Download citation
Download citation
link to html
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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804000169/wm6008sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804000169/wm6008Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](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

Computing details top

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 = 483.03Dx = 3.836 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 5262 reflections
a = 9.6254 (6) Åθ = 2.7–28.9°
b = 7.0218 (5) ŵ = 26.27 mm1
c = 12.3761 (8) ÅT = 153 K
V = 836.47 (10) Å3Plate, yellow
Z = 40.25 × 0.12 × 0.03 mm
Data collection top
Bruker 1000 CCD
diffractometer
1119 independent reflections
Radiation source: fine-focus sealed tube1027 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
ω scansθmax = 28.9°, θmin = 2.7°
Absorption correction: numerical
face-indexed absorption correction using XPREP in SHELXTL (Sheldrick, 2003)
h = 1212
Tmin = 0.027, Tmax = 0.438k = 99
6582 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary 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 = 1.33Δρmax = 2.40 e Å3
1119 reflectionsΔρmin = 3.99 e Å3
41 parametersExtinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction 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
xyzUiso*/Ueq
W0.247210 (19)0.25000.572267 (18)0.01097 (12)
Rb10.46060 (5)0.25000.16753 (5)0.01700 (15)
Rb20.65907 (5)0.25000.60935 (5)0.01949 (16)
S10.28728 (18)0.25000.39964 (14)0.0225 (3)
S20.34374 (10)0.00204 (13)0.64407 (10)0.0208 (2)
S30.02249 (14)0.25000.60702 (13)0.0169 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W0.01112 (16)0.01050 (16)0.01130 (17)0.0000.00023 (7)0.000
Rb10.0170 (3)0.0182 (3)0.0158 (3)0.0000.0003 (2)0.000
Rb20.0175 (3)0.0208 (3)0.0202 (3)0.0000.0030 (2)0.000
S10.0258 (7)0.0275 (8)0.0141 (8)0.0000.0023 (7)0.000
S20.0197 (5)0.0141 (5)0.0286 (6)0.0004 (3)0.0061 (4)0.0050 (4)
S30.0121 (6)0.0234 (7)0.0152 (7)0.0000.0036 (5)0.000
Geometric parameters (Å, º) top
W—S12.1710 (17)Rb2—S3xiii3.4982 (15)
W—S2i2.1875 (10)Rb2—S23.5396 (11)
W—S22.1875 (9)Rb2—S2i3.5396 (11)
W—S32.2053 (14)Rb2—S1vii3.5504 (4)
W—Rb23.9908 (6)Rb2—S1vi3.5504 (4)
W—Rb2ii4.0306 (7)Rb2—S2vi3.5873 (14)
W—Rb1iii4.0519 (6)Rb2—S2xi3.5873 (14)
W—Rb1iv4.2092 (4)Rb2—S3xiv3.7483 (17)
W—Rb1v4.2092 (4)Rb2—S2xv3.9503 (13)
W—Rb2vi4.2653 (4)Rb2—S2xiv3.9503 (13)
W—Rb2vii4.2653 (4)Rb2—Wxiv4.0306 (7)
Rb1—S1viii3.2525 (18)S1—Rb1iii3.2525 (18)
Rb1—S13.3219 (18)S1—Rb2vii3.5504 (4)
Rb1—S2ix3.4202 (11)S1—Rb2vi3.5504 (4)
Rb1—S2x3.4202 (11)S2—Rb1iv3.4202 (11)
Rb1—S3viii3.4496 (17)S2—Rb1vi3.4663 (12)
Rb1—S2xi3.4663 (12)S2—Rb2vi3.5873 (14)
Rb1—S2vi3.4663 (12)S2—Rb2ii3.9503 (13)
Rb1—S3xii3.5936 (4)S3—Rb1iii3.4496 (17)
Rb1—S3ix3.5936 (4)S3—Rb2xvi3.4982 (15)
Rb1—Wviii4.0519 (6)S3—Rb1v3.5936 (4)
Rb1—Wix4.2092 (4)S3—Rb1iv3.5936 (4)
Rb1—Wxii4.2092 (4)S3—Rb2ii3.7483 (17)
S1—W—S2i108.92 (4)S3viii—Rb1—Wxii78.825 (15)
S1—W—S2108.92 (4)S2xi—Rb1—Wxii91.583 (17)
S2i—W—S2108.01 (6)S2vi—Rb1—Wxii149.95 (2)
S1—W—S3111.48 (6)S3xii—Rb1—Wxii31.60 (2)
S2i—W—S3109.72 (3)S3ix—Rb1—Wxii141.08 (3)
S2—W—S3109.72 (3)Wviii—Rb1—Wxii96.800 (10)
S1—W—Rb286.37 (5)Wix—Rb1—Wxii113.045 (13)
S2i—W—Rb262.05 (3)S3xiii—Rb2—S2149.144 (17)
S2—W—Rb262.05 (3)S3xiii—Rb2—S2i149.144 (17)
S3—W—Rb2162.15 (4)S2—Rb2—S2i60.00 (3)
S1—W—Rb2ii178.08 (5)S3xiii—Rb2—S1vii81.62 (3)
S2i—W—Rb2ii72.08 (3)S2—Rb2—S1vii128.53 (3)
S2—W—Rb2ii72.08 (3)S2i—Rb2—S1vii68.54 (3)
S3—W—Rb2ii66.60 (4)S3xiii—Rb2—S1vi81.62 (3)
Rb2—W—Rb2ii95.546 (11)S2—Rb2—S1vi68.54 (3)
S1—W—Rb1iii53.14 (5)S2i—Rb2—S1vi128.53 (3)
S2i—W—Rb1iii125.93 (3)S1vii—Rb2—S1vi162.89 (6)
S2—W—Rb1iii125.93 (3)S3xiii—Rb2—S2vi90.02 (3)
S3—W—Rb1iii58.34 (4)S2—Rb2—S2vi81.78 (3)
Rb2—W—Rb1iii139.515 (13)S2i—Rb2—S2vi110.02 (2)
Rb2ii—W—Rb1iii124.939 (12)S1vii—Rb2—S2vi116.98 (4)
S1—W—Rb1iv111.10 (2)S1vi—Rb2—S2vi59.58 (3)
S2i—W—Rb1iv139.72 (3)S3xiii—Rb2—S2xi90.02 (3)
S2—W—Rb1iv54.07 (3)S2—Rb2—S2xi110.02 (2)
S3—W—Rb1iv58.620 (11)S2i—Rb2—S2xi81.78 (3)
Rb2—W—Rb1iv116.094 (8)S1vii—Rb2—S2xi59.58 (3)
Rb2ii—W—Rb1iv68.047 (9)S1vi—Rb2—S2xi116.98 (4)
Rb1iii—W—Rb1iv83.200 (10)S2vi—Rb2—S2xi58.07 (3)
S1—W—Rb1v111.10 (2)S3xiii—Rb2—S3xiv111.00 (3)
S2i—W—Rb1v54.07 (3)S2—Rb2—S3xiv65.52 (3)
S2—W—Rb1v139.72 (3)S2i—Rb2—S3xiv65.52 (3)
S3—W—Rb1v58.620 (11)S1vii—Rb2—S3xiv94.61 (3)
Rb2—W—Rb1v116.094 (8)S1vi—Rb2—S3xiv94.61 (3)
Rb2ii—W—Rb1v68.047 (9)S2vi—Rb2—S3xiv144.70 (2)
Rb1iii—W—Rb1v83.200 (10)S2xi—Rb2—S3xiv144.70 (2)
Rb1iv—W—Rb1v113.045 (13)S3xiii—Rb2—S2xv63.67 (3)
S1—W—Rb2vi56.208 (10)S2—Rb2—S2xv121.07 (2)
S2i—W—Rb2vi142.20 (3)S2i—Rb2—S2xv93.90 (2)
S2—W—Rb2vi57.20 (3)S1vii—Rb2—S2xv61.04 (3)
S3—W—Rb2vi108.07 (2)S1vi—Rb2—S2xv113.69 (3)
Rb2—W—Rb2vi81.403 (10)S2vi—Rb2—S2xv153.669 (18)
Rb2ii—W—Rb2vi124.035 (8)S2xi—Rb2—S2xv117.475 (9)
Rb1iii—W—Rb2vi75.997 (9)S3xiv—Rb2—S2xv55.55 (2)
Rb1iv—W—Rb2vi63.994 (10)S3xiii—Rb2—S2xiv63.67 (3)
Rb1v—W—Rb2vi159.178 (12)S2—Rb2—S2xiv93.90 (2)
S1—W—Rb2vii56.208 (10)S2i—Rb2—S2xiv121.07 (2)
S2i—W—Rb2vii57.20 (3)S1vii—Rb2—S2xiv113.69 (3)
S2—W—Rb2vii142.20 (3)S1vi—Rb2—S2xiv61.04 (3)
S3—W—Rb2vii108.07 (2)S2vi—Rb2—S2xiv117.475 (9)
Rb2—W—Rb2vii81.403 (10)S2xi—Rb2—S2xiv153.669 (18)
Rb2ii—W—Rb2vii124.035 (8)S3xiv—Rb2—S2xiv55.55 (2)
Rb1iii—W—Rb2vii75.997 (9)S2xv—Rb2—S2xiv53.23 (3)
Rb1iv—W—Rb2vii159.178 (12)S3xiii—Rb2—W172.92 (3)
Rb1v—W—Rb2vii63.994 (10)S2—Rb2—W33.088 (16)
Rb2vi—W—Rb2vii110.799 (15)S2i—Rb2—W33.088 (16)
S1viii—Rb1—S1134.95 (4)S1vii—Rb2—W98.10 (3)
S1viii—Rb1—S2ix143.74 (3)S1vi—Rb2—W98.10 (3)
S1—Rb1—S2ix69.10 (3)S2vi—Rb2—W83.797 (19)
S1viii—Rb1—S2x143.74 (3)S2xi—Rb2—W83.797 (19)
S1—Rb1—S2x69.10 (3)S3xiv—Rb2—W76.07 (2)
S2ix—Rb1—S2x61.21 (3)S2xv—Rb2—W122.402 (19)
S1viii—Rb1—S3viii65.25 (4)S2xiv—Rb2—W122.402 (19)
S1—Rb1—S3viii159.80 (4)S3xiii—Rb2—Wxiv78.32 (3)
S2ix—Rb1—S3viii93.69 (3)S2—Rb2—Wxiv93.55 (2)
S2x—Rb1—S3viii93.69 (3)S2i—Rb2—Wxiv93.55 (2)
S1viii—Rb1—S2xi69.31 (3)S1vii—Rb2—Wxiv90.00 (3)
S1—Rb1—S2xi72.01 (3)S1vi—Rb2—Wxiv90.00 (3)
S2ix—Rb1—S2xi141.09 (2)S2vi—Rb2—Wxiv148.902 (17)
S2x—Rb1—S2xi105.47 (3)S2xi—Rb2—Wxiv148.902 (17)
S3viii—Rb1—S2xi124.66 (3)S3xiv—Rb2—Wxiv32.68 (2)
S1viii—Rb1—S2vi69.31 (3)S2xv—Rb2—Wxiv31.795 (16)
S1—Rb1—S2vi72.01 (3)S2xiv—Rb2—Wxiv31.795 (16)
S2ix—Rb1—S2vi105.47 (3)W—Rb2—Wxiv108.756 (14)
S2x—Rb1—S2vi141.09 (2)W—S1—Rb1iii94.57 (6)
S3viii—Rb1—S2vi124.66 (3)W—S1—Rb1160.09 (7)
S2xi—Rb1—S2vi60.31 (3)Rb1iii—S1—Rb1105.34 (5)
S1viii—Rb1—S3xii84.43 (2)W—S1—Rb2vii93.25 (3)
S1—Rb1—S3xii101.71 (2)Rb1iii—S1—Rb2vii97.62 (3)
S2ix—Rb1—S3xii121.23 (3)Rb1—S1—Rb2vii84.25 (3)
S2x—Rb1—S3xii61.56 (3)W—S1—Rb2vi93.25 (3)
S3viii—Rb1—S3xii77.70 (3)Rb1iii—S1—Rb2vi97.62 (3)
S2xi—Rb1—S3xii67.97 (3)Rb1—S1—Rb2vi84.25 (3)
S2vi—Rb1—S3xii127.32 (3)Rb2vii—S1—Rb2vi162.89 (6)
S1viii—Rb1—S3ix84.43 (2)W—S2—Rb1iv94.73 (3)
S1—Rb1—S3ix101.71 (3)W—S2—Rb1vi155.56 (5)
S2ix—Rb1—S3ix61.56 (3)Rb1iv—S2—Rb1vi98.77 (3)
S2x—Rb1—S3ix121.23 (3)W—S2—Rb284.86 (3)
S3viii—Rb1—S3ix77.70 (3)Rb1iv—S2—Rb2177.85 (4)
S2xi—Rb1—S3ix127.32 (3)Rb1vi—S2—Rb282.35 (2)
S2vi—Rb1—S3ix67.97 (3)W—S2—Rb2vi91.97 (4)
S3xii—Rb1—S3ix155.37 (5)Rb1iv—S2—Rb2vi79.67 (2)
S1viii—Rb1—Wviii32.28 (3)Rb1vi—S2—Rb2vi110.39 (3)
S1—Rb1—Wviii167.24 (3)Rb2—S2—Rb2vi98.22 (3)
S2ix—Rb1—Wviii121.40 (2)W—S2—Rb2ii76.13 (3)
S2x—Rb1—Wviii121.40 (2)Rb1iv—S2—Rb2ii77.12 (2)
S3viii—Rb1—Wviii32.97 (2)Rb1vi—S2—Rb2ii87.12 (3)
S2xi—Rb1—Wviii97.05 (2)Rb2—S2—Rb2ii104.81 (3)
S2vi—Rb1—Wviii97.05 (2)Rb2vi—S2—Rb2ii152.81 (3)
S3xii—Rb1—Wviii79.43 (2)W—S3—Rb1iii88.70 (5)
S3ix—Rb1—Wviii79.43 (2)W—S3—Rb2xvi169.23 (7)
S1viii—Rb1—Wix112.821 (16)Rb1iii—S3—Rb2xvi80.53 (3)
S1—Rb1—Wix90.204 (19)W—S3—Rb1v89.78 (2)
S2ix—Rb1—Wix31.192 (16)Rb1iii—S3—Rb1v102.30 (3)
S2x—Rb1—Wix89.65 (2)Rb2xvi—S3—Rb1v92.50 (2)
S3viii—Rb1—Wix78.825 (15)W—S3—Rb1iv89.78 (2)
S2xi—Rb1—Wix149.95 (2)Rb1iii—S3—Rb1iv102.30 (3)
S2vi—Rb1—Wix91.583 (17)Rb2xvi—S3—Rb1iv92.50 (2)
S3xii—Rb1—Wix141.08 (3)Rb1v—S3—Rb1iv155.37 (5)
S3ix—Rb1—Wix31.60 (2)W—S3—Rb2ii80.71 (4)
Wviii—Rb1—Wix96.800 (10)Rb1iii—S3—Rb2ii169.41 (4)
S1viii—Rb1—Wxii112.821 (16)Rb2xvi—S3—Rb2ii110.06 (4)
S1—Rb1—Wxii90.204 (18)Rb1v—S3—Rb2ii77.82 (3)
S2ix—Rb1—Wxii89.65 (2)Rb1iv—S3—Rb2ii77.82 (3)
S2x—Rb1—Wxii31.192 (16)
Symmetry codes: (i) x, y+1/2, z; (ii) x1/2, y, z+3/2; (iii) x1/2, 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, z1/2; (x) x+1/2, y+1/2, z1/2; (xi) x+1, y+1/2, z+1; (xii) x+1/2, y+1, z1/2; (xiii) x+1, y, z; (xiv) x+1/2, y, z+3/2; (xv) x+1/2, y+1/2, z+3/2; (xvi) x1, y, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds