Penta­aqua­oxovanadium(IV) bis­(sulfonatosalicylic acid) dihydrate

In the title compound, [VO(H₂O)₅](C₇H₅O₆S)₂·2H₂O, the V^IV atom is six-coordinated by O atoms (one vanadyl neighbour and five water mol­ecules) in a distorted octahedral configuration. The complex also contains two uncoordinated sulfosal­icylate anions and two uncoordinated water mol­ecules. Numerous O—H...O hydrogen bonds result in the formation of a three-dimensional network.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.033
• wR factor = 0.072
• Data-to-parameter ratio = 10.5

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  V1     -   O13     ..       5.30 su
PLAT417_ALERT_2_C Short Inter D-H..H-D       H20    ..  H25     ..       2.14 Ang.
PLAT731_ALERT_1_C Bond    Calc     0.89(3), Rep   0.894(10) ......       3.00 su-Rat
              O17  -H22     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.89(3), Rep   0.894(10) ......       3.00 su-Rat
              O20  -H28     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.89(3), Rep   0.894(10) ......       3.00 su-Rat
              O17  -H22     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.89(3), Rep   0.894(10) ......       3.00 su-Rat
              O20  -H28     1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.74(3), Rep   1.735(11) ......       2.73 su-Rat
              H22  -O4      1.555   1.565

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 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
   0 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL.

Pentaaquaoxovanadium(IV) bis(sulfosalicylate) dihydrate

Crystal data

[VO(H2O)5]2(C7H5O6S)·2H2O	F(000) = 1292
Mr = 627.39	Dx = 1.756 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2823 reflections
a = 12.873 (11) Å	θ = 5.0–26.3°
b = 6.777 (6) Å	µ = 0.69 mm^−1
c = 27.28 (2) Å	T = 298 K
β = 94.393 (12)°	Block, blue
V = 2373 (3) Å^3	0.22 × 0.19 × 0.11 mm
Z = 4

Data collection

CCD area detector diffractometer	4087 independent reflections
Radiation source: fine-focus sealed tube	2842 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.031
φ and ω scans	θmax = 25.0°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −11→15
Tmin = 0.863, Tmax = 0.928	k = −7→8
11246 measured reflections	l = −32→31

