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In the title compound, (CH6N3)2[Pr(NO3)5(H2O)2], the Pr3+ ion is coordinated by 12 O atoms, giving a distorted icosahedron. The Pr3+ cation, one N atom and one O atom lie on a twofold axis.
Supporting information
CCDC reference: 628009
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (N-C) = 0.005 Å
- R factor = 0.020
- wR factor = 0.052
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Pr - O11 .. 10.00 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Pr - O21 .. 12.97 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Pr - O22 .. 10.16 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Pr - O32 .. 12.75 su
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT213_ALERT_2_C Atom O12 has ADP max/min Ratio ............. 3.30 prola
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O31 .. 8.14 su
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Pr
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N11
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1A2 .. O23 .. 2.63 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem
4 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
8 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: IPDS Software (Stoe & Cie, 1998); cell refinement: IPDS Software; data reduction: IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.
Bis(guanidinium) diaquapentanitrato-
κ10O,
O'-praseodymium
top
Crystal data top
(CH6N3)2[Pr(NO3)5(H2O)2] | F(000) = 1200 |
Mr = 607.17 | Dx = 1.984 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 8002 reflections |
a = 10.931 (3) Å | θ = 3–25.9° |
b = 9.071 (3) Å | µ = 2.50 mm−1 |
c = 20.571 (5) Å | T = 293 K |
β = 94.78 (3)° | Block, green |
V = 2032.6 (10) Å3 | 0.56 × 0.41 × 0.41 mm |
Z = 4 | |
Data collection top
Stoe IPDS area-detector diffractometer | 1956 independent reflections |
Radiation source: medium-focus sealed tube | 1822 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
φ scans | θmax = 26.0°, θmin = 2.9° |
Absorption correction: numerical (Stoe & Cie, 1998) | h = −13→13 |
Tmin = 0.210, Tmax = 0.253 | k = −11→11 |
14022 measured reflections | l = −25→25 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.020 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.052 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.037P)2 + 0.3651P] where P = (Fo2 + 2Fc2)/3 |
1956 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.43 e Å−3 |
0 restraints | Δρmin = −0.79 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 | |
Pr | 0.5000 | 0.861324 (18) | 0.7500 | 0.02072 (8) | |
O11 | 0.59530 (16) | 0.5976 (2) | 0.73946 (11) | 0.0364 (4) | |
O12 | 0.5000 | 0.3910 (3) | 0.7500 | 0.0838 (17) | |
N11 | 0.5000 | 0.5229 (3) | 0.7500 | 0.0362 (8) | |
O21 | 0.6132 (2) | 0.8233 (2) | 0.63757 (11) | 0.0430 (5) | |
