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Acta Cryst. (2006). C62, m22-m26
https://doi.org/10.1107/S0108270105040606
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Compounds of glycine with metal sulfates and thio­sulfates: glycine cobalt sulfate penta­hydrate, glycine sodium thio­sulfate dihydrate and glycine potassium thio­sulfate

M. Fleck and L. Bohatý
In the crystal structures of the title compounds, hexa­aqua­cobalt(II) tetra­aqua­diglycinato­cobalt(II) bis(sulfate), [Co(H2O)6][Co(C2H5NO2)2(H2O)4](SO4)2, (I), poly[diaqua-μ3-glycinato-di-μ4-thio­sulfato-tetra­sodium(I)], [Na4(C2H5NO2)(S2O3)2(H2O)2]n, (II), and poly[μ2-glycinato-μ4-thio­sulfato-dipotassium(I)], [K2(C2H5NO2)(S2O3)]n, (III), all atoms are located on general positions, except the Co atoms in (I), which are located on inversion centres. In (I), hydrogen bonds play an important role, while the alkali thio­sulfate compounds are characterized by three-dimensional frameworks of polyhedra. Relations to other compounds of glycine and metal sulfates are commented on.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105040606/fg3001sup1.cif
Contains datablocks global, I, II, III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105040606/fg3001Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105040606/fg3001IIsup3.hkl
Contains datablock glynaso

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105040606/fg3001IIIsup4.hkl
Contains datablock glykso2

CCDC references: 296329; 296330; 296331

Comment top

During our studies of new compounds of glycine with inorganic salts (Fleck & Bohatý, 2005a,b,c), we have examined the group of glycine metal sulfates and thiosulfates. Two such compounds we have reported previously, namely glycine lithium sulfate, [Li2(SO4)(C2H5NO2)]n, and glycine zinc sulfate trihydrate, [Zn(SO4)(C2H5NO2)(H2O)3]n (Fleck & Bohatý, 2004). Only two members of this group have been described in the literature previous to our studies. These are glycinium ammonium sulfate, (C2H6NO2)(NH4)SO4 (Vilminot et al., 1974) and glycine nickel sulfate hexahydrate, [Ni(C2H5NO2)(H2O)5]SO4·H2O (Peterková et al., 1991). No glycine thiosulfate compounds have been reported to date. In the present paper, we present three new members of this group.

The crystal structure of compound (I) is characterized by two different, isolated [CoO6] octahedra. Atoms Co1 and Co2 are both located on inversion centres; for both atoms, the coordination is more or less octahedral. While all the ligands around atom Co1 are O atoms of water molecules (2 × OW1, 2 × OW2, 2 × OW3) with Co—O distances of between 2.0487 (10) and 2.1333 (11) Å, atom Co2 is surrounded by the O atoms of water molecules (2 × OW4 and 2 × OW5) as well as O atoms of the acid group of the glycine molecule (atom O2) with Co—O distances of between 2.0358 (11) and 2.1404 (10) Å. Thus, two glycine molecules are attached to each Co2 octahedron, forming a [Co(H2O)4(C2H5NO2)2] cluster. The sulfate tetrahedra are located in the interstices between these isolated groups. Consequently, the crystal structure can be considered as being composed of isolated units (Co1–water octahedra, Co2–water–glycine clusters and sulfate tetrahedra) that are connected to each other only by hydrogen bonds (Fig. 4).

In compound (II) there are four crystallographically different sodium positions. The Na atoms are coordinated by O and (in the case of atoms Na1 and Na4) S atoms; the coordination polyhedra are irregular. The Na—O distances range from 2.3359 (16) to 2.4765 (14) Å for Na1, from 2.3331 (12) to 2.9590 (19) Å for Na2, from 2.3526 (12) to 2.6736 (16) Å for Na3 and from 2.3883 (17) to 2.6930 (15) Å for Na4. The Na—S distances are 2.8990 (10) Å for Na1 and 3.0135 (10) Å for Na4. Bond-valence sums have been calculated and show that Na1 is slightly oversaturated, while the values for the other Na atoms are very close to the expected value of 1. The polyhedra share common corners and edges, thus forming sheets parallel to (100). These sheets are connected by thiosulfate groups into a three-dimensional framework. It is interesting to note that this framework leaves channels parallel to [010] in which there is virtually no electron density (the negligible electron density remaining after the refinement is mostly close to the O and S atoms). The glycine molecules are connected to the Na cations via the carboxlate O atoms and reach into the channels but do not fill them (Fig. 5). The remaining channels are rather large (diameter approximately 3.5 Å).

The main structural elements of compound (III) are the coordination polyhedra of the two crystallographically different K atoms. Atom K1 is eightfold coordinated; the polyhedron resembles an irregular hexagonal bipyramid. All ligands are O atoms with K—O distances of between 2.6225 (11) and 3.2050 (15) Å. In the case of atom K2, there is a sixfold coordination in the form of a distorted trigonal prism, the ligands being four O atoms and two S atoms, with K—O distances of between 2.6940 (12) and 2.8732 (12) Å, and K—S-distances of 3.1527 (9) and 3.1887 (10) Å. The calculation of bond-valence sums yields values slightly exceding the ideal value of 1 for both K atoms. The [K1O8] bipyramids share common faces and thus form a chain parallel to [001]. By sharing common corners, these chains are further connected to layers parallel to (010). These layers are again connected by the [K2O4S2] prisms to form a three-dimensional framework. The terminal O and S atoms of thiosulfate groups and glycine molecules act as ligands for this polyhedral framework. As in the case of (II), empty channels remain in the structure (parallel to [100]), although they are smaller in diameter (about 2.9 Å) (Fig. 6). As in (II), there is no significant electron density remaining in the channels.

As is usually the case for compounds of glycine with inorganic salts, the glycine molecules exist in the zwitterionic form, [H3N+CH2COO-], in all three compounds. However, there are examples of glycinium sulfates, for example triglycine sulfate (Matthias et al., 1956), which has been studied intensively because of its interesting physical properties, such as ferroelectricity. The conformation of the glycine molecules is similar in all three title compounds: The molecules are nearly planar (as far as the non-H atoms are concerned), the O1—C1—C2—N3 torsion angles are -178.92 (3), 174.23 (2) and 175.01 (1)° in compounds (I), (II) and (III), respectively. These angles are in good agreement with the values usually found in salts of glycine and inorganic compounds; perfectly planar molecules are very rare (as in glycine magnesium dichloride tetrahydrate; Fleck & Bohatý, 2005b). In addition, all the distances within the carboxylate groups are within the range of the values usually found [the C—O1 and C—O2 distances for compounds (I), (II) and (III) are 1.2328 (15) and 1.2714 (14), 1.2467 (18) and 1.2574 (19), and 1.2483 (16) and 1.2506 (17) Å, respectively). The role of the glycine molecule as a ligand is different in all three compounds. The molecule acts as a monodentate ligand in (I), as a bidentate ligand in (II) and as a bridging ligand in (III).

Remarkably, all the reported glycine metal sulfate and thiosulfate compounds are structurally different. This can be deduced from a quick comparison of the unit-cell parameters (see Table 1). When examining the atomic arrangements of these compounds, the structural diversity becomes obvious: glycine lithium sulfate, [Li2(SO4)(C2H5NO2)]n (Fleck & Bohatý, 2004), is mainly composed of tetrahedral sheets (made of SO4– and LiO4 tetrahedra). The structure of glycine zinc sulfate trihydrate, [Zn(SO4)(C2H5NO2)(H2O)3]n (Fleck & Bohatý, 2004), is made up of [O3SOZnO5] clusters. These clusters are linked by glycine molecules into zigzag chains. In glycinium ammonium sulfate, (C2H6NO2)(NH4)SO4 (Vilminot et al., 1974), all building units (glycinium ions, ammonium ions and sulfate groups) are isolated, connected only by hydrogen bonds. The connectivity in glycine nickel sulfate hexahydrate, [Ni(C2H5NO2)(H2O)5]SO4·H2O (Peterková et al., 1991), is again different: the Ni cations are octahedrally coordinated by five O atoms from water molecules and one from a glycine molecule. Thus, isolated [Ni(H2O)5(C2H5NO2)] clusters exist, which are connected by hydrogen bonds to the sulfate tetrahedra and non-coordinating water molecules.

Experimental top

For the syntheses of the title compounds, a stoichiometric mixture of glycine and the respective metal suphate or thiosulfate was dissolved in water. The solutions were evaporated slowly at a temperature of approximately 295 K over a period of several weeks. The syntheses yielded small crystals up to a size of several mm. The crystals of the Co compound were red; those of the Na and K compounds were colourless.

Structure description top

During our studies of new compounds of glycine with inorganic salts (Fleck & Bohatý, 2005a,b,c), we have examined the group of glycine metal sulfates and thiosulfates. Two such compounds we have reported previously, namely glycine lithium sulfate, [Li2(SO4)(C2H5NO2)]n, and glycine zinc sulfate trihydrate, [Zn(SO4)(C2H5NO2)(H2O)3]n (Fleck & Bohatý, 2004). Only two members of this group have been described in the literature previous to our studies. These are glycinium ammonium sulfate, (C2H6NO2)(NH4)SO4 (Vilminot et al., 1974) and glycine nickel sulfate hexahydrate, [Ni(C2H5NO2)(H2O)5]SO4·H2O (Peterková et al., 1991). No glycine thiosulfate compounds have been reported to date. In the present paper, we present three new members of this group.

The crystal structure of compound (I) is characterized by two different, isolated [CoO6] octahedra. Atoms Co1 and Co2 are both located on inversion centres; for both atoms, the coordination is more or less octahedral. While all the ligands around atom Co1 are O atoms of water molecules (2 × OW1, 2 × OW2, 2 × OW3) with Co—O distances of between 2.0487 (10) and 2.1333 (11) Å, atom Co2 is surrounded by the O atoms of water molecules (2 × OW4 and 2 × OW5) as well as O atoms of the acid group of the glycine molecule (atom O2) with Co—O distances of between 2.0358 (11) and 2.1404 (10) Å. Thus, two glycine molecules are attached to each Co2 octahedron, forming a [Co(H2O)4(C2H5NO2)2] cluster. The sulfate tetrahedra are located in the interstices between these isolated groups. Consequently, the crystal structure can be considered as being composed of isolated units (Co1–water octahedra, Co2–water–glycine clusters and sulfate tetrahedra) that are connected to each other only by hydrogen bonds (Fig. 4).

In compound (II) there are four crystallographically different sodium positions. The Na atoms are coordinated by O and (in the case of atoms Na1 and Na4) S atoms; the coordination polyhedra are irregular. The Na—O distances range from 2.3359 (16) to 2.4765 (14) Å for Na1, from 2.3331 (12) to 2.9590 (19) Å for Na2, from 2.3526 (12) to 2.6736 (16) Å for Na3 and from 2.3883 (17) to 2.6930 (15) Å for Na4. The Na—S distances are 2.8990 (10) Å for Na1 and 3.0135 (10) Å for Na4. Bond-valence sums have been calculated and show that Na1 is slightly oversaturated, while the values for the other Na atoms are very close to the expected value of 1. The polyhedra share common corners and edges, thus forming sheets parallel to (100). These sheets are connected by thiosulfate groups into a three-dimensional framework. It is interesting to note that this framework leaves channels parallel to [010] in which there is virtually no electron density (the negligible electron density remaining after the refinement is mostly close to the O and S atoms). The glycine molecules are connected to the Na cations via the carboxlate O atoms and reach into the channels but do not fill them (Fig. 5). The remaining channels are rather large (diameter approximately 3.5 Å).

The main structural elements of compound (III) are the coordination polyhedra of the two crystallographically different K atoms. Atom K1 is eightfold coordinated; the polyhedron resembles an irregular hexagonal bipyramid. All ligands are O atoms with K—O distances of between 2.6225 (11) and 3.2050 (15) Å. In the case of atom K2, there is a sixfold coordination in the form of a distorted trigonal prism, the ligands being four O atoms and two S atoms, with K—O distances of between 2.6940 (12) and 2.8732 (12) Å, and K—S-distances of 3.1527 (9) and 3.1887 (10) Å. The calculation of bond-valence sums yields values slightly exceding the ideal value of 1 for both K atoms. The [K1O8] bipyramids share common faces and thus form a chain parallel to [001]. By sharing common corners, these chains are further connected to layers parallel to (010). These layers are again connected by the [K2O4S2] prisms to form a three-dimensional framework. The terminal O and S atoms of thiosulfate groups and glycine molecules act as ligands for this polyhedral framework. As in the case of (II), empty channels remain in the structure (parallel to [100]), although they are smaller in diameter (about 2.9 Å) (Fig. 6). As in (II), there is no significant electron density remaining in the channels.

As is usually the case for compounds of glycine with inorganic salts, the glycine molecules exist in the zwitterionic form, [H3N+CH2COO-], in all three compounds. However, there are examples of glycinium sulfates, for example triglycine sulfate (Matthias et al., 1956), which has been studied intensively because of its interesting physical properties, such as ferroelectricity. The conformation of the glycine molecules is similar in all three title compounds: The molecules are nearly planar (as far as the non-H atoms are concerned), the O1—C1—C2—N3 torsion angles are -178.92 (3), 174.23 (2) and 175.01 (1)° in compounds (I), (II) and (III), respectively. These angles are in good agreement with the values usually found in salts of glycine and inorganic compounds; perfectly planar molecules are very rare (as in glycine magnesium dichloride tetrahydrate; Fleck & Bohatý, 2005b). In addition, all the distances within the carboxylate groups are within the range of the values usually found [the C—O1 and C—O2 distances for compounds (I), (II) and (III) are 1.2328 (15) and 1.2714 (14), 1.2467 (18) and 1.2574 (19), and 1.2483 (16) and 1.2506 (17) Å, respectively). The role of the glycine molecule as a ligand is different in all three compounds. The molecule acts as a monodentate ligand in (I), as a bidentate ligand in (II) and as a bridging ligand in (III).

Remarkably, all the reported glycine metal sulfate and thiosulfate compounds are structurally different. This can be deduced from a quick comparison of the unit-cell parameters (see Table 1). When examining the atomic arrangements of these compounds, the structural diversity becomes obvious: glycine lithium sulfate, [Li2(SO4)(C2H5NO2)]n (Fleck & Bohatý, 2004), is mainly composed of tetrahedral sheets (made of SO4– and LiO4 tetrahedra). The structure of glycine zinc sulfate trihydrate, [Zn(SO4)(C2H5NO2)(H2O)3]n (Fleck & Bohatý, 2004), is made up of [O3SOZnO5] clusters. These clusters are linked by glycine molecules into zigzag chains. In glycinium ammonium sulfate, (C2H6NO2)(NH4)SO4 (Vilminot et al., 1974), all building units (glycinium ions, ammonium ions and sulfate groups) are isolated, connected only by hydrogen bonds. The connectivity in glycine nickel sulfate hexahydrate, [Ni(C2H5NO2)(H2O)5]SO4·H2O (Peterková et al., 1991), is again different: the Ni cations are octahedrally coordinated by five O atoms from water molecules and one from a glycine molecule. Thus, isolated [Ni(H2O)5(C2H5NO2)] clusters exist, which are connected by hydrogen bonds to the sulfate tetrahedra and non-coordinating water molecules.

Computing details top

For all compounds, data collection: Collect (Nonius, 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; Farrugia 1997) for (I); SHELXL97 (Sheldrick, 1997; Farrugia, 1997) for (II); SHELXL97 (Sheldrick, 1997, Farrugia 1997) for (III). For all compounds, molecular graphics: DIAMOND (Version 2.1; Bergerhoff et al., 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. : The connectivity in (I), shown with displacement ellipsoids at the 50% probability level for all non-H atoms and at the 20% level for all H atoms. [Symmetry codes: (i) -x + 1, -y + 1, -z + 1; (ii) -x + 1, -y, -z.] (DIAMOND; Bergerhoff et al., 1997.)
[Figure 2] Fig. 2. : The connectivity in (II), shown as in Fig. 1. [Symmetry codes: (i) x + 1/2, y + 1/2, z; (ii) -x + 1/2, y + 1/2, -z + 1/2; (iii) -x, -y, -z; (iv) x, -y + 1, z - 1/2; (v) -x + 1/2, y - 1/2, -z + 1/2; (vi) -x, -y + 1, -z; (vii) x, - y - 1, z.]
[Figure 3] Fig. 3. : The connectivity in (III), shown as in Fig. 1. [Symmetry codes: (i) x, -y + 1/2, z - 1/2; (ii) x + 1, -y + 1/2, z - 1/2; (iii) x + 1, y, z; (iv) - x + 1, -y + 1, -z + 1; (v) x, y, z - 1.]
[Figure 4] Fig. 4. : A packing diagram of the structure of (I), viewed along [010]. M—O polyhedra (blue in the online version of the journal) and sulfate/thiosulfate tetrahedra (yellow online) are shaded; the glycine molecules are shown in a ball-and-stick representation.
[Figure 5] Fig. 5. : A packing diagram of the structure of (II), viewed along [010]; colours as in Fig. 4. Note the channels in the viewing direction.
[Figure 6] Fig. 6. : A packing diagram of the structure of (II), viewed along [100]; colours as in Fig. 4. Note the channels in the viewing direction.
(I) hexaaquacobalt(II) tetraaquadiglycinatocobalt(II) sulfate top
Crystal data top
[Co(H2O)6][Co(C2H5NO2)2(H2O)4](SO4)2Z = 1
Mr = 640.28F(000) = 330
Triclinic, P1Dx = 2.004 Mg m−3
a = 5.970 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 6.775 (1) ÅCell parameters from 2894 reflections
c = 13.335 (3) Åθ = 4.9–29.8°
α = 85.23 (3)°µ = 1.87 mm−1
β = 83.31 (3)°T = 293 K
γ = 83.22 (3)°Fragment, red
V = 530.62 (17) Å30.40 × 0.35 × 0.30 mm
Data collection top
Nonius KappaCCD
diffractometer		3191 independent reflections
Radiation source: fine-focus sealed tube3036 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.014
Detector resolution: 9 pixels mm-1θmax = 30.5°, θmin = 4.2°
ω scansh = −8→8
Absorption correction: multi-scan
(Otwinowski & Minor, 1997)		k = −9→9
Tmin = 0.479, Tmax = 0.571l = −19→19
5847 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.020H-atom parameters constrained
wR(F2) = 0.052 w = 1/[σ2(Fo2) + (0.0202P)2 + 0.2124P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
3191 reflectionsΔρmax = 0.46 e Å−3
209 parametersΔρmin = −0.43 e Å−3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.076 (4)
Crystal data top
[Co(H2O)6][Co(C2H5NO2)2(H2O)4](SO4)2γ = 83.22 (3)°
Mr = 640.28V = 530.62 (17) Å3
Triclinic, P1Z = 1
a = 5.970 (1) ÅMo Kα radiation
b = 6.775 (1) ŵ = 1.87 mm−1
c = 13.335 (3) ÅT = 293 K
α = 85.23 (3)°0.40 × 0.35 × 0.30 mm
β = 83.31 (3)°
Data collection top
Nonius KappaCCD
diffractometer		3191 independent reflections
Absorption correction: multi-scan
(Otwinowski & Minor, 1997)		3036 reflections with I > 2σ(I)
Tmin = 0.479, Tmax = 0.571Rint = 0.014
5847 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0200 restraints
wR(F2) = 0.052H-atom parameters constrained
S = 1.06Δρmax = 0.46 e Å−3
3191 reflectionsΔρmin = −0.43 e Å−3
209 parameters
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 303 frames with phi- and omega-increments of 1 degree and a counting time of 50 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 0.028.

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
xyzUiso*/Ueq
Co10.50000.00000.00000.01566 (6)
O1W0.54763 (15)0.23385 (14)0.08030 (9)0.0351 (2)
H1W10.46300.32390.09020.042*
H2W10.66800.24990.09230.042*
O2W0.20748 (14)0.15817 (13)−0.05029 (7)0.02450 (17)
H1W20.21800.2500−0.09080.029*
H2W20.11900.1960−0.00070.029*
O3W0.29385 (15)−0.10454 (13)0.13058 (7)0.02451 (17)
H1W30.2561−0.22000.13170.029*
H2W30.1791−0.02800.14370.029*
Co20.50000.50000.50000.01567 (6)
O10.97249 (16)0.82634 (18)0.38482 (9)0.0405 (3)
O20.64348 (15)0.77729 (13)0.47608 (6)0.02304 (17)
O4W0.19176 (14)0.65457 (15)0.53687 (7)0.02818 (19)
H1W40.11410.69600.49210.034*
H2W40.10710.63900.58880.034*
O5W0.43859 (14)0.53851 (14)0.34563 (6)0.02478 (18)
H1W50.54200.53000.30100.030*
H2W50.33500.49400.32820.030*
N10.39389 (18)0.99860 (17)0.34518 (8)0.0264 (2)
H1N0.36601.04200.40930.032*
H2N0.33900.89000.34210.032*
H3N0.32501.08300.30570.032*
C10.76362 (19)0.84857 (17)0.39963 (9)0.0206 (2)
C20.6424 (2)0.97830 (19)0.31948 (9)0.0244 (2)
H1C0.69501.10930.31290.029*
H2C0.67990.92000.25480.029*
S10.01339 (4)0.41135 (4)0.187221 (19)0.01505 (6)
O1S0.09684 (15)0.34647 (14)0.28635 (7)0.02613 (18)
O2S0.18447 (15)0.51719 (13)0.12291 (7)0.02591 (18)
O3S−0.02773 (14)0.23353 (13)0.13789 (7)0.02426 (17)
O4S−0.20125 (14)0.54266 (13)0.20217 (7)0.02488 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.01402 (9)0.01463 (10)0.01847 (10)−0.00038 (7)−0.00293 (7)−0.00207 (7)
O1W0.0186 (4)0.0282 (5)0.0628 (7)0.0016 (3)−0.0108 (4)−0.0249 (5)
O2W0.0217 (4)0.0266 (4)0.0226 (4)0.0065 (3)−0.0023 (3)0.0010 (3)
O3W0.0236 (4)0.0209 (4)0.0279 (4)−0.0032 (3)0.0012 (3)−0.0002 (3)
Co20.01228 (9)0.01925 (10)0.01489 (10)−0.00075 (7)−0.00090 (7)0.00010 (7)
O10.0175 (4)0.0558 (7)0.0442 (6)−0.0010 (4)−0.0030 (4)0.0159 (5)
O20.0257 (4)0.0229 (4)0.0206 (4)−0.0060 (3)−0.0016 (3)0.0017 (3)
O4W0.0168 (4)0.0392 (5)0.0248 (4)0.0060 (3)0.0014 (3)0.0016 (4)
O5W0.0186 (4)0.0398 (5)0.0170 (4)−0.0077 (3)−0.0014 (3)−0.0027 (3)
N10.0225 (5)0.0293 (5)0.0268 (5)0.0026 (4)−0.0076 (4)0.0012 (4)
C10.0195 (5)0.0202 (5)0.0222 (5)−0.0029 (4)−0.0034 (4)0.0006 (4)
C20.0222 (5)0.0272 (6)0.0229 (5)−0.0029 (4)−0.0030 (4)0.0044 (4)
S10.01277 (11)0.01520 (11)0.01667 (12)−0.00067 (8)−0.00031 (8)−0.00108 (9)
O1S0.0259 (4)0.0316 (5)0.0207 (4)0.0007 (3)−0.0070 (3)0.0001 (3)
O2S0.0213 (4)0.0195 (4)0.0343 (5)−0.0044 (3)0.0083 (3)0.0004 (3)
O3S0.0220 (4)0.0224 (4)0.0300 (4)−0.0045 (3)−0.0024 (3)−0.0089 (3)
O4S0.0183 (4)0.0264 (4)0.0260 (4)0.0066 (3)0.0036 (3)0.0005 (3)
Geometric parameters (Å, º) top
Co1—O1W2.0487 (10)O1—C11.2328 (15)
Co1—O1Wi2.0487 (10)O2—C11.2714 (14)
Co1—O2Wi2.0879 (10)O4W—H1W40.8103
Co1—O2W2.0879 (10)O4W—H2W40.8155
Co1—O3W2.1330 (11)O5W—H1W50.8064
Co1—O3Wi2.1330 (11)O5W—H2W50.7851
O1W—H1W10.7552N1—C21.4758 (16)
O1W—H2W10.7762N1—H1N0.9178
O2W—H1W20.7925N1—H2N0.8460
O2W—H2W20.8350N1—H3N0.8474
O3W—H1W30.8377C1—C21.5207 (17)
O3W—H2W30.8199C2—H1C0.9700
Co2—O4Wii2.0358 (11)C2—H2C0.9700
Co2—O4W2.0358 (11)S1—O2S1.4695 (10)
Co2—O5W2.1222 (10)S1—O4S1.4744 (10)
Co2—O5Wii2.1222 (10)S1—O3S1.4776 (9)
Co2—O2ii2.1404 (10)S1—O1S1.4812 (10)
Co2—O22.1404 (10)
O1W—Co1—O1Wi180.00 (5)O4Wii—Co2—O291.30 (4)
O1W—Co1—O2Wi89.46 (4)O4W—Co2—O288.70 (4)
O1Wi—Co1—O2Wi90.54 (4)O5W—Co2—O286.75 (4)
O1W—Co1—O2W90.54 (4)O5Wii—Co2—O293.25 (4)
O1Wi—Co1—O2W89.46 (4)O2ii—Co2—O2180.0
O2Wi—Co1—O2W180.00 (6)C1—O2—Co2130.14 (8)
O1W—Co1—O3W87.26 (5)Co2—O4W—H1W4118.9
O1Wi—Co1—O3W92.74 (5)Co2—O4W—H2W4127.0
O2Wi—Co1—O3W91.92 (4)H1W4—O4W—H2W4107.6
O2W—Co1—O3W88.08 (4)Co2—O5W—H1W5120.9
O1W—Co1—O3Wi92.74 (5)Co2—O5W—H2W5119.7
O1Wi—Co1—O3Wi87.26 (5)H1W5—O5W—H2W5108.6
O2Wi—Co1—O3Wi88.08 (4)C2—N1—H1N106.7
O2W—Co1—O3Wi91.92 (4)C2—N1—H2N112.0
O3W—Co1—O3Wi180.00 (3)H1N—N1—H2N111.1
Co1—O1W—H1W1125.8C2—N1—H3N112.9
Co1—O1W—H2W1120.7H1N—N1—H3N108.1
H1W1—O1W—H2W1111.9H2N—N1—H3N106.1
Co1—O2W—H1W2119.8O1—C1—O2126.01 (11)
Co1—O2W—H2W2109.6O1—C1—C2115.98 (11)
H1W2—O2W—H2W2108.2O2—C1—C2117.98 (10)
Co1—O3W—H1W3117.6N1—C2—C1111.74 (10)
Co1—O3W—H2W3112.3N1—C2—H1C109.3
H1W3—O3W—H2W3108.3C1—C2—H1C109.3
O4Wii—Co2—O4W180.000 (1)N1—C2—H2C109.3
O4Wii—Co2—O5W91.13 (5)C1—C2—H2C109.3
O4W—Co2—O5W88.87 (5)H1C—C2—H2C107.9
O4Wii—Co2—O5Wii88.87 (5)O2S—S1—O4S110.05 (6)
O4W—Co2—O5Wii91.13 (5)O2S—S1—O3S109.46 (6)
O5W—Co2—O5Wii180.0O4S—S1—O3S108.97 (6)
O4Wii—Co2—O2ii88.70 (4)O2S—S1—O1S109.69 (6)
O4W—Co2—O2ii91.30 (4)O4S—S1—O1S109.87 (6)
O5W—Co2—O2ii93.25 (4)O3S—S1—O1S108.79 (6)
O5Wii—Co2—O2ii86.75 (4)
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, −y+1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2S0.762.022.7605 (16)167
O1W—H2W1···O3Siii0.781.972.7329 (14)168
O2W—H1W2···O4Siv0.791.962.7438 (15)170
O2W—H2W2···O3S0.841.972.7843 (15)164
O3W—H1W3···O2Sv0.841.902.7311 (13)175
O3W—H2W3···O3S0.822.042.8101 (15)157
O4W—H1W4···O1vi0.811.852.6543 (16)170
O4W—H2W4···O1Svii0.821.952.7531 (16)170
O5W—H1W5···O4Siii0.811.912.7075 (15)172
O5W—H2W5···O1S0.791.992.7666 (14)172
N1—H1N···O2viii0.922.032.9042 (16)159
N1—H2N···O1vi0.852.282.8725 (17)128
N1—H2N···O5W0.852.383.0966 (15)142
N1—H3N···O1Six0.852.132.8887 (16)149
Symmetry codes: (iii) x+1, y, z; (iv) −x, −y+1, −z; (v) x, y−1, z; (vi) x−1, y, z; (vii) −x, −y+1, −z+1; (viii) −x+1, −y+2, −z+1; (ix) x, y+1, z.
(II) poly[diaqua-µ3-glycinato-di-µ4-thiosulfato-thiosulfatotetrasodium(I) top
Crystal data top
[Na4(C2H5NO2)(S2O3)2(H2O)2]F(000) = 1728
Mr = 427.30Dx = 1.964 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 17.775 (4) ÅCell parameters from 2906 reflections
b = 7.311 (1) Åθ = 4.9–26.8°
c = 22.595 (5) ŵ = 0.82 mm−1
β = 100.10 (3)°T = 293 K
V = 2890.8 (10) Å3Prism, colourless
Z = 80.20 × 0.10 × 0.08 mm
Data collection top
Nonius KappaCCD
diffractometer		3292 independent reflections
Radiation source: fine-focus sealed tube2966 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
Detector resolution: 9 pixels mm-1θmax = 27.5°, θmin = 4.2°
ω scansh = −20→22
Absorption correction: multi-scan
(Otwinowski & Minor, 1997)		k = −8→9
Tmin = 0.852, Tmax = 0.936l = −29→29
10482 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025All H-atom parameters refined
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0309P)2 + 3.48P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
3292 reflectionsΔρmax = 0.33 e Å−3
227 parametersΔρmin = −0.42 e Å−3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0013 (2)
Crystal data top
[Na4(C2H5NO2)(S2O3)2(H2O)2]V = 2890.8 (10) Å3
Mr = 427.30Z = 8
Monoclinic, C2/cMo Kα radiation
a = 17.775 (4) ŵ = 0.82 mm−1
b = 7.311 (1) ÅT = 293 K
c = 22.595 (5) Å0.20 × 0.10 × 0.08 mm
β = 100.10 (3)°
Data collection top
Nonius KappaCCD
diffractometer		3292 independent reflections
Absorption correction: multi-scan
(Otwinowski & Minor, 1997)		2966 reflections with I > 2σ(I)
Tmin = 0.852, Tmax = 0.936Rint = 0.020
10482 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0250 restraints
wR(F2) = 0.065All H-atom parameters refined
S = 1.04Δρmax = 0.33 e Å−3
3292 reflectionsΔρmin = −0.42 e Å−3
227 parameters
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 537 frames with phi- and omega-increments of 1 degree and a counting time of 15 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 0.028.

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
xyzUiso*/Ueq
Na10.25913 (4)0.91930 (9)0.25729 (3)0.02457 (15)
Na20.12801 (4)0.50352 (9)0.01748 (3)0.02565 (15)
Na30.13464 (4)0.00234 (9)0.01793 (3)0.02672 (15)
Na40.30292 (4)0.72979 (11)0.11821 (3)0.03851 (19)
S1A0.20069 (2)0.79607 (5)0.418024 (16)0.02016 (10)
S2A0.14715 (2)0.85596 (6)0.334142 (16)0.02408 (11)
O11A0.25729 (8)0.6516 (2)0.41573 (6)0.0453 (4)
O12A0.14236 (6)0.73716 (15)0.45257 (5)0.0237 (2)
O13A0.23671 (7)0.96536 (18)0.44458 (5)0.0349 (3)
S1B−0.01070 (2)0.25995 (5)0.081267 (17)0.01841 (10)
S2B0.00715 (2)0.24132 (6)0.170702 (19)0.03007 (12)
O11B0.02744 (8)0.10657 (17)0.05707 (6)0.0376 (3)
O12B−0.09356 (7)0.25188 (18)0.05774 (5)0.0325 (3)
O13B0.02017 (8)0.43232 (17)0.06254 (6)0.0386 (3)
O10.20722 (6)0.68746 (16)0.18107 (5)0.0250 (2)
O20.15005 (6)0.76264 (14)0.08848 (5)0.0219 (2)
C10.15013 (8)0.72934 (18)0.14309 (7)0.0173 (3)
C20.07511 (9)0.7411 (2)0.16640 (7)0.0234 (3)
H1C0.0653 (11)0.633 (3)0.1834 (9)0.031 (5)*
H2C0.0769 (12)0.842 (3)0.1948 (10)0.038 (6)*
N30.00993 (8)0.7727 (2)0.11775 (7)0.0252 (3)
H1N0.0181 (13)0.864 (4)0.0971 (11)0.047 (7)*
H2N−0.0280 (15)0.795 (3)0.1324 (11)0.043 (6)*
H3N0.0038 (11)0.679 (3)0.0939 (9)0.027 (5)*
O1W0.18642 (7)1.14291 (18)0.19280 (6)0.0276 (3)
H1W10.1995 (13)1.147 (3)0.1591 (11)0.041 (6)*
H2W10.1441 (16)1.165 (4)0.1882 (11)0.053 (8)*
O2W0.35473 (8)0.9307 (2)0.19842 (7)0.0350 (3)
H1W20.3943 (17)0.896 (4)0.1991 (13)0.066 (9)*
H2W20.3567 (18)1.042 (5)0.1862 (14)0.086 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0258 (3)0.0253 (3)0.0229 (3)−0.0003 (3)0.0050 (2)−0.0012 (2)
Na20.0291 (3)0.0236 (3)0.0249 (3)0.0003 (3)0.0066 (2)−0.0037 (2)
Na30.0349 (4)0.0232 (3)0.0234 (3)0.0022 (3)0.0091 (3)0.0039 (2)
Na40.0373 (4)0.0477 (5)0.0347 (4)−0.0104 (3)0.0179 (3)−0.0134 (3)
S1A0.01589 (18)0.0289 (2)0.01619 (18)0.00394 (14)0.00418 (13)0.00385 (14)
S2A0.01984 (19)0.0343 (2)0.01817 (18)0.00332 (15)0.00345 (13)0.00555 (15)
O11A0.0428 (8)0.0689 (10)0.0255 (6)0.0383 (7)0.0099 (5)0.0091 (6)
O12A0.0235 (6)0.0287 (6)0.0201 (5)−0.0031 (4)0.0069 (4)0.0047 (4)
O13A0.0312 (6)0.0404 (7)0.0294 (6)−0.0153 (5)−0.0050 (5)0.0083 (5)
S1B0.01865 (18)0.01649 (18)0.02108 (19)0.00057 (13)0.00617 (14)−0.00032 (13)
S2B0.0241 (2)0.0444 (3)0.0211 (2)0.00520 (17)0.00230 (15)−0.00188 (16)
O11B0.0543 (8)0.0284 (6)0.0348 (7)0.0158 (6)0.0205 (6)−0.0007 (5)
O12B0.0219 (6)0.0490 (8)0.0252 (6)−0.0012 (5)−0.0003 (5)0.0034 (5)
O13B0.0525 (8)0.0251 (6)0.0430 (7)−0.0118 (6)0.0216 (6)0.0013 (5)
O10.0191 (5)0.0305 (6)0.0237 (6)0.0030 (5)−0.0010 (4)0.0018 (5)
O20.0238 (6)0.0228 (5)0.0194 (5)0.0022 (4)0.0053 (4)0.0027 (4)
C10.0182 (7)0.0136 (6)0.0199 (7)−0.0007 (5)0.0029 (5)−0.0018 (5)
C20.0201 (8)0.0271 (8)0.0237 (8)0.0002 (6)0.0055 (6)0.0015 (6)
N30.0148 (6)0.0284 (8)0.0323 (8)0.0012 (5)0.0035 (6)−0.0014 (6)
O1W0.0210 (6)0.0368 (7)0.0251 (6)0.0006 (5)0.0039 (5)0.0017 (5)
O2W0.0275 (7)0.0336 (7)0.0460 (8)0.0012 (6)0.0125 (6)0.0004 (6)
Geometric parameters (Å, º) top
Na1—O2W2.3359 (16)S1A—O12A1.4676 (12)
Na1—O1W2.4095 (15)S1A—O13A1.4721 (13)
Na1—O1i2.4185 (13)S1A—S2A2.0142 (8)
Na1—O1Wii2.4308 (15)S1A—Na3viii3.0944 (10)
Na1—O12.4765 (14)S1A—Na4i3.2727 (10)
Na1—S2A2.8990 (10)S2A—Na4i3.0135 (10)
Na2—O12Aiii2.3331 (12)O11A—Na3i2.4735 (16)
Na2—O13B2.3803 (15)O12A—Na2viii2.3331 (13)
Na2—O13Aii2.4233 (15)O12A—Na3viii2.4285 (13)
Na2—O22.4689 (13)O13A—Na2i2.4233 (15)
Na2—O12Biv2.4692 (14)O13A—Na4i2.4281 (15)
Na2—O13Biv2.9590 (19)O13A—Na3viii2.6736 (16)
Na2—S1Biv3.2687 (11)S1B—O11B1.4649 (12)
Na3—O2v2.3526 (12)S1B—O13B1.4662 (12)
Na3—O11B2.3633 (15)S1B—O12B1.4767 (13)
Na3—O12Aiii2.4285 (13)S1B—S2B1.9945 (7)
Na3—O11Aii2.4735 (16)O1—C11.2467 (18)
Na3—O12Bvi2.5442 (15)O2—C11.2574 (19)
Na3—O13Aiii2.6736 (16)C1—C21.520 (2)
Na3—S1Aiii3.0944 (9)C2—N31.469 (2)
Na4—O2W2.3883 (17)C2—H1C0.91 (2)
Na4—O12.4196 (15)C2—H2C0.97 (2)
Na4—O13Aii2.4281 (15)N3—H1N0.84 (3)
Na4—O12Bvii2.4820 (16)N3—H2N0.82 (3)
Na4—O22.6930 (15)N3—H3N0.87 (2)
Na4—C12.8683 (18)O1W—H1W10.83 (2)
Na4—S2Aii3.0135 (10)O1W—H2W10.76 (3)
Na4—S1Aii3.2727 (10)O2W—H1W20.74 (3)
Na4—H1W22.53 (3)O2W—H2W20.86 (4)
S1A—O11A1.4656 (13)
O2W—Na1—O1W89.89 (6)O12A—S1A—O13A109.10 (7)
O2W—Na1—O1i99.67 (5)O11A—S1A—S2A109.71 (6)
O1W—Na1—O1i81.40 (5)O12A—S1A—S2A107.64 (5)
O2W—Na1—O1Wii91.35 (6)O13A—S1A—S2A107.50 (5)
O1W—Na1—O1Wii166.48 (5)O11A—S1A—Na3viii136.02 (6)
O1i—Na1—O1Wii111.63 (5)O12A—S1A—Na3viii50.05 (5)
O2W—Na1—O181.25 (5)O13A—S1A—Na3viii59.72 (6)
O1W—Na1—O187.07 (5)S2A—S1A—Na3viii113.94 (3)
O1i—Na1—O1168.43 (5)O11A—S1A—Na4i132.27 (7)
O1Wii—Na1—O179.81 (5)O12A—S1A—Na4i115.64 (5)
O2W—Na1—S2A172.41 (5)S2A—S1A—Na4i64.45 (2)
O1W—Na1—S2A96.82 (4)Na3viii—S1A—Na4i74.20 (2)
O1i—Na1—S2A84.89 (4)S1A—S2A—Na1109.73 (3)
O1Wii—Na1—S2A81.29 (4)S1A—S2A—Na4i78.46 (3)
O1—Na1—S2A95.51 (4)Na1—S2A—Na4i83.05 (2)
O12Aiii—Na2—O13B106.80 (5)S1A—O11A—Na3i139.59 (8)
O12Aiii—Na2—O13Aii85.66 (5)S1A—O12A—Na2viii136.14 (7)
O13B—Na2—O13Aii130.33 (6)S1A—O12A—Na3viii102.35 (6)
O12Aiii—Na2—O2164.74 (5)Na2viii—O12A—Na3viii100.67 (5)
O13B—Na2—O286.43 (5)S1A—O13A—Na2i125.07 (8)
O13Aii—Na2—O279.86 (5)S1A—O13A—Na4i111.74 (7)
O12Aiii—Na2—O12Biv98.90 (5)Na2i—O13A—Na4i106.45 (5)
O13B—Na2—O12Biv109.37 (5)S1A—O13A—Na3viii91.90 (6)
O13Aii—Na2—O12Biv115.96 (5)Na2i—O13A—Na3viii120.65 (5)
O2—Na2—O12Biv83.31 (5)Na4i—O13A—Na3viii97.64 (5)
O12Aiii—Na2—O13Biv85.37 (5)O11B—S1B—O13B109.21 (8)
O13B—Na2—O13Biv66.34 (5)O11B—S1B—O12B109.43 (8)
O13Aii—Na2—O13Biv162.96 (5)O13B—S1B—O12B109.30 (8)
O2—Na2—O13Biv107.35 (4)O11B—S1B—S2B108.91 (6)
O12Biv—Na2—O13Biv51.53 (4)O13B—S1B—S2B110.49 (6)
O12Aiii—Na2—S1Biv95.56 (4)O12B—S1B—S2B109.48 (6)
O13B—Na2—S1Biv86.70 (4)O11B—S1B—Na2iv115.58 (6)
O13Aii—Na2—S1Biv140.99 (4)O13B—S1B—Na2iv64.82 (6)
O2—Na2—S1Biv92.70 (4)O12B—S1B—Na2iv45.48 (5)
O12Biv—Na2—S1Biv25.24 (3)S2B—S1B—Na2iv134.18 (3)
O13Biv—Na2—S1Biv26.64 (3)S1B—O11B—Na3147.44 (9)
O2v—Na3—O11B89.56 (5)S1B—O12B—Na2iv109.27 (7)
O2v—Na3—O12Aiii169.73 (5)S1B—O12B—Na4ix126.40 (7)
O11B—Na3—O12Aiii96.31 (5)Na2iv—O12B—Na4ix107.93 (5)
O2v—Na3—O11Aii86.12 (5)S1B—O12B—Na3vi114.94 (7)
O11B—Na3—O11Aii102.85 (6)Na2iv—O12B—Na3vi93.39 (5)
O12Aiii—Na3—O11Aii84.36 (5)Na4ix—O12B—Na3vi99.74 (5)
O2v—Na3—O12Bvi84.08 (5)S1B—O13B—Na2132.97 (8)
O11B—Na3—O12Bvi109.38 (5)S1B—O13B—Na2iv88.54 (6)
O12Aiii—Na3—O12Bvi101.80 (5)Na2—O13B—Na2iv113.66 (5)
O11Aii—Na3—O12Bvi146.15 (6)C1—O1—Na1ii133.21 (10)
O2v—Na3—O13Aiii118.35 (5)C1—O1—Na497.80 (9)
O11B—Na3—O13Aiii151.98 (5)Na1ii—O1—Na4108.26 (5)
O12Aiii—Na3—O13Aiii55.74 (4)C1—O1—Na1118.01 (10)
O11Aii—Na3—O13Aiii78.31 (5)Na1ii—O1—Na197.47 (4)
O12Bvi—Na3—O13Aiii78.11 (4)Na4—O1—Na196.09 (5)
O2v—Na3—S1Aiii146.63 (4)C1—O2—Na3x142.11 (10)
O11B—Na3—S1Aiii123.60 (4)C1—O2—Na2117.50 (9)
O12Aiii—Na3—S1Aiii27.60 (3)Na3x—O2—Na298.33 (5)
O11Aii—Na3—S1Aiii83.01 (4)C1—O2—Na484.87 (9)
O12Bvi—Na3—S1Aiii87.63 (4)Na3x—O2—Na4103.17 (5)
O13Aiii—Na3—S1Aiii28.39 (3)Na2—O2—Na497.57 (5)
O2W—Na4—O181.40 (5)O1—C1—O2125.71 (14)
O2W—Na4—O13Aii165.17 (6)O1—C1—C2115.67 (13)
O1—Na4—O13Aii94.56 (5)O2—C1—C2118.62 (13)
O2W—Na4—O12Bvii98.82 (5)O1—C1—Na456.69 (8)
O1—Na4—O12Bvii175.46 (6)O2—C1—Na469.25 (9)
O13Aii—Na4—O12Bvii84.10 (5)C2—C1—Na4170.55 (11)
O2W—Na4—O2111.86 (5)N3—C2—C1111.99 (14)
O1—Na4—O251.34 (4)N3—C2—H1C105.6 (12)
O13Aii—Na4—O275.45 (4)C1—C2—H1C110.0 (13)
O12Bvii—Na4—O2132.06 (5)N3—C2—H2C107.8 (12)
O2W—Na4—C195.98 (5)C1—C2—H2C110.0 (13)
O1—Na4—C125.51 (4)H1C—C2—H2C111.4 (18)
O13Aii—Na4—C185.76 (5)C2—N3—H1N110.4 (16)
O12Bvii—Na4—C1157.94 (5)C2—N3—H2N109.1 (17)
O2—Na4—C125.89 (4)H1N—N3—H2N107 (2)
O2W—Na4—S2Aii103.67 (5)C2—N3—H3N109.6 (13)
O1—Na4—S2Aii82.39 (4)H1N—N3—H3N108 (2)
O13Aii—Na4—S2Aii61.56 (4)H2N—N3—H3N113 (2)
O12Bvii—Na4—S2Aii93.17 (4)Na1—O1W—Na1i98.96 (5)
O2—Na4—S2Aii113.02 (4)Na1—O1W—H1W1111.7 (16)
C1—Na4—S2Aii99.12 (4)Na1i—O1W—H1W1103.9 (16)
O2W—Na4—S1Aii140.68 (5)Na1—O1W—H2W1130 (2)
O1—Na4—S1Aii92.18 (4)Na1i—O1W—H2W1101 (2)
O13Aii—Na4—S1Aii24.70 (3)H1W1—O1W—H2W1107 (2)
O12Bvii—Na4—S1Aii84.79 (4)Na1—O2W—Na4100.84 (6)
O2—Na4—S1Aii92.83 (3)Na1—O2W—H1W2139 (2)
C1—Na4—S1Aii94.03 (4)Na4—O2W—H1W293 (2)
S2Aii—Na4—S1Aii37.087 (18)Na1—O2W—H2W2107 (2)
O11A—S1A—O12A111.15 (8)Na4—O2W—H2W2112 (2)
O11A—S1A—O13A111.59 (9)H1W2—O2W—H2W2104 (3)
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+1/2, y−1/2, −z+1/2; (iii) x, −y+1, z−1/2; (iv) −x, −y+1, −z; (v) x, y−1, z; (vi) −x, −y, −z; (vii) x+1/2, y+1/2, z; (viii) x, −y+1, z+1/2; (ix) x−1/2, y−1/2, z; (x) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H1N···O11Bx0.84 (3)2.01 (3)2.843 (2)170 (2)
N3—H2N···S2Axi0.82 (3)2.41 (3)3.2268 (17)174 (2)
N3—H3N···O13B0.87 (2)1.98 (2)2.804 (2)159.1 (18)
O1W—H1W1···O11Ai0.83 (2)1.98 (3)2.8069 (19)173 (2)
O1W—H2W1···S2Bx0.76 (3)2.46 (3)3.2191 (16)179 (3)
O2W—H1W2···S2Bvii0.74 (3)2.48 (3)3.2007 (16)162 (3)
O2W—H2W2···S2Ai0.86 (4)2.34 (4)3.1940 (16)171 (3)
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (vii) x+1/2, y+1/2, z; (x) x, y+1, z; (xi) −x, y, −z+1/2.
(III) poly[µ2-glycinato-µ4-thiosulfato-dipotassium(I)] top
Crystal data top
[K2(C2H5NO2)(S2O3)]F(000) = 536
Mr = 265.39Dx = 1.998 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 5.630 (1) ÅCell parameters from 904 reflections
b = 20.244 (4) Åθ = 4.1–27.5°
c = 7.762 (2) ŵ = 1.53 mm−1
β = 94.33 (3)°T = 293 K
V = 882.1 (3) Å3Sphere, colourless
Z = 40.10 × 0.08 × 0.04 mm
Data collection top
Nonius KappaCCD
diffractometer		2564 independent reflections
Radiation source: fine-focus sealed tube2251 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.013
Detector resolution: 9 pixels mm-1θmax = 30.0°, θmin = 4.2°
ω scansh = −7→7
Absorption correction: multi-scan
(Otwinowski & Minor, 1997)		k = −28→28
Tmin = 0.862, Tmax = 0.941l = −10→10
5037 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.023All H-atom parameters refined
wR(F2) = 0.058 w = 1/[σ2(Fo2) + (0.0247P)2 + 0.267P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.001
2564 reflectionsΔρmax = 0.25 e Å−3
130 parametersΔρmin = −0.34 e Å−3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0115 (11)
Crystal data top
[K2(C2H5NO2)(S2O3)]V = 882.1 (3) Å3
Mr = 265.39Z = 4
Monoclinic, P21/cMo Kα radiation
a = 5.630 (1) ŵ = 1.53 mm−1
b = 20.244 (4) ÅT = 293 K
c = 7.762 (2) Å0.10 × 0.08 × 0.04 mm
β = 94.33 (3)°
Data collection top
Nonius KappaCCD
diffractometer		2564 independent reflections
Absorption correction: multi-scan
(Otwinowski & Minor, 1997)		2251 reflections with I > 2σ(I)
Tmin = 0.862, Tmax = 0.941Rint = 0.013
5037 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0230 restraints
wR(F2) = 0.058All H-atom parameters refined
S = 1.10Δρmax = 0.25 e Å−3
2564 reflectionsΔρmin = −0.34 e Å−3
130 parameters
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 478 frames with phi- and omega-increments of 2 degree and a counting time of 180 s per frame. The crystal- to-detector-distance was 25 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 0.028.

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
xyzUiso*/Ueq
K10.40436 (5)0.260506 (16)−0.00755 (4)0.02916 (9)
K20.42910 (5)0.443399 (16)0.26787 (4)0.03081 (9)
S1−0.08645 (5)0.335937 (15)0.18622 (4)0.02172 (9)
S2−0.09362 (6)0.427232 (18)0.08420 (5)0.02970 (10)
O11−0.29668 (18)0.32692 (5)0.28484 (14)0.0340 (2)
O120.13520 (19)0.32843 (5)0.29576 (15)0.0358 (2)
O13−0.09317 (19)0.28780 (5)0.04247 (15)0.0354 (2)
O10.42678 (19)0.43672 (5)0.61542 (14)0.0344 (2)
O20.35030 (17)0.33763 (5)0.72092 (13)0.0288 (2)
C10.2888 (2)0.39303 (6)0.66189 (16)0.0222 (2)
C20.0247 (2)0.40925 (7)0.64319 (19)0.0268 (3)
H1C−0.008 (3)0.4422 (9)0.716 (2)0.033 (5)*
H2C−0.018 (3)0.4236 (10)0.527 (3)0.036 (5)*
N3−0.1229 (2)0.35224 (7)0.68732 (19)0.0306 (3)
H1N−0.103 (4)0.3209 (12)0.619 (3)0.053 (6)*
H2N−0.273 (4)0.3672 (11)0.677 (3)0.057 (6)*
H3N−0.090 (3)0.3404 (10)0.803 (3)0.038 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.02767 (15)0.02924 (16)0.03004 (16)−0.00446 (11)−0.00136 (11)0.00601 (11)
K20.02662 (16)0.02914 (16)0.03703 (17)−0.00290 (11)0.00488 (12)−0.00459 (12)
S10.01808 (15)0.02048 (15)0.02664 (16)−0.00026 (10)0.00183 (11)−0.00152 (11)
S20.03105 (18)0.02561 (17)0.03275 (18)−0.00012 (13)0.00450 (14)0.00488 (13)
O110.0277 (5)0.0329 (6)0.0432 (6)0.0010 (4)0.0134 (4)0.0087 (5)
O120.0264 (5)0.0319 (6)0.0470 (6)−0.0003 (4)−0.0110 (4)0.0053 (5)
O130.0375 (6)0.0291 (5)0.0397 (6)−0.0013 (4)0.0042 (5)−0.0125 (4)
O10.0344 (6)0.0307 (5)0.0388 (6)−0.0101 (4)0.0082 (4)0.0001 (4)
O20.0261 (5)0.0270 (5)0.0330 (5)0.0041 (4)0.0013 (4)0.0029 (4)
C10.0225 (6)0.0236 (6)0.0205 (6)−0.0010 (5)0.0029 (5)−0.0040 (5)
C20.0251 (6)0.0261 (7)0.0294 (7)0.0053 (5)0.0031 (5)−0.0002 (5)
N30.0180 (5)0.0395 (7)0.0344 (7)−0.0009 (5)0.0032 (5)−0.0054 (6)
Geometric parameters (Å, º) top
K1—O2i2.6225 (11)K2—C13.3745 (16)
K1—O2ii2.6958 (12)K2—S1iii3.5826 (7)
K1—O12ii2.7424 (12)K2—S13.6443 (7)
K1—O13iii2.8797 (12)K2—K2v4.2950 (11)
K1—O132.9098 (12)K2—K1vi4.4873 (9)
K1—O11iv2.9954 (12)S1—O121.4640 (11)
K1—O11iii3.0360 (14)S1—O111.4688 (11)
K1—O123.2050 (15)S1—O131.4800 (11)
K1—C1ii3.4560 (14)S1—S22.0100 (6)
K1—S1iii3.4874 (9)O1—C11.2483 (16)
K1—S13.5859 (9)O2—C11.2506 (17)
K1—K1ii3.9052 (10)C1—C21.5189 (18)
K2—O1v2.6940 (12)C2—N31.477 (2)
K2—O12.7028 (14)C2—H1C0.903 (19)
K2—O11iii2.8161 (12)C2—H2C0.959 (19)
K2—O122.8732 (12)N3—H1N0.84 (2)
K2—S2iii3.1527 (9)N3—H2N0.89 (2)
K2—S23.1887 (10)N3—H3N0.93 (2)
O2i—K1—O2ii162.87 (4)O1v—K2—S1144.29 (3)
O2i—K1—O12ii85.27 (4)O1—K2—S194.59 (3)
O2ii—K1—O12ii78.32 (4)O11iii—K2—S186.27 (3)
O2i—K1—O13iii92.72 (4)O12—K2—S122.17 (2)
O2ii—K1—O13iii102.19 (4)S2iii—K2—S1123.654 (16)
O12ii—K1—O13iii134.18 (4)S2—K2—S133.373 (11)
O2i—K1—O1386.55 (4)C1—K2—S174.90 (3)
O2ii—K1—O1383.94 (4)S1iii—K2—S1102.341 (18)
O12ii—K1—O1372.66 (4)O12—S1—O11111.67 (7)
O13iii—K1—O13153.04 (4)O12—S1—O13109.99 (7)
O2i—K1—O11iv87.42 (4)O11—S1—O13109.60 (7)
O2ii—K1—O11iv90.84 (4)O12—S1—S2108.37 (5)
O12ii—K1—O11iv67.78 (3)O11—S1—S2109.07 (5)
O13iii—K1—O11iv66.41 (3)O13—S1—S2108.04 (5)
O13—K1—O11iv140.33 (3)O12—S1—K1vii147.35 (5)
O2i—K1—O11iii111.20 (4)O11—S1—K1vii60.13 (5)
O2ii—K1—O11iii85.30 (3)O13—S1—K1vii54.05 (5)
O12ii—K1—O11iii163.53 (3)S2—S1—K1vii103.96 (2)
O13iii—K1—O11iii47.99 (3)O12—S1—K2vii125.95 (5)
O13—K1—O11iii107.52 (4)O11—S1—K2vii47.86 (4)
O11iv—K1—O11iii111.20 (4)O13—S1—K2vii123.83 (5)
O2i—K1—O12107.62 (4)S2—S1—K2vii61.21 (2)
O2ii—K1—O1275.50 (3)K1vii—S1—K2vii74.348 (16)
O12ii—K1—O12114.76 (4)O12—S1—K163.23 (5)
O13iii—K1—O12109.44 (4)O11—S1—K1147.42 (5)
O13—K1—O1246.14 (3)O13—S1—K151.67 (5)
O11iv—K1—O12164.78 (3)S2—S1—K1102.68 (2)
O11iii—K1—O1261.75 (3)K1vii—S1—K1105.481 (18)
O2i—K1—C1ii145.86 (3)K2vii—S1—K1162.536 (13)
O2ii—K1—C1ii18.72 (3)O12—S1—K247.79 (5)
O12ii—K1—C1ii60.63 (4)O11—S1—K2130.25 (5)
O13iii—K1—C1ii109.42 (3)O13—S1—K2119.93 (5)
O13—K1—C1ii84.79 (3)S2—S1—K260.77 (2)
O11iv—K1—C1ii78.64 (4)K1vii—S1—K2162.626 (13)
O11iii—K1—C1ii102.90 (3)K2vii—S1—K2102.341 (18)
O12—K1—C1ii89.61 (3)K1—S1—K272.443 (16)
O2i—K1—S1iii97.35 (3)S1—S2—K2vii84.817 (19)
O2ii—K1—S1iii99.72 (3)S1—S2—K285.855 (19)
O12ii—K1—S1iii158.34 (3)K2vii—S2—K2125.20 (2)
O13iii—K1—S1iii24.59 (2)S1—O11—K2vii109.39 (5)
O13—K1—S1iii128.87 (3)S1—O11—K1viii149.50 (6)
O11iv—K1—S1iii90.79 (3)K2vii—O11—K1viii101.05 (4)
O11iii—K1—S1iii24.81 (2)S1—O11—K1vii95.07 (6)
O12—K1—S1iii85.07 (3)K2vii—O11—K1vii93.71 (4)
C1ii—K1—S1iii113.69 (3)K1viii—O11—K1vii80.70 (3)
O2i—K1—S192.14 (3)S1—O12—K1vi143.37 (6)
O2ii—K1—S184.77 (3)S1—O12—K2110.04 (6)
O12ii—K1—S195.87 (3)K1vi—O12—K2106.06 (4)
O13iii—K1—S1129.94 (3)S1—O12—K192.71 (6)
O13—K1—S123.52 (2)K1vi—O12—K181.69 (3)
O11iv—K1—S1163.63 (2)K2—O12—K189.15 (4)
O11iii—K1—S184.20 (3)S1—O13—K1vii101.36 (6)
O12—K1—S124.07 (2)S1—O13—K1104.81 (6)
C1ii—K1—S192.87 (3)K1vii—O13—K1153.04 (4)
S1iii—K1—S1105.481 (18)C1—O1—K2v136.00 (9)
O1v—K2—O174.53 (4)C1—O1—K2111.96 (9)
O1v—K2—O11iii126.04 (4)K2v—O1—K2105.47 (4)
O1—K2—O11iii87.44 (4)C1—O2—K1ix147.21 (9)
O1v—K2—O12149.87 (4)C1—O2—K1vi117.50 (8)
O1—K2—O1280.68 (4)K1ix—O2—K1vi94.49 (4)
O11iii—K2—O1268.59 (3)O1—C1—O2125.48 (13)
O1v—K2—S2iii90.02 (3)O1—C1—C2116.44 (12)
O1—K2—S2iii120.99 (4)O2—C1—C2118.09 (12)
O11iii—K2—S2iii56.72 (2)O1—C1—K247.97 (7)
O12—K2—S2iii117.73 (3)O2—C1—K2121.73 (8)
O1v—K2—S2119.16 (3)C2—C1—K298.19 (8)
O1—K2—S2111.56 (4)O1—C1—K1vi112.84 (9)
O11iii—K2—S2114.78 (3)O2—C1—K1vi43.78 (7)
O12—K2—S255.48 (2)C2—C1—K1vi111.66 (8)
S2iii—K2—S2125.20 (2)K2—C1—K1vi82.13 (3)
O1v—K2—C193.01 (4)N3—C2—C1111.88 (12)
O1—K2—C120.06 (3)N3—C2—H1C106.7 (12)
O11iii—K2—C182.50 (4)C1—C2—H1C110.0 (12)
O12—K2—C160.75 (4)N3—C2—H2C110.5 (12)
S2iii—K2—C1130.13 (3)C1—C2—H2C109.1 (11)
S2—K2—C195.92 (3)H1C—C2—H2C108.6 (16)
O1v—K2—S1iii113.11 (3)C2—N3—H1N109.8 (15)
O1—K2—S1iii101.97 (4)C2—N3—H2N104.9 (15)
O11iii—K2—S1iii22.75 (2)H1N—N3—H2N112 (2)
O12—K2—S1iii88.39 (3)C2—N3—H3N110.4 (12)
S2iii—K2—S1iii33.969 (11)H1N—N3—H3N112.8 (19)
S2—K2—S1iii123.217 (16)H2N—N3—H3N106.9 (18)
C1—K2—S1iii102.14 (3)
Symmetry codes: (i) x, y, z−1; (ii) x, −y+1/2, z−1/2; (iii) x+1, y, z; (iv) x+1, −y+1/2, z−1/2; (v) −x+1, −y+1, −z+1; (vi) x, −y+1/2, z+1/2; (vii) x−1, y, z; (viii) x−1, −y+1/2, z+1/2; (ix) x, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H1N···O13vi0.84 (2)2.28 (2)3.059 (2)154 (2)
N3—H2N···O2vii0.89 (2)2.26 (2)3.0114 (16)142.0 (19)
N3—H3N···O13ix0.93 (2)2.15 (2)3.044 (2)161.2 (17)
Symmetry codes: (vi) x, −y+1/2, z+1/2; (vii) x−1, y, z; (ix) x, y, z+1.

Experimental details

(I)(II)(III)
Crystal data
Chemical formula[Co(H2O)6][Co(C2H5NO2)2(H2O)4](SO4)2[Na4(C2H5NO2)(S2O3)2(H2O)2][K2(C2H5NO2)(S2O3)]
Mr640.28427.30265.39
Crystal system, space groupTriclinic, P1Monoclinic, C2/cMonoclinic, P21/c
Temperature (K)293293293
a, b, c (Å)5.970 (1), 6.775 (1), 13.335 (3)17.775 (4), 7.311 (1), 22.595 (5)5.630 (1), 20.244 (4), 7.762 (2)
α, β, γ (°)85.23 (3), 83.31 (3), 83.22 (3)90, 100.10 (3), 9090, 94.33 (3), 90
V (Å3)530.62 (17)2890.8 (10)882.1 (3)
Z184
Radiation typeMo KαMo KαMo Kα
µ (mm−1)1.870.821.53
Crystal size (mm)0.40 × 0.35 × 0.300.20 × 0.10 × 0.080.10 × 0.08 × 0.04
Data collection
DiffractometerNonius KappaCCD
diffractometer		Nonius KappaCCD
diffractometer		Nonius KappaCCD
diffractometer
Absorption correctionMulti-scan
(Otwinowski & Minor, 1997)		Multi-scan
(Otwinowski & Minor, 1997)		Multi-scan
(Otwinowski & Minor, 1997)
Tmin, Tmax0.479, 0.5710.852, 0.9360.862, 0.941
No. of measured, independent and
observed [I > 2σ(I)] reflections		5847, 3191, 3036 10482, 3292, 2966 5037, 2564, 2251
Rint0.0140.0200.013
(sin θ/λ)max (Å−1)0.7130.6490.704
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.052, 1.06 0.025, 0.065, 1.04 0.023, 0.058, 1.10
No. of reflections319132922564
No. of parameters209227130
H-atom treatmentH-atom parameters constrainedAll H-atom parameters refinedAll H-atom parameters refined
Δρmax, Δρmin (e Å−3)0.46, −0.430.33, −0.420.25, −0.34

Computer programs: Collect (Nonius, 2003), HKL SCALEPACK (Otwinowski & Minor 1997), HKL DENZO (Otwinowski & Minor 1997) and SCALEPACK, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997; Farrugia 1997), SHELXL97 (Sheldrick, 1997; Farrugia, 1997), SHELXL97 (Sheldrick, 1997, Farrugia 1997), DIAMOND (Version 2.1; Bergerhoff et al., 1997), SHELXL97 (Sheldrick, 1997).

Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2S0.762.022.7605 (16)166.6
O1W—H2W1···O3Si0.781.972.7329 (14)167.7
O2W—H1W2···O4Sii0.791.962.7438 (15)169.6
O2W—H2W2···O3S0.841.972.7843 (15)163.5
O3W—H1W3···O2Siii0.841.902.7311 (13)175.0
O3W—H2W3···O3S0.822.042.8101 (15)156.8
O4W—H1W4···O1iv0.811.852.6543 (16)169.5
O4W—H2W4···O1Sv0.821.952.7531 (16)169.7
O5W—H1W5···O4Si0.811.912.7075 (15)172.0
O5W—H2W5···O1S0.791.992.7666 (14)172.4
N1—H1N···O2vi0.922.032.9042 (16)159.1
N1—H2N···O1iv0.852.282.8725 (17)127.5
N1—H2N···O5W0.852.383.0966 (15)142.4
N1—H3N···O1Svii0.852.132.8887 (16)148.8
Symmetry codes: (i) x+1, y, z; (ii) −x, −y+1, −z; (iii) x, y−1, z; (iv) x−1, y, z; (v) −x, −y+1, −z+1; (vi) −x+1, −y+2, −z+1; (vii) x, y+1, z.
Selected bond lengths (Å) for (II) top
Na1—O2W2.3359 (16)Na3—O12Bvi2.5442 (15)
Na1—O1W2.4095 (15)Na3—O13Aiii2.6736 (16)
Na1—O1i2.4185 (13)Na4—O2W2.3883 (17)
Na1—O1Wii2.4308 (15)Na4—O12.4196 (15)
Na1—O12.4765 (14)Na4—O13Aii2.4281 (15)
Na1—S2A2.8990 (10)Na4—O12Bvii2.4820 (16)
Na2—O12Aiii2.3331 (12)Na4—O22.6930 (15)
Na2—O13B2.3803 (15)Na4—S2Aii3.0135 (10)
Na2—O13Aii2.4233 (15)S1A—O11A1.4656 (13)
Na2—O22.4689 (13)S1A—O12A1.4676 (12)
Na2—O12Biv2.4692 (14)S1A—O13A1.4721 (13)
Na2—O13Biv2.9590 (19)S1A—S2A2.0142 (8)
Na3—O2v2.3526 (12)S1B—O11B1.4649 (12)
Na3—O11B2.3633 (15)S1B—O13B1.4662 (12)
Na3—O12Aiii2.4285 (13)S1B—O12B1.4767 (13)
Na3—O11Aii2.4735 (16)S1B—S2B1.9945 (7)
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+1/2, y−1/2, −z+1/2; (iii) x, −y+1, z−1/2; (iv) −x, −y+1, −z; (v) x, y−1, z; (vi) −x, −y, −z; (vii) x+1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
N3—H1N···O11Bviii0.84 (3)2.01 (3)2.843 (2)170 (2)
N3—H2N···S2Aix0.82 (3)2.41 (3)3.2268 (17)174 (2)
N3—H3N···O13B0.87 (2)1.98 (2)2.804 (2)159.1 (18)
O1W—H1W1···O11Ai0.83 (2)1.98 (3)2.8069 (19)173 (2)
O1W—H2W1···S2Bviii0.76 (3)2.46 (3)3.2191 (16)179 (3)
O2W—H1W2···S2Bvii0.74 (3)2.48 (3)3.2007 (16)162 (3)
O2W—H2W2···S2Ai0.86 (4)2.34 (4)3.1940 (16)171 (3)
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (vii) x+1/2, y+1/2, z; (viii) x, y+1, z; (ix) −x, y, −z+1/2.
Hydrogen-bond geometry (Å, º) for (III) top
D—H···AD—HH···AD···AD—H···A
N3—H1N···O13i0.84 (2)2.28 (2)3.059 (2)154 (2)
N3—H2N···O2ii0.89 (2)2.26 (2)3.0114 (16)142.0 (19)
N3—H3N···O13iii0.93 (2)2.15 (2)3.044 (2)161.2 (17)
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x−1, y, z; (iii) x, y, z+1.
Overview of the stoichiometries, symmetries and unit cell parameters (Å and °) of glycine metal sulphate and thiosulphate compounds. top
Glycine (NH4)2(SO4)8.2610.078.639092.6690P21/c(a)
Glycine Li2(SO4)16.425.007.65909090Pna21(b)
Glycine Co(SO4).5H2O5.576.7813.3485.2083.3083.21P-1(c)
Glycine Ni(SO4).6H2O5.7312.3017.019097.9290P21/c(d)
Glycine Zn(SO4).3H2O8.448.2812.52909090Pca21(b)
Glycine K2(S2O3)5.6320.247.769094.3390P21/c(c)
Glycine Na4(S2O3)2.2H2O17.787.3122.6090100.1090C21/C(c)
Reference: (a) Vilminot et al. (1974); (b) Fleck & Bohatý (2004); (c) this work; (d) Peterková et al. (1991).
 

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