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The title compound, [Zn(C2H3O2)(phen)2]BF4, where phen is 1,10-phenanthroline (C12H8N2), crystallizes in the monoclinic space group P21/n. Zinc is in a general crystallographic position and is coordinated by one acetate and two phenanthroline ligands in an approximate mm2 point-group symmetry. The two Zn-O bond distances are similar to each other, as are the Zn-N bond distances.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804017477/cv6341sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804017477/cv6341Isup2.hkl
Contains datablock I

CCDC reference: 248750

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.050
  • wR factor = 0.116
  • Data-to-parameter ratio = 12.6

checkCIF/PLATON results

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Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Zn1 - O1 .. 10.14 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Zn1 - O2 .. 14.55 su
Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for O1 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C41 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for B PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 B F4
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 6 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 5 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

acetatobis(1,10-phenantroline)zinc(II) tetrafluorborate top
Crystal data top
[Zn(C2H3O2)(C12H8N2)2]BF4Dx = 1.542 Mg m3
Mr = 571.63Melting point: not measured K
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.2289 (5) ÅCell parameters from 5441 reflections
b = 19.2134 (11) Åθ = 1.0–27.5°
c = 15.6534 (5) ŵ = 1.06 mm1
β = 95.803 (3)°T = 293 K
V = 2462.2 (2) Å3Prism, colorless
Z = 40.13 × 0.1 × 0.08 mm
F(000) = 1160
Data collection top
Nonius KappaCCD
diffractometer
2440 reflections with I > 2σ(I)
Radiation source: fine focus sealed tube, noniusRint = 0.055
Horizonally mounted graphite crystal monochromatorθmax = 25°, θmin = 2.7°
Detector resolution: 9 pixels mm-1h = 99
CCD scansk = 2122
7832 measured reflectionsl = 1818
4329 independent reflections
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)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.116H atoms treated by a mixture of independent and constrained refinement
S = 0.94 w = 1/[σ2(Fo2) + (0.0543P)2]
where P = (Fo2 + 2Fc2)/3
4329 reflections(Δ/σ)max = 0.001
343 parametersΔρmax = 0.4 e Å3
0 restraintsΔρmin = 0.33 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
F11.1895 (4)0.04229 (19)0.20489 (18)0.1146 (11)
B1.3417 (9)0.0207 (3)0.1908 (4)0.0735 (17)
F41.4353 (4)0.01471 (19)0.26683 (17)0.1171 (11)
F31.4075 (4)0.07134 (19)0.1439 (2)0.1397 (14)
F21.3377 (5)0.03776 (19)0.1475 (2)0.1514 (15)
Zn10.93732 (6)0.16594 (2)0.32563 (2)0.04793 (19)
N30.8902 (4)0.09970 (18)0.21536 (18)0.0513 (9)
N21.0042 (4)0.23372 (17)0.43280 (17)0.0451 (8)
C410.6354 (5)0.1656 (2)0.3495 (2)0.0505 (10)
N11.0924 (4)0.10123 (17)0.40428 (17)0.0446 (8)
C91.0854 (4)0.1983 (2)0.4989 (2)0.0416 (9)
N41.0561 (4)0.21999 (17)0.23161 (17)0.0467 (8)
C51.1347 (4)0.1291 (2)0.4835 (2)0.0395 (9)
O20.6974 (4)0.21101 (16)0.30573 (16)0.0684 (9)
C110.9880 (5)0.3316 (2)0.5255 (3)0.0572 (11)
H110.95450.37730.53260.069*
C31.2739 (6)0.0247 (2)0.5303 (3)0.0660 (13)
H31.33460.00160.5720.079*
C291.0321 (5)0.1904 (2)0.1519 (2)0.0446 (10)
O10.7223 (4)0.12268 (16)0.39153 (18)0.0709 (9)
C250.9451 (5)0.1270 (2)0.1439 (2)0.0458 (10)
C271.0530 (6)0.1886 (3)0.0018 (2)0.0650 (13)
H271.08990.20880.05030.078*
C301.1729 (5)0.2853 (2)0.0912 (3)0.0625 (12)
H301.21160.30760.04460.075*
C321.1371 (5)0.2793 (2)0.2393 (2)0.0547 (11)
H321.15440.29940.29350.066*
C120.9587 (5)0.2983 (2)0.4462 (2)0.0534 (11)
H120.90440.32280.40070.064*
C71.2076 (5)0.1870 (3)0.6465 (2)0.0612 (12)
H71.22870.20560.70130.073*
C101.0670 (5)0.2956 (2)0.5923 (3)0.0604 (12)
H101.08620.31660.64590.072*
C81.1189 (5)0.2281 (2)0.5810 (2)0.0480 (10)
C281.0881 (5)0.2222 (2)0.0798 (2)0.0524 (11)
C240.9117 (5)0.0955 (2)0.0627 (2)0.0535 (11)
C21.2333 (6)0.0026 (2)0.4506 (3)0.0756 (14)
H21.26670.04730.43740.091*
C41.2253 (5)0.0913 (2)0.5494 (2)0.0506 (11)
C210.8047 (6)0.0416 (2)0.2082 (3)0.0656 (13)
H210.76860.02240.25740.079*
C11.1408 (5)0.0375 (2)0.3888 (3)0.0593 (12)
H11.11240.01850.33470.071*
C61.2608 (5)0.1231 (3)0.6316 (2)0.0629 (13)
H61.32180.0990.67530.075*
C260.9689 (6)0.1292 (3)0.0100 (2)0.0640 (13)
H260.9470.10940.06420.077*
C230.8205 (6)0.0347 (3)0.0575 (3)0.0654 (13)
H230.79670.01250.0050.079*
C311.1983 (5)0.3138 (2)0.1710 (3)0.0655 (13)
H311.25530.35540.17980.079*
C220.7659 (6)0.0077 (3)0.1301 (3)0.0740 (14)
H220.70370.03280.12740.089*
C420.4546 (5)0.1629 (3)0.3500 (3)0.0894 (17)
H42A0.42570.12370.38350.134*
H42B0.40440.15810.29220.134*
H42C0.41710.2050.37460.134*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
F10.083 (2)0.151 (3)0.111 (2)0.016 (2)0.0131 (17)0.028 (2)
B0.087 (5)0.073 (5)0.062 (4)0.001 (4)0.011 (3)0.005 (3)
F40.103 (2)0.158 (3)0.0840 (19)0.006 (2)0.0215 (17)0.0035 (19)
F30.146 (3)0.118 (3)0.166 (3)0.004 (3)0.069 (2)0.056 (3)
F20.196 (4)0.103 (3)0.149 (3)0.004 (3)0.014 (3)0.059 (2)
Zn10.0525 (3)0.0521 (3)0.0390 (3)0.0006 (3)0.00350 (19)0.0001 (2)
N30.058 (2)0.050 (2)0.0460 (19)0.003 (2)0.0079 (16)0.0005 (16)
N20.051 (2)0.042 (2)0.0428 (18)0.0001 (17)0.0057 (15)0.0027 (16)
C410.050 (3)0.054 (3)0.047 (2)0.001 (3)0.006 (2)0.006 (2)
N10.049 (2)0.042 (2)0.0428 (18)0.0008 (17)0.0072 (14)0.0051 (15)
C90.039 (2)0.044 (3)0.043 (2)0.004 (2)0.0089 (17)0.0021 (19)
N40.046 (2)0.049 (2)0.0445 (18)0.0031 (18)0.0053 (14)0.0020 (16)
C50.036 (2)0.043 (3)0.040 (2)0.005 (2)0.0046 (17)0.0016 (19)
O20.074 (2)0.075 (2)0.0556 (16)0.0100 (19)0.0034 (14)0.0174 (16)
C110.061 (3)0.038 (3)0.072 (3)0.003 (2)0.007 (2)0.014 (2)
C30.080 (3)0.054 (3)0.062 (3)0.009 (3)0.002 (2)0.017 (2)
C290.045 (3)0.048 (3)0.041 (2)0.003 (2)0.0063 (17)0.0018 (19)
O10.073 (2)0.059 (2)0.080 (2)0.0009 (18)0.0030 (16)0.0192 (17)
C250.046 (3)0.051 (3)0.041 (2)0.005 (2)0.0050 (18)0.003 (2)
C270.078 (4)0.076 (4)0.043 (2)0.008 (3)0.018 (2)0.004 (2)
C300.070 (3)0.063 (3)0.057 (3)0.004 (3)0.020 (2)0.010 (2)
C320.059 (3)0.051 (3)0.054 (2)0.000 (2)0.006 (2)0.005 (2)
C120.061 (3)0.043 (3)0.055 (3)0.000 (2)0.0008 (19)0.001 (2)
C70.071 (3)0.068 (4)0.042 (2)0.006 (3)0.007 (2)0.002 (2)
C100.063 (3)0.062 (3)0.055 (3)0.012 (3)0.002 (2)0.012 (2)
C80.050 (3)0.047 (3)0.046 (2)0.004 (2)0.0007 (18)0.005 (2)
C280.054 (3)0.056 (3)0.049 (2)0.002 (2)0.0139 (19)0.002 (2)
C240.056 (3)0.057 (3)0.047 (2)0.002 (2)0.0032 (19)0.010 (2)
C20.101 (4)0.046 (3)0.080 (3)0.020 (3)0.012 (3)0.002 (3)
C40.055 (3)0.045 (3)0.051 (3)0.001 (2)0.003 (2)0.006 (2)
C210.081 (4)0.057 (3)0.060 (3)0.018 (3)0.013 (2)0.000 (2)
C10.072 (3)0.046 (3)0.060 (3)0.004 (3)0.011 (2)0.007 (2)
C60.067 (3)0.072 (4)0.047 (3)0.003 (3)0.009 (2)0.010 (2)
C260.075 (3)0.080 (4)0.038 (2)0.008 (3)0.010 (2)0.008 (2)
C230.072 (3)0.073 (4)0.051 (3)0.002 (3)0.002 (2)0.022 (2)
C310.077 (4)0.054 (3)0.067 (3)0.015 (3)0.014 (2)0.006 (2)
C220.087 (4)0.063 (3)0.072 (3)0.017 (3)0.009 (3)0.018 (3)
C420.048 (3)0.108 (5)0.113 (4)0.005 (3)0.015 (3)0.003 (3)
Geometric parameters (Å, º) top
F1—B1.359 (6)C27—C261.334 (6)
B—F21.311 (6)C27—C281.434 (5)
B—F41.356 (6)C30—C311.360 (5)
B—F31.363 (6)C30—C281.401 (5)
Zn1—O12.293 (3)C32—C311.393 (5)
Zn1—O22.149 (3)C7—C61.331 (6)
Zn1—N12.091 (3)C7—C81.433 (5)
Zn1—N22.151 (3)C10—C81.383 (6)
Zn1—N32.148 (3)C24—C231.386 (6)
Zn1—N42.119 (3)C24—C261.430 (5)
Zn1—C412.550 (4)C2—C11.401 (6)
N3—C211.319 (5)C4—C61.428 (5)
N3—C251.354 (4)C21—C221.394 (5)
N2—C121.319 (5)C23—C221.365 (5)
N2—C91.356 (4)C3—H30.9300
C41—O11.237 (5)C27—H270.9300
C41—O21.250 (5)C30—H300.9300
C41—C421.489 (6)C32—H320.9300
N1—C11.317 (5)C12—H120.9300
N1—C51.364 (4)C7—H70.9300
C9—C81.408 (5)C10—H100.9300
C9—C51.419 (5)C2—H20.9300
N4—C321.320 (5)C21—H210.9300
N4—C291.367 (4)C1—H10.9300
C5—C41.411 (5)C6—H60.9300
C11—C101.363 (5)C26—H260.9300
C11—C121.396 (5)C23—H230.9300
C3—C21.364 (5)C31—H310.9300
C3—C41.383 (5)C22—H220.9300
C29—C281.402 (5)C42—H42A0.9600
C29—C251.411 (5)C42—H42B0.9600
C25—C241.410 (5)C42—H42C0.9600
F2—B—F4111.3 (5)N4—C32—C31124.0 (4)
F2—B—F1111.7 (6)N2—C12—C11123.2 (4)
F4—B—F1109.5 (4)C6—C7—C8122.4 (4)
F2—B—F3108.9 (5)C11—C10—C8120.5 (4)
F4—B—F3108.2 (5)C10—C8—C9117.6 (4)
F1—B—F3107.0 (5)C10—C8—C7124.5 (4)
N1—Zn1—O188.41 (11)C9—C8—C7117.9 (4)
N1—Zn1—O2145.25 (11)C30—C28—C29118.3 (4)
N1—Zn1—N278.94 (12)C30—C28—C27123.8 (4)
N1—Zn1—N399.82 (12)C29—C28—C27117.9 (4)
N1—Zn1—N4113.81 (12)C23—C24—C25118.0 (4)
N2—Zn1—O190.95 (11)C23—C24—C26123.7 (4)
N2—Zn1—O291.59 (11)C25—C24—C26118.2 (4)
N2—Zn1—N3175.29 (12)C3—C2—C1119.0 (4)
N2—Zn1—N498.37 (12)C3—C4—C5117.4 (4)
N3—Zn1—O193.56 (11)C3—C4—C6123.7 (4)
N3—Zn1—O291.95 (11)C5—C4—C6118.9 (4)
N3—Zn1—N477.92 (12)N3—C21—C22122.9 (4)
N4—Zn1—O1157.13 (11)N1—C1—C2122.6 (4)
N4—Zn1—O2100.56 (11)C7—C6—C4120.8 (4)
O1—Zn1—O258.12 (11)C27—C26—C24121.3 (4)
N1—Zn1—C41117.24 (13)C22—C23—C24119.6 (4)
N4—Zn1—C41128.88 (13)C30—C31—C32118.6 (4)
N3—Zn1—C4190.98 (12)C23—C22—C21119.1 (4)
O2—Zn1—C4129.29 (11)C10—C11—H11120.8
N2—Zn1—C4193.63 (12)C12—C11—H11120.8
O1—Zn1—C4128.97 (11)C2—C3—H3119.8
C21—N3—C25118.5 (3)C4—C3—H3119.8
C21—N3—Zn1128.4 (3)C26—C27—H27119.1
C25—N3—Zn1112.7 (3)C28—C27—H27119.1
C12—N2—C9118.4 (3)C31—C30—H30120.2
C12—N2—Zn1129.8 (3)C28—C30—H30120.2
C9—N2—Zn1111.0 (3)N4—C32—H32118.0
O1—C41—O2120.7 (4)C31—C32—H32118.0
O1—C41—C42119.9 (4)N2—C12—H12118.4
O2—C41—C42119.4 (4)C11—C12—H12118.4
O1—C41—Zn163.9 (2)C6—C7—H7118.8
O2—C41—Zn157.3 (2)C8—C7—H7118.8
C42—C41—Zn1171.7 (3)C11—C10—H10119.8
C1—N1—C5118.6 (3)C8—C10—H10119.8
C1—N1—Zn1128.5 (3)C3—C2—H2120.5
C5—N1—Zn1112.8 (3)C1—C2—H2120.5
N2—C9—C8121.9 (4)N3—C21—H21118.5
N2—C9—C5117.9 (3)C22—C21—H21118.5
C8—C9—C5120.1 (3)N1—C1—H1118.7
C32—N4—C29117.8 (3)C2—C1—H1118.7
C32—N4—Zn1128.6 (3)C7—C6—H6119.6
C29—N4—Zn1113.3 (3)C4—C6—H6119.6
N1—C5—C4122.0 (4)C27—C26—H26119.3
N1—C5—C9118.1 (3)C24—C26—H26119.3
C4—C5—C9119.9 (3)C22—C23—H23120.2
C41—O2—Zn193.4 (3)C24—C23—H23120.2
C10—C11—C12118.4 (4)C30—C31—H31120.7
C2—C3—C4120.3 (4)C32—C31—H31120.7
N4—C29—C28121.6 (4)C23—C22—H22120.5
N4—C29—C25117.7 (3)C21—C22—H22120.5
C28—C29—C25120.6 (3)C41—C42—H42A109.5
C41—O1—Zn187.1 (2)C41—C42—H42B109.5
N3—C25—C24121.8 (4)H42A—C42—H42B109.5
N3—C25—C29118.0 (3)C41—C42—H42C109.5
C24—C25—C29120.1 (3)H42A—C42—H42C109.5
C26—C27—C28121.8 (4)H42B—C42—H42C109.5
C31—C30—C28119.6 (4)
Comparative bond lengths (Å) for [Zn(ac)(phen)2]Y complexes top
Zn—N1Zn—N2Zn—N3Zn—N4Zn—O1Zn—O2
[[Zn(ac)(phen)2]BF4a2.091 (3)2.151 (3)2.148 (3)2.119 (3)2.293 (3)2.149 (3)
[Zn(ac)(phen)2]BF4.2H2Ob2.116 (2)2.147 (2)2.147 (2)2.116 (2)2.184 (2)2.184 (2)
[Zn(ac)(phen)2]ClO4c2.135 (6)2.143 (6)2.160 (5)2.100 (5)2.296 (5)2.156 (5)
Notes: (a) this work; (b) Fitzgerald et al. (1985); (c) Chen et al. (1994).
Comparative bond angles (°) for [Zn(ac)(phen)2]Y complexes top
N1—Zn—N2N3—Zn—N4O1—Zn—O2
[Zn(ac)(phen)2]BF4a78.94 (12)77.92 (12)58.12 (11)
[Zn(ac)(phen)2]BF4.2H2Ob78.4778.4757.2
[Zn(ac)(phen)2]ClO4c78.1 (2)78.6 (2)57.8 (2)
Notes: (a) this work; (b) Fitzgerald et al. (1985); (c) Chen et al. (1994).
 

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