Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401668X/ci6390sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680401668X/ci6390Isup2.hkl |
CCDC reference: 248748
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.007 Å
- R factor = 0.060
- wR factor = 0.163
- Data-to-parameter ratio = 15.9
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 ............ 0.33 Ratio PLAT301_ALERT_3_C Main Residue Disorder ......................... 11.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C1 - C2 ... 1.56 Ang. PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C6 - C6_b ... 1.56 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O8 .. C1 .. 3.01 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O10 .. C2 .. 3.01 Ang.
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C4 H12 N2 O6 Zn1 Atom count from _chemical_formula_moiety:C4 H12 N6 O6 Zn1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 2002); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXTL.
[Zn(C2O4)(C2H8N2)]·2H2O | F(000) = 1536 |
Mr = 249.53 | Dx = 1.837 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 20214 reflections |
a = 25.757 (5) Å | θ = 2.9–27.6° |
b = 9.053 (3) Å | µ = 2.73 mm−1 |
c = 11.623 (2) Å | T = 173 K |
β = 93.05 (3)° | Prism, colorless |
V = 2706.4 (11) Å3 | 0.20 × 0.12 × 0.10 mm |
Z = 12 |
Nonius KappaCCD area-detector diffractometer | 3121 independent reflections |
Radiation source: fine-focus sealed tube | 2425 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
φ and ω scans | θmax = 27.6°, θmin = 2.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −33→33 |
Tmin = 0.606, Tmax = 0.764 | k = −11→11 |
20214 measured reflections | l = −14→15 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.060 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.163 | H-atom parameters constrained |
S = 1.23 | w = 1/[σ2(Fo2) + (0.0528P)2 + 25.3123P] where P = (Fo2 + 2Fc2)/3 |
3121 reflections | (Δ/σ)max = 0.001 |
196 parameters | Δρmax = 1.47 e Å−3 |
66 restraints | Δρmin = −2.17 e Å−3 |
Experimental. A crystal was selected for the X–ray measurements and mounted to the glass fiber using the oil drop method (Kottke & Stalke, 1993) and data were collected at 193 K. The intensity data were corrected for Lorentz and polarization effects and for absorption. one of the ethylenediamine ligands was found to be disordered and was refined in two positions with population parameter 0.5. The positional and atomic displacement factors of nitrogen N1A and N1B and N2A and N2B, respectively, of the disordered ethylenediammine ligand were fixed to be the same. N1A and N1B, as well as, N2A and N2B, effectively act as single nitrogen atom. The reason for this model is to model the hydrogen atoms at these N atoms correctly. |
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) | |
Zn1 | 0.33312 (2) | 0.07555 (6) | 0.57783 (4) | 0.01721 (19) | |
Zn2 | 0.5000 | 0.41017 (7) | 0.7500 | 0.0166 (2) | |
O1 | 0.35169 (12) | 0.2426 (3) | 0.7054 (3) | 0.0177 (7) | |
O2 | 0.41333 (13) | 0.1046 (4) | 0.5592 (3) | 0.0223 (7) | |
C1 | 0.39860 (17) | 0.2815 (4) | 0.7083 (4) | 0.0140 (8) | |
C2 | 0.43456 (17) | 0.2014 (5) | 0.6244 (4) | 0.0153 (8) | |
O3 | 0.41929 (12) | 0.3791 (3) | 0.7723 (3) | 0.0187 (7) | |
O4 | 0.48126 (12) | 0.2378 (3) | 0.6277 (3) | 0.0172 (6) | |
N1 | 0.34208 (16) | −0.1042 (4) | 0.6935 (3) | 0.0192 (8) | |
H11A | 0.3703 | −0.0919 | 0.7446 | 0.023* | 0.50 |
H12A | 0.3127 | −0.1197 | 0.7334 | 0.023* | 0.50 |
H11B | 0.3766 | −0.1124 | 0.7172 | 0.023* | 0.50 |
H12B | 0.3237 | −0.0849 | 0.7575 | 0.023* | 0.50 |
C3A | 0.3121 (4) | −0.2192 (10) | 0.5056 (7) | 0.0154 (17) | 0.50 |
H31A | 0.3154 | −0.3047 | 0.4533 | 0.019* | 0.50 |
H32A | 0.2763 | −0.2167 | 0.5322 | 0.019* | 0.50 |
C4A | 0.3510 (4) | −0.2300 (9) | 0.6062 (8) | 0.0143 (16) | 0.50 |
H41A | 0.3866 | −0.2230 | 0.5788 | 0.017* | 0.50 |
H42A | 0.3474 | −0.3268 | 0.6446 | 0.017* | 0.50 |
N2 | 0.32348 (18) | −0.0895 (4) | 0.4501 (4) | 0.0249 (9) | |
H21A | 0.2968 | −0.0647 | 0.3979 | 0.030* | 0.50 |
H22A | 0.3535 | −0.0998 | 0.4112 | 0.030* | 0.50 |
H21B | 0.2893 | −0.0970 | 0.4235 | 0.030* | 0.50 |
H22B | 0.3438 | −0.0709 | 0.3890 | 0.030* | 0.50 |
C3B | 0.3246 (4) | −0.2433 (9) | 0.6441 (7) | 0.0154 (17) | 0.50 |
H31B | 0.2863 | −0.2510 | 0.6433 | 0.018* | 0.50 |
H32B | 0.3400 | −0.3273 | 0.6885 | 0.018* | 0.50 |
C4B | 0.3432 (4) | −0.2425 (9) | 0.5217 (7) | 0.0156 (17) | 0.50 |
H41B | 0.3294 | −0.3307 | 0.4800 | 0.019* | 0.50 |
H42B | 0.3816 | −0.2479 | 0.5245 | 0.019* | 0.50 |
O5 | 0.25265 (12) | 0.1034 (4) | 0.5992 (3) | 0.0206 (7) | |
N3 | 0.51433 (18) | 0.5843 (5) | 0.8701 (4) | 0.0309 (10) | |
H31 | 0.5432 | 0.5651 | 0.9012 | 0.037* | |
H32 | 0.4892 | 0.5992 | 0.9233 | 0.037* | |
C5 | 0.5211 (2) | 0.7224 (6) | 0.7996 (5) | 0.0293 (11) | |
H5A | 0.5561 | 0.7238 | 0.7682 | 0.035* | |
H5B | 0.5175 | 0.8111 | 0.8484 | 0.035* | |
O6 | 0.31469 (12) | 0.2532 (4) | 0.4600 (3) | 0.0235 (7) | |
C6 | 0.26805 (18) | 0.2933 (5) | 0.4599 (4) | 0.0189 (9) | |
O8 | 0.43549 (12) | 0.0229 (3) | 0.8530 (3) | 0.0186 (7) | |
H81 | 0.4626 | 0.0741 | 0.8521 | 0.028* | |
H82 | 0.4332 | −0.0212 | 0.9190 | 0.028* | |
O9 | 0.26722 (17) | 0.4462 (6) | 0.7070 (4) | 0.0626 (17) | |
H91 | 0.2674 | 0.4962 | 0.7676 | 0.094* | |
H92 | 0.2959 | 0.4047 | 0.6974 | 0.094* | |
O10 | 0.09839 (15) | 0.0553 (5) | 0.5403 (4) | 0.0466 (12) | |
H102 | 0.1270 | 0.1003 | 0.5409 | 0.070* | |
H101 | 0.1035 | 0.0096 | 0.6031 | 0.070* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.0135 (3) | 0.0204 (3) | 0.0175 (3) | −0.00060 (18) | −0.00122 (19) | −0.00589 (19) |
Zn2 | 0.0127 (4) | 0.0087 (3) | 0.0280 (4) | 0.000 | −0.0011 (3) | 0.000 |
O1 | 0.0154 (16) | 0.0143 (14) | 0.0232 (16) | −0.0014 (12) | 0.0002 (12) | −0.0041 (12) |
O2 | 0.0166 (16) | 0.0294 (17) | 0.0207 (17) | −0.0019 (13) | −0.0004 (13) | −0.0146 (14) |
