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Acta Cryst. (2007). E63, m2045    [ doi:10.1107/S1600536807031200 ]

{[N,N'-Bis(4-methoxybenzyl)ethane-1,2-diyldiimino]diacetato}bis(1H-imidazole-[kappa]N3)cadmium(II) dihydrate

M. Zhang, S.-M. Lan, H.-L. Weng and X.-M. Xu

Abstract top

In the title complex, [Cd(C22H26N2O6)(C3H4N2)2]·2H2O, the Cd atom is in a distorted octahedral coordination environment. In the crystal structure, intermolecular hydrogen bonding links molecules into infinite one-dimensional chains. The atoms of one 4-methoxybenzyl group are disordered over two sites in approximately a 0.54:0.46 ratio.

Comment top

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).

Related literature top

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).

Experimental top

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).

Refinement top

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.

Computing details top

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.

Figures top
[Figure 1] Fig. 1. Molecular structure of (I) showing 30% probability displacement ellipsoids. Omit the water molecule for clear.
[Figure 2] Fig. 2. Part of the crystal structure of (1), showing the formation of a chain of rings along [100]. Dashed lines denote hydrogen bonds.
{[N,N'-Bis(4-methoxybenzyl)ethane-1,2-diyldiimino]diacetato}bis(1H- imidazole-kN3)cadmium(II) dihydrate top
Crystal data top
[Cd(C22H26N2O6)(C3H4N2)2]·2H2OF(000) = 2880
Mr = 699.04Dx = 1.459 Mg m−3
Orthorhombic, PcabMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2bc 2acCell parameters from 5642 reflections
a = 15.7646 (8) Åθ = 2.4–22.5°
b = 16.3172 (8) ŵ = 0.74 mm−1
c = 24.7351 (12) ÅT = 292 K
V = 6362.7 (5) Å3Plate, colorless
Z = 80.30 × 0.25 × 0.07 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		6253 independent reflections
Radiation source: fine-focus sealed tube3809 reflections with I > 2σ(I)
graphiteRint = 0.088
φ and ω scansθmax = 26.0°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)		h = −19→19
Tmin = 0.796, Tmax = 0.949k = −20→20
63596 measured reflectionsl = −30→30
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.059Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.179H-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 parametersΔρmax = 0.69 e Å−3
