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ISSN: 2056-9890

Di­ammonium tricadmium tris­­(sulfate) di­hydroxide dihydrate

aDepartment of Chemistry, East China University of Science and Technology, School of Chemistry and Molecular Engineering, Mei Long Road 130, Shanghai 200237, People's Republic of China
*Correspondence e-mail: yoshikiyin@ecust.edu.cn

(Received 23 March 2011; accepted 7 April 2011; online 13 April 2011)

The title compound, (NH4)2Cd3(SO4)3(OH)2(H2O)2, has been obtained serendipitously. It is isotypic with the heavier alkali analogues M2Cd3(SO4)3(OH)2(H2O)2 (M = K, Rb, Cs). The structure contains two Cd2+ ions, one in a general position and one with site symmetry m. The former Cd2+ ion is coordinated by three O atoms of three SO4 groups, two hydroxide O atoms and one water O atom, the latter Cd2+ ion by four O atoms of four SO4 groups and two hydroxide O atoms, both in a distorted octa­hedral coordination geometry. This arrangement leads to the formation of a layered framework extending parallel to (100), with the ammonium cations situated in the voids. O—H⋯O hydrogen bonds involving the water mol­ecules, hydroxide groups and sulfate O atoms, as well as N—H⋯O hydrogen bonds between ammonium cations and sulfate O atoms consolidate the crystal packing.

Related literature

For the isotypic K and Cs analogues, see: Louer & Louer (1982[Louer, M. & Louer, D. (1982). Rev. Chim. Miner.19, 162-171.]), and for the Rb analogue, see: Swain & Guru Row (2006[Swain, D. & Guru Row, T. N. (2006). Acta Cryst. E62, i74-i76.]).

Experimental

Crystal data
  • (NH4)2Cd3(SO4)3(OH)2(H2O)2

  • Mr = 731.51

  • Orthorhombic, C m c 21

  • a = 18.906 (3) Å

  • b = 7.9483 (11) Å

  • c = 9.9809 (13) Å

  • V = 1499.8 (4) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 4.72 mm−1

  • T = 296 K

  • 0.12 × 0.10 × 0.08 mm

Data collection
  • Bruker SMART CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2003[Sheldrick, G. M. (2003). SADABS. University of Gοttingen, Germany.]) Tmin = 0.601, Tmax = 0.704

  • 7060 measured reflections

  • 1770 independent reflections

  • 1739 reflections with I > 2σ(I)

  • Rint = 0.051

Refinement
  • R[F2 > 2σ(F2)] = 0.027

  • wR(F2) = 0.066

  • S = 1.08

  • 1770 reflections

  • 118 parameters

  • 1 restraint

  • H-atom parameters constrained

  • Δρmax = 0.68 e Å−3

  • Δρmin = −1.31 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 825 Friedel pairs

  • Flack parameter: −0.07 (4)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O10—H10B⋯O7i 0.85 2.25 3.087 (5) 167
O10—H10B⋯O5ii 0.85 2.36 2.985 (6) 131
O9—H9A⋯O6iii 0.85 2.18 3.029 (7) 173
O8—H8A⋯O5ii 0.85 2.56 3.322 (9) 150
O8—H8A⋯O5i 0.85 2.56 3.322 (9) 150
N1—H1B⋯O10iv 0.90 2.26 2.948 (6) 133
N1—H1D⋯O4ii 0.90 2.18 3.077 (5) 180
N1—H1C⋯O4v 0.90 2.19 3.074 (7) 168
N1—H1A⋯O3vi 0.90 2.38 2.995 (6) 126
N1—H1D⋯O2ii 0.90 2.64 3.196 (7) 121
Symmetry codes: (i) [-x+1, -y+1, z-{\script{1\over 2}}]; (ii) [x, -y+1, z-{\script{1\over 2}}]; (iii) x, y-1, z; (iv) x, y+1, z; (v) [-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]; (vi) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z].

Data collection: SMART (Bruker, 2001[Bruker (2001). SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2003[Bruker (2003). SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: Mercury (Macrae et al., 2006[Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.]) and DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The title compound, (NH4)2Cd3(SO4)3(OH)2(H2O)2, (I), formed accidentally under hydrothermal reaction conditions. Our intended target product was to synthesis a coordination compound from 1H-benzimidazole-5,6-dicarboxylate and CdSO4.8/3H2O. The presence of ammonium ions in the finally obtained compound points to an internal redox process that presumably has caused a (partly) reduction of the nitrogen atoms of 1H-benzimidazole-5,6-dicarboxylate or the nitrate anions. (NH4)2Cd3(SO4)3(OH)2(H2O)2 is isotypic with other M2Cd3(SO4)3(OH)2(H2O)2 members (M = K, Cs (Louer & Louer, 1982); M = Rb (Swain & Guru Row, 2006)).

The asymmetric unit of (I) is illustrated in Fig. 1. The crystal structure of (NH4)2Cd3(SO4)3(OH)2(H2O)2 is made up from two different Cd2+ ions (one on a general position (Cd1), one with site symmetry m (Cd2)), two sulfate ions (likewise one on a general position and the other with site symmetry m), two hydroxide groups, one water molecule and one NH4+ cation. Both Cd2+ cations are six-coordinated in an octahedral coordination geometry. Cd2 is coordinated by four sulfate ions and two hydroxide ions, while Cd1 is coordinated by three sulfate ons, two hydroxide anions and one water molecule. There are four types of oxygen atoms in the crystal structure of the title compound. The O3 atom of one SO42- anion is solely bound to the S atom, O8 and O9 represent the oxygen atoms of hydroxide groups shared by three Cd atoms, O10 is the water O atom bound to one Cd atom and all other O atoms represent sulfate O atoms coordinated to only one Cd atom.

As can be seen in Fig. 2, the Cd(1)O6 polyhedra are connected by sharing edges of OH groups. Cd(2)O6 octahedra and SO4 tetrahedra are linked to these dimers via common corners, thus forming a two-dimensional network extending parallel to the bc plane. The NH4+ cations are situated in the voids of the layers. Through formation of N—H···O and O—H···O hydrogen bonds a three-dimensional structure is formed. Since all water and hydroxide groups and most of the sulfate O atoms are involved in hydrogen bonding, the resulting network can be considered as relatively stable (Table 2, Fig. 3).

Related literature top

For the isotypic K and Cs analogues, see: Louer & Louer (1982), and for the Rb analogue, see: Swain & Guru Row (2006).

Experimental top

All reagents were obtained from commercial sources and used without further purification. A mixture of CdSO4.8/3H2O (0.2565 g, 1.0 mmol), 1H-benzimidazole-5,6-dicarboxylate (0.1236 g,0.6 mmol), CH3CN (6 ml) and 4 ml water were added to a 23 ml Teflon-lined stainless container, which was heated to 423 K and held at that temperature for 5 days. After cooling to room temperature in 24 h, colourless crystals were recovered by filtration (yield 49% based on CdSO4.8/3H2O).

Refinement top

The H atoms were localized from a difference Fourier map. Their coordinates were refined independently with O—H distances restrained to 0.85 (2) Å and the H—H = 1.30 (2)Å for the water H atoms. The isotropic temperature parameters of the H atoms were refined with 1.2Ueq of the parent atom. H atoms of the ammonium cation were placed in calculated positions, with N—H = 0.90Å, Uiso(H) = 1.2 Ueq(N). The deepest hole in the final Fourier map is 0.8 Å from Cd2.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2006) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), with displacement parameters shown at the 30% probability level.
[Figure 2] Fig. 2. View of the two-dimensional network structure of (I) parallel to (100) in the polyhedral representation.
[Figure 3] Fig. 3. Three-dimensional supramolecular structure of (I), built up through hydrogen bonding. NH4+ ions have been omitted for clarity.
Diammonium tricadmium tris(sulfate) dihydroxide dihydrate top
Crystal data top
Cd3H6O16S3·2NH4F(000) = 1392
Mr = 731.51Dx = 3.240 Mg m3
Orthorhombic, Cmc21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2Cell parameters from 12815 reflections
a = 18.906 (3) Åθ = 1.7–27.5°
b = 7.9483 (11) ŵ = 4.72 mm1
c = 9.9809 (13) ÅT = 296 K
V = 1499.8 (4) Å3Block, colourless
Z = 40.12 × 0.10 × 0.08 mm
Data collection top
Bruker SMART CCD
diffractometer
1770 independent reflections
Radiation source: fine-focus sealed tube1739 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
ϕ and ω–scansθmax = 27.5°, θmin = 3.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 2424
Tmin = 0.601, Tmax = 0.704k = 1010
7060 measured reflectionsl = 1212
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)] = 0.027H-atom parameters constrained
wR(F2) = 0.066 w = 1/[σ2(Fo2) + (0.0328P)2 + 1.1583P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max < 0.001
1770 reflectionsΔρmax = 0.68 e Å3
118 parametersΔρmin = 1.31 e Å3
1 restraintAbsolute structure: Flack (1983), 825 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.07 (4)
Crystal data top
Cd3H6O16S3·2NH4V = 1499.8 (4) Å3
Mr = 731.51Z = 4
Orthorhombic, Cmc21Mo Kα radiation
a = 18.906 (3) ŵ = 4.72 mm1
b = 7.9483 (11) ÅT = 296 K
c = 9.9809 (13) Å0.12 × 0.10 × 0.08 mm
Data collection top
Bruker SMART CCD
diffractometer
1770 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
1739 reflections with I > 2σ(I)
Tmin = 0.601, Tmax = 0.704Rint = 0.051
7060 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.066Δρmax = 0.68 e Å3
S = 1.08Δρmin = 1.31 e Å3
1770 reflectionsAbsolute structure: Flack (1983), 825 Friedel pairs
118 parametersAbsolute structure parameter: 0.07 (4)
1 restraint
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
Cd10.588435 (18)0.46065 (4)0.29502 (5)0.01981 (11)
Cd20.50000.19102 (5)0.58110 (4)0.01744 (12)
S10.67635 (6)0.30002 (13)0.57340 (14)0.0184 (2)
S20.50000.8103 (2)0.41513 (16)0.0192 (4)
O10.6589 (3)0.4252 (6)0.4718 (4)0.0387 (11)
O20.6223 (2)0.1661 (4)0.5730 (5)0.0299 (8)
O30.7446 (2)0.2229 (5)0.5454 (5)0.0357 (11)
O40.6794 (2)0.3814 (5)0.7053 (4)0.0299 (9)
O50.5621 (3)0.7036 (8)0.4165 (6)0.0583 (18)
O60.50000.9205 (6)0.3000 (7)0.0500 (19)
O70.50000.9098 (6)0.5395 (5)0.0303 (13)
O80.50000.5445 (5)0.1571 (5)0.0192 (11)
H8A0.50000.49220.08280.029*
O90.50000.2910 (6)0.3712 (5)0.0201 (10)
H9A0.50000.18960.34400.030*
O100.6329 (2)0.2327 (5)0.1789 (4)0.0293 (8)
H10A0.66950.24680.13080.044*
H10B0.59850.20250.12970.044*
N10.6921 (3)0.9615 (4)0.3464 (5)0.0238 (10)
H1A0.69500.94570.43560.029*
H1B0.65381.02440.32760.029*
H1C0.73121.01470.31740.029*
H1D0.68830.86120.30520.029*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02190 (18)0.01799 (18)0.01954 (18)0.00123 (11)0.00023 (14)0.00305 (13)
Cd20.0246 (3)0.0116 (2)0.0161 (2)0.0000.0000.00027 (18)
S10.0206 (6)0.0174 (5)0.0172 (5)0.0020 (4)0.0014 (5)0.0002 (4)
S20.0299 (10)0.0120 (7)0.0157 (8)0.0000.0000.0020 (5)
O10.051 (3)0.034 (2)0.032 (2)0.014 (2)0.024 (2)0.0156 (18)
O20.028 (2)0.0217 (15)0.040 (2)0.0028 (14)0.0029 (18)0.0014 (18)
O30.027 (2)0.036 (3)0.045 (2)0.0036 (19)0.0040 (16)0.0123 (17)
O40.036 (2)0.034 (2)0.0201 (17)0.0036 (18)0.0002 (15)0.0073 (15)
O50.059 (4)0.066 (3)0.051 (3)0.042 (3)0.027 (3)0.034 (3)
O60.120 (6)0.016 (2)0.014 (2)0.0000.0000.001 (3)
O70.063 (4)0.011 (2)0.016 (2)0.0000.0000.0070 (19)
O80.031 (3)0.014 (2)0.012 (2)0.0000.0000.0018 (16)
O90.023 (3)0.016 (2)0.021 (2)0.0000.0000.0034 (17)
O100.024 (2)0.0293 (19)0.034 (2)0.0021 (16)0.0009 (16)0.0066 (17)
N10.034 (3)0.016 (2)0.022 (2)0.0022 (15)0.0038 (19)0.0032 (17)
Geometric parameters (Å, º) top
Cd1—O12.228 (4)S2—O61.444 (6)
Cd1—O82.266 (3)S2—O5ii1.449 (5)
Cd1—O92.278 (3)S2—O51.449 (5)
Cd1—O102.309 (4)S2—O71.472 (5)
Cd1—O4i2.310 (4)O4—Cd1v2.310 (4)
Cd1—O52.333 (5)O6—Cd2vi2.358 (6)
Cd1—Cd1ii3.3439 (8)O7—Cd2vii2.274 (5)
Cd2—O8iii2.235 (4)O8—Cd2vi2.235 (4)
Cd2—O92.241 (5)O8—Cd1ii2.266 (3)
Cd2—O7iv2.274 (5)O8—H8A0.8500
Cd2—O22.323 (4)O9—Cd1ii2.278 (3)
Cd2—O2ii2.323 (4)O9—H9A0.8501
Cd2—O6iii2.358 (6)O10—H10A0.8500
Cd2—H9A2.3665O10—H10B0.8501
S1—O31.456 (4)N1—H1A0.9000
S1—O11.459 (4)N1—H1B0.9001
S1—O41.468 (4)N1—H1C0.9001
S1—O21.475 (4)N1—H1D0.9000
O1—Cd1—O8163.57 (18)O2—Cd2—Cd1iii120.64 (10)
O1—Cd1—O995.73 (17)O2ii—Cd2—Cd1iii69.55 (10)
O8—Cd1—O980.52 (14)O6iii—Cd2—Cd1iii76.00 (12)
O1—Cd1—O1094.62 (17)Cd1v—Cd2—Cd1iii51.115 (14)
O8—Cd1—O10101.21 (15)O8iii—Cd2—H9A110.1
O9—Cd1—O1088.27 (16)O9—Cd2—H9A21.0
O1—Cd1—O4i86.03 (15)O7iv—Cd2—H9A79.2
O8—Cd1—O4i98.85 (13)O2—Cd2—H9A88.0
O9—Cd1—O4i175.79 (16)O2ii—Cd2—H9A88.0
O10—Cd1—O4i87.77 (15)O6iii—Cd2—H9A157.7
O1—Cd1—O579.68 (19)Cd1v—Cd2—H9A123.7
O8—Cd1—O585.11 (16)Cd1iii—Cd2—H9A123.7
O9—Cd1—O599.2 (2)O3—S1—O1110.7 (3)
O10—Cd1—O5171.0 (2)O3—S1—O4108.8 (3)
O4i—Cd1—O584.9 (2)O1—S1—O4109.4 (3)
O1—Cd1—Cd1ii126.71 (14)O3—S1—O2108.0 (2)
O8—Cd1—Cd1ii42.45 (9)O1—S1—O2109.5 (3)
O9—Cd1—Cd1ii42.79 (8)O4—S1—O2110.3 (3)
O10—Cd1—Cd1ii111.34 (10)O6—S2—O5ii111.2 (3)
O4i—Cd1—Cd1ii138.11 (10)O6—S2—O5111.2 (3)
O5—Cd1—Cd1ii77.68 (16)O5ii—S2—O5108.3 (6)
O1—Cd1—Cd2vi141.66 (12)O6—S2—O7110.2 (3)
O8—Cd1—Cd2vi30.33 (10)O5ii—S2—O7107.9 (2)
O9—Cd1—Cd2vi106.86 (9)O5—S2—O7107.9 (2)
O10—Cd1—Cd2vi116.18 (10)S1—O1—Cd1140.5 (3)
O4i—Cd1—Cd2vi73.69 (10)S1—O2—Cd2128.9 (2)
O5—Cd1—Cd2vi66.61 (14)S1—O4—Cd1v123.9 (2)
Cd1ii—Cd1—Cd2vi64.443 (7)S2—O5—Cd1130.8 (3)
O8iii—Cd2—O989.07 (18)S2—O6—Cd2vi120.6 (3)
O8iii—Cd2—O7iv170.68 (18)S2—O7—Cd2vii133.0 (3)
O9—Cd2—O7iv100.25 (17)Cd2vi—O8—Cd1ii118.87 (13)
O8iii—Cd2—O295.29 (9)Cd2vi—O8—Cd1118.87 (13)
O9—Cd2—O289.88 (12)Cd1ii—O8—Cd195.09 (18)
O7iv—Cd2—O284.82 (8)Cd2vi—O8—H8A99.4
O8iii—Cd2—O2ii95.29 (9)Cd1ii—O8—H8A112.7
O9—Cd2—O2ii89.88 (12)Cd1—O8—H8A112.7
O7iv—Cd2—O2ii84.82 (9)Cd2—O9—Cd1ii121.45 (15)
O2—Cd2—O2ii169.42 (18)Cd2—O9—Cd1121.45 (15)
O8iii—Cd2—O6iii92.24 (18)Cd1ii—O9—Cd194.41 (17)
O9—Cd2—O6iii178.69 (19)Cd2—O9—H9A87.8
O7iv—Cd2—O6iii78.44 (18)Cd1ii—O9—H9A117.0
O2—Cd2—O6iii90.00 (12)Cd1—O9—H9A117.0
O2ii—Cd2—O6iii90.00 (12)Cd1—O10—H10A118.4
O8iii—Cd2—Cd1v30.80 (7)Cd1—O10—H10B103.5
O9—Cd2—Cd1v105.18 (11)H10A—O10—H10B109.5
O7iv—Cd2—Cd1v143.41 (9)H1A—N1—H1B109.5
O2—Cd2—Cd1v69.55 (10)H1A—N1—H1C109.5
O2ii—Cd2—Cd1v120.64 (10)H1B—N1—H1C109.5
O6iii—Cd2—Cd1v76.00 (12)H1A—N1—H1D109.5
O8iii—Cd2—Cd1iii30.80 (7)H1B—N1—H1D109.5
O9—Cd2—Cd1iii105.18 (11)H1C—N1—H1D109.5
O7iv—Cd2—Cd1iii143.41 (9)
O3—S1—O1—Cd1105.4 (5)O5—S2—O7—Cd2vii121.6 (4)
O4—S1—O1—Cd1134.6 (5)O1—Cd1—O8—Cd2vi72.2 (6)
O2—S1—O1—Cd113.6 (6)O9—Cd1—O8—Cd2vi150.2 (2)
O8—Cd1—O1—S1106.0 (6)O10—Cd1—O8—Cd2vi123.5 (2)
O9—Cd1—O1—S130.2 (6)O4i—Cd1—O8—Cd2vi34.0 (2)
O10—Cd1—O1—S158.5 (6)O5—Cd1—O8—Cd2vi50.0 (3)
O4i—Cd1—O1—S1146.0 (6)Cd1ii—Cd1—O8—Cd2vi127.1 (3)
O5—Cd1—O1—S1128.5 (6)O1—Cd1—O8—Cd1ii54.8 (6)
Cd1ii—Cd1—O1—S162.5 (6)O9—Cd1—O8—Cd1ii23.12 (17)
Cd2vi—Cd1—O1—S1156.8 (4)O10—Cd1—O8—Cd1ii109.44 (16)
O3—S1—O2—Cd2171.0 (3)O4i—Cd1—O8—Cd1ii161.09 (15)
O1—S1—O2—Cd250.3 (4)O5—Cd1—O8—Cd1ii77.1 (2)
O4—S1—O2—Cd270.2 (4)Cd2vi—Cd1—O8—Cd1ii127.1 (3)
O8iii—Cd2—O2—S118.0 (4)O8iii—Cd2—O9—Cd1ii59.33 (18)
O9—Cd2—O2—S171.1 (4)O7iv—Cd2—O9—Cd1ii120.67 (18)
O7iv—Cd2—O2—S1171.4 (4)O2—Cd2—O9—Cd1ii154.6 (2)
O2ii—Cd2—O2—S1159.8 (9)O2ii—Cd2—O9—Cd1ii36.0 (2)
O6iii—Cd2—O2—S1110.2 (4)Cd1v—Cd2—O9—Cd1ii85.89 (17)
Cd1v—Cd2—O2—S135.2 (3)Cd1iii—Cd2—O9—Cd1ii32.8 (2)
Cd1iii—Cd2—O2—S136.5 (4)O8iii—Cd2—O9—Cd159.33 (18)
O3—S1—O4—Cd1v175.6 (3)O7iv—Cd2—O9—Cd1120.67 (18)
O1—S1—O4—Cd1v54.5 (3)O2—Cd2—O9—Cd136.0 (2)
O2—S1—O4—Cd1v66.0 (3)O2ii—Cd2—O9—Cd1154.6 (2)
O6—S2—O5—Cd177.9 (6)Cd1v—Cd2—O9—Cd132.8 (2)
O5ii—S2—O5—Cd144.7 (8)Cd1iii—Cd2—O9—Cd185.89 (17)
O7—S2—O5—Cd1161.1 (5)O1—Cd1—O9—Cd29.6 (2)
O1—Cd1—O5—S2156.4 (6)O8—Cd1—O9—Cd2154.3 (2)
O8—Cd1—O5—S217.4 (6)O10—Cd1—O9—Cd2104.0 (2)
O9—Cd1—O5—S262.2 (6)O5—Cd1—O9—Cd270.9 (2)
O4i—Cd1—O5—S2116.8 (6)Cd1ii—Cd1—O9—Cd2131.3 (3)
Cd1ii—Cd1—O5—S224.9 (5)Cd2vi—Cd1—O9—Cd2139.10 (15)
Cd2vi—Cd1—O5—S242.3 (5)O1—Cd1—O9—Cd1ii140.89 (19)
O5ii—S2—O6—Cd2vi60.4 (3)O8—Cd1—O9—Cd1ii22.97 (17)
O5—S2—O6—Cd2vi60.4 (3)O10—Cd1—O9—Cd1ii124.63 (17)
O7—S2—O6—Cd2vi180.0O5—Cd1—O9—Cd1ii60.45 (19)
O6—S2—O7—Cd2vii0.000 (2)Cd2vi—Cd1—O9—Cd1ii7.76 (18)
O5ii—S2—O7—Cd2vii121.6 (4)
Symmetry codes: (i) x, y+1, z1/2; (ii) x+1, y, z; (iii) x+1, y+1, z+1/2; (iv) x, y1, z; (v) x, y+1, z+1/2; (vi) x+1, y+1, z1/2; (vii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10B···O7vi0.852.253.087 (5)167
O10—H10B···O5i0.852.362.985 (6)131
O9—H9A···O6iv0.852.183.029 (7)173
O8—H8A···O5i0.852.563.322 (9)150
O8—H8A···O5vi0.852.563.322 (9)150
N1—H1B···O10vii0.902.262.948 (6)133
N1—H1D···O4i0.902.183.077 (5)180
N1—H1C···O4viii0.902.193.074 (7)168
N1—H1A···O3ix0.902.382.995 (6)126
N1—H1D···O2i0.902.643.196 (7)121
Symmetry codes: (i) x, y+1, z1/2; (iv) x, y1, z; (vi) x+1, y+1, z1/2; (vii) x, y+1, z; (viii) x+3/2, y+3/2, z1/2; (ix) x+3/2, y+1/2, z.

Experimental details

Crystal data
Chemical formulaCd3H6O16S3·2NH4
Mr731.51
Crystal system, space groupOrthorhombic, Cmc21
Temperature (K)296
a, b, c (Å)18.906 (3), 7.9483 (11), 9.9809 (13)
V3)1499.8 (4)
Z4
Radiation typeMo Kα
µ (mm1)4.72
Crystal size (mm)0.12 × 0.10 × 0.08
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.601, 0.704
No. of measured, independent and
observed [I > 2σ(I)] reflections
7060, 1770, 1739
Rint0.051
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.066, 1.08
No. of reflections1770
No. of parameters118
No. of restraints1
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.68, 1.31
Absolute structureFlack (1983), 825 Friedel pairs
Absolute structure parameter0.07 (4)

Computer programs: SMART (Bruker, 2001), SAINT-Plus (Bruker, 2003), SHELXTL (Sheldrick, 2008), Mercury (Macrae et al., 2006) and DIAMOND (Brandenburg, 2006).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10B···O7i0.852.253.087 (5)167
O10—H10B···O5ii0.852.362.985 (6)131
O9—H9A···O6iii0.852.183.029 (7)173
O8—H8A···O5ii0.852.563.322 (9)150
O8—H8A···O5i0.852.563.322 (9)150
N1—H1B···O10iv0.902.262.948 (6)133
N1—H1D···O4ii0.902.183.077 (5)180
N1—H1C···O4v0.902.193.074 (7)168
N1—H1A···O3vi0.902.382.995 (6)126
N1—H1D···O2ii0.902.643.196 (7)121
Symmetry codes: (i) x+1, y+1, z1/2; (ii) x, y+1, z1/2; (iii) x, y1, z; (iv) x, y+1, z; (v) x+3/2, y+3/2, z1/2; (vi) x+3/2, y+1/2, z.
 

References

First citationBrandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
First citationBruker (2001). SMART. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationBruker (2003). SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationLouer, M. & Louer, D. (1982). Rev. Chim. Miner.19, 162-171.  Google Scholar
First citationMacrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453–457.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSheldrick, G. M. (2003). SADABS. University of Gοttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSwain, D. & Guru Row, T. N. (2006). Acta Cryst. E62, i74–i76.  Web of Science CrossRef IUCr Journals Google Scholar

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