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The title compound, [Yb(H2O)8](C7H5O6S)3·H2O, was synthesized by the reaction of Yb2O3 with 5-sulfosalicylic acid in water. The compound contains Yb(H2O)83+ monomers; the 3-carboxy-4-hydroxybenzenesulfonate anions do not coordinate to ytterbium, but act as counter-anions.
Supporting information
CCDC reference: 610927
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å
- Disorder in main residue
- R factor = 0.025
- wR factor = 0.052
- Data-to-parameter ratio = 11.5
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.94
Alert level C
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.93
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT213_ALERT_2_C Atom O32A has ADP max/min Ratio ............. 3.20 prolat
PLAT213_ALERT_2_C Atom O33A has ADP max/min Ratio ............. 3.20 prolat
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.03 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Yb1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S3
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.66
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.72
PLAT301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc.
PLAT417_ALERT_2_C Short Inter D-H..H-D H71O .. H92O .. 2.12 Ang.
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
12 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
7 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS Software (Stoe & Cie, 1998); cell refinement: IPDS Software; data reduction: IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.
Octaaquaytterbium(III) tris(3-carboxy-4-hydroxybenzenesulfonate) monohydrate
top
Crystal data top
[Yb(H2O)8](C7H5O6S)3·H2O | Z = 2 |
Mr = 986.69 | F(000) = 986 |
Triclinic, P1 | Dx = 1.913 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.523 (2) Å | Cell parameters from 8000 reflections |
b = 12.445 (4) Å | θ = 2.2–25.9° |
c = 19.475 (6) Å | µ = 3.02 mm−1 |
α = 74.74 (3)° | T = 298 K |
β = 82.28 (3)° | Needle, colourless |
γ = 77.68 (3)° | 0.59 × 0.07 × 0.07 mm |
V = 1712.6 (8) Å3 | |
Data collection top
Stoe IPDS diffractometer | 5073 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.051 |
Graphite monochromator | θmax = 25.9°, θmin = 2.2° |
Detector resolution: 0 pixels mm-1 | h = −8→8 |
φ scans | k = −15→15 |
24267 measured reflections | l = −23→23 |
6202 independent reflections | |
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)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.052 | H-atom parameters constrained |
S = 0.91 | w = 1/[σ2(Fo2) + (0.0265P)2] where P = (Fo2 + 2Fc2)/3 |
6202 reflections | (Δ/σ)max = 0.001 |
541 parameters | Δρmax = 0.87 e Å−3 |
27 restraints | Δρmin = −0.84 e Å−3 |
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 >
2σ(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) |
Yb1 | 1.00171 (3) | 0.049437 (14) | 0.319927 (9) | 0.02141 (5) | |
O1 | 0.9919 (5) | −0.1391 (2) | 0.32775 (15) | 0.0360 (7) | |
O2 | 1.2711 (4) | −0.0542 (2) | 0.36514 (14) | 0.0314 (6) | |
O3 | 1.0939 (4) | 0.1649 (2) | 0.38045 (15) | 0.0362 (7) | |
O4 | 0.9077 (5) | −0.0137 (3) | 0.43968 (14) | 0.0464 (9) | |
O5 | 1.2342 (5) | 0.1176 (2) | 0.23852 (16) | 0.0417 (8) | |
O6 | 0.9462 (5) | 0.0427 (3) | 0.20600 (14) | 0.0433 (8) | |
O7 | 0.8523 (5) | 0.2310 (2) | 0.28060 (18) | 0.0463 (8) | |
O8 | 0.6874 (5) | 0.0433 (3) | 0.32423 (17) | 0.0455 (8) | |
O9 | 0.5823 (6) | 0.2518 (4) | 0.2045 (2) | 0.0748 (13) | |
H11O | 1.066 (8) | −0.199 (5) | 0.352 (3) | 0.112* | |
H12O | 0.892 (7) | −0.152 (6) | 0.309 (4) | 0.112* | |
H21O | 1.288 (10) | −0.087 (5) | 0.412 (2) | 0.112* | |
H22O | 1.351 (9) | −0.093 (5) | 0.335 (3) | 0.112* | |
H31O | 1.217 (6) | 0.158 (6) | 0.390 (4) | 0.112* | |
H32O | 1.029 (8) | 0.230 (4) | 0.395 (4) | 0.112* | |
H41O | 0.853 (9) | 0.044 (4) | 0.464 (3) | 0.112* | |
H42O | 0.819 (9) | −0.060 (5) | 0.446 (4) | 0.112* | |
H51O | 1.344 (7) | 0.071 (5) | 0.233 (4) | 0.112* | |
H52O | 1.239 (10) | 0.191 (4) | 0.212 (3) | 0.112* | |
H61O | 1.008 (9) | 0.082 (5) | 0.168 (3) | 0.112* | |
H62O | 0.849 (8) | 0.017 (6) | 0.195 (4) | 0.112* | |
H71O | 0.767 (8) | 0.245 (6) | 0.246 (3) | 0.112* | |
H72O | 0.913 (9) | 0.288 (5) | 0.275 (4) | 0.112* | |
H81O | 0.590 (8) | 0.079 (5) | 0.348 (3) | 0.112* | |
H82O | 0.755 (9) | 0.101 (5) | 0.297 (3) | 0.112* | |
H91O | 0.591 (10) | 0.253 (6) | 0.157 (2) | 0.112* | |
H92O | 0.500 (9) | 0.317 (5) | 0.215 (3) | 0.112* | |
S1 | 0.46796 (14) | 0.18670 (7) | 0.48164 (5) | 0.0248 (2) | |
O11 | 0.6607 (4) | 0.1615 (2) | 0.49411 (13) | 0.0302 (6) | |
O12 | 0.4387 (4) | 0.1580 (2) | 0.41672 (15) | 0.0380 (7) | |
O13 | 0.3560 (4) | 0.1377 (2) | 0.54406 (15) | 0.0395 (7) | |
O14 | 0.0911 (5) | 0.6512 (2) | 0.56230 (15) | 0.0439 (8) | |
O15 | 0.1268 (5) | 0.4747 (2) | 0.63188 (14) | 0.0472 (9) | |
H15O | 0.0736 | 0.5082 | 0.6620 | 0.071* | |
O16 | 0.2088 (5) | 0.6825 (2) | 0.42807 (15) | 0.0473 (9) | |
H16O | 0.1576 | 0.7007 | 0.4643 | 0.071* | |
C11 | 0.3934 (6) | 0.3354 (3) | 0.46768 (19) | 0.0251 (9) | |
C12 | 0.3053 (6) | 0.3811 (3) | 0.52297 (18) | 0.0256 (9) | |
H12 | 0.2886 | 0.3340 | 0.5682 | 0.031* | |
C13 | 0.2407 (6) | 0.4980 (3) | 0.51158 (18) | 0.0255 (9) | |
C14 | 0.2687 (6) | 0.5681 (3) | 0.4429 (2) | 0.0308 (9) | |
C15 | 0.3595 (7) | 0.5212 (3) | 0.38801 (19) | 0.0363 (11) | |
H15 | 0.3790 | 0.5678 | 0.3428 | 0.044* | |
C16 | 0.4215 (6) | 0.4058 (3) | 0.39983 (19) | 0.0326 (10) | |
H16 | 0.4820 | 0.3749 | 0.3626 | 0.039* | |
C17 | 0.1467 (6) | 0.5486 (3) | 0.5702 (2) | 0.0306 (9) | |
S2 | 0.15238 (15) | 0.43018 (7) | 0.21159 (4) | 0.0296 (2) | |
O21 | −0.0127 (5) | 0.4266 (2) | 0.26154 (14) | 0.0418 (8) | |
O22 | 0.1636 (4) | 0.3524 (2) | 0.16579 (13) | 0.0343 (7) | |
O23 | 0.3159 (5) | 0.4113 (3) | 0.24781 (16) | 0.0503 (9) | |
O24 | −0.0297 (6) | 0.8289 (2) | −0.06420 (14) | 0.0574 (10) | |
O25 | −0.0078 (6) | 0.6436 (2) | −0.04849 (15) | 0.0590 (11) | |
H25O | −0.0354 | 0.6634 | −0.0899 | 0.089* | |
O26 | 0.0285 (6) | 0.9020 (2) | 0.04568 (17) | 0.0686 (13) | |
H26O | 0.0029 | 0.9084 | 0.0050 | 0.103* | |
C21 | 0.1256 (6) | 0.5689 (3) | 0.15740 (18) | 0.0265 (9) | |
C22 | 0.0840 (6) | 0.5935 (3) | 0.08762 (18) | 0.0281 (9) | |
H22 | 0.0782 | 0.5352 | 0.0669 | 0.034* | |
C23 | 0.0505 (6) | 0.7056 (3) | 0.04778 (18) | 0.0289 (9) | |
C24 | 0.0607 (7) | 0.7920 (3) | 0.0799 (2) | 0.0365 (11) | |
C25 | 0.1075 (7) | 0.7666 (3) | 0.1501 (2) | 0.0375 (11) | |
H25 | 0.1181 | 0.8243 | 0.1706 | 0.045* | |
C26 | 0.1376 (6) | 0.6565 (3) | 0.18854 (19) | 0.0323 (10) | |
H26 | 0.1662 | 0.6394 | 0.2357 | 0.039* | |
C27 | 0.0015 (7) | 0.7324 (3) | −0.02676 (19) | 0.0359 (11) | |
S3 | 0.60095 (17) | 0.86503 (9) | 0.21609 (5) | 0.0361 (3) | |
O31 | 0.7270 (6) | 0.8070 (3) | 0.26876 (18) | 0.0625 (11) | |
O32 | 0.675 (2) | 0.9654 (6) | 0.1689 (6) | 0.051 (4) | 0.74 (4) |
O33 | 0.4190 (10) | 0.8984 (16) | 0.2404 (9) | 0.075 (5) | 0.74 (4) |
O32A | 0.558 (8) | 0.9749 (14) | 0.1829 (8) | 0.057 (10) | 0.26 (4) |
O33A | 0.443 (6) | 0.833 (3) | 0.2709 (16) | 0.075 (9) | 0.26 (4) |
O34 | 0.4612 (6) | 0.7356 (3) | −0.06312 (16) | 0.0575 (10) | |
O35 | 0.4520 (7) | 0.9054 (3) | −0.04429 (17) | 0.0725 (13) | |
H35O | 0.4206 | 0.9265 | −0.0852 | 0.109* | |
O36 | 0.5739 (5) | 0.5538 (3) | 0.03787 (17) | 0.0562 (10) | |
H36O | 0.5413 | 0.5882 | −0.0018 | 0.084* | |
C31 | 0.6013 (6) | 0.7741 (3) | 0.16017 (19) | 0.0279 (9) | |
C32 | 0.5485 (6) | 0.8184 (3) | 0.09185 (19) | 0.0311 (9) | |
H32 | 0.5190 | 0.8966 | 0.0744 | 0.037* | |
C33 | 0.5388 (6) | 0.7464 (3) | 0.04820 (19) | 0.0297 (9) | |
C34 | 0.5824 (6) | 0.6290 (3) | 0.0759 (2) | 0.0347 (10) | |
C35 | 0.6353 (7) | 0.5858 (3) | 0.1446 (2) | 0.0391 (11) | |
H35 | 0.6647 | 0.5077 | 0.1626 | 0.047* | |
C36 | 0.6448 (6) | 0.6572 (3) | 0.1866 (2) | 0.0336 (10) | |
H36 | 0.6803 | 0.6273 | 0.2328 | 0.040* | |
C37 | 0.4812 (7) | 0.7941 (4) | −0.0245 (2) | 0.0394 (11) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Yb1 | 0.02389 (10) | 0.02284 (8) | 0.01850 (7) | −0.00327 (6) | −0.00470 (5) | −0.00615 (5) |
O1 | 0.046 (2) | 0.0266 (14) | 0.0377 (16) | −0.0058 (13) | −0.0158 (14) | −0.0061 (12) |
O2 | 0.0285 (19) | 0.0354 (15) | 0.0278 (13) | 0.0026 (12) | −0.0060 (12) | −0.0081 (11) |
O3 | 0.030 (2) | 0.0360 (16) | 0.0493 (17) | 0.0011 (13) | −0.0092 (14) | −0.0255 (13) |
O4 | 0.060 (3) | 0.065 (2) | 0.0251 (14) | −0.0344 (18) | 0.0093 (14) | −0.0184 (14) |
O5 | 0.040 (2) | 0.0344 (16) | 0.0405 (16) | −0.0043 (14) | 0.0083 (14) | 0.0006 (13) |
O6 | 0.067 (3) | 0.0471 (18) | 0.0206 (13) | −0.0194 (16) | −0.0096 (14) | −0.0074 (12) |
O7 | 0.049 (3) | 0.0311 (16) | 0.061 (2) | 0.0023 (14) | −0.0286 (17) | −0.0107 (14) |
O8 | 0.037 (2) | 0.0502 (19) | 0.056 (2) | −0.0084 (15) | −0.0007 (15) | −0.0268 (16) |
O9 | 0.064 (3) | 0.101 (3) | 0.059 (2) | 0.032 (2) | −0.038 (2) | −0.039 (2) |
S1 | 0.0258 (6) | 0.0239 (4) | 0.0276 (5) | −0.0036 (4) | −0.0035 (4) | −0.0114 (4) |
O11 | 0.0219 (18) | 0.0321 (14) | 0.0359 (14) | 0.0001 (11) | −0.0083 (11) | −0.0084 (11) |
O12 | 0.035 (2) | 0.0427 (16) | 0.0474 (17) | 0.0019 (13) | −0.0132 (14) | −0.0326 (14) |
O13 | 0.040 (2) | 0.0330 (15) | 0.0449 (17) | −0.0148 (13) | 0.0106 (14) | −0.0094 (12) |
O14 | 0.059 (2) | 0.0265 (15) | 0.0436 (17) | 0.0024 (14) | 0.0044 (15) | −0.0166 (12) |
O15 | 0.072 (3) | 0.0315 (15) | 0.0318 (15) | −0.0028 (15) | 0.0136 (15) | −0.0119 (12) |
O16 | 0.079 (3) | 0.0238 (14) | 0.0332 (15) | 0.0043 (15) | −0.0114 (15) | −0.0053 (12) |
C11 | 0.026 (3) | 0.0260 (19) | 0.0274 (19) | −0.0046 (16) | −0.0067 (16) | −0.0109 (15) |
C12 | 0.028 (3) | 0.0272 (19) | 0.0231 (18) | −0.0052 (16) | −0.0008 (15) | −0.0092 (15) |
C13 | 0.029 (3) | 0.0232 (18) | 0.0244 (18) | −0.0026 (16) | −0.0060 (16) | −0.0063 (14) |
C14 | 0.039 (3) | 0.0223 (18) | 0.032 (2) | −0.0003 (17) | −0.0129 (18) | −0.0066 (15) |
C15 | 0.053 (3) | 0.032 (2) | 0.0208 (18) | −0.0058 (19) | −0.0074 (18) | −0.0012 (16) |
C16 | 0.040 (3) | 0.039 (2) | 0.0198 (18) | −0.0043 (19) | −0.0031 (17) | −0.0107 (16) |
C17 | 0.027 (3) | 0.032 (2) | 0.035 (2) | −0.0048 (17) | −0.0006 (17) | −0.0129 (17) |
S2 | 0.0447 (7) | 0.0248 (5) | 0.0173 (4) | 0.0028 (4) | −0.0085 (4) | −0.0060 (3) |
O21 | 0.065 (3) | 0.0287 (14) | 0.0282 (14) | −0.0084 (14) | 0.0100 (14) | −0.0080 (11) |
O22 | 0.054 (2) | 0.0275 (14) | 0.0208 (12) | 0.0018 (13) | −0.0091 (12) | −0.0088 (10) |
O23 | 0.067 (3) | 0.0438 (17) | 0.0418 (17) | 0.0073 (16) | −0.0335 (16) | −0.0124 (14) |
O24 | 0.109 (3) | 0.0336 (17) | 0.0241 (15) | −0.0119 (18) | −0.0150 (16) | 0.0060 (13) |
O25 | 0.115 (4) | 0.0383 (17) | 0.0290 (15) | −0.0174 (18) | −0.0334 (18) | −0.0015 (13) |
O26 | 0.140 (4) | 0.0251 (16) | 0.0386 (17) | −0.0162 (19) | −0.022 (2) | 0.0026 (13) |
C21 | 0.032 (3) | 0.0269 (19) | 0.0195 (17) | −0.0021 (16) | −0.0046 (15) | −0.0061 (14) |
C22 | 0.035 (3) | 0.0278 (19) | 0.0230 (18) | −0.0050 (17) | −0.0050 (16) | −0.0079 (15) |
C23 | 0.039 (3) | 0.0281 (19) | 0.0192 (17) | −0.0091 (17) | −0.0033 (16) | −0.0029 (14) |
C24 | 0.054 (3) | 0.025 (2) | 0.029 (2) | −0.0092 (19) | −0.0019 (19) | −0.0029 (16) |
C25 | 0.054 (3) | 0.033 (2) | 0.030 (2) | −0.012 (2) | −0.0069 (19) | −0.0113 (17) |
C26 | 0.047 (3) | 0.032 (2) | 0.0209 (18) | −0.0101 (18) | −0.0062 (17) | −0.0072 (16) |
C27 | 0.054 (3) | 0.031 (2) | 0.0223 (19) | −0.008 (2) | −0.0042 (18) | −0.0046 (16) |
S3 | 0.0462 (8) | 0.0394 (6) | 0.0291 (5) | −0.0026 (5) | −0.0107 (5) | −0.0199 (4) |
O31 | 0.087 (3) | 0.055 (2) | 0.059 (2) | −0.0076 (19) | −0.042 (2) | −0.0230 (17) |
O32 | 0.094 (9) | 0.035 (3) | 0.033 (4) | −0.027 (4) | −0.024 (5) | −0.005 (2) |
O33 | 0.041 (4) | 0.111 (11) | 0.096 (8) | 0.004 (5) | −0.001 (4) | −0.082 (9) |
O32A | 0.11 (3) | 0.043 (8) | 0.023 (6) | −0.021 (11) | 0.019 (10) | −0.021 (6) |
O33A | 0.118 (19) | 0.056 (16) | 0.060 (13) | −0.045 (14) | 0.060 (12) | −0.041 (12) |
O34 | 0.092 (3) | 0.055 (2) | 0.0378 (17) | −0.0137 (19) | −0.0220 (18) | −0.0239 (15) |
O35 | 0.143 (4) | 0.0428 (19) | 0.0415 (18) | −0.020 (2) | −0.045 (2) | −0.0060 (15) |
O36 | 0.084 (3) | 0.0395 (17) | 0.057 (2) | −0.0048 (17) | −0.0266 (18) | −0.0281 (15) |
C31 | 0.029 (3) | 0.034 (2) | 0.0255 (19) | −0.0081 (17) | −0.0040 (16) | −0.0122 (16) |
C32 | 0.036 (3) | 0.031 (2) | 0.031 (2) | −0.0063 (18) | −0.0079 (17) | −0.0133 (16) |
C33 | 0.034 (3) | 0.035 (2) | 0.0248 (18) | −0.0079 (17) | −0.0060 (16) | −0.0125 (16) |
C34 | 0.036 (3) | 0.036 (2) | 0.040 (2) | −0.0092 (18) | −0.0084 (19) | −0.0197 (18) |
C35 | 0.046 (3) | 0.029 (2) | 0.045 (2) | −0.0040 (19) | −0.010 (2) | −0.0124 (18) |
C36 | 0.035 (3) | 0.038 (2) | 0.030 (2) | −0.0082 (18) | −0.0103 (17) | −0.0077 (17) |
C37 | 0.050 (3) | 0.043 (2) | 0.032 (2) | −0.011 (2) | −0.0060 (19) | −0.0160 (19) |
Geometric parameters (Å, º) top
Yb1—O7 | 2.278 (3) | C15—C16 | 1.378 (5) |
Yb1—O2 | 2.305 (3) | C15—H15 | 0.9300 |
Yb1—O4 | 2.321 (3) | C16—H16 | 0.9300 |
Yb1—O1 | 2.328 (3) | S2—O23 | 1.445 (3) |
Yb1—O6 | 2.338 (3) | S2—O22 | 1.462 (3) |
Yb1—O5 | 2.339 (3) | S2—O21 | 1.472 (3) |
Yb1—O3 | 2.339 (3) | S2—C21 | 1.756 (4) |
Yb1—O8 | 2.372 (4) | O24—C27 | 1.222 (5) |
Yb1—H82O | 1.91 (7) | O25—C27 | 1.300 (5) |
O1—H11O | 0.89 (4) | O25—H25O | 0.8200 |
O1—H12O | 0.94 (4) | O26—C24 | 1.341 (5) |
O2—H21O | 0.90 (4) | O26—H26O | 0.8200 |
O2—H22O | 0.93 (4) | C21—C22 | 1.376 (5) |
O3—H31O | 0.95 (4) | C21—C26 | 1.403 (5) |
O3—H32O | 0.95 (4) | C22—C23 | 1.394 (5) |
O4—H41O | 0.96 (4) | C22—H22 | 0.9300 |
O4—H42O | 0.95 (4) | C23—C24 | 1.398 (5) |
O5—H51O | 0.91 (4) | C23—C27 | 1.480 (5) |
O5—H52O | 0.93 (4) | C24—C25 | 1.397 (6) |
O6—H61O | 0.91 (4) | C25—C26 | 1.365 (5) |
O6—H62O | 0.92 (4) | C25—H25 | 0.9300 |
O7—H71O | 0.94 (4) | C26—H26 | 0.9300 |
O7—H72O | 0.90 (4) | S3—O32A | 1.340 (18) |
O8—H81O | 0.91 (4) | S3—O33 | 1.399 (8) |
O8—H82O | 0.97 (4) | S3—O31 | 1.433 (3) |
O9—H91O | 0.92 (4) | S3—O32 | 1.505 (10) |
O9—H92O | 0.96 (4) | S3—O33A | 1.533 (17) |
S1—O13 | 1.454 (3) | S3—C31 | 1.764 (4) |
S1—O11 | 1.456 (3) | O34—C37 | 1.218 (5) |
S1—O12 | 1.456 (3) | O35—C37 | 1.314 (5) |
S1—C11 | 1.773 (4) | O35—H35O | 0.8200 |
O14—C17 | 1.231 (5) | O36—C34 | 1.353 (4) |
O15—C17 | 1.319 (5) | O36—H36O | 0.8200 |
O15—H15O | 0.8200 | C31—C32 | 1.376 (5) |
O16—C14 | 1.363 (4) | C31—C36 | 1.392 (5) |
O16—H16O | 0.8200 | C32—C33 | 1.406 (5) |
C11—C12 | 1.376 (5) | C32—H32 | 0.9300 |
C11—C16 | 1.398 (5) | C33—C34 | 1.401 (6) |
C12—C13 | 1.400 (5) | C33—C37 | 1.469 (5) |
C12—H12 | 0.9300 | C34—C35 | 1.383 (6) |
C13—C14 | 1.408 (5) | C35—C36 | 1.374 (5) |
C13—C17 | 1.474 (5) | C35—H35 | 0.9300 |
C14—C15 | 1.383 (5) | C36—H36 | 0.9300 |
| | | |
O7—Yb1—O2 | 142.00 (12) | O16—C14—C15 | 118.0 (3) |
O7—Yb1—O4 | 108.23 (13) | O16—C14—C13 | 122.0 (3) |
O2—Yb1—O4 | 78.50 (12) | C15—C14—C13 | 120.0 (3) |
O7—Yb1—O1 | 143.45 (12) | C16—C15—C14 | 120.4 (3) |
O2—Yb1—O1 | 74.27 (11) | C16—C15—H15 | 119.8 |
O4—Yb1—O1 | 78.15 (11) | C14—C15—H15 | 119.8 |
O7—Yb1—O6 | 80.57 (12) | C15—C16—C11 | 120.1 (3) |
O2—Yb1—O6 | 118.03 (11) | C15—C16—H16 | 120.0 |
O4—Yb1—O6 | 141.44 (12) | C11—C16—H16 | 120.0 |
O1—Yb1—O6 | 74.21 (10) | O14—C17—O15 | 122.8 (3) |
O7—Yb1—O5 | 81.92 (13) | O14—C17—C13 | 122.8 (4) |
O2—Yb1—O5 | 74.39 (11) | O15—C17—C13 | 114.4 (3) |
O4—Yb1—O5 | 145.51 (12) | O23—S2—O22 | 112.82 (18) |
O1—Yb1—O5 | 113.65 (11) | O23—S2—O21 | 112.25 (19) |
O6—Yb1—O5 | 71.71 (13) | O22—S2—O21 | 110.44 (18) |
O7—Yb1—O3 | 71.21 (11) | O23—S2—C21 | 107.0 (2) |
O2—Yb1—O3 | 75.45 (10) | O22—S2—C21 | 108.10 (15) |
O4—Yb1—O3 | 73.53 (11) | O21—S2—C21 | 105.82 (18) |
O1—Yb1—O3 | 141.85 (10) | C27—O25—H25O | 109.5 |
O6—Yb1—O3 | 141.90 (11) | C24—O26—H26O | 109.5 |
O5—Yb1—O3 | 79.29 (12) | C22—C21—C26 | 120.1 (3) |
O7—Yb1—O8 | 72.84 (13) | C22—C21—S2 | 121.9 (3) |
O2—Yb1—O8 | 141.95 (11) | C26—C21—S2 | 117.9 (3) |
O4—Yb1—O8 | 73.94 (12) | C21—C22—C23 | 120.3 (3) |
O1—Yb1—O8 | 74.79 (12) | C21—C22—H22 | 119.8 |
O6—Yb1—O8 | 73.23 (12) | C23—C22—H22 | 119.8 |
O5—Yb1—O8 | 139.47 (12) | C22—C23—C24 | 118.9 (3) |
O3—Yb1—O8 | 119.66 (11) | C22—C23—C27 | 120.3 (3) |
O7—Yb1—H82O | 51.6 (15) | C24—C23—C27 | 120.8 (3) |
O2—Yb1—H82O | 165.0 (14) | O26—C24—C25 | 116.6 (3) |
O4—Yb1—H82O | 91.0 (16) | O26—C24—C23 | 122.7 (4) |
O1—Yb1—H82O | 93.2 (17) | C25—C24—C23 | 120.7 (3) |
O6—Yb1—H82O | 64.6 (19) | C26—C25—C24 | 119.5 (4) |
O5—Yb1—H82O | 119.1 (15) | C26—C25—H25 | 120.2 |
O3—Yb1—H82O | 112.1 (19) | C24—C25—H25 | 120.2 |
O8—Yb1—H82O | 23.1 (14) | C25—C26—C21 | 120.5 (3) |
Yb1—O1—H11O | 125 (4) | C25—C26—H26 | 119.8 |
Yb1—O1—H12O | 116 (4) | C21—C26—H26 | 119.8 |
H11O—O1—H12O | 118 (5) | O24—C27—O25 | 123.0 (4) |
Yb1—O2—H21O | 126 (5) | O24—C27—C23 | 123.3 (4) |
Yb1—O2—H22O | 117 (4) | O25—C27—C23 | 113.7 (3) |
H21O—O2—H22O | 111 (5) | O32A—S3—O33 | 75.2 (14) |
Yb1—O3—H31O | 123 (4) | O32A—S3—O31 | 131.3 (19) |
Yb1—O3—H32O | 131 (4) | O33—S3—O31 | 117.5 (7) |
H31O—O3—H32O | 106 (4) | O33—S3—O32 | 110.3 (5) |
Yb1—O4—H41O | 116 (4) | O31—S3—O32 | 108.4 (4) |
Yb1—O4—H42O | 112 (4) | O32A—S3—O33A | 108.5 (11) |
H41O—O4—H42O | 105 (5) | O31—S3—O33A | 89.6 (19) |
Yb1—O5—H51O | 120 (4) | O32—S3—O33A | 142.2 (10) |
Yb1—O5—H52O | 129 (4) | O32A—S3—C31 | 112.8 (9) |
H51O—O5—H52O | 110 (5) | O33—S3—C31 | 106.9 (4) |
Yb1—O6—H61O | 118 (4) | O31—S3—C31 | 107.62 (19) |
Yb1—O6—H62O | 125 (4) | O32—S3—C31 | 105.5 (5) |
H61O—O6—H62O | 115 (5) | O33A—S3—C31 | 99.9 (7) |
Yb1—O7—H71O | 118 (4) | C37—O35—H35O | 109.5 |
Yb1—O7—H72O | 119 (5) | C34—O36—H36O | 109.5 |
H71O—O7—H72O | 113 (5) | C32—C31—C36 | 120.0 (3) |
Yb1—O8—H81O | 129 (5) | C32—C31—S3 | 120.1 (3) |
Yb1—O8—H82O | 50 (4) | C36—C31—S3 | 119.9 (3) |
H81O—O8—H82O | 107 (5) | C31—C32—C33 | 120.5 (4) |
H91O—O9—H92O | 111 (5) | C31—C32—H32 | 119.8 |
O13—S1—O11 | 112.14 (18) | C33—C32—H32 | 119.8 |
O13—S1—O12 | 113.53 (19) | C34—C33—C32 | 118.6 (3) |
O11—S1—O12 | 111.66 (17) | C34—C33—C37 | 121.1 (3) |
O13—S1—C11 | 105.08 (18) | C32—C33—C37 | 120.2 (3) |
O11—S1—C11 | 107.55 (18) | O36—C34—C35 | 117.5 (4) |
O12—S1—C11 | 106.29 (17) | O36—C34—C33 | 122.4 (4) |
C17—O15—H15O | 109.5 | C35—C34—C33 | 120.2 (3) |
C14—O16—H16O | 109.5 | C36—C35—C34 | 120.6 (4) |
C12—C11—C16 | 120.1 (3) | C36—C35—H35 | 119.7 |
C12—C11—S1 | 120.2 (3) | C34—C35—H35 | 119.7 |
C16—C11—S1 | 119.7 (3) | C35—C36—C31 | 120.2 (4) |
C11—C12—C13 | 120.4 (3) | C35—C36—H36 | 119.9 |
C11—C12—H12 | 119.8 | C31—C36—H36 | 119.9 |
C13—C12—H12 | 119.8 | O34—C37—O35 | 122.7 (4) |
C12—C13—C14 | 119.0 (3) | O34—C37—C33 | 122.9 (4) |
C12—C13—C17 | 121.2 (3) | O35—C37—C33 | 114.4 (3) |
C14—C13—C17 | 119.8 (3) | | |
| | | |
O13—S1—C11—C12 | 22.1 (4) | O26—C24—C25—C26 | 178.4 (5) |
O11—S1—C11—C12 | −97.6 (4) | C23—C24—C25—C26 | −2.2 (7) |
O12—S1—C11—C12 | 142.7 (3) | C24—C25—C26—C21 | 1.4 (7) |
O13—S1—C11—C16 | −156.7 (3) | C22—C21—C26—C25 | 0.2 (7) |
O11—S1—C11—C16 | 83.7 (4) | S2—C21—C26—C25 | −176.2 (4) |
O12—S1—C11—C16 | −36.1 (4) | C22—C23—C27—O24 | 179.9 (5) |
C16—C11—C12—C13 | 1.0 (6) | C24—C23—C27—O24 | 1.1 (7) |
S1—C11—C12—C13 | −177.8 (3) | C22—C23—C27—O25 | 0.8 (6) |
C11—C12—C13—C14 | −0.6 (6) | C24—C23—C27—O25 | −178.0 (4) |
C11—C12—C13—C17 | −179.7 (4) | O32A—S3—C31—C32 | −4 (3) |
C12—C13—C14—O16 | 179.8 (4) | O33—S3—C31—C32 | 76.6 (10) |
C17—C13—C14—O16 | −1.0 (6) | O31—S3—C31—C32 | −156.4 (4) |
C12—C13—C14—C15 | −0.3 (6) | O32—S3—C31—C32 | −40.8 (7) |
C17—C13—C14—C15 | 178.9 (4) | O33A—S3—C31—C32 | 111 (2) |
O16—C14—C15—C16 | −179.4 (4) | O32A—S3—C31—C36 | 180 (3) |
C13—C14—C15—C16 | 0.7 (7) | O33—S3—C31—C36 | −99.7 (10) |
C14—C15—C16—C11 | −0.3 (7) | O31—S3—C31—C36 | 27.3 (4) |
C12—C11—C16—C15 | −0.6 (6) | O32—S3—C31—C36 | 142.9 (7) |
S1—C11—C16—C15 | 178.2 (3) | O33A—S3—C31—C36 | −65 (2) |
C12—C13—C17—O14 | 178.6 (4) | C36—C31—C32—C33 | −0.3 (7) |
C14—C13—C17—O14 | −0.5 (7) | S3—C31—C32—C33 | −176.5 (3) |
C12—C13—C17—O15 | −1.4 (6) | C31—C32—C33—C34 | 0.5 (6) |
C14—C13—C17—O15 | 179.4 (4) | C31—C32—C33—C37 | 179.6 (4) |
O23—S2—C21—C22 | 134.2 (4) | C32—C33—C34—O36 | 179.0 (4) |
O22—S2—C21—C22 | 12.4 (4) | C37—C33—C34—O36 | −0.1 (7) |
O21—S2—C21—C22 | −105.9 (4) | C32—C33—C34—C35 | −0.6 (7) |
O23—S2—C21—C26 | −49.4 (4) | C37—C33—C34—C35 | −179.6 (5) |
O22—S2—C21—C26 | −171.2 (3) | O36—C34—C35—C36 | −179.2 (4) |
O21—S2—C21—C26 | 70.5 (4) | C33—C34—C35—C36 | 0.4 (7) |
C26—C21—C22—C23 | −1.1 (7) | C34—C35—C36—C31 | −0.1 (7) |
S2—C21—C22—C23 | 175.2 (3) | C32—C31—C36—C35 | 0.1 (7) |
C21—C22—C23—C24 | 0.3 (6) | S3—C31—C36—C35 | 176.3 (4) |
C21—C22—C23—C27 | −178.6 (4) | C34—C33—C37—O34 | 3.0 (8) |
C22—C23—C24—O26 | −179.2 (4) | C32—C33—C37—O34 | −176.0 (5) |
C27—C23—C24—O26 | −0.4 (7) | C34—C33—C37—O35 | −177.3 (4) |
C22—C23—C24—C25 | 1.4 (7) | C32—C33—C37—O35 | 3.6 (7) |
C27—C23—C24—C25 | −179.8 (4) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H11O···O16i | 0.89 (4) | 2.04 (4) | 2.904 (4) | 165 (6) |
O1—H12O···O31ii | 0.94 (4) | 1.78 (4) | 2.707 (5) | 171 (7) |
O2—H21O···O11iii | 0.90 (4) | 1.88 (4) | 2.778 (4) | 176 (7) |
O2—H22O···O33Ai | 0.93 (4) | 1.73 (5) | 2.63 (2) | 163 (7) |
O2—H22O···O33i | 0.93 (4) | 1.88 (5) | 2.690 (10) | 145 (6) |
O3—H31O···O12iv | 0.95 (4) | 1.81 (4) | 2.757 (4) | 171 (6) |
O3—H32O···O14v | 0.95 (4) | 1.88 (4) | 2.825 (4) | 172 (6) |
O4—H41O···O11 | 0.96 (4) | 1.97 (5) | 2.880 (4) | 158 (6) |
O4—H42O···O13vi | 0.95 (4) | 1.75 (4) | 2.701 (4) | 176 (7) |
O5—H51O···O32Ai | 0.91 (4) | 2.08 (6) | 2.95 (4) | 158 (6) |
O5—H51O···O33i | 0.91 (4) | 2.07 (6) | 2.777 (15) | 133 (6) |
O5—H52O···O22iv | 0.93 (4) | 1.97 (4) | 2.862 (4) | 161 (6) |
O6—H61O···O24vii | 0.91 (4) | 2.03 (5) | 2.866 (4) | 152 (6) |
O6—H62O···O32ii | 0.92 (4) | 1.77 (4) | 2.688 (11) | 175 (7) |
O6—H62O···O32Aii | 0.92 (4) | 2.42 (7) | 3.33 (5) | 169 (6) |
O7—H71O···O9 | 0.94 (4) | 1.68 (4) | 2.602 (5) | 164 (7) |
O7—H72O···O21iv | 0.90 (4) | 1.87 (4) | 2.752 (4) | 167 (7) |
O8—H81O···O12 | 0.91 (4) | 1.96 (5) | 2.845 (4) | 163 (7) |
O8—H82O···O7 | 0.97 (4) | 1.85 (5) | 2.762 (5) | 155 (6) |
O8—H82O···O9 | 0.97 (4) | 2.50 (7) | 3.038 (5) | 115 (5) |
O9—H91O···O34vii | 0.92 (4) | 1.88 (5) | 2.776 (4) | 164 (7) |
O9—H92O···O23 | 0.96 (4) | 1.78 (4) | 2.720 (5) | 165 (7) |
O15—H15O···O21viii | 0.82 | 1.84 | 2.640 (4) | 165 |
O16—H16O···O14 | 0.82 | 1.88 | 2.600 (4) | 146 |
O25—H25O···O22ix | 0.82 | 1.94 | 2.689 (4) | 151 |
O26—H26O···O24 | 0.82 | 1.94 | 2.654 (4) | 146 |
O35—H35O···O32x | 0.82 | 1.93 | 2.700 (6) | 156 |
O35—H35O···O32Ax | 0.82 | 1.98 | 2.720 (16) | 150 |
O36—H36O···O34 | 0.82 | 1.93 | 2.644 (5) | 145 |
Symmetry codes: (i) x+1, y−1, z; (ii) x, y−1, z; (iii) −x+2, −y, −z+1; (iv) x+1, y, z; (v) −x+1, −y+1, −z+1; (vi) −x+1, −y, −z+1; (vii) −x+1, −y+1, −z; (viii) −x, −y+1, −z+1; (ix) −x, −y+1, −z; (x) −x+1, −y+2, −z. |
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