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Acta Crystallogr Sect E Struct Rep Online. 2008 February 1; 64(Pt 2): m322.
Published online 2008 January 9. doi:  10.1107/S1600536807056541
PMCID: PMC2960202

(5,6:19,20-Dibenzo-1,4,11,14-tetra­oxa-8,17-diaza­cyclo­eicosane-κ4 N 8,O 11,O 14,N 17)dinitrato-κ4 O,O′-cadmium(II)

Abstract

In the title compound, [Cd(NO3)2(C22H30N2O4)], the CdII atom is eight-coordinated by two amine N atoms and two O atoms from the 5,6:19,20-dibenzo-1,4,11,14-tetra­oxa-8,17-diaza­cyclo­eicosane ligand and four O atoms from two nitrate groups. The coordination geometry about Cd is antiprismatic. One nitro O atom is disordered equally over two positions.

Related literature

For related literature, see: López-Deber et al. (2005 [triangle]); Vicente et al. (2003 [triangle]); Meyerstein (1990 [triangle]); Popović et al. (2006 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m322-scheme1.jpg

Experimental

Crystal data

  • [Cd(NO3)2(C22H30N2O4)]
  • M r = 622.90
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m322-efi1.jpg
  • a = 13.167 (3) Å
  • b = 7.6750 (15) Å
  • c = 25.227 (5) Å
  • β = 92.568 (4)°
  • V = 2546.8 (9) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.92 mm−1
  • T = 293 (2) K
  • 0.22 × 0.21 × 0.19 mm

Data collection

  • Bruker APEX CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.82, T max = 0.84
  • 12190 measured reflections
  • 4558 independent reflections
  • 3767 reflections with I > 2σ(I)
  • R int = 0.056

Refinement

  • R[F 2 > 2σ(F 2)] = 0.041
  • wR(F 2) = 0.105
  • S = 1.04
  • 4558 reflections
  • 349 parameters
  • 1 restraint
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 1.00 e Å−3
  • Δρmin = −1.00 e Å−3

Data collection: SMART (Bruker, 1997 [triangle]); cell refinement: SAINT (Bruker, 1999 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL-Plus (Sheldrick, 1990 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807056541/cs2056sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807056541/cs2056Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We thank the National Natural Science Foundation of China (No. 20471014), the Program for New Century Excellent Talents in Chinese Universities (NCET-05-0320), the Fok Ying Tung Education Foundation, and the Analysis and Testing Foundation of Northeast Normal University for support.

supplementary crystallographic information

Comment

In the last few decades, the modification of the macrocycles to control and tune the properties of coordinated metal atoms has been the subject of much interest (Meyerstein, 1990; Vicente et al., 2003). We are involved in studies of oxaaza-macrocycles and their metal coordination compounds. In this paper, we report the preparation and crystal structure of the title macrocyclic complex of CdII.

In the structure of the title compound, CdII is eight-coordinated by two N atoms and two O atoms from ligand L and four O atoms from two nitrate groups. The title compound displays an antiprismatic geometry (Fig. 1). The bond distances and angles around the Cd atom are nomal (Popović et al., 2006).

Experimental

Ligand L was synthesized according to the reported method (López-Deber et al., 2005). A solution of Cd(NO3)2.4H2O (0.03 g, 0.10 mmol) in 5 ml e thanol was added dropwise to a solution of H2L (0.039 g, 0.10 mmol) in 6 ml e thanol. After stirring for 30 min, the mixture was filtered. Colorless crystals were obtained by evaporating the filtrate at room temperature (yield 50%).

Refinement

The C-bound H atoms were positioned geometrically and refined as riding atoms, with C—H distances of 0.93–0.97 Å and Uiso(H) = 1.2Ueq(C) for aromatic and methylene H atoms. The disordered nitrate group was refined using O atom split over two sites, with a total occupancy of 1.

Figures

Fig. 1.
A view of the molecule of I. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. Only one disorder site is shown for a nitrate.

