Download citation
Download citation
link to html
The asymmetric unit of the title complex, [Dy(C26H34N6O2)(NO3)2]NO3·H2O, comprises two cations and two anions, together with two water mol­ecules. The Dy atom exhibits a nine-coordinate distorted tricapped trigonal-prismatic coordination geometry. The water mol­ecules are disordered over five positions, each with a site-occupation factor of 0.4. The crystal structure involves N—H...O and N—H...N hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680702795X/bi2193sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680702795X/bi2193Isup2.hkl
Contains datablock I

CCDC reference: 654766

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](C-C) = 0.008 Å
  • Disorder in solvent or counterion
  • R factor = 0.051
  • wR factor = 0.115
  • Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 300 Deg. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 15.00 Perc.
Alert level G PLAT793_ALERT_1_G Check the Absolute Configuration of C18 = ... R PLAT793_ALERT_1_G Check the Absolute Configuration of C44 = ... R
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

Lanthanide macrocyclic complexes have received much attention due to their unique properties and many valuable applications such as fluorescent probes in biological systems, material science and chemical processes (Bunzli & Piguet, 2002). Generally, the syntheses of lanthanide macrocyclic complexes are carried out in the presence of a suitable lanthanide ion which acts as a template for macrocycle formation, Most of them are symmetric (Hu et al., 2005). There have been few reports of asymmetric lanthanide complexes.

Recently, Hu et al. (Hu, Qiu et al., 2007; Hu, Chen et al., 2007) have reported the crystal structures of GdIII and LuIII complexes with a macrocyclic ligand derived from 2,6-diformyl-4-methylphenol and 1,5-diamino-3-azapentane: [Gd(C26H34N6O2)(NO3)2]+(NO3)-.H2O and [Lu(C26H34N6O2)(NO3)2]+(NO3)-.0.5H2O.0.25CH3COOC2H5. In these complexes, the central lanthanide ion is nine-coordinate, being bound to five donor atoms from the cyclic polydentate ligand and to four O of two bidentate nitrate anions. Reported here is a new DyIII analogue [Dy(III)(C26H34N6O2)(NO3)2]+(NO3)-.H2O, which exhibits a similar nine-coordinate distorted tricapped trigonal prismatic coordination geometry (Fig. 1 & Fig. 2). The title complex is not isostructural with its GdIII and LuIII analogues. (space groups Cc and C2/c, respectively).

Related literature top

For a general discussion of macrocyclic lanthanide complexes, see Bunzli & Piguet (2002). Some examples of symmetric macrocyclic lanthanide complexes are given in Hu et al. (2005). The GdIII and LuIII analogues of the title complex have been reported recently (Hu, Qiu et al., 2007; Hu, Chen et al., 2007).

Experimental top

To a methanolic solution (20 ml) of 2,6-diformyl-4-methylphenol (1 mmol) and Dy(NO3)3.6H2O (0.5 mmol), 1,5-diamino-3-azapentane (1 mmol) was added dropwise. After refluxing for 3 h, the solvent was removed. The resulting yellow solid was recrystallized from CH3CN, yielding yellow block crystals suitable for X-ray analysis.

Refinement top

H atoms bound to C atoms were placed geometrically (C—H 0.93 to 0.97 Å) and were allowed to ride during refinement with Uiso(H) = 1.2Ueq(C). H atoms bound to N atoms were visible in difference Fourier maps, but were placed geometrically with N—H = 0.90 or 0.91 Å for N(sp3) and 0.86 Å for N(sp2), and allowed to ride during refinement with Uiso(H) = 1.2Ueq(N). H atoms of the water molecules were located in difference Fourier maps, then their O—H distances were normalized to 0.85 Å and they were refined as riding with Uiso(H) = 1.2Ueq(O).

Structure description top

Lanthanide macrocyclic complexes have received much attention due to their unique properties and many valuable applications such as fluorescent probes in biological systems, material science and chemical processes (Bunzli & Piguet, 2002). Generally, the syntheses of lanthanide macrocyclic complexes are carried out in the presence of a suitable lanthanide ion which acts as a template for macrocycle formation, Most of them are symmetric (Hu et al., 2005). There have been few reports of asymmetric lanthanide complexes.

Recently, Hu et al. (Hu, Qiu et al., 2007; Hu, Chen et al., 2007) have reported the crystal structures of GdIII and LuIII complexes with a macrocyclic ligand derived from 2,6-diformyl-4-methylphenol and 1,5-diamino-3-azapentane: [Gd(C26H34N6O2)(NO3)2]+(NO3)-.H2O and [Lu(C26H34N6O2)(NO3)2]+(NO3)-.0.5H2O.0.25CH3COOC2H5. In these complexes, the central lanthanide ion is nine-coordinate, being bound to five donor atoms from the cyclic polydentate ligand and to four O of two bidentate nitrate anions. Reported here is a new DyIII analogue [Dy(III)(C26H34N6O2)(NO3)2]+(NO3)-.H2O, which exhibits a similar nine-coordinate distorted tricapped trigonal prismatic coordination geometry (Fig. 1 & Fig. 2). The title complex is not isostructural with its GdIII and LuIII analogues. (space groups Cc and C2/c, respectively).

For a general discussion of macrocyclic lanthanide complexes, see Bunzli & Piguet (2002). Some examples of symmetric macrocyclic lanthanide complexes are given in Hu et al. (2005). The GdIII and LuIII analogues of the title complex have been reported recently (Hu, Qiu et al., 2007; Hu, Chen et al., 2007).