C1 | 0.0140 (11) | 0.0135 (11) | 0.0145 (11) | 0.0004 (9) | 0.0006 (9) | 0.0000 (9) |
C2 | 0.0153 (12) | 0.0152 (11) | 0.0155 (11) | 0.0008 (9) | 0.0003 (9) | −0.0002 (9) |
O3 | 0.0155 (15) | 0.0134 (14) | 0.0272 (17) | −0.0012 (12) | 0.0016 (13) | −0.0065 (13) |
O4 | 0.0122 (15) | 0.0193 (15) | 0.0200 (16) | 0.0008 (12) | 0.0007 (12) | −0.0041 (12) |
N1 | 0.0196 (10) | 0.0186 (10) | 0.0193 (10) | 0.0000 (7) | −0.0016 (7) | −0.0020 (7) |
C3A | 0.0163 (19) | 0.0157 (19) | 0.0143 (19) | −0.0003 (10) | −0.0001 (10) | −0.0001 (10) |
C4A | 0.0151 (18) | 0.0143 (18) | 0.0136 (18) | 0.0003 (10) | −0.0004 (10) | −0.0008 (10) |
N2 | 0.0257 (12) | 0.0272 (12) | 0.0222 (12) | −0.0029 (9) | 0.0033 (9) | −0.0020 (9) |
C3B | 0.016 (2) | 0.015 (2) | 0.015 (2) | −0.0015 (18) | −0.0026 (18) | 0.0012 (18) |
C4B | 0.018 (5) | 0.012 (4) | 0.017 (4) | 0.005 (3) | 0.000 (3) | −0.003 (3) |
O5 | 0.0152 (16) | 0.0262 (16) | 0.0205 (16) | −0.0002 (13) | 0.0017 (13) | 0.0009 (13) |
N3 | 0.0283 (13) | 0.0298 (13) | 0.0346 (13) | 0.0021 (9) | 0.0020 (9) | −0.0055 (9) |
C5 | 0.0270 (14) | 0.0267 (14) | 0.0344 (14) | −0.0005 (9) | 0.0023 (10) | −0.0021 (9) |
O6 | 0.0122 (16) | 0.0351 (19) | 0.0233 (17) | −0.0011 (14) | 0.0009 (13) | 0.0049 (15) |
C6 | 0.0184 (12) | 0.0202 (12) | 0.0182 (12) | −0.0005 (9) | 0.0007 (9) | −0.0005 (9) |
O8 | 0.0227 (17) | 0.0204 (16) | 0.0126 (15) | −0.0054 (13) | 0.0000 (12) | 0.0007 (12) |
O9 | 0.032 (2) | 0.087 (4) | 0.066 (3) | 0.029 (2) | −0.022 (2) | −0.057 (3) |
O10 | 0.021 (2) | 0.066 (3) | 0.051 (3) | −0.0101 (19) | −0.0055 (18) | 0.039 (2) |
Zn1—O2 | 2.105 (3) | C4A—H42A | 0.99 |
Zn1—N2 | 2.112 (4) | N2—H21A | 0.92 |
Zn1—N1 | 2.116 (4) | N2—H22A | 0.92 |
Zn1—O5 | 2.116 (3) | C3B—C4B | 1.524 (12) |
Zn1—O6 | 2.149 (3) | C3B—H31B | 0.99 |
Zn1—O1 | 2.154 (3) | C3B—H32B | 0.99 |
Zn2—N3 | 2.124 (4) | C4B—H41B | 0.99 |
Zn2—N3i | 2.124 (4) | C4B—H42B | 0.99 |
Zn2—O3 | 2.127 (3) | O5—C6ii | 1.262 (6) |
Zn2—O3i | 2.127 (3) | N3—C5 | 1.510 (7) |
Zn2—O4 | 2.148 (3) | N3—H31 | 0.83 |
Zn2—O4i | 2.148 (3) | N3—H32 | 0.93 |
O1—C1 | 1.257 (5) | C5—C5i | 1.543 (10) |
O2—C2 | 1.264 (5) | C5—H5A | 0.99 |
C1—O3 | 1.255 (5) | C5—H5B | 0.99 |
C1—C2 | 1.559 (6) | O6—C6 | 1.255 (6) |
C2—O4 | 1.246 (5) | C6—O5ii | 1.262 (6) |
N1—C4A | 1.549 (9) | C6—C6ii | 1.562 (9) |
N1—H11A | 0.92 | O8—H81 | 0.84 |
N1—H12A | 0.92 | O8—H82 | 0.87 |
C3A—N2 | 1.379 (9) | O9—H91 | 0.84 |
C3A—C4A | 1.501 (12) | O9—H92 | 0.84 |
C3A—H31A | 0.99 | O10—H102 | 0.84 |
C3A—H32A | 0.99 | O10—H101 | 0.84 |
C4A—H41A | 0.99 | ||
O2—Zn1—N2 | 95.48 (15) | H11A—N1—H12A | 109.6 |
O2—Zn1—N1 | 95.00 (15) | N2—C3A—C4A | 105.7 (7) |
N2—Zn1—N1 | 84.68 (16) | N2—C3A—H31A | 110.6 |
O2—Zn1—O5 | 165.94 (14) | C4A—C3A—H31A | 110.6 |
N2—Zn1—O5 | 95.03 (16) | N2—C3A—H32A | 110.6 |
N1—Zn1—O5 | 95.25 (15) | C4A—C3A—H32A | 110.6 |
O2—Zn1—O6 | 91.47 (13) | H31A—C3A—H32A | 108.7 |
N2—Zn1—O6 | 93.88 (15) | C3A—C4A—N1 | 110.3 (7) |
