Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807031200/bq2024sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807031200/bq2024Isup2.hkl |
CCDC reference: 657521
The title complex was prepared according to the literature method (Zhang et al., 2007a). Crystals were obtained by slow evaporation (one month) of a methanol solution(15 ml), with including the complex (1) (0.066 g, 0.1 mmol).
H atoms bound to C atoms were included in calculated positions and allowed to ride during subsequent refinement, with C—H = 0.93Å and Uiso(H) = 1.2Ueq(C) for Csp2, and C—H = 0.96Å and Uiso (H) = 1.5Ueq(C) for the methyl groups. H atoms bound to N atoms were located in difference Fourier map and refined with N—H = 0.86 Å, and Uiso(H) = 1.2Ueq(N). In the crystal structure, the aromatic ring and methoxyl is disordered. The occupancy of the major component of disordered is 0.527, and the occupancy of the minor part is 0.473, the disorder was refined by using the AFIX, FLAT and ISOR restrains.
Recently, we have reported the nickel and zinc complexes with the [N,N'-bis(4-methoxylbenzyl)ethane-1,2-diyldiimino] diacetate (Zhang, Weng & Xu, 2007; Zhang, Weng, Hu & Xu, 2007). In this paper, we continue reporting the structure of the Cd(II) complex, Cd(La)(Lb)2.2H2O(La=[N,N'-bis(4-methoxyl- benzyl)ethane-1,2-diyldiimino]diacetate, Lb=imidazole)(1). In (1), the cadmium atom is also in a slightly distorted octahedral coordination environment (Fig. 1), which is similar to the zinc complex without the longer bond lengths (Table 1), and there is a disorder in one of the 4-methoxylbenzyl groups. In the crystal structure, the hydrogen bonds (Table 2) consolidate the crystal packing into infinite one-dimensional chains (Fig 2).
Recently, we have reported similar nickel and zinc complexes with [N,N'-bis(4-methoxybenzyl)ethane-1,2-diyldiimino]diacetate (Zhang, Weng & Xu, 2007; Zhang, Weng, Hu & Xu, 2007).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[Cd(C22H26N2O6)(C3H4N2)2]·2H2O | F(000) = 2880 |
Mr = 699.04 | Dx = 1.459 Mg m−3 |
Orthorhombic, Pcab | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2bc 2ac | Cell parameters from 5642 reflections |
a = 15.7646 (8) Å | θ = 2.4–22.5° |
b = 16.3172 (8) Å | µ = 0.74 mm−1 |
c = 24.7351 (12) Å | T = 292 K |
V = 6362.7 (5) Å3 | Plate, colorless |
Z = 8 | 0.30 × 0.25 × 0.07 mm |
Bruker SMART CCD area-detector diffractometer | 6253 independent reflections |
Radiation source: fine-focus sealed tube | 3809 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.088 |
φ and ω scans | θmax = 26.0°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | h = −19→19 |
Tmin = 0.796, Tmax = 0.949 | k = −20→20 |
63596 measured reflections | l = −30→30 |
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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.179 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0819P)2 + 6.7434P] where P = (Fo2 + 2Fc2)/3 |
6253 reflections | (Δ/σ)max < 0.001 |
430 parameters | Δρmax = 0.69 e Å−3 |
102 restraints | Δρmin = −0.78 e Å−3 |
[Cd(C22H26N2O6)(C3H4N2)2]·2H2O | V = 6362.7 (5) Å3 |
Mr = 699.04 | Z = 8 |
Orthorhombic, Pcab | Mo Kα radiation |
a = 15.7646 (8) Å | µ = 0.74 mm−1 |
b = 16.3172 (8) Å | T = 292 K |
c = 24.7351 (12) Å | 0.30 × 0.25 × 0.07 mm |
