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In the title compound, [Na4(C8H16BO4)4(C4H10O2)]n, there are two coordination types for the four independent Na+ cations: two Na+ cations bond to six diolate O atoms [Na—O = 2.305 (2)–2.609 (2) Å], while the other two are five-coordinate via one 1,4-butane­diol [2.289 (2) and 2.349 (3) Å] and four diolate O atoms [2.295 (2)–2.408 (2) Å]. Corresponding to this, there are three- and four-coordinate diolate O atoms, the latter bridging Na atoms. The 1,4-butane­diol mol­ecules lie on inversion centres. The boron stereochemistry shows minor local perturbations from its usual tetrahedral state [B—O = 1.457 (4)–1.503 (4) Å]. The resulting polymer packs as sheets parallel to the (10\overline{1}) plane crosslinked by the butane­diol mol­ecules. The structure was solved using data from a multiple crystal.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105002520/fg1811sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105002520/fg1811Isup2.hkl
Contains datablock I

CCDC reference: 268083

Comment top

This study is part of a programme aimed at investigating boron diolates and alkoxides (Gainsford & Kemmitt, 2004). Although borates form a range of diolate complexes (Bachelier & Verchere, 1995; Springsteen & Wang, 2002), structural data are sparse, and no 1,4-diolates have been reported to date. Low solubility prevented us from obtaining useful NMR data, and the presence of hydroxyl groups of a `free' diol molecule in the structure made it difficult to determine the coordination mode of the diolate ligands by other techniques. Thus, in order to confirm the chelating nature of the 1,4-diolate ligand, we have carried out the present single-crystal X-ray analysis of the title compound, (I).

The basic polymeric fragment of (I), with asymmetric unit formula [Na4(C8H16BO4)4(C4H10O2)]n, is illustrated in Fig. 1. The use of the word `bound' here indicates atoms that are within either covalent or ionic attractive distances of each other. The Na+ cations are of two types. Cations Na1 and Na3 are bound to six O atoms, with four of these being monocoordinate diolate O atoms [Na—O 2.305 (2)–2.499 (2) Å] and two being shared with adjacent Na+ [2.459 (2)–2.609 (2) Å]. Cations Na2 and Na4 are five-coordinated through four diolate O atoms, one of which is shared [O2 2.355 (2) and O16 2.334 (2) Å], with the other three being monocoordinated [2.342 (2)–2.408 (2) Å]; the fifth position is taken by a singly coordinated butanediol O atom [O8 2.289 (2) and O15 2.349 (3) Å]. None of the Na+ cation geometries approaches an idealized stereochemistry. The butanediol molecules lie on inversion centres (see Fig. 1 and comments below).

The B atoms in the (butanedioxy)borate anions show minor perturbations from tetrahedral geometry, with B—O bond length and O—B—O angle ranges of 1.457 (4)–1.503 (4) Å and 101.8 (2)–115.1 (2)°, respectively. These variations can be related to the longer bonds involving O atoms bridging Na atoms (O2, O3, O13 and O16), with a mean B—O distance for these of 1.487 (4) Å, compared with the mean of 1.470 (13) Å for the other 12 three-coordinate O atoms. Thus, four diolate O atoms (O2, O3, O13 and O16) are four-coordinate through bridging two Na+ cations, and bond to one B atom and one methylene C atom; the remaining O atoms bond to one B atom, one C atom and one Na+ cation.

The polymeric units of (I) form sheets parallel to the (101) plane and are linked by two bound butanediol links per cell (Fig. 3). The butanediol H atoms are involved in strong intramolecular binding, strengthening these links (Fig. 1, Table 2). The contents of one sheet are shown in Fig. 2. The internal ring consists of 12 B—O and 16 Na—O bonds, involving eight Na and eight B atoms. The links between the sheets involve crystallographic inversion centres at the centres of the butanediol molecules (so the asymmetric unit shown in Fig. 1 reflects incomplete links), through Na2—O8—C9—C10—C10ii—C9ii—O8ii—Na2ii and Na4—O15—C27—C28—C28iii—C27iii—O15iii—Na4iii [symmetry codes: (ii) 1 − x, 2 − y, 1 − z; (iii) 2 − x, 1 − y, −z].

The title compound has a unique structure, with no directly comparable compounds containing seven-membered dioxygenboron rings; the closest two are a bis[ethylborandiyl-bis(oxy)]cyclobutane compound (Yalpani et al., 1983) and sodium scylloinositoldiborate decahydrate (Grainger, 1981). In the latter, the B—O bonds range from 1.486–1.502 Å, but the Na+ cations are completely surrounded by water molecules. The long Na—O distances in (I), involving the asymmetric bridging of the five- and six-coordinate Na atoms by atoms O2 and O16, are unique with respect to the subtended angles at the O atoms (Table 1), which are usually around 90°. Examples of such bridging distances are found in bis[(µ2-hydrogentriphenylborato)bis(tetrahydrofuran)sodium] (Bishop et al., 2000) and (µ2-dibenzo-30-crown-10)aquamethanoldisodium bis(tetraphenylborate) methanol solvate (Steed et al., 2003), with Na—O distances and Na—O—Na angles of 2.386 Å, 2.650 Å and 94.16°, and 2.380 Å, 2.648 Å and 103.24°, respectively, compared with the averages (for O2 and O16) of 2.345 (15) Å, 2.606 (5) Å and 134 (2)° in (I).

Experimental top

The title compound was prepared by the addition of excess 1,4-butanediol (75 ml) to a solution of sodium metaborate, (0.1 mol, 13.8 g) in distilled water, (10 ml). Water and excess diol were removed on a rotary evaporator equipped with a high-temperature oil bath, leaving a white solid. A sample was redissolved in a minimum of 1,4-butanediol, and an equal volume of anhydrous acetonitrile was added, causing the slow growth of crystals of (I) over 4 d.

Refinement top

Details of the handling of data from a multiple crystal are given in the supplementary material. All C-bound H atoms were constrained to their expected geometries (C—H = 0.99 Å). The hydroxyl (H8O and H15O) H atoms were freely refined, with O—H restrained (DFIX) to 0.84 (3) Å. All H atoms except H8O and H15O were refined with Uiso(H) = 1.2Ueq(C); the ratio was 1.5 for H8O and H15O.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001) and SADABS (Sheldrick, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1999) and Mercury (Bruno et al., 2002); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. A view of the molecular structure of (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. Atoms of the asymmetric unit and O atoms completing the interaction spheres around the Na atoms are shown. [Symmetry codes: (i) x, y − 1, z; (ii) 1 − x, 2 − y, 1 − z; (iii) 2 − x, 1 − y, −z; (iv) 1 − x, 2 − y, −z; (v) 2 − x, 1 − y, 1 − z.] Methylene H aoms have been omitted for clarity. The two intramolecular hydrogen bonds are shown by dotted lines.
[Figure 2] Fig. 2. A ce l l-packing view of (I), approximately normal to the (101) plane. H atoms have been omitted for clarity. Na+ purple, B pink, O and a axis red, C gray, b axis green.
[Figure 3] Fig. 3. A view of (I), edge on to the polymeric sheet. The C atoms (C10 and C28) which link the sheets are shown as spheres. H atoms have been omitted for clarity. Na+ purple, B pink, O and a axis red, C gray, b axis green.
Poly[tetrasodium(I)-tetra-µ2-bis(butanedioxy)borato-µ2-butanediol] top
Crystal data top
[Na4(C8H16BO4)4(C4H10O2)]Z = 2
Mr = 930.15F(000) = 992
Triclinic, P1Dx = 1.273 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.813 (4) ÅCell parameters from 7356 reflections
b = 13.349 (4) Åθ = 2.3–26.4°
c = 14.381 (5) ŵ = 0.13 mm1
α = 89.282 (5)°T = 163 K
β = 79.966 (4)°Block, colourless
γ = 89.837 (4)°0.75 × 0.42 × 0.15 mm
V = 2421.9 (14) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
7185 independent reflections
Radiation source: fine-focus sealed tube5247 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
Detector resolution: 8.192 pixels mm-1θmax = 26.6°, θmin = 2.0°
ϕ and ω scansh = 1516
Absorption correction: multi-scan
(Blessing, 1995)
k = 1616
Tmin = 0.685, Tmax = 0.981l = 018
7185 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.060Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.154H-atom parameters constrained
S = 0.99 w = 1/[σ2(Fo2) + (0.1104P)2]
where P = (Fo2 + 2Fc2)/3
7185 reflections(Δ/σ)max = 0.007
565 parametersΔρmax = 0.36 e Å3
2 restraintsΔρmin = 0.30 e Å3
Crystal data top
[Na4(C8H16BO4)4(C4H10O2)]γ = 89.837 (4)°
Mr = 930.15V = 2421.9 (14) Å3
Triclinic, P1Z = 2
a = 12.813 (4) ÅMo Kα radiation
b = 13.349 (4) ŵ = 0.13 mm1
c = 14.381 (5) ÅT = 163 K
α = 89.282 (5)°0.75 × 0.42 × 0.15 mm
β = 79.966 (4)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
7185 independent reflections
Absorption correction: multi-scan
(Blessing, 1995)
5247 reflections with I > 2σ(I)
Tmin = 0.685, Tmax = 0.981Rint = 0.000
7185 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0602 restraints
wR(F2) = 0.154H-atom parameters constrained
S = 0.99Δρmax = 0.36 e Å3
7185 reflectionsΔρmin = 0.30 e Å3
565 parameters
Special details top

Experimental. Crystal decay was monitored by repeating the initial 10 frames at the end of the data collection and analyzing duplicate reflections. The standard 0.8 mm diameter collimator was used.

Physical examination of the crystals using polarized light did not suggest they were twinned or multiple crystals. Examination of the full sphere of collected data, after structure solution, using RLATT [Bruker (2000). RLATT. Version 3.0. Bruker AXS Inc., Madison, Wisconsin, USA.], showed distinct domains. The two major ones were related by tilting the lattice 11.5 degrees with the twinning axis defined as [−1.0,-0.941,1.0]; no obvious systematic relation between these orientations could be established. The refinement gave an R1 at this point of 20% (9523 data, 7579> 2σ(I), Rint 0.034), with many data having Fo >> Fc as expected from accidental overlap of data from the (two) lattices. Other methods were tried (e.g. using TWINLAW (Bolte, 2004)) but no satisfactory way was found to systematically remove the affected data. Data were therefore excluded from the dataset where internal agreement was outside obervational error limits using 240 OMIT records (rather than down-weighting the averages as is usual) AND by comparing the ratio of Fo**2/Fc**2: if this ratio was exceeded and the difference was greater than 2 times the standard deviation of the observation, it was excluded. This process was cross- checked with the refinement results, so that the final worst data fits showed a spread of values with both Fo>Fc and Fc< Fo. The final ratio was 1.3, giving 7186 unique data (71% of the full data shell) and with 5429 > 2σ(I). The final refinements were stable with no unusual features and the two butanediol hydrogen atoms were located at the top of the final map. It is probable that some data is still affected by overlap; however (apart from improving the R factors), the chosen conservative ratio was considered a reasonable if rather arbitrayr compromise. The full dataset is available from the authors on request.

The large ratio of maximum/minimum transmision calculated by the analytical procedure of SADABS (1996) is thought to relate to the alignment of the major and minor twin domains in the crystal coupled with sinusoidal variations in beam intensity.

Bolte, M. (2004). J. Appl. Cryst. 37, 162–165.

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
xyzUiso*/Ueq
Na10.58135 (8)1.09761 (8)0.05098 (7)0.0253 (2)
Na20.62794 (9)0.88031 (8)0.28635 (7)0.0296 (3)
Na30.90690 (9)0.59663 (8)0.46093 (7)0.0255 (2)
Na40.84284 (9)0.39200 (8)0.22452 (7)0.0299 (3)
O10.52269 (17)0.81659 (15)0.04348 (13)0.0301 (4)
O20.62450 (15)0.92840 (14)0.12879 (12)0.0253 (4)
O30.44597 (14)0.96639 (15)0.10003 (13)0.0276 (4)
O40.73562 (17)1.19106 (17)0.05013 (13)0.0343 (5)
O50.60951 (16)1.20044 (15)0.18486 (13)0.0304 (4)
O60.71330 (19)1.35245 (16)0.13252 (16)0.0409 (5)
O70.48337 (16)0.83879 (18)0.21467 (14)0.0366 (5)
O80.59096 (19)1.04334 (16)0.32755 (14)0.0358 (5)
H8O0.604 (3)1.091 (3)0.288 (2)0.054*
O90.75401 (16)0.84636 (15)0.38870 (14)0.0303 (4)
O100.68898 (16)0.72164 (14)0.30905 (13)0.0284 (4)
O110.87525 (15)0.70910 (14)0.32840 (13)0.0281 (4)
O120.74746 (15)0.67609 (15)0.45829 (13)0.0287 (4)
O131.05144 (15)0.48381 (15)0.39287 (12)0.0258 (4)
O141.00062 (16)0.32219 (14)0.43594 (14)0.0299 (4)
O150.8581 (2)0.56258 (16)0.18214 (14)0.0392 (5)
H15O0.854 (4)0.603 (3)0.223 (2)0.059*
O160.87278 (15)0.43263 (14)0.37507 (12)0.0258 (4)
O171.01482 (16)0.37296 (17)0.26848 (14)0.0345 (5)
O180.79724 (16)1.22693 (15)0.19798 (14)0.0310 (4)
B10.5188 (2)0.8856 (2)0.1217 (2)0.0261 (6)
B20.7148 (3)1.2436 (2)0.1401 (2)0.0301 (7)
B30.7660 (2)0.7383 (2)0.3720 (2)0.0235 (6)
B40.9851 (2)0.4009 (2)0.3684 (2)0.0263 (6)
C10.5767 (3)0.7228 (2)0.0509 (2)0.0355 (7)
H1A0.54240.67010.01900.043*
H1B0.57020.70340.11840.043*
C20.6929 (3)0.7289 (2)0.0072 (2)0.0395 (7)
H2A0.72510.66160.00910.047*
H2B0.69920.74960.05990.047*
C30.7537 (3)0.8019 (2)0.0570 (2)0.0361 (7)
H3A0.82890.80100.02570.043*
H3B0.75090.77810.12290.043*
C40.7145 (2)0.9096 (2)0.0590 (2)0.0312 (6)
H4A0.77260.95420.06990.037*
H4B0.69710.92710.00360.037*
C50.3847 (3)1.0188 (3)0.1772 (2)0.0399 (8)
H5A0.36691.08640.15540.048*
H5B0.42741.02700.22770.048*
C60.2819 (3)0.9622 (4)0.2172 (2)0.0549 (10)
H6A0.24720.94220.16390.066*
H6B0.23331.00860.25680.066*
C70.2967 (3)0.8677 (4)0.2767 (3)0.0586 (11)
H7A0.31620.88880.33710.070*
H7B0.22810.83200.29170.070*
C80.3798 (3)0.7957 (3)0.2293 (2)0.0506 (10)
H8A0.37920.73440.26890.061*
H8B0.36230.77600.16770.061*
C90.6020 (3)1.0841 (2)0.4160 (2)0.0360 (7)
H9A0.56251.14810.42570.043*
H9B0.67771.09780.41710.043*
C100.5584 (2)1.0093 (2)0.4952 (2)0.0361 (7)
H10A0.59640.94480.48290.043*
H10B0.57341.03490.55590.043*
C110.8264 (3)0.8901 (2)0.4409 (2)0.0360 (7)
H11A0.85110.83840.48200.043*
H11B0.79000.94320.48180.043*
C120.9199 (3)0.9341 (2)0.3765 (3)0.0428 (8)
H12A0.96280.97250.41460.051*
H12B0.89410.98170.33220.051*
C130.9912 (3)0.8561 (3)0.3193 (2)0.0416 (8)
H13A1.04460.89190.27260.050*
H13B1.02970.81880.36270.050*
C140.9346 (2)0.7812 (2)0.2671 (2)0.0337 (6)
H14A0.88610.81780.23200.040*
H14B0.98760.74600.22040.040*
C150.6272 (3)0.6335 (2)0.3178 (2)0.0344 (7)
H15A0.67260.57560.32780.041*
H15B0.60030.62280.25820.041*
C160.5335 (2)0.6380 (3)0.3995 (2)0.0415 (8)
H16A0.48110.58650.38980.050*
H16B0.49900.70430.39810.050*
C170.5632 (2)0.6213 (3)0.4978 (2)0.0387 (7)
H17A0.49880.63030.54610.046*
H17B0.58720.55120.50260.046*
C180.6486 (2)0.6900 (3)0.5203 (2)0.0362 (7)
H18A0.62550.76040.51540.043*
H18B0.65860.67750.58620.043*
C191.0959 (2)0.5551 (2)0.32040 (19)0.0319 (6)
H19A1.10840.61950.35000.038*
H19B1.04470.56730.27730.038*
C201.2002 (3)0.5173 (3)0.2636 (2)0.0406 (7)
H20A1.23840.57480.22930.049*
H20B1.24460.49060.30810.049*
C211.1880 (2)0.4363 (3)0.1926 (2)0.0426 (8)
H21A1.15390.46580.14190.051*
H21B1.25920.41220.16340.051*
C221.1224 (3)0.3478 (3)0.2367 (2)0.0408 (8)
H22A1.12630.29380.18970.049*
H22B1.15310.32160.29080.049*
C230.9534 (3)0.2277 (2)0.4258 (2)0.0371 (7)
H23A0.99820.17400.44600.044*
H23B0.94960.21740.35840.044*
C240.8428 (3)0.2205 (2)0.4839 (2)0.0390 (7)
H24A0.84720.23310.55080.047*
H24B0.81650.15130.48000.047*
C250.7619 (3)0.2935 (2)0.4535 (2)0.0370 (7)
H25A0.75110.27590.38910.044*
H25B0.69330.28470.49660.044*
C260.7943 (2)0.4033 (2)0.45337 (19)0.0296 (6)
H26A0.73050.44550.45360.036*
H26B0.82150.41670.51230.036*
C270.9380 (2)0.5846 (2)0.10233 (19)0.0325 (6)
H27A1.00390.60590.12340.039*
H27B0.91420.63960.06420.039*
C280.9580 (2)0.4917 (2)0.04422 (19)0.0334 (7)
H28A0.89100.47010.02520.040*
H28B0.98180.43730.08310.040*
C290.5388 (3)1.2622 (2)0.2482 (2)0.0360 (7)
H29A0.58031.30090.28730.043*
H29B0.48901.21870.29110.043*
C300.4748 (3)1.3355 (3)0.1966 (2)0.0438 (8)
H30A0.44561.29800.14810.053*
H30B0.41411.36040.24280.053*
C310.5357 (3)1.4252 (3)0.1491 (3)0.0523 (10)
H31A0.48921.46280.11280.063*
H31B0.55281.47010.19860.063*
C320.6375 (3)1.3993 (3)0.0833 (3)0.0464 (9)
H32A0.62141.35360.03400.056*
H32B0.66871.46130.05160.056*
C330.8343 (3)1.2110 (3)0.0082 (2)0.0441 (8)
H33A0.85821.27910.00490.053*
H33B0.82561.20940.07520.053*
C340.9180 (3)1.1350 (3)0.0083 (3)0.0505 (9)
H34A0.98261.14680.03930.061*
H34B0.89171.06710.00190.061*
C350.9479 (3)1.1381 (3)0.1067 (3)0.0493 (9)
H35A0.98931.19980.11120.059*
H35B0.99461.08030.11370.059*
C360.8544 (3)1.1356 (2)0.1892 (2)0.0381 (7)
H36A0.80591.08050.17960.046*
H36B0.88121.12160.24860.046*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0245 (5)0.0209 (5)0.0315 (5)0.0038 (4)0.0078 (4)0.0000 (4)
Na20.0342 (6)0.0253 (6)0.0315 (5)0.0054 (5)0.0116 (5)0.0015 (4)
Na30.0250 (5)0.0203 (5)0.0323 (5)0.0024 (4)0.0081 (4)0.0024 (4)
Na40.0334 (6)0.0257 (6)0.0320 (5)0.0075 (5)0.0098 (4)0.0011 (4)
O10.0354 (11)0.0219 (10)0.0363 (10)0.0014 (8)0.0159 (8)0.0003 (8)
O20.0202 (9)0.0247 (10)0.0303 (9)0.0037 (8)0.0026 (7)0.0038 (8)
O30.0187 (9)0.0336 (11)0.0296 (9)0.0039 (8)0.0014 (7)0.0008 (8)
O40.0317 (11)0.0390 (12)0.0318 (10)0.0176 (9)0.0037 (8)0.0013 (9)
O50.0329 (11)0.0235 (10)0.0345 (10)0.0013 (9)0.0048 (8)0.0058 (8)
O60.0518 (14)0.0222 (10)0.0564 (13)0.0128 (10)0.0316 (11)0.0083 (10)
O70.0240 (10)0.0526 (14)0.0340 (10)0.0102 (10)0.0081 (8)0.0141 (10)
O80.0497 (13)0.0280 (11)0.0287 (10)0.0018 (10)0.0038 (9)0.0010 (8)
O90.0296 (11)0.0228 (10)0.0417 (10)0.0050 (8)0.0150 (8)0.0060 (8)
O100.0300 (10)0.0227 (10)0.0345 (9)0.0038 (8)0.0112 (8)0.0026 (8)
O110.0218 (9)0.0224 (9)0.0386 (10)0.0004 (8)0.0009 (8)0.0045 (8)
O120.0248 (10)0.0322 (11)0.0289 (9)0.0065 (8)0.0045 (7)0.0012 (8)
O130.0230 (9)0.0281 (10)0.0263 (8)0.0018 (8)0.0041 (7)0.0053 (8)
O140.0334 (11)0.0215 (10)0.0380 (10)0.0012 (8)0.0147 (8)0.0023 (8)
O150.0534 (14)0.0293 (11)0.0299 (10)0.0104 (11)0.0072 (10)0.0044 (9)
O160.0207 (9)0.0256 (10)0.0310 (9)0.0005 (8)0.0042 (7)0.0002 (8)
O170.0225 (10)0.0478 (13)0.0339 (10)0.0026 (9)0.0059 (8)0.0140 (9)
O180.0349 (11)0.0212 (9)0.0395 (10)0.0028 (9)0.0137 (9)0.0022 (8)
B10.0213 (15)0.0286 (16)0.0292 (14)0.0083 (13)0.0069 (11)0.0080 (13)
B20.0358 (18)0.0209 (15)0.0367 (16)0.0039 (14)0.0148 (14)0.0013 (13)
B30.0201 (14)0.0204 (14)0.0304 (14)0.0004 (12)0.0053 (11)0.0007 (12)
B40.0240 (16)0.0260 (16)0.0298 (15)0.0005 (13)0.0069 (12)0.0060 (13)
C10.0444 (18)0.0198 (14)0.0463 (16)0.0015 (13)0.0185 (14)0.0021 (12)
C20.0475 (19)0.0313 (16)0.0421 (16)0.0133 (15)0.0141 (14)0.0110 (13)
C30.0295 (16)0.0342 (16)0.0446 (16)0.0070 (13)0.0062 (13)0.0089 (13)
C40.0285 (15)0.0283 (15)0.0352 (14)0.0042 (12)0.0011 (12)0.0039 (12)
C50.0347 (17)0.055 (2)0.0302 (14)0.0133 (16)0.0049 (12)0.0066 (14)
C60.0289 (17)0.091 (3)0.0413 (17)0.0063 (19)0.0025 (14)0.0048 (19)
C70.0323 (18)0.097 (3)0.0447 (18)0.017 (2)0.0019 (14)0.017 (2)
C80.0362 (18)0.069 (3)0.0477 (18)0.0244 (18)0.0113 (15)0.0227 (18)
C90.0313 (16)0.0356 (16)0.0408 (15)0.0086 (14)0.0051 (12)0.0055 (14)
C100.0334 (17)0.0360 (17)0.0385 (15)0.0051 (14)0.0046 (12)0.0014 (13)
C110.0411 (18)0.0242 (15)0.0476 (16)0.0075 (13)0.0203 (14)0.0138 (13)
C120.050 (2)0.0218 (14)0.062 (2)0.0092 (14)0.0242 (17)0.0023 (14)
C130.0310 (16)0.0443 (19)0.0500 (17)0.0132 (14)0.0089 (14)0.0103 (15)
C140.0329 (16)0.0304 (15)0.0366 (14)0.0054 (13)0.0032 (12)0.0059 (12)
C150.0445 (18)0.0245 (14)0.0367 (14)0.0067 (13)0.0138 (13)0.0015 (12)
C160.0249 (15)0.0433 (19)0.0569 (19)0.0093 (14)0.0102 (13)0.0162 (16)
C170.0283 (15)0.0390 (17)0.0448 (16)0.0054 (14)0.0038 (13)0.0114 (14)
C180.0357 (17)0.0405 (17)0.0289 (13)0.0070 (14)0.0045 (12)0.0012 (12)
C190.0304 (15)0.0330 (16)0.0321 (14)0.0036 (13)0.0046 (12)0.0048 (12)
C200.0298 (16)0.049 (2)0.0407 (16)0.0098 (15)0.0017 (13)0.0039 (14)
C210.0252 (15)0.063 (2)0.0382 (16)0.0009 (15)0.0012 (12)0.0105 (15)
C220.0345 (17)0.0485 (19)0.0398 (15)0.0021 (15)0.0067 (13)0.0168 (14)
C230.0433 (18)0.0204 (14)0.0524 (17)0.0044 (13)0.0216 (14)0.0041 (13)
C240.052 (2)0.0223 (14)0.0471 (16)0.0139 (14)0.0213 (15)0.0089 (13)
C250.0331 (16)0.0343 (17)0.0438 (16)0.0112 (14)0.0077 (13)0.0030 (14)
C260.0225 (14)0.0303 (15)0.0346 (14)0.0025 (12)0.0005 (11)0.0027 (12)
C270.0348 (16)0.0275 (15)0.0314 (13)0.0001 (13)0.0046 (12)0.0008 (12)
C280.0351 (16)0.0342 (16)0.0295 (13)0.0017 (13)0.0014 (12)0.0043 (12)
C290.0412 (18)0.0348 (16)0.0321 (14)0.0052 (14)0.0061 (12)0.0038 (12)
C300.0441 (19)0.049 (2)0.0405 (16)0.0190 (16)0.0131 (14)0.0093 (15)
C310.067 (3)0.0334 (18)0.065 (2)0.0100 (18)0.036 (2)0.0056 (16)
C320.050 (2)0.0368 (18)0.0583 (19)0.0162 (16)0.0278 (17)0.0187 (16)
C330.0353 (17)0.057 (2)0.0374 (15)0.0186 (16)0.0004 (13)0.0016 (15)
C340.0337 (18)0.056 (2)0.057 (2)0.0167 (17)0.0066 (15)0.0158 (18)
C350.0379 (19)0.0374 (18)0.074 (2)0.0068 (16)0.0141 (17)0.0122 (17)
C360.0482 (19)0.0214 (14)0.0494 (17)0.0004 (14)0.0213 (15)0.0036 (13)
Geometric parameters (Å, º) top
Na1—O42.338 (2)C7—H7A0.9900
Na1—O1i2.349 (2)C7—H7B0.9900
Na1—O3i2.425 (2)C8—H8A0.9900
Na1—O52.456 (2)C8—H8B0.9900
Na1—O32.477 (2)C9—C101.536 (4)
Na1—O22.609 (2)C9—H9A0.9900
Na2—O82.289 (2)C9—H9B0.9900
Na2—O102.295 (2)C10—C10v1.501 (6)
Na2—O72.342 (2)C10—H10A0.9900
Na2—O22.355 (2)C10—H10B0.9900
Na2—O92.406 (2)C11—C121.497 (5)
Na3—O122.305 (2)C11—H11A0.9900
Na3—O14ii2.332 (2)C11—H11B0.9900
Na3—O132.459 (2)C12—C131.532 (5)
Na3—O13ii2.488 (2)C12—H12A0.9900
Na3—O112.499 (2)C12—H12B0.9900
Na3—O162.602 (2)C13—C141.517 (5)
Na4—O162.334 (2)C13—H13A0.9900
Na4—O18iii2.334 (2)C13—H13B0.9900
Na4—O152.350 (3)C14—H14A0.9900
Na4—O6iii2.361 (2)C14—H14B0.9900
Na4—O172.408 (2)C15—C161.528 (5)
O1—C11.441 (4)C15—H15A0.9900
O1—B11.457 (4)C15—H15B0.9900
O1—Na1i2.349 (2)C16—C171.540 (5)
O2—C41.414 (3)C16—H16A0.9900
O2—B11.491 (4)C16—H16B0.9900
O3—C51.431 (3)C17—C181.510 (5)
O3—B11.490 (4)C17—H17A0.9900
O3—Na1i2.425 (2)C17—H17B0.9900
O4—C331.414 (4)C18—H18A0.9900
O4—B21.463 (4)C18—H18B0.9900
O5—C291.435 (4)C19—C201.527 (4)
O5—B21.503 (4)C19—H19A0.9900
O6—C321.435 (4)C19—H19B0.9900
O6—B21.456 (4)C20—C211.523 (5)
O6—Na4iv2.361 (2)C20—H20A0.9900
O7—C81.428 (4)C20—H20B0.9900
O7—B11.467 (4)C21—C221.518 (5)
O8—C91.420 (4)C21—H21A0.9900
O8—H8O0.85 (3)C21—H21B0.9900
O9—C111.422 (4)C22—H22A0.9900
O9—B31.469 (4)C22—H22B0.9900
O10—C151.412 (4)C23—C241.517 (5)
O10—B31.471 (3)C23—H23A0.9900
O11—C141.426 (4)C23—H23B0.9900
O11—B31.484 (4)C24—C251.534 (5)
O12—C181.429 (3)C24—H24A0.9900
O12—B31.468 (4)C24—H24B0.9900
O13—C191.445 (4)C25—C261.525 (4)
O13—B41.480 (4)C25—H25A0.9900
O13—Na3ii2.488 (2)C25—H25B0.9900
O14—C231.421 (4)C26—H26A0.9900
O14—B41.458 (4)C26—H26B0.9900
O14—Na3ii2.332 (2)C27—C281.501 (4)
O15—C271.427 (3)C27—H27A0.9900
O15—H15O0.79 (3)C27—H27B0.9900
O16—C261.424 (3)C28—C28vi1.530 (6)
O16—B41.487 (4)C28—H28A0.9900
O17—C221.416 (4)C28—H28B0.9900
O17—B41.473 (4)C29—C301.538 (4)
O18—C361.415 (4)C29—H29A0.9900
O18—B21.468 (4)C29—H29B0.9900
O18—Na4iv2.334 (2)C30—C311.520 (6)
C1—C21.514 (5)C30—H30A0.9900
C1—H1A0.9900C30—H30B0.9900
C1—H1B0.9900C31—C321.514 (6)
C2—C31.512 (5)C31—H31A0.9900
C2—H2A0.9900C31—H31B0.9900
C2—H2B0.9900C32—H32A0.9900
C3—C41.521 (4)C32—H32B0.9900
C3—H3A0.9900C33—C341.521 (6)
C3—H3B0.9900C33—H33A0.9900
C4—H4A0.9900C33—H33B0.9900
C4—H4B0.9900C34—C351.531 (5)
C5—C61.540 (5)C34—H34A0.9900
C5—H5A0.9900C34—H34B0.9900
C5—H5B0.9900C35—C361.532 (5)
C6—C71.545 (6)C35—H35A0.9900
C6—H6A0.9900C35—H35B0.9900
C6—H6B0.9900C36—H36A0.9900
C7—C81.510 (6)C36—H36B0.9900
O4—Na1—O1i107.75 (9)C6—C7—H7B108.7
O4—Na1—O3i116.36 (8)H7A—C7—H7B107.6
O1i—Na1—O3i58.09 (7)O7—C8—C7111.9 (3)
O4—Na1—O557.29 (7)O7—C8—H8A109.2
O1i—Na1—O5110.89 (8)C7—C8—H8A109.2
O3i—Na1—O5166.60 (8)O7—C8—H8B109.2
O4—Na1—O3158.27 (8)C7—C8—H8B109.2
O1i—Na1—O393.59 (8)H8A—C8—H8B107.9
O3i—Na1—O378.17 (7)O8—C9—C10109.3 (3)
O5—Na1—O3111.69 (8)O8—C9—H9A109.8
O4—Na1—O2102.76 (8)C10—C9—H9A109.8
O1i—Na1—O2147.53 (8)O8—C9—H9B109.8
O3i—Na1—O298.37 (7)C10—C9—H9B109.8
O5—Na1—O294.71 (7)H9A—C9—H9B108.3
O3—Na1—O257.41 (7)C10v—C10—C9113.8 (3)
O8—Na2—O10154.25 (8)C10v—C10—H10A108.8
O8—Na2—O7101.71 (9)C9—C10—H10A108.8
O10—Na2—O798.80 (9)C10v—C10—H10B108.8
O8—Na2—O287.88 (8)C9—C10—H10B108.8
O10—Na2—O2116.13 (8)H10A—C10—H10B107.7
O7—Na2—O259.44 (7)O9—C11—C12111.2 (3)
O8—Na2—O998.21 (8)O9—C11—H11A109.4
O10—Na2—O957.77 (7)C12—C11—H11A109.4
O7—Na2—O9153.15 (9)O9—C11—H11B109.4
O2—Na2—O9139.66 (9)C12—C11—H11B109.4
O12—Na3—O14ii110.10 (8)H11A—C11—H11B108.0
O12—Na3—O13152.03 (8)C11—C12—C13113.9 (3)
O14ii—Na3—O1396.54 (8)C11—C12—H12A108.8
O12—Na3—O13ii121.83 (8)C13—C12—H12A108.8
O14ii—Na3—O13ii56.93 (7)C11—C12—H12B108.8
O13—Na3—O13ii79.63 (7)C13—C12—H12B108.8
O12—Na3—O1156.99 (7)H12A—C12—H12B107.7
O14ii—Na3—O11111.89 (8)C14—C13—C12115.5 (3)
O13—Na3—O11105.73 (7)C14—C13—H13A108.4
O13ii—Na3—O11168.52 (8)C12—C13—H13A108.4
O12—Na3—O1699.05 (8)C14—C13—H13B108.4
O14ii—Na3—O16148.18 (8)C12—C13—H13B108.4
O13—Na3—O1657.77 (7)H13A—C13—H13B107.5
O13ii—Na3—O1697.07 (7)O11—C14—C13112.9 (2)
O11—Na3—O1694.36 (7)O11—C14—H14A109.0
O16—Na4—O18iii117.99 (8)C13—C14—H14A109.0
O16—Na4—O1589.13 (8)O11—C14—H14B109.0
O18iii—Na4—O15152.14 (9)C13—C14—H14B109.0
O16—Na4—O6iii145.27 (10)H14A—C14—H14B107.8
O18iii—Na4—O6iii57.83 (7)O10—C15—C16112.5 (3)
O15—Na4—O6iii96.56 (9)O10—C15—H15A109.1
O16—Na4—O1758.34 (7)C16—C15—H15A109.1
O18iii—Na4—O17102.42 (8)O10—C15—H15B109.1
O15—Na4—O1797.23 (9)C16—C15—H15B109.1
O6iii—Na4—O17152.74 (9)H15A—C15—H15B107.8
C1—O1—B1116.8 (2)C15—C16—C17114.4 (3)
C1—O1—Na1i141.83 (18)C15—C16—H16A108.7
B1—O1—Na1i101.13 (16)C17—C16—H16A108.7
C4—O2—B1121.2 (2)C15—C16—H16B108.7
C4—O2—Na2119.02 (16)C17—C16—H16B108.7
B1—O2—Na297.71 (15)H16A—C16—H16B107.6
C4—O2—Na193.51 (15)C18—C17—C16114.8 (3)
B1—O2—Na192.32 (15)C18—C17—H17A108.6
Na2—O2—Na1132.65 (8)C16—C17—H17A108.6
C5—O3—B1118.3 (2)C18—C17—H17B108.6
C5—O3—Na1i136.86 (17)C16—C17—H17B108.6
B1—O3—Na1i96.85 (15)H17A—C17—H17B107.5
C5—O3—Na197.60 (18)O12—C18—C17112.3 (2)
B1—O3—Na197.70 (15)O12—C18—H18A109.1
Na1i—O3—Na1101.83 (7)C17—C18—H18A109.1
C33—O4—B2116.2 (2)O12—C18—H18B109.1
C33—O4—Na1140.26 (19)C17—C18—H18B109.1
B2—O4—Na1103.56 (17)H18A—C18—H18B107.9
C29—O5—B2118.1 (2)O13—C19—C20111.5 (3)
C29—O5—Na1131.70 (18)O13—C19—Na356.94 (12)
B2—O5—Na197.16 (15)C20—C19—Na3167.4 (2)
C32—O6—B2118.9 (2)O13—C19—H19A109.3
C32—O6—Na4iv141.16 (19)C20—C19—H19A109.3
B2—O6—Na4iv99.77 (17)Na3—C19—H19A73.0
C8—O7—B1115.7 (2)O13—C19—H19B109.3
C8—O7—Na2145.03 (18)C20—C19—H19B109.3
B1—O7—Na298.98 (16)Na3—C19—H19B81.0
C9—O8—Na2124.06 (19)H19A—C19—H19B108.0
C9—O8—H8O106 (3)C21—C20—C19114.6 (3)
Na2—O8—H8O121 (3)C21—C20—H20A108.6
C11—O9—B3116.0 (2)C19—C20—H20A108.6
C11—O9—Na2144.81 (17)C21—C20—H20B108.6
B3—O9—Na297.97 (15)C19—C20—H20B108.6
C15—O10—B3120.3 (2)H20A—C20—H20B107.6
C15—O10—Na2125.48 (18)C22—C21—C20113.0 (3)
B3—O10—Na2102.82 (16)C22—C21—H21A109.0
C14—O11—B3116.5 (2)C20—C21—H21A109.0
C14—O11—Na3136.66 (18)C22—C21—H21B109.0
B3—O11—Na395.77 (15)C20—C21—H21B109.0
C18—O12—B3116.6 (2)H21A—C21—H21B107.8
C18—O12—Na3138.01 (17)O17—C22—C21112.7 (3)
B3—O12—Na3104.73 (15)O17—C22—H22A109.0
C19—O13—B4119.3 (2)C21—C22—H22A109.0
C19—O13—Na393.56 (15)O17—C22—H22B109.0
B4—O13—Na397.70 (15)C21—C22—H22B109.0
C19—O13—Na3ii140.11 (16)H22A—C22—H22B107.8
B4—O13—Na3ii95.80 (15)O14—C23—C24111.7 (3)
Na3—O13—Na3ii100.37 (7)O14—C23—H23A109.3
C23—O14—B4117.1 (2)C24—C23—H23A109.3
C23—O14—Na3ii139.50 (17)O14—C23—H23B109.3
B4—O14—Na3ii103.27 (16)C24—C23—H23B109.3
C27—O15—Na4114.53 (18)H23A—C23—H23B107.9
C27—O15—H15O114 (3)C23—C24—C25114.7 (3)
Na4—O15—H15O118 (3)C23—C24—H24A108.6
C26—O16—B4121.2 (2)C25—C24—H24A108.6
C26—O16—Na4117.42 (16)C23—C24—H24B108.6
B4—O16—Na4100.63 (15)C25—C24—H24B108.6
C26—O16—Na390.28 (15)H24A—C24—H24B107.6
B4—O16—Na391.71 (15)C26—C25—C24114.1 (3)
Na4—O16—Na3135.70 (9)C26—C25—H25A108.7
C22—O17—B4116.7 (2)C24—C25—H25A108.7
C22—O17—Na4145.44 (18)C26—C25—H25B108.7
B4—O17—Na497.88 (16)C24—C25—H25B108.7
C36—O18—B2118.9 (2)H25A—C25—H25B107.6
C36—O18—Na4iv133.57 (19)O16—C26—C25114.3 (2)
B2—O18—Na4iv100.55 (16)O16—C26—Na361.09 (13)
O1—B1—O7113.6 (2)C25—C26—Na3166.1 (2)
O1—B1—O3103.8 (2)O16—C26—H26A108.7
O7—B1—O3112.6 (2)C25—C26—H26A108.7
O1—B1—O2113.1 (2)Na3—C26—H26A85.0
O7—B1—O2103.9 (2)O16—C26—H26B108.7
O3—B1—O2110.2 (2)C25—C26—H26B108.7
O6—B2—O4115.1 (3)Na3—C26—H26B63.6
O6—B2—O18101.8 (2)H26A—C26—H26B107.6
O4—B2—O18113.2 (3)O15—C27—C28108.2 (2)
O6—B2—O5112.9 (3)O15—C27—H27A110.1
O4—B2—O5101.8 (2)C28—C27—H27A110.1
O18—B2—O5112.6 (2)O15—C27—H27B110.1
O9—B3—O12114.3 (2)C28—C27—H27B110.1
O9—B3—O10101.3 (2)H27A—C27—H27B108.4
O12—B3—O10113.8 (2)C27—C28—C28vi112.1 (3)
O9—B3—O11113.2 (2)C27—C28—Na482.61 (16)
O12—B3—O11102.2 (2)C28vi—C28—Na4158.9 (3)
O10—B3—O11112.4 (2)C27—C28—H28A109.2
O14—B4—O17114.8 (2)C28vi—C28—H28A109.2
O14—B4—O13103.1 (2)Na4—C28—H28A78.0
O17—B4—O13111.7 (2)C27—C28—H28B109.2
O14—B4—O16113.6 (2)C28vi—C28—H28B109.2
O17—B4—O16102.7 (2)Na4—C28—H28B50.2
O13—B4—O16111.2 (2)H28A—C28—H28B107.9
O1—C1—C2112.0 (3)O5—C29—C30113.0 (2)
O1—C1—H1A109.2O5—C29—H29A109.0
C2—C1—H1A109.2C30—C29—H29A109.0
O1—C1—H1B109.2O5—C29—H29B109.0
C2—C1—H1B109.2C30—C29—H29B109.0
H1A—C1—H1B107.9H29A—C29—H29B107.8
C3—C2—C1112.8 (2)C31—C30—C29115.7 (3)
C3—C2—H2A109.0C31—C30—H30A108.3
C1—C2—H2A109.0C29—C30—H30A108.3
C3—C2—H2B109.0C31—C30—H30B108.3
C1—C2—H2B109.0C29—C30—H30B108.3
H2A—C2—H2B107.8H30A—C30—H30B107.4
C2—C3—C4115.4 (3)C32—C31—C30114.7 (3)
C2—C3—H3A108.4C32—C31—H31A108.6
C4—C3—H3A108.4C30—C31—H31A108.6
C2—C3—H3B108.4C32—C31—H31B108.6
C4—C3—H3B108.4C30—C31—H31B108.6
H3A—C3—H3B107.5H31A—C31—H31B107.6
O2—C4—C3114.4 (2)O6—C32—C31112.0 (3)
O2—C4—Na158.85 (13)O6—C32—H32A109.2
C3—C4—Na1164.2 (2)C31—C32—H32A109.2
O2—C4—H4A108.7O6—C32—H32B109.2
C3—C4—H4A108.7C31—C32—H32B109.2
Na1—C4—H4A87.1H32A—C32—H32B107.9
O2—C4—H4B108.7O4—C33—C34111.6 (3)
C3—C4—H4B108.7O4—C33—H33A109.3
Na1—C4—H4B64.2C34—C33—H33A109.3
H4A—C4—H4B107.6O4—C33—H33B109.3
O3—C5—C6111.4 (3)C34—C33—H33B109.3
O3—C5—Na154.38 (14)H33A—C33—H33B108.0
C6—C5—Na1164.3 (2)C33—C34—C35114.5 (3)
O3—C5—H5A109.3C33—C34—H34A108.6
C6—C5—H5A109.3C35—C34—H34A108.6
Na1—C5—H5A73.4C33—C34—H34B108.6
O3—C5—H5B109.3C35—C34—H34B108.6
C6—C5—H5B109.4H34A—C34—H34B107.6
Na1—C5—H5B83.7C34—C35—C36115.3 (3)
H5A—C5—H5B108.0C34—C35—H35A108.5
C5—C6—C7115.0 (3)C36—C35—H35A108.5
C5—C6—H6A108.5C34—C35—H35B108.5
C7—C6—H6A108.5C36—C35—H35B108.5
C5—C6—H6B108.5H35A—C35—H35B107.5
C7—C6—H6B108.5O18—C36—C35112.3 (3)
H6A—C6—H6B107.5O18—C36—H36A109.1
C8—C7—C6114.4 (3)C35—C36—H36A109.1
C8—C7—H7A108.7O18—C36—H36B109.1
C6—C7—H7A108.7C35—C36—H36B109.1
C8—C7—H7B108.7H36A—C36—H36B107.9
O8—Na2—O2—C4123.57 (19)C33—O4—B2—O1855.4 (4)
O10—Na2—O2—C446.8 (2)Na1—O4—B2—O18125.5 (2)
O7—Na2—O2—C4131.5 (2)C33—O4—B2—O5176.5 (2)
O9—Na2—O2—C423.4 (2)Na1—O4—B2—O54.4 (2)
O8—Na2—O2—B1104.13 (17)C36—O18—B2—O6153.3 (3)
O10—Na2—O2—B185.54 (17)Na4iv—O18—B2—O61.3 (2)
O7—Na2—O2—B10.81 (15)C36—O18—B2—O429.2 (4)
O9—Na2—O2—B1155.67 (17)Na4iv—O18—B2—O4125.5 (2)
O8—Na2—O2—Na13.74 (13)C36—O18—B2—O585.5 (3)
O10—Na2—O2—Na1174.08 (10)Na4iv—O18—B2—O5119.8 (2)
O7—Na2—O2—Na1101.20 (13)C29—O5—B2—O626.1 (3)
O9—Na2—O2—Na1103.95 (14)Na1—O5—B2—O6119.8 (2)
O4—Na1—O2—C458.93 (16)C29—O5—B2—O4150.0 (2)
O1i—Na1—O2—C4100.8 (2)Na1—O5—B2—O44.1 (2)
O3i—Na1—O2—C460.64 (16)C29—O5—B2—O1888.5 (3)
O5—Na1—O2—C4116.43 (15)Na1—O5—B2—O18125.6 (2)
O3—Na1—O2—C4130.77 (16)C11—O9—B3—O1263.2 (3)
O4—Na1—O2—B1179.61 (15)Na2—O9—B3—O12126.1 (2)
O1i—Na1—O2—B120.6 (2)C11—O9—B3—O10174.0 (2)
O3i—Na1—O2—B160.82 (15)Na2—O9—B3—O103.3 (2)
O5—Na1—O2—B1122.10 (15)C11—O9—B3—O1153.3 (3)
O3—Na1—O2—B19.30 (14)Na2—O9—B3—O11117.36 (19)
O4—Na1—O2—Na276.90 (13)C18—O12—B3—O954.3 (3)
O1i—Na1—O2—Na2123.34 (15)Na3—O12—B3—O9117.8 (2)
O3i—Na1—O2—Na2163.53 (11)C18—O12—B3—O1061.4 (3)
O5—Na1—O2—Na219.40 (13)Na3—O12—B3—O10126.5 (2)
O3—Na1—O2—Na293.40 (12)C18—O12—B3—O11177.1 (2)
O4—Na1—O3—C584.3 (3)Na3—O12—B3—O115.0 (2)
O1i—Na1—O3—C584.92 (16)C15—O10—B3—O9141.9 (2)
O3i—Na1—O3—C5141.26 (18)Na2—O10—B3—O93.5 (2)
O5—Na1—O3—C529.25 (17)C15—O10—B3—O1218.7 (3)
O2—Na1—O3—C5110.65 (16)Na2—O10—B3—O12126.64 (19)
O4—Na1—O3—B135.7 (3)C15—O10—B3—O1197.0 (3)
O1i—Na1—O3—B1155.04 (15)Na2—O10—B3—O11117.7 (2)
O3i—Na1—O3—B198.70 (16)C14—O11—B3—O931.1 (3)
O5—Na1—O3—B190.79 (16)Na3—O11—B3—O9119.03 (19)
O2—Na1—O3—B19.39 (14)C14—O11—B3—O12154.6 (2)
O4—Na1—O3—Na1i134.4 (2)Na3—O11—B3—O124.44 (19)
O1i—Na1—O3—Na1i56.34 (8)C14—O11—B3—O1083.0 (3)
O3i—Na1—O3—Na1i0.0Na3—O11—B3—O10126.9 (2)
O5—Na1—O3—Na1i170.51 (8)C23—O14—B4—O1753.2 (3)
O2—Na1—O3—Na1i108.08 (9)Na3ii—O14—B4—O17130.7 (2)
O1i—Na1—O4—C3378.0 (3)C23—O14—B4—O13174.9 (2)
O3i—Na1—O4—C3315.4 (4)Na3ii—O14—B4—O139.0 (2)
O5—Na1—O4—C33178.2 (4)C23—O14—B4—O1664.7 (3)
O3—Na1—O4—C33113.3 (3)Na3ii—O14—B4—O16111.5 (2)
O2—Na1—O4—C3390.8 (3)C22—O17—B4—O1461.9 (4)
O1i—Na1—O4—B2100.68 (17)Na4—O17—B4—O14118.2 (2)
O3i—Na1—O4—B2163.25 (16)C22—O17—B4—O1355.0 (3)
O5—Na1—O4—B23.16 (16)Na4—O17—B4—O13124.87 (19)
O3—Na1—O4—B268.0 (3)C22—O17—B4—O16174.2 (2)
O2—Na1—O4—B290.57 (17)Na4—O17—B4—O165.7 (2)
O4—Na1—O5—C29141.5 (3)C19—O13—B4—O14152.0 (2)
O1i—Na1—O5—C2943.3 (2)Na3—O13—B4—O14109.53 (18)
O3i—Na1—O5—C2976.2 (4)Na3ii—O13—B4—O148.21 (19)
O3—Na1—O5—C2959.7 (2)C19—O13—B4—O1728.2 (3)
O2—Na1—O5—C29116.4 (2)Na3—O13—B4—O17126.7 (2)
O4—Na1—O5—B23.02 (15)Na3ii—O13—B4—O17132.0 (2)
O1i—Na1—O5—B295.19 (16)C19—O13—B4—O1685.9 (3)
O3i—Na1—O5—B262.3 (4)Na3—O13—B4—O1612.6 (2)
O3—Na1—O5—B2161.87 (15)Na3ii—O13—B4—O16113.89 (19)
O2—Na1—O5—B2105.17 (16)C26—O16—B4—O1412.6 (3)
O8—Na2—O7—C893.6 (4)Na4—O16—B4—O14118.8 (2)
O10—Na2—O7—C870.7 (4)Na3—O16—B4—O14104.0 (2)
O2—Na2—O7—C8174.0 (4)C26—O16—B4—O17137.3 (2)
O9—Na2—O7—C843.5 (5)Na4—O16—B4—O175.9 (2)
O8—Na2—O7—B179.60 (18)Na3—O16—B4—O17131.35 (19)
O10—Na2—O7—B1116.06 (17)C26—O16—B4—O13103.1 (3)
O2—Na2—O7—B10.83 (16)Na4—O16—B4—O13125.47 (18)
O9—Na2—O7—B1143.3 (2)Na3—O16—B4—O1311.8 (2)
O10—Na2—O8—C95.8 (4)B1—O1—C1—C291.2 (3)
O7—Na2—O8—C9136.4 (2)Na1i—O1—C1—C295.7 (3)
O2—Na2—O8—C9165.5 (2)O1—C1—C2—C363.5 (3)
O9—Na2—O8—C925.5 (2)C1—C2—C3—C459.4 (4)
O8—Na2—O9—C1122.2 (3)B1—O2—C4—C369.0 (3)
O10—Na2—O9—C11167.8 (3)Na2—O2—C4—C352.1 (3)
O7—Na2—O9—C11159.8 (3)Na1—O2—C4—C3163.8 (2)
O2—Na2—O9—C1174.3 (3)B1—O2—C4—Na194.8 (2)
O8—Na2—O9—B3172.42 (16)Na2—O2—C4—Na1144.12 (15)
O10—Na2—O9—B32.42 (15)C2—C3—C4—O279.8 (3)
O7—Na2—O9—B334.8 (3)C2—C3—C4—Na118.7 (9)
O2—Na2—O9—B391.14 (19)O4—Na1—C4—O2123.28 (15)
O8—Na2—O10—C15117.2 (3)O1i—Na1—C4—O2119.81 (17)
O7—Na2—O10—C1525.4 (2)O3i—Na1—C4—O2119.97 (15)
O2—Na2—O10—C1585.5 (2)O5—Na1—C4—O268.31 (15)
O9—Na2—O10—C15140.5 (2)O3—Na1—C4—O240.88 (14)
O8—Na2—O10—B325.8 (3)O4—Na1—C4—C3167.9 (7)
O7—Na2—O10—B3168.30 (16)O1i—Na1—C4—C351.0 (8)
O2—Na2—O10—B3131.51 (16)O3i—Na1—C4—C351.2 (7)
O9—Na2—O10—B32.46 (15)O5—Na1—C4—C3137.1 (7)
O12—Na3—O11—C14142.8 (3)O3—Na1—C4—C327.9 (7)
O14ii—Na3—O11—C1442.4 (3)O2—Na1—C4—C368.8 (7)
O13—Na3—O11—C1461.5 (3)B1—O3—C5—C684.7 (3)
O13ii—Na3—O11—C1455.0 (5)Na1i—O3—C5—C655.9 (4)
O16—Na3—O11—C14119.2 (3)Na1—O3—C5—C6172.3 (2)
O12—Na3—O11—B33.29 (14)B1—O3—C5—Na1103.0 (2)
O14ii—Na3—O11—B397.11 (16)Na1i—O3—C5—Na1116.4 (2)
O13—Na3—O11—B3158.97 (15)O4—Na1—C5—O3141.83 (17)
O13ii—Na3—O11—B384.5 (4)O1i—Na1—C5—O396.17 (15)
O16—Na3—O11—B3101.26 (15)O3i—Na1—C5—O338.49 (17)
O14ii—Na3—O12—C1869.2 (3)O5—Na1—C5—O3152.96 (16)
O13—Na3—O12—C18129.5 (3)O2—Na1—C5—O356.83 (14)
O13ii—Na3—O12—C186.4 (3)O4—Na1—C5—C6169.3 (8)
O11—Na3—O12—C18172.8 (3)O1i—Na1—C5—C668.8 (9)
O16—Na3—O12—C1897.8 (3)O3i—Na1—C5—C611.1 (9)
O14ii—Na3—O12—B3100.21 (17)O5—Na1—C5—C6179.6 (9)
O13—Na3—O12—B361.1 (3)O3—Na1—C5—C627.4 (8)
O13ii—Na3—O12—B3163.04 (15)O2—Na1—C5—C684.2 (9)
O11—Na3—O12—B33.42 (15)O3—C5—C6—C774.2 (4)
O16—Na3—O12—B392.75 (16)Na1—C5—C6—C797.9 (9)
O12—Na3—O13—C1974.5 (2)C5—C6—C7—C850.9 (5)
O14ii—Na3—O13—C1987.86 (15)B1—O7—C8—C794.5 (3)
O13ii—Na3—O13—C19142.45 (17)Na2—O7—C8—C778.0 (5)
O11—Na3—O13—C1927.12 (16)C6—C7—C8—O764.7 (4)
O16—Na3—O13—C19112.28 (15)Na2—O8—C9—C1042.8 (3)
O12—Na3—O13—B445.6 (2)O8—C9—C10—C10v64.6 (4)
O14ii—Na3—O13—B4151.98 (15)B3—O9—C11—C1294.9 (3)
O13ii—Na3—O13—B497.38 (16)Na2—O9—C11—C1269.0 (4)
O11—Na3—O13—B493.05 (15)O9—C11—C12—C1367.0 (3)
O16—Na3—O13—B47.88 (14)C11—C12—C13—C1450.4 (4)
O12—Na3—O13—Na3ii143.00 (17)B3—O11—C14—C1385.6 (3)
O14ii—Na3—O13—Na3ii54.60 (8)Na3—O11—C14—C1348.1 (4)
O13ii—Na3—O13—Na3ii0.0C12—C13—C14—O1172.9 (4)
O11—Na3—O13—Na3ii169.57 (8)B3—O10—C15—C1679.0 (3)
O16—Na3—O13—Na3ii105.26 (9)Na2—O10—C15—C1658.1 (3)
O16—Na4—O15—C27122.8 (2)O10—C15—C16—C1776.9 (3)
O18iii—Na4—O15—C2769.9 (3)C15—C16—C17—C1854.4 (4)
O6iii—Na4—O15—C2791.5 (2)B3—O12—C18—C1790.4 (3)
O17—Na4—O15—C2764.9 (2)Na3—O12—C18—C17101.0 (3)
O18iii—Na4—O16—C2650.2 (2)C16—C17—C18—O1263.1 (3)
O15—Na4—O16—C26123.12 (18)B4—O13—C19—C2084.8 (3)
O6iii—Na4—O16—C2622.8 (3)Na3—O13—C19—C20174.3 (2)
O17—Na4—O16—C26137.83 (19)Na3ii—O13—C19—C2063.4 (3)
O18iii—Na4—O16—B483.50 (18)B4—O13—C19—Na3100.9 (2)
O15—Na4—O16—B4103.17 (17)Na3ii—O13—C19—Na3110.8 (2)
O6iii—Na4—O16—B4156.55 (18)O12—Na3—C19—O13140.26 (15)
O17—Na4—O16—B44.12 (16)O14ii—Na3—C19—O1395.09 (15)
O18iii—Na4—O16—Na3172.85 (11)O13ii—Na3—C19—O1337.99 (17)
O15—Na4—O16—Na30.48 (14)O11—Na3—C19—O13153.48 (15)
O6iii—Na4—O16—Na399.80 (18)O16—Na3—C19—O1355.31 (14)
O17—Na4—O16—Na399.53 (14)O12—Na3—C19—C20165.4 (9)
O12—Na3—O16—C2667.91 (15)O14ii—Na3—C19—C2070.0 (10)
O14ii—Na3—O16—C2688.5 (2)O13—Na3—C19—C2025.1 (9)
O13—Na3—O16—C26128.99 (16)O13ii—Na3—C19—C2012.9 (10)
O13ii—Na3—O16—C2656.00 (15)O11—Na3—C19—C20178.6 (10)
O11—Na3—O16—C26125.15 (15)O16—Na3—C19—C2080.4 (10)
O12—Na3—O16—B4170.88 (15)O13—C19—C20—C2175.6 (3)
O14ii—Na3—O16—B432.7 (2)Na3—C19—C20—C2198.1 (10)
O13—Na3—O16—B47.78 (14)C19—C20—C21—C2253.7 (4)
O13ii—Na3—O16—B465.21 (15)B4—O17—C22—C2194.1 (3)
O11—Na3—O16—B4113.64 (15)Na4—O17—C22—C2185.6 (4)
O12—Na3—O16—Na463.72 (14)C20—C21—C22—O1767.1 (4)
O14ii—Na3—O16—Na4139.83 (15)B4—O14—C23—C2491.3 (3)
O13—Na3—O16—Na499.38 (13)Na3ii—O14—C23—C2483.0 (3)
O13ii—Na3—O16—Na4172.37 (12)O14—C23—C24—C2564.4 (3)
O11—Na3—O16—Na46.48 (14)C23—C24—C25—C2656.6 (4)
O16—Na4—O17—C22175.6 (4)B4—O16—C26—C2573.2 (3)
O18iii—Na4—O17—C2269.0 (4)Na4—O16—C26—C2550.7 (3)
O15—Na4—O17—C2291.1 (4)Na3—O16—C26—C25165.4 (2)
O6iii—Na4—O17—C2228.7 (5)B4—O16—C26—Na392.2 (2)
O16—Na4—O17—B44.12 (16)Na4—O16—C26—Na3143.97 (14)
O18iii—Na4—O17—B4111.26 (17)C24—C25—C26—O1676.5 (3)
O15—Na4—O17—B488.60 (18)C24—C25—C26—Na39.0 (10)
O6iii—Na4—O17—B4151.6 (2)O12—Na3—C26—O16113.68 (14)
C1—O1—B1—O749.5 (3)O14ii—Na3—C26—O16128.48 (16)
Na1i—O1—B1—O7126.2 (2)O13—Na3—C26—O1642.29 (13)
C1—O1—B1—O3172.0 (2)O13ii—Na3—C26—O16123.57 (15)
Na1i—O1—B1—O33.7 (2)O11—Na3—C26—O1660.18 (15)
C1—O1—B1—O268.6 (3)O12—Na3—C26—C25172.2 (8)
Na1i—O1—B1—O2115.8 (2)O14ii—Na3—C26—C2554.4 (9)
C8—O7—B1—O159.9 (4)O13—Na3—C26—C2531.8 (8)
Na2—O7—B1—O1124.4 (2)O13ii—Na3—C26—C2549.5 (8)
C8—O7—B1—O357.6 (4)O11—Na3—C26—C25134.2 (8)
Na2—O7—B1—O3118.1 (2)O16—Na3—C26—C2574.1 (8)
C8—O7—B1—O2176.8 (3)Na4—O15—C27—C2823.6 (3)
Na2—O7—B1—O21.2 (2)O15—C27—C28—C28vi179.2 (3)
C5—O3—B1—O1150.5 (2)O15—C27—C28—Na416.5 (2)
Na1i—O3—B1—O13.5 (2)O16—Na4—C28—C2742.6 (2)
Na1—O3—B1—O1106.49 (18)O18iii—Na4—C28—C27167.84 (17)
C5—O3—B1—O727.3 (3)O15—Na4—C28—C2712.32 (17)
Na1i—O3—B1—O7126.7 (2)O6iii—Na4—C28—C27115.49 (19)
Na1—O3—B1—O7130.3 (2)O17—Na4—C28—C2790.26 (18)
C5—O3—B1—O288.1 (3)O16—Na4—C28—C28vi93.3 (8)
Na1i—O3—B1—O2117.83 (19)O18iii—Na4—C28—C28vi56.3 (8)
Na1—O3—B1—O214.8 (2)O15—Na4—C28—C28vi148.2 (8)
C4—O2—B1—O16.2 (3)O6iii—Na4—C28—C28vi108.7 (8)
Na2—O2—B1—O1124.72 (19)O17—Na4—C28—C28vi45.6 (8)
Na1—O2—B1—O1101.7 (2)B2—O5—C29—C3081.9 (3)
C4—O2—B1—O7129.7 (2)Na1—O5—C29—C3049.9 (4)
Na2—O2—B1—O71.1 (2)O5—C29—C30—C3174.8 (4)
Na1—O2—B1—O7134.76 (19)C29—C30—C31—C3252.4 (4)
C4—O2—B1—O3109.5 (3)B2—O6—C32—C3191.8 (4)
Na2—O2—B1—O3119.65 (19)Na4iv—O6—C32—C3181.8 (4)
Na1—O2—B1—O314.0 (2)C30—C31—C32—O663.6 (4)
C32—O6—B2—O459.9 (4)B2—O4—C33—C3493.4 (3)
Na4iv—O6—B2—O4124.1 (2)Na1—O4—C33—C3488.0 (4)
C32—O6—B2—O18177.2 (3)O4—C33—C34—C3565.4 (4)
Na4iv—O6—B2—O181.3 (2)C33—C34—C35—C3650.3 (4)
C32—O6—B2—O556.3 (4)B2—O18—C36—C3584.2 (3)
Na4iv—O6—B2—O5119.7 (2)Na4iv—O18—C36—C3560.2 (3)
C33—O4—B2—O661.1 (4)C34—C35—C36—O1872.2 (4)
Na1—O4—B2—O6117.9 (2)
Symmetry codes: (i) x+1, y+2, z; (ii) x+2, y+1, z+1; (iii) x, y1, z; (iv) x, y+1, z; (v) x+1, y+2, z+1; (vi) x+2, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8O···O50.85 (4)2.06 (2)2.897 (3)170 (4)
O15—H15O···O110.80 (4)2.14 (4)2.927 (3)169 (5)

Experimental details

Crystal data
Chemical formula[Na4(C8H16BO4)4(C4H10O2)]
Mr930.15
Crystal system, space groupTriclinic, P1
Temperature (K)163
a, b, c (Å)12.813 (4), 13.349 (4), 14.381 (5)
α, β, γ (°)89.282 (5), 79.966 (4), 89.837 (4)
V3)2421.9 (14)
Z2
Radiation typeMo Kα
µ (mm1)0.13
Crystal size (mm)0.75 × 0.42 × 0.15
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(Blessing, 1995)
Tmin, Tmax0.685, 0.981
No. of measured, independent and
observed [I > 2σ(I)] reflections
7185, 7185, 5247
Rint0.000
(sin θ/λ)max1)0.630
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.060, 0.154, 0.99
No. of reflections7185
No. of parameters565
No. of restraints2
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.36, 0.30

Computer programs: SMART (Bruker, 2001), SMART, SAINT (Bruker, 2001) and SADABS (Sheldrick, 1996), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1999) and Mercury (Bruno et al., 2002), SHELXL97.

Selected geometric parameters (Å, º) top
Na1—O42.338 (2)Na2—O72.342 (2)
Na1—O1i2.349 (2)Na2—O22.355 (2)
Na1—O3i2.425 (2)Na2—O92.406 (2)
Na1—O52.456 (2)Na3—O132.459 (2)
Na1—O32.477 (2)Na3—O162.602 (2)
Na1—O22.609 (2)Na4—O152.350 (3)
Na2—O82.289 (2)O1—B11.457 (4)
Na2—O102.295 (2)O2—B11.491 (4)
O1i—Na1—O3i58.09 (7)Na2—O2—Na1132.65 (8)
O3i—Na1—O5166.60 (8)Na1i—O3—Na1101.83 (7)
O7—Na2—O259.44 (7)Na3—O13—Na3ii100.37 (7)
O2—Na2—O9139.66 (9)Na4—O16—Na3135.70 (9)
O8—C9—C10—C10iii64.6 (4)O15—C27—C28—C28iv179.2 (3)
Symmetry codes: (i) x+1, y+2, z; (ii) x+2, y+1, z+1; (iii) x+1, y+2, z+1; (iv) x+2, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8O···O50.85 (4)2.06 (2)2.897 (3)170 (4)
O15—H15O···O110.80 (4)2.14 (4)2.927 (3)169 (5)
 

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