Crystal structure of tetra­guanidinium [hexa­hydrogen hexa­arsenato(V)tetra­vanadate(V)] tetra­hydrate

The complete polyoxidometallate anion in the title compound, (CH₆N₃)₄[H₆V₄As₆O₃₀]·4H₂O, is generated by crystallographic inversion symmetry. The polyhedral building units are distorted VO₆ octa­hedra and AsO₃OH tetra­hedra. The VO₆ units feature a short formal V=O double bond and are linked by a common edge. Two such V₂O₆ double octahedral units are linked by four isolated AsO₃OH tetra­hedra to complete the anion, which features two inter­nal O—H...O hydrogen bonds. In the crystal, O—H...O hydrogen bonds between the polyoxidometallate anions generate (01-1) sheets. The sheets are connected by cation-to-cluster N—H...O hydrogen bonds, and cation-to-water N—H...O links also occur. The O atom of one of the water mol­ecules is disordered over two sites in a 0.703 (17):0.297 (17) ratio.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](N-C) = 0.012 Å
• H-atom completeness 89%
• Disorder in solvent or counterion
• R factor = 0.047
• wR factor = 0.129
• Data-to-parameter ratio = 18.1

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check

Alert level C
RADNW01_ALERT_1_C  The radiation wavelength lies outside the expected range
            for the supplied radiation type. Expected range 0.71065-0.71075
            Wavelength given =    0.70173
PLAT041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
PLAT043_ALERT_1_C Calculated and Reported Mol. Weight Differ by ..       4.03 Check
PLAT051_ALERT_1_C Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       3.64 %
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check
PLAT125_ALERT_4_C No '_symmetry_space_group_name_Hall' Given .....     Please Do !
PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          1
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of          C1 Check
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of          C2 Check
PLAT420_ALERT_2_C D-H Without Acceptor       N6     -   H6A    ...     Please Check
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .         34 Ang3
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600         10 Why ?
PLAT971_ALERT_2_C Check Calcd Residual Density  2.75A From    O2WA       1.82 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  0.75A From    O2WA       1.24 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  1.06A From     O1W       0.63 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  0.70A From     O1W       0.58 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.94A From     O15      -0.65 eA-3

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C4 H34 As6 N12 O34 V4
            Atom count from _chemical_formula_moiety:C4 H38 As6 N12 O34 V4
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C4 H34 As6 N12 O34 V4
            Atom count from the _atom_site data:  C4 H30 As6 N12 O34 V4
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    1
           From the CIF: _chemical_formula_sum  C4 H34 As6 N12 O34 V4
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C          4.00      4.00    0.00
           H         34.00     30.00    4.00
           As         6.00      6.00    0.00
           N         12.00     12.00    0.00
           O         34.00     34.00    0.00
           V          4.00      4.00    0.00
PLAT005_ALERT_5_G No _iucr_refine_instructions_details  in the CIF     Please Do !
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         15 Why ?
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka ..     0.7017 Ang.
PLAT154_ALERT_1_G The su's on the Cell Angles are Equal ..........    0.00100 Degree
PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check
PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check
PLAT302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =         10 Note
PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....       O2WA Check
PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) .....       O2WB Check
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         11 Do !
            O8  -V2  -O3  -AS2  -152.00  2.00   1.555   1.555   1.555   2.566
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         16 Do !
            O8  -V2  -O3  -V1     37.00  3.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         21 Do !
            O1  -V1  -O3  -AS2    91.00 11.00   1.555   1.555   1.555   2.566
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         26 Do !
            O1  -V1  -O3  -V2    -97.00 10.00   1.555   1.555   1.555   1.555
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          2 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         34 Note
PLAT984_ALERT_1_G The As-f'=     0.050 Deviates from the B&C-Value      0.074
PLAT985_ALERT_1_G The As-f"=     2.006 Deviates from the B&C-Value      1.974

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
  17 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  22 ALERT level G = General information/check it is not something unexpected

  14 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  11 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
  11 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check


checkCIF publication errors

Alert level A
PUBL005_ALERT_1_A  _publ_contact_author_email, _publ_contact_author_fax and
            _publ_contact_author_phone are all missing.
            At least one of these should be present.
PUBL006_ALERT_1_A  _publ_requested_journal is missing
            e.g. 'Acta Crystallographica Section C'

   2 ALERT level A = Data missing that is essential or data in wrong format
   0 ALERT level G = General alerts. Data that may be required is missing

---

S1. Synthesis and crystallization

0.91 g of V₂O₅ and 0.90 g of (CN₃H₆)₂CO₃ were added to 10 ml of a 0.1 M H₃AsO₄ solution and placed in a Teflon-lined hydro­thermal vessel, which was heated to 423 K for 24 hours. After cooling to room temperature over several hours, solids were recovered by vacuum filtration to yield a few orange blocks of the title compound accompanied by an unidentified brown powder.

