In the title compound, (C
18H
23N
2)
4[SiW
12O
40]·14H
2O, the asymmetric unit contains two
trans-4-[(
N,
N-diethylamino)styryl]-
N-methylpyridinium (DEASP) cations, one half dodecatungstosilicate (SiW
12O
40) anion and seven water molecules. The two DEASP cations form a periodically layered arrangement perpendicular to their molecular planes and the SiW
12O
40 anions have a disordered `pseudo-Keggin' structure around an inversion centre. They are linked into an infinite three-dimensional assembly
via electrostatic forces and C—H
O hydrogen bonds.
Supporting information
CCDC reference: 624957
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.037 Å
- H-atom completeness 77%
- Disorder in main residue
- R factor = 0.061
- wR factor = 0.160
- Data-to-parameter ratio = 17.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 37
PLAT430_ALERT_2_B Short Inter D...A Contact OW6 .. OW12 .. 2.76 Ang.
Alert level C
PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 49 Perc.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Si1
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for OW8
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for OW2
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for OW6
PLAT301_ALERT_3_C Main Residue Disorder ......................... 7.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ OW5
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ OW9
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C21 - C22 ... 1.37 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C24 - C25 ... 1.35 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C28 - C33 ... 1.38 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 14
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7
O
Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C72 H120 N8 O54 Si1 W12
Atom count from the _atom_site data: C72 H92 N8 O54 Si1 W12
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 1
From the CIF: _chemical_formula_sum C72 H120 N8 O54 Si W12
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 72.00 72.00 0.00
H 120.00 92.00 28.00
N 8.00 8.00 0.00
O 54.00 54.00 0.00
Si 1.00 1.00 0.00
W 12.00 12.00 0.00
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
16 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
8 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
6 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXL97.
Tetrakis{
trans-4-[(
N,
N-diethylamino)styryl]-1-methylpyridinium} dodecatungstosilicate tetradecahydrate
top
Crystal data top
(C18H23N2)4[W12O40SiW12]·14H2O | Z = 1 |
Mr = 4195.91 | F(000) = 1914.0 |
Triclinic, P1 | Dx = 2.318 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 15.019 (4) Å | Cell parameters from 250 reflections |
b = 15.056 (4) Å | θ = 1.7–25.5° |
c = 16.080 (4) Å | µ = 11.60 mm−1 |
α = 64.393 (3)° | T = 298 K |
β = 79.436 (4)° | Block, red |
γ = 65.578 (3)° | 0.45 × 0.21 × 0.10 mm |
V = 2985.5 (14) Å3 | |
Data collection top
Bruker SMART CCD diffractometer | 10904 independent reflections |
Radiation source: fine-focus sealed tube | 5387 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
φ and ω scans | θmax = 25.5°, θmin = 1.7° |
Absorption correction: part of the refinement model (ΔF) (Parkin et al., 1995) | h = −10→18 |
Tmin = 0.065, Tmax = 0.311 | k = −15→18 |
16302 measured reflections | l = −18→19 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.061 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.160 | H-atom parameters constrained |
S = 0.89 | w = 1/[σ2(Fo2) + (0.0704P)2] where P = (Fo2 + 2Fc2)/3 |
10904 reflections | (Δ/σ)max < 0.001 |
627 parameters | Δρmax = 2.18 e Å−3 |
118 restraints | Δρmin = −1.51 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. The disorder of C atoms in DEASP cations contribute to the low bond precision on
C—C bonds and also to the high Ueq(max)/Ueq(min) values of
some of the carbons. So eighteen SHELXL97 (Sheldrick, 1997) ISOR
restraints were used in the refinement to lower these values, and other
geometric restraints (DFIX, DANG and SADI) were also used to make
geometric structure reasonable. Refinement of F2 against ALL
reflections. The weighted R-factor wR and goodness of fit
S are based on F2, conventional R-factors R are
based on F, with F set to zero for negative F2. The
threshold expression of F2 > σ(F2) is used only for
calculating R-factors(gt) etc. and is not relevant to the choice
of reflections for refinement. R-factors based on F2 are
statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
N1 | −0.0254 (13) | 1.0805 (14) | 0.5913 (11) | 0.081 (3) | |
N2 | 0.4099 (17) | 0.2409 (17) | 0.8961 (15) | 0.143 (5) | |
C1 | 0.0629 (13) | 1.0391 (16) | 0.6241 (12) | 0.084 (6) | |
H1A | 0.0902 | 1.0844 | 0.6240 | 0.101* | |
C2 | 0.1149 (13) | 0.9359 (18) | 0.6572 (14) | 0.083 (6) | |
H2A | 0.1803 | 0.9125 | 0.6712 | 0.099* | |
C3 | 0.0779 (15) | 0.8635 (15) | 0.6715 (12) | 0.082 (6) | |
C4 | −0.0204 (14) | 0.9090 (14) | 0.6439 (13) | 0.087 (4) | |
H4A | −0.0548 | 0.8659 | 0.6547 | 0.105* | |
C5 | −0.0618 (14) | 1.0101 (12) | 0.6037 (12) | 0.091 (6) | |
H5A | −0.1243 | 1.0364 | 0.5809 | 0.110* | |
C6 | 0.1199 (15) | 0.7468 (15) | 0.7105 (13) | 0.108 (5) | |
H6A | 0.0789 | 0.7152 | 0.7090 | 0.130* | |
C7 | 0.2046 (15) | 0.6810 (18) | 0.7466 (14) | 0.115 (4) | |
H7A | 0.2453 | 0.7139 | 0.7464 | 0.138* | |
C8 | 0.2463 (17) | 0.5715 (19) | 0.7853 (15) | 0.110 (4) | |
C9 | 0.3408 (16) | 0.5265 (19) | 0.8142 (14) | 0.107 (4) | |
H9A | 0.3697 | 0.5730 | 0.8084 | 0.128* | |
C10 | 0.3952 (18) | 0.4246 (19) | 0.8494 (14) | 0.111 (7) | |
H10A | 0.4584 | 0.4004 | 0.8698 | 0.133* | |
C11 | 0.3534 (19) | 0.352 (2) | 0.8551 (16) | 0.120 (8) | |
C12 | 0.2587 (16) | 0.3909 (18) | 0.8226 (14) | 0.106 (4) | |
H12A | 0.2305 | 0.3464 | 0.8223 | 0.127* | |
C13 | 0.2075 (17) | 0.5053 (19) | 0.7893 (15) | 0.116 (4) | |
H13A | 0.1434 | 0.5338 | 0.7696 | 0.140* | |
C14 | −0.0790 (14) | 1.1939 (15) | 0.5467 (13) | 0.100 (7) | |
H14A | −0.1422 | 1.2068 | 0.5288 | 0.151* | |
H14B | −0.0437 | 1.2236 | 0.4929 | 0.151* | |
H14C | −0.0866 | 1.2265 | 0.5886 | 0.151* | |
C15 | 0.524 (2) | 0.194 (2) | 0.9196 (16) | 0.149 (4) | |
H15A | 0.5579 | 0.1243 | 0.9175 | 0.179* | |
H15B | 0.5558 | 0.2415 | 0.8791 | 0.179* | |
C16 | 0.5141 (19) | 0.188 (2) | 1.0169 (16) | 0.162 (4) | |
H16A | 0.5780 | 0.1598 | 1.0420 | 0.243* | |
H16B | 0.4797 | 0.1423 | 1.0543 | 0.243* | |
H16C | 0.4785 | 0.2578 | 1.0163 | 0.243* | |
C17 | 0.3860 (18) | 0.160 (2) | 0.8826 (16) | 0.149 (4) | |
H17A | 0.4440 | 0.0976 | 0.8869 | 0.179* | |
H17B | 0.3545 | 0.1902 | 0.8238 | 0.179* | |
C18 | 0.3161 (19) | 0.135 (2) | 0.9630 (17) | 0.163 (4) | |
H18A | 0.2965 | 0.0822 | 0.9632 | 0.245* | |
H18B | 0.2594 | 0.1989 | 0.9566 | 0.245* | |
H18C | 0.3483 | 0.1095 | 1.0199 | 0.245* | |
C21 | 0.4443 (14) | 0.5122 (15) | 0.6031 (13) | 0.089 (6) | |
H21A | 0.4305 | 0.5844 | 0.5835 | 0.107* | |
C22 | 0.5332 (14) | 0.4395 (16) | 0.6421 (14) | 0.086 (4) | |
H22A | 0.5688 | 0.4729 | 0.6492 | 0.081* | |
C24 | 0.4889 (14) | 0.3074 (14) | 0.6611 (13) | 0.089 (6) | |
H24A | 0.5023 | 0.2351 | 0.6825 | 0.106* | |
C25 | 0.3998 (14) | 0.3756 (13) | 0.6244 (12) | 0.092 (6) | |
H25A | 0.3543 | 0.3501 | 0.6210 | 0.111* | |
C23A | 0.5570 (15) | 0.3345 (16) | 0.6689 (13) | 0.085 (4) | 0.57 (3) |
C26A | 0.657 (2) | 0.284 (3) | 0.710 (2) | 0.098 (11) | 0.57 (3) |
H26A | 0.6873 | 0.3258 | 0.7114 | 0.118* | 0.57 (3) |
C27A | 0.7014 (19) | 0.180 (3) | 0.743 (2) | 0.101 (7) | 0.57 (3) |
H27A | 0.6684 | 0.1394 | 0.7426 | 0.122* | 0.57 (3) |
C23B | 0.5570 (15) | 0.3345 (16) | 0.6689 (13) | 0.085 (4) | 0.43 (3) |
C26B | 0.641 (2) | 0.232 (3) | 0.712 (3) | 0.071 (4) | 0.43 (3) |
H26B | 0.6565 | 0.1592 | 0.7435 | 0.081* | 0.43 (3) |
C27B | 0.724 (2) | 0.229 (2) | 0.734 (3) | 0.0740 (9) | 0.43 (3) |
H27B | 0.7126 | 0.3021 | 0.7182 | 0.081* | 0.43 (3) |
C28 | 0.8012 (15) | 0.1235 (17) | 0.7811 (15) | 0.104 (7) | |
C29 | 0.8788 (18) | 0.1544 (17) | 0.7843 (15) | 0.119 (8) | |
H29A | 0.8688 | 0.2261 | 0.7614 | 0.143* | |
C30 | 0.9670 (17) | 0.079 (2) | 0.8208 (17) | 0.126 (9) | |
H30A | 1.0172 | 0.0991 | 0.8219 | 0.151* | |
C31 | 0.983 (2) | −0.029 (3) | 0.8566 (18) | 0.122 (9) | |
C32 | 0.9045 (18) | −0.057 (2) | 0.8569 (16) | 0.125 (7) | |
H32A | 0.9115 | −0.1280 | 0.8865 | 0.150* | |
C33 | 0.8201 (17) | 0.0160 (19) | 0.8158 (16) | 0.123 (7) | |
H33A | 0.7727 | −0.0060 | 0.8103 | 0.148* | |
C34 | 0.2837 (15) | 0.5549 (16) | 0.5553 (15) | 0.116 (8) | |
H34A | 0.2800 | 0.6261 | 0.5371 | 0.173* | |
H34B | 0.2344 | 0.5421 | 0.6010 | 0.173* | |
H34C | 0.2734 | 0.5463 | 0.5026 | 0.173* | |
C35 | 1.165 (2) | −0.075 (2) | 0.8747 (16) | 0.150 (4) | |
H35A | 1.2231 | −0.1328 | 0.8682 | 0.180* | |
H35B | 1.1574 | −0.0105 | 0.8200 | 0.180* | |
C36 | 1.1681 (19) | −0.061 (2) | 0.9604 (17) | 0.161 (4) | |
H36A | 1.2222 | −0.0411 | 0.9568 | 0.241* | |
H36B | 1.1759 | −0.1265 | 1.0130 | 0.241* | |
H36C | 1.1082 | −0.0062 | 0.9664 | 0.241* | |
C37 | 1.094 (2) | −0.222 (2) | 0.9371 (17) | 0.150 (4) | |
H37A | 1.0668 | −0.2425 | 0.9006 | 0.179* | |
H37B | 1.1639 | −0.2610 | 0.9414 | 0.179* | |
C38 | 1.0483 (19) | −0.245 (2) | 1.0305 (16) | 0.157 (4) | |
H38A | 1.0583 | −0.3192 | 1.0601 | 0.235* | |
H38B | 0.9795 | −0.2031 | 1.0251 | 0.235* | |
H38C | 1.0779 | −0.2279 | 1.0666 | 0.235* | |
N3 | 0.3776 (13) | 0.4814 (14) | 0.5928 (10) | 0.086 (4) | |
N4 | 1.069 (2) | −0.104 (2) | 0.8947 (16) | 0.146 (7) | |
O1 | 0.4716 (13) | 0.9822 (13) | 0.6066 (12) | 0.043 (4) | 0.50 |
O2 | 0.4834 (14) | 0.8928 (15) | 0.5508 (13) | 0.053 (5) | 0.50 |
O3 | 0.3969 (13) | 1.0999 (14) | 0.5082 (12) | 0.043 (5) | 0.50 |
O4 | 0.5865 (13) | 0.9951 (14) | 0.5507 (12) | 0.047 (5) | 0.50 |
O5 | 0.4549 (8) | 1.0636 (8) | 0.7027 (8) | 0.076 (3) | |
O6 | 0.5316 (8) | 0.8573 (8) | 0.7502 (7) | 0.0696 (9) | |
O7 | 0.3464 (8) | 0.9535 (8) | 0.7044 (7) | 0.0682 (9) | |
O8 | 0.2442 (10) | 1.1216 (10) | 0.5632 (9) | 0.099 (4) | |
O9 | 0.3571 (8) | 0.8311 (8) | 0.6308 (7) | 0.0688 (9) | |
O10 | 0.5476 (8) | 0.7270 (9) | 0.6729 (7) | 0.0722 (9) | |
O11 | 0.4873 (8) | 0.7532 (8) | 0.5183 (7) | 0.0670 (9) | |
O12 | 0.2578 (8) | 0.9966 (9) | 0.4845 (7) | 0.0735 (9) | |
O13 | 0.6105 (8) | 1.0825 (9) | 0.6242 (8) | 0.0796 (9) | |
O14 | 0.3520 (10) | 1.2256 (11) | 0.5609 (9) | 0.105 (4) | |
O15 | 0.7100 (8) | 0.7485 (9) | 0.5951 (7) | 0.0727 (9) | |
O16 | 0.6920 (8) | 0.8754 (8) | 0.6694 (7) | 0.0675 (9) | |
O20 | 0.6134 (8) | 0.9573 (8) | 0.8057 (7) | 0.0715 (9) | |
O21 | 0.2506 (8) | 1.1494 (9) | 0.7208 (7) | 0.0748 (9) | |
O22 | 0.4078 (8) | 0.7454 (8) | 0.8101 (7) | 0.0712 (9) | |
O23 | 0.2930 (8) | 0.7963 (9) | 0.5039 (7) | 0.0745 (9) | |
O24 | 0.6613 (9) | 0.5924 (10) | 0.5896 (9) | 0.094 (4) | |
O25 | 0.8652 (9) | 0.7977 (10) | 0.5867 (8) | 0.091 (4) | |
OW1 | 0.684 (6) | 0.388 (5) | 0.857 (5) | 0.32 (9)* | 0.50 |
OW2 | 0.927 (4) | 0.602 (4) | 0.850 (4) | 0.22 (9)* | 0.50 |
OW3 | 0.893 (2) | 0.400 (6) | 0.595 (8) | 0.26 (6)* | 0.50 |
OW4 | 1.044 (7) | 0.558 (6) | 0.581 (2) | 0.22 (6)* | 0.50 |
OW5 | 0.980 (5) | 0.432 (5) | 0.668 (4) | 0.26 (3)* | 0.50 |
OW6 | 0.824 (4) | 0.648 (4) | 0.883 (4) | 0.22 (3)* | 0.50 |
OW7 | 0.651 (6) | 0.480 (7) | 0.865 (6) | 0.35 (4)* | 0.50 |
OW8 | 0.886 (4) | 0.694 (5) | 0.884 (4) | 0.26 (9)* | 0.50 |
OW9 | 0.950 (3) | 0.440 (8) | 0.575 (2) | 0.25 (6)* | 0.50 |
OW10 | 0.982 (5) | 0.489 (5) | 0.615 (5) | 0.25 (3)* | 0.50 |
OW11 | 1.072 (4) | 0.365 (5) | 0.645 (4) | 0.27 (3)* | 0.50 |
OW12 | 0.703 (4) | 0.556 (4) | 0.874 (4) | 0.29 (4)* | 0.50 |
OW13 | 1.113 (4) | 0.428 (5) | 1.035 (4) | 0.25 (6)* | 0.50 |
OW14 | 0.599 (6) | 0.450 (7) | 0.959 (6) | 0.40 (4)* | 0.50 |
Si1 | 0.5000 | 1.0000 | 0.5000 | 0.0281 (12) | |
W1 | 0.57850 (6) | 0.96635 (6) | 0.70863 (5) | 0.0649 (2) | |
W2 | 0.32897 (5) | 1.10249 (6) | 0.64999 (5) | 0.0650 (2) | |
W3 | 0.43981 (5) | 0.82541 (6) | 0.71236 (5) | 0.0626 (2) | |
W4 | 0.35987 (5) | 0.86064 (5) | 0.50360 (5) | 0.0602 (2) | |
W5 | 0.60966 (5) | 0.72291 (5) | 0.56158 (5) | 0.0653 (2) | |
W6 | 0.74938 (5) | 0.86112 (6) | 0.55987 (5) | 0.0674 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
N1 | 0.096 | 0.080 (6) | 0.077 (6) | −0.037 (4) | −0.002 (4) | −0.034 (4) |
N2 | 0.166 | 0.098 (16) | 0.167 | −0.043 (14) | −0.057 (15) | −0.040 (13) |
C1 | 0.088 (16) | 0.102 (17) | 0.069 (13) | −0.047 (14) | 0.013 (11) | −0.036 (13) |
C2 | 0.038 (11) | 0.098 (16) | 0.115 (17) | −0.023 (11) | 0.018 (10) | −0.054 (14) |
C3 | 0.092 (10) | 0.084 (9) | 0.074 (9) | −0.028 (8) | 0.002 (7) | −0.041 (7) |
C4 | 0.081 | 0.090 (6) | 0.089 (6) | −0.030 (4) | −0.003 (5) | −0.035 (4) |
C5 | 0.085 (15) | 0.071 (14) | 0.084 (14) | −0.004 (11) | −0.049 (11) | −0.006 (11) |
C6 | 0.115 (10) | 0.095 | 0.101 (10) | −0.022 (7) | 0.003 (8) | −0.045 (7) |
C7 | 0.107 | 0.114 | 0.111 (10) | −0.030 (7) | 0.007 (8) | −0.049 (7) |
C8 | 0.122 | 0.103 (6) | 0.107 (6) | −0.042 (4) | 0.001 (5) | −0.045 (4) |
C9 | 0.107 | 0.105 (6) | 0.109 (6) | −0.042 (4) | 0.002 (5) | −0.043 (4) |
C10 | 0.116 (11) | 0.106 (11) | 0.112 (11) | −0.039 (8) | −0.008 (8) | −0.045 (8) |
C11 | 0.118 (11) | 0.118 (11) | 0.119 (11) | −0.041 (9) | −0.006 (8) | −0.043 (8) |
C12 | 0.092 | 0.110 (6) | 0.111 (6) | −0.039 (4) | −0.002 (5) | −0.037 (4) |
C13 | 0.109 | 0.118 (6) | 0.115 (6) | −0.040 (4) | 0.000 (5) | −0.043 (4) |
C14 | 0.111 (18) | 0.077 (15) | 0.094 (16) | −0.020 (13) | −0.003 (12) | −0.029 (12) |
C15 | 0.150 | 0.150 (7) | 0.148 (7) | −0.056 (4) | 0.002 (5) | −0.060 (4) |
C16 | 0.157 | 0.163 (7) | 0.160 (7) | −0.058 (5) | −0.002 (5) | −0.061 (5) |
C17 | 0.143 | 0.151 (7) | 0.151 (7) | −0.053 (5) | −0.003 (5) | −0.060 (5) |
C18 | 0.153 | 0.165 (7) | 0.165 (7) | −0.062 (5) | 0.000 (5) | −0.059 (5) |
C21 | 0.120 (19) | 0.062 (13) | 0.091 (15) | −0.040 (13) | −0.012 (13) | −0.025 (11) |
C22 | 0.077 | 0.089 (6) | 0.089 (6) | −0.031 (4) | 0.002 (5) | −0.033 (4) |
C24 | 0.092 (10) | 0.077 (9) | 0.092 (10) | −0.026 (8) | 0.000 (8) | −0.036 (7) |
C25 | 0.107 (10) | 0.085 (9) | 0.093 (10) | −0.044 (8) | 0.014 (8) | −0.042 (8) |
C23A | 0.080 | 0.084 (6) | 0.082 (6) | −0.027 (4) | 0.004 (5) | −0.032 (4) |
C26A | 0.094 | 0.109 | 0.09 (3) | −0.056 (17) | 0.03 (2) | −0.04 (2) |
C27A | 0.099 (13) | 0.111 | 0.101 (12) | −0.050 (8) | 0.004 (9) | −0.040 (8) |
C23B | 0.080 | 0.084 (6) | 0.082 (6) | −0.027 (4) | 0.004 (5) | −0.032 (4) |
C26B | 0.074 | 0.068 (7) | 0.070 (7) | −0.026 (5) | 0.002 (5) | −0.029 (5) |
C27B | 0.0741 (14) | 0.074 | 0.0740 (14) | −0.0279 (9) | −0.0004 (10) | −0.0295 (9) |
C28 | 0.087 (17) | 0.109 | 0.079 (16) | 0.008 (15) | −0.030 (13) | −0.036 (13) |
C29 | 0.11 (2) | 0.100 | 0.104 (19) | −0.005 (16) | −0.007 (16) | −0.035 (13) |
C30 | 0.09 (2) | 0.15 (3) | 0.12 (2) | −0.02 (2) | −0.011 (16) | −0.07 (2) |
C31 | 0.09 (2) | 0.15 (3) | 0.11 (2) | −0.02 (2) | −0.016 (16) | −0.06 (2) |
C32 | 0.10 (2) | 0.185 | 0.13 (2) | −0.072 (18) | 0.004 (16) | −0.084 (17) |
C33 | 0.078 (18) | 0.180 | 0.12 (2) | −0.048 (17) | −0.003 (15) | −0.065 (19) |
C34 | 0.087 (17) | 0.121 (19) | 0.119 (19) | 0.004 (15) | −0.033 (14) | −0.058 (16) |
C35 | 0.146 | 0.150 (7) | 0.146 (7) | −0.052 (5) | 0.002 (5) | −0.057 (4) |
C36 | 0.155 | 0.164 (7) | 0.162 (7) | −0.056 (5) | −0.006 (5) | −0.066 (5) |
C37 | 0.147 | 0.151 (7) | 0.150 (7) | −0.057 (5) | 0.000 (5) | −0.059 (5) |
C38 | 0.151 | 0.158 (7) | 0.157 (7) | −0.055 (4) | −0.003 (5) | −0.061 (5) |
N3 | 0.100 (15) | 0.103 | 0.073 (11) | −0.048 (11) | 0.007 (9) | −0.045 (9) |
N4 | 0.14 (2) | 0.15 (2) | 0.150 | −0.063 (18) | 0.003 (16) | −0.053 (15) |
O1 | 0.045 | 0.042 (8) | 0.054 (9) | −0.031 (6) | 0.001 (6) | −0.016 (6) |
O2 | 0.062 (14) | 0.058 (13) | 0.066 (14) | −0.045 (12) | 0.014 (11) | −0.034 (11) |
O3 | 0.042 (8) | 0.046 (8) | 0.050 (8) | −0.028 (7) | −0.002 (6) | −0.016 (6) |
O4 | 0.044 (6) | 0.047 (6) | 0.052 (6) | −0.019 (5) | −0.003 (4) | −0.018 (4) |
O5 | 0.086 | 0.058 (6) | 0.102 (7) | −0.036 (5) | −0.017 (5) | −0.033 (5) |
O6 | 0.068 | 0.0700 (14) | 0.0709 (14) | −0.0263 (9) | −0.0010 (10) | −0.0271 (9) |
O7 | 0.067 | 0.0688 (14) | 0.0693 (14) | −0.0264 (9) | −0.0013 (10) | −0.0266 (9) |
O8 | 0.099 (4) | 0.099 (4) | 0.100 (4) | −0.0388 (18) | −0.0009 (10) | −0.0385 (19) |
O9 | 0.066 | 0.0700 (14) | 0.0695 (14) | −0.0248 (9) | −0.0009 (10) | −0.0278 (9) |
O10 | 0.070 | 0.0735 (14) | 0.0724 (14) | −0.0263 (9) | −0.0013 (10) | −0.0288 (9) |
O11 | 0.065 | 0.0679 (14) | 0.0674 (14) | −0.0241 (9) | −0.0009 (10) | −0.0273 (9) |
O12 | 0.071 | 0.0736 (14) | 0.0738 (14) | −0.0271 (9) | 0.0014 (10) | −0.0285 (9) |
O13 | 0.078 | 0.0794 (14) | 0.0802 (14) | −0.0290 (9) | 0.0007 (10) | −0.0314 (9) |
O14 | 0.105 (4) | 0.105 (4) | 0.106 (4) | −0.0407 (19) | −0.0013 (10) | −0.041 (2) |
O15 | 0.071 | 0.0740 (14) | 0.0735 (14) | −0.0286 (9) | −0.0011 (10) | −0.0281 (9) |
O16 | 0.065 | 0.0671 (14) | 0.0681 (14) | −0.0247 (9) | 0.0013 (10) | −0.0260 (9) |
O20 | 0.070 | 0.0720 (14) | 0.0725 (14) | −0.0269 (9) | −0.0014 (10) | −0.0284 (9) |
O21 | 0.073 | 0.0752 (14) | 0.0755 (14) | −0.0280 (9) | 0.0001 (10) | −0.0299 (9) |
O22 | 0.069 | 0.0718 (14) | 0.0719 (14) | −0.0270 (9) | −0.0005 (10) | −0.0270 (9) |
O23 | 0.073 | 0.0748 (14) | 0.0756 (14) | −0.0284 (9) | −0.0003 (10) | −0.0296 (9) |
O24 | 0.099 (6) | 0.090 (6) | 0.102 (6) | −0.038 (4) | −0.011 (4) | −0.039 (4) |
O25 | 0.086 (7) | 0.089 (7) | 0.103 (7) | −0.048 (6) | −0.002 (6) | −0.027 (6) |
Si1 | 0.030 (3) | 0.028 (3) | 0.034 (3) | −0.016 (2) | −0.003 (2) | −0.012 (2) |
W1 | 0.0733 (6) | 0.0643 (5) | 0.0641 (5) | −0.0262 (4) | −0.0138 (4) | −0.0260 (4) |
W2 | 0.0584 (5) | 0.0737 (5) | 0.0790 (5) | −0.0308 (4) | 0.0105 (4) | −0.0432 (4) |
W3 | 0.0619 (5) | 0.0606 (5) | 0.0648 (5) | −0.0339 (4) | −0.0006 (4) | −0.0142 (4) |
W4 | 0.0500 (5) | 0.0564 (5) | 0.0943 (6) | −0.0321 (4) | 0.0020 (4) | −0.0370 (4) |
W5 | 0.0659 (5) | 0.0423 (4) | 0.0931 (6) | −0.0207 (4) | −0.0157 (4) | −0.0255 (4) |
W6 | 0.0426 (5) | 0.0628 (5) | 0.0922 (6) | −0.0211 (4) | −0.0124 (4) | −0.0210 (4) |
Geometric parameters (Å, º) top
N1—C1 | 1.31 (2) | C36—H36C | 0.9600 |
N1—C5 | 1.31 (2) | C37—C38 | 1.49 (4) |
N1—C14 | 1.45 (2) | C37—N4 | 1.51 (3) |
N2—C11 | 1.42 (3) | C37—H37A | 0.9700 |
N2—C17 | 1.50 (3) | C37—H37B | 0.9700 |
N2—C15 | 1.60 (3) | C38—H38A | 0.9600 |
C1—C2 | 1.32 (2) | C38—H38B | 0.9600 |
C1—H1A | 0.9300 | C38—H38C | 0.9600 |
C2—C3 | 1.34 (2) | Si1—O1i | 1.619 (17) |
C2—H2A | 0.9300 | Si1—O2 | 1.566 (17) |
C3—C4 | 1.41 (2) | Si1—O3 | 1.687 (18) |
C3—C6 | 1.468 (16) | Si1—O4 | 1.618 (18) |
C4—C5 | 1.279 (15) | O1—Si1 | 1.619 (17) |
C4—H4A | 0.9300 | O1—W1 | 2.375 (18) |
C5—H5A | 0.9300 | O1—W2 | 2.386 (18) |
C6—C7 | 1.29 (3) | O1—W3 | 2.419 (16) |
C6—H6A | 0.9300 | O2—W4 | 2.414 (18) |
C7—C8 | 1.38 (3) | O2—W3 | 2.420 (18) |
C7—H7A | 0.9300 | O2—W5 | 2.428 (19) |
C8—C13 | 1.32 (3) | O3—W2 | 2.330 (17) |
C8—C9 | 1.37 (4) | O3—W5i | 2.371 (17) |
C9—C10 | 1.31 (3) | O3—W6i | 2.374 (17) |
C9—H9A | 0.9300 | O4—W1 | 2.374 (18) |
C10—C11 | 1.43 (3) | O4—W4i | 2.382 (18) |
C10—H10A | 0.9300 | O4—W6 | 2.423 (18) |
C11—C12 | 1.40 (3) | O5—W1 | 1.815 (11) |
C12—C13 | 1.45 (3) | O5—W2 | 1.971 (11) |
C12—H12A | 0.9300 | O6—W1 | 1.863 (11) |
C13—H13A | 0.9300 | O6—W3 | 1.901 (11) |
C14—H14A | 0.9600 | O7—W3 | 1.823 (11) |
C14—H14B | 0.9600 | O7—W2 | 1.941 (10) |
C14—H14C | 0.9600 | O8—W6i | 1.871 (13) |
C15—C16 | 1.511 (17) | O8—W2 | 1.910 (13) |
C15—H15A | 0.9700 | O9—W4 | 1.892 (10) |
C15—H15B | 0.9700 | O9—W3 | 1.919 (11) |
C16—H16A | 0.9600 | O10—W5 | 1.874 (10) |
C16—H16B | 0.9600 | O10—W3 | 1.916 (11) |
C16—H16C | 0.9600 | O11—W5 | 1.890 (11) |
C17—C18 | 1.52 (4) | O11—W4 | 1.900 (10) |
C17—H17A | 0.9700 | O12—W6i | 1.903 (11) |
C17—H17B | 0.9700 | O12—W4 | 1.916 (11) |
C18—H18A | 0.9600 | O13—W1 | 1.880 (11) |
C18—H18B | 0.9600 | O13—W4i | 1.900 (11) |
C18—H18C | 0.9600 | O14—W5i | 1.856 (13) |
C21—N3 | 1.33 (2) | O14—W2 | 1.913 (13) |
C21—C22 | 1.37 (2) | O15—W6 | 1.850 (11) |
C21—H21A | 0.9300 | O15—W5 | 1.915 (11) |
C22—C23A | 1.35 (2) | O16—W6 | 1.873 (10) |
C22—H22A | 0.9200 | O16—W1 | 1.898 (10) |
C24—C23A | 1.29 (2) | O20—W1 | 1.669 (11) |
C24—C25 | 1.350 (16) | O21—W2 | 1.642 (11) |
C24—H24A | 0.9300 | O22—W3 | 1.649 (10) |
C25—N3 | 1.35 (2) | O23—W4 | 1.656 (11) |
C25—H25A | 0.9300 | O24—W5 | 1.663 (12) |
C23A—C26A | 1.50 (2) | O25—W6 | 1.634 (12) |
C26A—C27A | 1.32 (3) | OW1—OW7 | 1.32 (8) |
C26A—H26A | 0.9300 | OW2—OW6 | 1.50 (6) |
C26A—H27B | 1.03 (3) | OW2—OW8 | 1.55 (7) |
C27A—C28 | 1.476 (19) | OW2—OW13ii | 1.74 (6) |
C27A—H27A | 0.9300 | OW3—OW9 | 1.1668 (2) |
C27A—H26B | 0.85 (3) | OW4—OW10 | 1.55 (7) |
C26B—C27B | 1.34 (3) | OW5—OW10 | 0.92 (8) |
C26B—H26B | 0.93 (3) | OW5—OW11 | 1.44 (7) |
C27B—C28 | 1.483 (19) | OW5—OW9 | 1.57 (6) |
C27B—H27B | 0.96 (3) | OW6—OW8 | 1.38 (7) |
C28—C33 | 1.38 (4) | OW6—OW13ii | 1.48 (6) |
C28—C29 | 1.44 (4) | OW7—OW14 | 1.55 (9) |
C29—C30 | 1.36 (4) | OW7—OW12 | 1.69 (8) |
C29—H29A | 0.9300 | OW8—OW13ii | 1.73 (7) |
C30—C31 | 1.40 (5) | OW9—OW10 | 1.41 (7) |
C30—H30A | 0.9300 | OW10—OW11 | 1.72 (8) |
C31—N4 | 1.35 (3) | OW13—OW6ii | 1.48 (6) |
C31—C32 | 1.41 (5) | OW13—OW8ii | 1.73 (7) |
C32—C33 | 1.33 (4) | OW13—OW2ii | 1.74 (6) |
C32—H32A | 0.9300 | Si1—O2i | 1.566 (17) |
C33—H33A | 0.9300 | Si1—O4i | 1.618 (18) |
C34—N3 | 1.42 (2) | Si1—O1i | 1.619 (17) |
C34—H34A | 0.9600 | Si1—O3i | 1.687 (18) |
C34—H34B | 0.9600 | W4—O13i | 1.900 (11) |
C34—H34C | 0.9600 | W4—O4i | 2.382 (18) |
C35—C36 | 1.49 (4) | W5—O14i | 1.856 (13) |
C35—N4 | 1.61 (3) | W5—O3i | 2.371 (17) |
C35—H35A | 0.9700 | W6—O8i | 1.871 (13) |
C35—H35B | 0.9700 | W6—O12i | 1.903 (11) |
C36—H36A | 0.9600 | W6—O3i | 2.374 (17) |
C36—H36B | 0.9600 | | |
| | | |
C1—N1—C5 | 114.0 (19) | W5—O11—W4 | 136.9 (6) |
C1—N1—C14 | 123.2 (15) | W6i—O12—W4 | 135.8 (6) |
C5—N1—C14 | 122.7 (15) | W1—O13—W4i | 137.8 (7) |
C11—N2—C17 | 122 (2) | W5i—O14—W2 | 138.9 (8) |
C11—N2—C15 | 123 (2) | W6—O15—W5 | 137.0 (6) |
C17—N2—C15 | 110 (2) | W6—O16—W1 | 139.1 (6) |
N1—C1—C2 | 123 (2) | OW6—OW2—OW8 | 54 (3) |
N1—C1—H1A | 118.5 | OW6—OW2—OW13ii | 54 (3) |
C2—C1—H1A | 118.5 | OW8—OW2—OW13ii | 63 (3) |
C1—C2—C3 | 123 (2) | OW10—OW5—OW11 | 91 (7) |
C1—C2—H2A | 118.5 | OW10—OW5—OW9 | 63 (7) |
C3—C2—H2A | 118.5 | OW11—OW5—OW9 | 81 (4) |
C2—C3—C4 | 113.2 (18) | OW8—OW6—OW13ii | 75 (4) |
C2—C3—C6 | 132 (2) | OW8—OW6—OW2 | 65 (4) |
C4—C3—C6 | 114.5 (19) | OW13ii—OW6—OW2 | 72 (4) |
C5—C4—C3 | 119 (2) | OW1—OW7—OW14 | 99 (8) |
C5—C4—H4A | 120.3 | OW1—OW7—OW12 | 136 (7) |
C3—C4—H4A | 120.3 | OW14—OW7—OW12 | 101 (7) |
C4—C5—N1 | 127 (2) | OW6—OW8—OW2 | 61 (4) |
C4—C5—H5A | 116.6 | OW6—OW8—OW13ii | 55 (3) |
N1—C5—H5A | 116.6 | OW2—OW8—OW13ii | 64 (3) |
C7—C6—C3 | 130 (2) | OW3—OW9—OW10 | 134 (3) |
C7—C6—H6A | 114.8 | OW3—OW9—OW5 | 105 (2) |
C3—C6—H6A | 114.8 | OW5—OW10—OW9 | 82 (7) |
C6—C7—C8 | 132 (2) | OW5—OW10—OW4 | 135 (9) |
C6—C7—H7A | 113.8 | OW9—OW10—OW4 | 135 (5) |
C8—C7—H7A | 113.8 | OW5—OW10—OW11 | 57 (6) |
C13—C8—C9 | 116 (2) | OW9—OW10—OW11 | 77 (4) |
C13—C8—C7 | 127 (2) | OW4—OW10—OW11 | 101 (4) |
C9—C8—C7 | 117 (2) | OW6ii—OW13—OW8ii | 50 (3) |
C10—C9—C8 | 127 (3) | OW6ii—OW13—OW2ii | 55 (3) |
C10—C9—H9A | 116.6 | OW8ii—OW13—OW2ii | 53 (3) |
C8—C9—H9A | 116.6 | O2—Si1—O1i | 108.9 (9) |
C9—C10—C11 | 117 (2) | O3—Si1—O1i | 111.3 (9) |
C9—C10—H10A | 121.3 | O4—Si1—O1i | 110.7 (9) |
C11—C10—H10A | 121.3 | O2—Si1—O3 | 108.9 (9) |
C12—C11—N2 | 122 (3) | O2—Si1—O4 | 109.3 (10) |
C12—C11—C10 | 120 (3) | O3—Si1—O4 | 107.8 (9) |
N2—C11—C10 | 118 (2) | O2—Si1—O2i | 180.0 (8) |
C11—C12—C13 | 115 (2) | O2—Si1—O4i | 70.7 (10) |
C11—C12—H12A | 122.3 | O2i—Si1—O4i | 109.3 (10) |
C13—C12—H12A | 122.3 | O2i—Si1—O4 | 70.7 (10) |
C8—C13—C12 | 124 (2) | O4i—Si1—O4 | 180.000 (4) |
C8—C13—H13A | 117.9 | O2i—Si1—O1i | 71.1 (9) |
C12—C13—H13A | 117.9 | O4i—Si1—O1i | 69.3 (9) |
N1—C14—H14A | 109.5 | O2—Si1—O1 | 71.1 (9) |
N1—C14—H14B | 109.5 | O2i—Si1—O1 | 108.9 (9) |
H14A—C14—H14B | 109.5 | O4i—Si1—O1 | 110.7 (9) |
N1—C14—H14C | 109.5 | O4—Si1—O1 | 69.3 (9) |
H14A—C14—H14C | 109.5 | O1i—Si1—O1 | 180.000 (3) |
H14B—C14—H14C | 109.5 | O2i—Si1—O3 | 71.1 (9) |
C16—C15—N2 | 99 (2) | O4i—Si1—O3 | 72.2 (9) |
C16—C15—H15A | 112.0 | O3—Si1—O1 | 68.7 (9) |
N2—C15—H15A | 112.0 | O2—Si1—O3i | 71.1 (9) |
C16—C15—H15B | 112.0 | O2i—Si1—O3i | 108.9 (9) |
N2—C15—H15B | 112.0 | O4i—Si1—O3i | 107.8 (9) |
H15A—C15—H15B | 109.7 | O4—Si1—O3i | 72.2 (9) |
C15—C16—H16A | 109.5 | O1i—Si1—O3i | 68.7 (9) |
C15—C16—H16B | 109.5 | O1—Si1—O3i | 111.3 (9) |
H16A—C16—H16B | 109.5 | O3—Si1—O3i | 180.000 (3) |
C15—C16—H16C | 109.5 | O20—W1—O5 | 98.5 (5) |
H16A—C16—H16C | 109.5 | O20—W1—O6 | 103.0 (5) |
H16B—C16—H16C | 109.5 | O5—W1—O6 | 90.9 (5) |
N2—C17—C18 | 101 (2) | O20—W1—O13 | 99.0 (5) |
N2—C17—H17A | 111.5 | O5—W1—O13 | 85.4 (5) |
C18—C17—H17A | 111.5 | O6—W1—O13 | 158.0 (5) |
N2—C17—H17B | 111.5 | O20—W1—O16 | 103.8 (5) |
C18—C17—H17B | 111.5 | O5—W1—O16 | 157.6 (5) |
H17A—C17—H17B | 109.3 | O6—W1—O16 | 86.6 (4) |
C17—C18—H18A | 109.5 | O13—W1—O16 | 88.6 (5) |
C17—C18—H18B | 109.5 | O20—W1—O4 | 156.8 (6) |
H18A—C18—H18B | 109.5 | O5—W1—O4 | 94.9 (6) |
C17—C18—H18C | 109.5 | O6—W1—O4 | 95.6 (5) |
H18A—C18—H18C | 109.5 | O13—W1—O4 | 63.2 (6) |
H18B—C18—H18C | 109.5 | O16—W1—O4 | 63.2 (5) |
N3—C21—C22 | 121.1 (18) | O20—W1—O1 | 157.2 (6) |
N3—C21—H21A | 119.4 | O5—W1—O1 | 64.3 (5) |
C22—C21—H21A | 119.4 | O6—W1—O1 | 64.4 (5) |
C23A—C22—C21 | 121.3 (17) | O13—W1—O1 | 94.7 (5) |
C23A—C22—H22A | 128 (2) | O16—W1—O1 | 94.7 (5) |
C21—C22—H22A | 111.00 | O4—W1—O1 | 45.6 (6) |
C23A—C24—C25 | 125.2 (18) | O21—W2—O8 | 101.9 (6) |
C23A—C24—H24A | 117.4 | O21—W2—O14 | 102.4 (5) |
C25—C24—H24A | 117.4 | O8—W2—O14 | 88.3 (6) |
C24—C25—N3 | 119 (2) | O21—W2—O7 | 102.6 (5) |
C24—C25—H25A | 120.4 | O8—W2—O7 | 86.9 (5) |
N3—C25—H25A | 120.4 | O14—W2—O7 | 155.0 (5) |
C24—C23A—C22 | 115.7 (18) | O21—W2—O5 | 101.7 (5) |
C24—C23A—C26A | 139 (2) | O8—W2—O5 | 156.3 (5) |
C22—C23A—C26A | 104 (2) | O14—W2—O5 | 85.1 (5) |
C27A—C26A—C23A | 120 (3) | O7—W2—O5 | 89.5 (4) |
C27A—C26A—H26A | 120.2 | O21—W2—O3 | 156.8 (6) |
C23A—C26A—H26A | 120.2 | O8—W2—O3 | 63.0 (6) |
C26A—C27A—C28 | 123 (3) | O14—W2—O3 | 61.8 (6) |
C26A—C27A—H27A | 118.5 | O7—W2—O3 | 94.3 (5) |
C28—C27A—H27A | 118.5 | O5—W2—O3 | 94.1 (6) |
C27B—C26B—H26B | 94 (3) | O21—W2—O1 | 156.6 (6) |
C26B—C27B—C28 | 118 (3) | O8—W2—O1 | 95.6 (6) |
C26B—C27B—H27B | 104 (3) | O14—W2—O1 | 93.5 (6) |
C28—C27B—H27B | 137 (3) | O7—W2—O1 | 62.6 (5) |
C33—C28—C29 | 117.7 (15) | O5—W2—O1 | 62.3 (5) |
C33—C28—C27A | 107 (2) | O3—W2—O1 | 46.6 (6) |
C29—C28—C27A | 136 (2) | O22—W3—O7 | 100.6 (5) |
C33—C28—C27B | 142 (2) | O22—W3—O6 | 103.2 (5) |
C29—C28—C27B | 101 (2) | O7—W3—O6 | 89.6 (5) |
C30—C29—C28 | 119.9 (19) | O22—W3—O10 | 102.0 (5) |
C30—C29—H29A | 120.0 | O7—W3—O10 | 157.3 (5) |
C28—C29—H29A | 120.0 | O6—W3—O10 | 88.2 (5) |
C29—C30—C31 | 121 (3) | O22—W3—O9 | 98.5 (5) |
C29—C30—H30A | 119.5 | O7—W3—O9 | 85.0 (5) |
C31—C30—H30A | 119.5 | O6—W3—O9 | 158.3 (4) |
N4—C31—C30 | 121 (2) | O10—W3—O9 | 88.7 (5) |
N4—C31—C32 | 121 (3) | O22—W3—O1 | 157.2 (6) |
C30—C31—C32 | 118 (3) | O7—W3—O1 | 63.2 (5) |
C33—C32—C31 | 121 (3) | O6—W3—O1 | 63.0 (5) |
C33—C32—H32A | 119.3 | O10—W3—O1 | 95.9 (5) |
C31—C32—H32A | 119.3 | O9—W3—O1 | 96.0 (5) |
C32—C33—C28 | 121.6 (19) | O22—W3—O2 | 157.6 (6) |
C32—C33—H33A | 119.2 | O7—W3—O2 | 93.5 (6) |
C28—C33—H33A | 119.2 | O6—W3—O2 | 94.2 (5) |
N3—C34—H34A | 109.5 | O10—W3—O2 | 64.2 (6) |
N3—C34—H34B | 109.5 | O9—W3—O2 | 65.2 (5) |
H34A—C34—H34B | 109.5 | O1—W3—O2 | 45.0 (6) |
N3—C34—H34C | 109.5 | O23—W4—O9 | 100.1 (5) |
H34A—C34—H34C | 109.5 | O23—W4—O13i | 100.6 (5) |
H34B—C34—H34C | 109.5 | O9—W4—O13i | 159.3 (5) |
C36—C35—N4 | 100.6 (19) | O23—W4—O11 | 100.9 (5) |
C36—C35—H35A | 111.7 | O9—W4—O11 | 89.4 (5) |
N4—C35—H35A | 111.7 | O13i—W4—O11 | 87.1 (5) |
C36—C35—H35B | 111.7 | O23—W4—O12 | 99.0 (5) |
N4—C35—H35B | 111.7 | O9—W4—O12 | 88.9 (5) |
H35A—C35—H35B | 109.4 | O13i—W4—O12 | 87.5 (5) |
C35—C36—H36A | 109.5 | O11—W4—O12 | 160.1 (5) |
C35—C36—H36B | 109.5 | O23—W4—O4i | 156.1 (6) |
H36A—C36—H36B | 109.5 | O9—W4—O4i | 97.3 (5) |
C35—C36—H36C | 109.5 | O13i—W4—O4i | 62.8 (6) |
H36A—C36—H36C | 109.5 | O11—W4—O4i | 95.5 (5) |
H36B—C36—H36C | 109.5 | O12—W4—O4i | 65.0 (5) |
C38—C37—N4 | 105 (2) | O23—W4—O2 | 158.7 (6) |
C38—C37—H37A | 110.7 | O9—W4—O2 | 65.7 (5) |
N4—C37—H37A | 110.7 | O13i—W4—O2 | 94.5 (6) |
C38—C37—H37B | 110.7 | O11—W4—O2 | 64.8 (5) |
N4—C37—H37B | 112.0 | O12—W4—O2 | 96.6 (6) |
H37A—C37—H37B | 108.8 | O4i—W4—O2 | 45.2 (6) |
C37—C38—H38A | 109.5 | O24—W5—O14i | 101.1 (6) |
C37—C38—H38B | 109.5 | O24—W5—O10 | 100.9 (5) |
H38A—C38—H38B | 109.5 | O14i—W5—O10 | 158.0 (5) |
C37—C38—H38C | 109.5 | O24—W5—O11 | 100.4 (5) |
H38A—C38—H38C | 109.5 | O14i—W5—O11 | 87.5 (5) |
H38B—C38—H38C | 109.5 | O10—W5—O11 | 88.0 (5) |
C21—N3—C25 | 117.3 (19) | O24—W5—O15 | 101.3 (5) |
C21—N3—C34 | 122.2 (15) | O14i—W5—O15 | 89.3 (5) |
C25—N3—C34 | 120.3 (15) | O10—W5—O15 | 86.9 (5) |
C31—N4—C37 | 125 (3) | O11—W5—O15 | 158.2 (5) |
C31—N4—C35 | 120 (2) | O24—W5—O3i | 155.3 (6) |
C37—N4—C35 | 113 (2) | O14i—W5—O3i | 61.6 (6) |
Si1—O1—W1 | 122.5 (9) | O10—W5—O3i | 97.6 (5) |
Si1—O1—W2 | 122.5 (9) | O11—W5—O3i | 96.4 (5) |
W1—O1—W2 | 95.4 (6) | O15—W5—O3i | 63.4 (5) |
Si1—O1—W3 | 120.6 (9) | O24—W5—O2 | 158.2 (6) |
W1—O1—W3 | 94.2 (6) | O14i—W5—O2 | 94.3 (6) |
W2—O1—W3 | 94.4 (6) | O10—W5—O2 | 64.5 (5) |
Si1—O2—W4 | 122.4 (11) | O11—W5—O2 | 64.6 (5) |
Si1—O2—W3 | 123.2 (9) | O15—W5—O2 | 94.2 (5) |
W4—O2—W3 | 93.5 (6) | O3i—W5—O2 | 46.5 (6) |
Si1—O2—W5 | 122.6 (10) | O25—W6—O15 | 100.9 (5) |
W4—O2—W5 | 93.4 (6) | O25—W6—O8i | 100.3 (6) |
W3—O2—W5 | 93.6 (7) | O15—W6—O8i | 90.2 (5) |
Si1—O3—W2 | 122.2 (9) | O25—W6—O16 | 102.1 (5) |
Si1—O3—W5i | 119.8 (8) | O15—W6—O16 | 87.1 (5) |
W2—O3—W5i | 97.3 (6) | O8i—W6—O16 | 157.5 (5) |
Si1—O3—W6i | 119.6 (9) | O25—W6—O12i | 99.2 (5) |
W2—O3—W6i | 96.9 (6) | O15—W6—O12i | 159.9 (5) |
W5i—O3—W6i | 95.2 (6) | O8i—W6—O12i | 87.6 (5) |
Si1—O4—W1 | 122.6 (9) | O16—W6—O12i | 87.3 (5) |
Si1—O4—W4i | 121.7 (9) | O25—W6—O3i | 155.5 (6) |
W1—O4—W4i | 95.7 (7) | O15—W6—O3i | 64.1 (5) |
Si1—O4—W6 | 120.3 (9) | O8i—W6—O3i | 62.5 (6) |
W1—O4—W6 | 94.9 (6) | O16—W6—O3i | 96.5 (5) |
W4i—O4—W6 | 94.9 (6) | O12i—W6—O3i | 97.4 (5) |
W1—O5—W2 | 137.0 (6) | O25—W6—O4 | 156.5 (6) |
W1—O6—W3 | 138.0 (6) | O15—W6—O4 | 96.0 (5) |
W3—O7—W2 | 139.1 (6) | O8i—W6—O4 | 95.8 (6) |
W6i—O8—W2 | 137.2 (7) | O16—W6—O4 | 62.4 (5) |
W4—O9—W3 | 135.0 (6) | O12i—W6—O4 | 64.3 (5) |
W5—O10—W3 | 137.5 (6) | O3i—W6—O4 | 47.9 (6) |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+2, −y+1, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1A···O8 | 0.93 | 2.53 | 3.27 (2) | 137 |
C2—H2A···O9 | 0.93 | 2.52 | 3.34 (2) | 148 |
C4—H4A···O25iii | 0.93 | 2.48 | 3.30 (2) | 147 |
C14—H14A···O23iv | 0.96 | 2.44 | 3.39 (2) | 169 |
C22—H22A···O24 | 0.92 | 2.48 | 3.33 (2) | 153 |
C25—H25A···O14v | 0.93 | 2.47 | 3.20 (2) | 136 |
Symmetry codes: (iii) x−1, y, z; (iv) −x, −y+2, −z+1; (v) x, y−1, z. |