Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807055237/bt2561sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807055237/bt2561Isup2.hkl |
CCDC reference: 672613
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.003 Å
- Disorder in solvent or counterion
- R factor = 0.027
- wR factor = 0.067
- Data-to-parameter ratio = 12.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H5W2 .. H6W2 .. 2.08 Ang.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.742 0.878 Tmin and Tmax expected: 0.659 0.875 RR = 1.122 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.12 PLAT145_ALERT_4_C su on beta Small or Missing (x 10000) ..... 1 Deg. PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 5 PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.46 Ratio PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 13 PLAT736_ALERT_1_C H...A Calc 1.93(3), Rep 1.930(10) ...... 3.00 su-Ra H6# -O2 1.555 1.465 PLAT736_ALERT_1_C H...A Calc 1.91(3), Rep 1.910(10) ...... 3.00 su-Ra H7# -O4 1.555 2.667 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H2 O
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 18
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
The reaction of zinc cations and (5-carboxylato-m-phenylenedioxy)diacetate trianions in water gives crystalline hexaaquazinc bis[[(5-carboxylato-m-phenylenedioxy)diacetato]triaquazincate] heptahydrate, whose anion exists as a carboxylate-bridged chain (Wen & Ng, 2007).
(5-Carboxy-m-phenylenedioxy)diacetic acid (0.282 g, 1 mol) and zinc nitrate hexahydrate (0.298 g, 1 mmol)) were mixed in 20 ml e thanol-water (1:1, v/v) solution. The pH value was adjusted to 7 by sodium carbonate solution. The filtered solution was set aside for the growth of crystals which appeared after a week.
In an earlier attempt, the filtered solution was set aside for a week for the growth of hexaaquazinc bis[(5-carboxylato-m-phenylenedioxy)diacetatotriaquazincate] heptahydrate (Wen & Ng, 2007). In the present study, the solution was kept at 278 K for two months to yield a compound of a different composition.
The water H-atoms were located in a difference Fourier map, and were refined with distance restraints of O–H 0.85 (1) Å and H···H 1.39 (1) Å); their temperature factors were freely refined. For the disordered lattce water molecule, hydrogen atoms were placed on the major component only. The carbon-bound H-atoms were generated geometrically (C–H 0.93 to 0.97 Å); they were included in the refinement in the riding model approximation, with U(H) set to 1.2Ueq(C).