Crystal data

[Cd(NO3)2(C22H30N2O4)]F000 = 1272
Mr = 622.90Dx = 1.625 Mg m3
Monoclinic, P21/cMo Kα radiation λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 3767 reflections
a = 13.167 (3) Åθ = 1.6–25.2º
b = 7.6750 (15) ŵ = 0.92 mm1
c = 25.227 (5) ÅT = 293 (2) K
β = 92.568 (4)ºBlock, colourless
V = 2546.8 (9) Å30.22 × 0.21 × 0.19 mm
Z = 4

Data collection

Bruker APEX CCD area-detector diffractometer4558 independent reflections
Radiation source: fine-focus sealed tube3767 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.056
T = 293(2) Kθmax = 25.2º
ω scansθmin = 1.6º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −15→14
Tmin = 0.82, Tmax = 0.84k = −9→8
12190 measured reflectionsl = −30→23

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.041H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.105  w = 1/[σ2(Fo2) + (0.0554P)2 + 0.8726P] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
4558 reflectionsΔρmax = 1.00 e Å3
349 parametersΔρmin = −1.00 e Å3
1 restraintExtinction correction: none
Primary atom site location: structure-invariant direct methods

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Cd10.237559 (19)0.06536 (3)0.068001 (9)0.03453 (12)
C10.3037 (3)0.2975 (5)0.26599 (15)0.0463 (9)
C20.3327 (4)0.3662 (6)0.31505 (16)0.0567 (11)
H20.28980.44180.33230.068*
C30.4250 (3)0.3218 (6)0.33784 (16)0.0556 (11)
H30.44480.36690.37090.067*
C40.4888 (3)0.2114 (6)0.31257 (17)0.0566 (11)
H40.55220.18390.32810.068*
C50.4585 (3)0.1415 (5)0.26411 (16)0.0501 (10)
H50.50200.06650.24710.060*
C60.3642 (3)0.1809 (5)0.24025 (14)0.0422 (9)
C70.1505 (5)0.4558 (8)0.2560 (3)0.110 (3)
H7A0.18730.56510.25440.132*
H7B0.13730.43500.29300.132*
C80.0537 (3)0.4785 (6)0.22754 (19)0.0597 (12)
H8A0.00220.50320.25280.072*
H8B0.05790.57850.20420.072*
C9−0.0699 (3)0.3258 (5)0.17268 (16)0.0460 (9)
C10−0.1521 (3)0.4239 (5)0.18653 (18)0.0552 (11)
H10−0.14540.50670.21340.066*
C11−0.2452 (3)0.3972 (6)0.15981 (19)0.0587 (11)
H11−0.30150.46110.16950.070*
C12−0.2557 (3)0.2788 (6)0.11950 (17)0.0550 (10)
H12−0.31810.26420.10140.066*
C13−0.1727 (3)0.1810 (5)0.10590 (16)0.0479 (9)
H13−0.17980.09940.07870.057*
C14−0.0788 (3)0.2032 (5)0.13236 (14)0.0414 (8)
C150.3261 (3)0.0939 (5)0.18976 (15)0.0454 (9)
H15A0.37320.00170.18140.054*
H15B0.26120.03970.19600.054*
C160.0130 (3)0.1004 (4)0.11704 (16)0.0412 (8)
H16A0.05210.06780.14900.049*
H16B−0.0097−0.00590.09940.049*
C170.4099 (3)0.2851 (5)0.12706 (16)0.0478 (9)
H17A0.45570.19270.11730.057*
H17B0.44150.34820.15670.057*
C180.3922 (4)0.4067 (5)0.08089 (18)0.0577 (11)
H18A0.35280.50680.09140.069*
H18B0.45650.44760.06830.069*
C190.3169 (4)0.4064 (5)−0.00699 (17)0.0543 (11)
H19A0.37950.4405−0.02300.065*
H19B0.27820.51050.00030.065*
C200.2563 (3)0.2872 (6)−0.04333 (15)0.0541 (10)
H20A0.22930.3534−0.07350.065*
H20B0.30080.1979−0.05650.065*
C210.0930 (3)0.3238 (5)−0.00682 (16)0.0474 (9)
H21A0.05500.3526−0.03950.057*
H21B0.12020.43080.00860.057*
C220.0255 (3)0.2383 (5)0.03056 (15)0.0445 (9)
H22A−0.03140.31450.03700.053*
H22B−0.00120.13160.01480.053*
N10.3131 (2)0.2088 (4)0.14301 (11)0.0380 (7)
N20.0799 (2)0.1973 (4)0.08151 (12)0.0362 (7)
N30.1614 (3)−0.2792 (4)0.09950 (14)0.0510 (8)
N40.3934 (3)−0.1361 (4)0.02528 (15)0.0504 (8)
O10.2109 (2)0.3313 (4)0.24031 (13)0.0725 (10)
O20.0240 (2)0.3344 (4)0.19770 (14)0.0711 (10)
O30.3384 (2)0.3117 (3)0.04042 (10)0.0510 (7)
O40.1745 (2)0.2061 (3)−0.01765 (9)0.0444 (6)
O50.3898 (3)−0.1102 (5)0.07408 (14)0.0717 (9)
O60.3226 (3)−0.0730 (4)−0.00288 (13)0.0649 (9)
O70.4605 (3)−0.2216 (5)0.00709 (18)0.0926 (12)
O80.1473 (3)−0.2092 (4)0.05524 (13)0.0673 (8)
O90.1617 (10)−0.439 (3)0.1075 (11)0.067 (4)0.50
O100.1959 (3)−0.1895 (4)0.13589 (14)0.0847 (11)
O110.1198 (10)−0.424 (3)0.1043 (11)0.075 (4)0.50
H1N0.272 (4)0.298 (7)0.150 (2)0.090*
H2N0.098 (4)0.287 (8)0.096 (2)0.090*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cd10.04017 (18)0.02992 (17)0.03375 (17)0.00307 (10)0.00432 (12)−0.00144 (9)
C10.049 (2)0.047 (2)0.043 (2)−0.0025 (18)0.0002 (18)−0.0047 (17)
C20.070 (3)0.055 (2)0.045 (2)−0.006 (2)0.001 (2)−0.0145 (19)
C30.067 (3)0.062 (3)0.037 (2)−0.019 (2)−0.004 (2)−0.0040 (19)
C40.061 (3)0.052 (2)0.055 (2)−0.013 (2)−0.015 (2)0.011 (2)
C50.056 (2)0.043 (2)0.051 (2)0.0012 (19)0.000 (2)0.0005 (17)
