Bis­(tetra­methyl­ammonium) hexa­aqua­cobalt(II) β-octamolybdate(VI)

The title compound, (C₄H₁₂N)₂[Co(H₂O)₆][β–Mo₈O₂₆], contains β-octamolybdate ([β-Mo₈O₂₆]⁴⁻), tetra­methyl­ammonium and [Co(H₂O)₆]²⁺ ions. The [β-Mo₈O₂₆]⁴⁻ anion and [Co(H₂O)₆]²⁺ cations lie on inversion centers, and the tetramethylammonium cations lie on twofold rotation axes.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](N-C) = 0.014 Å
• R factor = 0.039
• wR factor = 0.105
• Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT244_ALERT_4_C Low Solvent  U(eq) as Compared to Neighbors ....         N1
PLAT244_ALERT_4_C Low Solvent  U(eq) as Compared to Neighbors ....         N2
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          9
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.18 Ratio
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2
              Co H12 O6
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          3
              C4 H12 N

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   7 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
   0 ALERT type 3 Indicator that the structure quality may be low
   6 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens,1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis(tetramethylammonium) hexaaquacobalt(II) β-octamolybdate(vi)

Crystal data

(C4H12N)2[Co(H2O)6][Mo8O26]	F(000) = 2868
Mr = 1498.84	Dx = 2.749 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3856 reflections
a = 16.0338 (10) Å	θ = 2.0–25.1°
b = 13.6400 (8) Å	µ = 3.23 mm^−1
c = 16.6764 (10) Å	T = 293 K
β = 96.779 (1)°	Prism, red
V = 3621.6 (4) Å^3	0.43 × 0.22 × 0.20 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer	3195 independent reflections
Radiation source: fine-focus sealed tube	2825 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.021
φ and ω scans	θmax = 25.1°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→19
Tmin = 0.421, Tmax = 0.525	k = −16→14
5426 measured reflections	l = −19→19

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.105	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	w = 1/[σ^2(Fo^2) + (0.0357P)^2 + 82.4908P] where P = (Fo^2 + 2Fc^2)/3
3195 reflections	(Δ/σ)max = 0.018
239 parameters	Δρmax = 0.68 e Å^−3
0 restraints	Δρmin = −1.02 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Mo1	0.25091 (4)	0.83709 (4)	0.42069 (4)	0.02126 (17)
Mo2	0.39635 (4)	0.85422 (5)	0.57132 (4)	0.02574 (18)
Mo3	0.10500 (4)	0.85708 (5)	0.53760 (4)	0.02534 (18)
Mo4	0.25069 (4)	0.87542 (5)	0.69005 (4)	0.02813 (18)
Co1	0.2500	1.2500	0.5000	0.0247 (3)
OW1	0.2267 (4)	1.1894 (5)	0.6112 (4)	0.0419 (14)
HW1A	0.2385	1.1309	0.6121	0.10 (5)*
HW1B	0.2196	1.2307	0.6454	0.13 (7)*
O1	0.5009 (3)	0.8290 (5)	0.5876 (4)	0.0400 (14)
OW2	0.3282 (3)	1.3546 (4)	0.5599 (3)	0.0329 (12)
HW2A	0.2997	1.3954	0.5804	0.06 (3)*
HW2B	0.3659	1.3802	0.5383	0.05 (3)*
O2	0.2503 (3)	0.7921 (4)	0.3226 (3)	0.0288 (11)
OW3	0.1489 (4)	1.3403 (4)	0.5117 (4)	0.0413 (15)
HW3B	0.1545	1.3919	0.4877	0.14 (7)*
HW3A	0.1108	1.3271	0.5386	0.07 (4)*
O3	0.1108 (4)	0.9798 (4)	0.5207 (4)	0.0381 (13)
O4	0.2506 (4)	0.8613 (4)	0.7913 (4)	0.0451 (15)
O5	0.0007 (3)	0.8312 (5)	0.5291 (4)	0.0431 (15)
O6	0.3906 (4)	0.9770 (4)	0.5537 (3)	0.0387 (14)
O7	0.2499 (3)	0.6687 (4)	0.4499 (3)	0.0245 (11)
O8	0.1344 (3)	0.8506 (4)	0.6511 (3)	0.0314 (12)
O9	0.1320 (3)	0.8131 (4)	0.4291 (3)	0.0244 (11)
O10	0.3690 (3)	0.8117 (4)	0.4570 (3)	0.0259 (11)
O11	0.2514 (4)	0.9986 (4)	0.6746 (4)	0.0421 (14)
O12	0.3661 (3)	0.8478 (4)	0.6769 (3)	0.0283 (11)
O13	0.2502 (3)	0.9597 (4)	0.4103 (3)	0.0306 (12)
N1	0.5000	1.1287 (7)	0.7500	0.034 (2)
N2	0.0000	0.9396 (7)	0.2500	0.030 (2)
C1	0.4479 (9)	1.1910 (13)	0.6923 (9)	0.105 (6)
H1A	0.4130	1.2323	0.7210	0.157*
H1B	0.4132	1.1505	0.6550	0.157*
H1C	0.4835	1.2310	0.6633	0.157*
C2	0.5554 (8)	1.0666 (11)	0.7059 (9)	0.086 (4)
H2A	0.5890	1.0253	0.7435	0.130*
H2B	0.5914	1.1077	0.6783	0.130*
H2C	0.5217	1.0267	0.6673	0.130*
C3	0.0569 (7)	0.8774 (9)	0.2072 (7)	0.065 (3)
H3A	0.0241	0.8370	0.1683	0.098*
H3B	0.0901	0.8366	0.2456	0.098*
H3C	0.0933	0.9186	0.1802	0.098*
C4	0.0514 (6)	1.0029 (7)	0.3098 (5)	0.044 (2)
H4A	0.0149	1.0434	0.3373	0.066*
H4B	0.0876	1.0437	0.2822	0.066*
H4C	0.0847	0.9624	0.3483	0.066*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.0183 (3)	0.0176 (3)	0.0288 (3)	0.0025 (2)	0.0069 (2)	0.0052 (2)
Mo2	0.0207 (3)	0.0224 (3)	0.0347 (4)	−0.0018 (2)	0.0053 (3)	0.0026 (3)
Mo3	0.0207 (3)	0.0236 (3)	0.0332 (4)	0.0067 (2)	0.0098 (3)	0.0041 (3)
Mo4	0.0325 (4)	0.0239 (3)	0.0290 (4)	0.0049 (3)	0.0084 (3)	0.0003 (3)
Co1	0.0214 (7)	0.0182 (7)	0.0355 (8)	−0.0006 (5)	0.0072 (6)	0.0009 (6)
OW1	0.059 (4)	0.030 (3)	0.038 (3)	−0.003 (3)	0.012 (3)	0.004 (3)
O1	0.022 (3)	0.048 (4)	0.050 (4)	−0.003 (2)	0.002 (2)	0.002 (3)
OW2	0.029 (3)	0.028 (3)	0.045 (3)	−0.006 (2)	0.015 (3)	−0.006 (2)
O2	0.028 (3)	0.028 (3)	0.031 (3)	0.006 (2)	0.008 (2)	0.010 (2)
OW3	0.031 (3)	0.030 (3)	0.067 (4)	0.008 (2)	0.022 (3)	0.014 (3)
O3	0.047 (3)	0.021 (3)	0.047 (3)	0.005 (3)	0.011 (3)	0.006 (2)
O4	0.060 (4)	0.040 (4)	0.036 (3)	0.007 (3)	0.010 (3)	0.000 (3)
O5	0.025 (3)	0.046 (4)	0.061 (4)	0.006 (3)	0.014 (3)	0.009 (3)
O6	0.046 (3)	0.023 (3)	0.045 (3)	−0.010 (3)	0.000 (3)	0.003 (2)
O7	0.024 (3)	0.019 (2)	0.031 (3)	0.001 (2)	0.006 (2)	0.001 (2)
O8	0.034 (3)	0.032 (3)	0.032 (3)	0.010 (2)	0.016 (2)	0.004 (2)
O9	0.016 (2)	0.024 (3)	0.033 (3)	0.002 (2)	0.005 (2)	0.004 (2)
O10	0.021 (2)	0.024 (3)	0.035 (3)	0.001 (2)	0.010 (2)	0.005 (2)
O11	0.056 (4)	0.026 (3)	0.045 (3)	0.003 (3)	0.008 (3)	−0.001 (3)
O12	0.026 (3)	0.029 (3)	0.029 (3)	0.003 (2)	0.002 (2)	0.001 (2)
O13	0.029 (3)	0.018 (3)	0.045 (3)	−0.002 (2)	0.006 (2)	0.005 (2)
N1	0.033 (5)	0.031 (5)	0.037 (5)	0.000	0.005 (4)	0.000
N2	0.021 (4)	0.033 (5)	0.033 (5)	0.000	−0.003 (4)	0.000
C1	0.089 (10)	0.127 (14)	0.094 (10)	0.046 (10)	−0.001 (8)	0.056 (10)
C2	0.068 (8)	0.091 (10)	0.107 (11)	0.021 (7)	0.039 (8)	−0.008 (8)
C3	0.052 (6)	0.067 (7)	0.078 (8)	0.017 (5)	0.012 (6)	−0.031 (6)
C4	0.041 (5)	0.046 (5)	0.041 (5)	−0.002 (4)	−0.010 (4)	−0.008 (4)

Geometric parameters (Å, º)

Mo1—O13	1.681 (5)	OW2—HW2A	0.8200
Mo1—O2	1.746 (5)	OW2—HW2B	0.8184
Mo1—O10	1.950 (5)	O2—Mo4^i	2.295 (5)
Mo1—O9	1.956 (5)	OW3—HW3B	0.8200
Mo1—O7^i	2.162 (5)	OW3—HW3A	0.8191
Mo1—O7	2.348 (5)	O7—Mo1^i	2.162 (5)
Mo2—O1	1.701 (5)	O7—Mo3^i	2.338 (5)
Mo2—O6	1.701 (5)	O7—Mo2^i	2.350 (5)
Mo2—O12	1.882 (5)	O7—Mo4^i	2.409 (5)
Mo2—O10	1.992 (5)	O9—Mo2^i	2.327 (5)
Mo2—O9^i	2.327 (5)	O10—Mo3^i	2.339 (5)
Mo2—O7^i	2.350 (5)	N1—C1^iii	1.469 (12)
Mo3—O5	1.699 (6)	N1—C1	1.469 (12)
Mo3—O3	1.701 (5)	N1—C2^iii	1.483 (12)
Mo3—O8	1.898 (5)	N1—C2	1.483 (12)
Mo3—O9	2.002 (5)	N2—C3	1.488 (11)
Mo3—O7^i	2.338 (5)	N2—C3^iv	1.488 (11)
Mo3—O10^i	2.339 (5)	N2—C4	1.492 (10)
Mo4—O4	1.699 (6)	N2—C4^iv	1.492 (10)
Mo4—O11	1.700 (6)	C1—H1A	0.9600
Mo4—O12	1.926 (5)	C1—H1B	0.9600
Mo4—O8	1.931 (6)	C1—H1C	0.9600
Mo4—O2^i	2.295 (5)	C2—H2A	0.9600
Mo4—O7^i	2.409 (5)	C2—H2B	0.9600
Co1—OW3^ii	2.063 (5)	C2—H2C	0.9600
Co1—OW3	2.063 (5)	C3—H3A	0.9600
Co1—OW2^ii	2.076 (5)	C3—H3B	0.9600
Co1—OW2	2.076 (5)	C3—H3C	0.9600
Co1—OW1	2.104 (6)	C4—H4A	0.9600
Co1—OW1^ii	2.104 (6)	C4—H4B	0.9600
OW1—HW1A	0.8200	C4—H4C	0.9600
OW1—HW1B	0.8200
O13—Mo1—O2	104.7 (3)	OW3^ii—Co1—OW1^ii	85.9 (3)
O13—Mo1—O10	101.7 (2)	OW3—Co1—OW1^ii	94.1 (3)
O2—Mo1—O10	97.2 (2)	OW2^ii—Co1—OW1^ii	90.3 (2)
O13—Mo1—O9	100.3 (2)	OW2—Co1—OW1^ii	89.7 (2)
O2—Mo1—O9	96.4 (2)	OW1—Co1—OW1^ii	180.000 (1)
O10—Mo1—O9	150.2 (2)	Co1—OW1—HW1A	109.5
O13—Mo1—O7^i	98.0 (2)	Co1—OW1—HW1B	113.4
O2—Mo1—O7^i	157.3 (2)	HW1A—OW1—HW1B	135.1
O10—Mo1—O7^i	78.67 (19)	Co1—OW2—HW2A	109.5
O9—Mo1—O7^i	78.57 (19)	Co1—OW2—HW2B	121.1
O13—Mo1—O7	173.8 (2)	HW2A—OW2—HW2B	111.8
O2—Mo1—O7	81.4 (2)	Mo1—O2—Mo4^i	115.8 (2)
O10—Mo1—O7	78.01 (19)	Co1—OW3—HW3B	109.5
O9—Mo1—O7	77.93 (18)	Co1—OW3—HW3A	124.4
O7^i—Mo1—O7	75.9 (2)	HW3B—OW3—HW3A	126.0
O1—Mo2—O6	105.0 (3)	Mo1^i—O7—Mo3^i	91.61 (18)
O1—Mo2—O12	101.5 (3)	Mo1^i—O7—Mo1	104.1 (2)
O6—Mo2—O12	101.1 (3)	Mo3^i—O7—Mo1	97.73 (18)
O1—Mo2—O10	101.2 (3)	Mo1^i—O7—Mo2^i	91.26 (17)
O6—Mo2—O10	96.9 (2)	Mo3^i—O7—Mo2^i	163.3 (2)
O12—Mo2—O10	146.1 (2)	Mo1—O7—Mo2^i	97.50 (18)
O1—Mo2—O9^i	89.5 (2)	Mo1^i—O7—Mo4^i	163.4 (2)
O6—Mo2—O9^i	163.4 (2)	Mo3^i—O7—Mo4^i	86.50 (16)
O12—Mo2—O9^i	83.4 (2)	Mo1—O7—Mo4^i	92.47 (17)
O10—Mo2—O9^i	71.99 (19)	Mo2^i—O7—Mo4^i	86.07 (16)
O1—Mo2—O7^i	160.7 (2)	Mo3—O8—Mo4	116.3 (3)
O6—Mo2—O7^i	94.1 (2)	Mo1—O9—Mo3	109.3 (2)
O12—Mo2—O7^i	76.8 (2)	Mo1—O9—Mo2^i	110.8 (2)
O10—Mo2—O7^i	73.42 (18)	Mo3—O9—Mo2^i	103.5 (2)
O9^i—Mo2—O7^i	71.21 (16)	Mo1—O10—Mo2	109.9 (2)
O5—Mo3—O3	105.3 (3)	Mo1—O10—Mo3^i	110.4 (2)
O5—Mo3—O8	101.5 (3)	Mo2—O10—Mo3^i	103.4 (2)
O3—Mo3—O8	101.5 (3)	Mo2—O12—Mo4	117.1 (3)
O5—Mo3—O9	100.3 (3)	C1^iii—N1—C1	109.2 (16)
O3—Mo3—O9	97.1 (2)	C1^iii—N1—C2^iii	109.4 (9)
O8—Mo3—O9	146.4 (2)	C1—N1—C2^iii	109.1 (9)
O5—Mo3—O7^i	159.4 (2)	C1^iii—N1—C2	109.1 (9)
O3—Mo3—O7^i	95.1 (2)	C1—N1—C2	109.4 (9)
O8—Mo3—O7^i	77.1 (2)	C2^iii—N1—C2	110.5 (13)
O9—Mo3—O7^i	73.54 (18)	C3—N2—C3^iv	110.5 (12)
O5—Mo3—O10^i	88.2 (2)	C3—N2—C4	109.2 (6)
O3—Mo3—O10^i	164.0 (2)	C3^iv—N2—C4	109.3 (6)
O8—Mo3—O10^i	83.9 (2)	C3—N2—C4^iv	109.3 (6)
O9—Mo3—O10^i	71.56 (18)	C3^iv—N2—C4^iv	109.2 (6)
O7^i—Mo3—O10^i	71.20 (17)	C4—N2—C4^iv	109.2 (9)
O4—Mo4—O11	105.2 (3)	N1—C1—H1A	109.5
O4—Mo4—O12	101.8 (3)	N1—C1—H1B	109.5
O11—Mo4—O12	98.7 (3)	H1A—C1—H1B	109.5
O4—Mo4—O8	101.6 (3)	N1—C1—H1C	109.5
O11—Mo4—O8	98.4 (3)	H1A—C1—H1C	109.5
O12—Mo4—O8	146.1 (2)	H1B—C1—H1C	109.5
O4—Mo4—O2^i	88.7 (2)	N1—C2—H2A	109.5
O11—Mo4—O2^i	166.0 (2)	N1—C2—H2B	109.5
O12—Mo4—O2^i	78.0 (2)	H2A—C2—H2B	109.5
O8—Mo4—O2^i	78.4 (2)	N1—C2—H2C	109.5
O4—Mo4—O7^i	159.0 (2)	H2A—C2—H2C	109.5
O11—Mo4—O7^i	95.7 (2)	H2B—C2—H2C	109.5
O12—Mo4—O7^i	74.59 (19)	N2—C3—H3A	109.5
O8—Mo4—O7^i	74.78 (19)	N2—C3—H3B	109.5
O2^i—Mo4—O7^i	70.28 (17)	H3A—C3—H3B	109.5
OW3^ii—Co1—OW3	180.000 (2)	N2—C3—H3C	109.5
OW3^ii—Co1—OW2^ii	88.9 (2)	H3A—C3—H3C	109.5
OW3—Co1—OW2^ii	91.1 (2)	H3B—C3—H3C	109.5
OW3^ii—Co1—OW2	91.1 (2)	N2—C4—H4A	109.5
OW3—Co1—OW2	88.9 (2)	N2—C4—H4B	109.5
OW2^ii—Co1—OW2	180.000 (1)	H4A—C4—H4B	109.5
OW3^ii—Co1—OW1	94.1 (3)	N2—C4—H4C	109.5
OW3—Co1—OW1	85.9 (3)	H4A—C4—H4C	109.5
OW2^ii—Co1—OW1	89.7 (2)	H4B—C4—H4C	109.5
OW2—Co1—OW1	90.3 (2)

Symmetry codes: (i) −x+1/2, −y+3/2, −z+1; (ii) −x+1/2, −y+5/2, −z+1; (iii) −x+1, y, −z+3/2; (iv) −x, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
OW1—HW1A···O11	0.82	2.08	2.819 (8)	150
OW1—HW1B···O4^v	0.82	2.10	2.852 (9)	153
OW2—HW2A···O13^ii	0.82	2.14	2.897 (7)	152
OW2—HW2A···O4^v	0.82	2.42	2.916 (8)	120
OW2—HW2B···O3^ii	0.82	2.20	2.859 (8)	138
OW2—HW2B···O5^vi	0.82	2.28	2.889 (8)	131
OW3—HW3B···O6^ii	0.82	2.02	2.764 (8)	151
OW3—HW3A···O1^vii	0.82	2.03	2.822 (8)	163

Symmetry codes: (ii) −x+1/2, −y+5/2, −z+1; (v) −x+1/2, y+1/2, −z+3/2; (vi) x+1/2, y+1/2, z; (vii) x−1/2, y+1/2, z.