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The title compound, dirubidium tricadmium tris(sulfate) dihydroxide dihydrate, consists of sheets of CdO6 octahedra and sulfate tetrahedra propagating in the (100) plane, with Rb+ ions in the interlayer positions. It is isostructural with K2Co3(SO4)3(OH)2·2H2O
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 500 K
- Mean (S-O) = 0.011 Å
- R factor = 0.058
- wR factor = 0.138
- Data-to-parameter ratio = 12.2
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O5
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for S2
Alert level C
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.89
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd2
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S1
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 27.29
From the CIF: _reflns_number_total 1616
Count of symmetry unique reflns 951
Completeness (_total/calc) 169.93%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 665
Fraction of Friedel pairs measured 0.699
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and CAMERON (Betteridge et
al.,
2003; software used to prepare material for publication: WinGX (Farrugia, 1999) and PLATON (Spek, 2003).
dirubidium tricadmium tris(sulfate) dihydroxide dihydrate
top
Crystal data top
Rb2Cd3(SO4)3(OH)2·2H2O | F(000) = 1600 |
Mr = 866.43 | Dx = 3.738 Mg m−3 |
Orthorhombic, Cmc21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C 2c -2 | Cell parameters from 746 reflections |
a = 19.116 (4) Å | θ = 0.9–27.3° |
b = 8.0147 (13) Å | µ = 10.88 mm−1 |
c = 10.0475 (17) Å | T = 500 K |
V = 1539.4 (5) Å3 | Block, colourless |
Z = 4 | 0.30 × 0.25 × 0.20 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1616 independent reflections |
Radiation source: fine-focus sealed tube | 1585 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ and ω scans | θmax = 27.3°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −23→23 |
Tmin = 0.043, Tmax = 0.114 | k = −9→9 |
7592 measured reflections | l = −12→12 |
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)] = 0.058 | H-atom parameters constrained |
wR(F2) = 0.138 | w = 1/[σ2(Fo2) + (0.1068P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.18 | (Δ/σ)max < 0.001 |
1616 reflections | Δρmax = 1.95 e Å−3 |
133 parameters | Δρmin = −1.17 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 665 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.04 (2) |
Special details top
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 | Uiso*/Ueq | |
Cd1 | 0.41228 (3) | 0.03574 (8) | 0.83389 (10) | 0.0510 (3) | |
Cd2 | 0.0000 | −0.19241 (11) | 0.55018 (9) | 0.0475 (3) | |
Rb | 0.19167 (7) | 0.03705 (14) | 0.78629 (15) | 0.0732 (4) | |
S1 | 0.32533 (11) | −0.1978 (3) | 1.0587 (3) | 0.0475 (5) | |
S2 | 0.0000 | −0.1875 (4) | 0.2154 (3) | 0.0466 (7) | |
O1 | 0.3225 (5) | −0.1159 (13) | 0.9275 (9) | 0.065 (2) | |
O2 | 0.3796 (4) | −0.3298 (10) | 1.0583 (12) | 0.067 (2) | |
O3 | 0.3412 (5) | −0.0744 (14) | 1.1591 (10) | 0.074 (2) | |
O4 | 0.2582 (4) | −0.2739 (15) | 1.0882 (13) | 0.075 (3) | |
O5 | 0.0000 | −0.0797 (19) | 0.3322 (16) | 0.087 (4) | |
O6 | 0.0000 | −0.0874 (16) | 0.0909 (12) | 0.064 (3) | |
O7 | −0.0587 (6) | −0.2950 (17) | 0.2120 (15) | 0.101 (5) | |
O8 | 0.0000 | −0.4529 (12) | 0.4711 (12) | 0.053 (2) | |
O9 | 0.5000 | 0.2046 (13) | 0.7598 (11) | 0.050 (2) | |
O10W | 0.3672 (5) | 0.2637 (14) | 0.9521 (10) | 0.069 (2) | |
H8 | 0.0000 | −0.5106 | 0.5433 | 0.079* | |
H9 | 0.5000 | 0.1684 | 0.6792 | 0.076* | |
H10A | 0.3245 | 0.2609 | 0.9585 | 0.103* | |
H10B | 0.3880 | 0.3243 | 1.0045 | 0.103* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0500 (4) | 0.0507 (5) | 0.0522 (4) | 0.0020 (2) | −0.0006 (3) | 0.0041 (3) |
Cd2 | 0.0531 (5) | 0.0410 (5) | 0.0483 (5) | 0.000 | 0.000 | −0.0009 (4) |
Rb | 0.0822 (9) | 0.0646 (8) | 0.0728 (8) | −0.0027 (5) | 0.0079 (6) | −0.0081 (6) |
S1 | 0.0447 (9) | 0.0488 (12) | 0.0489 (11) | −0.0029 (8) | −0.0010 (9) | 0.0011 (10) |
S2 | 0.0553 (16) | 0.0370 (16) | 0.0474 (17) | 0.000 | 0.000 | 0.0015 (11) |
O1 | 0.068 (4) | 0.069 (6) | 0.058 (4) | −0.003 (4) | 0.001 (4) | 0.007 (4) |
O2 | 0.060 (4) | 0.056 (4) | 0.085 (6) | 0.005 (3) | −0.004 (4) | −0.002 (4) |
O3 | 0.078 (5) | 0.076 (6) | 0.067 (5) | 0.016 (5) | −0.020 (5) | −0.015 (5) |
O4 | 0.048 (4) | 0.087 (7) | 0.090 (6) | −0.011 (4) | 0.000 (4) | 0.015 (5) |
O5 | 0.151 (13) | 0.058 (6) | 0.053 (6) | 0.000 | 0.000 | −0.004 (7) |
O6 | 0.096 (8) | 0.045 (5) | 0.051 (6) | 0.000 | 0.000 | 0.004 (4) |
O7 | 0.095 (7) | 0.096 (8) | 0.112 (9) | −0.048 (7) | −0.037 (7) | 0.048 (7) |
O8 | 0.061 (6) | 0.041 (6) | 0.055 (6) | 0.000 | 0.000 | −0.002 (4) |
O9 | 0.052 (4) | 0.046 (5) | 0.053 (5) | 0.000 | 0.000 | −0.002 (4) |
O10W | 0.072 (4) | 0.066 (5) | 0.069 (5) | 0.002 (4) | −0.006 (4) | −0.012 (4) |
Geometric parameters (Å, º) top
Cd1—O3i | 2.241 (9) | S1—O2 | 1.483 (8) |
Cd1—O8ii | 2.270 (8) | S2—O7x | 1.416 (10) |
Cd1—O9 | 2.280 (7) | S2—O7 | 1.416 (10) |
Cd1—O1 | 2.303 (9) | S2—O5 | 1.457 (16) |
Cd1—O10W | 2.343 (10) | S2—O6 | 1.486 (12) |
Cd1—O7iii | 2.352 (11) | O1—Rbviii | 3.134 (10) |
Cd2—O8 | 2.234 (10) | O2—Cd2ii | 2.309 (8) |
Cd2—O9iv | 2.262 (11) | O2—Rbii | 3.141 (11) |
Cd2—O6v | 2.280 (13) | O2—Rbviii | 3.235 (11) |
Cd2—O2vi | 2.309 (8) | O3—Cd1xi | 2.241 (9) |
Cd2—O2vii | 2.309 (8) | O3—Rbxi | 3.146 (11) |
Cd2—O5 | 2.370 (16) | O4—Rbxi | 3.030 (13) |
Rb—O10Wviii | 2.974 (11) | O4—Rbii | 3.054 (11) |
Rb—O4i | 3.030 (13) | O4—Rbviii | 3.524 (13) |
Rb—O4vi | 3.054 (11) | O6—Cd2xii | 2.280 (13) |
Rb—O1 | 3.126 (9) | O7—Cd1vii | 2.352 (11) |
Rb—O1ix | 3.134 (10) | O7—Rbxii | 3.360 (16) |
Rb—O2vi | 3.141 (11) | O8—Cd1vi | 2.270 (8) |
Rb—O3i | 3.146 (11) | O8—Cd1vii | 2.270 (8) |
Rb—O2ix | 3.235 (11) | O9—Cd2xiii | 2.262 (11) |
S1—O3 | 1.445 (10) | O9—Cd1xiv | 2.280 (7) |
S1—O4 | 1.452 (9) | O10W—Rbix | 2.974 (11) |
S1—O1 | 1.474 (9) | | |
| | | |
O3i—Cd1—O8ii | 164.5 (4) | O4i—Rb—O2ix | 121.7 (3) |
O3i—Cd1—O9 | 96.2 (3) | O4vi—Rb—O2ix | 155.6 (3) |
O8ii—Cd1—O9 | 80.1 (3) | O1—Rb—O2ix | 94.8 (2) |
O3i—Cd1—O1 | 86.6 (3) | O1ix—Rb—O2ix | 44.6 (2) |
O8ii—Cd1—O1 | 98.5 (3) | O2vi—Rb—O2ix | 127.4 (3) |
O9—Cd1—O1 | 173.9 (4) | O3i—Rb—O2ix | 134.0 (2) |
O3i—Cd1—O10W | 93.8 (4) | O3—S1—O4 | 109.3 (7) |
O8ii—Cd1—O10W | 101.1 (4) | O3—S1—O1 | 109.1 (6) |
O9—Cd1—O10W | 88.4 (4) | O4—S1—O1 | 109.7 (6) |
O1—Cd1—O10W | 86.0 (4) | O3—S1—O2 | 110.1 (6) |
O3i—Cd1—O7iii | 81.3 (5) | O4—S1—O2 | 108.6 (6) |
O8ii—Cd1—O7iii | 84.4 (4) | O1—S1—O2 | 109.9 (6) |
O9—Cd1—O7iii | 98.3 (5) | O7x—S2—O7 | 104.9 (12) |
O1—Cd1—O7iii | 87.4 (5) | O7x—S2—O5 | 112.4 (8) |
O10W—Cd1—O7iii | 172.0 (4) | O7—S2—O5 | 112.4 (8) |
O8—Cd2—O9iv | 89.4 (4) | O7x—S2—O6 | 107.9 (6) |
O8—Cd2—O6v | 169.5 (5) | O7—S2—O6 | 107.9 (6) |
O9iv—Cd2—O6v | 101.0 (4) | O5—S2—O6 | 111.0 (8) |
O8—Cd2—O2vi | 94.9 (2) | S1—O1—Cd1 | 125.0 (5) |
O9iv—Cd2—O2vi | 89.7 (3) | S1—O1—Rb | 127.6 (5) |
O6v—Cd2—O2vi | 85.3 (2) | Cd1—O1—Rb | 101.8 (3) |
O8—Cd2—O2vii | 94.9 (2) | S1—O1—Rbviii | 90.7 (5) |
O9iv—Cd2—O2vii | 89.7 (3) | Cd1—O1—Rbviii | 110.4 (3) |
O6v—Cd2—O2vii | 85.3 (2) | Rb—O1—Rbviii | 94.2 (2) |
O2vi—Cd2—O2vii | 170.3 (4) | S1—O2—Cd2ii | 130.0 (5) |
O8—Cd2—O5 | 91.6 (5) | S1—O2—Rbii | 94.1 (5) |
O9iv—Cd2—O5 | 179.0 (5) | Cd2ii—O2—Rbii | 119.9 (4) |
O6v—Cd2—O5 | 77.9 (5) | S1—O2—Rbviii | 86.7 (5) |
O2vi—Cd2—O5 | 90.2 (3) | Cd2ii—O2—Rbviii | 114.6 (4) |
O2vii—Cd2—O5 | 90.2 (3) | Rbii—O2—Rbviii | 105.0 (2) |
O10Wviii—Rb—O4i | 171.3 (3) | S1—O3—Cd1xi | 140.3 (6) |
O10Wviii—Rb—O4vi | 88.6 (3) | S1—O3—Rbxi | 99.0 (5) |
O4i—Rb—O4vi | 82.7 (3) | Cd1xi—O3—Rbxi | 102.7 (4) |
O10Wviii—Rb—O1 | 76.1 (3) | S1—O4—Rbxi | 104.0 (6) |
O4i—Rb—O1 | 102.0 (2) | S1—O4—Rbii | 98.4 (5) |
O4vi—Rb—O1 | 76.9 (3) | Rbxi—O4—Rbii | 97.8 (4) |
O10Wviii—Rb—O1ix | 111.6 (2) | S1—O4—Rbviii | 76.4 (5) |
O4i—Rb—O1ix | 77.2 (3) | Rbxi—O4—Rbviii | 161.6 (4) |
O4vi—Rb—O1ix | 159.2 (3) | Rbii—O4—Rbviii | 100.3 (3) |
O1—Rb—O1ix | 102.2 (3) | S2—O5—Cd2 | 121.2 (9) |
O10Wviii—Rb—O2vi | 81.6 (3) | S2—O6—Cd2xii | 133.0 (7) |
O4i—Rb—O2vi | 92.0 (3) | S2—O7—Cd1vii | 132.3 (7) |
O4vi—Rb—O2vi | 45.2 (2) | S2—O7—Rbxii | 102.7 (8) |
O1—Rb—O2vi | 118.1 (2) | Cd1vii—O7—Rbxii | 102.2 (5) |
O1ix—Rb—O2vi | 139.6 (2) | Cd2—O8—Cd1vi | 119.3 (3) |
O10Wviii—Rb—O3i | 129.9 (3) | Cd2—O8—Cd1vii | 119.3 (3) |
O4i—Rb—O3i | 45.0 (3) | Cd1vi—O8—Cd1vii | 95.2 (4) |
O4vi—Rb—O3i | 61.0 (3) | Cd2xiii—O9—Cd1xiv | 121.4 (3) |
O1—Rb—O3i | 59.6 (2) | Cd2xiii—O9—Cd1 | 121.4 (3) |
O1ix—Rb—O3i | 100.3 (3) | Cd1xiv—O9—Cd1 | 94.7 (4) |
O2vi—Rb—O3i | 98.5 (3) | Cd1—O10W—Rbix | 115.5 (4) |
O10Wviii—Rb—O2ix | 67.1 (2) | | |
Symmetry codes: (i) x, −y, z−1/2; (ii) −x+1/2, −y−1/2, z+1/2; (iii) x+1/2, −y−1/2, z+1/2; (iv) x−1/2, y−1/2, z; (v) −x, −y, z+1/2; (vi) −x+1/2, −y−1/2, z−1/2; (vii) x−1/2, −y−1/2, z−1/2; (viii) −x+1/2, y−1/2, z; (ix) −x+1/2, y+1/2, z; (x) −x, y, z; (xi) x, −y, z+1/2; (xii) −x, −y, z−1/2; (xiii) x+1/2, y+1/2, z; (xiv) −x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H8···O7xv | 0.86 | 2.56 | 3.347 (18) | 152 |
O8—H8···O7xvi | 0.86 | 2.56 | 3.347 (18) | 152 |
O10W—H10A···O4ix | 0.82 | 2.07 | 2.776 (13) | 145 |
O10W—H10B···O6xvii | 0.82 | 2.42 | 3.133 (12) | 147 |
O10W—H10B···O6xviii | 0.82 | 2.42 | 3.133 (12) | 147 |
O10W—H10B···O7xvii | 0.82 | 2.51 | 3.008 (17) | 120 |
Symmetry codes: (ix) −x+1/2, y+1/2, z; (xv) −x, −y−1, z+1/2; (xvi) x, −y−1, z+1/2; (xvii) x+1/2, y+1/2, z+1; (xviii) −x+1/2, y+1/2, z+1. |
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