The single-crystal structure of 2-S-(1′-deoxy-2′,3′:4′,5′-di-O-isopropylidene-D,L-xylit-1′-ylthio)-3-methylquinoxaline (C₂₀H₂₆N₂O₄S) was determined at 293 K and refined to R1 = 0.0510 and wR2 = 0.1514 for 5083 observed reflections. This crystal is orthorhombic, Pna2₁ with Z = 8. Two molecules constitute the asymmetric unit. The unit-cell dimensions are: a = 14.590(3)Å, b = 9.672(2)Å, c = 28.074(5)Å and V = 3964(2)ų.

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The crystal structure of [C₆H₄OCH₃NH₃]₂BiCl₅ was determined at room temperature. The compound crystallized in the following monoclinic space group: P2₁/c. The unit-cell dimensions are: a = 12.318(5), b = 21.486(5), c = 8.001(5)Å, β = 83.520(5)° with Z = 4. Its crystal structure was determined and refined down to R = 0.0365. The structure of this compound consists of corrugated layers of BiCl₅^2- chains in which slightly distorted [BiCl₆]^3- octahedral sharing two cis vertices are interconnected into chains separated by layers of organic [C₆H₄OCH₃NH₃]⁺ cations. These chains are themselves interconnected by means of the N-H…Cl hydrogen bonds, forming a three-dimensional network.

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The structure of 1,3,5-trimethyl-5-phenyl-2,4,6(1H,3H,5H)-pyrimidinetrithione was determined by X-ray crystallography. The phenyl ring exists in an axial position of the 2,4,6(1H,3H,5H)-pyrimidinetrithione ring. The pyrimidine-trithione ring system exhibits conjugation involving the lone pairs on the N atoms and three C=S bonds. Intermolecular C-H…S interactions and S…S contacts were observed in the crystal lattice.

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The synthesis and crystal structure are given for the bis(N,N,N′,N′-tetramethyl-ethylenediammonium)decachlorodibis-muthate(III) trihydrate salt. An X-ray investigation has shown that the title compound crystallizes in a non-centrosymmetric monoclinic system, space group C2 with the following lattice parameters: a = 13.535(4)Å, b = 14.893(5)Å, c = 10.158(4)Å, β = 121.54(3)°, V = 1745(1)ų, Z = 2 and ρ_cal = 2.053 g cm^-1. The structure was solved from 1921 independent reflections with R₁ = 0.0318 and wR₂ = 0.0743, and refined with 145 parameters. The structure shows a layer arrangement along the c-axis: planes of [Bi₂Cl₁₀]^4- bioctahedra alternate with planes of [((CH₃)₂NH)₂(CH₂)₂]²⁺ dications. Since the [Bi₂Cl₁₀]^4- anions are connected through O(W)-H…Cl hydrogen bonds (via water molecules), infinite unidimensional chains of composition [Bi₂Cl₁₀(H₂O)₃]_n^4n- are formed in ae structure parallel to the c-axis. These chains are themselves interconnected by means of N-H…Cl bonds originating from the [((CH₃)₂NH)₂(CH₂)₂]²⁺ entities, forming a three-dimensional network.

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The title compound crystallized in triclinic space group P1 with cell parameters a = 6.6634(3)Å, b = 12.3296(6)Å c = 17.0338(8)Å, α = 86.394(1)°, β = 81.052(1)°, γ = 85.002(1)°, V = 1375.43(11)ų, Z = 2, D_cal = 1.226 Mg/m³ at T = 100(2)K. The structure was refined by full-matrix least-squares procedures to find R₁ = 0.0480 and wR₂ = 0.1143 for 5663 reflections. All atoms in the furo-pyran ring are in a plane, except C₆. All three cyclohexyl rings of isocyanides adapt chair conformation, and their plane alignment is noncoplanar with respect to furo-pyran plane. The spiro cycloheptyl ring has a chair conformation.

