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1.  Tetra­kis(dihydrogen pefloxacinium) di-μ2-chlorido-bis­[tetra­chloridobismuthate(III)] tetra­chloride octa­hydrate 
The title compound {systematic name: tetra­kis[4-(3-carb­oxy-1-ethyl-6-fluoro-4-hydroxonio-1,4-dihydro-7-quinol­yl)-1-meth­yl­piperazin-1-ium] di-μ2-chlorido-bis­[tetra­chlorido­bismuth­ate(III)] tetra­chloride octa­hydrate}, (C17H22FN3O3)4[Bi2Cl10]Cl4·8H2O, is composed of edge-shared centrosymmetric dinuclear [Bi2Cl10]4− anions, Cl− anions, dihydrogen pefloxacinium cations and water mol­ecules. The BiIII coordination polyhedron is a distorted octa­hedron. There are four short terminal Bi—Cl bonds [2.5037 (10)–2.6911 (7) Å] and two longer bridging bonds [2.8834 (8) and 3.0687 (9) Å] in each octa­hedron. Two sets of chloride ions and water mol­ecules are disordered over the same sites with site occupancies of 1/3 and 2/3, respectively. Anions, cations and water mol­ecules are linked by O—H⋯O, O—H⋯Cl and N—H⋯Cl hydrogen bonds, forming a three-dimensional framework. There are also π–π stacking inter­actions between quinoline ring systems [centroid–centroid distance = 3.575 (1) Å].
PMCID: PMC2961801  PMID: 21202786
2.  Octa­kis(3-methyl­anilinium) hexa­chlorido­cadmate tetra­chloride 
The asymmetric unit of the title compound, (C7H10N)8[CdCl6]Cl4, contains four 3-methyl­anilinium cations, two chloride anions and half an octa­hedral hexa­chloridocadmate(II) anion, which lies on an inversion centre. In the crystal, numerous N—H⋯Cl and bifurcated N—H⋯(Cl,Cl) hydrogen bonds link the components.
PMCID: PMC3238727  PMID: 22199604
3.  Strontium disodium hexa­thio­diphosphate(IV) octa­hydrate 
The crystal structure of SrNa2(P2S6)·8H2O is isotypic with that of its calcium analogue. The asymmetric unit consists of one Sr2+ cation (2 symmetry), two Na+ cations (2 and symmetry, respectively), one-half of a centrosymmetric (P2S6)4− anion with a staggered confirmation and four water mol­ecules. The crystal structure is built up from layers of cations and anions extending parallel to (101). Each SrO8 polyhedron is connected via edge-sharing to two NaO4S2 octa­hedra and to one NaO2S4 octa­hedron. The NaO4S2 octa­edra are, in turn, connected with two (P2S6)4− anions through common corners. Adjacent layers are held together by several O—H⋯S hydrogen-bonding inter­actions.
PMCID: PMC3007201  PMID: 21588078
4.  Poly[octakis(1H-imidazole-κN 3)octa-μ-oxido-tetra­oxidodicopper(II)tetra­vanadate(V)] 
In the title inorganic–organic hybrid compound, [Cu2V4O12(C3H4N2)8]n, the VV ion is tetra­coordinated by four O atoms and the CuII ion is hexa­coordinated by four N atoms from four imidazole ligands and two O atoms from two tetra­hedral vanadate (VO4) units in a distorted octa­hedral geometry. The structure consists of two-dimensional sheets constructed from centrosymmetric cyclic [V4O12]4− anions covalently bound through O to [Cu(imidazole)4]2+ cations. Adjacent sheets are linked by N—H⋯O hydrogen bonds and weak C—H⋯π inter­actions (H⋯centroid distances = 2.59, 2.66, 2.76, 2.91 and 2.98 Å into a three-dimensional supra­molecular network.
PMCID: PMC3343785  PMID: 22589759
5.  Calcium disodium hexa­thio­diphosphate(IV) octa­hydrate 
Single crystals of the title compound, CaNa2(P2S6)·8H2O, were obtained by adding calcium hydroxide to an aqueous solution of Na4(P2S6)·6H2O. The structure is isotypic with that of its strontium analogue and consists of one Ca2+ cation, two Na+ cations, one-half of a centrosymmetric (P2S6)4− anion with staggered confirmation and four water mol­ecules in the asymmetric unit. The crystal structure can be described as being built up from layers of cations and anions extending parallel to (101). Within a layer, each CaO8 polyhedron is connected via edge-sharing to two NaO4S2 octa­hedra and to one NaO2S4 octa­edron. The NaO4S2 octa­hedra are, in turn, linked with two (P2S6)4− anions through common corners. Various O—H⋯S hydrogen-bonding inter­actions lead to cohesion of adjacent layers. The Ca2+ and one Na+ cation are situated on a twofold rotation axis and the second Na+ cation is situated on an inversion centre.
PMCID: PMC3007360  PMID: 21588077
6.  Hexaaqua­nickel(II) tetra­aqua­bis­(μ-pyridine-2,6-dicarboxyl­ato)bis­(pyridine-2,6-dicarboxyl­ato)trinickelate(II) octa­hydrate 
The title compound, [Ni(H2O)6][Ni3(C7H3NO4)4(H2O)4]·8H2O, was obtained by the reaction of nickel(II) nitrate hexa­hydrate with pyridine-2,6-dicarb­oxy­lic acid (pydcH2) and 1,10-phenanothroline (phen) in an aqueous solution. The latter ligand is not involved in formation of the title complex. There are three different NiII atoms in the asymmetric unit, two of which are located on inversion centers, and thus the [Ni(H2O)6]2+ cation and the trinuclear {[Ni(pydc)2]2-μ-Ni(H2O)4}2− anion are centrosymmetric. All NiII atoms exhibit an octa­hedral coordination geometry. Various inter­actions, including numerous O—H⋯O and C—H⋯O hydrogen bonds and C—O⋯π stacking of the pyridine and carboxyl­ate groups [3.570 (1), 3.758 (1) and 3.609 (1) Å], are observed in the crystal structure.
PMCID: PMC3007465  PMID: 21588093
7.  Monoclinic polymorph of poly[aqua(μ4-hydrogen tartrato)sodium] 
A monoclinic polymorph of the title compound, [Na(C4H5O6)(H2O)]n, is reported and complements an ortho­rhom­bic form [Kubozono, Hirano, Nagasawa, Maeda & Kashino (1993 ▶). Bull. Chem. Soc. Jpn, 66, 2166–2173]. The asymmetric unit contains a hydrogen tartrate anion, an Na+ cation and a water mol­ecule. The Na+ ion is surrounded by seven O atoms derived from one independent and three symmetry-related hydrogen tartrate anions, and a water mol­ecule, forming a distorted penta­gonal–bipyramidal geometry. Independent units are linked via a pair of inter­molecular bifurcated O—H⋯O acceptor bonds, generating an R 2 1(6) ring motif to form polymeric two-dimensional arrays parallel to the (100) plane. In the crystal packing, the arrays are linked by adjacent ring motifs, together with additional inter­molecular O—H⋯O inter­actions, into a three-dimensional network.
PMCID: PMC2979804  PMID: 21579620
8.  Octa­kis[2,2′,5,5′-tetra­thia­fulvalenium(0.5+)] bis­[hexa­molybdate(2−)] acetonitrile solvate 
The asymmetric unit of the title compound, (C6H4S4)8[Mo6O19]2·CH3CN, contains two halves of two centrosymmetric [Mo6O19]2− hexa­molybdate anions, which are each built up from six distorted MoO6 octa­hedra sharing common edges and one common vertex at the central O atom, six tetra­thia­fulvalene cations (three of which are located on mirror planes) to balance the charge and a half of an acetonitrile solvent mol­ecule, likewise located on a mirror plane. The two central hexa­molybdate O atoms occupy special positions 2a and 2d, respectively. The cations and anions are inter­linked through C—H⋯O contacts.
