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The structure of the title compound, (NH4)2[Ce(NO3)5(H2O)2]·2H2O, consists of complex diaqua­penta­nitrato­cerate(III) anions with 12-coordinate Ce atoms, ammonium cations and uncoordinated water mol­ecules. The complex anion lies on a crystallographic twofold axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806006593/br6226sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806006593/br6226Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](O-N) = 0.007 Å
  • H-atom completeness 63%
  • R factor = 0.027
  • wR factor = 0.075
  • Data-to-parameter ratio = 15.3

checkCIF/PLATON results

No syntax errors found



Alert level A TYPE101_ALERT_1_A _atom_site_fract_x is not of type numb. TYPE102_ALERT_1_A _atom_site_fract_y is not of type numb. TYPE103_ALERT_1_A _atom_site_fract_z is not of type numb. TYPE104_ALERT_1_A _atom_site_U_iso_or_equiv is not of type char. PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) H1W2 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW2
Author Response: This is water/ammonium; no attempt to locate the H atoms was undertaken

Alert level B PLAT220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.52 Ratio PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N1 PLAT430_ALERT_2_B Short Inter D...A Contact OW2 .. N4 .. 2.84 Ang.
Alert level C ABSTY02_ALERT_1_C An _exptl_absorpt_correction_type has been given without a literature citation. This should be contained in the _exptl_absorpt_process_details field. Absorption correction given as analytical CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 558.32 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 0.00 0.00 H 1.01 10.00 10.08 N 14.01 7.00 98.05 O 16.00 19.00 303.98 Ce 140.12 1.00 140.12 Calculated formula weight 552.23 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 558.32 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT150_ALERT_1_C Volume as Calculated Differs from that Given ... 1742.60 Ang-3 PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Ce PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N3 PLAT355_ALERT_3_C Long O-H Bond (0.82A) OW1 - H2W1 ... 1.07 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW2 .. O7 .. 2.85 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW2 .. OW2 .. 2.85 Ang. PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... H2W2 PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... H2W2 PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... H1N4 PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... H2N4 PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... H3N4 PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... H4N4 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:H16 Ce1 N7 O19 Atom count from the _atom_site data: H10 Ce1 N7 O19 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum Ce H16 N7 O19 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff Ce 4.00 4.00 0.00 H 64.00 40.00 24.00 N 28.00 28.00 0.00 O 76.00 76.00 0.00
6 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 22 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 20 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 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: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Crystal Impact, 2005); software used to prepare material for publication: SHELXL97.

Diammonium diaquapentanitratocerate(III) dihydrate top
Crystal data top
(NH4)2[Ce(NO3)5(H2O)2]·2H2OF(000) = 1100
Mr = 558.32Dx = 2.128 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 7829 reflections
a = 11.089 (7) Åθ = 3–28.5°
b = 8.936 (5) ŵ = 2.72 mm1
c = 17.963 (13) ÅT = 293 K
β = 101.77 (6)°Irregular fragment, colourless
V = 1742.6 (19) Å30.4 × 0.35 × 0.3 mm
Z = 4
Data collection top
Kuma KM-4 with a CCD counter
diffractometer
2014 independent reflections
Radiation source: fine-focus sealed tube1990 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
ω scansθmax = 28.4°, θmin = 3.3°
Absorption correction: analyticalh = 1414
Tmin = 0.392, Tmax = 0.467k = 1111
5214 measured reflectionsl = 1623
Refinement top
Refinement on F2Primary atom site location: real-space vector search
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: difference Fourier map
wR(F2) = 0.075All H-atom parameters refined
S = 1.16 w = 1/[σ2(Fo2) + (0.03P)2 + 9.6P]
where P = (Fo2 + 2Fc2)/3
2014 reflections(Δ/σ)max = 0.001
132 parametersΔρmax = 0.76 e Å3
0 restraintsΔρmin = 0.74 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
Ce0.00000.05663 (3)0.25000.02210 (10)
N10.00000.2931 (5)0.25000.0322 (9)
O10.0935 (2)0.2210 (3)0.25897 (18)0.0372 (6)
O20.00000.4280 (6)0.25000.115 (4)
N20.0185 (3)0.3229 (4)0.3566 (2)0.0389 (8)
O30.0792 (3)0.2498 (3)0.36000 (18)0.0418 (7)
O40.1076 (3)0.2922 (3)0.30223 (18)0.0414 (7)
O50.0276 (4)0.4195 (5)0.4037 (3)0.0737 (14)
N30.0139 (4)0.0787 (5)0.0926 (2)0.0488 (10)
O60.0843 (3)0.0852 (4)0.11837 (18)0.0407 (7)
O70.0990 (3)0.0027 (4)0.12858 (19)0.0481 (7)
O80.0258 (5)0.1478 (8)0.0360 (3)0.105 (2)
OW10.2338 (2)0.0545 (3)0.28986 (18)0.0327 (6)
OW20.2791 (5)0.1431 (8)0.0598 (3)0.112 (2)
N40.2963 (4)0.1148 (6)0.4699 (3)0.0660 (14)
H1W10.269 (6)0.013 (8)0.287 (3)0.051 (17)*
H2W10.266 (7)0.159 (10)0.273 (5)0.11 (3)*
H1W2????*
H2W2????*
H1N4????*
H2N4????*
H3N4????*
H4N4????*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ce0.01907 (14)0.01789 (14)0.02893 (15)0.0000.00396 (9)0.000
N10.035 (2)0.021 (2)0.045 (2)0.0000.0184 (19)0.000
O10.0266 (13)0.0288 (13)0.0591 (18)0.0007 (11)0.0153 (12)0.0011 (13)
O20.106 (6)0.020 (2)0.255 (12)0.0000.121 (7)0.000
N20.0346 (17)0.0321 (17)0.0445 (18)0.0076 (14)0.0047 (14)0.0116 (15)
O30.0287 (13)0.0384 (15)0.0524 (17)0.0103 (12)0.0053 (12)0.0096 (13)
O40.0324 (14)0.0325 (14)0.0511 (17)0.0050 (11)0.0105 (12)0.0108 (13)
O50.067 (2)0.068 (3)0.073 (3)0.031 (2)0.015 (2)0.042 (2)
N30.046 (2)0.065 (3)0.0361 (18)0.0033 (19)0.0117 (16)0.0165 (18)
O60.0365 (15)0.0426 (16)0.0438 (16)0.0029 (12)0.0102 (13)0.0081 (13)
O70.0411 (17)0.060 (2)0.0456 (17)0.0074 (16)0.0149 (14)0.0013 (16)
O80.097 (4)0.151 (5)0.076 (3)0.003 (4)0.038 (3)0.071 (3)
OW10.0199 (12)0.0261 (14)0.0521 (17)0.0016 (10)0.0076 (11)0.0076 (12)
OW20.091 (4)0.161 (6)0.091 (4)0.061 (4)0.038 (3)0.028 (4)
N40.054 (3)0.056 (3)0.076 (3)0.012 (2)0.016 (2)0.021 (2)
Geometric parameters (Å, º) top
Ce—OW1i2.545 (3)Ce—O1i2.707 (3)
Ce—OW12.545 (3)N1—O21.206 (7)
Ce—O32.636 (3)N1—O11.259 (3)
Ce—O3i2.636 (3)N1—O1i1.259 (3)
Ce—O62.678 (4)N2—O51.227 (5)
Ce—O6i2.678 (3)N2—O31.256 (4)
Ce—O7i2.678 (4)N2—O41.270 (4)
Ce—O72.678 (4)N3—O81.219 (5)
Ce—O42.681 (3)N3—O71.261 (5)
Ce—O4i2.681 (3)N3—O61.268 (5)
Ce—O12.707 (3)
OW1i—Ce—OW1179.16 (14)O6—Ce—O4i99.36 (11)
OW1i—Ce—O3112.36 (10)O6i—Ce—O4i125.49 (10)
OW1—Ce—O368.23 (10)O7i—Ce—O4i135.39 (11)
OW1i—Ce—O3i68.23 (10)O7—Ce—O4i64.58 (11)
OW1—Ce—O3i112.36 (10)O4—Ce—O4i76.57 (15)
O3—Ce—O3i98.19 (15)OW1i—Ce—O168.24 (9)
OW1i—Ce—O666.18 (11)OW1—Ce—O1110.93 (9)
OW1—Ce—O6113.39 (11)O3—Ce—O1128.96 (11)
O3—Ce—O6167.15 (10)O3i—Ce—O1124.87 (10)
O3i—Ce—O669.21 (11)O6—Ce—O163.23 (10)
OW1i—Ce—O6i113.39 (11)O6i—Ce—O165.32 (10)
OW1—Ce—O6i66.18 (11)O7i—Ce—O163.94 (11)
O3—Ce—O6i69.21 (11)O7—Ce—O196.27 (11)
O3i—Ce—O6i167.15 (10)O4—Ce—O1119.70 (10)
O6—Ce—O6i123.48 (15)O4i—Ce—O1160.67 (10)
OW1i—Ce—O7i70.39 (12)OW1i—Ce—O1i110.93 (9)
OW1—Ce—O7i109.45 (11)OW1—Ce—O1i68.24 (9)
O3—Ce—O7i68.70 (12)O3—Ce—O1i124.87 (10)
O3i—Ce—O7i126.81 (11)O3i—Ce—O1i128.96 (11)
O6—Ce—O7i120.44 (11)O6—Ce—O1i65.32 (10)
O6i—Ce—O7i47.38 (10)O6i—Ce—O1i63.23 (10)
OW1i—Ce—O7109.45 (11)O7i—Ce—O1i96.27 (11)
OW1—Ce—O770.39 (12)O7—Ce—O1i63.94 (11)
O3—Ce—O7126.81 (11)O4—Ce—O1i160.67 (10)
O3i—Ce—O768.70 (12)O4i—Ce—O1i119.70 (10)
O6—Ce—O747.38 (10)O1—Ce—O1i47.11 (12)
O6i—Ce—O7120.44 (11)O2—N1—O1120.8 (2)
O7i—Ce—O7159.25 (17)O2—N1—O1i120.8 (2)
OW1i—Ce—O466.66 (9)O1—N1—O1i118.5 (4)
OW1—Ce—O4114.06 (10)N1—O1—Ce97.2 (2)
O3—Ce—O447.76 (9)O5—N2—O3121.6 (4)
O3i—Ce—O469.16 (11)O5—N2—O4121.5 (4)
O6—Ce—O4125.49 (10)O3—N2—O4116.9 (3)
O6i—Ce—O499.36 (11)N2—O3—Ce98.7 (2)
O7i—Ce—O464.58 (11)N2—O4—Ce96.2 (2)
O7—Ce—O4135.39 (11)O8—N3—O7121.5 (5)
OW1i—Ce—O4i114.06 (10)O8—N3—O6121.9 (5)
OW1—Ce—O4i66.66 (9)O7—N3—O6116.6 (4)
O3—Ce—O4i69.16 (11)N3—O6—Ce97.5 (2)
O3i—Ce—O4i47.76 (9)N3—O7—Ce97.6 (2)
Symmetry code: (i) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW1—H1W1···O4ii0.72 (8)2.20 (7)2.912 (4)168 (8)
OW1—H2W1···O1iii1.07 (9)1.95 (9)2.903 (4)147 (7)
OW2—H2W2···OW2iv??2.849 (15)?
OW2—H1W2···N4v??2.842 (9)?
OW2—H2W2···O6iii??2.941 (7)?
N4—H1N4···O8vi??2.914 (8)?
N4—H2N4···N4vii??2.918 (9)?
N4—H3N4···O3??3.035 (6)?
N4—H4N4···O5ii??3.037 (6)?
Symmetry codes: (ii) x+1/2, y1/2, z; (iii) x+1/2, y+1/2, z; (iv) x+1/2, y+1/2, z; (v) x, y, z1/2; (vi) x+1/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1.
 

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