Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105015386/iz1055sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270105015386/iz1055Isup2.hkl |
Single crystals of La5Mo6O21 were prepared from a stoichiometric mixture of La2O3, MoO3 and Mo. The initial mixture (ca 5 g) was cold pressed and loaded into a molybdenum crucible, which was sealed under a low argon pressure using an arc welding system. The charge was heated at the rate of 300 K h−1 up to 2223 K; the temperature was held for 5 min, then cooled at 100 K h−1 down to 1373 K, and finally allowed to cool in the furnace.
Data collection: COLLECT (Nonius, 1998); cell refinement: COLLECT; data reduction: EVALCCD (Duisenberg, 1998); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: SHELXL97.
La5Mo6O21 | Dx = 6.584 Mg m−3 |
Mr = 1606.19 | Mo Kα radiation, λ = 0.71069 Å |
Orthorhombic, P212121 | Cell parameters from 48314 reflections |
a = 5.71550 (5) Å | θ = 1–40.3° |
b = 11.2429 (1) Å | µ = 17.45 mm−1 |
c = 25.2146 (2) Å | T = 293 K |
V = 1620.26 (2) Å3 | Needle, black |
Z = 4 | 0.45 × 0.04 × 0.03 mm |
F(000) = 2820 |
Nonius KappaCCD diffractometer | 9991 independent reflections |
Radiation source: fine-focus sealed tube | 9029 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.081 |
ϕ scans (κ = 0) + additional ω scans | θmax = 40.3°, θmin = 1.6° |
Absorption correction: analytical (de Meulenaar & Tompa, 1965) | h = −10→10 |
Tmin = 0.116, Tmax = 0.690 | k = −20→20 |
34498 measured reflections | l = −44→45 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0307P)2 + 6.5608P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.036 | (Δ/σ)max = 0.001 |
wR(F2) = 0.088 | Δρmax = 4.10 e Å−3 |
S = 1.07 | Δρmin = −4.15 e Å−3 |
9991 reflections | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
291 parameters | Extinction coefficient: 0.00036 (6) |
0 restraints | Absolute structure: Flack (1983), 4271 Friedel pairs? |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.393 (12) |
La5Mo6O21 | V = 1620.26 (2) Å3 |
Mr = 1606.19 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 5.71550 (5) Å | µ = 17.45 mm−1 |
b = 11.2429 (1) Å | T = 293 K |
c = 25.2146 (2) Å | 0.45 × 0.04 × 0.03 mm |
Nonius KappaCCD diffractometer | 9991 independent reflections |
Absorption correction: analytical (de Meulenaar & Tompa, 1965) | 9029 reflections with I > 2σ(I) |
Tmin = 0.116, Tmax = 0.690 | Rint = 0.081 |
34498 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 0 restraints |
wR(F2) = 0.088 | Δρmax = 4.10 e Å−3 |
S = 1.07 | Δρmin = −4.15 e Å−3 |
9991 reflections | Absolute structure: Flack (1983), 4271 Friedel pairs? |
291 parameters | Absolute structure parameter: 0.393 (12) |
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. |
x | y | z | Uiso*/Ueq | ||
La1 | 0.25191 (6) | 0.22146 (2) | 0.099731 (10) | 0.00815 (4) | |
La2 | 0.75734 (6) | 0.06237 (2) | 0.185580 (10) | 0.00796 (4) | |
La3 | 0.75409 (6) | 0.02754 (2) | 0.029854 (11) | 0.01038 (5) | |
La4 | 1.75479 (6) | 0.43400 (2) | 0.183542 (10) | 0.00954 (4) | |
La5 | 0.76670 (6) | −0.31817 (2) | 0.050029 (12) | 0.01101 (5) | |
Mo1 | 0.25545 (9) | 0.16004 (3) | −0.039840 (14) | 0.00633 (5) | |
Mo2 | 0.25851 (8) | −0.07928 (3) | 0.084057 (15) | 0.00697 (6) | |
Mo3 | 1.02722 (6) | 0.25011 (5) | 0.30992 (2) | 0.00566 (8) | |
Mo4 | 1.25868 (8) | 0.29643 (3) | 0.225608 (14) | 0.00599 (5) | |
Mo5 | 0.47633 (6) | 0.24838 (5) | 0.31147 (2) | 0.00586 (8) | |
Mo6 | 0.24310 (8) | 0.52726 (3) | 0.108097 (14) | 0.00643 (5) | |
O1 | 0.4759 (7) | 0.0280 (5) | 0.1128 (2) | 0.0134 (9) | |
O2 | 0.4843 (7) | −0.1624 (4) | 0.0438 (2) | 0.0125 (8) | |
O3 | 1.0097 (6) | 0.2387 (5) | 0.1789 (2) | 0.0101 (8) | |
O4 | 0.2004 (7) | 0.2834 (4) | −0.08339 (19) | 0.0162 (8) | |
O5 | 0.2468 (7) | 0.3296 (3) | 0.35820 (13) | 0.0084 (4) | |
O6 | 0.1876 (6) | 0.6051 (4) | 0.04771 (17) | 0.0128 (7) | |
O7 | 1.0125 (6) | 0.3973 (4) | 0.2638 (2) | 0.0083 (8) | |
O8 | 1.5190 (7) | 0.6145 (5) | 0.1331 (2) | 0.0089 (7) | |
O9 | 0.2770 (7) | 0.4298 (3) | 0.16923 (17) | 0.0138 (7) | |
O10 | 1.4922 (6) | 0.3958 (5) | 0.26592 (19) | 0.0085 (8) | |
O11 | 1.5051 (6) | 0.2369 (5) | 0.1809 (2) | 0.0096 (7) | |
O12 | 1.0148 (6) | 0.0372 (4) | 0.1065 (2) | 0.0086 (7) | |
O13 | 1.9803 (7) | 0.6128 (5) | 0.1405 (2) | 0.0100 (8) | |
O14 | 0.7541 (7) | 0.3223 (3) | 0.35564 (14) | 0.0090 (5) | |
O15 | 0.2533 (7) | 0.1393 (3) | 0.26764 (13) | 0.0079 (4) | |
O16 | 1.0175 (7) | −0.1452 (4) | 0.0360 (2) | 0.0112 (8) | |
O17 | 0.7476 (7) | 0.1758 (3) | 0.27448 (13) | 0.0078 (4) | |
O18 | 0.0457 (7) | 0.2530 (5) | 0.0139 (2) | 0.0203 (9) | |
O19 | −0.0337 (7) | 0.4148 (4) | 0.09050 (19) | 0.0135 (7) | |
O20 | 0.2973 (6) | 0.0457 (4) | 0.01562 (19) | 0.0153 (7) | |
O21 | −0.0350 (7) | 0.0775 (4) | −0.0646 (2) | 0.0151 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
La1 | 0.00808 (8) | 0.00789 (8) | 0.00849 (9) | −0.00012 (10) | −0.00048 (12) | −0.00002 (6) |
