(C₆H₁₆N₂)₂[Mo₈O₂₆]: a new β-octamolybdate salt

Crystals of the title compound, 2,5-di­methyl­piperazinediium β-octamolybdate, were grown under mild hydro­thermal conditions. The anion and cations lie on inversion centers. A network of N—H...O bonds helps to stabilize the crystal packing.

Key indicators

• Single-crystal X-ray study
• T = 153 K
• Mean [sigma](C-C) = 0.014 Å
• R factor = 0.043
• wR factor = 0.095
• Data-to-parameter ratio = 12.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         14
PLAT353_ALERT_3_C Long    N-H Bond (0.87A)   N1     -   H1     ...       1.01 Ang.
PLAT353_ALERT_3_C Long    N-H Bond (0.87A)   N2     -   H10    ...       1.02 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O9     ..  C5      ..       3.01 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2
              C6 H16 N2
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          3
              C6 H16 N2

   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
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: CrysAlis CCD (Oxford Diffraction, 2004); cell refinement: CrysAlis RED; data reduction: CrysAlis RED (Oxford Diffraction, 2004); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ATOMS (Dowty, 2002); software used to prepare material for publication: CRYSTALS.

2,5-dimethylpiperazinediium β-octamolybdate

Crystal data

(C6H16N2)2[Mo8O26]	F(000) = 1352
Mr = 1415.92	Dx = 2.867 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3088 reflections
a = 11.0450 (11) Å	θ = 3.9–33.3°
b = 12.3699 (11) Å	µ = 3.06 mm^−1
c = 13.0539 (15) Å	T = 153 K
β = 113.148 (10)°	Plate, colourless
V = 1639.9 (3) Å^3	0.09 × 0.08 × 0.02 mm
Z = 2

Data collection

CrysAlis CCD diffractometer	2797 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
ω scans	θmax = 33.4°, θmin = 3.9°
Absorption correction: analytical (multifaceted crystal model; Clark & Reid, 1995)	h = −15→16
Tmin = 0.636, Tmax = 0.862	k = −16→18
14643 measured reflections	l = −19→18
5519 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.043	H-atom parameters constrained
wR(F^2) = 0.095	Robust weighting scheme (Prince, 1982) fitted by a five-term Chebychev polynomial (Watkin, 1994) with coefficients 12.6, 20.2, 12.3, 5.21 and 1.63.
S = 0.85	(Δ/σ)max < 0.001
2797 reflections	Δρmax = 2.41 e Å^−3
226 parameters	Δρmin = −1.35 e Å^−3
0 restraints

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

	x	y	z	Uiso*/Ueq
Mo1	−0.03461 (7)	−0.07093 (6)	1.19739 (6)	0.0108
Mo2	0.14345 (6)	−0.08308 (5)	1.05363 (6)	0.0095
Mo3	0.18253 (6)	0.17511 (5)	1.06758 (6)	0.0105
Mo4	0.00342 (7)	0.19058 (5)	1.21254 (6)	0.0114
O1	0.1085 (6)	−0.0865 (5)	1.3120 (5)	0.0153
O2	−0.1479 (6)	−0.1510 (5)	1.2183 (5)	0.0177
O3	−0.0930 (6)	0.0681 (5)	1.2254 (5)	0.0133
O4	0.0150 (5)	−0.1609 (4)	1.0925 (5)	0.0112
O5	0.0530 (5)	0.0476 (5)	1.1038 (5)	0.0115
O6	−0.1937 (6)	−0.0417 (5)	1.0171 (5)	0.0125
O7	0.2826 (6)	−0.0935 (5)	1.1702 (5)	0.0142
O8	0.1596 (5)	−0.1804 (5)	0.9615 (5)	0.0116
O9	0.3192 (6)	0.1506 (5)	1.1862 (5)	0.0151
O10	0.2324 (6)	0.2640 (5)	0.9924 (5)	0.0155
O11	0.0759 (6)	0.2643 (5)	1.1193 (5)	0.0155
O12	0.1474 (6)	0.1665 (5)	1.3232 (5)	0.0150
O13	−0.0717 (6)	0.2938 (5)	1.2537 (5)	0.0163
N1	−0.4153 (7)	−0.0782 (6)	1.0756 (6)	0.0159
N2	0.0924 (9)	−0.4156 (7)	1.0492 (8)	0.0322
C1	−0.5441 (8)	−0.1125 (7)	0.9854 (7)	0.0166
C2	−0.4203 (8)	0.0366 (7)	1.1117 (7)	0.0169
C3	−0.5382 (9)	−0.2307 (8)	0.9527 (8)	0.0193
C4	0.1280 (10)	−0.5050 (9)	0.9916 (9)	0.0294
C5	−0.0012 (10)	−0.4520 (9)	1.0994 (9)	0.0301
C6	0.2297 (9)	−0.4772 (7)	0.9464 (8)	0.0204
H1	−0.3940	−0.1275	1.1419	0.0167*
H2	−0.3436	−0.0841	1.0472	0.0167*
H3	−0.6162	−0.1089	1.0141	0.0189*
H4	−0.5194	−0.2785	1.0187	0.0223*
H5	−0.4669	−0.2392	0.9239	0.0223*
H6	−0.6246	−0.2518	0.8925	0.0223*
H7	−0.4896	0.0418	1.1445	0.0202*
H8	−0.3333	0.0570	1.1708	0.0202*
H9	0.0502	−0.3554	0.9960	0.0212*
H10	0.1747	−0.3859	1.1111	0.0212*
H11	0.1739	−0.5617	1.0484	0.0364*
H12	0.1963	−0.4169	0.8911	0.0225*
H13	0.3127	−0.4541	1.0086	0.0225*
H14	0.2473	−0.5421	0.9087	0.0225*
H15	−0.0221	−0.3904	1.1404	0.0353*
H16	0.0417	−0.5114	1.1557	0.0353*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.0096 (3)	0.0121 (3)	0.0089 (3)	0.0005 (2)	0.0020 (2)	0.0007 (2)
Mo2	0.0076 (3)	0.0100 (3)	0.0090 (3)	0.0009 (2)	0.0011 (2)	0.0006 (2)
Mo3	0.0084 (3)	0.0104 (3)	0.0105 (3)	−0.0005 (2)	0.0013 (2)	0.0001 (2)
Mo4	0.0106 (3)	0.0121 (3)	0.0097 (3)	0.0005 (2)	0.0021 (2)	−0.0007 (2)
O1	0.013 (3)	0.016 (3)	0.012 (3)	0.003 (2)	−0.001 (2)	0.000 (2)
O2	0.011 (3)	0.025 (3)	0.016 (3)	−0.002 (2)	0.002 (2)	−0.001 (2)
O3	0.013 (3)	0.016 (3)	0.013 (3)	0.001 (2)	0.008 (2)	0.002 (2)
O4	0.010 (3)	0.010 (2)	0.010 (2)	0.000 (2)	0.000 (2)	0.001 (2)
O5	0.007 (3)	0.013 (3)	0.012 (3)	0.0017 (19)	0.001 (2)	−0.002 (2)
O6	0.012 (3)	0.013 (3)	0.013 (3)	0.001 (2)	0.005 (2)	0.002 (2)
O7	0.011 (3)	0.015 (3)	0.015 (3)	−0.001 (2)	0.003 (2)	0.003 (2)
O8	0.009 (2)	0.015 (3)	0.010 (2)	0.000 (2)	0.003 (2)	−0.004 (2)
O9	0.014 (3)	0.014 (3)	0.013 (3)	0.001 (2)	0.002 (2)	−0.002 (2)
O10	0.012 (3)	0.011 (3)	0.021 (3)	−0.004 (2)	0.004 (2)	0.001 (2)
O11	0.019 (3)	0.014 (3)	0.012 (3)	−0.001 (2)	0.004 (2)	0.000 (2)
O12	0.014 (3)	0.017 (3)	0.009 (3)	0.003 (2)	0.000 (2)	0.003 (2)
O13	0.017 (3)	0.020 (3)	0.012 (3)	0.003 (2)	0.005 (2)	−0.002 (2)
N1	0.011 (3)	0.021 (3)	0.012 (3)	−0.001 (3)	0.002 (3)	0.000 (3)
N2	0.026 (4)	0.029 (5)	0.028 (5)	0.002 (4)	−0.004 (4)	−0.002 (4)
C1	0.015 (4)	0.014 (4)	0.016 (4)	0.000 (3)	0.002 (3)	−0.001 (3)
C2	0.015 (4)	0.020 (4)	0.015 (4)	0.002 (3)	0.005 (3)	−0.002 (3)
C3	0.016 (4)	0.023 (4)	0.015 (4)	0.002 (3)	0.003 (3)	−0.003 (3)
C4	0.021 (5)	0.038 (6)	0.022 (5)	−0.004 (4)	0.002 (4)	0.000 (4)
C5	0.021 (5)	0.040 (6)	0.025 (5)	−0.011 (4)	0.005 (4)	−0.008 (4)
C6	0.015 (4)	0.015 (4)	0.025 (5)	−0.003 (3)	0.001 (3)	0.002 (3)

Geometric parameters (Å, º)

Mo1—O1	1.708 (6)	N1—C1	1.508 (10)
Mo1—O2	1.700 (6)	N1—C2	1.504 (11)
Mo1—O3	1.922 (6)	N1—H1	1.009
Mo1—O4	2.001 (6)	N1—H2	1.000
Mo1—O5	2.346 (6)	N2—C4	1.474 (15)
Mo1—O6	2.347 (6)	N2—C5	1.494 (15)
Mo2—O4	1.940 (6)	N2—H9	1.000
Mo2—O5	2.134 (6)	N2—H10	1.018
Mo2—O5^i	2.371 (5)	C1—C2^ii	1.500 (12)
Mo2—O6^i	1.986 (6)	C1—C3	1.531 (12)
Mo2—O7	1.690 (6)	C1—H3	1.005
Mo2—O8	1.760 (6)	C2—H7	1.015
Mo3—O4^i	2.360 (5)	C2—H8	1.000
Mo3—O5	2.301 (6)	C3—H4	0.997
Mo3—O6^i	2.016 (6)	C3—H5	1.003
Mo3—O9	1.712 (6)	C3—H6	1.004
Mo3—O10	1.702 (6)	C4—C5^iii	1.532 (14)
Mo3—O11	1.919 (6)	C4—C6	1.500 (14)
Mo4—O3	1.897 (6)	C4—H11	1.001
Mo4—O5	2.460 (6)	C5—H15	1.010
Mo4—O8^i	2.282 (5)	C5—H16	1.015
Mo4—O11	1.929 (6)	C6—H12	1.001
Mo4—O12	1.702 (6)	C6—H13	0.999
Mo4—O13	1.720 (6)	C6—H14	1.000
Mo2—Mo1—Mo4	89.31 (3)	Mo1—Mo4—O8^i	81.51 (14)
Mo2—Mo1—O1	86.4 (2)	Mo3—Mo4—O8^i	80.74 (14)
Mo4—Mo1—O1	90.3 (2)	O3—Mo4—O8^i	78.1 (2)
Mo2—Mo1—O2	136.5 (2)	O5—Mo4—O8^i	69.73 (19)
Mo4—Mo1—O2	130.9 (2)	Mo1—Mo4—O11	120.44 (18)
O1—Mo1—O2	106.2 (3)	Mo3—Mo4—O11	32.67 (18)
Mo2—Mo1—O3	118.80 (17)	O3—Mo4—O11	145.1 (3)
Mo4—Mo1—O3	31.22 (17)	O5—Mo4—O11	74.6 (2)
O1—Mo1—O3	101.5 (3)	O8^i—Mo4—O11	76.0 (2)
O2—Mo1—O3	99.7 (3)	Mo1—Mo4—O12	86.1 (2)
Mo2—Mo1—O4	34.79 (16)	Mo3—Mo4—O12	84.5 (2)
Mo4—Mo1—O4	122.03 (16)	O3—Mo4—O12	98.9 (3)
O1—Mo1—O4	97.4 (3)	O5—Mo4—O12	91.0 (2)
O2—Mo1—O4	101.7 (3)	O8^i—Mo4—O12	160.7 (3)
O3—Mo1—O4	146.2 (2)	Mo1—Mo4—O13	133.6 (2)
Mo2—Mo1—O5	41.63 (14)	Mo3—Mo4—O13	135.0 (2)
Mo4—Mo1—O5	48.82 (14)	O3—Mo4—O13	102.0 (3)
O1—Mo1—O5	95.6 (3)	O5—Mo4—O13	163.3 (2)
O2—Mo1—O5	158.1 (2)	O8^i—Mo4—O13	93.6 (2)
O3—Mo1—O5	77.2 (2)	O11—Mo4—O12	97.9 (3)
Mo2—Mo1—O6	79.06 (14)	O11—Mo4—O13	102.5 (3)
Mo4—Mo1—O6	86.32 (14)	O12—Mo4—O13	105.6 (3)
O1—Mo1—O6	165.1 (3)	Mo1—O3—Mo4	117.1 (3)
O2—Mo1—O6	86.7 (2)	Mo1—O4—Mo2	109.1 (3)
O3—Mo1—O6	83.0 (2)	Mo1—O4—Mo3^i	103.9 (2)
O4—Mo1—O5	73.2 (2)	Mo2—O4—Mo3^i	108.8 (3)
O4—Mo1—O6	72.4 (2)	Mo1—O5—Mo2	91.5 (2)
O5—Mo1—O6	71.41 (19)	Mo1—O5—Mo2^i	98.2 (2)
Mo1—Mo2—Mo3	91.13 (3)	Mo2—O5—Mo2^i	104.7 (2)
Mo1—Mo2—O4	36.06 (17)	Mo1—O5—Mo3	162.3 (3)
Mo3—Mo2—O4	124.98 (17)	Mo2—O5—Mo3	93.0 (2)
Mo1—Mo2—O5	46.91 (16)	Mo2^i—O5—Mo3	97.2 (2)
Mo3—Mo2—O5	45.55 (16)	Mo1—O5—Mo4	85.31 (19)
O4—Mo2—O5	79.4 (2)	Mo2—O5—Mo4	163.5 (3)
Mo1—Mo2—O5^i	86.33 (14)	Mo2^i—O5—Mo4	91.81 (19)
Mo3—Mo2—O5^i	85.52 (14)	Mo3—O5—Mo4	85.58 (18)
O4—Mo2—O5^i	78.7 (2)	Mo1—O6—Mo2^i	110.5 (3)
O5—Mo2—O5^i	75.3 (2)	Mo1—O6—Mo3^i	103.9 (2)
Mo1—Mo2—O6^i	125.61 (17)	Mo2^i—O6—Mo3^i	107.0 (3)
Mo3—Mo2—O6^i	36.80 (17)	Mo2—O8—Mo4^i	117.8 (3)
O4—Mo2—O6^i	150.9 (2)	Mo3—O11—Mo4	114.5 (3)
O5—Mo2—O6^i	78.7 (2)	C1—N1—C2	111.7 (6)
O5^i—Mo2—O6^i	77.3 (2)	C1—N1—H1	109.3
Mo1—Mo2—O7	91.5 (2)	C2—N1—H1	109.1
Mo3—Mo2—O7	88.3 (2)	C1—N1—H2	109.4
O4—Mo2—O7	103.1 (3)	C2—N1—H2	108.5
O5—Mo2—O7	98.7 (3)	H1—N1—H2	108.8
O5^i—Mo2—O7	173.4 (2)	C4—N2—C5	111.5 (9)
Mo1—Mo2—O8	132.95 (19)	C4—N2—H9	110.5
Mo3—Mo2—O8	132.09 (19)	C5—N2—H9	108.3
O4—Mo2—O8	96.9 (2)	C4—N2—H10	110.0
O5—Mo2—O8	156.0 (2)	C5—N2—H10	108.4
O5^i—Mo2—O8	80.7 (2)	H9—N2—H10	108.0
O6^i—Mo2—O7	99.0 (3)	N1—C1—C2^ii	109.7 (7)
O6^i—Mo2—O8	95.3 (2)	N1—C1—C3	110.9 (7)
O7—Mo2—O8	105.2 (3)	C2^ii—C1—C3	112.8 (7)
Mo2—Mo3—Mo4	89.57 (3)	N1—C1—H3	109.8
Mo2—Mo3—O4^i	79.59 (14)	C2^ii—C1—H3	107.7
Mo4—Mo3—O4^i	87.55 (15)	C3—C1—H3	105.8
Mo2—Mo3—O5	41.47 (14)	N1—C2—C1^ii	110.9 (7)
Mo4—Mo3—O5	49.29 (14)	N1—C2—H7	108.6
O4^i—Mo3—O5	72.4 (2)	C1^ii—C2—H7	109.1
Mo2—Mo3—O6^i	36.17 (16)	N1—C2—H8	109.7
Mo4—Mo3—O6^i	123.51 (17)	C1^ii—C2—H8	110.3
O4^i—Mo3—O6^i	71.9 (2)	H7—C2—H8	108.2
O5—Mo3—O6^i	74.3 (2)	C1—C3—H4	110.1
Mo2—Mo3—O9	85.8 (2)	C1—C3—H5	109.3
Mo4—Mo3—O9	90.3 (2)	H4—C3—H5	109.5
O4^i—Mo3—O9	165.2 (2)	C1—C3—H6	109.7
O5—Mo3—O9	95.2 (3)	H4—C3—H6	109.4
O6^i—Mo3—O9	97.4 (3)	H5—C3—H6	108.9
Mo2—Mo3—O10	132.4 (2)	N2—C4—C5^iii	108.1 (9)
Mo4—Mo3—O10	135.2 (2)	N2—C4—C6	114.8 (9)
O4^i—Mo3—O10	86.2 (2)	C5^iii—C4—C6	111.8 (9)
O5—Mo3—O10	158.4 (2)	N2—C4—H11	107.9
O6^i—Mo3—O10	96.3 (3)	C5^iii—C4—H11	112.0
Mo2—Mo3—O11	120.21 (18)	C6—C4—H11	102.2
Mo4—Mo3—O11	32.85 (18)	N2—C5—C4^iii	110.1 (9)
O4^i—Mo3—O11	82.7 (2)	N2—C5—H15	110.3
O5—Mo3—O11	78.7 (2)	C4^iii—C5—H15	110.1
O6^i—Mo3—O11	147.3 (2)	N2—C5—H16	109.2
O9—Mo3—O10	105.4 (3)	C4^iii—C5—H16	109.6
O9—Mo3—O11	103.2 (3)	H15—C5—H16	107.5
O10—Mo3—O11	102.3 (3)	C4—C6—H12	109.6
Mo1—Mo4—Mo3	89.98 (3)	C4—C6—H13	109.6
Mo1—Mo4—O3	31.68 (17)	H12—C6—H13	109.5
Mo3—Mo4—O3	119.88 (18)	C4—C6—H14	109.2
Mo1—Mo4—O5	45.87 (14)	H12—C6—H14	109.4
Mo3—Mo4—O5	45.13 (14)	H13—C6—H14	109.6
O3—Mo4—O5	74.7 (2)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O13^iv	1.01	1.83	2.783 (9)	156
N1—H2···O6	1.00	1.92	2.871 (9)	158
N2—H9···O11^i	1.00	1.96	2.929 (11)	164
N2—H10···O12^v	1.02	1.92	2.882 (10)	156

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