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Acta Crystallogr Sect E Struct Rep Online. 2008 June 1; 64(Pt 6): m784.
Published online 2008 May 7. doi:  10.1107/S1600536808012609
PMCID: PMC2961553

catena-Poly[[bis­[1-phenyl-3-(1H-1,2,4-triazol-1-yl)propan-1-one-κN 4]cadmium(II)]-di-μ-azido-κ4 N 1:N 3]

Abstract

In the crystal structure of the title complex, [Cd(N3)2(C11H11N31)2]n, there are two crystallographically independent CdII atoms. Both exist in an octa­hedral environment composed of four N atoms of the N3 groups and two N atoms from two monodentate 1-phenyl-3-(1H-1,2,4-triazol-1-yl)propan-1-one ligands that are positioned trans to each other. Adjacent CdII centres in the crystal structure are bridged by a pair of N3 anions in a μ-1,3-fashion, forming an infinite one-dimensional array.

Related literature

For related literature, see: Guo & Cai (2007 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m784-scheme1.jpg

Experimental

Crystal data

  • [Cd(N3)2(C11H11N31)2]
  • M r = 598.92
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m784-efi1.jpg
  • a = 10.1626 (16) Å
  • b = 17.732 (3) Å
  • c = 28.124 (4) Å
  • β = 91.980 (2)°
  • V = 5064.9 (14) Å3
  • Z = 8
  • Mo Kα radiation
  • μ = 0.91 mm−1
  • T = 294 (2) K
  • 0.24 × 0.22 × 0.14 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 2004 [triangle]) T min = 0.760, T max = 1.000 (expected range = 0.670–0.881)
  • 26797 measured reflections
  • 8928 independent reflections
  • 7054 reflections with I > 2σ(I)
  • R int = 0.021

Refinement

  • R[F 2 > 2σ(F 2)] = 0.031
  • wR(F 2) = 0.069
  • S = 1.09
  • 8928 reflections
  • 667 parameters
  • H-atom parameters constrained
  • Δρmax = 0.67 e Å−3
  • Δρmin = −0.72 e Å−3

Data collection: SMART (Bruker, 2001 [triangle]); cell refinement: SAINT (Bruker, 2001 [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 (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808012609/bv2096sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808012609/bv2096Isup2.hkl

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

supplementary crystallographic information

Comment

Pseudohalide anions N3-, NCS- and NCO- are known as extremely versatile ligands in coordination chemistry because of their multiple bridging modes. Recently, we initiated a research program involving synthesizing supramolecules based on a pseudohalide and a flexible ligand consisting of a propanone unit substituted with an imidazole and a phenyl group (Cai & Guo, 2007). To further explore this series, we synthesized the title compound, (I), a new CdII complex based on the mixed ligands azide and 3-(1H-1,2,4-triazol-1-yl) -1-phenylpropan-1-one (L), which consists of a propanone unit substituted with an triazole and a phenyl group.

The X-ray crystallographic analysis shows that the structure of complex I consists of 1-D CdII chains with two CdII atoms in the asymmetric unit. Two crystallographically independent CdII ions have similar coordination environment, but different bond parameters. In both cases, each CdII atom is in a distorted N6 octahedron environment, consisting of two terminal and two bridging azide N atoms and N atoms from two ligand (L) (arranged in a cis fation). The Cd—N bond distance range from 2.313 (3)Å to 2.369 (3) Å. Cd1 and Cd2 are displaced by 0.2047 and 0.7313Å from the mean basal plane toward the apical nitrogen atoms (N24 and N7). In this structure, the ligand L displays monodentate binding to CdII and the triazole and phenyl rings in each of the ligands are not coplanar. The dihedral angels formed by the least-squares planes of the phenyl and triazole rings are 78.1 (1)°, 74.5 (1)° 74.3 (1)° and 77.5 (1)°, respectively. Adjacent CdII centers are bridged by two azide anions in an end-to-end (µ-1,3) fashion forming a 1-D chain polymer, as illustrated in Fig.2. The minimum interdinuclear Cd···Cd distance is 5.415 Å.

Experimental

All the starting materials and solvents for syntheses were obtained commercially and used as received. Cd(NO3)2.4H2O (30.8 mg, 0.1 mmol), 3-(1H-1,2,4-triazol-1-yl)-1-phenylpropan-1-one (22.3 mg, 0.1 mmol) and NaN3 (6.7 mg, 0.1 mmol) were mixed in a CH3CN–H2O (20 ml, 1:1 v/v) solution with vigorous stirring for ca 30 min. The resulting solution was filtered and left to stand at room temperature. Colourless prismatic crystals of I suitable for X-ray analysis were obtained in 60% yield by slow evaporation of the solvent over a period of 1 week. Analysis, calculated for CdC22H22N12O2: C 44.12, H 3.70, N 28.06; found: C 44.15, H 3.83, N 28.10.

Refinement

Although all H atoms were visible in difference maps, they were placed in geometrically calculated positions, with C—H distances in the range 0.93–0.97 Å, and included in the final refinement in the riding model approximation,with Uiso(H) = 1.2Ueq(C) for aromatic and methylene H atoms.

Figures

Fig. 1.
The molecular structure of (I), with atom labels and 30% probability displacement ellipsoids.
Fig. 2.
One-dimensional chain connected by N3-. H atoms have been omitted.

Crystal data

[Cd(N3)2(C11H11N3)2]F000 = 2416
Mr = 598.92Dx = 1.571 Mg m3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 8981 reflections
a = 10.1626 (16) Åθ = 2.4–27.9º
b = 17.732 (3) ŵ = 0.91 mm1
c = 28.124 (4) ÅT = 294 (2) K
β = 91.980 (2)ºBlock, pale yellow
V = 5064.9 (14) Å30.24 × 0.22 × 0.14 mm
Z = 8

Data collection

Bruker SMART CCD area-detector diffractometer8928 independent reflections
Radiation source: fine-focus sealed tube7054 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.021
T = 294(2) Kθmax = 25.0º
[var phi] and ω scansθmin = 1.9º
Absorption correction: multi-scan(SADABS; Sheldrick, 2004)h = −12→12
Tmin = 0.760, Tmax = 1.000k = −21→17
26797 measured reflectionsl = −30→33

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.031H-atom parameters constrained
wR(F2) = 0.069  w = 1/[σ2(Fo2) + (0.0145P)2 + 5.5025P] where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
8928 reflectionsΔρmax = 0.67 e Å3
667 parametersΔρmin = −0.72 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none

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.
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)

xyzUiso*/Ueq
Cd10.50852 (2)0.061464 (13)0.240599 (8)0.03961 (7)
Cd21.00703 (2)0.168651 (13)0.237148 (8)0.03910 (7)
O10.4692 (3)−0.11356 (17)0.06491 (9)0.0803 (9)
O20.5268 (3)−0.09785 (16)0.44068 (9)0.0737 (8)
O30.9832 (3)0.34977 (16)0.05865 (9)0.0758 (8)
O41.0136 (3)0.33667 (16)0.43755 (10)0.0801 (9)
N10.5899 (2)−0.04669 (16)0.20487 (9)0.0472 (7)
N20.7191 (3)−0.13452 (19)0.17430 (11)0.0653 (9)
N30.5917 (2)−0.14797 (16)0.16199 (9)0.0437 (7)
N40.4138 (2)−0.01421 (16)0.29893 (9)0.0473 (7)
N50.2778 (3)−0.09947 (19)0.32893 (11)0.0618 (8)
N60.4052 (2)−0.11606 (16)0.34126 (9)0.0457 (7)
N70.9118 (2)0.24449 (17)0.29467 (9)0.0484 (7)
N80.7799 (3)0.3330 (2)0.32370 (11)0.0651 (9)
N90.9081 (2)0.34863 (16)0.33551 (9)0.0453 (7)
N101.0898 (2)0.27623 (16)0.20045 (9)0.0454 (7)
N111.2206 (3)0.36462 (19)0.17075 (11)0.0641 (9)
N121.0927 (2)0.37879 (15)0.15837 (9)0.0425 (6)
N130.1203 (3)0.10059 (19)0.18182 (10)0.0608 (8)
N140.2190 (3)0.06887 (15)0.18986 (8)0.0409 (6)
N150.3163 (3)0.03539 (18)0.19487 (10)0.0578 (8)
N160.6970 (3)0.06784 (18)0.29227 (9)0.0570 (8)
N170.8037 (3)0.06395 (15)0.27865 (9)0.0462 (7)
N180.9121 (3)0.05811 (17)0.26561 (11)0.0607 (8)
N190.6188 (3)0.1277 (2)0.18341 (10)0.0698 (10)
N200.7180 (3)0.15975 (16)0.18864 (8)0.0431 (6)
N210.8162 (3)0.19275 (18)0.19088 (10)0.0602 (8)
N221.1938 (3)0.16446 (18)0.28984 (10)0.0562 (8)
N231.3020 (3)0.16754 (15)0.27785 (9)0.0457 (7)
N241.4122 (3)0.17232 (17)0.26625 (12)0.0642 (9)
C10.5177 (3)−0.0957 (2)0.18030 (11)0.0475 (8)
H10.4265−0.09360.17650.057*
C20.7122 (3)−0.0734 (2)0.20004 (13)0.0623 (11)
H20.7862−0.05030.21390.075*
C30.5523 (4)−0.2140 (2)0.13389 (11)0.0533 (9)
H3A0.4571−0.21500.13020.064*
H3B0.5797−0.25920.15100.064*
C40.6107 (3)−0.21481 (19)0.08523 (10)0.0503 (8)
H4A0.7045−0.20520.08870.060*
H4B0.5993−0.26470.07160.060*
C50.5504 (3)−0.1578 (2)0.05133 (11)0.0491 (8)
C60.5919 (3)−0.1582 (2)0.00092 (11)0.0496 (8)
C70.6808 (4)−0.2096 (2)−0.01580 (13)0.0677 (11)
H70.7188−0.24510.00480.081*
C80.7136 (4)−0.2087 (3)−0.06316 (15)0.0869 (14)
H80.7745−0.2431−0.07420.104*
C90.6573 (5)−0.1578 (3)−0.09350 (15)0.0893 (15)
H90.6787−0.1583−0.12540.107*
C100.5698 (5)−0.1060 (3)−0.07781 (15)0.0910 (15)
H100.5327−0.0707−0.09870.109*
C110.5366 (4)−0.1064 (2)−0.03040 (13)0.0729 (11)
H110.4764−0.0713−0.01960.087*
C120.2887 (3)−0.0380 (2)0.30351 (12)0.0576 (10)
H120.2165−0.01300.28980.069*
C130.4829 (3)−0.06464 (19)0.32326 (11)0.0457 (8)
H130.5742−0.06410.32720.055*
C140.4417 (4)−0.1862 (2)0.36616 (12)0.0570 (9)
H14A0.5368−0.18830.37030.068*
H14B0.4142−0.22880.34650.068*
C150.3809 (3)−0.1935 (2)0.41427 (11)0.0540 (9)
H15A0.2876−0.18240.41090.065*
H15B0.3899−0.24530.42500.065*
C160.4416 (3)−0.1423 (2)0.45150 (12)0.0512 (8)
C170.3961 (3)−0.14650 (19)0.50138 (12)0.0480 (8)
C180.4449 (4)−0.0950 (2)0.53441 (14)0.0665 (10)
H180.5055−0.05890.52530.080*
C190.4047 (5)−0.0965 (3)0.58076 (15)0.0816 (13)
H190.4376−0.06140.60270.098*
C200.3166 (5)−0.1496 (3)0.59435 (15)0.0784 (13)
H200.2890−0.15040.62550.094*
C210.2687 (4)−0.2015 (3)0.56260 (15)0.0798 (13)
H210.2097−0.23800.57240.096*
C220.3071 (4)−0.2003 (2)0.51579 (13)0.0648 (10)
H220.2731−0.23550.49410.078*
C230.7883 (3)0.2704 (2)0.29933 (13)0.0621 (10)
H230.71480.24580.28630.075*
C240.9835 (3)0.29546 (19)0.31817 (11)0.0458 (8)
H241.07480.29400.32200.055*
C250.9481 (4)0.4190 (2)0.35863 (12)0.0566 (9)
H25A0.92900.46040.33690.068*
H25B1.04260.41790.36470.068*
C260.8818 (3)0.4346 (2)0.40490 (12)0.0550 (9)
H26A0.89280.48740.41300.066*
H26B0.78820.42480.40070.066*
C270.9364 (3)0.3870 (2)0.44546 (13)0.0527 (9)
C280.8959 (3)0.4038 (2)0.49479 (12)0.0526 (9)
C290.8199 (4)0.4657 (2)0.50574 (14)0.0670 (11)
H290.79000.49820.48180.080*
C300.7885 (4)0.4793 (3)0.55244 (16)0.0836 (13)
H300.73770.52110.55970.100*
C310.8313 (5)0.4320 (3)0.58799 (16)0.0857 (14)
H310.80910.44130.61920.103*
C320.9068 (5)0.3708 (3)0.57762 (15)0.0902 (15)
H320.93650.33870.60180.108*
C330.9391 (4)0.3566 (2)0.53122 (14)0.0730 (12)
H330.99050.31490.52440.088*
C341.0186 (3)0.3258 (2)0.17610 (11)0.0479 (8)
H340.92750.32360.17200.057*
C351.2127 (3)0.3027 (2)0.19569 (12)0.0596 (10)
H351.28640.27870.20910.072*
C361.0534 (3)0.44613 (19)0.13156 (11)0.0514 (8)
H36A1.07680.49030.15030.062*
H36B0.95850.44590.12670.062*
C371.1161 (3)0.45241 (19)0.08383 (11)0.0489 (8)
H37A1.10330.50330.07180.059*
H37B1.21010.44410.08810.059*
C381.0618 (3)0.3976 (2)0.04744 (11)0.0472 (8)
C391.1059 (3)0.40312 (19)−0.00248 (11)0.0449 (8)
C401.0632 (4)0.3493 (2)−0.03517 (13)0.0629 (10)
H401.00880.3104−0.02570.076*
C411.1009 (5)0.3532 (2)−0.08185 (14)0.0760 (12)
H411.07190.3168−0.10360.091*
C421.1803 (4)0.4101 (3)−0.09617 (14)0.0738 (12)
H421.20570.4122−0.12760.089*
C431.2228 (4)0.4640 (3)−0.06451 (14)0.0747 (12)
H431.27650.5029−0.07450.090*
C441.1860 (3)0.4608 (2)−0.01754 (12)0.0596 (10)
H441.21530.49750.00390.072*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cd10.02805 (11)0.04518 (14)0.04591 (13)−0.00049 (10)0.00570 (9)−0.00056 (11)
Cd20.02820 (11)0.04316 (14)0.04624 (13)−0.00053 (10)0.00576 (9)0.00231 (10)
O10.095 (2)0.088 (2)0.0581 (16)0.0446 (18)0.0029 (14)−0.0031 (15)
O20.0821 (19)0.0700 (19)0.0689 (17)−0.0344 (16)0.0020 (14)0.0044 (14)
O30.096 (2)0.071 (2)0.0602 (16)−0.0429 (17)0.0034 (14)0.0020 (14)
O40.102 (2)0.0661 (19)0.0718 (18)0.0399 (17)−0.0006 (15)−0.0043 (14)
N10.0327 (14)0.0584 (19)0.0509 (15)0.0039 (13)0.0053 (11)−0.0117 (14)
N20.0376 (16)0.082 (2)0.075 (2)0.0148 (15)−0.0063 (14)−0.0310 (19)
N30.0375 (14)0.0548 (19)0.0388 (14)0.0008 (13)0.0002 (11)−0.0063 (13)
N40.0322 (14)0.061 (2)0.0493 (15)−0.0042 (13)0.0060 (12)0.0060 (14)
N50.0357 (16)0.076 (2)0.073 (2)−0.0120 (15)0.0021 (14)0.0167 (18)
N60.0381 (15)0.0515 (19)0.0476 (15)−0.0049 (13)0.0033 (12)0.0012 (13)
N70.0337 (14)0.061 (2)0.0504 (16)0.0009 (13)0.0076 (12)−0.0027 (14)
N80.0365 (16)0.080 (2)0.079 (2)0.0155 (16)0.0037 (14)−0.0164 (19)
N90.0372 (15)0.0497 (19)0.0492 (15)0.0091 (13)0.0040 (12)0.0007 (13)
N100.0333 (14)0.0519 (18)0.0511 (15)−0.0004 (13)0.0059 (11)0.0112 (13)
N110.0367 (16)0.082 (2)0.073 (2)−0.0132 (15)−0.0052 (14)0.0301 (18)
N120.0385 (14)0.0466 (18)0.0422 (14)−0.0032 (13)−0.0004 (11)0.0036 (12)
N130.0482 (17)0.076 (2)0.0580 (18)0.0179 (17)−0.0023 (14)−0.0157 (16)
N140.0380 (15)0.0452 (17)0.0394 (14)−0.0024 (13)0.0004 (11)−0.0090 (12)
N150.0405 (16)0.064 (2)0.0684 (19)0.0066 (15)−0.0114 (14)−0.0116 (16)
N160.0415 (17)0.080 (2)0.0490 (16)−0.0104 (15)0.0005 (13)0.0002 (15)
N170.0451 (17)0.0447 (17)0.0484 (15)−0.0092 (13)−0.0067 (13)0.0127 (13)
N180.0431 (17)0.054 (2)0.085 (2)−0.0081 (15)0.0063 (15)0.0174 (16)
N190.0513 (18)0.099 (3)0.0590 (19)−0.0305 (19)−0.0032 (14)0.0234 (18)
N200.0378 (15)0.0520 (18)0.0392 (14)0.0007 (14)−0.0014 (11)0.0113 (12)
N210.0398 (16)0.072 (2)0.0675 (19)−0.0107 (16)−0.0099 (13)0.0173 (17)
N220.0398 (16)0.079 (2)0.0502 (16)0.0108 (15)0.0001 (13)−0.0016 (15)
N230.0460 (17)0.0425 (17)0.0478 (15)0.0077 (13)−0.0092 (13)−0.0092 (13)
N240.0423 (18)0.053 (2)0.097 (2)−0.0007 (15)0.0045 (16)−0.0172 (17)
C10.0293 (16)0.060 (2)0.0533 (19)−0.0016 (16)0.0060 (14)−0.0069 (17)
C20.0345 (18)0.082 (3)0.070 (2)0.0063 (18)−0.0061 (16)−0.030 (2)
C30.067 (2)0.049 (2)0.0432 (18)−0.0044 (18)−0.0014 (16)−0.0032 (16)
C40.062 (2)0.046 (2)0.0429 (18)0.0074 (17)−0.0039 (15)−0.0061 (15)
C50.054 (2)0.046 (2)0.0466 (19)0.0050 (17)−0.0017 (15)−0.0034 (16)
C60.055 (2)0.052 (2)0.0420 (18)−0.0061 (17)−0.0038 (15)−0.0009 (16)
C70.066 (2)0.086 (3)0.052 (2)0.011 (2)0.0080 (18)0.000 (2)
C80.076 (3)0.122 (4)0.064 (3)0.003 (3)0.020 (2)−0.010 (3)
C90.108 (4)0.111 (4)0.050 (2)−0.031 (3)0.016 (3)0.006 (3)
C100.134 (4)0.084 (4)0.053 (3)−0.010 (3)−0.010 (3)0.020 (2)
C110.097 (3)0.065 (3)0.057 (2)0.009 (2)−0.004 (2)0.003 (2)
C120.0357 (18)0.076 (3)0.061 (2)−0.0016 (18)0.0047 (15)0.017 (2)
C130.0318 (16)0.056 (2)0.0500 (18)−0.0032 (16)0.0049 (14)0.0006 (17)
C140.066 (2)0.046 (2)0.059 (2)−0.0013 (18)0.0030 (17)−0.0015 (18)
C150.061 (2)0.044 (2)0.057 (2)−0.0091 (17)−0.0012 (16)0.0073 (17)
C160.048 (2)0.046 (2)0.059 (2)−0.0029 (17)−0.0041 (16)0.0055 (17)
C170.0493 (19)0.040 (2)0.054 (2)0.0044 (16)−0.0054 (15)0.0068 (16)
C180.088 (3)0.044 (2)0.067 (2)−0.004 (2)−0.007 (2)0.001 (2)
C190.118 (4)0.062 (3)0.065 (3)0.013 (3)−0.008 (3)−0.010 (2)
C200.090 (3)0.088 (4)0.058 (3)0.026 (3)0.009 (2)0.009 (2)
C210.070 (3)0.102 (4)0.068 (3)−0.012 (3)0.009 (2)0.017 (3)
C220.060 (2)0.073 (3)0.060 (2)−0.014 (2)−0.0021 (18)0.008 (2)
C230.0306 (18)0.086 (3)0.070 (2)0.0037 (18)0.0050 (16)−0.016 (2)
C240.0325 (16)0.051 (2)0.0541 (19)0.0082 (16)0.0075 (14)0.0047 (17)
C250.057 (2)0.049 (2)0.064 (2)0.0054 (18)0.0049 (17)0.0031 (18)
C260.057 (2)0.046 (2)0.062 (2)0.0106 (17)0.0042 (17)−0.0043 (17)
C270.053 (2)0.041 (2)0.064 (2)0.0024 (17)−0.0003 (17)−0.0046 (17)
C280.051 (2)0.049 (2)0.058 (2)−0.0078 (17)0.0013 (16)−0.0068 (18)
C290.062 (2)0.073 (3)0.066 (2)0.007 (2)0.0058 (19)−0.006 (2)
C300.080 (3)0.089 (4)0.082 (3)0.010 (3)0.016 (2)−0.020 (3)
C310.093 (3)0.101 (4)0.063 (3)−0.018 (3)0.015 (2)−0.013 (3)
C320.121 (4)0.091 (4)0.059 (3)−0.009 (3)−0.003 (3)0.006 (3)
C330.092 (3)0.058 (3)0.068 (3)0.005 (2)−0.005 (2)0.000 (2)
C340.0326 (17)0.055 (2)0.056 (2)−0.0032 (16)0.0046 (14)0.0081 (17)
C350.0312 (17)0.079 (3)0.068 (2)−0.0041 (18)−0.0054 (15)0.027 (2)
C360.062 (2)0.046 (2)0.0460 (19)0.0012 (17)−0.0010 (16)0.0004 (16)
C370.057 (2)0.044 (2)0.0456 (18)−0.0104 (16)−0.0037 (15)0.0069 (15)
C380.053 (2)0.042 (2)0.0464 (18)−0.0059 (17)−0.0050 (15)0.0060 (16)
C390.0481 (19)0.042 (2)0.0445 (17)0.0041 (16)−0.0036 (14)0.0043 (16)
C400.083 (3)0.048 (2)0.057 (2)−0.004 (2)−0.0036 (19)−0.0060 (18)
C410.111 (4)0.060 (3)0.056 (2)0.012 (3)−0.008 (2)−0.017 (2)
C420.084 (3)0.087 (3)0.050 (2)0.018 (3)0.007 (2)−0.001 (2)
C430.072 (3)0.094 (3)0.058 (2)−0.014 (2)0.007 (2)0.012 (2)
C440.064 (2)0.065 (3)0.050 (2)−0.013 (2)−0.0009 (17)0.0007 (18)

