Guanyl­urea vanadium arsenate

The title compound consists of anionic [V₄As₆O₃₀H₆]^4- clusters, each accompanied by four guanyl­urea (C₂N₄OH₇⁺) cations. An extensive hydrogen-bonding network stabilizes the crystal packing.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](N-C) = 0.004 Å
• R factor = 0.024
• wR factor = 0.064
• Data-to-parameter ratio = 20.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



ABSTM_02  Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
          Tmin and Tmax reported:      0.291     0.408
          Tmin and Tmax expected:      0.213     0.335
          RR =      1.122
          Please check that your absorption correction is appropriate.

PLAT_420  Alert C D-H Without Acceptor       N(6)   -   H(6A)             ?

General Notes



ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      0.822
          Tmax scaled      0.335 Tmin scaled      0.239


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

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Computing details

Data collection: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SMART; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

(I)

Crystal data

(C2H7N4O)4[As6V4O30H6]	F(000) = 756
Mr = 1551.8	Dx = 2.360 Mg m^−3
Triclinic, P1	Melting point: decomposes before melting K
a = 8.5376 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.0544 (5) Å	Cell parameters from 5166 reflections
c = 12.4672 (5) Å	θ = 2.5–30.0°
α = 83.144 (1)°	µ = 5.46 mm^−1
β = 82.652 (1)°	T = 293 K
γ = 69.848 (1)°	Block, orange
V = 1091.94 (8) Å^3	0.30 × 0.30 × 0.20 mm
Z = 1

Data collection

Bruker SMART1000 CCD diffractometer	6216 independent reflections
Radiation source: fine-focus sealed tube	5186 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.014
ω scans	θmax = 30.1°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −11→12
Tmin = 0.291, Tmax = 0.408	k = −12→15
8831 measured reflections	l = −16→17

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: geom and difmap
R[F^2 > 2σ(F^2)] = 0.024	H-atom parameters constrained
wR(F^2) = 0.064	w = 1/[σ^2(Fo^2) + (0.0351P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max < 0.001
6216 reflections	Δρmax = 0.78 e Å^−3
308 parameters	Δρmin = −0.64 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0018 (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	−0.26946 (5)	0.18547 (4)	0.37820 (3)	0.01877 (9)
V2	−0.21925 (5)	−0.11316 (4)	0.40837 (3)	0.01860 (9)
As1	−0.04458 (3)	0.34667 (2)	0.457163 (19)	0.01793 (6)
As2	0.17156 (3)	−0.03041 (2)	0.396133 (18)	0.01588 (6)
As3	−0.12953 (3)	0.01510 (2)	0.171539 (19)	0.02164 (6)
O1	−0.2244 (2)	−0.08800 (15)	0.55962 (13)	0.0190 (3)
O2	−0.3534 (2)	−0.18402 (18)	0.42187 (15)	0.0298 (4)
O3	−0.2617 (2)	0.17401 (15)	0.53482 (13)	0.0195 (3)
O4	−0.0170 (2)	−0.25661 (15)	0.42544 (13)	0.0219 (3)
O5	−0.3555 (2)	0.06089 (16)	0.39118 (13)	0.0203 (3)
O6	−0.2280 (2)	0.46583 (16)	0.49477 (15)	0.0266 (4)
H6	−0.1976	0.5223	0.5310	0.032*
O7	−0.4287 (2)	0.31356 (17)	0.36692 (16)	0.0296 (4)
O8	−0.03300 (19)	0.00315 (15)	0.38898 (13)	0.0185 (3)
O9	−0.1777 (2)	−0.10362 (16)	0.25346 (14)	0.0250 (4)
O10	−0.0975 (2)	0.27133 (16)	0.36545 (13)	0.0229 (3)
O11	0.1011 (2)	0.40706 (18)	0.39949 (14)	0.0279 (4)
O12	−0.2017 (2)	0.16044 (16)	0.22329 (14)	0.0251 (4)
O13	0.2732 (2)	−0.04863 (17)	0.26822 (13)	0.0245 (4)
H13	0.2079	−0.0328	0.2195	0.029*
O14	−0.2441 (2)	0.0373 (2)	0.06210 (15)	0.0321 (4)
H14	−0.1759	0.0248	−0.0016	0.038*
O15	0.0729 (2)	−0.0325 (2)	0.12805 (14)	0.0321 (4)
O20	−0.1667 (3)	0.6046 (2)	0.07381 (18)	0.0474 (6)
N1	−0.2864 (3)	0.5152 (2)	0.22299 (19)	0.0319 (5)
H1	−0.2803	0.4441	0.2616	0.038*
N2	−0.0697 (3)	0.3878 (2)	0.1141 (2)	0.0431 (7)
H2A	0.0051	0.3745	0.0596	0.052*
H2B	−0.0794	0.3238	0.1577	0.052*
N3	−0.4219 (3)	0.7370 (2)	0.2048 (2)	0.0376 (6)
H3A	−0.5004	0.8051	0.2259	0.045*
H3B	−0.3530	0.7430	0.1494	0.045*
N4	−0.5102 (3)	0.6112 (2)	0.34181 (19)	0.0341 (5)
H4A	−0.5897	0.6779	0.3646	0.041*
H4B	−0.4980	0.5360	0.3746	0.041*
C1	−0.4075 (3)	0.6244 (2)	0.2568 (2)	0.0257 (5)
C2	−0.1706 (3)	0.5074 (3)	0.1310 (2)	0.0310 (6)
O21	0.3531 (3)	0.5687 (2)	0.07469 (19)	0.0550 (7)
N5	0.4783 (3)	0.3094 (2)	0.0895 (2)	0.0419 (6)
H5A	0.5415	0.2339	0.0716	0.050*
H5B	0.4874	0.3773	0.0517	0.050*
N6	0.3521 (4)	0.2176 (3)	0.2338 (2)	0.0456 (7)
H6A	0.4143	0.1415	0.2170	0.055*
H6B	0.2792	0.2267	0.2893	0.055*
N7	0.2652 (3)	0.4366 (2)	0.20497 (19)	0.0337 (5)
H7	0.1950	0.4361	0.2609	0.040*
N8	0.1495 (3)	0.6564 (3)	0.2032 (2)	0.0500 (7)
H8A	0.1392	0.7343	0.1776	0.060*
H8B	0.0874	0.6427	0.2600	0.060*
C3	0.3685 (3)	0.3207 (3)	0.1743 (2)	0.0317 (6)
