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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806038980/ng2104sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806038980/ng2104Isup2.hkl
Contains datablock I

CCDC reference: 628009

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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 = 607.17Dx = 1.984 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 8002 reflections
a = 10.931 (3) Åθ = 3–25.9°
b = 9.071 (3) ŵ = 2.50 mm1
c = 20.571 (5) ÅT = 293 K
β = 94.78 (3)°Block, green
V = 2032.6 (10) Å30.56 × 0.41 × 0.41 mm
Z = 4
Data collection top
Stoe IPDS area-detector
diffractometer
1956 independent reflections
Radiation source: medium-focus sealed tube1822 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
φ scansθmax = 26.0°, θmin = 2.9°
Absorption correction: numerical
(Stoe & Cie, 1998)
h = 1313
Tmin = 0.210, Tmax = 0.253k = 1111
14022 measured reflectionsl = 2525
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)] = 0.020Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.052H-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 parametersΔρmax = 0.43 e Å3
0 restraintsΔρmin = 0.79 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
Pr0.50000.861324 (18)0.75000.02072 (8)
O110.59530 (16)0.5976 (2)0.73946 (11)0.0364 (4)
O120.50000.3910 (3)0.75000.0838 (17)
N110.50000.5229 (3)0.75000.0362 (8)
O210.6132 (2)0.8233 (2)0.63757 (11)0.0430 (5)
O220.43183 (19)0.7291 (2)0.63608 (10)0.0404 (5)
O230.5299 (3)0.7213 (3)0.54893 (11)0.0648 (8)
N210.5256 (2)0.7578 (3)0.60669 (12)0.0375 (6)
O310.43540 (18)1.0491 (2)0.65959 (10)0.0390 (5)
O320.61354 (18)1.1021 (2)0.70610 (10)0.0363 (4)
O330.5420 (3)1.2247 (3)0.62082 (13)0.0657 (8)
N310.5318 (2)1.1291 (2)0.66136 (13)0.0353 (6)
C10.2403 (3)0.9993 (4)0.50270 (16)0.0457 (7)
N1A0.2079 (3)1.0080 (3)0.43994 (14)0.0602 (8)
H1A10.24211.07180.41640.072*
H1A20.15240.94980.42240.072*
N1B0.3246 (3)1.0880 (4)0.52926 (15)0.0633 (9)
H1B10.35871.15170.50560.076*
H1B20.34601.08260.57040.076*
N1C0.1876 (3)0.9011 (4)0.53889 (19)0.0674 (9)
H1C10.20870.89550.58000.081*
H1C20.13220.84300.52130.081*
O1W0.27266 (18)0.86096 (18)0.72199 (12)0.0380 (5)
H1W0.21600.78300.71860.046*
H2W0.21900.93230.72840.046*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pr0.01844 (11)0.01878 (11)0.02496 (12)0.0000.00193 (8)0.000
O110.0224 (9)0.0281 (9)0.0604 (13)0.0030 (7)0.0134 (9)0.0000 (9)
O120.064 (2)0.0180 (15)0.178 (5)0.0000.060 (3)0.000
N110.0278 (16)0.0236 (15)0.059 (2)0.0000.0139 (16)0.000
O210.0411 (12)0.0445 (11)0.0442 (12)0.0148 (9)0.0084 (10)0.0096 (9)
O220.0376 (11)0.0465 (12)0.0385 (11)0.0123 (9)0.0114 (9)0.0080 (9)
