Lithium(I) hexa­amminecobalt(III) tetra­kis(malonato-κ2O,O′′)plutonate(IV) penta­hydrate

Grigoriev, M.S.; Krot, N.N.; Bessonov, A.A.; Lyssenko, K.A.

doi:10.1107/S1600536806041328

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Lithium(I) hexaamminecobalt(III) tetrakis(malonato-κ²O,O′′)plutonate(IV) pentahydrate

M. S. Grigoriev, N. N. Krot, A. A. Bessonov and K. A. Lyssenko

The title compound, Li[Co(NH₃)₆][Pu(C₃H₂O₄)₄]·5H₂O, contains isolated [Pu(C₃H₂O₄)₄]⁴⁻ complex anions. Each malonate dianion binds to the Pu atom in a bidentate fashion, resulting in the formation of six-membered metallocycles. The coordination environment of the Pu atom is a distorted square antiprism. The average Pu—O distance is 2.318 (10) Å, about 0.08 Å shorter than in analogous Th^IV complexes.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806041328/ng2119sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806041328/ng2119Isup2.hkl Contains datablock I

CCDC reference: 628016

checkCIF report

Key indicators

Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.013 Å
R factor = 0.053
wR factor = 0.122
Data-to-parameter ratio = 17.2

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D       H1B    ..  H2B     ..       1.95 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D       H2C    ..  H4B     ..       1.81 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D       H3D    ..  H4B     ..       2.09 Ang.

Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.558     0.710
            Tmin and Tmax expected:      0.609     0.859
            RR =      1.110
            Please check that your absorption correction is appropriate.
CHEMW01_ALERT_1_C  The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       1.11
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       1.21
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.06 Ratio
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.59
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         13
PLAT417_ALERT_2_C Short Inter D-H..H-D       H1C    ..  H5B     ..       2.14 Ang.

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      1.211
            Tmax scaled      0.859 Tmin scaled      0.676

   0 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
   9 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
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus; 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.

Lithium hexaamminecobalt tetrakis(malonato-κ²O,O'')plutonium(IV) pentahydrate top

Crystal data top

Li[Co(NH₃)₆][Pu(C₃H₂O₄)₄]·5H₂O	Z = 2
M_r = 905.39	F(000) = 884
Triclinic, P1	D_x = 2.151 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.0547 (17) Å	Cell parameters from 13943 reflections
b = 11.229 (3) Å	θ = 2.2–28.0°
c = 18.518 (4) Å	µ = 3.03 mm⁻¹
α = 88.940 (5)°	T = 100 K
β = 89.014 (4)°	Plate, yellow-brown
γ = 72.403 (5)°	0.34 × 0.14 × 0.05 mm
V = 1398.0 (6) Å³

Data collection top

Bruker SMART APEX CCD area-detector diffractometer	6677 independent reflections
Radiation source: fine-focus sealed tube	5084 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.065
ω scans	θ_max = 28.0°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→9
T_min = 0.558, T_max = 0.710	k = −14→14
13943 measured reflections	l = −24→24

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.053	Hydrogen site location: mixed
wR(F²) = 0.122	H-atom parameters constrained
S = 1.01	w = 1/[σ²(F_o²) + (0.0591P)²] where P = (F_o² + 2F_c²)/3
6677 reflections	(Δ/σ)_max < 0.001
388 parameters	Δρ_max = 2.88 e Å⁻³
0 restraints	Δρ_min = −4.48 e Å⁻³

