Crystal Structure of Hexamine Cyclotriphosphazene, P3N3(NH2)6 In the presence of KNH2 hexamine cyclotriphosphazene semi ammoniate (molar ratio 12:1) in NH3 gives crystals of solvent free P3N3(NH2)6 within 5 d at 130°C and p(NH3) = 110 bar. The structure was solved by X-rax methods: P3N3(NH2)6: P21/c, Z = 4, a = 10.889(6) Å, b = 5.9531(6) Å, c = 13.744(8) Å, β = 97.83(3)°, Z(Fo) = 1 721 with (Fo)2 ≥ 3σ(Fo)2, Z(var.) = 157, R/Rw = 0,036/0,041 The structure contains columns of molecules P3N3(NH2)6 all in the same orientation. The six-membered rings within one molecule have boat conformation. The columns are stacked together in a way that one is surrounded by four others shifted by half a lattice constant in direction [010]. Strong hydrogen bridge-bonds N? H…?N connect molecules within the columns and between them. 相似文献
A new perchlorate salt of melem (2,6,10‐triamino‐s‐heptazine, C6N7(NH2)3) was obtained from an aqueous solution of HClO4 at lower concentration than the ones reported for the synthesis of melemium perchlorate monohydrate (HC6N7(NH2)3)ClO4·H2O. The new salt was identified as melemium melem perchlorate (HC6N7(NH2)3)ClO4·C6N7(NH2)3 representing a melem adduct of water free melemium perchlorate. The crystal structure was solved by single‐crystal X‐ray methods ( , no. 2, Z = 2, a = 892.1(2), b = 992.7(2), c = 1201.5(2) pm, α = 112.30(3), β = 96.96(3), γ = 95.38(3)°, V = 965.8(4)·106 pm3, 4340 data, 387 parameters, R1 = 0.039). Melemium melem perchlorate crystallizes in a layer‐like structure containing both protonated HC6N7(NH2)3 and non protonated C6N7(NH2)3 moieties in the coplanar layers as well as perchlorate ions between them, all of which being interconnected by hydrogen bonds. Vibrational spectroscopic investigations (FTIR and Raman) of the salt were conducted. 相似文献
On the Crystal Structure of Melem C6N7(NH2)3 Single crystals of melem ( 1 ) were grown from both DMSO‐solutions and the gas phase. The structure of melem ( 1 ) was solved by single‐crystal X‐ray diffraction (P21/c, Z = 4, a = 741.66(15), b = 862.28(17), c = 1335.9(3) pm, β = 99.91(3)° R1 = 0.037 for 1098 reflections). The structure determination by X‐ray powder diffraction, which has been previously conducted, is in agreement with our data. The increased quality of the structural information allows for a more detailed understanding of the hydrogen bonding network. 相似文献
Synthesis and Crystal Structure of Na10[P4(NH)6N4](NH2)6(NH3)0.5 with an Adamantane-like Anion [P4(NH)6N4]4? Crystals of Na10[P4(NH)6N4](NH2)6(NH3)0.5 were obtained by the reaction of P3N5 with NaNH2 (molar ratio 1:20) within 5 d at 600°C in autoclaves. The following data characterize X-ray investigations: Fm3 m, Z = 8, a = 15.423(2) Å, Z(F) = 261 with F ≥ 3 σ(F) Z(Variables) = 27, R/Rw = 0.086/0.089 The compound contains the hitherto unknown anion [P4(NH)6N4]4?, which resembles adamantane. The total structure can be described as follows: The centers of gravity of units of [Na8(NH2)6(NH3)]2+ – 8Na+ on the corners of a cube, 6NH2? on the ones of an inscribed octahedron with NH3 in the center – follow the motif of a cubic-closest packed arrangement. Units of [Na12(NH2)6]6+ – 12Na+ on the corners of a cuboctahedron and 6NH2? on the ones of an inscribed octahedron – occupy all octahedral and those of [P4(NH)6N4]4? all tetrahedral sites. 相似文献
