The triple molybdates K3–xNa1+xM4(MoO4)6 (M = Ni, Mg, Co) and K3+xLi1–xMg4(MoO4)6 were found upon studying the corresponding ternary molybdate systems, and their structures, thermal stability and electrical conductiviplusmnty were investigated. The compounds crystallize in the space group R3c and are isostructural with the sodium-ion conductor II-Na3Fe2(AsO4)3 and yurmarinite, Na7(Fe3+, Mg, Cu)4(AsO4)6; their basic structural units are flat polyhedral clusters of the central M1O6 octahedron sharing edges with three surrounding M2O6 octahedra, which combine with single NaO6 octahedra and bridging MoO4 tetrahedra to form open three-dimensional (3D) frameworks where the cavities are partially occupied by disordered potassium (sodium) ions. The split alkali-ion positions in K3–xNa1+xM4(MoO4)6 (M = Ni, Mg, Co) give their structural formulae as [(K,Na)0.5□0.5)]6(Na)[M1][M2]3(MoO4)6, whereas the lithium-containing compound (K0.5□0.5)6(Mg0.89K0.11)(Li0.89Mg0.11)Mg3(MoO4)6 shows an unexpected (Mg, K) isomorphism, which is similar to (Mn, K) and (Co, K) substitutions in isostructural K3+xLi1–xM4(MoO4)6 (M = Mn, Co). The crystal chemistry of the title compounds and related arsenates, phosphates and molybdates was considered, and the connections of the cationic distributions with potential 3D ionic conductivity were shown by means of calculating the bond valence sum (BVS) maps for the Na+, Li+ and K+ ions. Electrical conductivity measurements gave relatively low values for the triple molybdates [σ = 4.8 × 10−6 S cm−1 at 390°C for K3NaCo4(MoO4)6 and 5 × 10−7 S cm−1 at 400°C for K3LiMg4(MoO4)6] compared with II-Na3Fe2(AsO4)3 (σ = 8.3 × 10−4 S cm−1 at 300°C). This may be explained by a low concentration of sodium or lithium ions and the blocking of their transport by large potassium ions.
Supporting information
CCDC references: 2021110; 2021111; 2021112; 2021113; 2021114; 2021115
For all structures, data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXL2017/1 (Sheldrick, 2017); program(s) used to refine structure: SHELXL2017/1 (Sheldrick, 2017); molecular graphics: DIAMOND (Brandenburg, 2008).
Crystal data top
K3NaNi4·6(MoO4) | Dx = 3.812 Mg m−3 |
Mr = 1334.77 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 9130 reflections |
a = 14.2790 (2) Å | θ = 2.6–31.1° |
c = 19.7589 (4) Å | µ = 6.94 mm−1 |
V = 3488.90 (12) Å3 | T = 296 K |
Z = 6 | Fragment, yellow |
F(000) = 3744 | 0.06 × 0.04 × 0.04 mm |
Data collection top
Bruker-Nonius X8 APEX CCD diffractometer | 1192 reflections with I > 2σ(I) |
\ f scans, frame data integration | Rint = 0.035 |
Absorption correction: multi-scan SADABS (Bruker, 2005) | θmax = 31.1°, θmin = 2.6° |
Tmin = 0.724, Tmax = 0.758 | h = −17→20 |
9130 measured reflections | k = −17→19 |
1256 independent reflections | l = −28→27 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.024 | w = 1/[σ2(Fo2) + (0.0077P)2 + 33.3386P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.051 | (Δ/σ)max = 0.008 |
S = 1.29 | Δρmax = 0.57 e Å−3 |
1257 reflections | Δρmin = −0.80 e Å−3 |
76 parameters | Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
7 restraints | Extinction coefficient: 0.000140 (14) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo | 0.18717 (2) | 0.00775 (2) | 0.35438 (2) | 0.01308 (8) | |
Ni1 | 0.000000 | 0.000000 | 0.250000 | 0.00923 (17) | |
Ni2 | 0.21298 (4) | 0.21298 (4) | 0.250000 | 0.01184 (12) | |
Na1 | 0.000000 | 0.000000 | 0.500000 | 0.0334 (9) | |
K1 | 0.2596 (3) | 0.2417 (2) | 0.4415 (2) | 0.0301 (7) | 0.4259 (14) |
K2 | 0.3037 (13) | 0.2613 (15) | 0.4267 (9) | 0.035 (5) | 0.0741 (14) |
O1 | 0.1564 (2) | 0.0291 (2) | 0.43533 (13) | 0.0325 (6) | |
O2 | 0.26368 (19) | −0.05718 (19) | 0.35748 (13) | 0.0224 (5) | |
O3 | 0.26770 (18) | 0.13297 (19) | 0.31356 (12) | 0.0207 (5) | |
O4 | 0.06282 (17) | −0.07414 (17) | 0.30770 (11) | 0.0141 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo | 0.01283 (13) | 0.01344 (13) | 0.01335 (12) | 0.00685 (10) | −0.00340 (8) | −0.00136 (8) |
Ni1 | 0.0081 (2) | 0.0081 (2) | 0.0116 (4) | 0.00403 (12) | 0.000 | 0.000 |
Ni2 | 0.00910 (18) | 0.00910 (18) | 0.0164 (2) | 0.00386 (19) | 0.00085 (9) | −0.00085 (9) |
Na1 | 0.0392 (14) | 0.0392 (14) | 0.0218 (18) | 0.0196 (7) | 0.000 | 0.000 |
K1 | 0.045 (2) | 0.0192 (12) | 0.0278 (13) | 0.0170 (14) | −0.0111 (13) | −0.0065 (9) |
K2 | 0.047 (16) | 0.021 (7) | 0.038 (16) | 0.018 (9) | −0.030 (12) | −0.016 (8) |
O1 | 0.0322 (15) | 0.0445 (17) | 0.0193 (12) | 0.0180 (13) | −0.0026 (10) | −0.0111 (11) |
O2 | 0.0190 (11) | 0.0167 (11) | 0.0342 (13) | 0.0109 (9) | −0.0079 (9) | 0.0019 (9) |
O3 | 0.0137 (10) | 0.0149 (10) | 0.0318 (12) | 0.0058 (9) | −0.0043 (9) | 0.0037 (9) |
O4 | 0.0142 (10) | 0.0127 (9) | 0.0171 (10) | 0.0080 (8) | −0.0036 (8) | −0.0004 (8) |
Geometric parameters (Å, º) top
Mo—O1 | 1.726 (3) | K1—K2 | 0.620 (17) |
Mo—O2 | 1.752 (2) | K1—K2xi | 1.45 (2) |
Mo—O3 | 1.765 (2) | K1—K1xi | 2.072 (6) |
Mo—O4 | 1.815 (2) | K1—O1 | 2.632 (4) |
Ni1—O4 | 2.043 (2) | K1—O2xii | 2.675 (5) |
Ni1—O4i | 2.043 (2) | K1—O3xi | 2.821 (5) |
Ni1—O4ii | 2.043 (2) | K1—O3xii | 2.871 (4) |
Ni1—O4iii | 2.043 (2) | K1—O1viii | 2.945 (4) |
Ni1—O4iv | 2.043 (2) | K1—O2vi | 2.958 (5) |
Ni1—O4v | 2.043 (2) | K1—O3 | 3.000 (5) |
Ni2—O2vi | 2.017 (2) | K1—O4i | 3.504 (5) |
Ni2—O2vii | 2.017 (2) | K1—O1i | 3.598 (5) |
Ni2—O4iv | 2.063 (2) | K2—K2xi | 0.83 (4) |
Ni2—O4i | 2.063 (2) | K2—O2xii | 2.612 (17) |
Ni2—O3iii | 2.094 (2) | K2—O3xi | 2.693 (18) |
Ni2—O3 | 2.094 (2) | K2—O2vi | 2.735 (18) |
Na1—O1viii | 2.422 (3) | K2—O3 | 2.772 (17) |
Na1—O1v | 2.422 (3) | K2—O1 | 2.910 (18) |
Na1—O1ix | 2.422 (3) | K2—O3xii | 3.171 (19) |
Na1—O1i | 2.422 (3) | K2—O1xi | 3.460 (19) |
Na1—O1x | 2.422 (3) | K2—O1viii | 3.499 (19) |
Na1—O1 | 2.422 (3) | | |
| | | |
O1—Mo—O2 | 110.03 (13) | K2—O1—K1ix | 99.3 (4) |
O1—Mo—O3 | 109.80 (13) | Mo—O1—K2xi | 83.4 (3) |
O2—Mo—O3 | 106.82 (11) | Na1—O1—K2xi | 119.1 (3) |
O1—Mo—O4 | 109.36 (12) | K1—O1—K2xi | 22.8 (3) |
O2—Mo—O4 | 110.17 (10) | K2—O1—K2xi | 11.4 (5) |
O3—Mo—O4 | 110.63 (10) | K1ix—O1—K2xi | 99.0 (3) |
O4—Ni1—O4i | 91.89 (8) | Mo—O1—K2ix | 119.1 (3) |
O4—Ni1—O4ii | 84.94 (12) | Na1—O1—K2ix | 91.8 (3) |
O4i—Ni1—O4ii | 175.47 (12) | K1—O1—K2ix | 103.1 (4) |
O4—Ni1—O4iii | 175.47 (12) | K2—O1—K2ix | 101.9 (3) |
O4i—Ni1—O4iii | 91.45 (12) | K1ix—O1—K2ix | 4.9 (3) |
O4ii—Ni1—O4iii | 91.89 (8) | K2xi—O1—K2ix | 100.7 (3) |
O4—Ni1—O4iv | 91.45 (12) | Mo—O1—K1v | 85.42 (12) |
O4i—Ni1—O4iv | 84.94 (12) | Na1—O1—K1v | 74.64 (9) |
O4ii—Ni1—O4iv | 91.89 (8) | K1—O1—K1v | 170.94 (13) |
O4iii—Ni1—O4iv | 91.89 (8) | K2—O1—K1v | 177.6 (4) |
O4—Ni1—O4v | 91.89 (8) | K1ix—O1—K1v | 80.72 (11) |
O4i—Ni1—O4v | 91.89 (8) | K2xi—O1—K1v | 166.2 (4) |
O4ii—Ni1—O4v | 91.45 (12) | K2ix—O1—K1v | 77.9 (3) |
O4iii—Ni1—O4v | 84.94 (12) | Mo—O1—K1xi | 78.62 (11) |
O4iv—Ni1—O4v | 175.47 (12) | Na1—O1—K1xi | 124.94 (11) |
O2vi—Ni2—O2vii | 92.13 (14) | K1—O1—K1xi | 28.63 (9) |
O2vi—Ni2—O4iv | 175.65 (9) | K2—O1—K1xi | 17.2 (4) |
O2vii—Ni2—O4iv | 91.99 (9) | K1ix—O1—K1xi | 98.72 (10) |
O2vi—Ni2—O4i | 91.99 (9) | K2xi—O1—K1xi | 5.8 (3) |
O2vii—Ni2—O4i | 175.65 (9) | K2ix—O1—K1xi | 100.0 (3) |
O4iv—Ni2—O4i | 83.93 (11) | K1v—O1—K1xi | 160.42 (8) |
O2vi—Ni2—O3iii | 93.89 (10) | Mo—O1—K2v | 81.3 (3) |
O2vii—Ni2—O3iii | 92.97 (10) | Na1—O1—K2v | 77.3 (3) |
O4iv—Ni2—O3iii | 84.49 (9) | K1—O1—K2v | 172.6 (3) |
O4i—Ni2—O3iii | 88.15 (9) | K2—O1—K2v | 173.8 (6) |
O2vi—Ni2—O3 | 92.97 (10) | K1ix—O1—K2v | 84.1 (3) |
O2vii—Ni2—O3 | 93.89 (10) | K2xi—O1—K2v | 163.18 (13) |
O4iv—Ni2—O3 | 88.15 (9) | K2ix—O1—K2v | 81.1 (3) |
O4i—Ni2—O3 | 84.49 (9) | K1v—O1—K2v | 4.3 (3) |
O3iii—Ni2—O3 | 170.10 (13) | K1xi—O1—K2v | 157.5 (3) |
O1viii—Na1—O1v | 180.00 (13) | Mo—O2—Ni2xiii | 146.55 (16) |
O1viii—Na1—O1ix | 94.73 (9) | Mo—O2—K2xiv | 105.2 (4) |
O1v—Na1—O1ix | 85.27 (9) | Ni2xiii—O2—K2xiv | 101.6 (4) |
O1viii—Na1—O1i | 85.27 (9) | Mo—O2—K1xiv | 98.95 (12) |
O1v—Na1—O1i | 94.73 (9) | Ni2xiii—O2—K1xiv | 102.81 (12) |
O1ix—Na1—O1i | 180.00 (10) | K2xiv—O2—K1xiv | 13.4 (4) |
O1viii—Na1—O1x | 94.73 (9) | Mo—O2—K2xiii | 111.6 (4) |
O1v—Na1—O1x | 85.27 (9) | Ni2xiii—O2—K2xiii | 100.0 (4) |
O1ix—Na1—O1x | 94.73 (9) | K2xiv—O2—K2xiii | 17.8 (8) |
O1i—Na1—O1x | 85.27 (9) | K1xiv—O2—K2xiii | 31.1 (4) |
O1viii—Na1—O1 | 85.27 (9) | Mo—O2—K1xiii | 114.31 (13) |
O1v—Na1—O1 | 94.73 (9) | Ni2xiii—O2—K1xiii | 98.87 (12) |
O1ix—Na1—O1 | 85.27 (9) | K2xiv—O2—K1xiii | 29.4 (4) |
O1i—Na1—O1 | 94.73 (9) | K1xiv—O2—K1xiii | 42.79 (12) |
O1x—Na1—O1 | 180.0 | K2xiii—O2—K1xiii | 11.7 (4) |
O1—K1—O2xii | 140.20 (18) | Mo—O2—K1v | 74.13 (9) |
O1—K1—O3xi | 79.80 (12) | Ni2xiii—O2—K1v | 88.75 (10) |
O2xii—K1—O3xi | 65.65 (12) | K2xiv—O2—K1v | 156.7 (4) |
O1—K1—O3xii | 134.48 (14) | K1xiv—O2—K1v | 166.35 (14) |
O2xii—K1—O3xii | 61.09 (10) | K2xiii—O2—K1v | 140.3 (4) |
O3xi—K1—O3xii | 122.73 (15) | K1xiii—O2—K1v | 128.91 (10) |
O1—K1—O1viii | 71.83 (13) | Mo—O2—K1ix | 81.30 (10) |
O2xii—K1—O1viii | 83.08 (13) | Ni2xiii—O2—K1ix | 65.33 (8) |
O3xi—K1—O1viii | 80.42 (13) | K2xiv—O2—K1ix | 138.8 (4) |
O3xii—K1—O1viii | 74.01 (10) | K1xiv—O2—K1ix | 126.98 (11) |
O1—K1—O2vi | 113.36 (17) | K2xiii—O2—K1ix | 153.4 (4) |
O2xii—K1—O2vi | 105.12 (13) | K1xiii—O2—K1ix | 160.76 (10) |
O3xi—K1—O2vi | 134.93 (13) | K1v—O2—K1ix | 64.42 (7) |
O3xii—K1—O2vi | 79.82 (11) | Mo—O3—Ni2 | 126.52 (12) |
O1viii—K1—O2vi | 144.27 (15) | Mo—O3—K2xi | 109.7 (4) |
