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The dications and tetraanion in the title compound, (C6H16N2)2[Mo5O15(HPO4)2]·2H2O, occupy special positions in the crystal structure. One of the independent cations lies on a site of \overline 1 symmetry and the other lies on a site of 2 symmetry. The tetraanion, which has 2 site symmetry, consists of a five-unit ring of vertex/edge-sharing MoO6 octahedra; the ring is capped by two P(OH) units on opposite sides. The anions are linked via hydrogen bonds involving the H atom of the hydrogenphosphate group into a zigzag chain running along the c axis. The chains are incorporated into the network structure through hydrogen bonds involving the cations and lattice water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680400011X/ya6186sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680400011X/ya6186Isup2.hkl
Contains datablock I

CCDC reference: 234798

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • R factor = 0.034
  • wR factor = 0.095
  • Data-to-parameter ratio = 15.5

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT391_ALERT_3_A Deviating Methyl C3 H-C-H Bond Angle ...... 125.10 Deg.
Author Response: The cation on the two-fold axis is disordered. The treatment of the disorder is described. The angle is an artifact of the disorder.
PLAT391_ALERT_3_A Deviating Methyl C3      H-C-H Bond Angle ......      88.24 Deg.
Author Response: The cation on the two-fold axis is disordered. The treatment of the disorder is described. The angle is an artifact of the disorder.

Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O1W - H1W2 ... ?
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.438 0.662 Tmin' and Tmax expected: 0.509 0.662 RR' = 0.862 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.84 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 26.00 Perc. PLAT432_ALERT_2_C Short Inter X...Y Contact O6 .. C1' = 2.99 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 H2 O
2 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 7 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 4 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); 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.

Bis(3,5-dimethylpiperazinium) di-µ5-hydrogenphosphato-penta-µ2-oxo-pentakis[dioxomolybdenum(III)] dihydrate top
Crystal data top
(C6H16N2)2[Mo5O15(HPO4)2]·2H2OF(000) = 2312
Mr = 1180.10Dx = 2.395 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 6915 reflections
