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Single crystals of molybdenum(VI) tricopper(II) tellurium(IV) hepta­oxide dichloride hemihydrate, MoCu3TeO7Cl2·0.5H2O, were synthesized via a transport reaction in sealed evacuated silica tubes. All atoms occupy general positions within the triclinic (P \overline 1) unit cell. The building units are irregular CuO4Cl and CuO3Cl2 square pyramids, distorted TeO3+1E trigonal bipyramids (E is the lone pair of TeIV) and irregular MoO5 pyramids. The TeO3+1E, CuO4Cl and CuO3Cl2 polyhedra form (110) layers bridged by Mo atoms. The water mol­ecules are located in [100] channels.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106000679/bc1088sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106000679/bc1088Isup2.hkl
Contains datablock I

Comment top

Transition metal oxohalogenides containing elements such as TeIV, SeIV, AsIII or SbIII with stereochemically active lone pairs form a family with a very rich structural chemistry in which there is a high probability to find novel host–guest compounds and low-dimensional compounds with interesting physical properties (Johnsson et al., 2000, 2003, 2004; Becker et al., 2005). In these oxohalogenides, the lone-pair cations are most often coordinated by oxygen, while the late transition metal ions are coordinated by both oxygen and halogen anions. The aim of the present work was to introduce a highly charged transition metal in oxohalogenides containing late transition metals and asymmetrically coordinated lone-pair elements. The idea was to use the MoVI ion as a spacer to force the CuII ions to take low-dimensional arrangements.

The Te atom has a threefold asymmetric coordination by oxygen with Te—O distances in the range 1.876 (4)–1.892 (4) Å. A fourth, longer, Te—O4 distance of 2.836 (4) Å completes a TeO3 + 1 see-saw coordination. When the stereochemically active 5 s2 lone pair (E) is taken into account, the coordination becomes a distorted trigonal bipyramid [TeO3 + 1E], where E is located in the equatorial plane. Assuming a Te—E distance of 1.25 Å (Galy et al., 1975), the lone-pair centre is located at x = 0.7868, y = 0.7994 and z = 0.1781.

Atom Cu1 is coordinated by four O atoms in a square–planar configuration [Cu—O = 1.923 (4)– 1.962 (4) Å] and one Cl atom that completes a CuO4Cl square pyramid [Cu—Cl = 2.945 (2) Å]. Atoms Cu2 and Cu3 are coordinated by three O atoms and one Cl atom in a square-planar geometry, with Cu—O distances in the range 1.914 (4)–1.992 (4) Å and Cu—Cl distances in the range 2.2474 (18)–2.2628 (17) Å. The distorted square pyramid is completed by Cu—Cl distances in the range 2.7192 (19)–2.7259 (19) Å. This unusual CuO3Cl2 square-pyramidal coordination has been found before in Cu5Se2O8Cl2 (Galy et al., 1979). The Mo atom is coordinated by five O atoms in a distorted square-pyramidal configuration, with Mo—O distances in the range 1.698 (5)–2.085 (4) Å.

Each Cu1O4Cl polyhedron shares edges with one Cu1O4Cl, one Cu2O3Cl2 and one Cu3O3Cl2 polyhedron. Furthermore, it shares a corner with one MoO5 polyhedron and three TeO3 + 1E polyhedra. The different Cu polyhedra are arranged to form Cu8O20Cl6 rings in the structure (Fig. 1). The TeO3 + 1E polyhedra are isolated from each other and share corners with three Cu1O4Cl and three Cu2O3Cl2 polyhedra. Two MoO5 polyhedra share an edge and form Mo2O8 units that connect the layers built by the TeO3 + 1E, CuO4Cl and CuO3Cl2 polyhedra. These connections create voids that host water molecules with a partial occupancy of 50% (Fig. 2). When the water molecule is present, it may form hydrogen bonds to O5 that weaken the Mosc/Desktop/publCIF/symbols/dbnd.png" height="12" />O5 double bond and cause the observed large anisotropic displacement parameter of O5.

Structural refinements and thermal gravimetric analyses on MoCu3TeO7Cl2.xH2O crystals that were left in the laboratory for about one week support the fact that water is present in the channels of the crystal structure at the O8 position. During the refinements, the x value was found to be sc/Desktop/publCIF/symbols/sim.png" height="12" />0.5. Thermogravimetric analysis (TGA) gave a weight loss of 1.5 wt% that also corresponds to x sc/Desktop/publCIF/symbols/sim.png" height="12" />0.5. The uptake of water is relatively rapid and was found to be sc/Desktop/publCIF/symbols/sim.png" height="12" />0.3 H2O after exposing the crystals to air for 0.5 h and sc/Desktop/publCIF/symbols/sim.png" height="12" />0.4 H2O after 3 h (Fig. 3). The Mo—O8 distance of 2.495 (13) Å is close to the longest Mo—O distance in MoTe2O7 [2.589 (6) Å], with a distorted octahedral coordination around MoVI (Arnaud et al., 1976).

Experimental top

Single crystals of MoCu3TeO7Cl2.xH2O were synthesized from MoO3 (Chempur, 99.9%), CuO (Aldrich, 99.99%), CuCl2.xH2O (Aldrich, +99%), and TeO2 (Aldrich, 99.995%) as starting materials. The water in the CuCl2.xH2O powder was evaporated at 283 K before use. The preparation was made starting with MoO3, CuO, CuCl2 and TeO2 in a 1:2:1:1 stoichiometric molar ratio, mixed in a mortar and placed a Pyrex glass tube (length sc/Desktop/publCIF/symbols/sim.png" height="12" />5 cm) which was then evacuated. The tube was heated at 730 K for 65 h in a muffle furnace. The product formed as thin green plate-like crystals. The uptake of water upon exposure of the crystals to air was studied by use of thermogravimetry (TG, Perkin Elmer TGA7) at a heating rate of 10 K min −1.

Refinement top

Four different diffraction data sets were recorded with the crystal in different ϕ and χ orientations. Scale factors for the individual data sets were computed with SHELXL97 (Sheldrick, 1997) and finally the individual data sets were scaled and averaged with the program REFLEX (Eriksson, 2004). All atoms except for those of the water molecule were refined with anisotropic displacement parameters.

The H atoms were identified in the difference Fourier map in the final stage of the refinement by careful inspection of the electron-density peaks located at distances between 0.8 and 1.2 Å from the O atoms within the voids of the structure. They were then refined using a riding model with tetrahedral Mo—O—H angles. The displacement parameters of the H atoms were fixed at 1.5 times the Ueq value of the carrier O atom. The occupancy of the H atoms was fixed at the same value as that of the carrier O atom.

