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In the title compound, C25H26O5, the five-membered arabino­furan­oside ring displays an envelope conformation. Intra­molecular O—H...O hydrogen bonding helps to stabilize the mol­ecular structure, and inter­molecular O—H...O hydrogen bonding links the mol­ecules into infinite helical supra­molecular chains along the a axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807027110/xu2257sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807027110/xu2257Isup2.hkl
Contains datablock I

CCDC reference: 654921

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.038
  • wR factor = 0.082
  • Data-to-parameter ratio = 7.5

checkCIF/PLATON results

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Alert level C PLAT089_ALERT_3_C Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 7.51 PLAT340_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 5
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 25.03 From the CIF: _reflns_number_total 2110 Count of symmetry unique reflns 2131 Completeness (_total/calc) 99.01% 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 PLAT791_ALERT_1_G Confirm the Absolute Configuration of C2 = . S PLAT791_ALERT_1_G Confirm the Absolute Configuration of C3 = . S PLAT791_ALERT_1_G Confirm the Absolute Configuration of C4 = . R PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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

Comment top

The skeleton of the title compound, is composed of three benzene rings and a five-membered heterocyclic ring. And the five-membered ring have envelope conformations, with atom C2 at the flap of the envelope. It lie 0.484 (3) Å. The resultant puckering causes significant contractions of the C1—C2—C3 angles.

The title compound contains both intramolecular and intermolecular O—H···O hydrogen bonds. The intramolecule O—H···O hydrogen bonds join the compound to form a cage, and the intermolecule O—H···O hydrogen bonds link the molecules into infinite helical chains along the a axis.

Related literature top

For synthesis, see Mikhailopulo & Sivets (1999).

Experimental top

The title compound was synthesized according to the procedure of Mikhailopulo & Sivets (1999). The title compound is obtained from methyl alpha/beta-D-arabinofuranoside, which reacted with trityl chloride in the presence of 4-(dimethylamino)pyridine in anhydride pyridine at 333–343 K for 6 h, after treatment and column chromatography (hexene-ethyl acetate 1:1, Rf 0.42) yield 45% as a white solid. The compound was crystallized from hexane-ethyl acetate (1:1) to yield colorless block-like crystals after a week at room temperature.

Refinement top

The hydroxyl H atoms were initially located in a difference Fourier map, and the position was allowed refined freely along with an isotropic displacement parameter. All other H-atoms were refined using a riding model with d(C—H) = 0.93 Å, Uiso=1.2Ueq (C) for aromatic, 0.97 Å, Uiso = 1.2Ueq (C) for CH2, and 0.96 Å, Uiso = 1.5Ueq (C) for CH3. And the methyl H was allowed to rotate freely about its C—C bond. In the absence of significant anomalous dispersion effects, Friedel pairs were merged.

Structure description top

The skeleton of the title compound, is composed of three benzene rings and a five-membered heterocyclic ring. And the five-membered ring have envelope conformations, with atom C2 at the flap of the envelope. It lie 0.484 (3) Å. The resultant puckering causes significant contractions of the C1—C2—C3 angles.

The title compound contains both intramolecular and intermolecular O—H···O hydrogen bonds. The intramolecule O—H···O hydrogen bonds join the compound to form a cage, and the intermolecule O—H···O hydrogen bonds link the molecules into infinite helical chains along the a axis.

For synthesis, see Mikhailopulo & Sivets (1999).