N1—Zn1—O6 | 173.48 (14) | C3A—C4A—H41A | 109.6 |
O5—Zn1—O6 | 78.53 (13) | N1—C4A—H41A | 109.6 |
O2—Zn1—O1 | 78.45 (12) | C3A—C4A—H42A | 109.6 |
N2—Zn1—O1 | 173.90 (15) | N1—C4A—H42A | 109.6 |
N1—Zn1—O1 | 95.17 (14) | H41A—C4A—H42A | 108.1 |
O5—Zn1—O1 | 91.05 (13) | C3A—N2—Zn1 | 107.1 (4) |
O6—Zn1—O1 | 86.94 (14) | C3A—N2—H21A | 110.3 |
N3—Zn2—N3i | 84.2 (3) | Zn1—N2—H21A | 110.3 |
N3—Zn2—O3 | 98.91 (15) | C3A—N2—H22A | 110.3 |
N3i—Zn2—O3 | 92.36 (16) | Zn1—N2—H22A | 110.3 |
N3—Zn2—O3i | 92.36 (16) | H21A—N2—H22A | 108.6 |
N3i—Zn2—O3i | 98.91 (15) | C4B—C3B—H31B | 110.7 |
O3—Zn2—O3i | 164.82 (17) | C4B—C3B—H32B | 110.7 |
N3—Zn2—O4 | 176.95 (15) | H31B—C3B—H32B | 108.8 |
N3i—Zn2—O4 | 94.54 (16) | C3B—C4B—H41B | 109.3 |
O3—Zn2—O4 | 78.34 (12) | C3B—C4B—H42B | 109.3 |
O3i—Zn2—O4 | 90.58 (12) | H41B—C4B—H42B | 108.0 |
N3—Zn2—O4i | 94.54 (16) | C6ii—O5—Zn1 | 114.4 (3) |
N3i—Zn2—O4i | 176.95 (15) | C5—N3—Zn2 | 106.2 (3) |
O3—Zn2—O4i | 90.58 (12) | C5—N3—H31 | 106.5 |
O3i—Zn2—O4i | 78.34 (12) | Zn2—N3—H31 | 104.6 |
O4—Zn2—O4i | 86.82 (17) | C5—N3—H32 | 110.2 |
C1—O1—Zn1 | 113.2 (3) | Zn2—N3—H32 | 116.3 |
C2—O2—Zn1 | 114.9 (3) | H31—N3—H32 | 112.4 |
O1—C1—O3 | 126.2 (4) | N3—C5—C5i | 107.9 (4) |
O1—C1—C2 | 117.0 (4) | N3—C5—H5A | 110.1 |
O3—C1—C2 | 116.8 (4) | C5i—C5—H5A | 110.1 |
O4—C2—O2 | 126.0 (4) | N3—C5—H5B | 110.1 |
O4—C2—C1 | 117.5 (4) | C5i—C5—H5B | 110.1 |
O2—C2—C1 | 116.4 (4) | H5A—C5—H5B | 108.4 |
C1—O3—Zn2 | 114.1 (3) | C6—O6—Zn1 | 113.3 (3) |
C2—O4—Zn2 | 113.3 (3) | O6—C6—O5ii | 126.3 (4) |
C4A—N1—Zn1 | 99.5 (4) | O6—C6—C6ii | 117.0 (5) |
C4A—N1—H11A | 111.9 | O5ii—C6—C6ii | 116.7 (5) |
Zn1—N1—H11A | 111.9 | H81—O8—H82 | 111.0 |
C4A—N1—H12A | 111.9 | H91—O9—H92 | 112.8 |
Zn1—N1—H12A | 111.9 | H102—O10—H101 | 97.7 |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) −x+1/2, −y+1/2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H11A···O8 | 0.92 | 2.29 | 3.174 (5) | 160 |
N1—H11B···O8 | 0.92 | 2.46 | 3.174 (5) | 135 |
N1—H12A···O9iii | 0.92 | 2.29 | 3.133 (6) | 153 |
N1—H12B···O9iii | 0.92 | 2.42 | 3.133 (6) | 135 |
N2—H21A···O9ii | 0.92 | 2.27 | 3.166 (7) | 165 |
N2—H21B···O9ii | 0.92 | 2.46 | 3.166 (7) | 134 |
N2—H22A···O8iv | 0.92 | 2.36 | 3.210 (6) | 154 |
N2—H22B···O8iv | 0.92 | 2.46 | 3.210 (6) | 139 |
N3—H31···O10v | 0.83 | 2.36 | 3.121 (6) | 153 |
N3—H32···O10vi | 0.93 | 2.35 | 3.147 (6) | 144 |
O8—H81···O4i | 0.84 | 2.08 | 2.895 (4) | 166 |
O8—H82···O2vii | 0.87 | 1.89 | 2.747 (5) | 168 |
O9—H91···O5vi | 0.84 | 1.92 | 2.736 (6) | 164 |
O9—H92···O1 | 0.84 | 2.05 | 2.852 (6) | 159 |
O10—H101···O3iii | 0.84 | 1.98 | 2.757 (6) | 152 |
O10—H102···O6ii | 0.84 | 2.00 | 2.832 (5) | 167 |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) −x+1/2, −y+1/2, −z+1; (iii) −x+1/2, y−1/2, −z+3/2; (iv) x, −y, z−1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) −x+1/2, y+1/2, −z+3/2; (vii) x, −y, z+1/2. |
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