Buy article online - an online subscription or single-article purchase is required to access this article.
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
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.015 Å
- R factor = 0.064
- wR factor = 0.224
- Data-to-parameter ratio = 11.6
checkCIF/PLATON results
No syntax errors found
Alert level A ABSTM02_ALERT_3_A The ratio of expected to reported Tmax/Tmin(RR') is < 0.50 Tmin and Tmax reported: 0.368 0.971 Tmin' and Tmax expected: 0.904 0.971 RR' = 0.407 Please check that your absorption correction is appropriate.
Author Response: The range is given by SADABS. |
PLAT061_ALERT_3_A Tmax/Tmin Range Test RR' too Large ............. 0.41
Author Response: The range is given by SADABS. |
Alert level B PLAT341_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 16
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT733_ALERT_1_C Torsion Calc 164.9(5), Rep 164.9(2) ...... 2.50 su-Rat O3 -P1 -O3 -V1 4.565 1.555 1.555 3.767
2 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 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 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
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. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register