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The molecular structure of the title complex, [Sm{N(SiMe3)2}3]·C4H8O, an important key compound in lanthanide chemistry, has been determined. The crystal structure analysis reveals a trigonal-pyramidal structure, isotype to other structurally characterized lanthanide tris-silyl­amides. The molecule is disordered due to the D3 site symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804016435/lh6224sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804016435/lh6224Isup2.hkl
Contains datablock I

CCDC reference: 178900

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](Si-C) = 0.007 Å
  • R factor = 0.061
  • wR factor = 0.104
  • Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... O90
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.118 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C93 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C94 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C92 PLAT301_ALERT_3_C Main Residue Disorder ......................... 10.00 Perc. PLAT324_ALERT_2_C Check for Possibly Missing H on Coordinating.... N1 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 42.79 Deg. N1 -SI1 -SM1 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 25.95 Deg. SM1 -N1 -SM1 4.664 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C18 H54 N3 Si6 Sm PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C24 H48 O6
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C22 H62 N3 O1 Si6 Sm1 Atom count from the _atom_site data: C22.08 H62.16 N3 O1.02 Si6 Sm1 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G ALERT: Large difference may be due to a symmetry error - see SYMMG tests From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C22 H62 N3 O Si6 Sm TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 44.00 44.16 -0.16 H 124.00 124.32 -0.32 N 6.00 6.00 0.00 O 2.00 2.04 -0.04 Si 12.00 12.00 0.00 Sm 2.00 2.00 0.00
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 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: X-AREA (Stoe & Cie, 2003); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

Tris[bis(trimethylsilyl)amido]samarium tetrahydrofuran solvate top
Crystal data top
[Sm(C6H18NSi2)3]·C4H8OMelting point: 158 K
Mr = 703.64Mo Kα radiation, λ = 0.71073 Å
Trigonal, P31cCell parameters from 2000 reflections
a = 16.490 (3) Åθ = 2–25°
c = 8.3485 (11) ŵ = 1.69 mm1
V = 1966.0 (6) Å3T = 193 K
