The effect of coordinated water on the connectivity of uranium(IV) sulfate x-hydrate: [U(SO₄)₂(H₂O)₅]·H₂O and [U(SO₄)₂(H₂O)₆]·2H₂O, and a comparison with other known structures

Two new solid-state uranium(IV) sulfate x-hydrate complexes (where x is the total number of coordinated plus solvent waters), namely catena-poly[[penta­aqua­uranium(IV)]-di-μ-sulfato-κ⁴O:O′] monohydrate], {[U(SO₄)₂(H₂O)₅]·H₂O}_n, and hexa­aqua­bis­(sulfato-κ²O,O′)uranium(IV) dihydrate, [U(SO₄)₂(H₂O)₆]·2H₂O, have been synthesized, structurally characterized by single-crystal X-ray diffraction and analyzed by vibrational (IR and Raman) spectroscopy. By comparing these structures with those of four other known uranium(IV) sulfate x-hydrates, the effect of additional coordinated water mol­ecules on their structures has been elucidated. As the number of coordinated water mol­ecules increases, the sulfate bonds are displaced, thus changing the binding mode of the sulfate ligands to the uranium centre. As a result, uranium(IV) sulfate x-hydrate changes from being fully crosslinked in three dimensions in the anhydrous compound, through sheet and chain linking in the tetra- and hexa­hydrates, to fully unlinked mol­ecules in the octa- and nona­hydrates. It can be concluded that coordinated waters play an important role in determining the structure and connectivity of U^IV sulfate complexes.

Computing details

For both compounds, data collection: APEX2 (Bruker, 2013); cell refinement: SAINT (Bruker, 2013); data reduction: SAINT (Bruker, 2013); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2012 (Sheldrick, 2008); molecular graphics: CrystalMaker (Palmer, 2013); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

(1) catena-Poly[[pentaaquauranium(IV)]-di-µ-sulfato-κ⁴O:O'] monohydrate]

Crystal data

[U(SO4)2(H2O)5]·H2O	F(000) = 992
Mr = 538.25	Dx = 3.220 Mg m^−3
Monoclinic, I2/a	Mo Kα radiation, λ = 0.71073 Å
a = 7.5190 (2) Å	Cell parameters from 9987 reflections
b = 13.2464 (3) Å	θ = 2.4–30.1°
c = 11.5073 (4) Å	µ = 15.07 mm^−1
β = 104.388 (1)°	T = 296 K
V = 1110.18 (5) Å^3	Rod, purple-green
Z = 4	0.51 × 0.18 × 0.10 mm

Data collection

Bruker X8 APEXII area-detector diffractometer	1638 reflections with I > 2σ(I)
φ and ω scans	Rint = 0.032
Absorption correction: numerical (SADABS; Bruker, 2012)	θmax = 30.1°, θmin = 2.4°
Tmin = 0.016, Tmax = 0.239	h = −10→10
19813 measured reflections	k = −18→18
1642 independent reflections	l = −16→16

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.011	w = 1/[σ^2(Fo^2) + (0.0142P)^2 + 0.6936P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.028	(Δ/σ)max = 0.002
S = 1.31	Δρmax = 1.44 e Å^−3
1642 reflections	Δρmin = −0.93 e Å^−3
104 parameters	Extinction correction: SHELXL2012 (Sheldrick, 2012), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0168 (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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
O1	0.3217 (2)	0.17999 (12)	0.64215 (16)	0.0218 (3)
O2	0.3509 (2)	0.12171 (10)	0.84341 (13)	0.0176 (3)
O3	0.6119 (2)	0.19189 (11)	0.78823 (19)	0.0248 (4)
O4	0.4900 (2)	0.02965 (12)	0.70973 (14)	0.0251 (3)
O5	0.5371 (2)	0.22488 (13)	0.48634 (15)	0.0208 (3)
O6	0.2500	0.49828 (16)	0.5000	0.0189 (4)
O7	−0.0268 (2)	0.37983 (11)	0.36610 (14)	0.0193 (3)
O8	0.2500	−0.0559 (2)	0.5000	0.0420 (7)
S1	0.44809 (6)	0.13012 (3)	0.74577 (4)	0.01226 (8)
U1	0.2500	0.30685 (2)	0.5000	0.00952 (5)
H5A	0.574 (5)	0.242 (3)	0.429 (4)	0.038 (9)*
H5B	0.580 (7)	0.168 (4)	0.500 (4)	0.055 (12)*
H6	0.210 (4)	0.532 (2)	0.539 (3)	0.027 (8)*
H7A	−0.120 (5)	0.352 (3)	0.331 (4)	0.041 (9)*
H7B	0.001 (5)	0.431 (3)	0.313 (4)	0.046 (10)*
H8	0.297 (6)	−0.020 (3)	0.556 (4)	0.065 (13)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0254 (8)	0.0211 (6)	0.0163 (7)	0.0024 (5)	0.0003 (6)	0.0080 (5)
O2	0.0229 (6)	0.0183 (6)	0.0149 (6)	−0.0025 (5)	0.0107 (5)	−0.0010 (5)
O3	0.0154 (7)	0.0343 (10)	0.0253 (9)	−0.0047 (5)	0.0065 (7)	−0.0001 (5)
O4	0.0380 (8)	0.0194 (7)	0.0215 (7)	0.0117 (6)	0.0145 (6)	0.0009 (6)
O5	0.0200 (6)	0.0240 (7)	0.0198 (7)	0.0070 (6)	0.0076 (5)	0.0023 (6)
O6	0.0255 (10)	0.0143 (8)	0.0200 (10)	0.000	0.0113 (8)	0.000
O7	0.0170 (6)	0.0172 (6)	0.0201 (7)	−0.0022 (5)	−0.0023 (5)	0.0044 (5)
O8	0.070 (2)	0.0183 (11)	0.0302 (14)	0.000	−0.0025 (14)	0.000
S1	0.01439 (18)	0.01307 (18)	0.01051 (18)	0.00241 (13)	0.00533 (14)	0.00240 (13)
U1	0.01091 (6)	0.01005 (6)	0.00777 (6)	0.000	0.00263 (3)	0.000

Geometric parameters (Å, º)

O1—S1	1.4827 (16)	O6—H6	0.74 (3)
O1—U1	2.3133 (15)	O7—U1	2.4589 (14)
O2—S1	1.4888 (14)	O7—H7A	0.80 (4)
O2—U1^i	2.3234 (14)	O7—H7B	0.97 (4)
O3—S1	1.4583 (17)	O8—H8	0.80 (4)
O4—S1	1.4517 (15)	U1—O1^ii	2.3133 (15)
O5—U1	2.4563 (15)	U1—O2^i	2.3234 (14)
O5—H5A	0.80 (4)	U1—O2^iii	2.3234 (14)
O5—H5B	0.82 (5)	U1—O5^ii	2.4563 (15)
O6—U1	2.536 (2)	U1—O7^ii	2.4589 (14)
S1—O1—U1	151.93 (11)	O1^ii—U1—O5	71.80 (6)
S1—O2—U1^i	150.57 (8)	O2^i—U1—O5	133.74 (5)
U1—O5—H5A	115 (3)	O2^iii—U1—O5	70.65 (5)
U1—O5—H5B	135 (3)	O5^ii—U1—O5	127.53 (8)
H5A—O5—H5B	102 (4)	O1—U1—O7	137.81 (6)
U1—O6—H6	127 (2)	O1^ii—U1—O7	80.23 (6)
U1—O7—H7A	129 (3)	O2^i—U1—O7	86.40 (5)
U1—O7—H7B	113 (2)	O2^iii—U1—O7	75.08 (5)
H7A—O7—H7B	108 (4)	O5^ii—U1—O7	66.01 (5)
O4—S1—O3	112.63 (10)	O5—U1—O7	138.95 (5)
O4—S1—O1	108.67 (10)	O1—U1—O7^ii	80.23 (6)
O3—S1—O1	109.81 (10)	O1^ii—U1—O7^ii	137.81 (6)
O4—S1—O2	109.22 (9)	O2^i—U1—O7^ii	75.08 (5)
O3—S1—O2	108.73 (10)	O2^iii—U1—O7^ii	86.40 (5)
O1—S1—O2	107.67 (10)	O5^ii—U1—O7^ii	138.95 (5)
O1—U1—O1^ii	86.83 (9)	O5—U1—O7^ii	66.01 (5)
O1—U1—O2^i	79.11 (6)	O7—U1—O7^ii	133.69 (7)
O1^ii—U1—O2^i	141.32 (6)	O1—U1—O6	136.58 (4)
O1—U1—O2^iii	141.32 (6)	O1^ii—U1—O6	136.58 (4)
O1^ii—U1—O2^iii	79.11 (6)	O2^i—U1—O6	65.96 (3)
O2^i—U1—O2^iii	131.93 (7)	O2^iii—U1—O6	65.96 (3)
O1—U1—O5^ii	71.80 (6)	O5^ii—U1—O6	116.23 (4)
O1^ii—U1—O5^ii	70.74 (6)	O5—U1—O6	116.23 (4)
O2^i—U1—O5^ii	70.65 (5)	O7—U1—O6	66.85 (3)
O2^iii—U1—O5^ii	133.74 (5)	O7^ii—U1—O6	66.85 (3)
O1—U1—O5	70.74 (6)
U1—O1—S1—O4	−118.2 (2)	U1^i—O2—S1—O4	163.24 (17)
U1—O1—S1—O3	5.4 (3)	U1^i—O2—S1—O3	40.0 (2)
U1—O1—S1—O2	123.6 (2)	U1^i—O2—S1—O1	−78.94 (19)

Symmetry codes: (i) −x+1/2, −y+1/2, −z+3/2; (ii) −x+1/2, y, −z+1; (iii) x, −y+1/2, z−1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6···O7^iv	0.74 (3)	2.29 (3)	3.0140 (19)	167 (3)
O5—H5A···S1^iii	0.80 (4)	2.69 (4)	3.2985 (17)	134 (3)
O5—H5A···O3^iii	0.80 (4)	1.93 (4)	2.714 (3)	165 (4)
O7—H7A···O3^ii	0.80 (4)	2.54 (4)	3.033 (2)	121 (3)
O7—H7A···O3^v	0.80 (4)	2.04 (4)	2.806 (2)	160 (4)
O5—H5B···O8^vi	0.82 (5)	1.96 (5)	2.733 (3)	158 (5)
O7—H7B···S1^vii	0.97 (4)	2.75 (4)	3.5798 (14)	144 (3)
O7—H7B···O4^vii	0.97 (4)	1.76 (4)	2.703 (2)	165 (3)
O8—H8···S1	0.80 (4)	2.97 (4)	3.7678 (18)	174 (4)
O8—H8···O4	0.80 (4)	2.10 (4)	2.864 (2)	159 (4)

Symmetry codes: (ii) −x+1/2, y, −z+1; (iii) x, −y+1/2, z−1/2; (iv) −x, −y+1, −z+1; (v) x−1, −y+1/2, z−1/2; (vi) −x+1, −y, −z+1; (vii) x−1/2, y+1/2, z−1/2.

(2) Hexaaquabis(sulfato-κ²O,O')uranium(IV) dihydrate

Crystal data

[U(SO4)2(H2O)6]·2H2O	F(000) = 1072
Mr = 574.28	Dx = 2.922 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 8.4071 (3) Å	Cell parameters from 5137 reflections
b = 11.7144 (4) Å	θ = 2.8–30.0°
c = 13.2659 (4) Å	µ = 12.84 mm^−1
β = 92.510 (1)°	T = 90 K
V = 1305.23 (8) Å^3	Prism, purple-green
Z = 4	0.09 × 0.07 × 0.07 mm

Data collection

Bruker APEXII CCD area-detector diffractometer	3029 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.023
φ and ω scans	θmax = 30.0°, θmin = 2.8°
Absorption correction: multi-scan (SADABS; Bruker, 2012)	h = −11→11
Tmin = 0.408, Tmax = 0.463	k = −16→7
14870 measured reflections	l = −18→18
3784 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)] = 0.017	Hydrogen site location: difference Fourier map
wR(F^2) = 0.035	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0109P)^2 + 2.232P] where P = (Fo^2 + 2Fc^2)/3
3784 reflections	(Δ/σ)max < 0.001
231 parameters	Δρmax = 0.82 e Å^−3
0 restraints	Δρmin = −0.64 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
O1	0.7590 (2)	0.11062 (17)	0.17020 (14)	0.0073 (4)
O2	0.7678 (2)	0.10181 (17)	0.34676 (14)	0.0073 (4)
O3	0.9728 (2)	0.00488 (17)	0.25725 (15)	0.0087 (4)
O4	0.9733 (2)	0.21002 (17)	0.26602 (14)	0.0081 (4)
O5	0.4719 (2)	0.23501 (17)	0.10203 (14)	0.0075 (4)
O6	0.2509 (2)	0.12296 (16)	0.13666 (14)	0.0065 (4)
O7	0.2973 (2)	0.16549 (18)	−0.03765 (14)	0.0083 (4)
O8	0.2073 (2)	0.31477 (17)	0.07048 (14)	0.0082 (4)
O9	0.4857 (3)	0.11060 (18)	0.43226 (15)	0.0076 (4)
O10	0.6095 (2)	0.29128 (19)	0.29559 (16)	0.0078 (4)
O11	0.2945 (2)	0.24228 (18)	0.30440 (16)	0.0078 (4)
O12	0.2851 (2)	−0.01070 (18)	0.29694 (16)	0.0082 (4)
O13	0.4902 (3)	−0.02609 (19)	0.11334 (15)	0.0088 (4)
O14	0.5918 (3)	−0.08007 (19)	0.30292 (17)	0.0079 (4)
O15	0.1927 (3)	−0.0959 (2)	0.03936 (17)	0.0122 (4)
O16	0.8025 (3)	−0.1033 (2)	0.46805 (17)	0.0171 (5)
H16A	0.8613	−0.1607	0.4511	0.026*
H16B	0.8451	−0.0400	0.4480	0.026*
S1	0.87400 (7)	0.10736 (6)	0.26056 (5)	0.00489 (12)
S2	0.30351 (8)	0.21126 (6)	0.06517 (5)	0.00476 (12)
U1	0.49977 (2)	0.10818 (2)	0.25070 (2)	0.00329 (3)
H9A	0.555 (4)	0.130 (3)	0.468 (3)	0.010 (9)*
H9B	0.396 (6)	0.107 (4)	0.455 (3)	0.044 (14)*
H10A	0.666 (5)	0.297 (3)	0.341 (3)	0.018 (10)*
H10B	0.589 (5)	0.353 (4)	0.279 (3)	0.029 (12)*
H11A	0.304 (5)	0.288 (4)	0.354 (3)	0.028 (11)*
H11B	0.207 (5)	0.232 (4)	0.289 (3)	0.028 (12)*
H12A	0.202 (4)	0.001 (3)	0.282 (3)	0.007 (9)*
H12B	0.295 (5)	−0.066 (4)	0.340 (3)	0.041 (13)*
H13A	0.412 (5)	−0.044 (4)	0.088 (3)	0.026 (12)*
H13B	0.557 (5)	−0.066 (4)	0.094 (3)	0.027 (11)*
H14A	0.569 (5)	−0.133 (4)	0.285 (3)	0.016 (11)*
H14B	0.656 (5)	−0.084 (4)	0.347 (3)	0.033 (13)*
H15A	0.163 (5)	−0.034 (4)	0.052 (3)	0.027 (12)*
H15B	0.193 (6)	−0.106 (4)	−0.024 (4)	0.046 (15)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0058 (8)	0.0105 (10)	0.0056 (9)	−0.0006 (7)	−0.0009 (7)	0.0011 (7)
O2	0.0062 (8)	0.0094 (10)	0.0062 (9)	0.0001 (8)	0.0001 (7)	−0.0007 (7)
O3	0.0052 (9)	0.0043 (9)	0.0165 (10)	0.0028 (7)	−0.0007 (8)	−0.0019 (8)
O4	0.0056 (9)	0.0038 (9)	0.0150 (10)	−0.0005 (7)	0.0023 (7)	−0.0028 (7)
O5	0.0070 (8)	0.0083 (10)	0.0070 (9)	0.0006 (7)	−0.0011 (7)	0.0015 (7)
O6	0.0068 (9)	0.0058 (10)	0.0068 (9)	−0.0004 (7)	0.0002 (7)	0.0016 (7)
O7	0.0111 (9)	0.0095 (10)	0.0043 (9)	0.0035 (8)	−0.0003 (7)	−0.0013 (8)
O8	0.0115 (9)	0.0070 (10)	0.0058 (9)	0.0044 (8)	−0.0021 (7)	−0.0010 (8)
O9	0.0064 (9)	0.0112 (11)	0.0051 (9)	−0.0019 (8)	−0.0017 (7)	−0.0012 (8)
O10	0.0087 (9)	0.0052 (11)	0.0092 (10)	0.0009 (8)	−0.0029 (8)	0.0009 (8)
O11	0.0051 (9)	0.0085 (11)	0.0097 (10)	0.0011 (8)	−0.0005 (7)	−0.0029 (8)
O12	0.0048 (9)	0.0090 (11)	0.0105 (10)	−0.0006 (8)	−0.0016 (7)	0.0038 (8)
O13	0.0065 (9)	0.0109 (11)	0.0088 (10)	0.0035 (8)	−0.0008 (8)	−0.0049 (8)
O14	0.0097 (10)	0.0028 (11)	0.0107 (10)	0.0004 (8)	−0.0038 (8)	0.0005 (8)
O15	0.0176 (11)	0.0102 (12)	0.0089 (10)	0.0010 (9)	0.0007 (8)	−0.0005 (9)
O16	0.0164 (11)	0.0196 (13)	0.0156 (11)	0.0091 (10)	0.0028 (9)	0.0015 (10)
S1	0.0033 (3)	0.0044 (3)	0.0070 (3)	0.0003 (2)	0.0001 (2)	−0.0002 (2)
S2	0.0057 (3)	0.0049 (3)	0.0036 (3)	0.0011 (2)	−0.0006 (2)	−0.0004 (2)
U1	0.00331 (4)	0.00331 (5)	0.00323 (4)	0.00007 (4)	−0.00004 (3)	0.00004 (4)

Geometric parameters (Å, º)

O1—S1	1.5073 (19)	O7—S2	1.464 (2)
O1—U1	2.4686 (19)	O8—S2	1.461 (2)
O2—S1	1.483 (2)	O9—U1	2.417 (2)
O2—U1	2.5408 (19)	O10—U1	2.400 (2)
O3—S1	1.462 (2)	O11—U1	2.462 (2)
O4—S1	1.464 (2)	O12—U1	2.381 (2)
O5—S2	1.5034 (19)	O13—U1	2.406 (2)
O5—U1	2.4721 (19)	O14—U1	2.428 (2)
O6—S2	1.484 (2)	S1—U1	3.1432 (6)
O6—U1	2.5337 (19)	S2—U1	3.1436 (6)
S1—O1—U1	101.74 (9)	O10—U1—O11	67.95 (7)
S1—O2—U1	99.36 (9)	O13—U1—O11	129.47 (7)
S2—O5—U1	101.73 (10)	O9—U1—O11	68.81 (7)
S2—O6—U1	99.65 (9)	O14—U1—O11	135.70 (7)
U1—O9—H9A	123 (3)	O12—U1—O1	144.25 (7)
U1—O9—H9B	117 (3)	O10—U1—O1	76.11 (7)
H9A—O9—H9B	118 (4)	O13—U1—O1	71.38 (7)
U1—O10—H10A	120 (3)	O9—U1—O1	120.91 (7)
U1—O10—H10B	133 (3)	O14—U1—O1	81.81 (7)
H10A—O10—H10B	106 (4)	O11—U1—O1	139.56 (7)
U1—O11—H11A	126 (3)	O12—U1—O5	120.70 (7)
U1—O11—H11B	120 (3)	O10—U1—O5	71.50 (7)
H11A—O11—H11B	112 (4)	O13—U1—O5	77.87 (7)
U1—O12—H12A	123 (3)	O9—U1—O5	141.35 (7)
U1—O12—H12B	124 (3)	O14—U1—O5	142.31 (7)
H12A—O12—H12B	113 (4)	O11—U1—O5	78.71 (7)
U1—O13—H13A	121 (3)	O1—U1—O5	72.69 (6)
U1—O13—H13B	129 (3)	O12—U1—O6	65.06 (7)
H13A—O13—H13B	108 (4)	O10—U1—O6	112.68 (7)
U1—O14—H14A	130 (3)	O13—U1—O6	65.99 (7)
U1—O14—H14B	118 (3)	O9—U1—O6	121.27 (7)
H14A—O14—H14B	112 (4)	O14—U1—O6	118.49 (7)
H15A—O15—H15B	111 (4)	O11—U1—O6	63.78 (7)
H16A—O16—H16B	109.5	O1—U1—O6	117.55 (6)
O3—S1—O4	110.66 (11)	O5—U1—O6	55.64 (6)
O3—S1—O2	110.45 (12)	O12—U1—O2	121.28 (7)
O4—S1—O2	111.04 (11)	O10—U1—O2	65.09 (7)
O3—S1—O1	110.04 (11)	O13—U1—O2	111.11 (7)
O4—S1—O1	111.29 (12)	O9—U1—O2	65.27 (7)
O2—S1—O1	103.15 (11)	O14—U1—O2	64.26 (7)
O3—S1—U1	124.78 (8)	O11—U1—O2	119.42 (7)
O4—S1—U1	124.54 (8)	O1—U1—O2	55.74 (6)
O2—S1—U1	52.90 (7)	O5—U1—O2	117.95 (6)
O1—S1—U1	50.26 (7)	O6—U1—O2	173.00 (6)
O8—S2—O7	110.57 (11)	O12—U1—S1	139.12 (5)
O8—S2—O6	111.50 (11)	O10—U1—S1	67.61 (5)
O7—S2—O6	109.92 (12)	O13—U1—S1	91.70 (5)
O8—S2—O5	110.27 (12)	O9—U1—S1	92.94 (5)
O7—S2—O5	111.43 (11)	O14—U1—S1	71.30 (5)
O6—S2—O5	102.95 (11)	O11—U1—S1	134.67 (5)
O8—S2—U1	123.63 (8)	O1—U1—S1	28.00 (4)
O7—S2—U1	125.79 (8)	O5—U1—S1	95.44 (4)
O6—S2—U1	52.62 (7)	O6—U1—S1	145.49 (4)
O5—S2—U1	50.35 (7)	O2—U1—S1	27.74 (4)
O12—U1—O10	138.28 (7)	O12—U1—S2	92.78 (5)
O12—U1—O13	79.17 (7)	O10—U1—S2	91.94 (5)
O10—U1—O13	140.54 (7)	O13—U1—S2	70.07 (5)
O12—U1—O9	71.30 (7)	O9—U1—S2	136.78 (5)
O10—U1—O9	77.13 (7)	O14—U1—S2	136.22 (6)
O13—U1—O9	139.55 (7)	O11—U1—S2	68.34 (5)
O12—U1—O14	68.34 (7)	O1—U1—S2	95.73 (5)
O10—U1—O14	128.81 (8)	O5—U1—S2	27.92 (4)
O13—U1—O14	67.79 (7)	O6—U1—S2	27.73 (4)
O9—U1—O14	75.83 (7)	O2—U1—S2	145.84 (5)
O12—U1—O11	75.51 (7)	S1—U1—S2	121.591 (17)
U1—O2—S1—O3	−118.77 (10)	U1—O6—S2—O8	−116.63 (10)
U1—O2—S1—O4	118.08 (10)	U1—O6—S2—O7	120.39 (10)
U1—O2—S1—O1	−1.22 (12)	U1—O6—S2—O5	1.57 (11)
U1—O1—S1—O3	119.11 (10)	U1—O5—S2—O8	117.44 (10)
U1—O1—S1—O4	−117.86 (10)	U1—O5—S2—O7	−119.38 (11)
U1—O1—S1—O2	1.26 (12)	U1—O5—S2—O6	−1.62 (12)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O16—H16A···O5^i	0.87	2.01	2.864 (3)	167
O16—H16B···O2	0.87	2.22	2.899 (3)	135
O9—H9A···O8^ii	0.77 (4)	1.94 (4)	2.701 (3)	172 (4)
O9—H9B···O16^iii	0.83 (5)	1.99 (5)	2.812 (3)	171 (5)
O10—H10A···O7^ii	0.76 (4)	1.95 (4)	2.709 (3)	171 (4)
O10—H10B···O3^iv	0.78 (5)	1.91 (5)	2.681 (3)	176 (4)
O11—H11A···O15^v	0.85 (4)	1.96 (4)	2.807 (3)	174 (4)
O11—H11B···O4^vi	0.77 (4)	1.99 (4)	2.752 (3)	173 (4)
O12—H12A···O3^vi	0.73 (4)	1.94 (4)	2.661 (3)	168 (4)
O12—H12A···S1^vi	0.73 (4)	3.03 (4)	3.734 (2)	163 (3)
O12—H12B···O8^vii	0.87 (5)	1.83 (5)	2.696 (3)	174 (4)
O12—H12B···S2^vii	0.87 (5)	3.03 (5)	3.825 (2)	154 (4)
O13—H13A···O15	0.75 (4)	2.02 (4)	2.770 (3)	172 (4)
O13—H13B···O7^viii	0.78 (4)	1.87 (4)	2.650 (3)	174 (4)
O13—H13B···S2^viii	0.78 (4)	2.99 (4)	3.699 (2)	151 (4)
O14—H14A···O4^i	0.69 (4)	1.98 (4)	2.672 (3)	174 (4)
O14—H14B···O16	0.78 (5)	2.00 (5)	2.770 (3)	174 (4)
O15—H15A···O6	0.78 (4)	2.27 (4)	2.903 (3)	139 (4)
O15—H15B···O1^viii	0.86 (5)	1.99 (5)	2.832 (3)	167 (5)

Symmetry codes: (i) −x+3/2, y−1/2, −z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) −x+1, −y, −z+1; (iv) −x+3/2, y+1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) x−1, y, z; (vii) −x+1/2, y−1/2, −z+1/2; (viii) −x+1, −y, −z.