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The crystal structure of (C4H14N2)2[H2V10O28] symmetry lying on a centre of symmetry, and two butane-1,4-diammonium cations per anion for charge compensation. The anion is protonated on centrosymmetrically related μ-OV3 groups; this is a less common protonation mode for dihydrogendeca­vanadates. Anions are involved in a two-dimensional hydrogen-bonding network, forming a layered structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806026249/hk2073sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806026249/hk2073Isup2.hkl
Contains datablock I

CCDC reference: 618233

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.021
  • wR factor = 0.056
  • Data-to-parameter ratio = 19.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.46 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997); cell refinement: COLLECT and DENZO; data reduction: COLLECT and DENZO; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: publCIF (Westrip, 2006).

1,4-butanediamminium dihydrogendecavanadate top
Crystal data top
(C4H14N2)2H2V10O28F(000) = 2240
Mr = 1139.76Dx = 2.429 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2abCell parameters from 32381 reflections
a = 10.2268 (1) Åθ = 1.0–30.0°
b = 16.7196 (2) ŵ = 2.96 mm1
c = 18.2311 (2) ÅT = 150 K
V = 3117.30 (6) Å3Prism, yellow
Z = 40.30 × 0.28 × 0.10 mm
Data collection top
Enraf-Nonius KappaCCD κ-axis
diffractometer
4555 independent reflections
Radiation source: fine-focus sealed tube4375 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.092
Detector resolution: 9.091 pixels mm-1θmax = 30.0°, θmin = 3.2°
ω–scans to fill Ewald sphereh = 014
Absorption correction: analytical
PLATON (Spek, 2003), analytical numeric absorption correction using a multifaceted crystal model based on de Meulenaer Tompa (1965).
k = 023
Tmin = 0.423, Tmax = 0.742l = 025
59189 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.056 w = 1/[σ2(Fo2) + (0.018P)2 + 3.0702P]
where P = (Fo2 + 2Fc2)/3
S = 1.23(Δ/σ)max = 0.001
4555 reflectionsΔρmax = 0.39 e Å3
232 parametersΔρmin = 0.37 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00128 (13)
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.48514 (14)0.35583 (8)0.18008 (7)0.0142 (3)
H1A0.41000.36140.15390.021*
H1B0.55400.37280.15260.021*
H1C0.48000.38560.22180.021*
C20.50390 (16)0.26993 (10)0.19972 (9)0.0157 (3)
H2A0.58810.26330.22580.019*
