Buy article online - an online subscription or single-article purchase is required to access this article.
Crystals of the title compound, [HgI2(C18H14N4O2)]n, were obtained by the reaction of HgI2 and p-phenylene-bis(pyridine-3-carboxamide) in DMF. The asymmetric unit is composed of only half of the formula unit; the mercury atom lies on a crystallographic twofold rotation axis, and there is an inversion centre at the centre of the benzene ring. Each HgII atom is coordinated by two I atoms and two N atoms from two p-phenylene-bis(pyridine-3-carboxamide) (bpfb) ligands, in a distorted tetrahetral geometry. Bpfb acts as a bifunctional bridging ligand, linking HgII atoms into a one-dimensional chain. Hydrogen-bonding interactions between the O atom and the H atoms of bpfb ligands result in a two-dimensional supramolecular network.
Supporting information
CCDC reference: 644025
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.034
- wR factor = 0.083
- Data-to-parameter ratio = 16.0
checkCIF/PLATON results
No syntax errors found
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
0 ALERT level C = Check and explain
2 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
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL.
catena-Poly[[diiodidomercury(II)]-µ-
N,
N'-
p-phenylene-bis(pyridine-3- carboxamide)-k
2N:
N']
top
Crystal data top
[HgI2(C18H14N4O2)] | F(000) = 1408 |
Mr = 772.72 | Dx = 2.542 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 979 reflections |
a = 16.035 (4) Å | θ = 2.6–27.6° |
b = 5.0473 (14) Å | µ = 10.70 mm−1 |
c = 25.060 (7) Å | T = 293 K |
β = 95.558 (4)° | Block, colourless |
V = 2018.7 (9) Å3 | 0.26 × 0.20 × 0.10 mm |
Z = 4 | |
Data collection top
Bruker SMART APEX CCD area-detector diffractometer | 1964 independent reflections |
Radiation source: fine-focus sealed tube | 1806 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
φ and ω scans | θmax = 26.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −19→19 |
Tmin = 0.092, Tmax = 0.342 | k = −2→6 |
4801 measured reflections | l = −30→30 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.083 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) |
1964 reflections | (Δ/σ)max < 0.001 |
123 parameters | Δρmax = 1.20 e Å−3 |
0 restraints | Δρmin = −1.20 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.6234 (4) | 0.1798 (12) | 0.8275 (3) | 0.0440 (13) | |
H1 | 0.6619 | 0.1327 | 0.8037 | 0.053* | |
C2 | 0.6440 (4) | 0.3816 (11) | 0.8649 (3) | 0.0466 (14) | |
H2 | 0.6961 | 0.4639 | 0.8666 | 0.056* | |
C3 | 0.5855 (4) | 0.4568 (10) | 0.8993 (2) | 0.0423 (13) | |
H3 | 0.5967 | 0.5970 | 0.9230 | 0.051* | |
C4 | 0.5097 (4) | 0.3197 (9) | 0.8980 (2) | 0.0341 (11) | |
C5 | 0.4952 (3) | 0.1224 (9) | 0.8593 (2) | 0.0378 (12) | |
H5 | 0.4441 | 0.0339 | 0.8572 | 0.045* | |
C6 | 0.4448 (4) | 0.4000 (9) | 0.9326 (2) | 0.0373 (12) | |
C10 | 0.3055 (4) | 0.0462 (9) | 1.0124 (2) | 0.0401 (12) | |
H10 | 0.3430 | −0.0919 | 1.0205 | 0.048* | |
C11 | 0.3222 (4) | 0.2308 (7) | 0.9732 (3) | 0.0346 (12) | |
C12 | 0.2659 (4) | 0.4353 (9) | 0.9606 (2) | 0.0421 (13) | |
H12 | 0.2759 | 0.5584 | 0.9344 | 0.051* | |
Hg1 | 0.5000 | −0.25695 (5) | 0.7500 | 0.03837 (13) | |
I1 | 0.35420 (2) | −0.37587 (8) | 0.784428 (16) | 0.04962 (15) | |
N1 | 0.5500 (3) | 0.0533 (8) | 0.82530 (19) | 0.0393 (10) | |
N2 | 0.3947 (3) | 0.1996 (8) | 0.94642 (19) | 0.0384 (11) | |
H2A | 0.4083 | 0.0411 | 0.9382 | 0.046* | |
O1 | 0.4366 (3) | 0.6320 (6) | 0.94650 (16) | 0.0480 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.033 (3) | 0.050 (2) | 0.049 (4) | 0.000 (2) | 0.004 (3) | 0.006 (3) |
C2 | 0.035 (3) | 0.054 (3) | 0.049 (4) | −0.010 (3) | −0.002 (3) | 0.003 (3) |
C3 | 0.044 (3) | 0.040 (2) | 0.042 (3) | −0.008 (2) | −0.003 (3) | 0.001 (2) |
C4 | 0.037 (3) | 0.0292 (19) | 0.035 (3) | 0.000 (2) | −0.003 (2) | 0.000 (2) |
C5 | 0.035 (3) | 0.036 (2) | 0.043 (3) | −0.001 (2) | 0.007 (2) | −0.005 (2) |
C6 | 0.042 (3) | 0.031 (2) | 0.040 (3) | 0.004 (2) | 0.005 (2) | 0.000 (2) |
C10 | 0.043 (3) | 0.032 (2) | 0.044 (3) | 0.007 (2) | 0.000 (2) | 0.004 (2) |
C11 | 0.041 (4) | 0.028 (2) | 0.036 (3) | −0.002 (2) | 0.005 (2) | −0.0073 (19) |
C12 | 0.052 (4) | 0.033 (2) | 0.041 (3) | 0.003 (2) | 0.008 (3) | 0.007 (2) |
Hg1 | 0.0314 (2) | 0.04545 (19) | 0.0391 (2) | 0.000 | 0.00722 (14) | 0.000 |
I1 | 0.0330 (2) | 0.0635 (3) | 0.0533 (3) | −0.00897 (17) | 0.00918 (18) | −0.00167 (18) |
N1 | 0.034 (2) | 0.041 (2) | 0.044 (3) | −0.0026 (18) | 0.008 (2) | −0.0060 (19) |
N2 | 0.044 (3) | 0.0284 (17) | 0.044 (3) | 0.0016 (19) | 0.011 (2) | −0.0067 (18) |
O1 | 0.062 (3) | 0.0254 (16) | 0.057 (3) | 0.0003 (16) | 0.011 (2) | −0.0081 (16) |
Geometric parameters (Å, º) top
C1—N1 | 1.335 (7) | C10—C12i | 1.389 (8) |
C1—C2 | 1.401 (9) | C10—C11 | 1.398 (7) |
C1—H1 | 0.9300 | C10—H10 | 0.9300 |
C2—C3 | 1.387 (9) | C11—C12 | 1.387 (7) |
C2—H2 | 0.9300 | C11—N2 | 1.406 (8) |
C3—C4 | 1.397 (8) | C12—C10i | 1.389 (8) |
C3—H3 | 0.9300 | C12—H12 | 0.9300 |
C4—C5 | 1.393 (8) | Hg1—N1 | 2.523 (4) |
C4—C6 | 1.474 (8) | Hg1—N1ii | 2.523 (4) |
C5—N1 | 1.330 (7) | Hg1—I1ii | 2.6385 (7) |
C5—H5 | 0.9300 | Hg1—I1 | 2.6385 (7) |
C6—O1 | 1.232 (6) | N2—H2A | 0.8600 |
C6—N2 | 1.358 (7) | | |
| | | |
N1—C1—C2 | 121.7 (6) | C11—C10—H10 | 119.3 |
N1—C1—H1 | 119.1 | C12—C11—C10 | 119.4 (5) |
C2—C1—H1 | 119.1 | C12—C11—N2 | 121.6 (5) |
C3—C2—C1 | 119.0 (5) | C10—C11—N2 | 119.0 (5) |
C3—C2—H2 | 120.5 | C11—C12—C10i | 119.2 (5) |
C1—C2—H2 | 120.5 | C11—C12—H12 | 120.4 |
C2—C3—C4 | 119.3 (5) | C10i—C12—H12 | 120.4 |
C2—C3—H3 | 120.3 | N1—Hg1—N1ii | 103.3 (2) |
C4—C3—H3 | 120.3 | N1—Hg1—I1ii | 99.10 (10) |
C5—C4—C3 | 117.2 (5) | N1ii—Hg1—I1ii | 97.14 (10) |
C5—C4—C6 | 121.7 (5) | N1—Hg1—I1 | 97.14 (10) |
C3—C4—C6 | 120.8 (5) | N1ii—Hg1—I1 | 99.10 (10) |
N1—C5—C4 | 123.8 (5) | I1ii—Hg1—I1 | 153.70 (2) |
N1—C5—H5 | 118.1 | C5—N1—C1 | 118.9 (5) |
C4—C5—H5 | 118.1 | C5—N1—Hg1 | 117.4 (3) |
O1—C6—N2 | 123.6 (5) | C1—N1—Hg1 | 122.9 (4) |
O1—C6—C4 | 121.9 (5) | C6—N2—C11 | 125.2 (4) |
N2—C6—C4 | 114.5 (4) | C6—N2—H2A | 117.4 |
C12i—C10—C11 | 121.4 (5) | C11—N2—H2A | 117.4 |
C12i—C10—H10 | 119.3 | | |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+2; (ii) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2A···O1iii | 0.86 | 2.12 | 2.943 (5) | 160 |
Symmetry code: (iii) x, y−1, z. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.