Poly[tetra­kis(4-amino­pyridinium) [hexa­deca-μ-oxo-deca­oxoocta­molybdate(VI)]]

The title compound, {(C₅H₇N₂)₄[Mo₈O₂₆]}_n, contains extended [Mo₈O₂₆]_n⁴ⁿ⁻ chains, built up from distorted MoO₆ octa­hedra sharing vertices and edges. A network of N—H...O hydrogen bonds helps to stabilize the crystal packing.

Key indicators

• Single-crystal X-ray study
• T = 110 K
• Mean [sigma](C-C) = 0.007 Å
• R factor = 0.022
• wR factor = 0.047
• Data-to-parameter ratio = 11.4

checkCIF/PLATON results

No syntax errors found



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
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.36
PLAT432_ALERT_2_C Short Inter X...Y Contact  O2     ..  C7      ..       3.01 Ang.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 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
   2 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
   0 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.

Poly[tetrakis(4-aminopyridinium) [hexadeca-µ-oxo-decaoxooctamolybdate]]

Crystal data

4C5H7N2^+·Mo8O26^4^−	Z = 1
Mr = 1564.00	F(000) = 748
Triclinic, P1	Dx = 2.684 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.7680 (18) Å	Cell parameters from 5670 reflections
b = 11.923 (2) Å	θ = 4–29°
c = 12.208 (4) Å	µ = 2.61 mm^−1
α = 63.03 (2)°	T = 110 K
β = 74.37 (2)°	Block, colorless
γ = 79.220 (17)°	0.07 × 0.04 × 0.02 mm
V = 967.7 (5) Å^3

Data collection

CrysAlis CCD diffractometer	3196 reflections with I > 3.00σ(I)
Graphite monochromator	Rint = 0.02
ω scans	θmax = 29.1°, θmin = 3.8°
Absorption correction: multi-scan (DENZO/SCALEPACK; Otwinowski & Minor, 1997)	h = −10→10
Tmin = 0.88, Tmax = 0.95	k = −16→14
10827 measured reflections	l = −16→16
5089 independent reflections

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.022	w = [1-(Fo-Fc)^2/36σ^2(F)]^2/[A0To(x)-A1T1(x)··· + An-1T2(x)] where Ti are the Chebychev polynomials, x = Fc/Fmax and Ai are 0.511 × 10^4, -0.633 × 10^4, 0.587 × 10^4, -0.203 × 10^4, 891 (Prince, 1982; Watkin, 1994)
wR(F^2) = 0.047	(Δ/σ)max < 0.001
S = 0.88	Δρmax = 0.78 e Å^−3
3196 reflections	Δρmin = −0.71 e Å^−3
281 parameters	Extinction correction: Larson (1970)
0 restraints	Extinction coefficient: 3.2 (7)
Primary atom site location: structure-invariant direct methods

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

	x	y	z	Uiso*/Ueq
Mo1	0.56992 (5)	0.08764 (3)	0.19106 (3)	0.0066
Mo2	0.28413 (4)	−0.10542 (3)	0.41749 (3)	0.0057
Mo3	0.31667 (4)	0.09830 (3)	0.52015 (3)	0.0055
Mo4	0.06135 (5)	−0.12952 (3)	0.75724 (3)	0.0061
O1	0.6948 (4)	0.0655 (3)	0.0626 (3)	0.0119
O2	0.3984 (4)	0.1935 (3)	0.1395 (3)	0.0124
O3	0.7124 (4)	0.2014 (3)	0.1963 (3)	0.0077
O4	0.4504 (4)	0.0457 (3)	0.3897 (3)	0.0066
O5	0.4558 (4)	−0.0749 (3)	0.2665 (3)	0.0085
O6	0.2282 (4)	−0.2541 (3)	0.4646 (3)	0.0098
O7	0.1079 (4)	−0.0039 (3)	0.3449 (3)	0.0082
O8	0.2145 (4)	−0.0760 (3)	0.5643 (3)	0.0076
O9	0.4746 (4)	0.1995 (3)	0.5011 (3)	0.0075
O10	0.1527 (4)	0.2011 (3)	0.4521 (3)	0.0108
O11	0.2189 (4)	0.0386 (3)	0.6931 (3)	0.0080
O12	−0.0533 (4)	−0.1155 (3)	0.8917 (3)	0.0103
O13	−0.0071 (4)	−0.2627 (3)	0.7687 (3)	0.0098
N1	0.0309 (6)	0.4543 (4)	0.3044 (4)	0.0212
N2	0.0474 (5)	0.8363 (4)	0.1687 (4)	0.0172
N3	0.4038 (6)	0.5833 (3)	0.7390 (4)	0.0179
N4	0.3625 (5)	0.2029 (3)	0.8874 (4)	0.0137
C1	0.1371 (7)	0.5179 (5)	0.1918 (5)	0.0215
C2	0.1466 (7)	0.6445 (4)	0.1434 (5)	0.0175
C3	0.0425 (6)	0.7125 (4)	0.2118 (4)	0.0142
C4	−0.0673 (7)	0.6430 (4)	0.3295 (4)	0.0169
C5	−0.0699 (7)	0.5146 (4)	0.3726 (5)	0.0212
C6	0.3006 (7)	0.5248 (4)	0.8539 (5)	0.0168
C7	0.2841 (6)	0.3975 (4)	0.9067 (4)	0.0126
C8	0.3771 (6)	0.3262 (4)	0.8400 (4)	0.0115
C9	0.4855 (6)	0.3913 (4)	0.7194 (4)	0.0158
C10	0.4944 (7)	0.5181 (5)	0.6722 (5)	0.0210
H1	0.0274	0.3610	0.3374	0.0275*
H2	0.2111	0.4704	0.1426	0.0280*
H3	0.2272	0.6903	0.0594	0.0220*
H4	−0.1430	0.6873	0.3813	0.0213*
H5	−0.1485	0.4652	0.4563	0.0252*
H6	0.1254	0.8843	0.0854	0.0202*
H7	−0.0266	0.8814	0.2195	0.0202*
H8	0.4136	0.6764	0.7026	0.0208*
H9	0.2345	0.5756	0.9015	0.0204*
H10	0.2062	0.3550	0.9925	0.0147*
H11	0.5560	0.3435	0.6695	0.0177*
H12	0.5693	0.5645	0.5857	0.0237*
H13	0.2841	0.1591	0.9719	0.0152*
H14	0.4296	0.1539	0.8387	0.0152*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.00654 (16)	0.00691 (15)	0.00559 (16)	−0.00138 (12)	−0.00033 (12)	−0.00221 (12)
Mo2	0.00555 (15)	0.00549 (14)	0.00600 (16)	−0.00114 (11)	−0.00026 (12)	−0.00277 (12)
Mo3	0.00527 (15)	0.00515 (14)	0.00550 (16)	−0.00042 (11)	−0.00020 (12)	−0.00228 (12)
Mo4	0.00656 (15)	0.00585 (15)	0.00573 (16)	−0.00130 (11)	−0.00049 (12)	−0.00235 (12)
O1	0.0113 (14)	0.0142 (14)	0.0098 (15)	−0.0025 (12)	0.0010 (11)	−0.0061 (12)
O2	0.0097 (14)	0.0123 (14)	0.0129 (15)	0.0019 (11)	−0.0043 (12)	−0.0034 (12)
O3	0.0090 (13)	0.0052 (12)	0.0081 (14)	0.0019 (10)	−0.0020 (11)	−0.0029 (11)
O4	0.0067 (13)	0.0073 (12)	0.0067 (13)	−0.0005 (10)	−0.0018 (10)	−0.0035 (11)
O5	0.0089 (13)	0.0074 (13)	0.0081 (14)	−0.0032 (10)	0.0007 (11)	−0.0029 (11)
O6	0.0098 (14)	0.0078 (13)	0.0112 (14)	−0.0005 (11)	−0.0020 (11)	−0.0038 (11)
O7	0.0067 (13)	0.0074 (13)	0.0094 (14)	−0.0009 (10)	−0.0012 (11)	−0.0027 (11)
O8	0.0074 (13)	0.0053 (12)	0.0084 (14)	−0.0012 (10)	0.0004 (11)	−0.0024 (11)
O9	0.0065 (13)	0.0079 (13)	0.0081 (14)	−0.0007 (10)	−0.0015 (11)	−0.0033 (11)
O10	0.0112 (14)	0.0089 (13)	0.0093 (14)	0.0004 (11)	−0.0020 (11)	−0.0018 (11)
O11	0.0077 (13)	0.0062 (12)	0.0089 (14)	−0.0006 (10)	0.0000 (11)	−0.0030 (11)
O12	0.0097 (14)	0.0114 (14)	0.0100 (15)	0.0006 (11)	−0.0025 (11)	−0.0050 (12)
O13	0.0086 (13)	0.0098 (13)	0.0114 (14)	0.0007 (11)	−0.0031 (11)	−0.0047 (11)
N1	0.035 (2)	0.0073 (17)	0.026 (2)	−0.0003 (16)	−0.0168 (19)	−0.0055 (16)
N2	0.021 (2)	0.0119 (17)	0.017 (2)	−0.0057 (15)	0.0080 (16)	−0.0096 (15)
N3	0.023 (2)	0.0041 (15)	0.025 (2)	0.0003 (14)	−0.0076 (17)	−0.0044 (15)
N4	0.0183 (18)	0.0092 (16)	0.0106 (17)	−0.0009 (14)	0.0025 (14)	−0.0048 (14)
C1	0.027 (3)	0.017 (2)	0.026 (3)	0.0049 (19)	−0.008 (2)	−0.015 (2)
C2	0.021 (2)	0.016 (2)	0.016 (2)	−0.0004 (18)	−0.0035 (18)	−0.0079 (18)
C3	0.016 (2)	0.013 (2)	0.014 (2)	−0.0001 (16)	−0.0032 (17)	−0.0060 (17)
C4	0.024 (2)	0.012 (2)	0.015 (2)	−0.0054 (17)	0.0004 (18)	−0.0071 (17)
C5	0.036 (3)	0.013 (2)	0.016 (2)	−0.006 (2)	−0.005 (2)	−0.0062 (18)
C6	0.021 (2)	0.013 (2)	0.019 (2)	0.0029 (17)	−0.0084 (18)	−0.0080 (17)
C7	0.0134 (19)	0.0139 (19)	0.0093 (19)	0.0009 (15)	−0.0023 (16)	−0.0046 (16)
C8	0.0123 (19)	0.0107 (18)	0.010 (2)	0.0004 (15)	−0.0066 (16)	−0.0017 (16)
C9	0.018 (2)	0.012 (2)	0.014 (2)	−0.0019 (16)	0.0003 (17)	−0.0044 (17)
C10	0.016 (2)	0.016 (2)	0.023 (3)	−0.0042 (18)	−0.0001 (19)	−0.0032 (19)

Geometric parameters (Å, º)

Mo1—O1	1.712 (3)	N1—H1	1.000
Mo1—O2	1.693 (3)	N2—C3	1.327 (6)
Mo1—O3	1.936 (3)	N2—H6	1.000
Mo1—O4	2.204 (3)	N2—H7	1.000
Mo1—O5	1.994 (3)	N3—C6	1.346 (6)
Mo1—O11^i	2.314 (3)	N3—C10	1.352 (6)
Mo2—O4	2.261 (3)	N3—H8	1.000
Mo2—O5	1.886 (3)	N4—C8	1.328 (5)
Mo2—O6	1.701 (3)	N4—H13	1.000
Mo2—O7	1.785 (3)	N4—H14	1.000
Mo2—O8	1.899 (3)	C1—C2	1.357 (6)
Mo2—O9^i	2.228 (3)	C1—H2	1.007
Mo3—O4	1.943 (3)	C2—C3	1.419 (6)
Mo3—O4^i	2.373 (3)	C2—H3	1.008
Mo3—O8	2.147 (3)	C3—C4	1.415 (6)
Mo3—O9	1.777 (3)	C4—C5	1.377 (6)
Mo3—O10	1.696 (3)	C4—H4	1.005
Mo3—O11	1.875 (3)	C5—H5	1.008
Mo4—O3^i	1.918 (3)	C6—C7	1.370 (6)
Mo4—O7^ii	2.029 (3)	C6—H9	1.006
Mo4—O8	2.187 (3)	C7—C8	1.410 (6)
Mo4—O11	2.260 (3)	C7—H10	1.005
Mo4—O12	1.709 (3)	C8—C9	1.421 (6)
Mo4—O13	1.702 (3)	C9—C10	1.360 (6)
N1—C1	1.350 (7)	C9—H11	1.007
N1—C5	1.342 (7)	C10—H12	1.009
O1—Mo1—O2	105.34 (15)	O3^i—Mo4—O12	99.38 (13)
O1—Mo1—O3	100.73 (14)	O7^ii—Mo4—O12	91.79 (13)
O2—Mo1—O3	97.73 (13)	O8—Mo4—O12	159.50 (13)
O1—Mo1—O4	159.21 (12)	O11—Mo4—O12	92.60 (12)
O2—Mo1—O4	93.04 (13)	O3^i—Mo4—O13	97.18 (13)
O3—Mo1—O4	86.02 (11)	O7^ii—Mo4—O13	100.72 (13)
O1—Mo1—O5	93.66 (13)	O8—Mo4—O13	94.22 (12)
O2—Mo1—O5	101.46 (13)	O11—Mo4—O13	161.91 (13)
O3—Mo1—O5	152.00 (12)	O12—Mo4—O13	105.01 (15)
O1—Mo1—O11^i	90.09 (12)	C1—N1—C5	120.9 (4)
O2—Mo1—O11^i	163.72 (13)	C1—N1—H1	119.5
O3—Mo1—O11^i	73.86 (11)	C5—N1—H1	119.6
O4—Mo1—O5	72.86 (11)	C3—N2—H6	119.9
O4—Mo1—O11^i	72.77 (10)	C3—N2—H7	120.1
O5—Mo1—O11^i	82.30 (11)	H6—N2—H7	120.0
O4—Mo2—O5	73.46 (11)	C6—N3—C10	120.9 (4)
O4—Mo2—O6	157.19 (12)	C6—N3—H8	119.6
O5—Mo2—O6	103.64 (13)	C10—N3—H8	119.5
O4—Mo2—O7	97.84 (12)	C8—N4—H13	119.9
O5—Mo2—O7	95.80 (13)	C8—N4—H14	120.1
O6—Mo2—O7	104.97 (14)	H13—N4—H14	120.0
O4—Mo2—O8	72.19 (11)	N1—C1—C2	121.6 (4)
O5—Mo2—O8	144.95 (12)	N1—C1—H2	119.3
O6—Mo2—O8	105.26 (13)	C2—C1—H2	119.1
O4—Mo2—O9^i	71.68 (10)	C1—C2—C3	119.7 (5)
O5—Mo2—O9^i	81.31 (12)	C1—C2—H3	120.3
O6—Mo2—O9^i	85.51 (12)	C3—C2—H3	120.0
O7—Mo2—O8	95.49 (13)	N2—C3—C2	122.0 (4)
O7—Mo2—O9^i	169.51 (12)	N2—C3—C4	120.7 (4)
O8—Mo2—O9^i	81.61 (11)	C2—C3—C4	117.4 (4)
O4—Mo3—O4^i	75.97 (12)	C3—C4—C5	119.7 (4)
O4—Mo3—O8	74.04 (11)	C3—C4—H4	120.1
O4^i—Mo3—O8	80.42 (10)	C5—C4—H4	120.3
O4—Mo3—O9	96.92 (12)	N1—C5—C4	120.8 (5)
O4^i—Mo3—O9	77.13 (11)	N1—C5—H5	119.6
O8—Mo3—O9	157.27 (12)	C4—C5—H5	119.6
O4—Mo3—O10	102.55 (13)	N3—C6—C7	121.1 (4)
O4^i—Mo3—O10	178.50 (12)	N3—C6—H9	119.3
O8—Mo3—O10	99.40 (13)	C7—C6—H9	119.6
O9—Mo3—O10	102.95 (14)	C6—C7—C8	119.6 (4)
O4—Mo3—O11	143.34 (12)	C6—C7—H10	120.3
O4^i—Mo3—O11	77.30 (11)	C8—C7—H10	120.1
O8—Mo3—O11	77.15 (12)	N4—C8—C7	121.3 (4)
O9—Mo3—O11	101.09 (13)	N4—C8—C9	121.1 (4)
O10—Mo3—O11	104.13 (13)	C7—C8—C9	117.6 (4)
O3^i—Mo4—O7^ii	155.67 (12)	C8—C9—C10	119.7 (4)
O3^i—Mo4—O8	84.91 (11)	C8—C9—H11	120.0
O7^ii—Mo4—O8	77.50 (11)	C10—C9—H11	120.3
O3^i—Mo4—O11	75.47 (11)	N3—C10—C9	121.1 (5)
O7^ii—Mo4—O11	82.53 (11)	N3—C10—H12	119.4
O8—Mo4—O11	68.92 (11)	C9—C10—H12	119.6

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O10	1.00	2.04	2.859 (5)	138
N1—H1···O13^ii	1.00	2.15	2.854 (5)	126
N2—H6···O1^iii	1.00	1.88	2.861 (5)	165
N2—H7···O11^iv	1.00	1.95	2.932 (5)	166
N3—H8···O3^v	1.00	2.25	2.934 (5)	125
N3—H8···O9^v	1.00	2.26	2.955 (5)	125
N4—H13···O12^vi	1.00	2.05	3.004 (5)	158
N4—H14···O5^i	1.00	1.87	2.867 (5)	174

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