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The dimeric title complex, [Ho2(CH3COO)6(C12H8N2)2], lies about a centre of symmetry. Each cation is coordinated by a chelating 1,10-phenanthroline and two chelating acetato ligands, one of which also bridges the two Ho atoms. Two other bridging acetate ligands complete the coordination of the nine-coordinate holmium(III) atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806045144/sj2149sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806045144/sj2149Isup2.hkl
Contains datablock I

CCDC reference: 630468

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.019 Å
  • R factor = 0.058
  • wR factor = 0.133
  • Data-to-parameter ratio = 14.0

checkCIF/PLATON results

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Alert level C PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 19
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 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 0 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 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Tetra-µ-acetato-κ4O:O';κ3O,O':O';κ3O:O,O'- bis[(acetato-κ2O,O')(1,10-phenanthroline-κ2N,N')holmium(III)] top
Crystal data top
[Ho2(C2H3O2)6(C12H8N2)2]Z = 1
Mr = 1044.53F(000) = 508
Triclinic, P1Dx = 1.933 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.717 (4) ÅCell parameters from 2020 reflections
b = 8.926 (4) Åθ = 2.4–21.8°
c = 12.914 (6) ŵ = 4.45 mm1
α = 103.318 (7)°T = 298 K
β = 109.007 (6)°Block, colorless
γ = 98.380 (7)°0.05 × 0.03 × 0.03 mm
V = 897.5 (7) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
3449 independent reflections
Radiation source: fine-focus sealed tube2749 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.054
φ and ω scansθmax = 26.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1010
Tmin = 0.855, Tmax = 0.873k = 1010
6456 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)] = 0.058Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.133H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0675P)2]
where P = (Fo2 + 2Fc2)/3
3449 reflections(Δ/σ)max < 0.001
247 parametersΔρmax = 2.03 e Å3
0 restraintsΔρmin = 1.86 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
Ho1.02444 (6)0.15401 (6)0.14258 (4)0.02774 (18)
O50.7578 (9)0.1034 (9)0.0033 (6)0.0390 (18)
O40.9232 (9)0.1399 (9)0.0243 (6)0.0357 (17)
N10.8639 (10)0.2752 (10)0.2581 (7)0.031 (2)
O61.2559 (9)0.0469 (9)0.1678 (6)0.0390 (18)
O30.8802 (9)0.0692 (9)0.1833 (6)0.0413 (19)
O21.0007 (10)0.4114 (9)0.1139 (7)0.046 (2)
C170.6840 (12)0.0333 (13)0.1025 (10)0.033 (3)
N21.1377 (11)0.1765 (11)0.3598 (7)0.039 (2)
C111.0447 (14)0.2216 (15)0.4213 (10)0.042 (3)
C160.8562 (12)0.1691 (14)0.0920 (10)0.037 (3)
C141.1507 (15)0.4754 (14)0.1781 (10)0.043 (3)
C10.7321 (14)0.3321 (14)0.2082 (10)0.042 (3)
H10.70780.33490.13310.050*
O11.2378 (10)0.3958 (10)0.2289 (7)0.046 (2)
C150.7467 (16)0.3344 (14)0.0629 (10)0.047 (3)
H15A0.81560.40890.07050.071*
H15B0.66750.36450.01460.071*
H15C0.68810.33360.11430.071*
C120.8981 (13)0.2732 (13)0.3655 (10)0.039 (3)
C131.2253 (17)0.6419 (14)0.1840 (11)0.054 (3)
H13A1.18190.71550.22690.081*
H13B1.19680.65110.10780.081*
H13C1.34460.66530.22110.081*
C40.8033 (14)0.3322 (16)0.4319 (10)0.048 (3)
C180.5082 (14)0.0466 (15)0.1540 (11)0.049 (3)
H18A0.43450.03110.14060.074*
H18B0.47770.02880.23510.074*
H18C0.49930.15080.11950.074*
C30.6660 (15)0.3885 (15)0.3783 (11)0.051 (3)
H30.60000.42590.41740.061*
C20.6314 (16)0.3868 (16)0.2661 (12)0.055 (3)
H20.54000.42240.22840.066*
C101.2727 (15)0.1323 (16)0.4130 (11)0.053 (3)
H101.34210.10760.37340.064*
C71.0827 (15)0.2203 (15)0.5381 (10)0.047 (3)
C91.3184 (18)0.1203 (18)0.5234 (11)0.067 (4)
H91.41210.08370.55530.080*
C50.8505 (18)0.3322 (19)0.5513 (11)0.065 (4)
H50.78950.37060.59420.078*
C60.9833 (17)0.2761 (18)0.5987 (12)0.066 (4)
H61.01070.27390.67410.079*
C81.2224 (17)0.1635 (18)0.5838 (10)0.061 (4)
H81.25070.15500.65770.073*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ho0.0289 (3)0.0387 (3)0.0261 (3)0.0153 (2)0.01626 (19)0.0157 (2)
O50.038 (4)0.054 (5)0.033 (4)0.018 (4)0.016 (4)0.020 (4)
O40.040 (4)0.050 (5)0.039 (4)0.018 (4)0.032 (4)0.025 (4)
N10.023 (4)0.040 (5)0.031 (5)0.004 (4)0.015 (4)0.005 (4)
O60.037 (4)0.061 (5)0.028 (4)0.025 (4)0.015 (3)0.017 (4)
O30.048 (5)0.052 (5)0.036 (4)0.014 (4)0.028 (4)0.016 (4)
O20.042 (5)0.044 (5)0.062 (6)0.009 (4)0.027 (4)0.023 (4)
C170.031 (6)0.044 (7)0.046 (7)0.016 (5)0.027 (5)0.030 (6)
N20.035 (5)0.055 (6)0.031 (5)0.016 (5)0.015 (4)0.013 (4)
C110.038 (6)0.061 (8)0.041 (7)0.012 (6)0.025 (5)0.029 (6)
C160.027 (6)0.044 (7)0.048 (7)0.014 (5)0.016 (5)0.025 (6)
C140.047 (7)0.048 (7)0.048 (7)0.024 (6)0.028 (6)0.020 (6)
C10.051 (7)0.052 (8)0.033 (6)0.024 (6)0.018 (6)0.023 (6)
O10.045 (5)0.050 (5)0.046 (5)0.015 (4)0.015 (4)0.019 (4)
C150.065 (8)0.041 (7)0.046 (7)0.013 (6)0.030 (6)0.019 (6)
C120.036 (6)0.045 (7)0.048 (7)0.009 (5)0.028 (6)0.020 (6)
C130.069 (9)0.044 (8)0.052 (8)0.011 (7)0.027 (7)0.018 (6)
C40.039 (7)0.063 (9)0.041 (7)0.007 (6)0.024 (6)0.005 (6)
C180.048 (7)0.055 (8)0.058 (8)0.025 (6)0.024 (6)0.027 (7)
C30.047 (7)0.061 (9)0.056 (8)0.020 (6)0.032 (6)0.017 (7)
C20.049 (8)0.061 (9)0.066 (9)0.026 (7)0.032 (7)0.017 (7)
C100.050 (7)0.073 (10)0.044 (7)0.026 (7)0.019 (6)0.023 (7)
C70.052 (7)0.058 (8)0.030 (6)0.016 (6)0.015 (6)0.014 (6)
C90.068 (9)0.095 (12)0.040 (7)0.045 (9)0.010 (7)0.025 (8)
C50.073 (10)0.104 (12)0.047 (8)0.036 (9)0.046 (7)0.033 (8)
C60.065 (9)0.105 (13)0.043 (8)0.030 (9)0.031 (7)0.030 (8)
C80.063 (9)0.094 (11)0.030 (7)0.020 (8)0.013 (6)0.030 (7)
Geometric parameters (Å, º) top
Ho—O62.317 (7)C1—C21.396 (15)
Ho—O4i2.324 (7)C1—H10.9300
Ho—O52.332 (7)C15—H15A0.9600
Ho—O12.394 (8)C15—H15B0.9600
Ho—O22.437 (8)C15—H15C0.9600
Ho—O32.452 (8)C12—C41.440 (15)
Ho—N12.533 (8)C13—H13A0.9600
Ho—O42.568 (8)C13—H13B0.9600
Ho—N22.600 (9)C13—H13C0.9600
Ho—Hoi3.9082 (17)C4—C31.400 (16)
O5—C171.260 (13)C4—C51.461 (17)
O4—C161.252 (12)C18—H18A0.9600
O4—Hoi2.324 (7)C18—H18B0.9600
N1—C121.325 (13)C18—H18C0.9600
N1—C11.354 (13)C3—C21.376 (17)
O6—C17i1.271 (12)C3—H30.9300
O3—C161.237 (13)C2—H20.9300
O2—C141.258 (14)C10—C91.385 (17)
C17—O6i1.271 (12)C10—H100.9300
C17—C181.494 (14)C7—C81.392 (17)
N2—C101.321 (14)C7—C61.413 (16)
N2—C111.349 (13)C9—C81.355 (18)
C11—C71.439 (15)C9—H90.9300
C11—C121.445 (15)C5—C61.348 (18)
C16—C151.526 (15)C5—H50.9300
C14—O11.249 (13)C6—H60.9300
C14—C131.508 (16)C8—H80.9300
O6—Ho—O4i75.6 (2)N2—C11—C7123.8 (10)
O6—Ho—O5137.3 (3)N2—C11—C12117.6 (10)
O4i—Ho—O577.0 (2)C7—C11—C12118.6 (10)
O6—Ho—O181.4 (3)O3—C16—O4121.9 (10)
O4i—Ho—O186.8 (3)O3—C16—C15119.1 (10)
O5—Ho—O1128.9 (3)O4—C16—C15119.0 (10)
O6—Ho—O2127.4 (3)O1—C14—O2119.3 (11)
O4i—Ho—O276.8 (3)O1—C14—C13121.3 (11)
O5—Ho—O275.9 (3)O2—C14—C13119.1 (10)
O1—Ho—O253.2 (3)N1—C1—C2122.0 (10)
O6—Ho—O390.0 (3)N1—C1—H1119.0
O4i—Ho—O3125.2 (3)C2—C1—H1119.0
O5—Ho—O379.8 (3)C14—O1—Ho94.8 (7)
O1—Ho—O3143.7 (3)C16—C15—H15A109.5
O2—Ho—O3142.1 (3)C16—C15—H15B109.5
O6—Ho—N1139.6 (3)H15A—C15—H15B109.5
O4i—Ho—N1143.2 (3)C16—C15—H15C109.5
O5—Ho—N177.6 (3)H15A—C15—H15C109.5
O1—Ho—N188.8 (3)H15B—C15—H15C109.5
O2—Ho—N171.5 (3)N1—C12—C4122.7 (10)
O3—Ho—N175.2 (3)N1—C12—C11118.5 (9)
O6—Ho—O472.0 (2)C4—C12—C11118.5 (10)
