research papers
The single-crystal diffraction study of Ce10W22O81 and powder X-ray diffraction (XRD) experiments on Ce10W22O81 and Nd10W22O81 show that the true space group of these phases is Pbnm, contrary to the previous literature reports of the space groups Pbcn and Pbcm for the rare-earth tungstates (RE = La, Ce, Pr, Nd) with this general formula. The structure contains rare-earth cations in seven-, eight- and ninefold coordination. W atoms are found in corner-sharing WO5 groups, and also in WO6 and WO7 polyhedra which share edges and corners to form W6O17 units. The new model obtained from our single-crystal work gives better agreement with powder XRD data on both Ce10W22O81 and Nd10W22O81, and gives more plausible coordination environments and bond-valence sums.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768108033430/zb5001sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768108033430/zb5001Isup2.fcf |
Computing details top
Data collection: SMART (Siemens, 1993); cell refinement: SAINT (Siemens ,1995); data reduction: SAINT (Siemens ,1995); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); software used to prepare material for publication: CRYSTALS (Betteridge et al., 2003).
(I) top
Crystal data top
Ce10O81W22 | F(000) = 5712 |
Mr = 6741.85 | Dx = 7.285 Mg m−3 |
Orthorhombic, Pbnm | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2c 2ab | Cell parameters from 0 reflections |
a = 3.8891 (4) Å | θ = 0–0° |
b = 36.080 (4) Å | µ = 48.34 mm−1 |
c = 21.901 (2) Å | T = 120 K |
V = 3073.1 (5) Å3 | Elongated prism, brown |
Z = 2 | 0.08 × 0.02 × 0.02 mm |
Data collection top
Area diffractometer | 4244 independent reflections |
Graphite monochromator | Rint = 0.044 |
ω scans | θmax = 29.6°, θmin = 1.9° |
Absorption correction: multi-scan SADABS (Siemens, 1996) | h = −5→5 |
Tmin = 0.91, Tmax = 1.00 | k = −49→49 |
32374 measured reflections | l = −29→28 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
wR(F2) = 0.101 | Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A0*T0(x) + A1*T1(x) ··· + An-1]*Tn-1(x)]
where Ai are the Chebychev coefficients listed below and x = F /Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)2]2 Ai are: 5.48 8.03 4.81 1.83 0.648 |
S = 0.91 | (Δ/σ)max = 0.001 |
2524 reflections | Δρmax = 7.28 e Å−3 |
166 parameters | Δρmin = −7.55 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
W1 | 0.0653 (3) | 0.35277 (2) | 0.33588 (4) | 0.0059 | |
W2 | 0.4325 (5) | 0.55718 (3) | 0.2500 | 0.0060 | |
W3 | −0.0610 (4) | 0.27690 (4) | 0.2500 | 0.0065 | |
W4 | 0.0647 (3) | 0.25248 (3) | 0.39511 (4) | 0.0067 | |
W5 | 0.0661 (3) | 0.36527 (2) | 0.61692 (4) | 0.0058 | |
W6 | −0.4927 (5) | 0.44607 (4) | 0.47384 (6) | 0.0275 | |
W7 | −0.0455 (7) | 0.44219 (4) | 0.2500 | 0.0264 | |
Ce8 | −0.0128 (4) | 0.51857 (4) | 0.38391 (11) | 0.0269 | |
Ce9 | 0.0125 (6) | 0.17459 (6) | 0.2500 | 0.0290 | |
Ce10 | −0.4859 (5) | 0.32947 (6) | 0.47894 (14) | 0.0381 | |
O11 | 0.519 (10) | 0.3616 (9) | 0.6209 (15) | 0.056 (9)* | |
O12 | 0.014 (6) | 0.2109 (6) | 0.4317 (11) | 0.028 (5)* | |
O13 | 0.006 (5) | 0.2855 (5) | 0.4568 (10) | 0.019 (4)* | |
O14 | 0.509 (10) | 0.3493 (9) | 0.3345 (16) | 0.058 (9)* | |
O15 | 0.009 (6) | 0.3536 (6) | 0.4158 (9) | 0.021 (4)* | |
O16 | −0.012 (8) | 0.4732 (7) | 0.3118 (12) | 0.041 (7)* | |
O17 | −0.014 (7) | 0.3333 (7) | 0.2500 | 0.010 (5)* | |
O18 | −0.030 (9) | 0.5512 (8) | 0.2500 | 0.022 (7)* | |
O19 | −0.001 (6) | 0.3987 (6) | 0.3120 (9) | 0.019 (4)* | |
O20 | 0.010 (7) | 0.3471 (6) | 0.5406 (11) | 0.031 (5)* | |
O21 | −0.507 (7) | 0.2770 (7) | 0.2500 | 0.008 (5)* | |
O22 | 0.006 (5) | 0.2971 (5) | 0.3347 (9) | 0.015 (4)* | |
O23 | −0.492 (7) | 0.3980 (6) | 0.4680 (10) | 0.027 (5)* | |
O24 | 0.015 (5) | 0.4137 (5) | 0.6229 (9) | 0.014 (4)* | |
O25 | 0.487 (6) | 0.5346 (6) | 0.3218 (10) | 0.023 (5)* | |
O26 | −0.489 (11) | 0.4656 (11) | 0.5472 (19) | 0.073 (11)* | |
O28 | 0.519 (9) | 0.2548 (9) | 0.3937 (15) | 0.052 (8)* | |
O29 | 0.016 (6) | 0.1050 (6) | 0.2500 | 0.003 (4)* | |
O30 | −0.502 (10) | 0.4361 (9) | 0.2500 | 0.029 (8)* | |
O31 | −0.003 (5) | 0.2346 (4) | 0.1915 (8) | 0.010 (3)* | |
O32 | 0.020 (7) | 0.3376 (6) | 0.6859 (10) | 0.025 (5)* | |
O33 | −0.507 (13) | 0.4705 (12) | 0.408 (2) | 0.082 (12)* | |
O40 | 0.007 (16) | 0.4556 (15) | 0.475 (3) | 0.082 (17)* | 0.7500 |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.0043 (4) | 0.0066 (4) | 0.0066 (4) | −0.0005 (4) | −0.0011 (4) | 0.0006 (3) |
W2 | 0.0067 (6) | 0.0047 (5) | 0.0067 (6) | 0.0011 (6) | 0.0000 | 0.0000 |
W3 | 0.0052 (6) | 0.0051 (5) | 0.0094 (6) | −0.0003 (5) | 0.0000 | 0.0000 |
W4 | 0.0043 (4) | 0.0078 (4) | 0.0079 (4) | −0.0006 (4) | −0.0020 (4) | 0.0021 (3) |
W5 | 0.0045 (4) | 0.0072 (4) | 0.0058 (4) | 0.0002 (4) | −0.0006 (4) | 0.0002 (3) |
W6 | 0.0495 (11) | 0.0195 (5) | 0.0133 (5) | 0.0016 (6) | −0.0039 (6) | 0.0041 (4) |
W7 | 0.0492 (13) | 0.0060 (6) | 0.0240 (8) | −0.0005 (8) | 0.0000 | 0.0000 |
Ce8 | 0.0087 (8) | 0.0084 (6) | 0.0636 (14) | −0.0001 (5) | 0.0022 (8) | 0.0000 (7) |
Ce9 | 0.0003 (12) | 0.0060 (9) | 0.081 (2) | −0.0001 (7) | 0.0000 | 0.0000 |
Ce10 | 0.0030 (9) | 0.0235 (8) | 0.0879 (18) | −0.0019 (6) | −0.0050 (9) | 0.0368 (10) |
Geometric parameters (Å, º) top
W1—O14i | 2.17 (4) | W6—Ce8 | 3.769 (2) |
W1—W3 | 3.3573 (14) | W6—O23 | 1.74 (2) |
W1—O14 | 1.73 (4) | W6—O26 | 1.75 (4) |
W1—O15 | 1.76 (2) | W6—O33 | 1.70 (4) |
W1—O17 | 2.031 (9) | W6—O40 | 1.97 (6) |
W1—O19 | 1.76 (2) | W7—O30ii | 2.12 (4) |
W1—O22 | 2.023 (18) | W7—O19iii | 2.08 (2) |
W2—O18ii | 2.10 (4) | W7—O16iii | 1.76 (3) |
W2—Ce8iii | 3.680 (2) | W7—Ce8iii | 4.026 (2) |
W2—O25iii | 1.78 (2) | W7—Ce8 | 4.026 (2) |
W2—O29iv | 1.74 (2) | W7—O16 | 1.76 (3) |
W2—Ce8v | 3.898 (2) | W7—O19 | 2.08 (2) |
W2—Ce8ii | 3.898 (2) | W7—O30 | 1.79 (4) |
W2—Ce8 | 3.680 (2) | Ce8—O33ii | 2.67 (5) |
W2—O18 | 1.81 (4) | Ce8—O26ix | 2.53 (4) |
W2—O25 | 1.78 (2) | Ce8—O26x | 2.52 (4) |
W3—O21v | 2.15 (3) | Ce8—O24ix | 2.450 (17) |
W3—O22iii | 2.009 (19) | Ce8—O25i | 2.44 (2) |
W3—O31iii | 2.005 (17) | Ce8—O16 | 2.27 (3) |
W3—O17 | 2.04 (2) | Ce8—O18 | 3.160 (11) |
W3—O21 | 1.73 (3) | Ce8—O25 | 2.44 (2) |
W3—O22 | 2.009 (19) | Ce8—O33 | 2.64 (5) |
W3—O31 | 2.005 (17) | Ce8—O40 | 3.02 (6) |
W4—O28i | 2.12 (4) | Ce9—O31iii | 2.518 (17) |
W4—O31iii | 2.020 (18) | Ce9—O32xi | 2.46 (2) |
W4—Ce10ii | 3.760 (3) | Ce9—O32vi | 2.46 (2) |
W4—Ce10vi | 4.049 (2) | Ce9—O32xii | 2.42 (2) |
W4—Ce10 | 3.959 (3) | Ce9—O32xiii | 2.42 (2) |
W4—O12 | 1.71 (2) | Ce9—O11xii | 3.11 (3) |
W4—O13 | 1.82 (2) | Ce9—O11xiii | 3.11 (3) |
W4—O22 | 2.095 (18) | Ce9—O29 | 2.51 (2) |
W4—O28 | 1.77 (4) | Ce9—O31 | 2.518 (17) |
W5—O11i | 2.13 (4) | Ce10—O13i | 2.58 (2) |
W5—Ce9vii | 3.6848 (17) | Ce10—O15i | 2.56 (2) |
W5—Ce9viii | 3.8986 (18) | Ce10—O20i | 2.47 (3) |
W5—O11 | 1.77 (4) | Ce10—O12xiii | 2.44 (2) |
W5—O20 | 1.81 (2) | Ce10—O13 | 2.53 (2) |
W5—O24 | 1.762 (17) | Ce10—O15 | 2.53 (2) |
W5—O32 | 1.82 (2) | Ce10—O20 | 2.44 (3) |
W6—O40i | 1.97 (6) | Ce10—O23 | 2.49 (2) |
W6—Ce8i | 3.849 (2) | ||
O14i—W1—W3 | 78.4 (9) | O26ix—Ce8—O25 | 70.4 (10) |
O14i—W1—O14 | 172 (2) | O26x—Ce8—O25 | 153.1 (10) |
W3—W1—O14 | 94.4 (11) | O24ix—Ce8—O25 | 74.5 (7) |
O14i—W1—O15 | 83.7 (12) | O25i—Ce8—O25 | 105.6 (8) |
W3—W1—O15 | 123.5 (7) | O33ii—Ce8—O33 | 94.1 (14) |
O14—W1—O15 | 98.2 (13) | O26ix—Ce8—O33 | 126.3 (13) |
O14i—W1—O17 | 79.3 (12) | O26x—Ce8—O33 | 58.1 (13) |
W3—W1—O17 | 34.7 (6) | O24ix—Ce8—O33 | 131.6 (11) |
O14—W1—O17 | 96.4 (14) | O25i—Ce8—O33 | 71.7 (11) |
O15—W1—O17 | 154.9 (10) | O33ii—Ce8—O40 | 50.5 (15) |
O14i—W1—O19 | 84.5 (11) | O26ix—Ce8—O40 | 76.0 (15) |
W3—W1—O19 | 125.5 (7) | O26x—Ce8—O40 | 78.3 (15) |
O14—W1—O19 | 102.2 (13) | O24ix—Ce8—O40 | 142.3 (12) |
O15—W1—O19 | 105.1 (9) | O25i—Ce8—O40 | 124.4 (13) |
O17—W1—O19 | 91.6 (9) | W2—Ce8—W6 | 155.82 (7) |
O14i—W1—O22 | 80.1 (11) | W2—Ce8—W6ii | 114.69 (6) |
W3—W1—O22 | 33.5 (6) | W6—Ce8—W6ii | 61.39 (4) |
O14—W1—O22 | 92.4 (12) | W2—Ce8—W2xiv | 61.68 (4) |
O15—W1—O22 | 90.9 (9) | W6—Ce8—W2xiv | 111.54 (5) |
O17—W1—O22 | 68.1 (8) | W6ii—Ce8—W2xiv | 156.74 (6) |
O19—W1—O22 | 156.4 (9) | W2—Ce8—W7 | 72.15 (5) |
O18ii—W2—Ce8iii | 115.4 (4) | W6—Ce8—W7 | 83.68 (4) |
O18ii—W2—O25iii | 80.4 (8) | W6ii—Ce8—W7 | 85.65 (5) |
Ce8iii—W2—O25iii | 35.0 (8) | W2xiv—Ce8—W7 | 71.28 (5) |
O18ii—W2—O29iv | 89.3 (11) | W2—Ce8—O16 | 73.7 (7) |
Ce8iii—W2—O29iv | 115.5 (4) | W6—Ce8—O16 | 82.2 (7) |
O25iii—W2—O29iv | 116.1 (7) | W6ii—Ce8—O16 | 82.3 (7) |
O18ii—W2—Ce8v | 54.0 (3) | W2xiv—Ce8—O16 | 74.6 (7) |
Ce8iii—W2—Ce8v | 61.68 (4) | W7—Ce8—O16 | 3.4 (7) |
O25iii—W2—Ce8v | 26.8 (8) | W2—Ce8—O18 | 29.5 (6) |
O29iv—W2—Ce8v | 106.9 (5) | W6—Ce8—O18 | 137.1 (6) |
O18ii—W2—Ce8ii | 54.0 (3) | W6ii—Ce8—O18 | 137.6 (6) |
Ce8iii—W2—Ce8ii | 136.46 (6) | W2xiv—Ce8—O18 | 32.6 (6) |
O25iii—W2—Ce8ii | 115.7 (7) | W7—Ce8—O18 | 65.0 (5) |
O29iv—W2—Ce8ii | 106.9 (5) | W2—Ce8—O25 | 24.8 (5) |
Ce8v—W2—Ce8ii | 97.59 (7) | W6—Ce8—O25 | 148.1 (5) |
O18ii—W2—Ce8 | 115.4 (4) | W6ii—Ce8—O25 | 91.5 (5) |
Ce8iii—W2—Ce8 | 105.69 (7) | W2xiv—Ce8—O25 | 86.4 (5) |
O25iii—W2—Ce8 | 125.9 (7) | W7—Ce8—O25 | 77.4 (5) |
O29iv—W2—Ce8 | 115.5 (4) | W2—Ce8—O33 | 138.5 (9) |
Ce8v—W2—Ce8 | 136.46 (6) | W6—Ce8—O33 | 23.2 (10) |
O18ii—W2—O18 | 167.2 (18) | W6ii—Ce8—O33 | 80.5 (10) |
Ce8iii—W2—O18 | 59.2 (4) | W2xiv—Ce8—O33 | 88.9 (10) |
O25iii—W2—O18 | 93.7 (9) | W7—Ce8—O33 | 70.8 (9) |
O29iv—W2—O18 | 103.5 (12) | W2—Ce8—O40 | 142.8 (12) |
Ce8v—W2—O18 | 120.4 (5) | W6—Ce8—O40 | 31.4 (12) |
O18ii—W2—O25 | 80.4 (8) | W6ii—Ce8—O40 | 30.5 (12) |
Ce8iii—W2—O25 | 125.9 (7) | W2xiv—Ce8—O40 | 141.1 (12) |
O25iii—W2—O25 | 123.7 (14) | W7—Ce8—O40 | 88.0 (11) |
O29iv—W2—O25 | 116.1 (7) | O16—Ce8—O18 | 67.9 (9) |
Ce8v—W2—O25 | 115.7 (7) | O16—Ce8—O25 | 77.5 (9) |
Ce8ii—W2—Ce8 | 61.68 (4) | O18—Ce8—O25 | 54.0 (8) |
Ce8ii—W2—O18 | 120.4 (5) | O16—Ce8—O33 | 70.5 (12) |
Ce8—W2—O18 | 59.2 (4) | O18—Ce8—O33 | 114.4 (11) |
Ce8ii—W2—O25 | 26.8 (8) | O25—Ce8—O33 | 147.7 (11) |
Ce8—W2—O25 | 35.0 (8) | O16—Ce8—O40 | 85.1 (13) |
O18—W2—O25 | 93.7 (9) | O18—Ce8—O40 | 153.0 (12) |
O21v—W3—O22iii | 82.5 (6) | O25—Ce8—O40 | 121.6 (13) |
O21v—W3—O31iii | 83.7 (7) | O33—Ce8—O40 | 52.7 (15) |
O22iii—W3—O31iii | 148.3 (7) | O31iii—Ce9—O32xi | 117.6 (7) |
O21v—W3—W1 | 81.5 (5) | O31iii—Ce9—O32vi | 83.3 (6) |
O22iii—W3—W1 | 101.7 (5) | O32xi—Ce9—O32vi | 69.6 (11) |
O31iii—W3—W1 | 104.2 (5) | O31iii—Ce9—O32xii | 115.7 (7) |
O21v—W3—W1iii | 81.5 (5) | O32xi—Ce9—O32xii | 105.7 (8) |
O22iii—W3—W1iii | 33.8 (5) | O32vi—Ce9—O32xii | 159.2 (10) |
O31iii—W3—W1iii | 164.2 (5) | O31iii—Ce9—O32xiii | 80.9 (6) |
W1—W3—W1iii | 68.15 (4) | O32xi—Ce9—O32xiii | 159.2 (10) |
O21v—W3—O17 | 84.8 (10) | O32vi—Ce9—O32xiii | 105.7 (8) |
O22iii—W3—O17 | 68.2 (5) | O32xii—Ce9—O32xiii | 71.1 (11) |
O31iii—W3—O17 | 138.4 (5) | O31iii—Ce9—W5xii | 136.6 (4) |
W1—W3—O17 | 34.41 (10) | O32xi—Ce9—W5xii | 81.7 (5) |
W1iii—W3—O17 | 34.41 (10) | O32vi—Ce9—W5xii | 139.4 (5) |
O21v—W3—O21 | 179.8 (14) | O32xii—Ce9—W5xii | 25.2 (5) |
O22iii—W3—O21 | 97.4 (6) | O32xiii—Ce9—W5xii | 90.9 (5) |
O31iii—W3—O21 | 96.5 (8) | O31iii—Ce9—W5xiii | 85.5 (4) |
W1—W3—O21 | 98.3 (7) | O32xi—Ce9—W5xiii | 139.4 (5) |
W1iii—W3—O21 | 98.3 (7) | O32vi—Ce9—W5xiii | 81.7 (5) |
O21v—W3—O22 | 82.5 (6) | O32xii—Ce9—W5xiii | 90.9 (5) |
O22iii—W3—O22 | 134.8 (10) | O32xiii—Ce9—W5xiii | 25.2 (5) |
O31iii—W3—O22 | 70.8 (7) | O31iii—Ce9—O11xii | 145.4 (7) |
W1—W3—O22 | 33.8 (5) | O32xi—Ce9—O11xii | 53.2 (9) |
W1iii—W3—O22 | 101.7 (5) | O32vi—Ce9—O11xii | 115.9 (9) |
O21v—W3—O31 | 83.7 (7) | O32xii—Ce9—O11xii | 53.3 (9) |
O22iii—W3—O31 | 70.8 (7) | O32xiii—Ce9—O11xii | 117.2 (9) |
O31iii—W3—O31 | 79.5 (10) | O31iii—Ce9—O11xiii | 84.2 (7) |
W1—W3—O31 | 164.2 (5) | O32xi—Ce9—O11xiii | 115.9 (9) |
W1iii—W3—O31 | 104.2 (5) | O32vi—Ce9—O11xiii | 53.2 (9) |
O17—W3—O21 | 95.0 (11) | O32xii—Ce9—O11xiii | 117.2 (9) |
O17—W3—O22 | 68.2 (5) | O32xiii—Ce9—O11xiii | 53.3 (9) |
O21—W3—O22 | 97.4 (6) | O31iii—Ce9—W5xi | 135.4 (4) |
O17—W3—O31 | 138.4 (5) | O32xi—Ce9—W5xi | 20.7 (5) |
O21—W3—O31 | 96.5 (8) | O32vi—Ce9—W5xi | 85.3 (5) |
O22—W3—O31 | 148.3 (7) | O32xii—Ce9—W5xi | 86.3 (6) |
O28i—W4—O31iii | 82.5 (10) | O32xiii—Ce9—W5xi | 143.7 (5) |
O28i—W4—Ce10ii | 116.2 (9) | O31iii—Ce9—W5vi | 87.1 (4) |
O31iii—W4—Ce10ii | 139.0 (5) | O32xi—Ce9—W5vi | 85.3 (5) |
O28i—W4—Ce10vi | 89.5 (9) | O32vi—Ce9—W5vi | 20.7 (5) |
O31iii—W4—Ce10vi | 113.6 (5) | O32xii—Ce9—W5vi | 143.7 (5) |
Ce10ii—W4—Ce10vi | 103.26 (4) | O32xiii—Ce9—W5vi | 86.3 (6) |
O28i—W4—Ce10 | 55.8 (9) | O31iii—Ce9—O29 | 149.4 (4) |
O31iii—W4—Ce10 | 126.0 (5) | O32xi—Ce9—O29 | 79.5 (7) |
Ce10ii—W4—Ce10 | 60.44 (5) | O32vi—Ce9—O29 | 79.5 (7) |
Ce10vi—W4—Ce10 | 99.80 (4) | O32xii—Ce9—O29 | 79.7 (7) |
O28i—W4—O12 | 85.8 (12) | O32xiii—Ce9—O29 | 79.7 (7) |
O31iii—W4—O12 | 98.4 (9) | O31iii—Ce9—O31 | 61.2 (8) |
Ce10ii—W4—O12 | 118.1 (8) | O32xi—Ce9—O31 | 83.3 (6) |
Ce10vi—W4—O12 | 15.3 (8) | O32vi—Ce9—O31 | 117.6 (7) |
Ce10—W4—O12 | 109.6 (8) | O32xii—Ce9—O31 | 80.9 (6) |
O28i—W4—O13 | 81.9 (11) | O32xiii—Ce9—O31 | 115.7 (7) |
O31iii—W4—O13 | 153.0 (8) | W5xii—Ce9—W5xiii | 104.56 (6) |
Ce10ii—W4—O13 | 37.8 (7) | W5xii—Ce9—O11xii | 28.6 (7) |
Ce10vi—W4—O13 | 88.1 (6) | W5xiii—Ce9—O11xii | 123.9 (6) |
Ce10—W4—O13 | 29.2 (7) | W5xii—Ce9—O11xiii | 123.9 (6) |
O28i—W4—O22 | 81.4 (10) | W5xiii—Ce9—O11xiii | 28.6 (7) |
O31iii—W4—O22 | 68.8 (7) | O11xii—Ce9—O11xiii | 130.4 (12) |
Ce10ii—W4—O22 | 78.0 (5) | W5xii—Ce9—W5xi | 61.63 (2) |
Ce10vi—W4—O22 | 170.3 (6) | W5xiii—Ce9—W5xi | 135.04 (7) |
Ce10—W4—O22 | 72.3 (5) | O11xii—Ce9—W5xi | 33.1 (7) |
O28i—W4—O28 | 174.6 (19) | O11xiii—Ce9—W5xi | 121.3 (6) |
O31iii—W4—O28 | 97.5 (12) | W5xii—Ce9—W5vi | 135.04 (7) |
Ce10ii—W4—O28 | 60.6 (10) | W5xiii—Ce9—W5vi | 61.63 (2) |
Ce10vi—W4—O28 | 95.5 (10) | O11xii—Ce9—W5vi | 121.3 (6) |
Ce10—W4—O28 | 121.0 (10) | O11xiii—Ce9—W5vi | 33.1 (7) |
O12—W4—O13 | 102.3 (10) | W5xi—Ce9—W5vi | 96.77 (6) |
O12—W4—O22 | 162.9 (10) | W5xii—Ce9—O29 | 67.2 (3) |
O13—W4—O22 | 87.3 (8) | W5xiii—Ce9—O29 | 67.2 (3) |
O12—W4—O28 | 99.5 (13) | O11xii—Ce9—O29 | 65.2 (6) |
O13—W4—O28 | 96.1 (12) | O11xiii—Ce9—O29 | 65.2 (6) |
O22—W4—O28 | 93.5 (12) | W5xi—Ce9—O29 | 68.2 (3) |
O11i—W5—Ce9vii | 114.4 (9) | W5xii—Ce9—O31 | 85.5 (4) |
O11i—W5—Ce9viii | 52.8 (9) | W5xiii—Ce9—O31 | 136.6 (4) |
Ce9vii—W5—Ce9viii | 61.63 (2) | O11xii—Ce9—O31 | 84.2 (7) |
O11i—W5—O11 | 170.6 (19) | O11xiii—Ce9—O31 | 145.4 (7) |
Ce9vii—W5—O11 | 57.5 (11) | W5xi—Ce9—O31 | 87.1 (4) |
Ce9viii—W5—O11 | 119.0 (11) | W5vi—Ce9—O29 | 68.2 (3) |
O11i—W5—O20 | 84.0 (12) | W5vi—Ce9—O31 | 135.4 (4) |
Ce9vii—W5—O20 | 130.3 (8) | O29—Ce9—O31 | 149.4 (4) |
Ce9viii—W5—O20 | 119.4 (8) | O13i—Ce10—O15i | 61.2 (7) |
O11—W5—O20 | 98.0 (13) | O13i—Ce10—O20i | 69.7 (7) |
O11i—W5—O24 | 86.9 (11) | O15i—Ce10—O20i | 66.2 (7) |
Ce9vii—W5—O24 | 112.4 (6) | O13i—Ce10—O12xiii | 77.5 (7) |
Ce9viii—W5—O24 | 104.3 (6) | O15i—Ce10—O12xiii | 129.6 (7) |
O11—W5—O24 | 100.5 (12) | O20i—Ce10—O12xiii | 73.5 (8) |
O20—W5—O24 | 114.4 (10) | O13i—Ce10—W4i | 25.6 (5) |
O11i—W5—O32 | 80.4 (12) | O15i—Ce10—W4i | 68.3 (5) |
Ce9vii—W5—O32 | 34.5 (8) | O20i—Ce10—W4i | 95.1 (6) |
Ce9viii—W5—O32 | 28.6 (8) | O12xiii—Ce10—W4i | 87.1 (5) |
O11—W5—O32 | 90.9 (13) | O13i—Ce10—W4 | 84.0 (5) |
O20—W5—O32 | 123.8 (10) | O15i—Ce10—W4 | 113.8 (5) |
O24—W5—O32 | 118.1 (9) | O20i—Ce10—W4 | 150.0 (6) |
O40i—W6—Ce8i | 50.9 (16) | O12xiii—Ce10—W4 | 87.3 (5) |
O40i—W6—Ce8 | 111.8 (16) | W4i—Ce10—W4 | 60.44 (5) |
Ce8i—W6—Ce8 | 61.39 (4) | O13i—Ce10—W4xiii | 73.5 (5) |
O40i—W6—O23 | 100.1 (18) | O15i—Ce10—W4xiii | 130.9 (5) |
Ce8i—W6—O23 | 129.9 (8) | O20i—Ce10—W4xiii | 81.6 (5) |
Ce8—W6—O23 | 130.7 (8) | O12xiii—Ce10—W4xiii | 10.7 (5) |
O40i—W6—O26 | 86 (2) | W4i—Ce10—W4xiii | 79.38 (4) |
Ce8i—W6—O26 | 101.6 (13) | O13i—Ce10—O13 | 99.1 (7) |
Ce8—W6—O26 | 101.3 (13) | O15i—Ce10—O13 | 133.7 (7) |
O23—W6—O26 | 117.8 (15) | O20i—Ce10—O13 | 150.3 (7) |
O40i—W6—O33 | 83 (2) | O12xiii—Ce10—O13 | 77.3 (7) |
Ce8i—W6—O33 | 36.1 (16) | W4i—Ce10—O13 | 78.2 (5) |
Ce8—W6—O33 | 37.8 (16) | O13i—Ce10—O15 | 133.8 (7) |
O23—W6—O33 | 117.1 (16) | O15i—Ce10—O15 | 99.9 (7) |
O26—W6—O33 | 125.0 (19) | O20i—Ce10—O15 | 144.8 (7) |
O40i—W6—O40 | 160 (3) | O12xiii—Ce10—O15 | 130.2 (7) |
Ce8i—W6—O40 | 113.8 (16) | W4i—Ce10—O15 | 110.0 (5) |
Ce8—W6—O40 | 52.9 (16) | O13i—Ce10—O20 | 150.5 (7) |
O23—W6—O40 | 99.8 (18) | O15i—Ce10—O20 | 144.9 (7) |
O26—W6—O40 | 85 (2) | O20i—Ce10—O20 | 104.9 (9) |
O33—W6—O40 | 87 (2) | O12xiii—Ce10—O20 | 73.3 (8) |
O30ii—W7—O19iii | 80.8 (9) | W4i—Ce10—O20 | 146.2 (6) |
O30ii—W7—O16iii | 89.6 (12) | O13i—Ce10—O23 | 126.0 (7) |
O19iii—W7—O16iii | 88.4 (11) | O15i—Ce10—O23 | 66.6 (7) |
O30ii—W7—Ce8iii | 92.3 (6) | O20i—Ce10—O23 | 77.8 (8) |
O19iii—W7—Ce8iii | 92.2 (6) | O12xiii—Ce10—O23 | 132.2 (8) |
O16iii—W7—Ce8iii | 4.3 (9) | W4i—Ce10—O23 | 133.2 (6) |
O30ii—W7—Ce8 | 92.3 (6) | W4—Ce10—W4xiii | 77.13 (4) |
O19iii—W7—Ce8 | 171.2 (6) | W4—Ce10—O13 | 20.5 (5) |
O16iii—W7—Ce8 | 97.0 (9) | W4xiii—Ce10—O13 | 68.7 (5) |
Ce8iii—W7—Ce8 | 93.50 (7) | W4—Ce10—O15 | 64.9 (5) |
O30ii—W7—O16 | 89.6 (12) | W4xiii—Ce10—O15 | 126.0 (5) |
O19iii—W7—O16 | 167.0 (11) | O13—Ce10—O15 | 62.2 (7) |
O16iii—W7—O16 | 100.4 (18) | W4—Ce10—O20 | 90.7 (6) |
Ce8iii—W7—O16 | 97.0 (9) | W4xiii—Ce10—O20 | 77.0 (6) |
Ce8—W7—O16 | 4.3 (9) | O13—Ce10—O20 | 70.9 (7) |
O30ii—W7—O19 | 80.8 (9) | O15—Ce10—O20 | 67.1 (7) |
O19iii—W7—O19 | 81.5 (11) | W4—Ce10—O23 | 131.2 (6) |
O16iii—W7—O19 | 167.0 (11) | W4xiii—Ce10—O23 | 142.5 (5) |
Ce8iii—W7—O19 | 171.2 (6) | O13—Ce10—O23 | 127.7 (7) |
Ce8—W7—O19 | 92.2 (6) | O15—Ce10—O23 | 67.1 (7) |
O30ii—W7—O30 | 167.0 (19) | O20—Ce10—O23 | 78.5 (8) |
O19iii—W7—O30 | 89.4 (10) | W5ii—O11—Ce9vii | 94.1 (12) |
O16iii—W7—O30 | 98.7 (12) | W5ii—O11—W5 | 170.6 (19) |
Ce8iii—W7—O30 | 96.6 (7) | Ce9vii—O11—W5 | 93.9 (13) |
Ce8—W7—O30 | 96.6 (7) | Ce10vi—O12—W4 | 154.0 (13) |
O16—W7—O19 | 88.4 (11) | Ce10ii—O13—Ce10 | 99.1 (7) |
O16—W7—O30 | 98.7 (12) | Ce10ii—O13—W4 | 116.6 (10) |
O19—W7—O30 | 89.4 (10) | Ce10—O13—W4 | 130.4 (10) |
O33ii—Ce8—O26ix | 57.5 (13) | W1ii—O14—W1 | 172 (2) |
O33ii—Ce8—O26x | 126.5 (13) | Ce10ii—O15—Ce10 | 99.9 (7) |
O26ix—Ce8—O26x | 100.6 (14) | Ce10ii—O15—W1 | 115.9 (10) |
O33ii—Ce8—O24ix | 131.5 (11) | Ce10—O15—W1 | 129.2 (11) |
O26ix—Ce8—O24ix | 79.3 (10) | Ce8—O16—W7 | 172.3 (16) |
O26x—Ce8—O24ix | 78.9 (10) | W3—O17—W1iii | 110.9 (6) |
O33ii—Ce8—O25i | 148.0 (11) | W3—O17—W1 | 110.9 (6) |
O26ix—Ce8—O25i | 153.1 (10) | W1iii—O17—W1 | 135.7 (13) |
O26x—Ce8—O25i | 70.6 (11) | W2i—O18—W2 | 167.2 (18) |
O24ix—Ce8—O25i | 74.2 (7) | W2i—O18—Ce8 | 93.4 (7) |
O33ii—Ce8—W2 | 93.2 (10) | W2—O18—Ce8 | 91.4 (8) |
O26ix—Ce8—W2 | 91.5 (9) | W2i—O18—Ce8iii | 93.4 (7) |
O26x—Ce8—W2 | 138.8 (9) | W2—O18—Ce8iii | 91.4 (8) |
O24ix—Ce8—W2 | 64.9 (5) | Ce8—O18—Ce8iii | 136.3 (10) |
O25i—Ce8—W2 | 80.9 (5) | W7—O19—W1 | 156.5 (12) |
O33ii—Ce8—W6 | 79.1 (10) | Ce10ii—O20—Ce10 | 104.9 (9) |
O26ix—Ce8—W6 | 103.1 (9) | Ce10ii—O20—W5 | 120.3 (12) |
O26x—Ce8—W6 | 57.6 (9) | Ce10—O20—W5 | 134.6 (13) |
O24ix—Ce8—W6 | 136.3 (5) | W3i—O21—W3 | 179.8 (14) |
O25i—Ce8—W6 | 93.5 (5) | W4—O22—W1 | 137.9 (10) |
O33ii—Ce8—W6ii | 21.9 (10) | W4—O22—W3 | 108.6 (8) |
O26ix—Ce8—W6ii | 56.2 (9) | W1—O22—W3 | 112.7 (9) |
O26x—Ce8—W6ii | 104.6 (9) | Ce10—O23—W6 | 170.3 (13) |
O24ix—Ce8—W6ii | 135.4 (5) | Ce8ix—O24—W5 | 170.0 (11) |
O25i—Ce8—W6ii | 149.8 (5) | Ce8—O25—Ce8ii | 105.6 (8) |
O33ii—Ce8—W2xiv | 141.8 (9) | Ce8—O25—W2 | 120.2 (11) |
O26ix—Ce8—W2xiv | 142.6 (9) | Ce8ii—O25—W2 | 134.0 (12) |
O26x—Ce8—W2xiv | 86.8 (9) | Ce8ix—O26—Ce8x | 100.6 (14) |
O24ix—Ce8—W2xiv | 66.1 (5) | Ce8ix—O26—W6 | 130 (2) |
O25i—Ce8—W2xiv | 19.2 (5) | Ce8x—O26—W6 | 129 (2) |
O33ii—Ce8—W7 | 73.8 (9) | W4ii—O28—W4 | 174.6 (19) |
O26ix—Ce8—W7 | 127.8 (9) | Ce9—O29—W2xv | 173.6 (13) |
O26x—Ce8—W7 | 124.5 (9) | W7i—O30—W7 | 167.0 (19) |
O24ix—Ce8—W7 | 129.7 (5) | Ce9—O31—W4iii | 138.5 (8) |
O25i—Ce8—W7 | 74.4 (5) | Ce9—O31—W3 | 109.4 (7) |
O33ii—Ce8—O16 | 70.6 (12) | W4iii—O31—W3 | 111.9 (8) |
O26ix—Ce8—O16 | 125.2 (12) | Ce9viii—O32—Ce9vi | 105.7 (8) |
O26x—Ce8—O16 | 125.4 (12) | Ce9viii—O32—W5 | 130.6 (12) |
O24ix—Ce8—O16 | 132.5 (8) | Ce9vi—O32—W5 | 120.3 (12) |
O25i—Ce8—O16 | 77.5 (9) | Ce8i—O33—Ce8 | 94.1 (14) |
O33ii—Ce8—O18 | 116.0 (11) | Ce8i—O33—W6 | 122 (2) |
O26ix—Ce8—O18 | 119.0 (11) | Ce8—O33—W6 | 119 (2) |
O26x—Ce8—O18 | 117.1 (11) | W6—O40—W6ii | 160 (3) |
O24ix—Ce8—O18 | 64.7 (7) | W6—O40—Ce8 | 96 (2) |
O25i—Ce8—O18 | 51.6 (8) | W6ii—O40—Ce8 | 99 (2) |
O33ii—Ce8—O25 | 71.1 (11) |
Symmetry codes: (i) x−1, y, z; (ii) x+1, y, z; (iii) x, y, −z+1/2; (iv) −x+1/2, y+1/2, z; (v) x+1, y, −z+1/2; (vi) x+1/2, −y+1/2, −z+1; (vii) x+1/2, −y+1/2, z+1/2; (viii) x−1/2, −y+1/2, z+1/2; (ix) −x, −y+1, −z+1; (x) −x−1, −y+1, −z+1; (xi) x+1/2, −y+1/2, z−1/2; (xii) x−1/2, −y+1/2, z−1/2; (xiii) x−1/2, −y+1/2, −z+1; (xiv) x−1, y, −z+1/2; (xv) −x+1/2, y−1/2, z. |