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The title compounds, namely hexa­caesium tetra­niobium docosa­selenide and dodeca­potassium hexa­niobium penta­triacontaselenide, were formed from their respective alkali chalcogenide reactive flux and niobium metal. Both compounds fall into the larger family of solid-state compounds that contain the M2Q11 building block (M = Nb, Ta; Q = Se, S), where the metal chalcogenide forms dimers of face-shared penta­gonal bipyramids. Cs6Nb4Se22 contains two Nb2Se11 building blocks linked by an Se-Se bond to form isolated Nb4Se22 tetra­meric building blocks surrounded by caesium ions. K12Nb6Se35.3 contains similar Nb4Se22 tetra­mers that are linked by an Se-Se-Se unit to an Nb2Se11 dimer to form one-dimensional anionic chains surrounded by potassium ions. Further crystallographic studies of K12Nb6Se35.3 demonstrate a new M2Se12 building block because of disorder between an Se2- site (85%) and an (Se-Se)2- unit (15%). The subtle differences between the structures are discussed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110017038/ku3024sup1.cif
Contains datablocks I, II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110017038/ku3024Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110017038/ku3024IIsup3.hkl
Contains datablock II

Computing details top

For both compounds, data collection: APEX2 (Bruker, 2008); cell refinement: SAINT-Plus (Bruker, 2008). Data reduction: SAINT-Plus (Bruker, 2008) for (I); SAINT-Plus (Bruker 2008) for (II). For both compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalMaker (CrystalMaker Software, 2009); software used to prepare material for publication: APEX2 (Bruker, 2008).

(I) Hexacaesium tetraniobium docosaselenide top
Crystal data top
Cs6Nb4Se22F(000) = 2484
Mr = 2906.22Dx = 4.566 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 12.5887 (6) ÅCell parameters from 5633 reflections
b = 8.5127 (4) Åθ = 4.7–52.1°
c = 20.3151 (10) ŵ = 25.10 mm1
β = 103.853 (1)°T = 296 K
V = 2113.72 (18) Å3Needle, black
Z = 20.2 × 0.08 × 0.06 mm
Data collection top
Bruker APEXII CCD
diffractometer
4844 independent reflections
Radiation source: fine-focus sealed tube3550 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.065
ω and φ scansθmax = 27.5°, θmin = 1.7°
Absorption correction: empirical (using intensity measurements)
(SADABS; Bruker, 2008)
h = 1616
Tmin = 0.347, Tmax = 0.746k = 1110
35929 measured reflectionsl = 2626
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.038Secondary atom site location: difference Fourier map
wR(F2) = 0.089 w = 1/[σ2(Fo2) + (0.031P)2 + 18.3443P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
4844 reflectionsΔρmax = 4.93 e Å3
145 parametersΔρmin = 2.29 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nb10.80152 (6)0.23308 (9)0.50654 (4)0.02341 (17)
Nb20.70707 (7)0.35623 (10)0.66030 (4)0.03012 (19)
Se11.00252 (7)0.13484 (10)0.51394 (5)0.0294 (2)
Se20.89435 (7)0.23574 (11)0.65594 (4)0.0299 (2)
Se30.73578 (7)0.50305 (10)0.54883 (5)0.0303 (2)
Se40.75335 (8)0.05493 (11)0.52764 (5)0.0371 (2)
Se50.79063 (8)0.10354 (12)0.72163 (5)0.0388 (2)
Se60.51018 (8)0.43174 (14)0.59217 (6)0.0465 (3)
Se70.74133 (9)0.26233 (15)0.38919 (5)0.0486 (3)
Se80.62574 (7)0.14011 (11)0.54042 (4)0.0308 (2)
Se90.92141 (7)0.48537 (10)0.54525 (5)0.0316 (2)
Se100.52464 (10)0.27314 (17)0.68849 (6)0.0615 (3)
Se110.76529 (11)0.56779 (15)0.73383 (6)0.0614 (4)
Cs11.00418 (6)0.17210 (8)0.33806 (3)0.04514 (17)
Cs20.54136 (7)0.15562 (9)0.64033 (4)0.0602 (2)
Cs31.22961 (6)0.31969 (9)0.62045 (3)0.0537 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0223 (4)0.0250 (4)0.0232 (4)0.0013 (3)0.0058 (3)0.0011 (3)
Nb20.0288 (4)0.0372 (5)0.0244 (4)0.0052 (4)0.0065 (3)0.0027 (3)
Se10.0241 (4)0.0249 (4)0.0399 (5)0.0008 (4)0.0091 (4)0.0057 (4)
Se20.0266 (5)0.0329 (5)0.0283 (4)0.0025 (4)0.0030 (4)0.0020 (4)
Se30.0296 (5)0.0281 (5)0.0333 (5)0.0059 (4)0.0077 (4)0.0017 (4)
Se40.0404 (6)0.0267 (5)0.0456 (6)0.0062 (4)0.0130 (4)0.0052 (4)
Se50.0426 (6)0.0425 (6)0.0307 (5)0.0006 (5)0.0074 (4)0.0066 (4)
Se60.0284 (5)0.0624 (7)0.0478 (6)0.0093 (5)0.0072 (4)0.0012 (5)
Se70.0434 (6)0.0696 (8)0.0328 (5)0.0024 (5)0.0095 (5)0.0011 (5)
Se80.0253 (5)0.0384 (5)0.0289 (5)0.0066 (4)0.0070 (4)0.0013 (4)
Se90.0297 (5)0.0262 (4)0.0395 (5)0.0042 (4)0.0094 (4)0.0019 (4)