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title complex showing displacement ellipsoids at the 30% probability level. H atoms are omitted.
[Figure 2] Fig. 2. Distorted tricapped trigonal prismatic coordination environment of DyIII.
(13,27-Dimethyl-3,6,9,17,20,23-hexaazatricyclo[23.3.1.111,15]triaconta- 1(29),2,9,11,13,15 (30),16,23,25,27-decaene-29,30-diol- κ5N3,N6,N9,O29,O30)bis(nitrato-κ2O,O')dysprosium(III) nitrate monohydrate top
Crystal data top
[Dy(C26H34N6O2)(NO3)2]NO3·H2OZ = 4
Mr = 829.14F(000) = 1668
Triclinic, P1Dx = 1.504 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 14.005 (3) ÅCell parameters from 6195 reflections
b = 14.045 (3) Åθ = 2.5–22.7°
c = 21.896 (4) ŵ = 2.11 mm1
α = 96.386 (3)°T = 292 K
β = 99.094 (3)°Block, yellow
γ = 118.217 (3)°0.30 × 0.22 × 0.20 mm
V = 3661.0 (13) Å3
Data collection top
Bruker SMART CCD
diffractometer
14395 independent reflections
Radiation source: sealed tube10889 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
φ and ω scansθmax = 26.0°, θmin = 1.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1717
Tmin = 0.58, Tmax = 0.66k = 1717
36705 measured reflectionsl = 2727
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: full with fixed elements per cycleSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.06P)2]
where P = (Fo2 + 2Fc2)/3
14395 reflections(Δ/σ)max < 0.001
872 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = 1.42 e Å3
Crystal data top
[Dy(C26H34N6O2)(NO3)2]NO3·H2Oγ = 118.217 (3)°
Mr = 829.14V = 3661.0 (13) Å3
Triclinic, P1Z = 4
a = 14.005 (3) ÅMo Kα radiation
b = 14.045 (3) ŵ = 2.11 mm1
c = 21.896 (4) ÅT = 292 K
α = 96.386 (3)°0.30 × 0.22 × 0.20 mm
β = 99.094 (3)°
Data collection top
Bruker SMART CCD
diffractometer
14395 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
10889 reflections with I > 2σ(I)
Tmin = 0.58, Tmax = 0.66Rint = 0.042
36705 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0510 restraints
wR(F2) = 0.115H-atom parameters constrained
S = 1.04Δρmax = 0.45 e Å3
14395 reflectionsΔρmin = 1.42 e Å3
872 parameters
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)
C10.47785 (19)0.8435 (3)0.33060 (16)0.0424 (11)
C20.3861 (3)0.7491 (2)0.33767 (16)0.0457 (11)
C30.2811 (2)0.7395 (2)0.32526 (17)0.0501 (12)
H30.21970.67630.33000.060*
C40.2679 (2)0.8243 (3)0.30578 (16)0.0487 (12)
C50.3597 (3)0.9188 (2)0.29872 (17)0.0518 (12)
H50.35090.97550.28570.062*
C60.4647 (2)0.9284 (2)0.31113 (17)0.0626 (15)
C70.3928 (4)0.6602 (4)0.3563 (2)0.0423 (11)
H70.32670.59880.35800.051*
C80.1511 (5)0.8098 (5)0.2895 (3)0.0620 (15)
H8A0.14690.86250.31920.093*
H8B0.09720.73630.29150.093*
H8C0.13570.82140.24750.093*
C90.5574 (5)1.0360 (5)0.3046 (3)0.0622 (14)
H90.53921.09010.29700.075*
C100.8457 (3)0.7694 (3)0.34372 (15)0.0533 (13)
C110.9485 (3)0.83720 (19)0.38639 (15)0.0465 (11)
C121.0079 (2)0.7912 (2)0.41481 (14)0.0528 (13)
H121.07670.83650.44340.063*
C130.9645 (3)0.6774 (2)0.40058 (15)0.0461 (11)
C140.8618 (3)0.60959 (19)0.35791 (16)0.0528 (13)
H140.83270.53340.34840.063*
C150.8024 (2)0.6556 (2)0.32948 (14)0.0560 (13)
C161.0050 (5)0.9589 (5)0.4031 (2)0.0616 (15)
H161.07940.99560.42540.074*
C171.0299 (4)0.6233 (5)0.4289 (2)0.0531 (13)
H17A1.06930.61170.39940.080*
H17B0.97880.55360.43710.080*
H17C1.08230.67110.46770.080*
C180.6876 (5)0.5791 (5)0.2826 (2)0.0580 (14)
H180.67390.50320.27300.070*
C190.4863 (4)0.5560 (4)0.3875 (3)0.0500 (12)
H19A0.41480.49120.36680.060*
H19B0.49630.56110.43280.060*
C200.5788 (5)0.5432 (5)0.3666 (3)0.0619 (15)
H20A0.64770.58630.39920.074*
H20B0.55950.46620.36040.074*
C210.4973 (4)0.5106 (5)0.2517 (3)0.0616 (16)
H21A0.43370.52000.25470.074*
H21B0.47510.43300.24760.074*
C220.5480 (4)0.5575 (4)0.1967 (2)0.0515 (13)
H22A0.52540.60910.18370.062*
H22B0.52550.49860.16050.062*
C231.0414 (4)1.1413 (5)0.4118 (3)0.0549 (14)
H23A1.09111.15670.45240.066*
H23B1.08651.16750.38160.066*
C240.9790 (4)1.1999 (4)0.4176 (2)0.0549 (14)
H24A1.02941.27910.42530.066*
H24B0.94461.18420.45310.066*
C250.8306 (4)1.2242 (5)0.3592 (2)0.0531 (13)
H25A0.88001.30120.35920.064*
H25B0.80291.22120.39730.064*
C260.7338 (5)1.1730 (5)0.3014 (3)0.0654 (15)
H26A0.69691.21650.29900.078*
H26B0.75991.16960.26320.078*
C270.2983 (4)0.1020 (4)0.1215 (2)0.0450 (11)
