Related Articles
Single crystals of yttrium pentaphosphate(V), YP5O14, were obtained by solid-state reaction. The orthorhombic title compound belongs to the family of ultraphosphates and is the second polymorph of this composition. It is isotypic with its Ho and Er analogues. The structure contains two bridging Q
2-type PO4 tetrahedra and one branching Q
3-type PO4 tetrahedron, leading to infinite ultraphosphate ribbons running along the a axis. The coordination polyhedron around the Y3+ cation may be described as distorted bicapped trigonal-prismatic. The YO8 polyhedra are isolated from each other. They are linked by corner-sharing to the O atoms of six Q
2-type and of two Q
3-type PO4 tetrahedra into a three-dimensional framework.
doi:10.1107/S1600536809007193
PMCID: PMC2968816
PMID: 21582306
Crystals of the orthorhombic phase La4Mo7O27 (lanthanum molybdenum oxide) were obtained from a non-stoichiometric melt in the pseudo-ternary system La2O3–MoO3–B2O3. In the crystal structure, distorted square-antiprismatic [LaO8] and monocapped square-antiprismatic [LaO9] polyhedra are connected via common edges and faces into chains along [010]. These chains are arranged in layers that alternate with layers of [MoO4] and [MoO5] polyhedra parallel to (001). In the molybdate layers, a distorted [MoO5] trigonal bipyramid is axially connected to two [MoO4] tetrahedra, forming a [Mo3O11] unit.
doi:10.1107/S1600536809026415
PMCID: PMC2977117
PMID: 21583295
Cerium(III) ultraphosphate, CeP5O14, was synthesized by a high-temperature solution reaction between CeO2 and NH4H2PO4 in a Ce–P molar ratio of 1:12. Colourless crystals of the orthorhombic polymorph were obtained by cooling the melt of the mixture. The structure contains (P5O14)3− anionic ribbons linked by distorted CeO8 polyhedra.
doi:10.1107/S1600536808032972
PMCID: PMC2959646
PMID: 21580810
During an attempt to prepare a cocrystal of N-phenylphthalimide, C14H9NO2, with N-(2,3,4,5,6-pentafluorophenyl)phthalimide, a new orthorhombic polymorph of the first component was obtained. This new form has Z′ = 0.5 and the molecule is located around a twofold axis, whereas in the previously reported polymorph (space group Pbca), the molecule has no crystallographically imposed symmetry. Pairs of C—H⋯O interactions between inversion-related phthalimide units arrange molecules into tapes that are further assembled into (010) layers via stacking interactions between phthalimide fragments [interplanar distance = 3.37 (5) Å].
doi:10.1107/S1600536809006746
PMCID: PMC2968531
PMID: 21582305
Crystals of di-μ-bromido-bis[tetrabromidotantalum(V)], (TaBr5)2, were obtained by recrystallization at 773 K. A first crystal structure study of (TaBr5)2 was reported by Rolsten [J. Am. Chem. Soc. (1958) ▶, 80, 2952–2953], who analysed the powder diffraction pattern and came to the conclusion that it crystallizes isotypically with (NbBr5)2 in a primitive orthorhombic cell. These findings are not in agreement with our current results of a monoclinic C-centred structure. (TaBr5)2 is isotypic with α-(NbCl5)2. The crystal structure contains [TaBr6] octahedra sharing common edges forming [TaBr5]2 dimers. Two crystallographically independent dimers with symmetries m and 2/m and Ta⋯Ta distances of 4.1574 (11) and 4.1551 (15) Å, respectively, are present in the structure.
doi:10.1107/S1600536810032538
PMCID: PMC3007875
PMID: 21588474
The title compound, C10H24N+·C8H15O2
−, forms a layered structure in which intermolecular N+—H⋯O hydrogen bonds connect anions and cations, forming a two-dimensional network parallel to (010). The n-alkyl chains of the decylammonium cations pack according to an orthorhombic ‘subcell’ with approximate dimensions 5.1 × 7.3 Å, and they are significantly distorted from planarity.
doi:10.1107/S1600536811005125
PMCID: PMC3052094
PMID: 21522407
A new polymorph of the title compound, C8H8BrNO, has been determined at 173 K in the space group P21/c. The previous room-temperature structure was reported to crystallize in the orthorhombic space group Pna21 [Andreetti et al. (1968 ▶). Acta Cryst. B24, 1195–1198]. In the crystal, molecules are linked by N—H⋯O hydrogen bonds forming chains along [010]. Weak C—H⋯π interactions are also present.
doi:10.1107/S1600536813005448
PMCID: PMC3588444
PMID: 23476627
Single crystals of europium(III) scandate(III), with ideal formula EuScO3, were grown from the melt using the micro-pulling-down method. The title compound crystallizes in an orthorhombic distorted perovskite-type structure, where Eu occupies the eightfold coordinated A sites (site symmetry m) and Sc resides on the centres of corner-sharing [ScO6] octahedra (B sites with site symmetry ). The structure of EuScO3 has been reported previously based on powder diffraction data [Liferovich & Mitchell (2004). J. Solid State Chem.
