Bis­[tris(1,2-ethanedi­amine-N,N')nickel(II)] tetra­thio­antimonate(V) nitrate

The title double salt, [Ni(C₂H₈N₂)₃]₂(SbS₄)(NO₃), was crystallized under solvothermal conditions. Hydro­gen bonds between the SbS₄^3- 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 SbS₄^3- anion on a axis.

Computing details

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 ?

Crystal data

[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) Å^3	Plates, violet
Z = 4	0.15 × 0.12 × 0.1 mm
F(000) = 1624

Data collection

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

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.031	Calculated w = 1/[σ^2(Fo^2) + (0.0409P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 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+0.001xFc^2λ^3/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Sb1—S1^i	2.320 (2)	N4—O1^v	1.199 (19)
Sb1—S1^ii	2.320 (2)	N4—O1	1.199 (19)
Sb1—S1^iii	2.320 (2)	N4—O1^vi	1.199 (19)
Sb1—S1	2.320 (2)	N4—O1^vii	1.199 (19)
Ni1—N1^iv	2.113 (4)	N4—O2^v	1.225 (18)
Ni1—N1	2.113 (4)	N4—O2^vi	1.225 (18)
Ni1—N2	2.129 (4)	N4—O2	1.225 (18)
Ni1—N2^iv	2.129 (4)	N4—O2^vii	1.225 (18)
Ni1—N3	2.139 (5)	O1—O2^vi	0.88 (3)
Ni1—N3^iv	2.139 (5)	O1—O2	1.09 (3)
N1—C1	1.483 (7)	O1—O1^vi	1.79 (3)
N2—C2	1.473 (6)	O1—O1^vii	1.79 (3)
N3—C3	1.467 (7)	O2—O1^vii	0.88 (3)
C1—C3^iv	1.521 (9)	O2—O2^vi	1.74 (3)
C2—C2^iv	1.522 (11)	O2—O2^vii	1.74 (3)
C3—C1^iv	1.521 (9)
S1^i—Sb1—S1^ii	110.12 (4)	O1—N4—O2^vi	42.7 (14)
S1^i—Sb1—S1^iii	110.12 (4)	O1^vi—N4—O2^vi	53.5 (14)
S1^ii—Sb1—S1^iii	108.18 (7)	O1^vii—N4—O2^vi	129.9 (18)
S1^i—Sb1—S1	108.18 (7)	O2^v—N4—O2^vi	90.3 (4)
S1^ii—Sb1—S1	110.12 (4)	O1^v—N4—O2	129.9 (18)
S1^iii—Sb1—S1	110.12 (4)	O1—N4—O2	53.5 (14)
N1^iv—Ni1—N1	94.8 (2)	O1^vi—N4—O2	133 (2)
N1^iv—Ni1—N2	91.75 (17)	O1^vii—N4—O2	42.7 (14)
N1—Ni1—N2	173.07 (17)	O2^v—N4—O2	172 (6)
N1^iv—Ni1—N2^iv	173.07 (17)	O2^vi—N4—O2	90.3 (4)
N1—Ni1—N2^iv	91.75 (17)	O1^v—N4—O2^vii	42.7 (14)
N2—Ni1—N2^iv	81.8 (2)	O1—N4—O2^vii	133 (2)
N1^iv—Ni1—N3	81.65 (18)	O1^vi—N4—O2^vii	129.9 (18)
N1—Ni1—N3	92.23 (18)	O1^vii—N4—O2^vii	53.5 (14)
N2—Ni1—N3	91.03 (17)	O2^v—N4—O2^vii	90.3 (4)
N2^iv—Ni1—N3	95.78 (16)	O2^vi—N4—O2^vii	172 (6)
N1^iv—Ni1—N3^iv	92.23 (18)	O2—N4—O2^vii	90.3 (4)
N1—Ni1—N3^iv	81.65 (18)	O2^vi—O1—O2	123 (3)
N2—Ni1—N3^iv	95.78 (16)	O2^vi—O1—N4	70 (2)
N2^iv—Ni1—N3^iv	91.03 (17)	O2—O1—N4	64.5 (16)
N3—Ni1—N3^iv	171.0 (2)	O2^vi—O1—O1^vi	28 (2)
C1—N1—Ni1	108.5 (3)	O2—O1—O1^vi	99 (2)
C2—N2—Ni1	108.7 (3)	N4—O1—O1^vi	41.9 (4)
C3—N3—Ni1	108.2 (4)	O2^vi—O1—O1^vii	106 (3)
N1—C1—C3^iv	108.0 (6)	O2—O1—O1^vii	22.6 (16)
N2—C2—C2^iv	109.3 (4)	N4—O1—O1^vii	41.9 (4)
N3—C3—C1^iv	108.6 (5)	O1^vi—O1—O1^vii	78.8 (13)
O1^v—N4—O1	142 (2)	O1^vii—O2—O1	129 (3)
O1^v—N4—O1^vi	96.2 (8)	O1^vii—O2—N4	67 (2)
O1—N4—O1^vi	96.2 (8)	O1—O2—N4	62.0 (16)
O1^v—N4—O1^vii	96.2 (8)	O1^vii—O2—O2^vi	110 (2)
O1—N4—O1^vii	96.2 (8)	O1—O2—O2^vi	25.3 (17)
O1^vi—N4—O1^vii	142 (2)	N4—O2—O2^vi	44.9 (2)
O1^v—N4—O2^v	53.5 (14)	O1^vii—O2—O2^vii	31.9 (18)
O1—N4—O2^v	129.9 (18)	O1—O2—O2^vii	101 (3)
O1^vi—N4—O2^v	42.7 (14)	N4—O2—O2^vii	44.9 (2)
O1^vii—N4—O2^v	133 (2)	O2^vi—O2—O2^vii	89.4 (8)
O1^v—N4—O2^vi	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.