Crystal structure of NH3(CH2)2NH3BiCl5·2H2O

The ethylenediammonium pentachlorobismuthate(III) dihydrate salt is monoclinic with the following unit cell dimensions: a = 10.902(8)Å, b = 7.926(6)Å, c = 15.199(6)Å, = 96.40(1)°, space group P2₁/n with Z = 4. The structure shows a layer arrangement parallel to the axis: planes of the [Bi₂Cl₁₀]^4– bioctahedra alternate with planes of [NH₃(CH₂)₂NH₃]²⁺ dications. The [Bi₂Cl₁₀]^4– bioctahedra are connected through O(W)–H··· Cl hydrogen bonds, so that infinite unidimensional chains of composition [Bi₂Cl₁₀(H₂O)₂] _n ^4n– are formed in the structure parallel to the axis. These chains are themselves interconnected by means of the N–H···Cl bonds originating from the [NH₃(CH₂)₂NH₃]²⁺ entities, forming a three-dimensional network.     

Synthesis and crystal structure of bis(carbamide)chromatoneptunyl NpO2CrO4 · 2[OC(NH2)2]

The crystal structure of the hexavalent neptunium complex NpO₂CrO₄ · 2[OC(NH₂)₂] is determined. The crystal data are a = 7.192(2) Å, b = 12.902(4) Å, c = 11.226(3) Å, β = 92.19(2)°, V = 1040.9(4) ų, space group P2₁/n, Z = 4, d _calcd = 3.223 g/cm³, R = 0.045, and R _w = 0.130. The coordination polyhedron of the Np atom is the pentagonal bipyramid whose equatorial plane is formed by the oxygen atoms of the chromate ions and carbamide molecules.     

Crystal structure of triethylentetraammonium bis monohydrogenmonophosphate dihydrate, [NH3(CH2)2NH2(CH2)2NH2(CH2)2NH3](HPO4)2 · 2H2O

The salt triethylentetraammonium bis monohydrogenmonophosphate dihydrate is monoclinic with the following unit cell dimensions: a = 8.462(1), b = 10.500(1), c = 9.520 Å, = 99.297(1)°, space group P2₁/n with Z = 2. The structure was solved by the Patterson method and refined to final R value of 0.043 for 1590 independent reflections. The structure consists of infinite parallel two-dimensional [ 01] planes built of mutually connected ions and water molecules by strong O—H···O and N—H···O hydrogen bonding.     

Crystal structure of tris-(2,2′,2″)-triaminoethylamino-salicylidene iron(III) complex

Tris-(2,2,2)-triaminoethylamino-salicylidene iron(III) crystallizes in the monoclinic crystal system witha=7.766(2),b=25.423(5),c=13.318(5) Å, =118.04(3)°, space group P2₁/c,V=2320.8(6) ų,Z=4, andD _x=1.464 g cm^–3. The center of the axially distorted octahedron is occupied by the Fe atom which is coordinated by six donor nitrogen and oxygen atoms infac positions. The planes of coordinated atoms (N and O) with the Fe(III) atom are almost planar and the maximum elevated atom from these planes is O(1) (–0.1065 Å).     

Interaction of cystamine with palladium(II) monoethanolaminate complex: Crystal structure of [Pd(NH2CH2CH2OH)4][Pd6(NH2CH2CH2S)8]Cl6 · 5H2O

The new compound [Pd(NH₂CH₂CH₂OH)₄][Pd₆(NH₂CH₂CH₂S)₈]Cl₆ · 5H₂O (I) is synthesized and its crystal structure is determined. The crystals are monoclinic, a = 25.625(6) Å, b = 9.633(5) Å, c = 24.847(7) Å, β = 91.47(2)°, Z = 4, and space group C2/c. The structural units of crystals I are the centrosymmetric hexanuclear [Pd₆(NH₂CH₂CH₂S)₈]⁴⁺ cations, the mononuclear [Pd(NH₂CH₂CH₂OH)4]²⁺ cations with C ₂ symmetry, the Cl^? anions, and crystallization water molecules. In the hexanuclear cation, the interaction between the Pd atoms occurs through the S atoms of the mercaptoethylaminate ligands. The Pd(2) and Pd(3) atoms and the ligands form two metallochelate fragments in which the N and S atoms are located in cis positions. The average lengths of the Pd-S and Pd-N bonds are equal to 2.274(1) and 2.074(6) Å, respectively. The metallochelate fragments are joined to each other and to their centrosymmetric analogues through the Pd(1) atom, which coordinates four S atoms [the average Pd-S_av bond length is 2.332(1) Å]. In the mononuclear cation, the Pd(4) atom coordinates four N atoms of the monoethylaminate ligands [the Pd-N bond lengths are 2.045(6) and 2.056(6) Å]. The shortest Pd?Pd distance is equal to 3.207(1) Å. The bonding in the structure is provided by numerous hydrogen bonds with the participation of all the H₂O molecules, NH₂ groups, and Cl^? anions.     

