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In the title compound, [CdCl2(C3H7NO2)]n, the β-alanine residues exist in the zwitterionic form. The Cd atoms are coordinated by four Cl atoms and two O atoms, forming a distorted octahedral environment. These octahedra are linked through Cl—Cl edges and are bridged by the carboxyl groups of the β-alanine residues, to form a one-dimensional polymer chain that extends along [100].
Supporting information
CCDC reference: 189306
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.010 Å
- R factor = 0.032
- wR factor = 0.081
- Data-to-parameter ratio = 8.1
checkCIF results
No syntax errors found
Alert Level B:
PLAT_111 Alert B ADDSYM detects (pseudo) centre of symmetry ... 88 Perc Fit
PLAT_113 Alert B ADDSYM suggests Pseudo/New Spacegroup ........ Pnma
General Notes
REFLT_03
From the CIF: _diffrn_reflns_theta_max 25.00
From the CIF: _reflns_number_total 673
Count of symmetry unique reflns 682
Completeness (_total/calc) 98.68%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 0
Fraction of Friedel pairs measured 0.000
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
2 Alert Level B = Potential problem
0 Alert Level C = Please check
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.
Dichloro(
β-alanine)cadmium(II)
top
Crystal data top
[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 |
Data collection top
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 top
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) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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* | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |
Hydrogen-bond geometry (Å, º) top
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. |
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