In_0.87K₂Mo₁₅Se₁₉: a quaternary selenide containing Mo₆ and Mo₉ clusters

The structure of In_0.87K₂Mo₁₅Se₁₉ (indium dipotassium penta­deca­molybdate nona­deca­selenide), isotypic with In_2.9Mo₁₅Se₁₉, is characterized by a mixture of Mo₆Seⁱ₈Se^a₆ and Mo₉Seⁱ₁₁Se^a₆ 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 In_2.9Mo₁₅Se₁₉. One Mo, one Se and the In atom are situated on mirror planes, and two other Se atoms are situated on threefold axes.

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

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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

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Computing details

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

Crystal data

In0.875K2Mo15Se19	Dx = 6.339 (1) Mg m^−3
Mr = 3118	Mo Kα radiation, λ = 0.71069 Å
Hexagonal, P63/m	Cell parameters from 45013 reflections
Hall symbol: -P 6c	θ = 2.0–40.3°
a = 9.8076 (1) Å	µ = 27.57 mm^−1
c = 19.6036 (3) Å	T = 293 K
V = 1633.02 (3) Å^3	Irregular block, black
Z = 2	0.10 × 0.09 × 0.06 mm
F(000) = 2713.6

Data collection

Nonius KappaCCD area-detector diffractometer	3409 independent reflections
Radiation source: fine-focus sealed tube	2628 reflections with I > 2σ(I)
Horizontally mounted graphite crystal monochromator	Rint = 0.088
Detector resolution: 9 pixels mm^-1	θmax = 39.8°, θmin = 3.2°
φ and ω scans	h = −17→16
Absorption correction: analytical (de Meulenaer & Tompa, 1965)	k = −17→16
Tmin = 0.174, Tmax = 0.390	l = −27→35
34604 measured reflections

Refinement

Refinement on F	Weighting scheme based on measured s.u.'s w = 1/[σ^2(F) + 0.0004F^2]
R[F > 3σ(F)] = 0.037	(Δ/σ)max = 0.001
wR(F) = 0.040	Δρmax = 2.12 e Å^−3
S = 1.15	Δρmin = −1.37 e Å^−3
2628 reflections	Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
67 parameters	Extinction coefficient: 0.035 (6)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mo1	0.84956 (5)	−0.16539 (5)	0.443400 (18)	0.00856 (14)
Mo2	0.68172 (5)	0.18590 (5)	0.365506 (18)	0.00832 (13)
Mo3	0.51048 (7)	0.16913 (7)	0.25	0.00817 (19)
Se1	0.67930 (6)	−0.03257 (6)	0.44904 (2)	0.01054 (17)
Se2	0.37827 (6)	0.01337 (6)	0.35998 (2)	0.01186 (17)
Se3	0.68237 (9)	0.03619 (9)	0.25	0.0113 (3)
Se4	1	0	0.34018 (4)	0.0196 (2)
Se5	0.6667	0.3333	0.46787 (4)	0.01195 (19)
K	0.6667	0.3333	0.63172 (12)	0.0271 (6)
In	0.7951 (2)	−0.1712 (2)	0.25	0.0142 (7)	0.291 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.0087 (2)	0.00918 (18)	0.00839 (14)	0.00490 (16)	−0.00017 (12)	−0.00006 (12)
Mo2	0.00800 (17)	0.00788 (18)	0.00926 (14)	0.00410 (14)	0.00005 (13)	0.00053 (12)
Mo3	0.0083 (3)	0.0084 (2)	0.00844 (18)	0.0046 (2)	0	0
Se1	0.0092 (2)	0.0106 (2)	0.01248 (18)	0.00546 (19)	−0.00125 (16)	0.00095 (16)
Se2	0.0093 (2)	0.0094 (2)	0.01565 (18)	0.00379 (18)	0.00334 (16)	0.00108 (17)
Se3	0.0125 (3)	0.0095 (3)	0.0137 (3)	0.0069 (3)	0	0
Se4	0.0254 (3)	0.0254 (3)	0.0081 (3)	0.01268 (16)	0	0
Se5	0.0135 (2)	0.0135 (2)	0.0088 (3)	0.00675 (12)	0	0
K	0.0236 (7)	0.0236 (7)	0.0340 (11)	0.0118 (3)	0	0
In	0.0133 (9)	0.0087 (8)	0.0196 (8)	0.0047 (7)	0	0

Geometric parameters (Å, º)

Mo1—Mo1^i	3.8189 (5)	Se1—K^xii	3.5653 (11)
Mo1—Mo1^ii	2.6916 (6)	Se2—Se3	3.5954 (10)
Mo1—Mo1^iii	2.7091 (7)	Se2—Se3^ix	3.7850 (11)
Mo1—Mo1^iv	2.6916 (6)	Se2—Se4^xiii	3.6667 (7)
Mo1—Mo1^v	2.7091 (6)	Se2—Se5	3.6667 (6)
Mo1—Mo2^ii	3.5125 (8)	Se2—K^xii	3.2069 (6)
Mo1—Se1	2.5832 (9)	Se2—In^xi	2.8372 (16)
Mo1—Se1^ii	2.6160 (10)	Se3—Se4	3.7498 (10)
Mo1—Se1^v	2.5560 (6)	Se3—Se4^xiv	3.7498 (10)
Mo1—Se2^vi	2.6581 (6)	Se3—In	2.759 (3)
Mo1—Se4	2.5514 (7)	Se3—In^xiv	2.985 (3)
Mo1—In	3.8252 (5)	Se4—Se4^xiv	3.5355 (11)
Mo2—Mo2^vii	2.6417 (8)	Se4—In	2.5704 (13)
Mo2—Mo2^viii	2.6417 (10)	Se4—In^xiv	2.570 (2)
Mo2—Mo3	2.7746 (6)	Se4—In^ii	2.570 (2)
Mo2—Mo3^ix	3.8366 (8)	Se5—K	3.212 (2)
Mo2—Mo3^vii	2.7132 (5)	In—In^xiv	3.232 (3)
Mo2—Se1	2.6874 (8)	In—In^ii	3.232 (3)
Mo2—Se2	2.5877 (6)	K—Se1^xii	3.5652 (10)
Mo2—Se2^vii	2.6051 (6)	K—Se1^iii	3.5652 (11)
Mo2—Se3	2.7004 (7)	K—Se1^xv	3.5652 (11)
Mo2—Se5	2.5205 (7)	K—Se2^xii	3.2069 (6)
Mo3—Mo3^ix	2.7238 (8)	K—Se2^iii	3.2069 (5)
Mo3—Mo3^vii	2.7238 (8)	K—Se2^xv	3.2069 (9)
Mo3—Se2	2.5851 (5)	K—Se5	3.212 (2)
Mo3—Se2^x	2.5851 (5)	In—Mo1	3.8251 (5)
Mo3—Se3	2.5961 (13)	In—Mo1^x	3.8251 (5)
Mo3—Se3^ix	2.5923 (16)	In—Mo3^xvi	2.8999 (19)
Mo3—In^xi	2.9002 (19)	In—Se2^xvi	2.8373 (10)
Se1—Se1^iii	3.6032 (7)	In—Se2^vi	2.8373 (10)
Se1—Se1^v	3.6032 (9)	In—Se3	2.759 (3)
Se1—Se2	3.6466 (9)	In—Se3^ii	2.984 (3)
Se1—Se2^xii	3.8049 (7)	In—Se4	2.5703 (12)
Se1—Se2^vi	3.6416 (9)	In—Se4^xiv	2.5703 (12)
Se1—Se4	3.6803 (7)	In—In^xiv	3.232 (2)
Se1—Se5	3.6707 (7)	In—In^ii	3.232 (3)
Se1—Se5^xii	3.5859 (5)
Se1^xii—K—Se1^iii	101.79 (4)	Mo1^x—In—Se4^xiv	41.493 (14)
Se1^xii—K—Se1^xv	101.79 (4)	Mo1^x—In—In^xiv	88.11 (2)
Se1^xii—K—Se2^xii	64.906 (17)	Mo1^x—In—In^ii	82.67 (3)
Se1^xii—K—Se2^iii	156.56 (6)	Mo3^xvi—In—Se2^xvi	53.55 (3)
Se1^xii—K—Se2^xv	64.806 (17)	Mo3^xvi—In—Se2^vi	53.55 (3)
Se1^xii—K—Se5	63.64 (3)	Mo3^xvi—In—Se3	136.10 (7)
Se1^iii—K—Se1^xii	101.79 (4)	Mo3^xvi—In—Se3^ii	52.26 (5)
Se1^iii—K—Se1^xv	101.79 (4)	Mo3^xvi—In—Se4	120.75 (7)
Se1^iii—K—Se2^xii	64.806 (18)	Mo3^xvi—In—Se4^xiv	120.75 (7)
Se1^iii—K—Se2^iii	64.91 (2)	Mo3^xvi—In—In^xiv	164.78 (10)
Se1^iii—K—Se2^xv	156.56 (6)	Mo3^xvi—In—In^ii	104.78 (9)
Se1^iii—K—Se5	63.64 (3)	Se2^xvi—In—Se2^vi	98.92 (5)
Se1^xv—K—Se1^xii	101.79 (4)	Se2^xvi—In—Se3	104.20 (6)
Se1^xv—K—Se1^iii	101.79 (4)	Se2^xvi—In—Se3^ii	81.07 (5)
Se1^xv—K—Se2^xii	156.56 (6)	Se2^xvi—In—Se4	164.22 (10)
Se1^xv—K—Se2^iii	64.81 (2)	Se2^xvi—In—Se4^xiv	85.23 (2)
Se1^xv—K—Se2^xv	64.906 (18)	Se2^xvi—In—In^xiv	129.98 (3)
Se1^xv—K—Se5	63.64 (3)	Se2^xvi—In—In^ii	113.98 (6)
Se2^xii—K—Se2^iii	119.74 (2)	Se2^vi—In—Se2^xvi	98.92 (5)
Se2^xii—K—Se2^xv	119.744 (14)	Se2^vi—In—Se3	104.20 (6)
Se2^xii—K—Se5	92.91 (4)	Se2^vi—In—Se3^ii	81.07 (5)
Se2^iii—K—Se2^xii	119.74 (2)	Se2^vi—In—Se4	85.23 (2)
Se2^iii—K—Se2^xv	119.744 (19)	Se2^vi—In—Se4^xiv	164.22 (10)
Se2^iii—K—Se5	92.91 (4)	Se2^vi—In—In^xiv	129.98 (3)
Se2^xv—K—Se2^xii	119.744 (14)	Se2^vi—In—In^ii	113.98 (6)
Se2^xv—K—Se2^iii	119.744 (19)	Se3—In—Se3^ii	171.64 (6)
Se2^xv—K—Se5	92.91 (4)	Se3—In—Se4	89.36 (5)
Mo1—In—Mo1^x	164.76 (6)	Se3—In—Se4^xiv	89.36 (5)
Mo1—In—Mo3^xvi	89.89 (3)	Se3—In—In^xiv	59.12 (7)
Mo1—In—Se2^xvi	141.91 (5)	Se3—In—In^ii	119.12 (7)
Mo1—In—Se2^vi	43.991 (12)	Se3^ii—In—Se3	171.64 (6)
Mo1—In—Se3	95.35 (4)	Se3^ii—In—Se4	84.58 (6)
Mo1—In—Se3^ii	83.92 (4)	Se3^ii—In—Se4^xiv	84.58 (6)
Mo1—In—Se4	41.493 (14)	Se3^ii—In—In^xiv	112.52 (8)
Mo1—In—Se4^xiv	127.91 (5)	Se3^ii—In—In^ii	52.52 (6)
Mo1—In—In^xiv	88.11 (2)	Se4—In—Se4^xiv	86.91 (5)
Mo1—In—In^ii	82.67 (3)	Se4—In—In^xiv	51.05 (4)
Mo1^x—In—Mo1	164.76 (6)	Se4—In—In^ii	51.05 (4)
Mo1^x—In—Mo3^xvi	89.89 (3)	Se4^xiv—In—Se4	86.91 (5)
Mo1^x—In—Se2^xvi	43.991 (12)	Se4^xiv—In—In^xiv	51.05 (4)
Mo1^x—In—Se2^vi	141.91 (5)	Se4^xiv—In—In^ii	51.05 (4)
Mo1^x—In—Se3	95.35 (4)	In^xiv—In—In^ii	60.00 (8)
Mo1^x—In—Se3^ii	83.92 (4)	In^ii—In—In^xiv	60.00 (8)
Mo1^x—In—Se4	127.91 (5)

Symmetry codes: (i) −x+2, −y, −z+1; (ii) −y+1, x−y−1, z; (iii) y+1, −x+y+1, −z+1; (iv) −x+y+2, −x+1, z; (v) x−y, x−1, −z+1; (vi) −x+y+1, −x, z; (vii) −y+1, x−y, 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, x−y−1, z; (xii) −x+1, −y, −z+1; (xiii) x−1, y, z; (xiv) −x+y+2, −x+1, −z+1/2; (xv) x−y, x, −z+1; (xvi) −x+y+1, −x, −z+1/2.