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The title complex, [Ni(C8H4N2S2)2], is a mononuclear nickel(II) complex in which the coordination about the Ni atom to the four S atoms of the two quinoxaline-2,3-dithiolate (qt) ligands is slightly distorted square planar. The molecule has a crystallographic inversion centre.
Supporting information
CCDC reference: 170272
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.059
- wR factor = 0.163
- Data-to-parameter ratio = 12.0
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.492 0.794
Tmin' and Tmax expected: 0.652 0.870
RR' = 0.827
Please check that your absorption correction is appropriate.
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 1.095
Tmax scaled 0.870 Tmin scaled 0.539
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SAINT (Siemens, 1994); program(s) used to solve structure: SHELXL97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.
Bis(quinoxaline-2,3-dithiolato-S,
S')nickel(II)
top
Crystal data top
[Ni(C8H4N2S2)2] | F(000) = 448 |
Mr = 443.23 | Dx = 1.843 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 6.6528 (2) Å | Cell parameters from 1378 reflections |
b = 5.7251 (2) Å | θ = 1.9–25.0° |
c = 20.9637 (8) Å | µ = 1.75 mm−1 |
β = 90.205 (2)° | T = 293 K |
V = 798.46 (5) Å3 | Sheet, black |
Z = 2 | 0.24 × 0.18 × 0.08 mm |
Data collection top
Smart CCD diffractometer | 1378 independent reflections |
Radiation source: fine-focus sealed tube | 1022 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: empirical (using intensity measurements) SHELXTL (Siemens,1994) | h = −7→4 |
Tmin = 0.492, Tmax = 0.794 | k = −6→3 |
2114 measured reflections | l = −22→24 |
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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.163 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0965P)2] where P = (Fo2 + 2Fc2)/3 |
1378 reflections | (Δ/σ)max < 0.001 |
115 parameters | Δρmax = 0.89 e Å−3 |
0 restraints | Δρmin = −0.65 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 | |
Ni | 0.0000 | 0.0000 | 0.0000 | 0.0283 (4) | |
S1 | −0.2901 (2) | −0.1616 (3) | 0.01561 (8) | 0.0352 (5) | |
S2 | 0.1479 (2) | −0.2482 (3) | 0.06394 (7) | 0.0360 (5) | |
N1 | −0.3919 (7) | −0.5131 (8) | 0.0901 (2) | 0.0298 (12) | |
N2 | −0.0027 (7) | −0.5991 (9) | 0.1313 (2) | 0.0322 (12) | |
C1 | −0.5160 (9) | −0.8393 (10) | 0.1510 (3) | 0.0336 (15) | |
H1B | −0.6466 | −0.8099 | 0.1373 | 0.040* | |
C2 | −0.4769 (9) | −1.0224 (11) | 0.1909 (3) | 0.0384 (16) | |
H2B | −0.5815 | −1.1180 | 0.2044 | 0.046* | |
C3 | −0.2792 (10) | −1.0675 (13) | 0.2117 (3) | 0.0435 (17) | |
H3A | −0.2536 | −1.1934 | 0.2386 | 0.052* | |
C4 | −0.1237 (10) | −0.9254 (11) | 0.1923 (3) | 0.0404 (16) | |
H4A | 0.0063 | −0.9559 | 0.2064 | 0.048* | |
C5 | −0.1591 (9) | −0.7358 (11) | 0.1516 (3) | 0.0306 (14) | |
C6 | −0.3592 (8) | −0.6975 (11) | 0.1312 (3) | 0.0306 (14) | |
C7 | −0.0413 (8) | −0.4279 (10) | 0.0916 (3) | 0.0272 (13) | |
C8 | −0.2444 (8) | −0.3820 (10) | 0.0682 (2) | 0.0262 (13) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni | 0.0212 (6) | 0.0278 (7) | 0.0358 (6) | 0.0013 (5) | −0.0015 (4) | 0.0003 (5) |
S1 | 0.0235 (8) | 0.0366 (10) | 0.0453 (9) | 0.0014 (7) | −0.0057 (6) | 0.0086 (7) |
S2 | 0.0203 (8) | 0.0374 (10) | 0.0502 (10) | −0.0008 (7) | −0.0034 (6) | 0.0081 (8) |
N1 | 0.020 (2) | 0.033 (3) | 0.037 (3) | 0.001 (2) | −0.003 (2) | 0.004 (2) |
N2 | 0.019 (2) | 0.038 (3) | 0.040 (3) | 0.002 (2) | −0.004 (2) | 0.004 (3) |
C1 | 0.028 (3) | 0.040 (4) | 0.033 (3) | −0.001 (3) | 0.002 (2) | −0.002 (3) |
C2 | 0.032 (4) | 0.044 (4) | 0.039 (4) | 0.003 (3) | 0.005 (3) | 0.005 (3) |
C3 | 0.035 (4) | 0.048 (4) | 0.048 (4) | −0.004 (3) | 0.000 (3) | 0.009 (3) |
C4 | 0.032 (3) | 0.043 (4) | 0.045 (4) | 0.002 (3) | −0.005 (3) | 0.009 (3) |
C5 | 0.026 (3) | 0.032 (3) | 0.033 (3) | 0.007 (3) | −0.005 (2) | −0.001 (3) |
C6 | 0.020 (3) | 0.040 (4) | 0.032 (3) | 0.006 (3) | 0.000 (2) | −0.007 (3) |
C7 | 0.016 (3) | 0.029 (3) | 0.037 (3) | 0.005 (2) | −0.005 (2) | −0.006 (3) |
C8 | 0.023 (3) | 0.028 (3) | 0.028 (3) | 0.006 (3) | −0.001 (2) | 0.001 (3) |
Geometric parameters (Å, º) top
Ni—S1 | 2.1664 (15) | N2—C5 | 1.372 (8) |
Ni—S1i | 2.1664 (15) | C1—C2 | 1.365 (8) |
Ni—S2 | 2.1850 (15) | C1—C6 | 1.387 (8) |
Ni—S2i | 2.1850 (15) | C2—C3 | 1.408 (9) |
S1—C8 | 1.703 (5) | C3—C4 | 1.379 (9) |
S2—C7 | 1.727 (6) | C4—C5 | 1.400 (8) |
N1—C8 | 1.319 (7) | C5—C6 | 1.414 (8) |
N1—C6 | 1.380 (7) | C7—C8 | 1.460 (7) |
N2—C7 | 1.311 (7) | | |
| | | |
S1—Ni—S1i | 180.00 (11) | C3—C4—C5 | 120.8 (6) |
S1—Ni—S2 | 91.67 (5) | N2—C5—C4 | 120.4 (5) |
S1i—Ni—S2 | 88.33 (5) | N2—C5—C6 | 122.1 (5) |
S1—Ni—S2i | 88.33 (5) | C4—C5—C6 | 117.5 (6) |
S1i—Ni—S2i | 91.67 (5) | N1—C6—C1 | 121.2 (5) |
S2—Ni—S2i | 180.00 (7) | N1—C6—C5 | 117.0 (5) |
C8—S1—Ni | 104.90 (19) | C1—C6—C5 | 121.8 (6) |
C7—S2—Ni | 105.43 (19) | N2—C7—C8 | 121.8 (5) |
C8—N1—C6 | 122.5 (5) | N2—C7—S2 | 121.1 (4) |
C7—N2—C5 | 118.5 (5) | C8—C7—S2 | 117.1 (4) |
C2—C1—C6 | 119.4 (6) | N1—C8—C7 | 118.1 (5) |
C1—C2—C3 | 120.4 (6) | N1—C8—S1 | 121.0 (4) |
C4—C3—C2 | 120.1 (6) | C7—C8—S1 | 120.9 (4) |
Symmetry code: (i) −x, −y, −z. |
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