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Reported in this paper are the syntheses and X-ray investigations of C2 symmetrical molecular ABA triads consisting of two steroid units (lithocholic acid or its methyl ester) joined together by linkers derived from bifunctional molecules such as terephthalic acid or N,N′-dicarboxypiperazine. Unlike their monomeric analogues, some of these compounds form inclusion complexes. All steroidal triads form crystals that are highly pseudo-centrosymmetric, in which the constituting molecules are held together either exclusively by van der Waals forces or form lattice inclusion complexes, with guest molecules hydrogen bonded to the host. The presence of carboxyl groups promotes the inclusion of pyridine molecules and the formation of the well known carboxylic acid...pyridine hydrogen bonds. Combined with pairwise face-to-face π-stacking between pyridine rings, these hydrogen-bond interactions lead to the formation of extended supramolecular tapes, analogous to polymers. The co-crystals of pyridine and a lithocholic acid triad undergo a symmetry-lowering phase transition from a P1 cell with Z = 1 to a P1 cell with Z = 2. The two structures are virtually the same, the two independent molecules in the larger cell being related by pseudo-translation. Changes in the type of spacer between two methyl lithocholate units from planar aromatic (terephthalic acid) to highly puckered aliphatic six-membered ring (N,N′-dicarboxypiperazine) bring about inclusion properties and changes in side-chain conformation in a crystal. Although the efficient packing of these highly elongated molecules is hindered, as indicated by low values of crystal density, ranging from 1.16 to 1.19 g cm−3, several very short C...O and H...H contacts are present in the crystals.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768108006514/bk5073sup1.cif
Contains datablocks 52Py120K, 52Py180K, 6, 70.5MeOH

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108006514/bk507352Py120Ksup2.hkl
Contains datablocks 52Py120K, 5+2Py(180K), 6, 7+0.5MeOH

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108006514/bk50735_2Py120Ksup3.hkl
Contains datablock 5+2Py_120K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108006514/bk50735_2Py_280Ksup4.hkl
Contains datablock 5+2Py(180K)

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108006514/bk50736sup5.hkl
Contains datablock 6

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108006514/bk50737_0.5MeOHsup6.hkl
Contains datablock 7+0.5MeOH

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768108006514/bk5073sup7.pdf
Supplementary material

CCDC references: 691550; 691551; 691552; 691553

Computing details top

Data collection: CrysAlis CCD v.1.168 (Oxford Diffraction,2001) for 52Py120K; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.23 beta (release 19.07.2004 CrysAlis171 .NET) for 52Py180K; Kuma KM-4 Software (Kuma Diffraction, 1995) for (6); CrysAlis CCD, Oxford Diffraction (2004a) for 70.5MeOH. Cell refinement: CrysAlis RED v.1.168 (Oxford Diffraction,2001) for 52Py120K; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.23 beta (release 19.07.2004 CrysAlis171 .NET) for 52Py180K; Kuma KM-4 Software (Kuma Diffraction, 1995) for (6); CrysAlis RED, Oxford Diffraction (2004b) for 70.5MeOH. Data reduction: CrysAlis RED v.1.168 (Oxford Diffraction,2001) for 52Py120K; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.23 beta (release 19.07.2004 CrysAlis171 .NET) for 52Py180K; Kuma KM-4 Software (Kuma Diffraction, 1995) for (6); CrysAlis RED, Oxford Diffraction (2004b) for 70.5MeOH. For all compounds, program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: Simens Analytical X-Ray Instruments (1989) for 52Py120K, 52Py180K; Simens Analytical X-Ray Instruments (1989) Mercury (Bruno at al. 2002) for (6), 70.5MeOH. For all compounds, software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
(52Py120K) bis(23-carboxy-24-nor-5beta-cholan-3alpha-yl)terephtalate top
Crystal data top
C56H82O8·2(C5H5N)F(000) = 1132
Mr = 1041.42Dx = 1.192 Mg m3
Triclinic, P1Melting point: 320 K
a = 12.8559 (6) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.5462 (7) ÅCell parameters from 22008 reflections
c = 17.4215 (9) Åθ = 3.4–25.1°
α = 75.390 (4)°µ = 0.08 mm1
β = 83.254 (4)°T = 120 K
γ = 82.771 (4)°Plate, colourless
V = 2900.9 (3) Å30.40 × 0.40 × 0.20 mm
Z = 2
Data collection top
Kuma KM4CCD κ-geometry
diffractometer
6040 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.069
Graphite monochromatorθmax = 25.1°, θmin = 3.4°
ω scansh = 1415
22008 measured reflectionsk = 1616
10239 independent reflectionsl = 2019
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)] = 0.078Riding
wR(F2) = 0.146 w = 1/[σ2(Fo2) + (0.042P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.009
10239 reflectionsΔρmax = 0.21 e Å3
1381 parametersΔρmin = 0.19 e Å3
153 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
C56H82O8·2(C5H5N)γ = 82.771 (4)°
Mr = 1041.42V = 2900.9 (3) Å3
Triclinic, P1Z = 2
a = 12.8559 (6) ÅMo Kα radiation
b = 13.5462 (7) ŵ = 0.08 mm1
c = 17.4215 (9) ÅT = 120 K
α = 75.390 (4)°0.40 × 0.40 × 0.20 mm
β = 83.254 (4)°
Data collection top
Kuma KM4CCD κ-geometry
diffractometer
6040 reflections with I > 2σ(I)
22008 measured reflectionsRint = 0.069
10239 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.078Riding
wR(F2) = 0.146Δρmax = 0.21 e Å3
S = 1.02Δρmin = 0.19 e Å3
10239 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
1381 parametersAbsolute structure parameter: 0 (10)
153 restraints
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
C10.7548 (6)0.6269 (6)0.5199 (5)0.039 (2)
H1A0.75400.69330.48370.047*
H1B0.80350.62430.55830.047*
C20.7923 (6)0.5486 (6)0.4743 (5)0.038 (2)
H2A0.80180.48270.51080.046*
H2B0.85940.56410.44630.046*
C30.7178 (6)0.5443 (6)0.4154 (5)0.0334 (19)
H30.71500.60840.37610.040*
C40.6103 (5)0.5282 (6)0.4527 (4)0.0319 (19)
H4A0.61010.46050.48700.038*
H4B0.56470.53300.41180.038*
C50.5662 (5)0.6095 (6)0.5018 (5)0.0317 (19)
H5A0.56210.67520.46450.038*
C60.4537 (5)0.5922 (5)0.5391 (4)0.0367 (19)
H6A0.41200.58260.49980.044*
H6B0.42310.65260.55590.044*
C70.4509 (5)0.5000 (6)0.6102 (5)0.044 (2)
H7A0.46750.43850.59160.053*
H7B0.38080.49900.63620.053*
C80.5276 (6)0.5009 (6)0.6729 (5)0.034 (2)
H80.50440.55830.69580.041*
C90.6379 (5)0.5148 (6)0.6328 (5)0.034 (2)
H90.65540.45960.60670.041*
C100.6428 (6)0.6142 (6)0.5626 (5)0.039 (2)
C110.7218 (6)0.5006 (6)0.6907 (4)0.037 (2)
H11A0.71520.55950.71280.045*
H11B0.79000.49660.66200.045*
C120.7146 (6)0.4036 (6)0.7591 (5)0.044 (2)
H12A0.76420.40280.79640.053*
H12B0.73350.34430.73790.053*
C130.6053 (6)0.3976 (6)0.8020 (4)0.0318 (19)
C140.5285 (5)0.4054 (5)0.7377 (4)0.0276 (18)
H140.55270.35010.71270.033*
C150.4274 (6)0.3750 (6)0.7880 (5)0.051 (2)
H15A0.38500.34680.75860.061*
H15B0.38760.43340.80260.061*
C160.4599 (5)0.2942 (6)0.8626 (4)0.044 (2)
H16A0.44190.22790.86150.053*
H16B0.42540.31210.90990.053*
C170.5804 (5)0.2940 (5)0.8609 (4)0.0346 (19)
H170.61120.24090.83530.041*
C180.5792 (8)0.4809 (6)0.8482 (5)0.061 (3)
H18A0.62870.47040.88900.073*
H18B0.50730.47730.87390.073*
H18C0.58490.54840.81160.073*
C190.6079 (7)0.7101 (6)0.5952 (5)0.053 (2)
H19A0.65830.71610.63150.063*
H19B0.53790.70400.62400.063*
H19C0.60530.77130.55090.063*
C200.6210 (5)0.2634 (6)0.9447 (4)0.0291 (18)
H200.58930.31250.97400.035*
C210.7404 (6)0.2607 (7)0.9419 (5)0.058 (3)
H21A0.76330.22820.99500.070*
H21B0.76070.33080.92500.070*
H21C0.77390.22120.90400.070*
C220.5894 (6)0.1592 (5)0.9872 (4)0.0357 (19)
H22A0.62190.11130.95710.043*
H22B0.51460.16030.98730.043*
C230.6169 (6)0.1205 (6)1.0734 (4)0.038 (2)
H23A0.59780.17281.10220.046*
H23B0.69140.10151.07410.046*
C240.5588 (6)0.0291 (6)1.1107 (5)0.037 (2)
O10.5924 (4)0.0577 (4)1.1037 (3)0.0509 (15)
O20.4661 (4)0.0519 (4)1.1481 (3)0.0498 (16)
H2O0.41060.01601.17180.060*
C311.1772 (5)0.0204 (6)0.0004 (4)0.0295 (19)
H31A1.19720.04120.03850.035*
H31B1.24040.05050.02470.035*
C321.1117 (5)0.0945 (6)0.0423 (5)0.039 (2)
H32A1.09860.16020.00610.047*
H32B1.14900.10340.08430.047*
C331.0087 (5)0.0520 (6)0.0773 (4)0.034 (2)
H331.02300.01020.11720.040*
C340.9489 (5)0.0284 (6)0.0163 (4)0.0324 (19)
H34A0.92900.09060.02180.039*
H34B0.88600.00130.04190.039*
C351.0169 (6)0.0464 (6)0.0260 (5)0.033 (2)
H351.03270.10810.01400.040*
C360.9543 (6)0.0746 (6)0.0853 (4)0.042 (2)
H36A0.88810.09620.05930.050*
H36B0.99270.13090.10390.050*
C370.9332 (6)0.0188 (6)0.1580 (5)0.050 (2)
H37A0.88860.07250.14010.059*
H37B0.89760.00200.19590.059*
C381.0374 (5)0.0593 (6)0.1972 (4)0.0295 (19)
H381.07790.00740.21990.035*
C391.1032 (5)0.0838 (6)0.1378 (4)0.0265 (18)
H391.06090.13570.11630.032*
C401.1224 (6)0.0081 (6)0.0649 (4)0.031 (2)
C411.2011 (5)0.1327 (6)0.1811 (4)0.0311 (19)
H41A1.24730.08150.20080.037*
H41B1.23710.15380.14360.037*
C421.1791 (5)0.2247 (6)0.2496 (5)0.036 (2)
H42A1.24470.24830.27550.043*
H42B1.14030.27930.22910.043*
C431.1169 (5)0.2000 (5)0.3113 (4)0.0246 (17)
C441.0169 (6)0.1562 (6)0.2648 (5)0.0341 (19)
H440.98300.20760.23850.041*
C450.9447 (6)0.1534 (7)0.3273 (4)0.050 (2)
H45A0.87210.15770.30670.060*
H45B0.96120.09220.34630.060*
C460.9681 (6)0.2491 (6)0.3945 (5)0.048 (2)
H46A0.90880.30020.39780.058*
H46B0.98300.23160.44510.058*
C471.0654 (5)0.2902 (5)0.3725 (4)0.0280 (17)
H471.03990.34350.34570.034*
C481.1811 (6)0.1233 (6)0.3539 (4)0.044 (2)
H48A1.24770.15010.37840.053*
H48B1.14120.11290.39530.053*
H48C1.19570.05780.31530.053*
C491.1929 (6)0.0959 (6)0.0914 (5)0.044 (2)
H49A1.19580.15680.04680.052*
H49B1.26400.07520.10820.052*
H49C1.16390.11170.13600.052*
C501.1343 (5)0.3409 (6)0.4493 (4)0.0270 (18)
H501.15550.28990.47910.032*
C511.2332 (5)0.3794 (5)0.4325 (4)0.0317 (17)
H51A1.26610.41970.48220.038*
H51B1.28250.32090.41000.038*
H51C1.21470.42250.39440.038*
C521.0669 (5)0.4294 (5)0.5006 (4)0.0349 (19)
H52A1.05150.48340.47310.042*
H52B1.00120.40630.50610.042*
C531.1214 (6)0.4731 (6)0.5857 (4)0.038 (2)
H53A1.06790.49360.62230.046*
H53B1.16810.41940.60190.046*
C541.1820 (6)0.5641 (6)0.5937 (4)0.0316 (19)
O31.1571 (4)0.6297 (4)0.5585 (3)0.0548 (16)
O41.2666 (4)0.5595 (4)0.6451 (3)0.0467 (16)
H4O1.32240.62520.65120.056*
O50.7617 (4)0.4647 (4)0.3765 (3)0.0470 (16)
O60.7168 (4)0.5508 (4)0.2575 (3)0.0487 (16)
C1L0.7567 (6)0.4758 (6)0.2995 (5)0.0279 (18)
C2L0.8123 (5)0.3864 (5)0.2712 (5)0.0292 (19)
C3L0.7952 (5)0.3765 (5)0.1958 (5)0.0302 (19)
H3L0.75140.42850.16240.036*
C4L0.8409 (5)0.2929 (6)0.1702 (4)0.0309 (19)
H4L0.82910.28680.11820.037*
C5L0.9038 (6)0.2159 (6)0.2161 (5)0.0289 (19)
C6L0.9219 (5)0.2265 (6)0.2911 (4)0.0318 (19)
H6L0.96730.17520.32360.038*
C7L0.8749 (5)0.3104 (6)0.3192 (5)0.036 (2)
H7L0.88580.31620.37140.044*
C8L0.9616 (6)0.1262 (6)0.1911 (5)0.035 (2)
O70.9443 (4)0.1273 (4)0.1156 (3)0.0395 (14)
O81.0160 (4)0.0615 (4)0.2302 (3)0.0382 (14)
C1'0.7230 (5)0.1603 (6)0.4729 (5)0.034 (2)
H1'A0.71470.22480.51130.041*
H1'B0.75950.17010.43080.041*
C2'0.7908 (6)0.0824 (6)0.5124 (5)0.037 (2)
H2'A0.80210.01800.47420.045*
H2'B0.85810.10630.53300.045*
C3'0.7320 (5)0.0686 (6)0.5799 (5)0.0312 (19)
H3'0.72400.13170.61990.037*
C4'0.6232 (5)0.0315 (5)0.5459 (4)0.0261 (18)
H4'A0.63320.03400.50890.031*
H4'B0.58630.02290.58820.031*
C5'0.5578 (5)0.1065 (6)0.5036 (4)0.0268 (18)
H5'0.54700.17030.54250.032*
C6'0.4488 (5)0.0710 (5)0.4733 (4)0.037 (2)
H6'A0.41890.05420.51580.044*
H6'B0.40360.12610.45800.044*
C7'0.4515 (5)0.0216 (5)0.4024 (4)0.0297 (17)
H7'A0.48710.08010.41950.036*
H7'B0.38080.03630.38280.036*
C8'0.5080 (5)0.0039 (6)0.3364 (4)0.0283 (18)
H8'0.46670.04870.31500.034*
C9'0.6205 (5)0.0330 (6)0.3687 (4)0.0302 (19)
H9'0.65990.02130.38930.036*
C10'0.6133 (5)0.1284 (6)0.4365 (4)0.0265 (18)
C11'0.6760 (6)0.0428 (7)0.2960 (5)0.041 (2)
H11C0.63950.09790.27500.049*
H11D0.74610.06040.31490.049*
C12'0.6834 (6)0.0535 (6)0.2294 (5)0.043 (2)
H12C0.71700.04040.18710.051*
H12D0.72620.10720.24840.051*
C13'0.5751 (5)0.0900 (6)0.1975 (5)0.033 (2)
C14'0.5243 (5)0.1004 (6)0.2675 (5)0.0304 (19)
H14'0.57180.14790.29040.036*
C15'0.4266 (5)0.1561 (5)0.2338 (4)0.0310 (17)
H15C0.40900.19450.26900.037*
H15D0.36730.10880.22420.037*
C16'0.4612 (5)0.2282 (5)0.1548 (4)0.0326 (18)
H16C0.46480.29860.15710.039*
H16D0.41190.21780.11090.039*
C17'0.5740 (5)0.2001 (5)0.1445 (4)0.0292 (17)
H17'0.62480.24290.16980.035*
C18'0.5093 (6)0.0135 (6)0.1545 (5)0.043 (2)
H18D0.50330.05470.19100.052*
H18E0.54390.01060.10800.052*
H18F0.43890.03590.13720.052*
C19'0.5543 (6)0.2225 (6)0.4110 (5)0.048 (2)
H19D0.59710.24550.37710.057*
H19E0.48720.20410.38120.057*
H19F0.54110.27780.45840.057*
C20'0.5950 (6)0.2236 (6)0.0570 (5)0.041 (2)
H20'0.54120.18470.03060.050*
C21'0.6995 (6)0.1945 (6)0.0442 (5)0.045 (2)
H21D0.75590.22880.07420.054*
H21E0.71020.21580.01260.054*
H21F0.70070.12010.06290.054*
C22'0.5852 (6)0.3374 (6)0.0169 (5)0.041 (2)
H22C0.63550.37790.04460.049*
H22D0.51630.35280.02320.049*
C23'0.6046 (6)0.3712 (7)0.0717 (5)0.047 (2)
H23C0.57320.31900.09800.056*
H23D0.67840.38270.07880.056*
C24'0.5513 (7)0.4671 (8)0.1042 (5)0.049 (3)
O1'0.5867 (4)0.5525 (5)0.0939 (3)0.0502 (16)
O2'0.4586 (4)0.4522 (4)0.1426 (4)0.0525 (17)
H2'O0.41480.52250.14530.063*
C31'1.1654 (6)0.4774 (6)1.0036 (5)0.039 (2)
H31C1.18000.54180.96610.047*
H31D1.23120.45681.03120.047*
C32'1.1180 (6)0.3981 (6)0.9575 (4)0.037 (2)
H32C1.10560.33240.99390.045*
H32D1.16550.39200.92070.045*
C33'1.0138 (6)0.4318 (6)0.9124 (5)0.037 (2)
H33'1.02490.49480.87270.045*
C34'0.9407 (6)0.4406 (6)0.9703 (5)0.040 (2)
H34C0.92730.37521.00680.047*
H34D0.87490.46070.94240.047*
C35'0.9892 (6)0.5200 (6)1.0160 (5)0.038 (2)
H35'1.00120.58440.97810.046*
C36'0.9099 (7)0.5332 (6)1.0730 (5)0.058 (3)
H36C0.84360.54731.04300.069*
H36D0.93580.59101.09470.069*
C37'0.8932 (6)0.4382 (7)1.1411 (5)0.058 (3)
H37C0.86320.38111.11970.070*
H37D0.84470.44981.17500.070*
C38'0.9980 (6)0.4123 (6)1.1902 (5)0.038 (2)
H38'1.02520.46831.21370.045*
C39'1.0792 (5)0.3992 (5)1.1328 (4)0.0243 (17)
H39'1.04960.34341.10970.029*
C40'1.0963 (6)0.4941 (6)1.0653 (4)0.0274 (18)
C41'1.1839 (6)0.3654 (6)1.1829 (5)0.040 (2)
H41C1.21900.42171.20320.048*
H41D1.22950.34921.14890.048*
C42'1.1641 (5)0.2716 (6)1.2548 (4)0.0303 (18)
H42C1.23020.25631.28460.036*
H42D1.13580.21341.23430.036*
C43'1.0893 (5)0.2887 (6)1.3100 (4)0.0252 (18)
C44'0.9863 (5)0.3157 (6)1.2549 (4)0.036 (2)
H44'0.96510.26021.22950.043*
C45'0.9065 (6)0.3105 (7)1.3148 (5)0.060 (3)
H45C0.83640.29591.29200.072*
H45D0.91080.37391.33070.072*
C46'0.9367 (6)0.2223 (7)1.3856 (4)0.052 (2)
H46C0.88420.16471.38900.062*
H46D0.94230.24421.43430.062*
C47'1.0451 (5)0.1918 (5)1.3715 (4)0.0299 (17)
H47'1.03060.13691.34480.036*
C48'1.1356 (6)0.3748 (6)1.3500 (5)0.041 (2)
H48D1.20400.35841.37860.050*
H48E1.08770.38191.38760.050*
H48F1.14490.43931.30940.050*
C49'1.1502 (8)0.5859 (6)1.0917 (5)0.062 (3)
H49D1.22080.57131.11680.074*
H49E1.10930.60221.13010.074*
H49F1.15610.64451.04540.074*
C50'1.1099 (5)0.1528 (6)1.4503 (4)0.0303 (19)
H50'1.12100.20711.47760.036*
C51'1.2176 (5)0.1279 (5)1.4373 (4)0.0333 (18)
H51D1.25720.10411.48890.040*
H51E1.25600.18961.40660.040*
H51F1.20900.07411.40790.040*
C52'1.0516 (5)0.0633 (5)1.5027 (4)0.0324 (18)
H52C1.04070.00711.47750.039*
H52D0.98360.08231.50740.039*
C53'1.1048 (5)0.0263 (5)1.5864 (4)0.0318 (19)
H53C1.05160.00441.62320.038*
H53D1.14800.08321.60070.038*
C54'1.1709 (6)0.0579 (6)1.5952 (5)0.041 (2)
O3'1.1506 (4)0.1304 (4)1.5641 (3)0.0500 (15)
O4'1.2585 (4)0.0543 (4)1.6444 (3)0.0382 (14)
H4'O1.30190.13771.65890.046*
O5'0.7945 (4)0.0103 (4)0.6132 (3)0.0339 (13)
O6'0.7153 (4)0.0549 (4)0.7284 (3)0.0431 (15)
C1L'0.7733 (5)0.0114 (6)0.6877 (5)0.0313 (19)
C2L'0.8260 (5)0.1037 (6)0.7146 (5)0.032 (2)
C3L'0.8084 (6)0.1108 (6)0.7885 (5)0.036 (2)
H3L'0.76480.05810.82140.044*
C4L'0.8547 (6)0.1955 (6)0.8169 (5)0.0328 (19)
H4L'0.84300.20020.86920.039*
C5L'0.9173 (6)0.2720 (6)0.7693 (5)0.0306 (19)
C6L'0.9315 (6)0.2630 (6)0.6940 (4)0.036 (2)
H6L'0.97420.31620.66060.043*
C7L'0.8871 (6)0.1795 (6)0.6647 (5)0.034 (2)
H7L'0.89810.17500.61220.041*
C8L'0.9643 (6)0.3634 (7)0.7971 (6)0.040 (2)
O7'0.9646 (5)0.3474 (4)0.8762 (4)0.0567 (18)
O8'1.0044 (5)0.4401 (5)0.7550 (4)0.0586 (18)
N1S0.3380 (4)0.0907 (5)1.1720 (4)0.0329 (16)
C1S0.3615 (7)0.1692 (7)1.1371 (5)0.050 (2)
H1S0.42730.17371.10520.060*
C2S0.2966 (7)0.2425 (7)1.1435 (6)0.060 (3)
H2S0.31760.29911.11940.072*
C3S0.2004 (6)0.2365 (6)1.1884 (5)0.047 (2)
H3S0.15290.28801.19520.056*
C4S0.1741 (6)0.1540 (6)1.2226 (5)0.038 (2)
H4S0.10690.14571.25200.046*
C5S0.2442 (6)0.0810 (6)1.2126 (4)0.035 (2)
H5S0.22550.02431.23690.042*
N2S1.3949 (5)0.7043 (5)0.6634 (4)0.0320 (16)
C6S1.3765 (6)0.7827 (7)0.6287 (5)0.041 (2)
H6S1.31320.78860.59420.049*
C7S1.4432 (6)0.8556 (6)0.6389 (5)0.045 (2)
H7S1.42630.91200.61400.053*
C8S1.5350 (6)0.8496 (6)0.6878 (5)0.039 (2)
H8S1.58400.90010.69620.047*
C9S1.5551 (6)0.7680 (6)0.7237 (4)0.0332 (19)
H9S1.61800.76100.75830.040*
C10S1.4850 (6)0.6963 (7)0.7086 (5)0.039 (2)
H10S1.50030.63910.73270.047*
N3S0.3331 (5)0.5966 (6)0.1648 (4)0.0462 (19)
C11S0.3548 (7)0.6751 (7)0.1325 (5)0.047 (2)
H11S0.42030.68030.10040.057*
C12S0.2873 (7)0.7505 (7)0.1446 (5)0.051 (2)
H12S0.30490.80600.11880.061*
C13S0.1935 (7)0.7433 (8)0.1917 (6)0.062 (3)
H13S0.14700.79630.20210.074*
C14S0.1687 (7)0.6606 (7)0.2239 (6)0.053 (3)
H14S0.10320.65290.25550.063*
C15S0.2406 (7)0.5894 (6)0.2106 (5)0.043 (2)
H15S0.22410.53120.23350.051*
N4S1.3885 (5)0.1931 (5)1.6612 (4)0.0361 (17)
C16S1.3664 (6)0.2743 (6)1.6283 (5)0.040 (2)
H16S1.30190.27751.59460.048*
C17S1.4298 (6)0.3521 (6)1.6405 (5)0.043 (2)
H17S1.41120.40691.61410.052*
C18S1.5203 (6)0.3477 (7)1.6886 (5)0.044 (2)
H18S1.56450.40251.69910.053*
C19S1.5486 (6)0.2672 (7)1.7228 (5)0.051 (3)
H19S1.61340.26271.75580.061*
C20S1.4782 (6)0.1930 (6)1.7088 (5)0.039 (2)
H20S1.49620.13641.73330.047*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.035 (4)0.036 (5)0.041 (6)0.013 (4)0.007 (4)0.004 (4)
C20.039 (5)0.040 (5)0.027 (5)0.011 (4)0.004 (4)0.007 (4)
C30.039 (4)0.021 (4)0.037 (5)0.009 (3)0.010 (4)0.004 (4)
C40.037 (4)0.038 (5)0.023 (5)0.011 (3)0.003 (3)0.020 (4)
C50.036 (4)0.026 (4)0.026 (5)0.012 (3)0.001 (4)0.002 (4)
C60.039 (4)0.033 (4)0.024 (5)0.012 (3)0.009 (3)0.006 (4)
C70.023 (4)0.061 (6)0.049 (6)0.006 (4)0.001 (4)0.014 (5)
C80.040 (4)0.024 (4)0.039 (5)0.002 (3)0.005 (4)0.012 (4)
C90.031 (4)0.034 (5)0.039 (5)0.008 (4)0.014 (4)0.004 (4)
C100.052 (5)0.036 (5)0.028 (5)0.005 (4)0.003 (4)0.012 (4)
C110.051 (5)0.033 (5)0.026 (5)0.025 (4)0.008 (4)0.000 (4)
C120.042 (5)0.047 (5)0.045 (6)0.019 (4)0.008 (4)0.004 (4)
C130.047 (5)0.028 (4)0.026 (5)0.003 (4)0.017 (4)0.011 (4)
C140.032 (4)0.016 (4)0.033 (5)0.001 (3)0.002 (3)0.005 (3)
C150.037 (4)0.067 (6)0.038 (5)0.001 (4)0.002 (4)0.001 (5)
C160.046 (5)0.046 (5)0.033 (5)0.006 (4)0.009 (4)0.008 (4)
C170.043 (4)0.026 (4)0.034 (5)0.008 (3)0.012 (4)0.011 (4)
C180.131 (9)0.024 (5)0.027 (6)0.021 (5)0.001 (5)0.001 (4)
C190.085 (6)0.043 (5)0.038 (6)0.008 (5)0.009 (5)0.022 (5)
C200.035 (4)0.033 (4)0.018 (4)0.004 (3)0.009 (3)0.000 (3)
C210.052 (5)0.077 (7)0.042 (6)0.024 (5)0.025 (4)0.009 (5)
C220.043 (4)0.042 (5)0.018 (4)0.009 (4)0.009 (3)0.006 (4)
C230.052 (5)0.028 (4)0.028 (5)0.008 (4)0.007 (4)0.002 (4)
C240.049 (5)0.029 (5)0.034 (5)0.005 (4)0.005 (4)0.007 (4)
O10.056 (3)0.035 (3)0.057 (4)0.001 (3)0.004 (3)0.005 (3)
O20.041 (3)0.059 (4)0.044 (4)0.002 (3)0.007 (3)0.009 (3)
C310.028 (4)0.034 (5)0.025 (5)0.004 (3)0.005 (3)0.002 (4)
C320.041 (5)0.047 (5)0.040 (6)0.005 (4)0.002 (4)0.033 (4)
C330.036 (4)0.039 (5)0.021 (5)0.008 (4)0.000 (4)0.004 (4)
C340.029 (4)0.035 (4)0.024 (4)0.004 (3)0.001 (3)0.009 (4)
C350.049 (5)0.032 (5)0.021 (5)0.011 (4)0.001 (4)0.008 (4)
C360.042 (4)0.050 (5)0.037 (5)0.024 (4)0.002 (4)0.009 (4)
C370.051 (5)0.067 (6)0.036 (5)0.034 (4)0.004 (4)0.010 (5)
C380.031 (4)0.034 (4)0.022 (4)0.020 (3)0.001 (3)0.005 (3)
C390.031 (4)0.026 (4)0.025 (4)0.003 (3)0.005 (3)0.015 (3)
C400.033 (4)0.035 (5)0.028 (5)0.010 (4)0.001 (4)0.010 (4)
C410.027 (4)0.051 (5)0.021 (4)0.008 (4)0.002 (3)0.019 (4)
C420.025 (4)0.035 (5)0.049 (6)0.014 (4)0.002 (4)0.008 (4)
C430.022 (4)0.027 (4)0.028 (5)0.009 (3)0.003 (3)0.013 (3)
C440.034 (4)0.044 (5)0.029 (5)0.009 (4)0.002 (3)0.019 (4)
C450.048 (5)0.078 (6)0.020 (5)0.029 (5)0.007 (4)0.011 (4)
C460.044 (5)0.064 (6)0.038 (5)0.017 (4)0.010 (4)0.007 (5)
C470.027 (4)0.035 (4)0.026 (4)0.001 (3)0.005 (3)0.013 (4)
C480.069 (6)0.040 (5)0.020 (5)0.011 (4)0.011 (4)0.006 (4)
C490.049 (5)0.051 (5)0.032 (5)0.008 (4)0.010 (4)0.016 (4)
C500.028 (4)0.035 (4)0.014 (4)0.000 (3)0.005 (3)0.004 (3)
C510.031 (4)0.034 (4)0.027 (5)0.007 (3)0.005 (3)0.004 (4)
C520.028 (4)0.040 (5)0.038 (5)0.001 (3)0.003 (3)0.016 (4)
C530.048 (4)0.046 (5)0.019 (4)0.007 (4)0.003 (3)0.003 (4)
C540.044 (4)0.035 (4)0.018 (4)0.004 (4)0.009 (3)0.008 (4)
O30.071 (4)0.042 (4)0.056 (4)0.002 (3)0.006 (3)0.030 (3)
O40.055 (4)0.060 (4)0.021 (3)0.011 (3)0.017 (3)0.010 (3)
O50.080 (4)0.024 (3)0.025 (4)0.021 (3)0.005 (3)0.000 (3)
O60.071 (4)0.028 (3)0.041 (4)0.014 (3)0.010 (3)0.003 (3)
C1L0.031 (4)0.028 (4)0.023 (5)0.002 (3)0.008 (3)0.009 (4)
C2L0.020 (4)0.024 (4)0.035 (5)0.002 (3)0.006 (3)0.004 (4)
C3L0.028 (4)0.021 (4)0.035 (5)0.008 (3)0.001 (3)0.001 (4)
C4L0.037 (4)0.033 (5)0.018 (5)0.003 (4)0.002 (3)0.000 (4)
C5L0.030 (4)0.028 (4)0.025 (4)0.005 (3)0.005 (3)0.003 (4)
C6L0.032 (4)0.029 (4)0.026 (5)0.005 (3)0.014 (3)0.005 (4)
C7L0.025 (4)0.044 (5)0.036 (5)0.006 (4)0.004 (4)0.010 (4)
C8L0.045 (5)0.033 (4)0.023 (5)0.005 (4)0.011 (4)0.006 (4)
O70.049 (3)0.035 (3)0.025 (3)0.015 (3)0.006 (3)0.004 (3)
O80.056 (4)0.030 (3)0.023 (3)0.015 (3)0.010 (3)0.004 (3)
C1'0.025 (4)0.048 (5)0.027 (5)0.000 (4)0.004 (3)0.011 (4)
C2'0.032 (4)0.042 (5)0.034 (5)0.006 (4)0.007 (4)0.002 (4)
C3'0.025 (4)0.025 (4)0.039 (5)0.002 (3)0.014 (3)0.008 (4)
C4'0.025 (4)0.021 (4)0.026 (4)0.008 (3)0.005 (3)0.008 (3)
C5'0.033 (4)0.026 (4)0.024 (5)0.001 (3)0.002 (3)0.012 (4)
C6'0.018 (4)0.049 (5)0.048 (5)0.004 (3)0.000 (3)0.021 (4)
C7'0.028 (4)0.027 (4)0.028 (5)0.010 (3)0.000 (3)0.006 (3)
C8'0.030 (4)0.023 (4)0.033 (5)0.009 (3)0.002 (3)0.008 (4)
C9'0.023 (4)0.051 (5)0.021 (5)0.015 (4)0.001 (3)0.011 (4)
C10'0.030 (4)0.027 (4)0.022 (5)0.003 (3)0.001 (3)0.005 (4)
C11'0.032 (4)0.064 (6)0.032 (5)0.018 (4)0.003 (4)0.019 (5)
C12'0.042 (5)0.050 (5)0.040 (5)0.018 (4)0.028 (4)0.001 (4)
C13'0.024 (4)0.042 (5)0.034 (5)0.012 (3)0.002 (3)0.011 (4)
C14'0.025 (4)0.038 (5)0.033 (5)0.006 (3)0.004 (3)0.019 (4)
C15'0.033 (4)0.036 (4)0.030 (5)0.009 (3)0.006 (3)0.014 (4)
C16'0.029 (4)0.033 (4)0.036 (5)0.005 (3)0.000 (3)0.011 (4)
C17'0.020 (3)0.045 (4)0.030 (4)0.003 (3)0.005 (3)0.021 (4)
C18'0.054 (5)0.044 (5)0.035 (5)0.011 (4)0.005 (4)0.020 (4)
C19'0.068 (6)0.031 (5)0.043 (6)0.010 (4)0.001 (4)0.007 (4)
C20'0.036 (5)0.041 (5)0.053 (6)0.000 (4)0.013 (4)0.019 (5)
C21'0.053 (5)0.045 (5)0.038 (5)0.002 (4)0.012 (4)0.009 (4)
C22'0.037 (4)0.049 (5)0.040 (5)0.001 (4)0.004 (4)0.018 (4)
C23'0.036 (5)0.050 (6)0.054 (6)0.004 (4)0.005 (4)0.021 (5)
C24'0.042 (5)0.071 (7)0.025 (5)0.004 (5)0.001 (4)0.006 (5)
O1'0.044 (3)0.049 (4)0.053 (4)0.000 (3)0.003 (3)0.005 (3)
O2'0.048 (4)0.024 (3)0.082 (5)0.006 (3)0.013 (3)0.013 (3)
C31'0.040 (5)0.041 (5)0.035 (5)0.004 (4)0.002 (4)0.015 (4)
C32'0.058 (5)0.028 (4)0.022 (5)0.016 (4)0.009 (4)0.008 (4)
C33'0.055 (5)0.030 (5)0.028 (5)0.007 (4)0.001 (4)0.018 (4)
C34'0.033 (4)0.047 (5)0.030 (5)0.005 (4)0.010 (4)0.000 (4)
C35'0.057 (5)0.038 (5)0.023 (5)0.021 (4)0.001 (4)0.009 (4)
C36'0.076 (6)0.057 (6)0.038 (6)0.042 (5)0.007 (5)0.014 (5)
C37'0.060 (6)0.084 (7)0.032 (5)0.048 (5)0.003 (4)0.001 (5)
C38'0.043 (5)0.039 (5)0.038 (5)0.013 (4)0.011 (4)0.014 (4)
C39'0.034 (4)0.024 (4)0.016 (4)0.007 (3)0.006 (3)0.008 (3)
C40'0.042 (4)0.027 (4)0.015 (4)0.005 (3)0.001 (3)0.009 (3)
C41'0.040 (5)0.042 (5)0.033 (5)0.005 (4)0.010 (4)0.005 (4)
C42'0.030 (4)0.040 (5)0.017 (4)0.006 (3)0.001 (3)0.002 (4)
C43'0.020 (3)0.042 (4)0.019 (4)0.004 (3)0.000 (3)0.018 (3)
C44'0.033 (4)0.043 (5)0.032 (5)0.015 (4)0.004 (4)0.006 (4)
C45'0.044 (5)0.092 (7)0.043 (6)0.038 (5)0.020 (4)0.009 (5)
C46'0.043 (5)0.081 (6)0.024 (5)0.036 (4)0.014 (4)0.020 (4)
C47'0.031 (4)0.035 (4)0.028 (5)0.000 (3)0.009 (3)0.014 (4)
C48'0.058 (5)0.039 (5)0.030 (5)0.004 (4)0.005 (4)0.015 (4)
C49'0.128 (9)0.022 (5)0.024 (5)0.003 (5)0.008 (5)0.002 (4)
C50'0.038 (4)0.023 (4)0.032 (5)0.010 (4)0.006 (4)0.013 (4)
C51'0.024 (4)0.036 (4)0.038 (5)0.001 (3)0.000 (3)0.009 (4)
C52'0.037 (4)0.030 (4)0.025 (5)0.004 (3)0.016 (3)0.007 (3)
C53'0.029 (4)0.029 (4)0.034 (5)0.002 (3)0.004 (4)0.004 (4)
C54'0.034 (5)0.041 (5)0.036 (6)0.017 (4)0.001 (4)0.001 (4)
O3'0.062 (4)0.038 (3)0.051 (4)0.013 (3)0.017 (3)0.018 (3)
O4'0.030 (3)0.026 (3)0.058 (4)0.003 (2)0.000 (3)0.015 (3)
O5'0.032 (3)0.046 (3)0.027 (3)0.005 (2)0.004 (2)0.018 (3)
O6'0.045 (3)0.042 (4)0.043 (4)0.009 (3)0.005 (3)0.017 (3)
C1L'0.018 (4)0.038 (5)0.037 (6)0.001 (3)0.004 (4)0.012 (4)
C2L'0.029 (4)0.033 (5)0.028 (5)0.004 (3)0.007 (4)0.002 (4)
C3L'0.042 (5)0.037 (5)0.025 (5)0.001 (4)0.012 (4)0.004 (4)
C4L'0.040 (4)0.036 (4)0.021 (4)0.001 (4)0.007 (3)0.011 (4)
C5L'0.040 (4)0.026 (4)0.026 (5)0.003 (3)0.013 (3)0.013 (4)
C6L'0.043 (5)0.040 (5)0.020 (5)0.007 (4)0.002 (4)0.003 (4)
C7L'0.036 (4)0.039 (5)0.028 (5)0.010 (4)0.007 (4)0.011 (4)
C8L'0.030 (5)0.043 (6)0.039 (6)0.003 (4)0.004 (4)0.003 (5)
O7'0.085 (4)0.046 (4)0.032 (4)0.016 (3)0.014 (3)0.016 (3)
O8'0.088 (5)0.052 (4)0.039 (4)0.016 (4)0.014 (4)0.025 (4)
N1S0.034 (4)0.037 (4)0.029 (4)0.001 (3)0.001 (3)0.013 (3)
C1S0.043 (5)0.076 (7)0.040 (6)0.009 (5)0.011 (4)0.030 (5)
C2S0.047 (6)0.054 (6)0.090 (8)0.010 (5)0.020 (5)0.041 (6)
C3S0.043 (5)0.030 (5)0.061 (7)0.000 (4)0.016 (5)0.005 (5)
C4S0.044 (5)0.032 (5)0.046 (6)0.002 (4)0.020 (4)0.016 (4)
C5S0.040 (4)0.044 (5)0.017 (4)0.005 (4)0.004 (3)0.005 (4)
N2S0.034 (4)0.023 (4)0.033 (4)0.004 (3)0.002 (3)0.005 (3)
C6S0.034 (5)0.062 (6)0.029 (5)0.018 (4)0.009 (4)0.024 (5)
C7S0.051 (5)0.037 (5)0.054 (6)0.002 (4)0.021 (5)0.020 (5)
C8S0.034 (4)0.032 (4)0.045 (5)0.015 (4)0.002 (4)0.009 (4)
C9S0.038 (5)0.034 (5)0.024 (5)0.006 (4)0.002 (4)0.006 (4)
C10S0.041 (5)0.057 (6)0.018 (5)0.002 (4)0.007 (4)0.010 (4)
N3S0.042 (4)0.061 (5)0.037 (5)0.001 (4)0.014 (4)0.013 (4)
C11S0.054 (6)0.050 (6)0.033 (6)0.006 (5)0.010 (4)0.003 (5)
C12S0.054 (6)0.055 (6)0.045 (6)0.010 (5)0.010 (5)0.023 (5)
C13S0.035 (5)0.076 (7)0.088 (8)0.006 (5)0.014 (5)0.045 (6)
C14S0.043 (5)0.050 (6)0.064 (7)0.008 (5)0.001 (5)0.011 (5)
C15S0.055 (6)0.028 (5)0.044 (6)0.009 (4)0.008 (5)0.012 (4)
N4S0.030 (4)0.047 (5)0.025 (4)0.002 (3)0.001 (3)0.001 (3)
C16S0.029 (4)0.030 (5)0.049 (6)0.000 (4)0.009 (4)0.007 (4)
C17S0.052 (5)0.032 (5)0.038 (6)0.005 (4)0.006 (4)0.002 (4)
C18S0.038 (5)0.040 (5)0.056 (7)0.005 (4)0.005 (4)0.012 (5)
C19S0.033 (5)0.064 (7)0.040 (6)0.003 (5)0.014 (4)0.005 (5)
C20S0.043 (5)0.036 (5)0.043 (6)0.010 (4)0.016 (4)0.011 (4)
Geometric parameters (Å, º) top
C1—C21.481 (10)C8'—H8'0.9600
C1—C101.549 (10)C9'—C10'1.517 (10)
C1—H1A0.9600C9'—C11'1.567 (10)
C1—H1B0.9599C9'—H9'0.9600
C2—C31.499 (10)C10'—C19'1.536 (10)
C2—H2A0.9600C11'—C12'1.512 (11)
C2—H2B0.9601C11'—H11C0.9600
C3—O51.437 (8)C11'—H11D0.9600
C3—C41.475 (10)C12'—C13'1.531 (9)
C3—H30.9600C12'—H12C0.9601
C4—C51.570 (9)C12'—H12D0.9600
C4—H4A0.9601C13'—C14'1.493 (10)
C4—H4B0.9600C13'—C18'1.540 (10)
C5—C61.535 (9)C13'—C17'1.544 (10)
C5—C101.546 (11)C14'—C15'1.527 (9)
C5—H5A0.9600C14'—H14'0.9602
C6—C71.523 (10)C15'—C16'1.549 (9)
C6—H6A0.9599C15'—H15C0.9600
C6—H6B0.9601C15'—H15D0.9601
C7—C81.558 (10)C16'—C17'1.586 (8)
C7—H7A0.9600C16'—H16C0.9600
C7—H7B0.9600C16'—H16D0.9600
C8—C141.487 (10)C17'—C20'1.527 (10)
C8—C91.517 (9)C17'—H17'0.9600
C8—H80.9601C18'—H18D0.9800
C9—C111.524 (10)C18'—H18E0.9800
C9—C101.577 (11)C18'—H18F0.9800
C9—H90.9600C19'—H19D0.9800
C10—C191.543 (10)C19'—H19E0.9800
C11—C121.539 (10)C19'—H19F0.9800
C11—H11A0.9600C20'—C21'1.502 (9)
C11—H11B0.9600C20'—C22'1.537 (10)
C12—C131.513 (10)C20'—H20'0.9600
C12—H12A0.9601C21'—H21D0.9800
C12—H12B0.9599C21'—H21E0.9800
C13—C181.527 (10)C21'—H21F0.9800
C13—C141.553 (9)C22'—C23'1.537 (10)
C13—C171.560 (10)C22'—H22C0.9601
C14—C151.520 (9)C22'—H22D0.9602
C14—H140.9602C23'—C24'1.495 (11)
C15—C161.535 (10)C23'—H23C0.9599
C15—H15A0.9601C23'—H23D0.9600
C15—H15B0.9601C24'—O1'1.237 (10)
C16—C171.546 (9)C24'—O2'1.315 (9)
C16—H16A0.9601O2'—H2'O1.1539
C16—H16B0.9600C31'—C32'1.526 (10)
C17—C201.548 (10)C31'—C40'1.547 (10)
C17—H170.9599C31'—H31C0.9600
C18—H18A0.9800C31'—H31D0.9600
C18—H18B0.9800C32'—C33'1.531 (10)
C18—H18C0.9800C32'—H32C0.9600
C19—H19A0.9800C32'—H32D0.9598
C19—H19B0.9800C33'—O7'1.480 (8)
C19—H19C0.9800C33'—C34'1.493 (10)
C20—C221.501 (9)C33'—H33'0.9602
C20—C211.527 (9)C34'—C35'1.524 (10)
C20—H200.9598C34'—H34C0.9600
C21—H21A0.9800C34'—H34D0.9600
C21—H21B0.9800C35'—C36'1.559 (10)
C21—H21C0.9800C35'—C40'1.565 (10)
C22—C231.529 (9)C35'—H35'0.9601
C22—H22A0.9598C36'—C37'1.527 (11)
C22—H22B0.9599C36'—H36C0.9600
C23—C241.491 (9)C36'—H36D0.9597
C23—H23A0.9599C37'—C38'1.538 (10)
C23—H23B0.9601C37'—H37C0.9600
C24—O11.232 (8)C37'—H37D0.9601
C24—O21.330 (9)C38'—C44'1.501 (10)
O2—H2O1.1962C38'—C39'1.583 (10)
C31—C321.513 (9)C38'—H38'0.9599
C31—C401.544 (10)C39'—C40'1.520 (10)
C31—H31A0.9601C39'—C41'1.568 (9)
C31—H31B0.9599C39'—H39'0.9600
C32—C331.511 (9)C40'—C49'1.495 (10)
C32—H32A0.9600C41'—C42'1.562 (10)
C32—H32B0.9601C41'—H41C0.9600
C33—O71.475 (8)C41'—H41D0.9601
C33—C341.500 (10)C42'—C43'1.513 (9)
C33—H330.9600C42'—H42C0.9600
C34—C351.528 (10)C42'—H42D0.9598
C34—H34A0.9601C43'—C48'1.529 (9)
C34—H34B0.9600C43'—C47'1.562 (10)
C35—C361.528 (10)C43'—C44'1.567 (9)
C35—C401.534 (9)C44'—C45'1.530 (10)
C35—H350.9601C44'—H44'0.9599
C36—C371.569 (10)C45'—C46'1.536 (10)
C36—H36A0.9600C45'—H45C0.9600
C36—H36B0.9599C45'—H45D0.9602
C37—C381.531 (9)C46'—C47'1.564 (8)
C37—H37A0.9600C46'—H46C0.9600
C37—H37B0.9600C46'—H46D0.9599
C38—C391.531 (10)C47'—C50'1.527 (9)
C38—C441.544 (10)C47'—H47'0.9601
C38—H380.9599C48'—H48D0.9800
C39—C411.525 (9)C48'—H48E0.9800
C39—C401.556 (10)C48'—H48F0.9800
C39—H390.9599C49'—H49D0.9800
C40—C491.534 (10)C49'—H49E0.9800
C41—C421.517 (10)C49'—H49F0.9800
C41—H41A0.9600C50'—C52'1.496 (9)
C41—H41B0.9599C50'—C51'1.521 (9)
C42—C431.536 (10)C50'—H50'0.9600
C42—H42A0.9599C51'—H51D0.9800
C42—H42B0.9600C51'—H51E0.9800
C43—C481.529 (9)C51'—H51F0.9800
C43—C471.540 (10)C52'—C53'1.525 (9)
C43—C441.539 (9)C52'—H52C0.9600
C44—C451.522 (10)C52'—H52D0.9599
C44—H440.9599C53'—C54'1.475 (10)
C45—C461.546 (10)C53'—H53C0.9600
C45—H45A0.9600C53'—H53D0.9599
C45—H45B0.9601C54'—O3'1.223 (9)
C46—C471.555 (9)C54'—O4'1.336 (8)
C46—H46A0.9600O4'—H4'O1.2785
C46—H46B0.9599O5'—C1L'1.361 (9)
C47—C501.568 (9)O6'—C1L'1.225 (9)
C47—H470.9599C1L'—C2L'1.500 (10)
C48—H48A0.9800C2L'—C3L'1.362 (10)
C48—H48B0.9800C2L'—C7L'1.391 (10)
C48—H48C0.9800C3L'—C4L'1.400 (10)
C49—H49A0.9800C3L'—H3L'0.9599
C49—H49B0.9800C4L'—C5L'1.387 (10)
C49—H49C0.9800C4L'—H4L'0.9599
C50—C511.519 (9)C5L'—C6L'1.382 (10)
C50—C521.538 (9)C5L'—C8L'1.477 (11)
C50—H500.9599C6L'—C7L'1.387 (10)
C51—H51A0.9800C6L'—H6L'0.9601
C51—H51B0.9800C7L'—H7L'0.9600
C51—H51C0.9800C8L'—O8'1.206 (9)
C52—C531.568 (9)C8L'—O7'1.339 (10)
C52—H52A0.9600N1S—C5S1.334 (8)
C52—H52B0.9600N1S—C1S1.340 (10)
C53—C541.509 (10)N1S—H2O1.4602
C53—H53A0.9600C1S—C2S1.350 (11)
C53—H53B0.9601C1S—H1S0.9601
C54—O31.195 (8)C2S—C3S1.389 (11)
C54—O41.331 (8)C2S—H2S0.9599
O4—H4O1.1882C3S—C4S1.383 (10)
O5—C1L1.319 (8)C3S—H3S0.9600
O6—C1L1.189 (9)C4S—C5S1.384 (10)
C1L—C2L1.491 (10)C4S—H4S0.9600
C2L—C7L1.387 (10)C5S—H5S0.9597
C2L—C3L1.398 (10)N2S—C10S1.330 (9)
C3L—C4L1.362 (10)N2S—C6S1.334 (9)
C3L—H3L0.9601N2S—H4O1.4674
C4L—C5L1.378 (10)C6S—C7S1.352 (11)
C4L—H4L0.9599C6S—H6S0.9601
C5L—C6L1.398 (10)C7S—C8S1.378 (11)
C5L—C8L1.478 (10)C7S—H7S0.9600
C6L—C7L1.390 (10)C8S—C9S1.386 (10)
C6L—H6L0.9601C8S—H8S0.9601
C7L—H7L0.9599C9S—C10S1.364 (10)
C8L—O81.175 (9)C9S—H9S0.9601
C8L—O71.354 (9)C10S—H10S0.9600
C1'—C2'1.529 (10)N3S—C11S1.310 (10)
C1'—C10'1.544 (9)N3S—C15S1.359 (10)
C1'—H1'A0.9601N3S—H2'O1.4959
C1'—H1'B0.9600C11S—C12S1.382 (11)
C2'—C3'1.533 (10)C11S—H11S0.9601
C2'—H2'A0.9600C12S—C13S1.384 (11)
C2'—H2'B0.9600C12S—H12S0.9601
C3'—O5'1.453 (8)C13S—C14S1.363 (11)
C3'—C4'1.547 (9)C13S—H13S0.9599
C3'—H3'0.9600C14S—C15S1.379 (11)
C4'—C5'1.516 (9)C14S—H14S0.9600
C4'—H4'A0.9601C15S—H15S0.9600
C4'—H4'B0.9601N4S—C20S1.339 (9)
C5'—C6'1.530 (9)N4S—C16S1.349 (10)
C5'—C10'1.546 (10)N4S—H4'O1.4104
C5'—H5'0.9601C16S—C17S1.372 (10)
C6'—C7'1.523 (9)C16S—H16S0.9600
C6'—H6'A0.9600C17S—C18S1.356 (11)
C6'—H6'B0.9600C17S—H17S0.9600
C7'—C8'1.512 (10)C18S—C19S1.361 (11)
C7'—H7'A0.9602C18S—H18S0.9600
C7'—H7'B0.9598C19S—C20S1.393 (10)
C8'—C14'1.547 (10)C19S—H19S0.9599
C8'—C9'1.583 (9)C20S—H20S0.9599
C2—C1—C10113.3 (6)C8'—C7'—C6'111.7 (6)
C2—C1—H1A108.3C8'—C7'—H7'A108.9
C10—C1—H1A108.5C6'—C7'—H7'A109.1
C2—C1—H1B109.3C8'—C7'—H7'B109.8
C10—C1—H1B109.7C6'—C7'—H7'B109.3
H1A—C1—H1B107.5H7'A—C7'—H7'B108.0
C1—C2—C3112.8 (7)C7'—C8'—C14'113.5 (6)
C1—C2—H2A109.0C7'—C8'—C9'111.4 (6)
C3—C2—H2A109.3C14'—C8'—C9'107.2 (6)
C1—C2—H2B108.8C7'—C8'—H8'108.2
C3—C2—H2B108.9C14'—C8'—H8'108.1
H2A—C2—H2B108.0C9'—C8'—H8'108.5
O5—C3—C4112.2 (6)C10'—C9'—C11'115.3 (7)
O5—C3—C2107.4 (6)C10'—C9'—C8'111.5 (6)
C4—C3—C2112.4 (7)C11'—C9'—C8'107.9 (6)
O5—C3—H3108.3C10'—C9'—H9'107.9
C4—C3—H3108.3C11'—C9'—H9'107.4
C2—C3—H3108.1C8'—C9'—H9'106.4
C3—C4—C5112.2 (6)C9'—C10'—C19'113.3 (6)
C3—C4—H4A109.4C9'—C10'—C1'112.0 (6)
C5—C4—H4A109.5C19'—C10'—C1'105.7 (6)
C3—C4—H4B108.8C9'—C10'—C5'109.1 (6)
C5—C4—H4B108.8C19'—C10'—C5'109.3 (6)
H4A—C4—H4B107.9C1'—C10'—C5'107.2 (6)
C6—C5—C10113.5 (6)C12'—C11'—C9'114.5 (7)
C6—C5—C4111.3 (6)C12'—C11'—H11C108.9
C10—C5—C4111.4 (6)C9'—C11'—H11C109.3
C6—C5—H5A106.7C12'—C11'—H11D108.3
C10—C5—H5A106.7C9'—C11'—H11D108.0
C4—C5—H5A106.7H11C—C11'—H11D107.5
C7—C6—C5112.3 (6)C11'—C12'—C13'112.0 (7)
C7—C6—H6A109.3C11'—C12'—H12C109.0
C5—C6—H6A109.6C13'—C12'—H12C109.8
C7—C6—H6B109.2C11'—C12'—H12D109.5
C5—C6—H6B108.5C13'—C12'—H12D108.5
H6A—C6—H6B107.9H12C—C12'—H12D107.9
C6—C7—C8113.6 (6)C14'—C13'—C12'106.7 (6)
C6—C7—H7A109.0C14'—C13'—C18'111.9 (6)
C8—C7—H7A109.5C12'—C13'—C18'110.5 (6)
C6—C7—H7B108.8C14'—C13'—C17'100.6 (6)
C8—C7—H7B108.1C12'—C13'—C17'116.5 (6)
H7A—C7—H7B107.7C18'—C13'—C17'110.2 (6)
C14—C8—C9110.1 (6)C13'—C14'—C15'106.3 (6)
C14—C8—C7111.5 (6)C13'—C14'—C8'117.8 (6)
C9—C8—C7110.1 (6)C15'—C14'—C8'115.9 (6)
C14—C8—H8108.7C13'—C14'—H14'105.3
C9—C8—H8108.0C15'—C14'—H14'105.4
C7—C8—H8108.3C8'—C14'—H14'105.0
C8—C9—C11114.0 (7)C14'—C15'—C16'102.7 (5)
C8—C9—C10113.0 (6)C14'—C15'—H15C111.4
C11—C9—C10114.3 (6)C16'—C15'—H15C111.2
C8—C9—H9105.3C14'—C15'—H15D111.1
C11—C9—H9105.0C16'—C15'—H15D111.3
C10—C9—H9103.9H15C—C15'—H15D109.1
C19—C10—C5108.8 (7)C15'—C16'—C17'106.4 (5)
C19—C10—C1107.1 (7)C15'—C16'—H16C110.5
C5—C10—C1109.5 (6)C17'—C16'—H16C110.3
C19—C10—C9109.7 (7)C15'—C16'—H16D110.3
C5—C10—C9108.5 (6)C17'—C16'—H16D110.7
C1—C10—C9113.1 (7)H16C—C16'—H16D108.7
C9—C11—C12113.3 (6)C20'—C17'—C13'120.8 (6)
C9—C11—H11A109.1C20'—C17'—C16'111.7 (5)
C12—C11—H11A109.0C13'—C17'—C16'102.2 (5)
C9—C11—H11B109.0C20'—C17'—H17'107.5
C12—C11—H11B108.6C13'—C17'—H17'106.9
H11A—C11—H11B107.8C16'—C17'—H17'107.0
C13—C12—C11112.3 (7)C13'—C18'—H18D109.5
C13—C12—H12A109.4C13'—C18'—H18E109.5
C11—C12—H12A109.3H18D—C18'—H18E109.5
C13—C12—H12B109.1C13'—C18'—H18F109.5
C11—C12—H12B109.0H18D—C18'—H18F109.5
H12A—C12—H12B107.8H18E—C18'—H18F109.5
C12—C13—C18110.8 (7)C10'—C19'—H19D109.5
C12—C13—C14106.6 (6)C10'—C19'—H19E109.5
C18—C13—C14113.4 (6)H19D—C19'—H19E109.5
C12—C13—C17117.7 (6)C10'—C19'—H19F109.5
C18—C13—C17107.1 (6)H19D—C19'—H19F109.5
C14—C13—C17101.0 (5)H19E—C19'—H19F109.5
C8—C14—C15120.3 (6)C21'—C20'—C17'113.6 (6)
C8—C14—C13115.3 (6)C21'—C20'—C22'110.2 (7)
C15—C14—C13102.3 (6)C17'—C20'—C22'110.5 (6)
C8—C14—H14106.2C21'—C20'—H20'107.6
C15—C14—H14105.6C17'—C20'—H20'107.8
C13—C14—H14106.0C22'—C20'—H20'106.8
C14—C15—C16106.7 (6)C20'—C21'—H21D109.5
C14—C15—H15A110.0C20'—C21'—H21E109.5
C16—C15—H15A110.3H21D—C21'—H21E109.5
C14—C15—H15B110.7C20'—C21'—H21F109.5
C16—C15—H15B110.4H21D—C21'—H21F109.5
H15A—C15—H15B108.6H21E—C21'—H21F109.5
C15—C16—C17105.6 (6)C23'—C22'—C20'115.8 (6)
C15—C16—H16A110.7C23'—C22'—H22C107.4
C17—C16—H16A110.7C20'—C22'—H22C108.3
C15—C16—H16B110.7C23'—C22'—H22D109.0
C17—C16—H16B110.3C20'—C22'—H22D108.5
H16A—C16—H16B108.8H22C—C22'—H22D107.5
C16—C17—C20113.4 (5)C24'—C23'—C22'105.6 (7)
C16—C17—C13104.4 (6)C24'—C23'—H23C110.0
C20—C17—C13120.4 (6)C22'—C23'—H23C109.4
C16—C17—H17106.1C24'—C23'—H23D111.6
C20—C17—H17105.3C22'—C23'—H23D111.4
C13—C17—H17106.3H23C—C23'—H23D108.7
C13—C18—H18A109.5O1'—C24'—O2'121.7 (8)
C13—C18—H18B109.5O1'—C24'—C23'124.7 (8)
H18A—C18—H18B109.5O2'—C24'—C23'113.6 (9)
C13—C18—H18C109.5C24'—O2'—H2'O106.5
H18A—C18—H18C109.5C32'—C31'—C40'115.4 (6)
H18B—C18—H18C109.5C32'—C31'—H31C108.5
C10—C19—H19A109.5C40'—C31'—H31C108.5
C10—C19—H19B109.5C32'—C31'—H31D108.7
H19A—C19—H19B109.5C40'—C31'—H31D107.9
C10—C19—H19C109.5H31C—C31'—H31D107.6
H19A—C19—H19C109.5C31'—C32'—C33'108.7 (6)
H19B—C19—H19C109.5C31'—C32'—H32C109.7
C22—C20—C21108.6 (6)C33'—C32'—H32C109.8
C22—C20—C17109.1 (6)C31'—C32'—H32D110.3
C21—C20—C17112.8 (6)C33'—C32'—H32D110.0
C22—C20—H20109.2H32C—C32'—H32D108.3
C21—C20—H20108.4O7'—C33'—C34'106.0 (6)
C17—C20—H20108.6O7'—C33'—C32'107.0 (6)
C20—C21—H21A109.5C34'—C33'—C32'109.4 (6)
C20—C21—H21B109.5O7'—C33'—H33'111.4
H21A—C21—H21B109.5C34'—C33'—H33'111.5
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H21A—C21—H21C109.5C33'—C34'—C35'109.9 (6)
H21B—C21—H21C109.5C33'—C34'—H34C109.6
C20—C22—C23115.8 (6)C35'—C34'—H34C109.9
C20—C22—H22A108.0C33'—C34'—H34D109.7
C23—C22—H22A109.1C35'—C34'—H34D109.7
C20—C22—H22B108.5H34C—C34'—H34D108.1
C23—C22—H22B107.7C34'—C35'—C36'109.6 (7)
H22A—C22—H22B107.5C34'—C35'—C40'114.2 (6)
C24—C23—C22107.7 (6)C36'—C35'—C40'109.1 (6)
C24—C23—H23A110.4C34'—C35'—H35'107.9
C22—C23—H23A110.9C36'—C35'—H35'107.8
C24—C23—H23B109.9C40'—C35'—H35'108.1
C22—C23—H23B109.4C37'—C36'—C35'112.3 (6)
H23A—C23—H23B108.5C37'—C36'—H36C109.2
O1—C24—O2124.1 (7)C35'—C36'—H36C109.1
O1—C24—C23122.5 (7)C37'—C36'—H36D109.1
O2—C24—C23113.4 (7)C35'—C36'—H36D109.1
C24—O2—H2O116.7H36C—C36'—H36D107.9
C32—C31—C40115.0 (6)C36'—C37'—C38'110.9 (7)
C32—C31—H31A108.5C36'—C37'—H37C109.4
C40—C31—H31A108.8C38'—C37'—H37C109.4
C32—C31—H31B108.0C36'—C37'—H37D109.6
C40—C31—H31B108.7C38'—C37'—H37D109.5
H31A—C31—H31B107.7H37C—C37'—H37D108.1
C33—C32—C31109.2 (6)C44'—C38'—C37'112.7 (7)
C33—C32—H32A110.0C44'—C38'—C39'108.6 (6)
C31—C32—H32A110.3C37'—C38'—C39'109.0 (6)
C33—C32—H32B109.4C44'—C38'—H38'109.0
C31—C32—H32B109.5C37'—C38'—H38'108.5
H32A—C32—H32B108.3C39'—C38'—H38'108.9
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O7—C33—C32108.3 (6)C40'—C39'—C38'112.2 (6)
C34—C33—C32112.8 (6)C41'—C39'—C38'109.6 (6)
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C32—C33—H33108.8C38'—C39'—H39'106.9
C33—C34—C35110.0 (6)C49'—C40'—C39'114.1 (6)
C33—C34—H34A109.6C49'—C40'—C31'105.1 (7)
C35—C34—H34A109.8C39'—C40'—C31'112.5 (6)
C33—C34—H34B109.6C49'—C40'—C35'110.4 (7)
C35—C34—H34B109.6C39'—C40'—C35'110.2 (6)
H34A—C34—H34B108.3C31'—C40'—C35'104.0 (6)
C36—C35—C34110.2 (6)C42'—C41'—C39'112.5 (6)
C36—C35—C40111.9 (6)C42'—C41'—H41C108.3
C34—C35—C40113.5 (6)C39'—C41'—H41C108.9
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C34—C35—H35106.9C39'—C41'—H41D109.2
C40—C35—H35107.0H41C—C41'—H41D107.8
C35—C36—C37111.3 (6)C43'—C42'—C41'113.6 (6)
C35—C36—H36A109.5C43'—C42'—H42C109.1
C37—C36—H36A108.9C41'—C42'—H42C108.8
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C37—C36—H36B109.7C41'—C42'—H42D108.3
H36A—C36—H36B108.0H42C—C42'—H42D107.8
C38—C37—C36109.9 (6)C42'—C43'—C48'110.9 (6)
C38—C37—H37A109.3C42'—C43'—C47'116.6 (6)
C36—C37—H37A109.8C48'—C43'—C47'111.8 (6)
C38—C37—H37B110.1C42'—C43'—C44'104.4 (6)
C36—C37—H37B109.7C48'—C43'—C44'112.2 (6)
H37A—C37—H37B108.0C47'—C43'—C44'100.1 (5)
C37—C38—C39112.7 (6)C38'—C44'—C45'117.0 (6)
C37—C38—C44110.3 (6)C38'—C44'—C43'115.0 (7)
C39—C38—C44109.3 (6)C45'—C44'—C43'102.6 (6)
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C39—C38—H38107.8C45'—C44'—H44'107.3
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C41—C39—C38110.5 (6)C44'—C45'—C46'104.5 (6)
C41—C39—C40115.8 (6)C44'—C45'—H45C110.3
C38—C39—C40112.8 (6)C46'—C45'—H45C110.7
C41—C39—H39106.0C44'—C45'—H45D111.2
C38—C39—H39105.8C46'—C45'—H45D111.2
C40—C39—H39105.1H45C—C45'—H45D108.9
C49—C40—C35109.4 (6)C45'—C46'—C47'107.3 (6)
C49—C40—C31107.2 (6)C45'—C46'—H46C110.5
C35—C40—C31107.4 (6)C47'—C46'—H46C110.2
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C35—C40—C39109.7 (6)C47'—C46'—H46D110.4
C31—C40—C39112.8 (6)H46C—C46'—H46D108.5
C42—C41—C39114.4 (6)C50'—C47'—C43'119.6 (6)
C42—C41—H41A109.0C50'—C47'—C46'111.3 (6)
C39—C41—H41A108.2C43'—C47'—C46'102.6 (5)
C42—C41—H41B108.4C50'—C47'—H47'108.1
C39—C41—H41B108.9C43'—C47'—H47'107.3
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C41—C42—C43112.4 (6)C43'—C48'—H48D109.5
C41—C42—H42A109.1C43'—C48'—H48E109.5
C43—C42—H42A108.9H48D—C48'—H48E109.5
C41—C42—H42B109.2C43'—C48'—H48F109.5
C43—C42—H42B109.4H48D—C48'—H48F109.5
H42A—C42—H42B107.7H48E—C48'—H48F109.5
C48—C43—C42111.6 (6)C40'—C49'—H49D109.5
C48—C43—C47110.1 (6)C40'—C49'—H49E109.5
C42—C43—C47118.0 (6)H49D—C49'—H49E109.5
C48—C43—C44111.2 (6)C40'—C49'—H49F109.5
C42—C43—C44105.9 (6)H49D—C49'—H49F109.5
C47—C43—C4499.2 (5)H49E—C49'—H49F109.5
C45—C44—C43105.8 (6)C52'—C50'—C51'111.5 (6)
C45—C44—C38119.0 (6)C52'—C50'—C47'111.5 (6)
C43—C44—C38114.6 (6)C51'—C50'—C47'111.7 (6)
C45—C44—H44105.4C52'—C50'—H50'107.1
C43—C44—H44105.7C51'—C50'—H50'107.4
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C44—C45—C46103.3 (6)C50'—C51'—H51D109.5
C44—C45—H45A111.3C50'—C51'—H51E109.5
C46—C45—H45A111.2H51D—C51'—H51E109.5
C44—C45—H45B111.3C50'—C51'—H51F109.5
C46—C45—H45B110.7H51D—C51'—H51F109.5
H45A—C45—H45B109.1H51E—C51'—H51F109.5
C45—C46—C47106.3 (6)C50'—C52'—C53'115.4 (6)
C45—C46—H46A110.3C50'—C52'—H52C109.0
C47—C46—H46A110.4C53'—C52'—H52C108.5
C45—C46—H46B110.9C50'—C52'—H52D108.0
C47—C46—H46B110.4C53'—C52'—H52D108.2
H46A—C46—H46B108.6H52C—C52'—H52D107.5
C43—C47—C46105.2 (6)C54'—C53'—C52'114.4 (6)
C43—C47—C50118.6 (5)C54'—C53'—H53C109.0
C46—C47—C50110.8 (6)C52'—C53'—H53C108.8
C43—C47—H47107.6C54'—C53'—H53D108.5
C46—C47—H47107.5C52'—C53'—H53D108.4
C50—C47—H47106.5H53C—C53'—H53D107.5
C43—C48—H48A109.5O3'—C54'—O4'118.8 (8)
C43—C48—H48B109.5O3'—C54'—C53'126.0 (7)
H48A—C48—H48B109.5O4'—C54'—C53'115.1 (7)
C43—C48—H48C109.5C54'—O4'—H4'O111.1
H48A—C48—H48C109.5C1L'—O5'—C3'114.8 (6)
H48B—C48—H48C109.5O6'—C1L'—O5'123.8 (7)
C40—C49—H49A109.5O6'—C1L'—C2L'122.9 (8)
C40—C49—H49B109.5O5'—C1L'—C2L'113.2 (7)
H49A—C49—H49B109.5C3L'—C2L'—C7L'122.1 (8)
C40—C49—H49C109.5C3L'—C2L'—C1L'116.9 (7)
H49A—C49—H49C109.5C7L'—C2L'—C1L'120.9 (7)
H49B—C49—H49C109.5C2L'—C3L'—C4L'119.7 (7)
C51—C50—C52109.9 (6)C2L'—C3L'—H3L'120.6
C51—C50—C47113.9 (6)C4L'—C3L'—H3L'119.7
C52—C50—C47109.3 (5)C5L'—C4L'—C3L'119.8 (8)
C51—C50—H50107.9C5L'—C4L'—H4L'120.4
C52—C50—H50108.2C3L'—C4L'—H4L'119.9
C47—C50—H50107.5C6L'—C5L'—C4L'118.7 (7)
C50—C51—H51A109.5C6L'—C5L'—C8L'120.6 (8)
C50—C51—H51B109.5C4L'—C5L'—C8L'120.6 (8)
H51A—C51—H51B109.5C5L'—C6L'—C7L'122.6 (8)
C50—C51—H51C109.5C5L'—C6L'—H6L'119.0
H51A—C51—H51C109.5C7L'—C6L'—H6L'118.5
H51B—C51—H51C109.5C6L'—C7L'—C2L'117.1 (7)
C50—C52—C53113.6 (6)C6L'—C7L'—H7L'121.1
C50—C52—H52A108.3C2L'—C7L'—H7L'121.9
C53—C52—H52A109.2O8'—C8L'—O7'124.0 (8)
C50—C52—H52B109.3O8'—C8L'—C5L'124.3 (9)
C53—C52—H52B108.7O7'—C8L'—C5L'111.5 (7)
H52A—C52—H52B107.6C8L'—O7'—C33'117.0 (6)
C54—C53—C52115.5 (6)C5S—N1S—C1S119.0 (7)
C54—C53—H53A107.6C5S—N1S—H2O116.7
C52—C53—H53A108.2C1S—N1S—H2O124.2
C54—C53—H53B108.8N1S—C1S—C2S123.4 (8)
C52—C53—H53B109.0N1S—C1S—H1S118.9
H53A—C53—H53B107.5C2S—C1S—H1S117.8
O3—C54—O4125.7 (7)C1S—C2S—C3S118.6 (9)
O3—C54—C53124.5 (7)C1S—C2S—H2S120.8
O4—C54—C53109.8 (7)C3S—C2S—H2S120.5
C54—O4—H4O114.2C4S—C3S—C2S118.3 (8)
C1L—O5—C3121.3 (6)C4S—C3S—H3S120.8
O6—C1L—O5123.5 (7)C2S—C3S—H3S120.9
O6—C1L—C2L124.3 (7)C3S—C4S—C5S119.8 (8)
O5—C1L—C2L112.1 (7)C3S—C4S—H4S120.6
C7L—C2L—C3L119.5 (7)C5S—C4S—H4S119.6
C7L—C2L—C1L121.8 (8)N1S—C5S—C4S120.8 (8)
C3L—C2L—C1L118.6 (7)N1S—C5S—H5S120.0
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C2L—C3L—H3L120.1C10S—N2S—H4O119.2
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C3L—C4L—H4L119.2N2S—C6S—C7S123.4 (8)
C5L—C4L—H4L118.3N2S—C6S—H6S119.4
C4L—C5L—C6L117.8 (7)C7S—C6S—H6S117.3
C4L—C5L—C8L125.9 (7)C6S—C7S—C8S119.0 (8)
C6L—C5L—C8L116.1 (7)C6S—C7S—H7S120.9
C7L—C6L—C5L120.8 (7)C8S—C7S—H7S120.0
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C5L—C6L—H6L119.5C7S—C8S—H8S121.0
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C6L—C7L—H7L120.5C10S—C9S—H9S120.0
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O8—C8L—C5L125.5 (8)N2S—C10S—C9S122.3 (8)
O7—C8L—C5L111.2 (7)N2S—C10S—H10S118.9
C8L—O7—C33117.9 (6)C9S—C10S—H10S118.7
C2'—C1'—C10'114.7 (6)C11S—N3S—C15S118.3 (8)
C2'—C1'—H1'A109.1C11S—N3S—H2'O114.8
C10'—C1'—H1'A109.1C15S—N3S—H2'O126.8
C2'—C1'—H1'B108.5N3S—C11S—C12S122.0 (9)
C10'—C1'—H1'B107.6N3S—C11S—H11S118.2
H1'A—C1'—H1'B107.8C12S—C11S—H11S119.8
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C3'—C2'—H2'A109.9C13S—C12S—H12S120.7
C1'—C2'—H2'B110.4C14S—C13S—C12S119.0 (9)
C3'—C2'—H2'B110.3C14S—C13S—H13S120.5
H2'A—C2'—H2'B108.4C12S—C13S—H13S120.5
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O5'—C3'—C4'108.9 (6)C13S—C14S—H14S120.5
C2'—C3'—C4'109.7 (6)C15S—C14S—H14S121.2
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C2'—C3'—H3'110.5N3S—C15S—H15S118.4
C4'—C3'—H3'110.5C14S—C15S—H15S118.8
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C5'—C4'—H4'A109.1C20S—N4S—H4'O127.6
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C3'—C4'—H4'B109.7N4S—C16S—H16S117.4
H4'A—C4'—H4'B107.9C17S—C16S—H16S118.6
C4'—C5'—C6'110.8 (6)C18S—C17S—C16S118.4 (9)
C4'—C5'—C10'113.3 (6)C18S—C17S—H17S121.2
C6'—C5'—C10'111.6 (6)C16S—C17S—H17S120.4
C4'—C5'—H5'107.2C17S—C18S—C19S120.9 (8)
C6'—C5'—H5'106.7C17S—C18S—H18S119.3
C10'—C5'—H5'106.9C19S—C18S—H18S119.8
C7'—C6'—C5'112.9 (6)C18S—C19S—C20S116.8 (8)
C7'—C6'—H6'A109.1C18S—C19S—H19S121.3
C5'—C6'—H6'A109.0C20S—C19S—H19S121.9
C7'—C6'—H6'B108.6N4S—C20S—C19S124.6 (8)
C5'—C6'—H6'B109.4N4S—C20S—H20S117.4
H6'A—C6'—H6'B107.7C19S—C20S—H20S117.9
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C1—C2—C3—O5178.9 (6)C14'—C8'—C9'—C10'179.5 (6)
C1—C2—C3—C455.0 (9)C7'—C8'—C9'—C11'176.5 (7)
O5—C3—C4—C5174.8 (6)C14'—C8'—C9'—C11'51.9 (8)
C2—C3—C4—C553.7 (9)C11'—C9'—C10'—C19'58.5 (8)
C3—C4—C5—C6179.2 (6)C8'—C9'—C10'—C19'65.0 (8)
C3—C4—C5—C1053.0 (9)C11'—C9'—C10'—C1'61.0 (9)
C10—C5—C6—C752.1 (9)C8'—C9'—C10'—C1'175.5 (6)
C4—C5—C6—C774.5 (8)C11'—C9'—C10'—C5'179.5 (6)
C5—C6—C7—C850.7 (9)C8'—C9'—C10'—C5'57.0 (8)
C6—C7—C8—C14175.3 (6)C2'—C1'—C10'—C9'63.7 (9)
C6—C7—C8—C952.7 (8)C2'—C1'—C10'—C19'172.5 (7)
C14—C8—C9—C1148.0 (9)C2'—C1'—C10'—C5'55.9 (8)
C7—C8—C9—C11171.3 (7)C4'—C5'—C10'—C9'68.9 (8)
C14—C8—C9—C10179.3 (7)C6'—C5'—C10'—C9'56.9 (8)
C7—C8—C9—C1056.0 (9)C4'—C5'—C10'—C19'166.7 (6)
C6—C5—C10—C1965.8 (8)C6'—C5'—C10'—C19'67.5 (8)
C4—C5—C10—C19167.7 (6)C4'—C5'—C10'—C1'52.5 (8)
C6—C5—C10—C1177.5 (6)C6'—C5'—C10'—C1'178.4 (6)
C4—C5—C10—C150.9 (9)C10'—C9'—C11'—C12'179.4 (6)
C6—C5—C10—C953.6 (8)C8'—C9'—C11'—C12'55.2 (9)
C4—C5—C10—C973.0 (8)C9'—C11'—C12'—C13'57.2 (9)
C2—C1—C10—C19170.8 (7)C11'—C12'—C13'—C14'54.1 (9)
C2—C1—C10—C553.0 (9)C11'—C12'—C13'—C18'67.7 (9)
C2—C1—C10—C968.2 (9)C11'—C12'—C13'—C17'165.6 (7)
C8—C9—C10—C1962.2 (9)C12'—C13'—C14'—C15'169.3 (6)
C11—C9—C10—C1970.4 (9)C18'—C13'—C14'—C15'69.8 (8)
C8—C9—C10—C556.6 (9)C17'—C13'—C14'—C15'47.2 (7)
C11—C9—C10—C5170.9 (6)C12'—C13'—C14'—C8'58.8 (8)
C8—C9—C10—C1178.3 (6)C18'—C13'—C14'—C8'62.2 (8)
C11—C9—C10—C149.1 (10)C17'—C13'—C14'—C8'179.1 (6)
C8—C9—C11—C1247.4 (10)C7'—C8'—C14'—C13'177.3 (6)
C10—C9—C11—C12179.5 (6)C9'—C8'—C14'—C13'59.3 (8)
C9—C11—C12—C1352.4 (9)C7'—C8'—C14'—C15'49.8 (9)
C11—C12—C13—C1868.4 (8)C9'—C8'—C14'—C15'173.2 (6)
C11—C12—C13—C1455.5 (8)C13'—C14'—C15'—C16'32.9 (7)
C11—C12—C13—C17167.9 (6)C8'—C14'—C15'—C16'165.9 (6)
C9—C8—C14—C15179.1 (7)C14'—C15'—C16'—C17'5.6 (7)
C7—C8—C14—C1558.3 (9)C14'—C13'—C17'—C20'165.9 (6)
C9—C8—C14—C1355.7 (8)C12'—C13'—C17'—C20'79.3 (9)
C7—C8—C14—C13178.3 (6)C18'—C13'—C17'—C20'47.6 (8)
C12—C13—C14—C859.7 (8)C14'—C13'—C17'—C16'41.1 (6)
C18—C13—C14—C862.5 (9)C12'—C13'—C17'—C16'156.0 (6)
C17—C13—C14—C8176.8 (6)C18'—C13'—C17'—C16'77.1 (7)
C12—C13—C14—C15167.8 (6)C15'—C16'—C17'—C20'152.4 (6)
C18—C13—C14—C1569.9 (8)C15'—C16'—C17'—C13'21.9 (7)
C17—C13—C14—C1544.3 (7)C13'—C17'—C20'—C21'57.7 (9)
C8—C14—C15—C16163.5 (7)C16'—C17'—C20'—C21'177.8 (6)
C13—C14—C15—C1634.0 (8)C13'—C17'—C20'—C22'177.8 (6)
C14—C15—C16—C179.9 (9)C16'—C17'—C20'—C22'57.7 (8)
C15—C16—C17—C20150.9 (6)C21'—C20'—C22'—C23'53.7 (9)
C15—C16—C17—C1318.1 (8)C17'—C20'—C22'—C23'180.0 (6)
C12—C13—C17—C16154.0 (6)C20'—C22'—C23'—C24'158.4 (7)
C18—C13—C17—C1680.5 (7)C22'—C23'—C24'—O1'77.0 (10)
C14—C13—C17—C1638.4 (7)C22'—C23'—C24'—O2'99.9 (8)
C12—C13—C17—C2077.3 (8)C40'—C31'—C32'—C33'59.5 (9)
C18—C13—C17—C2048.2 (9)C31'—C32'—C33'—O7'173.6 (6)
C14—C13—C17—C20167.1 (6)C31'—C32'—C33'—C34'59.2 (8)
C16—C17—C20—C2257.6 (8)O7'—C33'—C34'—C35'175.3 (6)
C13—C17—C20—C22177.8 (6)C32'—C33'—C34'—C35'60.3 (8)
C16—C17—C20—C21178.4 (7)C33'—C34'—C35'—C36'176.8 (6)
C13—C17—C20—C2157.1 (9)C33'—C34'—C35'—C40'60.4 (9)
C21—C20—C22—C2360.8 (8)C34'—C35'—C36'—C37'68.5 (9)
C17—C20—C22—C23175.9 (6)C40'—C35'—C36'—C37'57.2 (9)
C20—C22—C23—C24167.2 (7)C35'—C36'—C37'—C38'58.2 (10)
C22—C23—C24—O183.9 (9)C36'—C37'—C38'—C44'176.6 (7)
C22—C23—C24—O293.0 (8)C36'—C37'—C38'—C39'55.9 (9)
C40—C31—C32—C3355.2 (9)C44'—C38'—C39'—C40'179.8 (6)
C31—C32—C33—O7177.6 (6)C37'—C38'—C39'—C40'57.1 (9)
C31—C32—C33—C3455.9 (9)C44'—C38'—C39'—C41'53.0 (8)
O7—C33—C34—C35177.7 (5)C37'—C38'—C39'—C41'176.1 (7)
C32—C33—C34—C3556.8 (8)C41'—C39'—C40'—C49'57.7 (9)
C33—C34—C35—C36177.3 (6)C38'—C39'—C40'—C49'67.0 (9)
C33—C34—C35—C4056.3 (8)C41'—C39'—C40'—C31'61.9 (8)
C34—C35—C36—C3769.5 (8)C38'—C39'—C40'—C31'173.3 (6)
C40—C35—C36—C3757.8 (9)C41'—C39'—C40'—C35'177.5 (6)
C35—C36—C37—C3855.3 (9)C38'—C39'—C40'—C35'57.8 (8)
C36—C37—C38—C3953.3 (9)C32'—C31'—C40'—C49'170.6 (6)
C36—C37—C38—C44175.8 (6)C32'—C31'—C40'—C39'64.6 (8)
C37—C38—C39—C41174.9 (6)C32'—C31'—C40'—C35'54.6 (8)
C44—C38—C39—C4151.9 (8)C34'—C35'—C40'—C49'166.4 (7)
C37—C38—C39—C4053.8 (9)C36'—C35'—C40'—C49'70.5 (9)
C44—C38—C39—C40176.7 (6)C34'—C35'—C40'—C39'66.7 (8)
C36—C35—C40—C4965.3 (8)C36'—C35'—C40'—C39'56.4 (8)
C34—C35—C40—C49169.2 (6)C34'—C35'—C40'—C31'54.1 (9)
C36—C35—C40—C31178.7 (6)C36'—C35'—C40'—C31'177.2 (6)
C34—C35—C40—C3153.2 (8)C40'—C39'—C41'—C42'176.7 (6)
C36—C35—C40—C3955.7 (8)C38'—C39'—C41'—C42'50.5 (8)
C34—C35—C40—C3969.8 (8)C39'—C41'—C42'—C43'55.7 (9)
C32—C31—C40—C49171.0 (6)C41'—C42'—C43'—C48'64.2 (8)
C32—C31—C40—C3553.5 (9)C41'—C42'—C43'—C47'166.3 (6)
C32—C31—C40—C3967.5 (8)C41'—C42'—C43'—C44'56.9 (8)
C41—C39—C40—C4961.6 (8)C37'—C38'—C44'—C45'56.1 (10)
C38—C39—C40—C4967.1 (8)C39'—C38'—C44'—C45'177.0 (7)
C41—C39—C40—C35177.9 (6)C37'—C38'—C44'—C43'176.7 (6)
C38—C39—C40—C3553.4 (8)C39'—C38'—C44'—C43'62.4 (9)
C41—C39—C40—C3158.2 (8)C42'—C43'—C44'—C38'63.0 (8)
C38—C39—C40—C31173.2 (6)C48'—C43'—C44'—C38'57.2 (9)
C38—C39—C41—C4252.6 (9)C47'—C43'—C44'—C38'175.9 (6)
C40—C39—C41—C42177.6 (7)C42'—C43'—C44'—C45'168.8 (6)
C39—C41—C42—C4355.7 (9)C48'—C43'—C44'—C45'71.0 (8)
C41—C42—C43—C4865.9 (8)C47'—C43'—C44'—C45'47.7 (7)
C41—C42—C43—C47165.1 (6)C38'—C44'—C45'—C46'162.7 (7)
C41—C42—C43—C4455.3 (8)C43'—C44'—C45'—C46'35.8 (9)
C48—C43—C44—C4570.6 (8)C44'—C45'—C46'—C47'10.0 (9)
C42—C43—C44—C45168.0 (7)C42'—C43'—C47'—C50'83.9 (8)
C47—C43—C44—C4545.2 (7)C48'—C43'—C47'—C50'45.2 (8)
C48—C43—C44—C3862.6 (8)C44'—C43'—C47'—C50'164.2 (6)
C42—C43—C44—C3858.8 (8)C42'—C43'—C47'—C46'152.4 (6)
C47—C43—C44—C38178.4 (6)C48'—C43'—C47'—C46'78.5 (7)
C37—C38—C44—C4550.2 (9)C44'—C43'—C47'—C46'40.5 (7)
C39—C38—C44—C45174.6 (6)C45'—C46'—C47'—C50'148.6 (7)
C37—C38—C44—C43176.8 (6)C45'—C46'—C47'—C43'19.6 (8)
C39—C38—C44—C4358.7 (8)C43'—C47'—C50'—C52'176.7 (6)
C43—C44—C45—C4634.3 (8)C46'—C47'—C50'—C52'57.3 (8)
C38—C44—C45—C46165.0 (7)C43'—C47'—C50'—C51'57.8 (8)
C44—C45—C46—C479.3 (8)C46'—C47'—C50'—C51'177.2 (6)
C48—C43—C47—C4678.6 (6)C51'—C50'—C52'—C53'60.8 (8)
C42—C43—C47—C46151.7 (6)C47'—C50'—C52'—C53'173.6 (6)
C44—C43—C47—C4638.1 (7)C50'—C52'—C53'—C54'94.1 (8)
C48—C43—C47—C5046.0 (8)C52'—C53'—C54'—O3'39.2 (11)
C42—C43—C47—C5083.7 (8)C52'—C53'—C54'—O4'143.5 (7)
C44—C43—C47—C50162.7 (6)C2'—C3'—O5'—C1L'160.7 (6)
C45—C46—C47—C4318.6 (8)C4'—C3'—O5'—C1L'81.0 (7)
C45—C46—C47—C50148.0 (6)C3'—O5'—C1L'—O6'8.0 (10)
C43—C47—C50—C5156.0 (8)C3'—O5'—C1L'—C2L'170.5 (5)
C46—C47—C50—C51177.9 (6)O6'—C1L'—C2L'—C3L'1.2 (11)
C43—C47—C50—C52179.3 (6)O5'—C1L'—C2L'—C3L'179.7 (6)
C46—C47—C50—C5258.8 (8)O6'—C1L'—C2L'—C7L'176.8 (7)
C51—C50—C52—C5364.6 (8)O5'—C1L'—C2L'—C7L'1.7 (10)
C47—C50—C52—C53169.7 (6)C7L'—C2L'—C3L'—C4L'1.5 (11)
C50—C52—C53—C5493.7 (8)C1L'—C2L'—C3L'—C4L'179.5 (6)
C52—C53—C54—O334.7 (11)C2L'—C3L'—C4L'—C5L'0.6 (11)
C52—C53—C54—O4144.9 (7)C3L'—C4L'—C5L'—C6L'0.6 (11)
C4—C3—O5—C1L95.5 (8)C3L'—C4L'—C5L'—C8L'178.2 (7)
C2—C3—O5—C1L140.5 (7)C4L'—C5L'—C6L'—C7L'1.1 (11)
C3—O5—C1L—O60.3 (11)C8L'—C5L'—C6L'—C7L'178.7 (7)
C3—O5—C1L—C2L176.9 (6)C5L'—C6L'—C7L'—C2L'0.3 (11)
O6—C1L—C2L—C7L166.9 (7)C3L'—C2L'—C7L'—C6L'1.1 (11)
O5—C1L—C2L—C7L9.6 (10)C1L'—C2L'—C7L'—C6L'178.9 (6)
O6—C1L—C2L—C3L16.9 (11)C6L'—C5L'—C8L'—O8'10.4 (12)
O5—C1L—C2L—C3L166.6 (6)C4L'—C5L'—C8L'—O8'167.1 (8)
C7L—C2L—C3L—C4L0.5 (10)C6L'—C5L'—C8L'—O7'164.5 (7)
C1L—C2L—C3L—C4L176.8 (6)C4L'—C5L'—C8L'—O7'17.9 (10)
C2L—C3L—C4L—C5L0.4 (11)O8'—C8L'—O7'—C33'2.6 (12)
C3L—C4L—C5L—C6L1.2 (11)C5L'—C8L'—O7'—C33'177.5 (6)
C3L—C4L—C5L—C8L175.9 (7)C34'—C33'—O7'—C8L'135.6 (7)
C4L—C5L—C6L—C7L2.1 (10)C32'—C33'—O7'—C8L'107.7 (7)
C8L—C5L—C6L—C7L177.4 (6)C5S—N1S—C1S—C2S2.9 (13)
C3L—C2L—C7L—C6L1.4 (10)N1S—C1S—C2S—C3S0.2 (14)
C1L—C2L—C7L—C6L177.5 (6)C1S—C2S—C3S—C4S1.8 (13)
C5L—C6L—C7L—C2L2.3 (11)C2S—C3S—C4S—C5S1.0 (12)
C4L—C5L—C8L—O8179.0 (7)C1S—N1S—C5S—C4S3.6 (11)
C6L—C5L—C8L—O84.2 (11)C3S—C4S—C5S—N1S1.7 (12)
C4L—C5L—C8L—O70.7 (10)C10S—N2S—C6S—C7S1.9 (12)
C6L—C5L—C8L—O7175.6 (6)N2S—C6S—C7S—C8S0.2 (13)
O8—C8L—O7—C338.9 (11)C6S—C7S—C8S—C9S0.6 (12)
C5L—C8L—O7—C33170.9 (6)C7S—C8S—C9S—C10S1.1 (11)
C34—C33—O7—C8L152.4 (6)C6S—N2S—C10S—C9S3.7 (12)
C32—C33—O7—C8L84.0 (8)C8S—C9S—C10S—N2S3.3 (12)
C10'—C1'—C2'—C3'60.4 (8)C15S—N3S—C11S—C12S0.8 (12)
C1'—C2'—C3'—O5'176.5 (5)N3S—C11S—C12S—C13S0.4 (13)
C1'—C2'—C3'—C4'58.6 (8)C11S—C12S—C13S—C14S1.3 (14)
O5'—C3'—C4'—C5'174.8 (6)C12S—C13S—C14S—C15S2.6 (14)
C2'—C3'—C4'—C5'58.4 (8)C11S—N3S—C15S—C14S0.5 (13)
C3'—C4'—C5'—C6'177.7 (6)C13S—C14S—C15S—N3S2.2 (14)
C3'—C4'—C5'—C10'56.1 (8)C20S—N4S—C16S—C17S0.7 (11)
C4'—C5'—C6'—C7'72.1 (8)N4S—C16S—C17S—C18S0.1 (13)
C10'—C5'—C6'—C7'55.1 (8)C16S—C17S—C18S—C19S1.2 (13)
C5'—C6'—C7'—C8'52.7 (8)C17S—C18S—C19S—C20S2.8 (13)
C6'—C7'—C8'—C14'173.1 (5)C16S—N4S—C20S—C19S2.5 (12)
C6'—C7'—C8'—C9'52.1 (8)C18S—C19S—C20S—N4S3.6 (13)
(52Py180K) bis(23-carboxy-24-nor-5beta-cholan-3alpha-yl)terephtalate top
Crystal data top
C56H82O8·2(C5H5N)F(000) = 566
Mr = 1041.42Dx = 1.182 Mg m3
Triclinic, P1Melting point: 285 K
a = 6.8044 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.8870 (9) ÅCell parameters from 2630 reflections
c = 17.0661 (11) Åθ = 3.0–25.1°
α = 94.431 (6)°µ = 0.08 mm1
β = 97.935 (6)°T = 180 K
γ = 97.341 (5)°Plate, colourless
V = 1463.14 (18) Å30.40 × 0.40 × 0.20 mm
Z = 1
Data collection top
Kuma KM4CCD κ-geometry
diffractometer
3150 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.037
Graphite monochromatorθmax = 25.1°, θmin = 3.0°
ω scansh = 88
11263 measured reflectionsk = 1515
5162 independent reflectionsl = 1120
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)] = 0.050Riding
wR(F2) = 0.124 w = 1/[σ2(Fo2) + (0.066P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.93(Δ/σ)max < 0.001
5162 reflectionsΔρmax = 0.20 e Å3
673 parametersΔρmin = 0.18 e Å3
77 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
C56H82O8·2(C5H5N)γ = 97.341 (5)°
Mr = 1041.42V = 1463.14 (18) Å3
Triclinic, P1Z = 1
a = 6.8044 (5) ÅMo Kα radiation
b = 12.8870 (9) ŵ = 0.08 mm1
c = 17.0661 (11) ÅT = 180 K
α = 94.431 (6)°0.40 × 0.40 × 0.20 mm
β = 97.935 (6)°
Data collection top
Kuma KM4CCD κ-geometry
diffractometer
3150 reflections with I > 2σ(I)
11263 measured reflectionsRint = 0.037
5162 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.050Riding
wR(F2) = 0.124Δρmax = 0.20 e Å3
S = 0.93Δρmin = 0.18 e Å3
5162 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
673 parametersAbsolute structure parameter: 0 (10)
77 restraints
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*/UeqOcc. (<1)
C12.0073 (10)0.9125 (5)0.6240 (3)0.073 (2)
H1A2.10070.91800.58660.088*
H1B2.05680.87040.66430.088*
C21.8061 (11)0.8584 (5)0.5815 (3)0.0732 (19)
H2A1.71440.84850.61920.088*
H2B1.82060.79050.55750.088*
C31.7239 (8)0.9229 (4)0.5189 (3)0.0513 (14)
H3A1.81070.92830.47910.062*
C41.7065 (7)1.0316 (4)0.5546 (3)0.0389 (11)
H4A1.60901.02600.59020.047*
H4B1.65941.07240.51290.047*
C51.9038 (7)1.0877 (4)0.5997 (3)0.0417 (12)
H5A1.99481.09530.56160.050*
C61.8867 (9)1.1977 (4)0.6344 (3)0.0622 (15)
H6A1.82101.23460.59390.075*
H6B2.01891.23510.65160.075*
C71.7701 (8)1.1960 (4)0.7047 (3)0.0569 (14)
H7A1.63271.16770.68590.068*
H7B1.77331.26660.72780.068*
C81.8545 (7)1.1309 (4)0.7685 (3)0.0465 (13)
H8A1.98671.16440.79090.056*
C91.8704 (8)1.0202 (4)0.7330 (3)0.0477 (13)
H9A1.73950.98120.71600.057*0.50
H9B1.73690.99800.70550.057*0.50
C101.9977 (8)1.0230 (5)0.6632 (3)0.0561 (15)
C111.9811 (17)0.9712 (9)0.8024 (5)0.046 (3)*0.50
H11A2.10741.01390.82130.055*0.50
H11B2.00680.90240.78450.055*0.50
C11'1.8949 (17)0.9329 (8)0.7927 (6)0.048 (3)*0.50
H11C2.03320.94000.81610.058*0.50
H11D1.86210.86500.76300.058*0.50
C121.8546 (16)0.9636 (8)0.8706 (6)0.041 (3)*0.50
H12A1.92820.93350.91310.049*0.50
H12B1.73440.91560.85180.049*0.50
C12'1.7657 (18)0.9365 (8)0.8605 (6)0.048 (3)*0.50
H12C1.80580.88980.89900.058*0.50
H12D1.62680.91500.83950.058*0.50
C131.8015 (8)1.0590 (4)0.9027 (3)0.0526 (14)
C141.7271 (7)1.1225 (3)0.8349 (3)0.0389 (11)
H14A1.60061.08420.81020.047*
C151.6767 (10)1.2221 (4)0.8765 (3)0.0733 (18)
H15A1.57231.24940.84390.088*
H15B1.79211.27510.88820.088*
C161.6053 (9)1.1876 (4)0.9532 (3)0.0626 (15)
H16A1.46551.19280.95210.075*
H16B1.67961.23110.99860.075*
C171.6430 (7)1.0718 (3)0.9574 (3)0.0441 (11)
H17A1.52181.02910.93180.053*
C182.0101 (15)1.1382 (8)0.9461 (6)0.043 (2)*0.50
H18A2.11501.14510.91210.051*0.50
H18B2.06231.11000.99530.051*0.50
H18C1.97571.20810.96050.051*0.50
C18'2.0038 (18)1.0758 (10)0.9473 (7)0.061 (3)*0.50
H18D2.09981.06730.91030.073*0.50
H18E2.01341.02390.98620.073*0.50
H18F2.03381.14610.97610.073*0.50
C192.2091 (16)1.0405 (10)0.6988 (7)0.055 (3)*0.50
H19A2.27811.02260.65390.066*0.50
H19B2.23410.99430.74100.066*0.50
H19C2.25231.11370.72070.066*0.50
C19'2.2224 (15)1.0929 (9)0.6888 (6)0.044 (3)*0.50
H19D2.29391.08880.64290.053*0.50
H19E2.29601.06480.73410.053*0.50
H19F2.20891.16620.70440.053*0.50
C201.6763 (9)1.0408 (5)1.0438 (3)0.0575 (15)
H20A1.77971.09501.06990.069*
C211.7665 (15)0.9468 (7)1.0557 (6)0.046 (2)*0.50
H21A1.76330.92141.10820.055*0.50
H21B1.90660.96131.04740.055*0.50
H21C1.69960.89051.01530.055*0.50
C21'1.6609 (18)0.9116 (8)1.0410 (7)0.062 (3)*0.50
H21D1.78680.89801.02300.074*0.50
H21E1.54510.87721.00310.074*0.50
H21F1.65110.88681.09330.074*0.50
C221.4985 (8)1.0604 (5)1.0841 (3)0.0614 (14)
H22A1.38191.01721.05510.074*
H22B1.47801.13241.08080.074*
C231.5144 (9)1.0376 (5)1.1713 (3)0.0628 (16)
H23A1.64621.06391.19890.075*
H23B1.48880.96341.17550.075*
C241.3632 (10)1.0928 (5)1.2060 (3)0.0598 (16)
O11.1849 (6)1.0580 (3)1.1985 (2)0.0762 (12)
O21.4379 (6)1.1860 (3)1.2438 (2)0.0806 (13)
H2O1.30401.23951.25610.097*
C310.2433 (8)0.4757 (4)0.0975 (3)0.0487 (14)
H31A0.15580.45710.13530.058*
H31B0.26900.41170.07070.058*
C320.4406 (8)0.5342 (4)0.1424 (3)0.0500 (13)
H32A0.53450.54790.10600.060*
H32B0.49660.49190.18120.060*
C330.4027 (8)0.6368 (4)0.1827 (3)0.0535 (15)
H33A0.31830.62280.22240.064*
C340.3066 (10)0.7020 (4)0.1235 (3)0.0662 (18)
H34A0.39170.71780.08430.079*
H34B0.28350.76700.14970.079*
C350.091 (2)0.6330 (10)0.0806 (8)0.049 (5)*0.50
H35A0.01180.61270.12080.059*0.50
C35'0.130 (2)0.6539 (10)0.0777 (8)0.052 (5)*0.50
H35B0.03510.64420.11410.062*0.50
C360.0304 (16)0.6927 (8)0.0202 (6)0.048 (3)*0.50
H36A0.05380.75770.04620.057*0.50
H36B0.15830.65110.00180.057*0.50
C36'0.0566 (18)0.7336 (9)0.0255 (6)0.058 (3)*0.50
H36C0.07100.80040.05640.069*0.50
H36D0.08310.71330.00550.069*0.50
C370.0769 (17)0.7152 (8)0.0500 (6)0.048 (3)*0.50
H37A0.16850.77870.03370.057*0.50
H37B0.02370.73240.09020.057*0.50
C37'0.1729 (18)0.7453 (8)0.0438 (6)0.054 (3)*0.50
H37C0.31380.76520.02590.065*0.50
H37D0.12520.79570.07760.065*0.50
C380.1861 (18)0.6445 (9)0.0908 (6)0.044 (3)*0.50
H38A0.07160.60200.12190.053*0.50
C38'0.1195 (18)0.6146 (8)0.0925 (5)0.036 (3)*0.50
H38B0.01900.58550.10710.044*0.50
C390.2480 (8)0.5575 (4)0.0353 (3)0.0438 (12)
H39A0.38000.58720.00970.053*
C400.1344 (8)0.5393 (4)0.0358 (3)0.0485 (14)
C410.2861 (8)0.4561 (4)0.0814 (3)0.0502 (13)
H41A0.16010.41310.10040.060*
H41B0.36370.41740.04580.060*
C420.3977 (7)0.4783 (4)0.1523 (3)0.0455 (13)
H42A0.40800.41260.18100.055*
H42B0.53130.51230.13250.055*
C430.2940 (7)0.5464 (4)0.2090 (3)0.0441 (13)
C440.3073 (17)0.6590 (8)0.1569 (5)0.034 (3)*0.50
H44A0.43960.69730.14210.041*0.50
C44'0.2409 (17)0.6353 (8)0.1602 (6)0.034 (3)*0.50
H44B0.36940.65440.12780.041*0.50
C450.1640 (17)0.7060 (8)0.2235 (6)0.049 (3)*0.50
H45A0.16020.77960.21120.058*0.50
H45B0.03030.66850.23310.058*0.50
C45'0.2554 (19)0.7357 (8)0.2146 (6)0.055 (3)*0.50
H45C0.32560.79770.18300.065*0.50
H45D0.12350.74940.23510.065*0.50
C460.2830 (17)0.6827 (8)0.2933 (6)0.045 (3)*0.50
H46A0.36820.74540.30080.054*0.50
H46B0.19260.66070.34180.054*0.50
C46'0.3689 (18)0.7070 (8)0.2836 (6)0.051 (3)*0.50
H46C0.48970.75530.28140.061*0.50
H46D0.28680.70800.33390.061*0.50
C470.4175 (7)0.5934 (4)0.2713 (3)0.0461 (12)
H47A0.54970.62360.24620.055*0.50
H47B0.55310.60450.24440.055*0.50
C480.0925 (8)0.4863 (6)0.2510 (3)0.0744 (19)
H48A0.01690.45580.21140.089*
H48B0.11700.43040.28920.089*
H48C0.01500.53400.28010.089*
C490.0747 (8)0.4730 (6)0.0091 (3)0.085 (2)
H49A0.15200.48120.05300.102*
H49B0.05880.39900.00210.102*
H49C0.14300.49710.03910.102*
C500.4281 (7)0.5270 (4)0.3486 (3)0.0438 (12)
H50A0.29430.50960.37690.053*
C510.5107 (7)0.4253 (4)0.3351 (3)0.0474 (12)
H51A0.52820.39130.38660.057*
H51B0.41790.37890.30980.057*
H51C0.63960.43980.30000.057*
C520.5541 (8)0.5915 (4)0.4010 (3)0.0532 (13)
H52A0.69010.60590.37460.064*
H52B0.50510.65760.40610.064*
C530.5527 (8)0.5372 (4)0.4847 (3)0.0516 (14)
H53A0.55780.59010.52130.062*
H53B0.42770.49180.50000.062*
C540.7206 (9)0.4731 (5)0.4931 (3)0.0533 (14)
O30.8887 (6)0.4972 (4)0.4608 (2)0.0811 (13)
O40.6615 (6)0.3865 (3)0.5426 (2)0.0624 (10)
H4O0.80290.32680.54660.075*
O51.5284 (6)0.8691 (3)0.4831 (2)0.0741 (13)
O61.5617 (5)0.9339 (3)0.3666 (2)0.0639 (11)
C1L1.4641 (8)0.8839 (4)0.4068 (3)0.0517 (14)
C2L1.2535 (8)0.8309 (4)0.3799 (3)0.0500 (14)
C3L1.1647 (8)0.8475 (4)0.3059 (3)0.0568 (15)
H3LA1.23820.89130.27370.068*
C4L0.9690 (9)0.8010 (4)0.2769 (3)0.0577 (15)
H4LA0.90800.81270.22470.069*
C5L0.8620 (8)0.7376 (4)0.3238 (3)0.0465 (13)
C6L0.9570 (8)0.7223 (4)0.3997 (3)0.0530 (14)
H6LA0.88570.67920.43300.064*
C7L1.1504 (8)0.7674 (4)0.4270 (3)0.0522 (14)
H7LA1.21430.75520.47860.063*
C8L0.6570 (9)0.6850 (4)0.2962 (3)0.0518 (14)
O70.5940 (6)0.6959 (3)0.2201 (2)0.0763 (13)
O80.5577 (6)0.6349 (3)0.3369 (2)0.0691 (12)
N1S1.1780 (8)1.3140 (4)1.2679 (3)0.0588 (12)
C1S0.9871 (11)1.2906 (5)1.2347 (3)0.0678 (17)
H1SA0.94481.22521.20220.081*
C2S0.8487 (11)1.3570 (6)1.2440 (4)0.0793 (19)
H2SA0.71211.33841.21900.095*
C3S0.9084 (11)1.4498 (5)1.2901 (4)0.0738 (18)
H3SA0.81401.49711.29910.089*
C4S1.1048 (10)1.4751 (5)1.3234 (3)0.0620 (16)
H4SA1.15041.54111.35480.074*
C5S1.2344 (9)1.4061 (5)1.3116 (3)0.0559 (15)
H5SA1.37221.42461.33520.067*
N2S0.9283 (7)0.2582 (4)0.5608 (3)0.0555 (12)
C6S1.1203 (10)0.2788 (5)0.5269 (3)0.0577 (15)
H6SA1.16220.34300.49290.069*
C7S1.2576 (9)0.2132 (5)0.5387 (4)0.0646 (16)
H7SA1.39320.23040.51230.078*
C8S1.1988 (10)0.1224 (5)0.5871 (4)0.0639 (17)
H8SA1.29550.07710.59770.077*
C9S1.0027 (9)0.0974 (4)0.6221 (3)0.0601 (16)
H9SA0.95760.03280.65520.072*
C10S0.8726 (9)0.1678 (4)0.6075 (3)0.0520 (14)
H10A0.73510.15220.63200.062*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.096 (5)0.093 (5)0.050 (3)0.068 (4)0.020 (3)0.017 (3)
C20.124 (6)0.048 (3)0.059 (4)0.029 (4)0.040 (4)0.007 (3)
C30.053 (3)0.046 (3)0.049 (3)0.016 (3)0.011 (3)0.006 (3)
C40.032 (3)0.045 (3)0.038 (3)0.002 (2)0.002 (2)0.008 (2)
C50.037 (3)0.049 (3)0.037 (3)0.004 (2)0.009 (2)0.001 (2)
C60.077 (4)0.052 (3)0.051 (3)0.017 (3)0.017 (3)0.005 (3)
C70.087 (4)0.032 (3)0.055 (3)0.005 (3)0.024 (3)0.004 (2)
C80.032 (3)0.059 (3)0.044 (3)0.001 (2)0.002 (2)0.003 (3)
C90.057 (4)0.054 (3)0.039 (3)0.032 (3)0.005 (2)0.010 (2)
C100.036 (3)0.086 (4)0.046 (3)0.018 (3)0.003 (3)0.002 (3)
C130.045 (3)0.076 (4)0.043 (3)0.032 (3)0.005 (2)0.007 (3)
C140.039 (3)0.034 (3)0.040 (3)0.003 (2)0.004 (2)0.000 (2)
C150.119 (5)0.041 (3)0.068 (4)0.015 (3)0.038 (4)0.002 (3)
C160.082 (4)0.052 (3)0.061 (3)0.013 (3)0.028 (3)0.010 (3)
C170.046 (3)0.040 (3)0.046 (3)0.013 (2)0.001 (2)0.003 (2)
C200.064 (4)0.069 (4)0.043 (3)0.023 (3)0.002 (3)0.012 (3)
C220.073 (4)0.067 (4)0.047 (3)0.019 (3)0.014 (3)0.003 (3)
C230.073 (4)0.066 (4)0.051 (3)0.009 (3)0.013 (3)0.010 (3)
C240.067 (4)0.066 (4)0.045 (3)0.004 (4)0.008 (3)0.012 (3)
O10.069 (3)0.072 (3)0.088 (3)0.001 (2)0.022 (2)0.007 (2)
O20.077 (3)0.069 (3)0.092 (3)0.002 (2)0.021 (3)0.011 (3)
C310.056 (3)0.047 (3)0.040 (3)0.001 (3)0.008 (3)0.001 (2)
C320.047 (3)0.066 (4)0.036 (3)0.007 (3)0.001 (2)0.013 (3)
C330.057 (4)0.064 (4)0.033 (3)0.014 (3)0.010 (3)0.002 (3)
C340.113 (5)0.049 (3)0.043 (3)0.019 (4)0.031 (4)0.000 (3)
C390.046 (3)0.051 (3)0.032 (3)0.015 (2)0.008 (2)0.000 (2)
C400.042 (3)0.068 (4)0.032 (3)0.013 (3)0.005 (2)0.005 (3)
C410.063 (4)0.046 (3)0.041 (3)0.010 (3)0.007 (3)0.001 (2)
C420.056 (3)0.043 (3)0.040 (3)0.022 (3)0.004 (2)0.003 (2)
C430.046 (3)0.060 (3)0.028 (2)0.021 (3)0.005 (2)0.003 (2)
C470.058 (3)0.045 (3)0.037 (3)0.017 (2)0.002 (2)0.004 (2)
C480.044 (3)0.144 (6)0.035 (3)0.021 (4)0.001 (3)0.008 (3)
C490.039 (3)0.163 (7)0.046 (3)0.008 (4)0.001 (3)0.011 (4)
C500.040 (3)0.049 (3)0.040 (3)0.004 (2)0.001 (2)0.001 (2)
C510.054 (3)0.040 (3)0.049 (3)0.008 (2)0.013 (2)0.000 (2)
C520.072 (4)0.043 (3)0.042 (3)0.003 (3)0.009 (3)0.001 (2)
C530.057 (3)0.061 (3)0.037 (3)0.001 (3)0.011 (3)0.013 (3)
C540.055 (4)0.061 (4)0.041 (3)0.004 (3)0.009 (3)0.006 (3)
O30.048 (3)0.107 (3)0.080 (3)0.003 (2)0.004 (2)0.011 (3)
O40.059 (3)0.058 (2)0.064 (2)0.003 (2)0.005 (2)0.006 (2)
O50.078 (3)0.084 (3)0.045 (2)0.044 (2)0.019 (2)0.014 (2)
O60.050 (2)0.074 (3)0.066 (2)0.012 (2)0.014 (2)0.018 (2)
C1L0.054 (4)0.049 (3)0.046 (3)0.012 (3)0.017 (3)0.012 (3)
C2L0.063 (4)0.047 (3)0.036 (3)0.007 (3)0.020 (3)0.011 (2)
C3L0.062 (4)0.055 (4)0.051 (4)0.011 (3)0.024 (3)0.006 (3)
C4L0.067 (4)0.057 (4)0.044 (3)0.014 (3)0.018 (3)0.007 (3)
C5L0.049 (3)0.045 (3)0.039 (3)0.013 (3)0.013 (3)0.015 (2)
C6L0.057 (4)0.053 (3)0.043 (3)0.017 (3)0.016 (3)0.005 (3)
C7L0.056 (4)0.051 (3)0.043 (3)0.009 (3)0.010 (3)0.009 (3)
C8L0.063 (4)0.043 (3)0.046 (3)0.004 (3)0.011 (3)0.006 (3)
O70.083 (3)0.098 (3)0.032 (2)0.039 (3)0.006 (2)0.002 (2)
O80.056 (3)0.095 (3)0.047 (2)0.020 (2)0.001 (2)0.019 (2)
N1S0.063 (3)0.057 (3)0.056 (3)0.002 (3)0.013 (3)0.007 (2)
C1S0.075 (5)0.054 (4)0.064 (4)0.019 (4)0.003 (4)0.009 (3)
C2S0.064 (5)0.068 (5)0.102 (5)0.003 (4)0.001 (4)0.027 (4)
C3S0.068 (5)0.058 (4)0.095 (5)0.014 (4)0.011 (4)0.006 (4)
C4S0.066 (5)0.060 (4)0.060 (4)0.007 (3)0.009 (3)0.009 (3)
C5S0.058 (4)0.054 (4)0.052 (3)0.002 (3)0.006 (3)0.005 (3)
N2S0.066 (3)0.056 (3)0.048 (3)0.008 (2)0.019 (3)0.009 (2)
C6S0.062 (4)0.058 (4)0.052 (3)0.000 (3)0.011 (3)0.008 (3)
C7S0.048 (4)0.072 (4)0.070 (4)0.008 (3)0.008 (3)0.010 (4)
C8S0.056 (4)0.064 (4)0.079 (4)0.011 (3)0.025 (4)0.018 (4)
C9S0.074 (5)0.053 (4)0.052 (3)0.000 (3)0.014 (3)0.003 (3)
C10S0.061 (4)0.055 (4)0.039 (3)0.003 (3)0.008 (3)0.003 (3)
Geometric parameters (Å, º) top
C1—C21.513 (9)C36—H36B0.9600
C1—C101.539 (8)C36'—C37'1.518 (13)
C1—H1A0.9603C36'—H36C0.9600
C1—H1B0.9600C36'—H36D0.9600
C2—C31.495 (8)C37—C381.444 (12)
C2—H2A0.9602C37—H37A0.9600
C2—H2B0.9599C37—H37B0.9600
C3—O51.448 (6)C37'—C38'1.790 (13)
C3—C41.509 (7)C37'—H37C0.9600
C3—H3A0.9601C37'—H37D0.9600
C4—C51.517 (6)C38—C441.496 (13)
C4—H4A0.9599C38—C391.583 (11)
C4—H4B0.9601C38—H38A0.9600
C5—C61.518 (7)C38'—C391.517 (10)
C5—C101.537 (7)C38'—C44'1.530 (13)
C5—H5A0.9597C38'—H38B0.9600
C6—C71.527 (7)C39—C411.542 (6)
C6—H6A0.9599C39—C401.543 (7)
C6—H6B0.9601C39—H39A0.9600
C7—C81.520 (7)C40—C491.554 (7)
C7—H7A0.9602C41—C421.541 (6)
C7—H7B0.9600C41—H41A0.9600
C8—C141.520 (6)C41—H41B0.9599
C8—C91.528 (6)C42—C431.520 (6)
C8—H8A0.9601C42—H42A0.9599
C9—C111.537 (10)C42—H42B0.9600
C9—C101.566 (7)C43—C44'1.476 (11)
C9—C11'1.586 (10)C43—C481.537 (7)
C9—H9A0.9601C43—C471.555 (6)
C9—H9B0.9600C43—C441.628 (11)
C10—C191.464 (12)C44—C451.600 (13)
C10—C19'1.656 (12)C44—H44A0.9600
C11—C121.542 (12)C44'—C45'1.651 (13)
C11—H11A0.9600C44'—H44B0.9600
C11—H11B0.9600C45—C461.562 (12)
C11'—C12'1.548 (13)C45—H45A0.9599
C11'—H11C0.9599C45—H45B0.9600
C11'—H11D0.9600C45'—C46'1.542 (13)
C12—C131.417 (10)C45'—H45C0.9600
C12—H12A0.9600C45'—H45D0.9600
C12—H12B0.9599C46—C471.595 (10)
C12'—C131.658 (11)C46—H46A0.9600
C12'—H12C0.9599C46—H46B0.9600
C12'—H12D0.9599C46'—C471.564 (10)
C13—C18'1.459 (13)C46'—H46C0.9600
C13—C141.535 (7)C46'—H46D0.9600
C13—C171.537 (6)C47—C501.532 (6)
C13—C181.681 (11)C47—H47A0.9600
C14—C151.520 (7)C47—H47B0.9599
C14—H14A0.9599C48—H48A0.9800
C15—C161.536 (7)C48—H48B0.9800
C15—H15A0.9599C48—H48C0.9800
C15—H15B0.9600C49—H49A0.9800
C16—C171.552 (7)C49—H49B0.9800
C16—H16A0.9601C49—H49C0.9799
C16—H16B0.9601C50—C511.512 (7)
C17—C201.551 (6)C50—C521.539 (6)
C17—H17A0.9601C50—H50A0.9602
C18—H18A0.9802C51—H51A0.9801
C18—H18B0.9799C51—H51B0.9801
C18—H18C0.9799C51—H51C0.9799
C18'—H18D0.9799C52—C531.540 (6)
C18'—H18E0.9801C52—H52A0.9600
C18'—H18F0.9801C52—H52B0.9601
C19—H19A0.9799C53—C541.509 (7)
C19—H19B0.9799C53—H53A0.9601
C19—H19C0.9800C53—H53B0.9600
C19'—H19D0.9800C54—O31.191 (6)
C19'—H19E0.9801C54—O41.329 (6)
C19'—H19F0.9799O4—H4O1.3120
C20—C211.441 (10)O5—C1L1.352 (6)
C20—C221.511 (7)O6—C1L1.188 (6)
C20—C21'1.651 (11)C1L—C2L1.500 (7)
C20—H20A0.9600C2L—C3L1.367 (7)
C21—H21A0.9801C2L—C7L1.385 (6)
C21—H21B0.9800C3L—C4L1.395 (7)
C21—H21C0.9800C3L—H3LA0.9602
C21'—H21D0.9800C4L—C5L1.396 (7)
C21'—H21E0.9801C4L—H4LA0.9603
C21'—H21F0.9801C5L—C6L1.406 (7)
C22—C231.531 (7)C5L—C8L1.468 (7)
C22—H22A0.9601C6L—C7L1.371 (7)
C22—H22B0.9599C6L—H6LA0.9599
C23—C241.485 (8)C7L—H7LA0.9601
C23—H23A0.9600C8L—O81.201 (6)
C23—H23B0.9599C8L—O71.335 (6)
C24—O11.224 (6)N1S—C1S1.330 (7)
C24—O21.324 (7)N1S—C5S1.336 (7)
O2—H2O1.2409N1S—H2O1.3872
C31—C321.525 (7)C1S—C2S1.367 (9)
C31—C401.549 (7)C1S—H1SA0.9601
C31—H31A0.9598C2S—C3S1.362 (9)
C31—H31B0.9601C2S—H2SA0.9600
C32—C331.512 (7)C3S—C4S1.366 (8)
C32—H32A0.9602C3S—H3SA0.9600
C32—H32B0.9600C4S—C5S1.353 (8)
C33—O71.457 (6)C4S—H4SA0.9599
C33—C341.498 (8)C5S—H5SA0.9600
C33—H33A0.9599N2S—C6S1.338 (7)
C34—C35'1.384 (14)N2S—C10S1.342 (6)
C34—C351.658 (14)N2S—H4O1.3358
C34—H34A0.9601C6S—C7S1.363 (8)
C34—H34B0.9599C6S—H6SA0.9600
C35—C401.463 (13)C7S—C8S1.360 (8)
C35—C361.546 (14)C7S—H7SA0.9599
C35—H35A0.9602C8S—C9S1.372 (8)
C35'—C36'1.499 (14)C8S—H8SA0.9599
C35'—C401.596 (14)C9S—C10S1.378 (7)
C35'—H35B0.9599C9S—H9SA0.9601
C36—C371.514 (12)C10S—H10A0.9600
C36—H36A0.9600
C2—C1—C10113.0 (5)C36'—C35'—C40116.9 (9)
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C10—C1—H1A109.0C36'—C35'—H35B105.3
C2—C1—H1B109.1C40—C35'—H35B105.2
C10—C1—H1B108.7C37—C36—C35112.0 (9)
H1A—C1—H1B107.8C37—C36—H36A109.2
C3—C2—C1110.4 (5)C35—C36—H36A109.4
C3—C2—H2A109.5C37—C36—H36B109.6
C1—C2—H2A109.5C35—C36—H36B108.7
C3—C2—H2B109.6H36A—C36—H36B107.8
C1—C2—H2B109.7C35'—C36'—C37'111.6 (9)
H2A—C2—H2B108.1C35'—C36'—H36C109.1
O5—C3—C2107.5 (5)C37'—C36'—H36C109.0
O5—C3—C4110.3 (4)C35'—C36'—H36D109.7
C2—C3—C4110.8 (4)C37'—C36'—H36D109.3
O5—C3—H3A109.4H36C—C36'—H36D108.0
C2—C3—H3A109.5C38—C37—C36126.3 (9)
C4—C3—H3A109.4C38—C37—H37A106.1
C3—C4—C5112.5 (4)C36—C37—H37A106.2
C3—C4—H4A108.9C38—C37—H37B105.2
C5—C4—H4A108.9C36—C37—H37B105.3
C3—C4—H4B109.1H37A—C37—H37B106.3
C5—C4—H4B109.4C36'—C37'—C38'100.7 (8)
H4A—C4—H4B107.8C36'—C37'—H37C111.5
C4—C5—C6112.4 (4)C38'—C37'—H37C111.7
C4—C5—C10112.5 (4)C36'—C37'—H37D111.7
C6—C5—C10111.6 (4)C38'—C37'—H37D111.7
C4—C5—H5A106.4H37C—C37'—H37D109.3
C6—C5—H5A106.9C37—C38—C44131.5 (9)
C10—C5—H5A106.5C37—C38—C39109.9 (7)
C5—C6—C7112.0 (4)C44—C38—C39114.3 (7)
C5—C6—H6A109.4C37—C38—H38A96.8
C7—C6—H6A109.3C44—C38—H38A96.8
C5—C6—H6B108.9C39—C38—H38A96.6
C7—C6—H6B109.2C39—C38'—C44'105.3 (7)
H6A—C6—H6B108.0C39—C38'—C37'100.4 (7)
C8—C7—C6112.5 (4)C44'—C38'—C37'96.4 (8)
C8—C7—H7A109.2C39—C38'—H38B117.3
C6—C7—H7A109.0C44'—C38'—H38B117.1
C8—C7—H7B108.9C37'—C38'—H38B117.2
C6—C7—H7B109.2C38'—C39—C41107.5 (5)
H7A—C7—H7B107.9C38'—C39—C40106.9 (5)
C7—C8—C14112.0 (4)C41—C39—C40114.6 (4)
C7—C8—C9110.9 (4)C41—C39—C38113.6 (5)
C14—C8—C9108.8 (4)C40—C39—C38117.8 (5)
C7—C8—H8A108.4C38'—C39—H39A123.0
C14—C8—H8A108.4C41—C39—H39A102.7
C9—C8—H8A108.3C40—C39—H39A102.5
C8—C9—C11103.7 (5)C38—C39—H39A102.8
C8—C9—C10111.6 (4)C35—C40—C39116.7 (7)
C11—C9—C10109.2 (5)C35—C40—C31106.2 (6)
C8—C9—C11'117.3 (5)C39—C40—C31112.7 (4)
C10—C9—C11'118.5 (5)C35—C40—C49104.0 (7)
C8—C9—H9A110.6C39—C40—C49111.6 (4)
C11—C9—H9A110.3C31—C40—C49104.6 (5)
C10—C9—H9A111.1C39—C40—C35'105.2 (6)
C8—C9—H9B101.8C31—C40—C35'108.1 (5)
C10—C9—H9B102.3C49—C40—C35'114.8 (7)
C11'—C9—H9B101.8C42—C41—C39112.6 (4)
C19—C10—C5124.5 (7)C42—C41—H41A109.1
C19—C10—C194.3 (6)C39—C41—H41A109.1
C5—C10—C1108.5 (4)C42—C41—H41B109.1
C19—C10—C9107.4 (6)C39—C41—H41B109.0
C5—C10—C9108.9 (4)H41A—C41—H41B107.8
C1—C10—C9112.5 (5)C43—C42—C41113.0 (4)
C5—C10—C19'100.7 (5)C43—C42—H42A108.8
C1—C10—C19'112.5 (6)C41—C42—H42A108.9
C9—C10—C19'112.9 (5)C43—C42—H42B109.2
C9—C11—C12110.2 (7)C41—C42—H42B109.0
C9—C11—H11A109.3H42A—C42—H42B107.8
C12—C11—H11A109.6C44'—C43—C42107.1 (5)
C9—C11—H11B109.7C44'—C43—C48105.0 (6)
C12—C11—H11B109.9C42—C43—C48110.1 (4)
H11A—C11—H11B108.2C44'—C43—C47107.4 (5)
C12'—C11'—C9115.2 (7)C42—C43—C47116.5 (4)
C12'—C11'—H11C108.4C48—C43—C47110.1 (4)
C9—C11'—H11C108.4C42—C43—C44104.4 (4)
C12'—C11'—H11D108.6C48—C43—C44121.6 (5)
C9—C11'—H11D108.5C47—C43—C4493.8 (5)
H11C—C11'—H11D107.5C38—C44—C43108.8 (8)
C13—C12—C11116.5 (8)C45—C44—C4393.8 (6)
C13—C12—H12A107.6C38—C44—H44A115.9
C11—C12—H12A108.1C45—C44—H44A115.7
C13—C12—H12B108.8C43—C44—H44A115.5
C11—C12—H12B108.1C43—C44'—C38'120.1 (8)
H12A—C12—H12B107.4C43—C44'—C45'105.7 (7)
C11'—C12'—C13107.5 (8)C38'—C44'—C45'129.7 (8)
C11'—C12'—H12C110.0C43—C44'—H44B97.0
C13—C12'—H12C109.9C38'—C44'—H44B97.0
C11'—C12'—H12D110.2C45'—C44'—H44B96.9
C13—C12'—H12D110.7C46—C45—C4496.4 (7)
H12C—C12'—H12D108.5C46—C45—H45A113.1
C12—C13—C18'85.4 (7)C44—C45—H45A112.1
C12—C13—C14109.6 (5)C46—C45—H45B111.9
C18'—C13—C14125.1 (6)C44—C45—H45B112.7
C12—C13—C17127.1 (6)H45A—C45—H45B110.0
C18'—C13—C17111.6 (6)C46'—C45'—C44'107.7 (7)
C14—C13—C17100.5 (4)C46'—C45'—H45C110.1
C18'—C13—C12'106.2 (7)C44'—C45'—H45C110.3
C14—C13—C12'103.5 (5)C46'—C45'—H45D110.1
C17—C13—C12'109.1 (5)C44'—C45'—H45D110.2
C12—C13—C18109.4 (7)H45C—C45'—H45D108.5
C14—C13—C18101.2 (5)C45—C46—C47108.8 (7)
C17—C13—C18106.1 (5)C45—C46—H46A109.4
C12'—C13—C18131.9 (6)C47—C46—H46A109.3
C15—C14—C8119.3 (4)C45—C46—H46B110.4
C15—C14—C13104.5 (4)C47—C46—H46B110.4
C8—C14—C13115.9 (4)H46A—C46—H46B108.4
C15—C14—H14A105.3C45'—C46'—C47104.8 (7)
C8—C14—H14A105.1C45'—C46'—H46C110.8
C13—C14—H14A105.5C47—C46'—H46C110.9
C14—C15—C16104.7 (4)C45'—C46'—H46D110.8
C14—C15—H15A110.5C47—C46'—H46D110.7
C16—C15—H15A110.7H46C—C46'—H46D108.9
C14—C15—H15B111.1C50—C47—C43119.8 (4)
C16—C15—H15B111.0C50—C47—C46'114.0 (5)
H15A—C15—H15B108.9C43—C47—C46'109.4 (5)
C15—C16—C17106.3 (4)C50—C47—C46107.6 (5)
C15—C16—H16A110.7C43—C47—C4696.9 (5)
C17—C16—H16A110.5C50—C47—H47A110.3
C15—C16—H16B110.4C43—C47—H47A110.4
C17—C16—H16B110.4C46'—C47—H47A88.7
H16A—C16—H16B108.6C46—C47—H47A111.0
C13—C17—C20120.4 (4)C50—C47—H47B103.9
C13—C17—C16104.1 (4)C43—C47—H47B104.0
C20—C17—C16112.8 (4)C46'—C47—H47B103.9
C13—C17—H17A106.5C46—C47—H47B126.1
C20—C17—H17A105.9C43—C48—H48A109.5
C16—C17—H17A106.2C43—C48—H48B109.4
C13—C18—H18A113.0H48A—C48—H48B109.8
C13—C18—H18B108.7C43—C48—H48C110.0
H18A—C18—H18B109.0H48A—C48—H48C109.8
C13—C18—H18C109.1H48B—C48—H48C108.3
H18A—C18—H18C109.0C40—C49—H49A107.0
H18B—C18—H18C107.8C40—C49—H49B109.6
C13—C18—H18D82.9H49A—C49—H49B110.4
C13—C18'—H18A107.8C40—C49—H49C110.8
C13—C18'—H18B135.0H49A—C49—H49C110.4
C13—C18'—H18D108.9H49B—C49—H49C108.6
C13—C18'—H18E108.9C51—C50—C47113.3 (4)
C12—C18'—H18E87.9C51—C50—C52109.9 (4)
H18D—C18'—H18E109.9C47—C50—C52110.0 (4)
C13—C18'—H18F110.9C51—C50—H50A107.8
H18D—C18'—H18F109.9C47—C50—H50A107.8
H18E—C18'—H18F108.3C52—C50—H50A107.8
C10—C19—H19A103.1C50—C51—H51A108.6
C10—C19—H19B110.8C50—C51—H51B109.9
H19A—C19—H19B111.1H51A—C51—H51B110.1
C10—C19—H19C111.7C50—C51—H51C109.8
H19A—C19—H19C111.1H51A—C51—H51C110.1
H19B—C19—H19C109.0H51B—C51—H51C108.4
C10—C19'—H19D108.0C50—C52—C53114.4 (4)
C10—C19'—H19E110.0C50—C52—H52A108.6
H19D—C19'—H19E110.2C53—C52—H52A108.6
C10—C19'—H19F109.9C50—C52—H52B108.8
H19D—C19'—H19F110.2C53—C52—H52B108.7
H19E—C19'—H19F108.5H52A—C52—H52B107.6
C21—C20—C22119.8 (6)C54—C53—C52115.5 (4)
C21—C20—C17116.6 (5)C54—C53—H53A108.6
C22—C20—C17109.6 (4)C52—C53—H53A108.4
C22—C20—C21'101.4 (6)C54—C53—H53B108.3
C17—C20—C21'108.7 (5)C52—C53—H53B108.3
C21—C20—H20A102.4H53A—C53—H53B107.5
C22—C20—H20A102.8O3—C54—O4123.0 (5)
C17—C20—H20A102.8O3—C54—C53124.6 (5)
C21'—C20—H20A130.5O4—C54—C53112.3 (5)
C20—C21—H21A115.1C54—O4—H4O112.9
C20—C21—H21B107.8C1L—O5—C3117.4 (4)
H21A—C21—H21B108.5O6—C1L—O5124.0 (5)
C20—C21—H21C109.2O6—C1L—C2L124.4 (5)
H21A—C21—H21C108.5O5—C1L—C2L111.5 (5)
H21B—C21—H21C107.5C3L—C2L—C7L120.4 (5)
C20—C21'—H21D102.8C3L—C2L—C1L117.2 (5)
C20—C21'—H21E111.0C7L—C2L—C1L122.3 (5)
H21D—C21'—H21E111.0C2L—C3L—C4L120.6 (5)
C20—C21'—H21F111.9C2L—C3L—H3LA119.6
H21D—C21'—H21F111.0C4L—C3L—H3LA119.9
H21E—C21'—H21F109.0C3L—C4L—C5L119.8 (5)
C20—C22—C23115.5 (5)C3L—C4L—H4LA120.1
C20—C22—H22A108.1C5L—C4L—H4LA120.1
C23—C22—H22A108.1C4L—C5L—C6L118.3 (5)
C20—C22—H22B108.8C4L—C5L—C8L122.5 (5)
C23—C22—H22B108.6C6L—C5L—C8L119.1 (5)
H22A—C22—H22B107.5C7L—C6L—C5L121.1 (5)
C24—C23—C22106.5 (4)C7L—C6L—H6LA119.3
C24—C23—H23A110.0C5L—C6L—H6LA119.5
C22—C23—H23A110.1C6L—C7L—C2L119.7 (5)
C24—C23—H23B110.7C6L—C7L—H7LA120.2
C22—C23—H23B110.8C2L—C7L—H7LA120.0
H23A—C23—H23B108.7O8—C8L—O7123.2 (5)
O1—C24—O2122.6 (6)O8—C8L—C5L123.9 (5)
O1—C24—C23123.9 (6)O7—C8L—C5L112.9 (5)
O2—C24—C23113.5 (6)C8L—O7—C33118.3 (4)
C24—O2—H2O111.7C1S—N1S—C5S118.0 (5)
C32—C31—C40114.1 (4)C1S—N1S—H2O117.6
C32—C31—H31A108.6C5S—N1S—H2O124.5
C40—C31—H31A108.7N1S—C1S—C2S122.5 (6)
C32—C31—H31B108.8N1S—C1S—H1SA119.0
C40—C31—H31B108.9C2S—C1S—H1SA118.5
H31A—C31—H31B107.6C3S—C2S—C1S118.6 (7)
C33—C32—C31109.2 (4)C3S—C2S—H2SA120.6
C33—C32—H32A109.8C1S—C2S—H2SA120.8
C31—C32—H32A109.8C2S—C3S—C4S119.3 (6)
C33—C32—H32B110.0C2S—C3S—H3SA120.6
C31—C32—H32B109.8C4S—C3S—H3SA120.1
H32A—C32—H32B108.3C5S—C4S—C3S119.1 (6)
O7—C33—C34108.0 (4)C5S—C4S—H4SA120.4
O7—C33—C32108.8 (4)C3S—C4S—H4SA120.5
C34—C33—C32110.8 (4)N1S—C5S—C4S122.4 (6)
O7—C33—H33A109.6N1S—C5S—H5SA118.9
C34—C33—H33A110.0C4S—C5S—H5SA118.6
C32—C33—H33A109.5C6S—N2S—C10S117.1 (5)
C35'—C34—C33115.6 (7)C6S—N2S—H4O119.4
C33—C34—C35107.4 (6)C10S—N2S—H4O123.5
C35'—C34—H34A102.6N2S—C6S—C7S122.9 (6)
C33—C34—H34A110.5N2S—C6S—H6SA118.1
C35—C34—H34A110.2C7S—C6S—H6SA119.0
C35'—C34—H34B109.0C8S—C7S—C6S119.2 (6)
C33—C34—H34B110.2C8S—C7S—H7SA120.7
C35—C34—H34B110.2C6S—C7S—H7SA120.1
H34A—C34—H34B108.4C7S—C8S—C9S119.8 (6)
C40—C35—C36106.3 (9)C7S—C8S—H8SA119.8
C40—C35—C34108.3 (8)C9S—C8S—H8SA120.4
C36—C35—C34113.3 (10)C8S—C9S—C10S117.8 (5)
C40—C35—H35A109.9C8S—C9S—H9SA121.0
C36—C35—H35A109.5C10S—C9S—H9SA121.2
C34—C35—H35A109.4N2S—C10S—C9S123.2 (5)
C34—C35'—C36'106.7 (10)N2S—C10S—H10A117.7
C34—C35'—C40116.1 (9)C9S—C10S—H10A119.1
C10—C1—C2—C358.3 (6)C37'—C38—C44'—C43168.3 (11)
C1—C2—C3—O5177.6 (4)C44—C38—C44'—C43116 (3)
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C3—C4—C5—C1053.9 (5)C39—C38—C44'—C38'77.8 (19)
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C16—C17—C20—C21'166.7 (6)C46—C45—C45'—C44104.5 (7)
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C21'—C20—C22—C2367.6 (7)C44—C45—C45'—C46104.5 (7)
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C22—C23—C24—O181.2 (7)C44'—C45—C45'—C46'103.5 (9)
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C40—C31—C32—C3356.6 (5)C44—C45—C45'—C46'102.6 (10)
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C31—C32—C33—C3456.9 (5)C44—C45—C45'—C44'0.9 (8)
O7—C33—C34—C35'175.0 (7)C46'—C45—C45'—C44'103.5 (9)
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C33—C34—C35—C4064.9 (9)C38'—C44—C45'—C4544.1 (15)
C33—C34—C35—C36177.4 (7)C44'—C44—C45'—C4684 (2)
C33—C34—C35'—C36'177.8 (7)C38—C44—C45'—C46141.1 (10)
C33—C34—C35'—C36170.1 (12)C45—C44—C45'—C4680.8 (14)
C33—C34—C35'—C4049.8 (11)C43—C44—C45'—C4618.3 (11)
C40—C35—C36—C3754.4 (13)C38'—C44—C45'—C46124.9 (9)
C34—C35—C36—C3764.4 (12)C44'—C44—C45'—C46'108 (2)
C36'—C35—C36—C3757.0 (12)C38—C44—C45'—C46'165.2 (10)
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C44'—C38'—C39—C4158.9 (8)C38—C44'—C45'—C4592.7 (16)
C37'—C38'—C39—C41158.5 (5)C43—C44'—C45'—C4585.6 (14)
C44'—C38'—C39—C40177.7 (6)C38'—C44'—C45'—C4570.0 (17)
C37'—C38'—C39—C4078.0 (7)C38—C44'—C45'—C4490 (2)
C37—C38—C39—C41156.7 (8)C43—C44'—C45'—C4491 (2)
C44—C38—C39—C4143.6 (11)C38'—C44'—C45'—C44113 (3)
C37—C38—C39—C4018.6 (12)C45—C44'—C45'—C44177 (3)
C44—C38—C39—C40178.4 (7)C44—C44'—C45'—C46100 (2)
C36—C35—C40—C3957.3 (11)C38—C44'—C45'—C46169.4 (11)
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C36—C35—C40—C31176.2 (8)C38'—C44'—C45'—C46146.7 (11)
C34—C35—C40—C3161.8 (9)C45—C44'—C45'—C4676.7 (14)
C36—C35—C40—C4966.1 (10)C44—C44'—C45'—C46'77 (2)
C34—C35—C40—C49171.8 (6)C38—C44'—C45'—C46'167.3 (11)
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C38—C39—C40—C31164.6 (6)C44—C45'—C46—C46'90.7 (16)
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C32—C31—C40—C3561.0 (8)C46'—C45'—C46—C4772.9 (14)
C32—C31—C40—C3968.0 (5)C44'—C45'—C46—C4735.7 (10)
C32—C31—C40—C49170.6 (4)C45'—C45—C46—C46'5 (2)
C32—C31—C40—C35'47.8 (8)C44'—C45—C46—C46'77.1 (18)
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C36'—C35'—C40—C35105 (4)C44'—C45—C46—C45'82.0 (14)
C36—C35'—C40—C3580 (4)C44—C45—C46—C45'64.8 (13)
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C36'—C35'—C40—C3951.2 (12)C45'—C45—C46—C4785.5 (14)
C36—C35'—C40—C3975.7 (9)C44'—C45—C46—C473.4 (11)
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C36'—C35'—C40—C31171.8 (9)C46'—C45—C46—C4780.5 (16)
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C36—C35'—C40—C4947.5 (10)C45—C46—C46'—C47105.7 (9)
C38'—C39—C41—C4260.7 (7)C45'—C46—C46'—C452.2 (9)
C40—C39—C41—C42179.4 (4)C47—C46—C46'—C45105.7 (9)
C38—C39—C41—C4239.9 (7)C45—C45'—C46'—C465 (2)
C39—C41—C42—C4354.6 (6)C44—C45'—C46'—C4695.0 (16)
C41—C42—C43—C44'46.6 (7)C44'—C45'—C46'—C4677.4 (16)
C41—C42—C43—C4867.0 (5)C45—C45'—C46'—C4771.8 (16)
C41—C42—C43—C47166.8 (4)C44—C45'—C46'—C4718.3 (11)
C41—C42—C43—C4465.1 (6)C46—C45'—C46'—C4776.7 (14)
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C38'—C38—C44—C45'92 (2)C45'—C45—C46'—C46174 (2)
C44'—C38—C44—C45'83 (2)C44'—C45—C46'—C46106.6 (18)
C37—C38—C44—C45'28.3 (19)C44—C45—C46'—C46120.6 (17)
C37'—C38—C44—C45'53.1 (14)C44'—C45—C46'—C45'79.3 (15)
C39—C38—C44—C45'177.4 (9)C46—C45—C46'—C45'174 (2)
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C44'—C38—C44—C4560 (2)C45'—C45—C46'—C47112.1 (16)
C37—C38—C44—C4550.7 (16)C44'—C45—C46'—C4732.8 (9)
C37'—C38—C44—C4575.5 (11)C46—C45—C46'—C4773.8 (16)
C39—C38—C44—C45155.1 (8)C44—C45—C46'—C4746.9 (8)
C38'—C38—C44—C4329 (3)C44'—C43—C47—C50157.0 (6)
C44'—C38—C44—C4338.8 (18)C42—C43—C47—C5083.0 (6)
C37—C38—C44—C43149.8 (12)C48—C43—C47—C5043.2 (6)
C37'—C38—C44—C43174.6 (8)C44—C43—C47—C50168.9 (5)
C39—C38—C44—C4355.9 (11)C44'—C43—C47—C46'22.8 (8)
C44'—C38—C44—C38'9 (3)C42—C43—C47—C46'142.8 (6)
C37—C38—C44—C38'120 (3)C48—C43—C47—C46'91.0 (6)
C37'—C38—C44—C38'145 (3)C44—C43—C47—C46'34.6 (7)
C39—C38—C44—C38'85 (2)C44'—C43—C47—C4642.2 (7)
C42—C43—C44—C44'101.1 (19)C42—C43—C47—C46162.2 (6)
C48—C43—C44—C44'24 (2)C48—C43—C47—C4671.6 (6)
C47—C43—C44—C44'140.3 (19)C44—C43—C47—C4654.1 (6)
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C42—C43—C44—C45'166.0 (7)C45'—C46'—C47—C50150.0 (7)
C48—C43—C44—C45'69.0 (9)C45—C46'—C47—C50130.0 (6)
C47—C43—C44—C45'47.4 (8)C46—C46'—C47—C4359.1 (15)
C44'—C43—C44—C3835.8 (17)C45'—C46'—C47—C4312.8 (9)
C42—C43—C44—C3865.2 (8)C45—C46'—C47—C437.1 (7)
C48—C43—C44—C3859.8 (9)C45'—C46'—C47—C4671.9 (15)
C47—C43—C44—C38176.2 (7)C45—C46'—C47—C4652.0 (13)
C44'—C43—C44—C4570.8 (19)C46'—C46—C47—C50110.3 (15)
C42—C43—C44—C45171.9 (6)C45'—C46—C47—C50172.6 (7)
C48—C43—C44—C4546.8 (8)C45—C46—C47—C50146.3 (7)
C47—C43—C44—C4569.5 (6)C46'—C46—C47—C43125.3 (14)
C44'—C43—C44—C38'28.8 (17)C45'—C46—C47—C4348.3 (8)
C42—C43—C44—C38'72.2 (6)C45—C46—C47—C4322.0 (9)
C48—C43—C44—C38'52.8 (7)C45'—C46—C47—C46'77.0 (16)
C47—C43—C44—C38'169.2 (5)C45—C46—C47—C46'103.4 (17)
C38—C38'—C44—C44'168 (4)C43—C47—C50—C5158.0 (6)
C39—C38'—C44—C44'118 (3)C46'—C47—C50—C51169.7 (6)
C37—C38'—C44—C44'129 (3)C46—C47—C50—C51167.0 (5)
C37'—C38'—C44—C44'142 (3)C43—C47—C50—C52178.6 (4)
C38—C38'—C44—C45'96 (3)C46'—C47—C50—C5246.3 (7)
C39—C38'—C44—C45'169.6 (8)C46—C47—C50—C5269.6 (6)
C37—C38'—C44—C45'56.2 (11)C51—C50—C52—C5361.9 (6)
C44'—C38'—C44—C45'73 (3)C47—C50—C52—C53172.6 (4)
C37'—C38'—C44—C45'69.6 (10)C50—C52—C53—C5492.7 (6)
C39—C38'—C44—C3874 (2)C52—C53—C54—O338.1 (7)
C37—C38'—C44—C3839 (2)C52—C53—C54—O4143.2 (4)
C44'—C38'—C44—C38168 (4)C2—C3—O5—C1L151.9 (4)
C37'—C38'—C44—C3826 (2)C4—C3—O5—C1L87.3 (5)
C38—C38'—C44—C45113 (2)C3—O5—C1L—O63.8 (8)
C39—C38'—C44—C45173.1 (7)C3—O5—C1L—C2L175.3 (4)
C37—C38'—C44—C4573.6 (9)O6—C1L—C2L—C3L4.5 (8)
C44'—C38'—C44—C4555 (2)O5—C1L—C2L—C3L174.6 (4)
C37'—C38'—C44—C4587.0 (8)O6—C1L—C2L—C7L175.4 (5)
C38—C38'—C44—C43152 (2)O5—C1L—C2L—C7L5.5 (7)
C39—C38'—C44—C4378.2 (7)C7L—C2L—C3L—C4L0.2 (7)
C37—C38'—C44—C43168.5 (7)C1L—C2L—C3L—C4L179.9 (4)
C44'—C38'—C44—C4339 (2)C2L—C3L—C4L—C5L0.5 (7)
C37'—C38'—C44—C43178.1 (6)C3L—C4L—C5L—C6L0.3 (7)
C45'—C44—C44'—C38117.9 (10)C3L—C4L—C5L—C8L178.9 (5)
C45—C44—C44'—C38119.2 (12)C4L—C5L—C6L—C7L0.6 (7)
C43—C44—C44'—C38138.6 (15)C8L—C5L—C6L—C7L178.1 (4)
C38'—C44—C44'—C383.4 (11)C5L—C6L—C7L—C2L1.3 (7)
C45'—C44—C44'—C43103.4 (9)C3L—C2L—C7L—C6L1.1 (7)
C38—C44—C44'—C43138.6 (15)C1L—C2L—C7L—C6L179.0 (5)
C45—C44—C44'—C43102.2 (8)C4L—C5L—C8L—O8175.7 (5)
C38'—C44—C44'—C43135 (2)C6L—C5L—C8L—O85.7 (8)
C45'—C44—C44'—C38'121.3 (16)C4L—C5L—C8L—O76.2 (7)
C38—C44—C44'—C38'3.4 (11)C6L—C5L—C8L—O7172.4 (5)
C45—C44—C44'—C38'122.5 (19)O8—C8L—O7—C335.4 (8)
C43—C44—C44'—C38'135 (2)C5L—C8L—O7—C33172.7 (4)
C45'—C44—C44'—C451.2 (11)C34—C33—O7—C8L146.4 (5)
C38—C44—C44'—C45119.2 (12)C32—C33—O7—C8L93.2 (5)
C43—C44—C44'—C45102.2 (8)C5S—N1S—C1S—C2S0.2 (8)
C38'—C44—C44'—C45122.5 (19)N1S—C1S—C2S—C3S1.1 (9)
C38—C44—C44'—C45'117.9 (10)C1S—C2S—C3S—C4S2.0 (9)
C45—C44—C44'—C45'1.2 (11)C2S—C3S—C4S—C5S1.8 (9)
C43—C44—C44'—C45'103.4 (9)C1S—N1S—C5S—C4S0.4 (8)
C38'—C44—C44'—C45'121.3 (16)C3S—C4S—C5S—N1S0.5 (8)
C38'—C38—C44'—C44172 (3)C10S—N2S—C6S—C7S0.7 (7)
C37—C38—C44'—C4487 (3)N2S—C6S—C7S—C8S0.0 (8)
C37'—C38—C44'—C4452 (3)C6S—C7S—C8S—C9S1.0 (8)
C39—C38—C44'—C4494 (2)C7S—C8S—C9S—C10S1.2 (8)
C38'—C38—C44'—C4356 (2)C6S—N2S—C10S—C9S0.5 (7)
C37—C38—C44'—C43157.0 (13)C8S—C9S—C10S—N2S0.4 (7)
(6) bis(23-methoxycarbonyl-24-nor-5beta-cholan −3alpha-yl)terephtalate top
Crystal data top
C58H86O8F(000) = 996
Mr = 911.27Dx = 1.167 Mg m3
Monoclinic, C2Cu Kα radiation, λ = 1.54178 Å
a = 31.731 (6) ÅCell parameters from 63 reflections
b = 7.727 (2) Åθ = 16.0–21.4°
c = 11.017 (2) ŵ = 0.59 mm1
β = 106.28 (3)°T = 293 K
V = 2592.9 (10) Å3Needle, colourless
Z = 20.2 × 0.1 × 0.1 mm
Data collection top
KM-4 four circle
diffractometer
Rint = 0.196
Radiation source: fine-focus sealed tubeθmax = 65.8°, θmin = 5.7°
Graphite monochromatorh = 3636
Θ–2Θ scansk = 99
4425 measured reflectionsl = 013
2419 independent reflections2 standard reflections every 100 reflections
715 reflections with I > 2σ(I)
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullRiding
R[F2 > 2σ(F2)] = 0.046 w = 1/[σ2(Fo2) + (0.0586P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.137(Δ/σ)max < 0.001
S = 0.86Δρmax = 0.20 e Å3
2419 reflectionsΔρmin = 0.14 e Å3
299 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.00071 (11)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0 (10)
Crystal data top
C58H86O8V = 2592.9 (10) Å3
Mr = 911.27Z = 2
Monoclinic, C2Cu Kα radiation
a = 31.731 (6) ŵ = 0.59 mm1
b = 7.727 (2) ÅT = 293 K
c = 11.017 (2) Å0.2 × 0.1 × 0.1 mm
β = 106.28 (3)°
Data collection top
KM-4 four circle
diffractometer
715 reflections with I > 2σ(I)
4425 measured reflectionsRint = 0.196
2419 independent reflections2 standard reflections every 100 reflections
Refinement top
R[F2 > 2σ(F2)] = 0.046Riding
wR(F2) = 0.137Δρmax = 0.20 e Å3
S = 0.86Δρmin = 0.14 e Å3
2419 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
299 parametersAbsolute structure parameter: 0 (10)
1 restraint
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
C10.1247 (2)0.2289 (11)0.0345 (7)0.063 (3)
H1A0.10170.21940.04330.075*
H1B0.14310.32450.02680.075*
C20.1033 (3)0.2701 (10)0.1412 (7)0.072 (3)
H2A0.12600.28640.21880.087*
H2B0.08560.37280.12440.087*
C30.0739 (2)0.1225 (13)0.1525 (7)0.072 (3)
H30.04910.11760.07890.087*
C40.0979 (3)0.0482 (12)0.1731 (8)0.073 (3)
H4A0.11870.05120.25530.088*
H4B0.07680.13830.17060.088*
C50.1217 (2)0.0867 (12)0.0728 (7)0.062 (2)
H50.09970.10120.00660.074*
C60.1452 (3)0.2604 (12)0.0990 (8)0.075 (3)
H6A0.12620.34860.11520.090*
H6B0.15440.29510.02670.090*
C70.1876 (3)0.2477 (11)0.2137 (7)0.074 (3)
H7A0.17880.22210.28840.089*
H7B0.20400.35370.22720.089*
C80.2177 (3)0.1015 (11)0.1955 (8)0.061 (3)
H80.22780.12970.12360.073*
C90.1922 (2)0.0709 (12)0.1687 (7)0.054 (2)
H90.18150.09230.24060.065*
C100.1513 (3)0.0601 (12)0.0518 (6)0.053 (2)
C110.2230 (3)0.2229 (11)0.1639 (8)0.075 (3)
H11A0.23250.20720.08930.090*
H11B0.20700.32960.15500.090*
C120.2645 (2)0.2281 (11)0.2769 (8)0.074 (3)
H12A0.28350.31840.26340.089*
H12B0.25540.25730.35040.089*
C130.2895 (2)0.0589 (12)0.2976 (7)0.058 (2)
C140.2569 (3)0.0789 (11)0.3110 (7)0.057 (2)
H140.24530.04460.37910.068*
C150.2855 (3)0.2370 (11)0.3585 (8)0.081 (3)
H15A0.27170.31310.40460.097*
H15B0.29030.29810.28760.097*
C160.3297 (3)0.1541 (13)0.4437 (8)0.085 (3)
H16A0.33310.18240.53070.102*
H16B0.35450.19720.41950.102*
C170.3253 (3)0.0410 (10)0.4253 (7)0.062 (2)
H170.31460.08970.49120.075*
C180.3086 (2)0.0227 (10)0.1883 (6)0.074 (3)
H18A0.32440.08460.20090.089*
H18B0.32810.11530.18200.089*
H18C0.28500.01660.11170.089*
C190.1637 (2)0.0328 (11)0.0699 (6)0.076 (3)
H19A0.18120.06940.06680.092*
H19B0.18020.13240.08170.092*
H19C0.13750.02400.13910.092*
C200.3707 (3)0.1219 (12)0.4403 (7)0.071 (3)
H200.38360.07180.37950.085*
C210.3670 (3)0.3160 (13)0.4184 (9)0.116 (4)
H21A0.34890.34190.33480.139*
H21B0.39540.36740.43070.139*
H21C0.35350.36190.47950.139*
C220.4015 (3)0.0883 (13)0.5720 (7)0.079 (3)
H22A0.39110.15850.62950.095*
H22B0.40060.03070.59620.095*
C230.4485 (3)0.1391 (14)0.5824 (8)0.104 (3)
H23A0.45800.07490.52020.124*
H23B0.44960.26010.56360.124*
C240.4799 (4)0.1115 (19)0.7105 (12)0.118 (5)
C250.5476 (4)0.094 (3)0.8394 (12)0.294 (11)
H25C0.57830.09700.84440.353*
H25B0.54040.01780.86670.353*
H25A0.54110.18170.89290.353*
C1L0.0173 (3)0.1362 (13)0.2566 (8)0.069 (3)
C2L0.0091 (3)0.1497 (10)0.3828 (7)0.055 (2)
C7L0.0423 (2)0.1538 (12)0.4911 (7)0.064 (2)
H7L0.07160.11450.49880.077*
C3L0.0341 (2)0.1547 (11)0.3914 (7)0.078 (3)
H3L0.05590.12760.31390.093*
O50.05878 (18)0.1524 (8)0.2655 (4)0.0811 (19)
O10.4700 (3)0.0817 (13)0.8018 (7)0.136 (4)
O20.5204 (2)0.1156 (13)0.7072 (6)0.148 (3)
O60.01065 (18)0.1132 (13)0.1614 (5)0.131 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.072 (7)0.069 (6)0.051 (6)0.001 (6)0.025 (5)0.006 (5)
C20.075 (6)0.082 (7)0.065 (6)0.009 (6)0.028 (5)0.012 (6)
C30.071 (6)0.097 (8)0.049 (5)0.006 (7)0.017 (5)0.000 (6)
C40.073 (6)0.077 (7)0.075 (6)0.014 (6)0.028 (5)0.002 (6)
C50.070 (6)0.075 (7)0.041 (5)0.018 (6)0.018 (4)0.002 (5)
C60.087 (7)0.062 (7)0.085 (6)0.013 (6)0.038 (5)0.010 (6)
C70.072 (6)0.056 (6)0.094 (7)0.007 (6)0.025 (5)0.003 (5)
C80.078 (7)0.047 (7)0.063 (6)0.012 (6)0.030 (5)0.007 (5)
C90.071 (6)0.041 (6)0.054 (5)0.001 (5)0.024 (4)0.007 (5)
C100.070 (6)0.052 (6)0.042 (5)0.013 (6)0.023 (4)0.008 (5)
C110.080 (7)0.051 (6)0.088 (7)0.013 (6)0.011 (6)0.013 (5)
C120.066 (7)0.064 (7)0.086 (7)0.004 (6)0.010 (6)0.002 (6)
C130.046 (5)0.071 (7)0.057 (6)0.013 (6)0.015 (4)0.007 (5)
C140.064 (6)0.057 (6)0.054 (5)0.002 (6)0.025 (5)0.004 (5)
C150.109 (7)0.049 (6)0.088 (7)0.002 (6)0.031 (6)0.004 (5)
C160.085 (7)0.092 (8)0.075 (7)0.005 (6)0.016 (6)0.003 (6)
C170.078 (6)0.047 (6)0.064 (6)0.005 (6)0.023 (5)0.001 (5)
C180.089 (7)0.076 (7)0.066 (5)0.000 (5)0.033 (5)0.000 (5)
C190.095 (6)0.084 (7)0.051 (5)0.002 (6)0.023 (5)0.004 (5)
C200.071 (6)0.072 (8)0.063 (6)0.005 (6)0.009 (4)0.008 (5)
C210.090 (8)0.090 (8)0.144 (10)0.030 (7)0.008 (7)0.032 (8)
C220.084 (6)0.071 (7)0.075 (6)0.003 (6)0.010 (5)0.007 (6)
C230.093 (7)0.116 (10)0.088 (7)0.009 (8)0.003 (6)0.003 (8)
C240.069 (8)0.113 (11)0.140 (12)0.009 (9)0.023 (9)0.022 (11)
C250.208 (14)0.251 (19)0.280 (17)0.043 (16)0.166 (14)0.084 (18)
C1L0.052 (5)0.104 (8)0.055 (6)0.004 (6)0.022 (5)0.002 (6)
C2L0.047 (5)0.068 (6)0.047 (5)0.002 (5)0.008 (4)0.001 (5)
C7L0.051 (5)0.083 (7)0.059 (5)0.016 (5)0.019 (5)0.006 (6)
C3L0.044 (5)0.123 (8)0.062 (6)0.003 (5)0.010 (4)0.006 (7)
O50.074 (4)0.116 (5)0.060 (4)0.024 (4)0.030 (3)0.017 (4)
O10.148 (7)0.141 (7)0.101 (6)0.001 (6)0.003 (5)0.029 (6)
O20.073 (4)0.239 (10)0.114 (6)0.001 (7)0.002 (4)0.020 (7)
O60.070 (4)0.262 (10)0.052 (3)0.018 (6)0.005 (3)0.017 (6)
Geometric parameters (Å, º) top
C1—C101.536 (9)C13—C171.547 (9)
C1—C21.546 (9)C14—C151.525 (10)
C2—C31.500 (10)C15—C161.586 (10)
C3—O51.472 (8)C16—C171.522 (11)
C3—C41.508 (12)C17—C201.535 (9)
C4—C51.533 (9)C20—C211.519 (11)
C5—C61.524 (11)C20—C221.527 (9)
C5—C101.530 (9)C22—C231.517 (9)
C6—C71.568 (10)C23—C241.497 (12)
C7—C81.528 (9)C24—O11.156 (12)
C8—C141.520 (11)C24—O21.296 (11)
C8—C91.543 (10)C25—O21.481 (11)
C9—C111.538 (10)C1L—O61.182 (8)
C9—C101.555 (8)C1L—O51.298 (7)
C10—C191.515 (8)C1L—C2L1.489 (9)
C11—C121.538 (10)C2L—C7L1.351 (8)
C12—C131.513 (10)C2L—C3L1.400 (8)
C13—C181.518 (9)C7L—C3Li1.390 (9)
C13—C141.521 (10)C3L—C7Li1.390 (9)
C10—C1—C2115.1 (6)C18—C13—C17110.5 (6)
C3—C2—C1108.8 (7)C14—C13—C17101.3 (7)
O5—C3—C2108.0 (7)C8—C14—C13114.7 (7)
O5—C3—C4106.3 (7)C8—C14—C15117.7 (7)
C2—C3—C4112.2 (6)C13—C14—C15103.7 (7)
C3—C4—C5113.0 (7)C14—C15—C16102.8 (7)
C6—C5—C10113.1 (7)C17—C16—C15106.8 (7)
C6—C5—C4110.4 (7)C16—C17—C20110.0 (7)
C10—C5—C4114.4 (7)C16—C17—C13103.0 (7)
C5—C6—C7111.2 (7)C20—C17—C13119.3 (7)
C8—C7—C6111.5 (7)C21—C20—C22108.6 (8)
C14—C8—C7111.7 (7)C21—C20—C17110.9 (7)
C14—C8—C9108.8 (7)C22—C20—C17111.3 (7)
C7—C8—C9110.5 (6)C23—C22—C20112.5 (7)
C11—C9—C8111.2 (6)C24—C23—C22114.5 (9)
C11—C9—C10113.8 (7)O1—C24—O2122.8 (12)
C8—C9—C10112.5 (7)O1—C24—C23125.3 (12)
C19—C10—C5110.8 (7)O2—C24—C23111.8 (12)
C19—C10—C1106.2 (7)O6—C1L—O5125.1 (7)
C5—C10—C1108.0 (6)O6—C1L—C2L123.7 (8)
C19—C10—C9112.1 (6)O5—C1L—C2L111.2 (7)
C5—C10—C9108.7 (6)C7L—C2L—C3L118.3 (7)
C1—C10—C9111.1 (7)C7L—C2L—C1L122.0 (8)
C12—C11—C9113.6 (7)C3L—C2L—C1L119.7 (7)
C13—C12—C11113.1 (7)C2L—C7L—C3Li121.3 (6)
C12—C13—C18110.4 (7)C7Li—C3L—C2L120.3 (6)
C12—C13—C14106.1 (6)C1L—O5—C3119.0 (6)
C18—C13—C14112.5 (7)C24—O2—C25106.2 (10)
C12—C13—C17115.8 (7)
C10—C1—C2—C357.6 (9)C12—C13—C14—C861.6 (9)
C1—C2—C3—O5172.1 (6)C18—C13—C14—C859.2 (9)
C1—C2—C3—C455.4 (8)C17—C13—C14—C8177.1 (6)
O5—C3—C4—C5171.5 (6)C12—C13—C14—C15168.6 (7)
C2—C3—C4—C553.8 (9)C18—C13—C14—C1570.6 (8)
C3—C4—C5—C6180.0 (7)C17—C13—C14—C1547.4 (8)
C3—C4—C5—C1051.1 (10)C8—C14—C15—C16161.4 (7)
C10—C5—C6—C755.2 (9)C13—C14—C15—C1633.5 (8)
C4—C5—C6—C774.4 (8)C14—C15—C16—C177.1 (9)
C5—C6—C7—C853.4 (9)C15—C16—C17—C20149.5 (6)
C6—C7—C8—C14175.3 (7)C15—C16—C17—C1321.3 (9)
C6—C7—C8—C953.9 (8)C12—C13—C17—C16156.1 (7)
C14—C8—C9—C1151.1 (8)C18—C13—C17—C1677.5 (9)
C7—C8—C9—C11174.1 (7)C14—C13—C17—C1641.9 (8)
C14—C8—C9—C10179.8 (6)C12—C13—C17—C2081.8 (9)
C7—C8—C9—C1056.8 (8)C18—C13—C17—C2044.6 (11)
C6—C5—C10—C1967.5 (9)C14—C13—C17—C20164.0 (7)
C4—C5—C10—C19165.0 (7)C16—C17—C20—C21178.3 (7)
C6—C5—C10—C1176.6 (7)C13—C17—C20—C2159.7 (10)
C4—C5—C10—C149.1 (8)C16—C17—C20—C2260.7 (9)
C6—C5—C10—C956.0 (9)C13—C17—C20—C22179.3 (8)
C4—C5—C10—C971.5 (9)C21—C20—C22—C2367.6 (10)
C2—C1—C10—C19172.4 (7)C17—C20—C22—C23170.1 (7)
C2—C1—C10—C553.5 (8)C20—C22—C23—C24179.0 (10)
C2—C1—C10—C965.5 (8)C22—C23—C24—O112 (2)
C11—C9—C10—C1961.7 (10)C22—C23—C24—O2164.2 (10)
C8—C9—C10—C1966.1 (9)O6—C1L—C2L—C7L171.4 (12)
C11—C9—C10—C5175.6 (6)O5—C1L—C2L—C7L8.5 (13)
C8—C9—C10—C556.7 (9)O6—C1L—C2L—C3L7.2 (16)
C11—C9—C10—C156.9 (8)O5—C1L—C2L—C3L173.0 (8)
C8—C9—C10—C1175.3 (6)C3L—C2L—C7L—C3Li3.0 (12)
C8—C9—C11—C1249.0 (9)C1L—C2L—C7L—C3Li175.6 (8)
C10—C9—C11—C12177.3 (7)C7L—C2L—C3L—C7Li3.6 (11)
C9—C11—C12—C1352.6 (10)C1L—C2L—C3L—C7Li175.0 (9)
C11—C12—C13—C1866.7 (9)O6—C1L—O5—C36.9 (17)
C11—C12—C13—C1455.5 (9)C2L—C1L—O5—C3173.0 (7)
C11—C12—C13—C17166.9 (7)C2—C3—O5—C1L132.1 (8)
C7—C8—C14—C13177.2 (7)C4—C3—O5—C1L107.3 (9)
C9—C8—C14—C1360.4 (9)O1—C24—O2—C256 (2)
C7—C8—C14—C1554.8 (10)C23—C24—O2—C25177.9 (11)
C9—C8—C14—C15177.1 (6)
Symmetry code: (i) x, y, z+1.
(70.5MeOH) bis(23-methoxycarbonyl-24-nor-5beta-cholan-3alpha-yl) piperazine 1,4-dicarboxylate top
Crystal data top
C56H90N2O8·0.5(CH3OH)Z = 1
Mr = 935.32F(000) = 513
Triclinic, P1Dx = 1.194 Mg m3
a = 7.7755 (9) ÅMelting point: 290 K
b = 9.8697 (11) ÅMo Kα radiation, λ = 0.71073 Å
c = 17.754 (2) ÅCell parameters from 1437 reflections
α = 103.040 (13)°µ = 0.08 mm1
β = 101.086 (10)°T = 130 K
γ = 90.463 (9)°Plate, colourless
V = 1300.7 (3) Å30.40 × 0.40 × 0.05 mm
Data collection top
Kuma KM4CCD κ-geometry
diffractometer
2473 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.052
Graphite monochromatorθmax = 25.1°, θmin = 3.3°
ω scansh = 79
10039 measured reflectionsk = 1111
4568 independent reflectionsl = 2117
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)] = 0.070Riding
wR(F2) = 0.159 w = 1/[σ2(Fo2) + (0.0706P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max < 0.001
4568 reflectionsΔρmax = 0.29 e Å3
619 parametersΔρmin = 0.22 e Å3
27 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
C56H90N2O8·0.5(CH3OH)γ = 90.463 (9)°
Mr = 935.32V = 1300.7 (3) Å3
Triclinic, P1Z = 1
a = 7.7755 (9) ÅMo Kα radiation
b = 9.8697 (11) ŵ = 0.08 mm1
c = 17.754 (2) ÅT = 130 K
α = 103.040 (13)°0.40 × 0.40 × 0.05 mm
β = 101.086 (10)°
Data collection top
Kuma KM4CCD κ-geometry
diffractometer
2473 reflections with I > 2σ(I)
10039 measured reflectionsRint = 0.052
4568 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.070Riding
wR(F2) = 0.159Δρmax = 0.29 e Å3
S = 0.98Δρmin = 0.22 e Å3
4568 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
619 parametersAbsolute structure parameter: 0 (10)
27 restraints
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*/UeqOcc. (<1)
C10.2850 (9)0.4455 (7)0.2515 (4)0.0350 (19)
H1A0.37520.47500.28080.042*
H1B0.30270.48750.20700.042*
C20.3051 (9)0.2868 (7)0.2216 (4)0.0376 (19)
H2A0.42010.26000.19000.045*
H2B0.29010.24280.26530.045*
C30.1669 (9)0.2415 (7)0.1727 (4)0.0379 (19)
H30.18390.28190.12760.045*
C40.0158 (9)0.2840 (7)0.2236 (4)0.0332 (18)
H4A0.03380.23740.26620.040*
H4B0.10290.25560.19240.040*
C50.0372 (9)0.4426 (7)0.2571 (4)0.0327 (19)
H50.02430.48520.21290.039*
C60.2238 (9)0.4843 (7)0.3063 (4)0.0407 (19)
H6A0.24570.58290.31440.049*
H6B0.30730.43830.27730.049*
C70.2501 (8)0.4461 (7)0.3851 (4)0.0327 (17)
H7A0.24980.34650.37660.039*
H7B0.36310.48330.41560.039*
C80.1104 (8)0.4983 (7)0.4314 (4)0.0308 (18)
H80.11990.59830.44360.037*
C90.0753 (8)0.4521 (7)0.3821 (4)0.0249 (16)
H90.07920.35210.36810.030*
C100.1074 (9)0.4989 (7)0.3037 (4)0.0322 (18)
C110.2211 (9)0.4914 (8)0.4299 (4)0.041 (2)
H11A0.23400.59000.43810.049*
H11B0.33010.44570.39940.049*
C120.1857 (8)0.4527 (8)0.5123 (4)0.040 (2)
H12A0.19310.35320.50440.047*
H12B0.27440.48960.54100.047*
C130.0047 (8)0.5088 (7)0.5615 (4)0.0254 (17)
C140.1327 (8)0.4530 (7)0.5105 (4)0.0274 (18)
H140.11450.35350.49690.033*
C150.3097 (8)0.4843 (7)0.5672 (4)0.0303 (16)
H15A0.39460.42000.55060.036*
H15B0.35370.57750.57160.036*
C160.2645 (8)0.4677 (7)0.6459 (4)0.0389 (18)
H16A0.31760.38720.66020.047*
H16B0.30820.54810.68740.047*
C170.0612 (9)0.4502 (7)0.6343 (4)0.0338 (18)
H17A0.03050.35200.61960.041*
C180.0022 (9)0.6692 (6)0.5845 (4)0.0360 (18)
H18A0.09750.70020.60910.043*
H18B0.11210.70370.62180.043*
H18C0.00340.70560.53710.043*
C190.1021 (11)0.6576 (8)0.3165 (5)0.052 (2)
H19A0.20660.69330.33580.062*
H19B0.00330.69810.35530.062*
H19C0.09960.68300.26640.062*
C200.0083 (9)0.5105 (7)0.7096 (4)0.0376 (18)
H200.01730.60930.72250.045*
C210.2071 (8)0.4876 (7)0.6999 (4)0.0396 (18)
H21A0.24150.38910.67620.048*
H21B0.23980.51400.75170.048*
H21C0.26730.54490.66560.048*
C220.0906 (10)0.4549 (8)0.7796 (4)0.048 (2)
H22A0.21400.45980.77980.057*
H22B0.05480.35860.77170.057*
C230.0608 (12)0.5351 (9)0.8616 (5)0.059 (2)
H23A0.11690.48910.90130.071*
H23B0.06260.53420.86160.071*
C240.1327 (13)0.6802 (12)0.8801 (5)0.066 (3)
O10.2530 (8)0.7241 (7)0.8575 (4)0.085 (2)
O20.0498 (9)0.7651 (7)0.9288 (4)0.0841 (19)
C250.1195 (14)0.9120 (10)0.9567 (7)0.091 (3)
H25A0.12230.95200.91110.109*
H25B0.04360.96550.98930.109*
H25C0.23860.91560.98800.109*
C310.5709 (9)0.9424 (8)0.1914 (4)0.040 (2)
H31A0.68590.96730.22350.047*
H31B0.56170.98500.14730.047*
C320.5532 (9)0.7862 (8)0.1613 (4)0.043 (2)
H32A0.64090.75690.13060.052*
H32B0.57150.74210.20500.052*
C330.3740 (9)0.7429 (8)0.1119 (4)0.039 (2)
H330.36040.78180.06630.047*
C340.2335 (9)0.7949 (8)0.1568 (4)0.039 (2)
H34A0.12060.77030.12270.047*
H34B0.23980.74920.19950.047*
C350.2500 (9)0.9512 (7)0.1895 (4)0.037 (2)
H350.23310.99330.14500.045*
C360.1063 (8)0.9999 (7)0.2355 (4)0.0392 (18)
H36A0.00470.95990.20410.047*
H36B0.10271.09930.24390.047*
C370.1307 (8)0.9609 (7)0.3146 (4)0.042 (2)
H37A0.11520.86160.30590.050*
H37B0.04261.00200.34240.050*
C380.3132 (9)1.0080 (8)0.3665 (4)0.0349 (19)
H380.32201.10790.37960.042*
C390.4588 (8)0.9547 (8)0.3193 (4)0.0332 (19)
H390.44500.85480.30580.040*
C400.4368 (9)1.0017 (7)0.2390 (4)0.0332 (19)
C410.6432 (9)0.9930 (8)0.3723 (4)0.038 (2)
H41A0.72910.94920.34410.046*
H41B0.66621.09190.38310.046*
C420.6650 (9)0.9487 (8)0.4505 (4)0.038 (2)
H42A0.77960.97940.48160.045*
H42B0.65560.84890.44030.045*
C430.5243 (9)1.0099 (7)0.4973 (4)0.0308 (18)
C440.3460 (8)0.9587 (7)0.4426 (4)0.0282 (17)
H440.34580.85890.42790.034*
C450.2139 (8)0.9937 (7)0.4971 (4)0.0393 (18)
H45A0.11120.93170.47840.047*
H45B0.17931.08770.50090.047*
C460.3147 (8)0.9750 (7)0.5780 (4)0.0344 (17)
H46A0.26500.89590.59090.041*
H46B0.30741.05610.61870.041*
C470.5120 (8)0.9521 (7)0.5709 (4)0.0319 (18)
H470.52490.85340.55700.038*
C480.5454 (9)1.1688 (6)0.5208 (4)0.0329 (18)
H48A0.52301.20580.47330.039*
H48B0.66521.19740.55000.039*
H48C0.46171.20500.55420.039*
C490.4561 (10)1.1624 (7)0.2545 (4)0.046 (2)
H49A0.57781.19410.27930.055*
H49B0.37791.20410.28950.055*
H49C0.42471.19080.20430.055*
C500.6381 (9)1.0097 (7)0.6485 (4)0.0357 (17)
H500.62501.10830.66320.043*
C510.8324 (9)0.9864 (7)0.6414 (4)0.047 (2)
H51A0.84450.88820.61740.057*
H51B0.90791.01140.69400.057*
H51C0.86741.04470.60840.057*
C520.5906 (10)0.9461 (8)0.7139 (4)0.047 (2)
H52A0.46560.94410.70970.057*
H52B0.62570.85180.70620.057*
C530.6773 (11)1.0251 (10)0.7965 (5)0.064 (3)
H53A0.64630.97880.83460.076*
H53B0.80231.02430.80140.076*
C540.6252 (14)1.1757 (13)0.8152 (5)0.073 (3)
O30.4860 (10)1.2153 (8)0.7847 (4)0.127 (3)
O40.7380 (9)1.2594 (7)0.8674 (5)0.087 (2)
C550.6974 (13)1.4017 (11)0.8861 (6)0.091 (3)
H55A0.67491.43670.83780.110*
H55B0.79651.45610.92360.110*
H55C0.59281.41040.90970.110*
O50.1743 (7)0.0883 (5)0.1475 (3)0.0473 (14)
O60.3930 (7)0.0962 (5)0.0439 (3)0.0482 (14)
C1L0.2941 (10)0.0306 (8)0.0795 (5)0.044 (2)
N2L0.2843 (9)0.1088 (6)0.0612 (3)0.0541 (19)
C3L0.4336 (17)0.1899 (12)0.0041 (7)0.030 (3)*0.50
H3LA0.51800.22240.02980.036*0.50
H3LB0.49090.13250.02920.036*0.50
C3L'0.3607 (19)0.1774 (13)0.0239 (8)0.036 (4)*0.50
H3LC0.45800.12730.04360.044*0.50
H3LD0.27260.17500.05480.044*0.50
C4L0.349 (2)0.3133 (14)0.0471 (7)0.034 (4)*0.50
H4LA0.26320.28050.07220.041*0.50
H4LB0.43910.36820.08720.041*0.50
C4L'0.419 (2)0.3272 (13)0.0325 (8)0.039 (4)*0.50
H4LC0.45400.37390.08710.047*0.50
H4LD0.51720.33000.00740.047*0.50
N5L0.2687 (8)0.3968 (6)0.0070 (3)0.0510 (18)
C6L0.1201 (18)0.3133 (13)0.0703 (7)0.032 (4)*0.50
H6LA0.03490.27840.04580.039*0.50
H6LB0.06290.37110.10330.039*0.50
C6L'0.203 (2)0.3314 (14)0.0878 (8)0.045 (4)*0.50
H6LC0.10600.38130.10840.053*0.50
H6LD0.29080.33110.11890.053*0.50
C7L0.208 (2)0.1950 (14)0.1199 (8)0.042 (4)*0.50
H7LA0.12080.13930.16110.050*0.50
H7LB0.29590.22960.14340.050*0.50
C7L'0.1423 (19)0.1879 (13)0.0947 (9)0.040 (4)*0.50
H7LC0.05090.18840.06520.048*0.50
H7LD0.09480.14340.14880.048*0.50
C8L0.2546 (11)0.5369 (8)0.0172 (4)0.0385 (19)
O70.3624 (7)0.5912 (5)0.0854 (3)0.0437 (13)
O80.1537 (6)0.6037 (5)0.0223 (3)0.0484 (14)
C1S0.765 (2)0.2524 (19)0.0309 (11)0.051 (4)0.50
H1S10.74460.15580.03410.061*0.50
H1S20.83070.29550.07130.061*0.50
H1S30.83310.25380.02140.061*0.50
O1S0.6087 (19)0.3244 (11)0.0432 (5)0.075 (4)0.50
H1S0.53000.28470.06850.089*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.027 (4)0.044 (5)0.035 (4)0.001 (4)0.000 (3)0.016 (4)
C20.030 (5)0.041 (5)0.045 (5)0.003 (4)0.003 (4)0.020 (4)
C30.052 (5)0.022 (4)0.041 (5)0.001 (4)0.010 (4)0.009 (4)
C40.034 (5)0.037 (5)0.030 (4)0.004 (4)0.007 (3)0.010 (4)
C50.040 (5)0.027 (4)0.034 (4)0.017 (4)0.000 (4)0.019 (4)
C60.034 (5)0.050 (5)0.045 (5)0.008 (4)0.018 (4)0.018 (4)
C70.022 (4)0.039 (4)0.039 (4)0.002 (3)0.009 (3)0.012 (3)
C80.020 (4)0.028 (4)0.043 (5)0.005 (3)0.002 (3)0.014 (4)
C90.032 (4)0.015 (4)0.029 (4)0.003 (3)0.009 (3)0.005 (3)
C100.026 (4)0.024 (4)0.044 (5)0.000 (3)0.009 (4)0.000 (4)
C110.025 (4)0.042 (5)0.048 (5)0.001 (4)0.002 (4)0.002 (4)
C120.016 (4)0.058 (6)0.048 (5)0.006 (4)0.014 (3)0.011 (4)
C130.022 (4)0.027 (4)0.034 (4)0.009 (3)0.012 (3)0.014 (3)
C140.023 (4)0.016 (4)0.044 (5)0.005 (3)0.012 (3)0.005 (3)
C150.022 (4)0.033 (4)0.040 (4)0.003 (3)0.005 (3)0.019 (3)
C160.030 (4)0.035 (4)0.047 (5)0.002 (3)0.001 (3)0.007 (4)
C170.039 (5)0.025 (4)0.040 (4)0.002 (3)0.014 (3)0.008 (3)
C180.043 (5)0.023 (4)0.042 (5)0.008 (3)0.006 (3)0.008 (4)
C190.063 (6)0.042 (5)0.043 (5)0.008 (4)0.011 (4)0.013 (4)
C200.044 (5)0.034 (4)0.035 (4)0.000 (4)0.006 (3)0.009 (3)
C210.037 (5)0.046 (4)0.040 (4)0.002 (4)0.013 (3)0.015 (4)
C220.059 (5)0.045 (5)0.045 (5)0.003 (4)0.017 (4)0.017 (4)
C230.066 (6)0.066 (6)0.045 (5)0.017 (5)0.002 (4)0.016 (5)
C240.058 (6)0.123 (10)0.020 (5)0.006 (6)0.024 (4)0.006 (5)
O10.074 (5)0.097 (5)0.070 (4)0.024 (4)0.031 (4)0.019 (4)
O20.094 (5)0.081 (5)0.082 (5)0.005 (4)0.035 (4)0.014 (4)
C250.084 (8)0.064 (7)0.120 (9)0.004 (6)0.037 (7)0.000 (6)
C310.028 (5)0.051 (6)0.042 (5)0.010 (4)0.012 (4)0.010 (4)
C320.039 (5)0.051 (6)0.041 (5)0.013 (4)0.015 (4)0.008 (4)
C330.030 (5)0.046 (5)0.045 (5)0.004 (4)0.005 (4)0.018 (4)
C340.029 (5)0.041 (5)0.045 (5)0.002 (4)0.002 (4)0.012 (4)
C350.041 (5)0.025 (4)0.039 (5)0.015 (4)0.000 (4)0.000 (4)
C360.025 (4)0.052 (5)0.038 (4)0.010 (3)0.005 (3)0.014 (4)
C370.013 (4)0.046 (5)0.059 (5)0.003 (3)0.011 (4)0.005 (4)
C380.034 (5)0.029 (4)0.041 (5)0.009 (4)0.002 (4)0.011 (4)
C390.014 (4)0.031 (4)0.051 (5)0.001 (3)0.012 (3)0.001 (4)
C400.027 (4)0.032 (5)0.041 (5)0.002 (3)0.001 (3)0.015 (4)
C410.030 (5)0.042 (5)0.045 (5)0.000 (4)0.013 (4)0.007 (4)
C420.027 (4)0.049 (5)0.038 (5)0.002 (4)0.003 (3)0.014 (4)
C430.028 (4)0.017 (4)0.042 (5)0.003 (3)0.007 (3)0.004 (3)
C440.031 (4)0.016 (4)0.032 (4)0.005 (3)0.001 (3)0.001 (3)
C450.023 (4)0.034 (4)0.059 (5)0.001 (3)0.013 (4)0.003 (4)
C460.044 (5)0.027 (4)0.036 (4)0.000 (3)0.017 (3)0.007 (3)
C470.029 (4)0.022 (4)0.045 (5)0.005 (3)0.012 (3)0.005 (3)
C480.029 (4)0.029 (4)0.041 (4)0.008 (3)0.001 (3)0.013 (4)
C490.058 (5)0.027 (5)0.055 (5)0.010 (4)0.005 (4)0.019 (4)
C500.030 (4)0.035 (4)0.042 (4)0.001 (3)0.003 (3)0.012 (3)
C510.042 (5)0.040 (4)0.057 (5)0.010 (4)0.003 (4)0.018 (4)
C520.044 (5)0.059 (6)0.044 (5)0.003 (4)0.002 (4)0.027 (4)
C530.057 (6)0.078 (7)0.062 (6)0.006 (5)0.017 (5)0.026 (5)
C540.068 (7)0.108 (9)0.043 (6)0.041 (7)0.015 (5)0.013 (6)
O30.108 (6)0.142 (7)0.092 (5)0.084 (5)0.017 (5)0.025 (5)
O40.077 (5)0.056 (4)0.126 (6)0.014 (4)0.013 (5)0.020 (4)
C550.068 (7)0.093 (9)0.126 (10)0.020 (6)0.016 (6)0.054 (8)
O50.064 (4)0.029 (3)0.044 (3)0.008 (3)0.002 (3)0.007 (3)
O60.060 (4)0.033 (3)0.046 (3)0.008 (3)0.012 (3)0.017 (3)
C1L0.050 (5)0.040 (6)0.038 (5)0.002 (4)0.003 (4)0.012 (4)
N2L0.080 (5)0.024 (4)0.042 (4)0.000 (3)0.021 (3)0.003 (3)
N5L0.069 (5)0.042 (4)0.037 (4)0.015 (4)0.001 (3)0.008 (3)
C8L0.057 (5)0.027 (5)0.031 (5)0.002 (4)0.016 (4)0.001 (4)
O70.062 (4)0.024 (3)0.037 (3)0.002 (3)0.002 (3)0.001 (3)
O80.054 (4)0.037 (3)0.053 (4)0.010 (3)0.009 (3)0.008 (3)
C1S0.046 (9)0.034 (8)0.065 (9)0.004 (7)0.021 (7)0.014 (7)
O1S0.151 (12)0.050 (7)0.020 (5)0.077 (8)0.004 (6)0.011 (5)
Geometric parameters (Å, º) top
C1—C101.524 (9)C37—H37A0.9599
C1—C21.532 (9)C37—H37B0.9601
C1—H1A0.9600C38—C441.515 (9)
C1—H1B0.9599C38—C391.562 (9)
C2—C31.517 (9)C38—H380.9600
C2—H2A0.9599C39—C411.548 (9)
C2—H2B0.9601C39—C401.575 (10)
C3—O51.475 (8)C39—H390.9601
C3—C41.528 (9)C40—C491.548 (9)
C3—H30.9600C41—C421.527 (10)
C4—C51.539 (9)C41—H41A0.9600
C4—H4A0.9600C41—H41B0.9600
C4—H4B0.9599C42—C431.545 (9)
C5—C61.541 (9)C42—H42A0.9600
C5—C101.555 (9)C42—H42B0.9600
C5—H50.9601C43—C481.528 (9)
C6—C71.508 (8)C43—C441.539 (9)
C6—H6A0.9600C43—C471.558 (10)
C6—H6B0.9600C44—C451.531 (9)
C7—C81.511 (9)C44—H440.9599
C7—H7A0.9600C45—C461.549 (9)
C7—H7B0.9599C45—H45A0.9600
C8—C91.543 (9)C45—H45B0.9600
C8—C141.547 (9)C46—C471.577 (9)
C8—H80.9600C46—H46A0.9601
C9—C101.540 (10)C46—H46B0.9600
C9—C111.543 (9)C47—C501.517 (9)
C9—H90.9599C47—H470.9601
C10—C191.530 (10)C48—H48A0.9800
C11—C121.570 (10)C48—H48B0.9800
C11—H11A0.9601C48—H48C0.9800
C11—H11B0.9600C49—H49A0.9800
C12—C131.532 (9)C49—H49B0.9800
C12—H12A0.9600C49—H49C0.9800
C12—H12B0.9601C50—C521.539 (9)
C13—C171.535 (9)C50—C511.555 (9)
C13—C181.541 (9)C50—H500.9600
C13—C141.555 (8)C51—H51A0.9800
C14—C151.524 (9)C51—H51B0.9800
C14—H140.9599C51—H51C0.9800
C15—C161.549 (9)C52—C531.519 (11)
C15—H15A0.9600C52—H52A0.9600
C15—H15B0.9601C52—H52B0.9600
C16—C171.558 (9)C53—C541.523 (12)
C16—H16A0.9600C53—H53A0.9601
C16—H16B0.9599C53—H53B0.9599
C17—C201.535 (9)C54—O31.223 (10)
C17—H17A0.9600C54—O41.281 (11)
C18—H18A0.9800O4—C551.422 (11)
C18—H18B0.9800C55—H55A0.9800
C18—H18C0.9800C55—H55B0.9800
C19—H19A0.9800C55—H55C0.9800
C19—H19B0.9800O5—C1L1.378 (9)
C19—H19C0.9800O6—C1L1.190 (8)
C20—C211.531 (9)C1L—N2L1.346 (9)
C20—C221.543 (9)N2L—C7L'1.467 (13)
C20—H200.9600N2L—C3L1.478 (13)
C21—H21A0.9800N2L—C3L'1.512 (12)
C21—H21B0.9800N2L—C7L1.526 (14)
C21—H21C0.9800C3L—C4L1.577 (15)
C22—C231.553 (10)C3L—H3LA0.9601
C22—H22A0.9600C3L—H3LB0.9600
C22—H22B0.9601C3L'—C4L'1.508 (16)
C23—C241.475 (12)C3L'—H3LC0.9600
C23—H23A0.9600C3L'—H3LD0.9599
C23—H23B0.9600C4L—N5L1.458 (13)
C24—O11.200 (10)C4L—H4LA0.9600
C24—O21.327 (10)C4L—H4LB0.9600
O2—C251.483 (11)C4L'—N5L1.497 (13)
C25—H25A0.9800C4L'—H4LC0.9599
C25—H25B0.9800C4L'—H4LD0.9601
C25—H25C0.9800N5L—C8L1.364 (9)
C31—C401.507 (9)N5L—C6L'1.426 (13)
C31—C321.509 (10)N5L—C6L1.531 (13)
C31—H31A0.9601C6L—C7L1.548 (16)
C31—H31B0.9600C6L—H6LA0.9599
C32—C331.499 (10)C6L—H6LB0.9600
C32—H32A0.9601C6L'—C7L'1.459 (16)
C32—H32B0.9599C6L'—H6LC0.9599
C33—O71.461 (8)C6L'—H6LD0.9599
C33—C341.500 (10)C7L—H7LA0.9600
C33—H330.9599C7L—H7LB0.9599
C34—C351.516 (10)C7L'—H7LC0.9600
C34—H34A0.9600C7L'—H7LD0.9600
C34—H34B0.9599C8L—O81.244 (8)
C35—C361.526 (9)C8L—O71.329 (9)
C35—C401.560 (10)C1S—O1S1.36 (2)
C35—H350.9601C1S—H1S10.9800
C36—C371.516 (9)C1S—H1S20.9800
C36—H36A0.9601C1S—H1S30.9800
C36—H36B0.9601O1S—H1S0.8400
C37—C381.540 (9)
C10—C1—C2114.2 (6)C36—C37—H37B109.5
C10—C1—H1A108.7C38—C37—H37B108.9
C2—C1—H1A108.6H37A—C37—H37B107.8
C10—C1—H1B108.5C44—C38—C37113.6 (6)
C2—C1—H1B109.0C44—C38—C39109.0 (5)
H1A—C1—H1B107.6C37—C38—C39109.8 (6)
C3—C2—C1108.3 (5)C44—C38—H38108.3
C3—C2—H2A110.0C37—C38—H38107.9
C1—C2—H2A109.9C39—C38—H38108.3
C3—C2—H2B110.0C41—C39—C38110.5 (6)
C1—C2—H2B110.3C41—C39—C40113.4 (6)
H2A—C2—H2B108.4C38—C39—C40112.8 (5)
O5—C3—C2109.7 (6)C41—C39—H39106.6
O5—C3—C4106.0 (5)C38—C39—H39106.5
C2—C3—C4109.6 (6)C40—C39—H39106.5
O5—C3—H3110.4C31—C40—C49107.7 (6)
C2—C3—H3110.6C31—C40—C35108.7 (6)
C4—C3—H3110.4C49—C40—C35108.9 (6)
C3—C4—C5111.1 (6)C31—C40—C39112.5 (5)
C3—C4—H4A109.3C49—C40—C39110.5 (6)
C5—C4—H4A109.6C35—C40—C39108.5 (6)
C3—C4—H4B109.4C42—C41—C39113.8 (6)
C5—C4—H4B109.4C42—C41—H41A108.6
H4A—C4—H4B108.0C39—C41—H41A108.7
C4—C5—C6110.4 (6)C42—C41—H41B108.8
C4—C5—C10112.7 (5)C39—C41—H41B109.0
C6—C5—C10112.3 (6)H41A—C41—H41B107.7
C4—C5—H5107.0C41—C42—C43111.3 (6)
C6—C5—H5107.2C41—C42—H42A109.5
C10—C5—H5106.8C43—C42—H42A109.5
C7—C6—C5112.5 (5)C41—C42—H42B109.2
C7—C6—H6A109.3C43—C42—H42B109.4
C5—C6—H6A109.2H42A—C42—H42B107.9
C7—C6—H6B108.9C48—C43—C44111.8 (6)
C5—C6—H6B109.0C48—C43—C42110.8 (6)
H6A—C6—H6B107.9C44—C43—C42105.9 (5)
C6—C7—C8113.2 (5)C48—C43—C47109.8 (6)
C6—C7—H7A108.8C44—C43—C47102.0 (5)
C8—C7—H7A108.8C42—C43—C47116.1 (6)
C6—C7—H7B109.1C38—C44—C45118.1 (5)
C8—C7—H7B109.2C38—C44—C43114.6 (6)
H7A—C7—H7B107.6C45—C44—C43103.8 (5)
C7—C8—C9111.3 (6)C38—C44—H44106.5
C7—C8—C14113.1 (5)C45—C44—H44106.4
C9—C8—C14109.7 (5)C43—C44—H44106.8
C7—C8—H8107.6C44—C45—C46104.2 (5)
C9—C8—H8107.5C44—C45—H45A111.1
C14—C8—H8107.4C46—C45—H45A111.0
C10—C9—C8112.0 (6)C44—C45—H45B111.0
C10—C9—C11113.3 (5)C46—C45—H45B110.6
C8—C9—C11112.9 (5)H45A—C45—H45B108.9
C10—C9—H9106.0C45—C46—C47107.4 (5)
C8—C9—H9105.9C45—C46—H46A110.0
C11—C9—H9106.0C47—C46—H46A110.2
C1—C10—C19106.3 (6)C45—C46—H46B110.5
C1—C10—C9112.9 (6)C47—C46—H46B110.2
C19—C10—C9112.3 (6)H46A—C46—H46B108.5
C1—C10—C5107.9 (6)C50—C47—C43119.8 (5)
C19—C10—C5108.3 (6)C50—C47—C46112.1 (5)
C9—C10—C5109.1 (5)C43—C47—C46102.0 (5)
C9—C11—C12114.3 (5)C50—C47—H47107.3
C9—C11—H11A108.7C43—C47—H47107.5
C12—C11—H11A108.4C46—C47—H47107.4
C9—C11—H11B108.9C43—C48—H48A109.5
C12—C11—H11B108.8C43—C48—H48B109.5
H11A—C11—H11B107.6H48A—C48—H48B109.5
C13—C12—C11112.2 (6)C43—C48—H48C109.5
C13—C12—H12A108.9H48A—C48—H48C109.5
C11—C12—H12A109.0H48B—C48—H48C109.5
C13—C12—H12B109.2C40—C49—H49A109.5
C11—C12—H12B109.6C40—C49—H49B109.5
H12A—C12—H12B107.9H49A—C49—H49B109.5
C12—C13—C17116.5 (6)C40—C49—H49C109.5
C12—C13—C18110.0 (5)H49A—C49—H49C109.5
C17—C13—C18110.5 (6)H49B—C49—H49C109.5
C12—C13—C14107.1 (5)C47—C50—C52110.4 (6)
C17—C13—C14100.4 (5)C47—C50—C51112.0 (5)
C18—C13—C14112.0 (5)C52—C50—C51111.0 (5)
C15—C14—C8118.2 (5)C47—C50—H50107.8
C15—C14—C13105.0 (5)C52—C50—H50107.6
C8—C14—C13114.8 (5)C51—C50—H50107.9
C15—C14—H14105.8C50—C51—H51A109.5
C8—C14—H14106.0C50—C51—H51B109.5
C13—C14—H14105.9H51A—C51—H51B109.5
C14—C15—C16102.5 (5)C50—C51—H51C109.5
C14—C15—H15A111.6H51A—C51—H51C109.5
C16—C15—H15A111.6H51B—C51—H51C109.5
C14—C15—H15B110.9C53—C52—C50113.4 (7)
C16—C15—H15B111.0C53—C52—H52A108.8
H15A—C15—H15B109.2C50—C52—H52A109.2
C15—C16—C17108.1 (5)C53—C52—H52B108.7
C15—C16—H16A109.8C50—C52—H52B108.8
C17—C16—H16A110.0H52A—C52—H52B107.8
C15—C16—H16B110.4C52—C53—C54112.5 (7)
C17—C16—H16B110.1C52—C53—H53A109.6
H16A—C16—H16B108.5C54—C53—H53A109.2
C20—C17—C13118.0 (5)C52—C53—H53B108.8
C20—C17—C16113.3 (6)C54—C53—H53B108.8
C13—C17—C16103.2 (5)H53A—C53—H53B107.8
C20—C17—H17A107.4O3—C54—O4121.6 (10)
C13—C17—H17A107.2O3—C54—C53123.7 (11)
C16—C17—H17A107.2O4—C54—C53114.7 (8)
C13—C18—H18A109.5C54—O4—C55117.0 (8)
C13—C18—H18B109.5O4—C55—H55A109.5
H18A—C18—H18B109.5O4—C55—H55B109.5
C13—C18—H18C109.5H55A—C55—H55B109.5
H18A—C18—H18C109.5O4—C55—H55C109.5
H18B—C18—H18C109.5H55A—C55—H55C109.5
C10—C19—H19A109.5H55B—C55—H55C109.5
C10—C19—H19B109.5C1L—O5—C3115.7 (6)
H19A—C19—H19B109.5O6—C1L—N2L125.9 (7)
C10—C19—H19C109.5O6—C1L—O5124.0 (7)
H19A—C19—H19C109.5N2L—C1L—O5110.1 (7)
H19B—C19—H19C109.5C1L—N2L—C7L'126.1 (7)
C21—C20—C17113.8 (6)C1L—N2L—C3L116.9 (7)
C21—C20—C22111.0 (6)C1L—N2L—C3L'114.3 (7)
C17—C20—C22110.8 (6)C7L'—N2L—C3L'111.4 (8)
C21—C20—H20107.0C1L—N2L—C7L124.6 (7)
C17—C20—H20107.0C3L—N2L—C7L108.8 (8)
C22—C20—H20106.9N2L—C3L—C4L105.1 (9)
C20—C21—H21A109.5N2L—C3L—H3LA112.0
C20—C21—H21B109.5C4L—C3L—H3LA112.3
H21A—C21—H21B109.5N2L—C3L—H3LB109.4
C20—C21—H21C109.5C4L—C3L—H3LB109.4
H21A—C21—H21C109.5H3LA—C3L—H3LB108.6
H21B—C21—H21C109.5C4L'—C3L'—N2L110.9 (10)
C20—C22—C23114.4 (6)C4L'—C3L'—H3LC110.1
C20—C22—H22A108.8N2L—C3L'—H3LC110.0
C23—C22—H22A108.4C4L'—C3L'—H3LD108.7
C20—C22—H22B108.7N2L—C3L'—H3LD109.0
C23—C22—H22B108.9H3LC—C3L'—H3LD108.2
H22A—C22—H22B107.5N5L—C4L—C3L106.0 (9)
C24—C23—C22110.7 (7)N5L—C4L—H4LA110.9
C24—C23—H23A109.6C3L—C4L—H4LA112.2
C22—C23—H23A109.4N5L—C4L—H4LB109.9
C24—C23—H23B109.6C3L—C4L—H4LB109.3
C22—C23—H23B109.3H4LA—C4L—H4LB108.5
H23A—C23—H23B108.1N5L—C4L'—C3L'108.0 (10)
O1—C24—O2120.4 (10)N5L—C4L'—H4LC110.5
O1—C24—C23127.5 (9)C3L'—C4L'—H4LC110.9
O2—C24—C23112.1 (8)N5L—C4L'—H4LD109.9
C24—O2—C25117.0 (8)C3L'—C4L'—H4LD109.1
O2—C25—H25A109.5H4LC—C4L'—H4LD108.5
O2—C25—H25B109.5C8L—N5L—C6L'118.4 (7)
H25A—C25—H25B109.5C8L—N5L—C4L122.0 (7)
O2—C25—H25C109.5C8L—N5L—C4L'120.1 (7)
H25A—C25—H25C109.5C6L'—N5L—C4L'114.6 (9)
H25B—C25—H25C109.5C8L—N5L—C6L118.0 (7)
C40—C31—C32114.5 (6)C4L—N5L—C6L111.2 (9)
C40—C31—H31A108.6C6L'—C6L—C7L'88.5 (15)
C32—C31—H31A108.5N5L—C6L—C7L105.8 (9)
C40—C31—H31B108.5N5L—C6L—H6LA109.9
C32—C31—H31B109.0C7L—C6L—H6LA112.3
H31A—C31—H31B107.6N5L—C6L—H6LB110.5
C33—C32—C31110.2 (6)C7L—C6L—H6LB109.7
C33—C32—H32A109.9H6LA—C6L—H6LB108.6
C31—C32—H32A109.5N5L—C6L'—C7L'109.8 (10)
C33—C32—H32B109.4N5L—C6L'—H6LC109.3
C31—C32—H32B109.9C7L'—C6L'—H6LC109.3
H32A—C32—H32B108.1N5L—C6L'—H6LD111.4
O7—C33—C32108.1 (6)C7L'—C6L'—H6LD108.9
O7—C33—C34111.9 (6)H6LC—C6L'—H6LD108.1
C32—C33—C34111.2 (6)N2L—C7L—C6L103.7 (10)
O7—C33—H33108.4N2L—C7L—H7LA109.6
C32—C33—H33108.7C6L—C7L—H7LA109.4
C34—C33—H33108.5N2L—C7L—H7LB112.9
C33—C34—C35112.9 (6)C6L—C7L—H7LB112.4
C33—C34—H34A109.3H6LD—C7L—H7LB42.2
C35—C34—H34A108.9H7LA—C7L—H7LB108.7
C33—C34—H34B108.7C6L'—C7L'—N2L111.1 (10)
C35—C34—H34B109.2C6L'—C7L'—H7LC108.8
H34A—C34—H34B107.8N2L—C7L'—H7LC107.4
C34—C35—C36111.4 (6)C6L'—C7L'—H7LD110.5
C34—C35—C40112.2 (6)N2L—C7L'—H7LD110.7
C36—C35—C40112.0 (6)H7LC—C7L'—H7LD108.1
C34—C35—H35106.8O8—C8L—O7125.3 (7)
C36—C35—H35107.2O8—C8L—N5L122.5 (7)
C40—C35—H35106.8O7—C8L—N5L112.3 (7)
C37—C36—C35113.9 (5)C8L—O7—C33116.8 (6)
C37—C36—H36A108.7O1S—C1S—H1S1109.5
C35—C36—H36A108.6O1S—C1S—H1S2109.5
C37—C36—H36B108.9H1S1—C1S—H1S2109.5
C35—C36—H36B108.8O1S—C1S—H1S3109.5
H36A—C36—H36B107.8H1S1—C1S—H1S3109.5
C36—C37—C38112.8 (6)H1S2—C1S—H1S3109.5
C36—C37—H37A109.0C1S—O1S—H1S109.5
C38—C37—H37A108.7
C10—C1—C2—C360.8 (8)C36—C35—C40—C4966.3 (8)
C1—C2—C3—O5176.1 (6)C34—C35—C40—C3972.1 (8)
C1—C2—C3—C460.1 (7)C36—C35—C40—C3954.0 (8)
O5—C3—C4—C5177.2 (5)C41—C39—C40—C3157.0 (8)
C2—C3—C4—C558.9 (8)C38—C39—C40—C31176.4 (6)
C3—C4—C5—C6178.4 (5)C41—C39—C40—C4963.4 (7)
C3—C4—C5—C1055.1 (8)C38—C39—C40—C4963.2 (7)
C4—C5—C6—C774.2 (7)C41—C39—C40—C35177.3 (6)
C10—C5—C6—C752.5 (8)C38—C39—C40—C3556.1 (8)
C5—C6—C7—C851.8 (8)C38—C39—C41—C4251.7 (9)
C6—C7—C8—C953.2 (8)C40—C39—C41—C42179.6 (6)
C6—C7—C8—C14177.3 (5)C39—C41—C42—C4356.0 (8)
C7—C8—C9—C1056.1 (7)C41—C42—C43—C4864.1 (8)
C14—C8—C9—C10178.0 (5)C41—C42—C43—C4457.4 (8)
C7—C8—C9—C11174.5 (5)C41—C42—C43—C47169.8 (6)
C14—C8—C9—C1148.6 (7)C37—C38—C44—C4554.6 (8)
C2—C1—C10—C19171.3 (6)C39—C38—C44—C45177.4 (6)
C2—C1—C10—C965.3 (8)C37—C38—C44—C43177.4 (5)
C2—C1—C10—C555.3 (8)C39—C38—C44—C4359.9 (7)
C8—C9—C10—C1175.9 (5)C48—C43—C44—C3858.8 (7)
C11—C9—C10—C155.0 (8)C42—C43—C44—C3862.0 (7)
C8—C9—C10—C1964.0 (7)C47—C43—C44—C38176.1 (5)
C11—C9—C10—C1965.1 (8)C48—C43—C44—C4571.4 (7)
C8—C9—C10—C556.0 (7)C42—C43—C44—C45167.8 (6)
C11—C9—C10—C5174.9 (6)C47—C43—C44—C4545.9 (6)
C4—C5—C10—C151.5 (8)C38—C44—C45—C46161.4 (6)
C6—C5—C10—C1177.0 (5)C43—C44—C45—C4633.4 (7)
C4—C5—C10—C19166.1 (6)C44—C45—C46—C478.5 (7)
C6—C5—C10—C1968.4 (7)C48—C43—C47—C5044.8 (8)
C4—C5—C10—C971.4 (7)C44—C43—C47—C50163.5 (5)
C6—C5—C10—C954.1 (7)C42—C43—C47—C5081.8 (8)
C10—C9—C11—C12176.5 (6)C48—C43—C47—C4679.7 (6)
C8—C9—C11—C1247.8 (8)C44—C43—C47—C4639.0 (6)
C9—C11—C12—C1352.0 (8)C42—C43—C47—C46153.7 (6)
C11—C12—C13—C17166.5 (6)C45—C46—C47—C50148.5 (5)
C11—C12—C13—C1866.8 (7)C45—C46—C47—C4319.0 (6)
C11—C12—C13—C1455.1 (7)C43—C47—C50—C52175.1 (6)
C7—C8—C14—C1553.0 (8)C46—C47—C50—C5255.6 (7)
C9—C8—C14—C15177.9 (5)C43—C47—C50—C5160.7 (8)
C7—C8—C14—C13178.0 (6)C46—C47—C50—C51179.8 (5)
C9—C8—C14—C1357.1 (8)C47—C50—C52—C53164.6 (6)
C12—C13—C14—C15168.2 (5)C51—C50—C52—C5370.7 (8)
C17—C13—C14—C1546.1 (6)C50—C52—C53—C5460.4 (9)
C18—C13—C14—C1571.2 (7)C52—C53—C54—O327.4 (13)
C12—C13—C14—C860.2 (7)C52—C53—C54—O4154.1 (8)
C17—C13—C14—C8177.7 (6)O3—C54—O4—C552.5 (15)
C18—C13—C14—C860.4 (7)C53—C54—O4—C55179.0 (7)
C8—C14—C15—C16163.1 (5)C2—C3—O5—C1L85.5 (7)
C13—C14—C15—C1633.4 (6)C4—C3—O5—C1L156.2 (6)
C14—C15—C16—C178.4 (7)C3—O5—C1L—O63.5 (11)
C12—C13—C17—C2080.2 (8)C3—O5—C1L—N2L177.9 (6)
C18—C13—C17—C2046.3 (8)O6—C1L—N2L—C7L'167.0 (11)
C14—C13—C17—C20164.7 (6)O5—C1L—N2L—C7L'14.4 (13)
C12—C13—C17—C16154.0 (6)O6—C1L—N2L—C3L15.1 (13)
C18—C13—C17—C1679.5 (6)O5—C1L—N2L—C3L163.5 (8)
C14—C13—C17—C1638.9 (6)O6—C1L—N2L—C3L'21.4 (13)
C15—C16—C17—C20148.4 (6)O5—C1L—N2L—C3L'160.0 (9)
C15—C16—C17—C1319.7 (7)O6—C1L—N2L—C7L157.0 (11)
C13—C17—C20—C2162.1 (8)O5—C1L—N2L—C7L21.6 (13)
C16—C17—C20—C21177.2 (6)C1L—N2L—C3L—C4L143.0 (9)
C13—C17—C20—C22172.0 (6)C7L—N2L—C3L—C4L69.4 (12)
C16—C17—C20—C2251.3 (8)C1L—N2L—C3L'—C4L'154.9 (11)
C21—C20—C22—C2366.1 (8)C7L'—N2L—C3L'—C4L'54.5 (15)
C17—C20—C22—C23166.5 (6)N2L—C3L—C4L—N5L64.0 (13)
C20—C22—C23—C2464.7 (9)N2L—C3L'—C4L'—N5L51.8 (16)
C22—C23—C24—O128.3 (13)C3L—C4L—N5L—C8L149.6 (9)
C22—C23—C24—O2153.0 (7)C3L—C4L—N5L—C6L63.7 (13)
O1—C24—O2—C253.4 (13)C3L'—C4L'—N5L—C8L153.4 (9)
C23—C24—O2—C25175.4 (8)C3L'—C4L'—N5L—C6L'56.3 (15)
C40—C31—C32—C3357.6 (8)C8L—N5L—C6L—C7L146.4 (9)
C31—C32—C33—O7179.1 (6)C4L—N5L—C6L—C7L65.3 (13)
C31—C32—C33—C3455.9 (8)C8L—N5L—C6L'—C7L'149.8 (10)
O7—C33—C34—C35176.3 (6)C4L'—N5L—C6L'—C7L'59.3 (16)
C32—C33—C34—C3555.3 (9)C1L—N2L—C7L—C6L145.3 (10)
C33—C34—C35—C36179.3 (6)C3L—N2L—C7L—C6L70.2 (12)
C33—C34—C35—C4052.8 (9)N5L—C6L—C7L—N2L63.6 (13)
C34—C35—C36—C3772.5 (8)N5L—C6L'—C7L'—N2L58.0 (17)
C40—C35—C36—C3754.1 (8)C1L—N2L—C7L'—C6L'156.9 (10)
C35—C36—C37—C3853.1 (8)C3L'—N2L—C7L'—C6L'56.7 (15)
C36—C37—C38—C44174.8 (5)C6L'—N5L—C8L—O816.8 (13)
C36—C37—C38—C3952.5 (8)C4L—N5L—C8L—O8163.3 (10)
C44—C38—C39—C4151.4 (8)C4L'—N5L—C8L—O8166.0 (10)
C37—C38—C39—C41176.3 (6)C6L—N5L—C8L—O818.6 (12)
C44—C38—C39—C40179.6 (6)C6L'—N5L—C8L—O7161.9 (10)
C37—C38—C39—C4055.5 (8)C4L—N5L—C8L—O718.1 (12)
C32—C31—C40—C49171.8 (6)C4L'—N5L—C8L—O712.6 (11)
C32—C31—C40—C3554.0 (8)C6L—N5L—C8L—O7162.7 (9)
C32—C31—C40—C3966.2 (8)O8—C8L—O7—C335.9 (11)
C34—C35—C40—C3150.5 (8)N5L—C8L—O7—C33172.6 (6)
C36—C35—C40—C31176.7 (5)C32—C33—O7—C8L151.4 (6)
C34—C35—C40—C49167.6 (6)C34—C33—O7—C8L85.8 (7)

Experimental details

(52Py120K)(52Py180K)(6)(70.5MeOH)
Crystal data
Chemical formulaC56H82O8·2(C5H5N)C56H82O8·2(C5H5N)C58H86O8C56H90N2O8·0.5(CH3OH)
Mr1041.421041.42911.27935.32
Crystal system, space groupTriclinic, P1Triclinic, P1Monoclinic, C2Triclinic, P1
Temperature (K)120180293130
a, b, c (Å)12.8559 (6), 13.5462 (7), 17.4215 (9)6.8044 (5), 12.8870 (9), 17.0661 (11)31.731 (6), 7.727 (2), 11.017 (2)7.7755 (9), 9.8697 (11), 17.754 (2)
α, β, γ (°)75.390 (4), 83.254 (4), 82.771 (4)94.431 (6), 97.935 (6), 97.341 (5)90, 106.28 (3), 90103.040 (13), 101.086 (10), 90.463 (9)
V3)2900.9 (3)1463.14 (18)2592.9 (10)1300.7 (3)
Z2121
Radiation typeMo KαMo KαCu KαMo Kα
µ (mm1)0.080.080.590.08
Crystal size (mm)0.40 × 0.40 × 0.200.40 × 0.40 × 0.200.2 × 0.1 × 0.10.40 × 0.40 × 0.05
Data collection
DiffractometerKuma KM4CCD κ-geometry
diffractometer
Kuma KM4CCD κ-geometry
diffractometer
KM-4 four circle
diffractometer
Kuma KM4CCD κ-geometry
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
22008, 10239, 6040 11263, 5162, 3150 4425, 2419, 715 10039, 4568, 2473
Rint0.0690.0370.1960.052
(sin θ/λ)max1)0.5960.5960.5920.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.078, 0.146, 1.02 0.050, 0.124, 0.93 0.046, 0.137, 0.86 0.070, 0.159, 0.98
No. of reflections10239516224194568
No. of parameters1381673299619
No. of restraints15377127
H-atom treatmentRidingRidingRidingRiding
Δρmax, Δρmin (e Å3)0.21, 0.190.20, 0.180.20, 0.140.29, 0.22
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter0 (10)0 (10)0 (10)0 (10)

Computer programs: CrysAlis CCD v.1.168 (Oxford Diffraction,2001), CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.23 beta (release 19.07.2004 CrysAlis171 .NET), Kuma KM-4 Software (Kuma Diffraction, 1995), CrysAlis CCD, Oxford Diffraction (2004a), CrysAlis RED v.1.168 (Oxford Diffraction,2001), CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.23 beta (release 19.07.2004 CrysAlis171 .NET), CrysAlis RED, Oxford Diffraction (2004b), SHELXS86 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), Simens Analytical X-Ray Instruments (1989) Mercury (Bruno at al. 2002).

 

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