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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680602486X/hb2099sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680602486X/hb2099Isup2.hkl
Contains datablock I

CCDC reference: 618206

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

Computing details top

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]] top
Crystal data top
4C5H7N2+·Mo8O264Z = 1
Mr = 1564.00F(000) = 748
Triclinic, P1Dx = 2.684 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.7680 (18) ÅCell parameters from 5670 reflections
b = 11.923 (2) Åθ = 4–29°
c = 12.208 (4) ŵ = 2.61 mm1
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) Å3
Data collection top
CrysAlis CCD
diffractometer
3196 reflections with I > 3.00σ(I)
Graphite monochromatorRint = 0.02
ω scansθmax = 29.1°, θmin = 3.8°
Absorption correction: multi-scan
(DENZO/SCALEPACK; Otwinowski & Minor, 1997)
h = 1010
Tmin = 0.88, Tmax = 0.95k = 1614
10827 measured reflectionsl = 1616
5089 independent reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.022 w = [1-(Fo-Fc)2/36σ2(F)]2/[A0To(x)-A1T1(x)··· + An-1T2(x)]
where Ti are the Chebychev polynomials, x = Fc/Fmax and Ai are 0.511 × 104, -0.633 × 104, 0.587 × 104, -0.203 × 104, 891 (Prince, 1982; Watkin, 1994)
wR(F2) = 0.047(Δ/σ)max < 0.001
S = 0.88Δρmax = 0.78 e Å3
3196 reflectionsΔρmin = 0.71 e Å3
281 parametersExtinction correction: Larson (1970)
0 restraintsExtinction coefficient: 3.2 (7)
Primary atom site location: structure-invariant direct methods
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.56992 (5)0.08764 (3)0.19106 (3)0.0066
Mo20.28413 (4)0.10542 (3)0.41749 (3)0.0057
Mo30.31667 (4)0.09830 (3)0.52015 (3)0.0055
Mo40.06135 (5)0.12952 (3)0.75724 (3)0.0061
O10.6948 (4)0.0655 (3)0.0626 (3)0.0119
O20.3984 (4)0.1935 (3)0.1395 (3)0.0124
O30.7124 (4)0.2014 (3)0.1963 (3)0.0077
O40.4504 (4)0.0457 (3)0.3897 (3)0.0066
O50.4558 (4)0.0749 (3)0.2665 (3)0.0085
O60.2282 (4)0.2541 (3)0.4646 (3)0.0098
O70.1079 (4)0.0039 (3)0.3449 (3)0.0082
O80.2145 (4)0.0760 (3)0.5643 (3)0.0076
O90.4746 (4)0.1995 (3)0.5011 (3)0.0075
O100.1527 (4)0.2011 (3)0.4521 (3)0.0108
O110.2189 (4)0.0386 (3)0.6931 (3)0.0080
O120.0533 (4)0.1155 (3)0.8917 (3)0.0103
O130.0071 (4)0.2627 (3)0.7687 (3)0.0098
N10.0309 (6)0.4543 (4)0.3044 (4)0.0212
N20.0474 (5)0.8363 (4)0.1687 (4)0.0172
N30.4038 (6)0.5833 (3)0.7390 (4)0.0179
N40.3625 (5)0.2029 (3)0.8874 (4)0.0137
C10.1371 (7)0.5179 (5)0.1918 (5)0.0215
C20.1466 (7)0.6445 (4)0.1434 (5)0.0175
C30.0425 (6)0.7125 (4)0.2118 (4)0.0142
C40.0673 (7)0.6430 (4)0.3295 (4)0.0169
C50.0699 (7)0.5146 (4)0.3726 (5)0.0212
C60.3006 (7)0.5248 (4)0.8539 (5)0.0168
C70.2841 (6)0.3975 (4)0.9067 (4)0.0126
C80.3771 (6)0.3262 (4)0.8400 (4)0.0115
C90.4855 (6)0.3913 (4)0.7194 (4)0.0158
C100.4944 (7)0.5181 (5)0.6722 (5)0.0210
