Di-μ-bromo-2κ²Br:2′κ²Br-bis­[bis­(μ-acetylacetonato-1κO:2κO′)bromo-2κBr-bis­(tetra­hydro­furan-1κO)cadmium(II)nickel(II)]

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.

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            superseded by _reflns_threshold_expression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            superseded by _reflns_number_gt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

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)]

Crystal data

[Cd2Ni2Br4(C5H7O2)4(C4H8O)4]	F(000) = 1328
Mr = 1346.68	Dx = 1.830 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P2yn	Cell parameters from 25 reflections
a = 10.143 (3) Å	θ = 18.7–25.8°
b = 11.378 (12) Å	µ = 4.94 mm^−1
c = 21.483 (2) Å	T = 173 K
β = 99.66 (3)°	Block, light blue
V = 2444 (3) Å^3	0.06 × 0.03 × 0.02 mm
Z = 2

Data collection

Enraf–Nonius CAD-4 diffractometer	4378 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.058
Graphite monochromator	θmax = 27.4°, θmin = 2.0°
ω/2θ scans	h = −13→12
Absorption correction: ψ scan (North et al., 1968)	k = 0→14
Tmin = 0.768, Tmax = 0.906	l = 0→27
5686 measured reflections	3 standard reflections every 600 min
5544 independent reflections	intensity decay: −2.4%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.067	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.195	H-atom parameters constrained
S = 1.12	w = 1/[σ^2(Fo^2) + (0.1177P)^2 + 10.9432P] where P = (Fo^2 + 2Fc^2)/3
5544 reflections	(Δ/σ)max = 0.001
257 parameters	Δρmax = 3.91 e Å^−3
0 restraints	Δρmin = −2.02 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Cd	−0.08354 (5)	0.65873 (4)	0.00555 (2)	0.02774 (17)
Br1	0.16528 (7)	0.56536 (7)	0.01366 (5)	0.0402 (2)
Br2	−0.12110 (10)	0.80114 (8)	−0.08634 (4)	0.0449 (2)
Ni	−0.18284 (8)	0.73867 (8)	0.14021 (4)	0.0257 (2)
O1	−0.0237 (5)	0.7647 (4)	0.0971 (2)	0.0278 (10)
O2	−0.0809 (5)	0.7846 (5)	0.2234 (2)	0.0323 (11)
O3	−0.2706 (5)	0.6913 (5)	0.0533 (2)	0.0290 (10)
O4	−0.3488 (5)	0.7103 (5)	0.1758 (2)	0.0330 (11)
O5	−0.2430 (6)	0.9148 (5)	0.1201 (3)	0.0379 (13)
O6	−0.1189 (5)	0.5639 (5)	0.1532 (3)	0.0409 (14)
C1	0.0752 (7)	0.8334 (6)	0.1208 (4)	0.0295 (15)
C2	0.1012 (7)	0.8695 (7)	0.1820 (4)	0.0328 (15)
H2	0.1756	0.9205	0.1931	0.039*
C3	0.0289 (7)	0.8391 (7)	0.2313 (4)	0.0329 (16)
C4	0.1622 (8)	0.8716 (7)	0.0745 (4)	0.0359 (17)
H4A	0.1985	0.8022	0.0562	0.054*
H4B	0.2360	0.9198	0.0962	0.054*
H4C	0.1090	0.9178	0.0407	0.054*
C5	0.0876 (9)	0.8701 (10)	0.2976 (4)	0.050 (2)
H5A	0.0162	0.8953	0.3202	0.075*
H5B	0.1522	0.9342	0.2975	0.075*
H5C	0.1329	0.8013	0.3187	0.075*
C6	−0.3975 (7)	0.6782 (6)	0.0360 (4)	0.0295 (15)
C7	−0.4892 (7)	0.6813 (7)	0.0769 (4)	0.0361 (17)
H7	−0.5807	0.6749	0.0582	0.043*
C8	−0.4625 (7)	0.6926 (7)	0.1425 (4)	0.0326 (16)
C9	−0.4433 (8)	0.6573 (8)	−0.0320 (4)	0.0404 (18)
H9A	−0.4030	0.5847	−0.0446	0.061*
H9B	−0.4162	0.7234	−0.0562	0.061*
H9C	−0.5409	0.6500	−0.0402	0.061*
C10	−0.5784 (8)	0.6860 (9)	0.1779 (4)	0.043 (2)
H10A	−0.5470	0.6572	0.2208	0.065*
H10B	−0.6462	0.6321	0.1560	0.065*
H10C	−0.6176	0.7644	0.1799	0.065*
C11	−0.2409 (15)	0.9765 (9)	0.0630 (5)	0.073 (4)
H11A	−0.2860	0.9298	0.0267	0.088*
H11B	−0.1475	0.9911	0.0573	0.088*
C12	−0.3118 (15)	1.0893 (10)	0.0670 (6)	0.071 (3)
H12A	−0.3861	1.0979	0.0310	0.085*
H12B	−0.2498	1.1565	0.0669	0.085*
C13	−0.3644 (13)	1.0833 (11)	0.1286 (5)	0.066 (3)
H13A	−0.3573	1.1606	0.1501	0.079*
H13B	−0.4590	1.0575	0.1218	0.079*
C14	−0.2765 (11)	0.9948 (9)	0.1660 (5)	0.053 (2)
H14A	−0.1952	1.0325	0.1896	0.063*
H14B	−0.3244	0.9541	0.1963	0.063*
C15	−0.2086 (8)	0.4681 (7)	0.1588 (4)	0.0392 (18)
H15A	−0.2680	0.4538	0.1181	0.047*
H15B	−0.2646	0.4858	0.1912	0.047*
C16	−0.1215 (10)	0.3622 (8)	0.1779 (5)	0.047 (2)
H16A	−0.1090	0.3149	0.1406	0.056*
H16B	−0.1600	0.3117	0.2078	0.056*
C17	0.0103 (10)	0.4177 (10)	0.2095 (6)	0.059 (3)
H17A	0.0097	0.4329	0.2549	0.071*
H17B	0.0873	0.3666	0.2054	0.071*
C18	0.0156 (9)	0.5275 (9)	0.1748 (5)	0.052 (2)
H18A	0.0642	0.5882	0.2027	0.063*
H18B	0.0626	0.5152	0.1385	0.063*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd	0.0229 (3)	0.0249 (3)	0.0367 (3)	0.00307 (18)	0.0088 (2)	−0.0037 (2)
Br1	0.0188 (3)	0.0286 (4)	0.0741 (6)	−0.0005 (3)	0.0101 (3)	−0.0128 (4)
Br2	0.0529 (5)	0.0390 (5)	0.0448 (5)	0.0085 (4)	0.0141 (4)	0.0078 (4)
Ni	0.0182 (4)	0.0280 (5)	0.0316 (5)	−0.0013 (3)	0.0060 (3)	−0.0018 (3)
O1	0.019 (2)	0.028 (2)	0.037 (3)	−0.0027 (19)	0.0073 (19)	−0.002 (2)
O2	0.023 (2)	0.045 (3)	0.028 (2)	−0.006 (2)	0.0009 (19)	0.001 (2)
O3	0.019 (2)	0.033 (3)	0.035 (3)	0.0015 (19)	0.0049 (19)	−0.008 (2)
O4	0.022 (2)	0.037 (3)	0.041 (3)	−0.005 (2)	0.010 (2)	−0.006 (2)
O5	0.048 (3)	0.028 (3)	0.043 (3)	0.008 (2)	0.021 (2)	0.001 (2)
O6	0.024 (3)	0.026 (3)	0.070 (4)	0.004 (2)	0.003 (3)	0.006 (3)
C1	0.020 (3)	0.026 (3)	0.045 (4)	−0.001 (3)	0.009 (3)	−0.001 (3)
C2	0.023 (3)	0.032 (4)	0.044 (4)	−0.006 (3)	0.008 (3)	−0.002 (3)
C3	0.023 (3)	0.031 (4)	0.046 (4)	0.000 (3)	0.007 (3)	−0.002 (3)
C4	0.033 (4)	0.026 (4)	0.052 (5)	−0.006 (3)	0.020 (3)	−0.001 (3)
C5	0.033 (4)	0.067 (6)	0.048 (5)	−0.005 (4)	0.002 (4)	−0.017 (5)
C6	0.015 (3)	0.027 (3)	0.044 (4)	0.007 (3)	0.000 (3)	−0.009 (3)
C7	0.018 (3)	0.036 (4)	0.055 (5)	0.001 (3)	0.008 (3)	−0.012 (4)
C8	0.017 (3)	0.030 (4)	0.052 (4)	0.001 (3)	0.011 (3)	−0.004 (3)
C9	0.031 (4)	0.040 (4)	0.050 (5)	0.008 (3)	0.007 (3)	−0.008 (4)
C10	0.024 (4)	0.049 (5)	0.061 (5)	−0.004 (3)	0.018 (4)	−0.009 (4)
C11	0.129 (11)	0.044 (5)	0.060 (6)	0.041 (7)	0.055 (7)	0.024 (5)
C12	0.099 (9)	0.043 (6)	0.080 (8)	0.029 (6)	0.038 (7)	0.019 (5)
C13	0.073 (7)	0.067 (7)	0.066 (7)	0.025 (6)	0.034 (6)	0.003 (6)
C14	0.069 (6)	0.041 (5)	0.055 (5)	0.011 (5)	0.027 (5)	−0.011 (4)
C15	0.035 (4)	0.031 (4)	0.054 (5)	−0.005 (3)	0.014 (3)	0.002 (4)
C16	0.049 (5)	0.028 (4)	0.068 (6)	0.004 (4)	0.020 (4)	0.007 (4)
C17	0.046 (5)	0.056 (6)	0.075 (7)	0.015 (5)	0.009 (5)	0.017 (5)
C18	0.032 (4)	0.046 (5)	0.077 (7)	0.005 (4)	0.005 (4)	0.014 (5)

Geometric parameters (Å, º)

Cd—O1	2.301 (5)	C6—C9	1.476 (11)
Cd—O3	2.333 (5)	C7—C8	1.396 (12)
Cd—Br2	2.5328 (15)	C7—H7	0.9500
Cd—Br1^i	2.691 (3)	C8—C10	1.506 (10)
Cd—Br1	2.7168 (12)	C9—H9A	0.9800
Cd—Ni	3.3450 (11)	C9—H9B	0.9800
Br1—Cd^i	2.692 (3)	C9—H9C	0.9800
Ni—O2	1.979 (5)	C10—H10A	0.9800
Ni—O4	1.988 (5)	C10—H10B	0.9800
Ni—O3	2.002 (5)	C10—H10C	0.9800
Ni—O1	2.013 (5)	C11—C12	1.481 (14)
Ni—O6	2.096 (6)	C11—H11A	0.9900
Ni—O5	2.118 (6)	C11—H11B	0.9900
O1—C1	1.306 (8)	C12—C13	1.510 (15)
O2—C3	1.261 (9)	C12—H12A	0.9900
O3—C6	1.287 (8)	C12—H12B	0.9900
O4—C8	1.268 (9)	C13—C14	1.487 (15)
O5—C11	1.416 (11)	C13—H13A	0.9900
O5—C14	1.425 (10)	C13—H13B	0.9900
O6—C18	1.426 (10)	C14—H14A	0.9900
O6—C15	1.438 (9)	C14—H14B	0.9900
C1—C2	1.360 (11)	C15—C16	1.510 (12)
C1—C4	1.501 (10)	C15—H15A	0.9900
C2—C3	1.428 (11)	C15—H15B	0.9900
C2—H2	0.9500	C16—C17	1.531 (15)
C3—C5	1.492 (11)	C16—H16A	0.9900
C4—H4A	0.9800	C16—H16B	0.9900
C4—H4B	0.9800	C17—C18	1.460 (14)
C4—H4C	0.9800	C17—H17A	0.9900
C5—H5A	0.9800	C17—H17B	0.9900
C5—H5B	0.9800	C18—H18A	0.9900
C5—H5C	0.9800	C18—H18B	0.9900
C6—C7	1.382 (11)
O1—Cd—O3	69.99 (17)	H5B—C5—H5C	109.5
O1—Cd—Br2	108.36 (14)	O3—C6—C7	124.1 (7)
O3—Cd—Br2	102.37 (14)	O3—C6—C9	115.9 (7)
O1—Cd—Br1^i	131.14 (13)	C7—C6—C9	119.9 (7)
O3—Cd—Br1^i	88.02 (13)	C6—C7—C8	127.3 (7)
Br2—Cd—Br1^i	118.97 (5)	C6—C7—H7	116.3
O1—Cd—Br1	92.36 (12)	C8—C7—H7	116.3
O3—Cd—Br1	148.11 (13)	O4—C8—C7	126.1 (7)
Br2—Cd—Br1	108.47 (4)	O4—C8—C10	115.9 (7)
Br1^i—Cd—Br1	84.17 (5)	C7—C8—C10	118.0 (7)
O1—Cd—Ni	36.13 (12)	C6—C9—H9A	109.5
O3—Cd—Ni	36.03 (12)	C6—C9—H9B	109.5
Br2—Cd—Ni	118.19 (5)	H9A—C9—H9B	109.5
Br1^i—Cd—Ni	105.10 (3)	C6—C9—H9C	109.5
Br1—Cd—Ni	117.52 (3)	H9A—C9—H9C	109.5
Cd^i—Br1—Cd	95.84 (5)	H9B—C9—H9C	109.5
O2—Ni—O4	92.5 (2)	C8—C10—H10A	109.5
O2—Ni—O3	174.9 (2)	C8—C10—H10B	109.5
O4—Ni—O3	92.4 (2)	H10A—C10—H10B	109.5
O2—Ni—O1	92.2 (2)	C8—C10—H10C	109.5
O4—Ni—O1	175.3 (2)	H10A—C10—H10C	109.5
O3—Ni—O1	82.9 (2)	H10B—C10—H10C	109.5
O2—Ni—O6	91.5 (2)	O5—C11—C12	107.6 (8)
O4—Ni—O6	93.3 (2)	O5—C11—H11A	110.2
O3—Ni—O6	87.0 (2)	C12—C11—H11A	110.2
O1—Ni—O6	86.9 (2)	O5—C11—H11B	110.2
O2—Ni—O5	91.3 (2)	C12—C11—H11B	110.2
O4—Ni—O5	89.9 (2)	H11A—C11—H11B	108.5
O3—Ni—O5	89.8 (2)	C11—C12—C13	104.9 (9)
O1—Ni—O5	89.6 (2)	C11—C12—H12A	110.8
O6—Ni—O5	175.6 (2)	C13—C12—H12A	110.8
O2—Ni—Cd	131.70 (15)	C11—C12—H12B	110.8
O4—Ni—Cd	133.30 (15)	C13—C12—H12B	110.8
O3—Ni—Cd	43.25 (14)	H12A—C12—H12B	108.8
O1—Ni—Cd	42.38 (14)	C14—C13—C12	103.7 (8)
O6—Ni—Cd	74.10 (18)	C14—C13—H13A	111.0
O5—Ni—Cd	101.49 (15)	C12—C13—H13A	111.0
C1—O1—Ni	122.2 (5)	C14—C13—H13B	111.0
C1—O1—Cd	136.2 (5)	C12—C13—H13B	111.0
Ni—O1—Cd	101.5 (2)	H13A—C13—H13B	109.0
C3—O2—Ni	124.5 (5)	O5—C14—C13	104.4 (8)
C6—O3—Ni	124.5 (5)	O5—C14—H14A	110.9
C6—O3—Cd	134.6 (5)	C13—C14—H14A	110.9
Ni—O3—Cd	100.7 (2)	O5—C14—H14B	110.9
C8—O4—Ni	123.9 (5)	C13—C14—H14B	110.9
C11—O5—C14	108.8 (7)	H14A—C14—H14B	108.9
C11—O5—Ni	126.8 (5)	O6—C15—C16	106.2 (6)
C14—O5—Ni	123.9 (5)	O6—C15—H15A	110.5
C18—O6—C15	109.7 (6)	C16—C15—H15A	110.5
C18—O6—Ni	125.2 (5)	O6—C15—H15B	110.5
C15—O6—Ni	123.0 (5)	C16—C15—H15B	110.5
O1—C1—C2	124.6 (7)	H15A—C15—H15B	108.7
O1—C1—C4	114.5 (7)	C15—C16—C17	102.6 (7)
C2—C1—C4	120.9 (7)	C15—C16—H16A	111.2
C1—C2—C3	127.1 (7)	C17—C16—H16A	111.2
C1—C2—H2	116.5	C15—C16—H16B	111.2
C3—C2—H2	116.5	C17—C16—H16B	111.2
O2—C3—C2	124.9 (7)	H16A—C16—H16B	109.2
O2—C3—C5	116.5 (7)	C18—C17—C16	103.4 (8)
C2—C3—C5	118.6 (7)	C18—C17—H17A	111.1
C1—C4—H4A	109.5	C16—C17—H17A	111.1
C1—C4—H4B	109.5	C18—C17—H17B	111.1
H4A—C4—H4B	109.5	C16—C17—H17B	111.1
C1—C4—H4C	109.5	H17A—C17—H17B	109.1
H4A—C4—H4C	109.5	O6—C18—C17	107.4 (8)
H4B—C4—H4C	109.5	O6—C18—H18A	110.2
C3—C5—H5A	109.5	C17—C18—H18A	110.2
C3—C5—H5B	109.5	O6—C18—H18B	110.2
H5A—C5—H5B	109.5	C17—C18—H18B	110.2
C3—C5—H5C	109.5	H18A—C18—H18B	108.5
H5A—C5—H5C	109.5

Symmetry code: (i) −x, −y+1, −z.