Computing details top

Data collection: EXPOSE in IPDS Software (Stoe & Cie, 1997); cell refinement: CELL in IPDS Software; data reduction: INTEGRATE in IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. The Cu8O20Cl6 unit, with ellipsoids drawn at the 50% probability level. [Symmetry codes: (i) 1 − x, 1 − y, −z; (ii) 2 − x, 1 − y, −z; (vi) x, 1 + y, z; (vii) 2 − x, 2 − y, −z.]
[Figure 2] Fig. 2. An overview of the structure of MoCu3TeO7Cl2.xH2O. CuO4Cl and CuO3Cl2 polyhedra are ligth grey, MoO5 are striped. The O, Te and Cl atoms are white, grey and grey and checked, respectively. The H atoms are small black circles and the Te lone pairs (E) are shown as large black circles.
[Figure 3] Fig. 3. Thermogravimetric analysis of MoCu3TeO7Cl2.xH2O. The sample is continuously dehydrated between room temperature and 543 K. One week of exposure to air in the laboratory gives a weight loss of about 1.5 wt% (first run) that corresponds to x sc/Desktop/publCIF/symbols/sim.png" height="12" />0.5. The quick uptake of water is shown by subsequent experiments with exposure times of 0.5 and 3 h.
molybdenum(VI) tricopper(II) tellurium(IV) heptaoxide dichloride hemihydrate top
Crystal data top
MoCu3TeO7Cl2·0.5H2OZ = 2
Mr = 606.07F(000) = 552
Triclinic, P1Dx = 4.34 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.1393 (15) ÅCell parameters from 1691 reflections
b = 6.386 (2) Åθ = 1.9–28.2°
c = 12.005 (3) ŵ = 11.77 mm1
α = 81.75 (4)°T = 291 K
β = 85.76 (3)°Plate, green
γ = 86.18 (3)°0.08 × 0.04 × 0.01 mm
V = 463.8 (2) Å3
Data collection top
Stoe IPDS
diffractometer
1677 reflections with I > 2σ(I)
ϕ scansRint = 0.094
Absorption correction: numerical
(X-RED; Stoe & Cie, 2001)
θmax = 28.1°, θmin = 3.2°
Tmin = 0.37, Tmax = 0.524h = 88
13580 measured reflectionsk = 88
2214 independent reflectionsl = 1515
Refinement top
Refinement on F212 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.027 w = 1/[σ2(Fo2) + (0.0218P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.054(Δ/σ)max < 0.001
S = 0.85Δρmax = 1.18 e Å3
2214 reflectionsΔρmin = 0.93 e Å3
131 parameters
Crystal data top
MoCu3TeO7Cl2·0.5H2Oγ = 86.18 (3)°
Mr = 606.07V = 463.8 (2) Å3
Triclinic, P1Z = 2
a = 6.1393 (15) ÅMo Kα radiation
b = 6.386 (2) ŵ = 11.77 mm1
c = 12.005 (3) ÅT = 291 K
α = 81.75 (4)°0.08 × 0.04 × 0.01 mm
β = 85.76 (3)°
Data collection top
Stoe IPDS
diffractometer
2214 independent reflections
Absorption correction: numerical
(X-RED; Stoe & Cie, 2001)
1677 reflections with I > 2σ(I)
Tmin = 0.37, Tmax = 0.524Rint = 0.094
13580 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02712 restraints
wR(F2) = 0.054H-atom parameters constrained
S = 0.85Δρmax = 1.18 e Å3
2214 reflectionsΔρmin = 0.93 e Å3
131 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Te0.83915 (5)0.61434 (6)0.15978 (3)0.00860 (9)
Mo0.84960 (7)0.04469 (8)0.60778 (4)0.01124 (11)
Cu10.98898 (11)0.89752 (10)0.10435 (6)0.01029 (15)
Cu20.67111 (11)0.04450 (13)0.30700 (6)0.01585 (17)
Cu30.65568 (10)0.53174 (11)0.10432 (6)0.01191 (15)
Cl10.6604 (2)0.4627 (2)0.28419 (12)0.0192 (3)
Cl20.5153 (2)0.0512 (2)0.13337 (12)0.0190 (3)
O10.8354 (6)0.0209 (8)0.4469 (3)0.0191 (9)
O20.9575 (6)0.6068 (6)0.1254 (3)0.0120 (8)
O30.3902 (7)0.0721 (8)0.3712 (4)0.0293 (11)
O40.9865 (6)0.8222 (6)0.0600 (3)0.0106 (8)
O50.7965 (8)0.3089 (8)0.6448 (4)0.0288 (11)
O60.9747 (6)0.0160 (6)0.2604 (3)0.0124 (8)
O70.3603 (6)0.4510 (7)0.0605 (3)0.0131 (8)
O80.1077 (19)0.345 (2)0.4545 (11)0.048 (3)*0.5
H8A0.0770.40620.39940.073*0.5
H8B0.01550.40030.51540.073*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Te0.00801 (16)0.00911 (18)0.00872 (18)0.00291 (13)0.00016 (12)0.00062 (14)
Mo0.0075 (2)0.0186 (3)0.0075 (2)0.00059 (18)0.00172 (17)0.0007 (2)
Cu10.0144 (3)0.0080 (3)0.0089 (3)0.0033 (3)0.0018 (2)0.0008 (3)
