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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
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
Cs6Nb4Se22 | F(000) = 2484 |
Mr = 2906.22 | Dx = 4.566 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.5887 (6) Å | Cell parameters from 5633 reflections |
b = 8.5127 (4) Å | θ = 4.7–52.1° |
c = 20.3151 (10) Å | µ = 25.10 mm−1 |
β = 103.853 (1)° | T = 296 K |
V = 2113.72 (18) Å3 | Needle, black |
Z = 2 | 0.2 × 0.08 × 0.06 mm |
Data collection top
Bruker APEXII CCD diffractometer | 4844 independent reflections |
Radiation source: fine-focus sealed tube | 3550 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.065 |
ω and φ scans | θmax = 27.5°, θmin = 1.7° |
Absorption correction: empirical (using intensity measurements) (SADABS; Bruker, 2008) | h = −16→16 |
Tmin = 0.347, Tmax = 0.746 | k = −11→10 |
35929 measured reflections | l = −26→26 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.038 | Secondary 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 reflections | Δρmax = 4.93 e Å−3 |
145 parameters | Δρmin = −2.29 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Nb1 | 0.80152 (6) | 0.23308 (9) | 0.50654 (4) | 0.02341 (17) | |
Nb2 | 0.70707 (7) | 0.35623 (10) | 0.66030 (4) | 0.03012 (19) | |
Se1 | 1.00252 (7) | 0.13484 (10) | 0.51394 (5) | 0.0294 (2) | |
Se2 | 0.89435 (7) | 0.23574 (11) | 0.65594 (4) | 0.0299 (2) | |
Se3 | 0.73578 (7) | 0.50305 (10) | 0.54883 (5) | 0.0303 (2) | |
Se4 | 0.75335 (8) | −0.05493 (11) | 0.52764 (5) | 0.0371 (2) | |
Se5 | 0.79063 (8) | 0.10354 (12) | 0.72163 (5) | 0.0388 (2) | |
Se6 | 0.51018 (8) | 0.43174 (14) | 0.59217 (6) | 0.0465 (3) | |
Se7 | 0.74133 (9) | 0.26233 (15) | 0.38919 (5) | 0.0486 (3) | |
Se8 | 0.62574 (7) | 0.14011 (11) | 0.54042 (4) | 0.0308 (2) | |
Se9 | 0.92141 (7) | 0.48537 (10) | 0.54525 (5) | 0.0316 (2) | |
Se10 | 0.52464 (10) | 0.27314 (17) | 0.68849 (6) | 0.0615 (3) | |
Se11 | 0.76529 (11) | 0.56779 (15) | 0.73383 (6) | 0.0614 (4) | |
Cs1 | 1.00418 (6) | 0.17210 (8) | 0.33806 (3) | 0.04514 (17) | |
Cs2 | 0.54136 (7) | −0.15562 (9) | 0.64033 (4) | 0.0602 (2) | |
Cs3 | 1.22961 (6) | 0.31969 (9) | 0.62045 (3) | 0.0537 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nb1 | 0.0223 (4) | 0.0250 (4) | 0.0232 (4) | −0.0013 (3) | 0.0058 (3) | −0.0011 (3) |
Nb2 | 0.0288 (4) | 0.0372 (5) | 0.0244 (4) | 0.0052 (4) | 0.0065 (3) | −0.0027 (3) |
Se1 | 0.0241 (4) | 0.0249 (4) | 0.0399 (5) | −0.0008 (4) | 0.0091 (4) | −0.0057 (4) |
Se2 | 0.0266 (5) | 0.0329 (5) | 0.0283 (4) | 0.0025 (4) | 0.0030 (4) | −0.0020 (4) |
Se3 | 0.0296 (5) | 0.0281 (5) | 0.0333 (5) | 0.0059 (4) | 0.0077 (4) | 0.0017 (4) |
Se4 | 0.0404 (6) | 0.0267 (5) | 0.0456 (6) | −0.0062 (4) | 0.0130 (4) | −0.0052 (4) |
Se5 | 0.0426 (6) | 0.0425 (6) | 0.0307 (5) | 0.0006 (5) | 0.0074 (4) | 0.0066 (4) |
Se6 | 0.0284 (5) | 0.0624 (7) | 0.0478 (6) | 0.0093 (5) | 0.0072 (4) | −0.0012 (5) |
Se7 | 0.0434 (6) | 0.0696 (8) | 0.0328 (5) | −0.0024 (5) | 0.0095 (5) | 0.0011 (5) |
Se8 | 0.0253 (5) | 0.0384 (5) | 0.0289 (5) | −0.0066 (4) | 0.0070 (4) | −0.0013 (4) |
Se9 | 0.0297 (5) | 0.0262 (4) | 0.0395 (5) | −0.0042 (4) | 0.0094 (4) | −0.0019 (4) |
Se10 | 0.0458 (7) | 0.0906 (10) | 0.0580 (7) | 0.0078 (7) | 0.0321 (6) | 0.0115 (7) |
Se11 | 0.0697 (8) | 0.0578 (7) | 0.0471 (7) | 0.0178 (6) | −0.0050 (6) | −0.0236 (6) |
Cs1 | 0.0521 (4) | 0.0457 (4) | 0.0337 (3) | 0.0115 (3) | 0.0025 (3) | −0.0012 (3) |
Cs2 | 0.0660 (5) | 0.0573 (5) | 0.0511 (4) | −0.0158 (4) | 0.0019 (4) | 0.0129 (3) |
Cs3 | 0.0447 (4) | 0.0707 (5) | 0.0399 (4) | −0.0153 (4) | −0.0013 (3) | 0.0100 (3) |
Geometric parameters (Å, º) top
Nb1—Se7 | 2.3355 (13) | Se7—Cs1 | 3.7768 (13) |
Nb1—Se4 | 2.5859 (12) | Se8—Cs2 | 3.5522 (11) |
Nb1—Se8 | 2.5934 (12) | Se8—Cs2vii | 3.7719 (11) |
Nb1—Se9 | 2.6344 (11) | Se9—Cs1iii | 3.7331 (11) |
Nb1—Se1 | 2.6348 (12) | Se9—Cs3iii | 3.8255 (12) |
Nb1—Se3 | 2.6543 (11) | Se9—Cs3 | 4.0667 (12) |
Nb1—Se2 | 2.9799 (11) | Se10—Cs3vi | 3.6610 (15) |
Nb2—Se11 | 2.3425 (14) | Se10—Cs2 | 3.7976 (17) |
Nb2—Se5 | 2.5804 (13) | Se10—Cs2viii | 3.8124 (14) |
Nb2—Se2 | 2.5919 (12) | Se11—Cs3ix | 3.6436 (13) |
Nb2—Se10 | 2.5948 (14) | Se11—Cs2v | 3.8123 (15) |
Nb2—Se6 | 2.6134 (13) | Se11—Cs1ii | 3.8274 (14) |
Nb2—Se3 | 2.6856 (12) | Se11—Cs1iii | 4.1818 (17) |
Nb2—Se8 | 3.0283 (12) | Cs1—Se5x | 3.6640 (12) |
Se1—Se1i | 2.3616 (17) | Cs1—Se2i | 3.6913 (11) |
Se1—Cs3 | 3.5170 (11) | Cs1—Se2x | 3.7102 (11) |
Se1—Cs1 | 3.5920 (11) | Cs1—Se4i | 3.7105 (12) |
Se1—Cs1i | 3.9994 (11) | Cs1—Se9iii | 3.7331 (11) |
Se2—Se5 | 2.3636 (13) | Cs1—Se11x | 3.8274 (14) |
Se2—Cs1i | 3.6913 (11) | Cs1—Se5i | 3.8922 (12) |
Se2—Cs1ii | 3.7102 (11) | Cs1—Se1i | 3.9994 (11) |
Se3—Se9 | 2.3601 (13) | Cs1—Se11iii | 4.1818 (17) |
Se3—Cs3iii | 3.8743 (11) | Cs2—Se7vii | 3.5815 (14) |
Se4—Se8 | 2.3674 (13) | Cs2—Se6xi | 3.6423 (15) |
Se4—Cs1i | 3.7105 (12) | Cs2—Se8vii | 3.7719 (11) |
Se4—Cs3i | 3.8058 (12) | Cs2—Se11xi | 3.8123 (15) |
Se4—Cs2 | 4.0030 (13) | Cs2—Se10xii | 3.8124 (14) |
Se5—Cs1ii | 3.6640 (12) | Cs3—Se7iii | 3.5870 (15) |
Se5—Cs2 | 3.8678 (13) | Cs3—Se11iv | 3.6436 (13) |
