Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807060357/ci2501sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807060357/ci2501Isup2.hkl |
CCDC reference: 672741
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.004 Å
- R factor = 0.035
- wR factor = 0.099
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.587 1.000 Tmin(prime) and Tmax expected: 0.537 0.589 RR(prime) = 0.643 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.62
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.59 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.79 PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 4 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.59 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.01 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.842(10) ...... 3.00 su-Ra O1W -H1W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.841(10) ...... 3.00 su-Ra O2W -H2W2 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Ra O1W -H2# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Ra O2W -H4# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.90(3), Rep 1.900(10) ...... 3.00 su-Ra H2# -O8 1.555 1.545 PLAT736_ALERT_1_C H...A Calc 2.03(3), Rep 2.030(10) ...... 3.00 su-Ra H4# -O1 1.555 1.655 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.11 Ratio
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.589 Tmax scaled 0.589 Tmin scaled 0.345 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
The Cambridge Structural Database (Version 5.28, November 2006; Allen, 2002) lists several examples of zinc terephthalate systems. Some crystallize with DMF-type solvent molecules. For the DMF solvate, see: Edgar et al. (2001). For the N,N-diethylformamide solvate, see: Grzesiak et al. (2006).
A mixture of zinc chloride dihydrate (0.5 mmol), terephthalic acid (0.5 mmol) and N,N-dimethylacetamide (12 ml) was heated at 443 K for 3 d. The cooled mixture yielded colourless crystals of the title compound.
H atoms were positioned geometrically (C—H = 0.93–0.96 Å) and refined as riding, with Uiso(H) = 1.2–1.5Ueq(C). The methyl groups were allowed to rotate but not to tip. The water H-atoms were located in a difference Fourier map, and were refined with a distance restraint of O—H = 0.85 (1) Å. The four highest peaks in the final difference Fourier map were observed in the vicinity of the DMA molecules. The positions of the peaks indicate that the DMA molecules are probably not disordered.
Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001) and OLEX (Dolomanov et al., 2003); software used to prepare material for publication: publCIF (Westrip, 2007).
[Zn2(C8H4O4)2(H2O)2]·2C4H9NO | Z = 2 |
Mr = 669.24 | F(000) = 688 |
Triclinic, P1 | Dx = 1.632 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.9291 (5) Å | Cell parameters from 3838 reflections |
b = 10.0551 (7) Å | θ = 2.2–26.0° |
c = 20.620 (2) Å | µ = 1.83 mm−1 |
α = 78.030 (1)° | T = 295 K |
β = 81.044 (1)° | Block, colourless |
γ = 77.266 (1)° | 0.33 × 0.31 × 0.29 mm |
V = 1361.7 (2) Å3 |
Bruker APEXII area-detector diffractometer | 5269 independent reflections |
Radiation source: fine-focus sealed tube | 4503 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
ϕ and ω scans | θmax = 26.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→6 |
Tmin = 0.587, Tmax = 1.000 | k = −12→12 |
7748 measured reflections | l = −25→25 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.099 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0604P)2 + 0.7539P] where P = (Fo2 + 2Fc2)/3 |
5269 reflections | (Δ/σ)max = 0.001 |
383 parameters | Δρmax = 1.24 e Å−3 |
4 restraints | Δρmin = −0.44 e Å−3 |
[Zn2(C8H4O4)2(H2O)2]·2C4H9NO | γ = 77.266 (1)° |
Mr = 669.24 | V = 1361.7 (2) Å3 |
Triclinic, P1 | Z = 2 |
a = 6.9291 (5) Å | Mo Kα radiation |
b = 10.0551 (7) Å | µ = 1.83 mm−1 |
c = 20.620 (2) Å | T = 295 K |
α = 78.030 (1)° | 0.33 × 0.31 × 0.29 mm |
β = 81.044 (1)° |
Bruker APEXII area-detector diffractometer | 5269 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4503 reflections with I > 2σ(I) |
Tmin = 0.587, Tmax = 1.000 | Rint = 0.016 |
7748 measured reflections |
R[F2 > 2σ(F2)] = 0.035 | 4 restraints |
wR(F2) = 0.099 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 1.24 e Å−3 |
5269 reflections | Δρmin = −0.44 e Å−3 |
383 parameters |
x | y | z | Uiso*/Ueq | ||
Zn1 | 0.63480 (4) | 0.67635 (3) | 0.719133 (14) | 0.01316 (10) | |
Zn2 | 0.92767 (4) | 0.77920 (3) | 0.775812 (14) | 0.01324 (10) | |
O1 | 0.5123 (3) | 0.6234 (2) | 0.81850 (9) | 0.0236 (5) | |
O2 | 0.7888 (3) | 0.6531 (2) | 0.85183 (9) | 0.0245 (5) | |
O3 | 0.8096 (3) | 0.7535 (2) | 0.63769 (9) | 0.0250 (5) | |
O4 | 0.9806 (3) | 0.8735 (2) | 0.67983 (9) | 0.0246 (5) | |
O5 | 0.5119 (3) | 0.8748 (2) | 0.72861 (11) | 0.0299 (5) | |
O6 | 0.7024 (3) | 0.9401 (2) | 0.78959 (11) | 0.0309 (5) | |
O7 | −0.1614 (3) | 1.49770 (19) | 0.73505 (10) | 0.0219 (4) | |
O8 | 0.0874 (3) | 1.59581 (19) | 0.74699 (10) | 0.0206 (4) | |
O9 | 0.4592 (4) | 0.6915 (3) | 0.54349 (11) | 0.0450 (7) | |
O10 | 1.0286 (4) | 0.8186 (3) | 0.95154 (12) | 0.0467 (7) | |
O1W | 0.4426 (3) | 0.6272 (2) | 0.67268 (10) | 0.0236 (5) | |
O2W | 1.1323 (3) | 0.8078 (2) | 0.82510 (10) | 0.0217 (4) | |
N1 | 0.3480 (6) | 0.7018 (5) | 0.44740 (18) | 0.0657 (11) | |
N2 | 1.1224 (6) | 0.8029 (4) | 1.05090 (18) | 0.0602 (10) | |
C1 | 0.6258 (4) | 0.6158 (3) | 0.86252 (13) | 0.0178 (6) | |
C2 | 0.5584 (4) | 0.5557 (3) | 0.93373 (13) | 0.0181 (6) | |
C3 | 0.3839 (4) | 0.5026 (3) | 0.94995 (14) | 0.0226 (6) | |
H3 | 0.3063 | 0.5042 | 0.9167 | 0.027* | |
C4 | 0.3260 (4) | 0.4472 (3) | 1.01590 (14) | 0.0231 (6) | |
H4 | 0.2096 | 0.4118 | 1.0266 | 0.028* | |
C5 | 0.9142 (4) | 0.8430 (3) | 0.63250 (13) | 0.0192 (6) | |
C6 | 0.9616 (4) | 0.9236 (3) | 0.56353 (13) | 0.0201 (6) | |
C7 | 0.8558 (5) | 0.9188 (3) | 0.51209 (14) | 0.0257 (7) | |
H7 | 0.7594 | 0.8641 | 0.5203 | 0.031* | |
C8 | 0.8933 (5) | 0.9948 (3) | 0.44886 (14) | 0.0256 (7) | |
H8 | 0.8218 | 0.9915 | 0.4148 | 0.031* | |
C9 | 0.5516 (4) | 0.9592 (3) | 0.75905 (13) | 0.0199 (6) | |
C10 | 0.4100 (4) | 1.0962 (3) | 0.75689 (13) | 0.0180 (6) | |
C11 | 0.2208 (4) | 1.1129 (3) | 0.73742 (14) | 0.0206 (6) | |
H11 | 0.1796 | 1.0382 | 0.7274 | 0.025* | |
C12 | 0.0946 (4) | 1.2414 (3) | 0.73307 (14) | 0.0192 (6) | |
H12 | −0.0323 | 1.2522 | 0.7208 | 0.023* | |
C13 | 0.1558 (4) | 1.3544 (3) | 0.74688 (13) | 0.0158 (5) | |
C14 | 0.3456 (4) | 1.3378 (3) | 0.76604 (14) | 0.0198 (6) | |
H14 | 0.3878 | 1.4128 | 0.7753 | 0.024* | |
C15 | 0.4704 (4) | 1.2094 (3) | 0.77112 (14) | 0.0200 (6) | |
H15 | 0.5963 | 1.1982 | 0.7842 | 0.024* | |
C16 | 0.0166 (4) | 1.4929 (3) | 0.74250 (12) | 0.0157 (5) | |
C17 | 0.3473 (6) | 0.6572 (5) | 0.5108 (2) | 0.0507 (10) | |
C18 | 0.2010 (6) | 0.5604 (4) | 0.54366 (19) | 0.0452 (9) | |
H18A | 0.2192 | 0.5293 | 0.5900 | 0.068* | |
H18B | 0.2261 | 0.4819 | 0.5217 | 0.068* | |
H18C | 0.0668 | 0.6099 | 0.5398 | 0.068* | |
C19 | 0.4846 (7) | 0.7971 (5) | 0.41555 (19) | 0.0590 (12) | |
H19A | 0.5368 | 0.8269 | 0.4494 | 0.088* | |
H19B | 0.4133 | 0.8762 | 0.3883 | 0.088* | |
H19C | 0.5923 | 0.7499 | 0.3883 | 0.088* | |
C20 | 0.2240 (8) | 0.6634 (7) | 0.4052 (2) | 0.0832 (19) | |
H20A | 0.1502 | 0.5966 | 0.4315 | 0.125* | |
H20B | 0.3077 | 0.6242 | 0.3694 | 0.125* | |
H20C | 0.1330 | 0.7444 | 0.3870 | 0.125* | |
C21 | 1.3211 (6) | 0.9137 (4) | 0.9555 (2) | 0.0496 (10) | |
H21A | 1.3178 | 0.9395 | 0.9081 | 0.074* | |
H21B | 1.4445 | 0.8517 | 0.9646 | 0.074* | |
H21C | 1.3099 | 0.9952 | 0.9743 | 0.074* | |
C22 | 1.1458 (6) | 0.8407 (4) | 0.9868 (2) | 0.0478 (10) | |
C23 | 0.9614 (7) | 0.7308 (5) | 1.08110 (19) | 0.0524 (11) | |
H23A | 0.8818 | 0.7282 | 1.0474 | 0.079* | |
H23B | 0.8800 | 0.7787 | 1.1145 | 0.079* | |
H23C | 1.0160 | 0.6379 | 1.1014 | 0.079* | |
C24 | 1.2542 (9) | 0.8267 (6) | 1.0954 (2) | 0.0812 (17) | |
H24A | 1.3640 | 0.8633 | 1.0690 | 0.122* | |
H24B | 1.3037 | 0.7406 | 1.1233 | 0.122* | |
H24C | 1.1806 | 0.8916 | 1.1228 | 0.122* | |