102 restraintsΔρmin = −0.78 e Å−3
Crystal data top
[Cd(C22H26N2O6)(C3H4N2)2]·2H2OV = 6362.7 (5) Å3
Mr = 699.04Z = 8
Orthorhombic, PcabMo Kα radiation
a = 15.7646 (8) ŵ = 0.74 mm−1
b = 16.3172 (8) ÅT = 292 K
c = 24.7351 (12) Å0.30 × 0.25 × 0.07 mm
Data collection top
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 = 0.949Rint = 0.088
63596 measured reflectionsθmax = 26.0°
Refinement top
R[F2 > 2σ(F2)] = 0.059H-atom parameters constrained
wR(F2) = 0.179Δρmax = 0.69 e Å−3
S = 1.03Δρmin = −0.78 e Å−3
6253 reflectionsAbsolute structure: ?
430 parametersFlack parameter: ?
102 restraintsRogers parameter: ?
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cd10.36406 (3)0.17511 (2)0.249249 (14)0.06385 (18)
C10.606 (2)−0.2625 (18)0.4734 (13)0.139 (10)0.456 (14)
H1A0.5778−0.29720.44760.209*0.456 (14)
H1B0.6125−0.29160.50680.209*0.456 (14)
H1C0.6601−0.24660.45980.209*0.456 (14)
O10.5578 (12)−0.1948 (15)0.4820 (10)0.139 (7)0.456 (14)
C20.5431 (13)−0.1292 (13)0.4356 (15)0.118 (11)0.456 (14)
C30.5056 (7)−0.0690 (8)0.4603 (4)0.171 (13)0.456 (14)
H30.5014−0.05980.49730.205*0.456 (14)
C40.4733 (7)−0.0219 (8)0.4186 (4)0.113 (8)0.456 (14)
H40.43120.01470.42900.136*0.456 (14)
C50.4929 (7)−0.0197 (8)0.3641 (4)0.087 (10)0.456 (14)
C60.5234 (7)−0.0970 (8)0.3513 (4)0.080 (5)0.456 (14)
H60.5290−0.10930.31480.096*0.456 (14)
C70.5466 (7)−0.1580 (8)0.3877 (4)0.081 (8)0.456 (14)
H70.5714−0.20710.37710.097*0.456 (14)
C1'0.595 (3)−0.217 (2)0.4931 (16)0.194 (17)0.544 (14)
H1'10.6369−0.17570.49990.291*0.544 (14)
H1'20.6137−0.26850.50700.291*0.544 (14)
H1'30.5426−0.20160.51060.291*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)
H3'0.5149−0.08010.47600.137*0.544 (14)
C4'0.5029 (5)−0.0118 (5)0.4101 (3)0.082 (5)0.544 (14)
H4'0.49650.03940.42620.099*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)
H6'0.5296−0.09210.28950.075*0.544 (14)
C7'0.5553 (5)−0.1593 (5)0.3564 (3)0.078 (4)0.544 (14)
H7'0.5743−0.20660.33930.094*0.544 (14)
C80.4723 (3)0.0483 (3)0.3220 (2)0.0719 (14)
H8A0.49290.10020.33600.086*
H8B0.50370.03670.28910.086*
C90.3283 (3)0.0752 (3)0.3551 (2)0.0689 (13)
H9A0.35960.11010.37970.083*
H9B0.31610.02420.37370.083*
C100.2442 (3)0.1174 (4)0.3402 (2)0.0758 (15)
C110.3464 (3)−0.0126 (3)0.2774 (2)0.0692 (13)
H11A0.2849−0.01130.27950.083*
