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The crystal structures of the rare-earth members of the series RMo5O8 (R = Ce to Eu) have been investigated and compared with those of the La and Gd members previously published in order to understand the influences of the size and the charge of the cation on the different Mo-Mo bonds. The RMo5O8 compounds crystallize in the monoclinic space group P21/c. Their crystal structure is characterized by bioctahedral Mo10 clusters forming extended chains. The results of our single-crystal studies show that the modification of charge predominantly affects the Mo-Mo bonds between the Mo10 clusters and, to a lesser extent, the intra-cluster distances, while the cationic size induces only small variations. Theoretical investigations confirm this statement and allow the understanding of the bonding mode in these compounds.
Supporting information
For all compounds, data collection: COLLECT (Nonius, 1998); cell refinement: COLLECT; data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); 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: SHELXL97 (Sheldrick, 1997).
Crystal data top
CeMo5O8 | F(000) = 1328 |
Mr = 747.82 | Dx = 7.733 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71070 Å |
a = 7.5643 (1) Å | Cell parameters from 9841 reflections |
b = 9.0693 (1) Å | θ = 1–37.8° |
c = 9.9150 (2) Å | µ = 16.42 mm−1 |
β = 109.2113 (8)° | T = 293 K |
V = 642.32 (2) Å3 | Plate, black |
Z = 4 | 0.14 × 0.10 × 0.08 mm |
Data collection top
Nonius KappaCCD diffractometer | 3402 independent reflections |
Radiation source: fine-focus sealed tube | 3314 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.064 |
ϕ scans (κ = 0) + additional ω scans | θmax = 37.8°, θmin = 2.9° |
Absorption correction: gaussian '(Coppens, P., Leiserowitz, L. & Rabinovich, D. 1965)' | h = −12→11 |
Tmin = 0.064, Tmax = 0.181 | k = −15→15 |
12944 measured reflections | l = −12→17 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | w = 1/[σ2(Fo2) + (0.P)2 + 7.228P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.080 | (Δ/σ)max = 0.001 |
S = 1.26 | Δρmax = 2.54 e Å−3 |
3402 reflections | Δρmin = −2.50 e Å−3 |
128 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0171 (5) |
Crystal data top
CeMo5O8 | V = 642.32 (2) Å3 |
Mr = 747.82 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 7.5643 (1) Å | µ = 16.42 mm−1 |
b = 9.0693 (1) Å | T = 293 K |
c = 9.9150 (2) Å | 0.14 × 0.10 × 0.08 mm |
β = 109.2113 (8)° | |
Data collection top
Nonius KappaCCD diffractometer | 3402 independent reflections |
Absorption correction: gaussian '(Coppens, P., Leiserowitz, L. & Rabinovich, D. 1965)' | 3314 reflections with I > 2σ(I) |
Tmin = 0.064, Tmax = 0.181 | Rint = 0.064 |
12944 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.034 | 128 parameters |
wR(F2) = 0.080 | 0 restraints |
S = 1.26 | Δρmax = 2.54 e Å−3 |
3402 reflections | Δρmin = −2.50 e Å−3 |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ce | 0.26252 (3) | 0.50415 (3) | 0.53794 (2) | 0.00673 (7) | |
Mo1 | 0.60444 (5) | −0.11531 (4) | 0.48646 (3) | 0.00391 (7) | |
Mo2 | 0.38347 (5) | −0.11788 (4) | 0.67714 (4) | 0.00413 (7) | |
Mo3 | 0.17299 (5) | −0.12687 (4) | 0.38284 (4) | 0.00336 (7) | |
Mo4 | 0.80812 (5) | −0.12971 (4) | 0.29777 (3) | 0.00328 (7) | |
Mo5 | −0.00249 (5) | −0.12281 (4) | 0.58641 (3) | 0.00341 (7) | |
O1 | 0.3976 (4) | 0.0053 (3) | 0.8493 (3) | 0.0061 (5) | |
O2 | −0.0012 (4) | −0.2222 (3) | 0.9329 (3) | 0.0057 (5) | |
O3 | −0.0137 (5) | 0.0023 (3) | 0.2307 (3) | 0.0059 (5) | |
O4 | 0.3915 (4) | −0.2475 (4) | 0.0123 (3) | 0.0062 (5) | |
O5 | 0.7951 (4) | −0.2418 (4) | 0.1142 (3) | 0.0055 (5) | |
O6 | 0.1998 (4) | −0.2396 (4) | 0.2091 (3) | 0.0065 (5) | |
O7 | 0.6056 (4) | −0.2356 (3) | 0.8292 (3) | 0.0056 (5) | |
O8 | 0.3831 (4) | −0.0071 (3) | 0.3277 (3) | 0.0062 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ce | 0.00588 (10) | 0.00733 (10) | 0.00682 (10) | −0.00032 (6) | 0.00188 (7) | 0.00051 (6) |
Mo1 | 0.00351 (13) | 0.00360 (13) | 0.00403 (13) | 0.00009 (9) | 0.00045 (10) | −0.00009 (9) |
Mo2 | 0.00385 (13) | 0.00450 (13) | 0.00342 (13) | −0.00034 (9) | 0.00037 (10) | 0.00055 (9) |
Mo3 | 0.00327 (13) | 0.00388 (13) | 0.00301 (13) | 0.00020 (9) | 0.00114 (10) | −0.00017 (9) |
Mo4 | 0.00318 (13) | 0.00376 (12) | 0.00289 (13) | −0.00009 (9) | 0.00100 (10) | −0.00021 (9) |
Mo5 | 0.00331 (14) | 0.00362 (13) | 0.00323 (13) | −0.00013 (9) | 0.00099 (10) | 0.00020 (9) |
O1 | 0.0045 (12) | 0.0073 (12) | 0.0056 (11) | 0.0022 (9) | 0.0004 (9) | 0.0000 (9) |
O2 | 0.0064 (12) | 0.0057 (11) | 0.0043 (10) | −0.0010 (9) | 0.0007 (9) | 0.0004 (9) |
O3 | 0.0060 (12) | 0.0054 (11) | 0.0066 (12) | −0.0006 (9) | 0.0025 (10) | 0.0012 (9) |
O4 | 0.0061 (11) | 0.0066 (11) | 0.0072 (11) | −0.0008 (9) | 0.0040 (9) | −0.0014 (9) |
O5 | 0.0042 (11) | 0.0074 (11) | 0.0052 (11) | −0.0002 (9) | 0.0022 (9) | −0.0023 (9) |
O6 | 0.0038 (11) | 0.0091 (12) | 0.0066 (11) | 0.0000 (9) | 0.0015 (9) | −0.0020 (9) |
O7 | 0.0061 (11) | 0.0060 (11) | 0.0051 (10) | 0.0013 (9) | 0.0022 (9) | 0.0019 (9) |
O8 | 0.0033 (11) | 0.0078 (12) | 0.0070 (11) | −0.0020 (9) | 0.0012 (9) | 0.0013 (9) |
Geometric parameters (Å, º) top
Ce—O1i | 2.410 (3) | Mo2—Mo3 | 2.8282 (5) |
Ce—O1ii | 2.443 (3) | Mo2—Cexi | 3.3761 (4) |
Ce—O4iii | 2.459 (3) | Mo3—O3 | 2.059 (3) |
Ce—O7ii | 2.568 (3) | Mo3—O4vii | 2.069 (3) |
Ce—O5iv | 2.648 (3) | Mo3—O2viii | 2.070 (3) |
Ce—O3v | 2.709 (3) | Mo3—O6 | 2.070 (3) |
Ce—O8iii | 2.713 (3) | Mo3—O8 | 2.140 (3) |
Ce—O2i | 2.758 (3) | Mo3—Mo4xii | 2.6072 (5) |
Ce—O6iii | 2.862 (3) | Mo3—Mo5xiii | 2.6726 (5) |
Ce—O2vi | 2.930 (3) | Mo3—Mo5 | 2.7569 (5) |
Ce—Mo2ii | 3.3761 (4) | Mo3—Mo1ix | 2.8111 (5) |
Ce—Mo4iv | 3.4159 (4) | Mo3—Cexiv | 3.6519 (4) |
Mo1—O5vii | 2.040 (3) | Mo4—O5 | 2.059 (3) |
Mo1—O7viii | 2.066 (3) | Mo4—O7viii | 2.062 (3) |
Mo1—O4vii | 2.117 (3) | Mo4—O3x | 2.070 (3) |
Mo1—O8 | 2.124 (3) | Mo4—O1ix | 2.080 (3) |
Mo1—O8ix | 2.126 (3) | Mo4—O2xv | 2.099 (3) |
Mo1—Mo2ix | 2.6851 (5) | Mo4—Mo3x | 2.6072 (5) |
Mo1—Mo1ix | 2.6874 (7) | Mo4—Mo2ix | 2.7279 (5) |
Mo1—Mo4 | 2.7906 (5) | Mo4—Mo5x | 2.7474 (5) |
Mo1—Mo5x | 2.8086 (5) | Mo4—Mo5ix | 2.7594 (5) |
Mo1—Mo3ix | 2.8111 (5) | Mo4—Cexvi | 3.4159 (4) |
Mo1—Mo2 | 2.9066 (5) | Mo5—O6vii | 2.038 (3) |
Mo1—Mo3 | 3.0840 (5) | Mo5—O5xvii | 2.051 (3) |
Mo2—O6vii | 1.997 (3) | Mo5—O2viii | 2.074 (3) |
Mo2—O1 | 2.013 (3) | Mo5—O3xiii | 2.086 (3) |
Mo2—O4vii | 2.057 (3) | Mo5—Mo3xiii | 2.6726 (5) |
Mo2—O8ix | 2.112 (3) | Mo5—Mo4xii | 2.7474 (5) |
Mo2—O7 | 2.138 (3) | Mo5—Mo4ix | 2.7594 (5) |
Mo2—Mo1ix | 2.6851 (5) | Mo5—Mo1xii | 2.8086 (5) |
Mo2—Mo4ix | 2.7279 (5) | Mo5—Mo5xiii | 2.8183 (6) |
Mo2—Mo5 | 2.7579 (5) | | |
| | | |
Mo1ix—O8—Cei | 144.69 (15) | Mo3—O8—Cei | 104.86 (12) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1, y+1/2, −z+3/2; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+1/2; (v) −x, y+1/2, −z+1/2; (vi) −x, y+1/2, −z+3/2; (vii) x, −y−1/2, z+1/2; (viii) x, −y−1/2, z−1/2; (ix) −x+1, −y, −z+1; (x) x+1, y, z; (xi) −x+1, y−1/2, −z+3/2; (xii) x−1, y, z; (xiii) −x, −y, −z+1; (xiv) x, y−1, z; (xv) x+1, −y−1/2, z−1/2; (xvi) −x+1, y−1/2, −z+1/2; (xvii) x−1, −y−1/2, z+1/2. |
Crystal data top
PrMo5O8 | F(000) = 1332 |
Mr = 748.61 | Dx = 7.754 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71070 Å |
a = 7.5662 (1) Å | Cell parameters from 11309 reflections |
b = 9.0569 (1) Å | θ = 1.0–37.8° |
c = 9.9175 (1) Å | µ = 16.94 mm−1 |
β = 109.3293 (7)° | T = 293 K |
V = 641.30 (1) Å3 | Irregular plate, black |
Z = 4 | 0.24 × 0.11 × 0.04 mm |
Data collection top
Nonius KappaCCD diffractometer | 3411 independent reflections |
Radiation source: fine-focus sealed tube | 3329 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.091 |
ϕ scans (κ = 0) + additional ω scans | θmax = 37.8°, θmin = 2.9° |
Absorption correction: gaussian '(Coppens, P., Leiserowitz, L. & Rabinovich, D. 1965)' | h = −12→12 |
Tmin = 0.090, Tmax = 0.524 | k = −15→15 |
14762 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.029 | w = 1/[σ2(Fo2) + (0.0145P)2 + 1.922P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.070 | (Δ/σ)max = 0.002 |
S = 1.19 | Δρmax = 2.45 e Å−3 |
3411 reflections | Δρmin = −3.32 e Å−3 |
128 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0874 (12) |
Crystal data top
PrMo5O8 | V = 641.30 (1) Å3 |
Mr = 748.61 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 7.5662 (1) Å | µ = 16.94 mm−1 |
b = 9.0569 (1) Å | T = 293 K |
c = 9.9175 (1) Å | 0.24 × 0.11 × 0.04 mm |
β = 109.3293 (7)° | |
Data collection top
Nonius KappaCCD diffractometer | 3411 independent reflections |
Absorption correction: gaussian '(Coppens, P., Leiserowitz, L. & Rabinovich, D. 1965)' | 3329 reflections with I > 2σ(I) |
Tmin = 0.090, Tmax = 0.524 | Rint = 0.091 |
14762 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.029 | 128 parameters |
wR(F2) = 0.070 | 0 restraints |
S = 1.19 | Δρmax = 2.45 e Å−3 |
3411 reflections | Δρmin = −3.32 e Å−3 |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pr | 0.26407 (2) | 0.504028 (15) | 0.536858 (16) | 0.00703 (6) | |
Mo1 | 0.60429 (3) | −0.11548 (2) | 0.48668 (2) | 0.00438 (6) | |
Mo2 | 0.38377 (3) | −0.11796 (2) | 0.67725 (2) | 0.00447 (6) | |
Mo3 | 0.17258 (3) | −0.12700 (2) | 0.38258 (2) | 0.00375 (6) | |
Mo4 | 0.80778 (3) | −0.12994 (2) | 0.29783 (2) | 0.00364 (6) | |
Mo5 | −0.00233 (3) | −0.12309 (2) | 0.58646 (2) | 0.00375 (6) | |
O1 | 0.3989 (3) | 0.00591 (19) | 0.8497 (2) | 0.0059 (3) | |
O2 | −0.0014 (3) | −0.2214 (2) | 0.9331 (2) | 0.0057 (3) | |
O3 | −0.0146 (3) | 0.00289 (19) | 0.2304 (2) | 0.0051 (3) | |
O4 | 0.3909 (3) | −0.2466 (2) | 0.0128 (2) | 0.0062 (3) | |
O5 | 0.7947 (3) | −0.2413 (2) | 0.1138 (2) | 0.0063 (3) | |
O6 | 0.2003 (3) | −0.2393 (2) | 0.2087 (2) | 0.0071 (3) | |
O7 | 0.6063 (3) | −0.2341 (2) | 0.8299 (2) | 0.0059 (3) | |
O8 | 0.3831 (3) | −0.0066 (2) | 0.3275 (2) | 0.0055 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pr | 0.00619 (8) | 0.00675 (8) | 0.00800 (8) | −0.00036 (4) | 0.00215 (5) | 0.00049 (4) |
Mo1 | 0.00409 (10) | 0.00307 (10) | 0.00532 (10) | 0.00013 (5) | 0.00065 (7) | −0.00010 (5) |
Mo2 | 0.00444 (10) | 0.00380 (10) | 0.00452 (10) | −0.00041 (6) | 0.00060 (7) | 0.00059 (6) |
Mo3 | 0.00380 (10) | 0.00336 (9) | 0.00415 (10) | 0.00010 (5) | 0.00141 (7) | −0.00021 (6) |
Mo4 | 0.00361 (10) | 0.00325 (9) | 0.00412 (10) | −0.00024 (5) | 0.00137 (7) | −0.00031 (6) |
Mo5 | 0.00379 (10) | 0.00313 (10) | 0.00425 (10) | −0.00006 (5) | 0.00123 (7) | 0.00023 (5) |
O1 | 0.0068 (8) | 0.0053 (8) | 0.0046 (8) | 0.0018 (5) | 0.0006 (6) | 0.0001 (5) |
O2 | 0.0066 (8) | 0.0042 (7) | 0.0062 (7) | −0.0006 (5) | 0.0021 (6) | −0.0005 (6) |
O3 | 0.0052 (8) | 0.0043 (7) | 0.0056 (8) | −0.0001 (5) | 0.0017 (6) | 0.0006 (5) |
O4 | 0.0056 (8) | 0.0058 (8) | 0.0079 (8) | −0.0008 (5) | 0.0030 (6) | −0.0017 (6) |
O5 | 0.0059 (8) | 0.0058 (7) | 0.0074 (8) | 0.0001 (6) | 0.0023 (6) | −0.0018 (6) |
O6 | 0.0055 (8) | 0.0078 (8) | 0.0075 (8) | −0.0002 (6) | 0.0014 (6) | −0.0035 (6) |
O7 | 0.0056 (8) | 0.0057 (7) | 0.0064 (7) | 0.0019 (6) | 0.0020 (6) | 0.0016 (6) |
O8 | 0.0038 (8) | 0.0065 (8) | 0.0067 (8) | −0.0013 (5) | 0.0023 (6) | 0.0011 (5) |
Geometric parameters (Å, º) top
Pr—O1i | 2.397 (2) | Mo2—Mo3 | 2.8300 (3) |
Pr—O1ii | 2.423 (2) | Mo2—Prxi | 3.3702 (3) |
Pr—O4iii | 2.440 (2) | Mo3—O3 | 2.062 (2) |
Pr—O7ii | 2.550 (2) | Mo3—O6 | 2.0715 (19) |
Pr—O5iv | 2.632 (2) | Mo3—O4vii | 2.072 (2) |
Pr—O3v | 2.697 (2) | Mo3—O2viii | 2.075 (2) |
Pr—O8iii | 2.721 (2) | Mo3—O8 | 2.144 (2) |
Pr—O2i | 2.757 (2) | Mo3—Mo4xii | 2.6057 (3) |
Pr—O6iii | 2.868 (2) | Mo3—Mo5xiii | 2.6731 (3) |
Pr—O2vi | 2.933 (2) | Mo3—Mo5 | 2.7591 (3) |
Pr—Mo2ii | 3.3702 (3) | Mo3—Mo1ix | 2.8116 (3) |
Pr—Mo4iv | 3.4045 (3) | Mo3—Prxiv | 3.6451 (3) |
Mo1—O5vii | 2.036 (2) | Mo4—O5 | 2.058 (2) |
Mo1—O7viii | 2.071 (2) | Mo4—O7viii | 2.065 (2) |
Mo1—O8ix | 2.124 (2) | Mo4—O3x | 2.073 (2) |
Mo1—O4vii | 2.124 (2) | Mo4—O1ix | 2.082 (2) |
Mo1—O8 | 2.125 (2) | Mo4—O2xv | 2.101 (2) |
Mo1—Mo1ix | 2.6855 (4) | Mo4—Mo3x | 2.6057 (3) |
Mo1—Mo2ix | 2.6867 (3) | Mo4—Mo2ix | 2.7275 (3) |
Mo1—Mo4 | 2.7937 (3) | Mo4—Mo5x | 2.7458 (3) |
Mo1—Mo5x | 2.8094 (3) | Mo4—Mo5ix | 2.7599 (3) |
Mo1—Mo3ix | 2.8116 (3) | Mo4—Prxvi | 3.4045 (3) |
Mo1—Mo2 | 2.9058 (3) | Mo5—O6vii | 2.035 (2) |
Mo1—Mo3 | 3.0845 (3) | Mo5—O5xvii | 2.054 (2) |
Mo2—O6vii | 1.996 (2) | Mo5—O2viii | 2.074 (2) |
Mo2—O1 | 2.017 (2) | Mo5—O3xiii | 2.085 (2) |
Mo2—O4vii | 2.056 (2) | Mo5—Mo3xiii | 2.6731 (3) |
Mo2—O8ix | 2.108 (2) | Mo5—Mo4xii | 2.7458 (3) |
Mo2—O7 | 2.1321 (19) | Mo5—Mo4ix | 2.7599 (3) |
Mo2—Mo1ix | 2.6867 (3) | Mo5—Mo1xii | 2.8094 (3) |
Mo2—Mo4ix | 2.7275 (3) | Mo5—Mo5xiii | 2.8201 (4) |
Mo2—Mo5 | 2.7579 (3) | | |
| | | |
O1i—Pr—O1ii | 72.99 (8) | O1i—Pr—O4iii | 71.11 (6) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1, y+1/2, −z+3/2; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+1/2; (v) −x, y+1/2, −z+1/2; (vi) −x, y+1/2, −z+3/2; (vii) x, −y−1/2, z+1/2; (viii) x, −y−1/2, z−1/2; (ix) −x+1, −y, −z+1; (x) x+1, y, z; (xi) −x+1, y−1/2, −z+3/2; (xii) x−1, y, z; (xiii) −x, −y, −z+1; (xiv) x, y−1, z; (xv) x+1, −y−1/2, z−1/2; (xvi) −x+1, y−1/2, −z+1/2; (xvii) x−1, −y−1/2, z+1/2. |
Crystal data top
NdMo5O8 | F(000) = 1336 |
Mr = 751.94 | Dx = 7.822 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71070 Å |
a = 7.5606 (1) Å | Cell parameters from 12284 reflections |
b = 9.0392 (1) Å | θ = 1.0–37.8° |
c = 9.9082 (2) Å | µ = 17.52 mm−1 |
β = 109.4513 (7)° | T = 293 K |
V = 638.50 (2) Å3 | Irregular plate, black |
Z = 4 | 0.13 × 0.13 × 0.08 mm |
Data collection top
Nonius KappaCCD diffractometer | 3404 independent reflections |
Radiation source: fine-focus sealed tube | 3193 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
ϕ scans (κ = 0) + additional ω scans | θmax = 37.8°, θmin = 2.9° |
Absorption correction: multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 | h = −12→12 |
Tmin = 0.113, Tmax = 0.252 | k = −15→15 |
17433 measured reflections | l = −14→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.024 | w = 1/[σ2(Fo2) + (0.P)2 + 2.8951P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.055 | (Δ/σ)max = 0.001 |
S = 1.16 | Δρmax = 1.63 e Å−3 |
3404 reflections | Δρmin = −1.82 e Å−3 |
128 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0185 (3) |
Crystal data top
NdMo5O8 | V = 638.50 (2) Å3 |
Mr = 751.94 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 7.5606 (1) Å | µ = 17.52 mm−1 |
b = 9.0392 (1) Å | T = 293 K |
c = 9.9082 (2) Å | 0.13 × 0.13 × 0.08 mm |
β = 109.4513 (7)° | |
Data collection top
Nonius KappaCCD diffractometer | 3404 independent reflections |
Absorption correction: multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 | 3193 reflections with I > 2σ(I) |
Tmin = 0.113, Tmax = 0.252 | Rint = 0.052 |
17433 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.024 | 128 parameters |
wR(F2) = 0.055 | 0 restraints |
S = 1.16 | Δρmax = 1.63 e Å−3 |
3404 reflections | Δρmin = −1.82 e Å−3 |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Nd | 0.26519 (2) | 0.504029 (18) | 0.535724 (17) | 0.00884 (5) | |
Mo1 | 0.60423 (3) | −0.11559 (3) | 0.48678 (3) | 0.00600 (5) | |
Mo2 | 0.38404 (3) | −0.11803 (3) | 0.67733 (3) | 0.00602 (5) | |
Mo3 | 0.17229 (4) | −0.12707 (3) | 0.38235 (3) | 0.00532 (5) | |
Mo4 | 0.80740 (3) | −0.13019 (3) | 0.29785 (3) | 0.00517 (5) | |
Mo5 | −0.00215 (3) | −0.12333 (3) | 0.58651 (3) | 0.00528 (5) | |
O1 | 0.3997 (3) | 0.0063 (2) | 0.8502 (2) | 0.0081 (4) | |
O2 | −0.0013 (3) | −0.2210 (2) | 0.9331 (2) | 0.0071 (3) | |
O3 | −0.0162 (3) | 0.0029 (2) | 0.2297 (2) | 0.0071 (3) | |
O4 | 0.3908 (3) | −0.2461 (3) | 0.0127 (2) | 0.0077 (4) | |
O5 | 0.7948 (3) | −0.2405 (2) | 0.1137 (2) | 0.0076 (4) | |
O6 | 0.2006 (3) | −0.2387 (3) | 0.2084 (2) | 0.0082 (4) | |
O7 | 0.6067 (3) | −0.2336 (2) | 0.8304 (2) | 0.0071 (3) | |
O8 | 0.3828 (3) | −0.0067 (2) | 0.3273 (2) | 0.0076 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nd | 0.00757 (8) | 0.00914 (8) | 0.00971 (8) | −0.00033 (5) | 0.00275 (6) | 0.00051 (5) |
Mo1 | 0.00541 (10) | 0.00524 (10) | 0.00667 (11) | 0.00011 (6) | 0.00112 (8) | −0.00015 (7) |
Mo2 | 0.00570 (10) | 0.00585 (10) | 0.00584 (10) | −0.00047 (7) | 0.00102 (8) | 0.00058 (7) |
Mo3 | 0.00516 (10) | 0.00549 (10) | 0.00537 (10) | 0.00009 (7) | 0.00185 (8) | −0.00022 (7) |
Mo4 | 0.00488 (10) | 0.00532 (10) | 0.00529 (10) | −0.00015 (6) | 0.00167 (8) | −0.00032 (7) |
Mo5 | 0.00510 (10) | 0.00511 (10) | 0.00553 (11) | −0.00003 (6) | 0.00166 (8) | 0.00024 (7) |
O1 | 0.0081 (9) | 0.0091 (9) | 0.0062 (9) | 0.0010 (7) | 0.0012 (7) | −0.0002 (7) |
O2 | 0.0077 (8) | 0.0065 (8) | 0.0073 (8) | −0.0004 (6) | 0.0025 (7) | 0.0005 (7) |
O3 | 0.0070 (9) | 0.0076 (9) | 0.0063 (9) | −0.0003 (6) | 0.0016 (7) | 0.0001 (7) |
O4 | 0.0073 (8) | 0.0076 (9) | 0.0091 (9) | −0.0013 (6) | 0.0039 (7) | −0.0008 (7) |
O5 | 0.0069 (8) | 0.0074 (9) | 0.0088 (9) | 0.0008 (6) | 0.0029 (7) | −0.0017 (7) |
O6 | 0.0064 (8) | 0.0095 (9) | 0.0081 (9) | −0.0005 (7) | 0.0016 (7) | −0.0033 (7) |
O7 | 0.0066 (8) | 0.0072 (8) | 0.0071 (8) | 0.0023 (6) | 0.0020 (7) | 0.0018 (7) |
O8 | 0.0064 (8) | 0.0086 (9) | 0.0079 (9) | −0.0004 (6) | 0.0026 (7) | 0.0013 (7) |
Geometric parameters (Å, º) top
Nd—O1i | 2.380 (2) | Mo2—Mo3 | 2.8277 (4) |
Nd—O1ii | 2.406 (2) | Mo2—Ndxi | 3.3634 (3) |
Nd—O4iii | 2.427 (2) | Mo3—O3 | 2.064 (2) |
Nd—O7ii | 2.540 (2) | Mo3—O6 | 2.069 (2) |
Nd—O5iv | 2.615 (2) | Mo3—O4vii | 2.071 (2) |
Nd—O3v | 2.676 (2) | Mo3—O2viii | 2.074 (2) |
Nd—O8iii | 2.725 (2) | Mo3—O8 | 2.143 (2) |
Nd—O2i | 2.753 (2) | Mo3—Mo4xii | 2.6028 (3) |
Nd—O6iii | 2.868 (2) | Mo3—Mo5xiii | 2.6715 (3) |
Nd—O2vi | 2.937 (2) | Mo3—Mo5 | 2.7586 (3) |
Nd—Mo2ii | 3.3634 (3) | Mo3—Mo1ix | 2.8086 (3) |
Nd—Mo4iv | 3.3895 (3) | Mo3—Ndxiv | 3.6347 (3) |
Mo1—O5vii | 2.036 (2) | Mo4—O5 | 2.053 (2) |
Mo1—O7viii | 2.068 (2) | Mo4—O7viii | 2.061 (2) |
Mo1—O8ix | 2.123 (2) | Mo4—O3x | 2.069 (2) |
Mo1—O8 | 2.123 (2) | Mo4—O1ix | 2.080 (2) |
Mo1—O4vii | 2.123 (2) | Mo4—O2xv | 2.099 (2) |
Mo1—Mo1ix | 2.6822 (5) | Mo4—Mo3x | 2.6028 (3) |
Mo1—Mo2ix | 2.6847 (4) | Mo4—Mo2ix | 2.7253 (3) |
Mo1—Mo4 | 2.7922 (3) | Mo4—Mo5x | 2.7413 (3) |
Mo1—Mo5x | 2.8070 (3) | Mo4—Mo5ix | 2.7584 (3) |
Mo1—Mo3ix | 2.8086 (3) | Mo4—Ndxvi | 3.3895 (3) |
Mo1—Mo2 | 2.9034 (3) | Mo5—O6vii | 2.032 (2) |
Mo1—Mo3 | 3.0815 (4) | Mo5—O5xvii | 2.054 (2) |
Mo2—O6vii | 1.995 (2) | Mo5—O2viii | 2.073 (2) |
Mo2—O1 | 2.019 (2) | Mo5—O3xiii | 2.087 (2) |
Mo2—O4vii | 2.056 (2) | Mo5—Mo3xiii | 2.6715 (3) |
Mo2—O8ix | 2.106 (2) | Mo5—Mo4xii | 2.7413 (3) |
Mo2—O7 | 2.127 (2) | Mo5—Mo4ix | 2.7584 (3) |
Mo2—Mo1ix | 2.6847 (4) | Mo5—Mo1xii | 2.8070 (3) |
Mo2—Mo4ix | 2.7253 (3) | Mo5—Mo5xiii | 2.8192 (5) |
Mo2—Mo5 | 2.7545 (3) | | |
| | | |
O1i—Nd—O1ii | 73.10 (9) | O1ii—Nd—O4iii | 69.67 (7) |
O1i—Nd—O4iii | 71.44 (7) | | |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1, y+1/2, −z+3/2; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+1/2; (v) −x, y+1/2, −z+1/2; (vi) −x, y+1/2, −z+3/2; (vii) x, −y−1/2, z+1/2; (viii) x, −y−1/2, z−1/2; (ix) −x+1, −y, −z+1; (x) x+1, y, z; (xi) −x+1, y−1/2, −z+3/2; (xii) x−1, y, z; (xiii) −x, −y, −z+1; (xiv) x, y−1, z; (xv) x+1, −y−1/2, z−1/2; (xvi) −x+1, y−1/2, −z+1/2; (xvii) x−1, −y−1/2, z+1/2. |
Crystal data top
SmMo5O8 | F(000) = 1344 |
Mr = 758.05 | Dx = 7.900 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71070 Å |
a = 7.5620 (2) Å | Cell parameters from 6858 reflections |
b = 9.0197 (2) Å | θ = 2.9–37.8° |
c = 9.9226 (2) Å | µ = 18.62 mm−1 |
β = 109.6643 (12)° | T = 293 K |
V = 637.32 (3) Å3 | Irregular plate, black |
Z = 4 | 0.09 × 0.06 × 0.03 mm |
Data collection top
Nonius KappaCCD diffractometer | 3395 independent reflections |
Radiation source: fine-focus sealed tube | 2569 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.075 |
ϕ scans (κ = 0) + additional ω scans | θmax = 37.8°, θmin = 3.1° |
Absorption correction: multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 | h = −12→13 |
Tmin = 0.378, Tmax = 0.513 | k = −15→15 |
15935 measured reflections | l = −17→15 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.039 | w = 1/[σ2(Fo2) + (0.0313P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.087 | (Δ/σ)max = 0.001 |
S = 1.03 | Δρmax = 4.49 e Å−3 |
3395 reflections | Δρmin = −2.89 e Å−3 |
128 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00439 (19) |
Crystal data top
SmMo5O8 | V = 637.32 (3) Å3 |
Mr = 758.05 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 7.5620 (2) Å | µ = 18.62 mm−1 |
b = 9.0197 (2) Å | T = 293 K |
c = 9.9226 (2) Å | 0.09 × 0.06 × 0.03 mm |
β = 109.6643 (12)° | |
Data collection top
Nonius KappaCCD diffractometer | 3395 independent reflections |
Absorption correction: multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 | 2569 reflections with I > 2σ(I) |
Tmin = 0.378, Tmax = 0.513 | Rint = 0.075 |
15935 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.039 | 128 parameters |
wR(F2) = 0.087 | 0 restraints |
S = 1.03 | Δρmax = 4.49 e Å−3 |
3395 reflections | Δρmin = −2.89 e Å−3 |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sm | 0.26744 (4) | 0.50342 (3) | 0.53268 (3) | 0.00998 (8) | |
Mo1 | 0.60408 (6) | −0.11595 (4) | 0.48701 (4) | 0.00656 (9) | |
Mo2 | 0.38458 (6) | −0.11813 (4) | 0.67749 (4) | 0.00645 (9) | |
Mo3 | 0.17205 (6) | −0.12713 (4) | 0.38201 (4) | 0.00592 (9) | |
Mo4 | 0.80693 (6) | −0.13060 (4) | 0.29808 (4) | 0.00578 (9) | |
Mo5 | −0.00176 (6) | −0.12369 (4) | 0.58656 (4) | 0.00578 (8) | |
O1 | 0.4009 (5) | 0.0061 (3) | 0.8499 (3) | 0.0080 (6) | |
O2 | −0.0011 (5) | −0.2200 (4) | 0.9337 (3) | 0.0077 (6) | |
O3 | −0.0179 (5) | 0.0032 (3) | 0.2297 (3) | 0.0067 (6) | |
O4 | 0.3902 (5) | −0.2445 (4) | 0.0128 (3) | 0.0097 (7) | |
O5 | 0.7952 (5) | −0.2394 (4) | 0.1140 (3) | 0.0085 (6) | |
O6 | 0.2008 (5) | −0.2382 (4) | 0.2085 (3) | 0.0105 (7) | |
O7 | 0.6078 (5) | −0.2316 (4) | 0.8319 (3) | 0.0074 (6) | |
O8 | 0.3824 (5) | −0.0060 (3) | 0.3265 (4) | 0.0080 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sm | 0.00893 (13) | 0.01056 (13) | 0.01018 (13) | −0.00034 (8) | 0.00288 (9) | 0.00063 (8) |
Mo1 | 0.00622 (19) | 0.00606 (18) | 0.00656 (18) | 0.00017 (13) | 0.00102 (14) | −0.00023 (12) |
Mo2 | 0.00644 (18) | 0.00642 (18) | 0.00563 (17) | −0.00039 (13) | 0.00091 (13) | 0.00049 (13) |
Mo3 | 0.00645 (18) | 0.00621 (18) | 0.00491 (17) | 0.00024 (13) | 0.00165 (13) | −0.00006 (13) |
Mo4 | 0.00588 (18) | 0.00619 (17) | 0.00511 (17) | −0.00021 (13) | 0.00164 (13) | −0.00030 (12) |
Mo5 | 0.00617 (19) | 0.00582 (17) | 0.00506 (17) | −0.00013 (13) | 0.00150 (13) | 0.00032 (13) |
O1 | 0.0100 (17) | 0.0088 (16) | 0.0047 (14) | 0.0021 (12) | 0.0018 (12) | 0.0004 (11) |
O2 | 0.0104 (16) | 0.0056 (14) | 0.0058 (14) | −0.0018 (12) | 0.0010 (12) | −0.0011 (11) |
O3 | 0.0080 (16) | 0.0072 (15) | 0.0048 (14) | −0.0023 (11) | 0.0019 (12) | −0.0010 (11) |
O4 | 0.0096 (17) | 0.0104 (16) | 0.0091 (15) | −0.0005 (13) | 0.0033 (13) | 0.0005 (12) |
O5 | 0.0075 (16) | 0.0087 (15) | 0.0085 (15) | −0.0008 (12) | 0.0015 (12) | −0.0027 (12) |
O6 | 0.0103 (17) | 0.0114 (16) | 0.0099 (16) | −0.0024 (13) | 0.0034 (13) | −0.0048 (13) |
O7 | 0.0092 (16) | 0.0083 (14) | 0.0047 (13) | 0.0043 (12) | 0.0023 (12) | 0.0029 (11) |
O8 | 0.0049 (15) | 0.0106 (16) | 0.0072 (14) | 0.0016 (12) | 0.0002 (11) | 0.0013 (12) |
Geometric parameters (Å, º) top
Sm—O1i | 2.355 (3) | Mo2—Mo5 | 2.7527 (6) |
Sm—O1ii | 2.384 (4) | Mo2—Mo3 | 2.8309 (6) |
Sm—O4iii | 2.398 (4) | Mo2—Smxi | 3.3621 (5) |
Sm—O7ii | 2.517 (3) | Mo3—O6 | 2.065 (3) |
Sm—O5iv | 2.584 (3) | Mo3—O3 | 2.066 (3) |
Sm—O3v | 2.652 (3) | Mo3—O4vii | 2.075 (3) |
Sm—O8iii | 2.748 (3) | Mo3—O2viii | 2.081 (3) |
Sm—O2i | 2.750 (3) | Mo3—O8 | 2.148 (3) |
Sm—O6iii | 2.894 (3) | Mo3—Mo4xii | 2.6020 (6) |
Sm—O2vi | 2.947 (3) | Mo3—Mo5xiii | 2.6727 (6) |
Sm—Mo2ii | 3.3621 (5) | Mo3—Mo5 | 2.7647 (5) |
Sm—Mo4iv | 3.3626 (4) | Mo3—Mo1ix | 2.8073 (6) |
Mo1—O5vii | 2.038 (3) | Mo3—Smxiv | 3.6241 (5) |
Mo1—O7viii | 2.071 (3) | Mo4—O5 | 2.049 (3) |
Mo1—O8ix | 2.126 (3) | Mo4—O7viii | 2.065 (3) |
Mo1—O8 | 2.129 (3) | Mo4—O3x | 2.068 (3) |
Mo1—O4vii | 2.132 (4) | Mo4—O1ix | 2.082 (3) |
Mo1—Mo1ix | 2.6818 (8) | Mo4—O2xv | 2.102 (3) |
Mo1—Mo2ix | 2.6876 (5) | Mo4—Mo3x | 2.6020 (6) |
Mo1—Mo4 | 2.7964 (5) | Mo4—Mo2ix | 2.7249 (6) |
Mo1—Mo3ix | 2.8073 (6) | Mo4—Mo5x | 2.7393 (5) |
Mo1—Mo5x | 2.8077 (5) | Mo4—Mo5ix | 2.7580 (6) |
Mo1—Mo2 | 2.9050 (6) | Mo4—Smxvi | 3.3626 (4) |
Mo1—Mo3 | 3.0787 (6) | Mo5—O6vii | 2.028 (3) |
Mo2—O6vii | 1.998 (3) | Mo5—O5xvii | 2.059 (3) |
Mo2—O1 | 2.014 (3) | Mo5—O2viii | 2.072 (3) |
Mo2—O4vii | 2.063 (3) | Mo5—O3xiii | 2.085 (3) |
Mo2—O8ix | 2.100 (3) | Mo5—Mo3xiii | 2.6727 (6) |
Mo2—O7 | 2.122 (3) | Mo5—Mo4xii | 2.7393 (5) |
Mo2—Mo1ix | 2.6876 (5) | Mo5—Mo4ix | 2.7580 (6) |
Mo2—Mo4ix | 2.7249 (6) | Mo5—Mo1xii | 2.8077 (5) |
| | | |
O1i—Sm—O1ii | 73.97 (12) | O1i—Sm—O4iii | 72.04 (10) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1, y+1/2, −z+3/2; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+1/2; (v) −x, y+1/2, −z+1/2; (vi) −x, y+1/2, −z+3/2; (vii) x, −y−1/2, z+1/2; (viii) x, −y−1/2, z−1/2; (ix) −x+1, −y, −z+1; (x) x+1, y, z; (xi) −x+1, y−1/2, −z+3/2; (xii) x−1, y, z; (xiii) −x, −y, −z+1; (xiv) x, y−1, z; (xv) x+1, −y−1/2, z−1/2; (xvi) −x+1, y−1/2, −z+1/2; (xvii) x−1, −y−1/2, z+1/2. |
Crystal data top
EuMo5O8 | F(000) = 1348 |
Mr = 759.66 | Dx = 7.750 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71070 Å |
a = 7.5554 (1) Å | Cell parameters from 12022 reflections |
b = 9.1622 (2) Å | θ = 1.0–37.8° |
c = 9.9685 (2) Å | µ = 18.84 mm−1 |
β = 109.3560 (9)° | T = 293 K |
V = 651.06 (2) Å3 | Irregular plate, black |
Z = 4 | 0.10 × 0.07 × 0.05 mm |
Data collection top
Nonius KappaCCD diffractometer | 3471 independent reflections |
Radiation source: fine-focus sealed tube | 3034 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
ϕ scans (κ = 0) + additional ω scans | θmax = 37.8°, θmin = 2.9° |
Absorption correction: multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 | h = 0→13 |
Tmin = 0.168, Tmax = 0.358 | k = 0→15 |
6545 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.032 | w = 1/[σ2(Fo2) + (0.0324P)2 + 2.9295P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.077 | (Δ/σ)max = 0.001 |
S = 1.06 | Δρmax = 3.59 e Å−3 |
3471 reflections | Δρmin = −4.08 e Å−3 |
128 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0189 (4) |
Crystal data top
EuMo5O8 | V = 651.06 (2) Å3 |
Mr = 759.66 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 7.5554 (1) Å | µ = 18.84 mm−1 |
b = 9.1622 (2) Å | T = 293 K |
c = 9.9685 (2) Å | 0.10 × 0.07 × 0.05 mm |
β = 109.3560 (9)° | |
Data collection top
Nonius KappaCCD diffractometer | 3471 independent reflections |
Absorption correction: multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 | 3034 reflections with I > 2σ(I) |
Tmin = 0.168, Tmax = 0.358 | Rint = 0.031 |
6545 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.032 | 128 parameters |
wR(F2) = 0.077 | 0 restraints |
S = 1.06 | Δρmax = 3.59 e Å−3 |
3471 reflections | Δρmin = −4.08 e Å−3 |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Eu | 0.25260 (3) | 0.50439 (2) | 0.53847 (2) | 0.00844 (6) | |
Mo1 | 0.61048 (4) | −0.11430 (3) | 0.48321 (3) | 0.00357 (7) | |
Mo2 | 0.38030 (4) | −0.11665 (3) | 0.68171 (3) | 0.00373 (7) | |
Mo3 | 0.17803 (4) | −0.12587 (3) | 0.38692 (3) | 0.00352 (7) | |
Mo4 | 0.81246 (4) | −0.13160 (3) | 0.29888 (3) | 0.00356 (7) | |
Mo5 | −0.00146 (4) | −0.12247 (3) | 0.58633 (3) | 0.00343 (7) | |
O1 | 0.3947 (4) | 0.0057 (3) | 0.8401 (3) | 0.0061 (5) | |
O2 | 0.0046 (4) | −0.2247 (3) | 0.9347 (3) | 0.0059 (4) | |
O3 | −0.0077 (4) | 0.0004 (3) | 0.2363 (3) | 0.0068 (5) | |
O4 | 0.4015 (4) | −0.2558 (3) | 0.0200 (3) | 0.0057 (5) | |
O5 | 0.7988 (4) | −0.2484 (3) | 0.1175 (3) | 0.0055 (5) | |
O6 | 0.2015 (4) | −0.2470 (3) | 0.2162 (3) | 0.0064 (5) | |
O7 | 0.6030 (4) | −0.2405 (3) | 0.8267 (3) | 0.0051 (4) | |
O8 | 0.3864 (4) | −0.0015 (3) | 0.3330 (3) | 0.0058 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Eu | 0.00776 (10) | 0.00835 (10) | 0.00840 (10) | 0.00025 (6) | 0.00159 (7) | 0.00039 (6) |
Mo1 | 0.00322 (12) | 0.00361 (13) | 0.00387 (13) | −0.00012 (9) | 0.00118 (10) | 0.00004 (9) |
Mo2 | 0.00304 (12) | 0.00396 (13) | 0.00408 (13) | 0.00029 (9) | 0.00103 (10) | 0.00020 (9) |
Mo3 | 0.00348 (13) | 0.00383 (13) | 0.00346 (13) | 0.00001 (9) | 0.00141 (10) | −0.00017 (9) |
Mo4 | 0.00314 (13) | 0.00383 (13) | 0.00373 (13) | −0.00025 (9) | 0.00115 (10) | −0.00037 (9) |
Mo5 | 0.00305 (13) | 0.00346 (13) | 0.00382 (13) | 0.00023 (8) | 0.00117 (10) | 0.00018 (9) |
O1 | 0.0052 (11) | 0.0056 (12) | 0.0061 (11) | 0.0018 (8) | −0.0001 (9) | −0.0004 (8) |
O2 | 0.0042 (10) | 0.0067 (11) | 0.0061 (10) | 0.0004 (8) | 0.0011 (9) | 0.0000 (9) |
O3 | 0.0069 (11) | 0.0071 (12) | 0.0067 (12) | −0.0010 (9) | 0.0025 (10) | 0.0006 (8) |
O4 | 0.0040 (11) | 0.0065 (11) | 0.0070 (11) | −0.0011 (8) | 0.0022 (9) | −0.0010 (9) |
O5 | 0.0030 (10) | 0.0062 (11) | 0.0071 (11) | 0.0004 (8) | 0.0016 (9) | −0.0029 (9) |
O6 | 0.0059 (11) | 0.0074 (12) | 0.0057 (11) | 0.0000 (9) | 0.0016 (9) | −0.0029 (9) |
O7 | 0.0045 (11) | 0.0056 (11) | 0.0050 (10) | 0.0019 (9) | 0.0013 (9) | 0.0013 (9) |
O8 | 0.0058 (11) | 0.0061 (12) | 0.0067 (11) | −0.0002 (8) | 0.0039 (9) | −0.0001 (8) |
Bond lengths (Å) top
Eu—O1i | 2.535 (3) | Mo2—Mo3 | 2.8286 (4) |
Eu—O1ii | 2.545 (3) | Mo2—Euxi | 3.4022 (4) |
Eu—O4iii | 2.596 (3) | Mo2—Euxii | 3.7566 (4) |
Eu—O7i | 2.657 (3) | Mo3—O3 | 2.041 (3) |
Eu—O2ii | 2.715 (3) | Mo3—O2viii | 2.057 (3) |
Eu—O5iv | 2.744 (3) | Mo3—O4vii | 2.074 (3) |
Eu—O3v | 2.751 (3) | Mo3—O6 | 2.087 (3) |
Eu—O8iii | 2.771 (3) | Mo3—O8 | 2.151 (3) |
Eu—O2vi | 2.932 (3) | Mo3—Mo4xiii | 2.6067 (4) |
Eu—O6iii | 2.947 (3) | Mo3—Mo5xiv | 2.6951 (4) |
Eu—Mo2i | 3.4022 (4) | Mo3—Mo5 | 2.7529 (4) |
Eu—Mo4iv | 3.4651 (4) | Mo3—Mo1ix | 2.7749 (4) |
Mo1—O5vii | 2.034 (3) | Mo3—Euxii | 3.6758 (4) |
Mo1—O7viii | 2.037 (3) | Mo4—O7viii | 2.060 (3) |
Mo1—O4vii | 2.105 (3) | Mo4—O3x | 2.064 (3) |
Mo1—O8ix | 2.110 (3) | Mo4—O1ix | 2.065 (3) |
Mo1—O8 | 2.120 (3) | Mo4—O5 | 2.074 (3) |
Mo1—Mo2ix | 2.6947 (4) | Mo4—O2xv | 2.091 (3) |
Mo1—Mo4 | 2.7549 (4) | Mo4—Mo3x | 2.6067 (4) |
Mo1—Mo1ix | 2.7670 (6) | Mo4—Mo2ix | 2.7420 (4) |
Mo1—Mo5x | 2.7678 (4) | Mo4—Mo5x | 2.7430 (4) |
Mo1—Mo3ix | 2.7749 (4) | Mo4—Mo5ix | 2.7720 (4) |
Mo1—Mo2 | 3.0366 (4) | Mo4—Euxvi | 3.4651 (4) |
Mo1—Mo3 | 3.0869 (5) | Mo5—O5xvii | 2.021 (3) |
Mo2—O1 | 1.910 (3) | Mo5—O6vii | 2.035 (3) |
Mo2—O6vii | 1.953 (3) | Mo5—O2viii | 2.072 (3) |
Mo2—O4vii | 2.040 (3) | Mo5—O3xiv | 2.074 (3) |
Mo2—O8ix | 2.115 (3) | Mo5—Mo3xiv | 2.6951 (4) |
Mo2—O7 | 2.144 (3) | Mo5—Mo4xiii | 2.7430 (4) |
Mo2—Mo1ix | 2.6947 (4) | Mo5—Mo1xiii | 2.7678 (4) |
Mo2—Mo5 | 2.7218 (4) | Mo5—Mo4ix | 2.7720 (4) |
Mo2—Mo4ix | 2.7420 (4) | Mo5—Mo5xiv | 2.8327 (6) |
Symmetry codes: (i) −x+1, y+1/2, −z+3/2; (ii) x, −y+1/2, z−1/2; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+1/2; (v) −x, y+1/2, −z+1/2; (vi) −x, y+1/2, −z+3/2; (vii) x, −y−1/2, z+1/2; (viii) x, −y−1/2, z−1/2; (ix) −x+1, −y, −z+1; (x) x+1, y, z; (xi) −x+1, y−1/2, −z+3/2; (xii) x, y−1, z; (xiii) x−1, y, z; (xiv) −x, −y, −z+1; (xv) x+1, −y−1/2, z−1/2; (xvi) −x+1, y−1/2, −z+1/2; (xvii) x−1, −y−1/2, z+1/2. |
Experimental details
| (CeMo5O8) | (PrMo5O8) | (NdMo5O8) | (SmMo5O8) |
Crystal data |
Chemical formula | CeMo5O8 | PrMo5O8 | NdMo5O8 | SmMo5O8 |
Mr | 747.82 | 748.61 | 751.94 | 758.05 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 293 | 293 | 293 | 293 |
a, b, c (Å) | 7.5643 (1), 9.0693 (1), 9.9150 (2) | 7.5662 (1), 9.0569 (1), 9.9175 (1) | 7.5606 (1), 9.0392 (1), 9.9082 (2) | 7.5620 (2), 9.0197 (2), 9.9226 (2) |
α, β, γ (°) | 90, 109.2113 (8), 90 | 90, 109.3293 (7), 90 | 90, 109.4513 (7), 90 | 90, 109.6643 (12), 90 |
V (Å3) | 642.32 (2) | 641.30 (1) | 638.50 (2) | 637.32 (3) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 16.42 | 16.94 | 17.52 | 18.62 |
Crystal size (mm) | 0.14 × 0.10 × 0.08 | 0.24 × 0.11 × 0.04 | 0.13 × 0.13 × 0.08 | 0.09 × 0.06 × 0.03 |
|
Data collection |
Diffractometer | Nonius KappaCCD diffractometer | Nonius KappaCCD diffractometer | Nonius KappaCCD diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Gaussian '(Coppens, P., Leiserowitz, L. & Rabinovich, D. 1965)' | Gaussian '(Coppens, P., Leiserowitz, L. & Rabinovich, D. 1965)' | Multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 | Multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 |
Tmin, Tmax | 0.064, 0.181 | 0.090, 0.524 | 0.113, 0.252 | 0.378, 0.513 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12944, 3402, 3314 | 14762, 3411, 3329 | 17433, 3404, 3193 | 15935, 3395, 2569 |
Rint | 0.064 | 0.091 | 0.052 | 0.075 |
(sin θ/λ)max (Å−1) | 0.863 | 0.862 | 0.862 | 0.861 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.080, 1.26 | 0.029, 0.070, 1.19 | 0.024, 0.055, 1.16 | 0.039, 0.087, 1.03 |
No. of reflections | 3402 | 3411 | 3404 | 3395 |
No. of parameters | 128 | 128 | 128 | 128 |
Δρmax, Δρmin (e Å−3) | 2.54, −2.50 | 2.45, −3.32 | 1.63, −1.82 | 4.49, −2.89 |
| (EuMo5O8) |
Crystal data |
Chemical formula | EuMo5O8 |
Mr | 759.66 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 7.5554 (1), 9.1622 (2), 9.9685 (2) |
α, β, γ (°) | 90, 109.3560 (9), 90 |
V (Å3) | 651.06 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 18.84 |
Crystal size (mm) | 0.10 × 0.07 × 0.05 |
|
Data collection |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan r.h. blessing, acta cryst. (1995), a51, 33-38 |
Tmin, Tmax | 0.168, 0.358 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6545, 3471, 3034 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.863 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.077, 1.06 |
No. of reflections | 3471 |
No. of parameters | 128 |
Δρmax, Δρmin (e Å−3) | 3.59, −4.08 |
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