Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804005318/hg6023sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804005318/hg6023Isup2.hkl |
CCDC reference: 238653
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998; program(s) used to solve structure: SHELXTL (Bruker, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXTL.
Na+·C14H13O3 | F(000) = 528 |
Mr = 252.23 | Dx = 1.390 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 881 reflections |
a = 9.969 (3) Å | θ = 2.5–27.4° |
b = 5.9346 (16) Å | µ = 0.13 mm−1 |
c = 20.823 (6) Å | T = 298 K |
β = 102.025 (5)° | Prism, colorless |
V = 1204.9 (6) Å3 | 0.71 × 0.61 × 0.34 mm |
Z = 4 |
Bruker SMART 1000 diffractometer | 4036 independent reflections |
Radiation source: normal-focus sealed tube | 3269 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ω scans | θmax = 26.8°, θmin = 2.0° |
Absorption correction: multi-scan (Blessing, 1995) | h = −11→12 |
Tmin = 0.915, Tmax = 0.958 | k = −6→7 |
6886 measured reflections | l = −26→24 |
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)] = 0.050 | H-atom parameters constrained |
wR(F2) = 0.131 | w = 1/[σ2(Fo2) + (0.0807P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.004 |
4036 reflections | Δρmax = 0.32 e Å−3 |
329 parameters | Δρmin = −0.35 e Å−3 |
1 restraint | Absolute structure: (Flack, 1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.1 (4) |
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. |
x | y | z | Uiso*/Ueq | ||
Na1 | −0.10398 (10) | 0.48664 (18) | 0.00061 (5) | 0.0338 (3) | |
Na2 | −0.40560 (10) | 0.25104 (19) | −0.00854 (5) | 0.0346 (3) | |
O1a | −0.33202 (19) | 0.5662 (3) | −0.05815 (9) | 0.0323 (4) | |
O1b | −0.06803 (19) | −0.1564 (3) | 0.04241 (9) | 0.0338 (5) | |
O2a | −0.43654 (18) | 0.8879 (4) | −0.04611 (9) | 0.0337 (5) | |
C1a | −0.7203 (3) | 1.1676 (5) | −0.33536 (13) | 0.0380 (7) | |
H1 | −0.7657 | 1.3092 | −0.3332 | 0.046* | |
C1b | 0.1576 (3) | 0.1591 (6) | 0.36098 (14) | 0.0474 (8) | |
H1' | 0.1415 | 0.2942 | 0.3836 | 0.057* | |
C2a | −0.6072 (3) | 1.1051 (5) | −0.28458 (12) | 0.0326 (6) | |
C2b | 0.0641 (3) | 0.0937 (5) | 0.30248 (13) | 0.0381 (7) | |
C3a | −0.5566 (3) | 1.2458 (5) | −0.23121 (13) | 0.0347 (6) | |
H3 | −0.5955 | 1.3931 | −0.2296 | 0.042* | |
C3b | −0.0535 (3) | 0.2190 (5) | 0.27568 (14) | 0.0425 (7) | |
H3' | −0.0733 | 0.3544 | 0.2971 | 0.051* | |
C4b | −0.1408 (3) | 0.1498 (6) | 0.21891 (13) | 0.0383 (7) | |
H4' | −0.2216 | 0.2368 | 0.2020 | 0.046* | |
C4a | −0.4528 (3) | 1.1775 (5) | −0.18137 (13) | 0.0326 (6) | |
H4 | −0.4186 | 1.2794 | −0.1459 | 0.039* | |
C5a | −0.3950 (3) | 0.9616 (5) | −0.18078 (12) | 0.0282 (6) | |
C5b | −0.1147 (3) | −0.0449 (5) | 0.18498 (13) | 0.0313 (6) | |
C6b | −0.0021 (3) | −0.1694 (5) | 0.21093 (13) | 0.0367 (7) | |
H6' | 0.0160 | −0.3043 | 0.1888 | 0.044* | |
C6a | −0.4387 (3) | 0.8258 (5) | −0.23407 (13) | 0.0334 (6) | |
H6 | −0.3970 | 0.6805 | −0.2354 | 0.040* | |
C7a | −0.5436 (3) | 0.8935 (5) | −0.28734 (13) | 0.0333 (6) | |
C7b | 0.0899 (3) | −0.1058 (5) | 0.27003 (13) | 0.0360 (7) | |
C8b | 0.2085 (3) | −0.2346 (7) | 0.29674 (15) | 0.0482 (8) | |
H8' | 0.2275 | −0.3704 | 0.2752 | 0.058* | |
C8a | −0.5879 (3) | 0.7558 (6) | −0.34292 (14) | 0.0457 (8) | |
H8 | −0.5418 | 0.6160 | −0.3468 | 0.055* | |
C9a | −0.6955 (3) | 0.8202 (7) | −0.39107 (16) | 0.0524 (9) | |
H9 | −0.7254 | 0.7240 | −0.4284 | 0.063* | |
C9b | 0.2944 (3) | −0.1669 (7) | 0.35220 (16) | 0.0538 (9) | |
H9' | 0.3741 | −0.2559 | 0.3696 | 0.065* | |
C10b | 0.2705 (3) | 0.0296 (7) | 0.38501 (15) | 0.0507 (9) | |
C10a | −0.7638 (3) | 1.0262 (6) | −0.38696 (14) | 0.0440 (8) | |
C11b | −0.2102 (3) | −0.1069 (5) | 0.12103 (13) | 0.0301 (6) | |
H11' | −0.2946 | −0.0267 | 0.1191 | 0.036* | |
C11a | −0.2871 (3) | 0.8862 (5) | −0.12182 (12) | 0.0294 (6) | |
H11 | −0.2446 | 1.0203 | −0.1011 | 0.035* | |
C12a | −0.3570 (2) | 0.7688 (5) | −0.07157 (12) | 0.0242 (5) | |
C12b | −0.1486 (2) | −0.0253 (5) | 0.06357 (12) | 0.0252 (5) | |
C13b | −0.2440 (3) | −0.3571 (5) | 0.11613 (15) | 0.0405 (7) | |
H13D | −0.2860 | −0.4000 | 0.1518 | 0.061* | |
H13E | −0.1612 | −0.4421 | 0.1183 | 0.061* | |
H13F | −0.3060 | −0.3871 | 0.0752 | 0.061* | |
C13a | −0.1741 (3) | 0.7452 (6) | −0.14027 (14) | 0.0424 (7) | |
H13A | −0.1412 | 0.8179 | −0.1752 | 0.064* | |
H13B | −0.2094 | 0.5990 | −0.1545 | 0.064* | |
H13C | −0.1001 | 0.7296 | −0.1028 | 0.064* | |
C14a | −0.9586 (4) | 1.2517 (8) | −0.43119 (19) | 0.0709 (12) | |
H14A | −0.9056 | 1.3876 | −0.4291 | 0.106* | |
H14B | −0.9938 | 1.2371 | −0.3919 | 0.106* | |
H14C | −1.0335 | 1.2577 | −0.4685 | 0.106* | |
C14b | 0.3550 (5) | 0.2839 (9) | 0.4724 (2) | 0.0860 (15) | |
H14D | 0.2704 | 0.2867 | 0.4876 | 0.129* | |
H14E | 0.3563 | 0.4062 | 0.4424 | 0.129* | |
H14F | 0.4305 | 0.2991 | 0.5092 | 0.129* | |
O3a | −0.8740 (2) | 1.0633 (5) | −0.43720 (11) | 0.0599 (7) | |
O3b | 0.3664 (3) | 0.0764 (6) | 0.44008 (12) | 0.0704 (8) | |
O2b | −0.17852 (19) | 0.1665 (3) | 0.04152 (9) | 0.0353 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Na1 | 0.0275 (6) | 0.0249 (6) | 0.0515 (7) | 0.0022 (4) | 0.0142 (4) | 0.0028 (5) |
Na2 | 0.0290 (6) | 0.0250 (6) | 0.0531 (6) | 0.0029 (5) | 0.0165 (5) | 0.0039 (5) |
O1a | 0.0330 (10) | 0.0239 (10) | 0.0404 (10) | −0.0009 (8) | 0.0087 (8) | 0.0017 (8) |
O1b | 0.0294 (10) | 0.0296 (11) | 0.0463 (11) | 0.0004 (9) | 0.0172 (8) | −0.0017 (9) |
O2a | 0.0284 (10) | 0.0346 (12) | 0.0417 (10) | 0.0033 (9) | 0.0152 (8) | 0.0008 (9) |
C1a | 0.0358 (15) | 0.0379 (17) | 0.0382 (15) | 0.0049 (13) | 0.0030 (12) | 0.0070 (13) |
C1b | 0.054 (2) | 0.049 (2) | 0.0389 (16) | −0.0063 (16) | 0.0086 (14) | −0.0011 (15) |
C2a | 0.0341 (15) | 0.0320 (16) | 0.0321 (14) | −0.0009 (12) | 0.0076 (11) | 0.0044 (12) |
C2b | 0.0432 (17) | 0.0389 (18) | 0.0334 (14) | 0.0004 (14) | 0.0109 (12) | 0.0021 (13) |
C3a | 0.0382 (15) | 0.0258 (14) | 0.0395 (15) | 0.0061 (12) | 0.0064 (11) | 0.0032 (13) |
C3b | 0.0546 (19) | 0.0308 (17) | 0.0435 (16) | 0.0043 (14) | 0.0135 (14) | −0.0077 (13) |
C4b | 0.0391 (16) | 0.0339 (16) | 0.0438 (16) | 0.0062 (13) | 0.0132 (13) | 0.0021 (14) |
C4a | 0.0359 (15) | 0.0280 (15) | 0.0326 (14) | 0.0020 (12) | 0.0042 (11) | 0.0004 (11) |
C5a | 0.0255 (13) | 0.0283 (15) | 0.0326 (14) | −0.0002 (11) | 0.0098 (10) | 0.0061 (11) |
C5b | 0.0331 (14) | 0.0292 (15) | 0.0347 (14) | 0.0001 (12) | 0.0141 (11) | 0.0018 (12) |
C6b | 0.0393 (16) | 0.0327 (16) | 0.0398 (15) | 0.0054 (13) | 0.0121 (12) | −0.0034 (13) |
C6a | 0.0317 (14) | 0.0269 (15) | 0.0412 (15) | 0.0039 (12) | 0.0066 (11) | 0.0009 (12) |
C7a | 0.0334 (14) | 0.0328 (16) | 0.0332 (14) | −0.0003 (12) | 0.0056 (11) | 0.0019 (12) |
C7b | 0.0402 (16) | 0.0356 (17) | 0.0344 (14) | 0.0010 (13) | 0.0132 (12) | 0.0028 (13) |
C8b | 0.0431 (17) | 0.052 (2) | 0.0505 (18) | 0.0125 (16) | 0.0114 (14) | 0.0024 (17) |
C8a | 0.0502 (18) | 0.0398 (18) | 0.0453 (17) | 0.0035 (16) | 0.0053 (13) | −0.0078 (15) |
C9a | 0.054 (2) | 0.058 (2) | 0.0400 (17) | 0.0004 (18) | −0.0021 (14) | −0.0132 (17) |
C9b | 0.0415 (18) | 0.065 (2) | 0.053 (2) | 0.0071 (17) | 0.0040 (14) | 0.0077 (18) |
C10b | 0.0474 (19) | 0.065 (2) | 0.0376 (16) | −0.0085 (17) | 0.0044 (13) | 0.0060 (17) |
C10a | 0.0389 (17) | 0.054 (2) | 0.0362 (16) | −0.0015 (15) | 0.0009 (12) | 0.0046 (15) |
C11b | 0.0257 (13) | 0.0276 (15) | 0.0387 (15) | 0.0004 (11) | 0.0107 (11) | 0.0004 (12) |
C11a | 0.0244 (13) | 0.0322 (16) | 0.0327 (14) | −0.0040 (11) | 0.0087 (10) | 0.0025 (12) |
C12a | 0.0172 (11) | 0.0252 (15) | 0.0290 (13) | −0.0015 (10) | 0.0022 (9) | −0.0012 (11) |
C12b | 0.0175 (12) | 0.0256 (14) | 0.0319 (13) | −0.0061 (11) | 0.0038 (9) | −0.0025 (12) |
C13b | 0.0409 (17) | 0.0352 (17) | 0.0485 (17) | −0.0031 (13) | 0.0163 (13) | 0.0017 (14) |
C13a | 0.0296 (14) | 0.058 (2) | 0.0424 (16) | 0.0084 (15) | 0.0144 (12) | 0.0074 (16) |
C14a | 0.060 (2) | 0.079 (3) | 0.063 (2) | 0.021 (2) | −0.0121 (18) | 0.008 (2) |
C14b | 0.084 (3) | 0.101 (4) | 0.064 (3) | −0.020 (3) | −0.006 (2) | −0.013 (3) |
O3a | 0.0496 (14) | 0.0727 (19) | 0.0479 (13) | 0.0090 (13) | −0.0117 (10) | −0.0022 (13) |
O3b | 0.0614 (16) | 0.088 (2) | 0.0524 (15) | −0.0126 (16) | −0.0092 (12) | 0.0003 (15) |
O2b | 0.0311 (10) | 0.0244 (11) | 0.0495 (11) | −0.0007 (8) | 0.0063 (8) | 0.0093 (9) |
Na1—O1bi | 2.259 (2) | C5b—C6b | 1.358 (4) |
Na1—O2b | 2.270 (2) | C5b—C11b | 1.512 (4) |
Na1—O1bii | 2.290 (2) | C6b—C7b | 1.424 (4) |
Na1—O1a | 2.394 (2) | C6b—H6' | 0.9600 |
Na1—C12bi | 3.087 (3) | C6a—C7a | 1.415 (4) |
Na1—Na2 | 3.2853 (15) | C6a—H6 | 0.9600 |
Na1—Na1i | 3.6229 (13) | C7a—C8a | 1.410 (4) |
Na1—Na1iii | 3.6229 (13) | C7b—C8b | 1.421 (4) |
Na2—O2aiv | 2.276 (2) | C8b—C9b | 1.348 (4) |
Na2—O2av | 2.291 (2) | C8b—H8' | 0.9600 |
Na2—O1a | 2.328 (2) | C8a—C9a | 1.362 (4) |
Na2—O2b | 2.341 (2) | C8a—H8 | 0.9600 |
Na2—Na2iv | 3.5711 (13) | C9a—C10a | 1.410 (5) |
Na2—Na2vi | 3.5711 (13) | C9a—H9 | 0.9600 |
O1a—C12a | 1.248 (4) | C9b—C10b | 1.397 (6) |
O1b—C12b | 1.262 (3) | C9b—H9' | 0.9600 |
O1b—Na1iii | 2.259 (2) | C10b—O3b | 1.360 (4) |
O1b—Na1v | 2.290 (2) | C10a—O3a | 1.368 (3) |
O2a—C12a | 1.259 (3) | C11b—C13b | 1.521 (4) |
O2a—Na2vi | 2.276 (2) | C11b—C12b | 1.533 (4) |
O2a—Na2ii | 2.291 (2) | C11b—H11' | 0.9600 |
C1a—C10a | 1.361 (4) | C11a—C13a | 1.515 (4) |
C1a—C2a | 1.425 (4) | C11a—C12a | 1.539 (4) |
C1a—H1 | 0.9600 | C11a—H11 | 0.9600 |
C1b—C10b | 1.368 (5) | C12b—O2b | 1.240 (3) |
C1b—C2b | 1.425 (4) | C12b—Na1iii | 3.087 (3) |
C1b—H1' | 0.9600 | C13b—H13D | 0.9599 |
C2a—C3a | 1.398 (4) | C13b—H13E | 0.9599 |
C2a—C7a | 1.414 (4) | C13b—H13F | 0.9599 |
C2b—C3b | 1.402 (4) | C13a—H13A | 0.9599 |
C2b—C7b | 1.413 (4) | C13a—H13B | 0.9599 |
C3a—C4a | 1.365 (4) | C13a—H13C | 0.9599 |
C3a—H3 | 0.9600 | C14a—O3a | 1.422 (5) |
C3b—C4b | 1.377 (4) | C14a—H14A | 0.9599 |
C3b—H3' | 0.9600 | C14a—H14B | 0.9599 |
C4b—C5b | 1.406 (4) | C14a—H14C | 0.9599 |
C4b—H4' | 0.9600 | C14b—O3b | 1.419 (6) |
C4a—C5a | 1.404 (4) | C14b—H14D | 0.9599 |
C4a—H4 | 0.9600 | C14b—H14E | 0.9599 |
C5a—C6a | 1.367 (4) | C14b—H14F | 0.9599 |
C5a—C11a | 1.522 (3) | ||
O1bi—Na1—O2b | 99.73 (8) | C4a—C5a—C11a | 119.7 (2) |
O1bi—Na1—O1bii | 115.26 (7) | C6b—C5b—C4b | 118.1 (3) |
O2b—Na1—O1bii | 132.02 (8) | C6b—C5b—C11b | 122.3 (3) |
O1bi—Na1—O1a | 126.15 (9) | C4b—C5b—C11b | 119.6 (2) |
O2b—Na1—O1a | 90.38 (8) | C5b—C6b—C7b | 122.0 (3) |
O1bii—Na1—O1a | 93.94 (8) | C5b—C6b—H6' | 119.0 |
O1bi—Na1—C12bi | 20.77 (7) | C7b—C6b—H6' | 119.0 |
O2b—Na1—C12bi | 120.23 (8) | C5a—C6a—C7a | 121.8 (3) |
O1bii—Na1—C12bi | 96.23 (8) | C5a—C6a—H6 | 119.1 |
O1a—Na1—C12bi | 123.81 (8) | C7a—C6a—H6 | 119.1 |
O1bi—Na1—Na2 | 125.32 (7) | C8a—C7a—C2a | 118.8 (3) |
O2b—Na1—Na2 | 45.44 (5) | C8a—C7a—C6a | 122.2 (3) |
O1bii—Na1—Na2 | 118.99 (6) | C2a—C7a—C6a | 119.0 (3) |
O1a—Na1—Na2 | 45.08 (6) | C2b—C7b—C8b | 118.9 (3) |
C12bi—Na1—Na2 | 141.64 (6) | C2b—C7b—C6b | 119.1 (3) |
O1bi—Na1—Na1i | 79.76 (7) | C8b—C7b—C6b | 122.0 (3) |
O2b—Na1—Na1i | 157.05 (8) | C9b—C8b—C7b | 120.2 (3) |
O1bii—Na1—Na1i | 36.92 (5) | C9b—C8b—H8' | 119.9 |
O1a—Na1—Na1i | 108.59 (6) | C7b—C8b—H8' | 119.9 |
C12bi—Na1—Na1i | 59.75 (6) | C9a—C8a—C7a | 120.4 (3) |
Na2—Na1—Na1i | 150.03 (4) | C9a—C8a—H8 | 119.8 |
O1bi—Na1—Na1iii | 37.50 (6) | C7a—C8a—H8 | 119.8 |
O2b—Na1—Na1iii | 63.23 (6) | C8a—C9a—C10a | 121.0 (3) |
O1bii—Na1—Na1iii | 135.72 (7) | C8a—C9a—H9 | 119.5 |
O1a—Na1—Na1iii | 129.93 (7) | C10a—C9a—H9 | 119.5 |
C12bi—Na1—Na1iii | 57.23 (6) | C8b—C9b—C10b | 121.7 (3) |
Na2—Na1—Na1iii | 99.74 (4) | C8b—C9b—H9' | 119.2 |
Na1i—Na1—Na1iii | 109.98 (5) | C10b—C9b—H9' | 119.2 |
O2aiv—Na2—O2av | 116.65 (8) | O3b—C10b—C1b | 125.0 (4) |
O2aiv—Na2—O1a | 104.47 (8) | O3b—C10b—C9b | 114.9 (3) |
O2av—Na2—O1a | 129.53 (8) | C1b—C10b—C9b | 120.1 (3) |
O2aiv—Na2—O2b | 124.00 (9) | C1a—C10a—O3a | 125.3 (3) |
O2av—Na2—O2b | 89.96 (8) | C1a—C10a—C9a | 120.3 (3) |
O1a—Na2—O2b | 90.29 (7) | O3a—C10a—C9a | 114.4 (3) |
O2aiv—Na2—Na1 | 122.61 (7) | C5b—C11b—C13b | 112.7 (2) |
O2av—Na2—Na1 | 118.46 (6) | C5b—C11b—C12b | 109.2 (2) |
O1a—Na2—Na1 | 46.73 (5) | C13b—C11b—C12b | 112.0 (2) |
O2b—Na2—Na1 | 43.69 (5) | C5b—C11b—H11' | 107.5 |
O2aiv—Na2—Na2iv | 79.22 (7) | C13b—C11b—H11' | 107.5 |
O2av—Na2—Na2iv | 38.40 (5) | C12b—C11b—H11' | 107.5 |
O1a—Na2—Na2iv | 158.93 (8) | C13a—C11a—C5a | 113.3 (2) |
O2b—Na2—Na2iv | 104.97 (6) | C13a—C11a—C12a | 112.8 (2) |
Na1—Na2—Na2iv | 147.44 (4) | C5a—C11a—C12a | 109.7 (2) |
O2aiv—Na2—Na2vi | 38.72 (6) | C13a—C11a—H11 | 106.8 |
O2av—Na2—Na2vi | 141.19 (7) | C5a—C11a—H11 | 106.8 |
O1a—Na2—Na2vi | 66.30 (5) | C12a—C11a—H11 | 106.8 |
O2b—Na2—Na2vi | 127.93 (7) | O1a—C12a—O2a | 124.1 (3) |
Na1—Na2—Na2vi | 97.79 (4) | O1a—C12a—C11a | 119.4 (2) |
Na2iv—Na2—Na2vi | 112.39 (6) | O2a—C12a—C11a | 116.5 (2) |
C12a—O1a—Na2 | 143.82 (18) | O2b—C12b—O1b | 123.9 (2) |
C12a—O1a—Na1 | 115.34 (16) | O2b—C12b—C11b | 118.3 (2) |
Na2—O1a—Na1 | 88.18 (8) | O1b—C12b—C11b | 117.7 (2) |
C12b—O1b—Na1iii | 119.83 (18) | O2b—C12b—Na1iii | 88.50 (16) |
C12b—O1b—Na1v | 130.01 (17) | O1b—C12b—Na1iii | 39.41 (12) |
Na1iii—O1b—Na1v | 105.58 (8) | C11b—C12b—Na1iii | 147.21 (17) |
C12a—O2a—Na2vi | 124.91 (19) | C11b—C13b—H13D | 109.5 |
C12a—O2a—Na2ii | 128.30 (18) | C11b—C13b—H13E | 109.5 |
Na2vi—O2a—Na2ii | 102.88 (8) | H13D—C13b—H13E | 109.5 |
C10a—C1a—C2a | 119.9 (3) | C11b—C13b—H13F | 109.5 |
C10a—C1a—H1 | 120.1 | H13D—C13b—H13F | 109.5 |
C2a—C1a—H1 | 120.1 | H13E—C13b—H13F | 109.5 |
C10b—C1b—C2b | 120.1 (3) | C11a—C13a—H13A | 109.5 |
C10b—C1b—H1' | 119.9 | C11a—C13a—H13B | 109.5 |
C2b—C1b—H1' | 119.9 | H13A—C13a—H13B | 109.5 |
C3a—C2a—C7a | 118.2 (2) | C11a—C13a—H13C | 109.5 |
C3a—C2a—C1a | 122.2 (3) | H13A—C13a—H13C | 109.5 |
C7a—C2a—C1a | 119.6 (3) | H13B—C13a—H13C | 109.5 |
C3b—C2b—C7b | 118.3 (3) | O3a—C14a—H14A | 109.5 |
C3b—C2b—C1b | 122.7 (3) | O3a—C14a—H14B | 109.5 |
C7b—C2b—C1b | 119.0 (3) | H14A—C14a—H14B | 109.5 |
C4a—C3a—C2a | 121.2 (3) | O3a—C14a—H14C | 109.5 |
C4a—C3a—H3 | 119.4 | H14A—C14a—H14C | 109.5 |
C2a—C3a—H3 | 119.4 | H14B—C14a—H14C | 109.5 |
C4b—C3b—C2b | 120.7 (3) | O3b—C14b—H14D | 109.5 |
C4b—C3b—H3' | 119.7 | O3b—C14b—H14E | 109.5 |
C2b—C3b—H3' | 119.7 | H14D—C14b—H14E | 109.5 |
C3b—C4b—C5b | 121.8 (3) | O3b—C14b—H14F | 109.5 |
C3b—C4b—H4' | 119.1 | H14D—C14b—H14F | 109.5 |
C5b—C4b—H4' | 119.1 | H14E—C14b—H14F | 109.5 |
C3a—C4a—C5a | 121.5 (3) | C10a—O3a—C14a | 117.1 (3) |
C3a—C4a—H4 | 119.3 | C10b—O3b—C14b | 117.7 (3) |
C5a—C4a—H4 | 119.3 | C12b—O2b—Na1 | 146.59 (18) |
C6a—C5a—C4a | 118.0 (2) | C12b—O2b—Na2 | 119.85 (16) |
C6a—C5a—C11a | 122.2 (3) | Na1—O2b—Na2 | 90.87 (8) |
O1bi—Na1—Na2—O2aiv | 172.92 (10) | C5a—C6a—C7a—C2a | −1.6 (4) |
O2b—Na1—Na2—O2aiv | 106.93 (11) | C3b—C2b—C7b—C8b | −179.9 (3) |
O1bii—Na1—Na2—O2aiv | −14.96 (10) | C1b—C2b—C7b—C8b | −0.1 (4) |
O1a—Na1—Na2—O2aiv | −78.76 (10) | C3b—C2b—C7b—C6b | 1.4 (4) |
C12bi—Na1—Na2—O2aiv | −169.13 (11) | C1b—C2b—C7b—C6b | −178.9 (3) |
Na1i—Na1—Na2—O2aiv | −44.64 (14) | C5b—C6b—C7b—C2b | −0.5 (4) |
Na1iii—Na1—Na2—O2aiv | 142.78 (8) | C5b—C6b—C7b—C8b | −179.3 (3) |
O1bi—Na1—Na2—O2av | 10.63 (11) | C2b—C7b—C8b—C9b | 0.1 (5) |
O2b—Na1—Na2—O2av | −55.35 (10) | C6b—C7b—C8b—C9b | 178.9 (3) |
O1bii—Na1—Na2—O2av | −177.25 (9) | C2a—C7a—C8a—C9a | −4.0 (5) |
O1a—Na1—Na2—O2av | 118.96 (10) | C6a—C7a—C8a—C9a | 175.4 (3) |
C12bi—Na1—Na2—O2av | 28.59 (12) | C7a—C8a—C9a—C10a | 0.8 (6) |
Na1i—Na1—Na2—O2av | 153.08 (11) | C7b—C8b—C9b—C10b | 0.0 (5) |
Na1iii—Na1—Na2—O2av | −19.50 (8) | C2b—C1b—C10b—O3b | 179.7 (3) |
O1bi—Na1—Na2—O1a | −108.32 (11) | C2b—C1b—C10b—C9b | 0.1 (5) |
O2b—Na1—Na2—O1a | −174.31 (12) | C8b—C9b—C10b—O3b | −179.8 (3) |
O1bii—Na1—Na2—O1a | 63.80 (10) | C8b—C9b—C10b—C1b | −0.1 (5) |
C12bi—Na1—Na2—O1a | −90.37 (12) | C2a—C1a—C10a—O3a | 177.3 (3) |
Na1i—Na1—Na2—O1a | 34.12 (12) | C2a—C1a—C10a—C9a | −1.4 (5) |
Na1iii—Na1—Na2—O1a | −138.46 (9) | C8a—C9a—C10a—C1a | 1.9 (5) |
O1bi—Na1—Na2—O2b | 65.98 (11) | C8a—C9a—C10a—O3a | −177.0 (3) |
O1bii—Na1—Na2—O2b | −121.90 (10) | C6b—C5b—C11b—C13b | 44.3 (4) |
O1a—Na1—Na2—O2b | 174.31 (12) | C4b—C5b—C11b—C13b | −136.7 (3) |
C12bi—Na1—Na2—O2b | 83.94 (12) | C6b—C5b—C11b—C12b | −80.9 (3) |
Na1i—Na1—Na2—O2b | −151.57 (14) | C4b—C5b—C11b—C12b | 98.1 (3) |
Na1iii—Na1—Na2—O2b | 35.85 (8) | C6a—C5a—C11a—C13a | 37.7 (4) |
O1bi—Na1—Na2—Na2iv | 46.78 (14) | C4a—C5a—C11a—C13a | −142.3 (3) |
O2b—Na1—Na2—Na2iv | −19.20 (12) | C6a—C5a—C11a—C12a | −89.4 (3) |
O1bii—Na1—Na2—Na2iv | −141.09 (11) | C4a—C5a—C11a—C12a | 90.6 (3) |
O1a—Na1—Na2—Na2iv | 155.11 (13) | Na2—O1a—C12a—O2a | 14.9 (4) |
C12bi—Na1—Na2—Na2iv | 64.74 (15) | Na1—O1a—C12a—O2a | −111.2 (2) |
Na1i—Na1—Na2—Na2iv | −170.77 (10) | Na2—O1a—C12a—C11a | −165.6 (2) |
Na1iii—Na1—Na2—Na2iv | 16.65 (11) | Na1—O1a—C12a—C11a | 68.4 (3) |
O1bi—Na1—Na2—Na2vi | −155.01 (8) | Na2vi—O2a—C12a—O1a | −16.7 (3) |
O2b—Na1—Na2—Na2vi | 139.01 (9) | Na2ii—O2a—C12a—O1a | 137.1 (2) |
O1bii—Na1—Na2—Na2vi | 17.11 (8) | Na2vi—O2a—C12a—C11a | 163.68 (16) |
O1a—Na1—Na2—Na2vi | −46.69 (8) | Na2ii—O2a—C12a—C11a | −42.5 (3) |
C12bi—Na1—Na2—Na2vi | −137.05 (9) | C13a—C11a—C12a—O1a | −10.4 (3) |
Na1i—Na1—Na2—Na2vi | −12.56 (12) | C5a—C11a—C12a—O1a | 117.0 (3) |
Na1iii—Na1—Na2—Na2vi | 174.86 (5) | C13a—C11a—C12a—O2a | 169.3 (2) |
O2aiv—Na2—O1a—C12a | −11.6 (3) | C5a—C11a—C12a—O2a | −63.3 (3) |
O2av—Na2—O1a—C12a | 132.9 (3) | Na1iii—O1b—C12b—O2b | 29.7 (3) |
O2b—Na2—O1a—C12a | −136.9 (3) | Na1v—O1b—C12b—O2b | −122.6 (2) |
Na1—Na2—O1a—C12a | −133.0 (3) | Na1iii—O1b—C12b—C11b | −148.91 (18) |
Na2iv—Na2—O1a—C12a | 86.1 (4) | Na1v—O1b—C12b—C11b | 58.8 (3) |
Na2vi—Na2—O1a—C12a | −4.9 (3) | Na1v—O1b—C12b—Na1iii | −152.3 (3) |
O2aiv—Na2—O1a—Na1 | 121.44 (8) | C5b—C11b—C12b—O2b | −90.4 (3) |
O2av—Na2—O1a—Na1 | −94.11 (10) | C13b—C11b—C12b—O2b | 144.0 (2) |
O2b—Na2—O1a—Na1 | −3.93 (8) | C5b—C11b—C12b—O1b | 88.3 (3) |
Na2iv—Na2—O1a—Na1 | −140.94 (16) | C13b—C11b—C12b—O1b | −37.4 (3) |
Na2vi—Na2—O1a—Na1 | 128.07 (7) | C5b—C11b—C12b—Na1iii | 51.0 (4) |
O1bi—Na1—O1a—C12a | −102.1 (2) | C13b—C11b—C12b—Na1iii | −74.6 (4) |
O2b—Na1—O1a—C12a | 155.52 (19) | C1a—C10a—O3a—C14a | −7.4 (5) |
O1bii—Na1—O1a—C12a | 23.3 (2) | C9a—C10a—O3a—C14a | 171.3 (4) |
C12bi—Na1—O1a—C12a | −76.9 (2) | C1b—C10b—O3b—C14b | −5.2 (5) |
Na2—Na1—O1a—C12a | 151.5 (2) | C9b—C10b—O3b—C14b | 174.4 (4) |
Na1i—Na1—O1a—C12a | −11.3 (2) | O1b—C12b—O2b—Na1 | −37.5 (5) |
Na1iii—Na1—O1a—C12a | −150.06 (17) | C11b—C12b—O2b—Na1 | 141.1 (3) |
O1bi—Na1—O1a—Na2 | 106.42 (10) | Na1iii—C12b—O2b—Na1 | −19.1 (3) |
O2b—Na1—O1a—Na2 | 4.05 (8) | O1b—C12b—O2b—Na2 | 116.9 (2) |
O1bii—Na1—O1a—Na2 | −128.12 (8) | C11b—C12b—O2b—Na2 | −64.5 (3) |
C12bi—Na1—O1a—Na2 | 131.68 (9) | Na1iii—C12b—O2b—Na2 | 135.22 (13) |
Na1i—Na1—O1a—Na2 | −162.80 (6) | O1bi—Na1—O2b—C12b | 27.1 (3) |
Na1iii—Na1—O1a—Na2 | 58.47 (10) | O1bii—Na1—O2b—C12b | −110.4 (3) |
C10a—C1a—C2a—C3a | 178.7 (3) | O1a—Na1—O2b—C12b | 153.9 (3) |
C10a—C1a—C2a—C7a | −1.8 (4) | C12bi—Na1—O2b—C12b | 23.5 (4) |
C10b—C1b—C2b—C3b | 179.7 (3) | Na2—Na1—O2b—C12b | 158.0 (4) |
C10b—C1b—C2b—C7b | 0.0 (4) | Na1i—Na1—O2b—C12b | −59.6 (4) |
C7a—C2a—C3a—C4a | −3.0 (4) | Na1iii—Na1—O2b—C12b | 18.2 (3) |
C1a—C2a—C3a—C4a | 176.5 (3) | O1bi—Na1—O2b—Na2 | −130.87 (8) |
C7b—C2b—C3b—C4b | −0.5 (5) | O1bii—Na1—O2b—Na2 | 91.62 (11) |
C1b—C2b—C3b—C4b | 179.8 (3) | O1a—Na1—O2b—Na2 | −4.03 (8) |
C2b—C3b—C4b—C5b | −1.3 (5) | C12bi—Na1—O2b—Na2 | −134.42 (8) |
C2a—C3a—C4a—C5a | −1.6 (4) | Na1i—Na1—O2b—Na2 | 142.41 (15) |
C3a—C4a—C5a—C6a | 4.6 (4) | Na1iii—Na1—O2b—Na2 | −139.72 (8) |
C3a—C4a—C5a—C11a | −175.4 (3) | O2aiv—Na2—O2b—C12b | 90.2 (2) |
C3b—C4b—C5b—C6b | 2.1 (4) | O2av—Na2—O2b—C12b | −32.5 (2) |
C3b—C4b—C5b—C11b | −176.9 (3) | O1a—Na2—O2b—C12b | −162.1 (2) |
C4b—C5b—C6b—C7b | −1.2 (4) | Na1—Na2—O2b—C12b | −166.2 (2) |
C11b—C5b—C6b—C7b | 177.8 (3) | Na2iv—Na2—O2b—C12b | 3.2 (2) |
C4a—C5a—C6a—C7a | −3.0 (4) | Na2vi—Na2—O2b—C12b | 138.31 (19) |
C11a—C5a—C6a—C7a | 177.1 (3) | O2aiv—Na2—O2b—Na1 | −103.60 (10) |
C3a—C2a—C7a—C8a | −176.0 (3) | O2av—Na2—O2b—Na1 | 133.68 (8) |
C1a—C2a—C7a—C8a | 4.4 (4) | O1a—Na2—O2b—Na1 | 4.14 (8) |
C3a—C2a—C7a—C6a | 4.5 (4) | Na2iv—Na2—O2b—Na1 | 169.44 (6) |
C1a—C2a—C7a—C6a | −175.0 (3) | Na2vi—Na2—O2b—Na1 | −55.47 (10) |
C5a—C6a—C7a—C8a | 179.0 (3) |
Symmetry codes: (i) −x, y+1/2, −z; (ii) x, y+1, z; (iii) −x, y−1/2, −z; (iv) −x−1, y−1/2, −z; (v) x, y−1, z; (vi) −x−1, y+1/2, −z. |