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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804023931/kp6002sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804023931/kp6002Isup2.hkl
Contains datablock I

CCDC reference: 252956

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](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 = 686.24Dx = 1.884 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 298 reflections
a = 9.815 (2) Åθ = 2.6–19.6°
b = 6.372 (1) ŵ = 0.98 mm1
c = 9.919 (2) ÅT = 295 K
β = 102.753 (4)°Prism, red
V = 605.0 (2) Å30.10 × 0.10 × 0.03 mm
Z = 1
Data collection top
Bruker APEX area-detector
diffractometer
1434 independent reflections
Radiation source: fine-focus sealed tube852 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.072
φ and ω scanθmax = 27.1°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1212
Tmin = 0.368, Tmax = 0.971k = 86
3639 measured reflectionsl = 1212
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)] = 0.064Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.224H-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 parametersΔρmax = 1.08 e Å3
0 restraintsΔρmin = 0.70 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V10.79737 (17)0.25000.93114 (16)0.0174 (5)
P11.1208 (3)0.25001.0954 (2)0.0172 (6)
O10.7622 (8)0.25001.0819 (7)0.0362 (19)
O21.0564 (7)0.25001.2251 (7)0.0332 (18)
H2o0.96760.25001.20950.040*
O31.2121 (5)0.4404 (7)1.1025 (5)0.0259 (12)
O41.0024 (7)0.25000.9677 (6)0.0227 (16)
N10.5831 (8)0.25000.8254 (8)0.0191 (17)
N20.7975 (8)0.25000.7005 (8)0.0204 (18)
C10.4727 (11)0.25000.8872 (11)0.031 (3)
H10.49040.25000.98320.037*
C20.3422 (11)0.25000.8182 (13)0.040 (3)
H20.27000.25000.86520.048*
C30.3130 (11)0.25000.6771 (13)0.037 (3)
H30.22030.25000.62880.044*
C40.4161 (10)0.25000.6054 (11)0.024 (2)
C50.3963 (11)0.25000.4587 (11)0.029 (2)
H50.30560.25000.40520.034*
C60.5020 (13)0.25000.3953 (11)0.033 (3)
H60.48420.25000.29920.040*
C70.6405 (10)0.25000.4720 (10)0.024 (2)
C80.7593 (13)0.25000.4133 (11)0.040 (3)
H80.74850.25000.31770.049*
C90.8927 (12)0.25000.4989 (12)0.034 (3)
H90.97200.25000.46200.041*
C100.9038 (11)0.25000.6422 (11)0.029 (2)
H100.99280.25000.69910.035*
C110.6656 (9)0.25000.6168 (9)0.018 (2)
C120.5529 (10)0.25000.6844 (10)0.021 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0230 (10)0.0119 (8)0.0156 (9)0.0000.0003 (6)0.000
P10.0191 (14)0.0123 (12)0.0179 (14)0.0000.0012 (10)0.000
O10.054 (5)0.036 (4)0.018 (4)0.0000.009 (3)0.000
O20.030 (4)0.052 (5)0.017 (4)0.0000.004 (3)0.000
O30.035 (3)0.012 (2)0.028 (3)0.001 (2)0.001 (2)0.001 (2)
O40.026 (4)0.024 (4)0.017 (4)0.0000.000 (3)0.000
N10.019 (4)0.018 (4)0.020 (4)0.0000.005 (3)0.000
N20.020 (4)0.019 (4)0.025 (5)0.0000.009 (4)0.000
C10.041 (7)0.028 (6)0.031 (6)0.0000.022 (5)0.000
C20.014 (6)0.055 (8)0.056 (8)0.0000.016 (5)0.000
C30.027 (6)0.031 (6)0.050 (8)0.0000.004 (5)0.000
C40.013 (5)0.024 (5)0.031 (6)0.0000.000 (4)0.000
C50.016 (5)0.026 (5)0.038 (7)0.0000.008 (5)0.000
C60.053 (8)0.026 (6)0.016 (5)0.0000.002 (5)0.000
C70.025 (6)0.026 (5)0.020 (5)0.0000.000 (4)0.000
C80.077 (10)0.026 (6)0.021 (6)0.0000.016 (6)0.000
C90.026 (6)0.046 (7)0.036 (6)0.0000.017 (5)0.000
C100.022 (6)0.035 (6)0.031 (6)0.0000.005 (5)0.000
C110.018 (5)0.014 (4)0.018 (5)0.0000.001 (4)0.000
C120.021 (5)0.018 (5)0.023 (5)0.0000.003 (4)0.000
Geometric parameters (Å, º) top
V1—O11.607 (7)C2—H20.9300