S2. Refinement

The H atoms were located in different maps (O—H) or geometrically placed (N—H) and refined as riding atoms with U_iso(H) = 1.2U_eq(carrier). The water-molecule H atoms could not be located in the present experiment. One of the water molecule O atoms is disordered over two adjacent sites in a 0.703 (17):0.297 (17) ratio.

Related literature

For crystal structures containing the same type of anion accompanied by different counter-cations, see: Durif & Averbuch-Pouchot (1979); Nenoff et al. (1994); Bremner & Harrison (2002). The site symmetries of these anions include 1 (as seen for the title compound) as well as 2/m and mmm.

Computing details

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and ATOMS (Dowty, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures

	Fig. 1. The molecular structure of the (V4As6O30H6)^4- anion in the title compound showing 50% displacement ellipsoids. [Symmetry code: (i) –x, 1–y, 1–z.]
	Fig. 2. The packing of the title compound viewed down [100] with the anion shown in polyhedral representation (VO6 octahedra orange, AsO4 tetrahedra green). O—H···O hydrogen bonds within and between the anions are shown as yellow lines.

Tetraguanidinium [hexahydrogen hexaarsenato(V)tetravanadate(V)] tetrahydrate

Crystal data

(CH6N3)4[H6V4As6O30]·4H2O	Z = 1
Mr = 1447.71	F(000) = 704
Triclinic, P1	Dx = 2.244 Mg m^−3
a = 10.0403 (5) Å	Mo Kα radiation, λ = 0.70173 Å
b = 11.0199 (6) Å	Cell parameters from 3266 reflections
c = 11.9806 (6) Å	θ = 2.3–27.5°
α = 114.892 (1)°	µ = 5.56 mm^−1
β = 94.696 (1)°	T = 293 K
γ = 111.751 (1)°	Block, orange
V = 1071.39 (10) Å^3	0.30 × 0.20 × 0.20 mm

Data collection

Bruker SMART CCD diffractometer	4909 independent reflections
Radiation source: fine-focus sealed tube	3655 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.035
ω scans	θmax = 27.2°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −13→13
Tmin = 0.287, Tmax = 0.403	k = −14→12
8711 measured reflections	l = −11→15

