Eucranium Brulléé has been revised and now includes six species: E. arachnoides Brulléé, E. belenae Ocampo new species, E. cyclosoma Burmeister, E. dentifrons Guéérin-Mééneville, E. planicolle Burmeister, and E. simplicifrons Fairmaire. Eucranium pulvinatum Burmeister is a new junior synonym of Eucranium arachnoides Brulléé, and Eucranium lepidum Burmeister is a new junior synonym of E. dentifrons Guéérin-Mééneville. The following lectotypes and neotypes are designated: Eucranium pulvinatum Burmeister, lectotype; Eucranium planicolle Burmeister, lectotype; Psammotrupes dentifrons Guéérin-Mééneville, neotype; and Eucranium lepidum Burmeister, neotype. Description of the genus and new species, diagnosis and illustrations, and distribution maps are provided for all species. A key to the species of this genus is provided, and the biology and conservation status of the species are discussed.The South American genus  Anomiopsoides Blackwelder, Ennearabdus van Lansberge, Eucranium Brulléé, and Glyphoderus Westwood (Eucranium consists of six species. The genus is endemic to Argentina and distributed in the Monte and Chacoan biogeographic provinces (based on The tribe Eucraniini (Scarabaeidae: Scarabaeinae) constitutes a monophyletic group and includes four genera, Westwood . This wobased on  schema; based on .Eucranium was originally described by Brulléé (1834) for one species, E. arachnoides Brulléé (1834). The name was originally proposed by Dejean . Guéérin-Mééneville . Laporte (1840) described Pachysoma (Cyclodema) lacordairei (= E. arachnoides) and indicated that this was the only species of Pachysoma in America. Blanchard (Anomiopsis aelianus (= E. arachnoides). In 1845 Blanchard redescribed A. aelianus and referred to E. arachnoides and A. dioscorides with indication of their similarity to A. aelianus. Also Blanchard . Lacordaire (Eucranium to Brulléé (1834) and provided a synonymy list . Burmeister . Mouth parts and male genitalia were dissected and cleaned in a dilute solution (∼?10%) of potassium hydroxide and neutralized in a dilute solution (∼? 10%) of acetic acid. The male genitalia were placed in a glycerin-filled vial pinned under the specimen.Body measurements, puncture density, puncture size, and density of setae were based on the following standards: Body length was measured from the middle of the anterior margin of the pronotum (at the middle) to the apex of the elytra, plus head length from the apex of clypeal process to the base of the head . Body width was measured across mid-pronotum. Puncture density was considered ““dense”” if punctures were nearly confluent to less than 2 puncture diameters apart, ““moderately dense”” if punctures were 2–6 diameters apart, and ““sparse”” if punctures were separated by more than 6 diameters. Puncture size was defined as ““small”” if punctures were 0.02 mm or smaller, ““moderate”” if 0.02–0.07 mm, and ““large”” if 0.07 mm or larger. Setae were defined as ““sparse”” if there were few setae, ““moderately dense”” if the surface was visible but with many setae, and ““dense”” if the surface was not visible through the setae. Elytral carinae were counted from the elytral suture. Specimen labels were copied literally using ““/”” between lines and ““;”” between labels.Neotypes and Lectotypes were designated to provide the nomenclatural stability of the taxon studied, according to the Article 72 of the International Code of Zoological Nomenclature (1999).CMNC: Canadian Museum of Nature, Ottawa, Canada .HECO: Hope Entomological Museum, Oxford, England (Mann D).IAZA: Instituto Argentino de Investigaciones de las Zonas ÁÁridas, Mendoza, Argentina (F Ocampo).IMLA: Fundacióón e Instituto Miguel Lillo, Universidad Nacional de Tucumáán, Tucumáán, Argentina (MV Colomo).LEMQ: Lyman Entomological Museum, Mc Gill University, Quebec, Canada (S Boucher).MACN: Museo Argentino de Ciencias Naturales, Buenos Aires, Argentina (A Roig).MNHN: Musééum National d'Histoire Naturelle, Paris, France (O Montreuil).MLPA: Museo de La Plata, La Plata, Argentina (A Lanteri).UNSM: University of Nebraska State Museum, Lincoln, NE, USA (BC Ratcliffe).USNM: United States National Museum, Washington D.C. USA (D Furth).Specimens for this research were collected or borrowed from and deposited in the following institutions and collections:Eucranium genus were described and recognized based mostly on the shape and length of the clypeal processes, and the pronotal and elytral sculptures. These characters rendered variable within species and were not reliable for species identification or description. In this work, new characters were explored and used to define species. Among these are Elytral pseudoepipleuron, pseudoepipleural angle with respect to elytral disc, elytral 8th striae (shape and sculpture), and shape and development of mesotibial spurs. Species male genitalia were studied in order to find species-specific patterns in the shape of the paremares, but the findings were not informative at this level. Internal sacs of paremeres were extracted and studied and these structures provided highly valuable information for phylogenetic analysis, however, they are impractical for species identification. Nevertheless, the information from the paremeres internal sacs is currently being used in a separate project on Eucraniini evolutionary biology .Traditionally species in the Eucranium Brulléé 1834: 286.EucraniumNomen nudum).EucraniumAnomiopsisnecA. dioscoridesAnomiopsis Westwood 1838: 159, PsammotrupesP. dentifronsPsammotrupesCyclodema Laporte 1840: 68, (as subgenus of Pachysoma Mac Leay), junior synonym. Type species Pachysoma lacordairei Laporte 1840: 68.Anomiopsis Westwood 1838; Eucranium).Eucranium Brulléé; Eucranium Brulléé; Eucranium Brulléé; Eucranium Brulléé; Eucranium Brulléé; Eucranium Brulléé; Eucranium Brulléé; Eucranium arachnoides Brulléé 1834, by monotypy.Type species: DiagnosisThe Eucraniini genus thacan be distinguished from other members of the New World Scarabaeinae by the following combination of characters: Body relatively large (13–30 mm), black , 22, 24;RedescriptionHead . Venter: Surface smooth, glabrous or sparsely setose, prosternum pentagonal, anterior margins slightly concave. Mesosternum wider than long, mesometasternum suture visible or not. Metasternum flat, strongly narrowed in middle (metacoxae contiguous). Metepisternum 2.5–3 times longer than wide (at base). Ventrites narrower at middle. Pygidium with base grooved medially; disc slightly convex, sparsely punctate, punctures variable. Legs . These differences are not consistent among individuals of the same population. Based on the species concept used in this work to recognize Eucranium species, all these differences are attributed to intraspecific variation. Molecular information is needed to elucidate weather isolated populations ; Argerich (1); Bahíía Blanca (4); Bahíía San Blas (1); Bajo Hondo (4); Carmen de Patagones (2); Estancia Barrau (6); Felipe Soláá (7); La Colina (1); Maza (3); Villa Iris (1). Cóórdoba: no data (6); ““Sur de Cóórdoba”” (1); San Javier (2); Las Rosas (3); Potrero de Góómez (1); Yacanto de San Javier (1). La Pampa: no more data (1); Gaviotas (1); Santa Rosa (1); Victorica (4). Mendoza: no more data (1); Agua Escondida (2); Aguada de los Ciegos (1); Arroyo el Rosario, Puesto las Gateadas (1); Arroyo La Rinconada (1); Base del Volcáán Diamante (1); Blanco Encalada (1); Caverna de los Tigres (1); Confluencia ríío Diamante and ríío Salado (1); Costa de Araujo (1); Dique Agua del Toro (4); Dique Agua del Toro (20 km S) (3); Dique El Carrizal (3); Divisadero (2); El Mollar (2); El Nihuil, Méédanos (1); Embalse El Nihuil (4); Fortíín Malargüüe (1); Huayqueríías (1); From RN 40 to Puesto Alvarado (2); Malargüüe (no more data) (4); Malargüüe, Los Corrales (5); Monte Comáán (1); ÑÑacuññáán (9); Pareditas (2); Reserva de la Bióósfera ÑÑacuññáán (11); Reserva Natural Laguna del Diamante (15 km SE) (19); Reserva Natural La Payunia, Puesto La Senillosa (1); Reserva Natural La Payunia, Los Relinchos (11); Reserva Natural La Payunia, Valle del Saino (1); RN 40 and Arroyo Yaucha (3); RN 40 (km 143) (1); RN 40 (S of Pareditas) (2); Road to Paso de Los Tigres (1); Salar del Nihuil (2); San Rafael (10). Ríío Negro: Coronel Góómez (2); Ríío Colorado (3). San Luis: no more data (1); Arizona (19); Balde (2); San Luis, Departamento Capital (7); El Volcáán (1); San Geróónimo (1). ““Patagonia”” no more data (1).ARGENTINA . Buenos Temporal distributionJanuary (79); February (12); March (12); April (5); May (1); July (2); August (4); September (7); October (4); November (15); December (51); no data (41).Biology and conservationEucranium species. Populations of this species generally have a small, patchy distribution and consequently susceptibly to local extinction if changes in the environmental conditions occur. The only known populations of E. arachnoides that are currently in a protected area are those from Reserva Natural ÑÑacuññáán and Reserva Natural La Payunia in the Mendoza province.Biology and behavior of this species were recently discussed by Zunino et al. , MontereType materialEucranium belenae Ocampo holotype male at IAZA labeled: ““ARGENTINA: Mendoza / R.N 142 km 107. N. Rva. / Telteca / 510m. 32°°15′?12″?S / 67°°49′?13″?W. 30/III/2009/ F. C. Ocampo””; ““Eucranium / belenae / HOLOTYPE / F. C. Ocampo””, Allotype female labeled as holotype except: ““Eucranium / belenae / ALLOTYPE / F. C. Ocampo.”” Twenty eight male and twenty female paratypes at IAZA: labeled as holotype. Eleven male and six female paratypes at IAZA labeled: ““ARGENTINA: Mendoza / Reserva Telteca. 32°°22≈?59.58″? S, / 68°°03′?14.16″? W. 548m. / 11-IV-2008. Col. L. Muññoz.”” Fourteen male and nine female paratypes at IAZA labeled as previous except: ““12-IV-2008””. Three male paratypes at IAZA labeled as previous except: ““13-IV-2008””. Three male paratypes at IAZA labeled as previous except: ““14-IV-2008””. One male paratype at IAZA labeled as previous except: ““15-IV-2008””. Three male and two female paratypes at IAZA labeled: ““ARGENTINA: Mendoza / R.N. 142 Km 107, N Rva. / Telteca. 510m. 32°°15′?12″?S / 67°°49′?13″?W. 1-III-2009. / KS Sheldon, FC Ocampo.”” Four male and eight female paratype at IAZA labeled as previous except: ““1/III/2009””. Four male and Four female paratype at IAZA labeled as previous except: ““FC Ocampo, K Sheldon”” and ““17/III/2009””. Seven male and three female paratypes at IAZA labeled: ““ARGENTINA: Mendoza / Lavalle. Telteca. 32°°22′?59.58″?S. / 68°°03′?14.16″?W. 548m. 05-II-2008. / Col. F. Ocampo, E. Ruiz, G. San Blas.”” One paratype at IAZA labeled: ““ARGENTINA: Mendoza / Lavalle. Telteca. 32°°22′?59.58″?S. / 68°°03′?14.16″?W. 548m. 27-XI-2007. / Col. F. Ocampo””. One male and one female paratypes at IAZA labeled: ““ARGENTINA: Lavalle / Puente Ríío Mendoza. 21 Feb. 2006. E. Ruiz.”” One male and one female paratypes at IAZA labeled: ““ARGENTINA: Mendoza / Reserva Telteca. 563m. S32°°23′?33″? W68°°03′?00″? / Jan-3-2002. F. C. Ocampo.”” Four female paratypes at IAZA labeled: ““R.A. Mza. Lavalle / Telteca / 3/2-14/3 /1995 / S. Roig / G. Flores.”” Four female paratypes at IAZA labeled: ““RA. Mza. Lavalle / Telteca /2/11 – 1/12 /1994 / G. Flores.”” One male and two female paratypes at IAZA labeled: ““Ra. Mendoza Tel- / teca 17/VIII-24/IX / 1996. Flores/Roig.”” One male and one female paratypes at IAZA labeled: ““Ra. Mendoza Tel- / teca 25/XI-25/XII / 1995. Flores/Roig.”” One male and one female paratypes at IAZA labeled: ““Ra. Mendoza Tel- / teca 25/IX-5/XI / 1996. Flores/Roig””. One male paratype at IAZA labeled: ““Ra. Mendoza Tel- / teca 14/8 -24/9/ / 1995 Flores/Roig.”” Two female paratype at IAZA labeled: ““Mendoza, Lavalle / Telteca 15-2 al 25-3-96. Col. G. Flores / IADIZA.”” One female paratype at IAZA labeled as previous except: ““15-4-95””. One male and three female paratypes at IAZA labeled: ““Ra. Mendoza Tel- / teca 3/II -14/III / 1995. Flores/Roig.”” One male and two female paratype at IAZA labeled: Mendoza, Lavalle / Telteca 1 al 15/12/ 94 Flores/Roig / IADIZA.”” One female paratype at IAZA labeled: ““Mendoza, Lavalle / Telteca 10/10 al 3/12/96 / Col. Gonzalez / IADIZA.”” Three male paratypes at IAZA labeled: ““RA. Mza. Lavalle / Telteca / 01.III.94 / G. Flores / IADIZA.”” One male paratype at IAZA labeled: ““Mendoza. Lavalle / Parque Telteca / 10.5.93 / M. Gonzáález / IADIZA”” One female paratype at IAZA labeled: ““Mendoza Lavalle Telteca 3-XII-96 / 6-I-97 Flores-Roig.”” One female paratype at IAZA labeled: ““Mendoza Lavalle Telteca 25/9-31/10 / 1995 Flores/Roig.”” One female paratype at IAZA labeled: ““Mendoza Lavalle Telteca 2/V-14/6 / 96 Flores/Roig / IADIZA.”” One male paratype at IAZA labeled: ““RA. Mza. Lavalle / El Encóón 12-IV-84 / IADIZA””; ““CE.000131 / IADIZA””. One male paratype at IAZA labeled: ““RA.Mza. Lavalle / Rva. Telteca / 15/X/03 / col. G. Debandi.”” One female paratype at IAZA labeled: ““RA. Mza. Lavalle / Telteca 01.III.94. / G. Flores / IADIZA.”” Three male and one female paratypes at IAZA with no data. All paratypes with a yellow paratype label: ““Eucranium / belenae / PARATYPE / F. C. Ocampo.””Type localityArgentina, Mendoza, RN 142, km 107, 32°° 15′? 12″? S - 67°° 49′? 13″? W.DiagnosisE. belenae can be distinguished from other Eucranium species by the following combination of characters: Elytron with pseudoepipleuron not developed; elytral disc with interstriae becoming slightly convex toward margin, 8th stria slightly sulcate; apex of mesotarsus reaching apex of outer mesotibial spur or not   ; outer mal axis)  ; RN 142 Km 107 (114); RN 142 and Ríío Mendoza (2); Reserva Natural Telteca (27); Telteca (94).ARGENTINA . MendozaTemporal distributionJan (11); Feb (27); March (59); April (66); May (2); June (1); August (4); September (7); October (2); November (14); December (15).Biology and conservationE. belenae were observed carrying goat pellets and small pieces of dry horse dung at daylight hours ; Andalgaláá (2); Barranca Larga (4); Beléén (3); Capillitas (3); Corral Quemado (3); El Arenal (1); RP 47 N of Capillitas (9); El Ingenio (1); Hualfíín (3); Isla de Sauce (1); Loma Negra (2); Pipanaco (1); Punta de Balasto, 12 Km W. Campo El Arenal (3); Punta de Balasto (S. of Santa Maria) (28); RN 40 KM 892 (3). La Rioja: no more data (4); Aimogasta (1); Aminga (1); Anillaco (6); Anillaco (2 km N) (12); RN 40 E of Guandacol (1); La Rioja (1). Salta: La Caldera, Campo Alegre (1). Tucumáán: Tafíí del Valle (1).ARGENTINA . CatamarTemporal distributionJanuary (21); February (52); March (7); November (23); December (4).Biology and conservationE. cyclosoma were observed carrying small pieces of dry horse dung at daylight hours over sand dunes in Catamarca province (Specimens of province . ConservEucranium dentifrons (Psammotrupes)ntifrons : 46  and so these species are placed in synonymy.Based on morphological evidence it was concluded that there are no differences between Eucranium dentifrons presents considerable variation in pronotal and elytral sculpture. Variation in puncture size and density on the pronotum and elytra is found among specimens of the same population and among populations. Variation is also found in rugosity on elytral interval seven, been in most specimens obvious and in some specimens slightly evident . These differences are more obvious among specimens from Neuquéén and western Rííio Negro province.DistributionChubut: no data (1); Gaiman (1); Puerto Madryn (CENPAT) (5); Telsen (2); Peníínsula Valdez, Estancia la Irma (5); Peníínsula Valdez, Estancia Los Méédanos (5); Peníínsula Valdez, Estancia San Pablo (23); Peníínsula Valdez (no more data) (8); Peníínsula Valdez, Playa Fracaso (1); Peníínsula Valdez, Puerto Piráámides (1); Peníínsula Valdez, Punta Delgada (5). Neuquéén: Aguada Florencia (2); Arroyo Picúún Leufúú (1); Colonia Centenario (1); Las Lajas (19 Km S) (4); Las Lajas, Cerro de la Cuchilla (4); Neuquéén (1); Picúún Leufúú (11); Piedra del ÁÁguila (6); Plaza Huincul (16); Ríío Agrio  (7); RN 40 Km 2396, S of Las Lajas (14); RN 40, Bajada del Agrio (1); RN 40, El Marucho (1); Villa El Chocóón(2 km W) (3); Zapala (4). Ríío Negro: Barrancas del Gualicho (1); Cipolletti (1); Coronel Juan Joséé Góómez (2); General Roca (1); San Antonio Oeste, Las Grutas (8).ARGENTINA . Chubut:Temporal distributionJanuary (38); February (62); March (16); April (8); September (1); October (6); November (2); December (12).Biology and conservationE. dentifrons have been observed caring and provisioning their borrows with guanaco dung pellets and small pieces of dry horse dung at daylight over sand dunes in Peníínsula Valdez, Chubut, and in Chocóón and near Las Lajas, Neuquéén  (Specimens of rvation) .E. dentifrons is known to occur is Peníínsula Valdééz in Chubut province.Conservation status of this species has not been assessed. The only protected area where Eucranium planicolleType materialEucranium planicolle Burmeister lectotype male at MACN labeled: ““Pampa / occid.””; ““Eucranium / planicolle / planicolle 6””; ““Eucranium / planicolle / Burm. / LECTOTYPE / F. C. Ocampo det. 2009””. Lectotype here designated. One paralectotype male at MACN labeled as lactotype except: ““planicolle 5””.DiagnosisE. planicolle can be distinguished from other Eucranium species by the following combination of characters: Elytron with well defined pseudoepipleuron, pseudoepipleuron forming an ∼?45–60°° angle with elytral disc ; Bahíía Blanca (3); Bahíía San Blas (1); Bajo Hondo (6); Coronel Pringles (1); Estacióón Delta near Monte Hermoso (13); Estancia Barrau (30 Km SW Villa Iris) (8); Monte Hermoso (3); Villa Iris (7). La Pampa: no more data (1); Anguil (1). Mendoza: no more data (6); 25 de Mayo (1); Agua Escondida (1); Dique Agua del Toro (2); Dique Agua del Toro (20 Km S.) (2); Monte Comáán (1); RP 143, Km 33 (1); Pareditas (3 Km S) (1); Pareditas (10 Km S) (1); Pareditas (22 Km S.) (1); Piedra Póómez (1); Reserva Natural Laguna del Diamante, 10 Km E. (1); RN 40, Puesto Alvarado (1); RN 40 and Arroyo Yaucha (1); RN 40, S of Pareditas (4); RP 150 (1). Ríío Negro: no more data (2); Ríío Colorado (8); RP 4  (2). San Luis: Departamento Capital (5).ARGENTINA . No dataTemporal distributionJanuary (3); February (15); March (2); April (1); October (2); November (16); December (31).Biology and conservationE. planicolle are known to be diurnal and have been observed caring and provisioning their borrows with goat dung pellets in Mendoza province  . Conservation status of this species has not been assessed.Specimens of Eucranium simplicifrons Fairmaire 1873: 608.DiagnosisE. simplicifrons can be distinguished from other Eucranium species by the following combination of characters: Elytron with or without pseudoepipleuron, if present, pseudoepipleuron forming an <65°° angle with elytral disc ; Choya (8); El Charco (4); Fernáández (1); Guasayáán (1); Ramíírez deVelezco (1 Km N) (2).ARGENTINA . SantiagTemporal distributionFebruary (1); April (1); August (4); October (9); November (2).Biology and conservationE. simplicifrons. Conservation status of this species has not been assessed; the species does not occur in any protected area.With the exception that the species is diurnal  nothing is known about the biology of th striae carinated, carina sharp and reflexed or rounded and reflexed1. Elytron with well defined pseudoepipleuron, pseudoepipleura forming a 45–60°° angle with elytral disc , 23; ely2th stria not carinated, or if carinated, carinae poorly defined and never reflexed1′?. Elytron with or without pseudoepipleuron, if present pseudoepipleuron forming a <65°° angle with elytral disc , 15, 25;3th stria carinated, carina sharp 2. Elytron with outer margin of 8na sharp , 23; elyEucranium planicolle Burmeister  (neville) 3. Elytron with pseudoepipleuron absent43′?. Elytron with pseudoepipleuron present, sometimes poorly developedEucranium arachnoides Brulléé ; outer mesotibial spur distinctively broad at apical 1/2, obviously asymmetrical  ; mesotibial outer spur slightly broad on apical 1/3, nearly symmetrical . SantiagEucranium simplicifrons Lacordaireth stria slightly sulcate; west central Argentina (northeastern Mendoza province)5. Elytral disc with interstriae becoming slightly convex toward apical margin, 8Eucranium belenae Ocampo sp. nov. 5′?. Elytral disc with interstriae smooth, evenly flat, 8Eucranium cyclosoma Burmeister . Thus, the Monte and Chacoan biota have multiple origins with most genera being from Neotropical origin followed by groups with Patagonian or Andean affinities.Morphological divergence of n biotas . South An biotas . In the Eucranium are distributed across a ∼?2000 km long (North-South) and 500 km wide (East West) range. Nevertheless, species in this genus show little sympatry, E. arachnoides and E. planicolle partially share they distributional range, while the rest of the species, E. belenae, E. cyclosoma, E. dentifrons, and E. simplicifrons are isolated from other species in the genus or only share a few localities (ex. E. arachnoides and E. dentifrons in Ríío Negro province). Eucranium species have high endemicity and populations have patchy distributions that make them susceptibly to local extinction if changes in the environmental conditions occur. Nothing is known for Eucranium species' population dynamics or habitat conservation status. Only two species, E. belenae and E. dentifrons are distributed within natural reserves or protected areas. It is well documented that there are genetic implications for small population size, among these it is a decline of genomic variation resulting from allelic loss (and Carrol (1997) for the long term viability of a population it is important for it to maintain genetic variability which would enable the population to adaptively tolerate changes in environmental conditions. Further more, Keller et al. , in order to preserve these species it is critical to understand their population dynamics and their habitat conservation status. Eucranium is characterized by its unusual morphology and unique biology and behavior, and it constitutes an old evolutionary lineage. Vane-Wright et al. (Eucranium of high conservation value.Species of lic loss . Accordir et al. , based ot et al.  proposed


Each of the two independent AuIII ions lies on an inversion center and has a distorted square-planar geometry. In the crystal, intermolecular C—H⋯Cl hydrogen bonds, π–π interactions [centroid–centroid distances = 3.5548 (16) and 3.7507 (16) Å] and Au⋯π interactions [Au⋯centroid distance = 3.6424 (10) Å] are effective in the stabilization of the structure, resulting in the formation of a supramolecular structure. Intramolecular N—H⋯N hydrogen bonds are present in the cation.In the title compound, (C DOI: 10.1107/S1600536811036208/hy2466Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


II ion in the title complex, [PtCl2(C14H10N4)], is four-coordinated in a distorted square-planar environment by two N atoms of a chelating 2,3-di-2-pyridylpyrazine ligand and two chloride anions. The pyridyl ring coordinated to the PtII atom is inclined slightly to its carrier pyrazine ring [dihedral angle = 13.5 (1)°], whereas the uncoordinated pyridyl ring is inclined considerably to the pyrazine ring [dihedral angle = 54.3 (2)°]. The dihedral angle between the two pyridyl rings is 59.2 (2)°. In the crystal, the complexes are assembled through intermolecular C—H⋯N and C—H⋯Cl hydrogen bonds, forming a three-dimensional network. Intramolecular C—H⋯N and C—H⋯Cl hydrogen bonds are also present.The Pt DOI: 10.1107/S1600536811038906/tk2794Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The NO5 donor set is based on a distorted octahedron. Helical supramolecular chains along [010] are found in the crystal structure mediated by O—H⋯O hydrogen bonds formed between the coordinating methanol molecule and the phenolate O atom of the chlorobenzene residue.The title Schiff base complex, [V(C E)-2-(2-hydroxybenzylideneamino)phenolates containing halide atoms on the aromatic ring(s), see: Yenişehirli et al. (CH3O)O(CH4O)] = 0.046wR(F2) = 0.131S = 1.043453 reflections221 parameters1 restraintH atoms treated by a mixture of independent and constrained refinementmax = 1.37 e Å−3Δρmin = −0.93 e Å−3ΔρCrysAlis PRO  used to solve structure: SHELXS97  global, I. DOI: 10.1107/S160053681200311X/hg5167Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


II atoms in the title complex, [Ni2(CN)4(C16H36N4)]·C3H7NO·0.5H2O, are bridged by a cyanide ion. The macrocycle folds around one NiII atom, which is five-coordinated in an NiN5 square-pyramidal geometry. The other NiII atom is surrounded by the cyanide ions in an NiN4 square-planar geometry. The dimethylformamide solvent molecule is disordered over two positions in a 0.62 (1):0.38 (1) ratio and the water molecule is disordered about a center of inversion. The dinuclear molecule and solvent molecules are linked by N—H⋯O, N–H⋯N and O—H⋯O hydrogen bonds, forming a three-dimensional network.The two Ni DOI: 10.1107/S1600536810042625/bt5382Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Activation of the α-secretase processing pathway of amyloid precursor protein (APP) is recognized as an important mechanism which diverts APP processing from production of beta-amyloid (Aβ) to non toxic sAPPα, decreasing Alzheimer’s disease (AD) plaque formation and AD-associated cognitive deficits. Two potent classes of PKC modulators can activate the α-secretase pathway, the benzo/indolactams and bryostatin/bryologues. While both modulate PKC-dependent APP processing, no direct comparisons of their relative pharmacological potencies have been accomplished which could assist in the development of AD therapies. In this study, we measured the activation of α-secretase APP processing and PKC-α, -δ, and -ε induced by the benzolactam-APP modulator TPPB and bryostatin-1 in the neuroblastoma cell line SH-SY5Y which expresses APP and α- and β-secretase processing mechanisms. Bryostatin-1 produced a more rapid, potent, and sustained activation of α-secretase APP processing than TPPB and selectively activated PKC-δ and PKC-ε. Although TPPB also activated α-secretase, its potency was approximately 10- to 100-fold lower, possibly reflecting lower PKC-δ and -ε activation. Because bryostatin-1 is a highly potent PKC-δ and -ε activator which activates α-secretase APP processing, further characterization of bryostatin-1/bryologues may help refine their use as important tools for the clinical management of AD. N-methyl-d-aspartate receptor antagonist, which reduces glutamate-dependent excitotoxicity, Ca2+ influx, and oxidant stress in neurons , few effective treatment options have been developed  and “statins,” inhibitors of HMG-coA reductase, may also reduce formation and persistence of Aβ and have been suggested as potential adjuvant therapies for AD  include diphenylurea, derivatives of hydroxyethylamine, and celastol, all of which at least partly block conversion of APP to Aβ. Τhese drugs have been extensively studied in AD therapy , a disintegrin and metalloprotease (‘ADAM’)-17  activation. Several drugs which modulate PKC isoenzyme activity, particularly the PKC-δ and PKC-ε isoforms, potently activate α-secretase processing of APP, generating the non toxic sAPPα and preventing Aβ formation. Currently, PKC activators may represent the most important, novel, and specific treatments for AD. At least two important classes of agents can activate PKC-dependent APP processing at relatively low (μM to nM) doses: (1) the benzolactam/indolactams and (2) bryostatin-1 and related bryologues.Ki = 11.9 nM for inhibition of phorbol 12,13 dibutryrate binding to PKC-α) which enhances sAPPα secretion in fibroblasts and PC12 neuronal cells --8-(5-(4-(trifluoromethyl) phenyl)-2,4-pentadienoylamino) benzolactam] (CAS#497259-23-1) was purchased from Reagent 4 Research LLC  and was diluted in ethanol. All ethanol concentrations in this study were below 0.1 % in cellular assays.Bryostatin-1 in ethanol stock solutions was provided by Aphios Corporation . The benzolactam APP modulator TPPB , -δ , and -ε  antibodies . H-7 antibody is a mouse monoclonal antibody raised against amino acids 645–672 on human PKC-α which recognizes a single 80-kDA PKC-α isoform. G-9 antibody is a mouse monoclonal antibody raised against amino acids 647–673 of rat PKC-δ which recognizes a single 78-kDA band, and E-5 antibody is a mouse monoclonal antibody which was raised against amino acids 705–737 of human PKC-ε and recognizes a single 90-kDA PKC-ε band. PKC isoform bands were visualized using HRP-conjugated 2° antibody  with ECL plus  with SRX101 film. Band intensities were quantified by densitometric analysis using an HP Scanjet 3970 Densitometer and Image-J image analysis system software .Measurements of cytosolic and membrane-associated levels of PKC-α, -δ, and -ε isoenzymes were used to assess PKC translocation in response to bryostatin-1 or TPPB as described by Racchi et al.  with modp < 0.05 was considered as statistically significant.All data are presented as mean ± standard deviation and were analyzed by one-way ANOVA with Dunnett’s post-testing . A value of −7 M (**p < 0.01), 10−8 M (**p < 0.01), 10−9 M (*p < 0.05), and 10−10 M (*p < 0.05). TPPB also induced sAPPα release, but to a lesser extent and only at 10−7 M (p < 0.05) and 10−8 M (p < 0.05) ; TPPB was able to significantly increase sAPPα at 6 h (*p < 0.05) , 6 h (**p < 0.01), and 12 h (*p < 0.05). At this dose, TPPB only significantly increased the release of sAPPα at 6 h (*p < 0.05) , which persisted at 1 h (**p < 0.01) and 3 h time points (**p < 0.01). By comparison, TPPB only induced the significant release of sAPPα at 3 h (*p < 0.05) ; however, TPPB at 10−10 M did not significantly increase the release of sAPPα at any of the time points tested  Fig. . At 10−805) Fig. . Bryosta05) Fig. . Bryostated Fig. .Fig. 2a−8, 10−9, and 10−10 M bryostatin-1 significantly increased the activation of PKC-α in SH-SY5Y cells (**p < 0.01)   ; 10−10 M TPPB did not activate PKC-α at any time point tested. A dose-dependent comparison of bryostatin-1 and TPPB showed that, at 3 h, PKC-δ was activated by 10−8 M bryostatin-1 (**p < 0.01), 10−9 M bryostatin-1 (*p < 0.05), and 10−10 M bryostatin-1 (*p < 0.05) , 1 h (**p < 0.01), and 3 h (**p < 0.01); by comparison, 10−9 M TPPB did not activate PKC-δ at any time point tested  and 3 h (**p < 0.01); by comparison, 10−10 M TPPB did not activate PKC-δ at any time point , 10−9 M bryostatin-1 (**p < 0.01), and 10−10 M bryostatin-1 (*p < 0.05) , 1 h (**p < 0.01), and 3 h (**p < 0.01) , 1 h (*p < 0.01), and 3 h (**p < 0.01)  following treatment with bryostatin-1 or TPPB. Confluent cultures of SH-SY5Y neuroblastoma cells were treated with different concentrations of either bryostatin-1 or TPPB for time points up to 3 h, when membrane and cytosolic pools of PKCs were isolated by differential detergent extraction, and Western-blotted for each individual isoform. Actin was also Western-blotted in each fraction to ensure equal loading. At 3 h, 1001) Fig. ; 10−8, 1C-α Fig. . A time 01) Fig. ; 10−9 M 01) Fig. . Bryosta05) Fig. ; TPPB di05) Fig. . A time ted Fig. . A time int Fig. . A dose-05) Fig. ; TPPB di05) Fig. . A time 01) Fig. ; by compted Fig. . A time 01) Fig. ; by compted Fig. .Fig. 3aThe presence of Aβ-laden cerebral plaques in AD, a central feature of Alzheimer’s disease (AD), is thought to contribute to the disturbances in nerve structure, function, and memory which characterize AD dementia  GABA(A)R-regulated post-synaptic currents, and (3) cholinergic signaling  activates α-secretase via PKC-α  and “novel” PKC isoforms to stimulate sAPPα processing  to enhance non-amyloidogenic processing of APP to sAPPα. Currently, the toxicological properties of TPPB are not fully known. An important goal in PKC–APP modulator drug design must be to overcome the potential carcinogenic properties of benzolactams/indolactams because TPPB, like TPA and other phorbol esters, may still retain tumor-promoting activity  of TPPB needed to reach equivalent α-secretase activation as bryostatin-1 which may hamper its use in human AD therapy. There are, of course, relative factors of availability and cost of bryostatin-1 versus reduced potency and higher toxicity of TPPB which can ultimately determine clinical use.By comparison, TPPB is a novel, synthetic cell-permeable benzolactam PKC activator which has been used as a standard APP modulator . Bryostatin-1 also appears to be a more active, rapid, and persistent APP modulator which reflects its greater specificity toward PKC-δ or PKC-ε isoform activation at low doses.Novel PKC activators are important candidate treatments for AD because they activate beneficial APP processing through α-secretase. We compared how PKC-α , -δ, and -ε (novel PKC isoforms) were activated in neuroblastoma cells by bryostatin-1 and TPPB as a function of time and concentration. Bryostatin-1 significantly induced PKC-α, -δ, and -ε activation at 10Here, we found that bryostatin-1 exerted a more rapid, potent, and sustained activation of APP processing , which was associated with its more potent and specific activation of PKC-δ and PKC-ε at low doses. The further refinement of bryostatin-1 pharmacology in PKC mobilization and α-secretase activation may help move this drug class more rapidly into clinical treatment for AD.