H2B0.50690.23720.15450.019*
C30.39266 (15)0.24128 (9)0.24837 (9)0.0139 (3)
H3A0.30850.25220.22340.017*
H3B0.39370.27220.29470.017*
C40.40069 (17)0.15207 (10)0.26649 (9)0.0169 (3)
H4A0.31950.13660.29240.020*
H4B0.40320.12180.21980.020*
C50.51665 (18)0.12628 (10)0.31295 (10)0.0192 (3)
H5A0.53100.06810.30680.023*
H5B0.59620.15440.29590.023*
N60.49438 (13)0.14448 (8)0.39232 (8)0.0135 (3)
H6A0.47860.19770.39790.020*
H6B0.56660.13070.41860.020*
H6C0.42440.11610.40880.020*
V10.31278 (2)0.334615 (15)0.461549 (14)0.01013 (6)
V20.30078 (3)0.473143 (15)0.350252 (14)0.01023 (7)
V30.56972 (2)0.396026 (15)0.388983 (14)0.00908 (6)
V40.50658 (2)0.568692 (14)0.436648 (13)0.00785 (6)
V50.77021 (2)0.494385 (16)0.487300 (14)0.00965 (6)
O10.19362 (10)0.40246 (7)0.51538 (6)0.0122 (2)
O20.58476 (11)0.65697 (7)0.44252 (6)0.0115 (2)
O30.24626 (12)0.24798 (7)0.47064 (7)0.0174 (2)
O40.24288 (11)0.37318 (6)0.37677 (6)0.0117 (2)
O50.46855 (11)0.30955 (6)0.41925 (6)0.0109 (2)
O60.23025 (12)0.48715 (7)0.27361 (7)0.0182 (2)
O70.46435 (11)0.42647 (6)0.31780 (6)0.0113 (2)
O80.64380 (10)0.39533 (6)0.49615 (6)0.0089 (2)
O90.41364 (11)0.57258 (6)0.36031 (6)0.0113 (2)
O100.41753 (10)0.45880 (6)0.46008 (6)0.00841 (19)
O110.69027 (11)0.35162 (7)0.34986 (7)0.0159 (2)
O120.64297 (10)0.50302 (6)0.40476 (6)0.0097 (2)
O130.80903 (10)0.47667 (7)0.58406 (6)0.0119 (2)
O140.88803 (11)0.45033 (8)0.44546 (7)0.0176 (2)
H80.678 (2)0.3527 (16)0.5083 (13)0.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0154 (6)0.0160 (6)0.0113 (6)0.0022 (5)0.0005 (5)0.0012 (5)
C20.0156 (7)0.0143 (7)0.0170 (7)0.0007 (6)0.0031 (6)0.0008 (6)
C30.0130 (7)0.0155 (7)0.0131 (7)0.0007 (6)0.0010 (5)0.0025 (6)
C40.0217 (8)0.0148 (7)0.0141 (7)0.0026 (6)0.0000 (6)0.0001 (6)
C50.0216 (8)0.0165 (8)0.0196 (8)0.0067 (6)0.0066 (6)0.0027 (6)
N60.0120 (6)0.0112 (6)0.0171 (6)0.0002 (5)0.0026 (5)0.0018 (5)
V10.01050 (12)0.00739 (12)0.01248 (13)0.00232 (9)0.00018 (9)0.00007 (9)
V20.01091 (12)0.00934 (12)0.01043 (12)0.00056 (9)0.00260 (9)0.00061 (9)
V30.00880 (12)0.00900 (12)0.00943 (12)0.00056 (8)0.00059 (8)0.00173 (9)
V40.00894 (11)0.00665 (12)0.00797 (12)0.00034 (8)0.00014 (8)0.00110 (8)
V50.00670 (12)0.01013 (12)0.01211 (13)0.00021 (9)0.00073 (9)0.00139 (9)
O10.0093 (5)0.0124 (5)0.0148 (5)0.0024 (4)0.0019 (4)0.0011 (4)
O20.0136 (5)0.0096 (5)0.0115 (5)0.0015 (4)0.0002 (4)0.0018 (4)
O30.0193 (6)0.0116 (5)0.0214 (6)0.0053 (5)0.0006 (5)0.0012 (5)
