Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010402147X/ob1198sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827010402147X/ob1198Isup2.hkl |
CCDC reference: 235475
A solution of [NBu4]2[Mo6O19] (0.22 g, 0.16 mmol) and Na2MoO4 (0.10 g, 0.5 mmol) in DMF (7 ml) was added dropwise to a stirred ethanol solution (4 ml) of La(NO3)3·3H2O (0.25 g, 0.7 mmol). The mixture was then stirred at 333 K for 1 h. Colorless crystals of (I) were obtained after the mixture had been filted and the yellow filtrate had been kept in air for several days (yield 53% based on La). Analysis calculated: C 13.58, H 2.66, N 5.28%; found: C 13.61, H 2.52, N 5.33%.
All H atoms were positioned geometrically and refined using a riding model, with C—H distance of 0.93–0.96 Å and with Uiso(H) values of 1.2Ueq(C) or 1.5Ueq(Cmethyl). The peak in the diffence density map is located 1.14 Å from atom O5.
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens,1994); data reduction: XPREP in SHELXTL (Siemens, 1994) and SAINT?; program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[NaLaMo8O26(C3H7N)7] | F(000) = 3568 |
Mr = 1857.09 | Dx = 2.462 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 12241 reflections |
a = 9.418 (1) Å | θ = 1.8–25.0° |
b = 22.4088 (10) Å | µ = 2.87 mm−1 |
c = 23.7508 (13) Å | T = 293 K |
β = 92.098 (3)° | Prism, colorless |
V = 5009.2 (6) Å3 | 0.28 × 0.20 × 0.08 mm |
Z = 4 |
Bruker SMART P4 diffractometer | 8775 independent reflections |
Radiation source: fine-focus sealed tube | 8115 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
ω scans | θmax = 25.0°, θmin = 1.8° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −11→10 |
Tmin = 0.507, Tmax = 0.795 | k = −26→25 |
29069 measured reflections | l = −25→28 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.046P)2 + 34.1827P] where P = (Fo2 + 2Fc2)/3 |
8775 reflections | (Δ/σ)max = 0.011 |
654 parameters | Δρmax = 1.24 e Å−3 |
0 restraints | Δρmin = −0.86 e Å−3 |
[NaLaMo8O26(C3H7N)7] | V = 5009.2 (6) Å3 |
Mr = 1857.09 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 9.418 (1) Å | µ = 2.87 mm−1 |
b = 22.4088 (10) Å | T = 293 K |
c = 23.7508 (13) Å | 0.28 × 0.20 × 0.08 mm |
β = 92.098 (3)° |
Bruker SMART P4 diffractometer | 8775 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 8115 reflections with I > 2σ(I) |
Tmin = 0.507, Tmax = 0.795 | Rint = 0.037 |
29069 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.046P)2 + 34.1827P] where P = (Fo2 + 2Fc2)/3 |
8775 reflections | Δρmax = 1.24 e Å−3 |
654 parameters | Δρmin = −0.86 e Å−3 |
Experimental. IR (solid KBr pellet, v/cm−1): 3434m, 2928w, 1650 s, 1497w, 1434w, 1383m, 1252w, 1109w, 940m, 914 s, 842m, 727m, 674m, 523w, 413w. |
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 | 0.50502 (3) | 0.763587 (14) | 0.051399 (13) | 0.01294 (9) | |
Mo1 | 0.37412 (5) | 0.62786 (2) | 0.28401 (2) | 0.01263 (11) | |
Mo2 | 0.25046 (5) | 0.48938 (2) | 0.15207 (2) | 0.01715 (12) | |
Mo3 | 0.31467 (5) | 0.63049 (2) | 0.15027 (2) | 0.01366 (11) | |
Mo4 | 0.64368 (5) | 0.53271 (2) | 0.33429 (2) | 0.01661 (12) | |
Mo5 | 0.31451 (5) | 0.48623 (2) | 0.28789 (2) | 0.01605 (12) | |
Mo6 | 0.70535 (5) | 0.67458 (2) | 0.33079 (2) | 0.01464 (12) | |
Mo7 | 0.58226 (5) | 0.53361 (2) | 0.19953 (2) | 0.01401 (12) | |
Mo8 | 0.64550 (5) | 0.67367 (2) | 0.196852 (19) | 0.01254 (11) | |
Na1 | 0.9806 (2) | 0.58206 (11) | 0.24341 (10) | 0.0256 (5) | |
O1 | 0.0815 (4) | 0.51013 (19) | 0.16817 (18) | 0.0228 (9) | |
O2 | 0.3407 (5) | 0.4317 (2) | 0.33707 (19) | 0.0269 (10) | |
O3 | 0.2278 (5) | 0.4367 (2) | 0.10102 (19) | 0.0296 (10) | |
O4 | 0.6095 (4) | 0.72743 (18) | 0.14703 (16) | 0.0199 (9) | |
O5 | 0.5520 (4) | 0.48882 (17) | 0.26826 (17) | 0.0178 (8) | |
O6 | 0.1433 (4) | 0.51003 (19) | 0.29560 (17) | 0.0211 (9) | |
O7 | 0.8171 (4) | 0.65287 (19) | 0.18888 (16) | 0.0184 (8) | |
O8 | 0.7576 (4) | 0.52069 (19) | 0.19021 (18) | 0.0224 (9) | |
O9 | 0.6589 (4) | 0.60582 (18) | 0.37452 (16) | 0.0166 (8) | |
O10 | 0.6267 (5) | 0.4832 (2) | 0.3874 (2) | 0.0310 (11) | |
O11 | 0.8140 (4) | 0.52470 (19) | 0.31357 (18) | 0.0242 (9) | |