O22 | 0.43183 (19) | 0.7291 (2) | 0.63608 (10) | 0.0404 (5) | |
O23 | 0.5299 (3) | 0.7213 (3) | 0.54893 (11) | 0.0648 (8) | |
N21 | 0.5256 (2) | 0.7578 (3) | 0.60669 (12) | 0.0375 (6) | |
O31 | 0.43540 (18) | 1.0491 (2) | 0.65959 (10) | 0.0390 (5) | |
O32 | 0.61354 (18) | 1.1021 (2) | 0.70610 (10) | 0.0363 (4) | |
O33 | 0.5420 (3) | 1.2247 (3) | 0.62082 (13) | 0.0657 (8) | |
N31 | 0.5318 (2) | 1.1291 (2) | 0.66136 (13) | 0.0353 (6) | |
C1 | 0.2403 (3) | 0.9993 (4) | 0.50270 (16) | 0.0457 (7) | |
N1A | 0.2079 (3) | 1.0080 (3) | 0.43994 (14) | 0.0602 (8) | |
H1A1 | 0.2421 | 1.0718 | 0.4164 | 0.072* | |
H1A2 | 0.1524 | 0.9498 | 0.4224 | 0.072* | |
N1B | 0.3246 (3) | 1.0880 (4) | 0.52926 (15) | 0.0633 (9) | |
H1B1 | 0.3587 | 1.1517 | 0.5056 | 0.076* | |
H1B2 | 0.3460 | 1.0826 | 0.5704 | 0.076* | |
N1C | 0.1876 (3) | 0.9011 (4) | 0.53889 (19) | 0.0674 (9) | |
H1C1 | 0.2087 | 0.8955 | 0.5800 | 0.081* | |
H1C2 | 0.1322 | 0.8430 | 0.5213 | 0.081* | |
O1W | 0.27266 (18) | 0.86096 (18) | 0.72199 (12) | 0.0380 (5) | |
H1W | 0.2160 | 0.7830 | 0.7186 | 0.046* | |
H2W | 0.2190 | 0.9323 | 0.7284 | 0.046* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pr | 0.01844 (11) | 0.01878 (11) | 0.02496 (12) | 0.000 | 0.00193 (8) | 0.000 |
O11 | 0.0224 (9) | 0.0281 (9) | 0.0604 (13) | −0.0030 (7) | 0.0134 (9) | 0.0000 (9) |
O12 | 0.064 (2) | 0.0180 (15) | 0.178 (5) | 0.000 | 0.060 (3) | 0.000 |
N11 | 0.0278 (16) | 0.0236 (15) | 0.059 (2) | 0.000 | 0.0139 (16) | 0.000 |
O21 | 0.0411 (12) | 0.0445 (11) | 0.0442 (12) | −0.0148 (9) | 0.0084 (10) | −0.0096 (9) |
O22 | 0.0376 (11) | 0.0465 (12) | 0.0385 (11) | −0.0123 (9) | 0.0114 (9) | −0.0080 (9) |
O23 | 0.0756 (18) | 0.0846 (19) | 0.0370 (13) | −0.0320 (15) | 0.0219 (13) | −0.0234 (12) |
N21 | 0.0475 (14) | 0.0352 (12) | 0.0309 (12) | −0.0086 (10) | 0.0103 (11) | −0.0076 (9) |
O31 | 0.0355 (10) | 0.0407 (11) | 0.0393 (11) | −0.0120 (8) | −0.0067 (9) | 0.0100 (8) |
O32 | 0.0349 (10) | 0.0296 (9) | 0.0424 (12) | −0.0044 (8) | −0.0089 (9) | 0.0019 (8) |
O33 | 0.0751 (18) | 0.0611 (16) | 0.0580 (16) | −0.0293 (13) | −0.0107 (14) | 0.0334 (13) |
N31 | 0.0424 (14) | 0.0295 (12) | 0.0333 (13) | −0.0092 (9) | −0.0013 (12) | 0.0082 (9) |
C1 | 0.0445 (18) | 0.0461 (16) | 0.0460 (18) | −0.0096 (13) | 0.0007 (15) | 0.0093 (13) |
N1A | 0.066 (2) | 0.067 (2) | 0.0457 (16) | −0.0356 (16) | −0.0073 (15) | 0.0037 (14) |
N1B | 0.0623 (19) | 0.084 (2) | 0.0412 (16) | −0.0335 (19) | −0.0104 (15) | 0.0123 (16) |
N1C | 0.077 (2) | 0.0593 (18) | 0.067 (2) | −0.0203 (18) | 0.0092 (18) | 0.0214 (17) |
O1W | 0.0197 (9) | 0.0278 (10) | 0.0665 (15) | 0.0001 (7) | 0.0036 (10) | −0.0081 (8) |
Geometric parameters (Å, º) top
Pr—O1Wi | 2.504 (2) | O22—N21 | 1.260 (3) |
Pr—O1W | 2.504 (2) | O23—N21 | 1.238 (3) |
Pr—O31i | 2.577 (2) | O31—N31 | 1.277 (3) |
