metal-organic compounds
The crystal structure of [VO(HPO4)(C12H8N2)]n consists of a bis(vanadyl hydrogen phosphate) skeleton that assumes a linear ribbon conformation; the nitrogen heterocycles that chelate to the VIV atoms are connected to the sides of the flat ribbon. The compound is isostructural with the hydrogen arsenate, whose structure has been reported by Hou et al. [Inorg. Chem. Commun. (2004). 7, 128–130]. The asymmetric unit, with the exception of one O atom, lies on a mirror plane
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804023931/kp6002sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804023931/kp6002Isup2.hkl |
CCDC reference: 252956
Computing details top
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: Atomic coordinates taken from the published As analog (Hou et al., 2004); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly[bis[oxo(1,10-phenanthroline)vanadium(IV)]-di-µ-hydrogenphosphato] top
Crystal data top
[V2O2(HPO4)2(C12H8N2)2] | F(000) = 346 |
Mr = 686.24 | Dx = 1.884 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yb | Cell parameters from 298 reflections |
a = 9.815 (2) Å | θ = 2.6–19.6° |
b = 6.372 (1) Å | µ = 0.98 mm−1 |
c = 9.919 (2) Å | T = 295 K |
β = 102.753 (4)° | Prism, red |
V = 605.0 (2) Å3 | 0.10 × 0.10 × 0.03 mm |
Z = 1 |
Data collection top
Bruker APEX area-detector diffractometer | 1434 independent reflections |
Radiation source: fine-focus sealed tube | 852 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.072 |
φ and ω scan | θmax = 27.1°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −12→12 |
Tmin = 0.368, Tmax = 0.971 | k = −8→6 |
3639 measured reflections | l = −12→12 |
Refinement top
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.224 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.117P)2 + 0.0738P] where P = (Fo2 + 2Fc2)/3 |
1434 reflections | (Δ/σ)max = 0.001 |
124 parameters | Δρmax = 1.08 e Å−3 |
0 restraints | Δρmin = −0.70 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
V1 | 0.79737 (17) | 0.2500 | 0.93114 (16) | 0.0174 (5) | |
P1 | 1.1208 (3) | 0.2500 | 1.0954 (2) | 0.0172 (6) | |
O1 | 0.7622 (8) | 0.2500 | 1.0819 (7) | 0.0362 (19) | |
O2 | 1.0564 (7) | 0.2500 | 1.2251 (7) | 0.0332 (18) | |
H2o | 0.9676 | 0.2500 | 1.2095 | 0.040* | |