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)] = 0.047	Hydrogen site location: mixed
wR(F^2) = 0.129	H-atom parameters constrained
S = 0.99	w = 1/[σ^2(Fo^2) + (0.0766P)^2] where P = (Fo^2 + 2Fc^2)/3
4909 reflections	(Δ/σ)max < 0.001
271 parameters	Δρmax = 1.79 e Å^−3
0 restraints	Δρmin = −1.25 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	Occ. (<1)
V1	0.26837 (10)	0.46285 (10)	0.57607 (9)	0.0176 (2)
V2	0.05032 (10)	0.50770 (11)	0.74922 (9)	0.0193 (2)
As1	0.26156 (6)	0.46227 (6)	0.30244 (6)	0.02044 (15)
As2	−0.08161 (6)	0.30204 (6)	0.44111 (5)	0.01626 (14)
As3	0.39072 (6)	0.77706 (6)	0.84192 (5)	0.01955 (15)
O1	0.3661 (5)	0.3738 (5)	0.5506 (4)	0.0282 (10)
O2	0.1882 (4)	0.4284 (4)	0.6880 (4)	0.0192 (8)
O3	0.1265 (4)	0.6002 (4)	0.6171 (4)	0.0194 (8)
O4	0.4243 (4)	0.6617 (4)	0.7138 (4)	0.0202 (8)
O5	0.0880 (4)	0.3108 (4)	0.4329 (4)	0.0198 (8)
O6	0.3215 (4)	0.5543 (4)	0.4605 (4)	0.0211 (8)
O7	−0.0827 (4)	0.6107 (5)	0.7760 (4)	0.0254 (9)
O8	0.0098 (5)	0.4435 (5)	0.8461 (4)	0.0328 (10)
O9	−0.1059 (4)	0.3374 (4)	0.5863 (4)	0.0216 (8)
O10	0.2301 (4)	0.7032 (4)	0.8748 (4)	0.0253 (9)
O11	0.3741 (5)	0.5860 (6)	0.2582 (5)	0.0389 (12)
O12	0.2976 (5)	0.3108 (5)	0.2403 (4)	0.0299 (10)
H12	0.4043	0.3389	0.2643	0.036*
O13	0.4138 (4)	0.9295 (4)	0.8315 (4)	0.0260 (9)
O14	0.5335 (5)	0.8266 (5)	0.9655 (4)	0.0319 (10)
H14	0.5560	0.9049	1.0518	0.038*
O15	−0.2016 (5)	0.1152 (4)	0.3450 (4)	0.0290 (10)
H15	−0.2710	0.1031	0.2766	0.035*
C1	0.6359 (8)	−0.0343 (7)	0.5654 (7)	0.0336 (15)
N1	0.5480 (7)	−0.1219 (6)	0.6055 (6)	0.0441 (16)
H1A	0.5002	−0.2169	0.5551	0.053*
H1B	0.5389	−0.0834	0.6818	0.053*
N2	0.6494 (8)	−0.0929 (7)	0.4497 (7)	0.0530 (19)
H2A	0.7044	−0.0363	0.4229	0.064*
H2B	0.6033	−0.1882	0.4001	0.064*
N3	0.7054 (8)	0.1105 (7)	0.6418 (7)	0.0510 (18)
H3A	0.7607	0.1680	0.6159	0.061*
H3B	0.6959	0.1482	0.7180	0.061*
C2	0.9422 (9)	0.0768 (8)	0.8896 (7)	0.0406 (17)
N4	0.8450 (8)	0.0292 (9)	0.9471 (8)	0.069 (2)
H4A	0.7854	−0.0646	0.9131	0.082*
H4B	0.8411	0.0919	1.0186	0.082*
N5	1.0309 (9)	0.2208 (7)	0.9432 (7)	0.061 (2)
H5A	1.0945	0.2540	0.9067	0.073*
H5B	1.0254	0.2818	1.0147	0.073*
N6	0.9483 (9)	−0.0180 (8)	0.7813 (7)	0.064 (2)
H6A	1.0112	0.0134	0.7435	0.076*
H6B	0.8894	−0.1120	0.7475	0.076*
O1W	0.7341 (7)	0.3408 (9)	0.9023 (6)	0.074 (2)
O2WA	0.2417 (12)	0.2587 (12)	0.7880 (10)	0.082 (4)*	0.703 (17)
O2WB	0.063 (5)	0.108 (5)	0.631 (5)	0.18 (2)*	0.297 (17)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0164 (4)	0.0168 (5)	0.0200 (5)	0.0099 (3)	0.0038 (4)	0.0073 (4)
V2	0.0180 (4)	0.0218 (5)	0.0200 (5)	0.0095 (4)	0.0055 (4)	0.0113 (4)
As1	0.0179 (3)	0.0225 (3)	0.0212 (3)	0.0109 (2)	0.0055 (2)	0.0093 (2)
As2	0.0159 (3)	0.0134 (3)	0.0203 (3)	0.0069 (2)	0.0036 (2)	0.0089 (2)
As3	0.0180 (3)	0.0178 (3)	0.0190 (3)	0.0090 (2)	0.0025 (2)	0.0055 (2)
O1	0.026 (2)	0.029 (2)	0.034 (2)	0.0197 (18)	0.0072 (18)	0.0131 (19)
O2	0.0200 (18)	0.0169 (19)	0.022 (2)	0.0090 (15)	0.0038 (15)	0.0109 (16)
O3	0.0208 (18)	0.0184 (19)	0.025 (2)	0.0113 (15)	0.0075 (16)	0.0136 (17)
O4	0.0168 (18)	0.0189 (19)	0.0205 (19)	0.0072 (15)	0.0075 (15)	0.0062 (16)
O5	0.0183 (18)	0.0166 (19)	0.022 (2)	0.0088 (15)	0.0058 (15)	0.0067 (16)
O6	0.0197 (18)	0.0189 (19)	0.020 (2)	0.0072 (15)	0.0042 (15)	0.0069 (16)
O7	0.0196 (19)	0.027 (2)	0.027 (2)	0.0131 (16)	0.0031 (17)	0.0086 (18)
O8	0.032 (2)	0.044 (3)	0.033 (2)	0.018 (2)	0.013 (2)	0.027 (2)
O9	0.0207 (19)	0.023 (2)	0.022 (2)	0.0098 (16)	0.0057 (16)	0.0120 (17)
O10	0.022 (2)	0.025 (2)	0.024 (2)	0.0098 (16)	0.0073 (17)	0.0076 (18)
O11	0.027 (2)	0.046 (3)	0.052 (3)	0.010 (2)	0.014 (2)	0.035 (3)
O12	0.022 (2)	0.026 (2)	0.037 (2)	0.0171 (17)	0.0060 (18)	0.0053 (19)
O13	0.027 (2)	0.019 (2)	0.027 (2)	0.0086 (16)	0.0018 (17)	0.0084 (17)
O14	0.030 (2)	0.031 (2)	0.023 (2)	0.0181 (19)	−0.0040 (18)	0.0021 (19)
O15	0.029 (2)	0.0147 (19)	0.034 (2)	0.0065 (16)	−0.0027 (18)	0.0091 (18)
C1	0.039 (4)	0.026 (3)	0.049 (4)	0.018 (3)	0.018 (3)	0.026 (3)
N1	0.059 (4)	0.024 (3)	0.050 (4)	0.012 (3)	0.024 (3)	0.024 (3)
N2	0.082 (5)	0.036 (4)	0.052 (4)	0.026 (3)	0.042 (4)	0.028 (3)
N3	0.066 (4)	0.032 (3)	0.049 (4)	0.011 (3)	0.027 (3)	0.023 (3)
C2	0.048 (4)	0.030 (4)	0.037 (4)	0.019 (3)	0.007 (3)	0.011 (3)
N4	0.057 (5)	0.051 (5)	0.078 (6)	0.017 (4)	0.028 (4)	0.018 (4)
N5	0.090 (6)	0.031 (4)	0.045 (4)	0.016 (4)	0.032 (4)	0.012 (3)
N6	0.096 (6)	0.036 (4)	0.050 (4)	0.030 (4)	0.031 (4)	0.012 (3)
O1W	0.062 (4)	0.101 (5)	0.049 (4)	0.019 (4)	0.003 (3)	0.047 (4)

Geometric parameters (Å, º)

V1—O1	1.591 (4)	O3—As2^i	1.671 (4)
V1—O2	1.723 (4)	O7—As1^i	1.665 (4)
V1—O5	1.963 (4)	O12—H12	0.9769
V1—O4	1.992 (4)	O14—H14	0.9637
V1—O6	2.029 (4)	O15—H15	0.9600
V1—O3	2.376 (4)	C1—N2	1.304 (9)
V2—O8	1.603 (5)	C1—N3	1.309 (9)
V2—O2	1.934 (4)	C1—N1	1.330 (8)
V2—O9	2.006 (4)	N1—H1A	0.8600
V2—O7	2.015 (4)	N1—H1B	0.8600
V2—O10	2.027 (4)	N2—H2A	0.8600
V2—O3	2.260 (4)	N2—H2B	0.8600
As1—O6	1.649 (4)	N3—H3A	0.8600
As1—O7^i	1.665 (4)	N3—H3B	0.8600
As1—O12	1.708 (4)	C2—N6	1.304 (9)
As1—O11	1.726 (5)	C2—N5	1.313 (9)
As2—O3^i	1.671 (4)	C2—N4	1.318 (10)
As2—O9	1.675 (4)	N4—H4A	0.8600
As2—O5	1.683 (4)	N4—H4B	0.8600
As2—O15	1.719 (4)	N5—H5A	0.8600
As3—O13	1.669 (4)	N5—H5B	0.8600
As3—O10	1.679 (4)	N6—H6A	0.8600
As3—O4	1.687 (4)	N6—H6B	0.8600
As3—O14	1.714 (4)
O1—V1—O2	102.7 (2)	O13—As3—O4	109.0 (2)
O1—V1—O5	99.0 (2)	O10—As3—O4	117.33 (19)
O2—V1—O5	93.43 (17)	O13—As3—O14	108.5 (2)
O1—V1—O4	98.6 (2)	O10—As3—O14	107.1 (2)
O2—V1—O4	90.70 (17)	O4—As3—O14	101.8 (2)
O5—V1—O4	160.49 (18)	V1—O2—V2	119.8 (2)
O1—V1—O6	99.5 (2)	As2^i—O3—V2	136.2 (2)
O2—V1—O6	157.65 (18)	As2^i—O3—V1	137.1 (2)
O5—V1—O6	84.99 (16)	V2—O3—V1	86.10 (14)
O4—V1—O6	83.98 (16)	As3—O4—V1	124.0 (2)
O1—V1—O3	178.9 (2)	As2—O5—V1	121.6 (2)
O2—V1—O3	77.34 (16)	As1—O6—V1	125.2 (2)
O5—V1—O3	82.06 (15)	As1^i—O7—V2	127.5 (2)
O4—V1—O3	80.26 (15)	As2—O9—V2	122.6 (2)
O6—V1—O3	80.37 (15)	As3—O10—V2	124.8 (2)
O8—V2—O2	99.5 (2)	As1—O12—H12	112.3
O8—V2—O9	100.3 (2)	As3—O14—H14	122.9
O2—V2—O9	87.28 (16)	As2—O15—H15	109.3
O8—V2—O7	96.9 (2)	N2—C1—N3	120.6 (6)
O2—V2—O7	163.55 (18)	N2—C1—N1	119.8 (6)
O9—V2—O7	88.82 (16)	N3—C1—N1	119.5 (7)
O8—V2—O10	97.8 (2)	C1—N1—H1A	120.0
O2—V2—O10	87.81 (16)	C1—N1—H1B	120.0
O9—V2—O10	161.83 (17)	H1A—N1—H1B	120.0
O7—V2—O10	90.97 (17)	C1—N2—H2A	120.0
O8—V2—O3	175.3 (2)	C1—N2—H2B	120.0
O2—V2—O3	76.60 (15)	H2A—N2—H2B	120.0
O9—V2—O3	82.29 (15)	C1—N3—H3A	120.0
O7—V2—O3	87.04 (16)	C1—N3—H3B	120.0
O10—V2—O3	79.55 (16)	H3A—N3—H3B	120.0
O6—As1—O7^i	122.0 (2)	N6—C2—N5	121.2 (8)
O6—As1—O12	111.2 (2)	N6—C2—N4	120.1 (7)
O7^i—As1—O12	102.3 (2)	N5—C2—N4	118.7 (7)
O6—As1—O11	103.8 (2)	C2—N4—H4A	120.0
O7^i—As1—O11	110.7 (2)	C2—N4—H4B	120.0
O12—As1—O11	106.1 (2)	H4A—N4—H4B	120.0
O3^i—As2—O9	114.15 (19)	C2—N5—H5A	120.0
O3^i—As2—O5	112.86 (19)	C2—N5—H5B	120.0
O9—As2—O5	112.62 (19)	H5A—N5—H5B	120.0
O3^i—As2—O15	108.9 (2)	C2—N6—H6A	120.0
O9—As2—O15	103.6 (2)	C2—N6—H6B	120.0
O5—As2—O15	103.63 (19)	H6A—N6—H6B	120.0
O13—As3—O10	112.3 (2)
O1—V1—O2—V2	−178.0 (2)	O3^i—As2—O5—V1	92.3 (3)
O5—V1—O2—V2	−77.9 (2)	O9—As2—O5—V1	−38.8 (3)
O4—V1—O2—V2	83.0 (2)	O15—As2—O5—V1	−150.1 (3)
O6—V1—O2—V2	7.3 (6)	O1—V1—O5—As2	152.3 (3)
O3—V1—O2—V2	3.14 (19)	O2—V1—O5—As2	48.8 (3)
O8—V2—O2—V1	179.4 (2)	O4—V1—O5—As2	−53.1 (6)
O9—V2—O2—V1	79.4 (2)	O6—V1—O5—As2	−108.9 (3)
O7—V2—O2—V1	2.9 (7)	O3—V1—O5—As2	−27.9 (2)
O10—V2—O2—V1	−83.1 (2)	O7^i—As1—O6—V1	67.3 (3)
O3—V2—O2—V1	−3.3 (2)	O12—As1—O6—V1	−53.5 (3)
O8—V2—O3—As2^i	−152 (2)	O11—As1—O6—V1	−167.1 (3)
O2—V2—O3—As2^i	173.8 (3)	O1—V1—O6—As1	73.3 (3)
O9—V2—O3—As2^i	84.8 (3)	O2—V1—O6—As1	−111.9 (4)
O7—V2—O3—As2^i	−4.4 (3)	O5—V1—O6—As1	−25.0 (3)
O10—V2—O3—As2^i	−95.9 (3)	O4—V1—O6—As1	171.1 (3)
O8—V2—O3—V1	37 (3)	O3—V1—O6—As1	−107.8 (3)
O2—V2—O3—V1	2.09 (13)	O8—V2—O7—As1^i	−88.3 (3)
O9—V2—O3—V1	−86.94 (14)	O2—V2—O7—As1^i	88.2 (6)
O7—V2—O3—V1	−176.15 (14)	O9—V2—O7—As1^i	12.0 (3)
O10—V2—O3—V1	92.32 (15)	O10—V2—O7—As1^i	173.8 (3)
O1—V1—O3—As2^i	91 (11)	O3—V2—O7—As1^i	94.3 (3)
O2—V1—O3—As2^i	−174.0 (3)	O3^i—As2—O9—V2	−85.4 (3)
O5—V1—O3—As2^i	−78.6 (3)	O5—As2—O9—V2	45.0 (3)
O4—V1—O3—As2^i	93.1 (3)	O15—As2—O9—V2	156.3 (2)
O6—V1—O3—As2^i	7.6 (3)	O8—V2—O9—As2	−153.2 (3)
O1—V1—O3—V2	−97 (10)	O2—V2—O9—As2	−54.0 (3)
O2—V1—O3—V2	−2.33 (14)	O7—V2—O9—As2	110.0 (3)
O5—V1—O3—V2	93.02 (15)	O10—V2—O9—As2	20.5 (7)
O4—V1—O3—V2	−95.27 (15)	O3—V2—O9—As2	22.8 (2)
O6—V1—O3—V2	179.25 (15)	O13—As3—O10—V2	109.2 (3)
O13—As3—O4—V1	−112.7 (3)	O4—As3—O10—V2	−18.1 (4)
O10—As3—O4—V1	16.3 (4)	O14—As3—O10—V2	−131.8 (3)
O14—As3—O4—V1	132.8 (3)	O8—V2—O10—As3	137.6 (3)
O1—V1—O4—As3	−142.3 (3)	O2—V2—O10—As3	38.3 (3)
O2—V1—O4—As3	−39.3 (3)	O9—V2—O10—As3	−36.1 (7)
O5—V1—O4—As3	63.0 (6)	O7—V2—O10—As3	−125.3 (3)
O6—V1—O4—As3	118.9 (3)	O3—V2—O10—As3	−38.5 (3)
O3—V1—O4—As3	37.7 (3)

Symmetry code: (i) −x, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O12—H12···O4^ii	0.98	1.72	2.678 (5)	165
O14—H14···O13^iii	0.96	1.66	2.579 (6)	158
O15—H15···O13^i	0.96	1.67	2.619 (6)	170
N1—H1B···O13^iv	0.86	2.26	3.056 (8)	154
N1—H1A···O6^iv	0.86	2.18	3.007 (7)	160
N2—H2A···O15^v	0.86	2.20	3.042 (8)	167
N2—H2B···O11^iv	0.86	2.44	3.210 (8)	150
N2—H2B···O1^vi	0.86	2.47	3.040 (8)	125
N3—H3A···O9^v	0.86	2.05	2.895 (7)	169
N3—H3B···O1W	0.86	2.20	2.984 (10)	152
N4—H4A···O12^vi	0.86	2.30	3.089 (9)	152
N4—H4B···O10^vii	0.86	2.48	3.230 (9)	146
N5—H5A···O2WA^v	0.86	2.14	2.959 (13)	160
N5—H5B···O7^vii	0.86	2.19	2.963 (8)	150
N6—H6B···O12^vi	0.86	2.37	3.140 (9)	150
N6—H6B···O5^vi	0.86	2.45	3.022 (7)	125
N6—H6A···O2WB^v	0.86	2.01	2.78 (5)	148

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