Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680705115X/ng2340sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680705115X/ng2340Isup2.hkl |
CCDC reference: 667208
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.004 Å
- R factor = 0.028
- wR factor = 0.066
- Data-to-parameter ratio = 16.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O1 .. 15.57 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O4 .. 13.29 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O5 .. 16.58 su
Alert level C PLAT230_ALERT_2_C Hirshfeld Test Diff for O2 - C1 .. 5.08 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O5 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd1 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Cd1 (2) 2.06 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 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 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
Cadmium(II) diacetate dihydrate (2.66 g, 10 mmol) was added to an H2O/EtOH solution (1:1 v/v) of 4-formylbenzoic acid (3.00 g, 20 mmol) and 2,2'-bipydine (1.56 g, 10 mmol). Sodium hydroxide (0.1 M) was added dropwise until the solution registered a pH of 5. Colorless single crystals separated from the filtered solution after several days. CH&N analysis. Calc. for C26H22N2O8Cd: C 51.80, H 3.68, N 4.65. Found: C 51.85, H 3.64, N 4.61.
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., 2007) detailed the crystal structure of cadmium phenanthroline adduct of 4-FBAH; the CdII atom is six-coordinated and the 4-FBA- ligands act in both monodendate and chelating modes. Replacing the N-heterocycle by 2,2'-bipy furnishes the title compound as a monohydrated complex (Fig. 1) whose metal centre is seven-coordinate. It displays a mono-capped triangonal prismatic geometry (Fig. 2). The 4-FBA- ligand is chelating. Hydrogen-bonding interactions between the water molecules and O atoms of 4-FBA- ligands link the mononuclear complex into a chain structure along the b axis (Fig.3).
For the related cadmium phenanthroline adduct, see Deng et al. (2007).
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(C10H8N2)(H2O)]·H2O | F(000) = 1216 |
Mr = 602.86 | Dx = 1.610 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 18668 reflections |
a = 23.878 (5) Å | θ = 3.1–27.4° |
b = 6.3586 (13) Å | µ = 0.93 mm−1 |
c = 17.048 (3) Å | T = 295 K |
β = 106.10 (3)° | Prism, colourless |
V = 2486.8 (9) Å3 | 0.28 × 0.21 × 0.16 mm |
Z = 4 |
Rigaku R-AXIS RAPID diffractometer | 5636 independent reflections |
Radiation source: fine-focus sealed tube | 4810 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
Detector resolution: 10.000 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
ω scans | h = −30→30 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −8→8 |
Tmin = 0.780, Tmax = 0.865 | l = −22→20 |
22518 measured reflections |
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.066 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0255P)2 + 1.4537P] where P = (Fo2 + 2Fc2)/3 |
5636 reflections | (Δ/σ)max = 0.002 |
346 parameters | Δρmax = 0.56 e Å−3 |
6 restraints | Δρmin = −0.34 e Å−3 |
[Cd(C8H5O3)2(C10H8N2)(H2O)]·H2O | V = 2486.8 (9) Å3 |
Mr = 602.86 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 23.878 (5) Å | µ = 0.93 mm−1 |
b = 6.3586 (13) Å | T = 295 K |
c = 17.048 (3) Å | 0.28 × 0.21 × 0.16 mm |
β = 106.10 (3)° |
Rigaku R-AXIS RAPID diffractometer | 5636 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 4810 reflections with I > 2σ(I) |
Tmin = 0.780, Tmax = 0.865 | Rint = 0.030 |
22518 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 6 restraints |
wR(F2) = 0.066 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | Δρmax = 0.56 e Å−3 |
5636 reflections | Δρmin = −0.34 e Å−3 |
346 parameters |
x | y | z | Uiso*/Ueq | ||
Cd1 | 0.761606 (7) | 0.55282 (2) | 0.604765 (9) | 0.03165 (6) | |
O1W | 0.76278 (8) | 0.2404 (3) | 0.67240 (12) | 0.0517 (5) | |
H1W1 | 0.7304 (7) | 0.194 (4) | 0.676 (2) | 0.078* | |
H1W2 | 0.7864 (9) | 0.140 (3) | 0.674 (2) | 0.078* | |
O2W | 0.67003 (10) | 0.0390 (3) | 0.69629 (17) | 0.0674 (6) | |
H2W1 | 0.6537 (17) | 0.045 (5) | 0.7343 (18) | 0.101* | |
H2W2 | 0.6727 (17) | −0.088 (2) | 0.682 (2) | 0.101* | |
O1 | 0.65529 (8) | 0.4099 (3) | 0.54083 (12) | 0.0519 (5) | |
O2 | 0.67947 (7) | 0.6319 (3) | 0.64420 (11) | 0.0473 (4) | |
O3 | 0.39562 (10) | 0.5381 (4) | 0.68703 (16) | 0.0770 (7) | |
O4 | 0.85797 (9) | 0.5509 (3) | 0.69981 (13) | 0.0623 (6) | |
O5 | 0.81462 (7) | 0.8555 (3) | 0.67383 (12) | 0.0557 (5) | |
O6 | 1.06983 (12) | 1.3180 (4) | 0.92916 (16) | 0.0933 (8) | |
N1 | 0.73508 (8) | 0.7714 (3) | 0.48969 (11) | 0.0349 (4) | |
N2 | 0.79677 (8) | 0.4103 (3) | 0.50210 (11) | 0.0330 (4) | |
C1 | 0.64311 (10) | 0.5109 (4) | 0.59560 (15) | 0.0406 (5) | |
C2 | 0.58314 (10) | 0.4899 (4) | 0.60830 (15) | 0.0419 (5) | |
C3 | 0.56186 (12) | 0.6386 (6) | 0.6514 (2) | 0.0678 (9) | |
H3 | 0.5846 | 0.7547 | 0.6728 | 0.081* | |
