Rb2[WS4] crystallizes in the orthorhombic space group Pnma and is isostructural with Cs2[MoS4], Rb2[MoS4], K2[MoS4] and (NH4)2[WS4]. The structure contains discrete tetrahedral [WS4]2- anions of symmetry m, separated by Rb+ cations. One of the two unique Rb+ cations is surrounded by nine S atoms and the other by ten S atoms.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (W-S) = 0.001 Å
- R factor = 0.023
- wR factor = 0.061
- Data-to-parameter ratio = 27.3
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.94
Alert level C
REFLT03_ALERT_3_C Reflection count < 95% complete
From the CIF: _diffrn_reflns_theta_max 28.89
From the CIF: _diffrn_reflns_theta_full 0.00
From the CIF: _reflns_number_total 1119
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 1190
Completeness (_total/calc) 94.03%
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL.
Dirubidium tetrathiotungstate
top
Crystal data top
Rb2[WS4] | F(000) = 848 |
Mr = 483.03 | Dx = 3.836 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 5262 reflections |
a = 9.6254 (6) Å | θ = 2.7–28.9° |
b = 7.0218 (5) Å | µ = 26.27 mm−1 |
c = 12.3761 (8) Å | T = 153 K |
V = 836.47 (10) Å3 | Plate, yellow |
Z = 4 | 0.25 × 0.12 × 0.03 mm |
Data collection top
Bruker 1000 CCD diffractometer | 1119 independent reflections |
Radiation source: fine-focus sealed tube | 1027 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ω scans | θmax = 28.9°, θmin = 2.7° |
Absorption correction: numerical face-indexed absorption correction using XPREP in SHELXTL (Sheldrick,
2003) | h = −12→12 |
Tmin = 0.027, Tmax = 0.438 | k = −9→9 |
6582 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.023 | w = 1/[σ2(Fo2) + (0.03P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.061 | (Δ/σ)max = 0.001 |
S = 1.33 | Δρmax = 2.40 e Å−3 |
1119 reflections | Δρmin = −3.99 e Å−3 |
41 parameters | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0018 (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 | |
W | 0.247210 (19) | 0.2500 | 0.572267 (18) | 0.01097 (12) | |
Rb1 | 0.46060 (5) | 0.2500 | 0.16753 (5) | 0.01700 (15) | |
Rb2 | 0.65907 (5) | 0.2500 | 0.60935 (5) | 0.01949 (16) | |
S1 | 0.28728 (18) | 0.2500 | 0.39964 (14) | 0.0225 (3) | |
S2 | 0.34374 (10) | −0.00204 (13) | 0.64407 (10) | 0.0208 (2) | |
S3 | 0.02249 (14) | 0.2500 | 0.60702 (13) | 0.0169 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
W | 0.01112 (16) | 0.01050 (16) | 0.01130 (17) | 0.000 | 0.00023 (7) | 0.000 |
Rb1 | 0.0170 (3) | 0.0182 (3) | 0.0158 (3) | 0.000 | −0.0003 (2) | 0.000 |
Rb2 | 0.0175 (3) | 0.0208 (3) | 0.0202 (3) | 0.000 | 0.0030 (2) | 0.000 |
S1 | 0.0258 (7) | 0.0275 (8) | 0.0141 (8) | 0.000 | 0.0023 (7) | 0.000 |
S2 | 0.0197 (5) | 0.0141 (5) | 0.0286 (6) | 0.0004 (3) | −0.0061 (4) | 0.0050 (4) |
S3 | 0.0121 (6) | 0.0234 (7) | 0.0152 (7) | 0.000 | 0.0036 (5) | 0.000 |
Geometric parameters (Å, º) top
W—S1 | 2.1710 (17) | Rb2—S3xiii | 3.4982 (15) |
W—S2i | 2.1875 (10) | Rb2—S2 | 3.5396 (11) |
W—S2 | 2.1875 (9) | Rb2—S2i | 3.5396 (11) |
W—S3 | 2.2053 (14) | Rb2—S1vii | 3.5504 (4) |
W—Rb2 | 3.9908 (6) | Rb2—S1vi | 3.5504 (4) |
W—Rb2ii | 4.0306 (7) | Rb2—S2vi | 3.5873 (14) |
W—Rb1iii | 4.0519 (6) | Rb2—S2xi | 3.5873 (14) |
W—Rb1iv | 4.2092 (4) | Rb2—S3xiv | 3.7483 (17) |
W—Rb1v | 4.2092 (4) | Rb2—S2xv | 3.9503 (13) |
W—Rb2vi | 4.2653 (4) | Rb2—S2xiv | 3.9503 (13) |
W—Rb2vii | 4.2653 (4) | Rb2—Wxiv | 4.0306 (7) |
Rb1—S1viii | 3.2525 (18) | S1—Rb1iii | 3.2525 (18) |
Rb1—S1 | 3.3219 (18) | S1—Rb2vii | 3.5504 (4) |
Rb1—S2ix | 3.4202 (11) | S1—Rb2vi | 3.5504 (4) |
Rb1—S2x | 3.4202 (11) | S2—Rb1iv | 3.4202 (11) |
Rb1—S3viii | 3.4496 (17) | S2—Rb1vi | 3.4663 (12) |
Rb1—S2xi | 3.4663 (12) | S2—Rb2vi | 3.5873 (14) |
Rb1—S2vi | 3.4663 (12) | S2—Rb2ii | 3.9503 (13) |
Rb1—S3xii | 3.5936 (4) | S3—Rb1iii | 3.4496 (17) |
Rb1—S3ix | 3.5936 (4) | S3—Rb2xvi | 3.4982 (15) |
Rb1—Wviii | 4.0519 (6) | S3—Rb1v | 3.5936 (4) |
Rb1—Wix | 4.2092 (4) | S3—Rb1iv | 3.5936 (4) |
Rb1—Wxii | 4.2092 (4) | S3—Rb2ii | 3.7483 (17) |
| | | |
S1—W—S2i | 108.92 (4) | S3viii—Rb1—Wxii | 78.825 (15) |
S1—W—S2 | 108.92 (4) | S2xi—Rb1—Wxii | 91.583 (17) |
S2i—W—S2 | 108.01 (6) | S2vi—Rb1—Wxii | 149.95 (2) |
S1—W—S3 | 111.48 (6) | S3xii—Rb1—Wxii | 31.60 (2) |
S2i—W—S3 | 109.72 (3) | S3ix—Rb1—Wxii | 141.08 (3) |
S2—W—S3 | 109.72 (3) | Wviii—Rb1—Wxii | 96.800 (10) |
S1—W—Rb2 | 86.37 (5) | Wix—Rb1—Wxii | 113.045 (13) |
S2i—W—Rb2 | 62.05 (3) | S3xiii—Rb2—S2 | 149.144 (17) |
S2—W—Rb2 | 62.05 (3) | S3xiii—Rb2—S2i | 149.144 (17) |
S3—W—Rb2 | 162.15 (4) | S2—Rb2—S2i | 60.00 (3) |
S1—W—Rb2ii | 178.08 (5) | S3xiii—Rb2—S1vii | 81.62 (3) |
S2i—W—Rb2ii | 72.08 (3) | S2—Rb2—S1vii | 128.53 (3) |
S2—W—Rb2ii | 72.08 (3) | S2i—Rb2—S1vii | 68.54 (3) |
S3—W—Rb2ii | 66.60 (4) | S3xiii—Rb2—S1vi | 81.62 (3) |
Rb2—W—Rb2ii | 95.546 (11) | S2—Rb2—S1vi | 68.54 (3) |
S1—W—Rb1iii | 53.14 (5) | S2i—Rb2—S1vi | 128.53 (3) |
S2i—W—Rb1iii | 125.93 (3) | S1vii—Rb2—S1vi | 162.89 (6) |
S2—W—Rb1iii | 125.93 (3) | S3xiii—Rb2—S2vi | 90.02 (3) |
S3—W—Rb1iii | 58.34 (4) | S2—Rb2—S2vi | 81.78 (3) |
Rb2—W—Rb1iii | 139.515 (13) | S2i—Rb2—S2vi | 110.02 (2) |
Rb2ii—W—Rb1iii | 124.939 (12) | S1vii—Rb2—S2vi | 116.98 (4) |
S1—W—Rb1iv | 111.10 (2) | S1vi—Rb2—S2vi | 59.58 (3) |
S2i—W—Rb1iv | 139.72 (3) | S3xiii—Rb2—S2xi | 90.02 (3) |
S2—W—Rb1iv | 54.07 (3) | S2—Rb2—S2xi | 110.02 (2) |
S3—W—Rb1iv | 58.620 (11) | S2i—Rb2—S2xi | 81.78 (3) |
Rb2—W—Rb1iv | 116.094 (8) | S1vii—Rb2—S2xi | 59.58 (3) |
Rb2ii—W—Rb1iv | 68.047 (9) | S1vi—Rb2—S2xi | 116.98 (4) |
Rb1iii—W—Rb1iv | 83.200 (10) | S2vi—Rb2—S2xi | 58.07 (3) |
S1—W—Rb1v | 111.10 (2) | S3xiii—Rb2—S3xiv | 111.00 (3) |
S2i—W—Rb1v | 54.07 (3) | S2—Rb2—S3xiv | 65.52 (3) |
S2—W—Rb1v | 139.72 (3) | S2i—Rb2—S3xiv | 65.52 (3) |
S3—W—Rb1v | 58.620 (11) | S1vii—Rb2—S3xiv | 94.61 (3) |
Rb2—W—Rb1v | 116.094 (8) | S1vi—Rb2—S3xiv | 94.61 (3) |
Rb2ii—W—Rb1v | 68.047 (9) | S2vi—Rb2—S3xiv | 144.70 (2) |
Rb1iii—W—Rb1v | 83.200 (10) | S2xi—Rb2—S3xiv | 144.70 (2) |
Rb1iv—W—Rb1v | 113.045 (13) | S3xiii—Rb2—S2xv | 63.67 (3) |
S1—W—Rb2vi | 56.208 (10) | S2—Rb2—S2xv | 121.07 (2) |
S2i—W—Rb2vi | 142.20 (3) | S2i—Rb2—S2xv | 93.90 (2) |
S2—W—Rb2vi | 57.20 (3) | S1vii—Rb2—S2xv | 61.04 (3) |
S3—W—Rb2vi | 108.07 (2) | S1vi—Rb2—S2xv | 113.69 (3) |
Rb2—W—Rb2vi | 81.403 (10) | S2vi—Rb2—S2xv | 153.669 (18) |
Rb2ii—W—Rb2vi | 124.035 (8) | S2xi—Rb2—S2xv | 117.475 (9) |
Rb1iii—W—Rb2vi | 75.997 (9) | S3xiv—Rb2—S2xv | 55.55 (2) |
Rb1iv—W—Rb2vi | 63.994 (10) | S3xiii—Rb2—S2xiv | 63.67 (3) |
Rb1v—W—Rb2vi | 159.178 (12) | S2—Rb2—S2xiv | 93.90 (2) |
S1—W—Rb2vii | 56.208 (10) | S2i—Rb2—S2xiv | 121.07 (2) |
S2i—W—Rb2vii | 57.20 (3) | S1vii—Rb2—S2xiv | 113.69 (3) |
S2—W—Rb2vii | 142.20 (3) | S1vi—Rb2—S2xiv | 61.04 (3) |
S3—W—Rb2vii | 108.07 (2) | S2vi—Rb2—S2xiv | 117.475 (9) |
Rb2—W—Rb2vii | 81.403 (10) | S2xi—Rb2—S2xiv | 153.669 (18) |
Rb2ii—W—Rb2vii | 124.035 (8) | S3xiv—Rb2—S2xiv | 55.55 (2) |
Rb1iii—W—Rb2vii | 75.997 (9) | S2xv—Rb2—S2xiv | 53.23 (3) |
Rb1iv—W—Rb2vii | 159.178 (12) | S3xiii—Rb2—W | 172.92 (3) |
Rb1v—W—Rb2vii | 63.994 (10) | S2—Rb2—W | 33.088 (16) |
Rb2vi—W—Rb2vii | 110.799 (15) | S2i—Rb2—W | 33.088 (16) |
S1viii—Rb1—S1 | 134.95 (4) | S1vii—Rb2—W | 98.10 (3) |
S1viii—Rb1—S2ix | 143.74 (3) | S1vi—Rb2—W | 98.10 (3) |
S1—Rb1—S2ix | 69.10 (3) | S2vi—Rb2—W | 83.797 (19) |
S1viii—Rb1—S2x | 143.74 (3) | S2xi—Rb2—W | 83.797 (19) |
S1—Rb1—S2x | 69.10 (3) | S3xiv—Rb2—W | 76.07 (2) |
S2ix—Rb1—S2x | 61.21 (3) | S2xv—Rb2—W | 122.402 (19) |
S1viii—Rb1—S3viii | 65.25 (4) | S2xiv—Rb2—W | 122.402 (19) |
S1—Rb1—S3viii | 159.80 (4) | S3xiii—Rb2—Wxiv | 78.32 (3) |
S2ix—Rb1—S3viii | 93.69 (3) | S2—Rb2—Wxiv | 93.55 (2) |
S2x—Rb1—S3viii | 93.69 (3) | S2i—Rb2—Wxiv | 93.55 (2) |
S1viii—Rb1—S2xi | 69.31 (3) | S1vii—Rb2—Wxiv | 90.00 (3) |
S1—Rb1—S2xi | 72.01 (3) | S1vi—Rb2—Wxiv | 90.00 (3) |
S2ix—Rb1—S2xi | 141.09 (2) | S2vi—Rb2—Wxiv | 148.902 (17) |
S2x—Rb1—S2xi | 105.47 (3) | S2xi—Rb2—Wxiv | 148.902 (17) |
S3viii—Rb1—S2xi | 124.66 (3) | S3xiv—Rb2—Wxiv | 32.68 (2) |
S1viii—Rb1—S2vi | 69.31 (3) | S2xv—Rb2—Wxiv | 31.795 (16) |
S1—Rb1—S2vi | 72.01 (3) | S2xiv—Rb2—Wxiv | 31.795 (16) |
S2ix—Rb1—S2vi | 105.47 (3) | W—Rb2—Wxiv | 108.756 (14) |
S2x—Rb1—S2vi | 141.09 (2) | W—S1—Rb1iii | 94.57 (6) |
S3viii—Rb1—S2vi | 124.66 (3) | W—S1—Rb1 | 160.09 (7) |
S2xi—Rb1—S2vi | 60.31 (3) | Rb1iii—S1—Rb1 | 105.34 (5) |
S1viii—Rb1—S3xii | 84.43 (2) | W—S1—Rb2vii | 93.25 (3) |
S1—Rb1—S3xii | 101.71 (2) | Rb1iii—S1—Rb2vii | 97.62 (3) |
S2ix—Rb1—S3xii | 121.23 (3) | Rb1—S1—Rb2vii | 84.25 (3) |
S2x—Rb1—S3xii | 61.56 (3) | W—S1—Rb2vi | 93.25 (3) |
S3viii—Rb1—S3xii | 77.70 (3) | Rb1iii—S1—Rb2vi | 97.62 (3) |
S2xi—Rb1—S3xii | 67.97 (3) | Rb1—S1—Rb2vi | 84.25 (3) |
S2vi—Rb1—S3xii | 127.32 (3) | Rb2vii—S1—Rb2vi | 162.89 (6) |
S1viii—Rb1—S3ix | 84.43 (2) | W—S2—Rb1iv | 94.73 (3) |
S1—Rb1—S3ix | 101.71 (3) | W—S2—Rb1vi | 155.56 (5) |
S2ix—Rb1—S3ix | 61.56 (3) | Rb1iv—S2—Rb1vi | 98.77 (3) |
S2x—Rb1—S3ix | 121.23 (3) | W—S2—Rb2 | 84.86 (3) |
S3viii—Rb1—S3ix | 77.70 (3) | Rb1iv—S2—Rb2 | 177.85 (4) |
S2xi—Rb1—S3ix | 127.32 (3) | Rb1vi—S2—Rb2 | 82.35 (2) |
S2vi—Rb1—S3ix | 67.97 (3) | W—S2—Rb2vi | 91.97 (4) |
S3xii—Rb1—S3ix | 155.37 (5) | Rb1iv—S2—Rb2vi | 79.67 (2) |
S1viii—Rb1—Wviii | 32.28 (3) | Rb1vi—S2—Rb2vi | 110.39 (3) |
S1—Rb1—Wviii | 167.24 (3) | Rb2—S2—Rb2vi | 98.22 (3) |
S2ix—Rb1—Wviii | 121.40 (2) | W—S2—Rb2ii | 76.13 (3) |
S2x—Rb1—Wviii | 121.40 (2) | Rb1iv—S2—Rb2ii | 77.12 (2) |
S3viii—Rb1—Wviii | 32.97 (2) | Rb1vi—S2—Rb2ii | 87.12 (3) |
S2xi—Rb1—Wviii | 97.05 (2) | Rb2—S2—Rb2ii | 104.81 (3) |
S2vi—Rb1—Wviii | 97.05 (2) | Rb2vi—S2—Rb2ii | 152.81 (3) |
S3xii—Rb1—Wviii | 79.43 (2) | W—S3—Rb1iii | 88.70 (5) |
S3ix—Rb1—Wviii | 79.43 (2) | W—S3—Rb2xvi | 169.23 (7) |
S1viii—Rb1—Wix | 112.821 (16) | Rb1iii—S3—Rb2xvi | 80.53 (3) |
S1—Rb1—Wix | 90.204 (19) | W—S3—Rb1v | 89.78 (2) |
S2ix—Rb1—Wix | 31.192 (16) | Rb1iii—S3—Rb1v | 102.30 (3) |
S2x—Rb1—Wix | 89.65 (2) | Rb2xvi—S3—Rb1v | 92.50 (2) |
S3viii—Rb1—Wix | 78.825 (15) | W—S3—Rb1iv | 89.78 (2) |
S2xi—Rb1—Wix | 149.95 (2) | Rb1iii—S3—Rb1iv | 102.30 (3) |
S2vi—Rb1—Wix | 91.583 (17) | Rb2xvi—S3—Rb1iv | 92.50 (2) |
S3xii—Rb1—Wix | 141.08 (3) | Rb1v—S3—Rb1iv | 155.37 (5) |
S3ix—Rb1—Wix | 31.60 (2) | W—S3—Rb2ii | 80.71 (4) |
Wviii—Rb1—Wix | 96.800 (10) | Rb1iii—S3—Rb2ii | 169.41 (4) |
S1viii—Rb1—Wxii | 112.821 (16) | Rb2xvi—S3—Rb2ii | 110.06 (4) |
S1—Rb1—Wxii | 90.204 (18) | Rb1v—S3—Rb2ii | 77.82 (3) |
S2ix—Rb1—Wxii | 89.65 (2) | Rb1iv—S3—Rb2ii | 77.82 (3) |
S2x—Rb1—Wxii | 31.192 (16) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) x−1/2, y, −z+3/2; (iii) x−1/2, y, −z+1/2; (iv) −x+1/2, −y, z+1/2; (v) −x+1/2, −y+1, z+1/2; (vi) −x+1, −y, −z+1; (vii) −x+1, −y+1, −z+1; (viii) x+1/2, y, −z+1/2; (ix) −x+1/2, −y, z−1/2; (x) −x+1/2, y+1/2, z−1/2; (xi) −x+1, y+1/2, −z+1; (xii) −x+1/2, −y+1, z−1/2; (xiii) x+1, y, z; (xiv) x+1/2, y, −z+3/2; (xv) x+1/2, −y+1/2, −z+3/2; (xvi) x−1, y, z. |