Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801004822/wn6008sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801004822/wn6008Isup2.hkl |
CCDC reference: 162805
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.031
- wR factor = 0.077
- Data-to-parameter ratio = 9.4
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
ABSTM_02 Alert C The ratio of Tmax/Tmin expected RT(exp) is > 1.10 Absorption corrections should be applied. Tmin and Tmax expected: 0.417 0.469 RT(exp) = 1.125 General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.00 From the CIF: _reflns_number_total 1038 Count of symmetry unique reflns 972 Completeness (_total/calc) 106.79% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 66 Fraction of Friedel pairs measured 0.068 Are heavy atom types Z>Si present yes WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
A procedure similar to that employed in the synthesis of (dabcoH2)2Cl3[CuCl3(H2O)2]·H2O (Wei & Willett, 1996) was followed. Equimolar mixtures of the dabco ligand and ZnCl2 were dissolved in a dilute HCl solution. Colorless crystals separated out of the solution after several days of slow evaporation at room temperature. These were filtered off and air-dried.
Data collection: XSCANS (Siemens, 1992); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS90 (Sheldrick, 1990); program(s) used to refine structure: SHELXL92 (Sheldrick, 1992); molecular graphics: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.
[ZnCl3(C6H13N2)] | F(000) = 288 |
Mr = 284.94 | Dx = 1.789 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.7475 (10) Å | Cell parameters from 25 reflections |
b = 12.5446 (16) Å | θ = 13.5–14° |
c = 6.9788 (17) Å | µ = 3.03 mm−1 |
β = 116.430 (14)° | T = 293 K |
V = 528.98 (17) Å3 | Rhomboids, colorless |
Z = 2 | 0.3 × 0.3 × 0.25 mm |
Bruker P4 diffractometer | Rint = 0.030 |
Radiation source: fine-focus sealed tube | θmax = 25.0°, θmin = 3.3° |
Graphite monochromator | h = −1→7 |
ω scans | k = −1→14 |
1317 measured reflections | l = −8→7 |
1038 independent reflections | 3 standard reflections every 97 reflections |
1005 reflections with I > 2σ(I) | intensity decay: <1% |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.031 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.077 | w = 1/[σ2(Fo2) + (0.0523P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max < 0.001 |
1038 reflections | Δρmax = 0.80 e Å−3 |
110 parameters | Δρmin = −0.56 e Å−3 |
1 restraint | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.00 (2) |
[ZnCl3(C6H13N2)] | V = 528.98 (17) Å3 |
Mr = 284.94 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 6.7475 (10) Å | µ = 3.03 mm−1 |
b = 12.5446 (16) Å | T = 293 K |
c = 6.9788 (17) Å | 0.3 × 0.3 × 0.25 mm |
β = 116.430 (14)° |
Bruker P4 diffractometer | Rint = 0.030 |
1317 measured reflections | 3 standard reflections every 97 reflections |
1038 independent reflections | intensity decay: <1% |
1005 reflections with I > 2σ(I) |
R[F2 > 2σ(F2)] = 0.031 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.077 | Δρmax = 0.80 e Å−3 |
S = 1.08 | Δρmin = −0.56 e Å−3 |
1038 reflections | Absolute structure: Flack (1983) |
110 parameters | Absolute structure parameter: 0.00 (2) |
1 restraint |
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 | ||
Zn | −0.43560 (8) | −0.88492 (5) | −0.29074 (8) | 0.0255 (2) | |
Cl1 | −0.7743 (2) | −0.83248 (13) | −0.5277 (2) | 0.0355 (3) | |
Cl2 | −0.2905 (2) | −1.01529 (12) | −0.4079 (2) | 0.0353 (3) | |
Cl3 | −0.4150 (3) | −0.92037 (13) | 0.0336 (2) | 0.0430 (4) | |
C8 | −0.1499 (9) | −0.5639 (5) | −0.1314 (10) | 0.0340 (13) | |
H8A | −0.2459 | −0.5072 | −0.2178 | 0.041* | |
H8B | −0.0740 | −0.5396 | 0.0156 | 0.041* | |
C7 | −0.2853 (10) | −0.6642 (5) | −0.1460 (9) | 0.0303 (12) | |
H7A | −0.2591 | −0.6855 | −0.0031 | 0.036* | |
H7B | −0.4415 | −0.6479 | −0.2264 | 0.036* | |
C2 | 0.0077 (8) | −0.7823 (5) | −0.1193 (8) | 0.0309 (12) | |
H2A | 0.0496 | −0.8376 | −0.1914 | 0.037* | |
H2B | 0.0278 | −0.8101 | 0.0179 | 0.037* | |
C5 | −0.2563 (9) | −0.7170 (5) | −0.4636 (8) | 0.0295 (12) | |
H5A | −0.4088 | −0.6955 | −0.5492 | 0.035* | |
H5B | −0.2249 | −0.7756 | −0.5364 | 0.035* | |
C6 | −0.1057 (10) | −0.6247 (5) | −0.4461 (10) | 0.0382 (14) | |
H6A | −0.0007 | −0.6453 | −0.4993 | 0.046* | |
H6B | −0.1917 | −0.5649 | −0.5304 | 0.046* | |
N1 | −0.2286 (7) | −0.7538 (4) | −0.2503 (6) | 0.0227 (9) | |
C3 | 0.1564 (10) | −0.6847 (5) | −0.0838 (12) | 0.0458 (17) | |
H3A | 0.2277 | −0.6660 | 0.0668 | 0.055* | |
H3B | 0.2704 | −0.7004 | −0.1284 | 0.055* | |
N4 | 0.0151 (8) | −0.5936 (4) | −0.2132 (9) | 0.0399 (12) | |
H4A | 0.1032 | −0.5365 | −0.2000 | 0.048* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn | 0.0272 (3) | 0.0177 (3) | 0.0334 (3) | −0.0013 (3) | 0.0152 (2) | 0.0005 (3) |
Cl1 | 0.0289 (6) | 0.0310 (7) | 0.0419 (6) | 0.0043 (6) | 0.0115 (5) | −0.0035 (6) |
Cl2 | 0.0381 (7) | 0.0252 (7) | 0.0433 (7) | 0.0040 (6) | 0.0186 (6) | −0.0059 (6) |
Cl3 | 0.0510 (8) | 0.0456 (9) | 0.0426 (6) | 0.0143 (7) | 0.0301 (6) | 0.0166 (6) |
C8 | 0.033 (3) | 0.020 (3) | 0.052 (3) | 0.001 (2) | 0.022 (2) | −0.006 (3) |
C7 | 0.037 (3) | 0.023 (3) | 0.040 (3) | 0.000 (3) | 0.026 (2) | −0.006 (2) |
C2 | 0.023 (2) | 0.027 (3) | 0.035 (3) | 0.000 (2) | 0.005 (2) | 0.003 (2) |
C5 | 0.033 (3) | 0.031 (3) | 0.024 (2) | 0.000 (3) | 0.012 (2) | 0.004 (2) |
C6 | 0.052 (4) | 0.025 (3) | 0.052 (3) | −0.007 (3) | 0.037 (3) | 0.000 (3) |
N1 | 0.024 (2) | 0.018 (2) | 0.028 (2) | 0.0003 (19) | 0.0136 (16) | −0.0012 (18) |
C3 | 0.023 (3) | 0.033 (4) | 0.072 (4) | −0.003 (3) | 0.013 (3) | −0.016 (3) |
N4 | 0.033 (3) | 0.020 (2) | 0.072 (4) | −0.008 (2) | 0.027 (2) | −0.007 (2) |
Zn—N1 | 2.094 (4) | C2—N1 | 1.486 (6) |
Zn—Cl2 | 2.2394 (15) | C2—C3 | 1.532 (9) |
Zn—Cl1 | 2.2418 (14) | C5—N1 | 1.489 (6) |
Zn—Cl3 | 2.2495 (15) | C5—C6 | 1.509 (8) |
C8—N4 | 1.506 (7) | C6—N4 | 1.510 (8) |
C8—C7 | 1.531 (8) | C3—N4 | 1.505 (9) |
C7—N1 | 1.479 (7) | ||
N1—Zn—Cl2 | 104.43 (12) | C7—N1—C2 | 108.8 (4) |
N1—Zn—Cl1 | 105.59 (13) | C7—N1—C5 | 108.1 (4) |
Cl2—Zn—Cl1 | 114.38 (6) | C2—N1—C5 | 108.2 (4) |
N1—Zn—Cl3 | 106.31 (12) | C7—N1—Zn | 111.1 (3) |
Cl2—Zn—Cl3 | 112.44 (6) | C2—N1—Zn | 111.2 (3) |
Cl1—Zn—Cl3 | 112.73 (6) | C5—N1—Zn | 109.2 (3) |
N4—C8—C7 | 106.9 (5) | N4—C3—C2 | 108.4 (5) |
N1—C7—C8 | 112.3 (4) | C3—N4—C8 | 109.8 (5) |
N1—C2—C3 | 110.7 (5) | C3—N4—C6 | 110.2 (5) |
N1—C5—C6 | 112.1 (4) | C8—N4—C6 | 109.6 (5) |
N4—C6—C5 | 107.8 (5) | ||
N4—C8—C7—N1 | −5.0 (7) | Cl2—Zn—N1—C2 | −51.2 (3) |
N1—C5—C6—N4 | −4.2 (6) | Cl1—Zn—N1—C2 | −172.2 (3) |
C8—C7—N1—C2 | 62.1 (6) | Cl3—Zn—N1—C2 | 67.9 (3) |
C8—C7—N1—C5 | −55.3 (6) | Cl2—Zn—N1—C5 | 68.2 (3) |
C8—C7—N1—Zn | −175.1 (4) | Cl1—Zn—N1—C5 | −52.8 (3) |
C3—C2—N1—C7 | −55.1 (6) | Cl3—Zn—N1—C5 | −172.7 (3) |
C3—C2—N1—C5 | 62.2 (6) | N1—C2—C3—N4 | −5.7 (7) |
C3—C2—N1—Zn | −177.8 (4) | C2—C3—N4—C8 | 64.2 (6) |
C6—C5—N1—C7 | 60.9 (5) | C2—C3—N4—C6 | −56.6 (7) |
C6—C5—N1—C2 | −56.8 (6) | C7—C8—N4—C3 | −57.6 (6) |
C6—C5—N1—Zn | −178.0 (4) | C7—C8—N4—C6 | 63.5 (6) |
Cl2—Zn—N1—C7 | −172.6 (3) | C5—C6—N4—C3 | 62.3 (6) |
Cl1—Zn—N1—C7 | 66.5 (3) | C5—C6—N4—C8 | −58.6 (6) |
Cl3—Zn—N1—C7 | −53.5 (3) |
Experimental details
Crystal data | |
Chemical formula | [ZnCl3(C6H13N2)] |
Mr | 284.94 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 293 |
a, b, c (Å) | 6.7475 (10), 12.5446 (16), 6.9788 (17) |
β (°) | 116.430 (14) |
V (Å3) | 528.98 (17) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 3.03 |
Crystal size (mm) | 0.3 × 0.3 × 0.25 |
Data collection | |
Diffractometer | Bruker P4 diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1317, 1038, 1005 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.077, 1.08 |
No. of reflections | 1038 |
No. of parameters | 110 |
No. of restraints | 1 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.80, −0.56 |
Absolute structure | Flack (1983) |
Absolute structure parameter | 0.00 (2) |
Computer programs: XSCANS (Siemens, 1992), XSCANS, SHELXS90 (Sheldrick, 1990), SHELXL92 (Sheldrick, 1992), SHELXL97 (Sheldrick, 1997), SHELXL97.
The title compound, (I), was prepared in an attempt to make non-Jahn–Teller analogs to (dabcoH2)2Cl3[CuCl3(H2O)2]·H2O (Wei & Willett, 1996) and to (dabcoH2)CuCl4 and (dabco2)CuCl4·H2O (Wei & Willett, 2001).