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The crystal structure of (R,R)-tartaric acid complex of (R)-nipecotic acid ethyl ester has been determined. In the crystal packing, the corrugated layers from tartaric acid are parallel to the ac-plane. The carboxy group of tartaric acid bonds to the amine group of nipecotic acid, and the chair-ring moiety is fixed at the bottom of a valley.

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The structure of 4-phenyl-piperazine-1-sulfonamide was determined by X-ray crystallography. The compound crystallized in a monoclinic system and was characterized as follows: P2₁/c, a = 24.1829(7), b = 9.5485(3), c = 9.7885(2)Å, β = 92.2337(16)°, Z = 8, V = 2258.55(11)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0427 for 3206 reflections [I > 2σ(I)] and R1 = 0.0739, wR2 = 0.1083 for all the 4589 unique reflections. The crystal structure consists of layers of polar regions that enclose a sulfonamide function linked by hydrogen bonds and hydrophobic regions with π-π stacking interactions.

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The salt tris(2-amino-indolinium)hexachlorobismuthate(III) monohydrate [C₈H₉N₂]₃BiCl₆·H₂O crystallizes at room temperature in the monoclinic system with space group P2₁/n. The unit-cell dimensions are: a = 15.1853(14), b = 11.7761(9), c = 17.3168(13)Å, β = 103.937(8)° with Z = 4. The crystal structure of this salt was solved by Patterson methods and refined by full-matrix least squares on F² to final values of R = 0.0293 and wR = 0.0786. The structure consists of monomeric BiCl₆^3- anions, monoprotonated 2-amino-indolinium cations and water molecules. These entities are interconnected by means of hydrogen bonding contacts [N-H…O(Cl) and O(W)-H…Cl], forming a three-dimensional network.

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The structure of 4,4-dimethyl-1-[2-phenyl-1-(phenylamino)ethyl]piperidin-2,6-dione crystallizes in the orthorhombic space group Pna2₁ with unit-cell parameters a = 22.9565(14)Å, b = 6.3725(4)Å, c = 24.6677(17)Å, Z = 8 and V = 3608.6(4)ų. The structure was solved by direct methods, and the final R value is 0.0826. There exists two crystallographically independent molecules in the asymmetric unit. The piperidine ring makes dihedral angles of 65.24(2)° and 56.48(2)° respectively, with the phenyl and phenylamine moieties of molecule-I (the corresponding values for molecule-II are 53.17(2)° 59.02(2)° and respectively). Few X-H…A inter- and intramolecular hydrogen interactions have been observed.

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The salt NaH₂(PO₄)_0.48(AsO₄)_0.52·H₂O (abbreviated as NDAP) derives from the NaH₂PO₄·H₂O-NaH₂AsO₄·H₂O system. The structural characteristics of the crystals were analyzed by means of X-ray diffraction, and solved from 3737 independent reflections with R₁ = 0.019 and Rw₂ = 0.045, then refined with 84 parameters. The following results have been obtained: space group P2₁2₁2₁, a = 5.1383(5)Å, b = 8.3301(8)Å, c = 10.2492(10)Å and Z = 4. The crystal structure of NDAP is built up from a discrete tetrahedral P(As)O₄^3- connected with O-H…O hydrogen bonds and through the electrostatic actions of Na⁺ cations.

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The salt tris(4-dimethylaminopyridinium)tetrachoroantimonate C₇H₁₁Cl₄N₂Sb crystallizes at room temperature in the monoclinic system with space group C2/c. The unit-cell dimensions are: a = 13.6692(5), b = 15.1035(7), c = 7.5223(3)Å, β = 123.39(2)° with Z = 4. The crystal structure of this salt was solved by Patterson methods and refined by full-matrix least-squares on F² to final values of R = 0.0316 and wR = 0.0975. The structure consists of infinite chains formed by SbCl₄^- anions packed so as to make a rigid tunnel-like structure wherein the planar cations are stacked. The [SbCl₄^-]ⁿ anions have a slightly distorted octahedral geometry with Sb-Cl distances ranging between 2.4315(7) and 2.6395(11)Å. Chains of SbCl₆ octahedra oriented along the c axis are connected to the cations by hydrogen bonds, N-H…Cl.

