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
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.014 Å
- R factor = 0.068
- wR factor = 0.122
- Data-to-parameter ratio = 18.7
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT328_ALERT_2_B Check for Possibly Missing H on sp3? Phosphor .. P7 PLAT340_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 15
Alert level C PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 46 Perc. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.85 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.57 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C14 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Na1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O12 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O15 PLAT322_ALERT_2_C Check Hybridisation of P1 in Main Residue . ? PLAT322_ALERT_2_C Check Hybridisation of P2 in Main Residue . ? PLAT322_ALERT_2_C Check Hybridisation of P6 in Main Residue . ? PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C3 - C4 ... 1.42 Ang. PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 205 P3 -NA2 -O35 -C36 32.00 2.00 3.766 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 210 P3 -NA2 -O35 -C34 166.20 1.70 3.766 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 15 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 12 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
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. |