C60.054 (2)0.0334 (19)0.0387 (19)−0.0028 (17)−0.0029 (18)−0.0004 (15)
C70.088 (4)0.077 (4)0.160 (6)0.035 (3)−0.051 (4)−0.068 (4)
C80.069 (3)0.045 (2)0.065 (3)0.012 (2)−0.002 (2)−0.021 (2)
C90.049 (2)0.040 (2)0.049 (2)0.0082 (18)0.0055 (19)−0.0021 (17)
C100.058 (3)0.051 (2)0.057 (3)0.014 (2)0.010 (2)−0.0077 (19)
C110.052 (3)0.058 (3)0.068 (3)0.020 (2)0.015 (2)0.003 (2)
C120.045 (2)0.060 (3)0.060 (3)0.003 (2)0.008 (2)0.004 (2)
C130.047 (2)0.046 (2)0.051 (2)−0.0023 (18)0.0070 (19)−0.0009 (17)
C140.045 (2)0.0354 (19)0.044 (2)0.0011 (16)0.0102 (17)0.0007 (16)
C150.058 (2)0.036 (2)0.041 (2)0.0021 (17)−0.0024 (19)−0.0043 (15)
C160.047 (2)0.0306 (18)0.046 (2)0.0049 (16)0.0073 (18)−0.0012 (15)
C170.043 (2)0.050 (2)0.050 (2)−0.0066 (18)0.0027 (18)−0.0054 (18)
C180.067 (3)0.048 (2)0.057 (3)−0.013 (2)0.003 (2)0.0000 (19)
C190.055 (2)0.057 (3)0.052 (2)−0.002 (2)0.020 (2)0.0180 (19)
C200.063 (3)0.063 (3)0.038 (2)0.006 (2)0.0227 (19)0.0073 (19)
C210.056 (2)0.039 (2)0.047 (2)0.0117 (18)−0.0001 (19)0.0057 (17)
C220.047 (2)0.037 (2)0.050 (2)0.0064 (17)−0.0003 (18)0.0011 (16)
N10.0424 (17)0.0356 (16)0.0361 (16)0.0006 (13)0.0027 (14)−0.0016 (13)
N20.0402 (16)0.0287 (15)0.0401 (16)0.0027 (13)0.0037 (13)−0.0051 (12)
N30.064 (2)0.0343 (18)0.055 (2)−0.0062 (17)0.0082 (18)−0.0069 (16)
N40.051 (2)0.0383 (18)0.063 (2)0.0029 (16)0.0114 (18)−0.0043 (16)
O10.0618 (19)0.079 (2)0.074 (2)0.0264 (17)−0.0188 (17)−0.0395 (18)
O20.0611 (19)0.0554 (19)0.095 (2)0.0182 (15)−0.0221 (18)−0.0349 (17)
O30.0648 (18)0.0436 (15)0.0444 (14)−0.0110 (13)0.0024 (13)0.0079 (12)
O40.0554 (16)0.0399 (14)0.0385 (13)0.0078 (12)0.0076 (12)−0.0001 (11)
O50.076 (2)0.074 (2)0.063 (2)0.0211 (18)−0.0111 (19)−0.0101 (17)
O60.071 (2)0.065 (2)0.0579 (19)0.0131 (16)−0.0053 (17)−0.0043 (14)
O70.075 (2)0.071 (2)0.135 (3)0.0246 (19)0.044 (2)−0.018 (2)
O80.079 (2)0.0600 (19)0.0618 (19)−0.0019 (16)−0.0068 (17)0.0067 (16)
O90.076 (9)0.036 (5)0.091 (7)−0.017 (8)0.008 (9)−0.002 (4)
O100.122 (3)0.054 (2)0.075 (2)−0.0126 (19)−0.023 (2)−0.0153 (17)
O110.090 (11)0.048 (7)0.087 (7)−0.031 (9)0.006 (11)−0.004 (5)

Geometric parameters (Å, °)

Cd1—N22.348 (3)C14—C161.508 (5)
Cd1—N12.369 (3)C15—N11.476 (5)
Cd1—O62.399 (3)C15—H15A0.9700
Cd1—O52.415 (3)C15—H15B0.9700
Cd1—O32.430 (3)C16—N21.484 (5)
Cd1—O82.433 (3)C16—H16A0.9700
Cd1—O42.523 (2)C16—H16B0.9700
Cd1—O102.673 (2)C17—N11.475 (5)
C1—C61.380 (5)C17—C181.503 (6)
C1—O11.382 (5)C17—H17A0.9700
C1—C21.383 (5)C17—H17B0.9700
C2—C31.364 (6)C18—O31.418 (5)
C2—H20.9300C18—H18A0.9700
C3—C41.370 (6)C18—H18B0.9700
C3—H30.9300C19—O31.417 (5)
C4—C51.378 (6)C19—C201.499 (6)
C4—H40.9300C19—H19A0.9700
C5—C61.389 (5)C19—H19B0.9700
C5—H50.9300C20—O41.425 (5)
C6—C151.504 (5)C20—H20A0.9700
C7—O11.315 (6)C20—H20B0.9700
C7—C81.445 (6)C21—O41.439 (4)
C7—H7A0.9700C21—C221.477 (6)
C7—H7B0.9700C21—H21A0.9700
C8—O21.384 (5)C21—H21B0.9700
C8—H8A0.9700C22—N21.477 (5)
C8—H8B0.9700C22—H22A0.9700
C9—O21.364 (5)C22—H22B0.9700
C9—C101.377 (6)N1—H1N0.90 (6)
C9—C141.387 (5)N2—H2N0.81 (6)
C10—C111.387 (6)N3—O101.219 (4)
C10—H100.9300N3—O91.24 (2)
C11—C121.366 (6)N3—O81.245 (4)
C11—H110.9300N3—O111.25 (2)
C12—C131.381 (6)N4—O71.207 (4)
C12—H120.9300N4—O61.245 (4)
C13—C141.389 (5)N4—O51.250 (5)
C13—H130.9300O9—O110.57 (2)
N2—Cd1—N191.47 (10)N2—C16—C14113.4 (3)
N2—Cd1—O6138.07 (10)N2—C16—H16A108.9
N1—Cd1—O6127.43 (11)C14—C16—H16A108.9
N2—Cd1—O5165.52 (12)N2—C16—H16B108.9
N1—Cd1—O583.75 (11)C14—C16—H16B108.9
O6—Cd1—O552.16 (11)H16A—C16—H16B107.7
N2—Cd1—O3101.75 (10)N1—C17—C18110.6 (3)
N1—Cd1—O369.64 (10)N1—C17—H17A109.5
O6—Cd1—O381.48 (10)C18—C17—H17A109.5
O5—Cd1—O389.42 (12)N1—C17—H17B109.5
N2—Cd1—O887.88 (11)C18—C17—H17B109.5
N1—Cd1—O8133.87 (10)H17A—C17—H17B108.1
O6—Cd1—O876.09 (12)O3—C18—C17107.1 (3)
O5—Cd1—O885.66 (11)O3—C18—H18A110.3
O3—Cd1—O8154.93 (10)C17—C18—H18A110.3
N2—Cd1—O471.36 (9)O3—C18—H18B110.3
N1—Cd1—O4126.54 (10)C17—C18—H18B110.3
O6—Cd1—O472.42 (9)H18A—C18—H18B108.6
O5—Cd1—O4122.27 (10)O3—C19—C20106.5 (3)
O3—Cd1—O465.46 (8)O3—C19—H19A110.4
O8—Cd1—O496.74 (9)C20—C19—H19A110.4
C6—C1—O1114.7 (3)O3—C19—H19B110.4
C6—C1—C2121.8 (4)C20—C19—H19B110.4
O1—C1—C2123.4 (4)H19A—C19—H19B108.6
C3—C2—C1119.1 (4)O4—C20—C19112.4 (3)
C3—C2—H2120.4O4—C20—H20A109.1
C1—C2—H2120.4C19—C20—H20A109.1
C2—C3—C4120.8 (4)O4—C20—H20B109.1
C2—C3—H3119.6C19—C20—H20B109.1
C4—C3—H3119.6H20A—C20—H20B107.9
C3—C4—C5119.6 (4)O4—C21—C22108.5 (3)
