In order to clarify the polymorphism in the lithium sulfate family, LiREx(NH4)1 − xSO4 (0.5 ≤ x ≤ 4.0 mol%, nominal value; RE = Er3+, Yb3+ and Dy3+) crystals were grown from aqueous solution by slow evaporation between 298 and 313 K. The doping of the samples allowed us to obtain two polymorphic forms, α and β, of LiNH4SO4 (LAS). By means of X-ray diffraction (XRD) in single crystals, we determined the crystal structures of two new α-polytypes, which we have named α1- and α2-LAS. They present the same space group P21/c and the following relation among their lattice parameters: a2 = −c1, b2 = −b1, c2 = −2a1 − c1. In order to evaluate the stability of the new α-polytypes, we performed thermal analysis, X-ray diffraction and dielectric spectroscopy on single crystals and polycrystalline samples over the cyclic temperature range: 190 → 575 → 190 K. The results obtained by all the techniques used in this study demonstrate that α-polytypes are stable across a wide range of temperatures and they show an irreversible phase transition to the paraelectric β-phase above 500 K. In addition, a comparative study of α- and β-polytypes shows that both polymorphic structures have a common axis, with a possible intergrowth that facilitates their coexistence and promotes the reconstructive α → β transition. This intergrowth was related to small anomalies detected between 240 and 260 K, in crystals with an α-habit.
Supporting information
CCDC references: 1519626; 1530426
For both compounds, program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2014). Molecular graphics: Diamond 4.0 for alpha1_LAS.
Crystal data top
O4SYb0.005·0.984(H4N)·Li | F(000) = 497 |
Mr = 121.54 | Dx = 1.836 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 17.856 (8) Å | Cell parameters from 25 reflections |
b = 5.008 (3) Å | θ = 9–21° |
c = 10.264 (13) Å | µ = 0.73 mm−1 |
β = 106.46 (5)° | T = 293 K |
V = 880.2 (13) Å3 | Prism, colourless |
Z = 8 | 0.18 × 0.14 × 0.09 mm |
Data collection top
ENRAF-NONIUS CAD4 diffractometer | θmax = 30.0°, θmin = 2.4° |
ω/2Θ–scan | h = −25→0 |
4811 measured reflections | k = −7→7 |
2549 independent reflections | l = −13→14 |
2020 reflections with I > 2σ(I) | 3 standard reflections every 120 min |
Rint = 0.131 | intensity decay: none |
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)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.143 | Only H-atom coordinates refined |
S = 1.17 | w = 1/[σ2(Fo2) + (0.0484P)2 + 0.6832P] where P = (Fo2 + 2Fc2)/3 |
2549 reflections | (Δ/σ)max < 0.001 |
153 parameters | Δρmax = 1.05 e Å−3 |
74 restraints | Δρmin = −0.68 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) |
S1 | 0.40189 (3) | 0.78809 (13) | 0.35009 (6) | 0.01614 (17) | |
O11 | 0.40752 (12) | 0.7062 (5) | 0.4897 (2) | 0.0276 (5) | |
O12 | 0.41093 (12) | 1.0821 (4) | 0.3465 (2) | 0.0309 (5) | |
O13 | 0.32607 (11) | 0.7155 (5) | 0.2583 (2) | 0.0364 (6) | |
O14 | 0.46492 (11) | 0.6618 (4) | 0.3038 (2) | 0.0240 (4) | |
S2 | 0.09813 (3) | 0.28838 (12) | 0.44726 (6) | 0.01509 (16) | |
O21 | 0.09248 (11) | 0.2049 (5) | 0.58194 (19) | 0.0265 (4) | |
O22 | 0.08937 (11) | 0.5822 (4) | 0.4341 (2) | 0.0285 (5) | |
O23 | 0.03490 (10) | 0.1605 (4) | 0.33889 (18) | 0.0220 (4) | |
O24 | 0.17400 (11) | 0.2124 (5) | 0.4303 (2) | 0.0339 (5) | |
Yb1 | 0.33292 (13) | 0.2738 (5) | 0.0677 (3) | 0.0311 (11) | 0.0051 (12) |
N1 | 0.33292 (13) | 0.2738 (5) | 0.0677 (3) | 0.0311 (11) | 0.985 (4) |
H11 | 0.2772 (6) | 0.290 (6) | 0.031 (3) | 0.047* | 0.985 (4) |
H12 | 0.3512 (16) | 0.137 (5) | 0.016 (3) | 0.047* | 0.985 (4) |
H13 | 0.3573 (15) | 0.439 (4) | 0.055 (3) | 0.047* | 0.985 (4) |
H14 | 0.3461 (17) | 0.224 (6) | 0.1612 (13) | 0.047* | 0.985 (4) |
Yb2 | 0.16725 (13) | 0.7751 (5) | 0.2335 (3) | 0.0306 (10) | 0.0054 (12) |
