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Rubidium digadolinium copper tetra­sulfide, RbGd2CuS4, crystallizes in the orthorhombic space group Cmcm and is isostructural with KGd2CuS4. The structure has a three-dimensional tunnel framework, with tunnels built from GdS6 octahedra and CuS4 tetrahedra. These tunnels are filled with Rb atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804016460/wm6025sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804016460/wm6025Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](Cu-S) = 0.001 Å
  • R factor = 0.020
  • wR factor = 0.058
  • Data-to-parameter ratio = 18.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 1 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-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.

Rubidium digadolinium copper tetrasulfide top
Crystal data top
RbGd2CuS4F(000) = 1032
Mr = 591.75Dx = 5.184 Mg m3
Orthorhombic, CmcmMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2c 2Cell parameters from 4160 reflections
a = 4.0030 (3) Åθ = 3.0–28.3°
b = 13.7095 (10) ŵ = 27.44 mm1
c = 13.8146 (10) ÅT = 153 K
V = 758.13 (10) Å3Plate, red
Z = 40.25 × 0.16 × 0.12 mm
Data collection top
Bruker SMART 1000 CCD
diffractometer
546 independent reflections
Radiation source: fine-focus sealed tube542 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
ω scansθmax = 28.3°, θmin = 3.0°
Absorption correction: numerical
face indexed (SHELXTL; Sheldrick, 2003)
h = 55
Tmin = 0.012, Tmax = 0.122k = 1718
4276 measured reflectionsl = 1818
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)] = 0.020 w = 1/[σ2(Fo2) + (0.030P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.058(Δ/σ)max < 0.001
S = 1.40Δρmax = 1.40 e Å3
546 reflectionsΔρmin = 1.20 e Å3
30 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0049 (3)
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
Gd0.00000.365836 (16)0.061990 (17)0.00771 (17)
Rb0.00000.10763 (5)0.25000.0112 (2)
Cu0.00000.83481 (6)0.25000.0102 (2)
S10.00000.42618 (12)0.25000.0085 (3)
S20.00000.26137 (8)0.60954 (8)0.0086 (3)
S30.00000.00000.00000.0101 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd0.0068 (2)0.0103 (2)0.0061 (2)0.0000.0000.00004 (6)
Rb0.0091 (4)0.0119 (4)0.0125 (4)0.0000.0000.000
Cu0.0101 (4)0.0124 (5)0.0081 (4)0.0000.0000.000
S10.0070 (8)0.0127 (7)0.0059 (7)0.0000.0000.000
S20.0078 (5)0.0108 (5)0.0072 (5)0.0000.0000.0005 (4)
S30.0077 (7)0.0131 (8)0.0094 (8)0.0000.0000.0018 (6)
Geometric parameters (Å, º) top
Gd—S12.7259 (6)Cu—S1iv2.3612 (11)
Gd—S2i2.7348 (8)Cu—S1v2.3612 (11)
Gd—S2ii2.7348 (8)Cu—Gdxvii3.3065 (3)
Gd—S2iii2.7688 (11)Cu—Gdv3.3065 (3)
Gd—S3iv2.8500 (2)Cu—Gdxviii3.3065 (3)
Gd—S3v2.8500 (2)Cu—Gdiv3.3065 (3)
Gd—Cuvi3.3065 (3)Cu—Rbv3.7021 (9)
Gd—Cuvii3.3065 (3)Cu—Rbiv3.7021 (9)
Gd—Gdviii4.0030 (3)Cu—Rbxix3.7403 (11)
Gd—Gdix4.0030 (3)S1—Cuvii2.3612 (11)
Gd—Gdx4.0578 (5)S1—Cuvi2.3612 (11)
Gd—Rb4.3905 (6)S1—Gdiii2.7259 (6)
Rb—S1vii3.1928 (14)S1—Rbiv3.1929 (14)
Rb—S1vi3.1928 (14)S1—Rbv3.1929 (14)
Rb—S2xi3.3160 (9)S2—Cuxvi2.3460 (11)
Rb—S2i3.3160 (9)S2—Gdxx2.7348 (8)
Rb—S2ii3.3160 (9)S2—Gdxxi2.7348 (8)
Rb—S2xii3.3160 (9)S2—Gdiii2.7688 (11)
Rb—Cuvi3.7022 (9)S2—Rbxi3.3161 (9)
Rb—Cuvii3.7021 (9)S2—Rbxii3.3161 (9)
Rb—Cuxiii3.7403 (11)S3—Gdxxii2.8500 (2)
Rb—S33.7557 (4)S3—Gdvii2.8500 (2)
Rb—S3xiv3.7557 (4)S3—Gdxxiii2.8500 (2)
Rb—Rbviii4.0030 (3)S3—Gdvi2.8500 (2)
Cu—S2xv2.3460 (11)S3—Rbxxiv3.7557 (4)
Cu—S2xvi2.3460 (11)
S1—Gd—S2i87.98 (3)S2xii—Rb—S3xiv71.016 (19)
S1—Gd—S2ii87.98 (3)Cuvi—Rb—S3xiv109.301 (7)
S2i—Gd—S2ii94.09 (3)Cuvii—Rb—S3xiv109.301 (7)
S1—Gd—S2iii166.52 (4)Cuxiii—Rb—S3xiv66.865 (10)
S2i—Gd—S2iii82.86 (3)S3—Rb—S3xiv133.730 (19)
S2ii—Gd—S2iii82.86 (3)S1vii—Rb—Rbviii128.82 (2)
S1—Gd—S3iv95.19 (3)S1vi—Rb—Rbviii51.18 (2)
S2i—Gd—S3iv176.13 (2)S2xi—Rb—Rbviii52.873 (12)
S2ii—Gd—S3iv88.267 (18)S2i—Rb—Rbviii127.127 (12)
S2iii—Gd—S3iv94.396 (18)S2ii—Rb—Rbviii52.873 (12)
S1—Gd—S3v95.19 (3)S2xii—Rb—Rbviii127.127 (12)
S2i—Gd—S3v88.267 (18)Cuvi—Rb—Rbviii57.273 (10)
S2ii—Gd—S3v176.13 (2)Cuvii—Rb—Rbviii122.726 (10)
S2iii—Gd—S3v94.396 (18)Cuxiii—Rb—Rbviii90.0
S3iv—Gd—S3v89.221 (8)S3—Rb—Rbviii90.0
S1—Gd—Cuvi44.81 (2)S3xiv—Rb—Rbviii90.0
S2i—Gd—Cuvi99.92 (2)S2xv—Cu—S2xvi111.60 (6)
S2ii—Gd—Cuvi44.46 (2)S2xv—Cu—S1iv107.35 (2)
S2iii—Gd—Cuvi127.282 (19)S2xvi—Cu—S1iv107.35 (2)
S3iv—Gd—Cuvi83.912 (11)S2xv—Cu—S1v107.35 (2)
S3v—Gd—Cuvi138.088 (15)S2xvi—Cu—S1v107.35 (2)
S1—Gd—Cuvii44.81 (2)S1iv—Cu—S1v115.92 (8)
S2i—Gd—Cuvii44.46 (2)S2xv—Cu—Gdxvii136.22 (2)
S2ii—Gd—Cuvii99.92 (2)S2xvi—Cu—Gdxvii54.734 (19)
S2iii—Gd—Cuvii127.282 (19)S1iv—Cu—Gdxvii54.453 (10)
S3iv—Gd—Cuvii138.088 (15)S1v—Cu—Gdxvii116.41 (3)
S3v—Gd—Cuvii83.912 (11)S2xv—Cu—Gdv54.734 (19)
Cuvi—Gd—Cuvii74.505 (8)S2xvi—Cu—Gdv136.22 (2)
S1—Gd—Gdviii90.0S1iv—Cu—Gdv116.41 (3)
S2i—Gd—Gdviii137.043 (17)S1v—Cu—Gdv54.453 (10)
S2ii—Gd—Gdviii42.957 (17)Gdxvii—Cu—Gdv165.22 (3)
S2iii—Gd—Gdviii90.0S2xv—Cu—Gdxviii136.22 (2)
S3iv—Gd—Gdviii45.389 (4)S2xvi—Cu—Gdxviii54.734 (19)
S3v—Gd—Gdviii134.610 (4)S1iv—Cu—Gdxviii116.41 (3)
Cuvi—Gd—Gdviii52.748 (4)S1v—Cu—Gdxviii54.453 (10)
Cuvii—Gd—Gdviii127.253 (5)Gdxvii—Cu—Gdxviii74.504 (8)
S1—Gd—Gdix90.0Gdv—Cu—Gdxviii103.536 (9)
S2i—Gd—Gdix42.957 (17)S2xv—Cu—Gdiv54.734 (19)
S2ii—Gd—Gdix137.043 (17)S2xvi—Cu—Gdiv136.22 (2)
S2iii—Gd—Gdix90.0S1iv—Cu—Gdiv54.453 (10)
S3iv—Gd—Gdix134.610 (4)S1v—Cu—Gdiv116.41 (3)
S3v—Gd—Gdix45.389 (4)Gdxvii—Cu—Gdiv103.536 (9)
Cuvi—Gd—Gdix127.253 (4)Gdv—Cu—Gdiv74.504 (8)
Cuvii—Gd—Gdix52.748 (4)Gdxviii—Cu—Gdiv165.22 (3)
Gdviii—Gd—Gdix180.0S2xv—Cu—Rbv61.78 (3)
S1—Gd—Gdx97.30 (4)S2xvi—Cu—Rbv61.78 (3)
S2i—Gd—Gdx132.805 (17)S1iv—Cu—Rbv154.77 (5)
S2ii—Gd—Gdx132.805 (17)S1v—Cu—Rbv89.32 (4)
S2iii—Gd—Gdx96.18 (2)Gdxvii—Cu—Rbv115.816 (18)
S3iv—Gd—Gdx44.610 (4)Gdv—Cu—Rbv77.348 (11)
S3v—Gd—Gdx44.610 (4)Gdxviii—Cu—Rbv77.348 (11)
Cuvi—Gd—Gdx116.627 (16)Gdiv—Cu—Rbv115.816 (18)
Cuvii—Gd—Gdx116.627 (16)S2xv—Cu—Rbiv61.78 (3)
Gdviii—Gd—Gdx90.0S2xvi—Cu—Rbiv61.78 (3)
Gdix—Gd—Gdx90.0S1iv—Cu—Rbiv89.32 (4)
S1—Gd—Rb71.40 (3)S1v—Cu—Rbiv154.77 (5)
S2i—Gd—Rb48.985 (18)Gdxvii—Cu—Rbiv77.348 (11)
S2ii—Gd—Rb48.985 (18)Gdv—Cu—Rbiv115.816 (18)
S2iii—Gd—Rb95.12 (2)Gdxviii—Cu—Rbiv115.816 (18)
S3iv—Gd—Rb134.274 (5)Gdiv—Cu—Rbiv77.348 (11)
S3v—Gd—Rb134.274 (5)Rbv—Cu—Rbiv65.454 (19)
Cuvi—Gd—Rb55.361 (15)S2xv—Cu—Rbxix124.20 (3)
Cuvii—Gd—Rb55.361 (15)S2xvi—Cu—Rbxix124.20 (3)
Gdviii—Gd—Rb90.0S1iv—Cu—Rbxix57.96 (4)
Gdix—Gd—Rb90.0S1v—Cu—Rbxix57.96 (4)
Gdx—Gd—Rb168.698 (10)Gdxvii—Cu—Rbxix82.608 (15)
S1vii—Rb—S1vi77.64 (4)Gdv—Cu—Rbxix82.608 (15)
S1vii—Rb—S2xi143.16 (2)Gdxviii—Cu—Rbxix82.608 (15)
S1vi—Rb—S2xi92.50 (2)Gdiv—Cu—Rbxix82.608 (15)
S1vii—Rb—S2i92.50 (2)Rbv—Cu—Rbxix147.273 (10)
S1vi—Rb—S2i143.16 (2)Rbiv—Cu—Rbxix147.273 (10)
S2xi—Rb—S2i114.42 (4)Cuvii—S1—Cuvi115.92 (8)
S1vii—Rb—S2ii143.16 (2)Cuvii—S1—Gd80.73 (3)
S1vi—Rb—S2ii92.50 (2)Cuvi—S1—Gd80.73 (3)
S2xi—Rb—S2ii71.63 (4)Cuvii—S1—Gdiii80.73 (3)
S2i—Rb—S2ii74.25 (2)Cuvi—S1—Gdiii80.73 (3)
S1vii—Rb—S2xii92.50 (2)Gd—S1—Gdiii144.66 (7)
S1vi—Rb—S2xii143.16 (2)Cuvii—S1—Rbiv160.86 (6)
S2xi—Rb—S2xii74.25 (2)Cuvi—S1—Rbiv83.22 (3)
S2i—Rb—S2xii71.63 (3)Gd—S1—Rbiv103.68 (2)
S2ii—Rb—S2xii114.42 (4)Gdiii—S1—Rbiv103.68 (2)
S1vii—Rb—Cuvi173.91 (2)Cuvii—S1—Rbv83.22 (3)
S1vi—Rb—Cuvi108.45 (2)Cuvi—S1—Rbv160.86 (6)
S2xi—Rb—Cuvi38.564 (19)Gd—S1—Rbv103.68 (2)
S2i—Rb—Cuvi82.57 (2)Gdiii—S1—Rbv103.68 (2)
S2ii—Rb—Cuvi38.564 (19)Rbiv—S1—Rbv77.64 (4)
S2xii—Rb—Cuvi82.57 (2)Cuxvi—S2—Gdxx80.81 (3)
S1vii—Rb—Cuvii108.45 (2)Cuxvi—S2—Gdxxi80.81 (3)
S1vi—Rb—Cuvii173.91 (2)Gdxx—S2—Gdxxi94.09 (3)
S2xi—Rb—Cuvii82.57 (2)Cuxvi—S2—Gdiii176.95 (5)
S2i—Rb—Cuvii38.564 (19)Gdxx—S2—Gdiii97.14 (3)
S2ii—Rb—Cuvii82.57 (2)Gdxxi—S2—Gdiii97.14 (3)
S2xii—Rb—Cuvii38.564 (19)Cuxvi—S2—Rbxi79.65 (3)
Cuvi—Rb—Cuvii65.453 (19)Gdxx—S2—Rbxi158.07 (4)
S1vii—Rb—Cuxiii38.82 (2)Gdxxi—S2—Rbxi92.531 (13)
S1vi—Rb—Cuxiii38.82 (2)Gdiii—S2—Rbxi102.75 (3)
S2xi—Rb—Cuxiii122.790 (19)Cuxvi—S2—Rbxii79.65 (3)
S2i—Rb—Cuxiii122.790 (19)Gdxx—S2—Rbxii92.531 (13)
S2ii—Rb—Cuxiii122.790 (19)Gdxxi—S2—Rbxii158.07 (4)
S2xii—Rb—Cuxiii122.790 (19)Gdiii—S2—Rbxii102.75 (3)
Cuvi—Rb—Cuxiii147.273 (10)Rbxi—S2—Rbxii74.25 (2)
Cuvii—Rb—Cuxiii147.273 (10)Gdxxii—S3—Gdvii180.000 (11)
S1vii—Rb—S372.175 (10)Gdxxii—S3—Gdxxiii89.221 (8)
S1vi—Rb—S372.175 (10)Gdvii—S3—Gdxxiii90.779 (8)
S2xi—Rb—S3138.666 (15)Gdxxii—S3—Gdvi90.779 (8)
S2i—Rb—S371.016 (19)Gdvii—S3—Gdvi89.221 (8)
S2ii—Rb—S371.016 (18)Gdxxiii—S3—Gdvi180.000 (11)
S2xii—Rb—S3138.666 (15)Gdxxii—S3—Rb91.304 (8)
Cuvi—Rb—S3109.301 (7)Gdvii—S3—Rb88.696 (8)
Cuvii—Rb—S3109.301 (7)Gdxxiii—S3—Rb91.304 (8)
Cuxiii—Rb—S366.865 (10)Gdvi—S3—Rb88.696 (8)
S1vii—Rb—S3xiv72.175 (10)Gdxxii—S3—Rbxxiv88.697 (8)
S1vi—Rb—S3xiv72.175 (10)Gdvii—S3—Rbxxiv91.303 (8)
S2xi—Rb—S3xiv71.016 (19)Gdxxiii—S3—Rbxxiv88.697 (8)
S2i—Rb—S3xiv138.666 (15)Gdvi—S3—Rbxxiv91.303 (8)
S2ii—Rb—S3xiv138.666 (15)Rb—S3—Rbxxiv180.0
Symmetry codes: (i) x1/2, y+1/2, z1/2; (ii) x+1/2, y+1/2, z1/2; (iii) x, y, z+1/2; (iv) x+1/2, y+1/2, z; (v) x1/2, y+1/2, z; (vi) x+1/2, y1/2, z; (vii) x1/2, y1/2, z; (viii) x+1, y, z; (ix) x1, y, z; (x) x, y+1, z; (xi) x+1/2, y+1/2, z+1; (xii) x1/2, y+1/2, z+1; (xiii) x, y1, z; (xiv) x, y, z+1/2; (xv) x, y+1, z1/2; (xvi) x, y+1, z+1; (xvii) x+1/2, y+1/2, z+1/2; (xviii) x1/2, y+1/2, z+1/2; (xix) x, y+1, z; (xx) x1/2, y+1/2, z+1/2; (xxi) x+1/2, y+1/2, z+1/2; (xxii) x+1/2, y+1/2, z; (xxiii) x1/2, y+1/2, z; (xxiv) x, y, z.
 

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