Computing details top

Data collection: DENZO (Otwinowski & Minor, 1997); cell refinement: SCALE (Otwinowski & Minor, 1997); data reduction: SCALE; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. A view of (I) showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms are represented by circles of arbitrary size.
[Figure 2] Fig. 2. The molecular packing of (I) viewed along the a axis. Dashed lines indicate hydrogen bonding interactions.
Methyl 5-O-triphenylmethyl-α-D-arabinofuranoside top
Crystal data top
C25H26O5F(000) = 864
Mr = 406.46Dx = 1.311 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 6994 reflections
a = 7.4286 (15) Åθ = 2.4–25.0°
b = 8.1298 (16) ŵ = 0.09 mm1
c = 34.101 (7) ÅT = 295 K
V = 2059.5 (7) Å3Block, colorless
Z = 40.50 × 0.20 × 0.18 mm
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
2110 independent reflections
Radiation source: fine-focus sealed tube1522 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.043
Detector resolution: 10 pixels mm-1θmax = 25.0°, θmin = 2.4°
ω scansh = 88
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 99
Tmin = 0.946, Tmax = 0.992l = 4040
6994 measured 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)] = 0.038H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.082 w = 1/[σ2(Fo2) + (0.0321P)2 + 0.285P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max < 0.001
2110 reflectionsΔρmax = 0.15 e Å3
281 parametersΔρmin = 0.16 e Å3
1 restraintExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0260 (15)
Crystal data top
C25H26O5V = 2059.5 (7) Å3
Mr = 406.46Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 7.4286 (15) ŵ = 0.09 mm1
b = 8.1298 (16) ÅT = 295 K
c = 34.101 (7) Å0.50 × 0.20 × 0.18 mm
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
2110 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
1522 reflections with I > 2σ(I)
Tmin = 0.946, Tmax = 0.992Rint = 0.043
6994 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0381 restraint
wR(F2) = 0.082H atoms treated by a mixture of independent and constrained refinement
S = 1.01Δρmax = 0.15 e Å3
2110 reflectionsΔρmin = 0.16 e Å3
281 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
O10.5208 (3)0.5222 (3)0.08813 (6)0.0407 (6)
O20.4450 (3)0.6557 (3)0.02943 (6)0.0469 (6)
O30.6178 (4)0.2463 (3)0.03120 (7)0.0498 (7)
H3O0.646 (6)0.221 (5)0.0550 (7)0.080 (15)*
O40.1565 (3)0.3851 (3)0.04668 (7)0.0424 (6)
H4O0.143 (6)0.362 (6)0.0231 (10)0.081 (16)*
O50.5912 (3)0.2009 (2)0.11522 (5)0.0309 (5)
C10.5460 (5)0.5315 (4)0.04707 (9)0.0367 (8)
H10.67400.54550.04090.044*
C20.4782 (5)0.3666 (4)0.03127 (10)0.0361 (8)
H20.43070.38080.00470.043*
C30.3270 (4)0.3232 (4)0.05910 (8)0.0329 (8)
H30.32100.20380.06290.039*
C40.3786 (4)0.4081 (4)0.09739 (8)0.0340 (8)
H40.27440.47050.10690.041*
C50.4398 (4)0.2931 (4)0.12950 (8)0.0342 (8)
H5A0.47400.35550.15260.041*
H5B0.34280.21900.13660.041*
C60.5213 (6)0.8169 (4)0.03313 (10)0.0532 (11)