Bruker SMART CCD area-detector diffractometer | 6253 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | 3809 reflections with I > 2σ(I) |
Tmin = 0.796, Tmax = 0.949 | Rint = 0.088 |
63596 measured reflections |
R[F2 > 2σ(F2)] = 0.059 | 102 restraints |
wR(F2) = 0.179 | H-atom parameters constrained |
S = 1.03 | Δρmax = 0.69 e Å−3 |
6253 reflections | Δρmin = −0.78 e Å−3 |
430 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 | Occ. (<1) | |
Cd1 | 0.36406 (3) | 0.17511 (2) | 0.249249 (14) | 0.06385 (18) | |
C1 | 0.606 (2) | −0.2625 (18) | 0.4734 (13) | 0.139 (10) | 0.456 (14) |
H1A | 0.5778 | −0.2972 | 0.4476 | 0.209* | 0.456 (14) |
H1B | 0.6125 | −0.2916 | 0.5068 | 0.209* | 0.456 (14) |
H1C | 0.6601 | −0.2466 | 0.4598 | 0.209* | 0.456 (14) |
O1 | 0.5578 (12) | −0.1948 (15) | 0.4820 (10) | 0.139 (7) | 0.456 (14) |
C2 | 0.5431 (13) | −0.1292 (13) | 0.4356 (15) | 0.118 (11) | 0.456 (14) |
C3 | 0.5056 (7) | −0.0690 (8) | 0.4603 (4) | 0.171 (13) | 0.456 (14) |
H3 | 0.5014 | −0.0598 | 0.4973 | 0.205* | 0.456 (14) |
C4 | 0.4733 (7) | −0.0219 (8) | 0.4186 (4) | 0.113 (8) | 0.456 (14) |
H4 | 0.4312 | 0.0147 | 0.4290 | 0.136* | 0.456 (14) |
C5 | 0.4929 (7) | −0.0197 (8) | 0.3641 (4) | 0.087 (10) | 0.456 (14) |
C6 | 0.5234 (7) | −0.0970 (8) | 0.3513 (4) | 0.080 (5) | 0.456 (14) |
H6 | 0.5290 | −0.1093 | 0.3148 | 0.096* | 0.456 (14) |
C7 | 0.5466 (7) | −0.1580 (8) | 0.3877 (4) | 0.081 (8) | 0.456 (14) |
H7 | 0.5714 | −0.2071 | 0.3771 | 0.097* | 0.456 (14) |
C1' | 0.595 (3) | −0.217 (2) | 0.4931 (16) | 0.194 (17) | 0.544 (14) |
H1'1 | 0.6369 | −0.1757 | 0.4999 | 0.291* | 0.544 (14) |
H1'2 | 0.6137 | −0.2685 | 0.5070 | 0.291* | 0.544 (14) |
H1'3 | 0.5426 | −0.2016 | 0.5106 | 0.291* | 0.544 (14) |
O1' | 0.5810 (9) | −0.2234 (7) | 0.4373 (6) | 0.145 (5) | 0.544 (14) |
C2' | 0.5414 (8) | −0.1585 (11) | 0.4180 (13) | 0.107 (9) | 0.544 (14) |
C3' | 0.5194 (5) | −0.0834 (5) | 0.4385 (3) | 0.114 (7) | 0.544 (14) |
H3' | 0.5149 | −0.0801 | 0.4760 | 0.137* | 0.544 (14) |
C4' | 0.5029 (5) | −0.0118 (5) | 0.4101 (3) | 0.082 (5) | 0.544 (14) |
H4' | 0.4965 | 0.0394 | 0.4262 | 0.099* | 0.544 (14) |
C5' | 0.4973 (5) | −0.0255 (5) | 0.3552 (3) | 0.062 (5) | 0.544 (14) |
C6' | 0.5277 (5) | −0.0922 (5) | 0.3271 (3) | 0.062 (3) | 0.544 (14) |
H6' | 0.5296 | −0.0921 | 0.2895 | 0.075* | 0.544 (14) |
C7' | 0.5553 (5) | −0.1593 (5) | 0.3564 (3) | 0.078 (4) | 0.544 (14) |
H7' | 0.5743 | −0.2066 | 0.3393 | 0.094* | 0.544 (14) |
C8 | 0.4723 (3) | 0.0483 (3) | 0.3220 (2) | 0.0719 (14) | |
H8A | 0.4929 | 0.1002 | 0.3360 | 0.086* | |
H8B | 0.5037 | 0.0367 | 0.2891 | 0.086* | |
C9 | 0.3283 (3) | 0.0752 (3) | 0.3551 (2) | 0.0689 (13) | |
H9A | 0.3596 | 0.1101 | 0.3797 | 0.083* | |
H9B | 0.3161 | 0.0242 | 0.3737 | 0.083* | |
C10 | 0.2442 (3) | 0.1174 (4) | 0.3402 (2) | 0.0758 (15) | |
C11 | 0.3464 (3) | −0.0126 (3) | 0.2774 (2) | 0.0692 (13) | |
H11A | 0.2849 | −0.0113 | 0.2795 | 0.083* | |
H11B | 0.3655 | −0.0630 | 0.2943 | 0.083* | |
C12 | 0.3724 (3) | −0.0130 (3) | 0.2191 (2) | 0.0708 (14) | |
H12A | 0.4337 | −0.0159 | 0.2171 | 0.085* | |
H12B | 0.3497 | −0.0617 | 0.2020 | 0.085* | |
C13 | 0.2532 (3) | 0.0536 (3) | 0.1719 (2) | 0.0711 (14) | |
H13A | 0.2367 | 0.1062 | 0.1570 | 0.085* | |
H13B | 0.2189 | 0.0446 | 0.2039 | 0.085* | |
C14 | 0.2313 (3) | −0.0116 (4) | 0.1313 (2) | 0.0719 (14) | |
C15 | 0.2008 (3) | −0.0873 (4) | 0.1453 (3) | 0.0824 (16) | |
H15 | 0.1925 | −0.1001 | 0.1816 | 0.099* | |
C16 | 0.1814 (4) | −0.1468 (4) | 0.1046 (3) | 0.0864 (17) | |
H16 | 0.1607 | −0.1983 | 0.1138 | 0.104* | |
C17 | 0.1943 (4) | −0.1258 (5) | 0.0520 (3) | 0.0930 (18) | |
C18 | 0.2213 (5) | −0.0515 (5) | 0.0374 (3) | 0.119 (3) | |
H18 | 0.2278 | −0.0381 | 0.0011 | 0.143* | |
C19 | 0.2390 (4) | 0.0038 (4) | 0.0765 (2) | 0.100 (2) | |
H19 | 0.2576 | 0.0554 | 0.0659 | 0.120* | |
C20 | 0.1472 (6) | −0.2579 (6) | 0.0218 (4) | 0.158 (4) | |
H20A | 0.1911 | −0.2975 | 0.0153 | 0.236* | |
H20B | 0.0989 | −0.2702 | −0.0003 | 0.236* | |
H20C | 0.1311 | −0.2596 | 0.0593 | 0.236* | |
C21 | 0.4002 (4) | 0.0757 (3) | 0.1429 (2) | 0.0767 (15) | |
H21A | 0.3731 | 0.1142 | 0.1186 | 0.092* | |
H21B | 0.4098 | 0.0251 | 0.1232 | 0.092* | |
C22 | 0.4853 (3) | 0.1106 (4) | 0.1615 (2) | 0.0784 (15) | |
C23 | 0.2216 (3) | 0.2934 (3) | 0.1992 (2) | 0.0703 (13) | |
H23 | 0.1878 | 0.2848 | 0.2295 | 0.084* | |
C24 | 0.3236 (3) | 0.2919 (3) | 0.1431 (2) | 0.0717 (14) | |
H24 | 0.3761 | 0.2817 | 0.1274 | 0.086* | |
C25 | 0.2623 (4) | 0.3350 (4) | 0.1210 (2) | 0.0786 (16) | |
H25 | 0.2633 | 0.3595 | 0.0871 | 0.094* | |
C26 | 0.5097 (3) | 0.2857 (3) | 0.3045 (2) | 0.0728 (14) | |
H26 | 0.5452 | 0.2743 | 0.2754 | 0.087* | |
C27 | 0.4026 (3) | 0.2913 (3) | 0.3560 (2) | 0.0693 (13) | |
H27 | 0.3483 | 0.2840 | 0.3700 | 0.083* | |
C28 | 0.4646 (4) | 0.3341 (3) | 0.3792 (2) | 0.0770 (15) | |
H28 | 0.4615 | 0.3618 | 0.4120 | 0.092* | |
N1 | 0.3811 (2) | 0.0579 (2) | 0.30784 (17) | 0.0612 (10) | |
N2 | 0.3434 (3) | 0.0594 (3) | 0.18910 (17) | 0.0651 (11) | |
N3 | 0.2983 (3) | 0.2641 (2) | 0.19315 (15) | 0.0650 (10) | |
N4 | 0.1983 (3) | 0.3369 (3) | 0.15648 (19) | 0.0759 (12) | |
H4A | 0.1507 | 0.3619 | 0.1523 | 0.091* | |
N5 | 0.4319 (3) | 0.2597 (2) | 0.30825 (16) | 0.0656 (10) | |
N6 | 0.5323 (3) | 0.3302 (3) | 0.34665 (19) | 0.0773 (13) | |
H6A | 0.5811 | 0.3524 | 0.3521 | 0.093* | |
O2 | 0.2394 (2) | 0.1595 (2) | 0.29840 (15) | 0.0792 (10) | |
O3 | 0.1857 (3) | 0.1072 (3) | 0.37274 (18) | 0.1179 (17) | |
O4 | 0.4891 (2) | 0.1547 (2) | 0.20236 (15) | 0.0778 (10) | |
O5 | 0.5458 (3) | 0.0944 (3) | 0.1314 (2) | 0.1219 (18) | |
O6 | 0.1771 (4) | −0.1803 (4) | 0.0092 (2) | 0.1312 (19) | |
O7 | 0.1167 (7) | 0.0124 (8) | 0.4537 (5) | 0.337 (7)* | |
H7A | 0.1411 | 0.0432 | 0.4308 | 0.404* | |
H7B | 0.1498 | −0.0274 | 0.4605 | 0.404* | |
O8 | 0.990 (3) | 0.0651 (17) | 0.5068 (17) | 0.87 (3)* | |
H8C | 0.9998 | 0.1160 | 0.5108 | 1.042* | |
H8D | 0.9668 | 0.0586 | 0.4761 | 1.042* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0626 (3) | 0.0620 (3) | 0.0670 (3) | −0.00006 (17) | −0.00320 (17) | −0.00432 (18) |
C1 | 0.133 (16) | 0.17 (3) | 0.119 (19) | 0.078 (18) | 0.017 (14) | 0.032 (18) |
O1 | 0.138 (13) | 0.158 (16) | 0.120 (16) | 0.060 (11) | 0.020 (10) | 0.050 (12) |
C2 | 0.147 (19) | 0.050 (18) | 0.16 (2) | −0.014 (12) | −0.055 (16) | −0.005 (15) |
C3 | 0.24 (3) | 0.20 (2) | 0.076 (14) | 0.11 (2) | −0.052 (15) | −0.047 (13) |
C4 | 0.066 (10) | 0.16 (2) | 0.116 (15) | −0.002 (10) | −0.023 (9) | 0.012 (14) |
C5 | 0.057 (14) | 0.050 (13) | 0.16 (2) | 0.003 (11) | 0.001 (14) | −0.019 (16) |
