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Crystals of the title compound, tetrasodium pentanickel arsenic-phosphorus (2.64/3.36) docosaoxide, has been grown by a solid-state reaction and characterized by single-crystal X-ray diffraction. The structure is built up from corner- and edge-sharing (AsP)O4 tetrahedra, (AsP)2O7 groups, NiO6 octahedra and Ni2O9 units, giving rise to a polyhedral connectivity having tunnels running along the [001] direction. It is isostructural with Na4Ni5(PO4)2(P2O7)2.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803027375/br6129sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803027375/br6129Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Ni-O) = 0.003 Å
  • Disorder in solvent or counterion
  • R factor = 0.024
  • wR factor = 0.065
  • Data-to-parameter ratio = 10.4

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 ............ 0.50 Ratio PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT128_ALERT_4_C Non-standard setting of Space group P21/c .... P21/a PLAT301_ALERT_3_C Main Residue Disorder ......................... 9.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 33.00 Perc. PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P1 AS/P1 O8 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P1 AS/P1 O9 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P1 AS/P1 O6 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P1 AS/P1 O11 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P2 AS/P2 O10 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P2 AS/P2 O2 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P2 AS/P2 O7 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P2 AS/P2 O11 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P3 AS/P3 O4 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P3 AS/P3 O3 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P3 AS/P3 O1 PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... AS/P3 AS/P3 O5 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P1 O8 AS/P1 O9 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P1 O8 AS/P1 O6 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P1 O9 AS/P1 O6 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P1 O8 AS/P1 O11 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P1 O9 AS/P1 O11 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P1 O6 AS/P1 O11 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P2 O10 AS/P2 O2 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P2 O10 AS/P2 O7 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P2 O2 AS/P2 O7 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P2 O10 AS/P2 O11 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P2 O2 AS/P2 O11 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P2 O7 AS/P2 O11 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P3 O4 AS/P3 O3 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P3 O4 AS/P3 O1 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P3 O3 AS/P3 O1 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P3 O4 AS/P3 O5 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P3 O3 AS/P3 O5 PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... AS/P3 O1 AS/P3 O5
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 37 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 33 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 1 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: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

tetrasodium pentanickel arsenic-phosphorus (2.67/3.35) twentytwooxide top
Crystal data top
Na4Ni5[(As0.73·P0.27)O4]2[(As0.59·P1.41)O7]2F(000) = 995
Mr = 1039.26Dx = 3.868 Mg m3
Monoclinic, P21/aMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yabCell parameters from 25 reflections
a = 10.676 (2) Åθ = 10.4–15°
b = 6.716 (1) ŵ = 10.56 mm1
c = 12.812 (2) ÅT = 293 K
β = 103.77 (1)°Parallelepiped, brown
V = 892.2 (3) Å30.20 × 0.08 × 0.02 mm
Z = 2
Data collection top
Enraf-Nonius CAD-4
diffractometer
1672 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.012
Graphite monochromatorθmax = 27.0°, θmin = 3.3°
ω/2θ scansh = 013
Absorption correction: ψ scan
(North et al., 1968)
k = 08
Tmin = 0.368, Tmax = 0.784l = 1615
2051 measured reflections2 standard reflections every 120 min
1942 independent reflections intensity decay: 1.0%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024 w = 1/[σ2(Fo2) + (0.0309P)2 + 1.9015P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.065(Δ/σ)max = 0.032
S = 1.10Δρmax = 0.61 e Å3
1942 reflectionsΔρmin = 0.72 e Å3
187 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
4 restraintsExtinction coefficient: 0.0013 (2)
Primary atom site location: structure-invariant direct methods
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*/UeqOcc. (<1)
Ni10.00000.00000.50000.00915 (17)
Ni20.19757 (5)0.01111 (8)0.16483 (4)0.01275 (15)
Ni30.21707 (5)0.23704 (7)0.36451 (4)0.00782 (14)
As10.08907 (7)0.20966 (11)0.91873 (6)0.0093 (3)0.25 (1)
P10.08907 (7)0.20966 (11)0.91873 (6)0.0093 (3)0.75 (2)
As20.93149 (6)0.10195 (10)0.24501 (5)0.0071 (2)0.34 (1)
P20.93149 (6)0.10195 (10)0.24501 (5)0.0071 (2)0.66 (2)
As30.27348 (4)0.23408 (7)0.58506 (4)0.00626 (17)0.73 (1)
P30.27348 (4)0.23408 (7)0.58506 (4)0.00626 (17)0.27 (2)
Na10.62987 (19)0.0226 (3)0.14797 (15)0.0220 (4)
Na20.5442 (3)0.0767 (7)0.6627 (7)0.0311 (14)0.84 (2)
Na2'0.5314 (17)0.018 (4)0.605 (4)0.030 (8)0.16 (2)
O10.1336 (3)0.2085 (4)0.4930 (2)0.0100 (6)
O20.3311 (3)0.2314 (4)0.2571 (2)0.0114 (6)
O30.7598 (3)0.0742 (4)0.6610 (2)0.0120 (6)
O40.3262 (3)0.0379 (4)0.6576 (2)0.0121 (6)
O50.8679 (3)0.2285 (4)0.4989 (2)0.0103 (6)
O60.9392 (3)0.2021 (4)0.8880 (3)0.0178 (7)
O70.0633 (3)0.1958 (4)0.2318 (2)0.0120 (6)
O80.1514 (3)0.2014 (5)0.0391 (2)0.0188 (7)
O90.6368 (3)0.1135 (5)0.8602 (3)0.0219 (7)
O100.0479 (3)0.0556 (5)0.6634 (2)0.0136 (6)
O110.1402 (3)0.0038 (4)0.8694 (2)0.0139 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0085 (3)0.0095 (3)0.0096 (3)0.0001 (3)0.0024 (3)0.0002 (3)
Ni20.0138 (3)0.0112 (3)0.0128 (3)0.0005 (2)0.0023 (2)0.0011 (2)
Ni30.0075 (3)0.0092 (3)0.0068 (3)0.00033 (19)0.00181 (19)0.00006 (18)
As10.0107 (4)0.0087 (4)0.0086 (4)0.0009 (3)0.0023 (3)0.0002 (3)
P10.0107 (4)0.0087 (4)0.0086 (4)0.0009 (3)0.0023 (3)0.0002 (3)
As20.0066 (3)0.0080 (4)0.0066 (3)0.0003 (2)0.0018 (2)0.0001 (2)
P20.0066 (3)0.0080 (4)0.0066 (3)0.0003 (2)0.0018 (2)0.0001 (2)
As30.0064 (3)0.0058 (3)0.0065 (3)0.00081 (17)0.00136 (17)0.00039 (17)
P30.0064 (3)0.0058 (3)0.0065 (3)0.00081 (17)0.00136 (17)0.00039 (17)
Na10.0294 (10)0.0156 (9)0.0196 (9)0.0046 (8)0.0033 (8)0.0025 (7)
Na20.0148 (12)0.0264 (17)0.053 (4)0.0004 (11)0.0091 (15)0.010 (2)
Na2'0.009 (7)0.032 (11)0.051 (19)0.011 (6)0.012 (8)0.017 (12)
O10.0083 (13)0.0128 (14)0.0092 (13)0.0017 (11)0.0028 (11)0.0016 (11)
O20.0132 (14)0.0095 (14)0.0130 (14)0.0028 (11)0.0061 (11)0.0003 (11)
O30.0138 (14)0.0097 (13)0.0128 (14)0.0025 (12)0.0037 (11)0.0007 (12)
O40.0143 (14)0.0085 (14)0.0138 (14)0.0009 (11)0.0037 (12)0.0018 (11)
O50.0102 (13)0.0124 (14)0.0080 (13)0.0017 (11)0.0019 (11)0.0015 (11)
O60.0168 (15)0.0133 (15)0.0216 (16)0.0010 (12)0.0010 (13)0.0019 (12)
O70.0108 (14)0.0119 (14)0.0130 (14)0.0002 (11)0.0023 (11)0.0013 (11)
O80.0233 (17)0.0178 (16)0.0143 (15)0.0001 (13)0.0029 (13)0.0017 (12)
O90.0254 (17)0.0162 (16)0.0238 (17)0.0069 (14)0.0051 (14)0.0036 (13)
O100.0128 (14)0.0170 (15)0.0105 (13)0.0004 (12)0.0017 (11)0.0013 (12)
O110.0121 (14)0.0156 (15)0.0146 (14)0.0048 (12)0.0041 (12)0.0025 (12)
Geometric parameters (Å, º) top
Ni1—O1i2.016 (3)As/P3—O41.633 (3)
Ni1—O12.016 (3)As/P3—O3iv1.642 (3)
Ni1—O102.068 (3)As/P3—O11.677 (3)
Ni1—O10i2.068 (3)As/P3—O5iv1.682 (3)
Ni1—O5ii2.082 (3)Na1—O6ix2.287 (3)
Ni1—O5iii2.082 (3)Na1—O8vii2.364 (4)
Ni2—O82.023 (3)Na1—O7vii2.366 (3)
Ni2—O6iii2.042 (3)Na1—O4iii2.456 (3)
Ni2—O9iii2.049 (3)Na1—O11iii2.523 (4)
Ni2—O22.195 (3)Na1—O2vii2.805 (3)
Ni2—O72.217 (3)Na1—O9iii2.968 (4)
Ni2—O3iii2.243 (3)Na2—O32.307 (4)
Ni3—O22.042 (3)Na2—O42.327 (4)
Ni3—O12.059 (3)Na2—O10vii2.469 (6)
Ni3—O5iv2.071 (3)Na2—O92.501 (9)
Ni3—O4v2.077 (3)Na2—O2iii2.542 (4)
Ni3—O72.081 (3)Na2—O5iv2.789 (5)
Ni3—O3iii2.139 (3)Na2—O1vii2.951 (6)
As/P1—O8vi1.528 (3)Na2'—O32.40 (2)
As/P1—O9iv1.554 (3)Na2'—O42.444 (18)
As/P1—O6ii1.555 (3)Na2'—O5iv2.580 (15)
As/P1—O111.666 (3)Na2'—O2iii2.619 (19)
As/P2—O10iii1.556 (3)Na2'—O1vii2.713 (16)
As/P2—O2vii1.583 (3)Na2'—O5ix2.72 (4)
As/P2—O7viii1.587 (3)Na2'—O1x2.82 (4)
As/P2—O11iii1.644 (3)Na2'—O10vii2.95 (4)
O1i—Ni1—O1180.00 (17)O1—Ni3—O5iv75.21 (11)
O1i—Ni1—O1095.03 (11)O2—Ni3—O4v94.29 (11)
O1—Ni1—O1084.97 (11)O1—Ni3—O4v94.32 (11)
O1i—Ni1—O10i84.97 (11)O5iv—Ni3—O4v96.23 (11)
O1—Ni1—O10i95.03 (11)O2—Ni3—O785.87 (11)
O10—Ni1—O10i180.0O1—Ni3—O7103.48 (11)
O1i—Ni1—O5ii91.55 (11)O5iv—Ni3—O7178.30 (11)
O1—Ni1—O5ii88.45 (11)O4v—Ni3—O784.92 (11)
O10—Ni1—O5ii82.99 (11)O2—Ni3—O3iii76.70 (11)
O10i—Ni1—O5ii97.01 (11)O1—Ni3—O3iii96.83 (11)
O1i—Ni1—O5iii88.45 (11)O5iv—Ni3—O3iii98.11 (11)
O1—Ni1—O5iii91.55 (11)O4v—Ni3—O3iii163.68 (11)
O10—Ni1—O5iii97.01 (11)O7—Ni3—O3iii80.92 (11)
O10i—Ni1—O5iii82.99 (11)O8vi—As/P1—O9iv113.61 (18)
O5ii—Ni1—O5iii180.000 (1)O8vi—As/P1—O6ii115.41 (18)
O8—Ni2—O6iii99.18 (13)O9iv—As/P1—O6ii109.80 (17)
O8—Ni2—O9iii100.89 (13)O8vi—As/P1—O11104.45 (16)
O6iii—Ni2—O9iii103.71 (13)O9iv—As/P1—O11106.07 (16)
O8—Ni2—O290.41 (12)O6ii—As/P1—O11106.69 (16)
O6iii—Ni2—O2166.58 (12)O10iii—As/P2—O2vii112.59 (15)
O9iii—Ni2—O283.45 (12)O10iii—As/P2—O7viii112.37 (15)
O8—Ni2—O784.12 (12)O2vii—As/P2—O7viii111.60 (15)
O6iii—Ni2—O792.49 (12)O10iii—As/P2—O11iii109.30 (16)
O9iii—Ni2—O7161.90 (12)O2vii—As/P2—O11iii102.14 (15)
O2—Ni2—O779.10 (11)O7viii—As/P2—O11iii108.24 (15)
O8—Ni2—O3iii155.06 (12)O4—As/P3—O3iv111.25 (14)
O6iii—Ni2—O3iii96.33 (12)O4—As/P3—O1116.50 (14)
O9iii—Ni2—O3iii94.21 (12)O3iv—As/P3—O1107.91 (14)
O2—Ni2—O3iii71.59 (10)O4—As/P3—O5iv108.37 (14)
O7—Ni2—O3iii75.78 (10)O3iv—As/P3—O5iv115.09 (14)
O2—Ni3—O1167.81 (11)O1—As/P3—O5iv97.23 (13)
O2—Ni3—O5iv95.28 (11)
Symmetry codes: (i) x, y, z+1; (ii) x1, y, z; (iii) x+1, y, z+1; (iv) x1/2, y+1/2, z; (v) x+1/2, y+1/2, z+1; (vi) x, y, z+1; (vii) x+1/2, y+1/2, z; (viii) x+1, y, z; (ix) x+3/2, y1/2, z+1; (x) x+1/2, y1/2, z+1.
 

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