II coordination polymer has been prepared via solvothermal synthesis using dimethyl sulfoxide as solvent. The coordination polymer forms double-chains along [010] and exhibits π–π stacking and C—H⋯π interactions forming the interior of the double-chains, separated from a C—H⋯π hydrogen-bonding network in the space between the double-chains.A one-dimensional Ni 7H3NO4)(C4H4N2)(C2H6OS)]n, consists of [010] chains composed of NiII ions linked by bis-monodentate-bridging pyrazine molecules. Each of the two crystallographically distinct NiII ions is located on a mirror plane and is additionally coordinated by a dimethyl sulfoxide (DMSO) ligand through the oxygen atom and by a tridentate 2,6-pyridine-dicarboxylic acid dianion through one of each of the carboxylate oxygen atoms and the pyridine nitrogen atom, leading to a distorted octahedral coordination environment. The title structure exhibits an interesting complementarity between coordinative bonding and π–π stacking where the Ni—Ni distance of 7.0296 (4) Å across bridging pyrazine ligands allows the pyridine moieties on two adjacent chains to interdigitate at halfway of the Ni—Ni distance, resulting in π–π stacking between pyridine moieties with a centroid-to-plane distance of 3.5148 (2) Å. The double-chain thus formed also exhibits C—H⋯π interactions between pyridine C—H groups on one chain and pyrazine molecules on the other chain. As a result, the interior of the double-chain structure is dominated by π–π stacking and C—H⋯ π interactions, while the space between the double-chains is occupied by a C—H⋯O hydrogen-bonding network involving DMSO ligands and carboxylate groups located on the exterior of the double-chains. This separation of dissimilar interactions in the interior and exterior of the double-chains further stabilizes the crystal structure.The title coordination polymer, [Ni(C II complex obtained by reacting 2,6-pyridine dicarboxylic acid and nickel carbonate using water as solvent , where each of the NiII atoms is coordinated by a 2,6-pyridine-dicarboxylic acid dianion, a pyrazine molecule, and a DMSO ligand  Å, i.e. the length of the b axis.The asymmetric unit contains two half Nind Fig. 1. The triII chains form a double-chain structure via π–π stacking between their pyridine moieties . Double-chains of molecule A are linked by C21A—H21E⋯O2Ai/iv, C12A—H12A⋯O1Ai, C21A—H21D⋯O4Aiii, and C22A—H22D⋯O4Aiii hydrogen bonds to form sheets extending along the same direction. Thus, alternating sheets with an ABAB pattern can be observed. Two neighboring sheets are connected via C11A—H11A⋯O5B and C11B—H11B⋯O5A hydrogen bonds to form a three-dimensional network. The hydrogen-bond lengths and angles are summarized in Table 1In contrast to the π–π stacking and C—H⋯π interactions forming the interior of the double-chains, the exterior of the double-chains is mainly occupied by polar DMSO molecules and carboxylate groups. As a result, a network of C—H⋯O hydrogen bonds exists in the space between the double-chains Fig. 3, linkingIn summary, a separation of dissimilar interactions can be observed between the non-covalent lipophilic π–π stacking and C—H⋯π interactions in the interior of the double-chains and the polar hydrogen bonds in the exterior of the double-chains, further stabilizing the crystal structure.3 , 2,6-pyridine dicarboxylic acid , and pyrazine  were dissolved in 10 ml dimethyl sulfoxide. The resulting mixture was transferred into a stainless steel autoclave which was heated at 373 K for 24 h and cooled to room temperature at a cooling rate of 0.1 K per minute. Green needle-like crystals of the title compound were collected by filtration. Selected IR bands : 1640.6 (C=O), 1367.9 (C—O), 950.9 (S=O), 480.6 (bridging pyrazine).Anhydrous NiCOUiso(H)= 1.2/1.5Ueq(C). Methyl H atoms were allowed to rotate around the corresponding C—C bond. There are two disordered parts, both of which are in molecule A. The carboxylate atom O2A sits just outside of the mirror plane (occupancy 0.5) and one of the DMSO methyl groups is disordered over two positions in a ratio of 0.54 (2):0.46 (2). The C atom of this group was refined with isotropic displacement parameters.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989016007064/wm5288sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989016007064/wm5288Isup2.hklStructure factors: contains datablock(s) I. DOI: 1476677CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


We have evaluated the efficacy of dapagliflozin in patients with type 1 diabetes mellitus (DM1) without adequate control. We expected that adding dapagliflozin to this population on top of their base treatment would lower their HbA1c levels.We conducted a pragmatic, open, 24-week study of treatment with 10 mg of oral dapagliflozin in patients with DM1 and chronic hyperglycemia. We evaluated glycemic control, lipid profile, weight, and insulin dose. Safety was assessed by adverse event reporting.p = 0.08). The hemoglobin A1C (HbA1C) level decreased from 9.18 ± 1.02 (77 ± 11.1 mmol/mol) to 8.05 ± 1.09 % (64 ± 11.9 mmol/mol) (p = 0.0156); total cholesterol decreased from 299 ± 12 to 199 ± 7 mg/dL (p = 0.02); triglycerides decreased from 184 ± 15 to 160 ± 11 mg/dL (p = 0.0002), HDL-C decreased from 40 ± 17 to 42 ± 9 mg/dL (p = 0.54); and LDL-C decreased from 187 ± 19 to 170 ± 21 mg/dL (p = 0.049). No adverse events were reported.Fasting glucose levels decreased from 176.42 ± 45.33 mg/dL to 139.67 ± 44.42 mg/dL (p = 0.05); although no significant valued was reached, postprandial glucose showed a decreased tendency from 230.25 ± 52.06 mg/dL to 193.83 ± 45.43 mg/dL (The beneficial effects of SGLT2 inhibitors on metabolic control and their safety after a 24-week open study demonstrate their potential indication as an adjunctive treatment with insulin in patients with DM1; however, long-term clinical trials should be considered. Treatment of Type 1 diabetes mellitus (DM1) is presently restricted to insulin and in selected cases, pramlintide and islet or pancreas transplantation .In contrast the management of DM1 with oral drugs is limited. Sodium/glucose cotransporter 2 inhibitors (SGLT2I), as initial or in combination therapy have recently been used to treat type 2 diabetes mellitus (DM2) . These dThe aim of this study was to evaluate the efficacy of dapagliflozin in a group of patients with poorly controlled DM1. We expected that adding dapagliflozin to this population’s insulin regimen, would improve their glycemic control.We performed an open, 24-week, pragmatic clinical trial in a group of patients with poorly controlled DM1 in a private clinic in Monterrey, Nuevo Leon, México from 2013–2014. Twelve patients met the following inclusion criteria: DM1 according to the American Diabetes Association classification ; both geChanges in fasting and postprandial glucose  and HbA1C were considered to be the primary outcomes. Appearance of hypoglycemia, genitourinary or micotic infections and ketonuria were routinely revised.The study protocol was approved by the local research ethics committee.2.Twelve patients were included  with a mean age of 27 ± 11 years and a mean duration of disease of 9.17 ± 7.41 years. All were overweight with a body mass index (BMI) of 27.98 ± 1.97 kg/mp = 0.05). The postprandial glucose decreased from 230.25 ± 52.06 mg/dL to 193.83 ± 45.43 mg/dL; however, it did not reach a significant value (p = 0.08). HbA1C significally decreased from 9.18 ± 1.02 % (77 ± 11.1 mmol/mol) to 8.05 ± 1.09 % (64 ± 11.9 mmol/mol) (p = 0.0156). The lipid profile was modified favorably, with total cholesterol decreasing from 299 ± 12 to 199 ± 7 mg/dL (p = 0.02), LDL-C from 187 ± 19 to 170 ± 21 mg/dL (p = 0.049) and triglycerides from 184 ± 15 to 160 ± 11 mg/dL (p = 0.0002). HDL-C was unchanged at 40 ± 17 and 42 ± 9 mg/dL (p = 0.54)  [ weeks [8The lipid profile also improved following treatment, with reductions in total cholesterol, c-LDL cholesterol and triglycerides . This is inconsistent with previous SGLT-2 studies and may have resulted from improved glycemic control, weight loss, or other causes , 9.An unattained metabolic control of DM1 has prompted a search for other therapeutic options, like pramlintide or islets transplantation , 10–12.Evidence of efficacy of SGLT2I in DM1 is limited ; howeverWe believe that dapagliflozin is safe and well tolerated with no clinically documented adverse effects. In addition, our study had the strength of a pragmatic design with a relatively long treatment period.However, recently the U.S. Food and Drug Administration (FDA) issued a Drug Safety Communication warning of an increased risk of diabetic ketoacidosis associated with the used of all the approved SGLT2I. This potential complication related is predictable, detectable, and preventable, with the full picture still favoring the use of SGLT2I DM1 patient .Nevertheless, we recognize that the data should be cautiously considered because the study was performed in a specialized care center with educated patients and a small sample size of overweight individuals. Also, we do not have information regarding the follow up of the patients.Dapagliflozin as an adjunct therapy to insulin caused significant changes in the HbA1C level, fasting and postprandial glucose and atherogenic lipid in patients with DM1. Thus, dapagliflozin may represent a new therapeutic approach, although long-term controlled clinical trials with a greater number of patients are needed to confirm our data.


