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The title compound, [Cd2Ni2Br4(C5H7O2)4(C4H8O)4], is a tetra­nuclear coordination compound with two Ni and two Cd centres. The Ni atoms are octa­hedrally surrounded by two tetra­hydro­furan ligands in trans positions and two acetyl­acetonate ligands. One O atom of each acetyl­acetonate ligand acts as a bridging atom to a Cd atom. The two Cd atoms are bridged by two Br ligands and each of them bears one additional Br substituent. The mol­ecule is located on a crystallographic centre of inversion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806003643/bt6810sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806003643/bt6810Isup2.hkl
Contains datablock I

CCDC reference: 601123

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.013 Å
  • R factor = 0.067
  • wR factor = 0.195
  • Data-to-parameter ratio = 21.6

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level C DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given = 3.908 Test value = 3.600 DIFMX02_ALERT_1_C The maximum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 3.91 e/A   3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C11 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13 PLAT731_ALERT_1_C Bond Calc 2.717(3), Rep 2.7168(12) ...... 2.50 su-Rat CD -BR1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 3.345(4), Rep 3.3450(11) ...... 3.64 su-Rat CD -NI 1.555 1.555
Alert level G REFLE01_ALERT_1_G _reflns_observed_criterion is an old dataname which has been superseded by _reflns_threshold_expression REFLG01_ALERT_1_G _reflns_number_observed is an old dataname which has been superseded by _reflns_number_gt
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 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: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: SET4 (de Boer & Duisenberg, 1984); data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1990); software used to prepare material for publication: SHELXL97.

Di-µ-bromo-2κ2Br:2'κ2Br-bis[bis(µ-acetylacetonato-1κO:2κO')bromo- 2κBr-bis(tetrahydrofuran-1κO)cadmium(II)nickel(II)] top
Crystal data top
[Cd2Ni2Br4(C5H7O2)4(C4H8O)4]F(000) = 1328
Mr = 1346.68Dx = 1.830 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P2ynCell parameters from 25 reflections
a = 10.143 (3) Åθ = 18.7–25.8°
b = 11.378 (12) ŵ = 4.94 mm1
c = 21.483 (2) ÅT = 173 K
β = 99.66 (3)°Block, light blue
V = 2444 (3) Å30.06 × 0.03 × 0.02 mm
Z = 2
Data collection top
Enraf–Nonius CAD-4
diffractometer
4378 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.058
Graphite monochromatorθmax = 27.4°, θmin = 2.0°
ω/2θ scansh = 1312
Absorption correction: ψ scan
(North et al., 1968)
k = 014
Tmin = 0.768, Tmax = 0.906l = 027
5686 measured reflections3 standard reflections every 600 min
5544 independent reflections intensity decay: 2.4%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.067Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.195H-atom parameters constrained
S = 1.12 w = 1/[σ2(Fo2) + (0.1177P)2 + 10.9432P]
where P = (Fo2 + 2Fc2)/3
5544 reflections(Δ/σ)max = 0.001
257 parametersΔρmax = 3.91 e Å3
0 restraintsΔρmin = 2.02 e Å3
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 on F2 for ALL reflections except for 10 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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
Cd0.08354 (5)0.65873 (4)0.00555 (2)0.02774 (17)
Br10.16528 (7)0.56536 (7)0.01366 (5)0.0402 (2)
Br20.12110 (10)0.80114 (8)0.08634 (4)0.0449 (2)
Ni0.18284 (8)0.73867 (8)0.14021 (4)0.0257 (2)
O10.0237 (5)0.7647 (4)0.0971 (2)0.0278 (10)
O20.0809 (5)0.7846 (5)0.2234 (2)0.0323 (11)
O30.2706 (5)0.6913 (5)0.0533 (2)0.0290 (10)
O40.3488 (5)0.7103 (5)0.1758 (2)0.0330 (11)
O50.2430 (6)0.9148 (5)0.1201 (3)0.0379 (13)
O60.1189 (5)0.5639 (5)0.1532 (3)0.0409 (14)
C10.0752 (7)0.8334 (6)0.1208 (4)0.0295 (15)
C20.1012 (7)0.8695 (7)0.1820 (4)0.0328 (15)
H20.17560.92050.19310.039*
C30.0289 (7)0.8391 (7)0.2313 (4)0.0329 (16)
C40.1622 (8)0.8716 (7)0.0745 (4)0.0359 (17)
H4A0.19850.80220.05620.054*
H4B0.23600.91980.09620.054*
H4C0.10900.91780.04070.054*
C50.0876 (9)0.8701 (10)0.2976 (4)0.050 (2)
H5A0.01620.89530.32020.075*
H5B0.15220.93420.29750.075*
H5C0.13290.80130.31870.075*
C60.3975 (7)0.6782 (6)0.0360 (4)0.0295 (15)
C70.4892 (7)0.6813 (7)0.0769 (4)0.0361 (17)
H70.58070.67490.05820.043*
C80.4625 (7)0.6926 (7)0.1425 (4)0.0326 (16)
C90.4433 (8)0.6573 (8)0.0320 (4)0.0404 (18)
H9A0.40300.58470.04460.061*
H9B0.41620.72340.05620.061*
H9C0.54090.65000.04020.061*
C100.5784 (8)0.6860 (9)0.1779 (4)0.043 (2)
H10A0.54700.65720.22080.065*
H10B0.64620.63210.15600.065*
H10C0.61760.76440.17990.065*
C110.2409 (15)0.9765 (9)0.0630 (5)0.073 (4)
H11A0.28600.92980.02670.088*
H11B0.14750.99110.05730.088*
C120.3118 (15)1.0893 (10)0.0670 (6)0.071 (3)
H12A0.38611.09790.03100.085*
H12B0.24981.15650.06690.085*
C130.3644 (13)1.0833 (11)0.1286 (5)0.066 (3)
H13A0.35731.16060.15010.079*
H13B0.45901.05750.12180.079*
C140.2765 (11)0.9948 (9)0.1660 (5)0.053 (2)
H14A0.19521.03250.18960.063*
H14B0.32440.95410.19630.063*
C150.2086 (8)0.4681 (7)0.1588 (4)0.0392 (18)
H15A0.26800.45380.11810.047*
H15B0.26460.48580.19120.047*
C160.1215 (10)0.3622 (8)0.1779 (5)0.047 (2)
H16A0.10900.31490.14060.056*
H16B0.16000.31170.20780.056*
C170.0103 (10)0.4177 (10)0.2095 (6)0.059 (3)
H17A0.00970.43290.25490.071*
H17B0.08730.36660.20540.071*
C180.0156 (9)0.5275 (9)0.1748 (5)0.052 (2)
H18A0.06420.58820.20270.063*
H18B0.06260.51520.13850.063*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd0.0229 (3)0.0249 (3)0.0367 (3)0.00307 (18)0.0088 (2)0.0037 (2)
Br10.0188 (3)0.0286 (4)0.0741 (6)0.0005 (3)0.0101 (3)0.0128 (4)
Br20.0529 (5)0.0390 (5)0.0448 (5)0.0085 (4)0.0141 (4)0.0078 (4)
Ni0.0182 (4)0.0280 (5)0.0316 (5)0.0013 (3)0.0060 (3)0.0018 (3)
O10.019 (2)0.028 (2)0.037 (3)0.0027 (19)0.0073 (19)0.002 (2)
O20.023 (2)0.045 (3)0.028 (2)0.006 (2)0.0009 (19)0.001 (2)
O30.019 (2)0.033 (3)0.035 (3)0.0015 (19)0.0049 (19)0.008 (2)
O40.022 (2)0.037 (3)0.041 (3)0.005 (2)0.010 (2)0.006 (2)
O50.048 (3)0.028 (3)0.043 (3)0.008 (2)0.021 (2)0.001 (2)
O60.024 (3)0.026 (3)0.070 (4)0.004 (2)0.003 (3)0.006 (3)
C10.020 (3)0.026 (3)0.045 (4)0.001 (3)0.009 (3)0.001 (3)
C20.023 (3)0.032 (4)0.044 (4)0.006 (3)0.008 (3)0.002 (3)
C30.023 (3)0.031 (4)0.046 (4)0.000 (3)0.007 (3)0.002 (3)
C40.033 (4)0.026 (4)0.052 (5)0.006 (3)0.020 (3)0.001 (3)
C50.033 (4)0.067 (6)0.048 (5)0.005 (4)0.002 (4)0.017 (5)
C60.015 (3)0.027 (3)0.044 (4)0.007 (3)0.000 (3)0.009 (3)
C70.018 (3)0.036 (4)0.055 (5)0.001 (3)0.008 (3)0.012 (4)
C80.017 (3)0.030 (4)0.052 (4)0.001 (3)0.011 (3)0.004 (3)
C90.031 (4)0.040 (4)0.050 (5)0.008 (3)0.007 (3)0.008 (4)
C100.024 (4)0.049 (5)0.061 (5)0.004 (3)0.018 (4)0.009 (4)
C110.129 (11)0.044 (5)0.060 (6)0.041 (7)0.055 (7)0.024 (5)
C120.099 (9)0.043 (6)0.080 (8)0.029 (6)0.038 (7)0.019 (5)
C130.073 (7)0.067 (7)0.066 (7)0.025 (6)0.034 (6)0.003 (6)
C140.069 (6)0.041 (5)0.055 (5)0.011 (5)0.027 (5)0.011 (4)
C150.035 (4)0.031 (4)0.054 (5)0.005 (3)0.014 (3)0.002 (4)
C160.049 (5)0.028 (4)0.068 (6)0.004 (4)0.020 (4)0.007 (4)
C170.046 (5)0.056 (6)0.075 (7)0.015 (5)0.009 (5)0.017 (5)
C180.032 (4)0.046 (5)0.077 (7)0.005 (4)0.005 (4)0.014 (5)
Geometric parameters (Å, º) top
Cd—O12.301 (5)C6—C91.476 (11)
Cd—O32.333 (5)C7—C81.396 (12)
Cd—Br22.5328 (15)C7—H70.9500
Cd—Br1i2.691 (3)C8—C101.506 (10)
Cd—Br12.7168 (12)C9—H9A0.9800
Cd—Ni3.3450 (11)C9—H9B0.9800
Br1—Cdi2.692 (3)C9—H9C0.9800
Ni—O21.979 (5)C10—H10A0.9800
Ni—O41.988 (5)C10—H10B0.9800
Ni—O32.002 (5)C10—H10C0.9800
Ni—O12.013 (5)C11—C121.481 (14)
Ni—O62.096 (6)C11—H11A0.9900
Ni—O52.118 (6)C11—H11B0.9900
O1—C11.306 (8)C12—C131.510 (15)
O2—C31.261 (9)C12—H12A0.9900
O3—C61.287 (8)C12—H12B0.9900
O4—C81.268 (9)C13—C141.487 (15)
O5—C111.416 (11)C13—H13A0.9900
O5—C141.425 (10)C13—H13B0.9900
O6—C181.426 (10)C14—H14A0.9900
O6—C151.438 (9)C14—H14B0.9900
C1—C21.360 (11)C15—C161.510 (12)
C1—C41.501 (10)C15—H15A0.9900
C2—C31.428 (11)C15—H15B0.9900
C2—H20.9500C16—C171.531 (15)
C3—C51.492 (11)C16—H16A0.9900
C4—H4A0.9800C16—H16B0.9900
C4—H4B0.9800C17—C181.460 (14)
C4—H4C0.9800C17—H17A0.9900
C5—H5A0.9800C17—H17B0.9900
C5—H5B0.9800C18—H18A0.9900
C5—H5C0.9800C18—H18B0.9900
C6—C71.382 (11)
O1—Cd—O369.99 (17)H5B—C5—H5C109.5
O1—Cd—Br2108.36 (14)O3—C6—C7124.1 (7)
O3—Cd—Br2102.37 (14)O3—C6—C9115.9 (7)
O1—Cd—Br1i131.14 (13)C7—C6—C9119.9 (7)
O3—Cd—Br1i88.02 (13)C6—C7—C8127.3 (7)
Br2—Cd—Br1i118.97 (5)C6—C7—H7116.3
O1—Cd—Br192.36 (12)C8—C7—H7116.3
O3—Cd—Br1148.11 (13)O4—C8—C7126.1 (7)
Br2—Cd—Br1108.47 (4)O4—C8—C10115.9 (7)
Br1i—Cd—Br184.17 (5)C7—C8—C10118.0 (7)
O1—Cd—Ni36.13 (12)C6—C9—H9A109.5
O3—Cd—Ni36.03 (12)C6—C9—H9B109.5
Br2—Cd—Ni118.19 (5)H9A—C9—H9B109.5
Br1i—Cd—Ni105.10 (3)C6—C9—H9C109.5
Br1—Cd—Ni117.52 (3)H9A—C9—H9C109.5
Cdi—Br1—Cd95.84 (5)H9B—C9—H9C109.5
O2—Ni—O492.5 (2)C8—C10—H10A109.5
O2—Ni—O3174.9 (2)C8—C10—H10B109.5
O4—Ni—O392.4 (2)H10A—C10—H10B109.5
O2—Ni—O192.2 (2)C8—C10—H10C109.5
O4—Ni—O1175.3 (2)H10A—C10—H10C109.5
O3—Ni—O182.9 (2)H10B—C10—H10C109.5
O2—Ni—O691.5 (2)O5—C11—C12107.6 (8)
O4—Ni—O693.3 (2)O5—C11—H11A110.2
O3—Ni—O687.0 (2)C12—C11—H11A110.2
O1—Ni—O686.9 (2)O5—C11—H11B110.2
O2—Ni—O591.3 (2)C12—C11—H11B110.2
O4—Ni—O589.9 (2)H11A—C11—H11B108.5
O3—Ni—O589.8 (2)C11—C12—C13104.9 (9)
O1—Ni—O589.6 (2)C11—C12—H12A110.8
O6—Ni—O5175.6 (2)C13—C12—H12A110.8
O2—Ni—Cd131.70 (15)C11—C12—H12B110.8
O4—Ni—Cd133.30 (15)C13—C12—H12B110.8
O3—Ni—Cd43.25 (14)H12A—C12—H12B108.8
O1—Ni—Cd42.38 (14)C14—C13—C12103.7 (8)
O6—Ni—Cd74.10 (18)C14—C13—H13A111.0
O5—Ni—Cd101.49 (15)C12—C13—H13A111.0
C1—O1—Ni122.2 (5)C14—C13—H13B111.0
C1—O1—Cd136.2 (5)C12—C13—H13B111.0
Ni—O1—Cd101.5 (2)H13A—C13—H13B109.0
C3—O2—Ni124.5 (5)O5—C14—C13104.4 (8)
C6—O3—Ni124.5 (5)O5—C14—H14A110.9
C6—O3—Cd134.6 (5)C13—C14—H14A110.9
Ni—O3—Cd100.7 (2)O5—C14—H14B110.9
C8—O4—Ni123.9 (5)C13—C14—H14B110.9
C11—O5—C14108.8 (7)H14A—C14—H14B108.9
C11—O5—Ni126.8 (5)O6—C15—C16106.2 (6)
C14—O5—Ni123.9 (5)O6—C15—H15A110.5
C18—O6—C15109.7 (6)C16—C15—H15A110.5
C18—O6—Ni125.2 (5)O6—C15—H15B110.5
C15—O6—Ni123.0 (5)C16—C15—H15B110.5
O1—C1—C2124.6 (7)H15A—C15—H15B108.7
O1—C1—C4114.5 (7)C15—C16—C17102.6 (7)
C2—C1—C4120.9 (7)C15—C16—H16A111.2
C1—C2—C3127.1 (7)C17—C16—H16A111.2
C1—C2—H2116.5C15—C16—H16B111.2
C3—C2—H2116.5C17—C16—H16B111.2
O2—C3—C2124.9 (7)H16A—C16—H16B109.2
O2—C3—C5116.5 (7)C18—C17—C16103.4 (8)
C2—C3—C5118.6 (7)C18—C17—H17A111.1
C1—C4—H4A109.5C16—C17—H17A111.1
C1—C4—H4B109.5C18—C17—H17B111.1
H4A—C4—H4B109.5C16—C17—H17B111.1
C1—C4—H4C109.5H17A—C17—H17B109.1
H4A—C4—H4C109.5O6—C18—C17107.4 (8)
H4B—C4—H4C109.5O6—C18—H18A110.2
C3—C5—H5A109.5C17—C18—H18A110.2
C3—C5—H5B109.5O6—C18—H18B110.2
H5A—C5—H5B109.5C17—C18—H18B110.2
C3—C5—H5C109.5H18A—C18—H18B108.5
H5A—C5—H5C109.5
Symmetry code: (i) x, y+1, z.
 

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