The pyridyl N atom of the Schiff base and the imino N atom of the 4-methyl-pyridine-2-ylimino ligand are not involved in the coordination. There is an intramolecular N—H⋯N hydrogen bond involving the pyridine N atom and the amino group of the 2-aminopyridine ligand. In the crystal, molecules are linked via N—H⋯Cl hydrogen bonds, forming chains propagating along [001].In the title complex, [Cu(C Cl(C6H8N2) = 0.055wR(F2) = 0.114S = 0.943339 reflections243 parameters2 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 0.40 e Å−3Δρmin = −0.45 e Å−3ΔρCrysAlis PRO  used to solve structure: SHELXS97  I, global. DOI: Click here for additional data file.10.1107/S1600536812047198/su2518Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The carboxylate groups of the HB ions are slightly twisted away from the attached benzene rings by 2.84 (15) and 4.8 (2)°. The planes of the two benzene rings of the HB ions are oriented with respect to each other at a dihedral angle of 84.41 (8)°. In the crystal, adjacent polymeric chains interact via O—H⋯O, N—H⋯O and weak C—H⋯O hydrogen bonds. The solvent water molecule links with the polymeric chains via O—H⋯O hydrogen bonding. π–π stacking between the benzene and pyridine rings and between the benzene rings [centroid–centroid distances = 3.731 (2) and 3.353 (2) Å] are present in the crystal.In the crystal of the title polymeric compound, {[Pb(C N,N-diethylnicotinamide, see: Bigoli et al. 2(C6H6N2O)]·H2O = 0.017wR(F2) = 0.050S = 1.194783 reflections304 parameters4 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 0.94 e Å−3Δρmin = −1.27 e Å−3ΔρAPEX2  used to solve structure: SHELXS97  I, global. DOI: 10.1107/S1600536812004357/xu5463Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


II atom in the polymeric title compound, {[Pb(C13H11N4O)]ClO4}n, is coordinated by the N′-[1-(pyridin-2-yl-κN)ethylidene]isonicotinohydrazidate ligand via its O,N,N′-donors and simultaneously bridged by a neighbouring ligand via the pyridin-2-yl N atom. The resultant supramolecular chain is a zigzag along the a axis. The stereochemistry of the PbII atom is defined by an N3OE donor set (E = lone pair of electrons), which results in a Ψ-trigonal–bipyramidal coordination with the O and pyridin-2-yl N atoms in axial positions. The dihedral angle between the pyridine rings of the ligand is 6.3 (3)°. The supramolecular cationic chains are linked into a three-dimensional array via secondary Pb⋯O [3.133 (6) and 3.28 (7) Å] and Pb⋯N [3.028 (4) Å] interactions. Weak C—H⋯O interactions and aromatic π–π stacking [centroid–centroid separation = 3.693 (2) Å] also occur in the crystal.The Pb N′-[1-(2-pyridyl)ethylidene]isonicotinohydrazide ligand, see: Maurya et al. ]ClO4                         = 0.022                           wR(F                           2) = 0.056                           S = 1.07                           2811 reflections218 parametersH-atom parameters constrainedmax = 0.55 e Å−3                        Δρmin = −0.45 e Å−3                        Δρ                                 SMART  used to solve structure: SHELXS97  global, I. DOI: 10.1107/S1600536811046691/hb6465Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The molecules are linked by O—H⋯O and O—H⋯N hydrogen bonds. Two types of π–π stacking interactions occur between the TPTZ ligands of adjacent complexes [centroid-to-centroid distances = 3.760 (4) and 3.870 (3) Å].In the title compound, [Nd(NO DOI: 10.1107/S1600536811014589/ff2007Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


One of the CuII ions is coordinated in a distorted square-planar geometry, whereas the other is coordinated in a distorted square-pyramidal geometry, the long apical Cu—O bond [2.885 (4) Å] of the square-pyramidal coordination being provided by a symmetry-related O atom creating a one-dimensional polymer along [010]. π–π stacking interactions [centroid–centroid distance = 3.783 (4) Å] and short interchain Br⋯Br interactions [3.6142 (12)–3.6797 (12) Å] are observed.The asymmetric unit of the title coordination polymer consists of a dinuclear neutral complex molecule of formula [Cu DOI: 10.1107/S1600536812029285/rz2776Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


Adjacent complex molecules are stacked through aromatic π–π interactions; the closest distance between adjacent aromatic rings is 3.598 (2) Å.In the mononuclear title compound, [ZnCl DOI: 10.1107/S1600536812022313/rk2337Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The four O atoms in the equatorial plane around the CoII cation form a slightly distorted square-planar arrangement, while the slightly distorted octahedral coordination is completed by the two N atoms of the NA ligands in the axial positions. The dihedral angle between the carboxylate group and the adjacent benzene ring is 23.91 (9)°, while the pyridine and benzene rings are oriented at a dihedral angle of 88.84 (4)°. The coordinating water molecule links with the carboxylate group via an intramolecular O—H⋯O hydrogen bond. In the crystal, N—H⋯O, O—H⋯O and weak C—H⋯O hydrogen bonds link the molecules into a three-dimensional supramolecular network. π–π stacking between the parallel benzene rings of adjacent molecules [centroid–centroid distance = 3.8505 (8) Å] may further stabilize the structure. A weak C—H⋯π interaction also occurs in the crystal.In the title complex, [Co(C N,N-diethylnicotinamide, see: Bigoli et al. 2(C6H6N2O)2(H2O)2] = 0.026wR(F2) = 0.069S = 1.053527 reflections216 parametersH atoms treated by a mixture of independent and constrained refinementmax = 0.42 e Å−3Δρmin = −0.36 e Å−3ΔρAPEX2  used to solve structure: SHELXS97  I, global. DOI: 10.1107/S1600536812032205/xu5597Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


This is only possible as the molecule has a hinged cis arrangement about the Pd2+ coordination spheres. For this hinged dimeric structure, the angles between the two coordination planes in each molecule are 21.59 (4) and 22.10 (4)°. This hinged cis arrangement also allows the two molecules to form pairs linked by secondary interactions between the Pd and Te atoms of an adjoining molecule, leading to a tetrameric overall structure. C—H⋯Cl interactions consolidate the crystal packing.The asymmetric unit of the title compound, [Pd For related structures of bridged dimers of palladium mediated by Se, see: Brown & Corrigan 2004; Chakrab al. 2011; Dey et  al. 2006; Ford et al. 2004; Kaur et al. 2009; Morley  al. 2006; Nakata  al. 2009; Oilunka al. 1999, 2001 ▶.2(C9H12NTe)2Cl2]·0.5CH2Cl2 = 0.039wR(F2) = 0.102S = 1.065506 reflections254 parametersH-atom parameters constrainedmax = 2.12 e Å−3Δρmin = −0.90 e Å−3ΔρAbsolute structure: Flack 1983, 2355 FrFlack parameter: 0.06 (4)APEX2  used to solve structure: SHELXS97  I, global. DOI: 10.1107/S1600536812000104/jj2116Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The CuII atom lies 0.065 (1) Å above the N2O2 plane and the Cu—O [2 × 1.945 (2) Å] and Cu—N bond lengths [1.968 (3) and 1.962 (3) Å] lie in expected ranges. The two aromatic ring planes make a dihedral angle of 85.48 (1)°.The molecular structure of the title compound, [Cu(C DOI: Click here for additional data file.10.1107/S1600536812046387/aa2076Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The metal-coordinated pyridine rings are almost coplanar, making a dihedral angle of 1.5 (2)°, while the two pendent pyrazine rings are arranged on the same side of the N—Ag—N line. Along the a axis, the mononuclear coordination units are stacked with π–π interactions between the pyridine rings [centroid–centroid distance = 3.569 (4) Å], leading to infinite chains. The chains are interconnected through intermolecular N(pyrazine)⋯π(pyrazine) interactions forming layers parallel to the ab plane [N⋯centroid = 3.268 (5) Å]. These layers are further stacked along the c-axis direction, furnishing a three-dimensional supramolecular framework with the tetrafluoridoborate anions embedded within the interstices.In the title mononuclear complex, [Ag(C DOI: 10.1107/S1600536811051270/zq2141Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the crystal, the complex cations and the monodeprotonated 2-carboxybenzoate anions are connected by O—H⋯O and N—H⋯O hydrogen bonds, forming a tape along [100]. Adjacent tapes are further linked into a three-dimensional arrangement via π–π stacking interactions between the triazole and benzene rings and between the pyridine and benzene rings [centroid–centroid distances = 3.6734 (14)/3.9430 (16) and 3.8221 (14) Å]. Intramolecular N—H⋯N and O—H⋯O hydrogen bonds are also observed.In the complex cation of the title salt, [Cu(C DOI: 10.1107/S1600536812000128/hy2503Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The coordination geometry around the CuII atom is square-pyramidal, comprising two N atoms from a symmetrically chelating 1,10-phenanthroline ligand, one O atom from a trichloroacetate ligand and two Cl− anions. In addition, there is a weak intramolecular Cu⋯O interaction of 2.9403 (14) Å involving the carbonyl O atom of the trichloroacetate ligand. The central Cu2Cl2 core takes the form of a rhombus, owing to the disparate Cu—Cl bond lengths. Molecules are connected in the crystal structure by C—H⋯Cl and C—H⋯O interactions.The title compound, [Cu II 1,10-phenanthroline complexes, see: De Burgomaster et al. 2Cl2(C12H8N2)2] = 0.026wR(F2) = 0.070S = 1.053233 reflections208 parametersH-atom parameters constrainedmax = 0.52 e Å−3Δρmin = −0.46 e Å−3ΔρCrysAlis PRO  used to solve structure: SHELXS97  global, I. DOI: 10.1107/S1600536812003947/bt5807Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


In the crystal, each palladium dimer is accompanied by a dichloromethane solvent molecule. Coordination of the carbonate and chelated phosphane ligands gives distorted square-planar environments at the Pd atoms. Important geometrical parameters include Pd—P(av.) = 2.2135 (4) Å, Pd—C(av.) = 1.9648 (16) Å and P—Pd—C = 84.05 (5) and 87.98 (5)°, and O—Pd—O′ = 60.56 (4) and 61.13 (4)°. Bonding with the carbonate O atoms shows values of 2.1616 (11) and 2.1452 (11) Å for the Pd—O—Pd bridge, whereas other Pd—O distances are slightly longer at 2.2136 (11) and 2.1946 (11) Å. One of the tert-butyl groups is disordered over two set of sites with an occupancy ratio of 0.723 (6):0.277 (6). Weak C—H⋯O interactions are observed propagating the molecules along the [100] direction. The title compound, [(μ DOI: Click here for additional data file.10.1107/S1600536812048702/yk2080Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


