Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680200805X/bt6137sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680200805X/bt6137Isup2.hkl |
CCDC reference: 189306
Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: CAD-4 Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1999); software used to prepare material for publication: SHELXL97.
[CdCl2(C3H7NO2)] | F(000) = 520 |
Mr = 272.40 | Dx = 2.527 Mg m−3 Dm = 2.53 Mg m−3 Dm measured by floatation in a mixture of carbon tetrachloride and bromoform |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 25 reflections |
a = 6.9391 (10) Å | θ = 12–18° |
b = 12.945 (2) Å | µ = 3.72 mm−1 |
c = 7.9714 (10) Å | T = 293 K |
V = 716.05 (18) Å3 | Hexagonal needle, colourless |
Z = 4 | 0.30 × 0.20 × 0.10 mm |
Enraf-Nonius CAD-4 diffractometer | 652 reflections with I > 2s(I) |
Radiation source: fine-focus sealed tube | Rint = 0.037 |
Graphite monochromator | θmax = 25.0°, θmin = 3.0° |
ω–2θ scans | h = 0→8 |
Absorption correction: ψ scan (North et al., 1968) | k = −15→15 |
Tmin = 0.42, Tmax = 0.68 | l = −9→9 |
1727 measured reflections | 2 standard reflections every 100 reflections |
673 independent reflections | intensity decay: 0.1% |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.032 | w = 1/[σ2(Fo2) + (0.0489P)2 + 1.0571P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.081 | (Δ/σ)max = 0.001 |
S = 1.23 | Δρmax = 1.26 e Å−3 |
673 reflections | Δρmin = −0.80 e Å−3 |
83 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.0162 (18) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 0000 Friedel reflections |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.05 (11) |
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 | ||
Cd1 | 0.82893 (6) | 0.72845 (3) | 0.8492 (4) | 0.0246 (3) | |
Cl1 | 0.5940 (8) | 0.8072 (4) | 1.0744 (3) | 0.0399 (10) | |
Cl2 | 0.5951 (8) | 0.8102 (4) | 0.6266 (2) | 0.0394 (11) | |
O1 | 0.4558 (9) | 0.6036 (4) | 0.837 (3) | 0.065 (3) | |
O2 | 0.7522 (8) | 0.5585 (4) | 0.8818 (18) | 0.055 (3) | |
N1 | 0.1682 (9) | 0.4623 (7) | 0.7906 (12) | 0.040 (2) | |
H1A | 0.0496 | 0.4509 | 0.8288 | 0.059* | |
H1B | 0.1784 | 0.4380 | 0.6866 | 0.059* | |
H1C | 0.1918 | 0.5299 | 0.7907 | 0.059* | |
C1 | 0.5803 (9) | 0.5371 (4) | 0.845 (2) | 0.0222 (13) | |
C2 | 0.5127 (10) | 0.4254 (5) | 0.843 (2) | 0.0327 (16) | |
H2A | 0.5252 | 0.3991 | 0.7293 | 0.039* | |
H2B | 0.5974 | 0.3850 | 0.9139 | 0.039* | |
C3 | 0.3092 (12) | 0.4094 (8) | 0.8999 (13) | 0.040 (2) | |
H3A | 0.2812 | 0.3360 | 0.9013 | 0.049* | |
H3B | 0.2957 | 0.4352 | 1.0136 | 0.049* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0227 (3) | 0.0218 (4) | 0.0292 (4) | 0.00109 (14) | 0.0001 (5) | −0.0009 (4) |
Cl1 | 0.030 (3) | 0.056 (2) | 0.033 (2) | −0.003 (2) | 0.0003 (18) | −0.0161 (18) |
Cl2 | 0.035 (3) | 0.060 (3) | 0.024 (2) | 0.007 (2) | 0.0040 (17) | 0.0171 (18) |
O1 | 0.038 (3) | 0.021 (2) | 0.136 (8) | 0.002 (2) | −0.022 (9) | −0.004 (6) |
O2 | 0.028 (3) | 0.029 (3) | 0.108 (10) | −0.009 (2) | −0.007 (4) | 0.016 (5) |
N1 | 0.027 (4) | 0.040 (5) | 0.052 (5) | −0.006 (3) | −0.004 (3) | −0.010 (4) |
C1 | 0.027 (3) | 0.021 (3) | 0.018 (3) | −0.001 (2) | −0.003 (7) | −0.010 (5) |
C2 | 0.036 (3) | 0.019 (3) | 0.044 (4) | −0.002 (2) | 0.001 (9) | 0.004 (6) |
C3 | 0.042 (5) | 0.036 (4) | 0.044 (6) | −0.004 (4) | −0.010 (4) | 0.015 (4) |
Cd1—O2 | 2.278 (5) | N1—C3 | 1.478 (12) |
Cd1—O1i | 2.348 (5) | N1—H1A | 0.8900 |
Cd1—Cl1i | 2.612 (5) | N1—H1B | 0.8900 |
Cd1—Cl2i | 2.609 (5) | N1—H1C | 0.8900 |
Cd1—Cl1 | 2.631 (5) | C1—C2 | 1.520 (8) |
Cd1—Cl2 | 2.627 (4) | C2—C3 | 1.498 (12) |
Cl1—Cd1ii | 2.612 (5) | C2—H2A | 0.9700 |
Cl2—Cd1ii | 2.609 (4) | C2—H2B | 0.9700 |
O1—C1 | 1.221 (8) | C3—H3A | 0.9700 |
O1—Cd1ii | 2.348 (5) | C3—H3B | 0.9700 |
O2—C1 | 1.259 (10) | ||
O2—Cd1—O1i | 170.6 (3) | C3—N1—H1B | 109.5 |
O2—Cd1—Cl1i | 85.2 (3) | H1A—N1—H1B | 109.5 |
O1i—Cd1—Cl1i | 85.8 (4) | C3—N1—H1C | 109.5 |
O2—Cd1—Cl2i | 93.3 (3) | H1A—N1—H1C | 109.5 |
O1i—Cd1—Cl2i | 83.4 (4) | H1B—N1—H1C | 109.5 |
Cl1i—Cd1—Cl2i | 86.27 (6) | O1—C1—O2 | 121.8 (6) |
O2—Cd1—Cl1 | 98.7 (3) | O1—C1—C2 | 116.8 (6) |
O1i—Cd1—Cl1 | 84.3 (4) | O2—C1—C2 | 120.3 (6) |
Cl1i—Cd1—Cl1 | 92.05 (16) | C3—C2—C1 | 114.7 (8) |
Cl2i—Cd1—Cl1 | 167.67 (18) | C3—C2—H2A | 108.6 |
O2—Cd1—Cl2 | 108.8 (3) | C1—C2—H2A | 108.6 |
O1i—Cd1—Cl2 | 80.3 (4) | C3—C2—H2B | 108.6 |
Cl1i—Cd1—Cl2 | 166.08 (19) | C1—C2—H2B | 108.6 |
Cl2i—Cd1—Cl2 | 93.17 (15) | H2A—C2—H2B | 107.6 |
Cl1—Cd1—Cl2 | 85.52 (6) | N1—C3—C2 | 112.4 (8) |
Cd1ii—Cl1—Cd1 | 84.19 (11) | N1—C3—H3A | 109.1 |
Cd1ii—Cl2—Cd1 | 84.32 (10) | C2—C3—H3A | 109.1 |
C1—O1—Cd1ii | 156.3 (6) | N1—C3—H3B | 109.1 |
C1—O2—Cd1 | 114.1 (5) | C2—C3—H3B | 109.1 |
C3—N1—H1A | 109.5 | H3A—C3—H3B | 107.9 |
O2—Cd1—Cl1—Cd1ii | −75.8 (3) | Cl1—Cd1—O2—C1 | 63.3 (12) |
O1i—Cd1—Cl1—Cd1ii | 113.2 (4) | Cl2—Cd1—O2—C1 | −24.9 (13) |
Cl1i—Cd1—Cl1—Cd1ii | −161.19 (19) | Cd1ii—O1—C1—O2 | 1 (6) |
Cl2i—Cd1—Cl1—Cd1ii | 116.9 (7) | Cd1ii—O1—C1—C2 | 170 (3) |
Cl2—Cd1—Cl1—Cd1ii | 32.54 (9) | Cd1—O2—C1—O1 | −18 (3) |
O2—Cd1—Cl2—Cd1ii | 65.1 (3) | Cd1—O2—C1—C2 | 173.5 (12) |
O1i—Cd1—Cl2—Cd1ii | −117.6 (4) | O1—C1—C2—C3 | −24 (3) |
Cl1i—Cd1—Cl2—Cd1ii | −113.0 (5) | O2—C1—C2—C3 | 145.0 (15) |
Cl2i—Cd1—Cl2—Cd1ii | 159.73 (17) | C1—C2—C3—N1 | 62.5 (17) |
Cl1—Cd1—Cl2—Cd1ii | −32.56 (15) |
Symmetry codes: (i) x+1/2, −y+3/2, z; (ii) x−1/2, −y+3/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O2iii | 0.89 | 2.53 | 3.227 (10) | 136 |
N1—H1B···O2iv | 0.89 | 2.48 | 3.317 (16) | 157 |
N1—H1B···Cl1v | 0.89 | 2.69 | 3.212 (9) | 119 |
N1—H1C···O1 | 0.89 | 2.10 | 2.732 (10) | 127 |
N1—H1C···Cl2ii | 0.89 | 2.54 | 3.262 (11) | 139 |
Symmetry codes: (ii) x−1/2, −y+3/2, z; (iii) x−1, y, z; (iv) −x+1, −y+1, z−1/2; (v) −x+1/2, y−1/2, z−1/2. |