Geometric parameters (Å, °)

Cd1—N192.313 (3)C9—C101.363 (7)
Cd1—N24i2.322 (3)C9—H90.9300
Cd1—N12.330 (3)C10—C111.387 (6)
Cd1—N152.347 (3)C10—H100.9300
Cd1—N42.351 (3)C11—H110.9300
Cd1—N162.366 (3)C12—H120.9300
Cd2—N13ii2.308 (3)C13—H130.9300
Cd2—N212.337 (3)C14—C151.512 (4)
Cd2—N182.338 (3)C14—H14A0.9700
Cd2—N72.339 (3)C14—H14B0.9700
Cd2—N102.339 (3)C15—C161.503 (5)
Cd2—N222.369 (3)C15—H15A0.9700
O1—C51.210 (4)C15—H15B0.9700
O2—C161.217 (4)C16—C171.494 (5)
O3—C381.214 (4)C17—C181.382 (5)
O4—C271.215 (4)C17—C221.385 (5)
N1—C11.318 (4)C18—C191.380 (5)
N1—C21.341 (4)C18—H180.9300
N2—C21.306 (4)C19—C201.363 (6)
N2—N31.350 (3)C19—H190.9300
N3—C11.309 (4)C20—C211.360 (6)
N3—C31.460 (4)C20—H200.9300
N4—C131.315 (4)C21—C221.386 (5)
N4—C121.350 (4)C21—H210.9300
N5—C121.310 (4)C22—H220.9300
N5—N61.360 (4)C23—H230.9300
N6—C131.319 (4)C24—H240.9300
N6—C141.469 (4)C25—C261.511 (4)
N7—C241.323 (4)C25—H25A0.9700
N7—C231.348 (4)C25—H25B0.9700
N8—C231.308 (5)C26—C271.509 (5)
N8—N91.362 (4)C26—H26A0.9700
N9—C241.319 (4)C26—H26B0.9700
N9—C251.458 (4)C27—C281.490 (5)
N10—C341.315 (4)C28—C331.382 (5)
N10—C351.345 (4)C28—C291.383 (5)
N11—C351.307 (4)C29—C301.384 (5)
N11—N121.357 (3)C29—H290.9300
N12—C341.313 (4)C30—C311.365 (6)
N12—C361.460 (4)C30—H300.9300
N13—N141.165 (4)C31—C321.366 (6)
N13—Cd2i2.308 (3)C31—H310.9300
N14—N151.158 (4)C32—C331.379 (6)
N16—N171.165 (4)C32—H320.9300
N17—N181.178 (4)C33—H330.9300
N19—N201.162 (4)C34—H340.9300
N20—N211.156 (4)C35—H350.9300
N22—N231.163 (4)C36—C371.510 (4)
N23—N241.180 (4)C36—H36A0.9700
N24—Cd1ii2.322 (3)C36—H36B0.9700
C1—H10.9300C37—C381.502 (4)
C2—H20.9300C37—H37A0.9700
C3—C41.510 (4)C37—H37B0.9700
C3—H3A0.9700C38—C391.492 (4)
C3—H3B0.9700C39—C441.383 (5)
C4—C51.505 (4)C39—C401.384 (5)
C4—H4A0.9700C40—C411.382 (5)
C4—H4B0.9700C40—H400.9300
C5—C61.493 (4)C41—C421.361 (6)
C6—C71.378 (5)C41—H410.9300
C6—C111.379 (5)C42—C431.366 (6)
C7—C81.384 (5)C42—H420.9300
C7—H70.9300C43—C441.386 (5)
C8—C91.354 (6)C43—H430.9300
C8—H80.9300C44—H440.9300
N19—Cd1—N24i90.32 (12)N4—C13—H13124.7
N19—Cd1—N186.02 (12)N6—C13—H13124.7
N24i—Cd1—N1172.10 (10)N6—C14—C15113.2 (3)
N19—Cd1—N1597.65 (11)N6—C14—H14A108.9
N24i—Cd1—N1589.15 (10)C15—C14—H14A108.9
N1—Cd1—N1584.41 (10)N6—C14—H14B108.9
N19—Cd1—N4174.39 (11)C15—C14—H14B108.9
N24i—Cd1—N494.54 (11)H14A—C14—H14B107.7
N1—Cd1—N489.49 (10)C16—C15—C14113.7 (3)
N15—Cd1—N485.23 (10)C16—C15—H15A108.8
N19—Cd1—N1690.08 (10)C14—C15—H15A108.8
N24i—Cd1—N1696.30 (11)C16—C15—H15B108.8
N1—Cd1—N1690.71 (10)C14—C15—H15B108.8
N15—Cd1—N16170.53 (11)H15A—C15—H15B107.7
N4—Cd1—N1686.62 (9)O2—C16—C17120.9 (3)
N13ii—Cd2—N2198.27 (11)O2—C16—C15119.7 (3)
N13ii—Cd2—N1890.79 (12)C17—C16—C15119.4 (3)
N21—Cd2—N1889.98 (10)C18—C17—C22118.8 (3)
