Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100006704/bs0011sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100006704/bs0011sup2.hkl |
Data collection: Nonius Software; cell refinement: Nonius Software; data reduction: Nonius Software; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: Atoms (Dowty, 1999).
K3NdO17Si7 | Dx = 3.000 Mg m−3 |
Mr = 730.17 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P3 | Cell parameters from 22 reflections |
Hall symbol: -P 3 | θ = 23.6–33.3° |
a = 16.131 (2) Å | µ = 4.60 mm−1 |
c = 7.175 (2) Å | T = 293 K |
V = 1616.9 (5) Å3 | Irregular, colorless |
Z = 4 | × × mm |
F(000) = 1404 |
Nonius 4-circle diffractometer | 2469 reflections with I ≥ σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.028 |
Graphite monochromator | θmax = 27.5°, θmin = 2.5° |
?? X–ray diffraction ?? scans | h = 0→18 |
Absorption correction: ψ scan ? | k = 0→18 |
Tmin = 0.277, Tmax = 0.323 | l = −9→9 |
2740 measured reflections | 2 standard reflections |
2474 independent reflections | intensity decay: 1.3% |
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)] = 0.026 | Calculated w = 1/[σ2(Fo2) + (0.0257P)2 + 4.4536P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.071 | (Δ/σ)max = 0.001 |
S = 1.27 | Δρmax = 0.95 e Å−3 |
2469 reflections | Δρmin = −1.72 e Å−3 |
172 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0297 (7) |
K3NdO17Si7 | Z = 4 |
Mr = 730.17 | Mo Kα radiation |
Hexagonal, P3 | µ = 4.60 mm−1 |
a = 16.131 (2) Å | T = 293 K |
c = 7.175 (2) Å | × × mm |
V = 1616.9 (5) Å3 |
Nonius 4-circle diffractometer | 2469 reflections with I ≥ σ(I) |
Absorption correction: ψ scan ? | Rint = 0.028 |
Tmin = 0.277, Tmax = 0.323 | 2 standard reflections |
2740 measured reflections | intensity decay: 1.3% |
2474 independent reflections |
R[F2 > 2σ(F2)] = 0.026 | 172 parameters |
wR(F2) = 0.071 | 0 restraints |
S = 1.27 | Δρmax = 0.95 e Å−3 |
2469 reflections | Δρmin = −1.72 e Å−3 |
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 on F2 for ALL reflections except for 5 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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 | ||
Nd1 | 0.0000 | 0.0000 | 0.0000 | 0.00926 (12) | |
Nd2 | −0.5000 | −0.5000 | 0.0000 | 0.00952 (11) | |
Si1 | 0.6667 | 0.3333 | 0.4247 (2) | 0.0096 (3) | |
Si2 | −0.71320 (6) | −0.61966 (6) | −0.69845 (12) | 0.0092 (2) | |
Si3 | −0.69315 (6) | −0.52568 (6) | −0.32686 (12) | 0.0094 (2) | |
Si4 | 0.6667 | 0.3333 | 0.8654 (2) | 0.0095 (3) | |
Si5 | −0.84320 (6) | −0.83555 (6) | 0.37820 (12) | 0.0091 (2) | |
Si6 | −0.46020 (6) | −0.25155 (6) | −0.97903 (12) | 0.0096 (2) | |
K1 | −0.53819 (6) | −0.63419 (7) | −0.46846 (11) | 0.0248 (2) | |
K2 | −0.76102 (7) | −0.75708 (7) | −1.12460 (14) | 0.0300 (2) | |
O1 | −0.7815 (2) | −0.6254 (2) | −0.8735 (3) | 0.0138 (5) | |
O2 | −0.8184 (2) | −0.8893 (2) | −0.4567 (3) | 0.0149 (5) | |
O3 | −0.7477 (2) | −0.7296 (2) | −0.6374 (3) | 0.0146 (5) | |
O4 | −0.7720 (2) | −0.3628 (2) | −0.3536 (4) | 0.0165 (5) | |
O5 | −0.7888 (2) | −0.5590 (2) | −1.2006 (3) | 0.0140 (5) | |
O6 | −0.9802 (2) | −0.8692 (2) | −1.1837 (3) | 0.0164 (5) | |
O7 | −0.6217 (2) | −0.5550 (2) | −1.2425 (3) | 0.0167 (5) | |
O8 | −0.4585 (2) | −0.3436 (2) | −0.9172 (4) | 0.0186 (5) | |
O9 | −0.7409 (2) | −0.5710 (2) | −0.5283 (3) | 0.0157 (5) | |
O10 | −0.3971 (2) | −0.4366 (2) | −1.2560 (3) | 0.0157 (5) | |
O11 | −0.5614 (2) | −0.2550 (2) | −0.9349 (4) | 0.0179 (5) | |
O12 | 0.3333 | 0.6667 | 0.3548 (6) | 0.0345 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.00967 (14) | 0.00967 (14) | 0.0085 (2) | 0.00483 (7) | 0.000 | 0.000 |
Nd2 | 0.00946 (14) | 0.00860 (14) | 0.0088 (2) | 0.00325 (9) | 0.00054 (7) | 0.00065 (7) |
Si1 | 0.0104 (4) | 0.0104 (4) | 0.0081 (6) | 0.0052 (2) | 0.000 | 0.000 |
Si2 | 0.0090 (4) | 0.0094 (4) | 0.0084 (4) | 0.0040 (3) | 0.0005 (3) | 0.0005 (3) |
Si3 | 0.0098 (4) | 0.0105 (4) | 0.0093 (4) | 0.0061 (3) | −0.0002 (3) | 0.0005 (3) |
Si4 | 0.0102 (4) | 0.0102 (4) | 0.0080 (6) | 0.0051 (2) | 0.000 | 0.000 |
Si5 | 0.0091 (4) | 0.0090 (4) | 0.0095 (4) | 0.0048 (3) | 0.0001 (3) | 0.0001 (3) |
Si6 | 0.0111 (4) | 0.0087 (4) | 0.0095 (4) | 0.0055 (3) | 0.0006 (3) | 0.0008 (3) |
K1 | 0.0309 (4) | 0.0351 (5) | 0.0203 (4) | 0.0255 (4) | 0.0047 (3) | 0.0046 (3) |
K2 | 0.0313 (5) | 0.0266 (4) | 0.0311 (5) | 0.0138 (4) | 0.0029 (4) | −0.0036 (3) |
O1 | 0.0170 (11) | 0.0112 (11) | 0.0123 (11) | 0.0063 (9) | −0.0038 (8) | −0.0010 (8) |
O2 | 0.0181 (12) | 0.0110 (11) | 0.0168 (11) | 0.0081 (9) | −0.0020 (9) | 0.0013 (9) |
O3 | 0.0116 (11) | 0.0086 (10) | 0.0221 (12) | 0.0039 (9) | −0.0003 (9) | 0.0037 (9) |
O4 | 0.0116 (11) | 0.0122 (11) | 0.0265 (13) | 0.0065 (9) | 0.0013 (9) | −0.0011 (9) |
O5 | 0.0124 (11) | 0.0189 (12) | 0.0101 (10) | 0.0073 (9) | 0.0006 (8) | 0.0001 (9) |
O6 | 0.0197 (12) | 0.0158 (11) | 0.0127 (11) | 0.0083 (10) | −0.0030 (9) | 0.0009 (9) |
O7 | 0.0173 (12) | 0.0198 (12) | 0.0184 (12) | 0.0133 (10) | −0.0040 (9) | −0.0015 (9) |
O8 | 0.0289 (14) | 0.0130 (11) | 0.0181 (12) | 0.0136 (11) | −0.0011 (10) | 0.0022 (9) |
O9 | 0.0168 (11) | 0.0230 (12) | 0.0102 (11) | 0.0122 (10) | −0.0008 (9) | −0.0032 (9) |
O10 | 0.0106 (11) | 0.0168 (11) | 0.0168 (12) | 0.0047 (9) | 0.0036 (9) | 0.0055 (9) |
O11 | 0.0105 (11) | 0.0129 (11) | 0.0278 (13) | 0.0040 (9) | 0.0037 (9) | −0.0008 (10) |
O12 | 0.048 (2) | 0.048 (2) | 0.007 (2) | 0.0242 (10) | 0.000 | 0.000 |
Nd1—O6i | 2.371 (2) | Si6—O5xvi | 1.624 (2) |
Nd1—O6ii | 2.371 (2) | Si6—O11 | 1.636 (3) |
Nd1—O6iii | 2.371 (2) | Si6—O1xvi | 1.651 (2) |
Nd1—O6iv | 2.371 (2) | Si6—K2xv | 3.5792 (14) |
Nd1—O6v | 2.371 (2) | Si6—K1i | 3.6956 (14) |
Nd1—O6vi | 2.371 (2) | Si6—K2xvi | 3.9153 (13) |
Nd1—K2iii | 3.9886 (11) | K1—O10xv | 2.738 (3) |
Nd1—K2vi | 3.9887 (11) | K1—O8i | 2.787 (3) |
Nd1—K2i | 3.9887 (11) | K1—O7vii | 2.793 (3) |
Nd1—K2ii | 3.9887 (11) | K1—O4xviii | 2.854 (3) |
Nd1—K2iv | 3.9887 (11) | K1—O9xviii | 2.932 (3) |
Nd1—K2v | 3.9887 (11) | K1—O5xxi | 3.135 (2) |
Nd2—O10i | 2.340 (2) | K1—O3 | 3.172 (2) |
Nd2—O10vii | 2.340 (2) | K1—O10vii | 3.226 (3) |
Nd2—O8i | 2.340 (2) | K1—Si3xviii | 3.6165 (13) |
Nd2—O8vii | 2.340 (2) | K1—Si3i | 3.6208 (13) |
Nd2—O7i | 2.435 (2) | K1—Si1xxii | 3.6769 (10) |
Nd2—O7vii | 2.435 (2) | K2—O1 | 2.927 (3) |
Nd2—K1 | 3.8766 (12) | K2—O6xxi | 2.958 (3) |
Nd2—K1viii | 3.8767 (12) | K2—O7 | 3.011 (3) |
Nd2—K2vii | 4.2738 (11) | K2—O2xxiii | 3.018 (3) |
Nd2—K2i | 4.2738 (11) | K2—O8xv | 3.085 (3) |
Nd2—K1vii | 4.2750 (12) | K2—O6 | 3.092 (3) |
Nd2—K1i | 4.2750 (12) | K2—O1xxi | 3.133 (3) |
Si1—O12ix | 1.583 (5) | K2—Si6xv | 3.5793 (14) |
Si1—O4x | 1.601 (2) | K2—Si3xxiii | 3.6264 (14) |
Si1—O4xi | 1.601 (2) | K2—Si5xxiv | 3.796 (2) |
Si1—O4xii | 1.602 (2) | K2—Si5xviii | 3.8205 (13) |
Si1—K1xiii | 3.6754 (10) | O1—Si6xxv | 1.650 (2) |
Si1—K1xiv | 3.6760 (10) | O1—K2xxvi | 3.133 (3) |
Si1—K1ii | 3.6769 (10) | O2—Si5xxiii | 1.632 (2) |
Si2—O10xv | 1.576 (2) | O2—Si5xxvii | 1.642 (2) |
Si2—O9 | 1.630 (2) | O2—K2vii | 3.018 (3) |
Si2—O3 | 1.631 (2) | O3—Si5xxiii | 1.635 (2) |
Si2—O1 | 1.642 (2) | O4—Si1x | 1.601 (2) |
Si2—K1 | 3.3779 (13) | O4—Si3xxv | 1.639 (3) |
Si2—K2 | 3.6260 (14) | O4—K1xvii | 2.854 (3) |
Si3—O7vii | 1.569 (2) | O5—Si6xxv | 1.624 (2) |
Si3—O9 | 1.629 (2) | O5—Si3xxiii | 1.631 (2) |
Si3—O5vii | 1.631 (2) | O5—K1xxvi | 3.135 (2) |
Si3—O4xvi | 1.639 (3) | O6—Si5xvii | 1.582 (2) |
Si3—K1xvii | 3.6166 (13) | O6—Nd1xxii | 2.371 (2) |
Si3—K1i | 3.6208 (13) | O6—K2xxvi | 2.958 (3) |
Si3—K2vii | 3.6265 (14) | O7—Si3xxiii | 1.569 (2) |
Si3—K1 | 3.8367 (12) | O7—Nd2xxiii | 2.435 (2) |
Si4—O12ix | 1.579 (5) | O7—K1xxiii | 2.793 (3) |
Si4—O11xii | 1.607 (2) | O8—Nd2xxiii | 2.340 (2) |
Si4—O11x | 1.608 (2) | O8—K1i | 2.787 (3) |
Si4—O11xi | 1.608 (2) | O8—K2xv | 3.085 (3) |
Si5—O6xviii | 1.582 (2) | O9—K1xvii | 2.932 (3) |
Si5—O2vii | 1.632 (2) | O10—Si2xv | 1.576 (2) |
Si5—O3vii | 1.635 (2) | O10—Nd2xxiii | 2.340 (2) |
Si5—O2xix | 1.642 (2) | O10—K1xv | 2.738 (3) |
Si5—K2xx | 3.796 (2) | O10—K1xxiii | 3.226 (3) |
Si5—K2xvii | 3.8205 (13) | O11—Si4x | 1.608 (2) |
Si5—K2vii | 3.833 (2) | O12—Si4ix | 1.579 (5) |
Si6—O8 | 1.563 (2) | O12—Si1ix | 1.583 (5) |
O6i—Nd1—O6ii | 180.0 | O6xviii—Si5—K2xvii | 73.43 (10) |
O6i—Nd1—O6iii | 92.08 (8) | O2vii—Si5—K2xvii | 153.95 (10) |
O6ii—Nd1—O6iii | 87.92 (8) | O3vii—Si5—K2xvii | 94.08 (9) |
O6i—Nd1—O6iv | 87.92 (8) | O2xix—Si5—K2xvii | 49.30 (9) |
O6ii—Nd1—O6iv | 92.08 (8) | K2xx—Si5—K2xvii | 121.43 (3) |
O6iii—Nd1—O6iv | 87.92 (8) | O6xviii—Si5—K2vii | 45.86 (10) |
O6i—Nd1—O6v | 87.92 (8) | O2vii—Si5—K2vii | 136.25 (10) |
O6ii—Nd1—O6v | 92.08 (8) | O3vii—Si5—K2vii | 66.48 (9) |
O6iii—Nd1—O6v | 180.0 | O2xix—Si5—K2vii | 116.67 (9) |
O6iv—Nd1—O6v | 92.08 (8) | K2xx—Si5—K2vii | 140.25 (4) |
O6i—Nd1—O6vi | 92.08 (8) | K2xvii—Si5—K2vii | 67.98 (2) |
O6ii—Nd1—O6vi | 87.92 (8) | O8—Si6—O5xvi | 113.01 (13) |
O6iii—Nd1—O6vi | 92.08 (8) | O8—Si6—O11 | 113.82 (14) |
O6iv—Nd1—O6vi | 180.0 | O5xvi—Si6—O11 | 106.04 (14) |
O6v—Nd1—O6vi | 87.92 (8) | O8—Si6—O1xvi | 110.65 (14) |
O6i—Nd1—K2iii | 132.51 (6) | O5xvi—Si6—O1xvi | 105.49 (13) |
O6ii—Nd1—K2iii | 47.49 (6) | O11—Si6—O1xvi | 107.30 (13) |
O6iii—Nd1—K2iii | 50.73 (6) | O8—Si6—K2xv | 59.17 (10) |
O6iv—Nd1—K2iii | 114.62 (6) | O5xvi—Si6—K2xv | 96.66 (9) |
O6v—Nd1—K2iii | 129.27 (6) | O11—Si6—K2xv | 156.84 (10) |
O6vi—Nd1—K2iii | 65.38 (6) | O1xvi—Si6—K2xv | 61.05 (9) |
O6i—Nd1—K2vi | 65.38 (6) | O8—Si6—K1i | 43.85 (10) |
O6ii—Nd1—K2vi | 114.62 (6) | O5xvi—Si6—K1i | 155.66 (9) |
O6iii—Nd1—K2vi | 132.51 (6) | O11—Si6—K1i | 93.26 (10) |
O6iv—Nd1—K2vi | 129.27 (6) | O1xvi—Si6—K1i | 82.00 (9) |
O6v—Nd1—K2vi | 47.49 (6) | K2xv—Si6—K1i | 66.25 (3) |
O6vi—Nd1—K2vi | 50.73 (6) | O8—Si6—K2xvi | 127.81 (11) |
K2iii—Nd1—K2vi | 115.129 (11) | O5xvi—Si6—K2xvi | 62.71 (9) |
O6i—Nd1—K2i | 50.73 (6) | O11—Si6—K2xvi | 117.07 (9) |
O6ii—Nd1—K2i | 129.27 (6) | O1xvi—Si6—K2xvi | 42.79 (9) |
O6iii—Nd1—K2i | 65.38 (6) | K2xv—Si6—K2xvi | 69.46 (3) |
O6iv—Nd1—K2i | 47.49 (6) | K1i—Si6—K2xvi | 121.33 (3) |
O6v—Nd1—K2i | 114.62 (6) | O10xv—K1—O8i | 141.62 (8) |
O6vi—Nd1—K2i | 132.51 (6) | O10xv—K1—O7vii | 81.74 (8) |
K2iii—Nd1—K2i | 115.129 (11) | O8i—K1—O7vii | 60.01 (7) |
K2vi—Nd1—K2i | 115.128 (11) | O10xv—K1—O4xviii | 96.47 (8) |
O6i—Nd1—K2ii | 129.27 (6) | O8i—K1—O4xviii | 115.36 (8) |
O6ii—Nd1—K2ii | 50.73 (6) | O7vii—K1—O4xviii | 142.51 (8) |
O6iii—Nd1—K2ii | 114.62 (6) | O10xv—K1—O9xviii | 122.90 (8) |
O6iv—Nd1—K2ii | 132.51 (6) | O8i—K1—O9xviii | 83.55 (7) |
O6v—Nd1—K2ii | 65.38 (6) | O7vii—K1—O9xviii | 129.02 (8) |
O6vi—Nd1—K2ii | 47.49 (6) | O4xviii—K1—O9xviii | 83.30 (7) |
K2iii—Nd1—K2ii | 64.871 (11) | O10xv—K1—O5xxi | 79.35 (7) |
K2vi—Nd1—K2ii | 64.872 (11) | O8i—K1—O5xxi | 132.33 (7) |
K2i—Nd1—K2ii | 180.0 | O7vii—K1—O5xxi | 148.48 (7) |
O6i—Nd1—K2iv | 114.62 (6) | O4xviii—K1—O5xxi | 65.11 (7) |
O6ii—Nd1—K2iv | 65.38 (6) | O9xviii—K1—O5xxi | 48.79 (6) |
O6iii—Nd1—K2iv | 47.49 (6) | O10xv—K1—O3 | 52.44 (7) |
O6iv—Nd1—K2iv | 50.73 (6) | O8i—K1—O3 | 111.71 (8) |
O6v—Nd1—K2iv | 132.51 (6) | O7vii—K1—O3 | 78.63 (7) |
O6vi—Nd1—K2iv | 129.27 (6) | O4xviii—K1—O3 | 129.30 (8) |
K2iii—Nd1—K2iv | 64.872 (10) | O9xviii—K1—O3 | 84.25 (7) |
K2vi—Nd1—K2iv | 180.0 | O5xxi—K1—O3 | 69.86 (6) |
K2i—Nd1—K2iv | 64.871 (10) | O10xv—K1—O10vii | 99.02 (7) |
K2ii—Nd1—K2iv | 115.130 (11) | O8i—K1—O10vii | 67.45 (7) |
O6i—Nd1—K2v | 47.49 (6) | O7vii—K1—O10vii | 62.42 (7) |
O6ii—Nd1—K2v | 132.51 (6) | O4xviii—K1—O10vii | 81.14 (7) |
O6iii—Nd1—K2v | 129.27 (6) | O9xviii—K1—O10vii | 136.60 (7) |
O6iv—Nd1—K2v | 65.38 (6) | O5xxi—K1—O10vii | 145.61 (7) |
O6v—Nd1—K2v | 50.73 (6) | O3—K1—O10vii | 135.57 (7) |
O6vi—Nd1—K2v | 114.62 (6) | O10xv—K1—Si2 | 27.38 (5) |
K2iii—Nd1—K2v | 180.0 | O8i—K1—Si2 | 122.08 (6) |
K2vi—Nd1—K2v | 64.871 (11) | O7vii—K1—Si2 | 68.93 (6) |
K2i—Nd1—K2v | 64.871 (11) | O4xviii—K1—Si2 | 121.67 (6) |
K2ii—Nd1—K2v | 115.129 (11) | O9xviii—K1—Si2 | 111.37 (6) |
K2iv—Nd1—K2v | 115.128 (11) | O5xxi—K1—Si2 | 82.98 (5) |
O10i—Nd2—O10vii | 180.0 | O3—K1—Si2 | 28.61 (4) |
O10i—Nd2—O8i | 88.29 (9) | O10vii—K1—Si2 | 111.31 (5) |
O10vii—Nd2—O8i | 91.71 (9) | O10xv—K1—Si3xviii | 106.11 (6) |
O10i—Nd2—O8vii | 91.71 (9) | O8i—K1—Si3xviii | 107.17 (6) |
O10vii—Nd2—O8vii | 88.29 (9) | O7vii—K1—Si3xviii | 153.34 (6) |
O8i—Nd2—O8vii | 180.0 | O4xviii—K1—Si3xviii | 63.15 (5) |
O10i—Nd2—O7i | 82.23 (9) | O9xviii—K1—Si3xviii | 26.24 (5) |
O10vii—Nd2—O7i | 97.77 (9) | O5xxi—K1—Si3xviii | 26.76 (4) |
O8i—Nd2—O7i | 108.52 (8) | O3—K1—Si3xviii | 86.15 (5) |
O8vii—Nd2—O7i | 71.48 (8) | O10vii—K1—Si3xviii | 137.91 (5) |
O10i—Nd2—O7vii | 97.77 (9) | Si2—K1—Si3xviii | 106.34 (3) |
O10vii—Nd2—O7vii | 82.23 (9) | O10xv—K1—Si3i | 83.23 (5) |
O8i—Nd2—O7vii | 71.48 (8) | O8i—K1—Si3i | 116.15 (6) |
O8vii—Nd2—O7vii | 108.52 (8) | O7vii—K1—Si3i | 118.09 (6) |
O7i—Nd2—O7vii | 180.0 | O4xviii—K1—Si3i | 26.04 (5) |
O10i—Nd2—K1 | 123.82 (6) | O9xviii—K1—Si3i | 109.32 (6) |
O10vii—Nd2—K1 | 56.18 (6) | O5xxi—K1—Si3i | 84.43 (5) |
O8i—Nd2—K1 | 45.42 (6) | O3—K1—Si3i | 131.25 (5) |
O8vii—Nd2—K1 | 134.58 (6) | O10vii—K1—Si3i | 61.40 (5) |
O7i—Nd2—K1 | 134.19 (6) | Si2—K1—Si3i | 110.61 (3) |
O7vii—Nd2—K1 | 45.81 (6) | Si3xviii—K1—Si3i | 88.39 (3) |
O10i—Nd2—K1viii | 56.18 (6) | O10xv—K1—Si1xxii | 117.79 (6) |
O10vii—Nd2—K1viii | 123.81 (6) | O8i—K1—Si1xxii | 98.59 (6) |
O8i—Nd2—K1viii | 134.58 (6) | O7vii—K1—Si1xxii | 149.33 (6) |
O8vii—Nd2—K1viii | 45.42 (6) | O4xviii—K1—Si1xxii | 24.50 (5) |
O7i—Nd2—K1viii | 45.81 (6) | O9xviii—K1—Si1xxii | 62.31 (5) |
O7vii—Nd2—K1viii | 134.19 (6) | O5xxi—K1—Si1xxii | 62.08 (5) |
K1—Nd2—K1viii | 180.0 | O3—K1—Si1xxii | 131.83 (6) |
O10i—Nd2—K2vii | 66.47 (6) | O10vii—K1—Si1xxii | 89.95 (5) |
O10vii—Nd2—K2vii | 113.53 (6) | Si2—K1—Si1xxii | 138.60 (4) |
O8i—Nd2—K2vii | 44.69 (7) | Si3xviii—K1—Si1xxii | 48.50 (2) |
O8vii—Nd2—K2vii | 135.31 (7) | Si3i—K1—Si1xxii | 48.49 (2) |
O7i—Nd2—K2vii | 136.61 (6) | O1—K2—O6xxi | 79.73 (7) |
O7vii—Nd2—K2vii | 43.39 (6) | O1—K2—O7 | 71.40 (7) |
K1—Nd2—K2vii | 58.16 (2) | O6xxi—K2—O7 | 147.26 (7) |
K1viii—Nd2—K2vii | 121.84 (2) | O1—K2—O2xxiii | 153.23 (7) |
O10i—Nd2—K2i | 113.53 (6) | O6xxi—K2—O2xxiii | 102.71 (7) |
O10vii—Nd2—K2i | 66.47 (6) | O7—K2—O2xxiii | 110.03 (7) |
O8i—Nd2—K2i | 135.31 (7) | O1—K2—O8xv | 94.26 (7) |
O8vii—Nd2—K2i | 44.69 (7) | O6xxi—K2—O8xv | 114.50 (7) |
O7i—Nd2—K2i | 43.39 (6) | O7—K2—O8xv | 54.45 (6) |
O7vii—Nd2—K2i | 136.61 (6) | O2xxiii—K2—O8xv | 108.33 (7) |
K1—Nd2—K2i | 121.84 (2) | O1—K2—O6 | 89.88 (7) |
K1viii—Nd2—K2i | 58.16 (2) | O6xxi—K2—O6 | 65.88 (9) |
K2vii—Nd2—K2i | 180.0 | O7—K2—O6 | 127.64 (7) |
O10i—Nd2—K1vii | 35.66 (6) | O2xxiii—K2—O6 | 67.76 (7) |
O10vii—Nd2—K1vii | 144.34 (6) | O8xv—K2—O6 | 175.84 (7) |
O8i—Nd2—K1vii | 77.83 (6) | O1—K2—O1xxi | 133.20 (5) |
O8vii—Nd2—K1vii | 102.16 (6) | O6xxi—K2—O1xxi | 88.53 (7) |
O7i—Nd2—K1vii | 55.44 (6) | O7—K2—O1xxi | 99.95 (7) |
O7vii—Nd2—K1vii | 124.56 (6) | O2xxiii—K2—O1xxi | 73.53 (6) |
K1—Nd2—K1vii | 123.24 (3) | O8xv—K2—O1xxi | 50.30 (6) |
K1viii—Nd2—K1vii | 56.76 (3) | O6—K2—O1xxi | 126.03 (7) |
K2vii—Nd2—K1vii | 82.68 (2) | O1—K2—Si6xv | 108.41 (6) |
K2i—Nd2—K1vii | 97.32 (2) | O6xxi—K2—Si6xv | 95.20 (6) |
O10i—Nd2—K1i | 144.34 (6) | O7—K2—Si6xv | 80.01 (5) |
O10vii—Nd2—K1i | 35.66 (6) | O2xxiii—K2—Si6xv | 97.98 (5) |
O8i—Nd2—K1i | 102.17 (6) | O8xv—K2—Si6xv | 25.78 (5) |
O8vii—Nd2—K1i | 77.84 (6) | O6—K2—Si6xv | 151.38 (6) |
O7i—Nd2—K1i | 124.56 (6) | O1xxi—K2—Si6xv | 27.45 (4) |
O7vii—Nd2—K1i | 55.44 (6) | O1—K2—Si2 | 26.37 (5) |
K1—Nd2—K1i | 56.76 (3) | O6xxi—K2—Si2 | 71.20 (5) |
K1viii—Nd2—K1i | 123.24 (3) | O7—K2—Si2 | 76.09 (5) |
K2vii—Nd2—K1i | 97.32 (2) | O2xxiii—K2—Si2 | 173.76 (6) |
K2i—Nd2—K1i | 82.68 (2) | O8xv—K2—Si2 | 76.04 (5) |
K1vii—Nd2—K1i | 180.0 | O6—K2—Si2 | 107.74 (5) |
O12ix—Si1—O4x | 108.57 (11) | O1xxi—K2—Si2 | 107.12 (5) |
O12ix—Si1—O4xi | 108.56 (11) | Si6xv—K2—Si2 | 84.14 (3) |
O4x—Si1—O4xi | 110.41 (10) | O1—K2—Si3xxiii | 65.47 (5) |
O12ix—Si1—O4xii | 108.55 (11) | O6xxi—K2—Si3xxiii | 143.65 (6) |
O4x—Si1—O4xii | 110.35 (10) | O7—K2—Si3xxiii | 25.23 (5) |
O4xi—Si1—O4xii | 110.33 (10) | O2xxiii—K2—Si3xxiii | 103.87 (5) |
O12ix—Si1—K1xiii | 77.96 (3) | O8xv—K2—Si3xxiii | 79.68 (5) |
O4x—Si1—K1xiii | 87.34 (9) | O6—K2—Si3xxiii | 102.44 (5) |
O4xi—Si1—K1xiii | 47.66 (9) | O1xxi—K2—Si3xxiii | 122.65 (5) |
O4xii—Si1—K1xiii | 156.91 (9) | Si6xv—K2—Si3xxiii | 105.13 (3) |
O12ix—Si1—K1xiv | 77.96 (3) | Si2—K2—Si3xxiii | 81.12 (3) |
O4x—Si1—K1xiv | 47.63 (9) | O1—K2—Si5xxiv | 132.31 (6) |
O4xi—Si1—K1xiv | 156.97 (9) | O6xxi—K2—Si5xxiv | 118.75 (6) |
O4xii—Si1—K1xiv | 87.30 (9) | O7—K2—Si5xxiv | 92.53 (5) |
K1xiii—Si1—K1xiv | 115.79 (2) | O2xxiii—K2—Si5xxiv | 24.47 (5) |
O12ix—Si1—K1ii | 77.96 (3) | O8xv—K2—Si5xxiv | 112.62 (6) |
O4x—Si1—K1ii | 156.89 (9) | O6—K2—Si5xxiv | 64.49 (5) |
O4xi—Si1—K1ii | 87.28 (9) | O1xxi—K2—Si5xxiv | 93.00 (5) |
O4xii—Si1—K1ii | 47.62 (9) | Si6xv—K2—Si5xxiv | 112.54 (3) |
K1xiii—Si1—K1ii | 115.77 (2) | Si2—K2—Si5xxiv | 158.19 (4) |
K1xiv—Si1—K1ii | 115.75 (2) | Si3xxiii—K2—Si5xxiv | 80.94 (3) |
O10xv—Si2—O9 | 112.36 (13) | O1—K2—Si5xviii | 156.98 (6) |
O10xv—Si2—O3 | 110.83 (13) | O6xxi—K2—Si5xviii | 82.09 (5) |
O9—Si2—O3 | 107.21 (13) | O7—K2—Si5xviii | 129.46 (6) |
O10xv—Si2—O1 | 113.97 (13) | O2xxiii—K2—Si5xviii | 24.36 (5) |
O9—Si2—O1 | 105.20 (13) | O8xv—K2—Si5xviii | 106.11 (5) |
O3—Si2—O1 | 106.83 (12) | O6—K2—Si5xviii | 69.75 (5) |
O10xv—Si2—K1 | 53.05 (9) | O1xxi—K2—Si5xviii | 59.80 (5) |
O9—Si2—K1 | 96.17 (9) | Si6xv—K2—Si5xviii | 87.13 (3) |
O3—Si2—K1 | 68.67 (9) | Si2—K2—Si5xviii | 150.92 (3) |
O1—Si2—K1 | 158.42 (9) | Si3xxiii—K2—Si5xviii | 127.95 (4) |
O10xv—Si2—K2 | 90.63 (10) | Si5xxiv—K2—Si5xviii | 48.49 (2) |
O9—Si2—K2 | 154.18 (9) | Si2—O1—Si6xxv | 130.26 (15) |
O3—Si2—K2 | 73.08 (9) | Si2—O1—K2 | 101.28 (11) |
O1—Si2—K2 | 52.35 (9) | Si6xxv—O1—K2 | 114.69 (11) |
K1—Si2—K2 | 107.41 (3) | Si2—O1—K2xxvi | 122.98 (12) |
O7vii—Si3—O9 | 117.44 (13) | Si6xxv—O1—K2xxvi | 91.51 (10) |
O7vii—Si3—O5vii | 113.75 (13) | K2—O1—K2xxvi | 89.76 (7) |
O9—Si3—O5vii | 100.82 (12) | Si5xxiii—O2—Si5xxvii | 145.6 (2) |
O7vii—Si3—O4xvi | 108.92 (14) | Si5xxiii—O2—K2vii | 105.50 (11) |
O9—Si3—O4xvi | 106.03 (14) | Si5xxvii—O2—K2vii | 106.34 (11) |
O5vii—Si3—O4xvi | 109.32 (13) | Si2—O3—Si5xxiii | 141.8 (2) |
O7vii—Si3—K1xvii | 162.11 (10) | Si2—O3—K1 | 82.72 (9) |
O9—Si3—K1xvii | 52.71 (9) | Si5xxiii—O3—K1 | 134.37 (12) |
O5vii—Si3—K1xvii | 59.93 (9) | Si1x—O4—Si3xxv | 135.2 (2) |
O4xvi—Si3—K1xvii | 88.84 (9) | Si1x—O4—K1xvii | 107.89 (12) |
O7vii—Si3—K1i | 73.76 (10) | Si3xxv—O4—K1xvii | 104.10 (11) |
O9—Si3—K1i | 92.72 (9) | Si6xxv—O5—Si3xxiii | 126.19 (15) |
O5vii—Si3—K1i | 158.16 (9) | Si6xxv—O5—K1xxvi | 130.39 (12) |
O4xvi—Si3—K1i | 49.86 (9) | Si3xxiii—O5—K1xxvi | 93.31 (10) |
K1xvii—Si3—K1i | 118.73 (4) | Si5xvii—O6—Nd1xxii | 142.65 (14) |
O7vii—Si3—K2vii | 54.89 (10) | Si5xvii—O6—K2xxvi | 111.57 (12) |
O9—Si3—K2vii | 93.53 (10) | Nd1xxii—O6—K2xxvi | 96.30 (8) |
O5vii—Si3—K2vii | 71.90 (9) | Si5xvii—O6—K2 | 110.84 (12) |
O4xvi—Si3—K2vii | 159.51 (10) | Nd1xxii—O6—K2 | 92.86 (8) |
K1xvii—Si3—K2vii | 108.27 (3) | K2xxvi—O6—K2 | 89.99 (7) |
K1i—Si3—K2vii | 124.66 (3) | Si3xxiii—O7—Nd2xxiii | 138.23 (14) |
O7vii—Si3—K1 | 38.79 (9) | Si3xxiii—O7—K1xxiii | 120.60 (13) |
O9—Si3—K1 | 80.22 (9) | Nd2xxiii—O7—K1xxiii | 95.49 (8) |
O5vii—Si3—K1 | 136.16 (9) | Si3xxiii—O7—K2 | 99.88 (12) |
O4xvi—Si3—K1 | 112.41 (9) | Nd2xxiii—O7—K2 | 102.88 (8) |
K1xvii—Si3—K1 | 132.54 (3) | K1xxiii—O7—K2 | 86.40 (7) |
K1i—Si3—K1 | 62.81 (3) | Si6—O8—Nd2xxiii | 145.2 (2) |
K2vii—Si3—K1 | 64.32 (3) | Si6—O8—K1i | 113.30 (13) |
O12ix—Si4—O11xii | 108.08 (11) | Nd2xxiii—O8—K1i | 97.85 (8) |
O12ix—Si4—O11x | 108.06 (11) | Si6—O8—K2xv | 95.05 (12) |
O11xii—Si4—O11x | 110.87 (10) | Nd2xxiii—O8—K2xv | 103.08 (9) |
O12ix—Si4—O11xi | 108.06 (11) | K1i—O8—K2xv | 85.07 (7) |
O11xii—Si4—O11xi | 110.85 (10) | Si3—O9—Si2 | 134.3 (2) |
O11x—Si4—O11xi | 110.79 (10) | Si3—O9—K1xvii | 101.05 (11) |
O6xviii—Si5—O2vii | 114.78 (13) | Si2—O9—K1xvii | 124.60 (12) |
O6xviii—Si5—O3vii | 111.30 (13) | Si2xv—O10—Nd2xxiii | 139.87 (14) |
O2vii—Si5—O3vii | 104.61 (13) | Si2xv—O10—K1xv | 99.57 (11) |
O6xviii—Si5—O2xix | 112.23 (13) | Nd2xxiii—O10—K1xv | 114.46 (9) |
O2vii—Si5—O2xix | 107.00 (11) | Si2xv—O10—K1xxiii | 120.45 (12) |
O3vii—Si5—O2xix | 106.28 (13) | Nd2xxiii—O10—K1xxiii | 86.75 (7) |
O6xviii—Si5—K2xx | 164.49 (10) | K1xv—O10—K1xxiii | 80.98 (7) |
O2vii—Si5—K2xx | 50.02 (9) | Si4x—O11—Si6 | 136.9 (2) |
O3vii—Si5—K2xx | 74.12 (9) | Si4ix—O12—Si1ix | 179.997 (1) |
O2xix—Si5—K2xx | 78.74 (9) |
Symmetry codes: (i) −x−1, −y−1, −z−1; (ii) x+1, y+1, z+1; (iii) x−y, x+1, −z−1; (iv) −y−1, x−y, z+1; (v) −x+y, −x−1, z+1; (vi) y+1, −x+y, −z−1; (vii) x, y, z+1; (viii) −x−1, −y−1, −z; (ix) −x+1, −y+1, −z+1; (x) −x, −y, −z; (xi) x−y+1, x+1, −z; (xii) y+1, −x+y, −z; (xiii) −y, x−y, z+1; (xiv) −x+y+1, −x, z+1; (xv) −x−1, −y−1, −z−2; (xvi) −y−1, x−y, z; (xvii) x−y−1, x, −z−1; (xviii) y, −x+y−1, −z−1; (xix) x−y−1, x, −z; (xx) x, y, z+2; (xxi) y, −x+y−1, −z−2; (xxii) x−1, y−1, z−1; (xxiii) x, y, z−1; (xxiv) x, y, z−2; (xxv) −x+y−1, −x−1, z; (xxvi) x−y−1, x, −z−2; (xxvii) y, −x+y−1, −z. |
Experimental details
Crystal data | |
Chemical formula | K3NdO17Si7 |
Mr | 730.17 |
Crystal system, space group | Hexagonal, P3 |
Temperature (K) | 293 |
a, c (Å) | 16.131 (2), 7.175 (2) |
V (Å3) | 1616.9 (5) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 4.60 |
Crystal size (mm) | × × |
Data collection | |
Diffractometer | Nonius 4-circle diffractometer |
Absorption correction | ψ scan |
Tmin, Tmax | 0.277, 0.323 |
No. of measured, independent and observed [I ≥ σ(I)] reflections | 2740, 2474, 2469 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.071, 1.27 |
No. of reflections | 2469 |
No. of parameters | 172 |
Δρmax, Δρmin (e Å−3) | 0.95, −1.72 |
Computer programs: Nonius Software, SHELXS86 (Sheldrick, 1985), SHELXL93 (Sheldrick, 1993), Atoms (Dowty, 1999).