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The crystal structure of the title compound, [Zn(C12H8N2)2(H2O)2][NbF5O], consists of ZnII complex cations and NbV complex anions. The ZnII and NbV atoms each have a distorted octa­hedral coordination geometry. The Nb—F bond in the trans position with respect to the Nb=O bond is significantly longer than the other four Nb—F bonds in the same [NbOF5]2− anion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805020854/xu6024sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805020854/xu6024Isup2.hkl
Contains datablock I

CCDC reference: 282706

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.036
  • wR factor = 0.100
  • Data-to-parameter ratio = 13.6

checkCIF/PLATON results

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Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.01 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Nb1 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.59 PLAT432_ALERT_2_C Short Inter X...Y Contact O3 .. C10 .. 2.93 Ang.
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

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SMART; data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1995); software used to prepare material for publication: SHELXTL.

Diaquabis(1,10-phenanthroline-κ2N,N')zinc(II) pentafluorooxoniobate top
Crystal data top
[Zn(C12H8N2)2(H2O)2][NbF5O]Z = 2
Mr = 665.72F(000) = 664
Triclinic, P1Dx = 1.762 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.4833 (2) ÅCell parameters from 2965 reflections
b = 11.1136 (3) Åθ = 2.9–25.7°
c = 13.0749 (3) ŵ = 1.48 mm1
α = 73.486 (2)°T = 273 K
β = 72.134 (2)°Block, colorless
γ = 81.704 (2)°0.12 × 0.10 × 0.08 mm
V = 1254.99 (5) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
4843 independent reflections
Radiation source: fine-focus sealed tube3773 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
φ and ω scansθmax = 26.0°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 1111
Tmin = 0.806, Tmax = 0.875k = 1113
9091 measured reflectionsl = 1616
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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.100H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0527P)2 + 0.3561P]
where P = (Fo2 + 2Fc2)/3
4843 reflections(Δ/σ)max < 0.001
355 parametersΔρmax = 0.69 e Å3
4 restraintsΔρmin = 0.65 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
Nb10.62098 (4)0.26945 (3)0.31147 (3)0.04476 (12)
Zn10.69787 (4)0.77933 (3)0.27789 (3)0.03709 (12)
N10.6243 (3)0.7492 (3)0.1480 (2)0.0452 (7)
N20.7792 (3)0.9386 (3)0.1392 (2)0.0457 (7)
N30.8178 (3)0.8088 (3)0.3831 (2)0.0419 (7)
N40.8909 (3)0.6457 (3)0.2533 (2)0.0439 (7)
