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In the title compound, [Yb(NO3)3(C12H8N2)2], two bidentate 1,10-phenanthroline ligands and three bidentate nitrate anions are coordinated to the Yb cation. A crystallographic twofold rotation axis passes through the Yb atom and one nitrate group. The mol­ecules are linked into a three-dimensional network by five C—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051105/at2172sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051105/at2172Isup2.hkl
Contains datablock I

CCDC reference: 633586

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.014 Å
  • R factor = 0.033
  • wR factor = 0.079
  • Data-to-parameter ratio = 11.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Yb1 - O2 .. 6.15 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Yb1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15 PLAT480_ALERT_4_C Long H...A H-Bond Reported H12 .. O3 .. 2.67 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H12 .. O2 .. 2.70 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H2 .. O4 .. 2.71 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Tris(nitrato-κ2O,O')bis(1,10-phenanthroline-κ2N,N')ytterbium(III) top
Crystal data top
[Yb(NO3)3(C12H8N2)2]F(000) = 1404
Mr = 719.48Dx = 1.916 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2949 reflections
a = 9.456 (2) Åθ = 2.4–26.2°
b = 15.451 (3) ŵ = 3.82 mm1
c = 17.104 (3) ÅT = 298 K
β = 93.687 (2)°Block, yellow
V = 2493.8 (8) Å30.46 × 0.16 × 0.10 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
2162 independent reflections
Radiation source: fine-focus sealed tube1885 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
φ and ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1110
Tmin = 0.273, Tmax = 0.701k = 1518
6189 measured reflectionsl = 2018
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)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.044P)2 + 0.0077P]
where P = (Fo2 + 2Fc2)/3
2162 reflections(Δ/σ)max = 0.001
187 parametersΔρmax = 1.00 e Å3
48 restraintsΔρmin = 0.68 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*/Ueq
Yb10.50000.61150 (2)0.75000.03514 (15)
N10.6266 (6)0.5849 (3)0.6021 (3)0.0463 (13)
N20.50000.4283 (6)0.75000.070 (3)
N30.4766 (6)0.7479 (3)0.8302 (3)0.0495 (13)
N40.7217 (5)0.6571 (4)0.8203 (3)0.0489 (13)
O10.7012 (5)0.6019 (3)0.6641 (3)0.0557 (12)
O20.4980 (4)0.5693 (3)0.6118 (3)0.0508 (11)
O30.6759 (6)0.5873 (4)0.5387 (3)0.0744 (16)
O40.3890 (6)0.4720 (3)0.7386 (3)0.0689 (14)
