Literature DB >> 21754257

Diammonium tricadmium tris-(sulfate) dihydroxide dihydrate.

Xin Yin1.   

Abstract

The title compound, (NH(4))(2)Cd(3)(SO(4))(3)(OH)(2)(H(2)O)(2), has been obtained serendipitously. It is isotypic with the heavier alkali analogues M(2)Cd(3)(SO(4))(3)(OH)(2)(H(2)O)(2) (M = K, Rb, Cs). The structure contains two Cd(2+) ions, one in a general position and one with site symmetry m. The former Cd(2+) ion is coordinated by three O atoms of three SO(4) groups, two hydroxide O atoms and one water O atom, the latter Cd(2+) ion by four O atoms of four SO(4) groups and two hydroxide O atoms, both in a distorted octa-hedral 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 mol-ecules, 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.

Entities:  

Year:  2011        PMID： 21754257      PMCID： PMC3089235          DOI： 10.1107/S1600536811012979

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

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

Experimental

Crystal data

(NH4)2Cd3(SO4)3(OH)2(H2O)2 M = 731.51 Orthorhombic, 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 ▶) T min = 0.601, T max = 0.704 7060 measured reflections 1770 independent reflections 1739 reflections with I > 2σ(I) R int = 0.051

Refinement

R[F 2 > 2σ(F 2)] = 0.027 wR(F 2) = 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 ▶), 825 Friedel pairs Flack parameter: −0.07 (4) Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT-Plus (Bruker, 2003 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: Mercury (Macrae et al., 2006 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811012979/wm2470sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811012979/wm2470Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Cd3H6O16S3·2NH4F(000) = 1392
Mr = 731.51Dx = 3.240 Mg m−3
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 mm−1
c = 9.9809 (13) ÅT = 296 K
V = 1499.8 (4) Å3Block, colourless
Z = 40.12 × 0.10 × 0.08 mm
Bruker SMART CCD diffractometer1770 independent reflections
Radiation source: fine-focus sealed tube1739 reflections with I > 2σ(I)
graphiteRint = 0.051
φ and ω–scansθmax = 27.5°, θmin = 3.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)h = −24→24
Tmin = 0.601, Tmax = 0.704k = −10→10
7060 measured reflectionsl = −12→12
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) = 0.066w = 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 Å−3
118 parametersΔρmin = −1.31 e Å−3
1 restraintAbsolute structure: Flack (1983), 825 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: −0.07 (4)
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.
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*
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)0.0000.000−0.00027 (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)0.0000.000−0.0020 (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)0.0000.000−0.001 (3)
O70.063 (4)0.011 (2)0.016 (2)0.0000.000−0.0070 (19)
O80.031 (3)0.014 (2)0.012 (2)0.0000.000−0.0018 (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)
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—Cd1−134.6 (5)O1—Cd1—O8—Cd2vi72.2 (6)
O2—S1—O1—Cd1−13.6 (6)O9—Cd1—O8—Cd2vi150.2 (2)
O8—Cd1—O1—S1106.0 (6)O10—Cd1—O8—Cd2vi−123.5 (2)
O9—Cd1—O1—S130.2 (6)O4i—Cd1—O8—Cd2vi−34.0 (2)
O10—Cd1—O1—S1−58.5 (6)O5—Cd1—O8—Cd2vi50.0 (3)
O4i—Cd1—O1—S1−146.0 (6)Cd1ii—Cd1—O8—Cd2vi127.1 (3)
O5—Cd1—O1—S1128.5 (6)O1—Cd1—O8—Cd1ii−54.8 (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—Cd2−171.0 (3)O4i—Cd1—O8—Cd1ii−161.09 (15)
O1—S1—O2—Cd2−50.3 (4)O5—Cd1—O8—Cd1ii−77.1 (2)
O4—S1—O2—Cd270.2 (4)Cd2vi—Cd1—O8—Cd1ii−127.1 (3)
O8iii—Cd2—O2—S1−18.0 (4)O8iii—Cd2—O9—Cd1ii−59.33 (18)
O9—Cd2—O2—S171.1 (4)O7iv—Cd2—O9—Cd1ii120.67 (18)
O7iv—Cd2—O2—S1171.4 (4)O2—Cd2—O9—Cd1ii−154.6 (2)
O2ii—Cd2—O2—S1159.8 (9)O2ii—Cd2—O9—Cd1ii36.0 (2)
O6iii—Cd2—O2—S1−110.2 (4)Cd1v—Cd2—O9—Cd1ii−85.89 (17)
Cd1v—Cd2—O2—S1−35.2 (3)Cd1iii—Cd2—O9—Cd1ii−32.8 (2)
Cd1iii—Cd2—O2—S1−36.5 (4)O8iii—Cd2—O9—Cd159.33 (18)
O3—S1—O4—Cd1v175.6 (3)O7iv—Cd2—O9—Cd1−120.67 (18)
O1—S1—O4—Cd1v54.5 (3)O2—Cd2—O9—Cd1−36.0 (2)
O2—S1—O4—Cd1v−66.0 (3)O2ii—Cd2—O9—Cd1154.6 (2)
O6—S2—O5—Cd1−77.9 (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—S2−156.4 (6)O8—Cd1—O9—Cd2−154.3 (2)
O8—Cd1—O5—S217.4 (6)O10—Cd1—O9—Cd2104.0 (2)
O9—Cd1—O5—S2−62.2 (6)O5—Cd1—O9—Cd2−70.9 (2)
O4i—Cd1—O5—S2116.8 (6)Cd1ii—Cd1—O9—Cd2−131.3 (3)
Cd1ii—Cd1—O5—S2−24.9 (5)Cd2vi—Cd1—O9—Cd2−139.10 (15)
Cd2vi—Cd1—O5—S242.3 (5)O1—Cd1—O9—Cd1ii140.89 (19)
O5ii—S2—O6—Cd2vi−60.4 (3)O8—Cd1—O9—Cd1ii−22.97 (17)
O5—S2—O6—Cd2vi60.4 (3)O10—Cd1—O9—Cd1ii−124.63 (17)
O7—S2—O6—Cd2vi180.0O5—Cd1—O9—Cd1ii60.45 (19)
O6—S2—O7—Cd2vii0.000 (2)Cd2vi—Cd1—O9—Cd1ii−7.76 (18)
O5ii—S2—O7—Cd2vii−121.6 (4)
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
Table 1

Hydrogen-bond geometry (Å, °)

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) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .

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