Literature DB >> 22058836

Di-μ-chlorido-bis-{[4-amino-3,5-bis-(2-pyrid-yl)-4H-1,2,4-triazole-κN]chloridomercury(II)}.

Jian Guo1, Min Tang, Jing Chen, Cheng-Peng Li.   

Abstract

In the centrosymmetric binuclear title complex, [Hg(2)Cl(4)(C(12)H(10)N(6))(2)], the Hg(II) ion is five-coordinated by two N atoms and three chloride ions with a distorted square-pyramidal geometry. In the complex, there is an intra-molecular N-H⋯N hydrogen bond. In the crystal, the binuclear units are connected by inter-molecular N-H⋯Cl hydrogen bonds, as well as π-π stacking inter-actions [centroid-centroid distances = 3.526 (2) and 3.696 (2) Å], forming a two-dimensional layered structure parallel to (010).

Entities:  

Year:  2011        PMID： 22058836      PMCID： PMC3200639          DOI： 10.1107/S1600536811029886

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For background information on triazole derivatives, see: Klingele et al. (2009 ▶); Shao et al. (2004 ▶); Huang et al. (2011 ▶). For the coordination compounds synthesized with related triazole ligands, see: Du et al. (2007 ▶, 2008 ▶). For a description of the geometry of complexes with five-coordinate metal ions, see: Addison et al. (1984 ▶).

Experimental

Crystal data

[Hg2Cl4(C12H10N6)2] M = 1019.50 Orthorhombic, a = 11.3634 (4) Å b = 14.9962 (6) Å c = 17.2328 (7) Å V = 2936.6 (2) Å3 Z = 4 Mo Kα radiation μ = 10.85 mm−1 T = 296 K 0.28 × 0.22 × 0.20 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.475, T max = 1.000 14063 measured reflections 2596 independent reflections 2071 reflections with I > 2σ(I) R int = 0.023

Refinement

R[F 2 > 2σ(F 2)] = 0.022 wR(F 2) = 0.058 S = 1.08 2596 reflections 190 parameters H-atom parameters constrained Δρmax = 0.53 e Å−3 Δρmin = −1.26 e Å−3 Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811029886/su2294sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811029886/su2294Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Hg2Cl4(C12H10N6)2]F(000) = 1904
Mr = 1019.50Dx = 2.306 Mg m−3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 5032 reflections
a = 11.3634 (4) Åθ = 2.5–28.1°
b = 14.9962 (6) ŵ = 10.85 mm−1
c = 17.2328 (7) ÅT = 296 K
V = 2936.6 (2) Å3Block, colourless
Z = 40.28 × 0.22 × 0.20 mm
Bruker SMART CCD area-detector diffractometer2596 independent reflections
Radiation source: fine-focus sealed tube2071 reflections with I > 2σ(I)
graphiteRint = 0.023
phi and ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −8→13
Tmin = 0.475, Tmax = 1.000k = −16→17
14063 measured reflectionsl = −20→19
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058H-atom parameters constrained
S = 1.08w = 1/[σ2(Fo2) + (0.028P)2 + 2.8778P] where P = (Fo2 + 2Fc2)/3
2596 reflections(Δ/σ)max = 0.001
190 parametersΔρmax = 0.53 e Å−3
0 restraintsΔρmin = −1.26 e Å−3
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.
xyzUiso*/Ueq
Hg10.661120 (15)0.459756 (11)0.997612 (9)0.04268 (8)
Cl10.66817 (10)0.31955 (7)0.92929 (6)0.0460 (3)
Cl20.53708 (10)0.57586 (7)0.92105 (6)0.0486 (3)
N10.7468 (3)0.5214 (2)1.11219 (19)0.0384 (8)
N20.8392 (3)0.5359 (2)0.9665 (2)0.0381 (9)
N30.8938 (3)0.5633 (2)0.89923 (19)0.0377 (8)
N40.9726 (3)0.63366 (19)0.99779 (15)0.0266 (7)
N51.0319 (3)0.6981 (2)1.04316 (18)0.0356 (8)
H5A1.00210.74951.02640.053*
H5B1.10860.69321.03350.053*
N61.1599 (3)0.6863 (2)0.89418 (19)0.0413 (9)
C10.9194 (4)0.5833 (3)1.1697 (2)0.0377 (10)
H10.99160.61161.16360.045*
C20.8783 (5)0.5612 (3)1.2427 (2)0.0489 (12)
H20.92310.57351.28660.059*
C30.7707 (5)0.5210 (3)1.2493 (3)0.0554 (13)
H30.74060.50681.29800.066*
C40.7081 (4)0.5017 (3)1.1836 (3)0.0504 (12)
H40.63540.47381.18880.060*
C50.8509 (4)0.5626 (3)1.1058 (2)0.0326 (9)
C60.8872 (4)0.5792 (3)1.0255 (2)0.0292 (8)
C70.9726 (3)0.6220 (2)0.9190 (2)0.0286 (8)
C81.0551 (3)0.6651 (2)0.8653 (2)0.0300 (9)
C91.0248 (4)0.6771 (3)0.7884 (2)0.0438 (10)
H90.95120.65990.77020.053*
C101.1062 (5)0.7153 (3)0.7393 (2)0.0506 (13)
H101.08830.72500.68730.061*
C111.2143 (5)0.7389 (3)0.7688 (3)0.0536 (13)
H111.27100.76500.73710.064*
C121.2368 (4)0.7232 (3)0.8453 (3)0.0515 (12)
H121.31020.73920.86460.062*
U11U22U33U12U13U23
Hg10.04114 (12)0.03899 (12)0.04791 (13)−0.00931 (7)0.00559 (8)−0.00763 (7)
Cl10.0512 (7)0.0409 (6)0.0458 (6)−0.0077 (5)0.0005 (5)−0.0119 (5)
Cl20.0474 (7)0.0458 (6)0.0524 (7)0.0020 (5)0.0129 (5)0.0116 (5)
N10.038 (2)0.0356 (19)0.0413 (19)−0.0031 (16)0.0071 (16)0.0029 (15)
N20.039 (2)0.039 (2)0.0355 (19)−0.0087 (17)0.0010 (16)−0.0032 (16)
N30.041 (2)0.040 (2)0.0321 (18)−0.0088 (17)0.0007 (16)−0.0049 (15)
N40.0283 (17)0.0246 (16)0.0271 (16)−0.0013 (13)−0.0005 (14)−0.0011 (13)
N50.042 (2)0.0365 (19)0.0283 (17)−0.0086 (16)−0.0004 (16)−0.0082 (14)
N60.042 (2)0.048 (2)0.0347 (18)−0.0137 (17)0.0009 (16)0.0035 (16)
C10.043 (3)0.037 (2)0.033 (2)0.0008 (19)0.0031 (19)0.0026 (18)
C20.063 (3)0.049 (3)0.035 (2)0.005 (3)0.004 (2)0.004 (2)
C30.073 (4)0.053 (3)0.040 (3)0.002 (3)0.021 (3)0.008 (2)
C40.051 (3)0.047 (3)0.054 (3)−0.007 (2)0.017 (2)0.009 (2)
C50.036 (2)0.024 (2)0.038 (2)0.0060 (18)0.0041 (18)0.0025 (17)
C60.030 (2)0.025 (2)0.0319 (19)0.0008 (17)0.0031 (17)−0.0020 (16)
C70.033 (2)0.0270 (19)0.0261 (18)0.0032 (17)−0.0026 (17)−0.0008 (15)
C80.037 (2)0.028 (2)0.0251 (19)0.0000 (18)0.0040 (17)−0.0004 (15)
C90.052 (3)0.047 (3)0.032 (2)−0.002 (2)−0.007 (2)−0.0006 (18)
C100.085 (4)0.041 (2)0.026 (2)0.003 (3)0.007 (2)0.0065 (18)
C110.072 (4)0.045 (3)0.044 (3)−0.011 (3)0.017 (3)0.004 (2)
C120.050 (3)0.051 (3)0.054 (3)−0.018 (2)0.005 (2)0.002 (2)
Hg1—N22.385 (3)C1—C21.383 (6)
Hg1—N12.388 (3)C1—C51.384 (6)
Hg1—Cl12.4111 (10)C1—H10.9300
Hg1—Cl22.5998 (11)C2—C31.368 (7)
Hg1—Cl2i2.7061 (11)C2—H20.9300
Cl2—Hg1i2.7061 (11)C3—C41.368 (7)
N1—C51.339 (5)C3—H30.9300
N1—C41.340 (5)C4—H40.9300
N2—C61.324 (5)C5—C61.465 (5)
N2—N31.378 (5)C7—C81.468 (5)
N3—C71.301 (5)C8—C91.380 (5)
N4—C61.355 (5)C9—C101.378 (6)
N4—C71.368 (4)C9—H90.9300
N4—N51.414 (4)C10—C111.376 (8)
N5—H5A0.8901C10—H100.9300
N5—H5B0.8900C11—C121.365 (6)
N6—C81.329 (5)C11—H110.9300
N6—C121.333 (5)C12—H120.9300
N2—Hg1—N169.78 (12)C2—C3—C4119.3 (4)
N2—Hg1—Cl1106.24 (9)C2—C3—H3120.4
N1—Hg1—Cl1136.70 (9)C4—C3—H3120.4
N2—Hg1—Cl291.45 (9)N1—C4—C3122.9 (5)
N1—Hg1—Cl2112.43 (8)N1—C4—H4118.6
Cl1—Hg1—Cl2110.74 (4)C3—C4—H4118.6
N2—Hg1—Cl2i156.52 (9)N1—C5—C1122.3 (4)
N1—Hg1—Cl2i89.27 (8)N1—C5—C6113.9 (4)
Cl1—Hg1—Cl2i96.23 (4)C1—C5—C6123.7 (4)
Cl2—Hg1—Cl2i86.78 (3)N2—C6—N4108.6 (3)
Hg1—Cl2—Hg1i93.22 (3)N2—C6—C5121.7 (4)
C5—N1—C4117.9 (4)N4—C6—C5129.6 (4)
C5—N1—Hg1118.1 (3)N3—C7—N4110.3 (3)
C4—N1—Hg1122.7 (3)N3—C7—C8124.9 (3)
C6—N2—N3108.4 (3)N4—C7—C8124.8 (3)
C6—N2—Hg1114.3 (3)N6—C8—C9123.5 (4)
N3—N2—Hg1135.5 (3)N6—C8—C7116.2 (3)
C7—N3—N2106.9 (3)C9—C8—C7120.2 (4)
C6—N4—C7105.9 (3)C10—C9—C8118.4 (4)
C6—N4—N5123.9 (3)C10—C9—H9120.8
C7—N4—N5129.4 (3)C8—C9—H9120.8
N4—N5—H5A103.4C11—C10—C9118.7 (4)
N4—N5—H5B107.9C11—C10—H10120.6
H5A—N5—H5B112.5C9—C10—H10120.6
C8—N6—C12116.7 (4)C12—C11—C10118.6 (4)
C2—C1—C5118.7 (4)C12—C11—H11120.7
C2—C1—H1120.6C10—C11—H11120.7
C5—C1—H1120.6N6—C12—C11124.1 (5)
C3—C2—C1118.9 (4)N6—C12—H12118.0
C3—C2—H2120.6C11—C12—H12118.0
C1—C2—H2120.6
N2—Hg1—Cl2—Hg1i−156.57 (9)C2—C1—C5—C6−177.3 (4)
N1—Hg1—Cl2—Hg1i−87.88 (9)N3—N2—C6—N4−0.5 (4)
Cl1—Hg1—Cl2—Hg1i95.44 (4)Hg1—N2—C6—N4−167.7 (2)
Cl2i—Hg1—Cl2—Hg1i0.0N3—N2—C6—C5−177.9 (4)
N2—Hg1—N1—C5−3.4 (3)Hg1—N2—C6—C514.9 (5)
Cl1—Hg1—N1—C589.1 (3)C7—N4—C6—N20.9 (4)
Cl2—Hg1—N1—C5−86.3 (3)N5—N4—C6—N2171.6 (3)
Cl2i—Hg1—N1—C5−172.6 (3)C7—N4—C6—C5178.0 (4)
N2—Hg1—N1—C4−169.9 (4)N5—N4—C6—C5−11.2 (6)
Cl1—Hg1—N1—C4−77.4 (4)N1—C5—C6—N2−17.9 (5)
Cl2—Hg1—N1—C4107.1 (3)C1—C5—C6—N2159.1 (4)
Cl2i—Hg1—N1—C420.9 (3)N1—C5—C6—N4165.3 (4)
N1—Hg1—N2—C6−5.9 (3)C1—C5—C6—N4−17.8 (7)
Cl1—Hg1—N2—C6−140.4 (3)N2—N3—C7—N40.6 (4)
Cl2—Hg1—N2—C6107.5 (3)N2—N3—C7—C8176.7 (3)
Cl2i—Hg1—N2—C622.2 (4)C6—N4—C7—N3−0.9 (4)
N1—Hg1—N2—N3−168.5 (4)N5—N4—C7—N3−171.0 (4)
Cl1—Hg1—N2—N357.0 (4)C6—N4—C7—C8−177.0 (3)
Cl2—Hg1—N2—N3−55.1 (4)N5—N4—C7—C812.9 (6)
Cl2i—Hg1—N2—N3−140.3 (3)C12—N6—C8—C91.8 (6)
C6—N2—N3—C7−0.1 (4)C12—N6—C8—C7178.2 (4)
Hg1—N2—N3—C7163.2 (3)N3—C7—C8—N6−148.0 (4)
C5—C1—C2—C3−1.0 (6)N4—C7—C8—N627.6 (5)
C1—C2—C3—C41.6 (7)N3—C7—C8—C928.6 (6)
C5—N1—C4—C3−0.9 (7)N4—C7—C8—C9−155.9 (4)
Hg1—N1—C4—C3165.7 (4)N6—C8—C9—C10−1.8 (6)
C2—C3—C4—N1−0.6 (7)C7—C8—C9—C10−178.1 (4)
C4—N1—C5—C11.5 (6)C8—C9—C10—C110.7 (7)
Hg1—N1—C5—C1−165.7 (3)C9—C10—C11—C120.2 (7)
C4—N1—C5—C6178.5 (4)C8—N6—C12—C11−0.8 (7)
Hg1—N1—C5—C611.3 (4)C10—C11—C12—N6−0.2 (7)
C2—C1—C5—N1−0.5 (6)
D—H···AD—HH···AD···AD—H···A
N5—H5A···Cl2ii0.892.803.446 (3)131
N5—H5A···Cl1iii0.892.773.512 (4)142
N5—H5B···Cl1iv0.892.623.452 (4)155
N5—H5B···N60.892.472.956 (5)115
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
N5—H5A⋯Cl2i0.892.803.446 (3)131
N5—H5A⋯Cl1ii0.892.773.512 (4)142
N5—H5B⋯Cl1iii0.892.623.452 (4)155
N5—H5B⋯N60.892.472.956 (5)115

Symmetry codes: (i) ; (ii) ; (iii) .

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