Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805030394/rn6066sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805030394/rn6066Isup2.hkl |
CCDC reference: 287695
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.009 Å
- R factor = 0.034
- wR factor = 0.092
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT048_ALERT_1_C MoietyFormula Not Given ........................ ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Nb1 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.847(19) ...... 2.11 su-Rat O1 -H25 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 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 3 ALERT type 4 Improvement, methodology, query or suggestion
All reagents were of analytical grade from commercial sources and used without further purification. Nb2O5 (0.133 g, 0.5 mmol) was first dissolved in HF solution (1 ml, 42 wt% in H2O) at 383 K for 2 h in a Teflon-lined stainless steel vessel. After being cooled to room temperature, 3 CdSO4·8H2O (0.257 g, 0.33 mmol), phen (0.496 g, 2.5 mmol) and H2O (15 ml) were added to the above solution. The pH of the mixture was adjusted to about 6 usingy KOH solution. The mixture was then heated under autogenous hydrothermal conditions at 413 K for 3 d. The mixture was filtered, then the solution was allowed to evaporate slowly. After five d, colorless single crystals suitable for X-ray diffraction were obtained. The crystals were dried in air. Elemental analysis: found: C, 40.31%; H, 2.78%; N, 7.87%; calc. for C24H20CdF5N4NbO3: C, 40.34%;H, 2.82%;N, 7.85%.
The water H atoms were located in a different Fourier map and refined with the O—H bond length restrained to 0.85 (2) Å, and assigned fixed isotropic displacement parameters of 0.080 Å2. Other H atoms were placed at calculated positions and refined as riding, with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXTL (Siemens, 1995).
[Cd(C12H8N2)2(H2O)2]2+·[NbOF5]2− | Z = 2 |
Mr = 712.75 | F(000) = 700 |
Triclinic, P1 | Dx = 1.850 Mg m−3 |
a = 9.487 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.537 (5) Å | Cell parameters from 2883 reflections |
c = 13.007 (5) Å | θ = 2.2–27.2° |
α = 99.162 (6)° | µ = 1.35 mm−1 |
β = 109.646 (6)° | T = 298 K |
γ = 100.661 (5)° | Block, colorless |
V = 1279.3 (9) Å3 | 0.35 × 0.33 × 0.29 mm |
Bruker SMART CCD area-detector diffractometer | 4464 independent reflections |
Radiation source: fine-focus sealed tube | 3413 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
ϕ and w scans | θmax = 25.0°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | h = −11→11 |