PMCID: PMC2970104  PMID: 21577422
9.  Bis[tris­(ethyl­enediamine-κ2 N,N′)cobalt(III)] octa­kis-μ-3-oxido-hexa­deca-μ2-oxido-tetra­deca­oxido-μ12-tetra­oxo­silicato-octa­molybdenum(VI)hexa­vanadium(IV,V) hexa­hydrate 
The title compound, [Co(C2H8N2)3]2[SiMo8V4O40(VO)2]·6H2O, was prepared under hydro­thermal conditions. The asymmetric unit consists of a transition metal complex [Co(en)3]3+ cation (en is ethyl­enediamine), one half of an [SiMo8V4O40(VO)2]6− heteropolyanion, two solvent water mol­ecules in general positions and two half-mol­ecules of water located on a mirror plane. In the complex cation, the Co3+ ion is in a distorted octa­hedral coordination environment formed by six N atoms of the three chelating en ligands. One of the en ligands exhibits disorder of its aliphatic chain over two sets of sites of equal occupancy. The [SiMo8V4O40(VO)2]6− heteropolyanion is a four-electron reduced bivanadyl-capped α-Keggin-type molybdenum–vanadium–oxide cluster. In the crystal, it is located on a mirror plane, which results in disorder of the central tetra­hedral SiO4 group: the O atoms of this group occupy two sets of sites related by a mirror plane. Furthermore, all of the eight μ2-oxide groups are also disordered over two sets of sites with equal occupancy. There are extensive inter­molecular N—H⋯O hydrogen bonds between the complex cations and inorganic polyoxidoanions, leading to a three-dimensional supra­molecular network.
PMCID: PMC3238691  PMID: 22199568
10.  μ-Oxido-bis­[bis­(phenanthroline-κ2 N,N′)(sulfato-κO)iron(III)] octa­hydrate 
The title complex, [Fe2O(SO4)2(C12H8N2)4]·8H2O, contains two unique FeIII cations, one oxide anion, four 1,10-phenanthroline (phen) ligands, two coordinated sulfate anions and eight lattice water mol­ecules. Each FeIII ion has an approximate octa­hedral geometry, coordinated by four N atoms from two phen mol­ecules, two O atoms from oxide and sulfate anions, respectively. The parallel phen mol­ecules form two-dimensional supermolecules through π–π stacking inter­actions [centroid–centroid distances = 3.684 (3), 3.711 (3), 3.790 (3), 3.847 (3), 3.746 (3), 3.732 (3) and 3.729 (3) Å]. This architecture is further stabilized by O—H⋯O hydrogen bonds involving the lattice water mol­ecules and sulfate O atoms.
PMCID: PMC3246986  PMID: 22219806
11.  Tricaesium tris­(pyridine-2,6-dicarboxyl­ato-κ3 O 2,N,O 6)lutetium(III) octa­hydrate 
Colourless block crystals of the title compound, Cs3[Lu(dipic)3]·8H2O [dipic is dipicolinate or pyridine-2,6-dicarboxyl­ate, C7H3NO4] were synthesized by slow evaporation of the solvent. The crystal structure of this LuIII-complex, isostructural with the DyIII and EuIII complexes, was determined from a crystal twinned by inversion and consists of discrete [Lu(dipic)3]3− anions, Cs+ cations and water mol­ecules involving hydrogen bonding. The Lu atom lies on a twofold rotation axis and is coordinated by six O atoms and three N atoms of three dipicolinate ligands. One Cs atom is also on a twofold axis. The unit cell can be regarded as successive layers along the crystallographic c-axis formed by [Lu(dipic)3]3− anionic planes and [Cs+, H2O] cationic planes. In the crystal structure, although the H atoms attached to water mol­ecules could not be located, short O—O contacts clearly indicate the occurrence of an intricate hydrogen-bonded network through contacts with other water mol­ecules, Cs cations or with the O atoms of the dipicolinate ligands.
PMCID: PMC2959249  PMID: 21201028
12.  Decyl­ammonium octa­noate 
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.
PMCID: PMC3052094  PMID: 21522407
13.  Barium dierbium(III) tetra­sulfide 
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.
PMCID: PMC3588518  PMID: 23476480
14.  Rietveld refinement of Ba5(AsO4)3Cl from high-resolution synchrotron data 
The apatite-type compound Ba5(AsO4)3Cl, penta­barium tris­[arsenate(V)] chloride, has been synthesized by ion exchange at high temperature from a synthetic sample of mimetite (Pb5(AsO4)3Cl) with BaCO3 as a by-product. The results of the Rietveld refinement, based on high resolution synchrotron X-ray powder diffraction data, show that the title compound crystallizes in the same structure as other halogenoapatites with general formula A 5(YO4)3 X (A = divalent cation, Y = penta­valent cation, X = Cl, Br) in space group P63/m. The structure consists of isolated tetra­hedral AsO4 3− anions (m symmetry), separated by two crystallographically independent Ba2+ cations that are located on mirror planes and threefold rotation axes, respectively. The Cl− anions are at the 2b sites ( symmetry) and are located in the channels of the structure.
PMCID: PMC2960624  PMID: 21201569
15.  catena-Poly[bis­[octa­kis(dimethyl sulf­oxide)praseodymium(III)] hexa-μ3-sulfido-dodeca-μ2-sulfido-hexa­sul­fido­hexa­silverhexa­molybdenum] 
The title compound, {[Pr(C2H6OS)8]2[Mo6Ag6S24]}n, contains polymeric Mo6S24Ag6 2− anions and [Pr(Me2SO)8]3+ cations, forming a one-dimensional polymeric Mo/S/Ag cluster. The anion assumes the conformation of a zigzag chain. The trivalent cations are arrayed amongst the anionic chains and are well separated from each other. Each Mo and Ag atom is coordinated by four S atoms in a distorted tetra­hedral geometry. The Pr3+ atom is coordinated by eight dimethyl sulfoxide ligands, forming a polyhedron-shaped distorted square anti­prism.
PMCID: PMC2962003  PMID: 21203073
16.  An ionic organic–inorganic hybrid: tetra­kis[bis­(1,10-phenanthroline)copper(I)] dodeca­tungstophosphate(V) 
Single crystals of the title polyoxometallate-based organic–inorganic hybrid, [Cu(C12H8N2)2]4[SiW12O40], were grown under hydro­thermal conditions. The discrete [SiW12O40]4− anions are of the Keggin type and are packed in a slightly distorted ortho­rhom­bic F-centred mode, with the complex [CuI(phen)2]+ cations (phen is 1,10-phenanthroline) located in the voids of this arrangement. The four independent CuI cations are situated in the centres of more or less distorted tetra­hedra made up of N atoms from the phen ligands. The anions and cations are linked together via weak hydrogen-bonding inter­actions, forming an extended three-dimensional network. Additional stabilization is achieved via π–π inter­actions between different phen mol­ecules of adjacent [CuI(phen)2]+ cations with shortest distances between 3.416 and 3.499 Å.
PMCID: PMC2915059  PMID: 21200465
17.  Trilithium thio­arsenate octa­hydrate 
The title compound, Li3AsS4·8H2O, is built up from infinite cationic [Li3(H2O)8]3+ chains which extend along [001] and are cross-linked by isolated tetra­hedral AsS4 3− anions via O—H⋯S hydrogen bonds. Two Li and two As atoms lie on special positions with site symmetries -1 (1 × Li) and 2 (1 × Li and 2 × As). The [Li3(H2O)8]3+ chain contains four independent Li atoms of which two are in octa­hedral and two in tetra­hedral coordination by water O atoms. An outstanding feature of this chain is a linear group of three edge-sharing LiO6 octa­hedra to both ends of which two LiO4 tetra­hedra are attached by face-sharing. Such groups of composition Li5O16 are linked into branched chains by means of a further LiO4 tetra­hedron sharing vertices with four adjacent LiO6 octa­hedra. The Li—O bonds range from 1.876 (5) to 2.054 (6) Å for the LiO4 tetra­hedra and from 2.026 (5) to 2.319 (5) Å for the LiO6 octa­hedra. The two independent AsS4 3− anions have As—S bond lengths ranging from 2.1482 (6) to 2.1677 (6) Å [ = 2.161 (10) Å]. The eight independent water mol­ecules of the structure donate 16 relatively straight O—H⋯S hydrogen bonds to all S atoms of the AsS4 tetra­hedra [ = 3.295 (92) Å]. Seven water mol­ecules are in distorted tetra­hedral coordination by two Li and two S; one water mol­ecule has a flat pyramidal coordination by one Li and two S. At variance with related compounds like Schlippe’s salt, Na3SbS4·9H2O, there are neither alkali–sulfur bonds nor O—H⋯O hydrogen bonds in the structure.
PMCID: PMC3647787  PMID: 23723753
18.  Bis{1-[(1H-benzimidazol-1-yl)meth­yl]-1H-imidazole-κN 3}bis­(3,5-dicarb­oxy­benzoato-κ2 O 1,O 1′)nickel(II) octa­hydrate 
In the title complex, [Ni(C9H5O6)2(C11H10N4)2]·8H2O, the NiII ion exhibits site symmetry 2. It has a distorted octa­hedral coordination defined by two N atoms from two symmetry-related 1-[(1H-benzimidazol-1-yl)meth­yl]-1H-imidazole ligands and four O atoms from two symmetry-related 3,5-dicarb­oxy­benzoate anions. In the crystal, the complex mol­ecules and solvent water mol­ecules are linked via O—H⋯O, O—H⋯N and N—H⋯O hydrogen bonds, forming a three-dimensional structure. There are also a number of C—H⋯O inter­actions present.
PMCID: PMC3629470  PMID: 23633988
19.  Poly[[octaaqua-μ4-(benzene-1,2,4,5-tetra­carboxyl­ato)-dicobalt(II)] octa­hydrate] 
The title polymeric coordination compound, {[Co2(C10H2O8)(H2O)8]·8H2O}n, was obtained by slow diffusion of a dilute aqueous solution of CoCl2 and the sodium salt of benzene-1,2,4,5-tetracarboxylic acid (H4btec) through an agar–agar gel bridge in a U-shaped tube. The two independent Co2+ ions are each situated on an inversion centre and are coordinated in a slightly distorted octa­hedral geometry by four water O atoms and two carboxyl­ate O atoms from two btec4− ligands (-1> symmetry), forming a layer parallel to (11-1). This layer can be described as a mol­ecular two-dimensional square grid with the benzene rings at the nodes and the CoII atoms connecting the nodes. O—H⋯O hydrogen-bonding interactions involving the coordinating water molecules, the carboxylate O atoms and lattice water molecules lead to the formation of a three-dimensional network.
PMCID: PMC3885008  PMID: 24454183
20.  Thulium nickel/lithium distannide, TmNi1−xLixSn2 (x = 0.035) 
The quaternary thulium nickel/lithium distannide, TmNi1−xLixSn2 (x = 0.035), crystallizes in the ortho­rhom­bic LuNiSn2 structure type. The asymmetric unit contains three Tm sites, six Sn sites, two Ni sites and one Ni/Li site [relative occupancies = 0.895 (8):0.185 (8)]. Site symmetries are .m. for all atoms. The 17-, 18- and 19-vertex distorted pseudo-Frank–Kasper polyhedra are typical for all Tm atoms. Four Sn atoms are enclosed in a 12-vertex deformed cubo­octa­hedron, and another Sn atom is enclosed in a penta­gonal prism with three added atoms. A tricapped trigonal prism is typical for a further Sn atom. The coordination number for all Ni atoms and Ni/Li statistical mixtures is 12 (fourcapped trigonal prism [Ni/LiTm5Sn5]). Tm atoms form the base of a prism and Ni/Li atoms are at the centres of the side faces of an [SnTm6Ni/Li3] prism. These isolated prisms are implemented into three-dimensional-nets built out of Sn atoms. Electronic structure calculations using TB-LMTO-ASA suggest that the Tm and Ni/Li atoms form positively charged n[TmNi/Li]m+ polycations which compensate the negative charge of 2n[Sn]m− polyanions. Analysis of the inter­atomic distances and electronic structure calculations indicate the dominance of a metallic type of bonding.