O1—K1—O3 | 60.53 (10) | Ni2—O3—K2xi | 97.0 (4) |
O2xii—K1—O3 | 140.23 (13) | Mo—O3—K2 | 96.5 (4) |
O3xi—K1—O3 | 97.76 (12) | Ni2—O3—K2 | 96.9 (4) |
O3xii—K1—O3 | 137.07 (17) | K2xi—O3—K2 | 17.5 (8) |
O1viii—K1—O3 | 131.70 (13) | Mo—O3—K1xi | 119.13 (13) |
O2vi—K1—O3 | 60.06 (10) | Ni2—O3—K1xi | 96.21 (11) |
O1—K1—O4i | 66.73 (11) | K2xi—O3—K1xi | 12.6 (4) |
O2xii—K1—O4i | 151.82 (14) | K2—O3—K1xi | 30.1 (4) |
O3xi—K1—O4i | 141.77 (13) | Mo—O3—K1xiv | 91.87 (12) |
O3xii—K1—O4i | 94.57 (12) | Ni2—O3—K1xiv | 124.13 (14) |
O1viii—K1—O4i | 104.80 (11) | K2xi—O3—K1xiv | 106.7 (4) |
O2vi—K1—O4i | 53.21 (9) | K2—O3—K1xiv | 119.7 (3) |
O3—K1—O4i | 50.17 (9) | K1xi—O3—K1xiv | 97.10 (13) |
O1—K1—O1i | 67.74 (13) | Mo—O3—K1 | 87.99 (11) |
O2xii—K1—O1i | 124.09 (13) | Ni2—O3—K1 | 95.83 (11) |
O3xi—K1—O1i | 133.86 (12) | K2xi—O3—K1 | 28.9 (4) |
O3xii—K1—O1i | 69.24 (9) | K2—O3—K1 | 11.5 (4) |
O1viii—K1—O1i | 59.19 (10) | K1xi—O3—K1 | 41.56 (11) |
O2vi—K1—O1i | 89.07 (12) | K1xiv—O3—K1 | 127.98 (15) |
O3—K1—O1i | 93.92 (12) | Mo—O3—K2xiv | 85.5 (3) |
O4i—K1—O1i | 48.00 (8) | Ni2—O3—K2xiv | 122.8 (3) |
O2xii—K2—O3xi | 68.4 (4) | K2xi—O3—K2xiv | 116.5 (7) |
O2xii—K2—O2vi | 113.7 (7) | K2—O3—K2xiv | 128.6 (5) |
O3xi—K2—O2vi | 159.1 (8) | K1xi—O3—K2xiv | 107.3 (3) |
O2xii—K2—O3 | 164.9 (8) | K1xiv—O3—K2xiv | 10.3 (3) |
O3xi—K2—O3 | 106.8 (7) | K1—O3—K2xiv | 135.7 (3) |
O2vi—K2—O3 | 65.6 (4) | Mo—O3—K2xiii | 78.9 (3) |
O2xii—K2—O1 | 129.2 (7) | Ni2—O3—K2xiii | 119.8 (3) |
O3xi—K2—O1 | 77.2 (5) | K2xi—O3—K2xiii | 127.2 (5) |
O2vi—K2—O1 | 111.8 (5) | K2—O3—K2xiii | 137.8 (6) |
O3—K2—O1 | 60.3 (4) | K1xi—O3—K2xiii | 118.4 (3) |
O2xii—K2—O3xii | 57.5 (4) | K1xiv—O3—K2xiii | 21.6 (3) |
O3xi—K2—O3xii | 116.6 (6) | K1—O3—K2xiii | 143.0 (3) |
O2vi—K2—O3xii | 78.2 (5) | K2xiv—O3—K2xiii | 11.3 (5) |
O3—K2—O3xii | 133.5 (6) | Mo—O3—K1xiii | 75.00 (10) |
O1—K2—O3xii | 113.1 (6) | Ni2—O3—K1xiii | 117.44 (11) |
O2xii—K2—O1xi | 99.7 (5) | K2xi—O3—K1xiii | 133.6 (3) |
O3xi—K2—O1xi | 53.6 (3) | K2—O3—K1xiii | 142.9 (4) |
O2vi—K2—O1xi | 106.7 (6) | K1xi—O3—K1xiii | 125.14 (11) |
O3—K2—O1xi | 67.3 (4) | K1xiv—O3—K1xiii | 28.34 (9) |
O1—K2—O1xi | 87.8 (5) | K1—O3—K1xiii | 146.60 (10) |
O3xii—K2—O1xi | 155.5 (5) | K2xiv—O3—K1xiii | 18.0 (4) |
O2xii—K2—O1viii | 73.7 (4) | K2xiii—O3—K1xiii | 6.8 (3) |
O3xi—K2—O1viii | 72.6 (4) | Mo—O4—Ni1 | 119.42 (11) |
O2vi—K2—O1viii | 128.2 (6) | Mo—O4—Ni2v | 135.65 (11) |
O3—K2—O1viii | 119.3 (6) | Ni1—O4—Ni2v | 95.56 (9) |
O1—K2—O1viii | 60.8 (4) | Mo—O4—K1v | 87.10 (9) |
O3xii—K2—O1viii | 63.1 (3) | Ni1—O4—K1v | 138.49 (10) |
O1xi—K2—O1viii | 122.9 (5) | Ni2v—O4—K1v | 82.54 (8) |
Mo—O1—Na1 | 138.85 (15) | Mo—O4—K2v | 94.6 (3) |
Mo—O1—K1 | 101.66 (15) | Ni1—O4—K2v | 136.6 (3) |
Na1—O1—K1 | 96.31 (12) | Ni2v—O4—K2v | 73.2 (3) |
Mo—O1—K2 | 92.6 (4) | K1v—O4—K2v | 9.4 (3) |
Na1—O1—K2 | 107.8 (4) | Mo—O4—K2xv | 102.9 (3) |
K1—O1—K2 | 11.5 (4) | Ni1—O4—K2xv | 133.2 (3) |
Mo—O1—K1ix | 123.68 (16) | Ni2v—O4—K2xv | 62.2 (3) |
Na1—O1—K1ix | 88.62 (11) | K1v—O4—K2xv | 20.4 (3) |
K1—O1—K1ix | 99.65 (11) | K2v—O4—K2xv | 11.0 (6) |
Symmetry codes: (i) −y, x−y, z; (ii) −x, −x+y, −z+1/2; (iii) y, x, −z+1/2; (iv) x−y, −y, −z+1/2; (v) −x+y, −x, z; (vi) y+1/3, −x+y+2/3, −z+2/3; (vii) −x+y+2/3, y+1/3, z−1/6; (viii) x−y, x, −z+1; (ix) y, −x+y, −z+1; (x) −x, −y, −z+1; (xi) −x+2/3, −x+y+1/3, −z+5/6; (xii) −y+1/3, −x+2/3, z+1/6; (xiii) x−y+1/3, x−1/3, −z+2/3; (xiv) −y+2/3, −x+1/3, z−1/6; (xv) y−1/3, x−2/3, −z+5/6. |
Crystal data top
K2.51Na1.49Ni4·6(MoO4) | Dx = 3.784 Mg m−3 |
Mr = 1326.84 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 13749 reflections |
a = 14.2719 (2) Å | θ = 2.6–2.7° |
c = 19.8063 (4) Å | µ = 6.85 mm−1 |
V = 3493.80 (14) Å3 | T = 296 K |
Z = 6 | Fragment, yellow |
F(000) = 3721 | 0.07 × 0.07 × 0.06 mm |
Data collection top
Bruker-Nonius X8 APEX CCD diffractometer | 1062 reflections with I > 2σ(I) |
\ f scans, frame data integration | Rint = 0.027 |
Absorption correction: multi-scan SADABS (Bruker, 2005) | θmax = 29.7°, θmin = 2.6° |
Tmin = 0.625, Tmax = 0.663 | h = −19→19 |
13749 measured reflections | k = −19→19 |
1111 independent reflections | l = −27→27 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.014 | w = 1/[σ2(Fo2) + (0.0124P)2 + 12.1272P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.033 | (Δ/σ)max = 0.025 |
S = 1.16 | Δρmax = 0.67 e Å−3 |
1106 reflections | Δρmin = −0.43 e Å−3 |
86 parameters | Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
7 restraints | Extinction coefficient: 0.000093 (12) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo | 0.18781 (2) | 0.00850 (2) | 0.35417 (2) | 0.01230 (6) | |
Ni1 | 0.000000 | 0.000000 | 0.250000 | 0.00785 (11) | |
Ni2 | 0.21317 (2) | 0.21317 (2) | 0.250000 | 0.01112 (8) | |
Na1 | 0.000000 | 0.000000 | 0.500000 | 0.0341 (5) | |
K1 | 0.2579 (5) | 0.2401 (6) | 0.4432 (6) | 0.0253 (10) | 0.2611 (16) |
K2 | 0.2791 (12) | 0.2517 (12) | 0.4342 (10) | 0.063 (5) | 0.1578 (16) |
Na2 | 0.249 (2) | 0.2275 (17) | 0.4731 (10) | 0.043 (5) | 0.0810 (16) |
O1 | 0.15739 (15) | 0.03009 (16) | 0.43513 (9) | 0.0355 (4) | |
O2 | 0.26437 (12) | −0.05662 (12) | 0.35708 (9) | 0.0236 (3) | |
O3 | 0.26868 (12) | 0.13385 (12) | 0.31374 (8) | 0.0220 (3) | |
O4 | 0.06333 (11) | −0.07385 (11) | 0.30776 (7) | 0.0136 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo | 0.01203 (8) | 0.01256 (8) | 0.01260 (9) | 0.00636 (6) | −0.00403 (5) | −0.00181 (5) |
Ni1 | 0.00661 (14) | 0.00661 (14) | 0.0103 (3) | 0.00331 (7) | 0.000 | 0.000 |
Ni2 | 0.00843 (11) | 0.00843 (11) | 0.01552 (17) | 0.00348 (12) | 0.00094 (6) | −0.00094 (6) |
Na1 | 0.0392 (8) | 0.0392 (8) | 0.0241 (12) | 0.0196 (4) | 0.000 | 0.000 |
K1 | 0.0359 (14) | 0.0168 (14) | 0.024 (2) | 0.0137 (11) | −0.0049 (16) | −0.0058 (16) |
K2 | 0.128 (12) | 0.034 (5) | 0.040 (9) | 0.052 (7) | −0.051 (9) | −0.021 (5) |
Na2 | 0.062 (11) | 0.044 (10) | 0.018 (8) | 0.023 (9) | 0.002 (10) | −0.014 (8) |
O1 | 0.0328 (9) | 0.0511 (11) | 0.0188 (8) | 0.0180 (9) | −0.0023 (7) | −0.0130 (8) |
O2 | 0.0207 (7) | 0.0183 (7) | 0.0343 (9) | 0.0116 (6) | −0.0100 (6) | 0.0003 (6) |
O3 | 0.0149 (6) | 0.0165 (7) | 0.0325 (8) | 0.0064 (6) | −0.0050 (6) | 0.0041 (6) |
O4 | 0.0138 (6) | 0.0120 (6) | 0.0164 (7) | 0.0075 (5) | −0.0048 (5) | −0.0015 (5) |
Geometric parameters (Å, º) top
Mo—O1 | 1.7287 (17) | K1—O3xii | 2.862 (8) |
Mo—O2 | 1.7539 (15) | K1—O1ix | 2.912 (9) |
Mo—O3 | 1.7633 (15) | K1—O2vi | 2.989 (12) |
Mo—O4 | 1.8150 (13) | K1—O3 | 3.021 (11) |
Ni1—O4i | 2.0468 (13) | K1—O4i | 3.520 (12) |
Ni1—O4ii | 2.0468 (13) | K1—O1i | 3.591 (7) |
Ni1—O4iii | 2.0468 (13) | K2—Na2 | 0.86 (3) |
Ni1—O4iv | 2.0468 (13) | K2—K2xi | 1.51 (3) |
Ni1—O4v | 2.0468 (13) | K2—Na2xi | 2.26 (3) |
Ni1—O4 | 2.0468 (13) | K2—O2xii | 2.620 (18) |
Ni2—O2vi | 2.0190 (15) | K2—O1 | 2.744 (15) |
Ni2—O2vii | 2.0190 (15) | K2—O3xi | 2.757 (17) |
Ni2—O4iv | 2.0693 (13) | K2—O2vi | 2.818 (19) |
Ni2—O4i | 2.0693 (13) | K2—O3 | 2.881 (19) |
Ni2—O3iii | 2.0975 (15) | K2—O3xii | 2.976 (16) |
Ni2—O3 | 2.0975 (15) | K2—O1ix | 3.207 (19) |
Na1—O1viii | 2.4323 (18) | K2—O4i | 3.569 (17) |
Na1—O1i | 2.4323 (18) | K2—O1xi | 3.724 (15) |
Na1—O1ix | 2.4324 (18) | K2—O1i | 3.846 (14) |
Na1—O1v | 2.4324 (18) | Na2—O1ix | 2.37 (2) |
Na1—O1 | 2.4324 (18) | Na2—O2xii | 2.50 (2) |
Na1—O1x | 2.4324 (18) | Na2—O3xi | 2.53 (3) |
K1—K2 | 0.32 (2) | Na2—O1 | 2.555 (19) |
K1—Na2 | 0.61 (2) | Na2—O3xii | 2.86 (2) |
K1—K2xi | 1.824 (13) | Na2—Na2xi | 3.05 (5) |
K1—K1xi | 2.139 (13) | Na2—O2ix | 3.48 (2) |
K1—Na2xi | 2.57 (3) | Na2—O3 | 3.493 (18) |
K1—O1 | 2.602 (8) | Na2—O1i | 3.58 (3) |
K1—O2xii | 2.663 (11) | Na2—O2vi | 3.58 (2) |
K1—O3xi | 2.798 (11) | | |
| | | |
O1—Mo—O2 | 110.03 (9) | Na1—O1—K2viii | 89.9 (3) |
O1—Mo—O3 | 109.61 (9) | Na2—O1—K2viii | 89.7 (6) |
O2—Mo—O3 | 106.70 (7) | K1—O1—K2viii | 100.7 (5) |
O1—Mo—O4 | 109.48 (7) | K2—O1—K2viii | 101.3 (3) |
O2—Mo—O4 | 109.93 (6) | K1viii—O1—K2viii | 2.1 (5) |
O3—Mo—O4 | 111.05 (7) | Mo—O1—Na2v | 95.7 (4) |
O4i—Ni1—O4ii | 175.80 (8) | Na2viii—O1—Na2v | 70.6 (5) |
O4i—Ni1—O4iii | 91.29 (8) | Na1—O1—Na2v | 67.0 (4) |
O4ii—Ni1—O4iii | 91.80 (5) | Na2—O1—Na2v | 148.6 (8) |
O4i—Ni1—O4iv | 85.26 (7) | K1—O1—Na2v | 161.1 (5) |
O4ii—Ni1—O4iv | 91.80 (5) | K2—O1—Na2v | 166.8 (6) |
O4iii—Ni1—O4iv | 91.80 (5) | K1viii—O1—Na2v | 73.3 (3) |
O4i—Ni1—O4v | 91.80 (5) | K2viii—O1—Na2v | 72.7 (4) |
O4ii—Ni1—O4v | 91.29 (8) | Mo—O1—K1v | 86.0 (2) |
O4iii—Ni1—O4v | 85.26 (7) | Na2viii—O1—K1v | 76.6 (6) |
O4iv—Ni1—O4v | 175.80 (8) | Na1—O1—K1v | 73.84 (16) |
O4i—Ni1—O4 | 91.80 (5) | Na2—O1—K1v | 158.3 (6) |
O4ii—Ni1—O4 | 85.26 (7) | K1—O1—K1v | 169.5 (3) |
O4iii—Ni1—O4 | 175.80 (8) | K2—O1—K1v | 175.6 (4) |
O4iv—Ni1—O4 | 91.29 (8) | K1viii—O1—K1v | 80.0 (2) |
O4v—Ni1—O4 | 91.80 (5) | K2viii—O1—K1v | 79.2 (4) |
O2vi—Ni2—O2vii | 92.27 (9) | Na2v—O1—K1v | 9.8 (3) |
O2vi—Ni2—O4iv | 175.80 (6) | Mo—O1—K2xi | 81.0 (3) |
O2vii—Ni2—O4iv | 91.81 (6) | Na2viii—O1—K2xi | 101.0 (7) |
O2vi—Ni2—O4i | 91.81 (6) | Na1—O1—K2xi | 122.4 (3) |
O2vii—Ni2—O4i | 175.80 (6) | Na2—O1—K2xi | 36.4 (5) |
O4iv—Ni2—O4i | 84.12 (7) | K1—O1—K2xi | 26.7 (3) |
O2vi—Ni2—O3iii | 94.16 (6) | K2—O1—K2xi | 20.7 (5) |
O2vii—Ni2—O3iii | 92.28 (7) | K1viii—O1—K2xi | 99.2 (4) |
O4iv—Ni2—O3iii | 84.70 (6) | K2viii—O1—K2xi | 99.4 (3) |
O4i—Ni2—O3iii | 88.40 (6) | Na2v—O1—K2xi | 168.4 (4) |
O2vi—Ni2—O3 | 92.28 (7) | K1v—O1—K2xi | 163.7 (4) |
O2vii—Ni2—O3 | 94.16 (6) | Mo—O1—K2v | 83.1 (3) |
O4iv—Ni2—O3 | 88.40 (6) | Na2viii—O1—K2v | 78.4 (8) |
O4i—Ni2—O3 | 84.70 (6) | Na1—O1—K2v | 75.9 (3) |
O3iii—Ni2—O3 | 170.71 (8) | Na2—O1—K2v | 161.1 (5) |
O1viii—Na1—O1i | 180.00 (7) | K1—O1—K2v | 171.5 (3) |
O1viii—Na1—O1ix | 94.67 (6) | K2—O1—K2v | 176.8 (3) |
O1i—Na1—O1ix | 85.33 (6) | K1viii—O1—K2v | 82.0 (3) |
O1viii—Na1—O1v | 85.33 (6) | K2viii—O1—K2v | 81.1 (3) |
O1i—Na1—O1v | 94.67 (6) | Na2v—O1—K2v | 12.7 (5) |
O1ix—Na1—O1v | 180.00 (8) | K1v—O1—K2v | 2.9 (5) |
O1viii—Na1—O1 | 85.33 (6) | K2xi—O1—K2v | 161.54 (9) |
O1i—Na1—O1 | 94.67 (6) | Mo—O2—Ni2xiii | 146.10 (11) |
O1ix—Na1—O1 | 85.33 (6) | Mo—O2—Na2xiv | 101.4 (6) |
O1v—Na1—O1 | 94.67 (6) | Ni2xiii—O2—Na2xiv | 94.6 (6) |
O1viii—Na1—O1x | 94.67 (6) | Mo—O2—K2xiv | 101.4 (3) |
O1i—Na1—O1x | 85.33 (6) | Ni2xiii—O2—K2xiv | 103.3 (4) |
O1ix—Na1—O1x | 94.67 (6) | Na2xiv—O2—K2xiv | 19.2 (7) |
O1v—Na1—O1x | 85.33 (6) | Mo—O2—K1xiv | 99.00 (18) |
O1—Na1—O1x | 180.0 | Ni2xiii—O2—K1xiv | 102.8 (2) |
O1—K1—O2xii | 141.3 (5) | Na2xiv—O2—K1xiv | 13.2 (5) |
O1—K1—O3xi | 80.2 (2) | K2xiv—O2—K1xiv | 6.8 (5) |
O2xii—K1—O3xi | 65.8 (3) | Mo—O2—K2xiii | 113.2 (3) |
O1—K1—O3xii | 135.5 (2) | Ni2xiii—O2—K2xiii | 100.0 (3) |
O2xii—K1—O3xii | 61.3 (2) | Na2xiv—O2—K2xiii | 49.7 (6) |
O3xi—K1—O3xii | 123.2 (4) | K2xiv—O2—K2xiii | 32.0 (6) |
O1—K1—O1ix | 73.2 (2) | K1xiv—O2—K2xiii | 38.8 (3) |
O2xii—K1—O1ix | 83.5 (3) | Mo—O2—K1xiii | 114.46 (19) |
O3xi—K1—O1ix | 81.2 (3) | Ni2xiii—O2—K1xiii | 99.22 (19) |
O3xii—K1—O1ix | 74.1 (2) | Na2xiv—O2—K1xiii | 54.9 (5) |
O1—K1—O2vi | 112.7 (4) | K2xiv—O2—K1xiii | 37.2 (4) |
O2xii—K1—O2vi | 104.3 (2) | K1xiv—O2—K1xiii | 44.0 (2) |
O3xi—K1—O2vi | 133.8 (2) | K2xiii—O2—K1xiii | 5.2 (4) |
O3xii—K1—O2vi | 79.6 (2) | Mo—O2—Na2viii | 77.1 (4) |
O1ix—K1—O2vi | 144.6 (3) | Ni2xiii—O2—Na2viii | 69.0 (5) |
O1—K1—O3 | 60.4 (2) | Na2xiv—O2—Na2viii | 115.8 (6) |
O2xii—K1—O3 | 138.9 (2) | K2xiv—O2—Na2viii | 134.8 (5) |
O3xi—K1—O3 | 97.6 (2) | K1xiv—O2—Na2viii | 128.2 (4) |
O3xii—K1—O3 | 136.2 (4) | K2xiii—O2—Na2viii | 162.4 (5) |
O1ix—K1—O3 | 133.0 (3) | K1xiii—O2—Na2viii | 165.4 (5) |
O2vi—K1—O3 | 59.2 (2) | Mo—O2—Na2xiii | 112.5 (3) |
O1—K1—O4i | 66.8 (2) | Ni2xiii—O2—Na2xiii | 101.3 (3) |
O2xii—K1—O4i | 151.1 (3) | Na2xiv—O2—Na2xiii | 56.9 (9) |
O3xi—K1—O4i | 141.9 (3) | K2xiv—O2—Na2xiii | 38.9 (4) |
O3xii—K1—O4i | 94.3 (3) | K1xiv—O2—Na2xiii | 45.7 (6) |
O1ix—K1—O4i | 105.6 (2) | K2xiii—O2—Na2xiii | 7.3 (6) |
O2vi—K1—O4i | 52.9 (2) | K1xiii—O2—Na2xiii | 2.8 (3) |
O3—K1—O4i | 50.12 (19) | Na2viii—O2—Na2xiii | 168.2 (5) |
O1—K1—O1i | 68.43 (17) | Mo—O2—K1v | 73.91 (13) |
O2xii—K1—O1i | 124.8 (3) | Ni2xiii—O2—K1v | 88.27 (15) |
O3xi—K1—O1i | 135.1 (3) | Na2xiv—O2—K1v | 174.7 (6) |
O3xii—K1—O1i | 69.25 (14) | K2xiv—O2—K1v | 162.8 (3) |
O1ix—K1—O1i | 59.84 (12) | K1xiv—O2—K1v | 167.4 (3) |
O2vi—K1—O1i | 88.9 (3) | K2xiii—O2—K1v | 134.1 (4) |
O3—K1—O1i | 94.1 (3) | K1xiii—O2—K1v | 129.05 (16) |
O4i—K1—O1i | 48.02 (13) | Na2viii—O2—K1v | 61.2 (4) |
O2xii—K2—O1 | 135.7 (8) | Na2xiii—O2—K1v | 126.9 (4) |
O2xii—K2—O3xi | 67.0 (4) | Mo—O2—K1viii | 80.82 (10) |
O1—K2—O3xi | 78.5 (4) | Ni2xiii—O2—K1viii | 65.36 (9) |
O2xii—K2—O2vi | 110.4 (5) | Na2xiv—O2—K1viii | 113.7 (5) |
O1—K2—O2vi | 113.8 (6) | K2xiv—O2—K1viii | 133.0 (4) |
O3xi—K2—O2vi | 145.5 (6) | K1xiv—O2—K1viii | 126.5 (2) |
O2xii—K2—O3 | 150.9 (6) | K2xiii—O2—K1viii | 158.8 (4) |
O1—K2—O3 | 60.9 (4) | K1xiii—O2—K1viii | 161.47 (14) |
O3xi—K2—O3 | 101.9 (5) | Na2viii—O2—K1viii | 4.0 (4) |
O2vi—K2—O3 | 62.8 (4) | Na2xiii—O2—K1viii | 164.2 (3) |
O2xii—K2—O3xii | 60.2 (4) | K1v—O2—K1viii | 63.47 (18) |
O1—K2—O3xii | 124.3 (5) | Mo—O2—K2v | 76.1 (2) |
O3xi—K2—O3xii | 120.5 (7) | Ni2xiii—O2—K2v | 88.2 (3) |
O2vi—K2—O3xii | 80.5 (4) | Na2xiv—O2—K2v | 177.2 (7) |
O3—K2—O3xii | 137.5 (6) | K2xiv—O2—K2v | 159.4 (6) |
O2xii—K2—O1ix | 78.6 (5) | K1xiv—O2—K2v | 165.0 (2) |
O1—K2—O1ix | 66.8 (4) | K2xiii—O2—K2v | 129.9 (2) |
O3xi—K2—O1ix | 76.7 (5) | K1xiii—O2—K2v | 124.8 (3) |
O2vi—K2—O1ix | 137.8 (5) | Na2viii—O2—K2v | 65.1 (5) |
O3—K2—O1ix | 126.6 (5) | Na2xiii—O2—K2v | 122.7 (6) |
O3xii—K2—O1ix | 68.4 (4) | K1v—O2—K2v | 4.3 (3) |
O2xii—K2—O4i | 150.6 (6) | K1viii—O2—K2v | 67.3 (3) |
O1—K2—O4i | 64.8 (3) | Mo—O3—Ni2 | 126.06 (8) |
O3xi—K2—O4i | 141.4 (5) | Mo—O3—Na2xi | 130.3 (4) |
O2vi—K2—O4i | 53.2 (3) | Ni2—O3—Na2xi | 91.8 (4) |
O3—K2—O4i | 50.2 (3) | Mo—O3—K2xi | 115.1 (4) |
O3xii—K2—O4i | 91.3 (4) | Ni2—O3—K2xi | 96.8 (4) |
O1ix—K2—O4i | 98.4 (4) | Na2xi—O3—K2xi | 18.2 (7) |
O2xii—K2—O1xi | 92.8 (4) | Mo—O3—K1xi | 119.8 (2) |
O1—K2—O1xi | 84.5 (4) | Ni2—O3—K1xi | 96.5 (2) |
O3xi—K2—O1xi | 49.5 (2) | Na2xi—O3—K1xi | 11.9 (4) |
O2vi—K2—O1xi | 97.9 (5) | K2xi—O3—K1xi | 6.5 (5) |
O3—K2—O1xi | 62.1 (3) | Mo—O3—Na2xiv | 88.7 (5) |
O3xii—K2—O1xi | 149.5 (5) | Ni2—O3—Na2xiv | 134.6 (4) |
O1ix—K2—O1xi | 123.4 (5) | Na2xi—O3—Na2xiv | 82.9 (10) |
O4i—K2—O1xi | 112.3 (5) | K2xi—O3—Na2xiv | 91.8 (6) |
O2xii—K2—O1i | 117.3 (6) | K1xi—O3—Na2xiv | 87.4 (5) |
O1—K2—O1i | 63.2 (3) | Mo—O3—K1xiv | 91.9 (2) |
O3xi—K2—O1i | 126.3 (6) | Ni2—O3—K1xiv | 124.5 (3) |
O2vi—K2—O1i | 86.5 (4) | Na2xi—O3—K1xiv | 89.9 (6) |
O3—K2—O1i | 91.2 (4) | K2xi—O3—K1xiv | 101.2 (3) |
O3xii—K2—O1i | 64.5 (3) | K1xi—O3—K1xiv | 96.2 (3) |
O1ix—K2—O1i | 54.8 (2) | Na2xiv—O3—K1xiv | 12.3 (4) |
O4i—K2—O1i | 45.75 (18) | Mo—O3—K2 | 91.9 (3) |
O1xi—K2—O1i | 146.0 (5) | Ni2—O3—K2 | 96.1 (3) |
O1ix—Na2—O2xii | 99.7 (6) | Na2xi—O3—K2 | 48.7 (6) |
O1ix—Na2—O3xi | 98.7 (8) | K2xi—O3—K2 | 31.0 (6) |
O2xii—Na2—O3xi | 72.4 (7) | K1xi—O3—K2 | 37.4 (3) |
O1ix—Na2—O1 | 84.0 (7) | Na2xiv—O3—K2 | 112.6 (5) |
O2xii—Na2—O1 | 158.7 (12) | K1xiv—O3—K2 | 124.4 (3) |
O3xi—Na2—O1 | 86.4 (7) | Mo—O3—K2xiv | 88.9 (3) |
O1ix—Na2—O3xii | 82.9 (7) | Ni2—O3—K2xiv | 123.2 (4) |
O2xii—Na2—O3xii | 63.1 (4) | Na2xi—O3—K2xiv | 95.6 (6) |
O3xi—Na2—O3xii | 135.0 (8) | K2xi—O3—K2xiv | 107.0 (6) |
O1—Na2—O3xii | 138.0 (11) | K1xi—O3—K2xiv | 102.0 (3) |
O1ix—Na2—O2ix | 54.5 (4) | Na2xiv—O3—K2xiv | 16.9 (6) |
O2xii—Na2—O2ix | 55.4 (4) | K1xiv—O3—K2xiv | 5.8 (4) |
O3xi—Na2—O2ix | 57.7 (4) | K2—O3—K2xiv | 129.5 (5) |
O1—Na2—O2ix | 113.7 (8) | Mo—O3—K1 | 87.27 (16) |
O3xii—Na2—O2ix | 90.1 (4) | Ni2—O3—K1 | 96.4 (2) |
O1ix—Na2—O3 | 135.6 (8) | Na2xi—O3—K1 | 54.2 (6) |
O2xii—Na2—O3 | 124.5 (9) | K2xi—O3—K1 | 36.4 (3) |
O3xi—Na2—O3 | 91.9 (6) | K1xi—O3—K1 | 42.9 (2) |
O1—Na2—O3 | 53.6 (3) | Na2xiv—O3—K1 | 115.5 (5) |
O3xii—Na2—O3 | 118.2 (7) | K1xiv—O3—K1 | 127.6 (4) |
O2ix—Na2—O3 | 149.2 (8) | K2—O3—K1 | 5.5 (4) |
O1ix—Na2—O1i | 63.6 (6) | K2xiv—O3—K1 | 132.4 (3) |
O2xii—Na2—O1i | 131.4 (8) | Mo—O3—Na2 | 80.8 (4) |
O3xi—Na2—O1i | 150.4 (8) | Ni2—O3—Na2 | 102.4 (4) |
O1—Na2—O1i | 69.0 (6) | Na2xi—O3—Na2 | 58.3 (9) |
O3xii—Na2—O1i | 69.4 (6) | K2xi—O3—Na2 | 40.2 (4) |
O2ix—Na2—O1i | 116.6 (7) | K1xi—O3—Na2 | 46.6 (5) |
O3—Na2—O1i | 86.7 (5) | Na2xiv—O3—Na2 | 112.4 (6) |
O1ix—Na2—O2vi | 141.0 (11) | K1xiv—O3—Na2 | 124.7 (4) |
O2xii—Na2—O2vi | 92.8 (7) | K2—O3—Na2 | 11.0 (5) |
O3xi—Na2—O2vi | 120.2 (8) | K2xiv—O3—Na2 | 128.9 (7) |
O1—Na2—O2vi | 97.3 (5) | K1—O3—Na2 | 7.0 (4) |
O3xii—Na2—O2vi | 70.1 (5) | Mo—O3—K2xiii | 76.3 (2) |
O2ix—Na2—O2vi | 148.1 (7) | Ni2—O3—K2xiii | 118.3 (3) |
O3—Na2—O2vi | 49.6 (3) | Na2xi—O3—K2xiii | 116.1 (6) |
O1i—Na2—O2vi | 80.5 (5) | K2xi—O3—K2xiii | 126.9 (4) |
Mo—O1—Na2viii | 118.3 (6) | K1xi—O3—K2xiii | 122.3 (2) |
Mo—O1—Na1 | 138.64 (9) | Na2xiv—O3—K2xiii | 35.2 (5) |
Na2viii—O1—Na1 | 92.1 (5) | K1xiv—O3—K2xiii | 26.3 (3) |
Mo—O1—Na2 | 115.7 (5) | K2—O3—K2xiii | 144.2 (4) |
Na2viii—O1—Na2 | 93.1 (3) | K2xiv—O3—K2xiii | 20.5 (4) |
Na1—O1—Na2 | 87.6 (6) | K1—O3—K2xiii | 145.0 (4) |
Mo—O1—K1 | 102.7 (3) | Na2—O3—K2xiii | 139.4 (4) |
Na2viii—O1—K1 | 103.8 (8) | Mo—O4—Ni1 | 119.40 (7) |
Na1—O1—K1 | 95.72 (16) | Mo—O4—Ni2v | 135.89 (7) |
Na2—O1—K1 | 13.7 (5) | Ni1—O4—Ni2v | 95.31 (6) |
Mo—O1—K2 | 97.4 (4) | Mo—O4—K1v | 87.00 (13) |
Na2viii—O1—K2 | 104.1 (6) | Ni1—O4—K1v | 138.16 (14) |
Na1—O1—K2 | 101.7 (4) | Ni2v—O4—K1v | 83.19 (13) |
Na2—O1—K2 | 18.3 (7) | Mo—O4—K2v | 90.7 (3) |
K1—O1—K2 | 6.1 (5) | Ni1—O4—K2v | 137.9 (3) |
Mo—O1—K1viii | 124.0 (2) | Ni2v—O4—K2v | 78.1 (3) |
Na2viii—O1—K1viii | 6.1 (7) | K1v—O4—K2v | 5.1 (4) |
Na1—O1—K1viii | 88.2 (2) | Mo—O4—Na2v | 83.2 (4) |
Na2—O1—K1viii | 88.3 (6) | Ni1—O4—Na2v | 135.9 (3) |
K1—O1—K1viii | 99.5 (2) | Ni2v—O4—Na2v | 90.1 (4) |
K2—O1—K1viii | 100.3 (5) | K1v—O4—Na2v | 7.1 (3) |
Mo—O1—K2viii | 121.9 (3) | K2v—O4—Na2v | 12.0 (5) |
Na2viii—O1—K2viii | 4.1 (6) | | |
Symmetry codes: (i) −y, x−y, z; (ii) −x, −x+y, −z+1/2; (iii) y, x, −z+1/2; (iv) x−y, −y, −z+1/2; (v) −x+y, −x, z; (vi) y+1/3, −x+y+2/3, −z+2/3; (vii) −x+y+2/3, y+1/3, z−1/6; (viii) y, −x+y, −z+1; (ix) x−y, x, −z+1; (x) −x, −y, −z+1; (xi) −x+2/3, −x+y+1/3, −z+5/6; (xii) −y+1/3, −x+2/3, z+1/6; (xiii) x−y+1/3, x−1/3, −z+2/3; (xiv) −y+2/3, −x+1/3, z−1/6. |
Crystal data top
K3NaMg4·6(MoO4) | Dx = 3.315 Mg m−3 |
Mr = 1197.17 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 10553 reflections |
a = 14.4528 (2) Å | θ = 2.6–28.3° |
c = 19.8894 (3) Å | µ = 3.79 mm−1 |
V = 3597.96 (11) Å3 | T = 296 K |
Z = 6 | Fragment, colourless |
F(000) = 3360 | 0.06 × 0.04 × 0.03 mm |
Data collection top
Bruker-Nonius X8 APEX CCD diffractometer | 932 reflections with I > 2σ(I) |
\ f scans, frame data integration | Rint = 0.030 |
Absorption correction: multi-scan SADABS (Bruker, 2005) | θmax = 28.3°, θmin = 2.6° |
Tmin = 0.834, Tmax = 0.893 | h = −19→19 |
10553 measured reflections | k = −18→17 |
1001 independent reflections | l = −26→26 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.015 | w = 1/[σ2(Fo2) + (0.0111P)2 + 7.1525P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.034 | (Δ/σ)max = 0.004 |
S = 1.20 | Δρmax = 0.39 e Å−3 |
1001 reflections | Δρmin = −0.46 e Å−3 |
76 parameters | Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
7 restraints | Extinction coefficient: 0.000180 (16) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo | 0.18653 (2) | 0.00666 (2) | 0.35467 (2) | 0.01349 (7) | |
Mg1 | 0.000000 | 0.000000 | 0.250000 | 0.0106 (3) | |
Mg2 | 0.21486 (7) | 0.21486 (7) | 0.250000 | 0.0130 (2) | |
Na1 | 0.000000 | 0.000000 | 0.500000 | 0.0274 (5) | |
K1 | 0.2565 (3) | 0.2400 (3) | 0.44331 (17) | 0.0263 (6) | 0.4237 (14) |
K2 | 0.281 (2) | 0.252 (2) | 0.4288 (10) | 0.050 (6) | 0.0763 (14) |
O1 | 0.15435 (14) | 0.02413 (15) | 0.43545 (8) | 0.0337 (4) | |
O2 | 0.26341 (12) | −0.05651 (12) | 0.35676 (8) | 0.0234 (4) | |
O3 | 0.26436 (12) | 0.13186 (12) | 0.31610 (8) | 0.0219 (3) | |
O4 | 0.06533 (11) | −0.07261 (11) | 0.30737 (7) | 0.0146 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo | 0.01417 (11) | 0.01354 (11) | 0.01332 (10) | 0.00735 (8) | −0.00376 (6) | −0.00154 (6) |
Mg1 | 0.0087 (5) | 0.0087 (5) | 0.0144 (7) | 0.0043 (2) | 0.000 | 0.000 |
Mg2 | 0.0107 (3) | 0.0107 (3) | 0.0165 (5) | 0.0045 (4) | 0.00126 (17) | −0.00126 (17) |
Na1 | 0.0312 (8) | 0.0312 (8) | 0.0198 (11) | 0.0156 (4) | 0.000 | 0.000 |
K1 | 0.0407 (10) | 0.0197 (9) | 0.0197 (17) | 0.0160 (8) | −0.0064 (10) | −0.0028 (10) |
K2 | 0.122 (18) | 0.026 (7) | 0.006 (7) | 0.038 (10) | −0.010 (8) | −0.004 (5) |
O1 | 0.0363 (10) | 0.0428 (11) | 0.0180 (8) | 0.0167 (9) | −0.0023 (7) | −0.0085 (7) |
O2 | 0.0209 (8) | 0.0194 (8) | 0.0329 (9) | 0.0122 (7) | −0.0084 (6) | 0.0010 (6) |
O3 | 0.0155 (8) | 0.0170 (8) | 0.0307 (8) | 0.0062 (6) | −0.0056 (6) | 0.0021 (6) |
O4 | 0.0150 (7) | 0.0125 (7) | 0.0169 (7) | 0.0074 (6) | −0.0036 (5) | −0.0009 (5) |
Geometric parameters (Å, º) top
Mo—O1 | 1.7259 (16) | Na1—K1 | 3.767 (3) |
Mo—O2 | 1.7562 (16) | Na1—K1v | 3.767 (3) |
Mo—O3 | 1.7586 (15) | Na1—K1viii | 3.767 (3) |
Mo—O4 | 1.8053 (14) | K1—K2 | 0.42 (2) |
Mg1—O4i | 2.0701 (13) | K1—K2xi | 1.80 (2) |
Mg1—O4ii | 2.0701 (13) | K1—K1xi | 2.195 (6) |
Mg1—O4iii | 2.0701 (13) | K1—O2xii | 2.697 (4) |
Mg1—O4iv | 2.0701 (13) | K1—O1 | 2.707 (4) |
Mg1—O4v | 2.0701 (13) | K1—O3xi | 2.848 (4) |
Mg1—O4 | 2.0701 (13) | K1—O1viii | 2.902 (3) |
Mg2—O2vi | 2.0367 (16) | K1—O3xii | 2.936 (4) |
Mg2—O2vii | 2.0367 (16) | K1—O3 | 3.006 (4) |
Mg2—O4iv | 2.1163 (15) | K1—O2vi | 3.009 (4) |
Mg2—O4i | 2.1163 (16) | K1—O1i | 3.544 (4) |
Mg2—O3 | 2.1302 (15) | K1—O4i | 3.554 (4) |
Mg2—O3iii | 2.1303 (15) | K2—K2xi | 1.41 (5) |
Na1—O1viii | 2.4430 (18) | K2—O2xii | 2.71 (3) |
Na1—O1v | 2.4430 (18) | K2—O2vi | 2.74 (2) |
Na1—O1ix | 2.4430 (18) | K2—O3 | 2.77 (2) |
Na1—O1i | 2.4430 (18) | K2—O3xi | 2.84 (3) |
Na1—O1x | 2.4430 (18) | K2—O1 | 2.86 (2) |
Na1—O1 | 2.4431 (18) | K2—O3xii | 3.11 (3) |
Na1—K1ix | 3.767 (3) | K2—O1viii | 3.31 (2) |
Na1—K1i | 3.767 (3) | K2—O4i | 3.55 (3) |
Na1—K1x | 3.767 (3) | | |
| | | |
O1—Mo—O2 | 109.93 (8) | O3—K2—O1 | 60.7 (5) |
O1—Mo—O3 | 109.63 (8) | O3xi—K2—O1 | 78.0 (6) |
O2—Mo—O3 | 107.44 (7) | O2xii—K2—O3xii | 57.8 (5) |
O1—Mo—O4 | 109.33 (7) | O2vi—K2—O3xii | 81.0 (7) |
O2—Mo—O4 | 110.36 (6) | O3—K2—O3xii | 140.6 (10) |
O3—Mo—O4 | 110.13 (6) | O3xi—K2—O3xii | 117.5 (7) |
O4i—Mg1—O4ii | 177.09 (8) | O1—K2—O3xii | 122.9 (8) |
O4i—Mg1—O4iii | 89.60 (8) | O2xii—K2—O1viii | 76.8 (5) |
O4ii—Mg1—O4iii | 92.54 (5) | O2vi—K2—O1viii | 138.1 (10) |
O4i—Mg1—O4iv | 85.39 (8) | O3—K2—O1viii | 124.1 (8) |
O4ii—Mg1—O4iv | 92.54 (5) | O3xi—K2—O1viii | 75.1 (5) |
O4iii—Mg1—O4iv | 92.54 (5) | O1—K2—O1viii | 64.3 (4) |
O4i—Mg1—O4v | 92.54 (5) | O3xii—K2—O1viii | 67.9 (5) |
O4ii—Mg1—O4v | 89.60 (8) | O2xii—K2—O4i | 149.6 (10) |
O4iii—Mg1—O4v | 85.39 (8) | O2vi—K2—O4i | 54.8 (4) |
O4iv—Mg1—O4v | 177.09 (8) | O3—K2—O4i | 51.2 (4) |
O4i—Mg1—O4 | 92.54 (5) | O3xi—K2—O4i | 142.3 (9) |
O4ii—Mg1—O4 | 85.39 (8) | O1—K2—O4i | 66.0 (5) |
O4iii—Mg1—O4 | 177.09 (8) | O3xii—K2—O4i | 92.2 (7) |
O4iv—Mg1—O4 | 89.60 (8) | O1viii—K2—O4i | 97.7 (6) |
O4v—Mg1—O4 | 92.54 (5) | Mo—O1—Na1 | 139.63 (9) |
O2vi—Mg2—O2vii | 93.08 (10) | Mo—O1—K1 | 101.00 (10) |
O2vi—Mg2—O4iv | 174.99 (7) | Na1—O1—K1 | 93.85 (9) |
O2vii—Mg2—O4iv | 91.91 (5) | Mo—O1—K2 | 93.6 (4) |
O2vi—Mg2—O4i | 91.91 (5) | Na1—O1—K2 | 101.5 (5) |
O2vii—Mg2—O4i | 174.99 (7) | K1—O1—K2 | 8.0 (5) |
O4iv—Mg2—O4i | 83.10 (8) | Mo—O1—K1ix | 124.79 (12) |
O2vi—Mg2—O3 | 92.96 (6) | Na1—O1—K1ix | 89.19 (9) |
O2vii—Mg2—O3 | 96.01 (6) | K1—O1—K1ix | 98.24 (9) |
O4iv—Mg2—O3 | 86.96 (6) | K2—O1—K1ix | 100.4 (5) |
O4i—Mg2—O3 | 83.28 (6) | Mo—O1—K2ix | 123.3 (5) |
O2vi—Mg2—O3iii | 96.01 (6) | Na1—O1—K2ix | 90.2 (4) |
O2vii—Mg2—O3iii | 92.96 (6) | K1—O1—K2ix | 99.7 (5) |
O4iv—Mg2—O3iii | 83.28 (6) | K2—O1—K2ix | 101.7 (4) |
O4i—Mg2—O3iii | 86.96 (6) | K1ix—O1—K2ix | 1.8 (5) |
O3—Mg2—O3iii | 166.95 (10) | Mo—O1—K1v | 87.60 (8) |
O1viii—Na1—O1v | 180.00 (8) | Na1—O1—K1v | 75.48 (7) |
O1viii—Na1—O1ix | 94.92 (5) | K1—O1—K1v | 169.33 (10) |
O1v—Na1—O1ix | 85.08 (5) | K2—O1—K1v | 176.4 (6) |
O1viii—Na1—O1i | 85.08 (5) | K1ix—O1—K1v | 81.67 (8) |
O1v—Na1—O1i | 94.92 (5) | K2ix—O1—K1v | 80.5 (5) |
O1ix—Na1—O1i | 180.00 (6) | Mo—O2—Mg2xiii | 145.54 (10) |
O1viii—Na1—O1x | 94.92 (5) | Mo—O2—K1xiv | 99.77 (10) |
O1v—Na1—O1x | 85.08 (5) | Mg2xiii—O2—K1xiv | 102.15 (10) |
O1ix—Na1—O1x | 94.92 (5) | Mo—O2—K2xiv | 102.4 (6) |
O1i—Na1—O1x | 85.08 (5) | Mg2xiii—O2—K2xiv | 103.3 (6) |
O1viii—Na1—O1 | 85.08 (5) | K1xiv—O2—K2xiv | 8.8 (5) |
O1v—Na1—O1 | 94.92 (5) | Mo—O2—K2xiii | 115.2 (5) |
O1ix—Na1—O1 | 85.08 (5) | Mg2xiii—O2—K2xiii | 98.4 (5) |
O1i—Na1—O1 | 94.92 (5) | K1xiv—O2—K2xiii | 38.5 (5) |
O1x—Na1—O1 | 180.0 | K2xiv—O2—K2xiii | 29.9 (10) |
O2xii—K1—O1 | 141.42 (14) | Mo—O2—K1xiii | 115.55 (10) |
O2xii—K1—O3xi | 65.99 (9) | Mg2xiii—O2—K1xiii | 98.71 (10) |
O1—K1—O3xi | 80.35 (11) | K1xiv—O2—K1xiii | 44.84 (12) |
O2xii—K1—O1viii | 84.50 (11) | K2xiv—O2—K1xiii | 36.1 (4) |
O1—K1—O1viii | 72.07 (10) | K2xiii—O2—K1xiii | 6.4 (6) |
O3xi—K1—O1viii | 81.74 (10) | Mo—O3—Mg2 | 128.79 (8) |
O2xii—K1—O3xii | 60.22 (10) | Mo—O3—K2 | 95.9 (4) |
O1—K1—O3xii | 136.60 (12) | Mg2—O3—K2 | 95.3 (5) |
O3xi—K1—O3xii | 122.93 (14) | Mo—O3—K2xi | 115.6 (5) |
O1viii—K1—O3xii | 75.80 (9) | Mg2—O3—K2xi | 97.0 (5) |
O2xii—K1—O3 | 139.12 (12) | K2—O3—K2xi | 29.0 (9) |
O1—K1—O3 | 59.53 (9) | Mo—O3—K1xi | 122.20 (10) |
O3xi—K1—O3 | 96.16 (12) | Mg2—O3—K1xi | 95.12 (10) |
O1viii—K1—O3 | 131.08 (14) | K2—O3—K1xi | 37.2 (5) |
O3xii—K1—O3 | 137.41 (13) | K2xi—O3—K1xi | 8.4 (5) |
O2xii—K1—O2vi | 103.20 (12) | Mo—O3—K1xiv | 91.40 (9) |
O1—K1—O2vi | 113.40 (14) | Mg2—O3—K1xiv | 121.77 (9) |
O3xi—K1—O2vi | 131.68 (11) | K2—O3—K1xiv | 123.9 (6) |
O1viii—K1—O2vi | 146.17 (13) | K2xi—O3—K1xiv | 100.2 (5) |
O3xii—K1—O2vi | 79.73 (10) | K1xi—O3—K1xiv | 94.35 (13) |
O3—K1—O2vi | 60.33 (7) | Mo—O3—K1 | 89.81 (9) |
O2xii—K1—O1i | 125.09 (13) | Mg2—O3—K1 | 96.67 (9) |
O1—K1—O1i | 68.83 (10) | K2—O3—K1 | 6.9 (5) |
O3xi—K1—O1i | 136.77 (11) | K2xi—O3—K1 | 35.6 (4) |
O1viii—K1—O1i | 60.70 (8) | K1xi—O3—K1 | 43.95 (11) |
O3xii—K1—O1i | 70.28 (8) | K1xiv—O3—K1 | 127.51 (11) |
O3—K1—O1i | 93.58 (10) | Mo—O3—K2xiv | 88.7 (5) |
O2vi—K1—O1i | 89.25 (9) | Mg2—O3—K2xiv | 119.1 (4) |
O2xii—K1—O4i | 150.63 (14) | K2—O3—K2xiv | 130.9 (7) |
O1—K1—O4i | 67.30 (9) | K2xi—O3—K2xiv | 107.4 (9) |
O3xi—K1—O4i | 141.66 (15) | K1xi—O3—K2xiv | 101.5 (4) |
O1viii—K1—O4i | 105.95 (10) | K1xiv—O3—K2xiv | 7.2 (4) |
O3xii—K1—O4i | 95.14 (10) | K1—O3—K2xiv | 134.2 (3) |
O3—K1—O4i | 50.10 (7) | Mo—O4—Mg1 | 120.62 (7) |
O2vi—K1—O4i | 53.34 (7) | Mo—O4—Mg2v | 135.84 (7) |
O1i—K1—O4i | 47.90 (6) | Mg1—O4—Mg2v | 95.76 (6) |
O2xii—K2—O2vi | 110.2 (8) | Mo—O4—K2v | 91.2 (4) |
O2xii—K2—O3 | 153.9 (10) | Mg1—O4—K2v | 136.5 (4) |
O2vi—K2—O3 | 66.4 (5) | Mg2v—O4—K2v | 75.4 (3) |
O2xii—K2—O3xi | 65.9 (6) | Mo—O4—K1v | 86.14 (7) |
O2vi—K2—O3xi | 146.5 (9) | Mg1—O4—K1v | 137.12 (9) |
O3—K2—O3xi | 101.9 (9) | Mg2v—O4—K1v | 82.16 (6) |
O2xii—K2—O1 | 132.4 (8) | K2v—O4—K1v | 6.7 (4) |
O2vi—K2—O1 | 117.0 (9) | | |
Symmetry codes: (i) −y, x−y, z; (ii) −x, −x+y, −z+1/2; (iii) y, x, −z+1/2; (iv) x−y, −y, −z+1/2; (v) −x+y, −x, z; (vi) y+1/3, −x+y+2/3, −z+2/3; (vii) −x+y+2/3, y+1/3, z−1/6; (viii) x−y, x, −z+1; (ix) y, −x+y, −z+1; (x) −x, −y, −z+1; (xi) −x+2/3, −x+y+1/3, −z+5/6; (xii) −y+1/3, −x+2/3, z+1/6; (xiii) x−y+1/3, x−1/3, −z+2/3; (xiv) −y+2/3, −x+1/3, z−1/6. |
Crystal data top
K2.88Mg4Na1.12·6(MoO4) | Dx = 3.298 Mg m−3 |
Mr = 1195.26 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 11402 reflections |
a = 14.4673 (5) Å | θ = 2.6–33.3° |
c = 19.9186 (9) Å | µ = 3.76 mm−1 |
V = 3610.5 (3) Å3 | T = 296 K |
Z = 6 | Fragment, colourless |
F(000) = 3354.3 | 0.06 × 0.06 × 0.05 mm |
Data collection top
Bruker-Nonius X8 APEX CCD diffractometer | 1326 reflections with I > 2σ(I) |
\ f scans, frame data integration | Rint = 0.048 |
Absorption correction: multi-scan SADABS (Bruker, 2005) | θmax = 33.3°, θmin = 2.6° |
Tmin = 0.798, Tmax = 0.829 | h = −17→22 |
11402 measured reflections | k = −22→21 |