C280.3961 (4)0.1080 (5)0.1358 (2)0.0473 (12)
C290.3941 (4)0.2033 (4)0.1516 (2)0.0446 (11)
H290.46030.20490.16120.054*
C300.2948 (4)0.2947 (4)0.1532 (2)0.0450 (11)
C310.1949 (5)0.2905 (5)0.1391 (3)0.0565 (13)
H310.12780.35080.14050.068*
C320.1965 (5)0.1951 (4)0.1228 (3)0.0531 (12)
C330.5050 (4)0.0196 (5)0.1327 (2)0.0498 (12)
H330.56240.03600.13790.060*
C340.2921 (5)0.3957 (5)0.1720 (3)0.0557 (13)
H34A0.29480.44040.13660.084*
H34B0.22460.43770.18520.084*
H34C0.35530.37340.20640.084*
C350.0938 (4)0.2017 (4)0.1077 (2)0.0420 (11)
H350.03140.26540.11090.050*
C360.2392 (4)0.2650 (4)0.1082 (3)0.0543 (13)
C370.2605 (4)0.3269 (4)0.0600 (2)0.0492 (12)
C380.1853 (4)0.3658 (4)0.0384 (3)0.0514 (13)
H380.19950.40790.00760.062*
C390.0952 (5)0.3430 (4)0.0615 (3)0.0572 (15)
C400.0692 (5)0.2750 (4)0.1055 (2)0.0539 (13)
H400.00340.25400.11870.065*
C410.1393 (4)0.2397 (4)0.1287 (2)0.0433 (11)
C420.3492 (4)0.3483 (4)0.0306 (2)0.0421 (10)
H42A0.35680.39140.00040.050*
C430.0218 (4)0.3921 (4)0.0331 (2)0.0550 (14)
H43A0.04790.46410.05820.083*
H43B0.05470.34420.03330.083*
H43C0.02740.39790.00970.083*
C440.1037 (5)0.1637 (4)0.1756 (3)0.0586 (14)
H440.04030.16280.18970.070*
C450.1679 (4)0.0949 (5)0.2612 (2)0.0517 (12)
H45A0.22760.07750.26760.062*
H45B0.14780.10330.30110.062*
C460.0712 (4)0.0098 (5)0.2122 (2)0.0463 (11)
H46A0.07270.05890.20580.056*
H46B0.00210.00400.22320.056*
C470.0090 (4)0.0068 (4)0.1010 (3)0.0521 (13)
H47A0.00660.03080.06620.062*
H47B0.07620.01100.11030.062*
C480.0293 (4)0.1248 (4)0.0808 (2)0.0458 (11)
H48A0.07340.17190.10650.055*
H48B0.07050.15520.03690.055*
C490.6479 (4)0.1487 (4)0.1208 (2)0.0435 (11)
H49A0.68550.10590.11960.052*
H49B0.68740.20860.15800.052*
C500.6474 (4)0.1958 (4)0.0607 (2)0.0470 (11)
H50A0.72350.24430.05840.056*
H50B0.61160.13580.02360.056*
C510.5600 (4)0.2838 (5)0.0015 (2)0.0520 (13)
H51A0.50520.21630.03180.062*
H51B0.62650.31840.01750.062*
C520.5134 (4)0.3620 (4)0.0067 (2)0.0483 (12)
H52A0.57220.43420.03100.058*
H52B0.48500.37070.03440.058*
Dy10.75925 (2)0.95316 (2)0.336610 (11)0.05113 (8)
Dy20.407500 (18)0.16379 (2)0.100570 (12)0.04739 (8)
N10.4865 (4)0.6566 (4)0.3717 (2)0.0529 (11)
H1A0.54900.71380.37250.063*
N20.6562 (4)1.0606 (4)0.3082 (2)0.0573 (12)
N30.8918 (4)1.1639 (3)0.3585 (2)0.0463 (10)
H3A0.92671.17850.32620.056*
N40.9631 (4)1.0184 (4)0.3904 (2)0.0538 (11)
N50.6776 (4)0.6179 (4)0.2258 (2)0.0601 (12)
H5A0.71210.59970.19920.072*
H5B0.70720.69180.23420.072*
N60.5944 (3)0.5815 (4)0.3070 (2)0.0537 (11)
N70.7380 (4)0.9146 (4)0.1990 (2)0.0596 (12)
N80.7392 (4)0.9437 (4)0.4685 (2)0.0592 (13)
N90.5318 (4)0.0781 (4)0.1236 (2)0.0586 (12)
N100.0796 (3)0.1221 (4)0.0888 (2)0.0480 (10)
H10A0.13530.06690.08100.058*
N110.0828 (3)0.0565 (3)0.15591 (19)0.0438 (9)
N120.2046 (4)0.2077 (4)0.2318 (2)0.0575 (12)
H12A0.21150.26410.25970.069*
H12B0.26860.22910.21920.069*
N130.4212 (4)0.3152 (4)0.0404 (2)0.0567 (12)
N140.5880 (3)0.2569 (3)0.06133 (18)0.0430 (9)
H14A0.63450.32270.08910.052*
N150.5202 (4)0.2597 (3)0.2372 (2)0.0504 (11)
N160.2567 (3)0.0129 (3)0.01617 (18)0.0423 (9)
N170.1430 (4)0.3787 (3)0.3121 (2)0.0550 (12)
N180.8148 (4)0.5559 (4)0.1309 (2)0.0554 (11)
O10.5778 (3)0.8473 (3)0.33876 (17)0.0556 (9)
O20.7896 (3)0.8106 (3)0.31100 (18)0.0645 (11)
O30.6560 (3)0.8534 (3)0.22214 (19)0.0638 (11)
O40.8157 (3)0.9962 (3)0.23469 (16)0.0511 (9)
O50.7318 (3)0.8909 (3)0.14592 (18)0.0582 (10)
O60.7480 (3)0.8677 (3)0.43658 (16)0.0534 (9)
O70.7562 (3)1.0260 (3)0.44466 (17)0.0566 (10)
O80.7203 (3)0.9337 (3)0.52032 (18)0.0593 (10)
O90.2978 (3)0.0141 (3)0.10996 (16)0.0466 (8)
O100.3063 (3)0.2363 (3)0.13515 (16)0.0457 (8)
O110.4298 (3)0.1682 (3)0.21994 (16)0.0539 (9)
O120.5602 (3)0.3048 (3)0.19477 (16)0.0469 (8)
O130.5665 (3)0.3021 (3)0.29462 (19)0.0620 (10)
O140.3596 (2)0.0465 (3)0.00753 (15)0.0410 (7)
O150.2248 (3)0.0671 (3)0.01518 (15)0.0483 (8)
O160.1887 (3)0.0741 (3)0.05426 (17)0.0627 (11)
O170.0664 (3)0.2836 (3)0.28828 (18)0.0665 (12)
O180.2305 (3)0.4028 (3)0.29827 (19)0.0637 (11)
O190.1357 (3)0.4538 (3)0.34430 (18)0.0616 (10)
O200.7317 (3)0.5001 (3)0.13864 (19)0.0686 (12)
O210.8556 (4)0.6503 (4)0.15550 (19)0.0661 (11)
O220.8672 (3)0.5325 (4)0.09746 (18)0.0649 (11)
O230.9291 (9)0.4352 (9)0.2281 (5)0.071 (3)0.40