A chain along the c axis is formed by C—H⋯N hydrogen-bonding interactions and a weak π–π interaction is observed between the pyrimidine rings of two adjacent parallel chains [centroid–centroid distance = 3.722 (2) Å]. N—H⋯Cl, CN—H⋯Cl and N—H⋯O interactions also occur. In the title compound, (C DOI: 10.1107/S1600536811045995/vn2019Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The water molecules are involved in intra- and intermolecular O—H⋯O and O—H⋯Cl hydrogen bonding. Intermolecular N—H⋯O and N—H⋯Cl hydrogen bonds are formed between ligands. In addition, weak π–π interactions are observed between the benzene rings of the ligands [centroid–centroid distance = 3.580 (3) Å]. The intermolecular hydrogen bonds and π–π interactions lead to the formation of a three-dimensional supramolecular network.In the title complex, [NiCl H)-one, see: Turgunov & Englert (2010H)-one, see: Turgunov et al. (2010For a Cd(II) coordination polymer with quinazolin-42(H2O)2] = 0.052wR(F2) = 0.139S = 0.941686 reflections132 parameters2 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 0.75 e Å−3Δρmin = −0.51 e Å−3ΔρCrysAlis PRO  used to solve structure: SHELXS97  I, global. DOI: 10.1107/S1600536812019381/hg5221Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


Extensive intermolecular O—H⋯O, N—H⋯O and weak C—H⋯O hydrogen bonds lead to the stability of the crystal structure. Interactions between one C—H group of the 2,3-diaminopyridinium [+] cation and the aromatic ring of the pyridine-2,6-dicarboxylate (pydc) ligand (C—H⋯centroid distance = 2.78 Å) and π–π interactions between the + cations and between the + cation and the pydc ligand [centroid–centroid distances = 3.489 (5) and 3.694 (5) Å] are observed.In the centrosymmetric dinuclear complex anion of the title compound, (C DOI: 10.1107/S1600536811005629/hy2406Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The crystal structure is stabilized by π–π stacking interactions between the pyridine and benzene rings of adjacent molecules, with a centroid–centroid distance of 3.829 (2) Å.In the title centrosymmetric dinuclear complex, [Eu DOI: 10.1107/S1600536810046131/hy2358Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


III cations in the polymeric title compound, {[La2(C7H3NO4)3(H2O)4]·2H2O}n. One is nine-coordinated in an LaN2O7 tricapped trigonal–prismatic geometry formed by three pyridine-2,6-dicarboxylate anions and two water molecules, while the other is ten-coordinated in an LaNO9 bicapped square-antiprismatic geometry formed by four pyridine-2,6-dicarboxylate anions and two water molecules. The two LaIII cations are separated by a non-bonding distance of 5.026 (3) Å. The pyridine-2,6-dicarboxylate anions bridge the LaIII cations, forming a three-dimensional polymeric complex. The crystal structure contains extensive classical O—H⋯O hydrogen bonds and weak intermolecular C—H⋯O hydrogen bonds. The crystal structure is further consolidated by π–π stacking between pyridine rings, the shortest centroid–centroid distance between parallel pyridine rings being 3.700 (5) Å.There are two independent La DOI: 10.1107/S1600536811030807/xu5269Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


It is coordinated by two water molecules in the apical directions and four 4-fluorobenzoate (PFB) anions, bridging the symmetry related Mn atoms in the basal plane to form an infinite two-dimensional polymeric structure parallel to (100). The four O atoms of the PFB anions around the MnII atom form a slightly distorted square-planar arrangement, while the slightly distorted octahedral coordination is completed by the two O atoms of the water molecules. The dihedral angle between the carboxylate group and the adjacent benzene ring is 27.29 (16)°. The O—H⋯O hydrogen bonds further connect the manganese-carboxylate units. π–π contacts between the benzene rings [centroid-centroid distance = 3.6894 (15) Å] further stabilize the crystal structure.In the crystal structure of the title complex, [Mn(C N,N-diethylnicotinamide, see: Bigoli et al. 2(H2O)2] = 0.039                           wR(F                           2) = 0.111                           S = 1.28                           1758 reflections114 parametersH atoms treated by a mixture of independent and constrained refinementmax = 1.24 e Å−3                        Δρmin = −0.45 e Å−3                        Δρ                                 APEX2  used to solve structure: SHELXS97  I, global. DOI: 10.1107/S1600536811021921/su2282Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The coordination network can be described as an uninodal 4-connected net with the sql topology. The HgII ion lies on a site of -1 symmetry and the apym ligand lies on sites of m symmetry with the mirror plane perpendicular to the pyrimidine plane and passing through the NH2 group N atom. This polymeric structure is stabilized by N—H⋯Cl hydrogen bonds and columnar π–π stacking of pyrimidine rings, with a centroid–centroid distance of 3.832 (2) Å.The title compound, [HgCl For mer al. 2007. For the al. 2007; Xie & W al. 2007. For top al. 2007. For an  al. 2011. For our al. 2009, 2011 ▶.2(C4H5N3)] = 0.020wR(F2) = 0.049S = 1.12992 reflections52 parametersH-atom parameters constrainedmax = 0.84 e Å−3Δρmin = −1.01 e Å−3ΔρCrysAlis PRO  used to solve structure: SHELXS97  I, global. DOI: 10.1107/S1600536812008793/gk2458Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


II ion in the title compound, [Mn(CH3CO2)2(C15H11N3)]·2H2O, is seven-coordinated in a considerably distorted pentagonal–bipyramidal geometry by three N atoms of the tridentate 2,2′:6′,2′′-terpyridine ligand and four O atoms from two acetate anions which chelate the Mn atom via two O atoms. The lateral pyridine rings are slightly inclined to the central pyridine ring, making dihedral angles of 13.6 (2) and 5.7 (2)°. The complex and solvent water molecules are linked by intermolecular O—H⋯O hydrogen bonds into a three-dimensional network.The Mn For rel al. 2004; Rich et al. 2010.2H3O2)2(C15H11N3)]·2H2O = 0.055wR(F2) = 0.146S = 0.934936 reflections276 parameters4 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 0.69 e Å−3Δρmin = −0.52 e Å−3ΔρSMART  used to solve structure: SHELXS97  global. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The IrIII atom is coordinated by an η5-C5Me5 ligand, a chloride and a Ph2P(CH2)3SPh-κP,κS ligand, leading to a three-legged piano-stool geometry. In the crystal, two water molecules and two chloride anions are linked by weak O—H⋯Cl hydrogen bonding into tetramers that are located on centers of inversion. The H atoms of one of the methyl groups are disordered and were refined using a split model.The crystal structure of the title compound, [Ir(C For an  al. 2012.10H15)Cl(C21H21PS)]Cl·H2O = 0.041wR(F2) = 0.088S = 1.255513 reflections337 parameters147 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 1.68 e Å−3Δρmin = −1.50 e Å−3ΔρCrysAlis PRO  used to solve structure: SHELXS97  I, global. DOI: 10.1107/S1600536812021964/nc2278Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


An intramolecular N—H⋯O(carbonyl) hydrogen bond closes an S(6) ring. Supramolecular chains along [01-1] mediated by O—H⋯N(pyridine) hydrogen bonds feature in the crystal. A three-dimensional architecture is completed by π–π interactions occurring between the benzene ring and the two rings of the thienopyridine residue [centroid–centroid distances = 3.6963 (13) and 3.3812 (13) Å]. The F atom is disordered over the two meta sites in a near statistical ratio [0.545 (5):0.455 (5)].In the title compound, C DOI: 10.1107/S1600536812027195/hb6844Isup2.hklStructure factors: contains datablock(s) I. DOI: 10.1107/S1600536812027195/hb6844Isup3.cmlSupplementary material file. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


In the Me–salen ligand, the benzene rings are almost parallel, making a dihedral angle of 0.48 (13)°, but the torsion angle along the central C—C bond is 41.1 (2)°·The pyrrolidine rings are in slightly distorted chair conformations. The N atoms of the pyrrolidine axial ligands are involved in N—H⋯O hydrogen bonds with the perchlorate anions, and these hydrogen bonds connect the ionic species into infinite chains along the b axis. Some relatively short C—H⋯π interactions are also present in the crystal structure and C—H⋯O interactions occur. The guest solvent p-xylene molecule lies on a special position at the inversion centre.In the mononuclear title complex, [Co(C For rel al. 2003. For thebach 1969.       18H18N2O2)(C4H9N)2]ClO4·0.5C8H10                         = 0.040                           wR(F                           2) = 0.084                           S = 0.99                           7081 reflections502 parametersH atoms treated by a mixture of independent and constrained refinementmax = 0.67 e Å−3                        Δρmin = −0.51 e Å−3                        Δρ                                 CrysAlis PRO  used to solve structure: SIR92 (Altomare et al., 1993SHELXL97 (Sheldrick, 2008Stereochemical Workstation Operation Manual (Siemens, 1989SHELXL97.Data collection: 10.1107/S160053681004660X/jh2227sup1.cif            Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681004660X/jh2227Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The CeIII atom is coordinated by eight O atoms from six INAIP ligands and a water molecule in a distorted tricapped trigonal–prismatic geometry, while the AgI atom has a distorted trigonal–planar AgN2O geometry. O—H⋯O and N—H⋯O hydrogen bonds and π–π interactions between the pyridine and benzene rings [centroid–centroid distances = 3.642 (4) and 3.624 (3) Å] stabilize the crystal structure.The 4 DOI: 10.1107/S1600536811027668/hy2446Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The equatorial Cu—N and Cu—O bond lengths are in the range 1.979 (2)-1.998 (3) Å. The axial Cu—O bond distances are 2.365 (2) and 2.394 (2) Å. In the crystal, the complex cations and perchlorate anions are connected by numerous C—H⋯O hydrogen bonds, which leads to additional stabilization of the structure. The perchlorate anion is disordered over two sets of sites with a 0.716 (3):0.284 (3) occupancy ratio.The title compound, [Cu(C DOI: 10.1107/S1600536813018485/nr2046Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The Ag—C and Ag—Cl single-bond lengths are 2.087 (3) and 2.3267 (9) Å. The C—Ag—Cl bond angle is 172.84 (7)°. C—H⋯π interactions contribute to the stabilization of the crystal structure. A very weak π–π stacking interaction between adjacent tetramethylbenzene rings [centroid–centroid distance = 4.0610 (18) Å] is also observed.In the title compound, [AgCl(C DOI: 10.1107/S1600536812012998/sj5223Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


Each AgI ion is bicoordinated in a slightly distorted linear coordination geometry by the N atoms of two ligands, resulting in the formation of a 22-membered metallamacrocycle. In the dication, π–π interactions are observed between the imidazole rings, with centroid–centroid distances of 3.528 (3) Å and dihedral angles of 9.92 (9)°. The crystal structure is stabilized by intermolecular O—H⋯O hydrogen bonds and π–π interactions involving the benzene rings of adjacent dications, with centroid–centroid distances of 3.651 (2) Å.In the title compound, [Ag DOI: 10.1107/S1600536811018691/rz2589Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The CoII atom is situated on a crystallographic center of inversion and is octahedrally coordinated by two O atoms from two anions, two N atoms of two 1,2-bis(pyridin-4-yl)ethane molecules and two O atoms from two water molecules. A three-dimensional network is established by intermolecular O—H⋯O and O—H⋯N hydrogen bonds.The asymmetric unit of the title compound, [Co(C For general background to the design of metal-organic supramolecular solids with potential functionality, see: Moulton & Zaworotko 2001; Janiak 9H7O4)2(C12H10N2)2(H2O)2] = 0.055                           wR(F                           2) = 0.105                           S = 1.06                           3635 reflections268 parametersH atoms treated by a mixture of independent and constrained refinementmax = 0.71 e Å−3                        Δρmin = −0.36 e Å−3                        Δρ                                 SMART  used to solve structure: SHELXS97  global, I. DOI: 10.1107/S1600536811024755/im2300Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The CuII atom lies on a crystallographic twofold rotation axis and shows a significantly distorted tetrahedral coordination geometry. The dihedral angle between the phenyl rings is 74.3 (2)°. The crystal structure is stabilized by intermolecular π–π interactions [centroid–centroid distances = 3.635 (2)–3.803 (3) Å].The asymmetric unit of the title compound, [CuCl DOI: 10.1107/S1600536811050690/rz2665Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Intermolecular C—H⋯Cl hydrogen bonds and π–π contacts between the pyridine rings [centroid–centroid distance = 3.510 (3) Å] are present in the crystal.In the title compound, [InCl DOI: 10.1107/S1600536812038147/hy2584Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


