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1.
M. Férid D. Ben Hassen-Chehimi N. Kbir-Ariguib M. Trabelsi-Ayedi 《Journal of Thermal Analysis and Calorimetry》1994,42(5):913-918
The NaPO3?Pr(PO3)3 system was studied by microdifferential thermal analysis (DTA), IR and X-ray diffraction spectroscopies. The only new compound observed in the system is NaPr(PO3)4, which melts incongruently at 1149 K. A eutectic appears at 5% Pr(PO3)3 at 901 K. The new compound NaPr(PO3)4 was characterized by means of powder X-ray diffraction and IR absorption spectroscopy. NaPr(PO3)4 is a NaLa(PO3)4 isotype; it crystallizes in the monoclinic system P21/c witha=12.328(7),b=13.130(5),c=7.231(5) Å, β=126°, 18(5),Z=4,V=945 ?3. 相似文献
2.
Etude de phosphates condenses diagramme d’equilibre du systeme AgPO3−Pr(PO3)3 Données sur AgPr(PO3)4
D. Ben Hassen-Chehimi M. Trabelsi-Ayedi 《Journal of Thermal Analysis and Calorimetry》1995,44(4):961-967
The AgPO3?Pr(PO3)3 system has been studied for the first time by differential thermal analysis, X-ray diffraction and IR spectroscopy. The system shows one compound AgPr(PO3)4 which melts in a peritectic decomposition at 1069 K. An eutectic appears at 761 K. AgPr(PO3)4 belongs to the monoclinic system with space group P2t/c,Z=4. The parameters of the unit cell are:a=12.000(9),b=13.177(4),c=7.046(5) Å and β=123o,81(6),Z=4. Its IR absorption spectrum is typical of chain phosphates. 相似文献
3.
Synthesis and Crystal Structure of K2(HSO4)(H2PO4), K4(HSO4)3(H2PO4), and Na(HSO4)(H3PO4) Mixed hydrogen sulfate phosphates K2(HSO4)(H2PO4), K4(HSO4)3(H2PO4) and Na(HSO4)(H3PO4) were synthesized and characterized by X‐ray single crystal analysis. In case of K2(HSO4)(H2PO4) neutron powder diffraction was used additionally. For this compound an unknown supercell was found. According to X‐ray crystal structure analysis, the compounds have the following crystal data: K2(HSO4)(H2PO4) (T = 298 K), monoclinic, space group P 21/c, a = 11.150(4) Å, b = 7.371(2) Å, c = 9.436(3) Å, β = 92.29(3)°, V = 774.9(4) Å3, Z = 4, R1 = 0.039; K4(HSO4)3(H2PO4) (T = 298 K), triclinic, space group P 1, a = 7.217(8) Å, b = 7.521(9) Å, c = 7.574(8) Å, α = 71.52(1)°, β = 88.28(1)°, γ = 86.20(1)°, V = 389.1(8)Å3, Z = 1, R1 = 0.031; Na(HSO4)(H3PO4) (T = 298 K), monoclinic, space group P 21, a = 5.449(1) Å, b = 6.832(1) Å, c = 8.718(2) Å, β = 95.88(3)°, V = 322.8(1) Å3, Z = 2, R1 = 0,032. The metal atoms are coordinated by 8 or 9 oxygen atoms. The structure of K2(HSO4)(H2PO4) is characterized by hydrogen bonded chains of mixed HnS/PO4– tetrahedra. In the structure of K4(HSO4)3(H2PO4), there are dimers of HnS/PO4– tetrahedra, which are further connected to chains. Additional HSO4– tetrahedra are linked to these chains. In the structure of Na(HSO4)(H3PO4) the HSO4– tetrahedra and H3PO4 molecules form layers by hydrogen bonds. 相似文献
4.
The previously unknown binary system KPO3-Y(PO3)3 has been examined by thermal, X-ray and microscopic analysis and its phase diagram provided. The existence of the compound KY(PO3)4 has been confirmed. Its melting point (700°, incongruent) and basic parameters of the unit cell (monoclinic system, space group P21/n, lattice parameters: a=7.36, b=8.36, c=14.39 Å, =96.1°) have been determined. The new, so far unknown, compound has been discovered and assigned the formula K2Y(PO3)5. It has been found that it forms peritectoidally (in the solid phase) at 642°.
