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The Pr atom in the title complex, (C10H9N2)[Pr(NO3)4(C10H8N2)(H2O)]·0.5C10H8N2, is 11-coordinated. Hydrogen bonds between the coordinated water molecule, the uncoordinated 2,2′-bipyridylium [(HBipy)+] and the centrosymmetric 2,2′-bipyridyl (Bipy) solvent molecules link the structural components into layers parallel to the ab plane.
Supporting information
CCDC reference: 258642
Key indicators
- Single-crystal X-ray study
- T = 130 K
- Mean (C-C) = 0.005 Å
- R factor = 0.029
- wR factor = 0.067
- Data-to-parameter ratio = 12.7
checkCIF/PLATON results
No syntax errors found
Alert level A
REFLT03_ALERT_3_A Reflection count < 85% complete (theta max?)
From the CIF: _diffrn_reflns_theta_max 27.48
From the CIF: _diffrn_reflns_theta_full 0.00
From the CIF: _reflns_number_total 5632
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 6801
Completeness (_total/calc) 82.81%
PLAT022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.83
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.83
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.12 Ratio
PLAT230_ALERT_2_C Hirshfeld Test Diff for C17 - C18 .. 6.55 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O31 .. 7.32 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O32 .. 5.74 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O42 .. 5.99 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O51 .. 6.01 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O61 .. 5.09 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pr - O62 .. 5.90 su
PLAT353_ALERT_3_C Long N-H Bond (0.87A) N8 - H8 ... 1.07 Ang.
Alert level G
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
From the CIF: _diffrn_reflns_theta_max 27.48
From the CIF: _reflns_number_total 5632
From the CIF: _diffrn_reflns_limit_ max hkl 21. 12. 42.
From the CIF: _diffrn_reflns_limit_ min hkl -21. -13. -33.
TEST1: Expected hkl limits for theta max
Calculated maximum hkl 23. 13. 42.
Calculated minimum hkl -23. -13. -42.
3 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
10 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
4 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
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: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
2,2'-Bipyridyl-2-ium
aqua(2,2'-bipyridyl-
κ2N,
N')tetakis(nitrato-
κ2O,
O')praseodymium(III) 2,2'-bipyridyl solvate
top
Crystal data top
(C10H9N2)[Pr(NO3)4(C10H8N2)(H2O)]·0.5C10H8N2 | F(000) = 3192 |
Mr = 798.43 | Dx = 1.792 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from all [please provide number] reflections |
a = 17.7935 (4) Å | θ = 2–27.5° |
b = 10.2712 (3) Å | µ = 1.73 mm−1 |
c = 32.8924 (8) Å | T = 130 K |
β = 100.0016 (11)° | Prism, green |
V = 5920.1 (3) Å3 | 0.36 × 0.22 × 0.18 mm |
Z = 8 | |
Data collection top
Nonius KappaCCD diffractometer | 5632 independent reflections |
Radiation source: fine-focus sealed tube | 5000 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
φ–ω scans to cover a hemisphere of the reciprocal space | θmax = 27.5°, θmin = 2.3° |
Absorption correction: empirical (using intensity measurements) (MULABS; Blessing, 1995) | h = −21→21 |
Tmin = 0.638, Tmax = 0.732 | k = −13→12 |
15166 measured reflections | l = −33→42 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.067 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0144P)2 + 13.7668P] where P = (Fo2 + 2Fc2)/3 |
5632 reflections | (Δ/σ)max = 0.001 |
442 parameters | Δρmax = 0.52 e Å−3 |
0 restraints | Δρmin = −0.64 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 6 flagged for potential
systematic errors |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pr | 0.329865 (9) | 0.373465 (14) | 0.111752 (5) | 0.01409 (6) | |
N1 | 0.27926 (15) | 0.6215 (2) | 0.11025 (8) | 0.0178 (5) | |
N2 | 0.18090 (14) | 0.4153 (2) | 0.09983 (8) | 0.0155 (5) | |
N3 | 0.31562 (16) | 0.1416 (2) | 0.05214 (8) | 0.0192 (6) | |
N4 | 0.32199 (17) | 0.1558 (2) | 0.17358 (9) | 0.0229 (6) | |
N5 | 0.49371 (15) | 0.4554 (2) | 0.10817 (8) | 0.0203 (6) | |
N6 | 0.35665 (15) | 0.5133 (2) | 0.19454 (8) | 0.0189 (6) | |
N7 | 0.63127 (17) | −0.1031 (3) | 0.20245 (9) | 0.0288 (7) | |
N8 | 0.68206 (17) | 0.1453 (3) | 0.20935 (9) | 0.0298 (7) | |
H8 | 0.718 (2) | 0.063 (3) | 0.2073 (12) | 0.036* | |
N9 | 0.41251 (16) | 0.5846 (2) | 0.00387 (8) | 0.0232 (6) | |
O1W | 0.30918 (14) | 0.4441 (2) | 0.03931 (8) | 0.0229 (5) | |
H11 | 0.275 (2) | 0.435 (4) | 0.0239 (13) | 0.034* | |
H12 | 0.338 (2) | 0.484 (4) | 0.0303 (12) | 0.034* | |
O31 | 0.25483 (12) | 0.20000 (19) | 0.05501 (7) | 0.0222 (5) | |
O32 | 0.37510 (13) | 0.1680 (2) | 0.07837 (7) | 0.0243 (5) | |
O33 | 0.31835 (14) | 0.0613 (2) | 0.02441 (7) | 0.0297 (6) | |
O41 | 0.38354 (13) | 0.2175 (2) | 0.17246 (7) | 0.0268 (5) | |
O42 | 0.26494 (13) | 0.18605 (19) | 0.14651 (7) | 0.0247 (5) | |
O43 | 0.31851 (15) | 0.0720 (2) | 0.19981 (8) | 0.0370 (6) | |
O51 | 0.48010 (13) | 0.34101 (18) | 0.11932 (7) | 0.0223 (5) | |
O52 | 0.43580 (12) | 0.52476 (19) | 0.09346 (7) | 0.0210 (5) | |
O53 | 0.55862 (13) | 0.4985 (2) | 0.11144 (9) | 0.0360 (7) | |
O61 | 0.40918 (13) | 0.4958 (2) | 0.17360 (7) | 0.0234 (5) | |
