Crystal structure of bis­[tetra­kis­(tetra­hydro­furan-κO)lithium] bis[μ-2,2′,2′′-methanetriyltris(4,6-di-tert-butylphenolato)-κ4O,O′:O′,O′′]­dimagnesiate

Zhou, H.; Wang, L.

doi:10.1107/S2056989017008337

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ISSN: 2056-9890

Volume 73| Part 7| July 2017| Pages 1026-1028

https://doi.org/10.1107/S2056989017008337

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Crystal structure of bis[tetrakis(tetrahydrofuran-κO)lithium] bis[μ-2,2′,2′′-methanetriyltris(4,6-di-tert-butylphenolato)-κ⁴O,O′:O′,O′′]dimagnesiate

Hongyan Zhou ^a ^* and Lei Wang ^b

^aCollege of Science, Gansu Agricultural University, Lanzhou 730070, People's Republic of China, and ^bCollege of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070, People's Republic of China
^*Correspondence e-mail: zhouhy@gsau.edu.cn

Edited by G. Smith, Queensland University of Technology, Australia (Received 18 May 2017; accepted 6 June 2017; online 13 June 2017)

The title ion-association metal complex, [Li(C₄H₈O)₄]₂[Mg₂(C₄₃H₆₁O₃)₂], has been synthesized from the tridentate phenolic ligand tris(3,5-di-tert-butyl-2-hydroxyphenyl)methane in tetrahydrofuran (THF). The aryloxo magnesiate complex anion is binuclear with each Mg₂O₄ complex unit inversion-related and bridged through the two tridentate chelating phenolate O-donors of the ligand. The complex centres have a distorted tetrahedral stereochemistry [Mg—O range 1.8796 (17)–2.0005 (16) Å] and an Mg⋯Mg separation of 2.9430 (14) Å]. The LiO₄ coodination sphere of the cation comprises four THF O-donor atoms and has a slightly distorted tetrahedral conformation [Li—O range 1.899 (5)– 1.953 (5) Å]. In the crystal, a number of stabilizing intra-anion C—H⋯O hydrogen-bonding interactions are present but no inter-species associations are found.

Keywords: crystal structure; lithium; magnesiate; heterobimetallic complex.

CCDC reference: 1554461

1. Chemical context

Magnesium complexes (Wang et al., 2014 ) and lithium complexes (Ko & Lin, 2001 ) display a vigorous catalytic activity in the synthesis of biodegradable polymers, through ring-opening polymerization. Heterobimetallic compounds, also called `ate' complexes (Mulvey, 2009 ), have been systematically studied with a focus both on the elucidation of the solid-state structures and on the catalytic applications (Qiu et al., 2013 ). We have synthesized the title metal complex, 2{[Li(THF)₄]⁺}·[Mg₂(C₄₃H₆₁O₃)₂]²⁻ from the reaction of the tridentate phenolic ligand tris(3,5-di-tert-butyl-2-hydroxyphenyl)methane with n-butyl-lithium and diethyl magnesium in tetrahydrofuran (THF). The structure of this novel heterobimetallic complex, in an ion-association mode, is reported herein.

2. Structural commentary

In the title complex ion-association compound (Fig. 1), the binuclear aryloxo magnesiate dianionic Mg₂O₆ complex core is centrosymmetric and is bridged through the central oxygen atoms (O1 and O1ⁱ) of the two chelating phenolate groups [symmetry code: (i) −x + 1, −y + 2, −z + 1]. The stereochemistry about each four-coordinated Mg atom is distorted tetrahedral with Mg—O(Ar) in the range 1.8796 (17)–2.0005 (16) Å (Table 1). The dihedral angle between two planes comprising O1/Mg1/O1′ and O1/Mg1′/O1′ is 0.05 (5)°, suggesting these four atoms are almost coplanar. The Mg⋯Mg separation in the bimetallic complex is 2.9430 (14) Å. The LiO₄ unit of the counter-ion is composed of a Li⁺ cation coordinated by four O-atom donors of the THF ligand molecules, displaying a distorted tetrahedral stereochemistry [Li—O range 1.899 (5)– 1.953 (5) Å. Within the binuclear complex anion there are six stabilizing intra-ion methyl C—H⋯O hydrogen-bonding interactions (Table 2), two of which are between the inversion-related ligands involving methyl group H-atom donors with a common phenolic O-atom acceptor [C42—H⋯O2ⁱ and C43—H⋯O2ⁱ]. The absence of inter-species C—H⋯O interactions results in discrete cations and anions in the crystal packing (Fig. 2).

Table 1
Selected bond lengths (Å)

Li1—O6	1.899 (5)	Mg1—O3	1.8796 (17)
Li1—O5	1.918 (4)	Mg1—O2	1.8810 (15)
Li1—O4	1.951 (5)	Mg1—O1	1.9844 (16)
Li1—O7	1.953 (5)	Mg1—O1ⁱ	2.0005 (16)
Symmetry code: (i) -x+1, -y+2, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C36A—H36C⋯O3	0.96	2.30	2.935 (3)	123
C39—H39C⋯O1	0.96	2.41	3.030 (3)	122
C40—H40C⋯O1	0.96	2.40	3.025 (3)	122
C42—H42B⋯O2ⁱ	0.96	2.28	2.953 (3)	126
C43—H43B⋯O2ⁱ	0.96	2.48	3.091 (3)	122
C49—H49A⋯O3	0.96	2.47	3.094 (3)	122
Symmetry code: (i) -x+1, -y+2, -z+1.

Figure 1
Molecular structure of the title compound with displacement ellipsoids given at the 40% probability level. All of the hydrogen atoms are omitted for clarity. The non-labelled atoms of one of the two cations and the binuclear anion are generated by the symmetry operation −x + 1, −y + 2, −z + 1.

Figure 2
Molecular packing of the title compound in the unit cell viewed along the a axis.

3. Database survey

A search of the Cambridge Structural Database (Groom et al., 2016 ) revealed 39 structures of complexes having the ligand derived from tris(3,5-di-tert-butyl-2-hydroxyphenyl)methane. These include cage-like monometallic alkali complexes (Dinger & Scott, 2000 ) and an aluminum metal complex in an ion-association mode (Oishi et al., 2016 ). In addition, a zinc complex based on the same ligand has been found to be useful for polymerization of cyclohexene oxide and carbon dioxide (Dinger & Scott, 2001 ).

4. Synthesis and crystallization

A solution of tris(3,5-di-tert-butyl-2-hydroxyphenyl)methane (0.63 g, 1.0 mmol) and ⁿBuLi (0.5 mL, 1.2 mmol, 2.4 M in hexane) was stirred in THF (20 mL) at 273 K under an N₂ atmosphere for 2 h. MgEt₂ (1.1 mL, 1.1 mmol, 1.0 M in hexane) was gently added to the solution. After stirring at 298 K for 6 h, the solution was filtered through celite. The filtrate was concentrated to ca 10 mL and cooled to 273 K to furnish colourless crystals, suitable for the X-ray analysis. Yield: 0.46 g (49%).

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3. Hydrogen atoms were included in the refinement at calculated positions and were allowed to ride with C—H = 0.93–0.98 Å and with U_iso = 1.2U_eq(C), or 1.5U_eq(methyl C).