a = 10.8677 (5) Åθ = 2.4–27.0°
b = 21.960 (1) ŵ = 2.06 mm1
c = 13.7160 (6) ÅT = 298 K
β = 90.715 (1)°Prism, colorless
V = 3273.1 (3) Å30.32 × 0.26 × 0.20 mm
Z = 4
Data collection top
Bruker APEX area-detector
diffractometer
3538 independent reflections
Radiation source: fine-focus sealed tube3017 reflections with I > 2σ(I)'
Graphite monochromatorRint = 0.049
φ and ω scansθmax = 27.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1013
Tmin = 0.438, Tmax = 0.662k = 2527
9212 measured reflectionsl = 1716
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0473P)2]
where P = (Fo2 + 2Fc2)/3
3538 reflections(Δ/σ)max = 0.001
228 parametersΔρmax = 0.88 e Å3
13 restraintsΔρmin = 1.01 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.00000.69434 (2)0.25000.0209 (2)
Mo20.25271 (4)0.60436 (2)0.28370 (3)0.0220 (1)
Mo30.16853 (4)0.45807 (2)0.25107 (3)0.0181 (1)
P10.0189 (1)0.56061 (5)0.11368 (8)0.0168 (2)
O10.0185 (3)0.5845 (1)0.0104 (2)0.026 (1)
O20.0969 (3)0.5035 (1)0.1077 (2)0.019 (1)
O30.0887 (3)0.6129 (1)0.1621 (2)0.020 (1)
O40.0638 (4)0.7418 (2)0.3313 (3)0.039 (1)
O50.1435 (3)0.6676 (1)0.3201 (2)0.024 (1)
O60.3464 (3)0.6420 (2)0.2053 (3)0.038 (1)
O70.3357 (4)0.5994 (2)0.3895 (3)0.039 (1)
O80.2839 (3)0.5228 (1)0.2328 (3)0.025 (1)
O90.0988 (3)0.5447 (1)0.3311 (2)0.019 (1)
O100.00000.4329 (2)0.25000.020 (1)
O110.2317 (3)0.4072 (2)0.1714 (3)0.029 (1)
O120.2089 (3)0.4293 (2)0.3617 (3)0.030 (1)
O1W0.1881 (5)0.6924 (2)0.5060 (4)0.070 (2)
N10.0531 (8)0.6931 (4)0.8374 (6)0.038 (2)0.50
N1'0.0540 (8)0.7419 (4)0.6659 (6)0.038 (2)0.50
N20.3973 (4)0.5228 (2)0.5527 (3)0.037 (1)
C10.1339 (8)0.7127 (9)0.7549 (7)0.039 (3)0.50
C1'0.1309 (8)0.725 (1)0.7494 (7)0.039 (3)0.50
C20.0645 (8)0.7073 (5)0.6601 (6)0.040 (3)0.50
C2'0.0577 (9)0.7339 (5)0.8411 (6)0.040 (3)0.50
C30.1332 (7)0.7236 (3)0.5676 (5)0.053 (2)
C40.4025 (5)0.4577 (2)0.5229 (4)0.032 (1)
C50.4785 (5)0.4501 (2)0.4285 (4)0.030 (1)
C60.4890 (6)0.3839 (3)0.4037 (6)0.057 (2)
H10.03230.55560.02590.038*
H1w10.15430.70600.45360.084*
H1w20.24080.66560.48650.084*
H1n10.02910.65430.82840.046*0.50
H1n20.09530.69540.89410.046*0.50
H1n30.03680.78190.66940.046*0.50
H1n40.09760.73560.61060.046*0.50
H1a0.15990.75450.76470.047*0.50
H1b0.20680.68720.75340.047*0.50
H1'10.15690.68320.74360.047*0.50
H1'20.20370.75080.75050.047*0.50
H20.04180.66430.65370.048*0.50
H2'0.02840.77610.84230.048*0.50
H2n10.35230.52590.60710.044*
H2n20.35900.54420.50540.044*
H3a0.20840.70080.56510.079*
H3b0.15160.76630.56760.079*
H3c0.08290.71390.51170.079*