Crystal structure of triethylentetraammonium bis monohydrogen-monophosphate dihydrate β-NH3(CH2)2NH2(CH2)2NH2(CH2)2NH3(HPO4)2·2H2O

The salt triethylentetraammonium bis monohydrogen-monophosphate dihydrate is orthorhombic Pbca with unit cell dimensions a = 8.963(2), b = 10.326(2), c = 17.381(4)Å; Z = 4; D_m = 1.540 g cm^–3; D _x = 1.562 g cm^–3. The examination of the structure shows a layer arrangement parallel to the axis: planes of [HPO₄]^2– tetrahedra alternate with planes of [(NH₃(CH₂)₂NH₂CH₂)₂]⁴⁺. The [HPO₄]^2– tetrahedra are connected through O(W)s--H···O hydrogen bonds, so that infinite chains of the composition [HPO₄(H₂O)]_n ^2n– are formed in the structure parallel to the axis. The structure of this compound is built from [HPO₄]^2– anions, [(NH₃(CH₂)₂NH₂CH₂)₂]⁴⁺ cations and zeolitic water molecules connected by hydrogen bonds.     

Crystal structure of trans-W2(CO)6(PPh2H)2(μ2-PPh2)2

The molecular structure of trans-W²(CO)₆(PPh²H)²(₂-PPh²)² was determined by X-ray diffraction analysis. The two tungsten centers, bridged by two diphenylphosphido ligands, are separated by 3.0667(6) Å with W–P–W angles of 77.10(5) and 77.08(5). Average tungsten–phosphorus bond distances are 2.461(17) and 2.4576(21) Å for bridging and terminal phosphorus groups, respectively, with a range of 0.037 Å for the former and 0.001 Å for the latter. The complex crystallizes in the monoclinic space group P2₁/c with a = 19.282(4) Å, b = 12.158(2) Å, c = 21.294(9) Å, = 92.821(4), and Z = 4.     

Crystal structure of the addition compound of N,N′-bi(2-pyridylmethyl)-oxamide and complex of manganese with 1,10-phenanthroline

The structure of the addition compound, Mn(phen)₃(PMoxdH₂)(ClO₄)₂ was established by X-ray crystallography, where PMoxdH₂ is N,N-bi(2-pyridylmethyl)-oxamide. Six nitrogen atoms of the three 1,10-phenanthroline bind to the manganese ion and the oxygen atom of PMoxdH₂ is uncoordinated. The addition compound crystallizes in the monoclinic space group C2/c, with lattice parameters a = 23.780(6), b = 11.948(5), c = 18.466(6) Å, = 117.38(3)°, V = 4659(3) ų, and Z = 4.     

Crystal growth,structure, crystalline perfection and characterization of zinc magnesium ammonium sulfate hexahydrate mixed crystals ZnxMg(1−x)(NH4)2(SO4)2·6H2O

Mixed crystals Zn_xMg_(1?x)(NH₄)₂(SO₄)₂·6H₂O of the two well-known Tutton's salts Zn(NH₄)₂(SO₄)₂·6H₂O and Mg(NH₄)₂(SO₄)₂·6H₂O were grown with varying molar proportions (x=0.10–0.90) by slow evaporation solution growth technique. The mixed crystal Zn_0.54Mg_0.46(NH₄)₂(SO₄)₂·6H₂O is crystallizing in monoclinic system with space group P2₁/c and cell parameters a=6.2217(4) Å, b=12.5343(7) Å, c=9.2557(6) Å, β=106.912(3)°. The coexistence of zinc and magnesium ions in the mixed crystal was confirmed by inductively coupled plasma (ICP), atomic absorption spectroscopy (AAS) and energy dispersive X-ray spectroscopy (EDS). Compositional dependence of lattice parameters follows Vegard's relations. Slight variations are observed in FT-IR and XRD of pure and mixed crystals. Comparison of crystalline perfection as evaluated by high-resolution X-ray diffraction (HRXRD) for mixed crystals of various proportions reveals a reasonably good crystalline perfection for the mixed crystal with nearly equimolar ratio of Zn and Mg. The surface morphology of the mixed crystals changing with composition was studied by scanning electron microscopy (SEM). UV–vis studies reveal that the transparency of the mixed crystals was not much affected.     

Quaternary salts of oxo-sparteines: Crystal structure of N(16)-methyl-2-oxo-α-isosparteine iodide monohydrate

The molecular and crystal structure of N(16)-methyl-2-oxo--isosparteine iodide monohydrate have been determined by single crystal X-ray analysis using diffraction data collected on a diffractometer. The finalR for 1211 reflections and 196 parameters was 0.036. The configuration on the parent base, 2-oxo--isosparteine, remains unchanged after methyl substitution at thecisoidally oriented N(16) tertiary amino nitrogen. Because of an internal stress, four rings of the quaternary cation adopt a distorted conformation. The water molecule of crystallization links cation and anion by O_(lactam)H-O-HI^– hydrogen bonds. Weak C-HI^– interactions between the ions have been found in the crystal. Both the cation conformation and cation-anion interactions influence the position and shape ofv _CH bands in the IR spectrum of solid. The methyl C-H stretching vibrations are observed at 3090 and 3025 cm^–1, and the methylene absorption is observed in the region 3000-2800 cm^–1. Thev _OH water molecule absorption at 3490 and 3420 cm^–1 indicates two types of hydrogen bonding.     

Crystal structure of (ethylenediammonium-N,N′-di-3-propanoic acid) tetrachloropalladate(II) complex

The title compound was obtained by a synthesis from ethylenediamine-N,N-di-3-propanoic acid dihydrochloride (H₂eddp2HCl) and potassium hexachloropalladate(IV) (molar ratio 1:1, in water). Its structure has been determined by single-crystal X-ray diffraction: monoclinic space group P2₁/n, a = 8.198(1), b = 10.282(1), c = 9.080(1) Å, = 103.62(1)°, V = 743.9(2) ų, and Z = 2. The dianionic complex has a square-planar coordination geometry with four chloro ligands, and ethylenediamine-N,N-di-3-propanoic acid as dication in the second coordination sphere. This is the first reported Pd(II) structure with uncoordinated H₂eddp.     

Crystal and molecular structure of β-resorcylidene aminoguanidine copper(II) complex

The tridentate Schiff base, -resorcylidene aminoguanidine (RAG)1 was synthesized from 2,4-dihydroxybenzaldehyde and aminoguanidine and complexed with copper(II) to form a copper(II)--resorcylidene aminoguanidine (Cu-RAG)2 complex. X-ray diffraction analysis of compound2 (orthorhombic, Pnma,a=11.674(1);b=6.7198(7);c=17.836(2) ) revealed a square-planar copper(II) cation with a tridentate·ligand bound through two nitrogen atoms (N1 and N3) of the aminoguanidine moiety and an oxygen (O1) of the monodeprotonated dihydroxybenzaldehyde function. The remaining coordination site was occupied by chloride and the structure was rigidly planar as demanded by the restrictions of the crystallographic space group. The unit cell contents exhibited an extended sheet-like structure constructed via hydrogen bonds both intermolecularly and involving two water molecules (O3 and O4) also restricted by the same mirror symmetry. The remaining water (O5) provided for interlayer hydrogen bonding.     

Crystal structure of neptunium(V) sulfate hexahydrate, (NpO2)2SO4 · 6H2O

Single crystals of (NpO₂)₂SO₄ · 6H₂O are obtained, and their structure is determined. The structure is built of NpO ₂ ⁺ dioxo cations, SO ₄ ^2? anions, and molecules of coordination and crystallization water. The NpO ₂ ⁺ ions are linked into cationic ribbons stretched along the [001] direction. In the ribbons, neptunoyl ions of one type act as monodentate ligands, whereas neptunoyl ions of the other type coordinate the neighboring neptunoyl groups by two oxygen atoms. The Np(1) and Np(2) atoms have oxygen environments in the shape of a pentagonal bipyramid whose equatorial plane consists of oxygen atoms of the neighboring dioxo cations, sulfate ions, and water molecules. The sulfate ion acts as a bidentate ligand bridging the two neighboring atoms Np(1) and Np(2). Six water molecules are revealed in the structure; one of them is a crystallization water molecule. Hydrogen bonds link cationic ribbons into a three-dimensional network.     

Crystal structure of chlorotriphenyltin·diphenylcyclopropenone

Triphenyltin chloride forms with diphenylcyclopropenone a 1/1 molecular complex belonging to the triclinicP¯1 space group (a=10.267(4),b=12.095(2),c=12.319(3)Å,=90.67(2),=101.59(2), =112.58(2)°). The tin atom exists in a distortedtrans-trigonal bipyramidal (Sn-C=2.112(3), 2.123(3), 2.137(4), Sn-C1=2.440(1), Sn-O=2.510(2)Å) geometry, being displaced out of the equatorial plane (EC-Sn-C=354.3(3)°) towards the apical chlorine atom by 0.269(1)Å.     

Crystal structure of Al(tBu)3(NH2CH2CH2Ph): A molecular “slinky”

The molecular structure of Al(^tBu)₃(NH₂CH₂CH₂Ph) is determined by the crystal packing of the phenyl rings and the pseudo spherical Al(^tBu)₃ units, and may be viewed as a layered structure consisting of double sheets of the phenyl rings and the Al(^tBu)₃ units. The Al–N–C–C linkage shows severe disorder as a result of its flexibility. The structure of Al(^tBu)₃ (NH₂CH₂CH₂Ph) can be likened to a molecular slinky, in which the rigid ends are fixed in space by molecular packing forces, leaving the interior link to adopt multiple orientations. Crystal data: orthorhombic, Cmca,a=13.282(9),b=25.01(1),c=13.210(9), Å,V=4388(10) ų,Z=4,R=0.0957,R _w=0.0957.     

Crystal structure of a (μ-bis(carbene))dimetal complex of tungsten

The (-bis(carbene))ditungsten complex, (CO)₅W{(C(OCH₂Ph)C(CH₂C₂H₃)(Me)CH₂CH₂C(OCH₂Ph)}W(CO)₅ (1) is only the fifth such complex to be crystallographically characterized. The steric demands of one side of the bis(carbene) ligand gives rise to small, but statistically significant differences in the bonding parameters to W. The W=C distances are 2.195(4) and 2.171(6)Å. The carbonyltrans to the longest W=C bond has the shortest of the ten W-CO separations (1.994(5)Å) and the longest CO bond length (1.156(6)Å). The planes defined by the two carbene groups have a dihedral angle of 44.5°.     

Crystal structure of jinshajiangite from the Norra Kärr complex (Sweden)

The structure of the mineral jinshajiangite from the Norra Kärr alkaline complex (Sweden) was determined by single-crystal X-ray diffraction and refined to R = 6.7%. The monoclinic unit-cell parameters are a = 5.350(2) Å, b = 6.909(6) Å, c = 20.96(1) Å, β = 99.83(4)°, sp. gr. P2/m. This mineral is an Fe-rich analogue of surkhobite and perraultite, but it crystallizes in a different space group, and the unit-cell parameters a and b are two times smaller than those of these two minerals. The framework of jinshajiangite from Norra Kärr contains narrow and wide channels, which are occupied by Ca, Na, Ba, and K atoms in an ordered fashion.     

Crystal structure of N(1)-methyl-α-isosparteine iodide and 1,16-endomethylene-α-isosparteine diiodide

The crystal and molecular structures of mono- and di-quaternary salts ofa-isosparteine have been determined by X-ray analysis. Both N(1)-methyl--isosparteine iodide and 1,16-endomethylene-isosparteine diiodide crystallize in the space groupC222₁. The N-methylation does not change the configuration of parenttrans-cisoid-trans--isosparteine. The crystallographic twofold symmetry axis coincides with molecular symmetry of the diquaternary cation. Thetrans-cisoid-trans-1,16-endomethylene--isosparteine diiodide and its stereoisomer,trans-cisoid-cis-1,16-endo-methylenesparteine diiodide, form isomorphous crystals. Short cation-anion contacts in crystal structures suggest existence of C-H--I^– hydrogen bonds in the solid state. In the N(1)-methyl--isosparteine iodide crystal, 7CI^– distances in the range 3.85-4.15 Å have been found, while 17 distances of this type have been observed in 1,16-endomethylene--isosparteine diiodide.     

Crystal and molecular structure of 4-(3-indolyl)butyric acid-picric acid 2/2 π complex

The title compound, IBA-PIC, is 2C₁₂H₁₃NO₂·2C₆H₃N₃O₇, triclinic,P¯1,a=7.137(1),b=15.355(4),c=18.282(5) Å,=79.72(2),=79.85(2), =76.87(2)°. The structure was solved by direct methods and refined by least-squares techniques to anR factor of 0.068 for 3395 observed reflections. The IBA-PIC complex occurs as two independent molecules with different conformations. The crystallographic evidence for a prominent overlapping between the phenyl and indole rings corroborates earlier conclusions from UV spectroscopy. Molecules of both IBA and picric acid lie approximately parallel to (100) in layers and -bonding interactions across the 3.55 Å spacing. The angles between the indole ring and carboxyl-group planes are 82.9 and 86.9° for the A and B molecules, respectively.     

Crystal structure of [WI2(CO)2{P(OiPr)3}(η2-EtC2Et)]

[WI₂(CO)₂{P(OⁱPr)₃}(²-EtC₂Et)] crystallizes in the monoclinic space group P2₁/n, with a = 11.101(12), b = 16.272(18), c = 14.892(17) Å, = 93.27(1), Z = 4. The geometry can be considered to be pseudo-octahedral, with the 3-hexyne ligand occupying one site, with two iodo-groups, and the P(OⁱPr)₃ ligand completing the equational plane of ligands, with two trans-carbonyl groups occupying the axial sites.