N-{4-[(6-chloropyridin-3-yl)methoxy]phenyl}-2,6-difluorobenzamide is reported. The crystal packing is stabilized by N—H⋯N, C—H⋯O, C—H⋯F and C—H⋯π hydrogen bonds supplemented by offset π–π stacking interactions.The molecular and crystal structure of  19H13ClF2N2O2, the conformation of the N—H bond in the amide segment is anti to the C=O bond. The molecule is not planar, with dihedral angles between the central benzene ring and the outer benzene and pyridyl rings of 73.35 (7) and 81.26 (6)°, respectively. A weak intramolecular C—H⋯O hydrogen bond occurs. In the crystal, N—H⋯N, C—H⋯O and C—H⋯F hydrogen bonds lead to the formation of dimers. The N—H⋯N inversion dimers are linked by π–π contacts between adjacent pyridine rings [centroid–centroid = 3.8541 (12) Å] and C—H⋯π interactions. These contacts combine to stack the molecules along the a axis.In the title compound, C The mixture was stirred at 283–288 K for 2 h, then washed with 0.5% hydrochloric acid solution, and a saturated aqueous solution of sodium hydrogen carbonate, dried and evaporated. The residue was recrystallized from dichloromethane, giving colourless blocks of the title compound after three weeks.N-(4-(pyridin-3-ylmethoxy)phenyl)benzamide or its substituted derivatives gave no hits. However, structures of eight substituted 2,6-difluoro-N-phenylbenzamide derivatives were found, see for example Cockroft et al.   = 0.93–0.97 Å and Uiso(H) = 1.2Ueq(C).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015023701/sj5486sup1.cifCrystal structure: contains datablock(s) global, I. DOI: 10.1107/S2056989015023701/sj5486Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989015023701/sj5486Isup3.cmlSupporting information file. DOI: 1441555CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The position of the second non-linking cage C atom was established unambiguously by geometric and crystallographic methods and there is no evidence of C/B disorder.In 1,1′-bis[1,7-dicarba- 4H22B20, the two {1,7-closo-C2B10H11} cages are linked across a centre of inversion, with C—C = 1.5401 (16) Å. The position of the second non-linking cage C atom was established unambiguously by geometric and crystallographic methods and there is no evidence of C/B disorder.In the title compound, C There are several isomeric possibilities for bis(carboranes) composed of two C2B10 icosahedra. Bis(ortho-carborane), 1,1′-bis , 1,1′-bis, the subject of this study is, however, less well known. It was first prepared by Zakharkin & Kovredov ], (I)Whilst the chemistry of single-cage carboranes is well developed  linked across a crystallographic inversion centre by the C1—C1A bond  °, and the facing pentagons B2/B3/B4/B5/B6 and B2A/B3A/B4A/B5A/B6A are staggered. The five C1—B distances span the range 1.7107 (12)–1.7385 (12) Å, whilst C7—B connectivities lie between 1.6967 (13) and 1.7180 (13) Å, with, in both cases, the two shortest distances being to the B atoms (B2 and B3) that lie between the C atoms. The B2—B3 connectivity, 1.7947 (13) Å, is the longest B—B link, with all (19) others lying between 1.7709 (13) and 1.7891 (15) Å. In general terms these C—B and B—B distances are fully consistent with the averages recently calculated, 1.705 (14) and 1.772 (11) Å, respectively z] Fig. 1. The twoB at 2.39 Å . Although CH units and BH units in carboranes are protonic and hydridic, respectively, there is no evidence of dihydrogen bonding, the shortest such contact being H7⋯H12C at 2.61 Å [symmetry code: (C) −x + y + z + The only H⋯H contact less than 2.40 Å is H6⋯H6closo-C2B10 fragment using Conquest (Version 1.16) returned 132 hits of which only two involve the 1,1′-bis unit. In DUWJAH 2} groups attached to C7 and C7′ whilst in DUWJEL (OMe)} units. Of the remaining 130 hits there are five cases of the parent molecule 1,7-closo-C2B10H12 co-crystallized with other molecules, the first of these to be reported being the hexamethylphosphoramide adduct TOKGOP  was refined and then analysed by both the Vertex-to-Centroid Distance  = 1.2Ueq.Crystal data, data collection and structure refinement details are summarized in Table 110.1107/S1600536814022132/hb7290sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S1600536814022132/hb7290Isup2.hklStructure factors: contains datablock(s) I. DOI: 1027936CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


H = (1–3/Nr)In the Methods section, Equation 2b is incorrect. The correct equation is: θ


I ions complexed by ferrocenediyl-1,1′-dicarbonitrile forming a paddle-wheel with two acetone molecules, with one coordinating on top of one trigonal–planar-coordinated copper ion, and the other as a packing solvent.The first ferrocenylcarbonitrile copper complex is reported. The structure consists of two Cu O)trisdicopper(I) bis(tetrafluoridoborate) acetone monosolvate, [Cu2Fe3(C6H4N)6(C3H6O)](BF4)2·C3H6O, consists of two CuI ions bridged by a ferrocene-1,1′-dicarbonitrile moiety in a paddle-wheel-architectured sandwich complex with two BF4− units as counter-ions. One of the latter is equally disordered over two sets of sites. The two CuI ions are complexed in a trigonal–planar manner by three nitrile N-donor atoms. Further interactions by the O atom of an acetone molecule to one of the CuI atoms and a weak η2,π-interaction of two atoms of a cyclopentadienyl ring to the other CuI atom complete a distorted trigonal–pyramidal environment for each of the metal ions. A further acetone molecule is also present as a solvent molecule. The crystal packing is consolidated by several π–π interactions.The molecular structure of (acetone-κ M—C C— , showing moderate electron communication between two redox-active metallocenyl termini in the mixed-valence species –phenylene bridge shows a moderate delocalization. In contrast, a weak electron transfer by generation of the mixed-valence species [Ru(N CFc)(NH3)5]3+ [Fc = Fe(η5-C5H4)(η5-C5H5)] has been described  bridging unit between two redox-active ferrocenyl moieties 2CO}{μ-Fe(η5-C5H4C N)2}3](BF4)2·(CH3)2CO, (I)The electron-transfer properties of the acetylide function have been investigated intensively by using bridging units of the type —C C— al. 2011 describe2Fe3 complex molecule in the asymmetric unit consisting of two CuI ions bridged by three 1,1′-ferrocenediyl dicarbonitrile ligands that form a triangular paddle-wheel sandwich-type complex with iron⋯iron distances ranging from 9.1739 (13) (Fe2⋯Fe3) to 10.0385 (12) Å . The complex crystallizes with two BF4− counter-ions and two molecules of acetone. One acetone molecule coordinates with its oxygen atom to Cu1 [Cu1—O1 2.375 (2) Å], leading to an 18 VE complex and an overall distorted trigonal–pyramidal environment. The Cu2 ion exhibits a weak intermolecular η2, π interaction  as compared to Cu2 [0.0602 (16) Å] due to a stronger interaction with the axial moiety. The Cu⋯Cu distance [3.3818 (7) Å] exceeds the sum of the van der Waals radii  °; α C5⋯Cu2, 93.23 (1) °; Table 1Besides the already noted intermolecular interaction between Cu2 and the mid-point of the C26—C27 bond, π–π interactions are present in the crystal packing between the C23 atom and its symmetry-generated equivalent (BF4)2·(CH3)2CO: Copper powder , Cu(BF4)2·5H2O  and ferrocene-1,1′-dicarbonitrile  were stirred in 5 ml of dichloromethane at room temperature overnight. The resulting orange precipitate was filtered off using zeolite and washed several times with 20 ml of dichloromethane until the filtrate was colorless. The residue was taken up in acetone and this solution was evaporated to dryness using a rotary evaporator affording (I)4]2·5H2O). IR : ν = 2248 (CN). 1H NMR  = 5.12 , 4.82 . 13C{1H} NMR: Data not available due to low solubility. HRMS (ESI–TOF): M+ C12H8N2CuFe (C24H16N4CuFe2): m/z = 534.9342 ; M+ C24H16N4CuFe2 (C12H8N2CuFe): m/z = 298.9342 .Ferrocene-1,1′-dicarbonitrile was prepared according to a published procedure (Strehler Uiso(H) = 1.2Ueq(C) and a C—H distance of 0.93 Å for aromatic and Uiso(H) = 1.5Ueq(C) and a C—H distance of 0.96 Å for methyl H atoms. The F atoms of one of the two BF4− ions were refined as equally disordered over two sets of sites using DFIX [B—F 1.38 (2) Å] and DANG [F—F 2.25 (4) Å] instructions. Since some anisotropic displacement ellipsoids were rather elongated, DELU/SIMU/ISOR restraints were also applied  I. DOI: 10.1107/S2056989015001760/wm5104Isup2.hklStructure factors: contains datablock(s) I. DOI: 1045804CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


AbstractParaplonobia Wainstein and Neopetrobia Wainstein (Trombidiformes: Tetranychidae) are reported for the first time from Saudi Arabia. Three new species Paraplonobia (Anaplonobia) arabica Mirza & Alatawi, sp. n., Paraplonobia (Anaplonobia) haloxylonia Alatawi & Mirza, sp. n. and Paraplonobia (Anaplonobia) tabukensis Kamran & Alatawi, sp. n. are described and illustrated based on adult females, collected from Prosopisjuliflora (SW.) Dc. (Fabaceae) and Haloxylonsalicornicum Bunge (Amaranthaceae) from two different regions of Saudi Arabia. Neopetrobiamcgregori (Pritchard and Baker) is redescribed and illustrated based on female collected from Cynodondactylon L. (Poaceae).The diagnostic morphological features including leg chaetotaxy of all known species of the subgenus Anaplonobia is tabulated. A key to the world species of the genus Paraplonobia is also provided.The two tetranychid genera  Paraplonobia Wainstein belongs to the tribe Hystrichonychini Pritchard and Baker of the subfamily Bryobiinae (Acari: Prostigmata: Tetranychidae). Anaplonobia and Paraplonobia as subgenera of Aplonobia Womersley. Later, Anaplonobia and Paraplonobia as two valid genera. After that, Paraplonobia into three subgenera: Anaplonobia Wainstein, Brachynychus Mitrofanov & Strunkova and Paraplonobia Wainstein on the basis of coxal setal count and the aspect of peritremes and considered the genus Anaplonobia as subgenus of Paraplonobia , Eutetranychuspalmatus Attiah, Oligonychusafrasciaticus (McGregor), Oligonychuspratensis (Banks), Tetranychuscinnabarinus , Tetranychusturkrestzni (Ugarov & Nikolskii), and Tetranychusurticae (Koch)  harteni Meyer and Paraplonobia (Paraplonobia) dactyloni Smiley & Baker were reported from Yemen (A few tetranychid species have been reported from Saudi Arabia (SA): e (Koch) . The genom Yemen .Paraplonobia and Neopetrobia, are reported upon for the first time from Saudi Arabia with three new species: Paraplonobia (Anaplonobia) arabica sp. n., Paraplonobia (Anaplonobia) haloxylonia sp. n. and Paraplonobia (Anaplonobia) tabukensis sp. n. which are described and illustrated based on adult females. The male of Paraplonobia (Anaplonobia) haloxylonia sp. n. is also described and illustrated. Neopetrobiamcgregori (Pritchard & Baker) is redescribed and illustrated based on female.Two genera, Anaplonobia are provided including body morphological features, leg I length in comparison to body length, and leg chaetotaxy  haloxylonia sp. n., female paratype each of Paraplonobia (Anaplonobia) arabica sp. n., and Paraplonobia (Anaplonobia) tabukensis sp. n., with Accession numbers, OSAL 0115769, OSAL 00115768, OSAL 0110333 and OSAL 0110332 respectively, that were deposited at UniversityOhio State  Acarology Laboratory(OSAL), USA.The mite specimens were collected by shaking the plant parts, especially leaves, onto a white sheet of paper. Mites found moving on paper were collected with the help of a camel hairbrush and preserved in small vials containing 70% ethanol. Preserved mite specimens were observed under a stereomicroscope  and mounted on glass slides in Hoyer’s medium. The mounted specimens were examined under phase contrast microscope . Different body parts were pictured using an auto montage software system , then drawn with Adobe Illustrator . All measurements are in micrometers. The terminology used in this paper follows that of Taxon classificationAnimaliaProstigmataTetranychidaeGenusWainstein, 1960Aplonobia (Paraplonobia) Wainstein, 1960: 140.Paraplonobia : Aplonobia (Paraplonobia) echinopsili Wainstein, 1960 by original designation.Based on Baker and Tuttle 1968, Gutierrez 1955, 1 normal in position, coxal setal formula variable, most species with 2–2–1–1 except one species of the subgenus Brachynychus having 4–3–2–2 setae on coxae I–IV respectively; anal setae three pairs; peritremes simple/anastomosing; tarsus I with two sets of duplex setae, present close to distal end of tarsus; claws and empodium pad-like each with tenant hairs  Eight species with dorsal body setae slightly shorter/as long as or longer than distances to the bases of consecutive setae (Tables Paraplonobia (Anaplonobia) arabica sp. n., Paraplonobia (Anaplonobia) haloxylonia sp. n., and Paraplonobia (Anaplonobia) tabukensis sp. n.) reported in this study , comparative length of setae with respect to the distance of setae next behind, shape of peritremes , propodosomal shield , hysterosoma , comparative length of leg I with respect to body length (shorter/longer) and leg chaetotaxy are the major diagnostic characters vary among/within the species of subgenus ia Table , 2.Anaplonobia have been reported from USA, Mexico, South Africa and Pakistan and collected mostly from three host plants families Asteraceaea, Fabaceae and Poaceae (Most species of the subgenus  Poaceae  (Table 1Paraplonobia (Anaplonobia) arabica sp. n., collected from Prosopisjuliflora from three different regions  of Saudi Arabia, are morphologically similar except for some variations in setal counts on Tibia II and Tarsus I–II–III. (Table Paraplonobia (Anaplonobia) prosopis had been found also in the description made by Anaplonobia, setal variations on genua, tibiae and tarsi have been found among the different specimens collected from the same host and location within the same species. i.e. genua I (8–9) in Paraplonobia (Anaplonobia) candicans, tibia I (12–13) and tarsus II (12–13) of Paraplonobia (Anaplonobia) glebulanta, and tarsus III (12–13) of Paraplonobia (Anaplonobia) theroni . Measurement of holotype followed by 8 paratypes (in parenthesis) Figs –8.Dorsum , sc1 40 (38–41), sc2 41 (40–43), c1 45 (44–48), c2 42 (40–44), c3 40 (39–44), d1 34 (32–38), d2 44 (43–46), e1 45 (44–48), e2 44 (43–45), f1 45 (44–45), f2 44 (42–45), h1 46 (45–48). Distance between dorsal setae: v2–v2 53 (51–55), v2–sc1 97 PageBreak(95–98), sc1–sc2 56 (54–57), sc1–sc1 166 (162–167), sc2–sc2 263 (260–266), c1–c1 94 (92–96), c1–c2 82 (80–85), c2–c3 41 (39–44), c2–c2 261 (260–264), c3–c3 345 (340–346), d1–d1 82 (80–84), d1–d2 81 (80–82), d2–d2 226 (224–228), c1–d1 75 (74–78), c3–d2 97 (95–99), e1–e1 63 (61–65), e1–e2 78 (74–79), e2–d2 85 (83–86), e2–e2 79 (75–79), f1–f1 63 (60–65), f2–f2 107 (105–108), f1–f2 53 (50–54), f1–d1 69 (66–70), h1–h1 57 (55–59).sum Fig. . Body ovVenter , g2 40 (38–42), g1–g1 40 (39–44), g2–g2 56 (52–57), g1–g2 12 (10–14); anal setae three pairs, ps1 21 (18–24), ps2 37 (35–39), ps3 58 (54–60), ps1–ps1 33 (30–34), ps2–ps2 26 (24–27), ps3–ps3 19 (18–22); para-anal setae two pairs, h2 33 (31–34), h2– h2 17 (16–18), h3 38(35–40), h3–h3 46 (45–48).ter Fig. . IdiosomGnathosoma , Deesa Valley, Dessa, Tabuk, SA, 27°36.048'N, 036°25.592'E, October, 18, 2015, coll. J.H. Mirza.; seven paratype females, Prosopisjuliflora (Fabaceae), Sharma, Near Red Sea, Tabuk, SA, 28°03.479'N, 035°17.186'E, October, 19, 2015, coll. M. Kamran.Holotype and one paratype female, Paraplonobia (Anaplonobia) arabica sp. n. relates to Paraplonobia (Anaplonobia) prosopis , Paraplonobia (Anaplonobia) algarrobicola  and Paraplonobia (Anaplonobia) boutelouae Tuttle & Baker, 1968 because of sharing following similar characters: dorsal body setae spatulate and distinctly shorter to the distances of setae next behind and widely spaced dorsal hysterosomal striations. Also, the new species closely resembles Paraplonobia (Anaplonobia) prosopis by setae c1 at least reaching half distance to the bases of setae d1. However, the new species differs PageBreakfrom all related species by having stylophore anteriorly with slight incision (notch). The new species is also distinguished from Paraplonobia (Anaplonobia) prosopis by setae c1 reaching to the distance of setae d1 (2/3 vs.1/2), setae c1–c1 almost 1.5 times widely spaced than setae f1–f1 vs. almost sub/equally spaced in Paraplonobia (Anaplonobia) prosopis. The new species can be separated from other related species Paraplonobia (Anaplonobia) algarrobicola and Paraplonobia (Anaplonobia) boutelouae by the setae c1 reaching 2/3 to the distance of d1 vs. less than half as long as distances to the bases setae next behind in later speciesThe Taxon classificationAnimaliaProstigmataTetranychidaehttp://zoobank.org/09E8353-E635-4C38-B277-8D6DDC56C31ADorsal setae lanceolate, densely serrate, not set on tubercles and distinctly shorter to the distances of setae next behind, dorsocentral setae  almost 1/3 to the distance of setae next behind, propodosoma medially with weak, longitudinal irregular striations, hysterosoma with transverse and closely spacedstriations medially, stylophore slightly notched anteriorly, peritremes anastomosed distally, with few long thread like branches, and hysterosomal striations closely spaced, leg I shorter than body.n = 39). Measurements of holotype followed by 38 paratypes (in parenthesis) , sc1 24 (23–25), sc2 22 (21–24), c1 19 (18–21), c2 22 (21–23), c3 25 (24–28), d1 15 (12–16), d2 18 (17–19), e1 16 (15–17), e2 20 (19–20), f1 25 (24–28), f2 31 (29–32), h1 34 (32–35). Distance between dorsal setae: v2–v2 72 (70–73), v2–sc1 75 (72–78), sc1–sc2 66 (63–67), sc1–sc1 167 (163–172), sc2–sc2 254 (250–259), c1–c1 90 (88–92), c1–c2 75 (71–78), c2–c3 81 (78–85), c2–c2 231 (229–234), c3–c3 373 (372–375), d1–d1 91 (89–92), d1–d2 65 (62–69), d2–d2 204 (201–206), c1–d1 103 (100–104), c3–d2 160 (158–161), e1–e1 55 (53–57), e1–e2 53 (50–54), e2–d2 85 (82–86), e2–e2 150 (148–152), f1–f1 60 (59–62), f2–f2 80 (78–83), f1–f2 28 (25–29), f1–d1 93 (91–94), h1–h1 31 (28–32).sum Fig. . Body ovVenter , g2 20 (19–21), g1–g1 32 (31–33), g2–g2 35 (34–36), g1–g2 10 (10–12); anal setae three pairs, ps1 11 (10–12), ps2PageBreakPageBreakPageBreak16 (15–17), ps3 17(16–18), ps1–ps1 16 (15–18), ps2–ps2 22 (20–23), ps3–ps3 26 (25–26); para–anal setae two pairs, h2 16 (15–17), h2– h2 14 (13–16), h3 17 (15–17), h3–h3 31 (30–32)  Fig. .Gnathosoma –9–9–9; tarsi I with 15 tactile setae, two sets of duplex setae at distal end, 11 tactile setae and two solenidia well proximal to duplex setae, two eupathidia; tarsi II with 10 tactile setae, one set of duplex setae, two eupathidia and one solenidion; tarsi III with 12 tactile setae and one solenidion; tarsi IV with 12 tactile setae and one solenidion. True claws pad like each with one pair of tenant hair; empodium pad-like with two rows of small tenant hairs.egs Figs . Length Male (n = 11)  Figs –28. Dorssum Fig. . Body alVenter , anal setae three pairs ; para-anal setae two pairs ; aedeagus up turned, broadly sigmoid, sharply tapering distally , Salbookh Road, Dariyah, Riyadh, SA, 24°30.649'N, 46°46.615'E, September, 18, 2012, coll. M. Kamran; four males and 22 female paratypes, Hilaria sp. (Poaceae), Tashlia, Heyer Road, Riyadh, SA, 24°29.000'N, 46°47.890'E, January, 17, 2015, coll. J.H. Mirza; five males and four females paratypes, Hilaria spp. (Poaceae), Sanabal Farm, Kharaj, Riyadh, SA, 24°16.999'N, 47°11.854'E, January, 23, 2015, coll. M. Kamran.Holotype female, one male and two female paratypes, Remarks. The Paraplonobia (Anaplonobia) haloxylonia sp. n. closely resembles Paraplonobia (Anaplonobia) contiguus (Paraplonobia (Anaplonobia) contiguus by comparative length of leg I (shorter than body vs. longer than body), dorsocentral setae  almost 1/3 to the distance of setae next behind vs. more than half, number of setae on genu I (5 vs. 4) in Paraplonobia (Anaplonobia) contiguus.ontiguus  because Taxon classificationAnimaliaProstigmataTetranychidaehttp://zoobank.org/57BF2D3A-80B0-4C7E-90CD-FACB4543B5FFDorsal setae slightly lanceolate, densely serrate, not present on tubercles and distinctly shorter to the distances of setae next behind, prodorsum entirely with longitudinal striaitons, hysterosomal striations closely spaced, peritremes complex anastomosed distally, stylophore slightly rounded anteriorly, leg I shorter than body length, number of setae on femur I–IV 8–6–3–3, number of setae on genu I–IV 4–5–3–3.(n = 3). Measurements of holotype followed by 2 paratypes (in parenthesis) Figs –36.Dorsum , sc1 29 (28–31), sc2 30 (28–32), c1 28 (26–30), c2 26 (24–28), c3 29 (28–32), d1 23 (21–25), d2 22 (21–24), e1 21 (20–23), e2 22 (21–24), f1 23 (21–24), f2 26 (24–27), h1 27 (25–29). Distance between dorsal setae: v2–v2 89 (85–90), v2–sc1 68 (65–690), sc1–sc2 68 (67–70), sc1–sc1 204 (202–206), sc2–sc2 301 298–302), c1–c1 138 (135–140), c1–c2 91 (89–92), c2–c3 79 (75–80), c2–c2 327 (325–328), c3–c3 424 (422–426), d1–d1 119 (118–120), d1–d2 91 (89–92), d2–d2 295 (292–298), c1–d1 88 (86–89), c3–d2 110 (109–112), e1–e1 27 (25–28), e1–e2 85 (84–86), e2–d2 85 (84–86), e2–e2 229 (228–231), f1–f1 78 (76–80), f2–f2 113 (110–114), f1–f2 35 (33–36), f1–d1 82 (81–84), h1–h1 53 (52–56).sum Fig. . Body roVenter , g2 39 (35–40), g1–g1 52 (50–55), g2–g2 60 (58–64), g1–g2 12 (10–13); anal setae three pairs, ps1 20 (18–21), ps2 26 (24–27), ps3 28 (27–29), ps1–ps1 23 (20–24), ps2–ps2 32 (31–35), ps3–ps3 23 (21–26); para-anal setae two pairs, h2 27 (26–28), h2– h2 11 (10–13), h3 32 (31–34), h3–h3 28 (27–29).ter Fig. . IdiosomGnathosoma , 30 km Tabuk road, Sharma, Tabuk region, SA, 28°03.479'N, 035°17.186'E, October, 19, 2015, coll. M. Kamran and J.H. Mirza.Holotype female, two paratype females, Paraplonobia (Anaplonobia) tabukensis sp. n. closely resembles Paraplonobia (Anaplonobia) theroni (Paraplonobia (Anaplonobia) theroni by shape of stylophore anteriorly (rounded vs. slightly indented), number of setae on femur I–IV (8–6–3–3 vs. 9–6–4–4), number of setae on genu I–IV (4–5–3–3 vs. 5–5–6–6), number of setae on tibia III (8 vs. 6) and on tarsi I–II excluding duplex setae and solenidia (10–7 vs. 18–14) in Paraplonobia (Anaplonobia) theroni.The  theroni  because  theroni , 1987. TPageBreakTaxon classificationAnimaliaProstigmataTetranychidaeGenusWainstein, 1956Monoceronychus : Neopetrobia : Wainstein 1956: 151, Neopetrobiadubinini Wainstein, 1956.Based on Baker and Tuttle 1968, Gutierrez 1955, 1) widely spaced, not normal as c1; peritremes anastomosing distally.True claws pad like, each bearing a pair of tenant hairs; empodial pad longer than true claws, bearing a row of tenant hairs, distally not coalescent; dorsum with 3 pairs of prodorsal setae which are short and spindle shaped or spatulate; setal tubercles small or nonexistent; fourth pair of dorsocentral setae Monoceronychusmcgregori Pritchard & Baker, 1955.Neopetrobiamcgregori (Pritchard & Baker) Meyer, 1987. Female (n=9). Body oval; length of idiosoma 369–372, maximum width 238–241, length of body (gnathosoma + idiosoma) 430–433.Dorsum . Length of intercoxal and coxal setae: 1a 18–19, 3a 19–20, 4a 15–16, 1b 30–31, 1c 13–14, 2b 16–17, 2c 10–13, 3b 15–17, 4b 11–12; aggenital setae (ag) 26–27, ag–ag 38–39; genital setae two pairs, g1 17–18, g2 21–22, g1–g1 41–42, g2–g2 76–78, g1–g2 21–22; anal setae three pairs, ps1 11–12, ps2 10–11, ps3 12–13, ps1–ps1 11–13, ps2–ps2 16–18, ps3–ps3 11–13; para-anal setae two pairs, h2 11–13, h2– h2 7–9, h3 7–8, h3–h3 17–19.ter Fig. . IdiosomGnathosoma , near exit10, King Abdullah Road, Riyadh, SA, 24°45.826'N, 46°45.470'E, September 07, 2015, coll. M. Kamran and E. M. Khan.12 females, Neopetrobiamcgregori was originally described very briefly under the genus Monoceronychus and has been only reported from Miami shores of Florida, USA   . WorldwiPageBreak


II complex with a -N-phenyl-carbamohydrazinothioate ligand is reported. The crystal structure shows DMSO molecules bridging the complex units, building an one-dimensional H-bonded polymer.The synthesis and crystal structure of a Zn N-phenyl-2-hydrazinecarbothioamide ligand with zinc acetate dihydrate in a 2:1 molar ratio yielded a yellow solid, which was crystallized from DMSO to obtain the title compound, [Zn(C17H16N3S)2]·C2H6OS. The ZnII ion is four-coordinated in a distorted tetrahedral environment by two deprotonated ligands. Each ligand acts as an N,S-donor, forming a five-membered metallacycle. The maximum deviation from the mean plane of the N–N–C–S chelate group is 0.0029 (14) Å for the N-donor atom of one ligand and 0.0044 (14) Å for the non-coordinating N atom of the second. The dihedral angle between the planes of the two chelate groups is 72.80 (07)°. Bond lengths in the ligands are compared with those in the crystal structure of the free ligand. In the crystal, complex molecules are connected by dimethyl sulfoxide solvate molecules via N—H⋯O hydrogen-bonding interactions, building a one-dimensional hydrogen-bonded polymer along the a-axis direction. The S atom and one C atom of the dimethyl sulfoxide solvate molecules are disordered over two sets of sites with an occupancy ratio of 0.6:0.4.The reaction of the  II complex with the N-phenyl-2-hydrazinecarbothioamidate ligand. Thiosemicarbazone derivatives are N,S-donors with a wide range of coordination modes and a variety of applications in biological inorganic chemistry /N21—N22 = 1.393 (3) Å, N2—C11 = 1.303 (3)/N22—C31 = 1.304 (3) Å and C11—S1 = 1.755 (2)/C31—S21 = 1.749 (2) Å.The acidic hydrogen of the hydrazine fragment is lost by the reaction with the acetate anion. The negative charge of the deprotonated ligand is delocalized over the N—N—C—S entity, as indicated by their intermediate bond lengths. The bond lengths in the ligand are also affected by the coordination with the metal atom, especially the C—S bond length, which is consistent with increased single-bond character. In the crystal structure of the free ligand  is 58.25 (11)°. In the second ligand, the corresponding angle is 49.99 (11)° between the C25–C30 and C32–C37 rings. In addition, the aliphatic rings are also not planar. The maximum deviation from the mean plane for the C1–C5/C10 ring is 0.355 (3) Å for C3 and for the C21–C25/C30 ring the maximum deviation is 0.359 (3) Å for C23, with both of the aliphatic rings having an envelope conformationII complex molecules and the DMSO solvent molecules build a monomeric entity. The DMSO molecule bridges two complex molecules via intermolecular N—H⋯O hydrogen-bonding interactions, building a one-dimensional hydrogen-bonded polymer along the a-axis direction hydrazinecarbothioamide dissolved in THF (2 mmol/40 mL) with zinc acetate dihydrate dissolved in ethanol (1 mmol/30 mL) was refluxed for 4 h under continuous stirring. An orange solid was obtained, filtered and washed with ethanol. Suitable crystals for X-ray diffraction were obtained in DMSO by slow evaporation of the solvent.Starting materials were commercially available and used without further purification. The ligand synthesis was adapted from a procedure reported previously  = 1.2 Ueq(C) (1.5 for methyl H atoms) using a riding model with C—H = 0.95 Å for aromatic, C—H = 0.99 Å for methylene, C—H = 0.98 Å for methyl and N—H = 0.88 Å. In the DMSO solvate molecule, the S atom and methylene C atom C42 and attached H atoms are disordered and were refined using a split model with an occupancy ratio of 0.4:0.6.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S205698901500612X/im2462sup1.cifCrystal structure: contains datablock(s) I, publication_text. DOI: 10.1107/S205698901500612X/im2462Isup2.hklStructure factors: contains datablock(s) I. DOI: 1056177CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


All four phenyl rings in the two independent molecules are arranged in a propeller-like conformation. The two molecules exhibit S,R- and R,S- chirality and are connected via C—H⋯O intermolecular interactions.In the title compound, C 34H28O4, the cyclohexadiene ring has a screw-boat conformation with a torsion angle between the double bonds being on average ca 15° [15.2 (3) and −15.3 (3) in the two independent molecules]. All four phenyl rings in both molecules are arranged in a propeller-like conformation. The two molecules exhibit S,R- and R,S- chirality, respectively, and are connected via C—H⋯O intermolecular interactions. In turn, these weakly bound dimers form the molecular crystal.In the title compound, C Addition reactions of tetraphenylcyclopentadienone, often abbreviated to ‘tetracyclone’, were reviewed by Allen 1945, 1962 ▸.This study provides an opportunity to investigate the geometry of 1,3-cyclohexadiene rings surrounded by bulky substituents with no strong intermolecular interactions.s-gauche  Å, θ = 115.8 (3)° and φ = 213.1 (3); (C101–C106) Q = 0.463 (2) Å, θ = 63.7 (2)° and φ = 33.5 (3)°.The cyclohexadiene rings  and −15.3 (3) for the two independent molecules  form short contacts  with dimethylmaleate following Allen & Sheps 1934. GC–MS aUiso = 1.2iUso(C). All aromatic hydrogen atoms were refined with riding coordinates with C—H = 0.95–0.98 Å and Uiso = 1.2Uiso(C). Idealized methyl groups were refined as rotating groups with Uiso = 1.5Uiso(C).Crystal data, data collection and structure refinement details are summarized in Table 510.1107/S2056989016009403/zl2665sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989016009403/zl2665Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989016009403/zl2665Isup3.cdxSupporting information file. DOI: Click here for additional data file.10.1107/S2056989016009403/zl2665Isup4.cmlSupporting information file. DOI: 1484412CCDC reference: crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the crystal, O—H⋯O and O—H⋯N hydrogen bonds link complex molecules, forming a three-dimensional network incorporating The title complex, [Mg(C 7H7N4O2)2(H2O)4], lies across an inversion centre and the MgII atom is coordinated in a slightly distorted octahedral environment by four aqua ligands in the equatorial sites and two 1,3-dimethyl-2,6-dioxo-3,7-dihydro-1H-purin-9-ide ligands, through imidazole ring N atoms, in the axial sites. An intramolecular O—H⋯O hydrogen bond forms an S(7) graph-set motif. In the crystal, O—H⋯O and O—H⋯N hydrogen bonds link complex molecules forming a three-dimensional network incorporating R42(8) and R22(18) graph-set motifs.The title complex, [Mg(C II ion in a basic solution to give rise to a tetraaqua mononuclear MgII complex, (I)Co-crystallization represents a crystal engineering approach for modifying properties of active pharmaceutical ingredients (APIs) Sun, 2013. Metal cII atom is coordinated in a slightly distorted octahedral environment ], in the axial sites. The symmetry-unique purine ring system is essentially planar, with a maximum deviation of 0.030 (2) Å for N3 and the bonded methyl C atoms C4 and C5 deviate from this mean plane by −0.118 (3) and 0.136 (2) Å, respectively.The molecular structure of (I)t Table 1 by four et al., 1995iii = 2.829 (3) Å and O4⋯O1iv = 2.780 (2) Å; symmetry codes: (iii) −x, −y, −z; (iv) x, y, z + 1] between a coordinating water molecule and a carbonyl group of a symmetry-related theophylline group. The mononuclear units are connected into a layer parallel to (010)  Å; symmetry code: (ii) x, −y + z + In the crystal, the coordinating water molecules are involved in various hydrogen-bonding interactions Table 2. A (8) g0) Fig. 2, which i0) Fig. 2 by hydroA search of the Cambridge Structural Database  in water (15 ml) was then added. The resulting solution was kept in air and, after several days, colourless block-shaped crystals were obtained.Theophylline  was dissolved in water (20 ml). An aqueous solution (15 ml) of NaOH  was added slowly. MgClUiso(H) = 1.2Ueq(C) or 1.5Ueq(C). H atoms bonded to O atoms were located in difference Fourier maps and were refined with a distance restraint of O—H = 0.87 (1) Å. The isotropic displacement parameters were refined freely.Crystal data, data collection and structure refinement details are summarized in Table 310.1107/S2056989015003758/lh5752sup1.cifCrystal structure: contains datablock(s) I, LOU. DOI: 10.1107/S2056989015003758/lh5752Isup2.hklStructure factors: contains datablock(s) I. DOI: 1050901CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Two μ3-bridging I− anions are linked by three AgI ions, leading to the formation of a dicapped triangular motif with Ag⋯Ag separations in the range 3.0823 (5)–3.2999 (5) Å. Each AgI atom exhibits a distorted tetrahedral geometry, with coordination to two I atoms and two P atoms from bis(diphenylphosphanyl)methane ligands. In the crystal, the I− anion is linked to the ptu molecule through two N—H⋯I hydrogen bonds [graph-set motif R21(6)]. These N—H⋯I hydrogen bonds, in addition to weak C—H⋯S and C—H⋯I hydrogen bonds, form zigzag chains along [010]. Two of the phenyl rings of two dppm ligands are disordered over two sets of sites with refined occupancies of 0.557 (16) and 0.443 (16).The title complex, [Ag For the al. 2015.3I2(C25H22P2)3]I·C7H8N2S = 0.039wR(F2) = 0.104S = 1.0814160 reflections983 parameters216 restraintsH-atom parameters constrainedmax = 1.16 e Å−3Δρmin = −1.04 e Å−3ΔρAPEX2  used to solve structure: SHELXS97  I. DOI: 10.1107/S2056989015017120/lh5785Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989015017120/lh5785fig1.tif. DOI: The molecular structure with displacement ellipsoids drawn at the 50% probability level. All H atoms and the minor component of disorder are omitted for clarity.Click here for additional data file.10.1107/S2056989015017120/lh5785fig2.tif. DOI: Part of the crystal structure showing intermolecular N—H⋯I, C—H⋯S and C—H⋯I hydrogen bonds as dashed lines, forming a chain along [010].1424053CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Scientific Reports6: Article number: 2086410.1038/srep20864; Published online: 02122016; Updated: 04292016This Article contains typographical errors.In the Results section under subheading ‘Impact of ZLD1039 on breast cancer cell growth’,50 values of 0.99 ± 0.23 and 0.089 ± 0.019 μM, respectively”.“Among the cell lines, MCF-7 and ZR-75-1 were the most sensitive to ZLD1039 with ICshould read:50 values of 0.99 ± 0.23 and 1.089 ± 0.019 μM, respectively”.“Among the cell lines, MCF-7 and ZR-75-1 were the most sensitive to ZLD1039 with ICIn Figure 3d, the x-axis ‘1–8 days of treatment’ was incorrectly given as ‘0–7 days of treatment’. The correct Figure 3d appears below as Fig. 1


Z′ = 2) oriented almost perpendicular to each other [dihedral angle between the central core of each molecule = 77.95 (3)°]. The two molecules exhibit similar conformations with an extended structure and are linked by bifurcated hydrogen bonds into a ribbon along the a-axis direction.The title compound crystallizes with the two molecules in the asymmetric unit  oriented almost perpendicular to each other [dihedral angle between the central core of each molecule = 77.95 (3)°]. The two molecules exhibit similar conformations with an extended structure. An intramolecular C—H⋯N hydrogen bond occurs in each molecule. The two molecules are linked by a bifurcated N—H⋯ hydrogen bond involving the NH group in molecule A as donor. They are further linked into a ribbon along the a-axis direction by further bifurcated N—H⋯ hydrogen bonds involving the NH group in molecule B as donor. C—H⋯O interactions are also observed.The title compound, C E)-(methoxyimino){2-[(2-methylphenoxy)methyl]phenyl}acetate] derivatives are broad spectrum fungicides  labeled A and B and shown in Fig. 1A, the nitro group is coplanar with the p-nitrophenyl ring . The central ethane hydrazide moiety (N2A/N3A/C8A/O3A) is strictly planar with an r.m.s. deviation of 0.000 Å for the fitted atoms. The dihedral angles between this moiety and the adjacent aromatic are 18.99 (4)° for the nitrobenzylidene ring (C1A–C6A) and 62.20 (4)° for the benzene ring (C11A–C16A).The title compound crystallizes with two molecules in the asymmetric unit , 0.043 (2) and 0.127 (2) Å, respectively]. The central ethane hydrazide moiety (N2B/N3B/C8B/O3B) is planar (r.m.s. deviation = 0.002 Å). The dihedral angles between this moiety and the adjacent aromatic rings are 12.43 (4)° for the nitrobenzylidene ring (C1B–C6B) and 57.99 (4)° for the benzene ring (C11B–C16B).In molecule A and B are oriented almost perpendicular to each other, the dihedral angle between their central cores (atoms C7 N2 N3 and C8) being 77.95 (3)°.Molecules For both molecules, bond lengths and angles are all within the normal ranges; however, comparisons with similar molecules cannot be made as there are no similar overall structures although, of course, their fragments exist.A—H17B⋯N4A and C17B—H17C⋯N4B; Table 1An intramolecular hydrogen bond . The molecules are further linked into a ribbon along the a-axis direction a bifurcated N3B—H3B⋯ hydrogen bond involving the corresponding NH group in the other independent molecule, as shown in Fig. 2The two independent molecules are linked by a bifurcated hydrogen bond Table 1 between A search of the Cambridge Structural Database -2-Methoxyimino-2-{2-[(2-methylphenoxy)methyl]phenyl}ethanehydrazide  was refluxed with p-nitrobenzaldehyde  in the presence of 5 drops of glacial acetic acid in 20 ml absolute ethanol for about 10 h to get a white-colored product. This was dissolved in methanol and white crystals were obtained by slow evaporation.(2isoU(H) = 1.5Ueq(C) for methyl H atoms and = 1.2eqU(C) for other H atoms.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015004569/hg5434sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989015004569/hg5434Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989015004569/hg5434Isup3.cmlSupporting information file. DOI: 1052231CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The cations also form base pairs via N—H⋯O and C—H⋯N hydrogen bonds.The N 12H10N5O+·NO3−, the adenine unit has an N9-protonated N(7)—H tautomeric form with non-protonated N1 and N3 atoms. The dihedral angle between the adenine ring system and the phenyl ring is 51.10 (10)°. The typical intramolecular N7—H⋯O hydrogen bond with an S(7) graph-set motif is also present. The benzoyladeninium cations also form base pairs through N—H⋯O and C—H⋯N hydrogen bonds involving the Watson–Crick face of the adenine ring and the C and O atoms of the benzoyl ring of an adjacent cation, forming a supramolecular ribbon with R22(9) rings. Benzoyladeninum cations are also bridged by one of the oxygen atoms of the nitrate anion, which acts as a double acceptor, forming a pair of N—H⋯O hydrogen bonds to generate a second ribbon motif. These ribbons together with π–π stacking interactions between the phenyl ring and the five- and six-membered adenine rings of adjacent molecules generate a three-dimensional supramolecular architecture.In the title molecular salt, C N6-substituted adenine compounds continue to attract interest due to their biological activity as they can act as plant hormones and have anti-allergenic, antibacterial, antiviral and antifungal properties et al., 1997et al., 2003et al., 2005et al., 2011Non-covalent interactions, such as hydrogen bonding, halogen bonding and π–π interactions play major roles in molecular recognition and pharmaceutical drug design processes —H tautomeric form with N9 protonated and N1, N3 non-protonated. The internal angles at N7 [C8—N7—C5 = 108.9 (2)°] and N9 [C8—N9—C4 = 107.9 (2)°] are similar as both carry hydrogen atoms  ring motif. A similar bond was found in the crystal structure of the neutral N6-benzoyl adenine via N—H⋯O and C—H⋯N hydrogen bonds  Å . The other face of the phenyl ring makes offset π–π contacts with both the imidazole [Cg1⋯Cg3ii = 3.7213 (17) Å] and the pyrimidine rings , Fig. 3Cg1, Cg2 and Cg3 are the centroids of the imidazole, pyrimidine and phenyl rings, respectively. Similar contacts are found in related structures s Table 1 involvinN6-substituted adenines, adeninium salts and their metal complexes have been investigated in a variety of crystalline environments. Neutral molecules include N6-benzyladenine  and N6-benzoyladenine–dl-tartaric acid (1:1). In these, the benzoyladenine molecule has a conformation similar to that reported for the neutral benzoyladenine crystal structure , a few drops of nitric acid were added. The resulting solution was warmed over a water bath for half an hour and then kept at room temperature for crystallization. After a week colourless prismatic crystals of (I)To a hot methanol solution of Uiso(H) = 1.2Ueq.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015024871/sj5489sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989015024871/sj5489Isup2.hklStructure factors: contains datablock(s) I. DOI: 10.1107/S2056989015024871/sj5489Isup3.pdfSupporting information file. DOI: Click here for additional data file.10.1107/S2056989015024871/sj5489Isup4.cmlSupporting information file. DOI: 1444600CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The free 2,4-D anions are linked to the complex units through duplex water–carboxylate O—H⋯O hydrogen bonds through the coordinating water molecules. In the crystal, inter-unit O—H⋯O hydrogen-bonding interactions involving coordinating water molecules as well as the solvent water molecule (occupancy 0.5) with carboxylate O-atom acceptors, give a layered structure lying parallel to (001), in which π–π ligand–cation interactions [minimum ring centroid separation = 3.6405 (17) Å] and a short O—H⋯Cl interaction are also found.In the crystal structure of the title magnesium salt of the phenoxy herbicide acetic acid , [Mg(C These include discrete monomeric {[MgL2(H2O)4] [L = 2-(2-fluorophenoxy)acetate 5]·L }n  (H2O)5](C8H5Cl2O3)·0.5H2O, was obtained from the reaction of 2,4-D with MgCO3 in aqueous ethanol and its crystal structure is reported herein.The phenoxyacetic acids comprise an important group of chemicals which has among its members those ring-substituted representatives having selective herbicidal activity, 6 complex units have, as expected, essentially octahedral stereochemistry [Mg—O bond length range = 2.031 (2)–2.094 (2) Å], comprising a carboxylate O-donor from a monodentate 2,4-D− ligand and five water molecules. The free 2,4-D− counter-anion is linked to the complex unit through an unusual duplex water–carboxylate O—H⋯O hydrogen-bonding association involving the coordinating water molecules O1W and O2W  being 179.0 (2) and 174.8 (2)° (ligand A), and 175.7 (2) and 178.7 (2)° (anion B), respectively]. This contrasts with the parent acid 2,4-D  Å] is also observed [for symmetry codes (i) and (iii), see: Table 1In the crystal of the title compound, inter-unit O—H⋯O hydrogen-bonding interactions Table 1 involvin3 to 15 ml of a hot aqueous solution of acetic acid (0.1 mmol) in ethanol–water (1:10 v/v). After completion of the reaction, excess MgCO3 was removed by filtration and the solution was allowed to evaporate at room temperature, providing colourless prisms of the title compound from which a specimen was cleaved for the X-ray analysis.The title compound was synthesized by the addition of excess MgCOUiso(H) = 1.5Ueq(O). Other H atoms were included in the refinement at calculated positions (aromatic C—H = 0.95 Å or methylene 0.99 Å), with Uiso(H) = 1.2Ueq(C), using a riding-model approximation. The site-occupancy factor for the water molecule of solvation was determined as 0.502 (4) and was subsequently fixed at 0.50.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S1600536814019357/wm5045sup1.cifCrystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536814019357/wm5045Isup2.hklStructure factors: contains datablock(s) I. DOI: 1021287CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Within the complex cation, the CrIII atom is coordinated by six O atoms of six urea ligands, displaying a slightly distorted octahedral coordination environment. The Cr—O bond lengths involving the urea ligands are in the range 1.9534 (13)–1.9776 (12) Å. The Cr2O72− anion has a nearly staggered conformation, with a bridging angle of 130.26 (10)°. The individual components are arranged in rows extending parallel to [100]. The Br− anion links the complex cation, as well as the solvent water molecule, through N—H⋯Br and O—H⋯Br hydrogen-bonding interactions. The supramolecular architecture also includes N—H⋯O and O—H⋯O hydrogen bonding between urea N—H and water O—H donor groups and the O atoms of the Cr2O72− anion as acceptor atoms, leading to a three-dimensional network structure.The title bromide salt, [Cr{CO(NH On the other hand, CrVI is toxic and recognized as a carcinogen to humans and wildlife. The dichromate ion is environmentally important due to its high toxicity  in aqueous solution have been investigated. It was found that [Cr(urea)6]3+ is suitable to target these oxoanions Cl·H2O has been reported , b = 10.393 (1), c = 17.794 (3) Å and β = 94. 86 (2)°. Within our broader study of CrIII complexes as industrial materials Br·H2O, (I)Counter-ionic species in coordination compounds play important roles in chemistry, pharmacy, molecular assembly, biology and catalysis, as well as contributing significantly to environmental pollution; however, their binding characteristics have not received much recognition Cl·H2O investigated previously In order to check if compound (I)III ion is coordinated by six urea ligands through oxygen atoms with CrA—OA bond lengths ranging from 1.9534 (13) to 1.9776 (12) Å, and with OA—CrA—OA bond angles in the range 85.10 (5)–92.95 (5)°. The CrA—OA bond lengths involving the urea ligand are in good agreement with the value of 1.9630 (17) Å for [Cr(urea)6](BF4)3 2(cyclam)]ClO4 (cyclam)]ClO4 (cyclam)](ClO4)2·0.5H2O 2(cyclam)]NO2 (acac)] °, 173.94 (5)°, and 175.89 (5)°, respectively. The bond lengths within the urea ligand are in the ranges of 1.263 (2)–1.276 (2) and 1.316 (2)–1.328 (2) Å for C=O and C—N bonds, respectively. The C=O bonds are slightly longer than that in free non-coordinating urea 2Cr2O7, the tetrahedral CrO4 groups are in an almost eclipsed conformation  and 1.8011 (17) Å are longer than the terminal CrB—OB bonds that are in the range of 1.6014 (16)–1.6299 (14) Å. The Cr1B—O7B—Cr2B bridging angle in the complex anion is 130.26 (10)°. The OB—CrB—OB bond angles in the two tetrahedral CrO4 groups are between 105.21 (8) and 110.98 (10)°, indicating slight angular distortions.It is of interest to compare the conformation of Cr6]3+ moiety in compound (I)2O72− anions due to its high positive charge and the large number of hydrogen-bond donor groups of its six urea ligands.It is confirmed that the Br3·3H2O was used as the starting material and was prepared according to literature procedures , dissolved in 10 mL of water, was added to this solution. The mixture was refluxed at 353 K for 10 min and then cooled to room temperature. Green crystals of (I)2)2}6](Cr2O7)Br·H2O: C, 9.92; H, 3.61; N, 23.14%; found: C, 10.32; H, 3.08; N, 23.38%.All chemicals were reagent-grade materials and used without further purification. Chromium(III) tribromide hexahydrate was obtained from Aldrich Chemical Co. and used as supplied. [Cr(urea)Uiso(H) = 1.2Ueq(N). H atoms of the solvent water molecule were found from difference maps and refined with Uiso(H) = 1.2Ueq(O) and restrained to O—H = 0.84 (1) and H⋯H = 1.36 (2) Å.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015019258/wm5225sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989015019258/wm5225Isup2.hklStructure factors: contains datablock(s) I. DOI: 1430688CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the crystal, molecules are linked  33H26F2N2O2, both pyrrolidine rings of the pyrrolizidine moiety adopt an envelope conformation. The difluorophenyl group is oriented at an angle of 54.3 (1)° with respect to the oxindole moiety. The crystal packing features an N—H⋯O hydrogen bond, which forms an R22(8) motif, and a C—H⋯O interaction, which generates a C(8) chain along [010]. In addition, this chain structure is stabilized by C—H⋯π interactions. In one of the pyrrolidine rings, the methylene group forming the flap of an envelope and the H atoms of the adjacent methylene groups are disordered over two sets of sites, with site-occupancy factors of 0.571 (4) and 0.429 (4)In the title pyrrolizidine derivative, C H-indole-2,3-dione) has been exploited extensively as a key intermediate in organic multicomponent reactions due to its antibacterial   -1′,2,2′,3,5′,6′,7′,7a′-octahydro-1H-indan-2-spiro-3′-(3′H- pyrrolizine)-1′-spiro-3′′-1H-indoline-1,2′′,3-trione (IV) sp3 hybridization. The fluorine atoms, F1 and F2, deviate by 0.006 (2) and −0.010 (2) Å, respectively, from the plane of the benzene ring (C1–C6) to which they are attached. The oxindole group system is planar with maximum deviations from its plane for the carbonyl C30 [−0.048 (2) Å] and O2 atoms [−0.122 (1) Å]. The difluorophenyl group is oriented at an angle of 54.3 (1)° with respect to the oxindole moiety. The benzene rings C7–C12 and C21–C26 are oriented at a dihedral angle of 52.7 (1)°. The dihedral angles subtended by these two benzene rings with respect to the oxindole moiety are 21.2 (1) and 31.6 (1)°, respectively. The dihedral angle between the benzene rings of the biphenyl group is 44.3 (1)°. Atom C18 of the pyrrolizidine ring system, and the adjacent methylene group H atoms, are disordered over two sets of sites, with the site-occupancy factors of 0.571 (4) and 0.429 (4).The sum of the angles at N1 of the pyrrolizidine ring system (340°) is in accordance with q2 = 0.393 (2) Å and ϕ = −167.8 (2)° for N1/C20/C14–C16 ring, and q2 = 0.280 (3) Å and ϕ = 104.8 (4)° for N1/C16–C19. In the N1/C20/C14–C16 ring, atom C14 deviates by 0.594 (2) Å from the least-squares plane through the remaining four atoms, whereas in the N1/C16-C19 ring, atoms C18 and C18′ deviate by −0.401 (5) and 0.434 (4) Å, respectively, from the plane through the remaining four atoms.In the pyrrolizidine ring system, both pyrrolidine rings adopt envelope conformations; the puckering parameters are: via N—H⋯O hydrogen bonds into inversion dimers, generating an C(8) chains propagating along [010]; see Fig. 4C(8) chains propagating along [010]; see Fig. 5The geometry of interactions observed in this structure are given in Table 1To a solution of isatin (1 mmol) and L-proline (1 mmol) in methanol (25 ml), 1-[4-phenyl]3-phenylprop-2-en-1-one (1 mmol) was added and the solution was refluxed for 6–8 h. The completion of reaction was monitored by thin layer chromatography. After completion, the reaction mixture was poured onto crushed ice. The precipitate obtained was filtered and dried at room temperature. Suitable crystals were obtained by slow evaporation of a solution of the title compound in acetonitrile at room temperature.Uiso(H) = 1.5Ueq(C) for methyl H atoms and 1.2Ueq(C) for other H atoms. Atom C18 is disordered over two positions, with the major component having 0.571 (4) occupancy. Pairs of C—C distances were restrained to 1.54 (1) Å. The temperature factor of C18′ was set to that of C18 with the EADP instruction of SHELXL2014/7  I, global. DOI: 10.1107/S2056989015012931/gk2637Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989015012931/gk2637Isup3.cmlSupporting information file. DOI: 1410535CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The platinum(II) complex with notable antitumor activity shows a slightly distorted square-planar coordination and intramolecular C—H⋯Cl and intermolecular N—H⋯Cl and C—H⋯O hydrogen bonds. 10H6NO2)Cl(C5H11N)], crystallizes with one molecule in the asymmetric unit. The PtII cation has a slightly distorted square-planar coordination environment defined by a chloride anion, the quinoline N atom and a carboxylate O atom of the bidentate quinaldate ligand and a piperidine N atom. An intramolecular C—H⋯Cl hydrogen bond occurs. In the crystal, molecules are stacked into columns along the c axis by the formation of N—H⋯Cl and C—H⋯O hydrogen bonds.The title compound, [Pt(C The Cl− and the PtII atoms are displaced from the least-squares plane of the quinoline ring and all other coordinating atoms by 0.2936 (7) and 0.0052 (1) Å, respectively. The piperidine ring adopts a chair conformation and is almost perpendicular to the coordination plane of the PtII cation [dihedral angle between the best plane through the piperidine ring and the four atoms coordinating to the PtII cation = 79.66 (13)°]. Bond lengths are normal and agree well with related platinum compounds ] , prepared according to the synthetic protocol of Da et al. (2001v/v) was added gradually while stirring at room temperature for 1 h. The reaction mixture was stirred further for 4 h. The precipitated yellow substance was filtered off and washed consecutively with a 0.1 M HCl solution (2 × 2 ml), warm water (3 × 2 ml) and cold ethanol (2 ml). The product was then dried in a vacuum at 323 K for 4 h. The yield was 80%. Single crystals suitable for X-ray diffraction analysis were obtained by slow evaporation from an ethanol–water (1:1 v/v) solution at room temperature. Positive ESI–MS: m/z 1973 [4M + Na]+, 1483 [3M + Na]+, 998 [2M + Na]+, 510 [M + Na]+, 977 [2M + H]+, 489 [M + H]+; IR (KBr) cm−1: 3192 (νNH); 3080, 2930, 2866 (νCH); 1678 (νC=O); 1592, 1459 (νC=C arom); 1334 (νC—O); 1H NMR : 9.50 , 8.51 , 8.06 , 7.91–7.88 , 7.71 , 3.52 , 3.27  = 12.5 Hz, C510HNH), 1.76–1.61 , 4.00 .The starting complex K[PtCl al. 2001, was dis2 and N—H = 0.93 Å for amino H atoms, with Uiso = 1.2Ueq.All H atoms were refined using a riding model, with C—H = 0.95 Å for aromatic, C—H = 0.99 Å for CH10.1107/S160053681401191X/wm0005sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S160053681401191X/wm0005Isup2.hklStructure factors: contains datablock(s) I. DOI: 1004305CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The Cu—Cl bond measures 2.2287 (9) Å, and the two Cu—S bonds are significantly different from each other, with values of 2.2270 (10) and 2.2662 (10) Å. Also, the S—Cu—Cl angles differ, with values of 113.80 (4) and 124.42 (4)°, while the S—Cu—S angle is 121.51 (4)°. The two imidazole rings are almost parallel, making a dihedral angle of 2.1 (2)°. In the crystal, the shortest C—H⋯Cl interactions stabilize a three-dimensional network with molecules linked into centrosymmetric dimers that are stacked along the b-axis direction.The molecular structure of the title compound, [CuCl(C DOI: 10.1107/S1600536814024404/zq2228Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S1600536814024404/zq2228fig1.tif. DOI: Molecular structure of the title compound with anisotropic displacement parameters drawn at the 50% probability level.1032971CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The title compound comprises a 2-iminopyridine ring fused with a cyclooctane ring, which adopts a twist boat–chair conformation. Intermolecular C—H⋯N interactions form  25H24ClN3, comprises a 2-iminopyridine ring fused with a cyclooctane ring, which adopts a twist boat–chair conformation. In the crystal, C—H⋯N interactions form R22(14) ring motifs and molecules are further connected by weak C—H⋯π interactions. The resulting supramolecular structure is a two-dimensional framework parallel to the ab plane.The title compound, C They have gained importance in the medicinal and pharmaceutical fields due to their broad spectrum of biological activity, including anti-inflammatory, analgesic, antimicrobial, anticonvulsant, antitubercular ° shows the linearity of the cyano group, a feature systematically observed in carbonitrile compounds. Nitrile atoms C38 and N2 are displaced from the mean plane of the pyridine ring by 0.0258 (1) and 0.0363 (1) Å, respectively. The imino C1=N1 bond length is 1.286 (2) Å. The imino group is nearly coplanar with the pyridine ring, as indicated by the N1=C1—N3—C5 torsion angle of −178.89 (14)°. The chlorobenzene ring is attached to the pyridine ring with a C2=C3—C31 C36 torsion angle of 100.99 (19)°, indicating a (+)anticlinal conformation. The C33 C34 C35 bond angle of 121.11 (15)° deviates from 120° due to the presence of the chlorine substituent. The chlorine atom bonded to C34 deviates by 0.0446 (1) Å from the mean plane of the phenyl ring. The chlorine is attached to the benzene ring with a C32 C33 C34—Cl1 torsion angle of 178.95 (13)°. In the pyridine ring, the formal double bonds [C4=C5 = 1.375 (2) and C2=C3 = 1.369 (2) Å] are longer than standard C=C bonds (1.34 Å), while the other bond lengths are slightly shorter than standard C—C and C—N bond lengths, evidencing that there is a homo-conjugation effect for this ring.The molecular structure of the title compound is shown in Fig. 1et al., 1995ab plane.In the crystal, pairs of C—H⋯N interactions form b]pyridine-3-carbonitrile -5,6,7,8,9,10-hexahydrocycloocta[p-toluenesulfonic acid (0.5 mmol) was added. The reaction mixture was refluxed for 2–3 h. After completion of the reaction (followed by thin-layer chromatography), the mixture was poured into crushed ice and extracted with ethyl acetate. The excess of solvent was removed under reduced pressure and the residue was chromatographed using a petroleum ether/ethyl acetate mixture (97:3 v/v) as eluent, to afford the pure product. The product was recrystallized from ethyl acetate, affording colourless crystals .Cyclooctanone (1 mmol), 4-chlorobenzaldehyde (1 mmol) and malononitrile (1 mmol) were mixed in ethanol (10 ml), and 2). Imine atom H1 was found in a difference map and refined freely, with the N—H distance restrained to 0.84 (2) Å. Isotropic displacement parameters for H atoms were calculated as Uiso(H) = 1.2Ueq(C) for CH and CH2 groups, while the Uiso factor for H1 was refined. Crystal data, data collection and structure refinement details are summarized in Table 2.C-bound H atoms were placed in calculated positions and allowed to ride on their carrier atoms, with C—H = 0.93 (aromatic CH) or 0.97 Å  global, I. DOI: 10.1107/S160053681401962X/bh2503Isup2.hklStructure factors: contains datablock(s) I. DOI: 1021949CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


We used Sca1154Q/2Q mice, an established knock-in mouse model of the polyglutamine disease spinocerebellar ataxia type 1 (SCA1), which replicates human SCA1 features including ataxia, cognitive impairment, and neuronal death. We found that Sca1154Q/2Q mice exhibited greater synaptic instability than controls, without synaptic loss, in the cerebral cortex, where obvious neuronal death is not observed, even before the onset of distinct symptoms. Interestingly, this abnormal synaptic instability was evident in Sca1154Q/2Q mice from the synaptic developmental stage, and persisted into adulthood. Expression of synaptic scaffolding proteins was also lower in Sca1154Q/2Q mice than controls before synaptic maturation. As symptoms progressed, synaptic loss became evident. These results indicate that aberrant synaptic instability, accompanied by decreased expression of scaffolding proteins during synaptic development, is a very early pathology that precedes distinct neurological symptoms and neuronal cell death in SCA1.Late-onset neurodegenerative diseases are characterized by neurological symptoms and progressive neuronal death. Accumulating evidence suggests that neuronal dysfunction, rather than neuronal death, causes the symptoms of neurodegenerative diseases. However, the mechanisms underlying the dysfunction that occurs prior to cell death remain unclear. To investigate the synaptic basis of this dysfunction, we employed  Many late-onset neurodegenerative diseases, including Alzheimer’s, Parkinson’s, and prion and polyglutamine diseases, share common features, such as the aggregation of toxic proteins in neurons, and progressive neuronal cell death1ATXN1 geneSca1154Q/2Q knock-in mouse model, harbouring 154 CAG repeats within the endogenous ATXN1 locus, closely reproduces the features of human SCA16Sca1154Q/2Q mice is much higher than that in human patients, another knock-in SCA1 mouse model harbouring 78 CAG repeats, similar to the number in patients, displays only mild behavioural deficits late in lifeSca1154Q/2Q mice are suitable for studying symptom progression. Sca1154Q/2Q mice develop motor learning impairment before any obvious Purkinje cell death occurs or nuclear inclusions form in the cerebellumSca1154Q/2Q mice show nuclear inclusions in pyramidal neurons, and cognitive deficits are observed without evident neuronal lossMany neurodegenerative diseases are attributed to multiple factors, including genetic and environmental predispositions. On the other hand, spinocerebellar ataxia type 1 (SCA1), a polyglutamine disease, is a monogenic disorder caused by the expansion of an unstable CAG trinucleotide repeat tract encoding a polyglutamine stretch in the Sca1154Q/2Q knock-in mice to elucidate the synaptic basis of neuronal dysfunction. We analysed the dynamics, morphology, and density of dendritic protrusions, which are excitatory postsynaptic structures classified into mature ‘spines’ and immature ‘filopodia’. These features are strongly associated with synaptic developmentSca1154Q/2Q knock-in mice in vivo, maintaining contributions from peripheral tissues and non-neuronal cells expressing mutant ataxin-1, as well as neurons. To evaluate neuronal dysfunction while excluding the effects of neuronal death, we focused on the cerebral cortex and hippocampus, in which apparent neuronal death does not occur despite the presence of cognitive dysfunction in both Sca1154Q/2Q mice and human SCA1 patients5In the present study, we focused on SCA1 as a genetic model of neurodegenerative disease, and used Sca1154Q/2Q mice are observed by 5 weeks of age, and spatial and fear memory deficits by 8 weeks. Although nuclear inclusions of mutant ataxin-1 are observed by 6 weeks, there is no neuronal death in the limbic area during such early stages of the diseaseSca1154Q/2Q mice as a possible early SCA1 phenotype. We performed in vivo two-photon imaging in layer 1 dendrites of the primary somatosensory cortex in Sca1154Q/2Q and control Sca12Q/2Q mice, and analysed the morphology, formation, and elimination of dendritic protrusions over a 1 h period under anaesthesia  vs Sca1154Q/2Q (0.33 ± 0.05/μm), p = 0.4532; spines: Sca12Q/2Q (0.31 ± 0.02/μm) vs Sca1154Q/2Q (0.24 ± 0.03/μm), p = 0.0909; filopodia: Sca12Q/2Q (0.070 ± 0.005/μm) vs Sca1154Q/2Q (0.09 ± 0.02/μm), p = 0.4159; unpaired t-test]. There were also no significant differences between 4-week-old Sca12Q/2Q and Sca1154Q/2Q mice in the number of spines or filopodia as a percentage of the total protrusions (Sca12Q/2Q (81 ± 1%) vs Sca1154Q/2Q (76 ± 2%), p = 0.0747; filopodia: Sca12Q/2Q (19 ± 1%) vs Sca1154Q/2Q (24 ± 2%), p = 0.0747; unpaired t-test]. Next, we analysed the dynamics of the protrusions in order to estimate synaptic stability. Notably, we found that the rates of formation and elimination of spines over 1 h were significantly higher in Sca1154Q/2Q mice than in Sca12Q/2Q mice (Sca12Q/2Q (3.6 ± 0.9%) vs Sca1154Q/2Q (9 ± 2%), p = 0.0101; elimination rate: Sca12Q/2Q (4.5 ± 0.8%) vs Sca1154Q/2Q (12 ± 2%), p = 0.0017; unpaired t-test]. The elimination rate of filopodia over 1 h was also significantly higher in Sca1154Q/2Q mice, but the difference in their formation rate did not reach statistical significance (Sca12Q/2Q (27 ± 6%) vs Sca1154Q/2Q (35 ± 4%), p = 0.2711; elimination rate: Sca12Q/2Q (23 ± 4%) vs Sca1154Q/2Q (42 ± 7%), p = 0.0341; unpaired t-test]. Anaesthetics can increase the formation of filopodia within a 1 h periodin vivo imaging over 48 h, during which time the mice were allowed to recover from the anaesthesia after the first imaging session and were returned to their home cages until the next session. We confirmed that both formation and elimination rates of spines in Sca1154Q/2Q mice were also significantly higher than those in Sca12Q/2Q mice over a 48 h period (Sca12Q/2Q (8 ± 1%) vs Sca1154Q/2Q (23 ± 3%), p < 0.0001; elimination rate: Sca12Q/2Q (10 ± 1%) vs Sca1154Q/2Q (28 ± 4%), p = 0.0003; unpaired t-test]. Neither the formation nor elimination rates of filopodia over 48 h were significantly different between groups, probably owing to the very high rates measured over 48 h even in control mice (Sca12Q/2Q (59 ± 9%) vs Sca1154Q/2Q (52 ± 9%), p = 0.5763; elimination rate: Sca12Q/2Q (70 ± 10%) vs Sca1154Q/2Q (72 ± 7%), p = 0.8919; unpaired t-test]. These data indicate that Sca1154Q/2Q mice show abnormal synaptic instability during synaptic development, before the onset of obvious symptoms, and that these altered dynamics are detectable by imaging under anaesthesia during a 1 h period.Motor learning impairments in esthesia . Dendrits of age  . The number of spines as a percentage of total protrusions was significantly lower in Sca1154Q/2Q mice than in Sca12Q/2Q mice at 6 weeks (Sca12Q/2Q (88 ± 2%) vs Sca1154Q/2Q (81 ± 2%), p = 0.0284; unpaired t-test], whereas that of filopodia was higher (Sca12Q/2Q (12 ± 2% vs Sca1154Q/2Q (19 ± 2%), p = 0.0284; unpaired t-test]. Spine dynamics were significantly greater in Sca1154Q/2Q mice than in Sca12Q/2Q mice at 6 weeks of age (Sca12Q/2Q (2.3 ± 0.5%) vs Sca1154Q/2Q (9 ± 2%), p = 0.0018; elimination rate: Sca12Q/2Q (2.1 ± 0.6%) vs Sca1154Q/2Q (13 ± 2%), p < 0.0001; unpaired t-test]. Regarding the filopodium dynamics of 6-week-old Sca1154Q/2Q mice, the elimination rate was significantly higher, but the formation rate was not different from that in Sca12Q/2Q mice (Sca12Q/2Q (18 ± 7%) vs Sca1154Q/2Q (36 ± 6%), p = 0.0785; elimination rate: Sca12Q/2Q (14 ± 3%) vs Sca1154Q/2Q (35 ± 7%), p = 0.0100; unpaired t-test]. In 8-week-old Sca1154Q/2Q mice, total protrusion and spine densities were significantly lower than those in age-matched Sca12Q/2Q mice, whereas filopodium density was not different between the two groups (Sca12Q/2Q (0.36 ± 0.02/μm) vs Sca1154Q/2Q (0.30 ± 0.02/μm), p = 0.0343; spines: Sca12Q/2Q (0.33 ± 0.02/μm) vs Sca1154Q/2Q (0.25 ± 0.01/μm), p = 0.0175; filopodia: Sca12Q/2Q (0.033 ± 0.004/μm) vs Sca1154Q/2Q (0.044 ± 0.006/μm), p = 0.1621; unpaired t-test]. The number of spines as a percentage of the total protrusions was significantly lower in 8-week-old Sca1154Q/2Q mice than in Sca12Q/2Q mice (Sca12Q/2Q (90 ± 1%) vs Sca1154Q/2Q (85 ± 2%), p = 0.0403; unpaired t-test], whereas that of filopodia was higher in 8-week-old Sca1154Q/2Q mice than in Sca12Q/2Q mice (Sca12Q/2Q (10 ± 1%) vs Sca1154Q/2Q (15 ± 2%), p = 0.0403; unpaired t-test]. Both formation and elimination rates of spines in 8-week-old Sca1154Q/2Q mice were significantly higher than those in Sca12Q/2Q mice (Sca12Q/2Q (2.7 ± 0.7%) vs Sca1154Q/2Q (13 ± 2%), p < 0.0001; elimination rate: Sca12Q/2Q (2.0 ± 0.8%) vs Sca1154Q/2Q (12 ± 4%), p = 0.0176; unpaired t-test]. The formation rate of filopodia in 8-week-old Sca1154Q/2Q mice was higher than that in Sca12Q/2Q, whereas the elimination rate was not significantly different (Sca12Q/2Q (5 ± 3%) vs Sca1154Q/2Q (25 ± 8%), p = 0.0134; elimination rate: Sca12Q/2Q (21 ± 8% vs Sca1154Q/2Q (42 ± 11%), p = 0.1166; unpaired t-test]. These data indicate that SCA1 mice have immature dendritic morphology and a loss of dendritic protrusions associated with persisting synaptic instability and the progression of SCA1 symptoms.We demonstrated that synaptic instability occurs in SCA1 mice before the onset of distinct symptoms at 4 weeks of age. Next, we evaluated the progression of synaptic pathology in SCA1 mice until 8 weeks of age, by which time dendritic spines have normally stabilised and the density of filopodia has reached a minimumice at 6  and 8 weice at 6 . In 6-wee groups  , whereas at 12 weeks, dendritic protrusion density was significantly lower in Sca1154Q/2Q mice than in Sca12Q/2Q mice (Sca12Q/2Q (1.53 ± 0.06/μm) vs Sca1154Q/2Q (1.28 ± 0.04/μm), p = 0.0011; unpaired t-test]. An abnormal frequency distribution of dendritic protrusion width was observed in Sca1154Q/2Q mice, particularly at 12 weeks of age, when the distribution curve shifted to the left . The mean dendritic protrusion width in 12-week-old Sca1154Q/2Q mice was lower than that in Sca12Q/2Q mice . These results show that the dendritic protrusion width in Sca1154Q/2Q mice decreased as SCA1 symptoms developed. An abnormal frequency distribution of protrusion length in Sca1154Q/2Q mice was evident at 5 weeks of age, and the frequency distribution curve was shifted to the right . No difference was observed in the mean length of dendritic protrusions between Sca1154Q/2Q and Sca12Q/2Q mice at either age . These results indicate that the protrusion lengths in Sca1154Q/2Q mice differ little from those in Sca12Q/2Q mice from early life through to adulthood. In summary, SCA1 mice demonstrated progressive deficits in dendritic protrusions in the hippocampus from adult ages./2Q mice . We choss of age   with EDTA-free complete protease inhibitors and PhosSTOP (Roche Applied Science). Immunoblotting was performed using the following antibodies: anti-Homer1b/c , anti-pan-Shank , anti-PSD95 , anti-mGluR5 , anti-NR2B , anti-GluR1 , anti-Bassoon , and anti-β-actin . Total protein (10 μg/lane) was separated on sodium dodecyl sulphate-polyacrylamide gels, transferred to immunoblot polyvinylidene difluoride membranes , incubated with 3% BSA in TBST  for 1 h at room temperature, and incubated with each primary antibody overnight at 4 °C. The membranes were washed in TBST and further incubated with anti-mouse/rabbit IgG-horseradish peroxidase conjugate . After washing in TBST, the membranes were developed with Super Signal West Dura or Femto extended duration substrate (Pierce) and analysed using a ChemiImager . Proteins were identified by band position relative to a molecular weight marker.t-test, one-way ANOVA followed by Tukey multiple-comparison test, two-way ANOVA followed by Bonferroni multiple-comparison test, or the Kolmogorov–Smirnov test. All statistical analyses were performed with GraphPad Prism . All data are presented as the mean ± SEM.To determine statistical significance, we used the Student How to cite this article: Hatanaka, Y. et al. Abnormalities in synaptic dynamics during development in a mouse model of spinocerebellar ataxia type 1. Sci. Rep.5, 16102; doi: 10.1038/srep16102 (2015).


In the title compound, the ring conformations of the tricycles are in an envelope, a half-chair and a chair. In the crystal, intermolecular O—H⋯O and C—H⋯O hydrogen bonds and C—H⋯π interactions link the molecules into a three-dimensional architecture. 36H44O10·C6H6, the dioxolane ring adopts an envelope conformation with the C atom bonded to the H atom as the flap, while the cyclohexene and cyclohexane rings are in half-chair and chair conformations, respectively. In the crystal, a pair of O—H⋯O hydrogen bonds with an R22(26) graph-set motif connect the benzoate molecules into an inversion dimer. The dimers are linked by a weak C—H⋯O interaction into a tape structure along [01-1]. The benzene molecule links the tapes through C—H⋯O and C—H⋯π interactions, forming a sheet parallel to (100).In the title compound, C The title compound has been obtained in our synthetic study of paclitaxel as a cyclization precursor to build the taxane skeleton  = 0.165 (2) Å and ϕ(2) = 114.5 (6)°. The flap atom C4 deviates from the mean plane of other atoms by 0.270 (3) Å. The cyclohexene ring (C5–C10), which is spiro-fused to the dioxolane ring, is in a half-chair conformation with puckering parameters of Q = 0.469 (2) Å, θ = 127.5 (2)°, ϕ(2) = 197.2 (3)°, Q(2) = 0.372 (2) Å and Q(3) = −0.285 (2) Å. Atoms C5 and C6 deviate from the mean plane of the other atoms by −0.493 (4) and 0.212 (4) Å, respectively. The cyclohexane ring (C24–C29) is in a chair conformation with puckering parameters Q = 0.587 (2) Å, θ = 4.6 (2)°, ϕ = 246 (3)°, Q(2) = 0.042 (2) Å and Q(3) = 0.585 (2) Å. The large substituents  are in the equatorial positions. The methoxymethoxy group (O42/C43/O44/C45) shows a helical form with torsion angles of 76.5 (3)° for C29—O42—C43—O44 and 64.8 (3)° for O42—C43—O44—C45 held by weak intramolecular C—H⋯O interactions  was provided according to the reported procedure (Nicolaou Uiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C). The H atom of hydroxy group (O41) was placed guided by difference maps and then treated as riding, with O—H = 0.84 Å and with Uiso(H) = 1.5Ueq(O). 13 problematic reflections were omitted from the final refinement.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989014026048/is5382sup1.cifCrystal structure: contains datablock(s) global, I. DOI: 10.1107/S2056989014026048/is5382Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989014026048/is5382Isup3.cmlSupporting information file. DOI: 1036428CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The asymmetric unit contains two Co2+ ions, one L3− anion originating from 5-(4-carboxyphenoxy)isophthalic acid (H3L), one OH− ligand, one 1,4-bis[(1H-imidazol-l-yl)methyl]benzene (bix) ligand and one disordered lattice water molecule (occupancy 0.25). The two Co2+ ions have different environments. One has an octahedral O4N2 coordination sphere, defined by four O atoms from three carboxylate groups and one OH− ligand, and two N atoms from two symmetry-related bix ligands. The other has a trigonal-bipyramidal O5 coordination sphere resulting from three carboxylate groups and two OH− ligands. The dihedral angles between the two benzene rings in the L3− ligand and between the benzene ring and the two imidazole rings in the bix ligand are 67.05 (15), 75.27 (17) and 82.05 (17)°, respectively. Four neighbouring Co2+ ions are linked by six carboxylate groups and two μ3-OH ligands, forming a butterfly-shaped secondary building unit (SBU). These SBUs are connected by L3− anions into layers parallel to (1-10). Adjacent layers are cross-linked by the bix ligands, forming a three-dimensional framework that has a bimodal -connected tfz-d topology. The disordered lattice water molecule is located in the voids of the framework and has O⋯O and O⋯N contacts of 2.81 (2) and 2.95 (2) Å, suggesting medium-strength hydrogen bonds. The title compound may be a good candidate for artificial eye lenses.The title coordination polymer, {[Co For top al. 2010.2(C15H7O7)(OH)(C14H14N4)]·0.25H2O = 0.037wR(F2) = 0.086S = 1.045314 reflections396 parameters1 restraintH atoms treated by a mixture of independent and constrained refinementmax = 0.37 e Å−3Δρmin = −0.37 e Å−3ΔρAPEX2  I, New_Global_Publ_Block. DOI: 10.1107/S1600536814022806/wm5040Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S1600536814022806/wm5040fig1.tifx y z x y z x y z x y z x y z . DOI: x, 2 − y, 1 − z; ii) 2 − x, 1 − y, 1 − z; iii) −1 + x, −1 + y, z; iv) 2 − x, 2 − y, −z; v) 1 − x, 1 − y, z.]The extended asymmetric unit of the title compound. Displacement ellipsoids are drawn at the 50% probability level. The disordered lattice water molecule has been omitted for clarity. The tetranuclear SBU in the structure of the title compound. [Symmetry code: A) 1 − Click here for additional data file.10.1107/S1600536814022806/wm5040fig3.tifL 3− . DOI: L3− anions.View of the layered network formed by the SBUs and the 1029647CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The geometry of the title hemibiquinone is different from previous examples and may be correlated with the weak interactions in the crystal. 