C4	0.2613 (3)	0.5573 (3)	0.1548 (2)	0.0334 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.02214 (19)	0.01713 (18)	0.01638 (19)	−0.00579 (15)	−0.00246 (15)	−0.00047 (14)
V2	0.02208 (19)	0.01852 (19)	0.01661 (19)	−0.00855 (15)	−0.00123 (15)	−0.00201 (14)
As1	0.02189 (12)	0.01659 (11)	0.01637 (12)	−0.00879 (9)	0.00073 (9)	−0.00098 (8)
As2	0.01677 (11)	0.01719 (11)	0.01333 (11)	−0.00568 (8)	0.00048 (8)	−0.00184 (8)
As3	0.02475 (13)	0.02618 (13)	0.01307 (12)	−0.00717 (10)	−0.00201 (9)	−0.00182 (9)
O1	0.0244 (8)	0.0189 (8)	0.0159 (8)	−0.0108 (7)	0.0007 (6)	−0.0023 (6)
O2	0.0345 (10)	0.0330 (10)	0.0288 (10)	−0.0197 (9)	−0.0012 (8)	−0.0056 (8)
O3	0.0221 (8)	0.0174 (8)	0.0163 (8)	−0.0033 (6)	−0.0006 (6)	−0.0019 (6)
O4	0.0278 (9)	0.0189 (8)	0.0172 (8)	−0.0060 (7)	−0.0022 (7)	−0.0004 (6)
O5	0.0202 (8)	0.0213 (8)	0.0196 (8)	−0.0065 (7)	−0.0029 (6)	−0.0023 (6)
O6	0.0249 (9)	0.0211 (8)	0.0325 (10)	−0.0051 (7)	−0.0009 (7)	−0.0076 (7)
O7	0.0305 (10)	0.0220 (9)	0.0321 (10)	−0.0019 (8)	−0.0079 (8)	−0.0014 (7)
O8	0.0175 (7)	0.0185 (8)	0.0194 (8)	−0.0063 (6)	−0.0014 (6)	−0.0007 (6)
O9	0.0369 (10)	0.0234 (9)	0.0162 (8)	−0.0117 (8)	−0.0020 (7)	−0.0032 (7)
O10	0.0324 (9)	0.0232 (8)	0.0168 (8)	−0.0144 (7)	−0.0019 (7)	−0.0009 (6)
O11	0.0348 (10)	0.0327 (10)	0.0224 (9)	−0.0214 (8)	0.0064 (7)	−0.0049 (7)
O12	0.0355 (10)	0.0238 (9)	0.0157 (8)	−0.0096 (8)	−0.0041 (7)	0.0000 (7)
O13	0.0246 (9)	0.0346 (10)	0.0126 (8)	−0.0080 (7)	0.0023 (6)	−0.0055 (7)
O14	0.0318 (10)	0.0477 (12)	0.0159 (9)	−0.0104 (9)	−0.0057 (7)	−0.0044 (8)
O15	0.0237 (9)	0.0525 (12)	0.0164 (9)	−0.0081 (9)	0.0004 (7)	−0.0053 (8)
O20	0.0509 (13)	0.0312 (11)	0.0448 (13)	−0.0064 (10)	0.0213 (10)	0.0058 (10)
N1	0.0365 (12)	0.0228 (11)	0.0264 (12)	−0.0032 (9)	0.0104 (9)	0.0021 (9)
N2	0.0422 (14)	0.0311 (13)	0.0386 (15)	−0.0001 (11)	0.0198 (11)	0.0023 (11)
N3	0.0410 (14)	0.0242 (12)	0.0380 (14)	−0.0042 (10)	0.0107 (11)	−0.0005 (10)
N4	0.0342 (12)	0.0259 (11)	0.0320 (13)	−0.0019 (10)	0.0098 (10)	−0.0013 (10)
C1	0.0252 (12)	0.0249 (12)	0.0241 (13)	−0.0053 (10)	−0.0010 (10)	−0.0014 (10)
C2	0.0299 (14)	0.0306 (14)	0.0270 (14)	−0.0061 (11)	0.0045 (11)	−0.0012 (11)
O21	0.0648 (16)	0.0346 (12)	0.0480 (14)	−0.0090 (11)	0.0306 (12)	0.0026 (10)
N5	0.0430 (14)	0.0306 (13)	0.0386 (15)	−0.0032 (11)	0.0113 (11)	0.0056 (11)
N6	0.0523 (16)	0.0410 (15)	0.0436 (16)	−0.0225 (13)	0.0030 (13)	0.0095 (12)
N7	0.0326 (12)	0.0423 (14)	0.0228 (12)	−0.0136 (11)	0.0105 (9)	−0.0003 (10)
N8	0.0480 (16)	0.0423 (16)	0.0436 (17)	−0.0004 (13)	0.0132 (13)	−0.0052 (13)
C3	0.0304 (14)	0.0388 (15)	0.0263 (14)	−0.0147 (12)	−0.0034 (11)	0.0065 (11)
C4	0.0315 (14)	0.0364 (15)	0.0265 (14)	−0.0060 (12)	0.0019 (11)	−0.0016 (12)

Geometric parameters (Å, º)

V1—O7	1.5960 (18)	O20—C2	1.224 (3)
V1—O5	1.7541 (16)	N1—C1	1.362 (3)
V1—O3	1.9498 (17)	N1—C2	1.405 (3)
V1—O12	1.9678 (18)	N1—H1	0.8600
V1—O10	1.9864 (17)	N2—C2	1.330 (4)
V1—O8	2.3145 (16)	N2—H2A	0.8600
V2—O2	1.5782 (17)	N2—H2B	0.8600
V2—O5	1.8773 (17)	N3—C1	1.307 (3)
V2—O9	1.9154 (17)	N3—H3A	0.8600
V2—O4	1.9155 (17)	N3—H3B	0.8600
V2—O1	1.9314 (16)	N4—C1	1.314 (3)
V2—O8	2.3401 (16)	N4—H4A	0.8600
As1—O11	1.6546 (16)	N4—H4B	0.8600
As1—O10	1.6805 (17)	O21—C4	1.211 (3)
As1—O4^i	1.7023 (16)	N5—C3	1.307 (4)
As1—O6	1.7164 (17)	N5—H5A	0.8600
As2—O8	1.6677 (15)	N5—H5B	0.8600
As2—O3^i	1.6895 (16)	N6—C3	1.323 (3)
As2—O1^i	1.6921 (16)	N6—H6A	0.8600
As2—O13	1.7143 (17)	N6—H6B	0.8600
As3—O15	1.6611 (18)	N7—C3	1.348 (4)
As3—O12	1.6855 (18)	N7—C4	1.395 (4)
As3—O9	1.6969 (17)	N7—H7	0.8600
As3—O14	1.7247 (17)	N8—C4	1.328 (4)
O6—H6	0.9327	N8—H8A	0.8600
O13—H13	0.8390	N8—H8B	0.8600
O14—H14	0.9174
O7—V1—O5	103.46 (9)	As2^i—O3—V1	120.66 (9)
O7—V1—O3	98.51 (9)	As1^i—O4—V2	126.80 (10)
O5—V1—O3	91.06 (7)	V1—O5—V2	120.99 (9)
O7—V1—O12	99.00 (9)	As1—O6—H6	105.9
O5—V1—O12	90.92 (8)	As2—O8—V1	137.38 (9)
O3—V1—O12	161.40 (7)	As2—O8—V2	136.64 (8)
O7—V1—O10	97.23 (9)	V1—O8—V2	85.55 (5)
O5—V1—O10	159.28 (8)	As3—O9—V2	127.28 (10)
O3—V1—O10	86.85 (7)	As1—O10—V1	130.33 (10)
O12—V1—O10	84.79 (7)	As3—O12—V1	124.11 (9)
O7—V1—O8	177.75 (8)	As2—O13—H13	113.2
O5—V1—O8	78.14 (6)	As3—O14—H14	111.2
O3—V1—O8	82.99 (6)	C1—N1—C2	126.3 (2)
O12—V1—O8	79.33 (7)	C1—N1—H1	116.9
O10—V1—O8	81.14 (6)	C2—N1—H1	116.9
O2—V2—O5	101.50 (9)	C2—N2—H2A	120.0
O2—V2—O9	99.09 (9)	C2—N2—H2B	120.0
O5—V2—O9	86.36 (7)	H2A—N2—H2B	120.0
O2—V2—O4	101.18 (9)	C1—N3—H3A	120.0
O5—V2—O4	157.21 (7)	C1—N3—H3B	120.0
O9—V2—O4	92.27 (7)	H3A—N3—H3B	120.0
O2—V2—O1	97.47 (8)	C1—N4—H4A	120.0
O5—V2—O1	87.03 (7)	C1—N4—H4B	120.0
O9—V2—O1	163.09 (7)	H4A—N4—H4B	120.0
O4—V2—O1	87.84 (7)	N3—C1—N4	121.8 (3)
O2—V2—O8	176.72 (8)	N3—C1—N1	120.8 (2)
O5—V2—O8	75.26 (6)	N4—C1—N1	117.4 (2)
O9—V2—O8	81.30 (7)	O20—C2—N2	124.9 (3)
O4—V2—O8	82.04 (6)	O20—C2—N1	121.1 (3)
O1—V2—O8	81.97 (6)	N2—C2—N1	114.0 (2)
O11—As1—O10	109.24 (9)	C3—N5—H5A	120.0
O11—As1—O4^i	110.42 (9)	C3—N5—H5B	120.0
O10—As1—O4^i	115.88 (8)	H5A—N5—H5B	120.0
O11—As1—O6	111.88 (9)	C3—N6—H6A	120.0
O10—As1—O6	104.16 (8)	C3—N6—H6B	120.0
O4^i—As1—O6	105.07 (8)	H6A—N6—H6B	120.0
O8—As2—O3^i	113.03 (8)	C3—N7—C4	126.3 (2)
O8—As2—O1^i	115.14 (8)	C3—N7—H7	116.8
O3^i—As2—O1^i	110.93 (8)	C4—N7—H7	116.8
O8—As2—O13	109.15 (8)	C4—N8—H8A	120.0
O3^i—As2—O13	103.85 (8)	C4—N8—H8B	120.0
O1^i—As2—O13	103.66 (8)	H8A—N8—H8B	120.0
O15—As3—O12	114.29 (10)	N5—C3—N6	121.2 (3)
O15—As3—O9	110.90 (9)	N5—C3—N7	122.3 (3)
O12—As3—O9	114.03 (8)	N6—C3—N7	116.5 (3)
O15—As3—O14	108.74 (9)	O21—C4—N8	123.9 (3)
O12—As3—O14	103.77 (9)	O21—C4—N7	122.1 (3)
O9—As3—O14	104.21 (9)	N8—C4—N7	114.0 (3)
As2^i—O1—V2	123.98 (9)

Symmetry code: (i) −x, −y, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6···O11^ii	0.93	1.68	2.597 (2)	166
O13—H13···O15	0.84	1.72	2.548 (2)	168
O14—H14···O15^iii	0.92	1.71	2.617 (3)	169
N1—H1···O10	0.86	2.37	3.101 (3)	143
N1—H1···O7	0.86	2.41	3.165 (3)	147
N2—H2A···O20^iv	0.86	2.07	2.904 (3)	165
N2—H2B···O12	0.86	2.40	3.191 (3)	154
N2—H2B···O10	0.86	2.58	3.254 (3)	136
N3—H3A···O13^v	0.86	2.10	2.947 (3)	167
N3—H3B···O20	0.86	2.01	2.649 (3)	130
N4—H4A···O3^vi	0.86	2.12	2.952 (3)	161
N4—H4B···O7	0.86	2.33	3.105 (3)	149
N5—H5A···O14^vii	0.86	2.31	3.147 (3)	163
N5—H5B···O21	0.86	2.06	2.685 (3)	128
N5—H5B···O21^viii	0.86	2.12	2.829 (3)	140
N6—H6B···O1^i	0.86	2.39	3.058 (3)	135
N6—H6B···O11	0.86	2.49	3.171 (4)	137
N7—H7···O11	0.86	1.85	2.685 (3)	163
N8—H8A···O15^ix	0.86	2.46	3.312 (4)	171
N8—H8B···O4^ix	0.86	2.38	3.051 (3)	135

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