Hydrothermal Synthesis and Structure of Two New Mo(V)-Oxide Phosphates

43

1040-7278/02/0300-0043/0 © 2002 Plenum Publishing Corporation

Journal of Cluster Science, Vol. 13, No. 1, March 2002 (© 2002)

Hydrothermal Synthesis and Structure of Two NewMo(V)-Oxide Phosphates1

1 Dedicated to the memory of Professor Jiaxi Lu.

Wenbin Yang,2 Canzhong Lu,2 , 3 Chuande Wu,2 Shaofang Lu,2

2 The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on theStructure of Matter, The Chinese Academy of Sciences, Fuzhou, Fujian 350002, People’sRepublic of China.

3 To whom correspondence should be addressed. E-mail: [email protected].

Dingming Wu,2 and Honghui Zhuang2

Received March 8, 2001

Two new members of Mo(V) phosphates were synthesized by hydrothermalmethods. (enH2)(enH)[NaMo12O24(OH)6(HPO4)2(H2PO4)6] · (en)4 · 20H2O (1) (en=H2NCH2CH2NH2)[HAD-H2]2 [HAD-H]2 [Zn3Mo12O24 (OH)6 (PO4)2 (HPO4)6] ·6H2O (2) (HAD=H2N(CH2)6NH2). Compound 1 crystallized in the space groupP2(1)/n, a=15.93120(10) Å, b=15.8946(2) Å, c=17.0665(2) Å, V=4316.02(8),b=92.9060(10)°, Z=2. Compound 2 crystallized in the space group P(−1)with a=12.3726(3) Å, b=14.1948(3) Å, c=14.2310(4) Å, a=72.7100(10), b=65.0230(10), c=69.5600(10)°, Z=2089.70(9) Å3, and Z=1. The structureof 1 consists of sandwich-shaped cluster anion [Na{MoV

6O12(OH)3(HPO4)(H2PO4)3}2]3− ({Na(MoV

6)2}) held together via intermolecular hydrogen-bondingcontacts. For the compound 2, the sandwich-shaped clusters Zn[Mo6O12(OH)3(PO4)(HPO4)3]2 ({Zn(MoV

6)2} are linked by tetrahedrally-coordinated zinc intolayers. Organic cations ([H3N(CH2)6NH3]2+ and [H3N(CH2)6NH2]+) are filledin the spaces between lamellas. The layers are held together by a hydrogen-bonded network, which involves the terminal phosphate P-OH groups, as wellas organic cations and several waters of solvation.

KEY WORDS: Hydrothermal synthesis; Mo(V)-oxide phosphates; crystalstructures; hydrogen bonds.

INTRODUCTION

The transition metal-phosphate cluster compounds are attractive due totheir great structural diversity and useful properties as molecular sieves,

File: KAPP/880-jocl/13-1 369608 - Page : 1/12 - Op: KA - Time: 14:15 - Date: 10:04:2002

catalysts and ion-exchangers [1–7]. Of those clusters composed of oxome-talate polyhedra and phosphate tetrahedral units, one of the most interest-ing is the Mo(V) phosphate family with a variety of structural featuresincluding discrete molecular entities, one, two or three-dimensional (3-D)frameworks [1]. During the recent years, with extensive exploration ofthe hydrothermal techniques, a large number of molybdenum phosphateshave been reported, for example, Cs2Mo4P6O26 [8], Cs4Mo8P12O52 [8],AgMo5P8O33 [9],Cs4Mo10P18O66 [10],Mo3P5SiO19 [11], Cs3Mo5P6O25 [12],Cs3Mo4P3O16[13],(PPh4)2[(H3O)2NaMo6O15(HPO4)(H2PO4)3] · 5H2O[14],and Na2[(CH3)4N]4[Cd3Mo12O24(OH)6(PO4)2(HPO4)6] · 10H2O [15]. Inconsidering that Mo(V) phosphates are formed so readily in the solid stateas shown for [Mo6P4X31]n− (X=O, OH) phosphates easily stabilized byvarious transition or post-transition elements such as zinc, iron andcadmium [15–19], we made efforts to investigate the assembly of Mo(V)phosphates in the presence of the secondary metals such as Fe, V or Zn [20].In this paper, two new members of the family, (enH2)(enH)[NaMo12O24(OH)6(HPO4)2(H2PO4)6] · (en)4 · 20H2O (1) (en=H2NCH2CH2NH2) and[HAD-H2]2[HAD-H]2[Zn3Mo12O24(OH)6(PO4)2(HPO4)6] · 6H2O(2)(HAD=NH2(CH2)6NH2), are reported. Their synthesis and structural character-ization are described here.

EXPERIMENTAL

Reagents and Physical Measurements

Reagents were purchased from Aldrich Chemical Co. and usedwithout further purification. All of syntheses were carried out in polyte-trafluoroethylene-lined stainless containers under autogenous pressure. Theelemental analyses of C and H were performed on an EA1110 CHNS-0 CEelemental analyzer, and the contents of Na and Mo were determined byatomic absorption method. All IR (KBr pellet, 4000–400 cm−1) and Raman(l=1064 nm, KBr diluted) spectra were recorded using a Nicolet Magna750FT-IR spectrometer.

Synthesis

(enH2)(enH)[NaMo12O24(OH)6(HPO4)2(H2PO4)6]·(en)4 ·20H2O (1).A mixture containing Na2MoO4 · 2H2O (0.48 g), VOSO4 (0.16 g), H2N(CH2)2NH2 (0.4 ml), H3PO4 (0.4 ml), and H2O (13 ml) was sealed in a Teflon-lined stainless bomb and heated at 200°C for 3 days under autogenouspressure. The red crystalline product of 1 was isolated in low yield(20–35%) by mechanical separation from a brown amorphous solid, of

44 Yang et al.


which the composition is still unknown. Elemental analysis: Anal. Calcd.for C12H111Mo12 N12NaO82P8: Mo, 36.45, Na, 0.73, P, 7.85, C, 4.56, N,0.32, H, 3.54%, Found: Mo, 36.57, Na, 0.69, P, 7.74, C, 4.52, N, 5.41, H,3.56%.

[HAD-H2]2[HAD-H]2[Zn3Mo12O24(OH)6(PO4)2(HPO4)6]·6H2O (2)Hydrothermal treatment of a mixture of Na2MoO4 · 2H2O (0.484 g),(CH3COO)2Zn · 4H2O (0.219 g), H2N(CH2)6NH2(0.46 g), H3PO4 (0.4 ml),HCl (0.2 ml, 10%) and H2O (10 ml) for 3 days at 200°C gives an about85% (based on Mo) of orange-red plates of 2. Elemental analysis: Anal.Calcd. for C24H94Mo12N8O68P8Zn3: Mo, 36.22, Zn, 6.17, P, 7.80, C, 9.07,N, 3.53, H, 2.98%. Found: Mo, 36.15, Zn, 6.23, P, 7.69, C. 8.99, N, 5.61,H, 3.02%.

Table I. Crystal Data and Structure Refinement for(enH2)(enH)[NaMo12O24(OH)6(HPO4)2(H2PO4)6] · (en)4 · 20H2O (1) and[HAD-H2]2[HAD-H]2[Zn3Mo12O24(OH)6(PO4)2(HPO4)6] · 6H2O (2)

Formula C12H111 Mo12N12 Na O82 P8 C24H94Mo12N8O68P8Zn3

Formula weight 3158.16 3178.22Crystal size (mm) 0.40 × 0.19 × 0.10 0.15 × 0.10 × 0.06Crystal color Red Orange-redCrystal system Monoclinic TriclinicSpace group P2(1)/n P(−1)A (Å) 15.93120(10) 12.3726(3)b (Å) 15.8946(2) 14.1948(3)c (Å) 17.0665(2) 14.2310(4)a (°) 90 72.7100(10)b (°) 92.9060(10) 65.0230(10)c (°) 90 69.5600(10)V (Å) 4316.02(8) 2089.70(9)Z 2 1Dcalc (g · cm−3) 2.430 2.526Temperature (K) 293(2) 293(2)M (Mo Ka) (mm−1) 1.970 2.850F(000) 3116 1552Refinement method Full-matrix Full-matrix