16H9BrN2O4·0.5C6H6, the molecules stack in a centrosymmetric unit cell in a 2:1 stoichiometry with co-crystallized benzene solvent molecules and interact via various weak interactions. This induces a geometry different from that predicted by theory, and is unique among the hemibiquinones heretofore reported.In the crystal of the title compound, C Biphenyl derivatives have garnered great attention to themselves as conductors of electricity  molecule, 4′-bromo-2′,5′-dimethoxy-2,5-dioxo--3,4-dicarbonitrile 1 Fig. 1, has beenter 1974, where aet al., 20152(CN)2], Fig. 21 is comparable to that in the hydroquinone [1.481 (2) Å]. In this molecule, the C5—C4—C7—C8 torsion is 125.3 (2)°, compared to the hydroquinone torsion angle of −126.50°, ° and C5—C6—O1—C14 bent out of plane by −7.0 (3)°. The methoxy group bond angle C3—O2—C13 is measured at 117.4 (1)°, and C6—O1—C14 is measured at 117.3 (1)°. The methyl portions of each of these groups point away from the sterically restricting groups 1 [1.346 (2) Å] is shorter than than the corresponding hydroquinone C9—C10 bond [1.408 (2) Å] and the C1—C6 bond [1.334 (6) Å] of BrHBQBr  Å] compared to the same bond in the hydroquinone precursor [1.885 (1) Å], but is still shorter than that of the starting material BrHBQBr . Additionally, there is a short contact between C10 and C8, at 3.486 (3) Å. The N2 nitrile atom possibly accepts a very weak interaction from the methoxy C13 and H13A pair (2.82 Å and 97°). There is a long C13⋯N2 [(3.101 (3) Å] interaction as well. Even longer than those interactions, H13 also has a weak H⋯π interaction with the dimethoxybenzene ring on an adjacent molecule (H⋯π = 2.88 Å). The packing is shown in Fig. 5Each HBQ molecule interacts with a total of three benzene molecules by short contacts. As mentioned above, one molecule of benzene is sandwiched between two quinone rings. Additionally, the 3-substituted nitrile group accepts a C—H⋯N hydrogen bond from a solvent molecule . The third benzene molecule exhibits short contacts to the 4′-bromine atom on the opposite end of the molecule, where H17 and H18 link to Br1 almost symmetrically . Since the benzene molecule π-stacks parallel to the quinones, the benzene molecule is oriented in the same direction relative to the dimethoxybenzene ring. Although, in previous HBQ crystals the 4 and 4′ groups show evidence of intermolecular halogen bonding, due to the excess electron density around the aryl bromine atoms and the nitrile groups, an attractive interaction is not possible, rather a slightly repulsive interaction is favored. Instead, the protons on C17 and C18 bifurcate to Br1 as an acceptor, forming slightly asymmetric hydrogen bonds between the dimethoxybenzene ring and the benzene solvent molecule. As discussed above, the quinone carbonyl groups are deflected from perfect planarity. In previous structures, methoxy oxygen atoms tended to deflect the carbonyl groups through repulsive effects. However, this structure contains some attractive intermolecular hydrogen bonding character, including the C14—H142O and 100 mL of benzene. FeCl3  was added in one portion. The resulting mixture was capped and stirred overnight. The resulting phases were separated, and the organic phase was washed with water and dried over anhydrous Na2SO4. Evaporation of the solvent produced a crude product. The pure product was precipitated from a chloroform solution by addition of hexane, yielding 0.0460 g (36.7%). Black, block-shaped crystals of 1 were grown from chloroform solution with residual benzene at 296 K. 1H NMR  δ = 7.22 , 7.12 , 6.71 , 3.87 , 3.76 .4′-Bromo-2,5-dihydroxy-2′,5′-dimethoxy--3,4-dicarbonitrile  was suspended in a mixture of 100 mL of H3, 0.88 Å. Methyl H atoms were allowed to rotate but not to tip to best fit the experimental electron density. Uiso(H) values were set to a multiple of Ueq(C) with 1.5 for CH3. Crystal data, data collection and structure refinement details are summarized in Table 1H atoms attached to carbon atoms were positioned geometrically and constrained to ride on their parent atoms, with C—H-bond distances of 0.95 Å for aromatic C—H, 1.00, 0.99 and 0.98 Å for aliphatic CH10.1107/S2056989016005120/hb7567sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989016005120/hb7567Isup2.hklStructure factors: contains datablock(s) I. DOI: 1470649CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The two 2,2-diallylmalonate anions bridge four AgI ions in a μ4- mode, setting up an Ag4O8P4 core (point group symmetry -4..) of corner-sharing tetrahedra. The shortest intramolecular Ag⋯Ag distance of 3.9510 (3) Å reveals that no direct d10⋯d10 interactions are present. Four weak intramolecular C—H⋯O hydrogen bonds are observed in the crystal structure of the title compound, which most likely stabilize the tetranuclear silver core.In the tetranuclear molecule of the title compound, [Ag On a molecular level this is typically achieved by designing low aggregated metal compounds. In the case of silver, this can be realized by the use of phosphanes as a Lewis base; however, the concomitant increase of the molecular weight of the transition metal complex may decrease its vapour pressure. Circumventing this difficulty, we have investigated the use of olefines as ligands for silver(I) carboxylates, in which the olefin is covalently bonded to the carboxylate. In the context of this approach, the title compound [{ mode  Å], which is supported by the respective bond angles around Ag1 (Table 1The asymmetric unit of (I)de Fig. 1. There i1 Table 1 summing 1 Table 1. However3P tetrahedra gives the tetranuclear structure of (I)4O4 heterocubanes O,O′)-, - or -chelation Ag}4{(O2C)2C(CH2CH=CH2)2}2] was prepared by the addition of PPh3  to a suspension of [(AgO2C)2C(CH2CH=CH2)2]  in dichloromethane (30 ml) at 273 K. After stirring for 2 h at this temperature, the reaction mixture was filtered through a pad of celite. Afterwards, all volatiles were removed in oil-pump vacuum, and (I)2C)2C(CH2CH=CH2)2]).Complex [{(Ph90H80Ag4O8P4 (1844.96): C 58.59, H 4.37. Found: C 58.53, H 4.34. 1H NMR : δ = 2.79 , 4.97 , 5.03 , 5.90 , 7.30–7.51 . 31P{1H} NMR : δ = 15.7 . IR : ν = 1637 , 1559 , 1440 , 692 (vs), 521 (vs).Analysis calculated for CUiso(H) = 1.2Ueq(C) and a C—H distance of 0.93 Å for aromatic and vinylic as well as 0.97 Å for methylene protons. The unit cell contains two voids of 34(1.4) Å3. Void volume calculation using the SQUEEZE routine in PLATON ; however, this ambiguity is resolved as the Flack parameter of the inverted structure is calculated to 1.052 (9). This indicates that the original absolute structure has been assigned correctly.Crystal data, data collection and structure refinement details are summarized in Table 310.1107/S1600536814019394/wm5047sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S1600536814019394/wm5047Isup2.hklStructure factors: contains datablock(s) I. DOI: 1021407CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The chloride ion occupies an equatorial site and the dihedral angle between the 2,2′-bpy ring systems is 72.02 (6)°. In the crystal, the components are linked by C—H⋯O and O—H⋯O hydrogen bonds and aromatic π–π stacking interactions [shortest centroid–centroid separation = 3.635 (2) Å], generating a three-dimensional network.In the title hydrated salt, [NiCl(C DOI: 10.1107/S1600536814009064/hb7220Isup2.hklStructure factors: contains datablock(s) I. DOI: 998760CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II), the essentially planar cations are connected through N—H⋯Cl hydrogen bonds to the tetrahedral anion. 5H6ClN2)2[CoCl4], was synthesized by slow evaporation of an aqueous solution at room temperature. The asymmetric unit consists of two essentially planar (C5H6ClN2)+ cations [maximum deviations = 0.010 (3) and 0.014 (3) Å] that are nearly perpendicular to each other [dihedral angle = 84.12 (7)°]. They are bonded through N—H⋯Cl hydrogen bonds to distorted [CoCl4]2− tetrahedra, leading to the formation of undulating layers parallel to (100). The structure is isotypic with the Zn analogue The title salt, (C The bond angles C4—N2—C5 [123.6 (3)°] and C9—N3—C10 [123.3 (3)°] in the rings of cat1 and cat2, respectively, confirm the presence of pyridinium cations. Previous studies  to 2.2934 (12) Å and the Cl—Co—Cl angles range from 104.84 (5) to 118.58 (5)°, revealing considerable distortions from the ideal tetrahedral geometry. These values are in agreement with those observed in similar compounds  by hydrogen bonds  with a second symmetry-related cat1 cation. The hydrogen-bonding environments of the two cations are similar. Both are linked to two CoCl4 tetrahedra by three hydrogen bonds 2[ZnCl4]·H2O 2[ZnCl4] 2[CdCl4]·H2O 2[CuCl4] 2[CuBr4] 2[ZnCl4]  chloride and 2-amino-5-chloropyridine (molar ratio 1:1) was dissolved in an aqueous solution of hydrochloric acid with 5 ml of ethanol. The mixture was stirred and then kept at room temperature. Blue crystals of the title compound were obtained after two weeks.Uiso(H) = 1.2Ueq.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015007707/wm5146sup1.cifCrystal structure: contains datablock(s) I, New_Global_Publ_Block. DOI: 10.1107/S2056989015007707/wm5146Isup2.hklStructure factors: contains datablock(s) I. DOI: 990478CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The ReI ion is coordinated by two N atoms from the 1,10-phenanthroline ligand and one N atom from the 1,2-bis(pyridin-4-yl)ethane ligand [mean Re—N = 2.191 (15) Å] and by three carbonyl ligands [mean Re—C = 1.926 (3) Å] in a distorted octahedral geometry. The electrostatic forces and weak C—H⋯F(O) hydrogen bonds pack cations and anions into the crystal with voids of 82 Å3, which are filled by solvent molecules. The crystal packing exhibits short intermolecular O⋯O distance of 2.795 (5) Å between two cations related by inversion.The asymmetric unit of the title compound, [Re(C DOI: 10.1107/S1600536814014135/cv5465Isup2.hklStructure factors: contains datablock(s) I. DOI: 1008626CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The equatorial plane is formed by two N,O-bidentate 1H-pyrazole-3-carboxylate ligands in a trans configuration. The axial positions are occupied by two water molecules. The mononuclear complex molecules are arranged in layers parallel to the ab plane. Each complex molecule is linked to four adjacent species through intermolecular O—H⋯O and N—H⋯O hydrogen bonds that are established between the coordinating water molecules and carboxylate O atoms or protonated N atoms of the organic ligands. These layers are further connected into a three-dimensional network by additional hydrogen bonds involving solvent water molecules and non-coordinating carboxylate O atoms.In the title compound, [Cu(C H-pyrazole-3-carboxylate ligand, see: Artetxe et al. , nickel(II) and zinc complexes of the 1 al. 2015; López-V al. 2014.4H3N2O2)2(H2O)2]·2H2O = 0.028wR(F2) = 0.074S = 1.091216 reflections109 parameters4 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 0.36 e Å−3Δρmin = −0.35 e Å−3ΔρCrysAlis PRO  used to solve structure: OLEX2  I, global. DOI: 10.1107/S2056989015021593/im2473Isup2.hklStructure factors: contains datablock(s) global, a2013072_cupyc. DOI: Click here for additional data file.10.1107/S2056989015021593/im2473fig1.tif4 3 2 2 2 2 2 2 . DOI: 4H3N2O2)2(H2O)2] ·2H2O showing the atom labelling for the asymmetric unit and 50% probability displacement ellipsoids.Molecular structure of [Cu. Projection of a layer of [Cu(C4H3N2O2)2(H2O)2] complexes along the [010] direction (below). Cu(II) centres are represented as translucent octahedra and the O—H⋯O and N—H⋯O hydrogen bonds are depicted as dashed red lines.View of the crystal packing along the crystallographic 1437048CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information: