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The Pr atom in the title complex, [Pr(NO3)3(C10H8N8)(H2O)2]·1.5C10H8N2, is ten-coordinate and the relative arrangement of the ligands in the first coordination sphere is affected by the hydrogen bonds between the coordinated water mol­ecules and the uncoordinated 2,2′-bipyridyl (bipy) solvent molecules, one of which lies on a cystallographic inversion centre.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804021920/dn6155sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804021920/dn6155Isup2.hkl
Contains datablock I

CCDC reference: 252767

Key indicators

  • Single-crystal X-ray study
  • T = 130 K
  • R factor = 0.038
  • wR factor = 0.084
  • Data-to-parameter ratio = 15.6

checkCIF/PLATON results

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Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O31 .. 6.13 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O41 .. 5.38 su
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: KappaCCD Software (Nonius, 1997); cell refinement: HKL (Otwinowski & Minor, 1997); data reduction: HKL; program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997) CAMERON (Watkin et al., 1993); software used to prepare material for publication: SHELXTL (Sheldrick, 1997).

(2,2'-bipyridyl)-diaqua-tris(nitrato-O,O')-praseodymium(III) bipyridyl 1.5 solvate top
Crystal data top
C10H12N5O11Pr·1.5(C10H8N2)Z = 2
Mr = 753.43F(000) = 754
Triclinic, P1Dx = 1.721 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.4160 (5) ÅCell parameters from 13117 reflections
b = 11.4284 (6) Åθ = 2–27.5°
c = 14.0585 (10) ŵ = 1.75 mm1
α = 75.322 (4)°T = 130 K
β = 81.118 (4)°Prism, green
γ = 64.060 (4)°0.27 × 0.27 × 0.18 mm
V = 1453.96 (15) Å3
Data collection top
Nonius KappaCCD
diffractometer
6527 independent reflections
Radiation source: fine-focus sealed tube6042 reflections with I > 2s˘I)
Graphite monochromatorRint = 0.045
φω–scans to cover a hemisphere of the reciprocal spaceθmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan
'MULABS (Blessing, 1995)'
h = 1313
Tmin = 0.659, Tmax = 0.732k = 1314
13117 measured reflectionsl = 1618
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)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.P)2 + 3.9292P]
where P = (Fo2 + 2Fc2)/3
6527 reflections(Δ/σ)max = 0.003
418 parametersΔρmax = 1.14 e Å3
6 restraintsΔρmin = 1.89 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 on F2 for ALL reflections except for 18 flagged for potential systematic errors

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pr0.817210 (18)0.458632 (16)0.214690 (13)0.01378 (6)
N10.6049 (3)0.4018 (3)0.3146 (2)0.0195 (6)
N20.8210 (3)0.3824 (3)0.4110 (2)0.0182 (6)
N30.6632 (3)0.5196 (3)0.0328 (2)0.0208 (6)
N41.1355 (3)0.3138 (3)0.1794 (2)0.0211 (6)
N50.7219 (4)0.6940 (3)0.3082 (2)0.0240 (7)
N60.7965 (3)0.8730 (3)0.1050 (2)0.0201 (6)
N71.0361 (3)1.0065 (3)0.1467 (2)0.0212 (6)
N80.8767 (4)0.0318 (3)0.4093 (3)0.0256 (7)
O1W0.8895 (3)0.6168 (2)0.0898 (2)0.0222 (5)
H110.900 (5)0.613 (4)0.0298 (17)0.033*
H120.875 (5)0.694 (3)0.095 (3)0.033*
O2W0.8921 (3)0.2167 (2)0.2444 (2)0.0209 (5)
H210.885 (5)0.167 (4)0.2999 (18)0.031*
H220.929 (5)0.172 (4)0.201 (2)0.031*
O310.6090 (3)0.5928 (2)0.0957 (2)0.0251 (6)
O320.7726 (3)0.4127 (2)0.0578 (2)0.0264 (6)
O330.6140 (4)0.5494 (3)0.0477 (2)0.0382 (7)
O411.0510 (3)0.3368 (2)0.1136 (2)0.0220 (5)
O421.0794 (3)0.3644 (3)0.2545 (2)0.0237 (5)
O431.2629 (3)0.2427 (3)0.1735 (3)0.0400 (8)
O510.6324 (3)0.6621 (2)0.2806 (2)0.0254 (6)
O520.8531 (3)0.6246 (3)0.2910 (2)0.0247 (5)
O530.6819 (4)0.7871 (3)0.3497 (3)0.0414 (8)
C10.4990 (4)0.4112 (4)0.2650 (3)0.0272 (8)
H10.50330.43740.19670.033*
C20.3836 (4)0.3840 (4)0.3097 (4)0.0311 (9)
H20.31250.39210.27260.037*
C30.3780 (4)0.3445 (4)0.4108 (3)0.0308 (9)
H30.30200.32600.44330.037*
C40.4864 (4)0.3327 (4)0.4638 (3)0.0255 (8)
H40.48450.30540.53200.031*
C50.5985 (4)0.3624 (3)0.4134 (3)0.0192 (7)
C60.7183 (4)0.3506 (3)0.4664 (3)0.0177 (7)
C70.7250 (4)0.3082 (4)0.5689 (3)0.0267 (8)
H70.65380.28610.60620.032*
C80.8386 (5)0.2994 (4)0.6142 (3)0.0309 (9)
H80.84490.27090.68210.037*
C90.9426 (4)0.3334 (4)0.5575 (3)0.0273 (8)
H91.01970.32870.58640.033*
C100.9297 (4)0.3744 (4)0.4574 (3)0.0222 (7)
H100.99960.39790.41960.027*
C110.6563 (4)0.9083 (4)0.0995 (3)0.0234 (7)
H11A0.62780.84540.09060.028*
C120.5521 (4)1.0336 (4)0.1065 (3)0.0253 (8)
H12A0.45581.05390.10370.030*
C130.5948 (4)1.1277 (4)0.1177 (3)0.0263 (8)
H130.52751.21280.12250.032*
C140.7396 (4)1.0937 (3)0.1216 (3)0.0239 (8)
H140.77031.15660.12750.029*
C150.8388 (4)0.9642 (3)0.1167 (3)0.0181 (7)
C160.9951 (4)0.9215 (3)0.1225 (3)0.0178 (6)
C171.0954 (4)0.7983 (3)0.1036 (3)0.0215 (7)
H171.06580.74110.08590.026*
C181.2395 (4)0.7626 (4)0.1115 (3)0.0252 (8)
H181.30740.68100.09960.030*
C191.2813 (4)0.8493 (4)0.1371 (3)0.0257 (8)
H191.37720.82700.14360.031*
C201.1761 (4)0.9703 (4)0.1528 (3)0.0249 (8)
H201.20411.02980.16850.030*
C210.7612 (4)0.0135 (4)0.4011 (3)0.0285 (8)
H21A0.72430.03870.33930.034*
C220.6933 (4)0.0414 (4)0.4805 (3)0.0283 (8)
H22A0.61530.05590.47160.034*
C230.7442 (4)0.0737 (4)0.5727 (3)0.0312 (9)
H230.69800.10620.62780.037*
C240.8666 (4)0.0569 (4)0.5820 (3)0.0263 (8)
H240.90320.07860.64350.032*
C250.9329 (4)0.0074 (3)0.4983 (3)0.0210 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pr0.01442 (10)0.01375 (10)0.01467 (10)0.00648 (7)0.00097 (6)0.00419 (7)
