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A twofold rotation axis passes through the bridging O atom between the two sugar rings in the title compound, C62H62O17. Otherwise the geometry is much as would be expected for this type of mol­ecule. Neither solvent nor hydrogen bonds are present in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802005408/cf6162sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802005408/cf6162Isup2.hkl
Contains datablock I

CCDC reference: 185766

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.043
  • wR factor = 0.101
  • Data-to-parameter ratio = 8.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes

REFLT_03 From the CIF: _diffrn_reflns_theta_max 26.37 From the CIF: _reflns_number_total 3235 Count of symmetry unique reflns 3244 Completeness (_total/calc) 99.72% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present no Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.

Comment top

Trehalose continues to attract much attention due to its role in bio-protection (Sussich et al., 2001) and in certain drug formulations (Hatley & Blair, 1999). A crystal to glass transition by milling has also been observed for this non-reducing disaccharide (Willart et al., 2001). In search of materials with useful solid-state properties, a number of derivatives of trehalose have been prepared (Clow et al., 2001; Baddeley et al., 2001) and in this context the ditrityl hexaacetyl derivative of trehalose, (I), is now reported.

The molecule contains a twofold rotation axis with the bridging O atom (O1) in the special position (1/2,1,z). Hence, the geometry in Table 1 applies equally to both sugar rings in the molecule. No water is present in the crystal structure, which contains a maximum potential solvent volume of 32.7 Å3 compared to an expected volume of 40 Å3 for a hydrogen-bonded water molecule (Spek, 2001). No hydrogen bonds are present. The substitution at C1,C1' is α,α, with C1—O1 = 1.417 (3) Å and the angle subtended at O1 = 113.4 (2)°. The absolute configuration adopted in this refinement (see below) is R at C1, C2, C4 and C5, and S at C3. The sugar ring adopts a chair conformation with puckering parameters (Cremer & Pople, 1975) calculated with PLATON (Spek, 2001) of Q = 0.592 (2) Å, θ = 4.5 (2)° and ϕ = 246 (2)°.

Experimental top

The title compound was prepared by reacting anhydrous α,α-trehalose with trityl chloride in pyridine, followed by excess acetic anhydride after 30 min. The mixture was left stirring for 4 h, then evaporated to an oil and plunged into water. The precipitate was stirred in hot methanol and filtered when cool. Recrystallization of the product to form suitable crystals was from an ethyl acetate/methanol mixture, by slow evaporation.

Refinement top

The H atoms were initially placed in calculated positions and thereafter allowed to ride on their parent atoms, with common isotropic displacement parameters that converged at 0.049 (2) (non- methyl H atoms) and 0.096 (5) Å2 (methyl H atoms). The methyl H atoms attached to C12 were disordered into two distinct groups with occupations factors that refined to 0.33 (4) and 0.67 (4), respectively. In the absence of elements heavier than oxygen, Friedel pairs were merged prior to refinement. As a consequence, the Flack (1983) x parameter and absolute configuration are indeterminate from the intensity data alone. The latter has therefore been established simply on the basis of the known stereochemistry of the parent trehalose.

Computing details top

Data collection: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998); cell refinement: DENZO and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997).

Figures top
[Figure 1] Fig. 1. The atomic arrangement in the title molecule. Displacement ellipsoids are shown at the 50% probability level.
2,3,4-tri-O-acetyl-6-O-trityl-1-O-(2,3,4-tri-O-acetyl-6-O-tritylα-D– glucopyranosyl)-α-D-glucopyranose top
Crystal data top
C62H62O17Dx = 1.276 Mg m3
Mr = 1079.12Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 5000 reflections
a = 15.0595 (4) Åθ = 1.8–26.4°
b = 17.1977 (6) ŵ = 0.09 mm1
c = 10.8465 (4) ÅT = 150 K
V = 2809.12 (16) Å3Prism, colourless
Z = 20.50 × 0.30 × 0.20 mm
F(000) = 1140
Data collection top
Enraf Nonius KappaCCD area-detector
diffractometer
3235 independent reflections
Radiation source: Enraf-Nonius FR591 rotating anode2333 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.078
Detector resolution: 9.091 pixels mm-1θmax = 26.4°, θmin = 1.8°
ϕ and ω scansh = 1818
Absorption correction: multi-scan
(SORTAV; Blessing, 1995, 1997)
k = 2121
Tmin = 0.955, Tmax = 0.982l = 1313
16774 measured 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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.101H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0568P)2]
where P = (Fo2 + 2Fc2)/3
3235 reflections(Δ/σ)max < 0.001
363 parametersΔρmax = 0.21 e Å3
0 restraintsΔρmin = 0.25 e Å3
Crystal data top
C62H62O17V = 2809.12 (16) Å3
Mr = 1079.12Z = 2
Orthorhombic, P21212Mo Kα radiation
a = 15.0595 (4) ŵ = 0.09 mm1
b = 17.1977 (6) ÅT = 150 K
c = 10.8465 (4) Å0.50 × 0.30 × 0.20 mm
Data collection top
Enraf Nonius KappaCCD area-detector
diffractometer
3235 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1995, 1997)
2333 reflections with I > 2σ(I)
Tmin = 0.955, Tmax = 0.982Rint = 0.078
16774 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.101H-atom parameters constrained
S = 1.00Δρmax = 0.21 e Å3
3235 reflectionsΔρmin = 0.25 e Å3
363 parameters
Special details top

Experimental. Please note cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range.

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)
O10.50001.00000.8011 (2)0.0259 (6)
O20.33569 (10)0.98239 (10)0.88892 (17)0.0321 (5)
O30.20150 (13)0.92560 (11)0.8817 (2)0.0458 (5)
O40.35539 (11)0.81530 (10)0.96958 (17)0.0333 (5)
O50.48244 (11)0.90000 (9)0.65828 (16)0.0281 (4)
O60.36533 (15)0.89970 (13)1.1280 (2)0.0527 (6)
O70.51108 (12)0.74591 (10)0.88536 (18)0.0349 (5)
O80.41558 (15)0.65155 (12)0.8283 (2)0.0529 (6)
O90.51307 (11)0.74806 (10)0.57844 (17)0.0306 (4)
C10.43883 (16)0.95672 (14)0.7293 (3)0.0275 (6)
H10.40640.99300.67300.0493 (19)*
C20.37292 (16)0.92010 (14)0.8175 (3)0.0266 (6)
H20.32460.89450.76910.0493 (19)*
C30.41827 (16)0.85968 (14)0.8983 (3)0.0280 (6)
H30.46290.88500.95360.0493 (19)*
C40.46345 (16)0.80181 (14)0.8129 (2)0.0291 (6)
H40.41810.77490.76070.0493 (19)*
C50.53040 (16)0.84374 (14)0.7314 (3)0.0282 (6)
H50.57480.87120.78430.0493 (19)*
C60.57796 (17)0.79057 (15)0.6430 (3)0.0321 (7)
H6A0.61440.82130.58480.0493 (19)*
H6B0.61760.75480.68870.0493 (19)*
C70.24836 (17)0.97687 (16)0.9191 (3)0.0357 (7)
C80.2205 (2)1.04135 (19)1.0009 (4)0.0587 (10)
H8A0.15581.04041.01050.097 (5)*
H8B0.23851.09110.96450.097 (5)*
H8C0.24871.03531.08180.097 (5)*
C90.33984 (19)0.83878 (18)1.0864 (3)0.0395 (7)
C100.2863 (2)0.7796 (2)1.1545 (3)0.0594 (10)
H10A0.32610.74111.19160.097 (5)*
H10B0.24580.75351.09700.097 (5)*
H10C0.25190.80531.21940.097 (5)*
C110.4794 (2)0.67099 (16)0.8839 (3)0.0415 (7)
C120.5378 (2)0.62098 (19)0.9610 (4)0.0698 (12)
H12A0.58570.65250.99610.097 (5)*0.34 (4)
H12B0.56330.57960.90990.097 (5)*0.34 (4)
H12C0.50290.59781.02780.097 (5)*0.34 (4)
H12D0.51550.56740.95970.097 (5)*0.66 (4)
H12E0.53800.64041.04590.097 (5)*0.66 (4)
H12F0.59840.62220.92800.097 (5)*0.66 (4)
C130.54362 (16)0.70324 (15)0.4741 (3)0.0326 (6)
C140.46089 (17)0.65837 (15)0.4324 (3)0.0340 (7)
C150.37963 (17)0.66718 (17)0.4898 (3)0.0433 (8)
H150.37390.70230.55690.0493 (19)*
C160.3064 (2)0.62515 (19)0.4504 (4)0.0517 (9)
H160.25090.63170.49070.0493 (19)*
C170.3134 (2)0.57462 (18)0.3543 (4)0.0527 (9)
H170.26290.54630.32720.0493 (19)*
C180.3937 (2)0.5649 (2)0.2970 (4)0.0622 (10)
H180.39920.52930.23040.0493 (19)*
C190.4663 (2)0.60666 (19)0.3358 (3)0.0538 (9)
H190.52160.59970.29510.0493 (19)*
C200.56998 (18)0.75812 (17)0.3686 (3)0.0404 (7)
C210.53403 (19)0.83244 (18)0.3648 (3)0.0457 (8)
H210.49730.84990.43040.0493 (19)*
C220.5511 (3)0.8812 (2)0.2666 (4)0.0683 (11)
H220.52670.93210.26590.0493 (19)*
C230.6021 (3)0.8572 (4)0.1714 (5)0.0890 (15)
H230.61220.89070.10310.0493 (19)*
C240.6392 (3)0.7843 (4)0.1736 (4)0.0929 (16)
H240.67650.76790.10790.0493 (19)*
C250.6227 (2)0.7345 (2)0.2708 (4)0.0629 (10)
H250.64770.68380.27070.0493 (19)*
C260.61601 (17)0.64760 (17)0.5193 (3)0.0391 (7)
C270.70605 (19)0.6622 (2)0.5029 (4)0.0573 (10)
H270.72490.70620.45690.0493 (19)*
C280.7689 (2)0.6116 (3)0.5547 (5)0.0768 (14)
H280.83040.62140.54250.0493 (19)*
C290.7433 (3)0.5490 (3)0.6220 (4)0.0763 (13)
H290.78660.51520.65660.0493 (19)*
C300.6550 (3)0.5348 (2)0.6397 (4)0.0664 (11)
H300.63710.49120.68720.0493 (19)*
C310.5916 (2)0.58318 (18)0.5892 (3)0.0499 (9)
H310.53050.57240.60230.0493 (19)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0268 (12)0.0221 (12)0.0289 (14)0.0037 (10)0.0000.000
O20.0256 (9)0.0275 (9)0.0433 (12)0.0020 (8)0.0038 (8)0.0062 (9)
O30.0306 (10)0.0418 (11)0.0651 (15)0.0037 (10)0.0079 (11)0.0049 (11)
O40.0374 (10)0.0309 (10)0.0315 (11)0.0030 (9)0.0051 (9)0.0005 (9)
O50.0320 (9)0.0242 (9)0.0281 (10)0.0031 (8)0.0005 (8)0.0023 (8)
O60.0643 (14)0.0504 (13)0.0434 (14)0.0062 (12)0.0122 (12)0.0098 (11)
O70.0381 (10)0.0244 (9)0.0422 (11)0.0028 (8)0.0040 (9)0.0041 (9)
O80.0542 (13)0.0343 (11)0.0701 (17)0.0115 (11)0.0077 (12)0.0092 (12)
O90.0267 (9)0.0280 (9)0.0371 (10)0.0030 (8)0.0029 (8)0.0096 (9)
C10.0279 (13)0.0245 (13)0.0300 (15)0.0004 (11)0.0020 (12)0.0034 (12)
C20.0258 (13)0.0226 (13)0.0314 (15)0.0024 (11)0.0024 (12)0.0033 (12)
C30.0292 (13)0.0246 (13)0.0302 (16)0.0028 (11)0.0031 (12)0.0005 (12)
C40.0310 (14)0.0225 (13)0.0339 (16)0.0048 (11)0.0021 (13)0.0002 (12)
C50.0270 (13)0.0244 (13)0.0332 (15)0.0027 (11)0.0001 (12)0.0026 (12)
C60.0264 (13)0.0296 (14)0.0403 (17)0.0004 (11)0.0005 (13)0.0096 (14)
C70.0293 (14)0.0333 (15)0.0444 (18)0.0027 (13)0.0036 (14)0.0005 (14)
C80.0430 (17)0.056 (2)0.077 (3)0.0065 (16)0.0142 (18)0.0245 (19)
C90.0422 (16)0.0416 (17)0.0346 (18)0.0023 (14)0.0042 (14)0.0028 (15)
C100.076 (2)0.060 (2)0.043 (2)0.0112 (19)0.0170 (19)0.0044 (18)
C110.0456 (17)0.0282 (15)0.0507 (19)0.0049 (14)0.0069 (16)0.0067 (15)
C120.075 (2)0.0385 (19)0.096 (3)0.0071 (18)0.012 (2)0.024 (2)
C130.0306 (13)0.0318 (15)0.0355 (16)0.0030 (12)0.0010 (13)0.0143 (13)
C140.0329 (14)0.0263 (14)0.0429 (17)0.0009 (12)0.0060 (13)0.0026 (13)
C150.0327 (15)0.0413 (17)0.056 (2)0.0021 (13)0.0092 (15)0.0083 (16)
C160.0342 (16)0.054 (2)0.067 (2)0.0034 (15)0.0119 (16)0.005 (2)
C170.0491 (19)0.0426 (18)0.067 (2)0.0118 (15)0.0262 (18)0.0005 (18)
C180.061 (2)0.048 (2)0.077 (3)0.0039 (17)0.017 (2)0.025 (2)
C190.0463 (18)0.051 (2)0.064 (2)0.0042 (16)0.0058 (18)0.0227 (19)
C200.0335 (15)0.0457 (17)0.0420 (18)0.0055 (14)0.0007 (14)0.0112 (16)
C210.0407 (16)0.0516 (19)0.0449 (19)0.0015 (15)0.0018 (15)0.0049 (17)
C220.065 (2)0.068 (2)0.072 (3)0.013 (2)0.001 (2)0.021 (2)
C230.087 (3)0.116 (4)0.063 (3)0.031 (3)0.004 (3)0.025 (3)
C240.086 (3)0.134 (5)0.059 (3)0.025 (3)0.041 (3)0.013 (3)
C250.060 (2)0.071 (2)0.058 (2)0.0094 (19)0.0205 (19)0.021 (2)
C260.0332 (14)0.0391 (17)0.0451 (19)0.0059 (13)0.0076 (14)0.0204 (16)
C270.0364 (16)0.0569 (19)0.078 (3)0.0080 (16)0.0067 (17)0.0323 (19)
C280.0346 (18)0.082 (3)0.114 (4)0.022 (2)0.028 (2)0.055 (3)
C290.075 (3)0.064 (3)0.089 (3)0.037 (2)0.040 (3)0.038 (3)
C300.079 (3)0.053 (2)0.067 (3)0.026 (2)0.024 (2)0.011 (2)
C310.0482 (18)0.0445 (18)0.057 (2)0.0088 (15)0.0107 (17)0.0077 (18)
Geometric parameters (Å, º) top
O1—C11.417 (3)C11—C121.487 (4)
O1—C1i1.417 (3)C13—C261.531 (4)
O2—C71.359 (3)C13—C141.534 (4)
O2—C21.436 (3)C13—C201.536 (4)
O3—C71.200 (3)C14—C191.376 (4)
O4—C91.351 (3)C14—C151.382 (4)
O4—C31.441 (3)C15—C161.386 (4)
O5—C11.406 (3)C16—C171.361 (5)
O5—C51.444 (3)C17—C181.371 (5)
O6—C91.203 (4)C18—C191.374 (4)
O7—C111.374 (3)C20—C251.385 (5)
O7—C41.434 (3)C20—C211.389 (4)
O8—C111.183 (4)C21—C221.379 (5)
O9—C61.407 (3)C22—C231.351 (6)
O9—C131.444 (3)C23—C241.374 (6)
C1—C21.515 (4)C24—C251.380 (6)
C2—C31.521 (4)C26—C271.390 (4)
C3—C41.520 (4)C26—C311.392 (5)
C4—C51.523 (4)C27—C281.403 (5)
C5—C61.506 (4)C28—C291.357 (6)
C7—C81.481 (4)C29—C301.365 (6)
C9—C101.494 (4)C30—C311.380 (5)
C1—O1—C1i113.3 (3)O9—C13—C26108.0 (2)
C7—O2—C2117.1 (2)O9—C13—C14104.0 (2)
C9—O4—C3117.3 (2)C26—C13—C14111.0 (2)
C1—O5—C5113.41 (19)O9—C13—C20109.8 (2)
C11—O7—C4116.7 (2)C26—C13—C20116.0 (2)
C6—O9—C13116.49 (18)C14—C13—C20107.4 (2)
O5—C1—O1111.21 (18)C19—C14—C15117.8 (3)
O5—C1—C2111.3 (2)C19—C14—C13120.1 (3)
O1—C1—C2107.3 (2)C15—C14—C13122.1 (3)
O2—C2—C1106.63 (19)C14—C15—C16120.5 (3)
O2—C2—C3112.0 (2)C17—C16—C15120.5 (3)
C1—C2—C3110.7 (2)C16—C17—C18119.5 (3)
O4—C3—C4105.92 (18)C17—C18—C19120.0 (3)
O4—C3—C2112.08 (19)C18—C19—C14121.5 (3)
C4—C3—C2107.3 (2)C25—C20—C21118.0 (3)
O7—C4—C3109.2 (2)C25—C20—C13122.6 (3)
O7—C4—C5107.7 (2)C21—C20—C13119.1 (3)
C3—C4—C5109.9 (2)C22—C21—C20120.7 (3)
O5—C5—C6107.2 (2)C23—C22—C21120.7 (4)
O5—C5—C4107.76 (19)C22—C23—C24119.8 (4)
C6—C5—C4113.4 (2)C23—C24—C25120.4 (4)
O9—C6—C5107.58 (19)C24—C25—C20120.4 (4)
O3—C7—O2122.6 (3)C27—C26—C31118.1 (3)
O3—C7—C8125.9 (3)C27—C26—C13122.7 (3)
O2—C7—C8111.5 (3)C31—C26—C13118.9 (3)
O6—C9—O4123.8 (3)C26—C27—C28119.6 (4)
O6—C9—C10125.5 (3)C29—C28—C27121.1 (4)
O4—C9—C10110.7 (3)C28—C29—C30119.6 (4)
O8—C11—O7123.6 (3)C29—C30—C31120.7 (4)
O8—C11—C12127.1 (3)C30—C31—C26120.9 (3)
O7—C11—C12109.3 (3)
C5—O5—C1—O160.7 (2)C26—C13—C14—C1961.7 (4)
C5—O5—C1—C258.9 (3)C20—C13—C14—C1966.0 (3)
C1i—O1—C1—O563.35 (16)O9—C13—C14—C151.5 (4)
C1i—O1—C1—C2174.7 (2)C26—C13—C14—C15117.4 (3)
C7—O2—C2—C1143.4 (2)C20—C13—C14—C15114.8 (3)
C7—O2—C2—C395.4 (3)C19—C14—C15—C160.2 (5)
O5—C1—C2—O2177.29 (19)C13—C14—C15—C16179.4 (3)
O1—C1—C2—O255.4 (2)C14—C15—C16—C170.1 (5)
O5—C1—C2—C355.3 (3)C15—C16—C17—C180.5 (5)
O1—C1—C2—C366.6 (2)C16—C17—C18—C190.7 (5)
C9—O4—C3—C4147.3 (2)C17—C18—C19—C140.4 (6)
C9—O4—C3—C296.0 (3)C15—C14—C19—C180.1 (5)
O2—C2—C3—O470.2 (2)C13—C14—C19—C18179.3 (3)
C1—C2—C3—O4171.0 (2)O9—C13—C20—C25162.5 (3)
O2—C2—C3—C4173.96 (19)C26—C13—C20—C2539.7 (4)
C1—C2—C3—C455.1 (3)C14—C13—C20—C2585.1 (3)
C11—O7—C4—C3112.1 (2)O9—C13—C20—C2122.9 (3)
C11—O7—C4—C5128.6 (2)C26—C13—C20—C21145.7 (3)
O4—C3—C4—O763.1 (2)C14—C13—C20—C2189.5 (3)
C2—C3—C4—O7177.00 (19)C25—C20—C21—C220.4 (5)
O4—C3—C4—C5178.93 (19)C13—C20—C21—C22175.2 (3)
C2—C3—C4—C559.0 (3)C20—C21—C22—C230.9 (5)
C1—O5—C5—C6176.39 (19)C21—C22—C23—C241.7 (6)
C1—O5—C5—C461.3 (3)C22—C23—C24—C251.9 (7)
O7—C4—C5—O5179.94 (18)C23—C24—C25—C201.3 (6)
C3—C4—C5—O561.2 (3)C21—C20—C25—C240.6 (5)
O7—C4—C5—C661.5 (3)C13—C20—C25—C24175.2 (3)
C3—C4—C5—C6179.6 (2)O9—C13—C26—C27100.6 (3)
C13—O9—C6—C5169.7 (2)C14—C13—C26—C27146.1 (3)
O5—C5—C6—O966.6 (3)C20—C13—C26—C2723.1 (4)
C4—C5—C6—O952.2 (3)O9—C13—C26—C3173.5 (3)
C2—O2—C7—O35.1 (4)C14—C13—C26—C3139.8 (4)
C2—O2—C7—C8175.4 (2)C20—C13—C26—C31162.7 (3)
C3—O4—C9—O610.8 (4)C31—C26—C27—C281.1 (5)
C3—O4—C9—C10170.0 (2)C13—C26—C27—C28175.3 (3)
C4—O7—C11—O81.1 (4)C26—C27—C28—C290.8 (5)
C4—O7—C11—C12178.6 (3)C27—C28—C29—C300.0 (6)
C6—O9—C13—C2656.7 (3)C28—C29—C30—C310.4 (6)
C6—O9—C13—C14174.7 (2)C29—C30—C31—C260.1 (5)
C6—O9—C13—C2070.7 (3)C27—C26—C31—C300.6 (5)
O9—C13—C14—C19177.7 (3)C13—C26—C31—C30175.0 (3)
Symmetry code: (i) x+1, y+2, z.

Experimental details

Crystal data
Chemical formulaC62H62O17
Mr1079.12
Crystal system, space groupOrthorhombic, P21212
Temperature (K)150
a, b, c (Å)15.0595 (4), 17.1977 (6), 10.8465 (4)
V3)2809.12 (16)
Z2
Radiation typeMo Kα
µ (mm1)0.09
Crystal size (mm)0.50 × 0.30 × 0.20
Data collection
DiffractometerEnraf Nonius KappaCCD area-detector
diffractometer
Absorption correctionMulti-scan
(SORTAV; Blessing, 1995, 1997)
Tmin, Tmax0.955, 0.982
No. of measured, independent and
observed [I > 2σ(I)] reflections
16774, 3235, 2333
Rint0.078
(sin θ/λ)max1)0.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.101, 1.00
No. of reflections3235
No. of parameters363
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.21, 0.25

Computer programs: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998), DENZO and COLLECT, SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997).

Selected geometric parameters (Å, º) top
O1—C11.417 (3)O5—C51.444 (3)
O5—C11.406 (3)
C1—O1—C1i113.3 (3)O9—C13—C26108.0 (2)
C1—O5—C5113.41 (19)O9—C13—C14104.0 (2)
O4—C3—C4105.92 (18)O9—C13—C20109.8 (2)
C13—O9—C6—C5169.7 (2)C3—O4—C9—O610.8 (4)
C2—O2—C7—O35.1 (4)C4—O7—C11—O81.1 (4)
Symmetry code: (i) x+1, y+2, z.
 

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