H23D0.94090.40810.25930.085*0.40
H23E0.89110.38360.19530.085*0.40
O240.2786 (8)0.5461 (8)0.5132 (4)0.058 (2)0.40
H24C0.25830.49910.53660.069*0.40
H24E0.22170.53580.48660.069*0.40
O250.6348 (8)0.7333 (8)0.5865 (4)0.065 (3)0.40
H25D0.65970.68940.59200.078*0.40
H25E0.66460.77130.56030.078*0.40
O260.4610 (10)0.8251 (10)0.5315 (6)0.087 (4)0.40
H26E0.51630.81740.54600.105*0.40
H26D0.47350.85360.49930.105*0.40
O270.3462 (10)0.6915 (12)0.5223 (5)0.097 (5)0.40
H27C0.33880.66550.55560.117*0.40
H27A0.28930.69670.50760.117*0.40
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.039 (2)0.056 (3)0.043 (2)0.033 (2)0.0094 (19)0.007 (2)
C20.036 (2)0.037 (3)0.072 (3)0.024 (2)0.012 (2)0.013 (2)
C30.041 (3)0.052 (3)0.050 (3)0.017 (2)0.016 (2)0.008 (2)
C40.040 (3)0.047 (3)0.061 (3)0.021 (2)0.016 (2)0.016 (2)
C50.051 (3)0.054 (3)0.052 (3)0.027 (3)0.014 (2)0.008 (2)
C60.060 (3)0.065 (4)0.048 (3)0.019 (3)0.018 (3)0.009 (3)
C70.040 (2)0.032 (2)0.038 (2)0.009 (2)0.0065 (18)0.0072 (18)
C80.064 (4)0.055 (3)0.058 (3)0.021 (3)0.019 (3)0.012 (3)
C90.051 (3)0.051 (3)0.076 (4)0.019 (3)0.014 (3)0.014 (3)
C100.050 (3)0.062 (3)0.031 (2)0.016 (3)0.009 (2)0.004 (2)
C110.040 (3)0.039 (3)0.052 (3)0.012 (2)0.013 (2)0.013 (2)
C120.056 (3)0.037 (3)0.041 (2)0.007 (2)0.005 (2)0.008 (2)
C130.041 (3)0.054 (3)0.044 (2)0.021 (2)0.016 (2)0.019 (2)
C140.053 (3)0.031 (3)0.061 (3)0.009 (2)0.017 (2)0.009 (2)
C150.056 (3)0.047 (3)0.053 (3)0.017 (3)0.013 (2)0.006 (2)
C160.056 (3)0.059 (4)0.045 (3)0.013 (3)0.006 (2)0.002 (2)
C170.044 (3)0.051 (3)0.047 (3)0.012 (2)0.006 (2)0.010 (2)
C180.051 (3)0.059 (3)0.044 (3)0.021 (3)0.000 (2)0.016 (2)
C190.041 (3)0.046 (3)0.055 (3)0.015 (2)0.009 (2)0.015 (2)
C200.042 (3)0.059 (4)0.066 (3)0.010 (3)0.019 (3)0.006 (3)
C210.038 (3)0.062 (4)0.056 (3)0.019 (3)0.016 (2)0.025 (3)
C220.043 (3)0.040 (3)0.047 (3)0.013 (2)0.013 (2)0.012 (2)
C230.030 (2)0.066 (4)0.051 (3)0.010 (2)0.013 (2)0.007 (3)
C240.048 (3)0.033 (3)0.055 (3)0.000 (2)0.006 (2)0.006 (2)
C250.045 (3)0.049 (3)0.050 (3)0.010 (2)0.010 (2)0.022 (2)
C260.061 (4)0.065 (4)0.067 (4)0.029 (3)0.014 (3)0.017 (3)
C270.048 (3)0.045 (3)0.033 (2)0.019 (2)0.0073 (19)0.0041 (19)
C280.045 (3)0.053 (3)0.039 (2)0.027 (2)0.004 (2)0.001 (2)
C290.037 (2)0.046 (3)0.045 (2)0.022 (2)0.0017 (19)0.007 (2)
C300.052 (3)0.039 (3)0.045 (2)0.030 (2)0.002 (2)0.001 (2)
C310.057 (3)0.042 (3)0.065 (3)0.020 (3)0.010 (3)0.022 (3)
C320.049 (3)0.041 (3)0.057 (3)0.017 (2)0.006 (2)0.003 (2)
C330.029 (2)0.062 (3)0.045 (3)0.019 (2)0.0042 (19)0.005 (2)
C340.047 (3)0.067 (4)0.054 (3)0.029 (3)0.011 (2)0.015 (3)
C350.030 (2)0.021 (2)0.060 (3)0.0082 (18)0.0037 (19)0.0158 (19)
C360.041 (3)0.039 (3)0.062 (3)0.008 (2)0.008 (2)0.001 (2)
C370.042 (3)0.040 (3)0.052 (3)0.016 (2)0.000 (2)0.005 (2)
C380.043 (3)0.032 (3)0.058 (3)0.014 (2)0.012 (2)0.012 (2)
C390.060 (3)0.033 (3)0.060 (3)0.025 (3)0.018 (3)0.021 (2)
C400.059 (3)0.036 (3)0.044 (3)0.018 (2)0.009 (2)0.019 (2)
C410.039 (2)0.040 (3)0.049 (3)0.022 (2)0.005 (2)0.006 (2)
C420.043 (3)0.034 (2)0.055 (3)0.023 (2)0.012 (2)0.009 (2)
C430.046 (3)0.042 (3)0.050 (3)0.014 (2)0.021 (2)0.010 (2)
C440.055 (3)0.035 (3)0.071 (4)0.011 (2)0.008 (3)0.020 (3)
C450.041 (3)0.049 (3)0.051 (3)0.012 (2)0.011 (2)0.009 (2)
C460.038 (2)0.054 (3)0.049 (3)0.021 (2)0.016 (2)0.019 (2)
C470.040 (3)0.043 (3)0.054 (3)0.014 (2)0.010 (2)0.001 (2)
C480.043 (3)0.038 (3)0.050 (3)0.017 (2)0.007 (2)0.005 (2)
C490.031 (2)0.040 (3)0.052 (3)0.008 (2)0.023 (2)0.005 (2)
C500.054 (3)0.030 (2)0.047 (3)0.013 (2)0.014 (2)0.006 (2)
C510.038 (3)0.056 (3)0.052 (3)0.015 (2)0.012 (2)0.010 (2)
C520.043 (3)0.045 (3)0.057 (3)0.017 (2)0.017 (2)0.031 (2)
Dy10.04810 (14)0.04859 (15)0.04748 (14)0.01280 (12)0.01949 (11)0.01889 (11)
Dy20.02832 (11)0.04888 (15)0.05916 (15)0.01496 (10)0.01314 (10)0.00690 (11)
N10.048 (2)0.037 (2)0.060 (3)0.008 (2)0.011 (2)0.027 (2)
N20.071 (3)0.052 (3)0.045 (2)0.019 (2)0.032 (2)0.027 (2)
N30.055 (3)0.036 (2)0.049 (2)0.020 (2)0.0164 (19)0.0164 (18)
N40.049 (3)0.053 (3)0.063 (3)0.025 (2)0.021 (2)0.014 (2)
N50.057 (3)0.053 (3)0.048 (2)0.019 (2)0.005 (2)0.009 (2)
N60.032 (2)0.057 (3)0.046 (2)0.011 (2)0.0042 (17)0.013 (2)
N70.057 (3)0.058 (3)0.048 (3)0.019 (3)0.010 (2)0.007 (2)
N80.053 (3)0.053 (3)0.046 (2)0.014 (2)0.005 (2)0.015 (2)
