Tris(nitrato-κ²O,O′)bis­(1,10-phenanthroline-κ²N,N′)ytterbium(III)

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.

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

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Computing details

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)

Crystal data

[Yb(NO3)3(C12H8N2)2]	F(000) = 1404
Mr = 719.48	Dx = 1.916 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2949 reflections
a = 9.456 (2) Å	θ = 2.4–26.2°
b = 15.451 (3) Å	µ = 3.82 mm^−1
c = 17.104 (3) Å	T = 298 K
β = 93.687 (2)°	Block, yellow
V = 2493.8 (8) Å^3	0.46 × 0.16 × 0.10 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer	2162 independent reflections
Radiation source: fine-focus sealed tube	1885 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.040
φ and ω scans	θmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→10
Tmin = 0.273, Tmax = 0.701	k = −15→18
6189 measured reflections	l = −20→18

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.079	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.044P)^2 + 0.0077P] where P = (Fo^2 + 2Fc^2)/3
2162 reflections	(Δ/σ)max = 0.001
187 parameters	Δρmax = 1.00 e Å^−3
48 restraints	Δρmin = −0.68 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.5000	0.61150 (2)	0.7500	0.03514 (15)
N1	0.6266 (6)	0.5849 (3)	0.6021 (3)	0.0463 (13)
N2	0.5000	0.4283 (6)	0.7500	0.070 (3)
N3	0.4766 (6)	0.7479 (3)	0.8302 (3)	0.0495 (13)
N4	0.7217 (5)	0.6571 (4)	0.8203 (3)	0.0489 (13)
O1	0.7012 (5)	0.6019 (3)	0.6641 (3)	0.0557 (12)
O2	0.4980 (4)	0.5693 (3)	0.6118 (3)	0.0508 (11)
O3	0.6759 (6)	0.5873 (4)	0.5387 (3)	0.0744 (16)
O4	0.3890 (6)	0.4720 (3)	0.7386 (3)	0.0689 (14)
O5	0.5000	0.3496 (5)	0.7500	0.105 (3)
C1	0.3567 (9)	0.7902 (5)	0.8357 (4)	0.068 (2)
H1	0.2757	0.7679	0.8092	0.082*
C2	0.3432 (14)	0.8659 (6)	0.8785 (6)	0.095 (3)
H2	0.2560	0.8928	0.8827	0.113*
C3	0.4633 (16)	0.8979 (6)	0.9133 (6)	0.102 (3)
H3	0.4581	0.9495	0.9410	0.122*
C4	0.5958 (12)	0.8582 (6)	0.9103 (5)	0.083 (3)
