [110] direction.In the title complex, [Zn(C N,N-diethylnicotinamide (DENA) is an important respiratory stimulant 2(C7H4ClO2)2(H2O)2] 2(C10H14N2O)2(H2O)2]  is one form of niacin. A deficiency of this vitamin leads to loss of copper from the body, known as pellagra disease. Victims of pellagra show unusually high serum and urinary copper levels  and DENA ligands, namely trans-diaquabis(4-cyanobenzoato-κO)biszinc(II), [Zn(DENA)2(CB)2(H2O)2], and report herein its crystal structure.The structure-function–coordination relationships of the arylcarboxylate ion in ZnII atom located on an inversion centre, one 4-cyanobenzoate (CB) ligand, one N,N-diethylnicotinamide (DENA) ligand and one water molecule, all ligands coordinating to the ZnII atom in a monodentate manner  of the two symmetry-related monodentate CB anions and the two symmetry-related water O atoms (O4 and O4i) around the Zn1 atom form a slightly distorted square-planar arrangement, while the slightly distorted octahedral coordination sphere is completed by the two pyridine N atoms (N2 and N2i) of the two symmetry-related monodentate DENA ligands in the axial positions   Å below the planar (O1/O2/C1) carboxylate group. The O—Zn—O and O–Zn—N bond angles range from 87.64 (5) to 92.36 (5)°.In the carboxylate groups, the C—O bonds for coordinating O atoms are 0.0148 (19) Å longer than those of the non-coordinating ones [C1—O1 = 1.2436 (19) Å and C1—O2 = 1.2584 (18) Å], indicating delocalized bonding arrangements rather than localized single and double bonds. The Zn—O bond lengths are 2.1503 (11) Å (for water O atoms) and 2.0842 (10) Å (for benzoate O atoms) and the Zn—N bond length is 2.1501 (11) Å, the Zn—O bond lengths for water oxygen atoms are The dihedral angle between the planar carboxylate group (O1/O2/C1) and the adjacent benzene ring (C2–C7) is 9.50 (14)°, while the benzene and pyridine (N2/C9–C14) rings are oriented at a dihedral angle of 56.99 (5)°.w⋯Oc  hydrogen bonds (Table 1S(6) hydrogen-bonding motifs  hydrogen bonds  in H2O (50 ml) and diethylnicotinamide  in H2O (10 ml) with sodium 4-cyanobenzoate  in H2O (100 ml). The mixture was filtered and set aside to crystallize at ambient temperature for several days, giving translucent intense colourless single crystals.The title compound was prepared by the reaction of ZnSO2O) were located in a difference Fourier map and were refined freely. The C-bound H atoms were positioned geometrically with C—H = 0.93, 0.97 and 0.96 Å, for aromatic, methylene and methyl H atoms, respectively, and constrained to ride on their parent atoms, with Uiso(H) = k × Ueq(C), where k = 1.5 for methyl H atoms and k = 1.2 for aromatic and methylene H atoms.The experimental details including the crystal data, data collection and refinement are summarized in Table 210.1107/S2056989016013815/xu5890sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989016013815/xu5890Isup2.hklStructure factors: contains datablock(s) I. DOI: 1501337CCDC reference: crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the crystal, there are only weak C—H⋯O hydrogen bonds and offset π–π interactions present.The whole molecule of the title diarylcarbonate is generated by mirror symmetry, the mirror bisecting the central benzene ring, and the carbonate groups adopt an  20H14O6, is generated by mirror symmetry, the mirror bisecting the central benzene ring. The carbonate groups adopt an s-cis-s-cis conformation, with torsion angles of 58.7 (2) and 116.32 (15)°. The crystal structure of 1,3-phenylene bis(phenyl carbonate) contains no strong hydrogen bonds, though weak C—H⋯O and offset π–π interactions are observed, forming layers parallel to the ac plane.The whole molecule of the title compound, C We surmise this compound formed through a combination of intermolecular ‘self-alcoholysis’ reactions leading to a carbamate intermediate  structure reported herein was identified as an unexpected side product from the attempted recrystallization of 1- and 116.32 (15)°, respectively. The 1,3-substitution of the central aromatic ring imparts the molecule with a bent or ‘U-shape’ conformation and a significant net dipole moment.The molecular structure of the title compound is shown in Fig. 1a-axis direction are related by glide symmetry and assemble into polar chains  Å, interplanar distance = 3.438 (1) Å, with a slippage of 1.669 Å ; Cg2⋯Cg2iii,iv = 3.822 (1) Å, interplanar distance = 3.398 (1) Å, with a slippage of 1.749 Å , C—O bond lengths fall within 1.310 and 1.387 Å [average: 1.343 (9) Å], and O—C—O angles average 106 (1)°. However, torsion angles about the C—O—C—Carom bonds are extremely variable.A search of the Cambridge Structural Database  was identified in this search, 4,4′-isopropylidenediphenyl-bis(phenylcarbonate) -3-phenylurea was filtered, dried, and recrystallized in assorted organic solvents . Slow evaporation of an ethanolic solution in a 1 dram vial, capped with pierced lids, yielded large colorless plates of 1,3-phenylene bis(phenyl carbonate). Needle-like crystals identified within the same vials corresponded to 1-(m-phenol)-3-phenylurea. The appearance of 1,3-phenylene bis(phenyl carbonate) crystals was not consistent across multiple recrystallization experiments, suggesting that select impurities and/or longer, delayed evaporation methods that favor non-equilibrium products may be needed to obtain this material.Equimolar amounts of 3-aminophenol and phenyl isocyanate were added to benzene under nitrogen and stirred for 24 h. A white precipitate identified as 1-(Uiso(H) = 1.2Ueq(C).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989017016772/su5407sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989017016772/su5407Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989017016772/su5407Isup3.cmlSupporting information file. DOI: 1586885CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Intramolecular amine-N—H⋯N(imine) and hydroxy-O—H⋯O(methoxy) hydrogen bonds are noted. In the molecular packing, amide-N—H⋯O(amide), hydroxyl-O—H⋯N(imine) and phenylamine-N—H⋯O(methoxy) hydrogen bonding leads to layers in the  A and B) comprise the asymmetric unit of the title compound, C18H21N3O3. The urea moiety is disubstituted with one amine being linked to a phenyl ring, which is twisted out of the plane of the CN2O urea core [dihedral angles = 25.57 (11) (A) and 29.13 (10)° (B)]. The second amine is connected to an imine (E conformation), which is linked in turn to an ethane bridge that links a disubstituted benzene ring. Intramolecular amine-N—H⋯N(imine) and hydroxyl-O—H⋯O(methoxy) hydrogen bonds close S(5) loops in each case. The molecules have twisted conformations with the dihedral angles between the outer rings being 38.64 (81) (A) and 48.55 (7)° (B). In the crystal, amide-N—H⋯O(amide) hydrogen bonds link the molecules A and B via an eight-membered {⋯HNCO}2 synthon. Further associations between molecules, leading to supramolecular layers in the ac plane, are hydrogen bonds of the type hydroxyl-O—H⋯N(imine) and phenylamine-N—H⋯O(methoxy). Connections between layers, leading to a three-dimensional architecture, comprise benzene-C—H⋯O(hydroxy) interactions. A detailed analysis of the calculated Hirshfeld surfaces shows molecules A and B participate in very similar intermolecular interactions and that any variations relate to conformational differences between the molecules.Two independent molecules ( They have attracted considerable attention due to their wide spectrum of biological activities, including anti-convulsant B]. The phenyl ring is inclined to this plane, forming a dihedral angle of 25.57 (11)° [29.13 (10)° for molecule B]. Intramolecular N—H⋯N hydrogen bonds are found within the urea residues, Table 1B]. As a result, the molecule is twisted with the terminal rings inclined to each other, forming a (C2–C7)/(C11–C16) dihedral angle of 38.64 (8)° [(C20–C25)/(C29–C34) = 48.55 (7)° for B]. The latter represents the major difference between molecules A and B, as illustrated in the overlay diagram shown in Fig. 2E in each molecule. Finally, each of the methoxy substituents is twisted out of the plane of the ring to which it is bonded [C18—O2—C13—C12 = 11.7 (3) and C36—O5—C31—C30 = −16.5 (3)°].Two independent molecules, a. The two molecules comprising the asymmetric unit associate via an eight-membered amide synthon, {⋯OCNH}2. The hydroxy-O—H groups at each end of the dimeric aggregate hydrogen bond to an imine-N atom of the other independent molecule. The hydroxyl-O3—H⋯N6(imine) interaction is incorporated within a 10-membered {⋯HOC2O⋯HNCNN} heterosynthon owing to the formation of a relatively weak phenylamine-N4—H⋯O2(methoxy) hydrogen bond. The putative phenylamine-N1—H⋯O5(methoxy) hydrogen bond is beyond the standard limits . The most obvious connections between the supramolecular layers are of the type benzene-C—H⋯O(hydroxyl), which occur between centrosymmetrically related O6-benzene rings. A view of the unit-cell contents highlighting the stacking of layers is shown in Fig. 3c. Other C—H⋯O and several C—H⋯π interactions occur in the crystal but within the layers stabilized by hydrogen bonding. These and other weak interactions are discussed in more detail in Analysis of the Hirshfeld surface i.e. molecules A and B, and for overall (I)et al., 2017The Hirshfeld surface was calculated for the individual O1- and O4-molecules in (I)O and H6O, and imine-N3 and N6 atoms on the Hirshfeld surfaces mapped over dnorm shown with labels ‘1’ and ‘2’ in Fig. 4N and H5N, and amide-O1 and O4 atoms, i.e. ‘3’ and ‘4’ in Fig. 4dnorm-mapped Hirshfeld surfaces with labels ‘5–7’ in Fig. 4The bright-red spots appearing near the hydroxyl-H3a and C24 in Fig. 4b, of the independent molecules, respectively, reflect short interatomic edge-to-edge C⋯C contacts, Table 2i.e. 0.1%, to the Hirshfeld surface owing to the absence of π–π stacking between aromatic rings in the crystal, Table 3A, H18A, C28, C6, C33 and C24 atoms in the images of Fig. 4A and H18B atoms, Fig. 4a, and O5, C35, H22 and H36C atoms, Fig. 4b, indicate the contributions from the additional short interatomic C⋯H/H⋯C and O⋯H/H⋯O contacts, Table 2The presence of diminutive red spots viewed near phenyl atoms C6 in Fig. 4On the Hirshfeld surfaces mapped over the electrostatic potential for the independent molecules of (I)et al., 2007i.e. the twisting of the methoxy substituents on the respective benzene rings and the inclination of these benzene rings with respect to the ethane bridges.It is clear from the overall two-dimensional fingerprint plots for each independent molecule and for the entire asymmetric unit of (I)A and B have almost the same percentage contribution to their respective Hirshfeld surfaces, Table 3A and B. The single short peaks at de + di ∼ 2.1 Å in the delineated plots for both the molecules indicate the involvement of hydrogen atoms of both in short interatomic H⋯H contacts, Table 2de + di ∼ 2.0 Å (inner region) and at ∼ 2.2 Å (outer region) in the fingerprint plots delineated into O⋯H/H⋯O and N⋯H/H⋯N contacts, respectively. The forceps-like distribution of points linked with the donor spike for molecule A and the acceptor spike for molecule B at de + di ∼ 2.5 Å in the fingerprint plots delineated into O⋯H/H⋯O contacts are due to weak intermolecular C—H⋯O interactions and the short interatomic contacts summarized in Table 2de + di ∼ 2.6 Å in the acceptor and donor regions of fingerprint plots delineated into C⋯H/H⋯C contacts for molecules A and B, respectively, represent the involvement of these atoms in the short interatomic C⋯H/H⋯C contacts, Table 2de + di ∼ 2.7 Å in the donor and acceptor regions of molecules A and B, respectively. The other C⋯O/O⋯C, O⋯O and C⋯C interatomic contacts summarized in Table 3The fingerprint plot delineated into H⋯H contacts for molecules et al., 2016et al., 1980et al., 1980et al., 2011et al., 2014et al., 2014There are no direct precedents for the structure of (I)in vacuo; yield: 75%. Light-yellow prisms of (I)v/v 20 ml). IR (cm−1): 3201 ν(N—H), 1670 ν(C=N), 1213 ν(C—N), 1026 ν(C=O). MS m/z: 327.25 [M+1]+Analytical grade reagents were used as procured without further purification. 4-Phenylsemicarbazide  and vanillylacetone  were dissolved separately in hot absolute ethanol (30 ml) and mixed with stirring. The reaction mixture was heated and stirred for 20 min., then stirred for another 30 min. at room temperature. The resulting white precipitate was filtered off, washed with cold absolute ethanol and dried Uiso(H) set to 1.2–1.5Ueq(C). The oxygen- and nitrogen-bound H atoms were located in a difference-Fourier map but were refined with distance restraints of O—H = 0.84±0.01 Å and N—H = 0.88±0.01 Å, and with Uiso(H) set to 1.5Ueq(O) and 1.2Ueq(N), respectively. The maximum and minimum residual electron density peaks of 0.60 and 0.26 e Å−3, respectively, were located 0.95 and 0.75 Å from atoms H10A and H36A, respectively.Crystal data, data collection and structure refinement details are summarized in Table 410.1107/S2056989017017273/hb7720sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989017017273/hb7720Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989017017273/hb7720Isup3.cmlSupporting information file. DOI: 926756CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Scientific Reports6: Article number: 3657910.1038/srep36579; published online: 11152016; updated: 05042017This Article contains errors. In the legend of Figure 1,−1”“1.25 cGy minshould read:−1”.“1.25 Gy minIn addition, in the Methods section under subheading ‘Animals and Radiation Exposure’,−1”“For serial tissue analysis, age and sex-matched C57BL/6J and C57L/J mice at 10–12 weeks of age were irradiated to the whole lung with a single dose of 15 Gy of 320 kVp X-rays at a dose rate of 1.25 cGy minshould read:−1”“For serial tissue analysis, age and sex-matched C57BL/6J and C57L/J mice at 10–12 weeks of age were irradiated to the whole lung with a single dose of 15 Gy of 320 kVp X-rays at a dose rate of 1.25 Gy min