One AgI ion is coordinated by one O atom from a 3-carboxylato-4-hydroxybenzenesulfonate (L) ligand, two N atoms from two pyrazine ligands and a water molecule. The other AgI ion is coordinated by two O atoms from two L ligands and one N atom from a pyrazine ligand. One of the pyrazine ligands lies on an inversion center. The L and pyrazine ligands link the AgI ions into polymeric layers parallel to the ac plane. The layers are connected by intermolecular O—H⋯O hydrogen bonds. An intramolecular O—H⋯O hydrogen bond is also present in the L ligand.The title coordination polymer, {[Ag For a related structure, see: Nie & Qu 2011.       4(C7H4O6S)2(C4H4N2)3(H2O)2]·2H2O = 0.033                           wR(F                           2) = 0.073                           S = 0.88                           3387 reflections256 parameters5 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 0.70 e Å−3                        Δρmin = −1.09 e Å−3                        Δρ                                 SMART  used to solve structure: SHELXS97  global, I. DOI: 10.1107/S1600536811041626/hy2474Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The coordination environment of each ReI atom is distorted octahedral. Four intramolecular O—H⋯N and four intermolecular C—H⋯O hydrogen-bond interactions are observed. Relatively strong hydrogen bonds are found between the hydrogen-bond donor (μ3-OH) and acceptor (basic N atom of pyridine), with N⋯O distances between 2.586 (10) and 2.628 (10) Å. Intercube distances of 9.873 (2) and 12.376 (3) Å are observed.The title compound, [Re DOI: 10.1107/S1600536812036033/hg5243Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


Each RhI atom is coordinated by one O atom [Rh—O = 2.044 (2) and 2.026 (2) Å], one N atom [Rh—N = 2.083 (2) and 2.090 (2) Å], and one COD ligand via two η2-bonds, each directed toward the mid-point of a C=C bond (Cg): Rh—Cg = 2.007 (2), 2.013 (2), 2.000 (2) and 2.021 (2) Å. Each RhI atom has a quasi-square-planar coordination geometry, with average r.m.s. deviations of 0.159 (1) and 0.204 (1) Å from the mean planes defined by Rh and the termini of its four coordinating bonds. The two COD ligands have quasi-C2 symmetry, twisted from ideal Cv2 symmetry by 30.0 (3) and −33.1 (3)°, and are quasi-enantiomers of one another. The intramolecular Rh⋯Rh distance of 5.9432 (3) Å suggests that there is no direct metal–metal interaction.In the title solvate, [Rh DOI: 10.1107/S1600536812040603/cv5334Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The water ligands of the core are involved in hydrogen bonds with the triazole N atoms of the organic molecules, which generates a layer motif in the ab plane. There are π–π stacking interactions between benzene rings of 3.490 (6) Å, and between triazole rings of 3.543 (8) and 3.734 (7) Å in neighboring layers, forming a three-dimensional network.The title complex, [Fe DOI: 10.1107/S160053681202613X/pk2413Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


II atom in the title salt, [Cu(C10H24N4)(H2O)2](C8H7O2)2·H2O, is chelated by the four N atoms of the 1,4,8,11-tetraazacyclotetradecane (cyclam) ligand and is coordinated by two water molecules in a Jahn–Teller-type of tetragonally distorted octahedral geometry. The cations, anions and lattice water molecules are linked by N—H⋯O and O—H⋯O hydrogen bonds to form a layer structure parallel to (001).The Cu DOI: 10.1107/S1600536810026012/bt5288Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In each molecule, the fused six-membered rings have chair–chair–chair–chair conformations and the cyclopentane ring adopts an envelope conformation with the C atom bearing the hydroxymethyl group as the flap. All ring junctions are trans-fused. With the exception of one of the methyl groups adjacent to the C=O group, all the methyl groups are in axial positions. The isopropenyl group is equatorial and the hydroxymethyl group is in an axial orientation. In the crystal, weak C—H⋯O interactions link the molecules into chains along [010]. Weak intramolecular C—H⋯O hydrogen bonds are also observed but the hydroxy groups are not involved in hydrogen bonds.The asymmetric unit of the title compound, C Åb = 19.1818 (6) Åc = 28.1141 (7) ÅV = 5093.3 (3) Å3Z = 8Kα radiationMo −1μ = 0.07 mmT = 100 K0.60 × 0.56 × 0.20 mmOxford Diffraction diffractometer with a Sapphire3 detectorCrysAlis RED; Oxford Diffraction, 2008Tmin = 0.960, Tmax = 0.986Absorption correction: multi-scan (61473 measured reflections5036 independent reflectionsI > 2σ(I)4401 reflections with Rint = 0.055R[F2 > 2σ(F2)] = 0.051wR(F2) = 0.141S = 1.035036 reflections609 parametersH atoms treated by a mixture of independent and constrained refinementmax = 0.55 e Å−3Δρmin = −0.50 e Å−3ΔρCrysAlis CCD  used to solve structure: SHELXS97  I, global. DOI: Click here for additional data file.10.1107/S1600536813011008/lh5603Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The pyridinium rings are almost planar [maximum deviations = 0.004 (4) and 0.003 (4) Å]. The ethyl groups are approximately perpendicular to the corresponding pyridinium ring planes [N—C—C—C = 88.8 (4)° in each ligand]. The packing of the molecules is controlled by π–π interactions, with centroid–centroid distances of 3.625 (3) and 3.711 (2) Å, forming chains approximately parallel to (102). The crystal studied was non-merohedrally twinned .In the bioactive title compound, [ZnBr DOI: 10.1107/S1600536810052190/sj5050Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Two O,O′-bis(4-methylphenyl)dithiophosphate anions occupy the axial positions with long Cu⋯S distances of 3.0090 (8) Å. Intermolecular N—H⋯S and C—H⋯S hydrogen bonding is present between the anions and the cation.In the title compound, [Cu(C DOI: 10.1107/S1600536810046672/xu5079Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Four symmetry-equivalent mesitylacetamidate ligands bridge the Rh—Rh unit. Thus, each RhII atom has an approximately octahedral coordination by one Rh [Rh—Rh = 2.4290 (6) Å], two acetamidate O atoms trans to each other [Rh—O = 2.044 (3) Å], two acetamidate N atoms trans to each other [Rh—N = 2.091 (4) Å], and a benzonitrile N atom trans to Rh [Rh—N = 2.222 (3) Å]. The structure is held together by weak van der Waals forces.The title structure, [Rh DOI: 10.1107/S1600536812024518/qk2033Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


In the crystal, molecules are linked by O—H⋯O hydrogen bonds, generating [001] C               2               2(4) chains such that molecules A and B alternate. There is no aromatic π–π stacking in the crystal as the shortest centroid–centroid distance is greater than 4.74 Å.The previous structure determination [Gillier-Pandraud  al. 1972. C. R. A DOI: 10.1107/S1600536811013547/hb5838Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


II(TpivPP) {TpivPP is the dianion of 5,10,15,20-tetrakis[2-phenyl]porphyrin} with an excess of KCN salts and an excess of the 18-crown-6 in chlorobenzene leads to the polymeric title compound catena-polyporphyrinato-1κO5:2κ4N,N′,N′′,N′′′:1′κO15}cobalt(III)potassium] dihydrate], {[CoK(CN)2(C12H24O6)(CN)2]− ion complex and one half of a . In the crystal, the polymeric chains and the lattice water molecules are linked by N—H⋯O and O—H⋯N hydrogen bonds, as well as weak C—H⋯O, O—H⋯π and C—H⋯π interactions into a three-dimensional supramolecular architecture.The reaction of Co DOI: 10.1107/S1600536814003596/xu5770Isup2.hklStructure factors: contains datablock(s) I. DOI: 987431CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The asymmetric unit contains one half of the [Mg(TPP)(H2O)2] complex and one half of an 18-crown-6 molecule. The average equatorial magnesium–pyrrole N atom distance (Mg—Np) is 2.071 (1) Å and the axial Mg—O(H2O) bond length is 2.213 (1) Å. The crystal packing is stabilized by two O—H⋯O hydrogen bonds between coordinating water molecules and adjacent 18-crown-6 molecules, and exhibits a one-dimensional supramolecular structure along the a axis. The supramolecular architecture is futher stabilized by weak C—H⋯π interactions. The 18-crown-6 molecule is disordered over two sets of sites with an occupancy ratio of 0.8:0.2.In the title compound, [Mg(C DOI: Click here for additional data file.10.1107/S1600536813001219/xu5669Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


In the crystal, O—H⋯O and N—H⋯O hydrogen bonds link the molecules into a three-dimensional supramolecular network. π–π stacking interactions between the imidazole rings [centroid–centroid distances = 3.4914 (15) and 3.6167 (15) Å] further stabilize the crystal structure. In the title compound, [Co(C DOI: 10.1107/S1600536812037579/hy2579Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The CuI atom has a distorted tetrahedral coordination. The O—Cu—O angle is 80.07 (8)° and the P—Cu—P angle is 123.49 (3)°. The crystal packing is stablized by intramolecular C—H⋯O interactions and intermolecular C—H⋯O and O—H⋯O interactions.In the title compound, [Cu(C DOI: 10.1107/S1600536811011470/fi2105Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The ligator atoms comprise the two pyridine N atoms of the chelating di-2-pyridylamine (dpa) ligand and two N atoms from two azide anions. The dpa ligand coordinates the Pd atom in a boat conformation, the dihedral angle between the pyridine rings being 24.4 (1)°. The pyridine rings are somewhat inclined to the least-squares plane of the PdN4 unit, making dihedral angles of 29.02 (9) and 26.47 (9)°. The azide ligands are slightly bent, with N—N—N angles of 173.0 (4) and 174.2 (4)°. In the crystal, molecules are connected by N—H⋯N and C—H⋯N hydrogen bonds, forming chains along the c axis. When viewed down the b axis, successive chains are stacked in opposite directions. Intramolecular C—H⋯N hydrogen bonds are also observed.In the title complex, [Pd(N II complexes [PdX2(dpa)] (X = Cl or Br), see: Rauterkus et al. 2(C10H9N3)] = 0.029wR(F2) = 0.073S = 1.062322 reflections181 parametersH-atom parameters constrainedmax = 0.71 e Å−3Δρmin = −0.41 e Å−3ΔρSMART  used to solve structure: SHELXS97  global. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


These two constituents are linked by a remarkably short interaction between the Br atom of the imidazolium cation [C—Br = 1.85 (3) Å] and one N atom of the cyanidoargentate anion [Br⋯N = 2.96 (2) Å], which is much less than the sum of the van der Waals radii (3.40 Å). The crystal studied was twinned by merohedry.The title structure, (C DOI: 10.1107/S1600536811051828/qk2020Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The CoIII atom exhibits an octahedral geometry, coordinated by four N atoms from the tris(2-pyridylmethyl)amine ligand with an average Co—N distance of 1.953 (2) Å, and two cyanide C atoms with an average Co—C distance of 1.895 (2) Å. The crystal packing is stabilized by intermolecular C—H⋯N and C—H⋯F interactions.In the title complex, [Co(CN) DOI: 10.1107/S1600536811012001/vm2083Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the central Ti2(μ2-O)2 fragment, the metal–oxygen distances are significantly different [1.7962 (19) and 1.9292 (19) Å]. In the crystal, the chloroform molecule is anchored via an N—H⋯Cl and a bifurcated C—H⋯ hydrogen bond. Slipped π–π stacking [shortest C⋯C distance = 3.585 (4) Å] and C—H⋯π interactions contribute to the coherence of the structure.In the title structure, [Ti DOI: 10.1107/S1600536813029656/qk2062Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S1600536813029656/qk2062Isup3.molSupplementary material file. DOI: 969061 crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The two LaIII metal ions are linked by two bidentate bridging carboxylate groups with a κ2               O:O′ coordination mode and two bidentate chelating bridging carboxylate groups with a κ3               O:O,O′ coordination mode. The coordination sphere of lanthanum, completed by a terminal chloride and three water molecules, adopts a distorted tricapped trigonal–prismatic arrangement. N—H⋯Cl, N—H⋯O and O—Hwater⋯Cl hydrogen bonds, and slipped π–π interactions between parallel benzene rings [centroid–centroid distance of 3.647 (3) Å] are observed in the structure. These combine to stabilize a three-dimensional network.The tiltle complex, [La DOI: 10.1107/S1600536810052864/su2239Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The Ru—Ru distance and Ru—O—Ru angle are 3.2838 (3) Å and 121.79 (7)°, respectively, and the average Ru—N(pyridine) bond length is 2.164 (8) Å. Several C—H⋯F, C—H⋯O and C—H⋯N interactions generate a three-dimensional network in the crystal structure. π–π stacking interactions [centroid–centroid distance = 3.6389 (3) Å] between inversion-related 2,2′-bipyridine rings are also observed.The hemerythrin-type dinuclear title complex, [Ru DOI: Click here for additional data file.10.1107/S1600536813003334/gg2109Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The dihedral angles between the oxazole rings and their pendant rings are 2.0 (3) and 24.3 (2)°. The F atoms are disordered over two sites with occupancies of 0.627 (3) and 0.373 (3) in the phenylene–oxazolyl–phenyl and in oxazolyl–phenyl fragments, respectively. In the crystal structure, molecules are linked through a network of C—H⋯F and weak π–π stacking interactions.In the title compound, C DOI: 10.1107/S1600536810031235/fb2208Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The cation has a distorted octahedral coordination environment and is surrounded by two N and two Cl atoms in the equatorial plane, while the coordinating water O atoms occupy the axial positions. The crystal exhibits nonmerohedral twinning with two domain states, the volume fractions of which were refined to 0.883 (2) and 0.117 (3). The crystal packing is stabilized by O—H⋯Cl hydrogen-bond interactions, forming two-dimensional networks lying parallel to (001). The crystal packing also features π–π interactions between the pyridine rings, with centroid–centroid separations of 3.493 (3) and 3.545 (3) Å.The title molecule, [CoCl For related structures, see: Li et al. 2(H2O)2] = 0.047wR(F2) = 0.149S = 1.162211 reflections88 parameters3 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 0.71 e Å−3Δρmin = −0.99 e Å−3ΔρCrysAlis CCD  used to solve structure: SHELXS97  global, I. DOI: 10.1107/S1600536813022484/fb2288Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


In each molecule, the four-coordinated SnIV atom exists in a distorted tetrahedral geometry and two intramolecular N—H⋯O hydrogen bonds with S(6) ring motifs are present. In one molecule, the benzene ring of the 2-amino-3-nitrobenzoate ligand makes dihedral angles of 42.74 (11), 89.66 (13) and 53.04 (10)° with the three phenyl rings. The corresponding dihedral angles for the other molecule are 6.29 (11), 66.55 (11) and 62.33 (10)°. In the crystal, a weak intermolecular C—H⋯π interaction and a π–π stacking interaction with a centroid–centroid distance of 3.5877 (12) Å are observed.The asymmetric unit of the title compound, [Sn(C DOI: 10.1107/S160053681101244X/is2696Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Each PdII ion has a distorted square-planar coordination sphere, defined by three N atoms of the macrocyclic ligand and a chloride ion. The PdII complex cations and the methanol molecules are linked through N—H⋯O and O—H⋯O hydrogen bonds, forming a zigzag chain along [101]. An intramolecular N—H⋯Cl hydrogen bond is also observed.In the crystal structure of the title compound, [Pd For dipters 2010; Goforth al. 2013. For pal al. 2013; Parker  al. 1985. For a s al. 2003. For a s al. 2010.2(C36H42N6)Cl2](ClO4)2·2C3H7NO·2CH4O = 0.038wR(F2) = 0.097S = 1.085826 reflections324 parametersH atoms treated by a mixture of independent and constrained refinementmax = 0.80 e Å−3Δρmin = −0.81 e Å−3ΔρCrystalClear  used to solve structure: SIR92  global, I. DOI: 10.1107/S1600536813022666/is5294Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The compound is a tetranuclear ZnII complex centered about a fourfold roto-inversion axis, with the ligand coordinating in the doubly deprotonated form. The ZnII atom has a distorted square-pyramidal geometry being coordinated by one N and two O-atom donors from the doubly deprotonated L2− ligand, and by one N atom and one O-atom donor from a symmetry-related L2− ligand. In the crystal, four symmetry-related lattice water molecules, centred about a fourfold roto-inversion axis, form a cyclic tetramer through O—H⋯O hydrogen bonds. These tetramers connect to the complex molecules through O—H⋯N hydrogen bonds, forming a chain propagating along [100]. Neighbouring molecules are linked by π–π interactions [centroid–centroid distance = 3.660 (2) Å] involving the quinolidine rings.In the title compound, [Zn N-donor ligands, see: Palacios et al. 4]·4H2O = 0.036wR(F2) = 0.087S = 1.032900 reflections217 parametersH-atom parameters constrainedmax = 0.27 e Å−3Δρmin = −0.23 e Å−3ΔρSMART  used to solve structure: SHELXS97  I, global. DOI: 10.1107/S1600536812018995/su2415Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


One RhII atom is five-coordinate, in a distorted pyramidal geometry, while the other is six-coordinate, with a disorted octahedral geometry. For the six-coordinate RhII atom, the axial nitrile ligand shows a non-linear Rh–nitrile coordination with an Rh—N—C bond angle of 166.4 (4)° and a nitrile N—C bond length of 1.138 (6) Å. Each unique RhII atom is coordinated by a trans pair of N atoms and a trans pair of O atoms from the four acetamide ligands. The Neq—Rh—Rh—Oeq torsion angles on the acetamide bridge varies between 12.55 (11) and 14.04 (8)°. In the crystal, the 3-methylbenzonitrile ring shows a π–π interaction with an inversion-related equivalent [interplanar spacing = 3.360 (6) Å]. A phenyl ring on one of the acetamide ligands also has a face-to-face π–π interaction with an inversion-related equivalent [interplanar spacing = 3.416 (5) Å].In the title compound, [Rh DOI: 10.1107/S1600536813029838/pk2497Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


Am. Mineral.54, 19–30], all non-H atoms were refined with anisotropic displacement parameters and H-atoms were located by difference Fourier methods and refined from X-ray diffraction data. The structure is built up from nearly regular [Al(H2O)6]3+ octahedra and infinite double-stranded chains [Na(SO4)2]3− that extend parallel to [001]. The Na+ cation has a strongly distorted octahedral coordination by sulfate O atoms [Na—O = 2.2709 (11) – 2.5117 (12) Å], of which five are furnished by the chain-building sulfate group S2O4 and one by the non-bridging sulfate group S1O4. The [Na(SO4)2]3− chain features an unusual centrosymmetric group formed by two NaO6 octahedra and two S2O4 tetrahedra sharing five adjacent edges, one between two NaO6 octahedra and two each between the resulting double octahedron and two S2O4 tetrahedra. These groups are then linked into a double-stranded chain via corner-sharing between NaO6 octahedra and S2O4 tetrahedra. The S1O4 group, attached to Na in the terminal position, completes the chains. The [Al(H2O)6]3+ octahedron (〈Al—O〉 = 1.885 (11) Å) donates 12 comparatively strong hydrogen bonds (O⋯O = 2.6665 (14) – 2.7971 (15) Å) to the sulfate O atoms of three neighbouring [Na(SO4)2]3− chains, helping to connect them in three dimensions, but with a prevalence parallel to (010), the cleavage plane of the mineral. Compared with the previous work on tamarugite, the bond precision of Al—O bond lengths as an example improved from 0.024 to 0.001 Å.The crystal structure of tamarugite [sodium aluminium bis(sulfate) hexahydrate] was redetermined from a single crystal from Mina Alcaparossa, near Cerritos Bayos, southwest of Calama, Chile. In contrast to the previous work [Robinson & Fang 1969. Am. Min DOI: 10.1107/S1600536813025154/pj2005Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The crystal structure is stabilized by weak intermolecular C—H⋯O and C—H⋯π(arene) interactions. The Ru—η5-cyclopentadienyl centroid bond length is 1.946 (11) ÅIn the title molecule, [Ru(C DOI: 10.1107/S1600536810033180/lh5113Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The metal atom is further chelated by a carboxylate group and is covalently bonded to a monodentate carboxylate group as well as to a monodentate sulfonate group in a distorted square antiprismatic geometry. The coordinating water molecules and the lattice water molecules, one of which is disordered over two positions [major component 65 (3)%], are hydrogen bonded to the network.The 4-sulfophthalate trianion in the polymeric complex, {[Er(C III derivative, see: Xiao et al. Eu al. 2010.8H3O7S)(C12H8N2)(H2O)2]·2H2O = 0.037wR(F2) = 0.095S = 1.094014 reflections353 parameters33 restraintsH atoms treated by a mixture of independent and constrained refinementmax = 0.97 e Å−3Δρmin = −1.21 e Å−3ΔρAPEX2  used to solve structure: SHELXS97  global, I. DOI: 10.1107/S1600536812003467/xu5455Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


II atom in the title compound, {[Pb2(C7H6NO2)4]}n, is chelated by two 3-aminobenzoato ligands in a distorted pentagonal-bipyramidal coordination geometry with five oxygen donors in the equatorial positions, one nitrogen donor and one oxygen donor in the axial positions. Two molecules are linked through a centre of inversion, forming a dinuclear entity. These entities are linked in a μ3-bridging mode through the amino N atom and two carboxylate O atoms into a chain along the b axis. Classical intermolecular N—H⋯O hydrogen bonding is observed in the structure. The supramolecular structure is consolidated by π–π stacking interactions with  centroid–centroid distances between benzene rings of 3.837 (8) Å.The Pb DOI: 10.1107/S1600536810041322/rk2229Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the trigonal–pyramidal Ru3P core, one RuII atom is coordinated by a triphenylphosphane ligand in a terminal fashion. Two hydride ligands bridge over two Ru—Ru bonds. These Ru—Ru bonds [2.9400 (4) and 2.9432 (4) Å] are slightly longer than the nonhydride-bridged Ru—Ru bond [2.8146 (4) Å]. The terminal triphenylphosphane ligand coordinates to the RuII atom, which is involved in two hydride bridges.In the crystal structure of the title compound, [Ru H2(C18H15P)(CO)8] = 0.030wR(F2) = 0.118S = 1.238304 reflections444 parametersH atoms treated by a mixture of independent and constrained refinementmax = 0.74 e Å−3Δρmin = −1.79 e Å−3ΔρPROCESS-AUTO  I, global. DOI: 10.1107/S1600536812039499/nc2293Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The carbonyl and chloride ligands in the cation adopt a mutually cis arrangement and these are disordered over two sets of sites with site occupancies of 0.721 (6) and 0.279 (6). The Ru—N bond length [2.117 (2) Å] trans to the carbonyl ligand is slightly longer than the average of the other Ru—N bond lengths (2.08 Å), which can be explained by the expected trans influence of the carbonyl group. In the crystal, weak C—H⋯F interactions are observed between the complex cation and the PF6− anion, leading to the formation of a three-dimensional supramolecular structure. The crystal studied was an inversion twin with twin fractions of 0.78 (4) and 0.22 (4).In the title compound, [RuCl(C Cl]+, see: Ishida et al. 2(CO)]·PF6 = 0.032wR(F2) = 0.062S = 1.085177 reflections330 parametersH-atom parameters constrainedmax = 1.37 e Å−3Δρmin = −1.28 e Å−3ΔρAbsolute structure: Flack 1983, 2249 FrFlack parameter: 0.22 (4)CrystalClear-SM  used to solve structure: SIR97  global, I. DOI: Click here for additional data file.10.1107/S1600536812048246/is5220Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The molecular structure is stabilized by weak C—H⋯O and C—H⋯F hydrogen-bond interactions. The crystal structure is stabilized by π–π stacking interactions (centroid–centroid distance = 3.951 Å).The title compound, [Ir(C DOI: 10.1107/S1600536813026160/bx2449Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


In the crystal, pairs of molecules form inversion dimers via N—H⋯Cl hydrogen bonds. In addition, intramolecular N—H⋯Cl and weak C—H⋯Cl, C—H⋯N, N—H⋯π and C—H⋯π hydrogen bonds are observed. One of the Cl atoms of the solvent molecule is disordered over two sites with refined occupancies of 0.62 (1) and 0.38 (1).In the title compound, [RuCl DOI: 10.1107/S1600536812014080/lh5442Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


Within the pcp ligands, the dihedral angles between the polycyclic skeletons and pendant pyridine rings are 6.2 (2) and 8.3 (2)°. In the crystal, molecules are linked by O—H⋯N and N—H⋯O hydrogen bonds. Several aromatic π–π stacking interactions [shortest centroid–centroid separation = 3.516 (3) Å] are also observed.In the title compound, [Mn(C DOI: 10.1107/S1600536811004569/hb5800Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The NiII atom is in a distorted octahedral coordination by two N atoms in a cis disposition [Ni—N = 2.0753 (16) and 2.1048 (16) Å] and by four water O atoms [Ni—O = 2.0500 (15)–2.0822 (15) Å]. The crystal structure is completed by four further non-coordinating water molecules and all constituents are linked in a three-dimensional manner by an extensive system of 16 O—H⋯O hydrogen bonds.The title structure, [Ni(C DOI: 10.1107/S1600536812027122/qk2036Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The 4-(dimethylamino)pyridinium cations are protonated at the pyridine N atoms and form N—H⋯Cl hydrogen bonds with Cl− counter-ions. The dimethylamino groups (C/N/C) lie close to the plane of the pyridinium rings, making dihedral angles of 1.6 (6)° and 6.5 (3)°. In the crystal, the [Nd2Cl4(H2O)10]2+ dications are linked via O—H⋯O and O—H⋯Cl hydrogen bonds, forming sheets lying parallel to the bc plane. These sheets are linked via O—H⋯Cl hydrogen bonds, forming a three-dimensional network. The 4-(dimethylamino)pyridinium cations are located in the cavities and linked to the framework by C—H⋯Cl interactions.The title compound, (C DOI: Click here for additional data file.10.1107/S1600536812041724/su2506Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


II complex, [Cu(C7H3NO4)(C6H5NO2)(H2O)]·H2O, the environment of the Cu2+ ion is a distorted square pyramid with the axial site occupied by the O atom from the coordinated water molecule and the square base formed by two O and two N atoms from the tridentate anion and the neutral monodentate pyridine-3-carboxylic acid ligand. O—H⋯O hydrogen bonds, as well as π–π interactions [centroid–centroid distance = 3.945 (3) Å] contribute to the stabilization of this structure.In the title Cu DOI: 10.1107/S160053681101926X/yk2006Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


Intermolecular C—H⋯Br hydrogen bonds and π–π stacking between the pyridine rings in the bc plane [centroid–centroid distance = 3.725 (3) Å] are present in the crystal structure.In the title compound, [CoBr DOI: Click here for additional data file.10.1107/S1600536812041980/xu5630Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


The crystal packing exhibits a short O⋯Br interaction [Br⋯O = 3.185 (3) Å] and a weak intermolecular C—H⋯O contact.The title compound, C DOI: 10.1107/S1600536811010051/fy2003Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The octahedral environment around niobium is slightly distorted with Nb—O distances in the range 1.8603 (15)–2.1083 (15) Å and an Nb—Cl distance of 2.4693 (9) Å. The O—Nb—O angles vary between 80.74 (6) and 100.82 (7)°, while the trans Cl—Nb—O angle is 167.60 (5)°. There are no hydrogen bonds observed, only an intermolecular C—H⋯O interaction.In the title compound, [Nb(CH DOI: 10.1107/S1600536810021719/pv2289Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the crystal, the components are linked into a three-dimensional framework by intermolecular O—H⋯O, N—H⋯O and N—H⋯N and weak C—H⋯O hydrogen bonds. In addition, π–π stacking interactions with centroid–centroid distances in the range 3.4809 (7)–3.8145 (6) Å are observed.The asymmetric unit of the title complex, (C DOI: 10.1107/S1600536811027917/lh5282Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the crystal structure, weak intermolecular C—H⋯O hydrogen bonds connect molecules into chains along [100] and there are π–π stacking interactions between pairs of chains with a centroid–centroid distance of 3.5485 (15) Å.In the title compound, C DOI: 10.1107/S160053681002979X/lh5093Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The CdII atom is seven-coordinated in a distorted pentagonal–bipyramidal configuration, defined by five O atoms from the carboxylate groups of three 7-oxabicyclo[2.2.1]heptane-2,3-dicarboxylato ligands and two N atoms from the 2,2′-bipyridine ligand. Two O atoms link two CdII atoms, forming a dinuclear center: the Cd—O—Cd bridging angle is 110.19 (6)°. The polymeric structure extends along [100] and is linked by intermolecular O—H⋯O hydrogen bonds involving the solvent water molecule. Extensive π–π stacking exists between 2,2-bypiridine ligands along [010] with centroid-centroid distance of 3.650 (2) ÅThe title compound, {[Cd(C DOI: 10.1107/S1600536811036634/zb2016Isup2.hkl            Structure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the crystal, the components are linked via intermolecular O—H⋯O hydrogen bonds, forming layers parallel to (001). Additional stabilization within these layers is provided by π–π [centroid–centroid distances of 3.7848 (9)–4.4231 (9) Å] stacking interactions.The central CuN DOI: 10.1107/S1600536811013808/bq2292Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The range of Ag—O bond lengths is 2.169 (2)–2.433 (2) Å, whereas the Ag⋯Ag separations are in the range 2.8674 (4)–3.6256 (5) Å. The 2-methylbenzoate groups are oriented at a dihedral angle of 60.7 (1)° with respect to each other.The crystal structure of the title compound, [Ag DOI: 10.1107/S1600536811016801/ez2241Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


In the crystal, the dinuclear complex molecules are linked into one-dimensional supramolecular columns parallel to the b axis by O—H⋯N hydrogen bonds and π–π stacking interactions [centroid–centroid distance = 3.7259 (11) Å].The title complex, [Cu DOI: 10.1107/S1600536812039839/rz5004Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


Intramolecular O—H⋯N hydrogen bonds between the hydroxy O atoms and the imine N atoms, with O⋯N distances in the range 2.607 (3)–2.665 (3) Å, form nearly planar six-membered rings. In the crystal, weak intermolecular C—H⋯O and C—H⋯N hydrogen bonds occur and several intra- and intermolecular π–π interactions are present between adjacent benzene rings, with a shortest centroid–centroid distance of 3.507 (2) Å.In the title compound, C DOI: 10.1107/S1600536810047185/is2631Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The HgII atom is four-coordinated in a distorted tetrahedral geometry by one terminal Cl atom, two bridging Cl atoms, and one C atom from the ylidic ligand, resulting in a polymeric chain parallel to [010]. The terminal Cl atom is more strongly bound to the HgII ion [2.3916 (9) Å] than the bridging Cl atoms. The bridge is asymmetric, as indicated by the two different Hg—Cl(bridging) bond lengths [2.5840 (8) and 2.7876 (8) Å]. Intramolecular C—H⋯O and weak C—H⋯Cl contacts stabilize the polymeric chain. In the crystal, adjacent chains interact via C—H⋯O hydrogen bonds. In the title organometallic polymer, [HgCl II complex, see: Ebrahim et al. ] = 0.025wR(F2) = 0.067S = 1.036143 reflections307 parametersH-atom parameters constrainedmax = 0.96 e Å−3Δρmin = −0.45 e Å−3ΔρSMART  used to solve structure: SHELXS97  I, global. DOI: Click here for additional data file.10.1107/S1600536812043073/bh2457Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials:


II title compound, [Cd2(C9H10NO2)4(C6H6N2O)2(H2O)2], each seven-coordinated CdII atom is chelated by the carboxylate groups of the two 4-(dimethylamino)benzoate (DMAB) anions; the two monomeric units are bridged through the two O atoms of the two carboxyl groups. In the crystal structure, intermolecular O—H⋯O, N—H⋯O and C—H⋯O hydrogen bonds link the molecules into a three-dimensional network. π–π contacts between the pyridine rings [centroid–centroid distance = 3.974 (1) Å] may further stabilize the structure. Weak C—H⋯π interactions are also observed.In the centrosymmetric dimeric Cd DOI: 10.1107/S160053681002163X/xu2771Isup2.hkl            Structure factors: contains datablocks I. DOI:  crystallographic information; 3D view; checkCIF report            Additional supplementary materials:


The Zn—Br bond lengths range from 2.3901 (19) to 2.449 (2) Å and the Br—Zn—Br angles range from 107.09 (8) to 112.48 (8)°. In the crystal, each [ZnBr4]2− anion is connected to four cations through two N—H⋯Br and two C—H⋯Br hydrogen bonds, forming two-dimensional ⋯(cation)2⋯anion⋯(cation2)⋯ sheets parallel to the bc plane. Within each sheet, the anions are arranged in stacks with no significant inter-anion Br⋯Br interactions [the shortest being > 4.3 Å], while the cations are in chains, with weak π–π stacking interactions [centroid–centroid distance = 3.991 Å] between cations interacting with the same anion.In the title compound, (C DOI: Click here for additional data file.10.1107/S1600536812040925/pv2593Isup2.hklStructure factors: contains datablock(s) I. DOI:  crystallographic information; 3D view; checkCIF reportAdditional supplementary materials: