



Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536808033527/at2645sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536808033527/at2645Isup2.hkl |
CCDC reference: 709542
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean
(C-C) = 0.005 Å
- R factor = 0.026
- wR factor = 0.060
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level C Value of measurement temperature given = 296.000 Value of melting point given = 0.000 PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.20 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.67 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 -- Cl3 .. 5.53 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for Cl1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd2 PLAT412_ALERT_2_C Short Intra XH3 .. XHn H12A .. H15A .. 1.83 Ang. PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ?
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
A solution of CdCl2 (2 mmol) in methanol (20 ml) was added to a methanol solution (20 ml) of the Schiff base ligand (2 mmol, 0.48 g). Red crystals of (I) were isolated after two weeks.
The H atoms bonded to C and N atoms were positioned geometrically and refined using a riding model [aromatic C—H 0.93 Å, methylic C—H = 0.96 Å and N—H = 0.86 Å, Uiso(H) = 1.2 or 1.5Ueq(C, N)]. The H atoms bonded to O atoms were located in a difference Fourier maps and refined with O—H distance restraints of 0.85 (2) and Uiso(H) = 1.5Ueq(O).
Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
![]() | Fig. 1. The structure of title compound, with displacement ellipsoids for non-H atoms drawn at the 50% probability level. |
[Cd3Cl6(C15H15NO2)2(CH4O)2] | F(000) = 2152 |
Mr = 1096.57 | Dx = 1.860 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3942 reflections |
a = 19.7697 (5) Å | θ = 1.8–25.0° |
b = 13.9554 (3) Å | µ = 2.07 mm−1 |
c = 15.1449 (4) Å | T = 296 K |
β = 110.423 (1)° | Block, red |
V = 3915.74 (17) Å3 | 0.15 × 0.13 × 0.05 mm |
Z = 4 |
Bruker APEXII diffractometer | 3350 independent reflections |
Radiation source: fine-focus sealed tube | 2773 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ω scans | θmax = 25.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −23→23 |
Tmin = 0.736, Tmax = 0.898 | k = −16→16 |
13592 measured reflections | l = −15→18 |
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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.060 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0247P)2 + 2.9063P] where P = (Fo2 + 2Fc2)/3 |
3350 reflections | (Δ/σ)max = 0.002 |
226 parameters | Δρmax = 0.36 e Å−3 |
1 restraint | Δρmin = −0.34 e Å−3 |
[Cd3Cl6(C15H15NO2)2(CH4O)2] | V = 3915.74 (17) Å3 |
Mr = 1096.57 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 19.7697 (5) Å | µ = 2.07 mm−1 |
b = 13.9554 (3) Å | T = 296 K |
c = 15.1449 (4) Å | 0.15 × 0.13 × 0.05 mm |
β = 110.423 (1)° |
Bruker APEXII diffractometer | 3350 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2773 reflections with I > 2σ(I) |
Tmin = 0.736, Tmax = 0.898 | Rint = 0.033 |
13592 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 1 restraint |
wR(F2) = 0.060 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 0.36 e Å−3 |
3350 reflections | Δρmin = −0.34 e Å−3 |
226 parameters |
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. 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. |
x | y | z | Uiso*/Ueq | ||
Cd1 | 0.542829 (14) | 1.284415 (15) | −0.113758 (18) | 0.04061 (9) | |
Cd2 | 0.5000 | 1.5000 | 0.0000 | 0.04260 (11) | |
N1 | 0.46501 (15) | 0.97593 (18) | −0.16754 (19) | 0.0373 (6) | |
H1D | 0.4710 | 1.0367 | −0.1704 | 0.045* | |
O1 | 0.53998 (12) | 1.12806 (14) | −0.10453 (16) | 0.0440 (6) | |
O2 | 0.65586 (13) | 1.21264 (15) | 0.01463 (18) | 0.0502 (6) | |
O3 | 0.41084 (17) | 1.48567 (18) | −0.1495 (2) | 0.0734 (9) | |
H3C | 0.406 (3) | 1.431 (2) | −0.174 (3) | 0.110* | |
Cl1 | 0.59671 (6) | 1.44929 (6) | −0.07253 (8) | 0.0632 (3) | |
Cl2 | 0.48990 (5) | 1.31686 (6) | 0.02126 (6) | 0.0447 (2) | |
Cl3 | 0.41178 (5) | 1.27831 (6) | −0.24124 (6) | 0.0449 (2) | |
C1 | 0.2053 (2) | 0.8336 (3) | −0.4388 (3) | 0.0702 (12) | |
H1A | 0.2054 | 0.7648 | −0.4396 | 0.105* | |
H1B | 0.1995 | 0.8574 | −0.5005 | 0.105* | |
H1C | 0.1661 | 0.8558 | −0.4206 | 0.105* | |
C2 | 0.27528 (19) | 0.8692 (2) | −0.3696 (3) | 0.0470 (9) | |
C3 | 0.3294 (2) | 0.8076 (2) | −0.3173 (3) | 0.0534 (10) | |
H3A | 0.3228 | 0.7420 | −0.3272 | 0.064* | |
C4 | 0.3923 (2) | 0.8400 (2) | −0.2515 (3) | 0.0487 (9) | |
H4A | 0.4278 | 0.7968 | −0.2177 | 0.058* | |
C5 | 0.40256 (18) | 0.9373 (2) | −0.2360 (2) | 0.0361 (8) | |
C6 | 0.3509 (2) | 1.0007 (2) | −0.2894 (3) | 0.0433 (8) | |
H6A | 0.3586 | 1.0664 | −0.2814 | 0.052* | |
C7 | 0.28796 (19) | 0.9666 (2) | −0.3544 (3) | 0.0469 (9) | |
H7A | 0.2530 | 1.0098 | −0.3891 | 0.056* | |
C8 | 0.51477 (18) | 0.9305 (2) | −0.1005 (2) | 0.0373 (8) | |
H8A | 0.5095 | 0.8648 | −0.0947 | 0.045* | |
C9 | 0.57599 (18) | 0.9754 (2) | −0.0364 (2) | 0.0356 (8) | |
C10 | 0.6274 (2) | 0.9190 (2) | 0.0325 (3) | 0.0498 (9) | |
H10A | 0.6196 | 0.8537 | 0.0365 | 0.060* | |
C11 | 0.6876 (2) | 0.9600 (3) | 0.0925 (3) | 0.0557 (10) | |
H11A | 0.7218 | 0.9222 | 0.1367 | 0.067* | |
C12 | 0.6997 (2) | 1.0591 (3) | 0.0893 (3) | 0.0510 (9) | |
H12A | 0.7414 | 1.0863 | 0.1315 | 0.061* | |
C13 | 0.65035 (18) | 1.1156 (2) | 0.0245 (2) | 0.0398 (8) | |
C14 | 0.58669 (17) | 1.0755 (2) | −0.0415 (2) | 0.0344 (7) | |
C15 | 0.7108 (2) | 1.2622 (3) | 0.0885 (3) | 0.0693 (12) | |
H15A | 0.7460 | 1.2170 | 0.1252 | 0.104* | |
H15B | 0.6893 | 1.2942 | 0.1282 | 0.104* | |
H15C | 0.7338 | 1.3084 | 0.0614 | 0.104* | |
C16 | 0.3865 (3) | 1.5562 (4) | −0.2154 (3) | 0.110 (2) | |
H16A | 0.3495 | 1.5309 | −0.2701 | 0.165* | |
H16B | 0.4257 | 1.5796 | −0.2329 | 0.165* | |
H16C | 0.3670 | 1.6078 | −0.1897 | 0.165* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.04572 (18) | 0.02655 (13) | 0.04443 (16) | −0.00188 (10) | 0.00927 (13) | −0.00170 (10) |
Cd2 | 0.0499 (3) | 0.02725 (18) | 0.0422 (2) | 0.00221 (15) | 0.00547 (19) | −0.00150 (14) |
N1 | 0.0407 (18) | 0.0263 (13) | 0.0430 (17) | −0.0029 (12) | 0.0120 (15) | −0.0001 (12) |
O1 | 0.0432 (15) | 0.0273 (11) | 0.0472 (14) | 0.0025 (10) | −0.0022 (12) | 0.0032 (10) |
O2 | 0.0454 (16) | 0.0383 (13) | 0.0571 (16) | −0.0100 (11) | 0.0055 (13) | −0.0043 (11) |
O3 | 0.086 (2) | 0.0433 (16) | 0.0607 (19) | 0.0093 (15) | −0.0132 (17) | −0.0099 (14) |
Cl1 | 0.0737 (7) | 0.0389 (5) | 0.0889 (8) | −0.0198 (5) | 0.0433 (6) | −0.0183 (5) |
Cl2 | 0.0541 (6) | 0.0300 (4) | 0.0472 (5) | −0.0023 (4) | 0.0141 (5) | 0.0016 (4) |
Cl3 | 0.0422 (5) | 0.0437 (5) | 0.0436 (5) | −0.0017 (4) | 0.0085 (4) | −0.0031 (4) |
C1 | 0.044 (3) | 0.060 (3) | 0.087 (3) | −0.001 (2) | −0.002 (2) | −0.008 (2) |
C2 | 0.039 (2) | 0.045 (2) | 0.053 (2) | −0.0029 (17) | 0.0115 (19) | −0.0053 (17) |
C3 | 0.054 (3) | 0.0310 (18) | 0.065 (3) | −0.0059 (17) | 0.009 (2) | −0.0031 (17) |
C4 | 0.047 (2) | 0.0344 (19) | 0.052 (2) | 0.0025 (16) | 0.002 (2) | 0.0024 (16) |
C5 | 0.036 (2) | 0.0332 (17) | 0.0384 (19) | −0.0032 (14) | 0.0118 (17) | −0.0014 (14) |
C6 | 0.048 (2) | 0.0312 (17) | 0.048 (2) | −0.0007 (16) | 0.0138 (19) | 0.0014 (15) |
C7 | 0.038 (2) | 0.0418 (19) | 0.052 (2) | 0.0071 (16) | 0.005 (2) | 0.0014 (17) |
C8 | 0.043 (2) | 0.0285 (16) | 0.039 (2) | 0.0009 (15) | 0.0134 (18) | 0.0027 (14) |
C9 | 0.038 (2) | 0.0323 (16) | 0.0347 (19) | 0.0039 (14) | 0.0108 (17) | 0.0013 (14) |
C10 | 0.059 (3) | 0.0365 (19) | 0.047 (2) | 0.0086 (18) | 0.009 (2) | 0.0056 (16) |
C11 | 0.055 (3) | 0.048 (2) | 0.048 (2) | 0.0139 (19) | −0.002 (2) | 0.0068 (18) |
C12 | 0.040 (2) | 0.058 (2) | 0.044 (2) | 0.0038 (18) | 0.0008 (19) | −0.0074 (18) |
C13 | 0.040 (2) | 0.0357 (18) | 0.040 (2) | −0.0002 (15) | 0.0102 (18) | −0.0027 (15) |
C14 | 0.037 (2) | 0.0319 (17) | 0.0341 (18) | 0.0030 (14) | 0.0121 (17) | −0.0015 (14) |
C15 | 0.069 (3) | 0.059 (2) | 0.066 (3) | −0.026 (2) | 0.005 (2) | −0.016 (2) |
C16 | 0.148 (6) | 0.076 (3) | 0.062 (3) | 0.018 (3) | −0.018 (3) | −0.001 (3) |
Cd1—O1 | 2.188 (2) | C2—C7 | 1.387 (5) |
Cd1—Cl1 | 2.5208 (9) | C3—C4 | 1.371 (5) |
Cd1—O2 | 2.597 (2) | C3—H3A | 0.9300 |
Cd1—Cl3 | 2.6374 (9) | C4—C5 | 1.382 (4) |
Cd1—Cl2 | 2.6410 (9) | C4—H4A | 0.9300 |
Cd1—Cl3i | 2.6476 (9) | C5—C6 | 1.380 (4) |
Cd2—O3ii | 2.343 (3) | C6—C7 | 1.375 (5) |
Cd2—O3 | 2.343 (3) | C6—H6A | 0.9300 |
Cd2—Cl2 | 2.5924 (8) | C7—H7A | 0.9300 |
Cd2—Cl2ii | 2.5924 (8) | C8—C9 | 1.407 (4) |
Cd2—Cl1 | 2.6133 (10) | C8—H8A | 0.9300 |
Cd2—Cl1ii | 2.6133 (10) | C9—C10 | 1.414 (4) |
N1—C8 | 1.306 (4) | C9—C14 | 1.418 (4) |
N1—C5 | 1.413 (4) | C10—C11 | 1.348 (5) |
N1—H1D | 0.8600 | C10—H10A | 0.9300 |
O1—C14 | 1.299 (4) | C11—C12 | 1.408 (5) |
O2—C13 | 1.372 (4) | C11—H11A | 0.9300 |
O2—C15 | 1.435 (4) | C12—C13 | 1.366 (5) |
O3—C16 | 1.365 (5) | C12—H12A | 0.9300 |
O3—H3C | 0.838 (19) | C13—C14 | 1.421 (4) |
Cl3—Cd1i | 2.6476 (9) | C15—H15A | 0.9600 |
C1—C2 | 1.499 (5) | C15—H15B | 0.9600 |
C1—H1A | 0.9600 | C15—H15C | 0.9600 |
C1—H1B | 0.9600 | C16—H16A | 0.9600 |
C1—H1C | 0.9600 | C16—H16B | 0.9600 |
C2—C3 | 1.385 (5) | C16—H16C | 0.9600 |
O1—Cd1—Cl1 | 155.83 (6) | C3—C2—C1 | 122.3 (3) |
O1—Cd1—O2 | 66.56 (7) | C7—C2—C1 | 120.7 (3) |
Cl1—Cd1—O2 | 89.30 (5) | C4—C3—C2 | 122.4 (3) |
O1—Cd1—Cl3 | 88.51 (6) | C4—C3—H3A | 118.8 |
Cl1—Cd1—Cl3 | 115.66 (3) | C2—C3—H3A | 118.8 |
O2—Cd1—Cl3 | 154.74 (5) | C3—C4—C5 | 119.3 (3) |
O1—Cd1—Cl2 | 95.48 (6) | C3—C4—H4A | 120.3 |
Cl1—Cd1—Cl2 | 84.21 (3) | C5—C4—H4A | 120.3 |
O2—Cd1—Cl2 | 87.50 (6) | C6—C5—C4 | 119.7 (3) |
Cl3—Cd1—Cl2 | 91.09 (3) | C6—C5—N1 | 117.7 (3) |
O1—Cd1—Cl3i | 92.56 (6) | C4—C5—N1 | 122.6 (3) |
Cl1—Cd1—Cl3i | 89.92 (3) | C7—C6—C5 | 119.8 (3) |
O2—Cd1—Cl3i | 99.00 (6) | C7—C6—H6A | 120.1 |
Cl3—Cd1—Cl3i | 85.55 (3) | C5—C6—H6A | 120.1 |
Cl2—Cd1—Cl3i | 171.21 (3) | C6—C7—C2 | 121.7 (3) |
O3ii—Cd2—O3 | 180.00 (12) | C6—C7—H7A | 119.2 |
O3ii—Cd2—Cl2 | 91.64 (7) | C2—C7—H7A | 119.2 |
O3—Cd2—Cl2 | 88.36 (7) | N1—C8—C9 | 123.6 (3) |
O3ii—Cd2—Cl2ii | 88.36 (7) | N1—C8—H8A | 118.2 |
O3—Cd2—Cl2ii | 91.64 (7) | C9—C8—H8A | 118.2 |
Cl2—Cd2—Cl2ii | 180.000 (1) | C8—C9—C10 | 119.0 (3) |
O3ii—Cd2—Cl1 | 90.88 (9) | C8—C9—C14 | 120.7 (3) |
O3—Cd2—Cl1 | 89.12 (9) | C10—C9—C14 | 120.4 (3) |
Cl2—Cd2—Cl1 | 83.37 (3) | C11—C10—C9 | 120.0 (3) |
Cl2ii—Cd2—Cl1 | 96.63 (3) | C11—C10—H10A | 120.0 |
O3ii—Cd2—Cl1ii | 89.12 (9) | C9—C10—H10A | 120.0 |
O3—Cd2—Cl1ii | 90.88 (9) | C10—C11—C12 | 120.9 (3) |
Cl2—Cd2—Cl1ii | 96.63 (3) | C10—C11—H11A | 119.5 |
Cl2ii—Cd2—Cl1ii | 83.37 (3) | C12—C11—H11A | 119.5 |
Cl1—Cd2—Cl1ii | 180.000 (1) | C13—C12—C11 | 120.3 (3) |
C8—N1—C5 | 127.9 (3) | C13—C12—H12A | 119.9 |
C8—N1—H1D | 116.1 | C11—C12—H12A | 119.9 |
C5—N1—H1D | 116.1 | C12—C13—O2 | 125.7 (3) |
C14—O1—Cd1 | 125.63 (19) | C12—C13—C14 | 120.9 (3) |
C13—O2—C15 | 117.3 (3) | O2—C13—C14 | 113.4 (3) |
C13—O2—Cd1 | 112.48 (19) | O1—C14—C9 | 121.0 (3) |
C15—O2—Cd1 | 128.1 (2) | O1—C14—C13 | 121.5 (3) |
C16—O3—Cd2 | 126.9 (3) | C9—C14—C13 | 117.5 (3) |
C16—O3—H3C | 112 (4) | O2—C15—H15A | 109.5 |
Cd2—O3—H3C | 116 (4) | O2—C15—H15B | 109.5 |
Cd1—Cl1—Cd2 | 92.48 (3) | H15A—C15—H15B | 109.5 |
Cd2—Cl2—Cd1 | 90.25 (3) | O2—C15—H15C | 109.5 |
Cd1—Cl3—Cd1i | 94.33 (3) | H15A—C15—H15C | 109.5 |
C2—C1—H1A | 109.5 | H15B—C15—H15C | 109.5 |
C2—C1—H1B | 109.5 | O3—C16—H16A | 109.5 |
H1A—C1—H1B | 109.5 | O3—C16—H16B | 109.5 |
C2—C1—H1C | 109.5 | H16A—C16—H16B | 109.5 |
H1A—C1—H1C | 109.5 | O3—C16—H16C | 109.5 |
H1B—C1—H1C | 109.5 | H16A—C16—H16C | 109.5 |
C3—C2—C7 | 117.0 (3) | H16B—C16—H16C | 109.5 |
Cl1—Cd1—O1—C14 | 9.2 (3) | Cl2—Cd1—Cl3—Cd1i | 168.17 (2) |
O2—Cd1—O1—C14 | 6.0 (2) | Cl3i—Cd1—Cl3—Cd1i | −3.70 (4) |
Cl3—Cd1—O1—C14 | −169.9 (2) | C7—C2—C3—C4 | 1.6 (6) |
Cl2—Cd1—O1—C14 | −78.9 (2) | C1—C2—C3—C4 | −177.5 (4) |
Cl3i—Cd1—O1—C14 | 104.7 (2) | C2—C3—C4—C5 | 0.3 (6) |
O1—Cd1—O2—C13 | −5.0 (2) | C3—C4—C5—C6 | −2.7 (5) |
Cl1—Cd1—O2—C13 | 176.3 (2) | C3—C4—C5—N1 | 178.1 (3) |
Cl3—Cd1—O2—C13 | 4.8 (3) | C8—N1—C5—C6 | 168.6 (3) |
Cl2—Cd1—O2—C13 | 92.1 (2) | C8—N1—C5—C4 | −12.3 (5) |
Cl3i—Cd1—O2—C13 | −93.9 (2) | C4—C5—C6—C7 | 3.3 (5) |
O1—Cd1—O2—C15 | −167.6 (3) | N1—C5—C6—C7 | −177.6 (3) |
Cl1—Cd1—O2—C15 | 13.8 (3) | C5—C6—C7—C2 | −1.4 (5) |
Cl3—Cd1—O2—C15 | −157.7 (3) | C3—C2—C7—C6 | −1.0 (5) |
Cl2—Cd1—O2—C15 | −70.5 (3) | C1—C2—C7—C6 | 178.1 (4) |
Cl3i—Cd1—O2—C15 | 103.6 (3) | C5—N1—C8—C9 | 178.9 (3) |
Cl2—Cd2—O3—C16 | −174.9 (4) | N1—C8—C9—C10 | −178.8 (3) |
Cl2ii—Cd2—O3—C16 | 5.1 (4) | N1—C8—C9—C14 | 0.3 (5) |
Cl1—Cd2—O3—C16 | −91.5 (4) | C8—C9—C10—C11 | 177.7 (3) |
Cl1ii—Cd2—O3—C16 | 88.5 (4) | C14—C9—C10—C11 | −1.4 (5) |
O1—Cd1—Cl1—Cd2 | −113.74 (16) | C9—C10—C11—C12 | 1.6 (6) |
O2—Cd1—Cl1—Cd2 | −110.81 (6) | C10—C11—C12—C13 | −0.4 (6) |
Cl3—Cd1—Cl1—Cd2 | 65.17 (4) | C11—C12—C13—O2 | 179.8 (3) |
Cl2—Cd1—Cl1—Cd2 | −23.25 (3) | C11—C12—C13—C14 | −0.9 (5) |
Cl3i—Cd1—Cl1—Cd2 | 150.19 (3) | C15—O2—C13—C12 | −12.1 (5) |
O3ii—Cd2—Cl1—Cd1 | 115.31 (7) | Cd1—O2—C13—C12 | −176.7 (3) |
O3—Cd2—Cl1—Cd1 | −64.69 (7) | C15—O2—C13—C14 | 168.6 (3) |
Cl2—Cd2—Cl1—Cd1 | 23.75 (3) | Cd1—O2—C13—C14 | 4.0 (3) |
Cl2ii—Cd2—Cl1—Cd1 | −156.25 (3) | Cd1—O1—C14—C9 | 173.8 (2) |
O3ii—Cd2—Cl2—Cd1 | −113.28 (9) | Cd1—O1—C14—C13 | −6.4 (4) |
O3—Cd2—Cl2—Cd1 | 66.72 (9) | C8—C9—C14—O1 | 0.8 (5) |
Cl1—Cd2—Cl2—Cd1 | −22.59 (3) | C10—C9—C14—O1 | 179.9 (3) |
Cl1ii—Cd2—Cl2—Cd1 | 157.41 (3) | C8—C9—C14—C13 | −178.9 (3) |
O1—Cd1—Cl2—Cd2 | 179.14 (6) | C10—C9—C14—C13 | 0.1 (5) |
Cl1—Cd1—Cl2—Cd2 | 23.43 (3) | C12—C13—C14—O1 | −178.8 (3) |
O2—Cd1—Cl2—Cd2 | 112.98 (5) | O2—C13—C14—O1 | 0.6 (4) |
O1—Cd1—Cl3—Cd1i | −96.38 (6) | C12—C13—C14—C9 | 1.0 (5) |
Cl1—Cd1—Cl3—Cd1i | 84.07 (3) | O2—C13—C14—C9 | −179.6 (3) |
O2—Cd1—Cl3—Cd1i | −105.40 (14) |
Symmetry codes: (i) −x+1, y, −z−1/2; (ii) −x+1, −y+3, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1D···O1 | 0.86 | 1.88 | 2.574 (3) | 137 |
O3—H3C···Cl3 | 0.84 (2) | 2.38 (2) | 3.213 (3) | 170 (5) |
Experimental details
Crystal data | |
Chemical formula | [Cd3Cl6(C15H15NO2)2(CH4O)2] |
Mr | 1096.57 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 296 |
a, b, c (Å) | 19.7697 (5), 13.9554 (3), 15.1449 (4) |
β (°) | 110.423 (1) |
V (Å3) | 3915.74 (17) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.07 |
Crystal size (mm) | 0.15 × 0.13 × 0.05 |
Data collection | |
Diffractometer | Bruker APEXII diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.736, 0.898 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13592, 3350, 2773 |
Rint | 0.033 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.060, 1.05 |
No. of reflections | 3350 |
No. of parameters | 226 |
No. of restraints | 1 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.36, −0.34 |
Computer programs: SMART (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1D···O1 | 0.86 | 1.88 | 2.574 (3) | 136.8 |
O3—H3C···Cl3 | 0.838 (19) | 2.38 (2) | 3.213 (3) | 170 (5) |
There has been an increasing interest in the coordination chemistry of cadmium in recent years due to the increased recognition of its role in biological organisms (Henkel & Krebs, 2004), as well as in molecular-based materials (De Girolamo et al., 2007). In the quest for molecular-based materials with interesting properties, much attention has been given to one-, two- and three-dimensional extended solids which involve cadmium (Suen & Wang, 2007; Wang et al., 2005; Zhang & Bu, 2008). Complexes of the type CdX2 (X = CI or Br) with organic bases typically form one- or two-dimensional halogen-bridged chain compounds with six-coordination octahedral cadmium(II). Here, we describe the synthesis and crystal structure of the cadmium(II) chloride complex with 2-[(4-methylphenylimino)methyl]-6-methoxyphenol.
The crystal structure of the title compound (I) has features of the monoclinic space group C2/c. As illustrated in Fig. 1, the structure comprises an alternating polymeric chain layer along the c axis. The CdII ions are linked into an infinite chain by double chlorine bridges, The Cd(1)···Cd(2) and Cd(1)···Cd(1A) distances in the molecule are 3.7087 (3) and 3.8756 (4) Å, respectively.