H1W1 | 0.438 (6) | 0.652 (4) | 0.6313 (6) | 0.041 (11)* | |
H1W2 | 0.329 (3) | 0.620 (4) | 0.6927 (18) | 0.060 (14)* | |
H2W1 | 1.095 (6) | 0.811 (4) | 0.8661 (7) | 0.048 (12)* | |
H2W2 | 1.246 (3) | 0.757 (3) | 0.8228 (19) | 0.050 (12)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.01266 (17) | 0.01296 (17) | 0.01259 (16) | −0.00214 (12) | −0.00050 (12) | −0.00054 (12) |
Zn2 | 0.01314 (17) | 0.01313 (17) | 0.01196 (16) | −0.00188 (12) | −0.00091 (12) | −0.00006 (12) |
O1 | 0.0223 (11) | 0.0349 (12) | 0.0117 (9) | −0.0074 (9) | −0.0020 (8) | 0.0016 (8) |
O2 | 0.0229 (11) | 0.0334 (12) | 0.0158 (10) | −0.0130 (9) | 0.0005 (8) | 0.0049 (8) |
O3 | 0.0275 (11) | 0.0304 (12) | 0.0159 (10) | −0.0136 (9) | 0.0000 (8) | 0.0049 (8) |
O4 | 0.0368 (12) | 0.0277 (11) | 0.0107 (9) | −0.0144 (10) | −0.0016 (9) | 0.0015 (8) |
O5 | 0.0283 (12) | 0.0173 (11) | 0.0415 (13) | 0.0057 (9) | −0.0045 (10) | −0.0099 (9) |
O6 | 0.0290 (12) | 0.0245 (11) | 0.0347 (12) | 0.0101 (9) | −0.0097 (10) | −0.0070 (9) |
O7 | 0.0157 (10) | 0.0156 (10) | 0.0333 (11) | 0.0009 (8) | −0.0069 (9) | −0.0032 (8) |
O8 | 0.0164 (10) | 0.0132 (9) | 0.0313 (11) | −0.0012 (8) | −0.0006 (8) | −0.0051 (8) |
O9 | 0.0446 (15) | 0.0735 (19) | 0.0225 (12) | −0.0206 (14) | −0.0096 (11) | −0.0071 (12) |
O10 | 0.0457 (16) | 0.073 (2) | 0.0252 (12) | −0.0122 (14) | −0.0069 (11) | −0.0158 (12) |
O1W | 0.0185 (11) | 0.0388 (13) | 0.0160 (10) | −0.0122 (9) | −0.0023 (9) | −0.0029 (9) |
O2W | 0.0167 (10) | 0.0306 (12) | 0.0183 (10) | −0.0030 (9) | −0.0021 (8) | −0.0073 (9) |
N1 | 0.050 (2) | 0.104 (3) | 0.043 (2) | −0.001 (2) | −0.0125 (17) | −0.023 (2) |
N2 | 0.071 (3) | 0.069 (3) | 0.044 (2) | −0.006 (2) | −0.0204 (19) | −0.0154 (18) |
C1 | 0.0162 (13) | 0.0167 (13) | 0.0164 (13) | 0.0005 (11) | 0.0011 (11) | −0.0003 (11) |
C2 | 0.0203 (14) | 0.0187 (14) | 0.0131 (12) | −0.0052 (11) | 0.0017 (11) | 0.0009 (11) |
C3 | 0.0226 (15) | 0.0318 (16) | 0.0141 (13) | −0.0106 (13) | −0.0022 (11) | 0.0002 (12) |
C4 | 0.0196 (14) | 0.0309 (16) | 0.0185 (14) | −0.0119 (12) | −0.0002 (11) | 0.0018 (12) |
C5 | 0.0206 (14) | 0.0174 (14) | 0.0148 (13) | −0.0017 (11) | 0.0016 (11) | 0.0026 (11) |
C6 | 0.0244 (15) | 0.0210 (14) | 0.0131 (13) | −0.0075 (12) | 0.0018 (11) | 0.0014 (11) |
C7 | 0.0300 (16) | 0.0296 (16) | 0.0185 (14) | −0.0156 (13) | −0.0019 (12) | 0.0034 (12) |
C8 | 0.0318 (17) | 0.0323 (17) | 0.0150 (14) | −0.0162 (14) | −0.0038 (12) | 0.0022 (12) |
C9 | 0.0213 (15) | 0.0141 (13) | 0.0178 (13) | 0.0016 (11) | 0.0030 (11) | 0.0025 (11) |
C10 | 0.0208 (14) | 0.0150 (13) | 0.0154 (13) | 0.0010 (11) | 0.0002 (11) | −0.0026 (10) |
C11 | 0.0226 (15) | 0.0137 (13) | 0.0254 (15) | −0.0029 (11) | −0.0022 (12) | −0.0041 (11) |
C12 | 0.0156 (13) | 0.0188 (14) | 0.0229 (14) | −0.0012 (11) | −0.0050 (11) | −0.0032 (11) |
C13 | 0.0155 (13) | 0.0137 (13) | 0.0156 (13) | 0.0000 (11) | 0.0001 (10) | −0.0010 (10) |
C14 | 0.0222 (15) | 0.0149 (13) | 0.0222 (14) | −0.0034 (11) | −0.0032 (12) | −0.0032 (11) |
C15 | 0.0159 (13) | 0.0214 (14) | 0.0210 (14) | 0.0006 (11) | −0.0051 (11) | −0.0023 (11) |
C16 | 0.0181 (14) | 0.0133 (13) | 0.0124 (12) | −0.0006 (11) | −0.0001 (10) | 0.0009 (10) |
C17 | 0.043 (2) | 0.064 (3) | 0.040 (2) | 0.006 (2) | −0.0035 (18) | −0.017 (2) |
C18 | 0.041 (2) | 0.054 (2) | 0.042 (2) | −0.0116 (18) | 0.0001 (17) | −0.0124 (18) |
C19 | 0.059 (3) | 0.080 (3) | 0.029 (2) | −0.015 (2) | −0.0006 (19) | 0.009 (2) |
C20 | 0.061 (3) | 0.147 (6) | 0.051 (3) | 0.001 (3) | −0.024 (2) | −0.048 (3) |
C21 | 0.051 (2) | 0.048 (2) | 0.052 (2) | −0.013 (2) | −0.005 (2) | −0.0104 (19) |
C22 | 0.055 (3) | 0.045 (2) | 0.040 (2) | 0.0051 (19) | −0.0066 (19) | −0.0160 (18) |
C23 | 0.064 (3) | 0.061 (3) | 0.030 (2) | −0.019 (2) | 0.0014 (19) | −0.0039 (18) |
C24 | 0.102 (4) | 0.097 (4) | 0.058 (3) | −0.009 (3) | −0.046 (3) | −0.029 (3) |
Zn1—O1 | 2.100 (2) | C5—C6 | 1.510 (4) |
Zn1—O3 | 2.032 (2) | C6—C7 | 1.394 (4) |
Zn1—O5 | 2.026 (2) | C6—C8iv | 1.395 (4) |
Zn1—O7i | 2.027 (2) | C7—C8 | 1.386 (4) |
Zn1—O1W | 1.954 (2) | C7—H7 | 0.93 |
Zn1—Zn2 | 2.9527 (4) | C8—C6iv | 1.395 (4) |
Zn2—O2 | 2.058 (2) | C8—H8 | 0.93 |
Zn2—O4 | 2.025 (2) | C9—C10 | 1.501 (4) |
Zn2—O6 | 2.018 (2) | C10—C15 | 1.394 (4) |
Zn2—O8i | 2.080 (2) | C10—C11 | 1.395 (4) |
Zn2—O2W | 1.969 (2) | C11—C12 | 1.386 (4) |
O1—C1 | 1.271 (3) | C11—H11 | 0.93 |
O2—C1 | 1.241 (3) | C12—C13 | 1.392 (4) |
O3—C5 | 1.253 (3) | C12—H12 | 0.93 |
O4—C5 | 1.258 (3) | C13—C14 | 1.397 (4) |
O5—C9 | 1.252 (4) | C13—C16 | 1.503 (4) |
O6—C9 | 1.262 (4) | C14—C15 | 1.381 (4) |
O7—C16 | 1.255 (3) | C14—H14 | 0.93 |
O7—Zn1ii | 2.0274 (19) | C15—H15 | 0.93 |
O8—C16 | 1.264 (3) | C17—C18 | 1.543 (6) |
O8—Zn2ii | 2.0804 (19) | C18—H18A | 0.96 |
O9—C17 | 1.246 (5) | C18—H18B | 0.96 |
O10—C22 | 1.252 (5) | C18—H18C | 0.96 |
O1W—H1W1 | 0.842 (10) | C19—H19A | 0.96 |
O1W—H1W2 | 0.842 (10) | C19—H19B | 0.96 |
O2W—H2W1 | 0.849 (10) | C19—H19C | 0.96 |
O2W—H2W2 | 0.841 (10) | C20—H20A | 0.96 |
N1—C17 | 1.290 (5) | C20—H20B | 0.96 |
N1—C19 | 1.479 (6) | C20—H20C | 0.96 |
N1—C20 | 1.472 (6) | C21—C22 | 1.544 (6) |
N2—C22 | 1.292 (5) | C21—H21A | 0.96 |
N2—C23 | 1.453 (6) | C21—H21B | 0.96 |
N2—C24 | 1.477 (5) | C21—H21C | 0.96 |
C1—C2 | 1.511 (4) | C23—H23A | 0.96 |
C2—C3 | 1.394 (4) | C23—H23B | 0.96 |
C2—C4iii | 1.399 (4) | C23—H23C | 0.96 |
C3—C4 | 1.391 (4) | C24—H24A | 0.96 |
C3—H3 | 0.93 | C24—H24B | 0.96 |
C4—C2iii | 1.399 (4) | C24—H24C | 0.96 |
C4—H4 | 0.93 | ||
O1W—Zn1—O5 | 102.58 (9) | C6—C7—H7 | 119.7 |
O1W—Zn1—O7i | 102.98 (9) | C7—C8—C6iv | 119.8 (3) |
O5—Zn1—O7i | 154.30 (9) | C7—C8—H8 | 120.1 |
O1W—Zn1—O3 | 98.14 (8) | C6iv—C8—H8 | 120.1 |
O5—Zn1—O3 | 87.61 (9) | O5—C9—O6 | 125.5 (3) |
O7i—Zn1—O3 | 91.40 (8) | O5—C9—C10 | 116.7 (3) |
O1W—Zn1—O1 | 100.14 (8) | O6—C9—C10 | 117.8 (3) |
O5—Zn1—O1 | 85.75 (9) | C15—C10—C11 | 119.5 (3) |
O7i—Zn1—O1 | 87.20 (8) | C15—C10—C9 | 120.1 (3) |
O3—Zn1—O1 | 161.51 (8) | C11—C10—C9 | 120.3 (3) |
O1W—Zn1—Zn2 | 173.06 (6) | C12—C11—C10 | 119.6 (3) |
O5—Zn1—Zn2 | 73.54 (6) | C12—C11—H11 | 120.2 |
O7i—Zn1—Zn2 | 81.29 (6) | C10—C11—H11 | 120.2 |
O3—Zn1—Zn2 | 76.13 (6) | C11—C12—C13 | 120.7 (3) |
O1—Zn1—Zn2 | 85.44 (6) | C11—C12—H12 | 119.6 |
O2W—Zn2—O6 | 102.78 (9) | C13—C12—H12 | 119.6 |
O2W—Zn2—O4 | 107.47 (9) | C12—C13—C14 | 119.6 (2) |
O6—Zn2—O4 | 88.71 (9) | C12—C13—C16 | 120.1 (2) |
O2W—Zn2—O2 | 98.12 (8) | C14—C13—C16 | 120.3 (2) |
O6—Zn2—O2 | 89.76 (9) | C15—C14—C13 | 119.6 (3) |
O4—Zn2—O2 | 154.05 (8) | C15—C14—H14 | 120.2 |
O2W—Zn2—O8i | 96.33 (8) | C13—C14—H14 | 120.2 |
O6—Zn2—O8i | 160.78 (9) | C14—C15—C10 | 120.9 (3) |
O4—Zn2—O8i | 87.53 (8) | C14—C15—H15 | 119.6 |
O2—Zn2—O8i | 85.46 (8) | C10—C15—H15 | 119.6 |
O2W—Zn2—Zn1 | 167.77 (6) | O7—C16—O8 | 124.9 (2) |
O6—Zn2—Zn1 | 84.84 (7) | O7—C16—C13 | 117.7 (2) |
O4—Zn2—Zn1 | 81.98 (6) | O8—C16—C13 | 117.5 (2) |
O2—Zn2—Zn1 | 72.09 (6) | O9—C17—N1 | 121.2 (4) |
O8i—Zn2—Zn1 | 75.97 (6) | O9—C17—C18 | 122.0 (4) |
C1—O1—Zn1 | 115.60 (17) | N1—C17—C18 | 116.7 (4) |
C1—O2—Zn2 | 135.28 (18) | C17—C18—H18A | 109.5 |
C5—O3—Zn1 | 128.33 (19) | C17—C18—H18B | 109.5 |
C5—O4—Zn2 | 122.57 (18) | H18A—C18—H18B | 109.5 |
C9—O5—Zn1 | 134.0 (2) | C17—C18—H18C | 109.5 |
C9—O6—Zn2 | 118.93 (19) | H18A—C18—H18C | 109.5 |
C16—O7—Zn1ii | 123.68 (17) | H18B—C18—H18C | 109.5 |
C16—O8—Zn2ii | 126.38 (17) | N1—C19—H19A | 109.5 |
Zn1—O1W—H1W1 | 123 (3) | N1—C19—H19B | 109.5 |
Zn1—O1W—H1W2 | 119 (3) | H19A—C19—H19B | 109.5 |
H1W1—O1W—H1W2 | 111 (4) | N1—C19—H19C | 109.5 |
Zn2—O2W—H2W1 | 114 (3) | H19A—C19—H19C | 109.5 |
Zn2—O2W—H2W2 | 120 (3) | H19B—C19—H19C | 109.5 |
H2W1—O2W—H2W2 | 107 (4) | N1—C20—H20A | 109.5 |
C17—N1—C19 | 117.3 (4) | N1—C20—H20B | 109.5 |
C17—N1—C20 | 124.4 (5) | H20A—C20—H20B | 109.5 |
C19—N1—C20 | 118.4 (4) | N1—C20—H20C | 109.5 |
C22—N2—C23 | 118.8 (4) | H20A—C20—H20C | 109.5 |
C22—N2—C24 | 123.3 (5) | H20B—C20—H20C | 109.5 |
C23—N2—C24 | 117.9 (4) | C22—C21—H21A | 109.5 |
O2—C1—O1 | 125.4 (3) | C22—C21—H21B | 109.5 |
O2—C1—C2 | 117.0 (2) | H21A—C21—H21B | 109.5 |
O1—C1—C2 | 117.6 (2) | C22—C21—H21C | 109.5 |
C3—C2—C4iii | 119.6 (3) | H21A—C21—H21C | 109.5 |
C3—C2—C1 | 121.2 (2) | H21B—C21—H21C | 109.5 |
C4iii—C2—C1 | 119.3 (2) | O10—C22—N2 | 120.5 (4) |
C4—C3—C2 | 119.9 (3) | O10—C22—C21 | 121.4 (4) |
C4—C3—H3 | 120.0 | N2—C22—C21 | 118.1 (4) |
C2—C3—H3 | 120.0 | N2—C23—H23A | 109.5 |
C3—C4—C2iii | 120.5 (3) | N2—C23—H23B | 109.5 |
C3—C4—H4 | 119.7 | H23A—C23—H23B | 109.5 |
C2iii—C4—H4 | 119.7 | N2—C23—H23C | 109.5 |
O3—C5—O4 | 125.8 (2) | H23A—C23—H23C | 109.5 |
O3—C5—C6 | 117.2 (2) | H23B—C23—H23C | 109.5 |
O4—C5—C6 | 117.0 (2) | N2—C24—H24A | 109.5 |
C7—C6—C8iv | 119.7 (3) | N2—C24—H24B | 109.5 |
C7—C6—C5 | 119.6 (3) | H24A—C24—H24B | 109.5 |
C8iv—C6—C5 | 120.7 (3) | N2—C24—H24C | 109.5 |
C8—C7—C6 | 120.5 (3) | H24A—C24—H24C | 109.5 |
C8—C7—H7 | 119.7 | H24B—C24—H24C | 109.5 |
O1W—Zn1—O1—C1 | 165.7 (2) | O3—C5—C6—C7 | 13.9 (4) |
O5—Zn1—O1—C1 | −92.2 (2) | O4—C5—C6—C7 | −165.0 (3) |
O7i—Zn1—O1—C1 | 63.1 (2) | O3—C5—C6—C8iv | −167.6 (3) |
O3—Zn1—O1—C1 | −23.0 (4) | O4—C5—C6—C8iv | 13.6 (4) |
O2W—Zn2—O2—C1 | 162.7 (3) | C8iv—C6—C7—C8 | −0.3 (5) |
O6—Zn2—O2—C1 | 59.8 (3) | C5—C6—C7—C8 | 178.3 (3) |
O4—Zn2—O2—C1 | −26.7 (4) | C6—C7—C8—C6iv | 0.3 (5) |
O8i—Zn2—O2—C1 | −101.5 (3) | Zn1—O5—C9—O6 | 6.5 (5) |
O1W—Zn1—O3—C5 | 152.7 (2) | Zn1—O5—C9—C10 | −175.55 (19) |
O5—Zn1—O3—C5 | 50.3 (2) | Zn2—O6—C9—O5 | 12.3 (4) |
O7i—Zn1—O3—C5 | −104.0 (2) | Zn2—O6—C9—C10 | −165.71 (18) |
O1—Zn1—O3—C5 | −18.7 (4) | O5—C9—C10—C15 | −160.6 (3) |
Zn2—Zn1—O3—C5 | −23.3 (2) | O6—C9—C10—C15 | 17.5 (4) |
O2W—Zn2—O4—C5 | 159.7 (2) | O5—C9—C10—C11 | 16.2 (4) |
O6—Zn2—O4—C5 | −97.3 (2) | O6—C9—C10—C11 | −165.7 (3) |
O2—Zn2—O4—C5 | −10.5 (4) | C15—C10—C11—C12 | −0.6 (4) |
O8i—Zn2—O4—C5 | 63.8 (2) | C9—C10—C11—C12 | −177.4 (3) |
Zn1—Zn2—O4—C5 | −12.3 (2) | C10—C11—C12—C13 | 1.0 (4) |
O1W—Zn1—O5—C9 | 171.8 (3) | C11—C12—C13—C14 | −0.7 (4) |
O7i—Zn1—O5—C9 | −2.1 (4) | C11—C12—C13—C16 | −179.5 (2) |
O3—Zn1—O5—C9 | −90.4 (3) | C12—C13—C14—C15 | −0.1 (4) |
O1—Zn1—O5—C9 | 72.4 (3) | C16—C13—C14—C15 | 178.7 (2) |
O2W—Zn2—O6—C9 | 173.9 (2) | C13—C14—C15—C10 | 0.5 (4) |
O4—Zn2—O6—C9 | 66.3 (2) | C11—C10—C15—C14 | −0.2 (4) |
O2—Zn2—O6—C9 | −87.8 (2) | C9—C10—C15—C14 | 176.7 (3) |
O8i—Zn2—O6—C9 | −12.4 (4) | Zn1ii—O7—C16—O8 | 6.6 (4) |
Zn2—O2—C1—O1 | 18.1 (5) | Zn1ii—O7—C16—C13 | −173.87 (16) |
Zn2—O2—C1—C2 | −162.33 (19) | Zn2ii—O8—C16—O7 | 22.5 (4) |
Zn1—O1—C1—O2 | 9.3 (4) | Zn2ii—O8—C16—C13 | −157.04 (17) |
Zn1—O1—C1—C2 | −170.23 (18) | C12—C13—C16—O7 | 9.4 (4) |
O2—C1—C2—C3 | −175.7 (3) | C14—C13—C16—O7 | −169.4 (2) |
O1—C1—C2—C3 | 3.9 (4) | C12—C13—C16—O8 | −171.0 (2) |
O2—C1—C2—C4iii | 3.9 (4) | C14—C13—C16—O8 | 10.1 (4) |
O1—C1—C2—C4iii | −176.5 (3) | C19—N1—C17—O9 | −0.9 (6) |
C4iii—C2—C3—C4 | 0.0 (5) | C20—N1—C17—O9 | 178.5 (4) |
C1—C2—C3—C4 | 179.6 (3) | C19—N1—C17—C18 | 178.7 (4) |
C2—C3—C4—C2iii | 0.0 (5) | C20—N1—C17—C18 | −1.8 (7) |
Zn1—O3—C5—O4 | 23.0 (4) | C23—N2—C22—O10 | 1.8 (6) |
Zn1—O3—C5—C6 | −155.74 (19) | C24—N2—C22—O10 | −179.5 (4) |
Zn2—O4—C5—O3 | 0.0 (4) | C23—N2—C22—C21 | −178.4 (4) |
Zn2—O4—C5—C6 | 178.80 (18) | C24—N2—C22—C21 | 0.3 (6) |
Symmetry codes: (i) x+1, y−1, z; (ii) x−1, y+1, z; (iii) −x+1, −y+1, −z+2; (iv) −x+2, −y+2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O9 | 0.84 (1) | 1.76 (1) | 2.598 (3) | 173 (4) |
O1w—H1w2···O8v | 0.84 (1) | 1.90 (1) | 2.734 (3) | 173 (4) |
O2w—H2w1···O10 | 0.85 (1) | 1.76 (1) | 2.613 (3) | 177 (4) |
O2w—H2w2···O1vi | 0.84 (1) | 2.03 (1) | 2.869 (3) | 176 (4) |
Symmetry codes: (v) x, y−1, z; (vi) x+1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Zn2(C8H4O4)2(H2O)2]·2C4H9NO |
Mr | 669.24 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 6.9291 (5), 10.0551 (7), 20.620 (2) |
α, β, γ (°) | 78.030 (1), 81.044 (1), 77.266 (1) |
V (Å3) | 1361.7 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.83 |
Crystal size (mm) | 0.33 × 0.31 × 0.29 |
Data collection | |
Diffractometer | Bruker APEXII area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.587, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7748, 5269, 4503 |
Rint | 0.016 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.099, 1.04 |
No. of reflections | 5269 |
No. of parameters | 383 |
No. of restraints | 4 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.24, −0.44 |
Computer programs: APEX2 (Bruker, 2006), SAINT (Bruker, 2006), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001) and OLEX (Dolomanov et al., 2003), publCIF (Westrip, 2007).
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O9 | 0.84 (1) | 1.76 (1) | 2.598 (3) | 173 (4) |
O1w—H1w2···O8i | 0.84 (1) | 1.90 (1) | 2.734 (3) | 173 (4) |
O2w—H2w1···O10 | 0.85 (1) | 1.76 (1) | 2.613 (3) | 177 (4) |
O2w—H2w2···O1ii | 0.84 (1) | 2.03 (1) | 2.869 (3) | 176 (4) |
Symmetry codes: (i) x, y−1, z; (ii) x+1, y, z. |
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The Cambridge Structural Database (Version 5.28, November 2006; Allen, 2002) lists several examples of zinc terephthalate systems. Some crystallize with DMF-type of solvent molecules. In the present compound, the terephthalate dianion uses both carboxylate ends to bridge a pair of water-coordinated zinc(II) atoms [Zn···Zn = 2.9527 (4) Å] into a two-dimensional square-grid motif (Fig. 1). Each of the grid cavity (Fig. 2) contains two solvent molecules.