Poly[[[diaquacobalt(II)]-di-μ-glycine] dichloride]

The crystal structure of the title compound, {[Co(C₂H₅NO₂)₂(H₂O)₂]Cl₂}_n, is presented and compared with other compounds of glycine and M^II 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–M^II chloride with a glycine–metal ratio of 2:1.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](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

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Computing details

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.

(I)

Crystal data

[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) Å^3	Fragment, pink
Z = 2	0.30 × 0.30 × 0.10 mm
F(000) = 322

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.022	All H-atom parameters refined
wR(F^2) = 0.058	w = 1/[σ^2(Fo^2) + (0.0275P)^2 + 0.3111P] where P = (Fo^2 + 2Fc^2)/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+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.033 (3)

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Co—O1W	2.0673 (14)	C1—C2	1.519 (2)
Co—O1W^i	2.0673 (14)	C2—N	1.476 (2)
Co—O1^ii	2.0924 (11)	C2—H1C	0.90 (3)
Co—O1^iii	2.0924 (11)	C2—H2C	0.94 (2)
Co—O2^i	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—Co^iv	2.0924 (11)	O1W—H1W	0.79 (3)
O2—C1	1.2520 (18)	O1W—H2W	0.70 (3)
O1W—Co—O1W^i	180.00 (8)	O1—C1—C2	115.92 (13)
O1W—Co—O1^ii	90.32 (5)	O2—C1—C2	118.25 (13)
O1W^i—Co—O1^ii	89.68 (5)	N—C2—C1	111.85 (12)
O1W—Co—O1^iii	89.68 (5)	N—C2—H1C	110.4 (15)
O1W^i—Co—O1^iii	90.32 (5)	C1—C2—H1C	110.9 (15)
O1^ii—Co—O1^iii	180.00 (4)	N—C2—H2C	108.0 (14)
O1W—Co—O2^i	91.14 (6)	C1—C2—H2C	106.0 (14)
O1W^i—Co—O2^i	88.86 (6)	H1C—C2—H2C	109 (2)
O1^ii—Co—O2^i	86.44 (5)	C2—N—H1N	109.0 (15)
O1^iii—Co—O2^i	93.56 (5)	C2—N—H2N	108.7 (14)
O1W—Co—O2	88.86 (6)	H1N—N—H2N	107 (2)
O1W^i—Co—O2	91.14 (6)	C2—N—H3N	111.7 (17)
O1^ii—Co—O2	93.56 (5)	H1N—N—H3N	114 (2)
O1^iii—Co—O2	86.44 (5)	H2N—N—H3N	107 (2)
O2^i—Co—O2	180.0	Co—O1W—H1W	126 (2)
C1—O1—Co^iv	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)

D—H···A	D—H	H···A	D···A	D—H···A
N—H1N···Cl^v	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···Cl^v	0.90 (3)	2.41 (3)	3.2905 (17)	163 (2)
O1W—H1W···Cl^vi	0.79 (3)	2.38 (3)	3.1457 (17)	167 (3)
O1W—H2W···O2^ii	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.