O62 | 0.29378 (12) | 0.45499 (19) | 0.18239 (7) | 0.0218 (5) | |
O63 | 0.36575 (14) | 0.5856 (2) | 0.22480 (7) | 0.0277 (5) | |
C1 | 0.32816 (18) | 0.7228 (3) | 0.11394 (10) | 0.0221 (7) | |
H1A | 0.3802 | 0.7053 | 0.1174 | 0.027* | |
C2 | 0.3048 (2) | 0.8519 (3) | 0.11285 (11) | 0.0245 (7) | |
H2A | 0.3404 | 0.9190 | 0.1155 | 0.029* | |
C3 | 0.2280 (2) | 0.8787 (3) | 0.10778 (11) | 0.0254 (7) | |
H3A | 0.2106 | 0.9642 | 0.1069 | 0.030* | |
C4 | 0.17696 (19) | 0.7754 (3) | 0.10407 (11) | 0.0236 (7) | |
H4A | 0.1248 | 0.7912 | 0.1006 | 0.028* | |
C5 | 0.20414 (18) | 0.6481 (2) | 0.10561 (9) | 0.0154 (6) | |
C6 | 0.15027 (17) | 0.5357 (3) | 0.10198 (9) | 0.0150 (6) | |
C7 | 0.07239 (18) | 0.5532 (3) | 0.10052 (10) | 0.0191 (7) | |
H7A | 0.0529 | 0.6365 | 0.1027 | 0.023* | |
C8 | 0.02379 (18) | 0.4473 (3) | 0.09585 (10) | 0.0211 (7) | |
H8A | −0.0285 | 0.4583 | 0.0943 | 0.025* | |
C9 | 0.05462 (18) | 0.3243 (3) | 0.09346 (9) | 0.0192 (7) | |
H9A | 0.0236 | 0.2508 | 0.0905 | 0.023* | |
C10 | 0.13217 (18) | 0.3136 (3) | 0.09550 (9) | 0.0184 (6) | |
H10A | 0.1524 | 0.2308 | 0.0938 | 0.022* | |
C11 | 0.6061 (2) | −0.2274 (3) | 0.19810 (11) | 0.0320 (8) | |
H11A | 0.6412 | −0.2936 | 0.1967 | 0.038* | |
C12 | 0.5304 (2) | −0.2595 (3) | 0.19568 (11) | 0.0333 (9) | |
H12A | 0.5147 | −0.3459 | 0.1931 | 0.040* | |
C13 | 0.4784 (2) | −0.1613 (4) | 0.19713 (11) | 0.0336 (9) | |
H13A | 0.4270 | −0.1813 | 0.1957 | 0.040* | |
C14 | 0.50189 (18) | −0.0336 (3) | 0.20070 (10) | 0.0213 (7) | |
H14A | 0.4672 | 0.0338 | 0.2013 | 0.026* | |
C15 | 0.57786 (18) | −0.0095 (3) | 0.20326 (9) | 0.0185 (6) | |
C16 | 0.60653 (18) | 0.1258 (3) | 0.20687 (9) | 0.0181 (6) | |
C17 | 0.55938 (19) | 0.2311 (3) | 0.20634 (11) | 0.0262 (7) | |
H17A | 0.5069 | 0.2204 | 0.2041 | 0.031* | |
C18 | 0.5921 (3) | 0.3560 (3) | 0.20927 (14) | 0.0528 (13) | |
H18A | 0.5612 | 0.4290 | 0.2093 | 0.063* | |
C19 | 0.6696 (3) | 0.3705 (4) | 0.21215 (13) | 0.0565 (15) | |
H19A | 0.6915 | 0.4531 | 0.2142 | 0.068* | |
C20 | 0.7137 (3) | 0.2635 (4) | 0.21196 (12) | 0.0442 (10) | |
H20A | 0.7662 | 0.2723 | 0.2137 | 0.053* | |
C21 | 0.3842 (2) | 0.7064 (3) | 0.00232 (11) | 0.0280 (8) | |
H21A | 0.3340 | 0.7179 | 0.0060 | 0.034* | |
C22 | 0.4260 (2) | 0.8153 (3) | −0.00450 (10) | 0.0260 (8) | |
H22A | 0.4043 | 0.8979 | −0.0056 | 0.031* | |
C23 | 0.5001 (2) | 0.7984 (3) | −0.00959 (11) | 0.0275 (8) | |
H23A | 0.5297 | 0.8697 | −0.0143 | 0.033* | |
C24 | 0.5306 (2) | 0.6737 (3) | −0.00772 (11) | 0.0256 (8) | |
H24A | 0.5810 | 0.6606 | −0.0109 | 0.031* | |
C25 | 0.48495 (19) | 0.5685 (3) | −0.00108 (9) | 0.0203 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pr | 0.01210 (11) | 0.01206 (8) | 0.01806 (9) | 0.00112 (6) | 0.00250 (7) | −0.00142 (6) |
N1 | 0.0172 (14) | 0.0147 (11) | 0.0221 (13) | 0.0020 (10) | 0.0055 (12) | −0.0006 (10) |
N2 | 0.0151 (14) | 0.0119 (11) | 0.0194 (13) | 0.0020 (9) | 0.0032 (12) | −0.0011 (9) |
N3 | 0.0207 (16) | 0.0153 (12) | 0.0222 (14) | 0.0022 (10) | 0.0056 (13) | −0.0006 (10) |
N4 | 0.0290 (17) | 0.0183 (13) | 0.0222 (15) | 0.0033 (11) | 0.0064 (14) | 0.0003 (10) |
N5 | 0.0155 (15) | 0.0180 (13) | 0.0283 (15) | 0.0005 (10) | 0.0062 (13) | −0.0049 (10) |
N6 | 0.0186 (15) | 0.0164 (12) | 0.0214 (14) | 0.0001 (10) | 0.0029 (13) | −0.0004 (10) |
N7 | 0.0266 (17) | 0.0292 (15) | 0.0315 (17) | 0.0023 (12) | 0.0074 (15) | 0.0037 (12) |
N8 | 0.0241 (17) | 0.0346 (16) | 0.0307 (17) | −0.0002 (12) | 0.0049 (15) | 0.0059 (12) |
N9 | 0.0256 (17) | 0.0226 (13) | 0.0228 (14) | 0.0021 (11) | 0.0080 (13) | 0.0029 (11) |
O1W | 0.0166 (14) | 0.0277 (12) | 0.0245 (13) | −0.0040 (10) | 0.0037 (11) | 0.0022 (10) |
O31 | 0.0177 (12) | 0.0198 (11) | 0.0299 (13) | 0.0031 (9) | 0.0062 (11) | −0.0042 (9) |
O32 | 0.0166 (13) | 0.0222 (11) | 0.0313 (13) | 0.0022 (9) | −0.0036 (11) | −0.0082 (9) |
O33 | 0.0298 (14) | 0.0269 (12) | 0.0305 (13) | 0.0070 (10) | 0.0004 (12) | −0.0160 (10) |
O41 | 0.0218 (13) | 0.0279 (12) | 0.0301 (13) | 0.0043 (9) | 0.0026 (11) | 0.0055 (10) |
O42 | 0.0254 (14) | 0.0199 (11) | 0.0269 (13) | −0.0006 (9) | −0.0010 (11) | 0.0027 (9) |
O43 | 0.0479 (18) | 0.0340 (13) | 0.0300 (14) | 0.0006 (11) | 0.0093 (14) | 0.0149 (11) |
O51 | 0.0199 (13) | 0.0110 (9) | 0.0370 (14) | 0.0010 (8) | 0.0074 (11) | 0.0001 (9) |
O52 | 0.0142 (12) | 0.0198 (10) | 0.0291 (13) | 0.0039 (8) | 0.0037 (10) | 0.0026 (9) |
O53 | 0.0120 (13) | 0.0230 (12) | 0.073 (2) | −0.0013 (9) | 0.0087 (14) | −0.0014 (12) |
O61 | 0.0179 (12) | 0.0295 (12) | 0.0242 (12) | −0.0019 (9) | 0.0073 (11) | −0.0067 (9) |
O62 | 0.0157 (12) | 0.0252 (11) | 0.0253 (12) | −0.0050 (9) | 0.0052 (11) | −0.0025 (9) |
O63 | 0.0327 (15) | 0.0281 (12) | 0.0225 (12) | −0.0040 (10) | 0.0058 (12) | −0.0110 (10) |
C1 | 0.0163 (18) | 0.0180 (14) | 0.0333 (19) | −0.0011 (11) | 0.0075 (16) | −0.0019 (13) |
C2 | 0.0244 (19) | 0.0155 (15) | 0.0340 (19) | −0.0018 (12) | 0.0064 (17) | −0.0011 (12) |
C3 | 0.0247 (19) | 0.0142 (14) | 0.036 (2) | 0.0036 (12) | 0.0021 (17) | −0.0003 (13) |
C4 | 0.0185 (18) | 0.0170 (14) | 0.0341 (19) | 0.0032 (12) | 0.0011 (16) | −0.0018 (13) |
C5 | 0.0168 (17) | 0.0145 (13) | 0.0144 (14) | 0.0032 (11) | 0.0016 (13) | −0.0005 (10) |
