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Rubidium diholmium tricopper penta­sulfide, RbHo2Cu3S5, crystallizes in the orthorhombic space group Cmcm and is isostructural with RbSm2Ag3Se5. In the asymmetric unit, the site symmetries of atoms Rb, Cu1, and S2 are mm and those of the other atoms are m. The structure has a three-dimensional tunnel framework, with tunnels built from HoS6 octahedra and CuS4 tetrahedra. The tunnels are filled with Rb atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804019786/br6161sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804019786/br6161Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](Cu-S) = 0.001 Å
  • R factor = 0.023
  • wR factor = 0.054
  • Data-to-parameter ratio = 17.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 28.97 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 673 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 709 Completeness (_total/calc) 94.92% PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
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; software used to prepare material for publication: SHELXTL.

rubidium diholmium tricopper pentasulfide top
Crystal data top
RbHo2Cu3S5F(000) = 1352
Mr = 766.25Dx = 5.650 Mg m3
Orthorhombic, CmcmMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2c 2Cell parameters from 4507 reflections
a = 3.9451 (11) Åθ = 2.5–29.0°
b = 13.915 (4) ŵ = 30.77 mm1
c = 16.408 (5) ÅT = 153 K
V = 900.8 (4) Å3Needle, yellow
Z = 40.42 × 0.07 × 0.03 mm
Data collection top
Bruker 1000 CCD
diffractometer
673 independent reflections
Radiation source: fine-focus sealed tube661 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
ω scansθmax = 29.0°, θmin = 2.5°
Absorption correction: numerical
face indexed
h = 55
Tmin = 0.047, Tmax = 0.405k = 1818
5433 measured reflectionsl = 2121
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) = 0.054(Δ/σ)max = 0.001
S = 1.39Δρmax = 2.37 e Å3
673 reflectionsΔρmin = 2.55 e Å3
38 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00404 (19)
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
Rb0.00000.43385 (4)0.25000.00977 (17)
Ho0.00000.307904 (13)0.593727 (13)0.00644 (14)
Cu10.00000.15215 (6)0.25000.0116 (2)
Cu20.00000.08234 (4)0.53920 (4)0.01149 (18)
S10.00000.06208 (8)0.11509 (7)0.0075 (2)
S20.00000.74007 (11)0.25000.0077 (3)
S30.00000.33060 (8)0.06943 (7)0.0075 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb0.0112 (3)0.0090 (3)0.0091 (3)0.0000.0000.000
Ho0.00684 (18)0.00646 (17)0.00601 (19)0.0000.0000.00007 (6)
Cu10.0089 (4)0.0129 (4)0.0131 (4)0.0000.0000.000
Cu20.0110 (3)0.0081 (3)0.0154 (3)0.0000.0000.0008 (2)
S10.0085 (5)0.0058 (5)0.0083 (5)0.0000.0000.0003 (4)
S20.0081 (6)0.0075 (7)0.0074 (7)0.0000.0000.000
S30.0081 (5)0.0071 (4)0.0074 (6)0.0000.0000.0001 (5)
Geometric parameters (Å, º) top
Rb—S33.2929 (15)Cu1—Hoxii3.2826 (7)
Rb—S3i3.2929 (15)Cu1—Hoxiii3.2826 (7)
Rb—S2ii3.3410 (15)Cu1—Rbii3.6218 (12)
Rb—S2iii3.3410 (15)Cu1—Rbiii3.6218 (12)
Rb—S1iv3.4604 (12)Cu2—S1xvi2.3641 (14)
Rb—S1v3.4604 (12)Cu2—S3x2.3674 (8)
Rb—S1vi3.4604 (12)Cu2—S3xi2.3674 (8)
Rb—S1vii3.4604 (12)Cu2—S1i2.5473 (15)
Rb—Cu1vii3.6219 (12)Cu2—Cu2xvii2.6278 (13)
Rb—Cu1vi3.6219 (12)Cu2—Hoxiii3.3137 (8)
Rb—Cu13.9200 (15)Cu2—Hoxii3.3137 (8)
Rb—Rbviii3.9451 (11)Cu2—Rbxii3.9883 (11)
Ho—S2ix2.6497 (8)Cu2—Rbxiii3.9883 (11)
Ho—S3i2.6957 (14)S1—Cu2xviii2.3642 (14)
Ho—S1x2.6995 (9)S1—Cu2i2.5473 (15)
Ho—S1xi2.6995 (9)S1—Hoxv2.6995 (9)
Ho—S3xi2.7865 (10)S1—Hoxiv2.6995 (9)
Ho—S3x2.7865 (10)S1—Rbiii3.4605 (12)
Ho—Cu23.2638 (11)S1—Rbii3.4605 (12)
Ho—Cu1xii3.2826 (7)S2—Cu1vi2.3212 (10)
Ho—Cu1xiii3.2826 (7)S2—Cu1vii2.3212 (10)
Ho—Cu2xiii3.3137 (8)S2—Hoxix2.6496 (8)
Ho—Cu2xii3.3137 (8)S2—Hoix2.6497 (8)
Ho—Hoviii3.9451 (11)S2—Rbvii3.3410 (15)
Cu1—S2iii2.3212 (10)S2—Rbvi3.3410 (15)
Cu1—S2ii2.3212 (10)S3—Cu2xv2.3674 (8)
Cu1—S1i2.5438 (14)S3—Cu2xiv2.3674 (8)
Cu1—S12.5438 (14)S3—Hoi2.6957 (14)
Cu1—Hoxiv3.2825 (7)S3—Hoxiv2.7864 (10)
Cu1—Hoxv3.2825 (7)S3—Hoxv2.7864 (10)
S3—Rb—S3i128.26 (5)S3x—Cu2—S1i105.36 (4)
S3—Rb—S2ii69.38 (2)S3xi—Cu2—S1i105.36 (4)
S3i—Rb—S2ii69.38 (2)Cu2xviii—S1—Cu1151.30 (6)
S3—Rb—S2iii69.38 (2)Cu2xviii—S1—Cu2i64.57 (4)
S3i—Rb—S2iii69.38 (2)Cu1—S1—Cu2i144.13 (5)
S2ii—Rb—S2iii72.37 (4)Cu2xviii—S1—Hoxv120.09 (4)
S3—Rb—S1iv143.184 (17)Cu1—S1—Hoxv77.45 (3)
S3i—Rb—S1iv69.48 (3)Cu2i—S1—Hoxv78.27 (3)
S2ii—Rb—S1iv138.82 (2)Cu2xviii—S1—Hoxiv120.09 (4)
S2iii—Rb—S1iv94.56 (2)Cu1—S1—Hoxiv77.45 (3)
S3—Rb—S1v143.184 (17)Cu2i—S1—Hoxiv78.27 (3)
S3i—Rb—S1v69.48 (3)Hoxv—S1—Hoxiv93.89 (4)
S2ii—Rb—S1v94.56 (2)Cu2xviii—S1—Rbiii84.19 (4)
S2iii—Rb—S1v138.82 (2)Cu1—S1—Rbiii72.38 (3)
S1iv—Rb—S1v69.51 (3)Cu2i—S1—Rbiii133.86 (3)
S3—Rb—S1vi69.48 (3)Hoxv—S1—Rbiii90.69 (2)
S3i—Rb—S1vi143.185 (17)Hoxiv—S1—Rbiii147.69 (4)
S2ii—Rb—S1vi94.57 (2)Cu2xviii—S1—Rbii84.19 (4)
S2iii—Rb—S1vi138.83 (2)Cu1—S1—Rbii72.38 (3)
S1iv—Rb—S1vi117.92 (4)Cu2i—S1—Rbii133.86 (3)
S1v—Rb—S1vi79.54 (4)Hoxv—S1—Rbii147.69 (4)
S3—Rb—S1vii69.48 (3)Hoxiv—S1—Rbii90.69 (2)
S3i—Rb—S1vii143.185 (17)Rbiii—S1—Rbii69.50 (3)
S2ii—Rb—S1vii138.83 (2)Cu1vi—S2—Cu1vii116.38 (7)
S2iii—Rb—S1vii94.57 (2)Cu1vi—S2—Hoxix82.37 (2)
S1iv—Rb—S1vii79.54 (4)Cu1vii—S2—Hoxix82.37 (2)
S1v—Rb—S1vii117.92 (4)Cu1vi—S2—Hoix82.37 (2)
S1vi—Rb—S1vii69.51 (3)Cu1vii—S2—Hoix82.37 (2)
S2ix—Ho—S3i172.13 (4)Hoxix—S2—Hoix150.81 (6)
S2ix—Ho—S1x92.47 (3)Cu1vi—S2—Rbvii157.99 (5)
S3i—Ho—S1x92.89 (3)Cu1vii—S2—Rbvii85.62 (3)
S2ix—Ho—S1xi92.47 (3)Hoxix—S2—Rbvii101.73 (2)
S3i—Ho—S1xi92.89 (3)Hoix—S2—Rbvii101.73 (2)
S1x—Ho—S1xi93.89 (4)Cu1vi—S2—Rbvi85.62 (3)
S2ix—Ho—S3xi87.95 (4)Cu1vii—S2—Rbvi157.99 (5)
S3i—Ho—S3xi86.50 (3)Hoxix—S2—Rbvi101.73 (2)
S1x—Ho—S3xi178.05 (3)Hoix—S2—Rbvi101.73 (2)
S1xi—Ho—S3xi87.99 (3)Rbvii—S2—Rbvi72.37 (4)
S2ix—Ho—S3x87.95 (4)Cu2xv—S3—Cu2xiv112.86 (5)
S3i—Ho—S3x86.50 (3)Cu2xv—S3—Hoi81.48 (3)
S1x—Ho—S3x87.99 (3)Cu2xiv—S3—Hoi81.48 (3)
S1xi—Ho—S3x178.05 (3)Cu2xv—S3—Hoxiv166.85 (4)
S3xi—Ho—S3x90.13 (4)Cu2xiv—S3—Hoxiv78.12 (2)
S2iii—Cu1—S2ii116.38 (7)Hoi—S3—Hoxiv93.50 (3)
S2iii—Cu1—S1i105.051 (19)Cu2xv—S3—Hoxv78.12 (2)
S2ii—Cu1—S1i105.05 (2)Cu2xiv—S3—Hoxv166.85 (4)
S2iii—Cu1—S1105.053 (19)Hoi—S3—Hoxv93.50 (3)
S2ii—Cu1—S1105.053 (19)Hoxiv—S3—Hoxv90.13 (4)
S1i—Cu1—S1120.96 (6)Cu2xv—S3—Rb88.01 (4)
S1xvi—Cu2—S3x108.94 (4)Cu2xiv—S3—Rb88.01 (4)
S1xvi—Cu2—S3xi108.94 (4)Hoi—S3—Rb160.86 (5)
S3x—Cu2—S3xi112.86 (5)Hoxiv—S3—Rb99.97 (3)
S1xvi—Cu2—S1i115.43 (4)Hoxv—S3—Rb99.97 (3)
Symmetry codes: (i) x, y, z+1/2; (ii) x1/2, y1/2, z; (iii) x+1/2, y1/2, z; (iv) x+1/2, y+1/2, z+1/2; (v) x1/2, y+1/2, z+1/2; (vi) x1/2, y+1/2, z; (vii) x+1/2, y+1/2, z; (viii) x+1, y, z; (ix) x, y+1, z+1; (x) x+1/2, y+1/2, z+1/2; (xi) x1/2, y+1/2, z+1/2; (xii) x+1/2, y+1/2, z+1; (xiii) x1/2, y+1/2, z+1; (xiv) x1/2, y+1/2, z1/2; (xv) x+1/2, y+1/2, z1/2; (xvi) x, y, z+1/2; (xvii) x, y, z+1; (xviii) x, y, z1/2; (xix) x, y+1, z1/2.
 

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