Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803027375/br6129sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803027375/br6129Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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.
Na4Ni5[(As0.73·P0.27)O4]2[(As0.59·P1.41)O7]2 | F(000) = 995 |
Mr = 1039.26 | Dx = 3.868 Mg m−3 |
Monoclinic, P21/a | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yab | Cell parameters from 25 reflections |
a = 10.676 (2) Å | θ = 10.4–15° |
b = 6.716 (1) Å | µ = 10.56 mm−1 |
c = 12.812 (2) Å | T = 293 K |
β = 103.77 (1)° | Parallelepiped, brown |
V = 892.2 (3) Å3 | 0.20 × 0.08 × 0.02 mm |
Z = 2 |
Enraf-Nonius CAD-4 diffractometer | 1672 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.012 |
Graphite monochromator | θmax = 27.0°, θmin = 3.3° |
ω/2θ scans | h = 0→13 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→8 |
Tmin = 0.368, Tmax = 0.784 | l = −16→15 |
2051 measured reflections | 2 standard reflections every 120 min |
1942 independent reflections | intensity decay: 1.0% |
Refinement on F2 | Secondary 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 = 1.10 | Δρmax = 0.61 e Å−3 |
1942 reflections | Δρmin = −0.72 e Å−3 |
187 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
4 restraints | Extinction coefficient: 0.0013 (2) |
Primary atom site location: structure-invariant direct methods |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.0000 | 0.0000 | 0.5000 | 0.00915 (17) | |
Ni2 | 0.19757 (5) | 0.01111 (8) | 0.16483 (4) | 0.01275 (15) | |
Ni3 | 0.21707 (5) | 0.23704 (7) | 0.36451 (4) | 0.00782 (14) | |
As1 | 0.08907 (7) | 0.20966 (11) | 0.91873 (6) | 0.0093 (3) | 0.25 (1) |
P1 | 0.08907 (7) | 0.20966 (11) | 0.91873 (6) | 0.0093 (3) | 0.75 (2) |
As2 | 0.93149 (6) | 0.10195 (10) | 0.24501 (5) | 0.0071 (2) | 0.34 (1) |
P2 | 0.93149 (6) | 0.10195 (10) | 0.24501 (5) | 0.0071 (2) | 0.66 (2) |
As3 | 0.27348 (4) | 0.23408 (7) | 0.58506 (4) | 0.00626 (17) | 0.73 (1) |
P3 | 0.27348 (4) | 0.23408 (7) | 0.58506 (4) | 0.00626 (17) | 0.27 (2) |
Na1 | 0.62987 (19) | 0.0226 (3) | 0.14797 (15) | 0.0220 (4) | |
Na2 | 0.5442 (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) |
O1 | 0.1336 (3) | 0.2085 (4) | 0.4930 (2) | 0.0100 (6) | |
O2 | 0.3311 (3) | 0.2314 (4) | 0.2571 (2) | 0.0114 (6) | |
O3 | 0.7598 (3) | 0.0742 (4) | 0.6610 (2) | 0.0120 (6) | |
O4 | 0.3262 (3) | 0.0379 (4) | 0.6576 (2) | 0.0121 (6) | |
O5 | 0.8679 (3) | 0.2285 (4) | 0.4989 (2) | 0.0103 (6) | |
O6 | 0.9392 (3) | 0.2021 (4) | 0.8880 (3) | 0.0178 (7) | |
O7 | 0.0633 (3) | 0.1958 (4) | 0.2318 (2) | 0.0120 (6) | |
O8 | 0.1514 (3) | 0.2014 (5) | 0.0391 (2) | 0.0188 (7) | |
O9 | 0.6368 (3) | 0.1135 (5) | 0.8602 (3) | 0.0219 (7) | |
O10 | 0.0479 (3) | 0.0556 (5) | 0.6634 (2) | 0.0136 (6) | |
O11 | 0.1402 (3) | 0.0038 (4) | 0.8694 (2) | 0.0139 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0085 (3) | 0.0095 (3) | 0.0096 (3) | 0.0001 (3) | 0.0024 (3) | −0.0002 (3) |
Ni2 | 0.0138 (3) | 0.0112 (3) | 0.0128 (3) | 0.0005 (2) | 0.0023 (2) | −0.0011 (2) |
Ni3 | 0.0075 (3) | 0.0092 (3) | 0.0068 (3) | −0.00033 (19) | 0.00181 (19) | −0.00006 (18) |
As1 | 0.0107 (4) | 0.0087 (4) | 0.0086 (4) | −0.0009 (3) | 0.0023 (3) | −0.0002 (3) |
P1 | 0.0107 (4) | 0.0087 (4) | 0.0086 (4) | −0.0009 (3) | 0.0023 (3) | −0.0002 (3) |
As2 | 0.0066 (3) | 0.0080 (4) | 0.0066 (3) | 0.0003 (2) | 0.0018 (2) | 0.0001 (2) |
P2 | 0.0066 (3) | 0.0080 (4) | 0.0066 (3) | 0.0003 (2) | 0.0018 (2) | 0.0001 (2) |
As3 | 0.0064 (3) | 0.0058 (3) | 0.0065 (3) | −0.00081 (17) | 0.00136 (17) | −0.00039 (17) |
P3 | 0.0064 (3) | 0.0058 (3) | 0.0065 (3) | −0.00081 (17) | 0.00136 (17) | −0.00039 (17) |
Na1 | 0.0294 (10) | 0.0156 (9) | 0.0196 (9) | −0.0046 (8) | 0.0033 (8) | −0.0025 (7) |
Na2 | 0.0148 (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) |
O1 | 0.0083 (13) | 0.0128 (14) | 0.0092 (13) | −0.0017 (11) | 0.0028 (11) | 0.0016 (11) |
O2 | 0.0132 (14) | 0.0095 (14) | 0.0130 (14) | −0.0028 (11) | 0.0061 (11) | −0.0003 (11) |
O3 | 0.0138 (14) | 0.0097 (13) | 0.0128 (14) | 0.0025 (12) | 0.0037 (11) | −0.0007 (12) |
O4 | 0.0143 (14) | 0.0085 (14) | 0.0138 (14) | −0.0009 (11) | 0.0037 (12) | −0.0018 (11) |
O5 | 0.0102 (13) | 0.0124 (14) | 0.0080 (13) | 0.0017 (11) | 0.0019 (11) | 0.0015 (11) |
O6 | 0.0168 (15) | 0.0133 (15) | 0.0216 (16) | −0.0010 (12) | 0.0010 (13) | −0.0019 (12) |
O7 | 0.0108 (14) | 0.0119 (14) | 0.0130 (14) | 0.0002 (11) | 0.0023 (11) | 0.0013 (11) |
O8 | 0.0233 (17) | 0.0178 (16) | 0.0143 (15) | −0.0001 (13) | 0.0029 (13) | 0.0017 (12) |
O9 | 0.0254 (17) | 0.0162 (16) | 0.0238 (17) | 0.0069 (14) | 0.0051 (14) | −0.0036 (13) |
O10 | 0.0128 (14) | 0.0170 (15) | 0.0105 (13) | 0.0004 (12) | 0.0017 (11) | 0.0013 (12) |
O11 | 0.0121 (14) | 0.0156 (15) | 0.0146 (14) | 0.0048 (12) | 0.0041 (12) | −0.0025 (12) |
Ni1—O1i | 2.016 (3) | As/P3—O4 | 1.633 (3) |
Ni1—O1 | 2.016 (3) | As/P3—O3iv | 1.642 (3) |
Ni1—O10 | 2.068 (3) | As/P3—O1 | 1.677 (3) |
Ni1—O10i | 2.068 (3) | As/P3—O5iv | 1.682 (3) |
Ni1—O5ii | 2.082 (3) | Na1—O6ix | 2.287 (3) |
Ni1—O5iii | 2.082 (3) | Na1—O8vii | 2.364 (4) |
Ni2—O8 | 2.023 (3) | Na1—O7vii | 2.366 (3) |
Ni2—O6iii | 2.042 (3) | Na1—O4iii | 2.456 (3) |
Ni2—O9iii | 2.049 (3) | Na1—O11iii | 2.523 (4) |
Ni2—O2 | 2.195 (3) | Na1—O2vii | 2.805 (3) |
Ni2—O7 | 2.217 (3) | Na1—O9iii | 2.968 (4) |
Ni2—O3iii | 2.243 (3) | Na2—O3 | 2.307 (4) |
Ni3—O2 | 2.042 (3) | Na2—O4 | 2.327 (4) |
Ni3—O1 | 2.059 (3) | Na2—O10vii | 2.469 (6) |
Ni3—O5iv | 2.071 (3) | Na2—O9 | 2.501 (9) |
Ni3—O4v | 2.077 (3) | Na2—O2iii | 2.542 (4) |
Ni3—O7 | 2.081 (3) | Na2—O5iv | 2.789 (5) |
Ni3—O3iii | 2.139 (3) | Na2—O1vii | 2.951 (6) |
As/P1—O8vi | 1.528 (3) | Na2'—O3 | 2.40 (2) |
As/P1—O9iv | 1.554 (3) | Na2'—O4 | 2.444 (18) |
As/P1—O6ii | 1.555 (3) | Na2'—O5iv | 2.580 (15) |
As/P1—O11 | 1.666 (3) | Na2'—O2iii | 2.619 (19) |
As/P2—O10iii | 1.556 (3) | Na2'—O1vii | 2.713 (16) |
As/P2—O2vii | 1.583 (3) | Na2'—O5ix | 2.72 (4) |
As/P2—O7viii | 1.587 (3) | Na2'—O1x | 2.82 (4) |
As/P2—O11iii | 1.644 (3) | Na2'—O10vii | 2.95 (4) |
O1i—Ni1—O1 | 180.00 (17) | O1—Ni3—O5iv | 75.21 (11) |
O1i—Ni1—O10 | 95.03 (11) | O2—Ni3—O4v | 94.29 (11) |
O1—Ni1—O10 | 84.97 (11) | O1—Ni3—O4v | 94.32 (11) |
O1i—Ni1—O10i | 84.97 (11) | O5iv—Ni3—O4v | 96.23 (11) |
O1—Ni1—O10i | 95.03 (11) | O2—Ni3—O7 | 85.87 (11) |
O10—Ni1—O10i | 180.0 | O1—Ni3—O7 | 103.48 (11) |
O1i—Ni1—O5ii | 91.55 (11) | O5iv—Ni3—O7 | 178.30 (11) |
O1—Ni1—O5ii | 88.45 (11) | O4v—Ni3—O7 | 84.92 (11) |
O10—Ni1—O5ii | 82.99 (11) | O2—Ni3—O3iii | 76.70 (11) |
O10i—Ni1—O5ii | 97.01 (11) | O1—Ni3—O3iii | 96.83 (11) |
O1i—Ni1—O5iii | 88.45 (11) | O5iv—Ni3—O3iii | 98.11 (11) |
O1—Ni1—O5iii | 91.55 (11) | O4v—Ni3—O3iii | 163.68 (11) |
O10—Ni1—O5iii | 97.01 (11) | O7—Ni3—O3iii | 80.92 (11) |
O10i—Ni1—O5iii | 82.99 (11) | O8vi—As/P1—O9iv | 113.61 (18) |
O5ii—Ni1—O5iii | 180.000 (1) | O8vi—As/P1—O6ii | 115.41 (18) |
O8—Ni2—O6iii | 99.18 (13) | O9iv—As/P1—O6ii | 109.80 (17) |
O8—Ni2—O9iii | 100.89 (13) | O8vi—As/P1—O11 | 104.45 (16) |
O6iii—Ni2—O9iii | 103.71 (13) | O9iv—As/P1—O11 | 106.07 (16) |
O8—Ni2—O2 | 90.41 (12) | O6ii—As/P1—O11 | 106.69 (16) |
O6iii—Ni2—O2 | 166.58 (12) | O10iii—As/P2—O2vii | 112.59 (15) |
O9iii—Ni2—O2 | 83.45 (12) | O10iii—As/P2—O7viii | 112.37 (15) |
O8—Ni2—O7 | 84.12 (12) | O2vii—As/P2—O7viii | 111.60 (15) |
O6iii—Ni2—O7 | 92.49 (12) | O10iii—As/P2—O11iii | 109.30 (16) |
O9iii—Ni2—O7 | 161.90 (12) | O2vii—As/P2—O11iii | 102.14 (15) |
O2—Ni2—O7 | 79.10 (11) | O7viii—As/P2—O11iii | 108.24 (15) |
O8—Ni2—O3iii | 155.06 (12) | O4—As/P3—O3iv | 111.25 (14) |
O6iii—Ni2—O3iii | 96.33 (12) | O4—As/P3—O1 | 116.50 (14) |
O9iii—Ni2—O3iii | 94.21 (12) | O3iv—As/P3—O1 | 107.91 (14) |
O2—Ni2—O3iii | 71.59 (10) | O4—As/P3—O5iv | 108.37 (14) |
O7—Ni2—O3iii | 75.78 (10) | O3iv—As/P3—O5iv | 115.09 (14) |
O2—Ni3—O1 | 167.81 (11) | O1—As/P3—O5iv | 97.23 (13) |
O2—Ni3—O5iv | 95.28 (11) |
Symmetry codes: (i) −x, −y, −z+1; (ii) x−1, y, z; (iii) −x+1, −y, −z+1; (iv) x−1/2, −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, y−1/2, −z+1; (x) −x+1/2, y−1/2, −z+1. |
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