177, 2188–2197]. The results of the current redetermination based on single-crystal diffraction data shows an improvement in the precision of the structral and geometric parameters and reveals a defect-type structure. Site-occupancy refinements indicate an Eu deficiency on the A site coupled with O defects on one of the two O-atom positions. The crystallochemical formula of the investigated sample may thus be written as A(□0.032Eu0.968)BScO2.952.
doi:10.1107/S1600536809001433
PMCID: PMC2968298
PMID: 21581742
The title compound, Yb2LiInGe2, a new ordered quaternary intermetallic phase, crystallizes with the orthorhombic Ca2LiInGe2 type (Pearson code oP24). The crystal structure contains six crystallographically unique sites in the asymmetric unit, all in special positions with site symmetry .m.. The structure is complex and based on [InGe4] tetrahedra, which share corners in two directions, forming layers parallel to (001). Yb atoms fill square-pyramidal (Yb1) and octahedral (Yb2) interstices between the [InGe4/2] layers, while the small Li+ atoms fill tetrahedral sites.
doi:10.1107/S1600536810014595
PMCID: PMC2979241
PMID: 21578989
Barium dierbium(III) tetrasulfide, BaEr2S4, crystallizes with four formula units in the orthorhombic space group Pnma in the CaFe2O4 structure type. The asymmetric unit contains two Er, one Ba, and four S atoms, each with .m. site symmetry. The structure consists of channels formed by corner- and edge-sharing ErS6 octahedra in which Ba atoms reside. The resultant coordination of Ba is that of a bicapped trigonal prism.
doi:10.1107/S1600536813003541
PMCID: PMC3588518
PMID: 23476480
A new orthorhombic polymorph of terephthalaldehyde, C8H6O2, with a melting point of 372 K, has been obtained by recrystallization from ethanol. At room temperature, the crystals transform into the well known monoclinic form, with a melting point of 389 K. The crystal structure of the monoclinic form involves C—H⋯O hydrogen bonds, but no such bonds are observed in the orthorhombic form. The molecule is planar.
doi:10.1107/S1600536808022381
PMCID: PMC2962184
PMID: 21203265
A new monoclinic polymorphic form of the title compound, [Cu(HCO2)2(C14H12N2)(H2O)], is described. It differs from the first orthorhombic polymorph [Pan, Lin & Zheng (2005 ▶). Z. Kristallogr. New Cryst. Struct.
220, 495–496] in the deviation of the Cu atom relative to the plane of the 2,9-dimethyl-1,10-phenanthroline (dmp) ligand. In the present structure, the Cu atom is shifted from the mean plane of the dmp ligand by only 0.005 (1) Å, compared with 0.318 (6) Å in the orthorhombic form. Hydrogen-bonding and π–π stacking interactions (mean interplanar distance of 3.59 Å in the title compound) in the two different polymorphs are both essential to the supramolecular assembly.
doi:10.1107/S1600536808022812
PMCID: PMC2961975
PMID: 21203045
A new polymorph of N,N′-bis(2,6-diisopropylphenyl)formamidine, C25H36N2, is reported, which is different from the previously reported orthorhombic structure. The molecule crystallizes in the E–anti configuration, with tautomeric disorder of the N-bonded H atoms and no clear distinction between imine and amine functionalities. The molecules form hydrogen-bonded dimers with intermolecular N⋯N distances shorter than those in the orthorhombic polymorph.
doi:10.1107/S160053680802076X
PMCID: PMC2962078
PMID: 21203162
The title compound, C14H12N2O2, is an orthorhombic polymorph of the previously reported monoclinic form [Bakir et al. (2005 ▶). Acta Cryst. E61, o1611–o1613]. The dihedral angle between the aromatic rings is 4.32 (13)°. The molecular structures of the two polymorphs, including short intramolecular O—H⋯O hydrogen bonds between the the hydroxy and keto groups, are quite similar but their crystal packings are distinct. Unlike the monoclinic form, in which centrosymmetrically related hydroxy and keto groups form {⋯H⋯O}2 synthons via weak O—H⋯O contacts, leading to dimeric aggregates, in the orthorhombic form, the hydrogen bonding between these groups leads to the formation of supramolecular chains orientated along the a axis.
doi:10.1107/S1600536809046868
PMCID: PMC2971774
PMID: 21578791
The asymmetric unit in the title compound, C5H5NO, comprises two independent but virtually identical molecules of 2-pyridone, and represents a monoclinic polymorph of the previously reported orthorhombic (P212121) form [Penfold (1953 ▶). Acta Cryst.
