Download citation
Download citation
link to html
The title compound was prepared by a solid-state reaction at 1123 K. Its structure is closely related to that of alluaudite. The main structural feature is the presence of infinite chains of edge-sharing Bi2O10 dimers, which are linked by AsO4 tetrahedra to form a framework enclosing two types of channels where K+ cations reside. The X1 site of the alluaudite structure is occupied by K+, whereas the X2 site is empty.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804011353/br6141sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804011353/br6141Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](As-O) = 0.007 Å
  • R factor = 0.026
  • wR factor = 0.051
  • Data-to-parameter ratio = 12.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT213_ALERT_2_B Atom O5 has ADP max/min Ratio ............. 4.60 oblate PLAT213_ALERT_2_B Atom O6 has ADP max/min Ratio ............. 4.80 oblate
Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT731_ALERT_1_C Bond Calc 3.9993(12), Rep 3.9993(3) ...... 4.00 su-Rat BI -K3 1.555 4.555 PLAT731_ALERT_1_C Bond Calc 3.5364(11), Rep 3.5364(5) ...... 2.20 su-Rat AS1 -K2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 3.5364(11), Rep 3.5364(5) ...... 2.20 su-Rat AS1 -K2 1.555 1.556 PLAT731_ALERT_1_C Bond Calc 3.5364(11), Rep 3.5364(5) ...... 2.20 su-Rat K2 -AS1 1.555 1.554 PLAT741_ALERT_1_C Bond Calc 3.5045(10), Rep 3.50440 ...... Missing su K3 -K3 1.555 2.655 PLAT741_ALERT_1_C Bond Calc 3.5045(10), Rep 3.50440 ...... Missing su K3 -K3 1.555 2.656
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 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: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1997); software used to prepare material for publication: SHELXL97.

Tripotassium dibismuth (III) arsenate (V) top
Crystal data top
K3Bi2(AsO4)3F(000) = 1672
Mr = 952.02Dx = 5.140 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 25 reflections
a = 14.030 (2) Åθ = 9.6–14.9°
b = 13.773 (2) ŵ = 37.65 mm1
c = 7.009 (2) ÅT = 293 K
β = 114.71 (2)°Prism, colourless
V = 1230.4 (3) Å30.11 × 0.04 × 0.04 mm
Z = 4
Data collection top
Enraf-Nonius CAD-4
diffractometer
1006 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.021
Graphite monochromatorθmax = 26.0°, θmin = 2.2°
ω–2θ scansh = 1715
Absorption correction: psi-scan
(North et al., 1968)
k = 016
Tmin = 0.164, Tmax = 0.255l = 08
1387 measured reflections2 standard reflections every 120 min
1203 independent reflections intensity decay: 2%
Refinement top
Refinement on F2Primary atom site location: real-space vector search
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026 w = 1/[σ2(Fo2) + (0.01P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.051(Δ/σ)max = 0.001
S = 1.08Δρmax = 1.09 e Å3
1203 reflectionsΔρmin = 1.22 e Å3
95 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00050 (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
Bi0.26492 (2)0.35529 (3)0.33414 (6)0.0074 (1)
As20.74345 (6)0.39168 (7)0.64105 (14)0.0059 (2)
As10.50000.2574 (1)0.75000.0064 (3)
K10.50000.4809 (2)0.25000.0146 (7)
K20.50000.2230 (2)0.25000.0166 (7)
K30.50000.00000.50000.0223 (7)
O10.4261 (5)0.1874 (5)0.829 (1)0.017 (2)
O20.5689 (4)0.3355 (5)0.952 (1)0.012 (2)
O30.8531 (5)0.4344 (5)0.636 (1)0.017 (2)
O40.6725 (5)0.3346 (5)0.408 (1)0.012 (2)
O50.6681 (4)0.4806 (5)0.674 (1)0.011 (1)
O60.7713 (5)0.3113 (5)0.845 (1)0.012 (1)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Bi0.0066 (2)0.0060 (2)0.0089 (2)0.0001 (1)0.0026 (1)0.0008 (2)
As20.0062 (4)0.0035 (5)0.0072 (4)0.0002 (4)0.0022 (3)0.0001 (4)
As10.0049 (6)0.0067 (7)0.0059 (6)0.0000.0005 (5)0.000
K10.012 (1)0.012 (2)0.018 (2)0.0000.005 (1)0.000
K20.012 (1)0.015 (2)0.020 (2)0.0000.004 (1)0.000
K30.017 (1)0.027 (2)0.019 (2)0.005 (2)0.004 (1)0.008 (2)
O10.012 (3)0.018 (4)0.017 (4)0.008 (3)0.004 (3)0.001 (3)
O20.010 (3)0.012 (4)0.013 (3)0.002 (3)0.002 (3)0.008 (3)
O30.012 (3)0.018 (4)0.019 (4)0.003 (3)0.005 (3)0.003 (3)
O40.021 (3)0.007 (4)0.011 (3)0.004 (3)0.009 (3)0.001 (3)
O50.010 (3)0.006 (4)0.020 (4)0.004 (3)0.008 (3)0.003 (3)
O60.017 (3)0.006 (3)0.008 (3)0.001 (3)0.002 (3)0.006 (3)
Geometric parameters (Å, º) top
Bi—O2i2.199 (6)K1—K1iv3.5435 (9)
Bi—O4ii2.231 (6)K2—O42.684 (6)
Bi—O6iii2.296 (7)K2—O4ii2.684 (6)
Bi—O5iv2.457 (7)K2—O1xii2.735 (7)
Bi—O1v2.505 (6)K2—O1i2.735 (7)
Bi—O6i2.579 (7)K2—O3iii2.865 (7)
Bi—K13.9809 (14)K2—O3viii2.865 (7)
Bi—K3vi3.9993 (3)K2—O2xii3.067 (7)
Bi—K24.0217 (15)K2—O2i3.067 (7)
Bi—K1iv4.0526 (18)K2—K3ii3.536 (3)
Bi—K2vii4.3607 (9)K2—K33.536 (3)
As2—O31.663 (6)K2—As1xii3.5364 (5)
As2—O51.694 (6)K3—O3xiv2.681 (7)
As2—O41.709 (6)K3—O3iii2.681 (7)
As2—O61.717 (6)K3—O3viii2.757 (7)
As2—K13.5865 (14)K3—O3xv2.757 (7)
As2—K2viii3.7060 (16)K3—O1xvi2.854 (7)
As2—K3ix3.7336 (8)K3—O1i2.854 (7)
As1—O1i1.668 (7)K3—K3ii3.5044
As1—O11.668 (7)K3—K3i3.5044
As1—O21.716 (6)K3—K2xvii3.536 (3)
As1—O2i1.716 (6)K3—As2xiv3.7336 (9)
As1—K23.5364 (5)K3—As2iii3.7336 (8)
As1—K2x3.5364 (5)O1—Biv2.505 (6)
As1—K1iv3.604 (3)O1—K2x2.735 (7)
As1—K33.9545 (12)O1—K3i2.854 (7)
As1—K3i3.9545 (12)O2—Bii2.199 (6)
K1—O5xi2.681 (6)O2—K1iv2.860 (7)
K1—O5iv2.681 (6)O2—K2x3.067 (7)
K1—O2xi2.860 (7)O2—K1x3.319 (6)
K1—O2iv2.860 (7)O3—K3ix2.681 (7)
K1—O52.919 (6)O3—K3xviii2.757 (7)
K1—O5ii2.919 (6)O3—K2viii2.865 (7)
K1—O4ii2.984 (7)O4—Biii2.231 (6)
K1—O42.984 (7)O5—Biiv2.457 (6)
K1—O2xii3.319 (6)O5—K1iv2.681 (6)
K1—O2i3.319 (7)O6—Bixix2.296 (7)
K1—K1xiii3.5435 (9)O6—Bii2.579 (7)
O2i—Bi—O4ii82.1 (2)O4ii—K2—O1i114.66 (19)
O2i—Bi—O6iii80.7 (2)O1xii—K2—O1i159.4 (3)
O4ii—Bi—O6iii82.8 (2)O4—K2—O3iii165.4 (2)
O2i—Bi—O5iv79.8 (2)O4ii—K2—O3iii84.20 (18)
O4ii—Bi—O5iv79.9 (2)O1xii—K2—O3iii70.0 (2)
O6iii—Bi—O5iv155.5 (2)O1i—K2—O3iii94.1 (2)
O2i—Bi—O1v155.3 (2)O4—K2—O3viii84.20 (18)
O4ii—Bi—O1v108.1 (2)O4ii—K2—O3viii165.4 (2)
O6iii—Bi—O1v78.5 (2)O1xii—K2—O3viii94.1 (2)
O5iv—Bi—O1v123.5 (2)O1i—K2—O3viii70.0 (2)
O2i—Bi—O6i85.1 (2)O3iii—K2—O3viii81.7 (3)
O4ii—Bi—O6i156.6 (2)O4—K2—O2xii60.32 (18)
O6iii—Bi—O6i75.9 (2)O4ii—K2—O2xii85.18 (19)
O5iv—Bi—O6i116.9 (2)O1xii—K2—O2xii55.87 (18)
O1v—Bi—O6i77.2 (2)O1i—K2—O2xii137.89 (19)
O3—As2—O5112.5 (3)O3iii—K2—O2xii125.91 (18)
O3—As2—O4108.4 (3)O3viii—K2—O2xii100.28 (18)
O5—As2—O4108.3 (3)O4—K2—O2i85.18 (19)
O3—As2—O6110.9 (3)O4ii—K2—O2i60.32 (18)
O5—As2—O6107.0 (3)O1xii—K2—O2i137.89 (19)
O4—As2—O6109.7 (3)O1i—K2—O2i55.87 (18)
O1i—As1—O1109.5 (5)O3iii—K2—O2i100.28 (18)
O1i—As1—O2114.8 (3)O3viii—K2—O2i125.91 (18)
O1—As1—O2107.7 (3)O2xii—K2—O2i119.3 (3)
O1i—As1—O2i107.7 (3)O3xiv—K3—O3iii180.0
O1—As1—O2i114.8 (3)O3xiv—K3—O3viii92.9 (2)
O2—As1—O2i102.3 (4)O3iii—K3—O3viii87.1 (2)
O5xi—K1—O5iv157.2 (3)O3xiv—K3—O3xv87.1 (2)
O5xi—K1—O2xi77.30 (19)O3iii—K3—O3xv92.9 (2)
O5iv—K1—O2xi82.58 (19)O3viii—K3—O3xv180.00 (13)
O5xi—K1—O2iv82.58 (19)O3xiv—K3—O1xvi95.5 (2)
O5iv—K1—O2iv77.30 (19)O3iii—K3—O1xvi84.5 (2)
O2xi—K1—O2iv55.8 (2)O3viii—K3—O1xvi110.1 (2)
O5xi—K1—O578.41 (15)O3xv—K3—O1xvi69.9 (2)
O5iv—K1—O5101.62 (14)O3xiv—K3—O1i84.5 (2)
O2xi—K1—O562.38 (18)O3iii—K3—O1i95.5 (2)
O2iv—K1—O5117.8 (2)O3viii—K3—O1i69.9 (2)
O5xi—K1—O5ii101.62 (14)O3xv—K3—O1i110.1 (2)
O5iv—K1—O5ii78.41 (15)O1xvi—K3—O1i180.0 (3)
O2xi—K1—O5ii117.8 (2)As1—O1—Biv132.8 (3)
O2iv—K1—O5ii62.38 (18)As1—O1—K2x104.2 (3)
O5—K1—O5ii179.8 (3)Biv—O1—K2x112.6 (2)
O5xi—K1—O4ii134.7 (2)As1—O1—K3i119.7 (3)
O5iv—K1—O4ii64.08 (18)Biv—O1—K3i96.3 (2)
O2xi—K1—O4ii146.59 (18)K2x—O1—K3i78.46 (19)
O2iv—K1—O4ii111.08 (17)As1—O2—Bii135.3 (3)
O5—K1—O4ii124.15 (19)As1—O2—K1iv101.0 (3)
O5ii—K1—O4ii55.70 (18)Bii—O2—K1iv105.7 (2)
O5xi—K1—O464.08 (18)As1—O2—K2x90.8 (3)
O5iv—K1—O4134.7 (2)Bii—O2—K2x98.2 (2)
O2xi—K1—O4111.08 (17)K1iv—O2—K2x130.2 (2)
O2iv—K1—O4146.59 (18)As1—O2—K1x133.2 (3)
O5—K1—O455.70 (18)Bii—O2—K1x89.99 (19)
O5ii—K1—O4124.15 (19)K1iv—O2—K1x69.54 (14)
O4ii—K1—O495.0 (3)K2x—O2—K1x67.49 (14)
O5xi—K1—O2xii58.71 (18)As2—O3—K3ix116.6 (3)
O5iv—K1—O2xii139.26 (18)As2—O3—K3xviii163.0 (4)
O2xi—K1—O2xii135.8 (2)K3ix—O3—K3xviii80.22 (17)
O2iv—K1—O2xii110.46 (14)As2—O3—K2viii106.8 (3)
O5—K1—O2xii108.39 (16)K3ix—O3—K2viii79.13 (17)
O5ii—K1—O2xii71.50 (16)K3xviii—O3—K2viii77.90 (17)
O4ii—K1—O2xii76.31 (17)As2—O4—Biii114.3 (3)
O4—K1—O2xii54.65 (17)As2—O4—K2136.3 (3)
O5xi—K1—O2i139.26 (18)Biii—O4—K2109.5 (2)
O5iv—K1—O2i58.71 (18)As2—O4—K195.8 (3)
O2xi—K1—O2i110.46 (14)Biii—O4—K198.5 (2)
O2iv—K1—O2i135.8 (2)K2—O4—K177.44 (17)
O5—K1—O2i71.50 (16)As2—O5—Biiv113.4 (3)
O5ii—K1—O2i108.39 (16)As2—O5—K1iv145.1 (3)
O4ii—K1—O2i54.65 (17)Biiv—O5—K1iv101.5 (2)
O4—K1—O2i76.31 (17)As2—O5—K198.6 (3)
O2xii—K1—O2i105.8 (2)Biiv—O5—K197.5 (2)
O4—K2—O4ii110.1 (3)K1iv—O5—K178.38 (14)
O4—K2—O1xii114.7 (2)As2—O6—Bixix128.7 (3)
O4ii—K2—O1xii77.7 (2)As2—O6—Bii120.9 (3)
O4—K2—O1i77.7 (2)Bixix—O6—Bii104.1 (2)
Symmetry codes: (i) x+1, y, z+3/2; (ii) x+1, y, z+1/2; (iii) x1/2, y+1/2, z1/2; (iv) x+1, y+1, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z; (viii) x+3/2, y+1/2, z+1; (ix) x+3/2, y+1/2, z+3/2; (x) x, y, z+1; (xi) x, y+1, z1/2; (xii) x, y, z1; (xiii) x+1, y+1, z; (xiv) x+3/2, y1/2, z+3/2; (xv) x1/2, y1/2, z; (xvi) x, y, z1/2; (xvii) x+1, y, z+1; (xviii) x+1/2, y+1/2, z; (xix) x+1/2, y+1/2, z+1/2.
 

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