This paper was included in the CPBP-01.18 problem and was financially supported by the Ministry of National Education. 相似文献
Zusammenfassung Das zuvor unbekannte binäre System KPO3-Y(PO3)3 wurde mittels Thermo-, Röntgendiffraktions- und mikroskopischer Analyse untersucht und das Phasendiagramm aufgestellt. Die Existenz der Verbindung KY(PO3)4 wurde dabei bekräftigt. Ihr Schmelzpunkt (700°, inkongruent) und die grundlegenden Parameter der Elementarzellen (monoklines System, Raumgruppe P21/n, Gitterkonstanten: a=7.36, b=8.36, c=14.39 Å, =96.1°) wurden ermittelt. Weiterhin wurde eine neue, bislang unbekannte Verbindung mit der Formel K2Y(PO3)5 entdeckt. Sie verfügt (in fester Phase) über ein Peritektikum bei 642°.
This paper was included in the CPBP-01.18 problem and was financially supported by the Ministry of National Education. 相似文献
5.
The new ternary calcium indium(III) phosphate CaIn2(PO4)2(HPO4) with mixed octahedral-tetrahedral framework was synthesized through hydrothermal reaction of stoichiometric amounts of CaO and InCl3 with excess of H3PO4 and H2O at pH = 1. Single crystal x-ray diffraction studies show the compound to crystallize in monoclinic symmetry, space group P21/n (#14) with a = 657.08(6), b = 2023.7(2), c = 665.72(7) pm, β = 91.20(1)°, Z = 4 and R = 0.043. The framework is built up of dimers of edge-sharing InO6 octahedra forming In2O10 units sharing all their OXO ligands with PO4 tetrahedra, and HPO4 groups. 相似文献
6.
Single crystals of Ga(PO3)3 were grown in polyphosphoric acid melts by heating a mixture of Ga2O3 and H3PO4 (350 °C, 7 d). The compound belongs to the series of metaphosphates MIII(PO3)3 forming the C-type structure (monclinic, Cc, Z = 12, a = 13.0058(21), b = 18.915(3), c = 9.3105(15) Å, β = 126.900(11), 5348 independent reflections (I > 0); 354 variables; 39 atoms in asymetric unit; R1 = 0.048, wR2 = 0.1034). The structure is characterized by a superstructure with tripled monoclinic b-axis. Three crystallographically independent GaIIIO6 octahedra (d¯(Ga–O) = 1.950 Å) are linked by 1∞(PO3)– chains. 相似文献
7.
Contributions on Crystal Chemistry and Thermal Behaviour of Anhydrous Phosphates. XXXII. New Orthophosphates of Divalent Chromium — Mg3Cr3(PO4)4, Mg3, 75Cr2, 25(PO4)4, Ca3Cr3(PO4)4 and Ca2, 00Cr4, 00(PO4)4 Solid state reactions via the gas phase led in the systems A3(PO4)2 / Cr3(PO4)2 (A = Mg, Ca) to the four new compounds Mg3Cr3(PO4)4 ( A ), Mg3.75Cr2.25(PO4)4 ( B ), Ca3Cr3(PO4)4 ( C ), and Ca2.00Cr4.00(PO4)4 ( D ). These were characterized by single crystal structure investigations [( A ): P21/n, Z = 1, a = 4.863(2) Å, b = 9.507(4) Å, c = 6.439(2) Å, β = 91.13(6)°, 1855 independend reflections, 63 parameters, R1 = 0.035, wR2 = 0.083; ( B ): P21/a, Z = 2, a = 6.427(2) Å, b = 9.363(2) Å, c = 10.051(3) Å, β = 106.16(3)°, 1687 indep. refl., 121 param., R1 = 0.032, wR2 = 0.085; ( C ): P‐1, Z = 2, a = 8.961(1) Å, b = 8.994(1) Å, c = 9.881(1) Å, α = 104.96(2)°, β = 106.03(2)°, γ = 110.19(2)°, 2908 indep. refl., 235 param., R1 = 0.036, wR2 = 0.111; ( D ): C2/c, Z = 4, a = 17.511(2) Å, b = 4.9933(6) Å, c = 16.825(2) Å, β = 117.95(1)°, 1506 indep. refl., 121 param., R1 = 0.034, wR2 = 0.098]. The crystal structures contain divalent chromium on various crystallographic sites, each showing a (4+n)‐coordination (n = 1, 2, 3). For the magnesium compounds and Ca2.00Cr4.00(PO4)4 a disorder of the divalent cations Mg2+/Cr2+ or Ca2+/Cr2+ is observed. Mg3.75Cr2.25(PO4)4 adopts a new structure type, while Mg3Cr3(PO4)4 is isotypic to Mg3(PO4)2. Ca3Cr3(PO4)4 and Ca2.00Cr4.00(PO4) 4 are structurally very closely related and belong to the Ca3Cu3(PO4)4‐structure family. The orthophosphate Ca9Cr(PO4)7, containing trivalent chromium, has been obtained besides C and D . 相似文献
8.
H. Dhaouadi H. Marouani M. Rzaigui A. Madani 《Phosphorus, sulfur, and silicon and the related elements》2013,188(8):1801-1814
Chemical preparation, crystal structure, thermogravimetric and differential analysis, solid state 31P MAS NMR characterization, and IR spectroscopic investigations are given for a new organic cation dihydrogenmonophosphate, (2-CH3OC6H4CH2NH3)H2PO4. This compound is monoclinic C2/c, with unit cell parameters a = 27.740(8), b = 4.827(2), c = 16.435(3) Å, β = 93.79(2)°, V = 2196 (1) Å3, Z = 8, and ρ = 1.422 g · cm?3. The crystal structure has been determined and refined to R = 0.046 (Rw = 0.056), using 1,746 independent reflections with I > 3σ (I). Its atomic arrangement can be described by infinite polyanions [H2PO4] n n ?, organized in ribbons alternating with organic cations. Strong hydrogen bonds connect the different components. Electrical conductivity measurements show that the [2-CH3OC6H4CH2NH3]H2PO4 has a low ionic conductivity value at 403 K. 相似文献
9.
Contributions on Crystal Structures and Thermal Behaviour of Anhydrous Phosphates. XXIII. Preparation, Crystal Structure, and Thermal Behaviour of the Mercury(I) Phosphates α-(Hg2)3(PO4)2, β-(Hg2)3(PO4)2, and (Hg2)2P2O7 Light-yellow single crystals of (Hg2)2P2O7 have been obtained via chemical vapour transport in a temperature gradient (500 °C → 450 °C, 23 d) using Hg2Cl2 as transport agent. Characteristic feature of the crystal structure (P2/n, Z = 2, a = 9,186(1), b = 4,902(1), c = 9,484(1) Å, β = 98,82(2)°, 1228 independent of 5004 reflections, R(F) = 0,066 for 61 variables, 7 atoms in the asymmetric unit) are Hg22+-units with d(Hg1–Hg1) = 2,508 Å and d(Hg2–Hg2) = 2,519 Å. The dumbbells Hg22+ are coordinated by oxygen, thus forming polyhedra [(Hg12)O4] and [(Hg22)O6]. These polyhedra share some oxygen atoms. In addition they are linked by the diphosphate anion P2O74– (ecliptic conformation; ∠(P,O,P) = 129°) to built up the 3-dimensional structure. Under hydrothermal conditions (T = 400 °C) orange single crystals of the mercury(I) orthophosphates α-(Hg2)3(PO4)2 and β-(Hg2)3(PO4)2 have been obtained from (Hg2)2P2O7 and H3PO4 (c = 1%). The crystal structures of both modifications have been refined from X-ray single crystal data [α-form (β-form): P21/c (P21/n), Z = 2 (2), a = 8,576(3) (7,869(3)), b = 4,956(1) (8,059(3)), c = 15,436(3) (9,217(4)) Å, β = 128,16(3) (108,76(4))°, 1218 (1602) independent reflections of 4339 (6358) reflections, R(F) = 0,039 (0,048) for 74 (74) variables, 8 (8) atoms in the asymmetric unit]. In the structure of α-(Hg2)3(PO4)2 three crystallographically independent mercury atoms, located in two independent dumbbells, are coordinated by three oxygen atoms each. Thus, [(Hg2)O6] dimers with a strongly distorted tetrahedral coordination of all mercury atoms are formed. Such dimers are present besides [(Hg2)O5]-polyhedra in the less dense crystal structure of β-(Hg2)3(PO4)2 (d(Hg–Hg) = 2,518 Å). The mercury(I) phosphates are thermally labile and disproportionate between 200 °C (β-(Hg2)3(PO4)2) and 480 °C (α-(Hg2)3(PO4)2) to elemental mercury and the corresponding mercury(II) phosphate. 相似文献
10.