O40.0106 (5)0.0107 (5)0.0139 (5)0.0008 (4)0.0021 (4)0.0012 (4)
O50.0121 (5)0.0078 (5)0.0129 (5)0.0000 (4)0.0011 (4)0.0010 (4)
O60.0225 (6)0.0164 (6)0.0156 (6)0.0025 (5)0.0074 (5)0.0018 (4)
O70.0130 (5)0.0108 (5)0.0101 (5)0.0002 (4)0.0005 (4)0.0010 (4)
O80.0088 (5)0.0067 (5)0.0111 (5)0.0015 (4)0.0006 (4)0.0002 (4)
O90.0138 (5)0.0095 (5)0.0107 (5)0.0001 (4)0.0008 (4)0.0015 (4)
O100.0084 (4)0.0077 (5)0.0092 (5)0.0005 (4)0.0003 (4)0.0004 (4)
O110.0141 (5)0.0162 (5)0.0175 (6)0.0028 (4)0.0025 (4)0.0044 (5)
O120.0097 (5)0.0101 (5)0.0093 (5)0.0009 (4)0.0014 (4)0.0001 (4)
O130.0096 (5)0.0115 (5)0.0147 (5)0.0022 (4)0.0025 (4)0.0010 (4)
O140.0104 (5)0.0209 (6)0.0216 (6)0.0016 (4)0.0016 (4)0.0060 (5)
Geometric parameters (Å, º) top
O8—V32.0956 (11)V1—V33.1159 (4)
O8—V4i2.0562 (11)V2—O61.5897 (12)
O8—V52.1072 (11)V2—O41.8379 (11)
O12—V31.9607 (11)V2—O13i1.8438 (11)
O12—V41.8679 (11)V2—O71.9384 (11)
O12—V51.9946 (11)V2—O92.0322 (11)
N1—C21.493 (2)V2—O102.3435 (11)
N1—H1A0.9100V2—V43.0761 (4)
N1—H1B0.9100V2—V5i3.0973 (4)
N1—H1C0.9100V2—V33.1185 (4)
C2—C31.520 (2)V3—O111.6062 (12)
C2—H2A0.9900V3—O71.7619 (11)
C2—H2B0.9900V3—O51.8615 (11)
C3—C41.530 (2)V3—O102.2812 (11)
C3—H3A0.9900V3—V43.0832 (4)
C3—H3B0.9900V4—O21.6819 (11)
C4—C51.520 (2)V4—O91.6866 (11)
C4—H4A0.9900V4—O10i2.0877 (11)
C4—H4B0.9900V4—O102.0947 (11)
C5—N61.496 (2)V4—V1i3.0775 (4)
C5—H5A0.9900V4—V53.1089 (4)
C5—H5B0.9900V5—O141.6050 (12)
N6—H6A0.9100V5—O1i1.7645 (12)
N6—H6B0.9100V5—O131.8323 (12)
N6—H6C0.9100V5—O10i2.2846 (11)
V1—O31.6088 (12)V5—V2i3.0973 (4)
V1—O51.8189 (11)O1—V5i1.7645 (11)
V1—O41.8209 (11)O2—V1i2.0437 (11)
V1—O11.9326 (11)O8—V4i2.0562 (11)
V1—O2i2.0437 (11)O8—H80.82 (3)
V1—O102.3365 (11)O10—V4i2.0877 (11)
V1—V4i3.0775 (4)O10—V5i2.2846 (11)
V1—V23.0817 (4)O13—V2i1.8438 (11)
C2—N1—H1A109.5O5—V3—O1079.03 (4)
C2—N1—H1B109.5O12—V3—O1075.97 (4)
H1A—N1—H1B109.5O8—V3—O1073.71 (4)
C2—N1—H1C109.5O11—V3—V4135.95 (5)
H1A—N1—H1C109.5O7—V3—V478.99 (4)
H1B—N1—H1C109.5O5—V3—V4121.82 (4)
N1—C2—C3110.30 (13)O12—V3—V435.35 (3)
N1—C2—H2A109.6O8—V3—V479.52 (3)
C3—C2—H2A109.6O10—V3—V442.79 (3)
N1—C2—H2B109.6O11—V3—V1133.12 (5)
C3—C2—H2B109.6O7—V3—V183.81 (4)
H2A—C2—H2B108.1O5—V3—V131.74 (3)
C2—C3—C4113.14 (14)O12—V3—V1124.09 (3)
C2—C3—H3A109.0O8—V3—V184.68 (3)
C4—C3—H3A109.0O10—V3—V148.32 (3)
C2—C3—H3B109.0V4—V3—V190.704 (9)
C4—C3—H3B109.0O11—V3—V2140.13 (5)
H3A—C3—H3B107.8O7—V3—V234.35 (4)
C5—C4—C3116.04 (14)O5—V3—V284.15 (3)
C5—C4—H4A108.3O12—V3—V289.60 (3)
C3—C4—H4A108.3O8—V3—V2122.16 (3)
C5—C4—H4B108.3O10—V3—V248.45 (3)
C3—C4—H4B108.3V4—V3—V259.470 (8)
H4A—C4—H4B107.4V1—V3—V259.247 (8)
N6—C5—C4111.25 (13)O2—V4—O9106.65 (5)
N6—C5—H5A109.4O2—V4—O12100.41 (5)
C4—C5—H5A109.4O9—V4—O12100.76 (5)
N6—C5—H5B109.4O2—V4—O8i93.49 (5)
C4—C5—H5B109.4O9—V4—O8i93.37 (5)
H5A—C5—H5B108.0O12—V4—O8i156.33 (5)
C5—N6—H6A109.5O2—V4—O10i87.66 (5)
C5—N6—H6B109.5O9—V4—O10i164.19 (5)
H6A—N6—H6B109.5O12—V4—O10i82.74 (4)
C5—N6—H6C109.5O8i—V4—O10i78.76 (4)
H6A—N6—H6C109.5O2—V4—O10164.45 (5)
H6B—N6—H6C109.5O9—V4—O1087.54 (5)
O3—V1—O5101.92 (6)O12—V4—O1082.68 (4)
O3—V1—O4103.90 (6)O8i—V4—O1079.04 (4)
O5—V1—O493.76 (5)O10i—V4—O1077.56 (5)
O3—V1—O1102.10 (6)O2—V4—V2144.44 (4)
O5—V1—O1154.53 (5)O9—V4—V238.00 (4)
O4—V1—O188.61 (5)O12—V4—V292.65 (3)
O3—V1—O2i100.99 (6)O8i—V4—V286.86 (3)
O5—V1—O2i85.97 (5)O10i—V4—V2127.00 (3)
O4—V1—O2i154.60 (5)O10—V4—V249.57 (3)
O1—V1—O2i81.27 (5)O2—V4—V1i38.31 (4)
O3—V1—O10174.33 (5)O9—V4—V1i144.65 (4)
O5—V1—O1078.36 (4)O12—V4—V1i92.76 (3)
O4—V1—O1081.70 (4)O8i—V4—V1i86.33 (3)
O1—V1—O1076.90 (4)O10i—V4—V1i49.35 (3)
O2i—V1—O1073.35 (4)O10—V4—V1i126.78 (3)
O3—V1—V4i131.66 (5)V2—V4—V1i172.893 (11)
O5—V1—V4i81.43 (4)O2—V4—V3137.73 (4)
O4—V1—V4i124.16 (4)O9—V4—V385.50 (4)
O1—V1—V4i76.34 (3)O12—V4—V337.39 (3)
O2i—V1—V4i30.68 (3)O8i—V4—V3126.76 (3)
O10—V1—V4i42.68 (3)O10i—V4—V388.29 (3)
O3—V1—V2136.69 (5)O10—V4—V347.72 (3)
O5—V1—V285.92 (4)V2—V4—V360.836 (8)
O4—V1—V232.79 (3)V1i—V4—V3122.422 (10)
O1—V1—V282.42 (4)O2—V4—V585.39 (4)
O2i—V1—V2122.15 (3)O9—V4—V5138.53 (4)
O10—V1—V248.91 (3)O12—V4—V537.81 (3)
V4i—V1—V291.500 (9)O8i—V4—V5126.05 (3)
O3—V1—V3134.18 (5)O10i—V4—V547.29 (3)
O5—V1—V332.57 (3)O10—V4—V588.05 (3)
O4—V1—V381.60 (4)V2—V4—V5122.541 (10)
O1—V1—V3123.64 (3)V1i—V4—V560.674 (8)
O2i—V1—V384.74 (3)V3—V4—V561.832 (8)
O10—V1—V346.82 (3)O14—V5—O1i106.14 (6)
V4i—V1—V364.960 (8)O14—V5—O13102.75 (6)
V2—V1—V360.419 (8)O1i—V5—O1398.01 (5)
O6—V2—O4102.65 (6)O14—V5—O1299.47 (6)
O6—V2—O13i103.15 (6)O1i—V5—O1292.58 (5)
O4—V2—O13i92.68 (5)O13—V5—O12151.56 (5)
O6—V2—O7100.52 (6)O14—V5—O897.83 (5)
O4—V2—O789.55 (5)O1i—V5—O8154.02 (5)
O13i—V2—O7155.11 (5)O13—V5—O886.11 (5)
O6—V2—O9102.50 (6)O12—V5—O873.41 (4)
O4—V2—O9154.59 (5)O14—V5—O10i171.00 (5)
O13i—V2—O985.12 (5)O1i—V5—O10i81.54 (4)
O7—V2—O982.35 (5)O13—V5—O10i80.40 (4)
O6—V2—O10175.66 (6)O12—V5—O10i75.15 (4)
O4—V2—O1081.16 (4)O8—V5—O10i73.83 (4)
O13i—V2—O1078.58 (4)O14—V5—V2i135.30 (5)
O7—V2—O1077.29 (4)O1i—V5—V2i84.51 (4)
O9—V2—O1073.58 (4)O13—V5—V2i32.70 (3)
O6—V2—V4133.15 (5)O12—V5—V2i123.76 (3)
O4—V2—V4123.92 (4)O8—V5—V2i85.45 (3)
O13i—V2—V481.24 (4)O10i—V5—V2i48.81 (3)
O7—V2—V476.99 (3)O14—V5—V4133.89 (5)
O9—V2—V430.72 (3)O1i—V5—V477.46 (4)
O10—V2—V442.87 (3)O13—V5—V4122.58 (4)
O6—V2—V1135.03 (5)O12—V5—V435.04 (3)
O4—V2—V132.45 (3)O8—V5—V478.74 (3)
O13i—V2—V186.48 (4)O10i—V5—V442.18 (3)
O7—V2—V182.19 (3)V2i—V5—V490.612 (9)
O9—V2—V1122.20 (3)V5i—O1—V1115.31 (6)
O10—V2—V148.72 (3)V4—O2—V1i111.01 (6)
V4—V2—V191.486 (9)V1—O4—V2114.76 (6)
O6—V2—V5i135.09 (5)V1—O5—V3115.69 (6)
O4—V2—V5i80.35 (4)V3—O7—V2114.79 (6)
O13i—V2—V5i32.47 (3)V4i—O8—V3106.47 (5)
O7—V2—V5i124.38 (3)V4i—O8—V5105.94 (5)
O9—V2—V5i84.46 (3)V3—O8—V598.40 (5)
O10—V2—V5i47.19 (3)V4i—O8—H8114.0 (17)
V4—V2—V5i65.149 (8)V3—O8—H8114.0 (17)
V1—V2—V5i60.756 (8)V5—O8—H8116.4 (17)
O6—V2—V3131.31 (5)V4—O9—V2111.28 (6)
O4—V2—V381.29 (4)V4i—O10—V4102.44 (5)
O13i—V2—V3125.33 (4)V4i—O10—V399.06 (4)
O7—V2—V330.86 (3)V4—O10—V389.49 (4)
O9—V2—V379.45 (3)V4i—O10—V5i90.52 (4)
O10—V2—V346.76 (3)V4—O10—V5i98.66 (4)
V4—V2—V359.694 (8)V3—O10—V5i165.84 (5)
V1—V2—V360.334 (8)V4i—O10—V187.96 (4)
V5i—V2—V393.595 (9)V4—O10—V1168.85 (5)
O11—V3—O7106.02 (6)V3—O10—V184.86 (4)
O11—V3—O5101.49 (6)V5i—O10—V185.08 (4)
O7—V3—O595.90 (5)V4i—O10—V2169.25 (5)
O11—V3—O12101.17 (6)V4—O10—V287.57 (4)
O7—V3—O1294.48 (5)V3—O10—V284.79 (4)
O5—V3—O12151.34 (5)V5i—O10—V284.00 (4)
O11—V3—O897.70 (5)V1—O10—V282.37 (3)
O7—V3—O8155.43 (5)V4—O12—V3107.26 (5)
O5—V3—O885.43 (5)V4—O12—V5107.16 (5)
O12—V3—O874.34 (4)V3—O12—V5107.09 (5)
O11—V3—O10171.36 (5)V5—O13—V2i114.82 (6)
O7—V3—O1082.44 (5)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8···O3ii0.82 (3)1.86 (3)2.6844 (16)175 (3)
N1—H1A···O11iii0.912.253.0655 (18)148
N1—H1A···O14iii0.912.352.9531 (18)123
N1—H1B···O4iv0.912.002.8471 (18)153
N1—H1C···O70.911.892.7829 (17)168
N6—H6A···O50.911.912.8158 (17)171
N6—H6B···O1ii0.911.862.7567 (17)170
N6—H6C···O13v0.911.952.8074 (17)156
C2—H2B···O2vi0.992.413.334 (2)155
C3—H3A···O11iii0.992.453.3007 (19)143
C3—H3B···O50.992.483.407 (2)157
C4—H4A···O6vii0.992.573.068 (2)111
C4—H4B···O9vi0.992.513.274 (2)133
Symmetry codes: (ii) x+1/2, y+1/2, z+1; (iii) x1/2, y, z+1/2; (iv) x+1/2, y, z+1/2; (v) x1/2, y+1/2, z+1; (vi) x+1, y1/2, z+1/2; (vii) x+1/2, y1/2, z.
 

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