Tris­(tri­phenyl­silyl)­phosphate di­chloro­methane solvate

The structure of the title monomeric phospho­silicate, C₅₄H₄₅O₄PSi₃·0.263CH₂Cl₂ or (Ph₃SiO)₃PO·0.263CH₂Cl₂, is reported and is the first of a phospho­siloxane mol­ecule with the general formula (R₃SiO)₃PO. Although the three P^V-O-Si angles are remarkably similar [143.57 (16), 144.47 (15) and 144.71 (15)°], the three P-O(Si) distances are remarkably different at 1.544 (2), 1.554 (2) and 1.561 (2) Å.

Key indicators

• Single-crystal X-ray study
• T = 294 K
• Mean [sigma](C-C) = 0.006 Å
• Disorder in solvent or counterion
• R factor = 0.059
• wR factor = 0.130
• Data-to-parameter ratio = 18.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT432_ALERT_2_A Short Inter X...Y Contact  C73    ..  C1      ..       2.85 Ang.

Author Response: Atom C73 has 0.5 occupancy (it is part of a disordered phenyl ring) and atom C1 (of a partial occupancy dichloromethane molecule) has occupancy 0.263(2). This contact between two partial occupancy atoms (occupancy sum 0.763) is thus of no significance.

Alert level B
PLAT026_ALERT_3_B Ratio Observed / Unique Reflections too Low ....         39 Perc.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..          ?
PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms .....         24
PLAT301_ALERT_3_C Main Residue  Disorder .........................      16.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      26.00 Perc.
PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          6

   1 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   6 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
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: DIFRAC with profile analysis (Gabe & White, 1993); cell refinement: DIFRAC; data reduction: DATRD2 in NRCVAX94 (Gabe et al., 1989); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) in WinGX (Version 1.70.01; Farrugia, 1999); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.

Tris(triphenylsilyl)phosphate dichloromethane solvate

Crystal data

C54H45O4PSi3·0.263CH2Cl2	Z = 2
Mr = 895.48	F(000) = 938.1
Triclinic, P1	Dx = 1.268 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.7107 Å
a = 10.284 (2) Å	Cell parameters from 25 reflections
b = 13.055 (3) Å	θ = 6.2–14.0°
c = 19.015 (4) Å	µ = 0.21 mm^−1
α = 91.75 (2)°	T = 294 K
β = 105.47 (2)°	Rectangular, colourless
γ = 106.31 (2)°	0.38 × 0.27 × 0.25 mm
V = 2346.0 (9) Å^3

Data collection

Enraf–Nonius CAD-4 diffractometer	Rint = 0.000
Radiation source: X-ray tube	θmax = 26.9°, θmin = 2.1°
Graphite monochromator	h = −13→12
ω/2θ scans	k = 0→16
10183 measured reflections	l = −24→24
10183 independent reflections	3 standard reflections every 120 min
4004 reflections with I > 2σ(I)	intensity decay: 3.8%

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)] = 0.059	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.130	H-atom parameters constrained
S = 0.86	w = 1/[σ^2(Fo^2) + (0.0501P)^2] where P = (Fo^2 + 2Fc^2)/3
10183 reflections	(Δ/σ)max = 0.004
564 parameters	Δρmax = 0.26 e Å^−3
4 restraints	Δρmin = −0.25 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.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
P1	0.25013 (9)	0.22162 (7)	0.20407 (5)	0.0355 (2)
Si1	0.37544 (10)	0.38255 (8)	0.34356 (5)	0.0389 (3)
Si2	0.35107 (10)	0.34472 (8)	0.08450 (5)	0.0391 (3)
Si3	0.36193 (9)	0.02775 (8)	0.21775 (5)	0.0427 (3)
O1	0.3275 (2)	0.32790 (17)	0.25689 (11)	0.0412 (6)
O2	0.2636 (2)	0.25299 (17)	0.12812 (11)	0.0427 (6)
O3	0.3505 (2)	0.15136 (17)	0.22721 (12)	0.0471 (6)
O4	0.1060 (2)	0.1708 (2)	0.20501 (14)	0.0590 (7)
C11	0.2222 (4)	0.4069 (3)	0.36612 (18)	0.0414 (9)
C12	0.0950 (4)	0.3268 (3)	0.3546 (2)	0.0640 (12)
H12	0.0842	0.2596	0.3319	0.077*
C13	−0.0163 (4)	0.3436 (4)	0.3759 (2)	0.0748 (14)
H13	−0.1007	0.2884	0.3671	0.090*
C14	−0.0022 (5)	0.4409 (4)	0.4097 (2)	0.0693 (13)
H14	−0.0765	0.4516	0.4251	0.083*
C15	0.1205 (5)	0.5232 (4)	0.4213 (2)	0.0661 (12)
H15	0.1293	0.5902	0.4436	0.079*
C16	0.2299 (4)	0.5059 (3)	0.39987 (19)	0.0516 (10)
H16	0.3129	0.5623	0.4080	0.062*
C21	0.5154 (4)	0.5108 (3)	0.34759 (19)	0.0413 (9)
C22	0.4906 (4)	0.5859 (3)	0.2992 (2)	0.0549 (11)
H22	0.4014	0.5735	0.2662	0.066*
C23	0.5971 (5)	0.6790 (3)	0.2997 (2)	0.0696 (13)
H23	0.5791	0.7283	0.2670	0.084*
C24	0.7284 (5)	0.6983 (4)	0.3481 (3)	0.0768 (14)
H24	0.8004	0.7599	0.3475	0.092*
C25	0.7539 (4)	0.6273 (4)	0.3974 (3)	0.0721 (13)
H25	0.8426	0.6418	0.4313	0.087*
C26	0.6488 (4)	0.5339 (3)	0.3974 (2)	0.0553 (11)
H26	0.6678	0.4860	0.4310	0.066*
C31	0.4465 (4)	0.2915 (3)	0.40531 (19)	0.0451 (9)
C32	0.5500 (4)	0.2495 (3)	0.3936 (2)	0.0655 (12)
H32	0.5834	0.2662	0.3532	0.079*
C33	0.6046 (5)	0.1833 (4)	0.4410 (3)	0.0837 (15)
H33	0.6719	0.1542	0.4315	0.100*
C34	0.5588 (6)	0.1608 (4)	0.5020 (3)	0.0920 (17)
H34	0.5960	0.1170	0.5340	0.110*
C35	0.4595 (6)	0.2020 (4)	0.5158 (3)	0.0905 (16)
H35	0.4286	0.1868	0.5571	0.109*
C36	0.4046 (4)	0.2672 (3)	0.4673 (2)	0.0633 (12)
H36	0.3370	0.2954	0.4772	0.076*
C41	0.2854 (3)	0.2855 (3)	−0.01307 (18)	0.0378 (8)
C42	0.2848 (4)	0.1825 (3)	−0.0333 (2)	0.0550 (11)
H42	0.3173	0.1419	0.0029	0.066*
C43	0.2370 (5)	0.1386 (3)	−0.1059 (2)	0.0698 (13)
H43	0.2403	0.0700	−0.1182	0.084*
C44	0.1848 (5)	0.1960 (4)	−0.1599 (2)	0.0732 (13)
H44	0.1501	0.1660	−0.2087	0.088*
C45	0.1843 (4)	0.2978 (4)	−0.1413 (2)	0.0676 (12)
H45	0.1503	0.3374	−0.1778	0.081*
C46	0.2335 (4)	0.3423 (3)	−0.0690 (2)	0.0535 (10)
H46	0.2320	0.4116	−0.0573	0.064*
C51	0.5447 (3)	0.3673 (3)	0.12188 (19)	0.0385 (9)
C52	0.6175 (4)	0.4158 (3)	0.1932 (2)	0.0528 (10)
H52	0.5677	0.4366	0.2224	0.063*
C53	0.7603 (4)	0.4337 (3)	0.2217 (2)	0.0683 (12)
H53	0.8057	0.4659	0.2697	0.082*
C54	0.8363 (4)	0.4042 (3)	0.1795 (3)	0.0654 (12)
H54	0.9329	0.4150	0.1990	0.078*
C55	0.7683 (4)	0.3585 (3)	0.1084 (3)	0.0617 (12)
H55	0.8197	0.3402	0.0791	0.074*
C56	0.6245 (4)	0.3395 (3)	0.0802 (2)	0.0513 (10)
H56	0.5798	0.3074	0.0322	0.062*
C61	0.3015 (4)	0.4691 (3)	0.09609 (18)	0.0388 (9)
C62	0.1634 (4)	0.4630 (3)	0.0928 (2)	0.0653 (12)
H62	0.0975	0.3960	0.0888	0.078*
C63	0.1212 (5)	0.5546 (4)	0.0954 (3)	0.0817 (15)
H63	0.0278	0.5490	0.0927	0.098*
C64	0.2186 (5)	0.6540 (4)	0.1021 (2)	0.0690 (13)
H64	0.1910	0.7158	0.1038	0.083*
C65	0.3559 (5)	0.6619 (3)	0.1063 (2)	0.0601 (11)
H65	0.4217	0.7292	0.1112	0.072*
C66	0.3967 (4)	0.5704 (3)	0.10317 (19)	0.0496 (10)
H66	0.4904	0.5768	0.1059	0.059*
C71	0.2619 (19)	−0.0512 (15)	0.2766 (9)	0.0525 (16)	0.50
C72	0.2384 (16)	0.0034 (8)	0.3336 (11)	0.072 (4)	0.50
H72	0.2704	0.0781	0.3410	0.087*	0.50
C73	0.1672 (14)	−0.0536 (7)	0.3797 (8)	0.093 (4)	0.50
H73	0.1515	−0.0170	0.4178	0.111*	0.50
C74	0.1194 (15)	−0.1652 (7)	0.3687 (6)	0.086 (5)	0.50
H74	0.0718	−0.2033	0.3995	0.103*	0.50
C75	0.1429 (16)	−0.2198 (9)	0.3117 (7)	0.085 (4)	0.50
H75	0.1109	−0.2944	0.3043	0.102*	0.50
C76	0.2141 (17)	−0.1628 (15)	0.2656 (7)	0.070 (4)	0.50
H76	0.2298	−0.1994	0.2275	0.084*	0.50
C711	0.2671 (19)	−0.0617 (14)	0.2742 (10)	0.0525 (16)	0.50
C721	0.1965 (17)	−0.0283 (8)	0.3191 (11)	0.072 (4)	0.50
H721	0.2009	0.0437	0.3251	0.087*	0.50
C731	0.1193 (13)	−0.1025 (7)	0.3550 (8)	0.093 (4)	0.50
H731	0.0720	−0.0802	0.3850	0.111*	0.50
C741	0.1127 (14)	−0.2101 (7)	0.3460 (7)	0.086 (5)	0.50
H741	0.0610	−0.2597	0.3700	0.103*	0.50
C751	0.1833 (15)	−0.2435 (10)	0.3011 (9)	0.085 (4)	0.50
H751	0.1789	−0.3154	0.2951	0.102*	0.50
C761	0.2605 (17)	−0.1693 (15)	0.2652 (8)	0.070 (4)	0.50
H761	0.3078	−0.1916	0.2352	0.084*	0.50
C81	0.5546 (5)	0.0427 (17)	0.2489 (12)	0.0451 (10)	0.50
C82	0.6412 (17)	0.1042 (16)	0.2110 (10)	0.046 (3)	0.50
H82	0.6037	0.1404	0.1732	0.055*	0.50
C83	0.7840 (15)	0.1116 (15)	0.2297 (12)	0.058 (2)	0.50
H83	0.8420	0.1528	0.2044	0.069*	0.50
C84	0.8402 (6)	0.0575 (17)	0.2862 (12)	0.080 (2)	0.50
H84	0.9357	0.0625	0.2987	0.096*	0.50
C85	0.7535 (16)	−0.0040 (14)	0.3241 (9)	0.069 (4)	0.50
H85	0.7911	−0.0402	0.3619	0.083*	0.50
C86	0.6107 (14)	−0.0115 (14)	0.3054 (10)	0.055 (3)	0.50
H86	0.5527	−0.0526	0.3307	0.066*	0.50
C811	0.5551 (5)	0.0443 (17)	0.2465 (12)	0.0451 (10)	0.50
C821	0.6469 (17)	0.1271 (15)	0.2233 (11)	0.046 (3)	0.50
H821	0.6137	0.1792	0.1987	0.055*	0.50
C831	0.7883 (15)	0.1319 (15)	0.2370 (12)	0.058 (2)	0.50
H831	0.8497	0.1873	0.2215	0.069*	0.50
C841	0.8379 (6)	0.0540 (17)	0.2739 (12)	0.080 (2)	0.50
H841	0.9325	0.0572	0.2830	0.096*	0.50
C851	0.7462 (16)	−0.0288 (14)	0.2971 (9)	0.069 (4)	0.50
H851	0.7794	−0.0809	0.3218	0.083*	0.50
C861	0.6047 (14)	−0.0337 (14)	0.2834 (10)	0.055 (3)	0.50
H861	0.5433	−0.0891	0.2990	0.066*	0.50
C91	0.2855 (4)	−0.0304 (3)	0.1195 (2)	0.0443 (9)
C92	0.1399 (4)	−0.0575 (3)	0.0865 (2)	0.0542 (10)
H92	0.0819	−0.0455	0.1140	0.065*
C93	0.0805 (4)	−0.1013 (3)	0.0146 (2)	0.0653 (12)
H93	−0.0170	−0.1188	−0.0058	0.078*
C94	0.1621 (5)	−0.1196 (3)	−0.0274 (2)	0.0655 (12)
H94	0.1210	−0.1484	−0.0763	0.079*
C95	0.3070 (5)	−0.0949 (3)	0.0036 (2)	0.0631 (11)
H95	0.3639	−0.1077	−0.0242	0.076*
C96	0.3665 (4)	−0.0507 (3)	0.0766 (2)	0.0545 (10)
H96	0.4638	−0.0343	0.0971	0.065*
Cl1	0.0618 (10)	0.1009 (11)	0.4839 (8)	0.127 (3)	0.263 (2)
Cl2	0.0136 (10)	−0.1147 (11)	0.5188 (8)	0.127 (3)	0.263 (2)
C1	0.128 (2)	0.0105 (19)	0.5151 (12)	0.130 (8)*	0.263 (2)
H1A	0.1891	0.0376	0.5644	0.156*	0.263 (2)
H1B	0.1877	−0.0002	0.4855	0.156*	0.263 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
P1	0.0323 (5)	0.0328 (5)	0.0409 (6)	0.0079 (4)	0.0116 (4)	0.0017 (4)
Si1	0.0394 (6)	0.0368 (6)	0.0397 (6)	0.0107 (5)	0.0110 (5)	0.0019 (5)
Si2	0.0423 (6)	0.0362 (6)	0.0413 (6)	0.0139 (5)	0.0139 (5)	0.0055 (5)
Si3	0.0410 (6)	0.0329 (6)	0.0542 (7)	0.0114 (5)	0.0127 (5)	0.0091 (5)
O1	0.0521 (15)	0.0346 (14)	0.0364 (14)	0.0122 (12)	0.0136 (12)	−0.0011 (11)
O2	0.0552 (15)	0.0365 (14)	0.0324 (14)	0.0078 (12)	0.0121 (11)	0.0033 (11)
O3	0.0520 (15)	0.0386 (15)	0.0514 (16)	0.0211 (12)	0.0082 (12)	0.0035 (12)
O4	0.0389 (15)	0.0628 (18)	0.0712 (19)	0.0052 (13)	0.0202 (13)	0.0014 (14)
C11	0.042 (2)	0.044 (2)	0.038 (2)	0.0130 (19)	0.0112 (17)	−0.0013 (18)
C12	0.048 (3)	0.065 (3)	0.074 (3)	0.011 (2)	0.019 (2)	−0.014 (2)
C13	0.045 (3)	0.099 (4)	0.080 (3)	0.018 (3)	0.023 (2)	−0.007 (3)
C14	0.063 (3)	0.108 (4)	0.056 (3)	0.054 (3)	0.020 (2)	0.005 (3)
C15	0.084 (3)	0.065 (3)	0.066 (3)	0.038 (3)	0.036 (3)	0.002 (2)
C16	0.058 (3)	0.051 (3)	0.053 (3)	0.021 (2)	0.022 (2)	0.009 (2)
C21	0.040 (2)	0.037 (2)	0.045 (2)	0.0065 (17)	0.0160 (18)	−0.0040 (18)
C22	0.054 (3)	0.047 (3)	0.056 (3)	0.011 (2)	0.008 (2)	0.001 (2)
C23	0.092 (4)	0.037 (3)	0.079 (3)	0.006 (3)	0.036 (3)	0.015 (2)
C24	0.061 (3)	0.050 (3)	0.106 (4)	−0.003 (2)	0.024 (3)	0.000 (3)
C25	0.050 (3)	0.063 (3)	0.086 (4)	0.002 (2)	0.008 (2)	−0.002 (3)
C26	0.048 (2)	0.049 (3)	0.062 (3)	0.008 (2)	0.011 (2)	0.001 (2)
C31	0.046 (2)	0.043 (2)	0.041 (2)	0.0096 (19)	0.0084 (18)	−0.0003 (18)
C32	0.063 (3)	0.078 (3)	0.062 (3)	0.036 (3)	0.011 (2)	0.011 (2)
C33	0.080 (4)	0.083 (4)	0.084 (4)	0.045 (3)	−0.002 (3)	−0.008 (3)
C34	0.104 (4)	0.075 (4)	0.082 (4)	0.036 (3)	−0.009 (3)	0.023 (3)
C35	0.115 (5)	0.093 (4)	0.064 (3)	0.036 (4)	0.017 (3)	0.033 (3)
C36	0.075 (3)	0.064 (3)	0.055 (3)	0.028 (2)	0.018 (2)	0.013 (2)
C41	0.039 (2)	0.034 (2)	0.041 (2)	0.0074 (17)	0.0155 (17)	0.0076 (17)
C42	0.080 (3)	0.045 (3)	0.046 (3)	0.028 (2)	0.018 (2)	0.012 (2)
C43	0.099 (4)	0.054 (3)	0.055 (3)	0.019 (3)	0.024 (3)	−0.008 (2)
C44	0.091 (4)	0.073 (4)	0.042 (3)	0.007 (3)	0.014 (2)	−0.001 (3)
C45	0.086 (3)	0.067 (3)	0.040 (3)	0.021 (3)	0.005 (2)	0.011 (2)
C46	0.063 (3)	0.042 (2)	0.055 (3)	0.013 (2)	0.018 (2)	0.009 (2)
C51	0.039 (2)	0.038 (2)	0.043 (2)	0.0153 (17)	0.0138 (18)	0.0075 (17)
C52	0.048 (2)	0.062 (3)	0.050 (3)	0.018 (2)	0.017 (2)	0.004 (2)
C53	0.045 (3)	0.087 (3)	0.066 (3)	0.019 (2)	0.006 (2)	−0.001 (2)
C54	0.037 (2)	0.066 (3)	0.086 (4)	0.014 (2)	0.007 (2)	0.013 (3)
C55	0.050 (3)	0.062 (3)	0.085 (3)	0.022 (2)	0.033 (2)	0.006 (2)
C56	0.050 (3)	0.047 (2)	0.058 (3)	0.016 (2)	0.015 (2)	0.004 (2)
C61	0.042 (2)	0.034 (2)	0.040 (2)	0.0134 (17)	0.0106 (17)	0.0061 (17)
C62	0.055 (3)	0.041 (3)	0.106 (4)	0.016 (2)	0.032 (3)	0.008 (2)
C63	0.067 (3)	0.068 (3)	0.130 (4)	0.038 (3)	0.042 (3)	0.013 (3)
C64	0.097 (4)	0.049 (3)	0.078 (3)	0.043 (3)	0.032 (3)	0.011 (2)
C65	0.080 (3)	0.036 (2)	0.065 (3)	0.015 (2)	0.024 (2)	0.008 (2)
C66	0.051 (2)	0.039 (2)	0.059 (3)	0.011 (2)	0.016 (2)	0.007 (2)
C71	0.046 (3)	0.048 (4)	0.058 (3)	0.011 (2)	0.008 (2)	0.015 (3)
C72	0.049 (9)	0.066 (6)	0.122 (8)	0.018 (6)	0.051 (8)	0.054 (7)
C73	0.081 (9)	0.076 (10)	0.154 (12)	0.040 (7)	0.067 (9)	0.066 (8)
C74	0.056 (4)	0.086 (10)	0.124 (9)	0.018 (6)	0.037 (6)	0.065 (9)
C75	0.078 (9)	0.054 (5)	0.102 (6)	−0.003 (5)	0.011 (5)	0.031 (5)
C76	0.067 (10)	0.059 (4)	0.069 (3)	−0.002 (6)	0.015 (5)	0.017 (3)
C711	0.046 (3)	0.048 (4)	0.058 (3)	0.011 (2)	0.008 (2)	0.015 (3)
C721	0.049 (9)	0.066 (6)	0.122 (8)	0.018 (6)	0.051 (8)	0.054 (7)
C731	0.081 (9)	0.076 (10)	0.154 (12)	0.040 (7)	0.067 (9)	0.066 (8)
C741	0.056 (4)	0.086 (10)	0.124 (9)	0.018 (6)	0.037 (6)	0.065 (9)
C751	0.078 (9)	0.054 (5)	0.102 (6)	−0.003 (5)	0.011 (5)	0.031 (5)
C761	0.067 (10)	0.059 (4)	0.069 (3)	−0.002 (6)	0.015 (5)	0.017 (3)
C81	0.043 (2)	0.032 (2)	0.061 (3)	0.0141 (18)	0.0137 (19)	0.0051 (19)
C82	0.043 (3)	0.034 (7)	0.053 (6)	0.006 (4)	0.007 (3)	−0.008 (5)
C83	0.046 (3)	0.040 (6)	0.079 (5)	−0.002 (3)	0.021 (3)	−0.012 (4)
C84	0.042 (3)	0.051 (3)	0.130 (7)	0.011 (2)	0.001 (3)	−0.020 (4)
C85	0.062 (4)	0.034 (7)	0.098 (11)	0.019 (4)	−0.001 (6)	−0.002 (6)
C86	0.049 (3)	0.030 (6)	0.080 (10)	0.012 (3)	0.010 (4)	−0.001 (6)
C811	0.043 (2)	0.032 (2)	0.061 (3)	0.0141 (18)	0.0137 (19)	0.0051 (19)
C821	0.043 (3)	0.034 (7)	0.053 (6)	0.006 (4)	0.007 (3)	−0.008 (5)
C831	0.046 (3)	0.040 (6)	0.079 (5)	−0.002 (3)	0.021 (3)	−0.012 (4)
C841	0.042 (3)	0.051 (3)	0.130 (7)	0.011 (2)	0.001 (3)	−0.020 (4)
C851	0.062 (4)	0.034 (7)	0.098 (11)	0.019 (4)	−0.001 (6)	−0.002 (6)
C861	0.049 (3)	0.030 (6)	0.080 (10)	0.012 (3)	0.010 (4)	−0.001 (6)
C91	0.041 (2)	0.031 (2)	0.061 (3)	0.0157 (18)	0.008 (2)	0.0046 (18)
C92	0.053 (3)	0.045 (2)	0.068 (3)	0.020 (2)	0.016 (2)	0.006 (2)
C93	0.055 (3)	0.058 (3)	0.067 (3)	0.012 (2)	−0.004 (2)	−0.005 (2)
C94	0.080 (3)	0.051 (3)	0.054 (3)	0.020 (3)	0.003 (3)	−0.001 (2)
C95	0.074 (3)	0.052 (3)	0.066 (3)	0.019 (2)	0.023 (3)	−0.002 (2)
C96	0.050 (2)	0.039 (2)	0.072 (3)	0.0126 (19)	0.013 (2)	0.005 (2)
Cl1	0.138 (9)	0.116 (4)	0.119 (3)	0.035 (6)	0.028 (7)	0.017 (3)
Cl2	0.138 (9)	0.116 (4)	0.119 (3)	0.035 (6)	0.028 (7)	0.017 (3)

Geometric parameters (Å, º)

P1—O1	1.561 (2)	C56—H56	0.93
P1—O2	1.544 (2)	C61—C66	1.384 (4)
P1—O3	1.554 (2)	C61—C62	1.385 (4)
P1—O4	1.449 (2)	C62—C63	1.386 (5)
Si1—O1	1.663 (2)	C62—H62	0.93
Si1—C11	1.844 (3)	C63—C64	1.377 (5)
Si1—C31	1.856 (4)	C63—H63	0.93
Si1—C21	1.860 (4)	C64—C65	1.366 (5)
Si2—O2	1.669 (2)	C64—H64	0.93
Si2—C61	1.857 (3)	C65—C66	1.379 (5)
Si2—C41	1.857 (3)	C65—H65	0.93
Si2—C51	1.860 (3)	C66—H66	0.93
Si3—O3	1.659 (2)	C71—C72	1.39
Si3—C711	1.8608 (11)	C71—C76	1.39
Si3—C71	1.8610 (11)	C72—C73	1.39
Si3—C81	1.8612 (11)	C72—H72	0.93
Si3—C811	1.8613 (11)	C73—C74	1.39
Si3—C91	1.865 (4)	C73—H73	0.93
C11—C12	1.385 (5)	C74—C75	1.39
C11—C16	1.398 (5)	C74—H74	0.93
C12—C13	1.380 (5)	C75—C76	1.39
C12—H12	0.93	C75—H75	0.93
C13—C14	1.358 (5)	C76—H76	0.93
C13—H13	0.93	C711—C721	1.39
C14—C15	1.367 (5)	C711—C761	1.39
C14—H14	0.93	C721—C731	1.39
C15—C16	1.366 (5)	C721—H721	0.93
C15—H15	0.93	C731—C741	1.39
C16—H16	0.93	C731—H731	0.93
C21—C26	1.388 (5)	C741—C751	1.39
C21—C22	1.394 (5)	C741—H741	0.93
C22—C23	1.386 (5)	C751—C761	1.39
C22—H22	0.93	C751—H751	0.93
C23—C24	1.366 (6)	C761—H761	0.93
C23—H23	0.93	C81—C82	1.39
C24—C25	1.367 (6)	C81—C86	1.39
C24—H24	0.93	C82—C83	1.39
C25—C26	1.383 (5)	C82—H82	0.93
C25—H25	0.93	C83—C84	1.39
C26—H26	0.93	C83—H83	0.93
C31—C36	1.376 (5)	C84—C85	1.39
C31—C32	1.388 (5)	C84—H84	0.93
C32—C33	1.387 (6)	C85—C86	1.39
C32—H32	0.93	C85—H85	0.93
C33—C34	1.374 (6)	C86—H86	0.93
C33—H33	0.93	C811—C821	1.39
C34—C35	1.358 (6)	C811—C861	1.39
C34—H34	0.93	C821—C831	1.39
C35—C36	1.390 (5)	C821—H821	0.93
C35—H35	0.93	C831—C841	1.39
C36—H36	0.93	C831—H831	0.93
C41—C42	1.385 (4)	C841—C851	1.39
C41—C46	1.390 (5)	C841—H841	0.93
C42—C43	1.381 (5)	C851—C861	1.39
C42—H42	0.93	C851—H851	0.93
C43—C44	1.373 (5)	C861—H861	0.93
C43—H43	0.93	C91—C96	1.380 (5)
C44—C45	1.366 (5)	C91—C92	1.395 (5)
C44—H44	0.93	C92—C93	1.373 (5)
C45—C46	1.378 (5)	C92—H92	0.93
C45—H45	0.93	C93—C94	1.362 (5)
C46—H46	0.93	C93—H93	0.93
C51—C56	1.389 (4)	C94—C95	1.386 (5)
C51—C52	1.393 (5)	C94—H94	0.93
C52—C53	1.371 (5)	C95—C96	1.390 (5)
C52—H52	0.93	C95—H95	0.93
C53—C54	1.374 (5)	C96—H96	0.93
C53—H53	0.93	Cl1—C1	1.58 (3)
C54—C55	1.373 (5)	Cl2—C1	1.74 (3)
C54—H54	0.93	C1—H1A	0.97
C55—C56	1.379 (5)	C1—H1B	0.97
C55—H55	0.93
O4—P1—O2	113.92 (14)	C54—C55—H55	119.8
O4—P1—O3	114.22 (15)	C56—C55—H55	119.8
O2—P1—O3	104.90 (13)	C55—C56—C51	121.5 (4)
O4—P1—O1	114.68 (14)	C55—C56—H56	119.3
O2—P1—O1	104.40 (12)	C51—C56—H56	119.3
O3—P1—O1	103.52 (12)	C66—C61—C62	117.5 (3)
O1—Si1—C11	109.83 (14)	C66—C61—Si2	122.1 (3)
O1—Si1—C31	109.37 (14)	C62—C61—Si2	120.2 (3)
C11—Si1—C31	110.59 (17)	C61—C62—C63	121.3 (4)
O1—Si1—C21	104.62 (14)	C61—C62—H62	119.3
C11—Si1—C21	111.28 (16)	C63—C62—H62	119.3
C31—Si1—C21	110.97 (17)	C64—C63—C62	119.5 (4)
O2—Si2—C61	107.50 (14)	C64—C63—H63	120.2
O2—Si2—C41	104.42 (13)	C62—C63—H63	120.2
C61—Si2—C41	111.07 (16)	C65—C64—C63	120.1 (4)
O2—Si2—C51	110.02 (14)	C65—C64—H64	120.0
C61—Si2—C51	112.15 (15)	C63—C64—H64	120.0
C41—Si2—C51	111.32 (16)	C64—C65—C66	120.0 (4)
O3—Si3—C711	111.7 (7)	C64—C65—H65	120.0
O3—Si3—C71	106.4 (7)	C66—C65—H65	120.0
O3—Si3—C81	105.2 (6)	C65—C66—C61	121.5 (4)
C711—Si3—C81	110.6 (10)	C65—C66—H66	119.3
C71—Si3—C81	113.2 (10)	C61—C66—H66	119.3
O3—Si3—C811	104.8 (6)	C72—C71—C76	120.0
C711—Si3—C811	112.1 (10)	C72—C71—Si3	118.7 (11)
C71—Si3—C811	114.7 (10)	C76—C71—Si3	121.3 (11)
O3—Si3—C91	110.07 (14)	C71—C72—C73	120.0
C711—Si3—C91	108.8 (7)	C71—C72—H72	120.0
C71—Si3—C91	111.2 (7)	C73—C72—H72	120.0
C81—Si3—C91	110.4 (6)	C74—C73—C72	120.0
C811—Si3—C91	109.3 (6)	C74—C73—H73	120.0
P1—O1—Si1	144.47 (15)	C72—C73—H73	120.0
P1—O2—Si2	144.71 (15)	C75—C74—C73	120.0
P1—O3—Si3	143.57 (16)	C75—C74—H74	120.0
C12—C11—C16	115.7 (3)	C73—C74—H74	120.0
C12—C11—Si1	122.3 (3)	C74—C75—C76	120.0
C16—C11—Si1	122.0 (3)	C74—C75—H75	120.0
C13—C12—C11	122.0 (4)	C76—C75—H75	120.0
C13—C12—H12	119.0	C75—C76—C71	120.0
C11—C12—H12	119.0	C75—C76—H76	120.0
C14—C13—C12	119.9 (4)	C71—C76—H76	120.0
C14—C13—H13	120.1	C721—C711—C761	120.0
C12—C13—H13	120.1	C721—C711—Si3	123.9 (11)
C13—C14—C15	120.4 (4)	C761—C711—Si3	115.9 (11)
C13—C14—H14	119.8	C731—C721—C711	120.0
C15—C14—H14	119.8	C731—C721—H721	120.0
C16—C15—C14	119.3 (4)	C711—C721—H721	120.0
C16—C15—H15	120.4	C721—C731—C741	120.0
C14—C15—H15	120.4	C721—C731—H731	120.0
C15—C16—C11	122.7 (4)	C741—C731—H731	120.0
C15—C16—H16	118.6	C751—C741—C731	120.0
C11—C16—H16	118.6	C751—C741—H741	120.0
C26—C21—C22	117.7 (3)	C731—C741—H741	120.0
C26—C21—Si1	121.4 (3)	C761—C751—C741	120.0
C22—C21—Si1	120.9 (3)	C761—C751—H751	120.0
C23—C22—C21	120.9 (4)	C741—C751—H751	120.0
C23—C22—H22	119.5	C751—C761—C711	120.0
C21—C22—H22	119.5	C751—C761—H761	120.0
C24—C23—C22	120.1 (4)	C711—C761—H761	120.0
C24—C23—H23	120.0	C82—C81—C86	120.0
C22—C23—H23	120.0	C82—C81—Si3	118.4 (13)
C23—C24—C25	120.0 (4)	C86—C81—Si3	121.5 (13)
C23—C24—H24	120.0	C81—C82—C83	120.0
C25—C24—H24	120.0	C81—C82—H82	120.0
C24—C25—C26	120.5 (4)	C83—C82—H82	120.0
C24—C25—H25	119.7	C84—C83—C82	120.0
C26—C25—H25	119.7	C84—C83—H83	120.0
C25—C26—C21	120.7 (4)	C82—C83—H83	120.0
C25—C26—H26	119.6	C83—C84—C85	120.0
C21—C26—H26	119.6	C83—C84—H84	120.0
C36—C31—C32	116.8 (4)	C85—C84—H84	120.0
C36—C31—Si1	121.3 (3)	C84—C85—C86	120.0
C32—C31—Si1	121.8 (3)	C84—C85—H85	120.0
C31—C32—C33	121.4 (4)	C86—C85—H85	120.0
C31—C32—H32	119.3	C85—C86—C81	120.0
C33—C32—H32	119.3	C85—C86—H86	120.0
C34—C33—C32	119.6 (5)	C81—C86—H86	120.0
C34—C33—H33	120.2	C821—C811—C861	120.0
C32—C33—H33	120.2	C821—C811—Si3	119.8 (13)
C35—C34—C33	120.5 (5)	C861—C811—Si3	119.7 (13)
C35—C34—H34	119.8	C831—C821—C811	120.0
C33—C34—H34	119.8	C831—C821—H821	120.0
C34—C35—C36	119.1 (5)	C811—C821—H821	120.0
C34—C35—H35	120.4	C821—C831—C841	120.0
C36—C35—H35	120.4	C821—C831—H831	120.0
C31—C36—C35	122.5 (4)	C841—C831—H831	120.0
C31—C36—H36	118.7	C851—C841—C831	120.0
C35—C36—H36	118.7	C851—C841—H841	120.0
C42—C41—C46	117.1 (3)	C831—C841—H841	120.0
C42—C41—Si2	121.5 (3)	C861—C851—C841	120.0
C46—C41—Si2	121.4 (3)	C861—C851—H851	120.0
C43—C42—C41	121.6 (4)	C841—C851—H851	120.0
C43—C42—H42	119.2	C851—C861—C811	120.0
C41—C42—H42	119.2	C851—C861—H861	120.0
C44—C43—C42	120.0 (4)	C811—C861—H861	120.0
C44—C43—H43	120.0	C96—C91—C92	116.9 (4)
C42—C43—H43	120.0	C96—C91—Si3	122.9 (3)
C45—C44—C43	119.4 (4)	C92—C91—Si3	120.1 (3)
C45—C44—H44	120.3	C93—C92—C91	121.5 (4)
C43—C44—H44	120.3	C93—C92—H92	119.3
C44—C45—C46	120.7 (4)	C91—C92—H92	119.3
C44—C45—H45	119.7	C94—C93—C92	120.9 (4)
C46—C45—H45	119.7	C94—C93—H93	119.5
C45—C46—C41	121.2 (4)	C92—C93—H93	119.5
C45—C46—H46	119.4	C93—C94—C95	119.3 (4)
C41—C46—H46	119.4	C93—C94—H94	120.3
C56—C51—C52	116.6 (3)	C95—C94—H94	120.3
C56—C51—Si2	122.3 (3)	C94—C95—C96	119.4 (4)
C52—C51—Si2	121.1 (3)	C94—C95—H95	120.3
C53—C52—C51	122.0 (4)	C96—C95—H95	120.3
C53—C52—H52	119.0	C91—C96—C95	121.9 (4)
C51—C52—H52	119.0	C91—C96—H96	119.0
C52—C53—C54	120.1 (4)	C95—C96—H96	119.0
C52—C53—H53	120.0	Cl1—C1—Cl2	118.2 (14)
C54—C53—H53	120.0	Cl1—C1—H1A	107.8
C55—C54—C53	119.4 (4)	Cl2—C1—H1A	107.8
C55—C54—H54	120.3	Cl1—C1—H1B	107.8
C53—C54—H54	120.3	Cl2—C1—H1B	107.8
C54—C55—C56	120.4 (4)	H1A—C1—H1B	107.1
O4—P1—O1—Si1	55.8 (3)	C52—C53—C54—C55	1.2 (6)
O2—P1—O1—Si1	−178.9 (2)	C53—C54—C55—C56	−1.9 (6)
O3—P1—O1—Si1	−69.3 (3)	C54—C55—C56—C51	1.1 (6)
C11—Si1—O1—P1	−77.8 (3)	C52—C51—C56—C55	0.4 (5)
C31—Si1—O1—P1	43.7 (3)	Si2—C51—C56—C55	178.9 (3)
C21—Si1—O1—P1	162.6 (3)	O2—Si2—C61—C66	145.2 (3)
O4—P1—O2—Si2	143.5 (3)	C41—Si2—C61—C66	−101.1 (3)
O3—P1—O2—Si2	−90.9 (3)	C51—Si2—C61—C66	24.2 (3)
O1—P1—O2—Si2	17.6 (3)	O2—Si2—C61—C62	−39.3 (3)
C61—Si2—O2—P1	−69.0 (3)	C41—Si2—C61—C62	74.4 (3)
C41—Si2—O2—P1	173.0 (3)	C51—Si2—C61—C62	−160.3 (3)
C51—Si2—O2—P1	53.4 (3)	C66—C61—C62—C63	0.9 (6)
O4—P1—O3—Si3	42.3 (3)	Si2—C61—C62—C63	−174.8 (3)
O2—P1—O3—Si3	−83.1 (3)	C61—C62—C63—C64	−0.6 (7)
O1—P1—O3—Si3	167.7 (2)	C62—C63—C64—C65	−0.1 (7)
C711—Si3—O3—P1	−76.6 (7)	C63—C64—C65—C66	0.5 (7)
C71—Si3—O3—P1	−76.3 (7)	C64—C65—C66—C61	−0.2 (6)
C81—Si3—O3—P1	163.3 (8)	C62—C61—C66—C65	−0.5 (5)
C811—Si3—O3—P1	161.8 (8)	Si2—C61—C66—C65	175.1 (3)
C91—Si3—O3—P1	44.4 (3)	O3—Si3—C71—C72	−21.1 (10)
O1—Si1—C11—C12	53.1 (3)	C711—Si3—C71—C72	155 (15)
C31—Si1—C11—C12	−67.7 (3)	C81—Si3—C71—C72	94.0 (11)
C21—Si1—C11—C12	168.5 (3)	C811—Si3—C71—C72	94.3 (11)
O1—Si1—C11—C16	−130.6 (3)	C91—Si3—C71—C72	−141.0 (7)
C31—Si1—C11—C16	108.5 (3)	O3—Si3—C71—C76	160.6 (8)
C21—Si1—C11—C16	−15.3 (3)	C711—Si3—C71—C76	−23 (13)
C16—C11—C12—C13	−0.7 (6)	C81—Si3—C71—C76	−84.3 (11)
Si1—C11—C12—C13	175.8 (3)	C811—Si3—C71—C76	−84.1 (12)
C11—C12—C13—C14	−0.5 (7)	C91—Si3—C71—C76	40.7 (10)
C12—C13—C14—C15	1.5 (7)	Si3—C71—C72—C73	−178.4 (14)
C13—C14—C15—C16	−1.3 (6)	Si3—C71—C76—C75	178.3 (14)
C14—C15—C16—C11	0.1 (6)	O3—Si3—C711—C721	−0.5 (11)
C12—C11—C16—C15	0.9 (5)	C71—Si3—C711—C721	−4 (13)
Si1—C11—C16—C15	−175.6 (3)	C81—Si3—C711—C721	116.4 (10)
O1—Si1—C21—C26	−124.0 (3)	C811—Si3—C711—C721	116.8 (10)
C11—Si1—C21—C26	117.5 (3)	C91—Si3—C711—C721	−122.2 (8)
C31—Si1—C21—C26	−6.2 (3)	O3—Si3—C711—C761	174.8 (7)
O1—Si1—C21—C22	54.3 (3)	C71—Si3—C711—C761	171 (15)
C11—Si1—C21—C22	−64.3 (3)	C81—Si3—C711—C761	−68.4 (11)
C31—Si1—C21—C22	172.1 (3)	C811—Si3—C711—C761	−68.0 (11)
C26—C21—C22—C23	1.7 (5)	C91—Si3—C711—C761	53.1 (9)
Si1—C21—C22—C23	−176.7 (3)	Si3—C711—C721—C731	175.0 (14)
C21—C22—C23—C24	−0.1 (6)	Si3—C711—C761—C751	−175.4 (13)
C22—C23—C24—C25	−1.7 (7)	O3—Si3—C81—C82	−61.3 (7)
C23—C24—C25—C26	2.0 (7)	C711—Si3—C81—C82	177.9 (9)
C24—C25—C26—C21	−0.4 (6)	C71—Si3—C81—C82	−177.2 (9)
C22—C21—C26—C25	−1.4 (5)	C811—Si3—C81—C82	11 (41)
Si1—C21—C26—C25	176.9 (3)	C91—Si3—C81—C82	57.4 (8)
O1—Si1—C31—C36	−133.3 (3)	O3—Si3—C81—C86	122.8 (7)
C11—Si1—C31—C36	−12.2 (4)	C711—Si3—C81—C86	2.0 (11)
C21—Si1—C31—C36	111.8 (3)	C71—Si3—C81—C86	6.9 (12)
O1—Si1—C31—C32	50.4 (3)	C811—Si3—C81—C86	−165 (42)
C11—Si1—C31—C32	171.5 (3)	C91—Si3—C81—C86	−118.5 (7)
C21—Si1—C31—C32	−64.5 (3)	Si3—C81—C82—C83	−176.0 (11)
C36—C31—C32—C33	2.2 (6)	Si3—C81—C86—C85	175.8 (11)
Si1—C31—C32—C33	178.6 (3)	O3—Si3—C811—C821	−43.2 (8)
C31—C32—C33—C34	−1.9 (7)	C711—Si3—C811—C821	−164.4 (9)
C32—C33—C34—C35	0.7 (8)	C71—Si3—C811—C821	−159.5 (9)
C33—C34—C35—C36	0.1 (8)	C81—Si3—C811—C821	−151 (42)
C32—C31—C36—C35	−1.4 (6)	C91—Si3—C811—C821	74.8 (8)
Si1—C31—C36—C35	−177.9 (3)	O3—Si3—C811—C861	144.7 (6)
C34—C35—C36—C31	0.3 (7)	C711—Si3—C811—C861	23.5 (12)
O2—Si2—C41—C42	−51.6 (3)	C71—Si3—C811—C861	28.4 (12)
C61—Si2—C41—C42	−167.2 (3)	C81—Si3—C811—C861	37 (41)
C51—Si2—C41—C42	67.1 (3)	C91—Si3—C811—C861	−97.3 (8)
O2—Si2—C41—C46	127.8 (3)	Si3—C811—C821—C831	−172.1 (12)
C61—Si2—C41—C46	12.2 (3)	Si3—C811—C861—C851	172.1 (12)
C51—Si2—C41—C46	−113.6 (3)	O3—Si3—C91—C96	111.3 (3)
C46—C41—C42—C43	1.1 (6)	C711—Si3—C91—C96	−126.0 (7)
Si2—C41—C42—C43	−179.5 (3)	C71—Si3—C91—C96	−131.0 (8)
C41—C42—C43—C44	−1.9 (6)	C81—Si3—C91—C96	−4.4 (9)
C42—C43—C44—C45	1.8 (7)	C811—Si3—C91—C96	−3.3 (9)
C43—C44—C45—C46	−1.0 (7)	O3—Si3—C91—C92	−70.0 (3)
C44—C45—C46—C41	0.2 (6)	C711—Si3—C91—C92	52.7 (7)
C42—C41—C46—C45	−0.3 (5)	C71—Si3—C91—C92	47.8 (8)
Si2—C41—C46—C45	−179.7 (3)	C81—Si3—C91—C92	174.3 (9)
O2—Si2—C51—C56	113.9 (3)	C811—Si3—C91—C92	175.5 (8)
C61—Si2—C51—C56	−126.5 (3)	C96—C91—C92—C93	−0.6 (5)
C41—Si2—C51—C56	−1.4 (3)	Si3—C91—C92—C93	−179.4 (3)
O2—Si2—C51—C52	−67.7 (3)	C91—C92—C93—C94	−0.3 (6)
C61—Si2—C51—C52	51.9 (3)	C92—C93—C94—C95	0.9 (6)
C41—Si2—C51—C52	177.0 (3)	C93—C94—C95—C96	−0.8 (6)
C56—C51—C52—C53	−1.1 (6)	C92—C91—C96—C95	0.7 (5)
Si2—C51—C52—C53	−179.6 (3)	Si3—C91—C96—C95	179.5 (3)
C51—C52—C53—C54	0.3 (6)	C94—C95—C96—C91	−0.1 (6)