(C₄H₁₄N₂)₂[Mo₈O₂₆]·2H₂O: a new molybdate salt

Crystals of the title compound, 2-(dimethyl­ammonio)­ethanaminium hexa­cosa­oxaocta­molybdate(VI) dihydrate, containing extended chains constructed from centrosymmetric octa­molybdate anions, were grown under mild hydro­thermal conditions in the presence of N,N-dimethyl­ethylenediamine. An extensive hydrogen-bonding network helps stabilize the crystal structure.

Key indicators

• Single-crystal X-ray study
• T = 110 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.026
• wR factor = 0.055
• Data-to-parameter ratio = 12.7

checkCIF/PLATON results

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Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       2.00 Ratio
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   4 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   3 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
   1 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 (Oxford Diffraction, 2004); data reduction: CrysAlis RED; 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-(dimethylammonio)ethanaminium hexacosaoxaoctamolybdate dihydrate

Crystal data

(C4H14N2)2[Mo8O26]·2H2O	Z = 1
Mr = 1399.88	F(000) = 668
Triclinic, P1	Dx = 2.928 Mg m^−3
a = 7.7451 (9) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.3145 (10) Å	Cell parameters from 3137 reflections
c = 10.8614 (11) Å	θ = 0.6–9.8°
α = 79.304 (8)°	µ = 3.16 mm^−1
β = 70.145 (10)°	T = 110 K
γ = 78.793 (9)°	Rod, colorless
V = 793.79 (15) Å^3	0.18 × 0.05 × 0.03 mm

Data collection

CrysAlis CCD diffractometer	2754 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.02
ω scans	θmax = 28.3°, θmin = 4.0°
Absorption correction: analytical (multifaceted crystal model; Clark & Reid, 1995)	h = −10→9
Tmin = 0.584, Tmax = 0.908	k = −13→13
7063 measured reflections	l = −14→8
3918 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)] = 0.027	H-atom parameters constrained
wR(F^2) = 0.055	Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A0*T0(x) + A1*T1(x) ··· + An-1]*Tn-1(x)] where Ai are the Chebychev coefficients listed below and x = F /Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 Ai are: 21.5 18.7 19.2 3.32 3.23
S = 0.90	(Δ/σ)max = 0.001
2754 reflections	Δρmax = 1.33 e Å^−3
217 parameters	Δρmin = −0.91 e Å^−3
0 restraints

