Crystal structures of rubidium scandium bis(hydrogenphosphate), RbSc(HPO4)2, and ammonium scandium bis(hydrogenphosphate), NH4Sc(HPO4)2 (original) (raw)
Inorganica Chimica Acta, 1997
The reaction of Rua(OaCCH3)4CI with water in the presence of AgaSO 4 and NH~PF 6 leads to the formation of [Ru 2-(OzCCH3)4(HaO)al(PF~) (1). The subsequent reaction of complex ] with dimethylformamida (DMF) and dimethylanlfoxule (DMSO) results in the formation of [Ru2(OaCCH3)4(DMF)2](PF6) (2); [Rna(OaCCH314(DMF/a](PF6).DMF (aa) aral [Rua(OaCCH3)~-(DMSO)2] (PF6) (3). All complexes were characterized using single crystal X-ray crystallography, IR and UV-Vis spectmscogff, cyclic vultammetry and magnetic susceptibility. The crystallographic data for [Rua(OaCCH3)4(HaO)a] (PF6). 3H20 (la) are as fullow~ nudeclinic, space group C2/e with unit cell dimensions a = 19.552(2). b= 12-853(2/. c= 8.487(2) A. fl= 93.09(2) °, V= 2129.6(61 A3,Z=4. The structure was refined to R = 0.0244 (R~ ~ 0.0266) with 1165 reflections having I> 3o'(1). The Ru-Rn distance is 2,2648(91 A; RwO distances are 2.023(4/, 2,039(3), 2.018(4) and 2.026 A; Ru-O(axial) =2.279(4) A. The relevant data for 2 a~: mthodmmbic, space group P212121 with unit cell dimensions a = 11.704(2), b~ 28.452( 101, c-8.415( 31 A, V-2802(2) A 3, Z-4. The stn.'ctme was reraned to R=0.0597 (wR2 ~0.1520) with 909 reflections having 1>2o-(/). The Ru-Ru distance is 2.262(3) A; Ru-O distances ate 1.999(14), 2.003(13), 2.004(13) and 2.009(13) ~; the Ru~(axial) distances are both 2.22(2) A. The pertinent crystal daul for 2a are: mo~x:tinic, space group P21/c with unit cell dimensions a=8.382(4), b= 11.918(3), c~30.715(5) A, fl=96.84(3) °, V=3046(11 ~3 Z~4. Tic: structure was refined to R=0.0558 (wR2=0.1388) with 1317 reflections having 1>2o'(/). The Ru-Ru distance is 2.265(2) A.; Ru-O distances are 2,021(13), 2.052(13). 2.009(13) and 2.023(14) A; the Ru--O(axial) distances are both 2.229(t4) A. The data for 3 are: tric~idic° space gr~p P~ with ~ni~ ea~ ~ dim~nsi~ns a ~ ~ ~ . 45 ( ~ ) ~ b~ ~ 4. ~ ~3 ( 4 ) ' c ~ 8.3~3 ( 3 ) .A~ a ~ 9~.46( 2 )~ ~ ~ ~ ~.~ 5 ( 41° ~/~ 78.93( 4 ) % V= 1232(1) A 3, Z=2. The structure was refined to R=0.0301 (R~ ~0.0382) with 2758 reflections having 1> 3o'(/}. The Ru--Ru bond distances are 2.274( 1 ) and 2.268( I ) A; Ru-O distances range from 2.017(51 to 2.035(51 ~; the Ru-O(asial) d~tances ate 2.240(5) and 2.243(51 A. Increasing the donor number of the axial ligand manifests only very small changes in Ru-Ru bond length, reducfico and ~'~ (Rua) ~ 7r( RuO, Ru2) transition energy and no changes in/~nimplying only minor perturbation of b'* and ~* offal energies. five) and labile trans axial sites for subsequent linenc chain construction.
Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry, 1973
In a study of the hydrogen-bond system in the alkali hydrogen salts of oxydiacetic acid the crystal and molecular structures of RbHO(CH2COO)2 have been determined from X-ray intensities collected with a four-circle diffractometer. The crystals are tetragonal, space group I2~2d, with a=8.4814 (2), c= 18-0985 (9) A, Z= 8. The structure has been refined to R= 0.028, Rw=0-054. It is built up of infinite chains of oxydiacetate ions linked by short, symmetric hydrogen bonds. The chains are cross-linked by rubidium ions. The hydrogen-oxygen distance in the hydrogen bond is 1.23 A and the oxygen-oxygen distance 2.45 (1) A. The molecular structures of a number of oxydiacetate residues determined in various alkali hydrogen oxydiacetates and tris(oxydiacetato)lanthanoidate(III)complexes by X-ray and neutron single-crystal diffractometry are compared by half-normal probability plots.
Solid State Sciences, 2000
Ammonium and barium cyclotriphosphate monohydrate, BaNH 4 P 3 O 9 ·1H 2 O, was prepared for the first time by using Boullé's process [1] by Durif et al. who reported a complete description of the atomic arrangement. BaNH 4 P 3 O 9 ·1H 2 O is monoclinic P2 1 /n with the following unit-cell dimensions: a=11.70(1)Å, b=12.12(1)Å, c=7.559(5)Å, β=101.05(5) and Z=4. Therefore, some discrepancies appear in the literature and stimulated further investigation of this compound to conclude concerning hydration level and structure. The thermal behavior of BaNH 4 P 3 O 9 ·nH 2 O showed that this cyclotriphosphate is a dihydrate and up to now no other hydrate has been described for this salt. So, the present study reports the chemical preparation, thermal behavior and crystal structure of BaNH 4 P 3 O 9 ·2H 2 O, the first cyclotriphosphate of mixed ammonium-bivalent cations M II with a new general formula M II NH 4 P 3 O 9 ·nH 2 O. Dehydration and decomposition of such cyclotriphosphates lead generally to long-chain polyphosphates, [M II (PO 3 ) 2 ] ∞ which can be used as corrosion inhibitors . The title compound has been studied through the following techniques: X-ray diffraction, IR spectrometry and thermal analyses TGA-DTA coupled. sablanca, Maroc. b Groupe des Matériaux Inorganiques, IPCMS, UMR 7504, 23 rue du Loess, 67037 Strasbourg Cedex, France. Thermal behavior and infrared studies of NiRb 4 (. Synthesis, thermal behavior and crystal structure of SrRbP 3 O 9 ·3H
Journal of …, 1991
acetylacetone, but not in all possible combinations) have been prepared from the corresponding [{LMCl),(p-Cl),] or [LMCl(acac)] and HPRR'. Complexes [LMCl,(HPPh,)] [L = C,Mq; M = Rh (I), Ir (IV), L= p-Cymene; M= Ru (VII)] react with [M'(~OMe)(diolefin)]s (M'= Rh; diolefin = tetrafluorobenxobarrelene (TFB), 1,5-cyclooctadie.ne (COD). M' = Ir; diolefin = COD) to yield diphenylphosphido-bridged complexes of formula [LMCl,(lr_PPh,)M'(diolefin)]. The structure of [(C,Mq)ClRh-(p-Cl)(p-PPh,)Rh(COD)]-$Et,O has been determined by X-ray diffraction methods. The complex consists of two moieties, (C,Me&hCl and Rh(COD), doubly-bridged by a diphenylphosphido group and a chlorine atom. The two rhodium atoms are separated by 3.3657(6) A.
Crystal structure of SrCo4(OH)(PO4)3, a new hydroxyphosphate
Acta Crystallographica Section E Crystallographic Communications
Single crystals of strontium tetracobalt tris(orthophosphate) hydroxide, SrCo4(OH)(PO4)3, were grown serendipitously under hydrothermal conditions at 473 K. The crystal structure consists of undulating chains of edge-sharing [CoO6] octahedra that are linked into (010) layers by common vertices between chains. Adjacent layers are linked along [010] into a framework structure by tetrahedral [CoO4] units and by PO4 tetrahedra. The framework delimits channels extending along [100] in which the eleven-coordinate strontium cations are situated. Bifurcated O—H...O hydrogen bonds of weak strengths consolidate the crystal packing. The title compound was also characterized by infrared spectroscopy.
Synthesis and crystal structure study of RbLaP
Current Chemical Genomics
Many recent studies have been devoted to the cyclophosphates materials, first because they have many interesting properties. For example, luminescence and spectroscopic properties CsPrP 4 O 12 and RbPrP 4 O 12 [1,2] , LiErP 4 O 12 [3] , have been carefully studied and because they can be used in a large number of technological applications such as mini LASER [4-9]. These cyclophosphates contain rings of up to 12 tetrahedrons, but those with three, four (cyclotetraphosphate), and six units are most common and have stoichiometries n n 3 n O P . An X-ray diffraction single crystal study of the monoclinic phase of RbLaP 4 O 12 , which occurs at room temperature, has been performed with the aim of determining the atomic structure. This compound crystallizes in the space group C2/c with unit cell dimensions a= 7.946(6)Å, b= 12.835(6)Å, c= 10.769(10)Å, â= 110.624(7)°, Z= 4 and V= 1027.9(13)Å 3. The refinement converged to R= 0.019 and wR= 0.019 using 6412 independent reflections (I > 2(I)). The P 4 O 12 anion has a twofold symmetry, the La atom is eightfold coordinated. The main characteristic of this atomic arrangement is a stacking of three dimensionally framework delimiting intersecting tunnels in which the Rb + cations are inserted, linked LaO 8 layers parallel to (001) planes connected together by P 4 O 12 groups lying in (010) planes. Infrared and Raman spectrum was investigated at room temperature in the frequencies range, 400-1600 cm-1 , showing some characteristic vibration bands of infinite chain structure of PO 4 tetrahedra linked by bridging oxygen.
Inorganic Chemistry, 1973
A black crystalline complex of stoichiometry Ru2Nl,0,H3,Cl, has been isolated from an ammoniacal solution of Ru(II1) chloride in the presence of air (ruthenium red solution). The crystal and molecular structure of this black complex, di-pamido-bis[tetraammineruthenium(III)J chloride tetrahydrate, [(NH,),Ru(NH,),Ru(NH~)~]C~, * 4H,O, has been determined from three-dimensional X-ray data collected by counter techniques. The structure was refined by full-matrix least-squares methods. The refinement was carried out using 21 14 nonzero reflections for which F2 > o(F2) and assuming anisotropic thermal motion for all nonhydrogen atoms. The least-squares refinement led to a final value of the conventional R factor (on F ) of 0.036. The centrosymmetric cation [(NH3),Ru(NH2)2Ru(NH3)4]4+ features distorted octahedral Ru centers, two amido bridging groups, and a relatively short Ru-Ru distance of 2.625 (1) A. The Ru-NH,-Ru bridging bond angle is acute [81.0 (l)"], suggesting Ru-Ru bonding interaction. The chloride ions and oxygen atoms of the water molecules occupy the "holes" in the crystal. Crystal data are as follows: monoclinic, space group P2,/n; a = 9.686 (1) A, b = 9.872