The quaternary tantalum thiophosphate K4Ta4P4S24 (tetrapotassium tetratantalum tetraphosphorus tetracosasulfide) was obtained by reacting elemental Ta with a melt formed in situ of K2S3, P2S5 and S. The crystal structure exhibits [Ta4P4S24]4- anionic layers, which consist of dimeric Ta2S11 units interconnected by PS4 tetrahedra. The layers are stacked in an ABAB sequence in the direction of the crystallographic a axis and are separated by the K+ ions. The title compound is isostructural with A4Ta4P4S24 (A = Rb and Cs).
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (S-S) = 0.002 Å
- R factor = 0.027
- wR factor = 0.055
- Data-to-parameter ratio = 26.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT220_ALERT_2_B Large Non-Solvent S Ueq(max)/Ueq(min) ... 4.10 Ratio
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293
PLAT200_ALERT_1_C Check the Reported cell_ambient_temperature .... 293
PLAT213_ALERT_2_C Atom S23 has ADP max/min Ratio ............. 3.10 prolat
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: CIFTAB in SHELXTL (Bruker, 1998).
tetrapotassium tetratantalum tetraphosphorus tetracosasulfide
top
Crystal data top
K4P4S24Ta4 | F(000) = 3248 |
Mr = 1773.52 | Dx = 3.251 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8000 reflections |
a = 13.6193 (7) Å | θ = 3–28° |
b = 17.7307 (13) Å | µ = 14.07 mm−1 |
c = 15.8077 (9) Å | T = 293 K |
β = 108.356 (6)° | Polyhedron, orange |
V = 3623.0 (4) Å3 | 0.11 × 0.08 × 0.08 mm |
Z = 4 | |
Data collection top
Stoe IPDS diffractometer | 8610 independent reflections |
Radiation source: fine-focus sealed tube | 6878 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
φ scans | θmax = 28.0°, θmin = 2.3° |
Absorption correction: numerical [X-SHAPE (Stoe & Cie, 1998) and X-RED (Stoe & Cie, 1998)] | h = −17→17 |
Tmin = 0.261, Tmax = 0.314 | k = −23→23 |
34379 measured reflections | l = −20→20 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.027 | w = 1/[σ2(Fo2) + (0.029P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.055 | (Δ/σ)max = 0.002 |
S = 0.97 | Δρmax = 1.11 e Å−3 |
8610 reflections | Δρmin = −1.66 e Å−3 |
326 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.000392 (16) |
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 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 >
σ(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 | |
