Ethyl­enediammonium gallic vanadium hydrogen sulfate monohydrate

The title compound, tetra­kis(ethylenediammonium) gallium trivanadium octa­kis(hydrogen sulfate) tetra­hydroxide tetra­hydrate, (C₂H₁₀N₂)₄[GaV₃(SO₄)₈(OH)₄]·4H₂O, was obtained hydro­thermally from an aqueous solution of VOSO₄, Ga₂O₃, ethyl­enediamine, glycol and sulfuric acid. The structure features a one-dimensional chain built from MO₆ octa­hedra (site symmetry , M = V or Ga) and bridging OH and SO₄ groups.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• Disorder in main residue
• R factor = 0.036
• wR factor = 0.098
• Data-to-parameter ratio = 12.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for         C1
PLAT301_ALERT_3_C Main Residue  Disorder .........................       8.00 Perc.
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M1
                    M1     O1
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M1
                    M1     O1
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M1
                    M1     O4
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M1
                    M1     O4
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M1
                    M1     O3
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M1
                    M1     O3
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M2
                    M2     O1
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M2
                    M2     O1
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M2
                    M2     O7
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M2
                    M2     O7
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M2
                    M2     O2
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........         M2
                    M2     O2
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

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

  15 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

tetrakis(thylenediammonium) gallium trivanadium octakis(hydrogen sulfate) tetrahydroxide tetrahydrate

Crystal data

(C2H10N2)4[GaV3(SO4)8(OH)4]·4H2O	F(000) = 704
Mr = 1379.68	Dx = 2.135 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 450 reflections
a = 6.9044 (1) Å	θ = 2.2–25.0°
b = 10.3038 (2) Å	µ = 1.77 mm^−1
c = 15.0875 (3) Å	T = 293 K
β = 90.847 (1)°	Rod-shaped, brown
V = 1073.23 (3) Å^3	0.20 × 0.11 × 0.10 mm
Z = 1

Data collection

Bruker APEXII CCD area-detector diffractometer	2118 independent reflections
Radiation source: fine-focus sealed tube	1690 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
ω scans	θmax = 26.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −8→8
Tmin = 0.718, Tmax = 0.843	k = −12→11
11551 measured reflections	l = −17→18

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.036	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.098	w = 1/[σ^2(Fo^2) + (0.0525P)^2 + 0.858P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max < 0.001
2118 reflections	Δρmax = 0.41 e Å^−3
167 parameters	Δρmin = −0.61 e Å^−3
3 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997a), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0098 (11)

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	Occ. (<1)
V1	0.5000	−0.5000	0.5000	0.0172 (2)	0.75
Ga1	0.5000	−0.5000	0.5000	0.0172 (2)	0.25
V2	0.0000	−0.5000	0.5000	0.0156 (2)	0.75
Ga2	0.0000	−0.5000	0.5000	0.0156 (2)	0.25
S1	−0.26026 (10)	−0.30497 (8)	0.37800 (5)	0.0190 (2)
S2	0.75148 (10)	−0.71787 (8)	0.39733 (5)	0.0178 (2)
O1	0.2483 (3)	−0.5051 (2)	0.44121 (15)	0.0194 (5)
H1O	0.243 (5)	−0.510 (3)	0.3867 (13)	0.023*
O2	−0.1099 (3)	−0.4060 (2)	0.39161 (13)	0.0215 (5)
O3	0.6049 (3)	−0.6127 (2)	0.39943 (13)	0.0198 (5)
O4	0.5704 (3)	−0.3369 (2)	0.43523 (14)	0.0238 (5)
O5	0.6767 (3)	−0.8334 (2)	0.44124 (16)	0.0317 (6)
O6	0.8072 (3)	−0.7460 (3)	0.30740 (14)	0.0369 (6)
O7	−0.0715 (3)	−0.6736 (2)	0.44828 (15)	0.0237 (5)
O8	−0.1855 (4)	−0.1796 (2)	0.40485 (19)	0.0384 (7)
O9	−0.3272 (4)	−0.3043 (3)	0.28663 (15)	0.0437 (8)
N1	0.2371 (4)	−0.1851 (3)	0.36920 (18)	0.0275 (7)
H1C	0.3168	−0.2408	0.3432	0.041*
H1D	0.1197	−0.1914	0.3444	0.041*
H1E	0.2303	−0.2036	0.4267	0.041*
N2	0.2608 (4)	0.1782 (3)	0.39194 (18)	0.0253 (6)
H2C	0.1812	0.2340	0.4179	0.038*
H2D	0.2705	0.1981	0.3348	0.038*
H2E	0.3773	0.1826	0.4178	0.038*
C1	0.3112 (6)	−0.0511 (4)	0.3581 (3)	0.0459 (11)
H1A	0.4403	−0.0449	0.3840	0.055*
H1B	0.3201	−0.0314	0.2954	0.055*
C2	0.1833 (5)	0.0448 (3)	0.4007 (3)	0.0332 (9)
H2A	0.1712	0.0236	0.4631	0.040*
H2B	0.0553	0.0405	0.3736	0.040*
O1W	0.2364 (6)	0.4907 (3)	0.2625 (2)	0.0515 (9)
H1WB	0.220 (7)	0.427 (4)	0.230 (3)	0.077*
H1WA	0.216 (7)	0.559 (3)	0.234 (3)	0.077*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0138 (3)	0.0180 (4)	0.0197 (4)	0.0004 (2)	0.0006 (3)	0.0014 (3)
Ga1	0.0138 (3)	0.0180 (4)	0.0197 (4)	0.0004 (2)	0.0006 (3)	0.0014 (3)
V2	0.0120 (3)	0.0164 (4)	0.0184 (4)	0.0003 (2)	0.0002 (3)	−0.0008 (3)
Ga2	0.0120 (3)	0.0164 (4)	0.0184 (4)	0.0003 (2)	0.0002 (3)	−0.0008 (3)
S1	0.0189 (4)	0.0209 (4)	0.0173 (4)	0.0015 (3)	0.0023 (3)	0.0052 (3)
S2	0.0172 (4)	0.0192 (4)	0.0170 (4)	0.0008 (3)	−0.0005 (3)	−0.0034 (3)
O1	0.0135 (10)	0.0278 (13)	0.0169 (11)	0.0009 (8)	0.0003 (9)	−0.0026 (9)
O2	0.0166 (10)	0.0254 (13)	0.0225 (11)	0.0034 (9)	0.0022 (9)	0.0034 (10)
O3	0.0176 (11)	0.0218 (12)	0.0199 (11)	0.0043 (9)	−0.0022 (8)	−0.0028 (9)
O4	0.0204 (11)	0.0218 (12)	0.0295 (12)	0.0033 (9)	0.0077 (9)	0.0066 (10)
O5	0.0280 (13)	0.0227 (13)	0.0443 (15)	−0.0020 (10)	−0.0016 (11)	0.0060 (11)
O6	0.0411 (14)	0.0503 (17)	0.0192 (12)	0.0152 (13)	0.0027 (10)	−0.0078 (11)
O7	0.0173 (11)	0.0200 (12)	0.0337 (13)	0.0035 (9)	−0.0087 (9)	−0.0077 (10)
O8	0.0308 (13)	0.0191 (13)	0.0652 (18)	−0.0062 (11)	0.0037 (13)	−0.0022 (12)
O9	0.0393 (15)	0.075 (2)	0.0167 (12)	0.0191 (14)	−0.0047 (10)	0.0056 (12)
N1	0.0331 (16)	0.0260 (16)	0.0233 (14)	0.0001 (13)	0.0000 (12)	−0.0015 (12)
N2	0.0229 (14)	0.0271 (16)	0.0259 (14)	−0.0012 (12)	0.0017 (11)	−0.0043 (13)
C1	0.051 (2)	0.029 (2)	0.059 (3)	−0.0051 (19)	0.026 (2)	−0.005 (2)
C2	0.0259 (18)	0.0274 (19)	0.047 (2)	0.0002 (15)	0.0101 (16)	0.0002 (18)
O1W	0.091 (3)	0.0384 (19)	0.0256 (15)	0.0124 (17)	−0.0022 (16)	−0.0014 (12)

Geometric parameters (Å, º)