La2 | 0.00718 (8) | 0.00723 (8) | 0.00949 (9) | 0.00005 (10) | 0.00018 (12) | 0.00028 (6) |
La3 | 0.00844 (9) | 0.01179 (9) | 0.01091 (10) | 0.00121 (12) | −0.00086 (12) | −0.00200 (7) |
La4 | 0.00810 (8) | 0.00974 (9) | 0.01079 (10) | −0.00007 (11) | 0.00012 (13) | 0.00026 (6) |
La5 | 0.01049 (10) | 0.00979 (9) | 0.01276 (11) | 0.00109 (10) | 0.00025 (11) | 0.00023 (7) |
Mo1 | 0.00506 (11) | 0.00662 (11) | 0.00730 (13) | 0.00027 (14) | −0.00025 (16) | 0.00010 (9) |
Mo2 | 0.00608 (12) | 0.00677 (11) | 0.00807 (13) | 0.00063 (15) | −0.00011 (16) | 0.00024 (9) |
Mo3 | 0.00432 (12) | 0.0060 (2) | 0.0067 (2) | 0.00009 (12) | 0.00024 (12) | 0.00003 (18) |
Mo4 | 0.00540 (11) | 0.00616 (11) | 0.00640 (12) | 0.00016 (13) | −0.00020 (15) | 0.00032 (9) |
Mo5 | 0.00430 (12) | 0.0058 (2) | 0.0074 (2) | 0.00006 (12) | −0.00018 (12) | 0.00004 (18) |
Mo6 | 0.00539 (11) | 0.00637 (11) | 0.00752 (13) | 0.00064 (15) | −0.00006 (16) | 0.00020 (9) |
O1 | 0.0085 (13) | 0.0110 (18) | 0.021 (2) | −0.0011 (12) | −0.0001 (14) | 0.0001 (17) |
O2 | 0.0099 (14) | 0.015 (2) | 0.012 (2) | 0.0014 (12) | 0.0018 (13) | 0.0000 (16) |
O3 | 0.0087 (13) | 0.012 (2) | 0.0091 (18) | 0.0007 (12) | −0.0014 (13) | −0.0014 (17) |
O4 | 0.0190 (17) | 0.0134 (16) | 0.0162 (19) | −0.0015 (12) | −0.0048 (14) | 0.0038 (13) |
O5 | 0.0052 (10) | 0.0105 (11) | 0.0095 (12) | 0.0012 (14) | −0.0016 (15) | −0.0026 (9) |
O6 | 0.0149 (14) | 0.0139 (16) | 0.0095 (16) | 0.0044 (11) | −0.0003 (12) | 0.0026 (13) |
O7 | 0.0071 (13) | 0.0076 (19) | 0.010 (2) | 0.0024 (11) | 0.0012 (13) | 0.0004 (16) |
O8 | 0.0066 (12) | 0.0109 (19) | 0.0093 (18) | −0.0008 (11) | 0.0002 (12) | −0.0020 (13) |
O9 | 0.0161 (17) | 0.0101 (13) | 0.0151 (16) | −0.0014 (13) | −0.0027 (14) | 0.0066 (11) |
O10 | 0.0070 (13) | 0.009 (2) | 0.009 (2) | −0.0008 (11) | 0.0016 (13) | 0.0018 (16) |
O11 | 0.0066 (12) | 0.012 (2) | 0.0100 (18) | 0.0031 (12) | 0.0007 (12) | −0.0021 (17) |
O12 | 0.0076 (12) | 0.0060 (16) | 0.0123 (18) | −0.0002 (10) | −0.0001 (12) | −0.0002 (13) |
O13 | 0.0077 (13) | 0.0094 (18) | 0.013 (2) | 0.0022 (11) | −0.0012 (12) | −0.0039 (14) |
O14 | 0.0045 (10) | 0.0104 (11) | 0.0121 (13) | 0.0011 (15) | 0.0030 (15) | −0.0027 (9) |
O15 | 0.0079 (10) | 0.0074 (10) | 0.0085 (12) | −0.0021 (15) | −0.0025 (16) | 0.0003 (8) |
O16 | 0.0114 (14) | 0.0104 (17) | 0.012 (2) | 0.0027 (12) | −0.0029 (13) | −0.0013 (14) |
O17 | 0.0047 (9) | 0.0093 (11) | 0.0094 (12) | 0.0047 (14) | −0.0010 (15) | −0.0025 (8) |
O18 | 0.0126 (15) | 0.035 (3) | 0.0130 (19) | 0.0117 (16) | 0.0009 (14) | −0.0069 (18) |
O19 | 0.0121 (14) | 0.0119 (16) | 0.017 (2) | −0.0035 (12) | −0.0025 (13) | −0.0020 (14) |
O20 | 0.0121 (15) | 0.0156 (16) | 0.018 (2) | 0.0035 (11) | 0.0003 (13) | 0.0065 (14) |
O21 | 0.0106 (13) | 0.0143 (17) | 0.020 (2) | −0.0050 (12) | −0.0042 (14) | −0.0048 (15) |
La1—O3i | 2.437 (5) | Mo3—O13xiii | 1.987 (5) |
La1—O12i | 2.481 (4) | Mo3—O17 | 2.013 (4) |
La1—O18 | 2.489 (5) | Mo3—O7 | 2.025 (5) |
La1—O11i | 2.513 (5) | Mo3—O15v | 2.087 (4) |
La1—O1 | 2.546 (5) | Mo3—O14 | 2.104 (4) |
La1—O4ii | 2.597 (4) | Mo3—Mo4 | 2.5574 (6) |
La1—O21ii | 2.716 (5) | Mo3—Mo5v | 2.5672 (4) |
La1—O19 | 2.729 (4) | Mo3—Mo5 | 3.1489 (4) |
La1—O20 | 2.910 (5) | Mo3—La2vi | 3.7221 (6) |
La1—O9 | 2.929 (4) | Mo4—O11 | 1.924 (4) |
La1—Mo4i | 3.2842 (4) | Mo4—O3 | 1.958 (4) |
La1—Mo2 | 3.4044 (4) | Mo4—O10 | 2.016 (5) |
La2—O11i | 2.438 (4) | Mo4—O7 | 2.048 (4) |
La2—O3 | 2.457 (5) | Mo4—O15v | 2.060 (3) |
La2—O1 | 2.471 (5) | Mo4—O9v | 2.069 (4) |
La2—O12 | 2.494 (5) | Mo4—Mo5v | 2.5548 (6) |
La2—O17 | 2.579 (3) | Mo4—La1v | 3.2842 (4) |
La2—O7iii | 2.608 (5) | Mo4—La4i | 3.4368 (5) |
La2—O10iii | 2.653 (5) | Mo5—O17 | 1.985 (3) |
La2—O5iv | 2.840 (3) | Mo5—O5 | 1.986 (4) |
La2—Mo3iii | 3.7221 (6) | Mo5—O10i | 2.019 (5) |
La2—La3 | 3.9461 (4) | Mo5—O8iii | 2.055 (5) |
La2—La1v | 3.9844 (4) | Mo5—O15 | 2.086 (3) |
La3—O12 | 2.443 (5) | Mo5—O14 | 2.110 (4) |
La3—O16 | 2.462 (4) | Mo5—Mo4i | 2.5548 (6) |
La3—O6ii | 2.489 (4) | Mo5—Mo3i | 2.5672 (4) |
La3—O4ii | 2.537 (5) | Mo6—O6 | 1.785 (4) |
La3—O1 | 2.627 (5) | Mo6—O9 | 1.901 (4) |
La3—O20 | 2.643 (4) | Mo6—O8i | 1.961 (4) |
La3—O2 | 2.658 (5) | Mo6—O13xiv | 1.962 (4) |
La3—O21v | 2.728 (5) | Mo6—O21ii | 2.049 (4) |
La3—O18ii | 2.954 (6) | Mo6—O19 | 2.073 (4) |
La3—Mo2 | 3.3665 (5) | Mo6—La3xii | 3.5331 (4) |
La3—Mo2v | 3.4091 (5) | Mo6—La4xiv | 3.5366 (5) |
La3—Mo1ii | 3.5215 (4) | Mo6—La5xv | 3.5465 (5) |
La4—O7v | 2.536 (5) | Mo6—La4i | 3.6430 (5) |
La4—O10 | 2.598 (4) | O2—La5ix | 2.682 (5) |
La4—O15vi | 2.617 (3) | O3—La1v | 2.437 (5) |
La4—O13 | 2.622 (5) | O3—La4i | 2.638 (5) |
La4—O11 | 2.636 (5) | O4—La3xii | 2.537 (5) |
La4—O3v | 2.638 (5) | O4—La1xii | 2.597 (4) |
La4—O19vii | 2.648 (5) | O5—Mo3i | 1.963 (4) |
La4—O8 | 2.749 (5) | O5—La2xvi | 2.840 (3) |
La4—O9v | 2.755 (4) | O5—La5xvi | 2.850 (3) |
La4—O9vii | 3.007 (4) | O6—La3xii | 2.489 (4) |
La4—Mo4 | 3.3996 (5) | O6—La5xv | 2.556 (4) |
La4—Mo4v | 3.4368 (5) | O7—La4i | 2.536 (5) |
La5—O2 | 2.387 (4) | O7—La2vi | 2.608 (5) |
La5—O16 | 2.442 (5) | O8—Mo6v | 1.961 (4) |
La5—O6viii | 2.556 (4) | O8—Mo5vi | 2.055 (5) |
La5—O16ix | 2.627 (5) | O8—La5xvii | 2.638 (5) |
La5—O8x | 2.638 (5) | O9—Mo4i | 2.069 (4) |
La5—O2xi | 2.682 (5) | O9—La4i | 2.755 (4) |
La5—O13x | 2.702 (5) | O9—La4xiv | 3.007 (4) |
La5—O5iv | 2.850 (3) | O10—Mo5v | 2.019 (5) |
La5—Mo6viii | 3.5465 (5) | O10—La2vi | 2.653 (5) |
La5—Mo2xi | 3.5724 (5) | O11—La2v | 2.438 (4) |
La5—La5xi | 4.1087 (4) | O11—La1v | 2.513 (5) |
Mo1—O4 | 1.797 (4) | O12—Mo2v | 1.994 (4) |
Mo1—O20 | 1.915 (4) | O12—La1v | 2.481 (4) |
Mo1—O19ii | 1.947 (4) | O13—Mo6vii | 1.962 (4) |
Mo1—O21 | 2.002 (4) | O13—Mo3xviii | 1.987 (5) |
Mo1—O18ii | 2.033 (4) | O13—La5xvii | 2.702 (5) |
Mo1—O18 | 2.090 (4) | O14—Mo2xvi | 1.882 (3) |
Mo1—La1ii | 3.4795 (5) | O15—Mo4i | 2.060 (3) |
Mo1—La1xii | 3.5126 (5) | O15—Mo3i | 2.087 (4) |
Mo1—La3xii | 3.5215 (4) | O15—La4iii | 2.617 (3) |
Mo1—La3i | 3.6767 (6) | O16—Mo2v | 1.980 (5) |
Mo2—O1 | 1.877 (5) | O16—La5xi | 2.627 (5) |
Mo2—O14iv | 1.882 (3) | O18—Mo1xii | 2.033 (4) |
Mo2—O2 | 1.889 (5) | O18—La3xii | 2.954 (6) |
Mo2—O16i | 1.980 (5) | O19—Mo1xii | 1.947 (4) |
Mo2—O12i | 1.994 (4) | O19—La4xiv | 2.648 (5) |
Mo2—O20 | 2.236 (4) | O21—Mo6xii | 2.049 (4) |
Mo2—La3i | 3.4091 (5) | O21—La1xii | 2.716 (5) |
Mo2—La5ix | 3.5724 (5) | O21—La3i | 2.728 (5) |
Mo3—O5v | 1.963 (4) | ||
O3i—La1—O12i | 72.51 (16) | O4—Mo1—La3 | 137.99 (13) |
O3i—La1—O18 | 115.56 (14) | O20—Mo1—La3 | 43.92 (11) |
O12i—La1—O18 | 85.44 (17) | O19ii—Mo1—La3 | 69.98 (13) |
O3i—La1—O11i | 69.79 (10) | O21—Mo1—La3 | 127.31 (14) |
O12i—La1—O11i | 108.41 (16) | O18ii—Mo1—La3 | 53.62 (16) |
O18—La1—O11i | 166.14 (18) | O18—Mo1—La3 | 109.77 (13) |
O3i—La1—O1 | 104.35 (17) | La1ii—Mo1—La3 | 74.309 (11) |
O12i—La1—O1 | 63.40 (11) | La1xii—Mo1—La3 | 175.975 (15) |
O18—La1—O1 | 118.19 (17) | La3xii—Mo1—La3 | 111.893 (14) |
O11i—La1—O1 | 70.37 (17) | La1—Mo1—La3 | 67.177 (9) |
O3i—La1—O4ii | 133.83 (15) | O4—Mo1—La3i | 117.93 (13) |
O12i—La1—O4ii | 122.17 (13) | O20—Mo1—La3i | 58.41 (11) |
O18—La1—O4ii | 109.42 (15) | O19ii—Mo1—La3i | 128.36 (13) |
O11i—La1—O4ii | 64.04 (14) | O21—Mo1—La3i | 46.77 (15) |
O1—La1—O4ii | 60.40 (13) | O18ii—Mo1—La3i | 132.62 (14) |
O3i—La1—O21ii | 117.10 (15) | O18—Mo1—La3i | 56.33 (15) |
O12i—La1—O21ii | 164.21 (16) | La1ii—Mo1—La3i | 176.500 (14) |
O18—La1—O21ii | 79.07 (17) | La1xii—Mo1—La3i | 73.775 (11) |
O11i—La1—O21ii | 87.12 (15) | La3xii—Mo1—La3i | 111.605 (14) |
O1—La1—O21ii | 121.86 (13) | La1—Mo1—La3i | 66.710 (9) |
O4ii—La1—O21ii | 61.52 (12) | La3—Mo1—La3i | 102.254 (11) |
O3i—La1—O19 | 70.52 (15) | O1—Mo2—O14iv | 95.2 (2) |
O12i—La1—O19 | 110.14 (12) | O1—Mo2—O2 | 94.2 (2) |
O18—La1—O19 | 61.90 (14) | O14iv—Mo2—O2 | 99.75 (19) |
O11i—La1—O19 | 111.04 (14) | O1—Mo2—O16i | 159.7 (2) |
O1—La1—O19 | 173.13 (13) | O14iv—Mo2—O16i | 104.38 (19) |
O4ii—La1—O19 | 126.43 (13) | O2—Mo2—O16i | 87.75 (16) |
O21ii—La1—O19 | 65.00 (12) | O1—Mo2—O12i | 86.03 (14) |
O3i—La1—O20 | 134.54 (14) | O14iv—Mo2—O12i | 97.46 (18) |
O12i—La1—O20 | 62.11 (14) | O2—Mo2—O12i | 162.7 (2) |
O18—La1—O20 | 60.37 (13) | O16i—Mo2—O12i | 86.21 (18) |
O11i—La1—O20 | 126.10 (13) | O1—Mo2—O20 | 80.1 (2) |
O1—La1—O20 | 57.94 (15) | O14iv—Mo2—O20 | 175.33 (16) |
O4ii—La1—O20 | 77.42 (13) | O2—Mo2—O20 | 80.12 (19) |
O21ii—La1—O20 | 106.72 (12) | O16i—Mo2—O20 | 80.29 (18) |
O19—La1—O20 | 122.15 (12) | O12i—Mo2—O20 | 82.88 (18) |
O3i—La1—O9 | 58.28 (14) | O1—Mo2—La3 | 50.99 (16) |
O12i—La1—O9 | 130.77 (14) | O14iv—Mo2—La3 | 124.74 (12) |
O18—La1—O9 | 115.42 (14) | O2—Mo2—La3 | 51.95 (14) |
O11i—La1—O9 | 55.18 (14) | O16i—Mo2—La3 | 118.06 (14) |
O1—La1—O9 | 125.54 (14) | O12i—Mo2—La3 | 117.96 (13) |
O4ii—La1—O9 | 93.63 (13) | O20—Mo2—La3 | 51.63 (9) |
O21ii—La1—O9 | 60.49 (12) | O1—Mo2—La1 | 47.50 (15) |
O19—La1—O9 | 56.17 (12) | O14iv—Mo2—La1 | 119.32 (10) |
O20—La1—O9 | 167.08 (11) | O2—Mo2—La1 | 124.15 (14) |
O3i—La1—Mo4i | 36.36 (10) | O16i—Mo2—La1 | 115.81 (14) |
O12i—La1—Mo4i | 98.85 (12) | O12i—Mo2—La1 | 46.14 (12) |
O18—La1—Mo4i | 143.99 (10) | O20—Mo2—La1 | 57.77 (12) |
O11i—La1—Mo4i | 35.73 (9) | La3—Mo2—La1 | 72.671 (10) |
O1—La1—Mo4i | 95.07 (13) | O1—Mo2—La3i | 119.23 (16) |
O4ii—La1—Mo4i | 98.46 (11) | O14iv—Mo2—La3i | 119.92 (12) |
O21ii—La1—Mo4i | 95.51 (10) | O2—Mo2—La3i | 122.44 (16) |
O19—La1—Mo4i | 83.40 (10) | O16i—Mo2—La3i | 45.39 (13) |
O20—La1—Mo4i | 151.34 (8) | O12i—Mo2—La3i | 44.92 (14) |
O9—La1—Mo4i | 38.36 (7) | O20—Mo2—La3i | 63.46 (9) |
O3i—La1—Mo2 | 100.39 (12) | La3—Mo2—La3i | 115.031 (12) |
O12i—La1—Mo2 | 35.41 (9) | La1—Mo2—La3i | 71.778 (10) |
O18—La1—Mo2 | 92.63 (12) | O1—Mo2—La5ix | 124.33 (17) |
O11i—La1—Mo2 | 99.02 (12) | O14iv—Mo2—La5ix | 125.13 (10) |
O1—La1—Mo2 | 32.93 (10) | O2—Mo2—La5ix | 47.38 (16) |
O4ii—La1—Mo2 | 87.12 (9) | O16i—Mo2—La5ix | 46.24 (14) |
O21ii—La1—Mo2 | 141.61 (8) | O12i—Mo2—La5ix | 119.35 (14) |
O19—La1—Mo2 | 142.00 (8) | O20—Mo2—La5ix | 58.07 (12) |
O20—La1—Mo2 | 40.54 (8) | La3—Mo2—La5ix | 73.734 (10) |
O9—La1—Mo2 | 149.67 (7) | La1—Mo2—La5ix | 115.503 (12) |
Mo4i—La1—Mo2 | 111.529 (11) | La3i—Mo2—La5ix | 75.248 (11) |
O11i—La2—O3 | 72.21 (11) | O5v—Mo3—O13xiii | 88.72 (17) |
O11i—La2—O1 | 72.86 (17) | O5v—Mo3—O17 | 166.33 (15) |
O3—La2—O1 | 117.21 (17) | O13xiii—Mo3—O17 | 86.52 (16) |
O11i—La2—O12 | 113.69 (16) | O5v—Mo3—O7 | 90.62 (16) |
O3—La2—O12 | 71.95 (16) | O13xiii—Mo3—O7 | 174.70 (18) |
O1—La2—O12 | 76.86 (12) | O17—Mo3—O7 | 92.95 (15) |
O11i—La2—O17 | 68.36 (14) | O5v—Mo3—O15v | 101.10 (15) |
O3—La2—O17 | 70.96 (14) | O13xiii—Mo3—O15v | 82.57 (17) |
O1—La2—O17 | 135.13 (14) | O17—Mo3—O15v | 90.98 (14) |
O12—La2—O17 | 139.77 (13) | O7—Mo3—O15v | 102.72 (15) |
O11i—La2—O7iii | 153.43 (16) | O5v—Mo3—O14 | 87.65 (15) |
O3—La2—O7iii | 108.15 (13) | O13xiii—Mo3—O14 | 86.52 (17) |
O1—La2—O7iii | 125.50 (17) | O17—Mo3—O14 | 79.29 (14) |
O12—La2—O7iii | 90.74 (15) | O7—Mo3—O14 | 88.20 (15) |
O17—La2—O7iii | 86.39 (13) | O15v—Mo3—O14 | 165.81 (13) |
O11i—La2—O10iii | 105.81 (14) | O5v—Mo3—Mo4 | 95.28 (11) |
O3—La2—O10iii | 156.46 (16) | O13xiii—Mo3—Mo4 | 133.80 (14) |
O1—La2—O10iii | 83.22 (16) | O17—Mo3—Mo4 | 97.26 (10) |
O12—La2—O10iii | 127.28 (15) | O7—Mo3—Mo4 | 51.50 (12) |
O17—La2—O10iii | 86.36 (14) | O15v—Mo3—Mo4 | 51.45 (8) |
O7iii—La2—O10iii | 62.83 (9) | O14—Mo3—Mo4 | 139.54 (9) |
O11i—La2—O5iv | 135.89 (14) | O5v—Mo3—Mo5v | 49.83 (11) |
O3—La2—O5iv | 136.17 (14) | O13xiii—Mo3—Mo5v | 90.34 (12) |
O1—La2—O5iv | 64.01 (15) | O17—Mo3—Mo5v | 142.90 (10) |
O12—La2—O5iv | 65.78 (13) | O7—Mo3—Mo5v | 93.25 (11) |
O17—La2—O5iv | 142.46 (10) | O15v—Mo3—Mo5v | 52.00 (10) |
O7iii—La2—O5iv | 62.55 (13) | O14—Mo3—Mo5v | 137.44 (11) |
O10iii—La2—O5iv | 61.59 (13) | Mo4—Mo3—Mo5v | 59.805 (19) |
O11i—La2—Mo3iii | 163.01 (10) | O5v—Mo3—Mo5 | 129.36 (11) |
O3—La2—Mo3iii | 124.67 (10) | O13xiii—Mo3—Mo5 | 88.04 (11) |
O1—La2—Mo3iii | 95.19 (13) | O17—Mo3—Mo5 | 37.72 (9) |
O12—La2—Mo3iii | 73.87 (11) | O7—Mo3—Mo5 | 88.31 (11) |
O17—La2—Mo3iii | 116.54 (7) | O15v—Mo3—Mo5 | 128.43 (10) |
O7iii—La2—Mo3iii | 31.49 (11) | O14—Mo3—Mo5 | 41.71 (10) |
O10iii—La2—Mo3iii | 59.87 (10) | Mo4—Mo3—Mo5 | 121.93 (2) |
O5iv—La2—Mo3iii | 31.30 (7) | Mo5v—Mo3—Mo5 | 178.22 (4) |
O11i—La2—La3 | 91.67 (12) | O5v—Mo3—La2vi | 48.73 (9) |
O3—La2—La3 | 90.82 (12) | O13xiii—Mo3—La2vi | 136.14 (15) |
O1—La2—La3 | 40.74 (11) | O17—Mo3—La2vi | 131.91 (9) |
O12—La2—La3 | 36.50 (10) | O7—Mo3—La2vi | 42.29 (13) |
O17—La2—La3 | 156.02 (7) | O15v—Mo3—La2vi | 111.94 (9) |
O7iii—La2—La3 | 114.77 (11) | O14—Mo3—La2vi | 82.23 (9) |
O10iii—La2—La3 | 112.72 (11) | Mo4—Mo3—La2vi | 70.255 (14) |
O5iv—La2—La3 | 61.44 (6) | Mo5v—Mo3—La2vi | 71.09 (2) |
Mo3iii—La2—La3 | 86.465 (10) | Mo5—Mo3—La2vi | 109.65 (2) |
O11i—La2—La1v | 91.84 (11) | O11—Mo4—O3 | 93.69 (14) |
O3—La2—La1v | 35.32 (12) | O11—Mo4—O10 | 90.19 (18) |
O1—La2—La1v | 97.39 (12) | O3—Mo4—O10 | 165.5 (2) |
O12—La2—La1v | 36.68 (10) | O11—Mo4—O7 | 166.2 (2) |
O17—La2—La1v | 105.41 (8) | O3—Mo4—O7 | 88.11 (18) |
O7iii—La2—La1v | 103.14 (9) | O10—Mo4—O7 | 84.90 (12) |
O10iii—La2—La1v | 161.59 (10) | O11—Mo4—O15v | 90.80 (19) |
O5iv—La2—La1v | 102.03 (8) | O3—Mo4—O15v | 90.83 (18) |
Mo3iii—La2—La1v | 101.847 (10) | O10—Mo4—O15v | 103.04 (17) |
La3—La2—La1v | 60.481 (7) | O7—Mo4—O15v | 102.88 (18) |
O11i—La2—La1 | 36.17 (12) | O11—Mo4—O9v | 79.2 (2) |
O3—La2—La1 | 91.47 (10) | O3—Mo4—O9v | 82.16 (19) |
O1—La2—La1 | 37.21 (13) | O10—Mo4—O9v | 84.91 (18) |
O12—La2—La1 | 92.53 (10) | O7—Mo4—O9v | 87.50 (18) |
O17—La2—La1 | 103.41 (7) | O15v—Mo4—O9v | 167.33 (15) |
O7iii—La2—La1 | 160.14 (10) | O11—Mo4—Mo5v | 93.80 (14) |
O10iii—La2—La1 | 100.11 (9) | O3—Mo4—Mo5v | 142.53 (15) |
O5iv—La2—La1 | 101.21 (7) | O10—Mo4—Mo5v | 50.76 (14) |
Mo3iii—La2—La1 | 132.251 (10) | O7—Mo4—Mo5v | 93.07 (13) |
La3—La2—La1 | 60.398 (7) | O15v—Mo4—Mo5v | 52.41 (9) |
La1v—La2—La1 | 91.002 (7) | O9v—Mo4—Mo5v | 135.31 (12) |
O12—La3—O16 | 67.22 (16) | O11—Mo4—Mo3 | 142.62 (16) |
O12—La3—O6ii | 137.87 (14) | O3—Mo4—Mo3 | 93.25 (14) |
O16—La3—O6ii | 70.72 (15) | O10—Mo4—Mo3 | 92.08 (13) |
O12—La3—O4ii | 67.38 (15) | O7—Mo4—Mo3 | 50.71 (14) |
O16—La3—O4ii | 134.57 (15) | O15v—Mo4—Mo3 | 52.41 (10) |
O6ii—La3—O4ii | 154.41 (14) | O9v—Mo4—Mo3 | 138.16 (12) |
O12—La3—O1 | 74.88 (11) | Mo5v—Mo4—Mo3 | 60.289 (13) |
O16—La3—O1 | 108.77 (17) | O11—Mo4—La1v | 49.71 (14) |
O6ii—La3—O1 | 122.29 (14) | O3—Mo4—La1v | 47.54 (14) |
O4ii—La3—O1 | 60.11 (15) | O10—Mo4—La1v | 129.59 (13) |
O12—La3—O20 | 134.94 (15) | O7—Mo4—La1v | 126.04 (13) |
O16—La3—O20 | 132.32 (14) | O15v—Mo4—La1v | 106.08 (9) |
O6ii—La3—O20 | 77.80 (14) | O9v—Mo4—La1v | 61.48 (12) |
O4ii—La3—O20 | 83.58 (14) | Mo5v—Mo4—La1v | 140.396 (18) |
O1—La3—O20 | 60.67 (14) | Mo3—Mo4—La1v | 138.157 (19) |
O12—La3—O2 | 106.55 (15) | O11—Mo4—La4 | 50.57 (15) |
O16—La3—O2 | 73.30 (12) | O3—Mo4—La4 | 124.70 (14) |
O6ii—La3—O2 | 62.20 (15) | O10—Mo4—La4 | 49.67 (13) |
O4ii—La3—O2 | 122.19 (14) | O7—Mo4—La4 | 117.89 (13) |
O1—La3—O2 | 62.93 (16) | O15v—Mo4—La4 | 124.27 (12) |
O20—La3—O2 | 60.45 (13) | O9v—Mo4—La4 | 54.10 (12) |
O12—La3—O21v | 114.35 (13) | Mo5v—Mo4—La4 | 87.391 (16) |
O16—La3—O21v | 86.95 (15) | Mo3—Mo4—La4 | 141.577 (18) |
O6ii—La3—O21v | 60.31 (12) | La1v—Mo4—La4 | 79.925 (11) |
O4ii—La3—O21v | 110.22 (13) | O11—Mo4—La4i | 126.11 (14) |
O1—La3—O21v | 164.18 (15) | O3—Mo4—La4i | 49.80 (14) |
O20—La3—O21v | 107.58 (13) | O10—Mo4—La4i | 117.46 (14) |
O2—La3—O21v | 122.50 (14) | O7—Mo4—La4i | 47.15 (13) |
O12—La3—O18ii | 120.31 (14) | O15v—Mo4—La4i | 122.15 (11) |
O16—La3—O18ii | 158.24 (15) | O9v—Mo4—La4i | 60.28 (12) |
O6ii—La3—O18ii | 98.35 (13) | Mo5v—Mo4—La4i | 139.885 (18) |
O4ii—La3—O18ii | 56.65 (14) | Mo3—Mo4—La4i | 85.107 (16) |
O1—La3—O18ii | 92.98 (15) | La1v—Mo4—La4i | 78.894 (11) |
O20—La3—O18ii | 59.10 (12) | La4—Mo4—La4i | 113.448 (11) |
O2—La3—O18ii | 119.12 (12) | O17—Mo5—O5 | 169.73 (15) |
O21v—La3—O18ii | 71.33 (13) | O17—Mo5—O10i | 92.02 (15) |
O12—La3—Mo2 | 101.99 (10) | O5—Mo5—O10i | 89.42 (16) |
O16—La3—Mo2 | 101.98 (11) | O17—Mo5—O8iii | 90.48 (15) |
O6ii—La3—Mo2 | 88.66 (9) | O5—Mo5—O8iii | 86.65 (16) |
O4ii—La3—Mo2 | 88.92 (9) | O10i—Mo5—O8iii | 171.18 (19) |
O1—La3—Mo2 | 33.72 (11) | O17—Mo5—O15 | 89.23 (15) |
O20—La3—Mo2 | 41.55 (9) | O5—Mo5—O15 | 100.42 (15) |
O2—La3—Mo2 | 34.04 (10) | O10i—Mo5—O15 | 102.05 (16) |
O21v—La3—Mo2 | 143.10 (8) | O8iii—Mo5—O15 | 86.44 (16) |
O18ii—La3—Mo2 | 96.34 (8) | O17—Mo5—O14 | 79.77 (14) |
O12—La3—Mo2v | 35.19 (10) | O5—Mo5—O14 | 90.16 (14) |
O16—La3—Mo2v | 34.92 (11) | O10i—Mo5—O14 | 86.73 (15) |
O6ii—La3—Mo2v | 103.48 (9) | O8iii—Mo5—O14 | 85.39 (16) |
O4ii—La3—Mo2v | 100.61 (10) | O15—Mo5—O14 | 166.22 (13) |
O1—La3—Mo2v | 101.15 (10) | O17—Mo5—Mo4i | 93.96 (10) |
O20—La3—Mo2v | 156.48 (9) | O5—Mo5—Mo4i | 94.81 (10) |
O2—La3—Mo2v | 98.90 (10) | O10i—Mo5—Mo4i | 50.66 (13) |
O21v—La3—Mo2v | 92.80 (9) | O8iii—Mo5—Mo4i | 137.56 (13) |
O18ii—La3—Mo2v | 141.73 (8) | O15—Mo5—Mo4i | 51.51 (8) |
Mo2—La3—Mo2v | 115.031 (12) | O14—Mo5—Mo4i | 136.92 (9) |
O12—La3—Mo1ii | 84.13 (11) | O17—Mo5—Mo3i | 140.97 (11) |
O16—La3—Mo1ii | 141.35 (11) | O5—Mo5—Mo3i | 49.08 (11) |
O6ii—La3—Mo1ii | 130.87 (10) | O10i—Mo5—Mo3i | 91.72 (11) |
O4ii—La3—Mo1ii | 29.12 (10) | O8iii—Mo5—Mo3i | 91.66 (11) |
O1—La3—Mo1ii | 86.71 (12) | O15—Mo5—Mo3i | 52.06 (11) |
O20—La3—Mo1ii | 86.27 (9) | O14—Mo5—Mo3i | 139.24 (10) |
O2—La3—Mo1ii | 142.50 (10) | Mo4i—Mo5—Mo3i | 59.91 (2) |
O21v—La3—Mo1ii | 81.73 (9) | O17—Mo5—Mo3 | 38.35 (10) |
O18ii—La3—Mo1ii | 36.34 (8) | O5—Mo5—Mo3 | 131.70 (11) |
Mo2—La3—Mo1ii | 109.187 (13) | O10i—Mo5—Mo3 | 86.72 (11) |
Mo2v—La3—Mo1ii | 108.714 (13) | O8iii—Mo5—Mo3 | 90.01 (11) |
O7v—La4—O10 | 70.78 (10) | O15—Mo5—Mo3 | 127.46 (11) |
O7v—La4—O15vi | 77.19 (13) | O14—Mo5—Mo3 | 41.57 (9) |
O10—La4—O15vi | 76.09 (14) | Mo4i—Mo5—Mo3 | 118.36 (2) |
O7v—La4—O13 | 99.73 (15) | Mo3i—Mo5—Mo3 | 178.22 (4) |
O10—La4—O13 | 137.82 (16) | O6—Mo6—O9 | 172.99 (18) |
O15vi—La4—O13 | 61.77 (13) | O6—Mo6—O8i | 99.9 (2) |
O7v—La4—O11 | 101.40 (15) | O9—Mo6—O8i | 86.9 (2) |
O10—La4—O11 | 64.43 (15) | O6—Mo6—O13xiv | 88.8 (2) |
O15vi—La4—O11 | 138.05 (13) | O9—Mo6—O13xiv | 91.3 (2) |
O13—La4—O11 | 154.14 (15) | O8i—Mo6—O13xiv | 103.70 (14) |
O7v—La4—O3v | 65.14 (15) | O6—Mo6—O21ii | 86.31 (19) |
O10—La4—O3v | 102.54 (15) | O9—Mo6—O21ii | 92.25 (19) |
O15vi—La4—O3v | 139.92 (13) | O8i—Mo6—O21ii | 87.78 (19) |
O13—La4—O3v | 110.38 (14) | O13xiv—Mo6—O21ii | 168.15 (19) |
O11—La4—O3v | 66.31 (10) | O6—Mo6—O19 | 88.89 (19) |
O7v—La4—O19vii | 115.37 (13) | O9—Mo6—O19 | 84.26 (18) |
O10—La4—O19vii | 163.44 (14) | O8i—Mo6—O19 | 170.9 (2) |
O15vi—La4—O19vii | 119.77 (12) | O13xiv—Mo6—O19 | 78.67 (19) |
O13—La4—O19vii | 58.10 (14) | O21ii—Mo6—O19 | 90.43 (17) |
O11—La4—O19vii | 99.01 (14) | O6—Mo6—La1 | 116.09 (14) |
O3v—La4—O19vii | 68.94 (15) | O9—Mo6—La1 | 58.19 (13) |
O7v—La4—O8 | 140.72 (16) | O8i—Mo6—La1 | 120.47 (15) |
O10—La4—O8 | 102.07 (14) | O13xiv—Mo6—La1 | 121.72 (15) |
O15vi—La4—O8 | 63.75 (13) | O21ii—Mo6—La1 | 52.01 (13) |
O13—La4—O8 | 58.90 (10) | O19—Mo6—La1 | 52.38 (12) |
O11—La4—O8 | 110.10 (13) | O6—Mo6—La3xii | 41.31 (14) |
O3v—La4—O8 | 149.86 (15) | O9—Mo6—La3xii | 134.09 (13) |
O19vii—La4—O8 | 82.74 (14) | O8i—Mo6—La3xii | 112.89 (15) |
O7v—La4—O9v | 132.63 (13) | O13xiv—Mo6—La3xii | 120.63 (15) |
O10—La4—O9v | 61.92 (13) | O21ii—Mo6—La3xii | 50.36 (14) |
O15vi—La4—O9v | 93.40 (12) | O19—Mo6—La3xii | 72.33 (13) |
O13—La4—O9v | 116.50 (12) | La1—Mo6—La3xii | 76.432 (9) |
O11—La4—O9v | 56.34 (11) | O6—Mo6—La4xiv | 117.64 (12) |
O3v—La4—O9v | 121.82 (12) | O9—Mo6—La4xiv | 58.23 (13) |
O19vii—La4—O9v | 109.57 (13) | O8i—Mo6—La4xiv | 127.61 (15) |
O8—La4—O9v | 57.73 (11) | O13xiv—Mo6—La4xiv | 46.91 (15) |
O7v—La4—O9vii | 61.10 (12) | O21ii—Mo6—La4xiv | 127.30 (13) |
O10—La4—O9vii | 131.81 (12) | O19—Mo6—La4xiv | 48.09 (13) |
O15vi—La4—O9vii | 95.04 (12) | La1—Mo6—La4xiv | 75.439 (10) |
O13—La4—O9vii | 58.31 (11) | La3xii—Mo6—La4xiv | 119.465 (13) |
O11—La4—O9vii | 121.40 (11) | O6—Mo6—La5xv | 43.19 (12) |
O3v—La4—O9vii | 55.48 (11) | O9—Mo6—La5xv | 134.07 (13) |
O19vii—La4—O9vii | 55.89 (12) | O8i—Mo6—La5xv | 120.32 (15) |
O8—La4—O9vii | 116.28 (11) | O13xiv—Mo6—La5xv | 49.02 (15) |
O9v—La4—O9vii | 165.46 (17) | O21ii—Mo6—La5xv | 122.42 (14) |
O7v—La4—Mo4 | 99.30 (10) | O19—Mo6—La5xv | 67.94 (12) |
O10—La4—Mo4 | 36.26 (10) | La1—Mo6—La5xv | 118.358 (13) |
O15vi—La4—Mo4 | 103.88 (9) | La3xii—Mo6—La5xv | 72.101 (10) |
O13—La4—Mo4 | 152.57 (9) | La4xiv—Mo6—La5xv | 76.200 (11) |
O11—La4—Mo4 | 34.31 (9) | O6—Mo6—La4i | 136.84 (12) |
O3v—La4—Mo4 | 95.50 (9) | O9—Mo6—La4i | 47.84 (13) |
O19vii—La4—Mo4 | 128.33 (9) | O8i—Mo6—La4i | 47.99 (15) |
O8—La4—Mo4 | 94.10 (9) | O13xiv—Mo6—La4i | 122.54 (15) |
O9v—La4—Mo4 | 37.46 (8) | O21ii—Mo6—La4i | 67.47 (13) |
O9vii—La4—Mo4 | 149.11 (7) | O19—Mo6—La4i | 123.30 (12) |
O7v—La4—Mo4v | 36.30 (10) | La1—Mo6—La4i | 74.513 (10) |
O10—La4—Mo4v | 99.38 (10) | La3xii—Mo6—La4i | 116.720 (13) |
O15vi—La4—Mo4v | 105.46 (8) | La4xiv—Mo6—La4i | 105.504 (11) |
O13—La4—Mo4v | 93.48 (9) | La5xv—Mo6—La4i | 166.648 (13) |
O11—La4—Mo4v | 94.76 (9) | Mo2—O1—La2 | 144.9 (3) |
O3v—La4—Mo4v | 34.54 (10) | Mo2—O1—La1 | 99.56 (18) |
O19vii—La4—Mo4v | 81.62 (9) | La2—O1—La1 | 106.8 (2) |
O8—La4—Mo4v | 152.38 (9) | Mo2—O1—La3 | 95.3 (2) |
O9v—La4—Mo4v | 149.69 (7) | La2—O1—La3 | 101.40 (13) |
O9vii—La4—Mo4v | 36.69 (7) | La1—O1—La3 | 101.7 (2) |
Mo4—La4—Mo4v | 113.448 (11) | Mo2—O2—La5 | 142.1 (3) |
O2—La5—O16 | 78.64 (13) | Mo2—O2—La3 | 94.01 (19) |
O2—La5—O6viii | 151.94 (14) | La5—O2—La3 | 101.88 (14) |
O16—La5—O6viii | 73.32 (14) | Mo2—O2—La5ix | 101.40 (18) |
O2—La5—O16ix | 72.17 (14) | La5—O2—La5ix | 108.18 (19) |
O16—La5—O16ix | 108.86 (10) | La3—O2—La5ix | 102.58 (18) |
O6viii—La5—O16ix | 116.02 (14) | Mo4—O3—La1v | 96.10 (15) |
O2—La5—O8x | 84.25 (15) | Mo4—O3—La2 | 130.7 (2) |
O16—La5—O8x | 131.21 (17) | La1v—O3—La2 | 109.0 (2) |
O6viii—La5—O8x | 115.23 (14) | Mo4—O3—La4i | 95.7 (2) |
O16ix—La5—O8x | 108.61 (14) | La1v—O3—La4i | 114.61 (19) |
O2—La5—O2xi | 108.38 (11) | La2—O3—La4i | 110.14 (13) |
O16—La5—O2xi | 70.39 (14) | Mo1—O4—La3xii | 107.5 (2) |
O6viii—La5—O2xi | 61.05 (14) | Mo1—O4—La1xii | 104.69 (17) |
O16ix—La5—O2xi | 60.69 (11) | La3xii—O4—La1xii | 102.80 (15) |
O8x—La5—O2xi | 157.76 (14) | Mo3i—O5—Mo5 | 81.09 (12) |
O2—La5—O13x | 124.89 (17) | Mo3i—O5—La2xvi | 99.97 (13) |
O16—La5—O13x | 94.96 (16) | Mo5—O5—La2xvi | 101.46 (14) |
O6viii—La5—O13x | 59.82 (13) | Mo3i—O5—La5xvi | 102.76 (13) |
O16ix—La5—O13x | 153.78 (15) | Mo5—O5—La5xvi | 103.39 (13) |
O8x—La5—O13x | 59.31 (11) | La2xvi—O5—La5xvi | 148.48 (12) |
O2xi—La5—O13x | 120.82 (13) | Mo6—O6—La3xii | 110.44 (18) |
O2—La5—O5iv | 66.89 (15) | Mo6—O6—La5xv | 108.26 (18) |
O16—La5—O5iv | 70.71 (14) | La3xii—O6—La5xv | 111.35 (16) |
O6viii—La5—O5iv | 103.93 (13) | Mo3—O7—Mo4 | 77.79 (17) |
O16ix—La5—O5iv | 138.33 (13) | Mo3—O7—La4i | 128.0 (2) |
O8x—La5—O5iv | 60.55 (13) | Mo4—O7—La4i | 96.55 (19) |
O2xi—La5—O5iv | 140.94 (12) | Mo3—O7—La2vi | 106.21 (19) |
O13x—La5—O5iv | 59.59 (12) | Mo4—O7—La2vi | 106.11 (15) |
O2—La5—Mo6viii | 154.95 (13) | La4i—O7—La2vi | 124.6 (2) |
O16—La5—Mo6viii | 89.98 (10) | Mo6v—O8—Mo5vi | 126.5 (2) |
O6viii—La5—Mo6viii | 28.55 (10) | Mo6v—O8—La5xvii | 108.7 (2) |
O16ix—La5—Mo6viii | 132.87 (11) | Mo5vi—O8—La5xvii | 108.8 (2) |
O8x—La5—Mo6viii | 86.78 (10) | Mo6v—O8—La4 | 100.0 (2) |
O2xi—La5—Mo6viii | 88.18 (10) | Mo5vi—O8—La4 | 102.67 (19) |
O13x—La5—Mo6viii | 33.25 (9) | La5xvii—O8—La4 | 108.44 (15) |
O5iv—La5—Mo6viii | 88.35 (8) | Mo6—O9—Mo4i | 165.9 (2) |
O2—La5—Mo2xi | 99.53 (13) | Mo6—O9—La4i | 101.38 (16) |
O16—La5—Mo2xi | 97.31 (12) | Mo4i—O9—La4i | 88.44 (14) |
O6viii—La5—Mo2xi | 83.21 (10) | Mo6—O9—La1 | 88.33 (16) |
O16ix—La5—Mo2xi | 32.98 (10) | Mo4i—O9—La1 | 80.16 (12) |
O8x—La5—Mo2xi | 130.65 (10) | La4i—O9—La1 | 98.09 (13) |
O2xi—La5—Mo2xi | 31.22 (9) | Mo6—O9—La4xiv | 89.25 (14) |
O13x—La5—Mo2xi | 135.44 (10) | Mo4i—O9—La4xiv | 83.03 (13) |
O5iv—La5—Mo2xi | 163.00 (6) | La4i—O9—La4xiv | 165.46 (17) |
Mo6viii—La5—Mo2xi | 104.042 (12) | La1—O9—La4xiv | 92.05 (11) |
O2—La5—La3 | 41.55 (11) | Mo4—O10—Mo5v | 78.58 (18) |
O16—La5—La3 | 37.10 (10) | Mo4—O10—La4 | 94.07 (18) |
O6viii—La5—La3 | 110.42 (9) | Mo5v—O10—La4 | 128.1 (2) |
O16ix—La5—La3 | 92.20 (11) | Mo4—O10—La2vi | 105.52 (15) |
O8x—La5—La3 | 112.18 (11) | Mo5v—O10—La2vi | 107.04 (18) |
O2xi—La5—La3 | 88.56 (10) | La4—O10—La2vi | 124.2 (2) |
O13x—La5—La3 | 113.75 (11) | Mo4—O11—La2v | 133.2 (3) |
O5iv—La5—La3 | 61.77 (6) | Mo4—O11—La1v | 94.56 (14) |
Mo6viii—La5—La3 | 123.605 (12) | La2v—O11—La1v | 108.91 (19) |
Mo2xi—La5—La3 | 101.357 (10) | Mo4—O11—La4 | 95.1 (2) |
O2—La5—La5xi | 98.99 (11) | La2v—O11—La4 | 110.81 (13) |
O16—La5—La5xi | 37.38 (12) | La1v—O11—La4 | 112.96 (19) |
O6viii—La5—La5xi | 57.13 (9) | Mo2v—O12—La3 | 99.9 (2) |
O16ix—La5—La5xi | 85.92 (10) | Mo2v—O12—La1v | 98.46 (14) |
O8x—La5—La5xi | 165.36 (10) | La3—O12—La1v | 108.39 (19) |
O2xi—La5—La5xi | 33.50 (10) | Mo2v—O12—La2 | 135.6 (2) |
O13x—La5—La5xi | 108.16 (9) | La3—O12—La2 | 106.12 (13) |
O5iv—La5—La5xi | 107.45 (7) | La1v—O12—La2 | 106.43 (18) |
Mo6viii—La5—La5xi | 84.394 (7) | Mo6vii—O13—Mo3xviii | 131.3 (2) |
Mo2xi—La5—La5xi | 63.153 (11) | Mo6vii—O13—La4 | 100.0 (2) |
La3—La5—La5xi | 64.103 (9) | Mo3xviii—O13—La4 | 109.0 (2) |
O4—Mo1—O20 | 170.6 (2) | Mo6vii—O13—La5xvii | 97.7 (2) |
O4—Mo1—O19ii | 92.4 (2) | Mo3xviii—O13—La5xvii | 107.3 (2) |
O20—Mo1—O19ii | 96.40 (19) | La4—O13—La5xvii | 110.34 (15) |
O4—Mo1—O21 | 91.26 (19) | Mo2xvi—O14—Mo3 | 134.3 (2) |
O20—Mo1—O21 | 91.16 (19) | Mo2xvi—O14—Mo5 | 129.0 (2) |
O19ii—Mo1—O21 | 96.19 (19) | Mo3—O14—Mo5 | 96.73 (13) |
O4—Mo1—O18ii | 88.2 (2) | Mo4i—O15—Mo5 | 76.08 (10) |
O20—Mo1—O18ii | 89.2 (2) | Mo4i—O15—Mo3i | 76.14 (11) |
O19ii—Mo1—O18ii | 85.05 (19) | Mo5—O15—Mo3i | 75.93 (10) |
O21—Mo1—O18ii | 178.7 (2) | Mo4i—O15—La4iii | 177.10 (15) |
O4—Mo1—O18 | 84.8 (2) | Mo5—O15—La4iii | 106.27 (13) |
O20—Mo1—O18 | 86.2 (2) | Mo3i—O15—La4iii | 105.98 (14) |
O19ii—Mo1—O18 | 175.3 (2) | Mo2v—O16—La5 | 128.1 (2) |
O21—Mo1—O18 | 87.64 (18) | Mo2v—O16—La3 | 99.7 (2) |
O18ii—Mo1—O18 | 91.10 (5) | La5—O16—La3 | 106.17 (15) |
O4—Mo1—La1ii | 65.29 (13) | Mo2v—O16—La5xi | 100.78 (16) |
O20—Mo1—La1ii | 118.18 (11) | La5—O16—La5xi | 108.27 (19) |
O19ii—Mo1—La1ii | 51.41 (13) | La3—O16—La5xi | 113.81 (19) |
O21—Mo1—La1ii | 135.91 (15) | Mo5—O17—Mo3 | 103.94 (14) |
O18ii—Mo1—La1ii | 44.76 (14) | Mo5—O17—La2 | 128.95 (17) |
O18—Mo1—La1ii | 123.90 (15) | Mo3—O17—La2 | 125.01 (17) |
O4—Mo1—La1xii | 45.65 (12) | Mo1xii—O18—Mo1 | 156.5 (3) |
O20—Mo1—La1xii | 132.15 (11) | Mo1xii—O18—La1 | 100.12 (19) |
O19ii—Mo1—La1xii | 112.89 (13) | Mo1—O18—La1 | 102.77 (16) |
O21—Mo1—La1xii | 50.38 (13) | Mo1xii—O18—La3xii | 92.72 (19) |
O18ii—Mo1—La1xii | 128.63 (16) | Mo1—O18—La3xii | 86.79 (17) |
O18—Mo1—La1xii | 67.62 (13) | La1—O18—La3xii | 104.66 (17) |
La1ii—Mo1—La1xii | 109.654 (11) | Mo1xii—O19—Mo6 | 151.2 (3) |
O4—Mo1—La3xii | 43.39 (15) | Mo1xii—O19—La4xiv | 109.50 (17) |
O20—Mo1—La3xii | 128.16 (15) | Mo6—O19—La4xiv | 96.27 (17) |
O19ii—Mo1—La3xii | 118.65 (13) | Mo1xii—O19—La1 | 94.68 (16) |
O21—Mo1—La3xii | 118.88 (13) | Mo6—O19—La1 | 90.62 (14) |
O18ii—Mo1—La3xii | 59.96 (16) | La4xiv—O19—La1 | 105.21 (16) |
O18—Mo1—La3xii | 56.87 (16) | Mo1—O20—Mo2 | 166.7 (2) |
La1ii—Mo1—La3xii | 69.569 (10) | Mo1—O20—La3 | 105.92 (16) |
La1xii—Mo1—La3xii | 69.550 (10) | Mo2—O20—La3 | 86.83 (13) |
O4—Mo1—La1 | 116.75 (16) | Mo1—O20—La1 | 93.73 (16) |
O20—Mo1—La1 | 54.08 (15) | Mo2—O20—La1 | 81.69 (15) |
O19ii—Mo1—La1 | 136.92 (13) | La3—O20—La1 | 92.38 (14) |
O21—Mo1—La1 | 113.01 (14) | Mo1—O21—Mo6xii | 161.3 (3) |
O18ii—Mo1—La1 | 66.23 (14) | Mo1—O21—La1xii | 95.03 (16) |
O18—Mo1—La1 | 42.59 (13) | Mo6xii—O21—La1xii | 91.51 (15) |
La1ii—Mo1—La1 | 110.900 (13) | Mo1—O21—La3i | 100.91 (19) |
La1xii—Mo1—La1 | 110.133 (13) | Mo6xii—O21—La3i | 94.32 (15) |
La3xii—Mo1—La1 | 74.797 (9) | La1xii—O21—La3i | 104.93 (15) |
Symmetry codes: (i) x−1, y, z; (ii) x+1/2, −y+1/2, −z; (iii) −x+2, y−1/2, −z+1/2; (iv) −x+1, y−1/2, −z+1/2; (v) x+1, y, z; (vi) −x+2, y+1/2, −z+1/2; (vii) x+2, y, z; (viii) x+1, y−1, z; (ix) x−1/2, −y−1/2, −z; (x) x−1, y−1, z; (xi) x+1/2, −y−1/2, −z; (xii) x−1/2, −y+1/2, −z; (xiii) −x+3, y−1/2, −z+1/2; (xiv) x−2, y, z; (xv) x−1, y+1, z; (xvi) −x+1, y+1/2, −z+1/2; (xvii) x+1, y+1, z; (xviii) −x+3, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | La5Mo6O21 |
Mr | 1606.19 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 293 |
a, b, c (Å) | 5.71550 (5), 11.2429 (1), 25.2146 (2) |
V (Å3) | 1620.26 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 17.45 |
Crystal size (mm) | 0.45 × 0.04 × 0.03 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Analytical (de Meulenaar & Tompa, 1965) |
Tmin, Tmax | 0.116, 0.690 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 34498, 9991, 9029 |
Rint | 0.081 |
(sin θ/λ)max (Å−1) | 0.909 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.088, 1.07 |
No. of reflections | 9991 |
No. of parameters | 291 |
Δρmax, Δρmin (e Å−3) | 4.10, −4.15 |
Absolute structure | Flack (1983), 4271 Friedel pairs? |
Absolute structure parameter | 0.393 (12) |
Computer programs: COLLECT (Nonius, 1998), COLLECT, EVALCCD (Duisenberg, 1998), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 1997), DIAMOND (Bergerhoff, 1996), SHELXL97.
La1—O3i | 2.437 (5) | La5—O2xi | 2.682 (5) |
La1—O12i | 2.481 (4) | La5—O13x | 2.702 (5) |
La1—O18 | 2.489 (5) | La5—O5iv | 2.850 (3) |
La1—O11i | 2.513 (5) | Mo1—O4 | 1.797 (4) |
La1—O1 | 2.546 (5) | Mo1—O20 | 1.915 (4) |
La1—O4ii | 2.597 (4) | Mo1—O19ii | 1.947 (4) |
La1—O21ii | 2.716 (5) | Mo1—O21 | 2.002 (4) |
La1—O19 | 2.729 (4) | Mo1—O18ii | 2.033 (4) |
La1—O20 | 2.910 (5) | Mo1—O18 | 2.090 (4) |
La1—O9 | 2.929 (4) | Mo2—O1 | 1.877 (5) |
La2—O11i | 2.438 (4) | Mo2—O14iv | 1.882 (3) |
La2—O3 | 2.457 (5) | Mo2—O2 | 1.889 (5) |
La2—O1 | 2.471 (5) | Mo2—O16i | 1.980 (5) |
La2—O12 | 2.494 (5) | Mo2—O12i | 1.994 (4) |
La2—O17 | 2.579 (3) | Mo2—O20 | 2.236 (4) |
La2—O7iii | 2.608 (5) | Mo3—O5v | 1.963 (4) |
La2—O10iii | 2.653 (5) | Mo3—O13xii | 1.987 (5) |
La2—O5iv | 2.840 (3) | Mo3—O17 | 2.013 (4) |
La3—O12 | 2.443 (5) | Mo3—O7 | 2.025 (5) |
La3—O16 | 2.462 (4) | Mo3—O15v | 2.087 (4) |
La3—O6ii | 2.489 (4) | Mo3—O14 | 2.104 (4) |
La3—O4ii | 2.537 (5) | Mo3—Mo4 | 2.5574 (6) |
La3—O1 | 2.627 (5) | Mo3—Mo5v | 2.5672 (4) |
La3—O20 | 2.643 (4) | Mo4—O11 | 1.924 (4) |
La3—O2 | 2.658 (5) | Mo4—O3 | 1.958 (4) |
La3—O21v | 2.728 (5) | Mo4—O10 | 2.016 (5) |
La3—O18ii | 2.954 (6) | Mo4—O7 | 2.048 (4) |
La4—O7v | 2.536 (5) | Mo4—O15v | 2.060 (3) |
La4—O10 | 2.598 (4) | Mo4—O9v | 2.069 (4) |
La4—O15vi | 2.617 (3) | Mo4—Mo5v | 2.5548 (6) |
La4—O13 | 2.622 (5) | Mo5—O17 | 1.985 (3) |
La4—O11 | 2.636 (5) | Mo5—O5 | 1.986 (4) |
La4—O3v | 2.638 (5) | Mo5—O10i | 2.019 (5) |
La4—O19vii | 2.648 (5) | Mo5—O8iii | 2.055 (5) |
La4—O8 | 2.749 (5) | Mo5—O15 | 2.086 (3) |
La4—O9v | 2.755 (4) | Mo5—O14 | 2.110 (4) |
La4—O9vii | 3.007 (4) | Mo6—O6 | 1.785 (4) |
La5—O2 | 2.387 (4) | Mo6—O9 | 1.901 (4) |
La5—O16 | 2.442 (5) | Mo6—O8i | 1.961 (4) |
La5—O6viii | 2.556 (4) | Mo6—O13xiii | 1.962 (4) |
La5—O16ix | 2.627 (5) | Mo6—O21ii | 2.049 (4) |
La5—O8x | 2.638 (5) | Mo6—O19 | 2.073 (4) |
Symmetry codes: (i) x−1, y, z; (ii) x+1/2, −y+1/2, −z; (iii) −x+2, y−1/2, −z+1/2; (iv) −x+1, y−1/2, −z+1/2; (v) x+1, y, z; (vi) −x+2, y+1/2, −z+1/2; (vii) x+2, y, z; (viii) x+1, y−1, z; (ix) x−1/2, −y−1/2, −z; (x) x−1, y−1, z; (xi) x+1/2, −y−1/2, −z; (xii) −x+3, y−1/2, −z+1/2; (xiii) x−2, y, z. |
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The M2Mo3O8 compounds (M = Mg, Zn, Fe, Co, Ni, Zn and Cd) were the first identified reduced molybdenum compounds containing Mo3O13 cluster units made up of three edge-sharing octahedral MoO6 units (McCarroll et al., 1957). In the latter compounds, the Mo atoms form strongly bonded triangular clusters containing six d electrons that fill three bonding orbitals. Six-electron Mo3 clusters are also found in the quaternary compounds LiRMo3O8 (R = Sc, Y, In, Sm, Gd, Tb, Dy, Ho, Er and Yb; McCarroll, 1977). Subsequently Mo3 clusters containing seven d electrons were observed in LiZn2Mo3O8 and ScZnMo3O8, and clusters containing eight electrons were observed in Zn3Mo3O8 (Torardi & McCarley, 1985). In addition, the Mo3O13 cluster unit has also been observed in coexistence with the tetrahedral MoO4 unit in Na2In2Mo5O16 (Collins et al., 1989) and with the octahedral MoO6 unit in La3Mo4SiO16 (Betteridge et al., 1984). In Na2In2Mo5O16, the number of electrons per Mo3 cluster has been evaluated to six, the Mo atom of the MoO4 unit having a valence of +6. The present paper reports the synthesis and crystal structure of a new Mo3O13 cluster compound, La5Mo6O21. The structure of La5Mo6O21 is made up of Mo3O13 units containing triangular Mo3 clusters (Fig. 1) and distorted MoO6 octahedra that are corner or edge-shared in a complex manner, as shown in Fig. 2. The Mo3O13 units share atoms O14 and O17 to form infinite chains parallel to the a axis. The Mo—Mo distances within the Mo3 triangle are 2.5548 (6), 2.5574 (6) and 2.5672 (4) Å, with an average value of 2.560 Å. This value differs from the values of 2.524 (2) and 2.6164 (5) Å found in Zn2Mo3O8 and Na2In2Mo5O16, respectively, which also contain six d electrons per Mo3O13 cluster. Furthermore, the shortest intercluster Mo—Mo distance is here 3.1489 (4) Å, compared with 3.1695 (5) and 3.235 (2) Å in Na2In2Mo5O16 and Zn2Mo3O8, respectively. The Mo—O distances around atoms Mo1, Mo2 and Mo6 range from 1.785 (4) to 2.236 (4) Å, while those around the Mo atoms of the Mo3 cluster are between 1.924 (4) and 2.110 (4) Å. From these Mo—O bonds, we could estimate the oxidation states of each independent Mo atom by using the empirical bond-length–bond-strength relationship developed by Brown & Wu (1976) for Mo—O bonds: s(Mo—O) = [d(Mo—O)/1.882]−6. In this formula, s(Mo—O) is the bond strength in valence unit, d(Mo—O) is the observed Mo—O bond distance in Å, 1.882 Å corresponds to a Mo—O single-bond distance and the exponential parameter −6 is characteristic of the Mo atom. These calculations for atoms Mo1, Mo2 and Mo6 resulted in values of +4.89 (5), +4.80 (5) and +5.03 (5), which are very close to the ideal value of +5. For atoms Mo3, Mo4 and Mo5 forming the Mo3 cluster, the calculated oxidation states are +3.86 (4), 4.08 (5) and 3.74 (5), respectively. Consequently, we could evaluate to six the number of electrons per Mo3 cluster in La5Mo6O21. The La atoms are surrounded by eight, nine or ten O atoms, forming complex polyhedra. The La—O distances range from 2.387 (4) to 3.007 (4) Å.