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.072	H atoms treated by a mixture of independent and constrained refinement
S = 0.90	w = 1/[σ^2(Fo^2) + (0.0294P)^2]
4087 reflections	(Δ/σ)max < 0.001
390 parameters	Δρmax = 0.37 e Å^−3
21 restraints	Δρmin = −0.26 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
V1	0.25359 (3)	0.67811 (6)	0.493887 (14)	0.02858 (13)
O1	0.30770 (12)	0.1429 (3)	0.18819 (6)	0.0404 (5)
H1	0.2796	0.1444	0.1602	0.061*
O2	0.45216 (13)	0.1354 (3)	0.14768 (6)	0.0423 (5)
O3	0.33453 (14)	0.3142 (2)	0.37504 (6)	0.0412 (5)
O4	0.33697 (14)	−0.0373 (3)	0.37529 (6)	0.0434 (5)
O5	0.47773 (14)	0.1422 (2)	0.41847 (6)	0.0428 (5)
O6	0.63290 (13)	0.1409 (2)	0.19963 (6)	0.0420 (5)
H6	0.5938	0.1386	0.1745	0.063*
O7	0.19299 (13)	0.3451 (3)	0.29631 (6)	0.0431 (5)
H7	0.2212	0.3429	0.3243	0.065*
O8	0.04854 (14)	0.3409 (3)	0.33681 (7)	0.0448 (5)
O9	0.16924 (14)	0.1887 (3)	0.10931 (6)	0.0446 (5)
O10	0.17127 (14)	0.5401 (3)	0.11511 (6)	0.0472 (5)
O11	0.03217 (13)	0.3773 (3)	0.06599 (6)	0.0423 (5)
O12	−0.13217 (14)	0.3390 (3)	0.28462 (7)	0.0478 (5)
H12	−0.0931	0.3394	0.3098	0.072*
O13	0.23697 (13)	0.9084 (3)	0.49103 (6)	0.0457 (5)
O14	0.23483 (14)	0.6477 (3)	0.56692 (6)	0.0374 (4)
O15	0.26747 (14)	0.3588 (2)	0.49502 (6)	0.0377 (5)
O16	0.40983 (13)	0.6618 (3)	0.51156 (7)	0.0388 (5)
O17	0.28594 (16)	0.6444 (3)	0.42276 (6)	0.0419 (5)
O18	0.10022 (14)	0.6065 (3)	0.47759 (7)	0.0411 (5)
O19	0.44545 (15)	0.2290 (3)	0.55028 (7)	0.0426 (5)
O20	0.08320 (17)	0.2493 (3)	0.43786 (8)	0.0517 (5)
S1	0.39957 (5)	0.13904 (9)	0.37718 (2)	0.02866 (16)
S2	0.10661 (5)	0.36646 (9)	0.10878 (2)	0.03077 (17)
C1	0.40921 (19)	0.1377 (3)	0.18629 (9)	0.0297 (6)
C2	0.46693 (17)	0.1353 (3)	0.23509 (8)	0.0242 (5)
C3	0.41381 (18)	0.1343 (3)	0.27796 (8)	0.0268 (6)
H3	0.3414	0.1309	0.2758	0.032*
C4	0.46878 (18)	0.1382 (3)	0.32357 (8)	0.0271 (6)
C5	0.57730 (18)	0.1421 (3)	0.32692 (9)	0.0321 (6)
H5	0.6141	0.1453	0.3576	0.038*
C6	0.63006 (19)	0.1412 (3)	0.28496 (9)	0.0349 (6)
H6A	0.7025	0.1423	0.2875	0.042*
C7	0.57629 (18)	0.1387 (3)	0.23899 (9)	0.0284 (6)
C8	0.09139 (19)	0.3444 (3)	0.29828 (10)	0.0327 (6)
C9	0.03432 (18)	0.3469 (3)	0.24948 (9)	0.0295 (6)
C10	0.08759 (18)	0.3540 (3)	0.20682 (9)	0.0296 (6)
H10	0.1600	0.3580	0.2093	0.035*
C11	0.03437 (18)	0.3551 (3)	0.16112 (9)	0.0296 (6)
C12	−0.07446 (19)	0.3497 (3)	0.15725 (10)	0.0362 (6)
H12A	−0.1107	0.3490	0.1264	0.043*
C13	−0.12813 (19)	0.3454 (4)	0.19901 (10)	0.0387 (7)
H13	−0.2006	0.3437	0.1961	0.046*
C14	−0.07547 (19)	0.3435 (3)	0.24526 (10)	0.0331 (6)
H15	0.211 (2)	0.752 (3)	0.5828 (10)	0.075 (11)*
H16	0.205 (2)	0.537 (2)	0.5771 (11)	0.083 (12)*
H17	0.2204 (15)	0.278 (3)	0.4794 (9)	0.064 (10)*
H18	0.3198 (16)	0.291 (4)	0.5103 (10)	0.082 (12)*
H19	0.4382 (18)	0.707 (4)	0.5404 (5)	0.053 (9)*
H20	0.4548 (18)	0.687 (4)	0.4885 (7)	0.087 (12)*
H21	0.307 (2)	0.535 (2)	0.4094 (10)	0.067 (10)*
H22	0.308 (3)	0.753 (3)	0.4082 (12)	0.110 (15)*
H23	0.0859 (19)	0.4871 (19)	0.4650 (9)	0.053 (9)*
H24	0.0572 (19)	0.695 (3)	0.4623 (10)	0.075 (11)*