O12 | 0.4904 (4) | 0.48529 (18) | 0.15301 (17) | 0.0207 (9) | |
O13 | 0.5535 (4) | 0.60584 (17) | 0.15500 (16) | 0.0154 (8) | |
O14 | 0.7253 (4) | 0.72979 (19) | 0.37966 (17) | 0.0224 (9) | |
O15 | 0.1978 (4) | 0.63906 (18) | 0.29305 (17) | 0.0196 (9) | |
O16 | 0.6064 (4) | 0.60317 (17) | 0.26185 (16) | 0.0139 (8) | |
O17 | 0.1431 (4) | 0.64012 (19) | 0.16792 (17) | 0.0205 (9) | |
O18 | 0.3508 (4) | 0.56095 (17) | 0.21963 (16) | 0.0136 (8) | |
O19 | 0.3477 (4) | 0.68322 (18) | 0.09928 (17) | 0.0200 (9) | |
O20 | 0.4036 (4) | 0.67378 (16) | 0.21563 (15) | 0.0131 (8) | |
O21 | 0.8750 (4) | 0.65414 (19) | 0.31509 (16) | 0.0194 (9) | |
O22 | 0.4642 (4) | 0.67801 (18) | 0.32975 (16) | 0.0172 (8) | |
O23 | 0.4073 (4) | 0.55619 (18) | 0.32886 (16) | 0.0173 (8) | |
O24 | 0.2959 (4) | 0.44334 (17) | 0.21931 (17) | 0.0182 (8) | |
O25 | 0.6619 (4) | 0.71967 (17) | 0.26300 (16) | 0.0155 (8) | |
O26 | 0.2982 (4) | 0.55951 (18) | 0.10862 (16) | 0.0176 (8) | |
O27 | 0.2524 (4) | 0.78793 (19) | 0.02508 (18) | 0.0221 (9) | |
O28 | 0.6809 (5) | 0.6773 (2) | 0.04240 (18) | 0.0258 (10) | |
O29 | 0.4045 (4) | 0.6874 (2) | −0.01967 (17) | 0.0241 (9) | |
O30 | 0.4110 (4) | 0.8235 (2) | 0.13172 (17) | 0.0233 (9) | |
O31 | 0.4970 (4) | 0.87486 (19) | 0.02539 (19) | 0.0251 (10) | |
O32 | 0.6139 (5) | 0.7794 (2) | −0.04065 (17) | 0.0235 (9) | |
O34 | 0.7393 (4) | 0.81257 (19) | 0.07944 (17) | 0.0204 (9) | |
N1 | 0.0672 (5) | 0.8513 (2) | 0.0098 (2) | 0.0208 (11) | |
N2 | 0.7558 (7) | 0.5814 (3) | 0.0429 (2) | 0.0365 (15) | |
N3 | 0.4848 (5) | 0.8621 (2) | 0.21619 (19) | 0.0163 (10) | |
N4 | 0.6454 (5) | 0.7349 (2) | −0.1252 (2) | 0.0208 (11) | |
N5 | 0.9231 (5) | 0.8022 (2) | 0.1432 (2) | 0.0242 (11) | |
N6 | 0.2386 (5) | 0.6396 (2) | −0.0742 (2) | 0.0231 (11) | |
N7 | 0.5986 (5) | 0.9418 (2) | −0.0320 (2) | 0.0229 (11) | |
C1 | 0.7190 (12) | 0.5188 (4) | 0.0322 (4) | 0.066 (3) | |
H1A | 0.6202 | 0.5158 | 0.0211 | 0.099* | |
H1B | 0.7372 | 0.4959 | 0.0659 | 0.099* | |
H1C | 0.7755 | 0.5035 | 0.0026 | 0.099* | |
C2 | 0.9000 (9) | 0.5950 (4) | 0.0642 (4) | 0.051 (2) | |
H2A | 0.9068 | 0.6366 | 0.0733 | 0.076* | |
H2B | 0.9665 | 0.5855 | 0.0358 | 0.076* | |
H2C | 0.9212 | 0.5717 | 0.0973 | 0.076* | |
C3 | 0.5059 (9) | 0.9290 (4) | −0.0798 (3) | 0.044 (2) | |
H3A | 0.4308 | 0.9032 | −0.0686 | 0.066* | |
H3B | 0.5588 | 0.9097 | −0.1085 | 0.066* | |
H3C | 0.4661 | 0.9655 | −0.0945 | 0.066* | |
C4 | 0.0051 (7) | 0.9090 (3) | 0.0217 (3) | 0.0362 (17) | |
H4A | 0.0583 | 0.9277 | 0.0521 | 0.054* | |
H4B | −0.0916 | 0.9037 | 0.0322 | 0.054* | |
H4C | 0.0075 | 0.9337 | −0.0112 | 0.054* | |
C5 | 0.3351 (8) | 0.6291 (3) | −0.1192 (3) | 0.0358 (17) | |
H5A | 0.4313 | 0.6310 | −0.1045 | 0.054* | |
H5B | 0.3207 | 0.6589 | −0.1479 | 0.054* | |
H5C | 0.3174 | 0.5902 | −0.1351 | 0.054* | |
C6 | 0.8649 (8) | 0.8446 (3) | 0.1830 (3) | 0.0367 (17) | |
H6A | 0.8008 | 0.8713 | 0.1633 | 0.055* | |
H6B | 0.9410 | 0.8671 | 0.2007 | 0.055* | |
H6C | 0.8148 | 0.8233 | 0.2112 | 0.055* | |
C7 | 0.0886 (7) | 0.6255 (3) | −0.0866 (3) | 0.0368 (17) | |
H7A | 0.0350 | 0.6324 | −0.0536 | 0.055* | |
H7B | 0.0799 | 0.5844 | −0.0976 | 0.055* | |
H7C | 0.0527 | 0.6505 | −0.1167 | 0.055* | |
C8 | 0.5887 (6) | 0.9129 (3) | 0.0158 (3) | 0.0203 (13) | |
H8A | 0.6552 | 0.9216 | 0.0445 | 0.024* | |
C9 | 0.7809 (7) | 0.7086 (3) | −0.1073 (3) | 0.0276 (14) | |
H9A | 0.7909 | 0.7098 | −0.0670 | 0.041* | |
H9B | 0.8568 | 0.7307 | −0.1233 | 0.041* | |
H9C | 0.7843 | 0.6679 | −0.1198 | 0.041* | |
C10 | −0.0099 (6) | 0.8145 (3) | −0.0310 (3) | 0.0269 (15) | |
H10A | 0.0382 | 0.7770 | −0.0348 | 0.040* | |
H10B | −0.0146 | 0.8345 | −0.0668 | 0.040* | |
H10C | −0.1044 | 0.8076 | −0.0186 | 0.040* | |
C11 | 0.7072 (7) | 0.9873 (3) | −0.0392 (3) | 0.0319 (16) | |
H11A | 0.7539 | 0.9957 | −0.0035 | 0.048* | |
H11B | 0.6636 | 1.0231 | −0.0539 | 0.048* | |
H11C | 0.7756 | 0.9731 | −0.0651 | 0.048* | |
C12 | 0.2808 (7) | 0.6697 (3) | −0.0295 (3) | 0.0235 (13) | |
H12A | 0.2134 | 0.6786 | −0.0031 | 0.028* | |
C13 | 0.8526 (6) | 0.7890 (3) | 0.0971 (2) | 0.0220 (13) | |
H13A | 0.8898 | 0.7589 | 0.0750 | 0.026* | |
C14 | 1.0577 (7) | 0.7751 (3) | 0.1596 (3) | 0.0342 (16) | |