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

	x	y	z	U_iso*/U_eq
Pu	0.53094 (5)	0.26045 (3)	0.725018 (16)	0.01126 (10)
Co1	0.5000	0.0000	1.0000	0.0147 (3)
Co2	0.0000	0.5000	0.5000	0.0125 (3)
O1W	−0.3290 (10)	0.7427 (6)	0.7459 (3)	0.0241 (14)
H1A	−0.4464	0.7668	0.7634	0.036*
H1B	−0.2878	0.6634	0.7492	0.036*
O2W	0.4427 (10)	0.3321 (7)	0.3860 (4)	0.0331 (17)
H2A	0.5437	0.2736	0.3999	0.050*
H2B	0.4084	0.3097	0.3459	0.050*
O3W	−0.1110 (13)	0.6745 (7)	0.9370 (4)	0.042 (2)
H3A	0.0138	0.6391	0.9355	0.063*
H3B	−0.1627	0.6445	0.9034	0.063*
O4W	0.4902 (16)	0.6492 (8)	0.9749 (6)	0.077 (4)
H4A	0.3958	0.6252	0.9928	0.116*
H4B	0.5602	0.6598	1.0097	0.116*
O5W	−0.0231 (10)	0.8898 (6)	0.7880 (3)	0.0212 (14)
H5A	0.0200	0.9503	0.7983	0.032*
H5B	−0.0645	0.8645	0.8270	0.032*
O11	0.3043 (9)	0.2211 (5)	0.6475 (3)	0.0178 (13)
O12	0.1114 (10)	0.1363 (6)	0.5864 (3)	0.0235 (15)
O13	0.3775 (9)	0.1246 (6)	0.7834 (3)	0.0173 (13)
O14	0.3477 (10)	−0.0636 (6)	0.8027 (3)	0.0205 (14)
O21	0.3078 (9)	0.4499 (5)	0.6915 (3)	0.0176 (13)
O22	0.0920 (10)	0.6384 (6)	0.6886 (3)	0.0241 (15)
O23	0.3753 (10)	0.3600 (6)	0.8296 (3)	0.0216 (14)
O24	0.2770 (11)	0.5008 (6)	0.9162 (3)	0.0269 (16)
O31	0.6617 (9)	0.2815 (5)	0.6137 (3)	0.0145 (12)
O32	0.7016 (10)	0.2671 (6)	0.4952 (3)	0.0225 (14)
O33	0.7142 (9)	0.0644 (6)	0.6879 (3)	0.0191 (13)
O34	0.8528 (11)	−0.1048 (6)	0.6250 (3)	0.0260 (15)
O41	0.7231 (9)	0.3878 (6)	0.7478 (3)	0.0167 (13)
O42	0.8035 (13)	0.5236 (7)	0.8173 (4)	0.044 (2)
O43	0.7540 (10)	0.1646 (6)	0.8163 (3)	0.0216 (14)
O44	0.9541 (9)	0.1181 (6)	0.9105 (3)	0.0197 (14)
N1	0.3348 (12)	0.0538 (8)	1.0870 (4)	0.0248 (18)
H1C	0.2484	0.1314	1.0792	0.037*
H1D	0.4141	0.0560	1.1249	0.037*
H1E	0.2654	−0.0009	1.0972	0.037*
N2	0.6542 (11)	−0.1520 (7)	1.0512 (4)	0.0192 (16)
H2C	0.6761	−0.2186	1.0215	0.029*
H2D	0.5852	−0.1644	1.0911	0.029*
H2E	0.7728	−0.1435	1.0647	0.029*
N3	0.3166 (11)	−0.0863 (7)	0.9659 (4)	0.0196 (16)
H3C	0.2029	−0.0635	0.9931	0.029*
H3D	0.3743	−0.1704	0.9700	0.029*
H3E	0.2871	−0.0653	0.9189	0.029*
N4	0.0596 (11)	0.5545 (7)	0.4026 (4)	0.0178 (16)
H4C	0.1586	0.5906	0.4052	0.027*
H4D	−0.0513	0.6109	0.3844	0.027*
H4E	0.0989	0.4872	0.3731	0.027*
N5	−0.0841 (11)	0.6738 (6)	0.5315 (4)	0.0158 (15)
H5C	−0.1973	0.6885	0.5587	0.024*
H5D	−0.1076	0.7257	0.4921	0.024*
H5E	0.0135	0.6882	0.5583	0.024*
N6	−0.2728 (11)	0.5176 (7)	0.4725 (3)	0.0155 (15)
H6A	−0.2926	0.4412	0.4733	0.023*
H6B	−0.2947	0.5513	0.4272	0.023*
H6C	−0.3585	0.5686	0.5042	0.023*
C11	0.2259 (13)	0.1329 (8)	0.6357 (4)	0.0133 (17)
C12	0.2876 (15)	0.0160 (8)	0.6836 (4)	0.0199 (19)
H12A	0.1780	−0.0221	0.6837	0.024*
H12B	0.4043	−0.0442	0.6605	0.024*
C13	0.3395 (13)	0.0293 (8)	0.7615 (4)	0.0183 (18)
C21	0.2180 (14)	0.5560 (9)	0.7196 (5)	0.021 (2)
C22	0.2758 (14)	0.5776 (8)	0.7964 (5)	0.0198 (19)
H22A	0.3988	0.6026	0.7931	0.024*
H22B	0.1700	0.6497	0.8160	0.024*
C23	0.3107 (14)	0.4711 (8)	0.8513 (5)	0.0185 (18)
C31	0.6915 (13)	0.2174 (8)	0.5551 (4)	0.0168 (18)
C32	0.7130 (14)	0.0801 (9)	0.5563 (4)	0.0208 (19)
H32A	0.8157	0.0396	0.5199	0.025*
H32B	0.5858	0.0699	0.5402	0.025*
C33	0.7673 (13)	0.0084 (8)	0.6273 (5)	0.0181 (18)
C41	0.8032 (14)	0.4170 (8)	0.8030 (5)	0.0198 (19)
C42	0.9080 (17)	0.3152 (9)	0.8577 (5)	0.029 (2)
H42A	1.0528	0.2986	0.8496	0.034*
H42B	0.8773	0.3523	0.9062	0.034*
C43	0.8711 (13)	0.1916 (8)	0.8615 (4)	0.0154 (17)
Li	−0.095 (3)	0.7932 (15)	0.7128 (8)	0.024 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pu	0.01509 (16)	0.01015 (15)	0.00839 (14)	−0.00380 (11)	−0.00344 (10)	0.00674 (9)
Co1	0.0175 (9)	0.0155 (9)	0.0118 (7)	−0.0062 (7)	−0.0029 (6)	0.0066 (6)
Co2	0.0159 (8)	0.0110 (8)	0.0106 (7)	−0.0045 (7)	−0.0018 (6)	0.0060 (6)
O1W	0.024 (4)	0.020 (4)	0.029 (3)	−0.006 (3)	−0.002 (3)	0.005 (3)
O2W	0.027 (4)	0.041 (5)	0.026 (4)	−0.003 (4)	0.000 (3)	−0.002 (3)
O3W	0.049 (5)	0.032 (5)	0.040 (4)	−0.004 (4)	0.004 (4)	−0.002 (3)
O4W	0.102 (9)	0.040 (6)	0.096 (8)	−0.028 (6)	−0.073 (7)	0.015 (5)
O5W	0.032 (4)	0.013 (3)	0.021 (3)	−0.010 (3)	−0.003 (3)	0.006 (2)
O11	0.023 (3)	0.014 (3)	0.019 (3)	−0.010 (3)	−0.012 (2)	0.012 (2)
O12	0.029 (4)	0.025 (4)	0.019 (3)	−0.013 (3)	−0.011 (3)	0.013 (3)
O13	0.024 (3)	0.021 (3)	0.011 (3)	−0.013 (3)	−0.002 (2)	0.004 (2)
O14	0.035 (4)	0.013 (3)	0.016 (3)	−0.012 (3)	−0.003 (3)	0.007 (2)
O21	0.022 (3)	0.012 (3)	0.016 (3)	−0.001 (3)	−0.003 (2)	0.004 (2)
O22	0.026 (4)	0.016 (3)	0.024 (3)	0.003 (3)	−0.005 (3)	0.006 (3)
O23	0.031 (4)	0.023 (4)	0.012 (3)	−0.010 (3)	−0.001 (3)	0.005 (2)
O24	0.040 (4)	0.025 (4)	0.013 (3)	−0.006 (3)	−0.002 (3)	0.002 (3)
O31	0.018 (3)	0.010 (3)	0.012 (3)	0.000 (3)	−0.001 (2)	0.007 (2)
O32	0.031 (4)	0.022 (4)	0.015 (3)	−0.008 (3)	0.000 (3)	0.005 (2)
O33	0.025 (4)	0.017 (3)	0.015 (3)	−0.005 (3)	0.000 (2)	0.005 (2)
O34	0.042 (4)	0.011 (3)	0.020 (3)	−0.001 (3)	−0.001 (3)	0.000 (2)
O41	0.022 (3)	0.017 (3)	0.013 (3)	−0.009 (3)	−0.003 (2)	0.008 (2)
O42	0.075 (6)	0.025 (4)	0.038 (4)	−0.022 (4)	−0.039 (4)	0.012 (3)
O43	0.034 (4)	0.019 (3)	0.015 (3)	−0.013 (3)	−0.013 (3)	0.005 (2)
O44	0.022 (4)	0.022 (4)	0.017 (3)	−0.011 (3)	−0.006 (3)	0.014 (2)
N1	0.031 (5)	0.031 (5)	0.012 (3)	−0.009 (4)	0.002 (3)	−0.001 (3)
N2	0.023 (4)	0.019 (4)	0.015 (3)	−0.005 (3)	−0.007 (3)	0.010 (3)
N3	0.022 (4)	0.026 (4)	0.012 (3)	−0.011 (4)	−0.003 (3)	0.009 (3)
N4	0.021 (4)	0.016 (4)	0.015 (3)	−0.004 (3)	−0.007 (3)	0.005 (3)
N5	0.017 (4)	0.016 (4)	0.014 (3)	−0.005 (3)	−0.002 (3)	0.008 (3)
N6	0.021 (4)	0.016 (4)	0.009 (3)	−0.005 (3)	−0.002 (3)	0.006 (3)
C11	0.017 (4)	0.011 (4)	0.011 (4)	−0.002 (4)	−0.004 (3)	0.004 (3)
C12	0.031 (5)	0.013 (4)	0.015 (4)	−0.006 (4)	−0.007 (4)	0.003 (3)
C13	0.019 (5)	0.019 (5)	0.017 (4)	−0.006 (4)	−0.002 (3)	0.007 (3)
C21	0.026 (5)	0.021 (5)	0.020 (4)	−0.012 (4)	−0.002 (4)	0.008 (4)
C22	0.019 (5)	0.015 (5)	0.023 (4)	−0.001 (4)	0.000 (4)	0.000 (3)
C23	0.021 (5)	0.017 (5)	0.020 (4)	−0.009 (4)	−0.005 (4)	0.001 (3)
C31	0.014 (4)	0.020 (5)	0.019 (4)	−0.009 (4)	−0.006 (3)	0.006 (3)
C32	0.026 (5)	0.022 (5)	0.016 (4)	−0.011 (4)	−0.003 (4)	0.006 (3)
C33	0.016 (5)	0.015 (5)	0.022 (4)	−0.004 (4)	0.003 (3)	0.010 (3)
C41	0.024 (5)	0.013 (5)	0.023 (4)	−0.008 (4)	−0.007 (4)	0.011 (3)
C42	0.046 (7)	0.020 (5)	0.025 (5)	−0.017 (5)	−0.019 (4)	0.013 (4)
C43	0.012 (4)	0.017 (4)	0.015 (4)	−0.002 (4)	0.004 (3)	0.002 (3)
Li	0.029 (9)	0.019 (8)	0.023 (8)	−0.003 (7)	−0.012 (7)	0.000 (6)

Geometric parameters (Å, º) top

Pu—O11	2.310 (6)	O33—C33	1.289 (10)
Pu—O13	2.360 (6)	O34—C33	1.233 (10)
Pu—O21	2.312 (6)	O34—Liⁱⁱⁱ	1.946 (17)
Pu—O23	2.339 (6)	O41—C41	1.272 (10)
Pu—O31	2.281 (5)	O42—C41	1.232 (11)
Pu—O33	2.302 (6)	O43—C43	1.288 (10)
Pu—O41	2.296 (6)	O44—C43	1.242 (10)
Pu—O43	2.344 (6)	N1—H1C	0.9100
Co1—N3	1.955 (7)	N1—H1D	0.9100
Co1—N3ⁱ	1.955 (7)	N1—H1E	0.9100
Co1—N2ⁱ	1.962 (7)	N2—H2C	0.9100
Co1—N2	1.962 (7)	N2—H2D	0.9100
Co1—N1ⁱ	1.965 (7)	N2—H2E	0.9100
Co1—N1	1.965 (7)	N3—H3C	0.9100
Co2—N6	1.950 (7)	N3—H3D	0.9100
Co2—N6ⁱⁱ	1.950 (7)	N3—H3E	0.9100
Co2—N5ⁱⁱ	1.958 (7)	N4—H4C	0.9100
Co2—N5	1.958 (7)	N4—H4D	0.9100
Co2—N4	1.974 (7)	N4—H4E	0.9100
Co2—N4ⁱⁱ	1.974 (7)	N5—H5C	0.9100
O1W—Li	1.984 (19)	N5—H5D	0.9100
O1W—H1A	0.8500	N5—H5E	0.9100
O1W—H1B	0.8499	N6—H6A	0.9100
O2W—H2A	0.8500	N6—H6B	0.9100
O2W—H2B	0.8501	N6—H6C	0.9100
O3W—H3A	0.8500	C11—C12	1.525 (11)
O3W—H3B	0.8500	C12—C13	1.516 (11)
O4W—H4A	0.8500	C12—H12A	0.9900
O4W—H4B	0.8500	C12—H12B	0.9900
O5W—Li	1.947 (16)	C21—C22	1.530 (12)
O5W—H5A	0.8500	C22—C23	1.520 (12)
O5W—H5B	0.8500	C22—H22A	0.9900
O11—C11	1.296 (10)	C22—H22B	0.9900
O12—C11	1.222 (10)	C31—C32	1.503 (12)
O13—C13	1.255 (10)	C32—C33	1.522 (11)
O14—C13	1.268 (10)	C32—H32A	0.9900
O21—C21	1.283 (11)	C32—H32B	0.9900
O22—C21	1.215 (11)	C41—C42	1.532 (12)
O22—Li	1.894 (18)	C42—C43	1.488 (12)
O23—C23	1.263 (11)	C42—H42A	0.9900
O24—C23	1.252 (10)	C42—H42B	0.9900
O31—C31	1.293 (10)	Li—O34^iv	1.946 (17)
O32—C31	1.244 (10)

O31—Pu—O41	77.6 (2)	H2D—N2—H2E	109.5
O31—Pu—O33	72.3 (2)	Co1—N3—H3C	109.5
O41—Pu—O33	113.1 (2)	Co1—N3—H3D	109.5
O31—Pu—O11	77.0 (2)	H3C—N3—H3D	109.5
O41—Pu—O11	145.30 (19)	Co1—N3—H3E	109.5
O33—Pu—O11	81.0 (2)	H3C—N3—H3E	109.5
O31—Pu—O21	81.6 (2)	H3D—N3—H3E	109.5
O41—Pu—O21	81.2 (2)	Co2—N4—H4C	109.5
O33—Pu—O21	146.0 (2)	Co2—N4—H4D	109.5
O11—Pu—O21	72.0 (2)	H4C—N4—H4D	109.5
O31—Pu—O23	146.9 (2)	Co2—N4—H4E	109.5
O41—Pu—O23	79.2 (2)	H4C—N4—H4E	109.5
O33—Pu—O23	139.3 (2)	H4D—N4—H4E	109.5
O11—Pu—O23	111.5 (2)	Co2—N5—H5C	109.5
O21—Pu—O23	71.8 (2)	Co2—N5—H5D	109.5
O31—Pu—O43	117.3 (2)	H5C—N5—H5D	109.5
O41—Pu—O43	72.3 (2)	Co2—N5—H5E	109.5
O33—Pu—O43	71.2 (2)	H5C—N5—H5E	109.5
O11—Pu—O43	141.3 (2)	H5D—N5—H5E	109.5
O21—Pu—O43	142.0 (2)	Co2—N6—H6A	109.5
O23—Pu—O43	76.8 (2)	Co2—N6—H6B	109.5
O31—Pu—O13	137.6 (2)	H6A—N6—H6B	109.5
O41—Pu—O13	141.69 (19)	Co2—N6—H6C	109.5
O33—Pu—O13	75.6 (2)	H6A—N6—H6C	109.5
O11—Pu—O13	71.13 (19)	H6B—N6—H6C	109.5
O21—Pu—O13	113.1 (2)	O12—C11—O11	123.5 (7)
O23—Pu—O13	72.8 (2)	O12—C11—C12	118.2 (7)
O43—Pu—O13	76.2 (2)	O11—C11—C12	118.2 (7)
N3—Co1—N3ⁱ	180.000 (1)	C13—C12—C11	118.4 (7)
N3—Co1—N2ⁱ	89.5 (3)	C13—C12—H12A	107.7
N3ⁱ—Co1—N2ⁱ	90.5 (3)	C11—C12—H12A	107.7
N3—Co1—N2	90.5 (3)	C13—C12—H12B	107.7
N3ⁱ—Co1—N2	89.5 (3)	C11—C12—H12B	107.7
N2ⁱ—Co1—N2	180.0 (3)	H12A—C12—H12B	107.1
N3—Co1—N1ⁱ	89.3 (3)	O13—C13—O14	122.1 (8)
N3ⁱ—Co1—N1ⁱ	90.7 (3)	O13—C13—C12	122.2 (7)
N2ⁱ—Co1—N1ⁱ	90.0 (3)	O14—C13—C12	115.7 (8)
N2—Co1—N1ⁱ	90.0 (3)	O22—C21—O21	123.7 (8)
N3—Co1—N1	90.7 (3)	O22—C21—C22	119.3 (9)
N3ⁱ—Co1—N1	89.3 (3)	O21—C21—C22	117.1 (8)
N2ⁱ—Co1—N1	90.0 (3)	C23—C22—C21	118.6 (7)
N2—Co1—N1	90.0 (3)	C23—C22—H22A	107.7
N1ⁱ—Co1—N1	180.000 (3)	C21—C22—H22A	107.7
N6—Co2—N6ⁱⁱ	180.000 (1)	C23—C22—H22B	107.7
N6—Co2—N5ⁱⁱ	90.5 (3)	C21—C22—H22B	107.7
N6ⁱⁱ—Co2—N5ⁱⁱ	89.5 (3)	H22A—C22—H22B	107.1
N6—Co2—N5	89.5 (3)	O24—C23—O23	124.3 (8)
N6ⁱⁱ—Co2—N5	90.5 (3)	O24—C23—C22	116.7 (8)
N5ⁱⁱ—Co2—N5	180.0 (4)	O23—C23—C22	119.0 (8)
N6—Co2—N4	90.9 (3)	O32—C31—O31	121.3 (8)
N6ⁱⁱ—Co2—N4	89.1 (3)	O32—C31—C32	117.2 (8)
N5ⁱⁱ—Co2—N4	89.9 (3)	O31—C31—C32	121.5 (7)
N5—Co2—N4	90.1 (3)	C31—C32—C33	118.1 (7)
N6—Co2—N4ⁱⁱ	89.1 (3)	C31—C32—H32A	107.8
N6ⁱⁱ—Co2—N4ⁱⁱ	90.9 (3)	C33—C32—H32A	107.8
N5ⁱⁱ—Co2—N4ⁱⁱ	90.1 (3)	C31—C32—H32B	107.8
N5—Co2—N4ⁱⁱ	89.9 (3)	C33—C32—H32B	107.8
N4—Co2—N4ⁱⁱ	180.000 (2)	H32A—C32—H32B	107.1
Li—O1W—H1A	146.1	O34—C33—O33	121.5 (8)
Li—O1W—H1B	105.4	O34—C33—C32	118.2 (8)
H1A—O1W—H1B	107.7	O33—C33—C32	120.2 (8)
H2A—O2W—H2B	106.8	O42—C41—O41	124.8 (8)
H3A—O3W—H3B	107.7	O42—C41—C42	115.5 (8)
H4A—O4W—H4B	107.7	O41—C41—C42	119.6 (8)
Li—O5W—H5A	147.2	C43—C42—C41	122.2 (8)
Li—O5W—H5B	104.6	C43—C42—H42A	106.8
H5A—O5W—H5B	107.7	C41—C42—H42A	106.8
C11—O11—Pu	138.3 (5)	C43—C42—H42B	106.8
C13—O13—Pu	131.2 (5)	C41—C42—H42B	106.8
C21—O21—Pu	138.8 (5)	H42A—C42—H42B	106.6
C21—O22—Li	137.1 (8)	O44—C43—O43	122.2 (8)
C23—O23—Pu	136.3 (6)	O44—C43—C42	117.4 (8)
C31—O31—Pu	134.6 (5)	O43—C43—C42	120.4 (7)
C33—O33—Pu	137.0 (5)	O22—Li—O34^iv	107.2 (8)
C33—O34—Liⁱⁱⁱ	121.0 (7)	O22—Li—O5W	117.4 (8)
C41—O41—Pu	136.1 (5)	O34^iv—Li—O5W	108.2 (8)
C43—O43—Pu	139.8 (5)	O22—Li—O1W	102.5 (8)
Co1—N1—H1C	109.5	O34^iv—Li—O1W	112.5 (8)
Co1—N1—H1D	109.5	O5W—Li—O1W	109.1 (8)
H1C—N1—H1D	109.5	O22—Li—C33^iv	128.6 (8)
Co1—N1—H1E	109.5	O34^iv—Li—C33^iv	22.3 (3)
H1C—N1—H1E	109.5	O5W—Li—C33^iv	90.3 (6)
H1D—N1—H1E	109.5	O1W—Li—C33^iv	107.9 (7)
Co1—N2—H2C	109.5	O22—Li—H5B	115.3
Co1—N2—H2D	109.5	O34^iv—Li—H5B	125.5
H2C—N2—H2D	109.5	O5W—Li—H5B	20.8
Co1—N2—H2E	109.5	O1W—Li—H5B	90.2
H2C—N2—H2E	109.5	C33^iv—Li—H5B	105.0

O31—Pu—O11—C11	123.4 (9)	O31—Pu—O43—C43	81.2 (9)
O41—Pu—O11—C11	167.4 (7)	O41—Pu—O43—C43	15.9 (8)
O33—Pu—O11—C11	49.6 (8)	O33—Pu—O43—C43	138.8 (9)
O21—Pu—O11—C11	−151.4 (9)	O11—Pu—O43—C43	−174.8 (8)
O23—Pu—O11—C11	−90.1 (9)	O21—Pu—O43—C43	−32.0 (10)
O43—Pu—O11—C11	5.6 (10)	O23—Pu—O43—C43	−66.8 (9)
O13—Pu—O11—C11	−28.2 (8)	O13—Pu—O43—C43	−142.0 (9)
O31—Pu—O13—C13	1.2 (9)	Pu—O11—C11—O12	−176.3 (6)
O41—Pu—O13—C13	−149.6 (7)	Pu—O11—C11—C12	0.5 (13)
O33—Pu—O13—C13	−40.5 (7)	O12—C11—C12—C13	−150.6 (9)
O11—Pu—O13—C13	44.7 (7)	O11—C11—C12—C13	32.4 (12)
O21—Pu—O13—C13	104.6 (8)	Pu—O13—C13—O14	145.2 (7)
O23—Pu—O13—C13	165.4 (8)	Pu—O13—C13—C12	−32.8 (13)
O43—Pu—O13—C13	−114.3 (8)	C11—C12—C13—O13	−16.6 (14)
O31—Pu—O21—C21	−138.3 (9)	C11—C12—C13—O14	165.4 (8)
O41—Pu—O21—C21	−59.6 (9)	Li—O22—C21—O21	169.7 (10)
O33—Pu—O21—C21	−178.2 (8)	Li—O22—C21—C22	−10.4 (16)
O11—Pu—O21—C21	142.7 (9)	Pu—O21—C21—O22	−174.0 (6)
O23—Pu—O21—C21	21.8 (8)	Pu—O21—C21—C22	6.1 (13)
O43—Pu—O21—C21	−13.9 (10)	O22—C21—C22—C23	139.4 (9)
O13—Pu—O21—C21	83.3 (9)	O21—C21—C22—C23	−40.7 (12)
O31—Pu—O23—C23	3.2 (10)	Pu—O23—C23—O24	−161.2 (7)
O41—Pu—O23—C23	49.3 (8)	Pu—O23—C23—C22	16.9 (13)
O33—Pu—O23—C23	162.3 (8)	C21—C22—C23—O24	−151.6 (9)
O11—Pu—O23—C23	−96.2 (8)	C21—C22—C23—O23	30.2 (13)
O21—Pu—O23—C23	−34.9 (8)	Pu—O31—C31—O32	155.1 (6)
O43—Pu—O23—C23	123.5 (9)	Pu—O31—C31—C32	−24.2 (12)
O13—Pu—O23—C23	−157.2 (9)	O32—C31—C32—C33	160.8 (8)
O41—Pu—O31—C31	158.0 (8)	O31—C31—C32—C33	−19.9 (13)
O33—Pu—O31—C31	38.6 (7)	Liⁱⁱⁱ—O34—C33—O33	2.0 (14)
O11—Pu—O31—C31	−45.9 (7)	Liⁱⁱⁱ—O34—C33—C32	−174.0 (8)
O21—Pu—O31—C31	−119.2 (8)	Pu—O33—C33—O34	−172.6 (6)
O23—Pu—O31—C31	−155.5 (7)	Pu—O33—C33—C32	3.4 (13)
O43—Pu—O31—C31	95.6 (8)	Pu—O33—C33—Liⁱⁱⁱ	−171.3 (7)
O13—Pu—O31—C31	−4.0 (9)	C31—C32—C33—O34	−154.5 (9)
O31—Pu—O33—C33	−27.6 (8)	C31—C32—C33—O33	29.4 (12)
O41—Pu—O33—C33	−95.3 (8)	C31—C32—C33—Liⁱⁱⁱ	−162.9 (13)
O11—Pu—O33—C33	51.6 (8)	Pu—O41—C41—O42	−136.9 (9)
O21—Pu—O33—C33	14.2 (10)	Pu—O41—C41—C42	42.7 (13)
O23—Pu—O33—C33	164.2 (7)	O42—C41—C42—C43	161.2 (10)
O43—Pu—O33—C33	−155.7 (9)	O41—C41—C42—C43	−18.5 (15)
O13—Pu—O33—C33	124.3 (8)	Pu—O43—C43—O44	170.8 (6)
O31—Pu—O41—C41	−159.0 (9)	Pu—O43—C43—C42	−7.8 (14)
O33—Pu—O41—C41	−94.5 (9)	C41—C42—C43—O44	−175.8 (9)
O11—Pu—O41—C41	157.1 (8)	C41—C42—C43—O43	2.9 (15)
O21—Pu—O41—C41	117.8 (9)	C21—O22—Li—O34^iv	154.2 (10)
O23—Pu—O41—C41	44.8 (8)	C21—O22—Li—O5W	32.3 (17)
O43—Pu—O41—C41	−34.7 (8)	C21—O22—Li—O1W	−87.2 (12)
O13—Pu—O41—C41	1.4 (10)	C21—O22—Li—C33^iv	147.3 (10)

Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x, −y+1, −z+1; (iii) x+1, y−1, z; (iv) x−1, y+1, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1A···O14^iv	0.85	2.15	2.836 (9)	138
O1W—H1B···O42^v	0.85	1.95	2.683 (9)	143
O2W—H2A···O32	0.85	2.09	2.688 (9)	127
O2W—H2B···O1Wⁱⁱ	0.85	1.95	2.804 (9)	180
O3W—H3A···O24	0.85	2.06	2.865 (11)	158
O3W—H3B···O42^v	0.85	2.18	2.993 (11)	161
O4W—H4A···O24	0.85	2.34	2.804 (11)	115
O4W—H4B···O24^vi	0.85	2.27	2.814 (11)	122
O5W—H5A···O14^vii	0.85	2.27	2.837 (9)	124

Symmetry codes: (ii) −x, −y+1, −z+1; (iv) x−1, y+1, z; (v) x−1, y, z; (vi) −x+1, −y+1, −z+2; (vii) x, y+1, z.

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