O. A. Plyusnina V. A. Emel’yanov I. A. Baidina I. V. Korol’kov S. A. Gromilov 《Journal of Structural Chemistry》2007,48(1):114-121
Double complex [RuNO(NH3)4OH][PtCl4] (I) and [RuNO(NH3)4OH][PdCl4] (II) salts have been prepared and explored with TGA, IR spectroscopy, powder and single crystals X-ray diffraction. Crystal phases
of I and II are isostructural (space group Cmc21) and have the following crystal chemical characteristics: a = 8.106 Å, b = 18.190(3) Å, c = 8.097 Å, V = 1194.0 Å3, Z = 4, ρcalc = 3.077 g/cm3 (I), and a = 8.116 Å, b = 18.135 Å, c = 8.062 Å, V = 1186.5 Å3, Z = 4, ρcalc = 2.600 g/cm3 (II). The product of thermal decomposition of I in inert and hydrogen atmospheres is a substitution solid solution Pt0.5Ru0.5 with the parameter of the FCC unit cell a = 3.856(3) Å. Thermolysis of II affords two-phase mixtures of limited solid solutions of the metals featuring Ru-based HCP and Pd-based FCC cells.
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No.1, pp.114–121, January–February, 2007. 相似文献
11.
Olga Yakubovich Galina Kiriukhina Anatoliy Volkov Olga Dimitrova 《Acta Crystallographica. Section C, Structural Chemistry》2019,75(5):514-522
A novel phosphate, sodium zinc aluminium bis(phosphate), NaZnAl(PO4)2, was obtained under mild‐temperature hydrothermal conditions at 553 K. The crystal structure has been studied using single‐crystal X‐ray experimental data. The pseudo‐hexagonal phase NaZnAl(PO4)2 crystallizes in the monoclinic space group P21/c. Its unique crystal structure is based on a three‐dimensional (3D) framework built by Zn‐, Al‐ and P‐centred tetrahedra sharing vertices. Channels parallel to the [101] and [01] directions are limited by six‐ and eight‐membered windows, and incorporate Na atoms. The new compound is discussed as a member of the morphotropic series AMM′PO4, where A = Na, K, Rb or NH4, M = Cu, Ni, Co, Fe, Zn or Mg and M′ = Fe, Al or Ga. The title compound is the first Na representative within the series and is characterized by a 3D architecture of tetrahedra populated in an ordered manner by Zn2+, Al3+ and P5+ ions. 相似文献
12.
C. Marhag D. Ben Hassen-Chehimi H. Said 《Journal of Thermal Analysis and Calorimetry》2006,86(1):249-254
The thermodynamic
exploitation of the solid–liquid equilibria in the MIPO3–Pb(PO3)2, MIPO3–Cu(PO3)2
and MIPO3–Ce(PO3)3
systems (with M
I=Li,
Na, K, Rb, Cs, Ag, Tl) is carried out using a semi-empirical equation of the
liquidus curves already used with success for similar binary systems.
