Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802023085/ya6146sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802023085/ya6146Isup2.hkl |
CCDC reference: 202977
Data collection: R3m Software (Nicolet, 1980); cell refinement: R3m Software; data reduction: R3m Software; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2002); software used to prepare material for publication: SHELXL97.
[CuCl2(C5H10N4)] | Z = 2 |
Mr = 260.61 | F(000) = 262 |
Triclinic, P1 | Dx = 1.716 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 6.1054 (15) Å | Cell parameters from 25 reflections |
b = 9.598 (3) Å | θ = 19.2–22.1° |
c = 9.813 (3) Å | µ = 2.65 mm−1 |
α = 108.92 (2)° | T = 293 K |
β = 106.899 (19)° | Prism, green |
γ = 97.39 (2)° | 0.60 × 0.42 × 0.10 mm |
V = 504.5 (2) Å3 |
Nicolet R3m four-circle diffractometer | 2663 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.028 |
Graphite monochromator | θmax = 30.1°, θmin = 2.3° |
ω/2θ scans | h = −8→8 |
Absorption correction: ψ scan (North et al., 1968) | k = −13→12 |
Tmin = 0.299, Tmax = 0.778 | l = 0→13 |
3216 measured reflections | 3 standard reflections every 100 reflections |
2961 independent reflections | intensity decay: 0.6% |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0593P)2 + 0.2094P] where P = (Fo2 + 2Fc2)/3 |
2961 reflections | (Δ/σ)max < 0.001 |
112 parameters | Δρmax = 1.04 e Å−3 |
0 restraints | Δρmin = −0.87 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 | ||
Cu1 | 0.22407 (4) | 0.41412 (3) | 0.49362 (3) | 0.03175 (10) | |
Cl1 | 0.59253 (8) | 0.45976 (6) | 0.66413 (6) | 0.03636 (12) | |
Cl2 | 0.16180 (9) | 0.62584 (6) | 0.65569 (6) | 0.04406 (15) | |
N1 | 0.3290 (4) | −0.0171 (3) | 0.3036 (3) | 0.0648 (7) | |
N2 | 0.0982 (3) | −0.03464 (19) | 0.2408 (2) | 0.0350 (3) | |
N3 | 0.0305 (3) | 0.0903 (2) | 0.2848 (2) | 0.0417 (4) | |
N4 | 0.2226 (3) | 0.1962 (2) | 0.3855 (2) | 0.0369 (4) | |
C5 | 0.4010 (5) | 0.1278 (3) | 0.3940 (4) | 0.0607 (8) | |
H5 | 0.5573 | 0.1769 | 0.4563 | 0.073* | |
C6 | −0.0690 (4) | −0.1850 (2) | 0.1303 (3) | 0.0394 (4) | |
C7 | −0.2789 (5) | −0.1530 (3) | 0.0281 (4) | 0.0599 (7) | |
H7A | −0.3599 | −0.0984 | 0.0898 | 0.090* | |
H7B | −0.3846 | −0.2472 | −0.0475 | 0.090* | |
H7C | −0.2250 | −0.0931 | −0.0228 | 0.090* | |
C8 | 0.0642 (6) | −0.2725 (3) | 0.0382 (4) | 0.0661 (8) | |
H8A | 0.1124 | −0.2173 | −0.0184 | 0.099* | |
H8B | −0.0365 | −0.3704 | −0.0323 | 0.099* | |
H8C | 0.2011 | −0.2854 | 0.1069 | 0.099* | |
C9 | −0.1393 (7) | −0.2653 (4) | 0.2264 (4) | 0.0780 (10) | |
H9A | −0.0004 | −0.2756 | 0.2956 | 0.117* | |
H9B | −0.2407 | −0.3641 | 0.1599 | 0.117* | |
H9C | −0.2215 | −0.2071 | 0.2845 | 0.117* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.02355 (13) | 0.03013 (14) | 0.03111 (14) | 0.00532 (9) | 0.00740 (9) | 0.00112 (10) |
Cl1 | 0.0283 (2) | 0.0393 (3) | 0.0319 (2) | 0.00523 (18) | 0.00467 (17) | 0.00819 (19) |
Cl2 | 0.0266 (2) | 0.0424 (3) | 0.0398 (3) | 0.00939 (19) | 0.00530 (19) | −0.0082 (2) |
N1 | 0.0396 (11) | 0.0377 (11) | 0.0812 (17) | 0.0125 (9) | −0.0026 (11) | −0.0019 (11) |
N2 | 0.0344 (8) | 0.0298 (8) | 0.0328 (8) | 0.0065 (6) | 0.0080 (7) | 0.0059 (6) |
N3 | 0.0314 (8) | 0.0319 (8) | 0.0458 (10) | 0.0053 (7) | 0.0086 (7) | 0.0002 (7) |
N4 | 0.0316 (8) | 0.0305 (8) | 0.0370 (8) | 0.0053 (6) | 0.0075 (7) | 0.0032 (7) |
C5 | 0.0364 (12) | 0.0378 (12) | 0.0744 (19) | 0.0097 (9) | −0.0034 (12) | −0.0005 (12) |
C6 | 0.0376 (10) | 0.0292 (9) | 0.0383 (10) | 0.0011 (8) | 0.0081 (8) | 0.0039 (8) |
C7 | 0.0442 (13) | 0.0483 (14) | 0.0569 (15) | 0.0058 (11) | −0.0026 (12) | 0.0026 (12) |
C8 | 0.0578 (16) | 0.0510 (15) | 0.0569 (16) | 0.0118 (12) | 0.0136 (13) | −0.0136 (12) |
C9 | 0.085 (2) | 0.0624 (19) | 0.081 (2) | −0.0088 (17) | 0.0273 (19) | 0.0328 (17) |
Cu1—Cl1 | 2.2661 (9) | C6—C9 | 1.512 (4) |
Cu1—Cl2i | 2.2892 (9) | C6—C8 | 1.515 (4) |
Cu1—Cl2 | 2.2931 (9) | C6—C7 | 1.516 (4) |
Cu1—Cl1ii | 2.6438 (8) | C7—H7A | 0.9600 |
Cu1—N4 | 2.0131 (19) | C7—H7B | 0.9600 |
N1—N2 | 1.327 (3) | C7—H7C | 0.9600 |
N1—C5 | 1.316 (3) | C8—H8A | 0.9600 |
N2—N3 | 1.300 (2) | C8—H8B | 0.9600 |
N2—C6 | 1.504 (3) | C8—H8C | 0.9600 |
N3—N4 | 1.324 (2) | C9—H9A | 0.9600 |
N4—C5 | 1.339 (3) | C9—H9B | 0.9600 |
C5—H5 | 0.9300 | C9—H9C | 0.9600 |
N4—Cu1—Cl1 | 91.54 (6) | N2—C6—C8 | 107.18 (19) |
N4—Cu1—Cl2i | 91.39 (6) | C9—C6—C8 | 111.1 (3) |
Cl1—Cu1—Cl2i | 173.63 (2) | N2—C6—C7 | 107.66 (19) |
N4—Cu1—Cl2 | 161.22 (6) | C9—C6—C7 | 112.1 (3) |
Cl1—Cu1—Cl2 | 90.59 (4) | C8—C6—C7 | 111.6 (2) |
Cl2i—Cu1—Cl2 | 84.83 (4) | C6—C7—H7A | 109.5 |
N4—Cu1—Cl1ii | 99.64 (6) | C6—C7—H7B | 109.5 |
Cl1—Cu1—Cl1ii | 89.26 (3) | H7A—C7—H7B | 109.5 |
Cl2i—Cu1—Cl1ii | 95.82 (3) | C6—C7—H7C | 109.5 |
Cl2—Cu1—Cl1ii | 99.05 (3) | H7A—C7—H7C | 109.5 |
Cu1—Cl1—Cu1ii | 90.74 (3) | H7B—C7—H7C | 109.5 |
Cu1i—Cl2—Cu1 | 95.17 (4) | C6—C8—H8A | 109.5 |
C5—N1—N2 | 102.2 (2) | C6—C8—H8B | 109.5 |
N3—N2—N1 | 113.55 (18) | H8A—C8—H8B | 109.5 |
N3—N2—C6 | 123.33 (18) | C6—C8—H8C | 109.5 |
N1—N2—C6 | 123.12 (18) | H8A—C8—H8C | 109.5 |
N2—N3—N4 | 106.15 (18) | H8B—C8—H8C | 109.5 |
N3—N4—C5 | 106.08 (19) | C6—C9—H9A | 109.5 |
N3—N4—Cu1 | 123.85 (14) | C6—C9—H9B | 109.5 |
C5—N4—Cu1 | 130.06 (16) | H9A—C9—H9B | 109.5 |
N1—C5—N4 | 111.9 (2) | C6—C9—H9C | 109.5 |
N1—C5—H5 | 124.0 | H9A—C9—H9C | 109.5 |
N4—C5—H5 | 124.0 | H9B—C9—H9C | 109.5 |
N2—C6—C9 | 106.9 (2) | ||
N4—Cu1—Cl1—Cu1ii | 99.62 (6) | Cl2—Cu1—N4—N3 | 70.2 (3) |
Cl2—Cu1—Cl1—Cu1ii | −99.04 (3) | Cl1ii—Cu1—N4—N3 | −103.87 (18) |
Cl1ii—Cu1—Cl1—Cu1ii | 0.0 | Cl1—Cu1—N4—C5 | −14.8 (3) |
N4—Cu1—Cl2—Cu1i | −79.02 (17) | Cl2i—Cu1—N4—C5 | 170.8 (3) |
Cl1—Cu1—Cl2—Cu1i | −175.57 (2) | Cl2—Cu1—N4—C5 | −111.2 (3) |
Cl2i—Cu1—Cl2—Cu1i | 0.0 | Cl1ii—Cu1—N4—C5 | 74.7 (3) |
Cl1ii—Cu1—Cl2—Cu1i | 95.08 (3) | N2—N1—C5—N4 | −0.7 (4) |
C5—N1—N2—N3 | 1.6 (3) | N3—N4—C5—N1 | −0.5 (4) |
C5—N1—N2—C6 | −177.9 (2) | Cu1—N4—C5—N1 | −179.2 (2) |
N1—N2—N3—N4 | −2.0 (3) | N3—N2—C6—C9 | −93.3 (3) |
C6—N2—N3—N4 | 177.52 (18) | N1—N2—C6—C9 | 86.2 (3) |
N2—N3—N4—C5 | 1.4 (3) | N3—N2—C6—C8 | 147.5 (2) |
N2—N3—N4—Cu1 | −179.71 (14) | N1—N2—C6—C8 | −33.0 (3) |
Cl1—Cu1—N4—N3 | 166.62 (18) | N3—N2—C6—C7 | 27.3 (3) |
Cl2i—Cu1—N4—N3 | −7.73 (18) | N1—N2—C6—C7 | −153.2 (3) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1. |