Table of Contents

Abstract: A new open-framework iron borophosphate, KFe[BP₂O₈(OH)], has been obtained by ionothermal synthesis from KH₂PO₄, FeCl₃∙4H₂O, H₃BO₃ and [C₄mpyr]Br (1-butyl-1-methylpyrrolidinium bromide). Single-crystal X-ray diffraction analysis shows that KFe[BP₂O₈(OH)] (monoclinic, P2₁/c, a = 9.372(2) Å , b = 8.146(2)Å , c = 9.587(2) Å, β = 101.18(3)°, V = 718.0(2)ų and Z = 4) has a three-dimensional (3-D) framework structure composed by {Fe(III)O₅(OH)} octahedra as well as {BO₃(OH)} and {PO₄} tetrahedra. As anionic structural sub-unit, KFe[BP₂O₈(OH)], contains an infinite open-branched {[BP₂O₈(OH)]^4-} chain which is formed by alternating {BO₃(OH)} and {PO₄} tetrahedra. {Fe(III)O₅(OH)} octahedra share common O corners with five phosphate tetrahedra and the OH corner links to the hydrogen borate group to give a 3D framework. The negative charges of the inorganic framework are balanced by K⁺ ions.

Abstract: A carbazole-triazine hybrid was prepared by addition-elimination between carbazole and 2,4,6-trichlorotriazine in the presence of base. The compound shows intensely blue fluorescence both in solution and solid state when irradiated with UV-radiation. The structure of (3) was supported by the spectroscopic data and unambiguously confirmed by the single crystal X-ray diffraction data. It was crystallized in the monoclinic space group C2/c with unit cell dimensions a = 20.280(3), b = 8.0726(14), c = 16.005(3) Å, α = γ = 90°, β = 98.947(3)°, V = 2588.3(8) ų, Z = 8.

Abstract: The title thiourea was synthesized by reaction of 3,4,5-trimethoxybenzoyl isothiocyante with 3-fluoroaniline. The 3,4,5-trimethoxybenzoyl isothiocyante was produced in situ by reaction of 3,4,5-trimethoxybenzoyl chloride with ammonium thiocyanate in dry acetonitrile. The structure was confirmed by the spectroscopic, elemental analysis and single crystal X-ray diffraction data. It crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a = 13.0966(9), b = 16.6460(13), c = 7.8448(5), β = 106.721(5)°, V 1637.9(2) ų, Z = 4.

Abstract: The reduction of hafnium tetraiodide, HfI₄, with aluminum at 600 °C or 850 °C in the presence of a NaI flux resulted in black single crystals of Hf_0.86(1)I₃. This composition corresponds well to the upper end of the non-stoichiometry range 0.89 ≤ x ≤ 1.00 previously reported for Hf_xI₃. The crystal structure (a = 1250.3(2), c = 1999.6(3) pm, R-3m, Z = 18) is made up of hexagonal closest packed layers of iodide ions. One third of the octahedral holes would be filled as in TiI₃ or ZrI₃ if it were Hf_1.00I₃. In Hf_0.86(1)I₃, one out of six octahedral holes along [001] are, however, only occupied by 16%. In contrast to TiI₃-I and ZrI₃, one striking structural feature is in the formation of linear hafnium trimers with identical Hf―Hf distances of 318.3(2) pm rather than the formation of dimers. These may be associated with Hf―Hf bonding although only 2.64 electrons are available for one Hf_5.16I₁₈ column.

Abstract: The syntheses and single-crystal structures of Mo(CO)₃(phen)(dipy) (1), Mo(CO)₃(biquin)(dipy) (2) and Mo(CO)₃(dpme)(dipy) (3), (phen = 1,10-phenanthroline, C₁₂H₈N₂; dipy = 2,2'-dipyridylamine, C₁₀H₉N₃; biquin = 2,2'-biquinoline, C₁₈H₁₂N₂; dpme = 2,2'-dipyridylmethane, C₁₁H₁₀N₂) are described. In each case, distorted fac-MoC₃N₃ octahedral coordination geometries arise for the metal atoms. Short intramolecular N–H…C interactions from the dipy N–H group to a carbonyl carbon atom occur in each structure. Crystal data: 1 (C₂₅H₁₇MoN₅O₃), M_r = 531.38, monoclinic, P2₁/n (No. 14), Z = 4, a = 11.0965 (5) Å, b = 13.0586 (6) Å, c = 16.6138 (8) Å, b = 108.324 (1)°, V = 2285.31 (18) ų, R(F) = 0.035, wR(F²) = 0.070. 2 (C₃₁H₂₁MoN₅O₃), M_r = 607.47, monoclinic, P2₁/n (No. 14), Z = 4, a = 11.4788 (6) Å, b = 19.073 (1) Å, c = 11.9881 (6) Å, b = 95.179 (1)°, V = 2613.9 (2) ų, R(F) = 0.030, wR(F²) = 0.076. 3 (C₂₄H₁₉MoN₅O₃), M_r = 521.38, monoclinic, P2₁/n (No. 14), Z = 4, a = 8.4222 (3) Å, b = 21.5966 (9) Å, c = 12.5011 (5) Å, b = 94.065 (1)°, V = 2268.12 (15) ų, R(F) = 0.025, wR(F²) = 0.065.

Abstract: The syntheses and single-crystal structures of Ba₂(C₂O₄)(H₂PO₃)₂ (1) and C₂H₁₀N₂·Ba(H₂O)₂(HC₂O₄)₄ (2) are described. Compound 1 is a three-dimensional mixed-anion framework containing BaO₉ coordination polyhedra, which approximate to monocapped square anti-prisms: the connectivity of the BaO₉ units via edges and triangular faces leads to a sheet structure. The oxalate ion in 1 is substantially twisted about its C–C bond [dihedral angle between the CO₂ groups = 33.8 (3)°]. Compound 2 is a molecular salt containing ethylenediammonium dications and [Ba(HC₂O₄)₄(H₂O)₂]^2– dianions, which are linked by O–HLO and N–HLO hydrogen bonds. The BaO₁₀ coordination polyhedron can be described as a distorted pentagonal anti-prism. Crystal data: 1 (C₂H₄Ba₂O₁₀P₂), M_r = 524.68, monoclinic, C2/c (No. 15), Z = 4, a = 12.3829 (3) Å, b = 7.9124 (2) Å, c = 11.0858 (3) Å, b = 114.788 (2)°, V = 986.10 (4) ų, R(F) = 0.016, wR(F²) = 0.040. 2 (C₁₀H₁₈BaN₂O₁₀), M_r = 591.60, monoclinic, C2/m (No. 12), Z = 2, a = 12.7393 (7) Å, b = 13.0111 (7) Å, c = 5.6050 (3) Å, b = 104.208 (4)°, V = 900.62 (8) ų, R(F) = 0.027, wR(F²) = 0.054.

Abstract: The syntheses and crystal structures of benzenesulfonylamino-3-(4-benzenesulfonyloxy-phenyl)-propionic acid (1) and 2-(toluene-4-sulfonylamino)-3-[4-(toluene-4-sulponyloxy)-phenyl]-propionic acid (2) are described. The L-tyrosine cores of the molecules show significant conformational differences. In 1, both organic molecules show intramolecular aromatic π–π stacking and in 2 a very short intermolecular C^α–H···O interaction is seen. The structures of 1 and 2 are compared with those of related materials. Crystal data: 1₂·H₂O·MeOH [2(C₂₁H₁₉NO7S₂)·H₂O·CH₄O], M_r = 973.04, monoclinic, P2₁ (No. 4), a = 8.0078 (4) Å, b = 34.0704 (16) Å, c = 8.5506 (3) Å, β = 94.239 (3)°, V = 2326.47 (18) ų, Z = 2, T = 296 K, R(F) = 0.062, wR(F²) = 0.157, 2·H₂O (C₂₃H₂₅NO7S₂·H₂O), M_r = 507.56, monoclinic, P2₁ (No. 4), a = 5.7171 (7) Å, b = 24.359 (3) Å, c = 9.1043 (10) Å, β = 104.563 (6)°, V = 1227.2 (2) ų, Z = 2, T = 296 K, R(F) = 0.055, wR(F²) = 0.092.