Cu20.0079 (3)0.0301 (4)0.0099 (4)0.0046 (3)0.0010 (2)0.0032 (3)
Cu30.0065 (3)0.0159 (4)0.0139 (4)0.0046 (2)0.0006 (3)0.0029 (3)
Cl10.0204 (7)0.0221 (7)0.0158 (7)0.0054 (6)0.0006 (6)0.0036 (6)
Cl20.0198 (7)0.0201 (7)0.0147 (7)0.0030 (6)0.0040 (5)0.0014 (6)
O10.0092 (18)0.040 (3)0.007 (2)0.0043 (17)0.0006 (15)0.0032 (19)
O20.0085 (17)0.0094 (19)0.018 (2)0.0010 (14)0.0021 (15)0.0003 (16)
O30.0226 (16)0.0398 (19)0.0262 (18)0.0091 (15)0.0022 (14)0.0034 (15)
O40.0126 (14)0.0087 (14)0.0103 (15)0.0057 (12)0.0007 (12)0.0016 (12)
O50.041 (3)0.022 (3)0.020 (3)0.005 (2)0.002 (2)0.003 (2)
O60.0082 (17)0.020 (2)0.009 (2)0.0016 (15)0.0029 (14)0.0017 (17)
O70.0115 (18)0.021 (2)0.0082 (19)0.0073 (16)0.0025 (14)0.0051 (17)
Geometric parameters (Å, º) top
Te—O7i1.876 (4)Cu2—Cl12.7192 (19)
Te—O41.887 (4)Cu2—Mov3.0868 (12)
Te—O2ii1.892 (4)Cu3—O71.933 (4)
Te—O5iii2.836 (5)Cu3—O21.934 (4)
Mo—O51.698 (5)Cu3—O7i1.992 (4)
Mo—O3iv1.745 (4)Cu3—Cl12.2628 (17)
Mo—O11.911 (4)Cu3—Cl2vi2.7259 (19)
Mo—O6v1.920 (4)Cu3—Cu3i3.0325 (17)
Mo—O1v2.085 (4)Cl2—Cu3viii2.7259 (19)
Mo—O8iv2.495 (13)O1—Mov2.085 (4)
Mo—Cu2v3.0868 (12)O2—Teii1.892 (4)
Cu1—O6vi1.923 (4)O3—Moiv1.745 (4)
Cu1—O21.933 (4)O4—Cu1vii1.957 (4)
Cu1—O4vii1.957 (4)O6—Mov1.920 (4)
Cu1—O41.962 (4)O6—Cu1viii1.923 (4)
Cu1—Cl2vi2.9452 (17)O7—Tei1.876 (4)
Cu1—Cu1vii3.0039 (16)O7—Cu3i1.992 (4)
Cu2—O11.914 (4)O8—Moiv2.495 (13)
Cu2—O31.927 (5)O8—H8A0.82
Cu2—O61.975 (4)O8—H8B0.9702
Cu2—Cl22.2474 (18)
O7i—Te—O498.01 (17)O6—Cu2—Cl295.51 (12)
O7i—Te—O2ii92.77 (17)O1—Cu2—Cl1105.27 (16)
O4—Te—O2ii93.19 (17)O3—Cu2—Cl192.77 (16)
O7i—Te—O5iii106.29 (16)O6—Cu2—Cl188.73 (13)
O4—Te—O5iii154.16 (15)Cl2—Cu2—Cl193.94 (7)
O2ii—Te—O5iii77.24 (16)O1—Cu2—Mov41.54 (12)
O5—Mo—O3iv105.2 (2)O3—Cu2—Mov136.08 (15)
O5—Mo—O1101.7 (2)O6—Cu2—Mov36.95 (11)
O3iv—Mo—O1101.0 (2)Cl2—Cu2—Mov127.65 (5)
O5—Mo—O6v99.3 (2)Cl1—Cu2—Mov102.51 (5)
O3iv—Mo—O6v99.97 (19)O7—Cu3—O2171.81 (16)
O1—Mo—O6v145.07 (17)O7—Cu3—O7i78.85 (17)
O5—Mo—O1v111.5 (2)O2—Cu3—O7i93.17 (16)
O3iv—Mo—O1v143.4 (2)O7—Cu3—Cl196.46 (12)
O1—Mo—O1v71.15 (18)O2—Cu3—Cl191.24 (13)
O6v—Mo—O1v75.33 (15)O7i—Cu3—Cl1171.64 (13)
O5—Mo—O8iv174.7 (3)O7—Cu3—Cl2vi90.49 (13)
O3iv—Mo—O8iv70.7 (3)O2—Cu3—Cl2vi90.90 (12)
O1—Mo—O8iv76.2 (3)O7i—Cu3—Cl2vi86.93 (13)
O6v—Mo—O8iv84.8 (3)Cl1—Cu3—Cl2vi100.11 (7)
O1v—Mo—O8iv72.7 (3)O7—Cu3—Cu3i40.13 (11)
O5—Mo—Cu2v105.56 (17)O2—Cu3—Cu3i131.86 (13)
O3iv—Mo—Cu2v131.29 (17)O7i—Cu3—Cu3i38.72 (11)
O1—Mo—Cu2v108.59 (12)Cl1—Cu3—Cu3i136.19 (5)
O6v—Mo—Cu2v38.20 (11)Cl2vi—Cu3—Cu3i88.30 (6)
O1v—Mo—Cu2v37.50 (11)Cu3—Cl1—Cu2114.97 (7)
O8iv—Mo—Cu2v79.7 (3)Cu2—Cl2—Cu3viii98.88 (7)
O6vi—Cu1—O296.39 (17)Mo—O1—Cu2150.0 (2)
O6vi—Cu1—O4vii91.64 (17)Mo—O1—Mov108.85 (18)
O2—Cu1—O4vii171.79 (17)Cu2—O1—Mov100.97 (18)
O6vi—Cu1—O4170.79 (17)Teii—O2—Cu1133.0 (2)
O2—Cu1—O491.96 (17)Teii—O2—Cu3115.04 (19)
O4vii—Cu1—O479.92 (17)Cu1—O2—Cu3111.99 (19)
O6vi—Cu1—Cl2vi76.88 (11)Moiv—O3—Cu2148.3 (3)
O2—Cu1—Cl2vi84.59 (12)Te—O4—Cu1vii119.4 (2)
O4vii—Cu1—Cl2vi95.60 (12)Te—O4—Cu1131.5 (2)
O4—Cu1—Cl2vi100.12 (12)Cu1vii—O4—Cu1100.08 (17)
O6vi—Cu1—Cu1vii131.54 (13)Mov—O6—Cu1viii131.1 (2)
O2—Cu1—Cu1vii131.86 (13)Mov—O6—Cu2104.86 (18)
O4vii—Cu1—Cu1vii40.01 (12)Cu1viii—O6—Cu2111.72 (18)
O4—Cu1—Cu1vii39.91 (11)Tei—O7—Cu3124.8 (2)
Cl2vi—Cu1—Cu1vii100.27 (5)Tei—O7—Cu3i134.0 (2)
O1—Cu2—O394.84 (19)Cu3—O7—Cu3i101.15 (17)
O1—Cu2—O678.10 (16)Moiv—O8—H8A109.5
O3—Cu2—O6172.93 (18)Moiv—O8—H8B120.3
O1—Cu2—Cl2159.49 (15)H8A—O8—H8B110.8
O3—Cu2—Cl291.29 (15)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+1, z; (iii) x, y, z+1; (iv) x+1, y, z1; (v) x+2, y, z1; (vi) x, y+1, z; (vii) x+2, y+2, z; (viii) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8A···O5ix0.822.172.772 (14)130
O8—H8B···O5x0.972.293.126 (14)144
O8—H8B···O8xi0.971.752.47 (3)129
Symmetry codes: (ix) x+1, y+1, z1; (x) x1, y, z; (xi) x, y+1, z1.

Experimental details

Crystal data
Chemical formulaMoCu3TeO7Cl2·0.5H2O
Mr606.07
Crystal system, space groupTriclinic, P1
Temperature (K)291
a, b, c (Å)6.1393 (15), 6.386 (2), 12.005 (3)
α, β, γ (°)81.75 (4), 85.76 (3), 86.18 (3)
V3)463.8 (2)
Z2
Radiation typeMo Kα
µ (mm1)11.77
Crystal size (mm)0.08 × 0.04 × 0.01
Data collection
DiffractometerStoe IPDS
diffractometer
Absorption correctionNumerical
(X-RED; Stoe & Cie, 2001)
Tmin, Tmax0.37, 0.524
No. of measured, independent and
observed [I > 2σ(I)] reflections
13580, 2214, 1677
Rint0.094
(sin θ/λ)max1)0.662
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.054, 0.85
No. of reflections2214
No. of parameters131
No. of restraints12
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.18, 0.93

Computer programs: EXPOSE in IPDS Software (Stoe & Cie, 1997), CELL in IPDS Software, INTEGRATE in IPDS Software, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Bergerhoff, 1996), WinGX (Farrugia, 1999).

Selected bond lengths (Å) top
Te—O7i1.876 (4)Cu1—O41.962 (4)
Te—O41.887 (4)Cu1—Cl2vi2.9452 (17)
Te—O2ii1.892 (4)Cu2—O11.914 (4)
Te—O5iii2.836 (5)Cu2—O31.927 (5)
Mo—O51.698 (5)Cu2—O61.975 (4)
Mo—O3iv1.745 (4)Cu2—Cl22.2474 (18)
Mo—O11.911 (4)Cu2—Cl12.7192 (19)
Mo—O6v1.920 (4)Cu3—O71.933 (4)
Mo—O1v2.085 (4)Cu3—O21.934 (4)
Mo—O8iv2.495 (13)Cu3—O7i1.992 (4)
Cu1—O6vi1.923 (4)Cu3—Cl12.2628 (17)
Cu1—O21.933 (4)Cu3—Cl2vi2.7259 (19)
Cu1—O4vii1.957 (4)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+1, z; (iii) x, y, z+1; (iv) x+1, y, z1; (v) x+2, y, z1; (vi) x, y+1, z; (vii) x+2, y+2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8A···O5viii0.822.172.772 (14)130
O8—H8B···O5ix0.972.293.126 (14)144
O8—H8B···O8x0.971.752.47 (3)129
Symmetry codes: (viii) x+1, y+1, z1; (ix) x1, y, z; (x) x, y+1, z1.
 

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