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The crystal structure of the title compound, (-)-(4R,5R,4''R,5''R)-di­spiro­[4,5-di­methyl-1,3-dioxalane-2,3'-[1',5'-(naphthalene-1,8-diyl)­bi­cyclo­[3.3.0]­octane]-7',2''-(4'',5''-di­methyl-1'',3''-dioxalane)], C26H30O4, contains two independent mol­ecules in the asymmetric unit separated by normal van der Waals distances. The five-membered rings in the trans-2,3-di­methyl-1,4-dioxa­spiro­[4.4]­nonane moieties exhibit envelope conformations and the acenaphthene moieties are essentially planar. The conformations of a dioxa­cyclo­pentane ring in the two mol­ecules are different. The molecular dimensions in both mol­ecules are as expected.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801004457/cv6010sup1.cif
Contains datablocks Global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801004457/cv6010Isup2.hkl
Contains datablock I

CCDC reference: 162825

Key indicators

  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](C-C) = 0.016 Å
  • R factor = 0.063
  • wR factor = 0.239
  • Data-to-parameter ratio = 7.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
ABSMU_01 Alert C The ratio of given/expected absorption coefficient lies outside the range 0.99 <> 1.01 Calculated value of mu = 0.081 Value of mu given = 0.080 STRVAL_01 From the CIF: _refine_ls_abs_structure_Flack 0.000 From the CIF: _refine_ls_abs_structure_Flack_su 4.000 Alert C Flack test results are meaningless. General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.00 From the CIF: _reflns_number_total 3990 Count of symmetry unique reflns 4003 Completeness (_total/calc) 99.68% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present no Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

This project was designed to prepare chiral naphthalene systems with C2 symmetry for subsequent use as a chiral catalytic transfer agent [Cr(CO)3 from naphthalene to prochiral arene]. The reaction of acenaphthoquinone, (I), and 1,3-acetonedicarboxylate, (II), led to diketone (III), which upon reaction with two equivalents of (-)-(2R,3R)-butane-2,3-diol, (IV), gave the bis-ketal (V). To assess the potential regiochemistry of the two C2 acial asymmetry naphthalene rings toward Cr(CO)3 complexation, an X-ray structure of (V) was determined and is presented in this paper.

The asymmetric unit of (V) is composed of two independent molecules 1 and 2 wherein an acenaphthene moiety has been fused with two trans-2,3-dimethyl,1,4-dioxaspiro[4.4]nonane moieties (Figs. 1 and 2). The conformations of the dioxacyclopentane ring (G) in the two molecules are different from each other. The molecular dimensions in both molecules are as expected with mean bond distances: Csp3—Csp3 1.526 (17), Csp3—Csp2 1.515 (12), O—Csp3 1.434 (16) and C—Caromatic 1.393 (16) Å.

In both molecules, the acenaphthene moieties (rings A, B and C) are essentially planar with the maximum deviation of any atom from the mean-planes being 0.051 (9) and 0.054 (9) Å for molecules 1 and 2, respectively. The five-membered rings D, E, F and G in molecule 1 exhibit C14A–, C19A–, C17A– and O4A-envelope conformations, respectively, with these atoms 0.544 (17), 0.597 (17), 0.564 (16) and 0.504 (16) Å, respectively, out of the least-squares planes of the remaining ring atoms. The corresponging rings in molecule 2 adopt C14B–, C19B–, C17B– and C23B-envelope conformations, with these atoms 0.566 (17), 0.557 (16), 0.568 (15) and 0.618 (16) Å, respectively, out of the least-squares planes of the remaining ring atoms. The molecules are separated by normal van der Waals distances. In Fig. 3, a direct facial projection of a molecule 2 of (V) is shown, where the second ketal ring and H atoms have been omitted for clarity. This view illustrates that there is a small steric differentiation of the two aromatic rings.

Experimental top

The Weiss–Cook reaction (Yang-Lau et al., 1976) between acenaphthoquinone, (I), and 1,3-acetonedicarboxylate, (II), led to diketone (III), which was purified by flash chromatography (SiO2, 9:1 CH2Cl2/ethyl acetate) and recrystallized to give 62% yield, characterized by 1H and 13C NMR and CH analysis (Simion, 1996). Reaction of (III) with two equivalents of (-)-(2R,3R)-butane-2,3-diol, (IV) (toluene, reflux, PTSA cat. Dean–Stark trap), for 48 h gave the bis-ketal (V), which was purified by flash chromatography (SiO2, 1:1 benzene/ethyl acetate) and recrystallized (pentane); 80% yield, m.p. 360 K, [α]23D = -1.3° (c = 0.097, CHCl3).

Refinement top

The space group, P21, was determined from the systematic absences, packing considerations, a statistical analysis of intensity distribution, and the successful solution and refinement of the structure. Most of the H atoms were located from difference maps. All the H atoms were included at geometrically idealized positions with C—H = 0.95–1.00 Å, in a riding mode with isotropic displacement parameters 1.2 (non-methyl) and 1.5 (methyl) times the thermal displacement parameters of the atoms to which they were attached. An absolute structure was not established in this analysis, since the absolute configuration of the starting material was already known. There is a pseudocentre of symmetry located at 0.724, 0.702, -0.011 relating some of the atoms of the two molecules in the asymmetric unit.

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1994); program(s) used to solve structure: SAPI91 (Fan, 1991); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: TEXSAN; software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. ORTEPII (Johnson, 1976) drawing of molecule 1 of (V). Displacement ellipsoids have been plotted at the 50% probability level.
[Figure 2] Fig. 2. ORTEPII (Johnson, 1976) drawing of molecule 2 of (V). Displacement ellipsoids have been plotted at the 50% probability level.
[Figure 3] Fig. 3. Facial projection of molecule 2 of (V); the second ketal and H atoms have been omitted for clarity.
(-)-(4R,5R,4'''R,5'''R)-Dispiro[1,3-(4,5-dimethyl)- dioxalane-2,3'-[1',5'-(1'',8''-naphthalene)]- bicyclo[3.3.0]octane-7',2'''-[1,3]- (4''',5'''-dimethyl)-dioxalane] top
Crystal data top
C26H30O4F(000) = 872
Mr = 406.50Dx = 1.222 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71069 Å
a = 8.1172 (11) ÅCell parameters from 25 reflections
b = 22.523 (4) Åθ = 10.0–15.0°
c = 12.5352 (13) ŵ = 0.08 mm1
β = 105.362 (12)°T = 200 K
V = 2209.9 (5) Å3Prism, colourless
Z = 40.50 × 0.40 × 0.32 mm
Data collection top
Rigaku AFC-6S
diffractometer
Rint = 0.05
Radiation source: fine-focus sealed tubeθmax = 25.0°, θmin = 2.5°
Graphite monochromatorh = 09
ω/2θ scansk = 026
4276 measured reflectionsl = 1414
3990 independent reflections3 standard reflections every 200 reflections
2388 reflections with I > 2σ(I) intensity decay: <0.1%
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)] = 0.063H-atom parameters constrained
wR(F2) = 0.239 w = 1/[σ2(Fo2) + (0.0563P)2 + 10.0719P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
3990 reflectionsΔρmax = 0.47 e Å3
549 parametersΔρmin = 0.52 e Å3
1 restraintAbsolute structure: (Flack, 1983)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0 (4)
Crystal data top
C26H30O4V = 2209.9 (5) Å3
Mr = 406.50Z = 4
Monoclinic, P21Mo Kα radiation
a = 8.1172 (11) ŵ = 0.08 mm1
b = 22.523 (4) ÅT = 200 K
c = 12.5352 (13) Å0.50 × 0.40 × 0.32 mm
β = 105.362 (12)°
Data collection top
Rigaku AFC-6S
diffractometer
Rint = 0.05
4276 measured reflections3 standard reflections every 200 reflections
3990 independent reflections intensity decay: <0.1%
2388 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.063H-atom parameters constrained
wR(F2) = 0.239 w = 1/[σ2(Fo2) + (0.0563P)2 + 10.0719P]
where P = (Fo2 + 2Fc2)/3
S = 1.07Δρmax = 0.47 e Å3
3990 reflectionsΔρmin = 0.52 e Å3
549 parametersAbsolute structure: (Flack, 1983)
1 restraintAbsolute structure parameter: 0 (4)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O1A0.6601 (9)0.6057 (4)0.5693 (6)0.043 (2)
O2A0.7519 (9)0.5093 (4)0.5993 (6)0.042 (2)
O3A0.3773 (9)0.6959 (4)0.8571 (6)0.041 (2)
O4A0.4220 (9)0.7458 (4)0.7120 (6)0.042 (2)
C1A0.4957 (11)0.5518 (5)0.9261 (8)0.027 (2)
C2A0.3754 (12)0.5512 (5)0.8210 (8)0.029 (2)
C3A0.2213 (13)0.5253 (6)0.8104 (9)0.036 (3)
H3A0.13720.52580.74130.043*
C4A0.1872 (14)0.4974 (6)0.9041 (9)0.041 (3)
H4A0.08080.47800.89640.049*
C5A0.3059 (14)0.4981 (6)1.0061 (9)0.044 (3)
H5A0.27790.48031.06780.052*
C6A0.4647 (13)0.5241 (5)1.0201 (8)0.035 (3)
C7A0.6014 (15)0.5303 (6)1.1187 (9)0.041 (3)
H7A0.58910.51331.18550.049*
C8A0.7445 (14)0.5591 (6)1.1199 (8)0.040 (3)
H8A0.83270.56101.18700.048*
C9A0.7703 (12)0.5873 (6)1.0235 (9)0.039 (3)
H9A0.87360.60801.02670.046*
C10A0.6446 (11)0.5842 (5)0.9270 (8)0.029 (2)
C11A0.6374 (11)0.6049 (5)0.8119 (8)0.027 (2)
C12A0.4540 (11)0.5823 (5)0.7382 (8)0.029 (2)
C13A0.4914 (12)0.5408 (5)0.6517 (8)0.035 (3)
H13A0.40640.54640.57950.042*
H13B0.48780.49890.67480.042*
C14A0.6696 (13)0.5570 (5)0.6433 (8)0.033 (2)
C15A0.7672 (12)0.5728 (5)0.7614 (8)0.034 (3)
H15A0.86500.59910.76160.041*
H15B0.81090.53650.80410.041*
C16A0.6343 (12)0.6735 (5)0.7988 (9)0.032 (2)
H16A0.69150.69290.86980.038*
H16B0.69250.68570.74220.038*
C17A0.4451 (12)0.6901 (6)0.7628 (8)0.033 (3)
C18A0.3608 (12)0.6399 (6)0.6863 (8)0.037 (3)
H18A0.37410.64610.61090.045*
H18B0.23740.63770.68210.045*
C19A0.7947 (13)0.5967 (6)0.5146 (9)0.040 (3)
H19A0.90710.60710.56680.048*
C20A0.7845 (14)0.5308 (6)0.4984 (9)0.043 (3)
H20A0.68230.52180.43590.052*
C21A0.7666 (15)0.6345 (6)0.4135 (9)0.041 (3)
H21A0.73810.67500.43090.062*
H21B0.67240.61810.35510.062*
H21C0.87090.63510.38810.062*
C22A0.9378 (16)0.4994 (7)0.4765 (11)0.059 (4)
H22A0.93080.45680.49070.088*
H22B1.04300.51560.52550.088*
H22C0.93860.50550.39930.088*
C23A0.2543 (12)0.7421 (6)0.8358 (9)0.042 (3)
H23A0.29240.77370.89320.050*
C24A0.2593 (13)0.7674 (6)0.7240 (10)0.046 (3)
H24A0.16460.74960.66480.055*
C25A0.0789 (13)0.7206 (7)0.8399 (12)0.065 (4)
H25A0.08730.70130.91130.098*
H25B0.03550.69200.78000.098*
H25C0.00060.75440.83120.098*
C26A0.2541 (17)0.8336 (8)0.7124 (13)0.075 (5)
H26A0.25660.84440.63710.113*
H26B0.35330.85100.76550.113*
H26C0.14900.84880.72690.113*
O1B0.7745 (9)0.7946 (4)1.4027 (6)0.042 (2)
O2B0.6671 (10)0.8896 (4)1.3713 (6)0.047 (2)
O3B1.1294 (9)0.7188 (4)1.1486 (6)0.0375 (18)
O4B1.0682 (9)0.6634 (4)1.2840 (6)0.0382 (19)
C1B0.9855 (12)0.8542 (5)1.0664 (8)0.031 (2)
C2B0.8361 (12)0.8237 (5)1.0578 (8)0.030 (2)
C3B0.7173 (12)0.8183 (6)0.9557 (8)0.038 (3)
H3B0.61320.79730.94790.045*
C4B0.7562 (15)0.8448 (6)0.8657 (9)0.044 (3)
H4B0.67640.84120.79530.053*
C5B0.9031 (15)0.8758 (6)0.8729 (9)0.044 (3)
H5B0.92250.89380.80870.052*
C6B1.0305 (13)0.8813 (5)0.9792 (8)0.033 (3)
C7B1.1854 (15)0.9122 (7)1.0013 (10)0.051 (3)
H7B1.21950.93170.94340.061*
C8B1.2871 (14)0.9139 (6)1.1075 (11)0.050 (3)
H8B1.39410.93371.12110.060*
C9B1.2418 (13)0.8883 (6)1.1967 (10)0.041 (3)
H9B1.31360.89241.26960.049*
C10B1.0916 (12)0.8569 (5)1.1776 (8)0.032 (2)
C11B1.0018 (12)0.8261 (5)1.2527 (8)0.030 (2)
C12B0.8307 (12)0.7992 (5)1.1705 (8)0.029 (2)
C13B0.6837 (13)0.8255 (6)1.2124 (8)0.037 (3)
H13C0.63220.86001.16690.045*
H13D0.59380.79531.20930.045*
C14B0.7645 (13)0.8443 (5)1.3311 (8)0.037 (3)
C15B0.9406 (13)0.8680 (6)1.3312 (8)0.040 (3)
H15C1.01920.86671.40650.048*
H15D0.93300.90941.30380.048*
C16B1.0984 (13)0.7706 (6)1.3120 (8)0.039 (3)
H16C1.22360.77601.32740.046*
H16D1.06910.76291.38250.046*
C17B1.0382 (12)0.7203 (6)1.2313 (8)0.035 (3)
C18B0.8486 (12)0.7322 (5)1.1816 (9)0.034 (3)
H18C0.80840.71291.10830.041*
H18D0.78080.71671.23060.041*
C19B0.7526 (14)0.8178 (6)1.5039 (8)0.040 (3)
H19B0.86190.83611.54760.047*
C20B0.6218 (14)0.8648 (6)1.4661 (8)0.044 (3)
H20B0.50560.84651.44220.053*
C21B0.703 (2)0.7680 (7)1.5691 (11)0.068 (4)
H21D0.79450.73841.58710.102*
H21E0.59760.74931.52500.102*
H21F0.68330.78381.63760.102*
C22B0.6209 (19)0.9145 (7)1.5449 (11)0.066 (4)
H22D0.53670.94431.50880.099*
H22E0.73450.93261.56730.099*
H22F0.59080.89901.61040.099*
C23B1.2745 (13)0.6818 (6)1.1931 (9)0.042 (3)
H23B1.35690.70341.25430.050*
C24B1.1907 (13)0.6323 (6)1.2415 (9)0.044 (3)
H24B1.12860.60561.18020.052*
C25B1.3598 (16)0.6670 (7)1.1047 (10)0.057 (4)
H25D1.39230.70371.07360.085*
H25E1.28100.64431.04610.085*
H25F1.46230.64321.13630.085*
C26B1.3017 (16)0.5952 (7)1.3310 (11)0.063 (4)
H26D1.23020.57241.36800.094*
H26E1.37860.62111.38490.094*
H26F1.36930.56801.29870.094*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O1A0.040 (4)0.064 (6)0.035 (4)0.011 (4)0.026 (3)0.009 (4)
O2A0.052 (4)0.046 (5)0.040 (4)0.018 (4)0.031 (4)0.012 (4)
O3A0.032 (4)0.059 (6)0.038 (4)0.005 (4)0.019 (3)0.005 (4)
O4A0.033 (4)0.042 (5)0.055 (5)0.016 (4)0.019 (4)0.014 (4)
C1A0.024 (5)0.033 (6)0.026 (5)0.001 (4)0.008 (4)0.001 (5)
C2A0.028 (5)0.036 (7)0.025 (5)0.003 (5)0.010 (4)0.001 (5)
C3A0.030 (5)0.046 (8)0.032 (5)0.011 (5)0.007 (4)0.004 (5)
C4A0.036 (6)0.044 (8)0.048 (7)0.012 (5)0.023 (5)0.000 (6)
C5A0.053 (7)0.049 (9)0.039 (6)0.011 (6)0.029 (6)0.006 (6)
C6A0.041 (6)0.036 (7)0.035 (6)0.002 (5)0.020 (5)0.001 (5)
C7A0.056 (7)0.043 (8)0.029 (6)0.010 (6)0.021 (5)0.006 (5)
C8A0.044 (6)0.054 (8)0.021 (5)0.010 (6)0.005 (5)0.001 (5)
C9A0.029 (5)0.049 (8)0.035 (6)0.004 (5)0.005 (4)0.001 (5)
C10A0.025 (5)0.038 (7)0.026 (5)0.007 (5)0.009 (4)0.004 (5)
C11A0.023 (4)0.035 (7)0.024 (5)0.003 (4)0.011 (4)0.004 (4)
C12A0.023 (4)0.038 (7)0.025 (5)0.005 (5)0.005 (4)0.002 (5)
C13A0.036 (5)0.045 (7)0.027 (5)0.005 (5)0.015 (4)0.002 (5)
C14A0.042 (6)0.033 (6)0.029 (5)0.004 (5)0.018 (5)0.009 (5)
C15A0.026 (5)0.048 (7)0.031 (5)0.009 (5)0.013 (4)0.004 (5)
C16A0.024 (5)0.038 (7)0.032 (5)0.004 (5)0.007 (4)0.004 (5)
C17A0.021 (5)0.051 (8)0.031 (5)0.009 (5)0.011 (4)0.004 (5)
C18A0.026 (5)0.056 (8)0.028 (5)0.003 (5)0.005 (4)0.005 (5)
C19A0.037 (5)0.053 (8)0.034 (6)0.010 (5)0.019 (5)0.002 (5)
C20A0.049 (6)0.056 (8)0.032 (6)0.017 (6)0.023 (5)0.012 (6)
C21A0.059 (7)0.033 (7)0.039 (6)0.002 (6)0.027 (5)0.004 (5)
C22A0.066 (8)0.071 (11)0.053 (8)0.022 (7)0.039 (7)0.001 (7)
C23A0.025 (5)0.055 (8)0.047 (6)0.001 (5)0.012 (5)0.002 (6)
C24A0.029 (5)0.055 (8)0.056 (7)0.019 (5)0.015 (5)0.018 (6)
C25A0.028 (6)0.093 (12)0.080 (9)0.017 (7)0.024 (6)0.033 (9)
C26A0.051 (8)0.089 (13)0.093 (11)0.027 (8)0.032 (8)0.029 (10)
O1B0.055 (5)0.044 (5)0.036 (4)0.017 (4)0.028 (4)0.013 (4)
O2B0.062 (5)0.055 (6)0.037 (4)0.028 (4)0.035 (4)0.010 (4)
O3B0.037 (4)0.045 (5)0.037 (4)0.006 (4)0.021 (3)0.005 (4)
O4B0.046 (4)0.032 (5)0.044 (4)0.004 (4)0.024 (3)0.004 (4)
C1B0.031 (5)0.037 (7)0.027 (5)0.009 (5)0.011 (4)0.005 (5)
C2B0.030 (5)0.032 (6)0.028 (5)0.003 (5)0.010 (4)0.005 (5)
C3B0.027 (5)0.054 (8)0.031 (5)0.004 (5)0.006 (4)0.011 (5)
C4B0.050 (7)0.051 (8)0.028 (6)0.014 (6)0.003 (5)0.005 (5)
C5B0.056 (7)0.052 (9)0.032 (6)0.014 (6)0.027 (5)0.000 (6)
C6B0.041 (6)0.029 (7)0.035 (6)0.009 (5)0.018 (5)0.005 (5)
C7B0.047 (7)0.064 (10)0.054 (8)0.007 (7)0.035 (6)0.004 (7)
C8B0.032 (6)0.045 (8)0.079 (9)0.003 (5)0.025 (6)0.009 (7)
C9B0.028 (5)0.044 (8)0.048 (7)0.008 (5)0.006 (5)0.006 (6)
C10B0.027 (5)0.041 (7)0.027 (5)0.010 (5)0.008 (4)0.004 (5)
C11B0.031 (5)0.034 (7)0.026 (5)0.011 (5)0.009 (4)0.002 (5)
C12B0.025 (5)0.033 (6)0.030 (5)0.006 (4)0.011 (4)0.000 (5)
C13B0.040 (6)0.045 (7)0.031 (5)0.017 (5)0.017 (5)0.009 (5)
C14B0.044 (6)0.038 (7)0.034 (6)0.007 (5)0.019 (5)0.004 (5)
C15B0.042 (6)0.052 (8)0.029 (5)0.009 (6)0.014 (5)0.000 (5)
C16B0.033 (5)0.058 (8)0.026 (5)0.007 (5)0.009 (4)0.005 (5)
C17B0.029 (5)0.053 (8)0.031 (5)0.012 (5)0.019 (4)0.020 (6)
C18B0.034 (5)0.038 (7)0.035 (5)0.000 (5)0.016 (4)0.006 (5)
C19B0.052 (7)0.042 (7)0.032 (6)0.008 (6)0.024 (5)0.005 (5)
C20B0.047 (6)0.061 (8)0.033 (6)0.008 (6)0.028 (5)0.007 (6)
C21B0.115 (12)0.053 (10)0.056 (8)0.011 (9)0.057 (8)0.009 (7)
C22B0.099 (11)0.064 (10)0.049 (7)0.029 (9)0.042 (8)0.021 (7)
C23B0.031 (5)0.064 (9)0.031 (5)0.009 (5)0.011 (5)0.001 (5)
C24B0.032 (5)0.056 (8)0.042 (6)0.018 (6)0.009 (5)0.007 (6)
C25B0.053 (7)0.072 (10)0.054 (8)0.013 (7)0.029 (6)0.005 (7)
C26B0.049 (7)0.076 (11)0.066 (8)0.022 (7)0.020 (6)0.024 (8)
Geometric parameters (Å, º) top
O1A—C14A1.424 (14)O1B—C14B1.423 (14)
O1A—C19A1.450 (11)O1B—C19B1.426 (12)
O2A—C20A1.442 (12)O2B—C20B1.446 (12)
O2A—C14A1.450 (13)O2B—C14B1.460 (13)
O3A—C23A1.417 (14)O3B—C17B1.425 (11)
O3A—C17A1.437 (12)O3B—C23B1.431 (13)
O4A—C17A1.396 (14)O4B—C24B1.429 (13)
O4A—C24A1.452 (12)O4B—C17B1.433 (14)
C1A—C10A1.409 (14)C1B—C2B1.372 (14)
C1A—C6A1.414 (14)C1B—C6B1.384 (14)
C1A—C2A1.417 (13)C1B—C10B1.433 (14)
C2A—C3A1.354 (14)C2B—C3B1.389 (14)
C2A—C12A1.526 (14)C2B—C12B1.528 (14)
C3A—C4A1.422 (16)C3B—C4B1.384 (17)
C3A—H3A0.9500C3B—H3B0.9500
C4A—C5A1.382 (16)C4B—C5B1.365 (17)
C4A—H4A0.9500C4B—H4B0.9500
C5A—C6A1.384 (15)C5B—C6B1.459 (15)
C5A—H5A0.9500C5B—H5B0.9500
C6A—C7A1.432 (15)C6B—C7B1.400 (16)
C7A—C8A1.327 (17)C7B—C8B1.369 (17)
C7A—H7A0.9500C7B—H7B0.9500
C8A—C9A1.429 (16)C8B—C9B1.391 (17)
C8A—H8A0.9500C8B—H8B0.9500
C9A—C10A1.362 (13)C9B—C10B1.374 (15)
C9A—H9A0.9500C9B—H9B0.9500
C10A—C11A1.503 (13)C10B—C11B1.503 (14)
C11A—C15A1.545 (13)C11B—C15B1.537 (15)
C11A—C16A1.554 (16)C11B—C16B1.557 (16)
C11A—C12A1.613 (12)C11B—C12B1.612 (13)
C12A—C13A1.521 (14)C12B—C18B1.518 (16)
C12A—C18A1.556 (16)C12B—C13B1.543 (13)
C13A—C14A1.523 (13)C13B—C14B1.518 (14)
C13A—H13A0.9900C13B—H13C0.9900
C13A—H13B0.9900C13B—H13D0.9900
C14A—C15A1.524 (13)C14B—C15B1.526 (15)
C15A—H15A0.9900C15B—H15C0.9900
C15A—H15B0.9900C15B—H15D0.9900
C16A—C17A1.527 (13)C16B—C17B1.510 (17)
C16A—H16A0.9900C16B—H16C0.9900
C16A—H16B0.9900C16B—H16D0.9900
C17A—C18A1.522 (17)C17B—C18B1.524 (13)
C18A—H18A0.9900C18B—H18C0.9900
C18A—H18B0.9900C18B—H18D0.9900
C19A—C21A1.493 (15)C19B—C20B1.486 (15)
C19A—C20A1.497 (18)C19B—C21B1.506 (18)
C19A—H19A1.0000C19B—H19B1.0000
C20A—C22A1.519 (15)C20B—C22B1.493 (18)
C20A—H20A1.0000C20B—H20B1.0000
C21A—H21A0.9800C21B—H21D0.9800
C21A—H21B0.9800C21B—H21E0.9800
C21A—H21C0.9800C21B—H21F0.9800
C22A—H22A0.9800C22B—H22D0.9800
C22A—H22B0.9800C22B—H22E0.9800
C22A—H22C0.9800C22B—H22F0.9800
C23A—C25A1.518 (15)C23B—C25B1.492 (15)
C23A—C24A1.524 (16)C23B—C24B1.514 (18)
C23A—H23A1.0000C23B—H23B1.0000
C24A—C26A1.50 (2)C24B—C26B1.493 (16)
C24A—H24A1.0000C24B—H24B1.0000
C25A—H25A0.9800C25B—H25D0.9800
C25A—H25B0.9800C25B—H25E0.9800
C25A—H25C0.9800C25B—H25F0.9800
C26A—H26A0.9800C26B—H26D0.9800
C26A—H26B0.9800C26B—H26E0.9800
C26A—H26C0.9800C26B—H26F0.9800
C14A—O1A—C19A106.4 (8)C14B—O1B—C19B105.9 (8)
C20A—O2A—C14A107.1 (8)C20B—O2B—C14B107.1 (8)
C23A—O3A—C17A108.4 (8)C17B—O3B—C23B105.2 (7)
C17A—O4A—C24A105.7 (8)C24B—O4B—C17B108.5 (8)
C10A—C1A—C6A124.3 (9)C2B—C1B—C6B124.9 (9)
C10A—C1A—C2A113.0 (9)C2B—C1B—C10B112.9 (9)
C6A—C1A—C2A122.7 (9)C6B—C1B—C10B122.2 (10)
C3A—C2A—C1A119.1 (9)C1B—C2B—C3B119.9 (10)
C3A—C2A—C12A132.3 (9)C1B—C2B—C12B110.4 (8)
C1A—C2A—C12A108.6 (8)C3B—C2B—C12B129.6 (10)
C2A—C3A—C4A119.1 (10)C4B—C3B—C2B117.5 (10)
C2A—C3A—H3A120.5C4B—C3B—H3B121.3
C4A—C3A—H3A120.5C2B—C3B—H3B121.3
C5A—C4A—C3A121.2 (10)C5B—C4B—C3B123.4 (10)
C5A—C4A—H4A119.4C5B—C4B—H4B118.3
C3A—C4A—H4A119.4C3B—C4B—H4B118.3
C4A—C5A—C6A121.3 (10)C4B—C5B—C6B119.9 (11)
C4A—C5A—H5A119.3C4B—C5B—H5B120.0
C6A—C5A—H5A119.3C6B—C5B—H5B120.0
C5A—C6A—C1A116.5 (10)C1B—C6B—C7B118.3 (10)
C5A—C6A—C7A129.3 (10)C1B—C6B—C5B114.4 (10)
C1A—C6A—C7A114.1 (9)C7B—C6B—C5B127.2 (11)
C8A—C7A—C6A122.2 (11)C8B—C7B—C6B119.1 (12)
C8A—C7A—H7A118.9C8B—C7B—H7B120.5
C6A—C7A—H7A118.9C6B—C7B—H7B120.5
C7A—C8A—C9A122.2 (10)C7B—C8B—C9B123.4 (11)
C7A—C8A—H8A118.9C7B—C8B—H8B118.3
C9A—C8A—H8A118.9C9B—C8B—H8B118.3
C10A—C9A—C8A118.9 (10)C10B—C9B—C8B119.0 (10)
C10A—C9A—H9A120.5C10B—C9B—H9B120.5
C8A—C9A—H9A120.5C8B—C9B—H9B120.5
C9A—C10A—C1A118.3 (10)C9B—C10B—C1B117.9 (10)
C9A—C10A—C11A131.7 (9)C9B—C10B—C11B133.1 (9)
C1A—C10A—C11A109.7 (8)C1B—C10B—C11B108.8 (9)
C10A—C11A—C15A113.0 (8)C10B—C11B—C15B114.2 (10)
C10A—C11A—C16A113.9 (9)C10B—C11B—C16B113.7 (8)
C15A—C11A—C16A114.6 (9)C15B—C11B—C16B113.2 (8)
C10A—C11A—C12A104.3 (8)C10B—C11B—C12B104.6 (8)
C15A—C11A—C12A104.1 (8)C15B—C11B—C12B105.7 (8)
C16A—C11A—C12A105.4 (8)C16B—C11B—C12B104.0 (9)
C13A—C12A—C2A113.7 (9)C18B—C12B—C2B114.7 (9)
C13A—C12A—C18A112.5 (8)C18B—C12B—C13B114.4 (9)
C2A—C12A—C18A115.0 (8)C2B—C12B—C13B113.0 (8)
C13A—C12A—C11A105.9 (7)C18B—C12B—C11B105.7 (8)
C2A—C12A—C11A104.1 (7)C2B—C12B—C11B102.9 (8)
C18A—C12A—C11A104.4 (9)C13B—C12B—C11B104.5 (8)
C12A—C13A—C14A105.9 (8)C14B—C13B—C12B105.6 (8)
C12A—C13A—H13A110.6C14B—C13B—H13C110.6
C14A—C13A—H13A110.6C12B—C13B—H13C110.6
C12A—C13A—H13B110.6C14B—C13B—H13D110.6
C14A—C13A—H13B110.6C12B—C13B—H13D110.6
H13A—C13A—H13B108.7H13C—C13B—H13D108.8
O1A—C14A—O2A105.9 (7)O1B—C14B—O2B106.1 (7)
O1A—C14A—C13A109.9 (9)O1B—C14B—C13B109.7 (10)
O2A—C14A—C13A113.0 (9)O2B—C14B—C13B113.6 (8)
O1A—C14A—C15A112.2 (9)O1B—C14B—C15B112.2 (9)
O2A—C14A—C15A111.7 (8)O2B—C14B—C15B110.4 (10)
C13A—C14A—C15A104.3 (8)C13B—C14B—C15B105.1 (8)
C14A—C15A—C11A105.8 (8)C14B—C15B—C11B104.3 (9)
C14A—C15A—H15A110.6C14B—C15B—H15C110.9
C11A—C15A—H15A110.6C11B—C15B—H15C110.9
C14A—C15A—H15B110.6C14B—C15B—H15D110.9
C11A—C15A—H15B110.6C11B—C15B—H15D110.9
H15A—C15A—H15B108.7H15C—C15B—H15D108.9
C17A—C16A—C11A105.2 (9)C17B—C16B—C11B104.5 (8)
C17A—C16A—H16A110.7C17B—C16B—H16C110.9
C11A—C16A—H16A110.7C11B—C16B—H16C110.9
C17A—C16A—H16B110.7C17B—C16B—H16D110.9
C11A—C16A—H16B110.7C11B—C16B—H16D110.9
H16A—C16A—H16B108.8H16C—C16B—H16D108.9
O4A—C17A—O3A105.0 (9)O3B—C17B—O4B104.9 (9)
O4A—C17A—C18A113.3 (8)O3B—C17B—C16B111.5 (9)
O3A—C17A—C18A112.3 (9)O4B—C17B—C16B112.1 (8)
O4A—C17A—C16A110.9 (9)O3B—C17B—C18B111.7 (8)
O3A—C17A—C16A110.7 (8)O4B—C17B—C18B112.0 (9)
C18A—C17A—C16A104.7 (9)C16B—C17B—C18B104.8 (9)
C17A—C18A—C12A105.6 (8)C12B—C18B—C17B105.9 (9)
C17A—C18A—H18A110.6C12B—C18B—H18C110.6
C12A—C18A—H18A110.6C17B—C18B—H18C110.6
C17A—C18A—H18B110.6C12B—C18B—H18D110.6
C12A—C18A—H18B110.6C17B—C18B—H18D110.6
H18A—C18A—H18B108.8H18C—C18B—H18D108.7
O1A—C19A—C21A110.9 (9)O1B—C19B—C20B103.0 (8)
O1A—C19A—C20A100.4 (9)O1B—C19B—C21B109.0 (11)
C21A—C19A—C20A117.3 (10)C20B—C19B—C21B115.6 (10)
O1A—C19A—H19A109.2O1B—C19B—H19B109.7
C21A—C19A—H19A109.2C20B—C19B—H19B109.7
C20A—C19A—H19A109.2C21B—C19B—H19B109.7
O2A—C20A—C19A103.3 (9)O2B—C20B—C19B102.8 (8)
O2A—C20A—C22A110.6 (9)O2B—C20B—C22B107.6 (11)
C19A—C20A—C22A117.9 (11)C19B—C20B—C22B116.8 (10)
O2A—C20A—H20A108.2O2B—C20B—H20B109.8
C19A—C20A—H20A108.2C19B—C20B—H20B109.8
C22A—C20A—H20A108.2C22B—C20B—H20B109.8
C19A—C21A—H21A109.5C19B—C21B—H21D109.5
C19A—C21A—H21B109.5C19B—C21B—H21E109.5
H21A—C21A—H21B109.5H21D—C21B—H21E109.5
C19A—C21A—H21C109.5C19B—C21B—H21F109.5
H21A—C21A—H21C109.5H21D—C21B—H21F109.5
H21B—C21A—H21C109.5H21E—C21B—H21F109.5
C20A—C22A—H22A109.5C20B—C22B—H22D109.5
C20A—C22A—H22B109.5C20B—C22B—H22E109.5
H22A—C22A—H22B109.5H22D—C22B—H22E109.5
C20A—C22A—H22C109.5C20B—C22B—H22F109.5
H22A—C22A—H22C109.5H22D—C22B—H22F109.5
H22B—C22A—H22C109.5H22E—C22B—H22F109.5
O3A—C23A—C25A112.3 (11)O3B—C23B—C25B109.7 (9)
O3A—C23A—C24A105.0 (8)O3B—C23B—C24B100.1 (8)
C25A—C23A—C24A113.9 (9)C25B—C23B—C24B118.7 (12)
O3A—C23A—H23A108.5O3B—C23B—H23B109.3
C25A—C23A—H23A108.5C25B—C23B—H23B109.3
C24A—C23A—H23A108.5C24B—C23B—H23B109.3
O4A—C24A—C26A109.1 (10)O4B—C24B—C26B109.6 (10)
O4A—C24A—C23A102.5 (8)O4B—C24B—C23B102.7 (10)
C26A—C24A—C23A117.0 (12)C26B—C24B—C23B117.8 (10)
O4A—C24A—H24A109.3O4B—C24B—H24B108.8
C26A—C24A—H24A109.3C26B—C24B—H24B108.8
C23A—C24A—H24A109.3C23B—C24B—H24B108.8
C23A—C25A—H25A109.5C23B—C25B—H25D109.5
C23A—C25A—H25B109.5C23B—C25B—H25E109.5
H25A—C25A—H25B109.5H25D—C25B—H25E109.5
C23A—C25A—H25C109.5C23B—C25B—H25F109.5
H25A—C25A—H25C109.5H25D—C25B—H25F109.5
H25B—C25A—H25C109.5H25E—C25B—H25F109.5
C24A—C26A—H26A109.5C24B—C26B—H26D109.5
C24A—C26A—H26B109.5C24B—C26B—H26E109.5
H26A—C26A—H26B109.5H26D—C26B—H26E109.5
C24A—C26A—H26C109.5C24B—C26B—H26F109.5
H26A—C26A—H26C109.5H26D—C26B—H26F109.5
H26B—C26A—H26C109.5H26E—C26B—H26F109.5
C10A—C1A—C2A—C3A175.3 (10)C6B—C1B—C2B—C3B0.1 (18)
C6A—C1A—C2A—C3A2.9 (17)C10B—C1B—C2B—C3B178.4 (10)
C10A—C1A—C2A—C12A4.8 (13)C6B—C1B—C2B—C12B179.4 (10)
C6A—C1A—C2A—C12A177.1 (10)C10B—C1B—C2B—C12B2.3 (13)
C1A—C2A—C3A—C4A2.4 (17)C1B—C2B—C3B—C4B0.2 (17)
C12A—C2A—C3A—C4A177.5 (12)C12B—C2B—C3B—C4B179.3 (11)
C2A—C3A—C4A—C5A2.2 (19)C2B—C3B—C4B—C5B0.6 (19)
C3A—C4A—C5A—C6A2 (2)C3B—C4B—C5B—C6B1.3 (19)
C4A—C5A—C6A—C1A2.5 (19)C2B—C1B—C6B—C7B178.3 (12)
C4A—C5A—C6A—C7A178.4 (13)C10B—C1B—C6B—C7B0.1 (17)
C10A—C1A—C6A—C5A175.1 (11)C2B—C1B—C6B—C5B0.6 (17)
C2A—C1A—C6A—C5A2.8 (17)C10B—C1B—C6B—C5B177.5 (10)
C10A—C1A—C6A—C7A1.4 (17)C4B—C5B—C6B—C1B1.3 (17)
C2A—C1A—C6A—C7A179.3 (11)C4B—C5B—C6B—C7B178.7 (12)
C5A—C6A—C7A—C8A176.8 (13)C1B—C6B—C7B—C8B0.7 (19)
C1A—C6A—C7A—C8A0.8 (18)C5B—C6B—C7B—C8B178.0 (12)
C6A—C7A—C8A—C9A2 (2)C6B—C7B—C8B—C9B3 (2)
C7A—C8A—C9A—C10A0.6 (19)C7B—C8B—C9B—C10B3 (2)
C8A—C9A—C10A—C1A1.5 (17)C8B—C9B—C10B—C1B2.4 (17)
C8A—C9A—C10A—C11A175.0 (11)C8B—C9B—C10B—C11B177.2 (12)
C6A—C1A—C10A—C9A2.6 (17)C2B—C1B—C10B—C9B177.6 (10)
C2A—C1A—C10A—C9A179.3 (10)C6B—C1B—C10B—C9B0.8 (17)
C6A—C1A—C10A—C11A177.4 (10)C2B—C1B—C10B—C11B1.6 (13)
C2A—C1A—C10A—C11A4.5 (13)C6B—C1B—C10B—C11B176.8 (10)
C9A—C10A—C11A—C15A63.7 (17)C9B—C10B—C11B—C15B64.6 (16)
C1A—C10A—C11A—C15A110.2 (10)C1B—C10B—C11B—C15B110.6 (10)
C9A—C10A—C11A—C16A69.4 (15)C9B—C10B—C11B—C16B67.5 (16)
C1A—C10A—C11A—C16A116.7 (10)C1B—C10B—C11B—C16B117.3 (10)
C9A—C10A—C11A—C12A176.1 (12)C9B—C10B—C11B—C12B179.7 (12)
C1A—C10A—C11A—C12A2.3 (12)C1B—C10B—C11B—C12B4.5 (12)
C3A—C2A—C12A—C13A68.2 (15)C1B—C2B—C12B—C18B109.4 (11)
C1A—C2A—C12A—C13A111.8 (10)C3B—C2B—C12B—C18B69.8 (14)
C3A—C2A—C12A—C18A63.4 (16)C1B—C2B—C12B—C13B117.0 (10)
C1A—C2A—C12A—C18A116.6 (10)C3B—C2B—C12B—C13B63.8 (16)
C3A—C2A—C12A—C11A177.0 (12)C1B—C2B—C12B—C11B4.8 (11)
C1A—C2A—C12A—C11A3.0 (11)C3B—C2B—C12B—C11B176.0 (11)
C10A—C11A—C12A—C13A119.7 (9)C10B—C11B—C12B—C18B115.2 (9)
C15A—C11A—C12A—C13A1.0 (11)C15B—C11B—C12B—C18B123.9 (9)
C16A—C11A—C12A—C13A120.0 (9)C16B—C11B—C12B—C18B4.4 (10)
C10A—C11A—C12A—C2A0.5 (11)C10B—C11B—C12B—C2B5.5 (10)
C15A—C11A—C12A—C2A119.2 (9)C15B—C11B—C12B—C2B115.4 (9)
C16A—C11A—C12A—C2A119.9 (9)C16B—C11B—C12B—C2B125.0 (8)
C10A—C11A—C12A—C18A121.4 (9)C10B—C11B—C12B—C13B123.7 (9)
C15A—C11A—C12A—C18A119.9 (9)C15B—C11B—C12B—C13B2.8 (11)
C16A—C11A—C12A—C18A1.1 (10)C16B—C11B—C12B—C13B116.7 (9)
C2A—C12A—C13A—C14A135.1 (9)C18B—C12B—C13B—C14B94.6 (11)
C18A—C12A—C13A—C14A92.1 (10)C2B—C12B—C13B—C14B131.7 (10)
C11A—C12A—C13A—C14A21.4 (11)C11B—C12B—C13B—C14B20.5 (11)
C19A—O1A—C14A—O2A24.2 (11)C19B—O1B—C14B—O2B23.8 (11)
C19A—O1A—C14A—C13A146.5 (8)C19B—O1B—C14B—C13B146.9 (8)
C19A—O1A—C14A—C15A97.9 (9)C19B—O1B—C14B—C15B96.8 (10)
C20A—O2A—C14A—O1A1.5 (11)C20B—O2B—C14B—O1B0.2 (11)
C20A—O2A—C14A—C13A118.8 (10)C20B—O2B—C14B—C13B120.3 (10)
C20A—O2A—C14A—C15A123.9 (10)C20B—O2B—C14B—C15B122.0 (9)
C12A—C13A—C14A—O1A84.3 (10)C12B—C13B—C14B—O1B83.9 (10)
C12A—C13A—C14A—O2A157.6 (8)C12B—C13B—C14B—O2B157.7 (9)
C12A—C13A—C14A—C15A36.2 (11)C12B—C13B—C14B—C15B36.9 (12)
O1A—C14A—C15A—C11A82.1 (10)O1B—C14B—C15B—C11B80.7 (10)
O2A—C14A—C15A—C11A159.2 (9)O2B—C14B—C15B—C11B161.3 (8)
C13A—C14A—C15A—C11A36.8 (11)C13B—C14B—C15B—C11B38.4 (11)
C10A—C11A—C15A—C14A135.5 (9)C10B—C11B—C15B—C14B139.2 (9)
C16A—C11A—C15A—C14A91.7 (10)C16B—C11B—C15B—C14B88.4 (10)
C12A—C11A—C15A—C14A23.0 (11)C12B—C11B—C15B—C14B24.8 (11)
C10A—C11A—C16A—C17A92.2 (9)C10B—C11B—C16B—C17B86.8 (10)
C15A—C11A—C16A—C17A135.5 (8)C15B—C11B—C16B—C17B140.6 (9)
C12A—C11A—C16A—C17A21.6 (10)C12B—C11B—C16B—C17B26.4 (10)
C24A—O4A—C17A—O3A37.0 (11)C23B—O3B—C17B—O4B32.0 (11)
C24A—O4A—C17A—C18A85.9 (10)C23B—O3B—C17B—C16B89.5 (11)
C24A—O4A—C17A—C16A156.6 (9)C23B—O3B—C17B—C18B153.6 (10)
C23A—O3A—C17A—O4A25.1 (11)C24B—O4B—C17B—O3B6.7 (11)
C23A—O3A—C17A—C18A98.4 (11)C24B—O4B—C17B—C16B114.5 (9)
C23A—O3A—C17A—C16A144.9 (10)C24B—O4B—C17B—C18B128.1 (9)
C11A—C16A—C17A—O4A159.6 (8)C11B—C16B—C17B—O3B81.9 (9)
C11A—C16A—C17A—O3A84.3 (11)C11B—C16B—C17B—O4B160.8 (8)
C11A—C16A—C17A—C18A36.9 (11)C11B—C16B—C17B—C18B39.1 (10)
O4A—C17A—C18A—C12A158.9 (8)C2B—C12B—C18B—C17B93.5 (10)
O3A—C17A—C18A—C12A82.3 (10)C13B—C12B—C18B—C17B133.6 (9)
C16A—C17A—C18A—C12A37.9 (10)C11B—C12B—C18B—C17B19.1 (11)
C13A—C12A—C18A—C17A137.9 (9)O3B—C17B—C18B—C12B84.3 (12)
C2A—C12A—C18A—C17A89.9 (9)O4B—C17B—C18B—C12B158.3 (8)
C11A—C12A—C18A—C17A23.5 (9)C16B—C17B—C18B—C12B36.6 (11)
C14A—O1A—C19A—C21A163.7 (10)C14B—O1B—C19B—C20B37.9 (11)
C14A—O1A—C19A—C20A38.9 (10)C14B—O1B—C19B—C21B161.1 (10)
C14A—O2A—C20A—C19A25.4 (11)C14B—O2B—C20B—C19B22.8 (12)
C14A—O2A—C20A—C22A152.4 (10)C14B—O2B—C20B—C22B146.6 (10)
O1A—C19A—C20A—O2A38.8 (10)O1B—C19B—C20B—O2B37.0 (11)
C21A—C19A—C20A—O2A159.1 (9)C21B—C19B—C20B—O2B155.7 (11)
O1A—C19A—C20A—C22A161.1 (9)O1B—C19B—C20B—C22B154.5 (10)
C21A—C19A—C20A—C22A78.6 (13)C21B—C19B—C20B—C22B86.8 (14)
C17A—O3A—C23A—C25A120.6 (11)C17B—O3B—C23B—C25B168.5 (11)
C17A—O3A—C23A—C24A3.7 (12)C17B—O3B—C23B—C24B42.9 (11)
C17A—O4A—C24A—C26A158.6 (11)C17B—O4B—C24B—C26B145.3 (11)
C17A—O4A—C24A—C23A33.9 (12)C17B—O4B—C24B—C23B19.3 (11)
O3A—C23A—C24A—O4A18.0 (12)O3B—C23B—C24B—O4B37.6 (10)
C25A—C23A—C24A—O4A141.2 (12)C25B—C23B—C24B—O4B156.8 (10)
O3A—C23A—C24A—C26A137.3 (11)O3B—C23B—C24B—C26B158.1 (11)
C25A—C23A—C24A—C26A99.5 (14)C25B—C23B—C24B—C26B82.7 (15)

Experimental details

Crystal data
Chemical formulaC26H30O4
Mr406.50
Crystal system, space groupMonoclinic, P21
Temperature (K)200
a, b, c (Å)8.1172 (11), 22.523 (4), 12.5352 (13)
β (°) 105.362 (12)
V3)2209.9 (5)
Z4
Radiation typeMo Kα
µ (mm1)0.08
Crystal size (mm)0.50 × 0.40 × 0.32
Data collection
DiffractometerRigaku AFC-6S
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
4276, 3990, 2388
Rint0.05
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.063, 0.239, 1.07
No. of reflections3990
No. of parameters549
No. of restraints1
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0563P)2 + 10.0719P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.47, 0.52
Absolute structure(Flack, 1983)
Absolute structure parameter0 (4)

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1994), SAPI91 (Fan, 1991), SHELXL97 (Sheldrick, 1997), TEXSAN.

 

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