O10.5782 (3)0.6340 (2)0.3993 (2)0.0531 (7)
O20.5136 (3)0.8987 (2)0.3298 (2)0.0450 (6)
O30.5793 (3)0.1361 (2)0.2773 (3)0.0634 (8)
F10.4207 (4)0.3234 (4)0.3624 (6)0.204 (3)
F20.6386 (6)0.3794 (3)0.1718 (3)0.155 (2)
F30.8295 (3)0.2331 (3)0.2746 (3)0.1023 (11)
F40.6236 (5)0.1728 (3)0.4601 (2)0.1254 (15)
F50.6463 (4)0.4138 (2)0.3673 (3)0.0995 (10)
C10.5483 (5)0.6550 (4)0.1538 (4)0.0592 (10)
H1A0.52410.59260.21990.071*
C20.5033 (6)0.6460 (5)0.0643 (4)0.0770 (14)
H2A0.44970.57880.07140.092*
C30.5376 (6)0.7348 (6)0.0323 (4)0.0839 (17)
H30.50870.72890.09250.101*
C40.6176 (5)0.8370 (5)0.0419 (3)0.0656 (12)
C50.6542 (6)0.9379 (7)0.1392 (4)0.0937 (19)
H50.62970.93550.20230.112*
C60.7232 (6)1.0364 (6)0.1419 (4)0.0935 (19)
H60.74261.10230.20580.112*
C70.7678 (5)1.0420 (5)0.0478 (3)0.0671 (12)
C80.8391 (6)1.1418 (5)0.0443 (4)0.0828 (16)
H80.85861.21110.10530.099*
C90.8801 (5)1.1387 (4)0.0468 (4)0.0738 (14)
H90.92811.20500.04870.089*
C100.8491 (4)1.0341 (4)0.1383 (3)0.0566 (10)
H100.87851.03150.20050.068*
C110.7390 (4)0.9424 (4)0.0479 (3)0.0483 (9)
C120.6590 (4)0.8396 (4)0.0522 (3)0.0481 (9)
C130.7788 (5)0.8871 (4)0.4485 (3)0.0554 (10)
H130.69490.94150.44600.066*
C140.8585 (5)0.8910 (4)0.5205 (4)0.0671 (12)
H140.82810.94750.56480.080*
C150.9815 (5)0.8117 (4)0.5260 (4)0.0675 (12)
H151.03500.81320.57450.081*
C161.0265 (4)0.7282 (4)0.4582 (3)0.0556 (10)
C171.1526 (5)0.6419 (5)0.4584 (4)0.0744 (13)
H171.21050.64100.50460.089*
C181.1895 (5)0.5621 (5)0.3938 (4)0.0763 (14)
H181.27300.50710.39580.092*
C191.1040 (4)0.5587 (4)0.3211 (4)0.0579 (10)
C201.1351 (5)0.4756 (4)0.2534 (4)0.0751 (13)
H201.21730.41870.25230.090*
C211.0462 (5)0.4776 (4)0.1894 (4)0.0756 (13)
H211.06650.42190.14470.091*
C220.9236 (5)0.5640 (4)0.1911 (4)0.0597 (10)
H220.86260.56440.14720.072*
C230.9786 (4)0.6438 (3)0.3182 (3)0.0430 (8)
C240.9396 (4)0.7295 (3)0.3873 (3)0.0430 (8)
H1B0.544 (5)0.634 (5)0.4655 (19)0.080*
H2B0.480 (5)0.873 (4)0.3992 (17)0.080*
H1C0.604 (5)0.557 (2)0.398 (4)0.080*
H2C0.530 (5)0.975 (2)0.312 (4)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0586 (2)0.03399 (19)0.04360 (19)0.00335 (15)0.01806 (16)0.01191 (14)
Zn10.0466 (2)0.0311 (2)0.0370 (2)0.00040 (17)0.01839 (17)0.00805 (16)
N10.0560 (18)0.0429 (17)0.0433 (16)0.0081 (14)0.0238 (14)0.0160 (13)
N20.0496 (18)0.0356 (16)0.0429 (16)0.0060 (14)0.0042 (13)0.0098 (13)
N30.0476 (17)0.0360 (15)0.0471 (16)0.0021 (13)0.0228 (13)0.0084 (13)
N40.0475 (17)0.0357 (15)0.0476 (16)0.0012 (13)0.0132 (13)0.0110 (13)
O10.0746 (19)0.0326 (13)0.0456 (14)0.0060 (13)0.0064 (13)0.0098 (12)
O20.0575 (15)0.0326 (13)0.0422 (13)0.0029 (12)0.0154 (12)0.0062 (11)
O30.0674 (18)0.0345 (14)0.103 (2)0.0016 (13)0.0395 (16)0.0244 (14)
F10.066 (2)0.110 (3)0.426 (9)0.036 (2)0.027 (3)0.119 (4)
F20.367 (7)0.0501 (17)0.077 (2)0.017 (3)0.116 (3)0.0015 (14)
F30.0612 (17)0.118 (3)0.147 (3)0.0120 (17)0.0143 (17)0.078 (2)
F40.230 (4)0.0628 (18)0.0427 (14)0.023 (2)0.006 (2)0.0012 (13)
F50.176 (3)0.0502 (15)0.108 (2)0.0191 (17)0.084 (2)0.0412 (15)
C10.075 (3)0.048 (2)0.070 (3)0.003 (2)0.038 (2)0.023 (2)
C20.083 (3)0.087 (4)0.092 (4)0.007 (3)0.050 (3)0.049 (3)
C30.081 (3)0.123 (5)0.074 (3)0.030 (3)0.049 (3)0.055 (3)
C40.059 (3)0.095 (3)0.043 (2)0.027 (2)0.0258 (19)0.020 (2)
C50.083 (4)0.146 (6)0.043 (3)0.027 (4)0.033 (2)0.010 (3)
C60.085 (4)0.119 (5)0.043 (3)0.025 (4)0.016 (2)0.016 (3)
C70.054 (2)0.069 (3)0.050 (2)0.015 (2)0.0031 (19)0.008 (2)
C80.070 (3)0.061 (3)0.067 (3)0.012 (3)0.015 (3)0.016 (2)
C90.062 (3)0.044 (2)0.087 (4)0.005 (2)0.016 (3)0.011 (2)
C100.055 (2)0.042 (2)0.061 (2)0.0037 (18)0.0036 (19)0.0164 (19)
C110.045 (2)0.049 (2)0.0383 (18)0.0140 (17)0.0074 (15)0.0052 (16)
C120.045 (2)0.057 (2)0.0408 (19)0.0181 (18)0.0181 (16)0.0139 (17)
C130.066 (3)0.046 (2)0.067 (2)0.0014 (19)0.032 (2)0.0208 (19)
C140.088 (3)0.060 (3)0.073 (3)0.006 (2)0.041 (3)0.026 (2)
C150.076 (3)0.071 (3)0.071 (3)0.014 (3)0.044 (2)0.012 (2)
C160.053 (2)0.055 (2)0.062 (2)0.0078 (19)0.0316 (19)0.0008 (19)
C170.060 (3)0.081 (3)0.087 (3)0.001 (3)0.044 (3)0.004 (3)
C180.051 (3)0.074 (3)0.095 (4)0.014 (2)0.034 (2)0.001 (3)
C190.049 (2)0.046 (2)0.069 (3)0.0041 (18)0.0154 (19)0.004 (2)
C200.059 (3)0.059 (3)0.094 (4)0.016 (2)0.013 (3)0.015 (3)
C210.073 (3)0.059 (3)0.092 (4)0.010 (2)0.011 (3)0.036 (3)
C220.059 (3)0.047 (2)0.074 (3)0.001 (2)0.017 (2)0.021 (2)
C230.0381 (18)0.0354 (18)0.0495 (19)0.0011 (15)0.0137 (15)0.0002 (15)
C240.047 (2)0.0345 (18)0.0452 (19)0.0053 (16)0.0195 (16)0.0022 (15)
Geometric parameters (Å, º) top
Nb1—O31.790 (2)C5—C61.341 (8)
Nb1—F21.860 (3)C5—H50.9300
Nb1—F11.879 (3)C6—C71.437 (7)
Nb1—F31.897 (3)C6—H60.9300
Nb1—F41.940 (3)C7—C81.397 (7)
Nb1—F52.012 (2)C7—C111.399 (5)
Zn1—O12.094 (3)C8—C91.351 (7)
Zn1—O22.095 (3)C8—H80.9300
Zn1—N12.144 (3)C9—C101.400 (6)
Zn1—N22.174 (3)C9—H90.9300
Zn1—N32.149 (3)C10—H100.9300
Zn1—N42.188 (3)C11—C121.439 (5)
N1—C11.328 (5)C13—C141.389 (5)
N1—C121.347 (4)C13—H130.9300
N2—C101.325 (5)C14—C151.364 (6)
N2—C111.349 (5)C14—H140.9300
N3—C131.327 (4)C15—C161.397 (6)
N3—C241.354 (4)C15—H150.9300
N4—C221.329 (5)C16—C241.412 (5)
N4—C231.353 (4)C16—C171.421 (6)
O1—H1B0.826 (19)C17—C181.333 (7)
O1—H1C0.861 (19)C17—H170.9300
O2—H2B0.841 (19)C18—C191.436 (6)
O2—H2C0.841 (19)C18—H180.9300
C1—C21.395 (5)C19—C201.396 (6)
C1—H1A0.9300C19—C231.412 (5)
C2—C31.344 (7)C20—C211.352 (7)
C2—H2A0.9300C20—H200.9300
C3—C41.411 (7)C21—C221.396 (6)
C3—H30.9300C21—H210.9300
C4—C121.411 (5)C22—H220.9300
C4—C51.424 (7)C23—C241.430 (5)
O3—Nb1—F296.11 (14)C6—C5—C4121.3 (5)
O3—Nb1—F194.11 (17)C6—C5—H5119.3
F2—Nb1—F191.7 (3)C4—C5—H5119.3
O3—Nb1—F395.51 (13)C5—C6—C7121.3 (5)
F2—Nb1—F390.6 (2)C5—C6—H6119.4
F1—Nb1—F3169.83 (19)C7—C6—H6119.4
O3—Nb1—F492.47 (14)C8—C7—C11116.4 (4)
F2—Nb1—F4170.58 (17)C8—C7—C6124.5 (5)
F1—Nb1—F491.6 (2)C11—C7—C6119.1 (5)
F3—Nb1—F484.71 (17)C9—C8—C7120.8 (4)
O3—Nb1—F5172.76 (14)C9—C8—H8119.6
F2—Nb1—F588.89 (12)C7—C8—H8119.6
F1—Nb1—F580.49 (18)C8—C9—C10119.0 (5)
F3—Nb1—F589.64 (13)C8—C9—H9120.5
F4—Nb1—F582.94 (13)C10—C9—H9120.5
O1—Zn1—O285.98 (10)N2—C10—C9122.3 (4)
O1—Zn1—N193.40 (11)N2—C10—H10118.9
O2—Zn1—N194.69 (10)C9—C10—H10118.9
O1—Zn1—N394.65 (11)N2—C11—C7123.2 (4)
O2—Zn1—N395.13 (10)N2—C11—C12117.3 (3)
N1—Zn1—N3167.71 (12)C7—C11—C12119.5 (4)
O1—Zn1—N2167.53 (11)N1—C12—C4122.1 (4)
O2—Zn1—N286.72 (10)N1—C12—C11118.1 (3)
N1—Zn1—N277.13 (11)C4—C12—C11119.8 (4)
N3—Zn1—N296.07 (11)N3—C13—C14122.5 (4)
O1—Zn1—N488.65 (11)N3—C13—H13118.7
O2—Zn1—N4170.22 (10)C14—C13—H13118.7
N1—Zn1—N493.78 (11)C15—C14—C13119.8 (4)
N3—Zn1—N477.15 (11)C15—C14—H14120.1
N2—Zn1—N499.94 (11)C13—C14—H14120.1
C1—N1—C12118.7 (3)C14—C15—C16119.4 (4)
C1—N1—Zn1127.3 (3)C14—C15—H15120.3
C12—N1—Zn1114.0 (2)C16—C15—H15120.3
C10—N2—C11118.4 (3)C15—C16—C24117.5 (4)
C10—N2—Zn1128.0 (3)C15—C16—C17123.4 (4)
C11—N2—Zn1113.3 (2)C24—C16—C17119.1 (4)
C13—N3—C24118.5 (3)C18—C17—C16121.3 (4)
C13—N3—Zn1127.3 (2)C18—C17—H17119.4
C24—N3—Zn1113.9 (2)C16—C17—H17119.4
C22—N4—C23118.7 (3)C17—C18—C19121.9 (4)
C22—N4—Zn1128.5 (3)C17—C18—H18119.1
C23—N4—Zn1112.6 (2)C19—C18—H18119.1
Zn1—O1—H1B124 (3)C20—C19—C23117.2 (4)
Zn1—O1—H1C120 (3)C20—C19—C18124.5 (4)
H1B—O1—H1C107 (4)C23—C19—C18118.3 (4)
Zn1—O2—H2B108 (3)C21—C20—C19120.3 (4)
Zn1—O2—H2C115 (3)C21—C20—H20119.8
H2B—O2—H2C110 (4)C19—C20—H20119.8
N1—C1—C2122.5 (4)C20—C21—C22119.4 (4)
N1—C1—H1A118.8C20—C21—H21120.3
C2—C1—H1A118.8C22—C21—H21120.3
C3—C2—C1119.8 (5)N4—C22—C21122.3 (4)
C3—C2—H2A120.1N4—C22—H22118.9
C1—C2—H2A120.1C21—C22—H22118.9
C2—C3—C4119.6 (4)N4—C23—C19122.1 (3)
C2—C3—H3120.2N4—C23—C24118.2 (3)
C4—C3—H3120.2C19—C23—C24119.7 (3)
C12—C4—C3117.3 (4)N3—C24—C16122.2 (3)
C12—C4—C5118.9 (5)N3—C24—C23118.0 (3)
C3—C4—C5123.7 (4)C16—C24—C23119.8 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···F5i0.83 (3)2.35 (3)3.090 (4)150 (5)
O1—H1C···F50.86 (3)1.71 (3)2.558 (3)167 (5)
O2—H2B···F4i0.84 (2)1.76 (2)2.595 (4)169 (5)
O2—H2C···O3ii0.84 (3)1.81 (3)2.646 (3)175 (4)
C17—H17···F5iii0.932.373.277 (6)166
C18—H18···F1iv0.932.373.225 (7)152
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z; (iii) x+2, y+1, z+1; (iv) x+1, y, z.
 

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