Z = 2Needle, colourless
F(000) = 7380.33 × 0.06 × 0.06 mm
Dx = 1.189 Mg m3
Data collection top
Stoe IPDS-2
diffractometer
1154 independent reflections
Radiation source: fine-focus sealed tube784 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.118
ω' scansθmax = 25.0°, θmin = 1.4°
Absorption correction: multi-scan
(Blessing, 1995)
h = 1919
Tmin = 0.855, Tmax = 0.903k = 1913
8924 measured reflectionsl = 89
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)] = 0.061H-atom parameters constrained
wR(F2) = 0.104 w = 1/[σ2(Fo2) + (0.0393P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
1154 reflectionsΔρmax = 0.34 e Å3
92 parametersΔρmin = 0.92 e Å3
72 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0145 (16)
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)
Sm10.66670.33330.31171 (12)0.0458 (3)0.50
Si10.45591 (11)0.28796 (11)0.38872 (19)0.0501 (5)
N10.5101 (4)0.2551 (2)0.25000.0459 (15)
C10.5460 (4)0.3674 (4)0.5369 (7)0.0661 (17)
H1A0.59460.42060.48180.099*
H1B0.51750.38810.61480.099*
H1C0.57230.33410.58980.099*
C20.4019 (4)0.3544 (5)0.3003 (8)0.0709 (18)
H2A0.34850.31300.23670.106*
H2B0.38250.38030.38500.106*
H2C0.44710.40400.23410.106*
C30.3634 (5)0.1881 (5)0.5046 (8)0.081 (2)
H3A0.39100.15840.56450.121*
H3B0.33400.21090.57690.121*
H3C0.31740.14370.43230.121*
O900.009 (3)0.028 (3)0.305 (5)0.088 (12)0.17
C910.033 (2)0.056 (3)0.206 (7)0.111 (17)0.17
H91A0.09100.10770.25230.133*0.17
H91B0.04230.04410.09370.133*0.17
C920.051 (3)0.068 (3)0.230 (10)0.104 (14)0.17
H92A0.04060.10950.32220.125*0.17
H92B0.06140.09600.13340.125*0.17
C930.135 (2)0.027 (4)0.261 (10)0.133 (18)0.17
H93A0.18180.04270.17380.159*0.17
H93B0.16500.02620.36330.159*0.17
C940.105 (3)0.098 (3)0.267 (10)0.14 (2)0.17
H94A0.11060.13000.16340.163*0.17
H94B0.13520.14510.35380.163*0.17
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.0469 (4)0.0469 (4)0.0437 (5)0.02344 (19)0.0000.000
Si10.0546 (9)0.0597 (9)0.0392 (9)0.0311 (7)0.0043 (7)0.0012 (7)
N10.048 (3)0.052 (3)0.036 (3)0.0240 (17)0.0000.006 (3)
C10.075 (4)0.081 (4)0.050 (4)0.044 (3)0.001 (3)0.017 (3)
C20.078 (4)0.084 (5)0.065 (4)0.050 (4)0.006 (4)0.002 (4)
C30.095 (5)0.085 (4)0.066 (5)0.048 (4)0.022 (4)0.010 (4)
O900.05 (2)0.18 (3)0.051 (13)0.07 (3)0.01 (2)0.016 (17)
C910.08 (3)0.19 (4)0.06 (3)0.07 (3)0.02 (2)0.01 (3)
C920.07 (2)0.17 (3)0.09 (3)0.07 (2)0.02 (2)0.01 (3)
C930.06 (2)0.18 (3)0.11 (3)0.02 (2)0.02 (2)0.02 (3)
C940.08 (3)0.17 (3)0.10 (3)0.03 (3)0.00 (3)0.01 (3)