N10.0205 (14)0.0205 (14)0.0213 (15)0.0106 (12)0.0002 (11)0.0079 (12)
N20.0201 (14)0.0190 (13)0.0161 (14)0.0073 (12)0.0009 (11)0.0063 (11)
N30.0267 (15)0.0166 (13)0.0202 (15)0.0085 (12)0.0086 (12)0.0022 (11)
N40.0186 (14)0.0206 (14)0.0274 (17)0.0106 (12)0.0023 (12)0.0081 (12)
N50.0367 (17)0.0224 (15)0.0193 (16)0.0174 (14)0.0042 (13)0.0085 (12)
N60.0179 (13)0.0168 (13)0.0258 (16)0.0073 (11)0.0027 (12)0.0039 (12)
N70.0203 (14)0.0182 (14)0.0280 (17)0.0090 (12)0.0008 (12)0.0076 (12)
N80.0305 (16)0.0258 (15)0.0242 (17)0.0150 (14)0.0015 (13)0.0052 (13)
O1W0.0314 (13)0.0174 (11)0.0202 (13)0.0134 (11)0.0034 (11)0.0048 (10)
O2W0.0292 (13)0.0141 (11)0.0182 (13)0.0081 (10)0.0001 (10)0.0038 (9)
O310.0205 (12)0.0232 (12)0.0300 (15)0.0043 (10)0.0033 (11)0.0109 (11)
O320.0293 (14)0.0195 (12)0.0265 (15)0.0004 (11)0.0124 (11)0.0098 (11)
O330.0555 (19)0.0293 (14)0.0286 (16)0.0119 (14)0.0258 (15)0.0007 (12)
O410.0218 (12)0.0261 (12)0.0205 (13)0.0111 (10)0.0000 (10)0.0073 (10)
O420.0180 (12)0.0279 (13)0.0263 (14)0.0080 (10)0.0001 (10)0.0112 (11)
O430.0138 (12)0.0480 (18)0.059 (2)0.0055 (13)0.0030 (13)0.0296 (17)
O510.0255 (13)0.0234 (12)0.0317 (15)0.0112 (11)0.0021 (11)0.0135 (11)
O520.0273 (13)0.0249 (13)0.0278 (15)0.0144 (11)0.0006 (11)0.0094 (11)
O530.063 (2)0.0366 (16)0.0383 (18)0.0298 (16)0.0154 (16)0.0252 (14)
C10.0250 (18)0.036 (2)0.028 (2)0.0168 (16)0.0035 (15)0.0093 (16)
C20.0269 (19)0.032 (2)0.044 (3)0.0183 (17)0.0043 (17)0.0123 (18)
C30.0253 (18)0.033 (2)0.042 (2)0.0193 (17)0.0070 (17)0.0122 (18)
C40.0271 (18)0.0269 (18)0.0240 (19)0.0140 (16)0.0042 (15)0.0059 (15)
C50.0208 (16)0.0140 (15)0.0234 (18)0.0077 (13)0.0028 (13)0.0067 (13)
C60.0205 (16)0.0129 (14)0.0195 (17)0.0061 (13)0.0009 (13)0.0060 (12)
C70.035 (2)0.0280 (18)0.0195 (19)0.0172 (17)0.0018 (15)0.0033 (15)
C80.042 (2)0.033 (2)0.0156 (18)0.0139 (18)0.0047 (16)0.0021 (15)
C90.031 (2)0.0271 (18)0.025 (2)0.0094 (16)0.0103 (16)0.0075 (15)
C100.0214 (17)0.0244 (17)0.0238 (19)0.0106 (14)0.0024 (14)0.0071 (14)
C110.0211 (17)0.0205 (16)0.031 (2)0.0108 (14)0.0019 (14)0.0048 (15)
C120.0153 (16)0.0262 (18)0.033 (2)0.0069 (14)0.0011 (14)0.0077 (16)
C130.0189 (17)0.0197 (17)0.036 (2)0.0012 (14)0.0042 (15)0.0093 (16)
C140.0224 (17)0.0160 (16)0.034 (2)0.0057 (14)0.0050 (15)0.0080 (15)
C150.0184 (16)0.0161 (15)0.0196 (17)0.0066 (13)0.0015 (13)0.0043 (13)
C160.0203 (16)0.0158 (15)0.0172 (16)0.0067 (13)0.0023 (13)0.0040 (12)
C170.0209 (16)0.0185 (16)0.0265 (19)0.0080 (14)0.0007 (14)0.0076 (14)
C180.0199 (17)0.0209 (17)0.031 (2)0.0031 (14)0.0005 (15)0.0086 (15)
C190.0173 (16)0.0293 (19)0.031 (2)0.0096 (15)0.0006 (14)0.0076 (16)
