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10 citations found for Otto, H.H.
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crystal data
Cs2[Pd(CN)4].H2O and Cs2[Ni(CN)4].H2O were found to be isotypic with the known hexagonal Pt compound which shows an unusual helical chain of six [Pt(CN)4]2- groups in the unit cell, space group P61 or P65. The crystal data are a = 9.559 (2) and c = 19.308 (4) Å, Dm = 2.87 (4), Dx = 2.912 Mg m-3 for the Ni compound, and a = 9.704 (2), c = 19.388 (4) Å, Dm = 3.12 (4), Dx = 3.115 Mg m-3 for the Pd compound. X-ray powder data are given.
crystal data
Completely transparent and colourless single crystals of PbGe3O7 were grown from a melt of composition PbO.2GeO2 at 1040 K by spontaneous crystallization. The compound melts incongruently at 1070 K. The unit cell is orthorhombic with lattice constants a = 5.270 (2), b = 14.088 (4), c = 16.054 (4) Å; D293 = 5.94 (4), Dx = 5.985 g cm−3 for Z = 8. The probable space group is Pcab (D152h). A reported phase of composition PbGe205 is shown to be a mixture of PbGe3O7 and α-PbGeO3. X-ray powder data are given.
crystal data
Single crystals of Pb3Bi2[□|(GeO4)3], a new apatite-like compound with space group P63/m or P63, were grown from the melt. The unit-cell parameters are a = 10.034 (1) and c = 7.267 (2) Å, Z = 2, Dm = 7.51 and Dx = 7.60 g cm−3. Indexed powder data are given. The possibility of a ferroic phase transformation is discussed.
crystal data
Transparent and light brownish single crystals of Pb5GeO7 were grown from a melt of composition 4.8PbO.GeO2 by spontaneous crystallization. The compound melts incongruently at 1014 K. The unit cell is orthorhombic with lattice constants a = 9.296 (2), b = 11.546 (2), c = 17.298 (5) Å; Dm (293 K) = 8.63 (4), Dx = 8.734 Mg m-3 for Z = 8. The space group is Pbca. Indexed X-ray powder data are given.
crystal data
Trilling crystals of PbGe[Ge3O9](h) were grown from the melt by spontaneous crystallization. The crystals develop pseudo-trigonal-prismatic habit. The unit cell is monoclinic but pseudo-rhombohedral. The probable space groups are C2/m, C2 or Cm. The lattice constants of the reduced monoclinic unit cell are a = 7.331 (7), b = 11.455 (3), c = 6.831 (6) Å, β = 141.97 (13)°. Dx = 6.029 Mg m-3 for Z = 2 formula units. The lattice constants of the pseudo-rhombohedral setting are a1 = a2 = 6.800 (6), a3 = 6.831 (6) Å, = β = 115.13 (19), γ = 114.76 (18)° and Z = 1. X-ray powder data are given. Improved crystal data of PbGe[Ge3O9](t) are also given.
short communications
Transparent yellow-greenish single crystals of Pb6GeO8 were obtained by spontaneous crystallization from a melt with a molar ratio of PbO:GeO2 = 4.7:1. The compound is monoclinic, probable space group P21/a, a = 52.665 (12), b = 15.063 (4), c = 23.949 (6) Å and β = 111.03 (5)°; Dm(293 K) = 8.65 (3), Dx = 8.653 Mg m−3 for Z = 64 formula units. Pb11Ge3O17 was synthesized by sintering high-purity oxides PbO and GeO2 of molar ratio 3.69:1 at 990 K. The compound is also monoclinic, probable space groups C2/c or Cc, a = 25.117 (5), b = 15.440 (2), c = 45.529 (13) Å and β = 103.20 (4)°; Dm(293 K) = 8.55 (2), Dx = 8.560 Mg m−3 for Z = 32.
crystal data
Metastable barysilite-like Pb3[Ge2O7] was obtained from the melt at a sufficiently high cooling rate together with stable Pb5Ge3O11, α-PbGeO3, and a homologous series of other metastable lead germanates. The crystal data derived from an indexed powder diagram are a = 10.2960(6), c = 39.805(4) Å, space group R
c, Dm = 7.18, and Dx = 7.188 Mg m−3 for Z = 18. The JCPDS Diffraction File No. for Pb3[Ge2O7] is 33-1487.
c, Dm = 7.18, and Dx = 7.188 Mg m−3 for Z = 18. The JCPDS Diffraction File No. for Pb3[Ge2O7] is 33-1487.laboratory notes
A double-radius Guinier diffractometer that uses Mo Kα 1 radiation and a curved imaging-plate detector is recommended as a competitive in-house apparatus for powder measurements of high resolution and accuracy.
research papers
The construction of a double-radius Gandolfi X-ray camera for the fast generation of well resolved powder-like diffraction patterns of very small single crystals is presented.
organic compounds
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The title nitrothiophene compound, C13H9N3O6S2, crystallizes with two independent molecules in the asymmetric unit; the molecular structure of each is stabilized by an intramolecular N—H
O hydrogen bond. The two molecules adopt flattened but slightly different conformations, viz. the dihedral angle between the thiophene ring and the essentailly planar 1,2-benzisothiazole fragment (r.m.s. deviations = 0.0227 and 0.0108 Å, respectively) is 15.62 (11)° in one molecule and 5.46 (11)° in the other. In the crystal, molecules are arranged into layers parallel to (-111) with weak Car—HO interactions formed within the layer. N—HO hydrogen bonds also occur. There are π–π stacking interactions between the molecules in neighbouring layers, the distance between the centroids of the 1,2-benzisothiazole benzene rings being 3.8660 (16) Å. Moreover, dipolar S=OC=O interactions with an OC distance of 2.893 (3) Å are observed between the symmetry-independent molecules in different layers. The title compound showed weak inhibition of HLE (human leukocyte elastase).
O hydrogen bond. The two molecules adopt flattened but slightly different conformations, viz. the dihedral angle between the thiophene ring and the essentailly planar 1,2-benzisothiazole fragment (r.m.s. deviations = 0.0227 and 0.0108 Å, respectively) is 15.62 (11)° in one molecule and 5.46 (11)° in the other. In the crystal, molecules are arranged into layers parallel to (-111) with weak Car—HO interactions formed within the layer. N—HO hydrogen bonds also occur. There are π–π stacking interactions between the molecules in neighbouring layers, the distance between the centroids of the 1,2-benzisothiazole benzene rings being 3.8660 (16) Å. Moreover, dipolar S=OC=O interactions with an OC distance of 2.893 (3) Å are observed between the symmetry-independent molecules in different layers. The title compound showed weak inhibition of HLE (human leukocyte elastase).