H11B0.3655−0.06300.29430.083*
C120.3724 (3)−0.0130 (3)0.2191 (2)0.0708 (14)
H12A0.4337−0.01590.21710.085*
H12B0.3497−0.06170.20200.085*
C130.2532 (3)0.0536 (3)0.1719 (2)0.0711 (14)
H13A0.23670.10620.15700.085*
H13B0.21890.04460.20390.085*
C140.2313 (3)−0.0116 (4)0.1313 (2)0.0719 (14)
C150.2008 (3)−0.0873 (4)0.1453 (3)0.0824 (16)
H150.1925−0.10010.18160.099*
C160.1814 (4)−0.1468 (4)0.1046 (3)0.0864 (17)
H160.1607−0.19830.11380.104*
C170.1943 (4)−0.1258 (5)0.0520 (3)0.0930 (18)
C180.2213 (5)−0.0515 (5)0.0374 (3)0.119 (3)
H180.2278−0.03810.00110.143*
C190.2390 (4)0.0038 (4)0.0765 (2)0.100 (2)
H190.25760.05540.06590.120*
C200.1472 (6)−0.2579 (6)0.0218 (4)0.158 (4)
H20A0.1911−0.29750.01530.236*
H20B0.0989−0.2702−0.00030.236*
H20C0.1311−0.25960.05930.236*
C210.4002 (4)0.0757 (3)0.1429 (2)0.0767 (15)
H21A0.37310.11420.11860.092*
H21B0.40980.02510.12320.092*
C220.4853 (3)0.1106 (4)0.1615 (2)0.0784 (15)
C230.2216 (3)0.2934 (3)0.1992 (2)0.0703 (13)
H230.18780.28480.22950.084*
C240.3236 (3)0.2919 (3)0.1431 (2)0.0717 (14)
H240.37610.28170.12740.086*
C250.2623 (4)0.3350 (4)0.1210 (2)0.0786 (16)
H250.26330.35950.08710.094*
C260.5097 (3)0.2857 (3)0.3045 (2)0.0728 (14)
H260.54520.27430.27540.087*
C270.4026 (3)0.2913 (3)0.3560 (2)0.0693 (13)
H270.34830.28400.37000.083*
C280.4646 (4)0.3341 (3)0.3792 (2)0.0770 (15)
H280.46150.36180.41200.092*
N10.3811 (2)0.0579 (2)0.30784 (17)0.0612 (10)
N20.3434 (3)0.0594 (3)0.18910 (17)0.0651 (11)
N30.2983 (3)0.2641 (2)0.19315 (15)0.0650 (10)
N40.1983 (3)0.3369 (3)0.15648 (19)0.0759 (12)
H4A0.15070.36190.15230.091*
N50.4319 (3)0.2597 (2)0.30825 (16)0.0656 (10)
N60.5323 (3)0.3302 (3)0.34665 (19)0.0773 (13)
H6A0.58110.35240.35210.093*
O20.2394 (2)0.1595 (2)0.29840 (15)0.0792 (10)
O30.1857 (3)0.1072 (3)0.37274 (18)0.1179 (17)
O40.4891 (2)0.1547 (2)0.20236 (15)0.0778 (10)
O50.5458 (3)0.0944 (3)0.1314 (2)0.1219 (18)
O60.1771 (4)−0.1803 (4)0.0092 (2)0.1312 (19)
O70.1167 (7)0.0124 (8)0.4537 (5)0.337 (7)*
H7A0.14110.04320.43080.404*
H7B0.1498−0.02740.46050.404*
O80.990 (3)0.0651 (17)0.5068 (17)0.87 (3)*
H8C0.99980.11600.51081.042*
H8D0.96680.05860.47611.042*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0626 (3)0.0620 (3)0.0670 (3)−0.00006 (17)−0.00320 (17)−0.00432 (18)
C10.133 (16)0.17 (3)0.119 (19)0.078 (18)0.017 (14)0.032 (18)
