metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

(Bi­phenyl-2-yl)bromidobis(2-methyl­tetra­hydro­furan-κO)magnesium(II)

aChemetall GmbH, Lithium Division, Trakehner Strasse 3, 60487 Frankfurt am Main, Germany, and bInstitut für Anorganische Chemie, J. W. Goethe-Universität Frankfurt, Max-von-Laue-Strasse 7, 60438 Frankfurt/Main, Germany
*Correspondence e-mail: bolte@chemie.uni-frankfurt.de

(Received 23 March 2009; accepted 1 April 2009; online 8 April 2009)

In the title Grignard reagent, [MgBr(C12H9)(C5H10O)2], the Mg centre adopts a distorted tetra­hedral MgCO2Br arrangement. The dihedral angle between the two aromatic rings of the biphenyl residue is 44.00 (14)°. Each mol­ecule incorporates one R- and one S-configured 2-methyl­tetra­hydro­furan mol­ecule.

Related literature

For background to Grignard-type compounds, see Elschenbroich (2008[Elschenbroich, C. (2008). In Organometallchemie. Stuttgart: Teubner BG.]); Schwetlick (1996[Schwetlick, K. (1996). In Organikum. Heidelberg: Johann Ambrosius Barth.]); Silverman & Rakita (1996[Silverman, G. S. & Rakita, P. E. (1996). In Handbook of Grignard Reagents. New York: Dekker.]).

[Scheme 1]

Experimental

Crystal data
  • [MgBr(C12H9)(C5H10O)2]

  • Mr = 429.67

  • Monoclinic, P 21 /n

  • a = 11.6887 (5) Å

  • b = 16.8061 (9) Å

  • c = 11.7888 (5) Å

  • β = 103.757 (4)°

  • V = 2249.38 (18) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.87 mm−1

  • T = 173 K

  • 0.29 × 0.28 × 0.26 mm

Data collection
  • Stoe IPDSII two-circle diffractometer

  • Absorption correction: multi-scan (MULABS; Spek, 2003[Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.]; Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.614, Tmax = 0.642

  • 54470 measured reflections

  • 4107 independent reflections

  • 3484 reflections with I > 2σ(I)

  • Rint = 0.069

Refinement
  • R[F2 > 2σ(F2)] = 0.045

  • wR(F2) = 0.108

  • S = 1.05

  • 4107 reflections

  • 236 parameters

  • H-atom parameters constrained

  • Δρmax = 0.76 e Å−3

  • Δρmin = −0.41 e Å−3

Table 1
Selected geometric parameters (Å, °)

Mg1—O1 2.022 (2)
Mg1—O11 2.030 (2)
Mg1—C21 2.143 (3)
Mg1—Br1 2.4750 (10)
O1—Mg1—O11 97.02 (10)
O1—Mg1—C21 114.41 (11)
O11—Mg1—C21 106.87 (11)
O1—Mg1—Br1 109.97 (9)
O11—Mg1—Br1 104.75 (7)
C21—Mg1—Br1 120.53 (8)

Data collection: X-AREA (Stoe & Cie, 2001[Stoe & Cie (2001). X-AREA. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

The title compound is a Grignard reagent, a kind of compounds which is widely used for C—C bond formation or as base in organic chemistry. The Mg centre is four coordinate in a distorted tetrahedral fashion. The bond angles range from 97.02 (1)° for O—Mg—O to 120.53 (8)° for C—Mg—Br. The bond lengths are 2.4750 (10)Å for Mg—Br, 2.143 (3)Å for Mg—C and 2.022 (2)° and 2.030 (2)Å for the Mg—O bonds. The dihedral angles between the two aromatic rings of the biphenyl residue is 44.00 (14)°.

Related literature top

For background to Grignard-type compounds, see Elschenbroich (2008); Schwetlick (1996); Silverman & Rakita (1996).

Experimental top

This compound is commercially available from Chemetall GmbH (CAS 82214–69-5, Product No. 408562). Colourless blocks of (I) were obtained from a solution due to long term storage at ambient temperature.

Refinement top

The H atoms bonded were geometrically positioned and refined with fixed individual displacement parameters [U(H) = 1.2 Ueq(C) or U(H) = 1.5 Ueq(Cmethyl)] using a riding model with Caromatic—H = 0.95 Å, Cmethyl—H = 0.98 Å, Cmethylene—H = 0.99Å and Ctertiary—H = 1.00 Å.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Perspective view of (I) with displacement ellipsoids drawn at the 50% probability level; H atoms omitted for clarity.
(Biphenyl-2-yl)bromidobis(2-methyltetrahydrofuran-κO)magnesium(II) top
Crystal data top
[MgBr(C12H9)(C5H10O)2]F(000) = 896
Mr = 429.67Dx = 1.269 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 40381 reflections
a = 11.6887 (5) Åθ = 3.6–26.6°
b = 16.8061 (9) ŵ = 1.87 mm1
c = 11.7888 (5) ÅT = 173 K
β = 103.757 (4)°Block, colourless
V = 2249.38 (18) Å30.29 × 0.28 × 0.26 mm
Z = 4
Data collection top
Stoe IPDSII two-circle
diffractometer
4107 independent reflections
Radiation source: fine-focus sealed tube3484 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.069
ω scansθmax = 25.4°, θmin = 3.6°
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
h = 1414
Tmin = 0.614, Tmax = 0.642k = 2020
54470 measured reflectionsl = 1414
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.108 w = 1/[σ2(Fo2) + (0.0462P)2 + 2.3133P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max < 0.001
4107 reflectionsΔρmax = 0.76 e Å3
236 parametersΔρmin = 0.41 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0043 (6)
Crystal data top
[MgBr(C12H9)(C5H10O)2]V = 2249.38 (18) Å3
Mr = 429.67Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.6887 (5) ŵ = 1.87 mm1
b = 16.8061 (9) ÅT = 173 K
c = 11.7888 (5) Å0.29 × 0.28 × 0.26 mm
β = 103.757 (4)°
Data collection top
Stoe IPDSII two-circle
diffractometer
4107 independent reflections
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
3484 reflections with I > 2σ(I)
Tmin = 0.614, Tmax = 0.642Rint = 0.069
54470 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.108H-atom parameters constrained
S = 1.05Δρmax = 0.76 e Å3
4107 reflectionsΔρmin = 0.41 e Å3
236 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
xyzUiso*/Ueq
Mg10.56815 (8)0.31486 (6)0.70780 (8)0.0349 (2)
Br10.60093 (3)0.24360 (2)0.89652 (3)0.05398 (15)
O10.4214 (2)0.38260 (15)0.6841 (2)0.0572 (6)
C20.4112 (4)0.4578 (4)0.6045 (5)0.0967 (17)
H2A0.48980.47810.60110.116*
H2B0.36490.44650.52430.116*
C30.3515 (7)0.5122 (4)0.6625 (8)0.159 (4)
H3A0.31140.55420.60850.190*
H3B0.40670.53760.72960.190*
C40.2618 (6)0.4595 (5)0.7036 (7)0.145 (3)
H4A0.23120.48600.76530.173*
H4B0.19510.44500.63790.173*
C50.3367 (5)0.3866 (6)0.7512 (5)0.143 (3)
H50.37630.39480.83540.172*
C60.2702 (6)0.3147 (6)0.7372 (7)0.170 (4)
H6A0.32120.27050.77200.256*
H6B0.23830.30440.65390.256*
H6C0.20520.31990.77620.256*
O110.50159 (19)0.23129 (11)0.58553 (18)0.0412 (5)
C120.4587 (3)0.2531 (2)0.4632 (3)0.0536 (8)
H12A0.49400.30400.44640.064*
H12B0.37180.25870.44300.064*
C130.4955 (5)0.1870 (3)0.3968 (4)0.0852 (15)
H13A0.43550.17770.32310.102*
H13B0.57130.19980.37740.102*
C140.5080 (4)0.1158 (2)0.4719 (4)0.0672 (11)
H14A0.58330.08840.47320.081*
H14B0.44260.07820.44220.081*
C150.5056 (3)0.14444 (18)0.5944 (3)0.0521 (9)
H150.57990.12790.65080.063*
C160.4023 (4)0.1148 (3)0.6359 (4)0.0790 (13)
H16A0.40650.13510.71470.119*
H16B0.40320.05650.63730.119*
H16C0.32940.13340.58290.119*
C210.7121 (2)0.37048 (16)0.6550 (2)0.0341 (6)
C220.7636 (2)0.44648 (17)0.6866 (3)0.0395 (7)
C230.8611 (3)0.4719 (2)0.6460 (3)0.0549 (9)
H230.89280.52340.66660.066*
C240.9121 (3)0.4234 (3)0.5767 (4)0.0627 (11)
H240.97940.44110.55180.075*
C250.8648 (3)0.3495 (2)0.5439 (3)0.0542 (9)
H250.89860.31590.49590.065*
C260.7668 (3)0.32490 (18)0.5821 (3)0.0419 (7)
H260.73450.27410.55770.050*
C310.6804 (3)0.4711 (2)0.8611 (3)0.0483 (8)
H310.69140.41630.88020.058*
C320.7136 (3)0.50025 (17)0.7624 (3)0.0442 (8)
C330.6971 (4)0.5819 (2)0.7384 (3)0.0638 (11)
H330.72050.60390.67320.077*
C340.6474 (5)0.6307 (2)0.8081 (4)0.0854 (16)
H340.63540.68550.78900.102*
C350.6154 (4)0.6014 (3)0.9041 (4)0.0853 (16)
H350.58210.63560.95170.102*
C360.6318 (4)0.5206 (2)0.9319 (3)0.0656 (11)
H360.60990.49970.99860.079*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.0308 (5)0.0364 (5)0.0377 (5)0.0051 (4)0.0085 (4)0.0023 (4)
Br10.0496 (2)0.0716 (3)0.0401 (2)0.01271 (17)0.00923 (14)0.00894 (16)
O10.0412 (13)0.0673 (16)0.0586 (15)0.0132 (11)0.0029 (11)0.0154 (12)
C20.059 (3)0.116 (4)0.106 (4)0.027 (3)0.002 (3)0.014 (3)
C30.129 (6)0.114 (5)0.174 (8)0.051 (5)0.082 (6)0.039 (5)
C40.103 (5)0.204 (8)0.133 (6)0.102 (6)0.039 (4)0.001 (5)
C50.080 (4)0.269 (10)0.082 (4)0.081 (5)0.023 (3)0.001 (5)
C60.086 (5)0.277 (12)0.145 (7)0.072 (6)0.022 (4)0.027 (7)
O110.0477 (12)0.0308 (11)0.0408 (11)0.0064 (9)0.0017 (9)0.0021 (8)
C120.065 (2)0.0477 (19)0.0407 (17)0.0002 (17)0.0019 (15)0.0043 (15)
C130.137 (5)0.065 (3)0.054 (2)0.002 (3)0.024 (3)0.013 (2)
C140.072 (3)0.050 (2)0.075 (3)0.0072 (19)0.009 (2)0.0172 (19)
C150.054 (2)0.0317 (16)0.061 (2)0.0068 (14)0.0061 (16)0.0057 (15)
C160.090 (3)0.069 (3)0.073 (3)0.043 (2)0.010 (2)0.003 (2)
C210.0299 (13)0.0292 (14)0.0409 (15)0.0013 (11)0.0038 (11)0.0036 (12)
C220.0312 (14)0.0343 (15)0.0451 (17)0.0061 (12)0.0063 (12)0.0082 (13)
C230.0436 (19)0.054 (2)0.058 (2)0.0204 (16)0.0055 (16)0.0150 (17)
C240.0345 (17)0.086 (3)0.067 (2)0.0100 (18)0.0113 (16)0.025 (2)
C250.0435 (18)0.066 (2)0.057 (2)0.0104 (17)0.0198 (16)0.0174 (18)
C260.0397 (16)0.0364 (16)0.0507 (18)0.0063 (13)0.0129 (14)0.0064 (13)
C310.0481 (18)0.0392 (17)0.0478 (19)0.0046 (14)0.0079 (14)0.0072 (14)
C320.0417 (16)0.0341 (16)0.0450 (18)0.0045 (13)0.0132 (13)0.0052 (13)
C330.082 (3)0.0333 (18)0.055 (2)0.0038 (17)0.0242 (19)0.0040 (16)
C340.124 (4)0.038 (2)0.065 (3)0.015 (2)0.035 (3)0.017 (2)
C350.103 (4)0.064 (3)0.066 (3)0.033 (2)0.025 (3)0.034 (2)
C360.069 (2)0.068 (2)0.049 (2)0.013 (2)0.0076 (18)0.0172 (18)
Geometric parameters (Å, º) top
Mg1—O12.022 (2)C14—H14A0.9900
Mg1—O112.030 (2)C14—H14B0.9900
Mg1—C212.143 (3)C15—C161.492 (5)
Mg1—Br12.4750 (10)C15—H151.0000
O1—C51.408 (6)C16—H16A0.9800
O1—C21.562 (6)C16—H16B0.9800
C2—C31.421 (9)C16—H16C0.9800
C2—H2A0.9900C21—C261.412 (4)
C2—H2B0.9900C21—C221.424 (4)
C3—C41.536 (11)C22—C231.403 (5)
C3—H3A0.9900C22—C321.485 (5)
C3—H3B0.9900C23—C241.385 (6)
C4—C51.533 (9)C23—H230.9500
C4—H4A0.9900C24—C251.377 (6)
C4—H4B0.9900C24—H240.9500
C5—C61.425 (11)C25—C261.390 (4)
C5—H51.0000C25—H250.9500
C6—H6A0.9800C26—H260.9500
C6—H6B0.9800C31—C361.393 (5)
C6—H6C0.9800C31—C321.399 (5)
O11—C121.456 (4)C31—H310.9500
O11—C151.463 (4)C32—C331.404 (4)
C12—C131.481 (5)C33—C341.384 (6)
C12—H12A0.9900C33—H330.9500
C12—H12B0.9900C34—C351.366 (7)
C13—C141.475 (6)C34—H340.9500
C13—H13A0.9900C35—C361.398 (6)
C13—H13B0.9900C35—H350.9500
C14—C151.529 (5)C36—H360.9500
O1—Mg1—O1197.02 (10)C13—C14—C15106.8 (3)
O1—Mg1—C21114.41 (11)C13—C14—H14A110.4
O11—Mg1—C21106.87 (11)C15—C14—H14A110.4
O1—Mg1—Br1109.97 (9)C13—C14—H14B110.4
O11—Mg1—Br1104.75 (7)C15—C14—H14B110.4
C21—Mg1—Br1120.53 (8)H14A—C14—H14B108.6
C5—O1—C2109.6 (4)O11—C15—C16110.0 (3)
C5—O1—Mg1129.5 (3)O11—C15—C14104.7 (3)
C2—O1—Mg1118.7 (2)C16—C15—C14113.8 (3)
C3—C2—O1102.0 (5)O11—C15—H15109.4
C3—C2—H2A111.4C16—C15—H15109.4
O1—C2—H2A111.4C14—C15—H15109.4
C3—C2—H2B111.4C15—C16—H16A109.5
O1—C2—H2B111.4C15—C16—H16B109.5
H2A—C2—H2B109.2H16A—C16—H16B109.5
C2—C3—C4103.3 (6)C15—C16—H16C109.5
C2—C3—H3A111.1H16A—C16—H16C109.5
C4—C3—H3A111.1H16B—C16—H16C109.5
C2—C3—H3B111.1C26—C21—C22114.9 (3)
C4—C3—H3B111.1C26—C21—Mg1116.1 (2)
H3A—C3—H3B109.1C22—C21—Mg1128.9 (2)
C5—C4—C3101.7 (5)C23—C22—C21120.8 (3)
C5—C4—H4A111.4C23—C22—C32119.2 (3)
C3—C4—H4A111.4C21—C22—C32120.0 (3)
C5—C4—H4B111.4C24—C23—C22121.3 (3)
C3—C4—H4B111.4C24—C23—H23119.3
H4A—C4—H4B109.3C22—C23—H23119.3
O1—C5—C6109.4 (6)C25—C24—C23119.7 (3)
O1—C5—C4104.4 (6)C25—C24—H24120.1
C6—C5—C4112.8 (7)C23—C24—H24120.1
O1—C5—H5110.0C24—C25—C26119.0 (3)
C6—C5—H5110.0C24—C25—H25120.5
C4—C5—H5110.0C26—C25—H25120.5
C5—C6—H6A109.5C25—C26—C21124.2 (3)
C5—C6—H6B109.5C25—C26—H26117.9
H6A—C6—H6B109.5C21—C26—H26117.9
C5—C6—H6C109.5C36—C31—C32121.6 (3)
H6A—C6—H6C109.5C36—C31—H31119.2
H6B—C6—H6C109.5C32—C31—H31119.2
C12—O11—C15108.6 (2)C31—C32—C33117.2 (3)
C12—O11—Mg1120.80 (18)C31—C32—C22121.0 (3)
C15—O11—Mg1129.73 (19)C33—C32—C22121.8 (3)
O11—C12—C13105.0 (3)C34—C33—C32121.1 (4)
O11—C12—H12A110.7C34—C33—H33119.5
C13—C12—H12A110.7C32—C33—H33119.5
O11—C12—H12B110.7C35—C34—C33121.0 (4)
C13—C12—H12B110.7C35—C34—H34119.5
H12A—C12—H12B108.8C33—C34—H34119.5
C14—C13—C12106.9 (3)C34—C35—C36119.7 (4)
C14—C13—H13A110.3C34—C35—H35120.1
C12—C13—H13A110.3C36—C35—H35120.1
C14—C13—H13B110.3C31—C36—C35119.4 (4)
C12—C13—H13B110.3C31—C36—H36120.3
H13A—C13—H13B108.6C35—C36—H36120.3
O11—Mg1—O1—C5101.5 (5)C13—C14—C15—C16115.6 (4)
C21—Mg1—O1—C5146.4 (5)O1—Mg1—C21—C26130.5 (2)
Br1—Mg1—O1—C57.1 (5)O11—Mg1—C21—C2624.4 (2)
O11—Mg1—O1—C297.5 (3)Br1—Mg1—C21—C2694.8 (2)
C21—Mg1—O1—C214.7 (3)O1—Mg1—C21—C2252.0 (3)
Br1—Mg1—O1—C2154.0 (3)O11—Mg1—C21—C22158.2 (2)
C5—O1—C2—C320.6 (6)Br1—Mg1—C21—C2282.6 (3)
Mg1—O1—C2—C3144.0 (4)C26—C21—C22—C230.3 (4)
O1—C2—C3—C438.6 (5)Mg1—C21—C22—C23177.7 (2)
C2—C3—C4—C543.7 (7)C26—C21—C22—C32179.6 (3)
C2—O1—C5—C6127.7 (6)Mg1—C21—C22—C322.9 (4)
Mg1—O1—C5—C669.9 (7)C21—C22—C23—C241.6 (5)
C2—O1—C5—C46.8 (7)C32—C22—C23—C24179.0 (3)
Mg1—O1—C5—C4169.2 (4)C22—C23—C24—C251.7 (5)
C3—C4—C5—O129.7 (8)C23—C24—C25—C260.4 (5)
C3—C4—C5—C6148.4 (7)C24—C25—C26—C211.0 (5)
O1—Mg1—O11—C1260.3 (3)C22—C21—C26—C251.1 (4)
C21—Mg1—O11—C1257.9 (3)Mg1—C21—C26—C25176.7 (2)
Br1—Mg1—O11—C12173.1 (2)C36—C31—C32—C330.8 (5)
O1—Mg1—O11—C15131.4 (3)C36—C31—C32—C22179.0 (3)
C21—Mg1—O11—C15110.4 (3)C23—C22—C32—C31136.9 (3)
Br1—Mg1—O11—C1518.6 (3)C21—C22—C32—C3143.7 (4)
C15—O11—C12—C1328.8 (4)C23—C22—C32—C3343.3 (4)
Mg1—O11—C12—C13141.7 (3)C21—C22—C32—C33136.1 (3)
O11—C12—C13—C1425.2 (5)C31—C32—C33—C341.6 (5)
C12—C13—C14—C1512.7 (5)C22—C32—C33—C34178.2 (3)
C12—O11—C15—C16102.0 (3)C32—C33—C34—C351.6 (6)
Mg1—O11—C15—C1688.6 (3)C33—C34—C35—C360.7 (7)
C12—O11—C15—C1420.7 (4)C32—C31—C36—C350.1 (5)
Mg1—O11—C15—C14148.7 (2)C34—C35—C36—C310.1 (6)
C13—C14—C15—O114.6 (4)

Experimental details

Crystal data
Chemical formula[MgBr(C12H9)(C5H10O)2]
Mr429.67
Crystal system, space groupMonoclinic, P21/n
Temperature (K)173
a, b, c (Å)11.6887 (5), 16.8061 (9), 11.7888 (5)
β (°) 103.757 (4)
V3)2249.38 (18)
Z4
Radiation typeMo Kα
µ (mm1)1.87
Crystal size (mm)0.29 × 0.28 × 0.26
Data collection
DiffractometerStoe IPDSII two-circle
diffractometer
Absorption correctionMulti-scan
(MULABS; Spek, 2003; Blessing, 1995)
Tmin, Tmax0.614, 0.642
No. of measured, independent and
observed [I > 2σ(I)] reflections
54470, 4107, 3484
Rint0.069
(sin θ/λ)max1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.108, 1.05
No. of reflections4107
No. of parameters236
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.76, 0.41

Computer programs: X-AREA (Stoe & Cie, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL-Plus (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Mg1—O12.022 (2)Mg1—C212.143 (3)
Mg1—O112.030 (2)Mg1—Br12.4750 (10)
O1—Mg1—O1197.02 (10)O1—Mg1—Br1109.97 (9)
O1—Mg1—C21114.41 (11)O11—Mg1—Br1104.75 (7)
O11—Mg1—C21106.87 (11)C21—Mg1—Br1120.53 (8)
 

References

First citationBlessing, R. H. (1995). Acta Cryst. A51, 33–38.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationElschenbroich, C. (2008). In Organometallchemie. Stuttgart: Teubner BG.  Google Scholar
First citationSchwetlick, K. (1996). In Organikum. Heidelberg: Johann Ambrosius Barth.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSilverman, G. S. & Rakita, P. E. (1996). In Handbook of Grignard Reagents. New York: Dekker.  Google Scholar
First citationSpek, A. L. (2003). J. Appl. Cryst. 36, 7–13.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationStoe & Cie (2001). X-AREA. Stoe & Cie, Darmstadt, Germany.  Google Scholar

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