6, 591–600; Ohms et al. (1984 ▶). Z. Kristallogr.
169, 185–200; Yang & Craven (1998 ▶). Acta Cryst. B54, 912–920]. The independent molecules are linked into supramolecular dimers via eight-membered {⋯HNC(O)}2 amide synthons in contrast to the helical supramolecular chains, mediated by {⋯HNC(O)} links, found in the orthorhombic form.
doi:10.1107/S1600536809049496
PMCID: PMC2972078
PMID: 21578899
The title heteroaryl chalcone, C21H14OS, is a second orthorhombic polymorph which crystallizes in the space group P212121. The structure was previously reported [Fun et al. (2009 ▶). Acta Cryst. E65, o2168-o2169] in the space group Pna21. The bond distances and angles are similar in both structures. In contrast, the overall crystal packing is different from that in the first orthorhombic Pna21 polymorph in which molecules were stacked into columns along the b axis and the thiophene units of two adjacent columns were stacked in a head to tail fashion. In the present polymorph, molecules are found to dimerize through a weak S⋯S interaction [3.6513 (7) Å] and these dimers are arranged into sheets parallel to the bc plane. There are no classical hydrogen bonds in the packing which features short C⋯O [3.2832 (2)–3.6251 (9) Å], C⋯S [3.4879 (17)–3.6251 (19) Å] and S⋯O [2.9948 (16) Å] contacts, together with C—H⋯π interactions. Similar contacts were found in the other polymorph.
doi:10.1107/S1600536810000061
PMCID: PMC2979950
PMID: 21579743
The title compound, C13H10Cl2N2S, represents a monoclinic polymorph of the previously reported orthorhombic form [Ramnathan et al. (1996 ▶). Acta Cryst. C52, 134–136]. The molecule is twisted with the dihedral angle between the benzene rings being 55.37 (7)°. The N—H atoms are syn to each other, which contrasts their anti disposition in the orthorhombic form. In the crystal, molecules assemble into zigzag chains along the c axis via N—H⋯S hydrogen bonds. Chains are connected into layers via C—H⋯Cl interactions, and these stack along the a axis.
doi:10.1107/S1600536811041894
PMCID: PMC3247371
PMID: 22219989
The crystal structure of the title compound, C12H11NO2, represents a new orthorhombic polymorph II of the previously reported orthorhombic form I [Zhang et al. (2009 ▶) Acta Cryst. E65, o3160]. In polymorph II, the six-membered rings form a dihedral angle of 13.8 (1)° [71.6 (1)° in I], and O—H⋯N hydrogen bonds link molecules into chains along [100], whereas the crystal structure of I features hydrogen-bonded centrosymmetric dimers.
doi:10.1107/S1600536812014067
PMCID: PMC3344498
PMID: 22590260
In the solid-state synthesis of impurity-doped CaGa2S4, calcium tetrathiodigallate(III), a novel phosphor material (denominated as the X-phase), with monoclinic symmetry in the space group P21/a, has been discovered. Its emission intensity is higher than that of the known orthorhombic polymorph of CaGa2S4 crystallizing in the space group Fddd. The asymmetric unit of the monoclinic phase consists of two Ca, four Ga and eight S sites. Each of the Ca and Ga atoms is surrounded by seven and four sulfide ions, respectively, thereby sharing each of the sulfur sites with the nearest neighbours. In contrast, the corresponding sites in the orthorhombic phase are surrounded by eight and four S atoms, respectively. The photoluminescence peaks from Mn2+ and Ce3+ in the doped X-phase, both of which are supposed to replace Ca2+ ions, have been observed to shift towards the high energy side in comparison with those in the orthorhombic phase. This suggests that the crystal field around the Mn2+ and Ce3+ ions in the X-phase is weaker than that in the orthorhombic phase.
