Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100002924/sk1361sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100002924/sk1361Isup2.hkl |
CCDC reference: 146033
Data collection: CAD-4 Software (Enraf-Nonius, 1994); cell refinement: PARAM (reference?); data reduction: NRCVAX (Gabe et al., 1989); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97; molecular graphics: ORTEPIII (Burnett & Johnson, 1996).
Na2[Zn(C6H11O2)4] | F(000) = 1216 |
Mr = 571.96 | Dx = 1.255 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 37.605 (7) Å | Cell parameters from 75 reflections |
b = 7.7797 (6) Å | θ = 8.1–14.7° |
c = 10.347 (2) Å | µ = 0.88 mm−1 |
β = 90.82 (2)° | T = 293 K |
V = 3026.8 (8) Å3 | Plate, colourless |
Z = 4 | 0.71 × 0.51 × 0.10 mm |
Enraf-Nonius CAD-4 diffractometer | 2108 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.124 |
Graphite monochromator | θmax = 28°, θmin = 1.1° |
pure ω scan | h = −49→49 |
Absorption correction: integration (NRCVAX; Gabe et al., 1989) | k = −10→0 |
Tmin = 0.55, Tmax = 0.92 | l = −13→13 |
7288 measured reflections | 3 standard reflections every 600 reflections |
3651 independent reflections | intensity decay: 2.1% |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.055 | H-atom parameters constrained |
wR(F2) = 0.133 | Calculated w = 1/[σ2(Fo2) + (0.0547P)2 + 0.1048P] where P = (Fo2 + 2Fc2)/3 |
S = 0.99 | (Δ/σ)max = 0.001 |
3651 reflections | Δρmax = 0.68 e Å−3 |
164 parameters | Δρmin = −0.81 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00101 (19) |
Experimental. There were only a few crystals which were suitable for the structure analysis. They were sealed in glass capillaries and tested on the diffractometer. The crystal with the best scattering properties was used for the subsequent analysis. However, the crystal size was too large for the homogeneous part of the X-ray beam, hence the rather large value of Rint = 0.12. |
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 | ||
Zn | 1/2 | 0.25161 (6) | 3/4 | 0.04063 (17) | |
O12 | 0.53875 (6) | −0.0710 (3) | 0.8296 (2) | 0.0556 (6) | |
O11 | 0.53850 (5) | 0.1215 (2) | 0.6711 (2) | 0.0469 (5) | |
O21 | 0.47426 (6) | 0.4262 (3) | 0.6484 (2) | 0.0502 (5) | |
C21 | 0.46385 (7) | 0.3958 (4) | 0.5310 (3) | 0.0408 (6) | |
O22 | 0.47551 (5) | 0.2755 (2) | 0.4663 (2) | 0.0502 (5) | |
C11 | 0.55251 (7) | −0.0017 (4) | 0.7358 (3) | 0.0457 (7) | |
C22 | 0.43519 (7) | 0.5132 (4) | 0.4801 (3) | 0.0513 (7) | |
H22A | 0.4331 | 0.5014 | 0.3870 | 0.062* | |
H22B | 0.4413 | 0.6316 | 0.4997 | 0.062* | |
C12 | 0.58816 (9) | −0.0638 (6) | 0.6889 (4) | 0.0706 (10) | |
H12A | 0.5892 | −0.1879 | 0.6972 | 0.085* | |
H12B | 0.5903 | −0.0359 | 0.5980 | 0.085* | |
C23 | 0.39983 (9) | 0.4678 (6) | 0.5420 (4) | 0.0737 (11) | |
H23A | 0.3964 | 0.3445 | 0.5362 | 0.088* | |
H23B | 0.4011 | 0.4978 | 0.6329 | 0.088* | |
C24 | 0.36822 (10) | 0.5555 (8) | 0.4819 (6) | 0.1016 (17) | |
H24A | 0.3677 | 0.5320 | 0.3899 | 0.122* | |
H24B | 0.3707 | 0.6787 | 0.4933 | 0.122* | |
C13 | 0.61794 (10) | 0.0110 (8) | 0.7595 (6) | 0.1042 (17) | |
H13A | 0.6161 | −0.0192 | 0.8501 | 0.125* | |
H13B | 0.6166 | 0.1352 | 0.7529 | 0.125* | |
C14 | 0.65414 (11) | −0.0485 (9) | 0.7103 (8) | 0.130 (2) | |
H14A | 0.6551 | −0.1729 | 0.7155 | 0.156* | |
H14B | 0.6557 | −0.0176 | 0.6197 | 0.156* | |
C25 | 0.33336 (12) | 0.4985 (11) | 0.5393 (9) | 0.142 (3) | |
H25A | 0.3319 | 0.3741 | 0.5359 | 0.170* | |
H25B | 0.3328 | 0.5326 | 0.6295 | 0.170* | |
C15 | 0.68435 (17) | 0.0188 (15) | 0.7763 (12) | 0.194 (5) | |
H15A | 0.6830 | −0.0116 | 0.8670 | 0.232* | |
H15B | 0.6839 | 0.1432 | 0.7703 | 0.232* | |
C26 | 0.30205 (17) | 0.5726 (17) | 0.4708 (12) | 0.237 (6) | |
H26A | 0.3019 | 0.6950 | 0.4822 | 0.355* | |
H26B | 0.2807 | 0.5246 | 0.5053 | 0.355* | |
H26C | 0.3033 | 0.5462 | 0.3803 | 0.355* | |
C16 | 0.71977 (14) | −0.0467 (15) | 0.7232 (14) | 0.240 (6) | |
H16A | 0.7183 | −0.1685 | 0.7092 | 0.360* | |
H16B | 0.7386 | −0.0224 | 0.7842 | 0.360* | |
H16C | 0.7246 | 0.0099 | 0.6429 | 0.360* | |
Na1 | 1/2 | 0 | 1 | 0.0441 (4) | |
Na2 | 1/2 | 0.6857 (2) | 3/4 | 0.0480 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn | 0.0575 (3) | 0.0346 (2) | 0.0298 (2) | 0 | 0.00081 (17) | 0 |
O12 | 0.0665 (12) | 0.0593 (13) | 0.0413 (13) | 0.0089 (10) | 0.0091 (11) | 0.0055 (12) |
O11 | 0.0564 (10) | 0.0450 (11) | 0.0394 (12) | 0.0026 (9) | 0.0057 (9) | 0.0020 (10) |
O21 | 0.0715 (12) | 0.0418 (10) | 0.0373 (12) | 0.0046 (10) | −0.0063 (10) | 0.0007 (10) |
C21 | 0.0540 (15) | 0.0382 (14) | 0.0302 (14) | −0.0036 (13) | 0.0027 (12) | 0.0030 (13) |
O22 | 0.0697 (11) | 0.0444 (12) | 0.0364 (11) | 0.0072 (10) | −0.0002 (9) | −0.0039 (10) |
C11 | 0.0499 (14) | 0.0514 (16) | 0.0358 (16) | 0.0000 (13) | 0.0017 (12) | −0.0077 (15) |
C22 | 0.0601 (17) | 0.0505 (16) | 0.0433 (19) | 0.0042 (14) | −0.0026 (14) | 0.0070 (16) |
C12 | 0.0590 (18) | 0.088 (3) | 0.065 (3) | 0.0120 (18) | 0.0096 (17) | −0.009 (2) |
C23 | 0.073 (2) | 0.091 (3) | 0.058 (2) | 0.016 (2) | 0.0069 (18) | 0.009 (2) |
C24 | 0.068 (2) | 0.139 (4) | 0.097 (4) | 0.021 (3) | 0.003 (2) | 0.018 (4) |
C13 | 0.070 (2) | 0.143 (4) | 0.100 (4) | 0.002 (3) | 0.004 (2) | −0.036 (4) |
C14 | 0.060 (3) | 0.173 (6) | 0.158 (7) | 0.011 (3) | 0.007 (3) | −0.030 (5) |
C25 | 0.079 (3) | 0.206 (7) | 0.142 (6) | 0.024 (4) | 0.020 (3) | 0.013 (6) |
C15 | 0.104 (4) | 0.271 (11) | 0.206 (11) | 0.003 (6) | 0.019 (5) | −0.047 (9) |
C26 | 0.085 (4) | 0.431 (18) | 0.194 (10) | 0.024 (7) | 0.013 (5) | 0.040 (14) |
C16 | 0.065 (3) | 0.353 (14) | 0.303 (16) | 0.020 (6) | 0.014 (5) | −0.006 (14) |
Na1 | 0.0634 (8) | 0.0383 (8) | 0.0306 (8) | −0.0018 (7) | 0.0022 (7) | 0.0018 (7) |
Na2 | 0.0711 (9) | 0.0395 (7) | 0.0336 (8) | 0 | 0.0047 (7) | 0 |
Zn—O11i | 1.955 (2) | C23—C24 | 1.498 (5) |
Zn—O11 | 1.955 (2) | C24—C25 | 1.514 (7) |
Zn—O21 | 1.964 (2) | C25—C26 | 1.483 (10) |
Zn—O21i | 1.964 (2) | O12—Na1 | 2.368 (2) |
Zn—Na1i | 3.2439 (5) | Na1—O22iv | 2.3567 (19) |
Zn—Na1 | 3.2439 (5) | Na1—O22i | 2.3567 (19) |
O12—C11 | 1.231 (4) | Na1—O12v | 2.368 (2) |
O12—Na2ii | 2.520 (3) | Na1—O11iv | 2.460 (2) |
O11—C11 | 1.279 (4) | Na1—O11i | 2.460 (2) |
C11—C12 | 1.511 (4) | Na1—C11i | 3.116 (3) |
C12—C13 | 1.450 (6) | Na1—C11iv | 3.116 (3) |
C13—C14 | 1.532 (7) | Na1—Znv | 3.2439 (5) |
C14—C15 | 1.418 (9) | Na1—Na2ii | 3.5594 (13) |
C15—C16 | 1.535 (11) | Na1—Na2vi | 3.5594 (13) |
O11—Na1i | 2.460 (2) | O21—Na2 | 2.468 (3) |
O21—C21 | 1.293 (4) | Na2—O22vii | 2.451 (2) |
C21—O22 | 1.235 (4) | Na2—O22iii | 2.451 (2) |
C21—C22 | 1.502 (4) | Na2—O21i | 2.468 (3) |
O22—Na1i | 2.3567 (19) | Na2—O12viii | 2.520 (3) |
O22—Na2iii | 2.451 (2) | Na2—O12ix | 2.520 (3) |
C11—Na1i | 3.116 (3) | Na2—Na1viii | 3.5594 (12) |
C22—C23 | 1.525 (5) | Na2—Na1ix | 3.5594 (12) |
O11i—Zn—O11 | 117.64 (12) | O11iv—Na1—C11iv | 22.85 (7) |
O11i—Zn—O21 | 102.67 (9) | O11i—Na1—C11iv | 157.15 (7) |
O11—Zn—O21 | 119.79 (10) | C11i—Na1—C11iv | 180.000 (1) |
O11i—Zn—O21i | 119.79 (10) | O22iv—Na1—Znv | 64.21 (6) |
O11—Zn—O21i | 102.67 (9) | O22i—Na1—Znv | 115.79 (6) |
O21—Zn—O21i | 92.50 (12) | O12v—Na1—Znv | 62.63 (6) |
O11i—Zn—Na1i | 91.67 (7) | O12—Na1—Znv | 117.37 (6) |
O11—Zn—Na1i | 49.16 (6) | O11iv—Na1—Znv | 36.96 (5) |
O21—Zn—Na1i | 89.78 (7) | O11i—Na1—Znv | 143.04 (5) |
O21i—Zn—Na1i | 146.97 (7) | C11i—Na1—Znv | 127.90 (6) |
O11i—Zn—Na1 | 49.16 (6) | C11iv—Na1—Znv | 52.10 (6) |
O11—Zn—Na1 | 91.67 (7) | O22iv—Na1—Zn | 115.79 (6) |
O21—Zn—Na1 | 146.97 (7) | O22i—Na1—Zn | 64.21 (6) |
O21i—Zn—Na1 | 89.78 (7) | O12v—Na1—Zn | 117.37 (6) |
Na1i—Zn—Na1 | 105.769 (17) | O12—Na1—Zn | 62.63 (6) |
C11—O12—Na1 | 139.0 (2) | O11iv—Na1—Zn | 143.04 (5) |
C11—O12—Na2ii | 108.6 (2) | O11i—Na1—Zn | 36.96 (5) |
Na1—O12—Na2ii | 93.42 (8) | C11i—Na1—Zn | 52.10 (6) |
C11—O11—Zn | 118.15 (19) | C11iv—Na1—Zn | 127.90 (6) |
C11—O11—Na1i | 108.80 (17) | Znv—Na1—Zn | 180.000 (1) |
Zn—O11—Na1i | 93.88 (8) | O22iv—Na1—Na2ii | 43.26 (6) |
C21—O21—Zn | 121.13 (19) | O22i—Na1—Na2ii | 136.74 (6) |
C21—O21—Na2 | 131.40 (18) | O12v—Na1—Na2ii | 135.04 (6) |
Zn—O21—Na2 | 98.66 (9) | O12—Na1—Na2ii | 44.96 (6) |
O22—C21—O21 | 122.9 (3) | O11iv—Na1—Na2ii | 104.65 (5) |
O22—C21—C22 | 122.0 (3) | O11i—Na1—Na2ii | 75.35 (5) |
O21—C21—C22 | 115.1 (3) | C11i—Na1—Na2ii | 55.58 (6) |
C21—O22—Na1i | 138.6 (2) | C11iv—Na1—Na2ii | 124.42 (6) |
C21—O22—Na2iii | 122.86 (18) | Znv—Na1—Na2ii | 99.50 (2) |
Na1i—O22—Na2iii | 95.52 (8) | Zn—Na1—Na2ii | 80.50 (2) |
O12—C11—O11 | 124.5 (3) | O22iv—Na1—Na2vi | 136.74 (6) |
O12—C11—C12 | 119.9 (3) | O22i—Na1—Na2vi | 43.26 (6) |
O11—C11—C12 | 115.6 (3) | O12v—Na1—Na2vi | 44.96 (6) |
O12—C11—Na1i | 110.52 (19) | O12—Na1—Na2vi | 135.04 (6) |
O11—C11—Na1i | 48.34 (14) | O11iv—Na1—Na2vi | 75.35 (5) |
C12—C11—Na1i | 107.8 (2) | O11i—Na1—Na2vi | 104.65 (5) |
C21—C22—C23 | 109.8 (3) | C11i—Na1—Na2vi | 124.42 (6) |
C13—C12—C11 | 113.1 (3) | C11iv—Na1—Na2vi | 55.58 (6) |
C24—C23—C22 | 114.3 (4) | Znv—Na1—Na2vi | 80.50 (2) |
C23—C24—C25 | 113.0 (5) | Zn—Na1—Na2vi | 99.50 (2) |
C12—C13—C14 | 113.2 (5) | Na2ii—Na1—Na2vi | 180.0 |
C15—C14—C13 | 115.9 (6) | O22vii—Na2—O22iii | 165.85 (12) |
C26—C25—C24 | 112.6 (6) | O22vii—Na2—O21 | 109.85 (8) |
C14—C15—C16 | 113.4 (9) | O22iii—Na2—O21 | 82.08 (8) |
O22iv—Na1—O22i | 180.0 | O22vii—Na2—O21i | 82.08 (8) |
O22iv—Na1—O12v | 94.54 (8) | O22iii—Na2—O21i | 109.85 (8) |
O22i—Na1—O12v | 85.46 (8) | O21—Na2—O21i | 70.18 (10) |
O22iv—Na1—O12 | 85.46 (8) | O22vii—Na2—O12viii | 80.33 (8) |
O22i—Na1—O12 | 94.54 (8) | O22iii—Na2—O12viii | 89.02 (8) |
O12v—Na1—O12 | 180.0 | O21—Na2—O12viii | 167.24 (8) |
O22iv—Na1—O11iv | 88.96 (7) | O21i—Na2—O12viii | 104.71 (7) |
O22i—Na1—O11iv | 91.04 (7) | O22vii—Na2—O12ix | 89.02 (8) |
O12v—Na1—O11iv | 85.19 (7) | O22iii—Na2—O12ix | 80.33 (8) |
O12—Na1—O11iv | 94.81 (7) | O21—Na2—O12ix | 104.71 (7) |
O22iv—Na1—O11i | 91.04 (7) | O21i—Na2—O12ix | 167.24 (8) |
O22i—Na1—O11i | 88.96 (7) | O12viii—Na2—O12ix | 82.63 (11) |
O12v—Na1—O11i | 94.81 (7) | O22vii—Na2—Na1viii | 41.23 (5) |
O12—Na1—O11i | 85.19 (7) | O22iii—Na2—Na1viii | 125.65 (7) |
O11iv—Na1—O11i | 180.0 | O21—Na2—Na1viii | 150.17 (6) |
O22iv—Na1—C11i | 68.79 (8) | O21i—Na2—Na1viii | 104.87 (5) |
O22i—Na1—C11i | 111.21 (8) | O12viii—Na2—Na1viii | 41.62 (6) |
O12v—Na1—C11i | 101.18 (8) | O12ix—Na2—Na1viii | 73.48 (7) |
O12—Na1—C11i | 78.82 (8) | O22vii—Na2—Na1ix | 125.65 (7) |
O11iv—Na1—C11i | 157.15 (7) | O22iii—Na2—Na1ix | 41.23 (5) |
O11i—Na1—C11i | 22.85 (7) | O21—Na2—Na1ix | 104.87 (5) |
O22iv—Na1—C11iv | 111.21 (8) | O21i—Na2—Na1ix | 150.17 (6) |
O22i—Na1—C11iv | 68.79 (8) | O12viii—Na2—Na1ix | 73.48 (7) |
O12v—Na1—C11iv | 78.82 (8) | O12ix—Na2—Na1ix | 41.62 (6) |
O12—Na1—C11iv | 101.18 (8) | Na1viii—Na2—Na1ix | 93.23 (4) |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) x, y−1, z; (iii) −x+1, −y+1, −z+1; (iv) x, −y, z+1/2; (v) −x+1, −y, −z+2; (vi) −x+1, −y+1, −z+2; (vii) x, −y+1, z+1/2; (viii) x, y+1, z; (ix) −x+1, y+1, −z+3/2. |
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