Dihydronium bromide tetra­kis(di-tert-butyl­methyl­silanol)

The asymmetric unit of the title compound, H₅O₂⁺·Br^-·4C₉H₂₂OSi, is composed of four di-tert-butyl­methyl­silanol mol­ecules, one Br^- anion, and two half H₅O₂⁺ ions, each of which has one disordered H atom. The silanol mol­ecules form hydrogen bonds to the Br anion and the H₅O₂⁺ ions form hydrogen bonds to the hydroxyl O atoms of the silanol mol­ecules.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.049
• wR factor = 0.111
• Data-to-parameter ratio = 22.5

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT222_ALERT_3_A Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       7.06 Ratio

Author Response: One methyl group shows high thermal motion or disorder.

Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.63 Ratio
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for         C1
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for         C2
PLAT417_ALERT_2_B Short Inter D-H..H-D       H1C    ..  H1WA    ..       2.05 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D       H2WB   ..  H2WC    ..       1.92 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.22
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Si1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for       Si1A
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C1A
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C2A
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for       Si1B
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C1B
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C1C
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C2C
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O1W
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O2W
PLAT354_ALERT_3_C Short   O-H Bond (0.82A)   O1     -   H1     ...       0.69 Ang.
PLAT354_ALERT_3_C Short   O-H Bond (0.82A)   O1A    -   H1A    ...       0.70 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H1     ..  H1WB    ..       2.14 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H1A    ..  H2WA    ..       2.14 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H1B    ..  H2WB    ..       2.10 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H1WA   ..  H1WC    ..       2.12 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H1WB   ..  H1WC    ..       2.11 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........         12

   1 ALERT level A = In general: serious problem
   5 ALERT level B = Potentially serious problem
  20 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  21 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
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check


checkCIF publication errors

Alert level A
PUBL023_ALERT_1_A There is a mismatched ^ on line 114
              H~3~O^+.Br^-^.4C~9~H~22~OSi.H~2~O, is composed of four
              If you require a ^ then it should be escaped
              with a \, i.e. \^
              Otherwise there must be a matching closing ~, e.g. ^12^C

   1 ALERT level A = Data missing that is essential or data in wrong format
   0 ALERT level G = General alerts. Data that may be required is missing

---

Computing details

Data collection: X-AREA (Stoe, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL and PLATON.

Hydroxonium bromide tetrakis(di-tert-butylmethylsilanol) monohydrate

Crystal data

H3O^+·Br^−·4C9H22OSi·H2O	F(000) = 1792
Mr = 814.36	Dx = 1.027 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 53702 reflections
a = 16.4814 (8) Å	θ = 3.5–25.7°
b = 16.1107 (5) Å	µ = 0.90 mm^−1
c = 20.0624 (10) Å	T = 173 K
β = 98.510 (4)°	Needle, colourless
V = 5268.5 (4) Å^3	0.30 × 0.13 × 0.12 mm
Z = 4

Data collection

Stoe IPDS-II two-circle diffractometer	9889 independent reflections
Radiation source: fine-focus sealed tube	8181 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.065
ω scans	θmax = 25.7°, θmin = 3.5°
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995)	h = −20→20
Tmin = 0.773, Tmax = 0.899	k = −18→19
69100 measured reflections	l = −24→24

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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.111	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0494P)^2 + 4.5021P] where P = (Fo^2 + 2Fc^2)/3
9889 reflections	(Δ/σ)max = 0.001
440 parameters	Δρmax = 1.37 e Å^−3
0 restraints	Δρmin = −0.43 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)
Si1	0.29278 (5)	0.49628 (5)	0.30925 (4)	0.02992 (17)
O1	0.33306 (13)	0.49827 (15)	0.39043 (11)	0.0387 (5)
H1	0.316 (2)	0.524 (2)	0.4122 (17)	0.032 (10)*
C1	0.3183 (2)	0.5988 (2)	0.2698 (2)	0.0536 (9)
C2	0.17986 (18)	0.4679 (2)	0.30236 (16)	0.0416 (7)
C3	0.3503 (2)	0.4097 (2)	0.27457 (17)	0.0519 (9)
H3A	0.4084	0.4246	0.2782	0.078*
H3B	0.3278	0.4005	0.2271	0.078*
H3C	0.3446	0.3589	0.3003	0.078*
C11	0.2838 (4)	0.6738 (3)	0.3024 (3)	0.104 (2)
H11M	0.2240	0.6687	0.2985	0.156*
H11N	0.2976	0.7245	0.2796	0.156*
H11O	0.3075	0.6764	0.3501	0.156*
C12	0.2856 (3)	0.6021 (3)	0.1939 (2)	0.0839 (15)
H12M	0.3069	0.5545	0.1713	0.126*
H12N	0.3037	0.6537	0.1748	0.126*
H12O	0.2256	0.6000	0.1872	0.126*
C13	0.4127 (3)	0.6048 (4)	0.2766 (4)	0.151 (4)
H13M	0.4341	0.5564	0.2553	0.226*
H13N	0.4361	0.6064	0.3244	0.226*
H13O	0.4279	0.6555	0.2544	0.226*
C21	0.1267 (2)	0.5389 (4)	0.3222 (3)	0.0965 (19)
H21M	0.1307	0.5865	0.2924	0.145*
H21N	0.1459	0.5551	0.3690	0.145*
H21O	0.0695	0.5206	0.3179	0.145*
C22	0.1457 (3)	0.4413 (3)	0.2300 (2)	0.0791 (14)
H22M	0.1493	0.4879	0.1993	0.119*
H22N	0.0882	0.4245	0.2280	0.119*
H22O	0.1778	0.3945	0.2168	0.119*
C23	0.1729 (3)	0.3942 (4)	0.3486 (3)	0.106 (2)
H23M	0.1940	0.4099	0.3952	0.159*
H23N	0.2051	0.3477	0.3349	0.159*
H23O	0.1153	0.3777	0.3455	0.159*
Si1A	0.20738 (4)	0.53436 (5)	0.69579 (4)	0.02799 (17)
O1A	0.17714 (13)	0.52933 (14)	0.61259 (11)	0.0346 (5)
H1A	0.202 (2)	0.547 (2)	0.591 (2)	0.049 (13)*
C1A	0.1812 (2)	0.6421 (2)	0.72526 (16)	0.0439 (8)
C2A	0.31957 (18)	0.5024 (2)	0.71410 (15)	0.0388 (7)
C3A	0.1427 (3)	0.4553 (3)	0.73082 (19)	0.0648 (11)
H3D	0.0849	0.4719	0.7214	0.097*
H3E	0.1594	0.4510	0.7797	0.097*
H3F	0.1498	0.4013	0.7099	0.097*
C11A	0.0861 (3)	0.6468 (4)	0.7217 (3)	0.0887 (16)
H11D	0.0679	0.6042	0.7511	0.133*
H11E	0.0599	0.6373	0.6752	0.133*
H11F	0.0706	0.7018	0.7366	0.133*
C12A	0.2189 (3)	0.6593 (3)	0.79851 (18)	0.0675 (12)
H12D	0.2017	0.6160	0.8278	0.101*
H12E	0.2003	0.7135	0.8124	0.101*
H12F	0.2789	0.6593	0.8022	0.101*
C13A	0.2075 (3)	0.7098 (2)	0.6792 (2)	0.0747 (14)
H13D	0.1832	0.6986	0.6325	0.112*
H13E	0.2674	0.7101	0.6826	0.112*
H13F	0.1888	0.7640	0.6930	0.112*
C21A	0.3436 (3)	0.4778 (3)	0.78904 (18)	0.0598 (10)
H21D	0.3362	0.5257	0.8177	0.090*
H21E	0.4011	0.4603	0.7970	0.090*
H21F	0.3086	0.4321	0.7999	0.090*
C22A	0.3313 (3)	0.4266 (3)	0.6700 (2)	0.0736 (13)
H22D	0.2947	0.3819	0.6800	0.110*
H22E	0.3884	0.4077	0.6796	0.110*
H22F	0.3185	0.4420	0.6224	0.110*
C23A	0.3783 (2)	0.5715 (3)	0.6972 (2)	0.0578 (10)
H23D	0.3721	0.6204	0.7250	0.087*
H23E	0.3651	0.5863	0.6495	0.087*
H23F	0.4350	0.5515	0.7065	0.087*
Si1B	0.02814 (5)	0.77140 (5)	0.44173 (4)	0.03002 (17)
O1B	0.07749 (14)	0.68906 (13)	0.47876 (12)	0.0384 (5)
H1B	0.120 (2)	0.679 (2)	0.4756 (18)	0.042 (11)*
C1B	−0.06817 (18)	0.7768 (2)	0.48320 (18)	0.0436 (8)
C2B	0.10014 (18)	0.86406 (18)	0.45230 (15)	0.0340 (6)
C3B	0.0002 (3)	0.7507 (3)	0.34907 (18)	0.0664 (11)
H3B1	0.0502	0.7480	0.3281	0.100*
H3B2	−0.0351	0.7955	0.3283	0.100*
H3B3	−0.0292	0.6978	0.3424	0.100*
C11B	−0.1241 (2)	0.7027 (3)	0.4577 (3)	0.0759 (14)
H11G	−0.0946	0.6505	0.4691	0.114*
H11H	−0.1393	0.7065	0.4087	0.114*
H11I	−0.1738	0.7040	0.4791	0.114*
C12B	−0.1160 (2)	0.8577 (2)	0.4648 (2)	0.0650 (11)
H12G	−0.1293	0.8621	0.4156	0.098*
H12H	−0.0823	0.9053	0.4822	0.098*
H12I	−0.1668	0.8572	0.4847	0.098*
C13B	−0.0490 (3)	0.7718 (3)	0.5603 (2)	0.0699 (12)
H13G	−0.0185	0.7206	0.5733	0.105*
H13H	−0.1003	0.7717	0.5794	0.105*
H13I	−0.0158	0.8198	0.5775	0.105*
C21B	0.1232 (2)	0.8902 (2)	0.52691 (18)	0.0524 (9)
H21G	0.1469	0.8427	0.5534	0.079*
H21H	0.0739	0.9091	0.5444	0.079*
H21I	0.1633	0.9355	0.5302	0.079*
C22B	0.1798 (2)	0.8402 (2)	0.42495 (19)	0.0493 (8)
H22G	0.2055	0.7928	0.4504	0.074*
H22H	0.2177	0.8875	0.4299	0.074*
H22I	0.1668	0.8254	0.3772	0.074*
C23B	0.0622 (2)	0.9392 (2)	0.41037 (19)	0.0495 (8)
H23G	0.0475	0.9226	0.3631	0.074*
H23H	0.1023	0.9845	0.4135	0.074*
H23I	0.0130	0.9579	0.4280	0.074*
Si1C	0.48370 (4)	0.78542 (5)	0.51337 (4)	0.02846 (17)
O1C	0.45820 (14)	0.68558 (13)	0.52059 (13)	0.0416 (5)
H1C	0.415 (3)	0.674 (3)	0.520 (2)	0.066 (14)*
C1C	0.59581 (18)	0.7820 (2)	0.50069 (16)	0.0400 (7)
C2C	0.45846 (18)	0.84031 (18)	0.59181 (14)	0.0334 (6)
C3C	0.4213 (2)	0.8311 (2)	0.43600 (16)	0.0461 (8)
H3C1	0.3635	0.8331	0.4421	0.069*
H3C2	0.4273	0.7966	0.3968	0.069*
H3C3	0.4408	0.8874	0.4288	0.069*
C11C	0.6255 (2)	0.8679 (3)	0.4816 (3)	0.0707 (12)
H11J	0.5898	0.8883	0.4415	0.106*
H11K	0.6819	0.8637	0.4720	0.106*
H11L	0.6236	0.9065	0.5190	0.106*
C12C	0.6512 (2)	0.7488 (3)	0.5637 (2)	0.0608 (10)
H12J	0.6316	0.6941	0.5755	0.091*
H12K	0.6496	0.7871	0.6014	0.091*
H12L	0.7077	0.7441	0.5543	0.091*
C13C	0.6032 (2)	0.7217 (3)	0.4419 (2)	0.0682 (12)
H13J	0.5846	0.6663	0.4531	0.102*
H13K	0.6606	0.7188	0.4344	0.102*
H13L	0.5692	0.7417	0.4008	0.102*
C21C	0.4942 (3)	0.9282 (2)	0.5985 (2)	0.0599 (10)
H21J	0.5542	0.9253	0.6036	0.090*
H21K	0.4777	0.9553	0.6381	0.090*
H21L	0.4736	0.9603	0.5580	0.090*
C22C	0.4886 (3)	0.7920 (3)	0.65692 (19)	0.0714 (12)
H22J	0.4658	0.7357	0.6533	0.107*
H22K	0.4705	0.8205	0.6953	0.107*
H22L	0.5486	0.7890	0.6636	0.107*
C23C	0.3642 (2)	0.8465 (3)	0.5841 (2)	0.0605 (11)
H23J	0.3405	0.7906	0.5798	0.091*
H23K	0.3439	0.8789	0.5437	0.091*
H23L	0.3484	0.8739	0.6238	0.091*
Br1	0.268207 (16)	0.621779 (18)	0.499702 (13)	0.03084 (9)
O1W	0.51633 (13)	0.53628 (13)	0.55359 (11)	0.0444 (5)
H1WA	0.5000	0.5855	0.5551	0.053*
H1WB	0.5625	0.5267	0.5762	0.053*
H1WC	0.5050	0.5112	0.5167	0.053*	0.50
O2W	0.03376 (13)	0.55318 (14)	0.53770 (11)	0.0443 (5)
H2WA	0.0710	0.5438	0.5702	0.053*
H2WB	0.0448	0.5874	0.5087	0.053*
H2WC	0.0107	0.5166	0.5117	0.053*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Si1	0.0273 (4)	0.0333 (4)	0.0269 (4)	0.0080 (3)	−0.0033 (3)	−0.0026 (3)
O1	0.0341 (11)	0.0466 (13)	0.0316 (11)	0.0179 (10)	−0.0078 (9)	−0.0138 (10)
C1	0.047 (2)	0.049 (2)	0.063 (2)	0.0012 (16)	0.0006 (17)	0.0145 (17)
C2	0.0317 (15)	0.0460 (18)	0.0424 (17)	0.0020 (14)	−0.0101 (13)	0.0016 (14)
C3	0.056 (2)	0.060 (2)	0.0383 (17)	0.0225 (18)	0.0038 (15)	−0.0098 (16)
C11	0.201 (7)	0.035 (2)	0.081 (3)	0.002 (3)	0.040 (4)	0.005 (2)
C12	0.114 (4)	0.084 (3)	0.059 (3)	0.016 (3)	0.030 (3)	0.028 (2)
C13	0.058 (3)	0.138 (6)	0.246 (9)	−0.032 (4)	−0.011 (4)	0.113 (6)
C21	0.0281 (19)	0.123 (4)	0.134 (5)	0.009 (2)	−0.002 (2)	−0.061 (4)
C22	0.059 (3)	0.101 (4)	0.066 (3)	−0.013 (2)	−0.028 (2)	−0.015 (3)
C23	0.046 (2)	0.132 (5)	0.133 (5)	−0.023 (3)	−0.011 (3)	0.078 (4)
Si1A	0.0259 (4)	0.0341 (4)	0.0231 (3)	−0.0051 (3)	0.0006 (3)	0.0051 (3)
O1A	0.0321 (11)	0.0432 (12)	0.0266 (10)	−0.0077 (10)	−0.0022 (9)	0.0044 (9)
C1A	0.0467 (18)	0.052 (2)	0.0337 (16)	0.0142 (15)	0.0077 (13)	−0.0038 (14)
C2A	0.0361 (16)	0.0420 (17)	0.0344 (15)	0.0074 (14)	−0.0075 (12)	−0.0059 (13)
C3A	0.062 (2)	0.080 (3)	0.052 (2)	−0.028 (2)	0.0068 (18)	0.020 (2)
C11A	0.056 (3)	0.126 (5)	0.085 (3)	0.039 (3)	0.014 (2)	−0.011 (3)
C12A	0.091 (3)	0.072 (3)	0.0388 (19)	0.019 (2)	0.0094 (19)	−0.0179 (18)
C13A	0.132 (4)	0.036 (2)	0.059 (2)	0.014 (2)	0.027 (3)	0.0012 (17)
C21A	0.065 (2)	0.061 (2)	0.045 (2)	0.014 (2)	−0.0194 (17)	0.0065 (17)
C22A	0.072 (3)	0.070 (3)	0.072 (3)	0.034 (2)	−0.013 (2)	−0.026 (2)
C23A	0.0267 (16)	0.084 (3)	0.061 (2)	−0.0068 (17)	0.0011 (15)	−0.001 (2)
Si1B	0.0290 (4)	0.0285 (4)	0.0313 (4)	0.0060 (3)	0.0003 (3)	0.0015 (3)
O1B	0.0256 (11)	0.0279 (11)	0.0617 (14)	0.0064 (9)	0.0066 (10)	0.0100 (10)
C1B	0.0265 (15)	0.0398 (18)	0.065 (2)	0.0050 (13)	0.0069 (14)	0.0106 (15)
C2B	0.0361 (15)	0.0287 (15)	0.0380 (15)	0.0045 (12)	0.0075 (12)	0.0084 (12)
C3B	0.086 (3)	0.066 (3)	0.041 (2)	0.005 (2)	−0.0091 (19)	−0.0132 (18)
C11B	0.0362 (19)	0.059 (3)	0.131 (4)	−0.0090 (18)	0.006 (2)	0.003 (3)
C12B	0.0371 (19)	0.052 (2)	0.107 (3)	0.0178 (17)	0.017 (2)	0.015 (2)
C13B	0.064 (3)	0.091 (3)	0.064 (3)	0.011 (2)	0.038 (2)	0.015 (2)
C21B	0.059 (2)	0.046 (2)	0.049 (2)	−0.0076 (17)	−0.0014 (16)	−0.0047 (16)
C22B	0.0395 (17)	0.0423 (18)	0.070 (2)	0.0080 (15)	0.0215 (16)	0.0182 (17)
C23B	0.053 (2)	0.0348 (17)	0.062 (2)	0.0114 (15)	0.0132 (17)	0.0163 (16)
Si1C	0.0252 (4)	0.0284 (4)	0.0321 (4)	0.0017 (3)	0.0054 (3)	−0.0033 (3)
O1C	0.0261 (11)	0.0273 (11)	0.0717 (16)	0.0004 (9)	0.0083 (11)	−0.0119 (10)
C1C	0.0286 (15)	0.0456 (18)	0.0472 (18)	0.0021 (13)	0.0096 (13)	0.0001 (14)
C2C	0.0384 (15)	0.0318 (15)	0.0315 (14)	−0.0015 (13)	0.0097 (12)	−0.0072 (12)
C3C	0.0404 (17)	0.057 (2)	0.0382 (17)	0.0065 (16)	−0.0030 (13)	0.0055 (15)
C11C	0.045 (2)	0.061 (3)	0.113 (4)	−0.0033 (19)	0.037 (2)	0.016 (2)
C12C	0.0269 (16)	0.083 (3)	0.069 (2)	0.0144 (17)	−0.0039 (16)	0.006 (2)
C13C	0.050 (2)	0.090 (3)	0.070 (3)	0.010 (2)	0.0291 (19)	−0.018 (2)
C21C	0.077 (3)	0.043 (2)	0.061 (2)	−0.0131 (19)	0.015 (2)	−0.0232 (17)
C22C	0.096 (3)	0.082 (3)	0.039 (2)	0.017 (3)	0.021 (2)	0.011 (2)
C23C	0.046 (2)	0.075 (3)	0.064 (2)	−0.0016 (19)	0.0217 (17)	−0.036 (2)
Br1	0.02711 (14)	0.03775 (15)	0.02840 (14)	0.00447 (12)	0.00660 (9)	−0.00006 (12)
O1W	0.0375 (11)	0.0353 (11)	0.0538 (13)	0.0102 (9)	−0.0150 (10)	−0.0070 (10)
O2W	0.0367 (11)	0.0442 (13)	0.0468 (12)	−0.0074 (10)	−0.0108 (9)	0.0138 (10)

Geometric parameters (Å, º)

Si1—O1	1.666 (2)	Si1B—C1B	1.900 (3)
Si1—C3	1.877 (3)	O1B—H1B	0.72 (4)
Si1—C2	1.902 (3)	C1B—C13B	1.535 (5)
Si1—C1	1.905 (4)	C1B—C12B	1.540 (4)
O1—H1	0.69 (3)	C1B—C11B	1.549 (5)
C1—C11	1.524 (6)	C2B—C22B	1.544 (4)
C1—C12	1.540 (6)	C2B—C21B	1.547 (4)
C1—C13	1.545 (6)	C2B—C23B	1.551 (4)
C2—C23	1.520 (5)	C3B—H3B1	0.9800
C2—C21	1.529 (5)	C3B—H3B2	0.9800
C2—C22	1.538 (5)	C3B—H3B3	0.9800
C3—H3A	0.9800	C11B—H11G	0.9800
C3—H3B	0.9800	C11B—H11H	0.9800
C3—H3C	0.9800	C11B—H11I	0.9800
C11—H11M	0.9800	C12B—H12G	0.9800
C11—H11N	0.9800	C12B—H12H	0.9800
C11—H11O	0.9800	C12B—H12I	0.9800
C12—H12M	0.9800	C13B—H13G	0.9800
C12—H12N	0.9800	C13B—H13H	0.9800
C12—H12O	0.9800	C13B—H13I	0.9800
C13—H13M	0.9800	C21B—H21G	0.9800
C13—H13N	0.9800	C21B—H21H	0.9800
C13—H13O	0.9800	C21B—H21I	0.9800
C21—H21M	0.9800	C22B—H22G	0.9800
C21—H21N	0.9800	C22B—H22H	0.9800
C21—H21O	0.9800	C22B—H22I	0.9800
C22—H22M	0.9800	C23B—H23G	0.9800
C22—H22N	0.9800	C23B—H23H	0.9800
C22—H22O	0.9800	C23B—H23I	0.9800
C23—H23M	0.9800	Si1C—O1C	1.674 (2)
C23—H23N	0.9800	Si1C—C3C	1.880 (3)
C23—H23O	0.9800	Si1C—C1C	1.903 (3)
Si1A—O1A	1.672 (2)	Si1C—C2C	1.904 (3)
Si1A—C3A	1.865 (4)	O1C—H1C	0.73 (4)
Si1A—C2A	1.902 (3)	C1C—C11C	1.535 (5)
Si1A—C1A	1.904 (3)	C1C—C12C	1.542 (5)
O1A—H1A	0.69 (4)	C1C—C13C	1.548 (5)
C1A—C12A	1.534 (5)	C2C—C21C	1.532 (4)
C1A—C13A	1.533 (5)	C2C—C22C	1.538 (5)
C1A—C11A	1.561 (5)	C2C—C23C	1.541 (4)
C2A—C22A	1.537 (5)	C3C—H3C1	0.9800
C2A—C23A	1.545 (5)	C3C—H3C2	0.9800
C2A—C21A	1.548 (4)	C3C—H3C3	0.9800
C3A—H3D	0.9800	C11C—H11J	0.9800
C3A—H3E	0.9800	C11C—H11K	0.9800
C3A—H3F	0.9800	C11C—H11L	0.9800
C11A—H11D	0.9800	C12C—H12J	0.9800
C11A—H11E	0.9800	C12C—H12K	0.9800
C11A—H11F	0.9800	C12C—H12L	0.9800
C12A—H12D	0.9800	C13C—H13J	0.9800
C12A—H12E	0.9800	C13C—H13K	0.9800
C12A—H12F	0.9800	C13C—H13L	0.9800
C13A—H13D	0.9800	C21C—H21J	0.9800
C13A—H13E	0.9800	C21C—H21K	0.9800
C13A—H13F	0.9800	C21C—H21L	0.9800
C21A—H21D	0.9800	C22C—H22J	0.9800
C21A—H21E	0.9800	C22C—H22K	0.9800
C21A—H21F	0.9800	C22C—H22L	0.9800
C22A—H22D	0.9800	C23C—H23J	0.9800
C22A—H22E	0.9800	C23C—H23K	0.9800
C22A—H22F	0.9800	C23C—H23L	0.9800
C23A—H23D	0.9800	O1W—H1WA	0.8400
C23A—H23E	0.9800	O1W—H1WB	0.8400
C23A—H23F	0.9800	O1W—H1WC	0.8400
Si1B—O1B	1.672 (2)	O2W—H2WA	0.8400
Si1B—C3B	1.878 (4)	O2W—H2WB	0.8399
Si1B—C2B	1.899 (3)	O2W—H2WC	0.8400
O1—Si1—C3	103.11 (13)	O1B—Si1B—C1B	103.00 (13)
O1—Si1—C2	108.65 (14)	C3B—Si1B—C1B	110.07 (19)
C3—Si1—C2	109.68 (17)	C2B—Si1B—C1B	117.62 (14)
O1—Si1—C1	107.99 (15)	Si1B—O1B—H1B	124 (3)
C3—Si1—C1	109.59 (18)	C13B—C1B—C12B	108.0 (3)
C2—Si1—C1	116.92 (15)	C13B—C1B—C11B	108.4 (3)
Si1—O1—H1	119 (3)	C12B—C1B—C11B	108.4 (3)
C11—C1—C12	107.4 (4)	C13B—C1B—Si1B	112.2 (2)
C11—C1—C13	110.3 (5)	C12B—C1B—Si1B	111.4 (2)
C12—C1—C13	106.6 (5)	C11B—C1B—Si1B	108.4 (3)
C11—C1—Si1	112.9 (3)	C22B—C2B—C21B	108.2 (3)
C12—C1—Si1	112.0 (3)	C22B—C2B—C23B	107.3 (3)
C13—C1—Si1	107.4 (3)	C21B—C2B—C23B	109.5 (3)
C23—C2—C21	109.1 (4)	C22B—C2B—Si1B	108.3 (2)
C23—C2—C22	108.0 (4)	C21B—C2B—Si1B	112.4 (2)
C21—C2—C22	108.1 (3)	C23B—C2B—Si1B	111.0 (2)
C23—C2—Si1	107.7 (2)	Si1B—C3B—H3B1	109.5
C21—C2—Si1	113.1 (3)	Si1B—C3B—H3B2	109.5
C22—C2—Si1	110.7 (3)	H3B1—C3B—H3B2	109.5
Si1—C3—H3A	109.5	Si1B—C3B—H3B3	109.5
Si1—C3—H3B	109.5	H3B1—C3B—H3B3	109.5
H3A—C3—H3B	109.5	H3B2—C3B—H3B3	109.5
Si1—C3—H3C	109.5	C1B—C11B—H11G	109.5
H3A—C3—H3C	109.5	C1B—C11B—H11H	109.5
H3B—C3—H3C	109.5	H11G—C11B—H11H	109.5
C1—C11—H11M	109.5	C1B—C11B—H11I	109.5
C1—C11—H11N	109.5	H11G—C11B—H11I	109.5
H11M—C11—H11N	109.5	H11H—C11B—H11I	109.5
C1—C11—H11O	109.5	C1B—C12B—H12G	109.5
H11M—C11—H11O	109.5	C1B—C12B—H12H	109.5
H11N—C11—H11O	109.5	H12G—C12B—H12H	109.5
C1—C12—H12M	109.5	C1B—C12B—H12I	109.5
C1—C12—H12N	109.5	H12G—C12B—H12I	109.5
H12M—C12—H12N	109.5	H12H—C12B—H12I	109.5
C1—C12—H12O	109.5	C1B—C13B—H13G	109.5
H12M—C12—H12O	109.5	C1B—C13B—H13H	109.5
H12N—C12—H12O	109.5	H13G—C13B—H13H	109.5
C1—C13—H13M	109.5	C1B—C13B—H13I	109.5
C1—C13—H13N	109.5	H13G—C13B—H13I	109.5
H13M—C13—H13N	109.5	H13H—C13B—H13I	109.5
C1—C13—H13O	109.5	C2B—C21B—H21G	109.5
H13M—C13—H13O	109.5	C2B—C21B—H21H	109.5
H13N—C13—H13O	109.5	H21G—C21B—H21H	109.5
C2—C21—H21M	109.5	C2B—C21B—H21I	109.5
C2—C21—H21N	109.5	H21G—C21B—H21I	109.5
H21M—C21—H21N	109.5	H21H—C21B—H21I	109.5
C2—C21—H21O	109.5	C2B—C22B—H22G	109.5
H21M—C21—H21O	109.5	C2B—C22B—H22H	109.5
H21N—C21—H21O	109.5	H22G—C22B—H22H	109.5
C2—C22—H22M	109.5	C2B—C22B—H22I	109.5
C2—C22—H22N	109.5	H22G—C22B—H22I	109.5
H22M—C22—H22N	109.5	H22H—C22B—H22I	109.5
C2—C22—H22O	109.5	C2B—C23B—H23G	109.5
H22M—C22—H22O	109.5	C2B—C23B—H23H	109.5
H22N—C22—H22O	109.5	H23G—C23B—H23H	109.5
C2—C23—H23M	109.5	C2B—C23B—H23I	109.5
C2—C23—H23N	109.5	H23G—C23B—H23I	109.5
H23M—C23—H23N	109.5	H23H—C23B—H23I	109.5
C2—C23—H23O	109.5	O1C—Si1C—C3C	109.51 (15)
H23M—C23—H23O	109.5	O1C—Si1C—C1C	104.19 (13)
H23N—C23—H23O	109.5	C3C—Si1C—C1C	108.90 (15)
O1A—Si1A—C3A	103.92 (15)	O1C—Si1C—C2C	106.64 (13)
O1A—Si1A—C2A	108.51 (13)	C3C—Si1C—C2C	109.94 (15)
C3A—Si1A—C2A	109.63 (18)	C1C—Si1C—C2C	117.32 (14)
O1A—Si1A—C1A	107.85 (13)	Si1C—O1C—H1C	120 (4)
C3A—Si1A—C1A	109.73 (19)	C11C—C1C—C12C	110.2 (3)
C2A—Si1A—C1A	116.46 (14)	C11C—C1C—C13C	108.1 (3)
Si1A—O1A—H1A	119 (3)	C12C—C1C—C13C	107.6 (3)
C12A—C1A—C13A	109.8 (3)	C11C—C1C—Si1C	111.0 (2)
C12A—C1A—C11A	107.3 (3)	C12C—C1C—Si1C	111.7 (2)
C13A—C1A—C11A	108.1 (4)	C13C—C1C—Si1C	107.9 (2)
C12A—C1A—Si1A	112.5 (2)	C21C—C2C—C22C	108.8 (3)
C13A—C1A—Si1A	111.3 (2)	C21C—C2C—C23C	108.5 (3)
C11A—C1A—Si1A	107.6 (3)	C22C—C2C—C23C	108.2 (3)
C22A—C2A—C23A	108.0 (3)	C21C—C2C—Si1C	111.9 (2)
C22A—C2A—C21A	108.6 (3)	C22C—C2C—Si1C	112.6 (2)
C23A—C2A—C21A	108.6 (3)	C23C—C2C—Si1C	106.7 (2)
C22A—C2A—Si1A	107.8 (2)	Si1C—C3C—H3C1	109.5
C23A—C2A—Si1A	112.7 (2)	Si1C—C3C—H3C2	109.5
C21A—C2A—Si1A	111.0 (2)	H3C1—C3C—H3C2	109.5
Si1A—C3A—H3D	109.5	Si1C—C3C—H3C3	109.5
Si1A—C3A—H3E	109.5	H3C1—C3C—H3C3	109.5
H3D—C3A—H3E	109.5	H3C2—C3C—H3C3	109.5
Si1A—C3A—H3F	109.5	C1C—C11C—H11J	109.5
H3D—C3A—H3F	109.5	C1C—C11C—H11K	109.5
H3E—C3A—H3F	109.5	H11J—C11C—H11K	109.5
C1A—C11A—H11D	109.5	C1C—C11C—H11L	109.5
C1A—C11A—H11E	109.5	H11J—C11C—H11L	109.5
H11D—C11A—H11E	109.5	H11K—C11C—H11L	109.5
C1A—C11A—H11F	109.5	C1C—C12C—H12J	109.5
H11D—C11A—H11F	109.5	C1C—C12C—H12K	109.5
H11E—C11A—H11F	109.5	H12J—C12C—H12K	109.5
C1A—C12A—H12D	109.5	C1C—C12C—H12L	109.5
C1A—C12A—H12E	109.5	H12J—C12C—H12L	109.5
H12D—C12A—H12E	109.5	H12K—C12C—H12L	109.5
C1A—C12A—H12F	109.5	C1C—C13C—H13J	109.5
H12D—C12A—H12F	109.5	C1C—C13C—H13K	109.5
H12E—C12A—H12F	109.5	H13J—C13C—H13K	109.5
C1A—C13A—H13D	109.5	C1C—C13C—H13L	109.5
C1A—C13A—H13E	109.5	H13J—C13C—H13L	109.5
H13D—C13A—H13E	109.5	H13K—C13C—H13L	109.5
C1A—C13A—H13F	109.5	C2C—C21C—H21J	109.5
H13D—C13A—H13F	109.5	C2C—C21C—H21K	109.5
H13E—C13A—H13F	109.5	H21J—C21C—H21K	109.5
C2A—C21A—H21D	109.5	C2C—C21C—H21L	109.5
C2A—C21A—H21E	109.5	H21J—C21C—H21L	109.5
H21D—C21A—H21E	109.5	H21K—C21C—H21L	109.5
C2A—C21A—H21F	109.5	C2C—C22C—H22J	109.5
H21D—C21A—H21F	109.5	C2C—C22C—H22K	109.5
H21E—C21A—H21F	109.5	H22J—C22C—H22K	109.5
C2A—C22A—H22D	109.5	C2C—C22C—H22L	109.5
C2A—C22A—H22E	109.5	H22J—C22C—H22L	109.5
H22D—C22A—H22E	109.5	H22K—C22C—H22L	109.5
C2A—C22A—H22F	109.5	C2C—C23C—H23J	109.5
H22D—C22A—H22F	109.5	C2C—C23C—H23K	109.5
H22E—C22A—H22F	109.5	H23J—C23C—H23K	109.5
C2A—C23A—H23D	109.5	C2C—C23C—H23L	109.5
C2A—C23A—H23E	109.5	H23J—C23C—H23L	109.5
H23D—C23A—H23E	109.5	H23K—C23C—H23L	109.5
C2A—C23A—H23F	109.5	H1WA—O1W—H1WB	115.1
H23D—C23A—H23F	109.5	H1WA—O1W—H1WC	117.1
H23E—C23A—H23F	109.5	H1WB—O1W—H1WC	116.8
O1B—Si1B—C3B	109.34 (16)	H2WA—O2W—H2WB	116.6
O1B—Si1B—C2B	108.62 (12)	H2WA—O2W—H2WC	124.5
C3B—Si1B—C2B	107.93 (18)	H2WB—O2W—H2WC	98.9
O1—Si1—C1—C11	−60.2 (4)	O1B—Si1B—C1B—C13B	49.2 (3)
C3—Si1—C1—C11	−171.9 (3)	C3B—Si1B—C1B—C13B	165.7 (3)
C2—Si1—C1—C11	62.6 (4)	C2B—Si1B—C1B—C13B	−70.2 (3)
O1—Si1—C1—C12	178.4 (3)	O1B—Si1B—C1B—C12B	170.4 (3)
C3—Si1—C1—C12	66.8 (3)	C3B—Si1B—C1B—C12B	−73.1 (3)
C2—Si1—C1—C12	−58.8 (3)	C2B—Si1B—C1B—C12B	51.1 (3)
O1—Si1—C1—C13	61.7 (5)	O1B—Si1B—C1B—C11B	−70.5 (3)
C3—Si1—C1—C13	−50.0 (5)	C3B—Si1B—C1B—C11B	46.0 (3)
C2—Si1—C1—C13	−175.5 (4)	C2B—Si1B—C1B—C11B	170.2 (2)
O1—Si1—C2—C23	−46.3 (4)	O1B—Si1B—C2B—C22B	54.4 (2)
C3—Si1—C2—C23	65.8 (4)	C3B—Si1B—C2B—C22B	−64.0 (3)
C1—Si1—C2—C23	−168.7 (3)	C1B—Si1B—C2B—C22B	170.8 (2)
O1—Si1—C2—C21	74.4 (3)	O1B—Si1B—C2B—C21B	−65.1 (3)
C3—Si1—C2—C21	−173.6 (3)	C3B—Si1B—C2B—C21B	176.5 (2)
C1—Si1—C2—C21	−48.1 (4)	C1B—Si1B—C2B—C21B	51.3 (3)
O1—Si1—C2—C22	−164.1 (3)	O1B—Si1B—C2B—C23B	171.9 (2)
C3—Si1—C2—C22	−52.1 (3)	C3B—Si1B—C2B—C23B	53.5 (3)
C1—Si1—C2—C22	73.4 (3)	C1B—Si1B—C2B—C23B	−71.7 (3)
O1A—Si1A—C1A—C12A	−170.3 (3)	O1C—Si1C—C1C—C11C	170.7 (3)
C3A—Si1A—C1A—C12A	77.1 (3)	C3C—Si1C—C1C—C11C	53.9 (3)
C2A—Si1A—C1A—C12A	−48.1 (3)	C2C—Si1C—C1C—C11C	−71.7 (3)
O1A—Si1A—C1A—C13A	−46.5 (3)	O1C—Si1C—C1C—C12C	−65.8 (3)
C3A—Si1A—C1A—C13A	−159.1 (3)	C3C—Si1C—C1C—C12C	177.4 (3)
C2A—Si1A—C1A—C13A	75.6 (3)	C2C—Si1C—C1C—C12C	51.8 (3)
O1A—Si1A—C1A—C11A	71.7 (3)	O1C—Si1C—C1C—C13C	52.3 (3)
C3A—Si1A—C1A—C11A	−40.9 (3)	C3C—Si1C—C1C—C13C	−64.5 (3)
C2A—Si1A—C1A—C11A	−166.1 (3)	C2C—Si1C—C1C—C13C	169.9 (2)
O1A—Si1A—C2A—C22A	−42.5 (3)	O1C—Si1C—C2C—C21C	168.8 (2)
C3A—Si1A—C2A—C22A	70.4 (3)	C3C—Si1C—C2C—C21C	−72.6 (3)
C1A—Si1A—C2A—C22A	−164.3 (3)	C1C—Si1C—C2C—C21C	52.5 (3)
O1A—Si1A—C2A—C23A	76.6 (2)	O1C—Si1C—C2C—C22C	45.9 (3)
C3A—Si1A—C2A—C23A	−170.5 (3)	C3C—Si1C—C2C—C22C	164.5 (3)
C1A—Si1A—C2A—C23A	−45.2 (3)	C1C—Si1C—C2C—C22C	−70.4 (3)
O1A—Si1A—C2A—C21A	−161.4 (2)	O1C—Si1C—C2C—C23C	−72.7 (3)
C3A—Si1A—C2A—C21A	−48.5 (3)	C3C—Si1C—C2C—C23C	46.0 (3)
C1A—Si1A—C2A—C21A	76.8 (3)	C1C—Si1C—C2C—C23C	171.1 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···Br1	0.69 (3)	2.57 (4)	3.256 (2)	174 (4)
O1A—H1A···Br1	0.69 (4)	2.57 (4)	3.257 (2)	170 (4)
O1B—H1B···Br1	0.72 (4)	2.59 (4)	3.293 (2)	163 (4)
O1C—H1C···Br1	0.73 (4)	2.54 (4)	3.263 (2)	171 (5)
O1W—H1WA···O1C	0.84	1.85	2.637 (3)	156
O1W—H1WB···O1^i	0.84	1.80	2.628 (3)	169
O1W—H1WC···O1W^i	0.84	1.60	2.437 (4)	180
O2W—H2WA···O1A	0.84	1.84	2.634 (3)	156
O2W—H2WB···O1B	0.84	1.85	2.639 (3)	155
O2W—H2WC···O2W^ii	0.84	1.60	2.442 (4)	180

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1.