H10.02740.36100.33740.0275*
H20.21110.47040.14260.0280*
H30.22720.69030.05940.0220*
H40.14300.68730.38130.0213*
H50.14850.46520.45630.0252*
H60.12540.88430.08540.0202*
H70.02660.88140.21950.0202*
H80.41360.67640.70260.0208*
H90.23450.57560.90150.0204*
H100.20620.35500.99250.0147*
H110.55600.34350.66950.0177*
H120.56930.56450.58570.0237*
H130.28410.15910.97190.0152*
H140.42960.15390.83870.0152*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.00654 (16)0.00691 (15)0.00559 (16)0.00138 (12)0.00033 (12)0.00221 (12)
Mo20.00555 (15)0.00549 (14)0.00600 (16)0.00114 (11)0.00026 (12)0.00277 (12)
Mo30.00527 (15)0.00515 (14)0.00550 (16)0.00042 (11)0.00020 (12)0.00228 (12)
Mo40.00656 (15)0.00585 (15)0.00573 (16)0.00130 (11)0.00049 (12)0.00235 (12)
O10.0113 (14)0.0142 (14)0.0098 (15)0.0025 (12)0.0010 (11)0.0061 (12)
O20.0097 (14)0.0123 (14)0.0129 (15)0.0019 (11)0.0043 (12)0.0034 (12)
O30.0090 (13)0.0052 (12)0.0081 (14)0.0019 (10)0.0020 (11)0.0029 (11)
O40.0067 (13)0.0073 (12)0.0067 (13)0.0005 (10)0.0018 (10)0.0035 (11)
O50.0089 (13)0.0074 (13)0.0081 (14)0.0032 (10)0.0007 (11)0.0029 (11)
O60.0098 (14)0.0078 (13)0.0112 (14)0.0005 (11)0.0020 (11)0.0038 (11)
O70.0067 (13)0.0074 (13)0.0094 (14)0.0009 (10)0.0012 (11)0.0027 (11)
O80.0074 (13)0.0053 (12)0.0084 (14)0.0012 (10)0.0004 (11)0.0024 (11)
O90.0065 (13)0.0079 (13)0.0081 (14)0.0007 (10)0.0015 (11)0.0033 (11)
O100.0112 (14)0.0089 (13)0.0093 (14)0.0004 (11)0.0020 (11)0.0018 (11)
O110.0077 (13)0.0062 (12)0.0089 (14)0.0006 (10)0.0000 (11)0.0030 (11)
O120.0097 (14)0.0114 (14)0.0100 (15)0.0006 (11)0.0025 (11)0.0050 (12)
O130.0086 (13)0.0098 (13)0.0114 (14)0.0007 (11)0.0031 (11)0.0047 (11)
N10.035 (2)0.0073 (17)0.026 (2)0.0003 (16)0.0168 (19)0.0055 (16)
N20.021 (2)0.0119 (17)0.017 (2)0.0057 (15)0.0080 (16)0.0096 (15)
N30.023 (2)0.0041 (15)0.025 (2)0.0003 (14)0.0076 (17)0.0044 (15)
N40.0183 (18)0.0092 (16)0.0106 (17)0.0009 (14)0.0025 (14)0.0048 (14)
C10.027 (3)0.017 (2)0.026 (3)0.0049 (19)0.008 (2)0.015 (2)
C20.021 (2)0.016 (2)0.016 (2)0.0004 (18)0.0035 (18)0.0079 (18)
C30.016 (2)0.013 (2)0.014 (2)0.0001 (16)0.0032 (17)0.0060 (17)
C40.024 (2)0.012 (2)0.015 (2)0.0054 (17)0.0004 (18)0.0071 (17)
C50.036 (3)0.013 (2)0.016 (2)0.006 (2)0.005 (2)0.0062 (18)
C60.021 (2)0.013 (2)0.019 (2)0.0029 (17)0.0084 (18)0.0080 (17)
C70.0134 (19)0.0139 (19)0.0093 (19)0.0009 (15)0.0023 (16)0.0046 (16)
C80.0123 (19)0.0107 (18)0.010 (2)0.0004 (15)0.0066 (16)0.0017 (16)
C90.018 (2)0.012 (2)0.014 (2)0.0019 (16)0.0003 (17)0.0044 (17)
C100.016 (2)0.016 (2)0.023 (3)0.0042 (18)0.0001 (19)0.0032 (19)
Geometric parameters (Å, º) top
Mo1—O11.712 (3)N1—H11.000
Mo1—O21.693 (3)N2—C31.327 (6)
Mo1—O31.936 (3)N2—H61.000
Mo1—O42.204 (3)N2—H71.000
Mo1—O51.994 (3)N3—C61.346 (6)
Mo1—O11i2.314 (3)N3—C101.352 (6)
Mo2—O42.261 (3)N3—H81.000
Mo2—O51.886 (3)N4—C81.328 (5)
Mo2—O61.701 (3)N4—H131.000
Mo2—O71.785 (3)N4—H141.000
Mo2—O81.899 (3)C1—C21.357 (6)
Mo2—O9i2.228 (3)C1—H21.007
Mo3—O41.943 (3)C2—C31.419 (6)
Mo3—O4i2.373 (3)C2—H31.008
Mo3—O82.147 (3)C3—C41.415 (6)
Mo3—O91.777 (3)C4—C51.377 (6)
Mo3—O101.696 (3)C4—H41.005
Mo3—O111.875 (3)C5—H51.008
Mo4—O3i1.918 (3)C6—C71.370 (6)
Mo4—O7ii2.029 (3)C6—H91.006
Mo4—O82.187 (3)C7—C81.410 (6)
Mo4—O112.260 (3)C7—H101.005
Mo4—O121.709 (3)C8—C91.421 (6)
Mo4—O131.702 (3)C9—C101.360 (6)
N1—C11.350 (7)C9—H111.007
N1—C51.342 (7)C10—H121.009
O1—Mo1—O2105.34 (15)O3i—Mo4—O1299.38 (13)
O1—Mo1—O3100.73 (14)O7ii—Mo4—O1291.79 (13)
O2—Mo1—O397.73 (13)O8—Mo4—O12159.50 (13)
O1—Mo1—O4159.21 (12)O11—Mo4—O1292.60 (12)
O2—Mo1—O493.04 (13)O3i—Mo4—O1397.18 (13)
O3—Mo1—O486.02 (11)O7ii—Mo4—O13100.72 (13)
O1—Mo1—O593.66 (13)O8—Mo4—O1394.22 (12)
O2—Mo1—O5101.46 (13)O11—Mo4—O13161.91 (13)
O3—Mo1—O5152.00 (12)O12—Mo4—O13105.01 (15)
O1—Mo1—O11i90.09 (12)C1—N1—C5120.9 (4)
O2—Mo1—O11i163.72 (13)C1—N1—H1119.5
O3—Mo1—O11i73.86 (11)C5—N1—H1119.6
O4—Mo1—O572.86 (11)C3—N2—H6119.9
O4—Mo1—O11i72.77 (10)C3—N2—H7120.1
O5—Mo1—O11i82.30 (11)H6—N2—H7120.0
O4—Mo2—O573.46 (11)C6—N3—C10120.9 (4)
O4—Mo2—O6157.19 (12)C6—N3—H8119.6
O5—Mo2—O6103.64 (13)C10—N3—H8119.5
O4—Mo2—O797.84 (12)C8—N4—H13119.9
O5—Mo2—O795.80 (13)C8—N4—H14120.1
O6—Mo2—O7104.97 (14)H13—N4—H14120.0
O4—Mo2—O872.19 (11)N1—C1—C2121.6 (4)
O5—Mo2—O8144.95 (12)N1—C1—H2119.3
O6—Mo2—O8105.26 (13)C2—C1—H2119.1
O4—Mo2—O9i71.68 (10)C1—C2—C3119.7 (5)
O5—Mo2—O9i81.31 (12)C1—C2—H3120.3
O6—Mo2—O9i85.51 (12)C3—C2—H3120.0
O7—Mo2—O895.49 (13)N2—C3—C2122.0 (4)
O7—Mo2—O9i169.51 (12)N2—C3—C4120.7 (4)
O8—Mo2—O9i81.61 (11)C2—C3—C4117.4 (4)
O4—Mo3—O4i75.97 (12)C3—C4—C5119.7 (4)
O4—Mo3—O874.04 (11)C3—C4—H4120.1
O4i—Mo3—O880.42 (10)C5—C4—H4120.3
O4—Mo3—O996.92 (12)N1—C5—C4120.8 (5)
O4i—Mo3—O977.13 (11)N1—C5—H5119.6
O8—Mo3—O9157.27 (12)C4—C5—H5119.6
O4—Mo3—O10102.55 (13)N3—C6—C7121.1 (4)
O4i—Mo3—O10178.50 (12)N3—C6—H9119.3
O8—Mo3—O1099.40 (13)C7—C6—H9119.6
O9—Mo3—O10102.95 (14)C6—C7—C8119.6 (4)
O4—Mo3—O11143.34 (12)C6—C7—H10120.3
O4i—Mo3—O1177.30 (11)C8—C7—H10120.1
O8—Mo3—O1177.15 (12)N4—C8—C7121.3 (4)
O9—Mo3—O11101.09 (13)N4—C8—C9121.1 (4)
O10—Mo3—O11104.13 (13)C7—C8—C9117.6 (4)
O3i—Mo4—O7ii155.67 (12)C8—C9—C10119.7 (4)
O3i—Mo4—O884.91 (11)C8—C9—H11120.0
O7ii—Mo4—O877.50 (11)C10—C9—H11120.3
O3i—Mo4—O1175.47 (11)N3—C10—C9121.1 (5)
O7ii—Mo4—O1182.53 (11)N3—C10—H12119.4
O8—Mo4—O1168.92 (11)C9—C10—H12119.6
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O101.002.042.859 (5)138
N1—H1···O13ii1.002.152.854 (5)126
N2—H6···O1iii1.001.882.861 (5)165
N2—H7···O11iv1.001.952.932 (5)166
N3—H8···O3v1.002.252.934 (5)125
N3—H8···O9v1.002.262.955 (5)125
N4—H13···O12vi1.002.053.004 (5)158
N4—H14···O5i1.001.872.867 (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.
 

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