H14A | 1.0812 | 0.7452 | 0.1325 | 0.051* | |
H14B | 1.0508 | 0.7569 | 0.1960 | 0.051* | |
H14C | 1.1305 | 0.8051 | 0.1612 | 0.051* | |
C15 | 0.5684 (7) | 0.9061 (3) | 0.2482 (3) | 0.0242 (13) | |
H15A | 0.6118 | 0.9332 | 0.2227 | 0.036* | |
H15B | 0.6409 | 0.8861 | 0.2706 | 0.036* | |
H15C | 0.5075 | 0.9279 | 0.2724 | 0.036* | |
C16 | 0.6617 (8) | 0.6236 (3) | 0.0350 (3) | 0.0334 (16) | |
H16A | 0.5712 | 0.6118 | 0.0227 | 0.040* | |
C17 | 0.4069 (7) | 0.8192 (3) | 0.2492 (3) | 0.0254 (14) | |
H17A | 0.3605 | 0.7908 | 0.2245 | 0.038* | |
H17B | 0.3372 | 0.8397 | 0.2704 | 0.038* | |
H17C | 0.4718 | 0.7986 | 0.2746 | 0.038* | |
C18 | 0.5740 (6) | 0.7675 (3) | −0.0902 (2) | 0.0221 (13) | |
H18A | 0.4871 | 0.7829 | −0.1031 | 0.027* | |
C19 | 0.1897 (6) | 0.8363 (3) | 0.0339 (3) | 0.0203 (12) | |
H19A | 0.2326 | 0.8631 | 0.0591 | 0.024* | |
C20 | 0.5965 (7) | 0.7252 (3) | −0.1829 (3) | 0.0306 (15) | |
H20A | 0.5062 | 0.7444 | −0.1893 | 0.046* | |
H20B | 0.5868 | 0.6832 | −0.1897 | 0.046* | |
H20C | 0.6641 | 0.7417 | −0.2078 | 0.046* | |
C21 | 0.4796 (6) | 0.8606 (3) | 0.1616 (2) | 0.0218 (13) | |
H21A | 0.5311 | 0.8895 | 0.1430 | 0.026* |
U11 | U22 | U33 | U12 | U13 | U23 | |
La1 | 0.01295 (16) | 0.01314 (16) | 0.01263 (16) | −0.00067 (12) | −0.00078 (12) | 0.00088 (12) |
Mo1 | 0.0089 (2) | 0.0134 (2) | 0.0156 (2) | 0.00081 (18) | 0.00178 (17) | −0.00064 (18) |
Mo2 | 0.0154 (3) | 0.0144 (3) | 0.0217 (3) | −0.00443 (19) | 0.0005 (2) | −0.00126 (19) |
Mo3 | 0.0109 (2) | 0.0138 (2) | 0.0162 (2) | −0.00208 (18) | −0.00123 (18) | 0.00226 (18) |
Mo4 | 0.0124 (2) | 0.0161 (3) | 0.0212 (3) | −0.00006 (19) | −0.00218 (19) | 0.0038 (2) |
Mo5 | 0.0123 (2) | 0.0151 (3) | 0.0207 (3) | −0.00246 (19) | 0.00079 (19) | 0.00400 (19) |
Mo6 | 0.0118 (2) | 0.0173 (3) | 0.0148 (2) | −0.00178 (19) | 0.00051 (18) | −0.00103 (18) |
Mo7 | 0.0105 (2) | 0.0125 (2) | 0.0193 (3) | 0.00077 (18) | 0.00347 (18) | −0.00108 (18) |
Mo8 | 0.0099 (2) | 0.0139 (2) | 0.0138 (2) | −0.00226 (18) | 0.00023 (17) | 0.00247 (18) |
Na1 | 0.0195 (12) | 0.0268 (14) | 0.0305 (14) | 0.0038 (10) | 0.0006 (10) | 0.0038 (11) |
O1 | 0.016 (2) | 0.022 (2) | 0.030 (2) | −0.0044 (17) | −0.0025 (17) | 0.0069 (18) |
O2 | 0.025 (2) | 0.025 (2) | 0.030 (2) | −0.0051 (19) | −0.0035 (19) | 0.0104 (19) |
O3 | 0.033 (3) | 0.023 (2) | 0.033 (3) | −0.010 (2) | 0.002 (2) | −0.010 (2) |
O4 | 0.022 (2) | 0.019 (2) | 0.018 (2) | −0.0063 (17) | −0.0024 (16) | 0.0034 (16) |
O5 | 0.018 (2) | 0.0092 (19) | 0.026 (2) | −0.0003 (16) | 0.0013 (17) | −0.0003 (16) |
O6 | 0.014 (2) | 0.026 (2) | 0.023 (2) | −0.0019 (17) | 0.0021 (16) | −0.0005 (18) |
O7 | 0.0122 (19) | 0.024 (2) | 0.019 (2) | −0.0013 (17) | 0.0015 (15) | −0.0005 (17) |
O8 | 0.013 (2) | 0.020 (2) | 0.034 (2) | 0.0030 (17) | 0.0057 (17) | −0.0009 (18) |
O9 | 0.015 (2) | 0.019 (2) | 0.015 (2) | −0.0022 (16) | −0.0003 (15) | 0.0010 (16) |
O10 | 0.031 (3) | 0.026 (3) | 0.035 (3) | −0.005 (2) | −0.006 (2) | 0.011 (2) |
O11 | 0.017 (2) | 0.023 (2) | 0.032 (2) | 0.0028 (18) | −0.0032 (18) | −0.0023 (19) |
O12 | 0.019 (2) | 0.019 (2) | 0.024 (2) | 0.0008 (17) | 0.0028 (17) | −0.0048 (17) |
O13 | 0.0147 (19) | 0.015 (2) | 0.0164 (19) | −0.0027 (16) | 0.0029 (15) | 0.0005 (15) |
O14 | 0.019 (2) | 0.027 (2) | 0.021 (2) | −0.0085 (18) | 0.0018 (17) | −0.0054 (18) |
O15 | 0.011 (2) | 0.021 (2) | 0.026 (2) | −0.0010 (16) | 0.0027 (16) | −0.0028 (17) |
O16 | 0.0098 (18) | 0.0118 (19) | 0.020 (2) | 0.0018 (15) | 0.0020 (15) | 0.0012 (15) |
O17 | 0.013 (2) | 0.020 (2) | 0.028 (2) | −0.0005 (17) | −0.0031 (16) | 0.0027 (17) |
O18 | 0.0113 (19) | 0.0106 (19) | 0.019 (2) | −0.0005 (15) | 0.0014 (15) | 0.0003 (15) |
O19 | 0.018 (2) | 0.019 (2) | 0.023 (2) | −0.0058 (17) | −0.0049 (16) | 0.0065 (17) |
O20 | 0.0109 (19) | 0.0112 (19) | 0.0173 (19) | 0.0014 (15) | 0.0027 (15) | 0.0008 (15) |
O21 | 0.012 (2) | 0.025 (2) | 0.020 (2) | −0.0030 (17) | 0.0008 (16) | 0.0033 (17) |
O22 | 0.017 (2) | 0.018 (2) | 0.017 (2) | 0.0017 (16) | 0.0033 (16) | −0.0032 (16) |
O23 | 0.014 (2) | 0.018 (2) | 0.020 (2) | −0.0020 (16) | 0.0013 (16) | 0.0019 (16) |
O24 | 0.018 (2) | 0.012 (2) | 0.024 (2) | −0.0038 (16) | −0.0035 (16) | −0.0007 (16) |