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The crystal structure of the title compound, C₆₁H₆₆N₄Si(I) displays a highly unsymmetric molecular entity involving three different substituents on the meso-positions. The molecular units in the crystal are intermolecularly bonded to each other via π-π, and CH-π interactions, resulting in the genesis of a 2D structural motif. This compound crystallizes in the triclinic system of the P1 space group with the following cell parameters: a = 8.9729(10), b = 19.167(2), c = 20.763(2)Å; α = 65.932(2)°, β = 81.356(2)°, γ = 86.051(2)°, Z = 2.

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The structure of 1-methyl-4-[2-(4-hydroxyphenyl)ethenyl)]pyridinium hydrogensquarate was determine by X-ray crystallography. A symmetry operation (-x+1, -y, -z) generates the whole molecule. The compound crystallized in a monoclinic system and was characterized thus: P2₁/c, a = 7.3400(15), b = 9.4400(19), c = 23.000(5)Å, β = 94.00(3)°, Z = 4, V = 1589.8(6)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0738 and wR2 = 0.1396.

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The structure of 4-isonicotinoylcoumarin was determine by X-ray crystallography. A symmetry operation (-x+2, -y+1, -z) generates the whole molecule. The compound crystallized in a monoclinic system, and was characterized thus: P2₁/c, a = 7.8507(16), b = 16.361(3), c = 9.826(2)Å, β = 107.13(3)°, Z = 4, V = 1206.2(4)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0568 and wR2 = 0.0926.

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The structure of 5,17-di-tert-butyl-26,28-dimethoxycalix[4]arene-25,27-diquinone, obtained by controlled potential electrolysis on a platinum electrode of 5,11,17,23-tetra-tert-butyl-26,28-dimethoxycalix[4]arene-25,27-diol, was determined by an X-ray diffraction method. Preparative oxidation of the calix[4]arene derivative in an acetonitrile solution leads to its corresponding calix[4]arenemonoquinone and calix[4]arenediquinone. 5,17-Di-tert-butyl-26,28-dimethoxycalix[4]arene-25,27-diquinone crystallizes from CH₂Cl₂ in monoclinic space group P2₁/a with a = 15.7058(6), b = 14.8399(10), c = 16.3334(9)Å, β = 117.778(4), V = 3368.2(3)ų, and Z = 4. A structural analysis revealed that this compound crystallises as a solvate with CH₂Cl₂ molecules embedded in pairs of calix[4]arenediquinone.

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1-Butyl-4,5-dibromo-3-methylimidazolium iodide has been synthesized and structurally characterized by X-ray crystallography. This salt crystallizes in the monoclinic system, space group P2₁/n with cell parameters of a = 7.8471(6), b = 14.8581(11), c = 10.9176(8)Å, β = 98.5950(10)°, V = 1258.62(16)ų, and Z = 4. The crystal structure was solved by a direct method and refined by full-matrix least squares to a final R value of 0.0253 with I > 2σ(I). This salt is organized into zigzag sheets with successive honeycomb-like frameworks through halogen bonding and hydrogen bonding.

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The structure of [RuCl(6-hydroxypicolinato)(2,2′;6′,2″-terpyridine)]·(N,N-dimethylformamide) was determined by X-ray crystallography. The compound crystallized in a monoclinic system and was characterized thus: P2₁/c, a = 15.7325(19), b = 10.0621(10), c = 15.6422(19)Å, β = 105.112(3)°, Z = 4, V = 2390.6(5)ų. The crystal structure was solved by the SIR97 direct method and refined by full-matrix least-squares on F² to final values of R1 = 0.1155 and wR2 = 0.1018 for all data.

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The crystal structure of a colorless phosphorus ylide, Ph₃PCHCOC₆H₄Cl, was determined by the X-ray diffraction method. All atoms occupy general positions in the monoclinic space group, C2/c, and have the following unit-cell dimensions: a = 16.6184(9)Å, b = 10.9196(6)Å, c = 23.5465(12)Å, β = 100.366(4)°, Z = 8 and V = 4203.2(4)ų.

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The structure of a trinuclear copper(II) complex with 1,1,1-tris(N-salicylideneaminomethyl)ethane ([Cu₃L₂]) of octahedral coordination geometry was determine by X-ray crystallography. [Cu₃L₂] crystallized in a monoclinic system, and was characterized thus: C2/c, a = 18.806(3), b = 12.832(2), c = 20.966(4)Å, β = 117.781(8)°, Z = 4, V = 4476.4(13)ų. The crystal structure was solved by direct methods and refined by full-matrix least squares on F² to final values of R1 = 0.0533.

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Interionic interactions in a crystal of 4,5-diiodo-3-methyl-1-propylimidazolium hexafluorophosphate were investigated. This salt crystallizes in the monoclinic system, space group P2₁/c with cell parameters of a = 11.5373(6), b = 8.6305(5), c = 15.3770(8)Å, β = 107.1410(10)°, V = 1463.12(14)ų, and Z = 4. The crystal structure was solved by a direct method and refined by full-matrix least squares to a final R value of 0.0291 with I > 2σ(I). C-I…F halogen bonding, C-H…F hydrogen bonding and C…F electrostatic interactions were found in this crystal.

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The author line should read
B. B. IVANOVA,^*† T. KOLEV,^* H. Mayer-FIGGE,^** W. S. SHELDRICK,^** and M. SPITELLER^*

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B. B. IVANOVA,^*,**† R. D. NIKOLOVA,^*** S. ZAREVA,^**** H. MAYER-FIGGE,^* W. S. SHELDRICK,^* and M. SPITELLER^*

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Chemical preparation and structural caracterization by X-ray diffraction are given for a new organic cyclohexaphosphate, [o-C₇H₁₀NO]₄Li₂P₆O₁₈·5H₂O. This compound crystallizes in the orthorhombic space group Pna2₁, with unit-cell parameters a = 19.964(3)Å, b = 9.417(4)Å, c = 23.520(4)Å, Z = 4, V = 4421.8(17)ų. Its crystal structure has been determined and refined to a final R = 0.068 and Rw = 0.070 for 5276 independent reflections. The atomic arrangement can be described as a layer organization built by P₆O₁₈ rings, lithium and water molecules. Between these layers, [o-C₇H₁₀NO]⁺ organic cations are located giving rise to a three-dimensional network.

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The compound crystallized in a monoclinic system and was characterized thus: P2₁/n; a = 16.879(5)Å, b = 26.330(5)Å, c = 9.569(5)Å, β = 94.744(5)°, Z = 4, V = 4238.1(3)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R₁ = 0.041 and wR₂ = 0.117. The mixed metal compound consists of a [trans-Pt(η¹-C≅CPy)(PMe₂Ph)₂]-moiety and a cluster [Ru₃(CO)₉], whereby the other 2-ethynylpyridine crosslinks to the platinum site through a nitrogen atom and to the cluster by a perpendicular (η¹:η²:η²)-bond fashion with atomic distances of Ru1-C1 1.951(8)Å, Ru2-C1 2.222(8)Å, Ru3-C1 2.223(9)Å, Ru2-C2 2.264(8)Å, and Ru3-C2 2.252(8)Å, respectively.

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The title compound, phenoxo-bridged dinuclear copper(II) complex with N-salicylidene-2-hydroxy-5-bromobenzylamine (H₂shbb) [Cu₂(shbb)₂(dmso)₂]·2dmso (dmso = dimethyl sulfoxide), was synthesized and the crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the monoclinic space group P2₁/n with a = 16.994(3)Å, b = 8.3932(16)Å, c = 15.755(3)Å, β = 111.547(3)°, V = 2090.2(7)ų, D_x = 1.665 g/cm³, and Z = 2. The R1 and wR2 values are 0.0505 and 0.0649, respectively, for 4759 reflections. The molecule is a phenoxo-bridged dinuclear copper(II) complex having an elongated square-pyramidal coordination geometry with the O₃N basal atoms from the shbb₂^- ligands and the apical O atom from the dmso ligand.

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The title compound, 3-chloro-4-(3,3-dichloroallyloxy)benzenamine, crystallizes in the orthorhombic space group Pbca with the following unit-cell parameters: a = 5.5640(11), b = 14.832(3), c = 26.399(5)Å, V = 2178.6(8)ų. The crystal struture of this compound was solved by direct methods and refined to a final R = 0.051 for 1185 reflections with I > 2σ(I). In the crystal packing, the molecules are linked via N-H…O and N-H…N hydrogen bonds.

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The peptide Boc-Pro-Hyp-Gly-OMe (I) crystallizes in an orthorhombic system, and was characterized thus: P2₁2₁2₁, a = 8.882(1), b = 15.151(2), c = 30.928(4)Å, V = 4162.0(9)ų, Z = 4. The final R value was 0.0454 for measured reflections. Two peptide molecules were found in the asymmetric unit with a somewhat twisted structure. These molecules were arranged antiparallel, creating a sheet-like structure. A down-pucker was observed for Pro residues, but the both up- and down-puckers were observed for the Hyp residues.

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The crystal structure of 2-[1-(2,4-dinitrophenyl)ethyl]-1,10-phenanthroline was determined by X-ray crystallography. The compound crystallizes in a monoclinic system and was characterized thus: P2₁/n, a = 15.477(2), b = 5.1818(6), c = 21.754(2)Å, β = 96.295(3)°, Z = 4, V = 1734.12 ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R = 0.0600.

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The title compound crystallized in the monoclinic space group P2₁/c with cell parameters a = 17.5232(13)Å, b = 7.9269(5)Å, c = 13.6707(9)Å, β = 107.070(2)°, V = 1815.3(2)ų, Z = 4, D_x = 1.516 g/cm³. The structure was refined by full-matrix least-squares procedures to final R₁ = 0.0579 and wR₂ = 0.1620 for 3573 reflections. In the crystal structure of the title compound, weak intermolecular interactions of C3-H3…O4 and C2-H1…O3 link the molecules into zigzag chains along the c-axis.

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The structure of 1-(propa-1,2-dienyl)-1H-benzo[d]imidazole-2-carbaldehyde was determine by X-ray crystallography. The compound crystallized in a monoclinic system, and was characterized as: P2₁/n, a = 3.9124(8), b = 15.082(3), c = 15.407(3)Å, β = 91.784(4)°, Z = 4, V = 908.7(3)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.045 and wR2 = 0.133.

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X-ray structural investigations have been carried out for the title compound, 3-amino-2-benzyl-6-bromo-1,2,4-triazin-5(2H)-one (1-benzyl-5-bromo-6-azaisocytosine), molecular formula C₁₀H₉BrN₄O, which crystallizes in the monoclinic space group P2₁/n with a = 12.3645(1)Å, b = 6.9011(1)Å, c = 14.0685(2)Å, β = 111.947(1)°, V = 1113.45(2)ų and Z = 4, resulting in a density, D_calc, of 1.677 g/cm³. The title compound is linked by extensive intermolecular N-H…N hydrogen bonding [graph set R₂²(8)] and N-H…O hydrogen bonding [graph set C₁¹(6)].

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The title compound is a five-coordinate Na^I-bisazo complex used in imaging industries. This complex crystallizes in a triclinic system, as characterized by the crystallographic parameters: P1, a = 12.1100(8), b = 13.7781(9), c = 14.6695(9)Å, α = 63.125(3), β = 89.298(3), γ = 73.534(3)°, Z = 2, V = 2074.5(2)ų. The structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.1494 and wR2 = 0.4105.

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The structure of 1,4,5,8-tetrapentylanthracene was determined by X-ray crystallography. The compound crystallizes in a triclinic system and was characterized thus: P1, a = 5.350(4), b = 9.580(7), c = 14.946(10)Å, α = 99.685(9), β = 90.243(11), γ = 96.275(15)°, V = 750.4(9)ų, and Z = 1. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0915 with I > 2σ(I). The molecule has a crystallographic center of symmetry, and half of the formula unit is independent. The molecular structure takes a semi-chair form.

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The title compound is a novel yellow pyrazolyl azo pigment used in imaging industries. This compound crystallizes in a triclinic system, as characterized by the following crystallographic parameters: P1, a = 6.7561(12), b = 14.054(2), c = 16.203(3)Å, α = 83.924(6), β = 83.276(7), γ = 79.140(7)°, Z = 2, V = 1495.0(4)ų. The structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.1373 and wR2 = 0.3346.

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The complex [Pt₃Cl₃(μ-SeCH₂CH₂NH₂)₂(PPr₃)₃]Cl was prepared by a reaction between [Pt₂Cl₂(μ-Cl)₂(PPr₃)₂] and NaSeCH₂CH₂NH₂ in an acetone-water mixture. An X-ray structural analysis revealed that selenolate bridges hold three metal square planes that are mutually nearly perpendicular to each other.

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A dinuclear manganese(III) complex, [Mn(L1-Bz)(na)]₂ [H₂L1-Bz = 1-[(2-hydroxymethylphenyl)iminomethyl]-2-naphthol, Hna = o-hydroxynaphthaldehyde], was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in a monoclinic system, spaces group P2₁/n and Z = 4 with cell parameters a = 10.080(4)Å, b = 23.642(8)Å, c = 10.368(4)Å, β = 115.142(5)°, V = 2236.6(14)ų. The dinuclear structure is formed by two μ-hydoroxo bridges with a Mn…Mn separation of 3.1648(14)Å.

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A mixed solution of (Cs_3.5Rb_0.5)[(Se_0.85S_0.15)O₃]₂[Te(OH)₆]₃ (CsRbSSeTe) was synthesized from an aqueous solution of H₆TeO₆, Rb₂SO₄, Rb₂CO₃, Cs₂CO₃, Cs₂SO₄ and H₂SeO₄. The rubidium caesium sulfite selenite tellurate salt crystallizes in the orthorombic system with the Pccn space group. It was analyzed at room temperature using XRD data. The unit cell parameters are a = 19.758(1), b = 9.464(1), c = 14.056(1)Å, Z = 8, V = 2628.22(2)ų, giving D_x = 3.63 g/cm³. The refinement converged into R = 0.039, Rw = 0.040. The main feature of the atomic arrangements is the coexistence of three and different anions (SO₃^2-, SeO₃^2- and TeO₆^6-) in the unit cell, connected by O-H…O hydrogen bonds, which allow construction of the crystal. The structures are formed by planes of octahedral Te(OH)₆. Between these planes, we find mixed planes occupied by trigonal SO₃^2-/SeO₃^2- anions and Cs⁺/Rb⁺ cations.

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The title compound, C₂₀H₁₅N₃, was synthesized and the structure was investigated by X-ray crystallography. The compound crystallizes in the monoclinic crystal class in the space group P2₁/c with cell parameters a = 10.5700(6)Å, b = 12.2810(13)Å, c = 12.1750(13)Å, β = 94.429(7)° and Z = 4.

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The structure of dihydro-1,3,5,5-tetramethyl-2-(1-phenylethylidene)-4,6(1H,5H)-pyrimidinedione (1) was determined by X-ray crystallography. The phenyl group made an angle of 62.2(1)° with the ethylidene group. The dihydropyrimidine ring adopts a boat conformation. An intermolecular C-H…O and π…π interaction was observed in the crystal lattice.

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