Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807010100/hb2311sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807010100/hb2311Isup2.hkl |
CCDC reference: 643006
Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 and PLATON.
[Na4(P14)(C4H10O2)8] | F(000) = 1308 |
Mr = 1246.50 | Dx = 1.300 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6420 reflections |
a = 12.444 (2) Å | θ = 3.5–25.2° |
b = 20.264 (3) Å | µ = 0.45 mm−1 |
c = 12.874 (2) Å | T = 173 K |
β = 101.32 (1)° | Cut needle, yellow |
V = 3183.2 (9) Å3 | 0.26 × 0.14 × 0.13 mm |
Z = 2 |
Stoe IPDSII two-circle diffractometer | 5581 independent reflections |
Radiation source: fine-focus sealed tube | 2557 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.090 |
ω scans | θmax = 25.1°, θmin = 3.5° |
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995) | h = −14→14 |
Tmin = 0.892, Tmax = 0.944 | k = −24→24 |
9106 measured reflections | l = −15→11 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.068 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H-atom parameters constrained |
S = 0.89 | w = 1/[σ2(Fo2) + (0.02P)2] where P = (Fo2 + 2Fc2)/3 |
5581 reflections | (Δ/σ)max < 0.001 |
298 parameters | Δρmax = 0.32 e Å−3 |
0 restraints | Δρmin = −0.29 e Å−3 |
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 | 0.71143 (18) | 0.37461 (13) | 0.1408 (2) | 0.0496 (7) | |
Na2 | 0.83111 (16) | 0.60389 (11) | 0.6357 (2) | 0.0428 (6) | |
P1 | 0.93175 (13) | 0.58077 (8) | 0.34493 (17) | 0.0462 (4) | |
P2 | 0.93465 (13) | 0.51308 (10) | 0.20687 (16) | 0.0525 (5) | |
P3 | 0.93641 (12) | 0.41337 (9) | 0.26492 (16) | 0.0453 (5) | |
P4 | 0.83808 (12) | 0.42619 (8) | 0.38504 (14) | 0.0379 (4) | |
P5 | 0.91180 (11) | 0.51427 (9) | 0.47426 (14) | 0.0364 (4) | |
P6 | 0.77460 (13) | 0.55614 (9) | 0.23084 (17) | 0.0510 (5) | |
P7 | 0.69360 (11) | 0.47926 (9) | 0.30377 (15) | 0.0430 (4) | |
C1 | 0.8413 (7) | 0.2517 (5) | 0.0411 (10) | 0.114 (4) | |
H1A | 0.8327 | 0.2835 | −0.0172 | 0.171* | |
H1B | 0.8342 | 0.2067 | 0.0124 | 0.171* | |
H1C | 0.9137 | 0.2571 | 0.0866 | 0.171* | |
O2 | 0.7599 (6) | 0.2627 (3) | 0.1008 (7) | 0.100 (2) | |
C3 | 0.7613 (8) | 0.2214 (5) | 0.1838 (13) | 0.131 (6) | |
H3A | 0.8332 | 0.2261 | 0.2323 | 0.158* | |
H3B | 0.7569 | 0.1756 | 0.1564 | 0.158* | |
C4 | 0.6786 (11) | 0.2293 (5) | 0.2443 (10) | 0.112 (4) | |
H4A | 0.6181 | 0.1986 | 0.2157 | 0.135* | |
H4B | 0.7093 | 0.2151 | 0.3177 | 0.135* | |
O5 | 0.6363 (5) | 0.2884 (3) | 0.2487 (7) | 0.102 (2) | |
C6 | 0.5682 (8) | 0.2984 (5) | 0.3196 (9) | 0.104 (3) | |
H6A | 0.5417 | 0.3441 | 0.3142 | 0.157* | |
H6B | 0.6087 | 0.2901 | 0.3917 | 0.157* | |
H6C | 0.5056 | 0.2682 | 0.3034 | 0.157* | |
C11 | 0.9508 (7) | 0.7460 (5) | 0.6092 (11) | 0.147 (6) | |
H11A | 0.9806 | 0.7235 | 0.5537 | 0.221* | |
H11B | 0.9974 | 0.7368 | 0.6783 | 0.221* | |
H11C | 0.9488 | 0.7937 | 0.5962 | 0.221* | |
O12 | 0.8432 (4) | 0.7227 (3) | 0.6084 (6) | 0.0789 (18) | |
C13 | 0.7897 (10) | 0.7520 (5) | 0.6842 (12) | 0.125 (5) | |
H13A | 0.7096 | 0.7462 | 0.6603 | 0.150* | |
H13B | 0.8049 | 0.8000 | 0.6864 | 0.150* | |
C14 | 0.8222 (9) | 0.7248 (6) | 0.7944 (11) | 0.119 (5) | |
H14A | 0.9024 | 0.7292 | 0.8193 | 0.143* | |
H14B | 0.7852 | 0.7498 | 0.8434 | 0.143* | |
O15 | 0.7924 (4) | 0.6587 (3) | 0.7937 (5) | 0.0669 (16) | |
C16 | 0.8341 (7) | 0.6277 (5) | 0.8928 (8) | 0.090 (3) | |
H16A | 0.8121 | 0.5812 | 0.8893 | 0.135* | |
H16B | 0.8047 | 0.6499 | 0.9489 | 0.135* | |
H16C | 0.9143 | 0.6307 | 0.9084 | 0.135* | |
C21 | 0.4411 (5) | 0.3576 (4) | 0.0220 (8) | 0.083 (3) | |
H21A | 0.4426 | 0.3391 | 0.0926 | 0.125* | |
H21B | 0.4349 | 0.3217 | −0.0299 | 0.125* | |
H21C | 0.3781 | 0.3872 | 0.0031 | 0.125* | |
O22 | 0.5388 (3) | 0.3932 (3) | 0.0222 (4) | 0.0618 (14) | |
C23 | 0.5451 (5) | 0.4220 (4) | −0.0758 (6) | 0.066 (2) | |
H23A | 0.4864 | 0.4553 | −0.0950 | 0.079* | |
H23B | 0.5349 | 0.3878 | −0.1317 | 0.079* | |
C24 | 0.6527 (6) | 0.4535 (4) | −0.0682 (7) | 0.069 (2) | |
H24A | 0.6565 | 0.4748 | −0.1365 | 0.083* | |
H24B | 0.6620 | 0.4882 | −0.0129 | 0.083* | |
O25 | 0.7376 (3) | 0.4069 (3) | −0.0429 (4) | 0.0662 (15) | |
C26 | 0.8425 (6) | 0.4307 (5) | −0.0602 (7) | 0.087 (3) | |
H26A | 0.8978 | 0.3960 | −0.0415 | 0.130* | |
H26B | 0.8644 | 0.4696 | −0.0158 | 0.130* | |
H26C | 0.8364 | 0.4426 | −0.1349 | 0.130* | |
C31 | 0.7259 (5) | 0.4541 (3) | 0.6451 (7) | 0.057 (2) | |
H31A | 0.8026 | 0.4398 | 0.6626 | 0.085* | |
H31B | 0.7010 | 0.4542 | 0.5680 | 0.085* | |
H31C | 0.6805 | 0.4236 | 0.6770 | 0.085* | |
O32 | 0.7166 (3) | 0.5186 (2) | 0.6851 (4) | 0.0451 (11) | |
C33 | 0.6065 (4) | 0.5427 (3) | 0.6607 (6) | 0.052 (2) | |
H33A | 0.5975 | 0.5774 | 0.7125 | 0.062* | |
H33B | 0.5557 | 0.5063 | 0.6682 | 0.062* | |
C34 | 0.5759 (4) | 0.5706 (3) | 0.5512 (6) | 0.0516 (19) | |
H34A | 0.5876 | 0.5373 | 0.4983 | 0.062* | |
H34B | 0.4977 | 0.5836 | 0.5360 | 0.062* | |
O35 | 0.6438 (3) | 0.6271 (2) | 0.5459 (4) | 0.0516 (13) | |
C36 | 0.6216 (6) | 0.6576 (4) | 0.4445 (7) | 0.070 (2) | |
H36A | 0.6700 | 0.6957 | 0.4446 | 0.104* | |
H36B | 0.5451 | 0.6721 | 0.4281 | 0.104* | |
H36C | 0.6346 | 0.6258 | 0.3908 | 0.104* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Na1 | 0.0419 (12) | 0.0569 (16) | 0.0454 (19) | 0.0001 (12) | −0.0029 (11) | −0.0058 (14) |
Na2 | 0.0320 (11) | 0.0456 (14) | 0.0496 (18) | −0.0006 (10) | 0.0044 (11) | −0.0067 (13) |
P1 | 0.0433 (8) | 0.0382 (9) | 0.0508 (12) | −0.0062 (8) | −0.0062 (8) | 0.0030 (10) |
P2 | 0.0420 (9) | 0.0753 (13) | 0.0388 (12) | −0.0129 (9) | 0.0045 (8) | 0.0016 (11) |
P3 | 0.0298 (7) | 0.0562 (11) | 0.0469 (12) | 0.0055 (7) | 0.0000 (7) | −0.0164 (10) |
P4 | 0.0352 (7) | 0.0387 (9) | 0.0376 (11) | −0.0025 (7) | 0.0016 (7) | −0.0006 (8) |
P5 | 0.0304 (7) | 0.0425 (9) | 0.0349 (10) | 0.0018 (7) | 0.0029 (7) | −0.0048 (9) |
P6 | 0.0462 (9) | 0.0468 (10) | 0.0520 (13) | 0.0042 (8) | −0.0098 (9) | 0.0065 (10) |
P7 | 0.0285 (7) | 0.0518 (10) | 0.0462 (12) | 0.0025 (7) | 0.0011 (7) | −0.0064 (10) |
C1 | 0.079 (6) | 0.106 (8) | 0.154 (13) | 0.007 (6) | 0.015 (7) | −0.034 (8) |
O2 | 0.121 (5) | 0.071 (4) | 0.113 (7) | 0.013 (4) | 0.036 (5) | −0.015 (4) |
C3 | 0.086 (7) | 0.070 (7) | 0.238 (19) | 0.002 (6) | 0.033 (9) | 0.051 (9) |
C4 | 0.142 (10) | 0.080 (8) | 0.115 (11) | 0.008 (7) | 0.027 (8) | 0.004 (7) |
O5 | 0.116 (5) | 0.066 (4) | 0.137 (7) | 0.021 (4) | 0.057 (5) | 0.032 (4) |
C6 | 0.108 (7) | 0.109 (8) | 0.101 (10) | 0.008 (6) | 0.030 (7) | 0.027 (7) |
C11 | 0.087 (7) | 0.140 (10) | 0.190 (14) | −0.057 (7) | −0.036 (7) | 0.113 (9) |
O12 | 0.074 (3) | 0.054 (3) | 0.100 (5) | −0.010 (3) | −0.005 (3) | 0.007 (3) |
C13 | 0.139 (10) | 0.052 (6) | 0.162 (15) | 0.020 (6) | −0.021 (10) | −0.033 (8) |
C14 | 0.115 (8) | 0.111 (9) | 0.131 (13) | −0.005 (7) | 0.025 (8) | −0.077 (9) |
O15 | 0.056 (3) | 0.070 (4) | 0.077 (5) | −0.005 (3) | 0.018 (3) | −0.030 (3) |
C16 | 0.075 (5) | 0.140 (9) | 0.055 (7) | −0.011 (6) | 0.012 (5) | −0.021 (7) |
C21 | 0.046 (4) | 0.094 (6) | 0.102 (8) | −0.015 (4) | −0.003 (4) | 0.015 (6) |
O22 | 0.045 (2) | 0.080 (3) | 0.054 (4) | −0.009 (2) | −0.007 (2) | 0.010 (3) |
C23 | 0.050 (4) | 0.095 (6) | 0.045 (5) | 0.019 (4) | −0.008 (3) | 0.005 (5) |
C24 | 0.083 (5) | 0.074 (5) | 0.053 (6) | 0.010 (4) | 0.018 (4) | 0.017 (5) |
O25 | 0.049 (3) | 0.084 (4) | 0.063 (4) | 0.001 (3) | 0.005 (2) | 0.008 (3) |
C26 | 0.057 (4) | 0.144 (9) | 0.055 (6) | −0.015 (5) | −0.001 (4) | 0.001 (6) |
C31 | 0.050 (4) | 0.051 (4) | 0.069 (6) | −0.008 (3) | 0.012 (4) | −0.001 (4) |
O32 | 0.034 (2) | 0.050 (3) | 0.050 (3) | −0.003 (2) | 0.0066 (19) | −0.007 (3) |
C33 | 0.032 (3) | 0.061 (4) | 0.063 (6) | −0.007 (3) | 0.009 (3) | −0.017 (4) |
C34 | 0.029 (3) | 0.065 (5) | 0.057 (5) | −0.005 (3) | −0.002 (3) | −0.006 (4) |
O35 | 0.041 (2) | 0.053 (3) | 0.056 (4) | −0.004 (2) | −0.001 (2) | −0.003 (3) |
C36 | 0.073 (5) | 0.073 (5) | 0.056 (6) | 0.005 (4) | −0.005 (4) | 0.009 (5) |
Na1—O22 | 2.408 (5) | O12—C13 | 1.415 (14) |
Na1—O2 | 2.428 (7) | C13—C14 | 1.502 (16) |
Na1—O5 | 2.522 (7) | C13—H13A | 0.9900 |
Na1—O25 | 2.536 (6) | C13—H13B | 0.9900 |
Na1—P7 | 3.022 (3) | C14—O15 | 1.390 (11) |
Na1—P3 | 3.042 (3) | C14—H14A | 0.9900 |
Na2—O32 | 2.405 (5) | C14—H14B | 0.9900 |
Na2—O35 | 2.436 (5) | O15—C16 | 1.425 (10) |
Na2—O12 | 2.443 (6) | C16—H16A | 0.9800 |
Na2—O15 | 2.447 (6) | C16—H16B | 0.9800 |
Na2—P3i | 2.945 (3) | C16—H16C | 0.9800 |
Na2—P5 | 3.073 (3) | C21—O22 | 1.415 (7) |
P1—P5 | 2.194 (3) | C21—H21A | 0.9800 |
P1—P2 | 2.251 (3) | C21—H21B | 0.9800 |
P1—P6 | 2.259 (2) | C21—H21C | 0.9800 |
P2—P3 | 2.153 (3) | O22—C23 | 1.406 (8) |
P2—P6 | 2.250 (3) | C23—C24 | 1.468 (9) |
P3—P4 | 2.168 (2) | C23—H23A | 0.9900 |
P4—P7 | 2.178 (2) | C23—H23B | 0.9900 |
P4—P5 | 2.221 (2) | C24—O25 | 1.408 (8) |
P5—P5i | 2.241 (3) | C24—H24A | 0.9900 |
P6—P7 | 2.167 (3) | C24—H24B | 0.9900 |
P3—Na2i | 2.945 (3) | O25—C26 | 1.449 (8) |
C1—O2 | 1.404 (11) | C26—H26A | 0.9800 |
C1—H1A | 0.9800 | C26—H26B | 0.9800 |
C1—H1B | 0.9800 | C26—H26C | 0.9800 |
C1—H1C | 0.9800 | C31—O32 | 1.418 (7) |
O2—C3 | 1.354 (13) | C31—H31A | 0.9800 |
C3—C4 | 1.416 (14) | C31—H31B | 0.9800 |
C3—H3A | 0.9900 | C31—H31C | 0.9800 |
C3—H3B | 0.9900 | O32—C33 | 1.430 (6) |
C4—O5 | 1.315 (11) | C33—C34 | 1.497 (10) |
C4—H4A | 0.9900 | C33—H33A | 0.9900 |
C4—H4B | 0.9900 | C33—H33B | 0.9900 |
O5—C6 | 1.377 (11) | C34—O35 | 1.432 (7) |
C6—H6A | 0.9800 | C34—H34A | 0.9900 |
C6—H6B | 0.9800 | C34—H34B | 0.9900 |
C6—H6C | 0.9800 | O35—C36 | 1.422 (9) |
C11—O12 | 1.418 (9) | C36—H36A | 0.9800 |
C11—H11A | 0.9800 | C36—H36B | 0.9800 |
C11—H11B | 0.9800 | C36—H36C | 0.9800 |
C11—H11C | 0.9800 | ||
O22—Na1—O2 | 103.9 (2) | H11A—C11—H11B | 109.5 |
O22—Na1—O5 | 94.4 (2) | O12—C11—H11C | 109.5 |
O2—Na1—O5 | 66.7 (3) | H11A—C11—H11C | 109.5 |
O22—Na1—O25 | 68.28 (17) | H11B—C11—H11C | 109.5 |
O2—Na1—O25 | 87.7 (3) | C11—O12—C13 | 115.3 (9) |
O5—Na1—O25 | 145.2 (2) | C11—O12—Na2 | 114.3 (5) |
O22—Na1—P7 | 98.77 (15) | C13—O12—Na2 | 105.3 (6) |
O2—Na1—P7 | 149.1 (2) | O12—C13—C14 | 114.9 (9) |
O5—Na1—P7 | 91.0 (2) | O12—C13—H13A | 108.5 |
O25—Na1—P7 | 120.47 (16) | C14—C13—H13A | 108.5 |
O22—Na1—P3 | 155.08 (17) | O12—C13—H13B | 108.5 |
O2—Na1—P3 | 96.39 (19) | C14—C13—H13B | 108.5 |
O5—Na1—P3 | 107.0 (2) | H13A—C13—H13B | 107.5 |
O25—Na1—P3 | 98.61 (13) | O15—C14—C13 | 109.0 (9) |
P7—Na1—P3 | 68.87 (7) | O15—C14—H14A | 109.9 |
O32—Na2—O35 | 72.70 (15) | C13—C14—H14A | 109.9 |
O32—Na2—O12 | 143.5 (2) | O15—C14—H14B | 109.9 |
O35—Na2—O12 | 79.73 (18) | C13—C14—H14B | 109.9 |
O32—Na2—O15 | 83.27 (18) | H14A—C14—H14B | 108.3 |
O35—Na2—O15 | 88.90 (18) | C14—O15—C16 | 111.6 (8) |
O12—Na2—O15 | 72.5 (2) | C14—O15—Na2 | 110.3 (6) |
O32—Na2—P3i | 112.48 (14) | C16—O15—Na2 | 116.6 (5) |
O35—Na2—P3i | 174.82 (16) | O15—C16—H16A | 109.5 |
O12—Na2—P3i | 95.54 (15) | O15—C16—H16B | 109.5 |
O15—Na2—P3i | 91.70 (15) | H16A—C16—H16B | 109.5 |
O32—Na2—P5 | 92.49 (13) | O15—C16—H16C | 109.5 |
O35—Na2—P5 | 101.67 (15) | H16A—C16—H16C | 109.5 |
O12—Na2—P5 | 116.6 (2) | H16B—C16—H16C | 109.5 |
O15—Na2—P5 | 166.94 (18) | O22—C21—H21A | 109.5 |
P3i—Na2—P5 | 78.47 (7) | O22—C21—H21B | 109.5 |
P5—P1—P2 | 104.28 (10) | H21A—C21—H21B | 109.5 |
P5—P1—P6 | 98.35 (9) | O22—C21—H21C | 109.5 |
P2—P1—P6 | 59.87 (8) | H21A—C21—H21C | 109.5 |
P3—P2—P6 | 105.38 (9) | H21B—C21—H21C | 109.5 |
P3—P2—P1 | 107.36 (11) | C23—O22—C21 | 114.2 (6) |
P6—P2—P1 | 60.24 (8) | C23—O22—Na1 | 115.7 (4) |
P2—P3—P4 | 99.58 (10) | C21—O22—Na1 | 125.5 (5) |
P2—P3—Na2i | 101.80 (8) | O22—C23—C24 | 109.3 (6) |
P4—P3—Na2i | 110.38 (10) | O22—C23—H23A | 109.8 |
P2—P3—Na1 | 96.57 (9) | C24—C23—H23A | 109.8 |
P4—P3—Na1 | 79.36 (8) | O22—C23—H23B | 109.8 |
Na2i—P3—Na1 | 157.19 (10) | C24—C23—H23B | 109.8 |
P3—P4—P7 | 104.17 (10) | H23A—C23—H23B | 108.3 |
P3—P4—P5 | 103.39 (9) | O25—C24—C23 | 110.9 (6) |
P7—P4—P5 | 94.01 (9) | O25—C24—H24A | 109.5 |
P1—P5—P4 | 101.41 (10) | C23—C24—H24A | 109.5 |
P1—P5—P5i | 97.63 (11) | O25—C24—H24B | 109.5 |
P4—P5—P5i | 103.11 (11) | C23—C24—H24B | 109.5 |
P1—P5—Na2 | 104.54 (10) | H24A—C24—H24B | 108.0 |
P4—P5—Na2 | 131.91 (8) | C24—O25—C26 | 113.5 (6) |
P5i—P5—Na2 | 112.56 (11) | C24—O25—Na1 | 99.2 (4) |
P7—P6—P2 | 106.27 (10) | C26—O25—Na1 | 120.9 (4) |
P7—P6—P1 | 107.10 (10) | O25—C26—H26A | 109.5 |
P2—P6—P1 | 59.89 (8) | O25—C26—H26B | 109.5 |
P6—P7—P4 | 98.78 (8) | H26A—C26—H26B | 109.5 |
P6—P7—Na1 | 95.74 (10) | O25—C26—H26C | 109.5 |
P4—P7—Na1 | 79.68 (8) | H26A—C26—H26C | 109.5 |
O2—C1—H1A | 109.5 | H26B—C26—H26C | 109.5 |
O2—C1—H1B | 109.5 | O32—C31—H31A | 109.5 |
H1A—C1—H1B | 109.5 | O32—C31—H31B | 109.5 |
O2—C1—H1C | 109.5 | H31A—C31—H31B | 109.5 |
H1A—C1—H1C | 109.5 | O32—C31—H31C | 109.5 |
H1B—C1—H1C | 109.5 | H31A—C31—H31C | 109.5 |
C3—O2—C1 | 115.8 (9) | H31B—C31—H31C | 109.5 |
C3—O2—Na1 | 112.0 (7) | C31—O32—C33 | 112.3 (5) |
C1—O2—Na1 | 120.0 (6) | C31—O32—Na2 | 118.1 (4) |
O2—C3—C4 | 117.8 (10) | C33—O32—Na2 | 106.7 (4) |
O2—C3—H3A | 107.9 | O32—C33—C34 | 113.1 (6) |
C4—C3—H3A | 107.9 | O32—C33—H33A | 109.0 |
O2—C3—H3B | 107.9 | C34—C33—H33A | 109.0 |
C4—C3—H3B | 107.9 | O32—C33—H33B | 109.0 |
H3A—C3—H3B | 107.2 | C34—C33—H33B | 109.0 |
O5—C4—C3 | 117.8 (10) | H33A—C33—H33B | 107.8 |
O5—C4—H4A | 107.9 | O35—C34—C33 | 107.6 (5) |
C3—C4—H4A | 107.9 | O35—C34—H34A | 110.2 |
O5—C4—H4B | 107.9 | C33—C34—H34A | 110.2 |
C3—C4—H4B | 107.9 | O35—C34—H34B | 110.2 |
H4A—C4—H4B | 107.2 | C33—C34—H34B | 110.2 |
C4—O5—C6 | 117.8 (9) | H34A—C34—H34B | 108.5 |
C4—O5—Na1 | 114.4 (7) | C36—O35—C34 | 112.4 (5) |
C6—O5—Na1 | 127.3 (6) | C36—O35—Na2 | 121.0 (4) |
O5—C6—H6A | 109.5 | C34—O35—Na2 | 110.0 (4) |
O5—C6—H6B | 109.5 | O35—C36—H36A | 109.5 |
H6A—C6—H6B | 109.5 | O35—C36—H36B | 109.5 |
O5—C6—H6C | 109.5 | H36A—C36—H36B | 109.5 |
H6A—C6—H6C | 109.5 | O35—C36—H36C | 109.5 |
H6B—C6—H6C | 109.5 | H36A—C36—H36C | 109.5 |
O12—C11—H11A | 109.5 | H36B—C36—H36C | 109.5 |
O12—C11—H11B | 109.5 | ||
P5—P1—P2—P3 | −6.66 (11) | O22—Na1—O2—C3 | −114.9 (7) |
P6—P1—P2—P3 | −98.13 (10) | O5—Na1—O2—C3 | −26.0 (7) |
P5—P1—P2—P6 | 91.46 (9) | O25—Na1—O2—C3 | 178.1 (7) |
P6—P2—P3—P4 | −29.54 (11) | P7—Na1—O2—C3 | 21.0 (9) |
P1—P2—P3—P4 | 33.50 (10) | P3—Na1—O2—C3 | 79.7 (7) |
P6—P2—P3—Na2i | −142.87 (10) | P4—Na1—O2—C3 | 43.3 (7) |
P1—P2—P3—Na2i | −79.83 (10) | O22—Na1—O2—C1 | 104.2 (7) |
P6—P2—P3—Na1 | 50.73 (11) | O5—Na1—O2—C1 | −166.9 (8) |
P1—P2—P3—Na1 | 113.77 (9) | O25—Na1—O2—C1 | 37.3 (7) |
O22—Na1—P3—P2 | −2.6 (4) | P7—Na1—O2—C1 | −119.9 (7) |
O2—Na1—P3—P2 | 141.9 (2) | P3—Na1—O2—C1 | −61.1 (7) |
O5—Na1—P3—P2 | −150.6 (2) | P4—Na1—O2—C1 | −97.6 (7) |
O25—Na1—P3—P2 | 53.20 (16) | C1—O2—C3—C4 | −178.0 (10) |
P7—Na1—P3—P2 | −66.22 (9) | Na1—O2—C3—C4 | 39.3 (13) |
P4—Na1—P3—P2 | −98.56 (10) | O2—C3—C4—O5 | −28.1 (19) |
O22—Na1—P3—P4 | 96.0 (4) | C3—C4—O5—C6 | −170.6 (11) |
O2—Na1—P3—P4 | −119.6 (2) | C3—C4—O5—Na1 | 1.7 (15) |
O5—Na1—P3—P4 | −52.1 (2) | O22—Na1—O5—C4 | 116.0 (8) |
O25—Na1—P3—P4 | 151.76 (15) | O2—Na1—O5—C4 | 12.8 (8) |
P7—Na1—P3—P4 | 32.33 (7) | O25—Na1—O5—C4 | 58.7 (9) |
O22—Na1—P3—Na2i | −146.2 (4) | P7—Na1—O5—C4 | −145.1 (8) |
O2—Na1—P3—Na2i | −1.7 (4) | P3—Na1—O5—C4 | −76.9 (8) |
O5—Na1—P3—Na2i | 65.8 (3) | P4—Na1—O5—C4 | −106.9 (8) |
O25—Na1—P3—Na2i | −90.4 (3) | O22—Na1—O5—C6 | −72.5 (8) |
P7—Na1—P3—Na2i | 150.2 (3) | O2—Na1—O5—C6 | −175.8 (9) |
P4—Na1—P3—Na2i | 117.9 (3) | O25—Na1—O5—C6 | −129.9 (8) |
P2—P3—P4—P7 | 49.42 (10) | P7—Na1—O5—C6 | 26.3 (8) |
Na2i—P3—P4—P7 | 155.91 (9) | P3—Na1—O5—C6 | 94.5 (8) |
Na1—P3—P4—P7 | −45.54 (9) | P4—Na1—O5—C6 | 64.5 (8) |
P2—P3—P4—P5 | −48.30 (10) | O32—Na2—O12—C11 | 161.5 (7) |
Na2i—P3—P4—P5 | 58.19 (11) | O35—Na2—O12—C11 | −157.3 (8) |
Na1—P3—P4—P5 | −143.25 (9) | O15—Na2—O12—C11 | 110.6 (7) |
P2—P3—P4—Na1 | 94.95 (9) | P3i—Na2—O12—C11 | 20.6 (7) |
Na2i—P3—P4—Na1 | −158.56 (11) | P5—Na2—O12—C11 | −59.3 (8) |
O22—Na1—P4—P3 | −141.9 (2) | O32—Na2—O12—C13 | 33.9 (8) |
O2—Na1—P4—P3 | 70.1 (2) | O35—Na2—O12—C13 | 75.2 (6) |
O5—Na1—P4—P3 | 130.35 (18) | O15—Na2—O12—C13 | −16.9 (6) |
O25—Na1—P4—P3 | −38.70 (19) | P3i—Na2—O12—C13 | −107.0 (6) |
P7—Na1—P4—P3 | −127.82 (11) | P5—Na2—O12—C13 | 173.2 (6) |
O22—Na1—P4—P7 | −14.1 (2) | C11—O12—C13—C14 | −79.8 (11) |
O2—Na1—P4—P7 | −162.0 (2) | Na2—O12—C13—C14 | 47.1 (10) |
O5—Na1—P4—P7 | −101.83 (17) | O12—C13—C14—O15 | −63.4 (12) |
O25—Na1—P4—P7 | 89.1 (2) | C13—C14—O15—C16 | 172.1 (8) |
P3—Na1—P4—P7 | 127.82 (11) | C13—C14—O15—Na2 | 40.8 (10) |
O22—Na1—P4—P5 | −67.8 (3) | O32—Na2—O15—C14 | −166.0 (7) |
O2—Na1—P4—P5 | 144.3 (2) | O35—Na2—O15—C14 | −93.3 (6) |
O5—Na1—P4—P5 | −155.47 (19) | O12—Na2—O15—C14 | −13.7 (6) |
O25—Na1—P4—P5 | 35.5 (3) | P3i—Na2—O15—C14 | 81.6 (6) |
P7—Na1—P4—P5 | −53.64 (13) | P5—Na2—O15—C14 | 122.4 (8) |
P3—Na1—P4—P5 | 74.18 (14) | O32—Na2—O15—C16 | 65.3 (5) |
P2—P1—P5—P4 | −22.46 (10) | O35—Na2—O15—C16 | 138.1 (5) |
P6—P1—P5—P4 | 38.45 (10) | O12—Na2—O15—C16 | −142.4 (5) |
P2—P1—P5—P5i | 82.64 (12) | P3i—Na2—O15—C16 | −47.1 (5) |
P6—P1—P5—P5i | 143.55 (11) | P5—Na2—O15—C16 | −6.3 (10) |
P2—P1—P5—Na2 | −161.61 (8) | O2—Na1—O22—C23 | −92.2 (6) |
P6—P1—P5—Na2 | −100.70 (9) | O5—Na1—O22—C23 | −159.2 (5) |
P3—P4—P5—P1 | 44.73 (10) | O25—Na1—O22—C23 | −10.4 (5) |
P7—P4—P5—P1 | −60.87 (10) | P7—Na1—O22—C23 | 109.0 (5) |
Na1—P4—P5—P1 | −15.87 (16) | P3—Na1—O22—C23 | 51.3 (7) |
P3—P4—P5—P5i | −55.99 (14) | O2—Na1—O22—C21 | 62.3 (7) |
P7—P4—P5—P5i | −161.60 (12) | O5—Na1—O22—C21 | −4.7 (6) |
Na1—P4—P5—P5i | −116.59 (14) | O25—Na1—O22—C21 | 144.1 (6) |
P3—P4—P5—Na2 | 166.42 (11) | P7—Na1—O22—C21 | −96.5 (6) |
P7—P4—P5—Na2 | 60.81 (14) | P3—Na1—O22—C21 | −154.2 (6) |
Na1—P4—P5—Na2 | 105.82 (16) | C21—O22—C23—C24 | −176.0 (6) |
O32—Na2—P5—P1 | 145.08 (13) | Na1—O22—C23—C24 | −18.6 (8) |
O35—Na2—P5—P1 | 72.23 (15) | O22—C23—C24—O25 | 60.6 (9) |
O12—Na2—P5—P1 | −12.01 (18) | C23—C24—O25—C26 | 165.3 (7) |
O15—Na2—P5—P1 | −144.3 (6) | C23—C24—O25—Na1 | −65.0 (7) |
P3i—Na2—P5—P1 | −102.48 (8) | O22—Na1—O25—C24 | 37.4 (4) |
O32—Na2—P5—P4 | 24.58 (18) | O2—Na1—O25—C24 | 143.3 (4) |
O35—Na2—P5—P4 | −48.26 (19) | O5—Na1—O25—C24 | 102.1 (5) |
O12—Na2—P5—P4 | −132.51 (18) | P7—Na1—O25—C24 | −50.1 (4) |
O15—Na2—P5—P4 | 95.2 (6) | P3—Na1—O25—C24 | −120.6 (4) |
P3i—Na2—P5—P4 | 137.03 (12) | O22—Na1—O25—C26 | 162.1 (6) |
O32—Na2—P5—P5i | −110.08 (15) | O2—Na1—O25—C26 | −92.0 (6) |
O35—Na2—P5—P5i | 177.08 (16) | O5—Na1—O25—C26 | −133.3 (6) |
O12—Na2—P5—P5i | 92.8 (2) | P7—Na1—O25—C26 | 74.6 (6) |
O15—Na2—P5—P5i | −39.4 (7) | P3—Na1—O25—C26 | 4.1 (6) |
P3i—Na2—P5—P5i | 2.36 (13) | P4—Na1—O25—C26 | 27.5 (6) |
P3—P2—P6—P7 | 0.84 (14) | O35—Na2—O32—C31 | 109.7 (5) |
P1—P2—P6—P7 | −100.65 (11) | O12—Na2—O32—C31 | 152.5 (5) |
P3—P2—P6—P1 | 101.49 (11) | O15—Na2—O32—C31 | −159.3 (5) |
P5—P1—P6—P7 | −2.49 (13) | P3i—Na2—O32—C31 | −70.3 (5) |
P2—P1—P6—P7 | 99.23 (11) | P5—Na2—O32—C31 | 8.3 (5) |
P5—P1—P6—P2 | −101.72 (10) | O35—Na2—O32—C33 | −17.7 (4) |
P2—P6—P7—P4 | 28.01 (13) | O12—Na2—O32—C33 | 25.0 (6) |
P1—P6—P7—P4 | −34.80 (12) | O15—Na2—O32—C33 | 73.2 (4) |
P2—P6—P7—Na1 | −52.39 (11) | P3i—Na2—O32—C33 | 162.3 (4) |
P1—P6—P7—Na1 | −115.20 (10) | P5—Na2—O32—C33 | −119.2 (4) |
P3—P4—P7—P6 | −48.41 (11) | C31—O32—C33—C34 | −81.9 (7) |
P5—P4—P7—P6 | 56.49 (11) | Na2—O32—C33—C34 | 48.9 (6) |
Na1—P4—P7—P6 | −94.28 (10) | O32—C33—C34—O35 | −64.1 (7) |
P3—P4—P7—Na1 | 45.87 (9) | C33—C34—O35—C36 | 179.9 (6) |
P5—P4—P7—Na1 | 150.77 (9) | C33—C34—O35—Na2 | 41.9 (6) |
O22—Na1—P7—P6 | −91.75 (15) | O32—Na2—O35—C36 | −147.5 (5) |
O2—Na1—P7—P6 | 131.4 (4) | O12—Na2—O35—C36 | 56.8 (5) |
O5—Na1—P7—P6 | 173.61 (17) | O15—Na2—O35—C36 | 129.2 (5) |
O25—Na1—P7—P6 | −21.85 (15) | P3i—Na2—O35—C36 | 32 (2) |
P3—Na1—P7—P6 | 65.80 (8) | P5—Na2—O35—C36 | −58.5 (5) |
P4—Na1—P7—P6 | 97.92 (8) | O32—Na2—O35—C34 | −13.8 (4) |
O22—Na1—P7—P4 | 170.34 (16) | O12—Na2—O35—C34 | −169.5 (5) |
O2—Na1—P7—P4 | 33.5 (4) | O15—Na2—O35—C34 | −97.1 (4) |
O5—Na1—P7—P4 | 75.70 (18) | P3i—Na2—O35—C34 | 166.2 (17) |
O25—Na1—P7—P4 | −119.76 (15) | P5—Na2—O35—C34 | 75.2 (4) |
P3—Na1—P7—P4 | −32.12 (7) |
Symmetry code: (i) −x+2, −y+1, −z+1. |