Table 3
Experimental details

Crystal data
Chemical formula	[Li(C₄H₈O)₄]₂[Mg₂(C₄₃H₆₁O₃)₂]
M_r	1891.17
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	13.6185 (4), 22.6439 (18), 18.5341 (6)
β (°)	90.811 (3)
V (Å³)	5714.9 (5)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	0.08
Crystal size (mm)	0.40 × 0.21 × 0.19

Data collection
Diffractometer	Bruker SMART 1000
No. of measured, independent and observed [I > 2σ(I)] reflections	26088, 10054, 6836
R_int	0.058
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.059, 0.149, 1.05
No. of reflections	10054
No. of parameters	631
No. of restraints	1230
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.43, −0.29
Computer programs: SMART and SAINT (Bruker, 2004 ), SHELXS97, SHELXL97 and SHELXTL (Sheldrick, 2008 ) and publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 1554461

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2056989017008337/zs2380sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989017008337/zs2380Isup2.hkl

checkCIF report

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Bis[tetrakis(tetrahydrofuran-κO)lithium] bis[µ-2,2',2''-methanetriyltris(4,6-di-tert-butylphenolato)-κ⁴O,O':O',O'']dimagnesiate top

Crystal data top

[Li(C₄H₈O)₄][Mg₂(C₄₃H₆₁O₃)₂]	F(000) = 2072
M_r = 1891.17	D_x = 1.099 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 10054 reflections
a = 13.6185 (4) Å	θ = 2.5–26.7°
b = 22.6439 (18) Å	µ = 0.08 mm⁻¹
c = 18.5341 (6) Å	T = 293 K
β = 90.811 (3)°	Block, colorless
V = 5714.9 (5) Å³	0.40 × 0.21 × 0.19 mm
Z = 2

Data collection top

Bruker SMART 1000 diffractometer	6836 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.058
Graphite monochromator	θ_max = 25.0°, θ_min = 3.0°
phi and ω scans	h = −16→16
26088 measured reflections	k = −26→25
10054 independent reflections	l = −22→22

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.059	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.149	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0528P)² + 0.9025P] where P = (F_o² + 2F_c²)/3
10054 reflections	(Δ/σ)_max = 0.001
631 parameters	Δρ_max = 0.43 e Å⁻³
1230 restraints	Δρ_min = −0.29 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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

	x	y	z	U_iso*/U_eq
C1	0.44853 (15)	0.87990 (10)	0.57566 (10)	0.0143 (5)
C2	0.39975 (16)	0.90539 (10)	0.51568 (11)	0.0159 (5)
C3	0.62990 (16)	0.86092 (10)	0.58242 (11)	0.0160 (5)
C4	0.48446 (16)	0.97550 (10)	0.69623 (11)	0.0162 (5)
C5	0.55041 (16)	0.92857 (10)	0.67975 (10)	0.0159 (5)
C6	0.31307 (16)	0.88020 (10)	0.48672 (11)	0.0162 (5)
C7	0.68412 (16)	0.87114 (10)	0.51879 (11)	0.0163 (5)
C8	0.54795 (15)	0.90425 (10)	0.60218 (11)	0.0151 (5)
H8	0.5595	0.9389	0.5717	0.018*
C9	0.40800 (16)	0.82942 (10)	0.60705 (11)	0.0179 (5)
H9	0.4389	0.8130	0.6474	0.022*
C10	0.62079 (16)	0.91223 (11)	0.73083 (11)	0.0196 (5)
H10	0.6669	0.8838	0.7185	0.024*
C11	0.26051 (17)	0.90666 (11)	0.42000 (11)	0.0213 (5)
C12	0.64954 (17)	0.81067 (11)	0.62311 (11)	0.0198 (5)
H12	0.6101	0.8029	0.6625	0.024*
C13	0.83216 (16)	0.84588 (11)	0.43869 (12)	0.0206 (5)
C14	0.27818 (16)	0.82944 (10)	0.52025 (11)	0.0186 (5)
H14	0.2213	0.8121	0.5016	0.022*
C15	0.32317 (17)	0.80296 (10)	0.58002 (11)	0.0198 (5)
C16	0.76638 (16)	0.83422 (10)	0.50446 (11)	0.0183 (5)
C17	0.72462 (17)	0.77159 (11)	0.60822 (11)	0.0207 (5)
C18	0.41599 (17)	1.05073 (11)	0.78728 (11)	0.0225 (6)
C19	0.48607 (16)	0.99987 (10)	0.76694 (11)	0.0184 (5)
C20	0.78393 (16)	0.78616 (11)	0.54998 (11)	0.0209 (5)
H20	0.8382	0.7625	0.5410	0.025*
C21	0.27898 (18)	0.74571 (11)	0.61067 (12)	0.0229 (5)
C22	0.62541 (16)	0.93650 (11)	0.79964 (12)	0.0228 (6)
C23	0.55636 (17)	0.97928 (11)	0.81606 (12)	0.0222 (5)
H23	0.5571	0.9951	0.8624	0.027*
C24	0.74578 (18)	0.71642 (11)	0.65421 (12)	0.0254 (6)
C25	0.5483 (2)	0.57398 (15)	0.10178 (15)	0.0507 (9)
H25A	0.5606	0.6024	0.0638	0.061*
H25B	0.5452	0.5348	0.0808	0.061*
C26	0.8408 (2)	0.72517 (15)	0.69722 (16)	0.0547 (9)
H26A	0.8543	0.6905	0.7254	0.082*
H26B	0.8341	0.7586	0.7287	0.082*
H26C	0.8938	0.7320	0.6647	0.082*
C27	0.5095 (3)	0.44057 (17)	0.3707 (2)	0.0841 (13)
H27A	0.4457	0.4496	0.3906	0.101*
H27B	0.5076	0.4013	0.3498	0.101*
C28	0.5386 (2)	0.48648 (15)	0.31469 (18)	0.0539 (9)
H28A	0.5856	0.4703	0.2811	0.065*
H28B	0.4816	0.5007	0.2879	0.065*
C29	0.5060 (2)	0.76988 (14)	0.40393 (15)	0.0487 (8)
H29A	0.5357	0.8088	0.4045	0.058*
H29B	0.4351	0.7740	0.4022	0.058*
C30	0.7192 (3)	0.85111 (16)	0.85394 (17)	0.0687 (11)
H30A	0.7708	0.8405	0.8873	0.103*
H30B	0.7354	0.8375	0.8065	0.103*
H30C	0.6588	0.8332	0.8686	0.103*
C31	0.6866 (2)	0.93678 (18)	0.93004 (14)	0.0644 (11)
H31A	0.7387	0.9232	0.9613	0.097*
H31B	0.6256	0.9198	0.9449	0.097*
H31C	0.6824	0.9790	0.9327	0.097*
C32	0.8032 (2)	0.94579 (19)	0.82828 (18)	0.0698 (12)
H32A	0.7976	0.9880	0.8293	0.105*
H32B	0.8167	0.9331	0.7800	0.105*
H32C	0.8557	0.9336	0.8600	0.105*
C33	0.7558 (3)	0.66158 (13)	0.60625 (16)	0.0566 (9)
H33A	0.8119	0.6660	0.5759	0.085*
H33B	0.6977	0.6572	0.5768	0.085*
H33C	0.7640	0.6272	0.6361	0.085*
C34	0.5872 (3)	0.44511 (17)	0.4264 (2)	0.0826 (12)
H34A	0.6401	0.4177	0.4165	0.099*
H34B	0.5613	0.4365	0.4737	0.099*
C35	0.6222 (3)	0.50667 (15)	0.42268 (17)	0.0626 (10)
H35A	0.6005	0.5287	0.4644	0.075*
H35B	0.6934	0.5076	0.4218	0.075*
C36A	0.86788 (18)	0.90987 (11)	0.43636 (13)	0.0279 (6)
H36A	0.9112	0.9149	0.3964	0.042*
H36B	0.9023	0.9191	0.4805	0.042*
H36C	0.8125	0.9358	0.4307	0.042*
C37	0.17009 (18)	0.87032 (12)	0.39790 (13)	0.0315 (6)
H37A	0.1250	0.8691	0.4372	0.047*
H37B	0.1900	0.8309	0.3860	0.047*
H37C	0.1387	0.8882	0.3567	0.047*
C38	0.92361 (17)	0.80626 (12)	0.43914 (13)	0.0303 (6)
H38A	0.9628	0.8152	0.3979	0.045*
H38B	0.9038	0.7656	0.4374	0.045*
H38C	0.9614	0.8132	0.4824	0.045*
C39	0.22469 (19)	0.96932 (12)	0.43508 (13)	0.0309 (6)
H39A	0.1820	0.9689	0.4759	0.046*
H39B	0.1895	0.9840	0.3936	0.046*
H39C	0.2800	0.9944	0.4452	0.046*
C40	0.32951 (18)	0.90733 (12)	0.35515 (11)	0.0288 (6)
H40A	0.2946	0.9216	0.3133	0.043*
H40B	0.3528	0.8680	0.3462	0.043*
H40C	0.3843	0.9328	0.3654	0.043*
C41	0.70742 (18)	0.91836 (13)	0.85285 (12)	0.0318 (6)
C42	0.30853 (18)	1.03454 (12)	0.77105 (13)	0.0305 (6)
H42A	0.2898	1.0017	0.8006	0.046*
H42B	0.3013	1.0240	0.7211	0.046*
H42C	0.2673	1.0678	0.7813	0.046*
C43	0.44292 (19)	1.10648 (11)	0.74497 (13)	0.0289 (6)
H43A	0.4003	1.1382	0.7585	0.043*
H43B	0.4355	1.0990	0.6942	0.043*
H43C	0.5098	1.1171	0.7557	0.043*
C44I	0.2683 (2)	0.69991 (12)	0.54984 (14)	0.0363 (7)
H44A	0.3315	0.6922	0.5296	0.054*
H44B	0.2248	0.7150	0.5130	0.054*
H44C	0.2419	0.6640	0.5690	0.054*
C45	0.17617 (19)	0.75797 (12)	0.64056 (14)	0.0369 (7)
H45A	0.1481	0.7218	0.6577	0.055*
H45B	0.1350	0.7741	0.6030	0.055*
H45C	0.1813	0.7857	0.6797	0.055*
C46	0.82584 (19)	0.63296 (13)	0.28622 (13)	0.0348 (7)
H46A	0.8015	0.6598	0.2494	0.042*
H46B	0.8432	0.5959	0.2635	0.042*
C47	0.3430 (2)	0.71873 (12)	0.67013 (14)	0.0372 (7)
H47A	0.4069	0.7102	0.6516	0.056*
H47B	0.3133	0.6829	0.6868	0.056*
H47C	0.3490	0.7461	0.7095	0.056*
C48	0.4233 (2)	1.06616 (13)	0.86792 (13)	0.0409 (7)
H48A	0.4885	1.0798	0.8793	0.061*
H48B	0.4092	1.0317	0.8961	0.061*
H48C	0.3768	1.0966	0.8788	0.061*
C49	0.77385 (19)	0.83204 (13)	0.36928 (12)	0.0340 (7)
H49A	0.7155	0.8558	0.3674	0.051*
H49B	0.7560	0.7910	0.3688	0.051*
H49C	0.8135	0.8406	0.3282	0.051*
C50	0.5239 (2)	0.67180 (13)	0.44191 (13)	0.0375 (7)
H50A	0.5682	0.6451	0.4671	0.045*
H50B	0.4569	0.6590	0.4498	0.045*
C51	0.5422 (2)	0.73363 (12)	0.34117 (14)	0.0411 (7)
H51A	0.4982	0.7376	0.2999	0.049*
H51B	0.6073	0.7464	0.3273	0.049*
C52	0.48956 (19)	0.63168 (13)	0.19563 (14)	0.0364 (7)
H52A	0.4942	0.6710	0.1752	0.044*
H52B	0.4452	0.6328	0.2361	0.044*
C53	0.6279 (2)	0.57714 (13)	0.15967 (13)	0.0387 (7)
H53A	0.6464	0.5378	0.1757	0.046*
H53B	0.6858	0.5969	0.1416	0.046*
C54	0.91390 (19)	0.65918 (13)	0.32510 (13)	0.0382 (7)
H54A	0.9117	0.7020	0.3246	0.046*
H54B	0.9748	0.6460	0.3039	0.046*
C55	0.9026 (2)	0.63515 (14)	0.40088 (14)	0.0399 (7)
H55A	0.9274	0.5951	0.4047	0.048*
H55B	0.9363	0.6598	0.4361	0.048*
C56	0.7932 (2)	0.63710 (14)	0.41053 (13)	0.0420 (7)
H56A	0.7729	0.6082	0.4459	0.050*
H56B	0.7726	0.6760	0.4262	0.050*
C57	0.6634 (2)	0.70310 (14)	0.70703 (16)	0.0491 (8)
H57A	0.6778	0.6671	0.7323	0.074*
H57B	0.6024	0.6990	0.6809	0.074*
H57C	0.6582	0.7349	0.7410	0.074*
C58	0.5385 (2)	0.73428 (13)	0.46798 (14)	0.0416 (7)
H58A	0.4984	0.7426	0.5096	0.050*
H58B	0.6069	0.7418	0.4802	0.050*
C59	0.4546 (2)	0.58831 (14)	0.13988 (14)	0.0439 (8)
H59A	0.4065	0.6059	0.1073	0.053*
H59B	0.4264	0.5535	0.1620	0.053*
Li1	0.6174 (3)	0.6098 (2)	0.3193 (2)	0.0323 (10)
Mg1	0.56849 (5)	0.97310 (3)	0.44884 (4)	0.01547 (18)
O1	0.43576 (10)	0.95620 (7)	0.48655 (7)	0.0154 (3)
O2	0.57524 (11)	1.00281 (7)	0.35426 (7)	0.0184 (4)
O3	0.65886 (11)	0.91317 (7)	0.47250 (7)	0.0196 (4)
O4	0.54464 (13)	0.67304 (8)	0.36606 (8)	0.0329 (4)
O5	0.58526 (12)	0.61056 (8)	0.21824 (8)	0.0330 (5)
O6	0.75222 (13)	0.62355 (9)	0.34078 (9)	0.0417 (5)
O7	0.58148 (15)	0.53233 (9)	0.35698 (10)	0.0454 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0177 (12)	0.0123 (12)	0.0129 (10)	0.0016 (10)	0.0023 (9)	−0.0013 (9)
C2	0.0188 (12)	0.0125 (12)	0.0165 (11)	−0.0014 (10)	0.0055 (9)	−0.0031 (9)
C3	0.0156 (11)	0.0181 (13)	0.0142 (11)	−0.0009 (10)	−0.0022 (9)	−0.0022 (9)
C4	0.0177 (12)	0.0147 (13)	0.0163 (11)	−0.0035 (10)	0.0029 (9)	0.0040 (9)
C5	0.0163 (11)	0.0187 (13)	0.0129 (11)	−0.0052 (10)	0.0023 (9)	0.0021 (9)
C6	0.0154 (12)	0.0174 (13)	0.0156 (11)	0.0001 (10)	0.0015 (9)	−0.0041 (9)
C7	0.0165 (12)	0.0149 (13)	0.0173 (11)	−0.0012 (10)	−0.0021 (9)	−0.0007 (9)
C8	0.0158 (11)	0.0148 (12)	0.0147 (11)	−0.0005 (10)	0.0018 (9)	0.0028 (9)
C9	0.0212 (12)	0.0167 (13)	0.0160 (11)	0.0033 (10)	0.0048 (9)	0.0005 (9)
C10	0.0191 (12)	0.0218 (14)	0.0180 (11)	0.0011 (11)	0.0027 (9)	0.0003 (10)
C11	0.0216 (13)	0.0231 (14)	0.0192 (12)	−0.0039 (11)	−0.0037 (10)	−0.0010 (10)
C12	0.0222 (12)	0.0200 (13)	0.0174 (11)	0.0010 (11)	0.0005 (9)	0.0013 (10)
C13	0.0156 (12)	0.0236 (14)	0.0226 (12)	0.0013 (11)	0.0017 (9)	−0.0006 (10)
C14	0.0178 (12)	0.0175 (13)	0.0206 (12)	−0.0057 (10)	0.0041 (9)	−0.0033 (10)
C15	0.0240 (13)	0.0136 (13)	0.0219 (12)	−0.0008 (11)	0.0084 (10)	−0.0012 (10)
C16	0.0146 (12)	0.0203 (13)	0.0200 (11)	−0.0007 (10)	−0.0022 (9)	−0.0031 (10)
C17	0.0218 (12)	0.0183 (13)	0.0220 (12)	0.0014 (11)	−0.0040 (10)	−0.0002 (10)
C18	0.0256 (13)	0.0229 (14)	0.0191 (12)	0.0023 (11)	0.0035 (10)	−0.0038 (10)
C19	0.0186 (12)	0.0180 (13)	0.0186 (11)	−0.0026 (10)	0.0041 (9)	−0.0002 (10)
C20	0.0160 (12)	0.0199 (14)	0.0268 (12)	0.0066 (10)	−0.0023 (10)	−0.0016 (10)
C21	0.0274 (13)	0.0151 (13)	0.0265 (13)	−0.0030 (11)	0.0073 (10)	0.0015 (10)
C22	0.0178 (12)	0.0292 (15)	0.0213 (12)	−0.0025 (11)	−0.0015 (10)	−0.0001 (11)
C23	0.0236 (13)	0.0278 (15)	0.0151 (11)	−0.0028 (11)	−0.0002 (10)	−0.0054 (10)
C24	0.0291 (14)	0.0205 (14)	0.0265 (13)	0.0027 (12)	−0.0037 (11)	0.0075 (11)
C25	0.060 (2)	0.055 (2)	0.0366 (16)	0.0127 (18)	−0.0061 (15)	−0.0125 (15)
C26	0.054 (2)	0.045 (2)	0.064 (2)	0.0029 (17)	−0.0238 (17)	0.0214 (16)
C27	0.054 (2)	0.046 (2)	0.152 (4)	−0.014 (2)	−0.010 (2)	0.041 (2)
C28	0.0352 (18)	0.041 (2)	0.086 (2)	0.0002 (16)	−0.0012 (16)	0.0051 (18)
C29	0.0508 (19)	0.0290 (18)	0.066 (2)	0.0086 (15)	−0.0055 (16)	−0.0081 (15)
C30	0.092 (3)	0.060 (3)	0.053 (2)	0.025 (2)	−0.0426 (19)	−0.0009 (18)
C31	0.059 (2)	0.105 (3)	0.0287 (16)	0.035 (2)	−0.0208 (15)	−0.0112 (17)
C32	0.0282 (17)	0.117 (4)	0.063 (2)	−0.008 (2)	−0.0183 (16)	0.018 (2)
C33	0.094 (3)	0.0279 (18)	0.0485 (18)	0.0159 (18)	0.0055 (18)	0.0082 (15)
C34	0.076 (3)	0.051 (3)	0.120 (3)	0.001 (2)	−0.001 (2)	0.031 (2)
C35	0.091 (3)	0.050 (2)	0.0477 (19)	0.003 (2)	0.0140 (18)	0.0165 (16)
C36A	0.0258 (14)	0.0279 (16)	0.0302 (13)	0.0017 (12)	0.0078 (11)	0.0027 (11)
C37	0.0283 (14)	0.0401 (18)	0.0260 (13)	−0.0109 (13)	−0.0071 (11)	0.0007 (12)
C38	0.0234 (14)	0.0280 (16)	0.0398 (15)	0.0029 (12)	0.0098 (11)	−0.0011 (12)
C39	0.0284 (14)	0.0271 (16)	0.0369 (14)	0.0056 (12)	−0.0113 (12)	0.0017 (12)
C40	0.0315 (15)	0.0369 (17)	0.0179 (12)	−0.0066 (13)	−0.0009 (11)	0.0002 (11)
C41	0.0262 (14)	0.0467 (19)	0.0222 (13)	0.0050 (13)	−0.0070 (11)	−0.0023 (12)
C42	0.0265 (14)	0.0312 (16)	0.0342 (14)	0.0035 (12)	0.0126 (11)	−0.0012 (12)
C43	0.0321 (15)	0.0232 (15)	0.0316 (14)	0.0022 (12)	0.0038 (11)	−0.0053 (11)
C44I	0.0452 (17)	0.0204 (15)	0.0435 (16)	−0.0130 (13)	0.0122 (13)	−0.0027 (12)
C45	0.0376 (16)	0.0282 (16)	0.0452 (16)	−0.0104 (13)	0.0158 (13)	0.0049 (13)
C46	0.0369 (16)	0.0327 (17)	0.0349 (15)	−0.0003 (14)	0.0078 (12)	−0.0018 (12)
C47	0.0511 (18)	0.0188 (15)	0.0419 (15)	−0.0072 (14)	0.0047 (13)	0.0091 (12)
C48	0.0540 (19)	0.0411 (19)	0.0277 (14)	0.0174 (15)	0.0047 (13)	−0.0102 (13)
C49	0.0291 (15)	0.0468 (19)	0.0261 (13)	0.0027 (14)	0.0053 (11)	−0.0078 (12)
C50	0.0405 (17)	0.0394 (18)	0.0329 (15)	−0.0023 (14)	0.0084 (12)	−0.0017 (13)
C51	0.0541 (19)	0.0289 (17)	0.0399 (16)	0.0014 (15)	−0.0140 (14)	0.0050 (13)
C52	0.0290 (15)	0.0391 (18)	0.0412 (16)	−0.0013 (14)	0.0015 (12)	−0.0039 (13)
C53	0.0445 (17)	0.0407 (18)	0.0310 (14)	0.0056 (15)	0.0044 (13)	−0.0082 (13)
C54	0.0321 (15)	0.0406 (19)	0.0421 (16)	0.0041 (14)	0.0096 (12)	−0.0037 (13)
C55	0.0415 (17)	0.0377 (18)	0.0403 (16)	0.0074 (15)	−0.0056 (13)	−0.0035 (13)
C56	0.0466 (18)	0.050 (2)	0.0297 (15)	−0.0036 (16)	0.0037 (13)	−0.0040 (13)
C57	0.054 (2)	0.0378 (19)	0.0558 (19)	0.0061 (16)	0.0092 (15)	0.0231 (15)
C58	0.0430 (17)	0.0408 (19)	0.0413 (16)	−0.0056 (15)	0.0112 (13)	−0.0141 (14)
C59	0.0417 (17)	0.053 (2)	0.0364 (16)	−0.0059 (16)	−0.0067 (13)	−0.0076 (14)
Li1	0.038 (3)	0.031 (3)	0.028 (2)	0.002 (2)	0.0028 (19)	−0.0008 (19)
Mg1	0.0166 (4)	0.0146 (4)	0.0152 (4)	0.0004 (3)	0.0006 (3)	0.0011 (3)
O1	0.0165 (8)	0.0134 (9)	0.0163 (7)	−0.0017 (7)	−0.0011 (6)	0.0025 (6)
O2	0.0194 (8)	0.0188 (9)	0.0169 (8)	0.0036 (7)	−0.0003 (6)	0.0032 (7)
O3	0.0216 (9)	0.0193 (9)	0.0179 (8)	0.0060 (7)	0.0027 (6)	0.0046 (7)
O4	0.0433 (11)	0.0266 (11)	0.0288 (9)	0.0030 (9)	0.0064 (8)	−0.0029 (8)
O5	0.0347 (11)	0.0374 (12)	0.0270 (9)	0.0024 (9)	0.0014 (8)	−0.0064 (8)
O6	0.0349 (11)	0.0592 (15)	0.0312 (10)	−0.0059 (10)	0.0063 (8)	−0.0072 (9)
O7	0.0496 (13)	0.0292 (12)	0.0576 (12)	−0.0003 (10)	0.0047 (10)	0.0115 (10)

Geometric parameters (Å, º) top

Li1—O6	1.899 (5)	C31—H31C	0.9600
Li1—O5	1.918 (4)	C32—C41	1.520 (4)
Li1—O4	1.951 (5)	C32—H32A	0.9600
Li1—O7	1.953 (5)	C32—H32B	0.9600
Mg1—O3	1.8796 (17)	C32—H32C	0.9600
Mg1—O2	1.8810 (15)	C33—H33A	0.9600
Mg1—O1	1.9844 (16)	C33—H33B	0.9600
Mg1—O1ⁱ	2.0005 (16)	C33—H33C	0.9600
C1—C9	1.400 (3)	C34—C35	1.475 (5)
C1—C2	1.410 (3)	C34—H34A	0.9700
C1—C8	1.536 (3)	C34—H34B	0.9700
C2—O1	1.365 (3)	C35—O7	1.452 (4)
C2—C6	1.410 (3)	C35—H35A	0.9700
C3—C12	1.389 (3)	C35—H35B	0.9700
C3—C7	1.419 (3)	C36A—H36A	0.9600
C3—C8	1.534 (3)	C36A—H36B	0.9600
C4—O2ⁱ	1.325 (2)	C36A—H36C	0.9600
C4—C19	1.422 (3)	C37—H37A	0.9600
C4—C5	1.427 (3)	C37—H37B	0.9600
C5—C10	1.388 (3)	C37—H37C	0.9600
C5—C8	1.540 (3)	C38—H38A	0.9600
C6—C14	1.393 (3)	C38—H38B	0.9600
C6—C11	1.541 (3)	C38—H38C	0.9600
C7—O3	1.324 (3)	C39—H39A	0.9600
C7—C16	1.426 (3)	C39—H39B	0.9600
C8—H8	0.9800	C39—H39C	0.9600
C9—C15	1.389 (3)	C40—H40A	0.9600
C9—H9	0.9300	C40—H40B	0.9600
C10—C22	1.389 (3)	C40—H40C	0.9600
C10—H10	0.9300	C42—H42A	0.9600
C11—C39	1.527 (3)	C42—H42B	0.9600
C11—C37	1.532 (3)	C42—H42C	0.9600
C11—C40	1.536 (3)	C43—H43A	0.9600
C12—C17	1.383 (3)	C43—H43B	0.9600
C12—H12	0.9300	C43—H43C	0.9600
C13—C36A	1.529 (3)	C44I—H44A	0.9600
C13—C49	1.535 (3)	C44I—H44B	0.9600
C13—C38	1.535 (3)	C44I—H44C	0.9600
C13—C16	1.546 (3)	C45—H45A	0.9600
C14—C15	1.394 (3)	C45—H45B	0.9600
C14—H14	0.9300	C45—H45C	0.9600
C15—C21	1.541 (3)	C46—O6	1.450 (3)
C16—C20	1.396 (3)	C46—C54	1.512 (4)
C17—C20	1.397 (3)	C46—H46A	0.9700
C17—C24	1.537 (3)	C46—H46B	0.9700
C18—C43	1.533 (3)	C47—H47A	0.9600
C18—C42	1.534 (3)	C47—H47B	0.9600
C18—C48	1.537 (3)	C47—H47C	0.9600
C18—C19	1.546 (3)	C48—H48A	0.9600
C19—C23	1.392 (3)	C48—H48B	0.9600
C20—H20	0.9300	C48—H48C	0.9600
C21—C47	1.523 (3)	C49—H49A	0.9600
C21—C44I	1.537 (3)	C49—H49B	0.9600
C21—C45	1.538 (3)	C49—H49C	0.9600
C22—C23	1.387 (3)	C50—O4	1.438 (3)
C22—C41	1.535 (3)	C50—C58	1.507 (4)
C23—H23	0.9300	C50—H50A	0.9700
C24—C26	1.523 (4)	C50—H50B	0.9700
C24—C57	1.530 (4)	C51—O4	1.448 (3)
C24—C33	1.534 (4)	C51—H51A	0.9700
C25—C59	1.503 (4)	C51—H51B	0.9700
C25—C53	1.516 (4)	C52—O5	1.445 (3)
C25—H25A	0.9700	C52—C59	1.499 (4)
C25—H25B	0.9700	C52—H52A	0.9700
C26—H26A	0.9600	C52—H52B	0.9700
C26—H26B	0.9600	C53—O5	1.451 (3)
C26—H26C	0.9600	C53—H53A	0.9700
C27—C34	1.471 (5)	C53—H53B	0.9700
C27—C28	1.526 (4)	C54—C55	1.516 (4)
C27—H27A	0.9700	C54—H54A	0.9700
C27—H27B	0.9700	C54—H54B	0.9700
C28—O7	1.421 (4)	C55—C56	1.503 (4)
C28—H28A	0.9700	C55—H55A	0.9700
C28—H28B	0.9700	C55—H55B	0.9700
C29—C58	1.497 (4)	C56—O6	1.434 (3)
C29—C51	1.512 (4)	C56—H56A	0.9700
C29—H29A	0.9700	C56—H56B	0.9700
C29—H29B	0.9700	C57—H57A	0.9600
C30—C41	1.531 (4)	C57—H57B	0.9600
C30—H30A	0.9600	C57—H57C	0.9600
C30—H30B	0.9600	C58—H58A	0.9700
C30—H30C	0.9600	C58—H58B	0.9700
C31—C41	1.521 (3)	C59—H59A	0.9700
C31—H31A	0.9600	C59—H59B	0.9700
C31—H31B	0.9600	O2—C4ⁱ	1.325 (2)

O6—Li1—O5	114.2 (2)	C27—C34—H34A	110.7
O6—Li1—O4	106.4 (2)	C35—C34—H34A	110.7
O5—Li1—O4	108.5 (2)	C27—C34—H34B	110.7
O6—Li1—O7	108.6 (2)	C35—C34—H34B	110.7
O5—Li1—O7	107.6 (2)	H34A—C34—H34B	108.8
O4—Li1—O7	111.7 (2)	O7—C35—C34	107.3 (3)
O3—Mg1—O2	115.80 (7)	O7—C35—H35A	110.3
O3—Mg1—O1	112.04 (7)	C34—C35—H35A	110.3
O2—Mg1—O1	116.99 (7)	O7—C35—H35B	110.3
O3—Mg1—O1ⁱ	117.55 (7)	C34—C35—H35B	110.3
O2—Mg1—O1ⁱ	105.89 (7)	H35A—C35—H35B	108.5
O1—Mg1—O1ⁱ	84.79 (7)	C13—C36A—H36A	109.5
Mg1—O1—Mg1ⁱ	95.21 (7)	C13—C36A—H36B	109.5
C4ⁱ—O2—Mg1	138.86 (14)	H36A—C36A—H36B	109.5
C7—O3—Mg1	146.48 (14)	C13—C36A—H36C	109.5
C9—C1—C2	118.5 (2)	H36A—C36A—H36C	109.5
C9—C1—C8	120.74 (19)	H36B—C36A—H36C	109.5
C2—C1—C8	120.56 (19)	C11—C37—H37A	109.5
O1—C2—C6	119.60 (19)	C11—C37—H37B	109.5
O1—C2—C1	119.27 (19)	H37A—C37—H37B	109.5
C6—C2—C1	121.1 (2)	C11—C37—H37C	109.5
C12—C3—C7	119.1 (2)	H37A—C37—H37C	109.5
C12—C3—C8	122.0 (2)	H37B—C37—H37C	109.5
C7—C3—C8	118.87 (19)	C13—C38—H38A	109.5
O2ⁱ—C4—C19	120.6 (2)	C13—C38—H38B	109.5
O2ⁱ—C4—C5	120.42 (18)	H38A—C38—H38B	109.5
C19—C4—C5	118.99 (19)	C13—C38—H38C	109.5
C10—C5—C4	118.89 (19)	H38A—C38—H38C	109.5
C10—C5—C8	123.2 (2)	H38B—C38—H38C	109.5
C4—C5—C8	117.44 (18)	C11—C39—H39A	109.5
C14—C6—C2	116.9 (2)	C11—C39—H39B	109.5
C14—C6—C11	121.4 (2)	H39A—C39—H39B	109.5
C2—C6—C11	121.7 (2)	C11—C39—H39C	109.5
O3—C7—C3	121.5 (2)	H39A—C39—H39C	109.5
O3—C7—C16	119.9 (2)	H39B—C39—H39C	109.5
C3—C7—C16	118.6 (2)	C11—C40—H40A	109.5
C3—C8—C1	109.57 (18)	C11—C40—H40B	109.5
C3—C8—C5	116.45 (17)	H40A—C40—H40B	109.5
C1—C8—C5	115.76 (17)	C11—C40—H40C	109.5
C3—C8—H8	104.5	H40A—C40—H40C	109.5
C1—C8—H8	104.5	H40B—C40—H40C	109.5
C5—C8—H8	104.5	C32—C41—C31	110.0 (3)
C15—C9—C1	122.2 (2)	C32—C41—C30	108.7 (3)
C15—C9—H9	118.9	C31—C41—C30	106.3 (2)
C1—C9—H9	118.9	C32—C41—C22	108.5 (2)
C5—C10—C22	122.9 (2)	C31—C41—C22	112.8 (2)
C5—C10—H10	118.6	C30—C41—C22	110.5 (2)
C22—C10—H10	118.6	C18—C42—H42A	109.5
C39—C11—C37	106.9 (2)	C18—C42—H42B	109.5
C39—C11—C40	109.5 (2)	H42A—C42—H42B	109.5
C37—C11—C40	107.12 (18)	C18—C42—H42C	109.5
C39—C11—C6	111.12 (18)	H42A—C42—H42C	109.5
C37—C11—C6	111.6 (2)	H42B—C42—H42C	109.5
C40—C11—C6	110.45 (19)	C18—C43—H43A	109.5
C17—C12—C3	123.6 (2)	C18—C43—H43B	109.5
C17—C12—H12	118.2	H43A—C43—H43B	109.5
C3—C12—H12	118.2	C18—C43—H43C	109.5
C36A—C13—C49	109.3 (2)	H43A—C43—H43C	109.5
C36A—C13—C38	107.19 (19)	H43B—C43—H43C	109.5
C49—C13—C38	107.18 (19)	C21—C44I—H44A	109.5
C36A—C13—C16	111.86 (19)	C21—C44I—H44B	109.5
C49—C13—C16	109.11 (18)	H44A—C44I—H44B	109.5
C38—C13—C16	112.03 (19)	C21—C44I—H44C	109.5
C6—C14—C15	124.1 (2)	H44A—C44I—H44C	109.5
C6—C14—H14	118.0	H44B—C44I—H44C	109.5
C15—C14—H14	118.0	C21—C45—H45A	109.5
C9—C15—C14	117.1 (2)	C21—C45—H45B	109.5
C9—C15—C21	123.9 (2)	H45A—C45—H45B	109.5
C14—C15—C21	119.0 (2)	C21—C45—H45C	109.5
C20—C16—C7	118.2 (2)	H45A—C45—H45C	109.5
C20—C16—C13	120.9 (2)	H45B—C45—H45C	109.5
C7—C16—C13	120.8 (2)	O6—C46—C54	106.08 (19)
C12—C17—C20	116.1 (2)	O6—C46—H46A	110.5
C12—C17—C24	122.9 (2)	C54—C46—H46A	110.5
C20—C17—C24	121.0 (2)	O6—C46—H46B	110.5
C43—C18—C42	109.3 (2)	C54—C46—H46B	110.5
C43—C18—C48	107.3 (2)	H46A—C46—H46B	108.7
C42—C18—C48	107.1 (2)	C21—C47—H47A	109.5
C43—C18—C19	109.62 (19)	C21—C47—H47B	109.5
C42—C18—C19	111.4 (2)	H47A—C47—H47B	109.5
C48—C18—C19	112.0 (2)	C21—C47—H47C	109.5
C23—C19—C4	118.3 (2)	H47A—C47—H47C	109.5
C23—C19—C18	120.75 (19)	H47B—C47—H47C	109.5
C4—C19—C18	120.82 (19)	C18—C48—H48A	109.5
C16—C20—C17	123.7 (2)	C18—C48—H48B	109.5
C16—C20—H20	118.1	H48A—C48—H48B	109.5
C17—C20—H20	118.1	C18—C48—H48C	109.5
C47—C21—C44I	107.9 (2)	H48A—C48—H48C	109.5
C47—C21—C45	109.0 (2)	H48B—C48—H48C	109.5
C44I—C21—C45	108.0 (2)	C13—C49—H49A	109.5
C47—C21—C15	112.4 (2)	C13—C49—H49B	109.5
C44I—C21—C15	109.31 (19)	H49A—C49—H49B	109.5
C45—C21—C15	110.1 (2)	C13—C49—H49C	109.5
C23—C22—C10	117.1 (2)	H49A—C49—H49C	109.5
C23—C22—C41	122.4 (2)	H49B—C49—H49C	109.5
C10—C22—C41	120.5 (2)	O4—C50—C58	105.6 (2)
C22—C23—C19	123.5 (2)	O4—C50—H50A	110.6
C22—C23—H23	118.2	C58—C50—H50A	110.6
C19—C23—H23	118.2	O4—C50—H50B	110.6
C26—C24—C57	108.4 (2)	C58—C50—H50B	110.6
C26—C24—C33	109.1 (2)	H50A—C50—H50B	108.8
C57—C24—C33	106.5 (2)	O4—C51—C29	106.0 (2)
C26—C24—C17	109.6 (2)	O4—C51—H51A	110.5
C57—C24—C17	112.4 (2)	C29—C51—H51A	110.5
C33—C24—C17	110.7 (2)	O4—C51—H51B	110.5
C59—C25—C53	105.1 (2)	C29—C51—H51B	110.5
C59—C25—H25A	110.7	H51A—C51—H51B	108.7
C53—C25—H25A	110.7	O5—C52—C59	105.1 (2)
C59—C25—H25B	110.7	O5—C52—H52A	110.7
C53—C25—H25B	110.7	C59—C52—H52A	110.7
H25A—C25—H25B	108.8	O5—C52—H52B	110.7
C24—C26—H26A	109.5	C59—C52—H52B	110.7
C24—C26—H26B	109.5	H52A—C52—H52B	108.8
H26A—C26—H26B	109.5	O5—C53—C25	105.3 (2)
C24—C26—H26C	109.5	O5—C53—H53A	110.7
H26A—C26—H26C	109.5	C25—C53—H53A	110.7
H26B—C26—H26C	109.5	O5—C53—H53B	110.7
C34—C27—C28	103.8 (3)	C25—C53—H53B	110.7
C34—C27—H27A	111.0	H53A—C53—H53B	108.8
C28—C27—H27A	111.0	C46—C54—C55	102.1 (2)
C34—C27—H27B	111.0	C46—C54—H54A	111.3
C28—C27—H27B	111.0	C55—C54—H54A	111.3
H27A—C27—H27B	109.0	C46—C54—H54B	111.3
O7—C28—C27	103.4 (3)	C55—C54—H54B	111.3
O7—C28—H28A	111.1	H54A—C54—H54B	109.2
C27—C28—H28A	111.1	C56—C55—C54	102.3 (2)
O7—C28—H28B	111.1	C56—C55—H55A	111.3
C27—C28—H28B	111.1	C54—C55—H55A	111.3
H28A—C28—H28B	109.1	C56—C55—H55B	111.3
C58—C29—C51	102.8 (2)	C54—C55—H55B	111.3
C58—C29—H29A	111.2	H55A—C55—H55B	109.2
C51—C29—H29A	111.2	O6—C56—C55	105.1 (2)
C58—C29—H29B	111.2	O6—C56—H56A	110.7
C51—C29—H29B	111.2	C55—C56—H56A	110.7
H29A—C29—H29B	109.1	O6—C56—H56B	110.7
C41—C30—H30A	109.5	C55—C56—H56B	110.7
C41—C30—H30B	109.5	H56A—C56—H56B	108.8
H30A—C30—H30B	109.5	C24—C57—H57A	109.5
C41—C30—H30C	109.5	C24—C57—H57B	109.5
H30A—C30—H30C	109.5	H57A—C57—H57B	109.5
H30B—C30—H30C	109.5	C24—C57—H57C	109.5
C41—C31—H31A	109.5	H57A—C57—H57C	109.5
C41—C31—H31B	109.5	H57B—C57—H57C	109.5
H31A—C31—H31B	109.5	C29—C58—C50	102.4 (2)
C41—C31—H31C	109.5	C29—C58—H58A	111.3
H31A—C31—H31C	109.5	C50—C58—H58A	111.3
H31B—C31—H31C	109.5	C29—C58—H58B	111.3
C41—C32—H32A	109.5	C50—C58—H58B	111.3
C41—C32—H32B	109.5	H58A—C58—H58B	109.2
H32A—C32—H32B	109.5	C52—C59—C25	101.6 (2)
C41—C32—H32C	109.5	C52—C59—H59A	111.4
H32A—C32—H32C	109.5	C25—C59—H59A	111.4
H32B—C32—H32C	109.5	C52—C59—H59B	111.4
C24—C33—H33A	109.5	C25—C59—H59B	111.4
C24—C33—H33B	109.5	H59A—C59—H59B	109.3
H33A—C33—H33B	109.5	C50—O4—C51	109.0 (2)
C24—C33—H33C	109.5	C52—O5—C53	108.96 (18)
H33A—C33—H33C	109.5	C56—O6—C46	109.45 (19)
H33B—C33—H33C	109.5	C28—O7—C35	108.6 (2)
C27—C34—C35	105.3 (3)

C9—C1—C2—O1	176.94 (18)	C20—C17—C24—C26	68.6 (3)
C8—C1—C2—O1	−7.7 (3)	C12—C17—C24—C57	11.9 (3)
C9—C1—C2—C6	−1.2 (3)	C20—C17—C24—C57	−170.8 (2)
C8—C1—C2—C6	174.14 (19)	C12—C17—C24—C33	130.8 (3)
C9—C1—C2—Mg1ⁱ	141.50 (17)	C20—C17—C24—C33	−51.8 (3)
C8—C1—C2—Mg1ⁱ	−43.1 (2)	C34—C27—C28—O7	−34.5 (4)
O2ⁱ—C4—C5—C10	171.5 (2)	C28—C27—C34—C35	28.2 (4)
C19—C4—C5—C10	−6.5 (3)	C27—C34—C35—O7	−12.1 (4)
O2ⁱ—C4—C5—C8	−0.8 (3)	C23—C22—C41—C32	−104.3 (3)
C19—C4—C5—C8	−178.75 (19)	C10—C22—C41—C32	72.5 (3)
O1—C2—C6—C14	−177.94 (19)	C23—C22—C41—C31	17.8 (4)
C1—C2—C6—C14	0.2 (3)	C10—C22—C41—C31	−165.4 (3)
Mg1ⁱ—C2—C6—C14	−131.29 (18)	C23—C22—C41—C30	136.7 (3)
O1—C2—C6—C11	3.4 (3)	C10—C22—C41—C30	−46.6 (3)
C1—C2—C6—C11	−178.4 (2)	C58—C29—C51—O4	27.8 (3)
Mg1ⁱ—C2—C6—C11	50.1 (3)	C59—C25—C53—O5	−18.2 (3)
C12—C3—C7—O3	169.8 (2)	O6—C46—C54—C55	26.9 (3)
C8—C3—C7—O3	−7.3 (3)	C46—C54—C55—C56	−37.5 (3)
C12—C3—C7—C16	−9.0 (3)	C54—C55—C56—O6	35.2 (3)
C8—C3—C7—C16	173.85 (19)	C51—C29—C58—C50	−37.0 (3)
C12—C3—C8—C1	−80.2 (2)	O4—C50—C58—C29	33.7 (3)
C7—C3—C8—C1	96.8 (2)	O5—C52—C59—C25	−36.9 (3)
C12—C3—C8—C5	53.6 (3)	C53—C25—C59—C52	33.5 (3)
C7—C3—C8—C5	−129.4 (2)	C6—C2—O1—Mg1	−125.70 (18)
C9—C1—C8—C3	68.1 (2)	C1—C2—O1—Mg1	56.1 (3)
C2—C1—C8—C3	−107.2 (2)	Mg1ⁱ—C2—O1—Mg1	121.06 (18)
C9—C1—C8—C5	−66.0 (3)	C6—C2—O1—Mg1ⁱ	113.24 (18)
C2—C1—C8—C5	118.7 (2)	C1—C2—O1—Mg1ⁱ	−65.0 (2)
C10—C5—C8—C3	−1.2 (3)	O3—Mg1—O1—C2	−11.18 (18)
C4—C5—C8—C3	170.7 (2)	O2—Mg1—O1—C2	125.97 (16)
C10—C5—C8—C1	129.7 (2)	O1ⁱ—Mg1—O1—C2	−128.83 (18)
C4—C5—C8—C1	−58.4 (3)	C2ⁱ—Mg1—O1—C2	−146.02 (13)
C2—C1—C9—C15	1.7 (3)	Mg1ⁱ—Mg1—O1—C2	−128.83 (18)
C8—C1—C9—C15	−173.71 (19)	O3—Mg1—O1—Mg1ⁱ	117.65 (7)
C4—C5—C10—C22	5.0 (3)	O2—Mg1—O1—Mg1ⁱ	−105.19 (8)
C8—C5—C10—C22	176.8 (2)	O1ⁱ—Mg1—O1—Mg1ⁱ	0.0
C14—C6—C11—C39	118.9 (2)	C2ⁱ—Mg1—O1—Mg1ⁱ	−17.19 (7)
C2—C6—C11—C39	−62.5 (3)	O3—Mg1—O2—C4ⁱ	147.1 (2)
C14—C6—C11—C37	−0.3 (3)	O1—Mg1—O2—C4ⁱ	11.6 (2)
C2—C6—C11—C37	178.3 (2)	O1ⁱ—Mg1—O2—C4ⁱ	−80.7 (2)
C14—C6—C11—C40	−119.3 (2)	C2ⁱ—Mg1—O2—C4ⁱ	−90.0 (2)
C2—C6—C11—C40	59.3 (3)	Mg1ⁱ—Mg1—O2—C4ⁱ	−37.1 (2)
C7—C3—C12—C17	5.0 (3)	C3—C7—O3—Mg1	−2.4 (4)
C8—C3—C12—C17	−178.0 (2)	C16—C7—O3—Mg1	176.38 (18)
C2—C6—C14—C15	0.4 (3)	O2—Mg1—O3—C7	−166.1 (2)
C11—C6—C14—C15	179.1 (2)	O1—Mg1—O3—C7	−28.4 (3)
C1—C9—C15—C14	−1.0 (3)	O1ⁱ—Mg1—O3—C7	67.3 (3)
C1—C9—C15—C21	176.9 (2)	C2ⁱ—Mg1—O3—C7	96.4 (3)
C6—C14—C15—C9	−0.1 (3)	Mg1ⁱ—Mg1—O3—C7	18.3 (3)
C6—C14—C15—C21	−178.1 (2)	C58—C50—O4—C51	−16.7 (3)
O3—C7—C16—C20	−172.68 (19)	C58—C50—O4—Li1	139.7 (2)
C3—C7—C16—C20	6.2 (3)	C29—C51—O4—C50	−7.0 (3)
O3—C7—C16—C13	5.2 (3)	C29—C51—O4—Li1	−162.6 (2)
C3—C7—C16—C13	−175.93 (19)	O6—Li1—O4—C50	−79.6 (3)
C36A—C13—C16—C20	−130.1 (2)	O5—Li1—O4—C50	157.2 (2)
C49—C13—C16—C20	108.8 (2)	O7—Li1—O4—C50	38.8 (3)
C38—C13—C16—C20	−9.7 (3)	O6—Li1—O4—C51	73.1 (3)
C36A—C13—C16—C7	52.1 (3)	O5—Li1—O4—C51	−50.1 (3)
C49—C13—C16—C7	−69.0 (3)	O7—Li1—O4—C51	−168.6 (2)
C38—C13—C16—C7	172.5 (2)	C59—C52—O5—C53	26.8 (3)
C3—C12—C17—C20	2.0 (3)	C59—C52—O5—Li1	−135.9 (2)
C3—C12—C17—C24	179.5 (2)	C25—C53—O5—C52	−5.3 (3)
O2ⁱ—C4—C19—C23	−174.1 (2)	C25—C53—O5—Li1	155.0 (3)
C5—C4—C19—C23	3.9 (3)	O6—Li1—O5—C52	−147.6 (2)
O2ⁱ—C4—C19—C18	2.0 (3)	O4—Li1—O5—C52	−29.1 (3)
C5—C4—C19—C18	−180.0 (2)	O7—Li1—O5—C52	91.9 (3)
C43—C18—C19—C23	109.6 (2)	O6—Li1—O5—C53	53.8 (4)
C42—C18—C19—C23	−129.3 (2)	O4—Li1—O5—C53	172.2 (2)
C48—C18—C19—C23	−9.4 (3)	O7—Li1—O5—C53	−66.8 (3)
C43—C18—C19—C4	−66.4 (3)	C55—C56—O6—C46	−18.9 (3)
C42—C18—C19—C4	54.7 (3)	C55—C56—O6—Li1	172.0 (3)
C48—C18—C19—C4	174.6 (2)	C54—C46—O6—C56	−5.4 (3)
C7—C16—C20—C17	1.0 (3)	C54—C46—O6—Li1	164.0 (2)
C13—C16—C20—C17	−176.9 (2)	O5—Li1—O6—C56	166.7 (2)
C12—C17—C20—C16	−5.1 (3)	O4—Li1—O6—C56	47.1 (3)
C24—C17—C20—C16	177.3 (2)	O7—Li1—O6—C56	−73.3 (3)
C9—C15—C21—C47	−4.5 (3)	O5—Li1—O6—C46	−0.9 (4)
C14—C15—C21—C47	173.5 (2)	O4—Li1—O6—C46	−120.5 (2)
C9—C15—C21—C44I	−124.3 (2)	O7—Li1—O6—C46	119.1 (2)
C14—C15—C21—C44I	53.6 (3)	C27—C28—O7—C35	27.6 (3)
C9—C15—C21—C45	117.3 (2)	C27—C28—O7—Li1	−170.7 (3)
C14—C15—C21—C45	−64.8 (3)	C34—C35—O7—C28	−10.4 (4)
C5—C10—C22—C23	−0.7 (4)	C34—C35—O7—Li1	−172.0 (3)
C5—C10—C22—C41	−177.6 (2)	O6—Li1—O7—C28	−124.5 (3)
C10—C22—C23—C19	−2.1 (4)	O5—Li1—O7—C28	−0.5 (3)
C41—C22—C23—C19	174.8 (2)	O4—Li1—O7—C28	118.4 (3)
C4—C19—C23—C22	0.4 (4)	O6—Li1—O7—C35	34.3 (3)
C18—C19—C23—C22	−175.7 (2)	O5—Li1—O7—C35	158.3 (2)
C12—C17—C24—C26	−108.8 (3)	O4—Li1—O7—C35	−82.7 (3)

Symmetry code: (i) −x+1, −y+2, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C8—H8···O1	0.98	2.33	2.867 (2)	114
C8—H8···O3	0.98	2.37	2.864 (2)	110
C36A—H36C···O3	0.96	2.30	2.935 (3)	123
C39—H39C···O1	0.96	2.41	3.030 (3)	122
C40—H40C···O1	0.96	2.40	3.025 (3)	122
C42—H42B···O2ⁱ	0.96	2.28	2.953 (3)	126
C43—H43B···O2ⁱ	0.96	2.48	3.091 (3)	122
C49—H49A···O3	0.96	2.47	3.094 (3)	122

Symmetry code: (i) −x+1, −y+2, −z+1.

Acknowledgements

The authors thank Dr Yong-Liang Shao from the Center of Testing and Analysis, Lanzhou University, for the structure determination.

Funding information

Funding for this research was provided by: National Natural Science Foundation of China (award No. 21362034); Science and Technology Innovation Fund of Gansu Agricultural University (award No. GAU-CX1115).

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