Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680201214X/ob6148sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680201214X/ob6148Isup2.hkl | |
Text file https://doi.org/10.1107/S160053680201214X/ob6148sup3.txt | |
Text file https://doi.org/10.1107/S160053680201214X/ob6148295Ksup4.txt |
CCDC reference: 193708
Data collection: SMART (Siemens, 1996); cell refinement: MACH3 in CAD-4 UNIX Software (Enraf-Nonius, 1998); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: JANA2000 (Petricek & Dusek, 2000); molecular graphics: DIAMOND (Brandenburg, 1999) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: JANA2000.
(C3H10N)2[HgCl4] | F(000) = 872 |
Mr = 462.63 | Dx = 1.991 Mg m−3 |
Monoclinic, P1121/n | Synchrotron radiation, λ = 0.50000 Å |
a = 18.741 (2) Å | Cell parameters from 25 reflections |
b = 6.302 (2) Å | θ = 27.3–8.8° |
c = 13.069 (3) Å | µ = 5.79 mm−1 |
β = 90° | T = 343 K |
V = 1542.8 (6) Å3 | Polyhedron, colorless |
Z = 4 | 0.16 × 0.14 × 0.12 mm |
Huber four-circle Kappa diffractometer with Siemens SMART CCD area detector | 2174 independent reflections |
Si (111) monochromator | 1191 reflections with I > 2σ(I) |
Detector resolution: number of pixels: 1024 x 1024 (512 x 512 in binning mode), pixel size: 60 µm x 60 µm pixels mm-1 | Rint = 0.044 |
Rotation image scans | θmax = 16.3°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −19→20 |
Tmin = 0.474, Tmax = 0.695 | k = −7→7 |
6993 measured reflections | l = −14→14 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F > 3σ(F)] = 0.051 | H-atom parameters constrained |
wR(F) = 0.079 | w = 1/[σ2(Fo2) + (0.0876P)2 + 1.1621P] where P = (Fo2 + 2Fc2)/3 |
S = 2.30 | (Δ/σ)max < 0.001 |
1191 reflections | Δρmax = 1.90 e Å−3 |
77 parameters | Δρmin = −0.96 e Å−3 |
0 restraints | Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.24 (5) |
Experimental. During the crystal test on the F1 beamline (HASYLAB) we noticed that there is no single spot in the area corresponding to a theta higher than 20 degree, for different setting of diffractometer angles. The scans were made at theta equal 20 degree. This behavior is characteristic of this family of compounds. |
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. 700–900 data frames were collected by 0.01° steps in ω-scans with a crystal-to-detector distance of 30 mm. Preliminary orientation matrices were obtained from the first 100 frames using SMART (Siemens, 1995). The collected frames were integrated using the respective preliminary orientation matrix, which was updated every 100 frames. The data were empirically corrected for absorption and other effects (absorption by air, glue material and glass capillary) using SADABS (Sheldrick, 1996). The cell constants were obtained from setting angles of 25 reflections with 8.89 < θ <27.70°(graphite-monochromator Mo—Kα radiation). The systematic extinctions were in accordance with the space group P21/n for the room temperature and 343 K data. Structure refinement were performed by full-matrix least squares on F2 data using SHELXL97(Sheldrick, 1997). The non H-atoms were refined anisotropically, whereas H atoms were treated isotropically using appropriate rinding models. 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 | ||
Hg | 0.34318 (2) | 0.27039 (8) | 0.24946 (14) | 0.0722 (3) | |
CL1 | 0.3436 (2) | 0.6832 (6) | 0.2588 (7) | 0.0709 (14) | |
CL2 | 0.4084 (5) | 0.1961 (13) | 0.0923 (7) | 0.111 (3) | |
CL3 | 0.4135 (4) | 0.1849 (10) | 0.3993 (6) | 0.087 (2) | |
CL4 | 0.2175 (2) | 0.1760 (8) | 0.2535 (11) | 0.105 (2) | |
N1a | 0.4869 (6) | 0.1856 (18) | 0.7570 (17) | 0.086 (4) | |
H1a | 0.5362 (6) | 0.1457 (18) | 0.7609 (17) | 0.0513* | |
C1a | 0.4778 (11) | 0.280 (2) | 0.652 (2) | 0.123 (8) | |
C1/1a | 0.4770 (11) | 0.343 (3) | 0.8415 (19) | 0.123 (8) | |
C1/2a | 0.4435 (11) | −0.016 (3) | 0.7721 (19) | 0.123 (8) | |
N2a | 0.7727 (9) | 0.272 (2) | 0.0289 (15) | 0.100 (5) | |
H2a | 0.7924 (9) | 0.307 (2) | 0.0977 (15) | 0.038* | |
C4a | 0.7387 (12) | 0.458 (4) | 0.001 (3) | 0.228 (16) | |
C4/1a | 0.7269 (13) | 0.098 (3) | 0.048 (3) | 0.228 (16) | |
C4/2a | 0.8333 (13) | 0.228 (3) | −0.028 (3) | 0.228 (15) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg | 0.0576 (5) | 0.0872 (5) | 0.0721 (5) | 0.0009 (8) | 0.0033 (8) | 0.0074 (3) |
CL1 | 0.072 (2) | 0.0708 (19) | 0.070 (3) | −0.008 (3) | 0.012 (3) | 0.0033 (14) |
CL2 | 0.113 (6) | 0.133 (6) | 0.087 (5) | −0.017 (5) | 0.020 (5) | 0.035 (5) |
CL3 | 0.092 (5) | 0.098 (4) | 0.070 (4) | 0.003 (3) | −0.025 (4) | −0.001 (3) |
CL4 | 0.053 (2) | 0.117 (3) | 0.145 (5) | 0.035 (6) | 0.007 (6) | 0.000 (2) |
N1a | 0.037 (5) | 0.1080 (18) | 0.113 (10) | 0.001 (4) | −0.0042 (17) | 0.0243 (15) |
C1a | 0.108 (10) | 0.140 (18) | 0.122 (12) | 0.020 (11) | 0.005 (7) | 0.034 (10) |
C1/1a | 0.092 (10) | 0.147 (14) | 0.130 (18) | −0.026 (11) | 0.006 (9) | 0.011 (8) |
C1/2a | 0.092 (10) | 0.116 (13) | 0.160 (18) | 0.008 (11) | −0.018 (9) | 0.000 (8) |
N2a | 0.105 (3) | 0.107 (12) | 0.088 (10) | −0.005 (3) | −0.008 (4) | 0.001 (5) |
C4a | 0.11 (2) | 0.43 (4) | 0.152 (19) | −0.15 (2) | 0.022 (15) | 0.02 (2) |
C4/1a | 0.11 (2) | 0.43 (4) | 0.152 (19) | −0.15 (2) | 0.022 (15) | 0.02 (2) |
C4/2a | 0.11 (2) | 0.43 (4) | 0.152 (19) | −0.15 (2) | 0.022 (15) | 0.02 (2) |
Hg—CL1 | 2.604 (4) | Cl1—H2aii | 2.26 (2) |
Hg—CL2 | 2.442 (10) | N1a—H1a | 0.967 (16) |
Hg—CL3 | 2.430 (7) | N1a—C1a | 1.50 (3) |
Hg—CL4 | 2.414 (4) | N2a—H2a | 0.99 (3) |
Cl1—H1ai | 2.482 (12) | N2a—C4a | 1.40 (3) |
CL1—Hg—CL2 | 104.1 (3) | C1a—N1a—C1/2a | 112.9 (16) |
CL1—Hg—CL3 | 101.4 (2) | C1/1a—N1a—C1/2a | 112.9 (17) |
CL1—Hg—CL4 | 102.68 (15) | H2a—N2a—C4a | 103 (2) |
CL2—Hg—CL3 | 110.9 (3) | H2a—N2a—C4/1a | 103 (2) |
CL2—Hg—CL4 | 117.5 (4) | H2a—N2a—C4/2a | 103 (2) |
CL3—Hg—CL4 | 117.3 (4) | C4a—N2a—C4/1a | 114.9 (18) |
H1a—N1a—C1a | 106 (2) | C4a—N2a—C4/2a | 115 (2) |
H1a—N1a—C1/1a | 106 (2) | C4/1a—N2a—C4/2a | 114.9 (18) |
H1a—N1a—C1/2a | 105.7 (14) | CL1iii—H2a—N2a | 146.7 (15) |
C1a—N1a—C1/1a | 112.9 (13) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1/2, y+1/2, −z+1/2; (iii) x+1/2, y−1/2, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1a—H1a···CL1i | 0.97 | 2.48 | 3.272 (12) | 138 |
N1a—H1a···CL2iv | 0.97 | 3.09 | 3.699 (18) | 124 |
N1a—H1a···CL3iv | 0.97 | 3.12 | 3.656 (17) | 117 |
N2a—H2a···CL1iii | 1.00 | 2.26 | 3.13 (2) | 147 |
N2a—H2a···CL4v | 1.00 | 3.37 | 3.97 (2) | 121 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (iii) x+1/2, y−1/2, −z+1/2; (iv) −x+1, −y, −z+1; (v) x+1/2, y+1/2, −z+1/2. |