O4i—Ho—O474.1 (3)C14—C13—H13A109.5
O5—Ho—O469.3 (2)C14—C13—H13B109.5
O1—Ho—O4150.3 (2)H13A—C13—H13B109.5
O2—Ho—O4138.5 (3)C14—C13—H13C109.5
O3—Ho—O451.3 (2)H13A—C13—H13C109.5
N1—Ho—O4120.1 (2)H13B—C13—H13C109.5
O6—Ho—N276.1 (2)C3—C4—C12118.0 (11)
O4i—Ho—N2148.6 (3)C3—C4—C5121.7 (11)
O5—Ho—N2134.1 (3)C12—C4—C5120.3 (11)
O1—Ho—N275.8 (3)C17—C18—H18A109.5
O2—Ho—N2111.0 (3)C17—C18—H18B109.5
O3—Ho—N267.9 (3)H18A—C18—H18B109.5
N1—Ho—N263.5 (3)C17—C18—H18C109.5
O4—Ho—N2109.4 (3)H18A—C18—H18C109.5
O6—Ho—Hoi69.44 (18)H18B—C18—H18C109.5
O4i—Ho—Hoi39.19 (18)C2—C3—C4118.1 (11)
O5—Ho—Hoi68.52 (18)C2—C3—H3120.9
O1—Ho—Hoi122.5 (2)C4—C3—H3120.9
O2—Ho—Hoi110.9 (2)C3—C2—C1120.7 (11)
O3—Ho—Hoi86.07 (18)C3—C2—H2119.7
N1—Ho—Hoi143.69 (19)C1—C2—H2119.7
O4—Ho—Hoi34.87 (14)N2—C10—C9124.8 (12)
N2—Ho—Hoi136.5 (2)N2—C10—H10117.6
C17—O5—Ho137.5 (6)C9—C10—H10117.6
C16—O4—Hoi161.3 (8)C8—C7—C6124.7 (11)
C16—O4—Ho90.0 (7)C8—C7—C11114.8 (11)
Hoi—O4—Ho105.9 (3)C6—C7—C11120.5 (11)
C12—N1—C1118.4 (9)C8—C9—C10118.0 (12)
C12—N1—Ho121.0 (7)C8—C9—H9121.0
C1—N1—Ho120.3 (7)C10—C9—H9121.0
C17i—O6—Ho135.9 (7)C6—C5—C4119.3 (12)
C16—O3—Ho95.9 (6)C6—C5—H5120.3
C14—O2—Ho92.6 (7)C4—C5—H5120.3
O5—C17—O6i126.5 (9)C5—C6—C7122.5 (12)
O5—C17—C18115.5 (9)C5—C6—H6118.7
O6i—C17—C18117.9 (10)C7—C6—H6118.7
C10—N2—C11116.5 (10)C9—C8—C7121.9 (11)
C10—N2—Ho124.8 (7)C9—C8—H8119.1
C11—N2—Ho118.3 (7)C7—C8—H8119.1
O6—Ho—O5—C1721.5 (11)O4i—Ho—N2—C1024.5 (13)
O4i—Ho—O5—C1729.7 (10)O5—Ho—N2—C10146.1 (9)
O1—Ho—O5—C17104.7 (10)O1—Ho—N2—C1082.8 (10)
O2—Ho—O5—C17109.1 (10)O2—Ho—N2—C10123.5 (10)
O3—Ho—O5—C17100.2 (10)O3—Ho—N2—C1097.4 (10)
N1—Ho—O5—C17177.2 (10)N1—Ho—N2—C10178.7 (11)
O4—Ho—O5—C1747.9 (10)O4—Ho—N2—C1066.5 (10)
N2—Ho—O5—C17145.3 (9)Hoi—Ho—N2—C1039.8 (11)
Hoi—Ho—O5—C1710.5 (9)O6—Ho—N2—C11171.5 (9)
O6—Ho—O4—C16110.2 (6)O4i—Ho—N2—C11162.4 (7)
O4i—Ho—O4—C16170.2 (7)O5—Ho—N2—C1127.0 (10)
O5—Ho—O4—C1688.4 (6)O1—Ho—N2—C11104.0 (9)
O1—Ho—O4—C16137.9 (6)O2—Ho—N2—C1163.4 (9)
O2—Ho—O4—C16123.2 (6)O3—Ho—N2—C1175.8 (8)
O3—Ho—O4—C165.1 (6)N1—Ho—N2—C118.2 (8)
N1—Ho—O4—C1627.3 (6)O4—Ho—N2—C11106.6 (8)
N2—Ho—O4—C1642.6 (6)Hoi—Ho—N2—C11133.3 (7)
Hoi—Ho—O4—C16170.2 (7)C10—N2—C11—C71.5 (18)
O6—Ho—O4—Hoi79.6 (3)Ho—N2—C11—C7172.2 (9)
O4i—Ho—O4—Hoi0.0C10—N2—C11—C12178.9 (11)
O5—Ho—O4—Hoi81.8 (3)Ho—N2—C11—C127.4 (14)
O1—Ho—O4—Hoi52.0 (6)Ho—O3—C16—O49.9 (10)
O2—Ho—O4—Hoi47.0 (4)Ho—O3—C16—C15172.3 (8)
O3—Ho—O4—Hoi175.3 (4)Hoi—O4—C16—O3158.6 (15)
N1—Ho—O4—Hoi142.8 (3)Ho—O4—C16—O39.4 (10)
N2—Ho—O4—Hoi147.2 (3)Hoi—O4—C16—C1524 (3)
O6—Ho—N1—C128.4 (10)Ho—O4—C16—C15172.8 (8)
O4i—Ho—N1—C12166.6 (7)Ho—O2—C14—O13.3 (11)
O5—Ho—N1—C12146.1 (8)Ho—O2—C14—C13171.4 (9)
O1—Ho—N1—C1283.5 (8)C12—N1—C1—C20.6 (17)
O2—Ho—N1—C12134.9 (9)Ho—N1—C1—C2174.2 (9)
O3—Ho—N1—C1263.5 (8)O2—C14—O1—Ho3.4 (11)
O4—Ho—N1—C1289.2 (8)C13—C14—O1—Ho171.2 (10)
N2—Ho—N1—C128.8 (8)O6—Ho—O1—C14149.8 (7)
Hoi—Ho—N1—C12124.8 (7)O4i—Ho—O1—C1473.9 (7)
O6—Ho—N1—C1177.0 (7)O5—Ho—O1—C143.4 (8)
O4i—Ho—N1—C118.7 (10)O2—Ho—O1—C141.9 (6)
O5—Ho—N1—C128.6 (8)O3—Ho—O1—C14132.2 (7)
O1—Ho—N1—C1101.8 (8)N1—Ho—O1—C1469.5 (7)
O2—Ho—N1—C150.5 (8)O4—Ho—O1—C14123.2 (7)
O3—Ho—N1—C1111.2 (8)N2—Ho—O1—C14132.5 (7)
O4—Ho—N1—C185.5 (8)Hoi—Ho—O1—C1490.9 (7)
N2—Ho—N1—C1176.5 (9)C1—N1—C12—C41.4 (17)
Hoi—Ho—N1—C149.8 (9)Ho—N1—C12—C4176.2 (8)
O4i—Ho—O6—C17i26.1 (10)C1—N1—C12—C11176.3 (10)
O5—Ho—O6—C17i25.5 (12)Ho—N1—C12—C119.0 (14)
O1—Ho—O6—C17i115.0 (10)N2—C11—C12—N10.7 (17)
O2—Ho—O6—C17i86.5 (10)C7—C11—C12—N1179.6 (11)
O3—Ho—O6—C17i100.4 (10)N2—C11—C12—C4175.8 (11)
N1—Ho—O6—C17i167.1 (9)C7—C11—C12—C44.5 (17)
O4—Ho—O6—C17i51.5 (10)N1—C12—C4—C32.3 (18)
N2—Ho—O6—C17i167.6 (10)C11—C12—C4—C3177.2 (11)
Hoi—Ho—O6—C17i14.6 (9)N1—C12—C4—C5177.8 (12)
O6—Ho—O3—C1672.0 (6)C11—C12—C4—C52.9 (18)
O4i—Ho—O3—C160.3 (7)C12—C4—C3—C21.1 (19)
O5—Ho—O3—C1666.3 (6)C5—C4—C3—C2179.0 (13)
O1—Ho—O3—C16147.3 (6)C4—C3—C2—C11 (2)
O2—Ho—O3—C16117.0 (7)N1—C1—C2—C32 (2)
N1—Ho—O3—C16146.0 (7)C11—N2—C10—C94 (2)
O4—Ho—O3—C165.2 (6)Ho—N2—C10—C9169.1 (11)
N2—Ho—O3—C16146.9 (7)N2—C11—C7—C81.9 (19)
Hoi—Ho—O3—C162.6 (6)C12—C11—C7—C8177.7 (12)
O6—Ho—O2—C1434.3 (8)N2—C11—C7—C6177.2 (12)
O4i—Ho—O2—C1494.1 (7)C12—C11—C7—C63.2 (19)
O5—Ho—O2—C14173.8 (7)N2—C10—C9—C83 (2)
O1—Ho—O2—C141.9 (6)C3—C4—C5—C6179.7 (14)
O3—Ho—O2—C14134.5 (7)C12—C4—C5—C60 (2)
N1—Ho—O2—C14104.8 (7)C4—C5—C6—C72 (2)
O4—Ho—O2—C14140.4 (6)C8—C7—C6—C5179.0 (15)
N2—Ho—O2—C1453.9 (7)C11—C7—C6—C50 (2)
Hoi—Ho—O2—C14113.8 (6)C10—C9—C8—C71 (2)
Ho—O5—C17—O6i4.9 (17)C6—C7—C8—C9176.1 (15)
Ho—O5—C17—C18175.5 (7)C11—C7—C8—C93 (2)
O6—Ho—N2—C101.6 (10)
Symmetry code: (i) x+2, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···O50.932.533.042 (14)115
C10—H10···O60.932.413.031 (14)124
C15—H15A···O2ii0.962.463.419 (14)174
Symmetry code: (ii) x, y1, z.
 

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