O3 | 1.2121 (5) | 0.4404 (7) | 1.1025 (5) | 0.0259 (12) | |
O4 | 1.0024 (7) | 0.2500 | 0.9677 (6) | 0.0227 (16) | |
N1 | 0.5831 (8) | 0.2500 | 0.8254 (8) | 0.0191 (17) | |
N2 | 0.7975 (8) | 0.2500 | 0.7005 (8) | 0.0204 (18) | |
C1 | 0.4727 (11) | 0.2500 | 0.8872 (11) | 0.031 (3) | |
H1 | 0.4904 | 0.2500 | 0.9832 | 0.037* | |
C2 | 0.3422 (11) | 0.2500 | 0.8182 (13) | 0.040 (3) | |
H2 | 0.2700 | 0.2500 | 0.8652 | 0.048* | |
C3 | 0.3130 (11) | 0.2500 | 0.6771 (13) | 0.037 (3) | |
H3 | 0.2203 | 0.2500 | 0.6288 | 0.044* | |
C4 | 0.4161 (10) | 0.2500 | 0.6054 (11) | 0.024 (2) | |
C5 | 0.3963 (11) | 0.2500 | 0.4587 (11) | 0.029 (2) | |
H5 | 0.3056 | 0.2500 | 0.4052 | 0.034* | |
C6 | 0.5020 (13) | 0.2500 | 0.3953 (11) | 0.033 (3) | |
H6 | 0.4842 | 0.2500 | 0.2992 | 0.040* | |
C7 | 0.6405 (10) | 0.2500 | 0.4720 (10) | 0.024 (2) | |
C8 | 0.7593 (13) | 0.2500 | 0.4133 (11) | 0.040 (3) | |
H8 | 0.7485 | 0.2500 | 0.3177 | 0.049* | |
C9 | 0.8927 (12) | 0.2500 | 0.4989 (12) | 0.034 (3) | |
H9 | 0.9720 | 0.2500 | 0.4620 | 0.041* | |
C10 | 0.9038 (11) | 0.2500 | 0.6422 (11) | 0.029 (2) | |
H10 | 0.9928 | 0.2500 | 0.6991 | 0.035* | |
C11 | 0.6656 (9) | 0.2500 | 0.6168 (9) | 0.018 (2) | |
C12 | 0.5529 (10) | 0.2500 | 0.6844 (10) | 0.021 (2) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
V1 | 0.0230 (10) | 0.0119 (8) | 0.0156 (9) | 0.000 | 0.0003 (6) | 0.000 |
P1 | 0.0191 (14) | 0.0123 (12) | 0.0179 (14) | 0.000 | −0.0012 (10) | 0.000 |
O1 | 0.054 (5) | 0.036 (4) | 0.018 (4) | 0.000 | 0.009 (3) | 0.000 |
O2 | 0.030 (4) | 0.052 (5) | 0.017 (4) | 0.000 | 0.004 (3) | 0.000 |
O3 | 0.035 (3) | 0.012 (2) | 0.028 (3) | 0.001 (2) | 0.001 (2) | −0.001 (2) |
O4 | 0.026 (4) | 0.024 (4) | 0.017 (4) | 0.000 | 0.000 (3) | 0.000 |
N1 | 0.019 (4) | 0.018 (4) | 0.020 (4) | 0.000 | 0.005 (3) | 0.000 |
N2 | 0.020 (4) | 0.019 (4) | 0.025 (5) | 0.000 | 0.009 (4) | 0.000 |
C1 | 0.041 (7) | 0.028 (6) | 0.031 (6) | 0.000 | 0.022 (5) | 0.000 |
C2 | 0.014 (6) | 0.055 (8) | 0.056 (8) | 0.000 | 0.016 (5) | 0.000 |
C3 | 0.027 (6) | 0.031 (6) | 0.050 (8) | 0.000 | 0.004 (5) | 0.000 |
C4 | 0.013 (5) | 0.024 (5) | 0.031 (6) | 0.000 | 0.000 (4) | 0.000 |
C5 | 0.016 (5) | 0.026 (5) | 0.038 (7) | 0.000 | −0.008 (5) | 0.000 |
C6 | 0.053 (8) | 0.026 (6) | 0.016 (5) | 0.000 | −0.002 (5) | 0.000 |
C7 | 0.025 (6) | 0.026 (5) | 0.020 (5) | 0.000 | 0.000 (4) | 0.000 |
