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The crystal structure of the title compound, {(C2H10N2)[U(HPO3)(NO3)O2]·2H2O}n, consists of polymeric uranyl complex anions, ethyl­enediammonium cations and uncoord­inated water mol­ecules. The polymeric uranyl complex anion displays a ladder-like structure, each UO2 unit being coordinated by three phosphite dianions and one nitrate anion with a penta­gonal–bipyramidal geometry. The ethyl­enediammonium cation is located on an inversion center and is hydrogen bonded with the uranyl complex.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806008476/xu2007sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806008476/xu2007Isup2.hkl
Contains datablock I

CCDC reference: 605217

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.011 Å
  • R factor = 0.025
  • wR factor = 0.078
  • Data-to-parameter ratio = 15.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL.

catena-Poly[1,2-ethylenediammonium [[nitratouranyl]-µ3-phosphito] dihydrate] top
Crystal data top
(C2H10N2)[U(HPO3)(NO3)O2]·2H2OZ = 1
Mr = 922.18F(000) = 414
Triclinic, P1Dx = 3.250 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.0106 (17) ÅCell parameters from 3075 reflections
b = 7.643 (2) Åθ = 2.3–27.5°
c = 9.846 (1) ŵ = 17.43 mm1
α = 108.522 (7)°T = 298 K
β = 100.469 (8)°Needle, yellow
γ = 102.125 (9)°0.58 × 0.17 × 0.06 mm
V = 471.20 (18) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
2086 independent reflections
Radiation source: rotor target1949 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
ω scansθmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 98
Tmin = 0.040, Tmax = 0.342k = 99
3928 measured reflectionsl = 1211
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)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.078H-atom parameters constrained
S = 1.17 w = 1/[σ2(Fo2) + (0.0529P)2 + 0.6522P]
where P = (Fo2 + 2Fc2)/3
2086 reflections(Δ/σ)max = 0.002
131 parametersΔρmax = 1.53 e Å3
0 restraintsΔρmin = 1.31 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
U10.35166 (3)0.77670 (3)0.16936 (2)0.01811 (10)
P10.1796 (2)0.7259 (2)0.06503 (19)0.0190 (3)
H0.166 (13)0.883 (12)0.030 (9)0.023*
O10.4131 (8)0.7778 (8)0.3536 (6)0.0285 (11)
O20.2936 (9)0.7832 (9)0.0115 (7)0.0359 (13)
O30.0156 (7)0.7422 (8)0.1682 (6)0.0272 (10)
O40.2416 (8)0.5540 (7)0.0798 (6)0.0292 (11)
O50.3388 (7)0.7277 (8)0.1513 (6)0.0324 (12)
O60.3036 (8)1.1068 (8)0.2811 (7)0.0383 (13)
O70.6024 (8)1.1064 (8)0.2590 (6)0.0363 (12)
O80.5373 (14)1.3781 (9)0.3547 (10)0.067 (2)
OW10.9858 (10)0.5959 (9)0.6801 (7)0.0428 (14)
H1W0.90470.55610.72140.051*
H2W1.09220.64160.74650.051*
N10.4829 (11)1.2044 (9)0.2995 (8)0.0349 (14)
N21.1369 (10)1.2637 (9)0.5525 (8)0.0328 (14)
H2A1.08921.36200.54230.049*
H2B1.23881.25430.50750.049*
H2C1.18451.28700.65080.049*
C10.9695 (11)1.0794 (10)0.4818 (8)0.0288 (15)