In the crystal, N+(C)—H⋯Cl− hydrogen bonds and π–π stacking interactions lead to the formation of a three-dimensional supramolecular network.The title salt, C 18H26N42+·2Cl−, was obtained by the protonation of N,N-bis(pyridin-4-ylmethyl)cyclohexane-1,4-diamine with hydrochloric acid in ethanol. The asymmetric unit consists of one half of an N,N-bis(pyridin-3-ylmethyl)cyclohexane-1,4-diammonium dication, with a crystallographic inversion centre located at the centre of the cyclohexyl ring, and a chloride anion. The central cyclohexyl ring in the dication adopts a chair conformation. The two trans-(4-pyridine)–CH2–NH2– moieties at the 1- and 4-positions of the central cyclohexyl ring occupy equatorial sites. The terminal pyridine ring is tilted by 53.72 (6)° with respect to the mean plane of the central cyclohexyl ring (r.m.s. deviation = 0.2413 Å). In the crystal, N+—H⋯Cl− hydrogen bonds between the dications and the chloride anions, and π–π stacking interactions between the pyridine rings of the dications afford a two-dimensional sheet extending parallel to the ab plane. These sheets are further connected through weak C—H⋯Cl− hydrogen bonds, resulting in the formation of a three-dimensional supramolecular network.The title salt, C In the dication, the central cyclohexyl ring displays a chair conformation and the two trans-(4-pyridine)–CH2–NH2– moieties occupy equatorial sites at the 1- and 4-positions of the central cyclohexyl ring. The terminal pyridine ring is tilted by 53.72 (6)° with respect to the mean plane of the cyclohexyl ring (r.m.s. deviation = 0.2413 Å). This tilting angle is larger than that [27.98 (5)°] of the similar dication with 4-pyridine rings as the terminal groups  Å] between the pyridine rings cyclohexane-1,4-diaminium)cobalt(II) pentanitrate methanol solvate] cyclohexane-1,4-diamine, prepared according to a literature method  = 0.95 Å for Csp2—H, 0.99 Å for methylene, 1.00 Å for methine H atoms] and were refined as riding with Uiso(H) = 1.2Ueq(C). The N-bound H atoms involved in hydrogen bonds were located in difference Fourier maps and refined freely [N—H = 0.891 (15) and 0.876 (16) Å].Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989016017205/hg5479sup1.cifCrystal structure: contains datablock(s) I, New_Global_Publ_Block. DOI: 10.1107/S2056989016017205/hg5479Isup2.hklStructure factors: contains datablock(s) I. DOI: 1511616CCDC reference: crystallographic information; 3D view; checkCIF reportAdditional supporting information:


