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The structure of In0.87K2Mo15Se19 (indium dipotassium penta­deca­molybdate nona­deca­selenide), isotypic with In2.9Mo15Se19, is characterized by a mixture of Mo6Sei8Sea6 and Mo9Sei11Sea6 cluster units in the ratio 1:1. Both units are inter­connected through additional Mo-Se bonds. In the title compound, K+ replaces the monovalent In positions as observed in In2.9Mo15Se19. One Mo, one Se and the In atom are situated on mirror planes, and two other Se atoms are situated on threefold axes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806052974/wm2077sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806052974/wm2077Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](o-Mo) = 0.001 Å
  • Disorder in main residue
  • R factor = 0.037
  • wR factor = 0.040
  • Data-to-parameter ratio = 39.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc.
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: COLLECT; data reduction: EVALCCD (Duisenberg, 1998); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: JANA2000 (Petříček & Dušek, 2000); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: JANA2000.

indium dipotassium pentadecamolybdate nonadecaselenide top
Crystal data top
In0.875K2Mo15Se19Dx = 6.339 (1) Mg m3
Mr = 3118Mo Kα radiation, λ = 0.71069 Å
Hexagonal, P63/mCell parameters from 45013 reflections
Hall symbol: -P 6cθ = 2.0–40.3°
a = 9.8076 (1) ŵ = 27.57 mm1
c = 19.6036 (3) ÅT = 293 K
V = 1633.02 (3) Å3Irregular block, black
Z = 20.10 × 0.09 × 0.06 mm
F(000) = 2713.6
Data collection top
Nonius KappaCCD area-detector
diffractometer
3409 independent reflections
Radiation source: fine-focus sealed tube2628 reflections with I > 2σ(I)
Horizontally mounted graphite crystal monochromatorRint = 0.088
Detector resolution: 9 pixels mm-1θmax = 39.8°, θmin = 3.2°
φ and ω scansh = 1716
Absorption correction: analytical
(de Meulenaer & Tompa, 1965)
k = 1716
Tmin = 0.174, Tmax = 0.390l = 2735
34604 measured reflections
Refinement top
Refinement on FWeighting scheme based on measured s.u.'s w = 1/[σ2(F) + 0.0004F2]
R[F > 3σ(F)] = 0.037(Δ/σ)max = 0.001
wR(F) = 0.040Δρmax = 2.12 e Å3
S = 1.15Δρmin = 1.37 e Å3
2628 reflectionsExtinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
67 parametersExtinction coefficient: 0.035 (6)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.84956 (5)0.16539 (5)0.443400 (18)0.00856 (14)
Mo20.68172 (5)0.18590 (5)0.365506 (18)0.00832 (13)
Mo30.51048 (7)0.16913 (7)0.250.00817 (19)
Se10.67930 (6)0.03257 (6)0.44904 (2)0.01054 (17)
Se20.37827 (6)0.01337 (6)0.35998 (2)0.01186 (17)
Se30.68237 (9)0.03619 (9)0.250.0113 (3)
Se4100.34018 (4)0.0196 (2)
Se50.66670.33330.46787 (4)0.01195 (19)
K0.66670.33330.63172 (12)0.0271 (6)
In0.7951 (2)0.1712 (2)0.250.0142 (7)0.291 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0087 (2)0.00918 (18)0.00839 (14)0.00490 (16)0.00017 (12)0.00006 (12)
Mo20.00800 (17)0.00788 (18)0.00926 (14)0.00410 (14)0.00005 (13)0.00053 (12)
Mo30.0083 (3)0.0084 (2)0.00844 (18)0.0046 (2)00
Se10.0092 (2)0.0106 (2)0.01248 (18)0.00546 (19)0.00125 (16)0.00095 (16)
Se20.0093 (2)0.0094 (2)0.01565 (18)0.00379 (18)0.00334 (16)0.00108 (17)
Se30.0125 (3)0.0095 (3)0.0137 (3)0.0069 (3)00
Se40.0254 (3)0.0254 (3)0.0081 (3)0.01268 (16)00
Se50.0135 (2)0.0135 (2)0.0088 (3)0.00675 (12)00
K0.0236 (7)0.0236 (7)0.0340 (11)0.0118 (3)00
In0.0133 (9)0.0087 (8)0.0196 (8)0.0047 (7)00
Geometric parameters (Å, º) top
Mo1—Mo1i3.8189 (5)Se1—Kxii3.5653 (11)
Mo1—Mo1ii2.6916 (6)Se2—Se33.5954 (10)
Mo1—Mo1iii2.7091 (7)Se2—Se3ix3.7850 (11)
Mo1—Mo1iv2.6916 (6)Se2—Se4xiii3.6667 (7)
Mo1—Mo1v2.7091 (6)Se2—Se53.6667 (6)
Mo1—Mo2ii3.5125 (8)Se2—Kxii3.2069 (6)
Mo1—Se12.5832 (9)Se2—Inxi2.8372 (16)
Mo1—Se1ii2.6160 (10)Se3—Se43.7498 (10)
Mo1—Se1v2.5560 (6)Se3—Se4xiv3.7498 (10)
Mo1—Se2vi2.6581 (6)Se3—In2.759 (3)
Mo1—Se42.5514 (7)Se3—Inxiv2.985 (3)
Mo1—In3.8252 (5)Se4—Se4xiv3.5355 (11)
Mo2—Mo2vii2.6417 (8)Se4—In2.5704 (13)
Mo2—Mo2viii2.6417 (10)Se4—Inxiv2.570 (2)
Mo2—Mo32.7746 (6)Se4—Inii2.570 (2)
Mo2—Mo3ix3.8366 (8)Se5—K3.212 (2)
Mo2—Mo3vii2.7132 (5)In—Inxiv3.232 (3)
Mo2—Se12.6874 (8)In—Inii3.232 (3)
Mo2—Se22.5877 (6)K—Se1xii3.5652 (10)
Mo2—Se2vii2.6051 (6)K—Se1iii3.5652 (11)
Mo2—Se32.7004 (7)K—Se1xv3.5652 (11)
Mo2—Se52.5205 (7)K—Se2xii3.2069 (6)
Mo3—Mo3ix2.7238 (8)K—Se2iii3.2069 (5)
Mo3—Mo3vii2.7238 (8)K—Se2xv3.2069 (9)
Mo3—Se22.5851 (5)K—Se53.212 (2)
Mo3—Se2x2.5851 (5)In—Mo13.8251 (5)
Mo3—Se32.5961 (13)In—Mo1x3.8251 (5)
Mo3—Se3ix2.5923 (16)In—Mo3xvi2.8999 (19)
Mo3—Inxi2.9002 (19)In—Se2xvi2.8373 (10)
Se1—Se1iii3.6032 (7)In—Se2vi2.8373 (10)
Se1—Se1v3.6032 (9)In—Se32.759 (3)
Se1—Se23.6466 (9)In—Se3ii2.984 (3)
Se1—Se2xii3.8049 (7)In—Se42.5703 (12)
Se1—Se2vi3.6416 (9)In—Se4xiv2.5703 (12)
Se1—Se43.6803 (7)In—Inxiv3.232 (2)
Se1—Se53.6707 (7)In—Inii3.232 (3)
Se1—Se5xii3.5859 (5)
Se1xii—K—Se1iii101.79 (4)Mo1x—In—Se4xiv41.493 (14)
Se1xii—K—Se1xv101.79 (4)Mo1x—In—Inxiv88.11 (2)
Se1xii—K—Se2xii64.906 (17)Mo1x—In—Inii82.67 (3)
Se1xii—K—Se2iii156.56 (6)Mo3xvi—In—Se2xvi53.55 (3)
Se1xii—K—Se2xv64.806 (17)Mo3xvi—In—Se2vi53.55 (3)
Se1xii—K—Se563.64 (3)Mo3xvi—In—Se3136.10 (7)
Se1iii—K—Se1xii101.79 (4)Mo3xvi—In—Se3ii52.26 (5)
Se1iii—K—Se1xv101.79 (4)Mo3xvi—In—Se4120.75 (7)
Se1iii—K—Se2xii64.806 (18)Mo3xvi—In—Se4xiv120.75 (7)
Se1iii—K—Se2iii64.91 (2)Mo3xvi—In—Inxiv164.78 (10)
Se1iii—K—Se2xv156.56 (6)Mo3xvi—In—Inii104.78 (9)
Se1iii—K—Se563.64 (3)Se2xvi—In—Se2vi98.92 (5)
Se1xv—K—Se1xii101.79 (4)Se2xvi—In—Se3104.20 (6)
Se1xv—K—Se1iii101.79 (4)Se2xvi—In—Se3ii81.07 (5)
Se1xv—K—Se2xii156.56 (6)Se2xvi—In—Se4164.22 (10)
Se1xv—K—Se2iii64.81 (2)Se2xvi—In—Se4xiv85.23 (2)
Se1xv—K—Se2xv64.906 (18)Se2xvi—In—Inxiv129.98 (3)
Se1xv—K—Se563.64 (3)Se2xvi—In—Inii113.98 (6)
Se2xii—K—Se2iii119.74 (2)Se2vi—In—Se2xvi98.92 (5)
Se2xii—K—Se2xv119.744 (14)Se2vi—In—Se3104.20 (6)
Se2xii—K—Se592.91 (4)Se2vi—In—Se3ii81.07 (5)
Se2iii—K—Se2xii119.74 (2)Se2vi—In—Se485.23 (2)
Se2iii—K—Se2xv119.744 (19)Se2vi—In—Se4xiv164.22 (10)
Se2iii—K—Se592.91 (4)Se2vi—In—Inxiv129.98 (3)
Se2xv—K—Se2xii119.744 (14)Se2vi—In—Inii113.98 (6)
Se2xv—K—Se2iii119.744 (19)Se3—In—Se3ii171.64 (6)
Se2xv—K—Se592.91 (4)Se3—In—Se489.36 (5)
Mo1—In—Mo1x164.76 (6)Se3—In—Se4xiv89.36 (5)
Mo1—In—Mo3xvi89.89 (3)Se3—In—Inxiv59.12 (7)
Mo1—In—Se2xvi141.91 (5)Se3—In—Inii119.12 (7)
Mo1—In—Se2vi43.991 (12)Se3ii—In—Se3171.64 (6)
Mo1—In—Se395.35 (4)Se3ii—In—Se484.58 (6)
Mo1—In—Se3ii83.92 (4)Se3ii—In—Se4xiv84.58 (6)
Mo1—In—Se441.493 (14)Se3ii—In—Inxiv112.52 (8)
Mo1—In—Se4xiv127.91 (5)Se3ii—In—Inii52.52 (6)
Mo1—In—Inxiv88.11 (2)Se4—In—Se4xiv86.91 (5)
Mo1—In—Inii82.67 (3)Se4—In—Inxiv51.05 (4)
Mo1x—In—Mo1164.76 (6)Se4—In—Inii51.05 (4)
Mo1x—In—Mo3xvi89.89 (3)Se4xiv—In—Se486.91 (5)
Mo1x—In—Se2xvi43.991 (12)Se4xiv—In—Inxiv51.05 (4)
Mo1x—In—Se2vi141.91 (5)Se4xiv—In—Inii51.05 (4)
Mo1x—In—Se395.35 (4)Inxiv—In—Inii60.00 (8)
Mo1x—In—Se3ii83.92 (4)Inii—In—Inxiv60.00 (8)
Mo1x—In—Se4127.91 (5)
Symmetry codes: (i) x+2, y, z+1; (ii) y+1, xy1, z; (iii) y+1, x+y+1, z+1; (iv) x+y+2, x+1, z; (v) xy, x1, z+1; (vi) x+y+1, x, z; (vii) y+1, xy, z; (viii) x+y+1, x+1, z; (ix) x+y+1, x+1, z+1/2; (x) x, y, z+1/2; (xi) y, xy1, z; (xii) x+1, y, z+1; (xiii) x1, y, z; (xiv) x+y+2, x+1, z+1/2; (xv) xy, x, z+1; (xvi) x+y+1, x, z+1/2.
 

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