Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801005323/om6004sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801005323/om6004Isup2.hkl |
CCDC reference: 165624
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (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
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
The title compound was prepared during attempts to synthesize an NiBr2 complex of a substituted pyrazine ligand in acetonitrile.
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).
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.
[Ni(C2H3N)2(H2O)4]Br2 | F(000) = 364 |
Mr = 372.70 | Dx = 1.954 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 6.8839 (11) Å | Cell parameters from 3712 reflections |
b = 12.4630 (17) Å | θ = 3.2–26.0° |
c = 7.9173 (12) Å | µ = 7.83 mm−1 |
β = 111.127 (18)° | T = 153 K |
V = 633.60 (16) Å3 | Block, blue–green |
Z = 2 | 0.50 × 0.35 × 0.35 mm |
STOE Image Plate Diffraction System diffractometer | 1231 independent reflections |
Radiation source: fine-focus sealed tube | 1049 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.079 |
Detector resolution: 0.81 pixels mm-1 | θmax = 26.0°, θmin = 3.2° |
ϕ oscillation scans | h = −8→8 |
Absorption correction: multi-scan (PLATON; Spek, 1990) | k = −14→15 |
Tmin = 0.067, Tmax = 0.214 | l = −9→9 |
4033 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.040 | All 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 reflections | Δρmax = 1.01 e Å−3 |
90 parameters | Δρmin = −1.23 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.021 (3) |
[Ni(C2H3N)2(H2O)4]Br2 | V = 633.60 (16) Å3 |
Mr = 372.70 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 6.8839 (11) Å | µ = 7.83 mm−1 |
b = 12.4630 (17) Å | T = 153 K |
c = 7.9173 (12) Å | 0.50 × 0.35 × 0.35 mm |
β = 111.127 (18)° |
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 = 0.214 | Rint = 0.079 |
4033 measured reflections |
R[F2 > 2σ(F2)] = 0.040 | 0 restraints |
wR(F2) = 0.112 | All H-atom parameters refined |
S = 1.06 | Δρmax = 1.01 e Å−3 |
1231 reflections | Δρmin = −1.23 e Å−3 |
90 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.5000 | 0.0000 | 0.5000 | 0.0180 (3) | |
Br1 | 0.81150 (7) | −0.13685 (4) | 0.10018 (6) | 0.0240 (3) | |
O1W | 0.2310 (6) | 0.0131 (4) | 0.2765 (5) | 0.0314 (9) | |
H1WA | 0.156 (13) | −0.038 (7) | 0.263 (11) | 0.06 (2)* | |
H1WB | 0.240 (11) | 0.047 (7) | 0.184 (11) | 0.05 (2)* | |
O2W | 0.5782 (6) | −0.1389 (3) | 0.3950 (6) | 0.0264 (8) | |
H2WA | 0.644 (14) | −0.124 (6) | 0.329 (13) | 0.06 (2)* | |
H2WB | 0.640 (9) | −0.195 (6) | 0.463 (9) | 0.032 (16)* | |
N1 | 0.6463 (6) | 0.0889 (3) | 0.3623 (6) | 0.0240 (9) | |
C1 | 0.7047 (7) | 0.1253 (4) | 0.2586 (7) | 0.0202 (10) | |
C2 | 0.7786 (9) | 0.1714 (5) | 0.1257 (9) | 0.0291 (12) | |
H2A | 0.773 (11) | 0.232 (7) | 0.130 (10) | 0.04 (2)* | |
H2B | 0.756 (18) | 0.128 (8) | 0.026 (18) | 0.10 (4)* | |
H2C | 0.903 (19) | 0.175 (9) | 0.156 (14) | 0.09 (3)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0192 (4) | 0.0177 (5) | 0.0177 (5) | −0.0003 (3) | 0.0073 (3) | 0.0018 (3) |
Br1 | 0.0267 (4) | 0.0241 (4) | 0.0218 (4) | −0.00375 (17) | 0.0095 (2) | −0.00025 (17) |
O1W | 0.0258 (18) | 0.037 (2) | 0.028 (2) | −0.0070 (16) | 0.0052 (15) | 0.0109 (17) |
O2W | 0.036 (2) | 0.0193 (19) | 0.029 (2) | 0.0037 (15) | 0.0170 (17) | 0.0046 (15) |
N1 | 0.0246 (19) | 0.022 (2) | 0.025 (2) | 0.0006 (16) | 0.0093 (17) | 0.0000 (18) |
C1 | 0.021 (2) | 0.018 (2) | 0.023 (3) | −0.0007 (17) | 0.009 (2) | −0.0026 (18) |
C2 | 0.029 (3) | 0.022 (3) | 0.042 (3) | 0.000 (2) | 0.019 (2) | 0.010 (3) |
Ni1—N1i | 2.055 (4) | Ni1—O2Wi | 2.074 (4) |
Ni1—N1 | 2.055 (4) | Ni1—O2W | 2.074 (4) |
Ni1—O1Wi | 2.056 (4) | N1—C1 | 1.132 (6) |
Ni1—O1W | 2.056 (4) | C1—C2 | 1.443 (7) |
N1i—Ni1—N1 | 180.0 | O1W—Ni1—O2Wi | 89.74 (16) |
N1i—Ni1—O1Wi | 87.83 (16) | N1i—Ni1—O2W | 90.59 (17) |
N1—Ni1—O1Wi | 92.17 (16) | N1—Ni1—O2W | 89.41 (17) |
N1i—Ni1—O1W | 92.17 (16) | O1Wi—Ni1—O2W | 89.74 (16) |
N1—Ni1—O1W | 87.83 (16) | O1W—Ni1—O2W | 90.26 (16) |
O1Wi—Ni1—O1W | 180.0 | O2Wi—Ni1—O2W | 180.0 |
N1i—Ni1—O2Wi | 89.41 (17) | C1—N1—Ni1 | 166.3 (4) |
N1—Ni1—O2Wi | 90.59 (17) | N1—C1—C2 | 179.8 (6) |
O1Wi—Ni1—O2Wi | 90.26 (16) |
Symmetry code: (i) −x+1, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···Br1ii | 0.80 (9) | 2.57 (9) | 3.298 (4) | 152 (8) |
O1W—H1WB···Br1iii | 0.86 (8) | 2.42 (8) | 3.275 (4) | 168 (6) |
O2W—H2WA···Br1 | 0.83 (10) | 2.48 (10) | 3.275 (4) | 162 (7) |
O2W—H2WB···Br1iv | 0.89 (7) | 2.46 (7) | 3.339 (4) | 170 (6) |
Symmetry codes: (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x, −y−1/2, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Ni(C2H3N)2(H2O)4]Br2 |
Mr | 372.70 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 153 |
a, b, c (Å) | 6.8839 (11), 12.4630 (17), 7.9173 (12) |
β (°) | 111.127 (18) |
V (Å3) | 633.60 (16) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 7.83 |
Crystal size (mm) | 0.50 × 0.35 × 0.35 |
Data collection | |
Diffractometer | STOE Image Plate Diffraction System diffractometer |
Absorption correction | Multi-scan (PLATON; Spek, 1990) |
Tmin, Tmax | 0.067, 0.214 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4033, 1231, 1049 |
Rint | 0.079 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.112, 1.06 |
No. of reflections | 1231 |
No. of parameters | 90 |
H-atom treatment | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | 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.
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···Br1i | 0.80 (9) | 2.57 (9) | 3.298 (4) | 152 (8) |
O1W—H1WB···Br1ii | 0.86 (8) | 2.42 (8) | 3.275 (4) | 168 (6) |
O2W—H2WA···Br1 | 0.83 (10) | 2.48 (10) | 3.275 (4) | 162 (7) |
O2W—H2WB···Br1iii | 0.89 (7) | 2.46 (7) | 3.339 (4) | 170 (6) |
Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y, −z; (iii) x, −y−1/2, z+1/2. |
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).