Bis­(diethyl­enetri­amine)­mercury(II) bis­(thio­cyanate)

Mercury(II) in the title compound, [Hg(C₄H₁₃N₃)₂](SCN)₂, is six-coordinated with two diethyl­enetri­amine (dien) ligands in a sym-facial configuration. The complex cation has a twofold axis of symmetry, and the secondary amine groups are in trans positions.

Key indicators

• Single-crystal X-ray study
• T = 130 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.019
• wR factor = 0.049
• Data-to-parameter ratio = 16.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

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Computing details

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Bis(diethylenetriamine)mercury(II) thiocyanate

Crystal data

[Hg(C4H13N3)2](SCN)2	F(000) = 1016
Mr = 523.1	Dx = 1.953 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 25 reflections
a = 7.6710 (7) Å	θ = 11.3–14.3°
b = 13.9712 (6) Å	µ = 8.89 mm^−1
c = 16.639 (2) Å	T = 130 K
β = 93.809 (9)°	Prism, colourless
V = 1779.3 (3) Å^3	0.5 × 0.2 × 0.07 mm
Z = 4

Data collection

Enraf-Nonius TurboCAD-4 diffractometer	1485 reflections with I > 2σ(I)
Radiation source: Enraf-Nonius FR590	Rint = 0.023
Graphite monochromator	θmax = 25.0°, θmin = 2.5°
non–profiled ω scans	h = 0→9
Absorption correction: ψ scan (North et al., 1968)	k = 0→16
Tmin = 0.089, Tmax = 0.537	l = −19→19
1690 measured reflections	3 standard reflections every 120 min
1565 independent reflections	intensity decay: 9%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.049	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0341P)^2 + 3.0573P] where P = (Fo^2 + 2Fc^2)/3
1565 reflections	(Δ/σ)max < 0.001
96 parameters	Δρmax = 0.95 e Å^−3
0 restraints	Δρmin = −1.42 e Å^−3

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. The structure was solved with SHELX97 by Patterson methods and refined using SHELX97. 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
C1	0.3605 (5)	0.0453 (3)	0.0868 (2)	0.0201 (8)
H1A	0.2800	0.0012	0.0561	0.024*
H1B	0.4802	0.0334	0.0703	0.024*
C2	0.3091 (5)	0.1477 (3)	0.0674 (3)	0.0220 (9)
H2A	0.3141	0.1587	0.0088	0.026*
H2B	0.1872	0.1584	0.0815	0.026*
C3	0.5880 (5)	0.2367 (3)	0.0747 (2)	0.0228 (8)
H3A	0.5649	0.2785	0.0272	0.027*
H3B	0.6396	0.1762	0.0564	0.027*
C4	0.7150 (5)	0.2855 (3)	0.1351 (3)	0.0252 (9)
H4A	0.8237	0.3014	0.1091	0.03*
H4B	0.6632	0.3459	0.1534	0.03*
C5	0.7667 (5)	−0.0621 (3)	0.1500 (2)	0.0247 (9)
N1	0.3541 (4)	0.0261 (2)	0.17350 (19)	0.0181 (7)
H1C	0.4072	−0.0315	0.1859	0.022*
H1D	0.2397	0.0223	0.1865	0.022*
N2	0.4243 (4)	0.2164 (2)	0.1116 (2)	0.0196 (7)
H2	0.3639	0.2736	0.1164	0.024*
N3	0.7566 (4)	0.2229 (2)	0.2049 (2)	0.0225 (7)
H3C	0.8107	0.2581	0.2461	0.027*
H3D	0.8327	0.1758	0.1909	0.027*
N4	0.6682 (5)	−0.1178 (3)	0.1709 (2)	0.0312 (8)
S1	0.90594 (14)	0.01518 (9)	0.11620 (8)	0.0338 (3)
Hg1	0.5	0.151351 (13)	0.25	0.01504 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0225 (19)	0.0189 (19)	0.0182 (19)	−0.0024 (16)	−0.0041 (15)	−0.0038 (17)
C2	0.021 (2)	0.025 (2)	0.019 (2)	0.0006 (16)	−0.0062 (16)	0.0043 (16)
C3	0.027 (2)	0.023 (2)	0.019 (2)	−0.0002 (16)	0.0033 (16)	0.0031 (17)
C4	0.030 (2)	0.021 (2)	0.026 (2)	−0.0085 (17)	0.0089 (17)	0.0011 (17)
C5	0.028 (2)	0.026 (2)	0.020 (2)	0.0153 (18)	−0.0034 (16)	−0.0015 (17)
N1	0.0189 (15)	0.0168 (17)	0.0180 (17)	−0.0006 (12)	−0.0043 (13)	0.0014 (13)
N2	0.0210 (16)	0.0151 (15)	0.0229 (17)	0.0039 (13)	0.0025 (13)	−0.0010 (14)
N3	0.0195 (17)	0.0244 (18)	0.0234 (18)	−0.0035 (13)	−0.0002 (13)	−0.0034 (15)
N4	0.034 (2)	0.0259 (19)	0.033 (2)	0.0119 (18)	0.0025 (17)	0.0023 (17)
S1	0.0237 (5)	0.0375 (6)	0.0396 (7)	0.0036 (5)	−0.0011 (5)	−0.0021 (5)
Hg1	0.01616 (12)	0.01564 (12)	0.01302 (12)	0	−0.00128 (7)	0

Geometric parameters (Å, º)

C1—N1	1.471 (5)	C5—N4	1.154 (6)
C1—C2	1.513 (5)	C5—S1	1.644 (5)
C1—H1A	0.9900	N1—Hg1	2.396 (3)
C1—H1B	0.9900	N1—H1C	0.9200
C2—N2	1.468 (5)	N1—H1D	0.9200
C2—H2A	0.9900	N2—Hg1	2.508 (3)
C2—H2B	0.9900	N2—H2	0.9300
C3—N2	1.461 (5)	N3—Hg1	2.373 (3)
C3—C4	1.514 (6)	N3—H3C	0.9200
C3—H3A	0.9900	N3—H3D	0.9200
C3—H3B	0.9900	Hg1—N3^i	2.373 (3)
C4—N3	1.472 (5)	Hg1—N1^i	2.396 (3)
C4—H4A	0.9900	Hg1—N2^i	2.508 (3)
C4—H4B	0.9900
N1—C1—C2	110.9 (3)	Hg1—N1—H1D	109.6
N1—C1—H1A	109.5	H1C—N1—H1D	108.2
C2—C1—H1A	109.5	C3—N2—C2	115.0 (3)
N1—C1—H1B	109.5	C3—N2—Hg1	107.6 (2)
C2—C1—H1B	109.5	C2—N2—Hg1	108.5 (2)
H1A—C1—H1B	108.1	C3—N2—H2	108.5
N2—C2—C1	111.8 (3)	C2—N2—H2	108.5
N2—C2—H2A	109.3	Hg1—N2—H2	108.5
C1—C2—H2A	109.3	C4—N3—Hg1	111.0 (2)
N2—C2—H2B	109.3	C4—N3—H3C	109.4
C1—C2—H2B	109.3	Hg1—N3—H3C	109.4
H2A—C2—H2B	107.9	C4—N3—H3D	109.4
N2—C3—C4	110.0 (3)	Hg1—N3—H3D	109.4
N2—C3—H3A	109.7	H3C—N3—H3D	108.0
C4—C3—H3A	109.7	N3—Hg1—N3^i	130.19 (17)
N2—C3—H3B	109.7	N3—Hg1—N1	120.47 (11)
C4—C3—H3B	109.7	N3^i—Hg1—N1	96.18 (11)
H3A—C3—H3B	108.2	N3—Hg1—N1^i	96.18 (11)
N3—C4—C3	110.6 (3)	N3^i—Hg1—N1^i	120.47 (11)
N3—C4—H4A	109.5	N1—Hg1—N1^i	86.24 (15)
C3—C4—H4A	109.5	N3—Hg1—N2^i	89.52 (11)
N3—C4—H4B	109.5	N3^i—Hg1—N2^i	72.74 (11)
C3—C4—H4B	109.5	N1—Hg1—N2^i	145.46 (11)
H4A—C4—H4B	108.1	N1^i—Hg1—N2^i	72.85 (11)
N4—C5—S1	177.5 (4)	N3—Hg1—N2	72.74 (11)
C1—N1—Hg1	110.1 (2)	N3^i—Hg1—N2	89.52 (11)
C1—N1—H1C	109.6	N1—Hg1—N2	72.85 (11)
Hg1—N1—H1C	109.6	N1^i—Hg1—N2	145.46 (11)
C1—N1—H1D	109.6	N2^i—Hg1—N2	137.52 (15)

Symmetry code: (i) −x+1, y, −z+1/2.