V1—O3i2.000 (4)C3—C41.359 (14)
V1—O3ii2.000 (4)C3—H30.9300
V1—O41.964 (7)C4—C121.397 (13)
V1—N12.133 (8)C4—C51.424 (14)
V1—N22.288 (8)C5—C61.327 (15)
P1—O31.500 (5)C5—H50.9300
P1—O3iii1.500 (5)C6—C71.403 (15)
P1—O41.518 (7)C6—H60.9300
P1—O21.554 (7)C7—C111.402 (13)
O2—H2o0.85C7—C81.414 (15)
N1—C11.358 (12)C8—C91.395 (17)
N1—C121.364 (12)C8—H80.9300
N2—C101.300 (12)C9—C101.401 (15)
N2—C111.375 (12)C9—H90.9300
C1—C21.312 (16)C10—H100.9300
C1—H10.9300C11—C121.415 (13)
C2—C31.366 (16)
O1—V1—O3i98.3 (1)C1—C2—C3119.6 (11)
O1—V1—O3ii98.3 (1)C1—C2—H2120.2
O1—V1—O4104.5 (3)C3—C2—H2120.2
O1—V1—N193.8 (4)C4—C3—C2121.6 (11)
O1—V1—N2167.9 (4)C4—C3—H3119.2
O3i—V1—O3ii161.2 (3)C2—C3—H3119.2
O3i—V1—O492.2 (1)C3—C4—C12116.1 (10)
O3i—V1—N185.0 (1)C3—C4—C5125.8 (10)
O3i—V1—N281.0 (1)C12—C4—C5118.0 (9)
O3ii—V1—O492.2 (2)C6—C5—C4122.7 (10)
O3ii—V1—N185.0 (1)C6—C5—H5118.7
O3ii—V1—N281.0 (1)C4—C5—H5118.7
O4—V1—N1161.7 (3)C5—C6—C7120.5 (10)
O4—V1—N287.6 (3)C5—C6—H6119.7
N1—V1—N274.1 (3)C7—C6—H6119.7
O3—P1—O3iii107.9 (4)C11—C7—C6119.1 (9)
O3—P1—O4112.3 (2)C11—C7—C8116.6 (9)
O3iii—P1—O4112.3 (2)C6—C7—C8124.3 (10)
O3—P1—O2108.0 (3)C9—C8—C7119.9 (10)
O3iii—P1—O2108.0 (3)C9—C8—H8120.1
O4—P1—O2108.3 (4)C7—C8—H8120.1
P1—O2—H2o115.9C8—C9—C10118.0 (10)
P1—O3—V1ii141.7 (3)C8—C9—H9121.0
P1—O4—V1135.9 (4)C10—C9—H9121.0
C1—N1—C12116.6 (9)N2—C10—C9124.1 (10)
C1—N1—V1125.2 (7)N2—C10—H10117.9
C12—N1—V1118.2 (6)C9—C10—H10117.9
C10—N2—C11118.2 (8)N2—C11—C7123.2 (9)
C10—N2—V1128.5 (7)N2—C11—C12116.4 (8)
C11—N2—V1113.3 (6)C7—C11—C12120.4 (9)
C2—C1—N1123.3 (10)N1—C12—C4122.7 (9)
C2—C1—H1118.3N1—C12—C11118.0 (9)
N1—C1—H1118.3C4—C12—C11119.3 (9)
O3iii—P1—O3—V1ii164.9 (2)C1—C2—C3—C40.000 (5)
O4—P1—O3—V1ii40.7 (6)C2—C3—C4—C120.000 (4)
O2—P1—O3—V1ii78.7 (5)C2—C3—C4—C5180.000 (4)
O3—P1—O4—V1119.1 (2)C3—C4—C5—C6180.000 (2)
O3iii—P1—O4—V1119.1 (2)C12—C4—C5—C60.000 (3)
O2—P1—O4—V10.000 (2)C4—C5—C6—C70.000 (3)
O1—V1—O4—P10.000 (1)C5—C6—C7—C110.000 (2)
O3i—V1—O4—P199.13 (14)C5—C6—C7—C8180.000 (2)
O3ii—V1—O4—P199.13 (14)C11—C7—C8—C90.000 (3)
N1—V1—O4—P1180.000 (3)C6—C7—C8—C9180.000 (2)
N2—V1—O4—P1180.000 (1)C7—C8—C9—C100.000 (2)
O1—V1—N1—C10.000 (3)C11—N2—C10—C90.000 (3)
O4—V1—N1—C1180.000 (4)V1—N2—C10—C9180.000 (3)
O3i—V1—N1—C197.99 (14)C8—C9—C10—N20.000 (3)
O3ii—V1—N1—C197.99 (14)C10—N2—C11—C70.000 (3)
N2—V1—N1—C1180.000 (4)V1—N2—C11—C7180.000 (2)
O1—V1—N1—C12180.000 (2)C10—N2—C11—C12180.000 (2)
O4—V1—N1—C120.000 (5)V1—N2—C11—C120.000 (2)
O3i—V1—N1—C1282.01 (14)C6—C7—C11—N2180.000 (2)
O3ii—V1—N1—C1282.01 (14)C8—C7—C11—N20.000 (2)
N2—V1—N1—C120.000 (2)C6—C7—C11—C120.000 (3)
O1—V1—N2—C10180.000 (5)C8—C7—C11—C12180.000 (2)
O4—V1—N2—C100.000 (2)C1—N1—C12—C40.000 (3)
O3i—V1—N2—C1092.63 (14)V1—N1—C12—C4180.000 (2)
O3ii—V1—N2—C1092.63 (14)C1—N1—C12—C11180.000 (3)
N1—V1—N2—C10180.000 (3)V1—N1—C12—C110.000 (3)
O1—V1—N2—C110.000 (6)C3—C4—C12—N10.000 (3)
O4—V1—N2—C11180.000 (2)C5—C4—C12—N1180.000 (2)
O3i—V1—N2—C1187.37 (14)C3—C4—C12—C11180.000 (3)
O3ii—V1—N2—C1187.37 (14)C5—C4—C12—C110.000 (3)
N1—V1—N2—C110.000 (2)N2—C11—C12—N10.000 (3)
C12—N1—C1—C20.000 (5)C7—C11—C12—N1180.000 (2)
V1—N1—C1—C2180.000 (4)N2—C11—C12—C4180.000 (3)
N1—C1—C2—C30.000 (5)C7—C11—C12—C40.000 (3)
Symmetry codes: (i) x+2, y1/2, z+2; (ii) x+2, y+1, z+2; (iii) x, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2o···O10.852.132.92 (1)155
 

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