Pr—O31 | 2.577 (2) | O32—N31 | 1.253 (3) |
Pr—O11i | 2.625 (2) | O33—N31 | 1.214 (3) |
Pr—O11 | 2.625 (2) | C1—N1B | 1.309 (4) |
Pr—O22 | 2.682 (2) | C1—N1A | 1.312 (4) |
Pr—O22i | 2.682 (2) | C1—N1C | 1.323 (4) |
Pr—O32 | 2.704 (2) | N1A—H1A1 | 0.8600 |
Pr—O32i | 2.704 (2) | N1A—H1A2 | 0.8600 |
Pr—O21 | 2.734 (2) | N1B—H1B1 | 0.8600 |
Pr—O21i | 2.734 (2) | N1B—H1B2 | 0.8600 |
O11—N11 | 1.277 (2) | N1C—H1C1 | 0.8600 |
O12—N11 | 1.196 (5) | N1C—H1C2 | 0.8600 |
N11—O11i | 1.277 (2) | O1W—H1W | 0.9390 |
O21—N21 | 1.254 (3) | O1W—H2W | 0.8899 |
| | | |
O1Wi—Pr—O1W | 179.85 (8) | O31—Pr—O21 | 65.73 (7) |
O1Wi—Pr—O31i | 68.14 (7) | O11i—Pr—O21 | 99.54 (6) |
O1W—Pr—O31i | 111.96 (7) | O11—Pr—O21 | 66.71 (7) |
O1Wi—Pr—O31 | 111.96 (7) | O22—Pr—O21 | 46.92 (6) |
O1W—Pr—O31 | 68.14 (7) | O22i—Pr—O21 | 124.77 (7) |
O31i—Pr—O31 | 97.24 (10) | O32—Pr—O21 | 64.32 (6) |
O1Wi—Pr—O11i | 111.90 (6) | O32i—Pr—O21 | 129.57 (7) |
O1W—Pr—O11i | 67.96 (6) | O1Wi—Pr—O21i | 108.40 (8) |
O31i—Pr—O11i | 129.01 (7) | O1W—Pr—O21i | 71.58 (8) |
O31—Pr—O11i | 125.11 (7) | O31i—Pr—O21i | 65.73 (7) |
O1Wi—Pr—O11 | 67.96 (6) | O31—Pr—O21i | 125.29 (6) |
O1W—Pr—O11 | 111.90 (6) | O11i—Pr—O21i | 66.71 (7) |
O31i—Pr—O11 | 125.11 (7) | O11—Pr—O21i | 99.54 (6) |
O31—Pr—O11 | 129.01 (7) | O22—Pr—O21i | 124.77 (7) |
O11i—Pr—O11 | 48.67 (8) | O22i—Pr—O21i | 46.92 (6) |
O1Wi—Pr—O22 | 113.49 (7) | O32—Pr—O21i | 129.57 (7) |
O1W—Pr—O22 | 66.43 (7) | O32i—Pr—O21i | 64.32 (6) |
O31i—Pr—O22 | 164.93 (7) | O21—Pr—O21i | 165.51 (9) |
O31—Pr—O22 | 68.00 (7) | N11—O11—Pr | 97.75 (15) |
O11i—Pr—O22 | 65.26 (7) | O12—N11—O11 | 122.09 (15) |
O11—Pr—O22 | 66.66 (7) | O12—N11—O11i | 122.09 (15) |
O1Wi—Pr—O22i | 66.43 (7) | O11—N11—O11i | 115.8 (3) |
O1W—Pr—O22i | 113.49 (7) | N21—O21—Pr | 96.21 (15) |
O31i—Pr—O22i | 68.00 (7) | N21—O22—Pr | 98.57 (15) |
O31—Pr—O22i | 164.93 (7) | O23—N21—O21 | 121.7 (3) |
O11i—Pr—O22i | 66.66 (7) | O23—N21—O22 | 120.2 (3) |
O11—Pr—O22i | 65.26 (7) | O21—N21—O22 | 118.2 (2) |
O22—Pr—O22i | 126.89 (10) | N31—O31—Pr | 100.33 (16) |
O1Wi—Pr—O32 | 66.64 (6) | N31—O32—Pr | 94.84 (14) |
O1W—Pr—O32 | 113.49 (6) | O33—N31—O32 | 122.9 (3) |
O31i—Pr—O32 | 66.51 (7) | O33—N31—O31 | 120.6 (3) |
O31—Pr—O32 | 48.00 (6) | O32—N31—O31 | 116.5 (2) |
O11i—Pr—O32 | 163.70 (7) | N1B—C1—N1A | 119.8 (3) |
O11—Pr—O32 | 120.79 (6) | N1B—C1—N1C | 120.2 (3) |
O22—Pr—O32 | 99.85 (6) | N1A—C1—N1C | 119.9 (3) |
O22i—Pr—O32 | 123.44 (7) | C1—N1A—H1A1 | 120.0 |
O1Wi—Pr—O32i | 113.49 (6) | C1—N1A—H1A2 | 120.0 |
O1W—Pr—O32i | 66.64 (6) | H1A1—N1A—H1A2 | 120.0 |
O31i—Pr—O32i | 48.00 (6) | C1—N1B—H1B1 | 120.0 |
O31—Pr—O32i | 66.51 (7) | C1—N1B—H1B2 | 120.0 |
O11i—Pr—O32i | 120.79 (6) | H1B1—N1B—H1B2 | 120.0 |
O11—Pr—O32i | 163.70 (7) | C1—N1C—H1C1 | 120.0 |
O22—Pr—O32i | 123.44 (7) | C1—N1C—H1C2 | 120.0 |
O22i—Pr—O32i | 99.85 (6) | H1C1—N1C—H1C2 | 120.0 |