least-squares on F2 least-squares on F2

Absorption correction SADABS SADABSMax./min. effective transmission 1.000000/0.725121 1.000000/0.724070Goodness-of-fit on F2 1.356 0.983Final R indices [I > 2 s(I)]a R1=0.0716, wR2=0.1982 R1=0.0606, wR2=0.1344R indices (all data) R1=0.0971, wR2=0.2106 R1=0.1122, wR2=0.1836Max. shift (D/s) in final cycle 0.001 0.001Largest diff. peak and hole (e · Å−3) 2.712 and − 1.377 1.721 and − 2.137

Hydrothermal Synthesis and Structure of Two New Mo(V)-Oxide Phosphates 45


X-Ray Crystallographic Analysis

Suitable crystals of 1 and 2 were mounted on a glass fiber with epoxyresin, and used for data collection on a Siemens SMART CCD diffractom-eter with graphite monochromated Mo-Ka radiation (l=0.71073 Å) atroom temperature. An empirical absorption correction by SADABS wasapplied to the intensity data. A total of 16762 (1.71 [ h [ 25.22°) and10904 (1.56 [ h [ 25.06°) reflections were collected for 1 and 2, respec-tively, of which independent reflections 7670 [R(int)=0.0495] for 1 and7285 [R(int)=0.0484] for 2 were used in the structure analysis. Crystallo-graphic data and structure determination parameters are given in Table I.

Structures of 1 and 2 were solved by direct methods, successiveFourier difference synthesis, and refined by the full matrix least-squaresminimization of (Sw(Fo −Fc)2 with anisotropic thermal parameters for allnon-hydrogen atoms giving rise to final convergence 0.0716, wR2=0.1982(I > 2s(I)) with 593 parameters for 1 and 0.0624, wR2=0.1409 (I > 2s(I))with 558 parameters for 2. Final atomic coordinates and displacementparameters for non-hydrogen atoms, full lists of bond lengths and bondangles, and bond valence sum (BVS) calculations have been given insupplementary materials.

RESULTS AND DISCUSSIONS

The X-ray analysis revealed that both compounds have similar sandwich-shaped cluster anions, namely, {Na[MoV

6O12(OH)3(HPO4)(H2PO4)3]}3−

({Na(MoV6)2}) for1and[Zn{Mo6O12(OH)3(PO4)(HPO4)3}2]10−({Zn(MoV

6)2})for 2. The geometry of both sandwich-shaped anions (Figs. 1 and 3) is verysimilar to the unit already encountered in several sodium, iron, cadmium orzinc hydroxyphosphates [15–18]. Both cluster anions contain two co-planar {Mo6} rings of six Mo(O5OH) edge-sharing octahedra; the two{Mo6} rings are bonded together through one octahedral Na or Zn ion togenerate a sandwich-shaped cluster with rigorous ( − 1) symmetry. Sixmolybdenum atoms of each ring are co-planar with alternating shortMo–Mo bonds (approximately 2.59 Å) and non-bonding Mo · · · Mo con-tacts (approximately 3.55 Å). The Mo–Mo distances observed show thatthese {Mo6} rings can be considered as three {Mo2O4} units beingmutually connected by a peripheral phosphate ligand and by a hydroxogroup, with alternating short Mo–Mo bonds within the {Mo2O4} dimers,and non-bonding Mo · · · Mo contacts between the {Mo2O4} subunits, acommon feature among cyclic arrangements based on dinuclear [Mo2O2E2](E=O, S) units [15–20, 23]. Each ring encapsulates a central phosphate

46 Yang et al.


Fig. 1. (a) Building unit of 1 showing the atom labeling scheme. (b) Polyhedral representationshowing that six edge-sharing MoO6 octahedra are linked by alternating bonding (approxi-mately 2.59 Å) and non-bonding (3.52–3.59 Å) contacts into a {Mo6} ring. (c) Polyhedralrepresentation of the second-metal bridged dimmer {M(Mo6)2} (M=Na for 1 and Zn for 2)of the {Mo6} rings showing all of the PO4 groups lie on the side of the plane defined by thesix Mo atoms.

