Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801011072/ob6060sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801011072/ob6060Isup2.hkl |
CCDC reference: 170865
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.044
- wR factor = 0.126
- Data-to-parameter ratio = 12.8
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_420 Alert C D-H Without Acceptor N1 - H1A ? PLAT_420 Alert C D-H Without Acceptor N4 - H4A ? PLAT_731 Alert C Bond Calc 0.93(4), Rep 0.935(19) .... 2.11 s.u-Ratio O1 -HOB 1.555 1.555 PLAT_731 Alert C Bond Calc 0.95(5), Rep 0.95(2) .... 2.50 s.u-Ratio O101 -H02 1.555 1.555 PLAT_731 Alert C Bond Calc 0.88(4), Rep 0.875(18) .... 2.22 s.u-Ratio O101 -H01 1.555 1.555 PLAT_735 Alert C D-H Calc 0.93(4), Rep 0.935(19) .... 2.11 s.u-Ratio O1 -HOB 1.555 1.555 PLAT_735 Alert C D-H Calc 0.88(4), Rep 0.875(18) .... 2.22 s.u-Ratio O101 -H01 1.555 1.555 PLAT_735 Alert C D-H Calc 0.95(5), Rep 0.95(2) .... 2.50 s.u-Ratio O101 -H02 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
8 Alert Level C = Please check
A mixture of Cd(NO3)2 (0.08 g, 0.25 mmol) and dadpm (0.10 g, 0.50 mmol) in water/methanol (10/20) was stirred for 3 h. The colorless solution was allowed to evaporate slowly for a week, after which time, colorless crystals of (I) were obtained.
The positions of the H atoms were genetared geometrically (C—H bond fixed at 0.96 Å), assigned isotropic displacement parameters and allowed to ride on their respective parent C atoms, and the positions of the water H atoms were refined with isotropic displacement parameters before the final cycle of least-squares refinement. There are short intermolecular H···H contacts; HOB···H01i = 2.06 Å, H01···H4Bii = 2.09 Å and H02···H2Biii = 1.99 Å (see Table 2 for symmetry codes). However, the assumed H-atom positions are reasonable based on the following angles, O1···H01i—O101i = 63.9°, O101···H4Bii—N4ii = 89.4° and O101···H2Biii—N2iii = 95.9°.
Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SAINT (Siemens, 1994); program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. The structure of (I) with NO3- and uncoordinated water ommited for clarity. Displacement ellipsoids are plotted at the 50% probability level. |
[Cd(C13H14N2)4(H2O)2](NO3)2·2H2O | Z = 1 |
Mr = 1101.53 | F(000) = 574 |
Triclinic, P1 | Dx = 1.417 Mg m−3 |
a = 9.3189 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.6565 (3) Å | Cell parameters from 68 reflections |
c = 12.0590 (1) Å | θ = 1.7–25.1° |
α = 80.845 (1)° | µ = 0.49 mm−1 |
β = 86.638 (1)° | T = 293 K |
γ = 89.051 (1)° | Columnar, colorless |
V = 1290.97 (4) Å3 | 0.32 × 0.17 × 0.15 mm |
Smart CCD diffractometer | 4428 independent reflections |