H6A0.45040.89400.01840.080*
H6B0.64220.81620.02320.080*
H6C0.52230.84860.06020.080*
C70.6897 (4)0.1002 (4)0.14349 (8)0.0287 (7)
C80.8065 (4)0.0140 (4)0.11786 (8)0.0272 (7)
C90.9242 (4)0.0581 (4)0.09055 (8)0.0344 (8)
H90.92680.17190.08780.041*
C101.0355 (5)0.0378 (4)0.06784 (9)0.0373 (8)
H101.11040.01160.04950.045*
C111.0372 (5)0.2078 (4)0.07207 (9)0.0382 (8)
H111.11380.27200.05690.046*
C120.9242 (5)0.2801 (4)0.09896 (9)0.0389 (9)
H120.92360.39390.10180.047*
C130.8107 (5)0.1839 (4)0.12205 (9)0.0360 (8)
H130.73670.23410.14050.043*
C140.5546 (4)0.0034 (4)0.16861 (8)0.0283 (7)
C150.4268 (4)0.0927 (4)0.15044 (9)0.0403 (8)
H150.42440.09730.12320.048*
C160.3028 (5)0.1820 (4)0.17135 (11)0.0485 (9)
H160.21730.24510.15830.058*
C170.3051 (5)0.1779 (4)0.21152 (11)0.0484 (9)
H170.22280.23970.22580.058*
C180.4296 (5)0.0822 (5)0.23045 (9)0.0482 (10)
H180.43120.07870.25770.058*
C190.5529 (4)0.0092 (4)0.20932 (8)0.0368 (8)
H190.63540.07520.22250.044*
C200.8215 (4)0.2061 (4)0.16746 (8)0.0292 (7)
C210.9461 (4)0.1301 (4)0.19168 (9)0.0377 (8)
H210.94530.01600.19380.045*
C221.0720 (5)0.2198 (4)0.21282 (10)0.0434 (9)
H221.15450.16600.22880.052*
C231.0741 (5)0.3882 (5)0.20995 (10)0.0488 (10)
H231.15710.44930.22430.059*
C240.9544 (5)0.4649 (4)0.18615 (10)0.0496 (10)
H240.95630.57910.18430.060*
C250.8290 (5)0.3765 (4)0.16445 (9)0.0393 (8)
H250.74990.43150.14790.047*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0557 (15)0.0316 (12)0.0348 (12)0.0128 (12)0.0050 (11)0.0004 (10)
O20.0522 (15)0.0348 (13)0.0538 (14)0.0066 (13)0.0080 (14)0.0111 (12)
O30.0535 (17)0.0537 (16)0.0423 (14)0.0193 (14)0.0049 (13)0.0082 (14)
O40.0360 (13)0.0459 (14)0.0453 (14)0.0008 (13)0.0086 (13)0.0014 (13)
O50.0290 (11)0.0362 (11)0.0274 (10)0.0041 (11)0.0000 (10)0.0036 (10)
C10.0394 (19)0.0359 (18)0.0348 (18)0.0026 (18)0.0024 (18)0.0045 (16)
C20.038 (2)0.0373 (19)0.0326 (18)0.0037 (17)0.0051 (16)0.0032 (16)
C30.0318 (17)0.0281 (16)0.0387 (18)0.0008 (16)0.0057 (15)0.0022 (15)
C40.0365 (19)0.0364 (18)0.0293 (16)0.0012 (17)0.0005 (15)0.0027 (15)
C50.0310 (17)0.0401 (18)0.0313 (16)0.0024 (18)0.0041 (15)0.0025 (15)
C60.070 (3)0.0360 (19)0.053 (2)0.008 (2)0.000 (2)0.0026 (18)
C70.0275 (16)0.0317 (16)0.0268 (15)0.0019 (17)0.0012 (14)0.0045 (15)
C80.0279 (17)0.0272 (16)0.0266 (16)0.0010 (15)0.0030 (15)0.0016 (15)
C90.0351 (19)0.0325 (18)0.0355 (17)0.0028 (16)0.0047 (17)0.0049 (15)
C100.0305 (18)0.043 (2)0.0383 (18)0.0027 (17)0.0033 (17)0.0045 (16)
C110.0379 (19)0.0405 (19)0.0362 (18)0.0052 (18)0.0019 (18)0.0058 (17)
C120.043 (2)0.0292 (17)0.0451 (19)0.0038 (18)0.0015 (18)0.0005 (16)
C130.0361 (19)0.0360 (18)0.0361 (19)0.0024 (17)0.0023 (17)0.0023 (17)
C140.0262 (16)0.0291 (16)0.0295 (16)0.0009 (17)0.0023 (14)0.0038 (15)
C150.0337 (18)0.053 (2)0.0346 (18)0.011 (2)0.0013 (16)0.0028 (18)
C160.039 (2)0.050 (2)0.057 (2)0.014 (2)0.0022 (19)0.003 (2)
C170.039 (2)0.047 (2)0.059 (2)0.008 (2)0.011 (2)0.017 (2)
C180.053 (2)0.060 (2)0.0310 (17)0.001 (2)0.0077 (18)0.0144 (19)
C190.0364 (18)0.0429 (19)0.0311 (17)0.0034 (19)0.0024 (16)0.0024 (17)
C200.0275 (16)0.0304 (17)0.0298 (16)0.0046 (16)0.0021 (15)0.0008 (15)
C210.0364 (19)0.0338 (18)0.0428 (18)0.0004 (17)0.0047 (18)0.0015 (16)
C220.0326 (19)0.053 (2)0.0442 (19)0.000 (2)0.0094 (18)0.0020 (19)
C230.047 (2)0.052 (2)0.048 (2)0.014 (2)0.010 (2)0.009 (2)
C240.060 (3)0.0329 (19)0.056 (2)0.014 (2)0.009 (2)0.0010 (18)
C250.043 (2)0.0362 (18)0.0391 (19)0.0064 (19)0.0057 (18)0.0043 (16)
Geometric parameters (Å, º) top
O1—C11.415 (3)C10—C111.390 (4)
O1—C41.441 (4)C10—H100.9300
O2—C11.395 (4)C11—C121.375 (4)
O2—C61.434 (4)C11—H110.9300
O3—C21.425 (4)C12—C131.394 (4)
O3—H3O0.863 (19)C12—H120.9300
O4—C31.427 (4)C13—H130.9300
O4—H4O0.83 (4)C14—C151.377 (4)
O5—C51.437 (4)C14—C191.389 (4)
O5—C71.461 (3)C15—C161.372 (4)
C1—C21.530 (4)C15—H150.9300
C1—H10.9800C16—C171.371 (4)
C2—C31.512 (4)C16—H160.9300
C2—H20.9800C17—C181.370 (5)
C3—C41.526 (4)C17—H170.9300
C3—H30.9800C18—C191.382 (4)
C4—C51.510 (4)C18—H180.9300
C4—H40.9800C19—H190.9300
C5—H5A0.9700C20—C211.386 (4)
C5—H5B0.9700C20—C251.390 (4)
C6—H6A0.9600C21—C221.388 (4)
C6—H6B0.9600C21—H210.9300
C6—H6C0.9600C22—C231.373 (5)
C7—C141.536 (4)C22—H220.9300
C7—C201.539 (4)C23—C241.356 (5)
C7—C81.543 (4)C23—H230.9300
C8—C131.388 (4)C24—C251.390 (4)
C8—C91.405 (4)C24—H240.9300
C9—C101.375 (4)C25—H250.9300
C9—H90.9300
C1—O1—C4110.4 (2)C10—C9—H9119.7
C1—O2—C6114.3 (3)C8—C9—H9119.7
C2—O3—H3O110 (3)C9—C10—C11120.7 (3)
C3—O4—H4O108 (3)C9—C10—H10119.6
C5—O5—C7117.4 (2)C11—C10—H10119.6
O2—C1—O1113.3 (3)C12—C11—C10119.3 (3)
O2—C1—C2107.8 (3)C12—C11—H11120.4
O1—C1—C2105.0 (3)C10—C11—H11120.4
O2—C1—H1110.2C11—C12—C13120.4 (3)
O1—C1—H1110.2C11—C12—H12119.8
C2—C1—H1110.2C13—C12—H12119.8
O3—C2—C3112.4 (3)C8—C13—C12120.9 (3)
O3—C2—C1111.2 (3)C8—C13—H13119.6
C3—C2—C1103.2 (3)C12—C13—H13119.6
O3—C2—H2109.9C15—C14—C19117.5 (3)
C3—C2—H2109.9C15—C14—C7119.4 (3)
C1—C2—H2109.9C19—C14—C7123.1 (3)
O4—C3—C2113.0 (2)C16—C15—C14122.0 (3)
O4—C3—C4108.5 (3)C16—C15—H15119.0
C2—C3—C4104.2 (3)C14—C15—H15119.0
O4—C3—H3110.3C17—C16—C15119.9 (3)
C2—C3—H3110.3C17—C16—H16120.1
C4—C3—H3110.3C15—C16—H16120.1
O1—C4—C5109.7 (2)C16—C17—C18119.6 (3)
O1—C4—C3106.7 (2)C16—C17—H17120.2
C5—C4—C3114.6 (3)C18—C17—H17120.2
O1—C4—H4108.6C17—C18—C19120.5 (3)
C5—C4—H4108.6C17—C18—H18119.8
C3—C4—H4108.6C19—C18—H18119.8
O5—C5—C4108.3 (2)C18—C19—C14120.6 (3)
O5—C5—H5A110.0C18—C19—H19119.7
C4—C5—H5A110.0C14—C19—H19119.7
O5—C5—H5B110.0C21—C20—C25117.5 (3)
C4—C5—H5B110.0C21—C20—C7119.4 (3)
H5A—C5—H5B108.4C25—C20—C7122.9 (3)
O2—C6—H6A109.5C20—C21—C22121.7 (3)
O2—C6—H6B109.5C20—C21—H21119.2
H6A—C6—H6B109.5C22—C21—H21119.2
O2—C6—H6C109.5C23—C22—C21119.7 (4)
H6A—C6—H6C109.5C23—C22—H22120.2
H6B—C6—H6C109.5C21—C22—H22120.2
O5—C7—C14109.2 (2)C24—C23—C22119.6 (3)
O5—C7—C20110.8 (2)C24—C23—H23120.2
C14—C7—C20114.0 (2)C22—C23—H23120.2
O5—C7—C8104.2 (2)C23—C24—C25121.3 (3)
C14—C7—C8112.1 (3)C23—C24—H24119.3
C20—C7—C8106.2 (2)C25—C24—H24119.3
C13—C8—C9118.0 (3)C20—C25—C24120.2 (3)
C13—C8—C7123.5 (3)C20—C25—H25119.9
C9—C8—C7118.3 (3)C24—C25—H25119.9
C10—C9—C8120.7 (3)
C6—O2—C1—O179.8 (4)C9—C10—C11—C120.8 (6)
C6—O2—C1—C2164.6 (3)C10—C11—C12—C130.7 (5)
C4—O1—C1—O291.9 (3)C9—C8—C13—C121.9 (5)
C4—O1—C1—C225.4 (3)C7—C8—C13—C12177.6 (3)
O2—C1—C2—O3151.1 (3)C11—C12—C13—C81.3 (5)
O1—C1—C2—O387.9 (3)O5—C7—C14—C1553.9 (4)
O2—C1—C2—C388.2 (3)C20—C7—C14—C15178.4 (3)
O1—C1—C2—C332.8 (3)C8—C7—C14—C1560.9 (4)
O3—C2—C3—O4150.2 (3)O5—C7—C14—C19125.3 (3)
C1—C2—C3—O489.9 (3)C20—C7—C14—C190.8 (4)
O3—C2—C3—C492.3 (3)C8—C7—C14—C19119.9 (3)
C1—C2—C3—C427.7 (3)C19—C14—C15—C160.9 (5)
C1—O1—C4—C5132.3 (3)C7—C14—C15—C16179.9 (3)
C1—O1—C4—C37.6 (3)C14—C15—C16—C170.5 (6)
O4—C3—C4—O1107.2 (3)C15—C16—C17—C181.1 (6)
C2—C3—C4—O113.5 (3)C16—C17—C18—C190.3 (5)
O4—C3—C4—C5131.3 (3)C17—C18—C19—C141.1 (5)
C2—C3—C4—C5108.1 (3)C15—C14—C19—C181.7 (5)
C7—O5—C5—C4170.8 (2)C7—C14—C19—C18179.2 (3)
O1—C4—C5—O562.1 (3)O5—C7—C20—C21170.5 (3)
C3—C4—C5—O557.8 (3)C14—C7—C20—C2166.0 (4)
C5—O5—C7—C1445.8 (3)C8—C7—C20—C2157.9 (4)
C5—O5—C7—C2080.5 (3)O5—C7—C20—C255.8 (4)
C5—O5—C7—C8165.7 (2)C14—C7—C20—C25117.7 (4)
O5—C7—C8—C13128.3 (3)C8—C7—C20—C25118.4 (3)
C14—C7—C8—C1310.4 (4)C25—C20—C21—C221.2 (5)
C20—C7—C8—C13114.6 (3)C7—C20—C21—C22177.7 (3)
O5—C7—C8—C956.1 (3)C20—C21—C22—C230.2 (5)
C14—C7—C8—C9174.0 (3)C21—C22—C23—C240.8 (6)
C20—C7—C8—C961.0 (3)C22—C23—C24—C250.0 (6)
C13—C8—C9—C102.1 (5)C21—C20—C25—C241.9 (5)
C7—C8—C9—C10177.9 (3)C7—C20—C25—C24178.3 (3)
C8—C9—C10—C111.6 (5)C23—C24—C25—C201.4 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3O···O50.86 (2)2.10 (3)2.896 (3)153 (4)
O4—H4O···O3i0.83 (4)2.06 (4)2.877 (3)168 (4)
Symmetry code: (i) x1/2, y+1/2, z.

Experimental details

Crystal data
Chemical formulaC25H26O5
Mr406.46
Crystal system, space groupOrthorhombic, P212121
Temperature (K)295
a, b, c (Å)7.4286 (15), 8.1298 (16), 34.101 (7)
V3)2059.5 (7)
Z4
Radiation typeMo Kα
µ (mm1)0.09
Crystal size (mm)0.50 × 0.20 × 0.18
Data collection
DiffractometerRigaku R-AXIS RAPID IP
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.946, 0.992
No. of measured, independent and
observed [I > 2σ(I)] reflections
6994, 2110, 1522
Rint0.043
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.082, 1.01
No. of reflections2110
No. of parameters281
No. of restraints1
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.15, 0.16

Computer programs: DENZO (Otwinowski & Minor, 1997), SCALE (Otwinowski & Minor, 1997), SCALE, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), SHELXL97.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3O···O50.863 (19)2.10 (3)2.896 (3)153 (4)
O4—H4O···O3i0.83 (4)2.06 (4)2.877 (3)168 (4)
Symmetry code: (i) x1/2, y+1/2, z.
 

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