Fig. 2. Stereoview of a section of the three-dimensional network of complex 1 formed viaO · · · O and N · · · O hydrogen bonds (projected on the [100] direction).



Fig. 3. (a) Atoms in the asymmetric unit of 2 and the numbering scheme for the atoms(projected on the [001] direction. (b) A view down the b axis illustrating how the {Zn(Mo6)}2units are linked by tetrahedral Zn into layers with different ‘‘voids’’ in them marked as A, Band C (4.771×9.584 Å for A, 6.022×6.391 Å for B and 4.984×6.895 Å for C).

Table II. Selected Bonds (Å) for 1 and 2

1

Bonds Distances Bonds Distances

Mo(1)–O(2) 1.683(8) Mo(5)–O(18) 2.123(8)Mo(1)–O(3) 1.943(8) Mo(5)–O(16) 2.257(8)Mo(1)–O(6) 1.957(8) Mo(5)–Mo(6) 2.5837(15)Mo(1)–O(1) 2.047(8) Mo(6)–O(24) 1.682(9)Mo(1)–O(4) 2.094(7) Mo(6)–O(21) 1.955(8)Mo(1)–O(5) 2.284(7) Mo(6)–O(22) 1.966(8)Mo(1)–Mo(2) 2.5922(15) Mo(6)–O(23) 2.063(8)Mo(2)–O(7) 1.700(8) Mo(6)–O(4) 2.103(8)Mo(2)–O(3) 1.949(9) Mo(6)–O(5) 2.283(7)Mo(2)–O(6) 1.956(8) P(1)–O(26) 1.525(9)Mo(2)–O(10) 2.049(8) P(1)–O(25) 1.525(10)Mo(2)–O(9) 2.150(8) P(1)–O(23) 1.547(8)Mo(2)–O(8) 2.236(8) P(1)–O(1) 1.551(9)Mo(3)–O(11) 1.659(9) P(2)–O(28) 1.528(10)Mo(3)–O(12) 1.947(8)) P(2)–O(17) 1.533(9)Mo(3)–O(14) 1.952(7) P(2)–O(27) 1.541(9)Mo(3)–O(13) 2.049(9) P(2)–O(19) 1.544(9)Mo(3)–O(9) 2.140(8) P(3A)–O(30) 1.474(12)Mo(3)–O(8) 2.298(8) P(3A)–O(29) 1.488(17)Mo(3)–Mo(4) 2.5995(14) P(3A)–O(10) 1.540(11)

48 Yang et al.


Table II. (Continued)

1

Bonds Distances Bonds Distances

Mo(4)–O(15) 1.685(9) P(3A)–O(13) 1.591(11)Mo(4)–O(12) 1.936(9) P(3B)–O(30) 1.460(12)Mo(4)–O(14) 1.961(8) P(3B)–O(13) 1.527(12)Mo(4)–O(17) 2.061(8) P(3B)–O(10) 1.530(11)Mo(4)–O(18) 2.100(8) P(3B)–O(31) 1.60(2)Mo(4)–O(16) 2.347(8) P(4)–O(32) 1.495(9)Mo(5)–O(20) 1.670(8) P(4)–O(16) 1.543(8)Mo(5)–O(21) 1.932(8) P(4)–O(8) 1.552(8)Mo(5)–O(22) 1.940(7) P(4)–O(5) 1.578(8)Mo(5)–O(19) 2.096(8)

2

Mo(1)–O(6) 1.687(9) Mo(6)–O(24) 1.679(8)Mo(1)–O(3) 1.919(8) Mo(6)–O(20) 1.925(9)Mo(1)–O(5) 1.968(8) Mo(6)–O(21) 1.969(9)Mo(1)–O(1) 2.062(9) Mo(6)–O(23) 2.064(9)Mo(1)–O(4) 2.105(8) Mo(6)–O(4) 2.095(9)Mo(1)–O(2) 2.329(8) Mo(6)–O(2) 2.313(8)Mo(1)–Mo(2) 2.5765(16) Zn(1)–O(21)#1 2.153(9)Mo(2)–O(9) 1.681(9) Zn(1)–O(21) 2.153(9)Mo(2)–O(3) 1.928(9) Zn(1)–O(11) 2.169(7)Mo(2)–O(5) 1.981(8) Zn(1)–O(11)#1 2.169(7)Mo(2)–O(10) 2.072(8) Zn(1)–O(5)#1 2.216(8)Mo(2)–O(7) 2.123(8) Zn(1)–O(5) 2.216(8)Mo(2)–O(8) 2.283(8) Zn(2)–O(30) 1.915(9)Mo(3)–O(13) 1.676(9) Zn(2)–O(31) 1.932(8)Mo(3)–O(12) 1.944(9) Zn(2)–O(28)#2 1.933(9)Mo(3)–O(11) 1.976(8) Zn(2)–O(26)#3 1.956(9)Mo(3)–O(14) 2.069(8) P(1)–O(26) 1.517(9)Mo(3)–O(7) 2.097(8) P(1)–O(25) 1.526(10)Mo(3)–O(8) 2.289(8) P(1)–O(23) 1.549(10)Mo(3)–Mo(4) 2.5929(16) P(1)–O(1) 1.553(10)Mo(4)–O(17) 1.694(9) P(2)–O(28) 1.522(9)Mo(4)–O(12) 1.937(8) P(2)–O(27) 1.528(10)Mo(4)–O(11) 1.972(8) P(2)–O(10) 1.536(9)Mo(4)–O(18) 2.051(9) P(2)–O(14) 1.555(10)Mo(4)–O(16) 2.116(9) P(3)–O(18) 1.529(9)Mo(4)–O(15) 2.280(8) P(3)–O(30) 1.531(9)Mo(5)–O(22) 1.676(9) P(3)–O(19) 1.543(9)Mo(5)–O(20) 1.948(9) P(3)–O(29) 1.543(9)Mo(5)–O(21) 1.970(8) P(4)–O(31) 1.536(9)Mo(5)–O(19) 2.057(8) P(4)–O(2) 1.541(9)Mo(5)–O(16) 2.110(9) P(4)–O(8) 1.546(9)Mo(5)–O(15) 2.274(8) P(4)–O(15) 1.552(9)Mo(5)–Mo(6) 2.5958(16)



and is then stabilized by three peripheral phosphate ligands located on thesame side of the mean plane defined by six Mo atoms. It should be pointedout that one of the three peripheral phosphate groups in {Na(MoV

6)2} islocated at two sites (P(3A) and P(3B)) with partial occupancy of 0.5.

The analysis of selected bond lengths for 1 and 2 shows that all Mo–Ooctahedra present the characteristic geometry of MoV, with a short Mo–Obond (1.659–1.700 Å in 1 and 1.676–1.694 Å in 2) opposed to an abnor-mally long Mo–O bond lengths (2.236–2.347 Å in 1 and 2.274–2.313 Åin 2) and four intermediate equatorial Mo–O bonds within the range of1.932–2.150 Å in 1 and 1.919–2.123 Å in 2. The pentavalence character forall molybdenum atoms in both compounds was confirmed by bond valencesum calculations based on the Brown equation [24], since values rangingfrom 5.13 to 5.29 were obtained, and according to this procedure, the O(4),O(9), O(18) O(25), O(26), O(27), O(28), O(29), O(30), O(31) and O(32) sitesin 1 and O(4), O(7), O(16), O(25), O(27), O(29) sites in 2 are ascribed toOH− sites, as whose bond valence sum values (1.066–1.357) are significantsmaller than that of the others (1.671–1.955) that are normal for theO2− sites. The bond valence sum values for P atoms in 1 and 2 are in therange of 4.71–5.01, indicating normal pentavalence for P. These analysesshow that each central phosphate group (PO3OH) in {Na(MoV

6)2} has oneterminal OH, and each of the remaining peripheral phosphate groups(PO2(OH)2) has two terminal OH groups, whereas only three protonationsites (and symmetric positions) are found in the {Zn(MoV

6)2} cluster anion.In Fig. 2, a stereo-network structure of 1 is given, which shows how

the sandwiched-shaped anions are held together within the framework viahydrogen-bonding contacts as follows: the terminal groups of the organicamine interact with the anions via hydrogen bonds, with distances in therange of 2.64–3.01 Å for N · · · O; the crystallized water molecules arehydrogen bonded to anions with O · · · O distances in the range of2.62–2.97 Å.

The two-dimensional structure of 2 is built up from the sandwich-shaped cluster [Zn{Mo6O12(OH)3(PO4)(HPO4)3}2]10− ({Zn(MoV

6)2}) asfollows: each {Zn(MoV

6)2} cluster is linked to six additional building blocksthrough contacting six different tetrahedral Zn. These tetrahedral Zn,which are crystallographically identical, are coordinated to the terminalphosphate O atoms of the Mo6 rings in the following way: each Zntetrahedron shares the single terminal O atom of the central phosphate(P(4)), and one apex from a peripheral PO3OH tetrahedron (P(3)), whichare from the same Mo6 ring of one {Zn(MoV

6)2} cluster; the remaining Oatoms in its coordination sphere are bonded to two different atoms fromtwo different Mo6 rings of two neighboring {Zn(MoV

6)2} units. Therefore,each tetrahedral Zn atom contacts four phosphate groups from three

50 Yang et al.


Fig. 4. (a) A ball-and-stick view along the z axis illustrating how two neighboring layers areheld together via the terminal P-OH groups. (b) A polyhedral view parallel to the layer illus-trating how the 1,6-hexanediamines cations are interposed between the layers. Mo6 rings aremarked with dashed lines, ZnO6 octahedra with crosses, PO4 tetrahedra with parallel lines,while ZnO4 tehrahedra have a regular dot pattern, and the free big balls are crystallized watermolecules.

different {Zn(MoV6)2 units; each {Zn(MoV

6)2 cluster is in turn coordinatedto six tetrahedral Zn, forming a two-dimensional [Zn3Mo12O24(OH)6(PO4)2(HPO4)6]n 6n− layer.

A stereo-network structure of the zinc molybdenum (MoV) phosphate2 is given in Fig. 4, which shows how the 1,6-hexanediamines cations([H3N(CH2)6NH3]2+ and [H3N(CH2)6NH2]+) are pervaded in the spacebetween lamellas. These amine groups interact with the anions of thelayered frameworks via hydrogen bonds, with distances in the range of2.69–3.03 Å, so that the Zn-Mo-O-P layers are connected into a three-dimensional structure. In another word, these Zn-Mo-O-P layers are heldtogether by a O · · · O hydrogen-bonded network, involving (i) the terminalP(3)-O(29)H group, oriented perpendicular to the plane of the layer and



Fig. 5. IR spectra of (a) 1 and (b) 2.

52 Yang et al.


points into the interlamellar space, is hydrogen bonded to another P(3 i)-O(29 i)H group on a neighboring layer (O(29) · · · O(29 i), 2.48 Å); (ii) the Oatoms of the crystallized water within and between layers are all hydrogenbonded to the layers with O · · · O distances of 2.71-3.01 Å.

As shown in Fig. 5, the IR spectrum of 1 and 2 show similar charac-teristics features, namely, absorptions at 941 and 914 cm−1 are attributed ton(Mo=O); a series of bands in the 1530–1340 cm−1 region are assigned tothe C–C and C–N stretching vibrations of the organic amines; and bandsin the 995–1200 cm−1 range are associated to n(P-O) of the phosphate.However, the strength of the band at 914 cm−1 of 1 is much weaker thanthat of 2.

SUPPLEMENTARY INFORMATION

Crystallographic data have been deposited with the Cambridge Crys-tallographic Data Centre, 12 Union Road, Cambridge CB2 IEZ, UnitedKingdom, and copies can be obtained upon request, free of charge, byquoting the publication citation and the deposition number: 1 CCDC174208, 2 CCDC 174209.

ACKNOWLEDGMENTS

The authors thank the Chinese Academy of Sciences, the State KeyLab of Structural Chemistry, the State Education Ministry, the NationalScience Foundation of China (20073048) and Natural Science Foundationof Fujian for financial support.

REFERENCES

1. A. K. Cheetham, G. Férey, and T. Loiseau (1999). Angew. Chem. Int. Ed. Engl. 38, 3268.2. A. Choudhury and S. Natarajan (2000). J. Solid State Chem. 154, 507.3. V. Soghomonian, Q. Chen, R. C. Haushalter, and J. Zubieta (1993). Angew. Chem. Int.

Ed. Engl. 32, 610.4. V. Soghomonian, Q. Chen, R. C. Haushalter, J. Zubieta, and J. O’Connor (1993). Science

259, 1596.5. M. I. Khan, L. M. Meyer, R. C. Haushalter, A. L. Schweitzer, J. Zubieta, and J. L. Dye

(1996). Chem. Mater. 8, 43.6. S. Ekambaram and S. C. Sevov (1999). Angew. Chem. Int. Ed. Engl. 38, 372.7. S. Ekambaram, C. Serre, G. Férard, and S. C. Sevov (2000). Chem. Mater. 12, 444.8. K.-H. Lii and R. C. Haushalter (1987). J. Solid State Chem. 69, 320.9. K.-H. Lii, D. C. Johnston, D. P. Goshorn, and R. C. Haushalter (1987). J. Solid State

Chem. 71, 131.10. R. C. Haushalter and F. W. Lai (1988). J. Solid State Chem. 76, 218.11. S. L. Wang, C. C. Wang, and K.-H. Lii (1988). J. Solid State Chem. 74, 409.



12. R. C. Haushalter, K.-H. Lii, and C. M. O’Connor (1987). Angew. Chem. Int. Ed. Engl. 26,549.

13. R. C. Haushalter (1987). J. Chem. Soc. Chem. Commun. 374.14. R. C. Haushalter and F. W. Lai (1989). Inorg. Chem. 28, 2905.15. A. Guesdon, M. M. Borel, A. Leclaire, and B. Raveau (1997). Chem. Eur. J. 3, 1797.16. R. C. Haushalter and F. W. Lai (1989). Angew. Chem. Int. Ed. Engl. 28, 743.17. L. A. Mundi and R. C. Haushalter (1992). Inorg. Chem. 31, 3050.18. L. A. Meyer and R. C. Haushalter (1993). Inorg. Chem. 32, 1579.19. A. Müller, S. Dillinger, E. Krickemeyer, H. Bögge, W. plass, A. Stammler, and R. C.

Haushalter (1997). Z. Naturforsch. 52b, 1301.20. W. B. Yang, C. Lu, C. D. Wu, S. F. Lu, and H. H. Zhuang. Unpublished results.21. R. C. Haushalter and L. A. Mundi (1992). Chem. Mater. 4, 31.22. V. Soghomonian, Q. Chen, R. C. Haushalter, J. Zubieta, and J. O’Connor (1993). Science

259, 1596.23. E. Cadot, A. Dolbecq, B. Salignac, and F. Sécheresse (1999). Chem. Eur. J. 5, 2396.24. N. E. Brese and M. O’Keeffe (1991). Acta. Cryst. B47, 192.

54 Yang et al.


Hydrothermal Synthesis and Structure of Two New Mo(V)-Oxide Phosphates

Documents

Transcript of Hydrothermal Synthesis and Structure of Two New Mo(V)-Oxide Phosphates