Crystal structure of bis­(di­methyl­ammonium) hexa­aqua­cobalt(II) bis­(sulfate) dihydrate

Held, P.

doi:10.1107/S2056989015003400

metal-organic compounds

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Volume 71| Part 4| April 2015| Pages m77-m78

doi:10.1107/S2056989015003400

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Crystal structure of bis(dimethylammonium) hexaaquacobalt(II) bis(sulfate) dihydrate

Peter Held ^a ^*

^aInstitut für Kristallographie, Universität zu Köln, Greinstr. 6, D-50939 Köln, Germany
^*Correspondence e-mail: peter.held@uni-koeln.de

Edited by U. Flörke, University of Paderborn, Germany (Received 5 February 2015; accepted 18 February 2015; online 4 March 2015)

The title salt, (C₂H₈N)₂[Co(H₂O)₆)](SO₄)₂·2H₂O, is isotypic with (C₂H₈N)₂[Ni(H₂O)₆)](SO₄)₂·2H₂O. The Co—O bond lengths in the [Co(H₂O)₆]²⁺ complex cation show very similar distances as in the related Tutton salt (NH₄)₂[Co(H₂O)₆)](SO₄)₂ [average 2.093 (17) Å], but are significantly longer than in the isotypic Ni^II compound (Δd ≃ 0.04 Å). The cobalt cation reaches an overall bond-valence sum of 1.97 valence units. The S—O distances are nearly equal, ranging from 1.454 (4) to 1.470 (3) Å [mean 1.465 (12) Å]; however, the O—S—O angles vary clearly from 108.1 (2) to 110.2 (2)° [average bond angle 109.5 (9)°]. The non-coordinating water molecules and dimethylammonium cations connect the sulfate tetrahedra and the [Co(H₂O)₆]²⁺ octahedron via O—H⋯O and N—H⋯O hydrogen bonds of weak up to medium strength into a three-dimensional framework whereby the complex metal cations and sulfate anions are arranged in sheets parallel to (001).

Keywords: crystal structure; dimethylammonium salt; hexaaquacobalt(II) salt; sulfate; hydrogen bonding.

CCDC reference: 1050102

1. Related literature

For the synthesis and coordination geometry of the isotypic structure (C₂H₈N)₂[Ni(H₂O)₆)](SO₄)₂·2H₂O, see: Held (2014 ). For the related Tutton salt (NH₄)₂[Co(H₂O)₆)](SO₄)₂, see: Grimes et al. (1963 ). For the bond-valence-sum method, see: Brown & Altermatt (1985 ).

2. Experimental

2.1. Crystal data

(C₂H₈N)₂[Co(H₂O)₆](SO₄)₂·2H₂O
M_r = 487.37
Orthorhombic, P b c a
a = 8.975 (5) Å
b = 13.268 (5) Å
c = 16.528 (5) Å
V = 1968.2 (15) Å³
Z = 4
Mo Kα radiation
μ = 1.16 mm⁻¹
T = 295 K
0.30 × 0.27 × 0.24 mm

2.2. Data collection

Enraf–Nonius CAD-4 diffractometer
Absorption correction: ψ scan (North et al., 1968 ) T_min = 0.903, T_max = 1.000
3383 measured reflections
1733 independent reflections
936 reflections with I > 2σ(I)
R_int = 0.077
3 standard reflections every 100 reflections intensity decay: 1.5%