O25 | 0.0129 (19) | 0.014 (2) | 0.019 (2) | −0.0030 (15) | −0.0042 (15) | 0.0012 (15) |
O26 | 0.017 (2) | 0.017 (2) | 0.018 (2) | −0.0058 (16) | −0.0004 (16) | −0.0019 (16) |
O27 | 0.017 (2) | 0.020 (2) | 0.028 (2) | 0.0031 (17) | −0.0056 (17) | −0.0003 (18) |
O28 | 0.028 (2) | 0.024 (2) | 0.025 (2) | 0.0124 (19) | −0.0013 (18) | −0.0016 (18) |
O29 | 0.022 (2) | 0.027 (2) | 0.023 (2) | 0.0006 (19) | −0.0047 (17) | −0.0055 (18) |
O30 | 0.020 (2) | 0.031 (3) | 0.019 (2) | 0.0002 (19) | −0.0001 (17) | −0.0032 (18) |
O31 | 0.024 (2) | 0.016 (2) | 0.036 (3) | −0.0009 (18) | 0.0075 (19) | 0.0057 (18) |
O32 | 0.026 (2) | 0.027 (2) | 0.017 (2) | −0.0020 (19) | 0.0028 (17) | −0.0021 (17) |
O34 | 0.013 (2) | 0.024 (2) | 0.024 (2) | −0.0060 (17) | −0.0039 (16) | 0.0062 (17) |
N1 | 0.017 (3) | 0.022 (3) | 0.023 (3) | 0.001 (2) | 0.003 (2) | 0.004 (2) |
N2 | 0.056 (4) | 0.026 (3) | 0.028 (3) | 0.021 (3) | 0.007 (3) | 0.007 (2) |
N3 | 0.018 (2) | 0.015 (2) | 0.016 (2) | −0.003 (2) | 0.0019 (19) | 0.0009 (19) |
N4 | 0.023 (3) | 0.020 (3) | 0.019 (3) | 0.004 (2) | −0.001 (2) | −0.005 (2) |
N5 | 0.018 (3) | 0.025 (3) | 0.029 (3) | 0.000 (2) | −0.001 (2) | 0.005 (2) |
N6 | 0.021 (3) | 0.020 (3) | 0.028 (3) | 0.002 (2) | −0.006 (2) | −0.002 (2) |
N7 | 0.022 (3) | 0.022 (3) | 0.025 (3) | −0.002 (2) | 0.002 (2) | 0.005 (2) |
C1 | 0.105 (8) | 0.021 (4) | 0.072 (7) | 0.022 (5) | 0.003 (6) | 0.000 (4) |
C2 | 0.044 (5) | 0.063 (6) | 0.046 (5) | 0.027 (4) | 0.003 (4) | 0.005 (4) |
C3 | 0.048 (5) | 0.048 (5) | 0.035 (4) | −0.012 (4) | −0.016 (3) | 0.012 (4) |
C4 | 0.024 (4) | 0.026 (4) | 0.058 (5) | 0.007 (3) | 0.004 (3) | −0.001 (3) |
C5 | 0.035 (4) | 0.036 (4) | 0.037 (4) | 0.005 (3) | −0.001 (3) | −0.015 (3) |
C6 | 0.033 (4) | 0.041 (4) | 0.036 (4) | 0.005 (3) | −0.002 (3) | −0.014 (3) |
C7 | 0.020 (3) | 0.041 (4) | 0.048 (4) | 0.000 (3) | −0.014 (3) | −0.011 (3) |
C8 | 0.015 (3) | 0.022 (3) | 0.023 (3) | 0.007 (2) | 0.000 (2) | 0.000 (2) |
C9 | 0.026 (3) | 0.026 (4) | 0.031 (4) | 0.004 (3) | −0.001 (3) | −0.004 (3) |
C10 | 0.017 (3) | 0.047 (4) | 0.016 (3) | 0.002 (3) | 0.000 (2) | −0.002 (3) |
C11 | 0.022 (3) | 0.028 (4) | 0.046 (4) | −0.002 (3) | 0.000 (3) | 0.014 (3) |
C12 | 0.024 (3) | 0.017 (3) | 0.029 (3) | 0.000 (3) | −0.003 (3) | −0.003 (3) |
C13 | 0.024 (3) | 0.024 (3) | 0.018 (3) | −0.007 (3) | 0.004 (2) | 0.008 (2) |
C14 | 0.022 (3) | 0.037 (4) | 0.043 (4) | 0.006 (3) | −0.011 (3) | 0.008 (3) |
C15 | 0.027 (3) | 0.022 (3) | 0.023 (3) | −0.002 (3) | −0.002 (3) | −0.002 (3) |
C16 | 0.049 (4) | 0.020 (4) | 0.030 (4) | 0.008 (3) | −0.006 (3) | 0.001 (3) |
C17 | 0.031 (4) | 0.024 (3) | 0.023 (3) | −0.002 (3) | 0.013 (3) | 0.000 (3) |
C18 | 0.017 (3) | 0.031 (3) | 0.019 (3) | 0.004 (3) | 0.002 (2) | 0.001 (3) |
C19 | 0.017 (3) | 0.021 (3) | 0.024 (3) | −0.004 (2) | 0.003 (2) | 0.002 (2) |
C20 | 0.030 (4) | 0.041 (4) | 0.021 (3) | 0.008 (3) | 0.002 (3) | −0.004 (3) |
C21 | 0.019 (3) | 0.025 (3) | 0.021 (3) | 0.001 (3) | 0.001 (2) | 0.002 (3) |
La1—O32 | 2.474 (4) | O30—C21 | 1.257 (7) |
La1—O27 | 2.498 (4) | O31—C8 | 1.240 (7) |
La1—O30 | 2.519 (4) | O32—C18 | 1.251 (7) |
La1—O34 | 2.532 (4) | O34—C13 | 1.249 (7) |
La1—O29 | 2.557 (4) | N1—C19 | 1.313 (8) |
La1—O28 | 2.560 (4) | N1—C10 | 1.449 (8) |
La1—O31 | 2.569 (4) | N1—C4 | 1.450 (8) |
La1—O4 | 2.573 (4) | N2—C16 | 1.303 (9) |
La1—O19 | 2.618 (4) | N2—C2 | 1.464 (11) |
Mo1—O15 | 1.701 (4) | N2—C1 | 1.467 (10) |
Mo1—O22 | 1.759 (4) | N3—C21 | 1.295 (7) |
Mo1—O23 | 1.946 (4) | N3—C17 | 1.456 (7) |
Mo1—O20 | 1.951 (4) | N3—C15 | 1.458 (8) |
Mo1—O18 | 2.147 (4) | N4—C18 | 1.311 (8) |
Mo1—O16 | 2.335 (4) | N4—C20 | 1.444 (8) |
Mo1—Mo3 | 3.2057 (7) | N4—C9 | 1.455 (8) |
Mo2—O3 | 1.700 (4) | N5—C13 | 1.293 (8) |
Mo2—O1 | 1.715 (4) | N5—C14 | 1.447 (8) |
Mo2—O24 | 1.936 (4) | N5—C6 | 1.461 (8) |
Mo2—O26 | 1.942 (4) | N6—C12 | 1.308 (8) |
Mo2—O12 | 2.261 (4) | N6—C5 | 1.448 (8) |
Mo2—O18 | 2.435 (4) | N6—C7 | 1.467 (8) |
Mo3—O17 | 1.698 (4) | N7—C8 | 1.314 (8) |
Mo3—O19 | 1.728 (4) | N7—C3 | 1.437 (9) |
Mo3—O26 | 1.877 (4) | N7—C11 | 1.458 (8) |
Mo3—O20 | 1.989 (4) | C1—H1A | 0.9600 |
Mo3—O18 | 2.284 (4) | C1—H1B | 0.9600 |
Mo3—O13 | 2.315 (4) | C1—H1C | 0.9600 |
Mo4—O10 | 1.692 (4) | C2—H2A | 0.9600 |
Mo4—O11 | 1.705 (4) | C2—H2B | 0.9600 |
Mo4—O9 | 1.899 (4) | C2—H2C | 0.9600 |
Mo4—O5 | 2.018 (4) | C3—H3A | 0.9600 |
Mo4—O23 | 2.286 (4) | C3—H3B | 0.9600 |
Mo4—O16 | 2.352 (4) | C3—H3C | 0.9600 |
Mo5—O2 | 1.703 (4) | C4—H4A | 0.9600 |
Mo5—O6 | 1.715 (4) | C4—H4B | 0.9600 |
Mo5—O24 | 1.894 (4) | C4—H4C | 0.9600 |
Mo5—O23 | 2.027 (4) | C5—H5A | 0.9600 |
Mo5—O5 | 2.302 (4) | C5—H5B | 0.9600 |
Mo5—O18 | 2.364 (4) | C5—H5C | 0.9600 |
Mo6—O14 | 1.702 (4) | C6—H6A | 0.9600 |
Mo6—O21 | 1.716 (4) | C6—H6B | 0.9600 |
Mo6—O9 | 1.918 (4) | C6—H6C | 0.9600 |
Mo6—O25 | 1.932 (4) | C7—H7A | 0.9600 |
Mo6—O22 | 2.272 (4) | C7—H7B | 0.9600 |
Mo6—O16 | 2.449 (4) | C7—H7C | 0.9600 |
Mo6—Mo8 | 3.2103 (6) | C8—H8A | 0.9300 |
Mo7—O8 | 1.699 (4) | C9—H9A | 0.9600 |
Mo7—O12 | 1.753 (4) | C9—H9B | 0.9600 |
Mo7—O5 | 1.946 (4) | C9—H9C | 0.9600 |
Mo7—O13 | 1.947 (4) | C10—H10A | 0.9600 |
Mo7—O16 | 2.156 (4) | C10—H10B | 0.9600 |
Mo7—O18 | 2.330 (4) | C10—H10C | 0.9600 |
Mo7—Mo8 | 3.1957 (7) | C11—H11A | 0.9600 |
Mo8—O7 | 1.700 (4) | C11—H11B | 0.9600 |
Mo8—O4 | 1.714 (4) | C11—H11C | 0.9600 |
Mo8—O25 | 1.881 (4) | C12—H12A | 0.9300 |
Mo8—O13 | 1.997 (4) | C13—H13A | 0.9300 |
Mo8—O16 | 2.249 (4) | C14—H14A | 0.9600 |
Mo8—O20 | 2.338 (4) | C14—H14B | 0.9600 |
Na1—O6i | 2.520 (5) | C14—H14C | 0.9600 |
Na1—O7 | 2.534 (5) | C15—H15A | 0.9600 |
Na1—O21 | 2.573 (5) | C15—H15B | 0.9600 |
Na1—O1i | 2.611 (5) | C15—H15C | 0.9600 |
Na1—O15i | 2.651 (5) | C16—H16A | 0.9300 |
Na1—O11 | 2.661 (5) | C17—H17A | 0.9600 |
Na1—O17i | 2.730 (5) | C17—H17B | 0.9600 |
Na1—O8 | 2.776 (5) | C17—H17C | 0.9600 |
O1—Na1ii | 2.611 (5) | C18—H18A | 0.9300 |
O6—Na1ii | 2.520 (5) | C19—H19A | 0.9300 |
O15—Na1ii | 2.651 (5) | C20—H20A | 0.9600 |
O17—Na1ii | 2.730 (5) | C20—H20B | 0.9600 |
O27—C19 | 1.255 (7) | C20—H20C | 0.9600 |
O28—C16 | 1.230 (8) | C21—H21A | 0.9300 |
O29—C12 | 1.244 (7) | ||
O32—La1—O27 | 99.75 (14) | O21—Na1—O15i | 73.39 (14) |
O32—La1—O30 | 139.60 (14) | O1i—Na1—O15i | 107.91 (15) |
O27—La1—O30 | 73.45 (13) | O6i—Na1—O11 | 75.19 (14) |
O32—La1—O34 | 77.58 (13) | O7—Na1—O11 | 105.15 (15) |
O27—La1—O34 | 141.64 (14) | O21—Na1—O11 | 68.76 (14) |
O30—La1—O34 | 84.09 (14) | O1i—Na1—O11 | 111.59 (16) |
O32—La1—O29 | 70.59 (14) | O15i—Na1—O11 | 114.65 (16) |
O27—La1—O29 | 69.77 (14) | O6i—Na1—O17i | 106.43 (15) |
O30—La1—O29 | 136.31 (14) | O7—Na1—O17i | 73.19 (14) |
O34—La1—O29 | 139.55 (14) | O21—Na1—O17i | 112.03 (15) |
O32—La1—O28 | 75.16 (14) | O1i—Na1—O17i | 67.53 (14) |
O27—La1—O28 | 139.23 (14) | O15i—Na1—O17i | 67.69 (13) |
O30—La1—O28 | 135.39 (14) | O11—Na1—O17i | 177.61 (16) |
O34—La1—O28 | 77.81 (14) | O6i—Na1—O8 | 110.05 (16) |
O29—La1—O28 | 70.50 (14) | O7—Na1—O8 | 69.03 (14) |
O32—La1—O31 | 70.01 (14) | O21—Na1—O8 | 107.92 (14) |
O27—La1—O31 | 73.06 (14) | O1i—Na1—O8 | 70.79 (14) |
O30—La1—O31 | 69.95 (14) | O15i—Na1—O8 | 178.68 (16) |
O34—La1—O31 | 70.13 (14) | O11—Na1—O8 | 65.92 (14) |
O29—La1—O31 | 118.81 (14) | O17i—Na1—O8 | 111.74 (15) |
O28—La1—O31 | 136.57 (14) | Mo2—O1—Na1ii | 133.2 (2) |
O32—La1—O4 | 131.90 (14) | Mo8—O4—La1 | 152.9 (2) |
O27—La1—O4 | 128.28 (13) | Mo7—O5—Mo4 | 109.19 (18) |
O30—La1—O4 | 68.46 (13) | Mo7—O5—Mo5 | 110.87 (18) |
O34—La1—O4 | 66.61 (13) | Mo4—O5—Mo5 | 104.25 (17) |
O29—La1—O4 | 119.53 (13) | Mo5—O6—Na1ii | 134.7 (2) |
O28—La1—O4 | 66.93 (14) | Mo8—O7—Na1 | 132.7 (2) |
O31—La1—O4 | 121.65 (14) | Mo7—O8—Na1 | 125.4 (2) |
O32—La1—O19 | 137.87 (14) | Mo4—O9—Mo6 | 115.79 (19) |
O27—La1—O19 | 73.14 (13) | Mo4—O11—Na1 | 135.4 (2) |
O30—La1—O19 | 79.47 (14) | Mo7—O12—Mo2 | 116.82 (19) |
O34—La1—O19 | 133.28 (13) | Mo7—O13—Mo8 | 108.25 (18) |
O29—La1—O19 | 68.03 (13) | Mo7—O13—Mo3 | 109.90 (16) |
O28—La1—O19 | 83.97 (14) | Mo8—O13—Mo3 | 104.23 (16) |
O31—La1—O19 | 139.45 (13) | Mo1—O15—Na1ii | 127.9 (2) |
O4—La1—O19 | 66.68 (12) | Mo7—O16—Mo8 | 93.00 (14) |
O15—Mo1—O22 | 106.18 (19) | Mo7—O16—Mo1 | 104.48 (15) |
O15—Mo1—O23 | 100.99 (18) | Mo8—O16—Mo1 | 99.60 (14) |
O22—Mo1—O23 | 97.17 (18) | Mo7—O16—Mo4 | 91.49 (14) |
O15—Mo1—O20 | 101.34 (18) | Mo8—O16—Mo4 | 161.79 (18) |
O22—Mo1—O20 | 95.58 (17) | Mo1—O16—Mo4 | 96.33 (13) |
O23—Mo1—O20 | 149.99 (16) | Mo7—O16—Mo6 | 163.60 (18) |
O15—Mo1—O18 | 96.78 (17) | Mo8—O16—Mo6 | 86.10 (13) |
O22—Mo1—O18 | 156.97 (16) | Mo1—O16—Mo6 | 91.80 (13) |
O23—Mo1—O18 | 79.85 (16) | Mo4—O16—Mo6 | 84.64 (12) |
O20—Mo1—O18 | 77.84 (15) | Mo3—O17—Na1ii | 131.6 (2) |
O15—Mo1—O16 | 172.08 (17) | Mo1—O18—Mo3 | 92.63 (14) |
O22—Mo1—O16 | 81.73 (16) | Mo1—O18—Mo7 | 104.92 (15) |
O23—Mo1—O16 | 78.15 (14) | Mo3—O18—Mo7 | 98.48 (14) |
O20—Mo1—O16 | 76.97 (14) | Mo1—O18—Mo5 | 91.14 (13) |
O18—Mo1—O16 | 75.30 (14) | Mo3—O18—Mo5 | 162.99 (18) |
O15—Mo1—Mo3 | 89.23 (14) | Mo7—O18—Mo5 | 96.56 (14) |
O22—Mo1—Mo3 | 131.52 (13) | Mo1—O18—Mo2 | 163.01 (18) |
O23—Mo1—Mo3 | 125.19 (12) | Mo3—O18—Mo2 | 85.99 (12) |
O20—Mo1—Mo3 | 35.94 (11) | Mo7—O18—Mo2 | 92.02 (13) |
O18—Mo1—Mo3 | 45.38 (10) | Mo5—O18—Mo2 | 85.58 (12) |
O16—Mo1—Mo3 | 84.96 (9) | Mo3—O19—La1 | 153.4 (2) |
O3—Mo2—O1 | 104.7 (2) | Mo1—O20—Mo3 | 108.90 (17) |
O3—Mo2—O24 | 103.7 (2) | Mo1—O20—Mo8 | 109.12 (16) |
O1—Mo2—O24 | 98.01 (18) | Mo3—O20—Mo8 | 103.65 (15) |
O3—Mo2—O26 | 102.0 (2) | Mo6—O21—Na1 | 134.2 (2) |
O1—Mo2—O26 | 97.69 (18) | Mo1—O22—Mo6 | 116.37 (19) |
O24—Mo2—O26 | 145.21 (16) | Mo1—O23—Mo5 | 108.52 (18) |
O3—Mo2—O12 | 94.48 (19) | Mo1—O23—Mo4 | 110.94 (17) |
O1—Mo2—O12 | 160.79 (18) | Mo5—O23—Mo4 | 104.54 (17) |
O24—Mo2—O12 | 77.28 (16) | Mo5—O24—Mo2 | 116.7 (2) |
O26—Mo2—O12 | 77.72 (16) | Mo8—O25—Mo6 | 114.7 (2) |
O3—Mo2—O18 | 164.34 (18) | Mo3—O26—Mo2 | 114.98 (19) |
O1—Mo2—O18 | 90.88 (17) | C19—O27—La1 | 126.6 (4) |
O24—Mo2—O18 | 74.85 (15) | C16—O28—La1 | 131.3 (5) |
O26—Mo2—O18 | 74.06 (15) | C12—O29—La1 | 131.1 (4) |
O12—Mo2—O18 | 69.91 (13) | C21—O30—La1 | 126.3 (4) |
O17—Mo3—O19 | 106.5 (2) | C8—O31—La1 | 134.1 (4) |
O17—Mo3—O26 | 100.18 (19) | C18—O32—La1 | 132.9 (4) |
O19—Mo3—O26 | 102.92 (19) | C13—O34—La1 | 129.0 (4) |
O17—Mo3—O20 | 97.04 (18) | C19—N1—C10 | 123.8 (5) |
O19—Mo3—O20 | 97.59 (17) | C19—N1—C4 | 119.9 (6) |
O26—Mo3—O20 | 148.11 (16) | C10—N1—C4 | 116.2 (5) |
O17—Mo3—O18 | 91.52 (17) | C16—N2—C2 | 121.1 (7) |
O19—Mo3—O18 | 161.06 (16) | C16—N2—C1 | 120.9 (7) |
O26—Mo3—O18 | 78.99 (16) | C2—N2—C1 | 117.9 (7) |
O20—Mo3—O18 | 73.88 (14) | C21—N3—C17 | 121.4 (5) |
O17—Mo3—O13 | 161.83 (17) | C21—N3—C15 | 122.6 (5) |
O19—Mo3—O13 | 89.86 (17) | C17—N3—C15 | 116.0 (5) |
O26—Mo3—O13 | 83.38 (15) | C18—N4—C20 | 122.1 (5) |
O20—Mo3—O13 | 72.42 (14) | C18—N4—C9 | 120.3 (5) |
O18—Mo3—O13 | 71.54 (13) | C20—N4—C9 | 117.5 (5) |
O17—Mo3—Mo1 | 83.74 (14) | C13—N5—C14 | 123.4 (6) |
O19—Mo3—Mo1 | 132.65 (14) | C13—N5—C6 | 120.2 (6) |
O26—Mo3—Mo1 | 120.98 (12) | C14—N5—C6 | 116.4 (6) |
O20—Mo3—Mo1 | 35.15 (11) | C12—N6—C5 | 120.2 (6) |
O18—Mo3—Mo1 | 41.99 (9) | C12—N6—C7 | 122.4 (6) |
O13—Mo3—Mo1 | 79.24 (9) | C5—N6—C7 | 116.3 (5) |
O10—Mo4—O11 | 105.2 (2) | C8—N7—C3 | 121.6 (6) |
O10—Mo4—O9 | 101.5 (2) | C8—N7—C11 | 121.3 (5) |
O11—Mo4—O9 | 100.45 (19) | C3—N7—C11 | 117.1 (5) |
O10—Mo4—O5 | 102.1 (2) | N2—C1—H1A | 109.5 |
O11—Mo4—O5 | 96.02 (18) | N2—C1—H1B | 109.5 |
O9—Mo4—O5 | 146.47 (16) | H1A—C1—H1B | 109.5 |
O10—Mo4—O23 | 94.27 (19) | N2—C1—H1C | 109.5 |
O11—Mo4—O23 | 158.84 (18) | H1A—C1—H1C | 109.5 |
O9—Mo4—O23 | 83.42 (15) | H1B—C1—H1C | 109.5 |
O5—Mo4—O23 | 71.36 (15) | N2—C2—H2A | 109.5 |
O10—Mo4—O16 | 165.90 (19) | N2—C2—H2B | 109.5 |
O11—Mo4—O16 | 88.66 (17) | H2A—C2—H2B | 109.5 |
O9—Mo4—O16 | 78.20 (15) | N2—C2—H2C | 109.5 |
O5—Mo4—O16 | 73.18 (14) | H2A—C2—H2C | 109.5 |
O23—Mo4—O16 | 71.65 (13) | H2B—C2—H2C | 109.5 |
O2—Mo5—O6 | 105.3 (2) | N7—C3—H3A | 109.5 |
O2—Mo5—O24 | 103.4 (2) | N7—C3—H3B | 109.5 |
O6—Mo5—O24 | 101.05 (18) | H3A—C3—H3B | 109.5 |
O2—Mo5—O23 | 100.18 (19) | N7—C3—H3C | 109.5 |
O6—Mo5—O23 | 95.69 (18) | H3A—C3—H3C | 109.5 |
O24—Mo5—O23 | 146.14 (16) | H3B—C3—H3C | 109.5 |
O2—Mo5—O5 | 92.26 (18) | N1—C4—H4A | 109.5 |
O6—Mo5—O5 | 159.77 (17) | N1—C4—H4B | 109.5 |
O24—Mo5—O5 | 84.19 (16) | H4A—C4—H4B | 109.5 |
O23—Mo5—O5 | 70.88 (15) | N1—C4—H4C | 109.5 |
O2—Mo5—O18 | 163.33 (17) | H4A—C4—H4C | 109.5 |
O6—Mo5—O18 | 90.76 (17) | H4B—C4—H4C | 109.5 |