A New Double Salt, (NH4)2SiF6 · NH4NO3. From a aqueous solutions of (NH4)2SiF6 and NH4NO3 crystallizes by cooling to room-temperature a new double-salt of the composition (NH4)2SiF6 · NH4NO3. Its hexagonal unit containing two molecules has the dimensions: a0 = 5.868, c0 = 14.799 Å. 相似文献
Preparation and Crystal Structure of [Co(NH3)6]2P4O13 7·5H2O Single crystals of [Co(NH3)6]P4O13 · 5 H2O were obtained by diffusion controlled growth. To this end sodium polytetraphosphate was prepared by column chromatography and allowed to react with [Co(NH3)6]Cl3. The compound [Co(NH3)6]2P4O13 · 5 H2O contains the novel isolated polytetraphosphate anion. The expected systematic variation in bond length in the P? O? P bridges of the poly tetraphosphate anion was verified. The conformation of the anion is discussed. 相似文献
Metal Sulphur Nitrogen Compounds. 17. Compounds HgN2S · NH3 and Hg(NH3)2I2 · S4N4 The crystal and molecular structures of the known compounds HgN2S · NH3 and of the new inclusion compound 2Hg(NH3)2I2 · S4N4 are reported. HgN2S · NH3 is orthorhombic, space group Pbca with a = 5.548, b = 10.158, c = 14.919 Å, Z = 8. In the dimeric molecules two Hg atoms are bridged to form eight-membered rings . In addition, each Hg is coordinated by an NH3 molecule and by an N atom of an adjacent ring. This results in a two-dimensional network. 2Hg(NH3)2I2 · S4N4 is tetragonal, space group P42/nmc, a = 8.948, c = 13.188 Å, Z = 2. It is an inclusion compound with S4N4 molecules in the holes of the lattice of the large Hg(NH3)2I2 tetrahedra. 相似文献
A Comparison of the Crystal Structures of the Tetraammoniates of Lithium Halides, LiBr·4NH3 and LiI·4NH3, with the Structure of Tetramethylammonium Iodide, N(CH3)4I Crystals of the tetraammoniates of LiBr and LiI sufficient in size for X‐ray structure determinations were obtained by slow evaporation of NH3 at room temperature from a clear solution of the halides in liquid ammonia. The compounds crystallize in the space group Pnma (No. 62) with four formula units in the unit cell: LiBr·4NH3: a = 11.947(5)Å, b = 7.047(4)Å, c = 9.472(3)Å LiI·4NH3: a = 12.646(3)Å, b = 7.302 (1)Å, c = 9.790(2)Å For N(CH3)4I the structure was now successfully solved including the hydrogen positions of the methyl groups. N(CH3)4I: P4/nmm (No. 129), Z = 2, a = 7.948(1)Å, c = 5.738(1)Å The ammoniates of LiBr and LiI crystallize isotypic in a strongly distorted arrangement of the CsCl motif. Even N(CH3)4I has an CsCl‐like structure. Both structure types differ mainly in their orientation of the [Li(NH3)4]+ — resp. [N(CH3)4]+ — cations with respect to the surrounding “cube” of anions. 相似文献
Te(OH)6 · 2Na3P3O9 · 6H2O, is hexagonal (P63/m) with a = 11,67(1), c = 12,12(1) Å, Z = 2 and Dx = 2,225 g/cm3. Te(OH)6 · K3P3O9 · 2H2O, is monoklin (P21/c) with a = 19,61(5), b = 7,456(1), c = 14,84(6) Å, = 108,01(4), Z = 4 and Dx = 2,506 g/cm3. Both compounds are the first examples of phosphate tellurates in which the anion phosphate is condensed to the ring anion P3O9. As in phosphate tellurates already described the phosphate groups are independent of the TeO6 octahedra. 相似文献