C5	0.5967 (9)	0.7797 (4)	0.8673 (4)	0.059 (2)
C6	0.7252 (8)	0.7322 (5)	0.8630 (4)	0.060 (2)
C7	0.8521 (10)	0.7627 (7)	0.9022 (4)	0.082 (3)
C8	0.9682 (11)	0.7139 (8)	0.8988 (5)	0.095 (3)
H8	1.0526	0.7332	0.9238	0.114*
C9	0.9672 (9)	0.6371 (8)	0.8599 (5)	0.088 (3)
H9	1.0482	0.6029	0.8600	0.105*
C10	0.8394 (8)	0.6105 (6)	0.8191 (4)	0.070 (2)
H10	0.8380	0.5591	0.7908	0.085*
C11	0.7269 (16)	0.8856 (6)	0.9481 (6)	0.105 (4)
H11	0.7278	0.9361	0.9777	0.126*
C12	0.8447 (13)	0.8440 (7)	0.9435 (5)	0.102 (3)
H12	0.9273	0.8672	0.9676	0.123*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.0255 (2)	0.0408 (2)	0.0380 (2)	0.000	−0.00690 (14)	0.000
N1	0.045 (3)	0.052 (3)	0.042 (3)	0.013 (2)	0.002 (3)	0.003 (2)
N2	0.108 (9)	0.049 (5)	0.056 (6)	0.000	0.027 (6)	0.000
N3	0.065 (4)	0.046 (3)	0.038 (3)	0.007 (3)	−0.002 (3)	0.000 (2)
N4	0.035 (3)	0.075 (4)	0.036 (3)	−0.006 (3)	−0.006 (2)	0.009 (3)
O1	0.034 (2)	0.094 (4)	0.039 (3)	0.002 (2)	−0.0018 (19)	−0.001 (2)
O2	0.035 (2)	0.058 (3)	0.058 (3)	0.004 (2)	−0.006 (2)	−0.006 (2)
O3	0.085 (4)	0.095 (4)	0.046 (3)	0.020 (3)	0.023 (3)	0.006 (3)
O4	0.065 (3)	0.060 (3)	0.081 (4)	−0.016 (3)	0.004 (3)	−0.011 (3)
O5	0.183 (11)	0.038 (4)	0.100 (7)	0.000	0.042 (7)	0.000
C1	0.097 (6)	0.065 (5)	0.042 (4)	0.033 (4)	0.000 (4)	−0.002 (4)
C2	0.136 (8)	0.078 (5)	0.069 (5)	0.038 (5)	0.002 (5)	−0.001 (4)
C3	0.165 (9)	0.064 (5)	0.076 (6)	0.011 (6)	0.000 (6)	−0.004 (4)
C4	0.131 (7)	0.070 (5)	0.046 (4)	−0.029 (5)	−0.012 (4)	0.000 (4)
C5	0.096 (6)	0.046 (4)	0.034 (4)	−0.020 (4)	−0.009 (4)	0.006 (3)
C6	0.074 (5)	0.073 (5)	0.030 (4)	−0.043 (4)	−0.010 (3)	0.012 (3)
C7	0.084 (6)	0.113 (6)	0.046 (4)	−0.051 (5)	−0.015 (4)	0.017 (4)
C8	0.071 (6)	0.144 (8)	0.068 (5)	−0.044 (6)	−0.016 (4)	0.034 (6)
C9	0.040 (4)	0.157 (8)	0.067 (5)	0.001 (5)	0.007 (4)	0.045 (5)
C10	0.032 (4)	0.129 (8)	0.050 (4)	0.001 (4)	−0.005 (3)	0.016 (4)
C11	0.160 (9)	0.088 (6)	0.064 (5)	−0.062 (6)	−0.004 (6)	−0.004 (5)
C12	0.125 (7)	0.124 (7)	0.055 (5)	−0.085 (6)	−0.014 (5)	−0.003 (5)

