The structure of the title compound, [NiBr2(C3H4N2)2(H2O)2], consists of monomers with inversion symmetry. The three monodentate ligands (imidazole, bromine and aqua), together with their symmetry equivalents, define an almost perfect octahedral coordination. Hydrogen-bonding interactions via the NH group of imidazole, Br and aqua H atoms lead to a three-dimensional network.
Supporting information
CCDC reference: 277235
Key indicators
- Single-crystal X-ray study
- T = 223 K
- Mean (C-C)= 0.003 Å
- R factor = 0.020
- wR factor = 0.051
- Data-to-parameter ratio = 19.7
checkCIF/PLATON results
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Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.
Diaquadibromobis(1
H-imidazole)nickel(II)
top
Crystal data top
[NiBr2(C3H4N2)2(H2O)2] | F(000) = 380 |
Mr = 390.69 | Dx = 2.108 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 1538 reflections |
a = 7.8000 (18) Å | θ = 2.6–28.3° |
b = 9.366 (2) Å | µ = 8.05 mm−1 |
c = 8.474 (2) Å | T = 223 K |
β = 96.114 (4)° | Prism, green |
V = 615.6 (2) Å3 | 0.36 × 0.20 × 0.16 mm |
Z = 2 | |
Data collection top
Bruker AXS APEX CCD diffractometer | 1538 independent reflections |
Radiation source: fine-focus sealed tube | 1414 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ω scans | θmax = 28.3°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS in SAINT; Bruker, 1998) | h = −10→10 |
Tmin = 0.16, Tmax = 0.28 | k = −12→12 |
8270 measured reflections | l = −11→11 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.020 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.051 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0269P)2 + 0.0562P] where P = (Fo2 + 2Fc2)/3 |
1538 reflections | (Δ/σ)max < 0.001 |
78 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.63 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Ni1 | 0.5000 | 0.0000 | 1.0000 | 0.01679 (9) | |
Br1 | 0.39147 (2) | −0.264724 (19) | 0.99031 (2) | 0.02118 (8) | |
N1 | 0.25951 (19) | 0.06572 (18) | 0.9048 (2) | 0.0221 (3) | |
N2 | −0.0015 (2) | 0.1547 (2) | 0.8858 (3) | 0.0389 (5) | |
H2 | −0.0911 | 0.2019 | 0.9101 | 0.047* | |
C3 | 0.1503 (3) | 0.1427 (2) | 0.9765 (3) | 0.0320 (5) | |
H3 | 0.1749 | 0.1838 | 1.0776 | 0.038* | |
C4 | 0.1721 (3) | 0.0257 (3) | 0.7620 (3) | 0.0316 (5) | |
H4 | 0.2175 | −0.0308 | 0.6847 | 0.038* | |
C5 | 0.0098 (3) | 0.0805 (3) | 0.7501 (3) | 0.0392 (6) | |
H5 | −0.0768 | 0.0693 | 0.6651 | 0.047* | |
O1 | 0.41887 (19) | 0.02412 (18) | 1.22586 (17) | 0.0233 (3) | |
H1W | 0.460 (3) | 0.084 (3) | 1.283 (3) | 0.037 (8)* | |
H2W | 0.420 (3) | −0.050 (3) | 1.275 (3) | 0.039 (8)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.01500 (16) | 0.01698 (17) | 0.01828 (17) | 0.00154 (12) | 0.00120 (12) | 0.00005 (12) |
Br1 | 0.02362 (12) | 0.01741 (11) | 0.02244 (12) | −0.00084 (7) | 0.00210 (8) | −0.00044 (7) |
N1 | 0.0178 (7) | 0.0212 (8) | 0.0273 (8) | 0.0030 (6) | 0.0022 (6) | 0.0022 (7) |
N2 | 0.0207 (9) | 0.0381 (11) | 0.0585 (14) | 0.0122 (8) | 0.0071 (8) | 0.0101 (10) |
C3 | 0.0267 (10) | 0.0297 (12) | 0.0401 (12) | 0.0078 (9) | 0.0048 (9) | −0.0006 (9) |
C4 | 0.0232 (10) | 0.0435 (13) | 0.0273 (11) | 0.0037 (9) | −0.0013 (8) | −0.0005 (9) |
C5 | 0.0226 (10) | 0.0538 (15) | 0.0396 (13) | 0.0044 (10) | −0.0047 (9) | 0.0111 (12) |
O1 | 0.0265 (7) | 0.0227 (7) | 0.0205 (7) | −0.0028 (6) | 0.0023 (6) | −0.0013 (6) |
Geometric parameters (Å, º) top
Ni1—N1 | 2.0557 (16) | N2—C5 | 1.354 (3) |
Ni1—N1i | 2.0557 (16) | N2—H2 | 0.8700 |
Ni1—O1 | 2.0910 (15) | C3—H3 | 0.9400 |
Ni1—O1i | 2.0910 (15) | C4—C5 | 1.360 (3) |
Ni1—Br1 | 2.6184 (6) | C4—H4 | 0.9400 |
Ni1—Br1i | 2.6184 (6) | C5—H5 | 0.9400 |
N1—C3 | 1.313 (3) | O1—H1W | 0.79 (3) |
N1—C4 | 1.376 (3) | O1—H2W | 0.81 (3) |
N2—C3 | 1.346 (3) | | |
| | | |
N1—Ni1—N1i | 180.0 | C4—N1—Ni1 | 127.55 (14) |
N1—Ni1—O1 | 88.53 (6) | C3—N2—C5 | 108.01 (18) |
N1i—Ni1—O1 | 91.47 (6) | C3—N2—H2 | 126.0 |
N1—Ni1—O1i | 91.47 (6) | C5—N2—H2 | 126.0 |
N1i—Ni1—O1i | 88.53 (6) | N1—C3—N2 | 110.9 (2) |
O1—Ni1—O1i | 180.0 | N1—C3—H3 | 124.6 |
N1—Ni1—Br1 | 89.59 (5) | N2—C3—H3 | 124.6 |
N1i—Ni1—Br1 | 90.41 (5) | C5—C4—N1 | 109.4 (2) |
O1—Ni1—Br1 | 90.15 (5) | C5—C4—H4 | 125.3 |
O1i—Ni1—Br1 | 89.85 (5) | N1—C4—H4 | 125.3 |
N1—Ni1—Br1i | 90.41 (5) | N2—C5—C4 | 106.0 (2) |
N1i—Ni1—Br1i | 89.59 (5) | N2—C5—H5 | 127.0 |
O1—Ni1—Br1i | 89.85 (5) | C4—C5—H5 | 127.0 |
O1i—Ni1—Br1i | 90.15 (5) | Ni1—O1—H1W | 119.8 (18) |
Br1—Ni1—Br1i | 180.0 | Ni1—O1—H2W | 113.3 (19) |
C3—N1—C4 | 105.75 (18) | H1W—O1—H2W | 108 (3) |
C3—N1—Ni1 | 126.32 (15) | | |
Symmetry code: (i) −x+1, −y, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1W···Br1ii | 0.79 (3) | 2.56 (3) | 3.3356 (16) | 168 (3) |
O1—H2W···Br1iii | 0.81 (3) | 2.55 (3) | 3.3273 (17) | 164 (2) |
N2—H2···Br1iv | 0.87 | 2.64 | 3.4782 (19) | 162 |
Symmetry codes: (ii) −x+1, y+1/2, −z+5/2; (iii) x, −y−1/2, z+1/2; (iv) −x, −y, −z+2. |