Radiation source: fine-focus sealed tube | 3749 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
ω scans | θmax = 25.1°, θmin = 1.7° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −11→10 |
Tmin = 0.855, Tmax = 0.929 | k = −11→13 |
6516 measured reflections | l = −11→14 |
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.126 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0795P)2] where P = (Fo2 + 2Fc2)/3 |
4428 reflections | (Δ/σ)max < 0.001 |
347 parameters | Δρmax = 0.35 e Å−3 |
4 restraints | Δρmin = −0.75 e Å−3 |
[Cd(C13H14N2)4(H2O)2](NO3)2·2H2O | γ = 89.051 (1)° |
Mr = 1101.53 | V = 1290.97 (4) Å3 |
Triclinic, P1 | Z = 1 |
a = 9.3189 (2) Å | Mo Kα radiation |
b = 11.6565 (3) Å | µ = 0.49 mm−1 |
c = 12.0590 (1) Å | T = 293 K |
α = 80.845 (1)° | 0.32 × 0.17 × 0.15 mm |
β = 86.638 (1)° |
Smart CCD diffractometer | 4428 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 3749 reflections with I > 2σ(I) |
Tmin = 0.855, Tmax = 0.929 | Rint = 0.024 |
6516 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | 4 restraints |
wR(F2) = 0.126 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.10 | Δρmax = 0.35 e Å−3 |
4428 reflections | Δρmin = −0.75 e Å−3 |
347 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 | ||
Cd | 0.0000 | 1.0000 | −1.0000 | 0.04167 (16) | |
N1 | −0.1200 (4) | 1.0018 (3) | −1.1675 (3) | 0.0483 (8) | |
H1A | −0.0616 | 0.9688 | −1.2157 | 0.058* | |
H1B | −0.1982 | 0.9566 | −1.1512 | 0.058* | |
N2 | −0.3687 (4) | 1.4780 (3) | −1.8633 (3) | 0.0691 (11) | |
H2A | −0.3470 | 1.5406 | −1.9088 | 0.083* | |
H2B | −0.4035 | 1.4198 | −1.8884 | 0.083* | |
N3 | −0.2305 (3) | 1.0432 (3) | −0.9152 (3) | 0.0498 (8) | |
H3A | −0.2478 | 1.1196 | −0.9357 | 0.060* | |
H3C | −0.2973 | 1.0048 | −0.9456 | 0.060* | |
N4 | −0.0190 (5) | 0.5567 (4) | −0.1891 (3) | 0.0826 (13) | |
H4A | 0.0643 | 0.5362 | −0.2139 | 0.099* | |
H4B | −0.0561 | 0.5214 | −0.1261 | 0.099* | |
N11 | 0.4370 (4) | 0.2080 (3) | 0.0127 (3) | 0.0472 (8) | |
O1 | −0.0595 (4) | 0.8070 (3) | −0.9609 (3) | 0.0680 (9) | |
HOA | −0.154 (3) | 0.782 (4) | −0.964 (4) | 0.091 (17)* | |
HOB | 0.003 (4) | 0.748 (3) | −0.977 (4) | 0.072 (15)* | |
O11 | 0.5437 (3) | 0.2591 (3) | 0.0373 (3) | 0.0685 (9) | |
O12 | 0.3452 (3) | 0.2646 (3) | −0.0461 (2) | 0.0648 (8) | |
O13 | 0.4202 (4) | 0.1032 (3) | 0.0446 (3) | 0.0665 (8) | |
O101 | −0.1389 (6) | 0.3519 (4) | 0.0065 (6) | 0.1286 (19) | |
H02 | −0.236 (4) | 0.376 (8) | 0.017 (8) | 0.21 (4)* | |
H01 | −0.083 (4) | 0.401 (3) | 0.031 (3) | 0.039 (11)* | |
C1 | −0.1652 (4) | 1.1132 (3) | −1.2244 (3) | 0.0413 (8) | |
C2 | −0.3022 (4) | 1.1539 (4) | −1.2066 (3) | 0.0482 (9) | |
H2D | −0.3684 | 1.1080 | −1.1592 | 0.058* | |