Geometric parameters (Å, º)

Yb1—O4	2.400 (5)	C1—C2	1.390 (11)
Yb1—O4^i	2.400 (5)	C1—H1	0.9300
Yb1—O2	2.451 (4)	C2—C3	1.342 (17)
Yb1—O2^i	2.451 (4)	C2—H2	0.9300
Yb1—N4	2.452 (5)	C3—C4	1.398 (16)
Yb1—N4^i	2.452 (5)	C3—H3	0.9300
Yb1—O1^i	2.481 (5)	C4—C5	1.420 (11)
Yb1—O1	2.481 (5)	C4—C11	1.424 (16)
Yb1—N3	2.533 (5)	C5—C6	1.425 (11)
Yb1—N3^i	2.533 (5)	C6—C7	1.418 (10)
Yb1—N1^i	2.896 (5)	C7—C8	1.336 (14)
N1—O3	1.209 (7)	C7—C12	1.445 (14)
N1—O2	1.261 (7)	C8—C9	1.361 (14)
N1—O1	1.263 (7)	C8—H8	0.9300
N2—O5	1.217 (12)	C9—C10	1.416 (12)
N2—O4^i	1.252 (7)	C9—H9	0.9300
N2—O4	1.252 (6)	C10—H10	0.9300
N3—C1	1.317 (9)	C11—C12	1.293 (16)
N3—C5	1.356 (9)	C11—H11	0.9300
N4—C10	1.327 (9)	C12—H12	0.9300
N4—C6	1.370 (9)
O4—Yb1—O4^i	52.1 (3)	N3—Yb1—N1^i	65.75 (16)
O4—Yb1—O2	72.93 (17)	N3^i—Yb1—N1^i	130.30 (16)
O4^i—Yb1—O2	79.39 (17)	O3—N1—O2	123.7 (6)
O4—Yb1—O2^i	79.39 (17)	O3—N1—O1	121.4 (6)
O4^i—Yb1—O2^i	72.93 (17)	O2—N1—O1	114.9 (5)
O2—Yb1—O2^i	149.2 (2)	O5—N2—O4^i	122.6 (4)
O4—Yb1—N4	130.82 (19)	O5—N2—O4	122.6 (4)
O4^i—Yb1—N4	82.13 (19)	O4^i—N2—O4	114.8 (8)
O2—Yb1—N4	120.18 (15)	C1—N3—C5	119.1 (6)
O2^i—Yb1—N4	69.52 (15)	C1—N3—Yb1	123.8 (5)
O4—Yb1—N4^i	82.13 (19)	C5—N3—Yb1	117.0 (5)
O4^i—Yb1—N4^i	130.82 (19)	C10—N4—C6	118.5 (6)
O2—Yb1—N4^i	69.52 (15)	C10—N4—Yb1	121.8 (5)
O2^i—Yb1—N4^i	120.18 (15)	C6—N4—Yb1	119.7 (4)
N4—Yb1—N4^i	146.6 (3)	N1—O1—Yb1	95.8 (4)
O4—Yb1—O1^i	69.33 (17)	N1—O2—Yb1	97.3 (3)
O4^i—Yb1—O1^i	104.25 (17)	N2—O4—Yb1	96.5 (5)
O2—Yb1—O1^i	126.62 (15)	N3—C1—C2	124.3 (9)
O2^i—Yb1—O1^i	51.09 (15)	N3—C1—H1	117.9
N4—Yb1—O1^i	112.98 (16)	C2—C1—H1	117.9
N4^i—Yb1—O1^i	69.13 (16)	C3—C2—C1	116.1 (10)
O4—Yb1—O1	104.25 (17)	C3—C2—H2	122.0
O4^i—Yb1—O1	69.33 (17)	C1—C2—H2	122.0
O2—Yb1—O1	51.09 (15)	C2—C3—C4	123.9 (9)
O2^i—Yb1—O1	126.62 (15)	C2—C3—H3	118.1
N4—Yb1—O1	69.13 (16)	C4—C3—H3	118.1
N4^i—Yb1—O1	112.98 (16)	C3—C4—C5	115.3 (9)
O1^i—Yb1—O1	173.2 (2)	C3—C4—C11	127.5 (10)
O4—Yb1—N3	137.61 (19)	C5—C4—C11	117.1 (11)
O4^i—Yb1—N3	139.15 (18)	N3—C5—C4	121.3 (8)
O2—Yb1—N3	138.45 (16)	N3—C5—C6	118.7 (6)
O2^i—Yb1—N3	72.19 (16)	C4—C5—C6	120.0 (7)
N4—Yb1—N3	66.22 (19)	N4—C6—C7	121.6 (8)
N4^i—Yb1—N3	85.68 (18)	N4—C6—C5	118.2 (6)
O1^i—Yb1—N3	68.38 (17)	C7—C6—C5	120.2 (8)
O1—Yb1—N3	117.87 (17)	C8—C7—C6	117.7 (9)
O4—Yb1—N3^i	139.15 (18)	C8—C7—C12	125.3 (9)
O4^i—Yb1—N3^i	137.61 (19)	C6—C7—C12	117.0 (10)
O2—Yb1—N3^i	72.19 (16)	C7—C8—C9	122.3 (9)
O2^i—Yb1—N3^i	138.45 (16)	C7—C8—H8	118.9
N4—Yb1—N3^i	85.68 (18)	C9—C8—H8	118.9
N4^i—Yb1—N3^i	66.22 (19)	C8—C9—C10	118.2 (9)
O1^i—Yb1—N3^i	117.87 (17)	C8—C9—H9	120.9
O1—Yb1—N3^i	68.38 (17)	C10—C9—H9	120.9
N3—Yb1—N3^i	67.3 (2)	N4—C10—C9	121.6 (9)
O4—Yb1—N1^i	74.97 (16)	N4—C10—H10	119.2
O4^i—Yb1—N1^i	90.26 (17)	C9—C10—H10	119.2
O2—Yb1—N1^i	145.75 (14)	C12—C11—C4	123.6 (10)
O2^i—Yb1—N1^i	25.58 (14)	C12—C11—H11	118.2
N4—Yb1—N1^i	90.05 (15)	C4—C11—H11	118.2
N4^i—Yb1—N1^i	94.63 (16)	C11—C12—C7	122.0 (9)
O1^i—Yb1—N1^i	25.70 (15)	C11—C12—H12	119.0
O1—Yb1—N1^i	152.15 (15)	C7—C12—H12	119.0
O4—Yb1—N3—C1	−53.4 (6)	N4—Yb1—O2—N1	−3.0 (4)
O4^i—Yb1—N3—C1	−136.2 (5)	N4^i—Yb1—O2—N1	141.5 (4)
O2—Yb1—N3—C1	72.0 (6)	O1^i—Yb1—O2—N1	−177.2 (3)
O2^i—Yb1—N3—C1	−103.7 (5)	O1—Yb1—O2—N1	−5.4 (3)
N4—Yb1—N3—C1	−178.6 (6)	N3—Yb1—O2—N1	84.3 (4)
N4^i—Yb1—N3—C1	19.9 (5)	N3^i—Yb1—O2—N1	70.9 (4)
O1^i—Yb1—N3—C1	−49.3 (5)	N1^i—Yb1—O2—N1	−151.8 (4)
O1—Yb1—N3—C1	133.7 (5)	O5—N2—O4—Yb1	180.0
N3^i—Yb1—N3—C1	85.9 (5)	O4^i—N2—O4—Yb1	0.000 (1)
N1^i—Yb1—N3—C1	−77.1 (5)	O4^i—Yb1—O4—N2	0.0
O4—Yb1—N3—C5	128.8 (4)	O2—Yb1—O4—N2	89.7 (3)
O4^i—Yb1—N3—C5	45.9 (5)	O2^i—Yb1—O4—N2	−76.5 (3)
O2—Yb1—N3—C5	−105.8 (4)	N4—Yb1—O4—N2	−25.8 (4)
O2^i—Yb1—N3—C5	78.5 (4)	N4^i—Yb1—O4—N2	160.6 (3)
N4—Yb1—N3—C5	3.5 (4)	O1^i—Yb1—O4—N2	−128.8 (3)
N4^i—Yb1—N3—C5	−157.9 (4)	O1—Yb1—O4—N2	48.8 (3)
O1^i—Yb1—N3—C5	132.9 (5)	N3—Yb1—O4—N2	−124.7 (3)
O1—Yb1—N3—C5	−44.1 (5)	N3^i—Yb1—O4—N2	122.1 (3)
N3^i—Yb1—N3—C5	−91.9 (5)	N1^i—Yb1—O4—N2	−102.4 (3)
N1^i—Yb1—N3—C5	105.1 (4)	C5—N3—C1—C2	−1.1 (11)
O4—Yb1—N4—C10	42.9 (6)	Yb1—N3—C1—C2	−178.8 (6)
O4^i—Yb1—N4—C10	22.6 (5)	N3—C1—C2—C3	2.6 (14)
O2—Yb1—N4—C10	−50.2 (5)	C1—C2—C3—C4	−2.0 (16)
O2^i—Yb1—N4—C10	97.3 (5)	C2—C3—C4—C5	−0.1 (15)
N4^i—Yb1—N4—C10	−148.6 (5)	C2—C3—C4—C11	−177.1 (10)
O1^i—Yb1—N4—C10	124.8 (5)	C1—N3—C5—C4	−1.2 (10)
O1—Yb1—N4—C10	−48.2 (5)	Yb1—N3—C5—C4	176.7 (5)
N3—Yb1—N4—C10	176.2 (5)	C1—N3—C5—C6	178.2 (6)
N3^i—Yb1—N4—C10	−116.7 (5)	Yb1—N3—C5—C6	−3.9 (7)
N1^i—Yb1—N4—C10	112.9 (5)	C3—C4—C5—N3	1.8 (11)
O4—Yb1—N4—C6	−136.3 (4)	C11—C4—C5—N3	179.1 (7)
O4^i—Yb1—N4—C6	−156.6 (5)	C3—C4—C5—C6	−177.6 (7)
O2—Yb1—N4—C6	130.6 (4)	C11—C4—C5—C6	−0.3 (11)
O2^i—Yb1—N4—C6	−81.9 (4)	C10—N4—C6—C7	3.1 (9)
N4^i—Yb1—N4—C6	32.2 (4)	Yb1—N4—C6—C7	−177.7 (5)
O1^i—Yb1—N4—C6	−54.4 (5)	C10—N4—C6—C5	−176.9 (6)
O1—Yb1—N4—C6	132.6 (5)	Yb1—N4—C6—C5	2.3 (7)
N3—Yb1—N4—C6	−3.0 (4)	N3—C5—C6—N4	1.2 (9)
N3^i—Yb1—N4—C6	64.1 (4)	C4—C5—C6—N4	−179.4 (6)
N1^i—Yb1—N4—C6	−66.3 (4)	N3—C5—C6—C7	−178.8 (6)
O3—N1—O1—Yb1	168.2 (5)	C4—C5—C6—C7	0.6 (10)
O2—N1—O1—Yb1	−8.9 (5)	N4—C6—C7—C8	−2.5 (11)
O4—Yb1—O1—N1	58.9 (4)	C5—C6—C7—C8	177.5 (7)
O4^i—Yb1—O1—N1	98.3 (4)	N4—C6—C7—C12	178.1 (7)
O2—Yb1—O1—N1	5.4 (3)	C5—C6—C7—C12	−1.9 (10)
O2^i—Yb1—O1—N1	146.1 (3)	C6—C7—C8—C9	−0.5 (13)
N4—Yb1—O1—N1	−172.4 (4)	C12—C7—C8—C9	178.8 (8)
N4^i—Yb1—O1—N1	−28.5 (4)	C7—C8—C9—C10	2.8 (13)
N3—Yb1—O1—N1	−126.0 (3)	C6—N4—C10—C9	−0.8 (10)
N3^i—Yb1—O1—N1	−78.7 (4)	Yb1—N4—C10—C9	−179.9 (5)
N1^i—Yb1—O1—N1	143.6 (5)	C8—C9—C10—N4	−2.1 (12)
O3—N1—O2—Yb1	−168.0 (5)	C3—C4—C11—C12	178.6 (10)
O1—N1—O2—Yb1	9.1 (5)	C5—C4—C11—C12	1.6 (15)
O4—Yb1—O2—N1	−130.7 (4)	C4—C11—C12—C7	−3.2 (17)
O4^i—Yb1—O2—N1	−77.3 (4)	C8—C7—C12—C11	−176.1 (10)
O2^i—Yb1—O2—N1	−103.6 (3)	C6—C7—C12—C11	3.3 (14)

Symmetry code: (i) −x+1, y, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C12—H12···O3^ii	0.93	2.67	3.595 (12)	173
C12—H12···O2^ii	0.93	2.70	3.412 (10)	134
C9—H9···O1^iii	0.93	2.43	3.234 (9)	145
C11—H11···O3^iv	0.93	2.53	3.253 (10)	135
C2—H2···O4^v	0.93	2.71	3.309 (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.