Tmin = 0.650, Tmax = 0.696 | k = −13→13 |
6750 measured reflections | l = −15→12 |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0456P)2 + 1.0033P] where P = (Fo2 + 2Fc2)/3 |
4464 reflections | (Δ/σ)max = 0.001 |
355 parameters | Δρmax = 0.50 e Å−3 |
6 restraints | Δρmin = −0.79 e Å−3 |
[Cd(C12H8N2)2(H2O)2]2+·[NbOF5]2− | γ = 100.661 (5)° |
Mr = 712.75 | V = 1279.3 (9) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.487 (4) Å | Mo Kα radiation |
b = 11.537 (5) Å | µ = 1.35 mm−1 |
c = 13.007 (5) Å | T = 298 K |
α = 99.162 (6)° | 0.35 × 0.33 × 0.29 mm |
β = 109.646 (6)° |
Bruker SMART CCD area-detector diffractometer | 4464 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | 3413 reflections with I > 2σ(I) |
Tmin = 0.650, Tmax = 0.696 | Rint = 0.016 |
6750 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | 6 restraints |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Δρmax = 0.50 e Å−3 |
4464 reflections | Δρmin = −0.79 e Å−3 |
355 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Nb1 | 0.56044 (5) | 0.26190 (4) | 0.68194 (4) | 0.04562 (14) | |
Cd1 | 0.48108 (4) | 0.22250 (3) | 0.26707 (3) | 0.04084 (12) | |
F1 | 0.3689 (3) | 0.1749 (3) | 0.5529 (3) | 0.0645 (8) | |
F2 | 0.6539 (4) | 0.2892 (3) | 0.5737 (3) | 0.0877 (11) | |
F3 | 0.7403 (4) | 0.3686 (3) | 0.7989 (3) | 0.0948 (13) | |
F4 | 0.4467 (5) | 0.2584 (4) | 0.7758 (3) | 0.0957 (13) | |
F5 | 0.4931 (4) | 0.4141 (3) | 0.6460 (3) | 0.0840 (11) | |
N1 | 0.7174 (4) | 0.1902 (3) | 0.3678 (3) | 0.0432 (9) | |
N2 | 0.6781 (4) | 0.3698 (3) | 0.2523 (3) | 0.0459 (9) | |
N3 | 0.2769 (4) | 0.2571 (3) | 0.1263 (3) | 0.0480 (10) | |
N4 | 0.3873 (5) | 0.0544 (3) | 0.1105 (3) | 0.0444 (9) | |
O1 | 0.3448 (4) | 0.0971 (3) | 0.3408 (3) | 0.0493 (8) | |
O2 | 0.4641 (5) | 0.3733 (3) | 0.3952 (3) | 0.0556 (9) | |
O3 | 0.6210 (4) | 0.1283 (3) | 0.7002 (3) | 0.0592 (9) | |
C1 | 0.7350 (6) | 0.1069 (4) | 0.4266 (5) | 0.0564 (14) | |
H1 | 0.6480 | 0.0482 | 0.4188 | 0.068* | |
C2 | 0.8802 (6) | 0.1041 (5) | 0.5003 (5) | 0.0639 (15) | |
H2 | 0.8887 | 0.0456 | 0.5420 | 0.077* | |
C3 | 1.0069 (6) | 0.1863 (5) | 0.5104 (5) | 0.0648 (15) | |
H3 | 1.1038 | 0.1838 | 0.5583 | 0.078* | |
C4 | 0.9938 (5) | 0.2763 (5) | 0.4488 (5) | 0.0531 (13) | |
C5 | 0.8436 (5) | 0.2750 (4) | 0.3782 (4) | 0.0397 (10) | |
C6 | 0.8245 (5) | 0.3694 (4) | 0.3180 (4) | 0.0420 (11) | |
C7 | 0.9554 (6) | 0.4562 (5) | 0.3268 (5) | 0.0560 (13) | |
C8 | 0.9319 (8) | 0.5483 (6) | 0.2685 (6) | 0.0763 (18) | |
H8 | 1.0155 | 0.6083 | 0.2730 | 0.092* | |
C9 | 0.7860 (8) | 0.5479 (6) | 0.2063 (6) | 0.082 (2) | |
H9 | 0.7689 | 0.6086 | 0.1678 | 0.099* | |
C10 | 0.6600 (7) | 0.4574 (5) | 0.1987 (5) | 0.0632 (15) | |
H10 | 0.5606 | 0.4590 | 0.1546 | 0.076* | |
C11 | 1.1230 (6) | 0.3651 (5) | 0.4559 (5) | 0.0683 (16) | |
H11 | 1.2220 | 0.3641 | 0.5013 | 0.082* | |
C12 | 1.1044 (6) | 0.4513 (5) | 0.3974 (5) | 0.0700 (16) | |
H12 | 1.1912 | 0.5090 | 0.4033 | 0.084* | |
C13 | 0.2209 (6) | 0.3548 (5) | 0.1342 (5) | 0.0646 (15) | |
H13 | 0.2715 | 0.4178 | 0.1984 | 0.078* | |
C14 | 0.0918 (7) | 0.3664 (6) | 0.0519 (5) | 0.0732 (17) | |
H14 | 0.0559 | 0.4356 | 0.0611 | 0.088* | |
C15 | 0.0179 (6) | 0.2771 (7) | −0.0421 (5) | 0.0744 (19) | |
H15 | −0.0692 | 0.2847 | −0.0981 | 0.089* | |
C16 | 0.0711 (6) | 0.1723 (6) | −0.0564 (4) | 0.0584 (14) | |
C17 | 0.2041 (5) | 0.1665 (4) | 0.0323 (4) | 0.0450 (11) | |
C18 | 0.2603 (5) | 0.0591 (4) | 0.0244 (4) | 0.0455 (11) | |
C19 | 0.1809 (7) | −0.0387 (5) | −0.0701 (4) | 0.0601 (15) | |
C20 | 0.2364 (9) | −0.1435 (6) | −0.0713 (6) | 0.0789 (19) | |
H20 | 0.1865 | −0.2108 | −0.1318 | 0.095* | |
C21 | 0.3626 (9) | −0.1461 (5) | 0.0158 (6) | 0.0759 (19) | |
H21 | 0.3993 | −0.2154 | 0.0154 | 0.091* | |
C22 | 0.4373 (7) | −0.0456 (4) | 0.1054 (5) | 0.0570 (14) | |
H22 | 0.5252 | −0.0482 | 0.1639 | 0.068* | |
C23 | −0.0032 (7) | 0.0732 (7) | −0.1502 (5) | 0.080 (2) | |
H23 | −0.0898 | 0.0777 | −0.2087 | 0.096* | |
C24 | 0.0478 (8) | −0.0280 (7) | −0.1578 (5) | 0.082 (2) | |
H24 | −0.0044 | −0.0920 | −0.2210 | 0.098* | |
H25 | 0.359 (7) | 0.026 (3) | 0.330 (4) | 0.080* | |
H26 | 0.360 (7) | 0.120 (4) | 0.409 (2) | 0.080* | |
H27 | 0.484 (6) | 0.446 (2) | 0.389 (4) | 0.080* | |
H28 | 0.511 (6) | 0.374 (5) | 0.462 (2) | 0.080* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nb1 | 0.0455 (3) | 0.0366 (2) | 0.0480 (3) | 0.00582 (19) | 0.0094 (2) | 0.0156 (2) |
Cd1 | 0.03382 (19) | 0.03347 (19) | 0.0463 (2) | 0.00719 (14) | 0.00468 (15) | 0.00974 (15) |
F1 | 0.0536 (18) | 0.0518 (18) | 0.066 (2) | 0.0006 (14) | 0.0051 (15) | 0.0070 (15) |
F2 | 0.087 (3) | 0.093 (3) | 0.101 (3) | 0.014 (2) | 0.054 (2) | 0.045 (2) |
F3 | 0.081 (2) | 0.053 (2) | 0.093 (3) | 0.0164 (18) | −0.030 (2) | 0.0021 (18) |
F4 | 0.119 (3) | 0.133 (3) | 0.088 (3) | 0.081 (3) | 0.067 (2) | 0.055 (2) |
F5 | 0.078 (2) | 0.0386 (17) | 0.107 (3) | 0.0187 (16) | −0.006 (2) | 0.0261 (17) |
N1 | 0.033 (2) | 0.033 (2) | 0.056 (2) | 0.0069 (17) | 0.0087 (18) | 0.0082 (18) |
N2 | 0.046 (2) | 0.042 (2) | 0.053 (2) | 0.0124 (18) | 0.021 (2) | 0.0149 (19) |
N3 | 0.044 (2) | 0.036 (2) | 0.049 (2) | 0.0095 (18) | −0.0006 (19) | 0.0126 (19) |
N4 | 0.050 (2) | 0.039 (2) | 0.045 (2) | 0.0098 (18) | 0.019 (2) | 0.0148 (18) |
O1 | 0.055 (2) | 0.0308 (17) | 0.053 (2) | 0.0039 (16) | 0.0131 (18) | 0.0085 (15) |
O2 | 0.079 (3) | 0.0335 (18) | 0.052 (2) | 0.0184 (18) | 0.021 (2) | 0.0115 (16) |
O3 | 0.063 (2) | 0.0427 (19) | 0.080 (3) | 0.0250 (17) | 0.027 (2) | 0.0249 (18) |
C1 | 0.039 (3) | 0.042 (3) | 0.083 (4) | 0.012 (2) | 0.012 (3) | 0.024 (3) |
C2 | 0.048 (3) | 0.060 (3) | 0.082 (4) | 0.025 (3) | 0.010 (3) | 0.031 (3) |
C3 | 0.044 (3) | 0.059 (4) | 0.082 (4) | 0.020 (3) | 0.008 (3) | 0.017 (3) |
C4 | 0.032 (3) | 0.048 (3) | 0.067 (3) | 0.006 (2) | 0.012 (2) | 0.002 (3) |
C5 | 0.035 (2) | 0.034 (2) | 0.047 (3) | 0.0071 (19) | 0.015 (2) | 0.002 (2) |
C6 | 0.043 (3) | 0.037 (2) | 0.045 (3) | 0.009 (2) | 0.021 (2) | 0.002 (2) |
C7 | 0.052 (3) | 0.049 (3) | 0.071 (4) | 0.004 (2) | 0.033 (3) | 0.012 (3) |
C8 | 0.069 (4) | 0.067 (4) | 0.101 (5) | 0.006 (3) | 0.044 (4) | 0.031 (4) |
C9 | 0.097 (5) | 0.071 (4) | 0.107 (5) | 0.021 (4) | 0.058 (5) | 0.052 (4) |
C10 | 0.064 (4) | 0.064 (4) | 0.074 (4) | 0.022 (3) | 0.031 (3) | 0.031 (3) |
C11 | 0.033 (3) | 0.071 (4) | 0.088 (4) | 0.005 (3) | 0.014 (3) | 0.015 (3) |
C12 | 0.039 (3) | 0.067 (4) | 0.094 (5) | −0.006 (3) | 0.027 (3) | 0.013 (3) |
C13 | 0.063 (4) | 0.052 (3) | 0.066 (4) | 0.025 (3) | 0.002 (3) | 0.017 (3) |
C14 | 0.058 (4) | 0.073 (4) | 0.079 (4) | 0.025 (3) | 0.002 (3) | 0.032 (4) |
C15 | 0.044 (3) | 0.106 (5) | 0.076 (4) | 0.022 (3) | 0.009 (3) | 0.056 (4) |
C16 | 0.040 (3) | 0.079 (4) | 0.046 (3) | 0.002 (3) | 0.006 (2) | 0.023 (3) |
C17 | 0.039 (3) | 0.050 (3) | 0.037 (3) | 0.001 (2) | 0.007 (2) | 0.015 (2) |
C18 | 0.045 (3) | 0.048 (3) | 0.036 (3) | −0.003 (2) | 0.015 (2) | 0.008 (2) |
C19 | 0.066 (4) | 0.060 (4) | 0.041 (3) | −0.010 (3) | 0.026 (3) | −0.007 (3) |
C20 | 0.108 (6) | 0.056 (4) | 0.064 (4) | −0.005 (4) | 0.047 (4) | −0.012 (3) |
C21 | 0.118 (6) | 0.049 (3) | 0.082 (5) | 0.019 (4) | 0.068 (5) | 0.010 (3) |
C22 | 0.077 (4) | 0.044 (3) | 0.063 (3) | 0.022 (3) | 0.038 (3) | 0.018 (3) |
C23 | 0.048 (4) | 0.109 (6) | 0.052 (4) | −0.008 (4) | −0.003 (3) | 0.015 (4) |
C24 | 0.068 (4) | 0.092 (5) | 0.047 (4) | −0.023 (4) | 0.009 (3) | −0.009 (3) |
Nb1—O3 | 1.764 (3) | C5—C6 | 1.442 (6) |
Nb1—F4 | 1.882 (3) | C6—C7 | 1.402 (6) |
Nb1—F3 | 1.903 (3) | C7—C8 | 1.408 (8) |
Nb1—F2 | 1.935 (3) | C7—C12 | 1.421 (8) |
Nb1—F1 | 1.966 (3) | C8—C9 | 1.347 (9) |
Nb1—F5 | 2.046 (3) | C8—H8 | 0.9300 |
Cd1—O2 | 2.279 (3) | C9—C10 | 1.398 (8) |
Cd1—O1 | 2.296 (3) | C9—H9 | 0.9300 |
Cd1—N1 | 2.317 (4) | C10—H10 | 0.9300 |
Cd1—N3 | 2.324 (4) | C11—C12 | 1.348 (8) |
Cd1—N4 | 2.364 (4) | C11—H11 | 0.9300 |