doi:10.1107/S1600536812019113
PMCID: PMC3379052
PMID: 22719273
Crystals of manganese(II) dibarium bis(hydrogenphosphate) bis(dihydrogenphosphate), MnBa2(HPO4)2(H2PO4)2, were obtained by hydrothermal synthesis. The title compound is isotypic with its CdII and CaII analogues. The structure is built up of an infinite {[Mn(HPO4)2(H2PO4)2]4−}n chain running along [100], which consists of alternate MnO6 octahedra and [PO4] tetrahedra, in which the centrosymmetric MnO6 octahedra share their four equatorial O-atom corners with tetrahedral [PO3(OH)] groups and their two axial apices with tetrahedral [PO2(OH)2] groups. These chains are held together by BaO9 coordination polyhedra, developing into a three-dimensional structure. The O—H⋯O hydrogen bonds additionally stabilize the structural set-up. Due to the ionic radius of Mn2+ being much smaller than those of Ca2+ and Cd2+, this may imply that their adopted structure type has a great tolerance for incorporating various ions and the exploitation of more diverse compounds in the future is encouraged.
doi:10.1107/S1600536812022775
PMCID: PMC3379057
PMID: 22719278
The previous structure determination of the title compound, dibarium tritelluridocadmate, was based on powder X-ray diffraction data [Wang & DiSalvo (1999 ▶). J. Solid State Chem.
148, 464–467]. In the current redetermination from single-crystal X-ray data, all atoms were refined with anisotropic displacement parameters. The previous structure report is generally confirmed, but with some differences in bond lengths. Ba2CdTe3 is isotypic with Ba2
MX
3 (M = Mn, Cd; X = S, Se) and features 1
∞[CdTe2/2Te2/1]4− chains of corner-sharing CdTe4 tetrahedra running parallel [010]. The two Ba2+ cations are located between the chains, both within distorted monocapped trigonal–prismatic coordination polyhedra. All atoms in the structure are located on a mirror plane.
doi:10.1107/S1600536812038974
PMCID: PMC3470123
PMID: 23125567
A new iron phosphate, calcium triiron(III) tris(phosphate) oxide, CaFe3(PO4)3O, has been isolated and shown to exhibit a three-dimensional structure built by FeO6 octahedra, FeO5 trigonal bipyramids and PO4 tetrahedra. The FeOx (x = 5, 6) polyhedra are linked through common corners and edges, forming [Fe6O28]∞ chains with branches running along [010]. Adjacent chains are connected by the phosphate groups via common corners and edges, giving rise to a three-dimensional framework analogous to those of the previously reported SrFe3(PO4)3O and Bi0.4Fe3(PO4)3O structures, in which the Ca2+ cations occupy a single symmetry non-equivalent cavity.
doi:10.1107/S160053680902827X
PMCID: PMC2977148
PMID: 21583300
Single crystals of α-Ba2P2O7, dibarium diphosphate, were obtained under hydrothermal conditions. The structure belongs to the diphosphate A
2P2O7 series with A being an alkaline earth cation. α-Ba2P2O7 crystallizes isotypically with α-Sr2P2O7. All atomic sites have site symmetry m with the exception of two O atoms which reside on general positions. Both Ba2+ cations are coordinated by nine terminal O atoms from eclipsed diphosphate P2O7 anions to form a three-dimensional network throughout the structure.
doi:10.1107/S1600536810043527
PMCID: PMC3011656
PMID: 21589207
A crystallographic investigation of the title compound, C22H28Cl2N4O4, using crystals obtained under different crystallization conditions, revealed the presence of two distinct polymorphic forms. The molecular conformation in the two polymorphs is very different: one adopts a ‘C’ shape, whereas the other adopts an ‘S’ shape. In the latter, the molecule lies across a crystallographic twofold axis. The ‘S’-shaped polymorph undergoes a reversible orthorhombic-to-monoclinic phase transition on cooling, whereas the structure of the ‘C’-shaped polymorph is temperature insensitive.
doi:10.1107/S0108270109024457
PMCID: PMC2720150
PMID: 19652319
The title compound, cis,fac-dichloridotetrakis(dimethyl sulfoxide)-κ3
S,κO-ruthenium(II), [RuCl2(C2H6OS)4], was obtained from newly synthesized ruthenium complexes of 3-amino-2-chloropyridine. The Ru atom has a distorted octahedral coordination with two cis-oriented chloride ligands and four dimethyl sulfoxide ligands. Three of the sulfoxide ligands are S-bonded in a fac configuration, while the fourth is O-bonded. The title compound represents a new, and fourth, polymorph of the complex. Two other monoclinic forms and an orthorhombic modification have been reported previously.
doi:10.1107/S160053680801996X
PMCID: PMC2961945
PMID: 21203015