Se100.0458 (7)0.0906 (10)0.0580 (7)0.0078 (7)0.0321 (6)0.0115 (7)
Se110.0697 (8)0.0578 (7)0.0471 (7)0.0178 (6)0.0050 (6)0.0236 (6)
Cs10.0521 (4)0.0457 (4)0.0337 (3)0.0115 (3)0.0025 (3)0.0012 (3)
Cs20.0660 (5)0.0573 (5)0.0511 (4)0.0158 (4)0.0019 (4)0.0129 (3)
Cs30.0447 (4)0.0707 (5)0.0399 (4)0.0153 (4)0.0013 (3)0.0100 (3)
Geometric parameters (Å, º) top
Nb1—Se72.3355 (13)Se7—Cs13.7768 (13)
Nb1—Se42.5859 (12)Se8—Cs23.5522 (11)
Nb1—Se82.5934 (12)Se8—Cs2vii3.7719 (11)
Nb1—Se92.6344 (11)Se9—Cs1iii3.7331 (11)
Nb1—Se12.6348 (12)Se9—Cs3iii3.8255 (12)
Nb1—Se32.6543 (11)Se9—Cs34.0667 (12)
Nb1—Se22.9799 (11)Se10—Cs3vi3.6610 (15)
Nb2—Se112.3425 (14)Se10—Cs23.7976 (17)
Nb2—Se52.5804 (13)Se10—Cs2viii3.8124 (14)
Nb2—Se22.5919 (12)Se11—Cs3ix3.6436 (13)
Nb2—Se102.5948 (14)Se11—Cs2v3.8123 (15)
Nb2—Se62.6134 (13)Se11—Cs1ii3.8274 (14)
Nb2—Se32.6856 (12)Se11—Cs1iii4.1818 (17)
Nb2—Se83.0283 (12)Cs1—Se5x3.6640 (12)
Se1—Se1i2.3616 (17)Cs1—Se2i3.6913 (11)
Se1—Cs33.5170 (11)Cs1—Se2x3.7102 (11)
Se1—Cs13.5920 (11)Cs1—Se4i3.7105 (12)
Se1—Cs1i3.9994 (11)Cs1—Se9iii3.7331 (11)
Se2—Se52.3636 (13)Cs1—Se11x3.8274 (14)
Se2—Cs1i3.6913 (11)Cs1—Se5i3.8922 (12)
Se2—Cs1ii3.7102 (11)Cs1—Se1i3.9994 (11)
Se3—Se92.3601 (13)Cs1—Se11iii4.1818 (17)
Se3—Cs3iii3.8743 (11)Cs2—Se7vii3.5815 (14)
Se4—Se82.3674 (13)Cs2—Se6xi3.6423 (15)
Se4—Cs1i3.7105 (12)Cs2—Se8vii3.7719 (11)
Se4—Cs3i3.8058 (12)Cs2—Se11xi3.8123 (15)
Se4—Cs24.0030 (13)Cs2—Se10xii3.8124 (14)
Se5—Cs1ii3.6640 (12)Cs3—Se7iii3.5870 (15)
Se5—Cs23.8678 (13)Cs3—Se11iv3.6436 (13)
Se5—Cs1i3.8921 (12)Cs3—Se10xiii3.6610 (15)
Se5—Cs3iv4.0728 (12)Cs3—Se4i3.8058 (12)
Se6—Se102.3483 (17)Cs3—Se9iii3.8255 (12)
Se6—Cs2v3.6423 (14)Cs3—Se6xiii3.8323 (13)
Se6—Cs3vi3.8323 (13)Cs3—Se3iii3.8742 (11)
Se7—Cs2vii3.5815 (14)Cs3—Se5ix4.0728 (12)
Se7—Cs3iii3.5871 (15)
Se7—Nb1—Se4103.80 (5)Nb2—Se11—Cs1iii108.77 (5)
Se7—Nb1—Se8102.39 (4)Cs3ix—Se11—Cs1iii95.36 (3)
Se4—Nb1—Se854.40 (3)Cs2v—Se11—Cs1iii89.50 (3)
Se7—Nb1—Se9103.91 (4)Cs1ii—Se11—Cs1iii87.52 (3)
Se4—Nb1—Se9149.74 (4)Se1—Cs1—Se5x120.67 (3)
Se8—Nb1—Se9129.33 (4)Se1—Cs1—Se2i88.20 (2)
Se7—Nb1—Se199.47 (4)Se5x—Cs1—Se2i134.93 (3)
Se4—Nb1—Se187.12 (4)Se1—Cs1—Se2x157.07 (3)
Se8—Nb1—Se1139.18 (4)Se5x—Cs1—Se2x37.38 (2)
Se9—Nb1—Se176.59 (3)Se2i—Cs1—Se2x105.97 (2)
Se7—Nb1—Se3100.84 (4)Se1—Cs1—Se4i56.26 (2)
Se4—Nb1—Se3131.58 (4)Se5x—Cs1—Se4i164.17 (3)
Se8—Nb1—Se380.00 (4)Se2i—Cs1—Se4i60.37 (2)
Se9—Nb1—Se353.01 (3)Se2x—Cs1—Se4i146.58 (3)
Se1—Nb1—Se3128.75 (4)Se1—Cs1—Se9iii59.85 (2)
Se7—Nb1—Se2172.37 (5)Se5x—Cs1—Se9iii92.09 (3)
Se4—Nb1—Se283.61 (3)Se2i—Cs1—Se9iii132.96 (3)
Se8—Nb1—Se283.31 (3)Se2x—Cs1—Se9iii116.42 (3)
Se9—Nb1—Se268.46 (3)Se4i—Cs1—Se9iii72.89 (2)
Se1—Nb1—Se278.89 (3)Se1—Cs1—Se761.98 (2)
Se3—Nb1—Se274.95 (3)Se5x—Cs1—Se761.04 (3)
Se11—Nb2—Se5107.69 (5)Se2i—Cs1—Se7120.08 (3)
Se11—Nb2—Se2100.24 (5)Se2x—Cs1—Se795.13 (3)
Se5—Nb2—Se254.38 (3)Se4i—Cs1—Se7118.23 (3)
Se11—Nb2—Se10103.13 (6)Se9iii—Cs1—Se776.68 (3)
Se5—Nb2—Se1086.92 (5)Se1—Cs1—Se11x108.20 (3)
Se2—Nb2—Se10139.47 (5)Se5x—Cs1—Se11x64.09 (3)
Se11—Nb2—Se6105.12 (5)Se2i—Cs1—Se11x74.71 (3)
Se5—Nb2—Se6133.32 (5)Se2x—Cs1—Se11x60.35 (2)
Se2—Nb2—Se6146.55 (4)Se4i—Cs1—Se11x131.49 (3)
Se10—Nb2—Se653.60 (4)Se9iii—Cs1—Se11x144.35 (3)
Se11—Nb2—Se395.46 (5)Se7—Cs1—Se11x68.69 (3)
Se5—Nb2—Se3132.34 (4)Se1—Cs1—Se5i114.77 (3)
Se2—Nb2—Se381.27 (4)Se5x—Cs1—Se5i123.52 (2)
Se10—Nb2—Se3128.16 (5)Se2i—Cs1—Se5i36.20 (2)
Se6—Nb2—Se374.99 (4)Se2x—Cs1—Se5i86.18 (2)
Se11—Nb2—Se8166.86 (5)Se4i—Cs1—Se5i64.95 (2)
Se5—Nb2—Se884.38 (4)Se9iii—Cs1—Se5i125.76 (3)
Se2—Nb2—Se882.37 (3)Se7—Cs1—Se5i154.00 (3)
Se10—Nb2—Se882.25 (4)Se11x—Cs1—Se5i89.89 (3)
Se6—Nb2—Se868.18 (4)Se1—Cs1—Se1i35.74 (3)
Se3—Nb2—Se872.09 (3)Se5x—Cs1—Se1i132.97 (3)
Se1i—Se1—Nb1108.94 (5)Se2i—Cs1—Se1i55.26 (2)
Se1i—Se1—Cs3123.62 (5)Se2x—Cs1—Se1i144.87 (3)
Nb1—Se1—Cs3121.41 (4)Se4i—Cs1—Se1i55.48 (2)
Se1i—Se1—Cs181.58 (5)Se9iii—Cs1—Se1i94.60 (2)
Nb1—Se1—Cs198.60 (3)Se7—Cs1—Se1i75.44 (2)
Cs3—Se1—Cs1112.02 (3)Se11x—Cs1—Se1i84.96 (2)
Se1i—Se1—Cs1i62.68 (4)Se5i—Cs1—Se1i88.59 (2)
Nb1—Se1—Cs1i93.29 (3)Se1—Cs1—Se11iii124.33 (3)
Cs3—Se1—Cs1i89.44 (2)Se5x—Cs1—Se11iii87.81 (3)
Cs1—Se1—Cs1i144.26 (2)Se2i—Cs1—Se11iii104.24 (3)
Se5—Se2—Nb262.56 (4)Se2x—Cs1—Se11iii70.36 (2)
Se5—Se2—Nb1115.88 (4)Se4i—Cs1—Se11iii83.20 (3)
Nb2—Se2—Nb184.24 (3)Se9iii—Cs1—Se11iii73.65 (2)
Se5—Se2—Cs1i76.53 (4)Se7—Cs1—Se11iii135.67 (3)
Nb2—Se2—Cs1i132.96 (4)Se11x—Cs1—Se11iii127.47 (2)
Nb1—Se2—Cs1i94.28 (3)Se5i—Cs1—Se11iii69.06 (2)
Se5—Se2—Cs1ii70.25 (3)Se1i—Cs1—Se11iii138.57 (3)
Nb2—Se2—Cs1ii90.41 (3)Se8—Cs2—Se7vii120.34 (3)
Nb1—Se2—Cs1ii168.21 (4)Se8—Cs2—Se6xi123.90 (3)
Cs1i—Se2—Cs1ii97.04 (2)Se7vii—Cs2—Se6xi70.83 (3)
Se9—Se3—Nb163.07 (3)Se8—Cs2—Se8vii65.94 (3)
Se9—Se3—Nb2109.29 (4)Se7vii—Cs2—Se8vii62.98 (2)
Nb1—Se3—Nb289.16 (4)Se6xi—Cs2—Se8vii76.89 (3)
Se9—Se3—Cs3iii71.03 (3)Se8—Cs2—Se1060.57 (3)
Nb1—Se3—Cs3iii86.55 (3)Se7vii—Cs2—Se1099.95 (3)
Nb2—Se3—Cs3iii174.95 (4)Se6xi—Cs2—Se10170.77 (4)
Se8—Se4—Nb162.96 (4)Se8vii—Cs2—Se1099.48 (3)
Se8—Se4—Cs1i124.63 (4)Se8—Cs2—Se11xi115.83 (4)
Nb1—Se4—Cs1i101.10 (3)Se7vii—Cs2—Se11xi120.89 (4)
Se8—Se4—Cs3i132.08 (4)Se6xi—Cs2—Se11xi63.74 (3)
Nb1—Se4—Cs3i111.76 (4)Se8vii—Cs2—Se11xi132.86 (3)
Cs1i—Se4—Cs3i103.29 (3)Se10—Cs2—Se11xi123.04 (3)
Se8—Se4—Cs261.62 (3)Se8—Cs2—Se10xii142.58 (4)
Nb1—Se4—Cs2120.84 (4)Se7vii—Cs2—Se10xii71.80 (3)
Cs1i—Se4—Cs293.76 (3)Se6xi—Cs2—Se10xii93.36 (3)
Cs3i—Se4—Cs2119.78 (3)Se8vii—Cs2—Se10xii134.51 (3)
Se2—Se5—Nb263.06 (4)Se10—Cs2—Se10xii83.12 (3)
Se2—Se5—Cs1ii72.37 (3)Se11xi—Cs2—Se10xii75.16 (3)
Nb2—Se5—Cs1ii91.63 (4)Se8—Cs2—Se561.10 (2)
Se2—Se5—Cs2122.13 (4)Se7vii—Cs2—Se5152.65 (4)
Nb2—Se5—Cs294.25 (4)Se6xi—Cs2—Se5133.55 (3)
Cs1ii—Se5—Cs2165.43 (3)Se8vii—Cs2—Se5127.02 (3)
Se2—Se5—Cs1i67.27 (3)Se10—Cs2—Se555.33 (3)
Nb2—Se5—Cs1i125.19 (4)Se11xi—Cs2—Se573.26 (3)
Cs1ii—Se5—Cs1i94.37 (2)Se10xii—Cs2—Se591.89 (3)
Cs2—Se5—Cs1i93.11 (3)Se8—Cs2—Se435.90 (2)
Se2—Se5—Cs3iv150.98 (4)Se7vii—Cs2—Se4136.91 (3)
Nb2—Se5—Cs3iv141.24 (4)Se6xi—Cs2—Se495.54 (3)
Cs1ii—Se5—Cs3iv88.59 (2)Se8vii—Cs2—Se474.25 (2)
Cs2—Se5—Cs3iv78.50 (2)Se10—Cs2—Se491.56 (3)
Cs1i—Se5—Cs3iv93.39 (3)Se11xi—Cs2—Se484.40 (3)
Se10—Se6—Nb262.79 (4)Se10xii—Cs2—Se4151.22 (3)
Se10—Se6—Cs2v110.41 (5)Se5—Cs2—Se462.50 (2)
Nb2—Se6—Cs2v93.86 (4)Se1—Cs3—Se7iii119.26 (3)
Se10—Se6—Cs3vi67.81 (4)Se1—Cs3—Se11iv95.17 (3)
Nb2—Se6—Cs3vi130.59 (4)Se7iii—Cs3—Se11iv130.24 (3)
Cs2v—Se6—Cs3vi104.10 (3)Se1—Cs3—Se10xiii141.78 (4)
Nb1—Se7—Cs2vii102.15 (4)Se7iii—Cs3—Se10xiii91.17 (3)
Nb1—Se7—Cs3iii98.57 (4)Se11iv—Cs3—Se10xiii79.08 (3)
Cs2vii—Se7—Cs3iii110.65 (4)Se1—Cs3—Se4i55.95 (2)
Nb1—Se7—Cs199.65 (4)Se7iii—Cs3—Se4i121.23 (3)
Cs2vii—Se7—Cs1143.44 (4)Se11iv—Cs3—Se4i107.48 (3)
Cs3iii—Se7—Cs194.54 (3)Se10xiii—Cs3—Se4i89.45 (3)
Se4—Se8—Nb162.64 (4)Se1—Cs3—Se9iii59.55 (2)
Se4—Se8—Nb2113.99 (4)Se7iii—Cs3—Se9iii63.73 (2)
Nb1—Se8—Nb283.24 (3)Se11iv—Cs3—Se9iii151.47 (3)
Se4—Se8—Cs282.49 (4)Se10xiii—Cs3—Se9iii128.66 (3)
Nb1—Se8—Cs2139.36 (4)Se4i—Cs3—Se9iii70.83 (2)
Nb2—Se8—Cs293.49 (3)Se1—Cs3—Se6xiii131.43 (3)
Se4—Se8—Cs2vii98.78 (4)Se7iii—Cs3—Se6xiii68.61 (3)
Nb1—Se8—Cs2vii92.49 (3)Se11iv—Cs3—Se6xiii115.51 (3)
Nb2—Se8—Cs2vii139.82 (4)Se10xiii—Cs3—Se6xiii36.44 (3)
Cs2—Se8—Cs2vii114.06 (3)Se4i—Cs3—Se6xiii78.49 (3)
Se3—Se9—Nb163.93 (3)Se9iii—Cs3—Se6xiii92.40 (3)
Se3—Se9—Cs1iii91.74 (4)Se1—Cs3—Se3iii82.86 (2)
Nb1—Se9—Cs1iii149.89 (4)Se7iii—Cs3—Se3iii62.00 (2)
Se3—Se9—Cs3iii73.28 (3)Se11iv—Cs3—Se3iii165.15 (4)
Nb1—Se9—Cs3iii87.85 (3)Se10xiii—Cs3—Se3iii93.31 (3)
Cs1iii—Se9—Cs3iii102.48 (3)Se4i—Cs3—Se3iii59.30 (2)
Se3—Se9—Cs3150.83 (4)Se9iii—Cs3—Se3iii35.69 (2)
Nb1—Se9—Cs3104.85 (3)Se6xiii—Cs3—Se3iii57.75 (2)
Cs1iii—Se9—Cs387.74 (2)Se1—Cs3—Se950.37 (2)
Cs3iii—Se9—Cs3135.19 (3)Se7iii—Cs3—Se974.70 (3)
Se6—Se10—Nb263.61 (4)Se11iv—Cs3—Se9109.81 (3)
Se6—Se10—Cs3vi75.76 (4)Se10xiii—Cs3—Se9165.87 (3)
Nb2—Se10—Cs3vi139.35 (5)Se4i—Cs3—Se997.91 (2)
Se6—Se10—Cs2109.63 (5)Se9iii—Cs3—Se944.81 (3)
Nb2—Se10—Cs295.66 (4)Se6xiii—Cs3—Se9133.47 (3)
Cs3vi—Se10—Cs296.92 (4)Se3iii—Cs3—Se980.30 (2)
Se6—Se10—Cs2viii132.71 (6)Se1—Cs3—Se5ix123.72 (3)
Nb2—Se10—Cs2viii123.76 (5)Se7iii—Cs3—Se5ix58.73 (3)
Cs3vi—Se10—Cs2viii84.51 (3)Se11iv—Cs3—Se5ix72.62 (3)
Cs2—Se10—Cs2viii115.18 (4)Se10xiii—Cs3—Se5ix90.91 (3)
Nb2—Se11—Cs3ix155.85 (6)Se4i—Cs3—Se5ix179.64 (3)
Nb2—Se11—Cs2v94.36 (4)Se9iii—Cs3—Se5ix108.91 (3)
Cs3ix—Se11—Cs2v84.74 (3)Se6xiii—Cs3—Se5ix101.78 (3)
Nb2—Se11—Cs1ii91.55 (4)Se3iii—Cs3—Se5ix120.64 (3)
Cs3ix—Se11—Cs1ii90.33 (3)Se9—Cs3—Se5ix81.73 (2)
Cs2v—Se11—Cs1ii173.98 (4)
Symmetry codes: (i) x+2, y, z+1; (ii) x, y+1/2, z+1/2; (iii) x+2, y+1, z+1; (iv) x+2, y1/2, z+3/2; (v) x, y+1, z; (vi) x1, y, z; (vii) x+1, y, z+1; (viii) x+1, y+1/2, z+3/2; (ix) x+2, y+1/2, z+3/2; (x) x, y+1/2, z1/2; (xi) x, y1, z; (xii) x+1, y1/2, z+3/2; (xiii) x+1, y, z.
(II) dodecapotassium hexaniobium pentatriacontaselenide top
Crystal data top
K12Nb6Se35.30Dx = 4.099 Mg m3
Mr = 3810.00Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcnCell parameters from 8508 reflections
a = 8.3290 (4) Åθ = 4.4–48.7°
b = 13.2559 (7) ŵ = 22.69 mm1
c = 55.974 (3) ÅT = 100 K
V = 6180.0 (5) Å3Plate, black
Z = 40.16 × 0.12 × 0.02 mm
F(000) = 6697
Data collection top
Bruker APEXII CCD
diffractometer
5107 independent reflections
Radiation source: fine-focus sealed tube4470 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.074
ω and φ scansθmax = 24.4°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements)
(SADABS; Bruker, 2008)
h = 99
Tmin = 0.380, Tmax = 0.745k = 1515
53662 measured reflectionsl = 6565
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.031Secondary atom site location: difference Fourier map
wR(F2) = 0.063 w = 1/[σ2(Fo2) + (0.0014P)2 + 93.4847P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max = 0.001
5107 reflectionsΔρmax = 1.96 e Å3
263 parametersΔρmin = 0.97 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Nb10.04055 (8)0.13613 (5)0.047032 (13)0.00663 (16)
Nb20.56408 (9)0.21560 (5)0.218406 (13)0.00765 (16)
Nb30.04190 (8)0.05393 (5)0.110845 (13)0.00614 (16)
Se10.34720 (9)0.10761 (6)0.050461 (15)0.01015 (18)
Se20.19337 (9)0.14446 (6)0.077886 (14)0.00756 (17)
Se30.08333 (10)0.11819 (6)0.097098 (15)0.00894 (18)
Se40.43858 (10)0.09735 (6)0.186624 (15)0.01356 (19)
Se50.12568 (9)0.04697 (6)0.073411 (14)0.00742 (17)
Se60.00073 (10)0.24204 (6)0.119925 (15)0.00955 (18)
Se70.11822 (10)0.01882 (6)0.011250 (15)0.01058 (18)
Se80.71760 (9)0.15174 (6)0.255859 (14)0.00871 (18)
Se90.20400 (9)0.19291 (6)0.085980 (14)0.00792 (18)
Se100.67021 (10)0.03176 (6)0.225458 (15)0.01108 (18)
Se110.24578 (10)0.00344 (6)0.137888 (15)0.01300 (19)
Se120.23252 (9)0.04710 (6)0.042809 (14)0.01003 (18)
Se130.21767 (10)0.02909 (6)0.136669 (14)0.01073 (18)
Se140.32294 (10)0.33432 (6)0.211489 (15)0.01188 (19)
Se160.25798 (10)0.17889 (6)0.159701 (15)0.01254 (19)
Se150.50000.36262 (8)0.25000.0087 (2)
Se170.77138 (11)0.29302 (7)0.196531 (16)0.0174 (2)
Se180.01459 (15)0.29337 (8)0.02814 (2)0.0145 (2)0.85
Se190.1020 (8)0.2440 (5)0.01393 (12)0.0242 (15)0.15
Se200.0966 (9)0.3188 (5)0.03782 (14)0.0260 (16)0.15
K10.50000.00000.00000.0172 (6)
K20.50000.1672 (2)0.25000.0141 (6)
K30.0893 (3)0.19994 (16)0.03207 (4)0.0286 (5)
K40.0147 (2)0.04036 (16)0.18954 (4)0.0246 (5)
K50.0265 (2)0.44109 (17)0.08581 (4)0.0260 (5)
K60.5523 (2)0.11994 (14)0.16630 (3)0.0167 (4)
K70.3839 (2)0.24864 (15)0.14025 (3)0.0158 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0056 (4)0.0095 (4)0.0048 (4)0.0010 (3)0.0008 (3)0.0001 (3)
Nb20.0094 (4)0.0083 (4)0.0052 (4)0.0009 (3)0.0005 (3)0.0010 (3)
Nb30.0067 (4)0.0074 (4)0.0044 (4)0.0001 (3)0.0006 (3)0.0004 (3)
Se10.0057 (4)0.0170 (5)0.0077 (4)0.0009 (3)0.0013 (3)0.0015 (4)
Se20.0071 (4)0.0094 (4)0.0061 (4)0.0015 (3)0.0013 (3)0.0001 (3)
Se30.0094 (4)0.0075 (4)0.0099 (4)0.0012 (3)0.0000 (3)0.0002 (3)
Se40.0186 (5)0.0125 (4)0.0096 (4)0.0024 (4)0.0060 (4)0.0038 (4)
Se50.0072 (4)0.0085 (4)0.0066 (4)0.0017 (3)0.0003 (3)0.0007 (3)
Se60.0134 (4)0.0082 (4)0.0071 (4)0.0001 (3)0.0018 (3)0.0021 (3)
Se70.0071 (4)0.0180 (5)0.0066 (4)0.0008 (3)0.0000 (3)0.0045 (3)
Se80.0079 (4)0.0108 (4)0.0074 (4)0.0008 (3)0.0010 (3)0.0003 (3)
Se90.0088 (4)0.0088 (4)0.0061 (4)0.0029 (3)0.0009 (3)0.0003 (3)
Se100.0133 (4)0.0089 (4)0.0111 (4)0.0024 (3)0.0003 (3)0.0020 (3)
Se110.0140 (4)0.0134 (4)0.0116 (4)0.0006 (4)0.0049 (4)0.0013 (4)
Se120.0055 (4)0.0169 (5)0.0077 (4)0.0005 (3)0.0003 (3)0.0034 (3)
Se130.0108 (4)0.0135 (4)0.0079 (4)0.0017 (3)0.0036 (3)0.0021 (3)
Se140.0136 (4)0.0127 (4)0.0093 (4)0.0044 (4)0.0025 (4)0.0017 (4)
Se160.0120 (4)0.0136 (4)0.0120 (4)0.0004 (4)0.0040 (4)0.0026 (4)
Se150.0131 (6)0.0064 (6)0.0067 (6)0.0000.0010 (5)0.000
Se170.0185 (5)0.0198 (5)0.0138 (5)0.0059 (4)0.0042 (4)0.0004 (4)
Se180.0174 (6)0.0125 (6)0.0138 (6)0.0016 (5)0.0000 (5)0.0044 (5)
Se190.027 (4)0.020 (3)0.026 (4)0.002 (3)0.004 (3)0.005 (3)
Se200.028 (4)0.020 (4)0.030 (4)0.002 (3)0.009 (4)0.001 (3)
K10.0122 (13)0.0247 (15)0.0146 (14)0.0005 (12)0.0004 (11)0.0033 (12)
K20.0137 (13)0.0129 (13)0.0156 (15)0.0000.0020 (11)0.000
K30.0415 (14)0.0177 (11)0.0267 (13)0.0063 (10)0.0079 (10)0.0047 (9)
K40.0236 (11)0.0313 (12)0.0191 (11)0.0039 (10)0.0073 (9)0.0081 (9)
K50.0112 (10)0.0312 (12)0.0356 (13)0.0031 (9)0.0034 (9)0.0229 (10)
K60.0200 (10)0.0148 (10)0.0153 (10)0.0001 (8)0.0005 (8)0.0020 (8)
K70.0136 (10)0.0201 (10)0.0137 (10)0.0032 (8)0.0024 (8)0.0001 (8)
Geometric parameters (Å, º) top
Nb1—Se182.3473 (12)Se16—K6viii3.191 (2)
Nb1—Se202.520 (7)Se16—K7vii3.307 (2)
Nb1—Se122.5732 (11)Se16—K43.364 (2)
Nb1—Se12.5890 (11)Se15—Se14i2.6387 (9)
Nb1—Se22.6059 (10)Se15—Nb2i2.6853 (11)
Nb1—Se72.6169 (11)Se17—K6x3.110 (2)
Nb1—Se192.624 (7)Se17—K7vii3.456 (2)
Nb1—Se92.6781 (11)Se17—K2ix3.5863 (10)
Nb1—Se52.9281 (11)Se17—K4vii3.814 (2)
Nb2—Se172.3523 (11)Se17—K4x3.934 (2)
Nb2—Se142.5808 (11)Se18—Se200.935 (8)
Nb2—Se42.5913 (11)Se18—Se191.415 (7)
Nb2—Se82.5974 (11)Se18—K1v3.1619 (10)
Nb2—Se102.6222 (11)Se18—K3v3.550 (3)
Nb2—Se152.6852 (11)Se18—K33.644 (3)
Nb2—Se8i2.8803 (11)Se18—K53.791 (3)
Nb3—Se112.3713 (11)Se19—Se202.347 (11)
Nb3—Se62.5678 (10)Se19—K3v2.862 (7)
Nb3—Se52.5819 (10)Se19—K33.084 (7)
Nb3—Se132.6214 (11)Se19—K1v3.584 (7)
Nb3—Se32.6240 (10)Se20—K53.300 (8)
Nb3—Se92.6747 (10)Se20—K1v3.301 (7)
Nb3—Se22.9467 (11)K1—Se18ii3.1619 (10)
Se1—Se92.5794 (11)K1—Se18iii3.1619 (10)
Se1—K5ii3.319 (2)K1—Se7xii3.2512 (8)
Se1—K13.4106 (8)K1—Se20ii3.301 (7)
Se1—K3iii3.411 (2)K1—Se20iii3.301 (7)
Se2—Se122.3720 (11)K1—Se12vi3.3309 (8)
Se2—K5iv3.592 (2)K1—Se12xiii3.3309 (8)
Se2—K3v3.756 (2)K1—Se1xii3.4106 (8)
Se3—Se52.3833 (11)K1—Se19ii3.584 (7)
Se3—K5iv3.402 (2)K1—Se19iii3.584 (7)
Se3—K7ii3.422 (2)K2—Se10xiv3.294 (2)
Se3—K3vi3.798 (2)K2—Se10xiii3.294 (2)
Se4—Se162.3879 (12)K2—Se8iv3.377 (2)
Se4—K6vii3.098 (2)K2—Se8xv3.377 (2)
Se4—K7vii3.598 (2)K2—Se14ii3.4471 (9)
Se4—K43.853 (2)K2—Se14xvi3.4471 (9)
Se5—K5ii3.414 (2)K2—Se17iv3.5862 (10)
Se5—K3vi3.560 (2)K2—Se17xv3.5862 (10)
Se6—Se92.6269 (11)K3—Se19iii2.862 (7)
Se6—K6viii3.206 (2)K3—Se1v3.411 (2)
Se6—K53.265 (2)K3—Se12vi3.537 (2)
Se6—K73.389 (2)K3—Se18iii3.550 (3)
Se7—Se7vi2.3903 (16)K3—Se5vi3.560 (2)
Se7—K13.2512 (8)K3—Se7vi3.571 (2)
Se7—K33.421 (2)K3—Se12iii3.716 (2)
Se7—K3vi3.571 (2)K3—Se2iii3.756 (2)
Se8—Se102.3624 (11)K3—Se3vi3.798 (2)
Se8—Nb2i2.8803 (11)K4—Se10xiii3.308 (2)
Se8—K2ix3.377 (2)K4—Se14iv3.394 (2)
Se9—K73.467 (2)K4—Se17xiii3.814 (2)
Se9—K53.809 (2)K4—Se17iv3.934 (2)
Se10—K2vii3.294 (2)K5—Se1viii3.319 (2)
Se10—K4vii3.308 (2)K5—Se3x3.402 (2)
Se11—K63.424 (2)K5—Se5viii3.414 (2)
Se11—K73.450 (2)K5—Se12x3.434 (2)
Se11—K43.507 (2)K5—Se2x3.592 (2)
Se11—K7ii3.549 (2)K5—Se13x3.742 (2)
Se11—K5ii3.827 (2)K5—Se11viii3.827 (2)
Se12—K1vii3.3309 (8)K6—Se4xiii3.098 (2)
Se12—K5iv3.434 (2)K6—Se17iv3.110 (2)
Se12—K3vi3.537 (2)K6—Se16ii3.191 (2)
Se12—K3v3.716 (2)K6—Se6ii3.206 (2)
Se13—Se162.3912 (12)K6—Se13xiii3.213 (2)
Se13—K6vii3.213 (2)K6—Se14ii3.442 (2)
Se13—K43.539 (2)K7—Se16xiii3.307 (2)
Se13—K5iv3.742 (2)K7—Se3viii3.422 (2)
Se14—Se152.6386 (8)K7—Se17xiii3.456 (2)
Se14—K4x3.394 (2)K7—Se11viii3.549 (2)
Se14—K6viii3.442 (2)K7—Se4xiii3.598 (2)
Se14—K2xi3.4470 (9)
Se18—Nb1—Se2021.78 (18)Nb1—Se20—K5104.4 (2)
Se18—Nb1—Se12106.52 (5)Se18—Se20—K1v73.3 (4)
Se20—Nb1—Se12125.86 (18)Se19—Se20—K1v76.7 (3)
Se18—Nb1—Se1104.71 (4)Nb1—Se20—K1v141.7 (3)
Se20—Nb1—Se188.44 (18)K5—Se20—K1v95.10 (18)
Se12—Nb1—Se1144.27 (4)Se18ii—K1—Se18iii180.00 (4)
Se18—Nb1—Se2101.08 (4)Se18ii—K1—Se786.13 (3)
Se20—Nb1—Se2103.49 (17)Se18iii—K1—Se793.87 (3)
Se12—Nb1—Se254.51 (3)Se18ii—K1—Se7xii93.88 (3)
Se1—Nb1—Se2134.00 (4)Se18iii—K1—Se7xii86.12 (3)
Se18—Nb1—Se7101.86 (4)Se7—K1—Se7xii180.0
Se20—Nb1—Se7111.64 (17)Se18ii—K1—Se20ii16.46 (14)
Se12—Nb1—Se782.86 (3)Se18iii—K1—Se20ii163.54 (14)
Se1—Nb1—Se774.10 (3)Se7—K1—Se20ii72.14 (14)
Se2—Nb1—Se7135.83 (4)Se7xii—K1—Se20ii107.87 (14)
Se18—Nb1—Se1932.47 (15)Se18ii—K1—Se20iii163.54 (14)
Se20—Nb1—Se1954.2 (2)Se18iii—K1—Se20iii16.46 (14)
Se12—Nb1—Se1977.60 (15)Se7—K1—Se20iii107.86 (14)
Se1—Nb1—Se19125.32 (15)Se7xii—K1—Se20iii72.13 (14)
Se2—Nb1—Se1996.12 (15)Se20ii—K1—Se20iii180.0 (3)
Se7—Nb1—Se1983.99 (15)Se18ii—K1—Se12vi99.80 (2)
Se18—Nb1—Se999.44 (4)Se18iii—K1—Se12vi80.20 (2)
Se20—Nb1—Se978.59 (19)Se7—K1—Se12vi59.97 (2)
Se12—Nb1—Se9130.77 (4)Se7xii—K1—Se12vi120.03 (2)
Se1—Nb1—Se958.62 (3)Se20ii—K1—Se12vi99.32 (13)
Se2—Nb1—Se980.14 (3)Se20iii—K1—Se12vi80.68 (13)
Se7—Nb1—Se9131.63 (4)Se18ii—K1—Se12xiii80.20 (2)
Se19—Nb1—Se9130.66 (14)Se18iii—K1—Se12xiii99.80 (2)
Se18—Nb1—Se5170.25 (5)Se7—K1—Se12xiii120.03 (2)
Se20—Nb1—Se5148.76 (19)Se7xii—K1—Se12xiii59.97 (2)
Se12—Nb1—Se583.12 (3)Se20ii—K1—Se12xiii80.68 (13)
Se1—Nb1—Se566.59 (3)Se20iii—K1—Se12xiii99.32 (13)
Se2—Nb1—Se583.22 (3)Se12vi—K1—Se12xiii180.00 (3)
Se7—Nb1—Se580.42 (3)Se18ii—K1—Se186.30 (3)
Se19—Nb1—Se5156.52 (14)Se18iii—K1—Se193.70 (3)
Se9—Nb1—Se572.51 (3)Se7—K1—Se156.12 (2)
Se17—Nb2—Se14103.13 (4)Se7xii—K1—Se1123.88 (2)
Se17—Nb2—Se4101.69 (4)Se20ii—K1—Se171.47 (14)
Se14—Nb2—Se487.24 (3)Se20iii—K1—Se1108.53 (14)
Se17—Nb2—Se8101.59 (4)Se12vi—K1—Se1115.124 (19)
Se14—Nb2—Se8134.66 (4)Se12xiii—K1—Se164.876 (19)
Se4—Nb2—Se8123.75 (4)Se18ii—K1—Se1xii93.70 (3)
Se17—Nb2—Se10103.67 (4)Se18iii—K1—Se1xii86.30 (3)
Se14—Nb2—Se10148.39 (4)Se7—K1—Se1xii123.88 (2)
Se4—Nb2—Se1071.16 (3)Se7xii—K1—Se1xii56.12 (2)
Se8—Nb2—Se1053.82 (3)Se20ii—K1—Se1xii108.53 (14)
Se17—Nb2—Se1599.91 (4)Se20iii—K1—Se1xii71.47 (14)
Se14—Nb2—Se1560.10 (3)Se12vi—K1—Se1xii64.876 (19)
Se4—Nb2—Se15144.19 (4)Se12xiii—K1—Se1xii115.124 (19)
Se8—Nb2—Se1578.63 (3)Se1—K1—Se1xii179.999 (15)
Se10—Nb2—Se15129.97 (4)Se18ii—K1—Se19ii23.15 (11)
Se17—Nb2—Se8i170.54 (4)Se18iii—K1—Se19ii156.85 (11)
Se14—Nb2—Se8i67.69 (3)Se7—K1—Se19ii105.21 (11)
Se4—Nb2—Se8i80.62 (3)Se7xii—K1—Se19ii74.79 (11)
Se8—Nb2—Se8i84.35 (3)Se20ii—K1—Se19ii39.59 (18)
Se10—Nb2—Se8i85.76 (3)Se20iii—K1—Se19ii140.41 (18)
Se15—Nb2—Se8i73.86 (3)Se12vi—K1—Se19ii97.91 (11)
Se11—Nb3—Se6104.08 (4)Se12xiii—K1—Se19ii82.09 (11)
Se11—Nb3—Se5100.27 (4)Se1—K1—Se19ii107.71 (11)
Se6—Nb3—Se5134.41 (4)Se1xii—K1—Se19ii72.29 (11)
Se11—Nb3—Se13101.72 (4)Se18ii—K1—Se19iii156.85 (11)
Se6—Nb3—Se1384.42 (3)Se18iii—K1—Se19iii23.15 (11)
Se5—Nb3—Se13127.25 (4)Se7—K1—Se19iii74.79 (11)
Se11—Nb3—Se3103.09 (4)Se7xii—K1—Se19iii105.21 (11)
Se6—Nb3—Se3148.14 (4)Se20ii—K1—Se19iii140.41 (18)
Se5—Nb3—Se354.48 (3)Se20iii—K1—Se19iii39.59 (18)
Se13—Nb3—Se374.02 (3)Se12vi—K1—Se19iii82.09 (11)
Se11—Nb3—Se999.50 (4)Se12xiii—K1—Se19iii97.91 (11)
Se6—Nb3—Se960.10 (3)Se1—K1—Se19iii72.29 (11)
Se5—Nb3—Se978.35 (3)Se1xii—K1—Se19iii107.71 (11)
Se13—Nb3—Se9142.16 (4)Se19ii—K1—Se19iii180.0 (3)
Se3—Nb3—Se9130.31 (4)Se10xiv—K2—Se10xiii73.64 (6)
Se11—Nb3—Se2172.22 (4)Se10xiv—K2—Se8iv145.93 (2)
Se6—Nb3—Se268.88 (3)Se10xiii—K2—Se8iv108.05 (2)
Se5—Nb3—Se283.26 (3)Se10xiv—K2—Se8xv108.05 (2)
Se13—Nb3—Se281.25 (3)Se10xiii—K2—Se8xv145.93 (2)
Se3—Nb3—Se284.62 (3)Se8iv—K2—Se8xv89.38 (7)
Se9—Nb3—Se274.30 (3)Se10xiv—K2—Se14ii85.44 (4)
Se9—Se1—Nb162.42 (3)Se10xiii—K2—Se14ii94.04 (4)
Se9—Se1—K5ii92.30 (5)Se8iv—K2—Se14ii127.47 (6)
Nb1—Se1—K5ii125.82 (5)Se8xv—K2—Se14ii53.12 (2)
Se9—Se1—K1173.81 (4)Se10xiv—K2—Se14xvi94.04 (4)
Nb1—Se1—K1111.58 (3)Se10xiii—K2—Se14xvi85.44 (4)
K5ii—Se1—K192.73 (5)Se8iv—K2—Se14xvi53.12 (2)
Se9—Se1—K3iii100.27 (5)Se8xv—K2—Se14xvi127.47 (6)
Nb1—Se1—K3iii116.85 (5)Se14ii—K2—Se14xvi179.35 (9)
K5ii—Se1—K3iii114.28 (6)Se10xiv—K2—Se17iv133.98 (7)
K1—Se1—K3iii80.92 (4)Se10xiii—K2—Se17iv62.69 (3)
Se12—Se2—Nb162.04 (3)Se8iv—K2—Se17iv66.83 (3)
Se12—Se2—Nb3112.83 (4)Se8xv—K2—Se17iv100.61 (5)
Nb1—Se2—Nb384.29 (3)Se14ii—K2—Se17iv83.87 (2)
Se12—Se2—K5iv66.71 (5)Se14xvi—K2—Se17iv96.22 (2)
Nb1—Se2—K5iv122.38 (5)Se10xiv—K2—Se17xv62.69 (3)
Nb3—Se2—K5iv92.81 (4)Se10xiii—K2—Se17xv133.98 (7)
Se12—Se2—K3v70.57 (4)Se8iv—K2—Se17xv100.61 (5)
Nb1—Se2—K3v86.05 (4)Se8xv—K2—Se17xv66.83 (3)
Nb3—Se2—K3v166.30 (5)Se14ii—K2—Se17xv96.22 (2)
K5iv—Se2—K3v100.57 (5)Se14xvi—K2—Se17xv83.87 (2)
Se5—Se3—Nb361.86 (3)Se17iv—K2—Se17xv163.07 (9)
Se5—Se3—K5iv120.19 (5)Se19iii—K3—Se1996.83 (10)
Nb3—Se3—K5iv103.49 (5)Se19iii—K3—Se1v116.36 (15)
Se5—Se3—K7ii104.03 (4)Se19—K3—Se1v78.74 (13)
Nb3—Se3—K7ii92.79 (4)Se19iii—K3—Se782.39 (15)
K5iv—Se3—K7ii135.55 (5)Se19—K3—Se765.01 (13)
Se5—Se3—K3vi65.76 (4)Se1v—K3—Se7141.30 (8)
Nb3—Se3—K3vi122.30 (5)Se19iii—K3—Se12vi89.87 (14)
K5iv—Se3—K3vi82.84 (6)Se19—K3—Se12vi119.45 (14)
K7ii—Se3—K3vi122.39 (5)Se1v—K3—Se12vi147.20 (7)
Se16—Se4—Nb2114.43 (4)Se7—K3—Se12vi56.42 (4)
Se16—Se4—K6vii101.81 (5)Se19iii—K3—Se18iii22.38 (13)
Nb2—Se4—K6vii143.58 (5)Se19—K3—Se18iii117.33 (14)
Se16—Se4—K7vii63.34 (4)Se1v—K3—Se18iii126.15 (7)
Nb2—Se4—K7vii89.56 (4)Se7—K3—Se18iii84.45 (5)
K6vii—Se4—K7vii104.08 (5)Se12vi—K3—Se18iii72.37 (5)
Se16—Se4—K459.89 (4)Se19iii—K3—Se5vi146.12 (15)
Nb2—Se4—K4119.00 (5)Se19—K3—Se5vi113.00 (14)
K6vii—Se4—K481.80 (5)Se1v—K3—Se5vi86.13 (5)
K7vii—Se4—K4122.85 (5)Se7—K3—Se5vi95.53 (6)
Se3—Se5—Nb363.66 (3)Se12vi—K3—Se5vi62.08 (4)
Se3—Se5—Nb1115.59 (4)Se18iii—K3—Se5vi123.81 (7)
Nb3—Se5—Nb185.09 (3)Se19iii—K3—Se7vi121.99 (15)
Se3—Se5—K5ii125.66 (5)Se19—K3—Se7vi68.37 (13)
Nb3—Se5—K5ii97.09 (5)Se1v—K3—Se7vi114.81 (7)
Nb1—Se5—K5ii112.19 (4)Se7—K3—Se7vi39.91 (3)
Se3—Se5—K3vi76.62 (5)Se12vi—K3—Se7vi57.78 (4)
Nb3—Se5—K3vi133.36 (5)Se18iii—K3—Se7vi118.88 (6)
Nb1—Se5—K3vi91.29 (4)Se5vi—K3—Se7vi60.40 (4)
K5ii—Se5—K3vi126.70 (6)Se19iii—K3—Se1874.76 (14)
Nb3—Se6—Se961.97 (3)Se19—K3—Se1822.36 (13)
Nb3—Se6—K6viii137.12 (5)Se1v—K3—Se1885.64 (5)
Se9—Se6—K6viii144.67 (5)Se7—K3—Se1866.11 (5)
Nb3—Se6—K5132.71 (5)Se12vi—K3—Se18121.97 (6)
Se9—Se6—K579.76 (5)Se18iii—K3—Se1896.01 (6)
K6viii—Se6—K590.16 (6)Se5vi—K3—Se18135.14 (7)
Nb3—Se6—K788.04 (4)Se7vi—K3—Se1883.78 (5)
Se9—Se6—K769.05 (4)Se19iii—K3—Se12iii57.62 (14)
K6viii—Se6—K780.98 (5)Se19—K3—Se12iii99.82 (13)
K5—Se6—K7103.95 (5)Se1v—K3—Se12iii60.81 (4)
Se7vi—Se7—Nb1108.89 (5)Se7—K3—Se12iii136.05 (7)
Se7vi—Se7—K1133.45 (5)Se12vi—K3—Se12iii132.33 (7)
Nb1—Se7—K1115.82 (3)Se18iii—K3—Se12iii65.73 (5)
Se7vi—Se7—K373.44 (5)Se5vi—K3—Se12iii127.57 (6)
Nb1—Se7—K396.20 (5)Se7vi—K3—Se12iii168.18 (8)
K1—Se7—K389.16 (4)Se18—K3—Se12iii84.90 (5)
Se7vi—Se7—K3vi66.65 (5)Se19iii—K3—Se2iii70.54 (15)
Nb1—Se7—K3vi96.50 (5)Se19—K3—Se2iii135.65 (14)
K1—Se7—K3vi118.31 (4)Se1v—K3—Se2iii70.62 (4)
K3—Se7—K3vi140.09 (3)Se7—K3—Se2iii146.67 (7)
Se10—Se8—Nb263.63 (3)Se12vi—K3—Se2iii103.29 (6)
Se10—Se8—Nb2i114.96 (4)Se18iii—K3—Se2iii63.12 (4)
Nb2—Se8—Nb2i84.66 (3)Se5vi—K3—Se2iii96.39 (6)
Se10—Se8—K2ix121.67 (4)Se7vi—K3—Se2iii154.41 (7)
Nb2—Se8—K2ix91.88 (3)Se18—K3—Se2iii121.81 (6)
Nb2i—Se8—K2ix114.02 (4)Se12iii—K3—Se2iii37.02 (3)
Se1—Se9—Se6164.62 (4)Se19iii—K3—Se3vi115.20 (15)
Se1—Se9—Nb3109.43 (4)Se19—K3—Se3vi147.93 (14)
Se6—Se9—Nb357.93 (3)Se1v—K3—Se3vi85.20 (5)
Se1—Se9—Nb158.97 (3)Se7—K3—Se3vi118.68 (6)
Se6—Se9—Nb1109.32 (4)Se12vi—K3—Se3vi65.00 (4)
Nb3—Se9—Nb188.48 (3)Se18iii—K3—Se3vi94.57 (6)
Se1—Se9—K7124.68 (5)Se5vi—K3—Se3vi37.62 (3)
Se6—Se9—K765.92 (4)Se7vi—K3—Se3vi94.28 (5)
Nb3—Se9—K784.78 (4)Se18—K3—Se3vi168.82 (7)
Nb1—Se9—K7173.15 (5)Se12iii—K3—Se3vi96.18 (5)
Se1—Se9—K5127.57 (5)Se2iii—K3—Se3vi60.57 (4)
Se6—Se9—K557.51 (4)Se10xiii—K4—Se16148.87 (8)
Nb3—Se9—K5109.98 (4)Se10xiii—K4—Se14iv97.21 (6)
Nb1—Se9—K589.11 (4)Se16—K4—Se14iv107.54 (6)
K7—Se9—K592.06 (5)Se10xiii—K4—Se1193.48 (6)
Se8—Se10—Nb262.55 (3)Se16—K4—Se1192.15 (5)
Se8—Se10—K2vii108.09 (4)Se14iv—K4—Se11116.38 (7)
Nb2—Se10—K2vii131.43 (4)Se10xiii—K4—Se13160.15 (8)
Se8—Se10—K4vii106.38 (5)Se16—K4—Se1340.43 (3)
Nb2—Se10—K4vii98.28 (5)Se14iv—K4—Se1390.66 (5)
K2vii—Se10—K4vii128.50 (5)Se11—K4—Se1366.74 (4)
Nb3—Se11—K6164.87 (5)Se10xiii—K4—Se17xiii66.24 (4)
Nb3—Se11—K789.85 (4)Se16—K4—Se17xiii83.51 (5)
K6—Se11—K7100.58 (5)Se14iv—K4—Se17xiii152.79 (7)
Nb3—Se11—K495.38 (5)Se11—K4—Se17xiii87.18 (5)
K6—Se11—K495.34 (5)Se13—K4—Se17xiii112.24 (6)
K7—Se11—K491.14 (5)Se10xiii—K4—Se4144.07 (7)
Nb3—Se11—K7ii94.27 (4)Se16—K4—Se437.88 (3)
K6—Se11—K7ii75.81 (5)Se14iv—K4—Se473.27 (4)
K7—Se11—K7ii175.32 (7)Se11—K4—Se4122.02 (6)
K4—Se11—K7ii86.27 (5)Se13—K4—Se455.75 (3)
Nb3—Se11—K5ii90.70 (4)Se17xiii—K4—Se4106.85 (6)
K6—Se11—K5ii78.17 (5)Se10xiii—K4—Se17iv58.64 (4)
K7—Se11—K5ii91.66 (5)Se16—K4—Se17iv150.61 (7)
K4—Se11—K5ii173.31 (5)Se14iv—K4—Se17iv63.19 (4)
K7ii—Se11—K5ii90.51 (5)Se11—K4—Se17iv70.58 (4)
Se2—Se12—Nb163.45 (3)Se13—K4—Se17iv110.20 (6)
Se2—Se12—K1vii142.13 (4)Se17xiii—K4—Se17iv117.89 (5)
Nb1—Se12—K1vii138.01 (3)Se4—K4—Se17iv134.43 (6)
Se2—Se12—K5iv73.91 (5)Se6—K5—Se2093.30 (13)
Nb1—Se12—K5iv129.77 (5)Se6—K5—Se1viii148.73 (7)
K1vii—Se12—K5iv92.10 (4)Se20—K5—Se1viii72.64 (13)
Se2—Se12—K3vi126.73 (5)Se6—K5—Se3x76.77 (5)
Nb1—Se12—K3vi98.17 (5)Se20—K5—Se3x109.55 (16)
K1vii—Se12—K3vi85.97 (4)Se1viii—K5—Se3x133.96 (6)
K5iv—Se12—K3vi86.41 (6)Se6—K5—Se5viii95.07 (5)
Se2—Se12—K3v72.42 (5)Se20—K5—Se5viii63.47 (15)
Nb1—Se12—K3v87.36 (4)Se1viii—K5—Se5viii53.69 (4)
K1vii—Se12—K3v77.62 (4)Se3x—K5—Se5viii169.28 (8)
K5iv—Se12—K3v104.44 (5)Se6—K5—Se12x141.37 (7)
K3vi—Se12—K3v160.52 (7)Se20—K5—Se12x79.18 (14)
Se16—Se13—Nb3107.99 (4)Se1viii—K5—Se12x64.73 (4)
Se16—Se13—K6vii98.54 (5)Se3x—K5—Se12x70.53 (4)
Nb3—Se13—K6vii148.61 (5)Se5viii—K5—Se12x114.21 (6)
Se16—Se13—K465.85 (5)Se6—K5—Se2x136.37 (7)
Nb3—Se13—K490.27 (4)Se20—K5—Se2x118.03 (14)
K6vii—Se13—K485.44 (5)Se1viii—K5—Se2x73.72 (4)
Se16—Se13—K5iv126.09 (5)Se3x—K5—Se2x64.92 (4)
Nb3—Se13—K5iv95.12 (4)Se5viii—K5—Se2x125.12 (6)
K6vii—Se13—K5iv82.04 (5)Se12x—K5—Se2x39.38 (3)
K4—Se13—K5iv163.86 (5)Se6—K5—Se13x81.17 (5)
Nb2—Se14—Se1561.91 (3)Se20—K5—Se13x161.64 (16)
Nb2—Se14—K4x100.30 (5)Se1viii—K5—Se13x120.16 (7)
Se15—Se14—K4x85.32 (5)Se3x—K5—Se13x52.19 (3)
Nb2—Se14—K6viii136.67 (5)Se5viii—K5—Se13x134.18 (7)
Se15—Se14—K6viii160.28 (5)Se12x—K5—Se13x94.19 (5)
K4x—Se14—K6viii84.28 (5)Se2x—K5—Se13x59.36 (4)
Nb2—Se14—K2xi120.66 (5)Se6—K5—Se1894.26 (6)
Se15—Se14—K2xi85.76 (2)Se20—K5—Se1812.92 (14)
K4x—Se14—K2xi126.73 (6)Se1viii—K5—Se1878.19 (5)
K6viii—Se14—K2xi87.11 (4)Se3x—K5—Se1897.19 (6)
Se4—Se16—Se1393.03 (4)Se5viii—K5—Se1876.26 (5)
Se4—Se16—K6viii130.05 (5)Se12x—K5—Se1870.57 (5)
Se13—Se16—K6viii132.92 (5)Se2x—K5—Se18109.95 (6)
Se4—Se16—K7vii76.48 (5)Se13x—K5—Se18149.34 (6)
Se13—Se16—K7vii100.45 (5)Se6—K5—Se942.73 (3)
K6viii—Se16—K7vii106.78 (5)Se20—K5—Se954.64 (13)
Se4—Se16—K482.23 (5)Se1viii—K5—Se9110.42 (6)
Se13—Se16—K473.71 (5)Se3x—K5—Se9106.35 (6)
K6viii—Se16—K492.08 (5)Se5viii—K5—Se963.10 (4)
K7vii—Se16—K4157.64 (6)Se12x—K5—Se9130.52 (7)
Se14—Se15—Se14i163.65 (6)Se2x—K5—Se9167.35 (7)
Se14—Se15—Nb257.99 (3)Se13x—K5—Se9123.66 (6)
Se14i—Se15—Nb2108.89 (4)Se18—K5—Se960.69 (4)
Se14—Se15—Nb2i108.89 (4)Se6—K5—Se11viii71.73 (4)
Se14i—Se15—Nb2i57.99 (3)Se20—K5—Se11viii122.41 (15)
Nb2—Se15—Nb2i86.93 (4)Se1viii—K5—Se11viii92.03 (5)
Nb2—Se17—K6x175.88 (6)Se3x—K5—Se11viii119.47 (6)
Nb2—Se17—K7vii97.21 (5)Se5viii—K5—Se11viii63.08 (4)
K6x—Se17—K7vii81.30 (5)Se12x—K5—Se11viii143.36 (7)
Nb2—Se17—K2ix91.12 (4)Se2x—K5—Se11viii109.19 (6)
K6x—Se17—K2ix90.00 (4)Se13x—K5—Se11viii72.61 (5)
K7vii—Se17—K2ix169.89 (4)Se18—K5—Se11viii134.82 (6)
Nb2—Se17—K4vii90.76 (4)Se9—K5—Se11viii82.91 (4)
K6x—Se17—K4vii85.32 (5)Se4xiii—K6—Se17iv99.42 (6)
K7vii—Se17—K4vii86.09 (5)Se4xiii—K6—Se16ii143.74 (7)
K2ix—Se17—K4vii88.10 (5)Se17iv—K6—Se16ii99.03 (6)
Nb2—Se17—K4x90.94 (4)Se4xiii—K6—Se6ii146.23 (7)
K6x—Se17—K4x92.61 (5)Se17iv—K6—Se6ii97.19 (6)
K7vii—Se17—K4x81.24 (5)Se16ii—K6—Se6ii60.22 (4)
K2ix—Se17—K4x104.42 (5)Se4xiii—K6—Se13xiii66.62 (4)
K4vii—Se17—K4x167.33 (7)Se17iv—K6—Se13xiii163.27 (7)
Se20—Se18—Se19173.6 (5)Se16ii—K6—Se13xiii97.70 (6)
Se20—Se18—Nb189.5 (4)Se6ii—K6—Se13xiii90.87 (5)
Se19—Se18—Nb184.6 (3)Se4xiii—K6—Se1175.21 (5)
Se20—Se18—K1v90.2 (4)Se17iv—K6—Se1182.47 (5)
Se19—Se18—K1v95.4 (3)Se16ii—K6—Se11138.23 (7)
Nb1—Se18—K1v175.71 (5)Se6ii—K6—Se1178.10 (5)
Se20—Se18—K3v133.1 (5)Se13xiii—K6—Se1184.90 (5)
Se19—Se18—K3v50.3 (3)Se4xiii—K6—Se14ii82.98 (5)
Nb1—Se18—K3v94.94 (5)Se17iv—K6—Se14ii91.58 (5)
K1v—Se18—K3v88.33 (4)Se16ii—K6—Se14ii65.56 (4)
Se20—Se18—K3122.3 (5)Se6ii—K6—Se14ii125.78 (6)
Se19—Se18—K356.0 (3)Se13xiii—K6—Se14ii95.57 (5)
Nb1—Se18—K395.69 (5)Se11—K6—Se14ii156.04 (6)
K1v—Se18—K380.81 (4)Se16xiii—K7—Se6162.28 (7)
K3v—Se18—K3103.66 (6)Se16xiii—K7—Se3viii86.49 (5)
Se20—Se18—K552.1 (5)Se6—K7—Se3viii103.50 (5)
Se19—Se18—K5130.9 (3)Se16xiii—K7—Se1192.86 (5)
Nb1—Se18—K594.78 (5)Se6—K7—Se1169.44 (4)
K1v—Se18—K588.46 (4)Se3viii—K7—Se11128.37 (6)
K3v—Se18—K581.03 (5)Se16xiii—K7—Se17xiii94.88 (5)
K3—Se18—K5168.09 (6)Se6—K7—Se17xiii87.60 (5)
Se18—Se19—Se202.6 (2)Se3viii—K7—Se17xiii137.50 (6)
Se18—Se19—Nb162.9 (2)Se11—K7—Se17xiii94.05 (5)
Se20—Se19—Nb160.6 (2)Se16xiii—K7—Se9128.22 (6)
Se18—Se19—K3v107.3 (3)Se6—K7—Se945.04 (3)
Se20—Se19—K3v108.7 (3)Se3viii—K7—Se972.62 (4)
Nb1—Se19—K3v107.3 (2)Se11—K7—Se967.76 (4)
Se18—Se19—K3101.7 (3)Se17xiii—K7—Se9132.32 (6)
Se20—Se19—K3101.1 (3)Se16xiii—K7—Se11viii123.57 (6)
Nb1—Se19—K3104.6 (2)Se6—K7—Se11viii74.06 (4)
K3v—Se19—K3144.0 (3)Se3viii—K7—Se11viii68.31 (4)
Se18—Se19—K1v61.4 (2)Se11—K7—Se11viii142.53 (6)
Se20—Se19—K1v63.7 (2)Se17xiii—K7—Se11viii76.00 (4)
Nb1—Se19—K1v124.2 (2)Se9—K7—Se11viii92.21 (5)
K3v—Se19—K1v92.54 (17)Se16xiii—K7—Se4xiii40.19 (3)
K3—Se19—K1v82.83 (16)Se6—K7—Se4xiii127.93 (6)
Se18—Se20—Se193.9 (3)Se3viii—K7—Se4xiii126.67 (6)
Se18—Se20—Nb168.7 (4)Se11—K7—Se4xiii68.88 (4)
Se19—Se20—Nb165.2 (3)Se17xiii—K7—Se4xiii65.86 (4)
Se18—Se20—K5115.0 (5)Se9—K7—Se4xiii133.70 (6)
Se19—Se20—K5116.9 (3)Se11viii—K7—Se4xiii133.05 (6)
Symmetry codes: (i) x1, y, z+1/2; (ii) x+1/2, y1/2, z; (iii) x+1/2, y+1/2, z; (iv) x1/2, y1/2, z; (v) x1/2, y+1/2, z; (vi) x, y, z; (vii) x1, y, z; (viii) x+1/2, y+1/2, z; (ix) x3/2, y+1/2, z+1/2; (x) x1/2, y+1/2, z; (xi) x1/2, y+1/2, z+1/2; (xii) x+1, y, z; (xiii) x+1, y, z; (xiv) x, y, z+1/2; (xv) x+3/2, y1/2, z+1/2; (xvi) x+1/2, y1/2, z+1/2.
 

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