The enthalpy of fusion is calculated for each pure polyphosphate on
the assumption that the liquid solution is ideal and only formed by MIPO3
and M(PO3)q entities (q=2 for Pb and Cu, q=3
for M=Ce). In the most binary systems,
a wide difference between the calculated values of the melting enthalpies
of these polyphosphates and the measured ones determined from the DTA curves,
was observed. This difference is probably due to the existence of some molecular
associations in the liquid phase. 相似文献
13.
C. Marhag H. Said P. Satre C. Favotto J. Rogez 《Journal of Thermal Analysis and Calorimetry》2003,74(1):275-285
Study of solid-liquid phase diagram of LiPO3-Pb(PO3)2 binary system, in certain calcination conditions, shows the existence of several metastable phasis. When heated at a temperature
of 723 K the binary mixtures lead uncompletely to a defined compound Pb2Li(PO3). On heating these ternary solid mixtures, three eutectic reactions have been observed: LiPO3+Pb(PO3)2→Liquid at a temperature of 793 K(1) LiPO3+Pb2Li(PO3)5→Liquid at a temperature of 843 K (2) Pb2Li(PO3)5+Pb(PO3)2→Liquid at a temperature of 891 K (3) The metastable liquid phase appears in the system at temperature of 793 K. DTA experiments
performed on the binary LiPO3-Pb(PO3)2 mixtures, show a superposition of two diagrams. The first one is metastable and the second represents the stable equilibrium
phase diagram. Measurements of liquid enthalpy of binary LiPO3-Pb(PO3)2 system at temperature of 979.65 K were reported. The corresponding values were very small and so the binary system can be
considered as athermal. Assuming an ideal behaviour, the liquidus curves in the metastable diagram were calculated and the
eutectic reaction (LiPO3-Pb(PO3)2→Liquid) was confirmed at 793 K.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
14.
A new iron(II) orthophosphate K[Fe(PO4)] has been obtained by hydrothermal synthesis and its crystal structure was determined by single‐crystal X‐ray diffraction: space group P21/n, Z = 8, a = 9.6199(10), b = 8.6756(8), c = 10.8996(13) Å, β = 115.577(8)° at 193 K, R = 0.023. FeII shows coordination numbers (CN) 4 (distorted tetrahedral) and CN 5 (distorted trigonal bipyramidal). The [FeO4] and [FeO5] units form together with the [PO4] tetrahedra a microporous 3D para‐framework with open channels along the a and b directions. The potassium ions positioned in the channels show CN 7 and 8. The structural relations within the morphotropic row of non‐isotypic K[M(PO4)] structures (M = Zn, Ni, Mn, Fe) are discussed on the basis of common basic structural units. 相似文献
15.
The reaction of 3,6-di-(3-methyl-pyridin-2-yI)-s-tetrazine (DMPTZ, II) with CeIII salt [Ce(NO3)3 · 6H2O] generates a new ligand, N-(3-methyl-pyridin-2-yl)-formimidoyl-(3-methyl-pyridin-2-yl) hydrazone (L), and forms a new complex:
a mononuclear complex [Ce(L)(NO3)2 (H2O)3] · NO3 (III). Crystal data for III: space group P-1, with a = 0.7133(4) nm, b = 1.1139(2) nm, c = 1.4572(3) nm, α= 102.13(2)°, β=
99.81(3)°, γ= 91.10(3)°, Z = 2, V = 1113.6(7) nm3, μ = 2.123 mm−1 and F(000) = 630. L acts as a tri-dentate chelating ligand in III. There are 10 coordination sites around Ce3+ of III, which are respectively occupied by seven oxygen atoms (four from two nitrate anions and three from three H2O molecules) and three nitrogen atoms (all from L). The cerium atom and three chelating nitrogen atoms are coplanar. The mechanism
of the metal assisted decomposition is discussed briefly. 相似文献
16.
