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The title compound, poly[samarium(III)-tri-μ-formato], [Sm(HCO2)3]n, is isostructural with numerous lanthanide formates and comprises a three-dimensional framework assembled from SmO9 polyhedra and HCO2 anions. The Sm atom lies on a site of 3m symmetry and is coordinated by nine O atoms in a typical coordination geometry. The formate anions lie on mirror planes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806025608/bi2026sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806025608/bi2026Isup2.hkl
Contains datablock I

CCDC reference: 618125

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](O-C) = 0.010 Å
  • R factor = 0.027
  • wR factor = 0.061
  • Data-to-parameter ratio = 8.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96 PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 1 PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.36 Ratio
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.96 From the CIF: _reflns_number_total 201 Count of symmetry unique reflns 132 Completeness (_total/calc) 152.27% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 69 Fraction of Friedel pairs measured 0.523 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 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 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

poly[samarium(III)-tri-µ-formato] top
Crystal data top
[Sm(HCO2)3]Dx = 3.715 Mg m3
Mr = 285.40Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3mCell parameters from 56 reflections
Hall symbol: R 3 -2"θ = 3.9–28.1°
a = 10.503 (3) ŵ = 11.47 mm1
c = 4.006 (3) ÅT = 293 K
V = 382.7 (3) Å3Needle, colourless
Z = 30.06 × 0.04 × 0.04 mm
F(000) = 393
Data collection top
Bruker APEXII CCD
diffractometer
201 independent reflections
Radiation source: fine-focus sealed tube201 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
ω scansθmax = 29.0°, θmin = 3.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 1312
Tmin = 0.546, Tmax = 0.657k = 1313
825 measured reflectionsl = 53
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027All H-atom parameters refined
wR(F2) = 0.061 w = 1/[σ2(Fo2) + (0.0348P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.007
201 reflectionsΔρmax = 1.95 e Å3
25 parametersΔρmin = 1.25 e Å3
4 restraintsAbsolute structure: Flack (1983), 69 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.01 (9)
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*/Ueq
Sm10.66670.33330.1791 (5)0.0113 (3)
O10.7991 (5)0.2009 (5)0.164 (2)0.023 (2)
O20.9145 (5)0.0855 (5)0.343 (2)0.0163 (18)
C10.8459 (7)0.1541 (7)0.386 (3)0.018 (2)
H10.830 (2)0.170 (2)0.614 (7)0.021*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.0121 (3)0.0121 (3)0.0096 (4)0.00605 (15)0.0000.000
O10.030 (4)0.030 (4)0.016 (5)0.021 (4)0.0019 (18)0.0019 (18)
O20.015 (3)0.015 (3)0.018 (5)0.007 (4)0.0001 (17)0.0001 (17)
C10.020 (4)0.020 (4)0.014 (6)0.012 (5)0.000 (2)0.000 (2)
Geometric parameters (Å, º) top
Sm1—O12.409 (10)Sm1—O2viii2.543 (9)
Sm1—O2i2.543 (9)Sm1—Sm1ix4.006 (3)
Sm1—O1ii2.409 (10)Sm1—Sm1x4.006 (3)
Sm1—O1iii2.409 (10)O1—C11.235 (16)
Sm1—O2iv2.529 (9)O2—C11.259 (16)
Sm1—O2v2.529 (9)O2—Sm1xi2.529 (9)
Sm1—O2vi2.529 (9)O2—Sm1xii2.543 (9)
Sm1—O2vii2.543 (9)C1—H10.96 (2)
O1—Sm1—O1ii119.93 (2)O2vi—Sm1—O2viii144.27 (13)
O1—Sm1—O1iii119.93 (2)O2iv—Sm1—O2i144.27 (13)
O1—Sm1—O2i126.2 (3)O2v—Sm1—O2i144.27 (13)
O1—Sm1—O2vi129.4 (3)O2iv—Sm1—O2viii104.3 (3)
O1—Sm1—O2vii71.0 (2)O2vi—Sm1—O2i104.3 (3)
O1—Sm1—O2v73.3 (2)O1—Sm1—Sm1ix88.5 (2)
O1—Sm1—O2viii71.0 (2)O1iii—Sm1—Sm1ix88.5 (2)
O1—Sm1—O2iv73.3 (2)O1ii—Sm1—Sm1ix88.5 (2)
O2iv—Sm1—O2v64.4 (3)O2iv—Sm1—Sm1ix142.0 (2)
O2vi—Sm1—O2vii144.27 (13)O2v—Sm1—Sm1ix142.0 (2)
O2v—Sm1—O2vii104.3 (3)O2vi—Sm1—Sm1ix142.0 (2)
O2vii—Sm1—O2viii64.0 (3)O2vii—Sm1—Sm1ix37.7 (2)
O1iii—Sm1—O1ii119.93 (2)O2viii—Sm1—Sm1ix37.7 (2)
O1ii—Sm1—O2vii126.2 (3)O2i—Sm1—Sm1ix37.7 (2)
O1iii—Sm1—O2viii126.2 (3)O1—Sm1—Sm1x91.5 (2)
O1iii—Sm1—O2iv129.4 (3)O1iii—Sm1—Sm1x91.5 (2)
O1ii—Sm1—O2v129.4 (3)O1ii—Sm1—Sm1x91.5 (2)
O1iii—Sm1—O2vii71.0 (2)O2iv—Sm1—Sm1x38.0 (2)
O1ii—Sm1—O2viii71.0 (2)O2v—Sm1—Sm1x38.0 (2)
O1iii—Sm1—O2i71.0 (2)O2vi—Sm1—Sm1x38.0 (2)
O1ii—Sm1—O2i71.0 (2)O2vii—Sm1—Sm1x142.3 (2)
O1ii—Sm1—O2iv73.3 (2)O2viii—Sm1—Sm1x142.3 (2)
O1iii—Sm1—O2v73.3 (2)O2i—Sm1—Sm1x142.3 (2)
O1iii—Sm1—O2vi73.3 (2)Sm1ix—Sm1—Sm1x180.0
O1ii—Sm1—O2vi73.3 (2)C1—O1—Sm1132.2 (9)
O2iv—Sm1—O2vi64.4 (3)C1—O2—Sm1xi135.8 (9)
O2v—Sm1—O2vi64.4 (3)C1—O2—Sm1xii119.9 (8)
O2vii—Sm1—O2i64.0 (3)Sm1xi—O2—Sm1xii104.3 (3)
O2viii—Sm1—O2i64.0 (3)O1—C1—O2125.8 (13)
O2iv—Sm1—O2vii144.28 (13)O1—C1—H1118 (2)
O2v—Sm1—O2viii144.28 (13)O2—C1—H1116 (2)
Symmetry codes: (i) x1/3, y+1/3, z2/3; (ii) y+1, xy, z; (iii) x+y+1, x+1, z; (iv) x+y+5/3, x+4/3, z+1/3; (v) y+2/3, xy2/3, z+1/3; (vi) x1/3, y+1/3, z+1/3; (vii) y+2/3, xy2/3, z2/3; (viii) x+y+5/3, x+4/3, z2/3; (ix) x, y, z1; (x) x, y, z+1; (xi) x+1/3, y1/3, z1/3; (xii) x+1/3, y1/3, z+2/3.
 

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