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In the structure of the centrosymmetric title compound, C30H66O6Si6·2CH3OH, OSiMe3 groups are located above and below the plane defined by the central benzene ring in an alternating fashion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807017047/sg2156sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807017047/sg2156Isup2.hkl
Contains datablock I

CCDC reference: 647325

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in main residue
  • R factor = 0.057
  • wR factor = 0.213
  • Data-to-parameter ratio = 22.4

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT415_ALERT_2_B Short Inter D-H..H-X H4 .. H15C .. 2.04 Ang.
Alert level C DIFMN02_ALERT_2_C The minimum difference density is < -0.1*ZMAX*0.75 _refine_diff_density_min given = -1.062 Test value = -1.050 DIFMN03_ALERT_1_C The minimum difference density is < -0.1*ZMAX*0.75 The relevant atom site should be identified. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT098_ALERT_2_C Minimum (Negative) Residual Density ............ -1.06 e/A    PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 2 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.19 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.11 Ratio 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 Si2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Si3 PLAT301_ALERT_3_C Main Residue Disorder ......................... 8.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT410_ALERT_2_C Short Intra H...H Contact H4'2 .. H5B .. 1.98 Ang. PLAT415_ALERT_2_C Short Inter D-H..H-X H7A .. H4' .. 2.13 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H4' .. O1' .. 2.73 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 19.60 Deg. O1 -SI1 -O1' 1.555 1.555 1.555
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C32 H74 O8 Si6 Atom count from _chemical_formula_moiety:C32 H74 O10 Si6 REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 31.92 From the CIF: _reflns_number_total 5117 From the CIF: _diffrn_reflns_limit_ max hkl 12. 13. 15. From the CIF: _diffrn_reflns_limit_ min hkl -13. -7. -16. TEST1: Expected hkl limits for theta max Calculated maximum hkl 14. 15. 18. Calculated minimum hkl -14. -15. -18.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 17 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: STADI4 (Stoe & Cie, 1995); cell refinement: STADI4; data reduction: STADI4; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Hexakis(trimethylsiloxymethyl)benzene methanol disolvate top
Crystal data top
C30H66O6Si6·2CH4OZ = 1
Mr = 755.45F(000) = 414
Triclinic, P1Dx = 1.081 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.7075 (19) ÅCell parameters from 2000 reflections
b = 10.153 (2) Åθ = 5–50°
c = 12.227 (2) ŵ = 0.22 mm1
α = 101.34 (3)°T = 173 K
β = 97.61 (4)°Block, colourless
γ = 96.04 (3)°0.30 × 0.30 × 0.20 mm
V = 1160.4 (4) Å3
Data collection top
Stoe Stadi-4
diffractometer
3168 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.039
Graphite monochromatorθmax = 31.9°, θmin = 3.6°
Detector resolution: 6.67 pixels mm-1h = 1312
rotation scansk = 713
9084 measured reflectionsl = 1615
5117 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.213H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.1223P)2]
where P = (Fo2 + 2Fc2)/3
5117 reflections(Δ/σ)max < 0.001
228 parametersΔρmax = 0.77 e Å3
1 restraintΔρmin = 1.06 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Si10.90880 (9)0.31022 (9)0.29937 (7)0.0341 (3)
Si20.33061 (10)0.27694 (9)0.06752 (7)0.0356 (3)
Si30.26566 (10)0.86762 (9)0.31390 (8)0.0360 (3)
C10.5779 (3)0.4086 (3)0.4422 (2)0.0239 (6)
C20.4839 (3)0.4733 (3)0.3816 (2)0.0235 (6)
C30.4052 (3)0.5642 (3)0.4391 (2)0.0229 (6)
C50.4705 (3)0.4483 (3)0.2546 (2)0.0292 (6)
H5A0.44720.53080.22850.035*
H5B0.56080.42700.23090.035*
C60.2986 (3)0.6286 (3)0.3736 (3)0.0305 (7)
H6A0.26480.56930.29820.037*
H6B0.21720.63990.41380.037*
C70.9483 (5)0.4172 (5)0.1970 (4)0.0708 (13)
H7A0.95660.51310.23390.106*
H7B0.87230.39660.13230.106*
H7C1.03670.39800.17070.106*
C80.8447 (4)0.1313 (4)0.2281 (4)0.0588 (11)
H8A0.81450.08110.28340.088*
H8B0.92040.09010.19450.088*
H8C0.76530.12830.16860.088*
C91.0670 (4)0.3188 (4)0.4023 (3)0.0512 (9)
H9A1.05070.25270.44940.077*
H9B1.08890.41020.45020.077*
H9C1.14570.29810.36230.077*
C100.2869 (6)0.4140 (5)0.0054 (3)0.0690 (13)
H10A0.36160.49120.01900.104*
H10B0.19810.44260.01340.104*
H10C0.27780.38060.08720.104*
C110.4854 (5)0.2047 (4)0.0192 (3)0.0610 (11)
H11A0.56680.27540.03790.092*
H11B0.46590.17000.06280.092*
H11C0.50530.13050.05690.092*
C120.1787 (5)0.1428 (4)0.0464 (3)0.0616 (11)
H12A0.09820.18320.07230.092*
H12B0.20280.07470.08970.092*
H12C0.15480.09980.03400.092*
C130.1785 (5)0.7904 (4)0.1665 (3)0.0676 (13)
H13A0.24960.76280.11990.101*
H13B0.12820.85690.13540.101*
H13C0.11210.71080.16670.101*
C140.1326 (5)0.9085 (5)0.4081 (4)0.0730 (14)
H14A0.17990.94060.48630.109*
H14B0.06620.82690.40280.109*
H14C0.08190.97940.38470.109*
C150.3936 (4)1.0176 (4)0.3196 (4)0.0581 (11)
H15A0.44011.05300.39770.087*
H15B0.34491.08770.29260.087*
H15C0.46380.99190.27160.087*
O10.7812 (12)0.3839 (10)0.3462 (7)0.0328 (18)0.50
C40.6588 (3)0.3062 (3)0.3804 (3)0.0301 (6)0.50
H4A0.69270.24660.43030.036*0.50
H4B0.59790.24910.31280.036*0.50
O1'0.7948 (12)0.3646 (11)0.3863 (7)0.042 (2)0.50
C4'0.6588 (3)0.3062 (3)0.3804 (3)0.0301 (6)0.50
H4'10.65800.22590.41510.036*0.50
H4'20.61420.27600.30040.036*0.50
O20.3628 (2)0.3377 (2)0.20517 (15)0.0328 (5)
O30.3611 (2)0.7584 (2)0.36112 (18)0.0351 (5)
O40.6205 (5)0.7826 (5)0.2746 (4)0.0869 (14)*0.75
H40.59350.85440.30620.130*0.75
C160.7329 (9)0.7585 (8)0.3389 (7)0.064 (2)*0.75
H16A0.81800.79470.31370.096*0.75
H16B0.73050.66060.33260.096*0.75
H16C0.73290.80260.41780.096*0.75
O4'0.7951 (13)0.6648 (13)0.3058 (10)0.064 (3)*0.25
H4'0.83780.62060.34750.096*0.25
C16'0.720 (3)0.752 (2)0.3694 (19)0.064 (6)*0.25
H16D0.73090.73840.44710.097*0.25
H16E0.62050.73310.33630.097*0.25
H16F0.75560.84610.36960.097*0.25
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.0303 (5)0.0317 (5)0.0390 (5)0.0050 (4)0.0113 (4)0.0001 (4)
Si20.0491 (6)0.0330 (5)0.0214 (4)0.0060 (4)0.0012 (4)0.0006 (3)
Si30.0363 (5)0.0276 (5)0.0470 (5)0.0039 (4)0.0032 (4)0.0172 (4)
C10.0245 (14)0.0173 (13)0.0287 (14)0.0007 (11)0.0072 (11)0.0011 (11)
C20.0256 (14)0.0206 (13)0.0218 (12)0.0031 (11)0.0032 (10)0.0023 (10)
C30.0233 (14)0.0181 (13)0.0257 (13)0.0003 (11)0.0007 (10)0.0047 (11)
C50.0379 (17)0.0256 (14)0.0220 (13)0.0020 (13)0.0055 (11)0.0026 (11)
C60.0307 (16)0.0220 (14)0.0377 (16)0.0001 (12)0.0012 (12)0.0100 (12)
C70.083 (3)0.074 (3)0.065 (3)0.021 (3)0.008 (2)0.033 (2)
C80.052 (2)0.045 (2)0.068 (3)0.0072 (18)0.016 (2)0.0216 (19)
C90.051 (2)0.049 (2)0.054 (2)0.0052 (18)0.0004 (17)0.0176 (18)
C100.104 (4)0.067 (3)0.041 (2)0.024 (3)0.002 (2)0.023 (2)
C110.069 (3)0.061 (3)0.052 (2)0.018 (2)0.017 (2)0.003 (2)
C120.066 (3)0.054 (2)0.047 (2)0.010 (2)0.0062 (19)0.0154 (18)
C130.085 (3)0.053 (2)0.059 (2)0.004 (2)0.016 (2)0.023 (2)
C140.066 (3)0.059 (3)0.111 (4)0.029 (2)0.040 (3)0.030 (3)
C150.060 (3)0.039 (2)0.077 (3)0.0061 (19)0.002 (2)0.026 (2)
O10.035 (3)0.020 (3)0.047 (5)0.003 (2)0.028 (4)0.005 (3)
C40.0291 (16)0.0213 (14)0.0383 (16)0.0022 (12)0.0111 (12)0.0010 (12)
O1'0.038 (4)0.034 (5)0.051 (5)0.008 (3)0.030 (4)0.008 (4)
C4'0.0291 (16)0.0213 (14)0.0383 (16)0.0022 (12)0.0111 (12)0.0010 (12)
O20.0431 (13)0.0298 (11)0.0204 (9)0.0056 (10)0.0015 (8)0.0011 (8)
O30.0305 (12)0.0278 (11)0.0490 (13)0.0024 (9)0.0025 (9)0.0166 (10)
Geometric parameters (Å, º) top
Si1—O11.624 (11)C9—H9B0.9800
Si1—O1'1.694 (11)C9—H9C0.9800
Si1—C91.835 (4)C10—H10A0.9800
Si1—C81.855 (4)C10—H10B0.9800
Si1—C71.862 (4)C10—H10C0.9800
Si2—O21.650 (2)C11—H11A0.9800
Si2—C101.850 (4)C11—H11B0.9800
Si2—C121.853 (4)C11—H11C0.9800
Si2—C111.855 (4)C12—H12A0.9800
Si3—O31.658 (2)C12—H12B0.9800
Si3—C151.845 (4)C12—H12C0.9800
Si3—C131.865 (4)C13—H13A0.9800
Si3—C141.867 (4)C13—H13B0.9800
C1—C21.397 (4)C13—H13C0.9800
C1—C3i1.406 (4)C14—H14A0.9800
C1—C41.513 (4)C14—H14B0.9800
C2—C31.402 (4)C14—H14C0.9800
C2—C51.510 (4)C15—H15A0.9800
C3—C1i1.406 (4)C15—H15B0.9800
C3—C61.507 (4)C15—H15C0.9800
C5—O21.428 (3)O1—C41.507 (10)
C5—H5A0.9900C4—H4A0.9900
C5—H5B0.9900C4—H4B0.9900
C6—O31.436 (3)O4—C161.332 (9)
C6—H6A0.9900O4—H40.8400
C6—H6B0.9900C16—H16A0.9800
C7—H7A0.9800C16—H16B0.9800
C7—H7B0.9800C16—H16C0.9800
C7—H7C0.9800O4'—C16'1.391 (18)
C8—H8A0.9800O4'—H4'0.8400
C8—H8B0.9800C16'—H16D0.9800
C8—H8C0.9800C16'—H16E0.9800
C9—H9A0.9800C16'—H16F0.9800
O1—Si1—O1'19.6 (4)H9A—C9—H9B109.5
O1—Si1—C9116.5 (3)Si1—C9—H9C109.5
O1'—Si1—C9100.7 (4)H9A—C9—H9C109.5
O1—Si1—C8110.1 (4)H9B—C9—H9C109.5
O1'—Si1—C8108.2 (4)Si2—C10—H10A109.5
C9—Si1—C8110.0 (2)Si2—C10—H10B109.5
O1—Si1—C798.4 (3)H10A—C10—H10B109.5
O1'—Si1—C7116.0 (3)Si2—C10—H10C109.5
C9—Si1—C7109.3 (2)H10A—C10—H10C109.5
C8—Si1—C7112.0 (2)H10B—C10—H10C109.5
O2—Si2—C10109.40 (16)Si2—C11—H11A109.5
O2—Si2—C12104.65 (15)Si2—C11—H11B109.5
C10—Si2—C12111.2 (2)H11A—C11—H11B109.5
O2—Si2—C11110.01 (17)Si2—C11—H11C109.5
C10—Si2—C11110.6 (2)H11A—C11—H11C109.5
C12—Si2—C11110.8 (2)H11B—C11—H11C109.5
O3—Si3—C15104.43 (16)Si2—C12—H12A109.5
O3—Si3—C13108.77 (17)Si2—C12—H12B109.5
C15—Si3—C13111.79 (19)H12A—C12—H12B109.5
O3—Si3—C14109.25 (17)Si2—C12—H12C109.5
C15—Si3—C14111.6 (2)H12A—C12—H12C109.5
C13—Si3—C14110.7 (2)H12B—C12—H12C109.5
C2—C1—C3i120.0 (2)Si3—C13—H13A109.5
C2—C1—C4120.2 (2)Si3—C13—H13B109.5
C3i—C1—C4119.8 (3)H13A—C13—H13B109.5
C1—C2—C3119.9 (2)Si3—C13—H13C109.5
C1—C2—C5119.9 (3)H13A—C13—H13C109.5
C3—C2—C5120.1 (2)H13B—C13—H13C109.5
C2—C3—C1i120.0 (2)Si3—C14—H14A109.5
C2—C3—C6119.9 (2)Si3—C14—H14B109.5
C1i—C3—C6120.0 (3)H14A—C14—H14B109.5
O2—C5—C2109.4 (2)Si3—C14—H14C109.5
O2—C5—H5A109.8H14A—C14—H14C109.5
C2—C5—H5A109.8H14B—C14—H14C109.5
O2—C5—H5B109.8Si3—C15—H15A109.5
C2—C5—H5B109.8Si3—C15—H15B109.5
H5A—C5—H5B108.2H15A—C15—H15B109.5
O3—C6—C3109.7 (2)Si3—C15—H15C109.5
O3—C6—H6A109.7H15A—C15—H15C109.5
C3—C6—H6A109.7H15B—C15—H15C109.5
O3—C6—H6B109.7C4—O1—Si1122.0 (6)
C3—C6—H6B109.7O1—C4—C1107.6 (5)
H6A—C6—H6B108.2O1—C4—H4A110.2
Si1—C7—H7A109.5C1—C4—H4A110.2
Si1—C7—H7B109.5O1—C4—H4B110.2
H7A—C7—H7B109.5C1—C4—H4B110.2
Si1—C7—H7C109.5H4A—C4—H4B108.5
H7A—C7—H7C109.5C5—O2—Si2121.41 (17)
H7B—C7—H7C109.5C6—O3—Si3121.81 (19)
Si1—C8—H8A109.5C16'—O4'—H4'109.5
Si1—C8—H8B109.5O4'—C16'—H16D109.5
H8A—C8—H8B109.5O4'—C16'—H16E109.5
Si1—C8—H8C109.5H16D—C16'—H16E109.5
H8A—C8—H8C109.5O4'—C16'—H16F109.5
H8B—C8—H8C109.5H16D—C16'—H16F109.5
Si1—C9—H9A109.5H16E—C16'—H16F109.5
Si1—C9—H9B109.5
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4···O10.842.412.981 (15)126
O4—H4···O10.842.733.382 (15)135
O4—H4···O30.842.592.863 (6)101
 

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