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The structure of the title compound, [Mn2Br2(CO)8], has previously been determined at room temperature using film data [Dahl & Wei (1963). Acta Cryst. 16, 611–616]. The 100 K structure reported here is in good agreement with the previous study but of significantly higher precision.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005885/hb2008sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005885/hb2008Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](O-C) = 0.003 Å
  • R factor = 0.036
  • wR factor = 0.091
  • Data-to-parameter ratio = 20.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Br1 - Mn1 .. 6.07 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 - C3 .. 6.27 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn2 - C5 .. 5.47 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn2 - C8 .. 5.01 su
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97 and PLATON.

; top
Crystal data top
[Mn(CO)4Br]2F(000) = 928
Mr = 493.78Dx = 2.502 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25326 reflections
a = 9.4545 (7) Åθ = 3.6–29.5°
b = 11.5713 (8) ŵ = 8.06 mm1
c = 12.6818 (9) ÅT = 100 K
β = 109.148 (6)°Block, orange
V = 1310.64 (16) Å30.36 × 0.20 × 0.18 mm
Z = 4
Data collection top
STOE IPDS II two-circle-
diffractometer
3694 independent reflections
Radiation source: fine-focus sealed tube3267 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.070
ω scansθmax = 29.7°, θmin = 3.7°
Absorption correction: multi-scan
MULABS (Spek, 2003; Blessing, 1995)
h = 1313
Tmin = 0.160, Tmax = 0.225k = 1616
20694 measured reflectionsl = 1717
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.036Secondary atom site location: difference Fourier map
wR(F2) = 0.091 w = 1/[σ2(Fo2) + (0.0606P)2 + 0.3697P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
3694 reflectionsΔρmax = 1.16 e Å3
181 parametersΔρmin = 1.38 e Å3
Special details top

Experimental. ;

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
Mn10.60114 (5)0.37760 (4)0.32182 (3)0.01860 (10)
Mn20.18229 (5)0.37332 (3)0.21831 (3)0.01888 (10)
Br10.38850 (3)0.49547 (2)0.34632 (2)0.02118 (9)
Br20.39368 (3)0.25509 (2)0.19399 (2)0.02067 (9)
C10.5925 (3)0.4691 (2)0.1963 (2)0.0226 (5)
O10.5895 (3)0.5216 (2)0.12004 (19)0.0302 (5)
C20.7408 (3)0.4724 (2)0.4147 (2)0.0218 (5)
O20.8302 (3)0.53111 (19)0.47308 (18)0.0261 (4)
C30.7471 (3)0.2898 (2)0.2999 (2)0.0226 (5)
O30.8418 (3)0.2360 (2)0.2875 (2)0.0289 (4)
C40.6006 (3)0.2840 (2)0.4433 (2)0.0224 (5)
O40.6036 (3)0.22668 (19)0.51663 (19)0.0289 (4)
C50.1882 (3)0.4686 (2)0.0999 (2)0.0231 (5)
O50.1897 (3)0.5271 (2)0.0288 (2)0.0320 (5)
C60.0379 (3)0.4622 (2)0.2424 (2)0.0235 (5)
O60.0543 (3)0.5174 (2)0.2566 (2)0.0295 (4)
C70.0421 (3)0.2813 (2)0.1233 (2)0.0221 (5)
O70.0475 (3)0.2247 (2)0.0627 (2)0.0292 (4)
C80.1885 (3)0.2777 (2)0.3411 (2)0.0221 (5)
O80.1905 (3)0.2203 (2)0.41410 (19)0.0300 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.01640 (19)0.02144 (19)0.01695 (18)0.00025 (13)0.00410 (14)0.00001 (13)
Mn20.01675 (19)0.02175 (18)0.01689 (18)0.00017 (14)0.00382 (14)0.00000 (13)
Br10.01811 (14)0.02340 (14)0.02069 (14)0.00041 (9)0.00454 (10)0.00369 (8)
Br20.01841 (14)0.02235 (14)0.01980 (13)0.00020 (8)0.00428 (10)0.00257 (8)
C10.0208 (12)0.0243 (11)0.0216 (12)0.0002 (9)0.0054 (10)0.0015 (9)
O10.0373 (13)0.0299 (10)0.0226 (10)0.0002 (9)0.0084 (9)0.0026 (8)
C20.0192 (12)0.0268 (12)0.0194 (11)0.0014 (9)0.0062 (9)0.0014 (9)
O20.0230 (10)0.0288 (10)0.0235 (10)0.0026 (8)0.0037 (8)0.0017 (8)
C30.0225 (13)0.0246 (12)0.0202 (11)0.0032 (10)0.0062 (10)0.0008 (9)
O30.0244 (11)0.0302 (10)0.0327 (11)0.0024 (8)0.0101 (9)0.0021 (8)
C40.0192 (12)0.0257 (12)0.0221 (12)0.0006 (9)0.0066 (10)0.0011 (9)
O40.0335 (12)0.0287 (10)0.0249 (10)0.0002 (9)0.0103 (9)0.0033 (8)
C50.0209 (13)0.0249 (12)0.0216 (12)0.0006 (10)0.0045 (10)0.0017 (9)
O50.0353 (13)0.0321 (11)0.0285 (11)0.0009 (9)0.0104 (10)0.0064 (9)
C60.0211 (13)0.0261 (12)0.0221 (12)0.0013 (10)0.0055 (10)0.0006 (9)
O60.0248 (11)0.0307 (10)0.0342 (11)0.0025 (8)0.0114 (9)0.0011 (8)
C70.0201 (12)0.0253 (12)0.0202 (11)0.0016 (9)0.0058 (10)0.0018 (9)
O70.0249 (11)0.0298 (10)0.0285 (10)0.0019 (8)0.0028 (8)0.0036 (8)
C80.0206 (12)0.0234 (11)0.0199 (11)0.0004 (9)0.0035 (9)0.0024 (9)
O80.0342 (12)0.0326 (10)0.0221 (10)0.0001 (9)0.0075 (9)0.0044 (8)
Geometric parameters (Å, º) top
Mn1—C31.807 (3)Mn2—Br12.5215 (5)
Mn1—C21.820 (3)Mn2—Br22.5230 (5)
Mn1—C41.884 (3)C1—O11.134 (4)
Mn1—C11.892 (3)C2—O21.147 (4)
Mn1—Br22.5296 (5)C3—O31.144 (4)
Mn1—Br12.5315 (5)C4—O41.136 (4)
Mn2—C61.813 (3)C5—O51.132 (4)
Mn2—C71.815 (3)C6—O61.142 (4)
Mn2—C51.878 (3)C7—O71.145 (4)
Mn2—C81.895 (3)C8—O81.135 (4)
C3—Mn1—C290.57 (13)C5—Mn2—C8176.71 (13)
C3—Mn1—C490.53 (12)C6—Mn2—Br192.27 (9)
C2—Mn1—C490.76 (12)C7—Mn2—Br1176.61 (9)
C3—Mn1—C190.57 (13)C5—Mn2—Br188.08 (9)
C2—Mn1—C191.67 (12)C8—Mn2—Br189.40 (9)
C4—Mn1—C1177.32 (13)C6—Mn2—Br2176.82 (9)
C3—Mn1—Br293.26 (9)C7—Mn2—Br292.06 (9)
C2—Mn1—Br2176.15 (9)C5—Mn2—Br289.31 (9)
C4—Mn1—Br289.57 (9)C8—Mn2—Br288.36 (9)
C1—Mn1—Br287.93 (9)Br1—Mn2—Br284.632 (16)
C3—Mn1—Br1177.54 (9)Mn2—Br1—Mn195.533 (16)
C2—Mn1—Br191.88 (9)Mn2—Br2—Mn195.543 (17)
C4—Mn1—Br189.66 (9)O1—C1—Mn1178.0 (3)
C1—Mn1—Br189.13 (9)O2—C2—Mn1179.1 (3)
Br2—Mn1—Br184.291 (16)O3—C3—Mn1178.4 (3)
C6—Mn2—C791.05 (13)O4—C4—Mn1178.3 (3)
C6—Mn2—C591.33 (13)O5—C5—Mn2178.8 (3)
C7—Mn2—C591.15 (12)O6—C6—Mn2179.2 (3)
C6—Mn2—C890.87 (13)O7—C7—Mn2179.0 (3)
C7—Mn2—C891.25 (12)O8—C8—Mn2179.2 (3)
C6—Mn2—Br1—Mn1179.43 (9)C7—Mn2—Br2—Mn1179.09 (9)
C5—Mn2—Br1—Mn189.32 (9)C5—Mn2—Br2—Mn187.97 (9)
C8—Mn2—Br1—Mn188.58 (9)C8—Mn2—Br2—Mn189.72 (8)
Br2—Mn2—Br1—Mn10.166 (15)Br1—Mn2—Br2—Mn10.166 (15)
C2—Mn1—Br1—Mn2179.48 (9)C3—Mn1—Br2—Mn2179.63 (9)
C4—Mn1—Br1—Mn289.76 (9)C4—Mn1—Br2—Mn289.87 (9)
C1—Mn1—Br1—Mn287.84 (9)C1—Mn1—Br2—Mn289.17 (9)
Br2—Mn1—Br1—Mn20.165 (15)Br1—Mn1—Br2—Mn20.165 (15)
 

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