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A single-crystal neutron diffraction study of cyclodecaamylose (CA10) was carried out at 20 K. CA10 crystallizes with 27.18 water molecules [(C6H10O5)10·27.18H2O] in space group C2 with unit-cell constants a = 29.31 (5), b = 9.976 (10), c = 19.34 (2) Å, β = 121.07 (2)°. The asymmetric unit contains a half molecule of CA10 and 13.59 water molecules, the other half being related by a crystallographic twofold rotation axis. All H atoms except two water H atoms could be located from difference neutron-density maps; structure refinement converged at R = 0.635. Two of the five CH2—O6 groups and one of the 15 O2, O3 hydroxyl groups of CA10 are twofold orientationally disordered. A total of 13.59 water molecules in the asymmetric unit are distributed over 23 positions; 20 of which are in the CA10 cavity, and the other three occupy intermolecular interstices. Of the 123 symmetry-independent hydrogen bonds, 25 (= 20%) are three-centered and 7 (= 6%) are four-centered. Water molecules and O—H groups of CA10 form an extended network with cooperative O—H...O—H...O—H hydrogen bonds. They are arranged in 11 polygons with three, four, five, six and eight O—H bonds and in homodromic, antidromic and heterodromic arrangements. Nine polygons are located within the cavity and the others are outside.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101014288/jz0013sup1.cif
Contains datablocks global, ca10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101014288/jz0013ca10sup2.hkl
Contains datablock ca10

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101014288/jz0013finalsup3.fcf
Contains datablock final

CCDC reference: 179367

Computing details top

Data collection: ILL programs Hklgen and Mad; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: MOLSCRIPT, Xtal View; software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Cyclodecaamylose].27.18 H2 O top
Crystal data top
(C60H100O50)·27.18(H2O)Dx = 1.446 Mg m3
Mr = 2108.30Melting point: not measured K
Monoclinic, C2Neutron radiation, λ = 1.53200 Å
a = 29.31 (5) ÅCell parameters from 2193 reflections
b = 9.976 (10) Åθ = 3.6–50.9°
c = 19.34 (2) ŵ = 2.31 mm1
β = 121.07 (2)°T = 20 K
V = 4843 (11) Å3Plate, colorless
Z = 21.0 × 0.6 × 0.2 mm
F(000) = 546
Data collection top
D19
diffractometer
2355 reflections with I > 2σ(I)
Radiation source: neutron reactor at ILLRint = 0.048
Cu(220) monochromateorθmax = 50.8°, θmin = 2.7°
4x64 deg. position–sensitive detector (Thomas et. al., 1983) scansh = 2929
Absorption correction: analytical
?
k = 410
Tmin = 0.816, Tmax = 0.948l = 1919
3929 measured reflections3 standard reflections every 50 reflections
2494 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)] = 0.064H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.148 w = 1/[σ2(Fo2) + (0.054P)2 + 409.4507P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.073
2494 reflectionsΔρmax = 1.04 e Å3
736 parametersΔρmin = 1.08 e Å3
393 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0 (10)
Crystal data top
(C60H100O50)·27.18(H2O)V = 4843 (11) Å3
Mr = 2108.30Z = 2
Monoclinic, C2Neutron radiation, λ = 1.53200 Å
a = 29.31 (5) ŵ = 2.31 mm1
b = 9.976 (10) ÅT = 20 K
c = 19.34 (2) Å1.0 × 0.6 × 0.2 mm
β = 121.07 (2)°
Data collection top
D19
diffractometer
2355 reflections with I > 2σ(I)
Absorption correction: analytical
?
Rint = 0.048
Tmin = 0.816, Tmax = 0.948θmax = 50.8°
3929 measured reflections3 standard reflections every 50 reflections
2494 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.064H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.148 w = 1/[σ2(Fo2) + (0.054P)2 + 409.4507P]
where P = (Fo2 + 2Fc2)/3
S = 1.06Δρmax = 1.04 e Å3
2494 reflectionsΔρmin = 1.08 e Å3
736 parametersAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
393 restraintsAbsolute structure parameter: 0 (10)
Special details top

Experimental. atomic scattering factors were taken from Sears (1992).

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)
C110.2610 (3)0.0239 (9)0.2546 (5)0.0069 (18)*
H110.2751 (6)0.0462 (17)0.2933 (9)0.019 (4)*
C210.2251 (3)0.1351 (9)0.2551 (4)0.0075 (18)*
H210.2459 (6)0.2301 (18)0.2474 (9)0.020 (4)*
C310.2145 (3)0.1201 (9)0.1857 (4)0.0058 (17)*
H310.1922 (6)0.0267 (19)0.1957 (10)0.022 (4)*
C410.2676 (3)0.1117 (8)0.1061 (4)0.0030 (17)*
H410.2916 (6)0.206 (2)0.0931 (10)0.027 (4)*
C510.2993 (3)0.0090 (9)0.1116 (5)0.0076 (18)*
H510.2750 (6)0.0943 (19)0.1240 (9)0.023 (4)*
C61A0.3539 (5)0.0400 (11)0.0338 (7)0.004 (3)*0.77
H6110.3817 (10)0.051 (3)0.0172 (15)0.021*0.77
H6210.3472 (8)0.061 (2)0.0160 (13)0.020 (5)*0.77
C61B0.3548 (17)0.006 (3)0.040 (2)0.007*0.23
H6310.37490.09160.04880.024*0.23
H6410.35060.03220.01160.024*0.23
O210.1753 (4)0.1336 (11)0.3328 (5)0.010 (2)*
HO210.1558 (6)0.218 (2)0.3416 (10)0.026 (4)*
O310.1832 (3)0.2332 (10)0.1875 (5)0.005 (2)*
HO310.1492 (7)0.1995 (19)0.1982 (10)0.027 (4)*
O410.2605 (3)0.0779 (10)0.0403 (5)0.009 (2)*
O510.3085 (3)0.0159 (11)0.1762 (6)0.011 (2)*
O61A0.3773 (5)0.1505 (14)0.0470 (8)0.011 (3)*0.77
HO610.3998 (17)0.199 (5)0.001 (3)0.083 (11)*0.77
O61B0.3933 (14)0.100 (5)0.011 (2)0.005*0.23
HB610.42880.06270.01930.18 (5)*0.23
C120.2476 (3)0.1844 (8)0.0061 (5)0.0037 (17)*
H120.2182 (7)0.2521 (19)0.0540 (10)0.026 (4)*
C220.2253 (3)0.1196 (8)0.0411 (4)0.0020 (17)*
H220.2078 (6)0.1984 (18)0.0597 (9)0.018 (4)*
C320.2695 (3)0.0466 (7)0.1165 (4)0.0069 (18)*
H320.28370.03780.09590.024 (4)*
C420.3175 (3)0.1441 (9)0.1663 (4)0.0065 (18)*
H420.3063 (6)0.2221 (18)0.1915 (9)0.018 (4)*
C520.3373 (2)0.1983 (7)0.1123 (4)0.0057 (18)*
H520.34930.11360.08880.025 (4)*
C620.3844 (2)0.2930 (7)0.1577 (4)0.0070 (18)*
H6120.39360.33950.11470.028 (4)*
H6220.41950.23520.20160.031 (4)*
O220.1814 (3)0.0306 (11)0.0122 (5)0.009 (2)*
HO220.1956 (7)0.035 (2)0.0281 (10)0.026 (4)*
O320.2508 (4)0.0050 (10)0.1647 (5)0.009 (2)*
HO320.2301 (7)0.061 (2)0.1711 (10)0.026 (4)*
O420.3598 (3)0.0627 (10)0.2287 (5)0.011 (2)*
O520.2934 (4)0.2670 (10)0.0456 (5)0.012 (2)*
O620.3738 (4)0.3956 (12)0.1991 (5)0.014 (2)*
HB620.3917 (12)0.362 (3)0.2587 (9)0.014 (9)*0.40
HO620.3891 (13)0.480 (4)0.200 (2)0.036 (8)*0.60
C130.3834 (2)0.1035 (8)0.3102 (4)0.0080 (18)*
H130.35680.17420.31600.017 (4)*
C230.3881 (3)0.0258 (9)0.3565 (5)0.010 (2)*
H230.4052 (7)0.0027 (19)0.4212 (10)0.027 (4)*
C330.4243 (3)0.1221 (8)0.3461 (4)0.0053 (18)*
H330.4078 (7)0.138 (2)0.2808 (10)0.030 (4)*
C430.4795 (3)0.0542 (8)0.3811 (3)0.0095 (18)*
H430.49680.03820.44630.022 (4)*
C530.4742 (3)0.0808 (10)0.3407 (5)0.024 (2)*
H530.4617 (8)0.062 (2)0.2767 (7)0.042 (5)*
C63A0.5267 (5)0.1482 (18)0.3697 (13)0.030 (6)*0.57 (3)
H6130.5537 (12)0.091 (3)0.362 (2)0.042 (9)*0.57 (3)
H6230.5197 (15)0.243 (3)0.341 (2)0.042 (12)*0.57 (3)
C63B0.5228 (6)0.1701 (19)0.3954 (12)0.006 (6)*0.43 (3)
H6330.561 (2)0.115 (5)0.412 (4)0.046 (14)*0.43 (3)
H6430.5288 (17)0.202 (4)0.4552 (18)0.014 (12)*0.43 (3)
O230.3353 (3)0.0819 (10)0.3274 (6)0.007 (2)*
HO230.3133 (6)0.0730 (19)0.2687 (10)0.027 (4)*
O330.4294 (3)0.2439 (10)0.3873 (5)0.008 (2)*
HO330.4486 (7)0.308 (2)0.3749 (10)0.030 (4)*
O430.5135 (4)0.1403 (11)0.3693 (6)0.015 (2)*
O530.4344 (4)0.1631 (11)0.3418 (5)0.015 (2)*
O63A0.5436 (8)0.171 (2)0.4479 (12)0.008 (6)*0.57 (3)
HO630.5820 (9)0.211 (3)0.4792 (16)0.035 (9)*0.57 (3)
O63B0.5289 (10)0.295 (3)0.3636 (16)0.019 (8)*0.43 (3)
HB630.573 (2)0.320 (5)0.405 (3)0.060 (17)*0.43 (3)
C140.5506 (3)0.2137 (9)0.4389 (5)0.014 (2)*
H140.5367 (6)0.2228 (16)0.4798 (10)0.027 (4)*
C240.5574 (3)0.3560 (9)0.4131 (5)0.015 (2)*
H240.5833 (6)0.4122 (18)0.4658 (10)0.023 (4)*
C340.5846 (3)0.3455 (9)0.3647 (5)0.014 (2)*
H340.5597 (6)0.2839 (18)0.3098 (8)0.032 (4)*
C440.6380 (3)0.2687 (9)0.4162 (5)0.0076 (18)*
H440.6660 (6)0.3259 (17)0.4696 (9)0.018 (4)*
C540.6287 (3)0.1325 (8)0.4413 (4)0.0106 (18)*
H540.60450.07090.38720.024 (4)*
C640.6802 (2)0.0558 (7)0.5003 (4)0.0087 (18)*
H6140.66950.04500.51040.022 (4)*
H6240.70450.04400.47250.026 (4)*
O240.5055 (4)0.4158 (12)0.3672 (6)0.013 (2)*
HO240.5048 (9)0.479 (4)0.400 (2)0.031 (8)*0.60
HB240.5078 (14)0.529 (4)0.362 (2)0.009 (9)*0.40
O340.5935 (4)0.4747 (11)0.3459 (6)0.016 (2)*
HO340.6075 (6)0.4663 (19)0.3131 (10)0.027 (4)*
O440.6620 (3)0.2467 (10)0.3687 (5)0.009 (2)*
O540.6013 (3)0.1480 (10)0.4838 (5)0.010 (2)*
O640.7117 (3)0.1225 (10)0.5777 (5)0.009 (2)*
HO640.6929 (6)0.1125 (18)0.6057 (9)0.018 (4)*
C150.7032 (3)0.3388 (7)0.3807 (4)0.0046 (17)*
H150.70100.42820.41220.029 (4)*
C250.6924 (3)0.3791 (9)0.2986 (4)0.0068 (18)*
H250.7215 (6)0.4527 (18)0.3072 (9)0.019 (4)*
C350.6978 (3)0.2608 (9)0.2533 (4)0.0077 (18)*
H350.6658 (6)0.1830 (17)0.2408 (9)0.018 (4)*
C450.7549 (3)0.2024 (8)0.3099 (4)0.0038 (17)*
H450.7830 (6)0.2798 (18)0.3215 (9)0.020 (4)*
C550.7632 (3)0.1632 (8)0.3927 (4)0.0044 (18)*
H550.7341 (5)0.0838 (15)0.3848 (8)0.007 (3)*
C650.8200 (3)0.1139 (9)0.4519 (5)0.0101 (19)*
H6150.8241 (12)0.009 (3)0.4355 (18)0.012 (10)*0.75 (2)
H6250.8268 (12)0.099 (4)0.5149 (19)0.037 (12)*0.75 (2)
H6350.842 (4)0.193 (8)0.447 (6)0.044*0.25 (2)
H6450.825 (5)0.029 (9)0.425 (7)0.04 (4)*0.25 (2)
O250.6383 (4)0.4363 (11)0.2507 (6)0.015 (2)*
HO250.6426 (6)0.5206 (19)0.2258 (10)0.023 (4)*
O350.6909 (4)0.3053 (10)0.1795 (6)0.010 (2)*
HO350.6648 (8)0.259 (2)0.1360 (12)0.036 (5)*
O450.7687 (3)0.0965 (10)0.2754 (5)0.006 (2)*
O550.7541 (3)0.2802 (10)0.4273 (5)0.010 (2)*
O65A0.8611 (7)0.195 (2)0.4557 (11)0.032 (6)*0.75 (2)
HO650.8733 (8)0.157 (2)0.4249 (12)0.024 (6)*0.75 (2)
O65B0.8267 (19)0.121 (6)0.534 (3)0.012*0.25 (2)
HB650.859 (3)0.082 (10)0.579 (6)0.06 (3)*0.25 (2)
OW8A0.5483 (6)0.2909 (13)0.1440 (8)0.021 (3)*0.76
H1W80.5781 (11)0.338 (3)0.1806 (16)0.036 (6)*0.76
H2W80.5549 (17)0.201 (2)0.134 (3)0.086 (11)*0.76
OW8B0.5224 (13)0.443 (4)0.142 (2)0.016 (10)*0.24
H3W80.5593 (16)0.418 (11)0.174 (5)0.05 (2)*0.24
OW170.4731 (7)0.542 (2)0.0192 (10)0.018 (5)*0.50
H1170.467 (3)0.615 (4)0.055 (3)0.11 (2)*0.50
H2170.4360 (15)0.515 (6)0.027 (5)0.06 (2)*0.25
H3170.4807 (17)0.593 (5)0.033 (2)0.10 (4)*0.25
OW0A0.5771 (5)0.0344 (15)0.1350 (8)0.032 (4)*0.76
H1010.5909 (15)0.047 (2)0.1683 (18)0.139 (19)*0.76
H1020.598 (2)0.061 (4)0.111 (4)0.06 (2)*0.26
H1030.584 (2)0.113 (3)0.1697 (17)0.13 (3)*0.50
OW0B0.5336 (16)0.171 (4)0.083 (3)0.028 (11)*0.24
H1040.5035 (18)0.124 (9)0.0789 (19)0.060*0.24
H1050.5393 (7)0.111 (6)0.0474 (16)0.024 (16)*0.24
OW60.5801 (16)0.096 (5)0.237 (2)0.028 (11)*0.24
H1W60.605 (2)0.146 (8)0.284 (3)0.034 (18)*0.24
H2W60.567 (6)0.122 (17)0.183 (4)0.10 (4)*0.24
O11A0.4435 (8)0.238 (4)0.1084 (15)0.017 (6)*0.60
H1110.4815 (12)0.267 (4)0.1243 (17)0.025 (9)*0.60
H1120.4304 (17)0.295 (6)0.139 (3)0.069 (11)*0.60
O11B0.4392 (9)0.294 (4)0.0966 (16)0.009 (9)*0.40
H1130.4765 (11)0.316 (7)0.1260 (19)0.06 (2)*0.40
H1140.437 (3)0.197 (4)0.095 (7)0.09 (3)*0.40
OW10.4159 (4)0.3596 (9)0.2106 (5)0.010 (2)*
H1W10.4508 (7)0.362 (2)0.2616 (11)0.033 (5)*
H2W10.4029 (11)0.4497 (14)0.203 (3)0.056 (11)*0.60
H3W10.4250 (15)0.334 (5)0.1714 (18)0.024 (10)*0.40
O18A0.5306 (6)0.3281 (18)0.2257 (8)0.016 (4)*0.65
H1810.5394 (16)0.398 (3)0.2643 (19)0.073 (11)*0.65
H1820.5140 (11)0.249 (2)0.230 (2)0.17 (3)*0.65
O18B0.5243 (9)0.255 (3)0.2229 (17)0.013 (7)*0.35
H1830.5614 (10)0.272 (4)0.246 (2)0.013 (10)*0.35
H1840.516 (2)0.170 (4)0.196 (4)0.09 (2)*0.35
OW120.4649 (14)0.024 (3)0.1570 (19)0.069 (9)*0.50
H1210.462 (3)0.085 (7)0.116 (4)0.12 (2)*0.50
H1220.460 (4)0.069 (4)0.140 (6)0.08 (2)*0.30
H1230.501 (3)0.035 (4)0.175 (3)0.12 (5)*0.20
O13A0.4562 (8)0.219 (3)0.0760 (13)0.027 (6)*0.45
H1310.4809 (13)0.289 (3)0.1074 (17)0.13 (3)*0.45
H1320.4645 (18)0.167 (5)0.042 (3)0.058 (14)*0.45
O13B0.4816 (11)0.335 (3)0.0687 (18)0.016 (7)*0.32
H1330.503 (2)0.391 (5)0.0563 (15)0.045 (16)*0.32
H1340.493 (4)0.350 (8)0.131 (5)0.08 (2)*0.32
O13C0.471 (2)0.444 (6)0.086 (3)0.037*0.23
H1350.488 (3)0.458 (10)0.055 (4)0.031 (18)*0.23
OW50.3790 (4)0.3910 (13)0.0376 (6)0.037 (3)*
H1W50.3561 (6)0.437 (2)0.0243 (11)0.039 (5)*
H2W50.4090 (8)0.344 (3)0.0035 (14)0.095 (10)*
OW190.50000.0981 (19)0.00000.060 (6)*
H1190.4979 (16)0.170 (3)0.0309 (17)0.054 (12)*0.50
H2190.5258 (14)0.033 (3)0.0522 (14)0.049 (11)*0.50
OW140.403 (2)0.673 (5)0.043 (4)0.057*0.25
H1410.413 (2)0.703 (8)0.012 (4)0.021 (15)*0.25
H1420.401 (4)0.567 (5)0.051 (7)0.07 (3)*0.25
OW90.6200 (4)0.1557 (13)0.2598 (7)0.048 (4)*
H1W90.6513 (5)0.165 (2)0.3110 (9)0.050 (6)*
H2W90.5887 (7)0.204 (4)0.2454 (17)0.037 (9)*0.50
H3W90.6053 (17)0.068 (2)0.249 (3)0.054 (12)*0.50
OW20.7165 (4)0.1803 (11)0.4056 (6)0.016 (2)*
H1W20.7390 (7)0.242 (2)0.4029 (10)0.031 (4)*
H2W20.7159 (7)0.198 (2)0.4533 (12)0.038 (5)*
OW40.5056 (6)0.404 (2)0.4708 (10)0.019 (4)*0.60
H1W40.5152 (10)0.316 (3)0.4616 (14)0.038 (8)*0.60
H2W40.5411 (4)0.435 (4)0.5310 (19)0.056 (10)*0.60
OW70.6578 (4)0.3440 (13)0.1967 (6)0.020 (2)*
H1W70.6464 (8)0.353 (2)0.1412 (12)0.039 (5)*
H2W70.6423 (8)0.269 (3)0.2072 (13)0.046 (5)*
OW30.3958 (4)0.4242 (11)0.3652 (6)0.033 (3)*
H1W30.3724 (5)0.4978 (13)0.3515 (8)0.020 (4)*
H3W30.4313 (4)0.429 (2)0.4067 (14)0.026 (9)*0.45
H2W30.4046 (12)0.398 (3)0.3254 (15)0.039 (9)*0.55
Geometric parameters (Å, º) top
C11—O45i1.414 (13)C44—H441.091 (19)
C11—O511.437 (13)C54—O541.424 (12)
C11—C211.525 (12)C54—C641.544 (10)
C11—H111.051 (19)C54—H541.1000
C21—O211.458 (12)C64—O641.451 (12)
C21—C311.533 (11)C64—H6141.1000
C21—H211.10 (2)C64—H6241.1000
C31—O311.443 (13)O24—HO240.90 (5)
C31—C411.524 (11)O24—HB241.14 (4)
C31—H311.10 (2)O34—HO340.92 (3)
C41—O411.432 (12)O44—C151.437 (12)
C41—C511.557 (11)O64—HO640.96 (2)
C41—H411.12 (2)C15—O551.411 (12)
C51—O511.431 (13)C15—C251.506 (10)
C51—C61B1.49 (4)C15—H151.1000
C51—C61A1.560 (14)C25—O251.477 (13)
C51—H511.05 (2)C25—C351.526 (12)
C61A—O61A1.39 (2)C25—H251.07 (2)
C61A—H6111.15 (3)C35—O351.407 (13)
C61A—H6211.10 (2)C35—C451.565 (11)
C61B—O61B1.43 (6)C35—H351.142 (19)
C61B—H6311.1000C45—O451.416 (13)
C61B—H6411.1000C45—C551.541 (11)
O21—HO210.98 (3)C45—H451.07 (2)
O31—HO310.97 (2)C55—O551.437 (14)
O41—C121.402 (13)C55—C651.536 (11)
O61A—HO610.95 (6)C55—H551.114 (17)
O61B—HB610.9700C65—O65A1.42 (2)
C12—O521.447 (13)C65—O65B1.50 (5)
C12—C221.515 (11)C65—H6151.12 (3)
C12—H121.11 (2)C65—H6251.14 (3)
C22—O221.462 (13)C65—H6351.051 (11)
C22—C321.544 (10)C65—H6451.049 (11)
C22—H221.10 (2)O25—HO251.01 (3)
C32—O321.400 (12)O35—HO350.92 (3)
C32—C421.567 (11)O45—C11i1.414 (13)
C32—H321.1000O65A—HO650.92 (3)
C42—O421.452 (13)O65B—HB650.97 (13)
C42—C521.531 (10)OW8A—H1W80.92 (4)
C42—H421.06 (2)OW8A—H2W80.956 (11)
C52—O521.441 (12)OW8B—H3W80.959 (11)
C52—C621.522 (10)OW17—H1170.958 (11)
C52—H521.1000OW17—H2171.048 (11)
C62—O621.428 (13)OW17—H3171.046 (11)
C62—H6121.1000OW0A—H1010.988 (10)
C62—H6221.1000OW0A—H1020.971 (11)
O22—HO220.91 (3)OW0A—H1030.985 (11)
O32—HO320.95 (3)OW0B—H1040.96 (3)
O42—C131.414 (12)OW0B—H1051.00 (3)
O62—HB621.047 (11)OW6—H1W60.959 (11)
O62—HO620.95 (5)OW6—H2W60.960 (11)
C13—O531.419 (13)O11A—H1111.03 (4)
C13—C231.537 (12)O11A—H1121.02 (7)
C13—H131.1000O11B—H1130.960 (11)
C23—O231.458 (13)O11B—H1140.964 (11)
C23—C331.521 (12)OW1—H1W10.99 (2)
C23—H231.10 (2)OW1—H2W10.958 (11)
C33—O331.418 (13)OW1—H3W10.958 (11)
C33—C431.551 (11)O18A—H1810.957 (11)
C33—H331.11 (2)O18A—H1820.951 (11)
C43—O431.420 (13)O18B—H1830.952 (11)
C43—C531.525 (13)O18B—H1840.954 (11)
C43—H431.1000OW12—H1210.958 (11)
C53—O531.437 (14)OW12—H1220.961 (11)
C53—C63A1.497 (10)OW12—H1231.09 (8)
C53—C63B1.545 (10)O13A—H1310.962 (11)
C53—H531.109 (10)O13A—H1320.958 (11)
C63A—O63A1.35 (3)O13B—H1330.960 (11)
C63A—H6131.04 (3)O13B—H1341.07 (9)
C63A—H6231.06 (3)O13C—H1350.961 (11)
C63B—O63B1.44 (4)OW5—H1W50.951 (10)
C63B—H6331.12 (6)OW5—H2W50.950 (10)
C63B—H6431.12 (3)OW19—H1190.958 (11)
O23—HO230.98 (2)OW19—H2191.106 (11)
O33—HO330.96 (3)OW14—H1410.98 (12)
O43—C141.421 (14)OW14—H1421.06 (3)
O63A—HO631.04 (4)OW9—H1W90.946 (10)
O63B—HB631.14 (6)OW9—H2W90.945 (11)
C14—O541.437 (13)OW9—H3W90.953 (11)
C14—C241.551 (14)OW2—H1W20.92 (3)
C14—H141.06 (2)OW2—H2W20.94 (3)
C24—O241.437 (14)OW4—H1W40.96 (4)
C24—C341.513 (12)OW4—H2W41.13 (3)
C24—H241.06 (2)OW7—H1W70.95 (3)
C34—O341.400 (15)OW7—H2W70.95 (3)
C34—C441.554 (12)OW3—H1W30.944 (10)
C34—H341.113 (10)OW3—H3W30.931 (10)
C44—O441.434 (12)OW3—H2W30.966 (10)
C44—C541.514 (12)
O45i—C11—O51111.9 (8)O63B—C63B—H633103 (3)
O45i—C11—C21107.1 (6)C53—C63B—H633110 (3)
O51—C11—C21109.7 (7)H613—C63B—H63335 (3)
O45i—C11—H11112.8 (11)H623—C63B—H63399 (3)
O51—C11—H11103.8 (10)O63B—C63B—H643102 (3)
C21—C11—H11111.5 (11)C53—C63B—H643118 (2)
O21—C21—C11108.7 (7)H613—C63B—H643138 (3)
O21—C21—C31110.7 (7)H623—C63B—H643128 (3)
C11—C21—C31112.0 (6)H633—C63B—H643103 (4)
O21—C21—H21109.9 (11)C23—O23—HO23110.3 (12)
C11—C21—H21107.1 (11)C33—O33—HO33109.6 (14)
C31—C21—H21108.4 (10)C43—O43—C14114.6 (8)
O31—C31—C41111.9 (6)C13—O53—C53115.9 (8)
O31—C31—C21108.4 (7)C63A—O63A—H63344 (3)
C41—C31—C21109.0 (6)C63A—O63A—H643117 (3)
O31—C31—H31110.3 (11)H633—O63A—H643161 (4)
C41—C31—H31109.7 (11)C63A—O63A—HO63112 (2)
C21—C31—H31107.4 (10)H633—O63A—HO6382 (3)
O41—C41—C31111.6 (6)H643—O63A—HO63111 (4)
O41—C41—C51104.1 (6)C63B—O63B—H62360 (3)
C31—C41—C51107.9 (6)C63B—O63B—HB63104 (3)
O41—C41—H41111.1 (11)H623—O63B—HB63125 (5)
C31—C41—H41112.1 (11)O43—C14—O54112.6 (8)
C51—C41—H41109.7 (11)O43—C14—C24109.2 (7)
O51—C51—C61B101.3 (16)O54—C14—C24110.3 (7)
O51—C51—C41108.2 (7)O43—C14—H14110.4 (11)
C61B—C51—C41108.9 (10)O54—C14—H14105.3 (12)
O51—C51—C61A108.3 (8)C24—C14—H14108.9 (11)
C61B—C51—C61A13.6 (16)O24—C24—C34112.1 (8)
C41—C51—C61A116.0 (7)O24—C24—C14107.9 (7)
O51—C51—H51110.5 (11)C34—C24—C14109.4 (7)
C61B—C51—H51120.9 (19)O24—C24—H24112.1 (12)
C41—C51—H51106.5 (12)C34—C24—H24106.6 (11)
C61A—C51—H51107.2 (11)C14—C24—H24108.7 (12)
O61A—C61A—C51109.8 (10)O34—C34—C24109.0 (8)
O61A—C61A—H611109.4 (17)O34—C34—C44111.0 (7)
C51—C61A—H611109.8 (15)C24—C34—C44108.4 (7)
O61A—C61A—H621109.6 (16)O34—C34—H34112.2 (13)
C51—C61A—H621109.0 (13)C24—C34—H34109.4 (11)
H611—C61A—H621109.2 (19)C44—C34—H34106.7 (12)
O61B—C61B—C51130 (3)O44—C44—C54107.2 (7)
C51—C61B—H611138 (4)O44—C44—C34109.3 (7)
C51—C61B—H631104.9C54—C44—C34111.1 (6)
H611—C61B—H63199.6O44—C44—H44108.0 (11)
H621—C61B—H63197.4C54—C44—H44109.7 (11)
O61B—C61B—H641104.9C34—C44—H44111.4 (11)
C51—C61B—H641104.9O54—C54—C44109.6 (7)
H611—C61B—H641100.7O54—C54—C64104.7 (6)
H621—C61B—H64111.1C44—C54—C64114.4 (6)
H631—C61B—H641105.8O54—C54—H54109.3
C21—O21—HO21110.7 (13)C44—C54—H54109.3
C31—O31—HO31107.8 (14)C64—C54—H54109.3
C12—O41—C41116.1 (8)O64—C64—C54113.2 (6)
C51—O51—C11114.4 (7)O64—C64—H614108.9
C61A—O61A—HO61112 (3)C54—C64—H614108.9
C61B—O61B—HB61109.5O64—C64—H624108.9
O41—C12—O52112.2 (8)C54—C64—H624108.9
O41—C12—C22105.5 (7)H614—C64—H624107.8
O52—C12—C22111.1 (7)C24—O24—HO24104.8 (16)
O41—C12—H12110.5 (11)C24—O24—HB24112.0 (19)
O52—C12—H12105.8 (12)HO24—O24—HB2453 (2)
C22—C12—H12111.8 (11)C34—O34—HO34107.8 (15)
O22—C22—C12109.3 (7)C44—O44—C15116.5 (7)
O22—C22—C32112.5 (7)C54—O54—C14114.6 (7)
C12—C22—C32110.9 (6)C64—O64—HO64106.9 (12)
O22—C22—H22106.1 (11)O55—C15—O44111.2 (7)
C12—C22—H22108.2 (12)O55—C15—C25111.2 (6)
C32—C22—H22109.6 (10)O44—C15—C25107.3 (6)
O32—C32—C22112.1 (6)O55—C15—H15109.0
O32—C32—C42110.7 (6)O44—C15—H15109.0
C22—C32—C42109.7 (6)C25—C15—H15109.0
O32—C32—H32108.1O25—C25—C15109.7 (7)
C22—C32—H32108.1O25—C25—C35109.6 (7)
C42—C32—H32108.1C15—C25—C35111.8 (7)
O42—C42—C52107.7 (7)O25—C25—H25110.2 (12)
O42—C42—C32105.9 (7)C15—C25—H25107.5 (10)
C52—C42—C32109.6 (6)C35—C25—H25108.0 (11)
O42—C42—H42111.2 (11)O35—C35—C25109.6 (7)
C52—C42—H42111.9 (12)O35—C35—C45111.6 (7)
C32—C42—H42110.2 (11)C25—C35—C45106.1 (6)
O52—C52—C62110.3 (6)O35—C35—H35109.2 (10)
O52—C52—C42107.5 (6)C25—C35—H35109.3 (10)
C62—C52—C42112.0 (5)C45—C35—H35111.1 (10)
O52—C52—H52109.0O45—C45—C55111.7 (7)
C62—C52—H52109.0O45—C45—C35114.3 (6)
C42—C52—H52109.0C55—C45—C35111.0 (6)
O62—C62—C52112.0 (6)O45—C45—H45105.2 (11)
O62—C62—H612109.2C55—C45—H45105.9 (10)
C52—C62—H612109.2C35—C45—H45108.0 (11)
O62—C62—H622109.2O55—C55—C65107.7 (6)
C52—C62—H622109.2O55—C55—C45108.1 (7)
H612—C62—H622107.9C65—C55—C45112.6 (6)
C22—O22—HO22106.5 (13)O55—C55—H55109.2 (10)
C32—O32—HO32109.3 (14)C65—C55—H55109.4 (10)
C13—O42—C42118.9 (8)C45—C55—H55109.8 (9)
C52—O52—C12115.4 (8)O65A—C65—C55114.8 (9)
C62—O62—HB62104.9 (15)O65B—C65—C55106 (2)
C62—O62—HO62114 (2)O65A—C65—H615109.6 (19)
HB62—O62—HO62108 (3)C55—C65—H615108.9 (16)
O42—C13—O53113.8 (7)O65A—C65—H625110.0 (19)
O42—C13—C23104.6 (7)C55—C65—H625111.3 (17)
O53—C13—C23110.1 (7)H615—C65—H625101 (2)
O42—C13—H13109.4O65B—C65—H635108 (6)
O53—C13—H13109.4C55—C65—H635100 (6)
C23—C13—H13109.4O65B—C65—H645126 (8)
O23—C23—C33112.4 (7)C55—C65—H645106 (7)
O23—C23—C13109.9 (7)H635—C65—H645108 (10)
C33—C23—C13108.1 (6)C25—O25—HO25105.2 (12)
O23—C23—H23106.8 (11)C35—O35—HO35112.8 (15)
C33—C23—H23110.0 (11)C11i—O45—C45118.9 (7)
C13—C23—H23109.7 (12)C15—O55—C55115.3 (7)
O33—C33—C23110.2 (7)C65—O65A—HO65109 (2)
O33—C33—C43110.2 (6)C65—O65B—HB65117 (7)
C23—C33—C43108.0 (7)H1W8—OW8A—H2W8115 (3)
O33—C33—H33111.9 (13)H117—OW17—H217107 (6)
C23—C33—H33108.7 (11)H117—OW17—H317100.7 (14)
C43—C33—H33107.7 (11)H101—OW0A—H102112.6 (16)
O43—C43—C53110.3 (7)H101—OW0A—H103110.2 (15)
O43—C43—C33109.0 (7)H104—OW0B—H10597 (7)
C53—C43—C33110.8 (6)H1W6—OW6—H2W6126 (10)
O43—C43—H43108.9H111—O11A—H112110 (4)
C53—C43—H43108.9H113—O11B—H114106.0 (16)
C33—C43—H43108.9H1W1—OW1—H2W1104 (3)
O53—C53—C63A115.0 (11)H1W1—OW1—H3W1103 (3)
O53—C53—C43111.4 (7)H181—O18A—H182119.1 (18)
C63A—C53—C43113.0 (9)H183—O18B—H184108.5 (17)
O53—C53—C63B97.4 (10)H121—OW12—H122113 (8)
C43—C53—C63B110.1 (10)H121—OW12—H123106 (6)
O53—C53—H53108.0 (13)H131—O13A—H132117.0 (19)
C63A—C53—H53100.2 (15)H133—O13B—H134109 (6)
C43—C53—H53108.2 (13)H1W5—OW5—H2W5119.3 (16)
C63B—C53—H53121.1 (15)H119—OW19—H21996.0 (12)
O63A—C63A—C53102.0 (15)H141—OW14—H142116 (8)
O63A—C63A—H613112 (3)H1W9—OW9—H2W9121.9 (18)
C53—C63A—H613114 (2)H1W9—OW9—H3W9114 (3)
O63A—C63A—H623107 (3)H1W2—OW2—H2W2107.8 (19)
C53—C63A—H623109 (2)H1W4—OW4—H2W4104 (3)
H613—C63A—H623111 (3)H1W7—OW7—H2W7113 (2)
O63A—C63A—H63358 (4)H1W3—OW3—H3W3122.0 (14)
O63B—C63B—C53118.7 (18)H1W3—OW3—H2W3116.4 (16)
O45i—C11—C21—O2153.5 (9)C33—C43—C53—O5351.1 (8)
O51—C11—C21—O21175.2 (8)O43—C43—C53—C63A56.7 (12)
O45i—C11—C21—C3169.1 (8)C33—C43—C53—C63A177.5 (11)
O51—C11—C21—C3152.6 (9)O43—C43—C53—C63B81.2 (12)
O21—C21—C31—O3162.1 (9)C33—C43—C53—C63B158.1 (11)
C11—C21—C31—O31176.5 (6)O53—C53—C63A—O63A65.3 (17)
O21—C21—C31—C41175.9 (8)C43—C53—C63A—O63A64.2 (17)
C11—C21—C31—C4154.5 (8)O53—C53—C63B—O63B72 (2)
O31—C31—C41—O4168.7 (9)C43—C53—C63B—O63B171.9 (17)
C21—C31—C41—O41171.4 (7)C53—C43—O43—C14136.9 (8)
O31—C31—C41—C51177.6 (6)C33—C43—O43—C14101.3 (8)
C21—C31—C41—C5157.7 (8)O42—C13—O53—C5359.2 (10)
O41—C41—C51—O51179.9 (7)C23—C13—O53—C5358.0 (9)
C31—C41—C51—O5161.5 (8)C63A—C53—O53—C13176.5 (11)
O41—C41—C51—C61B70.5 (19)C43—C53—O53—C1353.2 (9)
C31—C41—C51—C61B170.8 (18)C63B—C53—O53—C13168.3 (11)
O41—C41—C51—C61A58.0 (9)C43—O43—C14—O5494.1 (10)
C31—C41—C51—C61A176.7 (7)C43—O43—C14—C24143.0 (8)
O51—C51—C61A—O61A58.8 (11)O43—C14—C24—O2454.7 (10)
C41—C51—C61A—O61A179.3 (9)O54—C14—C24—O24178.9 (8)
O51—C51—C61B—O61B60 (3)O43—C14—C24—C3467.5 (9)
C41—C51—C61B—O61B54 (4)O54—C14—C24—C3456.8 (9)
C31—C41—O41—C1282.4 (9)O24—C24—C34—O3463.9 (10)
C51—C41—O41—C12161.5 (7)C14—C24—C34—O34176.4 (7)
C61B—C51—O51—C11177.8 (13)O24—C24—C34—C44175.1 (8)
C41—C51—O51—C1163.4 (10)C14—C24—C34—C4455.4 (8)
C61A—C51—O51—C11170.1 (8)O34—C34—C44—O4465.6 (9)
O45i—C11—O51—C5160.3 (11)C24—C34—C44—O44174.6 (7)
C21—C11—O51—C5158.5 (10)O34—C34—C44—C54176.2 (7)
C41—O41—C12—O5276.5 (9)C24—C34—C44—C5456.5 (8)
C41—O41—C12—C22162.4 (6)O44—C44—C54—O54175.8 (6)
O41—C12—C22—O2254.6 (9)C34—C44—C54—O5456.4 (8)
O52—C12—C22—O22176.5 (8)O44—C44—C54—C6467.0 (8)
O41—C12—C22—C3270.1 (8)C34—C44—C54—C64173.7 (6)
O52—C12—C22—C3251.8 (9)O54—C54—C64—O6456.1 (8)
O22—C22—C32—O3262.0 (9)C44—C54—C64—O6464.0 (8)
C12—C22—C32—O32175.2 (7)C54—C44—O44—C15141.0 (7)
O22—C22—C32—C42174.6 (7)C34—C44—O44—C1598.5 (8)
C12—C22—C32—C4251.7 (8)C44—C54—O54—C1458.8 (9)
O32—C32—C42—O4263.7 (9)C64—C54—O54—C14178.0 (7)
C22—C32—C42—O42172.0 (6)O43—C14—O54—C5463.1 (11)
O32—C32—C42—C52179.7 (7)C24—C14—O54—C5459.2 (10)
C22—C32—C42—C5256.1 (8)C44—O44—C15—O55103.9 (8)
O42—C42—C52—O52174.0 (7)C44—O44—C15—C25134.3 (7)
C32—C42—C52—O5259.2 (8)O55—C15—C25—O25178.4 (8)
O42—C42—C52—C6264.7 (8)O44—C15—C25—O2556.5 (9)
C32—C42—C52—C62179.5 (6)O55—C15—C25—C3556.6 (8)
O52—C52—C62—O6268.3 (8)O44—C15—C25—C3565.2 (8)
C42—C52—C62—O6251.3 (8)O25—C25—C35—O3562.2 (9)
C52—C42—O42—C13116.3 (8)C15—C25—C35—O35176.0 (7)
C32—C42—O42—C13126.4 (8)O25—C25—C35—C45177.3 (7)
C62—C52—O52—C12175.3 (7)C15—C25—C35—C4555.4 (8)
C42—C52—O52—C1262.3 (9)O35—C35—C45—O4556.5 (10)
O41—C12—O52—C5258.7 (10)C25—C35—C45—O45175.7 (7)
C22—C12—O52—C5259.1 (10)O35—C35—C45—C55176.0 (7)
C42—O42—C13—O53103.4 (9)C25—C35—C45—C5556.7 (8)
C42—O42—C13—C23136.4 (8)O45—C45—C55—O55173.5 (7)
O42—C13—C23—O2361.0 (8)C35—C45—C55—O5557.5 (8)
O53—C13—C23—O23176.3 (8)O45—C45—C55—C6554.8 (9)
O42—C13—C23—C3361.9 (7)C35—C45—C55—C65176.3 (7)
O53—C13—C23—C3360.8 (8)O55—C55—C65—O65A72.6 (12)
O23—C23—C33—O3358.0 (9)C45—C55—C65—O65A46.4 (13)
C13—C23—C33—O33179.4 (6)O55—C55—C65—O65B44 (2)
O23—C23—C33—C43178.4 (7)C45—C55—C65—O65B163 (2)
C13—C23—C33—C4360.2 (7)C55—C45—O45—C11i64.2 (9)
O33—C33—C43—O4361.7 (8)C35—C45—O45—C11i63.0 (10)
C23—C33—C43—O43177.8 (7)O44—C15—O55—C5561.1 (9)
O33—C33—C43—C53176.8 (7)C25—C15—O55—C5558.5 (9)
C23—C33—C43—C5356.3 (7)C65—C55—O55—C15179.6 (7)
O43—C43—C53—O53171.9 (7)C45—C55—O55—C1558.5 (9)
Symmetry code: (i) x+1, y, z.

Experimental details

Crystal data
Chemical formula(C60H100O50)·27.18(H2O)
Mr2108.30
Crystal system, space groupMonoclinic, C2
Temperature (K)20
a, b, c (Å)29.31 (5), 9.976 (10), 19.34 (2)
β (°) 121.07 (2)
V3)4843 (11)
Z2
Radiation typeNeutron, λ = 1.53200 Å
µ (mm1)2.31
Crystal size (mm)1.0 × 0.6 × 0.2
Data collection
DiffractometerD19
diffractometer
Absorption correctionAnalytical
Tmin, Tmax0.816, 0.948
No. of measured, independent and
observed [I > 2σ(I)] reflections
3929, 2494, 2355
Rint0.048
θmax (°)50.8
(sin θ/λ)max1)0.506
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.064, 0.148, 1.06
No. of reflections2494
No. of parameters736
No. of restraints393
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
w = 1/[σ2(Fo2) + (0.054P)2 + 409.4507P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.04, 1.08
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter0 (10)

Computer programs: ILL programs Hklgen and Mad, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), MOLSCRIPT, Xtal View.

 

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