metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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catena-Poly[[bis­­(di­methyl sulfoxide-κO)cerium(III)]tris­­(μ2-3,5-di­nitro­benzoato-κ2O:O′)]

aDepartment of Applied Chemistry, College of Chemistry and Life Science, Yuncheng University, Yuncheng, Shanxi 044000, People's Republic of China, bPlant Protection and Plant Quarrantine Station, Agriculture and Animal Husbandry Bureau, Wulanchabu, Inner Mongolia 012000, People's Republic of China, and cDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 17 April 2011; accepted 27 April 2011; online 7 May 2011)

The polymeric title compound, [Ce(C7H3N2O6)3(C2H6OS)2]n, exists as a linear chain along [111] as the three dinitro­benzoate anions each engages in bridging adjacent dimethyl sulfoxide (DMSO) coordinated CeIII atoms. The metal atoms are surrounded by eight O atoms in a square-anti­prismatic environment. There are two independent formula units in the asymmetric unit. The S atoms of two of the four DMSO mol­ecules are disordered in a 0.926 (3):0.074 (3) ratio.

Related literature

For isotypic Pr(C7H3N2O6)3(C2H6OS)2, see: Niu et al. (2001[Niu, D.-Z., Mu, L.-L., Lu, Z.-S., Wang, Y.-C. & Chen, J.-T. (2001). Chin. J. Struct. Chem. 20, 473-477.]).

[Scheme 1]

Experimental

Crystal data
  • [Ce(C7H3N2O6)3(C2H6OS)2]

  • Mr = 929.72

  • Triclinic, [P \overline 1]

  • a = 14.3025 (10) Å

  • b = 14.3752 (10) Å

  • c = 21.9143 (16) Å

  • α = 101.8798 (9)°

  • β = 103.6758 (10)°

  • γ = 119.6828 (8)°

  • V = 3514.1 (4) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.51 mm−1

  • T = 293 K

  • 0.25 × 0.20 × 0.15 mm

Data collection
  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.760, Tmax = 1.000

  • 17917 measured reflections

  • 12456 independent reflections

  • 9611 reflections with I > 2σ(I)

  • Rint = 0.025

Refinement
  • R[F2 > 2σ(F2)] = 0.038

  • wR(F2) = 0.099

  • S = 1.03

  • 12456 reflections

  • 980 parameters

  • 6 restraints

  • H-atom parameters constrained

  • Δρmax = 0.91 e Å−3

  • Δρmin = −0.69 e Å−3

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

The background to the class of rare-earth 3,5-dinitrobenzoates is given in a report on Pr(C7H3N2O6)3(C2H6OS)2 (Niu et al., 2001). The DMSO used in the synthesis is incorporated into the crystal structure; DMF in other similar syntheses is also incorporated in the product. The title CeIII analog (Scheme I) is isostructural, the two compounds crystallizing with matching cell dimensions. Polymeric Ce(C7H3N2O6)3(C2H6OS)2 exists as a linear chain as the three dinitrobenzoate anions each engages in bridging adjacent DMSO-coordinated CeIII atoms (Fig. 1 and Fig. 2). The metal atoms are surrounded by eight O atoms in a square-antiprismatic environment (Fig. 3).

Related literature top

For isotypic Pr(C7H3N2O6)3(C2H6OS)2, see: Niu et al. (2001).

Experimental top

3, 5-Dinitrobenzoic acid (0.434 g) was heated in water (50 ml) at 333 K until it dissolved. Cerium trinitrate hexahydrate (0.442 g) was added followed by dimethyl sulfoxide (4 ml). The solution was heated for 5 h. The solution was filtered and the filtrate evaporated to dryness. The white product was recrystallized from ethanol to furnish colorless primatic crystals.

Refinement top

Carbon-bound H-atoms were placed in calculated positions (C—H 0.93 to 0.97 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2–1.5U(C).

The two DMSO molecules connected to Ce1 are both disordered over two positions in a 93 (1): 7 ratio in respect of the S atoms only. For each molecule, the temperature factors of the primed atom were set to those of the unprimed ones; the anisotropic temperature factors were restranied to be nearly isotropic. Each C–S and C–S' (as well O–S and O–S') pair of bonds were restrained to within 0.01 Å of each other. Their carbon atoms are ordered; however, because of the disordered S atoms, each C atom carries two sets of H-atoms. The ratio of the occupancies is that of the ratio for the S atoms, i.e., 93: 7.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of a portion of the polymeric chain of Ce(C7H3N2O6)3(C2H6OS)2 at the 50% probability level; hydrogen atoms are drawn as spheres of arbitrary radius. The disorder is not shown. Symmetry code: i = 1 - x, 1 - y, 1 - z.
[Figure 2] Fig. 2. Thermal ellipsoid plot (Barbour, 2001) of a portion of the polymeric chain of Ce(C7H3N2O6)3(C2H6OS)2 at the 50% probability level; hydrogen atoms are drawn as spheres of arbitrary radius. The disorder is not shown. Symmetry code: ii = 2 - x, 2 - y, 2 - z.
[Figure 3] Fig. 3. Geometry of Ce atoms.
catena-Poly[[bis(dimethyl sulfoxide-κO)cerium(III)]tris(µ2-3,5-dinitrobenzoato- κ2O:O')] top
Crystal data top
[Ce(C7H3N2O6)3(C2H6OS)2]Z = 4
Mr = 929.72F(000) = 1852
Triclinic, P1Dx = 1.757 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 14.3025 (10) ÅCell parameters from 5527 reflections
b = 14.3752 (10) Åθ = 2.4–24.9°
c = 21.9143 (16) ŵ = 1.51 mm1
α = 101.8798 (9)°T = 293 K
β = 103.6758 (10)°Prism, colorless
γ = 119.6828 (8)°0.25 × 0.20 × 0.15 mm
V = 3514.1 (4) Å3
Data collection top
Bruker SMART APEX
diffractometer
12456 independent reflections
Radiation source: fine-focus sealed tube9611 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
ω scansθmax = 25.3°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1714
Tmin = 0.760, Tmax = 1.000k = 1617
17917 measured reflectionsl = 2126
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)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.099H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0464P)2 + 1.0209P]
where P = (Fo2 + 2Fc2)/3
12456 reflections(Δ/σ)max = 0.001
980 parametersΔρmax = 0.91 e Å3
6 restraintsΔρmin = 0.69 e Å3
Crystal data top
[Ce(C7H3N2O6)3(C2H6OS)2]γ = 119.6828 (8)°
Mr = 929.72V = 3514.1 (4) Å3
Triclinic, P1Z = 4
a = 14.3025 (10) ÅMo Kα radiation
b = 14.3752 (10) ŵ = 1.51 mm1
c = 21.9143 (16) ÅT = 293 K
α = 101.8798 (9)°0.25 × 0.20 × 0.15 mm
β = 103.6758 (10)°
Data collection top
Bruker SMART APEX
diffractometer
12456 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
9611 reflections with I > 2σ(I)
Tmin = 0.760, Tmax = 1.000Rint = 0.025
17917 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0386 restraints
wR(F2) = 0.099H-atom parameters constrained
S = 1.03Δρmax = 0.91 e Å3
12456 reflectionsΔρmin = 0.69 e Å3
980 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ce10.55617 (2)0.62381 (2)0.604890 (12)0.02587 (8)
Ce20.88886 (2)0.94364 (2)0.895363 (12)0.02595 (8)
S10.65997 (14)0.92117 (12)0.62797 (10)0.0595 (6)0.926 (3)
S20.27585 (13)0.49215 (13)0.62830 (8)0.0489 (5)0.926 (3)
S1'0.5652 (11)0.9100 (8)0.6357 (5)0.0595 (6)0.074 (3)
S2'0.3250 (8)0.5992 (10)0.6758 (5)0.0489 (5)0.074 (3)
S31.03591 (12)1.22760 (11)0.87795 (7)0.0444 (3)
S40.58609 (13)0.84536 (13)0.86249 (10)0.0724 (5)
O10.7610 (3)0.7927 (3)0.67902 (15)0.0387 (8)
O20.8916 (3)0.9170 (3)0.78333 (15)0.0370 (7)
O31.2682 (4)0.9603 (4)0.8618 (2)0.0714 (12)
O41.3286 (4)0.9145 (5)0.7871 (3)0.1074 (19)
O51.0436 (5)0.6528 (5)0.5563 (3)0.126 (2)
O60.8807 (5)0.6300 (4)0.5236 (2)0.0901 (16)
O70.5827 (3)0.6188 (3)0.71728 (15)0.0370 (7)
O80.7161 (3)0.7416 (2)0.82119 (16)0.0423 (8)
O90.8682 (5)0.5956 (5)0.9696 (2)0.112 (2)
O100.8856 (5)0.4626 (5)0.9259 (3)0.121 (2)
O110.6372 (5)0.2095 (4)0.6876 (3)0.111 (2)
O120.5227 (5)0.2416 (4)0.6294 (2)0.0899 (16)
O130.6581 (3)0.6990 (3)0.53074 (16)0.0415 (8)
O140.5787 (3)0.5885 (2)0.42033 (15)0.0354 (7)
O150.7607 (5)0.7595 (4)0.2755 (2)0.0847 (15)
O160.8801 (5)0.9448 (4)0.3094 (3)0.1061 (19)
O171.0087 (4)1.1887 (4)0.5405 (3)0.0972 (18)
O180.9267 (5)1.1148 (4)0.6034 (3)0.1031 (19)
O190.4078 (3)0.5484 (3)0.49210 (15)0.0384 (8)
O200.3154 (3)0.4520 (3)0.38036 (16)0.0375 (8)
O210.0689 (4)0.5361 (5)0.2461 (2)0.0838 (15)
O220.0212 (5)0.6421 (5)0.2938 (3)0.114 (2)
O230.2391 (5)0.8722 (5)0.5359 (3)0.124 (2)
O240.3127 (4)0.8096 (5)0.5982 (2)0.0939 (17)
O250.7997 (3)0.8387 (3)0.96524 (17)0.0490 (9)
O260.8944 (3)0.9227 (3)1.07818 (15)0.0356 (7)
O270.6333 (5)0.8394 (5)1.2044 (3)0.0940 (17)
O280.4968 (4)0.6564 (5)1.1708 (3)0.1001 (18)
O290.2978 (4)0.4560 (4)0.9244 (3)0.1094 (19)
O300.3993 (4)0.4974 (4)0.8651 (3)0.0892 (16)