M1—O1	1.940 (2)	S2—O7^iv	1.505 (2)
M1—O1^i	1.940 (2)	O4—S1^iv	1.500 (2)
M1—O4	2.007 (2)	O7—S2^iii	1.505 (2)
M1—O4^i	2.007 (2)	N1—C1	1.483 (5)
M1—O3^i	2.051 (2)	N1—H1C	0.8900
M1—O3	2.051 (2)	N1—H1D	0.8900
M2—O1	1.942 (2)	N1—H1E	0.8900
M2—O1^ii	1.942 (2)	N2—C2	1.482 (4)
M2—O7	2.010 (2)	N2—H2C	0.8900
M2—O7^ii	2.010 (2)	N2—H2D	0.8900
M2—O2	2.038 (2)	N2—H2E	0.8900
M2—O2^ii	2.038 (2)	C1—C2	1.479 (5)
S1—O8	1.447 (2)	C1—H1A	0.9700
S1—O9	1.448 (2)	C1—H1B	0.9700
S1—O2	1.482 (2)	C2—H2A	0.9700
S1—O4^iii	1.500 (2)	C2—H2B	0.9700
S2—O6	1.445 (2)	O1W—H1WB	0.83 (4)
S2—O5	1.460 (2)	O1W—H1WA	0.84 (4)
S2—O3	1.484 (2)
O1—V1—O1^i	180.00 (12)	O6—S2—O3	110.97 (14)
O1—V1—O4	91.24 (9)	O5—S2—O3	109.87 (13)
O1^i—V1—O4	88.76 (9)	O6—S2—O7^iv	108.36 (14)
O1—V1—O4^i	88.76 (9)	O5—S2—O7^iv	107.76 (14)
O1^i—V1—O4^i	91.24 (9)	O3—S2—O7^iv	108.48 (12)
O4—V1—O4^i	180.0	V1—O1—V2	125.53 (12)
O1—V1—O3^i	91.71 (8)	V1—O1—H1O	119 (3)
O1^i—V1—O3^i	88.29 (8)	V2—O1—H1O	116 (3)
O4—V1—O3^i	88.68 (8)	S1—O2—V2	134.17 (12)
O4^i—V1—O3^i	91.32 (8)	S2—O3—V1	132.67 (13)
O1—V1—O3	88.29 (8)	S1^iv—O4—V1	131.33 (13)
O1^i—V1—O3	91.71 (8)	S2^iii—O7—V2	131.35 (13)
O4—V1—O3	91.32 (8)	C1—N1—H1C	109.5
O4^i—V1—O3	88.68 (8)	C1—N1—H1D	109.5
O3^i—V1—O3	180.0	H1C—N1—H1D	109.5
O1—V2—O1^ii	180.00 (12)	C1—N1—H1E	109.5
O1—V2—O7	90.69 (9)	H1C—N1—H1E	109.5
O1^ii—V2—O7	89.31 (9)	H1D—N1—H1E	109.5
O1—V2—O7^ii	89.31 (9)	C2—N2—H2C	109.5
O1^ii—V2—O7^ii	90.69 (9)	C2—N2—H2D	109.5
O7—V2—O7^ii	180.0	H2C—N2—H2D	109.5
O1—V2—O2	88.11 (8)	C2—N2—H2E	109.5
O1^ii—V2—O2	91.89 (8)	H2C—N2—H2E	109.5
O7—V2—O2	91.43 (8)	H2D—N2—H2E	109.5
O7^ii—V2—O2	88.57 (9)	C2—C1—N1	111.3 (3)
O1—V2—O2^ii	91.89 (8)	C2—C1—H1A	109.4
O1^ii—V2—O2^ii	88.11 (8)	N1—C1—H1A	109.4
O7—V2—O2^ii	88.57 (9)	C2—C1—H1B	109.4
O7^ii—V2—O2^ii	91.43 (9)	N1—C1—H1B	109.4
O2—V2—O2^ii	180.0	H1A—C1—H1B	108.0
O8—S1—O9	111.69 (17)	C1—C2—N2	111.2 (3)
O8—S1—O2	110.01 (14)	C1—C2—H2A	109.4
O9—S1—O2	110.39 (14)	N2—C2—H2A	109.4
O8—S1—O4^iii	108.23 (14)	C1—C2—H2B	109.4
O9—S1—O4^iii	107.98 (14)	N2—C2—H2B	109.4
O2—S1—O4^iii	108.43 (12)	H2A—C2—H2B	108.0
O6—S2—O5	111.29 (16)	H1WB—O1W—H1WA	110 (6)

Symmetry codes: (i) −x+1, −y−1, −z+1; (ii) −x, −y−1, −z+1; (iii) x−1, y, z; (iv) x+1, y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WB···O8^v	0.83 (4)	2.32 (4)	3.091 (4)	155 (4)
O1W—H1WB···O9^v	0.83 (4)	2.51 (4)	3.193 (4)	141 (4)
N1—H1D···O8	0.89	2.31	2.975 (4)	131
N1—H1E···O5^i	0.89	2.12	2.919 (4)	149
O1W—H1WA···O6^vi	0.84 (4)	2.11 (3)	2.925 (4)	165 (4)
O1—H1O···O1W^vii	0.82 (2)	1.87 (2)	2.697 (4)	176 (3)
N2—H2C···O7^viii	0.89	2.05	2.894 (4)	159
N2—H2D···O9^v	0.89	1.88	2.746 (4)	164
N2—H2E···O5^viii	0.89	2.10	2.958 (4)	162

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