C6 | 0.0164 (17) | 0.0147 (13) | 0.0148 (14) | 0.0031 (11) | 0.0049 (13) | 0.0004 (11) |
C7 | 0.0179 (17) | 0.0175 (14) | 0.0225 (16) | 0.0065 (12) | 0.0054 (15) | 0.0023 (12) |
C8 | 0.0107 (16) | 0.0277 (16) | 0.0259 (17) | 0.0025 (12) | 0.0058 (15) | 0.0036 (13) |
C9 | 0.0183 (18) | 0.0193 (14) | 0.0200 (16) | −0.0041 (12) | 0.0037 (14) | 0.0010 (12) |
C10 | 0.0213 (18) | 0.0126 (13) | 0.0218 (16) | −0.0015 (11) | 0.0054 (15) | −0.0012 (11) |
C11 | 0.039 (2) | 0.0216 (16) | 0.035 (2) | 0.0060 (14) | 0.0049 (19) | 0.0038 (14) |
C12 | 0.044 (2) | 0.0215 (16) | 0.032 (2) | −0.0117 (15) | −0.0003 (19) | 0.0043 (14) |
C13 | 0.022 (2) | 0.049 (2) | 0.0289 (19) | −0.0134 (16) | 0.0017 (17) | 0.0089 (16) |
C14 | 0.0172 (18) | 0.0281 (16) | 0.0190 (16) | 0.0027 (12) | 0.0042 (15) | 0.0024 (12) |
C15 | 0.0190 (17) | 0.0189 (14) | 0.0183 (15) | 0.0000 (12) | 0.0052 (14) | 0.0025 (11) |
C16 | 0.0169 (17) | 0.0203 (14) | 0.0163 (15) | −0.0027 (12) | 0.0007 (14) | −0.0008 (11) |
C17 | 0.0199 (19) | 0.0288 (17) | 0.0307 (19) | 0.0060 (13) | 0.0061 (16) | 0.0049 (14) |
C18 | 0.095 (4) | 0.0234 (19) | 0.045 (3) | 0.026 (2) | 0.024 (3) | 0.0024 (17) |
C19 | 0.100 (5) | 0.038 (2) | 0.035 (2) | −0.038 (2) | 0.022 (3) | −0.0118 (18) |
C20 | 0.041 (3) | 0.055 (3) | 0.035 (2) | −0.026 (2) | 0.002 (2) | 0.0031 (19) |
C21 | 0.026 (2) | 0.0273 (17) | 0.0316 (19) | 0.0076 (13) | 0.0075 (17) | 0.0035 (14) |
C22 | 0.035 (2) | 0.0218 (16) | 0.0219 (17) | 0.0067 (14) | 0.0068 (17) | 0.0009 (13) |
C23 | 0.039 (2) | 0.0172 (15) | 0.0296 (19) | −0.0033 (13) | 0.0139 (18) | −0.0012 (13) |
C24 | 0.030 (2) | 0.0196 (15) | 0.0314 (19) | 0.0002 (13) | 0.0168 (17) | −0.0012 (13) |
C25 | 0.027 (2) | 0.0205 (15) | 0.0148 (15) | 0.0006 (13) | 0.0079 (15) | 0.0007 (11) |
Geometric parameters (Å, º) top
Pr—O1W | 2.457 (2) | C3—C4 | 1.388 (4) |
Pr—O32 | 2.572 (2) | C3—H3A | 0.9300 |
Pr—O61 | 2.591 (2) | C4—C5 | 1.392 (4) |
Pr—O52 | 2.593 (2) | C4—H4A | 0.9300 |
Pr—O41 | 2.608 (2) | C5—C6 | 1.492 (4) |
Pr—O42 | 2.609 (2) | C6—C7 | 1.390 (4) |
Pr—N2 | 2.646 (2) | C7—C8 | 1.382 (4) |
Pr—O62 | 2.652 (2) | C7—H7A | 0.9300 |
Pr—O51 | 2.662 (2) | C8—C9 | 1.385 (4) |
Pr—N1 | 2.700 (2) | C8—H8A | 0.9300 |
Pr—O31 | 2.752 (2) | C9—C10 | 1.374 (4) |
N1—C5 | 1.347 (4) | C9—H9A | 0.9300 |
N1—C1 | 1.348 (4) | C10—H10A | 0.9300 |
N2—C10 | 1.349 (4) | C11—C12 | 1.375 (5) |
N2—C6 | 1.358 (3) | C11—H11A | 0.9300 |
N3—O33 | 1.237 (3) | C12—C13 | 1.376 (5) |
N3—O31 | 1.255 (3) | C12—H12A | 0.9300 |
N3—O32 | 1.273 (3) | C13—C14 | 1.375 (5) |
N4—O43 | 1.228 (3) | C13—H13A | 0.9300 |
N4—O42 | 1.267 (4) | C14—C15 | 1.362 (4) |
