Three orthorhombic crystals of chemical formula EuxVyMo8±zO14 were investigated by X-ray diffraction (Mo Kα radiation, λ = 0.71073 Å). They have nearly the same lattice parameters (a ≃ 11.3, b ≃ 10.0, c ≃ 9.2 Å), display one-dimensional incommensurate modulations of wavevector q* = γc* and are characterized by the same superspace group Cmca(00γ)s00. The crystals differ both in their compositions (namely Eu0.976(6)V1.13(5)Mo7.10(5)O14, Eu0.986(4)V1.10(3)Mo7.30(1)O14 and EuMo7.96(1)O14) and in their γ components [0.195 (2), 0.245 (2) and 0.286 (3), respectively]. The average structures of these crystals appear closely related to the structures of LaMo7.7O14 (not modulated) and LaMo8O14 (modulated); however, two main differences are outlined: first, the modulation direction is c in the Eu-containing crystals but b in the modulated La-containing crystal [q* = (1/3)b*], second, the Eu-containing crystals have centrosymmetric structures while the La-containing crystals have polar structures (space group C2ca). The Mo (or Mo and V) atoms are stacked to form (001) layers of metallic clusters. The density modulation of these structures implies the existence of the new types of clusters Mo9, Mo10, Mo6V4, Mo7V3 and Mo8V2 besides the clusters M8 (Mo8, Mo6V2 and Mo7V) and M7 (Mo7 and Mo6V) which are already known. Mo8 units with cis and trans configurations and Mo6V2 units with a trans configuration appear as the main cluster types in these crystals. The nature of the metallic clusters changes along c, but inside one (001) layer it is likely that only one cluster type with a given configuration is present. The main structural result is the formation, in some unit cells, of strong intercluster Mo—Mo, Mo—V or V—V bonds with distances close to 2.6 Å within a layer as well as between two neighbouring layers.
Supporting information
| Crystallographic Information File (CIF) Contains datablocks Crystal1, Crystal2, Crystal3 |
| Structure factor file (CIF format) Contains datablock Crystal1 |
| Structure factor file (CIF format) Contains datablock Crystal2 |
| Structure factor file (CIF format) Contains datablock Crystal3 |
Crystal data top
Eu0.976(6)V1.13(5)Mo7.10(5)O14 | F(000) = 1992 |
Mr = ? | Dx = 7.02 Mg m−3 |
Orthorhombic, ? | Mo Kα radiation, λ = 0.71073 Å |
q = 0.195(2)c* | Cell parameters from 25 reflections |
a = 11.306 (1) Å | θ = 18–25° |
b = 10.025 (1) Å | µ = 14.8 mm−1 |
c = 9.254 (1) Å | T = 293 K |
V = 1048.9 (2) Å3 | × × mm |
Z = 4 | |
Data collection top
CAD4 diffractometer | θmax = 45.0°, θmin = 3.5° |
θ/2/3θ scans | h = 0→22 |
Absorption correction: gaussian ? | k = 0→19 |
Tmin = 0.26, Tmax = 0.42 | l = 0→18 |
13556 measured reflections | 3 standard reflections every 3600 min |
2711 reflections with I > 3σ(I) | intensity decay: 0.1% |
Rint = 0.030 | |
Refinement top
Refinement on F | Unit |
R[F2 > 2σ(F2)] = 0.041 | (Δ/σ)max = 0.002 |
wR(F2) = 0.0481 | Δρmax = 3.5 e Å−3 |
132 parameters | Δρmin = −3.6 e Å−3 |
Crystal data top
Eu0.976(6)V1.13(5)Mo7.10(5)O14 | V = 1048.9 (2) Å3 |
Mr = ? | Z = 4 |
Orthorhombic, ? | Mo Kα radiation |
q = 0.195(2)c* | µ = 14.8 mm−1 |
a = 11.306 (1) Å | T = 293 K |
b = 10.025 (1) Å | × × mm |
c = 9.254 (1) Å | |
Data collection top
CAD4 diffractometer | 2711 reflections with I > 3σ(I) |
Absorption correction: gaussian ? | Rint = 0.030 |
Tmin = 0.26, Tmax = 0.42 | 3 standard reflections every 3600 min |
13556 measured reflections | intensity decay: 0.1% |
Refinement top
R[F2 > 2σ(F2)] = 0.041 | Δρmax = 3.5 e Å−3 |
wR(F2) = 0.0481 | Δρmin = −3.6 e Å−3 |
132 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Eu | 0.0022 (8) | 0 | 0 | 0.0200 (5) | 0.488 (3) |
Mo1 | −0.12075 (4) | 0.07793 (4) | 0.37758 (4) | 0.0054 (1) | 0.93 (1) |
V1 | −0.12075 (4) | 0.07793 (4) | 0.37758 (4) | 0.0054 (1) | 0.07 (1) |
Mo3 | 0 | −0.16077 (4) | 0.38118 (5) | 0.0063 (1) | 0.93 (1) |
V3 | 0 | −0.16077 (4) | 0.38118 (5) | 0.0063 (1) | 0.07 (1) |
Mo4 | 0.2331 (8) | −0.1609 (8) | 0.371 (1) | 0.0106 (1) | 0.380 (4) |
V4 | 0.2410 (6) | −0.1656 (5) | 0.3783 (7) | 0.0106 (1) | 0.178 (2) |
O1 | 0.2547 (5) | 0 | 0.5 | 0.0100 (7) | |
O2 | 0 | −0.1596 (4) | −0.2388 (4) | 0.0082 (6) | |
O3 | −0.1227 (3) | −0.0823 (3) | 0.2444 (4) | 0.0100 (5) | |
O5 | −0.25 | 0.1694 (4) | 0.25 | 0.0077 (7) | |
O6 | 0.1223 (3) | 0.2516 (3) | 0.4915 (4) | 0.0111 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Eu | 0.023 (1) | 0.029 (2) | 0.0097 (5) | 0 | 0 | −0.009 (1) |
Mo1 | 0.0043 (1) | 0.0060 (1) | 0.0059 (1) | 0.0007 (1) | −0.0005 (1) | 0.0015 (1) |
V1 | 0.0043 (1) | 0.0060 (1) | 0.0059 (1) | 0.0007 (1) | −0.0005 (1) | 0.0015 (1) |
Mo3 | 0.0088 (2) | 0.0046 (2) | 0.0055 (2) | 0 | 0 | 0.0004 (1) |
V3 | 0.0088 (2) | 0.0046 (2) | 0.0055 (2) | 0 | 0 | 0.0004 (1) |
Mo4 | 0.010 (2) | 0.011 (2) | 0.010 (2) | −0.004 (1) | −0.008 (1) | 0.008 (1) |
V4 | 0.010 (2) | 0.011 (2) | 0.010 (2) | −0.004 (1) | −0.008 (1) | 0.008 (1) |
Bond lengths (Å) top
Eu—Eu | 0.631 (3) | Mo4—O3 | 1.885 (6) |
Eu—Mo4 | 3.366 (5) | Mo4—O3 | 2.101 (6) |
Eu—Mo4 | 3.366 (5) | Mo4—O5 | 2.044 (7) |
Eu—V4 | 3.294 (2) | Mo4—O5 | 3.514 (5) |
Eu—V4 | 3.294 (2) | Mo4—O5 | 3.501 (7) |
Eu—O1 | 3.089 (6) | Mo4—O6 | 2.164 (6) |
Eu—O1 | 2.457 (6) | Mo4—O6 | 2.004 (6) |
Eu—O2 | 2.746 (4) | V4—V4 | 2.824 |
Eu—O2 | 2.746 (4) | V4—V4 | 2.3837 |
Eu—O3 | 2.949 (4) | V4—O1 | 2.0121 (4) |
Eu—O3 | 2.635 (4) | V4—O3 | 2.006 (3) |
Eu—O3 | 2.635 (4) | V4—O3 | 2.088 (3) |
Eu—O3 | 2.949 (4) | V4—O5 | 2.038 (4) |
Eu—O6 | 2.711 (4) | V4—O6 | 2.043 (3) |
Eu—O6 | 3.016 (4) | V4—O6 | 1.998 (3) |
Eu—O6 | 3.016 (4) | O1—O3 | 2.916 (4) |
Eu—O6 | 2.711 (4) | O1—O3 | 2.916 (4) |
Mo1—Mo1 | 2.7304 (6) | O1—O3 | 2.777 (4) |
Mo1—Mo1 | 2.7522 (5) | O1—O3 | 2.777 (4) |
Mo1—Mo3 | 2.7553 (6) | O1—O5 | 2.871 (2) |
Mo1—Mo3 | 2.7453 (6) | O1—O5 | 2.871 (2) |
Mo1—Mo4 | 3.096 (5) | O1—O6 | 2.934 (4) |
Mo1—Mo4 | 2.780 (5) | O1—O6 | 2.853 (4) |
Mo1—Mo4 | 2.712 (5) | O1—O6 | 2.853 (4) |
Mo1—V4 | 3.0087 (4) | O1—O6 | 2.934 (4) |
Mo1—V4 | 2.7792 (4) | O2—O3 | 2.794 (5) |
Mo1—V4 | 2.7946 (4) | O2—O3 | 2.794 (5) |
Mo1—O1 | 2.046 (4) | O2—O3 | 2.941 (5) |
Mo1—O2 | 2.045 (3) | O2—O3 | 2.941 (5) |
Mo1—O3 | 2.025 (3) | O2—O5 | 2.8301 (3) |
Mo1—O5 | 2.091 (2) | O2—O5 | 2.8301 (3) |
Mo1—O6 | 2.035 (3) | O2—O6 | 2.870 (5) |
Mo3—Mo4 | 2.638 (5) | O2—O6 | 2.870 (5) |
Mo3—Mo4 | 2.638 (5) | O2—O6 | 2.818 (5) |
Mo3—V4 | 2.7255 | O2—O6 | 2.818 (5) |
Mo3—V4 | 2.7255 | O3—O3 | 2.775 (4) |
Mo3—O2 | 2.116 (4) | O3—O3 | 2.880 (4) |
Mo3—O3 | 2.036 (3) | O3—O5 | 2.905 (5) |
Mo3—O3 | 2.036 (3) | O3—O5 | 2.875 (5) |
Mo3—O6 | 2.032 (3) | O3—O6 | 2.976 (5) |
Mo3—O6 | 2.032 (3) | O3—O6 | 2.746 (5) |
Mo4—Mo4 | 3.007 (8) | O5—O6 | 2.785 (4) |
Mo4—Mo4 | 2.270 (7) | O5—O6 | 2.904 (4) |
Mo4—V4 | 0.122 (5) | O5—O6 | 2.904 (4) |
Mo4—V4 | 2.914 (5) | O5—O6 | 2.785 (4) |
Mo4—V4 | 2.325 (5) | O6—O6 | 2.891 (5) |
Mo4—O1 | 2.023 (5) | O6—O6 | 2.766 (5) |
Mo4—O2 | 3.349 (6) | | |
Crystal data top
Eu0.986(4)V1.10(3)Mo7.30(1)O14 | F(000) = 2024 |
Mr = ? | Dx = 7.15 Mg m−3 |
Orthorhombic, ? | Mo Kα radiation, λ = 0.71073 Å |
q = 0.245(2)c* | Cell parameters from 25 reflections |
a = 11.325 (1) Å | θ = 18–25° |
b = 10.024 (1) Å | µ = 15.2 mm−1 |
c = 9.240 (1) Å | T = 293 K |
V = 1048.9 (2) Å3 | × × mm |
Z = 4 | |
Data collection top
CAD4 diffractometer | θmax = 45.0°, θmin = 3.5° |
θ/θ scans | h = 0→22 |
Absorption correction: gaussian ? | k = 0→19 |
Tmin = 0.23, Tmax = 0.49 | l = 0→18 |
13556 measured reflections | 3 standard reflections every 3600 min |
2423 reflections with I > 3σ(I) | intensity decay: 0.1% |
Rint = 0.031 | |
Refinement top
Refinement on F | Unit |
R[F2 > 2σ(F2)] = 0.041 | (Δ/σ)max = 0.002 |
wR(F2) = 0.0449 | Δρmax = 3.0 e Å−3 |
134 parameters | Δρmin = −3.7 e Å−3 |
Crystal data top
Eu0.986(4)V1.10(3)Mo7.30(1)O14 | V = 1048.9 (2) Å3 |
Mr = ? | Z = 4 |
Orthorhombic, ? | Mo Kα radiation |
q = 0.245(2)c* | µ = 15.2 mm−1 |
a = 11.325 (1) Å | T = 293 K |
b = 10.024 (1) Å | × × mm |
c = 9.240 (1) Å | |
Data collection top
CAD4 diffractometer | 2423 reflections with I > 3σ(I) |
Absorption correction: gaussian ? | Rint = 0.031 |
Tmin = 0.23, Tmax = 0.49 | 3 standard reflections every 3600 min |
13556 measured reflections | intensity decay: 0.1% |
Refinement top
R[F2 > 2σ(F2)] = 0.041 | Δρmax = 3.0 e Å−3 |
wR(F2) = 0.0449 | Δρmin = −3.7 e Å−3 |
134 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Eu | 0.0021 (6) | 0 | 0 | 0.0180 (5) | 0.493 (2) |
Mo1 | −0.12057 (4) | 0.07766 (4) | 0.37728 (4) | 0.00516 (6) | |
Mo3 | 0 | −0.16060 (5) | 0.38162 (5) | 0.00603 (8) | |
Mo4 | 0.238 (1) | −0.159 (1) | 0.371 (3) | 0.016 (5) | 0.325 (3) |
V4 | 0.2424 (5) | −0.1676 (4) | 0.377 (3) | 0.016 (5) | 0.274 (6) |
O1 | 0.2531 (4) | 0 | 0.5 | 0.008 (1) | |
O2 | 0 | −0.1589 (4) | −0.2385 (5) | 0.0071 (6) | |
O3 | −0.1224 (3) | −0.0835 (3) | 0.2449 (4) | 0.0094 (5) | |
O5 | −0.25 | 0.1684 (5) | 0.25 | 0.0071 (8) | |
O6 | 0.1221 (3) | 0.2508 (3) | 0.4910 (4) | 0.0090 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Eu | 0.020 (1) | 0.024 (2) | 0.0087 (5) | 0 | 0 | −0.006 (1) |
Mo1 | 0.0047 (1) | 0.0068 (1) | 0.0039 (1) | 0.0004 (1) | −0.0003 (1) | 0.0013 (1) |
Mo3 | 0.0092 (2) | 0.0051 (2) | 0.0038 (2) | 0 | 0 | 0.0006 (1) |
Mo4 | 0.023 (2) | 0.017 (2) | 0.009 (1) | −0.008 (1) | −0.011 (1) | 0.004 (1) |
V4 | 0.023 (2) | 0.017 (2) | 0.009 (1) | −0.008 (1) | −0.011 (1) | 0.004 (1) |
Bond lengths (Å) top
Eu—Eu | 0.664 (3) | Mo3—O2 | 2.122 (4) |
Eu—Mo4 | 3.31 (1) | Mo3—O3 | 2.029 (3) |
Eu—Mo4 | 3.31 (1) | Mo3—O3 | 2.029 (3) |
Eu—V4 | 3.285 (2) | Mo3—O6 | 2.029 (3) |
Eu—V4 | 3.285 (2) | Mo3—O6 | 2.029 (3) |
Eu—O1 | 3.128 (6) | Mo4—Eu | 3.31 (1) |
Eu—O1 | 2.464 (6) | Mo4—Mo1 | 3.09 (1) |
Eu—O2 | 2.739 (4) | Mo4—Mo1 | 2.81 (1) |
Eu—O2 | 2.739 (4) | Mo4—Mo1 | 2.72 (1) |
Eu—O3 | 2.962 (4) | Mo4—Mo3 | 2.70 (1) |
Eu—O3 | 2.633 (4) | Mo4—Mo4 | 3.02 (2) |
Eu—O3 | 2.633 (4) | Mo4—Mo4 | 2.24 (2) |
Eu—O3 | 2.962 (4) | Mo4—V4 | 0.12 (1) |
Eu—O6 | 2.711 (4) | Mo4—V4 | 2.91 (1) |
Eu—O6 | 3.031 (4) | Mo4—V4 | 2.30 (1) |
Eu—O6 | 3.031 (4) | Mo4—O1 | 2.00 (1) |
Eu—O6 | 2.711 (4) | Mo4—O2 | 3.41 (1) |
Mo1—Mo1 | 2.7309 (6) | Mo4—O3 | 1.91 (1) |
Mo1—Mo1 | 2.7509 (5) | Mo4—O3 | 2.05 (1) |
Mo1—Mo3 | 2.7513 (6) | Mo4—O5 | 2.06 (1) |
Mo1—Mo3 | 2.7420 (6) | Mo4—O5 | 3.51 (1) |
Mo1—Mo4 | 3.09 (1) | Mo4—O5 | 3.47 (1) |
Mo1—Mo4 | 2.81 (1) | Mo4—O6 | 2.14 (1) |
Mo1—Mo4 | 2.72 (1) | Mo4—O6 | 2.05 (1) |
Mo1—V4 | 2.9867 (4) | V4—Eu | 3.285 (2) |
Mo1—V4 | 2.8007 (4) | V4—Mo1 | 2.9867 (4) |
Mo1—V4 | 2.8205 (4) | V4—Mo1 | 2.8007 (4) |
Mo1—O1 | 2.036 (4) | V4—Mo1 | 2.8205 (4) |
Mo1—O2 | 2.043 (3) | V4—Mo3 | 2.7463 |
Mo1—O3 | 2.027 (3) | V4—Mo4 | 0.12 (1) |
Mo1—O5 | 2.088 (2) | V4—Mo4 | 2.91 (1) |
Mo1—O6 | 2.029 (4) | V4—Mo4 | 2.30 (1) |
Mo3—Mo1 | 2.7513 (6) | V4—V4 | 2.8026 |
Mo3—Mo1 | 2.7420 (6) | V4—V4 | 2.3663 |
Mo3—Mo1 | 2.7513 (6) | V4—O1 | 2.0295 (3) |
Mo3—Mo1 | 2.7420 (6) | V4—O3 | 2.016 (3) |
Mo3—Mo4 | 2.70 (1) | V4—O3 | 2.083 (3) |
Mo3—Mo4 | 2.70 (1) | V4—O5 | 2.024 (4) |
Mo3—V4 | 2.7463 | V4—O6 | 2.029 (3) |
Mo3—V4 | 2.7463 | V4—O6 | 2.005 (3) |
Crystal data top
EuMo7.96(1)O14 | F(000) = 2038 |
Mr = ? | Dx = 7.20 Mg m−3 |
Orthorhombic, ? | Mo Kα radiation, λ = 0.71073 Å |
q = 0.286(3)c* | Cell parameters from 25 reflections |
a = 11.315 (1) Å | θ = 18–25° |
b = 10.035 (1 Å | µ = 14.9 mm−1 |
c = 9.265 (1) Å | T = 293 K |
V = 1052 (2) Å3 | × × mm |
Z = 4 | |
Data collection top
CAD4 diffractometer | θmax = 45.0°, θmin = 3.5° |
θ/θ scans | h = 0→22 |
Absorption correction: gaussian ? | k = 0→19 |
Tmin = 0.21, Tmax = 0.52 | l = 0→18 |
13556 measured reflections | 3 standard reflections every 3600 min |
2695 reflections with I > 3σ(I) | intensity decay: 0.2% |
Rint = 0.029 | |
Refinement top
Refinement on F | Unit |
R[F2 > 2σ(F2)] = 0.048 | (Δ/σ)max = 0.010 |
wR(F2) = 0.0553 | Δρmax = 4.0 e Å−3 |
120 parameters | Δρmin = −4.4 e Å−3 |
Crystal data top
EuMo7.96(1)O14 | V = 1052 (2) Å3 |
Mr = ? | Z = 4 |
Orthorhombic, ? | Mo Kα radiation |
q = 0.286(3)c* | µ = 14.9 mm−1 |
a = 11.315 (1) Å | T = 293 K |
b = 10.035 (1 Å | × × mm |
c = 9.265 (1) Å | |
Data collection top
CAD4 diffractometer | 2695 reflections with I > 3σ(I) |
Absorption correction: gaussian ? | Rint = 0.029 |
Tmin = 0.21, Tmax = 0.52 | 3 standard reflections every 3600 min |
13556 measured reflections | intensity decay: 0.2% |
Refinement top
R[F2 > 2σ(F2)] = 0.048 | Δρmax = 4.0 e Å−3 |
wR(F2) = 0.0553 | Δρmin = −4.4 e Å−3 |
120 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Eu | 0.006 (3) | 0 | 0 | 0.0149 (5) | 0.500 (2) |
Mo1 | −0.12065 (2) | 0.07781 (2) | 0.37760 (2) | 0.00452 (3) | |
Mo3 | 0 | −0.16072 (2) | 0.38119 (3) | 0.00622 (4) | |
Mo4 | 0.2378 (2) | −0.1623 (2) | 0.3726 (7) | 0.0120 (3) | 0.489 (2) |
O1 | 0.2544 (3) | 0 | 0.5 | 0.0084 (5) | |
O2 | 0 | −0.1588 (2) | −0.2390 (2) | 0.0062 (3) | |
O3 | −0.1223 (2) | −0.0828 (2) | 0.2444 (2) | 0.0092 (2) | |
O5 | −0.25 | 0.1692 (2) | 0.25 | 0.0062 (4) | |
O6 | 0.1219 (2) | 0.2516 (2) | 0.4914 (2) | 0.0095 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Eu | 0.0176 (6) | 0.0154 (8) | 0.0089 (2) | 0 | 0 | −0.0034 (5) |
Mo1 | 0.0033 (1) | 0.0067 (1) | 0.0036 (1) | 0.0004 (1) | −0.0004 (1) | 0.0013 (1) |
Mo3 | 0.0081 (1) | 0.0043 (1) | 0.0032 (1) | 0 | 0 | 0.0002 (1) |
Mo4 | 0.0173 (7) | 0.0080 (5) | 0.0105 (5) | −0.0049 (1) | −0.0095 (6) | 0.0041 (5) |
Bond lengths (Å) top
Eu—Eu | 0.6063 (9) | Mo4—O3 | 1.938 (4) |
Eu—Mo4 | 3.338 (3) | Mo4—O3 | 2.077 (4) |
Eu—Mo4 | 3.338 (3) | Mo4—O5 | 2.042 (4) |
Eu—O1 | 3.082 (3) | Mo4—O6 | 2.116 (4) |
Eu—O1 | 2.475 (3) | Mo4—O6 | 2.027 (4) |
Eu—O2 | 2.745 (2) | O1—O3 | 2.921 (2) |
Eu—O2 | 2.745 (2) | O1—O3 | 2.921 (2) |
Eu—O3 | 2.944 (2) | O1—O3 | 2.786 (2) |
Eu—O3 | 2.643 (2) | O1—O3 | 2.786 (2) |
Eu—O3 | 2.643 (2) | O1—O5 | 2.872 (1) |
Eu—O3 | 2.944 (2) | O1—O5 | 2.872 (1) |
Eu—O6 | 2.717 (2) | O1—O6 | 2.937 (2) |
Eu—O6 | 3.009 (2) | O1—O6 | 2.860 (2) |
Eu—O6 | 3.009 (2) | O1—O6 | 2.860 (2) |
Eu—O6 | 2.717 (2) | O1—O6 | 2.937 (2) |
Mo1—Mo1 | 2.7302 (3) | O2—O3 | 2.793 (2) |
Mo1—Mo1 | 2.7538 (3) | O2—O3 | 2.793 (2) |
Mo1—Mo3 | 2.7558 (3) | O2—O3 | 2.943 (2) |
Mo1—Mo3 | 2.7478 (3) | O2—O3 | 2.943 (2) |
Mo1—Mo4 | 3.060 (2) | O2—O5 | 2.8325 (1) |
Mo1—Mo4 | 2.799 (5) | O2—O5 | 2.8325 (1) |
Mo1—Mo4 | 2.751 (2) | O2—O6 | 2.870 (3) |
Mo1—O1 | 2.046 (2) | O2—O6 | 2.870 (3) |
Mo1—O2 | 2.043 (2) | O2—O6 | 2.824 (3) |
Mo1—O3 | 2.030 (2) | O2—O6 | 2.824 (3) |
Mo1—O5 | 2.093 (1) | O3—O3 | 2.768 (2) |
Mo1—O6 | 2.038 (2) | O3—O3 | 2.891 (2) |
Mo3—Mo4 | 2.692 (2) | O3—O5 | 2.913 (2) |
Mo3—Mo4 | 2.692 (2) | O3—O5 | 2.878 (2) |
Mo3—O2 | 2.126 (2) | O3—O6 | 2.977 (2) |
Mo3—O3 | 2.033 (2) | O3—O6 | 2.745 (2) |
Mo3—O3 | 2.033 (2) | O5—O6 | 2.790 (2) |
Mo3—O6 | 2.032 (2) | O5—O6 | 2.911 (2) |
Mo3—O6 | 2.032 (2) | O5—O6 | 2.911 (2) |
Mo4—Mo4 | 2.958 (7) | O5—O6 | 2.790 (2) |
Mo4—Mo4 | 2.288 (9) | O6—O6 | 2.902 (2) |
Mo4—O1 | 2.021 (4) | O6—O6 | 2.760 (2) |
Experimental details
| (Crystal1) | (Crystal2) | (Crystal3) |
Crystal data |
Chemical formula | Eu0.976(6)V1.13(5)Mo7.10(5)O14 | Eu0.986(4)V1.10(3)Mo7.30(1)O14 | EuMo7.96(1)O14 |
Mr | ? | ? | ? |
Crystal system, space group | Orthorhombic, ? | Orthorhombic, ? | Orthorhombic, ? |
Temperature (K) | 293 | 293 | 293 |
Wave vectors | q = 0.195(2)c* | q = 0.245(2)c* | q = 0.286(3)c* |
a, b, c (Å) | 11.306 (1), 10.025 (1), 9.254 (1) | 11.325 (1), 10.024 (1), 9.240 (1) | 11.315 (1), 10.035 (1, 9.265 (1) |
V (Å3) | 1048.9 (2) | 1048.9 (2) | 1052 (2) |
Z | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 14.8 | 15.2 | 14.9 |
Crystal size (mm) | × × | × × | × × |
|
Data collection |
Diffractometer | CAD4 diffractometer | CAD4 diffractometer | CAD4 diffractometer |
Absorption correction | Gaussian | Gaussian | Gaussian |
Tmin, Tmax | 0.26, 0.42 | 0.23, 0.49 | 0.21, 0.52 |
No. of measured, independent and observed [I > 3σ(I)] reflections | 13556, ?, 2711 | 13556, ?, 2423 | 13556, ?, 2695 |
Rint | 0.030 | 0.031 | 0.029 |
(sin θ/λ)max (Å−1) | 0.995 | 0.995 | 0.995 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.0481, ? | 0.041, 0.0449, ? | 0.048, 0.0553, ? |
No. of reflections | ? | ? | ? |
No. of parameters | 132 | 134 | 120 |
No. of restraints | ? | ? | ? |
Δρmax, Δρmin (e Å−3) | 3.5, −3.6 | 3.0, −3.7 | 4.0, −4.4 |