H4a0.31970.44250.51170.038*
H4b0.43990.43380.57490.038*
H50.43770.47180.37470.036*
H6a0.53660.37930.34570.085*
H6b0.40830.36720.39300.085*
H6c0.52880.36270.45660.085*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0237 (3)0.0152 (3)0.0238 (3)0.0000.0039 (2)0.000
Mo20.0182 (2)0.0176 (2)0.0299 (3)0.0024 (2)0.0041 (2)0.0011 (2)
Mo30.0158 (2)0.0161 (2)0.0225 (2)0.0014 (2)0.0011 (2)0.0009 (2)
P10.0220 (6)0.0159 (6)0.0125 (6)0.0011 (5)0.0013 (4)0.0004 (4)
O10.041 (2)0.018 (2)0.018 (2)0.001 (2)0.006 (2)0.001 (1)
O20.024 (2)0.019 (2)0.014 (2)0.002 (1)0.000 (1)0.001 (1)
O30.024 (2)0.018 (2)0.020 (2)0.004 (1)0.000 (1)0.000 (1)
O40.038 (2)0.027 (2)0.051 (3)0.007 (2)0.001 (2)0.011 (2)
O50.025 (2)0.019 (2)0.027 (2)0.001 (1)0.008 (1)0.008 (1)
O60.032 (2)0.027 (2)0.055 (3)0.008 (2)0.011 (2)0.004 (2)
O70.036 (2)0.036 (2)0.044 (2)0.003 (2)0.020 (2)0.007 (2)
O80.013 (2)0.021 (2)0.040 (2)0.000 (1)0.001 (1)0.00192)
O90.021 (2)0.018 (2)0.018 (2)0.001 (1)0.000 (1)0.000 (1)
O100.016 (2)0.016 (2)0.029 (3)0.0000.000 (2)0.000
O110.026 (2)0.023 (2)0.039 (2)0.005 (2)0.007 (2)0.003 (2)
O120.031 (2)0.032 (2)0.028 (2)0.002 (2)0.009 (2)0.009 (2)
O1w0.069 (3)0.090 (4)0.049 (3)0.001 (3)0.013 (3)0.021 (3)
N10.051 (4)0.022 (3)0.043 (4)0.002 (3)0.004 (3)0.001 (3)
N1'0.051 (4)0.022 (3)0.043 (4)0.002 (3)0.004 (3)0.001 (3)
N20.018 (2)0.056 (3)0.036 (3)0.003 (2)0.003 (2)0.015 (2)
C10.039 (4)0.046 (8)0.033 (4)0.004 (6)0.010 (3)0.006 (6)
C1'0.039 (4)0.046 (8)0.033 (4)0.004 (6)0.010 (3)0.006 (6)
C20.042 (4)0.025 (8)0.053 (5)0.004 (3)0.018 (4)0.003 (3)
C2'0.042 (4)0.025 (8)0.053 (5)0.004 (3)0.018 (4)0.003 (3)
C30.061 (4)0.048 (4)0.049 (4)0.004 (3)0.027 (3)0.004 (3)
C40.022 (3)0.036 (3)0.038 (3)0.005 (2)0.000 (2)0.004 (2)
C50.021 (3)0.041 (3)0.029 (3)0.001 (2)0.003 (2)0.008 (2)
C60.038 (4)0.053 (4)0.079 (5)0.004 (3)0.009 (3)0.033 (4)
Geometric parameters (Å, º) top
Mo1—O32.369 (3)N2—C41.488 (7)
Mo1—O3i2.369 (3)N2—C5iii1.495 (6)
Mo1—O41.683 (4)C4—C51.553 (7)
Mo1—O4i1.683 (4)C5—N2iii1.495 (6)
Mo1—O51.914 (3)C5—C61.500 (8)
Mo1—O5i1.914 (3)O1—H10.82
Mo2—O32.433 (3)O1w—H1w10.86
Mo2—O51.897 (3)O1w—H1w20.86
Mo2—O61.704 (4)N1—H1n10.90
Mo2—O71.703 (4)N1—H1n20.90
Mo2—O81.953 (3)N1'—H1n30.90
Mo2—O92.228 (3)N1'—H1n40.90
Mo3—O22.331 (3)C1—H1a0.97
Mo3—O81.914 (3)C1—H1b0.97
Mo3—O92.328 (3)C1'—H1'10.97
Mo3—O101.913 (1)C1'—H1'20.97
Mo3—O111.713 (3)C2—H20.98
Mo3—O121.697 (3)C2'—H2'0.98
P1—O21.516 (3)N2—H2n10.90
P1—O31.524 (3)N2—H2n20.90
P1—O9i1.534 (3)C3—H3a0.96
P1—O11.560 (3)C3—H3b0.96
N1—C11.503 (9)C3—H3c0.96