N4—O41 | 1.272 (3) | C14—H14A | 0.9300 |
N5—O53 | 1.224 (3) | C15—C16 | 1.478 (4) |
N5—O51 | 1.267 (3) | C16—C17 | 1.367 (4) |
N5—O52 | 1.277 (3) | C17—C18 | 1.405 (5) |
N6—O63 | 1.230 (3) | C17—H17A | 0.9300 |
N6—O61 | 1.266 (3) | C18—C19 | 1.374 (7) |
N6—O62 | 1.271 (3) | C18—H18A | 0.9300 |
N7—C11 | 1.353 (4) | C19—C20 | 1.351 (6) |
N7—C15 | 1.355 (4) | C19—H19A | 0.9300 |
N8—C20 | 1.335 (4) | C20—H20A | 0.9300 |
N8—C16 | 1.347 (4) | C21—C22 | 1.383 (4) |
N8—H8 | 1.07 (4) | C21—H21A | 0.9300 |
N9—C25 | 1.337 (4) | C22—C23 | 1.369 (5) |
N9—C21 | 1.346 (4) | C22—H22A | 0.9300 |
O1W—H11 | 0.73 (4) | C23—C24 | 1.388 (4) |
O1W—H12 | 0.75 (4) | C23—H23A | 0.9300 |
C1—C2 | 1.388 (4) | C24—C25 | 1.392 (4) |
C1—H1A | 0.9300 | C24—H24A | 0.9300 |
C2—C3 | 1.376 (5) | C25—C25i | 1.503 (6) |
C2—H2A | 0.9300 | | |
| | | |
O1W—Pr—O32 | 80.41 (8) | N3—O32—Pr | 100.32 (15) |
O1W—Pr—O61 | 126.01 (7) | N4—O41—Pr | 97.22 (18) |
O32—Pr—O61 | 124.40 (7) | N4—O42—Pr | 97.32 (16) |
O1W—Pr—O52 | 65.83 (8) | N5—O51—Pr | 95.51 (16) |
O32—Pr—O52 | 95.67 (6) | N5—O52—Pr | 98.58 (15) |
O61—Pr—O52 | 64.71 (7) | N6—O61—Pr | 98.22 (17) |
O1W—Pr—O41 | 153.79 (7) | N6—O62—Pr | 95.19 (15) |
O32—Pr—O41 | 73.90 (7) | N1—C1—C2 | 123.3 (3) |
O61—Pr—O41 | 67.64 (7) | N1—C1—H1A | 118.4 |
O52—Pr—O41 | 111.19 (7) | C2—C1—H1A | 118.4 |
O1W—Pr—O42 | 129.77 (8) | C3—C2—C1 | 118.8 (3) |
O32—Pr—O42 | 77.10 (7) | C3—C2—H2A | 120.6 |
O61—Pr—O42 | 103.65 (7) | C1—C2—H2A | 120.6 |
O52—Pr—O42 | 159.88 (7) | C2—C3—C4 | 118.6 (3) |
O41—Pr—O42 | 48.89 (7) | C2—C3—H3A | 120.7 |
O1W—Pr—N2 | 80.26 (8) | C4—C3—H3A | 120.7 |
O32—Pr—N2 | 116.73 (7) | C3—C4—C5 | 119.8 (3) |
O61—Pr—N2 | 115.63 (7) | C3—C4—H4A | 120.1 |
O52—Pr—N2 | 128.17 (7) | C5—C4—H4A | 120.1 |
O41—Pr—N2 | 115.94 (7) | N1—C5—C4 | 121.7 (3) |
O42—Pr—N2 | 71.12 (7) | N1—C5—C6 | 117.6 (2) |
O1W—Pr—O62 | 137.60 (7) | C4—C5—C6 | 120.6 (3) |
O32—Pr—O62 | 140.77 (7) | N2—C6—C7 | 121.5 (3) |
O61—Pr—O62 | 48.74 (6) | N2—C6—C5 | 116.8 (3) |
O52—Pr—O62 | 108.09 (6) | C7—C6—C5 | 121.7 (2) |
O41—Pr—O62 | 68.61 (7) | C8—C7—C6 | 120.2 (3) |
O42—Pr—O62 | 69.88 (6) | C8—C7—H7A | 119.9 |
N2—Pr—O62 | 71.93 (7) | C6—C7—H7A | 119.9 |
O1W—Pr—O51 | 96.12 (8) | C7—C8—C9 | 118.6 (3) |
O32—Pr—O51 | 63.49 (7) | C7—C8—H8A | 120.7 |
O61—Pr—O51 | 65.55 (7) | C9—C8—H8A | 120.7 |
O52—Pr—O51 | 48.56 (6) | C10—C9—C8 | 118.3 (3) |
O41—Pr—O51 | 67.87 (7) | C10—C9—H9A | 120.8 |
O42—Pr—O51 | 112.36 (7) | C8—C9—H9A | 120.8 |
N2—Pr—O51 | 176.18 (7) | N2—C10—C9 | 124.4 (3) |
O62—Pr—O51 | 110.46 (7) | N2—C10—H10A | 117.8 |
O1W—Pr—N1 | 73.16 (8) | C9—C10—H10A | 117.8 |
