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10 citations found for Otto, H.

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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.

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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.

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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.

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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.

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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.

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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.

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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{\bar 3}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.

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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.

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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.

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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—H...O inter­actions formed within the layer. N—H...O 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=O...C=O inter­actions with an O...C 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).

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