Octa­aqua­ytterbium(III) tris­(3-carb­oxy-4-hydroxy­benzene­sulfonate) monohydrate

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.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](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

---

Computing details

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

Crystal data

[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) Å^3

Data collection

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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.052	H-atom parameters constrained
S = 0.91	w = 1/[σ^2(Fo^2) + (0.0265P)^2] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11O···O16^i	0.89 (4)	2.04 (4)	2.904 (4)	165 (6)
O1—H12O···O31^ii	0.94 (4)	1.78 (4)	2.707 (5)	171 (7)
O2—H21O···O11^iii	0.90 (4)	1.88 (4)	2.778 (4)	176 (7)
O2—H22O···O33A^i	0.93 (4)	1.73 (5)	2.63 (2)	163 (7)
O2—H22O···O33^i	0.93 (4)	1.88 (5)	2.690 (10)	145 (6)
O3—H31O···O12^iv	0.95 (4)	1.81 (4)	2.757 (4)	171 (6)
O3—H32O···O14^v	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···O13^vi	0.95 (4)	1.75 (4)	2.701 (4)	176 (7)
O5—H51O···O32A^i	0.91 (4)	2.08 (6)	2.95 (4)	158 (6)
O5—H51O···O33^i	0.91 (4)	2.07 (6)	2.777 (15)	133 (6)
O5—H52O···O22^iv	0.93 (4)	1.97 (4)	2.862 (4)	161 (6)
O6—H61O···O24^vii	0.91 (4)	2.03 (5)	2.866 (4)	152 (6)
O6—H62O···O32^ii	0.92 (4)	1.77 (4)	2.688 (11)	175 (7)
O6—H62O···O32A^ii	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···O21^iv	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···O34^vii	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···O21^viii	0.82	1.84	2.640 (4)	165
O16—H16O···O14	0.82	1.88	2.600 (4)	146
O25—H25O···O22^ix	0.82	1.94	2.689 (4)	151
O26—H26O···O24	0.82	1.94	2.654 (4)	146
O35—H35O···O32^x	0.82	1.93	2.700 (6)	156
O35—H35O···O32A^x	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.