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The title DyIII complex, [Dy2(C7H6NO2)4Cl2(C12H8N2)2] or [Dy2(μ3-PAA)4(Cl)2(phen)2] (PAA = 3-pyridyl­acetate, phen = 1,10-phenanthroline), obtained by reaction of Dy(ClO4)3, 3-pyridyl­acetic acid ligands and 1,10-phenanthroline, exhibits a dinuclear structure. Adjacent binuclear dimers are further connected via face-to-face ππ stacking inter­actions resulting in supra­molecular chains along the c-axis direction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314622002310/vm4049sup1.cif
Contains datablocks I, New_Global_Publ_Block

CCDC reference: 2155088

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.021
  • wR factor = 0.056
  • Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level C PLAT125_ALERT_4_C No '_symmetry_space_group_name_Hall' Given ..... Please Do ! PLAT220_ALERT_2_C NonSolvent Resd 1 C Ueq(max)/Ueq(min) Range 3.8 Ratio PLAT220_ALERT_2_C NonSolvent Resd 1 N Ueq(max)/Ueq(min) Range 3.7 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for O2 --C7 . 5.2 s.u. PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of N1 Check PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C3 Check PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C13 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C5 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C12 Check
Alert level G PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ... 2 Report PLAT005_ALERT_5_G No Embedded Refinement Details Found in the CIF Please Do ! PLAT143_ALERT_4_G s.u. on c - Axis Small or Missing .............. 0.00010 Ang. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Dy1 --Cl1 . 7.8 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Dy1 --O2 . 7.0 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Dy1 --N4 . 6.0 s.u. PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 1 Note PLAT899_ALERT_4_G SHELXL97 is Deprecated and Succeeded by SHELXL/ 2018 Note
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 9 ALERT level C = Check. Ensure it is not caused by an omission or oversight 8 ALERT level G = General information/check it is not something unexpected 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 12 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 3 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

\ Bis[µ3-2-(pyridin-3-yl)acetato-κ3O:O:O']\ bis[µ-2-(pyridin-3-yl)acetato-κ2O:O']bis[chlorido(1,10-\ phenanthroline-κ2N,N')dysprosium(III)], top
Crystal data top
[Dy2(C7H6NO2)4Cl2(C12H8N2)2]F(000) = 1276
Mr = 1300.82Dx = 1.773 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 8.8922 (1) ÅCell parameters from 7687 reflections
b = 21.5425 (3) Åθ = 2.5–27.3°
c = 12.9887 (1) ŵ = 3.22 mm1
β = 101.755 (1)°T = 296 K
V = 2435.94 (5) Å3Block, yellow
Z = 20.22 × 0.20 × 0.19 mm
Data collection top
Bruker SAINT CCD area detector
diffractometer
4487 independent reflections
Radiation source: fine-focus sealed tube3954 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
phi and ω scansθmax = 25.5°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
h = 1010
Tmin = 0.626, Tmax = 0.746k = 2623
16420 measured reflectionsl = 1515
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)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.035P)2]
where P = (Fo2 + 2Fc2)/3
4487 reflections(Δ/σ)max = 0.002
325 parametersΔρmax = 0.59 e Å3
1 restraintΔρmin = 0.34 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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.