Chemical preparations and crystal structures are described for two new bismuth salts: BiHNH4P3O10 and BiNH4(PO3)4. The first one is a new type of tripolyphosphate, while the second one, a long chain polyphosphate, is isostructural with RbNd(PO3)4 and some other MILn(PO3)4 compounds. BiHNH4P3O10 is triclinic, P1 , with a = 7.032(8), b = 7.696(4), c = 8.659(3) Å, α = 106.20(4), β = 105.86(4), γ = 82.78(4)°, Z = 2, V = 432.3 Å3, Dx = 3.694. BiNH4(PO3)4 is monoclinic, P21/n, with a = 10.925(9), b = 9.034(8), c = 10.438(9) Å, β = 106.18(4), Z = 4, V = 989.4 Å3, Dx = 3.644. The crystal structure of BiHNH4P3O10 has been solved by using 4253 independent reflexíons with a final R value of 0.056. The unit cell contains two P3O105? groups related by an inversion center while bismuth atoms in a eightfold coordination build infinite chains of edge-sharing BiO8 polyhedra running parallel to the a axis. The crystal structure of BiNH4(PO3)4 has been solved using 4330 independent reflexions with a final R value of 0.047. Infinite (PO3)∞ chains spread along the [101] direction, alternating with isolated BiO8 polyhedra. 相似文献
17.
Unusual Coordination Polyhedra around Oxygen in Li4Cl(OH)3 The pseudobinary system LiOH/LiCl was investigated by X-ray methods. Two compounds, Li4Cl(OH)3 and Li2Cl(OH), were obtained. The crystal structure of Li4Cl(OH)3 solved by single-crystal methods is delt with. For Li2Cl(OH) powder diffraction data are given: Li4Cl(OH)3: P21/m, Z = 2, a = 5.4096(8) Å, b = 7.382(2) Å, c = 6.2076(8) Å, β = 94.40(1)°, Z(Fo) with (Fo)2 ≧ 3σ(Fo)2 = 483, Z (parameter) = 50, R/Rw = 0.022/0.025 Li2Cl(OH): Pmma, Z = 2, a = 7.680(8) Å, b = 4.001(7) Å, c = 3.899(6) Å The hydroxide rich compound crystallizes in a new type of structure which contains puckered layers [Li4(OH)3+] connected via chloride ions. 相似文献
18.
Synthesis and Structure Determination of Two Salts of the Trimetaphosphimic Acid, K3(PO2NH)3 and Rb3(PO2NH)3 The reaction between P3N5 and the corresponding alkalimetal hydroxide monohydrate under ammonothermal conditions (6 kbar, 450 °C after 10 d) in autoclaves leads to the salts of the trimetaphosphimic acid K3(PO2NH)3 resp. Rb3(PO2NH)3. The structure of K3(PO2NH)3 was solved by single crystals X-ray methods. The isotypic structure of Rb3(PO2NH)3 was solved by X-ray powder diffraction methods. K3(PO2NH)3: R3 (No. 148), a = 12.615(3) Å, c = 10.224(2) Å, Z = 6, R1/wR2 = 0.0276/0.0726, N(F > 2σ(F)) = 769, N(Var.) = 51.Rb3(PO2NH)3: R3 (No. 148), a = 12.9971(5) Å, c = 10.5485(5), Z = 6, RBragg(F) = 0.0626, 289 reflections. K3(PO2NH)3 and Rb3(PO2NH)3 contain six-membered rings P3N3 substituted by oxygen which are connected to double molecules by N–H … O bridge bonds. These twinmolecules are stacked in columns which form the motive of close packed rods. K+ resp. Rb+ are between these columns. They are coordinated by 6 O which belong to 5 different rings. 相似文献
19.
20.
(NH4)2PO3H, H2O crystallizes in the monoclinic system, space group P21/c, with a = 6.322(1) Å, b = 8.323(1) Å, c = 12.676(1) Å, β = 98.84(1) and Z = 4. The structure was refined to R = 0.022 based on 853 independent X-Rays intensities. Improved dimensions of the tetrahedral PO3H2? ion have been obtained: P?H = 1.34(2) and P?O = 1.514(2) Å. The geometry of this ion is compared with that of PO3F2? and SO32? ions and we find a decrease of the volume: VF? > VH+ > Vlone pair. 相似文献