Trigonal Na₄[UO₂(CO₃)₃]

Tetrasodium tricarbonatodioxouranate(VI), Na₄[UO₂(CO₃)₃], crystallizes in the trigonal space group Pc1. Though the symmetry differs from other similar compounds (e.g. the NH₄⁺, K⁺ and Tl⁺ salts) which are monoclinic, there is a common structure motif consisting of UO₂(CO₃)₃ groups with a trigonal outline when viewed along the shortest O-U-O bond pair. In Na₄[UO₂(CO₃)₃], there are three non-equivalent Na atoms; Na1 (site symmetry ) and Na2 (site symmetry 3) are in centres of face-sharing octahedra, which form a chain running parallel to the c axis at each unit-cell corner, whereas the Na3 atom is surrounded by a deformed square pyramid of O atoms, forming edge-sharing triplets. The title compound has also a natural dimorph, namely the recently approved triclinic mineral cejkaite.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](O-C) = 0.006 Å
• R factor = 0.024
• wR factor = 0.062
• Data-to-parameter ratio = 12.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_741  Alert C Bond    Calc 3.20430(10), Rep     3.20420 ....    Missing s.u.
                     NA1  -NA2     1.555   7.555

PLAT_741  Alert C Bond    Calc 3.20430(10), Rep     3.20430 ....    Missing s.u.
                     NA1  -NA2     1.555   1.555

PLAT_741  Alert C Bond    Calc 3.20430(10), Rep     3.20430 ....    Missing s.u.
                     NA2  -NA1     1.555   4.555

General Notes



FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and _chemical_formula_moiety. This is
          usually due to the moiety formula being in the wrong format.
          Atom count from _chemical_formula_sum:   C3 Na4 O11 U1
          Atom count from _chemical_formula_moiety:C1 Na4 O11 U1


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 3 Alert Level C = Please check

---

S1. Comment

Recently, we have found a natural triclinic compound of Na₄[UO₂(CO₃)₃] composition in Jáchymov, the Czech Republic. This natural triclinic material does not form crystals suitable for single-crystal study. We recognized that a compound of the same chemistry but with trigonal symmetry had been described by Douglass (1956), who determined the extinction symbol, unit-cell dimensions and also additional physical parameters. An attempt to prepare a synthetic analogue of our natural triclinic compound failed; instead, we synthesized a trigonal dimorph equivalent to the material of Douglass for which we report a complete structure.

There are chemically similar compounds – NH₄[UO₂(CO₃)₃], K₄[UO₂(CO₃)₃] and Tl₄[UO₂(CO₃)₃] – for which the crystal structures are known (Graziani et al., 1972; Anderson et al., 1980; Mereiter, 1986; respectively). All these materials crystallize in the monoclinic space group C2/c. They share the common basic structural motif of UO₂(CO₃)₃ groups with the compound we synthesized. This group is, in our case, built up from the asymmetric unit (Fig. 1) due to threefold axis and contains three planar CO₃ triangles sharing one of their edges with the UO₂O₆ polyhedron. The lengths of the U—O bonds oriented along the direction of the c axis (U1—O1 and U1—O2) are significantly shorter compared to the U—O distances in the medial plane of the UO₂O₆ polyhedron (U1—O11 and U1—O12) in the compound Na₄[UO₂(CO₃)₃]. The planes of the CO₃ triangles attached to the UO₂O₆ polyhedron are inclined from the 001 plane. Atoms Na1 and Na2 are octahedrally coordinated by O13 atoms. The octahedra share a common face and form a chain of alternating polyhedra around Na1 and Na2 running parallel to the c axis and situated at each unit-cell corner. The octahedron around Na1 is fairly regular, with quadratic elongation of 1.012 and bond-angle s.u. of 6.87°. On the contrary, the polyhedron around Na2 departs significantly from ideal geometry, which results in quadratic elongation of 1.121 and bond-angle s.u. of 18.78°. Volumes of both octahedra are comparable; the polyhedron around Na1 has a volume of 19.02 ų and that around Na2 17.40 ų. Atom Na3 has a coordination number of 5; the polyhedron around it can be described as square pyramidal as τ = 0.15 (Addison et al., 1984). Three of these polyhedra build up edge-sharing triplets (Fig. 4). The shared edge is defined by the atoms O1—O2 and it runs parallel to the c axis (Fig. 2). The overall structure motif is apparent from Fig. 3. Triplets of polyhedra around Na3 atoms share vertices of their common edges with vertices of UO₂(CO₃)₃ complexes adjacent to them in the [001] direction. These complexes, in turn, share edges O11–O12 with laterally neighbouring square pyramids around Na3 atoms, building up two-dimensional sheets parallel to 001 typical for this structure. The sheets are stacked along [001] so the next sheet is rotated by 60° around [001] with respect to adjacent one. Finally, each of three apical carbonate O13 atoms from any UO₂(CO₃)₃ complex is shared by the octahedron around either Na1 or Na2 (depending on the height of the sheet along [001] in the unit cell) and also make a vertex of laterally adjacent triplet of polyhedra around Na3 (Fig. 4). Using the approach of effective coordination numbers (Hoppe, 1979) and the program of Rieder (1993), we calculated effective coordination numbers (ECoNs) for central atoms as U1 = 2.24, Na1 = 6.00, Na2 = 6.12, Na3 = 4.76 and C1 = 2.94; for U1 and Na3 polyedrathese ECoNs depart significantly from their ideal values. This could be ascribed to substantial irregularity of individual polyhedra. Their irregularity results results also in bond-valence sums departing from ideal values. Using the data of Brown & Altermatt (1985) and the program of Wills & Brown (1999), we calculated bond-valence sums as [central atom, bond valence sum in vu (valance units) and departure in percent from the ideal oxidation state] U1 6.59 [10], Na1 1.074 [7], Na2 1.02 [2], Na3 1.127 [13], C1 4.033 [1].

S2. Experimental

Clear yellow hexagonal prismatic crystals up to 1 mm long of the title compound have been synthesized from synthetic triclinic Na₄[(UO)₂(CO₃)₃] powder by recrystallization in sealed silica glass tubes under hydrothermal conditions at a pressure of about 20 MPa and a temperature of 408 K for 3 d. In addition to the crystals of the title compound, we recovered from the tube an orange powdered material which we identified to contain sodium di- and heptauranates.

Computing details

Data collection: COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997); cell refinement: COLLECT and DENZO; data reduction: COLLECT and DENZO; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Shape Software, 1999).

Figures

	Fig. 1. View of the asymmetric unit of Na4[UO2(CO3)3] with the atom-numbering scheme. Displacement ellipsoids are at the 50% probability (PLATON, Speck, 1999).
	Fig. 2. Polyhedral presentation of an edge-sharing triplet of NaO5 polyhedra.
	Fig. 3. Projection of the crystal structure of Na4[UO2(CO3)3] onto the 100 plane. Note the chain of alternating octahedra around the Na1 and Na2 atoms parallel to [001] at the unit-cell edge. Colour-coding of polyhedra, red: UO2O6 polyhedron; blue: planar CO3 triangles; yellow: NaO6 octahedra; green: NaO5 irregular trigonal bipyramid.
	Fig. 4. Polyhedral presentation of a single layer consisting of the UO2-(CO3)3 complex, triplets of polyhedra around Na3 and octahedra around Na1 or Na2 found in the Na4[UO2(CO3)3] viewed down [001]. Colour-coding of polyhedra, red: UO2O6 polyhedron; blue: planar CO3 triangles; yellow: NaO6 octahedra; green: NaO5 irregular trigonal bipyramid.

(I)

Crystal data

Na4[UO2(CO3)3]	Dx = 3.720 Mg m^−3
Mr = 542.02	Mo Kα radiation, λ = 0.71070 Å
Trigonal, P3c1	Cell parameters from 10249 reflections
a = 9.3380 (2) Å	θ = 1–27.5°
c = 12.8170 (3) Å	µ = 17.01 mm^−1
V = 967.89 (4) Å^3	T = 293 K
Z = 4	Bar, yellow
F(000) = 968	0.11 × 0.05 × 0.05 mm

Data collection

Nonius KappaCCD area-detector diffractometer	746 independent reflections
Radiation source: fine-focus sealed tube	615 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.090
Detector resolution: 9.091 pixels mm^-1	θmax = 27.5°, θmin = 3.2°
ϕ and ω scans to fill the Ewald sphere	h = −12→12
Absorption correction: gaussian (Coppens, 1970)	k = −12→12
Tmin = 0.208, Tmax = 0.617	l = −16→16
22328 measured 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)] = 0.024	w = 1/[σ^2(Fo^2) + (0.0358P)^2 + 2.8258P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.062	(Δ/σ)max < 0.001
S = 1.07	Δρmax = 2.33 e Å^−3
746 reflections	Δρmin = −1.73 e Å^−3
60 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0074 (5)

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 > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One strong reflections 010 were omitted from the final refinement due inaccuracy in measurement.

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

	x	y	z	Uiso*/Ueq
U1	0.3333	0.6667	0.130224 (17)	0.01212 (18)
Na1	0.0000	0.0000	0.0000	0.0221 (12)
Na2	0.0000	0.0000	0.2500	0.0229 (12)
Na3	−0.1233 (3)	0.5688 (2)	0.12367 (17)	0.0295 (5)
C1	0.0741 (6)	0.3279 (5)	0.1280 (3)	0.0171 (9)
O11	0.0462 (5)	0.4509 (4)	0.1186 (3)	0.0274 (8)
O12	0.2299 (5)	0.3771 (5)	0.1436 (3)	0.0283 (8)
O13	−0.0358 (4)	0.1805 (4)	0.1219 (3)	0.0235 (8)
O1	0.3333	0.6667	0.2714 (6)	0.0228 (15)
O2	0.3333	0.6667	−0.0110 (6)	0.0214 (15)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
U1	0.0117 (3)	0.011	0.0136 (2)	0.005	0.000	0.000
Na1	0.021 (2)	0.021	0.024 (3)	0.010	0.000	0.000
Na2	0.025 (3)	0.023	0.020 (3)	0.012	0.000	0.000
Na3	0.0174 (10)	0.0182 (10)	0.0522 (13)	0.0085 (9)	−0.0029 (9)	0.0014 (9)
C1	0.014 (2)	0.014 (2)	0.021 (2)	0.0051 (18)	0.0039 (17)	0.0022 (17)
O11	0.0211 (18)	0.0138 (17)	0.048 (2)	0.0092 (14)	0.0001 (16)	0.0017 (15)
O12	0.0125 (16)	0.0139 (17)	0.057 (2)	0.0058 (14)	0.0012 (16)	0.0022 (17)
O13	0.0149 (17)	0.0122 (16)	0.040 (2)	0.0042 (14)	0.0005 (14)	−0.0015 (14)
O1	0.023 (3)	0.025	0.022 (3)	0.012	0.000	0.000
O2	0.026 (4)	0.024	0.013 (3)	0.012	0.000	0.000

Geometric parameters (Å, º)

U1—O1	1.809 (8)	Na2—O13	2.492 (4)
U1—O2	1.810 (7)	Na2—Na1^xii	3.2043
U1—O12	2.379 (4)	Na2—Na3^xi	3.940 (2)
U1—O12^i	2.380 (4)	Na2—Na3^xiv	3.940 (2)
U1—O12^ii	2.380 (4)	Na2—Na3^xv	3.940 (2)
U1—O11^i	2.422 (4)	Na2—Na3^ii	3.940 (2)
U1—O11	2.422 (4)	Na3—O12^i	2.287 (4)
U1—O11^ii	2.422 (4)	Na3—O13^xvi	2.320 (4)
U1—C1^i	2.865 (4)	Na3—O11	2.338 (4)
U1—C1	2.865 (4)	Na3—O1^xvii	2.486 (5)
U1—C1^ii	2.865 (4)	Na3—O2^x	2.541 (5)
U1—Na3^iii	3.784 (2)	Na3—C1^xvi	3.092 (5)
Na1—O13^iv	2.440 (3)	Na3—Na3^xvi	3.620 (4)
Na1—O13^v	2.440 (3)	Na3—Na3^xi	3.620 (4)
Na1—O13	2.440 (3)	Na3—U1^xvii	3.784 (2)
Na1—O13^vi	2.440 (3)	Na3—Na3^iii	3.803 (4)
Na1—O13^vii	2.440 (3)	Na3—U1^x	3.868 (2)
Na1—O13^viii	2.440 (3)	C1—O13	1.242 (5)
Na1—Na2^vi	3.2042	C1—O12	1.303 (7)
Na1—Na2	3.2043	C1—O11	1.304 (6)
Na1—Na3^ix	3.926 (2)	C1—Na3^xi	3.092 (5)
Na1—Na3^x	3.926 (2)	O12—Na3^ii	2.287 (4)
Na1—Na3^xi	3.926 (2)	O13—Na3^xi	2.320 (4)
Na1—Na3^ii	3.926 (2)	O1—Na3^iii	2.486 (5)
Na2—O13^vii	2.492 (4)	O1—Na3^xviii	2.486 (5)
Na2—O13^viii	2.492 (4)	O1—Na3^xix	2.486 (5)
Na2—O13^xii	2.492 (4)	O2—Na3^x	2.541 (5)
Na2—O13^iii	2.492 (4)	O2—Na3^xx	2.541 (5)
Na2—O13^xiii	2.492 (4)	O2—Na3^v	2.541 (5)
O1—U1—O2	180.000 (1)	O13^xii—Na2—Na1	131.21 (8)
O1—U1—O12	85.88 (10)	O13^iii—Na2—Na1	131.21 (8)
O2—U1—O12	94.12 (10)	O13^xiii—Na2—Na1	131.21 (8)
O1—U1—O12^i	85.88 (10)	O13—Na2—Na1	48.79 (8)
O2—U1—O12^i	94.12 (10)	O13^vii—Na2—Na1^xii	131.21 (8)
O12—U1—O12^i	119.49 (3)	O13^viii—Na2—Na1^xii	131.21 (8)
O1—U1—O12^ii	85.88 (10)	O13^xii—Na2—Na1^xii	48.79 (8)
O2—U1—O12^ii	94.12 (10)	O13^iii—Na2—Na1^xii	48.79 (8)
O12—U1—O12^ii	119.49 (3)	O13^xiii—Na2—Na1^xii	48.79 (8)
O12^i—U1—O12^ii	119.49 (3)	O13—Na2—Na1^xii	131.21 (8)
O1—U1—O11^i	93.52 (9)	Na1—Na2—Na1^xii	180.0
O2—U1—O11^i	86.48 (9)	O13^vii—Na2—Na3^xi	70.70 (9)
O12—U1—O11^i	173.15 (12)	O13^viii—Na2—Na3^xi	110.53 (8)
O12^i—U1—O11^i	53.67 (12)	O13^xii—Na2—Na3^xi	90.31 (8)
O12^ii—U1—O11^i	67.22 (12)	O13^iii—Na2—Na3^xi	81.71 (8)
O1—U1—O11	93.52 (9)	O13^xiii—Na2—Na3^xi	162.01 (9)
O2—U1—O11	86.48 (9)	O13—Na2—Na3^xi	33.63 (9)
O12—U1—O11	53.67 (12)	Na1—Na2—Na3^xi	65.73 (3)
O12^i—U1—O11	67.22 (12)	Na1^xii—Na2—Na3^xi	114.27 (3)
O12^ii—U1—O11	173.15 (12)	O13^vii—Na2—Na3^xiv	33.63 (9)
O11^i—U1—O11	119.63 (2)	O13^viii—Na2—Na3^xiv	70.70 (9)
O1—U1—O11^ii	93.52 (9)	O13^xii—Na2—Na3^xiv	81.71 (8)
O2—U1—O11^ii	86.48 (9)	O13^iii—Na2—Na3^xiv	162.01 (9)
O12—U1—O11^ii	67.22 (12)	O13^xiii—Na2—Na3^xiv	90.31 (8)
O12^i—U1—O11^ii	173.15 (12)	O13—Na2—Na3^xiv	110.53 (8)
O12^ii—U1—O11^ii	53.67 (12)	Na1—Na2—Na3^xiv	65.73 (3)
O11^i—U1—O11^ii	119.63 (2)	Na1^xii—Na2—Na3^xiv	114.27 (3)
O11—U1—O11^ii	119.63 (2)	Na3^xi—Na2—Na3^xiv	104.28 (4)
O1—U1—C1^i	90.56 (8)	O13^vii—Na2—Na3^xv	81.71 (8)
O2—U1—C1^i	89.44 (8)	O13^viii—Na2—Na3^xv	162.01 (9)
O12—U1—C1^i	146.23 (14)	O13^xii—Na2—Na3^xv	33.63 (9)
O12^i—U1—C1^i	26.77 (14)	O13^iii—Na2—Na3^xv	70.70 (9)
O12^ii—U1—C1^i	93.65 (14)	O13^xiii—Na2—Na3^xv	110.53 (8)
O11^i—U1—C1^i	26.93 (14)	O13—Na2—Na3^xv	90.31 (8)
O11—U1—C1^i	93.18 (14)	Na1—Na2—Na3^xv	114.27 (3)
O11^ii—U1—C1^i	146.55 (14)	Na1^xii—Na2—Na3^xv	65.73 (3)
O1—U1—C1	90.56 (8)	Na3^xi—Na2—Na3^xv	57.72 (6)
O2—U1—C1	89.44 (8)	Na3^xiv—Na2—Na3^xv	97.84 (6)
O12—U1—C1	26.77 (14)	O13^vii—Na2—Na3^ii	110.53 (8)
O12^i—U1—C1	93.65 (14)	O13^viii—Na2—Na3^ii	33.63 (9)
O12^ii—U1—C1	146.23 (14)	O13^xii—Na2—Na3^ii	162.01 (9)
O11^i—U1—C1	146.55 (14)	O13^iii—Na2—Na3^ii	90.31 (8)
O11—U1—C1	26.93 (14)	O13^xiii—Na2—Na3^ii	81.71 (8)
O11^ii—U1—C1	93.18 (14)	O13—Na2—Na3^ii	70.70 (9)
C1^i—U1—C1	119.990 (4)	Na1—Na2—Na3^ii	65.73 (3)
O1—U1—C1^ii	90.56 (8)	Na1^xii—Na2—Na3^ii	114.27 (3)
O2—U1—C1^ii	89.44 (8)	Na3^xi—Na2—Na3^ii	104.28 (4)
O12—U1—C1^ii	93.65 (14)	Na3^xiv—Na2—Na3^ii	104.28 (4)
O12^i—U1—C1^ii	146.22 (14)	Na3^xv—Na2—Na3^ii	154.74 (7)
O12^ii—U1—C1^ii	26.77 (14)	O12^i—Na3—O13^xvi	85.84 (15)
O11^i—U1—C1^ii	93.17 (14)	O12^i—Na3—O11	70.15 (16)
O11—U1—C1^ii	146.55 (14)	O13^xvi—Na3—O11	155.48 (16)
O11^ii—U1—C1^ii	26.93 (14)	O12^i—Na3—O1^xvii	136.50 (19)
C1^i—U1—C1^ii	119.991 (4)	O13^xvi—Na3—O1^xvii	110.46 (13)
C1—U1—C1^ii	119.991 (3)	O11—Na3—O1^xvii	91.08 (11)
O1—U1—Na3^iii	33.53 (3)	O12^i—Na3—O2^x	146.30 (18)
O2—U1—Na3^iii	146.47 (3)	O13^xvi—Na3—O2^x	109.34 (14)
O12—U1—Na3^iii	94.76 (10)	O11—Na3—O2^x	89.31 (11)
O12^i—U1—Na3^iii	53.70 (11)	O1^xvii—Na3—O2^x	67.4 (2)
O12^ii—U1—Na3^iii	109.24 (10)	O12^i—Na3—C1^xvi	106.38 (16)
O11^i—U1—Na3^iii	81.14 (9)	O13^xvi—Na3—C1^xvi	20.92 (13)
O11—U1—Na3^iii	73.18 (10)	O11—Na3—C1^xvi	176.39 (15)
O11^ii—U1—Na3^iii	126.65 (10)	O1^xvii—Na3—C1^xvi	92.22 (11)
C1^i—U1—Na3^iii	66.02 (9)	O2^x—Na3—C1^xvi	93.32 (11)
C1—U1—Na3^iii	84.22 (9)	O12^i—Na3—Na3^xvi	168.08 (14)
C1^ii—U1—Na3^iii	122.11 (9)	O13^xvi—Na3—Na3^xvi	84.17 (13)
O13^iv—Na1—O13^v	83.42 (12)	O11—Na3—Na3^xvi	120.25 (11)
O13^iv—Na1—O13	96.58 (12)	O1^xvii—Na3—Na3^xvi	43.26 (11)
O13^v—Na1—O13	96.58 (12)	O2^x—Na3—Na3^xvi	44.56 (10)
O13^iv—Na1—O13^vi	83.42 (12)	C1^xvi—Na3—Na3^xvi	63.32 (12)
O13^v—Na1—O13^vi	83.42 (12)	O12^i—Na3—Na3^xi	129.78 (14)
O13—Na1—O13^vi	180.0	O13^xvi—Na3—Na3^xi	144.17 (13)
O13^iv—Na1—O13^vii	96.58 (12)	O11—Na3—Na3^xi	60.27 (11)
O13^v—Na1—O13^vii	180.0	O1^xvii—Na3—Na3^xi	43.26 (11)
O13—Na1—O13^vii	83.42 (12)	O2^x—Na3—Na3^xi	44.56 (10)
O13^vi—Na1—O13^vii	96.58 (12)	C1^xvi—Na3—Na3^xi	123.31 (12)
O13^iv—Na1—O13^viii	180.0	Na3^xvi—Na3—Na3^xi	60.0
O13^v—Na1—O13^viii	96.58 (12)	O12^i—Na3—U1^xvii	115.04 (13)
O13—Na1—O13^viii	83.42 (12)	O13^xvi—Na3—U1^xvii	103.56 (12)
O13^vi—Na1—O13^viii	96.58 (12)	O11—Na3—U1^xvii	91.46 (11)
O13^vii—Na1—O13^viii	83.42 (12)	O1^xvii—Na3—U1^xvii	23.70 (15)
O13^iv—Na1—Na2^vi	50.20 (8)	O2^x—Na3—U1^xvii	91.12 (14)
O13^v—Na1—Na2^vi	50.20 (8)	C1^xvi—Na3—U1^xvii	90.96 (10)
O13—Na1—Na2^vi	129.80 (8)	Na3^xvi—Na3—U1^xvii	61.42 (3)
O13^vi—Na1—Na2^vi	50.20 (8)	Na3^xi—Na3—U1^xvii	61.42 (3)
O13^vii—Na1—Na2^vi	129.80 (8)	O12^i—Na3—Na3^iii	53.38 (11)
O13^viii—Na1—Na2^vi	129.80 (8)	O13^xvi—Na3—Na3^iii	96.48 (12)
O13^iv—Na1—Na2	129.80 (8)	O11—Na3—Na3^iii	73.50 (12)
O13^v—Na1—Na2	129.80 (8)	O1^xvii—Na3—Na3^iii	84.12 (16)
O13—Na1—Na2	50.20 (8)	O2^x—Na3—Na3^iii	146.57 (13)
O13^vi—Na1—Na2	129.80 (8)	C1^xvi—Na3—Na3^iii	105.37 (10)
O13^vii—Na1—Na2	50.20 (8)	Na3^xvi—Na3—Na3^iii	121.46 (6)
O13^viii—Na1—Na2	50.20 (8)	Na3^xi—Na3—Na3^iii	102.48 (2)
Na2^vi—Na1—Na2	180.0	U1^xvii—Na3—Na3^iii	61.68 (6)
O13^iv—Na1—Na3^ix	33.46 (9)	O12^i—Na3—U1^x	126.78 (13)
O13^v—Na1—Na3^ix	112.25 (9)	O13^xvi—Na3—U1^x	102.29 (13)
O13—Na1—Na3^ix	108.64 (9)	O11—Na3—U1^x	88.81 (12)
O13^vi—Na1—Na3^ix	71.36 (9)	O1^xvii—Na3—U1^x	90.05 (16)
O13^vii—Na1—Na3^ix	67.75 (9)	O2^x—Na3—U1^x	22.64 (13)
O13^viii—Na1—Na3^ix	146.54 (9)	C1^xvi—Na3—U1^x	92.66 (10)
Na2^vi—Na1—Na3^ix	66.19 (3)	Na3^xvi—Na3—U1^x	62.09 (3)
Na2—Na1—Na3^ix	113.81 (3)	Na3^xi—Na3—U1^x	62.09 (3)
O13^iv—Na1—Na3^x	71.36 (9)	U1^xvii—Na3—U1^x	113.76 (5)
O13^v—Na1—Na3^x	33.46 (9)	Na3^iii—Na3—U1^x	161.21 (4)
O13—Na1—Na3^x	67.75 (9)	O12^i—Na3—U1	34.30 (10)
O13^vi—Na1—Na3^x	112.25 (9)	O13^xvi—Na3—U1	119.76 (11)
O13^vii—Na1—Na3^x	146.54 (9)	O11—Na3—U1	35.93 (10)
O13^viii—Na1—Na3^x	108.64 (9)	O1^xvii—Na3—U1	118.91 (9)
Na2^vi—Na1—Na3^x	66.19 (3)	O2^x—Na3—U1	119.78 (9)
Na2—Na1—Na3^x	113.81 (3)	C1^xvi—Na3—U1	140.54 (12)
Na3^ix—Na1—Na3^x	104.80 (4)	Na3^xvi—Na3—U1	156.05 (8)
O13^iv—Na1—Na3^xi	67.75 (9)	Na3^xi—Na3—U1	96.08 (8)
O13^v—Na1—Na3^xi	108.64 (9)	U1^xvii—Na3—U1	107.89 (5)
O13—Na1—Na3^xi	33.46 (9)	Na3^iii—Na3—U1	58.91 (5)
O13^vi—Na1—Na3^xi	146.54 (9)	U1^x—Na3—U1	109.66 (5)
O13^vii—Na1—Na3^xi	71.36 (9)	O13—C1—O12	124.0 (4)
O13^viii—Na1—Na3^xi	112.25 (9)	O13—C1—O11	123.5 (5)
Na2^vi—Na1—Na3^xi	113.81 (3)	O12—C1—O11	112.5 (4)
Na2—Na1—Na3^xi	66.19 (3)	O13—C1—U1	176.7 (3)
Na3^ix—Na1—Na3^xi	75.20 (4)	O12—C1—U1	55.3 (2)
Na3^x—Na1—Na3^xi	75.20 (4)	O11—C1—U1	57.2 (2)
O13^iv—Na1—Na3^ii	146.54 (9)	O13—C1—Na3^xi	41.8 (2)
O13^v—Na1—Na3^ii	67.75 (9)	O12—C1—Na3^xi	163.8 (3)
O13—Na1—Na3^ii	71.36 (9)	O11—C1—Na3^xi	82.3 (3)
O13^vi—Na1—Na3^ii	108.64 (9)	U1—C1—Na3^xi	139.37 (19)
O13^vii—Na1—Na3^ii	112.25 (9)	C1—O11—Na3	153.2 (3)
O13^viii—Na1—Na3^ii	33.46 (9)	C1—O11—U1	95.8 (3)
Na2^vi—Na1—Na3^ii	113.81 (3)	Na3—O11—U1	109.57 (15)
Na2—Na1—Na3^ii	66.19 (3)	C1—O12—Na3^ii	144.4 (3)
Na3^ix—Na1—Na3^ii	180.0	C1—O12—U1	97.9 (3)
Na3^x—Na1—Na3^ii	75.20 (4)	Na3^ii—O12—U1	112.90 (16)
Na3^xi—Na1—Na3^ii	104.80 (4)	C1—O13—Na3^xi	117.2 (3)
O13^vii—Na2—O13^viii	81.30 (12)	C1—O13—Na1	118.9 (3)
O13^vii—Na2—O13^xii	83.99 (15)	Na3^xi—O13—Na1	111.09 (15)
O13^viii—Na2—O13^xii	148.55 (15)	C1—O13—Na2	113.0 (3)
O13^vii—Na2—O13^iii	148.55 (15)	Na3^xi—O13—Na2	109.85 (16)
O13^viii—Na2—O13^iii	123.64 (16)	Na1—O13—Na2	81.01 (10)
O13^xii—Na2—O13^iii	81.30 (12)	U1—O1—Na3^iii	122.77 (15)
O13^vii—Na2—O13^xiii	123.64 (16)	U1—O1—Na3^xviii	122.77 (15)
O13^viii—Na2—O13^xiii	83.99 (15)	Na3^iii—O1—Na3^xviii	93.5 (2)
O13^xii—Na2—O13^xiii	81.30 (12)	U1—O1—Na3^xix	122.77 (15)
O13^iii—Na2—O13^xiii	81.30 (12)	Na3^iii—O1—Na3^xix	93.5 (2)
O13^vii—Na2—O13	81.30 (12)	Na3^xviii—O1—Na3^xix	93.5 (2)
O13^viii—Na2—O13	81.30 (12)	U1—O2—Na3^x	124.65 (14)
O13^xii—Na2—O13	123.64 (16)	U1—O2—Na3^xx	124.65 (14)
O13^iii—Na2—O13	83.99 (15)	Na3^x—O2—Na3^xx	90.9 (2)
O13^xiii—Na2—O13	148.55 (15)	U1—O2—Na3^v	124.65 (14)
O13^vii—Na2—Na1	48.79 (8)	Na3^x—O2—Na3^v	90.9 (2)
O13^viii—Na2—Na1	48.79 (8)	Na3^xx—O2—Na3^v	90.9 (2)

Symmetry codes: (i) −x+y, −x+1, z; (ii) −y+1, x−y+1, z; (iii) −x, −x+y, −z+1/2; (iv) x−y, x, −z; (v) y, −x+y, −z; (vi) −x, −y, −z; (vii) −y, x−y, z; (viii) −x+y, −x, z; (ix) y−1, −x+y−1, −z; (x) −x, −y+1, −z; (xi) −x+y−1, −x, z; (xii) x−y, −y, −z+1/2; (xiii) y, x, −z+1/2; (xiv) x, y−1, z; (xv) y−1, x, −z+1/2; (xvi) −y, x−y+1, z; (xvii) x−y, −y+1, −z+1/2; (xviii) y, x+1, −z+1/2; (xix) x−y+1, −y+1, −z+1/2; (xx) x−y+1, x+1, −z.