C4 | 0.50721 (13) | 0.6178 (6) | 0.6633 (2) | 0.0691 (9) | |
H4 | 0.4935 | 0.7196 | 0.6925 | 0.083* | |
C5 | 0.47330 (11) | 0.4472 (5) | 0.63218 (17) | 0.0489 (6) | |
C6 | 0.49400 (12) | 0.2990 (5) | 0.5880 (2) | 0.0605 (8) | |
H6 | 0.4710 | 0.1836 | 0.5662 | 0.073* | |
C7 | 0.54863 (11) | 0.3205 (5) | 0.57593 (18) | 0.0541 (7) | |
H7 | 0.5621 | 0.2201 | 0.5458 | 0.065* | |
C8 | 0.41517 (12) | 0.4242 (5) | 0.6460 (2) | 0.0630 (8) | |
H8 | 0.3922 | 0.3121 | 0.6207 | 0.076* | |
C9 | 0.85734 (10) | 0.7444 (4) | 0.70981 (14) | 0.0405 (5) | |
C10 | 0.90945 (9) | 0.8480 (4) | 0.76737 (14) | 0.0361 (5) | |
C11 | 0.92337 (11) | 1.0556 (4) | 0.75503 (16) | 0.0423 (5) | |
H11 | 0.9002 | 1.1316 | 0.7114 | 0.051* | |
C12 | 0.97161 (11) | 1.1490 (4) | 0.80751 (16) | 0.0465 (6) | |
H12 | 0.9812 | 1.2870 | 0.7986 | 0.056* | |
C13 | 1.00575 (10) | 1.0371 (4) | 0.87349 (17) | 0.0457 (6) | |
C14 | 0.99173 (11) | 0.8306 (4) | 0.88568 (17) | 0.0513 (6) | |
H14 | 1.0145 | 0.7553 | 0.9298 | 0.062* | |
C15 | 0.94405 (11) | 0.7359 (4) | 0.83257 (16) | 0.0454 (6) | |
H15 | 0.9352 | 0.5966 | 0.8406 | 0.054* | |
C16 | 1.05622 (13) | 1.1379 (6) | 0.9315 (2) | 0.0645 (8) | |
H16 | 1.0792 | 1.0548 | 0.9730 | 0.077* | |
C17 | 0.70356 (11) | 0.9470 (4) | 0.48623 (16) | 0.0429 (5) | |
H17 | 0.6942 | 0.9908 | 0.5331 | 0.051* | |
C18 | 0.68434 (12) | 1.0655 (4) | 0.41651 (17) | 0.0494 (6) | |
H18 | 0.6624 | 1.1865 | 0.4161 | 0.059* | |
C19 | 0.69833 (13) | 1.0009 (4) | 0.34751 (17) | 0.0500 (6) | |
H19 | 0.6857 | 1.0774 | 0.2993 | 0.060* | |
C20 | 0.73139 (11) | 0.8216 (4) | 0.35019 (14) | 0.0438 (6) | |
H20 | 0.7416 | 0.7768 | 0.3040 | 0.053* | |
C21 | 0.74927 (9) | 0.7089 (3) | 0.42260 (13) | 0.0325 (4) | |
C22 | 0.78480 (9) | 0.5124 (3) | 0.43018 (13) | 0.0311 (4) | |
C23 | 0.80441 (11) | 0.4359 (4) | 0.36645 (15) | 0.0428 (6) | |
H23 | 0.7964 | 0.5092 | 0.3174 | 0.051* | |
C24 | 0.83584 (11) | 0.2510 (4) | 0.37576 (16) | 0.0472 (6) | |
H24 | 0.8485 | 0.1972 | 0.3329 | 0.057* | |
C25 | 0.84809 (11) | 0.1478 (4) | 0.44941 (15) | 0.0451 (6) | |
H25 | 0.8696 | 0.0237 | 0.4576 | 0.054* | |
C26 | 0.82783 (10) | 0.2323 (4) | 0.51076 (14) | 0.0408 (5) | |
H26 | 0.8361 | 0.1624 | 0.5606 | 0.049* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.03319 (9) | 0.03734 (9) | 0.02606 (8) | −0.00243 (7) | 0.01094 (6) | −0.00048 (7) |
O1W | 0.0478 (10) | 0.0509 (10) | 0.0589 (11) | −0.0039 (8) | 0.0190 (9) | 0.0167 (10) |
O2W | 0.0700 (14) | 0.0525 (11) | 0.0972 (19) | −0.0107 (11) | 0.0524 (13) | −0.0017 (12) |
O1 | 0.0484 (10) | 0.0616 (11) | 0.0518 (11) | −0.0034 (9) | 0.0242 (8) | −0.0124 (9) |
O2 | 0.0363 (8) | 0.0622 (11) | 0.0465 (10) | −0.0096 (8) | 0.0167 (7) | −0.0118 (9) |
O3 | 0.0558 (13) | 0.1004 (18) | 0.0884 (18) | 0.0093 (12) | 0.0427 (12) | 0.0183 (14) |
O4 | 0.0636 (12) | 0.0451 (11) | 0.0648 (13) | −0.0172 (9) | −0.0045 (10) | −0.0019 (10) |
O5 | 0.0371 (9) | 0.0670 (12) | 0.0555 (11) | 0.0047 (9) | 0.0004 (8) | −0.0118 (10) |
O6 | 0.0939 (18) | 0.0898 (18) | 0.0856 (18) | −0.0442 (16) | 0.0074 (14) | −0.0313 (15) |
N1 | 0.0409 (10) | 0.0330 (9) | 0.0307 (9) | 0.0005 (8) | 0.0098 (8) | −0.0010 (8) |
N2 | 0.0357 (9) | 0.0369 (10) | 0.0266 (9) | 0.0004 (8) | 0.0090 (7) | 0.0026 (8) |
C1 | 0.0372 (12) | 0.0481 (13) | 0.0396 (13) | 0.0018 (10) | 0.0160 (10) | 0.0017 (11) |
C2 | 0.0337 (11) | 0.0537 (14) | 0.0391 (13) | −0.0040 (11) | 0.0115 (10) | −0.0035 (11) |
C3 | 0.0487 (15) | 0.082 (2) | 0.082 (2) | −0.0246 (16) | 0.0342 (15) | −0.0409 (19) |
C4 | 0.0489 (16) | 0.091 (2) | 0.077 (2) | −0.0111 (16) | 0.0333 (15) | −0.0319 (19) |
C5 | 0.0356 (12) | 0.0637 (17) | 0.0491 (15) | −0.0037 (12) | 0.0147 (11) | 0.0068 (13) |
C6 | 0.0457 (15) | 0.0585 (17) | 0.078 (2) | −0.0136 (13) | 0.0180 (14) | −0.0069 (16) |
C7 | 0.0466 (14) | 0.0538 (16) | 0.0648 (17) | −0.0038 (13) | 0.0202 (13) | −0.0095 (14) |
C8 | 0.0416 (14) | 0.076 (2) | 0.073 (2) | −0.0041 (14) | 0.0192 (14) | 0.0151 (17) |
C9 | 0.0381 (12) | 0.0498 (14) | 0.0348 (12) | −0.0104 (11) | 0.0121 (10) | −0.0062 (11) |
C10 | 0.0325 (11) | 0.0389 (12) | 0.0377 (11) | −0.0019 (10) | 0.0113 (9) | −0.0044 (11) |
C11 | 0.0407 (12) | 0.0415 (13) | 0.0433 (13) | 0.0003 (11) | 0.0095 (10) | 0.0011 (11) |
C12 | 0.0462 (13) | 0.0380 (12) | 0.0572 (15) | −0.0073 (11) | 0.0176 (12) | −0.0089 (12) |
C13 | 0.0345 (12) | 0.0512 (14) | 0.0504 (15) | −0.0048 (11) | 0.0104 (10) | −0.0147 (12) |
C14 | 0.0443 (13) | 0.0539 (16) | 0.0487 (14) | 0.0042 (12) | 0.0015 (11) | −0.0008 (13) |
C15 | 0.0466 (13) | 0.0376 (12) | 0.0493 (14) | −0.0028 (11) | 0.0089 (11) | −0.0003 (11) |
C16 | 0.0487 (16) | 0.075 (2) | 0.0651 (19) | −0.0121 (16) | 0.0086 (14) | −0.0249 (18) |
C17 | 0.0511 (14) | 0.0392 (12) | 0.0390 (13) | 0.0011 (11) | 0.0134 (11) | −0.0082 (11) |
C18 | 0.0565 (15) | 0.0361 (13) | 0.0511 (15) | 0.0085 (11) | 0.0075 (12) | 0.0001 (12) |
C19 | 0.0643 (17) | 0.0387 (13) | 0.0408 (14) | 0.0054 (12) | 0.0042 (12) | 0.0088 (11) |
C20 | 0.0602 (15) | 0.0414 (13) | 0.0293 (11) | 0.0013 (12) | 0.0114 (10) | 0.0037 (10) |
C21 | 0.0374 (11) | 0.0316 (10) | 0.0282 (10) | −0.0065 (9) | 0.0086 (8) | −0.0023 (9) |
C22 | 0.0339 (10) | 0.0320 (10) | 0.0283 (10) | −0.0039 (9) | 0.0099 (8) | −0.0007 (9) |
C23 | 0.0563 (15) | 0.0446 (13) | 0.0314 (11) | 0.0053 (12) | 0.0187 (10) | 0.0058 (10) |
C24 | 0.0546 (15) | 0.0504 (14) | 0.0415 (13) | 0.0092 (12) | 0.0215 (11) | −0.0028 (12) |
C25 | 0.0454 (13) | 0.0430 (13) | 0.0484 (14) | 0.0117 (11) | 0.0151 (11) | 0.0025 (12) |
C26 | 0.0417 (12) | 0.0451 (13) | 0.0355 (12) | 0.0065 (11) | 0.0102 (10) | 0.0093 (11) |
Cd1—O1W | 2.2930 (18) | C7—H7 | 0.9300 |
Cd1—O2 | 2.2983 (17) | C8—H8 | 0.9300 |
Cd1—N2 | 2.3248 (19) | C9—C10 | 1.506 (3) |
Cd1—N1 | 2.3438 (19) | C10—C15 | 1.385 (3) |
Cd1—O4 | 2.419 (2) | C10—C11 | 1.391 (3) |
Cd1—O5 | 2.422 (2) | C11—C12 | 1.381 (3) |
Cd1—O1 | 2.6312 (19) | C11—H11 | 0.9300 |
O1W—H1W1 | 0.85 (3) | C12—C13 | 1.388 (4) |
O1W—H1W2 | 0.85 (4) | C12—H12 | 0.9300 |
O2W—H2W1 | 0.85 (4) | C13—C14 | 1.385 (4) |
O2W—H2W2 | 0.85 (3) | C13—C16 | 1.476 (4) |
O1—C1 | 1.233 (3) | C14—C15 | 1.381 (3) |
O2—C1 | 1.278 (3) | C14—H14 | 0.9300 |
O3—C8 | 1.188 (4) | C15—H15 | 0.9300 |
O4—C9 | 1.242 (3) | C16—H16 | 0.9300 |
O5—C9 | 1.253 (3) | C17—C18 | 1.374 (4) |
O6—C16 | 1.194 (4) | C17—H17 | 0.9300 |
N1—C17 | 1.339 (3) | C18—C19 | 1.372 (4) |
N1—C21 | 1.340 (3) | C18—H18 | 0.9300 |
N2—C26 | 1.339 (3) | C19—C20 | 1.381 (4) |
N2—C22 | 1.346 (3) | C19—H19 | 0.9300 |
C1—C2 | 1.512 (3) | C20—C21 | 1.388 (3) |
C2—C7 | 1.375 (4) | C20—H20 | 0.9300 |
C2—C3 | 1.378 (4) | C21—C22 | 1.496 (3) |
C3—C4 | 1.382 (4) | C22—C23 | 1.385 (3) |
C3—H3 | 0.9300 | C23—C24 | 1.380 (3) |
C4—C5 | 1.369 (4) | C23—H23 | 0.9300 |
C4—H4 | 0.9300 | C24—C25 | 1.375 (3) |
C5—C6 | 1.380 (4) | C24—H24 | 0.9300 |
C5—C8 | 1.478 (4) | C25—C26 | 1.378 (3) |
C6—C7 | 1.383 (4) | C25—H25 | 0.9300 |
C6—H6 | 0.9300 | C26—H26 | 0.9300 |
O1W—Cd1—O2 | 86.27 (7) | O3—C8—H8 | 117.5 |
O1W—Cd1—N2 | 94.83 (7) | C5—C8—H8 | 117.5 |
O2—Cd1—N2 | 145.20 (6) | O4—C9—O5 | 122.0 (2) |
O1W—Cd1—N1 | 153.83 (7) | O4—C9—C10 | 118.9 (2) |
O2—Cd1—N1 | 93.47 (7) | O5—C9—C10 | 119.0 (2) |
N2—Cd1—N1 | 70.81 (6) | C15—C10—C11 | 119.7 (2) |
O1W—Cd1—O4 | 77.42 (7) | C15—C10—C9 | 119.9 (2) |
O2—Cd1—O4 | 122.37 (7) | C11—C10—C9 | 120.4 (2) |
N2—Cd1—O4 | 91.56 (8) | C12—C11—C10 | 120.1 (2) |
N1—Cd1—O4 | 123.34 (7) | C12—C11—H11 | 120.0 |
O1W—Cd1—O5 | 120.81 (7) | C10—C11—H11 | 120.0 |
O2—Cd1—O5 | 93.28 (6) | C11—C12—C13 | 120.1 (2) |
N2—Cd1—O5 | 115.25 (7) | C11—C12—H12 | 120.0 |
N1—Cd1—O5 | 85.35 (7) | C13—C12—H12 | 120.0 |
O4—Cd1—O5 | 53.60 (6) | C14—C13—C12 | 119.7 (2) |
O1W—Cd1—O1 | 77.58 (7) | C14—C13—C16 | 119.8 (3) |
O2—Cd1—O1 | 52.65 (6) | C12—C13—C16 | 120.4 (3) |
N2—Cd1—O1 | 93.55 (6) | C15—C14—C13 | 120.3 (2) |
N1—Cd1—O1 | 81.51 (7) | C15—C14—H14 | 119.9 |
O4—Cd1—O1 | 154.81 (6) | C13—C14—H14 | 119.9 |
O5—Cd1—O1 | 142.17 (6) | C14—C15—C10 | 120.1 (2) |
Cd1—O1W—H1W1 | 117 (2) | C14—C15—H15 | 119.9 |
Cd1—O1W—H1W2 | 126 (2) | C10—C15—H15 | 119.9 |
H1W1—O1W—H1W2 | 110.2 (16) | O6—C16—C13 | 125.0 (3) |
H2W1—O2W—H2W2 | 110.6 (17) | O6—C16—H16 | 117.5 |
C1—O1—Cd1 | 84.80 (15) | C13—C16—H16 | 117.5 |
C1—O2—Cd1 | 99.20 (15) | N1—C17—C18 | 123.0 (2) |
C9—O4—Cd1 | 92.39 (16) | N1—C17—H17 | 118.5 |
C9—O5—Cd1 | 91.97 (16) | C18—C17—H17 | 118.5 |
C17—N1—C21 | 118.8 (2) | C19—C18—C17 | 118.4 (2) |
C17—N1—Cd1 | 123.34 (16) | C19—C18—H18 | 120.8 |
C21—N1—Cd1 | 117.69 (14) | C17—C18—H18 | 120.8 |
C26—N2—C22 | 118.64 (19) | C18—C19—C20 | 119.5 (2) |
C26—N2—Cd1 | 123.46 (15) | C18—C19—H19 | 120.3 |
C22—N2—Cd1 | 117.90 (14) | C20—C19—H19 | 120.3 |
O1—C1—O2 | 123.0 (2) | C19—C20—C21 | 119.2 (2) |
O1—C1—C2 | 119.6 (2) | C19—C20—H20 | 120.4 |
O2—C1—C2 | 117.4 (2) | C21—C20—H20 | 120.4 |
C7—C2—C3 | 118.9 (2) | N1—C21—C20 | 121.2 (2) |
C7—C2—C1 | 119.8 (2) | N1—C21—C22 | 116.48 (19) |
C3—C2—C1 | 121.3 (2) | C20—C21—C22 | 122.4 (2) |
C2—C3—C4 | 121.1 (3) | N2—C22—C23 | 120.8 (2) |
C2—C3—H3 | 119.5 | N2—C22—C21 | 116.98 (19) |
C4—C3—H3 | 119.5 | C23—C22—C21 | 122.2 (2) |
C5—C4—C3 | 120.0 (3) | C24—C23—C22 | 120.0 (2) |
C5—C4—H4 | 120.0 | C24—C23—H23 | 120.0 |
C3—C4—H4 | 120.0 | C22—C23—H23 | 120.0 |
C4—C5—C6 | 119.3 (3) | C25—C24—C23 | 118.9 (2) |
C4—C5—C8 | 119.8 (3) | C25—C24—H24 | 120.6 |
C6—C5—C8 | 120.9 (3) | C23—C24—H24 | 120.6 |
C5—C6—C7 | 120.6 (3) | C24—C25—C26 | 118.5 (2) |
C5—C6—H6 | 119.7 | C24—C25—H25 | 120.8 |
C7—C6—H6 | 119.7 | C26—C25—H25 | 120.8 |
C2—C7—C6 | 120.2 (3) | N2—C26—C25 | 123.1 (2) |
C2—C7—H7 | 119.9 | N2—C26—H26 | 118.4 |
C6—C7—H7 | 119.9 | C25—C26—H26 | 118.4 |
O3—C8—C5 | 125.0 (3) | ||
O1W—Cd1—O1—C1 | 91.39 (16) | C1—C2—C3—C4 | −179.5 (3) |
O2—Cd1—O1—C1 | −3.45 (15) | C2—C3—C4—C5 | 0.1 (6) |
N2—Cd1—O1—C1 | −174.44 (15) | C3—C4—C5—C6 | −0.9 (5) |
N1—Cd1—O1—C1 | −104.45 (16) | C3—C4—C5—C8 | 179.2 (3) |
O4—Cd1—O1—C1 | 84.2 (2) | C4—C5—C6—C7 | 0.7 (5) |
O5—Cd1—O1—C1 | −33.5 (2) | C8—C5—C6—C7 | −179.4 (3) |
O1W—Cd1—O2—C1 | −73.86 (16) | C3—C2—C7—C6 | −1.2 (4) |
N2—Cd1—O2—C1 | 19.2 (2) | C1—C2—C7—C6 | 179.3 (3) |
N1—Cd1—O2—C1 | 79.92 (16) | C5—C6—C7—C2 | 0.4 (5) |
O4—Cd1—O2—C1 | −146.42 (15) | C4—C5—C8—O3 | −4.5 (5) |
O5—Cd1—O2—C1 | 165.45 (16) | C6—C5—C8—O3 | 175.5 (3) |
O1—Cd1—O2—C1 | 3.35 (14) | Cd1—O4—C9—O5 | 0.1 (3) |
O1W—Cd1—O4—C9 | −144.78 (18) | Cd1—O4—C9—C10 | 179.72 (19) |
O2—Cd1—O4—C9 | −67.51 (18) | Cd1—O5—C9—O4 | −0.1 (3) |
N2—Cd1—O4—C9 | 120.62 (17) | Cd1—O5—C9—C10 | −179.72 (19) |
N1—Cd1—O4—C9 | 52.7 (2) | O4—C9—C10—C15 | −28.3 (4) |
O5—Cd1—O4—C9 | −0.05 (15) | O5—C9—C10—C15 | 151.4 (2) |
O1—Cd1—O4—C9 | −137.63 (16) | O4—C9—C10—C11 | 151.2 (3) |
O1W—Cd1—O5—C9 | 41.05 (17) | O5—C9—C10—C11 | −29.2 (3) |
O2—Cd1—O5—C9 | 128.66 (15) | C15—C10—C11—C12 | 0.2 (4) |
N2—Cd1—O5—C9 | −71.88 (16) | C9—C10—C11—C12 | −179.3 (2) |
N1—Cd1—O5—C9 | −138.11 (15) | C10—C11—C12—C13 | −1.1 (4) |
O4—Cd1—O5—C9 | 0.05 (15) | C11—C12—C13—C14 | 1.0 (4) |
O1—Cd1—O5—C9 | 152.14 (14) | C11—C12—C13—C16 | −177.9 (3) |
O1W—Cd1—N1—C17 | 119.2 (2) | C12—C13—C14—C15 | 0.0 (4) |
O2—Cd1—N1—C17 | 30.57 (18) | C16—C13—C14—C15 | 178.9 (3) |
N2—Cd1—N1—C17 | 178.78 (19) | C13—C14—C15—C10 | −0.9 (4) |
O4—Cd1—N1—C17 | −102.43 (19) | C11—C10—C15—C14 | 0.8 (4) |
O5—Cd1—N1—C17 | −62.44 (18) | C9—C10—C15—C14 | −179.8 (2) |
O1—Cd1—N1—C17 | 81.99 (18) | C14—C13—C16—O6 | −175.4 (3) |
O1W—Cd1—N1—C21 | −56.5 (2) | C12—C13—C16—O6 | 3.6 (5) |
O2—Cd1—N1—C21 | −145.07 (16) | C21—N1—C17—C18 | 0.8 (4) |
N2—Cd1—N1—C21 | 3.14 (15) | Cd1—N1—C17—C18 | −174.77 (19) |
O4—Cd1—N1—C21 | 81.93 (17) | N1—C17—C18—C19 | −0.2 (4) |
O5—Cd1—N1—C21 | 121.92 (16) | C17—C18—C19—C20 | −0.5 (4) |
O1—Cd1—N1—C21 | −93.65 (16) | C18—C19—C20—C21 | 0.7 (4) |
O1W—Cd1—N2—C26 | −23.32 (18) | C17—N1—C21—C20 | −0.6 (3) |
O2—Cd1—N2—C26 | −113.74 (19) | Cd1—N1—C21—C20 | 175.21 (17) |
N1—Cd1—N2—C26 | 179.12 (19) | C17—N1—C21—C22 | 179.7 (2) |
O4—Cd1—N2—C26 | 54.18 (18) | Cd1—N1—C21—C22 | −4.5 (2) |
O5—Cd1—N2—C26 | 104.13 (18) | C19—C20—C21—N1 | −0.1 (4) |
O1—Cd1—N2—C26 | −101.14 (18) | C19—C20—C21—C22 | 179.6 (2) |
O1W—Cd1—N2—C22 | 156.28 (15) | C26—N2—C22—C23 | −0.3 (3) |
O2—Cd1—N2—C22 | 65.9 (2) | Cd1—N2—C22—C23 | −179.96 (17) |
N1—Cd1—N2—C22 | −1.28 (15) | C26—N2—C22—C21 | 179.14 (19) |
O4—Cd1—N2—C22 | −126.21 (16) | Cd1—N2—C22—C21 | −0.5 (2) |
O5—Cd1—N2—C22 | −76.26 (16) | N1—C21—C22—N2 | 3.3 (3) |
O1—Cd1—N2—C22 | 78.46 (16) | C20—C21—C22—N2 | −176.4 (2) |
Cd1—O1—C1—O2 | 5.9 (2) | N1—C21—C22—C23 | −177.2 (2) |
Cd1—O1—C1—C2 | −172.8 (2) | C20—C21—C22—C23 | 3.1 (3) |
Cd1—O2—C1—O1 | −6.8 (3) | N2—C22—C23—C24 | 1.1 (4) |
Cd1—O2—C1—C2 | 171.87 (19) | C21—C22—C23—C24 | −178.4 (2) |
O1—C1—C2—C7 | 18.1 (4) | C22—C23—C24—C25 | −1.2 (4) |
O2—C1—C2—C7 | −160.6 (3) | C23—C24—C25—C26 | 0.7 (4) |
O1—C1—C2—C3 | −161.4 (3) | C22—N2—C26—C25 | −0.2 (3) |
O2—C1—C2—C3 | 19.9 (4) | Cd1—N2—C26—C25 | 179.41 (19) |
C7—C2—C3—C4 | 1.0 (5) | C24—C25—C26—N2 | 0.0 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2W | 0.85 (3) | 1.85 (3) | 2.685 (3) | 167 (3) |
O1W—H1W2···O5i | 0.85 (4) | 1.93 (4) | 2.740 (3) | 159 (3) |
O2W—H2W1···O3ii | 0.85 (4) | 2.02 (4) | 2.854 (3) | 171 (4) |
O2W—H2W2···O2i | 0.85 (3) | 1.92 (3) | 2.766 (3) | 177 (3) |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, y−1/2, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C8H5O3)2(C10H8N2)(H2O)]·H2O |
Mr | 602.86 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 295 |
a, b, c (Å) | 23.878 (5), 6.3586 (13), 17.048 (3) |
β (°) | 106.10 (3) |
V (Å3) | 2486.8 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.93 |
Crystal size (mm) | 0.28 × 0.21 × 0.16 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.780, 0.865 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 22518, 5636, 4810 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.066, 1.08 |
No. of reflections | 5636 |
No. of parameters | 346 |
No. of restraints | 6 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.56, −0.34 |
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···O2W | 0.85 (3) | 1.85 (3) | 2.685 (3) | 167 (3) |
O1W—H1W2···O5i | 0.85 (4) | 1.93 (4) | 2.740 (3) | 159 (3) |
O2W—H2W1···O3ii | 0.85 (4) | 2.02 (4) | 2.854 (3) | 171 (4) |
O2W—H2W2···O2i | 0.85 (3) | 1.92 (3) | 2.766 (3) | 177 (3) |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, y−1/2, −z+3/2. |
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An earlier report (Deng et al., 2007) detailed the crystal structure of cadmium phenanthroline adduct of 4-FBAH; the CdII atom is six-coordinated and the 4-FBA- ligands act in both monodendate and chelating modes. Replacing the N-heterocycle by 2,2'-bipy furnishes the title compound as a monohydrated complex (Fig. 1) whose metal centre is seven-coordinate. It displays a mono-capped triangonal prismatic geometry (Fig. 2). The 4-FBA- ligand is chelating. Hydrogen-bonding interactions between the water molecules and O atoms of 4-FBA- ligands link the mononuclear complex into a chain structure along the b axis (Fig.3).