Two new inorganic-organic coordination polymers, namely poly[[
6-2-(4-{1-[4-(carboxymethoxy)phenyl]-1-methylethyl}phenoxy)acetato][
4-2-(4-{1-[4-(carboxymethoxy)phenyl]-1-methylethyl}phenoxy)acetato]disodium(I)], [Na
2(C
19H
19O
6)
2]
n, (I), and poly[hexa-
-aqua-diaquabis{
3-2,2'-[sulfonylbis(1,4-phenyleneoxy)]diacetato}tetrasodium(I)], [Na
4(C
16H
14O
8)
2(H
2O)
8]
n, (II), have been prepared. In (I), the asymmetric unit contains two Na
I cations and two 2-(4-{1-[4-(carboxymethoxy)phenyl]-1-methylethyl}phenoxy)acetate (H
L1-) ligands. Each Na
I cation is octahedrally coordinated by two ether O atoms and four carboxylate O atoms of three different H
L1- ligands. The NaO
6 polyhedra share edges to form an inorganic ribbon along the
a axis. These inorganic ribbons are further connected by the H
L1- ligands to generate two-dimensional layers parallel to the (001) plane. The structure of (II) consists of ribbons of four crystallographically independent Na atoms (three six- and one five-coordinate), which are bridged by carboxylate O atoms of 4,4'-[sulfonylbis(1,4-phenyleneoxy)]diacetate (
L22-) ligands and water molecules. These ribbons are interlinked by
L22- ligands through two different coordination modes to afford a three-dimensional network.
Supporting information
CCDC references: 962995; 962996
For both compounds, data collection: APEX2 (Bruker, 2001); cell refinement: APEX2 (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
(I) Poly[[µ
6-2-(4-{1-[4-(carboxymethoxy)phenyl]-1-methylethyl}phenoxy)acetato][µ
4-2-(4-{1-[4-(carboxymethoxy)phenyl]-1-methylethyl}phenoxy)acetato]disodium(I)]
top
Crystal data top
[Na2(C19H19O6)2] | F(000) = 1536 |
Mr = 732.66 | Dx = 1.462 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2081 reflections |
a = 5.7235 (11) Å | θ = 2.4–22.0° |
b = 27.444 (6) Å | µ = 0.13 mm−1 |
c = 21.287 (4) Å | T = 295 K |
β = 95.60 (3)° | Block, colourless |
V = 3327.7 (11) Å3 | 0.21 × 0.19 × 0.18 mm |
Z = 4 | |
Data collection top
Bruker APEXII CCD area-detector diffractometer | 5890 independent reflections |
Radiation source: fine-focus sealed tube | 3555 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
φ and ω scans | θmax = 25.1°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −6→6 |
Tmin = 0.973, Tmax = 0.977 | k = −32→29 |
17630 measured reflections | l = −25→18 |
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)] = 0.049 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.135 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0553P)2 + 0.6345P] where P = (Fo2 + 2Fc2)/3 |
5890 reflections | (Δ/σ)max < 0.001 |
473 parameters | Δρmax = 0.18 e Å−3 |
0 restraints | Δρmin = −0.31 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 | |
Na1 | 0.7534 (2) | 0.16149 (5) | 0.27052 (6) | 0.0685 (4) | |
Na2 | 0.2584 (2) | 0.10088 (5) | 0.25645 (6) | 0.0655 (4) | |
O1 | 0.4974 (4) | 0.54170 (7) | 0.33626 (9) | 0.0475 (6) | |
O2 | 0.0560 (4) | 0.61016 (8) | 0.39823 (10) | 0.0641 (7) | |
H1 | −0.0530 | 0.6270 | 0.3826 | 0.096* | |
O3 | 0.1029 (4) | 0.59378 (7) | 0.29769 (10) | 0.0529 (6) | |
O4 | 0.4950 (4) | 0.22201 (7) | 0.35655 (9) | 0.0509 (6) | |
O5 | 0.0675 (4) | 0.15193 (8) | 0.42416 (10) | 0.0595 (7) | |
O6 | 0.1114 (4) | 0.16682 (7) | 0.32322 (10) | 0.0546 (6) | |
O7 | 0.7728 (3) | 0.54103 (6) | 0.14552 (9) | 0.0411 (5) | |
O8 | 0.2455 (4) | 0.59224 (7) | 0.07347 (9) | 0.0496 (6) | |
H8 | 0.1539 | 0.6124 | 0.0854 | 0.074* | |
O9 | 0.4259 (4) | 0.60281 (7) | 0.17024 (9) | 0.0459 (5) | |
O10 | 0.7926 (3) | 0.21912 (6) | 0.16937 (8) | 0.0399 (5) | |
O11 | 0.2603 (4) | 0.16739 (7) | 0.10204 (9) | 0.0510 (6) | |
O12 | 0.4411 (4) | 0.15966 (7) | 0.19884 (9) | 0.0464 (5) | |
C1 | 0.6534 (5) | 0.50526 (9) | 0.35541 (13) | 0.0368 (7) | |
C2 | 0.7171 (5) | 0.49190 (10) | 0.41716 (13) | 0.0440 (8) | |
H2 | 0.6559 | 0.5085 | 0.4499 | 0.053* | |
C3 | 0.8721 (5) | 0.45372 (10) | 0.43026 (13) | 0.0403 (7) | |
H3 | 0.9124 | 0.4451 | 0.4722 | 0.048* | |
C4 | 0.9696 (4) | 0.42792 (9) | 0.38342 (12) | 0.0297 (6) | |
C5 | 0.9055 (5) | 0.44327 (9) | 0.32203 (12) | 0.0350 (7) | |
H5 | 0.9690 | 0.4273 | 0.2891 | 0.042* | |
C6 | 0.7520 (5) | 0.48106 (10) | 0.30793 (13) | 0.0372 (7) | |
H6 | 0.7146 | 0.4903 | 0.2661 | 0.045* | |
C7 | 0.3564 (5) | 0.55866 (11) | 0.38245 (13) | 0.0459 (8) | |
H7A | 0.4527 | 0.5775 | 0.4136 | 0.055* | |
H7B | 0.2946 | 0.5310 | 0.4038 | 0.055* | |
C8 | 0.1558 (5) | 0.58966 (10) | 0.35480 (15) | 0.0408 (7) | |
C9 | 1.1272 (5) | 0.38315 (9) | 0.39732 (12) | 0.0313 (6) | |
C10 | 1.3185 (5) | 0.38095 (10) | 0.35137 (14) | 0.0417 (7) | |
H10A | 1.2461 | 0.3790 | 0.3088 | 0.063* | |
H10B | 1.4149 | 0.3527 | 0.3605 | 0.063* | |
H10C | 1.4139 | 0.4097 | 0.3561 | 0.063* | |
C11 | 1.2567 (5) | 0.38593 (10) | 0.46382 (13) | 0.0409 (7) | |
H11A | 1.3562 | 0.4142 | 0.4669 | 0.061* | |
H11B | 1.3505 | 0.3572 | 0.4718 | 0.061* | |
H11C | 1.1444 | 0.3882 | 0.4944 | 0.061* | |
C12 | 0.9671 (5) | 0.33809 (9) | 0.38969 (12) | 0.0309 (6) | |
C13 | 0.8718 (6) | 0.31581 (10) | 0.43944 (13) | 0.0456 (8) | |
H13 | 0.9134 | 0.3271 | 0.4802 | 0.055* | |
C14 | 0.7161 (6) | 0.27710 (11) | 0.43076 (13) | 0.0506 (9) | |
H14 | 0.6554 | 0.2629 | 0.4654 | 0.061* | |
C15 | 0.6515 (5) | 0.25971 (9) | 0.37110 (13) | 0.0372 (7) | |
C16 | 0.7439 (5) | 0.28086 (10) | 0.32079 (13) | 0.0393 (7) | |
H16 | 0.7027 | 0.2692 | 0.2802 | 0.047* | |
C17 | 0.8970 (5) | 0.31915 (10) | 0.33005 (13) | 0.0365 (7) | |
H17 | 0.9566 | 0.3331 | 0.2951 | 0.044* | |
C18 | 0.3624 (6) | 0.20592 (11) | 0.40515 (14) | 0.0501 (9) | |
H18A | 0.2968 | 0.2339 | 0.4250 | 0.060* | |
H18B | 0.4648 | 0.1890 | 0.4370 | 0.060* | |
C19 | 0.1645 (5) | 0.17203 (10) | 0.38017 (15) | 0.0424 (8) | |
C20 | 0.9297 (5) | 0.50422 (9) | 0.13568 (12) | 0.0327 (7) | |
C21 | 1.0952 (5) | 0.49365 (9) | 0.18540 (12) | 0.0348 (7) | |
H21 | 1.1058 | 0.5129 | 0.2215 | 0.042* | |
C22 | 1.2450 (5) | 0.45447 (9) | 0.18162 (12) | 0.0325 (7) | |
H22 | 1.3521 | 0.4474 | 0.2161 | 0.039* | |
C23 | 1.2417 (4) | 0.42514 (9) | 0.12797 (12) | 0.0287 (6) | |
C24 | 1.0817 (5) | 0.43878 (9) | 0.07749 (12) | 0.0339 (7) | |
H24 | 1.0780 | 0.4213 | 0.0400 | 0.041* | |
C25 | 0.9280 (5) | 0.47735 (9) | 0.08101 (12) | 0.0354 (7) | |
H25 | 0.8232 | 0.4852 | 0.0463 | 0.042* | |
C26 | 0.5820 (5) | 0.54711 (10) | 0.09799 (12) | 0.0380 (7) | |
H26A | 0.5031 | 0.5161 | 0.0900 | 0.046* | |
H26B | 0.6414 | 0.5577 | 0.0591 | 0.046* | |
C27 | 0.4095 (5) | 0.58401 (10) | 0.11796 (14) | 0.0359 (7) | |
C28 | 1.3977 (5) | 0.37964 (9) | 0.12499 (12) | 0.0298 (6) | |
C29 | 1.6137 (5) | 0.38251 (10) | 0.17442 (13) | 0.0367 (7) | |
H29A | 1.7021 | 0.4114 | 0.1673 | 0.055* | |
H29B | 1.7107 | 0.3543 | 0.1707 | 0.055* | |
H29C | 1.5624 | 0.3836 | 0.2160 | 0.055* | |
C30 | 1.4936 (5) | 0.37693 (10) | 0.05984 (12) | 0.0377 (7) | |
H30A | 1.3652 | 0.3737 | 0.0276 | 0.057* | |
H30B | 1.5957 | 0.3493 | 0.0586 | 0.057* | |
H30C | 1.5796 | 0.4061 | 0.0528 | 0.057* | |
C31 | 1.2490 (4) | 0.33411 (9) | 0.13538 (12) | 0.0283 (6) | |
C32 | 1.2610 (5) | 0.30880 (9) | 0.19219 (12) | 0.0334 (7) | |
H32 | 1.3712 | 0.3184 | 0.2248 | 0.040* | |
C33 | 1.1154 (5) | 0.26990 (9) | 0.20197 (12) | 0.0340 (7) | |
H33 | 1.1307 | 0.2534 | 0.2403 | 0.041* | |
C34 | 0.9477 (5) | 0.25559 (9) | 0.15480 (12) | 0.0336 (7) | |
C35 | 0.9410 (5) | 0.27808 (10) | 0.09702 (12) | 0.0386 (7) | |
H35 | 0.8355 | 0.2673 | 0.0639 | 0.046* | |
C36 | 1.0893 (5) | 0.31652 (10) | 0.08754 (12) | 0.0360 (7) | |
H36 | 1.0818 | 0.3310 | 0.0479 | 0.043* | |
C37 | 0.6031 (5) | 0.21057 (10) | 0.12218 (13) | 0.0392 (7) | |
H37A | 0.6636 | 0.1969 | 0.0850 | 0.047* | |
H37B | 0.5276 | 0.2413 | 0.1102 | 0.047* | |
C38 | 0.4249 (5) | 0.17622 (9) | 0.14528 (14) | 0.0365 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.0651 (10) | 0.0752 (9) | 0.0597 (9) | −0.0263 (7) | −0.0210 (7) | 0.0189 (7) |
Na2 | 0.0626 (9) | 0.0715 (9) | 0.0575 (8) | −0.0239 (7) | −0.0190 (7) | 0.0196 (7) |
O1 | 0.0537 (14) | 0.0472 (12) | 0.0416 (12) | 0.0233 (11) | 0.0044 (10) | 0.0053 (10) |
O2 | 0.0652 (17) | 0.0737 (16) | 0.0533 (14) | 0.0381 (13) | 0.0054 (12) | 0.0038 (13) |
O3 | 0.0530 (15) | 0.0565 (14) | 0.0459 (14) | 0.0124 (11) | −0.0115 (11) | −0.0019 (11) |
O4 | 0.0667 (16) | 0.0463 (12) | 0.0390 (12) | −0.0254 (11) | 0.0015 (11) | −0.0014 (10) |
O5 | 0.0627 (16) | 0.0711 (15) | 0.0433 (13) | −0.0330 (13) | −0.0020 (11) | 0.0023 (12) |
O6 | 0.0564 (15) | 0.0608 (14) | 0.0433 (13) | −0.0113 (11) | −0.0123 (11) | −0.0007 (11) |
O7 | 0.0409 (13) | 0.0374 (11) | 0.0429 (12) | 0.0101 (9) | −0.0056 (9) | −0.0045 (9) |
O8 | 0.0515 (14) | 0.0563 (13) | 0.0396 (12) | 0.0189 (11) | −0.0026 (10) | −0.0033 (10) |
O9 | 0.0479 (14) | 0.0453 (12) | 0.0422 (12) | 0.0087 (10) | −0.0070 (10) | −0.0110 (10) |
O10 | 0.0436 (13) | 0.0368 (11) | 0.0380 (11) | −0.0114 (9) | −0.0035 (9) | 0.0049 (9) |
O11 | 0.0532 (14) | 0.0607 (14) | 0.0369 (12) | −0.0206 (11) | −0.0062 (10) | 0.0004 (10) |
O12 | 0.0501 (14) | 0.0471 (12) | 0.0407 (13) | −0.0068 (10) | −0.0024 (10) | 0.0100 (10) |
C1 | 0.0365 (18) | 0.0308 (15) | 0.0422 (17) | 0.0043 (13) | 0.0000 (13) | −0.0012 (13) |
C2 | 0.052 (2) | 0.0467 (18) | 0.0333 (16) | 0.0169 (15) | 0.0051 (14) | −0.0053 (14) |
C3 | 0.0448 (19) | 0.0440 (17) | 0.0312 (16) | 0.0093 (15) | 0.0001 (13) | −0.0011 (14) |
C4 | 0.0262 (16) | 0.0304 (15) | 0.0324 (16) | −0.0024 (12) | 0.0014 (12) | −0.0014 (12) |
C5 | 0.0394 (18) | 0.0359 (16) | 0.0306 (15) | 0.0045 (13) | 0.0084 (13) | 0.0001 (13) |
C6 | 0.0393 (18) | 0.0415 (17) | 0.0306 (15) | 0.0026 (14) | 0.0026 (13) | 0.0046 (13) |
C7 | 0.048 (2) | 0.0460 (18) | 0.0430 (18) | 0.0155 (16) | 0.0012 (15) | −0.0018 (15) |
C8 | 0.0400 (19) | 0.0348 (17) | 0.047 (2) | 0.0049 (14) | −0.0002 (15) | −0.0021 (15) |
C9 | 0.0267 (15) | 0.0332 (15) | 0.0338 (16) | −0.0002 (12) | 0.0019 (12) | 0.0009 (12) |
C10 | 0.0310 (16) | 0.0429 (17) | 0.0518 (19) | 0.0025 (14) | 0.0076 (14) | −0.0001 (14) |
C11 | 0.0353 (17) | 0.0422 (17) | 0.0436 (18) | 0.0013 (14) | −0.0033 (14) | 0.0012 (14) |
C12 | 0.0321 (16) | 0.0298 (15) | 0.0303 (15) | 0.0044 (12) | 0.0012 (12) | 0.0023 (12) |
C13 | 0.058 (2) | 0.0491 (18) | 0.0286 (16) | −0.0156 (16) | −0.0035 (14) | −0.0007 (14) |
C14 | 0.065 (2) | 0.0516 (19) | 0.0337 (18) | −0.0274 (17) | −0.0008 (15) | 0.0097 (15) |
C15 | 0.0406 (18) | 0.0319 (16) | 0.0376 (17) | −0.0079 (13) | −0.0039 (13) | 0.0016 (13) |
C16 | 0.0446 (19) | 0.0403 (17) | 0.0329 (17) | −0.0024 (14) | 0.0026 (13) | −0.0052 (14) |
C17 | 0.0377 (18) | 0.0411 (16) | 0.0311 (16) | −0.0034 (14) | 0.0061 (13) | −0.0005 (13) |
C18 | 0.056 (2) | 0.0510 (19) | 0.0416 (19) | −0.0219 (16) | −0.0028 (16) | 0.0027 (15) |
C19 | 0.046 (2) | 0.0360 (17) | 0.0427 (19) | −0.0045 (15) | −0.0062 (15) | 0.0005 (15) |
C20 | 0.0351 (17) | 0.0281 (15) | 0.0353 (16) | 0.0002 (13) | 0.0048 (13) | 0.0024 (12) |
C21 | 0.0373 (18) | 0.0351 (16) | 0.0322 (16) | −0.0026 (13) | 0.0035 (13) | −0.0034 (13) |
C22 | 0.0316 (17) | 0.0350 (16) | 0.0300 (15) | −0.0005 (13) | −0.0021 (12) | 0.0023 (13) |
C23 | 0.0253 (15) | 0.0291 (14) | 0.0318 (15) | −0.0058 (12) | 0.0034 (11) | 0.0030 (12) |
C24 | 0.0363 (17) | 0.0360 (16) | 0.0290 (15) | −0.0022 (13) | 0.0011 (12) | −0.0044 (13) |
C25 | 0.0362 (18) | 0.0354 (16) | 0.0331 (16) | 0.0061 (13) | −0.0042 (13) | 0.0030 (13) |
C26 | 0.0422 (18) | 0.0342 (16) | 0.0368 (17) | 0.0059 (14) | −0.0007 (13) | 0.0029 (13) |
C27 | 0.0375 (18) | 0.0309 (15) | 0.0388 (18) | −0.0014 (13) | 0.0015 (14) | 0.0067 (14) |
C28 | 0.0271 (15) | 0.0335 (14) | 0.0283 (15) | 0.0004 (12) | 0.0003 (11) | −0.0016 (12) |
C29 | 0.0273 (15) | 0.0421 (16) | 0.0395 (17) | −0.0005 (13) | −0.0020 (12) | 0.0005 (14) |
C30 | 0.0334 (17) | 0.0442 (17) | 0.0363 (17) | 0.0006 (13) | 0.0067 (13) | −0.0004 (13) |
C31 | 0.0272 (15) | 0.0289 (14) | 0.0288 (15) | 0.0027 (12) | 0.0031 (11) | −0.0003 (12) |
C32 | 0.0330 (17) | 0.0368 (16) | 0.0293 (15) | −0.0003 (13) | −0.0021 (12) | −0.0043 (13) |
C33 | 0.0374 (18) | 0.0355 (16) | 0.0288 (15) | 0.0015 (13) | 0.0022 (12) | 0.0026 (12) |
C34 | 0.0370 (17) | 0.0281 (15) | 0.0353 (16) | 0.0000 (13) | 0.0005 (13) | −0.0006 (13) |
C35 | 0.0404 (19) | 0.0419 (17) | 0.0310 (16) | −0.0086 (14) | −0.0088 (13) | −0.0022 (14) |
C36 | 0.0430 (18) | 0.0367 (16) | 0.0272 (15) | −0.0031 (14) | −0.0018 (13) | 0.0057 (13) |
C37 | 0.0443 (19) | 0.0368 (16) | 0.0357 (17) | −0.0078 (14) | −0.0004 (14) | −0.0004 (13) |
C38 | 0.0429 (19) | 0.0272 (15) | 0.0393 (18) | 0.0011 (13) | 0.0038 (14) | −0.0027 (13) |
Geometric parameters (Å, º) top
Na1—O12 | 2.235 (2) | C11—H11A | 0.9600 |
Na1—O6i | 2.242 (2) | C11—H11B | 0.9600 |
Na1—O9ii | 2.343 (2) | C11—H11C | 0.9600 |
Na1—O3ii | 2.544 (3) | C12—C13 | 1.380 (4) |
Na1—O10 | 2.698 (2) | C12—C17 | 1.394 (3) |
Na1—O4 | 2.971 (3) | C13—C14 | 1.388 (4) |
Na1—Na2 | 3.2740 (19) | C13—H13 | 0.9300 |
Na1—Na2i | 3.373 (2) | C14—C15 | 1.373 (4) |
Na2—O9ii | 2.270 (2) | C14—H14 | 0.9300 |
Na2—O3iii | 2.276 (2) | C15—C16 | 1.369 (4) |
Na2—O12 | 2.335 (2) | C16—C17 | 1.370 (4) |
Na2—O6 | 2.497 (3) | C16—H16 | 0.9300 |
Na2—O7ii | 2.675 (2) | C17—H17 | 0.9300 |
Na2—O1ii | 3.004 (3) | C18—C19 | 1.521 (4) |
O1—C1 | 1.376 (3) | C18—H18A | 0.9700 |
O1—C7 | 1.411 (3) | C18—H18B | 0.9700 |
O2—C8 | 1.265 (3) | C20—C25 | 1.377 (4) |
O2—H1 | 0.8200 | C20—C21 | 1.380 (3) |
O3—C8 | 1.229 (3) | C21—C22 | 1.383 (4) |
O4—C15 | 1.383 (3) | C21—H21 | 0.9300 |
O4—C18 | 1.412 (3) | C22—C23 | 1.396 (3) |
O5—C19 | 1.261 (3) | C22—H22 | 0.9300 |
O6—C19 | 1.229 (3) | C23—C24 | 1.394 (3) |
O7—C20 | 1.382 (3) | C23—C28 | 1.540 (3) |
O7—C26 | 1.424 (3) | C24—C25 | 1.383 (4) |
O8—C27 | 1.287 (3) | C24—H24 | 0.9300 |
O8—H8 | 0.8200 | C25—H25 | 0.9300 |
O9—C27 | 1.222 (3) | C26—C27 | 1.504 (4) |
O10—C34 | 1.393 (3) | C26—H26A | 0.9700 |
O10—C37 | 1.424 (3) | C26—H26B | 0.9700 |
O11—C38 | 1.275 (3) | C28—C31 | 1.540 (3) |
O12—C38 | 1.222 (3) | C28—C30 | 1.542 (4) |
C1—C6 | 1.376 (4) | C28—C29 | 1.545 (3) |
C1—C2 | 1.379 (4) | C29—H29A | 0.9600 |
C2—C3 | 1.384 (4) | C29—H29B | 0.9600 |
C2—H2 | 0.9300 | C29—H29C | 0.9600 |
C3—C4 | 1.384 (4) | C30—H30A | 0.9600 |
C3—H3 | 0.9300 | C30—H30B | 0.9600 |
C4—C5 | 1.388 (3) | C30—H30C | 0.9600 |
C4—C9 | 1.536 (3) | C31—C36 | 1.387 (3) |
C5—C6 | 1.373 (4) | C31—C32 | 1.390 (3) |
C5—H5 | 0.9300 | C32—C33 | 1.383 (4) |
C6—H6 | 0.9300 | C32—H32 | 0.9300 |
C7—C8 | 1.502 (4) | C33—C34 | 1.377 (3) |
C7—H7A | 0.9700 | C33—H33 | 0.9300 |
C7—H7B | 0.9700 | C34—C35 | 1.373 (4) |
C9—C11 | 1.534 (3) | C35—C36 | 1.381 (4) |
C9—C12 | 1.538 (4) | C35—H35 | 0.9300 |
C9—C10 | 1.539 (4) | C36—H36 | 0.9300 |
C10—H10A | 0.9600 | C37—C38 | 1.506 (4) |
C10—H10B | 0.9600 | C37—H37A | 0.9700 |
C10—H10C | 0.9600 | C37—H37B | 0.9700 |
| | | |
O12—Na1—O6i | 166.89 (11) | H10B—C10—H10C | 109.5 |
O12—Na1—O9ii | 89.35 (8) | C9—C11—H11A | 109.5 |
O6i—Na1—O9ii | 101.69 (9) | C9—C11—H11B | 109.5 |
O12—Na1—O3ii | 82.84 (8) | H11A—C11—H11B | 109.5 |
O6i—Na1—O3ii | 90.17 (9) | C9—C11—H11C | 109.5 |
O9ii—Na1—O3ii | 89.31 (8) | H11A—C11—H11C | 109.5 |
O12—Na1—O10 | 65.89 (7) | H11B—C11—H11C | 109.5 |
O6i—Na1—O10 | 102.59 (8) | C13—C12—C17 | 115.7 (3) |
O9ii—Na1—O10 | 155.10 (8) | C13—C12—C9 | 123.4 (2) |
O3ii—Na1—O10 | 85.19 (8) | C17—C12—C9 | 120.8 (2) |
O12—Na1—O4 | 91.16 (8) | C12—C13—C14 | 122.3 (3) |
O6i—Na1—O4 | 98.08 (8) | C12—C13—H13 | 118.9 |
O9ii—Na1—O4 | 77.40 (8) | C14—C13—H13 | 118.9 |
O3ii—Na1—O4 | 165.51 (8) | C15—C14—C13 | 120.1 (3) |
O10—Na1—O4 | 104.43 (7) | C15—C14—H14 | 120.0 |
O12—Na1—Na2i | 124.30 (8) | C13—C14—H14 | 120.0 |
O6i—Na1—Na2i | 47.76 (7) | C16—C15—C14 | 119.1 (3) |
O9ii—Na1—Na2i | 97.65 (7) | C16—C15—O4 | 115.7 (2) |
O3ii—Na1—Na2i | 42.41 (6) | C14—C15—O4 | 125.2 (3) |
O10—Na1—Na2i | 94.57 (7) | C15—C16—C17 | 120.2 (3) |
O4—Na1—Na2i | 144.36 (6) | C15—C16—H16 | 119.9 |
O9ii—Na2—O3iii | 166.73 (10) | C17—C16—H16 | 119.9 |
O9ii—Na2—O12 | 88.72 (8) | C16—C17—C12 | 122.7 (3) |
O3iii—Na2—O12 | 102.99 (9) | C16—C17—H17 | 118.7 |
O9ii—Na2—O6 | 83.20 (8) | C12—C17—H17 | 118.7 |
O3iii—Na2—O6 | 90.60 (9) | O4—C18—C19 | 111.7 (2) |
O12—Na2—O6 | 89.50 (9) | O4—C18—H18A | 109.3 |
O9ii—Na2—O7ii | 65.62 (7) | C19—C18—H18A | 109.3 |
O3iii—Na2—O7ii | 102.47 (8) | O4—C18—H18B | 109.3 |
O12—Na2—O7ii | 154.33 (8) | C19—C18—H18B | 109.3 |
O6—Na2—O7ii | 87.09 (8) | H18A—C18—H18B | 107.9 |
O9ii—Na2—O1ii | 94.25 (8) | O6—C19—O5 | 126.7 (3) |
O3iii—Na2—O1ii | 94.53 (8) | O6—C19—C18 | 121.3 (3) |
O12—Na2—O1ii | 76.56 (8) | O5—C19—C18 | 112.0 (3) |
O6—Na2—O1ii | 165.90 (8) | C25—C20—C21 | 118.9 (3) |
O7ii—Na2—O1ii | 104.54 (7) | C25—C20—O7 | 124.7 (2) |
O9ii—Na2—Na1iv | 123.98 (8) | C21—C20—O7 | 116.4 (2) |
O3iii—Na2—Na1iv | 48.93 (7) | C20—C21—C22 | 120.1 (2) |
O12—Na2—Na1iv | 97.91 (7) | C20—C21—H21 | 119.9 |
O6—Na2—Na1iv | 41.67 (6) | C22—C21—H21 | 119.9 |
O7ii—Na2—Na1iv | 96.35 (7) | C21—C22—C23 | 122.5 (2) |
O1ii—Na2—Na1iv | 141.49 (6) | C21—C22—H22 | 118.8 |
C1—O1—C7 | 115.6 (2) | C23—C22—H22 | 118.8 |
C1—O1—Na2v | 104.93 (17) | C24—C23—C22 | 115.6 (2) |
C7—O1—Na2v | 127.88 (17) | C24—C23—C28 | 121.8 (2) |
C8—O2—H1 | 109.5 | C22—C23—C28 | 122.7 (2) |
C8—O3—Na2vi | 129.2 (2) | C25—C24—C23 | 122.5 (2) |
C8—O3—Na1v | 124.74 (19) | C25—C24—H24 | 118.7 |
Na2vi—O3—Na1v | 88.66 (8) | C23—C24—H24 | 118.7 |
C15—O4—C18 | 116.9 (2) | C20—C25—C24 | 120.2 (2) |
C15—O4—Na1 | 101.87 (17) | C20—C25—H25 | 119.9 |
C18—O4—Na1 | 127.75 (18) | C24—C25—H25 | 119.9 |
C19—O6—Na1iv | 128.8 (2) | O7—C26—C27 | 110.9 (2) |
C19—O6—Na2 | 125.5 (2) | O7—C26—H26A | 109.5 |
Na1iv—O6—Na2 | 90.58 (9) | C27—C26—H26A | 109.5 |
C20—O7—C26 | 116.3 (2) | O7—C26—H26B | 109.5 |
C20—O7—Na2v | 131.39 (16) | C27—C26—H26B | 109.5 |
C26—O7—Na2v | 112.17 (15) | H26A—C26—H26B | 108.0 |
C27—O8—H8 | 109.5 | O9—C27—O8 | 125.6 (3) |
C27—O9—Na2v | 126.98 (19) | O9—C27—C26 | 123.2 (3) |
C27—O9—Na1v | 141.41 (19) | O8—C27—C26 | 111.2 (2) |
Na2v—O9—Na1v | 90.41 (8) | C23—C28—C31 | 108.7 (2) |
C34—O10—C37 | 114.8 (2) | C23—C28—C30 | 109.6 (2) |
C34—O10—Na1 | 134.69 (15) | C31—C28—C30 | 109.9 (2) |
C37—O10—Na1 | 110.47 (15) | C23—C28—C29 | 111.1 (2) |
C38—O12—Na1 | 127.7 (2) | C31—C28—C29 | 111.1 (2) |
C38—O12—Na2 | 138.54 (19) | C30—C28—C29 | 106.5 (2) |
Na1—O12—Na2 | 91.51 (8) | C28—C29—H29A | 109.5 |
C6—C1—O1 | 115.7 (2) | C28—C29—H29B | 109.5 |
C6—C1—C2 | 118.9 (3) | H29A—C29—H29B | 109.5 |
O1—C1—C2 | 125.4 (3) | C28—C29—H29C | 109.5 |
C1—C2—C3 | 119.9 (3) | H29A—C29—H29C | 109.5 |
C1—C2—H2 | 120.1 | H29B—C29—H29C | 109.5 |
C3—C2—H2 | 120.1 | C28—C30—H30A | 109.5 |
C2—C3—C4 | 122.5 (3) | C28—C30—H30B | 109.5 |
C2—C3—H3 | 118.7 | H30A—C30—H30B | 109.5 |
C4—C3—H3 | 118.7 | C28—C30—H30C | 109.5 |
C3—C4—C5 | 115.8 (2) | H30A—C30—H30C | 109.5 |
C3—C4—C9 | 122.8 (2) | H30B—C30—H30C | 109.5 |
C5—C4—C9 | 121.4 (2) | C36—C31—C32 | 116.0 (2) |
C6—C5—C4 | 122.7 (3) | C36—C31—C28 | 120.7 (2) |
C6—C5—H5 | 118.7 | C32—C31—C28 | 123.3 (2) |
C4—C5—H5 | 118.7 | C33—C32—C31 | 122.5 (2) |
C5—C6—C1 | 120.2 (3) | C33—C32—H32 | 118.8 |
C5—C6—H6 | 119.9 | C31—C32—H32 | 118.8 |
C1—C6—H6 | 119.9 | C34—C33—C32 | 119.9 (2) |
O1—C7—C8 | 112.4 (2) | C34—C33—H33 | 120.1 |
O1—C7—H7A | 109.1 | C32—C33—H33 | 120.1 |
C8—C7—H7A | 109.1 | C35—C34—C33 | 118.8 (3) |
O1—C7—H7B | 109.1 | C35—C34—O10 | 124.0 (2) |
C8—C7—H7B | 109.1 | C33—C34—O10 | 117.2 (2) |
H7A—C7—H7B | 107.9 | C34—C35—C36 | 120.7 (3) |
O3—C8—O2 | 126.6 (3) | C34—C35—H35 | 119.7 |
O3—C8—C7 | 123.0 (3) | C36—C35—H35 | 119.7 |
O2—C8—C7 | 110.4 (3) | C35—C36—C31 | 121.9 (3) |
C11—C9—C4 | 111.1 (2) | C35—C36—H36 | 119.0 |
C11—C9—C12 | 111.5 (2) | C31—C36—H36 | 119.0 |
C4—C9—C12 | 106.9 (2) | O10—C37—C38 | 111.5 (2) |
C11—C9—C10 | 106.2 (2) | O10—C37—H37A | 109.3 |
C4—C9—C10 | 110.5 (2) | C38—C37—H37A | 109.3 |
C12—C9—C10 | 110.8 (2) | O10—C37—H37B | 109.3 |
C9—C10—H10A | 109.5 | C38—C37—H37B | 109.3 |
C9—C10—H10B | 109.5 | H37A—C37—H37B | 108.0 |
H10A—C10—H10B | 109.5 | O12—C38—O11 | 125.9 (3) |
C9—C10—H10C | 109.5 | O12—C38—C37 | 123.0 (3) |
H10A—C10—H10C | 109.5 | O11—C38—C37 | 111.1 (2) |
| | | |
O12—Na1—O4—C15 | −129.52 (16) | C5—C4—C9—C10 | 38.1 (3) |
O6i—Na1—O4—C15 | 41.15 (16) | C11—C9—C12—C13 | 26.3 (4) |
O9ii—Na1—O4—C15 | 141.40 (16) | C4—C9—C12—C13 | −95.3 (3) |
O3ii—Na1—O4—C15 | 165.3 (3) | C10—C9—C12—C13 | 144.3 (3) |
O10—Na1—O4—C15 | −64.15 (16) | C11—C9—C12—C17 | −158.0 (2) |
Na2i—Na1—O4—C15 | 55.86 (19) | C4—C9—C12—C17 | 80.4 (3) |
O12—Na1—O4—C18 | 92.1 (2) | C10—C9—C12—C17 | −40.0 (3) |
O6i—Na1—O4—C18 | −97.2 (2) | C17—C12—C13—C14 | −0.1 (5) |
O9ii—Na1—O4—C18 | 3.0 (2) | C9—C12—C13—C14 | 175.8 (3) |
O3ii—Na1—O4—C18 | 27.0 (4) | C12—C13—C14—C15 | −0.1 (5) |
O10—Na1—O4—C18 | 157.5 (2) | C13—C14—C15—C16 | 0.4 (5) |
Na2i—Na1—O4—C18 | −82.5 (2) | C13—C14—C15—O4 | −178.8 (3) |
O9ii—Na2—O6—C19 | −27.7 (2) | C18—O4—C15—C16 | −167.9 (3) |
O3iii—Na2—O6—C19 | 140.6 (2) | Na1—O4—C15—C16 | 48.2 (3) |
O12—Na2—O6—C19 | −116.4 (2) | C18—O4—C15—C14 | 11.4 (4) |
O7ii—Na2—O6—C19 | 38.1 (2) | Na1—O4—C15—C14 | −132.5 (3) |
O1ii—Na2—O6—C19 | −108.0 (4) | C14—C15—C16—C17 | −0.6 (4) |
Na1iv—Na2—O6—C19 | 141.0 (3) | O4—C15—C16—C17 | 178.7 (3) |
O9ii—Na2—O6—Na1iv | −168.72 (9) | C15—C16—C17—C12 | 0.5 (4) |
O3iii—Na2—O6—Na1iv | −0.47 (9) | C13—C12—C17—C16 | −0.1 (4) |
O12—Na2—O6—Na1iv | 102.52 (9) | C9—C12—C17—C16 | −176.2 (3) |
O7ii—Na2—O6—Na1iv | −102.93 (8) | C15—O4—C18—C19 | 168.5 (2) |
O1ii—Na2—O6—Na1iv | 111.0 (3) | Na1—O4—C18—C19 | −58.3 (3) |
O12—Na1—O10—C34 | 168.6 (2) | Na1iv—O6—C19—O5 | 40.1 (5) |
O6i—Na1—O10—C34 | −18.0 (2) | Na2—O6—C19—O5 | −86.1 (4) |
O9ii—Na1—O10—C34 | 175.0 (2) | Na1iv—O6—C19—C18 | −138.9 (3) |
O3ii—Na1—O10—C34 | −107.1 (2) | Na2—O6—C19—C18 | 94.9 (3) |
O4—Na1—O10—C34 | 83.9 (2) | O4—C18—C19—O6 | −10.6 (4) |
Na2i—Na1—O10—C34 | −65.7 (2) | O4—C18—C19—O5 | 170.2 (3) |
O12—Na1—O10—C37 | −8.39 (17) | C26—O7—C20—C25 | 7.5 (4) |
O6i—Na1—O10—C37 | 165.00 (17) | Na2v—O7—C20—C25 | −177.5 (2) |
O9ii—Na1—O10—C37 | −2.0 (3) | C26—O7—C20—C21 | −171.1 (2) |
O3ii—Na1—O10—C37 | 75.90 (17) | Na2v—O7—C20—C21 | 3.9 (3) |
O4—Na1—O10—C37 | −93.10 (17) | C25—C20—C21—C22 | −4.6 (4) |
Na2i—Na1—O10—C37 | 117.31 (17) | O7—C20—C21—C22 | 174.1 (2) |
O6i—Na1—O12—C38 | −18.1 (6) | C20—C21—C22—C23 | 1.9 (4) |
O9ii—Na1—O12—C38 | −165.7 (2) | C21—C22—C23—C24 | 1.8 (4) |
O3ii—Na1—O12—C38 | −76.4 (2) | C21—C22—C23—C28 | −176.2 (2) |
O10—Na1—O12—C38 | 11.6 (2) | C22—C23—C24—C25 | −2.9 (4) |
O4—Na1—O12—C38 | 116.9 (2) | C28—C23—C24—C25 | 175.1 (2) |
Na2i—Na1—O12—C38 | −66.9 (2) | C21—C20—C25—C24 | 3.5 (4) |
O6i—Na1—O12—Na2 | 147.3 (4) | O7—C20—C25—C24 | −175.1 (2) |
O9ii—Na1—O12—Na2 | −0.27 (9) | C23—C24—C25—C20 | 0.4 (4) |
O3ii—Na1—O12—Na2 | 89.11 (9) | C20—O7—C26—C27 | 173.2 (2) |
O10—Na1—O12—Na2 | 177.03 (9) | Na2v—O7—C26—C27 | −2.8 (3) |
O4—Na1—O12—Na2 | −77.66 (8) | Na2v—O9—C27—O8 | −167.7 (2) |
Na2i—Na1—O12—Na2 | 98.55 (9) | Na1v—O9—C27—O8 | −4.4 (5) |
O9ii—Na2—O12—C38 | 162.8 (3) | Na2v—O9—C27—C26 | 13.2 (4) |
O3iii—Na2—O12—C38 | −23.4 (3) | Na1v—O9—C27—C26 | 176.5 (2) |
O6—Na2—O12—C38 | −113.9 (3) | O7—C26—C27—O9 | −5.3 (4) |
O7ii—Na2—O12—C38 | 163.8 (3) | O7—C26—C27—O8 | 175.4 (2) |
O1ii—Na2—O12—C38 | 68.2 (3) | C24—C23—C28—C31 | −77.7 (3) |
Na1iv—Na2—O12—C38 | −73.0 (3) | C22—C23—C28—C31 | 100.1 (3) |
O9ii—Na2—O12—Na1 | 0.28 (9) | C24—C23—C28—C30 | 42.4 (3) |
O3iii—Na2—O12—Na1 | 173.99 (9) | C22—C23—C28—C30 | −139.7 (2) |
O6—Na2—O12—Na1 | 83.49 (9) | C24—C23—C28—C29 | 159.7 (2) |
O7ii—Na2—O12—Na1 | 1.3 (2) | C22—C23—C28—C29 | −22.4 (3) |
O1ii—Na2—O12—Na1 | −94.39 (8) | C23—C28—C31—C36 | 76.2 (3) |
Na1iv—Na2—O12—Na1 | 124.43 (8) | C30—C28—C31—C36 | −43.7 (3) |
C7—O1—C1—C6 | 165.8 (3) | C29—C28—C31—C36 | −161.3 (2) |
Na2v—O1—C1—C6 | −47.8 (3) | C23—C28—C31—C32 | −102.6 (3) |
C7—O1—C1—C2 | −14.7 (4) | C30—C28—C31—C32 | 137.5 (3) |
Na2v—O1—C1—C2 | 131.7 (3) | C29—C28—C31—C32 | 19.9 (3) |
C6—C1—C2—C3 | −2.0 (4) | C36—C31—C32—C33 | −3.1 (4) |
O1—C1—C2—C3 | 178.5 (3) | C28—C31—C32—C33 | 175.7 (2) |
C1—C2—C3—C4 | 0.4 (5) | C31—C32—C33—C34 | −1.3 (4) |
C2—C3—C4—C5 | 1.1 (4) | C32—C33—C34—C35 | 5.0 (4) |
C2—C3—C4—C9 | −175.3 (3) | C32—C33—C34—O10 | −174.3 (2) |
C3—C4—C5—C6 | −1.1 (4) | C37—O10—C34—C35 | −7.8 (4) |
C9—C4—C5—C6 | 175.4 (3) | Na1—O10—C34—C35 | 175.3 (2) |
C4—C5—C6—C1 | −0.5 (4) | C37—O10—C34—C33 | 171.5 (2) |
O1—C1—C6—C5 | −178.4 (2) | Na1—O10—C34—C33 | −5.4 (4) |
C2—C1—C6—C5 | 2.0 (4) | C33—C34—C35—C36 | −4.2 (4) |
C1—O1—C7—C8 | −167.0 (2) | O10—C34—C35—C36 | 175.0 (3) |
Na2v—O1—C7—C8 | 55.7 (3) | C34—C35—C36—C31 | −0.3 (4) |
Na2vi—O3—C8—O2 | −36.7 (5) | C32—C31—C36—C35 | 3.9 (4) |
Na1v—O3—C8—O2 | 85.3 (4) | C28—C31—C36—C35 | −175.0 (3) |
Na2vi—O3—C8—C7 | 143.9 (2) | C34—O10—C37—C38 | −171.5 (2) |
Na1v—O3—C8—C7 | −94.1 (3) | Na1—O10—C37—C38 | 6.1 (3) |
O1—C7—C8—O3 | 9.6 (4) | Na1—O12—C38—O11 | 167.0 (2) |
O1—C7—C8—O2 | −169.9 (3) | Na2—O12—C38—O11 | 9.3 (5) |
C3—C4—C9—C11 | −28.1 (4) | Na1—O12—C38—C37 | −13.1 (4) |
C5—C4—C9—C11 | 155.7 (2) | Na2—O12—C38—C37 | −170.8 (2) |
C3—C4—C9—C12 | 93.8 (3) | O10—C37—C38—O12 | 2.4 (4) |
C5—C4—C9—C12 | −82.5 (3) | O10—C37—C38—O11 | −177.6 (2) |
C3—C4—C9—C10 | −145.6 (3) | | |
Symmetry codes: (i) x+1, y, z; (ii) −x+1, y−1/2, −z+1/2; (iii) −x, y−1/2, −z+1/2; (iv) x−1, y, z; (v) −x+1, y+1/2, −z+1/2; (vi) −x, y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H1···O11vi | 0.82 | 1.68 | 2.396 (3) | 145 |
O8—H8···O5vi | 0.82 | 1.66 | 2.431 (3) | 155 |
Symmetry code: (vi) −x, y+1/2, −z+1/2. |
(II) Poly[hexa-µ-aqua-diaquabis{µ
3-2,2'-[sulfonylbis(1,4-phenyleneoxy)]diacetato}tetrasodium(I)]
top
Crystal data top
[Na4(C16H14O8)2(H2O)8] | Z = 1 |
Mr = 964.72 | F(000) = 500 |
Triclinic, P1 | Dx = 1.598 Mg m−3 |
Hall symbol: P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.0980 (13) Å | Cell parameters from 1238 reflections |
b = 8.3820 (14) Å | θ = 2.5–22.0° |
c = 15.291 (2) Å | µ = 0.27 mm−1 |
α = 75.492 (1)° | T = 295 K |
β = 87.242 (2)° | Block, colourless |
γ = 86.712 (3)° | 0.16 × 0.12 × 0.09 mm |
V = 1002.6 (3) Å3 | |
Data collection top
Bruker APEXII CCD area-detector diffractometer | 4239 independent reflections |
Radiation source: fine-focus sealed tube | 3543 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
φ and ω scans | θmax = 25.0°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.958, Tmax = 0.976 | k = −9→9 |
5357 measured reflections | l = −18→8 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.051 | H-atom parameters constrained |
wR(F2) = 0.129 | w = 1/[σ2(Fo2) + (0.0669P)2 + 0.4471P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
4239 reflections | Δρmax = 0.93 e Å−3 |
559 parameters | Δρmin = −0.97 e Å−3 |
4 restraints | Absolute structure: Flack (1983), with 723 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.11 (12) |
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 | |
Na1 | 0.3124 (3) | 0.1109 (3) | 0.96519 (19) | 0.0345 (6) | |
Na2 | 0.6663 (3) | −0.2077 (3) | 0.96850 (18) | 0.0322 (6) | |
Na3 | 0.9677 (3) | −0.3232 (3) | 1.13537 (18) | 0.0326 (6) | |
Na4 | 1.2695 (3) | −0.6072 (3) | 1.09278 (19) | 0.0362 (6) | |
O1 | 0.2175 (6) | 0.2711 (5) | 0.8099 (3) | 0.0356 (11) | |
O2 | 0.3141 (6) | 0.3929 (5) | 0.9420 (3) | 0.0374 (11) | |
O3 | 0.2079 (7) | 0.6464 (6) | 0.8785 (4) | 0.0464 (13) | |
O4 | −0.1245 (6) | 0.0070 (6) | 0.4953 (3) | 0.0451 (12) | |
O5 | 0.0186 (6) | −0.2457 (5) | 0.5864 (3) | 0.0377 (11) | |
O6 | 0.5892 (5) | 0.0598 (5) | 0.2830 (3) | 0.0359 (11) | |
O7 | 0.8025 (6) | 0.1305 (6) | 0.1448 (3) | 0.0477 (14) | |
O8 | 0.9654 (6) | −0.0915 (5) | 0.1982 (3) | 0.0392 (12) | |
O9 | 0.6929 (6) | −0.2288 (5) | 0.8120 (3) | 0.0407 (12) | |
O10 | 0.7323 (6) | −0.4799 (5) | 0.9525 (3) | 0.0361 (11) | |
O11 | 0.7770 (6) | −0.6570 (5) | 0.8662 (3) | 0.0430 (13) | |
O12 | 0.4925 (6) | 0.5172 (5) | 0.6054 (3) | 0.0413 (12) | |
O13 | 0.3660 (6) | 0.3741 (6) | 0.5021 (3) | 0.0435 (13) | |
O14 | 1.0669 (5) | 0.5360 (5) | 0.2906 (3) | 0.0321 (10) | |
O15 | 1.2618 (5) | 0.6361 (5) | 0.1480 (3) | 0.0324 (10) | |
O16 | 1.4169 (6) | 0.7742 (6) | 0.2187 (3) | 0.0384 (11) | |
O17 | 0.3706 (5) | −0.1841 (5) | 0.9761 (3) | 0.0328 (10) | |
H33 | 0.3327 | −0.2313 | 1.0285 | 0.049* | |
H32 | 0.3236 | −0.2261 | 0.9392 | 0.049* | |
O18 | 0.6104 (6) | 0.0817 (5) | 0.9858 (3) | 0.0405 (12) | |
H34 | 0.6635 | 0.1653 | 0.9583 | 0.061* | |
H35 | 0.6511 | 0.0625 | 1.0378 | 0.061* | |
O19 | 0.0110 (5) | 0.1221 (5) | 0.9766 (3) | 0.0388 (11) | |
H37 | −0.0425 | 0.1129 | 1.0267 | 0.058* | |
H36 | −0.0625 | 0.1825 | 0.9444 | 0.058* | |
O20 | 0.2587 (6) | 0.0908 (6) | 1.1286 (3) | 0.0411 (12) | |
H38 | 0.1678 | 0.0489 | 1.1501 | 0.062* | |
H39 | 0.3319 | 0.0408 | 1.1649 | 0.062* | |
O21 | 0.6824 (5) | −0.3164 (4) | 1.1323 (3) | 0.0392 (11) | |
H40 | 0.6446 | −0.4099 | 1.1344 | 0.059* | |
H41 | 0.6203 | −0.2793 | 1.1698 | 0.059* | |
O22 | 0.9581 (5) | −0.1991 (5) | 0.9757 (3) | 0.0380 (11) | |
H42 | 1.0106 | −0.2433 | 0.9376 | 0.057* | |
H43 | 0.9890 | −0.1005 | 0.9629 | 0.057* | |
O23 | 0.9750 (5) | −0.5758 (5) | 1.0875 (3) | 0.0364 (11) | |
H45 | 0.9279 | −0.6660 | 1.1092 | 0.055* | |
H44 | 0.9341 | −0.5351 | 1.0361 | 0.055* | |
O24 | 1.5515 (5) | −0.6360 (4) | 1.1089 (3) | 0.0429 (12) | |
H47 | 1.5974 | −0.5914 | 1.0582 | 0.064* | |
H46 | 1.6117 | −0.7224 | 1.1296 | 0.064* | |
C1 | 0.2422 (8) | 0.4965 (8) | 0.8798 (4) | 0.0291 (15) | |
C2 | 0.1947 (8) | 0.4451 (7) | 0.7967 (4) | 0.0311 (15) | |
H2A | 0.0797 | 0.4783 | 0.7842 | 0.037* | |
H2B | 0.2622 | 0.5002 | 0.7450 | 0.037* | |
C3 | 0.1621 (8) | 0.2005 (7) | 0.7460 (4) | 0.0288 (15) | |
C4 | 0.0896 (9) | 0.2883 (8) | 0.6663 (5) | 0.0361 (17) | |
H4 | 0.0729 | 0.4023 | 0.6541 | 0.043* | |
C5 | 0.0429 (8) | 0.2030 (8) | 0.6053 (4) | 0.0309 (15) | |
H5 | −0.0034 | 0.2602 | 0.5512 | 0.037* | |
C6 | 0.0647 (8) | 0.0328 (8) | 0.6247 (4) | 0.0280 (15) | |
C7 | 0.1333 (9) | −0.0555 (8) | 0.7054 (4) | 0.0361 (17) | |
H7 | 0.1482 | −0.1697 | 0.7186 | 0.043* | |
C8 | 0.1782 (9) | 0.0316 (8) | 0.7650 (5) | 0.0376 (17) | |
H8 | 0.2210 | −0.0260 | 0.8200 | 0.045* | |
C9 | 0.1909 (8) | −0.0393 (8) | 0.4643 (4) | 0.0290 (15) | |
C10 | 0.3225 (8) | −0.1522 (8) | 0.4747 (4) | 0.0316 (15) | |
H10 | 0.3207 | −0.2467 | 0.5221 | 0.038* | |
C11 | 0.4593 (8) | −0.1261 (8) | 0.4144 (4) | 0.0331 (16) | |
H11 | 0.5469 | −0.2043 | 0.4199 | 0.040* | |
C12 | 0.4623 (8) | 0.0186 (8) | 0.3462 (4) | 0.0285 (14) | |
C13 | 0.3284 (8) | 0.1348 (8) | 0.3383 (5) | 0.0360 (16) | |
H13 | 0.3307 | 0.2329 | 0.2935 | 0.043* | |
C14 | 0.1951 (8) | 0.1033 (8) | 0.3967 (5) | 0.0346 (16) | |
H14 | 0.1057 | 0.1795 | 0.3906 | 0.041* | |
C15 | 0.7276 (8) | −0.0541 (8) | 0.2867 (5) | 0.0321 (15) | |
H15A | 0.6892 | −0.1630 | 0.2898 | 0.038* | |
H15B | 0.7882 | −0.0601 | 0.3407 | 0.038* | |
C16 | 0.8407 (8) | −0.0014 (8) | 0.2042 (5) | 0.0315 (15) | |
C17 | 0.7400 (8) | −0.5172 (8) | 0.8790 (5) | 0.0314 (15) | |
C18 | 0.6937 (9) | −0.3844 (7) | 0.7948 (5) | 0.0362 (16) | |
H18A | 0.7726 | −0.3899 | 0.7458 | 0.043* | |
H18B | 0.5849 | −0.4032 | 0.7765 | 0.043* | |
C19 | 0.6501 (8) | −0.0899 (7) | 0.7448 (4) | 0.0283 (14) | |
C20 | 0.6825 (9) | 0.0561 (8) | 0.7642 (5) | 0.0400 (17) | |
H20 | 0.7345 | 0.0545 | 0.8174 | 0.048* | |
C21 | 0.6387 (10) | 0.2058 (8) | 0.7057 (5) | 0.0391 (17) | |
H21 | 0.6610 | 0.3050 | 0.7186 | 0.047* | |
C22 | 0.5608 (7) | 0.2034 (7) | 0.6277 (4) | 0.0253 (14) | |
C23 | 0.5330 (8) | 0.0569 (8) | 0.6062 (5) | 0.0337 (16) | |
H23 | 0.4853 | 0.0581 | 0.5519 | 0.040* | |
C24 | 0.5762 (8) | −0.0922 (8) | 0.6659 (5) | 0.0355 (16) | |
H24 | 0.5558 | −0.1916 | 0.6528 | 0.043* | |
C25 | 0.6739 (8) | 0.4422 (7) | 0.4755 (4) | 0.0254 (14) | |
C26 | 0.7981 (8) | 0.5358 (7) | 0.4921 (4) | 0.0305 (15) | |
H26 | 0.7916 | 0.5761 | 0.5436 | 0.037* | |
C27 | 0.9332 (8) | 0.5700 (8) | 0.4315 (4) | 0.0331 (16) | |
H27 | 1.0169 | 0.6335 | 0.4421 | 0.040* | |
C28 | 0.9412 (8) | 0.5088 (7) | 0.3559 (4) | 0.0276 (14) | |
C29 | 0.8180 (9) | 0.4127 (8) | 0.3405 (5) | 0.0353 (16) | |
H29 | 0.8252 | 0.3710 | 0.2895 | 0.042* | |
C30 | 0.6850 (8) | 0.3784 (8) | 0.4003 (5) | 0.0354 (16) | |
H30 | 0.6028 | 0.3126 | 0.3902 | 0.042* | |
C31 | 1.2021 (8) | 0.6310 (8) | 0.3044 (4) | 0.0335 (15) | |
H31A | 1.2724 | 0.5649 | 0.3508 | 0.040* | |
H31B | 1.1595 | 0.7275 | 0.3239 | 0.040* | |
C32 | 1.3020 (8) | 0.6840 (7) | 0.2151 (5) | 0.0281 (14) | |
S1 | 0.0202 (2) | −0.0725 (2) | 0.54321 (13) | 0.0309 (4) | |
S2 | 0.5052 (2) | 0.39511 (19) | 0.55314 (12) | 0.0304 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.0341 (14) | 0.0268 (13) | 0.0434 (17) | 0.0004 (10) | −0.0034 (12) | −0.0104 (12) |
Na2 | 0.0319 (13) | 0.0325 (13) | 0.0327 (15) | 0.0003 (10) | −0.0042 (11) | −0.0088 (11) |
Na3 | 0.0289 (13) | 0.0352 (14) | 0.0363 (15) | 0.0027 (10) | −0.0042 (11) | −0.0141 (12) |
Na4 | 0.0350 (14) | 0.0378 (14) | 0.0405 (16) | 0.0031 (11) | −0.0042 (12) | −0.0187 (12) |
O1 | 0.058 (3) | 0.029 (2) | 0.023 (2) | 0.000 (2) | −0.009 (2) | −0.0127 (19) |
O2 | 0.054 (3) | 0.026 (2) | 0.032 (3) | 0.001 (2) | −0.010 (2) | −0.006 (2) |
O3 | 0.072 (4) | 0.030 (3) | 0.042 (3) | 0.005 (2) | −0.019 (3) | −0.016 (2) |
O4 | 0.032 (3) | 0.067 (3) | 0.040 (3) | 0.004 (2) | −0.012 (2) | −0.020 (3) |
O5 | 0.049 (3) | 0.036 (3) | 0.034 (3) | −0.016 (2) | 0.007 (2) | −0.018 (2) |
O6 | 0.036 (3) | 0.035 (3) | 0.032 (3) | 0.006 (2) | 0.005 (2) | −0.002 (2) |
O7 | 0.052 (3) | 0.040 (3) | 0.038 (3) | 0.012 (2) | 0.008 (2) | 0.010 (2) |
O8 | 0.032 (3) | 0.038 (3) | 0.047 (3) | 0.008 (2) | 0.004 (2) | −0.015 (2) |
O9 | 0.070 (4) | 0.021 (2) | 0.029 (3) | 0.003 (2) | −0.013 (2) | −0.002 (2) |
O10 | 0.053 (3) | 0.029 (2) | 0.027 (3) | 0.002 (2) | −0.008 (2) | −0.007 (2) |
O11 | 0.065 (3) | 0.023 (2) | 0.043 (3) | 0.009 (2) | −0.014 (3) | −0.010 (2) |
O12 | 0.058 (3) | 0.030 (2) | 0.031 (3) | 0.012 (2) | 0.005 (2) | −0.002 (2) |
O13 | 0.032 (3) | 0.050 (3) | 0.038 (3) | 0.001 (2) | −0.007 (2) | 0.008 (2) |
O14 | 0.039 (3) | 0.034 (2) | 0.024 (2) | −0.0114 (19) | 0.005 (2) | −0.0074 (19) |
O15 | 0.030 (2) | 0.042 (3) | 0.029 (3) | −0.0042 (19) | 0.003 (2) | −0.015 (2) |
O16 | 0.033 (3) | 0.044 (3) | 0.043 (3) | −0.012 (2) | 0.005 (2) | −0.019 (2) |
O17 | 0.037 (3) | 0.034 (2) | 0.028 (3) | −0.0079 (19) | −0.003 (2) | −0.008 (2) |
O18 | 0.038 (3) | 0.034 (2) | 0.049 (3) | −0.008 (2) | −0.006 (2) | −0.007 (2) |
O19 | 0.031 (3) | 0.041 (3) | 0.045 (3) | −0.002 (2) | −0.004 (2) | −0.011 (2) |
O20 | 0.041 (3) | 0.039 (3) | 0.040 (3) | −0.001 (2) | −0.007 (2) | −0.004 (2) |
O21 | 0.031 (3) | 0.044 (3) | 0.041 (3) | −0.001 (2) | 0.003 (2) | −0.009 (2) |
O22 | 0.039 (3) | 0.035 (3) | 0.043 (3) | −0.011 (2) | 0.000 (2) | −0.016 (2) |
O23 | 0.038 (3) | 0.027 (2) | 0.042 (3) | 0.0004 (19) | −0.008 (2) | −0.004 (2) |
O24 | 0.035 (3) | 0.041 (3) | 0.047 (3) | 0.007 (2) | −0.002 (2) | −0.002 (2) |
C1 | 0.030 (3) | 0.028 (4) | 0.029 (4) | −0.004 (3) | 0.003 (3) | −0.009 (3) |
C2 | 0.041 (4) | 0.024 (3) | 0.032 (4) | −0.002 (3) | −0.004 (3) | −0.012 (3) |
C3 | 0.034 (4) | 0.026 (3) | 0.027 (4) | 0.001 (3) | 0.001 (3) | −0.009 (3) |
C4 | 0.050 (4) | 0.029 (4) | 0.029 (4) | 0.009 (3) | −0.001 (3) | −0.010 (3) |
C5 | 0.039 (4) | 0.032 (4) | 0.025 (4) | 0.004 (3) | −0.003 (3) | −0.013 (3) |
C6 | 0.033 (4) | 0.033 (4) | 0.020 (3) | −0.001 (3) | 0.006 (3) | −0.012 (3) |
C7 | 0.061 (5) | 0.025 (3) | 0.025 (4) | 0.002 (3) | −0.003 (3) | −0.010 (3) |
C8 | 0.057 (4) | 0.032 (4) | 0.022 (4) | −0.004 (3) | −0.012 (3) | 0.000 (3) |
C9 | 0.038 (4) | 0.030 (3) | 0.022 (3) | 0.000 (3) | −0.004 (3) | −0.014 (3) |
C10 | 0.037 (4) | 0.032 (3) | 0.024 (4) | −0.002 (3) | 0.003 (3) | −0.005 (3) |
C11 | 0.036 (4) | 0.034 (4) | 0.026 (4) | 0.011 (3) | −0.005 (3) | −0.004 (3) |
C12 | 0.033 (4) | 0.034 (4) | 0.018 (3) | 0.002 (3) | −0.002 (3) | −0.007 (3) |
C13 | 0.042 (4) | 0.034 (4) | 0.029 (4) | 0.008 (3) | −0.003 (3) | −0.004 (3) |
C14 | 0.036 (4) | 0.031 (4) | 0.034 (4) | 0.010 (3) | −0.001 (3) | −0.007 (3) |
C15 | 0.032 (3) | 0.031 (3) | 0.032 (4) | 0.001 (3) | −0.006 (3) | −0.004 (3) |
C16 | 0.035 (4) | 0.025 (3) | 0.040 (4) | −0.007 (3) | 0.002 (3) | −0.016 (3) |
C17 | 0.031 (4) | 0.026 (3) | 0.035 (4) | −0.002 (3) | −0.001 (3) | −0.005 (3) |
C18 | 0.053 (4) | 0.027 (4) | 0.028 (4) | −0.002 (3) | 0.000 (3) | −0.008 (3) |
C19 | 0.041 (4) | 0.021 (3) | 0.022 (3) | 0.001 (3) | −0.001 (3) | −0.004 (3) |
C20 | 0.056 (5) | 0.035 (4) | 0.031 (4) | 0.000 (3) | −0.011 (3) | −0.010 (3) |
C21 | 0.062 (5) | 0.023 (3) | 0.032 (4) | −0.011 (3) | −0.007 (3) | −0.003 (3) |
C22 | 0.027 (3) | 0.027 (3) | 0.020 (3) | 0.000 (3) | −0.002 (3) | −0.001 (3) |
C23 | 0.042 (4) | 0.036 (4) | 0.024 (4) | 0.000 (3) | −0.003 (3) | −0.009 (3) |
C24 | 0.049 (4) | 0.028 (4) | 0.029 (4) | −0.008 (3) | −0.001 (3) | −0.005 (3) |
C25 | 0.033 (3) | 0.023 (3) | 0.017 (3) | 0.000 (3) | −0.004 (3) | 0.001 (3) |
C26 | 0.043 (4) | 0.026 (3) | 0.022 (3) | −0.005 (3) | −0.001 (3) | −0.005 (3) |
C27 | 0.038 (4) | 0.030 (3) | 0.030 (4) | −0.008 (3) | −0.001 (3) | −0.004 (3) |
C28 | 0.036 (4) | 0.022 (3) | 0.023 (4) | −0.002 (3) | −0.002 (3) | −0.002 (3) |
C29 | 0.044 (4) | 0.034 (4) | 0.027 (4) | −0.010 (3) | 0.001 (3) | −0.005 (3) |
C30 | 0.039 (4) | 0.030 (4) | 0.037 (4) | −0.013 (3) | −0.003 (3) | −0.006 (3) |
C31 | 0.036 (4) | 0.041 (4) | 0.026 (4) | −0.007 (3) | −0.001 (3) | −0.011 (3) |
C32 | 0.027 (3) | 0.020 (3) | 0.039 (4) | 0.006 (3) | 0.002 (3) | −0.011 (3) |
S1 | 0.0316 (9) | 0.0351 (10) | 0.0308 (10) | −0.0053 (7) | 0.0006 (7) | −0.0167 (8) |
S2 | 0.0313 (9) | 0.0280 (9) | 0.0276 (9) | 0.0015 (7) | 0.0001 (7) | 0.0002 (7) |
Geometric parameters (Å, º) top
Na1—O2 | 2.301 (5) | O23—H45 | 0.8500 |
Na1—O19 | 2.437 (5) | O23—H44 | 0.8500 |
Na1—O18 | 2.440 (5) | O24—H47 | 0.8501 |
Na1—O17 | 2.456 (5) | O24—H46 | 0.8500 |
Na1—O20 | 2.481 (5) | C1—C2 | 1.513 (9) |
Na1—O1 | 2.548 (5) | C2—H2A | 0.9700 |
Na1—Na4i | 3.415 (4) | C2—H2B | 0.9700 |
Na1—Na2 | 3.797 (3) | C3—C8 | 1.372 (9) |
Na2—O22 | 2.378 (5) | C3—C4 | 1.394 (9) |
Na2—O10 | 2.383 (5) | C4—C5 | 1.387 (9) |
Na2—O17 | 2.391 (5) | C4—H4 | 0.9300 |
Na2—O9 | 2.442 (5) | C5—C6 | 1.385 (8) |
Na2—O21 | 2.449 (5) | C5—H5 | 0.9300 |
Na2—O18 | 2.519 (5) | C6—C7 | 1.393 (9) |
Na2—Na3 | 3.535 (4) | C6—S1 | 1.759 (6) |
Na3—O21 | 2.310 (5) | C7—C8 | 1.374 (10) |
Na3—O8ii | 2.371 (5) | C7—H7 | 0.9300 |
Na3—O15iii | 2.396 (5) | C8—H8 | 0.9300 |
Na3—O23 | 2.403 (5) | C9—C14 | 1.371 (9) |
Na3—O22 | 2.405 (5) | C9—C10 | 1.372 (9) |
Na3—O14iii | 2.519 (5) | C9—S1 | 1.778 (7) |
Na3—Na4 | 3.467 (3) | C10—C11 | 1.398 (9) |
Na4—O24 | 2.301 (5) | C10—H10 | 0.9300 |
Na4—O2iv | 2.317 (5) | C11—C12 | 1.388 (9) |
Na4—O23 | 2.387 (5) | C11—H11 | 0.9300 |
Na4—O15iii | 2.391 (5) | C12—C13 | 1.404 (9) |
Na4—O20iv | 2.458 (5) | C13—C14 | 1.361 (9) |
Na4—Na1iv | 3.415 (4) | C13—H13 | 0.9300 |
O1—C3 | 1.367 (8) | C14—H14 | 0.9300 |
O1—C2 | 1.424 (7) | C15—C16 | 1.510 (9) |
O2—C1 | 1.256 (7) | C15—H15A | 0.9700 |
O3—C1 | 1.267 (7) | C15—H15B | 0.9700 |
O4—S1 | 1.450 (5) | C17—C18 | 1.522 (9) |
O5—S1 | 1.437 (5) | C18—H18A | 0.9700 |
O6—C12 | 1.374 (7) | C18—H18B | 0.9700 |
O6—C15 | 1.424 (7) | C19—C20 | 1.372 (9) |
O7—C16 | 1.276 (8) | C19—C24 | 1.376 (9) |
O8—C16 | 1.240 (7) | C20—C21 | 1.385 (9) |
O9—C19 | 1.386 (7) | C20—H20 | 0.9300 |
O9—C18 | 1.393 (8) | C21—C22 | 1.382 (9) |
O10—C17 | 1.237 (8) | C21—H21 | 0.9300 |
O11—C17 | 1.253 (8) | C22—C23 | 1.381 (9) |
O12—S2 | 1.444 (5) | C22—S2 | 1.770 (6) |
O13—S2 | 1.445 (5) | C23—C24 | 1.388 (9) |
O14—C28 | 1.378 (8) | C23—H23 | 0.9300 |
O14—C31 | 1.443 (7) | C24—H24 | 0.9300 |
O15—C32 | 1.255 (8) | C25—C26 | 1.381 (9) |
O16—C32 | 1.244 (7) | C25—C30 | 1.382 (9) |
O17—H33 | 0.8500 | C25—S2 | 1.762 (6) |
O17—H32 | 0.8500 | C26—C27 | 1.393 (9) |
O18—H34 | 0.8500 | C26—H26 | 0.9300 |
O18—H35 | 0.8499 | C27—C28 | 1.375 (9) |
O19—H37 | 0.8499 | C27—H27 | 0.9300 |
O19—H36 | 0.8500 | C28—C29 | 1.382 (9) |
O20—H38 | 0.8501 | C29—C30 | 1.374 (10) |
O20—H39 | 0.8500 | C29—H29 | 0.9300 |
O21—H40 | 0.8500 | C30—H30 | 0.9300 |
O21—H41 | 0.8500 | C31—C32 | 1.532 (9) |
O22—H42 | 0.8501 | C31—H31A | 0.9700 |
O22—H43 | 0.8500 | C31—H31B | 0.9700 |
| | | |
O2—Na1—O19 | 90.70 (18) | H38—O20—H39 | 105.6 |
O2—Na1—O18 | 91.65 (18) | Na3—O21—Na2 | 95.91 (18) |
O19—Na1—O18 | 168.8 (2) | Na3—O21—H40 | 113.1 |
O2—Na1—O17 | 167.8 (2) | Na2—O21—H40 | 96.3 |
O19—Na1—O17 | 100.84 (17) | Na3—O21—H41 | 122.4 |
O18—Na1—O17 | 77.78 (16) | Na2—O21—H41 | 122.7 |
O2—Na1—O20 | 88.47 (18) | H40—O21—H41 | 103.9 |
O19—Na1—O20 | 78.00 (18) | Na2—O22—Na3 | 95.33 (18) |
O18—Na1—O20 | 91.14 (18) | Na2—O22—H42 | 112.7 |
O17—Na1—O20 | 97.68 (17) | Na3—O22—H42 | 121.1 |
O2—Na1—O1 | 65.95 (16) | Na2—O22—H43 | 111.5 |
O19—Na1—O1 | 74.39 (17) | Na3—O22—H43 | 111.4 |
O18—Na1—O1 | 116.47 (19) | H42—O22—H43 | 104.8 |
O17—Na1—O1 | 113.23 (17) | Na4—O23—Na3 | 92.72 (17) |
O20—Na1—O1 | 141.60 (18) | Na4—O23—H45 | 112.7 |
O2—Na1—Na4i | 42.50 (13) | Na3—O23—H45 | 131.6 |
O19—Na1—Na4i | 83.13 (14) | Na4—O23—H44 | 117.1 |
O18—Na1—Na4i | 91.25 (14) | Na3—O23—H44 | 96.7 |
O17—Na1—Na4i | 142.29 (15) | H45—O23—H44 | 105.9 |
O20—Na1—Na4i | 45.98 (12) | Na4—O24—H47 | 107.9 |
O1—Na1—Na4i | 104.01 (13) | Na4—O24—H46 | 129.4 |
O2—Na1—Na2 | 130.58 (15) | H47—O24—H46 | 104.6 |
O19—Na1—Na2 | 138.65 (14) | O2—C1—O3 | 125.6 (6) |
O18—Na1—Na2 | 40.80 (12) | O2—C1—C2 | 119.4 (6) |
O17—Na1—Na2 | 37.82 (11) | O3—C1—C2 | 115.0 (6) |
O20—Na1—Na2 | 102.02 (13) | O1—C2—C1 | 110.5 (5) |
O1—Na1—Na2 | 116.35 (14) | O1—C2—H2A | 109.5 |
Na4i—Na1—Na2 | 126.83 (9) | C1—C2—H2A | 109.5 |
O22—Na2—O10 | 83.18 (17) | O1—C2—H2B | 109.5 |
O22—Na2—O17 | 170.55 (19) | C1—C2—H2B | 109.5 |
O10—Na2—O17 | 105.15 (18) | H2A—C2—H2B | 108.1 |
O22—Na2—O9 | 91.09 (19) | O1—C3—C8 | 115.9 (6) |
O10—Na2—O9 | 65.79 (16) | O1—C3—C4 | 124.3 (6) |
O17—Na2—O9 | 96.40 (18) | C8—C3—C4 | 119.7 (6) |
O22—Na2—O21 | 83.07 (17) | C5—C4—C3 | 118.9 (6) |
O10—Na2—O21 | 88.26 (16) | C5—C4—H4 | 120.5 |
O17—Na2—O21 | 92.58 (17) | C3—C4—H4 | 120.5 |
O9—Na2—O21 | 153.94 (17) | C6—C5—C4 | 120.2 (6) |
O22—Na2—O18 | 94.20 (17) | C6—C5—H5 | 119.9 |
O10—Na2—O18 | 177.37 (19) | C4—C5—H5 | 119.9 |
O17—Na2—O18 | 77.48 (16) | C5—C6—C7 | 120.8 (6) |
O9—Na2—O18 | 114.36 (18) | C5—C6—S1 | 119.8 (5) |
O21—Na2—O18 | 91.45 (17) | C7—C6—S1 | 119.2 (4) |
O22—Na2—Na3 | 42.64 (13) | C8—C7—C6 | 117.9 (6) |
O10—Na2—Na3 | 81.96 (13) | C8—C7—H7 | 121.0 |
O17—Na2—Na3 | 132.95 (15) | C6—C7—H7 | 121.0 |
O9—Na2—Na3 | 127.31 (15) | C3—C8—C7 | 122.2 (6) |
O21—Na2—Na3 | 40.55 (11) | C3—C8—H8 | 118.9 |
O18—Na2—Na3 | 96.13 (13) | C7—C8—H8 | 118.9 |
O22—Na2—Na1 | 133.25 (14) | C14—C9—C10 | 120.3 (6) |
O10—Na2—Na1 | 143.35 (15) | C14—C9—S1 | 120.0 (5) |
O17—Na2—Na1 | 39.05 (11) | C10—C9—S1 | 119.6 (5) |
O9—Na2—Na1 | 103.58 (13) | C9—C10—C11 | 120.3 (6) |
O21—Na2—Na1 | 98.80 (13) | C9—C10—H10 | 119.8 |
O18—Na2—Na1 | 39.27 (11) | C11—C10—H10 | 119.8 |
Na3—Na2—Na1 | 125.61 (9) | C12—C11—C10 | 118.9 (6) |
O21—Na3—O8ii | 92.76 (16) | C12—C11—H11 | 120.6 |
O21—Na3—O15iii | 173.21 (19) | C10—C11—H11 | 120.6 |
O8ii—Na3—O15iii | 91.36 (17) | O6—C12—C11 | 124.7 (6) |
O21—Na3—O23 | 88.42 (16) | O6—C12—C13 | 115.4 (5) |
O8ii—Na3—O23 | 174.0 (2) | C11—C12—C13 | 119.8 (6) |
O15iii—Na3—O23 | 86.92 (16) | C14—C13—C12 | 119.7 (6) |
O21—Na3—O22 | 85.46 (17) | C14—C13—H13 | 120.1 |
O8ii—Na3—O22 | 102.87 (18) | C12—C13—H13 | 120.1 |
O15iii—Na3—O22 | 98.87 (17) | C13—C14—C9 | 120.9 (6) |
O23—Na3—O22 | 83.13 (18) | C13—C14—H14 | 119.5 |
O21—Na3—O14iii | 111.09 (18) | C9—C14—H14 | 119.5 |
O8ii—Na3—O14iii | 80.65 (17) | O6—C15—C16 | 110.5 (5) |
O15iii—Na3—O14iii | 64.32 (15) | O6—C15—H15A | 109.5 |
O23—Na3—O14iii | 93.39 (16) | C16—C15—H15A | 109.5 |
O22—Na3—O14iii | 163.06 (18) | O6—C15—H15B | 109.5 |
O21—Na3—Na4 | 131.84 (14) | C16—C15—H15B | 109.5 |
O8ii—Na3—Na4 | 134.83 (15) | H15A—C15—H15B | 108.1 |
O15iii—Na3—Na4 | 43.54 (12) | O8—C16—O7 | 123.9 (6) |
O23—Na3—Na4 | 43.45 (12) | O8—C16—C15 | 117.2 (6) |
O22—Na3—Na4 | 89.44 (14) | O7—C16—C15 | 118.8 (5) |
O14iii—Na3—Na4 | 76.89 (12) | O10—C17—O11 | 126.6 (6) |
C32iii—Na3—Na4 | 63.81 (13) | O10—C17—C18 | 118.2 (6) |
O21—Na3—Na2 | 43.54 (12) | O11—C17—C18 | 115.2 (6) |
O8ii—Na3—Na2 | 103.21 (14) | O9—C18—C17 | 110.3 (5) |
O15iii—Na3—Na2 | 140.17 (15) | O9—C18—H18A | 109.6 |
O23—Na3—Na2 | 81.71 (13) | C17—C18—H18A | 109.6 |
O22—Na3—Na2 | 42.04 (12) | O9—C18—H18B | 109.6 |
O14iii—Na3—Na2 | 153.93 (14) | C17—C18—H18B | 109.6 |
C32iii—Na3—Na2 | 155.30 (16) | H18A—C18—H18B | 108.1 |
Na4—Na3—Na2 | 114.07 (9) | C20—C19—C24 | 121.1 (6) |
O24—Na4—O2iv | 88.47 (18) | C20—C19—O9 | 114.1 (6) |
O24—Na4—O23 | 175.7 (2) | C24—C19—O9 | 124.8 (6) |
O2iv—Na4—O23 | 95.82 (19) | C19—C20—C21 | 120.8 (7) |
O24—Na4—O15iii | 89.91 (16) | C19—C20—H20 | 119.6 |
O2iv—Na4—O15iii | 123.79 (18) | C21—C20—H20 | 119.6 |
O23—Na4—O15iii | 87.41 (17) | C22—C21—C20 | 118.0 (6) |
O24—Na4—O20iv | 89.14 (17) | C22—C21—H21 | 121.0 |
O2iv—Na4—O20iv | 88.68 (18) | C20—C21—H21 | 121.0 |
O23—Na4—O20iv | 91.30 (17) | C23—C22—C21 | 121.4 (6) |
O15iii—Na4—O20iv | 147.5 (2) | C23—C22—S2 | 120.7 (5) |
O24—Na4—Na1iv | 87.60 (13) | C21—C22—S2 | 117.8 (5) |
O2iv—Na4—Na1iv | 42.15 (12) | C22—C23—C24 | 119.9 (6) |
O23—Na4—Na1iv | 95.81 (14) | C22—C23—H23 | 120.1 |
O15iii—Na4—Na1iv | 165.76 (16) | C24—C23—H23 | 120.1 |
O20iv—Na4—Na1iv | 46.54 (13) | C19—C24—C23 | 118.7 (6) |
O24—Na4—Na3 | 133.57 (14) | C19—C24—H24 | 120.7 |
O2iv—Na4—Na3 | 115.25 (14) | C23—C24—H24 | 120.7 |
O23—Na4—Na3 | 43.83 (12) | C26—C25—C30 | 120.3 (6) |
O15iii—Na4—Na3 | 43.66 (12) | C26—C25—S2 | 120.1 (5) |
O20iv—Na4—Na3 | 128.17 (16) | C30—C25—S2 | 119.6 (5) |
Na1iv—Na4—Na3 | 137.11 (10) | C25—C26—C27 | 120.0 (6) |
C3—O1—C2 | 118.5 (5) | C25—C26—H26 | 120.0 |
C3—O1—Na1 | 124.5 (4) | C27—C26—H26 | 120.0 |
C2—O1—Na1 | 116.1 (4) | C28—C27—C26 | 119.2 (6) |
C1—O2—Na1 | 125.4 (4) | C28—C27—H27 | 120.4 |
C1—O2—Na4i | 122.1 (4) | C26—C27—H27 | 120.4 |
Na1—O2—Na4i | 95.35 (19) | C27—C28—O14 | 124.6 (6) |
C12—O6—C15 | 118.1 (5) | C27—C28—C29 | 120.5 (6) |
C16—O8—Na3v | 123.9 (4) | O14—C28—C29 | 114.9 (6) |
C19—O9—C18 | 119.8 (5) | C30—C29—C28 | 120.3 (7) |
C19—O9—Na2 | 117.7 (4) | C30—C29—H29 | 119.8 |
C18—O9—Na2 | 118.7 (4) | C28—C29—H29 | 119.8 |
C17—O10—Na2 | 123.7 (4) | C29—C30—C25 | 119.6 (6) |
C28—O14—C31 | 117.5 (5) | C29—C30—H30 | 120.2 |
C28—O14—Na3vi | 113.3 (3) | C25—C30—H30 | 120.2 |
C31—O14—Na3vi | 105.1 (3) | O14—C31—C32 | 108.5 (5) |
C32—O15—Na4vi | 140.7 (4) | O14—C31—H31A | 110.0 |
C32—O15—Na3vi | 108.2 (4) | C32—C31—H31A | 110.0 |
Na4vi—O15—Na3vi | 92.81 (17) | O14—C31—H31B | 110.0 |
Na2—O17—Na1 | 103.13 (18) | C32—C31—H31B | 110.0 |
Na2—O17—H33 | 111.2 | H31A—C31—H31B | 108.4 |
Na1—O17—H33 | 104.0 | O16—C32—O15 | 127.3 (6) |
Na2—O17—H32 | 114.5 | O16—C32—C31 | 113.5 (6) |
Na1—O17—H32 | 117.4 | O15—C32—C31 | 119.2 (6) |
H33—O17—H32 | 106.2 | O16—C32—Na3vi | 143.9 (4) |
Na1—O18—Na2 | 99.93 (18) | O15—C32—Na3vi | 48.7 (3) |
Na1—O18—H34 | 114.6 | C31—C32—Na3vi | 82.5 (4) |
Na2—O18—H34 | 125.5 | O5—S1—O4 | 118.6 (3) |
Na1—O18—H35 | 121.8 | O5—S1—C6 | 108.2 (3) |
Na2—O18—H35 | 94.8 | O4—S1—C6 | 109.0 (3) |
H34—O18—H35 | 100.4 | O5—S1—C9 | 108.4 (3) |
Na1—O19—H37 | 122.5 | O4—S1—C9 | 106.9 (3) |
Na1—O19—H36 | 132.7 | C6—S1—C9 | 104.9 (3) |
H37—O19—H36 | 95.9 | O12—S2—O13 | 119.5 (3) |
Na4i—O20—Na1 | 87.49 (17) | O12—S2—C25 | 107.7 (3) |
Na4i—O20—H38 | 117.5 | O13—S2—C25 | 106.8 (3) |
Na1—O20—H38 | 114.9 | O12—S2—C22 | 107.4 (3) |
Na4i—O20—H39 | 113.5 | O13—S2—C22 | 108.9 (3) |
Na1—O20—H39 | 117.7 | C25—S2—C22 | 105.8 (3) |
| | | |
O2—Na1—Na2—O22 | 13.5 (3) | O10—Na2—O9—C18 | 14.4 (5) |
O19—Na1—Na2—O22 | −170.3 (3) | O17—Na2—O9—C18 | −89.4 (5) |
O18—Na1—Na2—O22 | −7.3 (3) | O21—Na2—O9—C18 | 20.1 (7) |
O17—Na1—Na2—O22 | −171.9 (3) | O18—Na2—O9—C18 | −168.5 (5) |
O20—Na1—Na2—O22 | −84.9 (2) | Na3—Na2—O9—C18 | 72.0 (5) |
O1—Na1—Na2—O22 | 93.5 (2) | Na1—Na2—O9—C18 | −128.4 (5) |
Na4i—Na1—Na2—O22 | −41.6 (2) | O22—Na2—O10—C17 | −99.3 (5) |
O2—Na1—Na2—O10 | −158.7 (3) | O17—Na2—O10—C17 | 85.3 (5) |
O19—Na1—Na2—O10 | 17.5 (4) | O9—Na2—O10—C17 | −5.0 (5) |
O18—Na1—Na2—O10 | −179.6 (3) | O21—Na2—O10—C17 | 177.5 (5) |
O17—Na1—Na2—O10 | 15.8 (3) | Na3—Na2—O10—C17 | −142.3 (5) |
O20—Na1—Na2—O10 | 102.9 (3) | Na1—Na2—O10—C17 | 75.0 (6) |
O1—Na1—Na2—O10 | −78.8 (3) | O10—Na2—O17—Na1 | −170.29 (17) |
Na4i—Na1—Na2—O10 | 146.1 (2) | O9—Na2—O17—Na1 | −103.69 (18) |
O2—Na1—Na2—O17 | −174.5 (3) | O21—Na2—O17—Na1 | 100.82 (18) |
O19—Na1—Na2—O17 | 1.6 (3) | O18—Na2—O17—Na1 | 9.90 (18) |
O18—Na1—Na2—O17 | 164.6 (3) | Na3—Na2—O17—Na1 | 96.6 (2) |
O20—Na1—Na2—O17 | 87.1 (2) | O2—Na1—O17—Na2 | 20.1 (10) |
O1—Na1—Na2—O17 | −94.6 (2) | O19—Na1—O17—Na2 | −178.89 (19) |
Na4i—Na1—Na2—O17 | 130.3 (2) | O18—Na1—O17—Na2 | −10.21 (19) |
O2—Na1—Na2—O9 | −91.2 (2) | O20—Na1—O17—Na2 | −99.7 (2) |
O19—Na1—Na2—O9 | 85.0 (3) | O1—Na1—O17—Na2 | 103.6 (2) |
O18—Na1—Na2—O9 | −112.0 (2) | Na4i—Na1—O17—Na2 | −86.1 (3) |
O17—Na1—Na2—O9 | 83.4 (2) | O2—Na1—O18—Na2 | −164.3 (2) |
O20—Na1—Na2—O9 | 170.42 (19) | O19—Na1—O18—Na2 | 93.7 (10) |
O1—Na1—Na2—O9 | −11.2 (2) | O17—Na1—O18—Na2 | 9.58 (18) |
Na4i—Na1—Na2—O9 | −146.32 (15) | O20—Na1—O18—Na2 | 107.19 (19) |
O2—Na1—Na2—O21 | 102.3 (2) | O1—Na1—O18—Na2 | −100.5 (2) |
O19—Na1—Na2—O21 | −81.5 (3) | Na4i—Na1—O18—Na2 | 153.18 (16) |
O18—Na1—Na2—O21 | 81.4 (2) | O22—Na2—O18—Na1 | 174.67 (19) |
O17—Na1—Na2—O21 | −83.2 (2) | O17—Na2—O18—Na1 | −9.85 (18) |
O20—Na1—Na2—O21 | 3.87 (17) | O9—Na2—O18—Na1 | 81.6 (2) |
O1—Na1—Na2—O21 | −177.76 (17) | O21—Na2—O18—Na1 | −102.18 (19) |
Na4i—Na1—Na2—O21 | 47.13 (16) | Na3—Na2—O18—Na1 | −142.55 (15) |
O2—Na1—Na2—O18 | 20.9 (3) | O2—Na1—O20—Na4i | −0.99 (18) |
O19—Na1—Na2—O18 | −163.0 (3) | O19—Na1—O20—Na4i | −92.03 (17) |
O17—Na1—Na2—O18 | −164.6 (3) | O18—Na1—O20—Na4i | 90.63 (16) |
O20—Na1—Na2—O18 | −77.6 (2) | O17—Na1—O20—Na4i | 168.45 (16) |
O1—Na1—Na2—O18 | 100.8 (2) | O1—Na1—O20—Na4i | −47.3 (3) |
Na4i—Na1—Na2—O18 | −34.3 (2) | Na2—Na1—O20—Na4i | 130.29 (12) |
O2—Na1—Na2—Na3 | 68.9 (2) | O8ii—Na3—O21—Na2 | 106.33 (17) |
O19—Na1—Na2—Na3 | −114.9 (2) | O23—Na3—O21—Na2 | −79.60 (17) |
O18—Na1—Na2—Na3 | 48.0 (2) | O22—Na3—O21—Na2 | 3.63 (17) |
O17—Na1—Na2—Na3 | −116.6 (2) | O14iii—Na3—O21—Na2 | −172.62 (16) |
O20—Na1—Na2—Na3 | −29.52 (17) | C32iii—Na3—O21—Na2 | 153.0 (4) |
O1—Na1—Na2—Na3 | 148.84 (15) | Na4—Na3—O21—Na2 | −81.5 (2) |
Na4i—Na1—Na2—Na3 | 13.74 (17) | O22—Na2—O21—Na3 | −3.69 (17) |
O22—Na2—Na3—O21 | 174.6 (3) | O10—Na2—O21—Na3 | 79.65 (17) |
O10—Na2—Na3—O21 | −96.8 (2) | O17—Na2—O21—Na3 | −175.27 (16) |
O17—Na2—Na3—O21 | 6.5 (2) | O9—Na2—O21—Na3 | 74.5 (4) |
O9—Na2—Na3—O21 | −147.8 (2) | O18—Na2—O21—Na3 | −97.74 (17) |
O18—Na2—Na3—O21 | 85.0 (2) | Na1—Na2—O21—Na3 | −136.50 (13) |
Na1—Na2—Na3—O21 | 56.80 (17) | O10—Na2—O22—Na3 | −85.53 (18) |
O22—Na2—Na3—O8ii | 94.7 (2) | O9—Na2—O22—Na3 | −150.99 (17) |
O10—Na2—Na3—O8ii | −176.69 (19) | O21—Na2—O22—Na3 | 3.54 (16) |
O17—Na2—Na3—O8ii | −73.5 (2) | O18—Na2—O22—Na3 | 94.49 (19) |
O9—Na2—Na3—O8ii | 132.2 (2) | Na1—Na2—O22—Na3 | 99.1 (2) |
O21—Na2—Na3—O8ii | −79.9 (2) | O21—Na3—O22—Na2 | −3.73 (17) |
O18—Na2—Na3—O8ii | 5.13 (19) | O8ii—Na3—O22—Na2 | −95.54 (19) |
Na1—Na2—Na3—O8ii | −23.13 (18) | O15iii—Na3—O22—Na2 | 171.00 (17) |
O22—Na2—Na3—O15iii | −14.0 (3) | O23—Na3—O22—Na2 | 85.22 (17) |
O10—Na2—Na3—O15iii | 74.7 (3) | O14iii—Na3—O22—Na2 | 164.2 (6) |
O17—Na2—Na3—O15iii | 177.9 (3) | C32iii—Na3—O22—Na2 | −170.93 (17) |
O9—Na2—Na3—O15iii | 23.6 (3) | Na4—Na3—O22—Na2 | 128.33 (14) |
O21—Na2—Na3—O15iii | 171.4 (3) | O2iv—Na4—O23—Na3 | −120.86 (18) |
O18—Na2—Na3—O15iii | −103.5 (2) | O15iii—Na4—O23—Na3 | 2.85 (18) |
Na1—Na2—Na3—O15iii | −131.8 (2) | O20iv—Na4—O23—Na3 | 150.33 (18) |
O22—Na2—Na3—O23 | −88.9 (2) | Na1iv—Na4—O23—Na3 | −163.24 (14) |
O10—Na2—Na3—O23 | −0.28 (18) | O21—Na3—O23—Na4 | −177.91 (18) |
O17—Na2—Na3—O23 | 103.0 (2) | O15iii—Na3—O23—Na4 | −2.85 (18) |
O9—Na2—Na3—O23 | −51.4 (2) | O22—Na3—O23—Na4 | 96.47 (18) |
O21—Na2—Na3—O23 | 96.49 (19) | O14iii—Na3—O23—Na4 | −66.87 (18) |
O18—Na2—Na3—O23 | −178.46 (18) | C32iii—Na3—O23—Na4 | −16.9 (2) |
Na1—Na2—Na3—O23 | 153.28 (14) | Na2—Na3—O23—Na4 | 138.88 (15) |
O10—Na2—Na3—O22 | 88.6 (2) | Na1—O2—C1—O3 | 161.8 (5) |
O17—Na2—Na3—O22 | −168.1 (3) | Na4i—O2—C1—O3 | 36.3 (9) |
O9—Na2—Na3—O22 | 37.6 (2) | Na1—O2—C1—C2 | −20.3 (8) |
O21—Na2—Na3—O22 | −174.6 (3) | Na4i—O2—C1—C2 | −145.7 (5) |
O18—Na2—Na3—O22 | −89.5 (2) | C3—O1—C2—C1 | 172.3 (5) |
Na1—Na2—Na3—O22 | −117.8 (2) | Na1—O1—C2—C1 | 2.9 (7) |
O22—Na2—Na3—O14iii | −169.6 (4) | O2—C1—C2—O1 | 9.7 (8) |
O10—Na2—Na3—O14iii | −81.0 (3) | O3—C1—C2—O1 | −172.1 (5) |
O17—Na2—Na3—O14iii | 22.3 (4) | C2—O1—C3—C8 | −176.1 (6) |
O9—Na2—Na3—O14iii | −132.0 (3) | Na1—O1—C3—C8 | −7.7 (8) |
O21—Na2—Na3—O14iii | 15.8 (3) | C2—O1—C3—C4 | 2.5 (9) |
O18—Na2—Na3—O14iii | 100.9 (3) | Na1—O1—C3—C4 | 170.9 (5) |
Na1—Na2—Na3—O14iii | 72.6 (3) | O1—C3—C4—C5 | 178.1 (6) |
O22—Na2—Na3—C32iii | 20.1 (4) | C8—C3—C4—C5 | −3.3 (10) |
O10—Na2—Na3—C32iii | 108.7 (4) | C3—C4—C5—C6 | 1.5 (10) |
O17—Na2—Na3—C32iii | −148.0 (3) | C4—C5—C6—C7 | 0.2 (10) |
O9—Na2—Na3—C32iii | 57.7 (4) | C4—C5—C6—S1 | −175.0 (5) |
O21—Na2—Na3—C32iii | −154.5 (4) | C5—C6—C7—C8 | 0.1 (10) |
O18—Na2—Na3—C32iii | −69.4 (4) | S1—C6—C7—C8 | 175.2 (6) |
Na1—Na2—Na3—C32iii | −97.7 (4) | O1—C3—C8—C7 | −177.6 (7) |
O22—Na2—Na3—Na4 | −59.22 (19) | C4—C3—C8—C7 | 3.7 (11) |
O10—Na2—Na3—Na4 | 29.41 (16) | C6—C7—C8—C3 | −2.0 (11) |
O17—Na2—Na3—Na4 | 132.65 (19) | C14—C9—C10—C11 | −2.5 (10) |
O9—Na2—Na3—Na4 | −21.7 (2) | S1—C9—C10—C11 | −178.6 (5) |
O21—Na2—Na3—Na4 | 126.19 (18) | C9—C10—C11—C12 | 2.4 (10) |
O18—Na2—Na3—Na4 | −148.77 (14) | C15—O6—C12—C11 | 0.6 (9) |
Na1—Na2—Na3—Na4 | −177.02 (10) | C15—O6—C12—C13 | −179.2 (6) |
O21—Na3—Na4—O24 | −172.4 (3) | C10—C11—C12—O6 | 179.7 (6) |
O8ii—Na3—Na4—O24 | −3.5 (3) | C10—C11—C12—C13 | −0.6 (10) |
O15iii—Na3—Na4—O24 | 0.7 (3) | O6—C12—C13—C14 | 178.5 (6) |
O23—Na3—Na4—O24 | −175.2 (3) | C11—C12—C13—C14 | −1.2 (10) |
O22—Na3—Na4—O24 | 104.3 (2) | C12—C13—C14—C9 | 1.2 (10) |
O14iii—Na3—Na4—O24 | −65.7 (2) | C10—C9—C14—C13 | 0.6 (10) |
C32iii—Na3—Na4—O24 | −13.4 (3) | S1—C9—C14—C13 | 176.7 (5) |
Na2—Na3—Na4—O24 | 139.4 (2) | C12—O6—C15—C16 | 171.1 (5) |
O21—Na3—Na4—O2iv | 73.6 (3) | Na3v—O8—C16—O7 | −93.1 (7) |
O8ii—Na3—Na4—O2iv | −117.5 (3) | Na3v—O8—C16—C15 | 86.0 (7) |
O15iii—Na3—Na4—O2iv | −113.4 (2) | O6—C15—C16—O8 | −178.9 (5) |
O23—Na3—Na4—O2iv | 70.8 (2) | O6—C15—C16—O7 | 0.3 (8) |
O22—Na3—Na4—O2iv | −9.8 (2) | Na2—O10—C17—O11 | 178.6 (5) |
O14iii—Na3—Na4—O2iv | −179.7 (2) | Na2—O10—C17—C18 | −4.2 (8) |
C32iii—Na3—Na4—O2iv | −127.5 (2) | C19—O9—C18—C17 | −178.5 (5) |
Na2—Na3—Na4—O2iv | 25.30 (19) | Na2—O9—C18—C17 | −20.7 (7) |
O21—Na3—Na4—O23 | 2.8 (2) | O10—C17—C18—O9 | 16.3 (9) |
O8ii—Na3—Na4—O23 | 171.7 (3) | O11—C17—C18—O9 | −166.1 (6) |
O15iii—Na3—Na4—O23 | 175.9 (3) | C18—O9—C19—C20 | −168.9 (6) |
O22—Na3—Na4—O23 | −80.6 (2) | Na2—O9—C19—C20 | 33.1 (7) |
O14iii—Na3—Na4—O23 | 109.5 (2) | C18—O9—C19—C24 | 13.3 (10) |
C32iii—Na3—Na4—O23 | 161.8 (2) | Na2—O9—C19—C24 | −144.8 (6) |
Na2—Na3—Na4—O23 | −45.47 (18) | C24—C19—C20—C21 | 1.3 (11) |
O21—Na3—Na4—O15iii | −173.1 (3) | O9—C19—C20—C21 | −176.6 (6) |
O8ii—Na3—Na4—O15iii | −4.2 (3) | C19—C20—C21—C22 | 0.3 (11) |
O23—Na3—Na4—O15iii | −175.9 (3) | C20—C21—C22—C23 | −2.6 (11) |
O22—Na3—Na4—O15iii | 103.5 (2) | C20—C21—C22—S2 | −180.0 (5) |
O14iii—Na3—Na4—O15iii | −66.36 (19) | C21—C22—C23—C24 | 3.2 (10) |
C32iii—Na3—Na4—O15iii | −14.1 (2) | S2—C22—C23—C24 | −179.5 (5) |
Na2—Na3—Na4—O15iii | 138.66 (19) | C20—C19—C24—C23 | −0.7 (10) |
O21—Na3—Na4—O20iv | −36.2 (3) | O9—C19—C24—C23 | 177.0 (6) |
O8ii—Na3—Na4—O20iv | 132.7 (3) | C22—C23—C24—C19 | −1.5 (10) |
O15iii—Na3—Na4—O20iv | 136.9 (3) | C30—C25—C26—C27 | 1.7 (9) |
O23—Na3—Na4—O20iv | −39.0 (2) | S2—C25—C26—C27 | 178.7 (5) |
O22—Na3—Na4—O20iv | −119.6 (2) | C25—C26—C27—C28 | −0.3 (9) |
O14iii—Na3—Na4—O20iv | 70.5 (2) | C26—C27—C28—O14 | 179.0 (5) |
C32iii—Na3—Na4—O20iv | 122.8 (2) | C26—C27—C28—C29 | −0.8 (9) |
Na2—Na3—Na4—O20iv | −84.5 (2) | C31—O14—C28—C27 | 2.2 (8) |
O21—Na3—Na4—Na1iv | 27.7 (3) | Na3vi—O14—C28—C27 | −120.7 (6) |
O8ii—Na3—Na4—Na1iv | −163.4 (2) | C31—O14—C28—C29 | −178.0 (5) |
O15iii—Na3—Na4—Na1iv | −159.2 (2) | Na3vi—O14—C28—C29 | 59.1 (6) |
O23—Na3—Na4—Na1iv | 24.9 (2) | C27—C28—C29—C30 | 0.6 (9) |
O22—Na3—Na4—Na1iv | −55.65 (19) | O14—C28—C29—C30 | −179.2 (6) |
O14iii—Na3—Na4—Na1iv | 134.44 (18) | C28—C29—C30—C25 | 0.7 (10) |
C32iii—Na3—Na4—Na1iv | −173.3 (2) | C26—C25—C30—C29 | −1.9 (9) |
Na2—Na3—Na4—Na1iv | −20.53 (19) | S2—C25—C30—C29 | −178.9 (5) |
O2—Na1—O1—C3 | −177.0 (5) | C28—O14—C31—C32 | −165.5 (5) |
O19—Na1—O1—C3 | −79.1 (5) | Na3vi—O14—C31—C32 | −38.5 (5) |
O18—Na1—O1—C3 | 103.8 (5) | Na4vi—O15—C32—O16 | 108.2 (7) |
O17—Na1—O1—C3 | 16.3 (5) | Na3vi—O15—C32—O16 | −133.0 (6) |
O20—Na1—O1—C3 | −124.6 (5) | Na4vi—O15—C32—C31 | −72.5 (8) |
Na4i—Na1—O1—C3 | −157.6 (5) | Na3vi—O15—C32—C31 | 46.3 (6) |
Na2—Na1—O1—C3 | 58.0 (5) | Na4vi—O15—C32—Na3vi | −118.8 (7) |
O2—Na1—O1—C2 | −8.3 (4) | O14—C31—C32—O16 | 176.5 (5) |
O19—Na1—O1—C2 | 89.6 (4) | O14—C31—C32—O15 | −3.0 (8) |
O18—Na1—O1—C2 | −87.5 (4) | O14—C31—C32—Na3vi | 30.3 (4) |
O17—Na1—O1—C2 | −175.0 (4) | C5—C6—S1—O5 | −167.8 (5) |
O20—Na1—O1—C2 | 44.1 (5) | C7—C6—S1—O5 | 17.0 (6) |
Na4i—Na1—O1—C2 | 11.0 (4) | C5—C6—S1—O4 | −37.4 (6) |
Na2—Na1—O1—C2 | −133.4 (4) | C7—C6—S1—O4 | 147.3 (5) |
O19—Na1—O2—C1 | −57.1 (5) | C5—C6—S1—C9 | 76.7 (6) |
O18—Na1—O2—C1 | 133.9 (5) | C7—C6—S1—C9 | −98.5 (5) |
O17—Na1—O2—C1 | 104.3 (10) | C14—C9—S1—O5 | 161.5 (5) |
O20—Na1—O2—C1 | −135.0 (5) | C10—C9—S1—O5 | −22.4 (6) |
O1—Na1—O2—C1 | 15.5 (5) | C14—C9—S1—O4 | 32.5 (6) |
Na4i—Na1—O2—C1 | −136.1 (6) | C10—C9—S1—O4 | −151.4 (5) |
Na2—Na1—O2—C1 | 120.4 (5) | C14—C9—S1—C6 | −83.1 (6) |
O19—Na1—O2—Na4i | 79.03 (19) | C10—C9—S1—C6 | 93.0 (5) |
O18—Na1—O2—Na4i | −90.0 (2) | C26—C25—S2—O12 | 22.4 (5) |
O17—Na1—O2—Na4i | −119.6 (9) | C30—C25—S2—O12 | −160.6 (5) |
O20—Na1—O2—Na4i | 1.05 (19) | C26—C25—S2—O13 | 151.9 (5) |
O1—Na1—O2—Na4i | 151.6 (2) | C30—C25—S2—O13 | −31.1 (6) |
Na2—Na1—O2—Na4i | −103.5 (2) | C26—C25—S2—C22 | −92.2 (5) |
O22—Na2—O9—C19 | −105.3 (4) | C30—C25—S2—C22 | 84.8 (6) |
O10—Na2—O9—C19 | 172.7 (5) | C23—C22—S2—O12 | 159.7 (5) |
O17—Na2—O9—C19 | 68.9 (5) | C21—C22—S2—O12 | −22.9 (6) |
O21—Na2—O9—C19 | 178.4 (4) | C23—C22—S2—O13 | 28.9 (6) |
O18—Na2—O9—C19 | −10.2 (5) | C21—C22—S2—O13 | −153.7 (5) |
Na3—Na2—O9—C19 | −129.7 (4) | C23—C22—S2—C25 | −85.5 (6) |
Na1—Na2—O9—C19 | 29.9 (5) | C21—C22—S2—C25 | 91.9 (6) |
O22—Na2—O9—C18 | 96.4 (5) | | |
Symmetry codes: (i) x−1, y+1, z; (ii) x, y, z+1; (iii) x, y−1, z+1; (iv) x+1, y−1, z; (v) x, y, z−1; (vi) x, y+1, z−1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O24—H46···O6vii | 0.85 | 2.59 | 3.204 (6) | 130 |
O24—H46···O7vii | 0.85 | 1.91 | 2.716 (6) | 159 |
O24—H47···O10viii | 0.85 | 1.97 | 2.809 (7) | 171 |
O23—H44···O10 | 0.85 | 2.08 | 2.856 (6) | 151 |
O23—H45···O7iii | 0.85 | 1.98 | 2.824 (7) | 173 |
O22—H43···O19viii | 0.85 | 1.95 | 2.754 (6) | 158 |
O22—H42···O3iv | 0.85 | 2.08 | 2.890 (7) | 159 |
O19—H36···O11i | 0.85 | 2.02 | 2.865 (7) | 175 |
O20—H38···O8ix | 0.85 | 2.07 | 2.910 (6) | 170 |
O19—H37···O7ix | 0.85 | 2.18 | 3.021 (7) | 170 |
O18—H35···O7ii | 0.85 | 2.29 | 3.071 (8) | 153 |
O18—H34···O11x | 0.85 | 2.01 | 2.838 (7) | 166 |
O17—H32···O3xi | 0.85 | 1.89 | 2.730 (7) | 168 |
O21—H41···O16xii | 0.85 | 1.85 | 2.643 (6) | 154 |
O20—H39···O16xii | 0.85 | 2.26 | 2.921 (6) | 135 |
O17—H33···O15xii | 0.85 | 1.96 | 2.810 (6) | 173 |
O21—H40···O24xiii | 0.85 | 2.21 | 3.044 (3) | 168 |
Symmetry codes: (i) x−1, y+1, z; (ii) x, y, z+1; (iii) x, y−1, z+1; (iv) x+1, y−1, z; (vii) x+1, y−1, z+1; (viii) x+1, y, z; (ix) x−1, y, z+1; (x) x, y+1, z; (xi) x, y−1, z; (xii) x−1, y−1, z+1; (xiii) x−1, y, z. |