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The Sm atom of the title compound, [Sm(CH4N2O)8]I3, is eight-coordinate, with eight monodentate urea ligands bound through their O atoms; the corresponding polyhedron is a distorted double-capped trigonal prism. All the urea mol­ecules are involved in intramolecular hydrogen bonds. This compound is a rare example of a lanthanide complex containing no water and in which the anions do not serve as ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805006781/sj6053sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805006781/sj6053Isup2.hkl
Contains datablock I

CCDC reference: 270524

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](N-C) = 0.008 Å
  • Disorder in main residue
  • R factor = 0.036
  • wR factor = 0.058
  • Data-to-parameter ratio = 21.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C8
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293 PLAT200_ALERT_1_C Check the Reported cell_ambient_temperature .... 293 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Sm1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C3 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C6 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C7 PLAT301_ALERT_3_C Main Residue Disorder ......................... 6.00 Perc. PLAT420_ALERT_2_C D-H Without Acceptor N11 - H11A ... ? PLAT420_ALERT_2_C D-H Without Acceptor N11 - H11B ... ? PLAT420_ALERT_2_C D-H Without Acceptor N22 - H22A ... ? PLAT420_ALERT_2_C D-H Without Acceptor N31 - H31A ... ? PLAT420_ALERT_2_C D-H Without Acceptor N31 - H31B ... ? PLAT420_ALERT_2_C D-H Without Acceptor N51 - H51B ... ? PLAT420_ALERT_2_C D-H Without Acceptor N52 - H52B ... ? PLAT420_ALERT_2_C D-H Without Acceptor N72 - H72B ... ?
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 17 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 14 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Octaureasamarium(III) triiodide top
Crystal data top
[Sm(CH4N2O)8]I3Z = 2
Mr = 1011.55F(000) = 954
Triclinic, P1Dx = 2.173 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.597 (5) ÅCell parameters from 25 reflections
b = 11.996 (11) Åθ = 12–13°
c = 13.046 (6) ŵ = 4.95 mm1
α = 85.58 (6)°T = 293 K
β = 73.76 (4)°Prism, yellow
γ = 76.20 (7)°0.23 × 0.21 × 0.19 mm
V = 1546.2 (17) Å3
Data collection top
Enraf–Nonius CAD-4
diffractometer
4875 reflections with I > 2σ(I)