Se5—Cs1i | 3.8921 (12) | Cs3—Se10xiii | 3.6610 (15) |
Se5—Cs3iv | 4.0728 (12) | Cs3—Se4i | 3.8058 (12) |
Se6—Se10 | 2.3483 (17) | Cs3—Se9iii | 3.8255 (12) |
Se6—Cs2v | 3.6423 (14) | Cs3—Se6xiii | 3.8323 (13) |
Se6—Cs3vi | 3.8323 (13) | Cs3—Se3iii | 3.8742 (11) |
Se7—Cs2vii | 3.5815 (14) | Cs3—Se5ix | 4.0728 (12) |
Se7—Cs3iii | 3.5871 (15) | | |
| | | |
Se7—Nb1—Se4 | 103.80 (5) | Nb2—Se11—Cs1iii | 108.77 (5) |
Se7—Nb1—Se8 | 102.39 (4) | Cs3ix—Se11—Cs1iii | 95.36 (3) |
Se4—Nb1—Se8 | 54.40 (3) | Cs2v—Se11—Cs1iii | 89.50 (3) |
Se7—Nb1—Se9 | 103.91 (4) | Cs1ii—Se11—Cs1iii | 87.52 (3) |
Se4—Nb1—Se9 | 149.74 (4) | Se1—Cs1—Se5x | 120.67 (3) |
Se8—Nb1—Se9 | 129.33 (4) | Se1—Cs1—Se2i | 88.20 (2) |
Se7—Nb1—Se1 | 99.47 (4) | Se5x—Cs1—Se2i | 134.93 (3) |
Se4—Nb1—Se1 | 87.12 (4) | Se1—Cs1—Se2x | 157.07 (3) |
Se8—Nb1—Se1 | 139.18 (4) | Se5x—Cs1—Se2x | 37.38 (2) |
Se9—Nb1—Se1 | 76.59 (3) | Se2i—Cs1—Se2x | 105.97 (2) |
Se7—Nb1—Se3 | 100.84 (4) | Se1—Cs1—Se4i | 56.26 (2) |
Se4—Nb1—Se3 | 131.58 (4) | Se5x—Cs1—Se4i | 164.17 (3) |
Se8—Nb1—Se3 | 80.00 (4) | Se2i—Cs1—Se4i | 60.37 (2) |
Se9—Nb1—Se3 | 53.01 (3) | Se2x—Cs1—Se4i | 146.58 (3) |
Se1—Nb1—Se3 | 128.75 (4) | Se1—Cs1—Se9iii | 59.85 (2) |
Se7—Nb1—Se2 | 172.37 (5) | Se5x—Cs1—Se9iii | 92.09 (3) |
Se4—Nb1—Se2 | 83.61 (3) | Se2i—Cs1—Se9iii | 132.96 (3) |
Se8—Nb1—Se2 | 83.31 (3) | Se2x—Cs1—Se9iii | 116.42 (3) |
Se9—Nb1—Se2 | 68.46 (3) | Se4i—Cs1—Se9iii | 72.89 (2) |
Se1—Nb1—Se2 | 78.89 (3) | Se1—Cs1—Se7 | 61.98 (2) |
Se3—Nb1—Se2 | 74.95 (3) | Se5x—Cs1—Se7 | 61.04 (3) |
Se11—Nb2—Se5 | 107.69 (5) | Se2i—Cs1—Se7 | 120.08 (3) |
Se11—Nb2—Se2 | 100.24 (5) | Se2x—Cs1—Se7 | 95.13 (3) |
Se5—Nb2—Se2 | 54.38 (3) | Se4i—Cs1—Se7 | 118.23 (3) |
Se11—Nb2—Se10 | 103.13 (6) | Se9iii—Cs1—Se7 | 76.68 (3) |
Se5—Nb2—Se10 | 86.92 (5) | Se1—Cs1—Se11x | 108.20 (3) |
Se2—Nb2—Se10 | 139.47 (5) | Se5x—Cs1—Se11x | 64.09 (3) |
Se11—Nb2—Se6 | 105.12 (5) | Se2i—Cs1—Se11x | 74.71 (3) |
Se5—Nb2—Se6 | 133.32 (5) | Se2x—Cs1—Se11x | 60.35 (2) |
Se2—Nb2—Se6 | 146.55 (4) | Se4i—Cs1—Se11x | 131.49 (3) |
Se10—Nb2—Se6 | 53.60 (4) | Se9iii—Cs1—Se11x | 144.35 (3) |
Se11—Nb2—Se3 | 95.46 (5) | Se7—Cs1—Se11x | 68.69 (3) |
Se5—Nb2—Se3 | 132.34 (4) | Se1—Cs1—Se5i | 114.77 (3) |
Se2—Nb2—Se3 | 81.27 (4) | Se5x—Cs1—Se5i | 123.52 (2) |
Se10—Nb2—Se3 | 128.16 (5) | Se2i—Cs1—Se5i | 36.20 (2) |
Se6—Nb2—Se3 | 74.99 (4) | Se2x—Cs1—Se5i | 86.18 (2) |
Se11—Nb2—Se8 | 166.86 (5) | Se4i—Cs1—Se5i | 64.95 (2) |
Se5—Nb2—Se8 | 84.38 (4) | Se9iii—Cs1—Se5i | 125.76 (3) |
Se2—Nb2—Se8 | 82.37 (3) | Se7—Cs1—Se5i | 154.00 (3) |
Se10—Nb2—Se8 | 82.25 (4) | Se11x—Cs1—Se5i | 89.89 (3) |
Se6—Nb2—Se8 | 68.18 (4) | Se1—Cs1—Se1i | 35.74 (3) |
Se3—Nb2—Se8 | 72.09 (3) | Se5x—Cs1—Se1i | 132.97 (3) |
Se1i—Se1—Nb1 | 108.94 (5) | Se2i—Cs1—Se1i | 55.26 (2) |
Se1i—Se1—Cs3 | 123.62 (5) | Se2x—Cs1—Se1i | 144.87 (3) |
Nb1—Se1—Cs3 | 121.41 (4) | Se4i—Cs1—Se1i | 55.48 (2) |
Se1i—Se1—Cs1 | 81.58 (5) | Se9iii—Cs1—Se1i | 94.60 (2) |
Nb1—Se1—Cs1 | 98.60 (3) | Se7—Cs1—Se1i | 75.44 (2) |
Cs3—Se1—Cs1 | 112.02 (3) | Se11x—Cs1—Se1i | 84.96 (2) |
Se1i—Se1—Cs1i | 62.68 (4) | Se5i—Cs1—Se1i | 88.59 (2) |
Nb1—Se1—Cs1i | 93.29 (3) | Se1—Cs1—Se11iii | 124.33 (3) |
Cs3—Se1—Cs1i | 89.44 (2) | Se5x—Cs1—Se11iii | 87.81 (3) |
Cs1—Se1—Cs1i | 144.26 (2) | Se2i—Cs1—Se11iii | 104.24 (3) |
Se5—Se2—Nb2 | 62.56 (4) | Se2x—Cs1—Se11iii | 70.36 (2) |
Se5—Se2—Nb1 | 115.88 (4) | Se4i—Cs1—Se11iii | 83.20 (3) |
Nb2—Se2—Nb1 | 84.24 (3) | Se9iii—Cs1—Se11iii | 73.65 (2) |
Se5—Se2—Cs1i | 76.53 (4) | Se7—Cs1—Se11iii | 135.67 (3) |
Nb2—Se2—Cs1i | 132.96 (4) | Se11x—Cs1—Se11iii | 127.47 (2) |
Nb1—Se2—Cs1i | 94.28 (3) | Se5i—Cs1—Se11iii | 69.06 (2) |
Se5—Se2—Cs1ii | 70.25 (3) | Se1i—Cs1—Se11iii | 138.57 (3) |
Nb2—Se2—Cs1ii | 90.41 (3) | Se8—Cs2—Se7vii | 120.34 (3) |
Nb1—Se2—Cs1ii | 168.21 (4) | Se8—Cs2—Se6xi | 123.90 (3) |
Cs1i—Se2—Cs1ii | 97.04 (2) | Se7vii—Cs2—Se6xi | 70.83 (3) |
Se9—Se3—Nb1 | 63.07 (3) | Se8—Cs2—Se8vii | 65.94 (3) |
Se9—Se3—Nb2 | 109.29 (4) | Se7vii—Cs2—Se8vii | 62.98 (2) |
Nb1—Se3—Nb2 | 89.16 (4) | Se6xi—Cs2—Se8vii | 76.89 (3) |
Se9—Se3—Cs3iii | 71.03 (3) | Se8—Cs2—Se10 | 60.57 (3) |
Nb1—Se3—Cs3iii | 86.55 (3) | Se7vii—Cs2—Se10 | 99.95 (3) |
Nb2—Se3—Cs3iii | 174.95 (4) | Se6xi—Cs2—Se10 | 170.77 (4) |
Se8—Se4—Nb1 | 62.96 (4) | Se8vii—Cs2—Se10 | 99.48 (3) |
Se8—Se4—Cs1i | 124.63 (4) | Se8—Cs2—Se11xi | 115.83 (4) |
Nb1—Se4—Cs1i | 101.10 (3) | Se7vii—Cs2—Se11xi | 120.89 (4) |
Se8—Se4—Cs3i | 132.08 (4) | Se6xi—Cs2—Se11xi | 63.74 (3) |
Nb1—Se4—Cs3i | 111.76 (4) | Se8vii—Cs2—Se11xi | 132.86 (3) |
Cs1i—Se4—Cs3i | 103.29 (3) | Se10—Cs2—Se11xi | 123.04 (3) |
Se8—Se4—Cs2 | 61.62 (3) | Se8—Cs2—Se10xii | 142.58 (4) |
Nb1—Se4—Cs2 | 120.84 (4) | Se7vii—Cs2—Se10xii | 71.80 (3) |
Cs1i—Se4—Cs2 | 93.76 (3) | Se6xi—Cs2—Se10xii | 93.36 (3) |
Cs3i—Se4—Cs2 | 119.78 (3) | Se8vii—Cs2—Se10xii | 134.51 (3) |
Se2—Se5—Nb2 | 63.06 (4) | Se10—Cs2—Se10xii | 83.12 (3) |
Se2—Se5—Cs1ii | 72.37 (3) | Se11xi—Cs2—Se10xii | 75.16 (3) |
Nb2—Se5—Cs1ii | 91.63 (4) | Se8—Cs2—Se5 | 61.10 (2) |
Se2—Se5—Cs2 | 122.13 (4) | Se7vii—Cs2—Se5 | 152.65 (4) |
Nb2—Se5—Cs2 | 94.25 (4) | Se6xi—Cs2—Se5 | 133.55 (3) |