N90.043 (2)0.045 (3)0.066 (3)0.006 (2)0.010 (2)0.009 (2)
N100.038 (2)0.048 (3)0.057 (2)0.0151 (19)0.0163 (19)0.029 (2)
N110.035 (2)0.044 (2)0.049 (2)0.0150 (18)0.0192 (17)0.0096 (18)
N120.054 (3)0.051 (3)0.044 (2)0.016 (2)0.0008 (19)0.0120 (19)
N130.043 (2)0.050 (3)0.057 (3)0.009 (2)0.011 (2)0.008 (2)
N140.045 (2)0.037 (2)0.0387 (19)0.0139 (18)0.0148 (16)0.0022 (16)
N150.050 (3)0.034 (2)0.049 (2)0.016 (2)0.005 (2)0.0042 (19)
N160.040 (2)0.030 (2)0.045 (2)0.0095 (18)0.0063 (17)0.0066 (17)
N170.063 (3)0.024 (2)0.053 (2)0.002 (2)0.015 (2)0.0093 (18)
N180.055 (3)0.054 (3)0.049 (2)0.019 (3)0.015 (2)0.013 (2)
O10.056 (2)0.044 (2)0.053 (2)0.0139 (18)0.0120 (17)0.0167 (16)
O20.056 (2)0.058 (3)0.052 (2)0.016 (2)0.0029 (18)0.0034 (18)
O30.048 (2)0.052 (2)0.066 (2)0.0084 (19)0.0002 (18)0.0196 (19)
O40.048 (2)0.043 (2)0.0514 (19)0.0108 (17)0.0169 (16)0.0214 (17)
O50.056 (2)0.052 (2)0.051 (2)0.0130 (19)0.0194 (17)0.0093 (17)
O60.056 (2)0.045 (2)0.0489 (19)0.0133 (18)0.0217 (17)0.0146 (16)
O70.049 (2)0.047 (2)0.049 (2)0.0067 (18)0.0152 (16)0.0047 (17)
O80.046 (2)0.058 (2)0.060 (2)0.0141 (18)0.0161 (17)0.0123 (19)
O90.0417 (18)0.043 (2)0.0535 (19)0.0170 (16)0.0133 (15)0.0192 (16)
O100.051 (2)0.0321 (17)0.060 (2)0.0260 (16)0.0118 (16)0.0098 (15)
O110.064 (2)0.044 (2)0.0434 (18)0.0184 (19)0.0120 (16)0.0125 (15)
O120.0435 (19)0.044 (2)0.0459 (18)0.0181 (16)0.0133 (15)0.0010 (15)
O130.059 (2)0.040 (2)0.067 (2)0.0138 (19)0.0045 (19)0.0006 (18)
O140.0268 (15)0.0415 (18)0.0496 (17)0.0160 (14)0.0104 (13)0.0058 (14)
O150.0468 (19)0.045 (2)0.0423 (17)0.0196 (17)0.0039 (15)0.0036 (15)
O160.045 (2)0.059 (2)0.052 (2)0.0145 (19)0.0167 (17)0.0159 (18)
O170.059 (2)0.046 (2)0.053 (2)0.0071 (19)0.0226 (18)0.0012 (17)
O180.050 (2)0.059 (3)0.064 (2)0.018 (2)0.0196 (18)0.0154 (19)
O190.059 (2)0.053 (2)0.057 (2)0.017 (2)0.0195 (18)0.0032 (18)
O200.053 (2)0.052 (2)0.060 (2)0.001 (2)0.0174 (19)0.0151 (19)
O210.070 (3)0.056 (3)0.061 (2)0.020 (2)0.019 (2)0.020 (2)
O220.061 (2)0.065 (3)0.053 (2)0.019 (2)0.0144 (19)0.0162 (19)
O230.068 (7)0.054 (6)0.067 (6)0.019 (5)0.012 (5)0.021 (5)
O240.052 (5)0.054 (6)0.042 (4)0.008 (5)0.006 (4)0.016 (4)
O250.065 (6)0.054 (6)0.057 (5)0.022 (5)0.015 (5)0.024 (5)
O260.064 (7)0.077 (8)0.084 (8)0.007 (6)0.032 (6)0.005 (6)
O270.078 (8)0.112 (11)0.066 (7)0.046 (8)0.028 (6)0.046 (7)
Geometric parameters (Å, º) top
C1—O11.358 (4)C39—C431.576 (5)
C1—C21.390C40—C411.353 (6)
C1—C61.390C40—H400.930
C2—C31.390C41—C441.530 (8)
C2—C71.396 (6)C42—N131.296 (7)
C3—C41.390C42—H42A0.930
C3—H30.930C43—H43A0.960
C4—C51.390C43—H43B0.960
C4—C81.526 (6)C43—H43C0.960
C5—C61.390C44—N111.391 (7)
C5—H50.930C44—N121.533 (7)
C6—C91.498 (6)C44—H440.980
C7—N11.328 (5)C45—C461.463 (7)
C7—H70.930C45—N121.659 (7)
C8—H8A0.960C45—H45A0.970
C8—H8B0.960C45—H45B0.970
C8—H8C0.960C46—N111.455 (6)
C9—N21.244 (6)C46—H46A0.970
C9—H90.930C46—H46B0.970
C10—O21.346 (4)C47—N111.443 (6)
C10—C111.390C47—C481.541 (7)
C10—C151.390C47—H47A0.970
C11—C121.390C47—H47B0.970
C11—C161.474 (7)C48—N101.490 (6)
C12—C131.390C48—H48A0.970
C12—H120.930C48—H48B0.970
C13—C141.390C49—N91.467 (6)
C13—C171.542 (6)C49—C501.538 (7)
C14—C151.390C49—H49A0.970
C14—H140.930C49—H49B0.970
C15—C181.546 (5)C50—N141.451 (7)
C16—N41.259 (7)C50—H50A0.970
C16—H160.930C50—H50B0.970
C17—H17A0.960C51—N141.507 (6)
C17—H17B0.960C51—C521.528 (8)
C17—H17C0.960C51—H51A0.970
C18—N51.425 (6)C51—H51B0.970
C18—N61.501 (6)C52—N131.500 (6)
C18—H180.980C52—H52A0.970
C19—N11.490 (5)C52—H52B0.970
C19—C201.519 (8)Dy1—O22.265 (4)
C19—H19A0.970Dy1—O12.269 (4)
C19—H19B0.970Dy1—O72.486 (3)
C20—N61.475 (6)Dy1—O42.525 (3)
C20—H20A0.970Dy1—O32.548 (4)
C20—H20B0.970Dy1—N42.569 (5)
C21—N61.495 (5)Dy1—N32.578 (4)
C21—C221.548 (8)Dy1—N22.595 (5)
C21—H21A0.970Dy1—O62.602 (3)
C21—H21B0.970Dy2—O102.270 (3)
C22—N51.575 (5)Dy2—O92.287 (3)
C22—H22A0.970Dy2—O142.520 (3)
C22—H22B0.970Dy2—O122.538 (3)
C23—C241.467 (8)Dy2—O152.555 (3)
C23—N41.506 (6)Dy2—N92.564 (5)
C23—H23A0.970Dy2—N132.571 (5)
C23—H23B0.970Dy2—O112.573 (3)
C24—N31.480 (5)Dy2—N142.578 (4)
C24—H24A0.970N1—H1A0.860
C24—H24B0.970N3—H3A0.910
C25—N31.463 (6)N5—H5A0.900
C25—C261.513 (8)N5—H5B0.900
C25—H25A0.970N7—O51.151 (6)
C25—H25B0.970N7—O41.209 (6)
C26—N21.475 (6)N7—O31.288 (6)
C26—H26A0.970N8—O81.214 (6)
C26—H26B0.970N8—O71.257 (7)
C27—O91.291 (5)N8—O61.275 (6)
C27—C281.401 (7)N10—H10A0.860
C27—C321.415 (7)N12—H12A0.900
C28—C291.408 (7)N12—H12B0.900
C28—C331.460 (7)N14—H14A0.910
C29—C301.385 (7)N15—O121.240 (6)
C29—H290.930N15—O131.252 (5)
C30—C311.414 (7)N15—O111.265 (6)
C30—C341.507 (7)N16—O161.231 (5)
C31—C321.416 (8)N16—O151.246 (5)
C31—H310.930N16—O141.259 (5)
C32—C351.379 (7)N17—O181.206 (6)
C33—N91.289 (6)N17—O171.233 (5)
C33—H330.930N17—O191.257 (6)
C34—H34A0.960N18—O201.107 (6)
C34—H34B0.960N18—O211.185 (6)
C34—H34C0.960N18—O221.235 (6)
C35—N101.321 (5)O23—H23D0.850
C35—H350.930O23—H23E0.850
C36—O101.276 (6)O24—H24C0.850
C36—C371.421 (8)O24—H24E0.850
C36—C411.431 (6)O25—H25D0.850
C37—C421.411 (5)O25—H25E0.850
C37—C381.442 (7)O26—H26E0.850
C38—C391.343 (8)O26—H26D0.850
C38—H380.930O27—H27C0.850
C39—C401.400 (8)O27—H27A0.850
O1—C1—C2118.6 (2)N11—C47—H47B109.2
O1—C1—C6121.2 (2)C48—C47—H47B109.2
C2—C1—C6120.0H47A—C47—H47B107.9
C1—C2—C3120.0N10—C48—C47109.7 (4)
C1—C2—C7123.1 (3)N10—C48—H48A109.7
C3—C2—C7116.9 (3)C47—C48—H48A109.7
C4—C3—C2120.0N10—C48—H48B109.7
C4—C3—H3120.0C47—C48—H48B109.7
C2—C3—H3120.0H48A—C48—H48B108.2
C3—C4—C5120.0N9—C49—C50108.3 (4)
C3—C4—C8119.1 (3)N9—C49—H49A110.0
C5—C4—C8120.9 (3)C50—C49—H49A110.0
C6—C5—C4120.0N9—C49—H49B110.0
C6—C5—H5120.0C50—C49—H49B110.0
C4—C5—H5120.0H49A—C49—H49B108.4
C5—C6—C1120.0N14—C50—C49110.2 (4)
C5—C6—C9114.8 (3)N14—C50—H50A109.6
C1—C6—C9125.1 (3)C49—C50—H50A109.6
N1—C7—C2124.9 (4)N14—C50—H50B109.6
N1—C7—H7117.5C49—C50—H50B109.6
C2—C7—H7117.5H50A—C50—H50B108.1
C4—C8—H8A109.5N14—C51—C52109.6 (4)
C4—C8—H8B109.5N14—C51—H51A109.7
H8A—C8—H8B109.5C52—C51—H51A109.7
C4—C8—H8C109.5N14—C51—H51B109.7
H8A—C8—H8C109.5C52—C51—H51B109.7
H8B—C8—H8C109.5H51A—C51—H51B108.2
N2—C9—C6126.7 (5)N13—C52—C51109.2 (4)
N2—C9—H9116.7N13—C52—H52A109.8
C6—C9—H9116.7C51—C52—H52A109.8
O2—C10—C11122.2 (2)N13—C52—H52B109.8
O2—C10—C15117.6 (2)C51—C52—H52B109.8
C11—C10—C15120.0H52A—C52—H52B108.3
C12—C11—C10120.0O2—Dy1—O196.09 (15)
C12—C11—C16115.1 (3)O2—Dy1—O7124.77 (15)
C10—C11—C16124.9 (3)O1—Dy1—O777.37 (13)
C11—C12—C13120.0O2—Dy1—O482.30 (14)
C11—C12—H12120.0O1—Dy1—O4121.63 (12)
C13—C12—H12120.0O7—Dy1—O4147.27 (13)
C12—C13—C14120.0O2—Dy1—O370.77 (14)
C12—C13—C17121.7 (3)O1—Dy1—O374.58 (13)
C14—C13—C17118.3 (3)O7—Dy1—O3149.38 (13)
C15—C14—C13120.0O4—Dy1—O349.67 (12)
C15—C14—H14120.0O2—Dy1—N472.73 (14)
C13—C14—H14120.0O1—Dy1—N4145.61 (14)
C14—C15—C10120.0O7—Dy1—N482.75 (14)
C14—C15—C18119.4 (3)O4—Dy1—N489.71 (13)
C10—C15—C18120.6 (3)O3—Dy1—N4127.77 (14)
N4—C16—C11126.8 (5)O2—Dy1—N3130.87 (14)
N4—C16—H16116.6O1—Dy1—N3133.02 (14)
C11—C16—H16116.6O7—Dy1—N374.39 (13)
C13—C17—H17A109.5O4—Dy1—N373.54 (12)
C13—C17—H17B109.5O3—Dy1—N3117.53 (13)
H17A—C17—H17B109.5N4—Dy1—N365.19 (14)
C13—C17—H17C109.5O2—Dy1—N2149.91 (14)
H17A—C17—H17C109.5O1—Dy1—N271.76 (14)
H17B—C17—H17C109.5O7—Dy1—N280.41 (14)
N5—C18—N6100.7 (4)O4—Dy1—N281.32 (12)
N5—C18—C15112.2 (4)O3—Dy1—N279.39 (14)
N6—C18—C15111.9 (3)N4—Dy1—N2132.06 (15)
N5—C18—H18110.5N3—Dy1—N267.11 (14)
N6—C18—H18110.5O2—Dy1—O675.76 (14)
C15—C18—H18110.5O1—Dy1—O670.35 (12)
N1—C19—C20111.3 (4)O7—Dy1—O650.09 (13)
N1—C19—H19A109.4O4—Dy1—O6156.28 (13)
C20—C19—H19A109.4O3—Dy1—O6127.74 (12)
N1—C19—H19B109.4N4—Dy1—O675.35 (13)
C20—C19—H19B109.4N3—Dy1—O6114.73 (12)
H19A—C19—H19B108.0N2—Dy1—O6122.36 (12)
N6—C20—C19109.7 (5)O10—Dy2—O998.05 (12)
N6—C20—H20A109.7O10—Dy2—O14125.75 (11)
C19—C20—H20A109.7O9—Dy2—O1474.94 (12)
N6—C20—H20B109.7O10—Dy2—O1283.54 (12)
C19—C20—H20B109.7O9—Dy2—O12119.82 (12)
H20A—C20—H20B108.2O14—Dy2—O12147.03 (10)
N6—C21—C22100.6 (4)O10—Dy2—O1576.39 (12)
N6—C21—H21A111.7O9—Dy2—O1569.21 (12)
C22—C21—H21A111.7O14—Dy2—O1550.44 (10)
N6—C21—H21B111.7O12—Dy2—O15159.19 (11)
C22—C21—H21B111.7O10—Dy2—N9149.36 (14)
H21A—C21—H21B109.4O9—Dy2—N971.61 (13)
C21—C22—N5103.5 (3)O14—Dy2—N980.44 (13)
C21—C22—H22A111.1O12—Dy2—N977.60 (13)
N5—C22—H22A111.1O15—Dy2—N9122.92 (13)
C21—C22—H22B111.1O10—Dy2—N1371.20 (14)
N5—C22—H22B111.1O9—Dy2—N13145.54 (13)
H22A—C22—H22B109.0O14—Dy2—N1385.04 (13)
C24—C23—N4110.8 (4)O12—Dy2—N1392.10 (13)
C24—C23—H23A109.5O15—Dy2—N1376.39 (13)
N4—C23—H23A109.5N9—Dy2—N13132.80 (15)
C24—C23—H23B109.5O10—Dy2—O1172.68 (13)
N4—C23—H23B109.5O9—Dy2—O1173.55 (12)
H23A—C23—H23B108.1O14—Dy2—O11145.53 (12)
C23—C24—N3109.5 (4)O12—Dy2—O1149.39 (12)
C23—C24—H24A109.8O15—Dy2—O11126.79 (12)
N3—C24—H24A109.8N9—Dy2—O1176.71 (14)
C23—C24—H24B109.8N13—Dy2—O11129.33 (14)
N3—C24—H24B109.8O10—Dy2—N14129.84 (13)
H24A—C24—H24B108.2O9—Dy2—N14132.09 (13)
N3—C25—C26109.5 (4)O14—Dy2—N1475.68 (11)
N3—C25—H25A109.8O12—Dy2—N1473.20 (11)
C26—C25—H25A109.8O15—Dy2—N14116.04 (12)
N3—C25—H25B109.8N9—Dy2—N1466.83 (14)
C26—C25—H25B109.8N13—Dy2—N1466.10 (14)
H25A—C25—H25B108.2O11—Dy2—N14117.08 (12)
N2—C26—C25106.7 (4)C7—N1—C19121.9 (3)
N2—C26—H26A110.4C7—N1—H1A119.1
C25—C26—H26A110.4C19—N1—H1A119.0
N2—C26—H26B110.4C9—N2—C26117.1 (4)
C25—C26—H26B110.4C9—N2—Dy1130.9 (3)
H26A—C26—H26B108.6C26—N2—Dy1111.7 (3)
O9—C27—C28123.0 (4)C25—N3—C24112.7 (3)
O9—C27—C32118.8 (4)C25—N3—Dy1111.6 (2)
C28—C27—C32118.1 (5)C24—N3—Dy1110.0 (2)
C27—C28—C29121.3 (5)C25—N3—H3A107.4
C27—C28—C33123.0 (5)C24—N3—H3A107.4
C29—C28—C33115.7 (4)Dy1—N3—H3A107.4
C30—C29—C28121.0 (4)C16—N4—C23115.4 (3)
C30—C29—H29119.5C16—N4—Dy1127.2 (3)
C28—C29—H29119.5C23—N4—Dy1117.3 (2)
C29—C30—C31118.8 (5)C18—N5—C22104.1 (3)
C29—C30—C34121.4 (4)C18—N5—H5A110.9
C31—C30—C34119.8 (5)C22—N5—H5A110.9
C30—C31—C32120.4 (5)C18—N5—H5B110.9
C30—C31—H31119.8C22—N5—H5B110.9
C32—C31—H31119.8H5A—N5—H5B108.9
C35—C32—C27124.1 (5)C20—N6—C21113.7 (3)
C35—C32—C31115.5 (5)C20—N6—C18115.4 (3)
C27—C32—C31120.4 (5)C21—N6—C18101.1 (3)
N9—C33—C28128.5 (4)O5—N7—O4123.9 (5)
N9—C33—H33115.7O5—N7—O3118.9 (5)
C28—C33—H33115.7O4—N7—O3117.2 (4)
C30—C34—H34A109.5O8—N8—O7125.0 (5)
C30—C34—H34B109.5O8—N8—O6118.0 (5)
H34A—C34—H34B109.5O7—N8—O6116.8 (4)
C30—C34—H34C109.5C33—N9—C49116.4 (4)
H34A—C34—H34C109.5C33—N9—Dy2129.3 (3)
H34B—C34—H34C109.5C49—N9—Dy2114.2 (3)
N10—C35—C32123.4 (4)C35—N10—C48122.3 (4)
N10—C35—H35118.3C35—N10—H10A118.7
C32—C35—H35118.3C48—N10—H10A119.0
O10—C36—C37123.3 (5)C44—N11—C47113.7 (4)
O10—C36—C41119.8 (4)C44—N11—C46104.9 (4)
C37—C36—C41116.8 (5)C47—N11—C46115.4 (4)
C42—C37—C36123.2 (4)C44—N12—C4599.6 (4)
C42—C37—C38118.5 (5)C44—N12—H12A111.8
C36—C37—C38118.3 (5)C45—N12—H12A111.8
C39—C38—C37121.9 (6)C44—N12—H12B111.8
C39—C38—H38119.0C45—N12—H12B111.8
C37—C38—H38119.0H12A—N12—H12B109.6
C38—C39—C40119.9 (5)C42—N13—C52115.2 (5)
C38—C39—C43115.6 (5)C42—N13—Dy2126.2 (4)
C40—C39—C43124.4 (5)C52—N13—Dy2118.2 (3)
C41—C40—C39120.1 (5)C50—N14—C51114.0 (4)
C41—C40—H40119.9C50—N14—Dy2114.4 (3)
C39—C40—H40119.9C51—N14—Dy2108.1 (3)
C40—C41—C36122.7 (4)C50—N14—H14A106.6
C40—C41—C44116.9 (4)C51—N14—H14A106.6
C36—C41—C44120.3 (4)Dy2—N14—H14A106.6
N13—C42—C37127.9 (4)O12—N15—O13122.0 (4)
N13—C42—H42A116.1O12—N15—O11117.0 (4)
C37—C42—H42A116.1O13—N15—O11121.0 (5)
C39—C43—H43A109.5O16—N16—O15120.7 (4)
C39—C43—H43B109.5O16—N16—O14120.0 (4)
H43A—C43—H43B109.5O15—N16—O14119.4 (4)
C39—C43—H43C109.5O18—N17—O17115.5 (5)
H43A—C43—H43C109.5O18—N17—O19117.9 (4)
H43B—C43—H43C109.5O17—N17—O19126.3 (5)
N11—C44—C41116.3 (5)O20—N18—O21115.5 (5)
N11—C44—N12100.6 (4)O20—N18—O22128.0 (5)
C41—C44—N12107.4 (4)O21—N18—O22116.4 (5)
N11—C44—H44110.7C1—O1—Dy1143.9 (2)
C41—C44—H44110.7C10—O2—Dy1133.4 (2)
N12—C44—H44110.7N7—O3—Dy194.4 (3)
C46—C45—N12102.9 (4)N7—O4—Dy197.7 (3)
C46—C45—H45A111.2N8—O6—Dy193.0 (3)
N12—C45—H45A111.2N8—O7—Dy199.0 (3)
C46—C45—H45B111.2C27—O9—Dy2144.3 (2)
N12—C45—H45B111.2C36—O10—Dy2134.5 (3)
H45A—C45—H45B109.1N15—O11—Dy295.6 (3)
N11—C46—C45103.9 (4)N15—O12—Dy298.0 (3)
N11—C46—H46A111.0N16—O14—Dy293.6 (2)
C45—C46—H46A111.0N16—O15—Dy292.4 (3)
N11—C46—H46B111.0H23D—O23—H23E109.5
C45—C46—H46B111.0H24C—O24—H24E109.5
H46A—C46—H46B109.0H25D—O25—H25E109.5
N11—C47—C48112.1 (4)H26E—O26—H26D107.3
N11—C47—H47A109.2H27C—O27—H27A109.8
C48—C47—H47A109.2
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N14—H14A···O200.912.233.118 (6)166
N12—H12B···O100.901.992.696 (6)134
N12—H12A···N170.902.503.332 (7)155
N12—H12A···O170.902.342.972 (7)127
N12—H12A···O180.901.912.786 (6)164
N5—H5B···O20.901.972.684 (6)135
N5—H5A···N180.902.453.348 (7)177
N5—H5A···O210.902.213.015 (7)149
N5—H5A···O200.901.962.809 (6)156
N1—H1A···O10.861.982.610 (5)130
N10—H10A···O90.861.992.620 (5)129
N3—H3A···O17i0.912.183.008 (5)151
Symmetry code: (i) x+1, y+1, z.

Experimental details

Crystal data
Chemical formula[Dy(C26H34N6O2)(NO3)2]NO3·H2O
Mr829.14
Crystal system, space groupTriclinic, P1
Temperature (K)292
a, b, c (Å)14.005 (3), 14.045 (3), 21.896 (4)
α, β, γ (°)96.386 (3), 99.094 (3), 118.217 (3)
V3)3661.0 (13)
Z4
Radiation typeMo Kα
µ (mm1)2.11
Crystal size (mm)0.30 × 0.22 × 0.20
Data collection
DiffractometerBruker SMART CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.58, 0.66
No. of measured, independent and
observed [I > 2σ(I)] reflections
36705, 14395, 10889
Rint0.042
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.115, 1.04
No. of reflections14395
No. of parameters872
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.45, 1.42

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXTL (Bruker, 2000), SHELXTL.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N14—H14A···O200.912.233.118 (6)165.6
N12—H12B···O100.901.992.696 (6)133.8
N12—H12A···N170.902.503.332 (7)154.9
N12—H12A···O170.902.342.972 (7)126.9
N12—H12A···O180.901.912.786 (6)163.6
N5—H5B···O20.901.972.684 (6)135.1
N5—H5A···N180.902.453.348 (7)177.1
N5—H5A···O210.902.213.015 (7)149.1
N5—H5A···O200.901.962.809 (6)155.9
N1—H1A···O10.861.982.610 (5)129.5
N10—H10A···O90.861.992.620 (5)128.9
N3—H3A···O17i0.912.183.008 (5)150.9
Symmetry code: (i) x+1, y+1, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds