Di­bromo­tetra-μ3-methoxo-di-μ2-methoxo-hexakis­(tetra­hydro­furan-d8)­tetramagnesium

Walfort, B.; Yousef, R.I.; Rüffer, T.; Steinborn, D.

doi:10.1107/S010827010401933X

Dibromotetra-μ₃-methoxo-di-μ₂-methoxo-hexakis(tetrahydrofuran-d₈)tetramagnesium

B. Walfort, R. I. Yousef, T. Rüffer and D. Steinborn

The crystal structure of the title compound, [Mg₄Br₂(CH₃O)₆(C₄D₈O)₆], consists of discrete molecules with imposed symmetry C_i. The tetranuclear compound exhibits two crystallographically independent Mg atoms having distorted octahedral and trigonal–bipyramidal coordination spheres. The Mg atoms are bridged by two μ₃-OMe and four μ₂-OMe ligands, and their coordination is completed by two terminal Br and six tetrahydrofuran ligands.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010401933X/jz1633sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S010827010401933X/jz1633Isup2.hkl Contains datablock I

CCDC reference: 254896

Comment top

Mg exhibits a rich coordination chemistry, ranging from mononuclear to polymeric species with linear two-coordinate up to ten-coordinate Mg atoms. With typical bridging ligands, such as halides, alkoxides, amides and organyls, Mg tends to form cluster and cage compounds (Fenton, 1987; Holloway & Melnik, 1994). Here, we report the structure of the title methoxo-bridged tetranuclear complex, (I), having µ₂– and µ₃-bridging methoxo ligands and also terminal Br and tetrahydrofuran (THF) ligands. \sch

Complex (I) crystallizes as discrete molecules without unusual intermolecular contacts (Fig. 1); the smallest distance between non-H atoms is 3.597 (4) Å between atoms C7 and C15ⁱ [symmetry code: (i) x − 1, y, z]. The molecule lies on a crystallographic inversion centre located at the centre of the Mg2—Mg2ⁱⁱ—O2—O2ⁱⁱ rhomboid [symmetry code: (ii) 1 − x, 1 − y, 2 − z].

The two independent Mg atoms exhibit six- (Mg2) or five- (Mg1) coordination. The six-coordinated Mg atoms have a distorted octahedral coordination sphere built up from two terminal THF ligands in mutually cis positions, and two µ₂– and two µ₃-bridging methoxo ligands in mutually trans and cis positions, respectively. The angles of the coordination octahedron lie between 78.97 (7) and 101.74 (7)° or 170.12 (7) and 175.87 (8)°. The five-coordinated Mg atoms exhibit a trigonal-bipyramidal coordination sphere. The apical positions (L_ap) are occupied by a µ₃-OMe lignad (O2) and a terminal THF (O6) ligand; the O2—Mg1—O6 angle is 170.24 (7)°. The equatorial coordination sites (L_eq) are occupied by a Br ligand and two µ₂-OMe ligands. The angles between the equatorial ligands range from 114.67 (8) to 125.37 (6)° (sum of angles 359.83°). The L_eq—Mg1—L_ap angles lie between 82.98 (7) and 98.37 (5)°. The Mg-µ-OMe distances are in the order Mg1/2-µ₃-OMe [2.093 (2)–2.117 (2) Å] > Mg2-µ₂-OMe [1.999 (2) and 2.015 (2) Å] > Mg1-µ₂-OMe [1.950 (2) and 1.968 (2) Å], so that bonds to the µ₃-bridging methoxy ligands are longer than to the µ₂-bound ligands. Furthermore, the five-coordinate Mg atoms bind the µ₂ ligands more tightly than the six-coordinate Mg atoms. On the other hand, the Mg—O bonds to µ₃-OMe and to THF ligands do not exhibit statistically significant (3σ criterion) length dependence on coordination number (5 versus 6).

As shown in Fig. 2, the tetranuclear complex (I) can be (formally) viewed as being built up from two octahedra and two trigonal bipyramids that are edge-shared. Thus, a tetranuclear cluster is formed with a core of two face-linked open cuboidal building blocks having the composition [Mg₄(µ₂-OMe)₄(µ₃-OMe)₂]²⁺. Due to the crystallographically imposed inversion symmetry, the four Mg atoms define an exact plane. An analogous structural motif has also been found in other Mg clusters having [Mg₄(µ₂-X)₄(µ₃-X)₂]²⁺ cores with Cl bridges (X = Cl) (Toney & Stucky, 1971; Casellato & Ossola, 1994) or with bridging deprotonated ether-alcohol ligands such as 2-hydroxymethyltetrahydrofuran, 2,3-dihydro-2,2-dimethyl-7-hydroxybenzofuran (Sobota et al., 1996; Sobota Utko Sztajnowska et al., 2000; Sobota Utko Ejfler & Jerzykiewicz, 2000), and 1-methoxypropan-2-ol (Albaric et al., 1997). All these structures exhibit crystallographically imposed inversion symmetry.

Experimental top

Dissolution of [MgMeBr(diglyme)] (prepared by addition of diglyme to a concentrated solution of MgMeBr in diethyl ether) in THF-d₈ resulted in a clear solution. Due to slow decomposition of this solution at 233 K, crystals of (I) appeared within several weeks.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.

Figures top

	Fig. 1. A view of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. Only one of the two disordered positions of C10 is displayed.
	Fig. 2. A drawing of the edge-sharing octahedra and trigonal bipyramids in the structure of (I).

Dibromotetra-µ₂-methoxo-di-µ₃-methoxo-hexakis(tetrahydrofuran-d₈– κO)tetramagnesium top

Crystal data top

[Mg₄Br₂(CH₃O)₆(C₄D₈O)₆]	F(000) = 920
M_r = 924.18	D_x = 1.497 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 8574 reflections
a = 8.4836 (4) Å	θ = 2.4–28.3°
b = 18.9094 (9) Å	µ = 2.09 mm⁻¹
c = 12.8907 (6) Å	T = 173 K
β = 97.457 (1)°	Block, colourless
V = 2050.43 (17) Å³	0.4 × 0.3 × 0.2 mm
Z = 2

Data collection top

Bruker SMART CCD area-detector diffractometer	5081 independent reflections
Radiation source: fine-focus sealed tube	4061 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.035
ω scans	θ_max = 28.3°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	h = −11→11
T_min = 0.476, T_max = 0.658	k = 0→25
17714 measured reflections	l = 0→17

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.099	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0394P)² + 1.3532P] where P = (F_o² + 2F_c²)/3
5081 reflections	(Δ/σ)_max = 0.042
230 parameters	Δρ_max = 0.92 e Å⁻³
32 restraints	Δρ_min = −0.36 e Å⁻³

Crystal data top

[Mg₄Br₂(CH₃O)₆(C₄D₈O)₆]	V = 2050.43 (17) Å³
M_r = 924.18	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 8.4836 (4) Å	µ = 2.09 mm⁻¹
b = 18.9094 (9) Å	T = 173 K
c = 12.8907 (6) Å	0.4 × 0.3 × 0.2 mm
β = 97.457 (1)°

Data collection top

Bruker SMART CCD area-detector diffractometer	5081 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	4061 reflections with I > 2σ(I)
T_min = 0.476, T_max = 0.658	R_int = 0.035
17714 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	32 restraints
wR(F²) = 0.099	H-atom parameters constrained
S = 1.03	Δρ_max = 0.92 e Å⁻³
5081 reflections	Δρ_min = −0.36 e Å⁻³
230 parameters

Special details top

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Br1	0.27721 (3)	0.405228 (15)	0.68375 (2)	0.04558 (10)
Mg2	0.45363 (8)	0.57885 (4)	0.95620 (5)	0.02374 (15)
Mg1	0.50196 (8)	0.45599 (4)	0.81074 (5)	0.02684 (16)
O1	0.5342 (2)	0.55901 (8)	0.81879 (11)	0.0325 (3)
C1	0.5294 (4)	0.60039 (15)	0.7317 (2)	0.0535 (8)
H1A	0.6358	0.6095	0.7174	0.064*
H1B	0.4778	0.6443	0.7433	0.064*
H1C	0.4713	0.5764	0.6732	0.064*
O2	0.37570 (16)	0.47264 (7)	0.93847 (11)	0.0244 (3)
C2	0.2138 (2)	0.45762 (12)	0.94659 (19)	0.0330 (5)
H2A	0.1797	0.4180	0.9028	0.040*
H2B	0.1498	0.4981	0.9245	0.040*
H2C	0.2023	0.4466	1.0179	0.040*
O3	0.35780 (18)	0.59838 (8)	1.08700 (12)	0.0312 (3)
C3	0.2205 (4)	0.63500 (17)	1.0980 (2)	0.0549 (8)
H3A	0.1996	0.6321	1.1693	0.066*
H3B	0.1332	0.6148	1.0529	0.066*
H3C	0.2331	0.6837	1.0795	0.066*
O4	0.2549 (2)	0.63660 (9)	0.86328 (14)	0.0403 (4)
C4	0.2335 (4)	0.71230 (14)	0.8525 (2)	0.0509 (7)
H4A	0.3244	0.7337	0.8262	0.061*
H4B	0.2213	0.7335	0.9195	0.061*
C5	0.0853 (4)	0.72281 (16)	0.7763 (2)	0.0552 (7)
H5A	−0.0090	0.7230	0.8115	0.066*
H5B	0.0899	0.7665	0.7374	0.066*
C6	0.0886 (5)	0.65939 (18)	0.7062 (3)	0.0716 (10)
H6A	0.1615	0.6662	0.6550	0.086*
H6B	−0.0164	0.6487	0.6703	0.086*
C7	0.1462 (4)	0.60231 (16)	0.7836 (3)	0.0645 (10)
H7A	0.0578	0.5817	0.8137	0.077*
H7B	0.1998	0.5652	0.7498	0.077*
O5	0.57503 (19)	0.68104 (8)	0.97351 (12)	0.0324 (3)
C8	0.7007 (3)	0.70616 (13)	0.9175 (2)	0.0405 (6)
H8A	0.6590	0.7383	0.8619	0.049*
H8B	0.7525	0.6669	0.8871	0.049*
C9	0.8164 (3)	0.74417 (14)	0.9984 (2)	0.0461 (6)
H9A	0.9144	0.7175	1.0134	0.055*	0.343 (18)
H9B	0.8411	0.7908	0.9736	0.055*	0.343 (18)
H9C	0.8879	0.7113	1.0385	0.055*	0.657 (18)
H9D	0.8780	0.7793	0.9663	0.055*	0.657 (18)
C10A	0.7326 (14)	0.7496 (10)	1.0951 (12)	0.061 (4)	0.343 (18)
H10A	0.7839	0.7196	1.1504	0.074*	0.343 (18)
H10B	0.7345	0.7980	1.1203	0.074*	0.343 (18)
C11	0.5707 (4)	0.72675 (15)	1.0635 (2)	0.0513 (7)
H11A	0.5022	0.7671	1.0451	0.062*	0.343 (18)
H11B	0.5307	0.7012	1.1199	0.062*	0.343 (18)
H11C	0.5827	0.6990	1.1273	0.062*	0.657 (18)
H11D	0.4698	0.7515	1.0582	0.062*	0.657 (18)
C10B	0.7035 (7)	0.7782 (4)	1.0652 (5)	0.0423 (14)	0.657 (18)
H10C	0.7550	0.7856	1.1360	0.051*	0.657 (18)
H10D	0.6655	0.8233	1.0361	0.051*	0.657 (18)
O6	0.6659 (2)	0.44822 (10)	0.69411 (12)	0.0414 (4)
C12	0.6437 (4)	0.41772 (17)	0.5911 (2)	0.0548 (8)
H12A	0.5515	0.4382	0.5494	0.066*
H12B	0.6286	0.3670	0.5950	0.066*
C13	0.7937 (4)	0.4345 (2)	0.5436 (2)	0.0631 (9)
H13A	0.8679	0.3952	0.5524	0.076*
H13B	0.7695	0.4451	0.4696	0.076*
C14	0.8604 (3)	0.49822 (18)	0.6035 (2)	0.0529 (7)
H14A	0.9745	0.5018	0.6033	0.064*
H14B	0.8102	0.5414	0.5753	0.064*
C15	0.8201 (3)	0.48328 (18)	0.7103 (2)	0.0507 (7)
H15A	0.8995	0.4528	0.7484	0.061*
H15B	0.8140	0.5268	0.7494	0.061*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Br1	0.04077 (15)	0.05488 (17)	0.03910 (15)	−0.00895 (11)	−0.00236 (10)	−0.01575 (11)
Mg2	0.0241 (3)	0.0245 (3)	0.0232 (3)	−0.0010 (3)	0.0055 (3)	−0.0003 (3)
Mg1	0.0293 (4)	0.0285 (4)	0.0233 (3)	−0.0043 (3)	0.0056 (3)	−0.0035 (3)
O1	0.0415 (9)	0.0308 (8)	0.0261 (7)	−0.0059 (7)	0.0078 (6)	−0.0027 (6)
C1	0.079 (2)	0.0448 (15)	0.0410 (14)	−0.0151 (14)	0.0244 (14)	−0.0071 (12)
O2	0.0191 (6)	0.0272 (7)	0.0272 (7)	−0.0023 (5)	0.0042 (5)	−0.0004 (6)
C2	0.0221 (10)	0.0366 (12)	0.0411 (12)	−0.0022 (8)	0.0068 (9)	0.0032 (10)
O3	0.0307 (8)	0.0328 (8)	0.0319 (8)	0.0048 (6)	0.0110 (6)	−0.0005 (6)
C3	0.0526 (17)	0.0576 (18)	0.0602 (18)	0.0153 (14)	0.0290 (14)	0.0126 (14)
O4	0.0401 (9)	0.0331 (9)	0.0440 (10)	0.0033 (7)	−0.0086 (7)	0.0037 (7)
C4	0.0568 (17)	0.0350 (13)	0.0583 (17)	0.0077 (12)	−0.0022 (13)	0.0038 (12)
C5	0.0555 (17)	0.0496 (16)	0.0604 (18)	0.0108 (13)	0.0066 (14)	0.0186 (14)
C6	0.081 (2)	0.060 (2)	0.065 (2)	0.0195 (18)	−0.0274 (18)	0.0013 (16)
C7	0.0593 (19)	0.0451 (16)	0.078 (2)	0.0022 (14)	−0.0342 (17)	0.0012 (15)
O5	0.0356 (8)	0.0275 (8)	0.0353 (8)	−0.0071 (6)	0.0089 (7)	−0.0057 (6)
C8	0.0464 (14)	0.0346 (12)	0.0433 (13)	−0.0120 (10)	0.0164 (11)	−0.0010 (10)
C9	0.0368 (13)	0.0406 (14)	0.0605 (17)	−0.0067 (11)	0.0050 (12)	−0.0034 (12)
C10A	0.056 (6)	0.048 (8)	0.078 (8)	−0.008 (5)	−0.002 (5)	−0.031 (6)
C11	0.0591 (17)	0.0445 (15)	0.0544 (16)	−0.0167 (13)	0.0234 (13)	−0.0242 (13)
C10B	0.042 (3)	0.035 (3)	0.049 (3)	−0.004 (2)	0.003 (2)	−0.014 (2)
O6	0.0408 (9)	0.0602 (11)	0.0256 (8)	−0.0126 (8)	0.0134 (7)	−0.0101 (8)
C12	0.0652 (19)	0.0684 (19)	0.0337 (13)	−0.0140 (15)	0.0177 (13)	−0.0218 (13)
C13	0.0607 (19)	0.093 (2)	0.0401 (15)	−0.0044 (18)	0.0237 (14)	−0.0193 (16)
C14	0.0448 (15)	0.078 (2)	0.0395 (14)	−0.0075 (14)	0.0170 (12)	0.0030 (14)
C15	0.0384 (14)	0.077 (2)	0.0382 (14)	−0.0142 (13)	0.0114 (11)	−0.0082 (13)

Geometric parameters (Å, º) top

Br1—Mg1	2.5350 (7)	C6—H6A	0.9700
Mg2—O3	1.9989 (16)	C6—H6B	0.9700
Mg2—O1	2.0149 (16)	C7—H7A	0.9700
Mg2—O2ⁱ	2.0923 (15)	C7—H7B	0.9700
Mg2—O2	2.1174 (15)	O5—C8	1.444 (3)
Mg2—O5	2.1874 (16)	O5—C11	1.451 (3)
Mg2—O4	2.2236 (17)	C8—C9	1.517 (4)
Mg2—Mg1	3.0464 (10)	C8—H8A	0.9700
Mg2—Mg1ⁱ	3.0508 (10)	C8—H8B	0.9700
Mg2—Mg2ⁱ	3.2489 (13)	C9—C10B	1.512 (6)
Mg1—O3ⁱ	1.9502 (17)	C9—C10A	1.516 (12)
Mg1—O1	1.9681 (17)	C9—H9A	0.9700
Mg1—O2	2.1012 (15)	C9—H9B	0.9700
Mg1—O6	2.1818 (17)	C9—H9C	0.9700
Mg1—Mg2ⁱ	3.0508 (10)	C9—H9D	0.9700
O1—C1	1.365 (3)	C10A—C11	1.447 (10)
C1—H1A	0.9600	C10A—H10A	0.9700
C1—H1B	0.9600	C10A—H10B	0.9700
C1—H1C	0.9600	C11—C10B	1.487 (6)
O2—C2	1.420 (2)	C11—H11A	0.9700
O2—Mg2ⁱ	2.0923 (15)	C11—H11B	0.9700
C2—H2A	0.9600	C11—H11C	0.9700
C2—H2B	0.9600	C11—H11D	0.9700
C2—H2C	0.9600	C10B—H10C	0.9700
O3—C3	1.378 (3)	C10B—H10D	0.9700
O3—Mg1ⁱ	1.9502 (17)	O6—C12	1.437 (3)
C3—H3A	0.9600	O6—C15	1.457 (3)
C3—H3B	0.9600	C12—C13	1.516 (4)
C3—H3C	0.9600	C12—H12A	0.9700
O4—C7	1.442 (3)	C12—H12B	0.9700
O4—C4	1.447 (3)	C13—C14	1.502 (5)
C4—C5	1.505 (4)	C13—H13A	0.9700
C4—H4A	0.9700	C13—H13B	0.9700
C4—H4B	0.9700	C14—C15	1.488 (4)
C5—C6	1.503 (5)	C14—H14A	0.9700
C5—H5A	0.9700	C14—H14B	0.9700
C5—H5B	0.9700	C15—H15A	0.9700
C6—C7	1.508 (4)	C15—H15B	0.9700

O3—Mg2—O1	175.86 (8)	C6—C5—H5B	111.4
O3—Mg2—O2ⁱ	82.04 (6)	C4—C5—H5B	111.4
O1—Mg2—O2ⁱ	101.47 (7)	H5A—C5—H5B	109.2
O3—Mg2—O2	96.37 (6)	C5—C6—C7	101.7 (3)
O1—Mg2—O2	82.26 (6)	C5—C6—H6A	111.4
O2ⁱ—Mg2—O2	78.98 (6)	C7—C6—H6A	111.4
O3—Mg2—O5	89.33 (7)	C5—C6—H6B	111.4
O1—Mg2—O5	92.59 (6)	C7—C6—H6B	111.4
O2ⁱ—Mg2—O5	93.89 (6)	H6A—C6—H6B	109.3
O2—Mg2—O5	170.12 (7)	O4—C7—C6	105.8 (2)
O3—Mg2—O4	90.05 (7)	O4—C7—H7A	110.6
O1—Mg2—O4	86.43 (7)	C6—C7—H7A	110.6
O2ⁱ—Mg2—O4	172.08 (7)	O4—C7—H7B	110.6
O2—Mg2—O4	101.74 (6)	C6—C7—H7B	110.6
O5—Mg2—O4	86.28 (7)	H7A—C7—H7B	108.7
O3—Mg2—Mg1	139.64 (5)	C8—O5—C11	107.53 (17)
O1—Mg2—Mg1	39.54 (5)	C8—O5—Mg2	127.45 (13)
O2ⁱ—Mg2—Mg1	84.69 (4)	C11—O5—Mg2	123.18 (14)
O2—Mg2—Mg1	43.56 (4)	O5—C8—C9	105.4 (2)
O5—Mg2—Mg1	129.59 (5)	O5—C8—H8A	110.7
O4—Mg2—Mg1	101.31 (5)	C9—C8—H8A	110.7
O3—Mg2—Mg1ⁱ	38.84 (5)	O5—C8—H8B	110.7
O1—Mg2—Mg1ⁱ	144.38 (6)	C9—C8—H8B	110.7
O2ⁱ—Mg2—Mg1ⁱ	43.44 (4)	H8A—C8—H8B	108.8
O2—Mg2—Mg1ⁱ	84.17 (4)	C10B—C9—C8	101.1 (3)
O5—Mg2—Mg1ⁱ	95.39 (5)	C10A—C9—C8	105.5 (4)
O4—Mg2—Mg1ⁱ	128.66 (6)	C10B—C9—H9A	134.2
Mg1—Mg2—Mg1ⁱ	115.60 (3)	C10A—C9—H9A	110.6
O3—Mg2—Mg2ⁱ	89.03 (5)	C8—C9—H9A	110.6
O1—Mg2—Mg2ⁱ	92.31 (5)	C10B—C9—H9B	88.9
O2ⁱ—Mg2—Mg2ⁱ	39.77 (4)	C10A—C9—H9B	110.6
O2—Mg2—Mg2ⁱ	39.21 (4)	C8—C9—H9B	110.6
O5—Mg2—Mg2ⁱ	133.30 (6)	H9A—C9—H9B	108.8
O4—Mg2—Mg2ⁱ	140.39 (6)	C10B—C9—H9C	111.6
Mg1—Mg2—Mg2ⁱ	57.87 (2)	C10A—C9—H9C	86.2
Mg1ⁱ—Mg2—Mg2ⁱ	57.74 (2)	C8—C9—H9C	111.6
O3ⁱ—Mg1—O1	114.70 (8)	H9B—C9—H9C	127.7
O3ⁱ—Mg1—O2	82.97 (6)	C10B—C9—H9D	111.6
O1—Mg1—O2	83.79 (6)	C10A—C9—H9D	129.7
O3ⁱ—Mg1—O6	92.45 (7)	C8—C9—H9D	111.6
O1—Mg1—O6	90.36 (7)	H9A—C9—H9D	86.9
O2—Mg1—O6	170.24 (7)	H9C—C9—H9D	109.4
O3ⁱ—Mg1—Br1	125.35 (6)	C11—C10A—C9	106.1 (7)
O1—Mg1—Br1	119.77 (6)	C11—C10A—H10A	110.5
O2—Mg1—Br1	98.37 (5)	C9—C10A—H10A	110.5
O6—Mg1—Br1	91.31 (5)	C11—C10A—H10B	110.5
O3ⁱ—Mg1—Mg2	96.03 (5)	C9—C10A—H10B	110.5
O1—Mg1—Mg2	40.68 (5)	H10A—C10A—H10B	108.7
O2—Mg1—Mg2	43.98 (4)	C10A—C11—O5	106.3 (5)
O6—Mg1—Mg2	128.63 (6)	O5—C11—C10B	107.7 (3)
Br1—Mg1—Mg2	122.43 (3)	C10A—C11—H11A	110.5
O3ⁱ—Mg1—Mg2ⁱ	40.00 (5)	O5—C11—H11A	110.5
O1—Mg1—Mg2ⁱ	99.40 (5)	C10B—C11—H11A	85.3
O2—Mg1—Mg2ⁱ	43.21 (4)	C10A—C11—H11B	110.5
O6—Mg1—Mg2ⁱ	130.97 (6)	O5—C11—H11B	110.5
Br1—Mg1—Mg2ⁱ	122.72 (3)	C10B—C11—H11B	130.8
Mg2—Mg1—Mg2ⁱ	64.40 (3)	H11A—C11—H11B	108.7
C1—O1—Mg1	122.35 (15)	C10A—C11—H11C	86.1
C1—O1—Mg2	129.74 (16)	O5—C11—H11C	110.2
Mg1—O1—Mg2	99.78 (7)	C10B—C11—H11C	110.2
O1—C1—H1A	109.5	H11A—C11—H11C	128.9
O1—C1—H1B	109.5	C10A—C11—H11D	132.2
H1A—C1—H1B	109.5	O5—C11—H11D	110.2
O1—C1—H1C	109.5	C10B—C11—H11D	110.2
H1A—C1—H1C	109.5	H11B—C11—H11D	84.5
H1B—C1—H1C	109.5	H11C—C11—H11D	108.5
C2—O2—Mg2ⁱ	116.98 (13)	C11—C10B—C9	104.4 (3)
C2—O2—Mg1	128.63 (13)	C11—C10B—H10C	110.9
Mg2ⁱ—O2—Mg1	93.36 (6)	C9—C10B—H10C	110.9
C2—O2—Mg2	118.24 (13)	C11—C10B—H10D	110.9
Mg2ⁱ—O2—Mg2	101.02 (6)	C9—C10B—H10D	110.9
Mg1—O2—Mg2	92.46 (6)	H10C—C10B—H10D	108.9
O2—C2—H2A	109.5	C12—O6—C15	108.82 (19)
O2—C2—H2B	109.5	C12—O6—Mg1	130.13 (16)
H2A—C2—H2B	109.5	C15—O6—Mg1	120.76 (14)
O2—C2—H2C	109.5	O6—C12—C13	105.8 (2)
H2A—C2—H2C	109.5	O6—C12—H12A	110.6
H2B—C2—H2C	109.5	C13—C12—H12A	110.6
C3—O3—Mg1ⁱ	130.15 (16)	O6—C12—H12B	110.6
C3—O3—Mg2	128.42 (16)	C13—C12—H12B	110.6
Mg1ⁱ—O3—Mg2	101.16 (7)	H12A—C12—H12B	108.7
O3—C3—H3A	109.5	C14—C13—C12	103.9 (2)
O3—C3—H3B	109.5	C14—C13—H13A	111.0
H3A—C3—H3B	109.5	C12—C13—H13A	111.0
O3—C3—H3C	109.5	C14—C13—H13B	111.0
H3A—C3—H3C	109.5	C12—C13—H13B	111.0
H3B—C3—H3C	109.5	H13A—C13—H13B	109.0
C7—O4—C4	108.4 (2)	C15—C14—C13	101.9 (2)
C7—O4—Mg2	122.20 (15)	C15—C14—H14A	111.4
C4—O4—Mg2	127.90 (16)	C13—C14—H14A	111.4
O4—C4—C5	106.1 (2)	C15—C14—H14B	111.4
O4—C4—H4A	110.5	C13—C14—H14B	111.4
C5—C4—H4A	110.5	H14A—C14—H14B	109.2
O4—C4—H4B	110.5	O6—C15—C14	105.3 (2)
C5—C4—H4B	110.5	O6—C15—H15A	110.7
H4A—C4—H4B	108.7	C14—C15—H15A	110.7
C6—C5—C4	102.0 (2)	O6—C15—H15B	110.7
C6—C5—H5A	111.4	C14—C15—H15B	110.7
C4—C5—H5A	111.4	H15A—C15—H15B	108.8

O3—Mg2—Mg1—O3ⁱ	−64.86 (11)	O2ⁱ—Mg2—O2—Mg2ⁱ	0.0
O1—Mg2—Mg1—O3ⁱ	121.45 (9)	O4—Mg2—O2—Mg2ⁱ	−171.96 (7)
O2ⁱ—Mg2—Mg1—O3ⁱ	6.23 (6)	Mg1—Mg2—O2—Mg2ⁱ	93.91 (6)
O2—Mg2—Mg1—O3ⁱ	−73.34 (8)	Mg1ⁱ—Mg2—O2—Mg2ⁱ	−43.63 (5)
O5—Mg2—Mg1—O3ⁱ	96.90 (8)	O3—Mg2—O2—Mg1	−174.49 (6)
O4—Mg2—Mg1—O3ⁱ	−168.55 (7)	O1—Mg2—O2—Mg1	9.44 (6)
Mg1ⁱ—Mg2—Mg1—O3ⁱ	−25.21 (5)	O2ⁱ—Mg2—O2—Mg1	−93.91 (6)
Mg2ⁱ—Mg2—Mg1—O3ⁱ	−25.21 (5)	O4—Mg2—O2—Mg1	94.14 (7)
O3—Mg2—Mg1—O1	173.68 (12)	Mg1ⁱ—Mg2—O2—Mg1	−137.54 (4)
O2ⁱ—Mg2—Mg1—O1	−115.22 (9)	Mg2ⁱ—Mg2—O2—Mg1	−93.91 (7)
O2—Mg2—Mg1—O1	165.20 (10)	O2ⁱ—Mg2—O3—C3	−179.9 (2)
O5—Mg2—Mg1—O1	−24.56 (10)	O2—Mg2—O3—C3	−102.0 (2)
O4—Mg2—Mg1—O1	70.00 (9)	O5—Mg2—O3—C3	86.0 (2)
Mg1ⁱ—Mg2—Mg1—O1	−146.66 (9)	O4—Mg2—O3—C3	−0.2 (2)
Mg2ⁱ—Mg2—Mg1—O1	−146.66 (9)	Mg1—Mg2—O3—C3	−107.9 (2)
O3—Mg2—Mg1—O2	8.48 (10)	Mg1ⁱ—Mg2—O3—C3	−174.5 (3)
O1—Mg2—Mg1—O2	−165.20 (10)	Mg2ⁱ—Mg2—O3—C3	−140.6 (2)
O2ⁱ—Mg2—Mg1—O2	79.57 (7)	O2ⁱ—Mg2—O3—Mg1ⁱ	−5.43 (7)
O5—Mg2—Mg1—O2	170.24 (9)	O2—Mg2—O3—Mg1ⁱ	72.45 (8)
O4—Mg2—Mg1—O2	−95.21 (8)	O5—Mg2—O3—Mg1ⁱ	−99.46 (8)
Mg1ⁱ—Mg2—Mg1—O2	48.14 (6)	O4—Mg2—O3—Mg1ⁱ	174.27 (7)
Mg2ⁱ—Mg2—Mg1—O2	48.14 (6)	Mg1—Mg2—O3—Mg1ⁱ	66.58 (11)
O3—Mg2—Mg1—O6	−162.87 (10)	Mg2ⁱ—Mg2—O3—Mg1ⁱ	33.87 (6)
O1—Mg2—Mg1—O6	23.44 (10)	O3—Mg2—O4—C7	−117.5 (2)
O2ⁱ—Mg2—Mg1—O6	−91.78 (8)	O1—Mg2—O4—C7	60.3 (2)
O2—Mg2—Mg1—O6	−171.35 (10)	O2—Mg2—O4—C7	−21.0 (3)
O5—Mg2—Mg1—O6	−1.11 (10)	O5—Mg2—O4—C7	153.2 (2)
O4—Mg2—Mg1—O6	93.44 (9)	Mg1—Mg2—O4—C7	23.5 (2)
Mg1ⁱ—Mg2—Mg1—O6	−123.22 (8)	Mg1ⁱ—Mg2—O4—C7	−112.9 (2)
Mg2ⁱ—Mg2—Mg1—O6	−123.22 (8)	Mg2ⁱ—Mg2—O4—C7	−29.0 (3)
O3—Mg2—Mg1—Br1	74.28 (9)	O3—Mg2—O4—C4	78.1 (2)
O1—Mg2—Mg1—Br1	−99.40 (8)	O1—Mg2—O4—C4	−104.0 (2)
O2ⁱ—Mg2—Mg1—Br1	145.37 (5)	O2—Mg2—O4—C4	174.6 (2)
O2—Mg2—Mg1—Br1	65.80 (6)	O5—Mg2—O4—C4	−11.2 (2)
O5—Mg2—Mg1—Br1	−123.96 (7)	Mg1—Mg2—O4—C4	−140.9 (2)
O4—Mg2—Mg1—Br1	−29.40 (6)	Mg1ⁱ—Mg2—O4—C4	82.7 (2)
Mg1ⁱ—Mg2—Mg1—Br1	113.94 (4)	Mg2ⁱ—Mg2—O4—C4	166.67 (19)
Mg2ⁱ—Mg2—Mg1—Br1	113.94 (4)	C7—O4—C4—C5	10.7 (3)
O3—Mg2—Mg1—Mg2ⁱ	−39.65 (8)	Mg2—O4—C4—C5	176.77 (17)
O1—Mg2—Mg1—Mg2ⁱ	146.66 (9)	O4—C4—C5—C6	−31.6 (3)
O2ⁱ—Mg2—Mg1—Mg2ⁱ	31.44 (4)	C4—C5—C6—C7	39.3 (4)
O2—Mg2—Mg1—Mg2ⁱ	−48.14 (6)	C4—O4—C7—C6	14.7 (4)
O5—Mg2—Mg1—Mg2ⁱ	122.11 (7)	Mg2—O4—C7—C6	−152.3 (2)
O4—Mg2—Mg1—Mg2ⁱ	−143.34 (6)	C5—C6—C7—O4	−33.9 (4)
Mg1ⁱ—Mg2—Mg1—Mg2ⁱ	0.0	O3—Mg2—O5—C8	167.84 (19)
O3ⁱ—Mg1—O1—C1	139.7 (2)	O1—Mg2—O5—C8	−15.83 (19)
O2—Mg1—O1—C1	−141.0 (2)	O2ⁱ—Mg2—O5—C8	85.86 (19)
O6—Mg1—O1—C1	46.8 (2)	O4—Mg2—O5—C8	−102.07 (19)
Br1—Mg1—O1—C1	−44.9 (2)	Mg1—Mg2—O5—C8	−0.5 (2)
Mg2—Mg1—O1—C1	−151.3 (2)	Mg1ⁱ—Mg2—O5—C8	129.42 (18)
Mg2ⁱ—Mg1—O1—C1	178.5 (2)	Mg2ⁱ—Mg2—O5—C8	79.8 (2)
O3ⁱ—Mg1—O1—Mg2	−69.03 (9)	O3—Mg2—O5—C11	5.2 (2)
O2—Mg1—O1—Mg2	10.28 (7)	O1—Mg2—O5—C11	−178.4 (2)
O6—Mg1—O1—Mg2	−161.89 (8)	O2ⁱ—Mg2—O5—C11	−76.8 (2)
Br1—Mg1—O1—Mg2	106.39 (6)	O4—Mg2—O5—C11	95.3 (2)
Mg2ⁱ—Mg1—O1—Mg2	−30.16 (7)	Mg1—Mg2—O5—C11	−163.08 (18)
O2ⁱ—Mg2—O1—C1	−145.1 (2)	Mg1ⁱ—Mg2—O5—C11	−33.2 (2)
O2—Mg2—O1—C1	137.9 (2)	Mg2ⁱ—Mg2—O5—C11	−82.8 (2)
O5—Mg2—O1—C1	−50.5 (2)	C11—O5—C8—C9	25.4 (3)
O4—Mg2—O1—C1	35.6 (2)	Mg2—O5—C8—C9	−139.40 (17)
Mg1—Mg2—O1—C1	148.2 (3)	O5—C8—C9—C10B	−36.6 (4)
Mg1ⁱ—Mg2—O1—C1	−153.5 (2)	O5—C8—C9—C10A	−9.9 (9)
Mg2ⁱ—Mg2—O1—C1	175.9 (2)	C10B—C9—C10A—C11	74.8 (14)
O2ⁱ—Mg2—O1—Mg1	66.80 (8)	C8—C9—C10A—C11	−8.9 (14)
O2—Mg2—O1—Mg1	−10.23 (7)	C9—C10A—C11—O5	24.5 (14)
O5—Mg2—O1—Mg1	161.30 (8)	C9—C10A—C11—C10B	−72.5 (14)
O4—Mg2—O1—Mg1	−112.60 (8)	C8—O5—C11—C10A	−31.8 (10)
Mg1ⁱ—Mg2—O1—Mg1	58.32 (12)	Mg2—O5—C11—C10A	133.8 (10)
Mg2ⁱ—Mg2—O1—Mg1	27.76 (7)	C8—O5—C11—C10B	−3.4 (5)
O3ⁱ—Mg1—O2—C2	−123.89 (17)	Mg2—O5—C11—C10B	162.2 (4)
O1—Mg1—O2—C2	120.21 (17)	C10A—C11—C10B—C9	71.6 (11)
Br1—Mg1—O2—C2	0.94 (17)	O5—C11—C10B—C9	−19.9 (6)
Mg2—Mg1—O2—C2	129.85 (18)	C10A—C9—C10B—C11	−68.7 (10)
Mg2ⁱ—Mg1—O2—C2	−128.95 (18)	C8—C9—C10B—C11	33.9 (5)
O3ⁱ—Mg1—O2—Mg2ⁱ	5.07 (6)	O3ⁱ—Mg1—O6—C12	119.9 (2)
O1—Mg1—O2—Mg2ⁱ	−110.84 (7)	O1—Mg1—O6—C12	−125.4 (2)
Br1—Mg1—O2—Mg2ⁱ	129.90 (5)	Br1—Mg1—O6—C12	−5.6 (2)
Mg2—Mg1—O2—Mg2ⁱ	−101.20 (6)	Mg2—Mg1—O6—C12	−140.4 (2)
O3ⁱ—Mg1—O2—Mg2	106.27 (7)	Mg2ⁱ—Mg1—O6—C12	131.8 (2)
O1—Mg1—O2—Mg2	−9.64 (7)	O3ⁱ—Mg1—O6—C15	−66.9 (2)
Br1—Mg1—O2—Mg2	−128.90 (4)	O1—Mg1—O6—C15	47.8 (2)
Mg2ⁱ—Mg1—O2—Mg2	101.20 (6)	Br1—Mg1—O6—C15	167.6 (2)
O3—Mg2—O2—C2	48.42 (15)	Mg2—Mg1—O6—C15	32.8 (2)
O1—Mg2—O2—C2	−127.65 (15)	Mg2ⁱ—Mg1—O6—C15	−55.0 (2)
O2ⁱ—Mg2—O2—C2	129.00 (16)	C15—O6—C12—C13	0.9 (4)
O4—Mg2—O2—C2	−42.95 (15)	Mg1—O6—C12—C13	174.7 (2)
Mg1—Mg2—O2—C2	−137.09 (16)	O6—C12—C13—C14	−23.3 (4)
Mg1ⁱ—Mg2—O2—C2	85.37 (14)	C12—C13—C14—C15	35.9 (3)
Mg2ⁱ—Mg2—O2—C2	129.00 (16)	C12—O6—C15—C14	22.2 (3)
O3—Mg2—O2—Mg2ⁱ	−80.58 (7)	Mg1—O6—C15—C14	−152.25 (19)
O1—Mg2—O2—Mg2ⁱ	103.35 (7)	C13—C14—C15—O6	−35.9 (3)

Symmetry code: (i) −x+1, −y+1, −z+2.

Experimental details

Crystal data
Chemical formula	[Mg₄Br₂(CH₃O)₆(C₄D₈O)₆]
M_r	924.18
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	173
a, b, c (Å)	8.4836 (4), 18.9094 (9), 12.8907 (6)
β (°)	97.457 (1)
V (Å³)	2050.43 (17)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.09
Crystal size (mm)	0.4 × 0.3 × 0.2

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2001)
T_min, T_max	0.476, 0.658
No. of measured, independent and observed [I > 2σ(I)] reflections	17714, 5081, 4061
R_int	0.035
(sin θ/λ)_max (Å⁻¹)	0.666

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.099, 1.03
No. of reflections	5081
No. of parameters	230
No. of restraints	32
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.92, −0.36

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 1999), SHELXL97.

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Di­bromo­tetra-μ3-methoxo-di-μ2-methoxo-hexakis­(tetra­hydro­furan-d8)­tetramagnesium

Supporting information

Dibromotetra-μ₃-methoxo-di-μ₂-methoxo-hexakis(tetrahydrofuran-d₈)tetramagnesium