N2 | 0.16725 (13) | 0.7751 (5) | 0.2335 (3) | 0.0306 (10) | 0.984 (4) |
H21 | 0.2230 (6) | 0.773 (6) | 0.255 (3) | 0.046* | 0.984 (4) |
H22 | 0.1446 (16) | 0.660 (5) | 0.157 (2) | 0.046* | 0.984 (4) |
H23 | 0.1509 (17) | 0.713 (6) | 0.310 (2) | 0.046* | 0.984 (4) |
H24 | 0.1476 (16) | 0.953 (3) | 0.209 (3) | 0.046* | 0.984 (4) |
Li1 | 0.0011 (2) | 0.2967 (10) | 0.1505 (5) | 0.0202 (8) | |
Li2 | 0.5016 (2) | 0.2965 (10) | 0.3519 (5) | 0.0226 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
S1 | 0.0186 (3) | 0.0195 (3) | 0.0119 (3) | 0.0004 (2) | 0.00700 (19) | 0.0006 (2) |
O11 | 0.0352 (9) | 0.0369 (12) | 0.0142 (8) | 0.0014 (8) | 0.0125 (7) | 0.0070 (10) |
O12 | 0.0404 (10) | 0.0197 (9) | 0.0394 (13) | 0.0025 (8) | 0.0223 (9) | 0.0033 (10) |
O13 | 0.0224 (8) | 0.0535 (15) | 0.0296 (11) | −0.0027 (9) | 0.0015 (7) | −0.0163 (12) |
O14 | 0.0313 (8) | 0.0232 (10) | 0.0235 (9) | 0.0072 (7) | 0.0178 (7) | 0.0024 (9) |
S2 | 0.0180 (3) | 0.0167 (3) | 0.0109 (3) | −0.00004 (19) | 0.00455 (18) | 0.0003 (2) |
O21 | 0.0346 (9) | 0.0341 (11) | 0.0116 (8) | −0.0002 (8) | 0.0076 (7) | 0.0051 (9) |
O22 | 0.0368 (10) | 0.0144 (9) | 0.0292 (11) | −0.0016 (7) | 0.0009 (8) | 0.0019 (9) |
O23 | 0.0282 (8) | 0.0196 (9) | 0.0152 (8) | −0.0050 (7) | 0.0012 (6) | −0.0003 (8) |
O24 | 0.0214 (8) | 0.0491 (14) | 0.0339 (12) | 0.0053 (8) | 0.0122 (8) | −0.0118 (11) |
Yb1 | 0.0309 (14) | 0.0371 (16) | 0.0259 (15) | 0.0004 (9) | 0.0087 (8) | 0.0005 (11) |
N1 | 0.0309 (14) | 0.0371 (16) | 0.0259 (15) | 0.0004 (9) | 0.0087 (8) | 0.0005 (11) |
Yb2 | 0.0344 (14) | 0.0325 (15) | 0.0266 (15) | −0.0006 (9) | 0.0113 (9) | −0.0024 (11) |
N2 | 0.0344 (14) | 0.0325 (15) | 0.0266 (15) | −0.0006 (9) | 0.0113 (9) | −0.0024 (11) |
Li1 | 0.0261 (18) | 0.021 (2) | 0.0142 (19) | 0.0014 (16) | 0.0060 (15) | −0.0006 (19) |
Li2 | 0.0269 (19) | 0.023 (2) | 0.020 (2) | 0.0022 (17) | 0.0094 (16) | 0.004 (2) |
Geometric parameters (Å, º) top
S1—O13 | 1.459 (2) | Yb1—Li2 | 3.551 (6) |
S1—O11 | 1.466 (3) | Yb1—Li2xi | 3.707 (5) |
S1—O14 | 1.482 (2) | Yb1—Li2i | 3.858 (5) |
S1—O12 | 1.483 (2) | Yb1—H11 | 0.962 (9) |
S1—Li2 | 3.035 (5) | Yb1—H12 | 0.976 (9) |
S1—Li2i | 3.049 (5) | Yb1—H13 | 0.963 (9) |
O11—Li2ii | 1.945 (5) | Yb1—H14 | 0.954 (9) |
O11—Yb1iii | 2.966 (4) | Yb2—O24iv | 2.958 (4) |
O12—Li2iv | 1.930 (5) | Yb2—O21ix | 2.967 (4) |
O12—Yb1iv | 2.965 (5) | Yb2—O22x | 3.077 (5) |
O12—Yb1v | 3.067 (4) | Yb2—Li1vii | 3.534 (5) |
O13—Yb2 | 2.791 (3) | Yb2—Li1 | 3.720 (5) |
O13—Yb1 | 2.978 (4) | Yb2—Li1iv | 3.863 (5) |
O14—Li2 | 1.958 (5) | Yb2—H21 | 0.957 (9) |
O14—Li2i | 1.976 (6) | Yb2—H22 | 0.968 (9) |
S2—O24 | 1.464 (2) | Yb2—H23 | 0.963 (9) |
S2—O21 | 1.475 (3) | Yb2—H24 | 0.966 (9) |
S2—O22 | 1.482 (2) | Li1—O22vi | 1.929 (5) |
S2—O23 | 1.487 (2) | Li1—O23vii | 1.945 (5) |
S2—Li1vi | 3.033 (5) | Li1—O21ix | 1.952 (5) |
S2—Li1 | 3.048 (6) | Li1—S2vii | 3.033 (5) |
O21—Li1iii | 1.952 (5) | Li1—Li1vi | 3.238 (6) |
O21—Yb2iii | 2.967 (4) | Li1—Li1vii | 3.238 (6) |
O22—Li1vii | 1.929 (5) | Li1—Yb2vi | 3.534 (5) |
O22—Yb2 | 2.955 (4) | Li1—Yb2viii | 3.863 (5) |
O22—Yb2v | 3.077 (5) | Li2—O12viii | 1.930 (5) |
O23—Li1vi | 1.945 (5) | Li2—O11ii | 1.945 (5) |
O23—Li1 | 1.976 (5) | Li2—O14xi | 1.976 (6) |
O24—Yb1iii | 2.789 (3) | Li2—S1xi | 3.049 (5) |
O24—Yb2viii | 2.958 (4) | Li2—Li2i | 3.253 (7) |
Yb1—O24ix | 2.789 (3) | Li2—Li2xi | 3.253 (7) |
Yb1—O12viii | 2.965 (5) | Li2—Yb1i | 3.707 (5) |
Yb1—O11ix | 2.966 (4) | Li2—Yb1xi | 3.858 (5) |
Yb1—O12x | 3.067 (4) | | |
| | | |
O13—S1—O11 | 110.81 (15) | O22x—Yb2—Li1iv | 61.38 (10) |
O13—S1—O14 | 109.66 (14) | Li1vii—Yb2—Li1iv | 51.69 (10) |
O11—S1—O14 | 110.26 (13) | Li1—Yb2—Li1iv | 82.64 (10) |
O13—S1—O12 | 108.61 (14) | O13—Yb2—H21 | 9.4 (18) |
O11—S1—O12 | 108.90 (14) | O22—Yb2—H21 | 120.3 (18) |
O14—S1—O12 | 108.54 (13) | O24iv—Yb2—H21 | 90.8 (18) |
O13—S1—Li2 | 103.71 (14) | O21ix—Yb2—H21 | 113.3 (18) |
O11—S1—Li2 | 83.67 (14) | O22x—Yb2—H21 | 112.0 (18) |
O14—S1—Li2 | 32.67 (13) | Li1vii—Yb2—H21 | 148.6 (18) |
O12—S1—Li2 | 137.54 (13) | Li1—Yb2—H21 | 139.2 (18) |
O13—S1—Li2i | 99.45 (15) | Li1iv—Yb2—H21 | 137.8 (18) |
O11—S1—Li2i | 140.63 (13) | O13—Yb2—H22 | 100.9 (18) |
O14—S1—Li2i | 32.93 (12) | O22—Yb2—H22 | 101.6 (19) |
O12—S1—Li2i | 83.28 (13) | O24iv—Yb2—H22 | 157.5 (18) |
Li2—S1—Li2i | 64.64 (12) | O21ix—Yb2—H22 | 21.2 (19) |
S1—O11—Li2ii | 128.97 (19) | O22x—Yb2—H22 | 50.2 (19) |
S1—O11—Yb1iii | 125.36 (13) | Li1vii—Yb2—H22 | 95.3 (18) |
Li2ii—O11—Yb1iii | 95.78 (17) | Li1—Yb2—H22 | 46.2 (18) |
S1—O12—Li2iv | 130.39 (19) | Li1iv—Yb2—H22 | 96.1 (18) |
S1—O12—Yb1iv | 108.70 (13) | H21—Yb2—H22 | 110.3 (15) |
Li2iv—O12—Yb1iv | 90.47 (17) | O13—Yb2—H23 | 115.2 (18) |
S1—O12—Yb1v | 98.04 (12) | O22—Yb2—H23 | 10.0 (18) |
Li2iv—O12—Yb1v | 113.64 (19) | O24iv—Yb2—H23 | 69.4 (19) |
Yb1iv—O12—Yb1v | 116.77 (11) | O21ix—Yb2—H23 | 88.2 (19) |
S1—O13—Yb2 | 139.91 (15) | O22x—Yb2—H23 | 137.1 (18) |
S1—O13—Yb1 | 113.95 (13) | Li1vii—Yb2—H23 | 41.6 (18) |
Yb2—O13—Yb1 | 104.44 (10) | Li1—Yb2—H23 | 64.6 (18) |
S1—O14—Li2 | 123.22 (19) | Li1iv—Yb2—H23 | 90.4 (18) |
S1—O14—Li2i | 123.01 (19) | H21—Yb2—H23 | 110.4 (15) |
Li2—O14—Li2i | 111.50 (19) | H22—Yb2—H23 | 108.4 (15) |
O24—S2—O21 | 110.42 (14) | O13—Yb2—H24 | 114.0 (17) |
O24—S2—O22 | 108.95 (14) | O22—Yb2—H24 | 106.0 (18) |
O21—S2—O22 | 109.47 (14) | O24iv—Yb2—H24 | 55.6 (18) |
O24—S2—O23 | 109.34 (14) | O21ix—Yb2—H24 | 122.4 (18) |
O21—S2—O23 | 109.88 (14) | O22x—Yb2—H24 | 59.8 (18) |
O22—S2—O23 | 108.75 (12) | Li1vii—Yb2—H24 | 77.2 (18) |
O24—S2—Li1vi | 102.87 (14) | Li1—Yb2—H24 | 109.1 (17) |
O21—S2—Li1vi | 83.77 (14) | Li1iv—Yb2—H24 | 28.1 (17) |
O22—S2—Li1vi | 137.68 (12) | H21—Yb2—H24 | 110.2 (15) |
O23—S2—Li1vi | 32.26 (12) | H22—Yb2—H24 | 107.5 (14) |
O24—S2—Li1 | 99.68 (14) | H23—Yb2—H24 | 109.9 (15) |
O21—S2—Li1 | 140.35 (13) | O22vi—Li1—O23vii | 107.4 (2) |
O22—S2—Li1 | 83.12 (12) | O22vi—Li1—O21ix | 120.9 (3) |
O23—S2—Li1 | 33.07 (12) | O23vii—Li1—O21ix | 110.3 (2) |
Li1vi—S2—Li1 | 64.34 (11) | O22vi—Li1—O23 | 103.5 (2) |
S2—O21—Li1iii | 128.71 (17) | O23vii—Li1—O23 | 106.4 (2) |
S2—O21—Yb2iii | 125.53 (13) | O21ix—Li1—O23 | 107.2 (2) |
Li1iii—O21—Yb2iii | 96.06 (17) | O22vi—Li1—S2vii | 88.12 (16) |
S2—O22—Li1vii | 130.33 (18) | O23vii—Li1—S2vii | 24.07 (8) |
S2—O22—Yb2 | 109.24 (13) | O21ix—Li1—S2vii | 110.7 (2) |
Li1vii—O22—Yb2 | 90.18 (17) | O23—Li1—S2vii | 126.3 (2) |
S2—O22—Yb2v | 97.69 (11) | O22vi—Li1—S2 | 127.5 (2) |
Li1vii—O22—Yb2v | 113.85 (18) | O23vii—Li1—S2 | 93.46 (17) |
Yb2—O22—Yb2v | 116.82 (11) | O21ix—Li1—S2 | 93.64 (17) |
S2—O23—Li1vi | 123.67 (17) | O23—Li1—S2 | 24.23 (9) |
S2—O23—Li1 | 122.70 (19) | S2vii—Li1—S2 | 117.07 (15) |
Li1vi—O23—Li1 | 111.31 (18) | O22vi—Li1—Li1vi | 72.28 (16) |
S2—O24—Yb1iii | 140.94 (15) | O23vii—Li1—Li1vi | 128.8 (3) |
S2—O24—Yb2viii | 114.43 (13) | O21ix—Li1—Li1vi | 112.6 (2) |
Yb1iii—O24—Yb2viii | 101.68 (10) | O23—Li1—Li1vi | 34.03 (16) |
O24ix—Yb1—O12viii | 128.95 (12) | S2vii—Li1—Li1vi | 136.6 (2) |
O24ix—Yb1—O11ix | 110.73 (11) | S2—Li1—Li1vi | 57.61 (16) |
O12viii—Yb1—O11ix | 82.76 (10) | O22vi—Li1—Li1vii | 123.8 (3) |
O24ix—Yb1—O13 | 95.07 (11) | O23vii—Li1—Li1vii | 34.65 (7) |
O12viii—Yb1—O13 | 72.67 (11) | O21ix—Li1—Li1vii | 113.0 (2) |
O11ix—Yb1—O13 | 152.18 (10) | O23—Li1—Li1vii | 72.8 (2) |
O24ix—Yb1—O12x | 103.30 (12) | S2vii—Li1—Li1vii | 58.05 (10) |
O12viii—Yb1—O12x | 127.07 (12) | S2—Li1—Li1vii | 59.03 (16) |
O11ix—Yb1—O12x | 70.00 (9) | Li1vi—Li1—Li1vii | 101.3 (3) |
O13—Yb1—O12x | 115.03 (12) | O22vi—Li1—Yb2vi | 56.74 (15) |
O24ix—Yb1—Li2 | 156.80 (13) | O23vii—Li1—Yb2vi | 71.59 (15) |
O12viii—Yb1—Li2 | 32.93 (10) | O21ix—Li1—Yb2vi | 177.6 (2) |
O11ix—Yb1—Li2 | 84.64 (11) | O23—Li1—Yb2vi | 73.35 (16) |
O13—Yb1—Li2 | 67.66 (11) | S2vii—Li1—Yb2vi | 70.35 (10) |
O12x—Yb1—Li2 | 98.22 (13) | S2—Li1—Yb2vi | 87.72 (14) |
O24ix—Yb1—Li2xi | 139.57 (13) | Li1vi—Li1—Yb2vi | 66.48 (17) |
O12viii—Yb1—Li2xi | 56.60 (10) | Li1vii—Li1—Yb2vi | 69.41 (17) |
O11ix—Yb1—Li2xi | 31.46 (9) | O22vi—Li1—Yb2 | 166.7 (2) |
O13—Yb1—Li2xi | 120.74 (12) | O23vii—Li1—Yb2 | 68.81 (14) |
O12x—Yb1—Li2xi | 79.39 (11) | O21ix—Li1—Yb2 | 52.48 (13) |
Li2—Yb1—Li2xi | 53.19 (11) | O23—Li1—Yb2 | 89.73 (16) |
O24ix—Yb1—Li2i | 134.36 (13) | S2vii—Li1—Yb2 | 84.61 (13) |
O12viii—Yb1—Li2i | 83.77 (11) | S2—Li1—Yb2 | 65.74 (10) |
O11ix—Yb1—Li2i | 103.43 (11) | Li1vi—Li1—Yb2 | 120.3 (2) |
O13—Yb1—Li2i | 61.78 (10) | Li1vii—Li1—Yb2 | 60.57 (12) |
O12x—Yb1—Li2i | 61.16 (11) | Yb2vi—Li1—Yb2 | 129.94 (15) |
Li2—Yb1—Li2i | 51.88 (10) | O22vi—Li1—Yb2viii | 102.44 (19) |
Li2xi—Yb1—Li2i | 82.88 (10) | O23vii—Li1—Yb2viii | 150.02 (19) |
O24ix—Yb1—H11 | 7.4 (18) | O21ix—Li1—Yb2viii | 53.72 (13) |
O12viii—Yb1—H11 | 124.0 (17) | O23—Li1—Yb2viii | 63.13 (14) |
O11ix—Yb1—H11 | 117.0 (18) | S2vii—Li1—Yb2viii | 164.14 (16) |
O13—Yb1—H11 | 88.1 (18) | S2—Li1—Yb2viii | 65.58 (9) |
O12x—Yb1—H11 | 108.8 (17) | Li1vi—Li1—Yb2viii | 58.90 (12) |
Li2—Yb1—H11 | 149.7 (18) | Li1vii—Li1—Yb2viii | 122.0 (2) |
Li2xi—Yb1—H11 | 144.2 (18) | Yb2vi—Li1—Yb2viii | 125.35 (15) |
Li2i—Yb1—H11 | 132.1 (18) | Yb2—Li1—Yb2viii | 82.64 (10) |
O24ix—Yb1—H12 | 101.1 (17) | O12viii—Li2—O11ii | 120.9 (3) |
O12viii—Yb1—H12 | 99.1 (18) | O12viii—Li2—O14 | 107.1 (2) |
O11ix—Yb1—H12 | 16.4 (18) | O11ii—Li2—O14 | 111.0 (3) |
O13—Yb1—H12 | 163.5 (17) | O12viii—Li2—O14xi | 103.3 (2) |
O12x—Yb1—H12 | 58.1 (19) | O11ii—Li2—O14xi | 107.5 (2) |
Li2—Yb1—H12 | 97.6 (17) | O14—Li2—O14xi | 105.7 (2) |
Li2xi—Yb1—H12 | 45.7 (18) | O12viii—Li2—S1 | 88.02 (17) |
Li2i—Yb1—H12 | 103.8 (18) | O11ii—Li2—S1 | 111.1 (2) |
H11—Yb1—H12 | 108.1 (14) | O14—Li2—S1 | 24.11 (9) |
O24ix—Yb1—H13 | 110.1 (17) | O14xi—Li2—S1 | 125.7 (2) |
O12viii—Yb1—H13 | 107.7 (18) | O12viii—Li2—S1xi | 127.2 (2) |
O11ix—Yb1—H13 | 114.0 (18) | O11ii—Li2—S1xi | 94.00 (19) |
O13—Yb1—H13 | 63.5 (18) | O14—Li2—S1xi | 93.13 (19) |
O12x—Yb1—H13 | 51.6 (18) | O14xi—Li2—S1xi | 24.06 (9) |
Li2—Yb1—H13 | 76.9 (18) | S1—Li2—S1xi | 116.79 (16) |
Li2xi—Yb1—H13 | 102.9 (17) | O12viii—Li2—Li2i | 123.2 (3) |
Li2i—Yb1—H13 | 25.4 (17) | O11ii—Li2—Li2i | 113.7 (2) |
H11—Yb1—H13 | 109.2 (15) | O14—Li2—Li2i | 34.43 (7) |
H12—Yb1—H13 | 107.2 (14) | O14xi—Li2—Li2i | 72.4 (2) |
O24ix—Yb1—H14 | 116.2 (18) | S1—Li2—Li2i | 57.88 (9) |
O12viii—Yb1—H14 | 14.1 (18) | S1xi—Li2—Li2i | 58.92 (17) |
O11ix—Yb1—H14 | 93.3 (19) | O12viii—Li2—Li2xi | 72.04 (16) |
O13—Yb1—H14 | 65.1 (19) | O11ii—Li2—Li2xi | 113.0 (2) |
O12x—Yb1—H14 | 140.5 (18) | O14—Li2—Li2xi | 127.8 (3) |
Li2—Yb1—H14 | 43.3 (18) | O14xi—Li2—Li2xi | 34.07 (17) |
Li2xi—Yb1—H14 | 69.7 (18) | S1—Li2—Li2xi | 135.8 (2) |
Li2i—Yb1—H14 | 90.4 (18) | S1xi—Li2—Li2xi | 57.48 (17) |
H11—Yb1—H14 | 110.7 (15) | Li2i—Li2—Li2xi | 100.7 (3) |
H12—Yb1—H14 | 109.7 (15) | O12viii—Li2—Yb1 | 56.60 (14) |
H13—Yb1—H14 | 111.8 (15) | O11ii—Li2—Yb1 | 177.4 (2) |
O13—Yb2—O22 | 124.64 (12) | O14—Li2—Yb1 | 71.20 (14) |
O13—Yb2—O24iv | 99.98 (10) | O14xi—Li2—Yb1 | 72.88 (17) |
O22—Yb2—O24iv | 72.69 (10) | S1—Li2—Yb1 | 70.22 (10) |
O13—Yb2—O21ix | 104.82 (11) | S1xi—Li2—Yb1 | 87.27 (15) |
O22—Yb2—O21ix | 82.52 (10) | Li2i—Li2—Yb1 | 68.93 (17) |
O24iv—Yb2—O21ix | 152.00 (11) | Li2xi—Li2—Yb1 | 65.86 (17) |
O13—Yb2—O22x | 106.02 (11) | O12viii—Li2—Yb1i | 166.9 (2) |
O22—Yb2—O22x | 127.10 (12) | O11ii—Li2—Yb1i | 52.76 (14) |
O24iv—Yb2—O22x | 115.42 (12) | O14—Li2—Yb1i | 69.04 (15) |
O21ix—Yb2—O22x | 69.85 (9) | O14xi—Li2—Yb1i | 89.74 (17) |
O13—Yb2—Li1vii | 155.77 (13) | S1—Li2—Yb1i | 84.70 (13) |
O22—Yb2—Li1vii | 33.09 (9) | S1xi—Li2—Yb1i | 65.90 (11) |
O24iv—Yb2—Li1vii | 67.76 (10) | Li2i—Li2—Yb1i | 60.94 (13) |
O21ix—Yb2—Li1vii | 84.38 (11) | Li2xi—Li2—Yb1i | 120.5 (2) |
O22x—Yb2—Li1vii | 98.18 (12) | Yb1—Li2—Yb1i | 129.83 (15) |
O13—Yb2—Li1 | 132.54 (13) | O12viii—Li2—Yb1xi | 102.3 (2) |
O22—Yb2—Li1 | 56.40 (10) | O11ii—Li2—Yb1xi | 53.79 (14) |
O24iv—Yb2—Li1 | 120.57 (11) | O14—Li2—Yb1xi | 150.3 (2) |
O21ix—Yb2—Li1 | 31.46 (9) | O14xi—Li2—Yb1xi | 63.41 (15) |
O22x—Yb2—Li1 | 79.36 (10) | S1—Li2—Yb1xi | 164.60 (16) |
Li1vii—Yb2—Li1 | 52.95 (10) | S1xi—Li2—Yb1xi | 65.78 (10) |
O13—Yb2—Li1iv | 142.16 (13) | Li2i—Li2—Yb1xi | 122.2 (2) |
O22—Yb2—Li1iv | 83.74 (10) | Li2xi—Li2—Yb1xi | 59.19 (12) |
O24iv—Yb2—Li1iv | 61.97 (10) | Yb1—Li2—Yb1xi | 125.02 (16) |
O21ix—Yb2—Li1iv | 103.22 (11) | Yb1i—Li2—Yb1xi | 82.88 (10) |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x, y+1, z; (v) x, −y+3/2, z+1/2; (vi) −x, y−1/2, −z+1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y−1, z; (ix) x, −y+1/2, z−1/2; (x) x, −y+3/2, z−1/2; (xi) −x+1, y−1/2, −z+1/2. |
Crystal data top
O4SYb0.013·0.961(H4N)·Li | F(000) = 1000.0 |
Mr = 122.51 | Dx = 1.831 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.177 (15) Å | Cell parameters from 25 reflections |
b = 5.106 (4) Å | θ = 9–19° |
c = 34.234 (16) Å | µ = 0.89 mm−1 |
β = 90.2 (1)° | T = 293 K |
V = 1779 (3) Å3 | Prism, colourless |
Z = 16 | 0.17 × 0.11 × 0.09 mm |
Data collection top
ENRAF-Nonius CAD4 diffractometer | θmax = 30.0°, θmin = 2.0° |
ω/2Θ–scan | h = −14→14 |
9573 measured reflections | k = −7→7 |
5071 independent reflections | l = −48→0 |
3231 reflections with I > 2σ(I) | 3 standard reflections every 120 min |
Rint = 0.068 | |
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)] = 0.060 | Hydrogen site location: notdet |
wR(F2) = 0.163 | H-atom parameters not defined |
S = 1.20 | w = 1/[σ2(Fo2) + (0.0263P)2 + 6.4506P] where P = (Fo2 + 2Fc2)/3 |
5071 reflections | (Δ/σ)max < 0.001 |
256 parameters | Δρmax = 1.89 e Å−3 |
0 restraints | Δρmin = −1.04 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
S1 | 0.64805 (7) | 0.73307 (14) | 0.20089 (2) | 0.00608 (14) | |
O11 | 0.6399 (4) | 0.4374 (5) | 0.20610 (11) | 0.0406 (9) | |
O12 | 0.7859 (3) | 0.8058 (10) | 0.20413 (11) | 0.0521 (12) | |
O13 | 0.5709 (3) | 0.8568 (6) | 0.23235 (9) | 0.0274 (7) | |
O14 | 0.5950 (4) | 0.7924 (10) | 0.16305 (10) | 0.0566 (13) | |
S2 | 0.89820 (8) | 0.28368 (18) | 0.04920 (3) | 0.01657 (19) | |
O21 | 0.8934 (3) | 0.5828 (6) | 0.04414 (10) | 0.0324 (8) | |
O22 | 1.0370 (3) | 0.2110 (6) | 0.04620 (9) | 0.0298 (7) | |
O23 | 0.8456 (3) | 0.2180 (7) | 0.08669 (9) | 0.0368 (8) | |
O24 | 0.8213 (3) | 0.1630 (6) | 0.01798 (9) | 0.0280 (7) | |
S3 | 0.39959 (8) | 0.21622 (18) | 0.04902 (3) | 0.01718 (19) | |
O31 | 0.5355 (3) | 0.2891 (6) | 0.04630 (10) | 0.0304 (7) | |
O32 | 0.3211 (3) | 0.3371 (6) | 0.01735 (9) | 0.0273 (7) | |
O33 | 0.3916 (3) | −0.0811 (6) | 0.04468 (10) | 0.0330 (8) | |
O34 | 0.3434 (3) | 0.2813 (7) | 0.08748 (9) | 0.0324 (7) | |
S4 | 0.14878 (11) | 0.8032 (3) | 0.20093 (4) | 0.0364 (3) | |
O41 | 0.1414 (3) | 1.1054 (7) | 0.20461 (9) | 0.0314 (7) | |
O42 | 0.2864 (2) | 0.7278 (5) | 0.20357 (8) | 0.0211 (5) | |
O43 | 0.0927 (3) | 0.7312 (6) | 0.16299 (9) | 0.0272 (6) | |
O44 | 0.0714 (3) | 0.6850 (7) | 0.23248 (9) | 0.0292 (7) | |
N1 | 0.4006 (3) | 0.2369 (6) | 0.16624 (10) | 0.0417 (11) | 0.907 (4) |
N2 | 0.6508 (3) | 0.7697 (7) | 0.08377 (10) | 0.0364 (13) | 0.959 (4) |
N3 | 0.1517 (3) | 0.7309 (7) | 0.08326 (11) | 0.0331 (14) | 0.978 (4) |
N4 | 0.9005 (4) | 0.2744 (9) | 0.16666 (12) | 0.0381 (10) | |
Yb1 | 0.4006 (3) | 0.2369 (6) | 0.16624 (10) | 0.0417 (11) | 0.0311 (15) |
Yb2 | 0.6508 (3) | 0.7697 (7) | 0.08377 (10) | 0.0364 (13) | 0.0137 (15) |
Yb3 | 0.1517 (3) | 0.7309 (7) | 0.08326 (11) | 0.0331 (14) | 0.0074 (14) |
Li1 | 0.3992 (7) | 0.7198 (14) | 0.2497 (2) | 0.0237 (14) | |
Li2 | 0.1017 (7) | 0.3041 (15) | 0.2508 (2) | 0.0278 (16) | |
Li3 | 0.1488 (7) | 0.2123 (13) | 0.0001 (2) | 0.0218 (14) | |
Li4 | 0.6491 (6) | 0.2976 (12) | 0.0013 (2) | 0.0190 (13) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
S1 | 0.0035 (3) | 0.0084 (3) | 0.0063 (3) | −0.0004 (3) | −0.0014 (2) | −0.0003 (3) |
O11 | 0.065 (2) | 0.0118 (13) | 0.045 (2) | −0.0014 (14) | 0.0142 (18) | −0.0014 (13) |
O12 | 0.0098 (13) | 0.114 (4) | 0.0322 (19) | −0.0037 (18) | 0.0014 (12) | −0.005 (2) |
O13 | 0.0287 (15) | 0.0257 (14) | 0.0279 (17) | −0.0020 (12) | 0.0078 (13) | −0.0013 (12) |
O14 | 0.0377 (19) | 0.122 (4) | 0.0099 (14) | 0.016 (2) | −0.0061 (13) | 0.001 (2) |
S2 | 0.0104 (3) | 0.0249 (4) | 0.0144 (4) | 0.0028 (3) | −0.0027 (3) | −0.0003 (3) |
O21 | 0.0384 (18) | 0.0255 (14) | 0.0332 (19) | 0.0041 (13) | −0.0138 (14) | −0.0020 (13) |
O22 | 0.0117 (11) | 0.051 (2) | 0.0270 (16) | 0.0109 (12) | −0.0030 (11) | −0.0023 (14) |
O23 | 0.0348 (17) | 0.060 (2) | 0.0155 (14) | −0.0126 (16) | 0.0031 (12) | −0.0080 (15) |
O24 | 0.0218 (14) | 0.0364 (16) | 0.0257 (17) | 0.0053 (12) | −0.0079 (12) | −0.0079 (13) |
S3 | 0.0114 (3) | 0.0266 (5) | 0.0135 (4) | 0.0016 (3) | −0.0026 (3) | −0.0019 (3) |
O31 | 0.0112 (11) | 0.0487 (19) | 0.0313 (17) | −0.0048 (12) | −0.0051 (11) | −0.0013 (14) |
O32 | 0.0209 (14) | 0.0369 (15) | 0.0238 (16) | 0.0019 (12) | −0.0116 (12) | 0.0060 (13) |
O33 | 0.0323 (17) | 0.0259 (15) | 0.041 (2) | −0.0004 (12) | −0.0165 (15) | 0.0033 (14) |
O34 | 0.0259 (14) | 0.0484 (19) | 0.0230 (15) | 0.0146 (14) | 0.0050 (12) | −0.0002 (14) |
S4 | 0.0179 (4) | 0.0704 (9) | 0.0209 (5) | −0.0018 (5) | 0.0000 (4) | −0.0005 (6) |
O41 | 0.0173 (13) | 0.057 (2) | 0.0205 (15) | 0.0063 (14) | 0.0055 (11) | 0.0008 (15) |
O42 | 0.0074 (10) | 0.0309 (14) | 0.0249 (14) | 0.0036 (10) | −0.0002 (9) | −0.0053 (12) |
O43 | 0.0234 (13) | 0.0381 (16) | 0.0200 (14) | −0.0162 (13) | −0.0093 (11) | −0.0002 (13) |
O44 | 0.0111 (12) | 0.056 (2) | 0.0207 (15) | 0.0053 (12) | 0.0038 (11) | 0.0073 (13) |
N1 | 0.0405 (18) | 0.0413 (17) | 0.0432 (19) | −0.0032 (13) | −0.0030 (12) | −0.0037 (14) |
N2 | 0.034 (2) | 0.043 (2) | 0.032 (2) | 0.0015 (15) | 0.0024 (13) | −0.0043 (15) |
N3 | 0.0247 (18) | 0.043 (2) | 0.032 (2) | −0.0003 (15) | −0.0039 (13) | −0.0048 (16) |
N4 | 0.0216 (16) | 0.067 (3) | 0.0252 (19) | −0.0026 (19) | −0.0052 (14) | 0.002 (2) |
Yb1 | 0.0405 (18) | 0.0413 (17) | 0.0432 (19) | −0.0032 (13) | −0.0030 (12) | −0.0037 (14) |
Yb2 | 0.034 (2) | 0.043 (2) | 0.032 (2) | 0.0015 (15) | 0.0024 (13) | −0.0043 (15) |
Yb3 | 0.0247 (18) | 0.043 (2) | 0.032 (2) | −0.0003 (15) | −0.0039 (13) | −0.0048 (16) |
Li1 | 0.019 (3) | 0.034 (4) | 0.018 (3) | −0.001 (3) | 0.004 (2) | 0.002 (3) |
Li2 | 0.018 (3) | 0.040 (4) | 0.025 (4) | 0.003 (3) | −0.006 (3) | 0.000 (3) |
Li3 | 0.024 (3) | 0.021 (3) | 0.021 (3) | 0.002 (2) | −0.002 (3) | −0.006 (3) |
Li4 | 0.011 (3) | 0.023 (3) | 0.023 (3) | 0.000 (2) | −0.002 (2) | −0.006 (2) |
Geometric parameters (Å, º) top
S1—O14 | 1.434 (3) | S4—O43 | 1.464 (3) |
S1—O12 | 1.455 (4) | S4—O44 | 1.469 (3) |
S1—O13 | 1.477 (3) | S4—O41 | 1.550 (4) |
S1—O11 | 1.522 (3) | S4—Li2ix | 3.043 (9) |
S1—Li1 | 3.040 (8) | O41—Li2iii | 1.922 (9) |
S1—Li1i | 3.045 (7) | O41—Yb1iii | 3.027 (6) |
O11—Li1ii | 1.920 (8) | O42—Li1 | 1.950 (8) |
O12—Li2i | 1.918 (8) | O44—Li2ix | 1.951 (8) |
O13—Li1i | 1.976 (8) | O44—Li2 | 2.066 (8) |
O13—Li1 | 1.976 (8) | Li1—O11i | 1.920 (8) |
O14—Yb1iii | 3.013 (6) | Li1—O13ii | 1.976 (8) |
S2—O23 | 1.432 (3) | Li1—S1ii | 3.045 (7) |
S2—O24 | 1.459 (3) | Li1—Li1ii | 3.275 (9) |
S2—O22 | 1.464 (3) | Li1—Li1i | 3.275 (9) |
S2—O21 | 1.538 (3) | Li1—Yb1i | 3.520 (8) |
S2—Li4 | 3.016 (7) | Li1—Yb1iii | 3.891 (8) |
O21—Li3iv | 1.890 (8) | Li2—O12ii | 1.918 (8) |
O21—Yb3v | 3.042 (6) | Li2—O41vii | 1.922 (9) |
O22—Li3v | 1.948 (8) | Li2—O44x | 1.951 (8) |
O22—Yb3vi | 2.996 (5) | Li2—S4x | 3.043 (9) |
O23—Yb2vii | 3.030 (5) | Li2—Li2ix | 3.287 (9) |
O24—Li4 | 1.966 (7) | Li2—Li2x | 3.287 (9) |
O24—Li3viii | 2.037 (7) | Li3—O21iv | 1.890 (8) |
S3—O31 | 1.436 (3) | Li3—O22xi | 1.948 (8) |
S3—O34 | 1.475 (3) | Li3—O24viii | 2.037 (7) |
S3—O32 | 1.479 (3) | Li3—Li4iv | 3.239 (9) |
S3—O33 | 1.527 (3) | Li3—Li4viii | 3.319 (9) |
S3—Li3 | 3.047 (8) | Li3—Yb2iv | 3.530 (9) |
O31—Li4 | 1.930 (8) | Li3—Yb3vii | 3.760 (8) |
O32—Li3 | 1.954 (8) | Li4—O33viii | 1.966 (7) |
O32—Li4iv | 1.995 (7) | Li4—O32iv | 1.995 (7) |
O33—Li4viii | 1.966 (7) | Li4—Li3iv | 3.239 (9) |
O33—Yb3vii | 2.941 (6) | Li4—Li3viii | 3.319 (9) |
O33—Yb2vii | 3.050 (6) | Li4—Yb3iv | 3.542 (9) |
S4—O42 | 1.455 (3) | Li4—Yb2vii | 3.904 (8) |
| | | |
O14—S1—O12 | 112.0 (2) | O13ii—Li1—Yb1i | 71.4 (2) |
O14—S1—O13 | 111.7 (2) | O13—Li1—Yb1i | 74.2 (2) |
O12—S1—O13 | 110.5 (2) | S1—Li1—Yb1i | 88.2 (2) |
O14—S1—O11 | 107.2 (3) | S1ii—Li1—Yb1i | 70.03 (16) |
O12—S1—O11 | 107.3 (3) | Li1ii—Li1—Yb1i | 69.8 (3) |
O13—S1—O11 | 108.0 (2) | Li1i—Li1—Yb1i | 67.4 (3) |
O14—S1—Li1 | 101.0 (2) | O11i—Li1—Yb1iii | 100.8 (3) |
O12—S1—Li1 | 140.2 (2) | O42—Li1—Yb1iii | 52.7 (2) |
O13—S1—Li1 | 33.14 (19) | O13ii—Li1—Yb1iii | 149.8 (3) |
O11—S1—Li1 | 82.4 (2) | O13—Li1—Yb1iii | 62.2 (2) |
O14—S1—Li1i | 105.6 (2) | S1—Li1—Yb1iii | 64.90 (15) |
O12—S1—Li1i | 84.5 (2) | S1ii—Li1—Yb1iii | 164.3 (2) |
O13—S1—Li1i | 32.91 (18) | Li1ii—Li1—Yb1iii | 122.0 (3) |
O11—S1—Li1i | 137.4 (2) | Li1i—Li1—Yb1iii | 58.09 (19) |
Li1—S1—Li1i | 65.12 (16) | Yb1i—Li1—Yb1iii | 125.4 (2) |
S1—O11—Li1ii | 132.7 (3) | O12ii—Li2—O41vii | 122.5 (4) |
S1—O12—Li2i | 129.2 (3) | O12ii—Li2—O44x | 107.6 (4) |
S1—O13—Li1i | 123.1 (3) | O41vii—Li2—O44x | 105.6 (4) |
S1—O13—Li1 | 122.7 (3) | O12ii—Li2—O44 | 109.1 (4) |
Li1i—O13—Li1 | 112.0 (3) | O41vii—Li2—O44 | 106.2 (4) |
S1—O14—Yb1iii | 111.8 (2) | O44x—Li2—O44 | 104.4 (3) |
O23—S2—O24 | 110.9 (2) | O12ii—Li2—S4x | 93.5 (3) |
O23—S2—O22 | 111.5 (2) | O41vii—Li2—S4x | 128.7 (3) |
O24—S2—O22 | 110.9 (2) | O44x—Li2—S4x | 23.27 (15) |
O23—S2—O21 | 108.8 (2) | O44—Li2—S4x | 92.4 (3) |
O24—S2—O21 | 108.67 (18) | O12ii—Li2—Li2ix | 112.5 (4) |
O22—S2—O21 | 105.90 (19) | O41vii—Li2—Li2ix | 122.1 (4) |
O23—S2—Li4 | 100.2 (2) | O44x—Li2—Li2ix | 71.2 (4) |
O24—S2—Li4 | 33.25 (17) | O44—Li2—Li2ix | 33.96 (10) |
O22—S2—Li4 | 140.99 (19) | S4x—Li2—Li2ix | 58.8 (3) |
O21—S2—Li4 | 83.62 (17) | O12ii—Li2—Li2x | 113.0 (4) |
S2—O21—Li3iv | 130.3 (3) | O41vii—Li2—Li2x | 73.2 (3) |
S2—O21—Yb3v | 99.80 (16) | O44x—Li2—Li2x | 36.3 (3) |
Li3iv—O21—Yb3v | 114.2 (3) | O44—Li2—Li2x | 129.3 (4) |
S2—O22—Li3v | 128.5 (3) | S4x—Li2—Li2x | 58.6 (3) |
S2—O22—Yb3vi | 123.5 (2) | Li2ix—Li2—Li2x | 101.9 (4) |
Li3v—O22—Yb3vi | 96.8 (2) | O21iv—Li3—O22xi | 121.3 (4) |
S2—O23—Yb2vii | 113.19 (18) | O21iv—Li3—O32 | 105.2 (4) |
S2—O24—Li4 | 122.7 (3) | O22xi—Li3—O32 | 106.4 (4) |
S2—O24—Li3viii | 122.7 (3) | O21iv—Li3—O24viii | 108.1 (3) |
Li4—O24—Li3viii | 112.0 (3) | O22xi—Li3—O24viii | 109.4 (4) |
O31—S3—O34 | 112.1 (2) | O32—Li3—O24viii | 105.3 (3) |
O31—S3—O32 | 111.2 (2) | O21iv—Li3—S3 | 128.6 (3) |
O34—S3—O32 | 110.49 (19) | O22xi—Li3—S3 | 92.6 (3) |
O31—S3—O33 | 107.58 (19) | O32—Li3—S3 | 23.58 (14) |
O34—S3—O33 | 106.9 (2) | O24viii—Li3—S3 | 92.7 (2) |
O32—S3—O33 | 108.37 (18) | O21iv—Li3—Li4iv | 72.7 (3) |
O31—S3—Li3 | 140.5 (2) | O22xi—Li3—Li4iv | 112.8 (3) |
O34—S3—Li3 | 99.5 (2) | O32—Li3—Li4iv | 35.30 (19) |
O32—S3—Li3 | 31.90 (19) | O24viii—Li3—Li4iv | 128.8 (3) |
O33—S3—Li3 | 84.04 (17) | S3—Li3—Li4iv | 58.17 (16) |
S3—O31—Li4 | 129.6 (3) | O21iv—Li3—Li4viii | 124.2 (3) |
S3—O32—Li3 | 124.5 (3) | O22xi—Li3—Li4viii | 111.9 (3) |
S3—O32—Li4iv | 122.8 (3) | O32—Li3—Li4viii | 72.8 (2) |
Li3—O32—Li4iv | 110.2 (3) | O24viii—Li3—Li4viii | 33.33 (19) |
S3—O33—Li4viii | 130.4 (3) | S3—Li3—Li4viii | 59.68 (16) |
S3—O33—Yb3vii | 108.95 (19) | Li4iv—Li3—Li4viii | 102.3 (2) |
Li4viii—O33—Yb3vii | 90.2 (2) | O21iv—Li3—Yb2iv | 57.5 (2) |
S3—O33—Yb2vii | 99.22 (15) | O22xi—Li3—Yb2iv | 178.6 (3) |
Li4viii—O33—Yb2vii | 113.0 (2) | O32—Li3—Yb2iv | 73.5 (3) |
Yb3vii—O33—Yb2vii | 116.06 (16) | O24viii—Li3—Yb2iv | 71.9 (2) |
O42—S4—O43 | 111.2 (2) | S3—Li3—Yb2iv | 87.8 (2) |
O42—S4—O44 | 111.4 (2) | Li4iv—Li3—Yb2iv | 66.37 (18) |
O43—S4—O44 | 109.9 (2) | Li4viii—Li3—Yb2iv | 69.43 (18) |
O42—S4—O41 | 107.78 (18) | O21iv—Li3—Yb3vii | 165.9 (3) |
O43—S4—O41 | 107.7 (2) | O22xi—Li3—Yb3vii | 52.3 (2) |
O44—S4—O41 | 108.9 (2) | O32—Li3—Yb3vii | 88.9 (3) |
O42—S4—Li2ix | 140.8 (2) | O24viii—Li3—Yb3vii | 67.3 (2) |
O43—S4—Li2ix | 99.1 (2) | S3—Li3—Yb3vii | 65.44 (15) |
O44—S4—Li2ix | 31.65 (19) | Li4iv—Li3—Yb3vii | 120.9 (2) |
O41—S4—Li2ix | 85.04 (19) | Li4viii—Li3—Yb3vii | 59.66 (18) |
S4—O41—Li2iii | 127.1 (3) | Yb2iv—Li3—Yb3vii | 129.0 (2) |
S4—O41—Yb1iii | 98.23 (15) | O31—Li4—O33viii | 120.1 (3) |
Li2iii—O41—Yb1iii | 115.2 (3) | O31—Li4—O24 | 107.2 (4) |
S4—O42—Li1 | 128.3 (3) | O33viii—Li4—O24 | 102.8 (3) |
S4—O44—Li2ix | 125.1 (3) | O31—Li4—O32iv | 111.6 (3) |
S4—O44—Li2 | 122.0 (3) | O33viii—Li4—O32iv | 107.6 (4) |
Li2ix—O44—Li2 | 109.8 (3) | O24—Li4—O32iv | 106.5 (3) |
O11i—Li1—O42 | 120.2 (4) | O31—Li4—S2 | 94.0 (3) |
O11i—Li1—O13ii | 109.3 (4) | O33viii—Li4—S2 | 126.6 (3) |
O42—Li1—O13ii | 111.2 (4) | O24—Li4—S2 | 24.01 (13) |
O11i—Li1—O13 | 102.6 (4) | O32iv—Li4—S2 | 93.9 (2) |
O42—Li1—O13 | 105.5 (4) | O31—Li4—Li3iv | 114.3 (3) |
O13ii—Li1—O13 | 106.9 (3) | O33viii—Li4—Li3iv | 123.7 (3) |
O11i—Li1—S1 | 126.6 (3) | O24—Li4—Li3iv | 73.1 (2) |
O42—Li1—S1 | 92.5 (3) | O32iv—Li4—Li3iv | 34.47 (19) |
O13ii—Li1—S1 | 93.7 (3) | S2—Li4—Li3iv | 59.59 (16) |
O13—Li1—S1 | 24.12 (14) | O31—Li4—Li3viii | 111.5 (3) |
O11i—Li1—S1ii | 90.1 (3) | O33viii—Li4—Li3viii | 71.1 (2) |
O42—Li1—S1ii | 111.9 (3) | O24—Li4—Li3viii | 34.71 (18) |
O13ii—Li1—S1ii | 23.96 (13) | O32iv—Li4—Li3viii | 129.3 (3) |
O13—Li1—S1ii | 126.7 (3) | S2—Li4—Li3viii | 57.96 (15) |
S1—Li1—S1ii | 117.2 (2) | Li3iv—Li4—Li3viii | 102.3 (2) |
O11i—Li1—Li1ii | 125.3 (4) | O31—Li4—Yb3iv | 175.9 (3) |
O42—Li1—Li1ii | 112.8 (4) | O33viii—Li4—Yb3iv | 56.1 (2) |
O13ii—Li1—Li1ii | 34.03 (11) | O24—Li4—Yb3iv | 73.2 (2) |
O13—Li1—Li1ii | 73.9 (3) | O32iv—Li4—Yb3iv | 71.9 (2) |
S1—Li1—Li1ii | 59.8 (2) | S2—Li4—Yb3iv | 87.77 (18) |
S1ii—Li1—Li1ii | 57.36 (15) | Li3iv—Li4—Yb3iv | 69.78 (18) |
O11i—Li1—Li1i | 71.1 (2) | Li3viii—Li4—Yb3iv | 66.38 (18) |
O42—Li1—Li1i | 110.8 (3) | O31—Li4—Yb2vii | 53.7 (2) |
O13ii—Li1—Li1i | 129.3 (4) | O33viii—Li4—Yb2vii | 101.0 (3) |
O13—Li1—Li1i | 34.0 (2) | O24—Li4—Yb2vii | 63.0 (2) |
S1—Li1—Li1i | 57.5 (2) | O32iv—Li4—Yb2vii | 151.2 (3) |
S1ii—Li1—Li1i | 137.1 (4) | S2—Li4—Yb2vii | 65.70 (15) |
Li1ii—Li1—Li1i | 102.4 (4) | Li3iv—Li4—Yb2vii | 122.9 (2) |
O11i—Li1—Yb1i | 57.5 (2) | Li3viii—Li4—Yb2vii | 57.83 (17) |
O42—Li1—Yb1i | 177.3 (3) | Yb3iv—Li4—Yb2vii | 124.17 (19) |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1, y−1/2, −z+1/2; (iii) x, y+1, z; (iv) −x+1, −y+1, −z; (v) x+1, y, z; (vi) x+1, y−1, z; (vii) x, y−1, z; (viii) −x+1, −y, −z; (ix) −x, y+1/2, −z+1/2; (x) −x, y−1/2, −z+1/2; (xi) x−1, y, z. |