O310.9693 (3)0.8182 (3)0.88109 (16)0.0375 (8)
O321.0418 (3)0.9103 (2)0.99178 (15)0.0361 (7)
O331.2835 (4)0.8154 (4)1.1331 (2)0.0831 (15)
O341.3600 (5)0.7397 (6)1.0878 (3)0.119 (2)
O351.2544 (5)0.6112 (5)0.8471 (3)0.113 (2)
O361.1658 (5)0.6658 (4)0.7884 (2)0.0875 (15)
O370.5604 (3)0.8033 (3)0.6161 (2)0.0531 (10)
O380.3792 (3)0.5956 (3)0.62754 (17)0.0437 (8)
O390.9244 (3)1.1215 (3)0.87207 (16)0.0384 (8)
O400.7093 (3)0.9428 (3)0.8785 (2)0.0616 (11)
N11.2541 (4)0.9173 (4)0.8036 (3)0.0634 (14)
N20.9755 (5)0.6729 (4)0.5663 (3)0.0619 (14)
N30.8461 (4)0.5189 (5)0.9216 (3)0.0644 (14)
N40.5960 (5)0.2655 (4)0.6810 (3)0.0672 (14)
N50.8163 (5)0.8577 (5)0.3180 (3)0.0695 (15)
N60.9404 (5)1.1072 (4)0.5513 (3)0.0687 (15)
N70.0741 (4)0.5967 (5)0.2959 (3)0.0649 (14)
N80.2656 (5)0.8066 (5)0.5436 (3)0.0751 (17)
N90.5690 (5)0.7395 (6)1.1622 (3)0.0690 (15)
N100.3889 (4)0.5138 (4)0.9179 (3)0.0620 (14)
N111.2961 (5)0.7739 (5)1.0839 (3)0.0664 (14)
N121.2013 (5)0.6556 (4)0.8403 (3)0.0648 (14)
C10.8600 (4)0.8476 (4)0.7262 (2)0.0290 (10)
C20.9502 (4)0.8311 (4)0.7113 (2)0.0287 (10)
C31.0585 (4)0.8819 (4)0.7636 (2)0.0375 (11)
H31.07600.92550.80760.045*
C41.1393 (4)0.8657 (4)0.7484 (3)0.0440 (12)
C51.1166 (5)0.8000 (5)0.6848 (3)0.0518 (14)
H51.17200.78970.67590.062*
C61.0079 (5)0.7498 (4)0.6346 (3)0.0445 (12)
C70.9246 (4)0.7658 (4)0.6467 (2)0.0377 (11)
H70.85280.73280.61160.045*
C80.6579 (4)0.6469 (4)0.7738 (2)0.0291 (10)
C90.6745 (4)0.5549 (4)0.7839 (2)0.0293 (10)
C100.7461 (4)0.5751 (4)0.8466 (2)0.0374 (11)
H100.77870.64260.88360.045*
C110.7690 (4)0.4947 (4)0.8543 (3)0.0418 (12)
C120.7234 (5)0.3931 (5)0.8011 (3)0.0486 (13)
H120.74220.34110.80640.058*
C130.6491 (4)0.3738 (4)0.7402 (3)0.0414 (12)
C140.6235 (4)0.4514 (4)0.7301 (2)0.0382 (11)
H140.57260.43470.68770.046*
C150.6482 (4)0.6822 (4)0.4706 (2)0.0308 (10)
C160.7287 (4)0.7881 (4)0.4581 (2)0.0332 (10)
C170.7315 (4)0.7759 (4)0.3945 (2)0.0374 (11)
H170.68380.70340.35930.045*
C180.8052 (5)0.8720 (4)0.3839 (3)0.0461 (13)
C190.8742 (4)0.9825 (4)0.4340 (3)0.0504 (14)
H190.92181.04750.42590.060*
C200.8684 (4)0.9905 (4)0.4967 (3)0.0451 (13)
C210.7980 (4)0.8956 (4)0.5091 (3)0.0388 (11)
H210.79740.90410.55220.047*
C220.3370 (4)0.5223 (4)0.4346 (2)0.0326 (10)
C230.1498 (4)0.6191 (5)0.3641 (3)0.0438 (12)
C240.2013 (4)0.5593 (4)0.3675 (2)0.0389 (11)
H240.18710.50550.32830.047*
C250.2745 (4)0.5814 (4)0.4306 (2)0.0318 (10)
C260.2942 (4)0.6602 (4)0.4889 (2)0.0392 (11)
H260.34150.67380.53160.047*
C270.2412 (5)0.7180 (4)0.4818 (3)0.0477 (13)
C280.1679 (5)0.6989 (5)0.4202 (3)0.0510 (14)
H280.13240.73820.41680.061*
C290.8052 (4)0.8515 (4)1.0240 (2)0.0327 (10)
C300.6926 (4)0.7723 (4)1.0308 (2)0.0318 (10)
C310.6830 (4)0.7907 (4)1.0925 (3)0.0404 (12)
H310.74720.85181.13150.048*
C320.5784 (5)0.7186 (5)1.0962 (3)0.0473 (13)
C330.4809 (4)0.6260 (5)1.0400 (3)0.0508 (14)
H330.41100.57651.04350.061*
C340.4913 (4)0.6103 (4)0.9793 (3)0.0455 (13)
C350.5951 (4)0.6810 (4)0.9731 (2)0.0395 (11)
H350.59970.66780.93090.047*
C361.0328 (4)0.8443 (4)0.9396 (2)0.0324 (10)
C371.1041 (4)0.7946 (4)0.9482 (2)0.0337 (10)
C381.1634 (4)0.8043 (4)1.0115 (2)0.0388 (11)
H381.15800.83951.04990.047*
C391.2309 (5)0.7606 (4)1.0166 (3)0.0447 (13)
C401.2424 (5)0.7093 (5)0.9612 (3)0.0489 (14)
H401.28820.68060.96540.059*
C411.1835 (5)0.7026 (4)0.8998 (3)0.0476 (13)
C421.1140 (4)0.7429 (4)0.8916 (2)0.0386 (11)
H421.07420.73560.84870.046*
C430.5956 (7)0.9690 (6)0.5743 (4)0.097 (3)
H43A0.57270.92500.52770.146*0.926 (3)
H43B0.65141.04960.58480.146*0.926 (3)
H43C0.52770.95820.58140.146*0.926 (3)
H43D0.56490.90760.53190.146*0.074 (3)
H43E0.67891.02180.58890.146*0.074 (3)
H43F0.55941.00950.56850.146*0.074 (3)
C440.6918 (7)1.0145 (6)0.7068 (4)0.111 (3)
H44A0.72840.99930.74240.167*0.926 (3)
H44B0.62051.00210.70900.167*0.926 (3)
H44C0.74411.09340.71220.167*0.926 (3)
H44D0.74911.06680.69330.167*0.074 (3)
H44E0.72170.97820.72910.167*0.074 (3)
H44F0.67551.05680.73740.167*0.074 (3)
C450.1736 (5)0.5297 (6)0.6256 (3)0.0753 (19)
H45A0.14410.53070.58180.113*0.926 (3)
H45B0.21200.60500.66010.113*0.926 (3)
H45C0.10960.47360.63370.113*0.926 (3)
H45D0.16540.54220.58390.113*0.074 (3)
H45E0.14180.56130.65010.113*0.074 (3)
H45F0.13200.44810.61580.113*0.074 (3)
C460.3100 (7)0.4971 (6)0.7116 (3)0.084 (2)
H46A0.36660.47910.72240.126*0.926 (3)
H46B0.24010.44160.71550.126*0.926 (3)
H46C0.34190.57330.74260.126*0.926 (3)
H46D0.22970.43120.69120.126*0.074 (3)
H46E0.33290.53110.75970.126*0.074 (3)
H46F0.35920.47300.70350.126*0.074 (3)
C470.9983 (5)1.3264 (5)0.8680 (3)0.0576 (15)
H47A0.98861.35610.90770.086*
H47B0.92631.28690.82880.086*
H47C1.05971.38930.86210.086*
C481.0478 (6)1.1914 (5)0.7987 (3)0.0693 (18)
H48A1.06811.13670.79510.104*
H48B1.10761.26020.79600.104*
H48C0.97411.15790.76220.104*
C490.5422 (6)0.9107 (7)0.9170 (4)0.115 (3)
H49A0.58280.92490.96310.173*
H49B0.45920.85970.90400.173*
H49C0.56110.98270.91310.173*
C500.4992 (6)0.8331 (7)0.7853 (4)0.113 (3)
H50A0.51090.79720.74860.169*
H50B0.52120.90880.78720.169*
H50C0.41800.78650.77820.169*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ce10.02805 (14)0.02672 (14)0.02143 (14)0.01626 (12)0.00806 (11)0.00719 (11)
Ce20.02582 (14)0.02641 (14)0.02261 (14)0.01464 (11)0.00890 (11)0.00577 (11)
S10.0554 (10)0.0356 (8)0.0907 (14)0.0271 (8)0.0314 (9)0.0240 (8)
S20.0449 (9)0.0527 (9)0.0509 (10)0.0269 (8)0.0280 (7)0.0157 (7)
S1'0.0554 (10)0.0356 (8)0.0907 (14)0.0271 (8)0.0314 (9)0.0240 (8)
S2'0.0449 (9)0.0527 (9)0.0509 (10)0.0269 (8)0.0280 (7)0.0157 (7)
S30.0472 (8)0.0394 (7)0.0475 (8)0.0233 (6)0.0206 (6)0.0199 (6)
S40.0393 (8)0.0551 (9)0.1187 (15)0.0258 (8)0.0290 (9)0.0321 (10)
O10.0277 (17)0.0409 (18)0.0308 (18)0.0150 (15)0.0068 (15)0.0026 (15)
O20.0374 (18)0.0415 (18)0.0220 (17)0.0206 (16)0.0087 (14)0.0033 (15)
O30.053 (3)0.080 (3)0.064 (3)0.034 (2)0.009 (2)0.027 (3)
O40.054 (3)0.146 (5)0.119 (5)0.069 (3)0.023 (3)0.023 (4)
O50.107 (4)0.155 (5)0.111 (5)0.094 (4)0.044 (4)0.012 (4)
O60.088 (4)0.108 (4)0.048 (3)0.053 (3)0.026 (3)0.006 (3)
O70.0425 (19)0.0360 (17)0.0228 (17)0.0192 (16)0.0079 (15)0.0094 (14)
O80.046 (2)0.0228 (16)0.036 (2)0.0125 (15)0.0066 (16)0.0015 (15)
O90.171 (6)0.128 (5)0.045 (3)0.111 (5)0.004 (3)0.020 (3)
O100.134 (5)0.127 (5)0.108 (5)0.102 (4)0.001 (4)0.038 (4)
O110.178 (6)0.080 (3)0.103 (4)0.103 (4)0.043 (4)0.020 (3)
O120.114 (4)0.069 (3)0.051 (3)0.053 (3)0.004 (3)0.006 (2)
O130.044 (2)0.0359 (18)0.0288 (19)0.0125 (16)0.0154 (16)0.0113 (15)
O140.0347 (18)0.0266 (16)0.0330 (19)0.0112 (15)0.0122 (15)0.0091 (15)
O150.127 (4)0.078 (3)0.066 (3)0.054 (3)0.065 (3)0.038 (3)
O160.147 (5)0.084 (3)0.115 (4)0.053 (3)0.098 (4)0.069 (3)
O170.066 (3)0.035 (2)0.160 (5)0.016 (2)0.037 (3)0.027 (3)
O180.122 (5)0.045 (3)0.084 (4)0.026 (3)0.030 (4)0.006 (3)
O190.0353 (18)0.051 (2)0.0305 (19)0.0279 (17)0.0079 (15)0.0152 (16)
O200.0408 (19)0.0450 (19)0.0301 (19)0.0296 (17)0.0106 (15)0.0104 (16)
O210.098 (4)0.140 (4)0.048 (3)0.091 (4)0.026 (3)0.037 (3)
O220.155 (5)0.182 (6)0.080 (4)0.150 (5)0.031 (3)0.054 (4)
O230.173 (6)0.121 (4)0.102 (4)0.130 (5)0.019 (4)0.000 (3)
O240.107 (4)0.127 (4)0.054 (3)0.094 (4)0.014 (3)0.005 (3)
O250.040 (2)0.048 (2)0.033 (2)0.0081 (17)0.0180 (16)0.0110 (16)
O260.0278 (17)0.0361 (17)0.0325 (19)0.0127 (15)0.0111 (15)0.0110 (15)
O270.133 (5)0.115 (4)0.066 (3)0.079 (4)0.065 (3)0.041 (3)
O280.092 (4)0.147 (5)0.111 (4)0.068 (4)0.080 (3)0.091 (4)
O290.038 (3)0.080 (3)0.134 (5)0.005 (3)0.014 (3)0.036 (3)
O300.068 (3)0.070 (3)0.066 (3)0.020 (3)0.000 (3)0.003 (3)
O310.0426 (19)0.0351 (17)0.0297 (19)0.0241 (16)0.0112 (16)0.0021 (14)
O320.049 (2)0.0336 (17)0.0320 (18)0.0275 (16)0.0200 (16)0.0076 (14)
O330.129 (4)0.115 (4)0.048 (3)0.099 (4)0.028 (3)0.035 (3)
O340.152 (5)0.212 (6)0.094 (4)0.162 (5)0.051 (4)0.076 (4)
O350.176 (5)0.178 (5)0.100 (4)0.162 (5)0.080 (4)0.061 (4)
O360.152 (5)0.112 (4)0.064 (3)0.104 (4)0.069 (3)0.042 (3)
O370.047 (2)0.0344 (19)0.076 (3)0.0262 (17)0.0195 (19)0.0157 (18)
O380.0404 (19)0.052 (2)0.046 (2)0.0280 (18)0.0226 (17)0.0205 (17)
O390.0429 (19)0.0369 (18)0.043 (2)0.0237 (16)0.0222 (16)0.0192 (16)
O400.0302 (19)0.039 (2)0.108 (3)0.0208 (17)0.021 (2)0.018 (2)
N10.043 (3)0.066 (3)0.081 (4)0.035 (3)0.016 (3)0.030 (3)
N20.064 (3)0.063 (3)0.057 (3)0.036 (3)0.037 (3)0.009 (3)
N30.062 (3)0.071 (4)0.060 (4)0.041 (3)0.009 (3)0.033 (3)
N40.098 (4)0.042 (3)0.064 (4)0.042 (3)0.034 (3)0.017 (3)
N50.095 (4)0.074 (4)0.078 (4)0.052 (4)0.061 (4)0.055 (3)
N60.057 (3)0.036 (3)0.092 (5)0.024 (3)0.013 (3)0.012 (3)
N70.071 (3)0.102 (4)0.061 (4)0.070 (3)0.025 (3)0.047 (3)
N80.077 (4)0.088 (4)0.063 (4)0.067 (4)0.012 (3)0.001 (3)
N90.073 (4)0.110 (5)0.072 (4)0.064 (4)0.050 (3)0.059 (4)
N100.032 (3)0.043 (3)0.081 (4)0.013 (2)0.005 (3)0.017 (3)
N110.085 (4)0.091 (4)0.058 (4)0.070 (4)0.027 (3)0.038 (3)
N120.092 (4)0.075 (4)0.066 (4)0.065 (3)0.048 (3)0.029 (3)
C10.035 (3)0.032 (2)0.029 (3)0.020 (2)0.019 (2)0.016 (2)
C20.028 (2)0.029 (2)0.028 (2)0.015 (2)0.013 (2)0.0097 (19)
C30.037 (3)0.043 (3)0.037 (3)0.023 (2)0.016 (2)0.019 (2)
C40.034 (3)0.044 (3)0.054 (3)0.022 (2)0.016 (3)0.023 (3)
C50.053 (3)0.057 (3)0.069 (4)0.040 (3)0.037 (3)0.028 (3)
C60.049 (3)0.042 (3)0.045 (3)0.026 (3)0.025 (3)0.014 (2)
C70.039 (3)0.033 (3)0.041 (3)0.017 (2)0.023 (2)0.013 (2)
C80.027 (2)0.032 (2)0.029 (3)0.013 (2)0.019 (2)0.014 (2)
C90.033 (2)0.026 (2)0.027 (2)0.014 (2)0.013 (2)0.0116 (19)
C100.035 (3)0.037 (3)0.039 (3)0.019 (2)0.015 (2)0.018 (2)
C110.043 (3)0.047 (3)0.041 (3)0.026 (3)0.019 (2)0.025 (3)
C120.053 (3)0.054 (3)0.061 (4)0.038 (3)0.030 (3)0.032 (3)
C130.054 (3)0.036 (3)0.049 (3)0.029 (3)0.032 (3)0.019 (2)
