Literature DB >> 21580248

Bis(N-{bis-[meth-yl(phen-yl)amino]phos-phor-yl}-2,2,2-trichloro-acetamide)di-nitrato-dioxidouranium(VI).

Kateryna O Znovjyak, Vladimir A Ovchynnikov, Tetyana Yu Sliva, Svitlana V Shishkina, Vladimir M Amirkhanov.   

Abstract

In the title compound, [UO(2)L(2)(NO(3))(2)] {L = N-{bis-[meth-yl(phen-yl)amino]phosphor-yl}-2,2,2-trichloro-acetamide, C(16)H(17)Cl(3)N(3)O(2)P}, the U(VI) ions are eight-coordinated by axial oxido ligands and six equatorial O atoms from the phosphoryl and nitrate groups in a distorted hexa-gonal-bipyramidal geometry. There are disordered fragments in the two coordinating L ligands: the trichloro-methyl group is rotationally disordered between two orientations [occupancy ratio 0.567 (15):0.433 (15)] in one ligand, and a meth-yl(phen-yl)amine fragment is disordered over two conformations [occupancy ratio 0.60 (4):0.40 (4)] in the other ligand. In the crystal structure, intra-molecular N-H⋯O hydrogen bonds between the amine and nitrate groups are observed.

Entities:  

Year:  2010        PMID: 21580248      PMCID: PMC2983606          DOI: 10.1107/S1600536810005611

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For the synthesis and structural investigation of the ligand L, see: Znovjyak et al. (2009 ▶). For a uranium(IV)-containing complex with a similar ligand, see: Amirkhanov et al. (1997 ▶). For inter­pretation of the coordination polyhedra of uranium ions, see: Keppert (1982 ▶).

Experimental

Crystal data

[U(NO3)2O2(C16H17Cl3N3O2P)2] M = 1235.34 Monoclinic, a = 10.2180 (4) Å b = 16.2228 (6) Å c = 28.4327 (7) Å β = 97.421 (3)° V = 4673.7 (3) Å3 Z = 4 Mo Kα radiation μ = 3.95 mm−1 T = 293 K 0.40 × 0.30 × 0.20 mm

Data collection

Oxford Diffraction Xcalibur3 diffractometer Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006 ▶) T min = 0.301, T max = 0.506 24426 measured reflections 10643 independent reflections 7638 reflections with I > 2σ(I) R int = 0.041

Refinement

R[F 2 > 2σ(F 2)] = 0.048 wR(F 2) = 0.142 S = 0.97 10643 reflections 618 parameters 24 restraints H-atom parameters constrained Δρmax = 1.39 e Å−3 Δρmin = −1.02 e Å−3 Data collection: CrysAlis CCD (Oxford Diffraction, 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810005611/cv2695sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810005611/cv2695Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[U(NO3)2O2(C16H17Cl3N3O2P)2]F(000) = 2408
Mr = 1235.34Dx = 1.756 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.2180 (4) ÅCell parameters from 37686 reflections
b = 16.2228 (6) Åθ = 2.9–34.9°
c = 28.4327 (7) ŵ = 3.95 mm1
β = 97.421 (3)°T = 293 K
V = 4673.7 (3) Å3Block, yellow
Z = 40.40 × 0.30 × 0.20 mm
Oxford Diffraction Xcalibur3 diffractometer10643 independent reflections
Radiation source: Enhance (Mo) X-ray Source7638 reflections with I > 2σ(I)
graphiteRint = 0.041
Detector resolution: 16.1827 pixels mm-1θmax = 27.5°, θmin = 2.9°
ω scansh = −13→13
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006)k = −21→8
Tmin = 0.301, Tmax = 0.506l = −36→24
24426 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.142H-atom parameters constrained
S = 0.97w = 1/[σ2(Fo2) + (0.0899P)2] where P = (Fo2 + 2Fc2)/3
10643 reflections(Δ/σ)max = 0.049
618 parametersΔρmax = 1.39 e Å3
24 restraintsΔρmin = −1.02 e Å3
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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.
xyzUiso*/UeqOcc. (<1)
U0.871559 (19)0.121947 (13)0.140066 (7)0.04079 (9)
P10.70900 (15)0.16278 (10)0.01657 (5)0.0436 (3)
P21.03225 (13)0.08951 (9)0.26388 (5)0.0372 (3)
O110.7295 (5)0.1454 (3)0.06851 (15)0.0549 (11)
O211.0084 (4)0.0994 (3)0.21199 (15)0.0483 (10)
N110.7594 (5)0.2608 (3)0.01177 (16)0.0447 (11)
H11A0.81350.27980.03490.054*
O80.8433 (4)−0.0173 (3)0.17804 (14)0.0543 (11)
N210.9692 (5)−0.0036 (3)0.27361 (17)0.0444 (11)
H21A0.9185−0.02560.25040.053*
O100.7016 (6)−0.1106 (3)0.15164 (19)0.0695 (15)
O60.8993 (4)0.2611 (3)0.10364 (15)0.0585 (12)
O40.7473 (4)0.1592 (3)0.17174 (15)0.0534 (10)
O30.9941 (5)0.0840 (3)0.10814 (16)0.0579 (11)
O51.0157 (5)0.2449 (3)0.17055 (16)0.0661 (13)
N40.7533 (5)−0.0451 (3)0.14771 (18)0.0487 (12)
O71.0225 (7)0.3611 (3)0.1343 (2)0.0839 (18)
N221.1892 (4)0.0966 (3)0.28134 (17)0.0434 (11)
N230.9589 (5)0.1539 (3)0.2961 (2)0.0563 (13)
N130.7957 (6)0.1049 (3)−0.0149 (2)0.0573 (14)
O90.7204 (5)0.0014 (3)0.11269 (15)0.0648 (13)
N30.9823 (5)0.2920 (3)0.13605 (19)0.0534 (13)
N120.5536 (5)0.1541 (4)−0.00397 (17)0.0520 (12)
Cl50.7477 (3)−0.1115 (2)0.3015 (2)0.196 (3)
O120.6630 (5)0.2949 (3)−0.06185 (15)0.0647 (13)
Cl60.9530 (6)−0.19012 (19)0.26862 (15)0.197 (2)
O221.0626 (6)−0.0249 (3)0.34914 (16)0.0727 (15)
C510.8482 (6)0.1325 (4)0.3194 (2)0.0497 (14)
C210.9902 (6)−0.0475 (4)0.3143 (2)0.0477 (14)
C520.8613 (8)0.1282 (4)0.3677 (3)0.0658 (19)
H52A0.94210.13930.38560.079*
C410.8742 (8)0.1335 (4)−0.0495 (3)0.0611 (18)
C110.7230 (7)0.3129 (4)−0.0250 (2)0.0495 (14)
C310.4569 (7)0.1903 (5)0.0203 (3)0.0636 (18)
C560.7273 (7)0.1217 (6)0.2935 (3)0.077 (3)
H56A0.71620.12850.26080.092*
C530.7531 (10)0.1072 (6)0.3897 (3)0.085 (3)
H53A0.76220.10340.42260.102*
C220.9179 (9)−0.1300 (4)0.3144 (3)0.067 (2)
C540.6373 (8)0.0924 (8)0.3650 (3)0.094 (3)
H54A0.56620.07660.38030.113*
C320.4102 (9)0.1501 (7)0.0586 (3)0.082 (2)