Cs1ii—Se5—Cs2 | 165.43 (3) | Se8vii—Cs2—Se5 | 127.02 (3) |
Se2—Se5—Cs1i | 67.27 (3) | Se10—Cs2—Se5 | 55.33 (3) |
Nb2—Se5—Cs1i | 125.19 (4) | Se11xi—Cs2—Se5 | 73.26 (3) |
Cs1ii—Se5—Cs1i | 94.37 (2) | Se10xii—Cs2—Se5 | 91.89 (3) |
Cs2—Se5—Cs1i | 93.11 (3) | Se8—Cs2—Se4 | 35.90 (2) |
Se2—Se5—Cs3iv | 150.98 (4) | Se7vii—Cs2—Se4 | 136.91 (3) |
Nb2—Se5—Cs3iv | 141.24 (4) | Se6xi—Cs2—Se4 | 95.54 (3) |
Cs1ii—Se5—Cs3iv | 88.59 (2) | Se8vii—Cs2—Se4 | 74.25 (2) |
Cs2—Se5—Cs3iv | 78.50 (2) | Se10—Cs2—Se4 | 91.56 (3) |
Cs1i—Se5—Cs3iv | 93.39 (3) | Se11xi—Cs2—Se4 | 84.40 (3) |
Se10—Se6—Nb2 | 62.79 (4) | Se10xii—Cs2—Se4 | 151.22 (3) |
Se10—Se6—Cs2v | 110.41 (5) | Se5—Cs2—Se4 | 62.50 (2) |
Nb2—Se6—Cs2v | 93.86 (4) | Se1—Cs3—Se7iii | 119.26 (3) |
Se10—Se6—Cs3vi | 67.81 (4) | Se1—Cs3—Se11iv | 95.17 (3) |
Nb2—Se6—Cs3vi | 130.59 (4) | Se7iii—Cs3—Se11iv | 130.24 (3) |
Cs2v—Se6—Cs3vi | 104.10 (3) | Se1—Cs3—Se10xiii | 141.78 (4) |
Nb1—Se7—Cs2vii | 102.15 (4) | Se7iii—Cs3—Se10xiii | 91.17 (3) |
Nb1—Se7—Cs3iii | 98.57 (4) | Se11iv—Cs3—Se10xiii | 79.08 (3) |
Cs2vii—Se7—Cs3iii | 110.65 (4) | Se1—Cs3—Se4i | 55.95 (2) |
Nb1—Se7—Cs1 | 99.65 (4) | Se7iii—Cs3—Se4i | 121.23 (3) |
Cs2vii—Se7—Cs1 | 143.44 (4) | Se11iv—Cs3—Se4i | 107.48 (3) |
Cs3iii—Se7—Cs1 | 94.54 (3) | Se10xiii—Cs3—Se4i | 89.45 (3) |
Se4—Se8—Nb1 | 62.64 (4) | Se1—Cs3—Se9iii | 59.55 (2) |
Se4—Se8—Nb2 | 113.99 (4) | Se7iii—Cs3—Se9iii | 63.73 (2) |
Nb1—Se8—Nb2 | 83.24 (3) | Se11iv—Cs3—Se9iii | 151.47 (3) |
Se4—Se8—Cs2 | 82.49 (4) | Se10xiii—Cs3—Se9iii | 128.66 (3) |
Nb1—Se8—Cs2 | 139.36 (4) | Se4i—Cs3—Se9iii | 70.83 (2) |
Nb2—Se8—Cs2 | 93.49 (3) | Se1—Cs3—Se6xiii | 131.43 (3) |
Se4—Se8—Cs2vii | 98.78 (4) | Se7iii—Cs3—Se6xiii | 68.61 (3) |
Nb1—Se8—Cs2vii | 92.49 (3) | Se11iv—Cs3—Se6xiii | 115.51 (3) |
Nb2—Se8—Cs2vii | 139.82 (4) | Se10xiii—Cs3—Se6xiii | 36.44 (3) |
Cs2—Se8—Cs2vii | 114.06 (3) | Se4i—Cs3—Se6xiii | 78.49 (3) |
Se3—Se9—Nb1 | 63.93 (3) | Se9iii—Cs3—Se6xiii | 92.40 (3) |
Se3—Se9—Cs1iii | 91.74 (4) | Se1—Cs3—Se3iii | 82.86 (2) |
Nb1—Se9—Cs1iii | 149.89 (4) | Se7iii—Cs3—Se3iii | 62.00 (2) |
Se3—Se9—Cs3iii | 73.28 (3) | Se11iv—Cs3—Se3iii | 165.15 (4) |
Nb1—Se9—Cs3iii | 87.85 (3) | Se10xiii—Cs3—Se3iii | 93.31 (3) |
Cs1iii—Se9—Cs3iii | 102.48 (3) | Se4i—Cs3—Se3iii | 59.30 (2) |
Se3—Se9—Cs3 | 150.83 (4) | Se9iii—Cs3—Se3iii | 35.69 (2) |
Nb1—Se9—Cs3 | 104.85 (3) | Se6xiii—Cs3—Se3iii | 57.75 (2) |
Cs1iii—Se9—Cs3 | 87.74 (2) | Se1—Cs3—Se9 | 50.37 (2) |
Cs3iii—Se9—Cs3 | 135.19 (3) | Se7iii—Cs3—Se9 | 74.70 (3) |
Se6—Se10—Nb2 | 63.61 (4) | Se11iv—Cs3—Se9 | 109.81 (3) |
Se6—Se10—Cs3vi | 75.76 (4) | Se10xiii—Cs3—Se9 | 165.87 (3) |
Nb2—Se10—Cs3vi | 139.35 (5) | Se4i—Cs3—Se9 | 97.91 (2) |
Se6—Se10—Cs2 | 109.63 (5) | Se9iii—Cs3—Se9 | 44.81 (3) |
Nb2—Se10—Cs2 | 95.66 (4) | Se6xiii—Cs3—Se9 | 133.47 (3) |
Cs3vi—Se10—Cs2 | 96.92 (4) | Se3iii—Cs3—Se9 | 80.30 (2) |
Se6—Se10—Cs2viii | 132.71 (6) | Se1—Cs3—Se5ix | 123.72 (3) |
Nb2—Se10—Cs2viii | 123.76 (5) | Se7iii—Cs3—Se5ix | 58.73 (3) |
Cs3vi—Se10—Cs2viii | 84.51 (3) | Se11iv—Cs3—Se5ix | 72.62 (3) |
Cs2—Se10—Cs2viii | 115.18 (4) | Se10xiii—Cs3—Se5ix | 90.91 (3) |
Nb2—Se11—Cs3ix | 155.85 (6) | Se4i—Cs3—Se5ix | 179.64 (3) |
Nb2—Se11—Cs2v | 94.36 (4) | Se9iii—Cs3—Se5ix | 108.91 (3) |
Cs3ix—Se11—Cs2v | 84.74 (3) | Se6xiii—Cs3—Se5ix | 101.78 (3) |
Nb2—Se11—Cs1ii | 91.55 (4) | Se3iii—Cs3—Se5ix | 120.64 (3) |
Cs3ix—Se11—Cs1ii | 90.33 (3) | Se9—Cs3—Se5ix | 81.73 (2) |
Cs2v—Se11—Cs1ii | 173.98 (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, y−1/2, −z+3/2; (v) x, y+1, z; (vi) x−1, 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, z−1/2; (xi) x, y−1, z; (xii) −x+1, y−1/2, −z+3/2; (xiii) x+1, y, z. |
(II) dodecapotassium hexaniobium pentatriacontaselenide
top
Crystal data top
K12Nb6Se35.30 | Dx = 4.099 Mg m−3 |
Mr = 3810.00 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pbcn | Cell parameters from 8508 reflections |
a = 8.3290 (4) Å | θ = 4.4–48.7° |
b = 13.2559 (7) Å | µ = 22.69 mm−1 |
c = 55.974 (3) Å | T = 100 K |
V = 6180.0 (5) Å3 | Plate, black |
Z = 4 | 0.16 × 0.12 × 0.02 mm |
F(000) = 6697 | |
Data collection top
Bruker APEXII CCD diffractometer | 5107 independent reflections |
Radiation source: fine-focus sealed tube | 4470 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.074 |
ω and φ scans | θmax = 24.4°, θmin = 1.5° |
Absorption correction: empirical (using intensity measurements) (SADABS; Bruker, 2008) | h = −9→9 |
Tmin = 0.380, Tmax = 0.745 | k = −15→15 |
53662 measured reflections | l = −65→65 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.031 | Secondary 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 reflections | Δρmax = 1.96 e Å−3 |
263 parameters | Δρmin = −0.97 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Nb1 | 0.04055 (8) | 0.13613 (5) | 0.047032 (13) | 0.00663 (16) | |
Nb2 | −0.56408 (9) | 0.21560 (5) | 0.218406 (13) | 0.00765 (16) | |
Nb3 | 0.04190 (8) | 0.05393 (5) | 0.110845 (13) | 0.00614 (16) | |
Se1 | 0.34720 (9) | 0.10761 (6) | 0.050461 (15) | 0.01015 (18) | |
Se2 | −0.19337 (9) | 0.14446 (6) | 0.077886 (14) | 0.00756 (17) | |
Se3 | −0.08333 (10) | −0.11819 (6) | 0.097098 (15) | 0.00894 (18) | |
Se4 | −0.43858 (10) | 0.09735 (6) | 0.186624 (15) | 0.01356 (19) | |
Se5 | 0.12568 (9) | −0.04697 (6) | 0.073411 (14) | 0.00742 (17) | |
Se6 | 0.00073 (10) | 0.24204 (6) | 0.119925 (15) | 0.00955 (18) | |
Se7 | 0.11822 (10) | 0.01882 (6) | 0.011250 (15) | 0.01058 (18) | |
Se8 | −0.71760 (9) | 0.15174 (6) | 0.255859 (14) | 0.00871 (18) | |
Se9 | 0.20400 (9) | 0.19291 (6) | 0.085980 (14) | 0.00792 (18) | |
Se10 | −0.67021 (10) | 0.03176 (6) | 0.225458 (15) | 0.01108 (18) | |
Se11 | 0.24578 (10) | 0.00344 (6) | 0.137888 (15) | 0.01300 (19) | |
Se12 | −0.23252 (9) | 0.04710 (6) | 0.042809 (14) | 0.01003 (18) | |
Se13 | −0.21767 (10) | 0.02909 (6) | 0.136669 (14) | 0.01073 (18) | |
Se14 | −0.32294 (10) | 0.33432 (6) | 0.211489 (15) | 0.01188 (19) | |
Se16 | −0.25798 (10) | 0.17889 (6) | 0.159701 (15) | 0.01254 (19) | |
Se15 | −0.5000 | 0.36262 (8) | 0.2500 | 0.0087 (2) | |
Se17 | −0.77138 (11) | 0.29302 (7) | 0.196531 (16) | 0.0174 (2) | |
Se18 | 0.01459 (15) | 0.29337 (8) | 0.02814 (2) | 0.0145 (2) | 0.85 |
Se19 | −0.1020 (8) | 0.2440 (5) | 0.01393 (12) | 0.0242 (15) | 0.15 |
Se20 | 0.0966 (9) | 0.3188 (5) | 0.03782 (14) | 0.0260 (16) | 0.15 |
K1 | 0.5000 | 0.0000 | 0.0000 | 0.0172 (6) | |
K2 | 0.5000 | −0.1672 (2) | 0.2500 | 0.0141 (6) | |
K3 | 0.0893 (3) | 0.19994 (16) | −0.03207 (4) | 0.0286 (5) | |
K4 | 0.0147 (2) | 0.04036 (16) | 0.18954 (4) | 0.0246 (5) | |
K5 | −0.0265 (2) | 0.44109 (17) | 0.08581 (4) | 0.0260 (5) | |
K6 | 0.5523 (2) | −0.11994 (14) | 0.16630 (3) | 0.0167 (4) | |
K7 | 0.3839 (2) | 0.24864 (15) | 0.14025 (3) | 0.0158 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nb1 | 0.0056 (4) | 0.0095 (4) | 0.0048 (4) | −0.0010 (3) | 0.0008 (3) | −0.0001 (3) |
Nb2 | 0.0094 (4) | 0.0083 (4) | 0.0052 (4) | −0.0009 (3) | 0.0005 (3) | −0.0010 (3) |
Nb3 | 0.0067 (4) | 0.0074 (4) | 0.0044 (4) | −0.0001 (3) | −0.0006 (3) | 0.0004 (3) |
Se1 | 0.0057 (4) | 0.0170 (5) | 0.0077 (4) | −0.0009 (3) | 0.0013 (3) | −0.0015 (4) |
Se2 | 0.0071 (4) | 0.0094 (4) | 0.0061 (4) | 0.0015 (3) | 0.0013 (3) | −0.0001 (3) |
Se3 | 0.0094 (4) | 0.0075 (4) | 0.0099 (4) | −0.0012 (3) | 0.0000 (3) | 0.0002 (3) |
Se4 | 0.0186 (5) | 0.0125 (4) | 0.0096 (4) | −0.0024 (4) | 0.0060 (4) | −0.0038 (4) |
Se5 | 0.0072 (4) | 0.0085 (4) | 0.0066 (4) | 0.0017 (3) | 0.0003 (3) | −0.0007 (3) |
Se6 | 0.0134 (4) | 0.0082 (4) | 0.0071 (4) | −0.0001 (3) | 0.0018 (3) | −0.0021 (3) |
Se7 | 0.0071 (4) | 0.0180 (5) | 0.0066 (4) | 0.0008 (3) | 0.0000 (3) | −0.0045 (3) |
Se8 | 0.0079 (4) | 0.0108 (4) | 0.0074 (4) | −0.0008 (3) | 0.0010 (3) | −0.0003 (3) |
Se9 | 0.0088 (4) | 0.0088 (4) | 0.0061 (4) | −0.0029 (3) | −0.0009 (3) | −0.0003 (3) |
Se10 | 0.0133 (4) | 0.0089 (4) | 0.0111 (4) | −0.0024 (3) | 0.0003 (3) | −0.0020 (3) |
Se11 | 0.0140 (4) | 0.0134 (4) | 0.0116 (4) | 0.0006 (4) | −0.0049 (4) | 0.0013 (4) |
Se12 | 0.0055 (4) | 0.0169 (5) | 0.0077 (4) | −0.0005 (3) | −0.0003 (3) | −0.0034 (3) |
Se13 | 0.0108 (4) | 0.0135 (4) | 0.0079 (4) | −0.0017 (3) | 0.0036 (3) | −0.0021 (3) |
Se14 | 0.0136 (4) | 0.0127 (4) | 0.0093 (4) | −0.0044 (4) | 0.0025 (4) | 0.0017 (4) |
Se16 | 0.0120 (4) | 0.0136 (4) | 0.0120 (4) | −0.0004 (4) | 0.0040 (4) | −0.0026 (4) |
Se15 | 0.0131 (6) | 0.0064 (6) | 0.0067 (6) | 0.000 | −0.0010 (5) | 0.000 |
Se17 | 0.0185 (5) | 0.0198 (5) | 0.0138 (5) | 0.0059 (4) | −0.0042 (4) | 0.0004 (4) |
Se18 | 0.0174 (6) | 0.0125 (6) | 0.0138 (6) | 0.0016 (5) | 0.0000 (5) | 0.0044 (5) |
Se19 | 0.027 (4) | 0.020 (3) | 0.026 (4) | 0.002 (3) | −0.004 (3) | −0.005 (3) |
Se20 | 0.028 (4) | 0.020 (4) | 0.030 (4) | 0.002 (3) | −0.009 (4) | 0.001 (3) |
K1 | 0.0122 (13) | 0.0247 (15) | 0.0146 (14) | 0.0005 (12) | 0.0004 (11) | −0.0033 (12) |
K2 | 0.0137 (13) | 0.0129 (13) | 0.0156 (15) | 0.000 | 0.0020 (11) | 0.000 |
K3 | 0.0415 (14) | 0.0177 (11) | 0.0267 (13) | 0.0063 (10) | −0.0079 (10) | 0.0047 (9) |
K4 | 0.0236 (11) | 0.0313 (12) | 0.0191 (11) | −0.0039 (10) | −0.0073 (9) | 0.0081 (9) |
K5 | 0.0112 (10) | 0.0312 (12) | 0.0356 (13) | 0.0031 (9) | 0.0034 (9) | 0.0229 (10) |
K6 | 0.0200 (10) | 0.0148 (10) | 0.0153 (10) | −0.0001 (8) | −0.0005 (8) | −0.0020 (8) |
K7 | 0.0136 (10) | 0.0201 (10) | 0.0137 (10) | −0.0032 (8) | −0.0024 (8) | −0.0001 (8) |
Geometric parameters (Å, º) top
Nb1—Se18 | 2.3473 (12) | Se16—K6viii | 3.191 (2) |
Nb1—Se20 | 2.520 (7) | Se16—K7vii | 3.307 (2) |
Nb1—Se12 | 2.5732 (11) | Se16—K4 | 3.364 (2) |
Nb1—Se1 | 2.5890 (11) | Se15—Se14i | 2.6387 (9) |
Nb1—Se2 | 2.6059 (10) | Se15—Nb2i | 2.6853 (11) |
Nb1—Se7 | 2.6169 (11) | Se17—K6x | 3.110 (2) |
Nb1—Se19 | 2.624 (7) | Se17—K7vii | 3.456 (2) |
Nb1—Se9 | 2.6781 (11) | Se17—K2ix | 3.5863 (10) |
Nb1—Se5 | 2.9281 (11) | Se17—K4vii | 3.814 (2) |
Nb2—Se17 | 2.3523 (11) | Se17—K4x | 3.934 (2) |
Nb2—Se14 | 2.5808 (11) | Se18—Se20 | 0.935 (8) |
Nb2—Se4 | 2.5913 (11) | Se18—Se19 | 1.415 (7) |
Nb2—Se8 | 2.5974 (11) | Se18—K1v | 3.1619 (10) |
Nb2—Se10 | 2.6222 (11) | Se18—K3v | 3.550 (3) |
Nb2—Se15 | 2.6852 (11) | Se18—K3 | 3.644 (3) |
Nb2—Se8i | 2.8803 (11) | Se18—K5 | 3.791 (3) |
Nb3—Se11 | 2.3713 (11) | Se19—Se20 | 2.347 (11) |
Nb3—Se6 | 2.5678 (10) | Se19—K3v | 2.862 (7) |
Nb3—Se5 | 2.5819 (10) | Se19—K3 | 3.084 (7) |
Nb3—Se13 | 2.6214 (11) | Se19—K1v | 3.584 (7) |
Nb3—Se3 | 2.6240 (10) | Se20—K5 | 3.300 (8) |
Nb3—Se9 | 2.6747 (10) | Se20—K1v | 3.301 (7) |
Nb3—Se2 | 2.9467 (11) | K1—Se18ii | 3.1619 (10) |
Se1—Se9 | 2.5794 (11) | K1—Se18iii | 3.1619 (10) |
Se1—K5ii | 3.319 (2) | K1—Se7xii | 3.2512 (8) |
Se1—K1 | 3.4106 (8) | K1—Se20ii | 3.301 (7) |
Se1—K3iii | 3.411 (2) | K1—Se20iii | 3.301 (7) |
Se2—Se12 | 2.3720 (11) | K1—Se12vi | 3.3309 (8) |
Se2—K5iv | 3.592 (2) | K1—Se12xiii | 3.3309 (8) |
Se2—K3v | 3.756 (2) | K1—Se1xii | 3.4106 (8) |
Se3—Se5 | 2.3833 (11) | K1—Se19ii | 3.584 (7) |
Se3—K5iv | 3.402 (2) | K1—Se19iii | 3.584 (7) |
Se3—K7ii | 3.422 (2) | K2—Se10xiv | 3.294 (2) |
Se3—K3vi | 3.798 (2) | K2—Se10xiii | 3.294 (2) |
Se4—Se16 | 2.3879 (12) | K2—Se8iv | 3.377 (2) |
Se4—K6vii | 3.098 (2) | K2—Se8xv | 3.377 (2) |
Se4—K7vii | 3.598 (2) | K2—Se14ii | 3.4471 (9) |
Se4—K4 | 3.853 (2) | K2—Se14xvi | 3.4471 (9) |
Se5—K5ii | 3.414 (2) | K2—Se17iv | 3.5862 (10) |
Se5—K3vi | 3.560 (2) | K2—Se17xv | 3.5862 (10) |
Se6—Se9 | 2.6269 (11) | K3—Se19iii | 2.862 (7) |
Se6—K6viii | 3.206 (2) | K3—Se1v | 3.411 (2) |
Se6—K5 | 3.265 (2) | K3—Se12vi | 3.537 (2) |
Se6—K7 | 3.389 (2) | K3—Se18iii | 3.550 (3) |
Se7—Se7vi | 2.3903 (16) | K3—Se5vi | 3.560 (2) |
Se7—K1 | 3.2512 (8) | K3—Se7vi | 3.571 (2) |
Se7—K3 | 3.421 (2) | K3—Se12iii | 3.716 (2) |
Se7—K3vi | 3.571 (2) | K3—Se2iii | 3.756 (2) |
Se8—Se10 | 2.3624 (11) | K3—Se3vi | 3.798 (2) |
Se8—Nb2i | 2.8803 (11) | K4—Se10xiii | 3.308 (2) |
Se8—K2ix | 3.377 (2) | K4—Se14iv | 3.394 (2) |
Se9—K7 | 3.467 (2) | K4—Se17xiii | 3.814 (2) |
Se9—K5 | 3.809 (2) | K4—Se17iv | 3.934 (2) |
Se10—K2vii | 3.294 (2) | K5—Se1viii | 3.319 (2) |
Se10—K4vii | 3.308 (2) | K5—Se3x | 3.402 (2) |
Se11—K6 | 3.424 (2) | K5—Se5viii | 3.414 (2) |
Se11—K7 | 3.450 (2) | K5—Se12x | 3.434 (2) |
Se11—K4 | 3.507 (2) | K5—Se2x | 3.592 (2) |
Se11—K7ii | 3.549 (2) | K5—Se13x | 3.742 (2) |
Se11—K5ii | 3.827 (2) | K5—Se11viii | 3.827 (2) |
Se12—K1vii | 3.3309 (8) | K6—Se4xiii | 3.098 (2) |
Se12—K5iv | 3.434 (2) | K6—Se17iv | 3.110 (2) |
Se12—K3vi | 3.537 (2) | K6—Se16ii | 3.191 (2) |
Se12—K3v | 3.716 (2) | K6—Se6ii | 3.206 (2) |
Se13—Se16 | 2.3912 (12) | K6—Se13xiii | 3.213 (2) |
Se13—K6vii | 3.213 (2) | K6—Se14ii | 3.442 (2) |
Se13—K4 | 3.539 (2) | K7—Se16xiii | 3.307 (2) |
Se13—K5iv | 3.742 (2) | K7—Se3viii | 3.422 (2) |
Se14—Se15 | 2.6386 (8) | K7—Se17xiii | 3.456 (2) |
Se14—K4x | 3.394 (2) | K7—Se11viii | 3.549 (2) |
Se14—K6viii | 3.442 (2) | K7—Se4xiii | 3.598 (2) |
Se14—K2xi | 3.4470 (9) | | |
| | | |
Se18—Nb1—Se20 | 21.78 (18) | Nb1—Se20—K5 | 104.4 (2) |
Se18—Nb1—Se12 | 106.52 (5) | Se18—Se20—K1v | 73.3 (4) |
Se20—Nb1—Se12 | 125.86 (18) | Se19—Se20—K1v | 76.7 (3) |
Se18—Nb1—Se1 | 104.71 (4) | Nb1—Se20—K1v | 141.7 (3) |
Se20—Nb1—Se1 | 88.44 (18) | K5—Se20—K1v | 95.10 (18) |
Se12—Nb1—Se1 | 144.27 (4) | Se18ii—K1—Se18iii | 180.00 (4) |
Se18—Nb1—Se2 | 101.08 (4) | Se18ii—K1—Se7 | 86.13 (3) |
Se20—Nb1—Se2 | 103.49 (17) | Se18iii—K1—Se7 | 93.87 (3) |
Se12—Nb1—Se2 | 54.51 (3) | Se18ii—K1—Se7xii | 93.88 (3) |
Se1—Nb1—Se2 | 134.00 (4) | Se18iii—K1—Se7xii | 86.12 (3) |
Se18—Nb1—Se7 | 101.86 (4) | Se7—K1—Se7xii | 180.0 |
Se20—Nb1—Se7 | 111.64 (17) | Se18ii—K1—Se20ii | 16.46 (14) |
Se12—Nb1—Se7 | 82.86 (3) | Se18iii—K1—Se20ii | 163.54 (14) |
Se1—Nb1—Se7 | 74.10 (3) | Se7—K1—Se20ii | 72.14 (14) |
Se2—Nb1—Se7 | 135.83 (4) | Se7xii—K1—Se20ii | 107.87 (14) |
Se18—Nb1—Se19 | 32.47 (15) | Se18ii—K1—Se20iii | 163.54 (14) |
Se20—Nb1—Se19 | 54.2 (2) | Se18iii—K1—Se20iii | 16.46 (14) |
Se12—Nb1—Se19 | 77.60 (15) | Se7—K1—Se20iii | 107.86 (14) |
Se1—Nb1—Se19 | 125.32 (15) | Se7xii—K1—Se20iii | 72.13 (14) |
Se2—Nb1—Se19 | 96.12 (15) | Se20ii—K1—Se20iii | 180.0 (3) |
Se7—Nb1—Se19 | 83.99 (15) | Se18ii—K1—Se12vi | 99.80 (2) |
Se18—Nb1—Se9 | 99.44 (4) | Se18iii—K1—Se12vi | 80.20 (2) |
Se20—Nb1—Se9 | 78.59 (19) | Se7—K1—Se12vi | 59.97 (2) |
Se12—Nb1—Se9 | 130.77 (4) | Se7xii—K1—Se12vi | 120.03 (2) |
Se1—Nb1—Se9 | 58.62 (3) | Se20ii—K1—Se12vi | 99.32 (13) |
Se2—Nb1—Se9 | 80.14 (3) | Se20iii—K1—Se12vi | 80.68 (13) |
Se7—Nb1—Se9 | 131.63 (4) | Se18ii—K1—Se12xiii | 80.20 (2) |
Se19—Nb1—Se9 | 130.66 (14) | Se18iii—K1—Se12xiii | 99.80 (2) |
Se18—Nb1—Se5 | 170.25 (5) | Se7—K1—Se12xiii | 120.03 (2) |
Se20—Nb1—Se5 | 148.76 (19) | Se7xii—K1—Se12xiii | 59.97 (2) |
Se12—Nb1—Se5 | 83.12 (3) | Se20ii—K1—Se12xiii | 80.68 (13) |
Se1—Nb1—Se5 | 66.59 (3) | Se20iii—K1—Se12xiii | 99.32 (13) |
Se2—Nb1—Se5 | 83.22 (3) | Se12vi—K1—Se12xiii | 180.00 (3) |
Se7—Nb1—Se5 | 80.42 (3) | Se18ii—K1—Se1 | 86.30 (3) |
Se19—Nb1—Se5 | 156.52 (14) | Se18iii—K1—Se1 | 93.70 (3) |
Se9—Nb1—Se5 | 72.51 (3) | Se7—K1—Se1 | 56.12 (2) |
Se17—Nb2—Se14 | 103.13 (4) | Se7xii—K1—Se1 | 123.88 (2) |
Se17—Nb2—Se4 | 101.69 (4) | Se20ii—K1—Se1 | 71.47 (14) |
Se14—Nb2—Se4 | 87.24 (3) | Se20iii—K1—Se1 | 108.53 (14) |
Se17—Nb2—Se8 | 101.59 (4) | Se12vi—K1—Se1 | 115.124 (19) |
Se14—Nb2—Se8 | 134.66 (4) | Se12xiii—K1—Se1 | 64.876 (19) |
Se4—Nb2—Se8 | 123.75 (4) | Se18ii—K1—Se1xii | 93.70 (3) |
Se17—Nb2—Se10 | 103.67 (4) | Se18iii—K1—Se1xii | 86.30 (3) |
Se14—Nb2—Se10 | 148.39 (4) | Se7—K1—Se1xii | 123.88 (2) |
Se4—Nb2—Se10 | 71.16 (3) | Se7xii—K1—Se1xii | 56.12 (2) |
Se8—Nb2—Se10 | 53.82 (3) | Se20ii—K1—Se1xii | 108.53 (14) |
Se17—Nb2—Se15 | 99.91 (4) | Se20iii—K1—Se1xii | 71.47 (14) |
Se14—Nb2—Se15 | 60.10 (3) | Se12vi—K1—Se1xii | 64.876 (19) |
Se4—Nb2—Se15 | 144.19 (4) | Se12xiii—K1—Se1xii | 115.124 (19) |
Se8—Nb2—Se15 | 78.63 (3) | Se1—K1—Se1xii | 179.999 (15) |
Se10—Nb2—Se15 | 129.97 (4) | Se18ii—K1—Se19ii | 23.15 (11) |
Se17—Nb2—Se8i | 170.54 (4) | Se18iii—K1—Se19ii | 156.85 (11) |
Se14—Nb2—Se8i | 67.69 (3) | Se7—K1—Se19ii | 105.21 (11) |
Se4—Nb2—Se8i | 80.62 (3) | Se7xii—K1—Se19ii | 74.79 (11) |
Se8—Nb2—Se8i | 84.35 (3) | Se20ii—K1—Se19ii | 39.59 (18) |
Se10—Nb2—Se8i | 85.76 (3) | Se20iii—K1—Se19ii | 140.41 (18) |
Se15—Nb2—Se8i | 73.86 (3) | Se12vi—K1—Se19ii | 97.91 (11) |
Se11—Nb3—Se6 | 104.08 (4) | Se12xiii—K1—Se19ii | 82.09 (11) |
Se11—Nb3—Se5 | 100.27 (4) | Se1—K1—Se19ii | 107.71 (11) |
Se6—Nb3—Se5 | 134.41 (4) | Se1xii—K1—Se19ii | 72.29 (11) |
Se11—Nb3—Se13 | 101.72 (4) | Se18ii—K1—Se19iii | 156.85 (11) |
Se6—Nb3—Se13 | 84.42 (3) | Se18iii—K1—Se19iii | 23.15 (11) |
Se5—Nb3—Se13 | 127.25 (4) | Se7—K1—Se19iii | 74.79 (11) |
Se11—Nb3—Se3 | 103.09 (4) | Se7xii—K1—Se19iii | 105.21 (11) |
Se6—Nb3—Se3 | 148.14 (4) | Se20ii—K1—Se19iii | 140.41 (18) |
Se5—Nb3—Se3 | 54.48 (3) | Se20iii—K1—Se19iii | 39.59 (18) |
Se13—Nb3—Se3 | 74.02 (3) | Se12vi—K1—Se19iii | 82.09 (11) |
Se11—Nb3—Se9 | 99.50 (4) | Se12xiii—K1—Se19iii | 97.91 (11) |
Se6—Nb3—Se9 | 60.10 (3) | Se1—K1—Se19iii | 72.29 (11) |
Se5—Nb3—Se9 | 78.35 (3) | Se1xii—K1—Se19iii | 107.71 (11) |
Se13—Nb3—Se9 | 142.16 (4) | Se19ii—K1—Se19iii | 180.0 (3) |
Se3—Nb3—Se9 | 130.31 (4) | Se10xiv—K2—Se10xiii | 73.64 (6) |
Se11—Nb3—Se2 | 172.22 (4) | Se10xiv—K2—Se8iv | 145.93 (2) |
Se6—Nb3—Se2 | 68.88 (3) | Se10xiii—K2—Se8iv | 108.05 (2) |
Se5—Nb3—Se2 | 83.26 (3) | Se10xiv—K2—Se8xv | 108.05 (2) |
Se13—Nb3—Se2 | 81.25 (3) | Se10xiii—K2—Se8xv | 145.93 (2) |
Se3—Nb3—Se2 | 84.62 (3) | Se8iv—K2—Se8xv | 89.38 (7) |
Se9—Nb3—Se2 | 74.30 (3) | Se10xiv—K2—Se14ii | 85.44 (4) |
Se9—Se1—Nb1 | 62.42 (3) | Se10xiii—K2—Se14ii | 94.04 (4) |
Se9—Se1—K5ii | 92.30 (5) | Se8iv—K2—Se14ii | 127.47 (6) |
Nb1—Se1—K5ii | 125.82 (5) | Se8xv—K2—Se14ii | 53.12 (2) |
Se9—Se1—K1 | 173.81 (4) | Se10xiv—K2—Se14xvi | 94.04 (4) |
Nb1—Se1—K1 | 111.58 (3) | Se10xiii—K2—Se14xvi | 85.44 (4) |
K5ii—Se1—K1 | 92.73 (5) | Se8iv—K2—Se14xvi | 53.12 (2) |
Se9—Se1—K3iii | 100.27 (5) | Se8xv—K2—Se14xvi | 127.47 (6) |
Nb1—Se1—K3iii | 116.85 (5) | Se14ii—K2—Se14xvi | 179.35 (9) |
K5ii—Se1—K3iii | 114.28 (6) | Se10xiv—K2—Se17iv | 133.98 (7) |
K1—Se1—K3iii | 80.92 (4) | Se10xiii—K2—Se17iv | 62.69 (3) |
Se12—Se2—Nb1 | 62.04 (3) | Se8iv—K2—Se17iv | 66.83 (3) |
Se12—Se2—Nb3 | 112.83 (4) | Se8xv—K2—Se17iv | 100.61 (5) |
Nb1—Se2—Nb3 | 84.29 (3) | Se14ii—K2—Se17iv | 83.87 (2) |
Se12—Se2—K5iv | 66.71 (5) | Se14xvi—K2—Se17iv | 96.22 (2) |
Nb1—Se2—K5iv | 122.38 (5) | Se10xiv—K2—Se17xv | 62.69 (3) |
Nb3—Se2—K5iv | 92.81 (4) | Se10xiii—K2—Se17xv | 133.98 (7) |
Se12—Se2—K3v | 70.57 (4) | Se8iv—K2—Se17xv | 100.61 (5) |
Nb1—Se2—K3v | 86.05 (4) | Se8xv—K2—Se17xv | 66.83 (3) |
Nb3—Se2—K3v | 166.30 (5) | Se14ii—K2—Se17xv | 96.22 (2) |
K5iv—Se2—K3v | 100.57 (5) | Se14xvi—K2—Se17xv | 83.87 (2) |
Se5—Se3—Nb3 | 61.86 (3) | Se17iv—K2—Se17xv | 163.07 (9) |
Se5—Se3—K5iv | 120.19 (5) | Se19iii—K3—Se19 | 96.83 (10) |
Nb3—Se3—K5iv | 103.49 (5) | Se19iii—K3—Se1v | 116.36 (15) |
Se5—Se3—K7ii | 104.03 (4) | Se19—K3—Se1v | 78.74 (13) |
Nb3—Se3—K7ii | 92.79 (4) | Se19iii—K3—Se7 | 82.39 (15) |
K5iv—Se3—K7ii | 135.55 (5) | Se19—K3—Se7 | 65.01 (13) |
Se5—Se3—K3vi | 65.76 (4) | Se1v—K3—Se7 | 141.30 (8) |
Nb3—Se3—K3vi | 122.30 (5) | Se19iii—K3—Se12vi | 89.87 (14) |
K5iv—Se3—K3vi | 82.84 (6) | Se19—K3—Se12vi | 119.45 (14) |
K7ii—Se3—K3vi | 122.39 (5) | Se1v—K3—Se12vi | 147.20 (7) |
Se16—Se4—Nb2 | 114.43 (4) | Se7—K3—Se12vi | 56.42 (4) |
Se16—Se4—K6vii | 101.81 (5) | Se19iii—K3—Se18iii | 22.38 (13) |
Nb2—Se4—K6vii | 143.58 (5) | Se19—K3—Se18iii | 117.33 (14) |
Se16—Se4—K7vii | 63.34 (4) | Se1v—K3—Se18iii | 126.15 (7) |
Nb2—Se4—K7vii | 89.56 (4) | Se7—K3—Se18iii | 84.45 (5) |
K6vii—Se4—K7vii | 104.08 (5) | Se12vi—K3—Se18iii | 72.37 (5) |
Se16—Se4—K4 | 59.89 (4) | Se19iii—K3—Se5vi | 146.12 (15) |
Nb2—Se4—K4 | 119.00 (5) | Se19—K3—Se5vi | 113.00 (14) |
K6vii—Se4—K4 | 81.80 (5) | Se1v—K3—Se5vi | 86.13 (5) |
K7vii—Se4—K4 | 122.85 (5) | Se7—K3—Se5vi | 95.53 (6) |
Se3—Se5—Nb3 | 63.66 (3) | Se12vi—K3—Se5vi | 62.08 (4) |
Se3—Se5—Nb1 | 115.59 (4) | Se18iii—K3—Se5vi | 123.81 (7) |
Nb3—Se5—Nb1 | 85.09 (3) | Se19iii—K3—Se7vi | 121.99 (15) |
Se3—Se5—K5ii | 125.66 (5) | Se19—K3—Se7vi | 68.37 (13) |
Nb3—Se5—K5ii | 97.09 (5) | Se1v—K3—Se7vi | 114.81 (7) |
Nb1—Se5—K5ii | 112.19 (4) | Se7—K3—Se7vi | 39.91 (3) |
Se3—Se5—K3vi | 76.62 (5) | Se12vi—K3—Se7vi | 57.78 (4) |
Nb3—Se5—K3vi | 133.36 (5) | Se18iii—K3—Se7vi | 118.88 (6) |
Nb1—Se5—K3vi | 91.29 (4) | Se5vi—K3—Se7vi | 60.40 (4) |
K5ii—Se5—K3vi | 126.70 (6) | Se19iii—K3—Se18 | 74.76 (14) |
Nb3—Se6—Se9 | 61.97 (3) | Se19—K3—Se18 | 22.36 (13) |
Nb3—Se6—K6viii | 137.12 (5) | Se1v—K3—Se18 | 85.64 (5) |
Se9—Se6—K6viii | 144.67 (5) | Se7—K3—Se18 | 66.11 (5) |
Nb3—Se6—K5 | 132.71 (5) | Se12vi—K3—Se18 | 121.97 (6) |
Se9—Se6—K5 | 79.76 (5) | Se18iii—K3—Se18 | 96.01 (6) |
K6viii—Se6—K5 | 90.16 (6) | Se5vi—K3—Se18 | 135.14 (7) |
Nb3—Se6—K7 | 88.04 (4) | Se7vi—K3—Se18 | 83.78 (5) |
Se9—Se6—K7 | 69.05 (4) | Se19iii—K3—Se12iii | 57.62 (14) |
K6viii—Se6—K7 | 80.98 (5) | Se19—K3—Se12iii | 99.82 (13) |
K5—Se6—K7 | 103.95 (5) | Se1v—K3—Se12iii | 60.81 (4) |
Se7vi—Se7—Nb1 | 108.89 (5) | Se7—K3—Se12iii | 136.05 (7) |
Se7vi—Se7—K1 | 133.45 (5) | Se12vi—K3—Se12iii | 132.33 (7) |
Nb1—Se7—K1 | 115.82 (3) | Se18iii—K3—Se12iii | 65.73 (5) |
Se7vi—Se7—K3 | 73.44 (5) | Se5vi—K3—Se12iii | 127.57 (6) |
Nb1—Se7—K3 | 96.20 (5) | Se7vi—K3—Se12iii | 168.18 (8) |
K1—Se7—K3 | 89.16 (4) | Se18—K3—Se12iii | 84.90 (5) |
Se7vi—Se7—K3vi | 66.65 (5) | Se19iii—K3—Se2iii | 70.54 (15) |
Nb1—Se7—K3vi | 96.50 (5) | Se19—K3—Se2iii | 135.65 (14) |
K1—Se7—K3vi | 118.31 (4) | Se1v—K3—Se2iii | 70.62 (4) |
K3—Se7—K3vi | 140.09 (3) | Se7—K3—Se2iii | 146.67 (7) |
Se10—Se8—Nb2 | 63.63 (3) | Se12vi—K3—Se2iii | 103.29 (6) |
Se10—Se8—Nb2i | 114.96 (4) | Se18iii—K3—Se2iii | 63.12 (4) |
Nb2—Se8—Nb2i | 84.66 (3) | Se5vi—K3—Se2iii | 96.39 (6) |
Se10—Se8—K2ix | 121.67 (4) | Se7vi—K3—Se2iii | 154.41 (7) |
Nb2—Se8—K2ix | 91.88 (3) | Se18—K3—Se2iii | 121.81 (6) |
Nb2i—Se8—K2ix | 114.02 (4) | Se12iii—K3—Se2iii | 37.02 (3) |
Se1—Se9—Se6 | 164.62 (4) | Se19iii—K3—Se3vi | 115.20 (15) |
Se1—Se9—Nb3 | 109.43 (4) | Se19—K3—Se3vi | 147.93 (14) |
Se6—Se9—Nb3 | 57.93 (3) | Se1v—K3—Se3vi | 85.20 (5) |
Se1—Se9—Nb1 | 58.97 (3) | Se7—K3—Se3vi | 118.68 (6) |
Se6—Se9—Nb1 | 109.32 (4) | Se12vi—K3—Se3vi | 65.00 (4) |
Nb3—Se9—Nb1 | 88.48 (3) | Se18iii—K3—Se3vi | 94.57 (6) |
Se1—Se9—K7 | 124.68 (5) | Se5vi—K3—Se3vi | 37.62 (3) |
Se6—Se9—K7 | 65.92 (4) | Se7vi—K3—Se3vi | 94.28 (5) |
Nb3—Se9—K7 | 84.78 (4) | Se18—K3—Se3vi | 168.82 (7) |
Nb1—Se9—K7 | 173.15 (5) | Se12iii—K3—Se3vi | 96.18 (5) |
Se1—Se9—K5 | 127.57 (5) | Se2iii—K3—Se3vi | 60.57 (4) |
Se6—Se9—K5 | 57.51 (4) | Se10xiii—K4—Se16 | 148.87 (8) |
Nb3—Se9—K5 | 109.98 (4) | Se10xiii—K4—Se14iv | 97.21 (6) |
Nb1—Se9—K5 | 89.11 (4) | Se16—K4—Se14iv | 107.54 (6) |
K7—Se9—K5 | 92.06 (5) | Se10xiii—K4—Se11 | 93.48 (6) |
Se8—Se10—Nb2 | 62.55 (3) | Se16—K4—Se11 | 92.15 (5) |
Se8—Se10—K2vii | 108.09 (4) | Se14iv—K4—Se11 | 116.38 (7) |
Nb2—Se10—K2vii | 131.43 (4) | Se10xiii—K4—Se13 | 160.15 (8) |
Se8—Se10—K4vii | 106.38 (5) | Se16—K4—Se13 | 40.43 (3) |
Nb2—Se10—K4vii | 98.28 (5) | Se14iv—K4—Se13 | 90.66 (5) |
K2vii—Se10—K4vii | 128.50 (5) | Se11—K4—Se13 | 66.74 (4) |
Nb3—Se11—K6 | 164.87 (5) | Se10xiii—K4—Se17xiii | 66.24 (4) |
Nb3—Se11—K7 | 89.85 (4) | Se16—K4—Se17xiii | 83.51 (5) |
K6—Se11—K7 | 100.58 (5) | Se14iv—K4—Se17xiii | 152.79 (7) |
Nb3—Se11—K4 | 95.38 (5) | Se11—K4—Se17xiii | 87.18 (5) |
K6—Se11—K4 | 95.34 (5) | Se13—K4—Se17xiii | 112.24 (6) |
K7—Se11—K4 | 91.14 (5) | Se10xiii—K4—Se4 | 144.07 (7) |
Nb3—Se11—K7ii | 94.27 (4) | Se16—K4—Se4 | 37.88 (3) |
K6—Se11—K7ii | 75.81 (5) | Se14iv—K4—Se4 | 73.27 (4) |
K7—Se11—K7ii | 175.32 (7) | Se11—K4—Se4 | 122.02 (6) |
K4—Se11—K7ii | 86.27 (5) | Se13—K4—Se4 | 55.75 (3) |
Nb3—Se11—K5ii | 90.70 (4) | Se17xiii—K4—Se4 | 106.85 (6) |
K6—Se11—K5ii | 78.17 (5) | Se10xiii—K4—Se17iv | 58.64 (4) |
K7—Se11—K5ii | 91.66 (5) | Se16—K4—Se17iv | 150.61 (7) |
K4—Se11—K5ii | 173.31 (5) | Se14iv—K4—Se17iv | 63.19 (4) |
K7ii—Se11—K5ii | 90.51 (5) | Se11—K4—Se17iv | 70.58 (4) |
Se2—Se12—Nb1 | 63.45 (3) | Se13—K4—Se17iv | 110.20 (6) |
Se2—Se12—K1vii | 142.13 (4) | Se17xiii—K4—Se17iv | 117.89 (5) |
Nb1—Se12—K1vii | 138.01 (3) | Se4—K4—Se17iv | 134.43 (6) |
Se2—Se12—K5iv | 73.91 (5) | Se6—K5—Se20 | 93.30 (13) |
Nb1—Se12—K5iv | 129.77 (5) | Se6—K5—Se1viii | 148.73 (7) |
K1vii—Se12—K5iv | 92.10 (4) | Se20—K5—Se1viii | 72.64 (13) |
Se2—Se12—K3vi | 126.73 (5) | Se6—K5—Se3x | 76.77 (5) |
Nb1—Se12—K3vi | 98.17 (5) | Se20—K5—Se3x | 109.55 (16) |
K1vii—Se12—K3vi | 85.97 (4) | Se1viii—K5—Se3x | 133.96 (6) |
K5iv—Se12—K3vi | 86.41 (6) | Se6—K5—Se5viii | 95.07 (5) |
Se2—Se12—K3v | 72.42 (5) | Se20—K5—Se5viii | 63.47 (15) |
Nb1—Se12—K3v | 87.36 (4) | Se1viii—K5—Se5viii | 53.69 (4) |
K1vii—Se12—K3v | 77.62 (4) | Se3x—K5—Se5viii | 169.28 (8) |
K5iv—Se12—K3v | 104.44 (5) | Se6—K5—Se12x | 141.37 (7) |
K3vi—Se12—K3v | 160.52 (7) | Se20—K5—Se12x | 79.18 (14) |
Se16—Se13—Nb3 | 107.99 (4) | Se1viii—K5—Se12x | 64.73 (4) |
Se16—Se13—K6vii | 98.54 (5) | Se3x—K5—Se12x | 70.53 (4) |
Nb3—Se13—K6vii | 148.61 (5) | Se5viii—K5—Se12x | 114.21 (6) |
Se16—Se13—K4 | 65.85 (5) | Se6—K5—Se2x | 136.37 (7) |
Nb3—Se13—K4 | 90.27 (4) | Se20—K5—Se2x | 118.03 (14) |
K6vii—Se13—K4 | 85.44 (5) | Se1viii—K5—Se2x | 73.72 (4) |
Se16—Se13—K5iv | 126.09 (5) | Se3x—K5—Se2x | 64.92 (4) |
Nb3—Se13—K5iv | 95.12 (4) | Se5viii—K5—Se2x | 125.12 (6) |
K6vii—Se13—K5iv | 82.04 (5) | Se12x—K5—Se2x | 39.38 (3) |
K4—Se13—K5iv | 163.86 (5) | Se6—K5—Se13x | 81.17 (5) |
Nb2—Se14—Se15 | 61.91 (3) | Se20—K5—Se13x | 161.64 (16) |
Nb2—Se14—K4x | 100.30 (5) | Se1viii—K5—Se13x | 120.16 (7) |
Se15—Se14—K4x | 85.32 (5) | Se3x—K5—Se13x | 52.19 (3) |
Nb2—Se14—K6viii | 136.67 (5) | Se5viii—K5—Se13x | 134.18 (7) |
Se15—Se14—K6viii | 160.28 (5) | Se12x—K5—Se13x | 94.19 (5) |
K4x—Se14—K6viii | 84.28 (5) | Se2x—K5—Se13x | 59.36 (4) |
Nb2—Se14—K2xi | 120.66 (5) | Se6—K5—Se18 | 94.26 (6) |
Se15—Se14—K2xi | 85.76 (2) | Se20—K5—Se18 | 12.92 (14) |
K4x—Se14—K2xi | 126.73 (6) | Se1viii—K5—Se18 | 78.19 (5) |
K6viii—Se14—K2xi | 87.11 (4) | Se3x—K5—Se18 | 97.19 (6) |
Se4—Se16—Se13 | 93.03 (4) | Se5viii—K5—Se18 | 76.26 (5) |
Se4—Se16—K6viii | 130.05 (5) | Se12x—K5—Se18 | 70.57 (5) |
Se13—Se16—K6viii | 132.92 (5) | Se2x—K5—Se18 | 109.95 (6) |
Se4—Se16—K7vii | 76.48 (5) | Se13x—K5—Se18 | 149.34 (6) |
Se13—Se16—K7vii | 100.45 (5) | Se6—K5—Se9 | 42.73 (3) |
K6viii—Se16—K7vii | 106.78 (5) | Se20—K5—Se9 | 54.64 (13) |
Se4—Se16—K4 | 82.23 (5) | Se1viii—K5—Se9 | 110.42 (6) |
Se13—Se16—K4 | 73.71 (5) | Se3x—K5—Se9 | 106.35 (6) |
K6viii—Se16—K4 | 92.08 (5) | Se5viii—K5—Se9 | 63.10 (4) |
K7vii—Se16—K4 | 157.64 (6) | Se12x—K5—Se9 | 130.52 (7) |
Se14—Se15—Se14i | 163.65 (6) | Se2x—K5—Se9 | 167.35 (7) |
Se14—Se15—Nb2 | 57.99 (3) | Se13x—K5—Se9 | 123.66 (6) |
Se14i—Se15—Nb2 | 108.89 (4) | Se18—K5—Se9 | 60.69 (4) |
Se14—Se15—Nb2i | 108.89 (4) | Se6—K5—Se11viii | 71.73 (4) |
Se14i—Se15—Nb2i | 57.99 (3) | Se20—K5—Se11viii | 122.41 (15) |
Nb2—Se15—Nb2i | 86.93 (4) | Se1viii—K5—Se11viii | 92.03 (5) |
Nb2—Se17—K6x | 175.88 (6) | Se3x—K5—Se11viii | 119.47 (6) |
Nb2—Se17—K7vii | 97.21 (5) | Se5viii—K5—Se11viii | 63.08 (4) |
K6x—Se17—K7vii | 81.30 (5) | Se12x—K5—Se11viii | 143.36 (7) |
Nb2—Se17—K2ix | 91.12 (4) | Se2x—K5—Se11viii | 109.19 (6) |
K6x—Se17—K2ix | 90.00 (4) | Se13x—K5—Se11viii | 72.61 (5) |
K7vii—Se17—K2ix | 169.89 (4) | Se18—K5—Se11viii | 134.82 (6) |
Nb2—Se17—K4vii | 90.76 (4) | Se9—K5—Se11viii | 82.91 (4) |
K6x—Se17—K4vii | 85.32 (5) | Se4xiii—K6—Se17iv | 99.42 (6) |
K7vii—Se17—K4vii | 86.09 (5) | Se4xiii—K6—Se16ii | 143.74 (7) |
K2ix—Se17—K4vii | 88.10 (5) | Se17iv—K6—Se16ii | 99.03 (6) |
Nb2—Se17—K4x | 90.94 (4) | Se4xiii—K6—Se6ii | 146.23 (7) |
K6x—Se17—K4x | 92.61 (5) | Se17iv—K6—Se6ii | 97.19 (6) |
K7vii—Se17—K4x | 81.24 (5) | Se16ii—K6—Se6ii | 60.22 (4) |
K2ix—Se17—K4x | 104.42 (5) | Se4xiii—K6—Se13xiii | 66.62 (4) |
K4vii—Se17—K4x | 167.33 (7) | Se17iv—K6—Se13xiii | 163.27 (7) |
Se20—Se18—Se19 | 173.6 (5) | Se16ii—K6—Se13xiii | 97.70 (6) |
Se20—Se18—Nb1 | 89.5 (4) | Se6ii—K6—Se13xiii | 90.87 (5) |
Se19—Se18—Nb1 | 84.6 (3) | Se4xiii—K6—Se11 | 75.21 (5) |
Se20—Se18—K1v | 90.2 (4) | Se17iv—K6—Se11 | 82.47 (5) |
Se19—Se18—K1v | 95.4 (3) | Se16ii—K6—Se11 | 138.23 (7) |
Nb1—Se18—K1v | 175.71 (5) | Se6ii—K6—Se11 | 78.10 (5) |
Se20—Se18—K3v | 133.1 (5) | Se13xiii—K6—Se11 | 84.90 (5) |
Se19—Se18—K3v | 50.3 (3) | Se4xiii—K6—Se14ii | 82.98 (5) |
Nb1—Se18—K3v | 94.94 (5) | Se17iv—K6—Se14ii | 91.58 (5) |
K1v—Se18—K3v | 88.33 (4) | Se16ii—K6—Se14ii | 65.56 (4) |
Se20—Se18—K3 | 122.3 (5) | Se6ii—K6—Se14ii | 125.78 (6) |
Se19—Se18—K3 | 56.0 (3) | Se13xiii—K6—Se14ii | 95.57 (5) |
Nb1—Se18—K3 | 95.69 (5) | Se11—K6—Se14ii | 156.04 (6) |
K1v—Se18—K3 | 80.81 (4) | Se16xiii—K7—Se6 | 162.28 (7) |
K3v—Se18—K3 | 103.66 (6) | Se16xiii—K7—Se3viii | 86.49 (5) |
Se20—Se18—K5 | 52.1 (5) | Se6—K7—Se3viii | 103.50 (5) |
Se19—Se18—K5 | 130.9 (3) | Se16xiii—K7—Se11 | 92.86 (5) |
Nb1—Se18—K5 | 94.78 (5) | Se6—K7—Se11 | 69.44 (4) |
K1v—Se18—K5 | 88.46 (4) | Se3viii—K7—Se11 | 128.37 (6) |
K3v—Se18—K5 | 81.03 (5) | Se16xiii—K7—Se17xiii | 94.88 (5) |
K3—Se18—K5 | 168.09 (6) | Se6—K7—Se17xiii | 87.60 (5) |
Se18—Se19—Se20 | 2.6 (2) | Se3viii—K7—Se17xiii | 137.50 (6) |
Se18—Se19—Nb1 | 62.9 (2) | Se11—K7—Se17xiii | 94.05 (5) |
Se20—Se19—Nb1 | 60.6 (2) | Se16xiii—K7—Se9 | 128.22 (6) |
Se18—Se19—K3v | 107.3 (3) | Se6—K7—Se9 | 45.04 (3) |
Se20—Se19—K3v | 108.7 (3) | Se3viii—K7—Se9 | 72.62 (4) |
Nb1—Se19—K3v | 107.3 (2) | Se11—K7—Se9 | 67.76 (4) |
Se18—Se19—K3 | 101.7 (3) | Se17xiii—K7—Se9 | 132.32 (6) |
Se20—Se19—K3 | 101.1 (3) | Se16xiii—K7—Se11viii | 123.57 (6) |
Nb1—Se19—K3 | 104.6 (2) | Se6—K7—Se11viii | 74.06 (4) |
K3v—Se19—K3 | 144.0 (3) | Se3viii—K7—Se11viii | 68.31 (4) |
Se18—Se19—K1v | 61.4 (2) | Se11—K7—Se11viii | 142.53 (6) |
Se20—Se19—K1v | 63.7 (2) | Se17xiii—K7—Se11viii | 76.00 (4) |
Nb1—Se19—K1v | 124.2 (2) | Se9—K7—Se11viii | 92.21 (5) |
K3v—Se19—K1v | 92.54 (17) | Se16xiii—K7—Se4xiii | 40.19 (3) |
K3—Se19—K1v | 82.83 (16) | Se6—K7—Se4xiii | 127.93 (6) |
Se18—Se20—Se19 | 3.9 (3) | Se3viii—K7—Se4xiii | 126.67 (6) |
Se18—Se20—Nb1 | 68.7 (4) | Se11—K7—Se4xiii | 68.88 (4) |
Se19—Se20—Nb1 | 65.2 (3) | Se17xiii—K7—Se4xiii | 65.86 (4) |
Se18—Se20—K5 | 115.0 (5) | Se9—K7—Se4xiii | 133.70 (6) |
Se19—Se20—K5 | 116.9 (3) | Se11viii—K7—Se4xiii | 133.05 (6) |
Symmetry codes: (i) −x−1, y, −z+1/2; (ii) −x+1/2, y−1/2, z; (iii) x+1/2, −y+1/2, −z; (iv) −x−1/2, y−1/2, z; (v) x−1/2, −y+1/2, −z; (vi) −x, −y, −z; (vii) x−1, y, z; (viii) −x+1/2, y+1/2, z; (ix) x−3/2, y+1/2, −z+1/2; (x) −x−1/2, y+1/2, z; (xi) x−1/2, 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, y−1/2, −z+1/2; (xvi) x+1/2, y−1/2, −z+1/2. |
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