Radiation source: Enraf Nonius FR590Rint = 0.000
Graphite monochromatorθmax = 28.0°, θmin = 1.6°
non–profiled ω scansh = 1313
Absorption correction: ψ scan
(North et al., 1968)
k = 1515
Tmin = 0.325, Tmax = 0.394l = 017
7442 measured reflections1 standard reflections every 60 min
7442 independent reflections intensity decay: 2%
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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058H-atom parameters constrained
S = 0.93 w = 1/[σ2(Fo2) + (0.0192P)2]
where P = (Fo2 + 2Fc2)/3
7442 reflections(Δ/σ)max < 0.001
344 parametersΔρmax = 1.12 e Å3
0 restraintsΔρmin = 1.21 e Å3
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)
Sm10.65000 (3)0.23710 (2)0.299191 (19)0.02667 (6)
I10.05607 (4)0.32884 (3)0.69067 (3)0.04692 (10)
I20.38712 (4)0.88576 (3)0.18637 (3)0.04688 (10)
I30.80742 (5)0.65329 (4)0.05948 (3)0.05726 (13)
O10.4953 (4)0.2305 (3)0.4719 (3)0.0435 (9)
C10.3821 (6)0.2777 (5)0.5318 (5)0.0481 (15)
N110.3585 (6)0.2738 (5)0.6372 (4)0.0674 (16)
H11A0.42100.23860.66600.081*
H11B0.28060.30650.67680.081*
N120.2833 (5)0.3306 (5)0.4917 (4)0.0782 (19)
H12A0.29510.33360.42370.094*
H12B0.20650.36250.53340.094*
O20.4260 (4)0.2894 (3)0.2676 (3)0.0452 (10)
C20.3752 (5)0.3008 (5)0.1891 (4)0.0420 (13)
N210.4057 (5)0.2192 (4)0.1202 (4)0.0604 (15)
H21A0.46140.15590.12740.073*
H21B0.37030.22850.06750.073*
N220.2846 (6)0.3937 (5)0.1800 (5)0.083 (2)
H22A0.25980.44670.22710.099*
H22B0.24980.40190.12690.099*
O30.8807 (4)0.1562 (3)0.2022 (3)0.0446 (9)
C30.9926 (5)0.1042 (5)0.2099 (4)0.0423 (14)
N311.0973 (5)0.1519 (5)0.1895 (4)0.0631 (15)
H31A1.08890.22280.16980.076*
H31B1.17380.11220.19590.076*
N321.0156 (6)0.0063 (5)0.2404 (5)0.089 (2)
H32A0.95140.04220.25510.107*
H32B1.09460.04130.24530.107*
O40.6407 (4)0.0949 (3)0.1860 (3)0.0437 (9)
C40.7085 (6)0.0013 (5)0.1505 (4)0.0400 (13)
N410.7551 (5)0.0848 (4)0.2136 (4)0.0526 (13)
H41A0.73860.07310.28080.063*
H41B0.80150.15010.18700.063*
N420.7390 (6)0.0242 (4)0.0475 (4)0.0683 (17)
H42A0.71200.02750.00400.082*
H42B0.78570.09070.02410.082*
O50.5595 (4)0.4363 (3)0.3558 (3)0.0378 (9)
C50.4820 (5)0.5255 (5)0.3344 (4)0.0368 (12)
N510.4871 (5)0.5594 (4)0.2342 (3)0.0544 (14)
H51A0.54470.51950.18230.065*
H51B0.43290.62110.22120.065*
N520.3902 (5)0.5893 (4)0.4101 (4)0.0601 (15)
H52A0.38240.56980.47600.072*
H52B0.33780.65040.39370.072*
O60.7128 (4)0.0592 (3)0.3962 (3)0.0454 (10)
C60.7167 (6)0.0460 (5)0.4916 (4)0.0464 (15)
N610.7867 (6)0.1027 (5)0.5293 (4)0.0696 (17)
H61A0.82980.14880.48830.084*
H61B0.78910.09330.59480.084*
N620.6485 (7)0.0228 (5)0.5574 (4)0.078 (2)
H62A0.60090.05900.53460.094*
H62B0.65210.03110.62260.094*
O70.8039 (4)0.3030 (3)0.3774 (3)0.0378 (8)
C70.8786 (5)0.3729 (5)0.3471 (4)0.0334 (11)
N710.9545 (5)0.3921 (4)0.4062 (4)0.0596 (15)
H71A0.95300.35640.46620.072*
H71B1.00530.44020.38460.072*
N720.8868 (5)0.4303 (4)0.2553 (4)0.0561 (14)
H72A0.83980.42030.21410.067*
H72B0.93900.47760.23700.067*
O80.6919 (4)0.3461 (3)0.1368 (3)0.0428 (9)
C80.7394 (7)0.3285 (5)0.0375 (4)0.0463 (15)
N810.8661 (13)0.3389 (12)0.0130 (9)0.077 (5)0.576 (10)
H81A0.91520.35760.02230.093*0.576 (10)
H81B0.89760.32680.08050.093*0.576 (10)
N820.6709 (15)0.3021 (13)0.0200 (10)0.095 (6)0.576 (10)
H82A0.58940.29570.00870.114*0.576 (10)
H82B0.70660.29080.08730.114*0.576 (10)
N830.836 (2)0.2461 (19)0.0055 (13)0.096 (9)0.424 (12)
H83A0.87420.19630.03380.115*0.424 (12)
H83B0.86220.24010.07380.115*0.424 (12)
N840.665 (2)0.3904 (17)0.0258 (13)0.090 (9)0.424 (12)
H84A0.59090.43810.00210.108*0.424 (12)
H84B0.69290.38180.09390.108*0.424 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.02722 (13)0.02752 (15)0.02331 (12)0.00368 (11)0.00522 (10)0.00240 (10)
I10.0487 (2)0.0512 (3)0.0378 (2)0.0138 (2)0.00523 (17)0.00174 (17)
I20.0419 (2)0.0487 (3)0.0461 (2)0.00208 (19)0.01232 (18)0.00081 (18)
I30.0793 (3)0.0421 (3)0.0484 (2)0.0011 (2)0.0261 (2)0.00208 (19)
O10.039 (2)0.050 (3)0.0325 (19)0.0043 (19)0.0004 (17)0.0015 (17)
C10.045 (4)0.041 (4)0.049 (4)0.014 (3)0.004 (3)0.005 (3)
N110.073 (4)0.084 (4)0.034 (3)0.024 (3)0.010 (3)0.001 (3)
N120.048 (3)0.097 (5)0.058 (3)0.015 (3)0.009 (3)0.006 (3)
O20.040 (2)0.059 (3)0.038 (2)0.006 (2)0.0151 (18)0.0083 (18)
C20.036 (3)0.051 (4)0.041 (3)0.012 (3)0.012 (3)0.005 (3)
N210.067 (4)0.053 (3)0.064 (3)0.015 (3)0.039 (3)0.023 (3)
N220.104 (5)0.061 (4)0.090 (4)0.025 (4)0.067 (4)0.026 (3)
O30.035 (2)0.048 (3)0.042 (2)0.0025 (19)0.0066 (17)0.0004 (18)
C30.029 (3)0.057 (4)0.031 (3)0.002 (3)0.003 (2)0.006 (3)
N310.039 (3)0.055 (4)0.093 (4)0.007 (3)0.018 (3)0.004 (3)
N320.051 (4)0.071 (5)0.147 (6)0.016 (3)0.037 (4)0.046 (4)
O40.057 (3)0.031 (2)0.046 (2)0.0032 (19)0.021 (2)0.0101 (17)
C40.043 (3)0.038 (3)0.043 (3)0.009 (3)0.018 (3)0.006 (3)
N410.078 (4)0.036 (3)0.045 (3)0.010 (3)0.021 (3)0.001 (2)
N420.097 (5)0.051 (4)0.043 (3)0.015 (3)0.021 (3)0.009 (3)
O50.044 (2)0.034 (2)0.0332 (19)0.0000 (18)0.0130 (17)0.0058 (16)
C50.038 (3)0.038 (3)0.038 (3)0.012 (3)0.011 (2)0.005 (2)
N510.067 (4)0.045 (3)0.045 (3)0.009 (3)0.024 (3)0.000 (2)
N520.060 (4)0.050 (3)0.054 (3)0.017 (3)0.011 (3)0.014 (3)
O60.062 (3)0.035 (2)0.0311 (19)0.0059 (19)0.0133 (19)0.0010 (16)
C60.067 (4)0.039 (3)0.030 (3)0.004 (3)0.015 (3)0.002 (2)
N610.091 (5)0.088 (5)0.048 (3)0.042 (4)0.036 (3)0.023 (3)
N620.138 (6)0.074 (4)0.043 (3)0.060 (4)0.034 (4)0.025 (3)
O70.037 (2)0.043 (2)0.0372 (19)0.0117 (18)0.0157 (17)0.0036 (17)
C70.027 (3)0.037 (3)0.034 (3)0.002 (2)0.008 (2)0.003 (2)
N710.071 (4)0.085 (4)0.044 (3)0.049 (3)0.027 (3)0.014 (3)
N720.073 (4)0.063 (4)0.047 (3)0.032 (3)0.031 (3)0.020 (3)
O80.058 (3)0.037 (2)0.0282 (19)0.0054 (19)0.0090 (18)0.0013 (16)
C80.066 (4)0.038 (4)0.034 (3)0.014 (3)0.012 (3)0.003 (3)
N810.060 (7)0.119 (17)0.042 (6)0.010 (8)0.002 (5)0.032 (7)
N820.108 (13)0.16 (2)0.051 (7)0.086 (15)0.022 (7)0.004 (9)
N830.108 (16)0.12 (2)0.031 (7)0.029 (15)0.010 (8)0.024 (9)
N840.136 (17)0.084 (17)0.041 (8)0.013 (14)0.042 (10)0.005 (9)
Geometric parameters (Å, º) top
Sm1—O42.378 (4)N42—H42B0.8600
Sm1—O82.391 (4)O5—C51.250 (6)
Sm1—O12.395 (4)C5—N521.315 (7)
Sm1—O32.418 (4)C5—N511.329 (6)
Sm1—O52.441 (4)N51—H51A0.8600
Sm1—O62.445 (4)N51—H51B0.8600
Sm1—O22.448 (4)N52—H52A0.8600
Sm1—O72.448 (3)N52—H52B0.8600
O1—C11.261 (6)O6—C61.253 (6)
C1—N121.308 (7)C6—N611.323 (7)
C1—N111.327 (7)C6—N621.330 (7)
N11—H11A0.8600N61—H61A0.8600
N11—H11B0.8600N61—H61B0.8600
N12—H12A0.8600N62—H62A0.8600
N12—H12B0.8600N62—H62B0.8600
O2—C21.268 (6)O7—C71.256 (6)
C2—N211.302 (7)C7—N711.325 (6)
C2—N221.308 (7)C7—N721.327 (6)
N21—H21A0.8600N71—H71A0.8600
N21—H21B0.8600N71—H71B0.8600
N22—H22A0.8600N72—H72A0.8600
N22—H22B0.8600N72—H72B0.8600
O3—C31.229 (6)O8—C81.266 (6)
C3—N311.321 (7)C8—N821.281 (12)
C3—N321.339 (8)C8—N811.350 (14)
N31—H31A0.8600N81—H81A0.8600
N31—H31B0.8600N81—H81B0.8600
N32—H32A0.8600N82—H82A0.8600
N32—H32B0.8600N82—H82B0.8600
O4—C41.250 (6)C8—N831.271 (19)
C4—N421.327 (6)C8—N841.356 (17)
C4—N411.337 (6)N83—H83A0.8600
N41—H41A0.8600N83—H83B0.8600
N41—H41B0.8600N84—H84A0.8600
N42—H42A0.8600N84—H84B0.8600
O4—Sm1—O883.47 (13)O4—C4—N42120.9 (5)
O4—Sm1—O1110.92 (14)O4—C4—N41122.0 (5)
O8—Sm1—O1143.97 (13)N42—C4—N41117.1 (5)
O4—Sm1—O373.70 (14)C4—N41—H41A120.0
O8—Sm1—O374.11 (14)C4—N41—H41B120.0
O1—Sm1—O3140.82 (12)H41A—N41—H41B120.0
O4—Sm1—O5144.63 (12)C4—N42—H42A120.0
O8—Sm1—O575.80 (13)C4—N42—H42B120.0
O1—Sm1—O574.12 (14)H42A—N42—H42B120.0
O3—Sm1—O5125.50 (14)C5—O5—Sm1140.2 (3)
O4—Sm1—O677.56 (13)O5—C5—N52121.5 (5)
O8—Sm1—O6147.96 (13)O5—C5—N51121.5 (5)
O1—Sm1—O667.82 (14)N52—C5—N51117.0 (5)
O3—Sm1—O675.90 (14)C5—N51—H51A120.0
O5—Sm1—O6132.43 (12)C5—N51—H51B120.0
O4—Sm1—O273.05 (14)H51A—N51—H51B120.0
O8—Sm1—O278.41 (14)C5—N52—H52A120.0
O1—Sm1—O274.99 (12)C5—N52—H52B120.0
O3—Sm1—O2138.70 (12)H52A—N52—H52B120.0
O5—Sm1—O274.90 (13)C6—O6—Sm1128.8 (3)
O6—Sm1—O2119.21 (14)O6—C6—N61120.3 (6)
O4—Sm1—O7142.61 (13)O6—C6—N62120.9 (6)
O8—Sm1—O796.62 (13)N61—C6—N62118.7 (5)
O1—Sm1—O790.86 (13)C6—N61—H61A120.0
O3—Sm1—O770.47 (13)C6—N61—H61B120.0
O5—Sm1—O769.19 (13)H61A—N61—H61B120.0
O6—Sm1—O783.67 (13)C6—N62—H62A120.0
O2—Sm1—O7143.82 (13)C6—N62—H62B120.0
C1—O1—Sm1144.7 (4)H62A—N62—H62B120.0
O1—C1—N12120.9 (6)C7—O7—Sm1133.5 (3)
O1—C1—N11121.3 (6)O7—C7—N71120.9 (5)
N12—C1—N11117.8 (6)O7—C7—N72122.4 (4)
C1—N11—H11A120.0N71—C7—N72116.7 (5)
C1—N11—H11B120.0C7—N71—H71A120.0
H11A—N11—H11B120.0C7—N71—H71B120.0
C1—N12—H12A120.0H71A—N71—H71B120.0
C1—N12—H12B120.0C7—N72—H72A120.0
H12A—N12—H12B120.0C7—N72—H72B120.0
C2—O2—Sm1138.2 (3)H72A—N72—H72B120.0
O2—C2—N21121.4 (5)C8—O8—Sm1138.6 (4)
O2—C2—N22119.6 (5)O8—C8—N82122.6 (10)
N21—C2—N22118.9 (5)O8—C8—N81120.6 (8)
C2—N21—H21A120.0N82—C8—N81116.8 (9)
C2—N21—H21B120.0C8—N81—H81A120.0
H21A—N21—H21B120.0C8—N81—H81B120.0
C2—N22—H22A120.0H81A—N81—H81B120.0
C2—N22—H22B120.0C8—N82—H82A120.0
H22A—N22—H22B120.0C8—N82—H82B120.0
C3—O3—Sm1145.3 (3)H82A—N82—H82B120.0
O3—C3—N31123.2 (6)O8—C8—N83125.6 (11)
O3—C3—N32121.3 (6)O8—C8—N84116.1 (12)
N31—C3—N32115.5 (5)N83—C8—N84117.2 (13)
C3—N31—H31A120.0C8—N83—H83A120.0
C3—N31—H31B120.0C8—N83—H83B120.0
H31A—N31—H31B120.0H83A—N83—H83B120.0
C3—N32—H32A120.0C8—N84—H84A120.0
C3—N32—H32B120.0C8—N84—H84B120.0
H32A—N32—H32B120.0H84A—N84—H84B120.0
C4—O4—Sm1138.4 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N12—H12A···O20.862.142.910 (8)149
N21—H21A···O40.862.192.895 (8)139
N32—H32A···N410.862.463.234 (10)150
N41—H41A···O60.862.192.920 (8)143
N51—H51A···O80.862.293.030 (8)145
N52—H52A···O5i0.862.433.224 (7)154
N52—H52A···O7i0.862.603.111 (8)119
N61—H61A···O70.862.273.002 (8)143
N62—H62A···O1ii0.862.523.310 (9)153
N72—H72A···O80.862.443.270 (8)163
N82—H82A···N210.862.413.227 (15)159
N83—H83A···O30.862.232.959 (17)143
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+1.
 

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