C200.0213 (17)0.0279 (18)0.032 (2)0.0137 (15)0.0000 (15)0.0120 (16)
C210.032 (2)0.0289 (19)0.028 (2)0.0144 (17)0.0042 (16)0.0064 (16)
C220.0242 (18)0.0260 (18)0.037 (2)0.0113 (16)0.0014 (16)0.0083 (17)
C230.030 (2)0.031 (2)0.033 (2)0.0166 (17)0.0035 (17)0.0036 (17)
C240.0291 (19)0.0289 (19)0.0219 (19)0.0146 (16)0.0015 (15)0.0021 (15)
C250.0234 (17)0.0134 (15)0.0261 (19)0.0069 (14)0.0008 (14)0.0051 (13)
Geometric parameters (Å, º) top
Pr—O2W2.461 (2)C3—C41.387 (6)
Pr—O1W2.468 (2)C3—H30.9300
Pr—O322.544 (3)C4—C51.397 (5)
Pr—O422.554 (2)C4—H40.9300
Pr—O512.568 (2)C5—C61.489 (5)
Pr—O522.582 (3)C6—C71.402 (5)
Pr—O312.601 (3)C7—C81.383 (6)
Pr—O412.618 (2)C7—H70.9300
Pr—N12.668 (3)C8—C91.380 (6)
Pr—N22.676 (3)C8—H80.9300
Pr—N32.997 (3)C9—C101.373 (6)
Pr—N43.014 (3)C9—H90.9300
Pr—N53.000 (3)C10—H100.9300
N1—C11.346 (5)C11—C121.385 (5)
N1—C51.347 (5)C11—H11A0.9300
N2—C101.351 (5)C12—C131.380 (5)
N2—C61.351 (4)C12—H12A0.9300
N3—O331.220 (4)C13—C141.390 (5)
N3—O321.266 (4)C13—H130.9300
N3—O311.268 (4)C14—C151.398 (5)
N4—O431.218 (4)C14—H140.9300
N4—O421.271 (4)C15—C161.490 (5)
N4—O411.274 (4)C16—C171.401 (5)
N5—O531.224 (4)C17—C181.387 (5)
N5—O521.266 (4)C17—H170.9300
N5—O511.278 (4)C18—C191.380 (6)
N6—C111.344 (5)C18—H180.9300
N6—C151.349 (4)C19—C201.384 (5)
N7—C201.340 (5)C19—H190.9300
N7—C161.348 (4)C20—H200.9300
N8—C211.334 (5)C21—C221.388 (6)
N8—C251.350 (5)C21—H21A0.9300
O1W—H110.85 (2)C22—C231.376 (6)
O1W—H120.85 (4)C22—H22A0.9300
O2W—H210.86 (2)C23—C241.399 (6)
O2W—H220.83 (4)C23—H230.9300
C1—C21.390 (5)C24—C251.391 (5)
C1—H10.9300C24—H240.9300
C2—C31.379 (7)C25—C25i1.488 (7)
C2—H20.9300
O2W—Pr—O1W133.48 (8)C11—N6—C15118.7 (3)
O2W—Pr—O3273.82 (9)C20—N7—C16118.4 (3)
O1W—Pr—O3279.68 (9)C21—N8—C25118.8 (3)
O2W—Pr—O4277.04 (8)Pr—O1W—H11120 (3)
O1W—Pr—O4280.96 (9)Pr—O1W—H12126 (3)
O32—Pr—O42115.42 (8)H11—O1W—H12110 (3)
O2W—Pr—O51139.96 (9)Pr—O2W—H21126 (3)
O1W—Pr—O5186.45 (9)Pr—O2W—H22124 (3)
O32—Pr—O51119.66 (8)H21—O2W—H22110 (3)
O42—Pr—O51119.77 (8)N3—O31—Pr95.32 (18)
O2W—Pr—O52137.80 (9)N3—O32—Pr98.10 (19)
O1W—Pr—O5267.69 (9)N4—O41—Pr95.23 (19)
O32—Pr—O52145.53 (9)N4—O42—Pr98.4 (2)
O42—Pr—O5271.15 (8)N5—O51—Pr96.77 (19)
O51—Pr—O5249.80 (8)N5—O52—Pr96.43 (19)
O2W—Pr—O31112.91 (9)N1—C1—C2123.8 (4)
O1W—Pr—O3173.63 (9)N1—C1—H1118.1
O32—Pr—O3149.45 (8)C2—C1—H1118.1
O42—Pr—O31152.21 (9)C3—C2—C1117.9 (4)
O51—Pr—O3170.26 (8)C3—C2—H2121.0
O52—Pr—O31108.13 (8)C1—C2—H2121.0
O2W—Pr—O4166.49 (8)C2—C3—C4119.5 (4)
O1W—Pr—O4168.00 (8)C2—C3—H3120.3
O32—Pr—O4166.12 (8)C4—C3—H3120.3
O42—Pr—O4149.48 (8)C3—C4—C5119.1 (4)
O51—Pr—O41152.89 (8)C3—C4—H4120.4
O52—Pr—O41109.01 (8)C5—C4—H4120.4
O31—Pr—O41108.87 (8)N1—C5—C4122.0 (3)
O2W—Pr—N171.51 (9)N1—C5—C6116.6 (3)
O1W—Pr—N1147.80 (9)C4—C5—C6121.4 (3)
O32—Pr—N192.22 (9)N2—C6—C7121.2 (3)
O42—Pr—N1129.77 (9)N2—C6—C5116.9 (3)
O51—Pr—N170.50 (9)C7—C6—C5121.9 (3)
O52—Pr—N1109.31 (9)C8—C7—C6119.4 (4)
O31—Pr—N177.47 (9)C8—C7—H7120.3
O41—Pr—N1136.53 (8)C6—C7—H7120.3
O2W—Pr—N276.33 (9)C9—C8—C7119.3 (4)
O1W—Pr—N2135.15 (9)C9—C8—H8120.3
O32—Pr—N2144.92 (9)C7—C8—H8120.3
O42—Pr—N274.52 (9)C10—C9—C8118.5 (4)
O51—Pr—N274.53 (9)C10—C9—H9120.7
O52—Pr—N269.05 (9)C8—C9—H9120.7
O31—Pr—N2132.22 (9)N2—C10—C9123.6 (4)
O41—Pr—N2117.12 (8)N2—C10—H10118.2
N1—Pr—N260.75 (9)C9—C10—H10118.2
O2W—Pr—N394.79 (8)N6—C11—C12123.3 (3)
O1W—Pr—N373.04 (9)N6—C11—H11A118.4
O32—Pr—N324.73 (8)C12—C11—H11A118.4
O42—Pr—N3134.82 (9)C13—C12—C11118.3 (3)
O51—Pr—N395.14 (9)C13—C12—H12A120.9
O52—Pr—N3127.33 (8)C11—C12—H12A120.9
O31—Pr—N324.92 (8)C12—C13—C14119.2 (3)
O41—Pr—N386.23 (8)C12—C13—H13120.4
N1—Pr—N386.58 (9)C14—C13—H13120.4
N2—Pr—N3147.33 (9)C13—C14—C15119.5 (3)
O2W—Pr—N5145.52 (9)C13—C14—H14120.2
O1W—Pr—N576.44 (9)C15—C14—H14120.2
O32—Pr—N5137.22 (8)N6—C15—C14121.0 (3)
O42—Pr—N595.25 (9)N6—C15—C16117.2 (3)
O51—Pr—N525.02 (9)C14—C15—C16121.8 (3)
O52—Pr—N524.80 (9)N7—C16—C17121.3 (3)
O31—Pr—N589.64 (9)N7—C16—C15117.2 (3)
O41—Pr—N5132.25 (8)C17—C16—C15121.5 (3)
N1—Pr—N589.61 (9)C18—C17—C16119.1 (3)
N2—Pr—N569.24 (9)C18—C17—H17120.5
N3—Pr—N5113.09 (9)C16—C17—H17120.5
C1—N1—C5117.7 (3)C19—C18—C17119.6 (3)
C1—N1—Pr119.2 (3)C19—C18—H18120.2
C5—N1—Pr123.2 (2)C17—C18—H18120.2
C10—N2—C6118.0 (3)C18—C19—C20118.0 (3)
C10—N2—Pr119.4 (2)C18—C19—H19121.0
C6—N2—Pr122.6 (2)C20—C19—H19121.0
O33—N3—O32121.2 (3)N7—C20—C19123.6 (3)
O33—N3—O31122.6 (3)N7—C20—H20118.2
O32—N3—O31116.2 (3)C19—C20—H20118.2
O33—N3—Pr171.7 (3)N8—C21—C22123.1 (4)
O32—N3—Pr57.17 (16)N8—C21—H21A118.4
O31—N3—Pr59.77 (17)C22—C21—H21A118.4
O43—N4—O42120.9 (3)C23—C22—C21118.5 (4)
O43—N4—O41122.5 (3)C23—C22—H22A120.7
O42—N4—O41116.6 (3)C21—C22—H22A120.7
O43—N4—Pr172.2 (3)C22—C23—C24118.8 (4)
O42—N4—Pr56.97 (16)C22—C23—H23120.6
O41—N4—Pr59.87 (16)C24—C23—H23120.6
O53—N5—O52121.8 (3)C25—C24—C23119.3 (4)
O53—N5—O51121.3 (3)C25—C24—H24120.3
O52—N5—O51116.9 (3)C23—C24—H24120.3
O53—N5—Pr177.5 (3)N8—C25—C24121.1 (3)
O52—N5—Pr58.77 (16)N8—C25—C25i116.4 (4)
O51—N5—Pr58.22 (16)C24—C25—C25i122.4 (4)
Symmetry code: (i) x+2, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H11···O41ii0.85 (2)2.00 (3)2.797 (4)156 (4)
O1W—H12···N60.85 (4)1.88 (2)2.707 (4)166 (5)
O2W—H21···N80.86 (2)1.90 (2)2.751 (4)170 (4)
O2W—H22···N7iii0.84 (3)2.01 (3)2.791 (4)157 (4)
Symmetry codes: (ii) x+2, y+1, z; (iii) x, y1, z.
 

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