catena-Poly[1,2-ethyl­enediammonium [[nitratouran­yl]-μ₃-phosphito] dihydrate]

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.

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

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Computing details

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]

Crystal data

(C2H10N2)[U(HPO3)(NO3)O2]·2H2O	Z = 1
Mr = 922.18	F(000) = 414
Triclinic, P1	Dx = 3.250 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.0106 (17) Å	Cell parameters from 3075 reflections
b = 7.643 (2) Å	θ = 2.3–27.5°
c = 9.846 (1) Å	µ = 17.43 mm^−1
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) Å^3

Data collection

Rigaku R-AXIS RAPID diffractometer	2086 independent reflections
Radiation source: rotor target	1949 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.038
ω scans	θmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −9→8
Tmin = 0.040, Tmax = 0.342	k = −9→9
3928 measured reflections	l = −12→11

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.078	H-atom parameters constrained
S = 1.17	w = 1/[σ^2(Fo^2) + (0.0529P)^2 + 0.6522P] where P = (Fo^2 + 2Fc^2)/3
2086 reflections	(Δ/σ)max = 0.002
131 parameters	Δρmax = 1.53 e Å^−3
0 restraints	Δρmin = −1.31 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
U1	0.35166 (3)	0.77670 (3)	0.16936 (2)	0.01811 (10)
P1	−0.1796 (2)	0.7259 (2)	0.06503 (19)	0.0190 (3)
H	−0.166 (13)	0.883 (12)	0.030 (9)	0.023*
O1	0.4131 (8)	0.7778 (8)	0.3536 (6)	0.0285 (11)
O2	0.2936 (9)	0.7832 (9)	−0.0115 (7)	0.0359 (13)
O3	0.0156 (7)	0.7422 (8)	0.1682 (6)	0.0272 (10)
O4	−0.2416 (8)	0.5540 (7)	−0.0798 (6)	0.0292 (11)
O5	−0.3388 (7)	0.7277 (8)	0.1513 (6)	0.0324 (12)
O6	0.3036 (8)	1.1068 (8)	0.2811 (7)	0.0383 (13)
O7	0.6024 (8)	1.1064 (8)	0.2590 (6)	0.0363 (12)
O8	0.5373 (14)	1.3781 (9)	0.3547 (10)	0.067 (2)
OW1	0.9858 (10)	0.5959 (9)	0.6801 (7)	0.0428 (14)
H1W	0.9047	0.5561	0.7214	0.051*
H2W	1.0922	0.6416	0.7465	0.051*
N1	0.4829 (11)	1.2044 (9)	0.2995 (8)	0.0349 (14)
N2	1.1369 (10)	1.2637 (9)	0.5525 (8)	0.0328 (14)
H2A	1.0892	1.3620	0.5423	0.049*
H2B	1.2388	1.2543	0.5075	0.049*
H2C	1.1845	1.2870	0.6508	0.049*
C1	0.9695 (11)	1.0794 (10)	0.4818 (8)	0.0288 (15)
H1A	0.8489	1.0977	0.5169	0.035*
H1B	0.9325	1.0436	0.3726	0.035*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
U1	0.01050 (14)	0.02447 (15)	0.01702 (14)	0.00560 (9)	0.00366 (9)	0.00430 (10)
P1	0.0122 (7)	0.0191 (7)	0.0231 (8)	0.0051 (6)	0.0045 (6)	0.0044 (6)
O1	0.026 (3)	0.031 (3)	0.027 (3)	0.008 (2)	0.007 (2)	0.010 (2)
O2	0.027 (3)	0.051 (3)	0.032 (3)	0.011 (3)	0.010 (2)	0.017 (3)
O3	0.012 (2)	0.039 (3)	0.028 (2)	0.0098 (19)	0.0080 (19)	0.007 (2)
O4	0.026 (3)	0.029 (3)	0.026 (2)	0.008 (2)	0.006 (2)	0.003 (2)
O5	0.014 (2)	0.038 (3)	0.039 (3)	0.012 (2)	0.009 (2)	0.003 (2)
O6	0.026 (3)	0.032 (3)	0.051 (3)	0.009 (2)	0.008 (2)	0.008 (2)
O7	0.026 (3)	0.039 (3)	0.039 (3)	0.002 (2)	0.008 (2)	0.013 (2)
O8	0.082 (6)	0.022 (3)	0.075 (5)	0.000 (3)	0.006 (4)	0.010 (3)
OW1	0.041 (3)	0.049 (4)	0.044 (3)	0.012 (3)	0.013 (3)	0.023 (3)
N1	0.035 (3)	0.028 (3)	0.038 (4)	0.011 (3)	0.004 (3)	0.009 (3)
N2	0.032 (3)	0.024 (3)	0.037 (3)	0.007 (3)	0.001 (3)	0.009 (3)
C1	0.022 (3)	0.032 (4)	0.028 (3)	0.011 (3)	0.002 (3)	0.006 (3)

Geometric parameters (Å, º)

U1—O1	1.784 (5)	O6—N1	1.268 (9)
U1—O2	1.772 (6)	O7—N1	1.272 (9)
U1—O3	2.313 (5)	O8—N1	1.207 (9)
U1—O4^i	2.298 (5)	OW1—H1W	0.8199
U1—O5^ii	2.307 (5)	OW1—H2W	0.8210
U1—O6	2.534 (6)	N2—C1	1.494 (9)
U1—O7	2.526 (5)	N2—H2A	0.9100
U1—N1	2.970 (7)	N2—H2B	0.9100
P1—O3	1.504 (5)	N2—H2C	0.9100
P1—O4	1.515 (5)	C1—C1^iii	1.491 (14)
P1—O5	1.520 (5)	C1—H1A	0.9900
P1—H	1.34 (8)	C1—H1B	0.9900
O2—U1—O1	178.3 (2)	O3—P1—O5	107.3 (3)
O2—U1—O4^i	92.5 (3)	O4—P1—O5	113.3 (3)
O1—U1—O4^i	89.2 (2)	O3—P1—H	111 (4)
O2—U1—O5^ii	92.2 (2)	O4—P1—H	107 (4)
O1—U1—O5^ii	87.9 (2)	O5—P1—H	105 (4)
O4^i—U1—O5^ii	83.55 (19)	P1—O3—U1	138.6 (3)
O2—U1—O3	89.2 (2)	P1—O4—U1^i	140.6 (3)
O1—U1—O3	91.1 (2)	P1—O5—U1^iv	147.0 (4)
O4^i—U1—O3	82.01 (19)	N1—O6—U1	97.1 (4)
O5^ii—U1—O3	165.5 (2)	N1—O7—U1	97.4 (4)
O2—U1—O7	89.0 (2)	H1W—OW1—H2W	102.4
O1—U1—O7	89.4 (2)	O8—N1—O6	122.2 (8)
O4^i—U1—O7	157.0 (2)	O8—N1—O7	122.4 (8)
O5^ii—U1—O7	73.4 (2)	O6—N1—O7	115.3 (6)
O3—U1—O7	120.98 (19)	O8—N1—U1	178.9 (7)
O2—U1—O6	91.2 (3)	O6—N1—U1	57.8 (4)
O1—U1—O6	87.3 (2)	O7—N1—U1	57.5 (4)
O4^i—U1—O6	152.58 (19)	C1—N2—H2A	109.5
O5^ii—U1—O6	123.44 (18)	C1—N2—H2B	109.5
O3—U1—O6	70.88 (18)	H2A—N2—H2B	109.5
O7—U1—O6	50.19 (19)	C1—N2—H2C	109.5
O2—U1—N1	90.0 (3)	H2A—N2—H2C	109.5
O1—U1—N1	88.3 (2)	H2B—N2—H2C	109.5
O4^i—U1—N1	176.65 (19)	C1^iii—C1—N2	111.3 (7)
O5^ii—U1—N1	98.5 (2)	C1^iii—C1—H1A	109.4
O3—U1—N1	95.89 (19)	N2—C1—H1A	109.4
O7—U1—N1	25.1 (2)	C1^iii—C1—H1B	109.4
O6—U1—N1	25.06 (19)	N2—C1—H1B	109.4
O3—P1—O4	113.3 (3)	H1A—C1—H1B	108.0

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···OW1^v	0.91	2.22	2.955 (10)	138
N2—H2A···OW1^iii	0.91	2.30	2.893 (10)	123
N2—H2B···O6^ii	0.91	2.33	3.104 (10)	143
N2—H2C···O3^vi	0.91	2.49	3.136 (9)	128
N2—H2C···O5^vi	0.91	2.10	2.975 (9)	161
OW1—H1W···O4^vii	0.82	2.37	3.142 (9)	157
OW1—H2W···O2^vii	0.82	2.31	3.080 (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.