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In the crystal structure of the title compound, (4aR,5R,6S,7S,8aS)-methyl 8a-ethenylocta­hydro-5-acet­oxy-7-{[2-(acetoxy­meth­yl)-1-oxo-2-propen­yl]­oxy}-α,4-bis­(methyl­ene)-3-oxo-1H-2-benzopyran-6-acetate, C24H28O10, the mol­ecule has a cis configuration at the junction of the two six-membered rings and not a trans configuration as was assigned on the basis of NMR data in solution [Asaka et al. (1977). Phytochemistry, 16, 1838–1839].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805029387/bt6736sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805029387/bt6736Isup2.hkl
Contains datablock I

CCDC reference: 287475

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.043
  • wR factor = 0.115
  • Data-to-parameter ratio = 8.3

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT220_ALERT_2_A Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.32 Ratio
Author Response: The crystal structure was performed at room temperature and the results are good except the high temperature factors of some O atoms.
PLAT242_ALERT_2_A Check Low       Ueq as Compared to Neighbors for        C16
Author Response: The crystal structure was performed at room temperature and the results are good except the high temperature factors of some O atoms.

Alert level B PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.11 Ratio
Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.27 Ratio
Author Response: The crystal structure was performed at room temperature and the results are good except the high temperature factors of some O atoms.
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C14
Author Response: The crystal structure was performed at room temperature and the results are good except the high temperature factors of some O atoms.
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C20
Author Response: The crystal structure was performed at room temperature and the results are good except the high temperature factors of some O atoms.
PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          6

Alert level G REFLT03_ALERT_4_G 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. From the CIF: _diffrn_reflns_theta_max 25.33 From the CIF: _reflns_number_total 2589 Count of symmetry unique reflns 2596 Completeness (_total/calc) 99.73% 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
2 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

No Comment

Experimental top

Epivernodalol was isolated from an ethanolic extract and acetylated according to the method of Koul et al. (2003). It was crystallized from ethyl acetate/petroleum ether (1:4) (m.p. 381 K). MS (diacetate of 2): m/z at M+ 476 (5), 474 (19), 435 (5), 357 (3), 329 (5), 316 (8), 291 (54), 273 (24), 244 (33), 214 (25), 182 (26), 154 (27), 136 (9), 127 (100).

Refinement top

H atoms were placed in calculated positions (C—H = 0.93–0.97 Å) with Uiso values constrained to be 1.5Ueq of the carrier atom for the methyl H atoms and 1.2Ueq for the remaining H atoms. The methyl groups were allowed to rotate but not to tip. The absolute configuration was assigned arbitrarily.

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97, PARST95 (Nardelli, 1995) and PLATON (Spek, 2001).

Figures top
[Figure 1] Fig. 1. View of the title compound (XP; Sheldrick, 1991), showing the labelling of all non-H atoms. Displacement ellipsoids are drawn at the 30% probability level. H atoms, except H1, have been omitted for clarity.
(4aR,5R,6S,7S,8aS)-methyl 8a-ethenyloctahydro-5-acetoxy-7-{[2-(acetoxymethyl)-1-oxo-2-propenyl]oxy}- α,4-bis(methylene)-3-oxo-1H-2-benzopyran-6-acetate top
Crystal data top
C24H28O10F(000) = 1008
Mr = 476.46Dx = 1.276 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 14723 reflections
a = 8.0887 (2) Åθ = 3.0–25.3°
b = 12.8750 (4) ŵ = 0.10 mm1
c = 23.8205 (8) ÅT = 291 K
V = 2480.71 (13) Å3Needle, colourless
Z = 40.20 × 0.05 × 0.05 mm
Data collection top
Nonius KappaCCD
diffractometer
1373 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.069
Graphite monochromatorθmax = 25.3°, θmin = 3.0°
Detector resolution: 19 vertical, 18 horizontal pixels mm-1h = 99
208 frames via ω–rotation (Δω=1°) and two times 60 s per frame (two sets at different κ–angles) scansk = 1515
14723 measured reflectionsl = 2828
2589 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.115 w = 1/[σ2(Fo2) + (0.0643P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.87(Δ/σ)max < 0.001
2589 reflectionsΔρmax = 0.23 e Å3
311 parametersΔρmin = 0.14 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0057 (15)
Crystal data top
C24H28O10V = 2480.71 (13) Å3
Mr = 476.46Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 8.0887 (2) ŵ = 0.10 mm1
b = 12.8750 (4) ÅT = 291 K
c = 23.8205 (8) Å0.20 × 0.05 × 0.05 mm
Data collection top
Nonius KappaCCD
diffractometer
1373 reflections with I > 2σ(I)
14723 measured reflectionsRint = 0.069
2589 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0430 restraints
wR(F2) = 0.115H-atom parameters constrained
S = 0.87Δρmax = 0.23 e Å3
2589 reflectionsΔρmin = 0.14 e Å3
311 parameters
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*/Ueq
O10.3229 (4)0.1415 (2)0.05742 (10)0.0680 (8)
O20.1082 (4)0.2420 (3)0.06704 (12)0.0796 (9)
O30.5712 (3)0.1161 (2)0.12470 (10)0.0635 (8)
O41.0192 (5)0.3231 (4)0.18172 (17)0.1296 (15)
O50.8171 (4)0.0850 (3)0.08519 (16)0.1040 (12)
O61.1947 (12)0.3692 (8)0.1219 (4)0.317 (6)
O70.4565 (4)0.0040 (2)0.27571 (11)0.0845 (10)
O80.2769 (5)0.0919 (3)0.22997 (13)0.1210 (16)
O90.1151 (3)0.1157 (2)0.12516 (10)0.0597 (7)
O100.1825 (5)0.2838 (3)0.11700 (17)0.0995 (12)
C10.1829 (5)0.0341 (3)0.03763 (15)0.0527 (10)
H10.10650.02070.04960.063*
C20.3158 (5)0.0179 (3)0.00147 (15)0.0569 (11)
C30.4274 (5)0.0893 (3)0.03653 (15)0.0625 (11)
H3A0.52110.11070.01390.075*
H3B0.36600.15120.04670.075*
C40.4906 (5)0.0372 (3)0.08978 (15)0.0588 (11)
H40.56800.01880.08060.071*
C50.3490 (5)0.0036 (3)0.12536 (14)0.0526 (10)
H50.27450.05480.13300.063*
C60.2528 (4)0.0833 (3)0.09085 (14)0.0520 (10)
H60.32320.14280.08150.062*
C70.0837 (5)0.1103 (3)0.00231 (14)0.0533 (10)
C80.1714 (6)0.1698 (4)0.04188 (16)0.0614 (11)
C90.4183 (5)0.0681 (3)0.02476 (15)0.0605 (11)
H9A0.50150.03700.04880.073*
H9B0.47540.10540.00490.073*
C100.0768 (6)0.1229 (4)0.00687 (17)0.0752 (13)
H10A0.13180.16810.01720.090*
H10B0.13540.08670.03420.090*
C110.2388 (6)0.0838 (3)0.04500 (17)0.0697 (13)
H110.30510.09500.07630.084*
C120.0934 (7)0.1263 (4)0.0467 (2)0.0993 (17)
H12A0.02090.11810.01670.119*
H12B0.06180.16490.07790.119*
C130.7339 (5)0.1295 (4)0.11881 (18)0.0651 (12)
C140.8013 (5)0.2067 (4)0.15872 (19)0.0673 (12)
C150.9826 (6)0.2296 (5)0.1509 (2)0.0993 (17)
H15A1.04870.17230.16490.119*
H15B1.00720.23920.11140.119*
C161.1194 (9)0.3922 (7)0.1639 (5)0.147 (3)
C171.1391 (9)0.4828 (5)0.1996 (4)0.170 (4)
H17A1.17430.54080.17740.255*
H17B1.22050.46850.22790.255*
H17C1.03540.49880.21720.255*
C180.7101 (7)0.2511 (5)0.1958 (2)0.121 (2)
H18A0.59820.23500.19820.145*
H18B0.75600.29940.22040.145*
C190.4114 (5)0.0433 (3)0.18111 (15)0.0552 (10)
C200.3722 (6)0.0225 (4)0.23068 (17)0.0681 (12)
C210.4309 (8)0.0571 (5)0.32603 (17)0.119 (2)
H21A0.43150.12960.31660.178*
H21B0.51780.04300.35240.178*
H21C0.32630.03930.34250.178*
C220.4987 (5)0.1292 (4)0.18622 (16)0.0747 (13)
H22A0.53710.14970.22130.090*
H22B0.52190.16940.15470.090*
C230.0956 (6)0.2190 (4)0.13534 (17)0.0693 (13)
C240.0544 (6)0.2346 (4)0.17112 (19)0.0919 (16)
H24A0.15180.21950.14960.138*
H24B0.04930.18910.20300.138*
H24C0.05830.30540.18370.138*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0704 (18)0.076 (2)0.0580 (16)0.0033 (18)0.0077 (15)0.0189 (16)
O20.086 (2)0.077 (2)0.0759 (19)0.0053 (19)0.0080 (18)0.0257 (18)
O30.0558 (17)0.0673 (19)0.0674 (16)0.0076 (15)0.0055 (14)0.0185 (16)
O40.123 (3)0.131 (4)0.135 (3)0.052 (3)0.009 (3)0.023 (3)
O50.070 (2)0.114 (3)0.128 (3)0.009 (2)0.018 (2)0.057 (3)
O60.304 (10)0.314 (11)0.333 (11)0.168 (9)0.170 (9)0.089 (9)
O70.106 (2)0.099 (3)0.0481 (15)0.021 (2)0.0066 (17)0.0103 (17)
O80.156 (3)0.140 (3)0.0670 (19)0.087 (3)0.014 (2)0.026 (2)
O90.0614 (16)0.065 (2)0.0523 (14)0.0042 (15)0.0101 (14)0.0005 (15)
O100.097 (2)0.062 (2)0.139 (3)0.003 (2)0.025 (2)0.015 (2)
C10.060 (2)0.047 (2)0.051 (2)0.001 (2)0.004 (2)0.007 (2)
C20.070 (3)0.055 (3)0.045 (2)0.001 (2)0.001 (2)0.000 (2)
C30.068 (3)0.059 (3)0.060 (2)0.012 (2)0.006 (2)0.001 (2)
C40.065 (3)0.056 (3)0.055 (2)0.005 (2)0.003 (2)0.017 (2)
C50.061 (2)0.049 (2)0.047 (2)0.000 (2)0.0008 (19)0.002 (2)
C60.052 (2)0.057 (3)0.047 (2)0.003 (2)0.0080 (19)0.002 (2)
C70.060 (3)0.050 (3)0.050 (2)0.000 (2)0.001 (2)0.002 (2)
C80.075 (3)0.056 (3)0.054 (2)0.004 (3)0.012 (2)0.001 (2)
C90.066 (3)0.065 (3)0.051 (2)0.007 (2)0.012 (2)0.004 (2)
C100.068 (3)0.075 (3)0.083 (3)0.005 (3)0.002 (3)0.020 (3)
C110.088 (3)0.064 (3)0.057 (3)0.002 (3)0.001 (2)0.009 (2)
C120.122 (5)0.085 (4)0.091 (4)0.018 (4)0.001 (3)0.022 (3)
C130.063 (3)0.067 (3)0.066 (3)0.002 (3)0.001 (2)0.010 (3)
C140.060 (3)0.069 (3)0.073 (3)0.003 (3)0.005 (2)0.006 (3)
C150.082 (3)0.103 (4)0.113 (4)0.010 (3)0.007 (3)0.029 (4)
C160.111 (5)0.104 (6)0.225 (10)0.043 (5)0.038 (6)0.011 (7)
C170.165 (7)0.086 (5)0.259 (10)0.040 (5)0.073 (7)0.017 (6)
C180.083 (4)0.155 (6)0.124 (4)0.024 (4)0.013 (4)0.072 (4)
C190.056 (2)0.058 (3)0.052 (2)0.002 (2)0.001 (2)0.004 (2)
C200.075 (3)0.076 (3)0.053 (3)0.009 (3)0.006 (3)0.004 (3)
C210.168 (6)0.138 (5)0.051 (3)0.043 (5)0.002 (3)0.026 (3)
C220.086 (3)0.085 (4)0.053 (2)0.016 (3)0.007 (2)0.010 (2)
C230.070 (3)0.071 (4)0.067 (3)0.017 (3)0.002 (3)0.008 (3)
C240.088 (3)0.113 (4)0.075 (3)0.032 (3)0.016 (3)0.005 (3)
Geometric parameters (Å, º) top
O1—C81.331 (5)C7—C81.483 (5)
O1—C91.447 (5)C9—H9A0.9700
O2—C81.219 (4)C9—H9B0.9700
O3—C131.335 (5)C10—H10A0.9300
O3—C41.467 (4)C10—H10B0.9300
O4—C161.276 (7)C11—C121.298 (6)
O4—C151.442 (6)C11—H110.9300
O5—C131.192 (5)C12—H12A0.9300
O6—C161.207 (10)C12—H12B0.9300
O7—C201.316 (5)C13—C141.479 (6)
O7—C211.449 (5)C14—C181.286 (6)
O8—C201.181 (5)C14—C151.507 (6)
O9—C231.361 (5)C15—H15A0.9700
O9—C61.443 (4)C15—H15B0.9700
O10—C231.175 (5)C16—C171.453 (11)
C1—C71.522 (5)C17—H17A0.9600
C1—C61.526 (5)C17—H17B0.9600
C1—C21.531 (5)C17—H17C0.9600
C1—H10.9800C18—H18A0.9300
C2—C91.517 (5)C18—H18B0.9300
C2—C111.528 (6)C19—C221.319 (6)
C2—C31.536 (5)C19—C201.487 (6)
C3—C41.523 (5)C21—H21A0.9600
C3—H3A0.9700C21—H21B0.9600
C3—H3B0.9700C21—H21C0.9600
C4—C51.518 (5)C22—H22A0.9300
C4—H40.9800C22—H22B0.9300
C5—C191.510 (5)C23—C241.497 (6)
C5—C61.527 (5)C24—H24A0.9600
C5—H50.9800C24—H24B0.9600
C6—H60.9800C24—H24C0.9600
C7—C101.313 (6)
C8—O1—C9121.4 (3)H10A—C10—H10B120.0
C13—O3—C4117.9 (3)C12—C11—C2128.8 (4)
C16—O4—C15122.9 (6)C12—C11—H11115.6
C20—O7—C21117.4 (4)C2—C11—H11115.6
C23—O9—C6118.2 (3)C11—C12—H12A120.0
C7—C1—C6112.8 (3)C11—C12—H12B120.0
C7—C1—C2109.9 (3)H12A—C12—H12B120.0
C6—C1—C2112.9 (3)O5—C13—O3124.4 (4)
C7—C1—H1107.0O5—C13—C14123.2 (4)
C6—C1—H1107.0O3—C13—C14112.5 (4)
C2—C1—H1107.0C18—C14—C13122.0 (4)
C9—C2—C11109.3 (3)C18—C14—C15123.8 (5)
C9—C2—C1107.3 (3)C13—C14—C15114.2 (4)
C11—C2—C1111.4 (3)O4—C15—C14107.5 (5)
C9—C2—C3109.8 (3)O4—C15—H15A110.2
C11—C2—C3107.5 (3)C14—C15—H15A110.2
C1—C2—C3111.6 (3)O4—C15—H15B110.2
C4—C3—C2112.7 (3)C14—C15—H15B110.2
C4—C3—H3A109.0H15A—C15—H15B108.5
C2—C3—H3A109.0O6—C16—O4115.2 (9)
C4—C3—H3B109.0O6—C16—C17128.8 (8)
C2—C3—H3B109.0O4—C16—C17115.7 (9)
H3A—C3—H3B107.8C16—C17—H17A109.5
O3—C4—C5105.0 (3)C16—C17—H17B109.5
O3—C4—C3108.4 (3)H17A—C17—H17B109.5
C5—C4—C3111.4 (3)C16—C17—H17C109.5
O3—C4—H4110.6H17A—C17—H17C109.5
C5—C4—H4110.6H17B—C17—H17C109.5
C3—C4—H4110.6C14—C18—H18A120.0
C19—C5—C4110.9 (3)C14—C18—H18B120.0
C19—C5—C6114.6 (3)H18A—C18—H18B120.0
C4—C5—C6108.4 (3)C22—C19—C20121.2 (4)
C19—C5—H5107.6C22—C19—C5123.0 (4)
C4—C5—H5107.6C20—C19—C5115.8 (4)
C6—C5—H5107.6O8—C20—O7123.1 (4)
O9—C6—C1107.7 (3)O8—C20—C19124.0 (4)
O9—C6—C5106.4 (3)O7—C20—C19112.9 (4)
C1—C6—C5110.9 (3)O7—C21—H21A109.5
O9—C6—H6110.6O7—C21—H21B109.5
C1—C6—H6110.6H21A—C21—H21B109.5
C5—C6—H6110.6O7—C21—H21C109.5
C10—C7—C8117.9 (4)H21A—C21—H21C109.5
C10—C7—C1123.7 (4)H21B—C21—H21C109.5
C8—C7—C1118.3 (4)C19—C22—H22A120.0
O2—C8—O1117.3 (4)C19—C22—H22B120.0
O2—C8—C7122.9 (4)H22A—C22—H22B120.0
O1—C8—C7119.7 (4)O10—C23—O9123.9 (4)
O1—C9—C2114.0 (3)O10—C23—C24126.9 (5)
O1—C9—H9A108.8O9—C23—C24109.1 (5)
C2—C9—H9A108.8C23—C24—H24A109.5
O1—C9—H9B108.8C23—C24—H24B109.5
C2—C9—H9B108.8H24A—C24—H24B109.5
H9A—C9—H9B107.7C23—C24—H24C109.5
C7—C10—H10A120.0H24A—C24—H24C109.5
C7—C10—H10B120.0H24B—C24—H24C109.5
C7—C1—C2—C955.3 (4)C1—C7—C8—O2169.9 (3)
C6—C1—C2—C971.5 (4)C10—C7—C8—O1163.4 (4)
C7—C1—C2—C1164.2 (4)C1—C7—C8—O113.4 (5)
C6—C1—C2—C11169.0 (3)C8—O1—C9—C236.3 (5)
C7—C1—C2—C3175.6 (3)C11—C2—C9—O164.0 (4)
C6—C1—C2—C348.8 (4)C1—C2—C9—O156.8 (4)
C9—C2—C3—C470.3 (4)C3—C2—C9—O1178.3 (3)
C11—C2—C3—C4170.9 (3)C9—C2—C11—C12142.4 (5)
C1—C2—C3—C448.6 (5)C1—C2—C11—C1224.1 (7)
C13—O3—C4—C5148.3 (4)C3—C2—C11—C1298.4 (6)
C13—O3—C4—C392.6 (4)C4—O3—C13—O53.7 (6)
C2—C3—C4—O3170.4 (3)C4—O3—C13—C14176.5 (3)
C2—C3—C4—C555.4 (4)O5—C13—C14—C18177.6 (5)
O3—C4—C5—C1956.0 (4)O3—C13—C14—C182.6 (6)
C3—C4—C5—C19173.1 (3)O5—C13—C14—C153.7 (7)
O3—C4—C5—C6177.4 (3)O3—C13—C14—C15176.0 (4)
C3—C4—C5—C660.3 (4)C16—O4—C15—C14142.1 (6)
C23—O9—C6—C1115.9 (4)C18—C14—C15—O413.3 (8)
C23—O9—C6—C5125.1 (3)C13—C14—C15—O4165.3 (4)
C7—C1—C6—O963.1 (4)C15—O4—C16—O67.2 (13)
C2—C1—C6—O9171.6 (3)C15—O4—C16—C17178.6 (6)
C7—C1—C6—C5179.1 (3)C4—C5—C19—C2270.9 (5)
C2—C1—C6—C555.6 (4)C6—C5—C19—C2252.2 (5)
C19—C5—C6—O958.5 (4)C4—C5—C19—C20107.4 (4)
C4—C5—C6—O9177.1 (3)C6—C5—C19—C20129.5 (4)
C19—C5—C6—C1175.4 (3)C21—O7—C20—O81.0 (7)
C4—C5—C6—C160.2 (4)C21—O7—C20—C19178.4 (4)
C6—C1—C7—C1092.4 (5)C22—C19—C20—O8169.4 (5)
C2—C1—C7—C10140.8 (4)C5—C19—C20—O812.3 (7)
C6—C1—C7—C891.0 (4)C22—C19—C20—O711.3 (6)
C2—C1—C7—C835.8 (5)C5—C19—C20—O7167.1 (4)
C9—O1—C8—O2170.2 (3)C6—O9—C23—O101.5 (6)
C9—O1—C8—C713.0 (5)C6—O9—C23—C24179.6 (3)
C10—C7—C8—O213.3 (6)

Experimental details

Crystal data
Chemical formulaC24H28O10
Mr476.46
Crystal system, space groupOrthorhombic, P212121
Temperature (K)291
a, b, c (Å)8.0887 (2), 12.8750 (4), 23.8205 (8)
V3)2480.71 (13)
Z4
Radiation typeMo Kα
µ (mm1)0.10
Crystal size (mm)0.20 × 0.05 × 0.05
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
14723, 2589, 1373
Rint0.069
(sin θ/λ)max1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.043, 0.115, 0.87
No. of reflections2589
No. of parameters311
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.23, 0.14

Computer programs: COLLECT (Nonius, 1998), DENZO and SCALEPACK (Otwinowski & Minor, 1997), DENZO and SCALEPACK, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1991), SHELXL97, PARST95 (Nardelli, 1995) and PLATON (Spek, 2001).

 

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