1561 independent reflections | l = −30→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.021 | w = 1/[σ2(Fo2) + (0.0169P)2 + 1.2304P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.044 | (Δ/σ)max = 0.005 |
S = 1.04 | Δρmax = 0.71 e Å−3 |
1552 reflections | Δρmin = −0.71 e Å−3 |
81 parameters | Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
7 restraints | Extinction coefficient: 0.000166 (19) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo | 0.18616 (2) | 0.00683 (2) | 0.35501 (2) | 0.01160 (6) | |
Mg1 | 0.000000 | 0.000000 | 0.250000 | 0.0090 (3) | |
Mg2 | 0.21506 (7) | 0.21506 (7) | 0.250000 | 0.01157 (18) | |
Na1 | 0.000000 | 0.000000 | 0.500000 | 0.0298 (5) | |
K1 | 0.2546 (4) | 0.2392 (5) | 0.4430 (4) | 0.0216 (11) | 0.2781 (16) |
K2 | 0.2622 (8) | 0.2446 (9) | 0.4397 (5) | 0.051 (3) | 0.2021 (16) |
Na2 | 0.247 (6) | 0.214 (5) | 0.469 (3) | 0.030 (15)* | 0.0198 (15) |
O1 | 0.15319 (13) | 0.02320 (15) | 0.43567 (8) | 0.0310 (4) | |
O2 | 0.26296 (12) | −0.05624 (12) | 0.35715 (8) | 0.0225 (3) | |
O3 | 0.26435 (12) | 0.13271 (12) | 0.31727 (7) | 0.0201 (3) | |
O4 | 0.06579 (11) | −0.07220 (11) | 0.30708 (7) | 0.0135 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo | 0.01121 (9) | 0.01207 (9) | 0.01189 (8) | 0.00610 (7) | −0.00308 (5) | −0.00137 (5) |
Mg1 | 0.0076 (4) | 0.0076 (4) | 0.0118 (7) | 0.0038 (2) | 0.000 | 0.000 |
Mg2 | 0.0093 (3) | 0.0093 (3) | 0.0146 (4) | 0.0035 (3) | 0.00073 (16) | −0.00073 (16) |
Na1 | 0.0334 (8) | 0.0334 (8) | 0.0224 (11) | 0.0167 (4) | 0.000 | 0.000 |
K1 | 0.0286 (16) | 0.0147 (19) | 0.022 (2) | 0.0116 (13) | −0.0013 (15) | −0.0043 (15) |
K2 | 0.094 (6) | 0.029 (4) | 0.037 (4) | 0.035 (4) | −0.041 (4) | −0.014 (3) |
O1 | 0.0296 (9) | 0.0418 (11) | 0.0172 (7) | 0.0145 (9) | −0.0005 (6) | −0.0079 (7) |
O2 | 0.0202 (8) | 0.0195 (8) | 0.0322 (9) | 0.0133 (6) | −0.0077 (6) | 0.0002 (6) |
O3 | 0.0143 (7) | 0.0159 (7) | 0.0282 (8) | 0.0062 (6) | −0.0028 (6) | 0.0040 (6) |
O4 | 0.0136 (7) | 0.0113 (6) | 0.0164 (6) | 0.0068 (5) | −0.0040 (5) | −0.0008 (5) |
Geometric parameters (Å, º) top
Mo—O1 | 1.7255 (15) | K1—O2xii | 2.724 (7) |
Mo—O2 | 1.7558 (15) | K1—O3xi | 2.853 (7) |
Mo—O3 | 1.7611 (15) | K1—O1viii | 2.897 (6) |
Mo—O4 | 1.8057 (13) | K1—O3xii | 2.947 (6) |
Mg1—O4 | 2.0697 (13) | K1—O3 | 2.980 (6) |
Mg1—O4i | 2.0697 (13) | K1—O2vi | 3.020 (8) |
Mg1—O4ii | 2.0697 (13) | K1—O1ii | 3.510 (6) |
Mg1—O4iii | 2.0697 (13) | K1—O4ii | 3.546 (7) |
Mg1—O4iv | 2.0697 (13) | K2—Na2 | 0.70 (7) |
Mg1—O4v | 2.0697 (13) | K2—K2xi | 2.00 (2) |
Mg2—O2vi | 2.0399 (16) | K2—Na2xi | 2.50 (7) |
Mg2—O2vii | 2.0399 (16) | K2—O2xii | 2.695 (11) |
Mg2—O4iii | 2.1221 (15) | K2—O1 | 2.775 (11) |
Mg2—O4ii | 2.1221 (15) | K2—O3xi | 2.840 (11) |
Mg2—O3iv | 2.1384 (14) | K2—O3 | 2.935 (10) |
Mg2—O3 | 2.1384 (14) | K2—O2vi | 2.943 (11) |
Na1—O1viii | 2.4337 (17) | K2—O3xii | 2.969 (10) |
Na1—O1v | 2.4337 (17) | K2—O1viii | 3.007 (11) |
Na1—O1ix | 2.4337 (17) | K2—O4ii | 3.559 (11) |
Na1—O1ii | 2.4337 (17) | K2—O1ii | 3.599 (11) |
Na1—O1x | 2.4337 (17) | Na2—O1viii | 2.40 (7) |
Na1—O1 | 2.4337 (17) | Na2—O1 | 2.48 (6) |
K1—K2 | 0.118 (16) | Na2—O3xi | 2.52 (7) |
K1—Na2 | 0.61 (7) | Na2—O2xii | 2.70 (6) |
K1—K2xi | 2.120 (7) | Na2—Na2xi | 3.01 (15) |
K1—K1xi | 2.235 (10) | Na2—O3xii | 3.13 (6) |
K1—Na2xi | 2.61 (7) | Na2—O3 | 3.30 (7) |
K1—O1 | 2.711 (7) | Na2—O1ii | 3.53 (7) |
| | | |
O1—Mo—O2 | 109.81 (8) | Na2—O1—K1v | 160.6 (17) |
O1—Mo—O3 | 109.53 (8) | K1—O1—K1v | 169.41 (18) |
O2—Mo—O3 | 107.55 (7) | K2—O1—K1v | 171.4 (3) |
O1—Mo—O4 | 109.51 (7) | K1ix—O1—K1v | 82.19 (16) |
O2—Mo—O4 | 110.14 (6) | K2ix—O1—K1v | 82.1 (3) |
O3—Mo—O4 | 110.28 (7) | Mo—O1—Na2v | 97.7 (12) |
O4—Mg1—O4i | 85.45 (7) | Na2ix—O1—Na2v | 71.5 (14) |
O4—Mg1—O4ii | 92.71 (5) | Na1—O1—Na2v | 67.1 (11) |
O4i—Mg1—O4ii | 177.43 (8) | Na2—O1—Na2v | 151 (3) |
O4—Mg1—O4iii | 89.17 (8) | K1—O1—Na2v | 160.1 (12) |
O4i—Mg1—O4iii | 92.71 (5) | K2—O1—Na2v | 162.2 (12) |
O4ii—Mg1—O4iii | 85.46 (7) | K1ix—O1—Na2v | 78.0 (10) |
O4—Mg1—O4iv | 177.43 (8) | K2ix—O1—Na2v | 78.1 (10) |
O4i—Mg1—O4iv | 92.71 (5) | K1v—O1—Na2v | 9.9 (11) |
O4ii—Mg1—O4iv | 89.17 (8) | Mo—O1—K2v | 86.65 (19) |
O4iii—Mg1—O4iv | 92.71 (5) | Na2ix—O1—K2v | 75.7 (16) |
O4—Mg1—O4v | 92.71 (5) | Na1—O1—K2v | 76.97 (19) |
O4i—Mg1—O4v | 89.17 (8) | Na2—O1—K2v | 161.8 (16) |
O4ii—Mg1—O4v | 92.71 (5) | K1—O1—K2v | 170.4 (2) |
O4iii—Mg1—O4v | 177.43 (8) | K2—O1—K2v | 172.4 (3) |
O4iv—Mg1—O4v | 85.46 (7) | K1ix—O1—K2v | 82.8 (2) |
O2vi—Mg2—O2vii | 92.81 (10) | K2ix—O1—K2v | 82.7 (2) |
O2vi—Mg2—O4iii | 175.01 (7) | K1v—O1—K2v | 1.2 (3) |
O2vii—Mg2—O4iii | 92.16 (6) | Na2v—O1—K2v | 11.2 (12) |
O2vi—Mg2—O4ii | 92.16 (6) | Mo—O1—K2xi | 77.64 (17) |
O2vii—Mg2—O4ii | 175.01 (7) | Na2ix—O1—K2xi | 103.1 (15) |
O4iii—Mg2—O4ii | 82.87 (8) | Na1—O1—K2xi | 122.14 (18) |
O2vi—Mg2—O3iv | 96.19 (6) | Na2—O1—K2xi | 35.7 (16) |
O2vii—Mg2—O3iv | 92.65 (6) | K1—O1—K2xi | 28.64 (17) |
O4iii—Mg2—O3iv | 83.11 (6) | K2—O1—K2xi | 26.6 (3) |
O4ii—Mg2—O3iv | 87.27 (6) | K1ix—O1—K2xi | 97.2 (2) |
O2vi—Mg2—O3 | 92.65 (6) | K2ix—O1—K2xi | 97.0 (2) |
O2vii—Mg2—O3 | 96.19 (6) | K1v—O1—K2xi | 161.9 (3) |
O4iii—Mg2—O3 | 87.27 (6) | Na2v—O1—K2xi | 169.9 (10) |
O4ii—Mg2—O3 | 83.11 (6) | K2v—O1—K2xi | 160.87 (7) |
O3iv—Mg2—O3 | 167.16 (9) | Mo—O2—Mg2xiii | 145.84 (10) |
O1viii—Na1—O1v | 180.00 (8) | Mo—O2—K2xiv | 100.1 (2) |
O1viii—Na1—O1ix | 94.83 (5) | Mg2xiii—O2—K2xiv | 102.6 (2) |
O1v—Na1—O1ix | 85.17 (5) | Mo—O2—Na2xiv | 104.9 (14) |
O1viii—Na1—O1ii | 85.17 (5) | Mg2xiii—O2—Na2xiv | 91.8 (14) |
O1v—Na1—O1ii | 94.83 (5) | K2xiv—O2—Na2xiv | 14.9 (15) |
O1ix—Na1—O1ii | 180.0 | Mo—O2—K1xiv | 99.57 (15) |
O1viii—Na1—O1x | 94.83 (5) | Mg2xiii—O2—K1xiv | 102.08 (17) |
O1v—Na1—O1x | 85.17 (5) | K2xiv—O2—K1xiv | 2.4 (3) |
O1ix—Na1—O1x | 94.83 (5) | Na2xiv—O2—K1xiv | 12.9 (15) |
O1ii—Na1—O1x | 85.17 (5) | Mo—O2—K2xiii | 115.2 (2) |
O1viii—Na1—O1 | 85.17 (5) | Mg2xiii—O2—K2xiii | 98.6 (2) |
O1v—Na1—O1 | 94.83 (5) | K2xiv—O2—K2xiii | 41.4 (4) |
O1ix—Na1—O1 | 85.17 (5) | Na2xiv—O2—K2xiii | 52.4 (15) |
O1ii—Na1—O1 | 94.83 (5) | K1xiv—O2—K2xiii | 43.72 (17) |
O1x—Na1—O1 | 180.0 | Mo—O2—K1xiii | 115.83 (14) |
O1—K1—O2xii | 141.0 (3) | Mg2xiii—O2—K1xiii | 98.15 (13) |
O1—K1—O3xi | 80.4 (2) | K2xiv—O2—K1xiii | 43.09 (19) |
O2xii—K1—O3xi | 65.59 (16) | Na2xiv—O2—K1xiii | 54.0 (15) |
O1—K1—O1viii | 71.84 (17) | K1xiv—O2—K1xiii | 45.44 (18) |
O2xii—K1—O1viii | 84.41 (19) | K2xiii—O2—K1xiii | 1.7 (3) |
O3xi—K1—O1viii | 81.8 (2) | Mo—O2—Na2ix | 76.6 (11) |
O1—K1—O3xii | 136.93 (19) | Mg2xiii—O2—Na2ix | 69.2 (11) |
O2xii—K1—O3xii | 59.87 (13) | K2xiv—O2—Na2ix | 132.7 (10) |
O3xi—K1—O3xii | 122.3 (2) | Na2xiv—O2—Na2ix | 119.4 (16) |
O1viii—K1—O3xii | 75.89 (13) | K1xiv—O2—Na2ix | 130.2 (10) |
O1—K1—O3 | 59.82 (13) | K2xiii—O2—Na2ix | 166.2 (11) |
O2xii—K1—O3 | 138.54 (19) | K1xiii—O2—Na2ix | 166.4 (11) |
O3xi—K1—O3 | 95.56 (16) | Mo—O2—Na2xiii | 116.5 (9) |
O1viii—K1—O3 | 131.2 (2) | Mg2xiii—O2—Na2xiii | 97.5 (9) |
O3xii—K1—O3 | 138.3 (3) | K2xiv—O2—Na2xiii | 43.6 (11) |
O1—K1—O2vi | 114.0 (2) | Na2xiv—O2—Na2xiii | 54 (2) |
O2xii—K1—O2vi | 102.9 (2) | K1xiv—O2—Na2xiii | 45.9 (11) |
O3xi—K1—O2vi | 130.61 (18) | K2xiii—O2—Na2xiii | 2.4 (11) |
O1viii—K1—O2vi | 147.1 (2) | K1xiii—O2—Na2xiii | 0.8 (10) |
O3xii—K1—O2vi | 80.27 (19) | Na2ix—O2—Na2xiii | 165.9 (13) |
O3—K1—O2vi | 60.49 (14) | Mo—O2—K1v | 73.12 (11) |
O1—K1—O1ii | 68.98 (15) | Mg2xiii—O2—K1v | 88.90 (10) |
O2xii—K1—O1ii | 125.25 (17) | K2xiv—O2—K1v | 166.3 (2) |
O3xi—K1—O1ii | 137.2 (2) | Na2xiv—O2—K1v | 177.2 (15) |
O1viii—K1—O1ii | 60.99 (11) | K1xiv—O2—K1v | 167.9 (2) |
O3xii—K1—O1ii | 70.72 (12) | K2xiii—O2—K1v | 130.2 (2) |
O3—K1—O1ii | 94.13 (18) | K1xiii—O2—K1v | 128.55 (12) |
O2vi—K1—O1ii | 89.95 (19) | Na2ix—O2—K1v | 58.4 (10) |
O1—K1—O4ii | 67.73 (15) | Na2xiii—O2—K1v | 128.2 (11) |
O2xii—K1—O4ii | 150.7 (3) | Mo—O2—K2v | 74.13 (17) |
O3xi—K1—O4ii | 141.7 (2) | Mg2xiii—O2—K2v | 88.70 (16) |
O1viii—K1—O4ii | 106.56 (17) | K2xiv—O2—K2v | 165.4 (3) |
O3xii—K1—O4ii | 95.82 (19) | Na2xiv—O2—K2v | 178.9 (15) |
O3—K1—O4ii | 50.42 (11) | K1xiv—O2—K2v | 167.28 (19) |
O2vi—K1—O4ii | 53.62 (13) | K2xiii—O2—K2v | 128.55 (18) |
O1ii—K1—O4ii | 48.25 (9) | K1xiii—O2—K2v | 126.9 (2) |
O2xii—K2—O1 | 139.0 (4) | Na2ix—O2—K2v | 59.9 (10) |
O2xii—K2—O3xi | 66.1 (2) | Na2xiii—O2—K2v | 126.6 (12) |
O1—K2—O3xi | 79.6 (3) | K1v—O2—K2v | 1.7 (2) |
O2xii—K2—O3 | 142.8 (4) | Mo—O2—K1ix | 80.01 (9) |
O1—K2—O3 | 59.8 (2) | Mg2xiii—O2—K1ix | 65.92 (8) |
O3xi—K2—O3 | 96.8 (3) | K2xiv—O2—K1ix | 128.0 (3) |
O2xii—K2—O2vi | 105.6 (4) | Na2xiv—O2—K1ix | 114.3 (15) |
O1—K2—O2vi | 114.5 (4) | K1xiv—O2—K1ix | 125.56 (12) |
O3xi—K2—O2vi | 134.6 (4) | K2xiii—O2—K1ix | 160.8 (3) |
O3—K2—O2vi | 61.9 (2) | K1xiii—O2—K1ix | 161.32 (10) |
O2xii—K2—O3xii | 59.9 (2) | Na2ix—O2—K1ix | 5.6 (10) |
O1—K2—O3xii | 132.9 (4) | Na2xiii—O2—K1ix | 160.9 (10) |
O3xi—K2—O3xii | 122.0 (4) | K1v—O2—K1ix | 63.57 (14) |
O3—K2—O3xii | 139.5 (4) | K2v—O2—K1ix | 64.98 (17) |
O2vi—K2—O3xii | 81.2 (3) | Mo—O3—Mg2 | 128.53 (8) |
O2xii—K2—O1viii | 82.8 (3) | Mo—O3—Na2xi | 129.7 (15) |
O1—K2—O1viii | 69.3 (3) | Mg2—O3—Na2xi | 94.7 (14) |
O3xi—K2—O1viii | 80.1 (3) | Mo—O3—K2xi | 121.7 (2) |
O3—K2—O1viii | 128.6 (4) | Mg2—O3—K2xi | 95.6 (2) |
O2vi—K2—O1viii | 145.0 (4) | Na2xi—O3—K2xi | 13.3 (17) |
O3xii—K2—O1viii | 73.9 (2) | Mo—O3—K1xi | 123.08 (13) |
O2xii—K2—O4ii | 151.8 (4) | Mg2—O3—K1xi | 95.64 (14) |
O1—K2—O4ii | 67.0 (2) | Na2xi—O3—K1xi | 11.0 (16) |
O3xi—K2—O4ii | 141.6 (4) | K2xi—O3—K1xi | 2.4 (3) |
O3—K2—O4ii | 50.48 (17) | Mo—O3—K2 | 92.1 (2) |
O2vi—K2—O4ii | 53.91 (18) | Mg2—O3—K2 | 96.6 (2) |
O3xii—K2—O4ii | 95.2 (3) | Na2xi—O3—K2 | 53.9 (17) |
O1viii—K2—O4ii | 103.8 (3) | K2xi—O3—K2 | 40.6 (4) |
O2xii—K2—O1ii | 123.0 (3) | K1xi—O3—K2 | 42.95 (17) |
O1—K2—O1ii | 67.0 (2) | Mo—O3—K1xiv | 91.70 (14) |
O3xi—K2—O1ii | 133.7 (4) | Mg2—O3—K1xiv | 120.57 (16) |
O3—K2—O1ii | 93.1 (3) | Na2xi—O3—K1xiv | 84.9 (16) |
O2vi—K2—O1ii | 89.5 (3) | K2xi—O3—K1xiv | 95.86 (15) |
O3xii—K2—O1ii | 69.2 (2) | K1xi—O3—K1xiv | 93.8 (2) |
O1viii—K2—O1ii | 59.00 (19) | K2—O3—K1xiv | 127.3 (2) |
O4ii—K2—O1ii | 47.51 (14) | Mo—O3—K2xiv | 90.5 (2) |
O1viii—Na2—O1 | 85 (2) | Mg2—O3—K2xiv | 120.1 (2) |
O1viii—Na2—O3xi | 100 (2) | Na2xi—O3—K2xiv | 87.1 (15) |
O1—Na2—O3xi | 92 (2) | K2xi—O3—K2xiv | 98.1 (4) |
O1viii—Na2—O2xii | 95 (2) | K1xi—O3—K2xiv | 96.08 (15) |
O1—Na2—O2xii | 162 (3) | K2—O3—K2xiv | 129.3 (3) |
O3xi—Na2—O2xii | 70.6 (17) | K1xiv—O3—K2xiv | 2.3 (3) |
O1viii—Na2—O3xii | 80.0 (18) | Mo—O3—K1 | 90.21 (14) |
O1—Na2—O3xii | 139 (3) | Mg2—O3—K1 | 97.09 (16) |
O3xi—Na2—O3xii | 128 (2) | Na2xi—O3—K1 | 56.0 (17) |
O2xii—Na2—O3xii | 57.7 (11) | K2xi—O3—K1 | 42.64 (17) |
O1viii—Na2—O3 | 139 (2) | K1xi—O3—K1 | 45.0 (2) |
O1—Na2—O3 | 56.9 (12) | K2—O3—K1 | 2.1 (3) |
O3xi—Na2—O3 | 95 (2) | K1xiv—O3—K1 | 128.3 (2) |
O2xii—Na2—O3 | 125 (3) | K2xiv—O3—K1 | 130.3 (2) |
O3xii—Na2—O3 | 119 (2) | Mo—O3—Na2xiv | 89.8 (12) |
O1viii—Na2—O1ii | 64.3 (16) | Mg2—O3—Na2xiv | 128.9 (12) |
O1—Na2—O1ii | 70.8 (16) | Na2xi—O3—Na2xiv | 78 (3) |
O3xi—Na2—O1ii | 157 (3) | K2xi—O3—Na2xiv | 87.6 (13) |
O2xii—Na2—O1ii | 125 (2) | K1xi—O3—Na2xiv | 85.8 (14) |
O3xii—Na2—O1ii | 68.6 (13) | K2—O3—Na2xiv | 116.6 (13) |
O3—Na2—O1ii | 88.5 (15) | K1xiv—O3—Na2xiv | 11.0 (13) |
O1viii—Na2—O2viii | 52.4 (13) | K2xiv—O3—Na2xiv | 12.8 (14) |
O1—Na2—O2viii | 115 (2) | K1—O3—Na2xiv | 117.5 (14) |
O3xi—Na2—O2viii | 58.2 (13) | Mo—O3—Na2 | 81.6 (12) |
O2xii—Na2—O2viii | 53.9 (11) | Mg2—O3—Na2 | 105.6 (11) |
O3xii—Na2—O2viii | 84.5 (14) | Na2xi—O3—Na2 | 60 (3) |
O3—Na2—O2viii | 153 (2) | K2xi—O3—Na2 | 47.4 (12) |
O1ii—Na2—O2viii | 114.4 (19) | K1xi—O3—Na2 | 49.6 (12) |
Mo—O1—Na2ix | 121.1 (16) | K2—O3—Na2 | 11.0 (12) |
Mo—O1—Na1 | 140.03 (9) | K1xiv—O3—Na2 | 124.2 (12) |
Na2ix—O1—Na1 | 90.0 (15) | K2xiv—O3—Na2 | 125.9 (13) |
Mo—O1—Na2 | 111.5 (17) | K1—O3—Na2 | 9.5 (11) |
Na2ix—O1—Na2 | 94.3 (9) | Na2xiv—O3—Na2 | 113.2 (19) |
Na1—O1—Na2 | 88.0 (16) | Mo—O3—K2xiii | 73.50 (16) |
Mo—O1—K1 | 100.42 (15) | Mg2—O3—K2xiii | 115.34 (15) |
Na2ix—O1—K1 | 105.6 (16) | Na2xi—O3—K2xiii | 113.9 (15) |
Na1—O1—K1 | 93.50 (11) | K2xi—O3—K2xiii | 124.5 (3) |
Na2—O1—K1 | 12.5 (16) | K1xi—O3—K2xiii | 122.56 (18) |
Mo—O1—K2 | 98.5 (2) | K2—O3—K2xiii | 147.4 (2) |
Na2ix—O1—K2 | 105.9 (15) | K1xiv—O3—K2xiii | 28.96 (17) |
Na1—O1—K2 | 95.6 (2) | K2xiv—O3—K2xiii | 26.7 (3) |
Na2—O1—K2 | 13.9 (16) | K1—O3—K2xiii | 147.3 (2) |
K1—O1—K2 | 2.1 (3) | Na2xiv—O3—K2xiii | 37.0 (13) |
Mo—O1—K1ix | 125.13 (16) | Na2—O3—K2xiii | 139.1 (11) |
Na2ix—O1—K1ix | 7.6 (16) | Mo—O4—Mg1 | 120.81 (7) |
Na1—O1—K1ix | 89.05 (14) | Mo—O4—Mg2v | 136.13 (7) |
Na2—O1—K1ix | 86.7 (16) | Mg1—O4—Mg2v | 95.84 (6) |
K1—O1—K1ix | 98.06 (12) | Mo—O4—K1v | 85.60 (9) |
K2—O1—K1ix | 98.5 (3) | Mg1—O4—K1v | 136.90 (12) |
Mo—O1—K2ix | 124.3 (2) | Mg2v—O4—K1v | 82.19 (10) |
Na2ix—O1—K2ix | 7.3 (16) | Mo—O4—K2v | 86.78 (17) |
Na1—O1—K2ix | 89.9 (2) | Mg1—O4—K2v | 137.17 (19) |
Na2—O1—K2ix | 87.0 (16) | Mg2v—O4—K2v | 80.31 (17) |
K1—O1—K2ix | 98.3 (3) | K1v—O4—K2v | 1.9 (3) |
K2—O1—K2ix | 98.68 (19) | Mo—O4—Na2v | 84.1 (10) |
K1ix—O1—K2ix | 0.9 (3) | Mg1—O4—Na2v | 132.0 (9) |
Mo—O1—K1v | 87.90 (14) | Mg2v—O4—Na2v | 88.4 (11) |
Na2ix—O1—K1v | 75.1 (15) | K1v—O4—Na2v | 7.6 (10) |
Na1—O1—K1v | 75.91 (13) | K2v—O4—Na2v | 9.4 (11) |
Symmetry codes: (i) −x, −x+y, −z+1/2; (ii) −y, x−y, z; (iii) x−y, −y, −z+1/2; (iv) y, x, −z+1/2; (v) −x+y, −x, z; (vi) y+1/3, −x+y+2/3, −z+2/3; (vii) −x+y+2/3, y+1/3, z−1/6; (viii) x−y, x, −z+1; (ix) y, −x+y, −z+1; (x) −x, −y, −z+1; (xi) −x+2/3, −x+y+1/3, −z+5/6; (xii) −y+1/3, −x+2/3, z+1/6; (xiii) x−y+1/3, x−1/3, −z+2/3; (xiv) −y+2/3, −x+1/3, z−1/6. |
Crystal data top
K3NaCo4·6(MoO4) | Dx = 3.703 Mg m−3 |
Mr = 1335.65 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 8646 reflections |
a = 14.4638 (1) Å | θ = 2.6–33.1° |
c = 19.8369 (3) Å | µ = 6.36 mm−1 |
V = 3593.93 (9) Å3 | T = 296 K |
Z = 6 | Fragment, blue |
F(000) = 3720 | 0.05 × 0.05 × 0.03 mm |
Data collection top
Bruker-Nonius X8 APEX CCD diffractometer | 1436 reflections with I > 2σ(I) |
\ f scans, frame data integration | Rint = 0.022 |
Absorption correction: multi-scan SADABS (Bruker, 2005) | θmax = 33.1°, θmin = 2.6° |
Tmin = 0.735, Tmax = 0.826 | h = −17→22 |
8646 measured reflections | k = −22→18 |
1535 independent reflections | l = −30→22 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.015 | w = 1/[σ2(Fo2) + (0.0161P)2 + 6.9365P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.037 | (Δ/σ)max = 0.004 |
S = 1.14 | Δρmax = 0.53 e Å−3 |
1534 reflections | Δρmin = −0.87 e Å−3 |
76 parameters | Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
7 restraints | Extinction coefficient: 0.00012 (2) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo | 0.18671 (2) | 0.00704 (2) | 0.35520 (2) | 0.01455 (5) | |
Co1 | 0.000000 | 0.000000 | 0.250000 | 0.01144 (8) | |
Co2 | 0.21416 (2) | 0.21416 (2) | 0.250000 | 0.01388 (6) | |
Na1 | 0.000000 | 0.000000 | 0.500000 | 0.0319 (4) | |
K1 | 0.2573 (2) | 0.2410 (2) | 0.44224 (17) | 0.0270 (5) | 0.3501 (14) |
K2 | 0.2682 (9) | 0.2456 (8) | 0.4377 (5) | 0.069 (3) | 0.1499 (14) |
O1 | 0.15458 (12) | 0.02484 (12) | 0.43627 (7) | 0.0335 (3) | |
O2 | 0.26342 (10) | −0.05645 (9) | 0.35690 (7) | 0.0246 (2) | |
O3 | 0.26572 (9) | 0.13284 (9) | 0.31640 (7) | 0.0233 (2) | |
O4 | 0.06507 (9) | −0.07307 (9) | 0.30783 (6) | 0.01682 (19) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo | 0.01466 (6) | 0.01531 (6) | 0.01417 (7) | 0.00786 (4) | −0.00291 (4) | −0.00140 (4) |
Co1 | 0.01007 (11) | 0.01007 (11) | 0.0142 (2) | 0.00504 (5) | 0.000 | 0.000 |
Co2 | 0.01178 (9) | 0.01178 (9) | 0.01683 (13) | 0.00494 (9) | 0.00090 (5) | −0.00090 (5) |
Na1 | 0.0359 (6) | 0.0359 (6) | 0.0239 (9) | 0.0179 (3) | 0.000 | 0.000 |
K1 | 0.0370 (8) | 0.0188 (9) | 0.0253 (10) | 0.0141 (6) | −0.0053 (7) | −0.0042 (7) |
K2 | 0.141 (8) | 0.042 (4) | 0.044 (4) | 0.060 (5) | −0.059 (4) | −0.026 (3) |
O1 | 0.0341 (7) | 0.0440 (8) | 0.0189 (6) | 0.0170 (6) | −0.0003 (5) | −0.0077 (5) |
O2 | 0.0226 (5) | 0.0209 (5) | 0.0336 (7) | 0.0134 (4) | −0.0075 (5) | 0.0013 (5) |
O3 | 0.0177 (5) | 0.0185 (5) | 0.0318 (6) | 0.0075 (4) | −0.0042 (4) | 0.0034 (4) |
O4 | 0.0166 (4) | 0.0148 (4) | 0.0198 (5) | 0.0084 (4) | −0.0048 (4) | −0.0013 (4) |
Geometric parameters (Å, º) top
Mo—O1 | 1.7288 (14) | K1—K1xi | 2.157 (5) |
Mo—O2 | 1.7589 (12) | K1—O2xii | 2.699 (4) |
Mo—O3 | 1.7691 (12) | K1—O1 | 2.712 (3) |
Mo—O4 | 1.8117 (11) | K1—O3xi | 2.841 (4) |
Co1—O4i | 2.0769 (10) | K1—O1ix | 2.910 (3) |
Co1—O4ii | 2.0769 (10) | K1—O3xii | 2.930 (3) |
Co1—O4iii | 2.0769 (10) | K1—O3 | 2.981 (4) |
Co1—O4iv | 2.0769 (10) | K1—O2vi | 2.982 (4) |
Co1—O4v | 2.0769 (10) | K1—O4i | 3.530 (4) |
Co1—O4 | 2.0770 (10) | K1—O1i | 3.563 (3) |
Co2—O2vi | 2.0417 (12) | K1—O2i | 3.990 (4) |
Co2—O2vii | 2.0417 (12) | K1—O2ix | 4.063 (4) |
Co2—O4iv | 2.1085 (11) | K2—K2xi | 1.83 (2) |
Co2—O4i | 2.1085 (11) | K2—O2xii | 2.680 (9) |
Co2—O3 | 2.1335 (12) | K2—O1 | 2.765 (10) |
Co2—O3iii | 2.1335 (12) | K2—O3xi | 2.799 (10) |
Na1—O1viii | 2.4336 (15) | K2—O3 | 2.897 (10) |
Na1—O1i | 2.4336 (15) | K2—O2vi | 2.902 (10) |
Na1—O1ix | 2.4336 (15) | K2—O3xii | 3.003 (10) |
Na1—O1v | 2.4336 (15) | K2—O1ix | 3.059 (11) |
Na1—O1 | 2.4336 (15) | K2—O4i | 3.554 (9) |
Na1—O1x | 2.4337 (15) | K2—O1i | 3.698 (11) |
K1—K2 | 0.163 (14) | K2—O1xi | 3.950 (11) |
K1—K2xi | 1.995 (10) | | |
| | | |
O1—Mo—O2 | 110.28 (7) | O3xi—K2—O1xi | 46.32 (17) |
O1—Mo—O3 | 109.57 (7) | O3—K2—O1xi | 60.3 (2) |
O2—Mo—O3 | 107.08 (6) | O2vi—K2—O1xi | 94.7 (3) |
O1—Mo—O4 | 109.28 (6) | O3xii—K2—O1xi | 145.7 (3) |
O2—Mo—O4 | 109.90 (5) | O1ix—K2—O1xi | 122.9 (3) |
O3—Mo—O4 | 110.70 (6) | O4i—K2—O1xi | 111.1 (3) |
O4i—Co1—O4ii | 176.81 (6) | O1i—K2—O1xi | 146.9 (3) |
O4i—Co1—O4iii | 89.92 (6) | Mo—O1—Na1 | 139.19 (8) |
O4ii—Co1—O4iii | 92.43 (4) | Mo—O1—K1 | 100.32 (9) |
O4i—Co1—O4iv | 85.31 (6) | Na1—O1—K1 | 94.65 (7) |
O4ii—Co1—O4iv | 92.43 (4) | Mo—O1—K2 | 97.6 (2) |
O4iii—Co1—O4iv | 92.43 (4) | Na1—O1—K2 | 97.9 (2) |
O4i—Co1—O4v | 92.43 (4) | K1—O1—K2 | 3.2 (3) |
O4ii—Co1—O4v | 89.92 (6) | Mo—O1—K1viii | 124.39 (10) |
O4iii—Co1—O4v | 85.31 (6) | Na1—O1—K1viii | 89.81 (8) |
O4iv—Co1—O4v | 176.81 (6) | K1—O1—K1viii | 98.96 (7) |
O4i—Co1—O4 | 92.43 (4) | K2—O1—K1viii | 99.2 (2) |
O4ii—Co1—O4 | 85.31 (6) | Mo—O1—K2viii | 123.3 (2) |
O4iii—Co1—O4 | 176.81 (6) | Na1—O1—K2viii | 90.52 (18) |
O4iv—Co1—O4 | 89.92 (6) | K1—O1—K2viii | 100.0 (2) |
O4v—Co1—O4 | 92.43 (4) | K2—O1—K2viii | 100.17 (18) |
O2vi—Co2—O2vii | 92.42 (7) | K1viii—O1—K2viii | 1.3 (2) |
O2vi—Co2—O4iv | 175.60 (5) | Mo—O1—K1v | 86.81 (8) |
O2vii—Co2—O4iv | 91.92 (5) | Na1—O1—K1v | 75.74 (7) |
O2vi—Co2—O4i | 91.92 (5) | K1—O1—K1v | 170.36 (9) |
O2vii—Co2—O4i | 175.60 (5) | K2—O1—K1v | 173.5 (3) |
O4iv—Co2—O4i | 83.74 (6) | K1viii—O1—K1v | 82.02 (8) |
O2vi—Co2—O3 | 92.63 (5) | K2viii—O1—K1v | 81.1 (2) |
O2vii—Co2—O3 | 95.38 (5) | Mo—O1—K2v | 85.44 (16) |
O4iv—Co2—O3 | 87.66 (5) | Na1—O1—K2v | 76.56 (16) |
O4i—Co2—O3 | 83.71 (5) | K1—O1—K2v | 170.98 (19) |
O2vi—Co2—O3iii | 95.38 (5) | K2—O1—K2v | 174.0 (3) |
O2vii—Co2—O3iii | 92.63 (5) | K1viii—O1—K2v | 83.20 (18) |
O4iv—Co2—O3iii | 83.71 (5) | K2viii—O1—K2v | 82.28 (18) |
O4i—Co2—O3iii | 87.66 (5) | K1v—O1—K2v | 1.5 (2) |
O3—Co2—O3iii | 168.42 (6) | Mo—O1—K2xi | 78.47 (15) |
O1viii—Na1—O1i | 180.00 (6) | Na1—O1—K2xi | 122.30 (16) |
O1viii—Na1—O1ix | 95.47 (5) | K1—O1—K2xi | 27.65 (16) |
O1i—Na1—O1ix | 84.53 (5) | K2—O1—K2xi | 24.4 (3) |
O1viii—Na1—O1v | 84.53 (5) | K1viii—O1—K2xi | 97.64 (17) |
O1i—Na1—O1v | 95.47 (5) | K2viii—O1—K2xi | 98.20 (18) |
O1ix—Na1—O1v | 180.00 (7) | K1v—O1—K2xi | 161.9 (2) |
O1viii—Na1—O1 | 84.54 (5) | K2v—O1—K2xi | 161.06 (7) |
O1i—Na1—O1 | 95.46 (5) | Mo—O1—K1xi | 77.25 (7) |
O1ix—Na1—O1 | 84.54 (5) | Na1—O1—K1xi | 123.63 (7) |
O1v—Na1—O1 | 95.46 (5) | K1—O1—K1xi | 28.99 (7) |
O1viii—Na1—O1x | 95.47 (5) | K2—O1—K1xi | 25.8 (2) |
O1i—Na1—O1x | 84.53 (5) | K1viii—O1—K1xi | 97.80 (8) |
O1ix—Na1—O1x | 95.46 (5) | K2viii—O1—K1xi | 98.3 (2) |
O1v—Na1—O1x | 84.54 (5) | K1v—O1—K1xi | 160.60 (5) |
O1—Na1—O1x | 180.0 | K2v—O1—K1xi | 159.7 (2) |
O2xii—K1—O3xi | 66.01 (8) | K2xi—O1—K1xi | 1.36 (19) |
O1—K1—O3xi | 79.65 (10) | Mo—O2—Co2xiii | 145.58 (8) |
O2xii—K1—O1ix | 84.29 (10) | Mo—O2—K2xiv | 101.4 (2) |
O1—K1—O1ix | 71.12 (8) | Co2xiii—O2—K2xiv | 102.3 (2) |
O3xi—K1—O1ix | 81.46 (10) | Mo—O2—K1xiv | 99.75 (9) |
O2xii—K1—O3xii | 60.38 (8) | Co2xiii—O2—K1xiv | 102.39 (9) |
O1—K1—O3xii | 135.56 (10) | K2xiv—O2—K1xiv | 3.5 (3) |
O3xi—K1—O3xii | 122.79 (12) | Mo—O2—K2xiii | 115.52 (19) |
O1ix—K1—O3xii | 75.06 (8) | Co2xiii—O2—K2xiii | 98.45 (19) |
O2xii—K1—O3 | 139.43 (10) | K2xiv—O2—K2xiii | 38.1 (5) |
O1—K1—O3 | 60.05 (8) | K1xiv—O2—K2xiii | 41.5 (2) |
O3xi—K1—O3 | 95.88 (10) | Mo—O2—K1xiii | 115.81 (9) |
O1ix—K1—O3 | 130.65 (11) | Co2xiii—O2—K1xiii | 98.40 (8) |
O3xii—K1—O3 | 138.34 (14) | K2xiv—O2—K1xiii | 40.8 (2) |
O2xii—K1—O2vi | 103.70 (11) | K1xiv—O2—K1xiii | 44.29 (10) |
O1—K1—O2vi | 114.19 (12) | K2xiii—O2—K1xiii | 2.8 (3) |
O3xi—K1—O2vi | 132.37 (9) | Mo—O2—K1v | 73.37 (6) |
O1ix—K1—O2vi | 145.81 (12) | Co2xiii—O2—K1v | 88.69 (6) |
O3xii—K1—O2vi | 80.25 (9) | K2xiv—O2—K1v | 165.4 (2) |
O3—K1—O2vi | 60.86 (7) | K1xiv—O2—K1v | 167.33 (11) |
O2xii—K1—O4i | 151.19 (13) | K2xiii—O2—K1v | 131.4 (2) |
O1—K1—O4i | 67.53 (8) | K1xiii—O2—K1v | 128.65 (6) |
O3xi—K1—O4i | 141.50 (12) | Mo—O2—K2v | 74.33 (15) |
O1ix—K1—O4i | 105.15 (8) | Co2xiii—O2—K2v | 88.84 (14) |
O3xii—K1—O4i | 95.21 (9) | K2xiv—O2—K2v | 163.8 (3) |
O3—K1—O4i | 50.68 (6) | K1xiv—O2—K2v | 166.04 (14) |
O2vi—K1—O4i | 53.74 (6) | K2xiii—O2—K2v | 129.25 (16) |
O2xii—K1—O1i | 124.58 (10) | K1xiii—O2—K2v | 126.50 (18) |
O1—K1—O1i | 68.52 (8) | K1v—O2—K2v | 2.17 (19) |
O3xi—K1—O1i | 135.61 (10) | Mo—O2—K1viii | 80.10 (6) |
O1ix—K1—O1i | 59.75 (6) | Co2xiii—O2—K1viii | 65.58 (5) |
O3xii—K1—O1i | 69.86 (7) | K2xiv—O2—K1viii | 129.2 (3) |
O3—K1—O1i | 94.19 (9) | K1xiv—O2—K1viii | 126.01 (8) |
O2vi—K1—O1i | 89.76 (9) | K2xiii—O2—K1viii | 159.3 (2) |
O4i—K1—O1i | 48.05 (5) | K1xiii—O2—K1viii | 160.86 (6) |
O2xii—K1—O2i | 107.88 (10) | K1v—O2—K1viii | 64.14 (6) |
O1—K1—O2i | 104.68 (10) | K2v—O2—K1viii | 66.14 (16) |
O3xi—K1—O2i | 172.86 (12) | Mo—O2—K2viii | 82.18 (16) |
O1ix—K1—O2i | 94.48 (8) | Co2xiii—O2—K2viii | 63.49 (16) |
O3xii—K1—O2i | 50.19 (6) | K2xiv—O2—K2viii | 129.2 (2) |
O3—K1—O2i | 91.22 (9) | K1xiv—O2—K2viii | 126.14 (17) |
O2vi—K1—O2i | 51.35 (6) | K2xiii—O2—K2viii | 157.9 (2) |
O4i—K1—O2i | 45.24 (5) | K1xiii—O2—K2viii | 159.24 (19) |
O1i—K1—O2i | 44.08 (5) | K1v—O2—K2viii | 64.33 (15) |
O2xii—K1—O2ix | 46.48 (7) | K2v—O2—K2viii | 66.3 (2) |
O1—K1—O2ix | 96.12 (10) | K1viii—O2—K2viii | 2.10 (19) |
O3xi—K1—O2ix | 49.34 (6) | Mo—O3—Co2 | 127.70 (6) |
O1ix—K1—O2ix | 44.78 (6) | Mo—O3—K2xi | 119.7 (2) |
O3xii—K1—O2ix | 78.76 (8) | Co2—O3—K2xi | 96.2 (2) |
O3—K1—O2ix | 142.87 (11) | Mo—O3—K1xi | 122.07 (9) |
O2vi—K1—O2ix | 149.67 (10) | Co2—O3—K1xi | 95.64 (8) |
O4i—K1—O2ix | 149.93 (7) | K2xi—O3—K1xi | 3.2 (3) |
O1i—K1—O2ix | 103.16 (7) | Mo—O3—K2 | 92.1 (2) |
O2i—K1—O2ix | 123.93 (8) | Co2—O3—K2 | 96.43 (19) |
O2xii—K2—O1 | 138.4 (4) | K2xi—O3—K2 | 37.5 (4) |
O2xii—K2—O3xi | 66.9 (2) | K1xi—O3—K2 | 40.7 (2) |
O1—K2—O3xi | 79.5 (3) | Mo—O3—K1xiv | 91.50 (8) |
O2xii—K2—O3 | 145.6 (5) | Co2—O3—K1xiv | 121.78 (9) |
O1—K2—O3 | 60.6 (2) | K2xi—O3—K1xiv | 97.94 (19) |
O3xi—K2—O3 | 98.7 (3) | K1xi—O3—K1xiv | 95.61 (11) |
O2xii—K2—O2vi | 106.4 (3) | K2—O3—K1xiv | 126.7 (2) |
O1—K2—O2vi | 115.1 (3) | Mo—O3—K1 | 90.05 (8) |
O3xi—K2—O2vi | 138.3 (4) | Co2—O3—K1 | 96.34 (8) |
O3—K2—O2vi | 62.8 (2) | K2xi—O3—K1 | 40.2 (2) |
O2xii—K2—O3xii | 59.6 (2) | K1xi—O3—K1 | 43.41 (9) |
O1—K2—O3xii | 129.7 (4) | K2—O3—K1 | 2.7 (3) |
O3xi—K2—O3xii | 121.7 (3) | K1xiv—O3—K1 | 128.60 (11) |
O3—K2—O3xii | 138.9 (3) | Mo—O3—K2xiv | 89.9 (2) |
O2vi—K2—O3xii | 80.4 (2) | Co2—O3—K2xiv | 121.31 (18) |
O2xii—K2—O1ix | 81.8 (3) | K2xi—O3—K2xiv | 100.8 (4) |
O1—K2—O1ix | 68.2 (2) | K1xi—O3—K2xiv | 98.43 (19) |
O3xi—K2—O1ix | 79.6 (2) | K2—O3—K2xiv | 129.2 (3) |
O3—K2—O1ix | 128.0 (4) | K1xiv—O3—K2xiv | 2.8 (3) |
O2vi—K2—O1ix | 141.8 (4) | K1—O3—K2xiv | 131.0 (2) |
O3xii—K2—O1ix | 71.9 (2) | Mo—O3—K2xiii | 74.45 (14) |
O2xii—K2—O4i | 150.7 (4) | Co2—O3—K2xiii | 116.55 (14) |
O1—K2—O4i | 66.7 (2) | K2xi—O3—K2xiii | 124.8 (2) |
O3xi—K2—O4i | 142.4 (3) | K1xi—O3—K2xiii | 122.64 (16) |
O3—K2—O4i | 50.80 (15) | K2—O3—K2xiii | 146.1 (2) |
O2vi—K2—O4i | 53.91 (15) | K1xiv—O3—K2xiii | 27.26 (15) |
O3xii—K2—O4i | 93.4 (3) | K1—O3—K2xiii | 146.69 (16) |
O1ix—K2—O4i | 101.4 (3) | K2xiv—O3—K2xiii | 24.5 (3) |
O2xii—K2—O1i | 120.4 (3) | Mo—O4—Co1 | 120.22 (6) |
O1—K2—O1i | 65.9 (2) | Mo—O4—Co2v | 136.21 (6) |
O3xi—K2—O1i | 131.6 (4) | Co1—O4—Co2v | 95.48 (5) |
O3—K2—O1i | 92.8 (3) | Mo—O4—K1v | 86.66 (6) |
O2vi—K2—O1i | 88.4 (2) | Co1—O4—K1v | 137.44 (7) |
O3xii—K2—O1i | 67.2 (2) | Co2v—O4—K1v | 82.02 (5) |
O1ix—K2—O1i | 57.0 (2) | Mo—O4—K2v | 88.78 (18) |
O4i—K2—O1i | 46.88 (13) | Co1—O4—K2v | 137.05 (16) |
O2xii—K2—O1xi | 90.2 (3) | Co2v—O4—K2v | 79.43 (19) |
O1—K2—O1xi | 83.2 (3) | K1v—O4—K2v | 2.6 (2) |
Symmetry codes: (i) −y, x−y, z; (ii) −x, −x+y, −z+1/2; (iii) y, x, −z+1/2; (iv) x−y, −y, −z+1/2; (v) −x+y, −x, z; (vi) y+1/3, −x+y+2/3, −z+2/3; (vii) −x+y+2/3, y+1/3, z−1/6; (viii) y, −x+y, −z+1; (ix) x−y, x, −z+1; (x) −x, −y, −z+1; (xi) −x+2/3, −x+y+1/3, −z+5/6; (xii) −y+1/3, −x+2/3, z+1/6; (xiii) x−y+1/3, x−1/3, −z+2/3; (xiv) −y+2/3, −x+1/3, z−1/6. |
Crystal data top
K3.11Li0.89Mg4·6(MoO4) | Dx = 3.352 Mg m−3 |
Mr = 1184.71 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 12163 reflections |
a = 14.3541 (2) Å | θ = 2.6–33.1° |
c = 19.7338 (4) Å | µ = 3.87 mm−1 |
V = 3521.22 (12) Å3 | T = 296 K |
Z = 6 | Fragment, colourless |
F(000) = 3323 | 0.14 × 0.08 × 0.06 mm |
Data collection top
Bruker-Nonius X8 APEX CCD diffractometer | 1356 reflections with I > 2σ(I) |
\ f scans, frame data integration | Rint = 0.027 |
Absorption correction: multi-scan SADABS (Bruker, 2005) | θmax = 33.1°, θmin = 2.6° |
Tmin = 0.697, Tmax = 0.793 | h = −20→22 |
12163 measured reflections | k = −22→12 |
1502 independent reflections | l = −27→30 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.018 | w = 1/[σ2(Fo2) + (0.0144P)2 + 19.5824P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.042 | (Δ/σ)max = 0.013 |
S = 1.06 | Δρmax = 1.54 e Å−3 |
1501 reflections | Δρmin = −1.48 e Å−3 |
77 parameters | Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.000104 (17) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo | 0.17938 (2) | 0.00765 (2) | 0.35913 (2) | 0.01155 (5) | |
Mg1 | 0.000000 | 0.000000 | 0.250000 | 0.0165 (16) | 0.112 (9) |
Li1 | 0.000000 | 0.000000 | 0.250000 | 0.0165 (16) | 0.888 (9) |
Mg2 | 0.21366 (6) | 0.21366 (6) | 0.250000 | 0.01093 (16) | |
Mg3 | 0.000000 | 0.000000 | 0.500000 | 0.0154 (4) | 0.888 (9) |
K3 | 0.000000 | 0.000000 | 0.500000 | 0.0154 (4) | 0.112 (9) |
K1 | 0.25444 (19) | 0.2466 (2) | 0.44311 (18) | 0.0245 (4) | 0.4561 (14) |
K2 | 0.382 (2) | 0.311 (3) | 0.4004 (18) | 0.030 (5) | 0.0440 (14) |
O1 | 0.13373 (14) | 0.02087 (14) | 0.43942 (8) | 0.0258 (3) | |
O2 | 0.25663 (13) | −0.05555 (13) | 0.36431 (9) | 0.0241 (3) | |
O3 | 0.26204 (11) | 0.13543 (12) | 0.32224 (8) | 0.0176 (3) | |
O4 | 0.06674 (11) | −0.07315 (11) | 0.30737 (7) | 0.0142 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo | 0.01206 (8) | 0.01108 (8) | 0.01089 (8) | 0.00531 (6) | −0.00325 (5) | −0.00035 (5) |
Mg1 | 0.015 (2) | 0.015 (2) | 0.019 (3) | 0.0075 (10) | 0.000 | 0.000 |
Li1 | 0.015 (2) | 0.015 (2) | 0.019 (3) | 0.0075 (10) | 0.000 | 0.000 |
Mg2 | 0.0094 (3) | 0.0094 (3) | 0.0125 (4) | 0.0037 (3) | 0.00088 (15) | −0.00088 (15) |
Mg3 | 0.0179 (5) | 0.0179 (5) | 0.0104 (7) | 0.0089 (3) | 0.000 | 0.000 |
K3 | 0.0179 (5) | 0.0179 (5) | 0.0104 (7) | 0.0089 (3) | 0.000 | 0.000 |
K1 | 0.0300 (11) | 0.0176 (10) | 0.0264 (9) | 0.0124 (9) | −0.0083 (8) | −0.0076 (7) |
K2 | 0.038 (13) | 0.033 (12) | 0.032 (13) | 0.027 (12) | −0.018 (10) | −0.015 (9) |
O1 | 0.0292 (8) | 0.0289 (8) | 0.0137 (7) | 0.0104 (7) | 0.0008 (6) | −0.0044 (6) |
O2 | 0.0221 (7) | 0.0199 (7) | 0.0337 (9) | 0.0131 (6) | −0.0092 (6) | 0.0023 (6) |
O3 | 0.0137 (6) | 0.0144 (6) | 0.0220 (7) | 0.0050 (5) | −0.0017 (5) | 0.0033 (5) |
O4 | 0.0152 (6) | 0.0126 (6) | 0.0153 (6) | 0.0073 (5) | −0.0057 (5) | −0.0031 (5) |
Geometric parameters (Å, º) top
Mo—O2 | 1.7519 (16) | K1—K1xi | 2.222 (4) |
Mo—O1 | 1.7606 (16) | K1—O2xii | 2.776 (4) |
Mo—O3 | 1.7680 (14) | K1—O1 | 2.810 (3) |
Mo—O4 | 1.7685 (14) | K1—O3xi | 2.830 (4) |
Mg1—O4i | 2.0755 (13) | K1—O3 | 2.902 (4) |
Mg1—O4ii | 2.0755 (13) | K1—O3xii | 2.908 (4) |
Mg1—O4iii | 2.0755 (13) | K1—O1viii | 2.973 (3) |
Mg1—O4 | 2.0755 (13) | K1—O2vi | 3.115 (4) |
Mg1—O4iv | 2.0755 (13) | K1—O1iii | 3.424 (3) |
Mg1—O4v | 2.0756 (13) | K1—O4iii | 3.508 (4) |
Mg2—O2vi | 2.0346 (16) | K1—O2iii | 3.760 (4) |
Mg2—O2vii | 2.0346 (16) | K2—K2xi | 1.37 (5) |
Mg2—O4iv | 2.0821 (15) | K2—O2vi | 2.70 (4) |
Mg2—O4iii | 2.0821 (15) | K2—O3 | 2.71 (4) |
Mg2—O3v | 2.1342 (14) | K2—O3xi | 2.76 (4) |
Mg2—O3 | 2.1343 (14) | K2—O2xii | 2.92 (4) |
Mg3—O1 | 2.1514 (17) | K2—O1xi | 3.04 (3) |
Mg3—O1viii | 2.1514 (17) | K2—O3vi | 3.08 (4) |
Mg3—O1ii | 2.1514 (17) | K2—O1vii | 3.36 (3) |
Mg3—O1ix | 2.1514 (17) | K2—O4xiii | 3.62 (3) |
Mg3—O1iii | 2.1514 (17) | K2—O1xiii | 3.80 (3) |
Mg3—O1x | 2.1514 (17) | K2—O3xii | 3.92 (3) |
K1—K2xi | 0.43 (3) | K2—O2xiii | 3.94 (3) |
K1—K2 | 1.79 (3) | | |
| | | |
O2—Mo—O1 | 111.68 (9) | O4xiii—K2—O3xii | 99.5 (8) |
O2—Mo—O3 | 106.92 (7) | O1xiii—K2—O3xii | 126.2 (9) |
O1—Mo—O3 | 110.59 (8) | O2vi—K2—O2xiii | 106.8 (11) |
O2—Mo—O4 | 107.57 (7) | O3—K2—O2xiii | 163.6 (10) |
O1—Mo—O4 | 108.84 (7) | O3xi—K2—O2xiii | 90.8 (9) |
O3—Mo—O4 | 111.21 (7) | O2xii—K2—O2xiii | 52.7 (6) |
O4i—Mg1—O4ii | 88.79 (8) | O1xi—K2—O2xiii | 92.1 (7) |
O4i—Mg1—O4iii | 177.46 (8) | O3vi—K2—O2xiii | 49.6 (5) |
O4ii—Mg1—O4iii | 93.08 (5) | O1vii—K2—O2xiii | 84.7 (6) |
O4i—Mg1—O4 | 85.11 (7) | O4xiii—K2—O2xiii | 43.9 (4) |
O4ii—Mg1—O4 | 93.07 (5) | O1xiii—K2—O2xiii | 44.1 (3) |
O4iii—Mg1—O4 | 93.07 (5) | O3xii—K2—O2xiii | 82.1 (7) |
O4i—Mg1—O4iv | 93.08 (5) | Mo—O1—Mg3 | 147.07 (10) |
O4ii—Mg1—O4iv | 177.46 (8) | Mo—O1—K1 | 95.71 (9) |
O4iii—Mg1—O4iv | 85.10 (7) | Mg3—O1—K1 | 97.99 (8) |
O4—Mg1—O4iv | 88.80 (8) | Mo—O1—K1ix | 115.39 (11) |
O4i—Mg1—O4v | 93.08 (5) | Mg3—O1—K1ix | 93.30 (8) |
O4ii—Mg1—O4v | 85.11 (7) | K1—O1—K1ix | 94.30 (8) |
O4iii—Mg1—O4v | 88.80 (8) | Mo—O1—K2xi | 89.6 (7) |
O4—Mg1—O4v | 177.46 (8) | Mg3—O1—K2xi | 105.1 (6) |
O4iv—Mg1—O4v | 93.08 (5) | K1—O1—K2xi | 7.1 (6) |
O2vi—Mg2—O2vii | 87.41 (10) | K1ix—O1—K2xi | 93.7 (7) |
O2vi—Mg2—O4iv | 175.39 (6) | Mo—O1—K2xiv | 112.7 (6) |
O2vii—Mg2—O4iv | 94.08 (6) | Mg3—O1—K2xiv | 95.3 (6) |
O2vi—Mg2—O4iii | 94.08 (6) | K1—O1—K2xiv | 96.5 (7) |
O2vii—Mg2—O4iii | 175.39 (6) | K1ix—O1—K2xiv | 3.3 (6) |
O4iv—Mg2—O4iii | 84.77 (8) | K2xi—O1—K2xiv | 95.6 (7) |
O2vi—Mg2—O3v | 93.79 (7) | Mo—O1—K1ii | 86.14 (8) |
O2vii—Mg2—O3v | 94.53 (7) | Mg3—O1—K1ii | 81.62 (8) |
O4iv—Mg2—O3v | 81.75 (6) | K1—O1—K1ii | 176.97 (14) |
O4iii—Mg2—O3v | 89.73 (6) | K1ix—O1—K1ii | 82.73 (8) |
O2vi—Mg2—O3 | 94.53 (7) | K2xi—O1—K1ii | 172.6 (6) |
O2vii—Mg2—O3 | 93.79 (7) | K2xiv—O1—K1ii | 80.5 (6) |
O4iv—Mg2—O3 | 89.73 (6) | Mo—O1—K2xv | 83.2 (5) |
O4iii—Mg2—O3 | 81.75 (6) | Mg3—O1—K2xv | 83.6 (5) |
O3v—Mg2—O3 | 168.48 (9) | K1—O1—K2xv | 178.3 (6) |
O1—Mg3—O1viii | 87.89 (6) | K1ix—O1—K2xv | 85.0 (6) |
O1—Mg3—O1ii | 92.11 (6) | K2xi—O1—K2xv | 171.3 (6) |
O1viii—Mg3—O1ii | 180.0 | K2xiv—O1—K2xv | 82.7 (6) |
O1—Mg3—O1ix | 87.89 (6) | K1ii—O1—K2xv | 3.2 (6) |
O1viii—Mg3—O1ix | 92.11 (6) | Mo—O1—K2 | 75.6 (5) |
O1ii—Mg3—O1ix | 87.89 (6) | Mg3—O1—K2 | 121.5 (4) |
O1—Mg3—O1iii | 92.11 (6) | K1—O1—K2 | 23.5 (5) |
O1viii—Mg3—O1iii | 87.89 (6) | K1ix—O1—K2 | 91.8 (6) |
O1ii—Mg3—O1iii | 92.11 (6) | K2xi—O1—K2 | 16.5 (7) |
O1ix—Mg3—O1iii | 180.00 (7) | K2xiv—O1—K2 | 92.9 (6) |
O1—Mg3—O1x | 180.0 | K1ii—O1—K2 | 156.6 (5) |
O1viii—Mg3—O1x | 92.11 (6) | K2xv—O1—K2 | 154.8 (2) |
O1ii—Mg3—O1x | 87.89 (6) | Mo—O2—Mg2xvi | 152.83 (11) |
O1ix—Mg3—O1x | 92.11 (6) | Mo—O2—K2xvi | 101.3 (7) |
O1iii—Mg3—O1x | 87.89 (6) | Mg2xvi—O2—K2xvi | 99.4 (8) |
O2xii—K1—O1 | 139.29 (15) | Mo—O2—K1xvii | 97.88 (10) |
O2xii—K1—O3xi | 66.22 (9) | Mg2xvi—O2—K1xvii | 99.87 (10) |
O1—K1—O3xi | 82.63 (10) | K2xvi—O2—K1xvii | 8.8 (6) |
O2xii—K1—O3 | 140.95 (9) | Mo—O2—K2xvii | 110.7 (7) |
O1—K1—O3 | 61.01 (8) | Mg2xvi—O2—K2xvii | 95.8 (7) |
O3xi—K1—O3 | 92.08 (10) | K2xvi—O2—K2xvii | 27.8 (10) |
O2xii—K1—O3xii | 59.62 (8) | K1xvii—O2—K2xvii | 36.6 (5) |
O1—K1—O3xii | 130.98 (9) | Mo—O2—K1xvi | 112.65 (9) |
O3xi—K1—O3xii | 123.25 (12) | Mg2xvi—O2—K1xvi | 94.37 (8) |
O3—K1—O3xii | 141.82 (15) | K2xvi—O2—K1xvi | 35.0 (5) |
O2xii—K1—O1viii | 88.31 (11) | K1xvii—O2—K1xvi | 43.84 (8) |
O1—K1—O1viii | 62.11 (8) | K2xvii—O2—K1xvi | 7.2 (5) |
O3xi—K1—O1viii | 84.39 (10) | Mo—O2—K1ii | 75.95 (7) |
O3—K1—O1viii | 122.99 (11) | Mg2xvi—O2—K1ii | 90.90 (7) |
O3xii—K1—O1viii | 78.56 (8) | K2xvi—O2—K1ii | 158.5 (6) |
O2xii—K1—O2vi | 106.29 (10) | K1xvii—O2—K1ii | 165.33 (11) |
O1—K1—O2vi | 113.64 (12) | K2xvii—O2—K1ii | 132.9 (6) |
O3xi—K1—O2vi | 128.29 (9) | K1xvi—O2—K1ii | 125.91 (7) |
O3—K1—O2vi | 61.07 (8) | Mo—O2—K1ix | 82.91 (7) |
O3xii—K1—O2vi | 83.81 (10) | Mg2xvi—O2—K1ix | 70.03 (6) |
O1viii—K1—O2vi | 147.20 (12) | K2xvi—O2—K1ix | 133.8 (6) |
O2xii—K1—O1iii | 127.38 (11) | K1xvii—O2—K1ix | 125.62 (8) |
O1—K1—O1iii | 58.62 (8) | K2xvii—O2—K1ix | 156.8 (7) |
O3xi—K1—O1iii | 132.76 (11) | K1xvi—O2—K1ix | 160.70 (7) |
O3—K1—O1iii | 91.39 (9) | K1ii—O2—K1ix | 67.44 (7) |
O3xii—K1—O1iii | 75.53 (7) | Mo—O2—K2xv | 79.1 (5) |
O1viii—K1—O1iii | 55.11 (6) | Mg2xvi—O2—K2xv | 90.1 (5) |
O2vi—K1—O1iii | 93.84 (10) | K2xvi—O2—K2xv | 153.7 (10) |
O2xii—K1—O4iii | 153.70 (13) | K1xvii—O2—K2xv | 161.5 (5) |
O1—K1—O4iii | 65.25 (8) | K2xvii—O2—K2xv | 127.3 (6) |
O3xi—K1—O4iii | 138.35 (12) | K1xvi—O2—K2xv | 120.3 (4) |
O3—K1—O4iii | 49.90 (7) | K1ii—O2—K2xv | 5.8 (4) |
O3xii—K1—O4iii | 98.20 (10) | K1ix—O2—K2xv | 72.5 (5) |
O1viii—K1—O4iii | 101.64 (8) | Mo—O2—K2xiv | 88.7 (4) |
O2vi—K1—O4iii | 53.72 (7) | Mg2xvi—O2—K2xiv | 64.2 (4) |
O1iii—K1—O4iii | 48.90 (5) | K2xvi—O2—K2xiv | 133.0 (6) |
O2xii—K1—O2iii | 109.94 (10) | K1xvii—O2—K2xiv | 125.3 (5) |
O1—K1—O2iii | 99.81 (9) | K2xvii—O2—K2xiv | 153.1 (5) |
O3xi—K1—O2iii | 175.62 (12) | K1xvi—O2—K2xiv | 155.9 (4) |
O3—K1—O2iii | 92.28 (10) | K1ii—O2—K2xiv | 68.5 (5) |
O3xii—K1—O2iii | 52.46 (6) | K1ix—O2—K2xiv | 5.8 (4) |
O1viii—K1—O2iii | 93.51 (8) | K2xv—O2—K2xiv | 73.2 (6) |
O2vi—K1—O2iii | 54.09 (7) | Mo—O3—Mg2 | 126.49 (8) |
O1iii—K1—O2iii | 47.45 (6) | Mo—O3—K2 | 121.0 (7) |
O4iii—K1—O2iii | 45.84 (5) | Mg2—O3—K2 | 96.4 (8) |
O2vi—K2—O3 | 68.9 (9) | Mo—O3—K2xi | 99.0 (6) |
O2vi—K2—O3xi | 157.2 (11) | Mg2—O3—K2xi | 98.2 (7) |
O3—K2—O3xi | 97.9 (12) | K2—O3—K2xi | 28.9 (10) |
O2vi—K2—O2xii | 114.2 (11) | Mo—O3—K1xi | 126.69 (9) |
O3—K2—O2xii | 143.7 (11) | Mg2—O3—K1xi | 95.78 (9) |
O3xi—K2—O2xii | 65.2 (8) | K2—O3—K1xi | 8.5 (5) |
O2vi—K2—O1xi | 131.6 (12) | K2xi—O3—K1xi | 37.4 (5) |
O3—K2—O1xi | 80.5 (9) | Mo—O3—K1 | 92.40 (8) |
O3xi—K2—O1xi | 59.8 (7) | Mg2—O3—K1 | 98.51 (9) |
O2xii—K2—O1xi | 112.7 (12) | K2—O3—K1 | 37.1 (6) |
O2vi—K2—O3vi | 58.2 (7) | K2xi—O3—K1 | 8.2 (5) |
O3—K2—O3vi | 121.2 (13) | K1xi—O3—K1 | 45.58 (8) |
O3xi—K2—O3vi | 140.3 (13) | Mo—O3—K1xvii | 92.92 (8) |
O2xii—K2—O3vi | 84.3 (9) | Mg2—O3—K1xvii | 116.33 (10) |
O1xi—K2—O3vi | 116.5 (8) | K2—O3—K1xvii | 102.5 (6) |
O2vi—K2—O1vii | 82.0 (9) | K2xi—O3—K1xvii | 125.4 (6) |
O3—K2—O1vii | 79.1 (8) | K1xi—O3—K1xvii | 95.28 (10) |
O3xi—K2—O1vii | 114.7 (10) | K1—O3—K1xvii | 131.13 (12) |
O2xii—K2—O1vii | 136.8 (10) | Mo—O3—K2xvi | 87.9 (6) |
O1xi—K2—O1vii | 55.3 (4) | Mg2—O3—K2xvi | 115.4 (7) |
O3vi—K2—O1vii | 70.5 (6) | K2—O3—K2xvi | 109.9 (10) |
O2vi—K2—O4xiii | 150.7 (13) | K2xi—O3—K2xvi | 132.0 (10) |
O3—K2—O4xiii | 138.3 (12) | K1xi—O3—K2xvi | 102.8 (5) |
O3xi—K2—O4xiii | 49.0 (6) | K1—O3—K2xvi | 137.1 (5) |
O2xii—K2—O4xiii | 53.5 (6) | K1xvii—O3—K2xvi | 7.5 (5) |
O1xi—K2—O4xiii | 61.8 (6) | Mo—O3—K2xvii | 76.3 (5) |
O3vi—K2—O4xiii | 92.8 (8) | Mg2—O3—K2xvii | 111.6 (6) |
O1vii—K2—O4xiii | 92.2 (6) | K2—O3—K2xvii | 127.5 (9) |
O2vi—K2—O1xiii | 116.7 (10) | K2xi—O3—K2xvii | 146.2 (10) |
O3—K2—O1xiii | 122.4 (9) | K1xi—O3—K2xvii | 120.6 (5) |
O3xi—K2—O1xiii | 86.0 (8) | K1—O3—K2xvii | 148.9 (6) |
O2xii—K2—O1xiii | 89.7 (8) | K1xvii—O3—K2xvii | 25.4 (5) |
O1xi—K2—O1xiii | 52.4 (4) | K2xvi—O3—K2xvii | 17.8 (7) |
O3vi—K2—O1xiii | 68.1 (5) | Mo—O4—Mg1 | 119.02 (7) |
O1vii—K2—O1xiii | 48.8 (3) | Mo—O4—Mg2ii | 140.92 (8) |
O4xiii—K2—O1xiii | 45.4 (4) | Mg1—O4—Mg2ii | 95.06 (6) |
O2vi—K2—O3xii | 72.3 (7) | Mo—O4—K1ii | 83.41 (6) |
O3—K2—O3xii | 110.5 (8) | Mg1—O4—K1ii | 138.16 (8) |
O3xi—K2—O3xii | 96.7 (8) | Mg2ii—O4—K1ii | 82.80 (6) |
O2xii—K2—O3xii | 46.0 (4) | Mo—O4—K2xv | 88.8 (5) |
O1xi—K2—O3xii | 155.8 (12) | Mg1—O4—K2xv | 137.7 (6) |
O3vi—K2—O3xii | 77.1 (7) | Mg2ii—O4—K2xv | 76.2 (4) |
O1vii—K2—O3xii | 146.1 (11) | K1ii—O4—K2xv | 6.6 (5) |
Symmetry codes: (i) −x, −x+y, −z+1/2; (ii) −x+y, −x, z; (iii) −y, x−y, z; (iv) x−y, −y, −z+1/2; (v) y, x, −z+1/2; (vi) y+1/3, −x+y+2/3, −z+2/3; (vii) −x+y+2/3, y+1/3, z−1/6; (viii) x−y, x, −z+1; (ix) y, −x+y, −z+1; (x) −x, −y, −z+1; (xi) −x+2/3, −x+y+1/3, −z+5/6; (xii) −y+1/3, −x+2/3, z+1/6; (xiii) y+2/3, x+1/3, −z+5/6; (xiv) −x+y+1/3, y−1/3, z+1/6; (xv) y−1/3, x−2/3, −z+5/6; (xvi) x−y+1/3, x−1/3, −z+2/3; (xvii) −y+2/3, −x+1/3, z−1/6. |