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Hydrothermal investigations in the high-silica region of the K2O-Nd2O3-SiO2 system, carried out in a search for novel fast-ion conductors (FICs), yielded the new compound tripotassium neodymium heptasilicate, K3NdSi7O17. Single-crystal X-ray methods revealed that K3NdSi7O17 crystallizes in space group P\bar 3, has lattice constants a = 16.131 (2) and c = 7.7146 (19) Å, Z = 4, and 22 atoms in the asymmetric unit. Refinement was carried out to a residual, R(F), of 0.0253 and a weighted residual, wR(F2), of 0.0702 using anisotropic displacement parameters for all atoms. The silicate anion forms an interrupted framework, within which both Nd octahedra and K polyhedra are situated. The structure is unusual in that it contains a symmetry-constrained Si-O-Si bond angle of 180°. No isomorphs to K3NdSi7O17 are known.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100006704/bs0011sup1.cif
Contains datablocks hai3, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100006704/bs0011sup2.hkl
Contains datablock hai3

Computing details top

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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
(hai3) top
Crystal data top
K3NdO17Si7Dx = 3.000 Mg m3
Mr = 730.17Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P3Cell parameters from 22 reflections
Hall symbol: -P 3θ = 23.6–33.3°
a = 16.131 (2) ŵ = 4.60 mm1
c = 7.175 (2) ÅT = 293 K
V = 1616.9 (5) Å3Irregular, colorless
Z = 4 × × mm
F(000) = 1404
Data collection top
Nonius 4-circle
diffractometer
2469 reflections with I σ(I)
Radiation source: fine-focus sealed tubeRint = 0.028
Graphite monochromatorθmax = 27.5°, θmin = 2.5°
?? X–ray diffraction ?? scansh = 018
Absorption correction: ψ scan
?
k = 018
Tmin = 0.277, Tmax = 0.323l = 99
2740 measured reflections2 standard reflections
2474 independent reflections intensity decay: 1.3%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026Calculated w = 1/[σ2(Fo2) + (0.0257P)2 + 4.4536P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.071(Δ/σ)max = 0.001
S = 1.27Δρmax = 0.95 e Å3
2469 reflectionsΔρmin = 1.72 e Å3
172 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0297 (7)
Crystal data top
K3NdO17Si7Z = 4
Mr = 730.17Mo Kα radiation
Hexagonal, P3µ = 4.60 mm1
a = 16.131 (2) ÅT = 293 K
c = 7.175 (2) Å × × mm
V = 1616.9 (5) Å3
Data collection top
Nonius 4-circle
diffractometer
2469 reflections with I σ(I)
Absorption correction: ψ scan
?
Rint = 0.028
Tmin = 0.277, Tmax = 0.3232 standard reflections
2740 measured reflections intensity decay: 1.3%
2474 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.026172 parameters
wR(F2) = 0.0710 restraints
S = 1.27Δρmax = 0.95 e Å3
2469 reflectionsΔρmin = 1.72 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nd10.00000.00000.00000.00926 (12)
Nd20.50000.50000.00000.00952 (11)
Si10.66670.33330.4247 (2)0.0096 (3)
Si20.71320 (6)0.61966 (6)0.69845 (12)0.0092 (2)
Si30.69315 (6)0.52568 (6)0.32686 (12)0.0094 (2)
Si40.66670.33330.8654 (2)0.0095 (3)
Si50.84320 (6)0.83555 (6)0.37820 (12)0.0091 (2)
Si60.46020 (6)0.25155 (6)0.97903 (12)0.0096 (2)
K10.53819 (6)0.63419 (7)0.46846 (11)0.0248 (2)
K20.76102 (7)0.75708 (7)1.12460 (14)0.0300 (2)
O10.7815 (2)0.6254 (2)0.8735 (3)0.0138 (5)
O20.8184 (2)0.8893 (2)0.4567 (3)0.0149 (5)
O30.7477 (2)0.7296 (2)0.6374 (3)0.0146 (5)
O40.7720 (2)0.3628 (2)0.3536 (4)0.0165 (5)
O50.7888 (2)0.5590 (2)1.2006 (3)0.0140 (5)
O60.9802 (2)0.8692 (2)1.1837 (3)0.0164 (5)
O70.6217 (2)0.5550 (2)1.2425 (3)0.0167 (5)
O80.4585 (2)0.3436 (2)0.9172 (4)0.0186 (5)
O90.7409 (2)0.5710 (2)0.5283 (3)0.0157 (5)
O100.3971 (2)0.4366 (2)1.2560 (3)0.0157 (5)
O110.5614 (2)0.2550 (2)0.9349 (4)0.0179 (5)
O120.33330.66670.3548 (6)0.0345 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.00967 (14)0.00967 (14)0.0085 (2)0.00483 (7)0.0000.000
Nd20.00946 (14)0.00860 (14)0.0088 (2)0.00325 (9)0.00054 (7)0.00065 (7)
Si10.0104 (4)0.0104 (4)0.0081 (6)0.0052 (2)0.0000.000
Si20.0090 (4)0.0094 (4)0.0084 (4)0.0040 (3)0.0005 (3)0.0005 (3)
Si30.0098 (4)0.0105 (4)0.0093 (4)0.0061 (3)0.0002 (3)0.0005 (3)
Si40.0102 (4)0.0102 (4)0.0080 (6)0.0051 (2)0.0000.000
Si50.0091 (4)0.0090 (4)0.0095 (4)0.0048 (3)0.0001 (3)0.0001 (3)
Si60.0111 (4)0.0087 (4)0.0095 (4)0.0055 (3)0.0006 (3)0.0008 (3)
K10.0309 (4)0.0351 (5)0.0203 (4)0.0255 (4)0.0047 (3)0.0046 (3)
K20.0313 (5)0.0266 (4)0.0311 (5)0.0138 (4)0.0029 (4)0.0036 (3)
O10.0170 (11)0.0112 (11)0.0123 (11)0.0063 (9)0.0038 (8)0.0010 (8)
O20.0181 (12)0.0110 (11)0.0168 (11)0.0081 (9)0.0020 (9)0.0013 (9)
O30.0116 (11)0.0086 (10)0.0221 (12)0.0039 (9)0.0003 (9)0.0037 (9)
O40.0116 (11)0.0122 (11)0.0265 (13)0.0065 (9)0.0013 (9)0.0011 (9)
O50.0124 (11)0.0189 (12)0.0101 (10)0.0073 (9)0.0006 (8)0.0001 (9)
O60.0197 (12)0.0158 (11)0.0127 (11)0.0083 (10)0.0030 (9)0.0009 (9)
O70.0173 (12)0.0198 (12)0.0184 (12)0.0133 (10)0.0040 (9)0.0015 (9)
O80.0289 (14)0.0130 (11)0.0181 (12)0.0136 (11)0.0011 (10)0.0022 (9)
O90.0168 (11)0.0230 (12)0.0102 (11)0.0122 (10)0.0008 (9)0.0032 (9)
O100.0106 (11)0.0168 (11)0.0168 (12)0.0047 (9)0.0036 (9)0.0055 (9)
O110.0105 (11)0.0129 (11)0.0278 (13)0.0040 (9)0.0037 (9)0.0008 (10)
O120.048 (2)0.048 (2)0.007 (2)0.0242 (10)0.0000.000
Geometric parameters (Å, º) top
Nd1—O6i2.371 (2)Si6—O5xvi1.624 (2)
Nd1—O6ii2.371 (2)Si6—O111.636 (3)
Nd1—O6iii2.371 (2)Si6—O1xvi1.651 (2)
Nd1—O6iv2.371 (2)Si6—K2xv3.5792 (14)
Nd1—O6v2.371 (2)Si6—K1i3.6956 (14)
Nd1—O6vi2.371 (2)Si6—K2xvi3.9153 (13)
Nd1—K2iii3.9886 (11)K1—O10xv2.738 (3)
Nd1—K2vi3.9887 (11)K1—O8i2.787 (3)
Nd1—K2i3.9887 (11)K1—O7vii2.793 (3)
Nd1—K2ii3.9887 (11)K1—O4xviii2.854 (3)
Nd1—K2iv3.9887 (11)K1—O9xviii2.932 (3)
Nd1—K2v3.9887 (11)K1—O5xxi3.135 (2)
Nd2—O10i2.340 (2)K1—O33.172 (2)
Nd2—O10vii2.340 (2)K1—O10vii3.226 (3)
Nd2—O8i2.340 (2)K1—Si3xviii3.6165 (13)
Nd2—O8vii2.340 (2)K1—Si3i3.6208 (13)
Nd2—O7i2.435 (2)K1—Si1xxii3.6769 (10)
Nd2—O7vii2.435 (2)K2—O12.927 (3)
Nd2—K13.8766 (12)K2—O6xxi2.958 (3)
Nd2—K1viii3.8767 (12)K2—O73.011 (3)
Nd2—K2vii4.2738 (11)K2—O2xxiii3.018 (3)
Nd2—K2i4.2738 (11)K2—O8xv3.085 (3)
Nd2—K1vii4.2750 (12)K2—O63.092 (3)
Nd2—K1i4.2750 (12)K2—O1xxi3.133 (3)
Si1—O12ix1.583 (5)K2—Si6xv3.5793 (14)
Si1—O4x1.601 (2)K2—Si3xxiii3.6264 (14)
Si1—O4xi1.601 (2)K2—Si5xxiv3.796 (2)
Si1—O4xii1.602 (2)K2—Si5xviii3.8205 (13)
Si1—K1xiii3.6754 (10)O1—Si6xxv1.650 (2)
Si1—K1xiv3.6760 (10)O1—K2xxvi3.133 (3)
Si1—K1ii3.6769 (10)O2—Si5xxiii1.632 (2)
Si2—O10xv1.576 (2)O2—Si5xxvii1.642 (2)
Si2—O91.630 (2)O2—K2vii3.018 (3)
Si2—O31.631 (2)O3—Si5xxiii1.635 (2)
Si2—O11.642 (2)O4—Si1x1.601 (2)
Si2—K13.3779 (13)O4—Si3xxv1.639 (3)
Si2—K23.6260 (14)O4—K1xvii2.854 (3)
Si3—O7vii1.569 (2)O5—Si6xxv1.624 (2)
Si3—O91.629 (2)O5—Si3xxiii1.631 (2)
Si3—O5vii1.631 (2)O5—K1xxvi3.135 (2)
Si3—O4xvi1.639 (3)O6—Si5xvii1.582 (2)
Si3—K1xvii3.6166 (13)O6—Nd1xxii2.371 (2)
Si3—K1i3.6208 (13)O6—K2xxvi2.958 (3)
Si3—K2vii3.6265 (14)O7—Si3xxiii1.569 (2)
Si3—K13.8367 (12)O7—Nd2xxiii2.435 (2)
Si4—O12ix1.579 (5)O7—K1xxiii2.793 (3)
Si4—O11xii1.607 (2)O8—Nd2xxiii2.340 (2)
Si4—O11x1.608 (2)O8—K1i2.787 (3)
Si4—O11xi1.608 (2)O8—K2xv3.085 (3)
Si5—O6xviii1.582 (2)O9—K1xvii2.932 (3)
Si5—O2vii1.632 (2)O10—Si2xv1.576 (2)
Si5—O3vii1.635 (2)O10—Nd2xxiii2.340 (2)
Si5—O2xix1.642 (2)O10—K1xv2.738 (3)
Si5—K2xx3.796 (2)O10—K1xxiii3.226 (3)
Si5—K2xvii3.8205 (13)O11—Si4x1.608 (2)
Si5—K2vii3.833 (2)O12—Si4ix1.579 (5)
Si6—O81.563 (2)O12—Si1ix1.583 (5)
O6i—Nd1—O6ii180.0O6xviii—Si5—K2xvii73.43 (10)
O6i—Nd1—O6iii92.08 (8)O2vii—Si5—K2xvii153.95 (10)
O6ii—Nd1—O6iii87.92 (8)O3vii—Si5—K2xvii94.08 (9)
O6i—Nd1—O6iv87.92 (8)O2xix—Si5—K2xvii49.30 (9)
O6ii—Nd1—O6iv92.08 (8)K2xx—Si5—K2xvii121.43 (3)
O6iii—Nd1—O6iv87.92 (8)O6xviii—Si5—K2vii45.86 (10)
O6i—Nd1—O6v87.92 (8)O2vii—Si5—K2vii136.25 (10)
O6ii—Nd1—O6v92.08 (8)O3vii—Si5—K2vii66.48 (9)
O6iii—Nd1—O6v180.0O2xix—Si5—K2vii116.67 (9)
O6iv—Nd1—O6v92.08 (8)K2xx—Si5—K2vii140.25 (4)
O6i—Nd1—O6vi92.08 (8)K2xvii—Si5—K2vii67.98 (2)
O6ii—Nd1—O6vi87.92 (8)O8—Si6—O5xvi113.01 (13)
O6iii—Nd1—O6vi92.08 (8)O8—Si6—O11113.82 (14)
O6iv—Nd1—O6vi180.0O5xvi—Si6—O11106.04 (14)
O6v—Nd1—O6vi87.92 (8)O8—Si6—O1xvi110.65 (14)
O6i—Nd1—K2iii132.51 (6)O5xvi—Si6—O1xvi105.49 (13)
O6ii—Nd1—K2iii47.49 (6)O11—Si6—O1xvi107.30 (13)
O6iii—Nd1—K2iii50.73 (6)O8—Si6—K2xv59.17 (10)
O6iv—Nd1—K2iii114.62 (6)O5xvi—Si6—K2xv96.66 (9)
O6v—Nd1—K2iii129.27 (6)O11—Si6—K2xv156.84 (10)
O6vi—Nd1—K2iii65.38 (6)O1xvi—Si6—K2xv61.05 (9)
O6i—Nd1—K2vi65.38 (6)O8—Si6—K1i43.85 (10)
O6ii—Nd1—K2vi114.62 (6)O5xvi—Si6—K1i155.66 (9)
O6iii—Nd1—K2vi132.51 (6)O11—Si6—K1i93.26 (10)
O6iv—Nd1—K2vi129.27 (6)O1xvi—Si6—K1i82.00 (9)
O6v—Nd1—K2vi47.49 (6)K2xv—Si6—K1i66.25 (3)
O6vi—Nd1—K2vi50.73 (6)O8—Si6—K2xvi127.81 (11)
K2iii—Nd1—K2vi115.129 (11)O5xvi—Si6—K2xvi62.71 (9)
O6i—Nd1—K2i50.73 (6)O11—Si6—K2xvi117.07 (9)
O6ii—Nd1—K2i129.27 (6)O1xvi—Si6—K2xvi42.79 (9)
O6iii—Nd1—K2i65.38 (6)K2xv—Si6—K2xvi69.46 (3)
O6iv—Nd1—K2i47.49 (6)K1i—Si6—K2xvi121.33 (3)
O6v—Nd1—K2i114.62 (6)O10xv—K1—O8i141.62 (8)
O6vi—Nd1—K2i132.51 (6)O10xv—K1—O7vii81.74 (8)
K2iii—Nd1—K2i115.129 (11)O8i—K1—O7vii60.01 (7)
K2vi—Nd1—K2i115.128 (11)O10xv—K1—O4xviii96.47 (8)
O6i—Nd1—K2ii129.27 (6)O8i—K1—O4xviii115.36 (8)
O6ii—Nd1—K2ii50.73 (6)O7vii—K1—O4xviii142.51 (8)
O6iii—Nd1—K2ii114.62 (6)O10xv—K1—O9xviii122.90 (8)
O6iv—Nd1—K2ii132.51 (6)O8i—K1—O9xviii83.55 (7)
O6v—Nd1—K2ii65.38 (6)O7vii—K1—O9xviii129.02 (8)
O6vi—Nd1—K2ii47.49 (6)O4xviii—K1—O9xviii83.30 (7)
K2iii—Nd1—K2ii64.871 (11)O10xv—K1—O5xxi79.35 (7)
K2vi—Nd1—K2ii64.872 (11)O8i—K1—O5xxi132.33 (7)
K2i—Nd1—K2ii180.0O7vii—K1—O5xxi148.48 (7)
O6i—Nd1—K2iv114.62 (6)O4xviii—K1—O5xxi65.11 (7)
O6ii—Nd1—K2iv65.38 (6)O9xviii—K1—O5xxi48.79 (6)
O6iii—Nd1—K2iv47.49 (6)O10xv—K1—O352.44 (7)
O6iv—Nd1—K2iv50.73 (6)O8i—K1—O3111.71 (8)
O6v—Nd1—K2iv132.51 (6)O7vii—K1—O378.63 (7)
O6vi—Nd1—K2iv129.27 (6)O4xviii—K1—O3129.30 (8)
K2iii—Nd1—K2iv64.872 (10)O9xviii—K1—O384.25 (7)
K2vi—Nd1—K2iv180.0O5xxi—K1—O369.86 (6)
K2i—Nd1—K2iv64.871 (10)O10xv—K1—O10vii99.02 (7)
K2ii—Nd1—K2iv115.130 (11)O8i—K1—O10vii67.45 (7)
O6i—Nd1—K2v47.49 (6)O7vii—K1—O10vii62.42 (7)
O6ii—Nd1—K2v132.51 (6)O4xviii—K1—O10vii81.14 (7)
O6iii—Nd1—K2v129.27 (6)O9xviii—K1—O10vii136.60 (7)
O6iv—Nd1—K2v65.38 (6)O5xxi—K1—O10vii145.61 (7)
O6v—Nd1—K2v50.73 (6)O3—K1—O10vii135.57 (7)
O6vi—Nd1—K2v114.62 (6)O10xv—K1—Si227.38 (5)
K2iii—Nd1—K2v180.0O8i—K1—Si2122.08 (6)
K2vi—Nd1—K2v64.871 (11)O7vii—K1—Si268.93 (6)
K2i—Nd1—K2v64.871 (11)O4xviii—K1—Si2121.67 (6)
K2ii—Nd1—K2v115.129 (11)O9xviii—K1—Si2111.37 (6)
K2iv—Nd1—K2v115.128 (11)O5xxi—K1—Si282.98 (5)
O10i—Nd2—O10vii180.0O3—K1—Si228.61 (4)
O10i—Nd2—O8i88.29 (9)O10vii—K1—Si2111.31 (5)
O10vii—Nd2—O8i91.71 (9)O10xv—K1—Si3xviii106.11 (6)
O10i—Nd2—O8vii91.71 (9)O8i—K1—Si3xviii107.17 (6)
O10vii—Nd2—O8vii88.29 (9)O7vii—K1—Si3xviii153.34 (6)
O8i—Nd2—O8vii180.0O4xviii—K1—Si3xviii63.15 (5)
O10i—Nd2—O7i82.23 (9)O9xviii—K1—Si3xviii26.24 (5)
O10vii—Nd2—O7i97.77 (9)O5xxi—K1—Si3xviii26.76 (4)
O8i—Nd2—O7i108.52 (8)O3—K1—Si3xviii86.15 (5)
O8vii—Nd2—O7i71.48 (8)O10vii—K1—Si3xviii137.91 (5)
O10i—Nd2—O7vii97.77 (9)Si2—K1—Si3xviii106.34 (3)
O10vii—Nd2—O7vii82.23 (9)O10xv—K1—Si3i83.23 (5)
O8i—Nd2—O7vii71.48 (8)O8i—K1—Si3i116.15 (6)
O8vii—Nd2—O7vii108.52 (8)O7vii—K1—Si3i118.09 (6)
O7i—Nd2—O7vii180.0O4xviii—K1—Si3i26.04 (5)
O10i—Nd2—K1123.82 (6)O9xviii—K1—Si3i109.32 (6)
O10vii—Nd2—K156.18 (6)O5xxi—K1—Si3i84.43 (5)
O8i—Nd2—K145.42 (6)O3—K1—Si3i131.25 (5)
O8vii—Nd2—K1134.58 (6)O10vii—K1—Si3i61.40 (5)
O7i—Nd2—K1134.19 (6)Si2—K1—Si3i110.61 (3)
O7vii—Nd2—K145.81 (6)Si3xviii—K1—Si3i88.39 (3)
O10i—Nd2—K1viii56.18 (6)O10xv—K1—Si1xxii117.79 (6)
O10vii—Nd2—K1viii123.81 (6)O8i—K1—Si1xxii98.59 (6)
O8i—Nd2—K1viii134.58 (6)O7vii—K1—Si1xxii149.33 (6)
O8vii—Nd2—K1viii45.42 (6)O4xviii—K1—Si1xxii24.50 (5)
O7i—Nd2—K1viii45.81 (6)O9xviii—K1—Si1xxii62.31 (5)
O7vii—Nd2—K1viii134.19 (6)O5xxi—K1—Si1xxii62.08 (5)
K1—Nd2—K1viii180.0O3—K1—Si1xxii131.83 (6)
O10i—Nd2—K2vii66.47 (6)O10vii—K1—Si1xxii89.95 (5)
O10vii—Nd2—K2vii113.53 (6)Si2—K1—Si1xxii138.60 (4)
O8i—Nd2—K2vii44.69 (7)Si3xviii—K1—Si1xxii48.50 (2)
O8vii—Nd2—K2vii135.31 (7)Si3i—K1—Si1xxii48.49 (2)
O7i—Nd2—K2vii136.61 (6)O1—K2—O6xxi79.73 (7)
O7vii—Nd2—K2vii43.39 (6)O1—K2—O771.40 (7)
K1—Nd2—K2vii58.16 (2)O6xxi—K2—O7147.26 (7)
K1viii—Nd2—K2vii121.84 (2)O1—K2—O2xxiii153.23 (7)
O10i—Nd2—K2i113.53 (6)O6xxi—K2—O2xxiii102.71 (7)
O10vii—Nd2—K2i66.47 (6)O7—K2—O2xxiii110.03 (7)
O8i—Nd2—K2i135.31 (7)O1—K2—O8xv94.26 (7)
O8vii—Nd2—K2i44.69 (7)O6xxi—K2—O8xv114.50 (7)
O7i—Nd2—K2i43.39 (6)O7—K2—O8xv54.45 (6)
O7vii—Nd2—K2i136.61 (6)O2xxiii—K2—O8xv108.33 (7)
K1—Nd2—K2i121.84 (2)O1—K2—O689.88 (7)
K1viii—Nd2—K2i58.16 (2)O6xxi—K2—O665.88 (9)
K2vii—Nd2—K2i180.0O7—K2—O6127.64 (7)
O10i—Nd2—K1vii35.66 (6)O2xxiii—K2—O667.76 (7)
O10vii—Nd2—K1vii144.34 (6)O8xv—K2—O6175.84 (7)
O8i—Nd2—K1vii77.83 (6)O1—K2—O1xxi133.20 (5)
O8vii—Nd2—K1vii102.16 (6)O6xxi—K2—O1xxi88.53 (7)
O7i—Nd2—K1vii55.44 (6)O7—K2—O1xxi99.95 (7)
O7vii—Nd2—K1vii124.56 (6)O2xxiii—K2—O1xxi73.53 (6)
K1—Nd2—K1vii123.24 (3)O8xv—K2—O1xxi50.30 (6)
K1viii—Nd2—K1vii56.76 (3)O6—K2—O1xxi126.03 (7)
K2vii—Nd2—K1vii82.68 (2)O1—K2—Si6xv108.41 (6)
K2i—Nd2—K1vii97.32 (2)O6xxi—K2—Si6xv95.20 (6)
O10i—Nd2—K1i144.34 (6)O7—K2—Si6xv80.01 (5)
O10vii—Nd2—K1i35.66 (6)O2xxiii—K2—Si6xv97.98 (5)
O8i—Nd2—K1i102.17 (6)O8xv—K2—Si6xv25.78 (5)
O8vii—Nd2—K1i77.84 (6)O6—K2—Si6xv151.38 (6)
O7i—Nd2—K1i124.56 (6)O1xxi—K2—Si6xv27.45 (4)
O7vii—Nd2—K1i55.44 (6)O1—K2—Si226.37 (5)
K1—Nd2—K1i56.76 (3)O6xxi—K2—Si271.20 (5)
K1viii—Nd2—K1i123.24 (3)O7—K2—Si276.09 (5)
K2vii—Nd2—K1i97.32 (2)O2xxiii—K2—Si2173.76 (6)
K2i—Nd2—K1i82.68 (2)O8xv—K2—Si276.04 (5)
K1vii—Nd2—K1i180.0O6—K2—Si2107.74 (5)
O12ix—Si1—O4x108.57 (11)O1xxi—K2—Si2107.12 (5)
O12ix—Si1—O4xi108.56 (11)Si6xv—K2—Si284.14 (3)
O4x—Si1—O4xi110.41 (10)O1—K2—Si3xxiii65.47 (5)
O12ix—Si1—O4xii108.55 (11)O6xxi—K2—Si3xxiii143.65 (6)
O4x—Si1—O4xii110.35 (10)O7—K2—Si3xxiii25.23 (5)
O4xi—Si1—O4xii110.33 (10)O2xxiii—K2—Si3xxiii103.87 (5)
O12ix—Si1—K1xiii77.96 (3)O8xv—K2—Si3xxiii79.68 (5)
O4x—Si1—K1xiii87.34 (9)O6—K2—Si3xxiii102.44 (5)
O4xi—Si1—K1xiii47.66 (9)O1xxi—K2—Si3xxiii122.65 (5)
O4xii—Si1—K1xiii156.91 (9)Si6xv—K2—Si3xxiii105.13 (3)
O12ix—Si1—K1xiv77.96 (3)Si2—K2—Si3xxiii81.12 (3)
O4x—Si1—K1xiv47.63 (9)O1—K2—Si5xxiv132.31 (6)
O4xi—Si1—K1xiv156.97 (9)O6xxi—K2—Si5xxiv118.75 (6)
O4xii—Si1—K1xiv87.30 (9)O7—K2—Si5xxiv92.53 (5)
K1xiii—Si1—K1xiv115.79 (2)O2xxiii—K2—Si5xxiv24.47 (5)
O12ix—Si1—K1ii77.96 (3)O8xv—K2—Si5xxiv112.62 (6)
O4x—Si1—K1ii156.89 (9)O6—K2—Si5xxiv64.49 (5)
O4xi—Si1—K1ii87.28 (9)O1xxi—K2—Si5xxiv93.00 (5)
O4xii—Si1—K1ii47.62 (9)Si6xv—K2—Si5xxiv112.54 (3)
K1xiii—Si1—K1ii115.77 (2)Si2—K2—Si5xxiv158.19 (4)
K1xiv—Si1—K1ii115.75 (2)Si3xxiii—K2—Si5xxiv80.94 (3)
O10xv—Si2—O9112.36 (13)O1—K2—Si5xviii156.98 (6)
O10xv—Si2—O3110.83 (13)O6xxi—K2—Si5xviii82.09 (5)
O9—Si2—O3107.21 (13)O7—K2—Si5xviii129.46 (6)
O10xv—Si2—O1113.97 (13)O2xxiii—K2—Si5xviii24.36 (5)
O9—Si2—O1105.20 (13)O8xv—K2—Si5xviii106.11 (5)
O3—Si2—O1106.83 (12)O6—K2—Si5xviii69.75 (5)
O10xv—Si2—K153.05 (9)O1xxi—K2—Si5xviii59.80 (5)
O9—Si2—K196.17 (9)Si6xv—K2—Si5xviii87.13 (3)
O3—Si2—K168.67 (9)Si2—K2—Si5xviii150.92 (3)
O1—Si2—K1158.42 (9)Si3xxiii—K2—Si5xviii127.95 (4)
O10xv—Si2—K290.63 (10)Si5xxiv—K2—Si5xviii48.49 (2)
O9—Si2—K2154.18 (9)Si2—O1—Si6xxv130.26 (15)
O3—Si2—K273.08 (9)Si2—O1—K2101.28 (11)
O1—Si2—K252.35 (9)Si6xxv—O1—K2114.69 (11)
K1—Si2—K2107.41 (3)Si2—O1—K2xxvi122.98 (12)
O7vii—Si3—O9117.44 (13)Si6xxv—O1—K2xxvi91.51 (10)
O7vii—Si3—O5vii113.75 (13)K2—O1—K2xxvi89.76 (7)
O9—Si3—O5vii100.82 (12)Si5xxiii—O2—Si5xxvii145.6 (2)
O7vii—Si3—O4xvi108.92 (14)Si5xxiii—O2—K2vii105.50 (11)
O9—Si3—O4xvi106.03 (14)Si5xxvii—O2—K2vii106.34 (11)
O5vii—Si3—O4xvi109.32 (13)Si2—O3—Si5xxiii141.8 (2)
O7vii—Si3—K1xvii162.11 (10)Si2—O3—K182.72 (9)
O9—Si3—K1xvii52.71 (9)Si5xxiii—O3—K1134.37 (12)
O5vii—Si3—K1xvii59.93 (9)Si1x—O4—Si3xxv135.2 (2)
O4xvi—Si3—K1xvii88.84 (9)Si1x—O4—K1xvii107.89 (12)
O7vii—Si3—K1i73.76 (10)Si3xxv—O4—K1xvii104.10 (11)
O9—Si3—K1i92.72 (9)Si6xxv—O5—Si3xxiii126.19 (15)
O5vii—Si3—K1i158.16 (9)Si6xxv—O5—K1xxvi130.39 (12)
O4xvi—Si3—K1i49.86 (9)Si3xxiii—O5—K1xxvi93.31 (10)
K1xvii—Si3—K1i118.73 (4)Si5xvii—O6—Nd1xxii142.65 (14)
O7vii—Si3—K2vii54.89 (10)Si5xvii—O6—K2xxvi111.57 (12)
O9—Si3—K2vii93.53 (10)Nd1xxii—O6—K2xxvi96.30 (8)
O5vii—Si3—K2vii71.90 (9)Si5xvii—O6—K2110.84 (12)
O4xvi—Si3—K2vii159.51 (10)Nd1xxii—O6—K292.86 (8)
K1xvii—Si3—K2vii108.27 (3)K2xxvi—O6—K289.99 (7)
K1i—Si3—K2vii124.66 (3)Si3xxiii—O7—Nd2xxiii138.23 (14)
O7vii—Si3—K138.79 (9)Si3xxiii—O7—K1xxiii120.60 (13)
O9—Si3—K180.22 (9)Nd2xxiii—O7—K1xxiii95.49 (8)
O5vii—Si3—K1136.16 (9)Si3xxiii—O7—K299.88 (12)
O4xvi—Si3—K1112.41 (9)Nd2xxiii—O7—K2102.88 (8)
K1xvii—Si3—K1132.54 (3)K1xxiii—O7—K286.40 (7)
K1i—Si3—K162.81 (3)Si6—O8—Nd2xxiii145.2 (2)
K2vii—Si3—K164.32 (3)Si6—O8—K1i113.30 (13)
O12ix—Si4—O11xii108.08 (11)Nd2xxiii—O8—K1i97.85 (8)
O12ix—Si4—O11x108.06 (11)Si6—O8—K2xv95.05 (12)
O11xii—Si4—O11x110.87 (10)Nd2xxiii—O8—K2xv103.08 (9)
O12ix—Si4—O11xi108.06 (11)K1i—O8—K2xv85.07 (7)
O11xii—Si4—O11xi110.85 (10)Si3—O9—Si2134.3 (2)
O11x—Si4—O11xi110.79 (10)Si3—O9—K1xvii101.05 (11)
O6xviii—Si5—O2vii114.78 (13)Si2—O9—K1xvii124.60 (12)
O6xviii—Si5—O3vii111.30 (13)Si2xv—O10—Nd2xxiii139.87 (14)
O2vii—Si5—O3vii104.61 (13)Si2xv—O10—K1xv99.57 (11)
O6xviii—Si5—O2xix112.23 (13)Nd2xxiii—O10—K1xv114.46 (9)
O2vii—Si5—O2xix107.00 (11)Si2xv—O10—K1xxiii120.45 (12)
O3vii—Si5—O2xix106.28 (13)Nd2xxiii—O10—K1xxiii86.75 (7)
O6xviii—Si5—K2xx164.49 (10)K1xv—O10—K1xxiii80.98 (7)
O2vii—Si5—K2xx50.02 (9)Si4x—O11—Si6136.9 (2)
O3vii—Si5—K2xx74.12 (9)Si4ix—O12—Si1ix179.997 (1)
O2xix—Si5—K2xx78.74 (9)
Symmetry codes: (i) x1, y1, z1; (ii) x+1, y+1, z+1; (iii) xy, x+1, z1; (iv) y1, xy, z+1; (v) x+y, x1, z+1; (vi) y+1, x+y, z1; (vii) x, y, z+1; (viii) x1, y1, z; (ix) x+1, y+1, z+1; (x) x, y, z; (xi) xy+1, x+1, z; (xii) y+1, x+y, z; (xiii) y, xy, z+1; (xiv) x+y+1, x, z+1; (xv) x1, y1, z2; (xvi) y1, xy, z; (xvii) xy1, x, z1; (xviii) y, x+y1, z1; (xix) xy1, x, z; (xx) x, y, z+2; (xxi) y, x+y1, z2; (xxii) x1, y1, z1; (xxiii) x, y, z1; (xxiv) x, y, z2; (xxv) x+y1, x1, z; (xxvi) xy1, x, z2; (xxvii) y, x+y1, z.

Experimental details

Crystal data
Chemical formulaK3NdO17Si7
Mr730.17
Crystal system, space groupHexagonal, P3
Temperature (K)293
a, c (Å)16.131 (2), 7.175 (2)
V3)1616.9 (5)
Z4
Radiation typeMo Kα
µ (mm1)4.60
Crystal size (mm) × ×
Data collection
DiffractometerNonius 4-circle
diffractometer
Absorption correctionψ scan
Tmin, Tmax0.277, 0.323
No. of measured, independent and
observed [I σ(I)] reflections
2740, 2474, 2469
Rint0.028
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.071, 1.27
No. of reflections2469
No. of parameters172
Δρmax, Δρmin (e Å3)0.95, 1.72

Computer programs: Nonius Software, SHELXS86 (Sheldrick, 1985), SHELXL93 (Sheldrick, 1993), Atoms (Dowty, 1999).

 

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