Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803001193/bt6229sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803001193/bt6229Isup2.hkl |
CCDC reference: 204657
Key indicators
- Single-crystal X-ray study
- T = 160 K
- Mean (C-C) = 0.003 Å
- R factor = 0.036
- wR factor = 0.094
- Data-to-parameter ratio = 16.4
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level B:
CRYSS_02 Alert B The value of _exptl_crystal_size_min is > 0.6 Minimum crystal size given = 0.800
Author response: Crystals are difficult to handle and prone to damage on cutting, leading to poorer diffraction. Also, intensities are generally weak, so a larger crystal is preferred. Excellent R~int~ and final R values show there is no problem resulting from the crystal size. |
Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.00 From the CIF: _reflns_number_total 22410 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 23943 Completeness (_total/calc) 93.60% Alert C: < 95% complete PLAT_601 Alert C Structure Contains Solvent Accessible VOIDS of 50.00 A 3
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
2 Alert Level C = Please check
The compound was prepared as described by Armstrong et al. (2000), but essentially the same procedure and conditions on this occasion produced a different polymorph.
H atoms were placed geometrically and refined with a riding model (including free rotation about C—C bonds), and with Uiso = 1.5Ueq(C).
Data collection: SMART (Bruker, 2001); cell refinement: local programs; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.
[Li4Na4(C4H9O)8] | Z = 6 |
Mr = 704.62 | F(000) = 2304 |
Triclinic, P1 | Dx = 1.033 Mg m−3 |
a = 11.1917 (8) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 21.0007 (14) Å | Cell parameters from 28018 reflections |
c = 29.450 (2) Å | θ = 2.3–28.1° |
α = 82.560 (2)° | µ = 0.10 mm−1 |
β = 89.492 (2)° | T = 160 K |
γ = 82.033 (2)° | Block, colourless |
V = 6796.8 (8) Å3 | 0.82 × 0.80 × 0.80 mm |
Bruker SMART 1K CCD diffractometer | 22410 independent reflections |
Radiation source: fine-focus sealed tube | 15221 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
Detector resolution: 8.192 pixels mm-1 | θmax = 25.0°, θmin = 1.1° |
fine–slice ω scans | h = −13→12 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | k = −24→24 |
Tmin = 0.890, Tmax = 0.950 | l = −33→35 |
32571 measured reflections |
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)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.094 | w = 1/[σ2(Fo2) + (0.0515P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max = 0.001 |
22410 reflections | Δρmax = 0.18 e Å−3 |
1370 parameters | Δρmin = −0.20 e Å−3 |
0 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00064 (9) |
[Li4Na4(C4H9O)8] | γ = 82.033 (2)° |
Mr = 704.62 | V = 6796.8 (8) Å3 |
Triclinic, P1 | Z = 6 |
a = 11.1917 (8) Å | Mo Kα radiation |
b = 21.0007 (14) Å | µ = 0.10 mm−1 |
c = 29.450 (2) Å | T = 160 K |
α = 82.560 (2)° | 0.82 × 0.80 × 0.80 mm |
β = 89.492 (2)° |
Bruker SMART 1K CCD diffractometer | 22410 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | 15221 reflections with I > 2σ(I) |
Tmin = 0.890, Tmax = 0.950 | Rint = 0.017 |
32571 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 0 restraints |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 0.92 | Δρmax = 0.18 e Å−3 |
22410 reflections | Δρmin = −0.20 e Å−3 |
1370 parameters |
x | y | z | Uiso*/Ueq | ||
Na1A | 0.27825 (6) | 0.12605 (3) | 0.52557 (2) | 0.02994 (16) | |
Na2A | 0.23625 (6) | 0.24545 (3) | 0.58710 (2) | 0.03054 (16) | |
Na3A | 0.19978 (6) | 0.34956 (3) | 0.49392 (2) | 0.03224 (17) | |
Na4A | 0.24200 (6) | 0.22987 (3) | 0.43183 (2) | 0.03152 (17) | |
Li1A | 0.4477 (3) | 0.20472 (14) | 0.54334 (10) | 0.0295 (7) | |
Li2A | 0.4207 (3) | 0.28172 (14) | 0.47338 (10) | 0.0291 (7) | |
Li3A | 0.0599 (3) | 0.18779 (14) | 0.48759 (10) | 0.0302 (7) | |
Li4A | 0.0278 (3) | 0.27742 (14) | 0.53302 (10) | 0.0309 (7) | |
O1A | 0.42512 (10) | 0.19082 (5) | 0.48179 (4) | 0.0262 (3) | |
O2A | 0.38870 (10) | 0.29510 (5) | 0.53487 (4) | 0.0277 (3) | |
O3A | 0.37756 (10) | 0.15261 (5) | 0.58784 (4) | 0.0289 (3) | |
O4A | 0.31420 (10) | 0.32844 (6) | 0.42977 (4) | 0.0320 (3) | |
O5A | 0.17017 (10) | 0.13412 (5) | 0.45810 (4) | 0.0285 (3) | |
O6A | 0.09590 (10) | 0.33488 (5) | 0.56307 (4) | 0.0299 (3) | |
O7A | 0.08608 (10) | 0.18852 (5) | 0.55103 (4) | 0.0266 (3) | |
O8A | 0.05403 (10) | 0.27809 (5) | 0.46928 (4) | 0.0278 (3) | |
C1A | 0.51260 (15) | 0.15081 (9) | 0.45959 (6) | 0.0300 (4) | |
C2A | 0.63592 (17) | 0.17272 (11) | 0.46397 (8) | 0.0533 (6) | |
H2A | 0.6331 | 0.2176 | 0.4495 | 0.080* | |
H2B | 0.6966 | 0.1446 | 0.4488 | 0.080* | |
H2C | 0.6572 | 0.1700 | 0.4964 | 0.080* | |
C3A | 0.51917 (18) | 0.08045 (9) | 0.48084 (7) | 0.0420 (5) | |
H3A | 0.5360 | 0.0771 | 0.5137 | 0.063* | |
H3B | 0.5838 | 0.0539 | 0.4663 | 0.063* | |
H3C | 0.4420 | 0.0651 | 0.4761 | 0.063* | |
C4A | 0.48060 (19) | 0.15483 (10) | 0.40865 (6) | 0.0459 (5) | |
H4A | 0.4779 | 0.1997 | 0.3941 | 0.069* | |
H4B | 0.4016 | 0.1406 | 0.4056 | 0.069* | |
H4C | 0.5419 | 0.1267 | 0.3938 | 0.069* | |
C5A | 0.45000 (16) | 0.33756 (9) | 0.55673 (6) | 0.0322 (4) | |
C6A | 0.58615 (17) | 0.31852 (12) | 0.55196 (8) | 0.0585 (6) | |
H6A | 0.6095 | 0.2740 | 0.5667 | 0.088* | |
H6B | 0.6292 | 0.3480 | 0.5667 | 0.088* | |
H6C | 0.6069 | 0.3214 | 0.5194 | 0.088* | |
C7A | 0.4137 (2) | 0.40772 (9) | 0.53517 (8) | 0.0580 (6) | |
H7A | 0.3267 | 0.4200 | 0.5387 | 0.087* | |
H7B | 0.4334 | 0.4118 | 0.5025 | 0.087* | |
H7C | 0.4576 | 0.4364 | 0.5504 | 0.087* | |
C8A | 0.41895 (18) | 0.33189 (10) | 0.60710 (6) | 0.0427 (5) | |
H8A | 0.4409 | 0.2869 | 0.6211 | 0.064* | |
H8B | 0.3321 | 0.3449 | 0.6105 | 0.064* | |
H8C | 0.4637 | 0.3602 | 0.6223 | 0.064* | |
C9A | 0.44492 (16) | 0.11032 (9) | 0.62220 (6) | 0.0311 (4) | |
C10A | 0.4341 (2) | 0.03970 (9) | 0.61722 (7) | 0.0500 (6) | |
H10A | 0.4612 | 0.0305 | 0.5867 | 0.075* | |
H10B | 0.3498 | 0.0325 | 0.6212 | 0.075* | |
H10C | 0.4844 | 0.0109 | 0.6406 | 0.075* | |
C11A | 0.4006 (2) | 0.12506 (11) | 0.66933 (6) | 0.0567 (6) | |
H11A | 0.4101 | 0.1698 | 0.6729 | 0.085* | |
H11B | 0.4478 | 0.0953 | 0.6931 | 0.085* | |
H11C | 0.3152 | 0.1195 | 0.6723 | 0.085* | |
C12A | 0.57846 (17) | 0.11849 (10) | 0.61831 (7) | 0.0467 (5) | |
H12A | 0.5881 | 0.1633 | 0.6216 | 0.070* | |
H12B | 0.6083 | 0.1084 | 0.5883 | 0.070* | |
H12C | 0.6245 | 0.0890 | 0.6425 | 0.070* | |
C13A | 0.35801 (17) | 0.37006 (9) | 0.39437 (6) | 0.0364 (5) | |
C14A | 0.3199 (2) | 0.35409 (12) | 0.34793 (7) | 0.0627 (7) | |
H14A | 0.3495 | 0.3086 | 0.3452 | 0.094* | |
H14B | 0.3542 | 0.3821 | 0.3234 | 0.094* | |
H14C | 0.2317 | 0.3614 | 0.3454 | 0.094* | |
C15A | 0.3088 (2) | 0.44069 (10) | 0.39872 (7) | 0.0542 (6) | |
H15A | 0.3317 | 0.4511 | 0.4287 | 0.081* | |
H15B | 0.2207 | 0.4470 | 0.3958 | 0.081* | |
H15C | 0.3426 | 0.4693 | 0.3745 | 0.081* | |
C16A | 0.49611 (18) | 0.36204 (11) | 0.39680 (8) | 0.0572 (6) | |
H16A | 0.5288 | 0.3168 | 0.3945 | 0.086* | |
H16B | 0.5215 | 0.3739 | 0.4260 | 0.086* | |
H16C | 0.5264 | 0.3903 | 0.3714 | 0.086* | |
C17A | 0.12795 (15) | 0.08548 (8) | 0.43669 (6) | 0.0301 (4) | |
C18A | 0.19008 (18) | 0.01871 (9) | 0.45761 (8) | 0.0491 (6) | |
H18A | 0.1761 | 0.0129 | 0.4907 | 0.074* | |
H18B | 0.2770 | 0.0155 | 0.4519 | 0.074* | |
H18C | 0.1569 | −0.0150 | 0.4437 | 0.074* | |
C19A | 0.15345 (19) | 0.09469 (11) | 0.38553 (7) | 0.0509 (6) | |
H19A | 0.1153 | 0.1377 | 0.3720 | 0.076* | |
H19B | 0.1207 | 0.0613 | 0.3710 | 0.076* | |
H19C | 0.2408 | 0.0910 | 0.3807 | 0.076* | |
C20A | −0.00817 (16) | 0.08851 (9) | 0.44333 (7) | 0.0381 (5) | |
H20A | −0.0485 | 0.1313 | 0.4303 | 0.057* | |
H20B | −0.0257 | 0.0811 | 0.4761 | 0.057* | |
H20C | −0.0377 | 0.0550 | 0.4279 | 0.057* | |
C21A | 0.02498 (16) | 0.38064 (9) | 0.58616 (6) | 0.0333 (4) | |
C22A | 0.0429 (2) | 0.44860 (10) | 0.56554 (9) | 0.0767 (8) | |
H22A | 0.0206 | 0.4552 | 0.5330 | 0.115* | |
H22B | 0.1278 | 0.4542 | 0.5688 | 0.115* | |
H22C | −0.0080 | 0.4803 | 0.5815 | 0.115* | |
C23A | 0.0585 (2) | 0.37104 (12) | 0.63675 (7) | 0.0621 (7) | |
H23A | 0.0489 | 0.3268 | 0.6501 | 0.093* | |
H23B | 0.0057 | 0.4022 | 0.6525 | 0.093* | |
H23C | 0.1426 | 0.3779 | 0.6402 | 0.093* | |
C24A | −0.10906 (18) | 0.37363 (11) | 0.58222 (8) | 0.0591 (6) | |
H24A | −0.1220 | 0.3299 | 0.5956 | 0.089* | |
H24B | −0.1335 | 0.3808 | 0.5499 | 0.089* | |
H24C | −0.1574 | 0.4057 | 0.5987 | 0.089* | |
C25A | 0.02105 (15) | 0.15338 (8) | 0.58463 (6) | 0.0293 (4) | |
C26A | −0.11301 (17) | 0.16425 (11) | 0.57124 (8) | 0.0521 (6) | |
H26A | −0.1229 | 0.1485 | 0.5418 | 0.078* | |
H26B | −0.1435 | 0.2106 | 0.5686 | 0.078* | |
H26C | −0.1584 | 0.1405 | 0.5948 | 0.078* | |
C27A | 0.0352 (2) | 0.17601 (10) | 0.63121 (6) | 0.0462 (5) | |
H27A | 0.1201 | 0.1668 | 0.6408 | 0.069* | |
H27B | −0.0139 | 0.1530 | 0.6538 | 0.069* | |
H27C | 0.0084 | 0.2228 | 0.6290 | 0.069* | |
C28A | 0.06718 (18) | 0.08103 (9) | 0.58835 (7) | 0.0414 (5) | |
H28A | 0.1524 | 0.0734 | 0.5976 | 0.062* | |
H28B | 0.0587 | 0.0659 | 0.5586 | 0.062* | |
H28C | 0.0201 | 0.0572 | 0.6112 | 0.062* | |
C29A | −0.03236 (16) | 0.31146 (9) | 0.43645 (6) | 0.0321 (4) | |
C30A | −0.15738 (18) | 0.29664 (12) | 0.45097 (9) | 0.0663 (7) | |
H30A | −0.1774 | 0.3125 | 0.4804 | 0.099* | |
H30B | −0.1585 | 0.2497 | 0.4542 | 0.099* | |
H30C | −0.2168 | 0.3182 | 0.4277 | 0.099* | |
C31A | −0.0296 (2) | 0.38421 (9) | 0.43261 (7) | 0.0517 (6) | |
H31A | −0.0470 | 0.3989 | 0.4625 | 0.078* | |
H31B | −0.0905 | 0.4067 | 0.4102 | 0.078* | |
H31C | 0.0505 | 0.3938 | 0.4226 | 0.078* | |
C32A | −0.0041 (2) | 0.28955 (11) | 0.38956 (7) | 0.0578 (6) | |
H32A | 0.0003 | 0.2423 | 0.3920 | 0.087* | |
H32B | 0.0733 | 0.3023 | 0.3789 | 0.087* | |
H32C | −0.0680 | 0.3100 | 0.3677 | 0.087* | |
Na1B | 0.00865 (6) | 0.12145 (4) | 0.24046 (2) | 0.04150 (19) | |
Na2B | 0.14025 (6) | 0.17822 (3) | 0.14684 (2) | 0.03725 (18) | |
Na3B | −0.10471 (6) | 0.17667 (3) | 0.08822 (2) | 0.03262 (17) | |
Na4B | −0.23747 (6) | 0.12154 (3) | 0.18133 (2) | 0.03135 (17) | |
Li1B | −0.0784 (3) | 0.04832 (14) | 0.12890 (10) | 0.0328 (7) | |
Li2B | 0.1042 (3) | 0.04957 (15) | 0.17178 (10) | 0.0344 (7) | |
Li3B | −0.1596 (3) | 0.22961 (15) | 0.21131 (10) | 0.0361 (7) | |
Li4B | −0.0622 (3) | 0.27144 (15) | 0.14189 (10) | 0.0353 (7) | |
O1B | −0.05381 (10) | 0.03884 (6) | 0.19296 (4) | 0.0321 (3) | |
O2B | 0.06214 (10) | 0.08634 (6) | 0.11086 (4) | 0.0298 (3) | |
O3B | 0.18955 (10) | 0.09469 (6) | 0.20598 (4) | 0.0374 (3) | |
O4B | −0.22261 (10) | 0.09307 (6) | 0.10757 (4) | 0.0314 (3) | |
O5B | −0.19235 (11) | 0.15898 (6) | 0.25008 (4) | 0.0354 (3) | |
O6B | 0.02971 (11) | 0.25200 (6) | 0.09264 (4) | 0.0347 (3) | |
O7B | 0.00447 (11) | 0.23987 (6) | 0.20064 (4) | 0.0364 (3) | |
O8B | −0.20859 (10) | 0.23396 (5) | 0.14901 (4) | 0.0300 (3) | |
C1B | −0.07833 (19) | −0.01830 (10) | 0.22023 (7) | 0.0453 (5) | |
C2B | −0.0286 (2) | −0.07708 (10) | 0.19672 (9) | 0.0694 (7) | |
H2D | −0.0706 | −0.0750 | 0.1674 | 0.104* | |
H2E | −0.0413 | −0.1169 | 0.2164 | 0.104* | |
H2F | 0.0579 | −0.0770 | 0.1913 | 0.104* | |
C3B | −0.0176 (2) | −0.02411 (13) | 0.26710 (8) | 0.0769 (8) | |
H3D | −0.0531 | 0.0118 | 0.2833 | 0.115* | |
H3E | 0.0690 | −0.0225 | 0.2631 | 0.115* | |
H3F | −0.0298 | −0.0654 | 0.2850 | 0.115* | |
C4B | −0.2144 (2) | −0.01698 (11) | 0.22624 (9) | 0.0693 (7) | |
H4D | −0.2461 | 0.0191 | 0.2430 | 0.104* | |
H4E | −0.2307 | −0.0579 | 0.2435 | 0.104* | |
H4F | −0.2537 | −0.0112 | 0.1961 | 0.104* | |
C5B | 0.13034 (16) | 0.06861 (9) | 0.07273 (6) | 0.0342 (4) | |
C6B | 0.1583 (2) | −0.00502 (10) | 0.07635 (8) | 0.0567 (6) | |
H6D | 0.0827 | −0.0236 | 0.0764 | 0.085* | |
H6E | 0.2030 | −0.0218 | 0.1048 | 0.085* | |
H6F | 0.2071 | −0.0170 | 0.0502 | 0.085* | |
C7B | 0.05991 (19) | 0.09397 (11) | 0.02823 (6) | 0.0513 (6) | |
H7D | 0.0441 | 0.1414 | 0.0250 | 0.077* | |
H7E | −0.0168 | 0.0764 | 0.0290 | 0.077* | |
H7F | 0.1074 | 0.0803 | 0.0022 | 0.077* | |
C8B | 0.24854 (17) | 0.09768 (11) | 0.07070 (7) | 0.0500 (6) | |
H8D | 0.2308 | 0.1451 | 0.0668 | 0.075* | |
H8E | 0.2964 | 0.0838 | 0.0448 | 0.075* | |
H8F | 0.2942 | 0.0828 | 0.0992 | 0.075* | |
C9B | 0.30542 (17) | 0.06687 (10) | 0.22165 (7) | 0.0430 (5) | |
C10B | 0.3115 (2) | 0.05923 (15) | 0.27388 (8) | 0.0804 (9) | |
H10D | 0.2525 | 0.0315 | 0.2865 | 0.121* | |
H10E | 0.2932 | 0.1019 | 0.2843 | 0.121* | |
H10F | 0.3927 | 0.0394 | 0.2843 | 0.121* | |
C11B | 0.39776 (18) | 0.11024 (11) | 0.20215 (8) | 0.0582 (6) | |
H11D | 0.3926 | 0.1163 | 0.1686 | 0.087* | |
H11E | 0.4791 | 0.0897 | 0.2119 | 0.087* | |
H11F | 0.3807 | 0.1525 | 0.2134 | 0.087* | |
C12B | 0.3388 (2) | 0.00038 (11) | 0.20504 (9) | 0.0645 (7) | |
H12D | 0.2807 | −0.0284 | 0.2169 | 0.097* | |
H12E | 0.4200 | −0.0185 | 0.2161 | 0.097* | |
H12F | 0.3372 | 0.0056 | 0.1715 | 0.097* | |
C13B | −0.29259 (16) | 0.06235 (10) | 0.07999 (7) | 0.0392 (5) | |
C14B | −0.41629 (19) | 0.05794 (14) | 0.10060 (10) | 0.0831 (9) | |
H14D | −0.4589 | 0.1017 | 0.1018 | 0.125* | |
H14E | −0.4074 | 0.0345 | 0.1317 | 0.125* | |
H14F | −0.4625 | 0.0347 | 0.0817 | 0.125* | |
C15B | −0.3064 (2) | 0.10065 (13) | 0.03238 (8) | 0.0811 (9) | |
H15D | −0.2265 | 0.1034 | 0.0190 | 0.122* | |
H15E | −0.3477 | 0.1444 | 0.0345 | 0.122* | |
H15F | −0.3539 | 0.0788 | 0.0130 | 0.122* | |
C16B | −0.23146 (19) | −0.00612 (10) | 0.07549 (8) | 0.0555 (6) | |
H16D | −0.1513 | −0.0041 | 0.0622 | 0.083* | |
H16E | −0.2804 | −0.0264 | 0.0556 | 0.083* | |
H16F | −0.2234 | −0.0318 | 0.1058 | 0.083* | |
C17B | −0.25939 (17) | 0.16482 (11) | 0.29043 (6) | 0.0415 (5) | |
C18B | −0.2838 (3) | 0.23578 (14) | 0.29815 (10) | 0.0899 (10) | |
H18D | −0.3337 | 0.2606 | 0.2729 | 0.135* | |
H18E | −0.2071 | 0.2531 | 0.2993 | 0.135* | |
H18F | −0.3264 | 0.2393 | 0.3271 | 0.135* | |
C19B | −0.1902 (2) | 0.12628 (17) | 0.33107 (7) | 0.0934 (11) | |
H19D | −0.1112 | 0.1410 | 0.3331 | 0.140* | |
H19E | −0.1789 | 0.0802 | 0.3273 | 0.140* | |
H19F | −0.2354 | 0.1327 | 0.3591 | 0.140* | |
C20B | −0.3791 (2) | 0.14055 (14) | 0.28630 (7) | 0.0715 (8) | |
H20D | −0.4224 | 0.1640 | 0.2590 | 0.107* | |
H20E | −0.4273 | 0.1478 | 0.3136 | 0.107* | |
H20F | −0.3654 | 0.0941 | 0.2836 | 0.107* | |
C21B | 0.06853 (18) | 0.30185 (9) | 0.06205 (6) | 0.0389 (5) | |
C22B | 0.0347 (2) | 0.29517 (12) | 0.01315 (7) | 0.0679 (7) | |
H22D | −0.0526 | 0.2951 | 0.0109 | 0.102* | |
H22E | 0.0769 | 0.2544 | 0.0046 | 0.102* | |
H22F | 0.0579 | 0.3317 | −0.0076 | 0.102* | |
C23B | 0.20601 (19) | 0.29939 (11) | 0.06531 (8) | 0.0562 (6) | |
H23D | 0.2286 | 0.3050 | 0.0965 | 0.084* | |
H23E | 0.2317 | 0.3342 | 0.0436 | 0.084* | |
H23F | 0.2455 | 0.2574 | 0.0580 | 0.084* | |
C24B | 0.0089 (2) | 0.36802 (10) | 0.07358 (9) | 0.0654 (7) | |
H24D | −0.0790 | 0.3705 | 0.0714 | 0.098* | |
H24E | 0.0359 | 0.4025 | 0.0519 | 0.098* | |
H24F | 0.0317 | 0.3733 | 0.1048 | 0.098* | |
C25B | 0.06754 (18) | 0.27632 (10) | 0.22750 (7) | 0.0424 (5) | |
C26B | 0.0988 (2) | 0.23734 (12) | 0.27413 (7) | 0.0638 (7) | |
H26D | 0.1513 | 0.1971 | 0.2701 | 0.096* | |
H26E | 0.0246 | 0.2270 | 0.2895 | 0.096* | |
H26F | 0.1408 | 0.2629 | 0.2928 | 0.096* | |
C27B | −0.0105 (2) | 0.33986 (12) | 0.23315 (9) | 0.0759 (8) | |
H27D | −0.0289 | 0.3649 | 0.2030 | 0.114* | |
H27E | 0.0329 | 0.3648 | 0.2518 | 0.114* | |
H27F | −0.0857 | 0.3310 | 0.2483 | 0.114* | |
C28B | 0.18488 (19) | 0.29091 (12) | 0.20412 (8) | 0.0600 (7) | |
H28D | 0.2355 | 0.2501 | 0.2000 | 0.090* | |
H28E | 0.2280 | 0.3154 | 0.2232 | 0.090* | |
H28F | 0.1664 | 0.3165 | 0.1742 | 0.090* | |
C29B | −0.32008 (17) | 0.27085 (9) | 0.13333 (6) | 0.0359 (5) | |
C30B | −0.42457 (17) | 0.23410 (11) | 0.14828 (8) | 0.0538 (6) | |
H30D | −0.4262 | 0.2261 | 0.1818 | 0.081* | |
H30E | −0.4143 | 0.1926 | 0.1359 | 0.081* | |
H30F | −0.5006 | 0.2599 | 0.1368 | 0.081* | |
C31B | −0.3351 (2) | 0.33415 (11) | 0.15402 (10) | 0.0748 (8) | |
H31D | −0.3362 | 0.3248 | 0.1875 | 0.112* | |
H31E | −0.4111 | 0.3605 | 0.1431 | 0.112* | |
H31F | −0.2676 | 0.3580 | 0.1448 | 0.112* | |
C32B | −0.3218 (2) | 0.28456 (13) | 0.08140 (7) | 0.0692 (7) | |
H32D | −0.2543 | 0.3078 | 0.0712 | 0.104* | |
H32E | −0.3980 | 0.3112 | 0.0711 | 0.104* | |
H32F | −0.3142 | 0.2435 | 0.0684 | 0.104* | |
Na1C | 0.53093 (6) | 0.36749 (3) | 0.75100 (2) | 0.03415 (17) | |
Na2C | 0.53576 (6) | 0.33844 (3) | 0.91121 (2) | 0.03200 (17) | |
Na3C | 0.50425 (6) | 0.46293 (3) | 0.83123 (2) | 0.03108 (17) | |
Na4C | 0.56458 (6) | 0.24296 (3) | 0.83135 (2) | 0.02946 (16) | |
Li1C | 0.3248 (3) | 0.39729 (14) | 0.80142 (10) | 0.0299 (7) | |
Li2C | 0.3481 (3) | 0.30543 (14) | 0.86172 (10) | 0.0301 (7) | |
Li3C | 0.7407 (3) | 0.31949 (14) | 0.80129 (10) | 0.0296 (7) | |
Li4C | 0.7223 (3) | 0.38860 (15) | 0.86155 (10) | 0.0316 (7) | |
O1C | 0.37459 (10) | 0.30814 (5) | 0.79798 (4) | 0.0271 (3) | |
O2C | 0.35151 (10) | 0.39472 (5) | 0.86558 (4) | 0.0267 (3) | |
O3C | 0.39797 (10) | 0.45642 (5) | 0.76361 (4) | 0.0298 (3) | |
O4C | 0.45345 (10) | 0.24726 (5) | 0.89833 (4) | 0.0298 (3) | |
O5C | 0.66358 (10) | 0.27477 (6) | 0.76361 (4) | 0.0283 (3) | |
O6C | 0.62053 (10) | 0.43354 (6) | 0.89876 (4) | 0.0314 (3) | |
O7C | 0.71967 (10) | 0.29793 (5) | 0.86510 (4) | 0.0258 (3) | |
O8C | 0.69110 (10) | 0.40991 (5) | 0.79765 (4) | 0.0284 (3) | |
C1C | 0.31129 (15) | 0.27032 (9) | 0.77280 (6) | 0.0300 (4) | |
C2C | 0.17769 (17) | 0.28002 (11) | 0.78600 (8) | 0.0571 (6) | |
H2G | 0.1448 | 0.3260 | 0.7790 | 0.086* | |
H2H | 0.1700 | 0.2661 | 0.8188 | 0.086* | |
H2I | 0.1330 | 0.2542 | 0.7686 | 0.086* | |
C3C | 0.32294 (19) | 0.29108 (10) | 0.72180 (6) | 0.0454 (5) | |
H3G | 0.2914 | 0.3372 | 0.7146 | 0.068* | |
H3H | 0.2769 | 0.2655 | 0.7047 | 0.068* | |
H3I | 0.4081 | 0.2840 | 0.7132 | 0.068* | |
C4C | 0.36115 (18) | 0.19862 (9) | 0.78360 (7) | 0.0418 (5) | |
H4G | 0.4451 | 0.1916 | 0.7735 | 0.063* | |
H4H | 0.3128 | 0.1729 | 0.7675 | 0.063* | |
H4I | 0.3576 | 0.1853 | 0.8167 | 0.063* | |
C5C | 0.26451 (15) | 0.42966 (9) | 0.89155 (6) | 0.0301 (4) | |
C6C | 0.13912 (17) | 0.41542 (12) | 0.87979 (8) | 0.0604 (7) | |
H6G | 0.1243 | 0.4267 | 0.8468 | 0.091* | |
H6H | 0.0783 | 0.4412 | 0.8965 | 0.091* | |
H6I | 0.1343 | 0.3692 | 0.8885 | 0.091* | |
C7C | 0.2688 (2) | 0.50197 (9) | 0.88069 (7) | 0.0515 (6) | |
H7G | 0.2563 | 0.5152 | 0.8477 | 0.077* | |
H7H | 0.3477 | 0.5117 | 0.8898 | 0.077* | |
H7I | 0.2052 | 0.5257 | 0.8976 | 0.077* | |
C8C | 0.28855 (19) | 0.40976 (11) | 0.94251 (6) | 0.0493 (6) | |
H8G | 0.3681 | 0.4199 | 0.9504 | 0.074* | |
H8H | 0.2867 | 0.3631 | 0.9500 | 0.074* | |
H8I | 0.2264 | 0.4335 | 0.9600 | 0.074* | |
C9C | 0.33197 (16) | 0.50041 (9) | 0.72992 (6) | 0.0311 (4) | |
C10C | 0.36993 (19) | 0.48453 (10) | 0.68206 (6) | 0.0463 (5) | |
H10G | 0.4554 | 0.4888 | 0.6776 | 0.069* | |
H10H | 0.3213 | 0.5146 | 0.6589 | 0.069* | |
H10I | 0.3573 | 0.4400 | 0.6791 | 0.069* | |
C11C | 0.3535 (2) | 0.56948 (9) | 0.73409 (7) | 0.0518 (6) | |
H11G | 0.4389 | 0.5734 | 0.7288 | 0.078* | |
H11H | 0.3314 | 0.5797 | 0.7649 | 0.078* | |
H11I | 0.3039 | 0.5997 | 0.7113 | 0.078* | |
C12C | 0.19679 (17) | 0.49620 (11) | 0.73511 (7) | 0.0499 (6) | |
H12G | 0.1703 | 0.5073 | 0.7652 | 0.075* | |
H12H | 0.1820 | 0.4520 | 0.7322 | 0.075* | |
H12I | 0.1517 | 0.5266 | 0.7111 | 0.075* | |
C13C | 0.41264 (16) | 0.20034 (9) | 0.93113 (6) | 0.0336 (4) | |
C14C | 0.48028 (19) | 0.13345 (9) | 0.92656 (7) | 0.0466 (5) | |
H14G | 0.4656 | 0.1222 | 0.8960 | 0.070* | |
H14H | 0.4518 | 0.1014 | 0.9498 | 0.070* | |
H14I | 0.5669 | 0.1337 | 0.9309 | 0.070* | |
C15C | 0.43236 (18) | 0.21696 (10) | 0.97928 (6) | 0.0450 (5) | |
H15G | 0.5182 | 0.2191 | 0.9840 | 0.068* | |
H15H | 0.4061 | 0.1834 | 1.0020 | 0.068* | |
H15I | 0.3854 | 0.2590 | 0.9828 | 0.068* | |
C16C | 0.27636 (17) | 0.19932 (11) | 0.92430 (7) | 0.0517 (6) | |
H16G | 0.2622 | 0.1870 | 0.8940 | 0.078* | |
H16H | 0.2324 | 0.2425 | 0.9265 | 0.078* | |
H16I | 0.2480 | 0.1678 | 0.9480 | 0.078* | |
C17C | 0.73400 (15) | 0.24135 (9) | 0.73208 (6) | 0.0295 (4) | |
C18C | 0.71948 (18) | 0.16942 (9) | 0.73969 (7) | 0.0449 (5) | |
H18G | 0.6350 | 0.1646 | 0.7347 | 0.067* | |
H18H | 0.7436 | 0.1512 | 0.7711 | 0.067* | |
H18I | 0.7706 | 0.1464 | 0.7181 | 0.067* | |
C19C | 0.69537 (18) | 0.26920 (11) | 0.68314 (6) | 0.0465 (5) | |
H19G | 0.7041 | 0.3154 | 0.6780 | 0.070* | |
H19H | 0.6109 | 0.2640 | 0.6784 | 0.070* | |
H19I | 0.7463 | 0.2461 | 0.6616 | 0.070* | |
C20C | 0.86795 (15) | 0.24820 (10) | 0.73845 (6) | 0.0389 (5) | |
H20G | 0.8785 | 0.2941 | 0.7326 | 0.058* | |
H20H | 0.9169 | 0.2240 | 0.7169 | 0.058* | |
H20I | 0.8936 | 0.2309 | 0.7699 | 0.058* | |
C21C | 0.66517 (16) | 0.46796 (9) | 0.93136 (6) | 0.0342 (5) | |
C22C | 0.80242 (17) | 0.46526 (11) | 0.92646 (8) | 0.0547 (6) | |
H22G | 0.8405 | 0.4199 | 0.9308 | 0.082* | |
H22H | 0.8334 | 0.4885 | 0.9496 | 0.082* | |
H22I | 0.8210 | 0.4856 | 0.8959 | 0.082* | |
C23C | 0.6074 (2) | 0.53875 (9) | 0.92419 (7) | 0.0512 (6) | |
H23G | 0.6251 | 0.5583 | 0.8933 | 0.077* | |
H23H | 0.6402 | 0.5623 | 0.9468 | 0.077* | |
H23I | 0.5199 | 0.5411 | 0.9279 | 0.077* | |
C24C | 0.63802 (19) | 0.43766 (11) | 0.97982 (6) | 0.0489 (6) | |
H24G | 0.6762 | 0.3924 | 0.9847 | 0.073* | |
H24H | 0.5506 | 0.4394 | 0.9835 | 0.073* | |
H24I | 0.6699 | 0.4618 | 1.0022 | 0.073* | |
C25C | 0.80542 (15) | 0.25309 (8) | 0.89205 (6) | 0.0284 (4) | |
C26C | 0.80823 (19) | 0.18512 (9) | 0.87815 (7) | 0.0481 (5) | |
H26G | 0.8238 | 0.1866 | 0.8453 | 0.072* | |
H26H | 0.7303 | 0.1699 | 0.8850 | 0.072* | |
H26I | 0.8724 | 0.1554 | 0.8953 | 0.072* | |
C27C | 0.93056 (16) | 0.27388 (11) | 0.88503 (7) | 0.0507 (6) | |
H27G | 0.9300 | 0.3170 | 0.8944 | 0.076* | |
H27H | 0.9520 | 0.2752 | 0.8526 | 0.076* | |
H27I | 0.9899 | 0.2427 | 0.9036 | 0.076* | |
C28C | 0.77351 (18) | 0.25031 (10) | 0.94238 (6) | 0.0432 (5) | |
H28G | 0.7712 | 0.2935 | 0.9518 | 0.065* | |
H28H | 0.8345 | 0.2198 | 0.9606 | 0.065* | |
H28I | 0.6943 | 0.2358 | 0.9472 | 0.065* | |
C29C | 0.75500 (16) | 0.45559 (9) | 0.77207 (6) | 0.0332 (4) | |
C30C | 0.7394 (2) | 0.45327 (11) | 0.72084 (7) | 0.0520 (6) | |
H30G | 0.6539 | 0.4648 | 0.7124 | 0.078* | |
H30H | 0.7680 | 0.4094 | 0.7138 | 0.078* | |
H30I | 0.7862 | 0.4842 | 0.7035 | 0.078* | |
C31C | 0.88954 (17) | 0.43959 (12) | 0.78448 (8) | 0.0587 (6) | |
H31G | 0.9005 | 0.4409 | 0.8173 | 0.088* | |
H31H | 0.9340 | 0.4715 | 0.7670 | 0.088* | |
H31I | 0.9202 | 0.3962 | 0.7771 | 0.088* | |
C32C | 0.7084 (2) | 0.52409 (9) | 0.78242 (8) | 0.0523 (6) | |
H32G | 0.6239 | 0.5355 | 0.7726 | 0.078* | |
H32H | 0.7568 | 0.5549 | 0.7659 | 0.078* | |
H32I | 0.7146 | 0.5257 | 0.8154 | 0.078* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Na1A | 0.0307 (4) | 0.0313 (4) | 0.0286 (4) | −0.0059 (3) | −0.0027 (3) | −0.0050 (3) |
Na2A | 0.0307 (4) | 0.0297 (4) | 0.0308 (4) | −0.0024 (3) | 0.0006 (3) | −0.0042 (3) |
Na3A | 0.0325 (4) | 0.0321 (4) | 0.0321 (4) | −0.0065 (3) | 0.0032 (3) | −0.0019 (3) |
Na4A | 0.0331 (4) | 0.0322 (4) | 0.0304 (4) | −0.0111 (3) | 0.0011 (3) | −0.0015 (3) |
Li1A | 0.0289 (16) | 0.0302 (17) | 0.0291 (16) | −0.0030 (13) | 0.0013 (13) | −0.0036 (13) |
Li2A | 0.0287 (16) | 0.0319 (17) | 0.0273 (16) | −0.0076 (13) | 0.0025 (13) | −0.0026 (13) |
Li3A | 0.0288 (16) | 0.0295 (17) | 0.0334 (17) | −0.0089 (13) | 0.0001 (13) | −0.0034 (13) |
Li4A | 0.0296 (17) | 0.0298 (17) | 0.0342 (17) | −0.0068 (13) | 0.0015 (13) | −0.0049 (14) |
O1A | 0.0264 (7) | 0.0276 (7) | 0.0252 (6) | −0.0034 (5) | 0.0023 (5) | −0.0061 (5) |
O2A | 0.0295 (7) | 0.0274 (7) | 0.0278 (7) | −0.0072 (5) | −0.0018 (5) | −0.0056 (5) |
O3A | 0.0308 (7) | 0.0297 (7) | 0.0244 (6) | −0.0019 (6) | −0.0024 (5) | 0.0011 (5) |
O4A | 0.0353 (7) | 0.0331 (7) | 0.0264 (7) | −0.0105 (6) | 0.0033 (5) | 0.0064 (6) |
O5A | 0.0317 (7) | 0.0264 (7) | 0.0308 (7) | −0.0099 (5) | 0.0002 (5) | −0.0097 (5) |
O6A | 0.0296 (7) | 0.0257 (7) | 0.0350 (7) | −0.0017 (5) | 0.0048 (5) | −0.0090 (6) |
O7A | 0.0305 (7) | 0.0246 (7) | 0.0256 (6) | −0.0078 (5) | 0.0047 (5) | −0.0023 (5) |
O8A | 0.0276 (7) | 0.0262 (7) | 0.0285 (7) | −0.0038 (5) | −0.0015 (5) | 0.0004 (5) |
C1A | 0.0279 (10) | 0.0332 (11) | 0.0300 (10) | −0.0049 (8) | 0.0034 (8) | −0.0079 (8) |
C2A | 0.0286 (12) | 0.0616 (15) | 0.0747 (16) | −0.0097 (10) | 0.0086 (11) | −0.0242 (13) |
C3A | 0.0483 (13) | 0.0345 (12) | 0.0418 (12) | 0.0043 (10) | 0.0053 (10) | −0.0111 (10) |
C4A | 0.0541 (14) | 0.0540 (14) | 0.0292 (11) | −0.0011 (11) | 0.0099 (10) | −0.0112 (10) |
C5A | 0.0299 (10) | 0.0350 (11) | 0.0343 (11) | −0.0095 (9) | −0.0015 (8) | −0.0094 (9) |
C6A | 0.0339 (12) | 0.0812 (18) | 0.0698 (16) | −0.0208 (12) | 0.0055 (11) | −0.0313 (14) |
C7A | 0.0858 (18) | 0.0334 (13) | 0.0585 (15) | −0.0221 (12) | −0.0139 (13) | −0.0038 (11) |
C8A | 0.0455 (12) | 0.0515 (13) | 0.0356 (11) | −0.0109 (10) | −0.0032 (9) | −0.0176 (10) |
C9A | 0.0369 (11) | 0.0307 (11) | 0.0241 (10) | −0.0021 (9) | −0.0049 (8) | −0.0006 (8) |
C10A | 0.0614 (15) | 0.0320 (12) | 0.0541 (14) | −0.0052 (11) | −0.0177 (11) | 0.0036 (10) |
C11A | 0.0690 (16) | 0.0651 (16) | 0.0282 (12) | 0.0130 (13) | −0.0016 (11) | 0.0004 (11) |
C12A | 0.0354 (12) | 0.0525 (14) | 0.0512 (13) | −0.0031 (10) | −0.0106 (10) | −0.0051 (11) |
C13A | 0.0407 (12) | 0.0373 (12) | 0.0287 (10) | −0.0102 (9) | 0.0033 (9) | 0.0099 (9) |
C14A | 0.0890 (19) | 0.0709 (17) | 0.0291 (12) | −0.0282 (14) | 0.0016 (12) | 0.0087 (11) |
C15A | 0.0658 (16) | 0.0404 (13) | 0.0515 (14) | −0.0103 (11) | 0.0013 (12) | 0.0155 (11) |
C16A | 0.0450 (14) | 0.0621 (16) | 0.0606 (15) | −0.0164 (12) | 0.0105 (11) | 0.0159 (12) |
C17A | 0.0306 (10) | 0.0271 (10) | 0.0349 (11) | −0.0069 (8) | −0.0009 (8) | −0.0102 (8) |
C18A | 0.0445 (13) | 0.0327 (12) | 0.0722 (15) | −0.0057 (10) | −0.0107 (11) | −0.0141 (11) |
C19A | 0.0546 (14) | 0.0660 (15) | 0.0400 (12) | −0.0201 (12) | 0.0045 (10) | −0.0244 (11) |
C20A | 0.0348 (11) | 0.0358 (11) | 0.0469 (12) | −0.0114 (9) | −0.0020 (9) | −0.0101 (10) |
C21A | 0.0310 (11) | 0.0268 (11) | 0.0427 (12) | −0.0018 (8) | 0.0040 (9) | −0.0096 (9) |
C22A | 0.094 (2) | 0.0308 (14) | 0.105 (2) | −0.0046 (13) | 0.0397 (17) | −0.0152 (14) |
C23A | 0.0583 (15) | 0.0799 (18) | 0.0499 (14) | 0.0059 (13) | 0.0030 (11) | −0.0326 (13) |
C24A | 0.0362 (13) | 0.0608 (16) | 0.0830 (18) | −0.0004 (11) | 0.0067 (12) | −0.0267 (13) |
C25A | 0.0305 (10) | 0.0267 (10) | 0.0308 (10) | −0.0067 (8) | 0.0058 (8) | −0.0013 (8) |
C26A | 0.0324 (12) | 0.0544 (14) | 0.0673 (15) | −0.0105 (10) | 0.0078 (11) | 0.0051 (12) |
C27A | 0.0687 (15) | 0.0372 (12) | 0.0327 (11) | −0.0112 (11) | 0.0143 (10) | −0.0014 (9) |
C28A | 0.0544 (13) | 0.0295 (11) | 0.0406 (12) | −0.0107 (10) | 0.0076 (10) | −0.0011 (9) |
C29A | 0.0313 (11) | 0.0289 (11) | 0.0352 (11) | −0.0048 (8) | −0.0055 (8) | 0.0000 (8) |
C30A | 0.0350 (13) | 0.0752 (18) | 0.0841 (18) | −0.0152 (12) | −0.0091 (12) | 0.0155 (14) |
C31A | 0.0604 (15) | 0.0331 (12) | 0.0585 (14) | −0.0041 (11) | −0.0183 (11) | 0.0044 (10) |
C32A | 0.0748 (17) | 0.0561 (15) | 0.0393 (13) | 0.0008 (13) | −0.0191 (11) | −0.0037 (11) |
Na1B | 0.0327 (4) | 0.0584 (5) | 0.0332 (4) | −0.0062 (4) | 0.0016 (3) | −0.0057 (4) |
Na2B | 0.0356 (4) | 0.0393 (4) | 0.0370 (4) | −0.0092 (3) | 0.0020 (3) | −0.0014 (3) |
Na3B | 0.0376 (4) | 0.0317 (4) | 0.0297 (4) | −0.0089 (3) | 0.0021 (3) | −0.0041 (3) |
Na4B | 0.0316 (4) | 0.0330 (4) | 0.0303 (4) | −0.0058 (3) | 0.0019 (3) | −0.0057 (3) |
Li1B | 0.0293 (17) | 0.0314 (17) | 0.0381 (18) | −0.0041 (14) | 0.0018 (14) | −0.0065 (14) |
Li2B | 0.0296 (17) | 0.0361 (18) | 0.0365 (18) | −0.0037 (14) | 0.0034 (14) | −0.0015 (14) |
Li3B | 0.0384 (19) | 0.0387 (19) | 0.0339 (17) | −0.0090 (15) | 0.0065 (14) | −0.0111 (15) |
Li4B | 0.0405 (19) | 0.0324 (18) | 0.0350 (18) | −0.0099 (15) | 0.0034 (14) | −0.0065 (14) |
O1B | 0.0304 (7) | 0.0306 (7) | 0.0326 (7) | −0.0043 (6) | 0.0037 (6) | 0.0065 (6) |
O2B | 0.0274 (7) | 0.0345 (7) | 0.0276 (7) | −0.0048 (6) | 0.0067 (5) | −0.0044 (6) |
O3B | 0.0259 (7) | 0.0491 (8) | 0.0354 (7) | −0.0037 (6) | −0.0048 (6) | −0.0001 (6) |
O4B | 0.0289 (7) | 0.0332 (7) | 0.0342 (7) | −0.0071 (6) | −0.0041 (5) | −0.0097 (6) |
O5B | 0.0364 (7) | 0.0467 (8) | 0.0243 (7) | −0.0097 (6) | 0.0095 (6) | −0.0055 (6) |
O6B | 0.0414 (8) | 0.0303 (7) | 0.0335 (7) | −0.0132 (6) | 0.0086 (6) | 0.0000 (6) |
O7B | 0.0355 (7) | 0.0450 (8) | 0.0327 (7) | −0.0134 (6) | 0.0015 (6) | −0.0122 (6) |
O8B | 0.0304 (7) | 0.0280 (7) | 0.0308 (7) | −0.0032 (6) | 0.0011 (5) | −0.0023 (5) |
C1B | 0.0466 (13) | 0.0351 (12) | 0.0479 (13) | −0.0017 (10) | 0.0076 (10) | 0.0136 (10) |
C2B | 0.0732 (18) | 0.0333 (14) | 0.095 (2) | 0.0024 (12) | 0.0107 (15) | 0.0049 (13) |
C3B | 0.099 (2) | 0.0725 (19) | 0.0487 (15) | −0.0081 (16) | −0.0005 (14) | 0.0292 (13) |
C4B | 0.0561 (16) | 0.0499 (15) | 0.098 (2) | −0.0159 (12) | 0.0296 (14) | 0.0141 (14) |
C5B | 0.0347 (11) | 0.0365 (11) | 0.0328 (11) | −0.0059 (9) | 0.0092 (9) | −0.0088 (9) |
C6B | 0.0620 (15) | 0.0438 (14) | 0.0648 (16) | −0.0020 (11) | 0.0172 (12) | −0.0164 (12) |
C7B | 0.0520 (14) | 0.0712 (16) | 0.0327 (12) | −0.0125 (12) | 0.0108 (10) | −0.0109 (11) |
C8B | 0.0357 (12) | 0.0677 (16) | 0.0491 (13) | −0.0146 (11) | 0.0156 (10) | −0.0102 (12) |
C9B | 0.0302 (11) | 0.0571 (14) | 0.0395 (12) | −0.0020 (10) | −0.0065 (9) | −0.0021 (10) |
C10B | 0.0600 (17) | 0.126 (3) | 0.0452 (15) | 0.0080 (16) | −0.0160 (12) | 0.0066 (15) |
C11B | 0.0351 (13) | 0.0728 (17) | 0.0704 (16) | −0.0143 (12) | −0.0046 (11) | −0.0163 (13) |
C12B | 0.0467 (14) | 0.0531 (15) | 0.0893 (19) | 0.0005 (12) | −0.0116 (13) | 0.0004 (14) |
C13B | 0.0300 (11) | 0.0458 (13) | 0.0460 (12) | −0.0055 (9) | −0.0034 (9) | −0.0215 (10) |
C14B | 0.0296 (13) | 0.110 (2) | 0.131 (2) | −0.0214 (13) | 0.0140 (14) | −0.080 (2) |
C15B | 0.096 (2) | 0.084 (2) | 0.0626 (17) | 0.0000 (16) | −0.0459 (15) | −0.0152 (15) |
C16B | 0.0469 (14) | 0.0506 (14) | 0.0770 (17) | −0.0135 (11) | 0.0025 (12) | −0.0316 (13) |
C17B | 0.0356 (11) | 0.0645 (15) | 0.0266 (11) | −0.0112 (10) | 0.0050 (9) | −0.0100 (10) |
C18B | 0.098 (2) | 0.096 (2) | 0.088 (2) | −0.0247 (18) | 0.0494 (17) | −0.0498 (18) |
C19B | 0.0605 (17) | 0.182 (3) | 0.0278 (13) | 0.0023 (19) | 0.0024 (12) | 0.0044 (16) |
C20B | 0.0501 (15) | 0.134 (3) | 0.0408 (14) | −0.0380 (15) | 0.0162 (11) | −0.0266 (15) |
C21B | 0.0501 (13) | 0.0337 (12) | 0.0344 (11) | −0.0145 (10) | 0.0084 (9) | −0.0009 (9) |
C22B | 0.100 (2) | 0.0718 (17) | 0.0363 (13) | −0.0436 (15) | 0.0015 (13) | 0.0102 (12) |
C23B | 0.0558 (15) | 0.0580 (15) | 0.0591 (15) | −0.0261 (12) | 0.0194 (12) | −0.0057 (12) |
C24B | 0.0768 (18) | 0.0367 (14) | 0.0819 (18) | −0.0154 (12) | 0.0167 (14) | 0.0015 (13) |
C25B | 0.0419 (12) | 0.0487 (13) | 0.0426 (12) | −0.0148 (10) | 0.0025 (9) | −0.0199 (10) |
C26B | 0.0687 (16) | 0.0912 (19) | 0.0419 (14) | −0.0353 (14) | −0.0071 (12) | −0.0209 (13) |
C27B | 0.0742 (18) | 0.0649 (17) | 0.099 (2) | −0.0120 (14) | 0.0019 (15) | −0.0455 (16) |
C28B | 0.0531 (15) | 0.0773 (17) | 0.0603 (15) | −0.0338 (13) | 0.0064 (12) | −0.0233 (13) |
C29B | 0.0350 (11) | 0.0269 (11) | 0.0430 (12) | 0.0005 (9) | −0.0021 (9) | 0.0008 (9) |
C30B | 0.0322 (12) | 0.0529 (14) | 0.0714 (16) | −0.0010 (10) | −0.0043 (11) | 0.0055 (12) |
C31B | 0.0684 (17) | 0.0389 (14) | 0.115 (2) | 0.0116 (12) | −0.0202 (16) | −0.0219 (15) |
C32B | 0.0509 (15) | 0.095 (2) | 0.0499 (15) | 0.0024 (14) | −0.0085 (12) | 0.0203 (14) |
Na1C | 0.0312 (4) | 0.0353 (4) | 0.0336 (4) | 0.0028 (3) | 0.0016 (3) | −0.0039 (3) |
Na2C | 0.0319 (4) | 0.0340 (4) | 0.0318 (4) | −0.0104 (3) | 0.0008 (3) | −0.0047 (3) |
Na3C | 0.0293 (4) | 0.0315 (4) | 0.0330 (4) | −0.0055 (3) | −0.0007 (3) | −0.0048 (3) |
Na4C | 0.0271 (4) | 0.0317 (4) | 0.0301 (4) | −0.0056 (3) | 0.0034 (3) | −0.0047 (3) |
Li1C | 0.0278 (16) | 0.0330 (17) | 0.0293 (16) | −0.0051 (13) | 0.0019 (13) | −0.0050 (14) |
Li2C | 0.0284 (16) | 0.0344 (18) | 0.0285 (16) | −0.0073 (14) | 0.0027 (13) | −0.0049 (14) |
Li3C | 0.0267 (16) | 0.0323 (17) | 0.0298 (16) | −0.0049 (13) | 0.0024 (13) | −0.0030 (13) |
Li4C | 0.0281 (17) | 0.0351 (18) | 0.0325 (17) | −0.0071 (14) | 0.0005 (13) | −0.0047 (14) |
O1C | 0.0267 (7) | 0.0290 (7) | 0.0272 (6) | −0.0056 (5) | −0.0012 (5) | −0.0076 (5) |
O2C | 0.0253 (7) | 0.0276 (7) | 0.0280 (7) | −0.0040 (5) | 0.0038 (5) | −0.0065 (5) |
O3C | 0.0287 (7) | 0.0277 (7) | 0.0306 (7) | −0.0004 (5) | −0.0003 (5) | 0.0022 (5) |
O4C | 0.0300 (7) | 0.0288 (7) | 0.0293 (7) | −0.0075 (6) | 0.0043 (5) | 0.0041 (5) |
O5C | 0.0261 (7) | 0.0329 (7) | 0.0262 (7) | −0.0008 (5) | 0.0041 (5) | −0.0095 (5) |
O6C | 0.0329 (7) | 0.0345 (7) | 0.0307 (7) | −0.0105 (6) | 0.0002 (5) | −0.0128 (6) |
O7C | 0.0239 (6) | 0.0263 (7) | 0.0262 (6) | −0.0022 (5) | −0.0013 (5) | −0.0003 (5) |
O8C | 0.0290 (7) | 0.0267 (7) | 0.0288 (7) | −0.0067 (5) | 0.0034 (5) | 0.0016 (5) |
C1C | 0.0273 (10) | 0.0348 (11) | 0.0302 (10) | −0.0072 (8) | −0.0004 (8) | −0.0092 (8) |
C2C | 0.0282 (12) | 0.0732 (17) | 0.0771 (17) | −0.0139 (11) | 0.0025 (11) | −0.0295 (14) |
C3C | 0.0606 (14) | 0.0456 (13) | 0.0329 (11) | −0.0104 (11) | −0.0089 (10) | −0.0116 (10) |
C4C | 0.0508 (13) | 0.0342 (12) | 0.0437 (12) | −0.0119 (10) | −0.0012 (10) | −0.0108 (10) |
C5C | 0.0257 (10) | 0.0336 (11) | 0.0320 (10) | −0.0033 (8) | 0.0063 (8) | −0.0089 (8) |
C6C | 0.0287 (12) | 0.0887 (19) | 0.0709 (16) | −0.0118 (12) | 0.0087 (11) | −0.0334 (14) |
C7C | 0.0634 (15) | 0.0345 (13) | 0.0551 (14) | 0.0028 (11) | 0.0186 (11) | −0.0119 (11) |
C8C | 0.0593 (15) | 0.0547 (14) | 0.0334 (12) | −0.0014 (11) | 0.0114 (10) | −0.0114 (10) |
C9C | 0.0317 (11) | 0.0275 (10) | 0.0318 (10) | −0.0001 (8) | −0.0006 (8) | 0.0010 (8) |
C10C | 0.0566 (14) | 0.0481 (13) | 0.0317 (11) | −0.0036 (11) | −0.0009 (10) | 0.0004 (10) |
C11C | 0.0643 (15) | 0.0316 (12) | 0.0563 (14) | −0.0028 (11) | −0.0095 (11) | 0.0022 (10) |
C12C | 0.0319 (12) | 0.0582 (15) | 0.0554 (14) | 0.0003 (10) | −0.0046 (10) | 0.0024 (11) |
C13C | 0.0292 (10) | 0.0346 (11) | 0.0347 (11) | −0.0071 (9) | 0.0035 (8) | 0.0066 (9) |
C14C | 0.0531 (14) | 0.0326 (12) | 0.0520 (13) | −0.0088 (10) | 0.0005 (11) | 0.0058 (10) |
C15C | 0.0467 (13) | 0.0511 (14) | 0.0333 (11) | −0.0043 (10) | 0.0075 (10) | 0.0065 (10) |
C16C | 0.0344 (12) | 0.0598 (15) | 0.0591 (14) | −0.0177 (11) | 0.0049 (10) | 0.0106 (12) |
C17C | 0.0245 (10) | 0.0375 (11) | 0.0268 (10) | −0.0009 (8) | 0.0014 (8) | −0.0090 (8) |
C18C | 0.0414 (12) | 0.0387 (12) | 0.0574 (14) | −0.0025 (10) | 0.0009 (10) | −0.0202 (11) |
C19C | 0.0424 (13) | 0.0651 (15) | 0.0311 (11) | 0.0001 (11) | −0.0018 (9) | −0.0108 (10) |
C20C | 0.0292 (11) | 0.0500 (13) | 0.0391 (11) | −0.0028 (9) | 0.0041 (9) | −0.0144 (10) |
C21C | 0.0308 (11) | 0.0376 (12) | 0.0377 (11) | −0.0079 (9) | −0.0006 (8) | −0.0151 (9) |
C22C | 0.0375 (13) | 0.0717 (16) | 0.0629 (15) | −0.0186 (11) | −0.0012 (11) | −0.0263 (13) |
C23C | 0.0633 (15) | 0.0388 (13) | 0.0555 (14) | −0.0082 (11) | −0.0042 (11) | −0.0194 (11) |
C24C | 0.0570 (14) | 0.0584 (15) | 0.0348 (12) | −0.0097 (11) | −0.0014 (10) | −0.0166 (11) |
C25C | 0.0250 (10) | 0.0292 (10) | 0.0300 (10) | −0.0029 (8) | −0.0012 (8) | −0.0001 (8) |
C26C | 0.0568 (14) | 0.0329 (12) | 0.0502 (13) | 0.0063 (10) | −0.0065 (11) | −0.0018 (10) |
C27C | 0.0252 (11) | 0.0619 (15) | 0.0611 (15) | −0.0055 (10) | −0.0011 (10) | 0.0064 (12) |
C28C | 0.0415 (12) | 0.0510 (13) | 0.0338 (11) | −0.0023 (10) | −0.0057 (9) | 0.0032 (10) |
C29C | 0.0300 (10) | 0.0356 (11) | 0.0327 (11) | −0.0086 (9) | 0.0025 (8) | 0.0046 (9) |
C30C | 0.0604 (15) | 0.0565 (15) | 0.0371 (12) | −0.0157 (12) | 0.0052 (10) | 0.0098 (11) |
C31C | 0.0304 (12) | 0.0748 (17) | 0.0677 (16) | −0.0169 (11) | 0.0002 (11) | 0.0125 (13) |
C32C | 0.0618 (15) | 0.0346 (13) | 0.0611 (15) | −0.0169 (11) | 0.0072 (12) | 0.0021 (11) |
Na1A—O1A | 2.5184 (13) | C11B—H11D | 0.980 |
Na1A—O3A | 2.3200 (12) | C11B—H11E | 0.980 |
Na1A—O5A | 2.3104 (12) | C11B—H11F | 0.980 |
Na1A—O7A | 2.5205 (13) | C12B—H12D | 0.980 |
Na2A—O2A | 2.5289 (13) | C12B—H12E | 0.980 |
Na2A—O3A | 2.3320 (13) | C12B—H12F | 0.980 |
Na2A—O6A | 2.3136 (13) | C13B—C14B | 1.517 (3) |
Na2A—O7A | 2.5100 (12) | C13B—C15B | 1.521 (3) |
Na3A—O2A | 2.5000 (13) | C13B—C16B | 1.526 (3) |
Na3A—O4A | 2.3285 (13) | C14B—H14D | 0.980 |
Na3A—O6A | 2.3426 (13) | C14B—H14E | 0.980 |
Na3A—O8A | 2.5341 (12) | C14B—H14F | 0.980 |
Na4A—O1A | 2.5125 (13) | C15B—H15D | 0.980 |
Na4A—O4A | 2.3177 (13) | C15B—H15E | 0.980 |
Na4A—O5A | 2.3071 (13) | C15B—H15F | 0.980 |
Na4A—O8A | 2.5151 (13) | C16B—H16D | 0.980 |
Li1A—O1A | 1.897 (3) | C16B—H16E | 0.980 |
Li1A—O2A | 1.906 (3) | C16B—H16F | 0.980 |
Li1A—O3A | 1.839 (3) | C17B—C18B | 1.523 (3) |
Li2A—O1A | 1.887 (3) | C17B—C19B | 1.510 (3) |
Li2A—O2A | 1.892 (3) | C17B—C20B | 1.510 (3) |
Li2A—O4A | 1.846 (3) | C18B—H18D | 0.980 |
Li3A—O5A | 1.843 (3) | C18B—H18E | 0.980 |
Li3A—O7A | 1.896 (3) | C18B—H18F | 0.980 |
Li3A—O8A | 1.895 (3) | C19B—H19D | 0.980 |
Li4A—O6A | 1.834 (3) | C19B—H19E | 0.980 |
Li4A—O7A | 1.898 (3) | C19B—H19F | 0.980 |
Li4A—O8A | 1.896 (3) | C20B—H20D | 0.980 |
O1A—C1A | 1.412 (2) | C20B—H20E | 0.980 |
O2A—C5A | 1.4164 (19) | C20B—H20F | 0.980 |
O3A—C9A | 1.406 (2) | C21B—C22B | 1.521 (3) |
O4A—C13A | 1.402 (2) | C21B—C23B | 1.536 (3) |
O5A—C17A | 1.4037 (19) | C21B—C24B | 1.534 (3) |
O6A—C21A | 1.401 (2) | C22B—H22D | 0.980 |
O7A—C25A | 1.414 (2) | C22B—H22E | 0.980 |
O8A—C29A | 1.419 (2) | C22B—H22F | 0.980 |
C1A—C2A | 1.526 (2) | C23B—H23D | 0.980 |
C1A—C3A | 1.520 (3) | C23B—H23E | 0.980 |
C1A—C4A | 1.534 (2) | C23B—H23F | 0.980 |
C2A—H2A | 0.980 | C24B—H24D | 0.980 |
C2A—H2B | 0.980 | C24B—H24E | 0.980 |
C2A—H2C | 0.980 | C24B—H24F | 0.980 |
C3A—H3A | 0.980 | C25B—C26B | 1.522 (3) |
C3A—H3B | 0.980 | C25B—C27B | 1.517 (3) |
C3A—H3C | 0.980 | C25B—C28B | 1.528 (3) |
C4A—H4A | 0.980 | C26B—H26D | 0.980 |
C4A—H4B | 0.980 | C26B—H26E | 0.980 |
C4A—H4C | 0.980 | C26B—H26F | 0.980 |
C5A—C6A | 1.531 (3) | C27B—H27D | 0.980 |
C5A—C7A | 1.528 (3) | C27B—H27E | 0.980 |
C5A—C8A | 1.514 (2) | C27B—H27F | 0.980 |
C6A—H6A | 0.980 | C28B—H28D | 0.980 |
C6A—H6B | 0.980 | C28B—H28E | 0.980 |
C6A—H6C | 0.980 | C28B—H28F | 0.980 |
C7A—H7A | 0.980 | C29B—C30B | 1.520 (3) |
C7A—H7B | 0.980 | C29B—C31B | 1.521 (3) |
C7A—H7C | 0.980 | C29B—C32B | 1.519 (3) |
C8A—H8A | 0.980 | C30B—H30D | 0.980 |
C8A—H8B | 0.980 | C30B—H30E | 0.980 |
C8A—H8C | 0.980 | C30B—H30F | 0.980 |
C9A—C10A | 1.530 (3) | C31B—H31D | 0.980 |
C9A—C11A | 1.525 (3) | C31B—H31E | 0.980 |
C9A—C12A | 1.529 (3) | C31B—H31F | 0.980 |
C10A—H10A | 0.980 | C32B—H32D | 0.980 |
C10A—H10B | 0.980 | C32B—H32E | 0.980 |
C10A—H10C | 0.980 | C32B—H32F | 0.980 |
C11A—H11A | 0.980 | Na1C—O1C | 2.5776 (13) |
C11A—H11B | 0.980 | Na1C—O3C | 2.2890 (13) |
C11A—H11C | 0.980 | Na1C—O5C | 2.2704 (13) |
C12A—H12A | 0.980 | Na1C—O8C | 2.5882 (13) |
C12A—H12B | 0.980 | Na2C—O2C | 2.5332 (13) |
C12A—H12C | 0.980 | Na2C—O4C | 2.3113 (13) |
C13A—C14A | 1.527 (3) | Na2C—O6C | 2.3137 (13) |
C13A—C15A | 1.530 (3) | Na2C—O7C | 2.5628 (13) |
C13A—C16A | 1.533 (3) | Na3C—O2C | 2.5041 (13) |
C14A—H14A | 0.980 | Na3C—O3C | 2.3574 (13) |
C14A—H14B | 0.980 | Na3C—O6C | 2.3526 (13) |
C14A—H14C | 0.980 | Na3C—O8C | 2.4887 (13) |
C15A—H15A | 0.980 | Na4C—O1C | 2.4985 (13) |
C15A—H15B | 0.980 | Na4C—O4C | 2.3276 (13) |
C15A—H15C | 0.980 | Na4C—O5C | 2.3395 (13) |
C16A—H16A | 0.980 | Na4C—O7C | 2.4934 (12) |
C16A—H16B | 0.980 | Li1C—O1C | 1.893 (3) |
C16A—H16C | 0.980 | Li1C—O2C | 1.908 (3) |
C17A—C18A | 1.531 (3) | Li1C—O3C | 1.833 (3) |
C17A—C19A | 1.524 (3) | Li2C—O1C | 1.893 (3) |
C17A—C20A | 1.528 (2) | Li2C—O2C | 1.899 (3) |
C18A—H18A | 0.980 | Li2C—O4C | 1.824 (3) |
C18A—H18B | 0.980 | Li3C—O5C | 1.836 (3) |
C18A—H18C | 0.980 | Li3C—O7C | 1.896 (3) |
C19A—H19A | 0.980 | Li3C—O8C | 1.893 (3) |
C19A—H19B | 0.980 | Li4C—O6C | 1.827 (3) |
C19A—H19C | 0.980 | Li4C—O7C | 1.898 (3) |
C20A—H20A | 0.980 | Li4C—O8C | 1.901 (3) |
C20A—H20B | 0.980 | O1C—C1C | 1.4142 (19) |
C20A—H20C | 0.980 | O2C—C5C | 1.4161 (19) |
C21A—C22A | 1.516 (3) | O3C—C9C | 1.404 (2) |
C21A—C23A | 1.521 (3) | O4C—C13C | 1.408 (2) |
C21A—C24A | 1.534 (3) | O5C—C17C | 1.407 (2) |
C22A—H22A | 0.980 | O6C—C21C | 1.4079 (19) |
C22A—H22B | 0.980 | O7C—C25C | 1.417 (2) |
C22A—H22C | 0.980 | O8C—C29C | 1.412 (2) |
C23A—H23A | 0.980 | C1C—C2C | 1.534 (3) |
C23A—H23B | 0.980 | C1C—C3C | 1.519 (2) |
C23A—H23C | 0.980 | C1C—C4C | 1.525 (3) |
C24A—H24A | 0.980 | C2C—H2G | 0.980 |
C24A—H24B | 0.980 | C2C—H2H | 0.980 |
C24A—H24C | 0.980 | C2C—H2I | 0.980 |
C25A—C26A | 1.533 (3) | C3C—H3G | 0.980 |
C25A—C27A | 1.525 (2) | C3C—H3H | 0.980 |
C25A—C28A | 1.526 (2) | C3C—H3I | 0.980 |
C26A—H26A | 0.980 | C4C—H4G | 0.980 |
C26A—H26B | 0.980 | C4C—H4H | 0.980 |
C26A—H26C | 0.980 | C4C—H4I | 0.980 |
C27A—H27A | 0.980 | C5C—C6C | 1.527 (2) |
C27A—H27B | 0.980 | C5C—C7C | 1.518 (3) |
C27A—H27C | 0.980 | C5C—C8C | 1.521 (3) |
C28A—H28A | 0.980 | C6C—H6G | 0.980 |
C28A—H28B | 0.980 | C6C—H6H | 0.980 |
C28A—H28C | 0.980 | C6C—H6I | 0.980 |
C29A—C30A | 1.521 (3) | C7C—H7G | 0.980 |
C29A—C31A | 1.522 (3) | C7C—H7H | 0.980 |
C29A—C32A | 1.528 (3) | C7C—H7I | 0.980 |
C30A—H30A | 0.980 | C8C—H8G | 0.980 |
C30A—H30B | 0.980 | C8C—H8H | 0.980 |
C30A—H30C | 0.980 | C8C—H8I | 0.980 |
C31A—H31A | 0.980 | C9C—C10C | 1.533 (3) |
C31A—H31B | 0.980 | C9C—C11C | 1.523 (3) |
C31A—H31C | 0.980 | C9C—C12C | 1.533 (3) |
C32A—H32A | 0.980 | C10C—H10G | 0.980 |
C32A—H32B | 0.980 | C10C—H10H | 0.980 |
C32A—H32C | 0.980 | C10C—H10I | 0.980 |
Na1B—O1B | 2.5372 (14) | C11C—H11G | 0.980 |
Na1B—O3B | 2.2895 (14) | C11C—H11H | 0.980 |
Na1B—O5B | 2.3059 (14) | C11C—H11I | 0.980 |
Na1B—O7B | 2.6030 (15) | C12C—H12G | 0.980 |
Na2B—O2B | 2.5735 (13) | C12C—H12H | 0.980 |
Na2B—O3B | 2.3178 (14) | C12C—H12I | 0.980 |
Na2B—O6B | 2.3112 (14) | C13C—C14C | 1.522 (3) |
Na2B—O7B | 2.5375 (14) | C13C—C15C | 1.528 (3) |
Na3B—O2B | 2.4986 (13) | C13C—C16C | 1.544 (2) |
Na3B—O4B | 2.3491 (13) | C14C—H14G | 0.980 |
Na3B—O6B | 2.3449 (13) | C14C—H14H | 0.980 |
Na3B—O8B | 2.4775 (13) | C14C—H14I | 0.980 |
Na4B—O1B | 2.4955 (13) | C15C—H15G | 0.980 |
Na4B—O4B | 2.3251 (13) | C15C—H15H | 0.980 |
Na4B—O5B | 2.3481 (13) | C15C—H15I | 0.980 |
Na4B—O8B | 2.4916 (13) | C16C—H16G | 0.980 |
Li1B—O1B | 1.890 (3) | C16C—H16H | 0.980 |
Li1B—O2B | 1.902 (3) | C16C—H16I | 0.980 |
Li1B—O4B | 1.824 (3) | C17C—C18C | 1.529 (3) |
Li2B—O1B | 1.903 (3) | C17C—C19C | 1.526 (2) |
Li2B—O2B | 1.895 (3) | C17C—C20C | 1.541 (2) |
Li2B—O3B | 1.828 (3) | C18C—H18G | 0.980 |
Li3B—O5B | 1.828 (3) | C18C—H18H | 0.980 |
Li3B—O7B | 1.897 (3) | C18C—H18I | 0.980 |
Li3B—O8B | 1.907 (3) | C19C—H19G | 0.980 |
Li4B—O6B | 1.827 (3) | C19C—H19H | 0.980 |
Li4B—O7B | 1.892 (3) | C19C—H19I | 0.980 |
Li4B—O8B | 1.913 (3) | C20C—H20G | 0.980 |
O1B—C1B | 1.413 (2) | C20C—H20H | 0.980 |
O2B—C5B | 1.413 (2) | C20C—H20I | 0.980 |
O3B—C9B | 1.402 (2) | C21C—C22C | 1.535 (3) |
O4B—C13B | 1.406 (2) | C21C—C23C | 1.525 (3) |
O5B—C17B | 1.409 (2) | C21C—C24C | 1.531 (3) |
O6B—C21B | 1.404 (2) | C22C—H22G | 0.980 |
O7B—C25B | 1.424 (2) | C22C—H22H | 0.980 |
O8B—C29B | 1.421 (2) | C22C—H22I | 0.980 |
C1B—C2B | 1.529 (3) | C23C—H23G | 0.980 |
C1B—C3B | 1.527 (3) | C23C—H23H | 0.980 |
C1B—C4B | 1.529 (3) | C23C—H23I | 0.980 |
C2B—H2D | 0.980 | C24C—H24G | 0.980 |
C2B—H2E | 0.980 | C24C—H24H | 0.980 |
C2B—H2F | 0.980 | C24C—H24I | 0.980 |
C3B—H3D | 0.980 | C25C—C26C | 1.531 (3) |
C3B—H3E | 0.980 | C25C—C27C | 1.528 (2) |
C3B—H3F | 0.980 | C25C—C28C | 1.517 (2) |
C4B—H4D | 0.980 | C26C—H26G | 0.980 |
C4B—H4E | 0.980 | C26C—H26H | 0.980 |
C4B—H4F | 0.980 | C26C—H26I | 0.980 |
C5B—C6B | 1.524 (3) | C27C—H27G | 0.980 |
C5B—C7B | 1.531 (3) | C27C—H27H | 0.980 |
C5B—C8B | 1.529 (2) | C27C—H27I | 0.980 |
C6B—H6D | 0.980 | C28C—H28G | 0.980 |
C6B—H6E | 0.980 | C28C—H28H | 0.980 |
C6B—H6F | 0.980 | C28C—H28I | 0.980 |
C7B—H7D | 0.980 | C29C—C30C | 1.528 (3) |
C7B—H7E | 0.980 | C29C—C31C | 1.533 (3) |
C7B—H7F | 0.980 | C29C—C32C | 1.529 (3) |
C8B—H8D | 0.980 | C30C—H30G | 0.980 |
C8B—H8E | 0.980 | C30C—H30H | 0.980 |
C8B—H8F | 0.980 | C30C—H30I | 0.980 |
C9B—C10B | 1.527 (3) | C31C—H31G | 0.980 |
C9B—C11B | 1.530 (3) | C31C—H31H | 0.980 |
C9B—C12B | 1.536 (3) | C31C—H31I | 0.980 |
C10B—H10D | 0.980 | C32C—H32G | 0.980 |
C10B—H10E | 0.980 | C32C—H32H | 0.980 |
C10B—H10F | 0.980 | C32C—H32I | 0.980 |
O1A—Na1A—O3A | 82.11 (4) | H8D—C8B—H8F | 109.5 |
O1A—Na1A—O5A | 87.83 (4) | H8E—C8B—H8F | 109.5 |
O1A—Na1A—O7A | 116.94 (4) | O3B—C9B—C10B | 110.50 (17) |
O3A—Na1A—O5A | 162.20 (5) | O3B—C9B—C11B | 109.56 (17) |
O3A—Na1A—O7A | 89.11 (4) | O3B—C9B—C12B | 110.19 (16) |
O5A—Na1A—O7A | 82.38 (4) | C10B—C9B—C11B | 109.14 (18) |
O2A—Na2A—O3A | 82.51 (4) | C10B—C9B—C12B | 109.63 (19) |
O2A—Na2A—O6A | 88.78 (4) | C11B—C9B—C12B | 107.77 (18) |
O2A—Na2A—O7A | 117.23 (4) | C9B—C10B—H10D | 109.5 |
O3A—Na2A—O6A | 162.71 (5) | C9B—C10B—H10E | 109.5 |
O3A—Na2A—O7A | 89.10 (4) | C9B—C10B—H10F | 109.5 |
O6A—Na2A—O7A | 81.63 (4) | H10D—C10B—H10E | 109.5 |
O2A—Na3A—O4A | 82.17 (4) | H10D—C10B—H10F | 109.5 |
O2A—Na3A—O6A | 88.83 (4) | H10E—C10B—H10F | 109.5 |
O2A—Na3A—O8A | 117.72 (4) | C9B—C11B—H11D | 109.5 |
O4A—Na3A—O6A | 161.77 (5) | C9B—C11B—H11E | 109.5 |
O4A—Na3A—O8A | 87.97 (4) | C9B—C11B—H11F | 109.5 |
O6A—Na3A—O8A | 82.21 (4) | H11D—C11B—H11E | 109.5 |
O1A—Na4A—O4A | 82.34 (4) | H11D—C11B—H11F | 109.5 |
O1A—Na4A—O5A | 88.04 (4) | H11E—C11B—H11F | 109.5 |
O1A—Na4A—O8A | 117.56 (4) | C9B—C12B—H12D | 109.5 |
O4A—Na4A—O5A | 162.00 (5) | C9B—C12B—H12E | 109.5 |
O4A—Na4A—O8A | 88.66 (4) | C9B—C12B—H12F | 109.5 |
O5A—Na4A—O8A | 82.33 (4) | H12D—C12B—H12E | 109.5 |
O1A—Li1A—O2A | 96.34 (14) | H12D—C12B—H12F | 109.5 |
O1A—Li1A—O3A | 116.75 (15) | H12E—C12B—H12F | 109.5 |
O2A—Li1A—O3A | 117.90 (16) | O4B—C13B—C14B | 110.59 (16) |
O1A—Li2A—O2A | 97.20 (14) | O4B—C13B—C15B | 109.42 (17) |
O1A—Li2A—O4A | 117.01 (15) | O4B—C13B—C16B | 110.55 (15) |
O2A—Li2A—O4A | 116.34 (16) | C14B—C13B—C15B | 109.43 (19) |
O5A—Li3A—O7A | 116.84 (16) | C14B—C13B—C16B | 108.48 (18) |
O5A—Li3A—O8A | 116.45 (16) | C15B—C13B—C16B | 108.33 (18) |
O7A—Li3A—O8A | 97.44 (13) | C13B—C14B—H14D | 109.5 |
O6A—Li4A—O7A | 115.47 (16) | C13B—C14B—H14E | 109.5 |
O6A—Li4A—O8A | 118.74 (16) | C13B—C14B—H14F | 109.5 |
O7A—Li4A—O8A | 97.34 (14) | H14D—C14B—H14E | 109.5 |
Na1A—O1A—Na4A | 81.37 (4) | H14D—C14B—H14F | 109.5 |
Na1A—O1A—Li1A | 76.50 (10) | H14E—C14B—H14F | 109.5 |
Na1A—O1A—Li2A | 127.54 (10) | C13B—C15B—H15D | 109.5 |
Na1A—O1A—C1A | 111.56 (9) | C13B—C15B—H15E | 109.5 |
Na4A—O1A—Li1A | 127.47 (10) | C13B—C15B—H15F | 109.5 |
Na4A—O1A—Li2A | 76.60 (9) | H15D—C15B—H15E | 109.5 |
Na4A—O1A—C1A | 111.38 (9) | H15D—C15B—H15F | 109.5 |
Li1A—O1A—Li2A | 80.38 (13) | H15E—C15B—H15F | 109.5 |
Li1A—O1A—C1A | 120.99 (13) | C13B—C16B—H16D | 109.5 |
Li2A—O1A—C1A | 120.74 (13) | C13B—C16B—H16E | 109.5 |
Na2A—O2A—Na3A | 81.12 (4) | C13B—C16B—H16F | 109.5 |
Na2A—O2A—Li1A | 75.80 (10) | H16D—C16B—H16E | 109.5 |
Na2A—O2A—Li2A | 126.83 (10) | H16D—C16B—H16F | 109.5 |
Na2A—O2A—C5A | 111.79 (10) | H16E—C16B—H16F | 109.5 |
Na3A—O2A—Li1A | 127.27 (10) | O5B—C17B—C18B | 109.79 (18) |
Na3A—O2A—Li2A | 77.18 (10) | O5B—C17B—C19B | 110.17 (17) |
Na3A—O2A—C5A | 113.70 (10) | O5B—C17B—C20B | 110.22 (15) |
Li1A—O2A—Li2A | 80.03 (13) | C18B—C17B—C19B | 109.0 (2) |
Li1A—O2A—C5A | 118.81 (13) | C18B—C17B—C20B | 108.2 (2) |
Li2A—O2A—C5A | 121.36 (13) | C19B—C17B—C20B | 109.4 (2) |
Na1A—O3A—Na2A | 88.97 (4) | C17B—C18B—H18D | 109.5 |
Na1A—O3A—Li1A | 82.92 (10) | C17B—C18B—H18E | 109.5 |
Na1A—O3A—C9A | 127.92 (10) | C17B—C18B—H18F | 109.5 |
Na2A—O3A—Li1A | 82.27 (10) | H18D—C18B—H18E | 109.5 |
Na2A—O3A—C9A | 134.65 (10) | H18D—C18B—H18F | 109.5 |
Li1A—O3A—C9A | 122.68 (14) | H18E—C18B—H18F | 109.5 |
Na3A—O4A—Na4A | 89.67 (4) | C17B—C19B—H19D | 109.5 |
Na3A—O4A—Li2A | 82.64 (10) | C17B—C19B—H19E | 109.5 |
Na3A—O4A—C13A | 131.45 (11) | C17B—C19B—H19F | 109.5 |
Na4A—O4A—Li2A | 82.58 (10) | H19D—C19B—H19E | 109.5 |
Na4A—O4A—C13A | 132.93 (11) | H19D—C19B—H19F | 109.5 |
Li2A—O4A—C13A | 119.18 (14) | H19E—C19B—H19F | 109.5 |
Na1A—O5A—Na4A | 90.51 (4) | C17B—C20B—H20D | 109.5 |
Na1A—O5A—Li3A | 83.01 (10) | C17B—C20B—H20E | 109.5 |
Na1A—O5A—C17A | 129.79 (10) | C17B—C20B—H20F | 109.5 |
Na4A—O5A—Li3A | 83.08 (10) | H20D—C20B—H20E | 109.5 |
Na4A—O5A—C17A | 134.12 (10) | H20D—C20B—H20F | 109.5 |
Li3A—O5A—C17A | 118.11 (13) | H20E—C20B—H20F | 109.5 |
Na2A—O6A—Na3A | 89.23 (5) | O6B—C21B—C22B | 110.30 (15) |
Na2A—O6A—Li4A | 83.69 (10) | O6B—C21B—C23B | 110.51 (16) |
Na2A—O6A—C21A | 133.39 (10) | O6B—C21B—C24B | 110.00 (16) |
Na3A—O6A—Li4A | 81.92 (10) | C22B—C21B—C23B | 108.81 (17) |
Na3A—O6A—C21A | 129.65 (10) | C22B—C21B—C24B | 108.72 (19) |
Li4A—O6A—C21A | 121.42 (14) | C23B—C21B—C24B | 108.46 (17) |
Na1A—O7A—Na2A | 80.79 (4) | C21B—C22B—H22D | 109.5 |
Na1A—O7A—Li3A | 76.38 (10) | C21B—C22B—H22E | 109.5 |
Na1A—O7A—Li4A | 126.95 (10) | C21B—C22B—H22F | 109.5 |
Na1A—O7A—C25A | 114.87 (10) | H22D—C22B—H22E | 109.5 |
Na2A—O7A—Li3A | 127.08 (10) | H22D—C22B—H22F | 109.5 |
Na2A—O7A—Li4A | 77.15 (9) | H22E—C22B—H22F | 109.5 |
Na2A—O7A—C25A | 111.26 (9) | C21B—C23B—H23D | 109.5 |
Li3A—O7A—Li4A | 79.75 (13) | C21B—C23B—H23E | 109.5 |
Li3A—O7A—C25A | 121.64 (13) | C21B—C23B—H23F | 109.5 |
Li4A—O7A—C25A | 118.03 (13) | H23D—C23B—H23E | 109.5 |
Na3A—O8A—Na4A | 80.90 (4) | H23D—C23B—H23F | 109.5 |
Na3A—O8A—Li3A | 126.07 (10) | H23E—C23B—H23F | 109.5 |
Na3A—O8A—Li4A | 75.70 (9) | C21B—C24B—H24D | 109.5 |
Na3A—O8A—C29A | 113.11 (9) | C21B—C24B—H24E | 109.5 |
Na4A—O8A—Li3A | 76.52 (10) | C21B—C24B—H24F | 109.5 |
Na4A—O8A—Li4A | 126.60 (10) | H24D—C24B—H24E | 109.5 |
Na4A—O8A—C29A | 111.69 (10) | H24D—C24B—H24F | 109.5 |
Li3A—O8A—Li4A | 79.83 (13) | H24E—C24B—H24F | 109.5 |
Li3A—O8A—C29A | 120.68 (13) | O7B—C25B—C26B | 109.61 (16) |
Li4A—O8A—C29A | 121.58 (14) | O7B—C25B—C27B | 109.55 (17) |
O1A—C1A—C2A | 109.58 (14) | O7B—C25B—C28B | 110.29 (15) |
O1A—C1A—C3A | 110.65 (14) | C26B—C25B—C27B | 110.18 (19) |
O1A—C1A—C4A | 110.46 (14) | C26B—C25B—C28B | 108.28 (18) |
C2A—C1A—C3A | 109.00 (16) | C27B—C25B—C28B | 108.91 (19) |
C2A—C1A—C4A | 109.01 (16) | C25B—C26B—H26D | 109.5 |
C3A—C1A—C4A | 108.10 (15) | C25B—C26B—H26E | 109.5 |
C1A—C2A—H2A | 109.5 | C25B—C26B—H26F | 109.5 |
C1A—C2A—H2B | 109.5 | H26D—C26B—H26E | 109.5 |
C1A—C2A—H2C | 109.5 | H26D—C26B—H26F | 109.5 |
H2A—C2A—H2B | 109.5 | H26E—C26B—H26F | 109.5 |
H2A—C2A—H2C | 109.5 | C25B—C27B—H27D | 109.5 |
H2B—C2A—H2C | 109.5 | C25B—C27B—H27E | 109.5 |
C1A—C3A—H3A | 109.5 | C25B—C27B—H27F | 109.5 |
C1A—C3A—H3B | 109.5 | H27D—C27B—H27E | 109.5 |
C1A—C3A—H3C | 109.5 | H27D—C27B—H27F | 109.5 |
H3A—C3A—H3B | 109.5 | H27E—C27B—H27F | 109.5 |
H3A—C3A—H3C | 109.5 | C25B—C28B—H28D | 109.5 |
H3B—C3A—H3C | 109.5 | C25B—C28B—H28E | 109.5 |
C1A—C4A—H4A | 109.5 | C25B—C28B—H28F | 109.5 |
C1A—C4A—H4B | 109.5 | H28D—C28B—H28E | 109.5 |
C1A—C4A—H4C | 109.5 | H28D—C28B—H28F | 109.5 |
H4A—C4A—H4B | 109.5 | H28E—C28B—H28F | 109.5 |
H4A—C4A—H4C | 109.5 | O8B—C29B—C30B | 110.49 (15) |
H4B—C4A—H4C | 109.5 | O8B—C29B—C31B | 108.48 (16) |
O2A—C5A—C6A | 109.03 (14) | O8B—C29B—C32B | 110.27 (16) |
O2A—C5A—C7A | 110.53 (14) | C30B—C29B—C31B | 108.96 (18) |
O2A—C5A—C8A | 109.74 (14) | C30B—C29B—C32B | 108.51 (17) |
C6A—C5A—C7A | 109.69 (17) | C31B—C29B—C32B | 110.11 (19) |
C6A—C5A—C8A | 108.90 (16) | C29B—C30B—H30D | 109.5 |
C7A—C5A—C8A | 108.94 (16) | C29B—C30B—H30E | 109.5 |
C5A—C6A—H6A | 109.5 | C29B—C30B—H30F | 109.5 |
C5A—C6A—H6B | 109.5 | H30D—C30B—H30E | 109.5 |
C5A—C6A—H6C | 109.5 | H30D—C30B—H30F | 109.5 |
H6A—C6A—H6B | 109.5 | H30E—C30B—H30F | 109.5 |
H6A—C6A—H6C | 109.5 | C29B—C31B—H31D | 109.5 |
H6B—C6A—H6C | 109.5 | C29B—C31B—H31E | 109.5 |
C5A—C7A—H7A | 109.5 | C29B—C31B—H31F | 109.5 |
C5A—C7A—H7B | 109.5 | H31D—C31B—H31E | 109.5 |
C5A—C7A—H7C | 109.5 | H31D—C31B—H31F | 109.5 |
H7A—C7A—H7B | 109.5 | H31E—C31B—H31F | 109.5 |
H7A—C7A—H7C | 109.5 | C29B—C32B—H32D | 109.5 |
H7B—C7A—H7C | 109.5 | C29B—C32B—H32E | 109.5 |
C5A—C8A—H8A | 109.5 | C29B—C32B—H32F | 109.5 |
C5A—C8A—H8B | 109.5 | H32D—C32B—H32E | 109.5 |
C5A—C8A—H8C | 109.5 | H32D—C32B—H32F | 109.5 |
H8A—C8A—H8B | 109.5 | H32E—C32B—H32F | 109.5 |
H8A—C8A—H8C | 109.5 | O1C—Na1C—O3C | 81.77 (4) |
H8B—C8A—H8C | 109.5 | O1C—Na1C—O5C | 88.41 (4) |
O3A—C9A—C10A | 110.62 (14) | O1C—Na1C—O8C | 116.08 (4) |
O3A—C9A—C11A | 110.04 (15) | O3C—Na1C—O5C | 161.40 (5) |
O3A—C9A—C12A | 110.14 (15) | O3C—Na1C—O8C | 88.55 (4) |
C10A—C9A—C11A | 109.50 (17) | O5C—Na1C—O8C | 81.61 (4) |
C10A—C9A—C12A | 107.70 (16) | O2C—Na2C—O4C | 81.80 (4) |
C11A—C9A—C12A | 108.78 (16) | O2C—Na2C—O6C | 89.28 (4) |
C9A—C10A—H10A | 109.5 | O2C—Na2C—O7C | 116.57 (4) |
C9A—C10A—H10B | 109.5 | O4C—Na2C—O6C | 161.57 (5) |
C9A—C10A—H10C | 109.5 | O4C—Na2C—O7C | 88.13 (4) |
H10A—C10A—H10B | 109.5 | O6C—Na2C—O7C | 81.46 (4) |
H10A—C10A—H10C | 109.5 | O2C—Na3C—O3C | 81.67 (4) |
H10B—C10A—H10C | 109.5 | O2C—Na3C—O6C | 89.12 (4) |
C9A—C11A—H11A | 109.5 | O2C—Na3C—O8C | 119.40 (5) |
C9A—C11A—H11B | 109.5 | O3C—Na3C—O6C | 161.74 (5) |
C9A—C11A—H11C | 109.5 | O3C—Na3C—O8C | 89.45 (4) |
H11A—C11A—H11B | 109.5 | O6C—Na3C—O8C | 81.35 (4) |
H11A—C11A—H11C | 109.5 | O1C—Na4C—O4C | 81.31 (4) |
H11B—C11A—H11C | 109.5 | O1C—Na4C—O5C | 88.81 (4) |
C9A—C12A—H12A | 109.5 | O1C—Na4C—O7C | 119.87 (4) |
C9A—C12A—H12B | 109.5 | O4C—Na4C—O5C | 161.53 (5) |
C9A—C12A—H12C | 109.5 | O4C—Na4C—O7C | 89.45 (4) |
H12A—C12A—H12B | 109.5 | O5C—Na4C—O7C | 81.96 (4) |
H12A—C12A—H12C | 109.5 | O1C—Li1C—O2C | 97.22 (14) |
H12B—C12A—H12C | 109.5 | O1C—Li1C—O3C | 117.92 (16) |
O4A—C13A—C14A | 110.16 (15) | O2C—Li1C—O3C | 116.47 (15) |
O4A—C13A—C15A | 110.38 (16) | O1C—Li2C—O2C | 97.57 (14) |
O4A—C13A—C16A | 109.82 (15) | O1C—Li2C—O4C | 115.70 (16) |
C14A—C13A—C15A | 109.02 (17) | O2C—Li2C—O4C | 117.12 (15) |
C14A—C13A—C16A | 108.80 (17) | O5C—Li3C—O7C | 116.39 (16) |
C15A—C13A—C16A | 108.62 (17) | O5C—Li3C—O8C | 117.30 (16) |
C13A—C14A—H14A | 109.5 | O7C—Li3C—O8C | 97.97 (14) |
C13A—C14A—H14B | 109.5 | O6C—Li4C—O7C | 117.68 (16) |
C13A—C14A—H14C | 109.5 | O6C—Li4C—O8C | 115.75 (16) |
H14A—C14A—H14B | 109.5 | O7C—Li4C—O8C | 97.62 (14) |
H14A—C14A—H14C | 109.5 | Na1C—O1C—Na4C | 80.32 (4) |
H14B—C14A—H14C | 109.5 | Na1C—O1C—Li1C | 74.97 (10) |
C13A—C15A—H15A | 109.5 | Na1C—O1C—Li2C | 126.55 (10) |
C13A—C15A—H15B | 109.5 | Na1C—O1C—C1C | 114.28 (9) |
C13A—C15A—H15C | 109.5 | Na4C—O1C—Li1C | 125.88 (10) |
H15A—C15A—H15B | 109.5 | Na4C—O1C—Li2C | 77.48 (10) |
H15A—C15A—H15C | 109.5 | Na4C—O1C—C1C | 110.49 (10) |
H15B—C15A—H15C | 109.5 | Li1C—O1C—Li2C | 80.02 (13) |
C13A—C16A—H16A | 109.5 | Li1C—O1C—C1C | 123.49 (13) |
C13A—C16A—H16B | 109.5 | Li2C—O1C—C1C | 118.96 (13) |
C13A—C16A—H16C | 109.5 | Na2C—O2C—Na3C | 80.86 (4) |
H16A—C16A—H16B | 109.5 | Na2C—O2C—Li1C | 126.78 (10) |
H16A—C16A—H16C | 109.5 | Na2C—O2C—Li2C | 76.23 (9) |
H16B—C16A—H16C | 109.5 | Na2C—O2C—C5C | 114.10 (9) |
O5A—C17A—C18A | 110.01 (14) | Na3C—O2C—Li1C | 77.33 (10) |
O5A—C17A—C19A | 110.61 (15) | Na3C—O2C—Li2C | 127.05 (10) |
O5A—C17A—C20A | 109.61 (14) | Na3C—O2C—C5C | 112.20 (9) |
C18A—C17A—C19A | 108.93 (16) | Li1C—O2C—Li2C | 79.49 (13) |
C18A—C17A—C20A | 109.06 (15) | Li1C—O2C—C5C | 119.05 (13) |
C19A—C17A—C20A | 108.59 (15) | Li2C—O2C—C5C | 120.70 (13) |
C17A—C18A—H18A | 109.5 | Na1C—O3C—Na3C | 89.69 (5) |
C17A—C18A—H18B | 109.5 | Na1C—O3C—Li1C | 83.83 (10) |
C17A—C18A—H18C | 109.5 | Na1C—O3C—C9C | 126.02 (10) |
H18A—C18A—H18B | 109.5 | Na3C—O3C—Li1C | 82.68 (10) |
H18A—C18A—H18C | 109.5 | Na3C—O3C—C9C | 136.31 (10) |
H18B—C18A—H18C | 109.5 | Li1C—O3C—C9C | 121.19 (14) |
C17A—C19A—H19A | 109.5 | Na2C—O4C—Na4C | 89.60 (4) |
C17A—C19A—H19B | 109.5 | Na2C—O4C—Li2C | 83.63 (10) |
C17A—C19A—H19C | 109.5 | Na2C—O4C—C13C | 127.70 (10) |
H19A—C19A—H19B | 109.5 | Na4C—O4C—Li2C | 83.44 (10) |
H19A—C19A—H19C | 109.5 | Na4C—O4C—C13C | 134.32 (11) |
H19B—C19A—H19C | 109.5 | Li2C—O4C—C13C | 121.41 (14) |
C17A—C20A—H20A | 109.5 | Na1C—O5C—Na4C | 90.50 (5) |
C17A—C20A—H20B | 109.5 | Na1C—O5C—Li3C | 84.61 (10) |
C17A—C20A—H20C | 109.5 | Na1C—O5C—C17C | 129.36 (10) |
H20A—C20A—H20B | 109.5 | Na4C—O5C—Li3C | 82.57 (10) |
H20A—C20A—H20C | 109.5 | Na4C—O5C—C17C | 134.33 (10) |
H20B—C20A—H20C | 109.5 | Li3C—O5C—C17C | 117.78 (13) |
O6A—C21A—C22A | 109.94 (16) | Na2C—O6C—Na3C | 88.86 (4) |
O6A—C21A—C23A | 110.69 (15) | Na2C—O6C—Li4C | 83.71 (10) |
O6A—C21A—C24A | 110.45 (15) | Na2C—O6C—C21C | 128.31 (11) |
C22A—C21A—C23A | 109.15 (19) | Na3C—O6C—Li4C | 82.92 (10) |
C22A—C21A—C24A | 108.64 (18) | Na3C—O6C—C21C | 134.71 (11) |
C23A—C21A—C24A | 107.91 (17) | Li4C—O6C—C21C | 121.18 (14) |
C21A—C22A—H22A | 109.5 | Na2C—O7C—Na4C | 80.54 (4) |
C21A—C22A—H22B | 109.5 | Na2C—O7C—Li3C | 125.83 (10) |
C21A—C22A—H22C | 109.5 | Na2C—O7C—Li4C | 75.69 (10) |
H22A—C22A—H22B | 109.5 | Na2C—O7C—C25C | 112.65 (9) |
H22A—C22A—H22C | 109.5 | Na4C—O7C—Li3C | 77.30 (9) |
H22B—C22A—H22C | 109.5 | Na4C—O7C—Li4C | 126.83 (10) |
C21A—C23A—H23A | 109.5 | Na4C—O7C—C25C | 111.82 (9) |
C21A—C23A—H23B | 109.5 | Li3C—O7C—Li4C | 79.44 (13) |
C21A—C23A—H23C | 109.5 | Li3C—O7C—C25C | 121.43 (13) |
H23A—C23A—H23B | 109.5 | Li4C—O7C—C25C | 121.14 (13) |
H23A—C23A—H23C | 109.5 | Na1C—O8C—Na3C | 80.38 (4) |
H23B—C23A—H23C | 109.5 | Na1C—O8C—Li3C | 74.98 (9) |
C21A—C24A—H24A | 109.5 | Na1C—O8C—Li4C | 126.36 (10) |
C21A—C24A—H24B | 109.5 | Na1C—O8C—C29C | 114.38 (9) |
C21A—C24A—H24C | 109.5 | Na3C—O8C—Li3C | 125.86 (10) |
H24A—C24A—H24B | 109.5 | Na3C—O8C—Li4C | 77.83 (10) |
H24A—C24A—H24C | 109.5 | Na3C—O8C—C29C | 111.81 (10) |
H24B—C24A—H24C | 109.5 | Li3C—O8C—Li4C | 79.44 (13) |
O7A—C25A—C26A | 109.38 (14) | Li3C—O8C—C29C | 122.20 (14) |
O7A—C25A—C27A | 110.34 (14) | Li4C—O8C—C29C | 119.18 (13) |
O7A—C25A—C28A | 110.42 (14) | O1C—C1C—C2C | 108.87 (14) |
C26A—C25A—C27A | 109.13 (16) | O1C—C1C—C3C | 110.13 (14) |
C26A—C25A—C28A | 108.82 (15) | O1C—C1C—C4C | 110.56 (14) |
C27A—C25A—C28A | 108.71 (15) | C2C—C1C—C3C | 109.40 (16) |
C25A—C26A—H26A | 109.5 | C2C—C1C—C4C | 108.94 (16) |
C25A—C26A—H26B | 109.5 | C3C—C1C—C4C | 108.92 (15) |
C25A—C26A—H26C | 109.5 | C1C—C2C—H2G | 109.5 |
H26A—C26A—H26B | 109.5 | C1C—C2C—H2H | 109.5 |
H26A—C26A—H26C | 109.5 | C1C—C2C—H2I | 109.5 |
H26B—C26A—H26C | 109.5 | H2G—C2C—H2H | 109.5 |
C25A—C27A—H27A | 109.5 | H2G—C2C—H2I | 109.5 |
C25A—C27A—H27B | 109.5 | H2H—C2C—H2I | 109.5 |
C25A—C27A—H27C | 109.5 | C1C—C3C—H3G | 109.5 |
H27A—C27A—H27B | 109.5 | C1C—C3C—H3H | 109.5 |
H27A—C27A—H27C | 109.5 | C1C—C3C—H3I | 109.5 |
H27B—C27A—H27C | 109.5 | H3G—C3C—H3H | 109.5 |
C25A—C28A—H28A | 109.5 | H3G—C3C—H3I | 109.5 |
C25A—C28A—H28B | 109.5 | H3H—C3C—H3I | 109.5 |
C25A—C28A—H28C | 109.5 | C1C—C4C—H4G | 109.5 |
H28A—C28A—H28B | 109.5 | C1C—C4C—H4H | 109.5 |
H28A—C28A—H28C | 109.5 | C1C—C4C—H4I | 109.5 |
H28B—C28A—H28C | 109.5 | H4G—C4C—H4H | 109.5 |
O8A—C29A—C30A | 109.29 (15) | H4G—C4C—H4I | 109.5 |
O8A—C29A—C31A | 110.25 (14) | H4H—C4C—H4I | 109.5 |
O8A—C29A—C32A | 109.98 (15) | O2C—C5C—C6C | 109.19 (15) |
C30A—C29A—C31A | 109.54 (17) | O2C—C5C—C7C | 110.31 (14) |
C30A—C29A—C32A | 109.22 (17) | O2C—C5C—C8C | 110.47 (15) |
C31A—C29A—C32A | 108.54 (17) | C6C—C5C—C7C | 109.14 (17) |
C29A—C30A—H30A | 109.5 | C6C—C5C—C8C | 109.14 (16) |
C29A—C30A—H30B | 109.5 | C7C—C5C—C8C | 108.57 (16) |
C29A—C30A—H30C | 109.5 | C5C—C6C—H6G | 109.5 |
H30A—C30A—H30B | 109.5 | C5C—C6C—H6H | 109.5 |
H30A—C30A—H30C | 109.5 | C5C—C6C—H6I | 109.5 |
H30B—C30A—H30C | 109.5 | H6G—C6C—H6H | 109.5 |
C29A—C31A—H31A | 109.5 | H6G—C6C—H6I | 109.5 |
C29A—C31A—H31B | 109.5 | H6H—C6C—H6I | 109.5 |
C29A—C31A—H31C | 109.5 | C5C—C7C—H7G | 109.5 |
H31A—C31A—H31B | 109.5 | C5C—C7C—H7H | 109.5 |
H31A—C31A—H31C | 109.5 | C5C—C7C—H7I | 109.5 |
H31B—C31A—H31C | 109.5 | H7G—C7C—H7H | 109.5 |
C29A—C32A—H32A | 109.5 | H7G—C7C—H7I | 109.5 |
C29A—C32A—H32B | 109.5 | H7H—C7C—H7I | 109.5 |
C29A—C32A—H32C | 109.5 | C5C—C8C—H8G | 109.5 |
H32A—C32A—H32B | 109.5 | C5C—C8C—H8H | 109.5 |
H32A—C32A—H32C | 109.5 | C5C—C8C—H8I | 109.5 |
H32B—C32A—H32C | 109.5 | H8G—C8C—H8H | 109.5 |
O1B—Na1B—O3B | 81.49 (5) | H8G—C8C—H8I | 109.5 |
O1B—Na1B—O5B | 89.09 (5) | H8H—C8C—H8I | 109.5 |
O1B—Na1B—O7B | 117.51 (4) | O3C—C9C—C10C | 110.25 (15) |
O3B—Na1B—O5B | 160.86 (5) | O3C—C9C—C11C | 110.49 (15) |
O3B—Na1B—O7B | 88.67 (5) | O3C—C9C—C12C | 110.16 (15) |
O5B—Na1B—O7B | 80.92 (5) | C10C—C9C—C11C | 108.81 (16) |
O2B—Na2B—O3B | 81.24 (5) | C10C—C9C—C12C | 108.22 (16) |
O2B—Na2B—O6B | 88.69 (4) | C11C—C9C—C12C | 108.86 (16) |
O2B—Na2B—O7B | 119.05 (4) | C9C—C10C—H10G | 109.5 |
O3B—Na2B—O6B | 161.36 (5) | C9C—C10C—H10H | 109.5 |
O3B—Na2B—O7B | 89.66 (5) | C9C—C10C—H10I | 109.5 |
O6B—Na2B—O7B | 81.54 (5) | H10G—C10C—H10H | 109.5 |
O2B—Na3B—O4B | 81.68 (4) | H10G—C10C—H10I | 109.5 |
O2B—Na3B—O6B | 89.76 (5) | H10H—C10C—H10I | 109.5 |
O2B—Na3B—O8B | 118.51 (4) | C9C—C11C—H11G | 109.5 |
O4B—Na3B—O6B | 162.39 (5) | C9C—C11C—H11H | 109.5 |
O4B—Na3B—O8B | 88.42 (4) | C9C—C11C—H11I | 109.5 |
O6B—Na3B—O8B | 82.16 (4) | H11G—C11C—H11H | 109.5 |
O1B—Na4B—O4B | 81.59 (4) | H11G—C11C—H11I | 109.5 |
O1B—Na4B—O5B | 89.16 (5) | H11H—C11C—H11I | 109.5 |
O1B—Na4B—O8B | 117.43 (4) | C9C—C12C—H12G | 109.5 |
O4B—Na4B—O5B | 162.01 (5) | C9C—C12C—H12H | 109.5 |
O4B—Na4B—O8B | 88.62 (4) | C9C—C12C—H12I | 109.5 |
O5B—Na4B—O8B | 81.98 (4) | H12G—C12C—H12H | 109.5 |
O1B—Li1B—O2B | 98.11 (14) | H12G—C12C—H12I | 109.5 |
O1B—Li1B—O4B | 116.15 (16) | H12H—C12C—H12I | 109.5 |
O2B—Li1B—O4B | 116.70 (17) | O4C—C13C—C14C | 110.25 (15) |
O1B—Li2B—O2B | 97.90 (14) | O4C—C13C—C15C | 109.88 (15) |
O1B—Li2B—O3B | 115.55 (17) | O4C—C13C—C16C | 110.01 (14) |
O2B—Li2B—O3B | 117.93 (17) | C14C—C13C—C15C | 109.47 (16) |
O5B—Li3B—O7B | 118.00 (18) | C14C—C13C—C16C | 109.00 (16) |
O5B—Li3B—O8B | 116.49 (16) | C15C—C13C—C16C | 108.20 (16) |
O7B—Li3B—O8B | 97.74 (15) | C13C—C14C—H14G | 109.5 |
O6B—Li4B—O7B | 117.01 (18) | C13C—C14C—H14H | 109.5 |
O6B—Li4B—O8B | 115.93 (16) | C13C—C14C—H14I | 109.5 |
O7B—Li4B—O8B | 97.72 (15) | H14G—C14C—H14H | 109.5 |
Na1B—O1B—Na4B | 81.09 (4) | H14G—C14C—H14I | 109.5 |
Na1B—O1B—Li1B | 127.75 (11) | H14H—C14C—H14I | 109.5 |
Na1B—O1B—Li2B | 76.59 (10) | C13C—C15C—H15G | 109.5 |
Na1B—O1B—C1B | 112.42 (11) | C13C—C15C—H15H | 109.5 |
Na4B—O1B—Li1B | 77.29 (10) | C13C—C15C—H15I | 109.5 |
Na4B—O1B—Li2B | 126.32 (11) | H15G—C15C—H15H | 109.5 |
Na4B—O1B—C1B | 111.61 (10) | H15G—C15C—H15I | 109.5 |
Li1B—O1B—Li2B | 79.17 (13) | H15H—C15C—H15I | 109.5 |
Li1B—O1B—C1B | 119.71 (15) | C13C—C16C—H16G | 109.5 |
Li2B—O1B—C1B | 121.99 (14) | C13C—C16C—H16H | 109.5 |
Na2B—O2B—Na3B | 79.94 (4) | C13C—C16C—H16I | 109.5 |
Na2B—O2B—Li1B | 125.72 (10) | H16G—C16C—H16H | 109.5 |
Na2B—O2B—Li2B | 75.58 (10) | H16G—C16C—H16I | 109.5 |
Na2B—O2B—C5B | 112.90 (9) | H16H—C16C—H16I | 109.5 |
Na3B—O2B—Li1B | 77.09 (10) | O5C—C17C—C18C | 110.10 (15) |
Na3B—O2B—Li2B | 125.38 (11) | O5C—C17C—C19C | 110.37 (14) |
Na3B—O2B—C5B | 111.87 (10) | O5C—C17C—C20C | 109.71 (14) |
Li1B—O2B—Li2B | 79.05 (13) | C18C—C17C—C19C | 108.97 (15) |
Li1B—O2B—C5B | 121.23 (13) | C18C—C17C—C20C | 108.97 (15) |
Li2B—O2B—C5B | 122.54 (14) | C19C—C17C—C20C | 108.69 (15) |
Na1B—O3B—Na2B | 90.77 (5) | C17C—C18C—H18G | 109.5 |
Na1B—O3B—Li2B | 84.76 (11) | C17C—C18C—H18H | 109.5 |
Na1B—O3B—C9B | 134.73 (11) | C17C—C18C—H18I | 109.5 |
Na2B—O3B—Li2B | 83.72 (11) | H18G—C18C—H18H | 109.5 |
Na2B—O3B—C9B | 127.31 (11) | H18G—C18C—H18I | 109.5 |
Li2B—O3B—C9B | 118.91 (15) | H18H—C18C—H18I | 109.5 |
Na3B—O4B—Na4B | 88.56 (4) | C17C—C19C—H19G | 109.5 |
Na3B—O4B—Li1B | 82.57 (10) | C17C—C19C—H19H | 109.5 |
Na3B—O4B—C13B | 130.72 (11) | C17C—C19C—H19I | 109.5 |
Na4B—O4B—Li1B | 83.17 (10) | H19G—C19C—H19H | 109.5 |
Na4B—O4B—C13B | 135.41 (11) | H19G—C19C—H19I | 109.5 |
Li1B—O4B—C13B | 117.40 (14) | H19H—C19C—H19I | 109.5 |
Na1B—O5B—Na4B | 89.32 (5) | C17C—C20C—H20G | 109.5 |
Na1B—O5B—Li3B | 84.01 (11) | C17C—C20C—H20H | 109.5 |
Na1B—O5B—C17B | 130.29 (11) | C17C—C20C—H20I | 109.5 |
Na4B—O5B—Li3B | 82.74 (10) | H20G—C20C—H20H | 109.5 |
Na4B—O5B—C17B | 131.56 (11) | H20G—C20C—H20I | 109.5 |
Li3B—O5B—C17B | 122.28 (15) | H20H—C20C—H20I | 109.5 |
Na2B—O6B—Na3B | 88.84 (5) | O6C—C21C—C22C | 109.73 (14) |
Na2B—O6B—Li4B | 83.26 (11) | O6C—C21C—C23C | 110.32 (15) |
Na2B—O6B—C21B | 129.01 (11) | O6C—C21C—C24C | 110.14 (15) |
Na3B—O6B—Li4B | 82.89 (10) | C22C—C21C—C23C | 108.75 (17) |
Na3B—O6B—C21B | 134.99 (11) | C22C—C21C—C24C | 108.57 (16) |
Li4B—O6B—C21B | 120.13 (14) | C23C—C21C—C24C | 109.30 (16) |
Na1B—O7B—Na2B | 79.27 (4) | C21C—C22C—H22G | 109.5 |
Na1B—O7B—Li3B | 74.77 (11) | C21C—C22C—H22H | 109.5 |
Na1B—O7B—Li4B | 124.68 (10) | C21C—C22C—H22I | 109.5 |
Na1B—O7B—C25B | 110.74 (11) | H22G—C22C—H22H | 109.5 |
Na2B—O7B—Li3B | 124.16 (10) | H22G—C22C—H22I | 109.5 |
Na2B—O7B—Li4B | 75.96 (10) | H22H—C22C—H22I | 109.5 |
Na2B—O7B—C25B | 113.26 (10) | C21C—C23C—H23G | 109.5 |
Li3B—O7B—Li4B | 79.76 (14) | C21C—C23C—H23H | 109.5 |
Li3B—O7B—C25B | 121.98 (14) | C21C—C23C—H23I | 109.5 |
Li4B—O7B—C25B | 124.40 (15) | H23G—C23C—H23H | 109.5 |
Na3B—O8B—Na4B | 82.11 (4) | H23G—C23C—H23I | 109.5 |
Na3B—O8B—Li3B | 127.85 (11) | H23H—C23C—H23I | 109.5 |
Na3B—O8B—Li4B | 77.69 (10) | C21C—C24C—H24G | 109.5 |
Na3B—O8B—C29B | 111.93 (10) | C21C—C24C—H24H | 109.5 |
Na4B—O8B—Li3B | 77.40 (10) | C21C—C24C—H24I | 109.5 |
Na4B—O8B—Li4B | 128.77 (11) | H24G—C24C—H24H | 109.5 |
Na4B—O8B—C29B | 110.91 (10) | H24G—C24C—H24I | 109.5 |
Li3B—O8B—Li4B | 79.00 (13) | H24H—C24C—H24I | 109.5 |
Li3B—O8B—C29B | 120.14 (14) | O7C—C25C—C26C | 110.38 (14) |
Li4B—O8B—C29B | 120.28 (14) | O7C—C25C—C27C | 109.50 (14) |
O1B—C1B—C2B | 109.24 (17) | O7C—C25C—C28C | 110.44 (14) |
O1B—C1B—C3B | 109.89 (18) | C26C—C25C—C27C | 108.94 (16) |
O1B—C1B—C4B | 110.12 (16) | C26C—C25C—C28C | 108.40 (16) |
C2B—C1B—C3B | 108.99 (19) | C27C—C25C—C28C | 109.15 (15) |
C2B—C1B—C4B | 109.02 (19) | C25C—C26C—H26G | 109.5 |
C3B—C1B—C4B | 109.55 (19) | C25C—C26C—H26H | 109.5 |
C1B—C2B—H2D | 109.5 | C25C—C26C—H26I | 109.5 |
C1B—C2B—H2E | 109.5 | H26G—C26C—H26H | 109.5 |
C1B—C2B—H2F | 109.5 | H26G—C26C—H26I | 109.5 |
H2D—C2B—H2E | 109.5 | H26H—C26C—H26I | 109.5 |
H2D—C2B—H2F | 109.5 | C25C—C27C—H27G | 109.5 |
H2E—C2B—H2F | 109.5 | C25C—C27C—H27H | 109.5 |
C1B—C3B—H3D | 109.5 | C25C—C27C—H27I | 109.5 |
C1B—C3B—H3E | 109.5 | H27G—C27C—H27H | 109.5 |
C1B—C3B—H3F | 109.5 | H27G—C27C—H27I | 109.5 |
H3D—C3B—H3E | 109.5 | H27H—C27C—H27I | 109.5 |
H3D—C3B—H3F | 109.5 | C25C—C28C—H28G | 109.5 |
H3E—C3B—H3F | 109.5 | C25C—C28C—H28H | 109.5 |
C1B—C4B—H4D | 109.5 | C25C—C28C—H28I | 109.5 |
C1B—C4B—H4E | 109.5 | H28G—C28C—H28H | 109.5 |
C1B—C4B—H4F | 109.5 | H28G—C28C—H28I | 109.5 |
H4D—C4B—H4E | 109.5 | H28H—C28C—H28I | 109.5 |
H4D—C4B—H4F | 109.5 | O8C—C29C—C30C | 110.24 (15) |
H4E—C4B—H4F | 109.5 | O8C—C29C—C31C | 109.32 (15) |
O2B—C5B—C6B | 109.88 (15) | O8C—C29C—C32C | 110.43 (15) |
O2B—C5B—C7B | 110.38 (15) | C30C—C29C—C31C | 108.86 (17) |
O2B—C5B—C8B | 110.21 (15) | C30C—C29C—C32C | 108.64 (16) |
C6B—C5B—C7B | 108.80 (16) | C31C—C29C—C32C | 109.33 (17) |
C6B—C5B—C8B | 109.34 (17) | C29C—C30C—H30G | 109.5 |
C7B—C5B—C8B | 108.19 (16) | C29C—C30C—H30H | 109.5 |
C5B—C6B—H6D | 109.5 | C29C—C30C—H30I | 109.5 |
C5B—C6B—H6E | 109.5 | H30G—C30C—H30H | 109.5 |
C5B—C6B—H6F | 109.5 | H30G—C30C—H30I | 109.5 |
H6D—C6B—H6E | 109.5 | H30H—C30C—H30I | 109.5 |
H6D—C6B—H6F | 109.5 | C29C—C31C—H31G | 109.5 |
H6E—C6B—H6F | 109.5 | C29C—C31C—H31H | 109.5 |
C5B—C7B—H7D | 109.5 | C29C—C31C—H31I | 109.5 |
C5B—C7B—H7E | 109.5 | H31G—C31C—H31H | 109.5 |
C5B—C7B—H7F | 109.5 | H31G—C31C—H31I | 109.5 |
H7D—C7B—H7E | 109.5 | H31H—C31C—H31I | 109.5 |
H7D—C7B—H7F | 109.5 | C29C—C32C—H32G | 109.5 |
H7E—C7B—H7F | 109.5 | C29C—C32C—H32H | 109.5 |
C5B—C8B—H8D | 109.5 | C29C—C32C—H32I | 109.5 |
C5B—C8B—H8E | 109.5 | H32G—C32C—H32H | 109.5 |
C5B—C8B—H8F | 109.5 | H32G—C32C—H32I | 109.5 |
H8D—C8B—H8E | 109.5 | H32H—C32C—H32I | 109.5 |
Experimental details
Crystal data | |
Chemical formula | [Li4Na4(C4H9O)8] |
Mr | 704.62 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 160 |
a, b, c (Å) | 11.1917 (8), 21.0007 (14), 29.450 (2) |
α, β, γ (°) | 82.560 (2), 89.492 (2), 82.033 (2) |
V (Å3) | 6796.8 (8) |
Z | 6 |
Radiation type | Mo Kα |
µ (mm−1) | 0.10 |
Crystal size (mm) | 0.82 × 0.80 × 0.80 |
Data collection | |
Diffractometer | Bruker SMART 1K CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2002) |
Tmin, Tmax | 0.890, 0.950 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 32571, 22410, 15221 |
Rint | 0.017 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.094, 0.92 |
No. of reflections | 22410 |
No. of parameters | 1370 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.18, −0.20 |
Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2001), SHELXTL and local programs.
Na1A—O1A | 2.5184 (13) | Na4B—O5B | 2.3481 (13) |
Na1A—O3A | 2.3200 (12) | Na4B—O8B | 2.4916 (13) |
Na1A—O5A | 2.3104 (12) | Li1B—O1B | 1.890 (3) |
Na1A—O7A | 2.5205 (13) | Li1B—O2B | 1.902 (3) |
Na2A—O2A | 2.5289 (13) | Li1B—O4B | 1.824 (3) |
Na2A—O3A | 2.3320 (13) | Li2B—O1B | 1.903 (3) |
Na2A—O6A | 2.3136 (13) | Li2B—O2B | 1.895 (3) |
Na2A—O7A | 2.5100 (12) | Li2B—O3B | 1.828 (3) |
Na3A—O2A | 2.5000 (13) | Li3B—O5B | 1.828 (3) |
Na3A—O4A | 2.3285 (13) | Li3B—O7B | 1.897 (3) |
Na3A—O6A | 2.3426 (13) | Li3B—O8B | 1.907 (3) |
Na3A—O8A | 2.5341 (12) | Li4B—O6B | 1.827 (3) |
Na4A—O1A | 2.5125 (13) | Li4B—O7B | 1.892 (3) |
Na4A—O4A | 2.3177 (13) | Li4B—O8B | 1.913 (3) |
Na4A—O5A | 2.3071 (13) | Na1C—O1C | 2.5776 (13) |
Na4A—O8A | 2.5151 (13) | Na1C—O3C | 2.2890 (13) |
Li1A—O1A | 1.897 (3) | Na1C—O5C | 2.2704 (13) |
Li1A—O2A | 1.906 (3) | Na1C—O8C | 2.5882 (13) |
Li1A—O3A | 1.839 (3) | Na2C—O2C | 2.5332 (13) |
Li2A—O1A | 1.887 (3) | Na2C—O4C | 2.3113 (13) |
Li2A—O2A | 1.892 (3) | Na2C—O6C | 2.3137 (13) |
Li2A—O4A | 1.846 (3) | Na2C—O7C | 2.5628 (13) |
Li3A—O5A | 1.843 (3) | Na3C—O2C | 2.5041 (13) |
Li3A—O7A | 1.896 (3) | Na3C—O3C | 2.3574 (13) |
Li3A—O8A | 1.895 (3) | Na3C—O6C | 2.3526 (13) |
Li4A—O6A | 1.834 (3) | Na3C—O8C | 2.4887 (13) |
Li4A—O7A | 1.898 (3) | Na4C—O1C | 2.4985 (13) |
Li4A—O8A | 1.896 (3) | Na4C—O4C | 2.3276 (13) |
Na1B—O1B | 2.5372 (14) | Na4C—O5C | 2.3395 (13) |
Na1B—O3B | 2.2895 (14) | Na4C—O7C | 2.4934 (12) |
Na1B—O5B | 2.3059 (14) | Li1C—O1C | 1.893 (3) |
Na1B—O7B | 2.6030 (15) | Li1C—O2C | 1.908 (3) |
Na2B—O2B | 2.5735 (13) | Li1C—O3C | 1.833 (3) |
Na2B—O3B | 2.3178 (14) | Li2C—O1C | 1.893 (3) |
Na2B—O6B | 2.3112 (14) | Li2C—O2C | 1.899 (3) |
Na2B—O7B | 2.5375 (14) | Li2C—O4C | 1.824 (3) |
Na3B—O2B | 2.4986 (13) | Li3C—O5C | 1.836 (3) |
Na3B—O4B | 2.3491 (13) | Li3C—O7C | 1.896 (3) |
Na3B—O6B | 2.3449 (13) | Li3C—O8C | 1.893 (3) |
Na3B—O8B | 2.4775 (13) | Li4C—O6C | 1.827 (3) |
Na4B—O1B | 2.4955 (13) | Li4C—O7C | 1.898 (3) |
Na4B—O4B | 2.3251 (13) | Li4C—O8C | 1.901 (3) |
We recently reported the structures of the complete series of compounds [Li4M4(tBuO)8], where M is Na, K, Rb and Cs (Clegg et al., 1999; Armstrong et al., 2000). Despite the differences in atomic size of the four heavier alkali metals, all the compounds have the same basic molecular structure, which is a tetramer with a `breastplate-like' appearance, having a planar and essentially square arrangement of four M+ ions sandwiched between two {(tBuO)4Li2}2− dianions, the overall molecular symmetry being 42m (D2 d). This common structure for all the compounds contrasts with the variety found for the homometallic tert-butoxides: those of K, Rb and Cs are tetrameric (Weiss et al., 1967, 1968; Chisholm et al., 1991; Mann & Jansen, 1994), the Li compound is hexameric (Thomas et al., 1998), and the Na compound is both hexameric and nonameric in the same crystal structure (Davies et al., 1982); none of them has an octanuclear structure. There appears to be no precedent for a complete set of homologous alkali metal complexes with the same molecular architecture, and these compounds are unusual in metal alkoxide chemistry generally (Bradley et al., 2001).
During experiments to confirm the reproducibility of the syntheses of these compounds, preparation of the mixed lithium–sodium complex by essentially the same route as previously reported led to crystals with a noticeably different habit. Preliminary X-ray diffraction indicated a different unit cell, and so we determined the crystal structure in full. The result is a second polymorphic modification of the compound. Like the previously reported form, it is unsolvated. This structure is triclinic, with three molecules in the asymmetric unit, whereas the other is monoclinic, with two molecules in the asymmetric unit. One molecule of the triclinic form is shown in Fig. 1, with generic atom labels; atoms of the three independent molecules are identified by a suffix A, B or C. Bond distances for the metal ions are given in Table 1.
There are no chemically significant differences among the three crystallographically independent molecules of this triclinic polymorph, or indeed within the whole set of molecules of both polymorphs. In each case, Li+ cations are coordinated by three tert-butoxy ligands in a trigonal pyramidal arrangement, and Na+ cations have a highly distorted fourfold coordination geometry. Half the ligands are triply bridging (to one Li+ and two Na+) and half are quadruply bridging (to two Li+ and two Na+). Li—O bond lengths range from 1.824 (3) to 1.913 (3) Å, while Na—O bond lengths cover the rather wider range 2.2704 (13)–2.6030 (15) Å, each Na+ ion having two shorter and two longer bonds, to µ3– and µ4-O atoms, respectively. In the homometallic tert-butoxy oligomers, all ligands are triply bridging. Further details of the molecular structures, together with theoretical calculations for comparison, are discussed by Armstrong et al. (2000).
There are no significant intermolecular interactions. The molecules are effectively covered by a sheath of H atoms and are essentially close packed (Fig. 2).