C6 | 0.080 (10) | 0.105 (13) | 0.055 (10) | −0.005 (9) | 0.011 (8) | −0.008 (9) |
C7 | 0.058 (9) | 0.079 (13) | 0.105 (17) | 0.020 (7) | 0.050 (12) | −0.017 (11) |
C1' | 0.26 (4) | 0.19 (3) | 0.13 (3) | 0.10 (3) | 0.01 (3) | 0.07 (2) |
O1' | 0.171 (11) | 0.121 (9) | 0.142 (11) | 0.054 (7) | 0.004 (9) | 0.060 (8) |
C2' | 0.089 (12) | 0.035 (12) | 0.20 (3) | 0.003 (7) | −0.058 (12) | −0.001 (11) |
C3' | 0.190 (18) | 0.089 (12) | 0.062 (9) | 0.047 (12) | −0.034 (9) | −0.005 (10) |
C4' | 0.100 (11) | 0.083 (9) | 0.063 (8) | 0.026 (7) | −0.012 (7) | 0.002 (7) |
C5' | 0.048 (10) | 0.072 (14) | 0.067 (7) | 0.015 (9) | −0.014 (6) | −0.008 (8) |
C6' | 0.053 (6) | 0.060 (6) | 0.073 (8) | 0.016 (5) | 0.008 (5) | −0.008 (5) |
C7' | 0.060 (7) | 0.077 (8) | 0.097 (10) | 0.025 (6) | 0.016 (7) | −0.008 (8) |
C8 | 0.057 (3) | 0.072 (3) | 0.087 (4) | 0.002 (3) | −0.008 (3) | −0.009 (3) |
C9 | 0.064 (3) | 0.072 (3) | 0.071 (3) | 0.004 (3) | 0.000 (3) | 0.004 (3) |
C10 | 0.061 (3) | 0.084 (4) | 0.082 (4) | 0.012 (3) | 0.004 (3) | 0.004 (3) |
C11 | 0.059 (3) | 0.062 (3) | 0.087 (4) | −0.007 (2) | −0.014 (3) | 0.004 (3) |
C12 | 0.060 (3) | 0.064 (3) | 0.088 (4) | 0.002 (3) | −0.008 (3) | −0.017 (3) |
C13 | 0.056 (3) | 0.082 (3) | 0.075 (3) | 0.003 (3) | −0.007 (3) | −0.004 (3) |
C14 | 0.051 (3) | 0.084 (4) | 0.080 (4) | −0.002 (3) | −0.009 (2) | −0.010 (3) |
C15 | 0.051 (3) | 0.109 (5) | 0.087 (4) | −0.007 (3) | −0.006 (3) | −0.007 (4) |
C16 | 0.065 (4) | 0.081 (4) | 0.113 (5) | −0.011 (3) | −0.011 (3) | −0.003 (4) |
C17 | 0.084 (4) | 0.123 (6) | 0.072 (4) | 0.000 (4) | 0.000 (3) | −0.013 (4) |
C18 | 0.144 (7) | 0.137 (6) | 0.077 (4) | −0.040 (6) | 0.005 (4) | −0.013 (5) |
C19 | 0.111 (5) | 0.113 (5) | 0.075 (4) | −0.026 (4) | −0.015 (4) | −0.008 (4) |
C20 | 0.183 (9) | 0.128 (7) | 0.162 (9) | −0.060 (7) | −0.014 (7) | −0.027 (7) |
C21 | 0.075 (4) | 0.083 (4) | 0.072 (3) | −0.003 (3) | 0.001 (3) | −0.011 (3) |
C22 | 0.063 (3) | 0.085 (4) | 0.087 (4) | −0.006 (3) | 0.009 (3) | −0.017 (3) |
C23 | 0.067 (3) | 0.071 (3) | 0.073 (3) | −0.005 (3) | 0.012 (3) | 0.006 (3) |
C24 | 0.062 (3) | 0.085 (4) | 0.069 (3) | −0.010 (3) | 0.009 (3) | −0.001 (3) |
C25 | 0.071 (4) | 0.098 (4) | 0.066 (3) | −0.009 (3) | 0.000 (3) | 0.017 (3) |
C26 | 0.069 (3) | 0.076 (4) | 0.073 (3) | −0.003 (3) | 0.010 (3) | −0.005 (3) |
C27 | 0.067 (3) | 0.068 (3) | 0.073 (3) | 0.003 (3) | 0.005 (3) | −0.003 (3) |
C28 | 0.087 (4) | 0.079 (4) | 0.065 (3) | 0.004 (3) | −0.003 (3) | −0.006 (3) |
N1 | 0.049 (2) | 0.064 (2) | 0.070 (3) | −0.0001 (18) | −0.0074 (19) | −0.005 (2) |
N2 | 0.054 (2) | 0.070 (3) | 0.071 (3) | −0.002 (2) | −0.003 (2) | −0.007 (2) |
N3 | 0.061 (2) | 0.067 (3) | 0.067 (2) | −0.003 (2) | 0.002 (2) | 0.000 (2) |
N4 | 0.059 (3) | 0.079 (3) | 0.090 (3) | 0.000 (2) | −0.002 (2) | 0.014 (2) |
N5 | 0.062 (2) | 0.064 (3) | 0.071 (3) | 0.000 (2) | −0.002 (2) | −0.001 (2) |
N6 | 0.068 (3) | 0.083 (3) | 0.081 (3) | −0.014 (2) | −0.008 (3) | −0.011 (2) |
O2 | 0.066 (2) | 0.088 (3) | 0.083 (2) | 0.0163 (19) | 0.0032 (19) | 0.017 (2) |
O3 | 0.082 (3) | 0.161 (4) | 0.111 (3) | 0.040 (3) | 0.032 (3) | 0.050 (3) |
O4 | 0.068 (2) | 0.086 (3) | 0.080 (2) | −0.0121 (19) | 0.0034 (19) | −0.018 (2) |
O5 | 0.074 (3) | 0.159 (4) | 0.133 (4) | −0.027 (3) | 0.026 (3) | −0.067 (3) |
O6 | 0.152 (5) | 0.146 (5) | 0.096 (3) | −0.027 (4) | 0.004 (3) | −0.033 (3) |
Cd1—N3 | 2.261 (4) | C11—H11A | 0.9700 |
Cd1—N5 | 2.276 (4) | C11—H11B | 0.9700 |
Cd1—O4 | 2.311 (4) | C12—N2 | 1.468 (7) |
Cd1—O2 | 2.325 (4) | C12—H12A | 0.9700 |
Cd1—N1 | 2.415 (4) | C12—H12B | 0.9700 |
Cd1—N2 | 2.426 (4) | C13—N2 | 1.487 (6) |
C1—O1 | 1.35 (4) | C13—C14 | 1.504 (7) |
C1—H1A | 0.9600 | C13—H13A | 0.9700 |
C1—H1B | 0.9600 | C13—H13B | 0.9700 |
C1—H1C | 0.9600 | C14—C15 | 1.372 (8) |
O1—C2 | 1.59 (4) | C14—C19 | 1.383 (7) |
C2—C7 | 1.28 (3) | C15—C16 | 1.432 (8) |
C2—C3 | 1.30 (3) | C15—H15 | 0.9300 |
C3—C4 | 1.3829 | C16—C17 | 1.361 (8) |
C3—H3 | 0.9300 | C16—H16 | 0.9300 |
C4—C5 | 1.3841 | C17—C18 | 1.334 (9) |
C4—H4 | 0.9300 | C17—O6 | 1.409 (7) |
C4—H4' | 1.0807 | C18—C19 | 1.351 (8) |
C5—C6 | 1.3860 | C18—H18 | 0.9300 |
C5—C8 | 1.556 (13) | C19—H19 | 0.9300 |
C6—C7 | 1.3910 | C20—O6 | 1.386 (9) |
C6—H6 | 0.9300 | C20—H20A | 0.9600 |
C7—H7 | 0.9300 | C20—H20B | 0.9600 |
C1'—O1' | 1.40 (5) | C20—H20C | 0.9600 |
C1'—H1'1 | 0.9600 | C21—N2 | 1.475 (7) |
C1'—H1'2 | 0.9600 | C21—C22 | 1.528 (8) |
C1'—H1'3 | 0.9600 | C21—H21A | 0.9700 |
O1'—C2' | 1.32 (2) | C21—H21B | 0.9700 |
C2'—C3' | 1.37 (2) | C22—O5 | 1.239 (6) |
C2'—C7' | 1.54 (3) | C22—O4 | 1.241 (6) |
C3'—C4' | 1.3893 | C23—N3 | 1.309 (6) |
C3'—H3' | 0.9300 | C23—N4 | 1.324 (6) |
C4'—C5' | 1.3786 | C23—H23 | 0.9300 |
C4'—H4 | 1.2981 | C24—C25 | 1.314 (7) |
C4'—H4' | 0.9300 | C24—N3 | 1.376 (6) |
C5'—C6' | 1.3787 | C24—H24 | 0.9300 |
C5'—C8 | 1.509 (9) | C25—N4 | 1.337 (7) |
C6'—C7' | 1.3835 | C25—H25 | 0.9300 |
C6'—H6 | 0.4131 | C26—N5 | 1.301 (6) |
C6'—H6' | 0.9300 | C26—N6 | 1.320 (6) |
C7'—H7 | 0.9680 | C26—H26 | 0.9300 |
C7'—H7' | 0.9300 | C27—C28 | 1.332 (7) |
C8—N1 | 1.489 (6) | C27—N5 | 1.370 (6) |
C8—H8A | 0.9700 | C27—H27 | 0.9300 |
C8—H8B | 0.9700 | C28—N6 | 1.339 (7) |
C9—N1 | 1.462 (7) | C28—H28 | 0.9300 |
C9—C10 | 1.538 (7) | N4—H4A | 0.8600 |
C9—H9A | 0.9700 | N6—H6A | 0.8600 |
C9—H9B | 0.9700 | O7—H7A | 0.8501 |
C10—O3 | 1.235 (6) | O7—H7B | 0.8500 |
C10—O2 | 1.244 (6) | O8—H8C | 0.8501 |
C11—N1 | 1.479 (6) | O8—H8D | 0.8500 |
C11—C12 | 1.499 (8) | ||
N3—Cd1—N5 | 102.70 (14) | N1—C11—H11A | 109.0 |
N3—Cd1—O4 | 100.12 (14) | C12—C11—H11A | 109.0 |
N5—Cd1—O4 | 90.49 (13) | N1—C11—H11B | 109.0 |
N3—Cd1—O2 | 90.21 (13) | C12—C11—H11B | 109.0 |
N5—Cd1—O2 | 97.39 (14) | H11A—C11—H11B | 107.8 |
O4—Cd1—O2 | 165.35 (14) | N2—C12—C11 | 113.5 (4) |
N3—Cd1—N1 | 158.18 (13) | N2—C12—H12A | 108.9 |
N5—Cd1—N1 | 92.47 (14) | C11—C12—H12A | 108.9 |
O4—Cd1—N1 | 95.28 (13) | N2—C12—H12B | 108.9 |
O2—Cd1—N1 | 72.15 (13) | C11—C12—H12B | 108.9 |
N3—Cd1—N2 | 93.55 (14) | H12A—C12—H12B | 107.7 |
N5—Cd1—N2 | 158.19 (14) | N2—C13—C14 | 117.0 (4) |
O4—Cd1—N2 | 72.21 (13) | N2—C13—H13A | 108.0 |
O2—Cd1—N2 | 96.99 (14) | C14—C13—H13A | 108.0 |
N1—Cd1—N2 | 76.49 (16) | N2—C13—H13B | 108.0 |
C1—O1—C2 | 121 (2) | C14—C13—H13B | 108.0 |
C7—C2—C3 | 137 (3) | H13A—C13—H13B | 107.3 |
C7—C2—O1 | 114.6 (19) | C15—C14—C19 | 116.2 (5) |
C3—C2—O1 | 104 (2) | C15—C14—C13 | 123.3 (5) |
C2—C3—C4 | 103.8 (17) | C19—C14—C13 | 120.5 (6) |
C2—C3—H3 | 128.1 | C14—C15—C16 | 120.5 (6) |
C4—C3—H3 | 128.1 | C14—C15—H15 | 119.8 |
C3—C4—C5 | 131.2 | C16—C15—H15 | 119.8 |
C3—C4—H4 | 114.4 | C17—C16—C15 | 118.0 (6) |
C5—C4—H4 | 114.4 | C17—C16—H16 | 121.0 |
C3—C4—H4' | 105.2 | C15—C16—H16 | 121.0 |
C5—C4—H4' | 94.0 | C18—C17—C16 | 122.4 (6) |
H4—C4—H4' | 66.3 | C18—C17—O6 | 115.6 (6) |
C4—C5—C6 | 106.0 | C16—C17—O6 | 122.0 (7) |
C4—C5—C8 | 128.6 (4) | C17—C18—C19 | 118.6 (7) |
C6—C5—C8 | 124.7 (5) | C17—C18—H18 | 120.7 |
C5—C6—C7 | 126.5 | C19—C18—H18 | 120.7 |
C5—C6—H6 | 116.8 | C18—C19—C14 | 124.2 (7) |
C7—C6—H6 | 116.8 | C18—C19—H19 | 117.9 |
C5—C6—H6' | 101.6 | C14—C19—H19 | 117.9 |
C7—C6—H6' | 131.8 | O6—C20—H20A | 109.5 |
C2—C7—C6 | 109.1 (14) | O6—C20—H20B | 109.5 |
C2—C7—H7 | 126.7 | H20A—C20—H20B | 109.5 |
C6—C7—H7 | 123.0 | O6—C20—H20C | 109.5 |
C2—C7—H7' | 161.4 | H20A—C20—H20C | 109.5 |
C6—C7—H7' | 86.5 | H20B—C20—H20C | 109.5 |
O1'—C1'—H1'1 | 109.5 | N2—C21—C22 | 111.5 (5) |
O1'—C1'—H1'2 | 109.5 | N2—C21—H21A | 109.3 |
H1'1—C1'—H1'2 | 109.5 | C22—C21—H21A | 109.3 |
O1'—C1'—H1'3 | 109.5 | N2—C21—H21B | 109.3 |
H1'1—C1'—H1'3 | 109.5 | C22—C21—H21B | 109.3 |
H1'2—C1'—H1'3 | 109.5 | H21A—C21—H21B | 108.0 |
C2'—O1'—C1' | 112 (2) | O5—C22—O4 | 125.1 (5) |
O1'—C2'—C3' | 135 (2) | O5—C22—C21 | 114.6 (5) |
O1'—C2'—C7' | 106.6 (17) | O4—C22—C21 | 120.2 (5) |
C3'—C2'—C7' | 114.2 (17) | N3—C23—N4 | 111.2 (5) |
O1'—C2'—H7 | 68.9 | N3—C23—H23 | 124.4 |
C3'—C2'—H7 | 151.5 | N4—C23—H23 | 124.4 |
C2'—C3'—C4' | 127.7 (13) | C25—C24—N3 | 109.7 (5) |
C2'—C3'—H3' | 116.2 | C25—C24—H24 | 125.1 |
C4'—C3'—H3' | 116.2 | N3—C24—H24 | 125.1 |
C5'—C4'—C3' | 112.0 | C24—C25—N4 | 107.2 (5) |
C5'—C4'—H4 | 110.7 | C24—C25—H25 | 126.4 |
C3'—C4'—H4 | 105.1 | N4—C25—H25 | 126.4 |
C5'—C4'—H4' | 124.0 | N5—C26—N6 | 112.2 (5) |
C3'—C4'—H4' | 124.0 | N5—C26—H26 | 123.9 |
H4—C4'—H4' | 56.8 | N6—C26—H26 | 123.9 |
C4'—C5'—C6' | 127.1 | C28—C27—N5 | 108.7 (5) |
C4'—C5'—C8 | 115.0 (4) | C28—C27—H27 | 125.6 |
C6'—C5'—C8 | 116.5 (4) | N5—C27—H27 | 125.6 |
C5'—C6'—C7' | 118.0 | C27—C28—N6 | 107.5 (5) |
C5'—C6'—H6 | 157.3 | C27—C28—H28 | 126.2 |
C7'—C6'—H6 | 80.5 | N6—C28—H28 | 126.2 |
C5'—C6'—H6' | 121.0 | C9—N1—C11 | 110.2 (4) |
C7'—C6'—H6' | 121.0 | C9—N1—C8 | 112.5 (4) |
C6'—C7'—C2' | 117.9 (7) | C11—N1—C8 | 113.3 (4) |
C2'—C7'—H6 | 133.8 | C9—N1—Cd1 | 105.3 (3) |
C6'—C7'—H7 | 176.9 | C11—N1—Cd1 | 105.6 (3) |
C2'—C7'—H7 | 61.2 | C8—N1—Cd1 | 109.4 (3) |
H6—C7'—H7 | 162.4 | C12—N2—C21 | 110.3 (4) |
C6'—C7'—H7' | 121.4 | C12—N2—C13 | 113.1 (4) |
C2'—C7'—H7' | 120.1 | C21—N2—C13 | 111.7 (4) |
H6—C7'—H7' | 104.5 | C12—N2—Cd1 | 105.9 (3) |
N1—C8—C5' | 117.6 (5) | C21—N2—Cd1 | 104.7 (3) |
N1—C8—C5 | 115.7 (6) | C13—N2—Cd1 | 110.7 (3) |
N1—C8—H8A | 108.4 | C23—N3—C24 | 104.5 (4) |
C5'—C8—H8A | 114.5 | C23—N3—Cd1 | 126.1 (3) |
C5—C8—H8A | 108.4 | C24—N3—Cd1 | 129.1 (4) |
N1—C8—H8B | 108.4 | C23—N4—C25 | 107.5 (5) |
C5'—C8—H8B | 99.6 | C23—N4—H4A | 126.2 |
C5—C8—H8B | 108.4 | C25—N4—H4A | 126.2 |
H8A—C8—H8B | 107.4 | C26—N5—C27 | 104.9 (4) |
N1—C9—C10 | 112.8 (4) | C26—N5—Cd1 | 126.5 (4) |
N1—C9—H9A | 109.0 | C27—N5—Cd1 | 128.5 (3) |
C10—C9—H9A | 109.0 | C26—N6—C28 | 106.6 (5) |
N1—C9—H9B | 109.0 | C26—N6—H6A | 126.7 |
C10—C9—H9B | 109.0 | C28—N6—H6A | 126.7 |
H9A—C9—H9B | 107.8 | C10—O2—Cd1 | 116.3 (3) |
O3—C10—O2 | 124.8 (5) | C22—O4—Cd1 | 116.8 (3) |
O3—C10—C9 | 115.3 (5) | C20—O6—C17 | 118.2 (6) |
O2—C10—C9 | 119.9 (5) | H7A—O7—H7B | 107.7 |
N1—C11—C12 | 113.0 (4) | H8C—O8—H8D | 107.7 |
C1—O1—C2—C7 | 28 (3) | O4—Cd1—N1—C8 | 36.9 (3) |
C1—O1—C2—C3 | −171 (2) | O2—Cd1—N1—C8 | −150.8 (3) |
C7—C2—C3—C4 | −11.3 (16) | N2—Cd1—N1—C8 | 107.1 (3) |
O1—C2—C3—C4 | −165.1 (11) | C11—C12—N2—C21 | 153.7 (4) |
C2—C3—C4—C5 | −17.6 (5) | C11—C12—N2—C13 | −80.3 (5) |
C3—C4—C5—C6 | 26.7 | C11—C12—N2—Cd1 | 41.0 (4) |
C3—C4—C5—C8 | −162.5 (6) | C22—C21—N2—C12 | −73.1 (5) |
C4—C5—C6—C7 | −12.3 | C22—C21—N2—C13 | 160.2 (4) |
C8—C5—C6—C7 | 176.5 (6) | C22—C21—N2—Cd1 | 40.4 (5) |
C3—C2—C7—C6 | 21.6 (16) | C14—C13—N2—C12 | −65.7 (6) |
O1—C2—C7—C6 | 173.4 (11) | C14—C13—N2—C21 | 59.5 (6) |
C5—C6—C7—C2 | −6.1 (6) | C14—C13—N2—Cd1 | 175.7 (4) |
C1'—O1'—C2'—C3' | 9 (3) | N3—Cd1—N2—C12 | −173.3 (3) |
C1'—O1'—C2'—C7' | 162 (2) | N5—Cd1—N2—C12 | 48.3 (6) |
O1'—C2'—C3'—C4' | 157.1 (17) | O4—Cd1—N2—C12 | 87.2 (3) |
C7'—C2'—C3'—C4' | 4.8 (9) | O2—Cd1—N2—C12 | −82.6 (3) |
C2'—C3'—C4'—C5' | 10.0 (5) | N1—Cd1—N2—C12 | −12.9 (3) |
C3'—C4'—C5'—C6' | −18.9 | N3—Cd1—N2—C21 | 70.1 (3) |
C3'—C4'—C5'—C8 | 175.2 (4) | N5—Cd1—N2—C21 | −68.3 (5) |
C4'—C5'—C6'—C7' | 11.0 | O4—Cd1—N2—C21 | −29.4 (3) |
C8—C5'—C6'—C7' | 176.7 (4) | O2—Cd1—N2—C21 | 160.8 (3) |
C5'—C6'—C7'—C2' | 6.3 (4) | N1—Cd1—N2—C21 | −129.5 (3) |
O1'—C2'—C7'—C6' | −173.0 (8) | N3—Cd1—N2—C13 | −50.4 (3) |
C3'—C2'—C7'—C6' | −13.3 (8) | N5—Cd1—N2—C13 | 171.2 (4) |
C4'—C5'—C8—N1 | −95.8 (4) | O4—Cd1—N2—C13 | −149.9 (4) |
C6'—C5'—C8—N1 | 96.8 (5) | O2—Cd1—N2—C13 | 40.3 (3) |
C4'—C5'—C8—C5 | −16 (4) | N1—Cd1—N2—C13 | 109.9 (4) |
C6'—C5'—C8—C5 | 177 (5) | N4—C23—N3—C24 | 0.0 (6) |
C4—C5—C8—N1 | −68.9 (7) | N4—C23—N3—Cd1 | −173.1 (3) |
C6—C5—C8—N1 | 100.2 (5) | C25—C24—N3—C23 | −0.8 (6) |
C4—C5—C8—C5' | −173 (5) | C25—C24—N3—Cd1 | 172.1 (4) |
C6—C5—C8—C5' | −4 (4) | N5—Cd1—N3—C23 | −90.8 (4) |
N1—C9—C10—O3 | 154.8 (5) | O4—Cd1—N3—C23 | 176.4 (4) |
N1—C9—C10—O2 | −26.5 (7) | O2—Cd1—N3—C23 | 6.9 (4) |
N1—C11—C12—N2 | −61.1 (5) | N1—Cd1—N3—C23 | 42.2 (6) |
N2—C13—C14—C15 | 95.5 (6) | N2—Cd1—N3—C23 | 103.9 (4) |
N2—C13—C14—C19 | −86.6 (7) | N5—Cd1—N3—C24 | 97.7 (4) |
C19—C14—C15—C16 | 2.2 (8) | O4—Cd1—N3—C24 | 4.9 (4) |
C13—C14—C15—C16 | −179.8 (5) | O2—Cd1—N3—C24 | −164.6 (4) |
C14—C15—C16—C17 | 0.0 (8) | N1—Cd1—N3—C24 | −129.3 (5) |
C15—C16—C17—C18 | −2.3 (10) | N2—Cd1—N3—C24 | −67.6 (4) |
C15—C16—C17—O6 | −180.0 (6) | N3—C23—N4—C25 | 0.7 (6) |
C16—C17—C18—C19 | 2.2 (12) | C24—C25—N4—C23 | −1.2 (6) |
O6—C17—C18—C19 | 180.0 (7) | N6—C26—N5—C27 | 1.1 (6) |
C17—C18—C19—C14 | 0.3 (12) | N6—C26—N5—Cd1 | −176.4 (3) |
C15—C14—C19—C18 | −2.4 (10) | C28—C27—N5—C26 | −0.8 (6) |
C13—C14—C19—C18 | 179.5 (7) | C28—C27—N5—Cd1 | 176.6 (3) |
N2—C21—C22—O5 | 151.3 (6) | N3—Cd1—N5—C26 | −93.5 (4) |
N2—C21—C22—O4 | −32.2 (8) | O4—Cd1—N5—C26 | 7.0 (4) |
N3—C24—C25—N4 | 1.2 (6) | O2—Cd1—N5—C26 | 174.6 (4) |
N5—C27—C28—N6 | 0.3 (6) | N1—Cd1—N5—C26 | 102.3 (4) |
C10—C9—N1—C11 | −74.8 (5) | N2—Cd1—N5—C26 | 43.8 (7) |
C10—C9—N1—C8 | 157.6 (4) | N3—Cd1—N5—C27 | 89.7 (4) |
C10—C9—N1—Cd1 | 38.6 (5) | O4—Cd1—N5—C27 | −169.8 (4) |
C12—C11—N1—C9 | 156.1 (4) | O2—Cd1—N5—C27 | −2.2 (4) |
C12—C11—N1—C8 | −76.8 (5) | N1—Cd1—N5—C27 | −74.5 (4) |
C12—C11—N1—Cd1 | 42.9 (4) | N2—Cd1—N5—C27 | −133.1 (5) |
C5'—C8—N1—C9 | 67.8 (6) | N5—C26—N6—C28 | −1.0 (6) |
C5—C8—N1—C9 | 57.8 (7) | C27—C28—N6—C26 | 0.4 (6) |
C5'—C8—N1—C11 | −58.1 (7) | O3—C10—O2—Cd1 | 175.2 (5) |
C5—C8—N1—C11 | −68.1 (7) | C9—C10—O2—Cd1 | −3.4 (7) |
C5'—C8—N1—Cd1 | −175.6 (5) | N3—Cd1—O2—C10 | −174.2 (4) |
C5—C8—N1—Cd1 | 174.4 (5) | N5—Cd1—O2—C10 | −71.3 (4) |
N3—Cd1—N1—C9 | −67.2 (5) | O4—Cd1—O2—C10 | 50.7 (7) |
N5—Cd1—N1—C9 | 67.2 (3) | N1—Cd1—O2—C10 | 18.9 (4) |
O4—Cd1—N1—C9 | 158.0 (3) | N2—Cd1—O2—C10 | 92.2 (4) |
O2—Cd1—N1—C9 | −29.7 (3) | O5—C22—O4—Cd1 | 178.9 (6) |
N2—Cd1—N1—C9 | −131.8 (3) | C21—C22—O4—Cd1 | 2.7 (7) |
N3—Cd1—N1—C11 | 49.5 (5) | N3—Cd1—O4—C22 | −74.9 (4) |
N5—Cd1—N1—C11 | −176.1 (3) | N5—Cd1—O4—C22 | −177.9 (4) |
O4—Cd1—N1—C11 | −85.4 (3) | O2—Cd1—O4—C22 | 59.3 (7) |
O2—Cd1—N1—C11 | 86.9 (3) | N1—Cd1—O4—C22 | 89.5 (4) |
N2—Cd1—N1—C11 | −15.2 (3) | N2—Cd1—O4—C22 | 15.6 (4) |
N3—Cd1—N1—C8 | 171.7 (4) | C18—C17—O6—C20 | −178.8 (8) |
N5—Cd1—N1—C8 | −53.9 (3) | C16—C17—O6—C20 | −0.9 (11) |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···O3 | 0.85 | 1.91 | 2.756 (14) | 173 |
N6—H6A···O3i | 0.86 | 1.85 | 2.703 (6) | 172 |
C28—H28···O8ii | 0.93 | 2.67 | 3.58 (4) | 167 |
N4—H4A···O5ii | 0.86 | 1.87 | 2.724 (6) | 170 |
Symmetry codes: (i) x+1/2, −y+1/2, z; (ii) x−1/2, −y+1/2, z. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C22H26N2O6)(C3H4N2)2]·2H2O |
Mr | 699.04 |
Crystal system, space group | Orthorhombic, Pcab |
Temperature (K) | 292 |
a, b, c (Å) | 15.7646 (8), 16.3172 (8), 24.7351 (12) |
V (Å3) | 6362.7 (5) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 0.74 |
Crystal size (mm) | 0.30 × 0.25 × 0.07 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2001) |
Tmin, Tmax | 0.796, 0.949 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 63596, 6253, 3809 |
Rint | 0.088 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.059, 0.179, 1.03 |
No. of reflections | 6253 |
No. of parameters | 430 |
No. of restraints | 102 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.69, −0.78 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b), SHELXTL.
Cd1—N3 | 2.261 (4) | Cd1—O2 | 2.325 (4) |
Cd1—N5 | 2.276 (4) | Cd1—N1 | 2.415 (4) |
Cd1—O4 | 2.311 (4) | Cd1—N2 | 2.426 (4) |
N5—Cd1—O4 | 90.49 (13) | O4—Cd1—N2 | 72.21 (13) |
N5—Cd1—O2 | 97.39 (14) | O2—Cd1—N2 | 96.99 (14) |
N3—Cd1—N1 | 158.18 (13) |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···O3 | 0.85 | 1.91 | 2.756 (14) | 172.7 |
N6—H6A···O3i | 0.86 | 1.85 | 2.703 (6) | 172.3 |
C28—H28···O8ii | 0.93 | 2.67 | 3.58 (4) | 167.0 |
N4—H4A···O5ii | 0.86 | 1.87 | 2.724 (6) | 169.6 |
Symmetry codes: (i) x+1/2, −y+1/2, z; (ii) x−1/2, −y+1/2, z. |
Recently, we have reported the nickel and zinc complexes with the [N,N'-bis(4-methoxylbenzyl)ethane-1,2-diyldiimino] diacetate (Zhang, Weng & Xu, 2007; Zhang, Weng, Hu & Xu, 2007). In this paper, we continue reporting the structure of the Cd(II) complex, Cd(La)(Lb)2.2H2O(La=[N,N'-bis(4-methoxyl- benzyl)ethane-1,2-diyldiimino]diacetate, Lb=imidazole)(1). In (1), the cadmium atom is also in a slightly distorted octahedral coordination environment (Fig. 1), which is similar to the zinc complex without the longer bond lengths (Table 1), and there is a disorder in one of the 4-methoxylbenzyl groups. In the crystal structure, the hydrogen bonds (Table 2) consolidate the crystal packing into infinite one-dimensional chains (Fig 2).