Showing papers in "Acta Crystallographica Section E: Crystallographic Communications in 2015"
TL;DR: High-precision structural parameters for cubic Na2MoO4 and Na2WO4 are reported based on refinement of high-resolution time-of-flight neutron powder diffraction data.
Abstract: Time-of-flight neutron powder diffraction data have been collected from Na2MoO4 and Na2WO4 to a resolution of sin (θ)/λ = 1.25 A−1, which is substantially better than the previous analyses using Mo Kα X-rays, providing roughly triple the number of measured reflections with respect to the previous studies [Okada et al. (1974). Acta Cryst. B30, 1872–1873; Bramnik & Ehrenberg (2004). Z. Anorg. Allg. Chem. 630, 1336–1341]. The unit-cell parameters are in excellent agreement with literature data [Swanson et al. (1962). NBS Monograph No. 25, sect. 1, pp. 46–47] and the structural parameters for the molybdate agree very well with those of Bramnik & Ehrenberg (2004). However, the tungstate structure refinement of Okada et al. (1974) stands apart as being conspicuously inaccurate, giving significantly longer W—O distances, 1.819 (8) A, and shorter Na—O distances, 2.378 (8) A, than are reported here or in other simple tungstates. As such, this work represents an order-of-magnitude improvement in precision for sodium molybdate and an equally substantial improvement in both accuracy and precision for sodium tungstate. Both compounds adopt the spinel structure type. The Na+ ions have site symmetry .-3m and are in octahedral coordination while the transition metal atoms have site symmetry -43m and are in tetrahedral coordination.
25 citations
TL;DR: The transition metal orthophosphates Na2 M 2Fe(PO4)3 (M = Co, Ni)3 crystallize in an alluaudite-type structure that is composed of chains built up from [M 2O10] units alternating with [FeO6] octahedra.
Abstract: The title compound, Na2Co2Fe(PO4)3, was synthesized by a solid-state reaction. This new stoichiometric phase crystallizes in an alluaudite-like structure. In this structure, all atoms are in general positions except for four atoms which are located at the special positions of the C2/c space group. One Co atom, one P and one Na atom are all located on Wyckoff position 4e (2), while the second Na atom is located on an inversion centre 4a (-1). The other Co and Fe atoms occupy a general position with a statistical distribution. The open framework results from [(Co,Fe)2O10] units of edge-sharing [(Co,Fe)O6] octahedra, which alternate with [CoO6] octahedra that form infinite chains running along the [10-1] direction. These chains are linked together through PO4 tetrahedra by the sharing of vertices so as to build layers perpendicular to [010]. The three-dimensional framework is accomplished by the stacking of these layers, leading to the formation of two types of tunnels parallel to [010] in which the Na+ cations are located, each cation being surrounded by eight O atoms.
20 citations
TL;DR: In the title compound, C15H13NOS, the thiazine ring adopts a twisted boat conformation and the dihedral angle between the aromatic rings is 86.54 (4)°.
Abstract: In the title compound, C15H13NOS, the thiazine ring adopts a twisted boat conformation and the dihedral angle between the aromatic rings is 86.54 (4)°. In the crystal, molecules are linked by weak C—H⋯O interactions, resulting in chains along [010].
20 citations
TL;DR: The transition-metal orthophosphate Na1.67Zn1.33(PO4)3 cristallizes in an alluaudite-type structure characterized by a cationic disorder in one tunnel and in the general position.
Abstract: The new title compound, disodium dizinc iron(III) tris(phosphate), Na1.67Zn1.67Fe1.33(PO4)3, which belongs to the alluaudite family, has been synthesized by solid-state reactions. In this structure, all atoms are in general positions except for four, which are located on special positions of the C2/c space group. This structure is characterized by cation substitutional disorder at two sites, one situated on the special position 4e (2) and the other on the general position 8f. The 4e site is partially occupied by Na+ [0.332 (3)], whereas the 8f site is entirely filled by a mixture of Fe and Zn. The full-occupancy sodium and zinc atoms are located at the Wyckoff positions on the inversion center 4a (-1) and on the twofold rotation axis 4e, respectively. Refinement of the occupancy ratios, bond-valence analysis and the electrical neutrality requirement of the structure lead to the given composition for the title compound. The three-dimensional framework of this structure consists of kinked chains of edge-sharing octahedra stacked parallel to [10-1]. The chains are formed by a succession of trimers based on [ZnO6] octahedra and the mixed-cation FeIII/ZnII [(Fe/Zn)O6] octahedra [FeIII:ZnIII ratio 0.668 (3)/0.332 (3)]. Continuous chains are held together by PO4 phosphate groups, forming polyhedral sheets perpendicular to [010]. The stacked sheets delimit two types of tunnels parallel to the c axis in which the sodium cations are located. Each Na+ cation is coordinated by eight O atoms. The disorder of Na in the tunnel might presage ionic mobility for this material.
19 citations
TL;DR: NaMg3(PO4)(HPO4)2 crystallizes in the alluaudite-type structure, which consists of two types of [MgO6] octahedra, one [NaO10] polyhedron, one orthophosphate and one hydrogenphosphate tetrahedron.
Abstract: The title compound, sodium trimagnesium bis(hydrogen phosphate) phosphate, was obtained under hydrothermal conditions. In the crystal, two types of [MgO6] octahedra, one with point group symmetry 2, share edges to build chains extending parallel to [10-1]. These chains are linked together by two kinds of phosphate tetrahedra, HPO4 and PO4, the latter with point group symmetry 2. The three-dimensional framework delimits two different types of channels extending along [001]. One channel hosts the Na+ cations (site symmetry 2) surrounded by eight O atoms, with Na—O bond lengths varying between 2.2974 (13) and 2.922 (2) A. The OH group of the HPO4 tetrahedron points into the other type of channel and exhibits a strong hydrogen bond to an O atom of the PO4 tetrahedron on the opposite side.
16 citations
TL;DR: In the title compound, C18H16N4O, the planes of the phenyl rings are approximately perpendicular to each other and form dihedral angles of 56.43 (8) and 24.59 (8)° with the pyrazole ring, resulting in one-dimensional chains parallel to the [010] direction.
Abstract: In the title compound, C18H16N4O, the planes of the phenyl rings are approximately perpendicular to each other [dihedral angle = 78.07 (8)°] and form dihedral angles of 56.43 (8) and 24.59 (8)° with the pyrazole ring. In the crystal, molecules are linked by N—H⋯O hydrogen bonds to form one-dimensional chains parallel to the [010] direction.
15 citations
TL;DR: The title compound, C22H20N4O3S, features two fused six-membered rings linked to a 1,2,3-triazole ring which is attached to an ethyl acetate group which has an envelope conformation with the S atom being the flap.
Abstract: The title compound, C22H20N4O3S, features two fused six-membered rings linked to a 1,2,3-triazole ring which is attached to an ethyl acetate group. The heterocycle in the benzothiazine residue has an envelope conformation with the S atom being the flap. The conformation of the ethyl acetate side chain, which is directed to the same side of the molecule as the C6 ring of the fused-ring system, may be partially established by a pair of weak intramolecular C—H⋯O(carbonyl) interactions. The three-dimensional packing is aided by intermolecular C—H⋯O and C—H⋯N interactions.
14 citations
TL;DR: The structure of β-dl-methionine, C5H11NO2S, in the space group C2/c, is here confirmed to be fully ordered all the way up to the phase transition at approximately 326 K, where displacive sliding of molecular bilayers gives the disordered P21/c α form.
Abstract: The structure of β-dl-methionine, C5H11NO2S, in the space group C2/c, is here confirmed to be fully ordered all the way up to the phase transition at approximately 326 K, where displacive sliding of molecular bilayers gives the disordered P21/c α form [data at 340 K; Gorbitz (2014). Acta Cryst. E70, 341–343]. The geometry of hydrogen bonds in LD–LD hydrogen-bonding patterns [Gorbitz et al. (2009). Acta Cryst. B65, 393–400] at the hydrophilic core of each molecular bilayer are virtually unperturbed by the phase shift, but the C—C—S—C torsion angle of the side chain changes from trans at 320 K to gauche+ for the major conformation at 340 K.
13 citations
TL;DR: The title molecular salt, obtained by the reaction of sulfamic acid with 2-amino-5-nitropyridine, is the result of a proton transfer from sulfamic Acid to the N atom of the pyridine ring.