H32A0.44630.09990.06950.099*
C360.4023 (9)0.2673 (6)0.0069 (3)0.091 (3)
H36A0.43410.2974−0.01700.110*
C120.7731 (5)0.3968 (3)−0.01573 (12)0.084 (3)
C240.9943 (10)0.2414 (5)0.2964 (4)0.107 (4)
H24A0.94310.27100.31690.160*
H24B0.97670.26300.26480.160*
H24C1.08650.24750.30770.160*
C420.8354 (15)0.1152 (7)−0.0970 (4)0.121 (3)
H42A0.75920.0846−0.10590.145*
C290.7946 (12)0.0162 (5)−0.0064 (4)0.106 (4)
H29A0.8488−0.0109−0.02680.159*
H29B0.7058−0.0040−0.01280.159*
H29C0.82850.00520.02610.159*
C550.6225 (8)0.1005 (7)0.3167 (4)0.099 (3)
H55A0.54020.09150.29930.119*
C460.9891 (12)0.1742 (7)−0.0377 (5)0.127 (3)
H46A1.01550.1856−0.00580.153*
C350.3010 (14)0.2981 (10)0.0294 (6)0.154 (6)
H35A0.26330.34840.01960.184*
Cl40.9432 (4)−0.1782 (2)0.36751 (10)0.1564 (17)
C430.9124 (14)0.1433 (8)−0.1318 (4)0.121 (3)
H43A0.88620.1332−0.16390.145*
C441.0247 (13)0.1852 (7)−0.1174 (6)0.127 (3)
H44A1.07370.2051−0.14040.153*
C451.0703 (13)0.1998 (7)−0.0707 (5)0.127 (3)
H45A1.15090.2255−0.06150.153*
C130.5054 (8)0.1276 (6)−0.0522 (3)0.082 (3)
H13A0.41070.1271−0.05650.124*
H13B0.53770.0733−0.05740.124*
H13C0.53610.1652−0.07450.124*
C330.3089 (13)0.1862 (11)0.0799 (4)0.119 (4)
H33A0.27800.15970.10530.143*
C340.2554 (13)0.2578 (14)0.0648 (5)0.142 (6)
H34A0.18600.27980.07890.170*
C61A1.277 (3)0.0532 (18)0.2554 (12)0.035 (7)0.40 (4)
C62A1.325 (3)0.084 (2)0.2186 (12)0.080 (8)0.40 (4)
H62A1.29540.13610.20820.096*0.40 (4)
C63A1.414 (3)0.048 (2)0.1948 (11)0.080 (8)0.40 (4)
H63A1.44560.07420.16940.096*0.40 (4)
C64A1.454 (5)−0.026 (3)0.2086 (11)0.119 (19)0.40 (4)
H64A1.5097−0.05510.19080.143*0.40 (4)
C65A1.415 (2)−0.0641 (16)0.2503 (14)0.076 (9)0.40 (4)
H65A1.4524−0.11330.26240.092*0.40 (4)
C66A1.318 (3)−0.0223 (15)0.2719 (9)0.050 (6)0.40 (4)
H66A1.2823−0.04620.29710.060*0.40 (4)
C23A1.235 (4)0.1244 (19)0.3328 (12)0.045 (7)0.40 (4)
H23A1.32950.12590.33820.068*0.40 (4)
H23B1.20270.08640.35440.068*0.40 (4)
H23C1.20060.17850.33760.068*0.40 (4)
C62B1.3294 (17)0.1168 (16)0.2199 (7)0.067 (5)0.60 (4)
H62B1.30080.17120.21900.080*0.60 (4)
C61B1.280 (3)0.0668 (16)0.2495 (10)0.057 (8)0.60 (4)
C63B1.417 (2)0.096 (3)0.1911 (7)0.108 (9)0.60 (4)
H63B1.45340.13520.17280.129*0.60 (4)
C64B1.452 (2)0.018 (3)0.1893 (14)0.123 (14)0.60 (4)
H64B1.4957−0.00130.16480.147*0.60 (4)
C65B1.421 (3)−0.038 (3)0.2255 (18)0.157 (17)0.60 (4)
H65B1.4650−0.08790.23120.188*0.60 (4)
C66B1.320 (3)−0.0131 (16)0.2518 (17)0.137 (14)0.60 (4)
H66B1.2815−0.05080.27040.164*0.60 (4)
C23B1.257 (3)0.116 (2)0.3260 (10)0.086 (11)0.60 (4)
H23D1.35020.11500.32460.129*0.60 (4)
H23E1.23520.07670.34890.129*0.60 (4)
H23F1.23160.17030.33510.129*0.60 (4)
Cl1A0.9423 (8)0.4061 (6)0.0048 (7)0.310 (13)0.567 (15)
Cl2A0.7365 (18)0.4709 (5)−0.0607 (3)0.168 (6)0.567 (15)
Cl3A0.701 (2)0.4297 (7)0.0339 (4)0.312 (13)0.567 (15)
Cl1B0.9345 (8)0.3982 (7)−0.0312 (7)0.159 (6)0.433 (15)
Cl2B0.6768 (16)0.4636 (6)−0.0549 (5)0.121 (5)0.433 (15)
Cl3B0.7851 (17)0.4390 (6)0.04167 (19)0.145 (5)0.433 (15)
U11U22U33U12U13U23
U0.03685 (13)0.04673 (14)0.03773 (13)−0.00300 (9)0.00076 (8)0.00362 (9)
P10.0466 (8)0.0454 (8)0.0363 (7)−0.0095 (7)−0.0034 (6)0.0026 (6)
P20.0280 (6)0.0385 (7)0.0443 (8)−0.0023 (6)0.0012 (5)0.0020 (6)
O110.055 (3)0.064 (3)0.042 (2)−0.014 (2)−0.0080 (19)0.008 (2)
O210.039 (2)0.053 (2)0.049 (2)−0.0072 (18)−0.0080 (18)0.0098 (19)
N110.054 (3)0.046 (3)0.032 (2)−0.004 (2)−0.006 (2)0.005 (2)
O80.058 (3)0.057 (2)0.045 (2)−0.013 (2)−0.005 (2)0.003 (2)
N210.045 (3)0.041 (3)0.044 (3)−0.012 (2)−0.004 (2)0.003 (2)
O100.083 (4)0.059 (3)0.064 (3)−0.029 (3)0.000 (3)0.005 (2)
O60.062 (3)0.052 (3)0.056 (3)−0.016 (2)−0.013 (2)0.007 (2)
O40.049 (2)0.059 (3)0.053 (3)0.009 (2)0.0075 (19)0.007 (2)
O30.059 (3)0.058 (3)0.060 (3)0.004 (2)0.022 (2)0.000 (2)
O50.077 (3)0.061 (3)0.054 (3)−0.016 (2)−0.016 (2)0.011 (2)
N40.053 (3)0.049 (3)0.043 (3)−0.013 (2)0.002 (2)−0.001 (2)
O70.109 (5)0.060 (3)0.078 (4)−0.034 (3)−0.006 (3)0.004 (3)
N220.032 (2)0.056 (3)0.041 (3)−0.005 (2)−0.0008 (19)−0.001 (2)
N230.051 (3)0.043 (3)0.079 (4)0.002 (2)0.025 (3)−0.002 (3)
N130.064 (4)0.047 (3)0.060 (3)−0.008 (3)0.005 (3)0.001 (2)
O90.073 (3)0.065 (3)0.049 (3)−0.021 (2)−0.018 (2)0.008 (2)
N30.055 (3)0.053 (3)0.052 (3)−0.013 (3)0.002 (2)0.001 (3)
N120.047 (3)0.066 (3)0.040 (3)−0.008 (3)−0.003 (2)0.003 (3)
Cl50.086 (2)0.150 (3)0.336 (7)−0.052 (2)−0.036 (3)0.115 (4)
O120.089 (4)0.063 (3)0.036 (2)−0.007 (3)−0.014 (2)0.005 (2)
Cl60.366 (7)0.0752 (18)0.177 (3)−0.072 (3)0.140 (4)−0.052 (2)
O220.094 (4)0.068 (3)0.048 (3)−0.018 (3)−0.023 (3)0.004 (2)
C510.041 (3)0.055 (4)0.054 (4)0.007 (3)0.009 (3)−0.007 (3)
C210.048 (3)0.046 (3)0.047 (3)−0.003 (3)−0.006 (3)0.004 (3)
C520.059 (4)0.078 (5)0.059 (4)−0.004 (4)0.000 (3)−0.006 (4)
C410.059 (4)0.051 (4)0.075 (5)0.009 (3)0.017 (4)−0.001 (3)
C110.063 (4)0.051 (3)0.034 (3)−0.002 (3)0.004 (3)0.004 (3)
C310.048 (4)0.080 (5)0.060 (4)−0.012 (4)−0.004 (3)0.002 (4)
C560.051 (4)0.134 (8)0.046 (4)0.008 (4)0.008 (3)0.007 (4)
C530.091 (7)0.115 (7)0.052 (4)0.006 (6)0.025 (4)−0.003 (4)
C220.086 (5)0.052 (4)0.059 (4)−0.015 (4)−0.008 (4)0.013 (3)
C540.055 (5)0.149 (9)0.087 (7)−0.014 (5)0.039 (5)−0.006 (6)
C320.066 (5)0.120 (7)0.061 (5)−0.018 (5)0.010 (4)0.006 (5)
C360.086 (6)0.100 (7)0.089 (6)0.030 (5)0.014 (5)0.020 (5)
C120.139 (9)0.051 (4)0.053 (4)0.002 (5)−0.013 (5)0.011 (3)
C240.110 (8)0.048 (4)0.178 (11)−0.012 (5)0.077 (8)−0.016 (5)
C420.141 (8)0.146 (7)0.083 (5)0.016 (6)0.046 (5)0.001 (5)
C290.160 (10)0.055 (5)0.112 (8)−0.009 (6)0.052 (7)−0.008 (5)
C550.039 (4)0.160 (9)0.099 (7)−0.011 (5)0.009 (4)−0.028 (7)
C460.109 (5)0.101 (4)0.184 (8)−0.005 (4)0.065 (5)−0.009 (5)
C350.110 (10)0.156 (13)0.188 (15)0.064 (10)−0.005 (10)−0.032 (12)
Cl40.230 (4)0.127 (2)0.0944 (19)−0.088 (3)−0.047 (2)0.0574 (18)
C430.141 (8)0.146 (7)0.083 (5)0.016 (6)0.046 (5)0.001 (5)
C440.109 (5)0.101 (4)0.184 (8)−0.005 (4)0.065 (5)−0.009 (5)
C450.109 (5)0.101 (4)0.184 (8)−0.005 (4)0.065 (5)−0.009 (5)
C130.060 (4)0.135 (8)0.049 (4)−0.030 (5)−0.008 (3)−0.021 (4)
C330.098 (9)0.181 (14)0.082 (7)−0.012 (9)0.026 (6)−0.001 (8)
C340.086 (9)0.24 (2)0.101 (10)−0.004 (11)0.031 (7)−0.045 (12)
C61A0.022 (12)0.046 (13)0.036 (11)0.006 (9)−0.003 (8)−0.003 (9)
C62A0.109 (19)0.069 (16)0.069 (12)0.028 (13)0.038 (11)0.016 (12)
C63A0.109 (19)0.069 (16)0.069 (12)0.028 (13)0.038 (11)0.016 (12)
C64A0.20 (5)0.12 (3)0.053 (18)0.01 (3)0.07 (2)−0.020 (18)
C65A0.052 (12)0.047 (12)0.13 (2)0.036 (9)0.000 (13)0.013 (13)
C66A0.046 (12)0.051 (12)0.056 (12)0.005 (9)0.018 (8)−0.001 (8)
C23A0.051 (17)0.058 (12)0.026 (10)−0.010 (10)0.001 (10)0.008 (10)
C62B0.052 (8)0.087 (12)0.063 (9)−0.002 (8)0.016 (6)0.004 (9)
C61B0.038 (11)0.062 (11)0.071 (17)−0.001 (8)0.005 (10)−0.012 (10)
C63B0.083 (12)0.16 (3)0.087 (13)0.008 (16)0.042 (10)0.007 (16)
C64B0.083 (14)0.15 (3)0.15 (3)−0.001 (16)0.065 (16)−0.05 (2)
C65B0.15 (3)0.12 (3)0.19 (5)0.08 (2)−0.02 (3)−0.03 (2)
C66B0.073 (15)0.096 (18)0.26 (4)−0.003 (13)0.08 (2)−0.03 (2)
C23B0.035 (8)0.17 (3)0.052 (12)−0.018 (10)0.004 (7)−0.048 (11)
Cl1A0.332 (17)0.126 (7)0.40 (2)−0.145 (9)−0.229 (17)0.104 (11)
Cl2A0.360 (18)0.075 (4)0.057 (3)−0.049 (6)−0.020 (6)0.021 (3)
Cl3A0.77 (4)0.076 (5)0.104 (6)−0.019 (13)0.097 (13)−0.050 (4)
Cl1B0.113 (7)0.113 (6)0.266 (15)−0.065 (6)0.077 (8)−0.060 (8)
Cl2B0.192 (10)0.045 (4)0.112 (7)0.015 (5)−0.040 (6)0.034 (3)
Cl3B0.334 (15)0.059 (4)0.034 (3)−0.061 (6)−0.007 (5)−0.008 (3)
U—O31.750 (4)C36—C351.379 (16)
U—O41.756 (4)C36—H36A0.9300
U—O212.352 (4)C12—Cl1A1.7587 (10)
U—O112.372 (4)C12—Cl2A1.7590 (10)
U—O62.515 (4)C12—Cl3B1.7591 (10)
U—O82.537 (4)C12—Cl2B1.7593 (10)
U—O92.550 (4)C12—Cl3A1.7600 (10)
U—O52.564 (4)C12—Cl1B1.7606 (10)
U—N42.986 (5)C24—H24A0.9600
U—N32.989 (5)C24—H24B0.9600
P1—O111.492 (4)C24—H24C0.9600
P1—N121.626 (5)C42—C431.418 (16)
P1—N131.634 (6)C42—H42A0.9300
P1—N111.683 (5)C29—H29A0.9600
P2—O211.473 (4)C29—H29B0.9600
P2—N221.621 (5)C29—H29C0.9600
P2—N231.635 (6)C55—H55A0.9300
P2—N211.680 (5)C46—C451.395 (15)
N11—C111.358 (7)C46—H46A0.9300
N11—H11A0.8600C35—C341.33 (2)
O8—N41.260 (6)C35—H35A0.9300
N21—C211.350 (7)C43—C441.351 (17)
N21—H21A0.8600C43—H43A0.9300
O10—N41.198 (6)C44—C451.371 (17)
O6—N31.271 (6)C44—H44A0.9300
O5—N31.255 (7)C45—H45A0.9300
N4—O91.260 (6)C13—H13A0.9600
O7—N31.198 (7)C13—H13B0.9600
N22—C23B1.40 (3)C13—H13C0.9600
N22—C61A1.42 (2)C33—C341.33 (2)
N22—C61B1.46 (2)C33—H33A0.9300
N22—C23A1.54 (4)C34—H34A0.9300
N23—C511.424 (8)C61A—C62A1.315 (19)
N23—C241.464 (9)C61A—C66A1.36 (2)
N13—C411.425 (10)C62A—C63A1.33 (2)
N13—C291.459 (10)C62A—H62A0.9300
N12—C311.405 (9)C63A—C64A1.32 (4)
N12—C131.461 (8)C63A—H63A0.9300
Cl5—C221.756 (9)C64A—C65A1.44 (4)
O12—C111.180 (7)C64A—H64A0.9300
Cl6—C221.702 (9)C65A—C66A1.41 (3)
O22—C211.215 (7)C65A—H65A0.9300
C51—C561.365 (10)C66A—H66A0.9300
C51—C521.365 (10)C23A—H23A0.9600
C21—C221.530 (9)C23A—H23B0.9600
C52—C531.381 (12)C23A—H23C0.9600
C52—H52A0.9300C62B—C63B1.336 (17)
C41—C461.351 (14)C62B—C61B1.315 (18)
C41—C421.390 (15)C62B—H62B0.9300
C11—C121.467 (8)C61B—C66B1.360 (19)
C31—C361.400 (11)C63B—C64B1.32 (3)
C31—C321.403 (11)C63B—H63B0.9300
C56—C551.371 (11)C64B—C65B1.43 (4)
C56—H56A0.9300C64B—H64B0.9300
C53—C541.317 (12)C65B—C66B1.41 (2)
C53—H53A0.9300C65B—H65B0.9300
C22—Cl41.690 (7)C66B—H66B0.9300
C54—C551.371 (12)C23B—H23D0.9600
C54—H54A0.9300C23B—H23E0.9600
C32—C331.395 (15)C23B—H23F0.9600
C32—H32A0.9300
O3—U—O4179.3 (2)C21—C22—Cl5108.4 (5)
O3—U—O2190.65 (19)Cl4—C22—Cl5107.5 (5)
O4—U—O2189.76 (17)Cl6—C22—Cl5103.8 (5)
O3—U—O1190.6 (2)C53—C54—C55119.4 (8)
O4—U—O1188.96 (18)C53—C54—H54A120.3
O21—U—O11178.71 (15)C55—C54—H54A120.3
O3—U—O688.62 (19)C33—C32—C31119.1 (10)
O4—U—O691.73 (18)C33—C32—H32A120.4
O21—U—O6114.30 (13)C31—C32—H32A120.4
O11—U—O665.94 (14)C35—C36—C31119.6 (11)
O3—U—O892.05 (19)C35—C36—H36A120.2
O4—U—O887.61 (18)C31—C36—H36A120.2
O21—U—O865.11 (13)C11—C12—Cl1A116.4 (5)
O11—U—O8114.64 (14)C11—C12—Cl2A117.9 (5)
O6—U—O8179.10 (14)Cl1A—C12—Cl2A106.9 (6)
O3—U—O991.0 (2)C11—C12—Cl3B120.6 (5)
O4—U—O988.3 (2)Cl1A—C12—Cl3B73.2 (7)
O21—U—O9114.52 (14)Cl2A—C12—Cl3B113.0 (6)
O11—U—O965.26 (15)C11—C12—Cl2B107.7 (5)
O6—U—O9131.19 (13)Cl1A—C12—Cl2B127.1 (7)
O8—U—O949.41 (13)Cl2A—C12—Cl2B21.7 (9)
O3—U—O591.8 (2)Cl3B—C12—Cl2B108.3 (7)
O4—U—O588.9 (2)C11—C12—Cl3A104.7 (6)
O21—U—O564.90 (14)Cl1A—C12—Cl3A101.8 (8)
O11—U—O5115.25 (15)Cl2A—C12—Cl3A107.6 (7)
O6—U—O549.47 (13)Cl3B—C12—Cl3A28.9 (8)
O8—U—O5129.89 (14)Cl2B—C12—Cl3A93.5 (7)
O9—U—O5177.16 (17)C11—C12—Cl1B106.4 (5)
O3—U—N492.39 (19)Cl1A—C12—Cl1B33.9 (6)
O4—U—N487.04 (18)Cl2A—C12—Cl1B85.9 (7)
O21—U—N489.79 (14)Cl3B—C12—Cl1B105.7 (7)
O11—U—N489.96 (14)Cl2B—C12—Cl1B107.4 (8)
O6—U—N4155.89 (13)Cl3A—C12—Cl1B134.5 (8)
O8—U—N424.69 (13)N23—C24—H24A109.5
O9—U—N424.74 (13)N23—C24—H24B109.5
O5—U—N4154.40 (14)H24A—C24—H24B109.5
O3—U—N390.31 (19)N23—C24—H24C109.5
O4—U—N390.27 (19)H24A—C24—H24C109.5
O21—U—N389.49 (14)H24B—C24—H24C109.5
O11—U—N390.70 (15)C41—C42—C43119.7 (13)
O6—U—N324.85 (13)C41—C42—H42A120.1
O8—U—N3154.51 (14)C43—C42—H42A120.1
O9—U—N3155.93 (14)N13—C29—H29A109.5
O5—U—N324.62 (13)N13—C29—H29B109.5
N4—U—N3177.22 (14)H29A—C29—H29B109.5
O11—P1—N12110.2 (3)N13—C29—H29C109.5
O11—P1—N13114.6 (3)H29A—C29—H29C109.5
N12—P1—N13109.1 (3)H29B—C29—H29C109.5
O11—P1—N11104.7 (2)C54—C55—C56120.9 (8)
N12—P1—N11110.3 (3)C54—C55—H55A119.5
N13—P1—N11107.8 (3)C56—C55—H55A119.5
O21—P2—N22109.1 (3)C41—C46—C45123.5 (14)
O21—P2—N23117.6 (3)C41—C46—H46A118.3
N22—P2—N23106.9 (3)C45—C46—H46A118.3
O21—P2—N21104.2 (2)C34—C35—C36122.0 (14)
N22—P2—N21113.5 (3)C34—C35—H35A119.0
N23—P2—N21105.6 (3)C36—C35—H35A119.0
P1—O11—U150.6 (3)C44—C43—C42118.4 (13)
P2—O21—U152.9 (3)C44—C43—H43A120.8
C11—N11—P1126.4 (4)C42—C43—H43A120.8
C11—N11—H11A116.8C43—C44—C45123.4 (13)
P1—N11—H11A116.8C43—C44—H44A118.3
N4—O8—U98.1 (3)C45—C44—H44A118.3
C21—N21—P2126.3 (4)C44—C45—C46116.4 (13)
C21—N21—H21A116.8C44—C45—H45A121.8
P2—N21—H21A116.8C46—C45—H45A121.8
N3—O6—U98.9 (3)N12—C13—H13A109.5
N3—O5—U97.0 (3)N12—C13—H13B109.5
O10—N4—O8123.0 (5)H13A—C13—H13B109.5
O10—N4—O9121.9 (5)N12—C13—H13C109.5
O8—N4—O9115.1 (5)H13A—C13—H13C109.5
O10—N4—U177.2 (5)H13B—C13—H13C109.5
O8—N4—U57.3 (3)C34—C33—C32121.6 (13)
O9—N4—U57.9 (3)C34—C33—H33A119.2
C23B—N22—C61A108 (2)C32—C33—H33A119.2
C23B—N22—C61B111.1 (17)C33—C34—C35120.1 (14)
C61A—N22—C61B11.1 (17)C33—C34—H34A119.9
C23B—N22—C23A12 (2)C35—C34—H34A119.9
C61A—N22—C23A120 (2)C62A—C61A—C66A119.2 (18)
C61B—N22—C23A123.2 (19)C62A—C61A—N22124 (2)
C23B—N22—P2130.2 (13)C66A—C61A—N22117 (2)
C61A—N22—P2118.2 (16)C63A—C62A—C61A126 (2)
C61B—N22—P2118.0 (13)C63A—C62A—H62A117.1
C23A—N22—P2118.4 (16)C61A—C62A—H62A117.0
C51—N23—C24116.4 (6)C64A—C63A—C62A117 (2)
C51—N23—P2123.6 (4)C64A—C63A—H63A121.3
C24—N23—P2119.4 (5)C62A—C63A—H63A121.3
C41—N13—C29116.9 (7)C63A—C64A—C65A122 (2)
C41—N13—P1125.7 (4)C63A—C64A—H64A119.1
C29—N13—P1117.4 (6)C65A—C64A—H64A119.2
N4—O9—U97.4 (3)C66A—C65A—C64A116 (2)
O7—N3—O5122.8 (6)C66A—C65A—H65A121.9
O7—N3—O6122.6 (6)C64A—C65A—H65A121.9
O5—N3—O6114.6 (5)C61A—C66A—C65A119 (2)
O7—N3—U177.9 (5)C61A—C66A—H66A120.4
O5—N3—U58.3 (3)C65A—C66A—H66A120.4
O6—N3—U56.2 (3)N22—C23A—H23A109.5
C31—N12—C13114.3 (6)N22—C23A—H23B109.5
C31—N12—P1120.2 (4)H23A—C23A—H23B109.5
C13—N12—P1123.9 (5)N22—C23A—H23C109.5
C56—C51—C52120.0 (7)H23A—C23A—H23C109.5
C56—C51—N23119.9 (6)H23B—C23A—H23C109.5
C52—C51—N23119.9 (6)C63B—C62B—C61B125.5 (18)
O22—C21—N21123.6 (6)C63B—C62B—H62B117.3
O22—C21—C22120.3 (6)C61B—C62B—H62B117.3
N21—C21—C22116.1 (5)C62B—C61B—C66B118.6 (16)
C51—C52—C53119.2 (7)C62B—C61B—N22121.4 (18)
C51—C52—H52A120.4C66B—C61B—N22119.9 (18)
C53—C52—H52A120.4C64B—C63B—C62B118 (2)
C46—C41—C42118.4 (10)C64B—C63B—H63B120.9
C46—C41—N13122.4 (9)C62B—C63B—H63B120.9
C42—C41—N13119.1 (8)C63B—C64B—C65B120 (2)
O12—C11—N11126.1 (6)C63B—C64B—H64B120.2
O12—C11—C12121.3 (5)C65B—C64B—H64B120.2
N11—C11—C12112.6 (5)C66B—C65B—C64B116 (2)
C36—C31—C32117.6 (8)C66B—C65B—H65B121.9
C36—C31—N12121.3 (7)C64B—C65B—H65B121.9
C32—C31—N12121.1 (7)C61B—C66B—C65B119 (2)
C51—C56—C55118.8 (7)C61B—C66B—H66B120.5
C51—C56—H56A120.6C65B—C66B—H66B120.4
C55—C56—H56A120.6N22—C23B—H23D109.5
C54—C53—C52121.4 (8)N22—C23B—H23E109.5
C54—C53—H53A119.3H23D—C23B—H23E109.5
C52—C53—H53A119.3N22—C23B—H23F109.5
C21—C22—Cl4112.9 (5)H23D—C23B—H23F109.5
C21—C22—Cl6110.5 (6)H23E—C23B—H23F109.5
Cl4—C22—Cl6113.3 (5)
N12—P1—O11—U171.1 (5)O4—U—N3—O7−36 (12)
N13—P1—O11—U47.7 (7)O21—U—N3—O7−126 (12)
N11—P1—O11—U−70.2 (6)O11—U—N3—O753 (12)
O3—U—O11—P1−26.7 (6)O6—U—N3—O757 (12)
O4—U—O11—P1153.9 (6)O8—U—N3—O7−121 (12)
O21—U—O11—P1162 (6)O9—U—N3—O750 (13)
O6—U—O11—P161.5 (6)O5—U—N3—O7−123 (13)
O8—U—O11—P1−119.2 (6)N4—U—N3—O7−51 (14)
O9—U—O11—P1−117.5 (6)O3—U—N3—O5−93.6 (4)
O5—U—O11—P165.6 (6)O4—U—N3—O586.8 (4)
N4—U—O11—P1−119.1 (6)O21—U—N3—O5−2.9 (4)
N3—U—O11—P163.6 (6)O11—U—N3—O5175.8 (4)
N22—P2—O21—U−166.1 (5)O6—U—N3—O5−179.6 (6)
N23—P2—O21—U−44.2 (7)O8—U—N3—O51.8 (6)
N21—P2—O21—U72.3 (6)O9—U—N3—O5173.2 (4)
O3—U—O21—P2−162.8 (6)N4—U—N3—O572 (3)
O4—U—O21—P216.7 (6)O3—U—N3—O686.1 (4)
O11—U—O21—P28(7)O4—U—N3—O6−93.5 (4)
O6—U—O21—P2108.4 (6)O21—U—N3—O6176.7 (4)
O8—U—O21—P2−70.8 (6)O11—U—N3—O6−4.6 (4)
O9—U—O21—P2−71.4 (6)O8—U—N3—O6−178.5 (4)
O5—U—O21—P2105.6 (6)O9—U—N3—O6−7.1 (6)
N4—U—O21—P2−70.4 (6)O5—U—N3—O6179.6 (6)
N3—U—O21—P2106.9 (6)N4—U—N3—O6−108 (3)
O11—P1—N11—C11−157.5 (5)O11—P1—N12—C3146.0 (6)
N12—P1—N11—C11−39.0 (6)N13—P1—N12—C31172.6 (5)
N13—P1—N11—C1180.1 (6)N11—P1—N12—C31−69.2 (6)
O3—U—O8—N4−91.3 (4)O11—P1—N12—C13−149.1 (6)
O4—U—O8—N488.1 (4)N13—P1—N12—C13−22.5 (7)
O21—U—O8—N4179.0 (4)N11—P1—N12—C1395.7 (6)
O11—U—O8—N40.4 (4)C24—N23—C51—C5698.3 (9)
O6—U—O8—N4131 (9)P2—N23—C51—C56−72.9 (8)
O9—U—O8—N4−1.7 (3)C24—N23—C51—C52−77.4 (9)
O5—U—O8—N4174.7 (3)P2—N23—C51—C52111.4 (7)
N3—U—O8—N4173.7 (3)P2—N21—C21—O22−2.3 (10)
O21—P2—N21—C21165.7 (5)P2—N21—C21—C22178.4 (5)
N22—P2—N21—C2147.1 (6)C56—C51—C52—C534.4 (11)
N23—P2—N21—C21−69.7 (6)N23—C51—C52—C53−179.8 (7)
O3—U—O6—N3−93.7 (4)C29—N13—C41—C46−107.2 (10)
O4—U—O6—N386.9 (4)P1—N13—C41—C4671.8 (10)
O21—U—O6—N3−3.6 (4)C29—N13—C41—C4269.2 (11)
O11—U—O6—N3175.0 (4)P1—N13—C41—C42−111.9 (8)
O8—U—O6—N345 (9)P1—N11—C11—O12−9.6 (10)
O9—U—O6—N3176.1 (3)P1—N11—C11—C12173.6 (4)
O5—U—O6—N3−0.2 (3)C13—N12—C31—C36−68.8 (9)
N4—U—O6—N3173.5 (4)P1—N12—C31—C3697.5 (8)
O3—U—O5—N386.9 (4)C13—N12—C31—C32110.2 (8)
O4—U—O5—N3−93.0 (4)P1—N12—C31—C32−83.5 (8)
O21—U—O5—N3176.8 (4)C52—C51—C56—C55−4.8 (12)
O11—U—O5—N3−4.7 (4)N23—C51—C56—C55179.5 (8)
O6—U—O5—N30.2 (3)C51—C52—C53—C54−1.0 (14)
O8—U—O5—N3−179.0 (3)O22—C21—C22—Cl43.8 (10)
O9—U—O5—N3−104 (3)N21—C21—C22—Cl4−176.9 (6)
N4—U—O5—N3−173.9 (3)O22—C21—C22—Cl6−124.2 (7)
U—O8—N4—O10−176.7 (6)N21—C21—C22—Cl655.1 (8)
U—O8—N4—O92.8 (6)O22—C21—C22—Cl5122.7 (7)
O3—U—N4—O10−174 (100)N21—C21—C22—Cl5−58.0 (8)
O4—U—N4—O106(9)C52—C53—C54—C55−2.1 (18)
O21—U—N4—O1096 (9)C36—C31—C32—C332.7 (12)
O11—U—N4—O10−83 (9)N12—C31—C32—C33−176.4 (8)
O6—U—N4—O10−82 (9)C32—C31—C36—C35−3.8 (14)
O8—U—N4—O1096 (9)N12—C31—C36—C35175.3 (9)
O9—U—N4—O10−87 (9)O12—C11—C12—Cl1A−127.1 (9)
O5—U—N4—O1087 (9)N11—C11—C12—Cl1A49.9 (9)
N3—U—N4—O1020 (11)O12—C11—C12—Cl2A1.9 (11)
O3—U—N4—O889.7 (4)N11—C11—C12—Cl2A178.9 (8)
O4—U—N4—O8−90.7 (4)O12—C11—C12—Cl3B147.6 (8)
O21—U—N4—O8−0.9 (4)N11—C11—C12—Cl3B−35.4 (9)
O11—U—N4—O8−179.7 (4)O12—C11—C12—Cl2B22.8 (10)
O6—U—N4—O8−178.3 (4)N11—C11—C12—Cl2B−160.2 (8)
O9—U—N4—O8177.0 (6)O12—C11—C12—Cl3A121.4 (10)
O5—U—N4—O8−9.4 (6)N11—C11—C12—Cl3A−61.6 (9)
N3—U—N4—O8−76 (3)O12—C11—C12—Cl1B−92.2 (9)
O3—U—N4—O9−87.2 (4)N11—C11—C12—Cl1B84.8 (8)
O4—U—N4—O992.3 (4)C46—C41—C42—C43−3.6 (15)
O21—U—N4—O9−177.9 (4)N13—C41—C42—C43180.0 (9)
O11—U—N4—O93.4 (4)C53—C54—C55—C561.7 (19)
O6—U—N4—O94.7 (6)C51—C56—C55—C541.7 (16)
O8—U—N4—O9−177.0 (6)C42—C41—C46—C451.0 (16)
O5—U—N4—O9173.6 (4)N13—C41—C46—C45177.3 (9)
N3—U—N4—O9107 (3)C31—C36—C35—C342(2)
O21—P2—N22—C23B158.1 (17)C41—C42—C43—C442.2 (18)
N23—P2—N22—C23B29.9 (18)C42—C43—C44—C452(2)
N21—P2—N22—C23B−86.1 (17)C43—C44—C45—C46−4.5 (19)
O21—P2—N22—C61A−45.1 (14)C41—C46—C45—C443.0 (18)
N23—P2—N22—C61A−173.3 (14)C31—C32—C33—C340.2 (18)
N21—P2—N22—C61A70.7 (14)C32—C33—C34—C35−2(2)
O21—P2—N22—C61B−32.5 (13)C36—C35—C34—C331(2)
N23—P2—N22—C61B−160.7 (12)C23B—N22—C61A—C62A−110 (3)
N21—P2—N22—C61B83.3 (13)C61B—N22—C61A—C62A−3(12)
O21—P2—N22—C23A154.7 (12)C23A—N22—C61A—C62A−112 (3)
N23—P2—N22—C23A26.5 (12)P2—N22—C61A—C62A89 (2)
N21—P2—N22—C23A−89.5 (12)C23B—N22—C61A—C66A66 (3)
O21—P2—N23—C51105.4 (6)C61B—N22—C61A—C66A173 (16)
N22—P2—N23—C51−131.5 (5)C23A—N22—C61A—C66A64 (3)
N21—P2—N23—C51−10.3 (6)P2—N22—C61A—C66A−96 (3)
O21—P2—N23—C24−65.5 (8)C66A—C61A—C62A—C63A0(2)
N22—P2—N23—C2457.6 (8)N22—C61A—C62A—C63A176 (3)
N21—P2—N23—C24178.7 (7)C61A—C62A—C63A—C64A2(3)
O11—P1—N13—C41−130.9 (6)C62A—C63A—C64A—C65A−6(5)
N12—P1—N13—C41105.1 (6)C63A—C64A—C65A—C66A8(6)
N11—P1—N13—C41−14.7 (7)C62A—C61A—C66A—C65A3(4)
O11—P1—N13—C2948.1 (7)N22—C61A—C66A—C65A−173 (3)
N12—P1—N13—C29−75.9 (7)C64A—C65A—C66A—C61A−6(5)
N11—P1—N13—C29164.2 (7)C63B—C62B—C61B—C66B0(2)
O10—N4—O9—U176.7 (5)C63B—C62B—C61B—N22177 (2)
O8—N4—O9—U−2.8 (6)C23B—N22—C61B—C62B−95 (2)
O3—U—O9—N493.5 (4)C61A—N22—C61B—C62B−172 (16)
O4—U—O9—N4−86.6 (4)C23A—N22—C61B—C62B−94 (2)
O21—U—O9—N42.3 (4)P2—N22—C61B—C62B94 (2)
O11—U—O9—N4−176.3 (4)C23B—N22—C61B—C66B82 (3)
O6—U—O9—N4−177.4 (3)C61A—N22—C61B—C66B5(13)
O8—U—O9—N41.7 (3)C23A—N22—C61B—C66B83 (3)
O5—U—O9—N4−75 (3)P2—N22—C61B—C66B−90 (2)
N3—U—O9—N4−173.5 (4)C61B—C62B—C63B—C64B5(2)
U—O5—N3—O7177.9 (6)C62B—C63B—C64B—C65B−15 (4)
U—O5—N3—O6−0.3 (6)C63B—C64B—C65B—C66B20 (5)
U—O6—N3—O7−177.9 (6)C62B—C61B—C66B—C65B5(4)
U—O6—N3—O50.3 (6)N22—C61B—C66B—C65B−171 (3)
O3—U—N3—O7143 (12)C64B—C65B—C66B—C61B−15 (5)
D—H···AD—HH···AD···AD—H···A
N11—H11A···O60.862.062.811 (6)146
N21—H21A···O80.862.112.861 (6)146
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
N11—H11A⋯O60.862.062.811 (6)146
N21—H21A⋯O80.862.112.861 (6)146
  2 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  N-{Bis[meth-yl(phen-yl)amino]phosphor-yl}-2,2,2-trichloro-acetamide.

Authors:  Kateryna O Znovjyak; Vladimir A Ovchynnikov; Tetyana Yu Sliva; Svitlana V Shishkina; Vladimir M Amirkhanov
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-10-23
  2 in total

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