C3 | −0.3420 (4) | 1.2635 (4) | −1.2592 (3) | 0.0525 (10) | |
H3B | −0.4350 | 1.2902 | −1.2459 | 0.063* | |
C4 | −0.2483 (4) | 1.3335 (3) | −1.3303 (3) | 0.0463 (9) | |
C5 | −0.2930 (5) | 1.4507 (3) | −1.3919 (3) | 0.0577 (11) | |
H5B | −0.3847 | 1.4725 | −1.3586 | 0.069* | |
H5C | −0.2230 | 1.5079 | −1.3809 | 0.069* | |
C6 | −0.3067 (4) | 1.4549 (3) | −1.5161 (3) | 0.0445 (9) | |
C7 | −0.3587 (4) | 1.3630 (3) | −1.5607 (4) | 0.0508 (10) | |
H7B | −0.3803 | 1.2940 | −1.5129 | 0.061* | |
C8 | −0.3797 (4) | 1.3698 (3) | −1.6735 (4) | 0.0535 (10) | |
H8C | −0.4158 | 1.3060 | −1.6999 | 0.064* | |
C9 | −0.3477 (4) | 1.4707 (3) | −1.7488 (3) | 0.0497 (10) | |
C10 | −0.2919 (5) | 1.5628 (3) | −1.7058 (4) | 0.0542 (10) | |
H10A | −0.2674 | 1.6309 | −1.7540 | 0.065* | |
C11 | −0.2724 (4) | 1.5546 (3) | −1.5920 (3) | 0.0510 (10) | |
H11A | −0.2350 | 1.6178 | −1.5654 | 0.061* | |
C12 | −0.1107 (5) | 1.2918 (4) | −1.3469 (3) | 0.0581 (11) | |
H12A | −0.0448 | 1.3377 | −1.3945 | 0.070* | |
C13 | −0.0684 (4) | 1.1833 (4) | −1.2946 (3) | 0.0572 (11) | |
H13A | 0.0253 | 1.1575 | −1.3065 | 0.069* | |
C14 | −0.2535 (4) | 1.0169 (3) | −0.7946 (3) | 0.0417 (9) | |
C15 | −0.3160 (4) | 0.9136 (3) | −0.7447 (3) | 0.0451 (9) | |
H15A | −0.3449 | 0.8610 | −0.7893 | 0.054* | |
C16 | −0.3360 (4) | 0.8876 (4) | −0.6295 (3) | 0.0470 (9) | |
H16A | −0.3783 | 0.8175 | −0.5975 | 0.056* | |
C17 | −0.2943 (4) | 0.9639 (4) | −0.5603 (3) | 0.0474 (9) | |
C18 | −0.3232 (5) | 0.9370 (4) | −0.4336 (3) | 0.0626 (12) | |
H18A | −0.3003 | 1.0054 | −0.4018 | 0.075* | |
H18B | −0.4252 | 0.9228 | −0.4180 | 0.075* | |
C19 | −0.2418 (4) | 0.8349 (4) | −0.3737 (3) | 0.0483 (10) | |
C20 | −0.2991 (5) | 0.7752 (4) | −0.2711 (3) | 0.0529 (10) | |
H20A | −0.3882 | 0.7978 | −0.2426 | 0.064* | |
C21 | −0.2268 (5) | 0.6840 (4) | −0.2113 (4) | 0.0618 (12) | |
H21A | −0.2677 | 0.6464 | −0.1433 | 0.074* | |
C22 | −0.0941 (5) | 0.6472 (4) | −0.2509 (3) | 0.0560 (11) | |
C23 | −0.0366 (4) | 0.7052 (4) | −0.3523 (3) | 0.0572 (11) | |
H23A | 0.0521 | 0.6821 | −0.3810 | 0.069* | |
C24 | −0.1098 (4) | 0.7971 (4) | −0.4113 (3) | 0.0544 (10) | |
H24A | −0.0682 | 0.8349 | −0.4790 | 0.065* | |
C25 | −0.2316 (5) | 1.0660 (4) | −0.6112 (4) | 0.0547 (11) | |
H25A | −0.2022 | 1.1184 | −0.5666 | 0.066* | |
C26 | −0.2106 (5) | 1.0933 (4) | −0.7269 (4) | 0.0530 (10) | |
H26A | −0.1677 | 1.1631 | −0.7589 | 0.064* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd | 0.0408 (3) | 0.0429 (3) | 0.0404 (2) | −0.00008 (16) | −0.00823 (16) | −0.00149 (16) |
N1 | 0.047 (2) | 0.0497 (19) | 0.0485 (18) | 0.0075 (15) | −0.0138 (15) | −0.0061 (15) |
N2 | 0.086 (3) | 0.058 (2) | 0.065 (2) | −0.002 (2) | −0.020 (2) | −0.0080 (19) |