Abstract: The title molecular salt, C5H6N3O2+ ·H2NO3S−, was obtained from the reaction of sulfamic acid with 2-amino-5-nitropyridine. A proton transfer from sulfamic acid to the pyridine N atom occurred, resulting in the formation of a salt. As expected, this protonation leads to the widening of the C—N—C angle of the pyridine ring, to 122.9 (3)°, with the pyridinium ring being essentially planar (r.m.s. deviation = 0.025 A). In the crystal, the ion pairs are joined by three N—H⋯O and one N—H⋯N hydrogen bonds in which the pyridinium N atom and the amino N atom act as donors, and are hydrogen bonded to the carboxylate O atoms and the N atom of the sulfamate anion, thus generating an R33(22) ring motif. These motifs are linked by further N—H⋯O hydrogen bonds enclosing R33(8) loops, forming sheets parallel to (100). The sheets are linked via weak C—H⋯O hydrogen bonds, forming a three-dimensional structure. The O atoms of the nitro group are disordered over two sets of sites with a refined occupancy ratio of 0.737 (19):0.263 (19).
12 citations
TL;DR: The title compound is an example of a 12-metallacrown-4 self-assembled supramolecular coordination complex with ring MnIII ions that is tethered to the metallac Crown with four trimethylacetate anions.
Abstract: The synthesis and crystal structure for the title compound, [YNaMn4(C7H4NO3)4(C5H9O2)4(H2O)3.76(C3H7NO)0.24]·8.04C3H7NO·0.62H2O or [YIIINa(OTMA)4[12-MCMn(III)N(shi)-4](H2O)3.76(DMF)0.24·8.04DMF·0.62H2O, where OTMA is trimethylacetate, MC is metallacrown, shi3− is salicylhydroximate, and DMF is N,N-dimethylformamide, is reported. The macrocyclic metallacrown consists of an –[MnIII–N–O]4– ring repeat unit, and the metallacrown captures one YIII ion and one NaI ion in the central cavity on opposite faces of the metallacrown. Overall the metallacrown is domed towards the side of the NaI ion. Both the YIII and NaI ions are eight-coordinate, and the trimethylacetate anions bridge the central YIII to each ring MnIII ion. The ring MnIII ions are six-coordinate with a tetragonally distorted octahedral geometry.
12 citations
TL;DR: The high-pressure phase of SrGeO3 synthesized at 6 GPa and 1223 K adopts the ideal cubic perovskite-type structure because the Ge—O bond is largely covalent, which influences the thermal vibration behavior of the O atom.
Abstract: Single crystals of the SrGeO3 (strontium germanium trioxide) high-pressure phase have been synthesized successfully at 6 GPa and 1223 K. The compound crystallizes with the ideal cubic perovskite-type structure (space group Pm-3m), which consists of a network of corner-linked regular GeO6 octahedra (point-group symmetry m-3m), with the larger Sr atoms located at the centers of cavities in the form of SrO12 cuboctahedra (point-group symmetry m-3m) in the network. The degrees of covalencies included in the Sr—O and the Ge—O bonds calculated from bond valences are 20.4 and 48.9%, respectively. Thus, the Ge—O bond of the GeO6 octahedron in the SrGeO3 perovskite has a strong covalency, comparable to those of the Si—O bonds of the SiO4 tetrahedra in silicates with about 50% covalency. The thermal vibrations of the O atoms in the title compound are remarkably suppressed in the directions of the Ge—O bonds. This anisotropy ranks among the largest observed in stoichiometric cubic perovskites.
TL;DR: The whole molecule of the title complex, [Hg2Cl4(C18H15N3)2], is generated by inversion symmetry, and the five-coordinated Hg2+ ions have a distorted square-pyramidal environment defined by two N atoms.
Abstract: The whole molecule of the title complex, [Hg2Cl4(C18H15N3)2], is generated by inversion symmetry. It was synthesized from the pyridine-derived Schiff base N-phenyl-N′-[(pyridin-2-yl)methylidene]benzene-1,4-diamine (PPMBD). The five-coordinated Hg2+ ions have a distorted square-pyramidal environment defined by two N atoms, viz. the imine and the other pyridyl [Hg—N = 2.467 (6) and 2.310 (6) A, respectively] belonging to the bidentate iminopyridine ligand, and three Cl atoms [Hg—Cl = 2.407 (2), 2.447 (2) and 3.031 (2) A]. The longest Hg—Cl bond is bridging about the inversion centre. In the ligand, the central ring and pyridine ring are oriented at a dihedral angle of 8.1 (4)°, while the planes of the pyridine ring and the terminal phenyl ring are oriented at a dihedral angle of 53.8 (4)°. In the crystal, molecules are linked by N—H⋯Cl and C—H⋯Cl hydrogen bonds, forming sheets parallel to (001).
TL;DR: In the title adduct, C5H5N·I2, the N—I distance [2.424 (8) Å] is remarkably shorter than the sum of the van der Waals radii.
Abstract: In the title adduct, C5H5N·I2, the N—I distance [2.424 (8) A] is remarkably shorter than the sum of the van der Waals radii. The line through the I atoms forms an angle of 78.39 (16)° with the normal to the pyridine ring.
TL;DR: In the new molybdenum oxide potassium pentasodium trimanganese hexakis(molybdate), KNa5Mn3Mo6O24, the structure is composed of M 2O10 (M = Mn, Na) dimers and MoO4 tetrahedra sharing corners and forming layers which are linked via common corners of another type of MO4 tetRAhedra, forming a three-dimensional structure.
Abstract: The new phase potassium pentasodium trimanganese hexakis(molybdate), KNa5Mn3Mo6O24, has been synthesized using solid-state methods The structure is composed of M2O10 (M = Mn, Na) dimers and MoO4 tetrahedra (point group symmetry 2) sharing corners and forming layers parallel to (100), which are linked via common corners of another type of MO4 tetrahedra, forming a three-dimensional structure with two types of large channels along [001] in which two types of Na+ cations (one with site symmetry 2, one with -1) and K+ cations (site symmetry 2, half-occupation) are located Mn2+ and the third type of Na+ cations are located at the same site M with occupancies of 075 and 025, respectively A comparative structural description is provided between the structure of the title compound and those of the related phases Cu135Fe3(PO4)3 and NaAgFeMn2(PO4)3
TL;DR: The title compound, (C5H7N2)2[Cu(H2O)6](SO4)2·4 H2O], comprises axially elongated hexaaqua-coordinated octahedral CuII ions located on an inversion centre, non-coordinating sulfate anions, 2-aminopyridinium cations and lattice water molecules.
Abstract: The title compound, (C5H7N2)2[Cu(H2O)6](SO4)2·4H2O [systematic name: bis(2-aminopyridinium) hexaaquacopper(II) bis(sulfate) tetrahydrate], comprises axially elongated hexaaqua-coordinated octahedral CuII ions located on an inversion centre, non-coordinating sulfate anions, 2-aminopyridinium cations and lattice water molecules. The crystal structure is built of successive inorganic and organic layers extending parallel to (001) that are connected by an extensive three-dimensional hydrogen-bonded network of the type O—H⋯O and N—H⋯O, as well as π–π interactions [centroid–centroid distance 3.4140 (14) A, offset 0.277 A].
TL;DR: The title compound is isotypic with the corresponding chloride salt and consists of discrete [Cr(urea)6]3+ cations, staggered Cr2O7 4− and Br− anions and water solvent molecules that are held together by an intricate three-dimensional network of hydrogen-bonding interactions.
Abstract: The title bromide salt, [Cr{CO(NH2)2}6](Cr2O7)Br·H2O, is isotypic to the corresponding chloride salt. Within the complex cation, the CrIII atom is coordinated by six O atoms of six urea ligands, displaying a slightly distorted octahedral coordination environment. The Cr—O bond lengths involving the urea ligands are in the range 1.9534 (13)–1.9776 (12) A. The Cr2O72− anion has a nearly staggered conformation, with a bridging angle of 130.26 (10)°. The individual components are arranged in rows extending parallel to [100]. The Br− anion links the complex cation, as well as the solvent water molecule, through N—H⋯Br and O—H⋯Br hydrogen-bonding interactions. The supramolecular architecture also includes N—H⋯O and O—H⋯O hydrogen bonding between urea N—H and water O—H donor groups and the O atoms of the Cr2O72− anion as acceptor atoms, leading to a three-dimensional network structure.
TL;DR: The transition metal orthophosphates SrM 2Fe(PO4)3 (M = Co, Ni) crystallize in an α-CrPO4-type structure, nearly the same as that observed in MMnII 2MnIII(PO 4)3(M = Pb, Sr, Ba).
Abstract: The title compound, SrNi2Fe(PO4)3, synthesized by solid-state reaction, crystallizes in an ordered variant of the α-CrPO4 structure. In the asymmetric unit, two O atoms are in general positions, whereas all others atoms are in special positions of the space group Imma: the Sr cation and one P atom occupy the Wyckoff position 4e (mm2), Fe is on 4b (2/m), Ni and the other P atom are on 8g (2), one O atom is on 8h (m) and the other on 8i (m). The three-dimensional framework of the crystal structure is built up by [PO4] tetrahedra, [FeO6] octahedra and [Ni2O10] dimers of edge-sharing octahedra, linked through common corners or edges. This structure comprises two types of layers stacked alternately along the [100] direction. The first layer is formed by edge-sharing octahedra ([Ni2O10] dimer) linked to [PO4] tetrahedra via common edges while the second layer is built up from a strontium row followed by infinite chains of alternating [PO4] tetrahedra and FeO6 octahedra sharing apices. The layers are held together through vertices of [PO4] tetrahedra and [FeO6] octahedra, leading to the appearance of two types of tunnels parallel to the a- and b-axis directions in which the Sr cations are located. Each Sr cation is surrounded by eight O atoms.
TL;DR: In Na9Cr(MoO4)6 the basic structure units are isolated polyhedral clusters composed of a central CrO6 octahedron sharing vertices with six MoO4 to form an open (0D) framework in which the Na+ cations are oriented at the free vertices of the MoO 4 tetrahedra.
Abstract: The title compound, nonasodium chromium(III) hexakis[molybdate(VI)], Na9Cr(MoO4)6 was prepared by solid-state reactions. The basic structure units are isolated polyhedral clusters composed of a central CrO6 octahedron sharing vertices with six MoO4 tetrahedra to form an open framework in which the Na+ cations are bound to the free vertices of the MoO4 tetrahedra. The Cr3+ cation has site symmetry of 32 (6a), one Na atom sits on a twofold axis (18e), and all other atoms are at general positions. The bond-valance-sum model confirms the expected values of ion charges. The title compound is isotypic with Na9Sc(MoO4)6 and Na9Fe(MoO4)6. It is compared and discussed with similar structures.
TL;DR: The asymmetric unit of the title compound, C22H21N3O2, consists of two independent molecules (A and B) having differing conformations, which mainly concern the dihedral angles which the hydroxyphenyl and dimethylphenyl rings subtend to the central phenylene ring.
Abstract: The asymmetric unit of the title compound, C22H21N3O2, consists of two independent molecules (A and B) having differing conformations. The differences mainly concern the dihedral angles which the hydroxyphenyl and dimethylphenyl rings subtend to the central phenylene ring, these being 30.16 (6) and 58.60 (6)° in molecule A and 13.42 (7) and 60.31 (7)° in B. With the exception of the dimethyphenyl substituent, the conformations of the rest of each molecule are largely determined by intramolecular O—H⋯N and N—H⋯O hydrogen bonds. In the crystal, N—H⋯O hydrogen bonds link the molecules into chains extending parallel to the a axis in which the types of molecules alternate in an …A…B…A…B… fashion.
TL;DR: The title compounds, (I) and (II), are hydrazinecarbothioamide derivatives, and in the crystal of (I), molecules are linked by pairs of N—H⋯S hydrogen bonds, forming inversion dimers with an (8) ring motif.
Abstract: The title compounds, C13H13N3O2S·05H2O, (I), and C17H14ClN3OS, (II), are hydrazinecarbothioamide derivatives Compound (I) crystallizes with two independent molecules (A and B) and a water molecule of crystallization in the asymmetric unit The chromene moiety is essentially planar in molecules A and B, with maximum deviations of 0028 (3) and 0016 (3) A, respectively, for the carbonyl C atoms In (II), the pyran ring of the chromene moiety adopts a screw-boat conformation and the phenyl ring is inclined by 6118 (9)° to its mean plane In the crystal of (I), bifurcated N—H⋯O and C—H⋯O hydrogen bonds link the two independent molecules forming A–B dimers with two R21(6) ring motifs, and R22(10) and R22(14) ring motifs In addition to these, the water molecule forms tetrafurcated hydrogen bonds which alternately generate R44(12) and R66(22) graph-set ring motifs There are also π–π [inter-centroid distances = 35648 (14) and 36825 (15) A] interactions present, leading to the formation of columns along the c-axis direction In the crystal of (II), molecules are linked by pairs of N—H⋯S hydrogen bonds, forming inversion dimers with an R22(8) ring motif The dimers are linked by C—H⋯π interactions, forming ribbons lying parallel to (210)
TL;DR: In each of the title compounds, the anion shows evidence of extensive electronic delocalization.
Abstract: In 2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-ethoxyprop-2-en-1-ide, C10H9N2+·C9H5N4O−, (I), the ethyl group in the anion is disordered over two sets of atomic sites with occupancies 0.634 (9) and 0.366 (9), and the dihedral angle between the ring planes in the cation is 2.11 (7)°. The two independent C(CN)2 groups in the anion make dihedral angles of 10.60 (6) and 12.44 (4)° with the central propenide unit, and the bond distances in the anion provide evidence for extensive electronic delocalization. In bis(2,2′-bipyridin-1-ium) 1,1,3,3-tetracyano-2-(dicyanomethylene)propane-1,3-diide [alternative name bis(2,2′-bipyridin-1-ium) tris(dicyanomethylene)methanediide], 2C10H9N2+·C10N62− (II), the dihedral angles between the ring planes in the two independent cations are 7.7 (2) and 10.92 (17)°. The anion exhibits approximate C3 symmetry, consistent with extensive electronic delocalization, and the three independent C(CN)2 groups make dihedral angles of 23.8 (2), 27.0 (3) and 27.4 (2)° with the central plane. The ions in (I) are linked by an N—H⋯N hydrogen bond and the resulting ion pairs are linked by two independent C—H⋯N hydrogen bonds, forming a ribbon containing alternating R44(18) and R44(26) rings, where both ring types are centrosymmetric. The ions in (II) are linked by two independent N—H⋯N hydrogen bonds and the resulting ion triplets are linked by a C—H⋯N hydrogen bond, forming a C21(7) chain containing anions and only one type of cation, with the other cation linked to the chain by a further C—H⋯N hydrogen bond.
TL;DR: A new triple molybdate K0.4Na3.6Co(MoO4)3 was synthesized using solid-state reaction at 973 K and characterized by X-ray diffraction, characterized by M 2O10 (M = Co/Na) dimers, which are linked by MoO4 tetrahedra, forming infinite layers.
Abstract: A new triple molybdate, potassium sodium cobalt tris(molybdate), K0.4Na3.6Co(MoO4)3, was synthesized using solid-state reactions. The Co2+ and one Na+ cation are located at the same general site, each with occupancy 0.5. Another site (site symmetry 2) is occupied by Na+ and K+ cations, with occupancies of 0.597 (7) and 0.402 (6), respectively. The other two Na+ cations and one of the two Mo atoms lie on special positions (site symmetries -1, 2 and 2, respectively). The structure is characterized by M2O10 (M = Co/Na) dimers, which are linked by MoO4 tetrahedra, forming infinite layers. The latter are connected firstly by insertion of one type of MoO4 tetrahedra and secondly by sharing corners with the other type of MoO4 tetrahedra. This results in an open three-dimensional framework with the cavities occupied by the Na+ and K+ cations. The structure is isotypic with Na3In2As3O12 and Na3In2P3O12. A comparison is made with structures such as K2Co2(MoO4)3 and β-NaFe2(MoO4)3 and their differences are discussed.
TL;DR: In the title compound, C25H20N2O2S, the dihydroisoxazole ring exhibits an envelope conformation with the methine atom being the flap, while the 1,4-thiazine ring displays a screw-boat conformation.
Abstract: In the title compound, C25H20N2O2S, the dihydroisoxazole ring exhibits an envelope conformation with the methine atom being the flap, while the 1,4-thiazine ring displays a screw-boat conformation. The six-membered ring fused to the 1,4-thiazine ring makes dihedral angles of 63.04 (2) and 54.7 (2)° with the mean planes through the five-membered heterocycle and the attached phenyl ring, respectively. The phenyl group connected to the 1,4-thiazine ring is disordered over two sites [major component = 0.57 (2)]. The most prominent interactions in the crystal structure are C—H⋯O hydrogen bonds that link molecules, forming inversion dimers, and C—H⋯N hydrogen bonds that link the dimers into columns parallel to the b axis.
TL;DR: In the title copper(II) complex containing chloride and a derivative of 3-methyl-1-phenyl-4-hydrazopyrazolin-5-one, acting as a tridentate ligand, the CuII atom is in a slightly distorted square-planar coordination.
Abstract: In the title compound, [Cu(C21H19N6O2)Cl], the CuII atom is in a slightly distorted square-planar coordination involving two O atoms from the pyrazolone rings [Cu—O = 2.088 (10) and 1.975 (10) A], an N atom of the azo group [Cu—N = 2.048 (13) A] and a chloride anion [Cu—Cl = 2.183 (5) A]. The organic anions act as tridentate chelating ligands. The molecules stack in columns along the c axis.
TL;DR: The title compound, C15H17NO2, was synthesized from a mixture of α-himachalene (2-methylene-6,6,9-trimethylbicyclo[5.4.01,7]undeca-1,8-diene), which were isolated from an oil of the Atlas cedar (Cedrus Atlantica).
Abstract: The title compound, C15H17NO2, was synthesized from a mixture of α-himachalene (2-methylene-6,6,9-trimethylbicyclo[5.4.01,7]undec-8-ene) and β-himachalene (2,6,6,9-tetramethylbicyclo[5.4.01,7]undeca-1,8-diene), which were isolated from an oil of the Atlas cedar (Cedrus Atlantica). The naphthalene ring system makes dihedral angles of 68.6 (2) and 44.3 (2)°, respectively, with its attached isopropyl C/C/C plane and the nitro group. In the crystal, molecules held together by a C—H⋯O interaction, forming a chain along [-101].
TL;DR: In four N-(4-halophenyl)-4-oxo-4H-chromene-3-carboxamides, halo = -F, -Cl, -Br and -I, the molecules are essentially planar and exhibit anti conformations with respect to the C—N rotamer of the amide.
Abstract: Four N-(4-halophenyl)-4-oxo-4H-chromene-3-carboxamides (halo = F, Cl, Br and I), N-(4-fluorophenyl)-4-oxo-4H-chromene-3-carboxamide, C16H10FNO3, N-(4-chlorophenyl)-4-oxo-4H-chromene-3-carboxamide, C16H10ClNO3, N-(4-bromophenyl)-4-oxo-4H-chromene-3-carboxamide, C16H10BrNO3, N-(4-iodophenyl)-4-oxo-4H-chromene-3-carboxamide, C16H10INO3, have been structurally characterized. The molecules are essentially planar and each exhibits an anti conformation with respect to the C—N rotamer of the amide and a cis geometry with respect to the relative positions of the Carom—Carom bond of the chromone ring and the carbonyl group of the amide. The structures each exhibit an intramolecular hydrogen-bonding network comprising an N—H⋯O hydrogen bond between the amide N atom and the O atom of the carbonyl group of the pyrone ring, forming an S(6) ring, and a weak Carom—H⋯O interaction with the O atom of the carbonyl group of the amide as acceptor, which forms another S(6) ring. All four compounds have the same supramolecular structure, consisting of R22(13) rings that are propagated along the a-axis direction by unit translation. There is π–π stacking involving inversion-related molecules in each structure.
TL;DR: The complex cation of the title compound includes one CoII atom with a distorted octahedral coordination environment defined by six N atoms from three bidentate phenanthroline ligands, and observed non-covalent interactions contribute to the consolidation of the supramolecular network.
