Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803029234/ww6150sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803029234/ww6150Isup2.hkl |
CCDC reference: 220265
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- H-atom completeness 51%
- R factor = 0.038
- wR factor = 0.093
- Data-to-parameter ratio = 9.2
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O3W PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O4W
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O4W = 2.68 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O2W .. O3W = 2.64 Ang.
Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 361.60 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 10.00 120.11 H 1.01 8.00 8.06 O 16.00 10.00 159.99 Zn 65.39 1.00 65.39 Calculated formula weight 353.55 REFNR01_ALERT_3_C Ratio of reflections to parameters is < 10 for a non-centrosymmetric structure, where ZMAX > 18 sine(theta)/lambda 0.6492 Proportion of unique data used 0.9203 Ratio reflections to parameters 9.1737 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 361.60 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.69 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O3 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O4 PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.18 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT430_ALERT_2_C Short Inter D...A Contact O3W .. O6 = 2.87 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact O4W .. O6 = 2.85 Ang. PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ ! PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ ! PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ ! PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ ! PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ ! PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C10 H16 O10 Zn1 Atom count from the _atom_site data: C10 H8 O10 Zn1 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C10 H16 O10 Zn TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 40.00 40.00 0.00 H 64.00 32.00 32.00 O 40.00 40.00 0.00 Zn 4.00 4.00 0.00 REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 27.48 From the CIF: _reflns_number_total 1894 Count of symmetry unique reflns 1749 Completeness (_total/calc) 108.29% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 145 Fraction of Friedel pairs measured 0.083 Are heavy atom types Z>Si present yes
2 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 20 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 12 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 7 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.
[Zn(C10H8O6)(H2O)2]·2H2O | Dx = 1.731 Mg m−3 |
Mr = 361.60 | Melting point: not measured K |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 12865 reflections |
a = 8.604 (2) Å | θ = 3.5–27.4° |
b = 27.271 (6) Å | µ = 1.82 mm−1 |
c = 5.914 (1) Å | T = 293 K |
V = 1387.7 (5) Å3 | Sheet, colorless |
Z = 4 | 0.24 × 0.14 × 0.08 mm |
F(000) = 744 |
Rigaku R-AXIS RAPID diffractometer | 1894 independent reflections |
Radiation source: fine-focus sealed tube | 1329 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
Detector resolution: 10.000 pixels mm-1 | θmax = 27.5°, θmin = 3.3° |
ω scans | h = 0→11 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = 0→35 |
Tmin = 0.669, Tmax = 0.868 | l = 0→7 |
13514 measured reflections |
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)] = 0.038 | H-atom parameters constrained |
wR(F2) = 0.093 | w = 1/[σ2(Fo2) + (0.0591P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max = 0.001 |
1743 reflections | Δρmax = 1.15 e Å−3 |
190 parameters | Δρmin = −0.31 e Å−3 |
1 restraint | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.07 (3) |
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 | ||
Zn1 | 0.33986 (7) | 0.595051 (17) | 0.21902 (16) | 0.03328 (17) | |
O1 | 0.4292 (5) | 0.64105 (13) | 0.4354 (7) | 0.0365 (10) | |
O2 | 0.5326 (5) | 0.57999 (13) | 0.6328 (7) | 0.0401 (10) | |
O3 | 0.6805 (5) | 0.64030 (13) | 0.9048 (8) | 0.0462 (12) | |
O4 | 1.0172 (5) | 0.64130 (13) | 1.5185 (7) | 0.0488 (12) | |
O5 | 1.2569 (5) | 0.64131 (13) | 2.0007 (7) | 0.0346 (9) | |
O6 | 1.1441 (4) | 0.58064 (13) | 1.8075 (7) | 0.0392 (10) | |
O1W | 0.1770 (5) | 0.55237 (14) | 0.3504 (8) | 0.0455 (11) | |
O2W | 0.4861 (5) | 0.54992 (13) | 0.0791 (8) | 0.0463 (11) | |
O3W | 0.7430 (6) | 0.51800 (14) | 0.2754 (9) | 0.0612 (14) | |
O4W | 0.1595 (4) | 0.45763 (12) | 0.2333 (15) | 0.0527 (10) | |
C1 | 0.5126 (6) | 0.62376 (19) | 0.5932 (9) | 0.0314 (12) | |
C2 | 0.5891 (6) | 0.66310 (17) | 0.7405 (14) | 0.0293 (11) | |
H2A | 0.6531 | 0.6843 | 0.6475 | 0.035* | |
H2B | 0.5098 | 0.6830 | 0.8124 | 0.035* | |
C3 | 0.7584 (6) | 0.66886 (19) | 1.0566 (10) | 0.0281 (12) | |
C4 | 0.7537 (6) | 0.71957 (18) | 1.0605 (10) | 0.0346 (13) | |
H4 | 0.6936 | 0.7367 | 0.9563 | 0.042* | |
C5 | 0.8400 (6) | 0.74457 (15) | 1.2225 (18) | 0.0379 (10) | |
H5 | 0.8370 | 0.7787 | 1.2250 | 0.045* | |
C6 | 0.9289 (6) | 0.72054 (18) | 1.3773 (11) | 0.0336 (13) | |
H6 | 0.9856 | 0.7379 | 1.4847 | 0.040* | |
C7 | 0.9331 (6) | 0.66971 (19) | 1.3717 (10) | 0.0308 (12) | |
C8 | 0.8491 (6) | 0.64395 (15) | 1.2104 (16) | 0.0302 (10) | |
H8A | 0.8540 | 0.6099 | 1.2061 | 0.036* | |
C9 | 1.0997 (6) | 0.66450 (17) | 1.6983 (13) | 0.0299 (13) | |
H9A | 1.0295 | 0.6846 | 1.7871 | 0.036* | |
H9B | 1.1808 | 0.6854 | 1.6377 | 0.036* | |
C10 | 1.1700 (6) | 0.62504 (18) | 1.8444 (9) | 0.0276 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.0433 (3) | 0.0303 (2) | 0.0262 (2) | −0.0025 (3) | −0.0106 (4) | 0.0015 (5) |
O1 | 0.045 (2) | 0.035 (2) | 0.030 (2) | −0.0026 (18) | −0.020 (2) | 0.002 (2) |
O2 | 0.049 (2) | 0.0308 (17) | 0.041 (2) | 0.0043 (18) | −0.017 (2) | −0.0034 (18) |
O3 | 0.062 (3) | 0.0276 (18) | 0.049 (3) | 0.0016 (19) | −0.042 (3) | −0.002 (2) |
O4 | 0.070 (3) | 0.0308 (18) | 0.046 (3) | 0.007 (2) | −0.043 (3) | −0.006 (2) |
O5 | 0.039 (2) | 0.0360 (19) | 0.029 (2) | −0.0052 (19) | −0.017 (2) | 0.003 (2) |
O6 | 0.047 (2) | 0.0302 (16) | 0.040 (2) | −0.0001 (18) | −0.017 (2) | 0.0006 (17) |
O1W | 0.056 (3) | 0.041 (2) | 0.040 (2) | −0.012 (2) | 0.013 (2) | −0.005 (2) |
O2W | 0.046 (2) | 0.042 (2) | 0.051 (3) | 0.006 (2) | 0.003 (2) | 0.003 (2) |
O3W | 0.074 (3) | 0.048 (2) | 0.061 (4) | 0.017 (2) | −0.004 (3) | 0.010 (2) |
O4W | 0.0424 (19) | 0.0421 (17) | 0.074 (3) | −0.0017 (18) | −0.001 (3) | −0.005 (4) |
C1 | 0.025 (3) | 0.043 (3) | 0.026 (3) | −0.002 (2) | −0.003 (3) | −0.004 (3) |
C2 | 0.031 (2) | 0.031 (2) | 0.026 (3) | −0.0001 (19) | −0.012 (3) | 0.002 (3) |
C3 | 0.028 (3) | 0.027 (2) | 0.029 (3) | 0.001 (2) | −0.013 (3) | −0.001 (2) |
C4 | 0.036 (3) | 0.031 (3) | 0.037 (3) | 0.003 (2) | −0.015 (3) | 0.004 (3) |
C5 | 0.045 (3) | 0.0244 (18) | 0.044 (2) | 0.001 (2) | −0.012 (4) | −0.007 (5) |
C6 | 0.042 (3) | 0.026 (2) | 0.033 (3) | −0.007 (2) | −0.012 (3) | −0.006 (2) |
C7 | 0.033 (3) | 0.032 (2) | 0.027 (3) | 0.003 (2) | −0.010 (3) | 0.005 (2) |
C8 | 0.037 (2) | 0.0237 (17) | 0.030 (2) | 0.000 (2) | −0.011 (3) | −0.008 (4) |
C9 | 0.031 (2) | 0.029 (2) | 0.029 (3) | 0.0026 (19) | −0.014 (3) | −0.006 (3) |
C10 | 0.025 (3) | 0.036 (3) | 0.022 (3) | 0.000 (2) | −0.005 (3) | 0.001 (2) |
Zn1—O5i | 1.941 (4) | C2—H2B | 0.9700 |
Zn1—O2W | 1.945 (4) | C3—C8 | 1.377 (9) |
Zn1—O1 | 1.950 (4) | C3—C4 | 1.384 (7) |
Zn1—O1W | 1.981 (4) | C4—C5 | 1.391 (9) |
O1—C1 | 1.268 (6) | C4—H4 | 0.9300 |
O2—C1 | 1.228 (6) | C5—C6 | 1.361 (10) |
O3—C3 | 1.364 (6) | C5—H5 | 0.9300 |
O3—C2 | 1.397 (8) | C6—C7 | 1.387 (7) |
O4—C7 | 1.370 (6) | C6—H6 | 0.9300 |
O4—C9 | 1.427 (7) | C7—C8 | 1.388 (9) |
O5—C10 | 1.269 (6) | C8—H8A | 0.9300 |
O5—Zn1ii | 1.941 (4) | C9—C10 | 1.507 (8) |
O6—C10 | 1.250 (6) | C9—H9A | 0.9700 |
C1—C2 | 1.531 (8) | C9—H9B | 0.9700 |
C2—H2A | 0.9700 | ||
O5i—Zn1—O2W | 111.5 (2) | C3—C4—H4 | 120.5 |
O5i—Zn1—O1 | 99.4 (1) | C5—C4—H4 | 120.5 |
O2W—Zn1—O1 | 115.5 (2) | C6—C5—C4 | 121.8 (4) |
O5i—Zn1—O1W | 112.5 (2) | C6—C5—H5 | 119.1 |
O2W—Zn1—O1W | 104.7 (2) | C4—C5—H5 | 119.1 |
O1—Zn1—O1W | 113.6 (2) | C5—C6—C7 | 118.7 (5) |
C1—O1—Zn1 | 117.8 (3) | C5—C6—H6 | 120.7 |
C3—O3—C2 | 118.7 (4) | C7—C6—H6 | 120.7 |
C7—O4—C9 | 119.0 (4) | O4—C7—C6 | 124.3 (5) |
C10—O5—Zn1ii | 118.3 (3) | O4—C7—C8 | 115.1 (5) |
O2—C1—O1 | 125.5 (5) | C6—C7—C8 | 120.5 (5) |
O2—C1—C2 | 120.8 (5) | C3—C8—C7 | 120.0 (4) |
O1—C1—C2 | 113.7 (4) | C3—C8—H8A | 120.0 |
O3—C2—C1 | 109.0 (4) | C7—C8—H8A | 120.0 |
O3—C2—H2A | 109.9 | O4—C9—C10 | 108.1 (4) |
C1—C2—H2A | 109.9 | O4—C9—H9A | 110.1 |
O3—C2—H2B | 109.9 | C10—C9—H9A | 110.1 |
C1—C2—H2B | 109.9 | O4—C9—H9B | 110.1 |
H2A—C2—H2B | 108.3 | C10—C9—H9B | 110.1 |
O3—C3—C8 | 115.5 (5) | H9A—C9—H9B | 108.4 |
O3—C3—C4 | 124.5 (5) | O6—C10—O5 | 124.8 (5) |
C8—C3—C4 | 119.9 (5) | O6—C10—C9 | 121.3 (5) |
C3—C4—C5 | 119.1 (5) | O5—C10—C9 | 113.8 (4) |
O5i—Zn1—O1—C1 | −171.5 (4) | C9—O4—C7—C6 | 3.7 (9) |
O2W—Zn1—O1—C1 | −52.2 (5) | C9—O4—C7—C8 | −176.3 (6) |
O1W—Zn1—O1—C1 | 68.8 (4) | C5—C6—C7—O4 | −179.7 (6) |
Zn1—O1—C1—O2 | −6.1 (8) | C5—C6—C7—C8 | 0.4 (10) |
Zn1—O1—C1—C2 | 174.7 (4) | O3—C3—C8—C7 | 179.9 (6) |
C3—O3—C2—C1 | −179.4 (5) | C4—C3—C8—C7 | 1.3 (10) |
O2—C1—C2—O3 | 2.1 (8) | O4—C7—C8—C3 | 178.9 (5) |
O1—C1—C2—O3 | −178.7 (5) | C6—C7—C8—C3 | −1.1 (10) |
C2—O3—C3—C8 | −178.5 (6) | C7—O4—C9—C10 | 175.2 (5) |
C2—O3—C3—C4 | 0.0 (9) | Zn1ii—O5—C10—O6 | −6.6 (8) |
O3—C3—C4—C5 | −179.2 (6) | Zn1ii—O5—C10—C9 | 174.4 (4) |
C8—C3—C4—C5 | −0.7 (9) | O4—C9—C10—O6 | −4.3 (8) |
C3—C4—C5—C6 | −0.1 (11) | O4—C9—C10—O5 | 174.7 (4) |
C4—C5—C6—C7 | 0.2 (11) |
Symmetry codes: (i) x−1, y, z−2; (ii) x+1, y, z+2. |