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The title compound, (NH4)2[Na2Ni(OH)6Mo6O18(H2O)2], features inversion-generated hexa­molybdonickelate(II) anions (Ni site symmetry \overline{1}). The anions are linked by the five-coordinate sodium cations into layers. Adjacent layers are linked through N—H...O and O—H...O hydrogen bonds involving the ammonium ions and water mol­ecules, thus forming a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806053761/hb2232sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806053761/hb2232Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](a-O) = 0.015 Å
  • R factor = 0.056
  • wR factor = 0.098
  • Data-to-parameter ratio = 14.3

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT416_ALERT_2_B Short Intra D-H..H-D H2 .. H2 .. 1.10 Ang. PLAT420_ALERT_2_B D-H Without Acceptor O1 - H1 ... ? PLAT420_ALERT_2_B D-H Without Acceptor O3 - H3 ... ? PLAT420_ALERT_2_B D-H Without Acceptor OW3 - HW3B ... ?
Alert level C PLAT213_ALERT_2_C Atom O6 has ADP max/min Ratio ............. 3.80 oblat PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.52 Ratio PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 84.00 A   3 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 13
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 4 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 7 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.

Poly[diammonium hexahydroxyoctadecaoxodisodiohexamolybdonickelate dihydrate] top
Crystal data top
(NH4)2[Na2Ni(OH)6Mo6O18]·2H2OF(000) = 1164
Mr = 1214.54Dx = 2.964 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ycCell parameters from 7685 reflections
a = 11.7792 (10) Åθ = 0.3–0.7°
b = 10.9353 (9) ŵ = 3.50 mm1
c = 11.7793 (10) ÅT = 296 K
β = 116.223 (4)°Block, light green
V = 1361.1 (2) Å30.16 × 0.12 × 0.11 mm
Z = 2
Data collection top
Bruker SMART CCD APEX II
diffractometer
2674 independent reflections
Radiation source: fine-focus sealed tube1396 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
ω scansθmax = 26.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1314
Tmin = 0.605, Tmax = 0.680k = 1313
7181 measured reflectionsl = 1214
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)] = 0.056Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.098H-atom parameters constrained
S = 0.95 w = 1/[σ2(Fo2) + (0.038P)2]
where P = (Fo2 + 2Fc2)/3
2674 reflections(Δ/σ)max < 0.001
187 parametersΔρmax = 0.75 e Å3
0 restraintsΔρmin = 0.67 e Å3
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
Ni0.50000.00000.00000.0203 (5)
Mo10.66140 (9)0.23128 (9)0.17284 (9)0.0236 (3)
Mo20.18736 (9)0.00712 (9)0.13713 (10)0.0254 (3)
Mo30.34982 (9)0.23942 (9)0.03826 (9)0.0234 (3)
Na0.9161 (9)0.3036 (9)0.0681 (10)0.041 (2)
O10.6445 (7)0.1090 (6)0.0168 (7)0.0209 (18)
H10.64180.14590.05010.025*
O20.5023 (7)0.1086 (6)0.1401 (7)0.0216 (18)
H20.50260.06830.20450.026*
O30.3572 (7)0.1142 (6)0.1057 (7)0.0225 (19)
H30.36000.15140.17010.027*
O40.7677 (7)0.0902 (7)0.2457 (7)0.028 (2)
O50.7639 (7)0.3216 (6)0.1453 (8)0.033 (2)
O60.6677 (7)0.2872 (7)0.3064 (7)0.032 (2)
O70.5069 (7)0.3068 (6)0.0507 (7)0.0244 (19)
O80.3515 (7)0.2902 (7)0.1731 (7)0.032 (2)
O90.2531 (7)0.3397 (7)0.0730 (8)0.033 (2)
O100.2343 (7)0.1050 (6)0.0124 (7)0.0259 (19)
O110.0886 (7)0.1044 (7)0.2473 (8)0.036 (2)
O120.0900 (7)0.0897 (7)0.1066 (8)0.039 (2)
OW10.9912 (11)0.2577 (10)0.0731 (11)0.048 (2)
HW1A0.94700.26450.15550.057*
HW1B1.05510.22940.07960.057*
OW20.4796 (9)0.0467 (7)0.3465 (8)0.053 (3)
HW2A0.40680.02350.32510.064*
HW2B0.51860.00100.41650.064*
OW30.8692 (9)0.4746 (10)0.0089 (9)0.082 (4)
HW3A0.89210.54220.03180.099*
HW3B0.86910.49820.07700.099*
N0.1695 (9)0.0346 (8)0.1939 (9)0.040 (3)
HN10.20090.03860.14210.048*
HN20.20210.10140.24740.048*
HN30.20190.01990.25000.048*
HN40.09010.03860.15890.048*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0232 (12)0.0228 (11)0.0154 (11)0.0013 (10)0.0090 (9)0.0017 (10)
Mo10.0287 (6)0.0229 (6)0.0181 (6)0.0044 (5)0.0094 (5)0.0062 (5)
Mo20.0227 (6)0.0285 (6)0.0215 (6)0.0015 (6)0.0066 (5)0.0025 (5)
Mo30.0294 (6)0.0221 (6)0.0189 (6)0.0040 (5)0.0108 (5)0.0011 (5)
Na0.041 (2)0.040 (2)0.042 (2)0.0002 (10)0.0175 (14)0.0002 (10)
O10.029 (5)0.018 (4)0.014 (4)0.002 (3)0.007 (4)0.004 (3)
O20.028 (5)0.024 (4)0.011 (4)0.000 (4)0.007 (4)0.001 (3)
O30.024 (5)0.021 (4)0.014 (4)0.002 (4)0.000 (4)0.002 (3)
O40.031 (5)0.036 (5)0.014 (4)0.000 (4)0.008 (4)0.001 (4)
O50.032 (5)0.029 (5)0.041 (6)0.002 (4)0.018 (5)0.004 (4)