N1—C2'1.501 (8)C4—H4a0.97
N1'—C1'1.471 (9)C4—H4b0.97
N1'—C21.499 (8)C5—H50.98
C1—C21.500 (9)C6—H6a0.96
C1'—C2'1.491 (9)C6—H6b0.96
C2—C31.523 (7)C6—H6c0.96
C2'—C3ii1.52 (1)
O3—Mo1—O3i81.9 (2)N1'—C2—C1109.7 (7)
O3—Mo1—O4168.2 (2)N1'—C2—C3110.8 (7)
O3—Mo1—O4i87.5 (2)C1—C2—C3117.3 (8)
O3—Mo1—O571.9 (1)C1'—C2'—N1108.4 (7)
O3—Mo1—O5i81.2 (1)C1'—C2'—C3ii112.8 (8)
O3i—Mo1—O487.5 (2)N1—C2'—C3ii112.3 (7)
O3i—Mo1—O4i168.2 (2)C4—N2—C5iii113.1 (4)
O3i—Mo1—O581.2 (1)N2—C4—C5110.7 (4)
O3i—Mo1—O5i71.9 (1)N2iii—C5—C6110.8 (4)
O4—Mo1—O4i103.4 (3)N2iii—C5—C4107.6 (4)
O4—Mo1—O5101.4 (2)C6—C5—C4109.6 (5)
O4—Mo1—O5i100.6 (2)P1—O1—H1109.5
O4i—Mo1—O5100.6 (2)H1w1—O1w—H1w2105.4
O4i—Mo1—O5i101.4 (2)C2'—N1—H1n1109.8
O5—Mo1—O5i144.2 (2)C1—N1—H1n1109.8
O3—Mo2—O887.4 (1)C2'—N1—H1n2109.8
O3—Mo2—O972.5 (1)C1—N1—H1n2109.8
O3—Mo2—O570.7 (1)H1n1—N1—H1n2108.2
O3—Mo2—O688.2 (2)C1'—N1'—H1n3108.7
O3—Mo2—O7164.8 (2)C2—N1'—H1n3108.7
O5—Mo2—O6101.1 (2)C1'—N1'—H1n4108.7
O5—Mo2—O798.6 (2)C2—N1'—H1n4108.7
O5—Mo2—O8151.3 (1)H1n3—N1'—H1n4107.6
O5—Mo2—O983.1 (1)C2—C1—H1a109.7
O6—Mo2—O7104.7 (2)N1—C1—H1a109.7
O6—Mo2—O896.4 (2)C2—C1—H1b109.7
O6—Mo2—O9157.9 (2)N1—C1—H1b109.7
O7—Mo2—O898.8 (2)H1a—C1—H1b108.2
O7—Mo2—O996.0 (2)N1'—C1'—H1'1109.9
O8—Mo2—O972.5 (1)C2'—C1'—H1'1109.9
O2—Mo3—O877.5 (1)N1'—C1'—H1'2109.9
O2—Mo3—O986.6 (1)C2'—C1'—H1'2109.9
O2—Mo3—O1078.9 (1)H1'1—C1'—H1'2108.3
O2—Mo3—O1182.7 (1)N1'—C2—H2106.1
O2—Mo3—O12173.8 (2)C1—C2—H2106.1
O8—Mo3—O970.9 (1)C3—C2—H2106.1
O8—Mo3—O10147.4 (2)C1'—C2'—H2'107.7
O8—Mo3—O1197.6 (2)N1—C2'—H2'107.7
O8—Mo3—O12103.4 (2)C3ii—C2'—H2'107.7
O9—Mo3—O1085.6 (1)C4—N2—H2n1109.0
O9—Mo3—O11165.8 (1)C5iii—N2—H2n1109.0
O9—Mo3—O1287.9 (1)C4—N2—H2n2109.0
O10—Mo3—O11101.4 (2)C5iii—N2—H2n2109.0
O10—Mo3—O1297.8 (1)H2n1—N2—H2n2107.8
O11—Mo3—O12103.1 (2)C2—C3—H3a109.5
O2—P1—O3111.7 (2)C2—C3—H3b109.5
O2—P1—O9i108.0 (2)H3a—C3—H3b109.5
O3—P1—O9i111.7 (2)C2—C3—H3c109.5
O2—P1—O1111.6 (2)H3a—C3—H3c109.5
O3—P1—O1105.4 (2)H3b—C3—H3c109.5
O9i—P1—O1108.4 (2)N2—C4—H4a109.5
P1—O2—Mo3119.3 (2)C5—C4—H4a109.5
P1—O3—Mo1125.9 (2)N2—C4—H4b109.5
P1—O3—Mo2126.7 (2)C5—C4—H4b109.5
Mo1—O3—Mo290.5 (1)H4a—C4—H4b108.1
Mo2—O5—Mo1127.0 (2)N2iii—C5—H5109.6
Mo3—O8—Mo2121.2 (2)C6—C5—H5109.6
P1i—O9—Mo2130.0 (2)C4—C5—H5109.6
P1i—O9—Mo3134.2 (2)C5—C6—H6a109.5
Mo2—O9—Mo395.3 (1)C5—C6—H6b109.5
Mo3i—O10—Mo3146.3 (2)H6a—C6—H6b109.5
C2'—N1—C1109.4 (7)C5—C6—H6c109.5
C1'—N1'—C2114.3 (7)H6a—C6—H6c109.5
C2—C1—N1109.8 (7)H6b—C6—H6c109.5
N1'—C1'—C2'108.9 (7)
O3—P1—O2—Mo361.5 (2)O9—Mo3—O8—Mo23.3 (2)
O9i—P1—O2—Mo361.7 (2)O2—Mo3—O8—Mo287.5 (2)
O1—P1—O2—Mo3179.3 (2)O7—Mo2—O8—Mo396.9 (2)
O11—Mo3—O2—P1179.5 (2)O6—Mo2—O8—Mo3157.0 (2)
O10—Mo3—O2—P176.3 (2)O5—Mo2—O8—Mo329.7 (4)
O8—Mo3—O2—P181.0 (2)O9—Mo2—O8—Mo33.37 (17)
O9—Mo3—O2—P19.8 (2)O3—Mo2—O8—Mo369.1 (2)
O2—P1—O3—Mo1152.3 (2)O7—Mo2—O9—P1i87.2 (3)
O9i—P1—O3—Mo131.2 (3)O6—Mo2—O9—P1i113.1 (4)
O1—P1—O3—Mo186.3 (2)O5—Mo2—O9—P1i10.8 (2)
O2—P1—O3—Mo228.7 (3)O8—Mo2—O9—P1i175.4 (3)
O9i—P1—O3—Mo292.4 (2)O3—Mo2—O9—P1i82.6 (2)
O1—P1—O3—Mo2150.1 (2)O7—Mo2—O9—Mo399.8 (2)
O4i—Mo1—O3—P1120.5 (2)O6—Mo2—O9—Mo360.0 (4)
O4—Mo1—O3—P180.9 (8)O5—Mo2—O9—Mo3162.3 (1)
O5i—Mo1—O3—P118.5 (2)O8—Mo2—O9—Mo32.4 (1)
O5—Mo1—O3—P1137.6 (2)O3—Mo2—O9—Mo390.4 (1)
O3i—Mo1—O3—P154.3 (2)O12—Mo3—O9—P1i80.1 (3)
O4i—Mo1—O3—Mo2101.4 (2)O11—Mo3—O9—P1i138.2 (5)
O4—Mo1—O3—Mo257.2 (8)O10—Mo3—O9—P1i17.9 (2)
O5i—Mo1—O3—Mo2156.7 (1)O8—Mo3—O9—P1i175.0 (3)
O5—Mo1—O3—Mo20.5 (1)O2—Mo3—O9—P1i97.1 (2)
O3i—Mo1—O3—Mo283.8 (1)O12—Mo3—O9—Mo2107.4 (2)
O7—Mo2—O3—P190.6 (6)O11—Mo3—O9—Mo234.4 (6)
O6—Mo2—O3—P1120.6 (3)O10—Mo3—O9—Mo2154.7 (1)
O5—Mo2—O3—P1137.1 (3)O8—Mo3—O9—Mo22.5 (1)
O8—Mo2—O3—P124.1 (2)O2—Mo3—O9—Mo275.5 (1)
O9—Mo2—O3—P148.4 (2)O12—Mo3—O10—Mo3i115.7 (1)
O7—Mo2—O3—Mo147.0 (6)O11—Mo3—O10—Mo3i139.1 (1)
O6—Mo2—O3—Mo1101.8 (1)O8—Mo3—O10—Mo3i14.6 (2)
O5—Mo2—O3—Mo10.5 (1)O9—Mo3—O10—Mo3i28.41 (8)
O8—Mo2—O3—Mo1161.7 (1)O2—Mo3—O10—Mo3i58.99 (8)
O9—Mo2—O3—Mo189.2 (1)C2'—N1—C1—C261 (1)
O7—Mo2—O5—Mo1169.7 (2)C2—N1'—C1'—C2'57 (2)
O6—Mo2—O5—Mo183.3 (2)C1'—N1'—C2—C154 (2)
O8—Mo2—O5—Mo143.0 (4)C1'—N1'—C2—C3175 (1)
O9—Mo2—O5—Mo174.6 (2)N1—C1—C2—N1'54 (1)
O3—Mo2—O5—Mo10.8 (2)N1—C1—C2—C3178 (1)
O4i—Mo1—O5—Mo283.0 (2)N1'—C1'—C2'—N160 (1)
O4—Mo1—O5—Mo2170.8 (2)N1'—C1'—C2'—C3ii175 (1)
O5i—Mo1—O5—Mo244.0 (2)C1—N1—C2'—C1'64 (1)
O3i—Mo1—O5—Mo285.1 (2)C1—N1—C2'—C3ii170.7 (9)
O3—Mo1—O5—Mo20.8 (2)C5iii—N2—C4—C559.2 (6)
O12—Mo3—O8—Mo286.3 (2)N2—C4—C5—N2iii56.0 (6)
O11—Mo3—O8—Mo2168.2 (2)N2—C4—C5—C6176.5 (4)
O10—Mo3—O8—Mo242.8 (3)
Symmetry codes: (i) x, y, z+1/2; (ii) x, y, z+3/2; (iii) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O2iv0.821.852.656 (4)168
O1w—H1w1···O40.862.112.970 (7)177
N1—H1n1···O10v0.902.223.067 (9)158
N1—H1n2···O1wii0.901.692.59 (1)172
N1—H1n3···O6vi0.902.162.825 (9)130
N1—H1n4···O1w0.901.972.84 (1)160
N2—H2n1···O8vii0.902.172.950 (6)145
N2—H2n1···O11vii0.902.162.886 (6)137
N2—H2n2···O70.902.012.872 (6)160
Symmetry codes: (ii) x, y, z+3/2; (iv) x, y+1, z; (v) x, y+1, z+1; (vi) x1/2, y+3/2, z+1/2; (vii) x, y+1, z+1/2.
 

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