N13ii—Cd2—N7174.22 (10)C18—C17—C16118.8 (3)
N21—Cd2—N785.69 (10)C22—C17—C16122.4 (3)
N18—Cd2—N793.43 (10)C19—C18—C17120.7 (4)
N13ii—Cd2—N1086.19 (11)C19—C18—H18119.6
N21—Cd2—N1084.79 (10)C17—C18—H18119.6
N18—Cd2—N10173.53 (10)C20—C19—C18119.8 (4)
N7—Cd2—N1090.00 (10)C20—C19—H19120.1
N13ii—Cd2—N2289.88 (10)C18—C19—H19120.1
N21—Cd2—N22170.29 (11)C21—C20—C19120.4 (4)
N18—Cd2—N2295.21 (11)C21—C20—H20119.8
N7—Cd2—N2285.81 (9)C19—C20—H20119.8
N10—Cd2—N2290.52 (10)C20—C21—C22120.5 (4)
C1—N1—C2102.4 (3)C20—C21—H21119.8
C1—N1—Cd1124.8 (2)C22—C21—H21119.8
C2—N1—Cd1132.7 (2)C17—C22—C21119.8 (4)
C2—N2—N3102.7 (3)C17—C22—H22120.1
C1—N3—N2109.4 (3)C21—C22—H22120.1
C1—N3—C3129.0 (3)N8—C23—N7114.7 (3)
N2—N3—C3121.5 (3)N8—C23—H23122.6
C13—N4—C12103.1 (3)N7—C23—H23122.6
C13—N4—Cd1121.81 (19)N9—C24—N7110.9 (3)
C12—N4—Cd1130.9 (2)N9—C24—H24124.6
C12—N5—N6102.8 (3)N7—C24—H24124.6
C13—N6—N5109.3 (3)N9—C25—C26114.5 (3)
C13—N6—C14128.6 (3)N9—C25—H25A108.6
N5—N6—C14121.8 (3)C26—C25—H25A108.6
C24—N7—C23102.5 (3)N9—C25—H25B108.6
C24—N7—Cd2120.30 (19)C26—C25—H25B108.6
C23—N7—Cd2132.3 (2)H25A—C25—H25B107.6
C23—N8—N9102.8 (3)C27—C26—C25112.7 (3)
C24—N9—N8109.1 (3)C27—C26—H26A109.0
C24—N9—C25128.3 (3)C25—C26—H26A109.0
N8—N9—C25122.2 (3)C27—C26—H26B109.0
C34—N10—C35102.2 (3)C25—C26—H26B109.0
C34—N10—Cd2125.1 (2)H26A—C26—H26B107.8
C35—N10—Cd2132.6 (2)O4—C27—C28121.2 (3)
C35—N11—N12102.5 (3)O4—C27—C26119.7 (3)
C34—N12—N11109.1 (3)C28—C27—C26119.1 (3)
C34—N12—C36129.1 (3)C33—C28—C29118.7 (4)
N11—N12—C36121.7 (3)C33—C28—C27118.6 (3)
N14—N13—Cd2i124.6 (2)C29—C28—C27122.7 (3)
N15—N14—N13175.5 (3)C28—C29—C30119.9 (4)
N14—N15—Cd1131.1 (2)C28—C29—H29120.1
N17—N16—Cd1122.6 (2)C30—C29—H29120.1
N16—N17—N18178.1 (4)C31—C30—C29120.7 (4)
N17—N18—Cd2115.8 (2)C31—C30—H30119.7
N20—N19—Cd1126.8 (2)C29—C30—H30119.7
N21—N20—N19175.7 (3)C30—C31—C32119.9 (4)
N20—N21—Cd2129.5 (2)C30—C31—H31120.0
N23—N22—Cd2124.2 (2)C32—C31—H31120.0
N22—N23—N24178.4 (4)C31—C32—C33120.0 (5)
N23—N24—Cd1ii116.1 (2)C31—C32—H32120.0
N3—C1—N1110.9 (3)C33—C32—H32120.0
N3—C1—H1124.6C32—C33—C28120.7 (4)
N1—C1—H1124.6C32—C33—H33119.6
N2—C2—N1114.6 (3)C28—C33—H33119.6
N2—C2—H2122.7N12—C34—N10111.3 (3)
N1—C2—H2122.7N12—C34—H34124.3
N3—C3—C4112.9 (3)N10—C34—H34124.3
N3—C3—H3A109.0N11—C35—N10114.9 (3)
C4—C3—H3A109.0N11—C35—H35122.6
N3—C3—H3B109.0N10—C35—H35122.6
C4—C3—H3B109.0N12—C36—C37113.8 (3)
H3A—C3—H3B107.8N12—C36—H36A108.8
C5—C4—C3113.8 (3)C37—C36—H36A108.8
C5—C4—H4A108.8N12—C36—H36B108.8
C3—C4—H4A108.8C37—C36—H36B108.8
C5—C4—H4B108.8H36A—C36—H36B107.7
C3—C4—H4B108.8C38—C37—C36113.7 (3)
H4A—C4—H4B107.7C38—C37—H37A108.8
O1—C5—C6121.4 (3)C36—C37—H37A108.8
O1—C5—C4120.2 (3)C38—C37—H37B108.8
C6—C5—C4118.5 (3)C36—C37—H37B108.8
C7—C6—C11118.7 (3)H37A—C37—H37B107.7
C7—C6—C5122.5 (3)O3—C38—C39120.8 (3)
C11—C6—C5118.8 (3)O3—C38—C37120.3 (3)
C6—C7—C8120.2 (4)C39—C38—C37118.9 (3)
C6—C7—H7119.9C44—C39—C40118.7 (3)
C8—C7—H7119.9C44—C39—C38122.4 (3)
C9—C8—C7120.2 (4)C40—C39—C38118.9 (3)
C9—C8—H8119.9C41—C40—C39120.4 (4)
C7—C8—H8119.9C41—C40—H40119.8
C8—C9—C10120.7 (4)C39—C40—H40119.8
C8—C9—H9119.6C42—C41—C40120.3 (4)
C10—C9—H9119.6C42—C41—H41119.8
C9—C10—C11119.5 (4)C40—C41—H41119.8
C9—C10—H10120.3C41—C42—C43120.2 (4)
C11—C10—H10120.3C41—C42—H42119.9
C6—C11—C10120.6 (4)C43—C42—H42119.9
C6—C11—H11119.7C42—C43—C44120.2 (4)
C10—C11—H11119.7C42—C43—H43119.9
N5—C12—N4114.2 (3)C44—C43—H43119.9
N5—C12—H12122.9C39—C44—C43120.2 (4)
N4—C12—H12122.9C39—C44—H44119.9
N4—C13—N6110.7 (3)C43—C44—H44119.9
N19—Cd1—N1—C1−110.3 (3)C1—N1—C2—N20.3 (4)
N24i—Cd1—N1—C1−47.7 (8)Cd1—N1—C2—N2−175.3 (3)
N15—Cd1—N1—C1−12.2 (3)C1—N3—C3—C4120.8 (4)
N4—Cd1—N1—C173.0 (3)N2—N3—C3—C4−61.7 (4)
N16—Cd1—N1—C1159.7 (3)N3—C3—C4—C5−72.4 (4)
N19—Cd1—N1—C264.4 (3)C3—C4—C5—O14.5 (5)
N24i—Cd1—N1—C2127.0 (7)C3—C4—C5—C6−174.6 (3)
N15—Cd1—N1—C2162.5 (3)O1—C5—C6—C7−177.7 (4)
N4—Cd1—N1—C2−112.3 (3)C4—C5—C6—C71.4 (5)
N16—Cd1—N1—C2−25.6 (3)O1—C5—C6—C110.5 (5)
C2—N2—N3—C10.2 (4)C4—C5—C6—C11179.6 (3)
C2—N2—N3—C3−177.7 (3)C11—C6—C7—C80.3 (6)
N19—Cd1—N4—C1315.4 (12)C5—C6—C7—C8178.5 (4)
N24i—Cd1—N4—C13−134.7 (3)C6—C7—C8—C9−0.9 (7)
N1—Cd1—N4—C1352.1 (3)C7—C8—C9—C101.3 (8)
N15—Cd1—N4—C13136.5 (3)C8—C9—C10—C11−1.1 (8)
N16—Cd1—N4—C13−38.6 (3)C7—C6—C11—C10−0.1 (6)
N19—Cd1—N4—C12−137.3 (10)C5—C6—C11—C10−178.3 (4)
N24i—Cd1—N4—C1272.6 (3)C9—C10—C11—C60.5 (7)
N1—Cd1—N4—C12−100.6 (3)N6—N5—C12—N4−0.2 (4)
N15—Cd1—N4—C12−16.2 (3)C13—N4—C12—N5−0.1 (4)
N16—Cd1—N4—C12168.7 (3)Cd1—N4—C12—N5156.3 (3)
C12—N5—N6—C130.4 (4)C12—N4—C13—N60.3 (4)
C12—N5—N6—C14−173.4 (3)Cd1—N4—C13—N6−158.8 (2)
N13ii—Cd2—N7—C24−2.9 (12)N5—N6—C13—N4−0.5 (4)
N21—Cd2—N7—C24−136.3 (3)C14—N6—C13—N4172.7 (3)
N18—Cd2—N7—C24133.9 (2)C13—N6—C14—C15126.3 (3)
N10—Cd2—N7—C24−51.6 (2)N5—N6—C14—C15−61.2 (4)
N22—Cd2—N7—C2439.0 (2)N6—C14—C15—C16−72.9 (4)
N13ii—Cd2—N7—C23147.6 (9)C14—C15—C16—O23.5 (5)
N21—Cd2—N7—C2314.2 (3)C14—C15—C16—C17−176.7 (3)
N18—Cd2—N7—C23−75.5 (3)O2—C16—C17—C185.0 (5)
N10—Cd2—N7—C2399.0 (3)C15—C16—C17—C18−174.8 (3)
N22—Cd2—N7—C23−170.5 (3)O2—C16—C17—C22−174.8 (4)
C23—N8—N9—C24−0.4 (4)C15—C16—C17—C225.4 (5)
C23—N8—N9—C25172.9 (3)C22—C17—C18—C19−0.7 (6)
N13ii—Cd2—N10—C34112.7 (3)C16—C17—C18—C19179.5 (3)
N21—Cd2—N10—C3414.0 (3)C17—C18—C19—C200.5 (6)
N18—Cd2—N10—C3450.3 (10)C18—C19—C20—C210.4 (7)
N7—Cd2—N10—C34−71.7 (3)C19—C20—C21—C22−1.1 (7)
N22—Cd2—N10—C34−157.5 (3)C18—C17—C22—C210.1 (6)
N13ii—Cd2—N10—C35−63.6 (3)C16—C17—C22—C21179.9 (3)
N21—Cd2—N10—C35−162.3 (3)C20—C21—C22—C170.8 (6)
N18—Cd2—N10—C35−126.0 (8)N9—N8—C23—N70.2 (4)
N7—Cd2—N10—C35112.0 (3)C24—N7—C23—N80.1 (4)
N22—Cd2—N10—C3526.2 (3)Cd2—N7—C23—N8−154.1 (3)
C35—N11—N12—C34−0.2 (4)N8—N9—C24—N70.5 (4)
C35—N11—N12—C36177.0 (3)C25—N9—C24—N7−172.2 (3)
Cd2i—N13—N14—N15173 (4)C23—N7—C24—N9−0.4 (4)
N13—N14—N15—Cd1149 (4)Cd2—N7—C24—N9157.7 (2)
N19—Cd1—N15—N14−90.0 (3)C24—N9—C25—C26−131.6 (3)
N24i—Cd1—N15—N140.2 (3)N8—N9—C25—C2656.5 (4)
N1—Cd1—N15—N14−175.2 (3)N9—C25—C26—C2775.4 (4)
N4—Cd1—N15—N1494.9 (3)C25—C26—C27—O4−8.1 (5)
N16—Cd1—N15—N14125.5 (6)C25—C26—C27—C28170.8 (3)
N19—Cd1—N16—N17−36.4 (3)O4—C27—C28—C33−5.6 (5)
N24i—Cd1—N16—N17−126.7 (3)C26—C27—C28—C33175.5 (3)
N1—Cd1—N16—N1749.6 (3)O4—C27—C28—C29172.6 (4)
N15—Cd1—N16—N17108.5 (6)C26—C27—C28—C29−6.3 (5)
N4—Cd1—N16—N17139.1 (3)C33—C28—C29—C30−0.1 (6)
Cd1—N16—N17—N18−116 (12)C27—C28—C29—C30−178.3 (4)
N16—N17—N18—Cd2−161 (11)C28—C29—C30—C31−0.2 (7)
N13ii—Cd2—N18—N17−145.7 (3)C29—C30—C31—C320.5 (7)
N21—Cd2—N18—N17−47.4 (3)C30—C31—C32—C33−0.4 (8)
N7—Cd2—N18—N1738.3 (3)C31—C32—C33—C280.1 (7)
N10—Cd2—N18—N17−83.5 (9)C29—C28—C33—C320.2 (6)
N22—Cd2—N18—N17124.4 (3)C27—C28—C33—C32178.5 (4)
N24i—Cd1—N19—N2084.1 (4)N11—N12—C34—N100.6 (4)
N1—Cd1—N19—N20−103.0 (4)C36—N12—C34—N10−176.3 (3)
N15—Cd1—N19—N20173.2 (3)C35—N10—C34—N12−0.7 (4)
N4—Cd1—N19—N20−66.1 (12)Cd2—N10—C34—N12−177.9 (2)
N16—Cd1—N19—N20−12.2 (4)N12—N11—C35—N10−0.3 (4)
Cd1—N19—N20—N21179 (100)C34—N10—C35—N110.6 (4)
N19—N20—N21—Cd2−145 (5)Cd2—N10—C35—N11177.5 (2)
N13ii—Cd2—N21—N2094.3 (3)C34—N12—C36—C37−124.4 (4)
N18—Cd2—N21—N203.5 (3)N11—N12—C36—C3759.1 (4)
N7—Cd2—N21—N20−90.0 (3)N12—C36—C37—C3872.5 (4)
N10—Cd2—N21—N20179.6 (3)C36—C37—C38—O3−5.9 (5)
N22—Cd2—N21—N20−119.0 (6)C36—C37—C38—C39174.0 (3)
N13ii—Cd2—N22—N2336.0 (3)O3—C38—C39—C44174.2 (4)
N21—Cd2—N22—N23−111.2 (6)C37—C38—C39—C44−5.8 (5)
N18—Cd2—N22—N23126.8 (3)O3—C38—C39—C40−4.6 (5)
N7—Cd2—N22—N23−140.1 (3)C37—C38—C39—C40175.4 (3)
N10—Cd2—N22—N23−50.2 (3)C44—C39—C40—C410.4 (6)
Cd2—N22—N23—N24115 (14)C38—C39—C40—C41179.2 (3)
N22—N23—N24—Cd1ii162 (100)C39—C40—C41—C42−0.1 (6)
N2—N3—C1—N10.0 (4)C40—C41—C42—C43−0.3 (7)
C3—N3—C1—N1177.7 (3)C41—C42—C43—C440.4 (7)
C2—N1—C1—N3−0.1 (4)C40—C39—C44—C43−0.3 (5)
Cd1—N1—C1—N3175.9 (2)C38—C39—C44—C43−179.1 (3)
N3—N2—C2—N1−0.3 (5)C42—C43—C44—C39−0.1 (6)

Symmetry codes: (i) x−1, y, z; (ii) x+1, y, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BV2096).

References

  • Bruker (2001). SMART and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Guo, J.-H. & Cai, H. (2007). Acta Cryst. E63, m1322–m1324.
  • Sheldrick, G. M. (2004). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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