H atoms were placed in calculated positions with C—H = 0.93 Å in phenyl and pyridine rings while C–H = 0.97 Å in CH2 groups and refined in riding mode with Uiso(H) = 1.2Ueq(C).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Dy10.387207 (12)0.510416 (5)0.855827 (7)0.03127 (3)
Cl10.13833 (7)0.58009 (3)0.81071 (5)0.05938 (19)
O30.57734 (18)0.58550 (8)0.90135 (12)0.0487 (5)
N30.4153 (2)0.55350 (10)0.67882 (13)0.0420 (5)
O10.57990 (18)0.44419 (8)0.80320 (11)0.0472 (4)
N40.2364 (2)0.45183 (9)0.69718 (13)0.0383 (5)
C70.6642 (3)0.43988 (11)0.89307 (17)0.0365 (6)
C140.6799 (3)0.60069 (12)0.97945 (18)0.0455 (6)
C180.3415 (3)0.54877 (14)0.48832 (18)0.0544 (7)
C260.3341 (3)0.52662 (12)0.58975 (17)0.0416 (6)
C250.2402 (3)0.47369 (12)0.59934 (17)0.0420 (6)
C210.1571 (3)0.44537 (15)0.50734 (18)0.0545 (8)
C60.8200 (3)0.41057 (12)0.90869 (18)0.0441 (6)
H6A0.87550.42800.85850.053*
H6B0.87700.42020.97880.053*
C240.1525 (3)0.40185 (12)0.7037 (2)0.0498 (7)
H24A0.14800.38710.77020.060*
C50.8108 (3)0.34153 (13)0.8952 (2)0.0476 (7)
C190.2538 (4)0.51931 (16)0.3983 (2)0.0687 (10)
H19A0.25830.53440.33190.082*
C220.0729 (3)0.39253 (16)0.5185 (2)0.0696 (9)
H22A0.01810.37240.45920.084*
C120.7310 (3)0.69858 (12)0.8813 (2)0.0494 (7)
C80.7993 (3)0.70351 (14)0.7954 (2)0.0662 (9)
H8A0.88290.67810.79290.079*
C110.6079 (3)0.73727 (15)0.8813 (2)0.0690 (9)
H11A0.55740.73590.93740.083*
C230.0701 (3)0.36993 (15)0.6167 (2)0.0657 (9)
H23A0.01490.33430.62520.079*
N20.7518 (3)0.74312 (14)0.7148 (2)0.0894 (9)
C170.4394 (4)0.59840 (15)0.4816 (2)0.0658 (8)
H17A0.44930.61330.41610.079*
C130.7883 (3)0.65317 (14)0.9671 (2)0.0682 (9)
H13A0.81290.67571.03310.082*
H13B0.88310.63520.95470.082*
O20.61601 (17)0.46036 (8)0.97223 (11)0.0421 (4)
O40.70410 (19)0.57482 (8)1.06850 (12)0.0509 (5)
C150.5041 (3)0.60095 (13)0.6677 (2)0.0565 (8)
H15A0.55970.61970.72810.068*
C200.1653 (4)0.47066 (18)0.4064 (2)0.0720 (10)
H20A0.10780.45270.34580.086*
C160.5196 (4)0.62483 (14)0.5697 (2)0.0690 (9)
H16A0.58420.65830.56590.083*
C10.7804 (4)0.30426 (16)0.9734 (3)0.0882 (12)
H1A0.76790.32351.03520.106*
C100.5589 (4)0.77733 (16)0.8009 (3)0.0875 (12)
H10A0.47590.80350.80110.105*
C40.8326 (4)0.31262 (18)0.8051 (3)0.0958 (12)
H4A0.85260.33560.74870.115*
N10.7671 (5)0.24248 (16)0.9688 (3)0.1415 (16)
C30.8239 (5)0.2480 (2)0.8001 (4)0.1398 (18)
H3A0.84160.22670.74130.168*
C90.6330 (5)0.77806 (17)0.7218 (3)0.0939 (13)
H9A0.59800.80550.66680.113*
C20.7889 (5)0.2167 (2)0.8833 (5)0.140 (2)
H2A0.78000.17380.87810.168*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Dy10.03380 (6)0.03284 (7)0.02427 (6)0.00167 (4)0.00091 (4)0.00130 (4)
Cl10.0556 (4)0.0664 (4)0.0473 (3)0.0255 (3)0.0104 (3)0.0088 (3)
O30.0544 (10)0.0502 (11)0.0343 (8)0.0156 (8)0.0077 (7)0.0103 (8)
N30.0500 (11)0.0439 (12)0.0303 (9)0.0042 (10)0.0043 (8)0.0054 (8)
O10.0509 (9)0.0605 (11)0.0286 (8)0.0160 (9)0.0047 (7)0.0012 (7)
N40.0372 (10)0.0439 (12)0.0312 (9)0.0055 (9)0.0009 (8)0.0030 (8)
C70.0383 (12)0.0338 (13)0.0362 (12)0.0016 (10)0.0051 (10)0.0017 (10)
C140.0493 (14)0.0429 (15)0.0403 (13)0.0087 (12)0.0003 (11)0.0052 (11)
C180.0604 (16)0.0681 (19)0.0349 (13)0.0217 (14)0.0098 (11)0.0097 (12)
C260.0482 (14)0.0459 (15)0.0290 (11)0.0127 (12)0.0041 (10)0.0035 (10)
C250.0397 (13)0.0538 (15)0.0303 (12)0.0140 (12)0.0020 (10)0.0057 (11)
C210.0440 (14)0.080 (2)0.0353 (13)0.0073 (14)0.0017 (11)0.0138 (13)
C60.0365 (12)0.0509 (16)0.0445 (13)0.0049 (11)0.0071 (10)0.0035 (11)
C240.0494 (14)0.0535 (17)0.0448 (14)0.0060 (13)0.0053 (11)0.0079 (12)
C50.0319 (12)0.0499 (16)0.0566 (15)0.0096 (11)0.0013 (11)0.0084 (12)
C190.078 (2)0.095 (3)0.0318 (14)0.0236 (18)0.0077 (14)0.0053 (14)
C220.0583 (17)0.097 (2)0.0471 (15)0.0097 (18)0.0034 (13)0.0313 (16)
C120.0444 (13)0.0429 (15)0.0568 (15)0.0134 (10)0.0005 (12)0.0090 (12)
C80.0567 (17)0.0577 (19)0.086 (2)0.0059 (15)0.0176 (16)0.0155 (16)
C110.0628 (16)0.067 (2)0.078 (2)0.0037 (13)0.0156 (16)0.0113 (17)
C230.0564 (16)0.072 (2)0.0648 (17)0.0175 (15)0.0045 (14)0.0239 (15)
N20.101 (2)0.090 (2)0.0763 (17)0.0263 (18)0.0171 (16)0.0270 (16)
C170.0842 (19)0.076 (2)0.0398 (14)0.0175 (18)0.0187 (13)0.0244 (14)
C130.0551 (16)0.072 (2)0.0658 (18)0.0288 (15)0.0150 (14)0.0267 (15)
O20.0440 (9)0.0520 (10)0.0284 (8)0.0135 (8)0.0028 (7)0.0033 (7)
O40.0602 (11)0.0502 (11)0.0347 (8)0.0181 (9)0.0083 (8)0.0070 (8)
C150.0703 (18)0.0530 (17)0.0455 (14)0.0066 (15)0.0101 (13)0.0103 (12)
C200.072 (2)0.111 (3)0.0272 (13)0.016 (2)0.0040 (13)0.0135 (16)
C160.094 (2)0.0609 (19)0.0574 (17)0.0034 (17)0.0266 (15)0.0194 (14)
C10.128 (3)0.057 (2)0.065 (2)0.012 (2)0.016 (2)0.0032 (17)
C100.069 (2)0.051 (2)0.129 (3)0.0161 (17)0.011 (2)0.004 (2)
C40.077 (2)0.103 (3)0.116 (3)0.003 (2)0.041 (2)0.048 (2)
N10.183 (3)0.057 (2)0.146 (3)0.026 (2)0.057 (3)0.026 (2)
C30.079 (2)0.124 (3)0.222 (4)0.001 (3)0.044 (3)0.118 (3)
C90.103 (3)0.060 (2)0.100 (3)0.015 (2)0.025 (2)0.026 (2)
C20.082 (3)0.062 (3)0.240 (6)0.028 (2)0.052 (3)0.042 (3)
Geometric parameters (Å, º) top
Dy1—O4i2.3069 (17)C19—C201.327 (5)
Dy1—O32.3275 (16)C19—H19A0.9300
Dy1—O2i2.3261 (14)C22—C231.371 (4)
Dy1—O12.4323 (16)C22—H22A0.9300
Dy1—O22.5170 (15)C12—C111.376 (4)
Dy1—N32.5386 (18)C12—C81.378 (4)
Dy1—N42.5516 (17)C12—C131.493 (4)
Dy1—Cl12.6392 (6)C8—N21.350 (4)
Dy1—C72.850 (2)C8—H8A0.9300
Dy1—Dy1i3.8976 (2)C11—C101.356 (4)
O3—C141.261 (3)C11—H11A0.9300
N3—C151.317 (3)C23—H23A0.9300
N3—C261.362 (3)N2—C91.315 (5)
O1—C71.256 (2)C17—C161.346 (4)
N4—C241.323 (3)C17—H17A0.9300
N4—C251.362 (3)C13—H13A0.9700
C7—O21.271 (3)C13—H13B0.9700
C7—C61.498 (3)O2—Dy1i2.3261 (14)
C14—O41.262 (3)O4—Dy1i2.3069 (17)
C14—C131.515 (4)C15—C161.405 (4)
C18—C191.417 (4)C15—H15A0.9300
C18—C261.415 (3)C20—H20A0.9300
C18—C171.393 (4)C16—H16A0.9300
C26—C251.434 (4)C1—N11.336 (5)
C25—C211.409 (3)C1—H1A0.9300
C21—C221.386 (4)C10—C91.329 (5)
C21—C201.435 (4)C10—H10A0.9300
C6—C51.498 (4)C4—C31.395 (6)
C6—H6A0.9700C4—H4A0.9300
C6—H6B0.9700N1—C21.291 (7)
C24—C231.396 (4)C3—C21.362 (7)
C24—H24A0.9300C3—H3A0.9300
C5—C11.364 (4)C9—H9A0.9300
C5—C41.374 (4)C2—H2A0.9300
O4i—Dy1—O3138.19 (5)C25—C21—C20119.7 (3)
O4i—Dy1—O2i74.46 (6)C5—C6—C7112.05 (19)
O3—Dy1—O2i73.64 (6)C5—C6—H6A109.2
O4i—Dy1—O188.97 (6)C7—C6—H6A109.2
O3—Dy1—O187.84 (6)C5—C6—H6B109.2
O2i—Dy1—O1125.15 (5)C7—C6—H6B109.2
O4i—Dy1—O273.42 (6)H6A—C6—H6B107.9
O3—Dy1—O271.86 (6)N4—C24—C23124.0 (3)
O2i—Dy1—O272.89 (6)N4—C24—H24A118.0
O1—Dy1—O252.27 (5)C23—C24—H24A118.0
O4i—Dy1—N3141.73 (6)C1—C5—C4116.8 (3)
O3—Dy1—N377.03 (6)C1—C5—C6120.8 (3)
O2i—Dy1—N3142.50 (7)C4—C5—C6122.4 (3)
O1—Dy1—N375.81 (6)C20—C19—C18121.6 (3)
O2—Dy1—N3118.94 (6)C20—C19—H19A119.2
O4i—Dy1—N477.16 (6)C18—C19—H19A119.2
O3—Dy1—N4141.62 (6)C21—C22—C23120.1 (3)
O2i—Dy1—N4143.32 (6)C21—C22—H22A120.0
O1—Dy1—N476.54 (5)C23—C22—H22A120.0
O2—Dy1—N4120.04 (6)C11—C12—C8115.8 (3)
N3—Dy1—N465.29 (6)C11—C12—C13123.2 (3)
O4i—Dy1—Cl1101.26 (5)C8—C12—C13121.0 (3)
O3—Dy1—Cl1101.19 (5)N2—C8—C12123.8 (3)
O2i—Dy1—Cl183.42 (4)N2—C8—H8A118.1
O1—Dy1—Cl1151.41 (4)C12—C8—H8A118.1
O2—Dy1—Cl1156.30 (4)C12—C11—C10121.0 (3)
N3—Dy1—Cl179.86 (5)C12—C11—H11A119.5
N4—Dy1—Cl179.81 (4)C10—C11—H11A119.5
O4i—Dy1—C782.55 (6)C24—C23—C22118.2 (3)
O3—Dy1—C776.68 (6)C24—C23—H23A120.9
O2i—Dy1—C799.24 (6)C22—C23—H23A120.9
O1—Dy1—C725.99 (5)C9—N2—C8115.9 (3)
O2—Dy1—C726.47 (5)C16—C17—C18120.1 (3)
N3—Dy1—C796.17 (6)C16—C17—H17A120.0
N4—Dy1—C799.62 (6)C18—C17—H17A120.0
Cl1—Dy1—C7175.87 (5)C12—C13—C14116.1 (2)
O4i—Dy1—Dy1i69.87 (4)C12—C13—H13A108.3
O3—Dy1—Dy1i68.34 (4)C14—C13—H13A108.3
O2i—Dy1—Dy1i38.11 (4)C12—C13—H13B108.3
O1—Dy1—Dy1i87.04 (3)C14—C13—H13B108.3
O2—Dy1—Dy1i34.78 (3)H13A—C13—H13B107.4
N3—Dy1—Dy1i141.81 (4)C7—O2—Dy1i160.55 (14)
N4—Dy1—Dy1i143.32 (4)C7—O2—Dy191.55 (12)
Cl1—Dy1—Dy1i121.533 (15)Dy1i—O2—Dy1107.11 (6)
C7—Dy1—Dy1i61.17 (4)C14—O4—Dy1i137.13 (15)
C14—O3—Dy1138.89 (15)N3—C15—C16123.7 (3)
C15—N3—C26117.5 (2)N3—C15—H15A118.1
C15—N3—Dy1123.72 (16)C16—C15—H15A118.1
C26—N3—Dy1118.73 (16)C19—C20—C21120.9 (3)
C7—O1—Dy195.93 (14)C19—C20—H20A119.6
C24—N4—C25117.5 (2)C21—C20—H20A119.6
C24—N4—Dy1124.18 (15)C17—C16—C15118.9 (3)
C25—N4—Dy1118.28 (15)C17—C16—H16A120.6
O1—C7—O2119.4 (2)C15—C16—H16A120.6
O1—C7—C6121.2 (2)N1—C1—C5125.6 (4)
O2—C7—C6119.44 (19)N1—C1—H1A117.2
O1—C7—Dy158.08 (12)C5—C1—H1A117.2
O2—C7—Dy161.98 (11)C9—C10—C11118.1 (3)
C6—C7—Dy1172.26 (17)C9—C10—H10A120.9
O4—C14—O3125.6 (2)C11—C10—H10A120.9
O4—C14—C13115.7 (2)C5—C4—C3118.4 (4)
O3—C14—C13118.7 (2)C5—C4—H4A120.8
C19—C18—C26119.7 (3)C3—C4—H4A120.8
C19—C18—C17122.6 (3)C2—N1—C1116.0 (4)
C26—C18—C17117.7 (2)C2—C3—C4118.4 (4)
N3—C26—C18122.0 (2)C2—C3—H3A120.8
N3—C26—C25118.8 (2)C4—C3—H3A120.8
C18—C26—C25119.2 (2)N2—C9—C10125.3 (3)
N4—C25—C21122.2 (2)N2—C9—H9A117.4
N4—C25—C26118.8 (2)C10—C9—H9A117.4
C21—C25—C26119.0 (2)N1—C2—C3124.7 (4)
C22—C21—C25117.9 (2)N1—C2—H2A117.6
C22—C21—C20122.4 (3)C3—C2—H2A117.6
Symmetry code: (i) x+1, y+1, z+2.
 

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