Data collection: SMART (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
[Zn3(C11H7O8)2(H2O)10]·2H2O | Z = 1 |
Mr = 946.63 | F(000) = 484 |
Triclinic, P1 | Dx = 1.866 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.3125 (1) Å | Cell parameters from 5082 reflections |
b = 9.0935 (1) Å | θ = 2.6–27.2° |
c = 13.4543 (2) Å | µ = 2.23 mm−1 |
α = 79.271 (1)° | T = 295 K |
β = 82.6340 (1)° | Prism, colorless |
γ = 74.064 (1)° | 0.32 × 0.16 × 0.06 mm |
V = 842.42 (2) Å3 |
Bruker APEX-II area-detector diffractometer | 3858 independent reflections |
Radiation source: fine-focus sealed tube | 3176 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
ϕ and ω scans | θmax = 27.5°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.742, Tmax = 0.878 | k = −11→11 |
14462 measured reflections | l = −16→17 |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.067 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.032P)2 + 0.2695P] where P = (Fo2 + 2Fc2)/3 |
3858 reflections | (Δ/σ)max = 0.001 |
299 parameters | Δρmax = 0.42 e Å−3 |
18 restraints | Δρmin = −0.29 e Å−3 |
[Zn3(C11H7O8)2(H2O)10]·2H2O | γ = 74.064 (1)° |
Mr = 946.63 | V = 842.42 (2) Å3 |
Triclinic, P1 | Z = 1 |
a = 7.3125 (1) Å | Mo Kα radiation |
b = 9.0935 (1) Å | µ = 2.23 mm−1 |
c = 13.4543 (2) Å | T = 295 K |
α = 79.271 (1)° | 0.32 × 0.16 × 0.06 mm |
β = 82.6340 (1)° |
Bruker APEX-II area-detector diffractometer | 3858 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3176 reflections with I > 2σ(I) |
Tmin = 0.742, Tmax = 0.878 | Rint = 0.027 |
14462 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 18 restraints |
wR(F2) = 0.067 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 0.42 e Å−3 |
3858 reflections | Δρmin = −0.29 e Å−3 |
299 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Zn1 | 1.0000 | 0.0000 | 0.5000 | 0.02497 (9) | |
Zn2 | 0.25698 (3) | 0.73433 (3) | 0.898344 (17) | 0.02466 (8) | |
O1 | 0.9264 (2) | −0.15104 (16) | 0.61275 (10) | 0.0281 (3) | |
O2 | 0.7610 (2) | −0.19883 (17) | 0.75921 (11) | 0.0298 (3) | |
O3 | 0.7885 (2) | 0.15379 (15) | 0.60092 (10) | 0.0262 (3) | |
O4 | 0.4623 (2) | 0.54817 (17) | 0.84086 (10) | 0.0281 (3) | |
O5 | 0.3464 (2) | 0.75350 (16) | 0.73226 (11) | 0.0281 (3) | |
O6 | 0.7776 (2) | 0.65455 (16) | 0.41363 (10) | 0.0270 (3) | |
O7 | 0.8774 (3) | 0.83786 (18) | 0.25159 (12) | 0.0449 (5) | |
O8 | 0.9369 (2) | 0.65423 (17) | 0.15490 (11) | 0.0310 (4) | |
O1w | 0.7706 (2) | −0.00283 (19) | 0.42077 (12) | 0.0326 (4) | |