O230.0756 (18)0.0846 (19)0.0370 (13)0.0320 (15)0.0219 (13)0.0234 (12)
N210.0475 (14)0.0352 (12)0.0309 (12)0.0086 (10)0.0103 (11)0.0076 (9)
O310.0355 (10)0.0407 (11)0.0393 (11)0.0120 (8)0.0067 (9)0.0100 (8)
O320.0349 (10)0.0296 (9)0.0424 (12)0.0044 (8)0.0089 (9)0.0019 (8)
O330.0751 (18)0.0611 (16)0.0580 (16)0.0293 (13)0.0107 (14)0.0334 (13)
N310.0424 (14)0.0295 (12)0.0333 (13)0.0092 (9)0.0013 (12)0.0082 (9)
C10.0445 (18)0.0461 (16)0.0460 (18)0.0096 (13)0.0007 (15)0.0093 (13)
N1A0.066 (2)0.067 (2)0.0457 (16)0.0356 (16)0.0073 (15)0.0037 (14)
N1B0.0623 (19)0.084 (2)0.0412 (16)0.0335 (19)0.0104 (15)0.0123 (16)
N1C0.077 (2)0.0593 (18)0.067 (2)0.0203 (18)0.0092 (18)0.0214 (17)
O1W0.0197 (9)0.0278 (10)0.0665 (15)0.0001 (7)0.0036 (10)0.0081 (8)
Geometric parameters (Å, º) top
Pr—O1Wi2.504 (2)O22—N211.260 (3)
Pr—O1W2.504 (2)O23—N211.238 (3)
Pr—O31i2.577 (2)O31—N311.277 (3)
Pr—O312.577 (2)O32—N311.253 (3)
Pr—O11i2.625 (2)O33—N311.214 (3)
Pr—O112.625 (2)C1—N1B1.309 (4)
Pr—O222.682 (2)C1—N1A1.312 (4)
Pr—O22i2.682 (2)C1—N1C1.323 (4)
Pr—O322.704 (2)N1A—H1A10.8600
Pr—O32i2.704 (2)N1A—H1A20.8600
Pr—O212.734 (2)N1B—H1B10.8600
Pr—O21i2.734 (2)N1B—H1B20.8600
O11—N111.277 (2)N1C—H1C10.8600
O12—N111.196 (5)N1C—H1C20.8600
N11—O11i1.277 (2)O1W—H1W0.9390
O21—N211.254 (3)O1W—H2W0.8899
O1Wi—Pr—O1W179.85 (8)O31—Pr—O2165.73 (7)
O1Wi—Pr—O31i68.14 (7)O11i—Pr—O2199.54 (6)
O1W—Pr—O31i111.96 (7)O11—Pr—O2166.71 (7)
O1Wi—Pr—O31111.96 (7)O22—Pr—O2146.92 (6)
O1W—Pr—O3168.14 (7)O22i—Pr—O21124.77 (7)
O31i—Pr—O3197.24 (10)O32—Pr—O2164.32 (6)
O1Wi—Pr—O11i111.90 (6)O32i—Pr—O21129.57 (7)
O1W—Pr—O11i67.96 (6)O1Wi—Pr—O21i108.40 (8)
O31i—Pr—O11i129.01 (7)O1W—Pr—O21i71.58 (8)
O31—Pr—O11i125.11 (7)O31i—Pr—O21i65.73 (7)
O1Wi—Pr—O1167.96 (6)O31—Pr—O21i125.29 (6)
O1W—Pr—O11111.90 (6)O11i—Pr—O21i66.71 (7)
O31i—Pr—O11125.11 (7)O11—Pr—O21i99.54 (6)
O31—Pr—O11129.01 (7)O22—Pr—O21i124.77 (7)
O11i—Pr—O1148.67 (8)O22i—Pr—O21i46.92 (6)
O1Wi—Pr—O22113.49 (7)O32—Pr—O21i129.57 (7)
O1W—Pr—O2266.43 (7)O32i—Pr—O21i64.32 (6)
O31i—Pr—O22164.93 (7)O21—Pr—O21i165.51 (9)
O31—Pr—O2268.00 (7)N11—O11—Pr97.75 (15)
O11i—Pr—O2265.26 (7)O12—N11—O11122.09 (15)
O11—Pr—O2266.66 (7)O12—N11—O11i122.09 (15)
O1Wi—Pr—O22i66.43 (7)O11—N11—O11i115.8 (3)
O1W—Pr—O22i113.49 (7)N21—O21—Pr96.21 (15)
O31i—Pr—O22i68.00 (7)N21—O22—Pr98.57 (15)
O31—Pr—O22i164.93 (7)O23—N21—O21121.7 (3)
O11i—Pr—O22i66.66 (7)O23—N21—O22120.2 (3)
O11—Pr—O22i65.26 (7)O21—N21—O22118.2 (2)
O22—Pr—O22i126.89 (10)N31—O31—Pr100.33 (16)
O1Wi—Pr—O3266.64 (6)N31—O32—Pr94.84 (14)
O1W—Pr—O32113.49 (6)O33—N31—O32122.9 (3)
O31i—Pr—O3266.51 (7)O33—N31—O31120.6 (3)
O31—Pr—O3248.00 (6)O32—N31—O31116.5 (2)
O11i—Pr—O32163.70 (7)N1B—C1—N1A119.8 (3)
O11—Pr—O32120.79 (6)N1B—C1—N1C120.2 (3)
O22—Pr—O3299.85 (6)N1A—C1—N1C119.9 (3)
O22i—Pr—O32123.44 (7)C1—N1A—H1A1120.0
O1Wi—Pr—O32i113.49 (6)C1—N1A—H1A2120.0
O1W—Pr—O32i66.64 (6)H1A1—N1A—H1A2120.0
O31i—Pr—O32i48.00 (6)C1—N1B—H1B1120.0
O31—Pr—O32i66.51 (7)C1—N1B—H1B2120.0
O11i—Pr—O32i120.79 (6)H1B1—N1B—H1B2120.0
O11—Pr—O32i163.70 (7)C1—N1C—H1C1120.0
O22—Pr—O32i123.44 (7)C1—N1C—H1C2120.0
O22i—Pr—O32i99.85 (6)H1C1—N1C—H1C2120.0
O32—Pr—O32i72.27 (9)Pr—O1W—H1W130.8
O1Wi—Pr—O2171.58 (8)Pr—O1W—H2W128.2
O1W—Pr—O21108.40 (8)H1W—O1W—H2W96.9
O31i—Pr—O21125.29 (7)
O1Wi—Pr—O11—N11153.12 (14)O21—Pr—O22—N212.05 (15)
O1W—Pr—O11—N1126.85 (14)O21i—Pr—O22—N21166.74 (15)
O31i—Pr—O11—N11113.98 (12)Pr—O21—N21—O23176.5 (3)
O31—Pr—O11—N11105.86 (12)Pr—O21—N21—O223.6 (3)
O11i—Pr—O11—N110.0Pr—O22—N21—O23176.4 (3)
O22—Pr—O11—N1176.86 (12)Pr—O22—N21—O213.7 (3)
O22i—Pr—O11—N1179.88 (12)O1Wi—Pr—O31—N3116.84 (18)
O32—Pr—O11—N11164.55 (10)O1W—Pr—O31—N31163.27 (18)
O32i—Pr—O11—N1154.6 (3)O31i—Pr—O31—N3152.46 (15)
O21—Pr—O11—N11128.24 (14)O11i—Pr—O31—N31157.65 (15)
O21i—Pr—O11—N1147.02 (13)O11—Pr—O31—N3195.65 (17)
Pr—O11—N11—O12180.0O22—Pr—O31—N31124.34 (17)
Pr—O11—N11—O11i0.0O22i—Pr—O31—N3163.9 (3)
O1Wi—Pr—O21—N21154.52 (18)O32—Pr—O31—N313.39 (15)
O1W—Pr—O21—N2125.33 (18)O32i—Pr—O31—N3190.22 (17)
O31i—Pr—O21—N21161.25 (15)O21—Pr—O31—N3173.09 (16)
O31—Pr—O21—N2179.85 (18)O21i—Pr—O31—N31117.78 (17)
O11i—Pr—O21—N2144.48 (18)O1Wi—Pr—O32—N31156.13 (18)
O11—Pr—O21—N2181.21 (17)O1W—Pr—O32—N3123.79 (18)
O22—Pr—O21—N212.05 (15)O31i—Pr—O32—N31128.61 (17)
O22i—Pr—O21—N21112.61 (18)O31—Pr—O32—N313.42 (15)
O32—Pr—O21—N21133.16 (19)O11i—Pr—O32—N3167.8 (3)
O32i—Pr—O21—N2199.83 (17)O11—Pr—O32—N31113.29 (16)
O21i—Pr—O21—N2162.17 (17)O22—Pr—O32—N3144.68 (16)
O1Wi—Pr—O22—N2130.62 (18)O22i—Pr—O32—N31167.67 (15)
O1W—Pr—O22—N21149.53 (18)O32i—Pr—O32—N3177.44 (16)
O31i—Pr—O22—N2162.4 (3)O21—Pr—O32—N3176.17 (16)
O31—Pr—O22—N2174.71 (17)O21i—Pr—O32—N31108.75 (16)
O11i—Pr—O22—N21134.94 (18)Pr—O32—N31—O33173.5 (3)
O11—Pr—O22—N2181.32 (16)Pr—O32—N31—O315.7 (2)
O22i—Pr—O22—N21107.98 (17)Pr—O31—N31—O33173.1 (3)
O32—Pr—O22—N2138.08 (17)Pr—O31—N31—O326.1 (3)
O32i—Pr—O22—N21113.27 (16)
Symmetry code: (i) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1A—H1A1···O21ii0.862.223.038 (4)159
N1A—H1A2···O22iii0.862.183.001 (4)160
N1A—H1A2···O23iii0.862.633.351 (4)142
N1B—H1B1···O23ii0.862.072.921 (4)169
N1B—H1B2···O310.862.032.870 (4)166
N1C—H1C2···O23iii0.862.273.071 (5)156
O1W—H1W···O32iv0.941.992.925 (3)172
O1W—H2W···O11v0.892.052.935 (3)178
Symmetry codes: (ii) x+1, y+2, z+1; (iii) x+1/2, y+3/2, z+1; (iv) x1/2, y1/2, z; (v) x1/2, y+1/2, z.
 

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