H25	0.470 (2)	0.108 (2)	0.5570 (10)	0.081 (12)*
H26	0.433 (3)	0.290 (4)	0.5784 (7)	0.095 (13)*
H27	0.086 (3)	0.269 (5)	0.4055 (5)	0.108 (15)*
H28	0.042 (2)	0.147 (4)	0.4435 (11)	0.091 (13)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0335 (2)	0.0252 (2)	0.0269 (2)	−0.0003 (2)	0.00149 (18)	−0.00046 (18)
O1	0.0297 (10)	0.0618 (13)	0.0286 (10)	0.0046 (9)	−0.0040 (8)	−0.0017 (8)
O2	0.0431 (11)	0.0572 (13)	0.0276 (10)	0.0042 (9)	0.0091 (8)	0.0027 (8)
O3	0.0507 (11)	0.0431 (11)	0.0299 (10)	0.0126 (9)	0.0046 (8)	−0.0023 (8)
O4	0.0548 (12)	0.0439 (12)	0.0322 (10)	−0.0184 (10)	0.0064 (8)	−0.0007 (8)
O5	0.0496 (12)	0.0487 (12)	0.0280 (10)	0.0003 (9)	−0.0115 (8)	−0.0012 (8)
O6	0.0314 (10)	0.0552 (13)	0.0408 (11)	0.0009 (9)	0.0114 (8)	0.0038 (9)
O7	0.0294 (10)	0.0645 (14)	0.0347 (10)	0.0033 (9)	−0.0017 (8)	−0.0043 (9)
O8	0.0458 (12)	0.0529 (13)	0.0368 (11)	0.0015 (9)	0.0096 (9)	0.0003 (9)
O9	0.0507 (12)	0.0492 (12)	0.0333 (10)	0.0148 (10)	−0.0001 (8)	−0.0041 (8)
O10	0.0521 (12)	0.0522 (12)	0.0372 (11)	−0.0230 (10)	0.0028 (9)	0.0030 (9)
O11	0.0421 (11)	0.0470 (12)	0.0358 (10)	−0.0019 (9)	−0.0100 (8)	0.0015 (8)
O12	0.0323 (10)	0.0634 (14)	0.0490 (12)	−0.0006 (9)	0.0128 (9)	0.0038 (10)
O13	0.0623 (13)	0.0324 (10)	0.0434 (11)	0.0046 (9)	0.0106 (9)	0.0001 (8)
O14	0.0498 (12)	0.0320 (11)	0.0312 (10)	−0.0014 (10)	0.0089 (8)	−0.0026 (9)
O15	0.0421 (12)	0.0272 (10)	0.0426 (11)	−0.0004 (9)	−0.0052 (9)	−0.0010 (9)
O16	0.0313 (10)	0.0509 (13)	0.0339 (11)	−0.0066 (9)	0.0003 (9)	−0.0082 (9)
O17	0.0634 (13)	0.0334 (12)	0.0301 (11)	−0.0006 (10)	0.0121 (9)	−0.0011 (9)
O18	0.0326 (11)	0.0384 (12)	0.0508 (12)	−0.0004 (10)	−0.0061 (9)	−0.0004 (10)
O19	0.0495 (12)	0.0431 (13)	0.0344 (11)	0.0045 (10)	−0.0015 (9)	0.0039 (9)
O20	0.0650 (15)	0.0449 (14)	0.0440 (14)	−0.0135 (11)	−0.0041 (11)	−0.0042 (10)
S1	0.0337 (4)	0.0301 (4)	0.0216 (3)	−0.0006 (3)	−0.0014 (2)	0.0000 (3)
S2	0.0300 (4)	0.0324 (4)	0.0291 (4)	−0.0014 (3)	−0.0034 (3)	0.0006 (3)
C1	0.0334 (15)	0.0238 (14)	0.0320 (15)	0.0010 (11)	0.0047 (11)	0.0004 (11)
C2	0.0247 (13)	0.0226 (13)	0.0256 (13)	0.0015 (10)	0.0027 (10)	0.0015 (10)
C3	0.0222 (13)	0.0253 (14)	0.0328 (14)	0.0000 (10)	0.0017 (10)	−0.0014 (10)
C4	0.0301 (14)	0.0239 (14)	0.0271 (13)	−0.0010 (11)	0.0018 (10)	0.0010 (10)
C5	0.0284 (14)	0.0332 (15)	0.0333 (14)	−0.0029 (12)	−0.0057 (11)	0.0017 (11)
C6	0.0229 (13)	0.0342 (16)	0.0469 (17)	0.0007 (11)	−0.0009 (12)	0.0019 (12)
C7	0.0304 (14)	0.0202 (13)	0.0357 (15)	0.0007 (11)	0.0099 (11)	0.0037 (10)
C8	0.0318 (15)	0.0266 (15)	0.0406 (16)	0.0012 (12)	0.0076 (12)	−0.0027 (11)
C9	0.0260 (14)	0.0227 (14)	0.0397 (15)	0.0007 (11)	0.0025 (11)	0.0007 (11)
C10	0.0240 (13)	0.0262 (14)	0.0387 (15)	−0.0004 (11)	0.0030 (11)	0.0002 (11)
C11	0.0291 (14)	0.0229 (14)	0.0368 (14)	−0.0009 (11)	0.0018 (11)	0.0021 (11)
C12	0.0303 (15)	0.0349 (16)	0.0418 (16)	−0.0027 (12)	−0.0068 (12)	0.0032 (12)
C13	0.0225 (14)	0.0385 (17)	0.0549 (18)	−0.0019 (12)	0.0012 (12)	0.0061 (13)
C14	0.0269 (14)	0.0271 (15)	0.0463 (16)	−0.0012 (11)	0.0088 (12)	0.0030 (12)

