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The title double salt, [Ni(C2H8N2)3]2(SbS4)(NO3), was crystallized under solvothermal conditions. Hydro­gen bonds between the SbS43- anions (at four sites) and the [Ni(en)3]2+ (en = ethyl­enedi­amine) cations (at two sites) form a three-dimensional network. The NO3- anion is disordered over four sites. The cation lies on a twofold rotation axis and the SbS43- anion on a \bar 4 axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100009082/sk1373sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100009082/sk1373Isup2.hkl
Contains datablock I

CCDC reference: 150775

Computing details top

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 m3
Mr = 790.04Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I42dCell parameters from 90 reflections
Hall symbol: I -4 2bwθ = 16–22°
a = 10.276 (2) ŵ = 2.31 mm1
c = 30.249 (4) ÅT = 293 K
V = 3194.3 (13) Å3Plates, violet
Z = 40.15 × 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 tubeθmax = 27.5°, θmin = 2.1°
Graphite monochromatorh = 113
ωθ–scank = 013
2222 measured reflectionsl = 039
1233 independent reflections4 standard reflections every every 2 h min
934 reflections with I > 2σ(I) intensity decay: neglible
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.031Calculated w = 1/[σ2(Fo2) + (0.0409P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.070(Δ/σ)max < 0.001
S = 1.00Δρmax = 1.08 e Å3
1233 reflectionsΔρmin = 0.87 e Å3
92 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00055 (10)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983)
Secondary atom site location: difference Fourier mapAbsolute 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
xyzUiso*/UeqOcc. (<1)
Sb10.00000.00000.00000.02445 (15)
S10.15240 (13)0.10100 (14)0.04498 (4)0.0378 (3)
Ni10.00000.50000.04330 (2)0.0340 (2)
N10.1145 (5)0.4011 (4)0.0906 (1)0.046 (1)
H1A0.11990.31620.08360.055*
H1B0.07800.40810.11750.055*
N20.0970 (4)0.5949 (4)0.0099 (1)0.0388 (9)
H2A0.06820.67730.01240.047*
H2B0.18320.59710.00470.047*
N30.1542 (5)0.3612 (4)0.0489 (2)0.0545 (13)
H3A0.12130.28030.05120.065*
H3B0.20520.36440.02470.065*
C10.2462 (7)0.4601 (6)0.0909 (2)0.0584 (17)
H1C0.29180.43630.11780.070*
H1D0.29630.42900.06590.070*
C20.0705 (5)0.5227 (5)0.05099 (14)0.0427 (15)
H2C0.12810.44820.05310.051*
H2D0.08610.57840.07630.051*
C30.2306 (7)0.3929 (6)0.0884 (2)0.0589 (17)
H3C0.31530.35170.08680.071*
H3D0.18640.36120.11460.071*
N40.50000.50000.00000.054 (2)
O10.489 (8)0.390 (2)0.0130 (9)0.090 (9)0.375
O20.403 (5)0.431 (7)0.003 (2)0.10 (1)0.375
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.02461 (18)0.02461 (18)0.0241 (2)0.0000.0000.000
S10.0341 (6)0.0396 (7)0.0397 (7)0.0026 (6)0.0100 (5)0.0116 (6)
Ni10.0502 (5)0.0236 (4)0.0282 (4)0.0027 (8)0.0000.000
N10.076 (4)0.031 (2)0.032 (2)0.003 (3)0.003 (2)0.0019 (18)
N20.048 (2)0.032 (2)0.037 (2)0.002 (2)0.0032 (19)0.0030 (18)
N30.076 (3)0.037 (2)0.051 (3)0.017 (3)0.011 (3)0.005 (2)
C10.075 (4)0.060 (4)0.040 (3)0.006 (4)0.011 (3)0.001 (3)
C20.059 (3)0.035 (4)0.033 (2)0.010 (3)0.006 (2)0.001 (2)
C30.073 (4)0.055 (4)0.049 (4)0.012 (4)0.014 (3)0.002 (3)
N40.056 (3)0.056 (3)0.049 (4)0.0000.0000.000
O10.12 (2)0.048 (10)0.105 (12)0.026 (18)0.025 (19)0.016 (8)
O20.06 (2)0.10 (2)0.14 (2)0.034 (15)0.027 (18)0.07 (2)
Geometric parameters (Å, º) top
Sb1—S1i2.320 (2)N4—O1v1.199 (19)
Sb1—S1ii2.320 (2)N4—O11.199 (19)
Sb1—S1iii2.320 (2)N4—O1vi1.199 (19)
Sb1—S12.320 (2)N4—O1vii1.199 (19)
Ni1—N1iv2.113 (4)N4—O2v1.225 (18)
Ni1—N12.113 (4)N4—O2vi1.225 (18)
Ni1—N22.129 (4)N4—O21.225 (18)
Ni1—N2iv2.129 (4)N4—O2vii1.225 (18)
Ni1—N32.139 (5)O1—O2vi0.88 (3)
Ni1—N3iv2.139 (5)O1—O21.09 (3)
N1—C11.483 (7)O1—O1vi1.79 (3)
N2—C21.473 (6)O1—O1vii1.79 (3)
N3—C31.467 (7)O2—O1vii0.88 (3)
C1—C3iv1.521 (9)O2—O2vi1.74 (3)
C2—C2iv1.522 (11)O2—O2vii1.74 (3)
C3—C1iv1.521 (9)
S1i—Sb1—S1ii110.12 (4)O1—N4—O2vi42.7 (14)
S1i—Sb1—S1iii110.12 (4)O1vi—N4—O2vi53.5 (14)
S1ii—Sb1—S1iii108.18 (7)O1vii—N4—O2vi129.9 (18)
S1i—Sb1—S1108.18 (7)O2v—N4—O2vi90.3 (4)
S1ii—Sb1—S1110.12 (4)O1v—N4—O2129.9 (18)
S1iii—Sb1—S1110.12 (4)O1—N4—O253.5 (14)
N1iv—Ni1—N194.8 (2)O1vi—N4—O2133 (2)
N1iv—Ni1—N291.75 (17)O1vii—N4—O242.7 (14)
N1—Ni1—N2173.07 (17)O2v—N4—O2172 (6)
N1iv—Ni1—N2iv173.07 (17)O2vi—N4—O290.3 (4)
N1—Ni1—N2iv91.75 (17)O1v—N4—O2vii42.7 (14)
N2—Ni1—N2iv81.8 (2)O1—N4—O2vii133 (2)
N1iv—Ni1—N381.65 (18)O1vi—N4—O2vii129.9 (18)
N1—Ni1—N392.23 (18)O1vii—N4—O2vii53.5 (14)
N2—Ni1—N391.03 (17)O2v—N4—O2vii90.3 (4)
N2iv—Ni1—N395.78 (16)O2vi—N4—O2vii172 (6)
N1iv—Ni1—N3iv92.23 (18)O2—N4—O2vii90.3 (4)
N1—Ni1—N3iv81.65 (18)O2vi—O1—O2123 (3)
N2—Ni1—N3iv95.78 (16)O2vi—O1—N470 (2)
N2iv—Ni1—N3iv91.03 (17)O2—O1—N464.5 (16)
N3—Ni1—N3iv171.0 (2)O2vi—O1—O1vi28 (2)
C1—N1—Ni1108.5 (3)O2—O1—O1vi99 (2)
C2—N2—Ni1108.7 (3)N4—O1—O1vi41.9 (4)
C3—N3—Ni1108.2 (4)O2vi—O1—O1vii106 (3)
N1—C1—C3iv108.0 (6)O2—O1—O1vii22.6 (16)
N2—C2—C2iv109.3 (4)N4—O1—O1vii41.9 (4)
N3—C3—C1iv108.6 (5)O1vi—O1—O1vii78.8 (13)
O1v—N4—O1142 (2)O1vii—O2—O1129 (3)
O1v—N4—O1vi96.2 (8)O1vii—O2—N467 (2)
O1—N4—O1vi96.2 (8)O1—O2—N462.0 (16)
O1v—N4—O1vii96.2 (8)O1vii—O2—O2vi110 (2)
O1—N4—O1vii96.2 (8)O1—O2—O2vi25.3 (17)
O1vi—N4—O1vii142 (2)N4—O2—O2vi44.9 (2)
O1v—N4—O2v53.5 (14)O1vii—O2—O2vii31.9 (18)
O1—N4—O2v129.9 (18)O1—O2—O2vii101 (3)
O1vi—N4—O2v42.7 (14)N4—O2—O2vii44.9 (2)
O1vii—N4—O2v133 (2)O2vi—O2—O2vii89.4 (8)
O1v—N4—O2vi133 (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.
 

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