O60.040 (5)0.032 (5)0.019 (5)0.001 (4)0.009 (4)0.020 (4)
O70.026 (5)0.025 (4)0.023 (5)0.004 (4)0.012 (4)0.003 (4)
O80.042 (6)0.035 (5)0.021 (5)0.006 (4)0.015 (4)0.009 (4)
O90.035 (6)0.037 (5)0.030 (5)0.007 (4)0.016 (4)0.005 (4)
O100.027 (5)0.032 (5)0.020 (5)0.002 (4)0.011 (4)0.004 (4)
O110.033 (6)0.043 (5)0.024 (5)0.017 (4)0.005 (4)0.000 (4)
O120.028 (6)0.047 (5)0.040 (6)0.003 (4)0.013 (5)0.009 (5)
OW10.048 (3)0.049 (3)0.048 (3)0.0015 (10)0.0226 (15)0.0011 (10)
OW20.100 (9)0.037 (5)0.030 (6)0.002 (5)0.035 (6)0.008 (4)
OW30.077 (9)0.118 (10)0.042 (7)0.013 (7)0.019 (6)0.023 (7)
N0.037 (7)0.058 (7)0.028 (6)0.003 (6)0.019 (5)0.003 (6)
Geometric parameters (Å, º) top
Ni—O12.015 (7)Mo3—O71.935 (7)
Ni—O32.022 (7)Mo3—O22.193 (7)
Ni—O22.023 (7)Mo3—O32.211 (7)
Ni—O1i2.015 (7)Na—OW32.045 (14)
Ni—O3i2.022 (7)Na—OW12.258 (16)
Ni—O2i2.023 (7)Na—O52.350 (13)
Mo1—O61.659 (7)Na—O12i2.389 (13)
Mo1—O51.698 (8)Na—O11ii2.442 (13)
Mo1—O41.933 (7)O1—H10.8740
Mo1—O71.937 (7)O2—H20.8764
Mo1—O22.196 (7)O3—H30.8742
Mo1—O12.209 (7)OW1—HW1A0.8794
Mo2—O111.684 (8)OW1—HW1B0.8487
Mo2—O121.712 (8)OW2—HW2A0.8195
Mo2—O4i1.909 (8)OW2—HW2B0.9100
Mo2—O101.922 (7)OW3—HW3A0.8577
Mo2—O32.204 (7)OW3—HW3B0.8422
Mo2—O1i2.250 (7)N—HN10.8438
Mo3—O81.674 (7)N—HN20.9301
Mo3—O91.702 (7)N—HN30.8446
Mo3—O101.934 (7)N—HN40.8406
O1—Ni—O1i180.0O2—Mo3—O373.4 (3)
O1—Ni—O3i82.4 (3)OW3—Na—OW189.6 (6)
O1i—Ni—O3i97.6 (3)OW3—Na—O589.6 (5)
O1—Ni—O397.6 (3)OW1—Na—O5156.6 (6)
O1i—Ni—O382.4 (3)OW3—Na—O12i162.6 (6)
O3i—Ni—O3180.0OW1—Na—O12i88.7 (5)
O1—Ni—O2i97.7 (3)O5—Na—O12i85.2 (4)
O1i—Ni—O2i82.3 (3)OW3—Na—O11ii88.5 (5)
O3i—Ni—O2i81.2 (3)OW1—Na—O11ii107.7 (5)
O3—Ni—O2i98.8 (3)O5—Na—O11ii95.6 (5)
O1—Ni—O282.3 (3)O12i—Na—O11ii108.5 (5)
O1i—Ni—O297.7 (3)OW3—Na—HW3A15.3
O3i—Ni—O298.8 (3)OW1—Na—HW3A98.6
O3—Ni—O281.2 (3)O5—Na—HW3A86.2
O2i—Ni—O2180.0O12i—Na—HW3A171.3
O6—Mo1—O5103.2 (4)O11ii—Na—HW3A74.0
O6—Mo1—O497.2 (3)OW3—Na—HW3B15.0
O5—Mo1—O4100.0 (3)OW1—Na—HW3B74.9
O6—Mo1—O7100.4 (3)O5—Na—HW3B101.9
O5—Mo1—O797.2 (4)O12i—Na—HW3B154.1
O4—Mo1—O7151.9 (3)O11ii—Na—HW3B95.6
O6—Mo1—O294.0 (3)HW3A—Na—HW3B28.1
O5—Mo1—O2160.9 (3)Ni—O1—Mo1101.6 (3)
O4—Mo1—O285.7 (3)Ni—O1—Mo2i101.4 (3)
O7—Mo1—O271.4 (3)Mo1—O1—Mo2i95.0 (3)
O6—Mo1—O1164.1 (3)Ni—O1—H1119.5