O50.50000.3496 (5)0.75000.105 (3)
C10.3567 (9)0.7902 (5)0.8357 (4)0.068 (2)
H10.27570.76790.80920.082*
C20.3432 (14)0.8659 (6)0.8785 (6)0.095 (3)
H20.25600.89280.88270.113*
C30.4633 (16)0.8979 (6)0.9133 (6)0.102 (3)
H30.45810.94950.94100.122*
C40.5958 (12)0.8582 (6)0.9103 (5)0.083 (3)
C50.5967 (9)0.7797 (4)0.8673 (4)0.059 (2)
C60.7252 (8)0.7322 (5)0.8630 (4)0.060 (2)
C70.8521 (10)0.7627 (7)0.9022 (4)0.082 (3)
C80.9682 (11)0.7139 (8)0.8988 (5)0.095 (3)
H81.05260.73320.92380.114*
C90.9672 (9)0.6371 (8)0.8599 (5)0.088 (3)
H91.04820.60290.86000.105*
C100.8394 (8)0.6105 (6)0.8191 (4)0.070 (2)
H100.83800.55910.79080.085*
C110.7269 (16)0.8856 (6)0.9481 (6)0.105 (4)
H110.72780.93610.97770.126*
C120.8447 (13)0.8440 (7)0.9435 (5)0.102 (3)
H120.92730.86720.96760.123*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Yb10.0255 (2)0.0408 (2)0.0380 (2)0.0000.00690 (14)0.000
N10.045 (3)0.052 (3)0.042 (3)0.013 (2)0.002 (3)0.003 (2)
N20.108 (9)0.049 (5)0.056 (6)0.0000.027 (6)0.000
N30.065 (4)0.046 (3)0.038 (3)0.007 (3)0.002 (3)0.000 (2)
N40.035 (3)0.075 (4)0.036 (3)0.006 (3)0.006 (2)0.009 (3)
O10.034 (2)0.094 (4)0.039 (3)0.002 (2)0.0018 (19)0.001 (2)
O20.035 (2)0.058 (3)0.058 (3)0.004 (2)0.006 (2)0.006 (2)
O30.085 (4)0.095 (4)0.046 (3)0.020 (3)0.023 (3)0.006 (3)
O40.065 (3)0.060 (3)0.081 (4)0.016 (3)0.004 (3)0.011 (3)
O50.183 (11)0.038 (4)0.100 (7)0.0000.042 (7)0.000
C10.097 (6)0.065 (5)0.042 (4)0.033 (4)0.000 (4)0.002 (4)
C20.136 (8)0.078 (5)0.069 (5)0.038 (5)0.002 (5)0.001 (4)
C30.165 (9)0.064 (5)0.076 (6)0.011 (6)0.000 (6)0.004 (4)
C40.131 (7)0.070 (5)0.046 (4)0.029 (5)0.012 (4)0.000 (4)
C50.096 (6)0.046 (4)0.034 (4)0.020 (4)0.009 (4)0.006 (3)
C60.074 (5)0.073 (5)0.030 (4)0.043 (4)0.010 (3)0.012 (3)
C70.084 (6)0.113 (6)0.046 (4)0.051 (5)0.015 (4)0.017 (4)
C80.071 (6)0.144 (8)0.068 (5)0.044 (6)0.016 (4)0.034 (6)
C90.040 (4)0.157 (8)0.067 (5)0.001 (5)0.007 (4)0.045 (5)
C100.032 (4)0.129 (8)0.050 (4)0.001 (4)0.005 (3)0.016 (4)
C110.160 (9)0.088 (6)0.064 (5)0.062 (6)0.004 (6)0.004 (5)
C120.125 (7)0.124 (7)0.055 (5)0.085 (6)0.014 (5)0.003 (5)
Geometric parameters (Å, º) top
Yb1—O42.400 (5)C1—C21.390 (11)
Yb1—O4i2.400 (5)C1—H10.9300
Yb1—O22.451 (4)C2—C31.342 (17)
Yb1—O2i2.451 (4)C2—H20.9300
Yb1—N42.452 (5)C3—C41.398 (16)
Yb1—N4i2.452 (5)C3—H30.9300
Yb1—O1i2.481 (5)C4—C51.420 (11)
Yb1—O12.481 (5)C4—C111.424 (16)
Yb1—N32.533 (5)C5—C61.425 (11)
Yb1—N3i2.533 (5)C6—C71.418 (10)
Yb1—N1i2.896 (5)C7—C81.336 (14)
N1—O31.209 (7)C7—C121.445 (14)
N1—O21.261 (7)C8—C91.361 (14)
N1—O11.263 (7)C8—H80.9300
N2—O51.217 (12)C9—C101.416 (12)
N2—O4i1.252 (7)C9—H90.9300
N2—O41.252 (6)C10—H100.9300
N3—C11.317 (9)C11—C121.293 (16)
N3—C51.356 (9)C11—H110.9300
N4—C101.327 (9)C12—H120.9300
N4—C61.370 (9)
O4—Yb1—O4i52.1 (3)N3—Yb1—N1i65.75 (16)
O4—Yb1—O272.93 (17)N3i—Yb1—N1i130.30 (16)
O4i—Yb1—O279.39 (17)O3—N1—O2123.7 (6)
O4—Yb1—O2i79.39 (17)O3—N1—O1121.4 (6)
O4i—Yb1—O2i72.93 (17)O2—N1—O1114.9 (5)
O2—Yb1—O2i149.2 (2)O5—N2—O4i122.6 (4)
O4—Yb1—N4130.82 (19)O5—N2—O4122.6 (4)
O4i—Yb1—N482.13 (19)O4i—N2—O4114.8 (8)
O2—Yb1—N4120.18 (15)C1—N3—C5119.1 (6)
O2i—Yb1—N469.52 (15)C1—N3—Yb1123.8 (5)
O4—Yb1—N4i82.13 (19)C5—N3—Yb1117.0 (5)
O4i—Yb1—N4i130.82 (19)C10—N4—C6118.5 (6)
O2—Yb1—N4i69.52 (15)C10—N4—Yb1121.8 (5)
O2i—Yb1—N4i120.18 (15)C6—N4—Yb1119.7 (4)
N4—Yb1—N4i146.6 (3)N1—O1—Yb195.8 (4)
O4—Yb1—O1i69.33 (17)N1—O2—Yb197.3 (3)
O4i—Yb1—O1i104.25 (17)N2—O4—Yb196.5 (5)
O2—Yb1—O1i126.62 (15)N3—C1—C2124.3 (9)
O2i—Yb1—O1i51.09 (15)N3—C1—H1117.9
N4—Yb1—O1i112.98 (16)C2—C1—H1117.9
N4i—Yb1—O1i69.13 (16)C3—C2—C1116.1 (10)
O4—Yb1—O1104.25 (17)C3—C2—H2122.0
O4i—Yb1—O169.33 (17)C1—C2—H2122.0
O2—Yb1—O151.09 (15)C2—C3—C4123.9 (9)
O2i—Yb1—O1126.62 (15)C2—C3—H3118.1
N4—Yb1—O169.13 (16)C4—C3—H3118.1
N4i—Yb1—O1112.98 (16)C3—C4—C5115.3 (9)
O1i—Yb1—O1173.2 (2)C3—C4—C11127.5 (10)
O4—Yb1—N3137.61 (19)C5—C4—C11117.1 (11)
O4i—Yb1—N3139.15 (18)N3—C5—C4121.3 (8)
O2—Yb1—N3138.45 (16)N3—C5—C6118.7 (6)
O2i—Yb1—N372.19 (16)C4—C5—C6120.0 (7)
N4—Yb1—N366.22 (19)N4—C6—C7121.6 (8)
N4i—Yb1—N385.68 (18)N4—C6—C5118.2 (6)
O1i—Yb1—N368.38 (17)C7—C6—C5120.2 (8)
O1—Yb1—N3117.87 (17)C8—C7—C6117.7 (9)
O4—Yb1—N3i139.15 (18)C8—C7—C12125.3 (9)
O4i—Yb1—N3i137.61 (19)C6—C7—C12117.0 (10)
O2—Yb1—N3i72.19 (16)C7—C8—C9122.3 (9)
O2i—Yb1—N3i138.45 (16)C7—C8—H8118.9
N4—Yb1—N3i85.68 (18)C9—C8—H8118.9
N4i—Yb1—N3i66.22 (19)C8—C9—C10118.2 (9)
O1i—Yb1—N3i117.87 (17)C8—C9—H9120.9
O1—Yb1—N3i68.38 (17)C10—C9—H9120.9
N3—Yb1—N3i67.3 (2)N4—C10—C9121.6 (9)
O4—Yb1—N1i74.97 (16)N4—C10—H10119.2
O4i—Yb1—N1i90.26 (17)C9—C10—H10119.2
O2—Yb1—N1i145.75 (14)C12—C11—C4123.6 (10)
O2i—Yb1—N1i25.58 (14)C12—C11—H11118.2
N4—Yb1—N1i90.05 (15)C4—C11—H11118.2
N4i—Yb1—N1i94.63 (16)C11—C12—C7122.0 (9)
O1i—Yb1—N1i25.70 (15)C11—C12—H12119.0
O1—Yb1—N1i152.15 (15)C7—C12—H12119.0
O4—Yb1—N3—C153.4 (6)N4—Yb1—O2—N13.0 (4)
O4i—Yb1—N3—C1136.2 (5)N4i—Yb1—O2—N1141.5 (4)
O2—Yb1—N3—C172.0 (6)O1i—Yb1—O2—N1177.2 (3)
O2i—Yb1—N3—C1103.7 (5)O1—Yb1—O2—N15.4 (3)
N4—Yb1—N3—C1178.6 (6)N3—Yb1—O2—N184.3 (4)
N4i—Yb1—N3—C119.9 (5)N3i—Yb1—O2—N170.9 (4)
O1i—Yb1—N3—C149.3 (5)N1i—Yb1—O2—N1151.8 (4)