C3—C4—H4120.2O4—C21—H21A110.0
C5—C4—H4120.2C22—C21—H21A110.0
C4—C5—C6121.1 (4)O4—C21—H21B110.0
C4—C5—H5119.4C22—C21—H21B110.0
C6—C5—H5119.4H21A—C21—H21B108.4
C1—C6—C5117.5 (3)N2—C22—C21111.6 (3)
C1—C6—C15120.6 (3)N2—C22—H22A109.3
C5—C6—C15121.9 (4)C21—C22—H22A109.3
O1—C7—C8118.0 (4)N2—C22—H22B109.3
O1—C7—H7A107.8C21—C22—H22B109.3
C8—C7—H7A107.8H22A—C22—H22B108.0
O1—C7—H7B107.8C17—N1—C15112.6 (3)
C8—C7—H7B107.8C17—N1—Cd1107.7 (2)
H7A—C7—H7B107.1C15—N1—Cd1113.0 (2)
O2—C8—C7113.3 (4)C17—N1—H1N107 (4)
O2—C8—H8A108.9C15—N1—H1N110 (4)
C7—C8—H8A108.9Cd1—N1—H1N106 (3)
O2—C8—H8B108.9C22—N2—C16110.8 (3)
C7—C8—H8B108.9C22—N2—Cd1111.3 (2)
H8A—C8—H8B107.7C16—N2—Cd1115.1 (2)
O2—C9—C10124.3 (4)C22—N2—H2N110 (4)
O2—C9—C14114.7 (3)C16—N2—H2N109 (4)
C10—C9—C14121.0 (4)Cd1—N2—H2N101 (4)
C9—C10—C11118.9 (4)O10—N3—O9115.9 (12)
C9—C10—H10120.5O10—N3—O8117.9 (3)
C11—C10—H10120.5O9—N3—O8124.8 (13)
C12—C11—C10121.1 (4)O10—N3—O11125.5 (13)
C12—C11—H11119.4O8—N3—O11115.0 (12)
C10—C11—H11119.4O7—N4—O6122.5 (4)
C11—C12—C13119.5 (4)O7—N4—O5121.5 (4)
C11—C12—H12120.3O6—N4—O5116.0 (4)
C13—C12—H12120.3C7—O1—C1121.9 (3)
C12—C13—C14120.7 (4)C9—O2—C8121.2 (3)
C12—C13—H13119.6C19—O3—C18114.7 (3)
C14—C13—H13119.6C19—O3—Cd1123.4 (2)
C9—C14—C13118.7 (4)C18—O3—Cd1117.1 (2)
C9—C14—C16120.0 (3)C20—O4—C21113.4 (3)
C13—C14—C16121.3 (3)C20—O4—Cd1110.5 (2)
N1—C15—C6115.7 (3)C21—O4—Cd1109.0 (2)
N1—C15—H15A108.4N4—O5—Cd195.4 (2)
C6—C15—H15A108.4N4—O6—Cd196.3 (2)
N1—C15—H15B108.4N3—O8—Cd1101.7 (2)
C6—C15—H15B108.4O11—O9—N377 (5)
H15A—C15—H15B107.4O9—O11—N377 (4)
C6—C1—C2—C32.1 (7)C10—C9—O2—C8−20.9 (7)
O1—C1—C2—C3178.4 (4)C14—C9—O2—C8161.5 (4)
C1—C2—C3—C40.4 (7)C7—C8—O2—C9173.2 (6)
C2—C3—C4—C5−1.4 (7)C20—C19—O3—C18−177.5 (3)
C3—C4—C5—C60.0 (6)C20—C19—O3—Cd1−22.8 (4)
O1—C1—C6—C5−180.0 (4)C17—C18—O3—C19−178.7 (4)
C2—C1—C6—C5−3.4 (6)C17—C18—O3—Cd124.9 (4)
O1—C1—C6—C15−3.1 (6)N2—Cd1—O3—C19−64.3 (3)
C2—C1—C6—C15173.5 (4)N1—Cd1—O3—C19−151.5 (3)
C4—C5—C6—C12.3 (6)O6—Cd1—O3—C1973.2 (3)
C4—C5—C6—C15−174.6 (4)O5—Cd1—O3—C19125.0 (3)
O1—C7—C8—O218.3 (10)O8—Cd1—O3—C1946.5 (4)
O2—C9—C10—C11−176.8 (4)O4—Cd1—O3—C19−1.3 (3)
C14—C9—C10—C110.7 (7)N2—Cd1—O3—C1889.8 (3)
C9—C10—C11—C12−1.5 (7)N1—Cd1—O3—C182.7 (3)
C10—C11—C12—C131.5 (7)O6—Cd1—O3—C18−132.7 (3)
C11—C12—C13—C14−0.7 (6)O5—Cd1—O3—C18−80.9 (3)
O2—C9—C14—C13177.8 (4)O8—Cd1—O3—C18−159.3 (3)
C10—C9—C14—C130.1 (6)O4—Cd1—O3—C18152.8 (3)
O2—C9—C14—C16−3.8 (5)C19—C20—O4—C2171.5 (4)
C10—C9—C14—C16178.5 (4)C19—C20—O4—Cd1−51.3 (4)
C12—C13—C14—C9−0.1 (6)C22—C21—O4—C20−166.5 (3)
C12—C13—C14—C16−178.5 (4)C22—C21—O4—Cd1−43.0 (3)
C1—C6—C15—N168.8 (5)N2—Cd1—O4—C20140.1 (2)
C5—C6—C15—N1−114.5 (4)N1—Cd1—O4—C2062.6 (3)
C9—C14—C16—N2−80.7 (4)O6—Cd1—O4—C20−61.4 (2)
C13—C14—C16—N297.7 (4)O5—Cd1—O4—C20−45.4 (3)
N1—C17—C18—O3−54.4 (5)O3—Cd1—O4—C2027.1 (2)
O3—C19—C20—O448.3 (5)O8—Cd1—O4—C20−134.5 (2)
O4—C21—C22—N261.4 (4)N2—Cd1—O4—C2114.8 (2)
C18—C17—N1—C15−177.6 (3)N1—Cd1—O4—C21−62.7 (2)
C18—C17—N1—Cd157.3 (3)O6—Cd1—O4—C21173.3 (2)
C6—C15—N1—C1763.5 (4)O5—Cd1—O4—C21−170.7 (2)
C6—C15—N1—Cd1−174.3 (3)O3—Cd1—O4—C21−98.2 (2)
N2—Cd1—N1—C17−132.3 (2)O8—Cd1—O4—C21100.2 (2)
O6—Cd1—N1—C1730.8 (3)O7—N4—O5—Cd1179.6 (4)
O5—Cd1—N1—C1761.4 (2)O6—N4—O5—Cd1−2.4 (4)
O3—Cd1—N1—C17−30.3 (2)N2—Cd1—O5—N4140.9 (4)
O8—Cd1—N1—C17139.2 (2)N1—Cd1—O5—N4−147.8 (3)
O4—Cd1—N1—C17−64.6 (3)O6—Cd1—O5—N41.4 (2)
N2—Cd1—N1—C15102.8 (3)O3—Cd1—O5—N4−78.2 (3)
O6—Cd1—N1—C15−94.1 (3)O8—Cd1—O5—N477.1 (3)
O5—Cd1—N1—C15−63.5 (3)O4—Cd1—O5—N4−18.1 (3)
O3—Cd1—N1—C15−155.2 (3)O7—N4—O6—Cd1−179.6 (4)
O8—Cd1—N1—C1514.3 (3)O5—N4—O6—Cd12.4 (4)
O4—Cd1—N1—C15170.5 (2)N2—Cd1—O6—N4−167.3 (2)
C21—C22—N2—C16−176.0 (3)N1—Cd1—O6—N438.4 (3)
C21—C22—N2—Cd1−46.6 (3)O5—Cd1—O6—N4−1.4 (2)
C14—C16—N2—C22−62.8 (4)O3—Cd1—O6—N494.5 (2)
C14—C16—N2—Cd1169.9 (2)O8—Cd1—O6—N4−96.8 (2)
N1—Cd1—N2—C22144.3 (2)O4—Cd1—O6—N4161.4 (2)
O6—Cd1—N2—C22−15.5 (3)O10—N3—O8—Cd112.1 (4)
O5—Cd1—N2—C22−145.3 (4)O9—N3—O8—Cd1−153.4 (9)
O3—Cd1—N2—C2274.8 (2)O11—N3—O8—Cd1178.3 (10)
O8—Cd1—N2—C22−81.9 (2)N2—Cd1—O8—N3−99.4 (3)
O4—Cd1—N2—C2216.0 (2)N1—Cd1—O8—N3−9.4 (3)
N1—Cd1—N2—C16−88.7 (2)O6—Cd1—O8—N3119.7 (3)
O6—Cd1—N2—C16111.5 (2)O5—Cd1—O8—N367.6 (3)
O5—Cd1—N2—C16−18.3 (5)O3—Cd1—O8—N3146.9 (3)
O3—Cd1—N2—C16−158.2 (2)O4—Cd1—O8—N3−170.4 (3)
O8—Cd1—N2—C1645.2 (2)O10—N3—O9—O11118 (5)
O4—Cd1—N2—C16143.0 (2)O8—N3—O9—O11−76 (6)
C8—C7—O1—C1−178.4 (5)O10—N3—O11—O9−76 (6)
C6—C1—O1—C7−170.9 (6)O8—N3—O11—O9118 (5)
C2—C1—O1—C712.6 (8)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CS2056).

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