Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801018414/ob6086sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801018414/ob6086Isup2.hkl |
CCDC reference: 177175
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.045
- wR factor = 0.147
- Data-to-parameter ratio = 14.0
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.453 0.718 Tmin' and Tmax expected: 0.549 0.718 RR' = 0.826 Please check that your absorption correction is appropriate.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994a); data reduction: SHELXTL XPREP (Siemens, 1994b); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
(C9H8N)[ZnCl3(C9H7N)] | Z = 2 |
Mr = 431.04 | F(000) = 436 |
Triclinic, P1 | Dx = 1.618 Mg m−3 |
a = 8.2360 (7) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.5392 (7) Å | Cell parameters from 2580 reflections |
c = 11.9512 (10) Å | θ = 1.7–25.0° |
α = 98.499 (1)° | µ = 1.84 mm−1 |
β = 94.670 (1)° | T = 293 K |
γ = 106.104 (1)° | Prism, colorless |
V = 884.76 (12) Å3 | 0.32 × 0.20 × 0.18 mm |
Siemens SMART CCD diffractometer | 3047 independent reflections |
Radiation source: fine-focus sealed tube | 2232 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
ω scan | θmax = 25.0°, θmin = 1.7° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −9→8 |
Tmin = 0.453, Tmax = 0.718 | k = −11→9 |
4503 measured reflections | l = −14→13 |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.147 | H-atom parameters constrained |
S = 0.91 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
3047 reflections | (Δ/σ)max < 0.001 |
217 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.45 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. |
x | y | z | Uiso*/Ueq | ||
Zn | 0.25938 (7) | 0.65346 (6) | 0.22987 (5) | 0.0415 (2) | |
Cl1 | 0.3906 (2) | 0.67933 (19) | 0.07290 (13) | 0.0729 (5) | |
Cl2 | −0.02428 (15) | 0.57513 (13) | 0.16743 (11) | 0.0496 (3) | |
Cl3 | 0.32993 (18) | 0.85753 (14) | 0.36355 (12) | 0.0559 (4) | |
C1 | 0.5142 (6) | 0.5023 (5) | 0.2803 (4) | 0.0459 (12) | |
H1A | 0.5695 | 0.5673 | 0.2352 | 0.055* | |
C2 | 0.6009 (6) | 0.4121 (6) | 0.3252 (5) | 0.0507 (13) | |
H2A | 0.7115 | 0.4178 | 0.3103 | 0.061* | |
C3 | 0.5225 (6) | 0.3167 (6) | 0.3903 (4) | 0.0479 (13) | |
H3A | 0.5788 | 0.2557 | 0.4201 | 0.057* | |
C4 | 0.3562 (6) | 0.3091 (5) | 0.4134 (4) | 0.0387 (11) | |
C5 | 0.2670 (7) | 0.2127 (5) | 0.4802 (4) | 0.0502 (13) | |
H5A | 0.3187 | 0.1494 | 0.5111 | 0.060* | |
C6 | 0.1068 (7) | 0.2099 (6) | 0.5008 (5) | 0.0528 (13) | |
H6A | 0.0489 | 0.1445 | 0.5447 | 0.063* | |
C7 | 0.0286 (7) | 0.3062 (6) | 0.4555 (5) | 0.0503 (13) | |
H7A | −0.0805 | 0.3052 | 0.4710 | 0.060* | |
C8 | 0.1098 (6) | 0.4012 (5) | 0.3892 (4) | 0.0405 (11) | |
H8A | 0.0560 | 0.4638 | 0.3592 | 0.049* | |
C9 | 0.2747 (6) | 0.4041 (4) | 0.3664 (4) | 0.0333 (10) | |
C10 | 0.2021 (8) | 0.2643 (6) | 0.0404 (5) | 0.0550 (14) | |
H10A | 0.2596 | 0.3323 | −0.0019 | 0.066* | |
C11 | 0.2795 (7) | 0.1675 (6) | 0.0810 (5) | 0.0511 (13) | |
H11A | 0.3892 | 0.1699 | 0.0660 | 0.061* | |
C12 | 0.1949 (6) | 0.0681 (6) | 0.1432 (4) | 0.0469 (12) | |
H12A | 0.2476 | 0.0034 | 0.1710 | 0.056* | |
C13 | 0.0292 (6) | 0.0632 (5) | 0.1653 (4) | 0.0352 (10) | |
C14 | −0.0675 (7) | −0.0399 (6) | 0.2252 (5) | 0.0494 (13) | |
H14A | −0.0205 | −0.1079 | 0.2531 | 0.059* | |
C15 | −0.2280 (7) | −0.0411 (6) | 0.2427 (5) | 0.0563 (14) | |
H15A | −0.2904 | −0.1100 | 0.2823 | 0.068* | |
C16 | −0.3009 (7) | 0.0604 (6) | 0.2016 (5) | 0.0581 (15) | |
H16A | −0.4116 | 0.0580 | 0.2139 | 0.070* | |
C17 | −0.2124 (7) | 0.1623 (6) | 0.1438 (5) | 0.0544 (14) | |
H17A | −0.2609 | 0.2310 | 0.1184 | 0.065* | |
C18 | −0.0479 (6) | 0.1633 (5) | 0.1230 (4) | 0.0398 (11) | |
N1 | 0.3564 (5) | 0.4998 (4) | 0.2990 (3) | 0.0377 (9) | |
N2 | 0.0460 (6) | 0.2603 (4) | 0.0618 (4) | 0.0511 (11) | |
H2B | 0.0007 | 0.3220 | 0.0359 | 0.061* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn | 0.0446 (4) | 0.0387 (3) | 0.0423 (4) | 0.0123 (2) | 0.0004 (2) | 0.0129 (2) |
Cl1 | 0.0697 (10) | 0.0945 (12) | 0.0535 (9) | 0.0098 (9) | 0.0149 (7) | 0.0345 (8) |
Cl2 | 0.0442 (7) | 0.0472 (7) | 0.0587 (8) | 0.0159 (6) | −0.0060 (6) | 0.0154 (6) |
Cl3 | 0.0637 (9) | 0.0435 (7) | 0.0579 (9) | 0.0197 (6) | −0.0074 (6) | 0.0020 (6) |
C1 | 0.041 (3) | 0.046 (3) | 0.050 (3) | 0.012 (2) | 0.005 (2) | 0.006 (2) |
C2 | 0.033 (3) | 0.064 (3) | 0.060 (4) | 0.024 (2) | 0.005 (2) | 0.008 (3) |
C3 | 0.050 (3) | 0.057 (3) | 0.043 (3) | 0.031 (3) | −0.006 (2) | 0.004 (2) |
C4 | 0.051 (3) | 0.036 (2) | 0.032 (3) | 0.022 (2) | −0.001 (2) | 0.003 (2) |
C5 | 0.073 (4) | 0.044 (3) | 0.039 (3) | 0.025 (3) | 0.002 (3) | 0.015 (2) |
C6 | 0.065 (4) | 0.049 (3) | 0.046 (3) | 0.014 (3) | 0.009 (3) | 0.020 (2) |
C7 | 0.044 (3) | 0.057 (3) | 0.049 (3) | 0.012 (3) | 0.008 (2) | 0.012 (3) |
C8 | 0.040 (3) | 0.047 (3) | 0.041 (3) | 0.021 (2) | 0.004 (2) | 0.014 (2) |
C9 | 0.038 (2) | 0.030 (2) | 0.030 (2) | 0.0109 (19) | −0.0020 (19) | 0.0010 (18) |
C10 | 0.065 (4) | 0.046 (3) | 0.044 (3) | −0.002 (3) | 0.003 (3) | 0.015 (2) |
C11 | 0.040 (3) | 0.057 (3) | 0.052 (3) | 0.009 (2) | 0.005 (2) | 0.005 (3) |
C12 | 0.046 (3) | 0.053 (3) | 0.045 (3) | 0.019 (2) | 0.002 (2) | 0.009 (2) |
C13 | 0.039 (3) | 0.035 (2) | 0.030 (2) | 0.011 (2) | −0.0024 (19) | 0.0056 (19) |
C14 | 0.053 (3) | 0.047 (3) | 0.051 (3) | 0.018 (2) | 0.006 (2) | 0.012 (2) |
C15 | 0.054 (3) | 0.058 (3) | 0.052 (3) | 0.003 (3) | 0.010 (3) | 0.015 (3) |
C16 | 0.041 (3) | 0.065 (4) | 0.066 (4) | 0.018 (3) | 0.000 (3) | 0.004 (3) |
C17 | 0.051 (3) | 0.055 (3) | 0.063 (4) | 0.030 (3) | −0.007 (3) | 0.006 (3) |
C18 | 0.049 (3) | 0.031 (2) | 0.037 (3) | 0.013 (2) | −0.002 (2) | 0.003 (2) |
N1 | 0.036 (2) | 0.036 (2) | 0.041 (2) | 0.0104 (17) | 0.0051 (17) | 0.0072 (17) |
N2 | 0.067 (3) | 0.040 (2) | 0.049 (3) | 0.019 (2) | −0.001 (2) | 0.012 (2) |
Zn—N1 | 2.090 (4) | C14—C15 | 1.352 (7) |
Zn—Cl3 | 2.2319 (14) | C15—C16 | 1.398 (8) |
Zn—Cl1 | 2.2512 (15) | C16—C17 | 1.357 (8) |
Zn—Cl2 | 2.2707 (13) | C17—C18 | 1.394 (7) |
C1—N1 | 1.330 (6) | C18—N2 | 1.372 (6) |
C1—C2 | 1.398 (7) | C1—H1A | 0.9300 |
C2—C3 | 1.347 (7) | C2—H2A | 0.9300 |
C3—C4 | 1.403 (7) | C3—H3A | 0.9300 |
C4—C5 | 1.401 (7) | C5—H5A | 0.9300 |
C4—C9 | 1.420 (6) | C6—H6A | 0.9300 |
C5—C6 | 1.356 (7) | C7—H7A | 0.9300 |
C6—C7 | 1.404 (7) | C8—H8A | 0.9300 |
C7—C8 | 1.364 (7) | C10—H10A | 0.9300 |
C8—C9 | 1.400 (6) | C11—H11A | 0.9300 |
C9—N1 | 1.379 (5) | C12—H12A | 0.9300 |
C10—N2 | 1.322 (7) | C14—H14A | 0.9300 |
C10—C11 | 1.380 (7) | C15—H15A | 0.9300 |
C11—C12 | 1.364 (7) | C16—H16A | 0.9300 |
C12—C13 | 1.401 (6) | C17—H17A | 0.9300 |
C13—C14 | 1.407 (7) | N2—H2B | 0.8600 |
C13—C18 | 1.414 (6) | ||
N1—Zn—Cl3 | 106.18 (11) | C1—N1—Zn | 116.0 (3) |
N1—Zn—Cl1 | 102.89 (11) | C9—N1—Zn | 125.5 (3) |
Cl3—Zn—Cl1 | 114.49 (6) | C10—N2—C18 | 123.9 (4) |
N1—Zn—Cl2 | 115.41 (11) | N1—C1—H1A | 118.4 |
Cl3—Zn—Cl2 | 111.92 (5) | C2—C1—H1A | 118.3 |
Cl1—Zn—Cl2 | 105.86 (6) | C3—C2—H2A | 120.4 |
N1—C1—C2 | 123.3 (5) | C1—C2—H2A | 120.4 |
C3—C2—C1 | 119.2 (5) | C2—C3—H3A | 119.9 |
C2—C3—C4 | 120.3 (4) | C4—C3—H3A | 119.8 |
C5—C4—C3 | 123.4 (4) | C6—C5—H5A | 119.4 |
C5—C4—C9 | 118.5 (4) | C4—C5—H5A | 119.4 |
C3—C4—C9 | 118.1 (4) | C5—C6—H6A | 120.2 |
C6—C5—C4 | 121.3 (5) | C7—C6—H6A | 120.2 |
C5—C6—C7 | 119.7 (5) | C8—C7—H7A | 119.4 |
C8—C7—C6 | 121.2 (5) | C6—C7—H7A | 119.4 |
C7—C8—C9 | 119.7 (4) | C7—C8—H8A | 120.2 |
N1—C9—C8 | 119.6 (4) | C9—C8—H8A | 120.2 |
N1—C9—C4 | 120.7 (4) | N2—C10—H10A | 120.1 |
C8—C9—C4 | 119.7 (4) | C11—C10—H10A | 120.1 |
N2—C10—C11 | 119.8 (5) | C12—C11—H11A | 120.0 |
C12—C11—C10 | 120.0 (5) | C10—C11—H11A | 120.0 |
C11—C12—C13 | 120.2 (5) | C11—C12—H12A | 119.9 |
C12—C13—C14 | 123.2 (4) | C13—C12—H12A | 119.9 |
C12—C13—C18 | 119.0 (4) | C15—C14—H14A | 119.6 |
C14—C13—C18 | 117.8 (4) | C13—C14—H14A | 119.6 |
C15—C14—C13 | 120.8 (5) | C14—C15—H15A | 119.7 |
C14—C15—C16 | 120.5 (5) | C16—C15—H15A | 119.8 |
C17—C16—C15 | 120.9 (5) | C17—C16—H16A | 119.6 |
C16—C17—C18 | 119.4 (5) | C15—C16—H16A | 119.5 |
N2—C18—C17 | 122.2 (4) | C16—C17—H17A | 120.3 |
N2—C18—C13 | 117.2 (4) | C18—C17—H17A | 120.3 |
C17—C18—C13 | 120.6 (4) | C10—N2—H2B | 118.1 |
C1—N1—C9 | 118.4 (4) | C18—N2—H2B | 118.1 |
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