C8 | 0.077 (10) | 0.026 (6) | 0.021 (6) | 0.000 | 0.016 (6) | 0.000 |
C9 | 0.026 (6) | 0.046 (7) | 0.036 (6) | 0.000 | 0.017 (5) | 0.000 |
C10 | 0.022 (6) | 0.035 (6) | 0.031 (6) | 0.000 | 0.005 (5) | 0.000 |
C11 | 0.018 (5) | 0.014 (4) | 0.018 (5) | 0.000 | −0.001 (4) | 0.000 |
C12 | 0.021 (5) | 0.018 (5) | 0.023 (5) | 0.000 | 0.003 (4) | 0.000 |
Geometric parameters (Å, º) top
V1—O1 | 1.607 (7) | C2—H2 | 0.9300 |
V1—O3i | 2.000 (4) | C3—C4 | 1.359 (14) |
V1—O3ii | 2.000 (4) | C3—H3 | 0.9300 |
V1—O4 | 1.964 (7) | C4—C12 | 1.397 (13) |
V1—N1 | 2.133 (8) | C4—C5 | 1.424 (14) |
V1—N2 | 2.288 (8) | C5—C6 | 1.327 (15) |
P1—O3 | 1.500 (5) | C5—H5 | 0.9300 |
P1—O3iii | 1.500 (5) | C6—C7 | 1.403 (15) |
P1—O4 | 1.518 (7) | C6—H6 | 0.9300 |
P1—O2 | 1.554 (7) | C7—C11 | 1.402 (13) |
O2—H2o | 0.85 | C7—C8 | 1.414 (15) |
N1—C1 | 1.358 (12) | C8—C9 | 1.395 (17) |
N1—C12 | 1.364 (12) | C8—H8 | 0.9300 |
N2—C10 | 1.300 (12) | C9—C10 | 1.401 (15) |
N2—C11 | 1.375 (12) | C9—H9 | 0.9300 |
C1—C2 | 1.312 (16) | C10—H10 | 0.9300 |
C1—H1 | 0.9300 | C11—C12 | 1.415 (13) |
C2—C3 | 1.366 (16) | ||
O1—V1—O3i | 98.3 (1) | C1—C2—C3 | 119.6 (11) |
O1—V1—O3ii | 98.3 (1) | C1—C2—H2 | 120.2 |
O1—V1—O4 | 104.5 (3) | C3—C2—H2 | 120.2 |
O1—V1—N1 | 93.8 (4) | C4—C3—C2 | 121.6 (11) |
O1—V1—N2 | 167.9 (4) | C4—C3—H3 | 119.2 |
O3i—V1—O3ii | 161.2 (3) | C2—C3—H3 | 119.2 |
O3i—V1—O4 | 92.2 (1) | C3—C4—C12 | 116.1 (10) |
O3i—V1—N1 | 85.0 (1) | C3—C4—C5 | 125.8 (10) |
O3i—V1—N2 | 81.0 (1) | C12—C4—C5 | 118.0 (9) |
O3ii—V1—O4 | 92.2 (2) | C6—C5—C4 | 122.7 (10) |
O3ii—V1—N1 | 85.0 (1) | C6—C5—H5 | 118.7 |
O3ii—V1—N2 | 81.0 (1) | C4—C5—H5 | 118.7 |
O4—V1—N1 | 161.7 (3) | C5—C6—C7 | 120.5 (10) |
O4—V1—N2 | 87.6 (3) | C5—C6—H6 | 119.7 |
N1—V1—N2 | 74.1 (3) | C7—C6—H6 | 119.7 |
O3—P1—O3iii | 107.9 (4) | C11—C7—C6 | 119.1 (9) |
O3—P1—O4 | 112.3 (2) | C11—C7—C8 | 116.6 (9) |
O3iii—P1—O4 | 112.3 (2) | C6—C7—C8 | 124.3 (10) |
O3—P1—O2 | 108.0 (3) | C9—C8—C7 | 119.9 (10) |
O3iii—P1—O2 | 108.0 (3) | C9—C8—H8 | 120.1 |
O4—P1—O2 | 108.3 (4) | C7—C8—H8 | 120.1 |
P1—O2—H2o | 115.9 | C8—C9—C10 | 118.0 (10) |
P1—O3—V1ii | 141.7 (3) | C8—C9—H9 | 121.0 |
P1—O4—V1 | 135.9 (4) | C10—C9—H9 | 121.0 |
C1—N1—C12 | 116.6 (9) | N2—C10—C9 | 124.1 (10) |
C1—N1—V1 | 125.2 (7) | N2—C10—H10 | 117.9 |
C12—N1—V1 | 118.2 (6) | C9—C10—H10 | 117.9 |
C10—N2—C11 | 118.2 (8) | N2—C11—C7 | 123.2 (9) |
C10—N2—V1 | 128.5 (7) | N2—C11—C12 | 116.4 (8) |
C11—N2—V1 | 113.3 (6) | C7—C11—C12 | 120.4 (9) |
C2—C1—N1 | 123.3 (10) | N1—C12—C4 | 122.7 (9) |
C2—C1—H1 | 118.3 | N1—C12—C11 | 118.0 (9) |
N1—C1—H1 | 118.3 | C4—C12—C11 | 119.3 (9) |
O3iii—P1—O3—V1ii | 164.9 (2) | C1—C2—C3—C4 | 0.000 (5) |
O4—P1—O3—V1ii | 40.7 (6) | C2—C3—C4—C12 | 0.000 (4) |
O2—P1—O3—V1ii | −78.7 (5) | C2—C3—C4—C5 | 180.000 (4) |
O3—P1—O4—V1 | −119.1 (2) | C3—C4—C5—C6 | 180.000 (2) |
O3iii—P1—O4—V1 | 119.1 (2) | C12—C4—C5—C6 | 0.000 (3) |
O2—P1—O4—V1 | 0.000 (2) | C4—C5—C6—C7 | 0.000 (3) |
O1—V1—O4—P1 | 0.000 (1) | C5—C6—C7—C11 | 0.000 (2) |
O3i—V1—O4—P1 | −99.13 (14) | C5—C6—C7—C8 | 180.000 (2) |
O3ii—V1—O4—P1 | 99.13 (14) | C11—C7—C8—C9 | 0.000 (3) |
N1—V1—O4—P1 | 180.000 (3) | C6—C7—C8—C9 | 180.000 (2) |
N2—V1—O4—P1 | 180.000 (1) | C7—C8—C9—C10 | 0.000 (2) |
O1—V1—N1—C1 | 0.000 (3) | C11—N2—C10—C9 | 0.000 (3) |
O4—V1—N1—C1 | 180.000 (4) | V1—N2—C10—C9 | 180.000 (3) |
O3i—V1—N1—C1 | 97.99 (14) | C8—C9—C10—N2 | 0.000 (3) |
O3ii—V1—N1—C1 | −97.99 (14) | C10—N2—C11—C7 | 0.000 (3) |
N2—V1—N1—C1 | 180.000 (4) | V1—N2—C11—C7 | 180.000 (2) |
O1—V1—N1—C12 | 180.000 (2) | C10—N2—C11—C12 | 180.000 (2) |
O4—V1—N1—C12 | 0.000 (5) | V1—N2—C11—C12 | 0.000 (2) |
O3i—V1—N1—C12 | −82.01 (14) | C6—C7—C11—N2 | 180.000 (2) |
O3ii—V1—N1—C12 | 82.01 (14) | C8—C7—C11—N2 | 0.000 (2) |
N2—V1—N1—C12 | 0.000 (2) | C6—C7—C11—C12 | 0.000 (3) |
O1—V1—N2—C10 | 180.000 (5) | C8—C7—C11—C12 | 180.000 (2) |
O4—V1—N2—C10 | 0.000 (2) | C1—N1—C12—C4 | 0.000 (3) |
O3i—V1—N2—C10 | −92.63 (14) | V1—N1—C12—C4 | 180.000 (2) |
O3ii—V1—N2—C10 | 92.63 (14) | C1—N1—C12—C11 | 180.000 (3) |
N1—V1—N2—C10 | 180.000 (3) | V1—N1—C12—C11 | 0.000 (3) |
O1—V1—N2—C11 | 0.000 (6) | C3—C4—C12—N1 | 0.000 (3) |
O4—V1—N2—C11 | 180.000 (2) | C5—C4—C12—N1 | 180.000 (2) |
O3i—V1—N2—C11 | 87.37 (14) | C3—C4—C12—C11 | 180.000 (3) |
O3ii—V1—N2—C11 | −87.37 (14) | C5—C4—C12—C11 | 0.000 (3) |
N1—V1—N2—C11 | 0.000 (2) | N2—C11—C12—N1 | 0.000 (3) |
C12—N1—C1—C2 | 0.000 (5) | C7—C11—C12—N1 | 180.000 (2) |
V1—N1—C1—C2 | 180.000 (4) | N2—C11—C12—C4 | 180.000 (3) |
N1—C1—C2—C3 | 0.000 (5) | C7—C11—C12—C4 | 0.000 (3) |
Symmetry codes: (i) −x+2, y−1/2, −z+2; (ii) −x+2, −y+1, −z+2; (iii) x, −y+1/2, z. |