Geometric parameters (Å, º)

V1—O13	1.576 (2)	O17—H22	0.894 (10)
V1—O17	2.028 (2)	O18—H23	0.893 (10)
V1—O16	2.035 (2)	O18—H24	0.895 (10)
V1—O14	2.036 (2)	O19—H25	0.891 (10)
V1—O18	2.049 (2)	O19—H26	0.894 (10)
V1—O15	2.171 (2)	O20—H27	0.896 (10)
O1—C1	1.312 (3)	O20—H28	0.894 (10)
O1—H1	0.8200	S1—C4	1.770 (3)
O2—C1	1.227 (3)	S2—C11	1.764 (3)
O3—S1	1.4512 (19)	C1—C2	1.474 (3)
O4—S1	1.4403 (19)	C2—C3	1.399 (3)
O5—S1	1.4520 (19)	C2—C7	1.404 (3)
O6—C7	1.343 (3)	C3—C4	1.384 (3)
O6—H6	0.8200	C3—H3	0.9300
O7—C8	1.313 (3)	C4—C5	1.393 (3)
O7—H7	0.8200	C5—C6	1.375 (4)
O8—C8	1.224 (3)	C5—H5	0.9300
O9—S2	1.449 (2)	C6—C7	1.385 (3)
O10—S2	1.444 (2)	C6—H6A	0.9300
O11—S2	1.4542 (19)	C8—C9	1.471 (4)
O12—C14	1.344 (3)	C9—C10	1.396 (3)
O12—H12	0.8200	C9—C14	1.409 (3)
O14—H15	0.896 (10)	C10—C11	1.376 (3)
O14—H16	0.897 (10)	C10—H10	0.9300
O15—H17	0.898 (10)	C11—C12	1.397 (3)
O15—H18	0.893 (10)	C12—C13	1.377 (4)
O16—H19	0.897 (10)	C12—H12A	0.9300
O16—H20	0.905 (10)	C13—C14	1.386 (4)
O17—H21	0.881 (10)	C13—H13	0.9300
O13—V1—O17	95.82 (9)	O10—S2—C11	105.88 (11)
O13—V1—O16	101.16 (8)	O9—S2—C11	106.43 (11)
O17—V1—O16	87.07 (9)	O11—S2—C11	107.22 (13)
O13—V1—O14	97.05 (8)	O2—C1—O1	123.4 (2)
O17—V1—O14	166.72 (8)	O2—C1—C2	123.1 (2)
O16—V1—O14	87.24 (8)	O1—C1—C2	113.5 (2)
O13—V1—O18	95.67 (9)	C3—C2—C7	119.2 (2)
O17—V1—O18	91.76 (9)	C3—C2—C1	120.7 (2)
O16—V1—O18	163.16 (8)	C7—C2—C1	120.1 (2)
O14—V1—O18	90.22 (8)	C4—C3—C2	120.2 (2)
O13—V1—O15	176.44 (8)	C4—C3—H3	119.9
O17—V1—O15	83.02 (7)	C2—C3—H3	119.9
O16—V1—O15	82.16 (7)	C3—C4—C5	120.0 (2)
O14—V1—O15	84.33 (7)	C3—C4—S1	119.21 (19)
O18—V1—O15	81.02 (8)	C5—C4—S1	120.77 (18)
C1—O1—H1	109.5	C6—C5—C4	120.1 (2)
C7—O6—H6	109.5	C6—C5—H5	119.9
C8—O7—H7	109.5	C4—C5—H5	119.9
C14—O12—H12	109.5	C5—C6—C7	120.6 (2)
V1—O14—H15	117.7 (19)	C5—C6—H6A	119.7
V1—O14—H16	118.3 (19)	C7—C6—H6A	119.7
H15—O14—H16	110 (2)	O6—C7—C6	117.4 (2)
V1—O15—H17	123.1 (17)	O6—C7—C2	122.8 (2)
V1—O15—H18	125.5 (18)	C6—C7—C2	119.8 (2)
H17—O15—H18	111 (2)	O8—C8—O7	123.4 (2)
V1—O16—H19	121.2 (16)	O8—C8—C9	123.4 (2)
V1—O16—H20	119.9 (18)	O7—C8—C9	113.1 (2)
H19—O16—H20	107.9 (19)	C10—C9—C14	119.1 (2)
V1—O17—H21	125.7 (18)	C10—C9—C8	120.8 (2)
V1—O17—H22	115 (2)	C14—C9—C8	120.1 (2)
H21—O17—H22	113 (2)	C11—C10—C9	120.9 (2)
V1—O18—H23	117.7 (16)	C11—C10—H10	119.6
V1—O18—H24	119.7 (19)	C9—C10—H10	119.6
H23—O18—H24	108.8 (18)	C10—C11—C12	119.7 (2)
H25—O19—H26	109 (2)	C10—C11—S2	118.5 (2)
H27—O20—H28	111 (2)	C12—C11—S2	121.84 (19)
O4—S1—O3	110.97 (13)	C13—C12—C11	120.1 (2)
O4—S1—O5	113.12 (11)	C13—C12—H12A	119.9
O3—S1—O5	112.48 (11)	C11—C12—H12A	119.9
O4—S1—C4	106.48 (11)	C12—C13—C14	120.8 (2)
O3—S1—C4	107.14 (11)	C12—C13—H13	119.6
O5—S1—C4	106.17 (13)	C14—C13—H13	119.6
O10—S2—O9	111.17 (13)	O12—C14—C13	118.0 (2)
O10—S2—O11	113.14 (11)	O12—C14—C9	122.5 (2)
O9—S2—O11	112.46 (11)	C13—C14—C9	119.4 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O9	0.82	1.93	2.705 (3)	157
O6—H6···O2	0.82	1.91	2.630 (3)	146
O7—H7···O3	0.82	1.94	2.716 (3)	157
O12—H12···O8	0.82	1.91	2.633 (3)	146
O14—H15···O10^i	0.90 (1)	1.76 (1)	2.653 (3)	177 (3)
O14—H16···O9^ii	0.90 (1)	1.84 (1)	2.720 (3)	166 (3)
O15—H17···O20	0.90 (1)	2.03 (2)	2.836 (3)	148 (2)
O15—H18···O19	0.89 (1)	1.93 (1)	2.787 (3)	161 (3)
O16—H19···O5^iii	0.90 (1)	1.81 (1)	2.661 (3)	157 (2)
O16—H20···O19^iii	0.91 (1)	1.82 (1)	2.710 (3)	170 (3)
O17—H21···O3	0.88 (1)	1.81 (1)	2.687 (3)	171 (3)
O17—H22···O4^iv	0.89 (1)	1.74 (1)	2.625 (3)	173 (4)
O18—H23···O20	0.89 (1)	1.77 (1)	2.655 (3)	169 (2)
O18—H24···O11^v	0.90 (1)	1.82 (1)	2.716 (3)	177 (3)
O19—H25···O5^vi	0.89 (1)	1.93 (1)	2.812 (3)	172 (3)
O19—H26···O2^ii	0.89 (1)	1.96 (2)	2.807 (3)	159 (3)
O20—H27···O8	0.90 (1)	1.96 (2)	2.828 (4)	163 (3)
O20—H28···O11^vii	0.89 (1)	2.07 (2)	2.924 (3)	160 (3)

Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, −y+1/2, z+1/2; (iii) −x+1, −y+1, −z+1; (iv) x, y+1, z; (v) −x, y+1/2, −z+1/2; (vi) −x+1, −y, −z+1; (vii) −x, y−1/2, −z+1/2.