The Pr atom in the title complex, [Pr(NO3)3(C15H11N3)(H2O)]·C3H6O, is ten-coordinated and the arrangement can be described as a distorted bicapped square antiprism.
Supporting information
CCDC reference: 200845
Key indicators
- Single-crystal X-ray study
- T = 130 K
- Mean (C-C) = 0.007 Å
- R factor = 0.045
- wR factor = 0.098
- Data-to-parameter ratio = 15.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.01
PLAT230_ALERT_2_C Hirshfeld Test Diff for O51 - N5 .. 5.24 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr1 - O42 .. 5.81 su
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C21
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 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
0 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
Aquatris(nitrato-
κ2O,
O')(2,2':6,2''-terpyridine)praseodymium(III) acetone solvate
top
Crystal data top
[Pr(NO3)3(C15H11N3)(H2O)]·C3H6O | F(000) = 1264 |
Mr = 636.30 | Dx = 1.838 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 16338 reflections |
a = 9.7282 (6) Å | θ = 2–27.5° |
b = 15.7656 (10) Å | µ = 2.19 mm−1 |
c = 15.1477 (10) Å | T = 130 K |
β = 98.183 (6)° | Plate, green |
V = 2299.6 (3) Å3 | 0.44 × 0.19 × 0.03 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD area-detector diffractometer | 5204 independent reflections |
Radiation source: fine-focus sealed tube | 3727 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.099 |
φ and ω scans | θmax = 27.5°, θmin = 1.9° |
Absorption correction: multi-scan (MULABS; Blessing, 1995) | h = −12→10 |
Tmin = 0.619, Tmax = 0.925 | k = −20→19 |
16338 measured reflections | l = −19→16 |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0334P)2] where P = (Fo2 + 2Fc2)/3 |
5204 reflections | (Δ/σ)max = 0.001 |
335 parameters | Δρmax = 1.12 e Å−3 |
0 restraints | Δρmin = −1.48 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 on F2 for ALL reflections except for 33 flagged for
potential systematic errors |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pr1 | 0.17142 (2) | 0.240499 (15) | 0.357444 (16) | 0.01889 (10) | |
N1 | −0.0367 (4) | 0.3363 (2) | 0.3829 (2) | 0.0205 (9) | |
N2 | −0.0629 (4) | 0.1651 (2) | 0.3810 (2) | 0.0183 (8) | |
N3 | 0.1557 (4) | 0.0760 (2) | 0.3368 (3) | 0.0227 (9) | |
C1 | −0.0201 (5) | 0.4213 (3) | 0.3841 (3) | 0.0222 (10) | |
H1A | 0.0666 | 0.4431 | 0.3775 | 0.027* | |
C2 | −0.1252 (5) | 0.4772 (3) | 0.3945 (3) | 0.0289 (12) | |
H2A | −0.1096 | 0.5354 | 0.3958 | 0.035* | |
C3 | −0.2542 (5) | 0.4446 (3) | 0.4029 (3) | 0.0297 (12) | |
H3A | −0.3276 | 0.4808 | 0.4094 | 0.036* | |
C4 | −0.2737 (5) | 0.3579 (3) | 0.4015 (3) | 0.0261 (11) | |
H4A | −0.3606 | 0.3352 | 0.4063 | 0.031* | |
C5 | −0.1623 (5) | 0.3048 (3) | 0.3929 (3) | 0.0217 (11) | |
C6 | −0.1753 (4) | 0.2105 (3) | 0.3951 (3) | 0.0193 (10) | |
C7 | −0.2996 (5) | 0.1724 (3) | 0.4106 (3) | 0.0279 (12) | |
H7A | −0.3746 | 0.2052 | 0.4220 | 0.034* | |
C8 | −0.3084 (5) | 0.0854 (3) | 0.4084 (3) | 0.0276 (12) | |
H8A | −0.3902 | 0.0588 | 0.4180 | 0.033* | |
C9 | −0.1959 (5) | 0.0375 (3) | 0.3919 (3) | 0.0258 (11) | |
H9A | −0.2018 | −0.0213 | 0.3888 | 0.031* | |
C10 | −0.0733 (5) | 0.0791 (3) | 0.3800 (3) | 0.0205 (10) | |
C11 | 0.0503 (5) | 0.0304 (3) | 0.3624 (3) | 0.0233 (11) | |
C12 | 0.0584 (5) | −0.0571 (3) | 0.3717 (3) | 0.0260 (11) | |
H12A | −0.0154 | −0.0876 | 0.3885 | 0.031* | |
C13 | 0.1782 (5) | −0.0982 (3) | 0.3555 (3) | 0.0316 (12) | |
H13A | 0.1859 | −0.1566 | 0.3630 | 0.038* | |
C14 | 0.2865 (5) | −0.0527 (3) | 0.3282 (3) | 0.0278 (12) | |
H14A | 0.3675 | −0.0792 | 0.3165 | 0.033* | |
C15 | 0.2681 (5) | 0.0341 (3) | 0.3193 (3) | 0.0285 (12) | |
H15A | 0.3390 | 0.0655 | 0.2998 | 0.034* | |
N4 | 0.0804 (4) | 0.2086 (2) | 0.1613 (3) | 0.0248 (9) | |
O41 | −0.0011 (3) | 0.2362 (2) | 0.2134 (2) | 0.0252 (7) | |
O42 | 0.2069 (3) | 0.1987 (2) | 0.1939 (2) | 0.0269 (8) | |
O43 | 0.0383 (3) | 0.1921 (2) | 0.0834 (2) | 0.0312 (8) | |
N5 | 0.3483 (4) | 0.3725 (3) | 0.2886 (3) | 0.0264 (9) | |
O51 | 0.2161 (3) | 0.3773 (2) | 0.2739 (2) | 0.0247 (8) | |
O52 | 0.3984 (3) | 0.3042 (2) | 0.3250 (2) | 0.0283 (8) | |
O53 | 0.4232 (3) | 0.4305 (2) | 0.2701 (2) | 0.0339 (9) | |
N6 | 0.3309 (4) | 0.1492 (2) | 0.5128 (3) | 0.0295 (10) | |
O61 | 0.2005 (3) | 0.1615 (2) | 0.5100 (2) | 0.0255 (8) | |
O62 | 0.3858 (3) | 0.1759 (2) | 0.4464 (2) | 0.0291 (8) | |
O63 | 0.3990 (4) | 0.1142 (2) | 0.5764 (3) | 0.0488 (12) | |
O21 | 0.5084 (4) | 0.3932 (2) | 0.5506 (3) | 0.0397 (10) | |
C21 | 0.5929 (5) | 0.3690 (3) | 0.6123 (4) | 0.0287 (12) | |
C22 | 0.7284 (5) | 0.4129 (4) | 0.6368 (4) | 0.0433 (15) | |
H22A | 0.7355 | 0.4589 | 0.5963 | 0.065* | |
H22B | 0.8028 | 0.3735 | 0.6335 | 0.065* | |
H22C | 0.7345 | 0.4345 | 0.6965 | 0.065* | |
C23 | 0.5648 (8) | 0.2935 (4) | 0.6641 (5) | 0.066 (2) | |
H23A | 0.5503 | 0.2453 | 0.6251 | 0.100* | |
H23B | 0.4832 | 0.3030 | 0.6917 | 0.100* | |
H23C | 0.6426 | 0.2829 | 0.7093 | 0.100* | |
O1W | 0.2506 (4) | 0.3444 (2) | 0.4799 (2) | 0.0255 (8) | |
H1 | 0.207 (6) | 0.330 (4) | 0.533 (4) | 0.06 (2)* | |
H2 | 0.324 (6) | 0.357 (3) | 0.508 (4) | 0.039 (18)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pr1 | 0.01654 (15) | 0.01933 (15) | 0.02062 (15) | −0.00030 (11) | 0.00206 (10) | −0.00003 (11) |
N1 | 0.023 (2) | 0.023 (2) | 0.016 (2) | 0.0014 (16) | 0.0023 (16) | 0.0016 (16) |
N2 | 0.018 (2) | 0.019 (2) | 0.017 (2) | 0.0008 (15) | 0.0013 (15) | −0.0012 (16) |
N3 | 0.024 (2) | 0.018 (2) | 0.027 (2) | −0.0004 (16) | 0.0065 (17) | 0.0019 (16) |
C1 | 0.027 (3) | 0.018 (3) | 0.021 (3) | −0.0039 (19) | 0.004 (2) | 0.001 (2) |
C2 | 0.036 (3) | 0.019 (3) | 0.031 (3) | 0.004 (2) | 0.002 (2) | −0.001 (2) |
C3 | 0.030 (3) | 0.027 (3) | 0.033 (3) | 0.006 (2) | 0.006 (2) | −0.005 (2) |
C4 | 0.019 (3) | 0.026 (3) | 0.033 (3) | 0.000 (2) | 0.001 (2) | −0.003 (2) |
C5 | 0.024 (3) | 0.026 (3) | 0.015 (3) | −0.0010 (19) | 0.001 (2) | 0.0005 (19) |
C6 | 0.021 (3) | 0.018 (2) | 0.018 (3) | −0.0028 (17) | 0.0025 (19) | −0.0025 (18) |
C7 | 0.027 (3) | 0.024 (3) | 0.032 (3) | 0.002 (2) | 0.003 (2) | 0.001 (2) |
C8 | 0.023 (3) | 0.025 (3) | 0.036 (3) | −0.006 (2) | 0.010 (2) | 0.004 (2) |
C9 | 0.030 (3) | 0.021 (3) | 0.027 (3) | −0.003 (2) | 0.003 (2) | 0.000 (2) |
C10 | 0.025 (3) | 0.018 (3) | 0.016 (2) | 0.0004 (19) | −0.0029 (19) | −0.0020 (19) |
C11 | 0.027 (3) | 0.019 (3) | 0.022 (3) | −0.0022 (19) | −0.002 (2) | −0.002 (2) |
C12 | 0.027 (3) | 0.024 (3) | 0.026 (3) | −0.002 (2) | 0.000 (2) | 0.000 (2) |
C13 | 0.035 (3) | 0.020 (3) | 0.038 (3) | 0.004 (2) | −0.004 (2) | −0.002 (2) |
C14 | 0.027 (3) | 0.024 (3) | 0.032 (3) | 0.009 (2) | 0.001 (2) | −0.005 (2) |
C15 | 0.027 (3) | 0.030 (3) | 0.028 (3) | −0.002 (2) | 0.003 (2) | −0.007 (2) |
N4 | 0.032 (3) | 0.018 (2) | 0.025 (2) | −0.0023 (17) | 0.0037 (19) | 0.0014 (18) |
O41 | 0.0244 (19) | 0.0296 (19) | 0.0213 (18) | 0.0014 (14) | 0.0028 (14) | −0.0045 (14) |
O42 | 0.0211 (19) | 0.0254 (19) | 0.034 (2) | 0.0037 (14) | 0.0048 (15) | −0.0006 (15) |
O43 | 0.037 (2) | 0.037 (2) | 0.019 (2) | −0.0061 (16) | 0.0016 (15) | −0.0028 (16) |
N5 | 0.033 (3) | 0.029 (2) | 0.018 (2) | −0.0005 (19) | 0.0048 (18) | 0.0021 (18) |
O51 | 0.0173 (19) | 0.0269 (19) | 0.030 (2) | 0.0014 (13) | 0.0046 (14) | 0.0057 (15) |
O52 | 0.0221 (19) | 0.027 (2) | 0.037 (2) | 0.0014 (14) | 0.0085 (15) | 0.0046 (16) |
O53 | 0.031 (2) | 0.033 (2) | 0.038 (2) | −0.0130 (16) | 0.0094 (16) | 0.0077 (17) |
N6 | 0.026 (3) | 0.019 (2) | 0.040 (3) | −0.0046 (17) | −0.006 (2) | 0.0017 (19) |
O61 | 0.023 (2) | 0.0257 (19) | 0.028 (2) | −0.0021 (14) | 0.0017 (14) | 0.0042 (14) |
O62 | 0.025 (2) | 0.031 (2) | 0.031 (2) | 0.0013 (15) | 0.0029 (16) | 0.0053 (16) |
O63 | 0.035 (2) | 0.046 (3) | 0.058 (3) | −0.0081 (18) | −0.0193 (19) | 0.031 (2) |
O21 | 0.029 (2) | 0.042 (2) | 0.045 (3) | −0.0068 (17) | −0.0063 (18) | 0.0042 (18) |
C21 | 0.024 (3) | 0.030 (3) | 0.033 (3) | 0.005 (2) | 0.006 (2) | −0.009 (2) |
C22 | 0.029 (3) | 0.053 (4) | 0.045 (4) | −0.004 (3) | −0.003 (3) | −0.007 (3) |
C23 | 0.071 (5) | 0.046 (4) | 0.079 (6) | −0.002 (4) | 0.002 (4) | 0.025 (4) |
O1W | 0.026 (2) | 0.025 (2) | 0.024 (2) | −0.0057 (15) | −0.0017 (17) | −0.0047 (15) |
Geometric parameters (Å, º) top
Pr1—O1W | 2.513 (3) | C9—H9A | 0.93 |
Pr1—O62 | 2.530 (3) | C10—C11 | 1.482 (6) |
Pr1—O52 | 2.537 (3) | C11—C12 | 1.387 (6) |
Pr1—O41 | 2.558 (3) | C12—C13 | 1.386 (6) |
Pr1—O51 | 2.569 (3) | C12—H12A | 0.93 |
Pr1—N1 | 2.598 (4) | C13—C14 | 1.385 (7) |
Pr1—O61 | 2.605 (3) | C13—H13A | 0.93 |
Pr1—N3 | 2.614 (4) | C14—C15 | 1.385 (7) |
Pr1—O42 | 2.632 (3) | C14—H14A | 0.93 |
Pr1—N2 | 2.640 (4) | C15—H15A | 0.93 |
N1—C5 | 1.347 (6) | N4—O43 | 1.220 (5) |
N1—C1 | 1.349 (6) | N4—O42 | 1.269 (5) |
N2—C6 | 1.348 (6) | N4—O41 | 1.272 (5) |
N2—C10 | 1.360 (6) | N5—O53 | 1.225 (5) |
N3—C15 | 1.336 (6) | N5—O52 | 1.276 (5) |
N3—C11 | 1.354 (6) | N5—O51 | 1.276 (5) |
C1—C2 | 1.376 (7) | N6—O63 | 1.221 (5) |
C1—H1A | 0.93 | N6—O62 | 1.275 (5) |
C2—C3 | 1.378 (7) | N6—O61 | 1.278 (5) |
C2—H2A | 0.93 | O21—C21 | 1.215 (6) |
C3—C4 | 1.380 (7) | C21—C23 | 1.472 (8) |
C3—H3A | 0.93 | C21—C22 | 1.488 (7) |
C4—C5 | 1.391 (6) | C22—H22A | 0.96 |
C4—H4A | 0.93 | C22—H22B | 0.96 |
C5—C6 | 1.493 (7) | C22—H22C | 0.96 |
C6—C7 | 1.400 (6) | C23—H23A | 0.96 |
C7—C8 | 1.374 (7) | C23—H23B | 0.96 |
C7—H7A | 0.93 | C23—H23C | 0.96 |
C8—C9 | 1.381 (7) | O1W—H1 | 0.99 (6) |
C8—H8A | 0.93 | O1W—H2 | 0.80 (6) |
C9—C10 | 1.395 (6) | | |
| | | |
O1W—Pr1—O62 | 74.12 (11) | N1—C5—C4 | 121.3 (5) |
O1W—Pr1—O52 | 72.61 (12) | N1—C5—C6 | 116.8 (4) |
O62—Pr1—O52 | 65.69 (11) | C4—C5—C6 | 121.9 (4) |
O1W—Pr1—O41 | 137.92 (11) | N2—C6—C7 | 122.6 (5) |
O62—Pr1—O41 | 146.60 (11) | N2—C6—C5 | 116.9 (4) |
O52—Pr1—O41 | 109.18 (11) | C7—C6—C5 | 120.6 (4) |
O1W—Pr1—O51 | 76.14 (11) | C8—C7—C6 | 118.4 (5) |
O62—Pr1—O51 | 114.58 (10) | C8—C7—H7A | 120.8 |
O52—Pr1—O51 | 50.15 (10) | C6—C7—H7A | 120.8 |
O41—Pr1—O51 | 74.83 (10) | C7—C8—C9 | 120.1 (5) |
O1W—Pr1—N1 | 71.03 (12) | C7—C8—H8A | 119.9 |
O62—Pr1—N1 | 139.06 (11) | C9—C8—H8A | 119.9 |
O52—Pr1—N1 | 121.14 (12) | C8—C9—C10 | 118.8 (5) |
O41—Pr1—N1 | 73.23 (11) | C8—C9—H9A | 120.6 |
O51—Pr1—N1 | 77.02 (11) | C10—C9—H9A | 120.6 |
O1W—Pr1—O61 | 70.97 (11) | N2—C10—C9 | 122.0 (4) |
O62—Pr1—O61 | 50.04 (11) | N2—C10—C11 | 117.2 (4) |
O52—Pr1—O61 | 111.94 (10) | C9—C10—C11 | 120.7 (4) |
O41—Pr1—O61 | 136.02 (10) | N3—C11—C12 | 121.5 (4) |
O51—Pr1—O61 | 146.51 (10) | N3—C11—C10 | 116.3 (4) |
N1—Pr1—O61 | 97.74 (11) | C12—C11—C10 | 122.2 (4) |
O1W—Pr1—N3 | 137.90 (12) | C13—C12—C11 | 119.0 (5) |
O62—Pr1—N3 | 72.19 (11) | C13—C12—H12A | 120.5 |
O52—Pr1—N3 | 114.02 (11) | C11—C12—H12A | 120.5 |
O41—Pr1—N3 | 81.47 (11) | C14—C13—C12 | 120.4 (5) |
O51—Pr1—N3 | 141.74 (11) | C14—C13—H13A | 119.8 |
N1—Pr1—N3 | 124.10 (12) | C12—C13—H13A | 119.8 |
O61—Pr1—N3 | 68.20 (11) | C13—C14—C15 | 116.6 (4) |
O1W—Pr1—O42 | 142.21 (12) | C13—C14—H14A | 121.7 |
O62—Pr1—O42 | 101.07 (10) | C15—C14—H14A | 121.7 |
O52—Pr1—O42 | 71.48 (10) | N3—C15—C14 | 124.6 (5) |
O41—Pr1—O42 | 49.34 (10) | N3—C15—H15A | 117.7 |
O51—Pr1—O42 | 72.10 (10) | C14—C15—H15A | 117.7 |
N1—Pr1—O42 | 119.63 (11) | O43—N4—O42 | 121.6 (4) |
O61—Pr1—O42 | 134.63 (10) | O43—N4—O41 | 121.3 (4) |
N3—Pr1—O42 | 69.66 (11) | O42—N4—O41 | 117.1 (4) |
O1W—Pr1—N2 | 111.95 (12) | N4—O41—Pr1 | 98.5 (3) |
O62—Pr1—N2 | 114.11 (11) | N4—O42—Pr1 | 95.0 (2) |
O52—Pr1—N2 | 175.36 (11) | O53—N5—O52 | 121.7 (4) |
O41—Pr1—N2 | 68.25 (11) | O53—N5—O51 | 122.2 (4) |
O51—Pr1—N2 | 130.91 (10) | O52—N5—O51 | 116.0 (4) |
N1—Pr1—N2 | 62.32 (12) | N5—O51—Pr1 | 95.8 (2) |
O61—Pr1—N2 | 69.59 (11) | N5—O52—Pr1 | 97.4 (3) |
N3—Pr1—N2 | 62.12 (11) | O63—N6—O62 | 122.1 (4) |
O42—Pr1—N2 | 104.24 (11) | O63—N6—O61 | 121.3 (4) |
C5—N1—C1 | 118.3 (4) | O62—N6—O61 | 116.7 (4) |
C5—N1—Pr1 | 122.7 (3) | N6—O61—Pr1 | 94.8 (3) |
C1—N1—Pr1 | 119.0 (3) | N6—O62—Pr1 | 98.5 (3) |
C6—N2—C10 | 118.0 (4) | O21—C21—C23 | 120.5 (5) |
C6—N2—Pr1 | 121.2 (3) | O21—C21—C22 | 121.6 (5) |
C10—N2—Pr1 | 120.8 (3) | C23—C21—C22 | 117.9 (5) |
C15—N3—C11 | 118.0 (4) | C21—C22—H22A | 109.5 |
C15—N3—Pr1 | 118.6 (3) | C21—C22—H22B | 109.5 |
C11—N3—Pr1 | 121.8 (3) | H22A—C22—H22B | 109.5 |
N1—C1—C2 | 123.2 (4) | C21—C22—H22C | 109.5 |
N1—C1—H1A | 118.4 | H22A—C22—H22C | 109.5 |
C2—C1—H1A | 118.4 | H22B—C22—H22C | 109.5 |
C1—C2—C3 | 118.3 (5) | C21—C23—H23A | 109.5 |
C1—C2—H2A | 120.9 | C21—C23—H23B | 109.5 |
C3—C2—H2A | 120.9 | H23A—C23—H23B | 109.5 |
C2—C3—C4 | 119.5 (4) | C21—C23—H23C | 109.5 |
C2—C3—H3A | 120.3 | H23A—C23—H23C | 109.5 |
C4—C3—H3A | 120.3 | H23B—C23—H23C | 109.5 |
C3—C4—C5 | 119.4 (5) | Pr1—O1W—H1 | 109 (3) |
C3—C4—H4A | 120.3 | Pr1—O1W—H2 | 135 (4) |
C5—C4—H4A | 120.3 | H1—O1W—H2 | 95 (5) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1···O43i | 0.99 (6) | 1.94 (6) | 2.825 (5) | 148 (5) |
O1W—H2···O21 | 0.80 (6) | 1.90 (6) | 2.694 (5) | 168 (6) |
Symmetry code: (i) x, −y+1/2, z+1/2. |