Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805015771/mg6034sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805015771/mg6034Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 291 K
- Mean (N-C) = 0.017 Å
- R factor = 0.047
- wR factor = 0.119
- Data-to-parameter ratio = 27.2
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ?
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 30.00 From the CIF: _reflns_number_total 896 Count of symmetry unique reflns 502 Completeness (_total/calc) 178.49% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 394 Fraction of Friedel pairs measured 0.785 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 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
Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1997); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: program (reference)?.
CdHg(NCSe)4 | Dx = 3.974 Mg m−3 |
Mr = 732.91 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I4 | Cell parameters from 39 reflections |
Hall symbol: I -4 | θ = 7.4–17.8° |
a = 11.6495 (6) Å | µ = 26.11 mm−1 |
c = 4.5128 (8) Å | T = 291 K |
V = 612.44 (12) Å3 | Prism, colourless |
Z = 2 | 0.14 × 0.10 × 0.10 mm |
F(000) = 632 |
Bruker P4 diffractometer | 822 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.029 |
Graphite monochromator | θmax = 30.0°, θmin = 2.5° |
ω/2θ scans | h = −16→16 |
Absorption correction: ψ scan (XSCANS; Bruker,1996) | k = −16→16 |
Tmin = 0.044, Tmax = 0.073 | l = −6→6 |
1090 measured reflections | 3 standard reflections every 97 reflections |
896 independent reflections | intensity decay: none |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0753P)2 + 2.6748P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.047 | (Δ/σ)max < 0.001 |
wR(F2) = 0.119 | Δρmax = 2.20 e Å−3 |
S = 1.09 | Δρmin = −1.58 e Å−3 |
896 reflections | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
33 parameters | Extinction coefficient: 0.0103 (12) |
0 restraints | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.02 (2) |
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. |
x | y | z | Uiso*/Ueq | ||
Hg1 | 0.0000 | 0.5000 | 0.2500 | 0.0378 (3) | |
Cd1 | 0.0000 | 0.0000 | 0.0000 | 0.0450 (5) | |
Se1 | 0.12879 (11) | 0.35662 (11) | 0.5688 (3) | 0.0412 (4) | |
N1 | 0.0551 (10) | 0.1467 (9) | 0.266 (4) | 0.049 (2) | |
C1 | 0.0814 (10) | 0.2271 (10) | 0.377 (3) | 0.038 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg1 | 0.0338 (3) | 0.0338 (3) | 0.0460 (5) | 0.000 | 0.000 | 0.000 |
Cd1 | 0.0366 (5) | 0.0366 (5) | 0.0616 (13) | 0.000 | 0.000 | 0.000 |
Se1 | 0.0405 (6) | 0.0357 (6) | 0.0473 (8) | 0.0021 (4) | −0.0080 (5) | 0.0002 (5) |
N1 | 0.045 (5) | 0.038 (5) | 0.063 (7) | 0.000 (4) | −0.004 (7) | −0.004 (6) |
C1 | 0.033 (5) | 0.033 (5) | 0.049 (7) | −0.003 (4) | 0.008 (5) | 0.009 (5) |
Hg1—Se1i | 2.6666 (12) | Cd1—N1iv | 2.185 (12) |
Hg1—Se1ii | 2.6666 (12) | Cd1—N1v | 2.185 (12) |
Hg1—Se1iii | 2.6666 (12) | Cd1—N1vi | 2.185 (12) |
Hg1—Se1 | 2.6666 (12) | Se1—C1 | 1.825 (13) |
Cd1—N1 | 2.185 (12) | N1—C1 | 1.106 (18) |
Se1i—Hg1—Se1ii | 114.69 (6) | N1iv—Cd1—N1v | 113.3 (8) |
Se1i—Hg1—Se1iii | 106.92 (3) | N1—Cd1—N1vi | 113.3 (8) |
Se1ii—Hg1—Se1iii | 106.92 (3) | N1iv—Cd1—N1vi | 107.6 (4) |
Se1i—Hg1—Se1 | 106.92 (3) | N1v—Cd1—N1vi | 107.6 (4) |
Se1ii—Hg1—Se1 | 106.92 (3) | C1—Se1—Hg1 | 95.2 (4) |
Se1iii—Hg1—Se1 | 114.69 (6) | C1—N1—Cd1 | 173.2 (14) |
N1—Cd1—N1iv | 107.6 (4) | N1—C1—Se1 | 177.7 (13) |
N1—Cd1—N1v | 107.6 (4) |
Symmetry codes: (i) y−1/2, −x+1/2, −z+1/2; (ii) −y+1/2, x+1/2, −z+1/2; (iii) −x, −y+1, z; (iv) y, −x, −z; (v) −y, x, −z; (vi) −x, −y, z. |