2.3. Refinement

R[F² > 2σ(F²)] = 0.039
wR(F²) = 0.111
S = 0.98
1733 reflections
148 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.41 e Å⁻³
Δρ_min = −0.37 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H51⋯O2ⁱ	0.82 (6)	1.91 (6)	2.724 (6)	169 (5)
O5—H52⋯O8	0.84 (7)	1.97 (8)	2.806 (7)	171 (7)
O6—H61⋯O3ⁱⁱ	0.85 (7)	1.85 (7)	2.687 (6)	173 (6)
O6—H62⋯O1	0.69 (5)	2.08 (5)	2.740 (6)	161 (6)
O7—H71⋯O4ⁱⁱⁱ	0.74 (6)	2.01 (6)	2.740 (6)	173 (6)
O7—H72⋯O1^iv	0.72 (4)	2.04 (4)	2.756 (6)	176 (5)
O8—H81⋯O3ⁱⁱⁱ	0.71 (6)	2.32 (6)	2.975 (7)	154 (7)
O8—H82⋯O2^v	0.83 (6)	2.02 (6)	2.849 (6)	169 (7)
N3—H3A⋯O6^iv	0.90	2.63	3.265 (6)	128
N3—H3B⋯O4^vi	0.90	2.00	2.823 (6)	152
Symmetry codes: (i) -x, -y+1, -z+1; (ii) $[x-{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1]$ ; (iii) -x+1, -y+1, -z+1; (iv) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, z]$ ; (v) $[-x+{\script{1\over 2}}, -y+1, z-{\script{1\over 2}}]$ ; (vi) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1]$ .

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1989 ); cell refinement: CAD-4 EXPRESS; data reduction: MolEN (Fair, 1990 ); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: ATOMS (Dowty, 2011 ); software used to prepare material for publication: SHELXL97 and publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 1050102

Crystal structure: contains datablocks I, global. DOI: 10.1107/S2056989015003400/fk2085sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S2056989015003400/fk2085Isup2.hkl

checkCIF report

Refinement top

All H atoms were clearly discernible from difference Fourier maps. However, to all hydrogen atoms riding model contraints were applied in the least squares refinement, with C—H = 0.96 Å and U_iso(H) = 1.5U_eq(C) for methyl H atoms and with N—H = 0.90 Å and U_iso(H) = 1.2U_eq(N) for ammonium H atoms. The H atoms of water molecules were refined with a distance restraint of O—H = 0.84 Å and individual U_iso values for each H atom.

Related literature top

For the synthesis and coordination geometry of the isotypic structure (C₂H₈N)₂[Ni(H₂O)₆)](SO₄)₂·2H₂O, see: Held (2014). For the related Tutton salt (NH₄)₂[Co(H₂O)₆)](SO₄)₂ , see: Grimes et al. (1963). For the bond-valence-sum method, see: Brown & Altermatt (1985).

Structure description top

For the synthesis and coordination geometry of the isotypic structure (C₂H₈N)₂[Ni(H₂O)₆)](SO₄)₂·2H₂O, see: Held (2014). For the related Tutton salt (NH₄)₂[Co(H₂O)₆)](SO₄)₂ , see: Grimes et al. (1963). For the bond-valence-sum method, see: Brown & Altermatt (1985).

Refinement details top

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1989); cell refinement: CAD-4 EXPRESS (Enraf–Nonius, 1989); data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ATOMS (Dowty, 2011); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010).

Figures top

	Fig. 1. The molecular entities in the structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry code: (i) -x, -y + 1, -z - 1.]
	Fig. 2. (100)-projection of the crystal structure of the title compound. Colour scheme: S (yellow), Co (red), O (blue), N (orange), C (grey), H (colourless), H···O bonds up to 1.8 Å are given as red dashed lines, and from 1.85 to 2.7 Å as light-blue dashed lines.

Bis(dimethylammonium) hexaaquacobalt(II) bis(sulfate) dihydrate top

Crystal data top

(C₂H₈N)₂[Co(H₂O)₆](SO₄)₂·2H₂O	F(000) = 1028
M_r = 487.37	D_x = 1.645 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 25 reflections
a = 8.975 (5) Å	θ = 12.0–20.8°
b = 13.268 (5) Å	µ = 1.16 mm⁻¹
c = 16.528 (5) Å	T = 295 K
V = 1968.2 (15) Å³	Parallelepiped, light blue
Z = 4	0.30 × 0.27 × 0.24 mm

Data collection top

Enraf–Nonius CAD-4 diffractometer	936 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.077
Graphite monochromator	θ_max = 25.0°, θ_min = 2.5°
ω/2θ scans	h = 0→10
Absorption correction: ψ scan (North et al., 1968)	k = 0→15
T_min = 0.903, T_max = 1.000	l = −19→19
3383 measured reflections	3 standard reflections every 100 reflections
1733 independent reflections	intensity decay: 1.5%

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.039	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.111	w = 1/[σ²(F_o²) + (0.0529P)²] where P = (F_o² + 2F_c²)/3
S = 0.98	(Δ/σ)_max < 0.001
1733 reflections	Δρ_max = 0.41 e Å⁻³
148 parameters	Δρ_min = −0.37 e Å⁻³
2 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0022 (6)

Crystal data top

(C₂H₈N)₂[Co(H₂O)₆](SO₄)₂·2H₂O	V = 1968.2 (15) Å³
M_r = 487.37	Z = 4
Orthorhombic, Pbca	Mo Kα radiation
a = 8.975 (5) Å	µ = 1.16 mm⁻¹
b = 13.268 (5) Å	T = 295 K
c = 16.528 (5) Å	0.30 × 0.27 × 0.24 mm

Data collection top

Enraf–Nonius CAD-4 diffractometer	936 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.077
T_min = 0.903, T_max = 1.000	3 standard reflections every 100 reflections
3383 measured reflections	intensity decay: 1.5%
1733 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.039	2 restraints
wR(F²) = 0.111	H atoms treated by a mixture of independent and constrained refinement
S = 0.98	Δρ_max = 0.41 e Å⁻³
1733 reflections	Δρ_min = −0.37 e Å⁻³
148 parameters

Special details top

Experimental. A suitable single-crystal was carefully selected under a polarizing microscope and mounted in a glass capillary.

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	U_iso*/U_eq
Co	0.0000	0.5000	0.5000	0.0278 (3)
S1	0.44510 (13)	0.65726 (9)	0.59555 (8)	0.0319 (3)
O1	0.3702 (4)	0.6999 (2)	0.5243 (2)	0.0466 (10)
O2	0.3355 (4)	0.6107 (3)	0.6497 (2)	0.0419 (9)
O3	0.5255 (5)	0.7366 (3)	0.6378 (2)	0.0634 (12)
O4	0.5493 (5)	0.5793 (3)	0.5696 (3)	0.0791 (15)
O5	−0.0505 (5)	0.4446 (3)	0.3854 (2)	0.0422 (10)
H51	−0.136 (7)	0.422 (4)	0.380 (3)	0.040 (18)*
H52	0.010 (8)	0.403 (5)	0.365 (5)	0.11 (3)*
O6	0.1413 (5)	0.6068 (3)	0.4439 (3)	0.0391 (10)
H61	0.103 (8)	0.653 (5)	0.415 (4)	0.09 (3)*
H62	0.198 (6)	0.620 (4)	0.470 (3)	0.03 (2)*
O7	0.1808 (5)	0.4036 (3)	0.5066 (3)	0.0444 (10)
H71	0.251 (7)	0.412 (4)	0.484 (3)	0.037 (19)*
H72	0.172 (5)	0.350 (3)	0.512 (3)	0.021 (16)*
O8	0.1675 (5)	0.3224 (4)	0.3135 (3)	0.0558 (13)
H81	0.245 (7)	0.326 (5)	0.322 (4)	0.06 (2)*
H82	0.174 (8)	0.348 (5)	0.268 (4)	0.09 (3)*
N3	0.0327 (6)	0.1120 (3)	0.3563 (3)	0.0567 (14)
H3A	0.1016	0.1541	0.3769	0.068*
H3B	0.0187	0.0622	0.3925	0.068*
C1	0.0909 (10)	0.0689 (5)	0.2833 (4)	0.094 (3)
H1A	0.1825	0.0344	0.2950	0.141*
H1B	0.1092	0.1214	0.2446	0.141*
H1C	0.0201	0.0219	0.2615	0.141*
C2	−0.1060 (7)	0.1669 (5)	0.3473 (4)	0.074 (2)
H2A	−0.1450	0.1833	0.3998	0.111*
H2B	−0.1767	0.1260	0.3187	0.111*
H2C	−0.0883	0.2279	0.3175	0.111*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.0269 (5)	0.0257 (4)	0.0309 (4)	0.0003 (5)	−0.0026 (5)	−0.0010 (5)
S1	0.0249 (6)	0.0340 (6)	0.0368 (7)	−0.0010 (6)	−0.0005 (6)	0.0065 (6)
O1	0.055 (2)	0.042 (2)	0.044 (2)	−0.0080 (19)	−0.0180 (18)	0.0107 (17)
O2	0.0289 (19)	0.052 (2)	0.045 (2)	−0.0104 (17)	0.0059 (17)	0.0093 (18)
O3	0.084 (3)	0.060 (2)	0.047 (2)	−0.034 (3)	−0.023 (2)	0.0151 (19)
O4	0.063 (3)	0.067 (3)	0.108 (4)	0.026 (2)	0.042 (3)	0.032 (3)
O5	0.034 (2)	0.053 (2)	0.040 (2)	−0.004 (2)	−0.002 (2)	−0.0102 (19)
O6	0.035 (2)	0.039 (2)	0.043 (2)	−0.004 (2)	−0.007 (2)	0.007 (2)
O7	0.035 (2)	0.036 (3)	0.062 (3)	0.007 (2)	0.012 (2)	0.010 (2)
O8	0.035 (3)	0.093 (4)	0.039 (3)	−0.004 (3)	−0.001 (2)	−0.009 (3)
N3	0.069 (4)	0.047 (3)	0.054 (3)	0.005 (3)	−0.018 (3)	−0.004 (2)
C1	0.135 (8)	0.056 (4)	0.090 (6)	0.016 (5)	0.054 (5)	0.009 (4)
C2	0.057 (4)	0.084 (5)	0.080 (5)	0.005 (4)	0.007 (4)	0.016 (4)

Geometric parameters (Å, º) top

Co—O7ⁱ	2.069 (4)	O7—H71	0.74 (6)
Co—O7	2.069 (4)	O7—H72	0.72 (4)
Co—O5ⁱ	2.081 (4)	O8—H81	0.71 (6)
Co—O5	2.081 (4)	O8—H82	0.83 (6)
Co—O6	2.116 (4)	N3—C1	1.434 (7)
Co—O6ⁱ	2.116 (4)	N3—C2	1.450 (7)
S1—O3	1.454 (4)	N3—H3A	0.9000
S1—O4	1.459 (4)	N3—H3B	0.9000
S1—O2	1.467 (3)	C1—H1A	0.9600
S1—O1	1.470 (3)	C1—H1B	0.9600
O5—H51	0.82 (6)	C1—H1C	0.9600
O5—H52	0.84 (7)	C2—H2A	0.9600
O6—H61	0.85 (7)	C2—H2B	0.9600
O6—H62	0.69 (5)	C2—H2C	0.9600

O7ⁱ—Co—O7	180.0 (3)	Co—O6—H62	109 (4)
O7ⁱ—Co—O5ⁱ	90.04 (18)	H61—O6—H62	119 (6)
O7—Co—O5ⁱ	89.96 (18)	Co—O7—H71	123 (4)
O7ⁱ—Co—O5	89.96 (18)	Co—O7—H72	122 (4)
O7—Co—O5	90.04 (18)	H71—O7—H72	109 (6)
O5ⁱ—Co—O5	180.000 (1)	H81—O8—H82	95 (7)
O7ⁱ—Co—O6	91.87 (19)	C1—N3—C2	115.3 (5)
O7—Co—O6	88.13 (19)	C1—N3—H3A	108.5
O5ⁱ—Co—O6	91.80 (18)	C2—N3—H3A	108.5
O5—Co—O6	88.20 (18)	C1—N3—H3B	108.5
O7ⁱ—Co—O6ⁱ	88.13 (19)	C2—N3—H3B	108.5
O7—Co—O6ⁱ	91.87 (19)	H3A—N3—H3B	107.5
O5ⁱ—Co—O6ⁱ	88.20 (18)	N3—C1—H1A	109.5
O5—Co—O6ⁱ	91.80 (18)	N3—C1—H1B	109.5
O6—Co—O6ⁱ	180.0	H1A—C1—H1B	109.5
O3—S1—O4	109.6 (3)	N3—C1—H1C	109.5
O3—S1—O2	110.1 (2)	H1A—C1—H1C	109.5
O4—S1—O2	108.1 (2)	H1B—C1—H1C	109.5
O3—S1—O1	109.5 (2)	N3—C2—H2A	109.5
O4—S1—O1	109.3 (3)	N3—C2—H2B	109.5
O2—S1—O1	110.2 (2)	H2A—C2—H2B	109.5
Co—O5—H51	116 (4)	N3—C2—H2C	109.5
Co—O5—H52	117 (5)	H2A—C2—H2C	109.5
H51—O5—H52	108 (6)	H2B—C2—H2C	109.5
Co—O6—H61	119 (5)

Symmetry code: (i) −x, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H51···O2ⁱ	0.82 (6)	1.91 (6)	2.724 (6)	169 (5)
O5—H52···O8	0.84 (7)	1.97 (8)	2.806 (7)	171 (7)
O6—H61···O3ⁱⁱ	0.85 (7)	1.85 (7)	2.687 (6)	173 (6)
O6—H62···O1	0.69 (5)	2.08 (5)	2.740 (6)	161 (6)
O7—H71···O4ⁱⁱⁱ	0.74 (6)	2.01 (6)	2.740 (6)	173 (6)
O7—H72···O1^iv	0.72 (4)	2.04 (4)	2.756 (6)	176 (5)
O8—H81···O3ⁱⁱⁱ	0.71 (6)	2.32 (6)	2.975 (7)	154 (7)
O8—H82···O2^v	0.83 (6)	2.02 (6)	2.849 (6)	169 (7)
N3—H3A···O6^iv	0.90	2.63	3.265 (6)	128
N3—H3B···O4^vi	0.90	2.00	2.823 (6)	152

Symmetry codes: (i) −x, −y+1, −z+1; (ii) x−1/2, −y+3/2, −z+1; (iii) −x+1, −y+1, −z+1; (iv) −x+1/2, y−1/2, z; (v) −x+1/2, −y+1, z−1/2; (vi) x−1/2, −y+1/2, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H51···O2ⁱ	0.82 (6)	1.91 (6)	2.724 (6)	169 (5)
O5—H52···O8	0.84 (7)	1.97 (8)	2.806 (7)	171 (7)
O6—H61···O3ⁱⁱ	0.85 (7)	1.85 (7)	2.687 (6)	173 (6)
O6—H62···O1	0.69 (5)	2.08 (5)	2.740 (6)	161 (6)
O7—H71···O4ⁱⁱⁱ	0.74 (6)	2.01 (6)	2.740 (6)	173 (6)
O7—H72···O1^iv	0.72 (4)	2.04 (4)	2.756 (6)	176 (5)
O8—H81···O3ⁱⁱⁱ	0.71 (6)	2.32 (6)	2.975 (7)	154 (7)
O8—H82···O2^v	0.83 (6)	2.02 (6)	2.849 (6)	169 (7)
N3—H3A···O6^iv	0.90	2.63	3.265 (6)	127.8
N3—H3B···O4^vi	0.90	2.00	2.823 (6)	151.5

Symmetry codes: (i) −x, −y+1, −z+1; (ii) x−1/2, −y+3/2, −z+1; (iii) −x+1, −y+1, −z+1; (iv) −x+1/2, y−1/2, z; (v) −x+1/2, −y+1, z−1/2; (vi) x−1/2, −y+1/2, −z+1.

References

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ISSN: 2056-9890

Volume 71| Part 4| April 2015| Pages m77-m78

doi:10.1107/S2056989015003400

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Crystal structure of bis­­(di­methyl­ammonium) hexa­aqua­cobalt(II) bis­­(sulfate) dihydrate

1. Related literature

2. Experimental

2.1. Crystal data

2.2. Data collection

2.3. Refinement

Supporting information

References

metal-organic compounds

Crystal structure of bis(dimethylammonium) hexaaquacobalt(II) bis(sulfate) dihydrate