Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807048787/im2036sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807048787/im2036Isup2.hkl |
CCDC reference: 667136
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.005 Å
- R factor = 0.025
- wR factor = 0.063
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.27 PLAT230_ALERT_2_C Hirshfeld Test Diff for O1 - C1 .. 5.92 su PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.44 From the CIF: _reflns_number_total 4825 Count of symmetry unique reflns 2872 Completeness (_total/calc) 168.00% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1953 Fraction of Friedel pairs measured 0.680 Are heavy atom types Z>Si present yes PLAT794_ALERT_5_G Check Predicted Bond Valency for Cd1 (2) 2.16 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For the zinc phenanthroline adduct, see Deng, Gao, Huo et al. (2006), and for the cadmium phenanthroline complex, see Deng, Gao & Ng (2006).
Cadmium(II) diacetate trihydrate (0.14 g, 0.5 mmol) was added to an H2O/EtOH solution (1:1 v/v) of 4-formylbenzoic acid (0.15 g, 1 mmol) and 1,10-phenanthroline (0.099 g 0.5 mmol). Sodium hydroxide (0.1 M) was added dropwise until the solution registered a pH of 5. Pale yellow single crystals separated from the filtered solution after several days. Elemental analysis: calcd. for C28H20N2O7Cd: C 55.23, H 3.31, N 4.60. Found: C 55.25, H 3.24, N 4.62.
Carbon-bound H atoms were placed in calculated positions, with C—H = 0.93 and Uiso(H) = 1.2Ueq (C), and were included in the refinement in the riding model approximation. The H atoms of water molecules were located in difference Fourier maps and refined with the O—H and H···H distance restraints to 0.85 (1) and 1.39 (1) Å, and with Uiso(H) = 1.5Ueq(O).
An earlier report (Deng et al., 2006a) detailed the synthesis and crystal structure of a zinc complex with 1,10-phenanthroline and 4-formylbenzoato ligands. Replacing zinc by cadmium in a similar reaction leads to the formation of the title complex, (I) (Fig. 1). The Cd(II) atom displays a trigonal prismatic geometry, which is different from the zinc complex and another cadmium phenanthroline adduct, (II) (Deng et al., 2006b). The two basal planes of the trigonal prism are built up by O1, O1, N2 and O2, O4, N1, respectively. The Cd—O and Cd—N bond lengths are similar to complex (II). Interestingly, one of the 4-formylbenzoato ligands shows a coordination to cadmium only via one of the oxygen atoms whereas the other oxygen atom is engaged in a strong intramolecular hydrogen bond toward the aqua ligand. Adjacent complex molecules are linked into a two-dimensional layer structure via hydrogen-bonding interactions (Table 1, Fig. 2).
For the zinc phenanthroline adduct, see Deng, Gao, Huo et al. (2006), and for the cadmium phenanthroline complex, see Deng, Gao & Ng (2006).
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); 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: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Cd(C8H5O3)2(C12H8N2)(H2O)] | F(000) = 612 |
Mr = 608.86 | Dx = 1.656 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 11052 reflections |
a = 6.357 (1) Å | θ = 3.2–27.4° |
b = 19.668 (4) Å | µ = 0.95 mm−1 |
c = 9.766 (2) Å | T = 295 K |
β = 90.11 (3)° | Prism, pale yellow |
V = 1221.0 (4) Å3 | 0.34 × 0.21 × 0.18 mm |
Z = 2 |
Rigaku R-AXIS RAPID diffractometer | 4825 independent reflections |
Radiation source: fine-focus sealed tube | 4537 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
Detector resolution: 10.000 pixels mm-1 | θmax = 27.4°, θmin = 3.2° |
ω scans | h = −8→8 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −25→21 |
Tmin = 0.739, Tmax = 0.848 | l = −12→12 |
11897 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)] = 0.025 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.063 | w = 1/[σ2(Fo2) + (0.0347P)2 + 0.1062P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max < 0.001 |
4825 reflections | Δρmax = 0.56 e Å−3 |
349 parameters | Δρmin = −0.25 e Å−3 |
4 restraints | Absolute structure: Flack (1983), from 1957 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.01 (2) |
[Cd(C8H5O3)2(C12H8N2)(H2O)] | V = 1221.0 (4) Å3 |
Mr = 608.86 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 6.357 (1) Å | µ = 0.95 mm−1 |
b = 19.668 (4) Å | T = 295 K |
c = 9.766 (2) Å | 0.34 × 0.21 × 0.18 mm |
β = 90.11 (3)° |
Rigaku R-AXIS RAPID diffractometer | 4825 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 4537 reflections with I > 2σ(I) |
Tmin = 0.739, Tmax = 0.848 | Rint = 0.024 |
11897 measured reflections |
R[F2 > 2σ(F2)] = 0.025 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.063 | Δρmax = 0.56 e Å−3 |
S = 1.05 | Δρmin = −0.25 e Å−3 |
4825 reflections | Absolute structure: Flack (1983), from 1957 Friedel pairs |
349 parameters | Absolute structure parameter: 0.01 (2) |
4 restraints |
x | y | z | Uiso*/Ueq | ||
Cd1 | 0.77987 (3) | 0.712516 (17) | 0.315510 (15) | 0.04216 (7) | |
O1W | 1.1049 (4) | 0.73572 (17) | 0.3948 (3) | 0.0812 (10) | |
H1W1 | 1.211 (7) | 0.709 (3) | 0.401 (5) | 0.122* | |
H1W2 | 1.074 (8) | 0.749 (3) | 0.476 (2) | 0.122* | |
O1 | 0.7527 (4) | 0.61002 (14) | 0.4439 (3) | 0.0509 (6) | |
O2 | 0.4560 (4) | 0.65579 (13) | 0.3778 (3) | 0.0565 (6) | |
O3 | 0.1403 (6) | 0.3939 (2) | 0.8716 (4) | 0.1075 (12) | |
O4 | 0.6851 (4) | 0.79973 (15) | 0.4452 (3) | 0.0553 (7) | |
O5 | 0.9706 (4) | 0.82545 (17) | 0.5680 (3) | 0.0810 (10) | |
O6 | 0.3252 (5) | 1.0274 (2) | 0.9929 (3) | 0.0981 (12) | |
N1 | 0.5860 (4) | 0.75318 (13) | 0.1303 (2) | 0.0437 (6) | |
N2 | 0.9394 (4) | 0.67398 (13) | 0.1142 (2) | 0.0424 (5) | |
C1 | 0.5570 (5) | 0.61234 (16) | 0.4443 (3) | 0.0413 (6) | |
C2 | 0.4344 (5) | 0.56143 (16) | 0.5297 (3) | 0.0404 (6) | |
C3 | 0.5283 (6) | 0.53018 (18) | 0.6406 (3) | 0.0462 (7) | |
H3 | 0.6674 | 0.5400 | 0.6627 | 0.055* | |
C4 | 0.4147 (6) | 0.48377 (18) | 0.7196 (4) | 0.0486 (8) | |
H4 | 0.4774 | 0.4634 | 0.7953 | 0.058* | |
C5 | 0.2109 (5) | 0.46823 (19) | 0.6856 (3) | 0.0478 (7) | |
C6 | 0.1167 (5) | 0.49958 (18) | 0.5737 (3) | 0.0491 (7) | |
H6 | −0.0210 | 0.4887 | 0.5501 | 0.059* | |
C7 | 0.2267 (5) | 0.54710 (16) | 0.4970 (3) | 0.0444 (6) | |
H7 | 0.1616 | 0.5692 | 0.4242 | 0.053* | |
C8 | 0.0849 (7) | 0.4194 (2) | 0.7671 (4) | 0.0691 (10) | |
H8 | −0.0476 | 0.4078 | 0.7340 | 0.083* | |
C9 | 0.7805 (5) | 0.83037 (17) | 0.5412 (3) | 0.0505 (7) | |
C10 | 0.6485 (6) | 0.87646 (16) | 0.6317 (3) | 0.0453 (7) | |
C11 | 0.7320 (5) | 0.90185 (18) | 0.7532 (3) | 0.0499 (7) | |
H11 | 0.8690 | 0.8909 | 0.7784 | 0.060* | |
C12 | 0.6124 (5) | 0.94315 (18) | 0.8366 (3) | 0.0528 (8) | |
H12 | 0.6685 | 0.9598 | 0.9180 | 0.063* | |
C13 | 0.4075 (5) | 0.95998 (17) | 0.7986 (4) | 0.0495 (7) | |
C14 | 0.3249 (6) | 0.93475 (19) | 0.6781 (4) | 0.0500 (8) | |
H14 | 0.1885 | 0.9461 | 0.6524 | 0.060* | |
C15 | 0.4445 (6) | 0.89241 (18) | 0.5951 (4) | 0.0480 (8) | |
H15 | 0.3871 | 0.8748 | 0.5149 | 0.058* | |
C16 | 0.2764 (7) | 1.0020 (2) | 0.8867 (5) | 0.0696 (11) | |
H16 | 0.1397 | 1.0100 | 0.8568 | 0.083* | |
C17 | 0.4134 (6) | 0.79067 (18) | 0.1388 (4) | 0.0572 (8) | |
H17 | 0.3730 | 0.8071 | 0.2241 | 0.069* | |
C18 | 0.2888 (6) | 0.8067 (2) | 0.0242 (5) | 0.0632 (10) | |
H18 | 0.1673 | 0.8325 | 0.0338 | 0.076* | |
C19 | 0.3491 (6) | 0.78362 (18) | −0.1008 (4) | 0.0582 (8) | |
H19 | 0.2690 | 0.7940 | −0.1778 | 0.070* | |
C20 | 0.5308 (5) | 0.74446 (15) | −0.1141 (3) | 0.0467 (7) | |
C21 | 0.6059 (6) | 0.7193 (3) | −0.2424 (3) | 0.0562 (8) | |
H21 | 0.5297 | 0.7282 | −0.3218 | 0.067* | |
C22 | 0.7857 (6) | 0.68279 (18) | −0.2503 (3) | 0.0565 (8) | |
H22 | 0.8318 | 0.6680 | −0.3355 | 0.068* | |
C23 | 0.9054 (5) | 0.66654 (16) | −0.1326 (3) | 0.0455 (7) | |
C24 | 1.0926 (6) | 0.62859 (17) | −0.1353 (3) | 0.0549 (8) | |
H24 | 1.1460 | 0.6134 | −0.2185 | 0.066* | |
C25 | 1.1962 (6) | 0.61390 (19) | −0.0170 (4) | 0.0575 (9) | |
H25 | 1.3195 | 0.5885 | −0.0186 | 0.069* | |
C26 | 1.1154 (5) | 0.63739 (18) | 0.1059 (3) | 0.0510 (7) | |
H26 | 1.1872 | 0.6271 | 0.1863 | 0.061* | |
C27 | 0.8340 (5) | 0.68927 (14) | −0.0025 (3) | 0.0389 (6) | |
C28 | 0.6459 (5) | 0.72926 (13) | 0.0058 (3) | 0.0399 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.04758 (10) | 0.04581 (11) | 0.03311 (9) | −0.00347 (12) | 0.00606 (6) | −0.00381 (13) |
O1W | 0.0490 (14) | 0.102 (2) | 0.0932 (19) | 0.0088 (13) | −0.0024 (13) | −0.0504 (17) |
O1 | 0.0371 (12) | 0.0630 (16) | 0.0527 (14) | −0.0030 (11) | 0.0002 (10) | 0.0125 (12) |
O2 | 0.0487 (13) | 0.0534 (14) | 0.0675 (14) | 0.0010 (10) | 0.0033 (11) | 0.0188 (12) |
O3 | 0.102 (3) | 0.120 (3) | 0.100 (3) | −0.027 (2) | 0.006 (2) | 0.045 (2) |
O4 | 0.0585 (17) | 0.0584 (16) | 0.0489 (13) | 0.0005 (13) | −0.0046 (12) | −0.0139 (11) |
O5 | 0.0510 (15) | 0.095 (2) | 0.097 (2) | −0.0037 (14) | 0.0073 (14) | −0.0544 (19) |
O6 | 0.087 (2) | 0.116 (3) | 0.091 (2) | 0.032 (2) | −0.0099 (17) | −0.058 (2) |
N1 | 0.0517 (14) | 0.0401 (13) | 0.0393 (12) | 0.0007 (11) | 0.0097 (10) | 0.0020 (10) |
N2 | 0.0485 (14) | 0.0406 (13) | 0.0381 (12) | −0.0036 (11) | 0.0051 (10) | −0.0012 (10) |
C1 | 0.0498 (17) | 0.0401 (15) | 0.0339 (13) | −0.0004 (13) | 0.0027 (12) | −0.0038 (12) |
C2 | 0.0404 (15) | 0.0406 (16) | 0.0401 (14) | 0.0019 (12) | 0.0044 (12) | −0.0039 (12) |
C3 | 0.0381 (18) | 0.0547 (19) | 0.0460 (17) | −0.0008 (14) | −0.0046 (14) | 0.0011 (15) |
C4 | 0.0498 (19) | 0.052 (2) | 0.0441 (17) | 0.0009 (15) | −0.0026 (14) | 0.0085 (15) |
C5 | 0.0509 (19) | 0.0442 (18) | 0.0482 (17) | −0.0007 (14) | 0.0061 (14) | −0.0020 (13) |
C6 | 0.0419 (16) | 0.0565 (19) | 0.0489 (16) | −0.0082 (13) | −0.0008 (13) | −0.0018 (14) |
C7 | 0.0418 (15) | 0.0490 (16) | 0.0424 (14) | −0.0003 (13) | −0.0020 (11) | 0.0007 (13) |
C8 | 0.071 (3) | 0.071 (3) | 0.066 (2) | −0.014 (2) | 0.0047 (19) | 0.016 (2) |
C9 | 0.058 (2) | 0.0454 (18) | 0.0481 (17) | −0.0082 (14) | 0.0107 (14) | −0.0070 (14) |
C10 | 0.0492 (18) | 0.0404 (16) | 0.0464 (15) | −0.0092 (13) | 0.0018 (14) | −0.0046 (13) |
C11 | 0.0489 (17) | 0.0514 (18) | 0.0494 (17) | 0.0017 (14) | −0.0025 (13) | −0.0106 (15) |
C12 | 0.0541 (19) | 0.0557 (19) | 0.0484 (17) | 0.0035 (15) | −0.0063 (14) | −0.0149 (15) |
C13 | 0.0521 (18) | 0.0422 (16) | 0.0542 (18) | 0.0016 (14) | 0.0006 (14) | −0.0065 (15) |
C14 | 0.045 (2) | 0.053 (2) | 0.0516 (19) | 0.0052 (15) | −0.0092 (15) | −0.0007 (15) |
C15 | 0.051 (2) | 0.0509 (19) | 0.0417 (17) | −0.0057 (15) | −0.0059 (14) | −0.0044 (15) |
C16 | 0.060 (2) | 0.071 (3) | 0.078 (3) | 0.0143 (19) | −0.0025 (19) | −0.026 (2) |
C17 | 0.065 (2) | 0.0492 (18) | 0.0573 (19) | 0.0038 (16) | 0.0151 (16) | 0.0040 (16) |
C18 | 0.055 (2) | 0.051 (2) | 0.083 (3) | 0.0109 (18) | 0.0106 (19) | 0.0154 (19) |
C19 | 0.063 (2) | 0.0502 (19) | 0.062 (2) | −0.0018 (16) | −0.0046 (16) | 0.0161 (16) |
C20 | 0.0604 (19) | 0.0378 (15) | 0.0417 (14) | −0.0101 (14) | −0.0002 (13) | 0.0074 (12) |
C21 | 0.081 (2) | 0.051 (2) | 0.0364 (11) | −0.010 (2) | −0.0048 (12) | 0.0092 (18) |
C22 | 0.082 (2) | 0.0528 (18) | 0.0348 (14) | −0.0080 (17) | 0.0051 (14) | −0.0051 (13) |
C23 | 0.0585 (18) | 0.0381 (15) | 0.0399 (14) | −0.0081 (13) | 0.0110 (13) | −0.0037 (12) |
C24 | 0.067 (2) | 0.0455 (18) | 0.0519 (17) | −0.0034 (15) | 0.0189 (15) | −0.0102 (15) |
C25 | 0.057 (2) | 0.0475 (19) | 0.068 (2) | 0.0011 (17) | 0.0150 (18) | −0.0067 (17) |
C26 | 0.0498 (18) | 0.0514 (18) | 0.0519 (17) | 0.0006 (14) | 0.0034 (13) | −0.0008 (15) |
C27 | 0.0488 (16) | 0.0327 (13) | 0.0351 (12) | −0.0090 (10) | 0.0049 (11) | −0.0009 (10) |
C28 | 0.0488 (15) | 0.0327 (17) | 0.0382 (12) | −0.0085 (10) | 0.0053 (10) | 0.0022 (10) |
Cd1—O1 | 2.381 (3) | C10—C15 | 1.381 (5) |
Cd1—O2 | 2.420 (2) | C10—C11 | 1.392 (5) |
Cd1—O1W | 2.252 (3) | C11—C12 | 1.379 (5) |
Cd1—O4 | 2.216 (3) | C11—H11 | 0.9300 |
Cd1—N1 | 2.328 (3) | C12—C13 | 1.394 (5) |
Cd1—N2 | 2.340 (2) | C12—H12 | 0.9300 |
Cd1—C1 | 2.735 (3) | C13—C14 | 1.380 (5) |
O1W—H1W1 | 0.86 (5) | C13—C16 | 1.457 (5) |
O1W—H1W2 | 0.86 (3) | C14—C15 | 1.390 (5) |
O1—C1 | 1.245 (4) | C14—H14 | 0.9300 |
O2—C1 | 1.250 (4) | C15—H15 | 0.9300 |
O3—C8 | 1.190 (5) | C16—H16 | 0.9300 |
O4—C9 | 1.268 (4) | C17—C18 | 1.406 (6) |
O5—C9 | 1.239 (4) | C17—H17 | 0.9300 |
O6—C16 | 1.191 (5) | C18—C19 | 1.358 (6) |
N1—C17 | 1.324 (4) | C18—H18 | 0.9300 |
N1—C28 | 1.359 (3) | C19—C20 | 1.395 (5) |
N2—C26 | 1.333 (4) | C19—H19 | 0.9300 |
N2—C27 | 1.355 (4) | C20—C28 | 1.412 (4) |
C1—C2 | 1.519 (4) | C20—C21 | 1.430 (4) |
C2—C3 | 1.380 (4) | C21—C22 | 1.352 (6) |
C2—C7 | 1.387 (4) | C21—H21 | 0.9300 |
C3—C4 | 1.397 (5) | C22—C23 | 1.414 (5) |
C3—H3 | 0.9300 | C22—H22 | 0.9300 |
C4—C5 | 1.371 (5) | C23—C24 | 1.405 (5) |
C4—H4 | 0.9300 | C23—C27 | 1.422 (4) |
C5—C6 | 1.389 (5) | C24—C25 | 1.360 (6) |
C5—C8 | 1.483 (5) | C24—H24 | 0.9300 |
C6—C7 | 1.388 (5) | C25—C26 | 1.386 (5) |
C6—H6 | 0.9300 | C25—H25 | 0.9300 |
C7—H7 | 0.9300 | C26—H26 | 0.9300 |
C8—H8 | 0.9300 | C27—C28 | 1.434 (4) |
C9—C10 | 1.520 (5) | ||
O4—Cd1—O1W | 84.07 (10) | O5—C9—O4 | 125.7 (3) |
O4—Cd1—N1 | 91.94 (10) | O5—C9—C10 | 117.6 (3) |
O1W—Cd1—N1 | 132.97 (11) | O4—C9—C10 | 116.7 (3) |
O4—Cd1—N2 | 148.15 (10) | C15—C10—C11 | 119.7 (3) |
O1W—Cd1—N2 | 87.48 (9) | C15—C10—C9 | 120.3 (3) |
N1—Cd1—N2 | 71.84 (9) | C11—C10—C9 | 120.0 (3) |
O4—Cd1—O1 | 109.54 (9) | C12—C11—C10 | 120.3 (3) |
O1W—Cd1—O1 | 93.32 (11) | C12—C11—H11 | 119.8 |
N1—Cd1—O1 | 131.38 (9) | C10—C11—H11 | 119.8 |
N2—Cd1—O1 | 101.55 (9) | C11—C12—C13 | 119.9 (3) |
O4—Cd1—O2 | 88.91 (10) | C11—C12—H12 | 120.0 |
O1W—Cd1—O2 | 141.94 (10) | C13—C12—H12 | 120.0 |
N1—Cd1—O2 | 84.49 (9) | C14—C13—C12 | 119.7 (3) |
N2—Cd1—O2 | 115.59 (9) | C14—C13—C16 | 119.4 (3) |
O1—Cd1—O2 | 54.18 (8) | C12—C13—C16 | 120.9 (3) |
O4—Cd1—C1 | 98.82 (10) | C13—C14—C15 | 120.4 (3) |
O1W—Cd1—C1 | 117.62 (12) | C13—C14—H14 | 119.8 |
N1—Cd1—C1 | 109.32 (9) | C15—C14—H14 | 119.8 |
N2—Cd1—C1 | 112.26 (9) | C10—C15—C14 | 120.0 (3) |
O1—Cd1—C1 | 27.05 (9) | C10—C15—H15 | 120.0 |
O2—Cd1—C1 | 27.21 (9) | C14—C15—H15 | 120.0 |
Cd1—O1W—H1W1 | 128 (4) | O6—C16—C13 | 127.2 (4) |
Cd1—O1W—H1W2 | 100 (4) | O6—C16—H16 | 116.4 |
H1W1—O1W—H1W2 | 108 (5) | C13—C16—H16 | 116.4 |
C1—O1—Cd1 | 92.5 (2) | N1—C17—C18 | 122.7 (3) |
C1—O2—Cd1 | 90.5 (2) | N1—C17—H17 | 118.6 |
C9—O4—Cd1 | 131.3 (3) | C18—C17—H17 | 118.6 |
C17—N1—C28 | 118.8 (3) | C19—C18—C17 | 118.8 (4) |
C17—N1—Cd1 | 125.5 (2) | C19—C18—H18 | 120.6 |
C28—N1—Cd1 | 115.28 (19) | C17—C18—H18 | 120.6 |
C26—N2—C27 | 118.8 (3) | C18—C19—C20 | 120.2 (3) |
C26—N2—Cd1 | 126.2 (2) | C18—C19—H19 | 119.9 |
C27—N2—Cd1 | 114.89 (19) | C20—C19—H19 | 119.9 |
O1—C1—O2 | 122.4 (3) | C19—C20—C28 | 117.9 (3) |
O1—C1—C2 | 119.4 (3) | C19—C20—C21 | 123.4 (3) |
O2—C1—C2 | 118.2 (3) | C28—C20—C21 | 118.7 (3) |
O1—C1—Cd1 | 60.42 (18) | C22—C21—C20 | 121.2 (3) |
O2—C1—Cd1 | 62.26 (17) | C22—C21—H21 | 119.4 |
C2—C1—Cd1 | 173.8 (2) | C20—C21—H21 | 119.4 |
C3—C2—C7 | 120.0 (3) | C21—C22—C23 | 121.8 (3) |
C3—C2—C1 | 120.2 (3) | C21—C22—H22 | 119.1 |
C7—C2—C1 | 119.8 (3) | C23—C22—H22 | 119.1 |
C2—C3—C4 | 120.1 (3) | C24—C23—C22 | 124.0 (3) |
C2—C3—H3 | 120.0 | C24—C23—C27 | 117.1 (3) |
C4—C3—H3 | 120.0 | C22—C23—C27 | 118.9 (3) |
C5—C4—C3 | 120.0 (3) | C25—C24—C23 | 120.4 (3) |
C5—C4—H4 | 120.0 | C25—C24—H24 | 119.8 |
C3—C4—H4 | 120.0 | C23—C24—H24 | 119.8 |
C4—C5—C6 | 119.8 (3) | C24—C25—C26 | 119.0 (4) |
C4—C5—C8 | 121.7 (3) | C24—C25—H25 | 120.5 |
C6—C5—C8 | 118.5 (3) | C26—C25—H25 | 120.5 |
C7—C6—C5 | 120.4 (3) | N2—C26—C25 | 123.0 (3) |
C7—C6—H6 | 119.8 | N2—C26—H26 | 118.5 |
C5—C6—H6 | 119.8 | C25—C26—H26 | 118.5 |
C2—C7—C6 | 119.6 (3) | N2—C27—C23 | 121.6 (3) |
C2—C7—H7 | 120.2 | N2—C27—C28 | 119.0 (2) |
C6—C7—H7 | 120.2 | C23—C27—C28 | 119.4 (3) |
O3—C8—C5 | 125.0 (4) | N1—C28—C20 | 121.6 (3) |
O3—C8—H8 | 117.5 | N1—C28—C27 | 118.4 (3) |
C5—C8—H8 | 117.5 | C20—C28—C27 | 120.0 (2) |
O4—Cd1—O1—C1 | 70.3 (2) | C4—C5—C6—C7 | −0.7 (5) |
O1W—Cd1—O1—C1 | 155.2 (2) | C8—C5—C6—C7 | 178.1 (3) |
N1—Cd1—O1—C1 | −40.9 (2) | C3—C2—C7—C6 | −2.1 (4) |
N2—Cd1—O1—C1 | −116.7 (2) | C1—C2—C7—C6 | 178.7 (3) |
O2—Cd1—O1—C1 | −3.40 (18) | C5—C6—C7—C2 | 2.3 (5) |
O4—Cd1—O2—C1 | −111.9 (2) | C4—C5—C8—O3 | 5.8 (7) |
O1W—Cd1—O2—C1 | −32.9 (3) | C6—C5—C8—O3 | −173.0 (5) |
N1—Cd1—O2—C1 | 156.09 (19) | Cd1—O4—C9—O5 | 14.3 (6) |
N2—Cd1—O2—C1 | 89.3 (2) | Cd1—O4—C9—C10 | −165.0 (2) |
O1—Cd1—O2—C1 | 3.38 (18) | O5—C9—C10—C15 | 169.9 (3) |
O1W—Cd1—O4—C9 | −15.6 (3) | O4—C9—C10—C15 | −10.7 (5) |
N1—Cd1—O4—C9 | −148.6 (3) | O5—C9—C10—C11 | −11.1 (5) |
N2—Cd1—O4—C9 | −91.0 (4) | O4—C9—C10—C11 | 168.2 (3) |
O1—Cd1—O4—C9 | 75.9 (3) | C15—C10—C11—C12 | −0.4 (5) |
O2—Cd1—O4—C9 | 127.0 (3) | C9—C10—C11—C12 | −179.4 (3) |
C1—Cd1—O4—C9 | 101.5 (3) | C10—C11—C12—C13 | −0.4 (5) |
O4—Cd1—N1—C17 | −29.0 (3) | C11—C12—C13—C14 | 0.5 (5) |
O1W—Cd1—N1—C17 | −112.7 (3) | C11—C12—C13—C16 | 178.4 (4) |
N2—Cd1—N1—C17 | 179.0 (3) | C12—C13—C14—C15 | 0.4 (5) |
O1—Cd1—N1—C17 | 89.5 (3) | C16—C13—C14—C15 | −177.6 (4) |
O2—Cd1—N1—C17 | 59.8 (3) | C11—C10—C15—C14 | 1.3 (5) |
C1—Cd1—N1—C17 | 71.1 (3) | C9—C10—C15—C14 | −179.8 (3) |
O4—Cd1—N1—C28 | 158.7 (2) | C13—C14—C15—C10 | −1.3 (5) |
O1W—Cd1—N1—C28 | 75.0 (2) | C14—C13—C16—O6 | −179.9 (5) |
N2—Cd1—N1—C28 | 6.61 (19) | C12—C13—C16—O6 | 2.2 (7) |
O1—Cd1—N1—C28 | −82.9 (2) | C28—N1—C17—C18 | 0.2 (5) |
O2—Cd1—N1—C28 | −112.6 (2) | Cd1—N1—C17—C18 | −171.9 (3) |
C1—Cd1—N1—C28 | −101.3 (2) | N1—C17—C18—C19 | −1.0 (6) |
O4—Cd1—N2—C26 | 115.0 (3) | C17—C18—C19—C20 | 0.4 (6) |
O1W—Cd1—N2—C26 | 40.4 (3) | C18—C19—C20—C28 | 0.8 (5) |
N1—Cd1—N2—C26 | 177.5 (3) | C18—C19—C20—C21 | −179.0 (4) |
O1—Cd1—N2—C26 | −52.4 (3) | C19—C20—C21—C22 | 178.5 (4) |
O2—Cd1—N2—C26 | −108.1 (3) | C28—C20—C21—C22 | −1.3 (6) |
C1—Cd1—N2—C26 | −78.5 (3) | C20—C21—C22—C23 | 1.3 (6) |
O4—Cd1—N2—C27 | −67.5 (3) | C21—C22—C23—C24 | 179.8 (4) |
O1W—Cd1—N2—C27 | −142.1 (2) | C21—C22—C23—C27 | 0.1 (5) |
N1—Cd1—N2—C27 | −4.96 (19) | C22—C23—C24—C25 | −178.6 (3) |
O1—Cd1—N2—C27 | 125.07 (19) | C27—C23—C24—C25 | 1.1 (5) |
O2—Cd1—N2—C27 | 69.4 (2) | C23—C24—C25—C26 | −0.5 (5) |
C1—Cd1—N2—C27 | 99.0 (2) | C27—N2—C26—C25 | −0.2 (5) |
Cd1—O1—C1—O2 | 6.3 (3) | Cd1—N2—C26—C25 | 177.2 (3) |
Cd1—O1—C1—C2 | −172.9 (2) | C24—C25—C26—N2 | 0.0 (6) |
Cd1—O2—C1—O1 | −6.2 (3) | C26—N2—C27—C23 | 0.8 (4) |
Cd1—O2—C1—C2 | 173.0 (2) | Cd1—N2—C27—C23 | −176.9 (2) |
O4—Cd1—C1—O1 | −116.14 (19) | C26—N2—C27—C28 | −179.3 (3) |
O1W—Cd1—C1—O1 | −28.2 (2) | Cd1—N2—C27—C28 | 3.0 (3) |
N1—Cd1—C1—O1 | 148.7 (2) | C24—C23—C27—N2 | −1.2 (4) |
N2—Cd1—C1—O1 | 71.0 (2) | C22—C23—C27—N2 | 178.5 (3) |
O2—Cd1—C1—O1 | 174.0 (3) | C24—C23—C27—C28 | 178.9 (3) |
O4—Cd1—C1—O2 | 69.9 (2) | C22—C23—C27—C28 | −1.4 (4) |
O1W—Cd1—C1—O2 | 157.79 (18) | C17—N1—C28—C20 | 1.1 (4) |
N1—Cd1—C1—O2 | −25.3 (2) | Cd1—N1—C28—C20 | 174.1 (2) |
N2—Cd1—C1—O2 | −103.0 (2) | C17—N1—C28—C27 | 179.4 (3) |
O1—Cd1—C1—O2 | −174.0 (3) | Cd1—N1—C28—C27 | −7.7 (3) |
O1—C1—C2—C3 | 23.3 (4) | C19—C20—C28—N1 | −1.6 (4) |
O2—C1—C2—C3 | −155.9 (3) | C21—C20—C28—N1 | 178.2 (3) |
O1—C1—C2—C7 | −157.6 (3) | C19—C20—C28—C27 | −179.9 (3) |
O2—C1—C2—C7 | 23.2 (4) | C21—C20—C28—C27 | 0.0 (4) |
C7—C2—C3—C4 | 0.4 (5) | N2—C27—C28—N1 | 3.2 (4) |
C1—C2—C3—C4 | 179.5 (3) | C23—C27—C28—N1 | −176.9 (3) |
C2—C3—C4—C5 | 1.2 (5) | N2—C27—C28—C20 | −178.5 (3) |
C3—C4—C5—C6 | −1.1 (5) | C23—C27—C28—C20 | 1.4 (4) |
C3—C4—C5—C8 | −179.8 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2i | 0.86 (5) | 1.89 (5) | 2.735 (4) | 168 (5) |
O1W—H1W2···O5 | 0.86 (5) | 1.88 (3) | 2.590 (4) | 140 (5) |
Symmetry code: (i) x+1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C8H5O3)2(C12H8N2)(H2O)] |
Mr | 608.86 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 295 |
a, b, c (Å) | 6.357 (1), 19.668 (4), 9.766 (2) |
β (°) | 90.11 (3) |
V (Å3) | 1221.0 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.95 |
Crystal size (mm) | 0.34 × 0.21 × 0.18 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.739, 0.848 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11897, 4825, 4537 |
Rint | 0.024 |
(sin θ/λ)max (Å−1) | 0.648 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.063, 1.05 |
No. of reflections | 4825 |
No. of parameters | 349 |
No. of restraints | 4 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.56, −0.25 |
Absolute structure | Flack (1983), from 1957 Friedel pairs |
Absolute structure parameter | 0.01 (2) |
Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2i | 0.86 (5) | 1.89 (5) | 2.735 (4) | 168 (5) |
O1W—H1W2···O5 | 0.86 (5) | 1.88 (3) | 2.590 (4) | 140 (5) |
Symmetry code: (i) x+1, y, z. |
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An earlier report (Deng et al., 2006a) detailed the synthesis and crystal structure of a zinc complex with 1,10-phenanthroline and 4-formylbenzoato ligands. Replacing zinc by cadmium in a similar reaction leads to the formation of the title complex, (I) (Fig. 1). The Cd(II) atom displays a trigonal prismatic geometry, which is different from the zinc complex and another cadmium phenanthroline adduct, (II) (Deng et al., 2006b). The two basal planes of the trigonal prism are built up by O1, O1, N2 and O2, O4, N1, respectively. The Cd—O and Cd—N bond lengths are similar to complex (II). Interestingly, one of the 4-formylbenzoato ligands shows a coordination to cadmium only via one of the oxygen atoms whereas the other oxygen atom is engaged in a strong intramolecular hydrogen bond toward the aqua ligand. Adjacent complex molecules are linked into a two-dimensional layer structure via hydrogen-bonding interactions (Table 1, Fig. 2).