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A novel (3,9)-connected lanthanide-based network of lanthanum trinitrite, La(NO2)3, was synthesized and characterized by single-crystal X-ray diffraction. The central LaIII atom is coordinated by nine O atoms from nine nitrite anions. These unidentate O atoms are arranged in a capped trigonal prism. The resulting [LaO9] polyhedron shows 3m symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804000297/wm6006sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804000297/wm6006Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • R factor = 0.013
  • wR factor = 0.029
  • Data-to-parameter ratio = 8.9

checkCIF/PLATON results

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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 26.99 From the CIF: _reflns_number_total 195 Count of symmetry unique reflns 114 Completeness (_total/calc) 171.05% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 81 Fraction of Friedel pairs measured 0.711 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 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

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Lanthanum(III) nitrite top
Crystal data top
La(NO2)3Dx = 3.447 Mg m3
Mr = 276.94Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3mCell parameters from 746 reflections
Hall symbol: R 3 -2"θ = 3.8–28.0°
a = 10.6226 (19) ŵ = 7.99 mm1
c = 4.0954 (15) ÅT = 273 K
V = 400.21 (18) Å3Needle, colorless
Z = 30.12 × 0.01 × 0.01 mm
F(000) = 378
Data collection top
Bruker SMART APEX 2000
diffractometer
195 independent reflections
Radiation source: fine-focus sealed tube195 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
φ and ω scansθmax = 27.0°, θmin = 3.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1313
Tmin = 0.447, Tmax = 0.924k = 1013
738 measured reflectionsl = 35
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)] = 0.013 w = 1/[σ2(Fo2) + (0.0156P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.029(Δ/σ)max = 0.025
S = 1.14Δρmax = 0.35 e Å3
195 reflectionsΔρmin = 0.45 e Å3
22 parametersAbsolute structure: Flack (1983), 40 Friedel pairs
1 restraintAbsolute structure parameter: 0.06 (5)
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
La10.00000.00000.27230.00817 (6)
O10.3960 (3)0.19798 (15)0.9551 (7)0.0199 (7)
O20.1705 (3)0.08523 (13)0.7754 (7)0.0125 (5)
N10.3069 (4)0.15346 (18)0.7324 (10)0.0218 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La10.00908 (7)0.00908 (7)0.00635 (12)0.00454 (3)0.0000.000
O10.0113 (11)0.0282 (11)0.0146 (17)0.0057 (6)0.0032 (11)0.0016 (5)
O20.0066 (10)0.0155 (9)0.0124 (13)0.0033 (5)0.0006 (9)0.0003 (4)
N10.0188 (15)0.0255 (12)0.0189 (18)0.0094 (8)0.0004 (13)0.0002 (6)
Geometric parameters (Å, º) top
La1—O1i2.491 (3)La1—O22.589 (3)
La1—O1ii2.491 (3)La1—La1iv4.0954 (15)
La1—O1iii2.491 (3)La1—La1ix4.0954 (15)
La1—O2iv2.569 (3)O1—N11.226 (5)
La1—O2v2.569 (3)O1—La1x2.491 (3)
La1—O2vi2.569 (3)O2—N11.268 (4)
La1—O2vii2.589 (3)O2—La1ix2.569 (3)
La1—O2viii2.589 (3)
O1i—La1—O1ii119.932 (6)O1iii—La1—O271.11 (6)
O1i—La1—O1iii119.930 (6)O2iv—La1—O2105.11 (9)
O1ii—La1—O1iii119.930 (6)O2v—La1—O2144.60 (4)
O1i—La1—O2iv73.50 (6)O2vi—La1—O2144.60 (4)
O1ii—La1—O2iv129.13 (9)O2vii—La1—O263.27 (10)
O1iii—La1—O2iv73.50 (6)O2viii—La1—O263.27 (10)
O1i—La1—O2v73.50 (6)O1i—La1—La1iv91.52 (6)
O1ii—La1—O2v73.50 (6)O1ii—La1—La1iv91.52 (6)
O1iii—La1—O2v129.13 (9)O1iii—La1—La1iv91.52 (6)
O2iv—La1—O2v63.82 (10)O2iv—La1—La1iv37.61 (6)
O1i—La1—O2vi129.13 (9)O2v—La1—La1iv37.61 (6)
O1ii—La1—O2vi73.50 (6)O2vi—La1—La1iv37.61 (6)
O1iii—La1—O2vi73.50 (6)O2vii—La1—La1iv142.72 (6)
O2iv—La1—O2vi63.82 (10)O2viii—La1—La1iv142.72 (6)
O2v—La1—O2vi63.82 (10)O2—La1—La1iv142.72 (6)
O1i—La1—O2vii125.76 (9)O1i—La1—La1ix88.48 (6)
O1ii—La1—O2vii71.11 (6)O1ii—La1—La1ix88.48 (6)
O1iii—La1—O2vii71.11 (6)O1iii—La1—La1ix88.48 (6)
O2iv—La1—O2vii144.60 (4)O2iv—La1—La1ix142.39 (6)
O2v—La1—O2vii144.60 (4)O2v—La1—La1ix142.39 (6)
O2vi—La1—O2vii105.11 (9)O2vi—La1—La1ix142.39 (6)
O1i—La1—O2viii71.11 (6)O2vii—La1—La1ix37.28 (6)
O1ii—La1—O2viii71.11 (6)O2viii—La1—La1ix37.28 (6)
O1iii—La1—O2viii125.76 (9)O2—La1—La1ix37.28 (6)
O2iv—La1—O2viii144.60 (4)La1iv—La1—La1ix180.0
O2v—La1—O2viii105.11 (9)N1—O1—La1x130.4 (2)
O2vi—La1—O2viii144.60 (4)N1—O2—La1ix135.6 (3)
O2vii—La1—O2viii63.27 (10)N1—O2—La1119.3 (2)
O1i—La1—O271.11 (6)La1ix—O2—La1105.11 (9)
O1ii—La1—O2125.76 (9)O1—N1—O2124.0 (4)
Symmetry codes: (i) x+y1/3, x2/3, z2/3; (ii) x+2/3, y+1/3, z2/3; (iii) y1/3, xy+1/3, z2/3; (iv) x, y, z1; (v) y, xy, z1; (vi) x+y, x, z1; (vii) x+y, x, z; (viii) y, xy, z; (ix) x, y, z+1; (x) x2/3, y1/3, z+2/3.
 

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