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In the title compound, (C2H8N)3[Mo12O40P], the Keggin ion [PO40Mo12]3- lies on a special position of site symmetry 3m and the [(CH3)2NH2]+ cation on a special position of site symmetry m.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804027941/tk6195sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804027941/tk6195Isup2.hkl
Contains datablock I

CCDC reference: 258646

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](N-C) = 0.009 Å
  • R factor = 0.027
  • wR factor = 0.069
  • Data-to-parameter ratio = 11.2

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 .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.56 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.58 Ratio PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 44.00 A   3 PLAT731_ALERT_1_C Bond Calc 1.909(4), Rep 1.9100(10) ...... 4.00 su-Rat MO1 -O2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.911(3), Rep 1.9100(10) ...... 3.00 su-Rat MO1 -O2 1.555 4.555 PLAT731_ALERT_1_C Bond Calc 1.926(5), Rep 1.927(2) ...... 2.50 su-Rat MO3 -O8 1.555 2.555 PLAT733_ALERT_1_C Torsion Calc 179.7(3), Rep 179.70(10) ...... 3.00 su-Rat O10 -P1 -O10 -MO2 21.555 1.555 1.555 23.555 PLAT733_ALERT_1_C Torsion Calc -179.7(3), Rep -179.70(10) ...... 3.00 su-Rat O10 -P1 -O10 -MO2 2.555 1.555 1.555 1.555
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.565 Tmax scaled 0.274 Tmin scaled 0.167
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 9 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 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: XSCANS (Bruker, 1994); cell refinement: LEAST SQUARES in XSCANS (Bruker, 1994); data reduction: REDUCE in XSCANS (Bruker, 1994); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

tris(dimethylammonium) dodecamolybdophosphate top
Crystal data top
(C2H8N)3[Mo12O40P]Dx = 3.277 Mg m3
Mr = 1960.53Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3mCell parameters from 34 reflections
Hall symbol: -R 3 2"θ = 5.0–12.9°
a = 16.541 (2) ŵ = 3.81 mm1
c = 25.154 (7) ÅT = 295 K
V = 5960 (2) Å3Block, yellow
Z = 60.52 × 0.34 × 0.34 mm
F(000) = 5520
Data collection top
Siemens P4 four-circle
diffractometer
1150 reflections with I > 2σ(I)
Radiation source: medium-focus sealed tubeRint = 0.037
Graphite monochromatorθmax = 25.0°, θmin = 1.6°
ω scansh = 119
Absorption correction: empirical (using intensity measurements)
via ψ scan (North et al., 1968)
k = 191
Tmin = 0.295, Tmax = 0.484l = 629
3044 measured reflections3 standard reflections every 97 reflections
1304 independent reflections intensity decay: none
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)] = 0.027H-atom parameters constrained
wR(F2) = 0.069 w = 1/[σ2(Fo2) + (0.038P)2 + 0.2473P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
1304 reflectionsΔρmax = 1.35 e Å3
116 parametersΔρmin = 0.91 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00054 (3)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.14951 (4)0.07476 (2)0.15295 (2)0.0182 (2)
Mo20.21887 (3)0.00563 (3)0.26271 (2)0.0187 (2)
Mo30.06896 (2)0.06896 (2)0.38322 (2)0.0178 (2)
P10.00000.00000.26541 (9)0.0102 (5)
O10.1960 (3)0.0980 (2)0.0916 (2)0.027 (1)
O20.0520 (2)0.1041 (3)0.1459 (2)0.020 (1)
O30.2239 (2)0.0319 (2)0.1886 (1)0.020 (1)
O40.1175 (1)0.1175 (1)0.2503 (2)0.020 (1)
O50.2753 (3)0.1377 (1)0.2747 (2)0.022 (1)
O60.3118 (2)0.0095 (2)0.2699 (1)0.026 (1)
O70.1707 (2)0.0126 (2)0.3341 (1)0.022 (1)
O80.0539 (2)0.1077 (3)0.4107 (2)0.020 (1)
O90.1102 (2)0.1102 (2)0.4304 (2)0.028 (1)
O100.1008 (3)0.0504 (1)0.2452 (2)0.014 (1)
O110.00000.00000.3261 (3)0.011 (1)
N10.4930 (2)0.0140 (4)0.2694 (2)0.0230 (1)
C10.5405 (3)0.0809 (5)0.2921 (3)0.038 (2)
C20.4920 (3)0.0159 (5)0.2107 (3)0.040 (2)
H10.43370.04470.28120.044*0.50
H1a0.53840.07700.33020.057*
H1b0.50960.11380.28040.057*
H2a0.46060.07950.19860.060*
H2b0.55500.01550.19760.060*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0185 (3)0.0228 (2)0.0119 (3)0.0092 (2)0.0038 (2)0.0019 (1)
Mo20.0156 (2)0.0221 (2)0.0219 (3)0.0121 (2)0.0005 (1)0.0024 (2)
Mo30.0209 (2)0.0209 (2)0.0144 (3)0.0128 (2)0.0021 (1)0.0021 (1)
P10.0105 (8)0.0105 (8)0.0095 (12)0.0053 (4)0.0000.000
O10.028 (3)0.033 (2)0.017 (2)0.014 (1)0.005 (2)0.003 (1)
O20.019 (2)0.024 (2)0.020 (2)0.012 (1)0.001 (1)0.002 (2)
O30.018 (2)0.026 (2)0.018 (2)0.013 (1)0.003 (1)0.000 (1)
O40.020 (2)0.020 (2)0.023 (2)0.011 (2)0.001 (1)0.001 (1)
O50.015 (2)0.021 (2)0.028 (2)0.008 (1)0.001 (2)0.001 (1)
O60.020 (2)0.031 (2)0.033 (2)0.016 (1)0.002 (1)0.006 (2)
O70.021 (2)0.028 (2)0.017 (1)0.014 (1)0.000 (1)0.003 (1)
O80.022 (2)0.024 (2)0.015 (2)0.012 (1)0.002 (1)0.004 (2)
O90.037 (2)0.037 (2)0.021 (2)0.027 (2)0.002 (1)0.002 (1)
O100.011 (2)0.015 (2)0.015 (2)0.006 (1)0.001 (2)0.001 (1)
O110.011 (2)0.011 (2)0.011 (3)0.006 (1)0.0000.000
N10.038 (3)0.026 (3)0.021 (3)0.013 (2)0.004 (1)0.008 (2)
C10.045 (4)0.025 (4)0.037 (4)0.012 (2)0.001 (2)0.001 (3)
C20.055 (4)0.035 (4)0.023 (4)0.017 (2)0.000 (2)0.000 (3)
Geometric parameters (Å, º) top
Mo1—O11.680 (4)Mo3—O8iv1.927 (2)
Mo1—O21.910 (1)Mo3—O91.676 (4)
Mo1—O2i1.910 (1)Mo3—O112.443 (4)
Mo1—O31.922 (3)P1—O111.525 (7)
Mo1—O3ii1.922 (3)P1—O10iii1.531 (4)
Mo1—O102.423 (4)P1—O101.531 (4)
Mo2—O31.907 (3)P1—O10iv1.531 (4)
Mo2—O41.909 (1)N1—C11.475 (9)
Mo2—O51.922 (2)N1—C21.476 (9)
Mo2—O61.687 (3)N1—H10.90
Mo2—O71.926 (3)C1—H1a0.96
Mo2—O102.450 (3)C1—H1b0.96
Mo3—O71.913 (3)C2—H2a0.96
Mo3—O7iii1.913 (3)C2—H2b0.96
Mo3—O81.927 (2)
O1—Mo1—O2101.8 (2)O8—Mo3—O8iv87.8 (2)
O1—Mo1—O2i101.8 (2)O8—Mo3—O9100.7 (2)
O1—Mo1—O3102.0 (1)O8—Mo3—O1172.9 (1)
O1—Mo1—O3ii102.0 (1)O8iv—Mo3—O9100.7 (2)
O1—Mo1—O10173.4 (2)O8iv—Mo3—O1172.9 (1)
O2—Mo1—O2i85.1 (2)O9—Mo3—O11170.9 (2)
O2—Mo1—O3156.2 (2)O11—P1—O10iii109.4 (2)
O2—Mo1—O3ii89.0 (2)O11—P1—O10109.4 (2)
O2—Mo1—O1083.0 (1)O10iii—P1—O10109.6 (2)
O2i—Mo1—O389.0 (2)O11—P1—O10iv109.4 (2)
O2i—Mo1—O3ii156.2 (2)O10iii—P1—O10iv109.6 (2)
O2i—Mo1—O1083.0 (1)O10—P1—O10iv109.6 (2)
O3—Mo1—O3ii87.2 (2)Mo1iv—O2—Mo1152.4 (2)
O3—Mo1—O1073.3 (1)Mo2—O3—Mo1125.2 (2)
O3ii—Mo1—O1073.3 (1)Mo2—O4—Mo2iii153.2 (2)
O3—Mo2—O489.9 (2)Mo2—O5—Mo2ii126.6 (2)
O3—Mo2—O587.4 (2)Mo3—O7—Mo2150.8 (2)
O3—Mo2—O6101.5 (1)Mo3—O8—Mo3i125.2 (2)
O3—Mo2—O7156.2 (1)P1—O10—Mo1126.1 (2)
O3—Mo2—O1072.9 (1)P1—O10—Mo2ii126.3 (1)
O4—Mo2—O5155.1 (2)Mo1—O10—Mo2ii88.5 (1)
O4—Mo2—O6103.8 (2)P1—O10—Mo2126.3 (1)
O4—Mo2—O785.0 (2)Mo1—O10—Mo288.5 (1)
O4—Mo2—O1083.4 (1)Mo2ii—O10—Mo289.0 (1)
O5—Mo2—O6101.0 (2)P1—O11—Mo3iv126.1 (1)
O5—Mo2—O787.7 (2)P1—O11—Mo3126.1 (1)
O5—Mo2—O1072.1 (1)Mo3iv—O11—Mo388.9 (2)
O6—Mo2—O7102.3 (1)P1—O11—Mo3i126.1 (1)
O6—Mo2—O10171.0 (1)Mo3iv—O11—Mo3i88.9 (2)
O7—Mo2—O1083.4 (1)Mo3—O11—Mo3i88.9 (2)
O7—Mo3—O7iii86.3 (2)C1—N1—C2113.9 (6)
O7—Mo3—O8156.7 (1)C1—N1—H1108.8
O7—Mo3—O8iv88.3 (2)C2—N1—H1108.8
O7—Mo3—O9102.6 (1)N1—C1—H1a109.5
O7—Mo3—O1184.0 (1)N1—C1—H1b109.5
O7iii—Mo3—O888.3 (2)H1a—C1—H1b109.5
O7iii—Mo3—O8iv156.7 (1)N1—C2—H2a109.5
O7iii—Mo3—O9102.6 (1)N1—C2—H2b109.5
O7iii—Mo3—O1184.0 (1)H2a—C2—H2b109.5
O1—Mo1—O2—Mo1iv128.2 (5)O11—P1—O10—Mo2ii60.4 (2)
O2i—Mo1—O2—Mo1iv27.2 (6)O10iii—P1—O10—Mo2ii179.7 (1)
O3ii—Mo1—O2—Mo1iv129.7 (5)O10iv—P1—O10—Mo2ii59.5 (4)
O3—Mo1—O2—Mo1iv49.0 (8)O11—P1—O10—Mo260.4 (2)
O10—Mo1—O2—Mo1iv56.4 (5)O10iii—P1—O10—Mo259.5 (4)
O6—Mo2—O3—Mo1170.4 (2)O10iv—P1—O10—Mo2179.7 (1)
O4—Mo2—O3—Mo185.5 (2)O2i—Mo1—O10—P142.9 (1)
O5—Mo2—O3—Mo169.7 (2)O2—Mo1—O10—P142.9 (1)
O7—Mo2—O3—Mo18.4 (4)O3ii—Mo1—O10—P1134.0 (1)
O10—Mo2—O3—Mo12.3 (2)O3—Mo1—O10—P1134.0 (1)
O1—Mo1—O3—Mo2172.8 (2)O2i—Mo1—O10—Mo2ii178.4 (1)
O2i—Mo1—O3—Mo285.4 (2)O2—Mo1—O10—Mo2ii92.6 (1)
O2—Mo1—O3—Mo210.0 (5)O3ii—Mo1—O10—Mo2ii1.5 (1)
O3ii—Mo1—O3—Mo271.1 (2)O3—Mo1—O10—Mo2ii90.6 (1)
O10—Mo1—O3—Mo22.4 (2)O2i—Mo1—O10—Mo292.6 (1)
O6—Mo2—O4—Mo2iii131.6 (5)O2—Mo1—O10—Mo2178.4 (1)
O3—Mo2—O4—Mo2iii126.6 (5)O3ii—Mo1—O10—Mo290.6 (1)
O5—Mo2—O4—Mo2iii43.2 (8)O3—Mo1—O10—Mo21.5 (1)
O7—Mo2—O4—Mo2iii30.1 (5)O3—Mo2—O10—P1133.8 (3)
O10—Mo2—O4—Mo2iii53.8 (5)O4—Mo2—O10—P142.0 (2)
O6—Mo2—O5—Mo2ii169.7 (3)O5—Mo2—O10—P1133.4 (3)
O3—Mo2—O5—Mo2ii68.5 (3)O7—Mo2—O10—P143.7 (2)
O4—Mo2—O5—Mo2ii15.4 (6)O3—Mo2—O10—Mo11.5 (1)
O7—Mo2—O5—Mo2ii88.2 (3)O4—Mo2—O10—Mo193.4 (1)
O10—Mo2—O5—Mo2ii4.4 (2)O5—Mo2—O10—Mo191.3 (2)
O9—Mo3—O7—Mo2131.1 (3)O7—Mo2—O10—Mo1179.1 (1)
O7iii—Mo3—O7—Mo229.0 (4)O3—Mo2—O10—Mo2ii90.0 (1)
O8—Mo3—O7—Mo247.8 (6)O4—Mo2—O10—Mo2ii178.1 (2)
O8iv—Mo3—O7—Mo2128.3 (4)O5—Mo2—O10—Mo2ii2.8 (2)
O11—Mo3—O7—Mo255.3 (3)O7—Mo2—O10—Mo2ii92.4 (1)
O6—Mo2—O7—Mo3131.7 (3)O7iii—Mo3—O11—P143.43 (9)
O3—Mo2—O7—Mo349.4 (5)O7—Mo3—O11—P143.43 (9)
O4—Mo2—O7—Mo328.6 (4)O8—Mo3—O11—P1133.5 (1)
O5—Mo2—O7—Mo3127.5 (4)O8iv—Mo3—O11—P1133.5 (1)
O10—Mo2—O7—Mo355.3 (3)O7iii—Mo3—O11—Mo3iv179.0 (1)
O9—Mo3—O8—Mo3i170.1 (2)O7—Mo3—O11—Mo3iv92.1 (1)
O7iii—Mo3—O8—Mo3i87.4 (3)O8—Mo3—O11—Mo3iv91.0 (2)
O7—Mo3—O8—Mo3i10.9 (6)O8iv—Mo3—O11—Mo3iv2.1 (1)
O8iv—Mo3—O8—Mo3i69.6 (3)O7iii—Mo3—O11—Mo3i92.1 (1)
O11—Mo3—O8—Mo3i3.2 (2)O7—Mo3—O11—Mo3i179.0 (1)
O10iii—P1—O10—Mo160.1 (2)O8—Mo3—O11—Mo3i2.1 (1)
O10iv—P1—O10—Mo160.1 (2)O8iv—Mo3—O11—Mo3i91.0 (2)
Symmetry codes: (i) x+y, x, z; (ii) x, xy, z; (iii) y, x, z; (iv) y, xy, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O60.902.383.035 (3)130
N1—H1···O7v0.902.313.112 (5)149
Symmetry code: (v) y+1/3, x1/3, z+2/3.
 

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