The crystal structure of cadmium copper hydroxide nitrate, CdCu3 (OH)6 (NO3)2 · H2O, has been determined from three dimensional single crystal X-ray data. One single elementary cell of the compound has to be of triclinic symmetry, but as either the crystal is built up from such triclinic domains grown together regularly at angles of 120 degrees, or the nitrate groups of the whole crystal are distributed statistically over three possible orientations standing at 120 degree angles respectively to each other, the structure can also be described in the hexagonal system: a = 6.522 ± 0.005 Å, c = 7.012 ± 0.006 Å, space group D – P 3 m 1, cell content one formula unit. Mixed layers (00.1) of Cu and Cd atoms are embedded between layers consisting of the OH groups and one oxygen atom per nitrate group. The nitrate groups extend with their trigonal plane nearly perpendicular to the layers (00.1) and connect them by hydrogen bridges between the remaining two oxygen atoms and OH groups of the next layer. The Cd atoms are coordinated octahedrally by six equidistant OH groups, and the Cu atoms have a strongly distorted octahedral (4 + 2) coordination with four OH groups and two nitrate oxygens. Thermogravimetric measurements allowed to distinguish the crystal water molecule from variable amounts of excess water. The hydrogen bonds between OH groups and nitrate oxygen atoms and the deformation of the nitrate groups were confirmed by infrared spectra. 相似文献
Synthesis and Crystal Structure of a Cesium-tetraimidophosphate-diamide, Cs5[P(NH)4](NH2)2 = Cs3[P(NH)4] · 2 CsNH2 Well crystallized Cesium-tetraimidophosphate-diamide is obtained by the reaction of CsNH2 with P3N5 in autoclaves at 673 K within three days. X-ray single crystal investigations led to the following data
Crystal Structure of Na5P3O10 · 6 H2O Na5P3O10 · 6 H2O crystallizes triclinic in P1 with a = 1 037.0(2), b = 984.8(4), c = 761.5(3) pm; α = 92.24(7)°, β = 94.55(9), γ = 90.87(6)°; Z = 2. The structure has been determined from fourcycle diffractometer data (2 089 independent reflections, R = 0.053). All hydrogen positions have been taken from a weighted difference-fourier-syntheses. Na5P3O10 · 6 H2O forms colorless, plate-like crystals, which are twinned systematically parallel (001) and can be divided mechanically into single-crystalline portions. 相似文献
Synthesis and Crystal Structure of Rb8[P4N6(NH)4](NH2)2 with the Adamantane-like Anion [P4N6(NH)4]6? RbNH2 reacts with P3N5 (molar ratio 6:1) at 400°C within 5 d to colourless Rb8[P4N6(NH)4](NH2)2. Suitable crystals for a X-ray structure determination were obtained: The compound contains adamantane-like molecular anions [P4N6(NH)4]6?. Their centres of gravity are arranged in a distorted hexagonal primitive array. All trigonal prisms of this array contain one amide ion. Rubidium ions connect the anions irregularly. 相似文献
Crystal Growth and Structure of CoSO4 · Pyrazine · 6 H2O (I) and (CoSO4)2 · Pyrazine · 12 H2O (II) Single crystals of μ-pyrazino-bis[pentaquacobalt(II)]-sulfate-dihydrate CoSO4(pz) · 6 H2O and Tetraqua-μ-pyrazino-cobalt(II)sulfate-dihydrate (CoSO4)2(pz) · 12 H2O were grown by using gel methods and investigated by X-ray analysis. CoSO4(pz) · 6 H2O (I) shows monoclinic symmetry, space group C2/c; a = 1006.4(4) pm, b = 1026.9(4) pm, c = 1261.5(2) pm; β = 104.01(4)°; Z = 4. (CoSO4)2(pz) · 12 H2O (II) shows orthorhombic symmetry, space group Pbam; a = 1262.3(4) pm, b = 1231.3(4) pm, c = 684.1(2) pm; Z = 2. CoSO4 and Pyrazine crystallize in a polymeric (I) as well as in a dimeric (II) compound. In the polymeric compound the molecules are bonded by pyrazine to form alternating linear chains. The dimer is a dinuclear complex with a bridging pyrazine molecule. 相似文献