O32—Pr—N1 | 153.47 (8) | N7—C11—C12 | 122.3 (3) |
O61—Pr—N1 | 72.02 (8) | N7—C11—H11A | 118.8 |
O52—Pr—N1 | 71.56 (7) | C12—C11—H11A | 118.8 |
O41—Pr—N1 | 132.09 (7) | C11—C12—C13 | 118.7 (3) |
O42—Pr—N1 | 122.19 (7) | C11—C12—H12A | 120.6 |
N2—Pr—N1 | 61.42 (7) | C13—C12—H12A | 120.6 |
O62—Pr—N1 | 65.62 (7) | C14—C13—C12 | 120.3 (3) |
O51—Pr—N1 | 116.49 (7) | C14—C13—H13A | 119.8 |
O1W—Pr—O31 | 63.90 (7) | C12—C13—H13A | 119.8 |
O32—Pr—O31 | 47.95 (7) | C15—C14—C13 | 117.6 (3) |
O61—Pr—O31 | 168.63 (7) | C15—C14—H14A | 121.2 |
O52—Pr—O31 | 121.15 (6) | C13—C14—H14A | 121.2 |
O41—Pr—O31 | 101.04 (7) | N7—C15—C14 | 124.2 (3) |
O42—Pr—O31 | 67.66 (7) | N7—C15—C16 | 115.8 (3) |
N2—Pr—O31 | 69.47 (6) | C14—C15—C16 | 120.1 (3) |
O62—Pr—O31 | 129.48 (6) | N8—C16—C17 | 119.1 (3) |
O51—Pr—O31 | 110.08 (6) | N8—C16—C15 | 118.2 (3) |
N1—Pr—O31 | 118.52 (7) | C17—C16—C15 | 122.7 (3) |
C5—N1—C1 | 117.8 (2) | C16—C17—C18 | 118.4 (3) |
C5—N1—Pr | 120.96 (17) | C16—C17—H17A | 120.8 |
C1—N1—Pr | 121.2 (2) | C18—C17—H17A | 120.8 |
C10—N2—C6 | 117.0 (3) | C19—C18—C17 | 120.2 (3) |
C10—N2—Pr | 119.91 (19) | C19—C18—H18A | 119.9 |
C6—N2—Pr | 122.75 (19) | C17—C18—H18A | 119.9 |
O33—N3—O31 | 121.3 (3) | C20—C19—C18 | 119.2 (4) |
O33—N3—O32 | 120.5 (2) | C20—C19—H19A | 120.4 |
O31—N3—O32 | 118.2 (2) | C18—C19—H19A | 120.4 |
O43—N4—O42 | 122.3 (3) | N8—C20—C19 | 120.1 (4) |
O43—N4—O41 | 121.2 (3) | N8—C20—H20A | 119.9 |
O42—N4—O41 | 116.5 (2) | C19—C20—H20A | 119.9 |
O53—N5—O51 | 122.3 (3) | N9—C21—C22 | 123.3 (3) |
O53—N5—O52 | 121.3 (2) | N9—C21—H21A | 118.3 |
O51—N5—O52 | 116.4 (2) | C22—C21—H21A | 118.3 |
O63—N6—O61 | 121.3 (3) | C23—C22—C21 | 118.3 (3) |
O63—N6—O62 | 121.6 (2) | C23—C22—H22A | 120.9 |
O61—N6—O62 | 117.1 (2) | C21—C22—H22A | 120.9 |
C11—N7—C15 | 116.8 (3) | C22—C23—C24 | 119.3 (3) |
C20—N8—C16 | 123.0 (3) | C22—C23—H23A | 120.4 |
C20—N8—H8 | 118.2 (19) | C24—C23—H23A | 120.4 |
C16—N8—H8 | 119 (2) | C23—C24—C25 | 119.3 (3) |
C25—N9—C21 | 118.2 (3) | C23—C24—H24A | 120.4 |
Pr—O1W—H11 | 127 (3) | C25—C24—H24A | 120.4 |
Pr—O1W—H12 | 123 (3) | N9—C25—C24 | 121.6 (3) |
H11—O1W—H12 | 110 (4) | N9—C25—C25i | 116.9 (3) |
N3—O31—Pr | 92.15 (17) | C24—C25—C25i | 121.4 (4) |
Symmetry code: (i) −x+1, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N8—H8···O62ii | 1.07 (4) | 2.03 (4) | 3.028 (4) | 155 (3) |
O1W—H12···N9 | 0.75 (4) | 2.00 (4) | 2.751 (3) | 177 (4) |
O1W—H11···O33iii | 0.73 (4) | 2.09 (4) | 2.809 (3) | 171 (4) |
Symmetry codes: (ii) x+1/2, y−1/2, z; (iii) −x+1/2, −y+1/2, −z. |
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