The title complex, [Ni2Br2(C2H8N2)4]Br2, consists of two bromide anions and a complex dication. The dication is a centrosymmetric unit of two Ni atoms bridged unsymmetrically by two Br atoms. The Ni atoms are pseudo-octahedral, six-coordinate, with four N atoms from two 1,2-diaminoethane ligands completing the coordination environment.
Supporting information
CCDC reference: 601262
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.008 Å
- R factor = 0.035
- wR factor = 0.049
- Data-to-parameter ratio = 22.3
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Br1 - Ni1_a .. 12.55 su
Alert level C
PLAT021_ALERT_1_C Ratio Unique / Expected Reflections too High ... 1.04
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8
PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1 ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N3 - H6 ... ?
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 11
NI1 -BR1 -NI1 -N3 86.00 1.00 1.555 1.555 3.656 3.656
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 23
N2 -NI1 -N4 -C4 -5.00 1.00 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 29
N4 -NI1 -N2 -C2 -67.00 1.00 1.555 1.555 1.555 1.555
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 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
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1999); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN for Windows (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: TEXSAN for Windows; molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN for Windows.
Di-µ-bromo-bis[bis(1,2-diaminoethane-
κ2N,
N)nickel(II)]
dibromide
top
Crystal data top
[Ni2Br2(C2H8N2)4]Br2 | F(000) = 664 |
Mr = 677.41 | Dx = 2.097 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 6.6235 (14) Å | θ = 23.3–25.1° |
b = 11.329 (2) Å | µ = 9.23 mm−1 |
c = 14.3470 (17) Å | T = 294 K |
β = 94.753 (15)° | Prism, blue |
V = 1072.9 (3) Å3 | 0.50 × 0.30 × 0.30 mm |
Z = 2 | |
Data collection top
Rigaku AFC-7R diffractometer | 2250 reflections with I > 3σ(I) |
Radiation source: Rigaku rotating anode | Rint = 0.034 |
Graphite monochromator | θmax = 32.5°, θmin = 1.8° |
ω–2θ scans | h = 0→10 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→17 |
Tmin = 0.035, Tmax = 0.063 | l = −21→21 |
4342 measured reflections | 3 standard reflections every 150 reflections |
4049 independent reflections | intensity decay: 2.7% |
Refinement top
Refinement on F | 0 constraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.035 | Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo) + 0.00106|Fo|2] |
wR(F2) = 0.049 | (Δ/σ)max = 0.005 |
S = 1.04 | Δρmax = 0.93 e Å−3 |
2250 reflections | Δρmin = −0.80 e Å−3 |
101 parameters | Extinction correction: Zachariasen (1967), equation (3), Acta Cryst.(1968) A24, p213. |
0 restraints | Extinction coefficient: 0.0000011 (1) |
Special details top
Experimental. The scan width was (1.05 + 0.35tanθ)° with an ω scan speed of 16° per minute
(up to 5 scans to achieve I/σ(I) > 10). Stationary background counts were
recorded at each end of the scan, and the scan time:background time ratio was
2:1. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Br1 | 0.30343 (6) | 0.10561 (4) | 0.47055 (3) | 0.0336 (1) | |
Br2 | 0.68101 (8) | 0.13052 (4) | 0.19650 (4) | 0.0448 (1) | |
Ni1 | 0.65731 (7) | 0.13017 (5) | 0.56562 (4) | 0.0261 (1) | |
N1 | 0.9295 (5) | 0.1134 (3) | 0.6480 (3) | 0.0341 (9) | |
N2 | 0.5313 (6) | 0.1069 (3) | 0.6920 (3) | 0.0345 (9) | |
N3 | 0.6383 (6) | 0.3148 (3) | 0.5807 (3) | 0.036 (1) | |
N4 | 0.7891 (5) | 0.1761 (3) | 0.4441 (2) | 0.0340 (9) | |
C1 | 0.8820 (8) | 0.0650 (5) | 0.7394 (3) | 0.048 (1) | |
C2 | 0.6916 (9) | 0.1221 (5) | 0.7680 (3) | 0.047 (1) | |
C3 | 0.6587 (9) | 0.3677 (4) | 0.4880 (4) | 0.050 (1) | |
C4 | 0.8271 (8) | 0.3040 (5) | 0.4436 (3) | 0.045 (1) | |
H1 | 1.0175 | 0.0613 | 0.6189 | 0.041* | |
H2 | 0.9925 | 0.1885 | 0.6564 | 0.041* | |
H3 | 0.4276 | 0.1637 | 0.6979 | 0.041* | |
H4 | 0.4756 | 0.0298 | 0.6947 | 0.041* | |
H5 | 0.5112 | 0.3356 | 0.6022 | 0.043* | |
H6 | 0.7443 | 0.3420 | 0.6241 | 0.043* | |
H7 | 0.9136 | 0.1350 | 0.4418 | 0.041* | |
H8 | 0.7002 | 0.1555 | 0.3912 | 0.041* | |
H9 | 0.8626 | −0.0179 | 0.7343 | 0.058* | |
H10 | 0.9907 | 0.0812 | 0.7851 | 0.058* | |
H11 | 0.7148 | 0.2038 | 0.7791 | 0.056* | |
H12 | 0.6520 | 0.0858 | 0.8233 | 0.056* | |
H13 | 0.5352 | 0.3591 | 0.4499 | 0.059* | |
H14 | 0.6908 | 0.4491 | 0.4947 | 0.059* | |
H15 | 0.9527 | 0.3204 | 0.4781 | 0.054* | |
H16 | 0.8321 | 0.3304 | 0.3810 | 0.054* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Br1 | 0.0248 (2) | 0.0350 (2) | 0.0405 (2) | 0.0031 (2) | −0.0007 (2) | −0.0060 (2) |
Br2 | 0.0489 (3) | 0.0384 (3) | 0.0482 (3) | 0.0036 (2) | 0.0110 (2) | 0.0110 (2) |
Ni1 | 0.0248 (2) | 0.0290 (3) | 0.0247 (2) | −0.0007 (2) | 0.0036 (2) | −0.0010 (2) |
N1 | 0.030 (2) | 0.034 (2) | 0.038 (2) | 0.000 (1) | 0.002 (1) | −0.007 (1) |
N2 | 0.035 (2) | 0.041 (2) | 0.028 (2) | −0.003 (2) | 0.007 (1) | 0.002 (2) |
N3 | 0.043 (2) | 0.032 (2) | 0.035 (2) | 0.002 (2) | 0.010 (2) | 0.000 (2) |
N4 | 0.033 (2) | 0.041 (2) | 0.028 (2) | 0.001 (2) | 0.006 (1) | 0.002 (1) |
C1 | 0.043 (3) | 0.068 (3) | 0.034 (2) | 0.007 (2) | −0.006 (2) | 0.006 (2) |
C2 | 0.053 (3) | 0.059 (3) | 0.030 (2) | 0.003 (2) | 0.004 (2) | −0.006 (2) |
C3 | 0.059 (3) | 0.039 (3) | 0.052 (3) | 0.012 (2) | 0.013 (2) | 0.015 (2) |
C4 | 0.054 (3) | 0.043 (3) | 0.041 (3) | 0.001 (2) | 0.024 (2) | 0.009 (2) |
Geometric parameters (Å, º) top
Br1—Ni1 | 2.6272 (8) | N2—H3 | 0.950 |
Br1—Ni1i | 2.7377 (8) | N2—H4 | 0.950 |
Ni1—N1 | 2.081 (4) | N3—H5 | 0.950 |
Ni1—N2 | 2.075 (4) | N3—H6 | 0.950 |
Ni1—N3 | 2.108 (4) | N4—H7 | 0.950 |
Ni1—N4 | 2.079 (4) | N4—H8 | 0.950 |
N1—C1 | 1.480 (6) | C1—H9 | 0.950 |
N2—C2 | 1.467 (6) | C1—H10 | 0.950 |
N3—C3 | 1.475 (6) | C2—H11 | 0.950 |
N4—C4 | 1.471 (6) | C2—H12 | 0.950 |
C1—C2 | 1.504 (8) | C3—H13 | 0.950 |
C3—C4 | 1.512 (7) | C3—H14 | 0.950 |
N1—H1 | 0.950 | C4—H15 | 0.950 |
N1—H2 | 0.950 | C4—H16 | 0.950 |
| | | |
Br1···Br1i | 3.586 (1) | Br2···H2ii | 2.445 |
Ni1···Ni1i | 3.992 (1) | Br2···N1ii | 3.389 (4) |
Br2···N1ii | 3.389 (4) | Br2···H4i | 2.661 |
Br2···N2i | 3.484 (4) | Br2···N2i | 3.484 (4) |
Br2···N3iii | 3.627 (4) | Br2···H5iii | 2.693 |
Br2···N4 | 3.603 (4) | Br2···H8 | 2.800 |
Br1···H7iv | 2.603 | Br2···H3iii | 2.846 |
Br1···N4iv | 3.489 (4) | | |
| | | |
Ni1—Br1—Ni1i | 96.15 (2) | C2—N2—H4 | 109.75 |
Br1—Ni1—Br1i | 83.85 (2) | H3—N2—H4 | 109.46 |
Br1—Ni1—N1 | 168.2 (1) | Ni1—N3—H5 | 109.97 |
Br1—Ni1—N2 | 91.9 (1) | Ni1—N3—H6 | 109.97 |
Br1—Ni1—N3 | 95.7 (1) | C3—N3—H5 | 109.98 |
Br1—Ni1—N4 | 90.5 (1) | C3—N3—H6 | 109.98 |
Br1i—Ni1—N1 | 85.8 (1) | H5—N3—H6 | 109.46 |
Br1i—Ni1—N2 | 95.3 (1) | Ni1—N4—H7 | 109.46 |
Br1i—Ni1—N3 | 174.4 (1) | Ni1—N4—H8 | 109.46 |
Br1i—Ni1—N4 | 91.8 (1) | C4—N4—H7 | 109.46 |
N1—Ni1—N2 | 83.4 (2) | C4—N4—H8 | 109.46 |
N1—Ni1—N3 | 95.1 (1) | H7—N4—H8 | 109.46 |
N1—Ni1—N4 | 95.4 (1) | N1—C1—H9 | 109.58 |
N2—Ni1—N3 | 90.3 (1) | N1—C1—H10 | 109.58 |
N2—Ni1—N4 | 172.6 (2) | C2—C1—H9 | 109.58 |
N3—NI1—N4 | 82.5 (1) | C2—C1—H10 | 109.57 |
Ni1—N1—C1 | 107.4 (3) | H9—C1—H10 | 109.46 |
Ni1—N2—C2 | 108.4 (3) | N2—C2—H11 | 109.69 |
Ni1—N3—C3 | 107.5 (3) | N2—C2—H12 | 109.69 |
Ni1—N4—C4 | 109.5 (3) | C1—C2—H11 | 109.69 |
N1—C1—C2 | 109.1 (4) | C1—C2—H12 | 109.69 |
N2—C2—C1 | 108.6 (4) | H11—C2—H12 | 109.46 |
N3—C3—C4 | 108.1 (4) | N3—C3—H13 | 109.81 |
N4—C4—C3 | 109.6 (4) | N3—C3—H14 | 109.81 |
Ni1—N1—H1 | 109.99 | C4—C3—H13 | 109.81 |
Ni1—N1—H2 | 109.99 | C4—C3—H14 | 109.81 |
C1—N1—H1 | 109.98 | H13—C3—H14 | 109.46 |
C1—N1—H2 | 109.99 | N4—C4—H15 | 109.44 |
H1—N1—H2 | 109.46 | N4—C4—H16 | 109.44 |
Ni1—N2—H3 | 109.75 | C3—C4—H15 | 109.45 |
Ni1—N2—H4 | 109.75 | C3—C4—H16 | 109.45 |
C2—N2—H3 | 109.75 | H15—C4—H16 | 109.46 |
| | | |
Br1i—Ni1—Br1—Ni1i | 0 | Ni1—N4—C4—C3 | −35.7 (5) |
Br1—Ni1—N1—C1 | −52.7 (7) | N1—Ni1—N2—C2 | 14.1 (3) |
Br1—Ni1—N2—C2 | −176.7 (3) | N1—Ni1—N3—C3 | 113.8 (3) |
Br1—Ni1—N3—C3 | −70.9 (3) | N1—Ni1—N4—C4 | −85.1 (3) |
Br1—Ni1—N4—C4 | 105.0 (3) | N1—C1—C2—N2 | 54.1 (6) |
Br1—Ni1i—N1i—C1i | 81.5 (3) | N2—Ni1—N1—C1 | 14.4 (3) |
Br1—Ni1i—N2i—C2i | −99.3 (3) | N2—Ni1—N3—C3 | −162.9 (3) |
Br1—Ni1i—N4i—C4i | 171.1 (3) | N2—Ni1—N4—C4 | −5 (1) |
Ni1—Br1—Ni1i—N1i | −174.3 (1) | N3—Ni1—N1—C1 | 104.1 (3) |
Ni1—Br1—Ni1i—N2i | −91.4 (1) | N3—Ni1—N2—C2 | −81.0 (3) |
Ni1—Br1—Ni1i—N3i | 86 (1) | N3—Ni1—N4—C4 | 9.3 (3) |
Ni1—Br1—Ni1i—N4i | 90.4 (1) | N3—C3—C4—N4 | 53.1 (6) |
Ni1—N1—C1—C2 | −40.2 (5) | N4—Ni1—N1—C1 | −172.9 (3) |
Ni1—N2—C2—C1 | −39.8 (5) | N4—Ni1—N2—C2 | −67 (1) |
Ni1—N3—C3—C4 | −43.1 (5) | N4—Ni1—N3—C3 | 18.9 (3) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x−1/2, −y+1/2, z−1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) x−1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H2···Br2v | 0.95 | 2.45 | 3.389 (4) | 172 |
Symmetry code: (v) x+1/2, −y+1/2, z+1/2. |