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

Held, P.

doi:10.1107/S160053681402234X

research communications

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 70| Part 11| November 2014| Pages 403-405

doi:10.1107/S160053681402234X

Open

access

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

Peter Held ^a ^*

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

Edited by M. Weil, Vienna University of Technology, Austria (Received 2 October 2014; accepted 10 October 2014; online 24 October 2014)

In the title salt, (C₂H₈N)₂[Ni(H₂O)₆)](SO₄)₂·2H₂O, the Ni^II cation is located on a centre of inversion and exhibits a slightly distorted octahedral arrangement of water molecules. The Ni—O bond lengths in the complex [Ni(H₂O)₆]²⁺ cation show a distribution as in the related Tutton salt (NH₄)₂[Ni(H₂O)₆](SO₄)₂, but are longer in average [2.056 (13) versus 2.037 (12) Å]. The noncoordinating water molecules and dimethylammonium cations connect the sulfate and [Ni(H₂O)₆]²⁺ octahedra via O—H⋯O and N—H⋯O hydrogen bonds from weak up to medium strength into a three-dimensional framework whereby the complex metal cations and sulfate anions are arranged in sheets parallel (001).

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

CCDC reference: 1028557

1. Chemical context

In the course of a systematic search for new `double salts' of simple secondary amines and divalent cations of various inorganic acids, the structure of [(CH₃)₂NH₂][Cu(HSO₄)(SO₄)(H₂O)₄] has been described previously (Held, 2014 ). In continuation of these studies, copper(II) was replaced by nickel(II), yielding crystals of the title compound with composition (C₂H₈N)₂[Ni(H₂O)₆)](SO₄)₂·2H₂O.

2. Structural commentary

The asymmetric unit of the title compound consists of one [NH₂(CH₃)]⁺ cation, one Ni²⁺ cation situated on an inversion centre (Wyckoff position 4a), one SO₄²⁻ anion and four water molecules, one of which is not coordinating to the metal cation (Fig. 1). The Ni^II cation exhibits a slightly distorted octahedral arrangement of the water molecules. The Ni—O distances show the same bond lengths distribution [mean 2.055 (12) Å], as in the related Tutton salt (NH₄)₂[Ni(H₂O)₆](SO₄)₂ (Grimes et al., 1963 ), but are slightly longer (Δd = 0.02 Å). The Ni^II cation reaches an overall bond valence sum (Brown & Altermatt, 1985 ) of 2.03 valence units. The S—O distances are nearly equal [mean 1.463 (8) Å], however, the O—S—O angles vary clearly [average bond angle 109.5 (8)°].

Figure 1
The molecular entities in the structure of the title compound, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry code: (i) −x, −y + 1, −z − 1.]

3. Supramolecular features

Hydrogen bonds of weak up to medium strength involving coordinating and noncoordinating water molecules as donor groups and O atoms of the sulfate anions as acceptor groups interconnect neighbouring [Ni(H₂O)₆]²⁺ octahedra. Together with relatively weaker N—H⋯O hydrogen bonds of the ammonium H atoms to sulfate anions, a three-dimensional framework is formed with pronounced formation of sheets of complex metal cations and sulfate anions parallel (001) (Table 1 and Fig. 2).

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H51⋯O2ⁱ	0.97 (1)	1.77 (2)	2.727 (5)	166 (5)
O5—H52⋯O8	0.98 (1)	1.84 (1)	2.814 (6)	176 (7)
O6—H61⋯O3ⁱⁱ	0.97 (1)	1.73 (2)	2.689 (5)	169 (6)
O6—H62⋯O1	0.98 (1)	1.78 (2)	2.731 (5)	164 (5)
O7—H71⋯O4ⁱⁱⁱ	0.97 (1)	1.78 (2)	2.730 (6)	164 (5)
O7—H72⋯O1^iv	0.98 (1)	1.78 (2)	2.745 (5)	173 (7)
O8—H81⋯O3ⁱⁱⁱ	0.98 (1)	2.01 (2)	2.962 (6)	166 (6)
O8—H82⋯O2^v	0.98 (1)	1.93 (3)	2.856 (6)	158 (7)
N3—H3B⋯O4^vi	0.90	2.02	2.835 (7)	151
N3—H3A⋯O6^iv	0.90	2.65	3.274 (6)	127
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) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, -z-1]$ .

Figure 2
(100)-projection of the crystal structure of the title compound. Colour scheme: (SO₄) tetrahedra yellow, [Ni(OH₂)₆] octahedra red, O blue, N green, C grey and H colourless. H⋯O bonds up to 1.8 Å are given as orange dashed lines and from 1.85 to 2.7 Å as light-blue dashed lines.

4. Synthesis and crystallization

The title compound was obtained by reaction of an aqueous solution of nickel(II) sulfate with dimethylamine and sulfuric acid (18 mol l⁻¹) in a stoichiometric ratio of 1:2:1. The resulting solution was kept at room temperature by cooling. The title compound crystallized by slow evaporation of the solvent at room temperature in form of light-green crystals with dimensions up to 4 mm within 12 weeks.

5. Refinement

Details of structure refinement are given in Table 2. All H atoms were clearly discernible from difference Fourier maps. However, riding-model contraints were applied to all H atoms in the least-squares refinement, with C—H = 0.96 Å and U_iso(H) = 1.5U_eq(C) for methyl H atoms, and 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 = 0.98 Å and individual U_iso values for each H atom.

Table 2
Experimental details

Crystal data
Chemical formula	(C₂H₈N)₂[Ni(H₂O)₆](SO₄)₂·2H₂O
M_r	487.13
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	295
a, b, c (Å)	8.9363 (6), 13.2370 (8), 16.4810 (14)
V (Å³)	1949.5 (2)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	1.28
Crystal size (mm)	0.29 × 0.27 × 0.26

Data collection
Diffractometer	Enraf–Nonius MACH3
Absorption correction	ψ scan (North et al., 1968 )
T_min, T_max	0.935, 0.999
No. of measured, independent and observed [I > 2σ(I)] reflections	4902, 1719, 962
R_int	0.107
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.123, 1.07
No. of reflections	1719
No. of parameters	148
No. of restraints	8
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.44, −0.41
Computer programs: CAD-4 Software (Enraf–Nonius, 1998 ), MolEN (Fair, 1990 ), SIR97 (Altomare et al., 1999 ), ATOMS (Dowty, 2011 ), SHELXL97 (Sheldrick, 2008 ) and publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 1028557

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681402234X/wm5074sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053681402234X/wm5074Isup2.hkl

checkCIF report

Chemical context top

In the course of a systematic search for new `double salts' of simple secondary amines and divalent cations of various inorganic acids, the structure of [(CH₃)₂NH₂][Cu(HSO₄)(SO₄)(H₂O)₄] has been described previously (Held, 2014). In continuation of these studies, copper(II) was replaced by nickel(II), yielding crystals of the title compound with composition (C₂H₈N)₂[Ni(H₂O)₆)](SO₄)₂·2H₂O.

Structural commentary top

The asymmetric unit of the title compound consists of one [NH₂(CH₃)]⁺ cation, one Ni²⁺ cation situated on an inversion centre (Wyckoff position 4a), one SO₄^2- anion and four water molecules, one of which is not coordinating to the metal cation (Fig. 1). The Ni^II cation exhibits a slightly distorted octahedral arrangement of the water molecules. The Ni—O distances show the same bond lengths distribution [mean 2.055 (12) Å], as in the related Tutton salt (NH₄)₂[Ni(H₂O)₆)](SO₄)₂ (Grimes et al., 1963), but are slightly longer (Δd = 0.02 Å). The Ni^II cation reaches an overall bond valence sum (Brown & Altermatt, 1985) of 2.03 valence units. The S—O distances are nearly equal [mean 1.463 (8) Å], however, the O—S—O angles vary clearly [average bond angle 109.5 (8)°].

Supramolecular features top

Hydrogen bonds of weak up to medium strength involving coordinating and noncoordinating water molecules as donor groups and O atoms of the sulfate anions as acceptor groups interconnect neighbouring [Ni(H₂O)₆]²⁺ octahedra. Together with relatively weaker N—H···O hydrogen bonds of the ammonium H atoms to sulfate anions, a three-dimensional framework is formed with pronounced formation of sheets of complex metal cations and sulfate anions parallel (001) (Table 1 and Fig. 2).

Synthesis and crystallization top

The title compound was obtained by reaction of an aqueous solution of nickel(II) sulfate with dimethylamine and sulfuric acid (18 mol l^-1) in a stoichiometric ratio of 1:2:1. The resulting solution was kept at room temperature by cooling. The title compound crystallized by slow evaporation of the solvent at room temperature in form of light-green crystals with dimensions up to 4 mm within 12 weeks.

Refinement top

Details of structure refinement are given in Table 1. All H atoms were clearly discernible from difference Fourier maps. However, riding-model contraints were applied to all H atoms in the least-squares refinement, with C—H = 0.96 Å and U_iso(H) = 1.5U_eq(C) for methyl H atoms, and 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 = 0.98 Å and individual U_iso values for each H atom.

Related literature top

For related literature, see: Brown & Altermatt (1985); Grimes et al. (1963); Held (2014).

Computing details top

Data collection: CAD-4 Software (Enraf–Nonius, 1998); cell refinement: CAD-4 Software (Enraf–Nonius, 1998); 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 puplCIF (Westrip, 2010).

Figures top

The molecular entities in the structure of the title compound, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry code: (i) -x, -y+1, -z-1.]

(100)-projection of the crystal structure of the title compound. Colour scheme: (SO₄) tetrahedra yellow, [Ni(OH₂)₆] octahedra red, O blue, N green, C grey and H colourless. H···O bonds up to 1.8 Å are given as orange dashed lines and from 1.85 to 2.7 Å as light-blue dashed lines.

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

Crystal data top

(C₂H₈N)₂[Ni(H₂O)₆](SO₄)₂·2H₂O	F(000) = 1032
M_r = 487.13	D_x = 1.660 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 25 reflections
a = 8.9363 (6) Å	θ = 5.5–10.1°
b = 13.2370 (8) Å	µ = 1.28 mm⁻¹
c = 16.4810 (14) Å	T = 295 K
V = 1949.5 (2) Å³	Prism, light green
Z = 4	0.29 × 0.27 × 0.26 mm

Data collection top

Enraf–Nonius MACH3 diffractometer	962 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.107
Graphite monochromator	θ_max = 25.0°, θ_min = 2.5°
/w2/q scans	h = −10→10
Absorption correction: ψ scan (North et al., 1968)	k = −15→15
T_min = 0.935, T_max = 0.999	l = −19→19
4902 measured reflections	3 standard reflections every 100 reflections
1719 independent reflections	intensity decay: 0.3%

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)] = 0.040	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.123	w = 1/[σ²(F_o²) + (0.0578P)² + 0.0324P] where P = (F_o² + 2F_c²)/3
S = 1.07	(Δ/σ)_max < 0.001
1719 reflections	Δρ_max = 0.44 e Å⁻³
148 parameters	Δρ_min = −0.41 e Å⁻³
8 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0267 (19)

Crystal data top

(C₂H₈N)₂[Ni(H₂O)₆](SO₄)₂·2H₂O	V = 1949.5 (2) Å³
M_r = 487.13	Z = 4
Orthorhombic, Pbca	Mo Kα radiation
a = 8.9363 (6) Å	µ = 1.28 mm⁻¹
b = 13.2370 (8) Å	T = 295 K
c = 16.4810 (14) Å	0.29 × 0.27 × 0.26 mm

Data collection top

Enraf–Nonius MACH3 diffractometer	962 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.107
T_min = 0.935, T_max = 0.999	3 standard reflections every 100 reflections
4902 measured reflections	intensity decay: 0.3%
1719 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.040	8 restraints
wR(F²) = 0.123	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	Δρ_max = 0.44 e Å⁻³
1719 reflections	Δρ_min = −0.41 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
Ni	0.0000	0.5000	−0.5000	0.0269 (3)
S1	0.44455 (15)	0.65768 (10)	−0.40485 (8)	0.0314 (4)
O1	0.3690 (4)	0.7003 (3)	−0.4766 (2)	0.0446 (11)
O2	0.3354 (4)	0.6104 (3)	−0.3508 (2)	0.0424 (11)
O3	0.5247 (5)	0.7376 (3)	−0.3626 (3)	0.0617 (13)
O4	0.5509 (6)	0.5805 (3)	−0.4313 (3)	0.0764 (16)
O5	−0.0494 (5)	0.4469 (3)	−0.6145 (2)	0.0382 (10)
H51	−0.150 (3)	0.420 (4)	−0.619 (3)	0.06 (2)*
H52	0.023 (7)	0.401 (5)	−0.639 (5)	0.12 (3)*
O6	0.1383 (4)	0.6054 (3)	−0.5541 (2)	0.0339 (9)
H61	0.090 (6)	0.656 (3)	−0.588 (3)	0.07 (2)*
H62	0.209 (5)	0.639 (4)	−0.518 (3)	0.07 (2)*
O7	0.1783 (4)	0.4042 (3)	−0.4930 (2)	0.0379 (9)
H71	0.264 (4)	0.415 (5)	−0.528 (3)	0.07 (2)*
H72	0.169 (9)	0.3310 (10)	−0.490 (4)	0.11 (3)*
O8	0.1689 (5)	0.3224 (4)	−0.6862 (2)	0.0535 (12)
H81	0.275 (2)	0.311 (5)	−0.676 (4)	0.10 (3)*
H82	0.177 (10)	0.361 (5)	−0.736 (3)	0.12 (3)*
N3	0.0336 (6)	0.1126 (4)	−0.6424 (3)	0.0537 (15)
H3A	0.1022	0.1550	−0.6213	0.064*
H3B	0.0189	0.0628	−0.6061	0.064*
C1	0.0946 (11)	0.0689 (5)	−0.7152 (5)	0.097 (3)
H1A	0.1864	0.0346	−0.7027	0.145*
H1B	0.1138	0.1214	−0.7541	0.145*
H1C	0.0243	0.0216	−0.7375	0.145*
C2	−0.1071 (8)	0.1681 (6)	−0.6520 (5)	0.071 (2)
H2A	−0.1374	0.1951	−0.6005	0.106*
H2B	−0.1830	0.1231	−0.6720	0.106*
H2C	−0.0930	0.2223	−0.6899	0.106*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.0289 (5)	0.0233 (5)	0.0284 (5)	0.0004 (5)	−0.0020 (4)	0.0003 (5)
S1	0.0293 (7)	0.0309 (7)	0.0340 (8)	−0.0008 (6)	−0.0010 (6)	0.0055 (6)
O1	0.055 (3)	0.040 (2)	0.038 (2)	−0.009 (2)	−0.0177 (19)	0.0099 (18)
O2	0.031 (2)	0.053 (3)	0.043 (2)	−0.0083 (19)	0.0059 (19)	0.007 (2)
O3	0.083 (3)	0.054 (3)	0.047 (3)	−0.033 (3)	−0.027 (2)	0.015 (2)
O4	0.066 (3)	0.059 (3)	0.104 (4)	0.026 (3)	0.040 (3)	0.029 (3)
O5	0.032 (2)	0.045 (2)	0.038 (2)	−0.005 (2)	−0.0017 (19)	−0.0058 (19)
O6	0.036 (2)	0.029 (2)	0.037 (2)	−0.0031 (18)	−0.0059 (18)	0.0067 (18)
O7	0.032 (2)	0.032 (2)	0.050 (3)	0.0070 (18)	0.008 (2)	0.007 (2)
O8	0.041 (3)	0.080 (3)	0.040 (3)	−0.003 (3)	0.000 (2)	−0.008 (3)
N3	0.069 (4)	0.041 (3)	0.051 (3)	0.004 (3)	−0.016 (3)	−0.005 (3)
C1	0.147 (9)	0.049 (5)	0.094 (7)	0.008 (5)	0.065 (6)	0.013 (4)
C2	0.051 (4)	0.078 (6)	0.082 (5)	−0.001 (4)	0.011 (4)	0.021 (5)

Geometric parameters (Å, º) top

Ni—O7ⁱ	2.040 (3)	O7—H71	0.974 (10)
Ni—O7	2.040 (3)	O7—H72	0.975 (10)
Ni—O5	2.061 (4)	O8—H81	0.975 (10)
Ni—O5ⁱ	2.061 (4)	O8—H82	0.976 (10)
Ni—O6	2.066 (4)	N3—C1	1.440 (8)
Ni—O6ⁱ	2.066 (4)	N3—C2	1.464 (8)
S1—O3	1.455 (4)	N3—H3A	0.9000
S1—O4	1.461 (4)	N3—H3B	0.9000
S1—O2	1.461 (4)	C1—H1A	0.9600
S1—O1	1.474 (4)	C1—H1B	0.9600
O5—H51	0.974 (10)	C1—H1C	0.9600
O5—H52	0.976 (10)	C2—H2A	0.9600
O6—H61	0.973 (10)	C2—H2B	0.9600
O6—H62	0.976 (10)	C2—H2C	0.9600

O7ⁱ—Ni—O7	180.0 (2)	Ni—O6—H62	116 (4)
O7ⁱ—Ni—O5	89.60 (16)	H61—O6—H62	109 (5)
O7—Ni—O5	90.40 (16)	Ni—O7—H71	119 (4)
O7ⁱ—Ni—O5ⁱ	90.40 (16)	Ni—O7—H72	123 (5)
O7—Ni—O5ⁱ	89.60 (16)	H71—O7—H72	104 (6)
O5—Ni—O5ⁱ	180.0	H81—O8—H82	99 (6)
O7ⁱ—Ni—O6	91.33 (15)	C1—N3—C2	115.8 (6)
O7—Ni—O6	88.67 (15)	C1—N3—H3A	108.3
O5—Ni—O6	87.90 (15)	C2—N3—H3A	108.3
O5ⁱ—Ni—O6	92.10 (15)	C1—N3—H3B	108.3
O7ⁱ—Ni—O6ⁱ	88.67 (15)	C2—N3—H3B	108.3
O7—Ni—O6ⁱ	91.33 (15)	H3A—N3—H3B	107.4
O5—Ni—O6ⁱ	92.10 (15)	N3—C1—H1A	109.5
O5ⁱ—Ni—O6ⁱ	87.90 (15)	N3—C1—H1B	109.5
O6—Ni—O6ⁱ	180.00 (19)	H1A—C1—H1B	109.5
O3—S1—O4	109.3 (3)	N3—C1—H1C	109.5
O3—S1—O2	110.4 (3)	H1A—C1—H1C	109.5
O4—S1—O2	108.4 (3)	H1B—C1—H1C	109.5
O3—S1—O1	109.3 (2)	N3—C2—H2A	109.5
O4—S1—O1	109.0 (3)	N3—C2—H2B	109.5
O2—S1—O1	110.3 (2)	H2A—C2—H2B	109.5
Ni—O5—H51	113 (3)	N3—C2—H2C	109.5
Ni—O5—H52	117 (5)	H2A—C2—H2C	109.5
H51—O5—H52	110 (6)	H2B—C2—H2C	109.5
Ni—O6—H61	117 (4)

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	0.97 (1)	1.77 (2)	2.727 (5)	166 (5)
O5—H52···O8	0.98 (1)	1.84 (1)	2.814 (6)	176 (7)
O6—H61···O3ⁱⁱ	0.97 (1)	1.73 (2)	2.689 (5)	169 (6)
O6—H62···O1	0.98 (1)	1.78 (2)	2.731 (5)	164 (5)
O7—H71···O4ⁱⁱⁱ	0.97 (1)	1.78 (2)	2.730 (6)	164 (5)
O7—H72···O1^iv	0.98 (1)	1.78 (2)	2.745 (5)	173 (7)
O8—H81···O3ⁱⁱⁱ	0.98 (1)	2.01 (2)	2.962 (6)	166 (6)
O8—H82···O2^v	0.98 (1)	1.93 (3)	2.856 (6)	158 (7)
N3—H3B···O4^vi	0.90	2.02	2.835 (7)	151
N3—H3A···O6^iv	0.90	2.65	3.274 (6)	127

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	0.974 (10)	1.772 (19)	2.727 (5)	166 (5)
O5—H52···O8	0.976 (10)	1.840 (13)	2.814 (6)	176 (7)
O6—H61···O3ⁱⁱ	0.973 (10)	1.728 (16)	2.689 (5)	169 (6)
O6—H62···O1	0.976 (10)	1.78 (2)	2.731 (5)	164 (5)
O7—H71···O4ⁱⁱⁱ	0.974 (10)	1.78 (2)	2.730 (6)	164 (5)
O7—H72···O1^iv	0.975 (10)	1.776 (15)	2.745 (5)	173 (7)
O8—H81···O3ⁱⁱⁱ	0.975 (10)	2.01 (2)	2.962 (6)	166 (6)
O8—H82···O2^v	0.976 (10)	1.93 (3)	2.856 (6)	158 (7)
N3—H3B···O4^vi	0.90	2.02	2.835 (7)	150.8
N3—H3A···O6^iv	0.90	2.65	3.274 (6)	127.0

Experimental details

Crystal data
Chemical formula	(C₂H₈N)₂[Ni(H₂O)₆](SO₄)₂·2H₂O
M_r	487.13
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	295
a, b, c (Å)	8.9363 (6), 13.2370 (8), 16.4810 (14)
V (Å³)	1949.5 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.28
Crystal size (mm)	0.29 × 0.27 × 0.26

Data collection
Diffractometer	Enraf–Nonius MACH3 diffractometer
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.935, 0.999
No. of measured, independent and observed [I > 2σ(I)] reflections	4902, 1719, 962
R_int	0.107
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.123, 1.07
No. of reflections	1719
No. of parameters	148
No. of restraints	8
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.44, −0.41

Computer programs: CAD-4 Software (Enraf–Nonius, 1998), MolEN (Fair, 1990), SIR97 (Altomare et al., 1999), ATOMS (Dowty, 2011), SHELXL97 (Sheldrick, 2008) and puplCIF (Westrip, 2010).

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115–119. Web of Science CrossRef CAS IUCr Journals Google Scholar
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244–247. CrossRef CAS Web of Science IUCr Journals Google Scholar
Dowty, E. (2011). ATOMS. Shape Software, Hidden Valley Road, Kingsport, Tennessee, USA. Google Scholar
Enraf–Nonius (1998). CAD-4 Software. Enraf–Nonius, Delft, The Netherlands. Google Scholar
Fair, C. K. (1990). MolEN. Enraf–Nonius, Delft, The Netherlands. Google Scholar
Grimes, N. W., Kay, H. F. & Webb, M. W. (1963). Acta Cryst. 16, 823–829. CrossRef IUCr Journals Web of Science Google Scholar
Held, P. (2014). Acta Cryst. E70, m119. CSD CrossRef IUCr Journals Google Scholar
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351–359. CrossRef IUCr Journals Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 70| Part 11| November 2014| Pages 403-405

doi:10.1107/S160053681402234X

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

research communications\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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

1. Chemical context

2. Structural commentary

3. Supra­molecular features

4. Synthesis and crystallization

5. Refinement

Supporting information

References

research communications

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

3. Supramolecular features