Cobalt mercury tetra­seleno­cyanate, CoHg(SeCN)₄

The title compound, CoHg(SeCN)₄, was obtained by self-assembly. X-ray crystal structure analysis reveals that it has an extended three-dimensional network structure in which the slightly distorted CoN₄ and HgSe₄ tetra­hedra are connected by -SeCN- bridges. The Hg and Co atoms lie on positions of symmetry.

Key indicators

• Single-crystal X-ray study
• T = 213 K
• Mean [sigma](N-C) = 0.019 Å
• R factor = 0.041
• wR factor = 0.103
• Data-to-parameter ratio = 17.2

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound ..          ?
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           25.98
           From the CIF: _reflns_number_total                566
           Count of symmetry unique reflns          323
           Completeness (_total/calc)            175.23%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       243
           Fraction of Friedel pairs measured     0.752
           Are heavy atom types Z>Si present        yes

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   2 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 2003).

Cobalt mercury tetraselenocyanate

Crystal data

CoHg(SeCN)4	Dx = 3.838 Mg m^−3
Mr = 679.44	Melting point: 500.6 K
Tetragonal, I4	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: I -4	Cell parameters from 1547 reflections
a = 11.281 (3) Å	θ = 3.6–26.0°
c = 4.6207 (12) Å	µ = 26.79 mm^−1
V = 588.0 (3) Å^3	T = 213 K
Z = 2	Block, dark red
F(000) = 590	0.40 × 0.16 × 0.12 mm

Data collection

Siemens SMART CCD area-detector diffractometer	566 independent reflections
Radiation source: fine-focus sealed tube	545 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.083
Detector resolution: 8.33 pixels mm^-1	θmax = 26.0°, θmin = 3.6°
ω scans	h = −9→13
Absorption correction: numerical (SMART; Siemens, 1996)	k = −13→13
Tmin = 0.009, Tmax = 0.040	l = −5→5
1547 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0465P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.042	(Δ/σ)max = 0.001
wR(F^2) = 0.103	Δρmax = 1.57 e Å^−3
S = 1.10	Δρmin = −1.87 e Å^−3
566 reflections	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
33 parameters	Extinction coefficient: 0.0093 (13)
0 restraints	Absolute structure: Flack (1983); 245 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.06 (3)

Special details

Experimental. Absorption correction was performed using face-indexing techniques.

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
Hg1	0.0000	0.0000	0.0000	0.0221 (4)
Se1	−0.12363 (12)	−0.15290 (11)	−0.3183 (3)	0.0229 (4)
Co1	0.0000	−0.5000	0.2500	0.0216 (9)
N1	−0.0487 (10)	−0.3636 (8)	0.013 (4)	0.025 (2)
C1	−0.0770 (11)	−0.2837 (13)	−0.117 (3)	0.025 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Hg1	0.0166 (4)	0.0166 (4)	0.0330 (6)	0.000	0.000	0.000
Se1	0.0214 (7)	0.0161 (7)	0.0311 (9)	−0.0017 (5)	−0.0047 (5)	0.0001 (5)
Co1	0.0146 (11)	0.0146 (11)	0.036 (2)	0.000	0.000	0.000
N1	0.025 (5)	0.012 (5)	0.039 (6)	0.000 (4)	0.001 (7)	0.000 (6)
C1	0.011 (6)	0.027 (7)	0.038 (8)	0.004 (5)	0.002 (5)	−0.007 (6)

Geometric parameters (Å, º)

Hg1—Se1	2.6615 (14)	Co1—N1^iv	1.967 (13)
Hg1—Se1^i	2.6615 (14)	Co1—N1^v	1.967 (13)
Hg1—Se1^ii	2.6615 (14)	Co1—N1^vi	1.967 (13)
Hg1—Se1^iii	2.6615 (14)	Co1—N1	1.967 (13)
Se1—C1	1.822 (15)	N1—C1	1.13 (2)
Se1—Hg1—Se1^i	107.78 (3)	N1^iv—Co1—N1^vi	112.4 (9)
Se1—Hg1—Se1^ii	112.91 (6)	N1^v—Co1—N1^vi	108.0 (4)
Se1^i—Hg1—Se1^ii	107.78 (3)	N1^iv—Co1—N1	108.0 (4)
Se1—Hg1—Se1^iii	107.78 (3)	N1^v—Co1—N1	112.4 (9)
Se1^i—Hg1—Se1^iii	112.91 (6)	N1^vi—Co1—N1	108.0 (4)
Se1^ii—Hg1—Se1^iii	107.78 (3)	C1—N1—Co1	178.4 (15)
C1—Se1—Hg1	95.3 (4)	N1—C1—Se1	178.5 (14)
N1^iv—Co1—N1^v	108.0 (4)
Se1^i—Hg1—Se1—C1	−108.6 (4)	Se1^iii—Hg1—Se1—C1	13.6 (4)
Se1^ii—Hg1—Se1—C1	132.5 (4)

Symmetry codes: (i) y, −x, −z; (ii) −x, −y, z; (iii) −y, x, −z; (iv) −y−1/2, x−1/2, −z+1/2; (v) −x, −y−1, z; (vi) y+1/2, −x−1/2, −z+1/2.