ATP‐sensitive P2X7 receptor activates the NLRP3 inflammasome and is a key component of the innate immune system. We used a fluid‐resuscitated rat model of fecal peritonitis and acute kidney injury (AKI) to investigate the contribution of this purinergic receptor to renal dysfunction in sepsis. Six and 24 h time‐points were chosen to represent early and established sepsis, respectively. A selective P2X7 receptor antagonist (A‐438079) dissolved in dimethyl sulfoxide (DMSO) was infused 2 h following induction of sepsis. Compared with sham‐operated animals, septic animals had significant increases in heart rate (−1(−4 to 8)% vs. 21(12–26)%; P = 0.003), fever (37.4(37.2–37.6)°C vs. 38.6(38.2–39.0)°C; P = 0.0009), and falls in serum albumin (29(27–30)g/L vs. 26(24–28); P = 0.0242). Serum IL‐1β (0(0–10)(pg/mL) vs. 1671(1445–33778)(pg/mL); P < 0.001) and renal IL‐1β (86(50–102)pg/mg protein vs. 200 (147–248)pg/mg protein; P = 0.0031) were significantly elevated in septic compared with sham‐operated animals at 6 h. Serum creatinine was elevated in septic animals compared with sham‐operated animals at 24 h (23(22–25) μmol/L vs. 28 (25–30)μmol/L; P = 0.0321). Renal IL‐1β levels were significantly lower in A‐438079‐treated animals compared with untreated animals at 6 h (70(55–128)pg/mg protein vs. 200(147–248)pg/mg protein; P = 0.021). At 24 h, compared with untreated animals, A‐438079‐treated animals had more rapid resolution of tachycardia (22(13–36)% vs. −1(−6 to 7)%; P = 0.019) and fever (39.0(38.6–39.1)°C vs. 38.2(37.6–38.7)°C; P < 0.024), higher serum albumin (23(21–25)g/L vs. (27(25–28)g/L); P = 0.006), lower arterial lactate (3.2(2.5–4.3)mmol/L vs. 1.4(0.9–1.8)mmol/L; P = 0.037), and lower serum creatinine concentrations (28(25–30)μmol/L vs. 22(17–27)μmol/L; P = 0.019). P2X7A treatment ameliorates the systemic inflammatory response and renal dysfunction in this clinically relevant model of sepsis‐related AKI.Sepsis is a major clinical problem associated with significant organ dysfunction and high mortality. The  Sepsis is a common and serious global health issue, accounting for 20% of all admissions to intensive care units (ICU), and is the leading cause of death in noncardiac ICUs  mice subjected to cecal ligation and puncture have an attenuated inflammatory response and reduced lung injury compared with wild‐type mice  , P2X7 receptor contributes to renal injury in sepsis through an inflammatory response with local production of cytokines. We aimed to define the expression of this receptor within the kidney, and its relationship with cytokine production, and renal function; we sought to assess effects of P2X7 antagonism in a rat model of sepsis‐induced AKI. The primary objective of this study was to evaluate the effect of a selective P2X7 antagonist (A‐438079) in preventing renal dysfunction (as defined by an elevated serum creatinine) in an experimental model of sepsis.We hypothesized that upregulation of the ATP‐sensitive P2XAll animal experiments were performed under a Home Office Project License (PPL 70/7029) and local UCL Ethics Committee approval.7 receptor antagonist (A‐438079) dissolved in DMSO. Details on monocyte isolation from male Wistar rats are detailed in the supplementary data. Monocytes require priming with LPS  prior to release of IL‐1β by co‐stimulation with ATP . The duration of LPS‐priming is variable, although 4 h has been shown to be adequate   was kindly donated by Abbvie . Based on previously published data and personal communication with Abbvie, the pharmacokinetic profile of A‐438079 was determined. A‐438079 blocked BzATP (10 μmol/L)–mediated changes in intracellular Ca++ concentrations at rat P2X7 receptors but not at other P2 receptors  would achieve therapeutic levels in serum. We therefore administered a dose of 10 μg/kg. The antagonist was given as a single bolus to achieve a peak (therapeutic) concentration, followed by 4× the dose  for the first half‐life, followed by 2× the dose for the second half life, followed by 10 μg/(kg·h) thereafter.Unpublished data from Abbvie Pharmaceuticals demonstrates that the half‐life of intravenous A‐438079 is 0.69 h (41 min). An intravenous dose of 10 μmol/L, the pH at room temperature fell to 2.2, and at 38°C was 1.6. Dimethylsulfoxide (DMSO) was therefore selected as a drug solvent. Due to its amphipathic properties, DMSO is an effective solvent for water‐insoluble compounds and is a hydrogen‐bound disrupter. As such it is a commonly used solvent for many drugs in pharmacological studies. This is a commonly used drug solvent, however, itself has biological activity  weighing 300–375 g were used throughout. All experiments were performed in accordance with relevant guidelines and regulations and are detailed in the supplementary data and our characterization manuscript  initially comprised sham‐operated and untreated septic animals at both 6 h and 24 h time points, and DMSO ± A‐438079 treatment at 6 h and 24 h. On review of the results, we undertook further studies where twice the dose of A‐438079 was administered.Experimental groups .DuoSet ELISA kits  were used according to the manufacturer's instructions. The antibody supplied in the IL‐1β in sham and septic animals at 24 h. Details of methods for Western blot are included in the supplementary data.Protein was extracted and estimated from whole kidney tissue. Four animals were randomly selected from each of the sham and sepsis groups, for analysis. Kidney homogenate were assessed for expression of Caspase‐1, and IL‐1The number of antagonist‐treated animals and placebo‐treated controls was calculated based on previous laboratory experience. We regarded a 20% change in a tested variable as an important biological effect. The study was designed to have a power of 90% and a significance level of 5%. At least 6 replicate animals per group per time point.U test was used for comparison of continuous variables between 2 groups. A P < 0.05 was taken as statistically significant.Graphpad Prism  was used for statistical analyses and graphs. All data were regarded as nonparametric due to small sample sizes (6–12 per group). Continuous variables are presented as median (interquartile range). Data were analyzed in prospectively defined groups. All 6 h experiments were analyzed as a predefined group, as were all 24 h experiments. For comparison of continuous variables between more than two groups, Kruskal–Wallis test with post hoc Dunn's test is used. Mann–Whitney β production (P = 0.029). Addition of 2% DMSO significantly inhibited the release of IL‐1β (P = 0.025). Addition of 10 μmol/L A‐438079 had no added effect on the reduction in IL‐1β release. 5 μmol/L brilliant blue G (BBG) had a significant inhibitory effect on monocyte IL‐1β release (P = 0.029)  stimulation of cultured monocytes resulted in significant IL‐1P = 0.003), fever (37.4(37.2–37.6)°C vs. 38.6(38.2–39.0)°C; P = 0.0009), and falls in serum albumin (29(27–30)g/L vs. 26(24–28); P = 0.0242). Serum IL‐1β (0(0–10)(pg/mL) vs. 1671(1445–33778)(pg/mL); P < 0.001) and renal IL‐1β (86(50–102)pg/mg protein vs. 200 (147–248)pg/mg protein; P = 0.0031) were significantly elevated in septic compared with sham‐operated animals at 6 h. Serum creatinine, however, remained unchanged at 6 h (25(23–27)μmol/L vs. 23(21–28) μmol/L; P = 0.9155) in sham‐operated compared with septic animals.Clinical, biochemical, and cytokine changes in the septic model are detailed in our characterization manuscript , fever (37.5(37.4–37.8)°C vs. 39.0(38.6–39.1)°C; P = 0.0002), and fall in serum albumin (30(29–31)g/L vs. 23(21–25)g/L; P = 0.0003). Serum IL‐1β (0(0–10)(pg/mL) vs. 1463(927–2541)(pg/mL); P < 0.001) remains significantly elevated in septic compared with sham‐operated animals at 24 h although renal IL‐1 β levels were similar (168(154–176)pg/mg protein vs. 186(149–280)pg/mg protein; P = 0.053). Serum creatinine was significantly elevated in septic animals compared with sham‐operated animals at 24 h (23(22–25)μmol/L vs. 28 (25–30)μmol/L; P = 0.0321).At 24 h, septic animals had persistent changes of systemic inflammation Table , Fig. 2.7 on immunohistochemistry: there was minimal constitutive P2X7 expression limited to distal tubular epithelial cells   protein expression in septic animals compared with sham‐operated animals  vs. 1.35(1.25–1.37); μmol/L did not result in any clinical or biochemical differences between untreated and A‐438079‐treated septic animals (data not shown). We therefore undertook further studies where twice the dose of A‐438079 was administered.Initial in vivo experiments targeting a peak concentration of 3 β and between treated and untreated animals pg/mg protein vs. 200(147–248)pg/mg protein; P = 0.021). Arterial lactate concentration was different between DMSO‐treated and untreated animals (1.0 (0.9–1.0)mmol/L vs. 1.2(1.0–1.3)mmol/L; P = 0.033), although remained within the normal clinical range in all groups of animals.At 6 h there was no difference among the groups in core temperature, change in heart rate, serum creatinine, or serum IL‐1ls Table . Renal IP = 0.019) and fever (39.0(38.6–39.1)°C vs. 38.2(37.6–38.7)°C; P < 0.024), higher serum albumin (23(21–25)g/L vs. (27(25–28)g/L); P = 0.006), lower arterial lactate (3.2(2.5–4.3)mmol/L vs. 1.4(0.9–1.8)mmol/L; P = 0.037), and lower serum creatinine concentrations (28(25–30)μmol/L vs. 22(17–27)μmol/L; P = 0.019).At 24 h, there were a number of significant differences between A‐438079 treated animals and untreated septic animals Table , Fig. 2.P = 0.016), and lower arterial lactate (2.2 (2.1–2.2)mmol/L vs. 1.4(0.9–1.8)mmol/L; P = 0.001). Serum IL‐1β and renal IL‐1β were similar in A‐438079‐treated, DMSO‐treated, and untreated animals at 24 h.At 24 h, compared with DMSO‐treated animals, A‐438079‐treated animals had higher serum albumin (24(22–25)g/L vs. 27(25–28)g/L; 7 and IL‐1β, are expressed de novo within the renal tubular epithelial cells in this septic model. This is consistent with published data showing that LPS‐primed Madin–Darby canine kidney (MDCK) renal tubular epithelial cells express Toll‐like receptor 4, NLRP3, caspase‐1, and IL‐1β mRNA , though P2X7 activation accelerates mature IL‐1β release from monocytes  levels of IL‐1β ‐producing Escherichia coli had markedly lower survival, higher cytokine levels (including IL‐1β), and activated intravascular coagulation compared with wildtype mice  transplanted with wild‐type kidneys were protected from LPS‐induced AKI, whereas wild‐type mice transplanted with C3H/HeJ kidneys developed severe LPS‐induced AKI. This suggests that TLR4 expression in circulating cells propagates injury in septic AKI, rather than intra‐renal TLR4 , with better perfusion to organs including the kidney, rather than specific actions over the renal‐inflammasome activation.The changes found in animals treated with the P2Xβ measurement, which does not allow localization to specific cell types. Immunohistochemistry would enable localization of these cytokines. Although insights into renal expression of the inflammasome and P2X7 in sepsis have been demonstrated, the expression of the P2X7 in other organs and on immune cells also needs to be evaluated.ELISAs were performed on whole kidney homogenate for IL‐β and tubular cell P2X7 expression by 6 h and 24 h, respectively. Treatment with A‐438079 after the onset of sepsis abrogated the rise in serum creatinine at 24 h with reduced renal IL‐1β expression early. In addition, A‐438079 treatment reduced fever, improved resolution of tachycardia, increased serum albumin concentration and reduced lactate at 24 h. Given these encouraging results in an in vivo model of sepsis that is relevant to human disease, further studies targeting P2X7 in sepsis are warranted.We demonstrate a number of strengths of our experimental model relevant to potential therapeutics in sepsis. Sepsis is associated with an increase in renal IL‐1All animal experiments were performed under a Home Office Project License (PPL 70/7029) and local University College London Ethics Committee approval.7 antagonist (A‐438079). FWKT has received research project grants from AstraZeneca Limited, Baxter Biosciences, Boehringer Ingelheim, and MedImmune. He has consultancy agreements with Rigel Pharmaceuticals, Novartis and Baxter Biosciences.Materials: Abbvie pharmaceuticals  have provided the selective P2XData S1. Supplementary data.Click here for additional data file.


Scientific Reports6: Article number: 18631; 10.1038/srep18631 published online: 01112016; updated: 09012016.In this Article and Supplementary Information file, some instances of ‘0.001M PBS’ and ‘0.01M PBS’ are incorrectly written as ‘0.01M PBS’ and ‘0.1M PBS’ respectively. With the exception of the following:In the Materials and Methods section, under subheading ‘Specimen Preparation’,“Fixed samples were incubated in A4P0 hydrogel monomer solution (4% acrylamide in 0.1 M PBS) supplemented with 0.25% of the photoinitiator 2,2′-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride  overnight at 4 °C”.should read:“Fixed samples were incubated in A4P0 hydrogel monomer solution (4% acrylamide in 0.001 M PBS) supplemented with 0.25% of the photoinitiator 2,2′-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride  overnight at 4 °C”.Under subheading ‘ACT Reagents’,A4P0 solution, Forty ml of 40% acrylamide was added to 360 ml dH2O to prepare 400 ml of the hydrogel monomer solution (A4P0)”.“should read:A4P0 solution, Forty ml of 40% acrylamide was added to 360 ml 0.001M PBS to prepare 400 ml of the hydrogel monomer solution (A4P0)”.“Under subheading ‘Whole-body and Organ ACT Protocol,“Higher sodium concentrations in the clearing solution (0.03 M and 0.1 M PBS) ameliorated tissue swelling but resulted in tissue thinning (data not shown)”.should read:“Higher sodium concentrations in the clearing solution (0.003 M and 0.01 M PBS) ameliorated tissue swelling but resulted in tissue thinning (data not shown)”.“The head was freed from subcutaneous skin and hair and washed several times with 0.1 M PBS.should read:“The head was freed from subcutaneous skin and hair and washed several times with 0.001 M PBS”.In the Supplementary Information file, under subheading ‘’Hydrogel monomer infusion & polymerization,“1. Prepare the A4P0 hydrogel monomer solution.Take 40 ml of 4% acrylamide in 0.1 M PBS solution and add 100 mg of VA-044 Initiator to make a final concentration of 0.25%”.should read:“1. Prepare the A4P0 hydrogel monomer solution.Take 40 ml of 4% acrylamide in 0.001 M PBS solution and add 100 mg of VA-044 Initiator to make a final concentration of 0.25%”.Under the subheading ‘Immunolabeling ACT-processed brain tissue’,“1. Wash samples in 0.1 M PBS for 3–5 hours and change the buffer every hour”.should read:“1. Wash samples in 0.001 M PBS for 3–5 hours and change the buffer every hour”.“3. Wash samples in 0.1 M PBS for 3–5 hours, and change buffer every hour”.should read:“3. Wash samples in 0.001 M PBS for 3–5 hours, and change buffer every hour”.