H1A0.84891.09770.51690.035*
H1B0.93251.04360.37260.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U10.01050 (14)0.02447 (15)0.01702 (14)0.00560 (9)0.00366 (9)0.00430 (10)
P10.0122 (7)0.0191 (7)0.0231 (8)0.0051 (6)0.0045 (6)0.0044 (6)
O10.026 (3)0.031 (3)0.027 (3)0.008 (2)0.007 (2)0.010 (2)
O20.027 (3)0.051 (3)0.032 (3)0.011 (3)0.010 (2)0.017 (3)
O30.012 (2)0.039 (3)0.028 (2)0.0098 (19)0.0080 (19)0.007 (2)
O40.026 (3)0.029 (3)0.026 (2)0.008 (2)0.006 (2)0.003 (2)
O50.014 (2)0.038 (3)0.039 (3)0.012 (2)0.009 (2)0.003 (2)
O60.026 (3)0.032 (3)0.051 (3)0.009 (2)0.008 (2)0.008 (2)
O70.026 (3)0.039 (3)0.039 (3)0.002 (2)0.008 (2)0.013 (2)
O80.082 (6)0.022 (3)0.075 (5)0.000 (3)0.006 (4)0.010 (3)
OW10.041 (3)0.049 (4)0.044 (3)0.012 (3)0.013 (3)0.023 (3)
N10.035 (3)0.028 (3)0.038 (4)0.011 (3)0.004 (3)0.009 (3)
N20.032 (3)0.024 (3)0.037 (3)0.007 (3)0.001 (3)0.009 (3)
C10.022 (3)0.032 (4)0.028 (3)0.011 (3)0.002 (3)0.006 (3)
Geometric parameters (Å, º) top
U1—O11.784 (5)O6—N11.268 (9)
U1—O21.772 (6)O7—N11.272 (9)
U1—O32.313 (5)O8—N11.207 (9)
U1—O4i2.298 (5)OW1—H1W0.8199
U1—O5ii2.307 (5)OW1—H2W0.8210
U1—O62.534 (6)N2—C11.494 (9)
U1—O72.526 (5)N2—H2A0.9100
U1—N12.970 (7)N2—H2B0.9100
P1—O31.504 (5)N2—H2C0.9100
P1—O41.515 (5)C1—C1iii1.491 (14)
P1—O51.520 (5)C1—H1A0.9900
P1—H1.34 (8)C1—H1B0.9900
O2—U1—O1178.3 (2)O3—P1—O5107.3 (3)
O2—U1—O4i92.5 (3)O4—P1—O5113.3 (3)
O1—U1—O4i89.2 (2)O3—P1—H111 (4)
O2—U1—O5ii92.2 (2)O4—P1—H107 (4)
O1—U1—O5ii87.9 (2)O5—P1—H105 (4)
O4i—U1—O5ii83.55 (19)P1—O3—U1138.6 (3)
O2—U1—O389.2 (2)P1—O4—U1i140.6 (3)
O1—U1—O391.1 (2)P1—O5—U1iv147.0 (4)
O4i—U1—O382.01 (19)N1—O6—U197.1 (4)
O5ii—U1—O3165.5 (2)N1—O7—U197.4 (4)
O2—U1—O789.0 (2)H1W—OW1—H2W102.4
O1—U1—O789.4 (2)O8—N1—O6122.2 (8)
O4i—U1—O7157.0 (2)O8—N1—O7122.4 (8)
O5ii—U1—O773.4 (2)O6—N1—O7115.3 (6)
O3—U1—O7120.98 (19)O8—N1—U1178.9 (7)
O2—U1—O691.2 (3)O6—N1—U157.8 (4)
O1—U1—O687.3 (2)O7—N1—U157.5 (4)
O4i—U1—O6152.58 (19)C1—N2—H2A109.5
O5ii—U1—O6123.44 (18)C1—N2—H2B109.5
O3—U1—O670.88 (18)H2A—N2—H2B109.5
O7—U1—O650.19 (19)C1—N2—H2C109.5
O2—U1—N190.0 (3)H2A—N2—H2C109.5
O1—U1—N188.3 (2)H2B—N2—H2C109.5
O4i—U1—N1176.65 (19)C1iii—C1—N2111.3 (7)
O5ii—U1—N198.5 (2)C1iii—C1—H1A109.4
O3—U1—N195.89 (19)N2—C1—H1A109.4
O7—U1—N125.1 (2)C1iii—C1—H1B109.4
O6—U1—N125.06 (19)N2—C1—H1B109.4
O3—P1—O4113.3 (3)H1A—C1—H1B108.0
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z; (iii) x+2, y+2, z+1; (iv) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···OW1v0.912.222.955 (10)138
N2—H2A···OW1iii0.912.302.893 (10)123
N2—H2B···O6ii0.912.333.104 (10)143
N2—H2C···O3vi0.912.493.136 (9)128
N2—H2C···O5vi0.912.102.975 (9)161
OW1—H1W···O4vii0.822.373.142 (9)157
OW1—H2W···O2vii0.822.313.080 (9)156
Symmetry codes: (ii) x+1, y, z; (iii) x+2, y+2, z+1; (v) x, y+1, z; (vi) x+1, y+2, z+1; (vii) x+1, y, z+1.
 

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