O24—Mo5—O18 | 77.34 (15) | N6—C5—H5A | 109.5 |
O23—Mo5—O18 | 73.18 (14) | N6—C5—H5B | 109.5 |
O5—Mo5—O18 | 71.17 (13) | H5A—C5—H5B | 109.5 |
O14—Mo6—O21 | 105.2 (2) | N6—C5—H5C | 109.5 |
O14—Mo6—O9 | 103.67 (18) | H5A—C5—H5C | 109.5 |
O21—Mo6—O9 | 97.80 (18) | H5B—C5—H5C | 109.5 |
O14—Mo6—O25 | 101.70 (19) | N5—C6—H6A | 109.5 |
O21—Mo6—O25 | 97.43 (18) | N5—C6—H6B | 109.5 |
O9—Mo6—O25 | 145.69 (16) | H6A—C6—H6B | 109.5 |
O14—Mo6—O22 | 93.90 (17) | N5—C6—H6C | 109.5 |
O21—Mo6—O22 | 160.92 (17) | H6A—C6—H6C | 109.5 |
O9—Mo6—O22 | 77.61 (15) | H6B—C6—H6C | 109.5 |
O25—Mo6—O22 | 77.99 (15) | N6—C7—H7A | 109.5 |
O14—Mo6—O16 | 163.84 (17) | N6—C7—H7B | 109.5 |
O21—Mo6—O16 | 90.86 (16) | H7A—C7—H7B | 109.5 |
O9—Mo6—O16 | 75.43 (15) | N6—C7—H7C | 109.5 |
O25—Mo6—O16 | 73.78 (14) | H7A—C7—H7C | 109.5 |
O22—Mo6—O16 | 70.06 (13) | H7B—C7—H7C | 109.5 |
O14—Mo6—Mo8 | 133.73 (15) | O31—C8—N7 | 124.7 (6) |
O21—Mo6—Mo8 | 85.08 (13) | O31—C8—H8A | 117.6 |
O9—Mo6—Mo8 | 119.76 (12) | N7—C8—H8A | 117.6 |
O25—Mo6—Mo8 | 32.15 (12) | N4—C9—H9A | 109.5 |
O22—Mo6—Mo8 | 81.39 (10) | N4—C9—H9B | 109.5 |
O16—Mo6—Mo8 | 44.33 (9) | H9A—C9—H9B | 109.5 |
O8—Mo7—O12 | 105.8 (2) | N4—C9—H9C | 109.5 |
O8—Mo7—O5 | 101.20 (19) | H9A—C9—H9C | 109.5 |
O12—Mo7—O5 | 97.24 (18) | H9B—C9—H9C | 109.5 |
O8—Mo7—O13 | 100.81 (18) | N1—C10—H10A | 109.5 |
O12—Mo7—O13 | 96.63 (18) | N1—C10—H10B | 109.5 |
O5—Mo7—O13 | 149.61 (16) | H10A—C10—H10B | 109.5 |
O8—Mo7—O16 | 97.71 (17) | N1—C10—H10C | 109.5 |
O12—Mo7—O16 | 156.46 (16) | H10A—C10—H10C | 109.5 |
O5—Mo7—O16 | 79.17 (15) | H10B—C10—H10C | 109.5 |
O13—Mo7—O16 | 77.35 (15) | N7—C11—H11A | 109.5 |
O8—Mo7—O18 | 172.92 (17) | N7—C11—H11B | 109.5 |
O12—Mo7—O18 | 81.25 (16) | H11A—C11—H11B | 109.5 |
O5—Mo7—O18 | 78.28 (15) | N7—C11—H11C | 109.5 |
O13—Mo7—O18 | 77.30 (14) | H11A—C11—H11C | 109.5 |
O16—Mo7—O18 | 75.23 (13) | H11B—C11—H11C | 109.5 |
O8—Mo7—Mo8 | 88.97 (14) | O29—C12—N6 | 124.9 (6) |
O12—Mo7—Mo8 | 133.03 (14) | O29—C12—H12A | 117.6 |
O5—Mo7—Mo8 | 123.81 (12) | N6—C12—H12A | 117.6 |
O13—Mo7—Mo8 | 36.39 (11) | O34—C13—N5 | 126.4 (6) |
O16—Mo7—Mo8 | 44.64 (10) | O34—C13—H13A | 116.8 |
O18—Mo7—Mo8 | 85.54 (9) | N5—C13—H13A | 116.8 |
O7—Mo8—O4 | 106.3 (2) | N5—C14—H14A | 109.5 |
O7—Mo8—O25 | 101.20 (18) | N5—C14—H14B | 109.5 |
O4—Mo8—O25 | 101.52 (18) | H14A—C14—H14B | 109.5 |
O7—Mo8—O13 | 97.64 (18) | N5—C14—H14C | 109.5 |
O4—Mo8—O13 | 96.89 (17) | H14A—C14—H14C | 109.5 |
O25—Mo8—O13 | 148.65 (16) | H14B—C14—H14C | 109.5 |
O7—Mo8—O16 | 93.68 (16) | N3—C15—H15A | 109.5 |
O4—Mo8—O16 | 159.16 (17) | N3—C15—H15B | 109.5 |
O25—Mo8—O16 | 79.75 (15) | H15A—C15—H15B | 109.5 |
O13—Mo8—O16 | 74.21 (15) | N3—C15—H15C | 109.5 |
O7—Mo8—O20 | 163.57 (17) | H15A—C15—H15C | 109.5 |
O4—Mo8—O20 | 87.78 (17) | H15B—C15—H15C | 109.5 |
O25—Mo8—O20 | 83.73 (15) | O28—C16—N2 | 126.4 (7) |
O13—Mo8—O20 | 71.79 (14) | O28—C16—H16A | 116.8 |
O16—Mo8—O20 | 71.60 (13) | N2—C16—H16A | 116.8 |
O7—Mo8—Mo7 | 84.92 (14) | N3—C17—H17A | 109.5 |
O4—Mo8—Mo7 | 132.20 (13) | N3—C17—H17B | 109.5 |
O25—Mo8—Mo7 | 122.09 (12) | H17A—C17—H17B | 109.5 |
O13—Mo8—Mo7 | 35.35 (11) | N3—C17—H17C | 109.5 |
O16—Mo8—Mo7 | 42.35 (10) | H17A—C17—H17C | 109.5 |
O20—Mo8—Mo7 | 79.25 (9) | H17B—C17—H17C | 109.5 |
O7—Mo8—Mo6 | 88.79 (13) | O32—C18—N4 | 124.9 (6) |
O4—Mo8—Mo6 | 134.66 (14) | O32—C18—H18A | 117.5 |
O25—Mo8—Mo6 | 33.14 (12) | N4—C18—H18A | 117.5 |
O13—Mo8—Mo6 | 123.74 (11) | O27—C19—N1 | 124.0 (6) |
O16—Mo8—Mo6 | 49.56 (10) | O27—C19—H19A | 118.0 |
O20—Mo8—Mo6 | 87.02 (9) | N1—C19—H19A | 118.0 |
Mo7—Mo8—Mo6 | 90.720 (16) | N4—C20—H20A | 109.5 |
O6i—Na1—O7 | 178.63 (17) | N4—C20—H20B | 109.5 |
O6i—Na1—O21 | 108.63 (16) | H20A—C20—H20B | 109.5 |
O7—Na1—O21 | 72.70 (14) | N4—C20—H20C | 109.5 |
O6i—Na1—O1i | 73.22 (14) | H20A—C20—H20C | 109.5 |
O7—Na1—O1i | 105.45 (15) | H20B—C20—H20C | 109.5 |
O21—Na1—O1i | 178.10 (17) | O30—C21—N3 | 125.6 (6) |
O6i—Na1—O15i | 69.18 (14) | O30—C21—H21A | 117.2 |
O7—Na1—O15i | 111.73 (16) | N3—C21—H21A | 117.2 |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [NaLaMo8O26(C3H7N)7] |
Mr | 1857.09 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 9.418 (1), 22.4088 (10), 23.7508 (13) |
β (°) | 92.098 (3) |
V (Å3) | 5009.2 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.87 |
Crystal size (mm) | 0.28 × 0.20 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART P4 diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.507, 0.795 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 29069, 8775, 8115 |
Rint | 0.037 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.097, 0.99 |
No. of reflections | 8775 |
No. of parameters | 654 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.046P)2 + 34.1827P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.24, −0.86 |
Computer programs: SMART (Siemens, 1996), SMART and SAINT (Siemens,1994), XPREP in SHELXTL (Siemens, 1994) and SAINT?, SHELXTL.
La1—O32 | 2.474 (4) | Na1—O6i | 2.520 (5) |
La1—O27 | 2.498 (4) | Na1—O7 | 2.534 (5) |
La1—O30 | 2.519 (4) | Na1—O21 | 2.573 (5) |
La1—O34 | 2.532 (4) | Na1—O1i | 2.611 (5) |
La1—O29 | 2.557 (4) | Na1—O15i | 2.651 (5) |
La1—O28 | 2.560 (4) | Na1—O11 | 2.661 (5) |
La1—O31 | 2.569 (4) | Na1—O17i | 2.730 (5) |
La1—O4 | 2.573 (4) | Na1—O8 | 2.776 (5) |
La1—O19 | 2.618 (4) | ||
O32—La1—O4 | 131.90 (14) | O28—La1—O19 | 83.97 (14) |
O27—La1—O4 | 128.28 (13) | O31—La1—O19 | 139.45 (13) |
O30—La1—O4 | 68.46 (13) | O4—La1—O19 | 66.68 (12) |
O34—La1—O4 | 66.61 (13) | O7—Na1—O21 | 72.70 (14) |
O29—La1—O4 | 119.53 (13) | O7—Na1—O11 | 105.15 (15) |
O28—La1—O4 | 66.93 (14) | O21—Na1—O11 | 68.76 (14) |
O31—La1—O4 | 121.65 (14) | O7—Na1—O8 | 69.03 (14) |
O32—La1—O19 | 137.87 (14) | O21—Na1—O8 | 107.92 (14) |
O27—La1—O19 | 73.14 (13) | O1i—Na1—O8 | 70.79 (14) |
O30—La1—O19 | 79.47 (14) | O15i—Na1—O8 | 178.68 (16) |
O34—La1—O19 | 133.28 (13) | O11—Na1—O8 | 65.92 (14) |
O29—La1—O19 | 68.03 (13) | O17i—Na1—O8 | 111.74 (15) |
Symmetry code: (i) x+1, y, z. |
In the past decade, considerable progress had been made in the rational design and synthesis of new polyoxometalates (POMs) owing to their intriguing topological structures and applicable properties (Müller et al., 1995, 1998; Pope & Müller, 1991). One of the most challenging tasks is to obtain some POM building blocks and link them into larger discrete clusters, or one-, two- or even three-dimensional extended frameworks in appropriate ways. We are currently making great efforts to link some basic building blocks, such as [Mo6O19]2−, with rare earth salts to form new interesting extended compounds. We report here the synthesis and characterization of the title compound, (I).
The title compound consists of an infinite chain framework built up of octamolybdate-supported dimethylformamide-coordinated LaIII cations and Na+ ions (Fig. 1). The lanthanum center adopts a nine-coordinate geometry, and the locally centrosymmetric anion, β-Mo8O264−, is linked to the LaIII ion through two terminal O atoms (O4 and O19). The most interesting feature is that the LaIII ions are located on only one side of the infinite chain, thus producing a locally non-centrosymmetric anionic cluster. Finally, seven O atoms from dimethylformamide (DMF) solvents complete the nine-coordinate environment of the La atom, with La—O distances of 2.474 (4)–2.618 (4) Å and O—La—O bond angles of 66.61 (13)–83.97 (14)° for the neighboring O atoms (Table 1). In the plumb direction, the β-Mo8O26 units are linked by Na+ cations so that the structure extends to a one-dimensional infinite chain. The Na center is eight-coordinate, and one β-Mo8O26 unit supports four terminal O atoms; the Na atom is sandwiched between two β-Mo8O26 units (Fig. 2). The distance between two adjacent La atoms is 9.418 (1) Å, along the a axis. The backbone framework of (I) is roughly similar to that of [NH4][La(DMF)7(β-Mo8O26)], (II) (Wu et al., 2002), although the structure of (I) is extended into a one-dimensional infinite chain via Na atoms, while the complex in (II) is discrete.
In the preparation, the β-[Mo8O26]4− unit was formed unexpectedly from [Mo6O19]2− and Na2MoO4. The structure of (I) may give a hint for the synthesis of other transition-metal compounds by linking some appropriate basic building blocks in a controllable way.