Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801011904/cf6068sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801011904/cf6068Isup2.hkl |
CCDC reference: 170876
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.008 Å
- H-atom completeness 76%
- Disorder in solvent or counterion
- R factor = 0.035
- wR factor = 0.106
- Data-to-parameter ratio = 19.2
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level A:
DIFF_012 Alert A _diffrn_reflns_av_R_equivalents is missing R factor for symmetry-equivalent intensities. The following tests will not be performed RINTA
Alert Level C:
CHEMW_01 Alert C The difference between the given and expected weight for compound is greater 1 mass unit. Check that all hydrogen atoms have been taken into account. PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 2 PLAT_302 Alert C Anion/Solvent Disorder ....................... 25.00 Perc. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C26 H24 Cd2 Cl2 N4 O9 Atom count from the _atom_site data: C26 H18 Cd2 Cl2 N4 O9 CELLZ_01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C26 H24 Cd2 Cl2 N4 O9 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 104.00 104.00 0.00 H 96.00 72.00 24.00 Cd 8.00 8.00 0.00 Cl 8.00 8.00 0.00 N 16.00 16.00 0.00 O 36.00 36.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional? CHEMW_03 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 840.29 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 26.00 312.29 H 1.01 18.00 18.14 O 16.00 9.00 143.99 N 14.01 4.00 56.03 Cd 112.41 2.00 224.82 Cl 35.45 2.00 70.91 Calculated formula weight 826.17 The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
3 Alert Level C = Please check
A single colorless crystal was obtained by slow evaporation of a 90% ethanol–water solution of a 4:1 molar ratio mixture of 2-pyridinecarboxylic acid and CdCl2·2.5H2O at room temparature.
All H atoms were initially located from difference Fourier maps. All except those on carboxylate groups were positioned with ideal geometry.
Data collection: MSC/AFC Diffractometer Control (Molecular Structure Corporation, 1992); cell refinement: MSC/AFC Diffractometer Control; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: TEXSAN; molecular graphics: ORTEP II (Johnson, 1976); software used to prepare material for publication: TEXSAN.
Fig. 1. ORTEPII (Johnson, 1976) drawing of the title compound with the atomic numbering scheme. Ellipsoids for non-H atoms correspond to 50% probability. |
[Cd2Cl2(C6H4NO2)2(C6H5NO2)2]·C2H6O | Dx = 1.768 Mg m−3 |
Mr = 840.29 | Mo Kα radiation, λ = 0.7107 Å |
Orthorhombic, Pbcm | Cell parameters from 25 reflections |
a = 9.891 (2) Å | θ = 14.7–14.9° |
b = 15.443 (1) Å | µ = 1.57 mm−1 |
c = 20.664 (2) Å | T = 296 K |
V = 3156 (1) Å3 | Plate, colorless |
Z = 4 | 0.50 × 0.20 × 0.15 mm |
F(000) = 1616.0 |
Rigaku AFC-5R diffractometer | θmax = 27.5° |
ω–2θ scans | h = 0→12 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→20 |
Tmin = 0.525, Tmax = 0.790 | l = 0→26 |
3725 measured reflections | 3 standard reflections every 150 reflections |
3725 independent reflections | intensity decay: 1.5% |
2525 reflections with F2 > 2σ(F2) |
Refinement on F2 | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.035 | w = 1/[σ2(Fo2) + {0.03[Max(Fo2,0) + 2Fc2]/3}2] |
wR(F2) = 0.106 | (Δ/σ)max = 0.002 |
S = 1.58 | Δρmax = 0.68 e Å−3 |
3725 reflections | Δρmin = −1.09 e Å−3 |
194 parameters |
[Cd2Cl2(C6H4NO2)2(C6H5NO2)2]·C2H6O | V = 3156 (1) Å3 |
Mr = 840.29 | Z = 4 |
Orthorhombic, Pbcm | Mo Kα radiation |
a = 9.891 (2) Å | µ = 1.57 mm−1 |
b = 15.443 (1) Å | T = 296 K |
c = 20.664 (2) Å | 0.50 × 0.20 × 0.15 mm |
Rigaku AFC-5R diffractometer | 3725 independent reflections |
Absorption correction: ψ scan (North et al., 1968) | 2525 reflections with F2 > 2σ(F2) |
Tmin = 0.525, Tmax = 0.790 | 3 standard reflections every 150 reflections |
3725 measured reflections | intensity decay: 1.5% |
R[F2 > 2σ(F2)] = 0.035 | 194 parameters |
wR(F2) = 0.106 | H-atom parameters not refined |
S = 1.58 | Δρmax = 0.68 e Å−3 |
3725 reflections | Δρmin = −1.09 e Å−3 |
Refinement. Refinement using reflections with F2 > 0.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cd1 | 0.20564 (3) | 0.12230 (2) | 0.65888 (2) | 0.03931 (9) | |
Cl1 | 0.1025 (2) | 0.21642 (10) | 0.7500 | 0.0468 (4) | |
Cl2 | 0.3023 (2) | 0.0232 (1) | 0.7500 | 0.0541 (5) | |
O1 | 0.3435 (3) | 0.0558 (2) | 0.5833 (2) | 0.0526 (10) | |
O2 | 0.5308 (4) | 0.0687 (2) | 0.5256 (2) | 0.078 (1) | |
O3 | 0.0739 (3) | 0.1890 (2) | 0.5797 (2) | 0.0487 (9) | |
O4 | −0.1066 (3) | 0.1742 (2) | 0.5169 (2) | 0.058 (1) | |
O5 | 0.719 (2) | 0.123 (1) | 0.7500 | 0.305 (9)* | |
N1 | 0.3854 (4) | 0.2148 (2) | 0.6370 (2) | 0.0419 (10) | |
N8 | 0.0398 (4) | 0.0267 (2) | 0.6260 (2) | 0.0412 (10) | |
C2 | 0.4776 (5) | 0.1822 (3) | 0.5958 (2) | 0.045 (1) | |
C3 | 0.5942 (5) | 0.2270 (4) | 0.5794 (3) | 0.072 (2) | |
C4 | 0.6138 (6) | 0.3091 (4) | 0.6059 (3) | 0.086 (2) | |
C5 | 0.5199 (7) | 0.3419 (4) | 0.6466 (3) | 0.073 (2) | |
C6 | 0.4066 (5) | 0.2935 (3) | 0.6618 (2) | 0.054 (1) | |
C7 | 0.4465 (5) | 0.0951 (3) | 0.5673 (2) | 0.049 (1) | |
C9 | −0.0448 (4) | 0.0553 (3) | 0.5804 (2) | 0.040 (1) | |
C10 | −0.1442 (5) | 0.0037 (3) | 0.5533 (3) | 0.057 (2) | |
C11 | −0.1547 (6) | −0.0814 (4) | 0.5753 (3) | 0.065 (2) | |
C12 | −0.0686 (7) | −0.1101 (3) | 0.6215 (3) | 0.068 (2) | |
C13 | 0.0257 (6) | −0.0549 (3) | 0.6468 (2) | 0.055 (1) | |
C14 | −0.0221 (5) | 0.1473 (3) | 0.5584 (2) | 0.042 (1) | |
C15 | 0.643 (2) | −0.014 (1) | 0.7500 | 0.174 (7)* | |
C16 | 0.717 (2) | 0.043 (2) | 0.722 (1) | 0.179 (10)* | 0.50 |
H2 | 0.5000 | 0.0000 | 0.5000 | 0.0717* | |
H3 | 0.6586 | 0.2026 | 0.5504 | 0.0866* | |
H4 | −0.1341 | 0.2500 | 0.5000 | 0.0717* | |
H5 | 0.6924 | 0.3413 | 0.5957 | 0.1043* | |
H6 | 0.5321 | 0.3974 | 0.6652 | 0.0874* | |
H7 | 0.3416 | 0.3171 | 0.6905 | 0.0652* | |
H10 | −0.2039 | 0.0257 | 0.5211 | 0.0686* | |
H11 | −0.2215 | −0.1191 | 0.5578 | 0.0783* | |
H12 | −0.0747 | −0.1684 | 0.6362 | 0.0814* | |
H13 | 0.0825 | −0.0753 | 0.6806 | 0.0658* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0415 (2) | 0.0344 (2) | 0.0420 (2) | −0.0005 (1) | 0.0026 (1) | −0.0035 (1) |
Cl1 | 0.0572 (10) | 0.0411 (8) | 0.0420 (8) | 0.0181 (8) | 0.0000 | 0.0000 |
Cl2 | 0.064 (1) | 0.0466 (9) | 0.0520 (10) | 0.0239 (8) | 0.0000 | 0.0000 |
O1 | 0.052 (2) | 0.048 (2) | 0.058 (2) | −0.007 (2) | 0.015 (2) | −0.020 (2) |
O2 | 0.063 (2) | 0.078 (3) | 0.093 (3) | −0.015 (2) | 0.036 (2) | −0.043 (2) |
O3 | 0.056 (2) | 0.034 (2) | 0.057 (2) | −0.006 (1) | −0.010 (2) | 0.006 (1) |
O4 | 0.041 (2) | 0.064 (2) | 0.069 (2) | −0.004 (2) | −0.008 (2) | 0.027 (2) |
N1 | 0.045 (2) | 0.039 (2) | 0.042 (2) | −0.002 (2) | 0.002 (2) | −0.006 (2) |
N8 | 0.049 (2) | 0.030 (2) | 0.044 (2) | −0.004 (2) | 0.002 (2) | 0.002 (2) |
C2 | 0.042 (2) | 0.045 (2) | 0.048 (3) | −0.003 (2) | 0.005 (2) | −0.007 (2) |
C3 | 0.051 (3) | 0.081 (4) | 0.083 (4) | −0.018 (3) | 0.015 (3) | −0.021 (4) |
C4 | 0.069 (4) | 0.079 (4) | 0.110 (5) | −0.038 (3) | 0.018 (4) | −0.022 (4) |
C5 | 0.087 (4) | 0.056 (3) | 0.075 (4) | −0.025 (3) | 0.007 (3) | −0.014 (3) |
C6 | 0.062 (3) | 0.043 (2) | 0.058 (3) | −0.005 (2) | 0.003 (3) | −0.012 (2) |
C7 | 0.044 (3) | 0.051 (3) | 0.053 (3) | 0.001 (2) | 0.004 (2) | −0.011 (2) |
C9 | 0.044 (2) | 0.038 (2) | 0.039 (2) | −0.005 (2) | 0.009 (2) | 0.001 (2) |
C10 | 0.048 (3) | 0.060 (3) | 0.064 (3) | −0.016 (2) | 0.003 (3) | 0.000 (3) |
C11 | 0.072 (4) | 0.056 (3) | 0.068 (3) | −0.032 (3) | 0.000 (3) | −0.004 (3) |
C12 | 0.089 (4) | 0.033 (2) | 0.081 (4) | −0.018 (3) | 0.009 (4) | 0.002 (3) |
C13 | 0.068 (3) | 0.035 (2) | 0.061 (3) | −0.001 (2) | 0.000 (3) | 0.007 (2) |
C14 | 0.041 (2) | 0.044 (2) | 0.040 (2) | 0.001 (2) | 0.009 (2) | 0.006 (2) |
Cd1—Cl1 | 2.588 (1) | C2—C7 | 1.500 (6) |
Cd1—Cl2 | 2.608 (1) | C3—C4 | 1.396 (8) |
Cd1—O1 | 2.313 (3) | C3—H3 | 0.951 |
Cd1—O3 | 2.332 (3) | C4—C5 | 1.352 (8) |
Cd1—N1 | 2.326 (4) | C4—H5 | 0.946 |
Cd1—N8 | 2.309 (4) | C5—C6 | 1.383 (7) |
O1—C7 | 1.231 (5) | C5—H6 | 0.947 |
O2—C7 | 1.267 (5) | C6—H7 | 0.947 |
O2—H2 | 1.224 | C9—C10 | 1.385 (6) |
O3—C14 | 1.229 (5) | C9—C14 | 1.508 (6) |
O4—C14 | 1.267 (5) | C10—C11 | 1.395 (7) |
O4—H4 | 1.252 | C10—H10 | 0.952 |
O5—C16 | 1.36 (2) | C11—C12 | 1.355 (8) |
O5—C16i | 1.36 (2) | C11—H11 | 0.952 |
N1—C2 | 1.344 (5) | C12—C13 | 1.367 (7) |
N1—C6 | 1.335 (5) | C12—H12 | 0.951 |
N8—C9 | 1.335 (5) | C13—H13 | 0.950 |
N8—C13 | 1.340 (5) | C15—C16 | 1.27 (2) |
C2—C3 | 1.387 (7) | C15—C16i | 1.27 (2) |
Cd1···Cl1 | 2.588 (1) | O3···O4iv | 3.411 (4) |
Cd1···Cl2 | 2.608 (1) | O4···C14iv | 3.274 (5) |
Cl1···O3i | 3.556 (3) | O4···C3vii | 3.330 (6) |
Cl2···C15 | 3.42 (2) | O4···C12iii | 3.488 (7) |
Cl2···O1i | 3.504 (3) | O4···C11iii | 3.516 (7) |
O1···O2ii | 3.211 (4) | C3···C3iv | 3.36 (1) |
O1···C10iii | 3.563 (6) | C5···C15viii | 3.49 (2) |
O2···C7ii | 3.183 (6) | C6···C15viii | 3.53 (2) |
O2···C4iv | 3.409 (9) | C9···C10iii | 3.458 (6) |
O2···C10v | 3.416 (7) | C11···C14iii | 3.424 (7) |
O3···C12vi | 3.221 (6) | ||
Cl1—Cd1—Cl2 | 87.07 (4) | C4—C3—H3 | 120.9 |
Cl1—Cd1—O1 | 166.57 (9) | C3—C4—C5 | 119.3 (5) |
Cl1—Cd1—O3 | 92.41 (8) | C3—C4—H5 | 120.2 |
Cl1—Cd1—N1 | 95.63 (9) | C5—C4—H5 | 120.5 |
Cl1—Cd1—N8 | 107.04 (10) | C4—C5—C6 | 119.8 (5) |
Cl2—Cd1—O1 | 90.61 (9) | C4—C5—H6 | 120.2 |
Cl2—Cd1—O3 | 166.10 (9) | C6—C5—H6 | 120.0 |
Cl2—Cd1—N1 | 102.8 (1) | N1—C6—C5 | 122.1 (5) |
Cl2—Cd1—N8 | 95.61 (10) | N1—C6—H7 | 118.9 |
O1—Cd1—O3 | 93.0 (1) | C5—C6—H7 | 119.0 |
O1—Cd1—N1 | 72.0 (1) | O1—C7—O2 | 124.7 (4) |
O1—Cd1—N8 | 86.3 (1) | O1—C7—C2 | 120.4 (4) |
O3—Cd1—N1 | 91.1 (1) | O2—C7—C2 | 114.9 (4) |
O3—Cd1—N8 | 71.2 (1) | N8—C9—C10 | 122.7 (4) |
N1—Cd1—N8 | 151.5 (1) | N8—C9—C14 | 115.5 (4) |
Cd1—Cl1—Cd1i | 93.35 (5) | C10—C9—C14 | 121.7 (4) |
Cd1—Cl2—Cd1i | 92.43 (5) | C9—C10—C11 | 117.6 (5) |
Cd1—O1—C7 | 116.8 (3) | C9—C10—H10 | 121.2 |
C7—O2—H2 | 114.2 | C11—C10—H10 | 121.2 |
Cd1—O3—C14 | 116.8 (3) | C10—C11—C12 | 119.5 (5) |
C14—O4—H4 | 129.8 | C10—C11—H11 | 120.3 |
Cd1—N1—C2 | 114.3 (3) | C12—C11—H11 | 120.2 |
Cd1—N1—C6 | 127.2 (3) | C11—C12—C13 | 119.6 (5) |
C2—N1—C6 | 118.5 (4) | C11—C12—H12 | 119.7 |
Cd1—N8—C9 | 116.2 (3) | C13—C12—H12 | 120.7 |
Cd1—N8—C13 | 125.5 (3) | N8—C13—C12 | 122.4 (5) |
C9—N8—C13 | 118.2 (4) | N8—C13—H13 | 119.0 |
N1—C2—C3 | 122.1 (4) | C12—C13—H13 | 118.6 |
N1—C2—C7 | 116.4 (4) | O3—C14—O4 | 125.4 (4) |
C3—C2—C7 | 121.4 (4) | O3—C14—C9 | 120.1 (4) |
C2—C3—C4 | 118.2 (5) | O4—C14—C9 | 114.5 (4) |
C2—C3—H3 | 120.9 | O5—C16—C15 | 116 (2) |
Cd1—Cl1—Cd1i—Cl2 | −2.14 (6) | O1—Cd1—N1—C2 | −3.0 (3) |
Cd1—Cl1—Cd1i—O1i | 78.2 (4) | O1—Cd1—N1—C6 | 178.7 (4) |
Cd1—Cl1—Cd1i—O3i | −168.23 (8) | O1—Cd1—N8—C9 | −94.4 (3) |
Cd1—Cl1—Cd1i—N1i | 100.40 (10) | O1—Cd1—N8—C13 | 82.8 (4) |
Cd1—Cl1—Cd1i—N8i | −97.12 (10) | O1—C7—C2—N1 | −2.3 (7) |
Cd1—Cl2—Cd1i—Cl1 | 2.12 (6) | O1—C7—C2—C3 | 178.8 (5) |
Cd1—Cl2—Cd1i—O1i | −164.64 (9) | O2—C7—C2—N1 | 175.7 (4) |
Cd1—Cl2—Cd1i—O3i | 90.3 (4) | O2—C7—C2—C3 | −3.2 (7) |
Cd1—Cl2—Cd1i—N1i | −92.99 (10) | O3—Cd1—O1—C7 | 92.1 (4) |
Cd1—Cl2—Cd1i—N8i | 108.97 (10) | O3—Cd1—N1—C2 | −95.8 (3) |
Cd1—O1—C7—O2 | −178.3 (4) | O3—Cd1—N1—C6 | 85.9 (4) |
Cd1—O1—C7—C2 | −0.6 (6) | O3—Cd1—N8—C9 | 0.0 (3) |
Cd1—O3—C14—O4 | 177.6 (3) | O3—Cd1—N8—C13 | 177.1 (4) |
Cd1—O3—C14—C9 | −3.9 (5) | O3—C14—C9—N8 | 3.9 (6) |
Cd1—N1—C2—C3 | −177.3 (4) | O3—C14—C9—C10 | −174.1 (4) |
Cd1—N1—C2—C7 | 3.8 (5) | O4—C14—C9—N8 | −177.5 (4) |
Cd1—N1—C6—C5 | 178.0 (4) | O4—C14—C9—C10 | 4.6 (6) |
Cd1—N8—C9—C10 | 176.2 (4) | O5—C16—C15—C16i | −39 (2) |
Cd1—N8—C9—C14 | −1.7 (5) | O5—C16—C16i—C15 | 141 (2) |
Cd1—N8—C13—C12 | −174.8 (4) | O5—C16i—C15—C16 | 39 (2) |
Cl1—Cd1—O1—C7 | −21.4 (7) | O5—C16i—C16—C15 | −141 (2) |
Cl1—Cd1—O3—C14 | −105.0 (3) | N1—Cd1—O1—C7 | 1.9 (3) |
Cl1—Cd1—N1—C2 | 171.7 (3) | N1—Cd1—O3—C14 | 159.3 (3) |
Cl1—Cd1—N1—C6 | −6.6 (4) | N1—Cd1—N8—C9 | −54.5 (4) |
Cl1—Cd1—N8—C9 | 86.7 (3) | N1—Cd1—N8—C13 | 122.7 (4) |
Cl1—Cd1—N8—C13 | −96.2 (4) | N1—C2—C3—C4 | −1.2 (9) |
Cl1—Cd1i—O1i—C7i | 21.4 (7) | N1—C6—C5—C4 | −0.6 (10) |
Cl1—Cd1i—O3i—C14i | 105.0 (3) | N8—Cd1—O1—C7 | 163.1 (4) |
Cl1—Cd1i—N1i—C2i | −171.7 (3) | N8—Cd1—O3—C14 | 2.2 (3) |
Cl1—Cd1i—N1i—C6i | 6.6 (4) | N8—Cd1—N1—C2 | −45.4 (5) |
Cl1—Cd1i—N8i—C9i | −86.7 (3) | N8—Cd1—N1—C6 | 136.3 (4) |
Cl1—Cd1i—N8i—C13i | 96.2 (4) | N8—C9—C10—C11 | 0.1 (7) |
Cl2—Cd1—O1—C7 | −101.3 (4) | N8—C13—C12—C11 | −2.3 (9) |
Cl2—Cd1—O3—C14 | −17.5 (6) | C2—N1—C6—C5 | −0.3 (8) |
Cl2—Cd1—N1—C2 | 83.4 (3) | C2—C3—C4—C5 | 0 (1) |
Cl2—Cd1—N1—C6 | −94.9 (4) | C3—C2—N1—C6 | 1.2 (7) |
Cl2—Cd1—N8—C9 | 175.3 (3) | C3—C4—C5—C6 | 0 (1) |
Cl2—Cd1—N8—C13 | −7.5 (4) | C4—C3—C2—C7 | 177.6 (6) |
Cl2—Cd1i—O1i—C7i | 101.3 (4) | C6—N1—C2—C7 | −177.7 (4) |
Cl2—Cd1i—O3i—C14i | 17.5 (6) | C9—N8—C13—C12 | 2.3 (8) |
Cl2—Cd1i—N1i—C2i | −83.4 (3) | C9—C10—C11—C12 | −0.1 (8) |
Cl2—Cd1i—N1i—C6i | 94.9 (4) | C10—C9—N8—C13 | −1.2 (7) |
Cl2—Cd1i—N8i—C9i | −175.3 (3) | C10—C11—C12—C13 | 1.2 (9) |
Cl2—Cd1i—N8i—C13i | 7.5 (4) | C11—C10—C9—C14 | 177.9 (4) |
O1—Cd1—O3—C14 | 87.3 (3) | C13—N8—C9—C14 | −179.1 (4) |
Symmetry codes: (i) x, y, −z+3/2; (ii) −x+1, −y, −z+1; (iii) −x, −y, −z+1; (iv) x, −y+1/2, −z+1; (v) x+1, y, z; (vi) −x, y+1/2, z; (vii) x−1, y, z; (viii) −x+1, y+1/2, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Cd2Cl2(C6H4NO2)2(C6H5NO2)2]·C2H6O |
Mr | 840.29 |
Crystal system, space group | Orthorhombic, Pbcm |
Temperature (K) | 296 |
a, b, c (Å) | 9.891 (2), 15.443 (1), 20.664 (2) |
V (Å3) | 3156 (1) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.57 |
Crystal size (mm) | 0.50 × 0.20 × 0.15 |
Data collection | |
Diffractometer | Rigaku AFC-5R diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.525, 0.790 |
No. of measured, independent and observed [F2 > 2σ(F2)] reflections | 3725, 3725, 2525 |
Rint | ? |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.106, 1.58 |
No. of reflections | 3725 |
No. of parameters | 194 |
No. of restraints | ? |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.68, −1.09 |
Computer programs: MSC/AFC Diffractometer Control (Molecular Structure Corporation, 1992), MSC/AFC Diffractometer Control, TEXSAN (Molecular Structure Corporation, 1999), SIR97 (Altomare et al., 1999), TEXSAN, ORTEP II (Johnson, 1976).
Cd1—Cl1 | 2.588 (1) | Cd1—O3 | 2.332 (3) |
Cd1—Cl2 | 2.608 (1) | Cd1—N1 | 2.326 (4) |
Cd1—O1 | 2.313 (3) | Cd1—N8 | 2.309 (4) |
Cl1—Cd1—Cl2 | 87.07 (4) | O1—Cd1—O3 | 93.0 (1) |
Cl1—Cd1—O1 | 166.57 (9) | O1—Cd1—N1 | 72.0 (1) |
Cl1—Cd1—O3 | 92.41 (8) | O1—Cd1—N8 | 86.3 (1) |
Cl1—Cd1—N1 | 95.63 (9) | O3—Cd1—N1 | 91.1 (1) |
Cl1—Cd1—N8 | 107.04 (10) | O3—Cd1—N8 | 71.2 (1) |
Cl2—Cd1—O1 | 90.61 (9) | N1—Cd1—N8 | 151.5 (1) |
Cl2—Cd1—O3 | 166.10 (9) | Cd1—Cl1—Cd1i | 93.35 (5) |
Cl2—Cd1—N1 | 102.8 (1) | Cd1—Cl2—Cd1i | 92.43 (5) |
Cl2—Cd1—N8 | 95.61 (10) |
Symmetry code: (i) x, y, −z+3/2. |
2-Pyridinecarboxylic acid is one of the tryptophan metabolites and up until now the crystal structures of its NiII and ZnII (Takenaka et al., 1970), CuII (Faure et al., 1973) and MnII (Okabe & Koizumi, 1998) complexes have been determined. Kinetic studies of CoII, CuII and NiII in solution have also been reported (Das & Dash, 1993).
In this study, the structure of a cadmium complex, (I), of 2-pyridinecarboxylic acid has been determined. The Cd atom is coordinated octahedrally by N atoms of two pyridine rings [Cd1—N1 2.326 (5) Å and Cd1—N8 2.307 (5) Å], two O atoms of the carboxylic acid groups [Cd1—O1 2.318 (5) Å and Cd1—O3 2.334 (5) Å] and two Cl atoms [Cd1—Cl1 2.586 (2) Å and Cd1—Cl2 2.608 (2) Å]. The angles around the Cd atom are considerably distorted from ideal octahedral values of 90/180°. The main distortions are those of the chelate rings with narrow O—Cd—N angles: O1—Cd1—N1 72.3 (2)° and O3—Cd1—N8 71.3 (2)°. These values are much smaller than those observed in other metal complexes [O—Ni—N 81° and O—Zn—N 80° (Takenaka et al., 1970), and O—Cu—N 83.6 (1)° (Faure et al., 1973)] and similar to those in the Mn complex [O2—Mn1—N1 74.61 (7)° and O4—Mn1—N2 73.00 (7)°]. The 2-pyridinecarboxylic acid and 2-pyridinecarboxylate ligands lie roughly perpendicular to one another, a typical torsion angle being O1—Cd1—O3—C14 of 87.5 (5), and all corresponding pairs of ligand atoms lie in cis positions. The carboxyl group is nearly coplanar with the pyridine ring plane; O1—C7—C2—N1 - 3.7 (10)° and O3—C14—C9—N8 3.4 (9)°.
In the crystal packing, the complex molecules are bridged via carboxylic H atoms. One H atom bonds to each carboxylate group of two adjacent complex molecules, so that two carboxylate anions share the positive charge of one H+.