N3 | 0.045 (2) | 0.057 (2) | 0.0465 (18) | 0.0061 (15) | −0.0084 (15) | −0.0038 (15) |
N4 | 0.087 (3) | 0.081 (3) | 0.073 (3) | 0.020 (2) | 0.005 (2) | 0.003 (2) |
N11 | 0.048 (2) | 0.052 (2) | 0.0418 (17) | −0.0018 (16) | 0.0006 (15) | −0.0100 (15) |
O1 | 0.055 (2) | 0.0457 (18) | 0.103 (2) | −0.0043 (15) | −0.0125 (18) | −0.0062 (17) |
O11 | 0.059 (2) | 0.075 (2) | 0.076 (2) | −0.0205 (17) | −0.0060 (16) | −0.0218 (17) |
O12 | 0.063 (2) | 0.064 (2) | 0.0632 (18) | 0.0031 (16) | −0.0136 (16) | 0.0041 (15) |
O13 | 0.077 (2) | 0.0418 (18) | 0.080 (2) | −0.0035 (15) | −0.0131 (17) | −0.0045 (15) |
O101 | 0.089 (4) | 0.089 (3) | 0.207 (6) | 0.004 (3) | 0.039 (4) | −0.039 (3) |
C1 | 0.042 (2) | 0.049 (2) | 0.0353 (18) | 0.0070 (17) | −0.0134 (16) | −0.0085 (16) |
C2 | 0.035 (2) | 0.058 (3) | 0.047 (2) | −0.0034 (18) | 0.0003 (17) | 0.0037 (18) |
C3 | 0.036 (2) | 0.062 (3) | 0.057 (2) | 0.0107 (19) | 0.0034 (18) | −0.003 (2) |
C4 | 0.045 (2) | 0.050 (2) | 0.043 (2) | 0.0067 (18) | −0.0050 (17) | −0.0041 (17) |
C5 | 0.068 (3) | 0.045 (2) | 0.058 (2) | 0.010 (2) | −0.001 (2) | −0.0030 (19) |
C6 | 0.036 (2) | 0.037 (2) | 0.058 (2) | 0.0046 (16) | −0.0044 (17) | −0.0019 (17) |
C7 | 0.045 (2) | 0.036 (2) | 0.068 (3) | −0.0001 (17) | −0.005 (2) | 0.0033 (18) |
C8 | 0.047 (2) | 0.040 (2) | 0.075 (3) | 0.0000 (18) | −0.012 (2) | −0.009 (2) |
C9 | 0.047 (2) | 0.044 (2) | 0.059 (2) | 0.0062 (18) | −0.0114 (19) | −0.0082 (19) |
C10 | 0.057 (3) | 0.040 (2) | 0.062 (3) | −0.0031 (19) | −0.007 (2) | 0.0050 (19) |
C11 | 0.052 (3) | 0.035 (2) | 0.066 (3) | −0.0027 (17) | −0.007 (2) | −0.0063 (18) |
C12 | 0.046 (3) | 0.070 (3) | 0.052 (2) | −0.001 (2) | 0.0054 (19) | 0.010 (2) |
C13 | 0.035 (2) | 0.080 (3) | 0.051 (2) | 0.014 (2) | 0.0034 (18) | 0.005 (2) |
C14 | 0.033 (2) | 0.046 (2) | 0.046 (2) | 0.0084 (16) | −0.0046 (16) | −0.0100 (17) |
C15 | 0.036 (2) | 0.052 (2) | 0.050 (2) | −0.0041 (17) | −0.0046 (17) | −0.0184 (18) |
C16 | 0.041 (2) | 0.050 (2) | 0.050 (2) | −0.0033 (18) | 0.0000 (17) | −0.0092 (18) |
C17 | 0.038 (2) | 0.061 (3) | 0.045 (2) | 0.0112 (18) | −0.0038 (17) | −0.0160 (19) |
C18 | 0.061 (3) | 0.083 (3) | 0.046 (2) | 0.021 (2) | 0.001 (2) | −0.018 (2) |
C19 | 0.039 (2) | 0.070 (3) | 0.040 (2) | −0.0021 (19) | −0.0022 (17) | −0.0210 (19) |
C20 | 0.044 (2) | 0.072 (3) | 0.047 (2) | −0.007 (2) | 0.0060 (18) | −0.024 (2) |
C21 | 0.068 (3) | 0.067 (3) | 0.050 (2) | −0.009 (2) | 0.013 (2) | −0.014 (2) |
C22 | 0.059 (3) | 0.058 (3) | 0.053 (2) | −0.004 (2) | −0.004 (2) | −0.016 (2) |
C23 | 0.038 (2) | 0.075 (3) | 0.059 (3) | −0.003 (2) | 0.0044 (19) | −0.013 (2) |
C24 | 0.039 (2) | 0.072 (3) | 0.050 (2) | 0.000 (2) | 0.0032 (18) | −0.007 (2) |
C25 | 0.052 (3) | 0.054 (3) | 0.064 (3) | 0.006 (2) | −0.008 (2) | −0.030 (2) |
C26 | 0.050 (3) | 0.044 (2) | 0.065 (3) | −0.0022 (19) | −0.004 (2) | −0.0084 (19) |
Cd—O1i | 2.295 (3) | C5—H5C | 0.9700 |
Cd—O1 | 2.295 (3) | C6—C7 | 1.381 (5) |
Cd—N1 | 2.363 (3) | C6—C11 | 1.388 (5) |
Cd—N1i | 2.363 (3) | C7—C8 | 1.375 (6) |
Cd—N3 | 2.405 (3) | C7—H7B | 0.9300 |
Cd—N3i | 2.405 (3) | C8—C9 | 1.391 (5) |
N1—C1 | 1.438 (5) | C8—H8C | 0.9300 |
N1—H1A | 0.9000 | C9—C10 | 1.385 (6) |
N1—H1B | 0.9000 | C10—C11 | 1.384 (6) |
N2—C9 | 1.395 (5) | C10—H10A | 0.9300 |
N2—H2A | 0.8600 | C11—H11A | 0.9300 |
N2—H2B | 0.8600 | C12—C13 | 1.382 (6) |
N3—C14 | 1.442 (4) | C12—H12A | 0.9300 |
N3—H3A | 0.9000 | C13—H13A | 0.9300 |
N3—H3C | 0.9000 | C14—C26 | 1.378 (5) |
N4—C22 | 1.394 (6) | C14—C15 | 1.380 (5) |
N4—H4A | 0.8600 | C15—C16 | 1.375 (5) |
N4—H4B | 0.8600 | C15—H15A | 0.9300 |
N11—O13 | 1.231 (4) | C16—C17 | 1.387 (5) |
N11—O11 | 1.242 (4) | C16—H16A | 0.9300 |
N11—O12 | 1.254 (4) | C17—C25 | 1.372 (6) |
O1—O101ii | 2.691 (6) | C17—C18 | 1.519 (5) |
O1—O12ii | 2.796 (5) | C18—C19 | 1.508 (6) |
O1—HOA | 0.94 (2) | C18—H18A | 0.9700 |
O1—HOB | 0.935 (19) | C18—H18B | 0.9700 |
O101—N4iii | 3.054 (8) | C19—C24 | 1.376 (6) |
O101—N2iv | 3.074 (6) | C19—C20 | 1.400 (5) |
O101—H02 | 0.95 (2) | C20—C21 | 1.376 (6) |
O101—H01 | 0.875 (18) | C20—H20A | 0.9300 |
C1—C2 | 1.372 (5) | C21—C22 | 1.385 (6) |
C1—C13 | 1.383 (5) | C21—H21A | 0.9300 |
C2—C3 | 1.388 (5) | C22—C23 | 1.382 (6) |
C2—H2D | 0.9300 | C23—C24 | 1.382 (6) |
C3—C4 | 1.369 (5) | C23—H23A | 0.9300 |
C3—H3B | 0.9300 | C24—H24A | 0.9300 |
C4—C12 | 1.378 (6) | C25—C26 | 1.383 (6) |
C4—C5 | 1.513 (5) | C25—H25A | 0.9300 |
C5—C6 | 1.504 (5) | C26—H26A | 0.9300 |
C5—H5B | 0.9700 | ||
O1i—Cd—O1 | 180.000 (1) | C8—C7—H7B | 118.9 |
O1i—Cd—N1 | 94.44 (12) | C6—C7—H7B | 118.9 |
O1—Cd—N1 | 85.56 (12) | C7—C8—C9 | 121.1 (4) |
O1i—Cd—N1i | 85.56 (12) | C7—C8—H8C | 119.5 |
O1—Cd—N1i | 94.44 (12) | C9—C8—H8C | 119.5 |
N1—Cd—N1i | 180.0 | C10—C9—C8 | 117.4 (4) |
O1i—Cd—N3 | 92.03 (12) | C10—C9—N2 | 121.4 (4) |
O1—Cd—N3 | 87.97 (12) | C8—C9—N2 | 121.2 (4) |
N1—Cd—N3 | 86.30 (11) | C11—C10—C9 | 120.7 (4) |
N1i—Cd—N3 | 93.70 (11) | C11—C10—H10A | 119.6 |
O1i—Cd—N3i | 87.97 (12) | C9—C10—H10A | 119.6 |
O1—Cd—N3i | 92.03 (12) | C10—C11—C6 | 122.1 (4) |
N1—Cd—N3i | 93.70 (11) | C10—C11—H11A | 118.9 |
N1i—Cd—N3i | 86.30 (11) | C6—C11—H11A | 118.9 |
N3—Cd—N3i | 180.000 (1) | C4—C12—C13 | 121.6 (4) |
C1—N1—Cd | 116.9 (2) | C4—C12—H12A | 119.2 |
C1—N1—H1A | 108.1 | C13—C12—H12A | 119.2 |
Cd—N1—H1A | 108.1 | C12—C13—C1 | 120.1 (4) |
C1—N1—H1B | 108.1 | C12—C13—H13A | 119.9 |
Cd—N1—H1B | 108.1 | C1—C13—H13A | 119.9 |
H1A—N1—H1B | 107.3 | C26—C14—C15 | 118.7 (3) |
C9—N2—H2A | 120.0 | C26—C14—N3 | 120.7 (3) |
C9—N2—H2B | 120.0 | C15—C14—N3 | 120.5 (3) |
H2A—N2—H2B | 120.0 | C16—C15—C14 | 120.6 (3) |
C14—N3—Cd | 118.8 (2) | C16—C15—H15A | 119.7 |
C14—N3—H3A | 107.6 | C14—C15—H15A | 119.7 |
Cd—N3—H3A | 107.6 | C15—C16—C17 | 121.3 (4) |
C14—N3—H3C | 107.6 | C15—C16—H16A | 119.3 |
Cd—N3—H3C | 107.6 | C17—C16—H16A | 119.3 |
H3A—N3—H3C | 107.0 | C25—C17—C16 | 117.4 (3) |
C22—N4—H4A | 120.0 | C25—C17—C18 | 121.7 (4) |
C22—N4—H4B | 120.0 | C16—C17—C18 | 120.9 (4) |
H4A—N4—H4B | 120.0 | C19—C18—C17 | 116.0 (3) |
O13—N11—O11 | 121.2 (4) | C19—C18—H18A | 108.3 |
O13—N11—O12 | 119.6 (3) | C17—C18—H18A | 108.3 |
O11—N11—O12 | 119.1 (4) | C19—C18—H18B | 108.3 |
Cd—O1—HOA | 122 (3) | C17—C18—H18B | 108.3 |
Cd—O1—HOB | 123 (3) | H18A—C18—H18B | 107.4 |
HOA—O1—HOB | 108 (4) | C24—C19—C20 | 116.3 (4) |
H02—O101—H01 | 109 (6) | C24—C19—C18 | 124.2 (4) |
C2—C1—C13 | 118.9 (4) | C20—C19—C18 | 119.4 (4) |
C2—C1—N1 | 120.9 (3) | C21—C20—C19 | 121.6 (4) |
C13—C1—N1 | 120.1 (4) | C21—C20—H20A | 119.2 |
C1—C2—C3 | 120.0 (3) | C19—C20—H20A | 119.2 |
C1—C2—H2D | 120.0 | C20—C21—C22 | 121.1 (4) |
C3—C2—H2D | 120.0 | C20—C21—H21A | 119.5 |
C4—C3—C2 | 121.9 (4) | C22—C21—H21A | 119.5 |
C4—C3—H3B | 119.0 | C23—C22—C21 | 117.8 (4) |
C2—C3—H3B | 119.0 | C23—C22—N4 | 121.0 (4) |
C3—C4—C12 | 117.5 (4) | C21—C22—N4 | 121.1 (4) |
C3—C4—C5 | 122.1 (4) | C22—C23—C24 | 120.6 (4) |
C12—C4—C5 | 120.4 (4) | C22—C23—H23A | 119.7 |
C6—C5—C4 | 114.4 (3) | C24—C23—H23A | 119.7 |
C6—C5—H5B | 108.6 | C19—C24—C23 | 122.5 (4) |
C4—C5—H5B | 108.6 | C19—C24—H24A | 118.7 |
C6—C5—H5C | 108.6 | C23—C24—H24A | 118.7 |
C4—C5—H5C | 108.6 | C17—C25—C26 | 122.0 (4) |
H5B—C5—H5C | 107.6 | C17—C25—H25A | 119.0 |
C7—C6—C11 | 116.3 (4) | C26—C25—H25A | 119.0 |
C7—C6—C5 | 122.5 (3) | C14—C26—C25 | 120.0 (4) |
C11—C6—C5 | 121.1 (3) | C14—C26—H26A | 120.0 |
C8—C7—C6 | 122.3 (4) | C25—C26—H26A | 120.0 |
Symmetry codes: (i) −x, −y+2, −z−2; (ii) −x, −y+1, −z−1; (iii) −x, −y+1, −z; (iv) x, y−1, z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—HOA···O12ii | 0.94 (2) | 1.86 (2) | 2.796 (5) | 174 (5) |
O1—HOB···O101ii | 0.94 (2) | 1.76 (2) | 2.691 (6) | 173 (4) |
O101—H01···N4iii | 0.88 (2) | 2.30 (3) | 3.054 (8) | 144 (3) |
O101—H02···N2iv | 0.95 (2) | 2.30 (7) | 3.074 (6) | 138 (8) |
Symmetry codes: (ii) −x, −y+1, −z−1; (iii) −x, −y+1, −z; (iv) x, y−1, z+2. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C13H14N2)4(H2O)2](NO3)2·2H2O |
Mr | 1101.53 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 9.3189 (2), 11.6565 (3), 12.0590 (1) |
α, β, γ (°) | 80.845 (1), 86.638 (1), 89.051 (1) |
V (Å3) | 1290.97 (4) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.49 |
Crystal size (mm) | 0.32 × 0.17 × 0.15 |
Data collection | |
Diffractometer | Smart CCD diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.855, 0.929 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6516, 4428, 3749 |
Rint | 0.024 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.044, 0.126, 1.10 |
No. of reflections | 4428 |
No. of parameters | 347 |
No. of restraints | 4 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.35, −0.75 |
Computer programs: SMART (Siemens, 1994), SMART, SAINT (Siemens, 1994), SHELXTL (Sheldrick, 1997), SHELXTL.
Cd—O1 | 2.295 (3) | Cd—N3 | 2.405 (3) |
Cd—N1 | 2.363 (3) | ||
O1—Cd—N1 | 85.56 (12) | N1—Cd—N3 | 86.30 (11) |
O1—Cd—N3 | 87.97 (12) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—HOA···O12i | 0.94 (2) | 1.86 (2) | 2.796 (5) | 174 (5) |
O1—HOB···O101i | 0.935 (19) | 1.76 (2) | 2.691 (6) | 173 (4) |
O101—H01···N4ii | 0.875 (18) | 2.30 (3) | 3.054 (8) | 144 (3) |
O101—H02···N2iii | 0.95 (2) | 2.30 (7) | 3.074 (6) | 138 (8) |
Symmetry codes: (i) −x, −y+1, −z−1; (ii) −x, −y+1, −z; (iii) x, y−1, z+2. |
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In recent decades, there has been great interest in the study of metal–organic supramolecular frameworks owing to their intriguing structral diversity and potential application in catalysis, separation and molecular recognization (Piguet et al., 1997; Yaghi et al., 1998; Swiegers et al., 2000). In the construction of one-, two- and three-dimensional frameworks, the rational design and selection of ligands are crucial for the formation of metal–organic coordination frameworks. For example, many rigid ligands, such as 4,4-bipyridine or polycarboxylic acids, and flexible ligands, such as bipyridine derivatives with spacers, have been extensively employed in the formation of supramolecular architectures (Yang et al., 2001; Wang et al., 2001; Horikoshi et al., 2001). The displacement of oligopyridine by oligoaniline should result in new structural motifs and new topologies, but oligoaniline ligands are seldom employed (Zhang et al., 1999). In this paper, we report the crystal structure of [Cd(dadpm)4(H2O)2](NO3)2·2H2O, (I), obtained from the self-assembly of dadpm and Cd(NO3)2.
Compound (I) is a mononuclear CdII complex and dadpm serves as a monodentate ligand (Fig. 1). The Cd atom is coordinated by N atoms from four different dadpm ligands and O atoms from two water molecules, forming a distorted octahedral coordination fashion of CdN4O2. The Cd—N and Cd—O bond distances are 2.363 (3)–2.405 (3) and 2.295 (3) Å, respectively (Table 1).