The title double salt, [Ni(C
2H
8N
2)
3]
2(SbS
4)(NO
3), was crystallized under solvothermal conditions. Hydrogen bonds between the SbS
43- anions (at four sites) and the [Ni(en)
3]
2+ (en = ethylenediamine) cations (at two sites) form a three-dimensional network. The NO
3- anion is disordered over four sites. The cation lies on a twofold rotation axis and the SbS
43- anion on a
axis.
Supporting information
CCDC reference: 150775
Data collection: DIF4 (Stoe & Cie, 1992); cell refinement: DIF4; data reduction: REDU4 (Stoe & Cie, 1992); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-PC (Siemens, 1990); software used to prepare material for publication: CIFTAB in SHELXL97.
tris(ethylenediamine)-nickel(II)tetrathioantimonate nitrate ?
top
Crystal data top
[Ni(C2H8N2)3]2(SbS4)(NO3) | Dx = 1.643 Mg m−3 |
Mr = 790.04 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I42d | Cell parameters from 90 reflections |
Hall symbol: I -4 2bw | θ = 16–22° |
a = 10.276 (2) Å | µ = 2.31 mm−1 |
c = 30.249 (4) Å | T = 293 K |
V = 3194.3 (13) Å3 | Plates, violet |
Z = 4 | 0.15 × 0.12 × 0.1 mm |
F(000) = 1624 | |
Data collection top
STOE AED-II 4-circle diffractometer | Rint = 0.036 |
Radiation source: fine-focus sealed tube | θmax = 27.5°, θmin = 2.1° |
Graphite monochromator | h = −1→13 |
ω–θ–scan | k = 0→13 |
2222 measured reflections | l = 0→39 |
1233 independent reflections | 4 standard reflections every every 2 h min |
934 reflections with I > 2σ(I) | intensity decay: neglible |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.031 | Calculated w = 1/[σ2(Fo2) + (0.0409P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.070 | (Δ/σ)max < 0.001 |
S = 1.00 | Δρmax = 1.08 e Å−3 |
1233 reflections | Δρmin = −0.87 e Å−3 |
92 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00055 (10) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983) |
Secondary atom site location: difference Fourier map | Absolute structure parameter: −0.04 (5) |
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 | Occ. (<1) |
Sb1 | 0.0000 | 0.0000 | 0.0000 | 0.02445 (15) | |
S1 | 0.15240 (13) | −0.10100 (14) | 0.04498 (4) | 0.0378 (3) | |
Ni1 | 0.0000 | 0.5000 | 0.04330 (2) | 0.0340 (2) | |
N1 | −0.1145 (5) | 0.4011 (4) | 0.0906 (1) | 0.046 (1) | |
H1A | −0.1199 | 0.3162 | 0.0836 | 0.055* | |
H1B | −0.0780 | 0.4081 | 0.1175 | 0.055* | |
N2 | 0.0970 (4) | 0.5949 (4) | −0.0099 (1) | 0.0388 (9) | |
H2A | 0.0682 | 0.6773 | −0.0124 | 0.047* | |
H2B | 0.1832 | 0.5971 | −0.0047 | 0.047* | |
N3 | 0.1542 (5) | 0.3612 (4) | 0.0489 (2) | 0.0545 (13) | |
H3A | 0.1213 | 0.2803 | 0.0512 | 0.065* | |
H3B | 0.2052 | 0.3644 | 0.0247 | 0.065* | |
C1 | −0.2462 (7) | 0.4601 (6) | 0.0909 (2) | 0.0584 (17) | |
H1C | −0.2918 | 0.4363 | 0.1178 | 0.070* | |
H1D | −0.2963 | 0.4290 | 0.0659 | 0.070* | |
C2 | 0.0705 (5) | 0.5227 (5) | −0.05099 (14) | 0.0427 (15) | |
H2C | 0.1281 | 0.4482 | −0.0531 | 0.051* | |
H2D | 0.0861 | 0.5784 | −0.0763 | 0.051* | |
C3 | 0.2306 (7) | 0.3929 (6) | 0.0884 (2) | 0.0589 (17) | |
H3C | 0.3153 | 0.3517 | 0.0868 | 0.071* | |
H3D | 0.1864 | 0.3612 | 0.1146 | 0.071* | |
N4 | 0.5000 | 0.5000 | 0.0000 | 0.054 (2) | |
O1 | 0.489 (8) | 0.390 (2) | 0.0130 (9) | 0.090 (9) | 0.375 |
O2 | 0.403 (5) | 0.431 (7) | −0.003 (2) | 0.10 (1) | 0.375 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sb1 | 0.02461 (18) | 0.02461 (18) | 0.0241 (2) | 0.000 | 0.000 | 0.000 |
S1 | 0.0341 (6) | 0.0396 (7) | 0.0397 (7) | −0.0026 (6) | −0.0100 (5) | 0.0116 (6) |
Ni1 | 0.0502 (5) | 0.0236 (4) | 0.0282 (4) | 0.0027 (8) | 0.000 | 0.000 |
N1 | 0.076 (4) | 0.031 (2) | 0.032 (2) | −0.003 (3) | 0.003 (2) | −0.0019 (18) |
N2 | 0.048 (2) | 0.032 (2) | 0.037 (2) | −0.002 (2) | −0.0032 (19) | 0.0030 (18) |
N3 | 0.076 (3) | 0.037 (2) | 0.051 (3) | 0.017 (3) | −0.011 (3) | −0.005 (2) |
C1 | 0.075 (4) | 0.060 (4) | 0.040 (3) | −0.006 (4) | 0.011 (3) | −0.001 (3) |
C2 | 0.059 (3) | 0.035 (4) | 0.033 (2) | 0.010 (3) | 0.006 (2) | −0.001 (2) |
C3 | 0.073 (4) | 0.055 (4) | 0.049 (4) | 0.012 (4) | −0.014 (3) | 0.002 (3) |
N4 | 0.056 (3) | 0.056 (3) | 0.049 (4) | 0.000 | 0.000 | 0.000 |
O1 | 0.12 (2) | 0.048 (10) | 0.105 (12) | −0.026 (18) | −0.025 (19) | 0.016 (8) |
O2 | 0.06 (2) | 0.10 (2) | 0.14 (2) | −0.034 (15) | 0.027 (18) | −0.07 (2) |
Geometric parameters (Å, º) top
Sb1—S1i | 2.320 (2) | N4—O1v | 1.199 (19) |
Sb1—S1ii | 2.320 (2) | N4—O1 | 1.199 (19) |
Sb1—S1iii | 2.320 (2) | N4—O1vi | 1.199 (19) |
Sb1—S1 | 2.320 (2) | N4—O1vii | 1.199 (19) |
Ni1—N1iv | 2.113 (4) | N4—O2v | 1.225 (18) |
Ni1—N1 | 2.113 (4) | N4—O2vi | 1.225 (18) |
Ni1—N2 | 2.129 (4) | N4—O2 | 1.225 (18) |
Ni1—N2iv | 2.129 (4) | N4—O2vii | 1.225 (18) |
Ni1—N3 | 2.139 (5) | O1—O2vi | 0.88 (3) |
Ni1—N3iv | 2.139 (5) | O1—O2 | 1.09 (3) |
N1—C1 | 1.483 (7) | O1—O1vi | 1.79 (3) |
N2—C2 | 1.473 (6) | O1—O1vii | 1.79 (3) |
N3—C3 | 1.467 (7) | O2—O1vii | 0.88 (3) |
C1—C3iv | 1.521 (9) | O2—O2vi | 1.74 (3) |
C2—C2iv | 1.522 (11) | O2—O2vii | 1.74 (3) |
C3—C1iv | 1.521 (9) | | |
| | | |
S1i—Sb1—S1ii | 110.12 (4) | O1—N4—O2vi | 42.7 (14) |
S1i—Sb1—S1iii | 110.12 (4) | O1vi—N4—O2vi | 53.5 (14) |
S1ii—Sb1—S1iii | 108.18 (7) | O1vii—N4—O2vi | 129.9 (18) |
S1i—Sb1—S1 | 108.18 (7) | O2v—N4—O2vi | 90.3 (4) |
S1ii—Sb1—S1 | 110.12 (4) | O1v—N4—O2 | 129.9 (18) |
S1iii—Sb1—S1 | 110.12 (4) | O1—N4—O2 | 53.5 (14) |
N1iv—Ni1—N1 | 94.8 (2) | O1vi—N4—O2 | 133 (2) |
N1iv—Ni1—N2 | 91.75 (17) | O1vii—N4—O2 | 42.7 (14) |
N1—Ni1—N2 | 173.07 (17) | O2v—N4—O2 | 172 (6) |
N1iv—Ni1—N2iv | 173.07 (17) | O2vi—N4—O2 | 90.3 (4) |
N1—Ni1—N2iv | 91.75 (17) | O1v—N4—O2vii | 42.7 (14) |
N2—Ni1—N2iv | 81.8 (2) | O1—N4—O2vii | 133 (2) |
N1iv—Ni1—N3 | 81.65 (18) | O1vi—N4—O2vii | 129.9 (18) |
N1—Ni1—N3 | 92.23 (18) | O1vii—N4—O2vii | 53.5 (14) |
N2—Ni1—N3 | 91.03 (17) | O2v—N4—O2vii | 90.3 (4) |
N2iv—Ni1—N3 | 95.78 (16) | O2vi—N4—O2vii | 172 (6) |
N1iv—Ni1—N3iv | 92.23 (18) | O2—N4—O2vii | 90.3 (4) |
N1—Ni1—N3iv | 81.65 (18) | O2vi—O1—O2 | 123 (3) |
N2—Ni1—N3iv | 95.78 (16) | O2vi—O1—N4 | 70 (2) |
N2iv—Ni1—N3iv | 91.03 (17) | O2—O1—N4 | 64.5 (16) |
N3—Ni1—N3iv | 171.0 (2) | O2vi—O1—O1vi | 28 (2) |
C1—N1—Ni1 | 108.5 (3) | O2—O1—O1vi | 99 (2) |
C2—N2—Ni1 | 108.7 (3) | N4—O1—O1vi | 41.9 (4) |
C3—N3—Ni1 | 108.2 (4) | O2vi—O1—O1vii | 106 (3) |
N1—C1—C3iv | 108.0 (6) | O2—O1—O1vii | 22.6 (16) |
N2—C2—C2iv | 109.3 (4) | N4—O1—O1vii | 41.9 (4) |
N3—C3—C1iv | 108.6 (5) | O1vi—O1—O1vii | 78.8 (13) |
O1v—N4—O1 | 142 (2) | O1vii—O2—O1 | 129 (3) |
O1v—N4—O1vi | 96.2 (8) | O1vii—O2—N4 | 67 (2) |
O1—N4—O1vi | 96.2 (8) | O1—O2—N4 | 62.0 (16) |
O1v—N4—O1vii | 96.2 (8) | O1vii—O2—O2vi | 110 (2) |
O1—N4—O1vii | 96.2 (8) | O1—O2—O2vi | 25.3 (17) |
O1vi—N4—O1vii | 142 (2) | N4—O2—O2vi | 44.9 (2) |
O1v—N4—O2v | 53.5 (14) | O1vii—O2—O2vii | 31.9 (18) |
O1—N4—O2v | 129.9 (18) | O1—O2—O2vii | 101 (3) |
O1vi—N4—O2v | 42.7 (14) | N4—O2—O2vii | 44.9 (2) |
O1vii—N4—O2v | 133 (2) | O2vi—O2—O2vii | 89.4 (8) |
O1v—N4—O2vi | 133 (2) | | |
Symmetry codes: (i) −x, −y, z; (ii) y, −x, −z; (iii) −y, x, −z; (iv) −x, −y+1, z; (v) −x+1, −y+1, z; (vi) −y+1, x, −z; (vii) y, −x+1, −z. |