H1w1 | 0.741 (4) | 0.0793 (17) | 0.3784 (17) | 0.069 (10)* | |
H1w2 | 0.794 (5) | −0.0807 (19) | 0.3909 (19) | 0.080 (12)* | |
O2w | 0.0493 (2) | 0.94000 (19) | 0.89410 (14) | 0.0400 (4) | |
H2w1 | 0.066 (4) | 1.016 (2) | 0.8510 (17) | 0.062 (9)* | |
H2w2 | −0.061 (2) | 0.957 (3) | 0.922 (2) | 0.083 (12)* | |
O3w | 0.0360 (2) | 0.63529 (19) | 0.89035 (13) | 0.0331 (4) | |
H3w1 | 0.059 (3) | 0.5422 (12) | 0.8821 (18) | 0.044 (8)* | |
H3w2 | −0.042 (4) | 0.693 (2) | 0.8485 (19) | 0.070 (10)* | |
O4w | 0.2654 (3) | 0.6729 (2) | 1.05019 (12) | 0.0404 (4) | |
H4w1 | 0.355 (3) | 0.603 (3) | 1.079 (2) | 0.073 (10)* | |
H4w2 | 0.1602 (19) | 0.667 (3) | 1.0834 (18) | 0.054 (9)* | |
O5w | 0.4649 (2) | 0.8552 (2) | 0.89952 (12) | 0.0313 (4) | |
H5w1 | 0.550 (3) | 0.847 (3) | 0.8501 (12) | 0.047 (8)* | |
H5w2 | 0.520 (4) | 0.837 (4) | 0.9540 (11) | 0.090 (13)* | |
O6w | −0.2748 (4) | 0.8784 (3) | 1.0180 (2) | 0.0378 (10) | 0.671 (6) |
H6w1 | −0.223 (6) | 0.793 (3) | 1.054 (3) | 0.126 (17)* | |
H6w2 | −0.338 (7) | 0.941 (4) | 1.058 (3) | 0.17 (2)* | |
O6w' | −0.4015 (10) | 0.8303 (8) | 1.0841 (6) | 0.062 (3) | 0.329 (6) |
C1 | 0.8089 (3) | −0.1096 (2) | 0.68481 (15) | 0.0223 (4) | |
C2 | 0.7164 (3) | 0.0612 (2) | 0.68664 (16) | 0.0297 (5) | |
H2A | 0.5793 | 0.0811 | 0.6859 | 0.036* | |
H2B | 0.7422 | 0.0892 | 0.7486 | 0.036* | |
C3 | 0.7317 (3) | 0.3135 (2) | 0.59859 (14) | 0.0204 (4) | |
C4 | 0.6293 (3) | 0.3834 (2) | 0.67841 (15) | 0.0220 (4) | |
H4 | 0.5972 | 0.3243 | 0.7389 | 0.026* | |
C5 | 0.5750 (3) | 0.5446 (2) | 0.66633 (15) | 0.0205 (4) | |
C6 | 0.6244 (3) | 0.6330 (2) | 0.57711 (14) | 0.0215 (4) | |
H6 | 0.5864 | 0.7405 | 0.5693 | 0.026* | |
C7 | 0.7317 (3) | 0.5591 (2) | 0.49913 (14) | 0.0210 (4) | |
C8 | 0.7852 (3) | 0.3998 (2) | 0.50908 (15) | 0.0219 (4) | |
H8 | 0.8562 | 0.3510 | 0.4564 | 0.026* | |
C9 | 0.4563 (3) | 0.6204 (2) | 0.75028 (14) | 0.0207 (4) | |
C10 | 0.8699 (3) | 0.5819 (2) | 0.32888 (15) | 0.0229 (4) | |
H10A | 0.7941 | 0.5190 | 0.3120 | 0.027* | |
H10B | 0.9937 | 0.5147 | 0.3458 | 0.027* | |
C11 | 0.8944 (3) | 0.7035 (2) | 0.23948 (15) | 0.0252 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.0323 (2) | 0.01893 (18) | 0.02016 (18) | −0.00585 (14) | 0.00617 (14) | −0.00096 (13) |
Zn2 | 0.02595 (14) | 0.02400 (14) | 0.02075 (13) | −0.00288 (10) | 0.00454 (10) | −0.00511 (10) |
O1 | 0.0366 (9) | 0.0184 (7) | 0.0240 (8) | −0.0050 (6) | 0.0098 (6) | −0.0014 (6) |
O2 | 0.0328 (9) | 0.0246 (8) | 0.0268 (8) | −0.0082 (7) | 0.0064 (6) | 0.0040 (6) |
O3 | 0.0374 (9) | 0.0147 (7) | 0.0220 (7) | −0.0049 (6) | 0.0101 (6) | −0.0030 (6) |
O4 | 0.0319 (8) | 0.0261 (8) | 0.0195 (7) | 0.0005 (6) | 0.0040 (6) | −0.0029 (6) |
O5 | 0.0313 (8) | 0.0226 (8) | 0.0239 (8) | 0.0038 (6) | 0.0003 (6) | −0.0055 (6) |
O6 | 0.0405 (9) | 0.0179 (7) | 0.0188 (7) | −0.0066 (6) | 0.0097 (6) | −0.0032 (6) |
O7 | 0.0838 (14) | 0.0222 (8) | 0.0266 (8) | −0.0166 (9) | 0.0076 (9) | −0.0024 (7) |
O8 | 0.0445 (10) | 0.0279 (8) | 0.0183 (7) | −0.0088 (7) | 0.0053 (7) | −0.0042 (6) |
O1w | 0.0403 (10) | 0.0250 (9) | 0.0313 (9) | −0.0059 (7) | −0.0043 (7) | −0.0042 (7) |
O2w | 0.0313 (10) | 0.0245 (9) | 0.0532 (11) | −0.0030 (7) | 0.0090 (8) | 0.0067 (8) |
O3w | 0.0348 (9) | 0.0224 (8) | 0.0419 (10) | −0.0070 (7) | −0.0044 (8) | −0.0042 (7) |
O4w | 0.0290 (9) | 0.0576 (12) | 0.0245 (8) | −0.0037 (9) | 0.0030 (7) | 0.0043 (8) |
O5w | 0.0289 (9) | 0.0415 (10) | 0.0262 (8) | −0.0127 (7) | 0.0045 (7) | −0.0112 (7) |
O6w | 0.0391 (17) | 0.0333 (16) | 0.0384 (17) | 0.0018 (12) | −0.0112 (13) | −0.0101 (13) |
O6w' | 0.065 (5) | 0.049 (4) | 0.074 (5) | 0.001 (3) | −0.031 (4) | −0.018 (4) |
C1 | 0.0242 (11) | 0.0210 (10) | 0.0212 (10) | −0.0068 (8) | −0.0014 (8) | −0.0011 (8) |
C2 | 0.0355 (13) | 0.0222 (11) | 0.0262 (11) | −0.0072 (9) | 0.0113 (9) | −0.0011 (9) |
C3 | 0.0224 (10) | 0.0157 (9) | 0.0213 (10) | −0.0019 (8) | 0.0000 (8) | −0.0042 (8) |
C4 | 0.0246 (10) | 0.0206 (10) | 0.0181 (10) | −0.0049 (8) | 0.0030 (8) | −0.0010 (8) |
C5 | 0.0207 (10) | 0.0199 (10) | 0.0199 (10) | −0.0024 (8) | −0.0008 (8) | −0.0059 (8) |
C6 | 0.0246 (10) | 0.0168 (10) | 0.0217 (10) | −0.0027 (8) | −0.0005 (8) | −0.0042 (8) |
C7 | 0.0237 (10) | 0.0205 (10) | 0.0178 (10) | −0.0061 (8) | 0.0013 (8) | −0.0019 (8) |
C8 | 0.0248 (10) | 0.0209 (10) | 0.0180 (10) | −0.0038 (8) | 0.0039 (8) | −0.0048 (8) |
C9 | 0.0219 (10) | 0.0208 (10) | 0.0205 (10) | −0.0062 (8) | 0.0016 (8) | −0.0068 (8) |
C10 | 0.0278 (11) | 0.0208 (10) | 0.0196 (10) | −0.0061 (8) | 0.0034 (8) | −0.0059 (8) |
C11 | 0.0296 (11) | 0.0220 (11) | 0.0223 (11) | −0.0062 (9) | 0.0012 (9) | −0.0019 (8) |
Zn1—O1 | 1.9744 (14) | O2w—H2w2 | 0.84 (1) |
Zn1—O1i | 1.9744 (14) | O3w—H3w1 | 0.84 (1) |
Zn1—O1w | 2.1078 (16) | O3w—H3w2 | 0.85 (3) |
Zn1—O1wi | 2.1078 (16) | O4w—H4w1 | 0.86 (3) |
Zn1—O3i | 2.2742 (14) | O4w—H4w2 | 0.85 (1) |
Zn1—O3 | 2.2742 (14) | O5w—H5w1 | 0.85 (1) |
Zn2—O4w | 2.0194 (16) | O5w—H5w2 | 0.85 (1) |
Zn2—O2w | 2.0566 (16) | O6w—H6w1 | 0.85 (1) |
Zn2—O3w | 2.0771 (16) | O6w—H6w2 | 0.86 (1) |
Zn2—O5w | 2.1091 (16) | C1—C2 | 1.518 (3) |
Zn2—O4 | 2.1242 (15) | C2—H2A | 0.9700 |
Zn2—O5 | 2.2347 (14) | C2—H2B | 0.9700 |
O1—C1 | 1.251 (2) | C3—C4 | 1.380 (3) |
O2—C1 | 1.244 (2) | C3—C8 | 1.384 (3) |
O3—C3 | 1.392 (2) | C4—C5 | 1.393 (3) |
O3—C2 | 1.429 (2) | C4—H4 | 0.9300 |
O4—C9 | 1.272 (2) | C5—C6 | 1.381 (3) |
O5—C9 | 1.255 (2) | C5—C9 | 1.488 (3) |
O6—C7 | 1.371 (2) | C6—C7 | 1.389 (3) |
O6—C10 | 1.425 (2) | C6—H6 | 0.9300 |
O7—C11 | 1.233 (3) | C7—C8 | 1.378 (3) |
O8—C11 | 1.271 (2) | C8—H8 | 0.9300 |
O1w—H1w1 | 0.85 (1) | C10—C11 | 1.503 (3) |
O1w—H1w2 | 0.85 (1) | C10—H10A | 0.9700 |
O2w—H2w1 | 0.84 (1) | C10—H10B | 0.9700 |
O1—Zn1—O1i | 180.0 | Zn2—O4w—H4w2 | 115.9 (18) |
O1—Zn1—O1w | 90.41 (6) | H4w1—O4w—H4w2 | 108.3 (15) |
O1i—Zn1—O1w | 89.59 (6) | Zn2—O5w—H5w1 | 114.5 (17) |
O1—Zn1—O1wi | 89.59 (6) | Zn2—O5w—H5w2 | 116 (2) |
O1i—Zn1—O1wi | 90.41 (6) | H5w1—O5w—H5w2 | 108.2 (15) |
O1w—Zn1—O1wi | 180.00 (7) | H6w1—O6w—H6w2 | 107.9 (17) |
O1—Zn1—O3i | 102.88 (5) | H6w1—O6w'—H6w2 | 67.6 (17) |
O1i—Zn1—O3i | 77.12 (5) | O2—C1—O1 | 124.92 (19) |
O1w—Zn1—O3i | 91.35 (6) | O2—C1—C2 | 115.08 (18) |
O1wi—Zn1—O3i | 88.65 (6) | O1—C1—C2 | 119.98 (17) |
O1—Zn1—O3 | 77.12 (5) | O3—C2—C1 | 110.61 (17) |
O1i—Zn1—O3 | 102.88 (5) | O3—C2—H2A | 109.5 |
O1w—Zn1—O3 | 88.65 (6) | C1—C2—H2A | 109.5 |
O1wi—Zn1—O3 | 91.35 (6) | O3—C2—H2B | 109.5 |
O3i—Zn1—O3 | 180.00 (5) | C1—C2—H2B | 109.5 |
O4w—Zn2—O2w | 99.31 (8) | H2A—C2—H2B | 108.1 |
O4w—Zn2—O3w | 94.63 (7) | C4—C3—C8 | 121.46 (18) |
O2w—Zn2—O3w | 85.62 (7) | C4—C3—O3 | 123.55 (18) |
O4w—Zn2—O5w | 88.50 (7) | C8—C3—O3 | 114.99 (17) |
O2w—Zn2—O5w | 89.36 (7) | C3—C4—C5 | 118.54 (18) |
O3w—Zn2—O5w | 174.46 (6) | C3—C4—H4 | 120.7 |
O4w—Zn2—O4 | 103.16 (7) | C5—C4—H4 | 120.7 |
O2w—Zn2—O4 | 157.52 (7) | C6—C5—C4 | 120.94 (18) |
O3w—Zn2—O4 | 91.76 (6) | C6—C5—C9 | 120.35 (18) |
O5w—Zn2—O4 | 91.97 (6) | C4—C5—C9 | 118.68 (18) |
O4w—Zn2—O5 | 161.01 (6) | C5—C6—C7 | 119.11 (18) |
O2w—Zn2—O5 | 97.82 (6) | C5—C6—H6 | 120.4 |
O3w—Zn2—O5 | 94.79 (6) | C7—C6—H6 | 120.4 |
O5w—Zn2—O5 | 83.55 (6) | O6—C7—C8 | 123.42 (17) |
O4—Zn2—O5 | 60.09 (5) | O6—C7—C6 | 115.68 (17) |
C1—O1—Zn1 | 121.99 (13) | C8—C7—C6 | 120.90 (18) |
C3—O3—C2 | 116.78 (15) | C7—C8—C3 | 119.02 (18) |
C3—O3—Zn1 | 132.71 (12) | C7—C8—H8 | 120.5 |
C2—O3—Zn1 | 110.27 (11) | C3—C8—H8 | 120.5 |
C9—O4—Zn2 | 92.45 (11) | O5—C9—O4 | 119.59 (18) |
C9—O5—Zn2 | 87.87 (12) | O5—C9—C5 | 120.62 (17) |
C7—O6—C10 | 116.56 (15) | O4—C9—C5 | 119.76 (17) |
Zn1—O1w—H1w1 | 110 (2) | O6—C10—C11 | 109.57 (17) |
Zn1—O1w—H1w2 | 113 (2) | O6—C10—H10A | 109.8 |
H1w1—O1w—H1w2 | 109.8 (16) | C11—C10—H10A | 109.8 |
Zn2—O2w—H2w1 | 118.4 (18) | O6—C10—H10B | 109.8 |
Zn2—O2w—H2w2 | 128.7 (19) | C11—C10—H10B | 109.8 |
H2w1—O2w—H2w2 | 111.9 (16) | H10A—C10—H10B | 108.2 |
Zn2—O3w—H3w1 | 120.8 (17) | O7—C11—O8 | 125.04 (19) |
Zn2—O3w—H3w2 | 111.1 (19) | O7—C11—C10 | 120.39 (19) |
H3w1—O3w—H3w2 | 109.7 (15) | O8—C11—C10 | 114.55 (18) |
Zn2—O4w—H4w1 | 124 (2) | ||
O1w—Zn1—O1—C1 | −88.19 (16) | Zn1—O3—C3—C4 | −166.41 (14) |
O1wi—Zn1—O1—C1 | 91.81 (16) | C2—O3—C3—C8 | −172.49 (17) |
O3i—Zn1—O1—C1 | −179.67 (15) | Zn1—O3—C3—C8 | 13.7 (3) |
O3—Zn1—O1—C1 | 0.33 (15) | C8—C3—C4—C5 | 1.8 (3) |
O1—Zn1—O3—C3 | 172.76 (18) | O3—C3—C4—C5 | −177.99 (18) |
O1i—Zn1—O3—C3 | −7.24 (18) | C3—C4—C5—C6 | −0.9 (3) |
O1w—Zn1—O3—C3 | −96.51 (17) | C3—C4—C5—C9 | 177.00 (17) |
O1wi—Zn1—O3—C3 | 83.49 (17) | C4—C5—C6—C7 | −0.7 (3) |
O1—Zn1—O3—C2 | −1.31 (13) | C9—C5—C6—C7 | −178.56 (18) |
O1i—Zn1—O3—C2 | 178.69 (13) | C10—O6—C7—C8 | 6.0 (3) |
O1w—Zn1—O3—C2 | 89.42 (14) | C10—O6—C7—C6 | −173.57 (17) |
O1wi—Zn1—O3—C2 | −90.58 (14) | C5—C6—C7—O6 | −179.03 (17) |
O4w—Zn2—O4—C9 | −169.99 (12) | C5—C6—C7—C8 | 1.4 (3) |
O2w—Zn2—O4—C9 | 12.0 (2) | O6—C7—C8—C3 | 180.00 (17) |
O3w—Zn2—O4—C9 | 94.84 (12) | C6—C7—C8—C3 | −0.5 (3) |
O5w—Zn2—O4—C9 | −81.07 (12) | C4—C3—C8—C7 | −1.2 (3) |
O5—Zn2—O4—C9 | 0.33 (11) | O3—C3—C8—C7 | 178.66 (18) |
O4w—Zn2—O5—C9 | 29.9 (3) | Zn2—O5—C9—O4 | 0.56 (18) |
O2w—Zn2—O5—C9 | −175.84 (12) | Zn2—O5—C9—C5 | 178.66 (17) |
O3w—Zn2—O5—C9 | −89.61 (12) | Zn2—O4—C9—O5 | −0.58 (19) |
O5w—Zn2—O5—C9 | 95.70 (12) | Zn2—O4—C9—C5 | −178.70 (16) |
O4—Zn2—O5—C9 | −0.33 (11) | C6—C5—C9—O5 | 24.9 (3) |
Zn1—O1—C1—O2 | −177.86 (15) | C4—C5—C9—O5 | −152.95 (19) |
Zn1—O1—C1—C2 | 0.7 (3) | C6—C5—C9—O4 | −156.98 (18) |
C3—O3—C2—C1 | −173.21 (17) | C4—C5—C9—O4 | 25.1 (3) |
Zn1—O3—C2—C1 | 1.9 (2) | C7—O6—C10—C11 | 175.12 (16) |
O2—C1—C2—O3 | 176.85 (17) | O6—C10—C11—O7 | 16.0 (3) |
O1—C1—C2—O3 | −1.9 (3) | O6—C10—C11—O8 | −165.57 (17) |
C2—O3—C3—C4 | 7.4 (3) |
Symmetry code: (i) −x+2, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O5ii | 0.85 (1) | 1.95 (1) | 2.786 (2) | 170 (3) |
O1w—H1w2···O7iii | 0.85 (1) | 2.10 (2) | 2.836 (2) | 145 (3) |
O2w—H2w1···O7iv | 0.84 (1) | 1.82 (1) | 2.657 (2) | 172 (3) |
O2w—H2w2···O6w | 0.84 (1) | 2.09 (2) | 2.843 (4) | 150 (3) |
O3w—H3w1···O8ii | 0.84 (1) | 1.93 (1) | 2.761 (2) | 167 (2) |
O3w—H3w2···O2v | 0.85 (3) | 1.93 (1) | 2.772 (2) | 172 (3) |
O4w—H4w1···O4vi | 0.86 (3) | 1.91 (1) | 2.758 (2) | 173 (3) |
O4w—H4w2···O8vii | 0.85 (1) | 1.81 (1) | 2.655 (2) | 180 (3) |
O5w—H5w1···O2viii | 0.85 (1) | 1.84 (1) | 2.685 (2) | 170 (2) |
O5w—H5w2···O6wix | 0.85 (1) | 1.97 (2) | 2.708 (3) | 144 (3) |
O5w—H5w2···O6w′ix | 0.85 (1) | 1.90 (1) | 2.732 (6) | 168 (3) |
O6w—H6w1···O8vii | 0.85 (1) | 1.94 (2) | 2.747 (3) | 158 (4) |
O6w—H6w2···O5wx | 0.86 (1) | 1.98 (2) | 2.791 (3) | 156 (4) |
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x, y−1, z; (iv) −x+1, −y+2, −z+1; (v) x−1, y+1, z; (vi) −x+1, −y+1, −z+2; (vii) x−1, y, z+1; (viii) x, y+1, z; (ix) x+1, y, z; (x) −x, −y+2, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Zn3(C11H7O8)2(H2O)10]·2H2O |
Mr | 946.63 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 7.3125 (1), 9.0935 (1), 13.4543 (2) |
α, β, γ (°) | 79.271 (1), 82.6340 (1), 74.064 (1) |
V (Å3) | 842.42 (2) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 2.23 |
Crystal size (mm) | 0.32 × 0.16 × 0.06 |
Data collection | |
Diffractometer | Bruker APEX-II area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.742, 0.878 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14462, 3858, 3176 |
Rint | 0.027 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.067, 1.04 |
No. of reflections | 3858 |
No. of parameters | 299 |
No. of restraints | 18 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.42, −0.29 |
Computer programs: SMART (Bruker, 2006), SAINT (Bruker, 2006), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O5i | 0.85 (1) | 1.95 (1) | 2.786 (2) | 170 (3) |
O1w—H1w2···O7ii | 0.85 (1) | 2.10 (2) | 2.836 (2) | 145 (3) |
O2w—H2w1···O7iii | 0.84 (1) | 1.82 (1) | 2.657 (2) | 172 (3) |
O2w—H2w2···O6w | 0.84 (1) | 2.09 (2) | 2.843 (4) | 150 (3) |
O3w—H3w1···O8i | 0.84 (1) | 1.93 (1) | 2.761 (2) | 167 (2) |
O3w—H3w2···O2iv | 0.85 (3) | 1.93 (1) | 2.772 (2) | 172 (3) |
O4w—H4w1···O4v | 0.86 (3) | 1.91 (1) | 2.758 (2) | 173 (3) |
O4w—H4w2···O8vi | 0.85 (1) | 1.81 (1) | 2.655 (2) | 180 (3) |
O5w—H5w1···O2vii | 0.85 (1) | 1.84 (1) | 2.685 (2) | 170 (2) |
O5w—H5w2···O6wviii | 0.85 (1) | 1.97 (2) | 2.708 (3) | 144 (3) |
O5w—H5w2···O6w'viii | 0.85 (1) | 1.90 (1) | 2.732 (6) | 168 (3) |
O6w—H6w1···O8vi | 0.85 (1) | 1.94 (2) | 2.747 (3) | 158 (4) |
O6w—H6w2···O5wix | 0.86 (1) | 1.98 (2) | 2.791 (3) | 156 (4) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y−1, z; (iii) −x+1, −y+2, −z+1; (iv) x−1, y+1, z; (v) −x+1, −y+1, −z+2; (vi) x−1, y, z+1; (vii) x, y+1, z; (viii) x+1, y, z; (ix) −x, −y+2, −z+2. |
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