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
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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]·2H2O | F(000) = 1100 |
Mr = 558.32 | Dx = 2.128 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 7829 reflections |
a = 11.089 (7) Å | θ = 3–28.5° |
b = 8.936 (5) Å | µ = 2.72 mm−1 |
c = 17.963 (13) Å | T = 293 K |
β = 101.77 (6)° | Irregular fragment, colourless |
V = 1742.6 (19) Å3 | 0.4 × 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 tube | 1990 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
ω scans | θmax = 28.4°, θmin = 3.3° |
Absorption correction: analytical | h = −14→14 |
Tmin = 0.392, Tmax = 0.467 | k = −11→11 |
5214 measured reflections | l = −16→23 |
Refinement top
Refinement on F2 | Primary atom site location: real-space vector search |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.027 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.075 | All 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 parameters | Δρmax = 0.76 e Å−3 |
0 restraints | Δρmin = −0.74 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 | Uiso*/Ueq | |
Ce | 0.0000 | 0.05663 (3) | 0.2500 | 0.02210 (10) | |
N1 | 0.0000 | −0.2931 (5) | 0.2500 | 0.0322 (9) | |
O1 | −0.0935 (2) | −0.2210 (3) | 0.25897 (18) | 0.0372 (6) | |
O2 | 0.0000 | −0.4280 (6) | 0.2500 | 0.115 (4) | |
N2 | −0.0185 (3) | 0.3229 (4) | 0.3566 (2) | 0.0389 (8) | |
O3 | 0.0792 (3) | 0.2498 (3) | 0.36000 (18) | 0.0418 (7) | |
O4 | −0.1076 (3) | 0.2922 (3) | 0.30223 (18) | 0.0414 (7) | |
O5 | −0.0276 (4) | 0.4195 (5) | 0.4037 (3) | 0.0737 (14) | |
N3 | 0.0139 (4) | −0.0787 (5) | 0.0926 (2) | 0.0488 (10) | |
O6 | −0.0843 (3) | −0.0852 (4) | 0.11837 (18) | 0.0407 (7) | |
O7 | 0.0990 (3) | 0.0027 (4) | 0.12858 (19) | 0.0481 (7) | |
O8 | 0.0258 (5) | −0.1478 (8) | 0.0360 (3) | 0.105 (2) | |
OW1 | 0.2338 (2) | 0.0545 (3) | 0.28986 (18) | 0.0327 (6) | |
OW2 | 0.2791 (5) | 0.1431 (8) | 0.0598 (3) | 0.112 (2) | |
N4 | 0.2963 (4) | 0.1148 (6) | 0.4699 (3) | 0.0660 (14) | |
H1W1 | 0.269 (6) | −0.013 (8) | 0.287 (3) | 0.051 (17)* | |
H2W1 | 0.266 (7) | 0.159 (10) | 0.273 (5) | 0.11 (3)* | |
H1W2 | ? | ? | ? | ?* | |
H2W2 | ? | ? | ? | ?* | |
H1N4 | ? | ? | ? | ?* | |
H2N4 | ? | ? | ? | ?* | |
H3N4 | ? | ? | ? | ?* | |
H4N4 | ? | ? | ? | ?* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ce | 0.01907 (14) | 0.01789 (14) | 0.02893 (15) | 0.000 | 0.00396 (9) | 0.000 |
N1 | 0.035 (2) | 0.021 (2) | 0.045 (2) | 0.000 | 0.0184 (19) | 0.000 |
O1 | 0.0266 (13) | 0.0288 (13) | 0.0591 (18) | 0.0007 (11) | 0.0153 (12) | −0.0011 (13) |
O2 | 0.106 (6) | 0.020 (2) | 0.255 (12) | 0.000 | 0.121 (7) | 0.000 |
N2 | 0.0346 (17) | 0.0321 (17) | 0.0445 (18) | 0.0076 (14) | −0.0047 (14) | −0.0116 (15) |
O3 | 0.0287 (13) | 0.0384 (15) | 0.0524 (17) | 0.0103 (12) | −0.0053 (12) | −0.0096 (13) |
O4 | 0.0324 (14) | 0.0325 (14) | 0.0511 (17) | 0.0050 (11) | −0.0105 (12) | −0.0108 (13) |
O5 | 0.067 (2) | 0.068 (3) | 0.073 (3) | 0.031 (2) | −0.015 (2) | −0.042 (2) |
N3 | 0.046 (2) | 0.065 (3) | 0.0361 (18) | 0.0033 (19) | 0.0117 (16) | −0.0165 (18) |
O6 | 0.0365 (15) | 0.0426 (16) | 0.0438 (16) | −0.0029 (12) | 0.0102 (13) | −0.0081 (13) |
O7 | 0.0411 (17) | 0.060 (2) | 0.0456 (17) | −0.0074 (16) | 0.0149 (14) | −0.0013 (16) |
O8 | 0.097 (4) | 0.151 (5) | 0.076 (3) | −0.003 (4) | 0.038 (3) | −0.071 (3) |
OW1 | 0.0199 (12) | 0.0261 (14) | 0.0521 (17) | 0.0016 (10) | 0.0076 (11) | 0.0076 (12) |
OW2 | 0.091 (4) | 0.161 (6) | 0.091 (4) | −0.061 (4) | 0.038 (3) | −0.028 (4) |
N4 | 0.054 (3) | 0.056 (3) | 0.076 (3) | 0.012 (2) | −0.016 (2) | −0.021 (2) |
Geometric parameters (Å, º) top
Ce—OW1i | 2.545 (3) | Ce—O1i | 2.707 (3) |
Ce—OW1 | 2.545 (3) | N1—O2 | 1.206 (7) |
Ce—O3 | 2.636 (3) | N1—O1 | 1.259 (3) |
Ce—O3i | 2.636 (3) | N1—O1i | 1.259 (3) |
Ce—O6 | 2.678 (4) | N2—O5 | 1.227 (5) |
Ce—O6i | 2.678 (3) | N2—O3 | 1.256 (4) |
Ce—O7i | 2.678 (4) | N2—O4 | 1.270 (4) |
Ce—O7 | 2.678 (4) | N3—O8 | 1.219 (5) |
Ce—O4 | 2.681 (3) | N3—O7 | 1.261 (5) |
Ce—O4i | 2.681 (3) | N3—O6 | 1.268 (5) |
Ce—O1 | 2.707 (3) | | |
| | | |
OW1i—Ce—OW1 | 179.16 (14) | O6—Ce—O4i | 99.36 (11) |
OW1i—Ce—O3 | 112.36 (10) | O6i—Ce—O4i | 125.49 (10) |
OW1—Ce—O3 | 68.23 (10) | O7i—Ce—O4i | 135.39 (11) |
OW1i—Ce—O3i | 68.23 (10) | O7—Ce—O4i | 64.58 (11) |
OW1—Ce—O3i | 112.36 (10) | O4—Ce—O4i | 76.57 (15) |
O3—Ce—O3i | 98.19 (15) | OW1i—Ce—O1 | 68.24 (9) |
OW1i—Ce—O6 | 66.18 (11) | OW1—Ce—O1 | 110.93 (9) |
OW1—Ce—O6 | 113.39 (11) | O3—Ce—O1 | 128.96 (11) |
O3—Ce—O6 | 167.15 (10) | O3i—Ce—O1 | 124.87 (10) |
O3i—Ce—O6 | 69.21 (11) | O6—Ce—O1 | 63.23 (10) |
OW1i—Ce—O6i | 113.39 (11) | O6i—Ce—O1 | 65.32 (10) |
OW1—Ce—O6i | 66.18 (11) | O7i—Ce—O1 | 63.94 (11) |
O3—Ce—O6i | 69.21 (11) | O7—Ce—O1 | 96.27 (11) |
O3i—Ce—O6i | 167.15 (10) | O4—Ce—O1 | 119.70 (10) |
O6—Ce—O6i | 123.48 (15) | O4i—Ce—O1 | 160.67 (10) |
OW1i—Ce—O7i | 70.39 (12) | OW1i—Ce—O1i | 110.93 (9) |
OW1—Ce—O7i | 109.45 (11) | OW1—Ce—O1i | 68.24 (9) |
O3—Ce—O7i | 68.70 (12) | O3—Ce—O1i | 124.87 (10) |
O3i—Ce—O7i | 126.81 (11) | O3i—Ce—O1i | 128.96 (11) |
O6—Ce—O7i | 120.44 (11) | O6—Ce—O1i | 65.32 (10) |
O6i—Ce—O7i | 47.38 (10) | O6i—Ce—O1i | 63.23 (10) |
OW1i—Ce—O7 | 109.45 (11) | O7i—Ce—O1i | 96.27 (11) |
OW1—Ce—O7 | 70.39 (12) | O7—Ce—O1i | 63.94 (11) |
O3—Ce—O7 | 126.81 (11) | O4—Ce—O1i | 160.67 (10) |
O3i—Ce—O7 | 68.70 (12) | O4i—Ce—O1i | 119.70 (10) |
O6—Ce—O7 | 47.38 (10) | O1—Ce—O1i | 47.11 (12) |
O6i—Ce—O7 | 120.44 (11) | O2—N1—O1 | 120.8 (2) |
O7i—Ce—O7 | 159.25 (17) | O2—N1—O1i | 120.8 (2) |
OW1i—Ce—O4 | 66.66 (9) | O1—N1—O1i | 118.5 (4) |
OW1—Ce—O4 | 114.06 (10) | N1—O1—Ce | 97.2 (2) |
O3—Ce—O4 | 47.76 (9) | O5—N2—O3 | 121.6 (4) |
O3i—Ce—O4 | 69.16 (11) | O5—N2—O4 | 121.5 (4) |
O6—Ce—O4 | 125.49 (10) | O3—N2—O4 | 116.9 (3) |
O6i—Ce—O4 | 99.36 (11) | N2—O3—Ce | 98.7 (2) |
O7i—Ce—O4 | 64.58 (11) | N2—O4—Ce | 96.2 (2) |
O7—Ce—O4 | 135.39 (11) | O8—N3—O7 | 121.5 (5) |
OW1i—Ce—O4i | 114.06 (10) | O8—N3—O6 | 121.9 (5) |
OW1—Ce—O4i | 66.66 (9) | O7—N3—O6 | 116.6 (4) |
O3—Ce—O4i | 69.16 (11) | N3—O6—Ce | 97.5 (2) |
O3i—Ce—O4i | 47.76 (9) | N3—O7—Ce | 97.6 (2) |
Symmetry code: (i) −x, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—H1W1···O4ii | 0.72 (8) | 2.20 (7) | 2.912 (4) | 168 (8) |
OW1—H2W1···O1iii | 1.07 (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, y−1/2, z; (iii) x+1/2, y+1/2, z; (iv) −x+1/2, −y+1/2, −z; (v) x, −y, z−1/2; (vi) −x+1/2, y+1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1. |