C140.043 (3)0.036 (3)0.035 (3)0.019 (2)0.021 (2)0.017 (2)
C150.032 (2)0.034 (3)0.027 (3)0.017 (2)0.014 (2)0.014 (2)
C160.038 (3)0.030 (2)0.037 (3)0.021 (2)0.020 (2)0.015 (2)
C170.040 (3)0.033 (3)0.042 (3)0.019 (2)0.022 (2)0.017 (2)
C180.050 (3)0.047 (3)0.059 (4)0.030 (3)0.032 (3)0.032 (3)
C190.041 (3)0.041 (3)0.085 (4)0.024 (3)0.037 (3)0.037 (3)
C200.033 (3)0.028 (3)0.069 (4)0.016 (2)0.018 (3)0.014 (3)
C210.041 (3)0.034 (3)0.043 (3)0.023 (2)0.018 (2)0.013 (2)
C220.027 (2)0.028 (2)0.038 (3)0.015 (2)0.010 (2)0.013 (2)
C230.044 (3)0.060 (3)0.045 (3)0.037 (3)0.019 (3)0.030 (3)
C240.044 (3)0.045 (3)0.035 (3)0.030 (3)0.017 (2)0.014 (2)
C250.030 (2)0.034 (2)0.029 (3)0.018 (2)0.011 (2)0.010 (2)
C260.036 (3)0.045 (3)0.039 (3)0.027 (2)0.013 (2)0.013 (2)
C270.053 (3)0.047 (3)0.043 (3)0.034 (3)0.016 (3)0.005 (3)
C280.058 (3)0.058 (3)0.060 (4)0.049 (3)0.024 (3)0.022 (3)
C290.029 (3)0.032 (2)0.031 (3)0.014 (2)0.012 (2)0.011 (2)
C300.029 (2)0.033 (2)0.033 (3)0.016 (2)0.014 (2)0.015 (2)
C310.035 (3)0.041 (3)0.041 (3)0.018 (2)0.017 (2)0.016 (2)
C320.052 (3)0.062 (4)0.056 (4)0.038 (3)0.038 (3)0.037 (3)
C330.036 (3)0.049 (3)0.085 (5)0.026 (3)0.033 (3)0.041 (3)
C340.026 (3)0.037 (3)0.062 (4)0.014 (2)0.009 (3)0.020 (3)
C350.038 (3)0.035 (3)0.038 (3)0.019 (2)0.012 (2)0.011 (2)
C360.032 (3)0.029 (2)0.038 (3)0.019 (2)0.014 (2)0.013 (2)
C370.037 (3)0.031 (2)0.032 (3)0.021 (2)0.014 (2)0.008 (2)
C380.055 (3)0.040 (3)0.042 (3)0.036 (3)0.024 (2)0.021 (2)
C390.053 (3)0.049 (3)0.046 (3)0.037 (3)0.019 (3)0.023 (3)
C400.059 (3)0.062 (3)0.063 (4)0.051 (3)0.036 (3)0.032 (3)
C410.064 (4)0.051 (3)0.050 (3)0.043 (3)0.032 (3)0.020 (3)
C420.050 (3)0.037 (3)0.034 (3)0.029 (2)0.015 (2)0.011 (2)
C430.119 (7)0.080 (5)0.094 (6)0.054 (5)0.035 (5)0.050 (5)
C440.137 (7)0.065 (5)0.085 (6)0.053 (5)0.007 (5)0.003 (4)
C450.065 (4)0.103 (5)0.078 (5)0.057 (4)0.042 (4)0.029 (4)
C460.118 (6)0.092 (5)0.078 (5)0.064 (5)0.067 (5)0.052 (4)
C470.065 (4)0.048 (3)0.064 (4)0.034 (3)0.023 (3)0.030 (3)
C480.080 (5)0.075 (4)0.069 (4)0.041 (4)0.054 (4)0.035 (4)
C490.069 (5)0.127 (7)0.125 (8)0.042 (5)0.057 (5)0.024 (6)
C500.079 (5)0.131 (7)0.094 (6)0.066 (6)0.006 (5)0.002 (5)
Geometric parameters (Å, º) top
Ce1—O12.489 (3)C3—H30.9300
Ce1—O72.423 (3)C4—C51.371 (7)
Ce1—O132.493 (3)C5—C61.379 (7)
Ce1—O14i2.512 (3)C5—H50.9300
Ce1—O192.434 (3)C6—C71.392 (6)
Ce1—O20i2.552 (3)C7—H70.9300
Ce1—O372.509 (3)C8—C91.503 (6)
Ce1—O382.545 (3)C9—C101.377 (6)
Ce2—O22.418 (3)C9—C141.390 (6)
Ce2—O82.496 (3)C10—C111.379 (6)
Ce2—O252.493 (3)C10—H100.9300
Ce2—O26ii2.535 (3)C11—C121.383 (7)
Ce2—O312.582 (3)C12—C131.368 (7)
Ce2—O32ii2.479 (3)C12—H120.9300
Ce2—O392.535 (3)C13—C141.377 (6)
Ce2—O402.499 (3)C14—H140.9300
S1—O371.491 (4)C15—C161.517 (6)
S1—C441.749 (7)C16—C211.366 (6)
S1—C431.775 (7)C16—C171.381 (6)
S1—H43E1.7691C17—C181.371 (6)
S1—H44D1.8212C17—H170.9300
S2—O381.497 (3)C18—C191.385 (7)
S2—C461.752 (6)C19—C201.380 (8)
S2—C451.786 (6)C19—H190.9300
S2—H45F1.7546C20—C211.368 (6)
S1'—O371.468 (9)C21—H210.9300
S1'—C441.724 (11)C22—C251.508 (6)
S1'—C431.760 (11)C23—C281.368 (7)
S2'—O381.458 (9)C23—C241.385 (6)
S2'—C461.750 (11)C24—C251.384 (6)
S2'—C451.782 (10)C24—H240.9300
S3—O391.517 (3)C25—C261.383 (6)
S3—C481.781 (5)C26—C271.383 (6)
S3—C471.784 (5)C26—H260.9300
S4—O401.501 (4)C27—C281.375 (7)
S4—C501.761 (8)C28—H280.9300
S4—C491.783 (7)C29—C301.511 (6)
O1—C11.249 (5)C30—C311.376 (6)
O2—C11.240 (5)C30—C351.391 (6)
O3—N11.218 (6)C31—C321.369 (7)
O4—N11.217 (6)C31—H310.9300
O5—N21.199 (6)C32—C331.382 (7)
O6—N21.194 (6)C33—C341.359 (7)
O7—C81.260 (5)C33—H330.9300
O8—C81.229 (5)C34—C351.383 (7)
O9—N31.201 (6)C35—H350.9300
O10—N31.200 (6)C36—C371.508 (6)
O11—N41.222 (6)C37—C421.385 (6)
O12—N41.192 (6)C37—C381.382 (6)
O13—C151.251 (5)C38—C391.386 (6)
O14—C151.250 (5)C38—H380.9300
O14—Ce1i2.512 (3)C39—C401.374 (7)
O15—N51.220 (6)C40—C411.364 (7)
O16—N51.218 (6)C40—H400.9300
O17—N61.213 (7)C41—C421.373 (7)
O18—N61.194 (7)C42—H420.9300
O19—C221.257 (5)C43—H43A0.9600
O20—C221.245 (5)C43—H43B0.9600
O20—Ce1i2.552 (3)C43—H43C0.9600
O21—N71.209 (6)C43—H43D0.9600
O22—N71.219 (6)C43—H43E0.9600
O23—N81.204 (6)C43—H43F0.9600
O24—N81.206 (6)C44—H44A0.9600
O25—C291.240 (5)C44—H44B0.9600
O26—C291.255 (5)C44—H44C0.9600
O26—Ce2ii2.535 (3)C44—H44D0.9600
O27—N91.227 (7)C44—H44E0.9599
O28—N91.221 (7)C44—H44F0.9599
O29—N101.215 (6)C45—H45A0.9600
O30—N101.192 (6)C45—H45B0.9600
O31—C361.234 (5)C45—H45C0.9600
O32—C361.261 (5)C45—H45D0.9600
O32—Ce2ii2.479 (3)C45—H45E0.9598
O33—N111.217 (6)C45—H45F0.9600
O34—N111.228 (6)C46—H46A0.9600
O35—N121.214 (6)C46—H46B0.9600
O36—N121.202 (6)C46—H46C0.9600
N1—C41.482 (7)C46—H46D0.9599
N2—C61.471 (7)C46—H46E0.9598
N3—C111.467 (7)C46—H46F0.9600
N4—C131.489 (6)C47—H47A0.9600
N5—C181.473 (7)C47—H47B0.9600
N6—C201.479 (7)C47—H47C0.9600
N7—C231.482 (6)C48—H48A0.9600
N8—C271.484 (7)C48—H48B0.9600
N9—C321.468 (7)C48—H48C0.9600
N10—C341.472 (7)C49—H49A0.9600
N11—C391.462 (7)C49—H49B0.9600
N12—C411.479 (7)C49—H49C0.9600
C1—C21.517 (6)C50—H50A0.9600
C2—C71.373 (6)C50—H50B0.9600
C2—C31.393 (6)C50—H50C0.9600
C3—C41.385 (6)
O7—Ce1—O19143.08 (11)C13—C12—C11116.0 (5)
O7—Ce1—O175.32 (10)C13—C12—H12122.0
O19—Ce1—O1139.62 (11)C11—C12—H12122.0
O7—Ce1—O13145.04 (11)C12—C13—C14123.3 (5)
O19—Ce1—O1371.83 (10)C12—C13—N4118.7 (5)
O1—Ce1—O1371.68 (10)C14—C13—N4117.9 (5)
O7—Ce1—O37103.30 (12)C13—C14—C9119.3 (5)
O19—Ce1—O3783.09 (11)C13—C14—H14120.4
O1—Ce1—O3772.82 (11)C9—C14—H14120.4
O13—Ce1—O3777.73 (12)O14—C15—O13126.8 (4)
O7—Ce1—O14i77.27 (10)O14—C15—C16117.4 (4)
O19—Ce1—O14i76.32 (10)O13—C15—C16115.7 (4)
O1—Ce1—O14i140.00 (10)C21—C16—C17119.7 (4)
O13—Ce1—O14i123.16 (10)C21—C16—C15120.6 (4)
O37—Ce1—O14i142.52 (11)C17—C16—C15119.7 (4)
O7—Ce1—O3871.87 (11)C18—C17—C16119.3 (5)
O19—Ce1—O3876.24 (11)C18—C17—H17120.4
O1—Ce1—O38122.96 (10)C16—C17—H17120.4
O13—Ce1—O38137.47 (11)C17—C18—C19122.4 (5)
O37—Ce1—O3871.14 (11)C17—C18—N5119.3 (5)
O14i—Ce1—O3873.69 (10)C19—C18—N5118.3 (5)
O7—Ce1—O20i77.85 (10)C20—C19—C18116.3 (5)
O19—Ce1—O20i118.05 (10)C20—C19—H19121.9
O1—Ce1—O20i72.54 (10)C18—C19—H19121.9
O13—Ce1—O20i81.56 (11)C21—C20—C19122.4 (5)
O37—Ce1—O20i143.73 (11)C21—C20—N6119.9 (5)
O14i—Ce1—O20i73.63 (10)C19—C20—N6117.7 (5)
O38—Ce1—O20i139.33 (10)C16—C21—C20119.9 (5)
O2—Ce2—O32ii144.49 (10)C16—C21—H21120.0
O2—Ce2—O25143.39 (11)C20—C21—H21120.0
O32ii—Ce2—O2571.96 (10)O20—C22—O19124.9 (4)
O2—Ce2—O874.83 (11)O20—C22—C25117.4 (4)
O32ii—Ce2—O8137.53 (11)O19—C22—C25117.7 (4)
O25—Ce2—O869.52 (11)C28—C23—C24123.0 (5)
O2—Ce2—O40101.42 (13)C28—C23—N7119.2 (5)
O32ii—Ce2—O4081.26 (12)C24—C23—N7117.8 (5)
O25—Ce2—O4076.00 (13)C23—C24—C25118.4 (5)
O8—Ce2—O4072.80 (11)C23—C24—H24120.8
O2—Ce2—O3972.02 (10)C25—C24—H24120.8
O32ii—Ce2—O3975.57 (10)C26—C25—C24120.7 (4)
O25—Ce2—O39136.63 (11)C26—C25—C22120.4 (4)
O8—Ce2—O39124.05 (10)C24—C25—C22118.8 (4)
O40—Ce2—O3971.28 (11)C25—C26—C27117.9 (5)
O2—Ce2—O26ii77.55 (10)C25—C26—H26121.0
O32ii—Ce2—O26ii79.01 (10)C27—C26—H26121.0
O25—Ce2—O26ii127.03 (10)C28—C27—C26123.4 (5)
O8—Ce2—O26ii140.06 (10)C28—C27—N8118.0 (5)
O40—Ce2—O26ii141.57 (11)C26—C27—N8118.6 (5)
O39—Ce2—O26ii72.02 (10)C23—C28—C27116.5 (4)
O2—Ce2—O3176.18 (10)C23—C28—H28121.7
O32ii—Ce2—O31120.76 (10)C27—C28—H28121.7
O25—Ce2—O3185.94 (11)O25—C29—O26126.9 (4)
O8—Ce2—O3173.60 (10)O25—C29—C30116.4 (4)
O40—Ce2—O31145.67 (11)O26—C29—C30116.7 (4)
O39—Ce2—O31136.10 (10)C31—C30—C35119.2 (4)
O26ii—Ce2—O3172.17 (10)C31—C30—C29121.5 (4)
O32ii—Ce2—O3274.92 (10)C35—C30—C29119.3 (4)
O8—Ce2—O32103.40 (9)C32—C31—C30119.6 (5)
O26ii—Ce2—O3265.48 (9)C32—C31—H31120.2
O37—S1—C44106.9 (3)C30—C31—H31120.2
O37—S1—C43104.5 (3)C31—C32—C33122.4 (5)
C44—S1—C4399.1 (4)C31—C32—N9119.2 (5)
O38—S2—C46108.0 (3)C33—C32—N9118.4 (5)
O38—S2—C45103.9 (3)C34—C33—C32117.1 (5)
O37—S1'—C44109.3 (7)C34—C33—H33121.4
O37—S1'—C43106.3 (7)C32—C33—H33121.4
C44—S1'—C43100.6 (6)C33—C34—C35122.4 (5)
O38—S2'—C46110.0 (7)C33—C34—N10118.9 (5)
O38—S2'—C45105.8 (6)C35—C34—N10118.7 (5)
C46—S2'—C4598.0 (6)C34—C35—C30119.2 (5)
O39—S3—C48106.0 (2)C34—C35—H35120.4
O39—S3—C47104.9 (2)C30—C35—H35120.4
C48—S3—C4797.9 (3)O31—C36—O32123.8 (4)
O40—S4—C50105.5 (4)O31—C36—C37117.4 (4)
O40—S4—C49103.3 (3)O32—C36—C37118.8 (4)
C50—S4—C4997.5 (4)C42—C37—C38119.9 (4)
C1—O1—Ce1156.6 (3)C42—C37—C36118.8 (4)
C1—O2—Ce2147.1 (3)C38—C37—C36121.3 (4)
C8—O7—Ce1144.0 (3)C37—C38—C39118.8 (5)
C8—O8—Ce2157.4 (3)C37—C38—H38120.6
C15—O13—Ce1144.5 (3)C39—C38—H38120.6
C15—O14—Ce1i139.1 (3)C40—C39—C38122.3 (5)
C22—O19—Ce1172.9 (3)C40—C39—N11119.0 (5)
C22—O20—Ce1i113.0 (3)C38—C39—N11118.6 (5)
C29—O25—Ce2143.0 (3)C41—C40—C39117.0 (5)
C29—O26—Ce2ii133.4 (3)C41—C40—H40121.5
C36—O31—Ce2104.2 (3)C39—C40—H40121.5
C36—O32—Ce2ii165.7 (3)C40—C41—C42123.2 (5)
Ce2ii—O32—Ce2105.08 (10)C40—C41—N12117.9 (5)
S1'—O37—S153.8 (5)C42—C41—N12118.8 (5)
S1'—O37—Ce1169.4 (5)C41—C42—C37118.8 (5)
S1—O37—Ce1128.79 (19)C41—C42—H42120.6
S2'—O38—S255.1 (5)C37—C42—H42120.6
S2'—O38—Ce1149.0 (4)S1—C43—H43A109.5
S2—O38—Ce1131.60 (19)S1—C43—H43B109.5
S3—O39—Ce2130.77 (18)H43A—C43—H43B109.5
S4—O40—Ce2129.94 (19)S1—C43—H43C109.5
O4—N1—O3124.5 (5)H43A—C43—H43C109.5
O4—N1—C4117.3 (6)H43B—C43—H43C109.5
O3—N1—C4118.2 (5)S1'—C43—H43D109.3
O6—N2—O5122.7 (6)S1'—C43—H43E109.6
O6—N2—C6118.6 (5)H43D—C43—H43E109.5
O5—N2—C6118.6 (6)S1'—C43—H43F109.5
O9—N3—O10123.1 (6)H43D—C43—H43F109.5
O9—N3—C11118.3 (5)H43E—C43—H43F109.5
O10—N3—C11118.6 (6)S1—C44—H44A109.5
O12—N4—O11123.6 (6)S1—C44—H44B109.5
O12—N4—C13119.9 (5)H44A—C44—H44B109.5
O11—N4—C13116.4 (6)S1—C44—H44C109.5
O15—N5—O16124.2 (6)H44A—C44—H44C109.5
O15—N5—C18118.0 (5)H44B—C44—H44C109.5
O16—N5—C18117.9 (6)S1'—C44—H44D109.1
O18—N6—O17124.4 (6)S1'—C44—H44E109.4
O18—N6—C20117.3 (6)H44D—C44—H44E109.5
O17—N6—C20118.3 (6)S1'—C44—H44F109.8
O21—N7—O22123.8 (5)H44D—C44—H44F109.5
O21—N7—C23119.0 (5)H44E—C44—H44F109.5
O22—N7—C23117.2 (5)S2—C45—H45A109.5
O24—N8—O23124.3 (6)S2—C45—H45B109.5
O24—N8—C27117.9 (5)H45A—C45—H45B109.5
O23—N8—C27117.8 (6)S2—C45—H45C109.5
O28—N9—O27124.9 (6)H45A—C45—H45C109.5
O28—N9—C32117.6 (6)H45B—C45—H45C109.5
O27—N9—C32117.5 (5)S2'—C45—H45D109.4
O30—N10—O29123.9 (6)S2'—C45—H45E109.6
O30—N10—C34118.9 (5)H45D—C45—H45E109.5
O29—N10—C34117.2 (6)S2'—C45—H45F109.4
O33—N11—O34122.9 (5)H45D—C45—H45F109.5
O33—N11—C39119.6 (5)H45E—C45—H45F109.5
O34—N11—C39117.6 (5)S2—C46—H46A109.5
O36—N12—O35123.0 (5)S2—C46—H46B109.5
O36—N12—C41119.0 (5)H46A—C46—H46B109.5
O35—N12—C41117.9 (5)S2—C46—H46C109.5
O2—C1—O1125.6 (4)H46A—C46—H46C109.5
O2—C1—C2117.4 (4)H46B—C46—H46C109.5
O1—C1—C2117.0 (4)S2'—C46—H46D109.5
C7—C2—C3120.5 (4)S2'—C46—H46E109.5
C7—C2—C1120.0 (4)H46D—C46—H46E109.5
C3—C2—C1119.5 (4)S2'—C46—H46F109.4
C4—C3—C2118.2 (5)H46D—C46—H46F109.5
C4—C3—H3120.9H46E—C46—H46F109.5
C2—C3—H3120.9S3—C47—H47A109.5
C5—C4—C3123.1 (5)S3—C47—H47B109.5
C5—C4—N1117.8 (5)H47A—C47—H47B109.5
C3—C4—N1119.0 (5)S3—C47—H47C109.5
C4—C5—C6116.9 (5)H47A—C47—H47C109.5
C4—C5—H5121.5H47B—C47—H47C109.5
C6—C5—H5121.5S3—C48—H48A109.5
C5—C6—C7122.3 (5)S3—C48—H48B109.5
C5—C6—N2119.7 (5)H48A—C48—H48B109.5
C7—C6—N2117.9 (5)S3—C48—H48C109.5
C2—C7—C6118.9 (5)H48A—C48—H48C109.5
C2—C7—H7120.6H48B—C48—H48C109.5
C6—C7—H7120.6S4—C49—H49A109.5
O8—C8—O7125.4 (4)S4—C49—H49B109.5
O8—C8—C9118.1 (4)H49A—C49—H49B109.5
O7—C8—C9116.5 (4)S4—C49—H49C109.5
C10—C9—C14118.9 (4)H49A—C49—H49C109.5
C10—C9—C8119.8 (4)H49B—C49—H49C109.5
C14—C9—C8121.2 (4)S4—C50—H50A109.5
C9—C10—C11119.7 (5)S4—C50—H50B109.5
C9—C10—H10120.1H50A—C50—H50B109.5
C11—C10—H10120.1S4—C50—H50C109.5
C10—C11—C12122.7 (5)H50A—C50—H50C109.5
C10—C11—N3118.5 (5)H50B—C50—H50C109.5
C12—C11—N3118.8 (5)
O7—Ce1—O1—C137.3 (7)O9—N3—C11—C1013.7 (8)
O19—Ce1—O1—C1157.4 (7)O10—N3—C11—C10165.0 (6)
O13—Ce1—O1—C1131.0 (7)O9—N3—C11—C12166.9 (6)
O37—Ce1—O1—C1146.5 (7)O10—N3—C11—C1214.4 (8)
O14i—Ce1—O1—C110.9 (8)C10—C11—C12—C132.8 (8)
O38—Ce1—O1—C193.7 (7)N3—C11—C12—C13177.8 (5)
O20i—Ce1—O1—C144.4 (7)C11—C12—C13—C142.8 (8)
O32ii—Ce2—O2—C1179.2 (5)C11—C12—C13—N4179.4 (5)
O25—Ce2—O2—C18.1 (6)O12—N4—C13—C12173.0 (6)
O8—Ce2—O2—C121.5 (5)O11—N4—C13—C1211.6 (8)
O40—Ce2—O2—C189.9 (5)O12—N4—C13—C149.1 (8)
O39—Ce2—O2—C1155.7 (6)O11—N4—C13—C14166.3 (5)
O26ii—Ce2—O2—C1129.4 (5)C12—C13—C14—C90.3 (7)
O31—Ce2—O2—C155.0 (5)N4—C13—C14—C9178.1 (4)
O19—Ce1—O7—C8169.2 (4)C10—C9—C14—C132.3 (7)
O1—Ce1—O7—C826.7 (5)C8—C9—C14—C13174.4 (4)
O13—Ce1—O7—C87.0 (6)Ce1i—O14—C15—O1312.9 (8)
O37—Ce1—O7—C894.6 (5)Ce1i—O14—C15—C16168.1 (3)
O14i—Ce1—O7—C8123.9 (5)Ce1—O13—C15—O1422.0 (8)
O38—Ce1—O7—C8159.3 (5)Ce1—O13—C15—C16157.0 (4)
O20i—Ce1—O7—C848.2 (5)O14—C15—C16—C21173.0 (4)
O2—Ce2—O8—C831.2 (8)O13—C15—C16—C216.1 (6)
O32ii—Ce2—O8—C8166.5 (7)O14—C15—C16—C176.7 (6)
O25—Ce2—O8—C8140.3 (8)O13—C15—C16—C17174.2 (4)
O40—Ce2—O8—C8138.6 (8)C21—C16—C17—C180.8 (7)
O39—Ce2—O8—C886.5 (8)C15—C16—C17—C18179.4 (4)
O26ii—Ce2—O8—C816.6 (9)C16—C17—C18—C192.6 (8)
O31—Ce2—O8—C848.6 (8)C16—C17—C18—N5174.4 (5)
O7—Ce1—O13—C15155.5 (5)O15—N5—C18—C171.6 (8)
O19—Ce1—O13—C1522.1 (5)O16—N5—C18—C17178.2 (6)
O1—Ce1—O13—C15175.5 (5)O15—N5—C18—C19175.5 (5)
O37—Ce1—O13—C15108.8 (5)O16—N5—C18—C194.7 (8)
O14i—Ce1—O13—C1537.1 (6)C17—C18—C19—C202.4 (8)
O38—Ce1—O13—C1565.4 (6)N5—C18—C19—C20174.6 (5)
O20i—Ce1—O13—C15101.2 (5)C18—C19—C20—C210.5 (8)
O2—Ce2—O25—C29172.1 (5)C18—C19—C20—N6179.6 (4)
O32ii—Ce2—O25—C2912.4 (5)O18—N6—C20—C215.9 (8)
O8—Ce2—O25—C29174.1 (6)O17—N6—C20—C21174.4 (5)
O40—Ce2—O25—C2997.6 (5)O18—N6—C20—C19173.1 (6)
O39—Ce2—O25—C2955.8 (6)O17—N6—C20—C196.5 (8)
O26ii—Ce2—O25—C2947.8 (6)C17—C16—C21—C201.0 (7)
O31—Ce2—O25—C29111.9 (5)C15—C16—C21—C20178.7 (4)
O2—Ce2—O31—C36151.1 (3)C19—C20—C21—C161.1 (7)
O32ii—Ce2—O31—C365.1 (3)N6—C20—C21—C16177.9 (4)
O25—Ce2—O31—C3661.1 (3)Ce1i—O20—C22—O195.1 (6)
O8—Ce2—O31—C36130.9 (3)Ce1i—O20—C22—C25174.2 (3)
O40—Ce2—O31—C36118.8 (3)O21—N7—C23—C28171.8 (6)
O39—Ce2—O31—C36106.7 (3)O22—N7—C23—C287.6 (8)
O26ii—Ce2—O31—C3670.0 (3)O21—N7—C23—C246.8 (8)
O32ii—Ce2—O32—C36170.3 (3)O22—N7—C23—C24173.9 (6)
O8—Ce2—O32—C3653.6 (3)C28—C23—C24—C250.1 (8)
O26ii—Ce2—O32—C3685.7 (3)N7—C23—C24—C25178.5 (4)
O2—Ce2—O32—Ce2ii144.15 (10)C23—C24—C25—C261.0 (7)
O32ii—Ce2—O32—Ce2ii0.0C23—C24—C25—C22176.2 (4)
O25—Ce2—O32—Ce2ii76.85 (12)O20—C22—C25—C26179.8 (4)
O8—Ce2—O32—Ce2ii136.15 (11)O19—C22—C25—C260.9 (6)
O40—Ce2—O32—Ce2ii57.08 (18)O20—C22—C25—C243.0 (6)
O39—Ce2—O32—Ce2ii54.11 (16)O19—C22—C25—C24176.3 (4)
O26ii—Ce2—O32—Ce2ii84.59 (12)C24—C25—C26—C271.8 (7)
O31—Ce2—O32—Ce2ii172.95 (18)C22—C25—C26—C27175.3 (4)
C44—S1—O37—Ce1116.4 (4)C25—C26—C27—C281.8 (8)
C43—S1—O37—Ce1139.2 (3)C25—C26—C27—N8177.3 (5)
O7—Ce1—O37—S198.3 (3)O24—N8—C27—C28167.5 (6)
O19—Ce1—O37—S1118.6 (3)O23—N8—C27—C2813.9 (9)
O1—Ce1—O37—S128.6 (3)O24—N8—C27—C2613.3 (9)
O13—Ce1—O37—S145.8 (3)O23—N8—C27—C26165.3 (6)
O14i—Ce1—O37—S1175.3 (2)C24—C23—C28—C270.1 (8)
O38—Ce1—O37—S1163.6 (3)N7—C23—C28—C27178.4 (5)
O20i—Ce1—O37—S110.8 (4)C26—C27—C28—C231.0 (8)
C46—S2—O38—Ce191.7 (3)N8—C27—C28—C23178.2 (5)
C45—S2—O38—Ce1165.1 (3)Ce2—O25—C29—O2629.4 (9)
O7—Ce1—O38—S2'14.8 (9)Ce2—O25—C29—C30151.1 (4)
O19—Ce1—O38—S2'175.9 (10)Ce2ii—O26—C29—O2510.2 (7)
O1—Ce1—O38—S2'43.2 (10)Ce2ii—O26—C29—C30169.4 (3)
O13—Ce1—O38—S2'142.0 (9)O25—C29—C30—C31169.1 (4)
O37—Ce1—O38—S2'96.8 (10)O26—C29—C30—C3111.3 (6)
O14i—Ce1—O38—S2'96.4 (10)O25—C29—C30—C358.6 (6)
O20i—Ce1—O38—S2'58.7 (10)O26—C29—C30—C35171.0 (4)
O7—Ce1—O38—S274.8 (3)C35—C30—C31—C320.6 (7)
O19—Ce1—O38—S286.4 (3)C29—C30—C31—C32178.3 (4)
O1—Ce1—O38—S2132.8 (2)C30—C31—C32—C330.7 (8)
O13—Ce1—O38—S2128.5 (2)C30—C31—C32—N9179.6 (5)
O37—Ce1—O38—S2173.6 (3)O28—N9—C32—C31152.9 (5)
O14i—Ce1—O38—S26.8 (2)O27—N9—C32—C3127.8 (8)
O20i—Ce1—O38—S230.9 (3)O28—N9—C32—C3326.8 (8)
C48—S3—O39—Ce287.1 (3)O27—N9—C32—C33152.4 (6)
C47—S3—O39—Ce2170.0 (3)C31—C32—C33—C341.7 (8)
O2—Ce2—O39—S381.3 (2)N9—C32—C33—C34178.5 (5)
O32ii—Ce2—O39—S384.0 (2)C32—C33—C34—C351.6 (8)
O25—Ce2—O39—S3126.4 (2)C32—C33—C34—N10179.0 (4)
O8—Ce2—O39—S3137.8 (2)O30—N10—C34—C33177.2 (6)
O40—Ce2—O39—S3169.5 (3)O29—N10—C34—C333.4 (8)
O26ii—Ce2—O39—S31.1 (2)O30—N10—C34—C352.2 (8)
O31—Ce2—O39—S335.6 (3)O29—N10—C34—C35177.2 (5)
C50—S4—O40—Ce2121.1 (4)C33—C34—C35—C300.4 (7)
C49—S4—O40—Ce2137.1 (4)N10—C34—C35—C30179.8 (4)
O2—Ce2—O40—S495.7 (3)C31—C30—C35—C340.7 (7)
O32ii—Ce2—O40—S4120.2 (3)C29—C30—C35—C34178.5 (4)
O25—Ce2—O40—S446.8 (3)Ce2—O31—C36—O325.7 (5)
O8—Ce2—O40—S425.7 (3)Ce2—O31—C36—C37173.6 (3)
O39—Ce2—O40—S4162.1 (4)Ce2ii—O32—C36—O31143.5 (9)
O26ii—Ce2—O40—S4180.0 (2)Ce2ii—O32—C36—C3735.8 (14)
O31—Ce2—O40—S413.6 (5)O31—C36—C37—C4212.9 (6)
Ce2—O2—C1—O179.9 (7)O32—C36—C37—C42166.5 (4)
Ce2—O2—C1—C2102.5 (5)O31—C36—C37—C38170.0 (4)
Ce1—O1—C1—O298.1 (8)O32—C36—C37—C3810.7 (7)
Ce1—O1—C1—C284.3 (8)C42—C37—C38—C390.6 (7)
O2—C1—C2—C7172.6 (4)C36—C37—C38—C39177.7 (4)
O1—C1—C2—C75.2 (6)C37—C38—C39—C400.9 (8)
O2—C1—C2—C37.9 (6)C37—C38—C39—N11178.3 (5)
O1—C1—C2—C3174.3 (4)O33—N11—C39—C40177.4 (6)
C7—C2—C3—C40.7 (7)O34—N11—C39—C401.0 (9)
C1—C2—C3—C4179.7 (4)O33—N11—C39—C385.1 (8)
C2—C3—C4—C51.6 (7)O34—N11—C39—C38176.5 (6)
C2—C3—C4—N1178.9 (4)C38—C39—C40—C410.2 (8)
O4—N1—C4—C511.9 (8)N11—C39—C40—C41177.6 (5)
O3—N1—C4—C5168.8 (5)C39—C40—C41—C420.8 (8)
O4—N1—C4—C3170.6 (5)C39—C40—C41—N12175.6 (5)
O3—N1—C4—C38.6 (7)O36—N12—C41—C40168.2 (6)
C3—C4—C5—C60.7 (8)O35—N12—C41—C409.7 (8)
N1—C4—C5—C6178.0 (5)O36—N12—C41—C428.3 (8)
C4—C5—C6—C71.1 (8)O35—N12—C41—C42173.7 (6)
C4—C5—C6—N2176.6 (5)C40—C41—C42—C371.0 (8)
O6—N2—C6—C5179.7 (6)N12—C41—C42—C37175.4 (5)
O5—N2—C6—C52.3 (8)C38—C37—C42—C410.3 (7)
O6—N2—C6—C71.9 (8)C36—C37—C42—C41176.9 (4)
O5—N2—C6—C7175.5 (6)O37—S1'—C43—S152.5 (5)
C3—C2—C7—C60.9 (7)C44—S1'—C43—S161.4 (5)
C1—C2—C7—C6178.6 (4)O37—S1—C43—S1'50.8 (5)
C5—C6—C7—C21.9 (7)C44—S1—C43—S1'59.4 (4)
N2—C6—C7—C2175.8 (4)O37—S1'—C44—S150.2 (6)
Ce2—O8—C8—O796.2 (8)C43—S1'—C44—S161.4 (5)
Ce2—O8—C8—C985.4 (8)O37—S1—C44—S1'48.3 (5)
Ce1—O7—C8—O886.0 (6)C43—S1—C44—S1'60.0 (5)
Ce1—O7—C8—C995.6 (5)O38—S2'—C45—S252.3 (5)
O8—C8—C9—C105.2 (6)C46—S2'—C45—S261.1 (4)
O7—C8—C9—C10173.4 (4)O38—S2—C45—S2'49.9 (4)
O8—C8—C9—C14171.6 (4)C46—S2—C45—S2'60.9 (4)
O7—C8—C9—C149.9 (6)O38—S2'—C46—S248.6 (5)
C14—C9—C10—C112.3 (7)C45—S2'—C46—S261.5 (4)
C8—C9—C10—C11174.5 (4)O38—S2—C46—S2'46.2 (4)
C9—C10—C11—C120.4 (7)C45—S2—C46—S2'61.2 (4)
C9—C10—C11—N3179.7 (4)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+2, z+2.

Experimental details

Crystal data
Chemical formula[Ce(C7H3N2O6)3(C2H6OS)2]
Mr929.72
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)14.3025 (10), 14.3752 (10), 21.9143 (16)
α, β, γ (°)101.8798 (9), 103.6758 (10), 119.6828 (8)
V3)3514.1 (4)
Z4
Radiation typeMo Kα
µ (mm1)1.51
Crystal size (mm)0.25 × 0.20 × 0.15
Data collection
DiffractometerBruker SMART APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.760, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
17917, 12456, 9611
Rint0.025
(sin θ/λ)max1)0.601
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.099, 1.03
No. of reflections12456
No. of parameters980
No. of restraints6
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.91, 0.69

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

 

Acknowledgements

We thank Yuncheng University and the University of Malaya for supporting this study.

References

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