Crystal structure of 4,5-dinitroimidazole (45DNI)

A single-crystal X-ray diffraction study verified that the target oxidizer molecule, 4,5-dinitroimidazole (45DNI), had been synthesized. Some structural features of 45DNI are discussed and compared with those of 1,4-dinitroimidazole and 2,4 dinitroimidazole. 45DNI crystallizes with two crystallographically unique molecules in the monoclinic space group P2₁/n (#14) with unit-cell parameters a = 11.5360(8) Å, b = 9.071(1) Å, c = 11.822(1) Å, = 107.640(6)°, Z = 8, and has a density of 1.781 g/cm³. The molecular packing consists of infinite one-dimensional chains of 45DNI molecules approximately oriented in the ac direction which are linked by two different hydrogen bonds, and . In the lateral directions the chains are held together by molecular forces.     

Crystal and molecular structure of iso-grayanotoxin II

The crystal and molecular structure of a grayanotoxin derivative, iso-grayanotoxin II, is presented. The crystal is orthorhombic, space group . The molecule is based on a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered rings with various conformations.     

Crystallization of the $${\text{Mn}}^{{\text{II}}}[12{\text{-MC}}_{{\text{Mn}}^{{\text{III}}}{\text{(N)shi}}}{\text{-}}4]^{2+}$$ Mn II [ 12 -MC Mn III (N)shi - 4 ] 2 + Structure with 1,2,4-Triazolate from Methanol

Journal of Chemical Crystallography - The metallacrown (MC) dimer complex {MnII(OAc)(1,2,4-trz) $$[12{\text{-MC}}_{{\text{Mn}}^{{\text{III}}}{\text{(N)shi}}}{\text{-}}4]$$...     

Reaction of 2,3-bis(diphenylphosphino)maleic acid-thioanhydride (bmata) with PhCCo3(CO)9. X-ray diffraction structure of {\text{Co}}_{\text{3}} ({\text{CO)}}_{\text{6}} [\mu _2 ,\eta ^2 ,\eta ^1 {\text{ - C(Ph)}}{\text{(O)](}}\mu _2 {\text{ - PPh}}_{\text{2}} )

The benzylidyne-capped cluster PhCCo₃(CO)₉ (1) reacts with the diphosphine ligand 2,3-bis(diphenylphosphino)maleic acid-thioanhydride (bmata) to afford ultimately the new cluster ${\text{Co}}_{\text{3}} ({\text{CO)}}_{\text{6}} [\mu _2 ,\eta ^2 ,\eta ^1 {\text{ - C(Ph)}}{\text{(O)](}}\mu _2 {\text{ - PPh}}_{\text{2}} )$ (3) in low yield under thermolysis conditions or by Me₃NO activation of PhCCo₃(CO)₉. The intermediate cluster compound PhCCo₃(CO)₇(bmata) (2) has been confirmed by IR spectroscopy and is shown to give ${\text{Co}}_{\text{3}} ({\text{CO)}}_{\text{6}} [\mu _2 ,\eta ^2 ,\eta ^1 {\text{ - C(Ph)}}{\text{(O)](}}\mu _2 {\text{ - PPh}}_{\text{2}} )$ upon heating. Cluster 3 has been isolated and characterized in solution by IR and ³¹P NMR spectroscopies, and the solid-state structure of 3 was established by X-ray diffraction analysis. ${\text{Co}}_{\text{3}} ({\text{CO)}}_{\text{6}} [\mu _2 ,\eta ^2 ,\eta ^1 {\text{ - C(Ph)}}{\text{(O)](}}\mu _2 {\text{ - PPh}}_{\text{2}} )$ crystallizes in the triclinic space group P ${\bar 1}$ , a = 11.6053(8) Å, b = 11.8438(8) Å, c = 15.099(1) Å, α = 105.169(5)^○, β = 90.530(5)^○, γ = 104.976(6)^○, V = 1928.5(2) ų, Z = 2, and d _calc = 1.578; R = 0.0442, R _w = 0.481 for 2591 observed reflections with I > 3σ (I). The cyclic voltammetric properties of 3 have been investigated and are contrasted with the related bma-derived cluster ${\text{Co}}_{\text{3}} ({\text{CO)}}_{\text{6}} [\mu _2 ,\eta ^2 ,\eta ^1 {\text{ - }}{\text{(O)OC(O)](}}\mu _2 {\text{ - PPh}}_{\text{2}} )$ .     

The cubic space group of tungstogallate acid,H<Subscript>5</Subscript>GaW<Subscript>12</Subscript>O<Subscript>40</Subscript>

The space group of tungstogallate acid, H₅GaW₁₂O₄₀, reported by Niu et al. (J. Chem. Crystallogr. 2003, 33, 799) should be I–43m instead of Cm; the monoclinic C-centered cell is transformed to the I-centered cubic cell by (1 0 0; ,– , 1; – , – , –1).     

A crystallographic study of (2-acetylpyridine-κN 4-phenylthyosemicarbazonate-κ2N1,S) methyl-trans-dichlorotin(IV)

The preparation and characterization of [Sn(C₁₄H₁₃N₄S)(CH₃)Cl₂], an organotin(IV) complex containing 2-acetylpyridine(4)-phenylthiosemicarbazone, is described. The molecular structure was studied by single crystal X-ray diffraction, and IR and Mössbauer spectroscopies. The title compound crystallizes in the centric triclinic space group, P , as discrete neutral complexes, with the Sn(IV) ion in a distorted octahedral coordination geometry, with the thiosemicarbazone derivative in a meridional configuration and the chlorides in trans positions.     

Synthesis, crystal structure, and properties of the adduct of bis(O,O′-diisopropyl dithiophosphato)nickel(II) with pyridine [Ni(i-Pr2dtp)2(py)2]

A new adduct bis(pyridine)-bis(O,O-diisopropyl dithiophosphato-S,S)nickel(II), [Ni(i-Pr₂dtp)₂(py)₂] (dtp = dithiophosphate, py = pyridine) has been obtained by re-crystallization from CH₃COCH₃. The crystal and molecular structure of the title complex has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group P2₁/c, with lattice parameters a = 6.4890(13) Å, b = 16.386(3) Å, c = 14.830(3) Å, = 99.74(3)°, V = 1554.1(5) ų, and Z = 2. The crystal structure consists of discrete molecules of [Ni(i-Pr₂dtp)₂(py)₂], which displays a slightly distorted octahedral geometry for the NiS₄N₂ chromophore. Two O,O-diisopropyl dithiophosphate ions act as bidentate ligands with their S atoms coordinated to Ni atom. Each forms a four-membered chelate ring in the equatorial plane. The N atoms from two pyridine ligands are axially coordinated to the Ni atom. The Ni S bond distances are 2.4492(8) Å and 2.5711(9) Å, and the Ni bond distances are 2.127(3) Å. Thermal analyses show that the thermal decomposition of this adduct is so unstable that loss of two pyridine ligands begins at about 65°C. Electronic and IR spectra data is in agreement with the structural data.     

Synthesis and Crystal Structure of La(NO<Subscript>2</Subscript>)(SO<Subscript>4</Subscript>)(H<Subscript>2</Subscript>O)

Abstract Single crystals of new open-framework lanthanide sulphate nitrite La(NO₂)(SO₄)(H₂O) has been synthesized, in the presence of 2,6-diformyl-4-chlorophenol. His structure has been determined by X-ray diffraction data: the complex crystallizes in the tetragonal system, space group P4₃, with a = 7.0028(2) (?), b = 7.0028(2) (?), c = 11.8341(4) ?, V = 580.34(3) ?³, Z = 4, D _c = 3.582 Mg m⁻³. The three-dimensional (3D) framework of this compound is built up by the linkages of lanthanide atoms and the oxygen atoms of the sulphate and nitrite groups. The lanthanum atom is 9-fold coordinated. The structure is unfamiliar in lanthanide chemistry and this compound represents the first example of nitrite lanthanide sulphate complex. Graphical Abstract An unfamiliar structure in lanthanide chemistry represented by the first example of nitrite lanthanide sulphate complex is described.      

