Poly[bis­(4-amino­pyridinium) deca­oxotrimolybdate(VI)]

The hydro­thermally synthesized title compound, {(C₅H₇N₂)₂[Mo₃O₁₀]}_n, contains [Mo₃O₁₀]_n²ⁿ⁻ chains, which are generated through inversion symmetry. An extensive N—H...O hydrogen-bonding network is observed between the C₅H₇N₂⁺ cations and the chains.

Key indicators

• Single-crystal X-ray study
• T = 110 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.022
• wR factor = 0.046
• Data-to-parameter ratio = 14.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.84
PLAT432_ALERT_2_C Short Inter X...Y Contact  O8     ..  C5      ..       2.99 Ang.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 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
   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[bis(4-aminopyridinium) decaoxotrimolybdenum]

Crystal data

(C5H7N2)2[Mo3O10]	Z = 2
Mr = 638.06	F(000) = 616
Triclinic, P1	Dx = 2.565 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.045 (3) Å	Cell parameters from 6705 reflections
b = 10.376 (5) Å	θ = 3.8–32.0°
c = 11.538 (4) Å	µ = 2.31 mm^−1
α = 65.05 (4)°	T = 110 K
β = 89.94 (3)°	Needle, colorless
γ = 72.91 (3)°	0.22 × 0.10 × 0.07 mm
V = 826.3 (7) Å^3

Data collection

CrysAlis CCD diffractometer	3432 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.02
ω scans	θmax = 32.2°, θmin = 3.8°
Absorption correction: analytical multifaceted crystal model (Clark & Reid, 1995)	h = −11→11
Tmin = 0.76, Tmax = 0.85	k = −15→15
11942 measured reflections	l = −17→17
5309 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)] = 0.022	H-atom parameters constrained
wR(F^2) = 0.046	w = [1-(Fo-Fc)^2/36σ^2(F)]^2/[(0.176 × 10^5)To(x)- (0.227 × 10^5)T1(x) + (0.215 × 10^5)T2(x)- (0.768 × 10^4)T3(x) + (0.406 × 10^4)T4(x)] where Ti are the Chebychev polynomials and x = Fc/Fmax (Prince, 1982; Watkin, 1994)
S = 0.86	(Δ/σ)max = 0.001
3432 reflections	Δρmax = 1.56 e Å^−3
244 parameters	Δρmin = −0.55 e Å^−3
0 restraints

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

	x	y	z	Uiso*/Ueq
Mo1	0.70361 (3)	0.13745 (3)	0.77090 (2)	0.0070
Mo2	0.85271 (3)	0.12633 (3)	1.03909 (2)	0.0066
Mo3	0.36820 (3)	0.16537 (3)	0.90934 (2)	0.0066
O1	0.7593 (3)	0.2900 (3)	0.6703 (2)	0.0124
O2	0.7372 (3)	0.0265 (3)	0.6918 (2)	0.0121
O3	0.4522 (3)	0.2343 (2)	0.7382 (2)	0.0088
O4	0.9085 (3)	0.0290 (2)	0.9023 (2)	0.0082
O5	0.6353 (3)	0.1904 (2)	0.9383 (2)	0.0084
O6	0.4196 (3)	0.0373 (2)	1.0843 (2)	0.0079
O7	0.9133 (3)	0.2824 (3)	0.9646 (2)	0.0112
O8	0.8108 (3)	0.1256 (3)	1.1855 (2)	0.0108
O9	0.2041 (3)	0.1114 (2)	0.8643 (2)	0.0094
O10	0.2642 (3)	0.3350 (3)	0.9085 (2)	0.0108
N1	0.5752 (4)	−0.2276 (3)	0.7936 (3)	0.0113
N2	0.3959 (4)	−0.4380 (3)	0.6132 (3)	0.0133
N3	0.8192 (5)	−0.2675 (4)	0.4450 (3)	0.0231
N4	1.0494 (4)	−0.3557 (4)	0.7974 (3)	0.0214
C1	0.5932 (4)	−0.3743 (4)	0.8591 (3)	0.0122
C2	0.5347 (4)	−0.4477 (4)	0.8019 (3)	0.0121
C3	0.4523 (4)	−0.3684 (3)	0.6721 (3)	0.0093
C4	0.4337 (4)	−0.2145 (4)	0.6074 (3)	0.0109
C5	0.4964 (4)	−0.1487 (4)	0.6702 (3)	0.0117
C6	0.8392 (5)	−0.4000 (4)	0.5461 (4)	0.0208
C7	0.9199 (5)	−0.4360 (4)	0.6640 (3)	0.0137
C8	0.9788 (4)	−0.3286 (4)	0.6818 (3)	0.0108
C9	0.9591 (5)	−0.1914 (4)	0.5728 (4)	0.0169
C10	0.8817 (5)	−0.1654 (4)	0.4562 (4)	0.0210
H1	0.6210	−0.1768	0.8369	0.0147*
H2	0.6501	−0.4307	0.9512	0.0144*
H3	0.5504	−0.5571	0.8517	0.0135*
H4	0.3750	−0.1539	0.5159	0.0133*
H5	0.4831	−0.0394	0.6235	0.0146*
H6	0.4108	−0.5474	0.6614	0.0167*
H7	0.3391	−0.3806	0.5211	0.0167*
H8	0.7571	−0.2438	0.3599	0.0238*
H9	0.7936	−0.4742	0.5344	0.0268*
H10	0.9374	−0.5369	0.7376	0.0173*
H11	1.0013	−0.1138	0.5811	0.0198*
H12	0.8716	−0.0697	0.3783	0.0211*
H13	1.0890	−0.2781	0.8080	0.0251*
H14	1.0624	−0.4536	0.8737	0.0251*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.00710 (11)	0.00792 (11)	0.00564 (11)	−0.00268 (9)	−0.00009 (8)	−0.00263 (9)
Mo2	0.00644 (11)	0.00693 (11)	0.00677 (11)	−0.00194 (9)	−0.00027 (8)	−0.00354 (9)
Mo3	0.00656 (11)	0.00625 (11)	0.00653 (11)	−0.00215 (9)	−0.00025 (8)	−0.00245 (9)
O1	0.0135 (11)	0.0105 (10)	0.0105 (10)	−0.0054 (8)	0.0004 (8)	−0.0011 (8)
O2	0.0134 (11)	0.0140 (11)	0.0103 (10)	−0.0043 (9)	0.0011 (8)	−0.0068 (9)
O3	0.0095 (10)	0.0093 (10)	0.0064 (9)	−0.0031 (8)	0.0002 (7)	−0.0022 (8)
O4	0.0089 (9)	0.0096 (10)	0.0072 (9)	−0.0026 (8)	0.0007 (7)	−0.0050 (8)
O5	0.0076 (9)	0.0100 (10)	0.0070 (9)	−0.0017 (8)	−0.0012 (7)	−0.0040 (8)
O6	0.0092 (9)	0.0067 (9)	0.0073 (9)	−0.0023 (7)	0.0010 (7)	−0.0029 (8)
O7	0.0118 (10)	0.0087 (10)	0.0134 (10)	−0.0041 (8)	0.0013 (8)	−0.0045 (9)
O8	0.0112 (10)	0.0134 (11)	0.0084 (10)	−0.0032 (8)	0.0008 (8)	−0.0059 (8)
O9	0.0056 (9)	0.0060 (9)	0.0161 (11)	−0.0007 (7)	−0.0025 (8)	−0.0051 (9)
O10	0.0115 (10)	0.0082 (10)	0.0110 (10)	−0.0019 (8)	−0.0005 (8)	−0.0035 (8)
N1	0.0123 (12)	0.0135 (13)	0.0112 (12)	−0.0053 (10)	0.0009 (10)	−0.0078 (10)
N2	0.0180 (13)	0.0093 (12)	0.0123 (12)	−0.0041 (10)	−0.0034 (10)	−0.0047 (10)
N3	0.0284 (17)	0.0209 (16)	0.0108 (13)	0.0034 (13)	−0.0072 (12)	−0.0060 (12)
N4	0.0277 (17)	0.0144 (14)	0.0192 (15)	0.0013 (12)	−0.0096 (12)	−0.0101 (12)
C1	0.0131 (14)	0.0133 (14)	0.0096 (13)	−0.0042 (11)	−0.0012 (11)	−0.0046 (11)
C2	0.0129 (14)	0.0107 (14)	0.0106 (13)	−0.0035 (11)	−0.0017 (11)	−0.0030 (11)
C3	0.0095 (13)	0.0110 (13)	0.0083 (13)	−0.0019 (10)	0.0019 (10)	−0.0060 (11)
C4	0.0131 (14)	0.0109 (13)	0.0088 (13)	−0.0042 (11)	0.0007 (10)	−0.0040 (11)
C5	0.0137 (14)	0.0095 (13)	0.0124 (14)	−0.0038 (11)	0.0019 (11)	−0.0053 (11)
C6	0.0173 (16)	0.0227 (18)	0.0270 (19)	−0.0053 (14)	−0.0020 (14)	−0.0160 (16)
C7	0.0166 (15)	0.0130 (14)	0.0131 (14)	−0.0058 (12)	0.0021 (12)	−0.0066 (12)
C8	0.0115 (13)	0.0094 (13)	0.0121 (13)	−0.0008 (11)	0.0002 (11)	−0.0069 (11)
C9	0.0185 (16)	0.0104 (14)	0.0206 (17)	−0.0046 (12)	0.0016 (13)	−0.0058 (13)
C10	0.0258 (19)	0.0132 (16)	0.0142 (15)	−0.0008 (14)	0.0044 (14)	−0.0006 (13)

Geometric parameters (Å, º)

Mo1—O1	1.709 (2)	N2—H7	1.000
Mo1—O2	1.713 (2)	N3—C6	1.339 (5)
Mo1—O3	1.931 (2)	N3—C10	1.349 (5)
Mo1—O4	1.938 (2)	N3—H8	1.000
Mo1—O5	2.247 (2)	N4—C8	1.332 (4)
Mo1—O6^i	2.358 (2)	N4—H13	1.000
Mo2—O4	2.188 (2)	N4—H14	1.000
Mo2—O4^ii	2.002 (2)	C1—C2	1.368 (4)
Mo2—O5	1.877 (2)	C1—H2	1.000
Mo2—O7	1.700 (2)	C2—C3	1.415 (4)
Mo2—O8	1.720 (2)	C2—H3	1.000
Mo2—O9^i	2.424 (2)	C3—C4	1.409 (4)
Mo3—O3	1.990 (2)	C4—C5	1.367 (4)
Mo3—O5	2.280 (2)	C4—H4	1.000
Mo3—O6	1.852 (2)	C5—H5	1.000
Mo3—O6^i	2.258 (2)	C6—C7	1.357 (5)
Mo3—O9	1.735 (2)	C6—H9	1.000
Mo3—O10	1.708 (2)	C7—C8	1.418 (4)
N1—C1	1.345 (4)	C7—H10	1.000
N1—C5	1.346 (4)	C8—C9	1.411 (5)
N1—H1	1.000	C9—C10	1.366 (5)
N2—C3	1.339 (4)	C9—H11	1.000
N2—H6	1.000	C10—H12	1.000
O1—Mo1—O2	104.11 (11)	O9—Mo3—O10	105.75 (11)
O1—Mo1—O3	97.43 (10)	C1—N1—C5	120.6 (3)
O2—Mo1—O3	103.93 (10)	C1—N1—H1	119.7
O1—Mo1—O4	100.82 (10)	C5—N1—H1	119.7
O2—Mo1—O4	100.31 (10)	C3—N2—H6	120.0
O3—Mo1—O4	144.92 (9)	C3—N2—H7	120.0
O1—Mo1—O5	101.74 (10)	H6—N2—H7	120.000
O2—Mo1—O5	154.09 (10)	C6—N3—C10	121.0 (3)
O3—Mo1—O5	74.31 (8)	C6—N3—H8	119.5
O1—Mo1—O6^i	168.53 (10)	C10—N3—H8	119.5
O2—Mo1—O6^i	84.69 (10)	C8—N4—H13	120.0
O3—Mo1—O6^i	73.00 (8)	C8—N4—H14	120.0
O4—Mo1—O5	72.80 (8)	H13—N4—H14	120.000
O4—Mo1—O6^i	84.53 (8)	N1—C1—C2	121.2 (3)
O5—Mo1—O6^i	69.95 (8)	N1—C1—H2	119.5
O4—Mo2—O4^ii	71.07 (10)	C2—C1—H2	119.4
O4—Mo2—O5	75.31 (9)	C1—C2—C3	119.8 (3)
O4^ii—Mo2—O5	143.92 (9)	C1—C2—H3	120.1
O4—Mo2—O7	100.90 (10)	C3—C2—H3	120.1
O4^ii—Mo2—O7	98.92 (10)	N2—C3—C2	121.0 (3)
O5—Mo2—O7	99.90 (10)	N2—C3—C4	121.6 (3)
O4—Mo2—O8	155.51 (10)	C2—C3—C4	117.3 (3)
O4^ii—Mo2—O8	98.10 (10)	C3—C4—C5	119.7 (3)
O5—Mo2—O8	107.44 (10)	C3—C4—H4	120.1
O7—Mo2—O8	102.49 (11)	C5—C4—H4	120.2
O4—Mo2—O9^i	73.53 (8)	N1—C5—C4	121.4 (3)
O4^ii—Mo2—O9^i	75.48 (8)	N1—C5—H5	119.4
O5—Mo2—O9^i	82.88 (8)	C4—C5—H5	119.2
O7—Mo2—O9^i	173.05 (10)	N3—C6—C7	121.6 (3)
O8—Mo2—O9^i	82.58 (10)	N3—C6—H9	119.2
O3—Mo3—O5	72.52 (8)	C7—C6—H9	119.2
O3—Mo3—O6	147.82 (9)	C6—C7—C8	119.2 (3)
O5—Mo3—O6	83.90 (9)	C6—C7—H10	120.5
O3—Mo3—O6^i	74.29 (8)	C8—C7—H10	120.4
O5—Mo3—O6^i	71.17 (8)	N4—C8—C7	121.2 (3)
O6—Mo3—O6^i	77.59 (10)	N4—C8—C9	121.0 (3)
O3—Mo3—O9	95.72 (10)	C7—C8—C9	117.7 (3)
O5—Mo3—O9	161.37 (9)	C8—C9—C10	119.6 (3)
O6—Mo3—O9	100.61 (10)	C8—C9—H11	120.1
O3—Mo3—O10	99.86 (10)	C10—C9—H11	120.4
O5—Mo3—O10	90.75 (10)	N3—C10—C9	120.7 (3)
O6—Mo3—O10	102.07 (10)	N3—C10—H12	119.7
O6^i—Mo3—O9	91.99 (9)	C9—C10—H12	119.6
O6^i—Mo3—O10	161.89 (10)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O6^i	1.00	1.96	2.877 (3)	151
N2—H6···O3^iii	1.00	1.97	2.967 (4)	173
N2—H7···O1^iv	1.00	2.05	3.043 (4)	172
N3—H8···O3^iv	1.00	1.99	2.883 (4)	148
N4—H13···O8^ii	1.00	2.00	2.997 (4)	173
N4—H14···O10^v	1.00	2.19	2.864 (4)	124

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