O32—Pr—O32i | 72.27 (9) | Pr—O1W—H1W | 130.8 |
O1Wi—Pr—O21 | 71.58 (8) | Pr—O1W—H2W | 128.2 |
O1W—Pr—O21 | 108.40 (8) | H1W—O1W—H2W | 96.9 |
O31i—Pr—O21 | 125.29 (7) | | |
| | | |
O1Wi—Pr—O11—N11 | 153.12 (14) | O21—Pr—O22—N21 | −2.05 (15) |
O1W—Pr—O11—N11 | −26.85 (14) | O21i—Pr—O22—N21 | −166.74 (15) |
O31i—Pr—O11—N11 | 113.98 (12) | Pr—O21—N21—O23 | 176.5 (3) |
O31—Pr—O11—N11 | −105.86 (12) | Pr—O21—N21—O22 | −3.6 (3) |
O11i—Pr—O11—N11 | 0.0 | Pr—O22—N21—O23 | −176.4 (3) |
O22—Pr—O11—N11 | −76.86 (12) | Pr—O22—N21—O21 | 3.7 (3) |
O22i—Pr—O11—N11 | 79.88 (12) | O1Wi—Pr—O31—N31 | −16.84 (18) |
O32—Pr—O11—N11 | −164.55 (10) | O1W—Pr—O31—N31 | 163.27 (18) |
O32i—Pr—O11—N11 | 54.6 (3) | O31i—Pr—O31—N31 | 52.46 (15) |
O21—Pr—O11—N11 | −128.24 (14) | O11i—Pr—O31—N31 | −157.65 (15) |
O21i—Pr—O11—N11 | 47.02 (13) | O11—Pr—O31—N31 | −95.65 (17) |
Pr—O11—N11—O12 | 180.0 | O22—Pr—O31—N31 | −124.34 (17) |
Pr—O11—N11—O11i | 0.0 | O22i—Pr—O31—N31 | 63.9 (3) |
O1Wi—Pr—O21—N21 | 154.52 (18) | O32—Pr—O31—N31 | 3.39 (15) |
O1W—Pr—O21—N21 | −25.33 (18) | O32i—Pr—O31—N31 | 90.22 (17) |
O31i—Pr—O21—N21 | −161.25 (15) | O21—Pr—O31—N31 | −73.09 (16) |
O31—Pr—O21—N21 | −79.85 (18) | O21i—Pr—O31—N31 | 117.78 (17) |
O11i—Pr—O21—N21 | 44.48 (18) | O1Wi—Pr—O32—N31 | 156.13 (18) |
O11—Pr—O21—N21 | 81.21 (17) | O1W—Pr—O32—N31 | −23.79 (18) |
O22—Pr—O21—N21 | 2.05 (15) | O31i—Pr—O32—N31 | −128.61 (17) |
O22i—Pr—O21—N21 | 112.61 (18) | O31—Pr—O32—N31 | −3.42 (15) |
O32—Pr—O21—N21 | −133.16 (19) | O11i—Pr—O32—N31 | 67.8 (3) |
O32i—Pr—O21—N21 | −99.83 (17) | O11—Pr—O32—N31 | 113.29 (16) |
O21i—Pr—O21—N21 | 62.17 (17) | O22—Pr—O32—N31 | 44.68 (16) |
O1Wi—Pr—O22—N21 | −30.62 (18) | O22i—Pr—O32—N31 | −167.67 (15) |
O1W—Pr—O22—N21 | 149.53 (18) | O32i—Pr—O32—N31 | −77.44 (16) |
O31i—Pr—O22—N21 | 62.4 (3) | O21—Pr—O32—N31 | 76.17 (16) |
O31—Pr—O22—N21 | 74.71 (17) | O21i—Pr—O32—N31 | −108.75 (16) |
O11i—Pr—O22—N21 | −134.94 (18) | Pr—O32—N31—O33 | −173.5 (3) |
O11—Pr—O22—N21 | −81.32 (16) | Pr—O32—N31—O31 | 5.7 (2) |
O22i—Pr—O22—N21 | −107.98 (17) | Pr—O31—N31—O33 | 173.1 (3) |
O32—Pr—O22—N21 | 38.08 (17) | Pr—O31—N31—O32 | −6.1 (3) |
O32i—Pr—O22—N21 | 113.27 (16) | | |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1A—H1A1···O21ii | 0.86 | 2.22 | 3.038 (4) | 159 |
N1A—H1A2···O22iii | 0.86 | 2.18 | 3.001 (4) | 160 |
N1A—H1A2···O23iii | 0.86 | 2.63 | 3.351 (4) | 142 |
N1B—H1B1···O23ii | 0.86 | 2.07 | 2.921 (4) | 169 |
N1B—H1B2···O31 | 0.86 | 2.03 | 2.870 (4) | 166 |
N1C—H1C2···O23iii | 0.86 | 2.27 | 3.071 (5) | 156 |
O1W—H1W···O32iv | 0.94 | 1.99 | 2.925 (3) | 172 |
O1W—H2W···O11v | 0.89 | 2.05 | 2.935 (3) | 178 |
Symmetry codes: (ii) −x+1, −y+2, −z+1; (iii) −x+1/2, −y+3/2, −z+1; (iv) x−1/2, y−1/2, z; (v) x−1/2, y+1/2, z. |
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