Geometric parameters (Å, º) top
Sm1—Sm1i1.0304 (19)C3—H3B0.9599
Sm1—N12.294 (6)C3—H3C0.9599
Sm1—C12.988 (6)O90—C911.447 (9)
Sm1—Si13.2329 (16)O90—C941.448 (9)
Si1—N11.709 (3)C91—C921.500 (9)
Si1—C31.861 (7)C91—H91A0.9900
Si1—C11.873 (6)C91—H91B0.9900
Si1—C21.875 (6)C92—C931.502 (10)
C1—H1A0.9599C92—H92A0.9900
C1—H1B0.9599C92—H92B0.9900
C1—H1C0.9599C93—C941.500 (9)
C2—H2A0.9599C93—H93A0.9900
C2—H2B0.9600C93—H93B0.9900
C2—H2C0.9599C94—H94A0.9900
C3—H3A0.9599C94—H94B0.9900
Sm1i—Sm1—N1ii77.02 (4)C2—Si1—Sm1123.8 (2)
Sm1i—Sm1—N1iii77.02 (4)Si1—N1—Si1iv126.1 (4)
N1ii—Sm1—N1iii115.11 (3)Si1—N1—Sm1i126.4 (2)
Sm1i—Sm1—N177.02 (4)Si1iv—N1—Sm1i106.81 (15)
N1ii—Sm1—N1115.11 (3)Si1—N1—Sm1106.81 (16)
N1iii—Sm1—N1115.11 (3)Si1iv—N1—Sm1126.4 (2)
Sm1i—Sm1—C1ii129.00 (13)Sm1i—N1—Sm125.95 (8)
N1ii—Sm1—C1ii65.12 (12)Si1—C1—Sm179.8 (2)
N1iii—Sm1—C1ii149.52 (14)Si1—C1—H1A109.3
N1—Sm1—C1ii89.02 (12)Sm1—C1—H1A62.6
Sm1i—Sm1—C1iii129.00 (13)Si1—C1—H1B109.8
N1ii—Sm1—C1iii89.02 (12)Sm1—C1—H1B169.7
N1iii—Sm1—C1iii65.12 (12)H1A—C1—H1B109.5
N1—Sm1—C1iii149.52 (14)Si1—C1—H1C109.4
C1ii—Sm1—C1iii84.60 (19)Sm1—C1—H1C69.4
Sm1i—Sm1—C1129.00 (13)H1A—C1—H1C109.5
N1ii—Sm1—C1149.52 (14)H1B—C1—H1C109.5
N1iii—Sm1—C189.02 (12)Si1—C2—H2A109.7
N1—Sm1—C165.12 (12)Si1—C2—H2B109.4
C1ii—Sm1—C184.60 (19)H2A—C2—H2B109.5
C1iii—Sm1—C184.60 (19)Si1—C2—H2C109.4
Sm1i—Sm1—Si1ii101.47 (3)H2A—C2—H2C109.5
N1ii—Sm1—Si1ii30.39 (4)H2B—C2—H2C109.5
N1iii—Sm1—Si1ii139.16 (3)Si1—C3—H3A109.5
N1—Sm1—Si1ii103.89 (3)Si1—C3—H3B109.4
C1ii—Sm1—Si1ii34.76 (12)H3A—C3—H3B109.5
C1iii—Sm1—Si1ii87.48 (12)Si1—C3—H3C109.5
C1—Sm1—Si1ii119.34 (13)H3A—C3—H3C109.5
Sm1i—Sm1—Si1iii101.47 (3)H3B—C3—H3C109.5
N1ii—Sm1—Si1iii103.89 (3)C91—O90—C94117.1 (16)
N1iii—Sm1—Si1iii30.39 (4)O90—C91—C9291 (3)
N1—Sm1—Si1iii139.16 (3)O90—C91—H91A113.5
C1ii—Sm1—Si1iii119.34 (13)C92—C91—H91A113.5
C1iii—Sm1—Si1iii34.76 (12)O90—C91—H91B113.5
C1—Sm1—Si1iii87.48 (12)C92—C91—H91B113.5
Si1ii—Sm1—Si1iii116.15 (2)H91A—C91—H91B110.8
Sm1i—Sm1—Si1101.47 (3)C91—C92—C93108.8 (9)
N1ii—Sm1—Si1139.16 (3)C91—C92—H92A109.9
N1iii—Sm1—Si1103.89 (3)C93—C92—H92A109.9
N1—Sm1—Si130.39 (4)C91—C92—H92B109.9
C1ii—Sm1—Si187.48 (12)C93—C92—H92B109.9
C1iii—Sm1—Si1119.34 (13)H92A—C92—H92B108.3
C1—Sm1—Si134.76 (12)C94—C93—C92108.7 (9)
Si1ii—Sm1—Si1116.15 (2)C94—C93—H93A109.9
Si1iii—Sm1—Si1116.15 (2)C92—C93—H93A109.9
N1—Si1—C3113.5 (3)C94—C93—H93B109.9
N1—Si1—C1108.2 (3)C92—C93—H93B109.9
C3—Si1—C1106.7 (3)H93A—C93—H93B108.3
N1—Si1—C2113.3 (2)O90—C94—C9392 (3)
C3—Si1—C2107.6 (3)O90—C94—H94A113.3
C1—Si1—C2107.1 (3)C93—C94—H94A113.3
N1—Si1—Sm142.79 (17)O90—C94—H94B113.3
C3—Si1—Sm1128.3 (2)C93—C94—H94B113.3
C1—Si1—Sm165.44 (19)H94A—C94—H94B110.7
Sm1i—Sm1—Si1—N136.98 (7)C1—Si1—N1—Sm13.3 (2)
N1ii—Sm1—Si1—N146.38 (9)C2—Si1—N1—Sm1115.3 (2)
N1iii—Sm1—Si1—N1116.27 (9)Sm1i—Sm1—N1—Si1142.77 (7)
C1ii—Sm1—Si1—N192.36 (14)N1ii—Sm1—N1—Si1148.48 (7)
C1iii—Sm1—Si1—N1174.72 (14)N1iii—Sm1—N1—Si174.03 (11)
C1—Sm1—Si1—N1176.5 (2)C1ii—Sm1—N1—Si186.69 (14)
Si1ii—Sm1—Si1—N172.03 (10)C1iii—Sm1—N1—Si19.1 (2)
Si1iii—Sm1—Si1—N1145.99 (7)C1—Sm1—N1—Si12.19 (15)
Sm1i—Sm1—Si1—C3121.1 (3)Si1ii—Sm1—N1—Si1118.41 (8)
N1ii—Sm1—Si1—C337.7 (3)Si1iii—Sm1—N1—Si150.17 (10)
N1iii—Sm1—Si1—C3159.7 (3)Sm1i—Sm1—N1—Si1iv46.02 (9)
N1—Sm1—Si1—C384.1 (3)N1ii—Sm1—N1—Si1iv22.72 (13)
C1ii—Sm1—Si1—C38.3 (3)N1iii—Sm1—N1—Si1iv114.77 (7)
C1iii—Sm1—Si1—C390.6 (3)C1ii—Sm1—N1—Si1iv84.51 (15)
C1—Sm1—Si1—C392.4 (4)C1iii—Sm1—N1—Si1iv162.1 (2)
Si1ii—Sm1—Si1—C312.0 (3)C1—Sm1—N1—Si1iv169.01 (17)
Si1iii—Sm1—Si1—C3129.9 (3)Si1ii—Sm1—N1—Si1iv52.79 (11)
Sm1i—Sm1—Si1—C1146.5 (2)Si1iii—Sm1—N1—Si1iv138.63 (6)
N1ii—Sm1—Si1—C1130.1 (2)Si1—Sm1—N1—Si1iv171.20 (9)
N1iii—Sm1—Si1—C167.2 (2)N1ii—Sm1—N1—Sm1i68.75 (6)
N1—Sm1—Si1—C1176.5 (2)N1iii—Sm1—N1—Sm1i68.75 (6)
C1ii—Sm1—Si1—C184.2 (3)C1ii—Sm1—N1—Sm1i130.54 (12)
C1iii—Sm1—Si1—C11.8 (3)C1iii—Sm1—N1—Sm1i151.9 (2)
Si1ii—Sm1—Si1—C1104.5 (2)C1—Sm1—N1—Sm1i144.97 (14)
Si1iii—Sm1—Si1—C137.5 (2)Si1ii—Sm1—N1—Sm1i98.82 (4)
Sm1i—Sm1—Si1—C251.7 (3)Si1iii—Sm1—N1—Sm1i92.61 (8)
N1ii—Sm1—Si1—C2135.1 (3)Si1—Sm1—N1—Sm1i142.77 (7)
N1iii—Sm1—Si1—C227.6 (3)N1—Si1—C1—Sm12.49 (18)
N1—Sm1—Si1—C288.7 (3)C3—Si1—C1—Sm1125.0 (2)
C1ii—Sm1—Si1—C2178.9 (3)C2—Si1—C1—Sm1120.0 (2)
C1iii—Sm1—Si1—C296.6 (3)Sm1i—Sm1—C1—Si144.1 (3)
C1—Sm1—Si1—C294.8 (3)N1ii—Sm1—C1—Si199.7 (3)
Si1ii—Sm1—Si1—C2160.7 (3)N1iii—Sm1—C1—Si1116.47 (19)
Si1iii—Sm1—Si1—C257.3 (3)N1—Sm1—C1—Si11.95 (14)
C3—Si1—N1—Si1iv49.6 (3)C1ii—Sm1—C1—Si193.4 (3)
C1—Si1—N1—Si1iv167.9 (2)C1iii—Sm1—C1—Si1178.4 (2)
C2—Si1—N1—Si1iv73.5 (2)Si1ii—Sm1—C1—Si194.40 (19)
Sm1—Si1—N1—Si1iv171.24 (3)Si1iii—Sm1—C1—Si1146.83 (19)
C3—Si1—N1—Sm1i140.8 (3)C94—O90—C91—C9250 (6)
C1—Si1—N1—Sm1i22.5 (2)O90—C91—C92—C9327 (5)
C2—Si1—N1—Sm1i96.1 (3)C91—C92—C93—C944 (7)
Sm1—Si1—N1—Sm1i19.21 (9)C91—O90—C94—C9348 (6)
C3—Si1—N1—Sm1121.6 (3)C92—C93—C94—O9022 (5)
Symmetry codes: (i) y+1, x+1, z1/2; (ii) y+1, xy, z; (iii) x+y+1, x+1, z; (iv) x, xy, z1/2.
 

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