The title salt forms a racemate due to disorder of the hydroxy group [occupancy ratio 0.738 (3):0.262 (3)] at the stereogenic C atom. 13H22NO3+·C7H5O2−, comprises one salbutamol cation {systematic name: 4-[2-(tert-butylazaniumyl)-1-hydroxyethyl]-2-(hydroxymethyl)phenol} and a benzoate anion. The cation shows disorder of the hydroxy group [occupancy ratio 0.738 (3):0.262 (3)] at the stereogenic C atom. The non-planar benzoate anion [the dihedral angle between the benzene ring and the carboxyl group is 11.30 (8)°] is linked to the salbutamol cation by a medium-strength O—H⋯O hydrogen bond. Other intermolecular O—H⋯O and N—H⋯O hydrogen bonds of weaker nature give rise to [001] chains.The title salt, C The bond lengths of the carboxylate group of the BA− anion, C20—O4 and C20—O5, are 1.2617 (15) and 1.2604 (15) Å, respectively. The slight difference may be caused by the role of O4 as an acceptor atom of the O3—H3⋯O4 hydrogen bond with one of the hydroxy groups of +SAL. The +SAL cation also has an intramolecular hydrogen bond between the two hydroxy functions (O1—H1⋯O3), forming an S(6) ring motif °. There is some disorder at the stereogenic centre (C8) of the +SAL cation, but the space group is centrosymmetric and the +SAL cation is racemic.The +SAL cation is connected to the −BA anion via a medium-strength O3—H3⋯O4 hydrogen bond  was determined  and benzoic acid  were added to 10 ml methanol and stirred for 3 h. The solvent was then evaporated at room temperature to yield salbutamol benzoate. After recrystallization from water, pure crystals were again dissolved in ethanol and the solution filtered. The neat filtrate was evaporated slowly to give colourless block-like single crystals of salbutamol benzoate.Uiso(H) = 1.5Ueq(C) for methyl H atoms and Uiso(H) = 1.2Ueq(C) for all other H atoms. The H atoms of the NH2 group and the hydroxy group  were also constrained to ideal values and allowed to ride in the refinement, with Uiso(H) = 1.2Ueq(N) and 1.5Ueq(O).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989017011513/wm5403sup1.cifCrystal structure: contains datablock(s) I, New_Global_Publ_Block. DOI: 10.1107/S2056989017011513/wm5403Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989017011513/wm5403Isup3.cmlSupporting information file. DOI: 1482124CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The chemical modifications in terms of changes in substituents in the title compounds have not affected the type nor strength of two defining intermolecular interactions present in both crystal structures. 28H26N2O2, (I), and C27H22BrClN2O2, (II), differ in their substituents, viz.4-methylphenyl and benzoyl rings in (I) replaced by 2-chlorophenyl and 4- bromobenzoyl, respectively, in (II). A significant difference between the two molecules is found in the deviation of the benzoyl O atom from the least-squares plane of the ring to which it is attached , a fact which may be attributed to the different participation of the benzoyl O atoms as acceptors in their intermolecular C—H⋯O interactions. The chemical modifications in (I) and (II) do not seem to affect the type nor strength of the intermolecular N—H⋯N and C—H⋯O hydrogen bonds responsible for the two crystal structures, such that the aggregation of molecules appears similar in spite of the molecular changes.The two title compounds, C Indole, a pharmacologically significant nucleus, is known for anti-inflammatory viz. N2–C9–C10–C11–C12 and N2–C2–C14–C13–C12 are, respectively, Q = 0.362 (4) Å, φ = 264.4 (5)° indicating a twist about C10–C11, and Q = 0.408 (3) Å, φ=67.9 (4)° conforming to an envelope on C14. The corresponding values in (II)Q = 0.378 (3) Å, φ = 82.4 (4)° and Q = 0.423 (3) Å, φ = 251.4 (3)°, may differ slightly from those in (I)Q of the fused eight-membered pyrrolizine and the nine-membered indolone ring systems are respectively, 0.727 (3) and 0.129 (3) Å in (I)Molecular diagrams of (I)In both compounds, the spiro-fused ring systems tend to be rigid by remaining nearly perpendicular to each other, whereas the remaining substituted rings appear to be more ‘compromising’ towards hydrogen-bonding requirements, irrespective of their intra- or intermolecular nature. As an example, the free rotation of the benzoyl group in (II)A significant difference between the two structures is observed in the deviation of benzoyl atom O2 from the least-squares plane of the C15–C21 atoms: 0.593 (4) in (I)etc, these molecular modifications do not seem to affect the type nor strength of the two relevant N—H⋯N and C—H⋯O intermolecular hydrogen bonds defining the crystal structures (Tables 1x + y − z + dO⋯Br= 3.192 (2) Å] is present in structure (II)Even if the differences in the substituents produce differences in lattice types, space group, cell metrics,  Tables 1 and 2 ▸,et al., 2016et al., 1998A search of the Cambridge Structural Database -1-phenyl-3-(p-tolyl)prop-2-en-1-one (0.4 mmol) [for the synthesis of (II)E)-1-(4-bromophenyl)-3-(2-chlorophenyl)prop-2-en-1-one (0.4 mmol)], isatin (0.4 mmol) and l-proline (0.4 mmol), which was dissolved in 5 ml of methanol, and 1 mol% of CMPTC  was added and stirred at reflux temperature until the completion of reaction as indicated by TLC. After this step, the mixture was poured onto ice; the precipitate was filtered and recrystallized from ethanol solution, to get the pure product without column chromatography.The synthesis of (I)Uiso(H) set at 1.2–1.5Ueq(C). Compound (I)Crystal data, data collection and structure refinement details are summarized in Table 310.1107/S2056989016016741/bg2594sup1.cifCrystal structure: contains datablock(s) I, II, c1. DOI: 1503430, 1503429CCDC references: crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The ethyleneglycol ligand forms a non-planar metallacyclic ring by chelating the Ru atom via the O atoms. The O⋯O distances of 2.554 (2) and 2.568 (2) Å are indicative of hydrogen bonding between coordinated ethyleneglycol and outer-sphere trifluoromethanesulfonate fragments. The crystal packing is stabilized by ionic forces and several CH3⋯·F (2.585 and 2.640 Å) and CH3⋯O interactions  between the pentamethylcyclopentadienyl ligand and trifluoromethanesulfonate anion. There is noticeable short intermolecular contact [2.9039 (16) Å], between an O atom of the SO3 group and a C atom of the pentamethylcyclopentadienyl ligand.The title compound, [Ru(C DOI: 10.1107/S1600536807067426/bg2160Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


II complex, [Cu2(C8H7O2)4(C9H7N)2], the two Cu cations are bridged by four carboxylate groups of the phenylacetate anions; each Cu cation is further coordinated by an isoquinoline ligand to complete the distorted CuO4N square-pyramidal geometry. The Cu cation is displaced by 0.2092 (8) Å from the basal plane formed by the four O atoms. Within the dinuclear molecule, the Cu⋯Cu separation is 2.6453 (6) Å. Although a parallel, overlapped arrangement of isoquinoline ligands exists in the crystal structure; the longer face-to-face distance of 3.667 (5) Å suggests there is no π–π stacking between isoquinoline ring systems.In the title centrosymmetric binuclear Cu DOI: 10.1107/S1600536809048697/ng2685Isup2.hklStructure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


In the cation, the FeCo2 triangle is symmetrically capped on one face by an S atom and on the other by a C atom linked to a methyl trithiocarbonate residue that bridges the Fe—C bond. Each Co atom carries a cyclopentadienyl ligand while the Fe atom coordinates to one carbonyl and one triphenylphosphine ligand. In the crystal structure, the cation is linked to the anion by a number of weak non-classical C—H⋯O and C—H⋯F hydrogen bonds and weak S⋯O (3.317 Å) and S⋯F (3.198 Å) interactions. The structure is further stabilized by additional intermolecular C—H⋯O, C—H⋯F and O⋯O (2.942 Å) contacts, together with an unusual S⋯π(Cp) interaction (S⋯centroid distance = 3.385 Å), generating an extended network.The asymmetric unit of the title compound, [FeCo DOI: 10.1107/S1600536808008970/hb2713Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The initial reactant of CuI was oxidized to CuII. The asymmetric unit contains two independent complex molecules, two I− ions and one water molecule. Each CuII atom is coordinated by two O atoms from a 4-methylbenzoate ligand and four N atoms from two 2,2′-bipyridine ligands, displaying a distorted octahedral geometry. The structure involves O—H⋯I hydrogen bonds between the water molecule and iodide ions and π–π stacking interactions between the benzene and pyridyl rings [centroid–centroid distance = 3.79 (1) Å] and between the pyridyl rings [centroid–centroid distance = 3.87 (1) Å].The title compound, [Cu(C DOI: 10.1107/S1600536808024252/hy2148Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The N and O donor atoms are mutually cis. The dihedral angle between two benzene rings of the ligand is 38.86 (8)°. There are also three solvent water molecules, two of which lie across different crystallographic twofold rotation axes; one of these is partially occupied with a refined occupancy factor of 0.570 (7). The water molecules are linked together as tetramers in R               2               2(8) ring motifs, which also connect two neighbouring molecules of the complex through a network of O—H⋯O hydrogen bonds. The crystal structure is further stabilized by intermolecular C—H⋯O and C—H⋯π interactions, which link neighbouring molecules into extended chains along the b axis. Other interesting features of the crystal structure are the short intermolecular C⋯C [3.204 (3)–3.365 (3) Å] and the C⋯O [3.199 (2)–3.205 (2) Å] contacts which are shorter than the sum of the van der Waals radii of these atoms.In the title complex, [Ni(C DOI: 10.1107/S1600536809014500/sj2621Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the crystal, O—H⋯O hydrogen bonds between the coordinated water molecules and uncoordinated carboxylate O atoms, and weak π–π interactions [centroid–centroid distance = 4.105 (2) Å] between the benzene and pyrazine rings lead to a three-dimensional supramolecular network.In the title compound, [Co(C DOI: 10.1107/S1600536810037906/hy2354Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


A supramolecular network is formed via intermolecular O—H⋯O and C—H⋯O hydrogen-bonding interactions. π–π stacking interactions between neighboring pyridine rings are also present, the centroid—centroid distance being 3.808 (2) Å.In the title complex, [Cu(C DOI: 10.1107/S1600536810035555/pv2323Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Both MnIII centers are in a distorted octahedral geometry with the N2O2 donor atoms of the tetradentate Schiff base dianion in the equatorial plane. The axial positions in the coordination environment of one MnIII complex are occupied by a chloride ion and a water molecule, but a methanol molecule replaces the water molecule in the other complex. The coordinated water molecule takes part in an O—H⋯Cl hydrogen bond between the two MnIII complexes. In the crystal structure, O—H⋯Cl hydrogen bonds link the molecules into infinite one-dimensional chains along the [100] direction. The crystal structure is stabilized by O—H⋯Cl hydrogen bonds together with weak C—H⋯O and C—H⋯Cl interactions. A C—H⋯π interaction is also observed in the crystal structure.The asymmetric unit of the title complex, [Mn(C Cl(H2O)][Mn(C28H30N2O2)Cl(CH4O)] = 0.057                           wR(F                           2) = 0.147                           S = 1.03                           10108 reflections653 parametersH-atom parameters constrainedmax = 0.56 e Å−3                        Δρmin = −0.52 e Å−3                        Δρ                                 APEX2 (Bruker, 2005APEX2; data reduction: SAINT (Bruker, 2005SHELXTL (Sheldrick, 2008SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 2003Data collection: 10.1107/S1600536808006818/sj2472sup1.cif            Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808006818/sj2472Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the anion, the GaIII ion is coordinated by four O atoms [Ga—O = 1.9706 (16)–2.0494 (15) Å] and two N atoms [Ga—N = 1.9660 (18) and 1.9709 (17) Å] from two pydc ligands in a distorted octahedral geometry. The crystal structure exhibits intermolecular O—H⋯O, N—H⋯O and O—H⋯N hydrogen bonds and π–π interactions [centroid–centroid distances of 3.5359 (13) and 3.6550 (14) Å].The asymmetric unit of the title compound, (C DOI: 10.1107/S1600536808029140/cv2438Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The O atoms of two 4-pyridone ligands bridge two symmetrically related AgNO3 units, forming a dimer, with an Ag⋯Ag separation of 3.680 (2) Å. Neighbouring dimers are linked into an infinite chain through weak Ag⋯O interactions [2.765 (2) Å], Ag⋯Ag interactions [3.1511 (4) Å] and π–π stacking interactions [centroid–centroid distance = 3.623 (4) Å]. N—H⋯O and C—H⋯O hydrogen bonds assemble these chains into a three-dimensional network.In the title complex, [Ag(NO DOI: 10.1107/S1600536809019138/hy2199Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Both Ag+ cations show a distorted square-pyramidal coordination. Ag1 is bonded to two water molecules, one L N atom, one N atom and one carboxylate O atom from a neighbouring L, whereas Ag2 is surrounded by two L N atoms, two L carboxylate O atoms and one bridging water molecule. O—H⋯O hydrogen-bonding interactions involving water clusters and carboxylate O atoms link the molecules into a three-dimensional supramolecular architecture, which is further consolidated by weak C—H⋯O interactions and π–π stacking interactions [centroid–centroid distance 3.643 (5) Å].In the title silver(I) coordination polymer, {[Ag DOI: 10.1107/S160053680802984X/kj2095Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the two ligands, the pyridyl rings form dihedral angles of 21.0 (1) and 15.5 (1)°. The crystal packing exhibits an extensive network of O—H⋯O hydrogen bonds and π–π interactions proved by short distances of 3.650 (1) and 3.732 (2) Å between the centroids of pyridyl rings of neighbouring molecules.In the title compound, [Cu(C DOI: 10.1107/S1600536809009453/cv2529Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The crystal packing is stabilized by intermolecular O—H⋯N and O—H⋯O hydrogen bonds. A weak C—H⋯π interaction also occurs.In the title compound, C DOI: 10.1107/S1600536809055391/jj2016Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The OH group of the 2-hydroxybenzoate anion is disordered over two positions with site-occupancy factors of 0.5. The asymmetric unit is completed with by an uncoordinated half-molecule of dmphen, disordered about a crystallographic twofold axis. In the crystal structure, molecules are linked into a two-dimensional framework by O—H⋯N, O—H⋯O and C—H⋯O hydrogen bonds. The packing of the structure is further stabilized by π–π stacking interactions involving dmphen molecules, with centroid–centroid separations of 3.8027 (3) and 3.6319 (3) Å.In the asymmetric unit of the title complex, [Mn(C DOI: 10.1107/S1600536809000981/bh2207Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


There is a weak π–π stacking interaction between symmetry-related triazolyl rings with a centroid–centroid distance of 3.802 (4) Å and a perpendicular distance of 3.413 Å between the rings.In the title complex, [Zn(C DOI: 10.1107/S160053680903877X/bt5062Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Each NiII ion has a distorted square-pyramidal environment, with the basal plane formed by three O [Ni—O = 1.9290 (16)–1.9588 (10) Å] and one N [Ni—N = 1.9828 (18) Å] atoms and the apical position occupied by the water molecule [Ni—O = 2.2643 (11) Å]. The water molecules are involved in the formation of O—H⋯O hydrogen bonds.In the title compound, {[Ni DOI: 10.1107/S1600536808031619/cv2458Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


II compound, [Zn2(C12H9O3)4(H2O)2], is centrosymmetric. Each Zn atom is coordinated by two bridging 2-naphthoxyacetate anions, one terminal 2-naphthoxyacetate anion and one water molecule in a distorted ZnO4 tetrahedral geometry. The naphthalene system of the bridging ligand is nearly perpendicular to the naphthalene of the terminal ligand, with a dihedral angle of 78.26 (6)°. Within the binuclear molecule the Zn⋯Zn separation is 3.815 (5) Å. In the crystal structure, intermolecular O—H⋯O hydrogen bonding between the water molecule and carboxylate groups helps to stabilize the crystal structure.The title binuclear Zn DOI: 10.1107/S1600536809013750/xu2494Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


III compound, [In2(SO4)3(C12H8N2)2(H2O)2]·2H2O, each InIII cation is coordinated by a 1,10-phenanthroline (phen) ligand, a water molecule and three sulfate O atoms in a distorted InN2O4 octahedral geometry. Three sulfate anions bridge two InIII cations, forming the dinuclear entities. O—H⋯O and weak C—H⋯O hydrogen bonding is observed in the crystal structure. The crystal structure is further consolidated by π–π stacking between nearly parallel phen ring systems [dihedral angle = 4.2 (4)°], the centroid–centroid distance between benzene rings of adjacent phen ligands being 3.528 (9) Å.In the title dinuclear In DOI: 10.1107/S1600536810036330/xu5026Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The asymmetric unit contains one copper cation to which two acetate units bind asymmetrically; one of the Cu—O distances is rather long [2.740 (2) Å], almost at the limit of coordination. These Cu—O bonds define an equatorial plane to which the Cu—N bonds to the INA ligands are almost perpendicular, the Cu—N vectors subtending angles of 2.4 (1) and 2.3 (1)° to the normal to the plane. The metal coordination geometry can be described as a slightly distorted trigonal bipyramid if the extremely weak Cu—O bond is disregarded, or as a highly distorted square bipyramid if it is not. The double acetate bridge between the copper ions is not coplanar with the CuO4 equatorial planes, the dihedral angle between the (O—C—O)2 and O—Cu—O groups being 34.3 (1)°, resulting in a sofa-like conformation for the 8-member bridging loop. In the crystal, N—H⋯O hydrogen bonds occur, some of which generate a head-to tail-linkage between INA units, giving raise to chains along [101]; the remaining ones make inter-chain contacts, defining a three-dimensional network. There are in addition a number of C—H⋯O bonds involving aromatic H atoms. Probably due to steric hindrance, the aromatic rings are not involved in significant π⋯π interactions.The title centrosymmetric bimetallic complex, [Cu For coo al. 2003. For a c al. 2007.       2(C2H3O2)4(C6H6N2O)4] = 0.039                           wR(F                           2) = 0.099                           S = 1.08                           3736 reflections244 parametersH-atom parameters constrainedmax = 0.36 e Å−3                        Δρmin = −0.43 e Å−3                        Δρ                                 MSC/AFC Diffractometer Control Software  used to solve structure: SHELXS97 (Sheldrick, 2008SHELXL97 (Sheldrick, 2008SHELXTL-NT (Sheldrick, 2008SHELXTL-NT and PLATON (Spek, 2009Data collection: 10.1107/S1600536810004393/hb5326sup1.cif            Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S1600536810004393/hb5326Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The crystal packing is stabilized by intermolecular π–π interactions with centroid–centroid distances 3.572 (1) and 3.671 (1) Å together with C—H⋯Br hydrogen bonds.The title compound, [CdBr DOI: 10.1107/S1600536809020352/sj2628Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Longer Cu⋯O contacts [2.680 (2) Å] complete an approximate square-based pyramidal coordination geometry around CuII, forming a dimeric complex across a centre of inversion. The dimeric complexes form stacks along the a axis, with Cu⋯O contacts of 3.332 (2) Å between them. The Na+ cations and perchlorate anions lie on twofold rotation axes between the stacks. The former are coordinated by two disordered water molecules , and form Na⋯O contacts of 3.698 (3) Å to the perchlorate anions and Na⋯π contacts to neighbouring salicylideneglycinate ligands [shortest Na⋯C = 3.516 (3) Å].In the title compound, [Na(H DOI: 10.1107/S1600536808039561/bi2318Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


N-heterocycle in the title centrosymmetric dinuclear compound, [Ag2(NO3)2(C8H15N3)2], bridges two metal atoms through its imino N atoms. The N—Ag—N skeleton is bent [N—Ag—N = 127.2 (3)°]; as one of two O atoms of the nitrate anion is nearly coplanar with this N—Ag—N skeleton [Ag—O = 2.63 (1) Å], the coordination geometry around the AgI atom is regarded as trigonal-planar. One of the two isopropyl groups is disordered over two positions in respect of the methyl groups in a 1:1 ratio. In the crystal structure, intermolecular N—H⋯O hydrogen bonding is observed between the nitrate groups and triazole ligands.The neutral  DOI: 10.1107/S1600536809028384/xu2560Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The crystal structure is stabilized by intermolecular C—H⋯O and N—H⋯O hydrogen bonds and π–π interactions with a centroid–centroid distance of 3.6136 (16) Å.In the title mononuclear zinc(II) complex, [Zn(C DOI: 10.1107/S1600536809033893/rk2159Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Intermolecular O—H⋯O and O—H⋯N hydrogen bonds link the cations, anions and water molecules into a three-dimensional supramolecular structure. The crystal packing also exhibits intermolecular π–π interactions between the aromatic rings of the anions with a centroid–centroid distance of 3.604 (2) Å.The asymmetric unit of the title compound, [Mg(H DOI: 10.1107/S160053680904344X/cv2632Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The 2-aminoethyl group has a coiled conformation with an N—C—C—NH2 torsion angle of 53.6 (4)°. In the crystal structure, intermolecular N—H⋯N and weak C—H⋯O hydrogen bonds link molecules into chains along [001].In the title compound, C DOI: 10.1107/S160053680901962X/lh2821Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The Zn—Br bond lengths range from 2.400 (2) to 2.408 (3) Å and the Br—Zn—Br angles range from 108.14 (6) to 115.15 (15)°. In the crystal structure, the [ZnBr4]2− anion is connected to two cations through N—H⋯Br and H2C—H⋯Br hydrogen bonds, forming two-dimensional cation–anion–cation layers normal to the b axis. No significant Br⋯Br interactions [the shortest being 4.423 (4) Å] are observed in the structure.In the crystal structure of the title compound, (C DOI: 10.1107/S1600536809015219/at2771Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Edge-to-face C—H⋯π interactions exist between molecules, with a dihedral angle of 37.8 (1)° between the benzene ring planes and a shortest H⋯centroid distance of 3.62 (5) Å.In the title compound, [ZnCl DOI: 10.1107/S1600536808037860/bi2311Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The CuII atoms in each complex adopt a distorted square-pyramidal coordination geometry being pentacoordinated by one N and two O atoms of 4-hydroxypyridine-2,6-dicarboxylate anions and two N atoms of 2,9-dimethyl-1,10-phenanthroline (dmp) molecules. In the crystal structure, there are O—H⋯O and C—H⋯O hydrogen bonds and five π–π stacking interactions with centroid–centroid distances in the range 3.620 (1)–3.712 (1) Å. In addition, a C—H⋯π interaction between a heterocyclic ring of dmp is observed to reinforce the crystal cohesion.In the title complex, [Cu(C DOI: 10.1107/S1600536809021588/pv2164Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


These components are interconnected in the crystal structure by an extensive network of O—H⋯O, N—H⋯O, C—H⋯O, O—H⋯N, O—H⋯Cl, N—H⋯Cl and C—H⋯Cl hydrogen bonds. The shortest intermolecular interaction is realized between the cation and anion . C—H⋯O interactions also play a important role in the interconnection of the cations.The asymmetric unit of the title compound, (C DOI: 10.1107/S160053681000615X/rk2191Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the complex molecule, the two benzimidazole planes are twisted, making a dihedral angle of 55.93 (11)°. The three-dimensional framework is organized by intermolecular N—H⋯O hydrogen bonding and O—H⋯O interactions and π–π interactions between adjacent benzimidazole rings [centroid–centroid distance = 3.586 (3) Å].In the title compound, [Zn(C DOI: 10.1107/S1600536810015631/kp2256Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Intermolecular O—H⋯N interactions link the monomeric units into a two-dimensional hydrogen-bonded  network, which is extended to a three-dimensional supramolecular aggregate via π⋯π stacking interactions [centroid–centroid distances 3.809 (3) and 3.499 (3)  Å].In the molecular structure of the centrosymmetric mononuclear complex [Ni(2-bpt) DOI: 10.1107/S1600536809012598/hg2489Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The crystal structure is stabilized by π–π interactions between the benzene rings of neighbouring molecules [centroid–centroid distance = 3.698 (4) Å], and by C—H⋯π interactions between a methylene H atom of the butyl group and the benzene ring of the benzofuran system. Additionally, the crystal structure exhibits weak intermolecular C—H⋯O contacts. The butyl group is disordered over two positions, with site-occupancy factors, from refinement, of 0.720 (8) and 0.280 (8).In the title compound, C DOI: 10.1107/S1600536808043985/tk2347Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


This compound is composed of an anionic complex, [Cr(pydc)2]−, protonated 4,4′-bipyridine as a counter-ion, +, and four uncoordinated water molecules. The anion is a six-coordinate complex with a distorted octahedral geometry around the CrIII atom, formed by two tridentate pyridine-2,6-dicarboxylate, pydc2−, groups. Intermolecular O—H⋯O, N—H⋯O and C—H⋯O hydrogen bonds, and C—O⋯π stacking interactions (with distances of 3.3390 (13) and 3.4575 (13) Å) connect the various components into a supramolecular structure.The title compound, (C DOI: 10.1107/S1600536808006594/om2216Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The Fe2S2 unit exhibits a butterfly conformation and the ferrocenyldiphenylphosphine ligand is trans to the Fe—Fe bond. The Fe—Fe distance of 2.5160 (8) Å is longer than found in related model structures. Intramolecular C—H⋯S and intermolecular C—H⋯O hydrogen bonds are observed.The title compound, [Fe DOI: 10.1107/S1600536808032698/ci2685Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The water molecules and the 1-(4-chlorophenyl)piperazine-1,4-diium cations interact with the [ZnCl4]2− anions through O—H⋯Cl, N—H⋯Cl, N—H⋯O and C—H⋯Cl hydrogen bonds (five simple and one bifurcated). Intermolecular π–π stacking interactions are present between adjacent aromatic rings of 1-(4-chlorophenyl)piperazine-1,4-diium cations (the centroid–centroid distance is 3.453 Å).In the crystal structure of the title compound, (C DOI: 10.1107/S1600536808016590/bg2190Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Each Au atom is in a square-planar environment coordinated by diphenylphosphanide and 2,6-diphenylpyridine ligands. There are weak π–π stacking interactions between neighbouring molecules (the interplanar separations between two neighbouring dpp units are 3.40 and 3.57 Å). The intramolecular Au⋯Au separation is 3.788 (5) Å. The crystal structure shows weak intermolecular C—H⋯O and C—H⋯N hydrogen bonds involving an O atom of the perchlorate counter-ion and the N atom of the acetonitrile solvent molecule, respectively.The title complex, [Au DOI: 10.1107/S1600536808024537/bx2152Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The structure contains infinite chains of ZnCl2 units connected by the bifunctional thiadiazole ligands, with ZnII adopting a distorted tetrahedral coordination geometry. The dihedral angle between the two pyridyl rings in each ligand is 34.3 (1)°, and the dihedral angles between the thiadiazole ring and the two pyridyl rings are 18.3 (2) and 16.1 (2)°. The shortest Zn⋯Zn distance within each polymeric chain is 11.862 (3) Å, while the shortest interchain Zn⋯Zn distance is 7.057 (3) Å.The title compound, [ZnCl DOI: 10.1107/S1600536808001967/bi2274Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the anion, the S—O bond [1.551 (2) Å] involving the O atom bearing the acid H atom is longer than the other three S—O bonds, which range from 1.437 (1) to 1.454 (1) Å.The crystal structure of the title salt, C DOI: 10.1107/S1600536809048533/xu2677Isup2.hklStructure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