Ta1 | 0.749361 (16) | 0.381909 (12) | 0.250497 (13) | 0.00372 (5) | |
Ta2 | 0.638433 (16) | 0.217476 (12) | 0.297947 (13) | 0.00363 (5) | |
Ta3 | 0.708124 (17) | 0.217043 (12) | 0.727446 (13) | 0.00508 (5) | |
Ta4 | 0.670609 (16) | 0.383340 (12) | 0.825329 (13) | 0.00395 (5) | |
S1 | 0.89161 (11) | 0.47792 (8) | 0.28872 (9) | 0.0092 (3) | |
S2 | 0.68656 (11) | 0.47914 (8) | 0.33471 (9) | 0.0081 (3) | |
S3 | 0.66376 (11) | 0.45696 (8) | 0.09904 (8) | 0.0067 (2) | |
S4 | 0.86082 (11) | 0.34586 (8) | 0.15008 (8) | 0.0073 (3) | |
S5 | 0.63596 (11) | 0.27871 (8) | 0.15539 (8) | 0.0071 (2) | |
S6 | 0.56519 (11) | 0.34283 (8) | 0.22732 (9) | 0.0081 (3) | |
S7 | 0.82317 (11) | 0.29510 (8) | 0.35616 (8) | 0.0076 (3) | |
S8 | 0.76999 (11) | 0.13306 (7) | 0.25659 (8) | 0.0070 (3) | |
S9 | 0.50067 (11) | 0.15190 (8) | 0.22894 (9) | 0.0080 (3) | |
S10 | 0.71021 (11) | 0.13333 (7) | 0.43355 (8) | 0.0072 (3) | |
S11 | 0.58676 (12) | 0.28623 (8) | 0.41786 (9) | 0.0108 (3) | |
S12 | 0.57357 (12) | 0.16299 (9) | 0.57834 (9) | 0.0128 (3) | |
S13 | 0.78753 (11) | 0.25589 (8) | 0.60588 (9) | 0.0108 (3) | |
S14 | 0.83115 (12) | 0.11549 (8) | 0.72639 (11) | 0.0161 (3) | |
S15 | 0.65706 (11) | 0.11620 (8) | 0.81488 (9) | 0.0094 (3) | |
S16 | 0.55221 (11) | 0.27208 (8) | 0.75985 (8) | 0.0077 (3) | |
S17 | 0.82344 (11) | 0.28630 (8) | 0.83151 (8) | 0.0072 (2) | |
S18 | 0.59672 (11) | 0.33590 (8) | 0.66932 (8) | 0.0094 (3) | |
S19 | 0.78917 (11) | 0.45247 (8) | 0.75444 (9) | 0.0085 (3) | |
S20 | 0.54812 (11) | 0.46435 (8) | 0.81910 (10) | 0.0126 (3) | |
S21 | 0.66450 (11) | 0.30902 (8) | 0.96080 (8) | 0.0072 (3) | |
S22 | 0.80768 (11) | 0.44735 (8) | 0.95632 (8) | 0.0079 (3) | |
S23 | 0.87848 (13) | 0.59581 (9) | 0.45581 (9) | 0.0159 (3) | |
S24 | 0.87992 (15) | 0.02350 (11) | 0.92788 (11) | 0.0275 (4) | |
P1 | 0.80587 (11) | 0.55310 (8) | 0.33728 (8) | 0.0060 (3) | |
P2 | 0.66354 (11) | 0.20910 (8) | 0.51089 (9) | 0.0071 (3) | |
P3 | 0.78129 (11) | 0.04852 (8) | 0.81097 (9) | 0.0086 (3) | |
P4 | 0.75056 (11) | 0.39181 (8) | 1.04315 (8) | 0.0045 (2) | |
K1 | 0.98546 (11) | 0.51484 (9) | 0.12887 (9) | 0.0198 (3) | |
K2 | 0.84434 (14) | 0.17688 (10) | 1.01838 (11) | 0.0336 (4) | |
K3 | 0.84364 (17) | 0.42843 (10) | 0.54026 (10) | 0.0369 (4) | |
K4 | 0.44796 (12) | 0.37458 (10) | 0.96640 (12) | 0.0302 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ta1 | 0.00630 (11) | 0.00296 (10) | 0.00204 (9) | 0.00018 (8) | 0.00151 (8) | 0.00032 (7) |
Ta2 | 0.00559 (11) | 0.00343 (10) | 0.00206 (9) | −0.00026 (8) | 0.00150 (8) | 0.00023 (7) |
Ta3 | 0.00829 (11) | 0.00513 (11) | 0.00234 (9) | −0.00191 (8) | 0.00240 (8) | −0.00156 (7) |
Ta4 | 0.00516 (11) | 0.00385 (10) | 0.00200 (9) | 0.00019 (8) | −0.00006 (8) | −0.00017 (7) |
S1 | 0.0089 (7) | 0.0065 (6) | 0.0136 (6) | −0.0011 (5) | 0.0055 (5) | −0.0026 (5) |
S2 | 0.0125 (7) | 0.0062 (6) | 0.0078 (6) | −0.0010 (5) | 0.0065 (5) | −0.0007 (5) |
S3 | 0.0106 (7) | 0.0063 (6) | 0.0041 (5) | 0.0030 (5) | 0.0036 (5) | 0.0005 (5) |
S4 | 0.0074 (7) | 0.0099 (7) | 0.0043 (5) | 0.0031 (5) | 0.0012 (5) | −0.0001 (5) |
S5 | 0.0106 (7) | 0.0063 (6) | 0.0035 (5) | −0.0010 (5) | 0.0011 (5) | −0.0002 (5) |
S6 | 0.0078 (7) | 0.0069 (6) | 0.0100 (6) | 0.0009 (5) | 0.0036 (5) | 0.0016 (5) |
S7 | 0.0091 (7) | 0.0056 (6) | 0.0060 (6) | 0.0005 (5) | −0.0004 (5) | 0.0024 (5) |
S8 | 0.0085 (7) | 0.0054 (6) | 0.0069 (6) | −0.0004 (5) | 0.0021 (5) | −0.0023 (5) |
S9 | 0.0068 (7) | 0.0083 (6) | 0.0075 (6) | −0.0021 (5) | 0.0004 (5) | 0.0004 (5) |
S10 | 0.0116 (7) | 0.0070 (6) | 0.0033 (5) | 0.0011 (5) | 0.0025 (5) | 0.0007 (5) |
S11 | 0.0144 (7) | 0.0106 (7) | 0.0089 (6) | 0.0021 (5) | 0.0058 (5) | −0.0008 (5) |
S12 | 0.0167 (8) | 0.0177 (8) | 0.0069 (6) | −0.0122 (6) | 0.0080 (6) | −0.0062 (5) |
S13 | 0.0123 (7) | 0.0149 (7) | 0.0052 (6) | −0.0090 (6) | 0.0028 (5) | −0.0020 (5) |
S14 | 0.0197 (8) | 0.0060 (7) | 0.0309 (8) | −0.0006 (6) | 0.0202 (7) | −0.0003 (6) |
S15 | 0.0119 (7) | 0.0093 (7) | 0.0094 (6) | 0.0019 (5) | 0.0066 (5) | 0.0015 (5) |
S16 | 0.0082 (7) | 0.0091 (7) | 0.0049 (5) | −0.0018 (5) | 0.0009 (5) | −0.0011 (5) |
S17 | 0.0064 (6) | 0.0075 (6) | 0.0057 (5) | −0.0005 (5) | −0.0008 (5) | −0.0028 (5) |
S18 | 0.0123 (7) | 0.0098 (7) | 0.0039 (5) | −0.0007 (5) | −0.0008 (5) | 0.0005 (5) |
S19 | 0.0091 (7) | 0.0069 (6) | 0.0098 (6) | 0.0013 (5) | 0.0032 (5) | 0.0029 (5) |
S20 | 0.0090 (7) | 0.0086 (7) | 0.0202 (7) | 0.0042 (5) | 0.0047 (6) | 0.0021 (5) |
S21 | 0.0112 (7) | 0.0062 (6) | 0.0037 (5) | −0.0031 (5) | 0.0015 (5) | −0.0012 (5) |
S22 | 0.0110 (7) | 0.0093 (6) | 0.0039 (5) | −0.0054 (5) | 0.0031 (5) | −0.0022 (5) |
S23 | 0.0277 (9) | 0.0130 (7) | 0.0040 (6) | −0.0049 (6) | 0.0008 (6) | −0.0026 (5) |
S24 | 0.0277 (10) | 0.0290 (10) | 0.0143 (7) | 0.0137 (8) | −0.0097 (7) | −0.0066 (7) |
P1 | 0.0111 (7) | 0.0042 (6) | 0.0029 (6) | −0.0004 (5) | 0.0025 (5) | −0.0003 (5) |
P2 | 0.0100 (7) | 0.0093 (7) | 0.0030 (6) | −0.0042 (5) | 0.0034 (5) | −0.0025 (5) |
P3 | 0.0090 (7) | 0.0087 (7) | 0.0080 (6) | 0.0006 (5) | 0.0024 (5) | −0.0012 (5) |
P4 | 0.0056 (7) | 0.0053 (6) | 0.0023 (5) | −0.0010 (5) | 0.0009 (5) | −0.0008 (5) |
K1 | 0.0137 (7) | 0.0273 (8) | 0.0167 (6) | −0.0024 (6) | 0.0022 (5) | −0.0108 (6) |
K2 | 0.0350 (10) | 0.0271 (9) | 0.0275 (8) | 0.0123 (7) | −0.0061 (7) | −0.0090 (7) |
K3 | 0.0626 (13) | 0.0231 (9) | 0.0208 (7) | 0.0038 (8) | 0.0073 (8) | 0.0116 (6) |
K4 | 0.0106 (8) | 0.0293 (9) | 0.0464 (9) | 0.0007 (6) | 0.0029 (7) | 0.0022 (7) |
Geometric parameters (Å, º) top
Ta1—S7 | 2.2610 (13) | S14—P3 | 2.057 (2) |
Ta1—S2 | 2.4885 (13) | S15—P3 | 2.091 (2) |
Ta1—S1 | 2.5057 (14) | S15—K2 | 3.584 (2) |
Ta1—S6 | 2.5153 (14) | S16—S18 | 2.0597 (18) |
Ta1—S5 | 2.5556 (14) | S17—K2 | 3.470 (2) |
Ta1—S4 | 2.5981 (13) | S18—K2v | 3.520 (2) |
Ta1—S3 | 2.6653 (13) | S19—P3vii | 2.065 (2) |
Ta2—S9 | 2.1847 (14) | S19—K1viii | 3.097 (2) |
Ta2—S5 | 2.4922 (12) | S19—K3 | 3.712 (2) |
Ta2—S11 | 2.5326 (13) | S20—K4 | 3.438 (2) |
Ta2—S10 | 2.5411 (13) | S21—P4 | 2.0644 (19) |
Ta2—S6 | 2.5455 (14) | S21—K4 | 3.197 (2) |
Ta2—S8 | 2.5721 (13) | S21—K2 | 3.303 (2) |
Ta2—S7 | 2.7592 (14) | S22—P4 | 2.0326 (18) |
Ta3—S17 | 2.2479 (13) | S22—K1ix | 3.2519 (19) |
Ta3—S14 | 2.4632 (15) | S22—K1viii | 3.5481 (19) |
Ta3—S15 | 2.4892 (14) | S23—P1 | 1.9736 (19) |
Ta3—S16 | 2.5316 (14) | S23—K3 | 3.349 (2) |
Ta3—S13 | 2.5780 (13) | S23—K2vii | 3.496 (3) |
Ta3—S18 | 2.5903 (14) | S23—K3viii | 3.790 (3) |
Ta3—S12 | 2.6668 (14) | S24—P3 | 1.963 (2) |
Ta4—S20 | 2.1800 (14) | S24—K2 | 3.180 (2) |
Ta4—S18 | 2.4978 (13) | S24—K3x | 3.651 (3) |
Ta4—S21 | 2.5379 (13) | P1—S8xi | 2.0769 (19) |
Ta4—S19 | 2.5505 (13) | P1—K3 | 3.796 (2) |
Ta4—S16 | 2.5518 (14) | P3—S19x | 2.065 (2) |
Ta4—S22 | 2.5741 (14) | P3—K2 | 3.859 (2) |
Ta4—S17 | 2.6785 (14) | P4—S3ix | 2.0421 (18) |
S1—P1 | 2.0722 (19) | P4—S4ix | 2.0438 (19) |
S1—K1 | 3.2377 (19) | P4—K1ix | 3.755 (2) |
S2—P1 | 2.079 (2) | K1—S19viii | 3.097 (2) |
S2—K3 | 3.401 (2) | K1—S22i | 3.2519 (19) |
S3—P4i | 2.0421 (18) | K1—S9xi | 3.2751 (19) |
S3—K4i | 3.360 (2) | K1—S10xi | 3.291 (2) |
S3—K4ii | 3.364 (2) | K1—S22viii | 3.5481 (19) |
S4—P4i | 2.0438 (19) | K1—S12iii | 3.553 (2) |
S4—K1 | 3.511 (2) | K1—P4i | 3.755 (2) |
S4—K2i | 3.615 (2) | K1—K1xii | 4.248 (3) |
S5—S6 | 2.0505 (18) | K2—S23x | 3.496 (3) |
S5—K4i | 3.681 (2) | K2—S18xiii | 3.520 (2) |
S7—K4iii | 3.621 (2) | K2—S4ix | 3.615 (2) |
S7—K3 | 3.691 (2) | K2—K3x | 5.032 (3) |
S8—P1iv | 2.0769 (19) | K3—S9xiii | 3.388 (2) |
S8—K4iii | 3.440 (2) | K3—S24vii | 3.651 (3) |
S9—K1iv | 3.2751 (19) | K3—S23viii | 3.790 (3) |
S9—K3v | 3.388 (2) | K3—K2vii | 5.032 (3) |
S10—P2 | 2.0477 (18) | K4—S10vi | 3.117 (2) |
S10—K4iii | 3.117 (2) | K4—S3ix | 3.360 (2) |
S10—K1iv | 3.291 (2) | K4—S3ii | 3.364 (2) |
S11—P2 | 2.039 (2) | K4—S8vi | 3.440 (2) |
S12—P2 | 2.0321 (18) | K4—S7vi | 3.621 (2) |
S12—K1vi | 3.553 (2) | K4—S5ix | 3.681 (2) |
S13—P2 | 2.049 (2) | K4—K4xiv | 4.687 (3) |
S13—K3 | 3.394 (2) | | |
| | | |
S7—Ta1—S2 | 102.96 (5) | P3vii—S19—K3 | 80.38 (6) |
S7—Ta1—S1 | 98.87 (5) | Ta4—S19—K3 | 132.97 (6) |
S2—Ta1—S1 | 76.72 (4) | K1viii—S19—K3 | 96.86 (5) |
S7—Ta1—S6 | 96.37 (5) | Ta4—S20—K4 | 97.21 (5) |
S2—Ta1—S6 | 76.93 (4) | P4—S21—Ta4 | 90.00 (6) |
S1—Ta1—S6 | 151.89 (5) | P4—S21—K4 | 93.99 (7) |
S7—Ta1—S5 | 89.59 (5) | Ta4—S21—K4 | 96.33 (5) |
S2—Ta1—S5 | 124.39 (4) | P4—S21—K2 | 96.09 (7) |
S1—Ta1—S5 | 155.01 (4) | Ta4—S21—K2 | 112.47 (6) |
S6—Ta1—S5 | 47.69 (4) | K4—S21—K2 | 149.38 (6) |
S7—Ta1—S4 | 94.27 (4) | P4—S22—Ta4 | 89.70 (6) |
S2—Ta1—S4 | 149.61 (4) | P4—S22—K1ix | 87.37 (6) |
S1—Ta1—S4 | 76.02 (4) | Ta4—S22—K1ix | 175.40 (6) |
S6—Ta1—S4 | 126.22 (4) | P4—S22—K1viii | 150.03 (8) |
S5—Ta1—S4 | 79.95 (4) | Ta4—S22—K1viii | 103.85 (4) |
S7—Ta1—S3 | 166.03 (4) | K1ix—S22—K1viii | 77.19 (4) |
S2—Ta1—S3 | 90.45 (4) | P1—S23—K3 | 86.96 (7) |
S1—Ta1—S3 | 87.92 (4) | P1—S23—K2vii | 94.29 (8) |
S6—Ta1—S3 | 82.69 (4) | K3—S23—K2vii | 94.63 (6) |
S5—Ta1—S3 | 79.43 (4) | P1—S23—K3viii | 99.86 (7) |
S4—Ta1—S3 | 75.43 (4) | K3—S23—K3viii | 99.15 (6) |
S9—Ta2—S5 | 90.88 (5) | K2vii—S23—K3viii | 160.69 (6) |
S9—Ta2—S11 | 103.44 (5) | P3—S24—K2 | 94.26 (8) |
S5—Ta2—S11 | 122.63 (5) | P3—S24—K3x | 83.17 (8) |
S9—Ta2—S10 | 98.66 (5) | K2—S24—K3x | 94.64 (7) |
S5—Ta2—S10 | 155.60 (4) | S23—P1—S1 | 115.22 (9) |
S11—Ta2—S10 | 77.00 (4) | S23—P1—S8xi | 113.84 (9) |
S9—Ta2—S6 | 95.13 (5) | S1—P1—S8xi | 112.71 (8) |
S5—Ta2—S6 | 48.02 (4) | S23—P1—S2 | 114.55 (8) |
S11—Ta2—S6 | 75.23 (4) | S1—P1—S2 | 96.61 (8) |
S10—Ta2—S6 | 151.18 (4) | S8xi—P1—S2 | 101.93 (8) |
S9—Ta2—S8 | 96.94 (5) | S12—P2—S11 | 113.03 (9) |
S5—Ta2—S8 | 80.55 (4) | S12—P2—S10 | 113.65 (9) |
S11—Ta2—S8 | 148.24 (5) | S11—P2—S10 | 101.22 (7) |
S10—Ta2—S8 | 76.05 (4) | S12—P2—S13 | 105.81 (8) |
S6—Ta2—S8 | 127.21 (4) | S11—P2—S13 | 111.97 (9) |
S9—Ta2—S7 | 168.97 (4) | S10—P2—S13 | 111.35 (9) |
S5—Ta2—S7 | 80.53 (4) | S24—P3—S14 | 118.31 (11) |
S11—Ta2—S7 | 87.10 (4) | S24—P3—S19x | 110.93 (10) |
S10—Ta2—S7 | 86.75 (4) | S14—P3—S19x | 110.31 (8) |
S6—Ta2—S7 | 84.32 (4) | S24—P3—S15 | 114.96 (9) |
S8—Ta2—S7 | 74.93 (4) | S14—P3—S15 | 97.11 (8) |
S17—Ta3—S14 | 94.84 (5) | S19x—P3—S15 | 103.61 (9) |
S17—Ta3—S15 | 103.83 (5) | S22—P4—S3ix | 114.51 (9) |
S14—Ta3—S15 | 77.78 (5) | S22—P4—S4ix | 114.45 (9) |
S17—Ta3—S16 | 94.51 (5) | S3ix—P4—S4ix | 104.02 (7) |
S14—Ta3—S16 | 154.01 (5) | S22—P4—S21 | 100.41 (7) |
S15—Ta3—S16 | 76.45 (4) | S3ix—P4—S21 | 112.58 (8) |
S17—Ta3—S13 | 92.24 (5) | S4ix—P4—S21 | 111.19 (8) |
S14—Ta3—S13 | 75.19 (5) | S19viii—K1—S1 | 97.69 (5) |
S15—Ta3—S13 | 149.54 (5) | S19viii—K1—S22i | 154.80 (6) |
S16—Ta3—S13 | 128.56 (5) | S1—K1—S22i | 101.98 (5) |
S17—Ta3—S18 | 90.65 (5) | S19viii—K1—S9xi | 67.68 (4) |
S14—Ta3—S18 | 156.35 (4) | S1—K1—S9xi | 64.28 (4) |
S15—Ta3—S18 | 123.13 (5) | S22i—K1—S9xi | 135.68 (6) |
S16—Ta3—S18 | 47.41 (4) | S19viii—K1—S10xi | 128.03 (6) |
S13—Ta3—S18 | 81.64 (5) | S1—K1—S10xi | 83.20 (5) |
S17—Ta3—S12 | 166.01 (5) | S22i—K1—S10xi | 70.41 (5) |
S14—Ta3—S12 | 90.62 (5) | S9xi—K1—S10xi | 66.32 (4) |
S15—Ta3—S12 | 89.90 (5) | S19viii—K1—S4 | 121.40 (6) |
S16—Ta3—S12 | 86.02 (4) | S1—K1—S4 | 55.34 (4) |
S13—Ta3—S12 | 76.70 (4) | S22i—K1—S4 | 60.75 (4) |
S18—Ta3—S12 | 79.41 (5) | S9xi—K1—S4 | 119.52 (5) |
S20—Ta4—S18 | 96.47 (5) | S10xi—K1—S4 | 101.72 (5) |
S20—Ta4—S21 | 98.76 (5) | S19viii—K1—S22viii | 55.55 (4) |
S18—Ta4—S21 | 123.24 (5) | S1—K1—S22viii | 152.90 (6) |
S20—Ta4—S19 | 104.17 (5) | S22i—K1—S22viii | 102.81 (4) |
S18—Ta4—S19 | 80.91 (5) | S9xi—K1—S22viii | 103.84 (5) |
S21—Ta4—S19 | 144.46 (5) | S10xi—K1—S22viii | 115.49 (5) |
S20—Ta4—S16 | 96.56 (5) | S4—K1—S22viii | 131.53 (5) |
S18—Ta4—S16 | 48.13 (4) | S19viii—K1—S12iii | 87.62 (5) |
S21—Ta4—S16 | 75.90 (4) | S1—K1—S12iii | 103.90 (5) |
S19—Ta4—S16 | 126.86 (4) | S22i—K1—S12iii | 72.53 (5) |
S20—Ta4—S22 | 95.54 (5) | S9xi—K1—S12iii | 149.57 (6) |
S18—Ta4—S22 | 155.14 (4) | S10xi—K1—S12iii | 142.93 (5) |
S21—Ta4—S22 | 76.02 (4) | S4—K1—S12iii | 58.12 (4) |
S19—Ta4—S22 | 75.07 (4) | S22viii—K1—S12iii | 73.60 (4) |
S16—Ta4—S22 | 150.77 (4) | S24—K2—S21 | 133.42 (6) |
S20—Ta4—S17 | 178.65 (5) | S24—K2—S17 | 94.50 (6) |
S18—Ta4—S17 | 83.48 (4) | S21—K2—S17 | 60.92 (4) |
S21—Ta4—S17 | 82.37 (4) | S24—K2—S23x | 87.81 (6) |
S19—Ta4—S17 | 74.49 (4) | S21—K2—S23x | 74.23 (5) |
S16—Ta4—S17 | 84.42 (4) | S17—K2—S23x | 119.19 (6) |
S22—Ta4—S17 | 84.00 (4) | S24—K2—S18xiii | 89.73 (6) |
P1—S1—Ta1 | 92.48 (6) | S21—K2—S18xiii | 135.50 (6) |
P1—S1—K1 | 124.47 (7) | S17—K2—S18xiii | 114.45 (6) |
Ta1—S1—K1 | 114.49 (5) | S23x—K2—S18xiii | 126.34 (6) |
P1—S2—Ta1 | 92.82 (6) | S24—K2—S15 | 60.38 (5) |
P1—S2—K3 | 84.00 (7) | S21—K2—S15 | 73.10 (5) |
Ta1—S2—K3 | 96.27 (5) | S17—K2—S15 | 63.85 (4) |
P4i—S3—Ta1 | 87.55 (6) | S23x—K2—S15 | 65.34 (4) |
P4i—S3—K4i | 89.77 (6) | S18xiii—K2—S15 | 148.88 (6) |
Ta1—S3—K4i | 113.13 (5) | S24—K2—S4ix | 167.75 (7) |
P4i—S3—K4ii | 129.54 (7) | S21—K2—S4ix | 58.47 (4) |
Ta1—S3—K4ii | 138.34 (5) | S17—K2—S4ix | 90.03 (5) |
K4i—S3—K4ii | 88.40 (5) | S23x—K2—S4ix | 99.92 (5) |
P4i—S4—Ta1 | 89.36 (6) | S18xiii—K2—S4ix | 78.04 (5) |
P4i—S4—K1 | 80.34 (6) | S15—K2—S4ix | 131.55 (6) |
Ta1—S4—K1 | 103.97 (5) | S23—K3—S9xiii | 126.45 (7) |
P4i—S4—K2i | 87.59 (6) | S23—K3—S13 | 174.00 (7) |
Ta1—S4—K2i | 127.85 (6) | S9xiii—K3—S13 | 59.50 (4) |
K1—S4—K2i | 126.61 (5) | S23—K3—S2 | 60.68 (4) |
S6—S5—Ta2 | 67.35 (5) | S9xiii—K3—S2 | 170.04 (7) |
S6—S5—Ta1 | 65.12 (5) | S13—K3—S2 | 113.32 (6) |
Ta2—S5—Ta1 | 86.93 (4) | S23—K3—S24vii | 82.81 (6) |
S6—S5—K4i | 82.29 (6) | S9xiii—K3—S24vii | 113.28 (6) |
Ta2—S5—K4i | 137.98 (5) | S13—K3—S24vii | 95.52 (6) |
Ta1—S5—K4i | 106.49 (5) | S2—K3—S24vii | 73.07 (5) |
S5—S6—Ta1 | 67.18 (5) | S23—K3—S7 | 103.79 (5) |
S5—S6—Ta2 | 64.63 (5) | S9xiii—K3—S7 | 107.14 (6) |
Ta1—S6—Ta2 | 86.65 (4) | S13—K3—S7 | 72.26 (5) |
Ta1—S7—Ta2 | 86.94 (4) | S2—K3—S7 | 63.09 (4) |
Ta1—S7—K4iii | 162.42 (6) | S24vii—K3—S7 | 123.04 (6) |
Ta2—S7—K4iii | 89.23 (4) | S23—K3—S19 | 110.86 (6) |
Ta1—S7—K3 | 92.98 (5) | S9xiii—K3—S19 | 59.83 (4) |
Ta2—S7—K3 | 114.64 (5) | S13—K3—S19 | 72.29 (4) |
K4iii—S7—K3 | 104.20 (5) | S2—K3—S19 | 126.51 (7) |
P1iv—S8—Ta2 | 110.44 (7) | S24vii—K3—S19 | 53.58 (4) |
P1iv—S8—K4iii | 134.67 (7) | S7—K3—S19 | 143.66 (6) |
Ta2—S8—K4iii | 96.52 (5) | S23—K3—S23viii | 80.85 (6) |
Ta2—S9—K1iv | 101.38 (5) | S9xiii—K3—S23viii | 65.65 (5) |
Ta2—S9—K3v | 150.23 (6) | S13—K3—S23viii | 102.27 (6) |
K1iv—S9—K3v | 100.15 (5) | S2—K3—S23viii | 111.72 (5) |
P2—S10—Ta2 | 90.52 (6) | S24vii—K3—S23viii | 157.21 (7) |
P2—S10—K4iii | 115.57 (8) | S7—K3—S23viii | 76.55 (5) |
Ta2—S10—K4iii | 105.69 (5) | S19—K3—S23viii | 118.91 (6) |
P2—S10—K1iv | 102.91 (7) | S10vi—K4—S21 | 153.90 (7) |
Ta2—S10—K1iv | 93.54 (5) | S10vi—K4—S3ix | 141.47 (7) |
K4iii—S10—K1iv | 136.21 (6) | S21—K4—S3ix | 62.74 (4) |
P2—S11—Ta2 | 90.96 (6) | S10vi—K4—S3ii | 69.09 (5) |
P2—S12—Ta3 | 87.65 (6) | S21—K4—S3ii | 130.25 (6) |
P2—S12—K1vi | 141.00 (8) | S3ix—K4—S3ii | 91.60 (5) |
Ta3—S12—K1vi | 107.88 (5) | S10vi—K4—S20 | 121.40 (6) |
P2—S13—Ta3 | 89.75 (6) | S21—K4—S20 | 65.37 (5) |
P2—S13—K3 | 110.73 (7) | S3ix—K4—S20 | 76.45 (5) |
Ta3—S13—K3 | 131.02 (6) | S3ii—K4—S20 | 67.55 (5) |
P3—S14—Ta3 | 93.04 (6) | S10vi—K4—S8vi | 57.18 (4) |
P3—S15—Ta3 | 91.47 (6) | S21—K4—S8vi | 109.58 (6) |
P3—S15—K2 | 81.09 (7) | S3ix—K4—S8vi | 146.23 (6) |
Ta3—S15—K2 | 92.20 (5) | S3ii—K4—S8vi | 67.99 (5) |
S18—S16—Ta3 | 67.79 (5) | S20—K4—S8vi | 71.01 (5) |
S18—S16—Ta4 | 64.56 (5) | S10vi—K4—S7vi | 64.97 (4) |
Ta3—S16—Ta4 | 85.23 (4) | S21—K4—S7vi | 88.96 (5) |
Ta3—S17—Ta4 | 88.19 (5) | S3ix—K4—S7vi | 147.93 (6) |
Ta3—S17—K2 | 99.71 (5) | S3ii—K4—S7vi | 119.44 (6) |
Ta4—S17—K2 | 104.16 (5) | S20—K4—S7vi | 106.56 (6) |
S16—S18—Ta4 | 67.31 (5) | S8vi—K4—S7vi | 54.67 (4) |
S16—S18—Ta3 | 64.80 (5) | S10vi—K4—S5ix | 122.34 (6) |
Ta4—S18—Ta3 | 85.12 (4) | S21—K4—S5ix | 56.13 (4) |
S16—S18—K2v | 89.85 (7) | S3ix—K4—S5ix | 56.36 (4) |
Ta4—S18—K2v | 134.00 (6) | S3ii—K4—S5ix | 142.30 (6) |
Ta3—S18—K2v | 121.73 (6) | S20—K4—S5ix | 116.14 (5) |
P3vii—S19—Ta4 | 110.95 (7) | S8vi—K4—S5ix | 149.68 (6) |
P3vii—S19—K1viii | 111.15 (8) | S7vi—K4—S5ix | 96.20 (5) |
Ta4—S19—K1viii | 118.29 (5) | | |
Symmetry codes: (i) x, y, z−1; (ii) −x+1, −y+1, −z+1; (iii) x+1/2, −y+1/2, z−1/2; (iv) −x+3/2, y−1/2, −z+1/2; (v) x−1/2, −y+1/2, z−1/2; (vi) x−1/2, −y+1/2, z+1/2; (vii) −x+3/2, y+1/2, −z+3/2; (viii) −x+2, −y+1, −z+1; (ix) x, y, z+1; (x) −x+3/2, y−1/2, −z+3/2; (xi) −x+3/2, y+1/2, −z+1/2; (xii) −x+2, −y+1, −z; (xiii) x+1/2, −y+1/2, z+1/2; (xiv) −x+1, −y+1, −z+2. |