Cd1—N2 | 2.364 (4) | C12—H12 | 0.9300 |
N1—C1 | 1.321 (6) | C13—C14 | 1.375 (7) |
N1—C5 | 1.351 (5) | C13—H13 | 0.9300 |
N2—C10 | 1.321 (6) | C14—C15 | 1.342 (9) |
N2—C6 | 1.366 (6) | C14—H14 | 0.9300 |
N3—C13 | 1.336 (6) | C15—C16 | 1.403 (8) |
N3—C17 | 1.350 (6) | C15—H15 | 0.9300 |
N4—C22 | 1.326 (6) | C16—C23 | 1.404 (9) |
N4—C18 | 1.358 (6) | C16—C17 | 1.415 (7) |
O1—H25 | 0.847 (19) | C17—C18 | 1.439 (7) |
O1—H26 | 0.839 (19) | C18—C19 | 1.404 (7) |
O2—H27 | 0.848 (19) | C19—C20 | 1.405 (8) |
O2—H28 | 0.831 (19) | C19—C24 | 1.430 (8) |
C1—C2 | 1.398 (7) | C20—C21 | 1.353 (9) |
C1—H1 | 0.9300 | C20—H20 | 0.9300 |
C2—C3 | 1.338 (8) | C21—C22 | 1.384 (8) |
C2—H2 | 0.9300 | C21—H21 | 0.9300 |
C3—C4 | 1.408 (8) | C22—H22 | 0.9300 |
C3—H3 | 0.9300 | C23—C24 | 1.345 (9) |
C4—C5 | 1.408 (6) | C23—H23 | 0.9300 |
C4—C11 | 1.410 (7) | C24—H24 | 0.9300 |
O3—Nb1—F4 | 97.27 (16) | N1—C5—C4 | 122.0 (4) |
O3—Nb1—F3 | 95.20 (16) | N1—C5—C6 | 119.4 (4) |
F4—Nb1—F3 | 92.4 (2) | C4—C5—C6 | 118.7 (4) |
O3—Nb1—F2 | 94.16 (16) | N2—C6—C7 | 122.0 (4) |
F4—Nb1—F2 | 168.09 (15) | N2—C6—C5 | 118.4 (4) |
F3—Nb1—F2 | 89.83 (18) | C7—C6—C5 | 119.6 (4) |
O3—Nb1—F1 | 93.48 (15) | C6—C7—C8 | 117.9 (5) |
F4—Nb1—F1 | 89.08 (17) | C6—C7—C12 | 119.2 (5) |
F3—Nb1—F1 | 170.92 (13) | C8—C7—C12 | 122.8 (5) |
F2—Nb1—F1 | 86.89 (16) | C9—C8—C7 | 118.8 (6) |
O3—Nb1—F5 | 174.37 (16) | C9—C8—H8 | 120.6 |
F4—Nb1—F5 | 87.87 (16) | C7—C8—H8 | 120.6 |
F3—Nb1—F5 | 86.84 (13) | C8—C9—C10 | 120.8 (6) |
F2—Nb1—F5 | 80.58 (16) | C8—C9—H9 | 119.6 |
F1—Nb1—F5 | 84.27 (13) | C10—C9—H9 | 119.6 |
O2—Cd1—O1 | 83.87 (13) | N2—C10—C9 | 122.0 (6) |
O2—Cd1—N1 | 101.00 (13) | N2—C10—H10 | 119.0 |
O1—Cd1—N1 | 94.16 (13) | C9—C10—H10 | 119.0 |
O2—Cd1—N3 | 90.24 (14) | C12—C11—C4 | 120.7 (5) |
O1—Cd1—N3 | 99.79 (13) | C12—C11—H11 | 119.7 |
N1—Cd1—N3 | 162.96 (14) | C4—C11—H11 | 119.7 |
O2—Cd1—N4 | 156.25 (14) | C11—C12—C7 | 121.6 (5) |
O1—Cd1—N4 | 84.41 (13) | C11—C12—H12 | 119.2 |
N1—Cd1—N4 | 100.39 (13) | C7—C12—H12 | 119.2 |
N3—Cd1—N4 | 71.53 (14) | N3—C13—C14 | 123.0 (6) |
O2—Cd1—N2 | 86.50 (13) | N3—C13—H13 | 118.5 |
O1—Cd1—N2 | 161.40 (13) | C14—C13—H13 | 118.5 |
N1—Cd1—N2 | 72.10 (13) | C15—C14—C13 | 119.4 (6) |
N3—Cd1—N2 | 96.12 (14) | C15—C14—H14 | 120.3 |
N4—Cd1—N2 | 109.92 (13) | C13—C14—H14 | 120.3 |
C1—N1—C5 | 119.1 (4) | C14—C15—C16 | 120.6 (5) |
C1—N1—Cd1 | 124.7 (3) | C14—C15—H15 | 119.7 |
C5—N1—Cd1 | 115.5 (3) | C16—C15—H15 | 119.7 |
C10—N2—C6 | 118.5 (4) | C15—C16—C23 | 123.8 (6) |
C10—N2—Cd1 | 127.1 (4) | C15—C16—C17 | 116.8 (5) |
C6—N2—Cd1 | 113.9 (3) | C23—C16—C17 | 119.4 (6) |
C13—N3—C17 | 118.3 (4) | N3—C17—C16 | 121.9 (5) |
C13—N3—Cd1 | 125.3 (3) | N3—C17—C18 | 118.7 (4) |
C17—N3—Cd1 | 116.3 (3) | C16—C17—C18 | 119.3 (5) |
C22—N4—C18 | 119.1 (4) | N4—C18—C19 | 121.9 (5) |
C22—N4—Cd1 | 125.9 (4) | N4—C18—C17 | 118.7 (4) |
C18—N4—Cd1 | 114.6 (3) | C19—C18—C17 | 119.5 (5) |
Cd1—O1—H25 | 111 (4) | C18—C19—C20 | 117.2 (6) |
Cd1—O1—H26 | 118 (4) | C18—C19—C24 | 119.1 (6) |
H25—O1—H26 | 107 (3) | C20—C19—C24 | 123.7 (6) |
Cd1—O2—H27 | 120 (4) | C21—C20—C19 | 119.7 (6) |
Cd1—O2—H28 | 115 (4) | C21—C20—H20 | 120.1 |
H27—O2—H28 | 107 (3) | C19—C20—H20 | 120.1 |
N1—C1—C2 | 122.1 (5) | C20—C21—C22 | 120.1 (6) |
N1—C1—H1 | 118.9 | C20—C21—H21 | 120.0 |
C2—C1—H1 | 118.9 | C22—C21—H21 | 120.0 |
C3—C2—C1 | 119.6 (5) | N4—C22—C21 | 122.0 (6) |
C3—C2—H2 | 120.2 | N4—C22—H22 | 119.0 |
C1—C2—H2 | 120.2 | C21—C22—H22 | 119.0 |
C2—C3—C4 | 120.2 (5) | C24—C23—C16 | 121.7 (6) |
C2—C3—H3 | 119.9 | C24—C23—H23 | 119.1 |
C4—C3—H3 | 119.9 | C16—C23—H23 | 119.1 |
C3—C4—C5 | 116.9 (5) | C23—C24—C19 | 121.1 (6) |
C3—C4—C11 | 122.8 (5) | C23—C24—H24 | 119.5 |
C5—C4—C11 | 120.3 (5) | C19—C24—H24 | 119.5 |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H25···O3i | 0.85 (4) | 1.83 (4) | 2.672 (5) | 177 |
O1—H26···F1 | 0.84 (3) | 1.84 (3) | 2.679 (5) | 172 (6) |
O2—H27···F5ii | 0.85 (3) | 1.74 (3) | 2.582 (5) | 171 |
O2—H28···F2 | 0.83 (3) | 2.12 (5) | 2.851 (5) | 146 (5) |
O2—H28···F5 | 0.83 (3) | 2.44 (3) | 3.130 (5) | 142 (5) |
C11—H11···F5iii | 0.93 | 2.52 | 3.427 (7) | 166 |
C12—H12···F2iv | 0.93 | 2.43 | 3.299 (7) | 156 |
C13—H13···F3ii | 0.93 | 2.48 | 3.089 (7) | 123 |
C15—H15···F3v | 0.93 | 2.33 | 3.224 (8) | 161 |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x+1, y, z; (iv) −x+2, −y+1, −z+1; (v) x−1, y, z−1. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C12H8N2)2(H2O)2]2+·[NbOF5]2− |
Mr | 712.75 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 9.487 (4), 11.537 (5), 13.007 (5) |
α, β, γ (°) | 99.162 (6), 109.646 (6), 100.661 (5) |
V (Å3) | 1279.3 (9) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.35 |
Crystal size (mm) | 0.35 × 0.33 × 0.29 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2002) |
Tmin, Tmax | 0.650, 0.696 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6750, 4464, 3413 |
Rint | 0.016 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.092, 1.00 |
No. of reflections | 4464 |
No. of parameters | 355 |
No. of restraints | 6 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.50, −0.79 |
Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1994), SHELXTL (Siemens, 1995).
Nb1—O3 | 1.764 (3) | Cd1—O2 | 2.279 (3) |
Nb1—F4 | 1.882 (3) | Cd1—O1 | 2.296 (3) |
Nb1—F3 | 1.903 (3) | Cd1—N1 | 2.317 (4) |
Nb1—F2 | 1.935 (3) | Cd1—N3 | 2.324 (4) |
Nb1—F1 | 1.966 (3) | Cd1—N4 | 2.364 (4) |
Nb1—F5 | 2.046 (3) | Cd1—N2 | 2.364 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H25···O3i | 0.85 (4) | 1.83 (4) | 2.672 (5) | 177 |
O1—H26···F1 | 0.84 (3) | 1.84 (3) | 2.679 (5) | 172 (6) |
O2—H27···F5ii | 0.85 (3) | 1.74 (3) | 2.582 (5) | 171 |
O2—H28···F2 | 0.83 (3) | 2.12 (5) | 2.851 (5) | 146 (5) |
O2—H28···F5 | 0.83 (3) | 2.44 (3) | 3.130 (5) | 142 (5) |
C11—H11···F5iii | 0.93 | 2.52 | 3.427 (7) | 166 |
C12—H12···F2iv | 0.93 | 2.43 | 3.299 (7) | 156 |
C13—H13···F3ii | 0.93 | 2.48 | 3.089 (7) | 123 |
C15—H15···F3v | 0.93 | 2.33 | 3.224 (8) | 161 |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x+1, y, z; (iv) −x+2, −y+1, −z+1; (v) x−1, y, z−1. |
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Out-of-center `primary' electronic distortions are inherent to oxide fluoride anions of the early d0 transition metals. In the [NbOF5]2− anion, the NbV atom deviates from the center of the octahedron toward the oxygen ligand, forming a short Nb═O bond and long trans Nb—F bond. The trans-directing property of the [NbOF5]2− anion can be exploited when designing new materials that exhibit important structure-dependent properties such as piezoelectricity, second-order non-linear optical activity and ferroelectricity (Heier et al., 1998; Welk et al., 2002). Here the synthesis, crystal structure and characterization of a mixed-metal complex [Cd(C12H8N2)2(H2O)2]2+·[NbOF5]2− (I), which incorporates the [NbOF5]2− anion, is reported.
The molecular structure of (I) is shown in Fig. 1. The crystal structure of (I) is built up of CdII complex cations and NbV complex anions. The CdII atom has an octahedral coordination geometry with two 1,10-phenanthroline (phen) and two water molecules. The NbV atom assumes a distorted octahedral coordination with five F atoms and one O atom. The Nb—F bond trans to the Nb═O bond is significantly longer than the other four Nb—F bonds in the same anion (Table 1). This feature was also observed in previously reported structures (Halasyamani et al., 1996; Norquist et al., 1999; Izumi et al., 2005). The coordinated water molecules of the CdII complex cation form hydrogen bonds with the [NbOF5]2− anion. Some phen H atoms also interact with the [NbOF5]2− anion by C—H···F hydrogen bonds (Table 2).