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

	x	y	z	Uiso*/Ueq
Mo1	0.63926 (6)	0.24814 (4)	0.12848 (4)	0.0062
Mo2	0.79146 (6)	0.53429 (4)	0.11309 (4)	0.0056
Mo3	0.80704 (6)	0.50581 (4)	−0.18577 (4)	0.0060
Mo4	1.00602 (6)	0.77141 (4)	−0.23132 (4)	0.0069
O1	0.5347 (5)	0.1558 (4)	0.2750 (4)	0.0103
O2	0.6160 (5)	0.1700 (4)	0.0106 (4)	0.0103
O3	0.8941 (5)	0.1700 (4)	0.1103 (3)	0.0087
O4	0.5890 (5)	0.6126 (4)	−0.1586 (4)	0.0075
O5	0.7378 (5)	0.3756 (3)	0.2275 (3)	0.0071
O6	0.7473 (5)	0.4141 (3)	−0.0101 (3)	0.0068
O7	0.5858 (5)	0.6358 (4)	0.1471 (4)	0.0109
O8	0.9155 (5)	0.5996 (3)	0.1950 (3)	0.0075
O9	0.9195 (5)	0.6055 (4)	−0.0645 (4)	0.0084
O10	0.7998 (5)	0.3983 (4)	−0.2836 (4)	0.0108
O11	0.9488 (5)	0.6320 (4)	−0.3066 (3)	0.0084
O12	0.7918 (5)	0.8636 (4)	−0.1805 (4)	0.0111
O13	1.1221 (5)	0.8581 (4)	−0.3769 (4)	0.0120
O14	0.8636 (5)	0.8959 (4)	0.1375 (4)	0.0131
N1	0.7018 (6)	0.7558 (4)	0.3992 (4)	0.0121
N2	0.4796 (6)	0.9064 (5)	0.1902 (4)	0.0125
C1	0.5318 (7)	0.8605 (5)	0.4095 (5)	0.0118
C2	0.4099 (8)	0.8464 (6)	0.3322 (5)	0.0147
C3	0.8311 (8)	0.8022 (6)	0.4522 (6)	0.0194
C4	0.6512 (9)	0.6244 (6)	0.4698 (6)	0.0207
H1	0.9500	0.8423	0.0673	0.0154*
H2	0.9123	0.9806	0.1311	0.0154*
H3	0.7657	0.7435	0.3045	0.0142*
H4	0.6071	0.8605	0.1481	0.0166*
H5	0.3949	0.8950	0.1423	0.0166*
H6	0.4838	1.0036	0.1858	0.0166*
H7	0.4552	0.8568	0.5047	0.0147*
H8	0.5751	0.9497	0.3777	0.0147*
H9	0.2821	0.8926	0.3732	0.0173*
H10	0.4054	0.7495	0.3356	0.0173*
H11	0.9466	0.7362	0.4410	0.0235*
H12	0.7691	0.8108	0.5480	0.0235*
H13	0.8631	0.8907	0.4028	0.0235*
H14	0.5880	0.6317	0.5658	0.0231*
H15	0.5652	0.5957	0.4324	0.0231*
H16	0.7654	0.5571	0.4588	0.0231*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.00686 (18)	0.00558 (19)	0.00654 (18)	−0.00113 (14)	−0.00285 (14)	−0.00028 (15)
Mo2	0.00560 (18)	0.00501 (19)	0.00609 (18)	−0.00033 (14)	−0.00214 (14)	−0.00063 (14)
Mo3	0.00628 (18)	0.00615 (19)	0.00590 (18)	−0.00079 (14)	−0.00250 (15)	−0.00039 (14)
Mo4	0.00703 (18)	0.00619 (19)	0.00779 (19)	−0.00121 (14)	−0.00347 (15)	0.00076 (15)
O1	0.0058 (16)	0.0103 (17)	0.0154 (18)	−0.0009 (13)	−0.0041 (14)	−0.0023 (14)
O2	0.0111 (16)	0.0110 (17)	0.0104 (17)	0.0002 (14)	−0.0049 (14)	−0.0042 (14)
O3	0.0088 (16)	0.0079 (16)	0.0092 (16)	−0.0014 (13)	−0.0030 (13)	−0.0001 (13)
O4	0.0061 (15)	0.0079 (16)	0.0089 (16)	−0.0023 (13)	−0.0026 (13)	0.0002 (13)
O5	0.0091 (16)	0.0061 (16)	0.0061 (15)	−0.0022 (13)	−0.0014 (13)	−0.0016 (13)
O6	0.0084 (16)	0.0032 (15)	0.0071 (16)	−0.0002 (12)	−0.0007 (13)	−0.0008 (13)
O7	0.0099 (17)	0.0095 (17)	0.0123 (17)	0.0007 (14)	−0.0040 (14)	0.0000 (14)
O8	0.0096 (16)	0.0058 (16)	0.0055 (15)	−0.0002 (13)	−0.0010 (13)	−0.0002 (13)
O9	0.0081 (16)	0.0072 (16)	0.0096 (16)	−0.0002 (13)	−0.0035 (13)	0.0002 (13)
O10	0.0123 (17)	0.0102 (17)	0.0126 (18)	−0.0027 (14)	−0.0061 (14)	−0.0026 (14)
O11	0.0079 (16)	0.0077 (16)	0.0081 (16)	−0.0011 (13)	−0.0025 (13)	0.0029 (13)
O12	0.0105 (17)	0.0092 (17)	0.0131 (17)	0.0003 (14)	−0.0039 (14)	−0.0016 (14)
O13	0.0154 (18)	0.0117 (18)	0.0093 (17)	−0.0031 (14)	−0.0046 (14)	0.0005 (14)
O14	0.0123 (17)	0.0101 (18)	0.0153 (18)	0.0000 (14)	−0.0023 (14)	−0.0037 (15)
N1	0.015 (2)	0.011 (2)	0.008 (2)	0.0002 (17)	−0.0035 (17)	0.0007 (16)
N2	0.016 (2)	0.011 (2)	0.012 (2)	−0.0015 (17)	−0.0074 (18)	−0.0027 (17)
C1	0.014 (2)	0.009 (2)	0.013 (2)	−0.0004 (19)	−0.005 (2)	−0.0026 (19)
C2	0.012 (2)	0.018 (3)	0.012 (2)	0.000 (2)	0.000 (2)	−0.005 (2)
C3	0.016 (3)	0.024 (3)	0.018 (3)	0.004 (2)	−0.007 (2)	−0.007 (2)
C4	0.032 (3)	0.009 (2)	0.015 (3)	−0.002 (2)	0.000 (2)	−0.002 (2)

Geometric parameters (Å, º)

Mo1—O1	1.720 (4)	Mo4—O13	1.711 (4)
Mo1—O2	1.708 (4)	O14—H1	1.000
Mo1—O3	1.939 (4)	O14—H2	1.000
Mo1—O4^i	2.022 (4)	N1—C1	1.518 (7)
Mo1—O5	2.222 (4)	N1—C3	1.497 (8)
Mo1—O6	2.154 (3)	N1—C4	1.482 (7)
Mo2—O5	1.885 (4)	N1—H3	1.000
Mo2—O6	2.130 (4)	N2—C2	1.504 (7)
Mo2—O7	1.692 (4)	N2—H4	1.000
Mo2—O8	1.795 (4)	N2—H5	1.000
Mo2—O9	1.924 (4)	N2—H6	1.000
Mo2—O9^ii	2.365 (4)	C1—C2	1.501 (8)
Mo3—O4	1.792 (4)	C1—H7	1.000
Mo3—O6	1.911 (3)	C1—H8	1.000
Mo3—O8^ii	2.190 (3)	C2—H9	1.000
Mo3—O9	2.275 (4)	C2—H10	1.000
Mo3—O10	1.693 (4)	C3—H11	1.000
Mo3—O11	1.888 (4)	C3—H12	1.000
Mo4—O3^ii	1.964 (4)	C3—H13	1.000
Mo4—O5^ii	2.259 (4)	C4—H14	1.000
Mo4—O9	2.265 (4)	C4—H15	1.000
Mo4—O11	1.965 (4)	C4—H16	1.000
Mo4—O12	1.709 (4)
O1—Mo1—O2	104.21 (18)	O11—Mo4—O12	100.56 (16)
O1—Mo1—O3	98.01 (16)	O11—Mo4—O13	97.59 (16)
O2—Mo1—O3	96.25 (16)	O12—Mo4—O13	105.14 (18)
O1—Mo1—O4^i	89.90 (16)	Mo1—O3—Mo4^ii	113.22 (17)
O2—Mo1—O4^i	101.22 (16)	Mo1^i—O4—Mo3	172.7 (2)
O3—Mo1—O4^i	158.45 (16)	Mo1—O5—Mo2	108.59 (16)
O1—Mo1—O5	92.88 (15)	Mo1—O5—Mo4^ii	93.33 (13)
O2—Mo1—O5	162.00 (16)	Mo2—O5—Mo4^ii	113.08 (16)
O3—Mo1—O5	75.48 (14)	Mo1—O6—Mo2	102.52 (14)
O4^i—Mo1—O5	84.16 (14)	Mo1—O6—Mo3	149.2 (2)
O1—Mo1—O6	160.38 (16)	Mo2—O6—Mo3	108.09 (16)
O2—Mo1—O6	93.86 (16)	Mo2—O8—Mo3^ii	116.38 (17)
O3—Mo1—O6	87.38 (14)	Mo2—O9—Mo2^ii	102.95 (15)
O4^i—Mo1—O6	78.99 (13)	Mo2—O9—Mo3	102.08 (16)
O5—Mo1—O6	70.12 (13)	Mo2^ii—O9—Mo3	93.93 (13)
O5—Mo2—O6	77.29 (14)	Mo2—O9—Mo4	154.47 (19)
O5—Mo2—O7	103.89 (17)	Mo2^ii—O9—Mo4	96.80 (13)
O6—Mo2—O7	99.51 (16)	Mo3—O9—Mo4	92.43 (13)
O5—Mo2—O8	100.07 (15)	Mo3—O11—Mo4	116.54 (18)
O6—Mo2—O8	157.90 (14)	H1—O14—H2	109.6
O7—Mo2—O8	102.40 (17)	C1—N1—C3	109.1 (4)
O5—Mo2—O9	144.12 (15)	C1—N1—C4	111.7 (4)
O6—Mo2—O9	74.72 (14)	C3—N1—C4	111.0 (5)
O7—Mo2—O9	102.49 (17)	C1—N1—H3	109.1
O8—Mo2—O9	97.54 (16)	C3—N1—H3	109.2
O5—Mo2—O9^ii	76.71 (14)	C4—N1—H3	106.6
O6—Mo2—O9^ii	80.80 (13)	C2—N2—H4	109.3
O7—Mo2—O9^ii	179.37 (16)	C2—N2—H5	109.6
O8—Mo2—O9^ii	77.27 (14)	H4—N2—H5	109.5
O9—Mo2—O9^ii	77.05 (15)	C2—N2—H6	109.6
O4—Mo3—O6	94.84 (15)	H4—N2—H6	109.4
O4—Mo3—O8^ii	168.54 (16)	H5—N2—H6	109.4
O6—Mo3—O8^ii	81.95 (14)	N1—C1—C2	116.0 (4)
O4—Mo3—O9	96.23 (15)	N1—C1—H7	107.7
O6—Mo3—O9	71.56 (14)	C2—C1—H7	108.0
O8^ii—Mo3—O9	72.30 (13)	N1—C1—H8	107.8
O4—Mo3—O10	104.57 (18)	C2—C1—H8	107.8
O6—Mo3—O10	106.49 (17)	H7—C1—H8	109.5
O8^ii—Mo3—O10	86.89 (15)	N2—C2—C1	112.1 (4)
O4—Mo3—O11	95.65 (16)	N2—C2—H9	108.6
O6—Mo3—O11	144.96 (16)	C1—C2—H9	108.8
O8^ii—Mo3—O11	81.19 (14)	N2—C2—H10	108.9
O9—Mo3—O10	159.19 (15)	C1—C2—H10	108.8
O9—Mo3—O11	74.12 (15)	H9—C2—H10	109.5
O10—Mo3—O11	103.01 (17)	N1—C3—H11	109.5
O3^ii—Mo4—O5^ii	74.17 (14)	N1—C3—H12	109.3
O3^ii—Mo4—O9	84.15 (14)	H11—C3—H12	109.5
O5^ii—Mo4—O9	72.17 (12)	N1—C3—H13	109.2
O3^ii—Mo4—O11	152.05 (15)	H11—C3—H13	109.6
O5^ii—Mo4—O11	83.48 (13)	H12—C3—H13	109.6
O9—Mo4—O11	73.01 (14)	N1—C4—H14	109.4
O3^ii—Mo4—O12	95.77 (16)	N1—C4—H15	109.3
O5^ii—Mo4—O12	161.23 (16)	H14—C4—H15	109.4
O9—Mo4—O12	91.34 (16)	N1—C4—H16	109.7
O3^ii—Mo4—O13	99.85 (17)	H14—C4—H16	109.5
O5^ii—Mo4—O13	92.35 (15)	H15—C4—H16	109.5
O9—Mo4—O13	162.45 (15)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O14—H1···O3^ii	1.00	1.91	2.825 (5)	151
O14—H2···O3^iii	1.00	1.91	2.835 (5)	153
N1—H3···O8	1.00	2.00	2.838 (6)	139
N2—H4···O14	1.00	2.050	2.815 (6)	132
N2—H5···O2^i	1.00	1.936	2.809 (6)	144
N2—H6···O1^iii	1.00	2.151	3.036 (6)	147

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