O5—Mo1—O190.2 (3)Mo1—O1—H1115.2
O4—Mo1—O171.9 (3)Mo2i—O1—H1120.0
O7—Mo1—O186.0 (3)Ni—O2—Mo3103.0 (3)
O2—Mo1—O174.2 (3)Ni—O2—Mo1101.8 (3)
O11—Mo2—O12104.7 (4)Mo3—O2—Mo197.3 (3)
O11—Mo2—O4i97.9 (4)Ni—O2—H2113.9
O12—Mo2—O4i101.9 (4)Mo3—O2—H2119.4
O11—Mo2—O10100.1 (3)Mo1—O2—H2118.6
O12—Mo2—O1095.7 (4)Ni—O3—Mo2102.8 (3)
O4i—Mo2—O10150.7 (3)Ni—O3—Mo3102.4 (3)
O11—Mo2—O393.5 (3)Mo2—O3—Mo396.7 (3)
O12—Mo2—O3159.4 (3)Ni—O3—H3118.8
O4i—Mo2—O384.8 (3)Mo2—O3—H3118.7
O10—Mo2—O371.2 (3)Mo3—O3—H3114.0
O11—Mo2—O1i163.4 (3)Mo2i—O4—Mo1117.7 (4)
O12—Mo2—O1i90.2 (3)Mo1—O5—Na138.9 (5)
O4i—Mo2—O1i71.3 (3)Mo3—O7—Mo1116.6 (4)
O10—Mo2—O1i85.4 (3)Mo2—O10—Mo3117.7 (4)
O3—Mo2—O1i73.3 (2)Mo2—O11—Naiii165.1 (5)
O8—Mo3—O9103.9 (4)Mo2—O12—Nai136.4 (5)
O8—Mo3—O1096.6 (3)Na—OW1—HW1A124.1
O9—Mo3—O10100.6 (3)Na—OW1—HW1B143.1
O8—Mo3—O7101.0 (3)HW1A—OW1—HW1B92.7
O9—Mo3—O796.0 (3)HW2A—OW2—HW2B98.2
O10—Mo3—O7152.1 (3)Na—OW3—HW3A125.7
O8—Mo3—O292.0 (3)Na—OW3—HW3B126.1
O9—Mo3—O2161.6 (3)HW3A—OW3—HW3B97.8
O10—Mo3—O286.5 (3)HN1—N—HN2105.5
O7—Mo3—O271.5 (3)HN1—N—HN3114.3
O8—Mo3—O3160.9 (3)HN2—N—HN396.6
O9—Mo3—O392.8 (3)HN1—N—HN4113.0
O10—Mo3—O370.9 (3)HN2—N—HN4109.2
O7—Mo3—O386.2 (3)HN3—N—HN4116.2
O3i—Ni—O1—Mo198.5 (3)O11—Mo2—O3—Mo386.8 (3)
O3—Ni—O1—Mo181.5 (3)O12—Mo2—O3—Mo365.5 (9)
O2i—Ni—O1—Mo1178.5 (3)O4i—Mo2—O3—Mo3175.6 (3)
O2—Ni—O1—Mo11.5 (3)O10—Mo2—O3—Mo312.7 (3)
O3i—Ni—O1—Mo2i0.9 (3)O1i—Mo2—O3—Mo3103.5 (3)
O3—Ni—O1—Mo2i179.1 (3)O8—Mo3—O3—Ni41.4 (11)
O2i—Ni—O1—Mo2i80.9 (3)O9—Mo3—O3—Ni167.7 (4)
O2—Ni—O1—Mo2i99.1 (3)O10—Mo3—O3—Ni92.1 (4)
O6—Mo1—O1—Ni41.5 (13)O7—Mo3—O3—Ni71.8 (3)
O5—Mo1—O1—Ni170.3 (3)O2—Mo3—O3—Ni0.0 (3)
O4—Mo1—O1—Ni89.2 (3)O8—Mo3—O3—Mo263.4 (10)
O7—Mo1—O1—Ni73.2 (3)O9—Mo3—O3—Mo287.6 (3)
O2—Mo1—O1—Ni1.4 (3)O10—Mo3—O3—Mo212.7 (3)
O6—Mo1—O1—Mo2i61.3 (12)O7—Mo3—O3—Mo2176.5 (3)
O5—Mo1—O1—Mo2i86.9 (3)O2—Mo3—O3—Mo2104.7 (3)
O4—Mo1—O1—Mo2i13.5 (3)O6—Mo1—O4—Mo2i173.7 (4)
O7—Mo1—O1—Mo2i176.0 (3)O5—Mo1—O4—Mo2i68.8 (5)
O2—Mo1—O1—Mo2i104.2 (3)O7—Mo1—O4—Mo2i57.9 (8)
O1—Ni—O2—Mo398.9 (3)O2—Mo1—O4—Mo2i92.9 (4)
O1i—Ni—O2—Mo381.1 (3)O1—Mo1—O4—Mo2i18.1 (4)
O3i—Ni—O2—Mo3180.0 (3)O6—Mo1—O5—Na141.9 (7)
O3—Ni—O2—Mo30.0 (3)O4—Mo1—O5—Na42.0 (8)
O1—Ni—O2—Mo11.5 (3)O7—Mo1—O5—Na115.6 (8)
O1i—Ni—O2—Mo1178.5 (3)O2—Mo1—O5—Na64.1 (13)
O3i—Ni—O2—Mo179.6 (3)O1—Mo1—O5—Na29.6 (8)
O3—Ni—O2—Mo1100.4 (3)OW3—Na—O5—Mo1146.3 (7)
O8—Mo3—O2—Ni167.5 (4)OW1—Na—O5—Mo158.2 (18)
O9—Mo3—O2—Ni42.6 (11)O12i—Na—O5—Mo117.1 (8)
O10—Mo3—O2—Ni71.1 (3)O11ii—Na—O5—Mo1125.3 (7)
O7—Mo3—O2—Ni91.5 (3)O8—Mo3—O7—Mo172.6 (4)
O3—Mo3—O2—Ni0.0 (3)O9—Mo3—O7—Mo1178.1 (4)
O8—Mo3—O2—Mo188.5 (3)O10—Mo3—O7—Mo155.5 (8)
O9—Mo3—O2—Mo161.4 (11)O2—Mo3—O7—Mo115.7 (3)
O10—Mo3—O2—Mo1175.0 (3)O3—Mo3—O7—Mo189.5 (4)
O7—Mo3—O2—Mo112.5 (3)O6—Mo1—O7—Mo375.0 (4)
O3—Mo3—O2—Mo1104.0 (3)O5—Mo1—O7—Mo3179.9 (4)
O6—Mo1—O2—Ni167.9 (3)O4—Mo1—O7—Mo352.8 (8)
O5—Mo1—O2—Ni37.4 (10)O2—Mo1—O7—Mo315.7 (3)
O4—Mo1—O2—Ni70.9 (3)O1—Mo1—O7—Mo390.4 (4)
O7—Mo1—O2—Ni92.5 (3)O11—Mo2—O10—Mo373.9 (5)
O1—Mo1—O2—Ni1.4 (3)O12—Mo2—O10—Mo3180.0 (4)
O6—Mo1—O2—Mo387.2 (3)O4i—Mo2—O10—Mo353.2 (8)
O5—Mo1—O2—Mo367.5 (10)O3—Mo2—O10—Mo316.4 (3)
O4—Mo1—O2—Mo3175.9 (3)O1i—Mo2—O10—Mo390.3 (4)
O7—Mo1—O2—Mo312.5 (3)O8—Mo3—O10—Mo2178.4 (4)
O1—Mo1—O2—Mo3103.5 (3)O9—Mo3—O10—Mo272.9 (5)
O1—Ni—O3—Mo2179.1 (3)O7—Mo3—O10—Mo252.6 (9)
O1i—Ni—O3—Mo20.9 (3)O2—Mo3—O10—Mo290.0 (4)
O2i—Ni—O3—Mo280.1 (3)O3—Mo3—O10—Mo216.4 (3)
O2—Ni—O3—Mo299.9 (3)O12—Mo2—O11—Naiii46 (2)
O1—Ni—O3—Mo381.0 (3)O4i—Mo2—O11—Naiii59 (2)
O1i—Ni—O3—Mo399.0 (3)O10—Mo2—O11—Naiii144 (2)
O2i—Ni—O3—Mo3180.0 (3)O3—Mo2—O11—Naiii144 (2)
O2—Ni—O3—Mo30.0 (3)O1i—Mo2—O11—Naiii107 (2)
O11—Mo2—O3—Ni168.8 (4)O11—Mo2—O12—Nai140.2 (7)
O12—Mo2—O3—Ni38.9 (10)O4i—Mo2—O12—Nai38.6 (8)
O4i—Mo2—O3—Ni71.2 (3)O10—Mo2—O12—Nai117.8 (7)
O10—Mo2—O3—Ni91.7 (4)O3—Mo2—O12—Nai68.5 (13)
O1i—Mo2—O3—Ni0.8 (3)O1i—Mo2—O12—Nai32.3 (7)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1/2, z+1/2; (iii) x1, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N—HN1···O100.841.882.681 (12)157
N—HN2···O9iv0.932.032.830 (12)143
N—HN3···O5v0.842.062.883 (12)164
N—HN4···O12vi0.842.012.826 (12)164
O1—H1···O6vii0.871.982.847 (10)169
O2—H2···OW20.881.822.649 (11)156
O3—H3···O8vii0.871.912.781 (11)171
OW1—HW1B···O10viii0.852.343.074 (14)146
OW2—HW2B···O7v0.912.182.864 (10)131
OW3—HW3A···O9ix0.862.362.891 (13)121
OW3—HW3B···O4vii0.842.132.690 (12)124
Symmetry codes: (iv) x, y+1/2, z+1/2; (v) x+1, y1/2, z+1/2; (vi) x, y, z; (vii) x, y+1/2, z1/2; (viii) x+1, y, z; (ix) x+1, y+1, z.
 

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