From a solution containing uranyl nitrate and sodium citrate, single crystals of trisodium citrate dihydrate, 3Na+·C6H5O73-·2H2O, were obtained. The structure consists of a complex network of citrate and sodium ions. Additionally, hydrogen bonds between the citrate ions and the water of crystallization are formed.
Supporting information
CCDC reference: 226687
Key indicators
- Single-crystal X-ray study
- T = 299 K
- Mean (C-C) = 0.003 Å
- R factor = 0.040
- wR factor = 0.093
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.57 Ratio
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 42.78 Deg.
O1 -C1 -NA1 1.555 1.555 1.555
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: KappaCCD Software (Nonius, 1997); cell refinement: HKL SCALEPACK; data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: maXus (Mackay et al., 1997).
Crystal data top
3Na+·C6H5O73−·2H2O | F(000) = 1200 |
Mr = 294.10 | Dx = 1.814 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3843 reflections |
a = 15.7044 (4) Å | θ = 4.5–27.5° |
b = 12.5010 (4) Å | µ = 0.27 mm−1 |
c = 11.2837 (4) Å | T = 299 K |
β = 103.5841 (13)° | Cuboid, colourless |
V = 2153.26 (12) Å3 | 0.20 × 0.15 × 0.10 mm |
Z = 8 | |
Data collection top
Bruker–Nonius KappaCCD diffractometer | Rint = 0.055 |
Radiation source: fine-focus sealed tube | θmax = 27.5°, θmin = 4.5° |
ω scans | h = −17→20 |
8459 measured reflections | k = −14→16 |
2451 independent reflections | l = −14→12 |
1643 reflections with I > 2σ(I) | |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.093 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0385P)2 + 0.6276P] where P = (Fo2 + 2Fc2)/3 |
2451 reflections | (Δ/σ)max < 0.001 |
178 parameters | Δρmax = 0.43 e Å−3 |
6 restraints | Δρmin = −0.32 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 >
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C1 | 0.32032 (12) | 0.26746 (17) | −0.12039 (18) | 0.0167 (5) | |
C2 | 0.40138 (12) | 0.20513 (18) | −0.13157 (19) | 0.0195 (5) | |
H2A | 0.3843 | 0.1320 | −0.1542 | 0.023* | |
H2B | 0.4238 | 0.2360 | −0.1971 | 0.023* | |
C3 | 0.47454 (11) | 0.20354 (17) | −0.01659 (18) | 0.0157 (5) | |
C4 | 0.54966 (12) | 0.13205 (18) | −0.03589 (19) | 0.0205 (5) | |
H4A | 0.5241 | 0.0686 | −0.0795 | 0.025* | |
H4B | 0.5802 | 0.1701 | −0.0884 | 0.025* | |
C5 | 0.61747 (13) | 0.09605 (18) | 0.0773 (2) | 0.0232 (5) | |
C6 | 0.51190 (11) | 0.31612 (18) | 0.01854 (19) | 0.0166 (5) | |
Na1 | 0.39983 (5) | 0.49615 (7) | −0.10199 (8) | 0.0254 (2) | |
Na2 | 0.38687 (5) | 0.32751 (7) | 0.17398 (7) | 0.0248 (2) | |
Na3 | 0.31278 (5) | 0.07827 (7) | 0.12757 (8) | 0.0290 (2) | |
O1 | 0.32920 (8) | 0.34512 (12) | −0.04739 (13) | 0.0212 (3) | |
O2 | 0.24806 (9) | 0.23955 (13) | −0.18727 (14) | 0.0272 (4) | |
O3 | 0.69001 (10) | 0.06577 (17) | 0.06113 (16) | 0.0461 (5) | |
O4 | 0.59581 (9) | 0.09256 (14) | 0.17743 (14) | 0.0309 (4) | |
O5 | 0.52668 (9) | 0.37453 (13) | −0.06565 (14) | 0.0257 (4) | |
O6 | 0.52678 (8) | 0.34375 (12) | 0.12801 (13) | 0.0221 (4) | |
O7 | 0.43809 (9) | 0.16051 (12) | 0.07907 (13) | 0.0194 (3) | |
H7 | 0.4811 (14) | 0.1391 (19) | 0.130 (2) | 0.023* | |
O8 | 0.35892 (10) | 0.51957 (14) | 0.18550 (15) | 0.0293 (4) | |
H8A | 0.3903 (12) | 0.5577 (19) | 0.157 (2) | 0.035* | |
H8B | 0.3062 (10) | 0.534 (2) | 0.153 (2) | 0.035* | |
O9 | 0.23658 (10) | −0.08770 (14) | 0.13185 (16) | 0.0320 (4) | |
H9A | 0.2578 (16) | −0.105 (2) | 0.0759 (17) | 0.038* | |
H9B | 0.2422 (16) | −0.1312 (18) | 0.1864 (18) | 0.038* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0171 (10) | 0.0176 (12) | 0.0148 (11) | −0.0018 (8) | 0.0024 (8) | 0.0056 (9) |
C2 | 0.0162 (10) | 0.0202 (12) | 0.0203 (11) | −0.0001 (9) | 0.0008 (8) | −0.0056 (9) |
C3 | 0.0140 (9) | 0.0186 (12) | 0.0150 (11) | 0.0001 (8) | 0.0045 (8) | 0.0012 (9) |
C4 | 0.0189 (10) | 0.0228 (13) | 0.0194 (12) | 0.0046 (9) | 0.0040 (8) | −0.0011 (10) |
C5 | 0.0210 (11) | 0.0242 (13) | 0.0244 (13) | 0.0026 (9) | 0.0053 (9) | 0.0030 (10) |
C6 | 0.0091 (9) | 0.0187 (12) | 0.0215 (12) | 0.0014 (8) | 0.0023 (8) | 0.0016 (10) |
Na1 | 0.0225 (4) | 0.0211 (5) | 0.0301 (5) | −0.0031 (4) | 0.0013 (4) | 0.0031 (4) |
Na2 | 0.0196 (4) | 0.0303 (5) | 0.0240 (5) | −0.0031 (4) | 0.0043 (3) | −0.0051 (4) |
Na3 | 0.0185 (4) | 0.0289 (6) | 0.0372 (6) | −0.0015 (4) | 0.0022 (4) | 0.0035 (4) |
O1 | 0.0193 (7) | 0.0198 (9) | 0.0235 (8) | 0.0005 (6) | 0.0028 (6) | −0.0032 (7) |
O2 | 0.0138 (7) | 0.0349 (10) | 0.0297 (9) | −0.0028 (6) | −0.0014 (6) | −0.0074 (8) |
O3 | 0.0225 (9) | 0.0781 (15) | 0.0398 (11) | 0.0235 (9) | 0.0115 (7) | 0.0209 (10) |
O4 | 0.0245 (8) | 0.0466 (12) | 0.0207 (9) | 0.0089 (7) | 0.0034 (6) | 0.0061 (8) |
O5 | 0.0246 (8) | 0.0259 (9) | 0.0269 (9) | −0.0039 (7) | 0.0066 (6) | 0.0076 (7) |
O6 | 0.0222 (7) | 0.0242 (9) | 0.0190 (8) | −0.0065 (6) | 0.0028 (6) | −0.0047 (7) |
O7 | 0.0158 (7) | 0.0219 (9) | 0.0207 (8) | −0.0004 (6) | 0.0047 (6) | 0.0032 (7) |
O8 | 0.0207 (8) | 0.0350 (11) | 0.0309 (10) | 0.0001 (7) | 0.0032 (7) | 0.0090 (8) |
O9 | 0.0329 (9) | 0.0341 (11) | 0.0305 (11) | 0.0070 (8) | 0.0105 (8) | 0.0064 (8) |
Geometric parameters (Å, º) top
C1—O2 | 1.256 (2) | Na1—C6ii | 2.775 (2) |
C1—O1 | 1.260 (2) | Na1—Na2iii | 3.3240 (12) |
C1—C2 | 1.523 (3) | Na1—Na3i | 3.4123 (11) |
C1—Na3i | 2.831 (2) | Na1—Na1ii | 3.4358 (16) |
C1—Na1 | 3.107 (2) | Na2—O2i | 2.3163 (16) |
C2—C3 | 1.518 (3) | Na2—O6iv | 2.3342 (16) |
C2—H2A | 0.9700 | Na2—O6 | 2.3819 (15) |
C2—H2B | 0.9700 | Na2—O8 | 2.450 (2) |
C3—O7 | 1.440 (2) | Na2—O1 | 2.4588 (16) |
C3—C4 | 1.536 (3) | Na2—O7 | 2.5606 (17) |
C3—C6 | 1.540 (3) | Na2—Na3 | 3.3241 (13) |
C4—C5 | 1.526 (3) | Na2—Na2iv | 3.5644 (15) |
C4—H4A | 0.9700 | Na2—Na3i | 4.2172 (12) |
C4—H4B | 0.9700 | Na3—O4iv | 2.3346 (17) |
C5—O3 | 1.254 (3) | Na3—O7 | 2.3947 (15) |
C5—O4 | 1.255 (2) | Na3—O1i | 2.3999 (15) |
C6—O6 | 1.251 (2) | Na3—O9 | 2.4013 (19) |
C6—O5 | 1.262 (2) | Na3—O2i | 2.6184 (17) |
C6—Na1ii | 2.775 (2) | Na3—O3v | 2.781 (2) |
C6—Na2 | 2.927 (2) | Na3—C1i | 2.831 (2) |
C6—Na1 | 2.981 (2) | Na3—H9A | 2.47 (3) |
Na1—O8iii | 2.3404 (18) | O7—H7 | 0.82 (2) |
Na1—O1 | 2.3442 (16) | O8—H8A | 0.803 (15) |
Na1—O6ii | 2.3621 (16) | O8—H8B | 0.840 (15) |
Na1—O9i | 2.3819 (17) | O9—Na1i | 2.3819 (17) |
Na1—O5 | 2.4627 (17) | O9—H9A | 0.808 (15) |
Na1—O5ii | 2.5492 (18) | O9—H9B | 0.810 (16) |
| | | |
O2—C1—O1 | 123.56 (18) | O8—Na2—Na1vi | 44.72 (4) |
O2—C1—C2 | 117.58 (18) | O1—Na2—Na1vi | 130.95 (5) |
O1—C1—C2 | 118.84 (17) | O7—Na2—Na1vi | 152.82 (5) |
O2—C1—Na3i | 67.37 (11) | C6—Na2—Na1vi | 123.92 (5) |
O1—C1—Na3i | 57.40 (10) | O2i—Na2—Na3 | 51.63 (4) |
C2—C1—Na3i | 166.43 (14) | O6iv—Na2—Na3 | 109.60 (5) |
O2—C1—Na1 | 126.02 (14) | O6—Na2—Na3 | 110.62 (5) |
O1—C1—Na1 | 42.78 (9) | O8—Na2—Na3 | 150.06 (5) |
C2—C1—Na1 | 98.38 (12) | O1—Na2—Na3 | 83.80 (4) |
Na3i—C1—Na1 | 69.97 (5) | O7—Na2—Na3 | 45.78 (4) |
C3—C2—C1 | 114.56 (17) | C6—Na2—Na3 | 96.85 (5) |
C3—C2—H2A | 108.6 | Na1vi—Na2—Na3 | 134.27 (3) |
C1—C2—H2A | 108.6 | O2i—Na2—Na2iv | 142.43 (5) |
C3—C2—H2B | 108.6 | O6iv—Na2—Na2iv | 41.41 (4) |
C1—C2—H2B | 108.6 | O6—Na2—Na2iv | 40.41 (4) |
H2A—C2—H2B | 107.6 | O8—Na2—Na2iv | 98.35 (4) |
O7—C3—C2 | 106.94 (15) | O1—Na2—Na2iv | 125.22 (5) |
O7—C3—C4 | 110.05 (16) | O7—Na2—Na2iv | 79.97 (4) |
C2—C3—C4 | 109.81 (16) | C6—Na2—Na2iv | 63.60 (4) |
O7—C3—C6 | 110.05 (16) | Na1vi—Na2—Na2iv | 75.99 (3) |
C2—C3—C6 | 111.97 (17) | Na3—Na2—Na2iv | 110.384 (19) |
C4—C3—C6 | 108.02 (15) | O2i—Na2—Na1 | 118.62 (5) |
C5—C4—C3 | 117.47 (17) | O6iv—Na2—Na1 | 127.19 (5) |
C5—C4—H4A | 107.9 | O6—Na2—Na1 | 62.95 (4) |
C3—C4—H4A | 107.9 | O8—Na2—Na1 | 62.94 (4) |
C5—C4—H4B | 107.9 | O1—Na2—Na1 | 36.56 (4) |
C3—C4—H4B | 107.9 | O7—Na2—Na1 | 91.55 (4) |
H4A—C4—H4B | 107.2 | C6—Na2—Na1 | 50.53 (4) |
O3—C5—O4 | 124.6 (2) | Na1vi—Na2—Na1 | 104.44 (2) |
O3—C5—C4 | 116.52 (19) | Na3—Na2—Na1 | 118.32 (3) |
O4—C5—C4 | 118.71 (17) | Na2iv—Na2—Na1 | 98.92 (3) |
O6—C6—O5 | 124.0 (2) | O2i—Na2—Na3i | 68.60 (4) |
O6—C6—C3 | 118.56 (18) | O6iv—Na2—Na3i | 154.51 (5) |
O5—C6—C3 | 117.45 (18) | O6—Na2—Na3i | 110.46 (5) |
O6—C6—Na1ii | 57.92 (11) | O8—Na2—Na3i | 70.16 (4) |
O5—C6—Na1ii | 66.47 (11) | O1—Na2—Na3i | 29.38 (3) |
C3—C6—Na1ii | 171.72 (13) | O7—Na2—Na3i | 97.89 (4) |
O6—C6—Na2 | 52.47 (9) | C6—Na2—Na3i | 90.36 (4) |
O5—C6—Na2 | 133.68 (14) | Na1vi—Na2—Na3i | 109.24 (3) |
C3—C6—Na2 | 85.99 (10) | Na3—Na2—Na3i | 88.18 (3) |
Na1ii—C6—Na2 | 96.17 (7) | Na2iv—Na2—Na3i | 148.93 (3) |
O6—C6—Na1 | 101.28 (13) | Na1—Na2—Na3i | 50.023 (19) |
O5—C6—Na1 | 54.07 (10) | O4iv—Na3—O7 | 79.99 (6) |
C3—C6—Na1 | 115.08 (12) | O4iv—Na3—O1i | 129.49 (6) |
Na1ii—C6—Na1 | 73.19 (6) | O7—Na3—O1i | 118.89 (6) |
Na2—C6—Na1 | 80.18 (5) | O4iv—Na3—O9 | 104.25 (7) |
O8iii—Na1—O1 | 99.71 (6) | O7—Na3—O9 | 144.65 (7) |
O8iii—Na1—O6ii | 88.18 (6) | O1i—Na3—O9 | 85.93 (6) |
O1—Na1—O6ii | 171.85 (6) | O4iv—Na3—O2i | 82.63 (6) |
O8iii—Na1—O9i | 82.77 (6) | O7—Na3—O2i | 93.12 (6) |
O1—Na1—O9i | 87.64 (6) | O1i—Na3—O2i | 52.20 (5) |
O6ii—Na1—O9i | 91.38 (6) | O9—Na3—O2i | 122.19 (6) |
O8iii—Na1—O5 | 97.78 (6) | O4iv—Na3—O3v | 131.82 (6) |
O1—Na1—O5 | 82.72 (5) | O7—Na3—O3v | 88.23 (6) |
O6ii—Na1—O5 | 98.31 (6) | O1i—Na3—O3v | 97.10 (5) |
O9i—Na1—O5 | 170.30 (6) | O9—Na3—O3v | 62.46 (6) |
O8iii—Na1—O5ii | 141.35 (6) | O2i—Na3—O3v | 144.99 (6) |
O1—Na1—O5ii | 118.39 (6) | O4iv—Na3—C1i | 105.15 (7) |
O6ii—Na1—O5ii | 53.54 (5) | O7—Na3—C1i | 109.99 (6) |
O9i—Na1—O5ii | 92.04 (6) | O1i—Na3—C1i | 26.24 (5) |
O5—Na1—O5ii | 93.46 (6) | O9—Na3—C1i | 102.77 (6) |
O8iii—Na1—C6ii | 114.43 (7) | O2i—Na3—C1i | 26.27 (5) |
O1—Na1—C6ii | 145.22 (7) | O3v—Na3—C1i | 122.71 (6) |
O6ii—Na1—C6ii | 26.65 (5) | O4iv—Na3—Na2 | 70.42 (5) |
O9i—Na1—C6ii | 90.15 (6) | O7—Na3—Na2 | 50.03 (4) |
O5—Na1—C6ii | 98.36 (6) | O1i—Na3—Na2 | 86.86 (5) |
O5ii—Na1—C6ii | 27.00 (5) | O9—Na3—Na2 | 164.66 (5) |
O8iii—Na1—C6 | 113.24 (6) | O2i—Na3—Na2 | 43.91 (4) |
O1—Na1—C6 | 62.43 (5) | O3v—Na3—Na2 | 132.03 (5) |
O6ii—Na1—C6 | 116.32 (6) | C1i—Na3—Na2 | 66.10 (5) |
O9i—Na1—C6 | 147.38 (6) | O4iv—Na3—Na1i | 118.26 (5) |
O5—Na1—C6 | 24.52 (5) | O7—Na3—Na1i | 159.71 (5) |
O5ii—Na1—C6 | 91.39 (6) | O1i—Na3—Na1i | 43.36 (4) |
C6ii—Na1—C6 | 106.81 (6) | O9—Na3—Na1i | 44.26 (4) |
O8iii—Na1—C1 | 81.08 (6) | O2i—Na3—Na1i | 81.37 (4) |
O1—Na1—C1 | 21.41 (5) | O3v—Na3—Na1i | 85.38 (4) |
O6ii—Na1—C1 | 166.29 (6) | C1i—Na3—Na1i | 58.81 (4) |
O9i—Na1—C1 | 95.66 (6) | Na2—Na3—Na1i | 124.63 (3) |
O5—Na1—C1 | 74.92 (5) | O4iv—Na3—Na2i | 156.23 (5) |
O5ii—Na1—C1 | 137.55 (6) | O7—Na3—Na2i | 101.00 (5) |
C6ii—Na1—C1 | 164.07 (7) | O1i—Na3—Na2i | 30.18 (4) |
C6—Na1—C1 | 61.37 (5) | O9—Na3—Na2i | 88.74 (5) |
O8iii—Na1—Na2iii | 47.43 (5) | O2i—Na3—Na2i | 73.60 (4) |
O1—Na1—Na2iii | 141.79 (5) | O3v—Na3—Na2i | 71.82 (4) |
O6ii—Na1—Na2iii | 44.60 (4) | C1i—Na3—Na2i | 51.88 (4) |
O9i—Na1—Na2iii | 71.42 (5) | Na2—Na3—Na2i | 91.82 (3) |
O5—Na1—Na2iii | 116.02 (5) | Na1i—Na3—Na2i | 58.71 (2) |
O5ii—Na1—Na2iii | 94.58 (4) | O4iv—Na3—H9A | 113.4 (5) |
C6ii—Na1—Na2iii | 68.51 (5) | O7—Na3—H9A | 127.2 (4) |
C6—Na1—Na2iii | 140.51 (5) | O1i—Na3—H9A | 92.2 (6) |
C1—Na1—Na2iii | 127.41 (5) | O9—Na3—H9A | 19.0 (4) |
O8iii—Na1—Na3i | 82.11 (5) | O2i—Na3—H9A | 137.6 (5) |
O1—Na1—Na3i | 44.66 (4) | O3v—Na3—H9A | 43.7 (4) |
O6ii—Na1—Na3i | 135.79 (5) | C1i—Na3—H9A | 114.2 (5) |
O9i—Na1—Na3i | 44.72 (5) | Na2—Na3—H9A | 175.5 (4) |
O5—Na1—Na3i | 125.66 (5) | Na1i—Na3—H9A | 56.3 (5) |
O5ii—Na1—Na3i | 119.94 (5) | Na2i—Na3—H9A | 85.2 (6) |
C6ii—Na1—Na3i | 131.31 (5) | C1—O1—Na1 | 115.81 (12) |
C6—Na1—Na3i | 107.09 (5) | C1—O1—Na3i | 96.36 (12) |
C1—Na1—Na3i | 51.22 (4) | Na1—O1—Na3i | 91.98 (6) |
Na2iii—Na1—Na3i | 103.45 (3) | C1—O1—Na2 | 123.58 (13) |
O8iii—Na1—Na1ii | 132.57 (6) | Na1—O1—Na2 | 104.77 (6) |
O1—Na1—Na1ii | 105.18 (5) | Na3i—O1—Na2 | 120.44 (6) |
O6ii—Na1—Na1ii | 70.29 (4) | C1—O2—Na2i | 140.63 (14) |
O9i—Na1—Na1ii | 137.13 (6) | C1—O2—Na3i | 86.36 (12) |
O5—Na1—Na1ii | 47.78 (4) | Na2i—O2—Na3i | 84.46 (5) |
O5ii—Na1—Na1ii | 45.68 (4) | C5—O3—Na3v | 117.09 (16) |
C6ii—Na1—Na1ii | 56.16 (5) | C5—O4—Na3iv | 127.92 (13) |
C6—Na1—Na1ii | 50.65 (4) | C6—O5—Na1 | 101.41 (12) |
C1—Na1—Na1ii | 111.16 (5) | C6—O5—Na1ii | 86.54 (12) |
Na2iii—Na1—Na1ii | 111.94 (4) | Na1—O5—Na1ii | 86.54 (6) |
Na3i—Na1—Na1ii | 142.02 (4) | C6—O6—Na2iv | 148.56 (13) |
O2i—Na2—O6iv | 107.71 (6) | C6—O6—Na1ii | 95.43 (12) |
O2i—Na2—O6 | 161.75 (7) | Na2iv—O6—Na1ii | 90.11 (6) |
O6iv—Na2—O6 | 80.96 (6) | C6—O6—Na2 | 102.92 (11) |
O2i—Na2—O8 | 99.97 (6) | Na2iv—O6—Na2 | 98.18 (6) |
O6iv—Na2—O8 | 86.28 (6) | Na1ii—O6—Na2 | 126.96 (7) |
O6—Na2—O8 | 96.55 (6) | C3—O7—Na3 | 145.55 (12) |
O2i—Na2—O1 | 88.50 (5) | C3—O7—Na2 | 103.20 (11) |
O6iv—Na2—O1 | 163.17 (6) | Na3—O7—Na2 | 84.19 (5) |
O6—Na2—O1 | 84.82 (5) | C3—O7—H7 | 103.8 (15) |
O8—Na2—O1 | 86.46 (6) | Na3—O7—H7 | 106.6 (15) |
O2i—Na2—O7 | 96.55 (6) | Na2—O7—H7 | 105.1 (16) |
O6iv—Na2—O7 | 107.60 (6) | Na1vi—O8—Na2 | 87.86 (6) |
O6—Na2—O7 | 65.29 (5) | Na1vi—O8—H8A | 114.2 (18) |
O8—Na2—O7 | 154.04 (6) | Na2—O8—H8A | 115.2 (18) |
O1—Na2—O7 | 74.04 (5) | Na1vi—O8—H8B | 117.6 (16) |
O2i—Na2—C6 | 140.69 (6) | Na2—O8—H8B | 110.7 (17) |
O6iv—Na2—C6 | 104.90 (6) | H8A—O8—H8B | 110 (2) |
O6—Na2—C6 | 24.61 (5) | Na1i—O9—Na3 | 91.02 (6) |
O8—Na2—C6 | 103.49 (6) | Na1i—O9—H9A | 122.5 (18) |
O1—Na2—C6 | 62.26 (5) | Na3—O9—H9A | 85.1 (19) |
O7—Na2—C6 | 52.34 (5) | Na1i—O9—H9B | 111.3 (17) |
O2i—Na2—Na1vi | 94.84 (5) | Na3—O9—H9B | 129.0 (19) |
O6iv—Na2—Na1vi | 45.28 (4) | H9A—O9—H9B | 115 (2) |
O6—Na2—Na1vi | 102.37 (5) | | |
Symmetry codes: (i) −x+1/2, −y+1/2, −z; (ii) −x+1, −y+1, −z; (iii) x, −y+1, z−1/2; (iv) −x+1, y, −z+1/2; (v) −x+1, −y, −z; (vi) x, −y+1, z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7···O4 | 0.82 (2) | 1.85 (2) | 2.6072 (19) | 153 (2) |
O8—H8A···O5ii | 0.80 (2) | 2.03 (2) | 2.820 (2) | 168 (3) |
O8—H8B···O3vii | 0.84 (2) | 1.92 (2) | 2.755 (2) | 173 (2) |
O9—H9A···O3v | 0.81 (2) | 1.97 (2) | 2.706 (2) | 150 (2) |
O9—H9B···O2viii | 0.81 (2) | 1.95 (2) | 2.762 (2) | 176 (3) |
Symmetry codes: (ii) −x+1, −y+1, −z; (v) −x+1, −y, −z; (vii) x−1/2, y+1/2, z; (viii) x, −y, z+1/2. |