PMCID: PMC3884236  PMID: 24454012
21.  Redetermination of 4-(dimethyl­amino)­pyridinium tribromide 
In the title salt, C7H11N2 +·Br3 −, the essentially planar cation (r.m.s. deviation = 0.006 Å) forms an N—H⋯Br hydrogen bond to one of the Br atoms of the almost linear anion [Br—Br—Br = 179.31 (2)°]. The crystal studied was found to be a racemic twin. The whole-mol­ecule disorder of the cation and anion about a twofold rotation axis described earlier [Ng (2009). Acta Cryst. E65, o1276] is an artifact of halving one of the axes of the ortho­rhom­bic unit cell.
PMCID: PMC3008028  PMID: 21588594
22.  (R)-2-{2-[(S)-(2′-Benzo­yloxy-1,1′-binaphthyl-2-yl)oxycarbonyl­amino]-3-phenylpropanamido­meth­yl}pyridinium picrate acetone solvate 
In the crystal structure of the title compound, C43H34N3O5 +·C6H2N3O7 −·C3H6O, the large dimension and shape of the cation are responsible for the elongation of the ortho­rhom­bic unit cell. The ions and acetone mol­ecules are linked together by a system of hydrogen bonds involving an inter­molecular hydrogen bond between one N atom of the cation and the O atom of acetone and two inter­molecular hydrogen bonds between the cation N atoms and the O atoms of the picrate anion. No intra­molecular hydrogen bonds exist in the structure. The dihedral angle between the two naphthalene ring systems is 76.16 (13)°. The chiral C atom has a known R configuration, but this cannot be confirmed from this X-ray analysis.
PMCID: PMC2915369  PMID: 21200887
23.  Monoclinic form I of clopidogrel hydrogen sulfate from powder diffraction data 
The asymmetric unit of the title compound, C16H17ClNO2S+·HSO4 −, (I) [systematic name: (+)-(S)-5-[(2-chloro­phen­yl)(meth­oxy­carbon­yl)meth­yl]-4,5,6,7-tetra­hydro­thieno[3,2-c]pyridin-5-ium hydrogen sulfate], contains two independent cations of clopidogrel and two independent hydrogensulfate anions. The two independent cations are of similar conformation; however, this differs from that observed in ortho­rhom­bic form (II) [Bousquet et al. (2003 ▶). US Patent No. 6 504 030]. The H—N—Cchiral—H fragment shows a trans conformation in both independent cations in (I) and a gauche conformation in (II). In (I), classical inter­molecular N—H⋯O and O—H⋯O hydrogen bonds link two independent cations and two independent anions into an isolated cluster, in which two cations inter­act with one anion only via N—H⋯O hydrogen bonds. Weak inter­molecular C—H⋯O hydrogen bonds further consolidate the crystal packing.
PMCID: PMC3007342  PMID: 21588394
24.  An ortho­rhom­bic polymorph of the ultraphosphate YP5O14  
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.
PMCID: PMC2968816  PMID: 21582306
25.  Diytterbium(II) lithium indium(III) digermanide, Yb2LiInGe2  
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.
PMCID: PMC2979241  PMID: 21578989

Results 1-25 (139320)