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The configurations of four of the six chiral centers in the title compound, C
18H
30O
6, are the same as those in pinnatoxin A, while one is inverted. The configuration of the sixth chiral center, which has no equivalent in pinnatoxin A, has also been determined. The overall molecular structure is stabilized by intramolecular O—H
O hydrogen bonds.
Supporting information
CCDC reference: 620667
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.005 Å
- R factor = 0.040
- wR factor = 0.041
- Data-to-parameter ratio = 7.8
checkCIF/PLATON results
No syntax errors found
Alert level C
REFNR01_ALERT_3_C Ratio of reflections to parameters is < 8 for a
non-centrosymmetric structure, where ZMAX < 18
sine(theta)/lambda 0.6497
Proportion of unique data used 0.7110
Ratio reflections to parameters 7.7880
PLAT089_ALERT_3_C Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 7.79
PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O5 - H18 ... 0.71 Ang.
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 27.50
From the CIF: _reflns_number_total 2377
Count of symmetry unique reflns 2380
Completeness (_total/calc) 99.87%
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 = . R
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C6 = . R
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C9 = . R
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C10 = . S
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C14 = . S
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C16 = . S
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
7 ALERT level G = General alerts; check
6 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
4 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
Data collection: MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1988); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: CrystalStructure (Molecular Structure Corporation and Rigaku, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CrystalStructure; molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: CrystalStructure.
(3
S,2'
S,5'
S,6'
R,8'
R,10'
R)-3-Hydroxy-4-[5'-hydroxy-10'-hydroxymethyl-5'-methyl-
1',7',9'-trioxadispiro[5.1.5.2]pentadec-2'-yl]but-1-ene
top
Crystal data top
C18H30O6 | F(000) = 744.00 |
Mr = 342.42 | Dx = 1.253 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.7107 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 22 reflections |
a = 11.822 (5) Å | θ = 10.3–13.5° |
b = 16.841 (8) Å | µ = 0.09 mm−1 |
c = 9.117 (5) Å | T = 296 K |
V = 1815.1 (15) Å3 | Block, colourless |
Z = 4 | 0.55 × 0.45 × 0.35 mm |
Data collection top
Rigaku AFC-5S diffractometer | Rint = 0.004 |
ω–2θ scans | θmax = 27.5° |
Absorption correction: ψ scan (North et al., 1968) | h = −15→0 |
Tmin = 0.941, Tmax = 0.968 | k = 0→21 |
2380 measured reflections | l = 0→11 |
2377 independent reflections | 3 standard reflections every 150 reflections |
1690 reflections with I > 2σ(I) | intensity decay: −0.3% |
Refinement top
Refinement on F | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.040 | w = 1/[0.0002Fo2 + σ2(Fo)] |
wR(F2) = 0.041 | (Δ/σ)max = 0.0004 |
S = 1.53 | Δρmax = 0.15 e Å−3 |
1690 reflections | Δρmin = −0.22 e Å−3 |
217 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
O1 | 0.5398 (2) | −0.0851 (1) | 0.4989 (2) | 0.0535 (7) | |
O2 | 0.4279 (2) | 0.0567 (1) | 0.5956 (2) | 0.0364 (5) | |
O3 | 0.3771 (2) | 0.1529 (1) | 0.4227 (2) | 0.0358 (5) | |
O4 | 0.5642 (2) | 0.1840 (1) | 0.3619 (2) | 0.0358 (5) | |
O5 | 0.4761 (2) | 0.3352 (1) | 0.2654 (3) | 0.0505 (6) | |
O6 | 0.6813 (2) | 0.0529 (1) | 0.4718 (2) | 0.0495 (6) | |
C1 | 0.4318 (3) | −0.0815 (2) | 0.5654 (4) | 0.0494 (9) | |
C2 | 0.3665 (3) | −0.0072 (2) | 0.5276 (3) | 0.0402 (8) | |
C3 | 0.2446 (3) | −0.0107 (2) | 0.5794 (4) | 0.053 (1) | |
C4 | 0.1877 (2) | 0.0694 (2) | 0.5609 (4) | 0.053 (1) | |
C5 | 0.2579 (3) | 0.1338 (2) | 0.6331 (4) | 0.0459 (9) | |
C6 | 0.3793 (3) | 0.1328 (2) | 0.5776 (3) | 0.0354 (8) | |
C7 | 0.4571 (3) | 0.1932 (2) | 0.6498 (3) | 0.0410 (8) | |
C8 | 0.4666 (3) | 0.2599 (2) | 0.5378 (3) | 0.0409 (8) | |
C9 | 0.4541 (3) | 0.2159 (2) | 0.3926 (3) | 0.0343 (8) | |
C10 | 0.4077 (3) | 0.2652 (1) | 0.2637 (3) | 0.0376 (8) | |
C11 | 0.2841 (3) | 0.2870 (2) | 0.2831 (4) | 0.057 (1) | |
C12 | 0.4239 (3) | 0.2209 (2) | 0.1184 (3) | 0.0458 (9) | |
C13 | 0.5441 (3) | 0.1916 (2) | 0.0984 (3) | 0.049 (1) | |
C14 | 0.5756 (3) | 0.1393 (2) | 0.2271 (3) | 0.0392 (8) | |
C15 | 0.6961 (3) | 0.1088 (2) | 0.2253 (3) | 0.0422 (9) | |
C16 | 0.7150 (3) | 0.0370 (2) | 0.3233 (3) | 0.0403 (8) | |
C17 | 0.8341 (3) | 0.0078 (2) | 0.3209 (4) | 0.0476 (9) | |
C18 | 0.9079 (3) | 0.0149 (2) | 0.4240 (4) | 0.059 (1) | |
H1 | 0.5729 | −0.0442 | 0.4973 | 0.064* | |
H2 | 0.3892 | −0.1263 | 0.5341 | 0.059* | |
H3 | 0.4407 | −0.0832 | 0.6689 | 0.059* | |
H4 | 0.3678 | −0.0008 | 0.4241 | 0.048* | |
H5 | 0.2051 | −0.0497 | 0.5243 | 0.063* | |
H6 | 0.2432 | −0.0246 | 0.6803 | 0.063* | |
H7 | 0.1825 | 0.0807 | 0.4590 | 0.063* | |
H8 | 0.1140 | 0.0682 | 0.6023 | 0.063* | |
H9 | 0.2258 | 0.1843 | 0.6125 | 0.055* | |
H10 | 0.2579 | 0.1251 | 0.7360 | 0.055* | |
H11 | 0.5295 | 0.1707 | 0.6677 | 0.049* | |
H12 | 0.4259 | 0.2117 | 0.7395 | 0.049* | |
H13 | 0.5375 | 0.2863 | 0.5431 | 0.049* | |
H14 | 0.4074 | 0.2973 | 0.5511 | 0.049* | |
H15 | 0.2614 | 0.3203 | 0.2043 | 0.069* | |
H16 | 0.2747 | 0.3145 | 0.3733 | 0.069* | |
H17 | 0.2388 | 0.2403 | 0.2837 | 0.069* | |
H18 | 0.4639 | 0.3609 | 0.2058 | 0.061* | |
H19 | 0.4053 | 0.2556 | 0.0398 | 0.055* | |
H20 | 0.3746 | 0.1764 | 0.1172 | 0.055* | |
H21 | 0.5941 | 0.2357 | 0.0950 | 0.059* | |
H22 | 0.5505 | 0.1619 | 0.0103 | 0.059* | |
H23 | 0.5260 | 0.0949 | 0.2299 | 0.047* | |
H24 | 0.7440 | 0.1500 | 0.2602 | 0.050* | |
H25 | 0.7164 | 0.0957 | 0.1274 | 0.051* | |
H26 | 0.6680 | −0.0043 | 0.2873 | 0.048* | |
H27 | 0.6399 | 0.0891 | 0.4758 | 0.059* | |
H28 | 0.8598 | −0.0160 | 0.2371 | 0.057* | |
H29 | 0.8890 | 0.0408 | 0.5077 | 0.071* | |
H30 | 0.9860 | −0.0132 | 0.4237 | 0.071* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
O1 | 0.058 (1) | 0.043 (1) | 0.060 (1) | 0.006 (1) | 0.003 (1) | −0.013 (1) |
O2 | 0.039 (1) | 0.0323 (9) | 0.038 (1) | 0.0032 (9) | −0.0001 (9) | −0.0013 (9) |
O3 | 0.042 (1) | 0.032 (1) | 0.033 (1) | −0.0062 (9) | −0.001 (1) | 0.0008 (9) |
O4 | 0.036 (1) | 0.039 (1) | 0.032 (1) | 0.0028 (9) | 0.0000 (9) | −0.0028 (9) |
O5 | 0.071 (2) | 0.031 (1) | 0.050 (1) | −0.010 (1) | −0.009 (1) | 0.007 (1) |
O6 | 0.054 (1) | 0.058 (1) | 0.036 (1) | 0.016 (1) | 0.009 (1) | 0.003 (1) |
C1 | 0.061 (2) | 0.038 (2) | 0.049 (2) | −0.001 (2) | 0.006 (2) | −0.004 (2) |
C2 | 0.047 (2) | 0.038 (2) | 0.036 (2) | −0.002 (1) | 0.002 (2) | −0.001 (1) |
C3 | 0.052 (2) | 0.049 (2) | 0.058 (2) | −0.011 (2) | 0.010 (2) | −0.002 (2) |
C4 | 0.036 (2) | 0.056 (2) | 0.066 (2) | −0.005 (2) | 0.008 (2) | −0.001 (2) |
C5 | 0.044 (2) | 0.045 (2) | 0.049 (2) | 0.005 (2) | 0.013 (2) | −0.000 (2) |
C6 | 0.041 (2) | 0.032 (1) | 0.033 (1) | 0.001 (1) | 0.003 (1) | 0.002 (1) |
C7 | 0.048 (2) | 0.042 (2) | 0.033 (2) | −0.000 (1) | 0.001 (1) | −0.006 (1) |
C8 | 0.047 (2) | 0.034 (1) | 0.042 (2) | −0.002 (1) | 0.001 (2) | −0.006 (1) |
C9 | 0.038 (2) | 0.029 (1) | 0.036 (2) | −0.003 (1) | 0.001 (1) | −0.003 (1) |
C10 | 0.041 (2) | 0.028 (1) | 0.044 (2) | −0.004 (1) | −0.004 (1) | 0.001 (1) |
C11 | 0.053 (2) | 0.054 (2) | 0.065 (2) | 0.008 (2) | −0.007 (2) | 0.009 (2) |
C12 | 0.058 (2) | 0.038 (2) | 0.041 (2) | 0.001 (2) | −0.014 (2) | 0.003 (1) |
C13 | 0.067 (2) | 0.046 (2) | 0.035 (2) | 0.007 (2) | 0.000 (2) | 0.001 (2) |
C14 | 0.049 (2) | 0.036 (1) | 0.032 (2) | 0.002 (1) | 0.002 (1) | −0.004 (1) |
C15 | 0.049 (2) | 0.044 (2) | 0.033 (2) | 0.001 (2) | 0.009 (2) | 0.002 (1) |
C16 | 0.044 (2) | 0.044 (2) | 0.033 (2) | 0.002 (1) | 0.004 (1) | −0.001 (1) |
C17 | 0.049 (2) | 0.050 (2) | 0.044 (2) | 0.007 (2) | 0.011 (2) | 0.003 (2) |
C18 | 0.055 (2) | 0.060 (2) | 0.062 (2) | 0.003 (2) | −0.001 (2) | 0.009 (2) |
Geometric parameters (Å, º) top
O1—C1 | 1.415 (4) | O6—H27 | 0.782 |
O2—C2 | 1.438 (3) | C1—H2 | 0.950 |
O2—C6 | 1.414 (3) | C1—H3 | 0.950 |
O3—C6 | 1.452 (3) | C2—H4 | 0.950 |
O3—C9 | 1.426 (3) | C3—H5 | 0.950 |
O4—C9 | 1.436 (4) | C3—H6 | 0.950 |
O4—C14 | 1.447 (3) | C4—H7 | 0.950 |
O5—C10 | 1.430 (3) | C4—H8 | 0.950 |
O6—C16 | 1.436 (4) | C5—H9 | 0.950 |
C1—C2 | 1.511 (4) | C5—H10 | 0.950 |
C2—C3 | 1.517 (4) | C7—H11 | 0.950 |
C3—C4 | 1.516 (4) | C7—H12 | 0.950 |
C4—C5 | 1.516 (4) | C8—H13 | 0.950 |
C5—C6 | 1.522 (4) | C8—H14 | 0.950 |
C6—C7 | 1.521 (4) | C11—H15 | 0.950 |
C7—C8 | 1.522 (4) | C11—H16 | 0.950 |
C9—C10 | 1.540 (4) | C11—H17 | 0.950 |
C10—C11 | 1.517 (4) | C12—H19 | 0.950 |
C10—C12 | 1.532 (4) | C12—H20 | 0.950 |
C8—C9 | 1.524 (4) | C13—H21 | 0.950 |
C12—C13 | 1.515 (5) | C13—H22 | 0.950 |
C13—C14 | 1.514 (4) | C14—H23 | 0.950 |
C14—C15 | 1.515 (4) | C15—H24 | 0.950 |
C15—C16 | 1.520 (4) | C15—H25 | 0.950 |
C16—C17 | 1.491 (4) | C16—H26 | 0.950 |
C17—C18 | 1.288 (5) | C17—H28 | 0.915 |
O1—H1 | 0.792 | C18—H29 | 0.906 |
O5—H18 | 0.710 | C18—H30 | 1.038 |
| | | |
O1···O5i | 2.764 (3) | O1···H18i | 2.08 |
O1···C10i | 3.532 (4) | O1···H19i | 2.78 |
O1···C12i | 3.463 (4) | O2···H28ii | 2.90 |
O1···C17ii | 3.541 (4) | O4···H9iv | 2.94 |
O5···C1iii | 3.500 (4) | O5···H8iv | 2.60 |
O5···C4iv | 3.369 (4) | O6···H16iv | 2.86 |
O5···C5iv | 3.497 (4) | O6···H28ii | 2.54 |
O6···C17ii | 3.349 (4) | C1···H18i | 2.93 |
| | | |
C2—O2—C6 | 115.0 (2) | C4—C3—H6 | 108.6 |
C6—O3—C9 | 110.4 (2) | H5—C3—H6 | 109.5 |
C9—O4—C14 | 116.4 (2) | C3—C4—H7 | 108.4 |
O1—C1—C2 | 113.5 (2) | C5—C4—H7 | 108.4 |
O2—C2—C1 | 105.3 (2) | C3—C4—H8 | 110.1 |
O2—C2—C3 | 112.0 (2) | C5—C4—H8 | 110.2 |
C1—C2—C3 | 112.5 (3) | H7—C4—H8 | 109.5 |
C2—C3—C4 | 110.6 (3) | C4—C5—H9 | 109.6 |
C3—C4—C5 | 110.2 (3) | C6—C5—H9 | 108.7 |
C4—C5—C6 | 111.4 (3) | C4—C5—H10 | 108.6 |
O2—C6—O3 | 109.4 (2) | C6—C5—H10 | 109.1 |
O2—C6—C5 | 110.8 (2) | H9—C5—H10 | 109.5 |
O3—C6—C5 | 107.6 (2) | C6—C7—H11 | 110.7 |
O2—C6—C7 | 108.1 (2) | C8—C7—H11 | 110.0 |
O3—C6—C7 | 106.0 (2) | C6—C7—H12 | 110.9 |
C5—C6—C7 | 114.8 (2) | C8—C7—H12 | 111.3 |
C6—C7—C8 | 104.3 (2) | H11—C7—H12 | 109.5 |
C7—C8—C9 | 102.6 (2) | C7—C8—H13 | 112.1 |
O3—C9—O4 | 109.7 (2) | C9—C8—H13 | 110.9 |
O3—C9—C8 | 104.8 (2) | C7—C8—H14 | 110.5 |
O4—C9—C8 | 105.3 (2) | C9—C8—H14 | 111.2 |
O3—C9—C10 | 108.7 (2) | H13—C8—H14 | 109.5 |
O4—C9—C10 | 112.1 (2) | C10—C11—H15 | 109.0 |
C8—C9—C10 | 115.9 (2) | C10—C11—H16 | 109.3 |
O5—C10—C9 | 103.5 (2) | H15—C11—H16 | 109.5 |
O5—C10—C11 | 110.1 (2) | C10—C11—H17 | 110.1 |
C9—C10—C11 | 112.6 (3) | H15—C11—H17 | 109.5 |
O5—C10—C12 | 109.8 (2) | H16—C11—H17 | 109.5 |
C9—C10—C12 | 110.7 (2) | C10—C12—H19 | 108.9 |
C11—C10—C12 | 109.8 (3) | C13—C12—H19 | 109.1 |
C10—C12—C13 | 112.3 (3) | C10—C12—H20 | 108.4 |
C12—C13—C14 | 109.1 (3) | C13—C12—H20 | 108.5 |
O4—C14—C13 | 109.4 (2) | H19—C12—H20 | 109.5 |
O4—C14—C15 | 105.8 (2) | C12—C13—H21 | 109.4 |
C13—C14—C15 | 114.8 (3) | C14—C13—H21 | 109.1 |
C14—C15—C16 | 113.7 (2) | C12—C13—H22 | 110.4 |
O6—C16—C15 | 111.4 (2) | C14—C13—H22 | 109.3 |
O6—C16—C17 | 109.7 (3) | H21—C13—H22 | 109.5 |
C15—C16—C17 | 113.1 (3) | O4—C14—H23 | 109.2 |
C16—C17—C18 | 126.7 (3) | C13—C14—H23 | 109.1 |
C1—O1—H1 | 114.6 | C15—C14—H23 | 108.3 |
C10—O5—H18 | 112.4 | C14—C15—H24 | 108.0 |
C16—O6—H27 | 111.3 | C16—C15—H24 | 107.2 |
O1—C1—H2 | 108.4 | C14—C15—H25 | 109.1 |
C2—C1—H2 | 108.6 | C16—C15—H25 | 109.3 |
O1—C1—H3 | 108.9 | H24—C15—H25 | 109.5 |
C2—C1—H3 | 108.0 | O6—C16—H26 | 107.5 |
H2—C1—H3 | 109.5 | C15—C16—H26 | 107.0 |
O2—C2—H4 | 109.6 | C17—C16—H26 | 107.8 |
C1—C2—H4 | 108.2 | C16—C17—H28 | 118.1 |
C3—C2—H4 | 109.2 | C18—C17—H28 | 115.2 |
C2—C3—H5 | 109.2 | C17—C18—H29 | 119.5 |
C4—C3—H5 | 109.8 | C17—C18—H30 | 123.9 |
C2—C3—H6 | 109.1 | H29—C18—H30 | 116.2 |
| | | |
C6—O2—C2—C1 | −178.2 (4) | C5—C6—C7—C8 | −101.8 (4) |
C6—O2—C2—C3 | −55.7 (5) | C6—C7—C8—C9 | −30.7 (4) |
C2—O2—C6—O3 | −62.6 (4) | C7—C8—C9—O3 | 34.1 (4) |
C2—O2—C6—C5 | 55.9 (5) | C7—C8—C9—O4 | −81.7 (4) |
C2—O2—C6—C7 | −177.6 (3) | C7—C8—C9—C10 | 153.8 (4) |
C9—O3—C6—O2 | −111.3 (4) | O3—C9—C10—O5 | 167.3 (3) |
C9—O3—C6—C5 | 128.2 (4) | O3—C9—C10—C11 | 48.4 (4) |
C9—O3—C6—C7 | 4.9 (5) | O3—C9—C10—C12 | −75.1 (4) |
C6—O3—C9—O4 | 87.9 (4) | O4—C9—C10—O5 | −71.3 (3) |
C6—O3—C9—C8 | −24.7 (4) | O4—C9—C10—C11 | 169.8 (3) |
C6—O3—C9—C10 | −149.2 (3) | O4—C9—C10—C12 | 46.4 (4) |
C14—O4—C9—O3 | 68.1 (4) | C8—C9—C10—O5 | 49.6 (5) |
C14—O4—C9—C8 | −179.6 (3) | C8—C9—C10—C11 | −69.3 (5) |
C14—O4—C9—C10 | −52.7 (5) | C8—C9—C10—C12 | 167.3 (4) |
C9—O4—C14—C13 | 58.8 (5) | O5—C10—C12—C13 | 63.4 (4) |
C9—O4—C14—C15 | −177.0 (3) | C9—C10—C12—C13 | −50.3 (5) |
O1—C1—C2—O2 | −67.1 (4) | C11—C10—C12—C13 | −175.3 (4) |
O1—C1—C2—C3 | 170.7 (3) | C10—C12—C13—C14 | 56.6 (5) |
O2—C2—C3—C4 | 52.8 (4) | C12—C13—C14—O4 | −58.4 (5) |
C1—C2—C3—C4 | 171.1 (4) | C12—C13—C14—C15 | −177.2 (4) |
C2—C3—C4—C5 | −52.6 (5) | O4—C14—C15—C16 | 78.1 (4) |
C3—C4—C5—C6 | 53.7 (5) | C13—C14—C15—C16 | −161.1 (4) |
C4—C5—C6—O2 | −54.6 (5) | C14—C15—C16—O6 | −55.6 (5) |
C4—C5—C6—O3 | 65.0 (5) | C14—C15—C16—C17 | −179.8 (4) |
C4—C5—C6—C7 | −177.3 (4) | O6—C16—C17—C18 | −17.7 (6) |
O2—C6—C7—C8 | 134.0 (3) | C15—C16—C17—C18 | 107.4 (5) |
O3—C6—C7—C8 | 16.8 (4) | | |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+3/2, −y, z+1/2; (iii) −x+1, y+1/2, −z+1/2; (iv) x+1/2, −y+1/2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O2 | 0.79 | 2.58 | 2.869 (3) | 103.8 |
O1—H1···O6 | 0.79 | 2.09 | 2.875 (3) | 170.0 |
O6—H27···O4 | 0.78 | 2.11 | 2.791 (3) | 146.4 |
O5—H18···O1iii | 0.71 | 2.08 | 2.764 (3) | 163.7 |
Symmetry code: (iii) −x+1, y+1/2, −z+1/2. |
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