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The crystal structure of the title compound, {[Co(C2H5NO2)2(H2O)2]Cl2}n, is presented and compared with other compounds of glycine and MII chlorides. It contains CoO6 octahedra connected by glycine molecules into layers. The Co atoms lie on centres of inversion. Chloride ions are located between the layers. It is the first known example of a glycine–MII chloride with a glycine–metal ratio of 2:1.
Supporting information
CCDC reference: 252784
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.002 Å
- R factor = 0.022
- wR factor = 0.058
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 2
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for Co
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.08
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O1W - H2W ... 0.70 Ang.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius BV, 2003); cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: HKL DENZO (Otwinowski & Minor 1997) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff et al., 1997) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
Crystal data top
[Co(C2H5NO2)2(H2O)2]2Cl | Dx = 1.876 Mg m−3 |
Mr = 316.00 | Melting point: not determined K |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.568 (2) Å | Cell parameters from 1496 reflections |
b = 5.988 (1) Å | θ = 2.0–28.3° |
c = 8.844 (2) Å | µ = 2.02 mm−1 |
β = 91.55 (3)° | T = 293 K |
V = 559.45 (19) Å3 | Fragment, pink |
Z = 2 | 0.30 × 0.30 × 0.10 mm |
F(000) = 322 | |
Data collection top
Nonius Kappa CCD diffractometer | 1376 independent reflections |
Radiation source: fine-focus sealed tube | 1274 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.012 |
Detector resolution: 9 pixels mm-1 | θmax = 28.3°, θmin = 3.9° |
φ and ω scans | h = −14→14 |
Absorption correction: multi-scan (Program?; Otwinowski & Minor, 1997) | k = −7→7 |
Tmin = 0.582, Tmax = 0.823 | l = −11→11 |
2525 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.022 | All H-atom parameters refined |
wR(F2) = 0.058 | w = 1/[σ2(Fo2) + (0.0275P)2 + 0.3111P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max = 0.001 |
1376 reflections | Δρmax = 0.57 e Å−3 |
99 parameters | Δρmin = −0.50 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.033 (3) |
Special details top
Experimental. Single-crystal X-ray intensity data were collected at 293 K on a Nonius Kappa
diffractometer with CCD-area detector, using 271 frames with phi- and
omega-increments of 2 degrees and a counting time of 30 s per frame. The
crystal- to-detector-distance was 30 mm. The whole ewald sphere was measured.
The reflection data were processed with the Nonius program suite
DENZO-SMN and corrected for Lorentz, polarization, background and
absorption effects (Otwinowski and Minor, 1997). The crystal structure was
determined by Direct methods (SHELXS97, Sheldrick, 1997) and subsequent
Fourier and difference Fourier syntheses, followed by full-matrix
least-squares refinements on F2 (SHELXL97, Sheldrick, 1997). All
hydrogen atoms were refined freely. Using anisotropic treatment of the non-H
atoms and unrestrained isotropic treatment of the H atoms, the refinement
converged at R-values of 0.022. |
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 | |
Co | 0.5000 | 0.0000 | 0.5000 | 0.01638 (12) | |
O1 | 0.65086 (10) | 0.36581 (19) | 0.88140 (11) | 0.0229 (2) | |
O2 | 0.55048 (10) | 0.1680 (2) | 0.70159 (12) | 0.0286 (3) | |
C1 | 0.64769 (13) | 0.2505 (2) | 0.76336 (15) | 0.0187 (3) | |
C2 | 0.77360 (15) | 0.2165 (3) | 0.68777 (18) | 0.0265 (3) | |
H1C | 0.782 (2) | 0.074 (5) | 0.657 (3) | 0.042 (6)* | |
H2C | 0.772 (2) | 0.311 (4) | 0.603 (3) | 0.039 (6)* | |
N | 0.88136 (13) | 0.2833 (3) | 0.78734 (17) | 0.0267 (3) | |
H1N | 0.865 (2) | 0.419 (5) | 0.827 (3) | 0.044 (6)* | |
H2N | 0.952 (2) | 0.298 (4) | 0.730 (3) | 0.043 (6)* | |
H3N | 0.900 (2) | 0.179 (5) | 0.857 (3) | 0.052 (7)* | |
O1W | 0.38810 (13) | 0.2699 (3) | 0.43828 (17) | 0.0364 (3) | |
H1W | 0.316 (3) | 0.285 (5) | 0.456 (3) | 0.052 (7)* | |
H2W | 0.406 (3) | 0.316 (5) | 0.369 (3) | 0.056 (9)* | |
Cl | 1.11073 (4) | 0.28327 (8) | 0.55838 (5) | 0.03446 (14) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.01380 (16) | 0.02165 (18) | 0.01379 (16) | 0.00019 (9) | 0.00210 (10) | 0.00073 (9) |
O1 | 0.0167 (5) | 0.0321 (6) | 0.0201 (5) | 0.0005 (4) | 0.0027 (4) | −0.0086 (4) |
O2 | 0.0205 (5) | 0.0431 (7) | 0.0222 (5) | −0.0062 (5) | 0.0026 (4) | −0.0115 (5) |
C1 | 0.0185 (6) | 0.0215 (7) | 0.0162 (6) | 0.0007 (5) | 0.0030 (5) | 0.0001 (5) |
C2 | 0.0200 (7) | 0.0368 (9) | 0.0228 (7) | 0.0011 (6) | 0.0043 (6) | −0.0104 (7) |
N | 0.0174 (6) | 0.0350 (8) | 0.0280 (7) | −0.0002 (5) | 0.0041 (5) | −0.0061 (6) |
O1W | 0.0269 (7) | 0.0416 (8) | 0.0415 (8) | 0.0124 (6) | 0.0140 (6) | 0.0178 (6) |
Cl | 0.0270 (2) | 0.0331 (2) | 0.0438 (3) | 0.00645 (16) | 0.01172 (17) | 0.00402 (17) |
Geometric parameters (Å, º) top
Co—O1W | 2.0673 (14) | C1—C2 | 1.519 (2) |
Co—O1Wi | 2.0673 (14) | C2—N | 1.476 (2) |
Co—O1ii | 2.0924 (11) | C2—H1C | 0.90 (3) |
Co—O1iii | 2.0924 (11) | C2—H2C | 0.94 (2) |
Co—O2i | 2.1031 (11) | N—H1N | 0.90 (3) |
Co—O2 | 2.1031 (11) | N—H2N | 0.91 (3) |
O1—C1 | 1.2513 (17) | N—H3N | 0.89 (3) |
O1—Coiv | 2.0924 (11) | O1W—H1W | 0.79 (3) |
O2—C1 | 1.2520 (18) | O1W—H2W | 0.70 (3) |
| | | |
O1W—Co—O1Wi | 180.00 (8) | O1—C1—C2 | 115.92 (13) |
O1W—Co—O1ii | 90.32 (5) | O2—C1—C2 | 118.25 (13) |
O1Wi—Co—O1ii | 89.68 (5) | N—C2—C1 | 111.85 (12) |
O1W—Co—O1iii | 89.68 (5) | N—C2—H1C | 110.4 (15) |
O1Wi—Co—O1iii | 90.32 (5) | C1—C2—H1C | 110.9 (15) |
O1ii—Co—O1iii | 180.00 (4) | N—C2—H2C | 108.0 (14) |
O1W—Co—O2i | 91.14 (6) | C1—C2—H2C | 106.0 (14) |
O1Wi—Co—O2i | 88.86 (6) | H1C—C2—H2C | 109 (2) |
O1ii—Co—O2i | 86.44 (5) | C2—N—H1N | 109.0 (15) |
O1iii—Co—O2i | 93.56 (5) | C2—N—H2N | 108.7 (14) |
O1W—Co—O2 | 88.86 (6) | H1N—N—H2N | 107 (2) |
O1Wi—Co—O2 | 91.14 (6) | C2—N—H3N | 111.7 (17) |
O1ii—Co—O2 | 93.56 (5) | H1N—N—H3N | 114 (2) |
O1iii—Co—O2 | 86.44 (5) | H2N—N—H3N | 107 (2) |
O2i—Co—O2 | 180.0 | Co—O1W—H1W | 126 (2) |
C1—O1—Coiv | 128.79 (10) | Co—O1W—H2W | 112 (2) |
C1—O2—Co | 138.16 (10) | H1W—O1W—H2W | 115 (3) |
O1—C1—O2 | 125.80 (13) | | |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x, −y+1/2, z−1/2; (iii) −x+1, y−1/2, −z+3/2; (iv) −x+1, y+1/2, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N—H1N···Clv | 0.90 (3) | 2.41 (3) | 3.2905 (17) | 163 (2) |
N—H2N···Cl | 0.91 (3) | 2.30 (3) | 3.2002 (17) | 169 (2) |
N—H1N···Clv | 0.90 (3) | 2.41 (3) | 3.2905 (17) | 163 (2) |
O1W—H1W···Clvi | 0.79 (3) | 2.38 (3) | 3.1457 (17) | 167 (3) |
O1W—H2W···O2ii | 0.70 (3) | 2.16 (3) | 2.768 (2) | 146 (3) |
Symmetry codes: (ii) x, −y+1/2, z−1/2; (v) −x+2, y+1/2, −z+3/2; (vi) x−1, y, z. |
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