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The structure of trans-[Ni(CH3CN)2(H2O)4]Br2 has been determined at 153 K. The complex possesses Ci symmetry, with the NiII atom lying on an inversion center. The Ni atom is coordinated to four water mol­ecules in the equatorial plane and to two trans aceto­nitrile mol­ecules. In the crystal, a three-dimensional structure is formed by hydrogen bonding involving the lattice Br- ions and the coordinated water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801005323/om6004sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801005323/om6004Isup2.hkl
Contains datablock I

CCDC reference: 165624

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.040
  • wR factor = 0.112
  • Data-to-parameter ratio = 13.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_320 Alert C Check Hybridisation of C2 in main residue ? General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.302 Tmax scaled 0.065 Tmin scaled 0.020
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

trans-[Ni(CH3CN)2(H2O)4]Br2, (I), was prepared by accident during attempts to synthesize an NiBr2 complex of a substituted pyrazine ligand in acetonitrile. The structure is isomorphous with the cobalt(II) complex (Depree et al., 2000).

Experimental top

The title compound was prepared during attempts to synthesize an NiBr2 complex of a substituted pyrazine ligand in acetonitrile.

Refinement top

The H atoms were located from difference Fourier maps and were refined isotropically. A semi-empirical absorption correction was applied using the MULscanABS routine in PLATON99 (Spek, 1990).

Computing details top

Data collection: EXPOSE (Stoe & Cie, 2000); cell refinement: CELL (Stoe & Cie, 2000); data reduction: INTEGRATE (Stoe & Cie, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1990); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. A perspective view of [Ni(CH3CN)2(H2O)4]2+ cation, showing the numbering scheme and displacement ellipsoids at the 50% probability level.
[Figure 2] Fig. 2. Packing diagram illustrating the O—H···Br bonds in the structure of trans-[Ni(CH3CN)2(H2O)4]Br2 viewed down the a axis.
(I) top
Crystal data top
[Ni(C2H3N)2(H2O)4]Br2F(000) = 364
Mr = 372.70Dx = 1.954 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 6.8839 (11) ÅCell parameters from 3712 reflections
b = 12.4630 (17) Åθ = 3.2–26.0°
c = 7.9173 (12) ŵ = 7.83 mm1
β = 111.127 (18)°T = 153 K
V = 633.60 (16) Å3Block, blue–green
Z = 20.50 × 0.35 × 0.35 mm
Data collection top
STOE Image Plate Diffraction System
diffractometer
1231 independent reflections
Radiation source: fine-focus sealed tube1049 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.079
Detector resolution: 0.81 pixels mm-1θmax = 26.0°, θmin = 3.2°
ϕ oscillation scansh = 88
Absorption correction: multi-scan
(PLATON; Spek, 1990)
k = 1415
Tmin = 0.067, Tmax = 0.214l = 99
4033 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040All H-atom parameters refined
wR(F2) = 0.112 w = 1/[σ2(Fo2) + (0.0727P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
1231 reflectionsΔρmax = 1.01 e Å3
90 parametersΔρmin = 1.23 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.021 (3)
Crystal data top
[Ni(C2H3N)2(H2O)4]Br2V = 633.60 (16) Å3
Mr = 372.70Z = 2
Monoclinic, P21/cMo Kα radiation
a = 6.8839 (11) ŵ = 7.83 mm1
b = 12.4630 (17) ÅT = 153 K
c = 7.9173 (12) Å0.50 × 0.35 × 0.35 mm
β = 111.127 (18)°
Data collection top
STOE Image Plate Diffraction System
diffractometer
1231 independent reflections
Absorption correction: multi-scan
(PLATON; Spek, 1990)
1049 reflections with I > 2σ(I)
Tmin = 0.067, Tmax = 0.214Rint = 0.079
4033 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0400 restraints
wR(F2) = 0.112All H-atom parameters refined
S = 1.06Δρmax = 1.01 e Å3
1231 reflectionsΔρmin = 1.23 e Å3
90 parameters
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
xyzUiso*/Ueq
Ni10.50000.00000.50000.0180 (3)
Br10.81150 (7)0.13685 (4)0.10018 (6)0.0240 (3)
O1W0.2310 (6)0.0131 (4)0.2765 (5)0.0314 (9)
H1WA0.156 (13)0.038 (7)0.263 (11)0.06 (2)*
H1WB0.240 (11)0.047 (7)0.184 (11)0.05 (2)*
O2W0.5782 (6)0.1389 (3)0.3950 (6)0.0264 (8)
H2WA0.644 (14)0.124 (6)0.329 (13)0.06 (2)*
H2WB0.640 (9)0.195 (6)0.463 (9)0.032 (16)*
N10.6463 (6)0.0889 (3)0.3623 (6)0.0240 (9)
C10.7047 (7)0.1253 (4)0.2586 (7)0.0202 (10)
C20.7786 (9)0.1714 (5)0.1257 (9)0.0291 (12)
H2A0.773 (11)0.232 (7)0.130 (10)0.04 (2)*
H2B0.756 (18)0.128 (8)0.026 (18)0.10 (4)*
H2C0.903 (19)0.175 (9)0.156 (14)0.09 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0192 (4)0.0177 (5)0.0177 (5)0.0003 (3)0.0073 (3)0.0018 (3)
Br10.0267 (4)0.0241 (4)0.0218 (4)0.00375 (17)0.0095 (2)0.00025 (17)
O1W0.0258 (18)0.037 (2)0.028 (2)0.0070 (16)0.0052 (15)0.0109 (17)
O2W0.036 (2)0.0193 (19)0.029 (2)0.0037 (15)0.0170 (17)0.0046 (15)
N10.0246 (19)0.022 (2)0.025 (2)0.0006 (16)0.0093 (17)0.0000 (18)
C10.021 (2)0.018 (2)0.023 (3)0.0007 (17)0.009 (2)0.0026 (18)
C20.029 (3)0.022 (3)0.042 (3)0.000 (2)0.019 (2)0.010 (3)
Geometric parameters (Å, º) top
Ni1—N1i2.055 (4)Ni1—O2Wi2.074 (4)
Ni1—N12.055 (4)Ni1—O2W2.074 (4)
Ni1—O1Wi2.056 (4)N1—C11.132 (6)
Ni1—O1W2.056 (4)C1—C21.443 (7)
N1i—Ni1—N1180.0O1W—Ni1—O2Wi89.74 (16)
N1i—Ni1—O1Wi87.83 (16)N1i—Ni1—O2W90.59 (17)
N1—Ni1—O1Wi92.17 (16)N1—Ni1—O2W89.41 (17)
N1i—Ni1—O1W92.17 (16)O1Wi—Ni1—O2W89.74 (16)
N1—Ni1—O1W87.83 (16)O1W—Ni1—O2W90.26 (16)
O1Wi—Ni1—O1W180.0O2Wi—Ni1—O2W180.0
N1i—Ni1—O2Wi89.41 (17)C1—N1—Ni1166.3 (4)
N1—Ni1—O2Wi90.59 (17)N1—C1—C2179.8 (6)
O1Wi—Ni1—O2Wi90.26 (16)
Symmetry code: (i) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···Br1ii0.80 (9)2.57 (9)3.298 (4)152 (8)
O1W—H1WB···Br1iii0.86 (8)2.42 (8)3.275 (4)168 (6)
O2W—H2WA···Br10.83 (10)2.48 (10)3.275 (4)162 (7)
O2W—H2WB···Br1iv0.89 (7)2.46 (7)3.339 (4)170 (6)
Symmetry codes: (ii) x1, y, z; (iii) x+1, y, z; (iv) x, y1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Ni(C2H3N)2(H2O)4]Br2
Mr372.70
Crystal system, space groupMonoclinic, P21/c
Temperature (K)153
a, b, c (Å)6.8839 (11), 12.4630 (17), 7.9173 (12)
β (°) 111.127 (18)
V3)633.60 (16)
Z2
Radiation typeMo Kα
µ (mm1)7.83
Crystal size (mm)0.50 × 0.35 × 0.35
Data collection
DiffractometerSTOE Image Plate Diffraction System
diffractometer
Absorption correctionMulti-scan
(PLATON; Spek, 1990)
Tmin, Tmax0.067, 0.214
No. of measured, independent and
observed [I > 2σ(I)] reflections
4033, 1231, 1049
Rint0.079
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.040, 0.112, 1.06
No. of reflections1231
No. of parameters90
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)1.01, 1.23

Computer programs: EXPOSE (Stoe & Cie, 2000), CELL (Stoe & Cie, 2000), INTEGRATE (Stoe & Cie, 2000), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 1990), SHELXL97.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···Br1i0.80 (9)2.57 (9)3.298 (4)152 (8)
O1W—H1WB···Br1ii0.86 (8)2.42 (8)3.275 (4)168 (6)
O2W—H2WA···Br10.83 (10)2.48 (10)3.275 (4)162 (7)
O2W—H2WB···Br1iii0.89 (7)2.46 (7)3.339 (4)170 (6)
Symmetry codes: (i) x1, y, z; (ii) x+1, y, z; (iii) x, y1/2, z+1/2.
 

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