Abstract: The complex cation of the title compound, [Co(C12H8N2)3]2(NO3)4·C12H12N2O6·8H2O, contains a CoII atom with a distorted octahedral coordination environment defined by six N atoms from three bidentate 1,10-phenanthroline ligands. The asymmetric unit of the title compound is completed by one-half of the N,N′-(1,4-phenylenedicarbonyl)diglycine solvent molecule, which is located on a centre of inversion, by two nitrate counter-anions and four solvent water molecules. Two [Co(C12H8N2)3]2+ cations are connected through C—H⋯O contacts and through lone-pair⋯π interactions involving the non-coordinating N,N′-(1,4-phenylenedicarbonyl)diglycine and phenanthroline molecules. The different aromatic ring systems are involved in π–π stacking and C—H⋯π interactions, with centroid-to-centroid distances in the range 3.7094 (8)–3.9973 (9) A. The crystal structure is stabilized by further anion⋯π interactions and C—H⋯O contacts, as well as O—H⋯O and N—H⋯O hydrogen bonds between water molecules, the non-coordinating nitrate anions, N,N′-(1,4-phenylenedicarbonyl)diglycine and phenanthroline molecules. These non-covalent interactions give rise to a three-dimensional supramolecular network.
TL;DR: The crystal structure of the title compound displays boat and half-chair configurations of the thiazine ring.
Abstract: The asymmetric unit of the title compound, C18H18N2O2S.0.375H2O, has two independent organic molecules (A and B) and 3/4 of a water molecule distributed over three sites. In molecule A, the 1,3-thiazine ring is in a boat conformation, with the C atoms at the 2- and 5-positions out of the plane. The angle between the two phenyl rings is 51.70 (12)°. In molecule B, the thiazine ring is in a half-chair conformation, with the S atom forming the back of the half-chair. The angle between the two phenyl rings is 84.44 (14)°. The A molecule features an intramolecular N—H⋯O hydrogen bond, which closes an S(5) ring motif. In the crystal, the corresponding N—H grouping of the B molecule participates in an intermolecular hydrogen bond to the A molecule. The A molecule participates in a C—H⋯O interaction back to the B molecule, whilst the B molecule features an intramolecular C—H⋯O link, which generates an S(10) loop.
TL;DR: The reaction of terbium(III) nitrate pentahydrate in acetonitrile with N,N′-bis(2-hydroxybenzyl)-N,N −bis(pyridin-2-ylmethyl)ethylenediamine (H2bbpen) produced the mononuclear compound [Tb(Cbbpen)(NO3].
Abstract: The reaction of terbium(III) nitrate pentahydrate in acetonitrile with N,N′-bis(2-hydroxybenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (H2bbpen), previously deprotonated with triethylamine, produced the mononuclear compound [N,N′-bis(2-oxidobenzyl-κO)-N,N′-bis(pyridin-2-ylmethyl-κN)ethylenediamine-κ2N,N′](nitrato-κ2O,O′)terbium(III), [Tb(C28H28N4O2)(NO3)]. The molecule lies on a twofold rotation axis and the TbIII ion is eight-coordinate with a slightly distorted dodecahedral coordination geometry. In the symmetry-unique part of the molecule, the pyridine and benzene rings are both essentially planar and form a dihedral angle of 61.42 (7)°. In the molecular structure, the N4O4 coordination environment is defined by the hexadentate bbpen ligand and the bidentate nitrate anion. In the crystal, a weak C—H⋯O hydrogen bond links molecules into a two-dimensional network parallel to (001).
TL;DR: In the first reported crystal structure of the family of lithium phosphate diesters, the Li atom is in a slightly distorted tetrahedral coordination environment and exhibits one intramolecular O—H⋯O hydrogen bond between a coordinating methanol molecule and the terminal non-coordinating O atom of the phosphate group.
Abstract: Crystals of the title compound, [Li{OOP(O-2,6-iPr2C6H3)2}(CH3OH)3]·CH3OH or [Li(C24H34O4P)(CH3OH)3]·CH3OH, have been formed in the reaction between HOOP(O-2,6-iPr2C6H3)2 and LiOH in methanol. The title compound is of interest as it represents the first reported crystal structure of the family of lithium phosphate diesters. The {Li(CH3OH)3[O2P(O-iPr2C6H3)2]} unit displays the Li atom in a slightly distorted tetrahedral coordination environment and exhibits one intramolecular O—H⋯O hydrogen bond between a coordinating methanol molecule and the terminal non-coordinating O atom of the phosphate group. The unit is connected with two non-coordinating methanol molecules through two intermolecular O—H⋯O hydrogen bonds, and with a neighbouring unit through two other O—H⋯O interactions. These intermolecular hydrogen bonds lead to the formation of infinite chains along [100]. There are no significant interactions between the chains.