The crystal structure of the title compound, [Cd(C8H3FO4)(H2O)2]n, consists of polymeric sheets formed by the bridging of octahedrally coordinated CdII by carboxylate O atoms of the 3-fluorophthalate (3-fpt2−) ligand. The layers exhibit hydrogen bonding between each of two coordinated water molecules and two O atoms of the ligand. Adjacent sheets are connected through π–π interactions.
Supporting information
CCDC reference: 640266
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.003 Å
- R factor = 0.017
- wR factor = 0.042
- Data-to-parameter ratio = 12.0
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O6 - H6A ... ?
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.882 1.000
Tmin and Tmax expected: 0.548 0.688
RR = 1.108
Please check that your absorption correction is appropriate.
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.11
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.69
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 = 5
PLAT731_ALERT_1_C Bond Calc 0.76(4), Rep 0.758(19) ...... 2.11 su-Ra
O5 -H5B 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.76(4), Rep 0.758(19) ...... 2.11 su-Ra
O5 -H5B 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.99(4), Rep 1.994(19) ...... 2.11 su-Ra
H5B -O1 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.16 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 0.688
Tmax scaled 0.688 Tmin scaled 0.607
0 ALERT level A = In general: serious problem
1 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
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART-NT (Bruker, 2003); cell refinement: SAINT-Plus-NT (Bruker, 2003); data reduction: SAINT-Plus-NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL and DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXTL (Sheldrick, 2000).
Poly[diaqua(µ
4-3-fluorophthalato-
κ4O:
O:
O':
O'')cadmium(II)]
top
Crystal data top
[Cd(C8H3FO4)(H2O)2] | Z = 2 |
Mr = 330.54 | F(000) = 320 |
Triclinic, P1 | Dx = 2.326 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.9460 (5) Å | Cell parameters from 3703 reflections |
b = 7.2330 (5) Å | θ = 3.2–26.4° |
c = 10.8199 (8) Å | µ = 2.34 mm−1 |
α = 103.217 (1)° | T = 294 K |
β = 93.351 (1)° | Irregular cleavage fragment, colorless |
γ = 115.066 (1)° | 0.36 × 0.22 × 0.16 mm |
V = 471.86 (6) Å3 | |
Data collection top
Bruker SMART APEX CCD diffractometer | 1927 independent reflections |
Radiation source: fine-focus sealed tube | 1893 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.012 |
ω scans | θmax = 26.4°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2003) | h = −8→8 |
Tmin = 0.882, Tmax = 1.000 | k = −9→9 |
4370 measured reflections | l = −13→13 |
Refinement top
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)] = 0.017 | Hydrogen site location: mixed |
wR(F2) = 0.042 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0169P)2 + 0.4118P] where P = (Fo2 + 2Fc2)/3 |
1927 reflections | (Δ/σ)max = 0.001 |
161 parameters | Δρmax = 0.51 e Å−3 |
6 restraints | Δρmin = −0.40 e Å−3 |
Special details top
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. Six restraints used for water molecule O—H distances (SHELX SADI). 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0.23811 (2) | 0.69249 (2) | 0.449609 (14) | 0.02314 (6) | |
C1 | 0.7361 (4) | 0.4582 (3) | 0.0973 (2) | 0.0250 (4) | |
C2 | 0.7182 (3) | 0.5602 (3) | 0.21721 (19) | 0.0196 (4) | |
C3 | 0.7369 (3) | 0.7660 (3) | 0.2355 (2) | 0.0197 (4) | |
C4 | 0.7725 (4) | 0.8579 (4) | 0.1337 (2) | 0.0267 (5) | |
H4 | 0.7851 | 0.9944 | 0.1457 | 0.032* | |
C5 | 0.7892 (4) | 0.7487 (4) | 0.0149 (2) | 0.0310 (5) | |
H5 | 0.8124 | 0.8119 | −0.0522 | 0.037* | |
C6 | 0.7716 (4) | 0.5462 (4) | −0.0042 (2) | 0.0304 (5) | |
H6 | 0.7834 | 0.4717 | −0.0833 | 0.036* | |
C7 | 0.6893 (3) | 0.4510 (3) | 0.3228 (2) | 0.0204 (4) | |
C8 | 0.7081 (3) | 0.8865 (3) | 0.3602 (2) | 0.0205 (4) | |
O1 | 0.5135 (3) | 0.2983 (3) | 0.31762 (17) | 0.0322 (4) | |
O2 | 0.8514 (2) | 0.5188 (2) | 0.41002 (14) | 0.0246 (3) | |
O3 | 0.5836 (3) | 0.7846 (3) | 0.42525 (15) | 0.0295 (3) | |
O4 | 0.8109 (3) | 1.0858 (2) | 0.38932 (16) | 0.0316 (4) | |
O5 | 0.1602 (3) | 0.3772 (3) | 0.30211 (17) | 0.0293 (4) | |
H5A | 0.067 (4) | 0.293 (4) | 0.323 (3) | 0.035 (8)* | |
H5B | 0.254 (5) | 0.350 (6) | 0.309 (4) | 0.072 (13)* | |
O6 | 0.2474 (3) | 0.8679 (3) | 0.2925 (2) | 0.0384 (4) | |
H6A | 0.144 (4) | 0.859 (6) | 0.256 (3) | 0.069 (13)* | |
H6B | 0.319 (6) | 0.986 (4) | 0.300 (5) | 0.096 (16)* | |
F1 | 0.7185 (3) | 0.2598 (2) | 0.07806 (15) | 0.0438 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.02516 (10) | 0.02000 (9) | 0.02341 (9) | 0.00799 (7) | 0.01087 (6) | 0.00721 (6) |
C1 | 0.0274 (11) | 0.0225 (11) | 0.0257 (11) | 0.0131 (9) | 0.0043 (9) | 0.0042 (9) |
C2 | 0.0176 (9) | 0.0200 (10) | 0.0204 (10) | 0.0072 (8) | 0.0016 (8) | 0.0067 (8) |
C3 | 0.0190 (9) | 0.0185 (10) | 0.0205 (10) | 0.0069 (8) | 0.0042 (8) | 0.0064 (8) |
C4 | 0.0316 (12) | 0.0219 (10) | 0.0267 (11) | 0.0099 (9) | 0.0058 (9) | 0.0108 (9) |
C5 | 0.0368 (13) | 0.0335 (12) | 0.0219 (11) | 0.0118 (10) | 0.0085 (9) | 0.0138 (9) |
C6 | 0.0337 (12) | 0.0369 (13) | 0.0204 (10) | 0.0165 (10) | 0.0078 (9) | 0.0059 (9) |
C7 | 0.0232 (10) | 0.0201 (10) | 0.0222 (10) | 0.0124 (8) | 0.0077 (8) | 0.0075 (8) |
C8 | 0.0192 (9) | 0.0227 (10) | 0.0214 (10) | 0.0105 (8) | 0.0038 (8) | 0.0071 (8) |
O1 | 0.0263 (8) | 0.0264 (8) | 0.0439 (10) | 0.0071 (7) | 0.0092 (7) | 0.0185 (7) |
O2 | 0.0252 (8) | 0.0296 (8) | 0.0224 (7) | 0.0136 (7) | 0.0034 (6) | 0.0108 (6) |
O3 | 0.0267 (8) | 0.0320 (9) | 0.0308 (8) | 0.0110 (7) | 0.0139 (7) | 0.0127 (7) |
O4 | 0.0426 (10) | 0.0194 (8) | 0.0311 (9) | 0.0118 (7) | 0.0178 (7) | 0.0054 (7) |
O5 | 0.0251 (9) | 0.0271 (9) | 0.0322 (9) | 0.0093 (7) | 0.0097 (7) | 0.0054 (7) |
O6 | 0.0334 (10) | 0.0294 (10) | 0.0473 (11) | 0.0065 (8) | −0.0002 (8) | 0.0187 (8) |
F1 | 0.0700 (11) | 0.0318 (8) | 0.0387 (8) | 0.0322 (8) | 0.0125 (8) | 0.0072 (7) |
Geometric parameters (Å, º) top
Cd1—O2i | 2.3226 (15) | C5—C6 | 1.382 (3) |
Cd1—O2ii | 2.3951 (15) | C5—H5 | 0.9300 |
Cd1—O3 | 2.2518 (16) | C6—H6 | 0.9300 |
Cd1—O4iii | 2.2312 (16) | C7—O1 | 1.239 (3) |
Cd1—O5 | 2.2866 (17) | C7—O2 | 1.263 (3) |
Cd1—O6 | 2.3308 (19) | C8—O3 | 1.247 (3) |
C1—F1 | 1.353 (2) | C8—O4 | 1.257 (3) |
C1—C6 | 1.375 (3) | O2—Cd1i | 2.3226 (15) |
C1—C2 | 1.379 (3) | O2—Cd1iv | 2.3952 (15) |
C2—C3 | 1.404 (3) | O4—Cd1iii | 2.2312 (15) |
C2—C7 | 1.508 (3) | O5—H5A | 0.765 (18) |
C3—C4 | 1.394 (3) | O5—H5B | 0.758 (19) |
C3—C8 | 1.504 (3) | O6—H6A | 0.767 (19) |
C4—C5 | 1.387 (3) | O6—H6B | 0.764 (19) |
C4—H4 | 0.9300 | | |
| | | |
O2i—Cd1—O2ii | 75.64 (6) | C5—C4—H4 | 119.6 |
O2i—Cd1—O6 | 167.55 (6) | C3—C4—H4 | 119.6 |
O3—Cd1—O2i | 109.30 (6) | C6—C5—C4 | 120.2 (2) |
O3—Cd1—O2ii | 161.87 (6) | C6—C5—H5 | 119.9 |
O3—Cd1—O5 | 85.61 (6) | C4—C5—H5 | 119.9 |
O3—Cd1—O6 | 82.16 (7) | C1—C6—C5 | 118.0 (2) |
O4iii—Cd1—O2i | 81.61 (6) | C1—C6—H6 | 121.0 |
O4iii—Cd1—O2ii | 82.27 (6) | C5—C6—H6 | 121.0 |
O4iii—Cd1—O3 | 115.46 (6) | O1—C7—O2 | 123.89 (19) |
O4iii—Cd1—O5 | 157.03 (6) | O1—C7—C2 | 119.16 (19) |
O4iii—Cd1—O6 | 98.11 (7) | O2—C7—C2 | 116.91 (18) |
O5—Cd1—O2i | 82.75 (6) | O3—C8—O4 | 125.0 (2) |
O5—Cd1—O2ii | 77.62 (6) | O3—C8—C3 | 118.70 (19) |
O5—Cd1—O6 | 93.58 (7) | O4—C8—C3 | 116.31 (18) |
O6—Cd1—O2ii | 91.96 (6) | C7—O2—Cd1i | 108.62 (13) |
F1—C1—C6 | 117.8 (2) | C7—O2—Cd1iv | 142.24 (14) |
F1—C1—C2 | 118.20 (19) | Cd1i—O2—Cd1iv | 104.36 (5) |
C6—C1—C2 | 124.0 (2) | C8—O3—Cd1 | 136.06 (14) |
C1—C2—C3 | 117.46 (19) | C8—O4—Cd1iii | 124.39 (14) |
C1—C2—C7 | 119.10 (18) | Cd1—O5—H5A | 105 (2) |
C3—C2—C7 | 123.39 (18) | Cd1—O5—H5B | 110 (3) |
C4—C3—C2 | 119.47 (19) | H5A—O5—H5B | 106 (4) |
C4—C3—C8 | 118.71 (19) | Cd1—O6—H6A | 122 (3) |
C2—C3—C8 | 121.75 (18) | Cd1—O6—H6B | 126 (4) |
C5—C4—C3 | 120.9 (2) | H6A—O6—H6B | 97 (4) |
| | | |
F1—C1—C2—C3 | 180.00 (19) | C4—C3—C8—O3 | 146.5 (2) |
C6—C1—C2—C3 | 0.2 (3) | C2—C3—C8—O3 | −30.2 (3) |
F1—C1—C2—C7 | 2.5 (3) | C4—C3—C8—O4 | −32.3 (3) |
C6—C1—C2—C7 | −177.3 (2) | C2—C3—C8—O4 | 151.0 (2) |
C1—C2—C3—C4 | −0.1 (3) | O1—C7—O2—Cd1i | 0.9 (3) |
C7—C2—C3—C4 | 177.30 (19) | C2—C7—O2—Cd1i | −176.76 (14) |
C1—C2—C3—C8 | 176.66 (19) | O1—C7—O2—Cd1iv | 150.52 (18) |
C7—C2—C3—C8 | −6.0 (3) | C2—C7—O2—Cd1iv | −27.2 (3) |
C2—C3—C4—C5 | 0.1 (3) | O4—C8—O3—Cd1 | 81.5 (3) |
C8—C3—C4—C5 | −176.8 (2) | C3—C8—O3—Cd1 | −97.2 (2) |
C3—C4—C5—C6 | −0.2 (4) | O4iii—Cd1—O3—C8 | −93.2 (2) |
F1—C1—C6—C5 | 179.9 (2) | O5—Cd1—O3—C8 | 96.3 (2) |
C2—C1—C6—C5 | −0.4 (4) | O2i—Cd1—O3—C8 | 177.1 (2) |
C4—C5—C6—C1 | 0.4 (4) | O6—Cd1—O3—C8 | 2.1 (2) |
C1—C2—C7—O1 | −72.7 (3) | O2ii—Cd1—O3—C8 | 74.1 (3) |
C3—C2—C7—O1 | 110.0 (2) | O3—C8—O4—Cd1iii | −8.7 (3) |
C1—C2—C7—O2 | 105.1 (2) | C3—C8—O4—Cd1iii | 169.98 (13) |
C3—C2—C7—O2 | −72.2 (3) | | |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, y, z; (iii) −x+1, −y+2, −z+1; (iv) x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O4v | 0.77 (2) | 2.08 (2) | 2.840 (2) | 175 (3) |
O5—H5B···O1 | 0.76 (2) | 1.99 (2) | 2.749 (2) | 175 (4) |
O6—H6B···O1vi | 0.76 (2) | 2.04 (2) | 2.804 (2) | 179 (5) |
Symmetry codes: (v) x−1, y−1, z; (vi) x, y+1, z. |