O1—Yb1—N3—C1133.7 (5)O5—N2—O4—Yb1180.0
N3i—Yb1—N3—C185.9 (5)O4i—N2—O4—Yb10.000 (1)
N1i—Yb1—N3—C177.1 (5)O4i—Yb1—O4—N20.0
O4—Yb1—N3—C5128.8 (4)O2—Yb1—O4—N289.7 (3)
O4i—Yb1—N3—C545.9 (5)O2i—Yb1—O4—N276.5 (3)
O2—Yb1—N3—C5105.8 (4)N4—Yb1—O4—N225.8 (4)
O2i—Yb1—N3—C578.5 (4)N4i—Yb1—O4—N2160.6 (3)
N4—Yb1—N3—C53.5 (4)O1i—Yb1—O4—N2128.8 (3)
N4i—Yb1—N3—C5157.9 (4)O1—Yb1—O4—N248.8 (3)
O1i—Yb1—N3—C5132.9 (5)N3—Yb1—O4—N2124.7 (3)
O1—Yb1—N3—C544.1 (5)N3i—Yb1—O4—N2122.1 (3)
N3i—Yb1—N3—C591.9 (5)N1i—Yb1—O4—N2102.4 (3)
N1i—Yb1—N3—C5105.1 (4)C5—N3—C1—C21.1 (11)
O4—Yb1—N4—C1042.9 (6)Yb1—N3—C1—C2178.8 (6)
O4i—Yb1—N4—C1022.6 (5)N3—C1—C2—C32.6 (14)
O2—Yb1—N4—C1050.2 (5)C1—C2—C3—C42.0 (16)
O2i—Yb1—N4—C1097.3 (5)C2—C3—C4—C50.1 (15)
N4i—Yb1—N4—C10148.6 (5)C2—C3—C4—C11177.1 (10)
O1i—Yb1—N4—C10124.8 (5)C1—N3—C5—C41.2 (10)
O1—Yb1—N4—C1048.2 (5)Yb1—N3—C5—C4176.7 (5)
N3—Yb1—N4—C10176.2 (5)C1—N3—C5—C6178.2 (6)
N3i—Yb1—N4—C10116.7 (5)Yb1—N3—C5—C63.9 (7)
N1i—Yb1—N4—C10112.9 (5)C3—C4—C5—N31.8 (11)
O4—Yb1—N4—C6136.3 (4)C11—C4—C5—N3179.1 (7)
O4i—Yb1—N4—C6156.6 (5)C3—C4—C5—C6177.6 (7)
O2—Yb1—N4—C6130.6 (4)C11—C4—C5—C60.3 (11)
O2i—Yb1—N4—C681.9 (4)C10—N4—C6—C73.1 (9)
N4i—Yb1—N4—C632.2 (4)Yb1—N4—C6—C7177.7 (5)
O1i—Yb1—N4—C654.4 (5)C10—N4—C6—C5176.9 (6)
O1—Yb1—N4—C6132.6 (5)Yb1—N4—C6—C52.3 (7)
N3—Yb1—N4—C63.0 (4)N3—C5—C6—N41.2 (9)
N3i—Yb1—N4—C664.1 (4)C4—C5—C6—N4179.4 (6)
N1i—Yb1—N4—C666.3 (4)N3—C5—C6—C7178.8 (6)
O3—N1—O1—Yb1168.2 (5)C4—C5—C6—C70.6 (10)
O2—N1—O1—Yb18.9 (5)N4—C6—C7—C82.5 (11)
O4—Yb1—O1—N158.9 (4)C5—C6—C7—C8177.5 (7)
O4i—Yb1—O1—N198.3 (4)N4—C6—C7—C12178.1 (7)
O2—Yb1—O1—N15.4 (3)C5—C6—C7—C121.9 (10)
O2i—Yb1—O1—N1146.1 (3)C6—C7—C8—C90.5 (13)
N4—Yb1—O1—N1172.4 (4)C12—C7—C8—C9178.8 (8)
N4i—Yb1—O1—N128.5 (4)C7—C8—C9—C102.8 (13)
N3—Yb1—O1—N1126.0 (3)C6—N4—C10—C90.8 (10)
N3i—Yb1—O1—N178.7 (4)Yb1—N4—C10—C9179.9 (5)
N1i—Yb1—O1—N1143.6 (5)C8—C9—C10—N42.1 (12)
O3—N1—O2—Yb1168.0 (5)C3—C4—C11—C12178.6 (10)
O1—N1—O2—Yb19.1 (5)C5—C4—C11—C121.6 (15)
O4—Yb1—O2—N1130.7 (4)C4—C11—C12—C73.2 (17)
O4i—Yb1—O2—N177.3 (4)C8—C7—C12—C11176.1 (10)
O2i—Yb1—O2—N1103.6 (3)C6—C7—C12—C113.3 (14)
Symmetry code: (i) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C12—H12···O3ii0.932.673.595 (12)173
C12—H12···O2ii0.932.703.412 (10)134
C9—H9···O1iii0.932.433.234 (9)145
C11—H11···O3iv0.932.533.253 (10)135
C2—H2···O4v0.932.713.309 (11)123
Symmetry codes: (ii) x+1/2, y+3/2, z+1/2; (iii) x+2, y, z+3/2; (iv) x+3/2, y+1/2, z+3/2; (v) x+1/2, y+1/2, z+3/2.
 

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