Crystal structure analysis of norbornadiene adduct of diphenyl hexamethylenimino phosphiniminocyclotrithiazene

The title compound (C₆H₁₂N)Ph₂P-N S₃N₃ C₇H₈ crystallizes in the monoclinic space group P2₁/n with unit cell dimensions: a = 9.9200(5), b = 16.3316(11), c = 15.7009(17) Å, = 91.99(1)°, and Z = 4. The cyclotrithiazene ring adopts a chair conformation with equal bond distances and the norbornadiene is fused in an exo, exo fashion to the heterocycle. Norbornadiene addition to the cyclotrithiazene influences the bonding pattern in the ring as well as the P N S moiety.     

Crystal and molecular structure of Rebek's imide

The crystal and molecular structure of Rebek's imide 1 is reported. Crystal data for 1: triclinic, space group , a = 7.8733(7) Å, b = 12.712(1) Å, c = 12.789(1) Å, = 86.628(5)°, = 84.628(5)°, = 72.981(5)°, V = 1217.9(2) ų, and D _c = 1.305 g/cm³ for Z = 2 and R = 0.047. The molecule crystallizes as a cyclic, hydrogen-bonded dimer held together by two N H...O and two O H...O hydrogen bonds involving amide...carboxylic acid interactions. The dimer organizes in the solid state to form 1D ribbons.     

A new class of flexible energetic salts, part 5: The structures of two hexammonium polymorphs and the ethane-1,2-diammonium salts of dinitramide

The crystal structures of two hexammonium polymorphs, 1 and 2, and the ethane-1,2-diammonium, 3, salts of dinitramide have been determined. 1 crystallizes in the triclinic space group with cell dimensions a = 6.391(2), b = 7.5826(9), c = 10.828(1) Å, a = 77.58(1), = 88.18 (2), = 87.54(2)°, 2 crystallizes in the monoclinic space group P2₁/c with cell dimensions a = 6.4893(3), b = 14.5149(8), c = 10.6557(4) Å, = 94.300(4)°, and 3 crystallizes in the triclinic space group with cell dimensions a = 5.614(1), b = 6.867(2), c = 7.371(2) Å, = 68.89(2), = 89.00(2), = 78.90(2)°. The three structures all contain protonated amine cations which are involved in hydrogen bonding interactions with dinitramide anions.     

Crystal structure of hexakis(tetrahydrofuran)sodium hexacarbonylvanadate(−I), [Na(THF)6 +][V(CO)6 −]

The title compound crystallizes in the space group with unit cell parameters (hexagonal setting)a=14.922(5)Å,c=14.379(9)Å,V=2773(3)ų andZ=3. The cation and the anion each lie on a site of (S₆) symmetry. Interatomic distances include Na–O(THF)=2.40(1) Å and V–C(CO)=1.91(2) Å.     

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.     

Two Mononuclear Compounds with bis(Pyrimidin-2-yl)amine as a Ligand and as a Hydrogen-bonded Lattice Molecule. Synthesis, Structure and Spectroscopy of {[M(dipm)(H2O)(A)](dipm)(A)(H2O)} (M?=?Cd with A?=?ClO4; and Zn with A?=?BF4)

Abstract  Two isostructural mononuclear compounds with formula {[Cd(dipm)(H₂O)(ClO₄)](dipm)(ClO₄)(H₂O)} (1) {[Zn(dipm)(H₂O)(BF₄)](dipm)(BF₄)(H₂O)} (2) and (in which dipm = bis(pyrimidin-2-yl)amine) have been synthesised and characterised by X-ray crystallography and infrared spectroscopy. The structure of compound 1 has been solved in the space group P2₁/n with a = 18.860(4), b = 8.579(2), c = 20.917(4) ?, β = 101.33(3)°, V = 3318.4(12) ?³, Z = 4 with final R = 0.0454. The structure of compound 2 has also been solved in the space group P2₁/n with a = 19.026(4), b = 8.389(1), c = 20.720(4) ?, β = 101.37(3)°, V = 3242.2(10) ?³, Z = 4 with final R = 0.0689. The geometry around the metal ions is octahedral, and is constituted by four nitrogen atoms from two dipm molecules, an oxygen atom from a water molecule and a semi-coordinating anion atom ( for compound 1 and for compound 2). In the lattice are also present: a non-coordinating water molecule, an anion molecule and a dipm molecule. For compound 1, the Cd–N distances are between 2.296 and 2.328 ?. The distance is 2.310 ? and the is 2.477 ?. The Zn–N distances in compound 2 are between 2.121 and 2.164 ?. The distance is 2.147 ? and the distance is 2.373 ?. A hydrogen bond interaction of the Watson–Crick type is observed between the amine N atom of a dipm ligand to a pyrimidyl N atom and a non-coordinating dipm ligand with N···N distances, which vary from 3.066(5) to 3.109(5) ?. Furthermore medium to strong hydrogen bond interactions are present between oxygen atoms of the water molecules and the anions of the compounds. Index Abstract  Two isostructural mononuclear compounds with formula {[Cd(dipm)(H₂O)(ClO₄)](dipm)(ClO₄)(H₂O)} (1) {[Zn(dipm)(H₂O)(BF₄)](dipm)(BF₄)(H₂O)} (2) and (in which dipm = bis(pyrimidin-2-yl)amine) have been synthesised and characterised by X-ray crystallography and infrared spectroscopy. . Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Construction of a hexanuclear cluster composed of spatially separated Co3 and Ru3 units: X-ray diffraction structure of Co3(CO)9[μ3-CCO2CH2CC{HRu3(CO)9}]

Treatment of the tricobalt cluster with the activated triruthenium cluster Ru₃(CO)₁₀(MeCN)₂ affords the acetylide-bridged hexanuclear cluster Co₃(CO)₉[₃–CCO₂CH₂CC{HRu₃(CO)₉}] in moderate yield. The new cluster was characterized in solution by IR spectroscopy and molecular structure was established by X-ray diffraction analysis. Co₃(CO)₉[₃–CCO₂CH₂CC{HRu₃(CO)₉}] crystallizes in the triclinic space group P(–1), a = 8.728(1) Å, b = 12.916(2) Å, c = 14.663(2) Å, = 82.950(2)°, = 82.465(2)°, = 86.199(2)°, V = 1624.2(4) ų, Z = 2, d _calc = 2.207 mg/m³; R = 0.0263, R _w = 0.0623 for 3596 observed reflections with I > 2(I). The coordination of the triruthenium cluster to the acetylene ligand of Co₃(CO)₉(₃–CCO₂CH₂CCH) is confirmed, and the structural details associated with the acetylide-bridged triruthenium frame are contrasted with other structurally characterized Ru₃ clusters bound by a 5e-acetylide ligand.     

Crystal and molecular structure of dimethylpyridazino[2,3-b]benzo-1,2,4-triazine-3,4-dicarboxylate radical,C14H11N4O4

The crystal and molecular structure of dimethylpyridazino[2,3-b]benzo-1,2,4-triazine-3,4-dicarboxylate radical, C₁₄H₁₁N₄O₄, has been determined from X-ray diffractometer data by direct methods and refined by least-squares methods toR=0.040 for 590 observed reflections. Crystals of C₁₄H₁₁N₄O₄ are monoclinic:a=9.222 (7),b=15.335(10),c=9.544(2) Å,=102.18(2)),Z=4, space groupP2₁/c. Bond distances and internal angles in the ring system have average values:C-C 1.387, C-N 1.358, and N-N 1.356 Å, and C--C 121.5, C--N 120.4, C- -C 117.8, N- -N 121.4, and N- -N 119.8°, respectively. All these bonds have a partial double-bond character, consistent with an extensive conjugation within the molecule, thus giving stability to the free radical. The condensed rings are nonplanar. The carbomethoxy groups show a different slant, owing to overcrowding.     

Structure of monoclinic dicalcium pyrophosphate tetrahydrate

Ca₂P₂O₇·4H₂O, monoclinicP2₁/c, a=6.008(1),_b=25.034(4),c=6.837(1) Å,=109.7 (1)°,Z=4,D ₀=2.20,D _c =2.24 g cm^–3. The structure was solved by direct methods and refined by block-diagonal matrix least squares to a finalR value of 0.038. Both calcium atoms are seven coordinate. The distance is 1.510(6) Å, whereas the distance is 1.619(1) Å and the P-O_B-P angle is 125.9(1)°.     

Ionic Radii in Mixed-Valence and Nonstoichiometric Metal Oxides and Their Polymorphic Forms

Abstract  A linear dependence of was found for ionic radii on the cube root of molecular volume standardised per oxygen atom (M _a/b O) of MO oxides of alkali earth metals, M₂O oxides of alkali metals and MO₂ oxides of f-electron metals, and parameters of the linear equation were calculated. This equation makes it possible to predict mean ionic radii of metals in compact structures of polymorphic forms of oxides, mixed-valence oxides and oxides showing deviation from stoichiometry, otherwise not accessible. Index Abstract  It is possible to predict mean ionic radii of metals in compact structures of polymorphic forms of oxides, mixed-valence oxides and oxides showing deviation from stoichiometry, otherwise not accessible, knowing the molecular volume standardised per oxygen atom of (M _a/b O) of MO oxides of alkali earth metals, M₂O oxides of alkali metals and MO₂ oxides of f-electron metals. Fig. The relation between the cube root of the molecular volume of oxides and the radii of the respective metal ions.      

CO substitution in Ru3(CO)12 by 2,3-bis(diphenylphosphino)-N-phenyl-maleimide (bppm). X-ray diffraction structure of Ru2(CO)6(bppm)

The cluster Ru₃(CO)₁₂ reacts with the diphosphine ligand 2,3-bis(diphenylphosphino)-N-phenyl-maleimide (bppm) in toluene solution at 100C by fragmentation to give a 2:1 mixture of the donor–acceptor complex Ru₂(CO)₆(-bppm) and the phosphido-bridged species Ru₂(CO)₆ , respectively. The new diruthenium compounds have been isolated by chromatography and characterized in solution by IR and NMR (¹H and ³¹P) spectroscopies, in addition to X-ray diffraction analysis in the case of Ru₂(CO)₆( ₂ -bppm). Ru₂(CO)₆( ₂ -bppm), which exists as two crystallographically independent molecules in the unit cell, crystallizes in the orthorhombic space group Pbca, a = 18.8441(9), b = 21.352(2), c = 36.510(2) Å, V = 14,690(1) ų, z = 16, D _calc = 1.649 g/cm³; R = 0.0356, and R _w = 0.0812 for 17732 observed reflections. The reactivity of the bis(diphenylphosphino)-N-phenyl-maleimide ligand with Ru₃(CO)₁₂ under thermolysis conditions is contrasted with the related diphosphine ligands 2,3-bis(diphenylphosphino)maleic anhydride (bma) and 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd).     

X-ray crystal structure and1H-NMR chiral shift reagent study of a crown trimer

3,4,5-Trimethoxybenzyl alcohol was cyclooligomerized with a bentonite clay used as a catalyst. Results of the crystal structure analysis of the racemic (±) nonamethoxy[1,1,1]orthocyclophane trimer, C₃₀H₃₆O₉, are described. The structure was determined by X-ray diffraction at 293 K and shown to belong to the triclinic space group P . The compound possesses a distorted crown conformation with unusual C–H...O intermolecular interactions, and with a crystal packing not observed before in other related derivatives. The racemic mixture was also discriminated in its two enantiomeric isomers, using proton NMR and Eu(III) as a chiral shift reagent.