O10.138 (13)0.158 (16)0.120 (16)0.060 (11)0.020 (10)0.050 (12)
C20.147 (19)0.050 (18)0.16 (2)−0.014 (12)−0.055 (16)−0.005 (15)
C30.24 (3)0.20 (2)0.076 (14)0.11 (2)−0.052 (15)−0.047 (13)
C40.066 (10)0.16 (2)0.116 (15)−0.002 (10)−0.023 (9)0.012 (14)
C50.057 (14)0.050 (13)0.16 (2)0.003 (11)0.001 (14)−0.019 (16)
C60.080 (10)0.105 (13)0.055 (10)−0.005 (9)0.011 (8)−0.008 (9)
C70.058 (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)
C80.057 (3)0.072 (3)0.087 (4)0.002 (3)−0.008 (3)−0.009 (3)
C90.064 (3)0.072 (3)0.071 (3)0.004 (3)0.000 (3)0.004 (3)
C100.061 (3)0.084 (4)0.082 (4)0.012 (3)0.004 (3)0.004 (3)
C110.059 (3)0.062 (3)0.087 (4)−0.007 (2)−0.014 (3)0.004 (3)
C120.060 (3)0.064 (3)0.088 (4)0.002 (3)−0.008 (3)−0.017 (3)
C130.056 (3)0.082 (3)0.075 (3)0.003 (3)−0.007 (3)−0.004 (3)
C140.051 (3)0.084 (4)0.080 (4)−0.002 (3)−0.009 (2)−0.010 (3)
C150.051 (3)0.109 (5)0.087 (4)−0.007 (3)−0.006 (3)−0.007 (4)
C160.065 (4)0.081 (4)0.113 (5)−0.011 (3)−0.011 (3)−0.003 (4)
C170.084 (4)0.123 (6)0.072 (4)0.000 (4)0.000 (3)−0.013 (4)
C180.144 (7)0.137 (6)0.077 (4)−0.040 (6)0.005 (4)−0.013 (5)
C190.111 (5)0.113 (5)0.075 (4)−0.026 (4)−0.015 (4)−0.008 (4)
C200.183 (9)0.128 (7)0.162 (9)−0.060 (7)−0.014 (7)−0.027 (7)
C210.075 (4)0.083 (4)0.072 (3)−0.003 (3)0.001 (3)−0.011 (3)
C220.063 (3)0.085 (4)0.087 (4)−0.006 (3)0.009 (3)−0.017 (3)
C230.067 (3)0.071 (3)0.073 (3)−0.005 (3)0.012 (3)0.006 (3)
C240.062 (3)0.085 (4)0.069 (3)−0.010 (3)0.009 (3)−0.001 (3)
C250.071 (4)0.098 (4)0.066 (3)−0.009 (3)0.000 (3)0.017 (3)
C260.069 (3)0.076 (4)0.073 (3)−0.003 (3)0.010 (3)−0.005 (3)
C270.067 (3)0.068 (3)0.073 (3)0.003 (3)0.005 (3)−0.003 (3)
C280.087 (4)0.079 (4)0.065 (3)0.004 (3)−0.003 (3)−0.006 (3)
N10.049 (2)0.064 (2)0.070 (3)−0.0001 (18)−0.0074 (19)−0.005 (2)
N20.054 (2)0.070 (3)0.071 (3)−0.002 (2)−0.003 (2)−0.007 (2)
N30.061 (2)0.067 (3)0.067 (2)−0.003 (2)0.002 (2)0.000 (2)
N40.059 (3)0.079 (3)0.090 (3)0.000 (2)−0.002 (2)0.014 (2)
N50.062 (2)0.064 (3)0.071 (3)0.000 (2)−0.002 (2)−0.001 (2)
N60.068 (3)0.083 (3)0.081 (3)−0.014 (2)−0.008 (3)−0.011 (2)
O20.066 (2)0.088 (3)0.083 (2)0.0163 (19)0.0032 (19)0.017 (2)
O30.082 (3)0.161 (4)0.111 (3)0.040 (3)0.032 (3)0.050 (3)
O40.068 (2)0.086 (3)0.080 (2)−0.0121 (19)0.0034 (19)−0.018 (2)
O50.074 (3)0.159 (4)0.133 (4)−0.027 (3)0.026 (3)−0.067 (3)
O60.152 (5)0.146 (5)0.096 (3)−0.027 (4)0.004 (3)−0.033 (3)
Geometric parameters (Å, °) top
Cd1—N32.261 (4)C11—H11A0.9700
Cd1—N52.276 (4)C11—H11B0.9700
Cd1—O42.311 (4)C12—N21.468 (7)
Cd1—O22.325 (4)C12—H12A0.9700
Cd1—N12.415 (4)C12—H12B0.9700
Cd1—N22.426 (4)C13—N21.487 (6)
C1—O11.35 (4)C13—C141.504 (7)
C1—H1A0.9600C13—H13A0.9700
C1—H1B0.9600C13—H13B0.9700
C1—H1C0.9600C14—C151.372 (8)
O1—C21.59 (4)C14—C191.383 (7)
C2—C71.28 (3)C15—C161.432 (8)
C2—C31.30 (3)C15—H150.9300
C3—C41.3829C16—C171.361 (8)
C3—H30.9300C16—H160.9300
C4—C51.3841C17—C181.334 (9)
C4—H40.9300C17—O61.409 (7)
C4—H4'1.0807C18—C191.351 (8)
C5—C61.3860C18—H180.9300
C5—C81.556 (13)C19—H190.9300
C6—C71.3910C20—O61.386 (9)
C6—H60.9300C20—H20A0.9600
C7—H70.9300C20—H20B0.9600
C1'—O1'1.40 (5)C20—H20C0.9600
C1'—H1'10.9600C21—N21.475 (7)
C1'—H1'20.9600C21—C221.528 (8)
C1'—H1'30.9600C21—H21A0.9700
O1'—C2'1.32 (2)C21—H21B0.9700
C2'—C3'1.37 (2)C22—O51.239 (6)
C2'—C7'1.54 (3)C22—O41.241 (6)
C3'—C4'1.3893C23—N31.309 (6)
C3'—H3'0.9300C23—N41.324 (6)
C4'—C5'1.3786C23—H230.9300
C4'—H41.2981C24—C251.314 (7)
C4'—H4'0.9300C24—N31.376 (6)
C5'—C6'1.3787C24—H240.9300
C5'—C81.509 (9)C25—N41.337 (7)
C6'—C7'1.3835C25—H250.9300
C6'—H60.4131C26—N51.301 (6)
C6'—H6'0.9300C26—N61.320 (6)
C7'—H70.9680C26—H260.9300
C7'—H7'0.9300C27—C281.332 (7)
C8—N11.489 (6)C27—N51.370 (6)
C8—H8A0.9700C27—H270.9300
C8—H8B0.9700C28—N61.339 (7)
C9—N11.462 (7)C28—H280.9300
C9—C101.538 (7)N4—H4A0.8600
C9—H9A0.9700N6—H6A0.8600
C9—H9B0.9700O7—H7A0.8501
C10—O31.235 (6)O7—H7B0.8500
C10—O21.244 (6)O8—H8C0.8501
C11—N11.479 (6)O8—H8D0.8500
C11—C121.499 (8)
N3—Cd1—N5102.70 (14)N1—C11—H11A109.0
N3—Cd1—O4100.12 (14)C12—C11—H11A109.0
N5—Cd1—O490.49 (13)N1—C11—H11B109.0
N3—Cd1—O290.21 (13)C12—C11—H11B109.0
N5—Cd1—O297.39 (14)H11A—C11—H11B107.8
O4—Cd1—O2165.35 (14)N2—C12—C11113.5 (4)
N3—Cd1—N1158.18 (13)N2—C12—H12A108.9
N5—Cd1—N192.47 (14)C11—C12—H12A108.9
O4—Cd1—N195.28 (13)N2—C12—H12B108.9
O2—Cd1—N172.15 (13)C11—C12—H12B108.9
N3—Cd1—N293.55 (14)H12A—C12—H12B107.7
N5—Cd1—N2158.19 (14)N2—C13—C14117.0 (4)
O4—Cd1—N272.21 (13)N2—C13—H13A108.0
O2—Cd1—N296.99 (14)C14—C13—H13A108.0
N1—Cd1—N276.49 (16)N2—C13—H13B108.0
C1—O1—C2121 (2)C14—C13—H13B108.0
C7—C2—C3137 (3)H13A—C13—H13B107.3
C7—C2—O1114.6 (19)C15—C14—C19116.2 (5)
C3—C2—O1104 (2)C15—C14—C13123.3 (5)
C2—C3—C4103.8 (17)C19—C14—C13120.5 (6)
C2—C3—H3128.1C14—C15—C16120.5 (6)
C4—C3—H3128.1C14—C15—H15119.8
C3—C4—C5131.2C16—C15—H15119.8
C3—C4—H4114.4C17—C16—C15118.0 (6)
C5—C4—H4114.4C17—C16—H16121.0
C3—C4—H4'105.2C15—C16—H16121.0
C5—C4—H4'94.0C18—C17—C16122.4 (6)
H4—C4—H4'66.3C18—C17—O6115.6 (6)
C4—C5—C6106.0C16—C17—O6122.0 (7)
C4—C5—C8128.6 (4)C17—C18—C19118.6 (7)
C6—C5—C8124.7 (5)C17—C18—H18120.7
C5—C6—C7126.5C19—C18—H18120.7
C5—C6—H6116.8C18—C19—C14124.2 (7)
C7—C6—H6116.8C18—C19—H19117.9
C5—C6—H6'101.6C14—C19—H19117.9
C7—C6—H6'131.8O6—C20—H20A109.5
C2—C7—C6109.1 (14)O6—C20—H20B109.5
C2—C7—H7126.7H20A—C20—H20B109.5
C6—C7—H7123.0O6—C20—H20C109.5
C2—C7—H7'161.4H20A—C20—H20C109.5
C6—C7—H7'86.5H20B—C20—H20C109.5
O1'—C1'—H1'1109.5N2—C21—C22111.5 (5)
O1'—C1'—H1'2109.5N2—C21—H21A109.3
H1'1—C1'—H1'2109.5C22—C21—H21A109.3
O1'—C1'—H1'3109.5N2—C21—H21B109.3
H1'1—C1'—H1'3109.5C22—C21—H21B109.3
H1'2—C1'—H1'3109.5H21A—C21—H21B108.0
C2'—O1'—C1'112 (2)O5—C22—O4125.1 (5)
O1'—C2'—C3'135 (2)O5—C22—C21114.6 (5)
O1'—C2'—C7'106.6 (17)O4—C22—C21120.2 (5)
C3'—C2'—C7'114.2 (17)N3—C23—N4111.2 (5)
O1'—C2'—H768.9N3—C23—H23124.4
C3'—C2'—H7151.5N4—C23—H23124.4
C2'—C3'—C4'127.7 (13)C25—C24—N3109.7 (5)
C2'—C3'—H3'116.2C25—C24—H24125.1
C4'—C3'—H3'116.2N3—C24—H24125.1
C5'—C4'—C3'112.0C24—C25—N4107.2 (5)
C5'—C4'—H4110.7C24—C25—H25126.4
C3'—C4'—H4105.1N4—C25—H25126.4
C5'—C4'—H4'124.0N5—C26—N6112.2 (5)
C3'—C4'—H4'124.0N5—C26—H26123.9
H4—C4'—H4'56.8N6—C26—H26123.9
C4'—C5'—C6'127.1C28—C27—N5108.7 (5)
C4'—C5'—C8115.0 (4)C28—C27—H27125.6
C6'—C5'—C8116.5 (4)N5—C27—H27125.6
C5'—C6'—C7'118.0C27—C28—N6107.5 (5)
C5'—C6'—H6157.3C27—C28—H28126.2
C7'—C6'—H680.5N6—C28—H28126.2
C5'—C6'—H6'121.0C9—N1—C11110.2 (4)
C7'—C6'—H6'121.0C9—N1—C8112.5 (4)
C6'—C7'—C2'117.9 (7)C11—N1—C8113.3 (4)
C2'—C7'—H6133.8C9—N1—Cd1105.3 (3)
C6'—C7'—H7176.9C11—N1—Cd1105.6 (3)
C2'—C7'—H761.2C8—N1—Cd1109.4 (3)
H6—C7'—H7162.4C12—N2—C21110.3 (4)
C6'—C7'—H7'121.4C12—N2—C13113.1 (4)
C2'—C7'—H7'120.1C21—N2—C13111.7 (4)
H6—C7'—H7'104.5C12—N2—Cd1105.9 (3)
N1—C8—C5'117.6 (5)C21—N2—Cd1104.7 (3)
N1—C8—C5115.7 (6)C13—N2—Cd1110.7 (3)
N1—C8—H8A108.4C23—N3—C24104.5 (4)
C5'—C8—H8A114.5C23—N3—Cd1126.1 (3)
C5—C8—H8A108.4C24—N3—Cd1129.1 (4)
N1—C8—H8B108.4C23—N4—C25107.5 (5)
C5'—C8—H8B99.6C23—N4—H4A126.2
C5—C8—H8B108.4C25—N4—H4A126.2
H8A—C8—H8B107.4C26—N5—C27104.9 (4)
N1—C9—C10112.8 (4)C26—N5—Cd1126.5 (4)
N1—C9—H9A109.0C27—N5—Cd1128.5 (3)
C10—C9—H9A109.0C26—N6—C28106.6 (5)
N1—C9—H9B109.0C26—N6—H6A126.7
C10—C9—H9B109.0C28—N6—H6A126.7
H9A—C9—H9B107.8C10—O2—Cd1116.3 (3)
O3—C10—O2124.8 (5)C22—O4—Cd1116.8 (3)
O3—C10—C9115.3 (5)C20—O6—C17118.2 (6)
O2—C10—C9119.9 (5)H7A—O7—H7B107.7
N1—C11—C12113.0 (4)H8C—O8—H8D107.7
C1—O1—C2—C728 (3)O4—Cd1—N1—C836.9 (3)
C1—O1—C2—C3−171 (2)O2—Cd1—N1—C8−150.8 (3)
C7—C2—C3—C4−11.3 (16)N2—Cd1—N1—C8107.1 (3)
O1—C2—C3—C4−165.1 (11)C11—C12—N2—C21153.7 (4)
C2—C3—C4—C5−17.6 (5)C11—C12—N2—C13−80.3 (5)
C3—C4—C5—C626.7C11—C12—N2—Cd141.0 (4)
C3—C4—C5—C8−162.5 (6)C22—C21—N2—C12−73.1 (5)
C4—C5—C6—C7−12.3C22—C21—N2—C13160.2 (4)
C8—C5—C6—C7176.5 (6)C22—C21—N2—Cd140.4 (5)
C3—C2—C7—C621.6 (16)C14—C13—N2—C12−65.7 (6)
O1—C2—C7—C6173.4 (11)C14—C13—N2—C2159.5 (6)
C5—C6—C7—C2−6.1 (6)C14—C13—N2—Cd1175.7 (4)
C1'—O1'—C2'—C3'9(3)N3—Cd1—N2—C12−173.3 (3)
C1'—O1'—C2'—C7'162 (2)N5—Cd1—N2—C1248.3 (6)
O1'—C2'—C3'—C4'157.1 (17)O4—Cd1—N2—C1287.2 (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'−18.9N3—Cd1—N2—C2170.1 (3)
C3'—C4'—C5'—C8175.2 (4)N5—Cd1—N2—C21−68.3 (5)
C4'—C5'—C6'—C7'11.0O4—Cd1—N2—C21−29.4 (3)
C8—C5'—C6'—C7'176.7 (4)O2—Cd1—N2—C21160.8 (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—C13171.2 (4)
C4'—C5'—C8—N1−95.8 (4)O4—Cd1—N2—C13−149.9 (4)
C6'—C5'—C8—N196.8 (5)O2—Cd1—N2—C1340.3 (3)
C4'—C5'—C8—C5−16 (4)N1—Cd1—N2—C13109.9 (4)
C6'—C5'—C8—C5177 (5)N4—C23—N3—C240.0 (6)
C4—C5—C8—N1−68.9 (7)N4—C23—N3—Cd1−173.1 (3)
C6—C5—C8—N1100.2 (5)C25—C24—N3—C23−0.8 (6)
C4—C5—C8—C5'−173 (5)C25—C24—N3—Cd1172.1 (4)
C6—C5—C8—C5'−4(4)N5—Cd1—N3—C23−90.8 (4)
N1—C9—C10—O3154.8 (5)O4—Cd1—N3—C23176.4 (4)
N1—C9—C10—O2−26.5 (7)O2—Cd1—N3—C236.9 (4)
N1—C11—C12—N2−61.1 (5)N1—Cd1—N3—C2342.2 (6)
N2—C13—C14—C1595.5 (6)N2—Cd1—N3—C23103.9 (4)
N2—C13—C14—C19−86.6 (7)N5—Cd1—N3—C2497.7 (4)
C19—C14—C15—C162.2 (8)O4—Cd1—N3—C244.9 (4)
C13—C14—C15—C16−179.8 (5)O2—Cd1—N3—C24−164.6 (4)
C14—C15—C16—C170.0 (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—C250.7 (6)
C16—C17—C18—C192.2 (12)C24—C25—N4—C23−1.2 (6)
O6—C17—C18—C19180.0 (7)N6—C26—N5—C271.1 (6)
C17—C18—C19—C140.3 (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—C18179.5 (7)C28—C27—N5—Cd1176.6 (3)
N2—C21—C22—O5151.3 (6)N3—Cd1—N5—C26−93.5 (4)
N2—C21—C22—O4−32.2 (8)O4—Cd1—N5—C267.0 (4)
N3—C24—C25—N41.2 (6)O2—Cd1—N5—C26174.6 (4)
N5—C27—C28—N60.3 (6)N1—Cd1—N5—C26102.3 (4)
C10—C9—N1—C11−74.8 (5)N2—Cd1—N5—C2643.8 (7)
C10—C9—N1—C8157.6 (4)N3—Cd1—N5—C2789.7 (4)
C10—C9—N1—Cd138.6 (5)O4—Cd1—N5—C27−169.8 (4)
C12—C11—N1—C9156.1 (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—Cd142.9 (4)N2—Cd1—N5—C27−133.1 (5)
C5'—C8—N1—C967.8 (6)N5—C26—N6—C28−1.0 (6)
C5—C8—N1—C957.8 (7)C27—C28—N6—C260.4 (6)
C5'—C8—N1—C11−58.1 (7)O3—C10—O2—Cd1175.2 (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—Cd1174.4 (5)N5—Cd1—O2—C10−71.3 (4)
N3—Cd1—N1—C9−67.2 (5)O4—Cd1—O2—C1050.7 (7)
N5—Cd1—N1—C967.2 (3)N1—Cd1—O2—C1018.9 (4)
O4—Cd1—N1—C9158.0 (3)N2—Cd1—O2—C1092.2 (4)
O2—Cd1—N1—C9−29.7 (3)O5—C22—O4—Cd1178.9 (6)
N2—Cd1—N1—C9−131.8 (3)C21—C22—O4—Cd12.7 (7)
N3—Cd1—N1—C1149.5 (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—C2259.3 (7)
O2—Cd1—N1—C1186.9 (3)N1—Cd1—O4—C2289.5 (4)
N2—Cd1—N1—C11−15.2 (3)N2—Cd1—O4—C2215.6 (4)
N3—Cd1—N1—C8171.7 (4)C18—C17—O6—C20−178.8 (8)
N5—Cd1—N1—C8−53.9 (3)C16—C17—O6—C20−0.9 (11)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O30.851.912.756 (14)173
N6—H6A···O3i0.861.852.703 (6)172
C28—H28···O8ii0.932.673.58 (4)167
N4—H4A···O5ii0.861.872.724 (6)170
Symmetry codes: (i) x+1/2, −y+1/2, z; (ii) x−1/2, −y+1/2, z.
Table 1
Selected geometric parameters (Å, °) top
Cd1—N32.261 (4)Cd1—O22.325 (4)
Cd1—N52.276 (4)Cd1—N12.415 (4)
Cd1—O42.311 (4)Cd1—N22.426 (4)
N5—Cd1—O490.49 (13)O4—Cd1—N272.21 (13)
N5—Cd1—O297.39 (14)O2—Cd1—N296.99 (14)
N3—Cd1—N1158.18 (13)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O30.851.912.756 (14)173
N6—H6A···O3i0.861.852.703 (6)172
C28—H28···O8ii0.932.673.58 (4)167
N4—H4A···O5ii0.861.872.724 (6)170
Symmetry codes: (i) x+1/2, −y+1/2, z; (ii) x−1/2, −y+1/2, z.
references
References top

Bruker (2000). SMART, SAINT-Plus and SADABS (Version 6.10). Bruker AXS Inc., Madison, Wisconsin, USA. SAINT or SAINT-Plus?

Sheldrick, G. M. (1997a). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Sheldrick, G. M. (1997b). SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (2001). SADABS. Version 2.10. Bruker AXS Inc., Madison, Wisconsin, USA.

Zhang, M., Weng, H.-L., Hu, B. & Xu, X.-M. (2007). Acta Cryst. E63, m1797–?.

Zhang, M., Weng, H.-L. & Xu, X.-M. (2007). Acta Cryst. E63, m1465–m1466.