Hexa­kis­(adamantyl­trimethyl­ammonium) cyclo­octa­silicate tetra­tetra­conta­hydrate

The title compound, 6C₁₃H₂₄N⁺·H₂Si₈O₂₀^6-·44H₂O, belongs to the class of cyclo­silicate hydrates, which structurally can be positioned between the zeosils and the clathrate hydrates. [Si₈O₁₈(OH)₂] cubes carrying six negative charges are located on crystallographic inversion centres and are surrounded by six adamantyl­trimethyl­ammonium cations.

S1. Comment

Silicate hydrates are materials that structurally can be positioned between silicon dioxide-based zeolites, called zeosils, and silicate clathrate hydrates. In zeolites, (organic) template molecules are embedded in the pores of a four-connected silicon dioxide network. The template molecules reside in zero-, one-, two- or three-dimensional pores. In the crystal structure of clathrate hydrates, the template molecules are partially or entirely surrounded by water molecules. Silicate hydrates are crystalline materials consisting of water, individual silicate units and organic cations. The organic cations are embedded in cages or pores formed by a network of hydrogen-bonded water molecules and oligomeric silicate clusters (Wiebcke, 1991; Grube et al., 1993).

The templates used to synthesize silicate hydrate materials can be subdivided into different groups (Verlooy et al., 2010). The first group of organic templates consists of N-methyl quaternary amines (references 2–20 in Verlooy et al., 2010), the second group consists of the other quaternary amines (references 18 and 21–25 in Verlooy et al., 2010) and the third group comprises the metal–ethylenediamine complexes (references 26–30 in Verlooy et al., 2010). α-Cyclodextrine (Benner et al., 1997) and hexamethyleneimine (Verlooy et al., 2010) are the only reported templates that do not fit this classification.

In the group of silicate hydrate materials synthesized with N-methyl quaternary amines, which form the majority of reported silicate hydrate materials, silicate cubes are surrounded by a shell of 24 water molecules. This observation is generally referred to as the `24-water rule' (Wiebcke et al., 1994). Another generally observed property of silicate hydrate structures is the relationship between the environment and the C/N ratio of the organic template molecules. Among all reported silicate hydrates reported to date, organic template molecules with a low C/N ratio where found to reside in one-dimensional pores. Organic template molecules with a high C/N ratio are generally found in two- or three-dimensional pore architectures (Smolin, 1970; Bissert & Liebau, 1987; Emmer & Wiebcke, 1994; Wiebcke et al., 1995; Shantz & Lobo, 2001; Wiebcke & Felsche, 2001). So far no silicate hydrates with a C/N ratio higher then 10 have been synthesized (Wiebcke et al., 1995; Shantz & Lobo, 2001).

Here we report the title compound, (I), a silicate hydrate structure synthesized using an organic template with a C/N ratio of 13. In this new silicate hydrate structure the organic template cations, N,N,N-trimethyladamantylammonium (TMAda), reside in a two-dimensional pore structure enclosed by a hydrogen-bonded network formed by the silicate units and water molecules.

The crystals of (I) belong to the triclinic space group P1, with the silicate cage located on an inversion point (Fig. 1). The negative charges (6-) on the terminal O atoms are compensated by six TMAda cations (1+), pointing, with the trimethylammonium group, towards the faces of the silicate cage. Each template molecule is orientated in such a way that the distances between its N atom and the four Si atoms of one face of the cube are all in the range 4.8–5.1 Å.

Individual silicate cages are linked together by a hydrogen-bond network involving water molecules. The silicate units are separated by at least three water molecules. The hydrogen bonding gives rise to a pentagonal network (Fig. 2). The hydrophobic carbon-rich template molecules are grouped together, minimizing exposure to the hydrogen-bonded silicate–water network. This network surrounds the TMAda cations in two directions, where the template clusters are elongated along the c direction, basically forming hydrophobic columns embedded in a hydrophilic silicate–water matrix. When analysing the water network, most water molecules are located between the silicate cubes in the a and b directions. Along the c direction, the silicate cubes are less strongly connected through hydrogen bonding. Each terminal O atom (O^- or OH) on the silicate cube is engaged in three hydrogen bonds with neighbouring water molecules, arranged in a tetragonal geometry. The hydrogen-bond distances and angles for (I) are reported in Table 1. Anisotropic displacement parameters are represented in Fig. 3. The water OH bonds were fixed at 0.84 Å, with an angle of 108° between them. The reported hydrogen-bond H···A distances are in the range 1.78–2.12 Å, and the hydrogen-bond angles D—H···A are in the range 129.2–177.2°.

Single-crystal X-ray diffraction revealed half a silicate cube in the asymmetric unit of (I). The ²⁹Si MAS NMR spectrum of (I) shows three sharp signals at ca -98.7, -99.6 and -100.0 p.p.m. with respect to the reference trimethylsiloxane chemical shift, pointing to the presence of three types of silicate environments with a Q³ connectivity (Fig. 4). ²⁹Si NMR resonances of silicate cubes are generally found around -99.5 p.p.m. The reduced symmetry of the silicate cube can give rise to different local environments, thereby generating different ²⁹Si resonance signals (Harris et al., 1995; Harris & Naumov 1996; Wiebcke & Koller 1992; Wiebcke et al., 1993, 1994). Furthermore, a different charge on the terminal O atoms (O^- versus OH) could also result in small differences in the NMR frequency of the Si atoms. Therefore, the ²⁹Si MAS NMR spectrum of (I) can be explained by the presence of a single type of anionic silicate cube with a reduced symmetry, confirming the results obtained from single-crystal diffraction experiments.

S2. Experimental

N,N,N-Trimethyladamantylammonium hydroxide (TMAdaOH) was prepared by ion exchange from the iodide, which was obtained by reaction of 1-adamantylamine (Acros, 99%) with an excess of methyl iodide (Acros, 99%) according to the procedure of Zones (1985).

Silicate hydrate crystals were synthesized at room temperature from a clear solution, prepared by adding tetraethyl orthosilicate (TEOS; Acros, 98%) under vigorous stirring to a 0.7 M aqueous solution of TMAdaOH. The clear solution was then stirred continuously until crystals of (I) formed.

The ²⁹Si MAS NMR spectrum was recorded on a Bruker AMX300 spectrometer. 4000 scans with a recycle delay of 60 s were accumulated.

S3. Refinement

The crystal structure displays a high degree of disorder of the template molecules. Of the three TMAda cations in the asymmetric unit, only one shows no disorder. A second molecule is present in two conformations [refined occupancy = 0.522 (6):0.478 (6) for adamantane and 0.559 (22):0.441 (22) for trimethylammonium], rotated approximately 60° around the N–adamantyl bond. The third cation shows threefold disorder, also around the N–adamantyl bond (occupancies were fixed at 0.333). The amandantane substructures of this threefold disordered TMAda cation were refined to target values provided by the undisordered one. Distance restraints were set-up with a standard deviation of 0.01 Å, the standard deviation on the angle restraints, expressed as 1,3-distances, were set at twice this value (0.02°). No distance or angle restraints were applied to the second cation showing twofold disorder. Rigid-bond restraints (standard deviation = 0.005 Å) were applied within every part of the threefold disordered amandantane substructure and simultaneous the same anisotropic displacement parameters were used for all corresponding atoms in the three disordered parts. Moreover, the individual thermal displacement components of the threefold disordered amandantane are refined to approximate to isotropic behavior (standard deviation = 0.01 Ų). The same anisotropic displacement parameters were used for the C atoms of the two parts of the trimethylamonium group attached to the threefold disordered amandantane substructure (the C atoms of one disordered part are refined without thermal displacement restraints, the other disordered part is pairwise given the same displacement parameters. The twofold disordered methyl groups of the trimethylammonium group attached to the threefold disordered amandantane were refined with site-occupation factors of 0.455 (6):0.545 (6).

The silanol H atom was located in a difference map, as were the majority of water H atoms. These H atoms were, after location in a difference map, fixed on their parent O atoms and the water molecules were refined as rigid groups, with the H atoms as dependent atoms able to rotate around and move with their O atoms, while retaining an idealized geometry. For the remaining water H atoms that could not be unequivocally located, the H-atom position was chosen to optimize the hydrogen-bond network, and again the water molecules were treated as above. For all H atoms, U_iso(H) = 1.2U_eq(parent atom) or 1.5U_eq(C) for methyl groups. The solvent water OH bonds were fixed at 0.84 Å, with a 108° angle between them. The reported hydrogen-bond H···A distances are in the range 1.78–2.12 Å and the hydrogen-bond D—H···A angle is in the range 129.2–177.2°. This is on average 1.92 Å and 165.2° for 39 observed hydrogen bonds.

Part of the solvent, 55 electrons (presumably water or ethanol molecules), in a cavity of 158 ų centred about an inversion centre, could not be modelled and was treated with the SQUEEZE procedure in PLATON (Spek, 2009). This solvent has not been included in the reported empirical formula, M_r, F(000), calculated density or linear absorption coefficient.

Computing details

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLUTON (Spek, 2009); software used to prepare material for publication: PLATON (Spek, 2009).

Figures

	Fig. 1. Stick representation of the title compound. Six TMAda cations surround the silicate cage. Only water molecules in the first hydration shell are shown, for clarity.
	Fig. 2. Stick representation of the crystal packing of (I), with the water molecules connecting neighbouring silicate cages. The hydrogen bonds (dashed lines) form pentagonal networks. H atoms and TMAda cations have been omitted for clarity.
	Fig. 3. The structure of (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. Only one component of the disordered template is shown. [Symmetry code: (a) 2 - x, -y, 1 - z.]
	Fig. 4. The ^29Si MAS NMR spectrum of crystals of (I).

Hexakis(adamantyltrimethylammonium) cyclooctasilicate tetratetracontahydrate

Crystal data

6C13H24N^+·H2O20Si8^6^−·44H2O	V = 3356.8 (3) Å^3
Mr = 2505.44	Z = 1
Triclinic, P1	F(000) = 1368
Hall symbol: -P 1	Dx = 1.239 Mg m^−3
a = 15.5889 (8) Å	Cu Kα radiation, λ = 1.54178 Å
b = 15.9297 (8) Å	µ = 1.53 mm^−1
c = 16.2269 (11) Å	T = 100 K
α = 60.863 (2)°	Plate, colourless
β = 72.511 (3)°	0.24 × 0.24 × 0.10 mm
γ = 82.119 (2)°

Data collection

Bruker SMART 6000 diffractometer	12596 independent reflections
Radiation source: fine-focus sealed tube	10388 reflections with I > 2σ(I)
Crossed Goebel mirrors monochromator	Rint = 0.041
ω and ϕ scans	θmax = 71.2°, θmin = 3.0°
Absorption correction: multi-scan (SADABS; Bruker, 1997)	h = −18→17
Tmin = 0.587, Tmax = 0.858	k = −19→19
66631 measured reflections	l = −19→19

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.065	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.186	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.1073P)^2 + 3.7976P] where P = (Fo^2 + 2Fc^2)/3
12596 reflections	(Δ/σ)max = 0.001
942 parameters	Δρmax = 0.90 e Å^−3
399 restraints	Δρmin = −0.69 e Å^−3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.6760 (2)	0.9274 (2)	0.1490 (2)	0.0360 (7)
H1	0.6582	0.9791	0.0900	0.043*
C2	0.6078 (2)	0.9221 (3)	0.2411 (3)	0.0448 (8)
H2A	0.5470	0.9088	0.2425	0.054*
H2B	0.6064	0.9843	0.2414	0.054*
C3	0.6348 (3)	0.8415 (3)	0.3314 (3)	0.0463 (9)
H3	0.5900	0.8372	0.3922	0.056*
C4	0.6367 (3)	0.7462 (3)	0.3303 (3)	0.0518 (10)
H4A	0.6540	0.6940	0.3883	0.062*
H4B	0.5761	0.7310	0.3329	0.062*
C5	0.7040 (2)	0.7534 (2)	0.2371 (3)	0.0432 (8)
H5	0.7052	0.6908	0.2365	0.052*
C6	0.6787 (2)	0.8313 (3)	0.1486 (3)	0.0436 (8)
H6A	0.6190	0.8168	0.1486	0.052*
H6B	0.7232	0.8350	0.0886	0.052*
C7	0.7695 (2)	0.9506 (2)	0.1457 (2)	0.0288 (6)
H7A	0.8137	0.9555	0.0852	0.035*
H7B	0.7686	1.0130	0.1455	0.035*
C8	0.7275 (2)	0.8652 (2)	0.3289 (2)	0.0407 (8)
H8A	0.7451	0.8149	0.3877	0.049*
H8B	0.7257	0.9275	0.3290	0.049*
C9	0.7983 (2)	0.7745 (2)	0.2361 (2)	0.0342 (7)
H9A	0.8152	0.7228	0.2947	0.041*
H9B	0.8435	0.7769	0.1771	0.041*
C10	0.7967 (2)	0.8707 (2)	0.2357 (2)	0.0266 (6)
N11	0.89302 (19)	0.89321 (19)	0.2337 (2)	0.0350 (6)
C12	0.8899 (3)	0.9768 (3)	0.2518 (4)	0.0563 (11)
H12A	0.8572	0.9584	0.3202	0.084*
H12B	0.8591	1.0302	0.2083	0.084*
H12C	0.9513	0.9968	0.2390	0.084*
C13	0.9275 (3)	0.8110 (3)	0.3138 (4)	0.0660 (13)
H13A	0.9809	0.8321	0.3191	0.099*
H13B	0.9434	0.7576	0.2984	0.099*
H13C	0.8807	0.7898	0.3761	0.099*
C14	0.9594 (3)	0.9145 (4)	0.1385 (3)	0.0546 (10)
H14A	0.9411	0.9720	0.0861	0.082*
H14B	0.9623	0.8599	0.1258	0.082*
H14C	1.0188	0.9256	0.1408	0.082*
C21	0.5993 (7)	0.4542 (8)	0.2344 (8)	0.039 (2)	0.478 (6)
H21	0.6100	0.4733	0.1636	0.047*	0.478 (6)
C22	0.5721 (9)	0.5440 (9)	0.2503 (9)	0.043 (3)	0.478 (6)
H22A	0.6208	0.5930	0.2106	0.052*	0.478 (6)
H22B	0.5170	0.5723	0.2291	0.052*	0.478 (6)
C23	0.5556 (8)	0.5153 (9)	0.3557 (8)	0.040 (3)	0.478 (6)
H23	0.5365	0.5724	0.3667	0.048*	0.478 (6)
C24	0.4816 (8)	0.4369 (13)	0.4176 (11)	0.058 (4)	0.478 (6)
H24A	0.4713	0.4174	0.4878	0.069*	0.478 (6)
H24B	0.4247	0.4633	0.3997	0.069*	0.478 (6)
C25	0.5073 (10)	0.3498 (14)	0.4016 (14)	0.051 (4)	0.478 (6)
H25	0.4575	0.3010	0.4413	0.061*	0.478 (6)
C26	0.5244 (8)	0.3782 (9)	0.2963 (9)	0.048 (3)	0.478 (6)
H26A	0.4687	0.4043	0.2755	0.058*	0.478 (6)
H26B	0.5419	0.3211	0.2861	0.058*	0.478 (6)
C27	0.6849 (4)	0.4095 (5)	0.2665 (5)	0.0317 (16)	0.478 (6)
H27A	0.7012	0.3522	0.2564	0.038*	0.478 (6)
H27B	0.7353	0.4564	0.2263	0.038*	0.478 (6)
C28	0.6432 (5)	0.4732 (4)	0.3876 (5)	0.0313 (15)	0.478 (6)
H28A	0.6334	0.4556	0.4573	0.038*	0.478 (6)
H28B	0.6924	0.5217	0.3476	0.038*	0.478 (6)
C29	0.5914 (5)	0.3088 (5)	0.4385 (5)	0.0400 (19)	0.478 (6)
H29A	0.5791	0.2968	0.5069	0.048*	0.478 (6)
H29B	0.6074	0.2471	0.4373	0.048*	0.478 (6)
C71	0.5983 (6)	0.5163 (6)	0.2487 (7)	0.0269 (18)	0.522 (6)
H71	0.6095	0.5797	0.1879	0.032*	0.522 (6)
C72	0.5314 (7)	0.5276 (7)	0.3325 (9)	0.039 (2)	0.522 (6)
H72A	0.4742	0.5527	0.3150	0.047*	0.522 (6)
H72B	0.5553	0.5745	0.3437	0.047*	0.522 (6)
C73	0.5140 (7)	0.4318 (8)	0.4256 (9)	0.036 (2)	0.522 (6)
H73	0.4695	0.4403	0.4799	0.044*	0.522 (6)
C74	0.4777 (8)	0.3601 (11)	0.4088 (10)	0.035 (2)	0.522 (6)
H74A	0.4194	0.3829	0.3930	0.042*	0.522 (6)
H74B	0.4669	0.2977	0.4694	0.042*	0.522 (6)
C75	0.5432 (6)	0.3465 (6)	0.3251 (7)	0.0300 (18)	0.522 (6)
H75	0.5176	0.3002	0.3137	0.036*	0.522 (6)
C76	0.5630 (6)	0.4443 (6)	0.2310 (6)	0.0320 (18)	0.522 (6)
H76A	0.6081	0.4357	0.1778	0.038*	0.522 (6)
H76B	0.5073	0.4689	0.2099	0.038*	0.522 (6)
C77	0.6876 (4)	0.4773 (4)	0.2784 (4)	0.0264 (13)	0.522 (6)
H77A	0.7323	0.4686	0.2251	0.032*	0.522 (6)
H77B	0.7126	0.5240	0.2890	0.032*	0.522 (6)
C78	0.6019 (4)	0.3898 (4)	0.4554 (4)	0.0285 (13)	0.522 (6)
H78A	0.6259	0.4325	0.4719	0.034*	0.522 (6)
H78B	0.5896	0.3258	0.5140	0.034*	0.522 (6)
C79	0.6331 (4)	0.3090 (4)	0.3509 (4)	0.0251 (13)	0.522 (6)
H79A	0.6772	0.3031	0.2956	0.030*	0.522 (6)
H79B	0.6239	0.2446	0.4092	0.030*	0.522 (6)
C30	0.66948 (18)	0.38107 (18)	0.3724 (2)	0.0220 (6)
N31	0.75959 (18)	0.33984 (18)	0.4026 (2)	0.0314 (6)
C32	0.8093 (11)	0.4132 (9)	0.4011 (14)	0.059 (4)	0.56 (2)
H32A	0.7686	0.4432	0.4381	0.089*	0.56 (2)
H32B	0.8336	0.4623	0.3332	0.089*	0.56 (2)
H32C	0.8588	0.3827	0.4311	0.089*	0.56 (2)
C33	0.8254 (6)	0.3119 (10)	0.3265 (9)	0.048 (2)	0.56 (2)
H33A	0.8862	0.3056	0.3344	0.072*	0.56 (2)
H33B	0.8253	0.3620	0.2601	0.072*	0.56 (2)
H33C	0.8060	0.2506	0.3371	0.072*	0.56 (2)
C34	0.7458 (7)	0.2551 (9)	0.5004 (8)	0.055 (3)	0.56 (2)
H34A	0.8022	0.2401	0.5195	0.082*	0.56 (2)
H34B	0.7269	0.2001	0.4985	0.082*	0.56 (2)
H34C	0.6993	0.2689	0.5482	0.082*	0.56 (2)
C35	0.8302 (13)	0.4179 (15)	0.3560 (15)	0.063 (5)	0.44 (2)
H35A	0.8072	0.4674	0.3761	0.095*	0.44 (2)
H35B	0.8444	0.4467	0.2845	0.095*	0.44 (2)
H35C	0.8847	0.3901	0.3772	0.095*	0.44 (2)
C36	0.7961 (11)	0.2632 (13)	0.3763 (16)	0.056 (5)	0.44 (2)
H36A	0.8506	0.2376	0.3984	0.084*	0.44 (2)
H36B	0.8109	0.2895	0.3051	0.084*	0.44 (2)
H36C	0.7512	0.2116	0.4081	0.084*	0.44 (2)
C37	0.7427 (9)	0.2967 (15)	0.5138 (9)	0.059 (4)	0.44 (2)
H37A	0.7061	0.2380	0.5471	0.089*	0.44 (2)
H37B	0.7109	0.3433	0.5350	0.089*	0.44 (2)
H37C	0.8004	0.2812	0.5304	0.089*	0.44 (2)
C41	0.4525 (6)	0.7055 (7)	0.8792 (7)	0.0484 (13)	0.33
H41	0.4227	0.7003	0.8352	0.058*	0.33
C42	0.4140 (7)	0.7906 (7)	0.8960 (7)	0.0477 (12)	0.33
H42A	0.3477	0.7839	0.9220	0.057*	0.33
H42B	0.4282	0.8509	0.8332	0.057*	0.33
C43	0.4547 (6)	0.7949 (7)	0.9698 (7)	0.0465 (12)	0.33
H43	0.4266	0.8481	0.9846	0.056*	0.33
C44	0.4428 (8)	0.7000 (6)	1.0647 (6)	0.0445 (11)	0.33
H44A	0.4740	0.7031	1.1080	0.053*	0.33
H44B	0.3781	0.6868	1.0997	0.053*	0.33
C45	0.4820 (6)	0.6220 (6)	1.0385 (7)	0.0409 (12)	0.33
H45	0.4739	0.5598	1.1007	0.049*	0.33
C46	0.4380 (7)	0.6119 (7)	0.9752 (7)	0.0472 (11)	0.33
H46A	0.3729	0.5990	1.0075	0.057*	0.33
H46B	0.4644	0.5577	0.9626	0.057*	0.33
C47	0.5541 (6)	0.7235 (8)	0.8288 (7)	0.0471 (14)	0.33
H47A	0.5638	0.7814	0.7639	0.057*	0.33
H47B	0.5811	0.6680	0.8189	0.057*	0.33
C48	0.5548 (6)	0.8180 (6)	0.9147 (7)	0.0410 (12)	0.33
H48A	0.5599	0.8764	0.8507	0.049*	0.33
H48B	0.5843	0.8322	0.9529	0.049*	0.33
C49	0.5830 (6)	0.6407 (7)	0.9909 (7)	0.0375 (14)	0.33
H49A	0.6095	0.5893	0.9737	0.045*	0.33
H49B	0.6119	0.6387	1.0385	0.045*	0.33
C81	0.4545 (8)	0.8011 (7)	0.8681 (8)	0.0484 (13)	0.33
H81	0.4229	0.8386	0.8157	0.058*	0.33
C82	0.4454 (7)	0.8517 (7)	0.9285 (7)	0.0477 (12)	0.33
H82A	0.3810	0.8619	0.9544	0.057*	0.33
H82B	0.4756	0.9154	0.8866	0.057*	0.33
C83	0.4876 (6)	0.7918 (6)	1.0137 (7)	0.0465 (12)	0.33
H83	0.4772	0.8224	1.0569	0.056*	0.33
C84	0.4529 (8)	0.6881 (6)	1.0731 (6)	0.0445 (11)	0.33
H84A	0.4864	0.6504	1.1229	0.053*	0.33
H84B	0.3885	0.6868	1.1078	0.053*	0.33
C85	0.4643 (6)	0.6431 (7)	1.0073 (7)	0.0409 (12)	0.33
H85	0.4392	0.5761	1.0477	0.049*	0.33
C86	0.4173 (6)	0.6985 (6)	0.9300 (7)	0.0472 (11)	0.33
H86A	0.3520	0.6994	0.9603	0.057*	0.33
H86B	0.4260	0.6676	0.8879	0.057*	0.33
C87	0.5558 (7)	0.7956 (8)	0.8208 (7)	0.0471 (14)	0.33
H87A	0.5638	0.7653	0.7784	0.057*	0.33
H87B	0.5820	0.8613	0.7796	0.057*	0.33
C88	0.5894 (6)	0.7882 (7)	0.9664 (7)	0.0410 (12)	0.33
H88A	0.6209	0.7508	1.0181	0.049*	0.33
H88B	0.6152	0.8541	0.9268	0.049*	0.33
C89	0.5657 (6)	0.6392 (6)	0.9620 (7)	0.0375 (14)	0.33
H89A	0.5965	0.6040	1.0147	0.045*	0.33
H89B	0.5763	0.6048	0.9230	0.045*	0.33
C91	0.4656 (6)	0.7295 (7)	1.0286 (8)	0.0484 (13)	0.33
H91	0.4423	0.7256	1.0949	0.058*	0.33
C92	0.4384 (7)	0.6395 (7)	1.0321 (6)	0.0477 (12)	0.33
H92A	0.3720	0.6325	1.0556	0.057*	0.33
H92B	0.4642	0.5826	1.0794	0.057*	0.33
C93	0.4708 (6)	0.6431 (7)	0.9310 (7)	0.0465 (12)	0.33
H93	0.4504	0.5842	0.9348	0.056*	0.33
C94	0.4305 (7)	0.7320 (6)	0.8618 (7)	0.0445 (11)	0.33
H94A	0.4504	0.7379	0.7952	0.053*	0.33
H94B	0.3641	0.7267	0.8841	0.053*	0.33
C95	0.4599 (7)	0.8194 (7)	0.8590 (7)	0.0409 (12)	0.33
H95	0.4356	0.8774	0.8101	0.049*	0.33
C96	0.4318 (8)	0.8218 (7)	0.9525 (7)	0.0472 (11)	0.33
H96A	0.3654	0.8249	0.9739	0.057*	0.33
H96B	0.4578	0.8791	0.9453	0.057*	0.33
C97	0.5695 (6)	0.7326 (8)	0.9977 (7)	0.0471 (14)	0.33
H97A	0.5911	0.7891	0.9962	0.057*	0.33
H97B	0.5930	0.6739	1.0456	0.057*	0.33
C98	0.5736 (6)	0.6506 (7)	0.8977 (8)	0.0410 (12)	0.33
H98A	0.5959	0.6571	0.8309	0.049*	0.33
H98B	0.5994	0.5917	0.9425	0.049*	0.33
C99	0.5638 (6)	0.8253 (7)	0.8236 (7)	0.0375 (14)	0.33
H99A	0.5846	0.8263	0.7592	0.045*	0.33
H99B	0.5848	0.8853	0.8158	0.045*	0.33
C50	0.6026 (2)	0.7388 (2)	0.8981 (2)	0.0272 (6)
N51	0.7076 (2)	0.7443 (2)	0.8543 (2)	0.0433 (7)
C52	0.7318 (8)	0.8409 (8)	0.7578 (9)	0.075 (2)	0.455 (6)
H52A	0.7966	0.8534	0.7381	0.112*	0.455 (6)
H52B	0.6987	0.8932	0.7684	0.112*	0.455 (6)
H52C	0.7154	0.8369	0.7060	0.112*	0.455 (6)
C53	0.739 (6)	0.682 (5)	0.808 (4)	0.116 (9)	0.455 (6)
H53A	0.6975	0.6867	0.7709	0.174*	0.455 (6)
H53B	0.7409	0.6156	0.8585	0.174*	0.455 (6)
H53C	0.7992	0.7030	0.7633	0.174*	0.455 (6)
C54	0.7569 (6)	0.7487 (9)	0.9125 (8)	0.0607 (18)	0.455 (6)
H54A	0.7588	0.6846	0.9675	0.091*	0.455 (6)
H54B	0.7278	0.7933	0.9376	0.091*	0.455 (6)
H54C	0.8184	0.7713	0.8726	0.091*	0.455 (6)
C55	0.7488 (6)	0.8380 (7)	0.8260 (7)	0.075 (2)	0.545 (6)
H55A	0.8143	0.8317	0.8130	0.112*	0.545 (6)
H55B	0.7253	0.8542	0.8796	0.112*	0.545 (6)
H55C	0.7336	0.8889	0.7669	0.112*	0.545 (6)
C56	0.740 (5)	0.712 (4)	0.779 (3)	0.116 (9)	0.545 (6)
H56A	0.8051	0.7039	0.7666	0.174*	0.545 (6)
H56B	0.7250	0.7604	0.7190	0.174*	0.545 (6)
H56C	0.7107	0.6509	0.8030	0.174*	0.545 (6)
C57	0.7550 (5)	0.6742 (8)	0.9353 (6)	0.0607 (18)	0.545 (6)
H57A	0.7380	0.6078	0.9586	0.091*	0.545 (6)
H57B	0.7363	0.6889	0.9902	0.091*	0.545 (6)
H57C	0.8204	0.6821	0.9080	0.091*	0.545 (6)
Si1	0.83438 (4)	0.00022 (4)	0.49345 (5)	0.01540 (16)
Si2	0.98908 (4)	0.12550 (4)	0.31355 (5)	0.01513 (16)
Si3	1.04679 (4)	0.18139 (4)	0.45071 (5)	0.01549 (16)
Si4	0.88821 (4)	0.05645 (4)	0.63026 (5)	0.01530 (16)
O1	0.82257 (12)	0.09004 (13)	0.70369 (13)	0.0211 (4)
O2	0.83201 (13)	0.02394 (14)	0.57970 (14)	0.0237 (4)
O3	0.87266 (13)	−0.10566 (12)	0.51595 (14)	0.0218 (4)
O4	0.73191 (12)	0.00175 (14)	0.48772 (14)	0.0224 (4)
H4	0.6978	0.0243	0.5231	0.027*
O5	0.89129 (12)	0.07994 (13)	0.38886 (13)	0.0218 (4)
O6	1.05351 (13)	0.03611 (12)	0.31381 (13)	0.0210 (4)
O7	0.97992 (13)	0.19821 (12)	0.20719 (13)	0.0210 (4)
O8	1.02992 (13)	0.17834 (12)	0.35807 (13)	0.0209 (4)
O9	1.07315 (13)	0.28655 (12)	0.42231 (13)	0.0212 (4)
O10	0.95671 (13)	0.14254 (13)	0.54122 (13)	0.0228 (4)
O21	0.15723 (14)	0.74214 (12)	0.30518 (15)	0.0299 (4)
H21D	0.1618	0.7972	0.2985	0.036*
H21E	0.1150	0.7128	0.3553	0.036*
O22	0.06433 (15)	0.42982 (12)	0.24943 (15)	0.0315 (5)
H22D	0.0638	0.3893	0.3073	0.038*
H22E	0.0357	0.4781	0.2505	0.038*
O23	0.02431 (15)	0.63275 (14)	0.47239 (15)	0.0294 (4)
H23D	−0.0059	0.6602	0.5046	0.035*
H23E	0.0395	0.5788	0.5120	0.035*
O24	0.00855 (18)	0.38233 (14)	0.13337 (16)	0.0370 (5)
H24D	0.0040	0.3223	0.1589	0.044*
H24E	0.0209	0.3952	0.1730	0.044*
O25	0.07021 (17)	0.17180 (16)	0.05214 (15)	0.0357 (5)
H25D	0.0436	0.1776	0.1024	0.043*
H25E	0.1119	0.1322	0.0653	0.043*
O26	0.82267 (15)	0.22182 (16)	0.15971 (16)	0.0341 (5)
H26D	0.8633	0.2086	0.1883	0.041*
H26E	0.8444	0.2171	0.1081	0.041*
O27	0.86336 (17)	0.65388 (16)	0.11203 (16)	0.0385 (5)
H27D	0.8653	0.6108	0.0959	0.046*
H27E	0.8813	0.7056	0.0607	0.046*
O28	0.88650 (18)	0.51510 (16)	0.05309 (17)	0.0421 (6)
H28D	0.9152	0.5443	−0.0062	0.050*
H28E	0.9201	0.4728	0.0834	0.050*
O29	0.39883 (16)	0.93926 (19)	0.4037 (2)	0.0441 (6)
H29D	0.3948	0.9403	0.3528	0.053*
H29E	0.4385	0.9794	0.3871	0.053*
O30	0.2052 (2)	0.5585 (2)	0.1336 (2)	0.0524 (7)
H30D	0.2172	0.5430	0.0889	0.063*
H30E	0.1870	0.6154	0.1114	0.063*
O31	0.35432 (17)	0.9228 (2)	0.2638 (2)	0.0499 (6)
H31D	0.3573	0.8660	0.2727	0.060*
H31E	0.2998	0.9377	0.2748	0.060*
O32	0.35441 (17)	0.17892 (18)	0.42222 (19)	0.0433 (6)
H32D	0.3197	0.2239	0.4232	0.052*
H32E	0.3251	0.1271	0.4586	0.052*
O33	0.23910 (19)	0.32786 (18)	0.4150 (2)	0.0552 (8)
H33D	0.2111	0.3433	0.4586	0.066*
H33E	0.2013	0.3082	0.4005	0.066*
O34	0.31854 (18)	0.49364 (19)	0.2500 (2)	0.0556 (7)
H34D	0.2820	0.5194	0.2157	0.067*
H34E	0.2927	0.4461	0.3020	0.067*
O35	0.30247 (19)	0.6179 (2)	0.3288 (2)	0.0527 (7)
H35D	0.2595	0.6566	0.3230	0.063*
H35E	0.3087	0.5976	0.2883	0.063*
O36	0.9736 (2)	0.60024 (18)	0.2322 (2)	0.0564 (8)
H36D	1.0249	0.6228	0.1954	0.068*
H36E	0.9373	0.6210	0.1975	0.068*
O37	0.50648 (17)	1.0682 (2)	0.40103 (19)	0.0477 (6)
H37D	0.5090	1.0887	0.4392	0.057*
H37E	0.5561	1.0803	0.3582	0.057*
O38	0.1842 (2)	0.0105 (2)	0.10472 (18)	0.0600 (8)
H38D	0.2207	0.0517	0.0930	0.072*
H38E	0.1663	−0.0235	0.1658	0.072*
O39	0.68527 (17)	0.10889 (17)	0.31493 (19)	0.0557 (8)
H39D	0.7037	0.0820	0.3655	0.067*
H39E	0.7261	0.1461	0.2684	0.067*
O40	0.9194 (2)	0.55104 (16)	0.4210 (2)	0.0628 (9)
H40D	0.9500	0.5736	0.4406	0.075*
H40E	0.9356	0.5793	0.3595	0.075*
O41	0.76331 (18)	0.40699 (19)	0.05717 (17)	0.0501 (6)
H41D	0.8004	0.4413	0.0561	0.060*
H41E	0.7671	0.3505	0.1008	0.060*
O42	0.7486 (2)	0.5623 (2)	0.5015 (2)	0.0617 (8)
H42D	0.8034	0.5619	0.4730	0.074*
H42E	0.7352	0.5079	0.5506	0.074*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0348 (18)	0.0318 (16)	0.0362 (16)	−0.0002 (13)	−0.0165 (14)	−0.0082 (13)
C2	0.0323 (19)	0.0378 (18)	0.056 (2)	0.0059 (14)	−0.0100 (16)	−0.0185 (17)
C3	0.044 (2)	0.0403 (19)	0.0360 (18)	−0.0017 (15)	0.0053 (15)	−0.0129 (15)
C4	0.048 (2)	0.0364 (19)	0.046 (2)	−0.0110 (16)	0.0015 (17)	−0.0064 (16)
C5	0.043 (2)	0.0280 (16)	0.054 (2)	−0.0104 (14)	−0.0014 (16)	−0.0204 (15)
C6	0.035 (2)	0.052 (2)	0.050 (2)	−0.0135 (15)	−0.0097 (15)	−0.0268 (17)
C7	0.0339 (17)	0.0225 (14)	0.0258 (14)	−0.0030 (11)	−0.0115 (12)	−0.0055 (11)
C8	0.059 (2)	0.0323 (17)	0.0253 (15)	0.0110 (15)	−0.0124 (15)	−0.0118 (13)
C9	0.0398 (18)	0.0220 (14)	0.0387 (17)	0.0035 (12)	−0.0094 (14)	−0.0143 (13)
C10	0.0334 (16)	0.0201 (13)	0.0268 (14)	0.0051 (11)	−0.0121 (12)	−0.0104 (11)
N11	0.0413 (16)	0.0302 (13)	0.0471 (16)	0.0124 (11)	−0.0271 (13)	−0.0229 (12)
C12	0.062 (3)	0.047 (2)	0.090 (3)	0.0107 (18)	−0.043 (2)	−0.046 (2)
C13	0.067 (3)	0.061 (3)	0.073 (3)	0.023 (2)	−0.051 (3)	−0.021 (2)
C14	0.033 (2)	0.076 (3)	0.062 (2)	−0.0116 (18)	−0.0085 (17)	−0.038 (2)
C21	0.029 (6)	0.050 (6)	0.030 (4)	0.001 (5)	−0.014 (4)	−0.009 (4)
C22	0.050 (7)	0.041 (7)	0.038 (5)	0.022 (4)	−0.018 (5)	−0.020 (5)
C23	0.047 (7)	0.039 (5)	0.036 (5)	0.028 (5)	−0.026 (4)	−0.017 (4)
C24	0.021 (7)	0.100 (9)	0.033 (5)	−0.002 (6)	−0.003 (5)	−0.019 (5)
C25	0.031 (8)	0.051 (6)	0.048 (6)	−0.007 (6)	−0.002 (6)	−0.008 (4)
C26	0.043 (6)	0.051 (8)	0.050 (8)	−0.003 (5)	−0.024 (5)	−0.017 (6)
C27	0.022 (3)	0.034 (4)	0.037 (3)	0.000 (2)	−0.005 (3)	−0.017 (3)
C28	0.033 (4)	0.025 (3)	0.039 (4)	0.010 (2)	−0.018 (3)	−0.014 (3)
C29	0.035 (4)	0.029 (3)	0.039 (4)	−0.014 (3)	−0.016 (3)	0.004 (3)
C71	0.023 (5)	0.018 (4)	0.032 (3)	0.001 (3)	−0.006 (3)	−0.007 (3)
C72	0.031 (5)	0.030 (4)	0.053 (7)	0.015 (3)	−0.025 (4)	−0.012 (4)
C73	0.026 (6)	0.051 (5)	0.039 (4)	0.001 (4)	−0.010 (4)	−0.026 (4)
C74	0.021 (6)	0.044 (5)	0.032 (4)	−0.003 (5)	0.000 (4)	−0.014 (3)
C75	0.031 (5)	0.026 (4)	0.029 (5)	−0.011 (3)	−0.010 (3)	−0.006 (3)
C76	0.029 (5)	0.031 (4)	0.025 (3)	−0.003 (4)	−0.013 (4)	−0.001 (3)
C77	0.018 (3)	0.021 (3)	0.033 (3)	−0.0038 (19)	−0.007 (2)	−0.006 (2)
C78	0.031 (3)	0.030 (3)	0.025 (3)	0.006 (2)	−0.011 (2)	−0.013 (2)
C79	0.029 (3)	0.019 (2)	0.032 (3)	−0.001 (2)	−0.013 (2)	−0.013 (2)
C30	0.0198 (14)	0.0158 (12)	0.0303 (14)	0.0022 (10)	−0.0132 (11)	−0.0076 (11)
N31	0.0281 (14)	0.0247 (12)	0.0514 (16)	0.0093 (10)	−0.0250 (12)	−0.0196 (12)
C32	0.051 (8)	0.039 (5)	0.100 (11)	0.004 (4)	−0.051 (8)	−0.026 (7)
C33	0.034 (4)	0.042 (6)	0.074 (6)	0.014 (4)	−0.020 (4)	−0.032 (5)
C34	0.051 (5)	0.049 (6)	0.055 (5)	0.013 (4)	−0.037 (4)	−0.007 (4)
C35	0.030 (8)	0.076 (9)	0.083 (11)	−0.010 (6)	−0.034 (8)	−0.024 (9)
C36	0.052 (8)	0.051 (8)	0.110 (13)	0.039 (7)	−0.058 (9)	−0.061 (9)
C37	0.063 (7)	0.068 (10)	0.055 (6)	0.034 (7)	−0.042 (5)	−0.028 (6)
C41	0.040 (3)	0.054 (3)	0.046 (3)	−0.006 (2)	−0.017 (2)	−0.015 (2)
C42	0.043 (3)	0.044 (2)	0.041 (2)	−0.004 (2)	−0.011 (2)	−0.007 (2)
C43	0.046 (3)	0.038 (2)	0.053 (3)	0.009 (2)	−0.020 (2)	−0.017 (2)
C44	0.045 (2)	0.038 (2)	0.039 (2)	0.0010 (18)	−0.0106 (18)	−0.0098 (17)
C45	0.034 (3)	0.036 (2)	0.042 (3)	−0.001 (2)	−0.010 (2)	−0.010 (2)
C46	0.038 (3)	0.051 (2)	0.051 (3)	0.004 (2)	−0.015 (2)	−0.022 (2)
C47	0.040 (2)	0.065 (4)	0.044 (3)	−0.005 (2)	−0.016 (2)	−0.027 (3)
C48	0.044 (2)	0.036 (3)	0.052 (3)	−0.0015 (19)	−0.0196 (19)	−0.024 (2)
C49	0.036 (2)	0.032 (2)	0.030 (3)	0.0027 (19)	−0.0122 (19)	−0.002 (2)
C81	0.040 (3)	0.054 (3)	0.046 (3)	−0.006 (2)	−0.017 (2)	−0.015 (2)
C82	0.043 (3)	0.044 (2)	0.041 (2)	−0.004 (2)	−0.011 (2)	−0.007 (2)
C83	0.046 (3)	0.038 (2)	0.053 (3)	0.009 (2)	−0.020 (2)	−0.017 (2)
C84	0.045 (2)	0.038 (2)	0.039 (2)	0.0010 (18)	−0.0106 (18)	−0.0098 (17)
C85	0.034 (3)	0.036 (2)	0.042 (3)	−0.001 (2)	−0.010 (2)	−0.010 (2)
C86	0.038 (3)	0.051 (2)	0.051 (3)	0.004 (2)	−0.015 (2)	−0.022 (2)
C87	0.040 (2)	0.065 (4)	0.044 (3)	−0.005 (2)	−0.016 (2)	−0.027 (3)
C88	0.044 (2)	0.036 (3)	0.052 (3)	−0.0015 (19)	−0.0196 (19)	−0.024 (2)
C89	0.036 (2)	0.032 (2)	0.030 (3)	0.0027 (19)	−0.0122 (19)	−0.002 (2)
C91	0.040 (3)	0.054 (3)	0.046 (3)	−0.006 (2)	−0.017 (2)	−0.015 (2)
C92	0.043 (3)	0.044 (2)	0.041 (2)	−0.004 (2)	−0.011 (2)	−0.007 (2)
C93	0.046 (3)	0.038 (2)	0.053 (3)	0.009 (2)	−0.020 (2)	−0.017 (2)
C94	0.045 (2)	0.038 (2)	0.039 (2)	0.0010 (18)	−0.0106 (18)	−0.0098 (17)
C95	0.034 (3)	0.036 (2)	0.042 (3)	−0.001 (2)	−0.010 (2)	−0.010 (2)
C96	0.038 (3)	0.051 (2)	0.051 (3)	0.004 (2)	−0.015 (2)	−0.022 (2)
C97	0.040 (2)	0.065 (4)	0.044 (3)	−0.005 (2)	−0.016 (2)	−0.027 (3)
C98	0.044 (2)	0.036 (3)	0.052 (3)	−0.0015 (19)	−0.0196 (19)	−0.024 (2)
C99	0.036 (2)	0.032 (2)	0.030 (3)	0.0027 (19)	−0.0122 (19)	−0.002 (2)
C50	0.0272 (16)	0.0206 (13)	0.0263 (14)	−0.0019 (11)	−0.0078 (11)	−0.0045 (11)
N51	0.0278 (16)	0.0516 (18)	0.0387 (15)	−0.0125 (12)	−0.0027 (12)	−0.0127 (13)
C52	0.056 (4)	0.061 (4)	0.074 (5)	−0.036 (3)	−0.002 (4)	−0.006 (4)
C53	0.063 (4)	0.21 (3)	0.11 (2)	0.041 (19)	−0.013 (18)	−0.118 (19)
C54	0.035 (3)	0.093 (5)	0.055 (4)	0.002 (4)	−0.024 (3)	−0.029 (4)
C55	0.056 (4)	0.061 (4)	0.074 (5)	−0.036 (3)	−0.002 (4)	−0.006 (4)
C56	0.063 (4)	0.21 (3)	0.11 (2)	0.041 (19)	−0.013 (18)	−0.118 (19)
C57	0.035 (3)	0.093 (5)	0.055 (4)	0.002 (4)	−0.024 (3)	−0.029 (4)
Si1	0.0135 (3)	0.0129 (3)	0.0186 (3)	−0.0009 (2)	−0.0067 (2)	−0.0050 (3)
Si2	0.0170 (4)	0.0101 (3)	0.0164 (3)	−0.0008 (2)	−0.0077 (3)	−0.0029 (2)
Si3	0.0182 (4)	0.0089 (3)	0.0178 (3)	−0.0023 (2)	−0.0071 (3)	−0.0032 (2)
Si4	0.0151 (3)	0.0125 (3)	0.0175 (3)	−0.0001 (2)	−0.0056 (2)	−0.0057 (3)
O1	0.0208 (10)	0.0205 (9)	0.0222 (9)	0.0025 (7)	−0.0067 (7)	−0.0102 (7)
O2	0.0200 (10)	0.0274 (10)	0.0288 (10)	0.0000 (7)	−0.0096 (8)	−0.0153 (8)
O3	0.0218 (10)	0.0138 (8)	0.0296 (10)	0.0004 (7)	−0.0129 (8)	−0.0068 (7)
O4	0.0161 (9)	0.0267 (10)	0.0261 (9)	−0.0008 (7)	−0.0086 (7)	−0.0118 (8)
O5	0.0190 (10)	0.0175 (9)	0.0226 (9)	−0.0033 (7)	−0.0064 (7)	−0.0035 (7)
O6	0.0238 (10)	0.0147 (8)	0.0243 (9)	0.0036 (7)	−0.0110 (7)	−0.0075 (7)
O7	0.0270 (10)	0.0147 (8)	0.0192 (9)	−0.0004 (7)	−0.0110 (7)	−0.0036 (7)
O8	0.0258 (10)	0.0156 (8)	0.0214 (9)	−0.0033 (7)	−0.0094 (7)	−0.0063 (7)
O9	0.0286 (10)	0.0109 (8)	0.0250 (9)	−0.0037 (7)	−0.0109 (8)	−0.0061 (7)
O10	0.0252 (10)	0.0156 (8)	0.0232 (9)	−0.0034 (7)	−0.0033 (7)	−0.0068 (7)
O21	0.0327 (12)	0.0231 (10)	0.0355 (11)	0.0009 (8)	−0.0074 (9)	−0.0163 (9)
O22	0.0427 (13)	0.0149 (9)	0.0315 (11)	−0.0020 (8)	−0.0184 (9)	−0.0016 (8)
O23	0.0371 (12)	0.0172 (9)	0.0351 (11)	0.0000 (8)	−0.0117 (9)	−0.0120 (8)
O24	0.0686 (16)	0.0134 (9)	0.0278 (11)	−0.0035 (9)	−0.0201 (11)	−0.0039 (8)
O25	0.0517 (15)	0.0285 (11)	0.0254 (10)	0.0047 (9)	−0.0138 (10)	−0.0109 (9)
O26	0.0323 (12)	0.0369 (12)	0.0324 (11)	0.0007 (9)	−0.0176 (9)	−0.0108 (10)
O27	0.0511 (15)	0.0284 (11)	0.0298 (11)	0.0020 (10)	−0.0088 (10)	−0.0108 (9)
O28	0.0603 (16)	0.0232 (11)	0.0328 (12)	0.0004 (10)	−0.0111 (11)	−0.0067 (9)
O29	0.0279 (13)	0.0510 (15)	0.0572 (15)	0.0001 (10)	−0.0128 (11)	−0.0276 (13)
O30	0.0531 (17)	0.0415 (14)	0.0577 (16)	−0.0053 (12)	−0.0209 (14)	−0.0148 (12)
O31	0.0249 (13)	0.0701 (18)	0.0535 (15)	0.0013 (11)	−0.0088 (11)	−0.0293 (15)
O32	0.0348 (13)	0.0381 (13)	0.0508 (14)	−0.0139 (10)	−0.0054 (11)	−0.0163 (12)
O33	0.0579 (18)	0.0279 (12)	0.077 (2)	−0.0122 (11)	−0.0455 (16)	−0.0045 (12)
O34	0.0402 (15)	0.0357 (14)	0.0720 (19)	−0.0039 (11)	−0.0193 (13)	−0.0078 (13)
O35	0.0388 (15)	0.0450 (15)	0.0634 (18)	0.0138 (11)	−0.0154 (13)	−0.0199 (13)
O36	0.0665 (19)	0.0266 (12)	0.088 (2)	0.0100 (12)	−0.0523 (17)	−0.0205 (13)
O37	0.0336 (14)	0.0601 (17)	0.0403 (13)	−0.0052 (11)	−0.0109 (10)	−0.0148 (12)
O38	0.087 (2)	0.0511 (17)	0.0248 (12)	0.0139 (15)	−0.0156 (13)	−0.0076 (11)
O39	0.0342 (14)	0.0729 (19)	0.0391 (13)	−0.0136 (12)	−0.0154 (11)	−0.0042 (13)
O40	0.090 (2)	0.0280 (12)	0.088 (2)	−0.0029 (13)	−0.067 (2)	−0.0154 (13)
O41	0.0416 (15)	0.0417 (14)	0.0559 (16)	−0.0056 (11)	−0.0142 (12)	−0.0126 (12)
O42	0.064 (2)	0.0496 (16)	0.0714 (19)	−0.0003 (14)	−0.0262 (16)	−0.0234 (15)

Geometric parameters (Å, º)

C1—C2	1.522 (5)	C49—H49A	0.9900
C1—C6	1.529 (5)	C49—H49B	0.9900
C1—C7	1.532 (4)	C81—C82	1.511 (9)
C1—H1	1.0000	C81—C86	1.526 (9)
C2—C3	1.537 (5)	C81—C87	1.545 (9)
C2—H2A	0.9900	C81—H81	1.0000
C2—H2B	0.9900	C82—C83	1.531 (9)
C3—C4	1.524 (5)	C82—H82A	0.9900
C3—C8	1.527 (5)	C82—H82B	0.9900
C3—H3	1.0000	C83—C84	1.527 (8)
C4—C5	1.520 (5)	C83—C88	1.548 (9)
C4—H4A	0.9900	C83—H83	1.0000
C4—H4B	0.9900	C84—C85	1.511 (8)
C5—C6	1.493 (5)	C84—H84A	0.9900
C5—C9	1.546 (5)	C84—H84B	0.9900
C5—H5	1.0000	C85—C86	1.478 (9)
C6—H6A	0.9900	C85—C89	1.538 (8)
C6—H6B	0.9900	C85—H85	1.0000
C7—C10	1.532 (4)	C86—H86A	0.9900
C7—H7A	0.9900	C86—H86B	0.9900
C7—H7B	0.9900	C87—C50	1.480 (11)
C8—C10	1.541 (4)	C87—H87A	0.9900
C8—H8A	0.9900	C87—H87B	0.9900
C8—H8B	0.9900	C88—C50	1.599 (9)
C9—C10	1.525 (4)	C88—H88A	0.9900
C9—H9A	0.9900	C88—H88B	0.9900
C9—H9B	0.9900	C89—C50	1.487 (9)
C10—N11	1.578 (4)	C89—H89A	0.9900
N11—C14	1.482 (5)	C89—H89B	0.9900
N11—C12	1.490 (4)	C91—C92	1.519 (9)
N11—C13	1.504 (4)	C91—C96	1.541 (9)
C12—H12A	0.9800	C91—C97	1.546 (9)
C12—H12B	0.9800	C91—H91	1.0000
C12—H12C	0.9800	C92—C93	1.539 (9)
C13—H13A	0.9800	C92—H92A	0.9900
C13—H13B	0.9800	C92—H92B	0.9900
C13—H13C	0.9800	C93—C94	1.515 (8)
C14—H14A	0.9800	C93—C98	1.531 (9)
C14—H14B	0.9800	C93—H93	1.0000
C14—H14C	0.9800	C94—C95	1.500 (8)
C21—C26	1.529 (17)	C94—H94A	0.9900
C21—C27	1.534 (11)	C94—H94B	0.9900
C21—C22	1.555 (15)	C95—C96	1.465 (9)
C21—H21	1.0000	C95—C99	1.546 (8)
C22—C23	1.484 (17)	C95—H95	1.0000
C22—H22A	0.9900	C96—H96A	0.9900
C22—H22B	0.9900	C96—H96B	0.9900
C23—C24	1.54 (2)	C97—C50	1.499 (10)
C23—C28	1.556 (12)	C97—H97A	0.9900
C23—H23	1.0000	C97—H97B	0.9900
C24—C25	1.51 (3)	C98—C50	1.537 (9)
C24—H24A	0.9900	C98—H98A	0.9900
C24—H24B	0.9900	C98—H98B	0.9900
C25—C26	1.48 (2)	C99—C50	1.523 (9)
C25—C29	1.535 (16)	C99—H99A	0.9900
C25—H25	1.0000	C99—H99B	0.9900
C26—H26A	0.9900	C50—N51	1.572 (4)
C26—H26B	0.9900	N51—C54	1.416 (10)
C27—C30	1.497 (7)	N51—C53	1.47 (9)
C27—H27A	0.9900	N51—C56	1.47 (7)
C27—H27B	0.9900	N51—C55	1.506 (9)
C28—C30	1.584 (7)	N51—C52	1.556 (10)
C28—H28A	0.9900	N51—C57	1.566 (8)
C28—H28B	0.9900	C52—H52A	0.9800
C29—C30	1.535 (7)	C52—H52B	0.9800
C29—H29A	0.9900	C52—H52C	0.9800
C29—H29B	0.9900	C53—H53A	0.9800
C71—C76	1.514 (12)	C53—H53B	0.9800
C71—C72	1.517 (15)	C53—H53C	0.9800
C71—C77	1.559 (10)	C54—H54A	0.9800
C71—H71	1.0000	C54—H54B	0.9800
C72—C73	1.519 (17)	C54—H54C	0.9800
C72—H72A	0.9900	C55—H55A	0.9800
C72—H72B	0.9900	C55—H55B	0.9800
C73—C74	1.507 (19)	C55—H55C	0.9800
C73—C78	1.546 (10)	C56—H56A	0.9800
C73—H73	1.0000	C56—H56B	0.9800
C74—C75	1.525 (16)	C56—H56C	0.9800
C74—H74A	0.9900	C57—H57A	0.9800
C74—H74B	0.9900	C57—H57B	0.9800
C75—C79	1.541 (10)	C57—H57C	0.9800
C75—C76	1.544 (11)	Si1—O2	1.607 (2)
C75—H75	1.0000	Si1—O5	1.6079 (18)
C76—H76A	0.9900	Si1—O3	1.6092 (18)
C76—H76B	0.9900	Si1—O4	1.6239 (18)
C77—C30	1.529 (6)	Si2—O7	1.5801 (18)
C77—H77A	0.9900	Si2—O6	1.6252 (18)
C77—H77B	0.9900	Si2—O8	1.6284 (18)
C78—C30	1.494 (6)	Si2—O5	1.6322 (19)
C78—H78A	0.9900	Si3—O9	1.5845 (17)
C78—H78B	0.9900	Si3—O10	1.6203 (19)
C79—C30	1.566 (5)	Si3—O8	1.6258 (19)
C79—H79A	0.9900	Si3—O3^i	1.6377 (18)
C79—H79B	0.9900	Si4—O1	1.5783 (19)
C30—N31	1.578 (3)	Si4—O6^i	1.6273 (18)
N31—C36	1.471 (9)	Si4—O10	1.6290 (18)
N31—C34	1.475 (9)	Si4—O2	1.6369 (19)
N31—C32	1.476 (13)	O3—Si3^i	1.6377 (18)
N31—C35	1.513 (18)	O4—H4	0.8400
N31—C37	1.535 (12)	O6—Si4^i	1.6274 (18)
N31—C33	1.556 (9)	O21—H21D	0.8401
C32—H32A	0.9800	O21—H21E	0.8400
C32—H32B	0.9800	O22—H22D	0.8400
C32—H32C	0.9800	O22—H22E	0.8400
C33—H33A	0.9800	O23—H23D	0.8400
C33—H33B	0.9800	O23—H23E	0.8400
C33—H33C	0.9800	O24—H24D	0.8400
C34—H34A	0.9800	O24—H24E	0.8400
C34—H34B	0.9800	O25—H25D	0.8400
C34—H34C	0.9800	O25—H25E	0.8400
C35—H35A	0.9800	O26—H26D	0.8400
C35—H35B	0.9800	O26—H26E	0.8401
C35—H35C	0.9800	O27—H27D	0.8399
C36—H36A	0.9800	O27—H27E	0.8401
C36—H36B	0.9800	O28—H28D	0.8400
C36—H36C	0.9800	O28—H28E	0.8399
C37—H37A	0.9800	O29—H29D	0.8400
C37—H37B	0.9800	O29—H29E	0.8400
C37—H37C	0.9800	O30—H30D	0.8399
C41—C42	1.521 (9)	O30—H30E	0.8400
C41—C46	1.523 (9)	O31—H31D	0.8400
C41—C47	1.542 (9)	O31—H31E	0.8401
C41—H41	1.0000	O32—H32D	0.8400
C42—C43	1.546 (9)	O32—H32E	0.8400
C42—H42A	0.9900	O33—H33D	0.8400
C42—H42B	0.9900	O33—H33E	0.8399
C43—C44	1.526 (8)	O34—H34D	0.8400
C43—C48	1.540 (9)	O34—H34E	0.8400
C43—H43	1.0000	O35—H35D	0.8400
C44—C45	1.500 (8)	O35—H35E	0.8400
C44—H44A	0.9900	O36—H36D	0.8399
C44—H44B	0.9900	O36—H36E	0.8400
C45—C46	1.471 (9)	O37—H37D	0.8399
C45—C49	1.529 (8)	O37—H37E	0.8399
C45—H45	1.0000	O38—H38D	0.8400
C46—H46A	0.9900	O38—H38E	0.8400
C46—H46B	0.9900	O39—H39D	0.8400
C47—C50	1.650 (9)	O39—H39E	0.8400
C47—H47A	0.9900	O40—H40D	0.8400
C47—H47B	0.9900	O40—H40E	0.8400
C48—C50	1.474 (9)	O41—H41D	0.8400
C48—H48A	0.9900	O41—H41E	0.8400
C48—H48B	0.9900	O42—H42D	0.8400
C49—C50	1.538 (9)	O42—H42E	0.8400
C2—C1—C6	110.0 (3)	C43—C44—H44B	110.1
C2—C1—C7	109.7 (3)	H44A—C44—H44B	108.4
C6—C1—C7	109.3 (3)	C46—C45—C44	113.3 (8)
C2—C1—H1	109.3	C46—C45—C49	111.2 (7)
C6—C1—H1	109.3	C44—C45—C49	108.8 (7)
C7—C1—H1	109.3	C46—C45—H45	107.8
C1—C2—C3	108.9 (3)	C44—C45—H45	107.8
C1—C2—H2A	109.9	C49—C45—H45	107.8
C3—C2—H2A	109.9	C45—C46—C41	107.9 (7)
C1—C2—H2B	109.9	C45—C46—H46A	110.1
C3—C2—H2B	109.9	C41—C46—H46A	110.1
H2A—C2—H2B	108.3	C45—C46—H46B	110.1
C4—C3—C8	110.4 (3)	C41—C46—H46B	110.1
C4—C3—C2	109.5 (3)	H46A—C46—H46B	108.4
C8—C3—C2	108.8 (3)	C41—C47—C50	109.3 (6)
C4—C3—H3	109.4	C41—C47—H47A	109.8
C8—C3—H3	109.4	C50—C47—H47A	109.8
C2—C3—H3	109.4	C41—C47—H47B	109.8
C5—C4—C3	109.2 (3)	C50—C47—H47B	109.8
C5—C4—H4A	109.8	H47A—C47—H47B	108.3
C3—C4—H4A	109.8	C50—C48—C43	112.8 (6)
C5—C4—H4B	109.8	C50—C48—H48A	109.0
C3—C4—H4B	109.8	C43—C48—H48A	109.0
H4A—C4—H4B	108.3	C50—C48—H48B	109.0
C6—C5—C4	110.7 (3)	C43—C48—H48B	109.0
C6—C5—C9	109.9 (3)	H48A—C48—H48B	107.8
C4—C5—C9	108.8 (3)	C45—C49—C50	111.7 (6)
C6—C5—H5	109.1	C45—C49—H49A	109.3
C4—C5—H5	109.1	C50—C49—H49A	109.3
C9—C5—H5	109.1	C45—C49—H49B	109.3
C5—C6—C1	109.6 (3)	C50—C49—H49B	109.3
C5—C6—H6A	109.7	H49A—C49—H49B	107.9
C1—C6—H6A	109.7	C82—C81—C86	112.5 (8)
C5—C6—H6B	109.7	C82—C81—C87	107.8 (8)
C1—C6—H6B	109.7	C86—C81—C87	107.6 (8)
H6A—C6—H6B	108.2	C82—C81—H81	109.6
C10—C7—C1	109.0 (2)	C86—C81—H81	109.6
C10—C7—H7A	109.9	C87—C81—H81	109.6
C1—C7—H7A	109.9	C81—C82—C83	110.4 (7)
C10—C7—H7B	109.9	C81—C82—H82A	109.6
C1—C7—H7B	109.9	C83—C82—H82A	109.6
H7A—C7—H7B	108.3	C81—C82—H82B	109.6
C3—C8—C10	109.3 (3)	C83—C82—H82B	109.6
C3—C8—H8A	109.8	H82A—C82—H82B	108.1
C10—C8—H8A	109.8	C84—C83—C82	112.2 (7)
C3—C8—H8B	109.8	C84—C83—C88	106.8 (7)
C10—C8—H8B	109.8	C82—C83—C88	105.9 (7)
H8A—C8—H8B	108.3	C84—C83—H83	110.6
C10—C9—C5	109.1 (3)	C82—C83—H83	110.6
C10—C9—H9A	109.9	C88—C83—H83	110.6
C5—C9—H9A	109.9	C85—C84—C83	110.8 (7)
C10—C9—H9B	109.9	C85—C84—H84A	109.5
C5—C9—H9B	109.9	C83—C84—H84A	109.5
H9A—C9—H9B	108.3	C85—C84—H84B	109.5
C9—C10—C7	109.9 (2)	C83—C84—H84B	109.5
C9—C10—C8	109.3 (3)	H84A—C84—H84B	108.1
C7—C10—C8	108.9 (2)	C86—C85—C84	111.5 (7)
C9—C10—N11	109.4 (2)	C86—C85—C89	110.8 (7)
C7—C10—N11	109.8 (2)	C84—C85—C89	107.4 (7)
C8—C10—N11	109.6 (2)	C86—C85—H85	109.0
C14—N11—C12	108.6 (3)	C84—C85—H85	109.0
C14—N11—C13	108.4 (3)	C89—C85—H85	109.0
C12—N11—C13	105.4 (3)	C85—C86—C81	109.5 (7)
C14—N11—C10	111.7 (2)	C85—C86—H86A	109.8
C12—N11—C10	110.7 (3)	C81—C86—H86A	109.8
C13—N11—C10	111.8 (3)	C85—C86—H86B	109.8
N11—C12—H12A	109.5	C81—C86—H86B	109.8
N11—C12—H12B	109.5	H86A—C86—H86B	108.2
H12A—C12—H12B	109.5	C50—C87—C81	109.8 (7)
N11—C12—H12C	109.5	C50—C87—H87A	109.7
H12A—C12—H12C	109.5	C81—C87—H87A	109.7
H12B—C12—H12C	109.5	C50—C87—H87B	109.7
N11—C13—H13A	109.5	C81—C87—H87B	109.7
N11—C13—H13B	109.5	H87A—C87—H87B	108.2
H13A—C13—H13B	109.5	C83—C88—C50	108.8 (6)
N11—C13—H13C	109.5	C83—C88—H88A	109.9
H13A—C13—H13C	109.5	C50—C88—H88A	109.9
H13B—C13—H13C	109.5	C83—C88—H88B	109.9
N11—C14—H14A	109.5	C50—C88—H88B	109.9
N11—C14—H14B	109.5	H88A—C88—H88B	108.3
H14A—C14—H14B	109.5	C50—C89—C85	109.3 (6)
N11—C14—H14C	109.5	C50—C89—H89A	109.8
H14A—C14—H14C	109.5	C85—C89—H89A	109.8
H14B—C14—H14C	109.5	C50—C89—H89B	109.8
C26—C21—C27	107.8 (8)	C85—C89—H89B	109.8
C26—C21—C22	109.8 (10)	H89A—C89—H89B	108.3
C27—C21—C22	110.6 (9)	C92—C91—C96	112.2 (7)
C26—C21—H21	109.5	C92—C91—C97	106.5 (8)
C27—C21—H21	109.5	C96—C91—C97	108.4 (8)
C22—C21—H21	109.5	C92—C91—H91	109.9
C23—C22—C21	109.4 (9)	C96—C91—H91	109.9
C23—C22—H22A	109.8	C97—C91—H91	109.9
C21—C22—H22A	109.8	C91—C92—C93	111.9 (7)
C23—C22—H22B	109.8	C91—C92—H92A	109.2
C21—C22—H22B	109.8	C93—C92—H92A	109.2
H22A—C22—H22B	108.2	C91—C92—H92B	109.2
C22—C23—C24	109.6 (11)	C93—C92—H92B	109.2
C22—C23—C28	109.4 (9)	H92A—C92—H92B	107.9
C24—C23—C28	108.4 (9)	C94—C93—C98	110.3 (8)
C22—C23—H23	109.8	C94—C93—C92	106.8 (7)
C24—C23—H23	109.8	C98—C93—C92	108.3 (7)
C28—C23—H23	109.8	C94—C93—H93	110.4
C25—C24—C23	111.4 (12)	C98—C93—H93	110.4
C25—C24—H24A	109.3	C92—C93—H93	110.4
C23—C24—H24A	109.3	C95—C94—C93	109.7 (7)
C25—C24—H24B	109.3	C95—C94—H94A	109.7
C23—C24—H24B	109.3	C93—C94—H94A	109.7
H24A—C24—H24B	108.0	C95—C94—H94B	109.7
C26—C25—C24	109.9 (14)	C93—C94—H94B	109.7
C26—C25—C29	112.3 (11)	H94A—C94—H94B	108.2
C24—C25—C29	105.9 (14)	C96—C95—C94	115.5 (8)
C26—C25—H25	109.5	C96—C95—C99	108.1 (8)
C24—C25—H25	109.5	C94—C95—C99	108.1 (7)
C29—C25—H25	109.5	C96—C95—H95	108.3
C25—C26—C21	110.2 (12)	C94—C95—H95	108.3
C25—C26—H26A	109.6	C99—C95—H95	108.3
C21—C26—H26A	109.6	C95—C96—C91	107.8 (7)
C25—C26—H26B	109.6	C95—C96—H96A	110.1
C21—C26—H26B	109.6	C91—C96—H96A	110.1
H26A—C26—H26B	108.1	C95—C96—H96B	110.1
C30—C27—C21	109.8 (6)	C91—C96—H96B	110.1
C30—C27—H27A	109.7	H96A—C96—H96B	108.5
C21—C27—H27A	109.7	C50—C97—C91	108.8 (7)
C30—C27—H27B	109.7	C50—C97—H97A	109.9
C21—C27—H27B	109.7	C91—C97—H97A	109.9
H27A—C27—H27B	108.2	C50—C97—H97B	109.9
C23—C28—C30	108.3 (6)	C91—C97—H97B	109.9
C23—C28—H28A	110.0	H97A—C97—H97B	108.3
C30—C28—H28A	110.0	C93—C98—C50	109.0 (6)
C23—C28—H28B	110.0	C93—C98—H98A	109.9
C30—C28—H28B	110.0	C50—C98—H98A	109.9
H28A—C28—H28B	108.4	C93—C98—H98B	109.9
C30—C29—C25	109.2 (8)	C50—C98—H98B	109.9
C30—C29—H29A	109.8	H98A—C98—H98B	108.3
C25—C29—H29A	109.8	C50—C99—C95	109.4 (6)
C30—C29—H29B	109.8	C50—C99—H99A	109.8
C25—C29—H29B	109.8	C95—C99—H99A	109.8
H29A—C29—H29B	108.3	C50—C99—H99B	109.8
C76—C71—C72	110.2 (8)	C95—C99—H99B	109.8
C76—C71—C77	108.4 (7)	H99A—C99—H99B	108.2
C72—C71—C77	108.2 (7)	C48—C50—C87	71.3 (6)
C76—C71—H71	110.0	C48—C50—C89	119.6 (5)
C72—C71—H71	110.0	C87—C50—C89	111.8 (6)
C77—C71—H71	110.0	C48—C50—C97	57.3 (6)
C71—C72—C73	110.6 (8)	C87—C50—C97	122.2 (6)
C71—C72—H72A	109.5	C89—C50—C97	76.7 (6)
C73—C72—H72A	109.5	C48—C50—C99	55.3 (6)
C71—C72—H72B	109.5	C89—C50—C99	128.8 (5)
C73—C72—H72B	109.5	C97—C50—C99	111.4 (6)
H72A—C72—H72B	108.1	C48—C50—C98	134.8 (5)
C74—C73—C72	109.7 (9)	C87—C50—C98	85.5 (6)
C74—C73—C78	107.1 (8)	C89—C50—C98	36.1 (5)
C72—C73—C78	111.2 (9)	C97—C50—C98	111.8 (6)
C74—C73—H73	109.6	C99—C50—C98	105.7 (5)
C72—C73—H73	109.6	C48—C50—C49	112.7 (6)
C78—C73—H73	109.6	C87—C50—C49	133.3 (6)
C73—C74—C75	111.1 (10)	C97—C50—C49	59.3 (6)
C73—C74—H74A	109.4	C99—C50—C49	146.4 (5)
C75—C74—H74A	109.4	C98—C50—C49	58.1 (5)
C73—C74—H74B	109.4	C48—C50—N51	120.0 (4)
C75—C74—H74B	109.4	C87—C50—N51	111.6 (4)
H74A—C74—H74B	108.0	C89—C50—N51	114.1 (4)
C74—C75—C79	109.3 (8)	C97—C50—N51	115.7 (4)
C74—C75—C76	109.8 (9)	C99—C50—N51	107.0 (4)
C79—C75—C76	107.3 (6)	C98—C50—N51	104.4 (4)
C74—C75—H75	110.1	C49—C50—N51	105.6 (4)
C79—C75—H75	110.1	C87—C50—C88	109.4 (6)
C76—C75—H75	110.1	C89—C50—C88	107.4 (5)
C71—C76—C75	110.6 (7)	C99—C50—C88	91.9 (6)
C71—C76—H76A	109.5	C98—C50—C88	142.1 (5)
C75—C76—H76A	109.5	C49—C50—C88	88.8 (6)
C71—C76—H76B	109.5	N51—C50—C88	101.9 (4)
C75—C76—H76B	109.5	C48—C50—C47	106.4 (5)
H76A—C76—H76B	108.1	C89—C50—C47	77.2 (6)
C30—C77—C71	109.7 (5)	C97—C50—C47	133.7 (5)
C30—C77—H77A	109.7	C99—C50—C47	60.8 (5)
C71—C77—H77A	109.7	C98—C50—C47	45.6 (5)
C30—C77—H77B	109.7	C49—C50—C47	100.7 (5)
C71—C77—H77B	109.7	N51—C50—C47	109.8 (4)
H77A—C77—H77B	108.2	C88—C50—C47	142.8 (5)
C30—C78—C73	109.4 (6)	C54—N51—C53	119 (3)
C30—C78—H78A	109.8	C54—N51—C56	127 (3)
C73—C78—H78A	109.8	C54—N51—C55	59.7 (6)
C30—C78—H78B	109.8	C53—N51—C55	127 (3)
C73—C78—H78B	109.8	C56—N51—C55	114 (2)
H78A—C78—H78B	108.3	C54—N51—C52	103.5 (7)
C75—C79—C30	108.8 (5)	C53—N51—C52	96 (2)
C75—C79—H79A	109.9	C56—N51—C52	78 (2)
C30—C79—H79A	109.9	C55—N51—C52	45.8 (6)
C75—C79—H79B	109.9	C53—N51—C57	87 (3)
C30—C79—H79B	109.9	C56—N51—C57	103 (2)
H79A—C79—H79B	108.3	C55—N51—C57	99.4 (6)
C78—C30—C27	141.2 (4)	C52—N51—C57	136.4 (6)
C78—C30—C77	112.0 (4)	C54—N51—C50	114.8 (5)
C27—C30—C77	46.5 (4)	C53—N51—C50	112 (3)
C78—C30—C29	58.6 (4)	C56—N51—C50	114 (3)
C27—C30—C29	112.1 (4)	C55—N51—C50	113.7 (5)
C77—C30—C29	137.8 (4)	C52—N51—C50	108.3 (5)
C78—C30—C79	109.3 (4)	C57—N51—C50	110.6 (4)
C27—C30—C79	64.1 (3)	N51—C52—H52A	109.5
C77—C30—C79	107.7 (3)	N51—C52—H52B	109.5
C29—C30—C79	52.6 (4)	N51—C52—H52C	109.5
C78—C30—N31	109.2 (3)	N51—C53—H53A	109.5
C27—C30—N31	109.0 (3)	N51—C53—H53B	109.5
C77—C30—N31	110.3 (3)	N51—C53—H53C	109.5
C29—C30—N31	111.5 (3)	N51—C54—H54A	109.5
C79—C30—N31	108.3 (3)	N51—C54—H54B	109.5
C78—C30—C28	51.2 (4)	N51—C54—H54C	109.5
C27—C30—C28	109.2 (4)	N51—C55—H55A	109.5
C77—C30—C28	64.8 (3)	N51—C55—H55B	109.5
C29—C30—C28	106.7 (5)	N51—C55—H55C	109.5
C79—C30—C28	142.8 (4)	N51—C56—H56A	109.5
N31—C30—C28	108.3 (3)	N51—C56—H56B	109.5
C36—N31—C34	79.0 (7)	N51—C56—H56C	109.5
C36—N31—C32	128.2 (8)	N51—C57—H57A	109.5
C34—N31—C32	107.9 (7)	N51—C57—H57B	109.5
C36—N31—C35	109.2 (10)	N51—C57—H57C	109.5
C34—N31—C35	126.4 (8)	O2—Si1—O5	111.41 (10)
C36—N31—C37	107.4 (7)	O2—Si1—O3	111.41 (10)
C32—N31—C37	82.6 (8)	O5—Si1—O3	110.85 (10)
C35—N31—C37	106.4 (9)	O2—Si1—O4	108.22 (10)
C34—N31—C33	108.3 (6)	O5—Si1—O4	107.64 (10)
C32—N31—C33	104.4 (7)	O3—Si1—O4	107.10 (10)
C35—N31—C33	80.4 (8)	O7—Si2—O6	111.34 (10)
C37—N31—C33	132.0 (6)	O7—Si2—O8	111.42 (10)
C36—N31—C30	111.7 (4)	O6—Si2—O8	108.62 (10)
C34—N31—C30	113.6 (4)	O7—Si2—O5	110.96 (10)
C32—N31—C30	111.5 (6)	O6—Si2—O5	107.03 (10)
C35—N31—C30	111.6 (8)	O8—Si2—O5	107.28 (10)
C37—N31—C30	110.3 (5)	O9—Si3—O10	111.36 (10)
C33—N31—C30	110.7 (4)	O9—Si3—O8	111.02 (10)
N31—C32—H32A	109.5	O10—Si3—O8	108.60 (10)
N31—C32—H32B	109.5	O9—Si3—O3^i	110.97 (10)
N31—C32—H32C	109.5	O10—Si3—O3^i	107.47 (10)
N31—C33—H33A	109.5	O8—Si3—O3^i	107.25 (10)
N31—C33—H33B	109.5	O1—Si4—O6^i	111.38 (10)
N31—C33—H33C	109.5	O1—Si4—O10	111.65 (10)
N31—C34—H34A	109.5	O6^i—Si4—O10	109.12 (10)
N31—C34—H34B	109.5	O1—Si4—O2	111.00 (10)
N31—C34—H34C	109.5	O6^i—Si4—O2	106.74 (10)
N31—C35—H35A	109.5	O10—Si4—O2	106.72 (10)
N31—C35—H35B	109.5	Si1—O2—Si4	147.46 (13)
N31—C35—H35C	109.5	Si1—O3—Si3^i	145.37 (12)
N31—C36—H36A	109.5	Si1—O4—H4	109.5
N31—C36—H36B	109.5	Si1—O5—Si2	148.73 (13)
N31—C36—H36C	109.5	Si2—O6—Si4^i	149.48 (13)
N31—C37—H37A	109.5	Si3—O8—Si2	150.61 (12)
N31—C37—H37B	109.5	Si3—O10—Si4	151.87 (13)
N31—C37—H37C	109.5	H21D—O21—H21E	108.0
C42—C41—C46	111.5 (7)	H22D—O22—H22E	108.0
C42—C41—C47	108.4 (8)	H23D—O23—H23E	108.0
C46—C41—C47	109.5 (8)	H24D—O24—H24E	108.0
C42—C41—H41	109.2	H25D—O25—H25E	108.0
C46—C41—H41	109.2	H26D—O26—H26E	108.0
C47—C41—H41	109.2	H27D—O27—H27E	108.0
C41—C42—C43	109.6 (7)	H28D—O28—H28E	108.0
C41—C42—H42A	109.8	H29D—O29—H29E	108.0
C43—C42—H42A	109.8	H30D—O30—H30E	108.0
C41—C42—H42B	109.8	H31D—O31—H31E	108.0
C43—C42—H42B	109.8	H32D—O32—H32E	108.0
H42A—C42—H42B	108.2	H33D—O33—H33E	108.0
C44—C43—C48	111.2 (8)	H34D—O34—H34E	108.0
C44—C43—C42	112.0 (7)	H35D—O35—H35E	108.0
C48—C43—C42	103.8 (7)	H36D—O36—H36E	108.0
C44—C43—H43	109.9	H37D—O37—H37E	108.0
C48—C43—H43	109.9	H38D—O38—H38E	108.0
C42—C43—H43	109.9	H39D—O39—H39E	108.0
C45—C44—C43	107.9 (7)	H40D—O40—H40E	108.0
C45—C44—H44A	110.1	H41D—O41—H41E	108.0
C43—C44—H44A	110.1	H42D—O42—H42E	108.0
C45—C44—H44B	110.1

Symmetry code: (i) −x+2, −y, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H4···O29^ii	0.84	1.84	2.659 (4)	166
O21—H21D···O1^ii	0.84	1.83	2.664 (3)	173
O21—H21E···O23	0.84	1.94	2.775 (3)	174
O22—H22D···O9^iii	0.84	1.82	2.647 (3)	169
O22—H22E···O36^iii	0.84	1.98	2.809 (3)	172
O23—H23D···O9^ii	0.84	1.79	2.631 (3)	177
O23—H23E···O40^ii	0.84	1.93	2.758 (3)	167
O24—H24D···O7^iii	0.84	1.78	2.618 (3)	172
O24—H24E···O22	0.84	1.89	2.725 (3)	172
O25—H25D···O7^iii	0.84	1.85	2.689 (3)	176
O25—H25E···O38	0.84	2.02	2.831 (3)	163
O26—H26D···O7	0.84	1.91	2.710 (3)	160
O26—H26E	0.84
O27—H27D···O28	0.84	1.92	2.750 (3)	173
O27—H27E···O25^iv	0.84	1.96	2.794 (3)	174
O28—H28D···O24^iv	0.84	1.90	2.729 (3)	171
O28—H28E···O24^v	0.84	1.90	2.737 (3)	172
O29—H29D···O31	0.84	1.88	2.699 (3)	163
O29—H29E···O37	0.84	2.01	2.802 (3)	157
O30—H30D···O41^iv	0.84	2.03	2.763 (3)	145
O30—H30E	0.84
O31—H31D	0.84
O31—H31E···O1^ii	0.84	1.91	2.665 (3)	149
O32—H32D···O33	0.84	1.91	2.749 (3)	175
O32—H32E···O4^vi	0.84	2.01	2.831 (4)	164
O33—H33D···O42^ii	0.84	2.13	2.737 (3)	129
O33—H33E···O9^iii	0.84	1.97	2.710 (4)	147
O34—H34D···O30	0.84	1.88	2.712 (3)	170
O34—H34E···O33	0.84	1.94	2.774 (3)	174
O35—H35D···O21	0.84	1.94	2.783 (3)	176
O35—H35E···O34	0.84	2.01	2.785 (3)	154
O36—H36D	0.84
O36—H36E···O27	0.84	1.90	2.734 (3)	171
O37—H37D	0.84
O37—H37E···O39^vii	0.84	1.96	2.723 (3)	150
O38—H38D	0.84
O38—H38E···O1^vi	0.84	1.90	2.691 (3)	156
O39—H39D···O4	0.84	1.91	2.744 (3)	170
O39—H39E···O26	0.84	1.91	2.751 (3)	175
O40—H40D···O23^v	0.84	1.91	2.742 (3)	175
O40—H40E···O36	0.84	1.84	2.647 (3)	161
O41—H41D···O28	0.84	1.88	2.716 (3)	178
O41—H41E···O26	0.84	1.99	2.779 (3)	156
O42—H42D···O40	0.84	1.78	2.614 (3)	175
O42—H42E···O35^ii	0.84	2.00	2.840 (3)	177

Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) −x+1, −y+1, −z; (v) x+1, y, z; (vi) −x+1, −y, −z+1; (vii) x, y+1, z.