Intramolecular C—H⋯O hydrogen bonds result in the formation of two planar and two non-planar five-membered rings; the latter adopt envelope conformations. There are weak π–π interactions between aromatic rings, with centroid-to-centroid distances of 3.796 (2) and 4.171 (2) Å. There is also a single C—Cl⋯π interaction .In the molecule of the title compound, [Sn(C DOI: 10.1107/S1600536808018321/hk2473Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The Ni—O(phenolate) bond [1.9750 (16) Å] is shorter than the Ni—O(carbonyl) bond [2.0840 (16) Å] and the Ni—N bonds (mean 2.120 Å).In the title compound, [Ni(C DOI: 10.1107/S1600536808023489/is2292Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


I atom in the salt, [Ag(C4H6N2)2]NO3·2H2O, shows a nearly linear coordination [N—Ag—N = 178.26 (7)°]. The cation, anion and water molecules are linked by N—H⋯O and O—H⋯O hydrogen bonds into a layer motif extending parallel to (101).The Ag DOI: 10.1107/S1600536809045838/bt5122Isup2.hklStructure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The HfO8 coordination polyhedron shows a slightly distorted Archimedean square anti-prismatic coordination with average Hf—O, C—O, C—CMe distances of 2.19 (2), 1.26 (2) and 1.49 (2) Å, respectively, and an O—Hf—O bite angle of 75.3 (5)°. Weak O—H⋯O hydrogen bonding interactions are observed between one of the bridging hydroxy groups and the disordered solvent molecule.The binuclear title compound, [Hf DOI: 10.1107/S1600536809041658/wm2265Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The Cl ligands are trans to each other, with a Cl—Pt—Cl angle of 178.83 (8)°. The pyridine ring forms a dihedral angle of 48.8 (2)° with the planar PtCl2SN unit. Within the molecule, the distance between Pt atoms is 20.262 (5) Å and the N⋯N separation between the terminal pyridyl rings is 16.23 (1)Å.The title dinuclear platinum compound, [Pt DOI: 10.1107/S1600536808024914/gk2157Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Molecules are connected into layers in the ac plane via extensive C—H⋯Cl contacts as each Cl atom forms two such interactions. Contacts between the layers are of the type C=O⋯π [O⋯centroid distance = 3.110 (8) Å].In the title compound, [HgCl DOI: 10.1107/S1600536809049289/hy2254Isup2.hklStructure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The CuII atom is coordinated by one tridentate N-salicylideneglycinate Schiff base ligand, one 4-methylquinoline ligand and one water molecule, leading to a slightly distorted square-pyramidal N2O3 geometry. In the crystal structure, the molecules are linked by O—H⋯O hydrogen bonds into linear chains in the [100] direction. The structure is further stabilized by intermolecular C—H⋯O interactions and C⋯C contacts with C⋯C = 3.3058 (2), 3.3636 (2) and 3.3946 (2) Å.The title complex, [Cu(C DOI: 10.1107/S1600536807067852/tk2236Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


II complex, [Co(C8H5O3)2(C10H14N2O)2(H2O)2], the metal centre is located on an inversion center and is coordinated by two 4-formylbenzoate (FOB), two diethylnicotinamide (DENA) ligands and two water molecules in a slightly distorted CoO4N2 octahedral geometry. In the crystal structure, O—H⋯O hydrogen bonds link the molecules into infinite chains. π–π contacts between the parallel pyridine rings of neighboring DENA ligands [centroid–centroid distance = 3.652 (3) Å] further stabilize the crystal structure.In the crystal structure of the title Co DOI: 10.1107/S1600536809008265/xu2489Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


A Cu⋯Cu separation of 3.2281 (3) Å is observed. The in-plane Cu—Ophenolate distance [1.9342 (8) Å] is shorter than the axial distance [2.252 (8) Å]. The Cu—Namine and Cu—Npy distances are similar . The Cu—Nthiocyanate distance [1.9678 (11) Å] is in the range found for Cu—N distances in previously determined structures containing coordinated thiocyanate anions. There is an intermolecular hydrogen bond between the amine H atom and the S atom of a coordinated thiocyanate anion.The centrosymmetric binuclear complex, [Cu DOI: 10.1107/S1600536809031742/kp2227Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the structure, the ZrIV atom is nine-coordinated by three (pydc)2− groups, resulting in an anionic complex which is balanced by two (tataH)+ cations. One of the NH2 groups shows positional disorder, with site occupation factors of 0.60 and 0.40. There are four uncoordinated water molecules  (one of which is disordered with occupation factors of 0.70 and 0.30) in the crystal structure. Several intermolecular interactions, including O—H⋯O, O—H⋯N, N—H⋯O, N—H⋯N, C—H⋯O and C—H⋯N hydrogen bonds, a C—O⋯π interaction , and π–π stacking [with centroid–centroid distances of 3.694 (2) and 3.802 (2) Å] are also present.The title compound, (C DOI: 10.1107/S1600536808029887/om2259Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The hydroxonium hydrate (H5O2)+, also known as the Zundel cation, resides on a twofold rotation axis. The O—H distance is 1.274 (14) Å, the O⋯O distance is 2.518 (5) Å, and the O—H—O angle is 162 (8)°. One of the melamine H+ cations, the uncoordinated pydcH2, and two water molecules also reside on crystallographic twofold axes. The CuII atom has a tetragonally distorted octahedral coordination environment. The structure features extensive hydrogen bonding, with 21 distinct interactions. There is also a centrosymmetric C=O⋯π interaction with an O⋯centroid distance of 3.288 (3) Å. The structure is similar to a mixed-valence manganese(II/III) structure but shows interesting differences in the metal-atom coordination. One of the water molecules is equally disordered with respect to a twofold axis.The reaction of copper(II) nitrate hexahydrate with pyridine-2,6-dicarboxylic acid (pydcH DOI: 10.1107/S1600536809000828/gw2056Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The crystal structure is stabilized by intermolecular O—H⋯O and C—H⋯O interactions. In addition, the crystal structure exhibits a Br⋯π interaction of 3.551 (3) Å between the Br atom and the centroid of the benzene ring of an adjacent molecule.In the title compound, C DOI: 10.1107/S1600536809008101/zl2184Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The 2,5-dimethylpyrazine 1,4-dioxide ligand, which also lies on an inversion center, acts as a bridging ligand, linking symmetry-related CoII ions [Co⋯Co = 8.669 (3) Å] and forming one-dimensional chains along the b axis. In the crystal structure, these chains are linked by intermolecular aqua–perchlorate O—H⋯O hydrogen bonds, forming two-dimensional layers which are in turn connected into a three-dimensional network via π–π stacking interactions between quinoline rings, with a centroid–centroid distance of 3.580 (3) Å. An intermolecular O—H⋯Cl interaction is also present.In the title complex, {[Co(C DOI: 10.1107/S1600536810008895/lh5007Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The AgI ion is linearly coordinated by two dipyrazin-2-ylamine ligands through two pyrazine N atoms. (ClO4               −)⋯π(pyrazine) [O⋯centroid distances of 3.612 (3) and 3.664 (1) Å] and π–π interactions [centroid–centroid distance = 3.518 (2) Å] as well as O—H⋯O and N—H⋯O hydrogen-bonds assemble the chains into a three-dimensional supramolecular aggregation. In the title complex, {[Ag(C DOI: 10.1107/S1600536809037532/bg2275Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the crystal structure, inversion-related molecules are linked into dimers by O—H⋯O hydrogen bonds. The packing is further stabilized by π–π interactions involving the benzene rings of the dmphen and hydroxybenzoate units, with centroid–centroid distances of 3.4930 (14) or 3.5727 (14) Å.In the title compound, [Cu(C DOI: 10.1107/S1600536808034788/ci2692Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials: