Structure of CnCn+2Cn-type (n = even) β′-triacylglycerols

Van Langevelde, A.; Van Malssen, K.; Driessen, R.; Goubitz, K.; Hollander, F.; Peschar, R.; Zwart, P.; Schenk, H.

doi:10.1107/S0108768100009927

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Structure of C_nC_n+2C_n-type (n = even) β′-triacylglycerols

A. Van Langevelde, K. Van Malssen, R. Driessen, K. Goubitz, F. Hollander, R. Peschar, P. Zwart and H. Schenk

The crystal structures of the β′ phase of CLC (1,3-didecanoyl-2-dodecanoylglycerol) and MPM (1,3-ditetradecanoyl-2-hexadecanoylglycerol) have been determined from single-crystal X-ray diffraction and high-resolution X-ray powder diffraction data, respectively. Both these crystals are orthorhombic with space group Iba2 and Z = 8. The unit-cell parameters of β′-CLC are a = 57.368 (6), b = 22.783 (2) and c = 5.6945 (6) Å and the final R value is 0.175. The unit-cell parameters of β′-MPM are a = 76.21 (4), b = 22.63 (1) and c = 5.673 (2) Å and the final R_p value is 0.057. Both the β′-CLC and β′-MPM molecules are crystallized in a chair conformation, having a bend at the glycerol moiety. The zigzag planes of the acyl chains are orthogonally packed, as is typical for a β′ phase. Furthermore, unit-cell parameters of some other members of the C_nC_n+2C_n-type triacylglycerol series have been refined on their high-resolution X-ray powder diffraction pattern. Finally, the crystal structures are compared with the currently known structures and models of triacylglycerols.

Keywords: β′-Triacylglycerols; X-ray powder diffraction; Conformation.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100009927/na0109sup1.cif Contains datablocks global, CLC, MPM
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100009927/na0109CLCsup2.hkl Contains datablock CLC
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100009927/na0109MPMsup3.rtv Contains datablock profile

CCDC references: 156691; 156692

Computing details top

Data collection: SMART for CLC. Cell refinement: SAINT for CLC; UnitCell for MPM. Data reduction: SAINT for CLC; MRIA for MPM. Program(s) used to solve structure: Shake-and-Bake for CLC; MRIA for MPM. Program(s) used to refine structure: Xtal CRYLSQ for CLC; MRIA for MPM. For both compounds, molecular graphics: PLATON. Software used to prepare material for publication: Xtal BONDLA CIFIO for CLC.

(CLC) top

Crystal data top

C₃₅H₆₆O₆	F(000) = 2592
M_r = 582.91	D_x = 1.04 Mg m⁻³
Orthorhombic, Iba2	Melting point: 311 K K
Hall symbol: I 2 -2c	Synchrotron radiation, λ = 0.5061 Å
a = 57.368 (1) Å	µ = 0.04 mm⁻¹
b = 22.783 (1) Å	T = 293 K
c = 5.6945 (5) Å	Needle, white
V = 7442.8 (7) Å³	0.8 × 0.04 × 0.01 mm
Z = 8

Data collection top

Siemens CCD camera diffractometer	R_int = 0.21
Detector resolution: 0.936 pixels mm^-1	θ_max = 15.7°, θ_min = 0.7°
5706 measured reflections	h = −52→51
1642 independent reflections	k = −20→20
1642 reflections with F > 3.50σ(F)	l = −6→5

Refinement top

Refinement on F	0 constraints
Least-squares matrix: block diagonal per atom	Calculated and kept fixed with U = 0.1 Å²
R[F² > 2σ(F²)] = 0.175
wR(F²) = 0.165	(Δ/σ)_max = 0.252
S = 1.55	Δρ_max = 1.07 e Å⁻³
824 reflections	Δρ_min = −1.20 e Å⁻³
167 parameters	Extinction correction: Zachariasen, Eq22 p292 "Cryst. Comp." Munksgaard 1970
145 restraints	Extinction coefficient: 8731 (1494)

Crystal data top

C₃₅H₆₆O₆	V = 7442.8 (7) Å³
M_r = 582.91	Z = 8
Orthorhombic, Iba2	Synchrotron radiation, λ = 0.5061 Å
a = 57.368 (1) Å	µ = 0.04 mm⁻¹
b = 22.783 (1) Å	T = 293 K
c = 5.6945 (5) Å	0.8 × 0.04 × 0.01 mm

Data collection top

Siemens CCD camera diffractometer	1642 reflections with F > 3.50σ(F)
5706 measured reflections	R_int = 0.21
1642 independent reflections	θ_max = 15.7°

Refinement top

R[F² > 2σ(F²)] = 0.175	145 restraints
wR(F²) = 0.165	Calculated and kept fixed with U = 0.1 Å²
S = 1.55	(Δ/σ)_max = 0.252
824 reflections	Δρ_max = 1.07 e Å⁻³
167 parameters	Δρ_min = −1.20 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
C1	0.2394 (4)	0.07597 (7)	0.2021 (13)	0.095 (15)*
C2	0.2627 (4)	0.1016 (11)	0.267 (4)	0.119 (17)*
C3	0.2699 (3)	0.08108 (6)	0.510 (3)	0.085 (13)*
O1a	0.2234 (3)	0.0947 (10)	0.366 (4)	0.087 (9)*
C1a	0.2009 (3)	0.0825 (14)	0.335 (4)	0.082 (13)*
O2a	0.1942 (4)	0.0588 (11)	0.151 (5)	0.106 (10)*
O1b	0.2616 (3)	0.1676 (8)	0.292 (4)	0.062 (7)*
C1b	0.2732 (6)	0.1983 (10)	0.128 (5)	0.092 (15)*
O2b	0.2814 (4)	0.1784 (10)	−0.050 (5)	0.102 (10)*
O1c	0.2930 (3)	0.0962 (8)	0.539 (3)	0.061 (7)*
C1c	0.3031 (4)	0.0770 (13)	0.730 (5)	0.094 (14)*
O2c	0.2935 (4)	0.0387 (10)	0.850 (4)	0.087 (9)*
C2a	0.1829 (5)	0.10913 (17)	0.517 (2)	0.16 (2)*
C3a	0.1610 (4)	0.0697 (2)	0.505 (2)	0.056 (10)*
C4a	0.1469 (4)	0.08649 (4)	0.7190 (18)	0.070 (12)*
C5a	0.1211 (4)	0.07030 (6)	0.6884 (18)	0.085 (14)*
C6a	0.1062 (4)	0.09006 (4)	0.8946 (19)	0.090 (14)*
C7a	0.0811 (4)	0.06940 (6)	0.8651 (19)	0.116 (17)*
C8a	0.0662 (4)	0.09357 (5)	1.057 (2)	0.104 (15)*
C9a	0.0416 (5)	0.06708 (10)	1.039 (2)	0.20 (3)*
C10a	0.02665 (2)	0.09869 (5)	1.2077 (2)	0.21 (3)*
C2b	0.27672 (18)	0.2629 (8)	0.188 (3)	0.089 (14)*
C3b	0.2895 (5)	0.26955 (12)	0.429 (2)	0.118 (17)*
C4b	0.3149 (4)	0.25383 (4)	0.3795 (17)	0.079 (13)*
C5b	0.3304 (4)	0.27059 (8)	0.5930 (17)	0.058 (11)*
C6b	0.3542 (4)	0.24838 (4)	0.5609 (16)	0.056 (11)*
C7b	0.3696 (4)	0.26984 (4)	0.767 (2)	0.104 (15)*
C8b	0.3944 (4)	0.24753 (4)	0.749 (2)	0.129 (18)*
C9b	0.4089 (4)	0.26926 (7)	0.956 (2)	0.095 (15)*
C10b	0.4327 (4)	0.24288 (5)	0.948 (2)	0.102 (16)*
C11b	0.4472 (5)	0.26806 (4)	1.150 (2)	0.14 (2)*
C12b	0.47106 (3)	0.24508 (4)	1.11927 (15)	0.27 (4)*
C2c	0.3251 (4)	0.11090 (9)	0.817 (3)	0.19 (3)*
C3c	0.3391 (4)	0.07022 (11)	0.996 (2)	0.102 (15)*
C4c	0.3622 (4)	0.10017 (5)	1.032 (3)	0.102 (14)*
C5c	0.3754 (4)	0.07134 (6)	1.226 (2)	0.119 (17)*
C6c	0.3998 (4)	0.09744 (4)	1.245 (2)	0.115 (16)*
C7c	0.4133 (4)	0.07067 (11)	1.457 (3)	0.121 (18)*
C8c	0.4352 (5)	0.10473 (5)	1.498 (3)	0.17 (2)*
C9c	0.4498 (5)	0.07185 (15)	1.682 (2)	0.23 (3)*
C10c	0.47335 (3)	0.09280 (4)	1.65463 (15)	0.26 (4)*
H11	0.23474	0.08971	0.04216	0.10000*
H12	0.24032	0.03214	0.20340	0.10000*
H2	0.27470	0.09028	0.14844	0.10000*
H31	0.26010	0.10077	0.63219	0.10000*
H32	0.26800	0.03756	0.52289	0.10000*
H21a	0.18958	0.10844	0.67929	0.10000*
H22a	0.17882	0.15041	0.47365	0.10000*
H31a	0.15197	0.07757	0.35762	0.10000*
H32a	0.16540	0.02725	0.51055	0.10000*
H41a	0.15320	0.06534	0.85903	0.10000*
H42a	0.14815	0.12980	0.74439	0.10000*
H51a	0.11509	0.08942	0.54228	0.10000*
H52a	0.11978	0.02670	0.67279	0.10000*
H61a	0.11275	0.07322	1.04279	0.10000*
H62a	0.10648	0.13389	0.90382	0.10000*
H71a	0.07505	0.08317	0.70999	0.10000*
H72a	0.08067	0.02555	0.87086	0.10000*
H81a	0.07310	0.08336	1.21256	0.10000*
H82a	0.06518	0.13722	1.04102	0.10000*
H91a	0.03540	0.07213	0.87589	0.10000*
H92a	0.04206	0.02436	1.07884	0.10000*
H101a	0.03301	0.09361	1.36990	0.10000*
H102a	0.02635	0.14138	1.16695	0.10000*
H103a	0.01046	0.08252	1.20068	0.10000*
H21b	0.28630	0.28191	0.06294	0.10000*
H22b	0.26119	0.28270	0.19793	0.10000*
H31b	0.28822	0.31080	0.48724	0.10000*
H32b	0.28267	0.24212	0.54736	0.10000*
H41b	0.31619	0.21067	0.35024	0.10000*
H42b	0.32038	0.27573	0.23759	0.10000*
H51b	0.33092	0.31429	0.60848	0.10000*
H52b	0.32365	0.25315	0.73893	0.10000*
H61b	0.35398	0.20450	0.55836	0.10000*
H62b	0.36066	0.26335	0.40921	0.10000*
H71b	0.36987	0.31373	0.76564	0.10000*
H72b	0.36267	0.25567	0.91734	0.10000*
H81b	0.39429	0.20364	0.74934	0.10000*
H82b	0.40154	0.26201	0.59984	0.10000*
H91b	0.41020	0.31299	0.94882	0.10000*
H92b	0.40108	0.25768	1.10639	0.10000*
H101b	0.43151	0.19928	0.96450	0.10000*
H102b	0.44025	0.25267	0.79462	0.10000*
H111b	0.44728	0.31192	1.14353	0.10000*
H112b	0.44070	0.25500	1.30471	0.10000*
H121b	0.47073	0.20122	1.12508	0.10000*
H122b	0.47731	0.25814	0.96390	0.10000*
H123b	0.48129	0.26030	1.24772	0.10000*
H21c	0.33527	0.12094	0.68082	0.10000*
H22c	0.32014	0.14778	0.89871	0.10000*
H31c	0.33049	0.06694	1.14871	0.10000*
H32c	0.34138	0.03017	0.92835	0.10000*
H41c	0.37146	0.09779	0.88384	0.10000*
H42c	0.35946	0.14228	1.07346	0.10000*
H51c	0.36696	0.07733	1.37712	0.10000*
H52c	0.37673	0.02837	1.19229	0.10000*
H61c	0.40858	0.08910	1.09757	0.10000*
H62c	0.39846	0.14085	1.26773	0.10000*
H71c	0.40331	0.07249	1.60116	0.10000*
H72c	0.41728	0.02884	1.42248	0.10000*
H81c	0.44422	0.10802	1.34835	0.10000*
H82c	0.43135	0.14489	1.55734	0.10000*
H91c	0.44399	0.08066	1.84394	0.10000*
H92c	0.44910	0.02858	1.65378	0.10000*
H101c	0.47890	0.08406	1.49186	0.10000*
H102c	0.47378	0.13614	1.68202	0.10000*
H103c	0.48371	0.07274	1.77085	0.10000*

Geometric parameters (Å, º) top

C1—H11	1.000 (10)	C5b—H51b	1.000 (2)
C1—H12	1.000 (2)	C5b—C6b	1.47 (3)
C1—O1a	1.38 (3)	C6b—H62b	1.000 (11)
C1—C2	1.50 (3)	C6b—H61b	1.0000 (11)
C2—H2	1.00 (2)	C6b—C7b	1.55 (2)
C2—O1b	1.51 (3)	C7b—H71b	1.0000 (11)
C2—C3	1.52 (3)	C7b—H72b	1.000 (14)
C3—H31	1.000 (16)	C7b—C8b	1.51 (3)
C3—H32	1.000 (3)	C8b—H81b	0.9998 (10)
C3—O1c	1.38 (3)	C8b—H82b	1.000 (15)
O1a—C1a	1.33 (3)	C8b—C9b	1.53 (2)
C1a—O2a	1.24 (4)	C9b—H91b	1.000 (2)
C1a—C2a	1.59 (3)	C9b—H92b	1.000 (15)
C2a—H21a	1.000 (14)	C9b—C10b	1.49 (3)
C2a—H22a	1.000 (8)	C10b—H102b	1.000 (15)
C2a—C3a	1.55 (3)	C10b—H101b	1.000 (2)
C3a—H32a	1.000 (7)	C10b—C11b	1.53 (2)
C3a—H31a	1.000 (15)	C11b—H112b	1.000 (14)
C3a—C4a	1.51 (2)	C11b—H111b	1.0001 (11)
C4a—H41a	1.000 (12)	C11b—C12b	1.48 (3)
C4a—H42a	1.000 (2)	C12b—H121b	1.0000 (10)
C4a—C5a	1.53 (3)	C12b—H122b	1.0001 (10)
C5a—H51a	1.000 (12)	C12b—H123b	1.0001 (11)
C5a—H52a	1.000 (2)	O1c—C1c	1.31 (3)
C5a—C6a	1.52 (2)	C1c—O2c	1.24 (4)
C6a—H62a	0.9999 (12)	C1c—C2c	1.56 (3)
C6a—H61a	1.000 (13)	C2c—H21c	1.00 (2)
C6a—C7a	1.52 (3)	C2c—H22c	1.000 (11)
C7a—H71a	1.000 (13)	C2c—C3c	1.59 (2)
C7a—H72a	1.0000 (16)	C3c—H31c	1.000 (16)
C7a—C8a	1.49 (2)	C3c—H32c	1.000 (6)
C8a—H81a	1.000 (14)	C3c—C4c	1.51 (3)
C8a—H82a	1.000 (2)	C4c—H41c	1.000 (17)
C8a—C9a	1.54 (4)	C4c—H42c	1.000 (5)
C9a—H91a	1.000 (15)	C4c—C5c	1.49 (2)
C9a—H92a	1.000 (4)	C5c—H52c	1.000 (3)
C9a—C10a	1.48 (2)	C5c—H51c	1.000 (17)
O1b—C1b	1.34 (3)	C5c—C6c	1.52 (3)
C1b—O2b	1.20 (4)	C6c—H61c	1.000 (17)
C1b—C2b	1.53 (3)	C6c—H62c	1.000 (3)
C10a—H102a	0.9999 (11)	C6c—C7c	1.56 (2)
C10a—H103a	1.0000 (11)	C7c—H72c	1.000 (7)
C10a—H101a	1.0001 (12)	C7c—H71c	1.000 (19)
C2b—H22b	1.000 (13)	C7c—C8c	1.50 (3)
C2b—H21b	1.000 (17)	C8c—H82c	1.000 (8)
C2b—C3b	1.56 (2)	C8c—H81c	1.000 (19)
C3b—H31b	1.000 (5)	C8c—C9c	1.54 (3)
C3b—H32b	1.000 (13)	C9c—H91c	1.000 (15)
C3b—C4b	1.53 (3)	C9c—H92c	1.000 (4)
C4b—H41b	1.000 (3)	C9c—C10c	1.44 (3)
C4b—H42b	1.000 (11)	C10c—H101c	1.0000 (9)
C4b—C5b	1.55 (2)	C10c—H102c	1.0000 (9)
C5b—H52b	1.000 (12)	C10c—H103c	1.0000 (12)

O1a—C1—C2	107.8 (13)	H22b—C2b—H21b	109.5 (17)
O1b—C2—C1	112.0 (16)	H22b—C2b—C1b	109.2 (16)
O1b—C2—C3	103.5 (15)	H22b—C2b—C3b	109.1 (16)
C1—C2—C3	110.3 (15)	H21b—C2b—C1b	109.2 (18)
O1c—C3—C2	107.1 (15)	H21b—C2b—C3b	109.1 (13)
C1a—O1a—C1	119 (2)	H31b—C3b—H32b	109.5 (14)
O2a—C1a—O1a	120 (2)	H31b—C3b—C4b	110.4 (18)
O2a—C1a—C2a	121.4 (18)	H31b—C3b—C2b	110.6 (14)
O1a—C1a—C2a	118 (2)	H32b—C3b—C4b	110.4 (13)
C3a—C2a—C1a	106.0 (11)	H32b—C3b—C2b	110.5 (17)
C4a—C3a—C2a	104.5 (10)	H41b—C4b—H42b	109.5 (11)
C3a—C4a—C5a	111.3 (11)	H41b—C4b—C3b	109.3 (16)
C6a—C5a—C4a	112.4 (11)	H41b—C4b—C5b	109.2 (12)
C5a—C6a—C7a	110.7 (11)	H42b—C4b—C3b	109.3 (13)
C8a—C7a—C6a	110.4 (11)	H42b—C4b—C5b	109.2 (15)
C7a—C8a—C9a	109.5 (11)	H52b—C5b—H51b	109.4 (10)
C10a—C9a—C8a	107.3 (8)	H52b—C5b—C6b	109.2 (11)
C1b—O1b—C2	115.7 (19)	H52b—C5b—C4b	109.3 (15)
O2b—C1b—O1b	126 (2)	H51b—C5b—C6b	109.2 (16)
O2b—C1b—C2b	120 (2)	H51b—C5b—C4b	109.2 (10)
O1b—C1b—C2b	114 (2)	H62b—C6b—H61b	109.5 (9)
C1b—C2b—C3b	110.8 (15)	H62b—C6b—C5b	109.6 (11)
C4b—C3b—C2b	105.4 (11)	H62b—C6b—C7b	109.5 (15)
C3b—C4b—C5b	110.3 (11)	H61b—C6b—C5b	109.6 (15)
C6b—C5b—C4b	110.5 (10)	H61b—C6b—C7b	109.5 (10)
C5b—C6b—C7b	109.2 (10)	H71b—C7b—H72b	109.5 (11)
C8b—C7b—C6b	112.4 (11)	H71b—C7b—C8b	108.7 (17)
C7b—C8b—C9b	110.6 (11)	H71b—C7b—C6b	108.8 (12)
C10b—C9b—C8b	110.0 (11)	H72b—C7b—C8b	108.7 (13)
C9b—C10b—C11b	108.8 (11)	H72b—C7b—C6b	108.7 (17)
C12b—C11b—C10b	106.3 (10)	H81b—C8b—H82b	109.5 (12)
C1c—O1c—C3	116.3 (18)	H81b—C8b—C7b	109.2 (18)
O2c—C1c—O1c	120 (2)	H81b—C8b—C9b	109.2 (12)
O2c—C1c—C2c	122 (2)	H82b—C8b—C7b	109.2 (13)
O1c—C1c—C2c	117 (2)	H82b—C8b—C9b	109.1 (17)
C1c—C2c—C3c	108.9 (13)	H91b—C9b—H92b	109.5 (11)
C4c—C3c—C2c	105.5 (10)	H91b—C9b—C10b	109.3 (17)
C5c—C4c—C3c	110.5 (11)	H91b—C9b—C8b	109.4 (11)
C4c—C5c—C6c	110.5 (11)	H92b—C9b—C10b	109.3 (12)
C5c—C6c—C7c	111.2 (11)	H92b—C9b—C8b	109.3 (17)
C8c—C7c—C6c	109.6 (11)	H102b—C10b—H101b	109.5 (10)
C7c—C8c—C9c	108.2 (11)	H102b—C10b—C9b	109.6 (12)
C10c—C9c—C8c	105.9 (11)	H102b—C10b—C11b	109.6 (17)
H11—C1—H12	109.4 (7)	H101b—C10b—C9b	109.6 (18)
H11—C1—O1a	110 (2)	H101b—C10b—C11b	109.6 (12)
H11—C1—C2	110.0 (16)	H112b—C11b—H111b	109.5 (11)
H12—C1—O1a	109.8 (16)	H112b—C11b—C12b	110.3 (14)
H12—C1—C2	110 (2)	H112b—C11b—C10b	110.2 (18)
H2—C2—C1	110.3 (18)	H111b—C11b—C12b	110 (2)
H2—C2—O1b	110 (2)	H111b—C11b—C10b	110.2 (13)
H2—C2—C3	110.3 (18)	H121b—C12b—H122b	109.46 (9)
H31—C3—H32	109.5 (15)	H121b—C12b—H123b	109.46 (11)
H31—C3—O1c	110.0 (14)	H121b—C12b—C11b	109.5 (4)
H31—C3—C2	110.1 (14)	H122b—C12b—H123b	109.46 (14)
H32—C3—O1c	110.0 (15)	H122b—C12b—C11b	109.5 (4)
H32—C3—C2	110.1 (15)	H123b—C12b—C11b	109.5 (5)
H21a—C2a—H22a	109.5 (7)	H21c—C2c—H22c	109.5 (8)
H21a—C2a—C3a	110.2 (12)	H21c—C2c—C1c	109.7 (17)
H21a—C2a—C1a	110 (2)	H21c—C2c—C3c	109.6 (19)
H22a—C2a—C3a	110 (2)	H22c—C2c—C1c	110 (2)
H22a—C2a—C1a	110.4 (16)	H22c—C2c—C3c	109.6 (15)
H32a—C3a—H31a	109.4 (9)	H31c—C3c—H32c	109.5 (9)
H32a—C3a—C4a	110.7 (9)	H31c—C3c—C4c	110.5 (13)
H32a—C3a—C2a	110.8 (17)	H31c—C3c—C2c	110.5 (18)
H31a—C3a—C4a	110.7 (16)	H32c—C3c—C4c	110.4 (18)
H31a—C3a—C2a	110.7 (10)	H32c—C3c—C2c	110.5 (12)
H41a—C4a—H42a	109.5 (11)	H41c—C4c—H42c	109.5 (10)
H41a—C4a—C3a	109.0 (15)	H41c—C4c—C5c	109.2 (18)
H41a—C4a—C5a	109.0 (12)	H41c—C4c—C3c	109.3 (13)
H42a—C4a—C3a	109.0 (11)	H42c—C4c—C5c	109.2 (12)
H42a—C4a—C5a	109.0 (15)	H42c—C4c—C3c	109.2 (18)
H51a—C5a—H52a	109.5 (11)	H52c—C5c—H51c	109.5 (11)
H51a—C5a—C6a	108.7 (16)	H52c—C5c—C4c	109.2 (13)
H51a—C5a—C4a	108.7 (13)	H52c—C5c—C6c	109.2 (18)
H52a—C5a—C6a	108.7 (12)	H51c—C5c—C4c	109.2 (18)
H52a—C5a—C4a	108.7 (16)	H51c—C5c—C6c	109.2 (14)
H62a—C6a—H61a	109.5 (11)	H61c—C6c—H62c	109.5 (12)
H62a—C6a—C5a	109.2 (12)	H61c—C6c—C5c	109.0 (13)
H62a—C6a—C7a	109.2 (17)	H61c—C6c—C7c	109.1 (17)
H61a—C6a—C5a	109.2 (17)	H62c—C6c—C5c	109.1 (17)
H61a—C6a—C7a	109.1 (13)	H62c—C6c—C7c	109.0 (12)
H71a—C7a—H72a	109.5 (11)	H72c—C7c—H71c	109.5 (11)
H71a—C7a—C8a	109.2 (17)	H72c—C7c—C8c	109.4 (19)
H71a—C7a—C6a	109.3 (14)	H72c—C7c—C6c	109.4 (13)
H72a—C7a—C8a	109.2 (13)	H71c—C7c—C8c	109.4 (13)
H72a—C7a—C6a	109.3 (18)	H71c—C7c—C6c	109.4 (18)
H81a—C8a—H82a	109.5 (10)	H82c—C8c—H81c	109.5 (9)
H81a—C8a—C7a	109.5 (18)	H82c—C8c—C7c	110 (2)
H81a—C8a—C9a	109.4 (13)	H82c—C8c—C9c	109.8 (13)
H82a—C8a—C7a	109.5 (12)	H81c—C8c—C7c	109.8 (14)
H82a—C8a—C9a	109.4 (18)	H81c—C8c—C9c	110 (2)
H91a—C9a—H92a	109.5 (11)	H91c—C9c—H92c	109.5 (12)
H91a—C9a—C10a	110 (2)	H91c—C9c—C10c	110.4 (17)
H91a—C9a—C8a	110.0 (16)	H91c—C9c—C8c	110 (2)
H92a—C9a—C10a	110.0 (15)	H92c—C9c—C10c	110 (2)
H92a—C9a—C8a	110 (2)	H92c—C9c—C8c	110.3 (16)
H102a—C10a—H103a	109.47 (10)	H101c—C10c—H102c	109.47 (9)
H102a—C10a—H101a	109.45 (11)	H101c—C10c—H103c	109.47 (14)
H102a—C10a—C9a	109.5 (3)	H101c—C10c—C9c	109.5 (5)
H103a—C10a—H101a	109.46 (11)	H102c—C10c—H103c	109.48 (11)
H103a—C10a—C9a	109.5 (9)	H102c—C10c—C9c	109.5 (4)
H101a—C10a—C9a	109.5 (8)	H103c—C10c—C9c	109.5 (5)

O1a—C1—C2—C3	60.2 (18)	C3b—C4b—C5b—H52b	52.0 (9)
O1a—C1—C2—O1b	−54 (2)	H41b—C4b—C5b—C6b	52.0 (17)
O1a—C1—C2—H2	−177.8 (18)	H41b—C4b—C5b—H51b	172.2 (16)
H11—C1—C2—C3	179.9 (13)	H41b—C4b—C5b—H52b	−68 (2)
H11—C1—C2—O1b	65.2 (19)	H42b—C4b—C5b—C6b	−67.7 (11)
H11—C1—C2—H2	−58 (2)	H42b—C4b—C5b—H51b	52 (2)
H12—C1—C2—C3	−59.5 (17)	H42b—C4b—C5b—H52b	172.2 (12)
H12—C1—C2—O1b	−174.2 (14)	C4b—C5b—C6b—C7b	175.7 (6)
H12—C1—C2—H2	63 (2)	C4b—C5b—C6b—H61b	−64.4 (9)
C2—C1—O1a—C1a	174 (2)	C4b—C5b—C6b—H62b	55.7 (9)
H11—C1—O1a—C1a	54 (2)	H51b—C5b—C6b—C7b	55.5 (10)
H12—C1—O1a—C1a	−67 (3)	H51b—C5b—C6b—H61b	175.4 (8)
C1—C2—C3—O1c	168.3 (14)	H51b—C5b—C6b—H62b	−64.5 (11)
C1—C2—C3—H31	−72.1 (17)	H52b—C5b—C6b—C7b	−64.1 (9)
C1—C2—C3—H32	49 (2)	H52b—C5b—C6b—H61b	55.8 (11)
O1b—C2—C3—O1c	−71.8 (17)	H52b—C5b—C6b—H62b	175.9 (8)
O1b—C2—C3—H31	47.8 (18)	C5b—C6b—C7b—C8b	178.7 (7)
O1b—C2—C3—H32	168.6 (16)	C5b—C6b—C7b—H71b	−60.9 (18)
H2—C2—C3—O1c	46 (2)	C5b—C6b—C7b—H72b	58.3 (10)
H2—C2—C3—H31	165.8 (17)	H61b—C6b—C7b—C8b	58.7 (17)
H2—C2—C3—H32	−73 (2)	H61b—C6b—C7b—H71b	179.1 (17)
C1—C2—O1b—C1b	−112 (2)	H61b—C6b—C7b—H72b	−62 (2)
C3—C2—O1b—C1b	130 (2)	H62b—C6b—C7b—C8b	−61.4 (10)
H2—C2—O1b—C1b	11 (3)	H62b—C6b—C7b—H71b	59 (2)
C2—C3—O1c—C1c	−173 (2)	H62b—C6b—C7b—H72b	178.2 (11)
H31—C3—O1c—C1c	67 (2)	C6b—C7b—C8b—C9b	−179.5 (7)
H32—C3—O1c—C1c	−54 (2)	C6b—C7b—C8b—H81b	−59.3 (12)
C1—O1a—C1a—O2a	−6 (4)	C6b—C7b—C8b—H82b	60.4 (10)
C1—O1a—C1a—C2a	−175.5 (16)	H71b—C7b—C8b—C9b	60.1 (11)
O1a—C1a—C2a—C3a	−158 (2)	H71b—C7b—C8b—H81b	−179.8 (10)
O1a—C1a—C2a—H21a	−38 (3)	H71b—C7b—C8b—H82b	−60.1 (13)
O1a—C1a—C2a—H22a	83 (3)	H72b—C7b—C8b—C9b	−59.0 (10)
O2a—C1a—C2a—C3a	33 (3)	H72b—C7b—C8b—H81b	61.1 (13)
O2a—C1a—C2a—H21a	153 (2)	H72b—C7b—C8b—H82b	−179.2 (8)
O2a—C1a—C2a—H22a	−86 (3)	C7b—C8b—C9b—C10b	175.2 (8)
C2—O1b—C1b—O2b	11 (4)	C7b—C8b—C9b—H91b	−64.7 (18)
C2—O1b—C1b—C2b	−166.1 (18)	C7b—C8b—C9b—H92b	55.2 (10)
O1b—C1b—C2b—C3b	56 (3)	H81b—C8b—C9b—C10b	55 (2)
O1b—C1b—C2b—H21b	176 (2)	H81b—C8b—C9b—H91b	175.1 (18)
O1b—C1b—C2b—H22b	−64 (3)	H81b—C8b—C9b—H92b	−65 (2)
O2b—C1b—C2b—C3b	−121 (3)	H82b—C8b—C9b—C10b	−64.6 (11)
O2b—C1b—C2b—H21b	0 (3)	H82b—C8b—C9b—H91b	55 (2)
O2b—C1b—C2b—H22b	119 (3)	H82b—C8b—C9b—H92b	175.4 (11)
C3—O1c—C1c—O2c	13 (3)	C8b—C9b—C10b—C11b	177.0 (8)
C3—O1c—C1c—C2c	−157.3 (17)	C8b—C9b—C10b—H101b	−63.1 (12)
O1c—C1c—C2c—C3c	−162 (2)	C8b—C9b—C10b—H102b	57.1 (11)
O1c—C1c—C2c—H21c	−42 (3)	H91b—C9b—C10b—C11b	56.9 (12)
O1c—C1c—C2c—H22c	78 (3)	H91b—C9b—C10b—H101b	176.8 (10)
O2c—C1c—C2c—C3c	28 (3)	H91b—C9b—C10b—H102b	−63.0 (13)
O2c—C1c—C2c—H21c	147 (2)	H92b—C9b—C10b—C11b	−62.9 (11)
O2c—C1c—C2c—H22c	−92 (3)	H92b—C9b—C10b—H101b	57.0 (13)
C1a—C2a—C3a—C4a	166.4 (13)	H92b—C9b—C10b—H102b	177.2 (9)
C1a—C2a—C3a—H31a	−74.4 (16)	C9b—C10b—C11b—C12b	−174.5 (7)
C1a—C2a—C3a—H32a	47.2 (16)	C9b—C10b—C11b—H111b	−55 (2)
H21a—C2a—C3a—C4a	46.9 (15)	C9b—C10b—C11b—H112b	65.9 (12)
H21a—C2a—C3a—H31a	166.1 (12)	H101b—C10b—C11b—C12b	65.6 (18)
H21a—C2a—C3a—H32a	−72.3 (16)	H101b—C10b—C11b—H111b	−174.9 (19)
H22a—C2a—C3a—C4a	−74.1 (12)	H101b—C10b—C11b—H112b	−54 (2)
H22a—C2a—C3a—H31a	45.1 (15)	H102b—C10b—C11b—C12b	−54.6 (10)
H22a—C2a—C3a—H32a	166.7 (10)	H102b—C10b—C11b—H111b	65 (2)
C2a—C3a—C4a—C5a	158.1 (8)	H102b—C10b—C11b—H112b	−174.2 (12)
C2a—C3a—C4a—H41a	−81.6 (12)	C10b—C11b—C12b—H121b	−60.0 (7)
C2a—C3a—C4a—H42a	37.9 (18)	C10b—C11b—C12b—H122b	60.0 (6)
H31a—C3a—C4a—C5a	38.9 (8)	C10b—C11b—C12b—H123b	180.0 (5)
H31a—C3a—C4a—H41a	159.2 (11)	H111b—C11b—C12b—H121b	−179.5 (8)
H31a—C3a—C4a—H42a	−81.3 (17)	H111b—C11b—C12b—H122b	−59.5 (10)
H32a—C3a—C4a—C5a	−82.6 (16)	H111b—C11b—C12b—H123b	60.5 (10)
H32a—C3a—C4a—H41a	38 (2)	H112b—C11b—C12b—H121b	59.5 (10)
H32a—C3a—C4a—H42a	157.2 (16)	H112b—C11b—C12b—H122b	179.5 (7)
C3a—C4a—C5a—C6a	−176.5 (5)	H112b—C11b—C12b—H123b	−60.5 (9)
C3a—C4a—C5a—H51a	−56.0 (8)	C1c—C2c—C3c—C4c	168.3 (15)
C3a—C4a—C5a—H52a	63.1 (10)	C1c—C2c—C3c—H31c	−72.3 (16)
H41a—C4a—C5a—C6a	63.2 (8)	C1c—C2c—C3c—H32c	49 (2)
H41a—C4a—C5a—H51a	−176.3 (7)	H21c—C2c—C3c—C4c	48.3 (13)
H41a—C4a—C5a—H52a	−57.2 (11)	H21c—C2c—C3c—H31c	167.7 (11)
H42a—C4a—C5a—C6a	−56.2 (10)	H21c—C2c—C3c—H32c	−71 (2)
H42a—C4a—C5a—H51a	64.3 (11)	H22c—C2c—C3c—C4c	−72 (2)
H42a—C4a—C5a—H52a	−176.6 (9)	H22c—C2c—C3c—H31c	48 (2)
C4a—C5a—C6a—C7a	−176.0 (6)	H22c—C2c—C3c—H32c	168.9 (18)
C4a—C5a—C6a—H61a	−55.9 (10)	C2c—C3c—C4c—C5c	171.0 (11)
C4a—C5a—C6a—H62a	63.8 (17)	C2c—C3c—C4c—H41c	−68.8 (12)
H51a—C5a—C6a—C7a	63.5 (11)	C2c—C3c—C4c—H42c	50.9 (15)
H51a—C5a—C6a—H61a	−176.3 (12)	H31c—C3c—C4c—C5c	51.6 (14)
H51a—C5a—C6a—H62a	−57 (2)	H31c—C3c—C4c—H41c	171.8 (9)
H52a—C5a—C6a—C7a	−55.6 (17)	H31c—C3c—C4c—H42c	−68.5 (14)
H52a—C5a—C6a—H61a	65 (2)	H32c—C3c—C4c—C5c	−69.6 (15)
H52a—C5a—C6a—H62a	−175.8 (17)	H32c—C3c—C4c—H41c	50.5 (13)
C5a—C6a—C7a—C8a	−174.8 (6)	H32c—C3c—C4c—H42c	170.3 (11)
C5a—C6a—C7a—H71a	−54.7 (9)	C3c—C4c—C5c—C6c	174.2 (10)
C5a—C6a—C7a—H72a	65.1 (10)	C3c—C4c—C5c—H51c	−65.6 (12)
H61a—C6a—C7a—C8a	65.0 (9)	C3c—C4c—C5c—H52c	54 (2)
H61a—C6a—C7a—H71a	−174.9 (8)	H41c—C4c—C5c—C6c	54.0 (11)
H61a—C6a—C7a—H72a	−55.1 (12)	H41c—C4c—C5c—H51c	174.2 (10)
H62a—C6a—C7a—C8a	−54.6 (11)	H41c—C4c—C5c—H52c	−66 (2)
H62a—C6a—C7a—H71a	65.5 (12)	H42c—C4c—C5c—C6c	−66 (2)
H62a—C6a—C7a—H72a	−174.8 (9)	H42c—C4c—C5c—H51c	55 (2)
C6a—C7a—C8a—C9a	−174.1 (7)	H42c—C4c—C5c—H52c	174.2 (18)
C6a—C7a—C8a—H81a	−54.1 (10)	C4c—C5c—C6c—C7c	176.3 (10)
C6a—C7a—C8a—H82a	65.9 (18)	C4c—C5c—C6c—H61c	−63.5 (12)
H71a—C7a—C8a—C9a	65.8 (12)	C4c—C5c—C6c—H62c	56.0 (15)
H71a—C7a—C8a—H81a	−174.3 (12)	H51c—C5c—C6c—C7c	56.1 (12)
H71a—C7a—C8a—H82a	−54 (2)	H51c—C5c—C6c—H61c	176.4 (8)
H72a—C7a—C8a—C9a	−54 (2)	H51c—C5c—C6c—H62c	−64.2 (14)
H72a—C7a—C8a—H81a	66 (2)	H52c—C5c—C6c—C7c	−63.6 (15)
H72a—C7a—C8a—H82a	−173.9 (18)	H52c—C5c—C6c—H61c	56.7 (14)
C7a—C8a—C9a—C10a	−171.6 (7)	H52c—C5c—C6c—H62c	176.2 (12)
C7a—C8a—C9a—H91a	−52.0 (13)	C5c—C6c—C7c—C8c	−169.7 (11)
C7a—C8a—C9a—H92a	68.7 (12)	C5c—C6c—C7c—H71c	−49.7 (10)
H81a—C8a—C9a—C10a	68.3 (10)	C5c—C6c—C7c—H72c	70 (2)
H81a—C8a—C9a—H91a	−172.0 (10)	H61c—C6c—C7c—C8c	70.0 (12)
H81a—C8a—C9a—H92a	−51.3 (14)	H61c—C6c—C7c—H71c	−170.0 (9)
H82a—C8a—C9a—C10a	−51.6 (11)	H61c—C6c—C7c—H72c	−50 (2)
H82a—C8a—C9a—H91a	68.0 (14)	H62c—C6c—C7c—C8c	−49 (2)
H82a—C8a—C9a—H92a	−171.3 (10)	H62c—C6c—C7c—H71c	71 (2)
C8a—C9a—C10a—H101a	−60.0 (6)	H62c—C6c—C7c—H72c	−169.5 (18)
C8a—C9a—C10a—H102a	60.0 (10)	C6c—C7c—C8c—C9c	−171.6 (12)
C8a—C9a—C10a—H103a	180.0 (5)	C6c—C7c—C8c—H81c	−51.8 (15)
H91a—C9a—C10a—H101a	−179.7 (11)	C6c—C7c—C8c—H82c	68.6 (17)
H91a—C9a—C10a—H102a	−59.7 (16)	H71c—C7c—C8c—C9c	68.4 (15)
H91a—C9a—C10a—H103a	60.3 (12)	H71c—C7c—C8c—H81c	−171.8 (11)
H92a—C9a—C10a—H101a	60 (2)	H71c—C7c—C8c—H82c	−51.4 (16)
H92a—C9a—C10a—H102a	179.7 (15)	H72c—C7c—C8c—C9c	−51.5 (18)
H92a—C9a—C10a—H103a	−60 (2)	H72c—C7c—C8c—H81c	68.3 (16)
C1b—C2b—C3b—C4b	74.9 (16)	H72c—C7c—C8c—H82c	−171.3 (13)
C1b—C2b—C3b—H31b	−166 (2)	C7c—C8c—C9c—C10c	159.8 (10)
C1b—C2b—C3b—H32b	−44 (2)	C7c—C8c—C9c—H91c	−80.8 (16)
H21b—C2b—C3b—C4b	−45.3 (14)	C7c—C8c—C9c—H92c	40 (3)
H21b—C2b—C3b—H31b	74 (2)	H81c—C8c—C9c—C10c	40.0 (10)
H21b—C2b—C3b—H32b	−164.6 (16)	H81c—C8c—C9c—H91c	159.4 (15)
H22b—C2b—C3b—C4b	−164.8 (11)	H81c—C8c—C9c—H92c	−80 (2)
H22b—C2b—C3b—H31b	−46 (2)	H82c—C8c—C9c—C10c	−80 (2)
H22b—C2b—C3b—H32b	75.9 (18)	H82c—C8c—C9c—H91c	39 (3)
C2b—C3b—C4b—C5b	168.8 (8)	H82c—C8c—C9c—H92c	160 (2)
C2b—C3b—C4b—H41b	−71.1 (11)	C8c—C9c—C10c—H101c	−60.0 (7)
C2b—C3b—C4b—H42b	48.7 (11)	C8c—C9c—C10c—H102c	60.0 (8)
H31b—C3b—C4b—C5b	49.4 (11)	C8c—C9c—C10c—H103c	180.0 (6)
H31b—C3b—C4b—H41b	169.5 (10)	H91c—C9c—C10c—H101c	−179.4 (7)
H31b—C3b—C4b—H42b	−70.7 (13)	H91c—C9c—C10c—H102c	−59.4 (10)
H32b—C3b—C4b—C5b	−71.9 (10)	H91c—C9c—C10c—H103c	60.6 (10)
H32b—C3b—C4b—H41b	48.3 (14)	H92c—C9c—C10c—H101c	59.4 (11)
H32b—C3b—C4b—H42b	168.0 (9)	H92c—C9c—C10c—H102c	179.4 (8)
C3b—C4b—C5b—C6b	172.2 (5)	H92c—C9c—C10c—H103c	−60.6 (11)
C3b—C4b—C5b—H51b	−67.7 (15)

(MPM) top

Crystal data top

C₄₇H₉₀O₆	Z = 8
M_r = 751.23	Melting point: 334 K K
Orthorhombic, Iba2	? radiation, λ = 0.650515 Å
Hall symbol: I 2 -2c	µ = 0.49 mm⁻¹
a = 76.21 (4) Å	T = 295 K
b = 22.63 (1) Å	white
c = 5.673 (2) Å	cylinder, ? × 1.5 mm mm
V = 9784 (8) Å³

Data collection top

ESRF BM16 diffractometer	Data collection mode: transmission
Radiation source: synchrotron	Scan method: continuous
Specimen mounting: capillary	2θ_min = 2.07°, 2θ_max = 27.0°, 2θ_step = 0.003°

Refinement top

R_p = 7.9	Profile function: split-type pseudo-Voigt
R_wp = 11.4	775 parameters
R_exp = ?	276 restraints
R_Bragg = 5.7	Calculated and kept fixed
R(F²) = 7.4
χ² = 8.526	Background function: polynomal
12637 data points	Preferred orientation correction: 'Ahtee and Jarvinen'

Crystal data top

C₄₇H₉₀O₆	V = 9784 (8) Å³
M_r = 751.23	Z = 8
Orthorhombic, Iba2	? radiation, λ = 0.650515 Å
a = 76.21 (4) Å	µ = 0.49 mm⁻¹
b = 22.63 (1) Å	T = 295 K
c = 5.673 (2) Å	cylinder, ? × 1.5 mm mm

Data collection top

ESRF BM16 diffractometer	Scan method: continuous
Specimen mounting: capillary	2θ_min = 2.07°, 2θ_max = 27.0°, 2θ_step = 0.003°
Data collection mode: transmission

Refinement top

R_p = 7.9	χ² = 8.526
R_wp = 11.4	12637 data points
R_exp = ?	775 parameters
R_Bragg = 5.7	276 restraints
R(F²) = 7.4	Calculated and kept fixed

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
C1	0.242 (2)	0.074 (6)	−0.839 (10)	0.01800*
C2	0.259 (2)	0.100 (6)	−0.77 (2)	0.01800*
C3	0.264 (2)	0.081 (6)	−0.528 (17)	0.01800*
O1a	0.229 (2)	0.094 (4)	−0.681 (13)	0.01800*
C1a	0.213 (2)	0.081 (6)	−0.713 (19)	0.01800*
O2a	0.208 (2)	0.055 (4)	−0.896 (12)	0.01800*
C2a	0.199 (3)	0.111 (6)	−0.550 (16)	0.01800*
C3a	0.182 (3)	0.071 (6)	−0.558 (17)	0.01800*
C4a	0.172 (2)	0.090 (7)	−0.35 (2)	0.01800*
C5a	0.153 (3)	0.073 (7)	−0.37 (2)	0.01800*
C6a	0.142 (2)	0.094 (7)	−0.16 (2)	0.01800*
C7a	0.123 (3)	0.071 (5)	−0.17 (3)	0.01800*
C8a	0.113 (2)	0.095 (6)	0.025 (17)	0.01800*
C9a	0.095 (2)	0.066 (7)	0.023 (18)	0.01800*
C10a	0.083 (2)	0.096 (7)	0.21 (2)	0.01800*
C11a	0.065 (2)	0.067 (7)	0.20 (2)	0.01800*
C12a	0.053 (3)	0.096 (7)	0.381 (18)	0.01800*
C13a	0.035 (3)	0.067 (7)	0.373 (18)	0.01800*
C14a	0.023 (2)	0.097 (7)	0.555 (19)	0.01800*
O1b	0.258 (2)	0.167 (4)	−0.757 (14)	0.01800*
C1b	0.267 (3)	0.197 (6)	−0.92 (2)	0.01800*
O2b	0.273 (2)	0.178 (4)	−1.103 (13)	0.01800*
C2b	0.270 (2)	0.262 (6)	−0.87 (3)	0.01800*
C3b	0.280 (3)	0.269 (6)	−0.63 (2)	0.01800*
C4b	0.298 (3)	0.251 (6)	−0.68 (2)	0.01800*
C5b	0.310 (2)	0.268 (6)	−0.47 (2)	0.01800*
C6b	0.328 (2)	0.245 (7)	−0.50 (2)	0.01800*
C7b	0.339 (2)	0.267 (7)	−0.29 (2)	0.01800*
C8b	0.358 (2)	0.244 (7)	−0.31 (3)	0.01800*
C9b	0.368 (3)	0.267 (6)	−0.10 (2)	0.01800*
C10b	0.386 (3)	0.241 (6)	−0.109 (19)	0.01800*
C11b	0.397 (2)	0.267 (7)	0.09 (2)	0.01800*
C12b	0.416 (2)	0.244 (8)	0.08 (2)	0.01800*
C13b	0.426 (3)	0.267 (6)	0.29 (2)	0.01800*
C14b	0.444 (2)	0.239 (6)	0.29 (2)	0.01800*
C15b	0.455 (2)	0.261 (7)	0.505 (19)	0.01800*
C16b	0.473 (2)	0.231 (7)	0.51 (2)	0.01800*
O1c	0.281 (2)	0.095 (4)	−0.498 (10)	0.01800*
C1c	0.289 (2)	0.077 (7)	−0.303 (18)	0.01800*
O2c	0.281 (2)	0.041 (4)	−0.174 (13)	0.01800*
C2c	0.305 (2)	0.110 (7)	−0.22 (2)	0.01800*
C3c	0.316 (2)	0.070 (6)	−0.039 (18)	0.01800*
C4c	0.333 (3)	0.099 (6)	−0.009 (16)	0.01800*
C5c	0.343 (2)	0.071 (6)	0.19 (2)	0.01800*
C6c	0.361 (2)	0.096 (7)	0.20 (2)	0.01800*
C7c	0.372 (3)	0.070 (6)	0.41 (2)	0.01800*
C8c	0.388 (2)	0.104 (7)	0.443 (15)	0.01800*
C9c	0.399 (2)	0.072 (7)	0.629 (19)	0.01800*
C10c	0.418 (2)	0.095 (7)	0.615 (19)	0.01800*
C11c	0.429 (2)	0.068 (6)	0.81 (2)	0.01800*
C12c	0.448 (3)	0.090 (6)	0.79 (2)	0.01800*
C13c	0.459 (3)	0.064 (6)	0.987 (17)	0.01800*
C14c	0.478 (2)	0.088 (6)	0.96 (2)	0.01800*

Geometric parameters (Å, º) top

C1—O1a	1.41 (17)	C5b—C6b	1.5 (2)
C1—C2	1.5 (2)	C6b—C7b	1.5 (2)
C2—C3	1.50 (17)	C7b—C8b	1.5 (2)
C2—O1b	1.52 (16)	C8b—C9b	1.5 (2)
C3—O1c	1.3 (2)	C9b—C10b	1.5 (3)
O1a—C1a	1.3 (2)	C10b—C11b	1.5 (2)
C1a—O2a	1.25 (15)	C11b—C12b	1.5 (2)
C1a—C2a	1.6 (2)	C12b—C13b	1.5 (2)
C2a—C3a	1.6 (3)	C13b—C14b	1.5 (3)
C3a—C4a	1.5 (2)	C14b—C15b	1.56 (19)
C4a—C5a	1.5 (3)	C15b—C16b	1.5 (2)
C5a—C6a	1.5 (2)	O1c—C1c	1.33 (15)
C6a—C7a	1.5 (3)	C1c—O2c	1.25 (17)
C7a—C8a	1.5 (2)	C1c—C2c	1.5 (2)
C8a—C9a	1.5 (2)	C2c—C3c	1.6 (2)
C9a—C10a	1.5 (2)	C3c—C4c	1.5 (3)
C10a—C11a	1.5 (2)	C4c—C5c	1.5 (2)
C11a—C12a	1.5 (2)	C5c—C6c	1.5 (2)
C12a—C13a	1.5 (3)	C6c—C7c	1.6 (2)
C13a—C14a	1.5 (2)	C7c—C8c	1.5 (3)
O1b—C1b	1.35 (19)	C8c—C9c	1.53 (18)
C1b—O2b	1.20 (17)	C9c—C10c	1.5 (2)
C1b—C2b	1.5 (2)	C10c—C11c	1.53 (19)
C2b—C3b	1.6 (2)	C11c—C12c	1.5 (3)
C3b—C4b	1.5 (3)	C12c—C13c	1.5 (2)
C4b—C5b	1.6 (2)	C13c—C14c	1.6 (3)

O1a···O2a	2.20 (17)	O1a···C1b	4.0 (2)
O1c···O2c	2.21 (11)	C12cⁱ···C13cⁱⁱⁱ	4.0 (2)
O1b···O2b	2.29 (14)	O2aⁱ···C2aⁱⁱ	3.98 (13)
C2···O1c	2.29 (19)	C3ⁱ···O2cⁱⁱ	3.99 (14)
C3···C1c	2.3 (2)	C3···O2b	3.99 (14)
O2b···C2b	2.32 (16)	C10bⁱ···C8cⁱⁱ	4.01 (18)
C1···C1a	2.3 (2)	C3b···O1c	4.01 (16)
C2···O1a	2.3 (2)	C2···O2c	4.01 (17)
C3···O1b	2.38 (16)	O1cⁱ···O2cⁱⁱ	4.02 (10)
C2a···C4a	2.4 (2)	C3···C1a	4.0 (2)
C7c···C9c	2.4 (2)	C6aⁱ···C7b^vi	4.0 (2)
C2b···C4b	2.4 (3)	C1ⁱ···C3ⁱⁱⁱ	4.0 (2)
C8b···C10b	2.4 (3)	C8aⁱ···C11b^vii	4.0 (2)
C7a···C9a	2.4 (3)	C8aⁱ···C9b^vi	4.0 (2)
C3c···C5c	2.4 (2)	O1b···C1c	4.05 (18)
O2c···C2c	2.4 (2)	O2bⁱ···C5bⁱⁱ	4.05 (18)
C5b···C7b	2.4 (2)	C16b···C12c	4.1 (2)
O1b···C2b	2.42 (17)	C13cⁱ···C13c^v	4.05 (17)
O1c···C2c	2.43 (19)	C13cⁱ···C13cⁱⁱⁱ	4.05 (17)
C2···C1b	2.4 (2)	C1ⁱ···O2cⁱⁱⁱ	4.1 (2)
O1a···C2a	2.4 (3)	O1aⁱ···O2a^v	4.07 (14)
O2a···C2a	2.44 (15)	C3aⁱ···C4aⁱⁱⁱ	4.1 (2)
C1···C3	2.44 (17)	C2···O2a	4.1 (2)
C6a···C8a	2.4 (2)	O1aⁱ···C3b^vii	4.08 (16)
C4c···C6c	2.4 (3)	O1bⁱ···C1b^vi	4.09 (19)
C12b···C14b	2.4 (2)	C10aⁱ···C11b^vi	4.1 (2)
C3a···C5a	2.5 (3)	O1a···O1c	4.1 (2)
C2c···C4c	2.5 (3)	O1bⁱ···O2cⁱⁱ	4.10 (14)
C7b···C9b	2.5 (3)	C6aⁱ···C9b^vii	4.1 (2)
C3b···C5b	2.5 (3)	C1aⁱ···C5b^vii	4.1 (2)
C9b···C11b	2.5 (3)	O2bⁱ···C3cⁱⁱ	4.1 (2)
C1···O1b	2.48 (18)	O1cⁱ···C3cⁱⁱ	4.11 (17)
C11b···C13b	2.5 (3)	C4aⁱ···C5b^vi	4.1 (2)
C12c···C14c	2.5 (3)	C3cⁱ···C5cⁱⁱⁱ	4.1 (2)
C6c···C8c	2.5 (2)	C9aⁱ···C9aⁱⁱⁱ	4.1 (2)
C11a···C13a	2.5 (3)	C9aⁱ···C9a^v	4.1 (2)
C12a···C14a	2.5 (3)	O2bⁱ···C4bⁱⁱ	4.13 (18)
C11c···C13c	2.5 (3)	C1cⁱ···C3cⁱⁱⁱ	4.1 (2)
C10a···C12a	2.5 (3)	C7cⁱ···C9cⁱⁱⁱ	4.1 (2)
C8c···C10c	2.5 (2)	C1bⁱ···O1cⁱⁱ	4.14 (15)
C10c···C12c	2.5 (3)	C7aⁱ···C9aⁱⁱⁱ	4.1 (2)
C9a···C11a	2.5 (2)	C4b···C2c	4.1 (2)
C8a···C10a	2.5 (2)	C2bⁱ···C3b^vii	4.1 (3)
C9c···C11c	2.5 (2)	C8b···C4c	4.2 (2)
C4b···C6b	2.5 (3)	C11aⁱ···C11a^v	4.2 (2)
C1b···C3b	2.5 (2)	C13aⁱ···C13aⁱⁱⁱ	4.2 (2)
C13b···C15b	2.5 (3)	C11aⁱ···C11aⁱⁱⁱ	4.2 (2)
C10b···C12b	2.5 (3)	C13aⁱ···C13a^v	4.2 (2)
C6b···C8b	2.5 (2)	C10cⁱ···C11cⁱⁱⁱ	4.2 (2)
C14b···C16b	2.5 (2)	C7b···C4c	4.2 (2)
C1a···C3a	2.5 (3)	C16b···C14c	4.2 (2)
C4a···C6a	2.5 (2)	C8bⁱ···C8cⁱⁱ	4.2 (2)
C5a···C7a	2.5 (3)	C6aⁱ···C8b^vi	4.2 (2)
C1c···C3c	2.5 (2)	C5aⁱ···C9b^vii	4.2 (2)
C5c···C7c	2.6 (3)	C10b···C6c	4.2 (2)
C3···O2c	2.56 (16)	C1aⁱ···C3b^vii	4.18 (18)
C1···O2a	2.6 (2)	C7aⁱ···C11b^vii	4.2 (2)
O2a···C3a	2.8 (2)	C5cⁱ···C7cⁱⁱⁱ	4.2 (2)
C2···O2b	2.79 (17)	C9aⁱ···C10aⁱⁱⁱ	4.2 (2)
O1a···O1b	2.79 (19)	C11cⁱ···C11cⁱⁱⁱ	4.19 (18)
O1b···O1c	2.81 (16)	C11cⁱ···C11c^v	4.19 (18)
C3···O1a	2.8 (2)	C6cⁱ···C7cⁱⁱⁱ	4.2 (2)
O2bⁱ···C1cⁱⁱ	2.83 (18)	C11cⁱ···C13cⁱⁱⁱ	4.2 (2)
O2c···C3c	2.9 (2)	C4aⁱ···C7b^vii	4.2 (2)
O1b···C3b	2.9 (2)	C7aⁱ···C8aⁱⁱⁱ	4.20 (18)
O2bⁱ···C2cⁱⁱ	3.0 (2)	C10aⁱ···C12b^vi	4.2 (2)
O2bⁱ···O1cⁱⁱ	2.99 (12)	C9aⁱ···C11aⁱⁱⁱ	4.2 (2)
C1b···C4b	3.0 (3)	C2bⁱ···C2b^vi	4.2 (2)
C2ⁱ···O2cⁱⁱ	3.13 (18)	C2bⁱ···C2b^vii	4.2 (2)
C3ⁱ···O2cⁱⁱⁱ	3.16 (17)	C12aⁱ···C13b^vi	4.2 (2)
O2bⁱ···O2cⁱⁱ	3.19 (13)	C5aⁱ···C6aⁱⁱⁱ	4.2 (2)
O1cⁱ···O2cⁱⁱⁱ	3.24 (13)	O2cⁱ···C3cⁱⁱⁱ	4.21 (18)
C3ⁱ···O2b^iv	3.33 (15)	C11aⁱ···C12aⁱⁱⁱ	4.2 (2)
O2cⁱ···O2c^v	3.39 (11)	O2bⁱ···C3b^vii	4.2 (3)
O2cⁱ···O2cⁱⁱⁱ	3.39 (11)	C3aⁱ···C7b^vii	4.2 (2)
C1···C1b	3.4 (2)	C2···C3b	4.2 (2)
O2b···C3b	3.41 (15)	C10bⁱ···C9cⁱⁱ	4.2 (2)
O1bⁱ···C2b^vi	3.45 (18)	O2a···C4a	4.22 (18)
C1cⁱ···O2cⁱⁱⁱ	3.45 (17)	C13aⁱ···C14aⁱⁱⁱ	4.2 (2)
C3···C1b	3.46 (18)	C15b···C12c	4.2 (2)
O2b···C4b	3.5 (2)	C11aⁱ···C13aⁱⁱⁱ	4.2 (2)
C1b···O1c	3.50 (16)	C2aⁱ···C7b^vii	4.2 (2)
C2···C1c	3.5 (2)	C14b···C10c	4.2 (2)
C2···C1a	3.5 (2)	C4aⁱ···C6b^vi	4.2 (2)
C1···O1c	3.58 (19)	C11b···C8c	4.2 (2)
C1aⁱ···O2a^v	3.58 (16)	C1aⁱ···C2b^vi	4.3 (2)
O2aⁱ···C3aⁱⁱⁱ	3.6 (2)	C7cⁱ···C7c^v	4.25 (18)
C1ⁱ···O2cⁱⁱ	3.61 (19)	C3cⁱ···C3cⁱⁱⁱ	4.25 (17)
O1b···C4b	3.6 (2)	C3cⁱ···C3c^v	4.25 (17)
C3···C2c	3.6 (2)	C7cⁱ···C7cⁱⁱⁱ	4.25 (18)
C2ⁱ···O2cⁱⁱⁱ	3.65 (18)	C8aⁱ···C10b^vi	4.25 (18)
C1···O2b	3.66 (18)	O2aⁱ···C5b^vii	4.25 (17)
O2bⁱ···C3bⁱⁱ	3.68 (15)	C1ⁱ···C3ⁱⁱ	4.26 (13)
O1a···C3a	3.7 (3)	O2aⁱ···C3aⁱⁱ	4.26 (17)
C2aⁱ···C5b^vii	3.69 (18)	C9b···C6c	4.3 (2)
O1aⁱ···C2b^vi	3.70 (16)	C1ⁱ···C3b^vii	4.3 (2)
C3c···C6c	3.7 (2)	O2c···C4c	4.3 (3)
C7c···C10c	3.7 (3)	C12bⁱ···C10cⁱⁱ	4.3 (2)
C1a···C4a	3.8 (2)	O2aⁱ···C4aⁱⁱⁱ	4.3 (2)
C2a···C5a	3.8 (3)	C5cⁱ···C5cⁱⁱⁱ	4.29 (19)
C1···C2a	3.8 (2)	C7aⁱ···C7a^v	4.29 (18)
O1c···C3c	3.77 (17)	C3aⁱ···C3aⁱⁱⁱ	4.29 (17)
C2aⁱ···C4b^vi	3.77 (18)	C5cⁱ···C5c^v	4.29 (19)
O2aⁱ···O2aⁱⁱⁱ	3.77 (11)	C3aⁱ···C3a^v	4.29 (17)
O2aⁱ···O2a^v	3.77 (11)	C7aⁱ···C7aⁱⁱⁱ	4.29 (18)
C8b···C11b	3.8 (2)	C4cⁱ···C5cⁱⁱⁱ	4.29 (19)
C7a···C10a	3.8 (3)	C9cⁱ···C11cⁱⁱⁱ	4.3 (2)
C6a···C9a	3.8 (2)	O2aⁱ···C3b^vii	4.30 (17)
C1c···C4c	3.8 (3)	O1cⁱ···C1cⁱⁱⁱ	4.30 (17)
C7b···C10b	3.8 (3)	C9aⁱ···C13b^vii	4.3 (2)
C3b···C6b	3.8 (3)	C3aⁱ···C5aⁱⁱⁱ	4.3 (2)
C2···C2b	3.8 (2)	C1bⁱ···C2b^vi	4.3 (2)
C5c···C8c	3.8 (2)	O1bⁱ···O2b^vi	4.32 (16)
C5a···C8a	3.8 (2)	C2ⁱ···O2b^iv	4.32 (16)
C11b···C14b	3.8 (2)	C9cⁱ···C9c^v	4.3 (2)
C2c···C5c	3.8 (2)	C9cⁱ···C9cⁱⁱⁱ	4.3 (2)
C5b···C8b	3.8 (2)	C6b···C4c	4.32 (19)
C2b···C5b	3.8 (2)	C11aⁱ···C15b^vii	4.3 (2)
C6b···C9b	3.8 (2)	C3ⁱ···C1b^iv	4.33 (17)
C2ⁱ···C1cⁱⁱ	3.82 (19)	C2ⁱ···C3ⁱⁱ	4.33 (17)
C6c···C9c	3.8 (2)	C12b···C8c	4.3 (2)
C4b···C7b	3.8 (2)	C3ⁱ···C1cⁱⁱⁱ	4.3 (2)
C10a···C13a	3.8 (3)	C2ⁱ···C2cⁱⁱ	4.3 (2)
C9b···C12b	3.8 (3)	C13b···C10c	4.3 (2)
C10c···C13c	3.8 (2)	C2aⁱ···C5b^vi	4.34 (17)
O2aⁱ···C4aⁱⁱ	3.84 (18)	C5aⁱ···C7aⁱⁱⁱ	4.3 (2)
C11a···C14a	3.8 (2)	C5aⁱ···C5aⁱⁱⁱ	4.4 (2)
C3a···C6a	3.8 (2)	C5aⁱ···C5a^v	4.4 (2)
C8a···C11a	3.8 (2)	C2ⁱ···C3ⁱⁱⁱ	4.36 (19)
C12b···C15b	3.8 (2)	C3aⁱ···C5b^vii	4.37 (18)
C6b···C2c	3.9 (2)	C8aⁱ···C8b^vi	4.4 (2)
C9a···C12a	3.9 (2)	C4aⁱ···C4b^vi	4.4 (2)
C8c···C11c	3.9 (2)	C8bⁱ···C6cⁱⁱ	4.4 (2)
C1bⁱ···C1cⁱⁱ	3.9 (2)	C12bⁱ···C11cⁱⁱ	4.4 (2)
C1bⁱ···C3b^vii	3.9 (3)	C6cⁱ···C9cⁱⁱ	4.38 (19)
C10b···C13b	3.9 (3)	C1ⁱ···O1aⁱⁱⁱ	4.38 (16)
C11c···C14c	3.9 (2)	C8bⁱ···C7cⁱⁱ	4.4 (2)
C2aⁱ···C2b^vi	3.9 (2)	C1ⁱ···C1ⁱⁱⁱ	4.39 (16)
C5b···C2c	3.9 (2)	C1ⁱ···C1^v	4.39 (16)
O2bⁱ···C2b^vii	3.9 (2)	O1bⁱ···C2b^vii	4.39 (18)
C4c···C7c	3.9 (3)	C2bⁱ···C3bⁱⁱ	4.39 (19)
C13b···C16b	3.9 (3)	C14cⁱ···C14c^viii	4.4 (2)
C9c···C12c	3.9 (3)	C14cⁱ···C14c^ix	4.4 (2)
O1bⁱ···C3b^vii	3.9 (2)	C10bⁱ···C10cⁱⁱ	4.4 (2)
C4a···C7a	3.9 (3)	O1bⁱ···C1cⁱⁱ	4.40 (17)
O1bⁱ···O2b^iv	3.89 (12)	C6aⁱ···C6b^vi	4.4 (2)
C1bⁱ···C2cⁱⁱ	3.9 (2)	C5aⁱ···C7b^vii	4.4 (2)
C4b···O1c	3.90 (18)	C12aⁱ···C14b^vi	4.4 (2)
C1bⁱ···C2b^vii	3.9 (2)	C10b···C8c	4.41 (18)
O2aⁱ···C2aⁱⁱⁱ	3.92 (17)	C14b···C12c	4.41 (19)
C12aⁱ···C15b^vii	3.9 (2)	C7b···C2c	4.4 (2)
C2aⁱ···C3b^vi	3.9 (2)	C8b···C6c	4.4 (2)
C10aⁱ···C13b^vii	3.9 (2)	C6bⁱ···C4cⁱⁱ	4.42 (18)
C1a···O1b	4.0 (2)	C14bⁱ···C12cⁱⁱ	4.42 (19)
C1bⁱ···O2cⁱⁱ	3.95 (17)	C12bⁱ···C15bⁱⁱ	4.4 (2)
O2b···O1c	3.96 (11)	C14aⁱ···C15b^vi	4.4 (2)

O1a—C1—C2	109	C6b—C5b—C4b	112 (12)
C1—C2—O1b	112 (12)	C5b—C6b—C7b	109 (11)
C3—C2—O1b	104 (10)	C6b—C7b—C8b	112 (12)
C1—C2—C3	110 (11)	C9b—C8b—C7b	109 (13)
O1c—C3—C2	107 (10)	C8b—C9b—C10b	108 (12)
C1a—O1a—C1	121	C9b—C10b—C11b	109 (11)
O2a—C1a—O1a	121 (13)	C12b—C11b—C10b	110 (13)
O2a—C1a—C2a	119 (14)	C13b—C12b—C11b	108 (13)
O1a—C1a—C2a	118 (12)	C14b—C13b—C12b	108 (12)
C1a—C2a—C3a	107 (11)	C13b—C14b—C15b	110 (11)
C4a—C3a—C2a	103 (11)	C16b—C15b—C14b	110 (11)
C3a—C4a—C5a	112 (13)	C1c—O1c—C3	118 (11)
C4a—C5a—C6a	113 (12)	O2c—C1c—O1c	118 (14)
C5a—C6a—C7a	111 (13)	O2c—C1c—C2c	123 (11)
C8a—C7a—C6a	108 (12)	O1c—C1c—C2c	118 (13)
C7a—C8a—C9a	108 (12)	C1c—C2c—C3c	110 (12)
C8a—C9a—C10a	110 (11)	C4c—C3c—C2c	106 (11)
C11a—C10a—C9a	109 (12)	C3c—C4c—C5c	111 (11)
C12a—C11a—C10a	110 (13)	C4c—C5c—C6c	111 (13)
C11a—C12a—C13a	110 (12)	C5c—C6c—C7c	113 (13)
C12a—C13a—C14a	109 (12)	C8c—C7c—C6c	110 (11)
C1b—O1b—C2	116 (11)	C7c—C8c—C9c	107 (12)
O2b—C1b—O1b	127 (13)	C8c—C9c—C10c	109 (11)
O2b—C1b—C2b	117 (14)	C11c—C10c—C9c	110 (11)
O1b—C1b—C2b	115 (11)	C10c—C11c—C12c	109 (11)
C1b—C2b—C3b	110 (11)	C13c—C12c—C11c	109 (13)
C4b—C3b—C2b	106 (11)	C12c—C13c—C14c	108 (12)
C3b—C4b—C5b	110 (11)

O1a—C1—C2—C3	61 (14)	C2b—C3b—C4b—C5b	169 (11)
O1a—C1—C2—O1b	−54 (12)	C3b—C4b—C5b—C6b	−174 (12)
C2—C1—O1a—C1a	−175 (11)	C4b—C5b—C6b—C7b	−176 (11)
C1—C2—C3—O1c	167 (11)	C5b—C6b—C7b—C8b	−179 (12)
O1b—C2—C3—O1c	−73 (13)	C6b—C7b—C8b—C9b	180 (12)
C1—C2—O1b—C1b	−112 (15)	C7b—C8b—C9b—C10b	−176 (12)
C3—C2—O1b—C1b	129 (15)	C8b—C9b—C10b—C11b	−177 (12)
C2—C3—O1c—C1c	−173 (11)	C9b—C10b—C11b—C12b	176 (12)
C1—O1a—C1a—O2a	7 (18)	C10b—C11b—C12b—C13b	176 (12)
C1—O1a—C1a—C2a	−172	C11b—C12b—C13b—C14b	−174 (12)
O1a—C1a—C2a—C3a	−159 (11)	C12b—C13b—C14b—C15b	−180 (12)
O2a—C1a—C2a—C3a	35 (15)	C13b—C14b—C15b—C16b	−178 (12)
C1a—C2a—C3a—C4a	162 (11)	C3—O1c—C1c—O2c	10 (18)
C2a—C3a—C4a—C5a	161 (12)	C3—O1c—C1c—C2c	−157 (12)
C3a—C4a—C5a—C6a	178 (12)	O1c—C1c—C2c—C3c	−162 (12)
C4a—C5a—C6a—C7a	175 (12)	O2c—C1c—C2c—C3c	32 (19)
C5a—C6a—C7a—C8a	177 (12)	C1c—C2c—C3c—C4c	168 (11)
C6a—C7a—C8a—C9a	−173 (11)	C2c—C3c—C4c—C5c	171 (11)
C7a—C8a—C9a—C10a	−172 (11)	C3c—C4c—C5c—C6c	174 (11)
C8a—C9a—C10a—C11a	−180 (11)	C4c—C5c—C6c—C7c	−177 (11)
C9a—C10a—C11a—C12a	−180 (11)	C5c—C6c—C7c—C8c	−169 (12)
C10a—C11a—C12a—C13a	−180 (11)	C6c—C7c—C8c—C9c	−173 (11)
C11a—C12a—C13a—C14a	180 (11)	C7c—C8c—C9c—C10c	163 (11)
C2—O1b—C1b—O2b	15 (28)	C8c—C9c—C10c—C11c	−175 (11)
C2—O1b—C1b—C2b	−164 (14)	C9c—C10c—C11c—C12c	−178 (11)
O1b—C1b—C2b—C3b	58 (21)	C10c—C11c—C12c—C13c	−179 (11)
O2b—C1b—C2b—C3b	−121 (18)	C11c—C12c—C13c—C14c	179 (10)
C1b—C2b—C3b—C4b	73 (16)

Symmetry codes: (i) −x+1/2, y+1/2, z+1; (ii) −x+1/2, y+1/2, z; (iii) −x+1/2, −y+1/2, z+1/2; (iv) −x+1/2, y+1/2, z+2; (v) −x+1/2, −y+1/2, z+3/2; (vi) x, −y+1, z+3/2; (vii) x, −y+1, z+1/2; (viii) x−1/2, y+1/2, z+3/2; (ix) x−1/2, y+1/2, z+1/2.

Experimental details

	(CLC)	(MPM)
Crystal data
Chemical formula	C₃₅H₆₆O₆	C₄₇H₉₀O₆
M_r	582.91	751.23
Crystal system, space group	Orthorhombic, Iba2	Orthorhombic, Iba2
Temperature (K)	293	295
a, b, c (Å)	57.368 (1), 22.783 (1), 5.6945 (5)	76.21 (4), 22.63 (1), 5.673 (2)
V (Å³)	7442.8 (7)	9784 (8)
Z	8	8
Radiation type	Synchrotron, λ = 0.5061 Å	?, λ = 0.650515 Å
µ (mm⁻¹)	0.04	0.49
Specimen shape, size (mm)	0.8 × 0.04 × 0.01	Cylinder, ? × 1.5 mm

Data collection
Diffractometer	Siemens CCD camera diffractometer	ESRF BM16
Specimen mounting	–	Capillary
Data collection mode	–	Transmission
Data collection method	?	Continuous
Absorption correction	–	–
No. of measured, independent and observed [F > 3.50σ(F)] reflections	5706, 1642, 1642	–
R_int	0.21	–
θ values (°)	θ_max = 15.7, θ_min = 0.7	2θ_min = 2.07 2θ_max = 27.0 2θ_step = 0.003
(sin θ/λ)_max (Å⁻¹)	0.534	–

Refinement
R factors and goodness of fit	R[F² > 2σ(F²)] = 0.175, wR(F²) = 0.165, S = 1.55	R_p = 7.9, R_wp = 11.4, R_exp = ?, R_Bragg = 5.7, R(F²) = 7.4, χ² = 8.526
No. of reflections/data points	824	12637
No. of parameters	167	775
No. of restraints	145	276
H-atom treatment	Calculated and kept fixed with U = 0.1 Å²	Calculated and kept fixed
(Δ/σ)_max	0.252	?
Δρ_max, Δρ_min (e Å⁻³)	1.07, −1.20	–

Computer programs: SMART, SAINT, UnitCell, MRIA, Shake-and-Bake, Xtal CRYLSQ, PLATON, Xtal BONDLA CIFIO.

Selected geometric parameters (Å, º) for (CLC) top

C1—O1a	1.38 (3)	C4b—C5b	1.55 (2)
C1—C2	1.50 (3)	C5b—C6b	1.47 (3)
C2—O1b	1.51 (3)	C6b—C7b	1.55 (2)
C3—O1c	1.38 (3)	C7b—C8b	1.51 (3)
O1a—C1a	1.33 (3)	C8b—C9b	1.53 (2)
C1a—O2a	1.24 (4)	C9b—C10b	1.49 (3)
C1a—C2a	1.59 (3)	C10b—C11b	1.53 (2)
C2a—C3a	1.55 (3)	C11b—C12b	1.48 (3)
C3a—C4a	1.51 (2)	O1c—C1c	1.31 (3)
C4a—C5a	1.53 (3)	C1c—O2c	1.24 (4)
C5a—C6a	1.52 (2)	C1c—C2c	1.56 (3)
C6a—C7a	1.52 (3)	C2c—C3c	1.59 (2)
C7a—C8a	1.49 (2)	C3c—C4c	1.51 (3)
C8a—C9a	1.54 (4)	C4c—C5c	1.49 (2)
C9a—C10a	1.48 (2)	C5c—C6c	1.52 (3)
O1b—C1b	1.34 (3)	C6c—C7c	1.56 (2)
C1b—O2b	1.20 (4)	C7c—C8c	1.50 (3)
C1b—C2b	1.53 (3)	C8c—C9c	1.54 (3)
C2b—C3b	1.56 (2)	C9c—C10c	1.44 (3)
C3b—C4b	1.53 (3)

O1a—C1—C2	107.8 (13)	C4b—C3b—C2b	105.4 (11)
O1b—C2—C1	112.0 (16)	C3b—C4b—C5b	110.3 (11)
O1b—C2—C3	103.5 (15)	C6b—C5b—C4b	110.5 (10)
C1—C2—C3	110.3 (15)	C5b—C6b—C7b	109.2 (10)
O1c—C3—C2	107.1 (15)	C8b—C7b—C6b	112.4 (11)
C1a—O1a—C1	119 (2)	C7b—C8b—C9b	110.6 (11)
O2a—C1a—O1a	120 (2)	C10b—C9b—C8b	110.0 (11)
O2a—C1a—C2a	121.4 (18)	C9b—C10b—C11b	108.8 (11)
O1a—C1a—C2a	118 (2)	C12b—C11b—C10b	106.3 (10)
C3a—C2a—C1a	106.0 (11)	C1c—O1c—C3	116.3 (18)
C4a—C3a—C2a	104.5 (10)	O2c—C1c—O1c	120 (2)
C3a—C4a—C5a	111.3 (11)	O2c—C1c—C2c	122 (2)
C6a—C5a—C4a	112.4 (11)	O1c—C1c—C2c	117 (2)
C5a—C6a—C7a	110.7 (11)	C1c—C2c—C3c	108.9 (13)
C8a—C7a—C6a	110.4 (11)	C4c—C3c—C2c	105.5 (10)
C7a—C8a—C9a	109.5 (11)	C5c—C4c—C3c	110.5 (11)
C10a—C9a—C8a	107.3 (8)	C4c—C5c—C6c	110.5 (11)
C1b—O1b—C2	115.7 (19)	C5c—C6c—C7c	111.2 (11)
O2b—C1b—O1b	126 (2)	C8c—C7c—C6c	109.6 (11)
O2b—C1b—C2b	120 (2)	C7c—C8c—C9c	108.2 (11)
O1b—C1b—C2b	114 (2)	C10c—C9c—C8c	105.9 (11)
C1b—C2b—C3b	110.8 (15)

Selected geometric parameters (Å, º) for (MPM) top

C1—O1a	1.41 (17)	C5b—C6b	1.5 (2)
C1—C2	1.5 (2)	C6b—C7b	1.5 (2)
C2—C3	1.50 (17)	C7b—C8b	1.5 (2)
C2—O1b	1.52 (16)	C8b—C9b	1.5 (2)
C3—O1c	1.3 (2)	C9b—C10b	1.5 (3)
O1a—C1a	1.3 (2)	C10b—C11b	1.5 (2)
C1a—O2a	1.25 (15)	C11b—C12b	1.5 (2)
C1a—C2a	1.6 (2)	C12b—C13b	1.5 (2)
C2a—C3a	1.6 (3)	C13b—C14b	1.5 (3)
C3a—C4a	1.5 (2)	C14b—C15b	1.56 (19)
C4a—C5a	1.5 (3)	C15b—C16b	1.5 (2)
C5a—C6a	1.5 (2)	O1c—C1c	1.33 (15)
C6a—C7a	1.5 (3)	C1c—O2c	1.25 (17)
C7a—C8a	1.5 (2)	C1c—C2c	1.5 (2)
C8a—C9a	1.5 (2)	C2c—C3c	1.6 (2)
C9a—C10a	1.5 (2)	C3c—C4c	1.5 (3)
C10a—C11a	1.5 (2)	C4c—C5c	1.5 (2)
C11a—C12a	1.5 (2)	C5c—C6c	1.5 (2)
C12a—C13a	1.5 (3)	C6c—C7c	1.6 (2)
C13a—C14a	1.5 (2)	C7c—C8c	1.5 (3)
O1b—C1b	1.35 (19)	C8c—C9c	1.53 (18)
C1b—O2b	1.20 (17)	C9c—C10c	1.5 (2)
C1b—C2b	1.5 (2)	C10c—C11c	1.53 (19)
C2b—C3b	1.6 (2)	C11c—C12c	1.5 (3)
C3b—C4b	1.5 (3)	C12c—C13c	1.5 (2)
C4b—C5b	1.6 (2)	C13c—C14c	1.6 (3)

O1a—C1—C2	109	C6b—C5b—C4b	112 (12)
C1—C2—O1b	112 (12)	C5b—C6b—C7b	109 (11)
C3—C2—O1b	104 (10)	C6b—C7b—C8b	112 (12)
C1—C2—C3	110 (11)	C9b—C8b—C7b	109 (13)
O1c—C3—C2	107 (10)	C8b—C9b—C10b	108 (12)
C1a—O1a—C1	121	C9b—C10b—C11b	109 (11)
O2a—C1a—O1a	121 (13)	C12b—C11b—C10b	110 (13)
O2a—C1a—C2a	119 (14)	C13b—C12b—C11b	108 (13)
O1a—C1a—C2a	118 (12)	C14b—C13b—C12b	108 (12)
C1a—C2a—C3a	107 (11)	C13b—C14b—C15b	110 (11)
C4a—C3a—C2a	103 (11)	C16b—C15b—C14b	110 (11)
C3a—C4a—C5a	112 (13)	C1c—O1c—C3	118 (11)
C4a—C5a—C6a	113 (12)	O2c—C1c—O1c	118 (14)
C5a—C6a—C7a	111 (13)	O2c—C1c—C2c	123 (11)
C8a—C7a—C6a	108 (12)	O1c—C1c—C2c	118 (13)
C7a—C8a—C9a	108 (12)	C1c—C2c—C3c	110 (12)
C8a—C9a—C10a	110 (11)	C4c—C3c—C2c	106 (11)
C11a—C10a—C9a	109 (12)	C3c—C4c—C5c	111 (11)
C12a—C11a—C10a	110 (13)	C4c—C5c—C6c	111 (13)
C11a—C12a—C13a	110 (12)	C5c—C6c—C7c	113 (13)
C12a—C13a—C14a	109 (12)	C8c—C7c—C6c	110 (11)
C1b—O1b—C2	116 (11)	C7c—C8c—C9c	107 (12)
O2b—C1b—O1b	127 (13)	C8c—C9c—C10c	109 (11)
O2b—C1b—C2b	117 (14)	C11c—C10c—C9c	110 (11)
O1b—C1b—C2b	115 (11)	C10c—C11c—C12c	109 (11)
C1b—C2b—C3b	110 (11)	C13c—C12c—C11c	109 (13)
C4b—C3b—C2b	106 (11)	C12c—C13c—C14c	108 (12)
C3b—C4b—C5b	110 (11)

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